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Nine hydrated complexes of Group 2 (alkaline earth) cations with organic ligands which are N-substituted amino acids containing the 6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidin-2-yl group have been structurally characterized. The octahydrated calcium glycinate complex, where the six-coordinate Ca cation lies on an inversion centre in the space group P\bar 1, forms a finite (zero-dimensional) complex. The hexahydrated barium glycinate complex contains eight-coordinate Ba and it is isostructural with the known Sr analogue, and its one-dimensional coordination polymer takes the form of a simple chain. The octahydrated calcium and strontium threonine complexes are isostructural, with eight-coordinate cations lying on twofold rotation axes in the space group C2: the one-dimensional coordination polymers take the form of a chain of spiro-fused rings and a similar chain of spiro-fused rings is found in the heptahydrated barium serine complex, although here the ten-coordinate cation lies in a general position. In the tetrahydrated strontium and barium glycylglycinate complexes, the eight-coordinate cations lie on twofold rotation axes in the space group C2/c, but in the Sr complex the coordination polymer is a chain of spiro-fused rings, while in the Ba complex the coordination polymer forms deeply puckered sheets. There are two types of Ca site in the hexahydrated calcium valine complex: one is eight coordinate and gives rise to a two-dimensional coordination polymer, while the other is seven coordinate forming a finite, zero-dimensional coordination complex. In the heptahydrated barium methionine complex, the coordination polymer is three dimensional. In all of the complexes, the coordination aggregates are further linked by an extensive series of hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768103029136/na5011sup1.cif
Contains datablocks global, I, II, III, IV, V, VI, VII, VIII, IX

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50111sup2.fcf
Contains datablock 1

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50112sup3.fcf
Contains datablock 2

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50113sup4.fcf
Contains datablock 3

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50114sup5.fcf
Contains datablock 4

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50115sup6.fcf
Contains datablock 5

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50116sup7.fcf
Contains datablock 6

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50117sup8.fcf
Contains datablock 7

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50118sup9.fcf
Contains datablock 8

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103029136/na50119sup10.fcf
Contains datablock 9

CCDC references: 230832; 230833; 230834; 230835; 230836; 230837; 230838; 230839; 230840

Comment top

In full text version

Experimental top

In full text version

Refinement top

In full text version

Computing details top

For all compounds, data collection: Kappa-CCD server software (Nonius, 1997); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997a) and PRPKAPPA (Ferguson, 1999).

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In full text version.
(I) #Ca(py-gly)2. 8(H2O) top
Crystal data top
C14H24CaN10O12·4(H2O)Z = 1
Mr = 636.58F(000) = 334
Triclinic, P1Dx = 1.605 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.4540 (7) ÅCell parameters from 2833 reflections
b = 7.6148 (11) Åθ = 2.9–27.0°
c = 12.5939 (17) ŵ = 0.33 mm1
α = 95.850 (6)°T = 120 K
β = 97.040 (8)°Lath, pink
γ = 110.038 (8)°0.10 × 0.07 × 0.01 mm
V = 658.52 (14) Å3
Data collection top
Kappa-CCD
diffractometer
2833 independent reflections
Radiation source: fine-focus sealed X-ray tube1311 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.103
ϕ scans, and ω scans with κ offsetsθmax = 27.0°, θmin = 2.9°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 99
Tmin = 0.963, Tmax = 0.998k = 99
5368 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.150H-atom parameters constrained
S = 0.90 w = 1/[σ2(Fo2) + (0.0574P)2]
where P = (Fo2 + 2Fc2)/3
2833 reflections(Δ/σ)max < 0.001
188 parametersΔρmax = 0.39 e Å3
0 restraintsΔρmin = 0.51 e Å3
Crystal data top
C14H24CaN10O12·4(H2O)γ = 110.038 (8)°
Mr = 636.58V = 658.52 (14) Å3
Triclinic, P1Z = 1
a = 7.4540 (7) ÅMo Kα radiation
b = 7.6148 (11) ŵ = 0.33 mm1
c = 12.5939 (17) ÅT = 120 K
α = 95.850 (6)°0.10 × 0.07 × 0.01 mm
β = 97.040 (8)°
Data collection top
Kappa-CCD
diffractometer
2833 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
1311 reflections with I > 2σ(I)
Tmin = 0.963, Tmax = 0.998Rint = 0.103
5368 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0570 restraints
wR(F2) = 0.150H-atom parameters constrained
S = 0.90Δρmax = 0.39 e Å3
2833 reflectionsΔρmin = 0.51 e Å3
188 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.50000.50000.50000.0224 (3)
N10.1464 (4)0.6740 (4)0.9192 (3)0.0207 (8)
C20.0348 (5)0.6066 (5)0.8681 (3)0.0190 (9)
N20.0766 (4)0.4935 (4)0.7736 (3)0.0225 (8)
C1210.0710 (5)0.4482 (5)0.7239 (3)0.0237 (10)
C1220.1635 (5)0.5834 (6)0.6486 (3)0.0247 (10)
O1210.2939 (4)0.5489 (4)0.6072 (2)0.0311 (8)
O1220.1071 (4)0.7171 (4)0.6330 (2)0.0292 (7)
N30.1861 (4)0.6406 (4)0.9076 (3)0.0186 (8)
C30.3839 (5)0.5626 (6)0.8454 (3)0.0259 (10)
C40.1558 (5)0.7495 (5)1.0078 (3)0.0203 (9)
O40.2925 (3)0.7746 (4)1.0436 (2)0.0292 (7)
C50.0419 (5)0.8280 (5)1.0657 (3)0.0203 (9)
N50.0640 (4)0.9379 (5)1.1596 (3)0.0246 (8)
O50.2372 (4)1.0115 (4)1.2156 (2)0.0272 (7)
C60.1858 (5)0.7826 (5)1.0155 (3)0.0216 (10)
N60.3677 (4)0.8490 (5)1.0660 (3)0.0256 (9)
O10.2418 (3)0.2450 (4)0.3919 (2)0.0263 (7)
O20.4387 (4)0.7072 (4)0.3833 (2)0.0271 (7)
O30.2328 (4)0.8914 (4)0.4647 (2)0.0381 (8)
O4W0.6811 (4)0.9173 (4)0.2596 (2)0.0357 (8)
H20.19760.44480.74010.027*
H12A0.01220.31860.68250.028*
H12B0.17360.44840.78190.028*
H3A0.43040.42410.83610.039*
H3B0.38360.60400.77420.039*
H3C0.46950.60780.88450.039*
H6A0.45710.82121.03590.031*
H6B0.39930.92101.12970.031*
H1X0.12110.25980.38060.032*
H1Y0.25070.16240.33380.032*
H2X0.52860.77250.34160.033*
H2Y0.37000.77710.41350.033*
H3X0.17680.83790.52230.046*
H3Y0.22691.01310.46740.046*
H4X0.74380.90110.20100.043*
H4Y0.74181.04360.29350.043*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0213 (6)0.0253 (7)0.0219 (7)0.0101 (5)0.0052 (5)0.0017 (5)
N10.0195 (18)0.0234 (19)0.020 (2)0.0097 (15)0.0036 (15)0.0014 (16)
C20.020 (2)0.020 (2)0.020 (2)0.0086 (17)0.0068 (17)0.0050 (18)
N20.0181 (17)0.029 (2)0.020 (2)0.0080 (15)0.0039 (14)0.0001 (16)
C1210.024 (2)0.025 (2)0.028 (3)0.0130 (18)0.0120 (18)0.0071 (19)
C1220.020 (2)0.027 (3)0.022 (3)0.0050 (19)0.0022 (18)0.003 (2)
O1210.0297 (16)0.0368 (18)0.0344 (19)0.0179 (14)0.0149 (14)0.0072 (15)
O1220.0295 (15)0.0314 (18)0.0337 (19)0.0161 (14)0.0130 (14)0.0089 (14)
N30.0155 (16)0.0196 (18)0.021 (2)0.0073 (14)0.0020 (14)0.0013 (15)
C30.016 (2)0.032 (3)0.028 (3)0.0070 (18)0.0024 (18)0.005 (2)
C40.020 (2)0.020 (2)0.023 (2)0.0071 (18)0.0063 (18)0.0079 (18)
O40.0221 (14)0.0385 (18)0.0306 (18)0.0155 (13)0.0086 (13)0.0010 (14)
C50.017 (2)0.019 (2)0.027 (3)0.0090 (17)0.0054 (17)0.0041 (19)
N50.0291 (19)0.025 (2)0.020 (2)0.0102 (16)0.0038 (16)0.0024 (16)
O50.0240 (15)0.0319 (17)0.0220 (17)0.0091 (13)0.0025 (13)0.0006 (14)
C60.017 (2)0.018 (2)0.028 (3)0.0040 (17)0.0029 (18)0.0061 (19)
N60.0182 (18)0.033 (2)0.026 (2)0.0106 (15)0.0040 (15)0.0004 (17)
O10.0246 (14)0.0304 (17)0.0249 (17)0.0127 (13)0.0026 (12)0.0002 (13)
O20.0285 (15)0.0278 (17)0.0290 (18)0.0130 (13)0.0105 (13)0.0049 (14)
O30.055 (2)0.0322 (18)0.041 (2)0.0249 (16)0.0237 (16)0.0128 (15)
O4W0.0350 (16)0.0350 (19)0.0300 (19)0.0034 (14)0.0134 (14)0.0033 (15)
Geometric parameters (Å, º) top
Ca1—O1212.263 (3)C3—H3A0.98
Ca1—O121i2.263 (3)C3—H3B0.98
Ca1—O1i2.363 (3)C3—H3C0.98
Ca1—O12.363 (3)C4—O41.227 (4)
Ca1—O2i2.379 (3)C4—C51.451 (5)
Ca1—O22.379 (3)C5—N51.335 (5)
N1—C21.321 (5)C5—C61.430 (5)
N1—C61.336 (5)N5—O51.296 (4)
C2—N21.331 (5)C6—N61.323 (5)
C2—N31.377 (4)N6—H6A0.88
N2—C1211.451 (4)N6—H6B0.88
N2—H20.88O1—H1X0.94
C121—C1221.520 (5)O1—H1Y0.94
C121—H12A0.99O2—H2X0.94
C121—H12B0.99O2—H2Y0.94
C122—O1211.247 (4)O3—H3X0.94
C122—O1221.251 (5)O3—H3Y0.94
N3—C41.386 (5)O4W—H4X0.94
N3—C31.471 (4)O4W—H4Y0.94
O121—Ca1—O121i180.000 (1)C122—O121—Ca1167.9 (3)
O121—Ca1—O1i90.01 (9)C2—N3—C4120.7 (3)
O121i—Ca1—O1i89.99 (9)C2—N3—C3121.3 (3)
O121—Ca1—O189.99 (9)C4—N3—C3118.0 (3)
O121i—Ca1—O190.01 (9)N3—C3—H3A109.5
O1i—Ca1—O1180.0N3—C3—H3B109.5
O121—Ca1—O2i88.20 (10)H3A—C3—H3B109.5
O121i—Ca1—O2i91.80 (10)N3—C3—H3C109.5
O1i—Ca1—O2i89.41 (9)H3A—C3—H3C109.5
O1—Ca1—O2i90.59 (9)H3B—C3—H3C109.5
O121—Ca1—O291.80 (10)O4—C4—N3120.1 (3)
O121i—Ca1—O288.20 (10)O4—C4—C5123.4 (4)
O1i—Ca1—O290.59 (9)N3—C4—C5116.5 (3)
O1—Ca1—O289.41 (9)N5—C5—C6128.8 (3)
O2i—Ca1—O2180.00 (10)N5—C5—C4113.9 (3)
C2—N1—C6117.9 (3)C6—C5—C4117.3 (4)
N1—C2—N2118.3 (3)O5—N5—C5117.0 (3)
N1—C2—N3124.4 (3)N6—C6—N1117.4 (3)
N2—C2—N3117.2 (3)N6—C6—C5119.4 (4)
C2—N2—C121122.1 (3)N1—C6—C5123.2 (3)
C2—N2—H2119.0C6—N6—H6A120.0
C121—N2—H2119.0C6—N6—H6B120.0
N2—C121—C122114.2 (3)H6A—N6—H6B120.0
N2—C121—H12A108.7Ca1—O1—H1X116.3
C122—C121—H12A108.7Ca1—O1—H1Y126.6
N2—C121—H12B108.7H1X—O1—H1Y110.1
C122—C121—H12B108.7Ca1—O2—H2X122.9
H12A—C121—H12B107.6Ca1—O2—H2Y111.6
O121—C122—O122125.5 (4)H2X—O2—H2Y114.6
O121—C122—C121114.9 (4)H3X—O3—H3Y107.8
O122—C122—C121119.6 (3)H4X—O4W—H4Y107.4
C6—N1—C2—N2178.0 (4)C2—N3—C4—O4177.9 (3)
C6—N1—C2—N30.0 (6)C3—N3—C4—O41.9 (5)
N1—C2—N2—C1212.1 (6)C2—N3—C4—C51.7 (5)
N3—C2—N2—C121179.8 (3)C3—N3—C4—C5178.5 (3)
C2—N2—C121—C12290.3 (5)O4—C4—C5—N53.0 (6)
N2—C121—C122—O121178.4 (3)N3—C4—C5—N5177.4 (3)
N2—C121—C122—O1221.3 (5)O4—C4—C5—C6178.2 (4)
O122—C122—O121—Ca142.6 (15)N3—C4—C5—C61.4 (5)
C121—C122—O121—Ca1137.7 (11)C6—C5—N5—O51.7 (6)
O1i—Ca1—O121—C122116.5 (13)C4—C5—N5—O5179.6 (3)
O1—Ca1—O121—C12263.5 (13)C2—N1—C6—N6179.9 (3)
O2i—Ca1—O121—C122154.1 (13)C2—N1—C6—C50.2 (6)
O2—Ca1—O121—C12225.9 (13)N5—C5—C6—N62.2 (6)
N1—C2—N3—C41.0 (6)C4—C5—C6—N6179.1 (4)
N2—C2—N3—C4177.0 (4)N5—C5—C6—N1178.2 (4)
N1—C2—N3—C3179.2 (4)C4—C5—C6—N10.5 (6)
N2—C2—N3—C32.8 (5)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O2ii0.882.122.962 (4)159
N6—H6A···O4iii0.882.012.818 (4)152
N6—H6B···O50.881.962.613 (4)130
O1—H1X···O122ii0.941.762.698 (4)177
O1—H1Y···O5iv0.941.752.688 (4)172
O2—H2X···O4W0.941.802.733 (3)172
O2—H2Y···O30.941.702.635 (4)176
O3—H3X···O1220.941.782.710 (4)169
O3—H3Y···O1v0.942.072.914 (4)149
O4W—H4X···O4vi0.942.062.880 (4)145
O4W—H4X···N5vi0.942.433.220 (4)141
O4W—H4Y···O122vii0.941.852.787 (4)172
Symmetry codes: (ii) x, y+1, z+1; (iii) x+1, y, z; (iv) x, y1, z1; (v) x, y+1, z; (vi) x+1, y, z1; (vii) x+1, y+2, z+1.
(II) # Ba(py-gly)2·6(H2O) top
Crystal data top
C14H26BaN10O13·H2OF(000) = 1400
Mr = 697.79Dx = 1.836 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5709 reflections
a = 24.9613 (4) Åθ = 3.0–27.5°
b = 6.9157 (1) ŵ = 1.66 mm1
c = 14.6427 (2) ÅT = 120 K
β = 93.149 (1)°Plate, yellow
V = 2523.88 (6) Å30.42 × 0.36 × 0.08 mm
Z = 4
Data collection top
Kappa-CCD
diffractometer
5709 independent reflections
Radiation source: fine-focus sealed X-ray tube5255 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.074
ϕ scans, and ω scans with κ offsetsθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 3232
Tmin = 0.548, Tmax = 0.881k = 88
26202 measured reflectionsl = 1818
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.078Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.208H-atom parameters constrained
S = 1.19 w = 1/[σ2(Fo2) + (0.0001P)2 + 84.2219P]
where P = (Fo2 + 2Fc2)/3
5739 reflections(Δ/σ)max = 0.001
354 parametersΔρmax = 3.61 e Å3
0 restraintsΔρmin = 4.21 e Å3
Crystal data top
C14H26BaN10O13·H2OV = 2523.88 (6) Å3
Mr = 697.79Z = 4
Monoclinic, P21/cMo Kα radiation
a = 24.9613 (4) ŵ = 1.66 mm1
b = 6.9157 (1) ÅT = 120 K
c = 14.6427 (2) Å0.42 × 0.36 × 0.08 mm
β = 93.149 (1)°
Data collection top
Kappa-CCD
diffractometer
5709 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
5255 reflections with I > 2σ(I)
Tmin = 0.548, Tmax = 0.881Rint = 0.074
26202 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0780 restraints
wR(F2) = 0.208H-atom parameters constrained
S = 1.19 w = 1/[σ2(Fo2) + (0.0001P)2 + 84.2219P]
where P = (Fo2 + 2Fc2)/3
5739 reflectionsΔρmax = 3.61 e Å3
354 parametersΔρmin = 4.21 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.28290 (2)0.15712 (8)0.40763 (4)0.01888 (17)
N110.0197 (3)0.2742 (13)0.5389 (5)0.0230 (17)
C120.0508 (4)0.2492 (15)0.4676 (7)0.0227 (19)
N120.1031 (3)0.2668 (14)0.4842 (6)0.0272 (19)
C1210.1288 (4)0.3121 (17)0.5734 (7)0.028 (2)
C1220.1876 (4)0.3548 (15)0.5618 (7)0.025 (2)
O1210.2049 (3)0.3486 (14)0.4846 (6)0.0367 (19)
O1220.2148 (3)0.3955 (13)0.6343 (6)0.0361 (19)
C130.0689 (5)0.193 (2)0.3045 (8)0.037 (3)
N130.0315 (3)0.2104 (13)0.3803 (5)0.0232 (17)
C140.0234 (4)0.1826 (17)0.3593 (7)0.029 (2)
O140.0390 (3)0.1406 (15)0.2808 (5)0.043 (2)
C150.0580 (4)0.2084 (15)0.4343 (7)0.024 (2)
N150.1100 (3)0.1776 (14)0.4129 (6)0.0290 (19)
O150.1430 (3)0.2029 (14)0.4762 (6)0.041 (2)
C160.0339 (4)0.2567 (15)0.5230 (7)0.023 (2)
N160.0638 (4)0.2839 (16)0.5935 (7)0.036 (2)
N210.4570 (3)0.1253 (12)0.1756 (5)0.0219 (17)
C220.4304 (4)0.1476 (14)0.0969 (6)0.0197 (18)
N220.3784 (3)0.1054 (12)0.0892 (5)0.0204 (16)
C2210.3502 (4)0.0397 (15)0.1675 (6)0.0220 (19)
C2220.3302 (4)0.2007 (15)0.2291 (6)0.0211 (19)
O2210.3181 (3)0.1531 (11)0.3080 (5)0.0284 (16)
O2220.3252 (4)0.3676 (11)0.1962 (5)0.037 (2)
C230.4202 (4)0.2492 (16)0.0678 (6)0.027 (2)
N230.4533 (3)0.2130 (12)0.0163 (5)0.0198 (16)
C240.5076 (4)0.2567 (14)0.0174 (6)0.0204 (19)
O240.5274 (3)0.3210 (12)0.0523 (5)0.0301 (17)
C250.5388 (4)0.2191 (15)0.1021 (6)0.0218 (19)
N250.5909 (3)0.2507 (13)0.0981 (6)0.0266 (18)
O250.6215 (3)0.2189 (12)0.1707 (5)0.0299 (16)
C260.5096 (4)0.1528 (14)0.1798 (6)0.0203 (18)
N260.5374 (4)0.1197 (15)0.2577 (6)0.031 (2)
O10.2525 (3)0.3755 (12)0.2564 (5)0.0342 (18)
O20.3531 (3)0.1068 (13)0.5582 (5)0.0328 (18)
O30.3013 (3)0.5615 (11)0.4386 (5)0.0304 (16)
O40.2469 (3)0.1107 (15)0.5340 (6)0.044 (2)
O50.1944 (3)0.0024 (13)0.3132 (6)0.0388 (19)
O60.1579 (4)0.3867 (15)0.2901 (6)0.047 (2)
H120.12390.25010.43820.033*
H12A0.12530.20120.61540.033*
H12B0.11130.42570.60010.033*
H13A0.09130.07770.31420.056*
H13B0.09180.30790.30360.056*
H13C0.04800.18180.24600.056*
H16A0.04860.31200.64750.043*
H16B0.09890.27400.58650.043*
H220.36080.11760.03580.024*
H22A0.31910.03900.14520.026*
H22B0.37450.04570.20500.026*
H23A0.39280.34630.05590.040*
H23B0.44290.29670.11540.040*
H23C0.40270.12880.08830.040*
H26A0.52090.08000.30590.037*
H26B0.57240.13740.26140.037*
H11C0.27950.44100.23490.041*
H12D0.23150.30450.21100.041*
H21C0.38860.13220.54740.039*
H22D0.35820.01550.60140.039*
H31C0.30750.66080.39870.036*
H32D0.27190.60500.47720.036*
H41C0.21190.14900.54100.053*
H42D0.26780.12160.58700.053*
H51C0.18750.14610.31920.047*
H51D0.19760.02410.25320.047*
H61C0.13940.36810.22950.056*
H62D0.18980.47680.29370.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.0210 (3)0.0207 (3)0.0151 (3)0.0007 (2)0.00249 (18)0.0004 (2)
N110.020 (4)0.031 (5)0.019 (4)0.000 (3)0.002 (3)0.002 (3)
C120.024 (5)0.022 (5)0.022 (5)0.003 (4)0.000 (4)0.005 (4)
N120.019 (4)0.043 (5)0.020 (4)0.002 (4)0.000 (3)0.001 (4)
C1210.028 (5)0.031 (6)0.023 (5)0.004 (4)0.000 (4)0.007 (4)
C1220.018 (4)0.021 (5)0.036 (5)0.004 (4)0.001 (4)0.004 (4)
O1210.025 (4)0.051 (5)0.035 (4)0.001 (4)0.007 (3)0.009 (4)
O1220.025 (4)0.047 (5)0.035 (4)0.000 (4)0.009 (3)0.001 (4)
C130.031 (5)0.057 (8)0.025 (5)0.009 (5)0.010 (4)0.007 (5)
N130.021 (4)0.034 (5)0.015 (4)0.002 (3)0.004 (3)0.002 (3)
C140.025 (5)0.033 (6)0.028 (5)0.006 (4)0.002 (4)0.004 (4)
O140.039 (4)0.071 (7)0.019 (4)0.009 (4)0.007 (3)0.001 (4)
C150.021 (4)0.025 (5)0.024 (5)0.001 (4)0.005 (4)0.006 (4)
N150.023 (4)0.031 (5)0.032 (5)0.003 (4)0.002 (3)0.001 (4)
O150.026 (4)0.049 (5)0.049 (5)0.001 (4)0.005 (4)0.000 (4)
C160.025 (5)0.022 (5)0.022 (5)0.002 (4)0.001 (4)0.003 (4)
N160.021 (4)0.052 (6)0.034 (5)0.002 (4)0.006 (4)0.008 (5)
N210.027 (4)0.023 (4)0.016 (4)0.004 (3)0.005 (3)0.001 (3)
C220.028 (5)0.017 (4)0.015 (4)0.001 (4)0.009 (3)0.002 (3)
N220.022 (4)0.025 (4)0.014 (3)0.002 (3)0.005 (3)0.002 (3)
C2210.023 (4)0.021 (5)0.022 (4)0.003 (4)0.010 (4)0.001 (4)
C2220.021 (4)0.025 (5)0.018 (4)0.004 (4)0.003 (3)0.002 (4)
O2210.041 (4)0.029 (4)0.016 (3)0.002 (3)0.007 (3)0.001 (3)
O2220.062 (6)0.022 (4)0.029 (4)0.010 (4)0.017 (4)0.006 (3)
C230.034 (5)0.029 (6)0.017 (4)0.004 (4)0.004 (4)0.001 (4)
N230.026 (4)0.020 (4)0.013 (3)0.000 (3)0.005 (3)0.003 (3)
C240.033 (5)0.017 (4)0.012 (4)0.003 (4)0.010 (4)0.001 (3)
O240.029 (4)0.039 (5)0.023 (4)0.005 (3)0.009 (3)0.005 (3)
C250.020 (4)0.025 (5)0.022 (4)0.006 (4)0.009 (4)0.007 (4)
N250.026 (4)0.025 (5)0.030 (4)0.004 (4)0.007 (3)0.006 (4)
O250.020 (3)0.039 (4)0.031 (4)0.004 (3)0.003 (3)0.001 (3)
C260.024 (4)0.017 (4)0.021 (4)0.004 (4)0.011 (4)0.005 (4)
N260.027 (4)0.048 (6)0.018 (4)0.008 (4)0.004 (3)0.001 (4)
O10.038 (4)0.035 (5)0.029 (4)0.011 (4)0.000 (3)0.005 (3)
O20.024 (4)0.049 (5)0.026 (4)0.005 (3)0.004 (3)0.016 (4)
O30.036 (4)0.030 (4)0.027 (4)0.002 (3)0.007 (3)0.000 (3)
O40.030 (4)0.065 (6)0.037 (4)0.018 (4)0.000 (3)0.018 (4)
O50.037 (4)0.041 (5)0.038 (4)0.007 (4)0.001 (4)0.000 (4)
O60.037 (5)0.053 (6)0.049 (5)0.003 (4)0.008 (4)0.002 (5)
Geometric parameters (Å, º) top
Ba1—O1212.656 (8)C22—N231.414 (11)
Ba1—O12.752 (8)N22—C2211.450 (11)
Ba1—O22.762 (7)N22—H220.88
Ba1—O2212.765 (7)C221—C2221.534 (13)
Ba1—O52.771 (8)C221—H22A0.99
Ba1—O42.802 (8)C221—H22B0.99
Ba1—O25i2.837 (7)C222—O2221.254 (12)
Ba1—O32.866 (8)C222—O2211.255 (11)
Ba1—N25i3.220 (9)C23—N231.466 (12)
N11—C121.346 (12)C23—H23A0.98
N11—C161.350 (12)C23—H23B0.98
C12—N121.321 (12)C23—H23C0.98
C12—N131.367 (12)N23—C241.390 (12)
N12—C1211.458 (13)C24—O241.240 (11)
N12—H120.88C24—C251.451 (13)
C121—C1221.516 (14)C25—N251.323 (12)
C121—H12A0.99C25—C261.457 (12)
C121—H12B0.99N25—O251.293 (11)
C122—O1211.233 (13)N25—Ba1ii3.220 (9)
C122—O1221.259 (13)O25—Ba1ii2.837 (7)
C13—N131.493 (13)C26—N261.323 (13)
C13—H13A0.98N26—H26A0.88
C13—H13B0.98N26—H26B0.88
C13—H13C0.98O1—H11C0.8841
N13—C141.402 (13)O1—H12D0.9597
C14—O141.227 (13)O2—H21C0.9255
C14—C151.446 (15)O2—H22D0.8979
C15—N151.334 (12)O3—H31C0.9206
C15—C161.440 (13)O3—H32D0.9965
N15—O151.285 (12)O4—H41C0.9226
C16—N161.320 (13)O4—H42D0.9147
N16—H16A0.88O5—H51C1.0132
N16—H16B0.88O5—H51D0.9046
N21—C221.308 (12)O6—H61C0.9868
N21—C261.325 (12)O6—H62D1.0088
C22—N221.329 (12)
O121—Ba1—O183.8 (3)C16—C15—C14118.4 (9)
O121—Ba1—O299.9 (2)O15—N15—C15117.6 (9)
O1—Ba1—O2147.8 (2)N16—C16—N11116.7 (9)
O121—Ba1—O221150.7 (2)N16—C16—C15120.8 (9)
O1—Ba1—O22194.8 (2)N11—C16—C15122.5 (9)
O2—Ba1—O22196.8 (2)C16—N16—H16A120.0
O121—Ba1—O580.1 (3)C16—N16—H16B120.0
O1—Ba1—O568.9 (2)H16A—N16—H16B120.0
O2—Ba1—O5143.3 (2)C22—N21—C26118.6 (8)
O221—Ba1—O572.3 (2)N21—C22—N22119.8 (8)
O121—Ba1—O477.3 (3)N21—C22—N23124.3 (9)
O1—Ba1—O4144.1 (2)N22—C22—N23115.9 (8)
O2—Ba1—O466.5 (2)C22—N22—C221121.0 (8)
O221—Ba1—O487.6 (3)C22—N22—H22119.5
O5—Ba1—O477.9 (3)C221—N22—H22119.5
O121—Ba1—O25i132.3 (3)N22—C221—C222115.1 (8)
O1—Ba1—O25i73.1 (2)N22—C221—H22A108.5
O2—Ba1—O25i81.4 (2)C222—C221—H22A108.5
O221—Ba1—O25i73.9 (2)N22—C221—H22B108.5
O5—Ba1—O25i125.8 (2)C222—C221—H22B108.5
O4—Ba1—O25i140.8 (2)H22A—C221—H22B107.5
O121—Ba1—O364.0 (2)O222—C222—O221124.9 (10)
O1—Ba1—O368.1 (2)O222—C222—C221118.1 (8)
O2—Ba1—O384.7 (2)O221—C222—C221117.0 (9)
O221—Ba1—O3142.0 (2)C222—O221—Ba1142.1 (7)
O5—Ba1—O3125.7 (2)N23—C23—H23A109.5
O4—Ba1—O3126.5 (3)N23—C23—H23B109.5
O25i—Ba1—O368.8 (2)H23A—C23—H23B109.5
O121—Ba1—N25i130.8 (2)N23—C23—H23C109.5
O1—Ba1—N25i95.6 (2)H23A—C23—H23C109.5
O2—Ba1—N25i57.8 (2)H23B—C23—H23C109.5
O221—Ba1—N25i78.5 (2)C24—N23—C22120.0 (8)
O5—Ba1—N25i145.1 (2)C24—N23—C23118.5 (8)
O4—Ba1—N25i119.9 (2)C22—N23—C23121.4 (8)
O25i—Ba1—N25i23.6 (2)O24—C24—N23120.2 (9)
O3—Ba1—N25i70.3 (2)O24—C24—C25123.3 (9)
C12—N11—C16117.6 (8)N23—C24—C25116.6 (8)
N12—C12—N11116.9 (9)N25—C25—C24114.5 (9)
N12—C12—N13119.0 (9)N25—C25—C26128.3 (9)
N11—C12—N13124.2 (9)C24—C25—C26117.2 (8)
C12—N12—C121124.6 (9)O25—N25—C25118.3 (9)
C12—N12—H12117.7O25—N25—Ba1ii61.3 (5)
C121—N12—H12117.7C25—N25—Ba1ii177.8 (7)
N12—C121—C122108.8 (8)N25—O25—Ba1ii95.1 (5)
N12—C121—H12A109.9N26—C26—N21119.1 (9)
C122—C121—H12A109.9N26—C26—C25117.9 (9)
N12—C121—H12B109.9N21—C26—C25123.0 (9)
C122—C121—H12B109.9C26—N26—H26A120.0
H12A—C121—H12B108.3C26—N26—H26B120.0
O121—C122—O122125.5 (10)H26A—N26—H26B120.0
O121—C122—C121119.1 (9)Ba1—O1—H11C112.7
O122—C122—C121115.4 (9)Ba1—O1—H12D113.1
C122—O121—Ba1135.1 (7)H11C—O1—H12D114.4
N13—C13—H13A109.5Ba1—O2—H21C114.3
N13—C13—H13B109.5Ba1—O2—H22D135.3
H13A—C13—H13B109.5H21C—O2—H22D98.8
N13—C13—H13C109.5Ba1—O3—H31C131.2
H13A—C13—H13C109.5Ba1—O3—H32D105.6
H13B—C13—H13C109.5H31C—O3—H32D106.8
C12—N13—C14121.5 (8)Ba1—O4—H41C127.1
C12—N13—C13120.6 (8)Ba1—O4—H42D115.2
C14—N13—C13117.9 (8)H41C—O4—H42D112.5
O14—C14—N13119.6 (10)Ba1—O5—H51C118.7
O14—C14—C15124.6 (10)Ba1—O5—H51D107.0
N13—C14—C15115.7 (9)H51C—O5—H51D107.9
N15—C15—C16127.0 (10)H61C—O6—H62D117.2
N15—C15—C14114.5 (9)
C16—N11—C12—N12180.0 (9)C26—N21—C22—N234.7 (14)
C16—N11—C12—N131.1 (15)N21—C22—N22—C2211.7 (14)
N11—C12—N12—C1210.4 (16)N23—C22—N22—C221179.1 (8)
N13—C12—N12—C121178.6 (10)C22—N22—C221—C22284.1 (11)
C12—N12—C121—C122170.1 (10)N22—C221—C222—O22220.0 (13)
N12—C121—C122—O1210.7 (14)N22—C221—C222—O221162.5 (9)
N12—C121—C122—O122179.7 (9)O222—C222—O221—Ba1150.4 (9)
O122—C122—O121—Ba156.6 (17)C221—C222—O221—Ba126.9 (15)
C121—C122—O121—Ba1123.8 (9)O121—Ba1—O221—C222100.1 (11)
O1—Ba1—O121—C122176.3 (11)O1—Ba1—O221—C22214.3 (11)
O2—Ba1—O121—C12228.6 (11)O2—Ba1—O221—C222135.6 (11)
O221—Ba1—O121—C12295.1 (11)O5—Ba1—O221—C22280.3 (11)
O5—Ba1—O121—C122114.1 (11)O4—Ba1—O221—C222158.4 (11)
O4—Ba1—O121—C12234.4 (10)O25i—Ba1—O221—C22256.6 (11)
O25i—Ba1—O121—C122115.9 (10)O3—Ba1—O221—C22245.6 (12)
O3—Ba1—O121—C122107.7 (11)N25i—Ba1—O221—C22280.5 (11)
N25i—Ba1—O121—C12284.3 (11)N21—C22—N23—C240.6 (14)
N12—C12—N13—C14177.4 (10)N22—C22—N23—C24178.6 (9)
N11—C12—N13—C143.7 (16)N21—C22—N23—C23175.2 (9)
N12—C12—N13—C131.4 (15)N22—C22—N23—C235.7 (13)
N11—C12—N13—C13177.4 (10)C22—N23—C24—O24177.3 (9)
C12—N13—C14—O14177.2 (11)C23—N23—C24—O241.4 (14)
C13—N13—C14—O141.7 (17)C22—N23—C24—C254.0 (13)
C12—N13—C14—C153.4 (15)C23—N23—C24—C25179.8 (9)
C13—N13—C14—C15177.7 (10)O24—C24—C25—N252.9 (15)
O14—C14—C15—N151.7 (17)N23—C24—C25—N25175.8 (9)
N13—C14—C15—N15178.8 (9)O24—C24—C25—C26176.9 (9)
O14—C14—C15—C16179.7 (11)N23—C24—C25—C264.4 (13)
N13—C14—C15—C160.9 (15)C24—C25—N25—O25179.4 (9)
C16—C15—N15—O153.9 (17)C26—C25—N25—O250.7 (16)
C14—C15—N15—O15178.3 (10)C25—N25—O25—Ba1ii177.6 (8)
C12—N11—C16—N16179.2 (10)C22—N21—C26—N26176.1 (9)
C12—N11—C16—C151.5 (15)C22—N21—C26—C254.1 (14)
N15—C15—C16—N163.1 (17)N25—C25—C26—N260.5 (16)
C14—C15—C16—N16179.2 (10)C24—C25—C26—N26179.4 (9)
N15—C15—C16—N11176.1 (10)N25—C25—C26—N21179.7 (10)
C14—C15—C16—N111.6 (15)C24—C25—C26—N210.4 (14)
C26—N21—C22—N22174.4 (9)
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x+1, y1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N16—H16A···O14iii0.881.982.827 (13)161
N16—H16B···O150.881.972.608 (13)129
N22—H22···O3iv0.882.042.862 (10)156
N26—H26A···O24v0.882.182.837 (12)131
N26—H26B···O250.881.942.607 (12)131
O1—H11C···O222vi0.881.862.721 (12)165
O1—H12D···O122iv0.961.822.722 (12)156
O2—H21C···O24i0.932.113.030 (11)168
O2—H21C···N25i0.932.362.918 (11)118
O2—H22D···O222v0.901.942.731 (11)145
O3—H31C···O221vi0.921.882.796 (11)174
O3—H32D···O4vi1.002.243.024 (12)135
O4—H41C···O15vii0.921.762.667 (11)165
O4—H42D···O222v0.912.092.996 (12)171
O5—H51C···O61.011.862.824 (14158
O5—H51D···O122iv0.911.902.795 (12)170
O6—H61C···N15viii0.992.203.174 (12)172
O6—H62D···O1ix1.011.972.941 (13)160
Symmetry codes: (i) x+1, y+1/2, z+1/2; (iii) x, y+1/2, z+1/2; (iv) x, y+1/2, z1/2; (v) x, y1/2, z+1/2; (vi) x, y+1, z; (vii) x, y, z+1; (viii) x, y1/2, z+1/2; (ix) x, y1, z.
(III) # Ca(py-threo)2·6(H2O top
Crystal data top
C18H28CaN10O12·4(H2O)F(000) = 724
Mr = 688.65Dx = 1.609 Mg m3
Monoclinic, C2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2yCell parameters from 3182 reflections
a = 30.2259 (11) Åθ = 3.0–27.4°
b = 6.4043 (2) ŵ = 0.32 mm1
c = 7.3667 (3) ÅT = 120 K
β = 94.610 (2)°Plate, pink
V = 1421.40 (9) Å30.24 × 0.24 × 0.04 mm
Z = 2
Data collection top
Kappa-CCD
diffractometer
3182 independent reflections
Radiation source: fine-focus sealed X-ray tube2469 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.073
ϕ scans, and ω scans with κ offsetsθmax = 27.4°, θmin = 3.0°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 3838
Tmin = 0.867, Tmax = 0.990k = 88
9010 measured reflectionsl = 99
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.049H-atom parameters constrained
wR(F2) = 0.096 w = 1/[σ2(Fo2) + (0.0339P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max < 0.001
3182 reflectionsΔρmax = 0.30 e Å3
206 parametersΔρmin = 0.33 e Å3
1 restraintAbsolute structure: Flack (1983), 1412 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.08 (5)
Crystal data top
C18H28CaN10O12·4(H2O)V = 1421.40 (9) Å3
Mr = 688.65Z = 2
Monoclinic, C2Mo Kα radiation
a = 30.2259 (11) ŵ = 0.32 mm1
b = 6.4043 (2) ÅT = 120 K
c = 7.3667 (3) Å0.24 × 0.24 × 0.04 mm
β = 94.610 (2)°
Data collection top
Kappa-CCD
diffractometer
3182 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
2469 reflections with I > 2σ(I)
Tmin = 0.867, Tmax = 0.990Rint = 0.073
9010 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.049H-atom parameters constrained
wR(F2) = 0.096Δρmax = 0.30 e Å3
S = 1.03Δρmin = 0.33 e Å3
3182 reflectionsAbsolute structure: Flack (1983), 1412 Friedel pairs
206 parametersAbsolute structure parameter: 0.08 (5)
1 restraint
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca11.00000.23325 (12)0.50000.0152 (2)
N10.80400 (7)0.7798 (4)0.2875 (3)0.0150 (5)
C20.83047 (8)0.7773 (5)0.1529 (3)0.0139 (6)
N20.87444 (7)0.7755 (4)0.1953 (3)0.0156 (5)
C210.89310 (8)0.7782 (5)0.3845 (4)0.0141 (6)
C220.90594 (9)0.5593 (4)0.4570 (4)0.0159 (6)
O210.94321 (6)0.4799 (3)0.3682 (3)0.0173 (5)
C230.86750 (9)0.4052 (5)0.4443 (4)0.0198 (7)
C240.93285 (9)0.9259 (4)0.4113 (4)0.0157 (7)
O220.94650 (7)0.9676 (3)0.5730 (3)0.0206 (5)
O230.95003 (6)1.0024 (3)0.2762 (3)0.0194 (5)
N30.81585 (7)0.7775 (4)0.0295 (3)0.0145 (5)
C30.84744 (9)0.7775 (5)0.1707 (4)0.0184 (6)
C40.77063 (8)0.7760 (5)0.0850 (3)0.0143 (6)
O40.75843 (6)0.7758 (4)0.2471 (2)0.0231 (5)
C50.74062 (8)0.7752 (5)0.0603 (3)0.0137 (6)
N50.69742 (7)0.7761 (4)0.0010 (3)0.0172 (5)
O50.66907 (6)0.7746 (3)0.1243 (2)0.0206 (5)
C60.75991 (8)0.7761 (5)0.2456 (3)0.0148 (6)
N60.73384 (7)0.7724 (4)0.3809 (3)0.0196 (6)
O11.02434 (6)0.3724 (3)0.2231 (3)0.0191 (5)
O20.91546 (6)0.2882 (3)0.0294 (2)0.0195 (5)
O31.04686 (7)0.7819 (4)0.0791 (3)0.0379 (6)
H20.89250.77260.10730.019*
H210.86960.83300.46000.017*
H220.91590.57510.58910.019*
H21A0.93580.44370.26390.021*
H23A0.85870.37480.31610.030*
H23B0.84230.46580.50140.030*
H23C0.87670.27570.50740.030*
H3A0.83120.76850.29100.028*
H3B0.86740.65740.15280.028*
H3C0.86480.90680.16250.028*
H6A0.74550.77250.49440.024*
H6B0.70480.76990.35780.024*
H111.04580.31510.14500.023*
H121.01480.50680.17410.023*
H21B0.88880.28540.01150.023*
H22B0.92250.18370.09480.023*
H311.03630.87000.02230.045*
H321.04890.85590.19430.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0140 (4)0.0166 (5)0.0152 (4)0.0000.0013 (3)0.000
N10.0117 (11)0.0199 (14)0.0133 (11)0.0006 (11)0.0000 (9)0.0046 (12)
C20.0159 (14)0.0113 (15)0.0140 (13)0.0020 (12)0.0010 (10)0.0010 (13)
N20.0136 (12)0.0190 (14)0.0143 (11)0.0008 (11)0.0024 (9)0.0020 (12)
C210.0140 (14)0.0154 (16)0.0128 (13)0.0016 (13)0.0013 (10)0.0001 (13)
C220.0174 (16)0.0140 (15)0.0169 (16)0.0017 (12)0.0044 (13)0.0006 (12)
O210.0158 (11)0.0194 (11)0.0171 (11)0.0037 (9)0.0025 (9)0.0028 (10)
C230.0200 (17)0.0165 (16)0.0231 (18)0.0007 (13)0.0036 (13)0.0005 (13)
C240.0148 (16)0.0104 (15)0.0220 (17)0.0017 (11)0.0018 (13)0.0006 (13)
O220.0226 (11)0.0184 (11)0.0201 (12)0.0046 (9)0.0025 (9)0.0029 (10)
O230.0163 (11)0.0207 (12)0.0212 (12)0.0004 (9)0.0021 (9)0.0023 (10)
N30.0155 (12)0.0156 (13)0.0125 (11)0.0005 (11)0.0017 (9)0.0009 (11)
C30.0215 (15)0.0228 (17)0.0118 (13)0.0013 (14)0.0071 (11)0.0012 (14)
C40.0157 (14)0.0123 (15)0.0146 (14)0.0024 (12)0.0004 (11)0.0025 (13)
O40.0212 (10)0.0346 (14)0.0128 (10)0.0007 (11)0.0028 (8)0.0002 (11)
C50.0141 (14)0.0125 (15)0.0144 (13)0.0009 (12)0.0002 (10)0.0023 (13)
N50.0152 (12)0.0162 (14)0.0202 (12)0.0011 (11)0.0008 (10)0.0007 (12)
O50.0169 (10)0.0260 (12)0.0186 (10)0.0011 (10)0.0006 (8)0.0005 (10)
C60.0186 (15)0.0124 (15)0.0133 (14)0.0002 (13)0.0011 (11)0.0008 (13)
N60.0140 (12)0.0310 (15)0.0137 (11)0.0031 (13)0.0003 (9)0.0008 (13)
O10.0200 (11)0.0206 (12)0.0175 (11)0.0014 (9)0.0074 (9)0.0011 (9)
O20.0163 (10)0.0241 (12)0.0177 (10)0.0015 (9)0.0004 (8)0.0022 (10)
O30.0519 (15)0.0357 (16)0.0262 (12)0.0136 (12)0.0042 (10)0.0055 (12)
Geometric parameters (Å, º) top
Ca1—O12.395 (2)C24—O221.258 (3)
Ca1—O22i2.437 (2)C24—O231.259 (3)
Ca1—O212.473 (2)N3—C41.395 (3)
Ca1—O23i2.605 (2)N3—C31.467 (3)
Ca1—C24i2.865 (3)C3—H3A0.98
N1—C21.323 (3)C3—H3B0.98
N1—C61.344 (3)C3—H3C0.98
C2—N21.341 (3)C4—O41.221 (3)
C2—N31.380 (3)C4—C51.458 (4)
N2—C211.461 (3)C5—N51.343 (3)
N2—H20.88C5—C61.440 (3)
C21—C241.529 (4)N5—O51.298 (3)
C21—C221.539 (4)C6—N61.320 (3)
C21—H211.00N6—H6A0.88
C22—O211.440 (3)N6—H6B0.88
C22—C231.522 (4)O1—H110.97
C22—H221.00O1—H120.97
O21—H21A0.8173O2—H21B0.84
C23—H23A0.98O2—H22B0.84
C23—H23B0.98O3—H310.97
C23—H23C0.98O3—H320.97
O1ii—Ca1—O1136.32 (10)C21—C22—H22107.0
O1—Ca1—O22i134.61 (7)C22—O21—Ca1126.22 (17)
O1—Ca1—O22iii79.46 (7)C22—O21—H21A111.2
O22i—Ca1—O22iii91.44 (10)Ca1—O21—H21A108.5
O1—Ca1—O21ii81.12 (7)C22—C23—H23A109.5
O1ii—Ca1—O2181.12 (7)C22—C23—H23B109.5
O1—Ca1—O2171.29 (7)H23A—C23—H23B109.5
O22i—Ca1—O2194.63 (7)C22—C23—H23C109.5
O22iii—Ca1—O21144.22 (7)H23A—C23—H23C109.5
O21ii—Ca1—O21100.60 (10)H23B—C23—H23C109.5
O1ii—Ca1—O23i123.23 (6)O22—C24—O23122.8 (3)
O1—Ca1—O23i82.77 (7)O22—C24—C21116.6 (3)
O22i—Ca1—O23i51.84 (6)O23—C24—C21120.6 (3)
O22iii—Ca1—O23i79.94 (7)C2—N3—C4121.0 (2)
O21ii—Ca1—O23i163.70 (6)C2—N3—C3120.9 (2)
O21—Ca1—O23i76.42 (6)C4—N3—C3118.1 (2)
O1ii—Ca1—O23iii82.77 (7)N3—C3—H3A109.5
O1—Ca1—O23iii123.23 (6)N3—C3—H3B109.5
O22i—Ca1—O23iii79.94 (7)H3A—C3—H3B109.5
O22iii—Ca1—O23iii51.84 (6)N3—C3—H3C109.5
O21ii—Ca1—O23iii76.42 (6)H3A—C3—H3C109.5
O21—Ca1—O23iii163.70 (6)H3B—C3—H3C109.5
O23i—Ca1—O23iii110.85 (9)O4—C4—N3119.9 (2)
C2—N1—C6118.4 (2)O4—C4—C5124.2 (2)
N1—C2—N2118.3 (2)N3—C4—C5116.0 (2)
N1—C2—N3124.3 (2)N5—C5—C6128.1 (2)
N2—C2—N3117.4 (2)N5—C5—C4114.0 (2)
C2—N2—C21121.4 (2)C6—C5—C4117.9 (2)
C2—N2—H2119.3O5—N5—C5116.8 (2)
C21—N2—H2119.3N6—C6—N1117.9 (2)
N2—C21—C24111.7 (2)N6—C6—C5119.7 (2)
N2—C21—C22112.8 (2)N1—C6—C5122.4 (2)
C24—C21—C22110.2 (2)C6—N6—H6A120.0
N2—C21—H21107.3C6—N6—H6B120.0
C24—C21—H21107.3H6A—N6—H6B120.0
C22—C21—H21107.3Ca1—O1—H11128.9
O21—C22—C23111.4 (2)Ca1—O1—H12123.1
O21—C22—C21110.4 (2)H11—O1—H12107.9
C23—C22—C21113.6 (2)H21B—O2—H22B112.3
O21—C22—H22107.0H31—O3—H32112.5
C23—C22—H22107.0
C6—N1—C2—N2178.3 (3)O23—C24—O22—Ca1iv6.1 (3)
C6—N1—C2—N32.1 (4)C21—C24—O22—Ca1iv172.8 (2)
N1—C2—N2—C210.6 (4)O22—C24—O23—Ca1iv5.7 (3)
N3—C2—N2—C21179.1 (2)C21—C24—O23—Ca1iv173.2 (2)
C2—N2—C21—C24137.7 (3)N1—C2—N3—C41.4 (4)
C2—N2—C21—C2297.6 (3)N2—C2—N3—C4179.0 (2)
N2—C21—C22—O2168.5 (3)N1—C2—N3—C3179.1 (3)
C24—C21—C22—O2157.0 (3)N2—C2—N3—C30.5 (4)
N2—C21—C22—C2357.4 (3)C2—N3—C4—O4179.8 (3)
C24—C21—C22—C23177.0 (2)C3—N3—C4—O40.4 (4)
C23—C22—O21—Ca182.1 (3)C2—N3—C4—C50.3 (4)
C21—C22—O21—Ca1150.76 (17)C3—N3—C4—C5179.8 (3)
O1ii—Ca1—O21—C2223.3 (2)O4—C4—C5—N50.6 (4)
O1—Ca1—O21—C22169.0 (2)N3—C4—C5—N5179.3 (2)
O22i—Ca1—O21—C2255.2 (2)O4—C4—C5—C6179.9 (3)
O22iii—Ca1—O21—C22154.15 (19)N3—C4—C5—C60.0 (4)
O21ii—Ca1—O21—C2292.3 (2)C6—C5—N5—O51.1 (4)
O23i—Ca1—O21—C22104.1 (2)C4—C5—N5—O5179.7 (2)
O23iii—Ca1—O21—C2214.5 (4)C2—N1—C6—N6178.0 (3)
C24i—Ca1—O21—C2278.8 (2)C2—N1—C6—C51.7 (4)
N2—C21—C24—O22168.0 (2)N5—C5—C6—N61.8 (5)
C22—C21—C24—O2265.8 (3)C4—C5—C6—N6179.0 (3)
N2—C21—C24—O2310.9 (4)N5—C5—C6—N1178.4 (3)
C22—C21—C24—O23115.3 (3)C4—C5—C6—N10.7 (4)
Symmetry codes: (i) x, y1, z; (ii) x+2, y, z+1; (iii) x+2, y1, z+1; (iv) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3v0.882.373.243 (3)168
O21—H21A···O20.822.042.846 (3)167
N6—H6A···O4vi0.881.912.781 (3)168
N6—H6B···O50.881.952.609 (3)130
O1—H11···O2v0.971.822.758 (3)162
O1—H12···O30.972.162.931 (3)136
O2—H21B···N5vii0.842.613.402 (3)157
O2—H21B···O5vii0.841.882.711 (3)175
O2—H22B···O23i0.841.912.727 (3)164
O3—H31···O23v0.972.122.982 (3)147
O3—H32···O22ii0.971.852.818 (3)174
Symmetry codes: (i) x, y1, z; (ii) x+2, y, z+1; (v) x+2, y, z; (vi) x, y, z+1; (vii) x+3/2, y1/2, z.
(IV) # Sr(py-threo)2·6(H2O) top
Crystal data top
C18H28N10O12Sr·4(H2O)F(000) = 760
Mr = 736.19Dx = 1.673 Mg m3
Monoclinic, C2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2yCell parameters from 3314 reflections
a = 30.6420 (5) Åθ = 3.0–27.5°
b = 6.4888 (1) ŵ = 1.94 mm1
c = 7.3733 (1) ÅT = 120 K
β = 94.4319 (9)°Block, red
V = 1461.65 (4) Å30.70 × 0.50 × 0.25 mm
Z = 2
Data collection top
Kappa-CCD
diffractometer
3314 independent reflections
Radiation source: fine-focus sealed X-ray tube3291 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.062
ϕ scans, and ω scans with κ offsetsθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 3939
Tmin = 0.331, Tmax = 0.618k = 88
9899 measured reflectionsl = 99
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.028 w = 1/[σ2(Fo2) + (0.030P)2 + 1.5757P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.069(Δ/σ)max < 0.001
S = 1.04Δρmax = 0.33 e Å3
3314 reflectionsΔρmin = 0.46 e Å3
209 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.0164 (8)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), 1486 Friedel pairs
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.017 (4)
Crystal data top
C18H28N10O12Sr·4(H2O)V = 1461.65 (4) Å3
Mr = 736.19Z = 2
Monoclinic, C2Mo Kα radiation
a = 30.6420 (5) ŵ = 1.94 mm1
b = 6.4888 (1) ÅT = 120 K
c = 7.3733 (1) Å0.70 × 0.50 × 0.25 mm
β = 94.4319 (9)°
Data collection top
Kappa-CCD
diffractometer
3314 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
3291 reflections with I > 2σ(I)
Tmin = 0.331, Tmax = 0.618Rint = 0.062
9899 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.028H-atom parameters constrained
wR(F2) = 0.069Δρmax = 0.33 e Å3
S = 1.04Δρmin = 0.46 e Å3
3314 reflectionsAbsolute structure: Flack (1983), 1486 Friedel pairs
209 parametersAbsolute structure parameter: 0.017 (4)
1 restraint
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr11.00000.23593 (4)0.50000.01060 (9)
N10.80277 (6)0.7783 (3)0.2882 (2)0.0122 (5)
C20.82900 (8)0.7767 (3)0.1539 (3)0.0106 (5)
N20.87241 (6)0.7763 (3)0.1953 (2)0.0112 (5)
C210.89087 (7)0.7765 (3)0.3847 (3)0.0094 (5)
C220.90356 (7)0.5601 (4)0.4523 (3)0.0105 (4)
O210.93974 (6)0.4847 (3)0.3579 (2)0.0133 (4)
C230.86599 (8)0.4069 (4)0.4423 (3)0.0165 (5)
C240.93010 (8)0.9208 (4)0.4128 (3)0.0108 (5)
O220.94370 (6)0.9566 (3)0.5748 (2)0.0164 (4)
O230.94686 (6)0.9987 (3)0.2770 (2)0.0141 (4)
N30.81494 (6)0.7757 (3)0.0284 (2)0.0111 (5)
C30.84617 (8)0.7747 (4)0.1695 (3)0.0168 (6)
C40.77006 (8)0.7744 (3)0.0844 (3)0.0112 (5)
O40.75828 (6)0.7731 (3)0.2462 (2)0.0200 (5)
C50.74059 (7)0.7729 (3)0.0610 (3)0.0107 (5)
N50.69792 (6)0.7731 (3)0.0035 (3)0.0136 (5)
O50.66992 (5)0.7715 (3)0.1253 (2)0.0176 (5)
C60.75930 (8)0.7738 (3)0.2478 (3)0.0122 (5)
N60.73364 (6)0.7691 (4)0.3816 (2)0.0171 (6)
O11.02665 (6)0.3831 (3)0.2097 (2)0.0178 (4)
O20.91260 (5)0.2817 (2)0.0317 (2)0.0158 (4)
O31.04916 (7)0.7812 (3)0.0727 (3)0.0319 (6)
H20.89020.77600.10700.013*
H210.86770.82880.46140.011*
H220.91420.57340.58350.013*
H21A0.93230.44850.25350.016*
H23A0.85620.38130.31470.025*
H23B0.84170.46330.50580.025*
H23C0.87590.27730.50010.025*
H3A0.83020.77090.28980.025*
H3B0.86500.65300.15420.025*
H3C0.86420.89950.15880.025*
H6A0.74500.76890.49490.021*
H6B0.70510.76600.35820.021*
H111.04810.32580.13160.021*
H121.01710.51740.16080.021*
H21B0.88590.27880.00930.019*
H22B0.91960.17710.09700.019*
H311.03250.84520.00590.045 (11)*
H321.05240.84590.17310.063 (14)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.00890 (13)0.01194 (14)0.01074 (13)0.0000.00062 (9)0.000
N10.0091 (9)0.0187 (14)0.0084 (8)0.0005 (7)0.0023 (7)0.0009 (7)
C20.0116 (10)0.0088 (14)0.0112 (9)0.0003 (7)0.0013 (8)0.0008 (7)
N20.0091 (8)0.0155 (13)0.0090 (8)0.0004 (7)0.0002 (7)0.0005 (7)
C210.0069 (9)0.0116 (14)0.0094 (9)0.0000 (7)0.0007 (8)0.0011 (7)
C220.0059 (10)0.0140 (11)0.0114 (10)0.0004 (9)0.0002 (9)0.0022 (8)
O210.0127 (9)0.0143 (9)0.0126 (8)0.0011 (7)0.0011 (7)0.0034 (7)
C230.0162 (12)0.0118 (11)0.0218 (12)0.0016 (9)0.0032 (10)0.0003 (9)
C240.0118 (12)0.0089 (11)0.0110 (11)0.0001 (9)0.0029 (9)0.0000 (9)
O220.0176 (9)0.0201 (9)0.0111 (7)0.0039 (7)0.0015 (7)0.0000 (7)
O230.0134 (8)0.0150 (9)0.0138 (8)0.0022 (7)0.0001 (7)0.0028 (7)
N30.0102 (9)0.0162 (13)0.0069 (8)0.0005 (7)0.0005 (7)0.0001 (7)
C30.0149 (11)0.0246 (18)0.0111 (9)0.0004 (9)0.0025 (8)0.0006 (9)
C40.0133 (10)0.0104 (15)0.0096 (9)0.0011 (8)0.0016 (8)0.0007 (7)
O40.0177 (8)0.0332 (15)0.0084 (7)0.0013 (7)0.0035 (6)0.0001 (7)
C50.0115 (10)0.0105 (14)0.0095 (9)0.0005 (8)0.0023 (8)0.0004 (7)
N50.0119 (9)0.0154 (13)0.0131 (8)0.0002 (7)0.0015 (7)0.0004 (7)
O50.0089 (7)0.0263 (13)0.0177 (7)0.0003 (7)0.0006 (6)0.0006 (7)
C60.0126 (10)0.0130 (15)0.0104 (9)0.0005 (8)0.0033 (8)0.0015 (8)
N60.0094 (8)0.0327 (17)0.0088 (8)0.0010 (9)0.0016 (7)0.0019 (8)
O10.0192 (9)0.0189 (9)0.0159 (8)0.0015 (7)0.0045 (7)0.0010 (7)
O20.0118 (8)0.0207 (12)0.0143 (7)0.0002 (6)0.0021 (6)0.0031 (6)
O30.0473 (13)0.0284 (14)0.0196 (9)0.0112 (9)0.0007 (9)0.0023 (8)
Geometric parameters (Å, º) top
Sr1—O12.535 (2)C24—O231.265 (3)
Sr1—O22i2.591 (2)N3—C41.405 (3)
Sr1—O212.611 (2)N3—C31.467 (3)
Sr1—O23i2.704 (2)C3—H3A0.98
N1—C21.323 (3)C3—H3B0.98
N1—C61.343 (3)C3—H3C0.98
C2—N21.342 (3)C4—O41.220 (3)
C2—N31.379 (3)C4—C51.454 (3)
N2—C211.466 (3)C5—N51.343 (3)
N2—H20.88C5—C61.451 (3)
C21—C241.525 (3)N5—O51.289 (3)
C21—C221.530 (3)C6—N61.308 (3)
C21—H211.00N6—H6A0.88
C22—O211.440 (3)N6—H6B0.88
C22—C231.519 (3)O1—H110.9796
C22—H221.00O1—H120.9795
O21—H21A0.8201O2—H21B0.85
C23—H23A0.98O2—H22B0.8499
C23—H23B0.98O3—H310.8502
C23—H23C0.98O3—H320.8505
C24—O221.256 (3)
O1ii—Sr1—O1135.76 (8)C21—C22—H22107.0
O1—Sr1—O22i134.94 (6)C22—O21—Sr1124.28 (13)
O1—Sr1—O22iii79.66 (6)C22—O21—H21A112.5
O22i—Sr1—O22iii91.21 (8)Sr1—O21—H21A109.6
O1ii—Sr1—O2180.91 (6)C22—C23—H23A109.5
O1—Sr1—O2172.07 (6)C22—C23—H23B109.5
O22i—Sr1—O2193.22 (6)H23A—C23—H23B109.5
O22iii—Sr1—O21144.01 (5)C22—C23—H23C109.5
O21ii—Sr1—O21103.59 (8)H23A—C23—H23C109.5
O1ii—Sr1—O23i120.63 (6)H23B—C23—H23C109.5
O1—Sr1—O23i85.37 (5)O22—C24—O23123.6 (2)
O22i—Sr1—O23i49.57 (5)O22—C24—C21116.3 (2)
O22iii—Sr1—O23i81.48 (5)O23—C24—C21120.1 (2)
O21ii—Sr1—O23i165.99 (5)C2—N3—C4120.7 (2)
O21—Sr1—O23i74.57 (5)C2—N3—C3121.28 (19)
O1ii—Sr1—O23iii85.37 (5)C4—N3—C3117.98 (18)
O1—Sr1—O23iii120.63 (6)N3—C3—H3A109.5
O22i—Sr1—O23iii81.48 (5)N3—C3—H3B109.5
O22iii—Sr1—O23iii49.57 (5)H3A—C3—H3B109.5
O21ii—Sr1—O23iii74.57 (5)N3—C3—H3C109.5
O21—Sr1—O23iii165.99 (5)H3A—C3—H3C109.5
O23i—Sr1—O23iii110.60 (7)H3B—C3—H3C109.5
C2—N1—C6118.94 (19)O4—C4—N3119.8 (2)
N1—C2—N2118.60 (19)O4—C4—C5124.6 (2)
N1—C2—N3124.6 (2)N3—C4—C5115.67 (18)
N2—C2—N3116.8 (2)N5—C5—C6127.1 (2)
C2—N2—C21121.33 (19)N5—C5—C4114.36 (19)
C2—N2—H2119.3C6—C5—C4118.5 (2)
C21—N2—H2119.3O5—N5—C5117.65 (18)
N2—C21—C24111.85 (18)N6—C6—N1118.5 (2)
N2—C21—C22112.31 (17)N6—C6—C5120.0 (2)
C24—C21—C22109.96 (18)N1—C6—C5121.5 (2)
N2—C21—H21107.5C6—N6—H6A120.0
C24—C21—H21107.5C6—N6—H6B120.0
C22—C21—H21107.5H6A—N6—H6B120.0
O21—C22—C23111.31 (19)Sr1—O1—H11128.9
O21—C22—C21109.87 (18)Sr1—O1—H12122.7
C23—C22—C21114.35 (19)H11—O1—H12108.4
O21—C22—H22107.0H21B—O2—H22B112.2
C23—C22—H22107.0H31—O3—H32112.1
C6—N1—C2—N2178.44 (18)O23—C24—O22—Sr1iv6.3 (3)
C6—N1—C2—N31.7 (3)C21—C24—O22—Sr1iv173.04 (17)
N1—C2—N2—C210.4 (3)O22—C24—O23—Sr1iv6.0 (3)
N3—C2—N2—C21179.76 (17)C21—C24—O23—Sr1iv173.31 (19)
C2—N2—C21—C24138.5 (2)N1—C2—N3—C40.6 (3)
C2—N2—C21—C2297.3 (2)N2—C2—N3—C4179.49 (17)
N2—C21—C22—O2167.4 (2)N1—C2—N3—C3179.8 (2)
C24—C21—C22—O2157.9 (2)N2—C2—N3—C30.1 (3)
N2—C21—C22—C2358.6 (3)C2—N3—C4—O4179.8 (2)
C24—C21—C22—C23176.12 (19)C3—N3—C4—O40.2 (3)
C23—C22—O21—Sr184.0 (2)C2—N3—C4—C50.3 (3)
C21—C22—O21—Sr1148.26 (13)C3—N3—C4—C5179.27 (18)
O1ii—Sr1—O21—C2221.81 (16)O4—C4—C5—N51.0 (3)
O1—Sr1—O21—C22166.33 (17)N3—C4—C5—N5179.56 (18)
O22i—Sr1—O21—C2257.17 (16)O4—C4—C5—C6179.7 (2)
O22iii—Sr1—O21—C22153.69 (15)N3—C4—C5—C60.3 (3)
O21ii—Sr1—O21—C2290.75 (16)C6—C5—N5—O50.9 (3)
O23i—Sr1—O21—C22103.59 (17)C4—C5—N5—O5179.91 (19)
O23iii—Sr1—O21—C2210.1 (4)C2—N1—C6—N6177.9 (2)
C24i—Sr1—O21—C2279.27 (17)C2—N1—C6—C51.7 (3)
C24iii—Sr1—O21—C22149.7 (3)N5—C5—C6—N61.9 (3)
N2—C21—C24—O22169.0 (2)C4—C5—C6—N6178.9 (2)
C22—C21—C24—O2265.5 (3)N5—C5—C6—N1178.4 (2)
N2—C21—C24—O2310.4 (3)C4—C5—C6—N10.8 (3)
C22—C21—C24—O23115.1 (2)
Symmetry codes: (i) x, y1, z; (ii) x+2, y, z+1; (iii) x+2, y1, z+1; (iv) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3v0.882.363.224 (3)166
O21—H21A···O20.822.012.812 (2)164
N6—H6A···O4vi0.881.922.790 (2)169
N6—H6B···O50.881.952.610 (2)130
O1—H11···O2v0.981.792.753 (2)167
O1—H12···O30.982.102.877 (3)135
O2—H21B···N5vii0.852.573.377 (3)158
O2—H21B···O5vii0.851.852.699 (2)173
O2—H22B···O23i0.851.902.730 (2)163
O3—H31···O23v0.852.362.950 (4)127
O3—H31···O3v0.852.553.119 (4)126
O3—H32···O22ii0.851.992.831 (2)171
Symmetry codes: (i) x, y1, z; (ii) x+2, y, z+1; (v) x+2, y, z; (vi) x, y, z+1; (vii) x+3/2, y1/2, z.
(V) # Ba(py-serin)2·7H2O top
Crystal data top
C16H28BaN10O14·3(H2O)Z = 1
Mr = 775.45F(000) = 392
Triclinic, P1Dx = 1.834 Mg m3
Hall symbol: P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.1387 (2) ÅCell parameters from 5818 reflections
b = 7.4974 (2) Åθ = 2.9–27.4°
c = 13.5644 (4) ŵ = 1.51 mm1
α = 99.5040 (9)°T = 120 K
β = 94.308 (1)°Plate, pink
γ = 99.6000 (16)°0.40 × 0.26 × 0.02 mm
V = 702.05 (3) Å3
Data collection top
Kappa-CCD
diffractometer
5818 independent reflections
Radiation source: fine-focus sealed X-ray tube5773 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
ϕ scans, and ω scans with κ offsetsθmax = 27.4°, θmin = 2.9°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 99
Tmin = 0.625, Tmax = 0.970k = 99
10911 measured reflectionsl = 1717
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.075 w = 1/[σ2(Fo2) + (0.0297P)2 + 0.7753P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max < 0.001
5818 reflectionsΔρmax = 0.44 e Å3
397 parametersΔρmin = 0.93 e Å3
3 restraintsAbsolute structure: Flack (1983), 2609 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.006 (12)
Crystal data top
C16H28BaN10O14·3(H2O)γ = 99.6000 (16)°
Mr = 775.45V = 702.05 (3) Å3
Triclinic, P1Z = 1
a = 7.1387 (2) ÅMo Kα radiation
b = 7.4974 (2) ŵ = 1.51 mm1
c = 13.5644 (4) ÅT = 120 K
α = 99.5040 (9)°0.40 × 0.26 × 0.02 mm
β = 94.308 (1)°
Data collection top
Kappa-CCD
diffractometer
5818 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
5773 reflections with I > 2σ(I)
Tmin = 0.625, Tmax = 0.970Rint = 0.038
10911 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.075Δρmax = 0.44 e Å3
S = 1.01Δρmin = 0.93 e Å3
5818 reflectionsAbsolute structure: Flack (1983), 2609 Friedel pairs
397 parametersAbsolute structure parameter: 0.006 (12)
3 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ba10.931361 (8)0.378877 (8)0.479290 (8)0.01160 (7)
N110.2435 (10)0.1423 (8)0.0327 (5)0.0126 (13)
C120.2782 (6)0.0188 (6)0.0884 (3)0.0120 (9)
N120.3547 (9)0.0775 (8)0.1820 (4)0.0150 (11)
C1210.4022 (6)0.2722 (5)0.2289 (3)0.0091 (8)
C1220.5516 (6)0.2922 (6)0.3193 (3)0.0126 (9)
O110.5577 (4)0.4182 (4)0.3930 (2)0.0169 (7)
O120.6721 (4)0.1847 (4)0.3101 (3)0.0165 (7)
C1230.2255 (6)0.3480 (6)0.2557 (3)0.0110 (9)
O130.1169 (4)0.2415 (4)0.3176 (2)0.0143 (6)
N130.2437 (5)0.1694 (5)0.0548 (3)0.0113 (7)
C130.3026 (7)0.2946 (6)0.1198 (4)0.0169 (10)
C140.1633 (6)0.2453 (6)0.0421 (4)0.0133 (9)
O140.1416 (7)0.4112 (6)0.0727 (3)0.0234 (11)
C150.1080 (6)0.1147 (6)0.1021 (3)0.0116 (9)
N150.0158 (9)0.1957 (7)0.1925 (4)0.0160 (12)
O150.0422 (5)0.0901 (4)0.2499 (3)0.0207 (8)
C160.1564 (6)0.0798 (6)0.0609 (3)0.0104 (8)
N160.1130 (9)0.2000 (8)0.1155 (5)0.0129 (13)
N210.5817 (5)0.2463 (5)0.8511 (3)0.0116 (7)
C220.5248 (6)0.3650 (6)0.7981 (3)0.0102 (9)
N220.4342 (5)0.3016 (5)0.7067 (3)0.0134 (8)
C2210.3983 (6)0.1084 (5)0.6595 (3)0.0096 (8)
C2220.5586 (6)0.0617 (6)0.5963 (3)0.0100 (9)
O210.7001 (5)0.1833 (4)0.5944 (3)0.0187 (7)
O220.5353 (5)0.1017 (4)0.5480 (3)0.0143 (7)
C2230.2053 (6)0.0612 (6)0.5947 (3)0.0106 (8)
O230.2097 (5)0.1653 (4)0.5151 (2)0.0151 (7)
N230.5502 (5)0.5520 (5)0.8330 (3)0.0114 (7)
C230.4901 (11)0.6754 (9)0.7669 (5)0.0114 (7)
C240.6293 (11)0.6301 (10)0.9309 (6)0.0106 (14)
O240.6416 (5)0.7948 (4)0.9622 (3)0.0190 (7)
C250.6906 (6)0.5009 (6)0.9915 (3)0.0107 (8)
N250.7696 (9)0.5807 (8)1.0840 (5)0.0146 (14)
O250.8299 (5)0.4778 (4)1.1422 (3)0.0169 (7)
C260.6643 (6)0.3095 (6)0.9457 (3)0.0108 (9)
N260.7186 (7)0.1899 (7)0.9978 (4)0.0153 (11)
O11.3087 (4)0.5563 (4)0.5245 (3)0.0188 (7)
O20.8211 (5)0.6821 (4)0.5756 (3)0.0212 (8)
O30.9626 (5)0.6377 (4)0.3414 (2)0.0156 (7)
O41.0045 (5)0.4159 (4)0.7016 (3)0.0197 (7)
O50.8102 (7)0.0617 (6)0.4054 (3)0.0222 (14)0.796 (13)
O510.678 (3)0.146 (2)0.3782 (13)0.0222 (14)0.204 (13)
O60.1330 (7)0.0041 (6)0.1710 (4)0.0228 (12)
O70.3022 (5)0.1079 (5)0.3594 (3)0.0164 (7)
H120.37850.00470.21840.018*
H1210.46230.34200.17910.011*
H12A0.26370.47670.29180.013*
H12B0.14450.34860.19330.013*
H130.04630.15490.27590.017*
H13A0.43960.25790.14180.025*
H13B0.27670.42080.08200.025*
H13C0.23070.28790.17860.025*
H16A0.14110.31840.09060.015*
H16B0.05600.16180.17700.015*
H220.39370.38080.67280.016*
H22A0.39190.03250.71360.011*
H22B0.17710.07190.56610.013*
H22C0.10300.08950.63690.013*
H230.23980.10620.46130.018*
H23A0.56530.67140.70930.017*
H23B0.51100.80150.80470.017*
H23C0.35420.63490.74290.017*
H26A0.70050.07260.97060.018*
H26B0.77310.22741.05990.018*
H1A1.35720.49380.47720.023*
H1B1.36530.66930.54070.023*
H2A0.87150.75470.63240.025*
H2B0.72280.73270.56000.025*
H3A0.93150.58190.27850.019*
H3B0.88280.71500.35150.019*
H4A0.88610.34790.68770.024*
H4B1.01710.51970.74750.024*
H5A0.75540.00070.35750.027*0.796 (13)
H5B0.72540.07360.45560.027*0.796 (13)
H6A0.23850.04970.19140.027*
H6B0.18630.10590.11960.027*
H7A0.18070.17270.36900.020*
H7B0.38280.13510.41180.020*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.01037 (11)0.01203 (10)0.01140 (11)0.00041 (7)0.00032 (7)0.00156 (7)
N110.018 (3)0.009 (3)0.009 (3)0.004 (2)0.002 (2)0.003 (2)
C120.013 (2)0.0081 (19)0.015 (2)0.0040 (16)0.0007 (18)0.0003 (17)
N120.023 (3)0.010 (2)0.010 (2)0.0021 (18)0.0035 (19)0.0005 (17)
C1210.012 (2)0.0062 (18)0.008 (2)0.0031 (15)0.0006 (16)0.0026 (16)
C1220.008 (2)0.014 (2)0.015 (2)0.0008 (16)0.0023 (17)0.0036 (18)
O110.0113 (16)0.0235 (17)0.0135 (17)0.0054 (13)0.0014 (13)0.0047 (14)
O120.0128 (16)0.0136 (15)0.0229 (19)0.0059 (12)0.0016 (14)0.0001 (13)
C1230.014 (2)0.0091 (19)0.010 (2)0.0022 (16)0.0004 (17)0.0025 (16)
O130.0147 (16)0.0160 (15)0.0107 (16)0.0007 (12)0.0007 (13)0.0005 (12)
N130.0149 (19)0.0074 (16)0.0102 (19)0.0026 (14)0.0013 (15)0.0018 (14)
C130.025 (3)0.011 (2)0.016 (2)0.0054 (18)0.000 (2)0.0031 (18)
C140.015 (2)0.011 (2)0.015 (2)0.0035 (17)0.0027 (18)0.0015 (17)
O140.039 (3)0.0077 (18)0.021 (2)0.0034 (16)0.001 (2)0.0001 (16)
C150.014 (2)0.009 (2)0.009 (2)0.0018 (16)0.0012 (17)0.0040 (16)
N150.021 (3)0.015 (2)0.010 (2)0.0015 (19)0.0010 (19)0.0008 (19)
O150.032 (2)0.0152 (16)0.0144 (18)0.0042 (14)0.0061 (15)0.0038 (13)
C160.009 (2)0.0111 (19)0.010 (2)0.0017 (16)0.0046 (17)0.0012 (16)
N160.018 (3)0.009 (2)0.012 (3)0.004 (2)0.002 (2)0.003 (2)
N210.0109 (19)0.0120 (17)0.0122 (19)0.0021 (14)0.0030 (15)0.0021 (14)
C220.008 (2)0.014 (2)0.010 (2)0.0042 (16)0.0058 (16)0.0002 (17)
N220.018 (2)0.0094 (17)0.012 (2)0.0026 (14)0.0008 (16)0.0012 (15)
C2210.012 (2)0.0085 (19)0.009 (2)0.0023 (16)0.0026 (17)0.0012 (16)
C2220.010 (2)0.010 (2)0.010 (2)0.0004 (16)0.0009 (17)0.0020 (16)
O210.0171 (17)0.0128 (15)0.0227 (19)0.0059 (13)0.0034 (14)0.0010 (13)
O220.0102 (17)0.0129 (16)0.019 (2)0.0019 (12)0.0050 (15)0.0006 (15)
C2230.008 (2)0.0097 (19)0.014 (2)0.0022 (15)0.0005 (17)0.0029 (16)
O230.0215 (18)0.0152 (15)0.0114 (16)0.0101 (13)0.0031 (13)0.0032 (12)
N230.0181 (17)0.0061 (14)0.0107 (16)0.0053 (12)0.0019 (13)0.0023 (12)
C230.0181 (17)0.0061 (14)0.0107 (16)0.0053 (12)0.0019 (13)0.0023 (12)
C240.010 (3)0.010 (3)0.013 (4)0.000 (2)0.007 (3)0.004 (3)
O240.030 (2)0.0082 (15)0.0180 (19)0.0037 (13)0.0004 (15)0.0006 (13)
C250.007 (2)0.011 (2)0.014 (2)0.0008 (15)0.0031 (17)0.0021 (17)
N250.012 (3)0.015 (3)0.017 (3)0.002 (2)0.000 (2)0.004 (2)
O250.0174 (17)0.0170 (16)0.0168 (17)0.0051 (13)0.0022 (13)0.0042 (13)
C260.008 (2)0.013 (2)0.012 (2)0.0005 (16)0.0036 (17)0.0028 (17)
N260.013 (2)0.010 (2)0.021 (3)0.0023 (16)0.001 (2)0.0013 (18)
O10.0121 (17)0.0103 (15)0.029 (2)0.0017 (12)0.0058 (14)0.0068 (14)
O20.0266 (19)0.0164 (16)0.0175 (18)0.0084 (14)0.0061 (15)0.0068 (14)
O30.0179 (17)0.0139 (15)0.0153 (17)0.0053 (12)0.0007 (13)0.0020 (13)
O40.0198 (18)0.0182 (16)0.0160 (18)0.0009 (13)0.0045 (14)0.0044 (14)
O50.025 (3)0.025 (3)0.022 (3)0.0102 (18)0.009 (2)0.0128 (19)
O510.025 (3)0.025 (3)0.022 (3)0.0102 (18)0.009 (2)0.0128 (19)
O60.019 (2)0.023 (2)0.021 (2)0.0009 (17)0.0037 (17)0.0060 (18)
O70.0178 (18)0.0166 (17)0.0147 (19)0.0001 (13)0.0033 (15)0.0057 (15)
Geometric parameters (Å, º) top
Ba1—O22.695 (3)C22—N221.328 (6)
Ba1—O212.765 (3)C22—N231.380 (5)
Ba1—O12.773 (3)N22—C2211.456 (5)
Ba1—O13i2.787 (3)N22—H220.88
Ba1—O23i2.815 (3)C221—C2231.532 (6)
Ba1—O122.859 (3)C221—C2221.533 (6)
Ba1—O32.903 (3)C221—H22A1.00
Ba1—O112.912 (3)C222—O211.248 (5)
Ba1—O42.980 (3)C222—O221.268 (5)
Ba1—O53.238 (4)C223—O231.433 (5)
Ba1—C1223.247 (4)C223—H22B0.99
Ba1—H4A2.9124C223—H22C0.99
N11—C121.330 (7)O23—Ba1ii2.815 (3)
N11—C161.344 (8)O23—H230.8499
C12—N121.318 (7)N23—C241.395 (9)
C12—N131.383 (5)N23—C231.481 (7)
N12—C1211.465 (7)C23—H23A0.98
N12—H120.88C23—H23B0.98
C121—C1231.512 (6)C23—H23C0.98
C121—C1221.533 (6)C24—O241.224 (8)
C121—H1211.00C24—C251.469 (8)
C122—O111.249 (5)C25—N251.335 (8)
C122—O121.272 (5)C25—C261.442 (6)
C123—O131.434 (5)N25—O251.291 (6)
C123—H12A0.99C26—N261.318 (6)
C123—H12B0.99N26—H26A0.88
O13—Ba1ii2.787 (3)N26—H26B0.88
O13—H130.8498O1—H1A0.86
N13—C141.383 (6)O1—H1B0.86
N13—C131.478 (5)O2—H2A0.8799
C13—H13A0.98O2—H2B0.88
C13—H13B0.98O3—H3A0.88
C13—H13C0.98O3—H3B0.8799
C14—O141.225 (6)O4—H4A0.8999
C14—C151.456 (6)O4—H4B0.8999
C15—N151.343 (7)O5—H5A0.9501
C15—C161.447 (6)O5—H5B0.9501
N15—O151.292 (6)O51—H5A1.2214
C16—N161.317 (7)O51—H5B1.0980
N16—H16A0.88O6—H6A0.9498
N16—H16B0.88O6—H6B0.9499
N21—C221.327 (5)O7—H7A0.9499
N21—C261.346 (6)O7—H7B0.95
O2—Ba1—O2186.76 (10)H12A—C123—H12B107.9
O2—Ba1—O189.14 (10)C123—O13—Ba1ii126.2 (2)
O21—Ba1—O1129.23 (10)C123—O13—H13104.1
O2—Ba1—O13i144.28 (10)Ba1ii—O13—H13113.4
O21—Ba1—O13i128.05 (9)C14—N13—C12121.2 (4)
O1—Ba1—O13i75.07 (9)C14—N13—C13118.0 (3)
O2—Ba1—O23i136.89 (10)C12—N13—C13120.7 (4)
O21—Ba1—O23i88.31 (10)N13—C13—H13A109.5
O1—Ba1—O23i62.00 (9)N13—C13—H13B109.5
O13i—Ba1—O23i61.91 (9)H13A—C13—H13B109.5
O2—Ba1—O12113.87 (9)N13—C13—H13C109.5
O21—Ba1—O1286.32 (10)H13A—C13—H13C109.5
O1—Ba1—O12139.91 (10)H13B—C13—H13C109.5
O13i—Ba1—O1267.19 (9)O14—C14—N13120.8 (4)
O23i—Ba1—O12108.50 (9)O14—C14—C15124.0 (4)
O2—Ba1—O374.32 (10)N13—C14—C15115.2 (4)
O21—Ba1—O3147.28 (9)N15—C15—C16127.8 (4)
O1—Ba1—O377.84 (10)N15—C15—C14113.2 (4)
O13i—Ba1—O371.15 (9)C16—C15—C14119.0 (4)
O23i—Ba1—O3123.71 (9)O15—N15—C15117.4 (5)
O12—Ba1—O377.67 (9)N16—C16—N11118.6 (5)
O2—Ba1—O1168.64 (9)N16—C16—C15119.7 (4)
O21—Ba1—O1180.13 (10)N11—C16—C15121.7 (4)
O1—Ba1—O11143.20 (10)C16—N16—H16A120.0
O13i—Ba1—O11105.78 (9)C16—N16—H16B120.0
O23i—Ba1—O11151.63 (9)H16A—N16—H16B120.0
O12—Ba1—O1145.39 (8)C22—N21—C26118.7 (4)
O3—Ba1—O1168.27 (9)N21—C22—N22118.8 (4)
O2—Ba1—O468.59 (10)N21—C22—N23123.9 (4)
O21—Ba1—O455.96 (9)N22—C22—N23117.3 (4)
O1—Ba1—O475.57 (10)C22—N22—C221123.6 (4)
O13i—Ba1—O4134.08 (9)C22—N22—H22118.2
O23i—Ba1—O473.30 (9)C221—N22—H22118.2
O12—Ba1—O4142.28 (9)N22—C221—C223109.6 (3)
O3—Ba1—O4134.10 (9)N22—C221—C222111.6 (3)
O11—Ba1—O4118.84 (9)C223—C221—C222110.6 (3)
O2—Ba1—O5144.77 (11)N22—C221—H22A108.3
O21—Ba1—O562.24 (10)C223—C221—H22A108.3
O1—Ba1—O5122.80 (10)C222—C221—H22A108.3
O13i—Ba1—O566.31 (10)O21—C222—O22124.3 (4)
O23i—Ba1—O563.06 (10)O21—C222—C221119.4 (4)
O12—Ba1—O552.00 (10)O22—C222—C221116.2 (4)
O3—Ba1—O5123.05 (10)C222—O21—Ba1147.5 (3)
O11—Ba1—O588.70 (10)O23—C223—C221110.0 (3)
O4—Ba1—O5102.80 (10)O23—C223—H22B109.7
O2—Ba1—C12290.94 (10)C221—C223—H22B109.7
O21—Ba1—C12284.31 (11)O23—C223—H22C109.7
O1—Ba1—C122146.38 (11)C221—C223—H22C109.7
O13i—Ba1—C12285.69 (10)H22B—C223—H22C108.2
O23i—Ba1—C122131.09 (10)C223—O23—Ba1ii122.2 (2)
O12—Ba1—C12222.93 (10)C223—O23—H23112.1
O3—Ba1—C12269.87 (10)Ba1ii—O23—H23112.9
O11—Ba1—C12222.57 (10)C22—N23—C24121.7 (4)
O4—Ba1—C122134.94 (10)C22—N23—C23120.2 (4)
O5—Ba1—C12270.88 (11)C24—N23—C23118.0 (5)
O2—Ba1—H4A69.9N23—C23—H23A109.5
O21—Ba1—H4A38.8N23—C23—H23B109.5
O1—Ba1—H4A93.0H23A—C23—H23B109.5
O13i—Ba1—H4A141.2N23—C23—H23C109.5
O23i—Ba1—H4A79.8H23A—C23—H23C109.5
O12—Ba1—H4A125.0H23B—C23—H23C109.5
O3—Ba1—H4A143.2O24—C24—N23120.8 (6)
O11—Ba1—H4A105.4O24—C24—C25123.9 (6)
O4—Ba1—H4A17.5N23—C24—C25115.3 (6)
O5—Ba1—H4A92.1N25—C25—C26128.1 (4)
C122—Ba1—H4A118.5N25—C25—C24113.7 (5)
C12—N11—C16117.8 (5)C26—C25—C24118.2 (5)
N12—C12—N11118.5 (5)O25—N25—C25118.0 (5)
N12—C12—N13116.6 (4)N26—C26—N21118.1 (4)
N11—C12—N13124.8 (4)N26—C26—C25119.7 (4)
C12—N12—C121123.6 (5)N21—C26—C25122.2 (4)
C12—N12—H12118.2C26—N26—H26A120.0
C121—N12—H12118.2C26—N26—H26B120.0
N12—C121—C123111.5 (4)H26A—N26—H26B120.0
N12—C121—C122108.1 (4)Ba1—O1—H1A98.5
C123—C121—C122113.4 (4)Ba1—O1—H1B134.8
N12—C121—H121107.9H1A—O1—H1B113.5
C123—C121—H121107.9Ba1—O2—H2A129.2
C122—C121—H121107.9Ba1—O2—H2B129.5
O11—C122—O12124.0 (4)H2A—O2—H2B101.3
O11—C122—C121119.5 (4)Ba1—O3—H3A111.8
O12—C122—C121116.3 (4)Ba1—O3—H3B112.0
O11—C122—Ba163.4 (2)H3A—O3—H3B104.6
O12—C122—Ba161.1 (2)Ba1—O4—H4A77.0
C121—C122—Ba1167.2 (3)Ba1—O4—H4B126.9
C122—O11—Ba194.0 (3)H4A—O4—H4B116.0
C122—O12—Ba196.0 (3)Ba1—O5—H5A70.6
O13—C123—C121111.8 (3)Ba1—O5—H5B92.7
O13—C123—H12A109.3H5A—O5—H5B107.8
C121—C123—H12A109.3H5A—O51—H5B82.7
O13—C123—H12B109.3H6A—O6—H6B105.1
C121—C123—H12B109.3H7A—O7—H7B102.0
C16—N11—C12—N12176.6 (6)N12—C12—N13—C14179.8 (5)
C16—N11—C12—N134.9 (9)N11—C12—N13—C141.7 (7)
N11—C12—N12—C1210.6 (8)N12—C12—N13—C133.9 (7)
N13—C12—N12—C121179.3 (5)N11—C12—N13—C13174.7 (5)
C12—N12—C121—C12375.7 (7)C12—N13—C14—O14176.6 (5)
C12—N12—C121—C122158.9 (5)C13—N13—C14—O140.1 (7)
N12—C121—C122—O11150.5 (5)C12—N13—C14—C153.7 (6)
C123—C121—C122—O1126.3 (6)C13—N13—C14—C15179.9 (4)
N12—C121—C122—O1234.6 (6)O14—C14—C15—N155.1 (7)
C123—C121—C122—O12158.9 (4)N13—C14—C15—N15174.6 (4)
N12—C121—C122—Ba1109.5 (12)O14—C14—C15—C16174.5 (5)
C123—C121—C122—Ba1126.3 (12)N13—C14—C15—C165.7 (6)
O2—Ba1—C122—O118.7 (3)C16—C15—N15—O151.9 (8)
O21—Ba1—C122—O1177.9 (3)C14—C15—N15—O15178.5 (5)
O1—Ba1—C122—O1198.6 (3)C12—N11—C16—N16177.0 (6)
O13i—Ba1—C122—O11153.1 (3)C12—N11—C16—C152.4 (8)
O23i—Ba1—C122—O11160.7 (2)N15—C15—C16—N161.8 (8)
O12—Ba1—C122—O11171.9 (4)C14—C15—C16—N16177.7 (5)
O3—Ba1—C122—O1181.6 (3)N15—C15—C16—N11177.5 (6)
O4—Ba1—C122—O1151.3 (3)C14—C15—C16—N112.9 (7)
O5—Ba1—C122—O11140.5 (3)C26—N21—C22—N22176.5 (4)
O2—Ba1—C122—O12179.3 (3)C26—N21—C22—N232.0 (6)
O21—Ba1—C122—O1294.0 (3)N21—C22—N22—C2211.9 (6)
O1—Ba1—C122—O1289.5 (3)N23—C22—N22—C221179.4 (4)
O13i—Ba1—C122—O1234.9 (3)C22—N22—C221—C223145.1 (4)
O23i—Ba1—C122—O1211.3 (3)C22—N22—C221—C22292.0 (5)
O3—Ba1—C122—O12106.4 (3)N22—C221—C222—O212.8 (6)
O11—Ba1—C122—O12171.9 (4)C223—C221—C222—O21125.1 (4)
O4—Ba1—C122—O12120.6 (3)N22—C221—C222—O22176.5 (4)
O5—Ba1—C122—O1231.5 (3)C223—C221—C222—O2254.2 (5)
O2—Ba1—C122—C12197.9 (13)O22—C222—O21—Ba154.5 (8)
O21—Ba1—C122—C121175.4 (13)C221—C222—O21—Ba1124.8 (5)
O1—Ba1—C122—C1218.1 (14)O2—Ba1—O21—C222118.2 (5)
O13i—Ba1—C122—C12146.4 (12)O1—Ba1—O21—C222155.6 (5)
O23i—Ba1—C122—C12192.7 (12)O13i—Ba1—O21—C22253.1 (6)
O12—Ba1—C122—C12181.4 (13)O23i—Ba1—O21—C222104.7 (5)
O3—Ba1—C122—C12125.0 (12)O12—Ba1—O21—C2224.0 (5)
O11—Ba1—C122—C121106.7 (13)O3—Ba1—O21—C22264.3 (6)
O4—Ba1—C122—C121158.0 (12)O11—Ba1—O21—C22249.3 (5)
O5—Ba1—C122—C121112.8 (13)O4—Ba1—O21—C222175.6 (6)
O12—C122—O11—Ba18.5 (5)O5—Ba1—O21—C22244.4 (5)
C121—C122—O11—Ba1165.9 (3)C122—Ba1—O21—C22226.9 (5)
O2—Ba1—O11—C122170.6 (3)N22—C221—C223—O2362.9 (4)
O21—Ba1—O11—C12299.0 (3)C222—C221—C223—O2360.6 (4)
O1—Ba1—O11—C122114.0 (3)C221—C223—O23—Ba1ii127.4 (3)
O13i—Ba1—O11—C12227.9 (3)N21—C22—N23—C243.9 (7)
O23i—Ba1—O11—C12231.7 (4)N22—C22—N23—C24174.6 (5)
O12—Ba1—O11—C1224.4 (2)N21—C22—N23—C23177.2 (5)
O3—Ba1—O11—C12289.6 (3)N22—C22—N23—C234.3 (7)
O4—Ba1—O11—C122140.9 (3)C22—N23—C24—O24176.1 (5)
O5—Ba1—O11—C12237.0 (3)C23—N23—C24—O242.8 (9)
O11—C122—O12—Ba18.7 (5)C22—N23—C24—C252.7 (8)
C121—C122—O12—Ba1165.9 (3)C23—N23—C24—C25178.4 (6)
O2—Ba1—O12—C1220.7 (3)O24—C24—C25—N252.7 (9)
O21—Ba1—O12—C12284.1 (3)N23—C24—C25—N25178.5 (6)
O1—Ba1—O12—C122120.7 (3)O24—C24—C25—C26178.7 (6)
O13i—Ba1—O12—C122141.7 (3)N23—C24—C25—C260.0 (8)
O23i—Ba1—O12—C122171.1 (3)C26—C25—N25—O250.8 (9)
O3—Ba1—O12—C12267.2 (3)C24—C25—N25—O25179.2 (6)
O11—Ba1—O12—C1224.3 (2)C22—N21—C26—N26179.4 (4)
O4—Ba1—O12—C12284.7 (3)C22—N21—C26—C250.8 (6)
O5—Ba1—O12—C122141.3 (3)N25—C25—C26—N261.3 (8)
N12—C121—C123—O1354.7 (5)C24—C25—C26—N26179.7 (5)
C122—C121—C123—O1367.6 (4)N25—C25—C26—N21179.9 (5)
C121—C123—O13—Ba1ii140.8 (3)C24—C25—C26—N211.8 (7)
Symmetry codes: (i) x+1, y, z; (ii) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N12—H12···O70.882.252.989 (7)141
O13—H13···O60.851.932.772 (5)168
N16—H16A···O14iii0.882.002.845 (7)161
N16—H16B···O150.881.972.620 (7)130
O23—H23···O70.852.072.885 (5)160
N26—H26A···O24iv0.882.042.873 (6)158
N26—H26B···O250.881.982.631 (6)130
O1—H1A···O11i0.861.992.809 (4)158
O1—H1B···O22v0.861.912.750 (5)164
O2—H2A···O15vi0.881.812.691 (4)176
O2—H2A···N15vi0.882.463.261 (6)152
O2—H2B···O22iii0.881.992.849 (4)166
O3—H3A···O25vii0.881.922.793 (4)171
O3—H3B···O5iii0.881.882.707 (5)155
O3—H3B···O51iii0.881.962.831 (17)171
O4—H4A···O210.901.892.702 (5)149
O4—H4B···N15vi0.902.163.012 (6)159
O4—H4B···O14vi0.902.473.134 (4)131
O5—H5A···O120.951.792.695 (5)157
O5—H5B···O220.951.932.873 (6)175
O6—H6A···O12ii0.951.962.769 (6)141
O6—H6B···N25viii0.952.283.083 (8)142
O6—H6B···O24viii0.952.323.160 (6)147
O7—H7A···O3ix0.951.892.791 (4)157
O7—H7B···O220.952.032.935 (6)159
Symmetry codes: (i) x+1, y, z; (ii) x1, y, z; (iii) x, y+1, z; (iv) x, y1, z; (v) x+1, y+1, z; (vi) x+1, y+1, z+1; (vii) x, y, z1; (viii) x1, y1, z1; (ix) x1, y1, z.
(VI) # Sr(py-glygly)2·4H2O top
Crystal data top
C18H30N12O14SrF(000) = 1488
Mr = 726.16Dx = 1.837 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2982 reflections
a = 12.9517 (3) Åθ = 3.1–27.5°
b = 7.7020 (2) ŵ = 2.15 mm1
c = 26.5416 (7) ÅT = 120 K
β = 97.2770 (12)°Plate, purple
V = 2626.30 (11) Å30.25 × 0.25 × 0.06 mm
Z = 4
Data collection top
Kappa-CCD
diffractometer
2982 independent reflections
Radiation source: fine-focus sealed X-ray tube2369 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.073
ϕ scans, and ω scans with κ offsetsθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 1216
Tmin = 0.616, Tmax = 0.882k = 99
16348 measured reflectionsl = 3434
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.134H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0779P)2 + 5.4996P]
where P = (Fo2 + 2Fc2)/3
2982 reflections(Δ/σ)max < 0.001
205 parametersΔρmax = 1.43 e Å3
0 restraintsΔρmin = 0.74 e Å3
Crystal data top
C18H30N12O14SrV = 2626.30 (11) Å3
Mr = 726.16Z = 4
Monoclinic, C2/cMo Kα radiation
a = 12.9517 (3) ŵ = 2.15 mm1
b = 7.7020 (2) ÅT = 120 K
c = 26.5416 (7) Å0.25 × 0.25 × 0.06 mm
β = 97.2770 (12)°
Data collection top
Kappa-CCD
diffractometer
2982 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
2369 reflections with I > 2σ(I)
Tmin = 0.616, Tmax = 0.882Rint = 0.073
16348 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0490 restraints
wR(F2) = 0.134H-atom parameters constrained
S = 1.05Δρmax = 1.43 e Å3
2982 reflectionsΔρmin = 0.74 e Å3
205 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.50000.74133 (6)0.25000.01659 (17)
N10.7172 (2)0.9302 (4)0.03949 (10)0.0111 (6)
C20.8036 (2)0.9896 (4)0.06703 (12)0.0102 (6)
N210.8157 (2)0.9587 (4)0.11657 (10)0.0108 (6)
C210.7416 (3)0.8527 (4)0.14050 (13)0.0138 (7)
C220.6429 (3)0.9434 (4)0.15274 (12)0.0118 (7)
O210.58106 (19)0.8578 (3)0.17423 (9)0.0176 (5)
N220.6280 (2)1.1078 (4)0.13875 (10)0.0133 (6)
C230.5397 (3)1.2102 (4)0.14926 (13)0.0131 (7)
C240.5654 (3)1.3464 (4)0.19121 (12)0.0123 (7)
O220.64266 (19)1.3184 (4)0.22429 (9)0.0211 (6)
O230.50455 (18)1.4727 (3)0.18991 (8)0.0133 (5)
N30.8794 (2)1.0838 (4)0.04732 (10)0.0105 (6)
C30.9709 (3)1.1498 (5)0.08075 (12)0.0140 (7)
C40.8731 (3)1.1185 (4)0.00456 (12)0.0113 (7)
O40.94393 (19)1.1953 (3)0.02177 (9)0.0152 (5)
C50.7783 (3)1.0571 (4)0.03537 (12)0.0116 (7)
N50.7717 (2)1.1014 (4)0.08459 (10)0.0154 (6)
O50.69042 (19)1.0500 (3)0.11401 (9)0.0187 (6)
C60.7028 (3)0.9645 (4)0.01033 (12)0.0121 (7)
N60.6155 (2)0.9101 (4)0.03714 (11)0.0148 (6)
O10.6184 (2)1.0023 (4)0.28105 (10)0.0266 (6)
O20.6785 (2)0.6241 (4)0.27728 (10)0.0249 (6)
H210.86981.00320.13560.013*
H21A0.77820.80480.17250.017*
H21B0.72070.75330.11780.017*
H220.67471.15740.12210.016*
H23A0.48561.13120.15930.016*
H23B0.51031.27010.11770.016*
H3A1.01821.05330.09110.021*
H3B0.94801.20350.11090.021*
H3C1.00721.23630.06240.021*
H6A0.56900.85340.02210.018*
H6B0.60400.93090.07000.018*
H1A0.63181.10480.26460.032*
H1B0.66620.98940.31010.032*
H2A0.67870.52800.25610.030*
H2B0.73790.69030.27520.030*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0151 (3)0.0191 (3)0.0155 (2)0.0000.00167 (17)0.000
N10.0081 (13)0.0113 (14)0.0138 (13)0.0014 (11)0.0010 (10)0.0007 (10)
C20.0100 (16)0.0061 (15)0.0152 (16)0.0028 (12)0.0047 (12)0.0001 (11)
N210.0103 (14)0.0112 (14)0.0102 (13)0.0017 (11)0.0007 (10)0.0014 (10)
C210.0164 (17)0.0099 (17)0.0154 (16)0.0005 (14)0.0029 (13)0.0035 (12)
C220.0126 (16)0.0086 (16)0.0133 (15)0.0015 (13)0.0017 (12)0.0029 (12)
O210.0180 (13)0.0130 (13)0.0224 (13)0.0014 (10)0.0047 (10)0.0019 (10)
N220.0125 (14)0.0110 (14)0.0168 (14)0.0013 (11)0.0034 (11)0.0013 (11)
C230.0100 (16)0.0111 (16)0.0170 (17)0.0005 (13)0.0028 (13)0.0019 (12)
C240.0129 (17)0.0117 (18)0.0125 (16)0.0003 (13)0.0026 (13)0.0014 (12)
O220.0148 (13)0.0271 (15)0.0195 (13)0.0083 (11)0.0056 (10)0.0087 (11)
O230.0133 (12)0.0121 (12)0.0140 (11)0.0036 (10)0.0006 (9)0.0001 (9)
N30.0074 (13)0.0118 (14)0.0118 (13)0.0010 (11)0.0009 (10)0.0024 (10)
C30.0111 (16)0.0154 (18)0.0139 (16)0.0048 (14)0.0042 (13)0.0019 (12)
C40.0120 (17)0.0078 (16)0.0135 (16)0.0028 (13)0.0003 (12)0.0004 (12)
O40.0126 (12)0.0173 (13)0.0161 (12)0.0049 (10)0.0029 (9)0.0003 (9)
C50.0118 (16)0.0103 (16)0.0127 (15)0.0013 (13)0.0017 (12)0.0007 (12)
N50.0164 (15)0.0145 (16)0.0144 (14)0.0013 (12)0.0013 (11)0.0004 (11)
O50.0181 (13)0.0208 (14)0.0151 (12)0.0014 (11)0.0057 (10)0.0014 (9)
C60.0115 (17)0.0085 (16)0.0159 (16)0.0013 (13)0.0000 (13)0.0018 (12)
N60.0116 (14)0.0171 (16)0.0147 (14)0.0046 (12)0.0013 (11)0.0002 (11)
O10.0299 (16)0.0247 (15)0.0238 (14)0.0046 (12)0.0020 (11)0.0008 (11)
O20.0192 (14)0.0224 (14)0.0315 (15)0.0013 (11)0.0026 (11)0.0042 (11)
Geometric parameters (Å, º) top
Sr1—O22.502 (3)C23—H23B0.99
Sr1—O212.547 (2)C24—O231.249 (4)
Sr1—O12.598 (3)C24—O221.264 (4)
Sr1—O1i2.598 (3)N3—C41.395 (4)
Sr1—O23ii2.618 (2)N3—C31.477 (4)
Sr1—H2A2.8264C3—H3A0.98
N1—C21.337 (4)C3—H3B0.98
N1—C61.338 (4)C3—H3C0.98
C2—N211.326 (4)C4—O41.228 (4)
C2—N31.377 (4)C4—C51.464 (5)
N21—C211.465 (4)C5—N51.342 (4)
N21—H210.88C5—C61.439 (5)
C21—C221.528 (5)N5—O51.291 (4)
C21—H21A0.99C6—N61.326 (4)
C21—H21B0.99N6—H6A0.88
C22—O211.231 (4)N6—H6B0.88
C22—N221.327 (4)O1—H1A0.93
N22—C231.445 (4)O1—H1B0.9299
N22—H220.88O2—H2A0.9302
C23—C241.535 (5)O2—H2B0.9302
C23—H23A0.99
O2i—Sr1—O2137.70 (13)C22—C21—H21B108.1
O2i—Sr1—O21i84.11 (9)H21A—C21—H21B107.3
O2—Sr1—O21i110.90 (8)O21—C22—N22124.1 (3)
O2i—Sr1—O21110.90 (8)O21—C22—C21117.7 (3)
O2—Sr1—O2184.11 (9)N22—C22—C21118.2 (3)
O21i—Sr1—O21138.75 (11)C22—O21—Sr1155.7 (2)
O2i—Sr1—O1149.05 (9)C22—N22—C23123.9 (3)
O2—Sr1—O172.58 (9)C22—N22—H22118.1
O21i—Sr1—O176.28 (8)C23—N22—H22118.1
O21—Sr1—O172.08 (8)N22—C23—C24114.2 (3)
O2i—Sr1—O1i72.58 (9)N22—C23—H23A108.7
O2—Sr1—O1i149.05 (9)C24—C23—H23A108.7
O21i—Sr1—O1i72.08 (8)N22—C23—H23B108.7
O21—Sr1—O1i76.28 (8)C24—C23—H23B108.7
O1—Sr1—O1i78.66 (12)H23A—C23—H23B107.6
O2i—Sr1—O23iii78.45 (8)O23—C24—O22126.4 (3)
O2—Sr1—O23iii68.27 (8)O23—C24—C23115.7 (3)
O21i—Sr1—O23iii75.76 (7)O22—C24—C23117.8 (3)
O21—Sr1—O23iii143.40 (8)C24—O23—Sr1iv131.4 (2)
O1—Sr1—O23iii118.43 (8)C2—N3—C4121.4 (3)
O1i—Sr1—O23iii138.31 (8)C2—N3—C3120.6 (3)
O2i—Sr1—O23ii68.27 (8)C4—N3—C3118.0 (3)
O2—Sr1—O23ii78.45 (8)N3—C3—H3A109.5
O21i—Sr1—O23ii143.40 (8)N3—C3—H3B109.5
O21—Sr1—O23ii75.76 (7)H3A—C3—H3B109.5
O1—Sr1—O23ii138.31 (8)N3—C3—H3C109.5
O1i—Sr1—O23ii118.43 (8)H3A—C3—H3C109.5
O23iii—Sr1—O23ii75.54 (10)H3B—C3—H3C109.5
O2i—Sr1—H2A121.8O4—C4—N3120.4 (3)
O2—Sr1—H2A18.9O4—C4—C5124.1 (3)
O21i—Sr1—H2A125.2N3—C4—C5115.5 (3)
O21—Sr1—H2A80.4N5—C5—C6127.7 (3)
O1—Sr1—H2A89.2N5—C5—C4114.0 (3)
O1i—Sr1—H2A156.1C6—C5—C4118.2 (3)
O23iii—Sr1—H2A65.6O5—N5—C5117.2 (3)
O23ii—Sr1—H2A59.6N6—C6—N1118.1 (3)
C2—N1—C6118.4 (3)N6—C6—C5119.5 (3)
N21—C2—N1117.8 (3)N1—C6—C5122.4 (3)
N21—C2—N3118.1 (3)C6—N6—H6A120.0
N1—C2—N3124.1 (3)C6—N6—H6B120.0
C2—N21—C21121.9 (3)H6A—N6—H6B120.0
C2—N21—H21119.1Sr1—O1—H1A130.2
C21—N21—H21119.1Sr1—O1—H1B119.0
N21—C21—C22116.7 (3)H1A—O1—H1B109.6
N21—C21—H21A108.1Sr1—O2—H2A100.7
C22—C21—H21A108.1Sr1—O2—H2B121.7
N21—C21—H21B108.1H2A—O2—H2B109.6
C6—N1—C2—N21178.3 (3)C23—C24—O23—Sr1iv178.2 (2)
C6—N1—C2—N30.2 (5)N21—C2—N3—C4178.7 (3)
N1—C2—N21—C214.4 (5)N1—C2—N3—C42.8 (5)
N3—C2—N21—C21177.1 (3)N21—C2—N3—C30.6 (4)
C2—N21—C21—C2282.0 (4)N1—C2—N3—C3177.9 (3)
N21—C21—C22—O21177.9 (3)C2—N3—C4—O4176.4 (3)
N21—C21—C22—N223.4 (4)C3—N3—C4—O42.9 (5)
N22—C22—O21—Sr187.7 (6)C2—N3—C4—C53.5 (4)
C21—C22—O21—Sr193.7 (6)C3—N3—C4—C5177.2 (3)
O2i—Sr1—O21—C22161.8 (5)O4—C4—C5—N53.9 (5)
O2—Sr1—O21—C2259.1 (5)N3—C4—C5—N5176.3 (3)
O21i—Sr1—O21—C2256.2 (5)O4—C4—C5—C6178.3 (3)
O1—Sr1—O21—C2214.5 (5)N3—C4—C5—C61.6 (4)
O1i—Sr1—O21—C2296.8 (6)C6—C5—N5—O53.0 (5)
O23iii—Sr1—O21—C2299.3 (5)C4—C5—N5—O5179.4 (3)
O23ii—Sr1—O21—C22138.6 (6)C2—N1—C6—N6177.9 (3)
O21—C22—N22—C233.3 (5)C2—N1—C6—C52.2 (5)
C21—C22—N22—C23178.1 (3)N5—C5—C6—N61.3 (5)
C22—N22—C23—C24106.1 (4)C4—C5—C6—N6178.8 (3)
N22—C23—C24—O23156.5 (3)N5—C5—C6—N1178.7 (3)
N22—C23—C24—O2225.7 (4)C4—C5—C6—N11.2 (5)
O22—C24—O23—Sr1iv0.6 (5)
Symmetry codes: (i) x+1, y, z+1/2; (ii) x, y1, z; (iii) x+1, y1, z+1/2; (iv) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N21—H21···O23v0.882.132.928 (4)151
N21—H21···O2vi0.882.643.084 (4)112
N22—H22···N5vii0.882.263.041 (4)148
N6—H6A···O4viii0.882.032.841 (4)153
N6—H6B···O50.881.952.601 (4)130
O1—H1A···O220.931.982.901 (4)173
O1—H1B···O5ix0.932.022.852 (4)148
O2—H2A···O22ii0.931.852.752 (4)162
O2—H2B···O22x0.931.832.763 (4)176
Symmetry codes: (ii) x, y1, z; (v) x+1/2, y1/2, z; (vi) x+3/2, y+1/2, z+1/2; (vii) x+3/2, y+5/2, z; (viii) x1/2, y1/2, z; (ix) x, y+2, z+1/2; (x) x+3/2, y1/2, z+1/2.
(VII) Bis[N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidin-2-yl) glycylglycinato] diaquabariuium: top
Crystal data top
C18H30BaN12O14F(000) = 1560
Mr = 775.87Dx = 1.836 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3148 reflections
a = 13.3918 (3) Åθ = 3.1–27.4°
b = 7.4669 (2) ŵ = 1.51 mm1
c = 28.8211 (7) ÅT = 120 K
β = 103.131 (1)°Plate, pink
V = 2806.62 (12) Å30.20 × 0.15 × 0.04 mm
Z = 4
Data collection top
Kappa-CCD
diffractometer
3148 independent reflections
Radiation source: fine-focus sealed X-ray tube2905 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
ϕ scans, and ω scans with κ offsetsθmax = 27.4°, θmin = 3.1°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 178
Tmin = 0.753, Tmax = 0.942k = 98
7598 measured reflectionsl = 3737
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H-atom parameters constrained
S = 1.24 w = 1/[σ2(Fo2)P)2 + 16.8531P]
where P = (Fo2 + 2Fc2)/3
3148 reflections(Δ/σ)max = 0.001
205 parametersΔρmax = 0.99 e Å3
0 restraintsΔρmin = 0.84 e Å3
Crystal data top
C18H30BaN12O14V = 2806.62 (12) Å3
Mr = 775.87Z = 4
Monoclinic, C2/cMo Kα radiation
a = 13.3918 (3) ŵ = 1.51 mm1
b = 7.4669 (2) ÅT = 120 K
c = 28.8211 (7) Å0.20 × 0.15 × 0.04 mm
β = 103.131 (1)°
Data collection top
Kappa-CCD
diffractometer
3148 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
2905 reflections with I > 2σ(I)
Tmin = 0.753, Tmax = 0.942Rint = 0.046
7598 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.085H-atom parameters constrained
S = 1.24 w = 1/[σ2(Fo2)P)2 + 16.8531P]
where P = (Fo2 + 2Fc2)/3
3148 reflectionsΔρmax = 0.99 e Å3
205 parametersΔρmin = 0.84 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.50000.94154 (4)0.25000.01272 (10)
N10.4070 (2)0.4847 (4)0.03921 (10)0.0123 (6)
C20.4306 (3)0.3348 (4)0.06444 (13)0.0120 (7)
N210.4676 (2)0.3508 (4)0.11119 (10)0.0127 (6)
C210.4900 (3)0.5249 (5)0.13395 (13)0.0150 (7)
C220.3999 (3)0.6297 (5)0.14435 (12)0.0133 (7)
O210.4174 (2)0.7776 (3)0.16391 (9)0.0164 (5)
N220.3064 (2)0.5581 (4)0.13169 (11)0.0153 (6)
C230.2157 (3)0.6481 (5)0.14002 (13)0.0150 (7)
C240.1691 (3)0.5613 (5)0.17811 (12)0.0137 (7)
O220.22102 (19)0.4459 (3)0.20536 (9)0.0182 (5)
O230.08128 (19)0.6143 (3)0.17992 (9)0.0161 (5)
N30.4162 (2)0.1638 (4)0.04530 (10)0.0115 (6)
C30.4430 (3)0.0039 (5)0.07562 (13)0.0154 (7)
C40.3763 (3)0.1388 (5)0.00327 (12)0.0120 (7)
O40.3665 (2)0.0136 (3)0.01996 (9)0.0167 (5)
C50.3468 (3)0.2995 (4)0.03134 (13)0.0121 (7)
N50.2986 (2)0.2705 (4)0.07705 (11)0.0151 (6)
O50.2718 (2)0.4083 (3)0.10397 (9)0.0188 (6)
C60.3657 (3)0.4701 (4)0.00733 (12)0.0128 (7)
N60.3411 (2)0.6188 (4)0.03214 (11)0.0164 (6)
O10.6459 (2)1.1640 (4)0.30457 (10)0.0229 (6)
O20.3758 (2)0.6534 (4)0.26438 (10)0.0227 (6)
H210.47890.25350.12880.015*
H21A0.52310.59990.11340.018*
H21B0.54080.50710.16440.018*
H220.29930.45250.11780.018*
H2C0.16310.65130.10970.018*
H2D0.23390.77350.14950.018*
H3A0.42430.02370.10620.018*
H3B0.51690.01820.08120.018*
H3C0.40550.10000.05970.018*
H6A0.35200.72350.01790.020*
H6B0.31370.61310.06290.020*
H1A0.68431.13450.33340.027*
H1B0.67211.27310.30140.027*
H2A0.33530.57150.24630.027*
H2B0.33590.73290.27520.027*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.01633 (16)0.01032 (15)0.01042 (15)0.0000.00073 (11)0.000
N10.0128 (14)0.0088 (14)0.0148 (15)0.0003 (11)0.0021 (12)0.0008 (11)
C20.0088 (16)0.0112 (16)0.0167 (17)0.0011 (13)0.0042 (13)0.0012 (13)
N210.0158 (15)0.0103 (14)0.0123 (14)0.0010 (11)0.0036 (12)0.0006 (11)
C210.0124 (17)0.0162 (18)0.0153 (17)0.0005 (14)0.0010 (13)0.0029 (14)
C220.0165 (17)0.0130 (16)0.0103 (16)0.0008 (14)0.0032 (14)0.0000 (13)
O210.0205 (13)0.0116 (12)0.0159 (13)0.0010 (10)0.0018 (10)0.0020 (10)
N220.0132 (14)0.0119 (14)0.0219 (16)0.0001 (12)0.0064 (12)0.0029 (12)
C230.0130 (17)0.0133 (17)0.0201 (18)0.0023 (13)0.0064 (14)0.0023 (14)
C240.0157 (17)0.0119 (16)0.0124 (16)0.0038 (14)0.0009 (13)0.0036 (14)
O220.0193 (13)0.0165 (12)0.0174 (13)0.0029 (11)0.0012 (10)0.0019 (11)
O230.0114 (12)0.0201 (13)0.0177 (13)0.0028 (10)0.0052 (10)0.0014 (10)
N30.0137 (14)0.0083 (13)0.0120 (14)0.0009 (11)0.0018 (11)0.0014 (11)
C30.0201 (18)0.0087 (15)0.0161 (18)0.0028 (13)0.0016 (14)0.0042 (13)
C40.0111 (16)0.0119 (17)0.0134 (17)0.0004 (13)0.0031 (13)0.0007 (13)
O40.0240 (14)0.0069 (12)0.0182 (13)0.0009 (10)0.0027 (11)0.0021 (10)
C50.0105 (16)0.0110 (16)0.0149 (17)0.0008 (13)0.0030 (13)0.0024 (13)
N50.0153 (15)0.0132 (15)0.0164 (15)0.0002 (12)0.0025 (12)0.0015 (12)
O50.0242 (14)0.0135 (13)0.0166 (13)0.0015 (10)0.0007 (11)0.0036 (10)
C60.0115 (16)0.0116 (17)0.0160 (17)0.0013 (13)0.0050 (13)0.0011 (13)
N60.0260 (17)0.0060 (13)0.0153 (15)0.0003 (12)0.0008 (13)0.0009 (11)
O10.0247 (15)0.0202 (14)0.0209 (14)0.0089 (11)0.0010 (11)0.0016 (11)
O20.0164 (14)0.0260 (15)0.0249 (15)0.0041 (11)0.0030 (11)0.0031 (12)
Geometric parameters (Å, º) top
Ba1—O212.762 (2)C23—H2D0.9900
Ba1—O12.767 (3)C24—O231.254 (4)
Ba1—O22.808 (3)C24—O221.262 (4)
Ba1—O23i2.816 (2)N3—C41.393 (4)
Ba1—O23ii2.816 (2)N3—C31.475 (4)
Ba1—H2B2.9167C3—H3A0.9800
N1—C21.333 (4)C3—H3B0.9800
N1—C61.334 (5)C3—H3C0.9800
C2—N211.331 (4)C4—O41.230 (4)
C2—N31.386 (4)C4—C51.451 (5)
N21—C211.456 (4)C5—N51.346 (5)
N21—H210.8800C5—C61.444 (5)
C21—C221.524 (5)N5—O51.289 (4)
C21—H21A0.9900C6—N61.321 (4)
C21—H21B0.9900N6—H6A0.8800
C22—O211.238 (4)N6—H6B0.8800
C22—N221.334 (5)O1—H1A0.8999
N22—C231.455 (4)O1—H1B0.9000
N22—H220.8800O2—H2A0.9000
C23—C241.525 (5)O2—H2B0.9000
C23—H2C0.9900
O21—Ba1—O21iii127.40 (10)N22—C22—C21118.4 (3)
O21—Ba1—O1149.72 (8)C22—O21—Ba1143.1 (2)
O21iii—Ba1—O170.63 (8)C22—N22—C23122.4 (3)
O21—Ba1—O1iii70.63 (8)C22—N22—H22118.8
O21iii—Ba1—O1iii149.72 (8)C23—N22—H22118.8
O1—Ba1—O1iii106.22 (12)N22—C23—C24114.5 (3)
O21—Ba1—O270.32 (8)N22—C23—H2C108.6
O21iii—Ba1—O269.98 (8)C24—C23—H2C108.6
O1—Ba1—O2137.89 (8)N22—C23—H2D108.6
O1iii—Ba1—O2100.26 (8)C24—C23—H2D108.6
O21—Ba1—O2iii69.98 (8)H2C—C23—H2D107.6
O21iii—Ba1—O2iii70.32 (8)O23—C24—O22125.4 (3)
O1—Ba1—O2iii100.26 (8)O23—C24—C23115.9 (3)
O1iii—Ba1—O2iii137.89 (8)O22—C24—C23118.7 (3)
O2—Ba1—O2iii79.95 (11)C24—O23—Ba1iv113.9 (2)
O21—Ba1—O23i72.53 (7)C2—N3—C4120.7 (3)
O21iii—Ba1—O23i134.92 (7)C2—N3—C3121.1 (3)
O1—Ba1—O23i78.14 (8)C4—N3—C3118.2 (3)
O1iii—Ba1—O23i69.85 (8)N3—C3—H3A109.5
O2—Ba1—O23i142.72 (8)N3—C3—H3B109.5
O2iii—Ba1—O23i84.64 (8)H3A—C3—H3B109.5
O21—Ba1—O23ii134.92 (7)N3—C3—H3C109.5
O21iii—Ba1—O23ii72.53 (7)H3A—C3—H3C109.5
O1—Ba1—O23ii69.85 (8)H3B—C3—H3C109.5
O1iii—Ba1—O23ii78.14 (8)O4—C4—N3120.0 (3)
O2—Ba1—O23ii84.64 (8)O4—C4—C5123.7 (3)
O2iii—Ba1—O23ii142.72 (8)N3—C4—C5116.3 (3)
O23i—Ba1—O23ii125.46 (10)N5—C5—C6127.1 (3)
C2—N1—C6118.2 (3)N5—C5—C4115.0 (3)
N21—C2—N1117.7 (3)C6—C5—C4117.8 (3)
N21—C2—N3118.1 (3)O5—N5—C5117.8 (3)
N1—C2—N3124.2 (3)N6—C6—N1118.1 (3)
C2—N21—C21121.8 (3)N6—C6—C5119.1 (3)
C2—N21—H21119.1N1—C6—C5122.7 (3)
C21—N21—H21119.1C6—N6—H6A120.0
N21—C21—C22117.1 (3)C6—N6—H6B120.0
N21—C21—H21A108.0H6A—N6—H6B120.0
C22—C21—H21A108.0Ba1—O1—H1A124.1
N21—C21—H21B108.0Ba1—O1—H1B136.6
C22—C21—H21B108.0H1A—O1—H1B99.3
H21A—C21—H21B107.3Ba1—O2—H2A137.2
O21—C22—N22123.5 (3)Ba1—O2—H2B87.9
O21—C22—C21118.1 (3)H2A—O2—H2B108.8
C6—N1—C2—N21177.2 (3)C23—C24—O23—Ba1iv178.8 (2)
C6—N1—C2—N31.0 (5)N21—C2—N3—C4179.1 (3)
N1—C2—N21—C215.0 (5)N1—C2—N3—C41.0 (5)
N3—C2—N21—C21176.8 (3)N21—C2—N3—C31.1 (5)
C2—N21—C21—C2280.5 (4)N1—C2—N3—C3179.2 (3)
N21—C21—C22—O21179.6 (3)C2—N3—C4—O4178.2 (3)
N21—C21—C22—N220.8 (5)C3—N3—C4—O41.7 (5)
N22—C22—O21—Ba1106.5 (4)C2—N3—C4—C52.9 (5)
C21—C22—O21—Ba173.9 (5)C3—N3—C4—C5177.3 (3)
O21iii—Ba1—O21—C221.3 (4)O4—C4—C5—N55.6 (5)
O1—Ba1—O21—C22117.5 (4)N3—C4—C5—N5173.3 (3)
O1iii—Ba1—O21—C22153.3 (4)O4—C4—C5—C6178.1 (3)
O2—Ba1—O21—C2244.3 (4)N3—C4—C5—C63.0 (5)
O2iii—Ba1—O21—C2241.9 (4)C6—C5—N5—O55.2 (5)
O23i—Ba1—O21—C22132.5 (4)C4—C5—N5—O5178.9 (3)
O23ii—Ba1—O21—C22104.5 (4)C2—N1—C6—N6179.1 (3)
O21—C22—N22—C230.3 (5)C2—N1—C6—C50.8 (5)
C21—C22—N22—C23179.9 (3)N5—C5—C6—N65.3 (5)
C22—N22—C23—C24110.0 (4)C4—C5—C6—N6178.9 (3)
N22—C23—C24—O23167.1 (3)N5—C5—C6—N1174.5 (3)
N22—C23—C24—O2213.8 (5)C4—C5—C6—N11.2 (5)
O22—C24—O23—Ba1iv2.2 (4)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1, y, z+1/2; (iv) x1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N21—H21···O23v0.882.052.827 (4)146
N22—H22···N5vi0.882.273.077 (4)152
N6—H6A···O4vii0.881.972.779 (4)151
N6—H6B···O50.881.942.597 (4)131
O1—H1A···O5viii0.901.942.839 (4)175
O1—H1B···O22ix0.901.972.814 (4)156
O2—H2A···O220.901.952.826 (4)165
O2—H2B···O22ii0.901.902.779 (4)164
Symmetry codes: (ii) x+1/2, y+1/2, z+1/2; (v) x+1/2, y1/2, z; (vi) x+1/2, y+1/2, z; (vii) x, y+1, z; (viii) x+1/2, y+3/2, z+1/2; (ix) x+1, y+1, z+1/2.
(VIII) top
Crystal data top
C20H36CaN10O12·C20H38CaN10O13·3.123(H2O)F(000) = 1450
Mr = 1371.37Dx = 1.467 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 14077 reflections
a = 7.5557 (3) Åθ = 2.0–29.2°
b = 13.9726 (6) ŵ = 0.28 mm1
c = 29.4179 (12) ÅT = 120 K
β = 91.803 (2)°Plate, pink
V = 3104.2 (2) Å30.05 × 0.04 × 0.03 mm
Z = 2
Data collection top
Kappa-CCD
diffractometer
14077 independent reflections
Radiation source: fine-focus sealed X-ray tube13181 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ϕ scans, and ω scans with κ offsetsθmax = 29.2°, θmin = 2.0°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 107
Tmin = 0.967, Tmax = 0.992k = 1817
21417 measured reflectionsl = 4041
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.085 w = 1/[σ2(Fo2) + (0.0407P)2 + 0.4491P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.003
14077 reflectionsΔρmax = 0.40 e Å3
888 parametersΔρmin = 0.39 e Å3
48 restraintsAbsolute structure: Flack (1983), 5320 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.085 (17)
Crystal data top
C20H36CaN10O12·C20H38CaN10O13·3.123(H2O)V = 3104.2 (2) Å3
Mr = 1371.37Z = 2
Monoclinic, P21Mo Kα radiation
a = 7.5557 (3) ŵ = 0.28 mm1
b = 13.9726 (6) ÅT = 120 K
c = 29.4179 (12) Å0.05 × 0.04 × 0.03 mm
β = 91.803 (2)°
Data collection top
Kappa-CCD
diffractometer
14077 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
13181 reflections with I > 2σ(I)
Tmin = 0.967, Tmax = 0.992Rint = 0.027
21417 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.085Δρmax = 0.40 e Å3
S = 1.05Δρmin = 0.39 e Å3
14077 reflectionsAbsolute structure: Flack (1983), 5320 Friedel pairs
888 parametersAbsolute structure parameter: 0.085 (17)
48 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.26363 (5)0.88390 (3)0.653031 (13)0.01253 (8)
N110.1461 (2)1.21782 (12)0.55044 (6)0.0157 (3)
C120.2791 (2)1.20094 (14)0.57804 (7)0.0136 (4)
N120.2415 (2)1.17440 (13)0.62066 (6)0.0169 (3)
C1210.0589 (3)1.15611 (15)0.63785 (7)0.0178 (4)
C1220.0577 (3)1.06226 (15)0.66547 (7)0.0161 (4)
C1230.0256 (5)1.2376 (3)0.66582 (12)0.0168 (7)0.722 (7)
C1240.0238 (8)1.3316 (5)0.6396 (2)0.0239 (12)0.722 (7)
C1250.0656 (5)1.2483 (3)0.71088 (11)0.0308 (9)0.722 (7)
C1260.0370 (14)1.2422 (6)0.6740 (3)0.017 (2)0.278 (7)
C1270.011 (2)1.3392 (16)0.6477 (7)0.025 (3)0.278 (7)
C1280.1275 (11)1.2282 (6)0.7058 (3)0.025 (2)0.278 (7)
O1210.0895 (2)1.02203 (11)0.67081 (5)0.0211 (3)
O1220.2018 (2)1.03584 (12)0.68134 (6)0.0233 (3)
N130.4563 (2)1.21158 (13)0.56520 (6)0.0154 (3)
C130.5961 (3)1.19186 (16)0.59783 (8)0.0203 (4)
C140.5073 (3)1.24162 (15)0.52156 (7)0.0160 (4)
O140.66550 (19)1.25574 (12)0.51112 (5)0.0217 (3)
C150.3638 (2)1.25345 (15)0.48993 (7)0.0147 (4)
N150.4174 (2)1.27885 (13)0.44739 (6)0.0179 (3)
O150.29608 (19)1.28768 (11)0.41827 (5)0.0197 (3)
C160.1837 (2)1.24100 (14)0.50701 (7)0.0139 (4)
N160.0475 (2)1.25478 (13)0.48041 (6)0.0164 (3)
N210.6536 (2)0.55117 (12)0.55712 (6)0.0153 (3)
N220.7563 (2)0.59354 (13)0.62831 (6)0.0150 (3)
C220.7897 (3)0.56806 (14)0.58550 (7)0.0149 (4)
C2210.5766 (2)0.61530 (14)0.64328 (7)0.0137 (4)
C2220.5859 (3)0.70665 (14)0.67298 (6)0.0141 (4)
C2230.4956 (3)0.53136 (15)0.66992 (7)0.0172 (4)
C2240.4783 (3)0.44063 (16)0.64099 (8)0.0219 (4)
C2250.5982 (3)0.50783 (17)0.71403 (8)0.0258 (5)
O2210.44489 (19)0.75123 (11)0.67765 (5)0.0194 (3)
O2220.73560 (19)0.72704 (11)0.69154 (5)0.0183 (3)
N230.9658 (2)0.56010 (12)0.57432 (6)0.0146 (3)
C231.1076 (3)0.58315 (16)0.60790 (8)0.0193 (4)
C241.0125 (3)0.53036 (15)0.53056 (7)0.0163 (4)
O241.17004 (19)0.51910 (12)0.52193 (6)0.0233 (3)
C250.8660 (2)0.51559 (15)0.49834 (7)0.0161 (4)
N250.9141 (2)0.48840 (13)0.45655 (6)0.0188 (4)
O250.7915 (2)0.47627 (12)0.42620 (5)0.0226 (3)
C260.6865 (2)0.52693 (14)0.51398 (7)0.0145 (4)
N260.5480 (2)0.51160 (13)0.48640 (6)0.0178 (3)
Ca20.78157 (5)0.86695 (3)0.820057 (12)0.01109 (7)
N310.7190 (2)1.22780 (13)0.95151 (6)0.0179 (3)
C320.8649 (3)1.21763 (15)0.92771 (7)0.0156 (4)
N320.8498 (2)1.19927 (13)0.88329 (6)0.0173 (3)
C3210.6784 (3)1.19319 (15)0.85847 (7)0.0167 (4)
C3220.6297 (3)1.08855 (15)0.84779 (7)0.0152 (4)
C3230.6916 (4)1.2510 (2)0.81299 (10)0.0227 (6)0.880 (6)
C3240.6972 (4)1.3575 (2)0.82467 (15)0.0390 (9)0.880 (6)
C3250.5386 (4)1.2272 (2)0.77956 (10)0.0295 (7)0.880 (6)
C32A0.643 (3)1.2612 (13)0.8275 (7)0.025 (4)0.120 (6)
C32B0.774 (3)1.2525 (14)0.7895 (6)0.024 (4)0.120 (6)
C32C0.648 (4)1.3622 (14)0.8473 (8)0.034 (5)0.120 (6)
O3210.74986 (19)1.03343 (11)0.83569 (5)0.0198 (3)
O3220.46720 (19)1.06669 (11)0.85089 (5)0.0214 (3)
N331.0354 (2)1.22739 (14)0.94638 (6)0.0175 (4)
C331.1919 (3)1.2184 (2)0.91774 (8)0.0317 (6)
C341.0645 (3)1.24323 (15)0.99284 (7)0.0162 (4)
O341.21688 (19)1.24885 (13)1.00899 (5)0.0237 (3)
C350.9070 (2)1.25140 (15)1.01965 (7)0.0156 (4)
N350.9398 (2)1.26735 (13)1.06417 (6)0.0173 (3)
O350.80618 (19)1.27491 (11)1.09026 (5)0.0200 (3)
C360.7353 (3)1.24353 (16)0.99640 (7)0.0170 (4)
N360.5903 (2)1.25141 (16)1.02009 (6)0.0235 (4)
N411.1027 (2)0.53570 (13)0.92233 (6)0.0158 (3)
C420.9573 (3)0.55970 (14)0.89859 (7)0.0147 (4)
N420.9723 (2)0.58970 (13)0.85558 (6)0.0143 (3)
C4211.1463 (2)0.60741 (14)0.83639 (7)0.0128 (4)
C4221.1431 (2)0.70584 (14)0.81311 (6)0.0117 (3)
C4231.1983 (3)0.52945 (16)0.80203 (8)0.0211 (4)
C4241.0787 (4)0.53032 (19)0.75909 (8)0.0311 (5)
C4251.2027 (3)0.43049 (17)0.82423 (10)0.0315 (6)
O4210.99987 (18)0.75030 (11)0.80987 (5)0.0158 (3)
O4221.28779 (17)0.73306 (11)0.79682 (5)0.0172 (3)
N430.7868 (2)0.55310 (13)0.91490 (6)0.0161 (3)
C430.6305 (3)0.58025 (17)0.88629 (7)0.0199 (4)
C440.7595 (3)0.52354 (15)0.95983 (7)0.0170 (4)
O440.60858 (19)0.51259 (13)0.97294 (5)0.0260 (4)
C450.9191 (2)0.50926 (15)0.98794 (7)0.0164 (4)
N450.8889 (2)0.49749 (14)1.03247 (6)0.0201 (4)
O451.0243 (2)0.49013 (13)1.05954 (5)0.0243 (3)
C461.0891 (2)0.51441 (15)0.96673 (7)0.0150 (4)
N461.2379 (2)0.49987 (14)0.99072 (6)0.0205 (4)
O10.1356 (2)0.81358 (13)0.71722 (5)0.0258 (4)
O20.4045 (2)0.98115 (12)0.71621 (5)0.0256 (3)
O30.53083 (19)0.95519 (12)0.62691 (5)0.0210 (3)
O40.02268 (19)0.81439 (11)0.62902 (5)0.0188 (3)
O50.70706 (19)0.82060 (11)0.89450 (5)0.0186 (3)
O60.46995 (18)0.90155 (11)0.80506 (5)0.0179 (3)
O71.05569 (18)0.92594 (11)0.85617 (5)0.0161 (3)
O80.80439 (18)0.89036 (10)0.74071 (4)0.0158 (3)
O90.64609 (18)0.71165 (11)0.79250 (5)0.0174 (3)
O100.75757 (18)1.39181 (12)0.43758 (5)0.0201 (3)
O110.4993 (2)0.95912 (12)0.93242 (5)0.0249 (3)
O121.1144 (2)1.12407 (13)0.81881 (6)0.0300 (4)
O1S0.503 (2)1.1815 (14)0.6986 (6)0.047 (7)*0.123 (8)
H120.32901.16740.63940.020*
H1210.01591.14560.61090.021*
H1230.15201.22020.67260.020*0.722 (7)
H12A0.09751.32540.61290.036*0.722 (7)
H12B0.07071.38290.65920.036*0.722 (7)
H12C0.09801.34700.62970.036*0.722 (7)
H12D0.00891.29980.72860.046*0.722 (7)
H12E0.05581.18810.72790.046*0.722 (7)
H12F0.19081.26370.70520.046*0.722 (7)
H1260.14541.24630.69260.020*0.278 (7)
H12G0.00511.32630.61500.037*0.278 (7)
H12H0.09941.36980.65850.037*0.278 (7)
H12I0.11081.38200.65320.037*0.278 (7)
H12J0.22551.20340.68820.037*0.278 (7)
H12K0.09991.18250.72980.037*0.278 (7)
H12L0.16161.28970.71940.037*0.278 (7)
H13A0.59021.12450.60710.030*
H13B0.71221.20500.58340.030*
H13C0.57871.23290.62460.030*
H16A0.06141.24860.49150.020*
H16B0.06601.27010.45160.020*
H220.84530.59740.64830.018*
H2210.49910.62850.61580.016*
H2230.37350.55090.67820.021*
H22A0.59640.41720.63390.033*
H22B0.41180.45520.61270.033*
H22C0.41540.39140.65790.033*
H22D0.53830.45600.72990.039*
H22E0.60370.56470.73350.039*
H22F0.71860.48770.70700.039*
H23A1.09450.64950.61800.029*
H23B1.22290.57520.59400.029*
H23C1.09990.54010.63410.029*
H26A0.44020.51740.49660.021*
H26B0.56350.49560.45790.021*
H320.94701.19040.86810.021*
H3210.58461.22220.87730.020*
H3230.80521.23350.79850.027*0.880 (6)
H32A0.73631.39380.79830.058*0.880 (6)
H32B0.78021.36800.85050.058*0.880 (6)
H32C0.57881.37900.83270.058*0.880 (6)
H32D0.55021.16100.76910.044*0.880 (6)
H32E0.54181.27060.75340.044*0.880 (6)
H32F0.42591.23490.79470.044*0.880 (6)
H32G0.52151.24950.81420.030*0.120 (6)
H32H0.76271.18930.77520.037*0.120 (6)
H32I0.89501.26050.80200.037*0.120 (6)
H32J0.74951.30220.76660.037*0.120 (6)
H32K0.64161.40900.82250.052*0.120 (6)
H32L0.75911.37120.86500.052*0.120 (6)
H32M0.54771.37120.86710.052*0.120 (6)
H33A1.21021.15090.91010.048*
H33B1.29671.24290.93440.048*
H33C1.17251.25540.88970.048*
H36A0.48551.24631.00640.028*
H36B0.59851.26171.04960.028*
H420.87600.59900.83850.017*
H4211.23730.60870.86180.015*
H4231.32120.54410.79250.025*
H42A0.95700.51500.76710.047*
H42B1.12080.48260.73750.047*
H42C1.08160.59390.74510.047*
H42D1.08260.41210.83240.047*
H42E1.27940.43230.85170.047*
H42F1.24890.38360.80280.047*
H43A0.62690.65000.88290.030*
H43B0.52260.55840.90080.030*
H43C0.63840.55040.85630.030*
H46A1.34060.50430.97750.025*
H46B1.23420.48581.01980.025*
H1A0.21210.79580.73730.031*
H1B0.05010.84060.73030.031*
H2A0.30971.01170.72130.031*
H2B0.44550.95850.74120.031*
H3A0.59500.93570.60560.025*
H3B0.59710.96820.65000.025*
H4A0.08520.79310.65030.023*
H4B0.08950.84260.60950.023*
H5A0.63380.85710.90730.022*
H5B0.79170.80820.91330.022*
H6A0.44540.95060.82070.021*
H6B0.39140.85910.80900.021*
H7A1.02040.96060.87790.019*
H7B1.12460.88300.86700.019*
H8A0.76100.84400.72530.019*
H8B0.79740.94140.72500.019*
H9A0.52070.71070.79380.021*
H9B0.68690.71840.76250.021*
H10A0.69831.35170.45600.024*
H10B0.80631.43630.45480.024*
H11A0.45970.99090.90790.030*
H11B0.41670.96890.95280.030*
H12M1.05241.07020.82080.036*
H12N1.22881.10940.82190.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.00854 (15)0.01470 (19)0.01428 (17)0.00022 (14)0.00090 (13)0.00014 (14)
N110.0109 (7)0.0170 (9)0.0191 (8)0.0019 (6)0.0000 (6)0.0032 (6)
C120.0083 (8)0.0122 (9)0.0204 (10)0.0004 (7)0.0002 (7)0.0009 (7)
N120.0113 (8)0.0189 (9)0.0205 (9)0.0021 (7)0.0019 (7)0.0050 (7)
C1210.0143 (9)0.0175 (10)0.0211 (10)0.0015 (8)0.0057 (8)0.0059 (8)
C1220.0195 (9)0.0133 (9)0.0152 (9)0.0015 (8)0.0048 (8)0.0001 (7)
C1230.0097 (16)0.0172 (15)0.0236 (16)0.0050 (13)0.0015 (14)0.0041 (12)
C1240.023 (3)0.0150 (19)0.033 (3)0.0015 (18)0.0007 (19)0.0029 (18)
C1250.041 (2)0.0236 (17)0.0283 (18)0.0066 (15)0.0097 (15)0.0041 (13)
C1260.009 (3)0.019 (3)0.022 (4)0.007 (3)0.002 (3)0.001 (3)
C1270.028 (5)0.022 (4)0.024 (5)0.003 (4)0.003 (4)0.001 (3)
C1280.025 (3)0.025 (4)0.023 (3)0.003 (3)0.004 (2)0.003 (3)
O1210.0212 (7)0.0169 (8)0.0250 (8)0.0064 (6)0.0030 (6)0.0011 (6)
O1220.0162 (7)0.0239 (8)0.0295 (8)0.0046 (6)0.0045 (6)0.0113 (6)
N130.0070 (7)0.0177 (9)0.0215 (8)0.0001 (6)0.0022 (6)0.0023 (6)
C130.0101 (9)0.0245 (11)0.0267 (11)0.0014 (8)0.0075 (8)0.0021 (8)
C140.0096 (8)0.0140 (9)0.0242 (10)0.0005 (7)0.0005 (7)0.0016 (7)
O140.0081 (6)0.0273 (9)0.0295 (8)0.0028 (6)0.0012 (6)0.0033 (7)
C150.0086 (8)0.0144 (9)0.0210 (10)0.0022 (7)0.0008 (7)0.0021 (7)
N150.0155 (8)0.0166 (9)0.0214 (9)0.0001 (7)0.0016 (7)0.0030 (7)
O150.0162 (7)0.0227 (8)0.0201 (7)0.0008 (6)0.0002 (6)0.0053 (6)
C160.0092 (8)0.0123 (9)0.0200 (9)0.0010 (7)0.0002 (7)0.0013 (7)
N160.0103 (7)0.0197 (9)0.0190 (8)0.0021 (6)0.0007 (6)0.0059 (7)
N210.0095 (7)0.0164 (8)0.0198 (8)0.0013 (6)0.0024 (6)0.0044 (6)
N220.0062 (7)0.0188 (9)0.0197 (9)0.0012 (6)0.0052 (6)0.0051 (6)
C220.0092 (8)0.0128 (9)0.0228 (10)0.0008 (7)0.0007 (7)0.0022 (7)
C2210.0078 (8)0.0150 (9)0.0181 (9)0.0011 (7)0.0030 (7)0.0015 (7)
C2220.0134 (8)0.0143 (9)0.0144 (9)0.0001 (7)0.0011 (7)0.0014 (7)
C2230.0121 (8)0.0140 (9)0.0255 (11)0.0021 (7)0.0005 (8)0.0003 (8)
C2240.0179 (10)0.0164 (10)0.0311 (12)0.0036 (8)0.0035 (9)0.0032 (8)
C2250.0298 (12)0.0216 (11)0.0255 (11)0.0036 (9)0.0078 (9)0.0032 (9)
O2210.0160 (7)0.0192 (8)0.0230 (7)0.0063 (6)0.0008 (6)0.0010 (6)
O2220.0141 (6)0.0195 (8)0.0212 (7)0.0030 (6)0.0012 (6)0.0051 (6)
N230.0068 (7)0.0150 (8)0.0218 (9)0.0003 (6)0.0021 (6)0.0015 (6)
C230.0072 (8)0.0224 (11)0.0280 (11)0.0009 (8)0.0055 (8)0.0001 (8)
C240.0114 (8)0.0134 (9)0.0242 (10)0.0017 (7)0.0012 (8)0.0011 (7)
O240.0087 (6)0.0271 (9)0.0343 (9)0.0022 (6)0.0039 (6)0.0044 (7)
C250.0105 (8)0.0135 (9)0.0244 (10)0.0017 (7)0.0023 (8)0.0039 (7)
N250.0170 (8)0.0164 (9)0.0230 (9)0.0005 (7)0.0022 (7)0.0038 (7)
O250.0209 (7)0.0248 (8)0.0221 (8)0.0007 (6)0.0006 (6)0.0067 (6)
C260.0104 (8)0.0127 (9)0.0202 (10)0.0003 (7)0.0002 (7)0.0022 (7)
N260.0117 (7)0.0226 (9)0.0191 (8)0.0008 (7)0.0002 (6)0.0066 (7)
Ca20.00868 (15)0.01179 (18)0.01270 (16)0.00082 (13)0.00140 (13)0.00084 (13)
N310.0104 (7)0.0215 (9)0.0215 (9)0.0005 (6)0.0036 (6)0.0047 (7)
C320.0112 (8)0.0151 (10)0.0200 (10)0.0020 (7)0.0050 (7)0.0017 (7)
N320.0093 (7)0.0205 (9)0.0218 (9)0.0023 (6)0.0026 (6)0.0047 (7)
C3210.0120 (9)0.0157 (10)0.0221 (10)0.0006 (7)0.0062 (8)0.0051 (7)
C3220.0147 (9)0.0155 (9)0.0153 (9)0.0007 (7)0.0036 (7)0.0006 (7)
C3230.0184 (13)0.0229 (14)0.0261 (15)0.0040 (10)0.0100 (11)0.0089 (11)
C3240.0301 (16)0.0192 (15)0.066 (2)0.0074 (12)0.0155 (16)0.0082 (15)
C3250.0282 (14)0.0287 (15)0.0310 (15)0.0049 (11)0.0115 (11)0.0098 (11)
C32A0.023 (6)0.027 (6)0.025 (6)0.000 (5)0.001 (4)0.003 (4)
C32B0.028 (6)0.027 (6)0.019 (5)0.001 (4)0.003 (4)0.004 (4)
C32C0.039 (7)0.029 (6)0.035 (6)0.003 (4)0.000 (5)0.001 (4)
O3210.0147 (7)0.0168 (7)0.0276 (8)0.0024 (6)0.0029 (6)0.0043 (6)
O3220.0129 (7)0.0215 (8)0.0297 (8)0.0004 (6)0.0003 (6)0.0008 (6)
N330.0070 (7)0.0260 (10)0.0196 (8)0.0002 (7)0.0007 (6)0.0025 (7)
C330.0098 (9)0.0624 (18)0.0231 (11)0.0021 (10)0.0016 (8)0.0071 (11)
C340.0112 (8)0.0151 (9)0.0222 (10)0.0003 (7)0.0033 (7)0.0034 (8)
O340.0089 (6)0.0367 (9)0.0254 (8)0.0017 (6)0.0032 (6)0.0052 (7)
C350.0089 (8)0.0170 (10)0.0204 (10)0.0003 (7)0.0038 (7)0.0020 (7)
N350.0109 (7)0.0209 (9)0.0199 (8)0.0002 (7)0.0028 (6)0.0016 (7)
O350.0137 (7)0.0256 (8)0.0208 (7)0.0001 (6)0.0003 (6)0.0026 (6)
C360.0096 (8)0.0200 (10)0.0210 (10)0.0013 (7)0.0048 (7)0.0033 (8)
N360.0088 (7)0.0408 (12)0.0207 (9)0.0005 (8)0.0041 (7)0.0072 (8)
N410.0100 (7)0.0200 (9)0.0175 (8)0.0004 (6)0.0007 (6)0.0057 (6)
C420.0121 (8)0.0137 (9)0.0183 (9)0.0022 (7)0.0013 (7)0.0026 (7)
N420.0069 (7)0.0194 (9)0.0165 (8)0.0008 (6)0.0015 (6)0.0034 (6)
C4210.0075 (8)0.0147 (9)0.0163 (9)0.0004 (7)0.0001 (7)0.0021 (7)
C4220.0099 (8)0.0138 (9)0.0113 (8)0.0003 (7)0.0027 (7)0.0011 (7)
C4230.0166 (9)0.0166 (10)0.0303 (11)0.0021 (8)0.0063 (9)0.0014 (8)
C4240.0382 (13)0.0263 (13)0.0285 (12)0.0019 (11)0.0027 (11)0.0096 (10)
C4250.0261 (12)0.0169 (12)0.0516 (16)0.0050 (9)0.0052 (11)0.0011 (10)
O4210.0121 (6)0.0172 (7)0.0179 (7)0.0036 (5)0.0010 (5)0.0010 (5)
O4220.0089 (6)0.0207 (8)0.0220 (7)0.0019 (5)0.0003 (5)0.0047 (6)
N430.0076 (7)0.0205 (9)0.0202 (8)0.0002 (6)0.0009 (6)0.0056 (7)
C430.0098 (9)0.0265 (11)0.0232 (11)0.0008 (8)0.0014 (8)0.0095 (8)
C440.0111 (8)0.0200 (10)0.0199 (10)0.0016 (8)0.0009 (7)0.0052 (8)
O440.0110 (7)0.0409 (10)0.0263 (8)0.0016 (7)0.0033 (6)0.0116 (7)
C450.0098 (8)0.0198 (10)0.0197 (10)0.0016 (7)0.0014 (7)0.0055 (7)
N450.0168 (8)0.0234 (10)0.0202 (9)0.0004 (7)0.0007 (7)0.0074 (7)
O450.0184 (7)0.0344 (10)0.0199 (8)0.0001 (7)0.0023 (6)0.0084 (7)
C460.0106 (8)0.0159 (10)0.0187 (10)0.0004 (7)0.0016 (7)0.0034 (7)
N460.0091 (7)0.0317 (11)0.0208 (9)0.0017 (7)0.0004 (6)0.0095 (8)
O10.0136 (7)0.0445 (10)0.0194 (8)0.0077 (7)0.0023 (6)0.0124 (7)
O20.0222 (8)0.0314 (9)0.0227 (8)0.0024 (7)0.0062 (6)0.0032 (7)
O30.0135 (7)0.0272 (8)0.0223 (8)0.0037 (6)0.0004 (6)0.0019 (6)
O40.0137 (7)0.0230 (8)0.0198 (7)0.0025 (6)0.0007 (6)0.0024 (6)
O50.0156 (7)0.0238 (8)0.0161 (7)0.0024 (6)0.0024 (6)0.0006 (6)
O60.0118 (6)0.0169 (7)0.0249 (7)0.0021 (5)0.0011 (5)0.0037 (6)
O70.0121 (6)0.0186 (7)0.0175 (7)0.0018 (5)0.0016 (5)0.0033 (5)
O80.0184 (6)0.0140 (7)0.0150 (6)0.0018 (6)0.0008 (5)0.0033 (5)
O90.0124 (6)0.0192 (7)0.0204 (7)0.0017 (6)0.0002 (5)0.0024 (6)
O100.0123 (6)0.0266 (8)0.0212 (7)0.0048 (6)0.0000 (5)0.0014 (6)
O110.0198 (7)0.0339 (9)0.0213 (8)0.0052 (7)0.0056 (6)0.0005 (6)
O120.0188 (8)0.0315 (10)0.0398 (10)0.0024 (7)0.0023 (7)0.0036 (8)
Geometric parameters (Å, º) top
Ca1—O12.363 (2)N32—H320.88
Ca1—O22.512 (2)C321—C32A1.34 (2)
Ca1—O32.399 (12)C321—C3221.538 (3)
Ca1—O42.455 (2)C321—C3231.569 (4)
Ca1—O1212.403 (2)C321—H3211.00
Ca1—O2212.403 (2)C322—O3211.251 (2)
Ca1—O15i2.510 (2)C322—O3221.272 (2)
Ca1—O25ii2.685 (2)C323—C3241.527 (4)
N11—C121.333 (2)C323—C3251.530 (4)
N11—C161.340 (3)C323—H3231.00
C12—N121.330 (3)C324—H32A0.98
C12—N131.388 (2)C324—H32B0.98
N12—C1211.476 (3)C324—H32C0.98
N12—H120.88C325—H32D0.98
C121—C1231.533 (4)C325—H32E0.98
C121—C1221.543 (3)C325—H32F0.98
C121—C1261.612 (7)C32A—C32B1.523 (10)
C121—H1211.00C32A—C32C1.527 (10)
C122—O1211.252 (3)C32A—H32G1.00
C122—O1221.253 (2)C32B—H32H0.98
C123—C1251.520 (5)C32B—H32I0.98
C123—C1241.523 (8)C32B—H32J0.98
C123—H1231.00C32C—H32K0.98
C124—H12A0.98C32C—H32L0.98
C124—H12B0.98C32C—H32M0.98
C124—H12C0.98N33—C341.395 (3)
C125—H12D0.98N33—C331.479 (3)
C125—H12E0.98C33—H33A0.98
C125—H12F0.98C33—H33B0.98
C126—C1281.543 (13)C33—H33C0.98
C126—C1271.58 (2)C34—O341.234 (2)
C126—H1261.00C34—C351.453 (3)
C127—H12G0.98C35—N351.344 (3)
C127—H12H0.98C35—C361.452 (3)
C127—H12I0.98N35—O351.291 (2)
C128—H12J0.98C36—N361.321 (3)
C128—H12K0.98N36—H36A0.88
C128—H12L0.98N36—H36B0.88
N13—C141.393 (3)N41—C421.326 (3)
N13—C131.475 (2)N41—C461.347 (3)
C13—H13A0.98C42—N421.341 (2)
C13—H13B0.98C42—N431.392 (2)
C13—H13C0.98N42—C4211.468 (2)
C14—O141.241 (2)N42—H420.88
C14—C151.460 (3)C421—C4221.536 (3)
C15—N151.351 (3)C421—C4231.545 (3)
C15—C161.446 (3)C421—H4211.00
N15—O151.280 (2)C422—O4211.249 (2)
C16—N161.326 (2)C422—O4221.266 (2)
N16—H16A0.88C423—C4251.529 (3)
N16—H16B0.88C423—C4241.530 (4)
N21—C221.325 (3)C423—H4231.00
N21—C261.344 (3)C424—H42A0.98
N22—C221.340 (3)C424—H42B0.98
N22—C2211.472 (2)C424—H42C0.98
N22—H220.88C425—H42D0.98
C22—N231.385 (2)C425—H42E0.98
C221—C2221.547 (3)C425—H42F0.98
C221—C2231.547 (3)N43—C441.406 (3)
C221—H2211.00N43—C431.478 (3)
C222—O2211.246 (2)C43—H43A0.98
C222—O2221.273 (2)C43—H43B0.98
C223—C2251.526 (3)C43—H43C0.98
C223—C2241.530 (3)C44—O441.225 (2)
C223—H2231.00C44—C451.455 (3)
C224—H22A0.98C45—N451.347 (3)
C224—H22B0.98C45—C461.447 (2)
C224—H22C0.98N45—O451.281 (2)
C225—H22D0.98C46—N461.324 (3)
C225—H22E0.98N46—H46A0.88
C225—H22F0.98N46—H46B0.88
N23—C241.408 (3)O1—H1A0.85
N23—C231.470 (3)O1—H1B0.85
C23—H23A0.98O2—H2A0.85
C23—H23B0.98O2—H2B0.85
C23—H23C0.98O3—H3A0.85
C24—O241.235 (2)O3—H3B0.85
C24—C251.449 (3)O4—H4A0.85
C25—N251.347 (3)O4—H4B0.85
C25—C261.455 (3)O5—H5A0.85
N25—O251.278 (2)O5—H5B0.85
C26—N261.321 (3)O6—H6A0.85
N26—H26A0.88O6—H6B0.85
N26—H26B0.88O7—H7A0.85
Ca2—O4212.3445 (2)O7—H7B0.85
Ca2—O3212.385 (2)O8—H8A0.85
Ca2—O52.369 (2)O8—H8B0.85
Ca2—O62.430 (2)O9—H9A0.95
Ca2—O72.441 (2)O9—H9B0.95
Ca2—O82.369 (2)O10—H10A0.89
Ca2—O92.522 (2)O10—H10B0.89
N31—C321.332 (3)O11—H11A0.89
N31—C361.341 (3)O11—H11B0.89
C32—N321.333 (3)O12—H12M0.89
C32—N331.391 (2)O12—H12N0.89
N32—C3211.469 (3)
O1—Ca1—O3142.99 (6)O421—Ca2—O772.53 (5)
O1—Ca1—O12185.37 (6)O8—Ca2—O7107.17 (5)
O3—Ca1—O121102.02 (6)O5—Ca2—O785.01 (5)
O1—Ca1—O22171.46 (5)O321—Ca2—O771.08 (5)
O3—Ca1—O22186.53 (5)O6—Ca2—O7144.66 (5)
O121—Ca1—O221149.87 (5)O421—Ca2—O968.95 (5)
O1—Ca1—O471.71 (6)O8—Ca2—O980.99 (5)
O3—Ca1—O4144.58 (5)O5—Ca2—O987.48 (5)
O121—Ca1—O484.08 (5)O321—Ca2—O9149.20 (5)
O221—Ca1—O4105.68 (6)O6—Ca2—O974.44 (5)
O1—Ca1—O15i119.89 (6)O7—Ca2—O9139.51 (5)
O3—Ca1—O15i81.34 (5)O421—Ca2—H7A87.7
O121—Ca1—O15i132.90 (5)O8—Ca2—H7A118.3
O221—Ca1—O15i76.64 (5)O5—Ca2—H7A74.4
O4—Ca1—O15i69.88 (5)O321—Ca2—H7A59.2
O1—Ca1—O278.94 (6)O6—Ca2—H7A128.8
O3—Ca1—O270.80 (5)O7—Ca2—H7A17.4
O121—Ca1—O268.07 (5)O9—Ca2—H7A148.7
O221—Ca1—O288.29 (6)O421—Ca2—H9B64.4
O4—Ca1—O2140.90 (5)O8—Ca2—H9B61.6
O15i—Ca1—O2149.08 (5)O5—Ca2—H9B107.3
O1—Ca1—O25ii146.87 (5)O321—Ca2—H9B145.7
O3—Ca1—O25ii68.37 (5)O6—Ca2—H9B78.9
O121—Ca1—O25ii74.45 (5)O7—Ca2—H9B136.1
O221—Ca1—O25ii134.73 (5)O9—Ca2—H9B20.1
O4—Ca1—O25ii80.17 (5)H7A—Ca2—H9B152.1
O15i—Ca1—O25ii63.17 (5)C32—N31—C36118.88 (17)
O2—Ca1—O25ii115.64 (6)N31—C32—N32119.26 (18)
O1—Ca1—H2A74.2N31—C32—N33123.61 (18)
O3—Ca1—H2A82.7N32—C32—N33117.11 (17)
O121—Ca1—H2A50.7C32—N32—C321123.03 (16)
O221—Ca1—H2A103.1C32—N32—H32118.5
O4—Ca1—H2A124.6C321—N32—H32118.5
O15i—Ca1—H2A164.1C32A—C321—N32116.8 (9)
O2—Ca1—H2A18.3C32A—C321—C322119.7 (9)
O25ii—Ca1—H2A109.9N32—C321—C322110.97 (17)
O1—Ca1—H3B126.5N32—C321—C323108.38 (17)
O3—Ca1—H3B16.9C322—C321—C323109.66 (18)
O121—Ca1—H3B99.8C32A—C321—H32187.7
O221—Ca1—H3B80.1N32—C321—H321109.3
O4—Ca1—H3B161.4C322—C321—H321109.3
O15i—Ca1—H3B95.0C323—C321—H321109.3
O2—Ca1—H3B55.4O321—C322—O322125.7 (2)
O25ii—Ca1—H3B83.4O321—C322—C321118.22 (18)
H2A—Ca1—H3B69.5O322—C322—C321116.03 (17)
C12—N11—C16118.86 (17)C324—C323—C325111.8 (2)
N12—C12—N11118.74 (18)C324—C323—C321108.2 (3)
N12—C12—N13117.56 (16)C325—C323—C321111.7 (2)
N11—C12—N13123.68 (18)C324—C323—H323108.4
C12—N12—C121122.74 (16)C325—C323—H323108.4
C12—N12—H12118.6C321—C323—H323108.4
C121—N12—H12118.6C321—C32A—C32B108.9 (15)
N12—C121—C123115.1 (2)C321—C32A—C32C113.3 (17)
N12—C121—C122108.49 (16)C32B—C32A—C32C110.1 (12)
C123—C121—C122110.7 (2)C321—C32A—H32G108.2
N12—C121—C12699.9 (4)C32B—C32A—H32G108.2
C122—C121—C126106.7 (4)C32C—C32A—H32G108.2
N12—C121—H121107.4C32A—C32B—H32H109.5
C123—C121—H121107.4C32A—C32B—H32I109.5
C122—C121—H121107.4H32H—C32B—H32I109.5
C126—C121—H121125.9C32A—C32B—H32J109.5
O121—C122—O122126.9 (2)H32H—C32B—H32J109.5
O121—C122—C121115.97 (17)H32I—C32B—H32J109.5
O122—C122—C121117.13 (18)C32A—C32C—H32K109.5
C125—C123—C124111.1 (4)C32A—C32C—H32L109.5
C125—C123—C121110.4 (3)H32K—C32C—H32L109.5
C124—C123—C121111.8 (4)C32A—C32C—H32M109.5
C125—C123—H123107.8H32K—C32C—H32M109.5
C124—C123—H123107.8H32L—C32C—H32M109.5
C121—C123—H123107.8C322—O321—Ca2137.21 (14)
C128—C126—C127107.2 (10)C32—N33—C34121.21 (16)
C128—C126—C121111.6 (7)C32—N33—C33120.92 (17)
C127—C126—C121109.2 (9)C34—N33—C33117.84 (17)
C128—C126—H126109.6N33—C33—H33A109.5
C127—C126—H126109.6N33—C33—H33B109.5
C121—C126—H126109.6H33A—C33—H33B109.5
C126—C127—H12G109.5N33—C33—H33C109.5
C126—C127—H12H109.5H33A—C33—H33C109.5
H12G—C127—H12H109.5H33B—C33—H33C109.5
C126—C127—H12I109.5O34—C34—N33120.26 (17)
H12G—C127—H12I109.5O34—C34—C35123.78 (18)
H12H—C127—H12I109.5N33—C34—C35115.96 (17)
C126—C128—H12J109.5N35—C35—C36127.32 (17)
C126—C128—H12K109.5N35—C35—C34114.42 (17)
H12J—C128—H12K109.5C36—C35—C34118.25 (18)
C126—C128—H12L109.5O35—N35—C35117.99 (17)
H12J—C128—H12L109.5N36—C36—N31118.75 (18)
H12K—C128—H12L109.5N36—C36—C35119.26 (18)
C122—O121—Ca1145.47 (15)N31—C36—C35121.99 (17)
C12—N13—C14121.30 (16)C36—N36—H36A120.0
C12—N13—C13120.47 (17)C36—N36—H36B120.0
C14—N13—C13118.23 (17)H36A—N36—H36B120.0
N13—C13—H13A109.5C42—N41—C46118.62 (16)
N13—C13—H13B109.5N41—C42—N42118.86 (17)
H13A—C13—H13B109.5N41—C42—N43124.20 (17)
N13—C13—H13C109.5N42—C42—N43116.91 (18)
H13A—C13—H13C109.5C42—N42—C421121.25 (17)
H13B—C13—H13C109.5C42—N42—H42119.4
O14—C14—N13120.82 (17)C421—N42—H42119.4
O14—C14—C15123.59 (19)N42—C421—C422108.69 (15)
N13—C14—C15115.59 (17)N42—C421—C423112.45 (16)
N15—C15—C16127.25 (17)C422—C421—C423109.90 (16)
N15—C15—C14114.38 (17)N42—C421—H421108.6
C16—C15—C14118.32 (17)C422—C421—H421108.6
O15—N15—C15116.42 (17)C423—C421—H421108.6
N15—O15—Ca1iii134.56 (12)O421—C422—O422125.33 (18)
N16—C16—N11116.92 (18)O421—C422—C421118.75 (16)
N16—C16—C15121.11 (18)O422—C422—C421115.84 (16)
N11—C16—C15121.95 (16)C425—C423—C424111.4 (2)
C16—N16—H16A120.0C425—C423—C421111.15 (18)
C16—N16—H16B120.0C424—C423—C421112.25 (18)
H16A—N16—H16B120.0C425—C423—H423107.3
C22—N21—C26118.49 (16)C424—C423—H423107.3
C22—N22—C221122.60 (17)C421—C423—H423107.3
C22—N22—H22118.7C423—C424—H42A109.5
C221—N22—H22118.7C423—C424—H42B109.5
N21—C22—N22118.29 (17)H42A—C424—H42B109.5
N21—C22—N23124.62 (18)C423—C424—H42C109.5
N22—C22—N23117.09 (18)H42A—C424—H42C109.5
N22—C221—C222108.25 (16)H42B—C424—H42C109.5
N22—C221—C223112.21 (16)C423—C425—H42D109.5
C222—C221—C223110.55 (16)C423—C425—H42E109.5
N22—C221—H221108.6H42D—C425—H42E109.5
C222—C221—H221108.6C423—C425—H42F109.5
C223—C221—H221108.6H42D—C425—H42F109.5
O221—C222—O222126.33 (19)H42E—C425—H42F109.5
O221—C222—C221116.80 (18)C422—O421—Ca2161.34 (14)
O222—C222—C221116.81 (16)C42—N43—C44120.55 (17)
C225—C223—C224109.07 (18)C42—N43—C43121.21 (16)
C225—C223—C221113.31 (18)C44—N43—C43118.20 (15)
C224—C223—C221112.00 (17)N43—C43—H43A109.5
C225—C223—H223107.4N43—C43—H43B109.5
C224—C223—H223107.4H43A—C43—H43B109.5
C221—C223—H223107.4N43—C43—H43C109.5
C223—C224—H22A109.5H43A—C43—H43C109.5
C223—C224—H22B109.5H43B—C43—H43C109.5
H22A—C224—H22B109.5O44—C44—N43119.90 (19)
C223—C224—H22C109.5O44—C44—C45124.56 (19)
H22A—C224—H22C109.5N43—C44—C45115.54 (16)
H22B—C224—H22C109.5N45—C45—C46127.24 (19)
C223—C225—H22D109.5N45—C45—C44114.02 (16)
C223—C225—H22E109.5C46—C45—C44118.63 (17)
H22D—C225—H22E109.5O45—N45—C45117.26 (17)
C223—C225—H22F109.5N46—C46—N41117.45 (16)
H22D—C225—H22F109.5N46—C46—C45120.85 (18)
H22E—C225—H22F109.5N41—C46—C45121.69 (18)
C222—O221—Ca1146.51 (13)C46—N46—H46A120.0
C22—N23—C24120.73 (17)C46—N46—H46B120.0
C22—N23—C23120.52 (17)H46A—N46—H46B120.0
C24—N23—C23118.76 (16)Ca1—O1—H1A112.9
N23—C23—H23A109.5Ca1—O1—H1B120.9
N23—C23—H23B109.5H1A—O1—H1B109.0
H23A—C23—H23B109.5Ca1—O2—H2A93.6
N23—C23—H23C109.5Ca1—O2—H2B125.0
H23A—C23—H23C109.5H2A—O2—H2B108.6
H23B—C23—H23C109.5Ca1—O3—H3A127.5
O24—C24—N23119.75 (19)Ca1—O3—H3B108.2
O24—C24—C25124.65 (19)H3A—O3—H3B108.8
N23—C24—C25115.60 (16)Ca1—O4—H4A115.6
N25—C25—C24114.50 (17)Ca1—O4—H4B120.7
N25—C25—C26126.88 (19)H4A—O4—H4B109.2
C24—C25—C26118.55 (18)Ca2—O5—H5A115.0
O25—N25—C25117.68 (17)Ca2—O5—H5B117.5
N25—O25—Ca1iv139.42 (12)H5A—O5—H5B108.7
N26—C26—N21117.03 (16)Ca2—O6—H6A106.8
N26—C26—C25121.09 (18)Ca2—O6—H6B120.9
N21—C26—C25121.87 (18)H6A—O6—H6B108.9
C26—N26—H26A120.0Ca2—O7—H7A103.7
C26—N26—H26B120.0Ca2—O7—H7B115.2
H26A—N26—H26B120.0H7A—O7—H7B108.8
O421—Ca2—O884.07 (5)Ca2—O8—H8A112.4
O421—Ca2—O596.70 (5)Ca2—O8—H8B130.2
O8—Ca2—O5167.35 (5)H8A—O8—H8B109.5
O421—Ca2—O321141.08 (5)Ca2—O9—H9A113.2
O8—Ca2—O32193.80 (5)Ca2—O9—H9B94.2
O5—Ca2—O32193.45 (5)H9A—O9—H9B113.1
O421—Ca2—O6142.79 (5)H10A—O10—H10B107.6
O8—Ca2—O683.90 (5)H11A—O11—H11B104.1
O5—Ca2—O688.00 (5)H12M—O12—H12N108.1
O321—Ca2—O674.83 (5)
C16—N11—C12—N12177.47 (18)N25—C25—C26—N21177.5 (2)
C16—N11—C12—N134.1 (3)C24—C25—C26—N210.4 (3)
N11—C12—N12—C1214.5 (3)C36—N31—C32—N32178.1 (2)
N13—C12—N12—C121176.95 (18)C36—N31—C32—N333.5 (3)
C12—N12—C121—C123100.8 (3)N31—C32—N32—C3212.4 (3)
C12—N12—C121—C122134.6 (2)N33—C32—N32—C321176.04 (18)
C12—N12—C121—C126113.9 (4)C32—N32—C321—C32A113.2 (8)
N12—C121—C122—O121159.54 (18)C32—N32—C321—C322104.9 (2)
C123—C121—C122—O12173.3 (3)C32—N32—C321—C323134.7 (2)
C126—C121—C122—O12193.6 (4)C32A—C321—C322—O321100.6 (9)
N12—C121—C122—O12222.6 (3)N32—C321—C322—O32140.2 (3)
C123—C121—C122—O122104.6 (3)C323—C321—C322—O32179.5 (2)
C126—C121—C122—O12284.3 (4)C32A—C321—C322—O32277.4 (9)
N12—C121—C123—C12568.6 (3)N32—C321—C322—O322141.83 (18)
C122—C121—C123—C12554.9 (3)C323—C321—C322—O32298.5 (2)
C126—C121—C123—C12526.8 (12)C32A—C321—C323—C32445 (3)
N12—C121—C123—C12455.7 (4)N32—C321—C323—C32471.6 (3)
C122—C121—C123—C124179.2 (3)C322—C321—C323—C324167.1 (2)
C126—C121—C123—C12497.5 (13)C32A—C321—C323—C32578 (3)
N12—C121—C126—C128166.9 (6)N32—C321—C323—C325165.0 (2)
C123—C121—C126—C12850.9 (11)C322—C321—C323—C32543.7 (3)
C122—C121—C126—C12854.0 (7)N32—C321—C32A—C32B64.7 (15)
N12—C121—C126—C12774.8 (9)C322—C321—C32A—C32B73.8 (15)
C123—C121—C126—C12767.4 (13)C323—C321—C32A—C32B6.7 (16)
C122—C121—C126—C127172.3 (8)N32—C321—C32A—C32C58.1 (16)
O122—C122—O121—Ca169.1 (3)C322—C321—C32A—C32C163.3 (12)
C121—C122—O121—Ca1113.3 (2)C323—C321—C32A—C32C130 (3)
O1—Ca1—O121—C12286.8 (2)O322—C322—O321—Ca28.4 (3)
O3—Ca1—O121—C122129.9 (2)C321—C322—O321—Ca2173.85 (14)
O221—Ca1—O121—C122126.1 (2)O421—Ca2—O321—C322165.54 (18)
O4—Ca1—O121—C12214.8 (2)O8—Ca2—O321—C322109.2 (2)
O15i—Ca1—O121—C12240.6 (3)O5—Ca2—O321—C32260.4 (2)
O2—Ca1—O121—C122166.8 (3)O6—Ca2—O321—C32226.6 (2)
O25ii—Ca1—O121—C12266.6 (2)O7—Ca2—O321—C322143.9 (2)
N12—C12—N13—C14178.28 (19)O9—Ca2—O321—C32230.4 (3)
N11—C12—N13—C140.2 (3)N31—C32—N33—C343.9 (3)
N12—C12—N13—C131.3 (3)N32—C32—N33—C34177.7 (2)
N11—C12—N13—C13179.74 (19)N31—C32—N33—C33177.9 (2)
C12—N13—C14—O14176.20 (19)N32—C32—N33—C330.5 (3)
C13—N13—C14—O143.4 (3)C32—N33—C34—O34177.8 (2)
C12—N13—C14—C154.6 (3)C33—N33—C34—O340.4 (3)
C13—N13—C14—C15175.85 (18)C32—N33—C34—C351.7 (3)
O14—C14—C15—N151.7 (3)C33—N33—C34—C35179.9 (2)
N13—C14—C15—N15177.46 (18)O34—C34—C35—N351.0 (3)
O14—C14—C15—C16175.9 (2)N33—C34—C35—N35179.52 (19)
N13—C14—C15—C164.9 (3)O34—C34—C35—C36179.9 (2)
C16—C15—N15—O154.3 (3)N33—C34—C35—C360.6 (3)
C14—C15—N15—O15178.33 (17)C36—C35—N35—O351.6 (3)
C15—N15—O15—Ca1iii152.99 (15)C34—C35—N35—O35179.62 (18)
C12—N11—C16—N16178.30 (18)C32—N31—C36—N36178.5 (2)
C12—N11—C16—C153.5 (3)C32—N31—C36—C351.1 (3)
N15—C15—C16—N160.2 (3)N35—C35—C36—N360.8 (3)
C14—C15—C16—N16177.11 (19)C34—C35—C36—N36179.5 (2)
N15—C15—C16—N11178.3 (2)N35—C35—C36—N31179.7 (2)
C14—C15—C16—N111.0 (3)C34—C35—C36—N310.9 (3)
C26—N21—C22—N22179.06 (19)C46—N41—C42—N42173.75 (19)
C26—N21—C22—N231.8 (3)C46—N41—C42—N438.3 (3)
C221—N22—C22—N218.0 (3)N41—C42—N42—C4217.5 (3)
C221—N22—C22—N23172.81 (17)N43—C42—N42—C421174.45 (17)
C22—N22—C221—C222135.89 (19)C42—N42—C421—C422131.22 (19)
C22—N22—C221—C223101.8 (2)C42—N42—C421—C423106.9 (2)
N22—C221—C222—O221159.74 (17)N42—C421—C422—O4216.4 (2)
C223—C221—C222—O22177.0 (2)C423—C421—C422—O421117.03 (19)
N22—C221—C222—O22222.6 (2)N42—C421—C422—O422176.65 (17)
C223—C221—C222—O222100.6 (2)C423—C421—C422—O42259.9 (2)
N22—C221—C223—C22562.8 (2)N42—C421—C423—C42558.8 (2)
C222—C221—C223—C22558.1 (2)C422—C421—C423—C425180.00 (18)
N22—C221—C223—C22461.1 (2)N42—C421—C423—C42466.7 (2)
C222—C221—C223—C224177.97 (16)C422—C421—C423—C42454.5 (2)
O222—C222—O221—Ca183.9 (3)O422—C422—O421—Ca270.1 (5)
C221—C222—O221—Ca198.7 (3)C421—C422—O421—Ca2113.3 (4)
O1—Ca1—O221—C222172.4 (3)O8—Ca2—O421—C422118.5 (4)
O3—Ca1—O221—C22222.6 (3)O5—Ca2—O421—C42274.2 (4)
O121—Ca1—O221—C222130.7 (2)O321—Ca2—O421—C42229.8 (4)
O4—Ca1—O221—C222123.6 (3)O6—Ca2—O421—C422169.8 (4)
O15i—Ca1—O221—C22259.3 (3)O7—Ca2—O421—C4228.4 (4)
O2—Ca1—O221—C22293.4 (3)O9—Ca2—O421—C422158.9 (4)
O25ii—Ca1—O221—C22232.0 (3)N41—C42—N43—C443.0 (3)
N21—C22—N23—C241.4 (3)N42—C42—N43—C44179.10 (19)
N22—C22—N23—C24177.71 (19)N41—C42—N43—C43179.4 (2)
N21—C22—N23—C23178.2 (2)N42—C42—N43—C431.4 (3)
N22—C22—N23—C232.7 (3)C42—N43—C44—O44175.7 (2)
C22—N23—C24—O24176.39 (19)C43—N43—C44—O446.6 (3)
C23—N23—C24—O244.0 (3)C42—N43—C44—C455.1 (3)
C22—N23—C24—C253.9 (3)C43—N43—C44—C45172.65 (19)
C23—N23—C24—C25175.71 (18)O44—C44—C45—N4510.2 (3)
O24—C24—C25—N250.5 (3)N43—C44—C45—N45168.99 (19)
N23—C24—C25—N25179.16 (18)O44—C44—C45—C46173.2 (2)
O24—C24—C25—C26176.9 (2)N43—C44—C45—C467.6 (3)
N23—C24—C25—C263.4 (3)C46—C45—N45—O450.2 (3)
C24—C25—N25—O25178.44 (17)C44—C45—N45—O45176.05 (19)
C26—C25—N25—O254.4 (3)C42—N41—C46—N46173.53 (19)
C25—N25—O25—Ca1iv158.44 (16)C42—N41—C46—C455.3 (3)
C22—N21—C26—N26179.27 (19)N45—C45—C46—N465.4 (4)
C22—N21—C26—C252.2 (3)C44—C45—C46—N46178.5 (2)
N25—C25—C26—N260.9 (3)N45—C45—C46—N41173.4 (2)
C24—C25—C26—N26178.01 (19)C44—C45—C46—N412.7 (3)
Symmetry codes: (i) x, y1/2, z+1; (ii) x+1, y+1/2, z+1; (iii) x, y+1/2, z+1; (iv) x+1, y1/2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N16—H16A···O14v0.882.132.997 (2)170
N16—H16B···O150.881.982.620 (2)128
N16—H16B···O4iii0.882.563.383 (2)156
N26—H26A···O24vi0.882.203.073 (2)175
N26—H26B···O250.882.002.640 (2)128
N26—H26B···O3iv0.882.633.459 (2)157
N32—H32···O120.882.162.989 (2)156
N36—H36A···O34vi0.882.032.830 (2)150
N36—H36B···O350.881.952.611 (2)131
N46—H46A···O44v0.882.042.871 (2)158
N46—H46B···O450.882.002.632 (2)128
N46—H46B···O11vii0.882.453.016 (2)123
O1—H1A···O422vi0.852.032.811 (2)154
O1—H1B···O8vi0.852.022.828 (2)160
O2—H2A···O1210.852.202.752 (2)122
O2—H2B···O60.852.042.869 (2)164
O3—H3A···O10i0.851.902.743 (2)174
O3—H3B···O122v0.851.992.777 (2)153
O4—H4A···O222vi0.852.062.902 (2)168
O4—H4B···O10viii0.851.902.750 (2)173
O5—H5A···O110.851.912.750 (2)169
O5—H5B···N35vii0.852.192.991 (2)157
O5—H5B···O34vii0.852.433.048 (2)130
O6—H6A···O3220.851.852.673 (2)161
O6—H6B···O422vi0.851.962.734 (2)152
O7—H7A···O45ix0.851.932.723 (2)155
O7—H7B···O35vii0.852.022.815 (2)155
O7—H7B···N35vii0.852.653.225 (2)126
O8—H8A···O2220.851.922.743 (2)163
O8—H8B···O122v0.851.842.680 (2)168
O9—H9A···O422vi0.951.792.730 (2)169
O9—H9B···O2220.952.133.074 (2)171
O9—H9B···O80.952.653.178 (2)116
O10—H10A···O140.892.112.947 (2)156
O10—H10A···N150.892.373.022 (2)130
O10—H10B···N25x0.892.242.894 (2)130
O10—H10B···O24x0.892.303.115 (2)152
O11—H11A···O3220.891.992.834 (2)159
O11—H11B···O44xi0.892.283.019 (2)140
O11—H11B···N45xi0.892.403.185 (2)148
O12—H12M···O70.892.273.017 (2)142
O12—H12M···O3210.892.403.086 (2)135
O12—H12N···O322v0.892.062.912 (2)161
Symmetry codes: (i) x, y1/2, z+1; (iii) x, y+1/2, z+1; (iv) x+1, y1/2, z+1; (v) x+1, y, z; (vi) x1, y, z; (vii) x+2, y1/2, z+2; (viii) x1, y1/2, z+1; (ix) x+2, y+1/2, z+2; (x) x2, y+1, z; (xi) x+1, y+1/2, z+2.
(IX) # Ba(py-met)2·7H2O top
Crystal data top
C20H36BaN10O12S2·3(H2O)Dx = 1.646 Mg m3
Mr = 864.11Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P43Cell parameters from 7394 reflections
Hall symbol: P 4cwθ = 3.0–27.5°
a = 21.6978 (2) ŵ = 1.34 mm1
c = 7.4057 (1) ÅT = 120 K
V = 3486.56 (7) Å3Plate, pink
Z = 40.60 × 0.03 × 0.02 mm
F(000) = 1760
Data collection top
Kappa-CCD
diffractometer
7394 independent reflections
Radiation source: fine-focus sealed X-ray tube7035 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.072
ϕ scans, and ω scans with κ offsetsθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 2823
Tmin = 0.501, Tmax = 0.974k = 2826
21371 measured reflectionsl = 97
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.089 w = 1/[σ2(Fo2) + (0.0289P)2 + 4.0203P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
7394 reflectionsΔρmax = 0.74 e Å3
478 parametersΔρmin = 0.71 e Å3
46 restraintsAbsolute structure: Flack (1983), 3077 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.022 (13)
Crystal data top
C20H36BaN10O12S2·3(H2O)Z = 4
Mr = 864.11Mo Kα radiation
Tetragonal, P43µ = 1.34 mm1
a = 21.6978 (2) ÅT = 120 K
c = 7.4057 (1) Å0.60 × 0.03 × 0.02 mm
V = 3486.56 (7) Å3
Data collection top
Kappa-CCD
diffractometer
7394 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
7035 reflections with I > 2σ(I)
Tmin = 0.501, Tmax = 0.974Rint = 0.072
21371 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.089Δρmax = 0.74 e Å3
S = 1.05Δρmin = 0.71 e Å3
7394 reflectionsAbsolute structure: Flack (1983), 3077 Friedel pairs
478 parametersAbsolute structure parameter: 0.022 (13)
46 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ba10.957253 (10)0.462796 (9)0.21367 (4)0.01623 (6)
N110.81697 (14)0.19326 (14)0.4534 (5)0.0180 (6)
C120.85107 (19)0.20849 (18)0.3112 (6)0.0191 (8)
N120.90398 (16)0.23818 (16)0.3398 (5)0.0217 (7)
C1210.9245 (2)0.25853 (19)0.5156 (6)0.0236 (9)
C1220.94256 (17)0.32663 (17)0.5134 (5)0.0140 (7)
O110.96619 (13)0.34813 (12)0.3717 (4)0.0207 (6)
O120.93432 (13)0.35532 (13)0.6595 (4)0.0211 (6)
C1230.9803 (3)0.22122 (18)0.5826 (9)0.0450 (15)
C12A0.9821 (5)0.1512 (3)0.568 (3)0.042 (3)0.39
S1A1.04813 (18)0.10993 (17)0.5036 (8)0.0556 (13)0.39
C12D1.0326 (12)0.1124 (11)0.2713 (12)0.085 (7)0.39
C12B0.9669 (5)0.1528 (4)0.605 (5)0.042 (3)0.27
S1B1.0321 (3)0.1090 (3)0.6610 (9)0.0402 (15)0.27
C12E1.0365 (10)0.1320 (9)0.8879 (14)0.043 (5)0.27
C12C0.9587 (9)0.1554 (5)0.616 (4)0.042 (3)0.34
S1C1.0062 (3)0.1086 (3)0.7504 (13)0.079 (3)0.34
C12F0.9591 (11)0.0444 (9)0.788 (6)0.130 (13)0.34
N130.83557 (17)0.19498 (17)0.1346 (5)0.0231 (8)
C1310.8732 (2)0.2181 (3)0.0147 (7)0.0378 (12)
C140.7834 (2)0.15979 (19)0.0938 (6)0.0243 (9)
O140.77333 (15)0.14408 (16)0.0624 (4)0.0321 (8)
C150.74418 (19)0.14520 (18)0.2475 (6)0.0205 (9)
N150.69166 (15)0.11603 (15)0.2017 (6)0.0213 (7)
O150.65552 (13)0.10002 (15)0.3312 (4)0.0267 (7)
C160.76370 (18)0.16220 (18)0.4246 (6)0.0194 (9)
N160.73105 (17)0.14872 (18)0.5679 (5)0.0257 (8)
N210.69870 (15)0.67143 (15)0.2500 (5)0.0196 (7)
C220.72001 (17)0.64154 (18)0.1063 (6)0.0269 (8)
N220.74292 (16)0.58507 (15)0.1249 (5)0.0194 (7)
C2210.74280 (18)0.55149 (19)0.2962 (6)0.0198 (8)
C2220.80928 (19)0.53628 (19)0.3560 (6)0.0200 (8)
O210.84853 (12)0.52709 (13)0.2390 (4)0.0238 (6)
O220.81792 (14)0.53351 (14)0.5266 (4)0.0234 (6)
C2230.7085 (2)0.4896 (2)0.2734 (7)0.0252 (9)
C2240.6403 (2)0.4970 (2)0.2298 (9)0.0367 (12)
S20.60579 (6)0.42868 (6)0.1335 (2)0.0450 (4)
C2250.6341 (3)0.4343 (3)0.0931 (9)0.0510 (16)
N230.72092 (15)0.66618 (15)0.0655 (5)0.0181 (7)
C2310.7461 (2)0.6308 (2)0.2175 (6)0.0258 (9)
C240.69186 (19)0.72212 (18)0.1035 (6)0.0191 (8)
O240.69041 (16)0.74174 (14)0.2600 (4)0.0280 (7)
C250.66617 (18)0.75384 (18)0.0503 (6)0.0170 (8)
N250.63596 (15)0.80634 (15)0.0074 (5)0.0200 (7)
O250.60948 (13)0.83649 (13)0.1321 (4)0.0226 (6)
C260.67291 (16)0.72692 (17)0.2261 (6)0.0179 (7)
N260.65346 (17)0.75685 (17)0.3697 (5)0.0244 (8)
O10.93625 (13)0.54798 (11)0.0689 (4)0.0184 (6)
O21.06933 (13)0.52130 (12)0.0827 (4)0.0190 (6)
O31.01385 (12)0.41948 (12)0.1166 (4)0.0188 (6)
O40.87330 (12)0.40261 (12)0.0322 (5)0.0223 (6)
O50.7905 (2)0.49769 (17)0.8651 (5)0.0559 (12)
O61.10685 (14)0.36521 (14)0.0764 (5)0.0272 (7)
O71.01064 (16)0.26337 (17)0.1120 (6)0.0429 (9)
H120.92780.24580.24620.026*
H1210.89000.25290.60340.028*
H1AA1.01690.23710.51780.054*0.39
H1AB0.98610.23150.71170.054*0.39
H1BA1.01460.22630.49580.054*0.27
H1BB0.99400.23810.70010.054*0.27
H1CA1.01340.22160.49070.054*0.34
H1CB0.99670.23940.69550.054*0.34
H12A0.94920.13950.48180.051*0.39
H12B0.96960.13490.68710.051*0.39
H12G1.06500.09030.20570.127*0.195
H12H1.03150.15540.23100.127*0.195
H12I0.99260.09290.24750.127*0.195
H12J0.99440.13550.25040.127*0.195
H12K1.02790.07030.22520.127*0.195
H12L1.06670.13280.20860.127*0.195
H12C0.94930.13680.49070.051*0.27
H12D0.93550.14740.70040.051*0.27
H12M1.06960.10920.94830.064*0.135
H12N0.99720.12340.94810.064*0.135
H12O1.04520.17630.89400.064*0.135
H12P1.00510.16340.91190.064*0.135
H12Q1.07750.14920.91220.064*0.135
H12R1.02950.09630.96630.064*0.135
H12E0.95350.13490.49790.051*0.34
H12F0.91760.15720.67390.051*0.34
H12S0.98090.01470.86470.195*0.17
H12T0.94900.02500.67220.195*0.17
H12U0.92110.05750.84820.195*0.17
H12V0.91980.05010.72540.195*0.17
H12Y0.95170.03980.91790.195*0.17
H12Z0.97960.00730.74190.195*0.17
H13A0.88020.26240.00090.057*
H13B0.85180.21080.12920.057*
H13C0.91290.19650.01580.057*
H16A0.74410.15980.67560.031*
H16B0.69610.12860.55650.031*
H220.75890.56700.02950.023*
H2210.72200.57680.39120.024*
H22A0.72840.46580.17540.030*
H22B0.71270.46550.38630.030*
H22C0.63530.53160.14410.044*
H22D0.61800.50780.34200.044*
H22E0.61670.47100.15100.076*
H22F0.62200.39760.16110.076*
H22G0.67920.43750.09120.076*
H23A0.78910.61990.19200.039*
H23B0.74420.65580.32760.039*
H23C0.72190.59310.23430.039*
H26A0.65760.74030.47750.029*
H26B0.63630.79340.35790.029*
H11W0.90160.53410.09900.022*
H12W0.92720.58180.02040.022*
H21W1.07290.55850.11280.023*
H22W1.10410.50460.07140.023*
H31W1.04190.39830.06920.023*
H32W0.99280.39710.18560.023*
H41W0.85060.38410.04180.027*
H42W0.88390.37750.11290.027*
H51W0.81590.47080.89880.067*
H52W0.79300.50210.75260.067*
H61W1.13120.39520.08430.033*
H62W1.10860.35110.18200.033*
H71W1.01230.29500.17710.052*
H72W1.04670.24980.12330.052*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.02159 (11)0.01554 (10)0.01155 (11)0.00029 (8)0.00143 (9)0.00103 (9)
N110.0230 (15)0.0178 (14)0.0132 (17)0.0080 (11)0.0011 (15)0.0015 (14)
C120.024 (2)0.0162 (18)0.017 (2)0.0076 (15)0.0014 (16)0.0006 (15)
N120.0250 (17)0.0230 (17)0.0171 (19)0.0125 (14)0.0009 (15)0.0022 (14)
C1210.035 (2)0.0185 (19)0.017 (2)0.0065 (17)0.0050 (17)0.0007 (15)
C1220.0141 (16)0.0160 (17)0.0119 (19)0.0013 (13)0.0048 (13)0.0007 (13)
O110.0209 (14)0.0176 (13)0.0237 (17)0.0021 (11)0.0035 (12)0.0003 (12)
O120.0270 (15)0.0197 (14)0.0165 (16)0.0018 (11)0.0028 (11)0.0023 (11)
C1230.070 (4)0.021 (2)0.044 (4)0.004 (2)0.034 (3)0.001 (2)
C12A0.086 (9)0.016 (3)0.026 (7)0.010 (4)0.005 (6)0.006 (3)
S1A0.0432 (19)0.0331 (18)0.091 (4)0.0097 (15)0.022 (2)0.006 (2)
C12D0.105 (16)0.074 (13)0.074 (15)0.029 (12)0.010 (13)0.008 (11)
C12B0.086 (9)0.016 (3)0.026 (7)0.010 (4)0.005 (6)0.006 (3)
S1B0.048 (4)0.032 (3)0.041 (4)0.016 (3)0.014 (3)0.006 (2)
C12E0.047 (11)0.029 (9)0.052 (13)0.012 (8)0.017 (10)0.013 (9)
C12C0.086 (9)0.016 (3)0.026 (7)0.010 (4)0.005 (6)0.006 (3)
S1C0.061 (4)0.042 (3)0.134 (8)0.009 (3)0.053 (4)0.040 (4)
C12F0.12 (2)0.11 (2)0.16 (3)0.018 (19)0.05 (2)0.03 (2)
N130.0261 (18)0.0290 (19)0.0143 (18)0.0146 (15)0.0015 (15)0.0004 (15)
C1310.044 (3)0.058 (3)0.012 (2)0.027 (2)0.003 (2)0.001 (2)
C140.030 (2)0.023 (2)0.020 (2)0.0105 (17)0.0009 (18)0.0015 (17)
O140.0398 (18)0.0464 (19)0.0101 (16)0.0203 (15)0.0032 (14)0.0023 (14)
C150.0251 (19)0.0198 (18)0.017 (2)0.0040 (15)0.0002 (16)0.0009 (15)
N150.0220 (15)0.0224 (15)0.0195 (18)0.0040 (12)0.0009 (15)0.0000 (16)
O150.0223 (15)0.0363 (17)0.0214 (17)0.0129 (13)0.0051 (13)0.0075 (13)
C160.0233 (19)0.0195 (18)0.015 (2)0.0041 (15)0.0001 (15)0.0010 (15)
N160.0241 (18)0.039 (2)0.0141 (19)0.0127 (15)0.0035 (14)0.0025 (16)
N210.0244 (16)0.0211 (16)0.0131 (19)0.0050 (13)0.0004 (13)0.0001 (13)
C220.0244 (18)0.032 (2)0.024 (2)0.0017 (15)0.0032 (16)0.0028 (17)
N220.0270 (18)0.0210 (17)0.0103 (18)0.0084 (13)0.0039 (14)0.0035 (14)
C2210.0203 (19)0.022 (2)0.017 (2)0.0061 (15)0.0042 (16)0.0028 (16)
C2220.023 (2)0.0183 (19)0.019 (2)0.0042 (15)0.0026 (17)0.0064 (16)
O210.0214 (13)0.0313 (15)0.0185 (17)0.0051 (11)0.0023 (12)0.0038 (13)
O220.0265 (15)0.0262 (15)0.0176 (16)0.0031 (12)0.0008 (12)0.0036 (12)
C2230.026 (2)0.024 (2)0.026 (2)0.0039 (17)0.0014 (17)0.0070 (17)
C2240.026 (2)0.036 (2)0.047 (3)0.0016 (18)0.001 (2)0.011 (3)
S20.0360 (7)0.0393 (7)0.0596 (10)0.0125 (5)0.0058 (6)0.0117 (7)
C2250.056 (4)0.048 (3)0.049 (4)0.001 (3)0.008 (3)0.005 (3)
N230.0225 (16)0.0195 (15)0.0122 (19)0.0063 (12)0.0015 (13)0.0039 (13)
C2310.033 (2)0.029 (2)0.015 (2)0.0074 (18)0.0032 (18)0.0005 (17)
C240.0233 (19)0.0191 (18)0.015 (2)0.0038 (15)0.0005 (15)0.0027 (15)
O240.0447 (18)0.0251 (14)0.0143 (17)0.0108 (13)0.0016 (14)0.0018 (13)
C250.0212 (19)0.0153 (18)0.014 (2)0.0003 (14)0.0016 (15)0.0001 (15)
N250.0228 (16)0.0140 (15)0.023 (2)0.0014 (12)0.0015 (14)0.0025 (13)
O250.0275 (15)0.0169 (13)0.0232 (16)0.0033 (11)0.0020 (13)0.0034 (12)
C260.0151 (16)0.0231 (17)0.015 (2)0.0005 (13)0.0023 (16)0.0001 (18)
N260.034 (2)0.0280 (19)0.0110 (18)0.0114 (15)0.0005 (15)0.0013 (15)
O10.0231 (13)0.0137 (12)0.0182 (17)0.0007 (10)0.0020 (12)0.0016 (10)
O20.0213 (14)0.0163 (13)0.0195 (16)0.0042 (11)0.0053 (11)0.0033 (11)
O30.0159 (13)0.0195 (13)0.0212 (16)0.0002 (10)0.0039 (11)0.0048 (12)
O40.0227 (13)0.0248 (13)0.0193 (15)0.0044 (10)0.0035 (14)0.0010 (14)
O50.106 (4)0.045 (2)0.017 (2)0.042 (2)0.009 (2)0.0061 (17)
O60.0332 (17)0.0257 (15)0.0228 (17)0.0006 (13)0.0080 (14)0.0024 (13)
O70.0344 (19)0.047 (2)0.047 (3)0.0118 (16)0.0079 (17)0.0118 (19)
Geometric parameters (Å, º) top
Ba1—O112.756 (3)N13—C141.399 (5)
Ba1—O212.747 (3)N13—C1311.463 (6)
Ba1—O2i2.815 (3)C131—H13A0.98
Ba1—O1i2.826 (3)C131—H13B0.98
Ba1—O12.829 (3)C131—H13C0.98
Ba1—O22.909 (3)C14—O141.226 (6)
Ba1—O32.894 (3)C14—C151.456 (6)
Ba1—O42.888 (3)C15—N151.347 (5)
Ba1—O3i2.915 (3)C15—C161.427 (6)
Ba1—O25ii3.299 (3)N15—O151.286 (5)
Ba1—Ba1i4.4451 (2)C16—N161.309 (5)
Ba1—Ba1iii4.4451 (2)N16—H16A0.88
N11—C121.329 (5)N16—H16B0.88
N11—C161.355 (5)N21—C221.329 (5)
C12—N121.333 (5)N21—C261.339 (5)
C12—N131.382 (5)C22—N221.329 (5)
N12—C1211.446 (6)C22—N231.380 (5)
N12—H120.88N22—C2211.463 (5)
C121—C1221.529 (5)N22—H220.88
C121—C1231.538 (7)C221—C2221.545 (6)
C121—H1211.00C221—C2231.545 (6)
C122—O111.258 (5)C221—H2211.00
C122—O121.261 (5)C222—O211.231 (5)
C123—C12B1.523 (5)C222—O221.279 (6)
C123—C12A1.523 (5)C223—C2241.523 (6)
C123—C12C1.524 (5)C223—H22A0.99
C123—H1AA0.99C223—H22B0.99
C123—H1AB0.99C224—S21.807 (5)
C123—H1BA0.99C224—H22C0.99
C123—H1BB0.99C224—H22D0.99
C123—H1CA0.99S2—C2251.791 (7)
C123—H1CB0.99C225—H22E0.98
C12A—S1A1.756 (5)C225—H22F0.98
C12A—H12A0.99C225—H22G0.98
C12A—H12B0.99N23—C241.396 (5)
S1A—C12D1.753 (5)N23—C2311.468 (5)
C12D—H12G0.98C231—H23A0.98
C12D—H12H0.98C231—H23B0.98
C12D—H12I0.98C231—H23C0.98
C12D—H12J0.98C24—O241.235 (5)
C12D—H12K0.98C24—C251.442 (6)
C12D—H12L0.98C25—N251.352 (5)
C12B—S1B1.754 (5)C25—C261.435 (6)
C12B—H12C0.99N25—O251.269 (5)
C12B—H12D0.99O25—Ba1iv3.299 (3)
S1B—C12E1.756 (5)C26—N261.316 (6)
C12E—H12M0.98N26—H26A0.88
C12E—H12N0.98N26—H26B0.88
C12E—H12O0.98O1—H11W0.84
C12E—H12P0.98O1—H12W0.84
C12E—H12Q0.98O2—H21W0.84
C12E—H12R0.98O2—H22W0.84
C12C—S1C1.754 (5)O3—H31W0.84
C12C—H12E0.99O3—H32W0.84
C12C—H12F0.99O4—H41W0.84
S1C—C12F1.750 (5)O4—H42W0.84
C12F—H12S0.98O5—H51W0.84
C12F—H12T0.98O5—H52W0.84
C12F—H12U0.98O6—H61W0.84
C12F—H12V0.98O6—H62W0.84
C12F—H12Y0.98O7—H71W0.84
C12F—H12Z0.98O7—H72W0.84
O21—Ba1—O11119.33 (8)H12M—C12E—H12Q56.3
O21—Ba1—O2i72.27 (9)H12N—C12E—H12Q141.1
O11—Ba1—O2i73.31 (8)H12O—C12E—H12Q56.3
O21—Ba1—O1i134.84 (9)H12P—C12E—H12Q109.5
O11—Ba1—O1i68.03 (8)S1B—C12E—H12R109.5
O2i—Ba1—O1i67.93 (8)H12M—C12E—H12R56.3
O21—Ba1—O165.19 (9)H12N—C12E—H12R56.3
O11—Ba1—O1156.23 (8)H12O—C12E—H12R141.1
O2i—Ba1—O1127.24 (8)H12P—C12E—H12R109.5
O1i—Ba1—O1127.39 (4)H12Q—C12E—H12R109.5
O21—Ba1—O474.40 (9)C123—C12C—S1C117.0 (6)
O11—Ba1—O484.49 (8)C123—C12C—H12E108.0
O2i—Ba1—O4122.58 (8)S1C—C12C—H12E108.0
O1i—Ba1—O4146.89 (7)C123—C12C—H12F108.0
O1—Ba1—O474.18 (8)S1C—C12C—H12F108.0
O21—Ba1—O3125.96 (9)H12E—C12C—H12F107.3
O11—Ba1—O392.05 (8)C12F—S1C—C12C102.0 (11)
O2i—Ba1—O3161.36 (8)S1C—C12F—H12S109.5
O1i—Ba1—O396.19 (8)S1C—C12F—H12T109.5
O1—Ba1—O369.85 (8)H12S—C12F—H12T109.5
O4—Ba1—O365.66 (8)S1C—C12F—H12U109.5
O21—Ba1—O2121.26 (8)H12S—C12F—H12U109.5
O11—Ba1—O2118.46 (8)H12T—C12F—H12U109.5
O2i—Ba1—O2116.19 (7)S1C—C12F—H12V109.5
O1i—Ba1—O262.78 (8)H12S—C12F—H12V141.1
O1—Ba1—O266.61 (8)H12T—C12F—H12V56.3
O4—Ba1—O2120.96 (8)H12U—C12F—H12V56.3
O3—Ba1—O260.35 (8)S1C—C12F—H12Y109.5
O21—Ba1—O3i73.16 (8)H12S—C12F—H12Y56.3
O11—Ba1—O3i126.35 (9)H12T—C12F—H12Y141.1
O2i—Ba1—O3i61.17 (8)H12U—C12F—H12Y56.3
O1i—Ba1—O3i69.57 (7)H12V—C12F—H12Y109.5
O1—Ba1—O3i77.36 (8)S1C—C12F—H12Z109.5
O4—Ba1—O3i143.50 (8)H12S—C12F—H12Z56.3
O3—Ba1—O3i123.91 (6)H12T—C12F—H12Z56.3
O2—Ba1—O3i65.27 (8)H12U—C12F—H12Z141.1
O21—Ba1—O25ii62.19 (8)H12V—C12F—H12Z109.5
O11—Ba1—O25ii57.74 (8)H12Y—C12F—H12Z109.5
O2i—Ba1—O25ii61.85 (8)C12—N13—C14121.1 (3)
O1i—Ba1—O25ii113.24 (8)C12—N13—C131120.5 (3)
O1—Ba1—O25ii117.54 (8)C14—N13—C131118.4 (4)
O4—Ba1—O25ii61.47 (8)N13—C131—H13A109.5
O3—Ba1—O25ii120.16 (8)N13—C131—H13B109.5
O2—Ba1—O25ii175.84 (8)H13A—C131—H13B109.5
O3i—Ba1—O25ii115.10 (8)N13—C131—H13C109.5
C12—N11—C16118.3 (4)H13A—C131—H13C109.5
N11—C12—N12118.3 (4)H13B—C131—H13C109.5
N11—C12—N13124.2 (3)O14—C14—N13120.0 (4)
N12—C12—N13117.5 (4)O14—C14—C15125.0 (4)
C12—N12—C121123.8 (4)N13—C14—C15115.0 (4)
C12—N12—H12118.1N15—C15—C16127.2 (4)
C121—N12—H12118.1N15—C15—C14113.5 (4)
N12—C121—C122111.4 (3)C16—C15—C14119.3 (4)
N12—C121—C123111.9 (4)O15—N15—C15117.1 (4)
C122—C121—C123108.1 (3)N16—C16—N11116.4 (4)
N12—C121—H121108.5N16—C16—C15121.8 (4)
C122—C121—H121108.5N11—C16—C15121.8 (4)
C123—C121—H121108.5C16—N16—H16A120.0
O11—C122—O12126.2 (3)C16—N16—H16B120.0
O11—C122—C121118.2 (4)H16A—N16—H16B120.0
O12—C122—C121115.6 (3)C22—N21—C26118.6 (4)
C122—O11—Ba1131.3 (2)N21—C22—N22119.8 (4)
C12B—C123—C121113.4 (5)N21—C22—N23123.6 (3)
C12A—C123—C121121.4 (7)N22—C22—N23116.6 (4)
C12C—C123—C121107.7 (6)C22—N22—C221123.3 (3)
C12B—C123—H1AA123.1C22—N22—H22118.4
C12A—C123—H1AA107.0C221—N22—H22118.4
C12C—C123—H1AA130.7N22—C221—C222110.7 (3)
C121—C123—H1AA107.0N22—C221—C223109.8 (3)
C12B—C123—H1AB98.1C222—C221—C223107.2 (3)
C12A—C123—H1AB107.0N22—C221—H221109.7
C12C—C123—H1AB95.3C222—C221—H221109.7
C121—C123—H1AB107.0C223—C221—H221109.7
H1AA—C123—H1AB106.7O21—C222—O22125.9 (4)
C12B—C123—H1BA108.9O21—C222—C221118.6 (4)
C12A—C123—H1BA92.6O22—C222—C221115.5 (4)
C12C—C123—H1BA116.3C222—O21—Ba1136.4 (3)
C121—C123—H1BA108.9C224—C223—C221113.6 (3)
H1AB—C123—H1BA120.4C224—C223—H22A108.9
C12B—C123—H1BB108.9C221—C223—H22A108.9
C12A—C123—H1BB115.2C224—C223—H22B108.9
C12C—C123—H1BB107.2C221—C223—H22B108.9
C121—C123—H1BB108.9H22A—C223—H22B107.7
H1AA—C123—H1BB93.3C223—C224—S2113.6 (3)
H1BA—C123—H1BB107.7C223—C224—H22C108.8
C12B—C123—H1CA102.9S2—C224—H22C108.8
C12A—C123—H1CA86.6C223—C224—H22D108.8
C12C—C123—H1CA110.2S2—C224—H22D108.8
C121—C123—H1CA110.2H22C—C224—H22D107.7
H1AB—C123—H1CA124.8C225—S2—C22499.9 (3)
H1BB—C123—H1CA112.6S2—C225—H22E109.5
C12B—C123—H1CB111.4S2—C225—H22F109.5
C12A—C123—H1CB116.7H22E—C225—H22F109.5
C12C—C123—H1CB110.2S2—C225—H22G109.5
C121—C123—H1CB110.2H22E—C225—H22G109.5
H1AA—C123—H1CB89.0H22F—C225—H22G109.5
H1BA—C123—H1CB103.5C22—N23—C24121.1 (3)
H1CA—C123—H1CB108.5C22—N23—C231120.6 (3)
C123—C12A—S1A123.3 (6)C24—N23—C231117.9 (3)
C123—C12A—H12A106.5N23—C231—H23A109.5
S1A—C12A—H12A106.5N23—C231—H23B109.5
C123—C12A—H12B106.5H23A—C231—H23B109.5
S1A—C12A—H12B106.5N23—C231—H23C109.5
H12A—C12A—H12B106.5H23A—C231—H23C109.5
C12D—S1A—C12A95.3 (11)H23B—C231—H23C109.5
S1A—C12D—H12G109.5O24—C24—N23120.0 (4)
S1A—C12D—H12H109.5O24—C24—C25124.5 (4)
H12G—C12D—H12H109.5N23—C24—C25115.5 (4)
S1A—C12D—H12I109.5N25—C25—C26127.3 (4)
H12G—C12D—H12I109.5N25—C25—C24113.9 (4)
H12H—C12D—H12I109.5C26—C25—C24118.9 (3)
S1A—C12D—H12J109.5O25—N25—C25118.9 (4)
H12G—C12D—H12J141.1N25—O25—Ba1iv110.5 (2)
H12H—C12D—H12J56.3N26—C26—N21118.1 (4)
H12I—C12D—H12J56.3N26—C26—C25120.0 (3)
S1A—C12D—H12K109.5N21—C26—C25121.9 (4)
H12G—C12D—H12K56.3C26—N26—H26A120.0
H12H—C12D—H12K141.1C26—N26—H26B120.0
H12I—C12D—H12K56.3H26A—N26—H26B120.0
H12J—C12D—H12K109.5Ba1iii—O1—Ba1103.64 (9)
S1A—C12D—H12L109.5Ba1iii—O1—H11W123.4
H12G—C12D—H12L56.3Ba1—O1—H11W96.1
H12H—C12D—H12L56.3Ba1iii—O1—H12W120.4
H12I—C12D—H12L141.1Ba1—O1—H12W107.0
H12J—C12D—H12L109.5H11W—O1—H12W102.6
H12K—C12D—H12L109.5Ba1iii—O2—Ba1101.88 (9)
C123—C12B—S1B113.5 (6)Ba1iii—O2—H21W99.1
C123—C12B—H12C108.9Ba1—O2—H21W114.1
S1B—C12B—H12C108.9Ba1iii—O2—H22W98.0
C123—C12B—H12D108.9Ba1—O2—H22W126.5
S1B—C12B—H12D108.9H21W—O2—H22W110.9
H12C—C12B—H12D107.7Ba1—O4—H41W100.1
C12B—S1B—C12E96.7 (15)Ba1—O4—H42W124.7
S1B—C12E—H12M109.5H41W—O4—H42W108.3
S1B—C12E—H12N109.5Ba1—O3—Ba1iii99.85 (8)
H12M—C12E—H12N109.5Ba1—O3—H31W97.6
S1B—C12E—H12O109.5Ba1iii—O3—H31W120.2
H12M—C12E—H12O109.5Ba1—O3—H32W118.1
H12N—C12E—H12O109.5Ba1iii—O3—H32W111.1
S1B—C12E—H12P109.5H31W—O3—H32W109.5
H12M—C12E—H12P141.1H51W—O5—H52W109.5
H12N—C12E—H12P56.3H61W—O6—H62W100.8
H12O—C12E—H12P56.3H71W—O7—H72W100.9
S1B—C12E—H12Q109.5
C16—N11—C12—N12178.9 (4)N22—C221—C222—O22149.5 (4)
C16—N11—C12—N130.4 (6)C223—C221—C222—O2290.7 (4)
N11—C12—N12—C1214.4 (6)O22—C222—O21—Ba124.8 (7)
N13—C12—N12—C121176.3 (4)C221—C222—O21—Ba1154.0 (3)
C12—N12—C121—C122128.6 (4)O11—Ba1—O21—C22240.2 (4)
C12—N12—C121—C123110.3 (5)O2i—Ba1—O21—C22218.1 (4)
N12—C121—C122—O1133.5 (5)O1i—Ba1—O21—C22247.1 (4)
C123—C121—C122—O1189.8 (5)O1—Ba1—O21—C222166.0 (4)
N12—C121—C122—O12149.4 (4)O4—Ba1—O21—C222114.5 (4)
C123—C121—C122—O1287.4 (5)O3—Ba1—O21—C222157.5 (4)
O12—C122—O11—Ba137.4 (6)O2—Ba1—O21—C222128.4 (4)
C121—C122—O11—Ba1145.8 (3)O3i—Ba1—O21—C22282.5 (4)
O21—Ba1—O11—C12234.1 (3)O25ii—Ba1—O21—C22248.9 (4)
O2i—Ba1—O11—C12223.7 (3)Ba1i—Ba1—O21—C22249.9 (4)
O1i—Ba1—O11—C12296.1 (3)Ba1iii—Ba1—O21—C222165.3 (4)
O1—Ba1—O11—C122128.7 (3)N22—C221—C223—C22464.6 (5)
O4—Ba1—O11—C122102.7 (3)C222—C221—C223—C224175.1 (4)
O3—Ba1—O11—C122168.0 (3)C221—C223—C224—S2161.3 (3)
O2—Ba1—O11—C122134.9 (3)C223—C224—S2—C22577.4 (5)
O3i—Ba1—O11—C12256.0 (3)N21—C22—N23—C248.3 (6)
O25ii—Ba1—O11—C12243.1 (3)N22—C22—N23—C24172.8 (4)
Ba1i—Ba1—O11—C12261.9 (3)N21—C22—N23—C231179.0 (4)
Ba1iii—Ba1—O11—C122179.6 (3)N22—C22—N23—C2310.0 (6)
N12—C121—C123—C12B61.4 (17)C22—N23—C24—O24176.2 (4)
C122—C121—C123—C12B175.6 (17)C231—N23—C24—O243.2 (6)
N12—C121—C123—C12A45.4 (10)C22—N23—C24—C255.1 (5)
C122—C121—C123—C12A168.4 (9)C231—N23—C24—C25178.0 (4)
N12—C121—C123—C12C66.9 (15)O24—C24—C25—N254.2 (6)
C122—C121—C123—C12C170.1 (14)N23—C24—C25—N25177.1 (3)
C12B—C123—C12A—S1A157 (6)O24—C24—C25—C26177.8 (4)
C12C—C123—C12A—S1A161 (3)N23—C24—C25—C260.9 (5)
C121—C123—C12A—S1A138.9 (12)C26—C25—N25—O250.6 (6)
C123—C12A—S1A—C12D88.9 (17)C24—C25—N25—O25177.2 (3)
C12A—C123—C12B—S1B52 (4)C25—N25—O25—Ba1iv177.6 (3)
C12C—C123—C12B—S1B142 (16)C22—N21—C26—N26178.2 (4)
C121—C123—C12B—S1B174.5 (15)C22—N21—C26—C251.8 (6)
C123—C12B—S1B—C12E75 (2)N25—C25—C26—N266.7 (6)
C12B—C123—C12C—S1C58 (12)C24—C25—C26—N26175.6 (4)
C12A—C123—C12C—S1C68 (3)N25—C25—C26—N21173.2 (4)
C121—C123—C12C—S1C162.8 (17)C24—C25—C26—N214.5 (6)
C123—C12C—S1C—C12F170 (2)O21—Ba1—O1—Ba1iii178.89 (12)
N11—C12—N13—C144.3 (7)O11—Ba1—O1—Ba1iii74.3 (2)
N12—C12—N13—C14175.0 (4)O2i—Ba1—O1—Ba1iii139.51 (8)
N11—C12—N13—C131174.8 (4)O1i—Ba1—O1—Ba1iii50.25 (13)
N12—C12—N13—C1315.9 (7)O4—Ba1—O1—Ba1iii101.30 (9)
C12—N13—C14—O14174.0 (4)O3—Ba1—O1—Ba1iii31.93 (8)
C131—N13—C14—O146.9 (7)O2—Ba1—O1—Ba1iii33.53 (8)
C12—N13—C14—C156.6 (6)O3i—Ba1—O1—Ba1iii101.81 (9)
C131—N13—C14—C15172.6 (4)O25ii—Ba1—O1—Ba1iii146.27 (8)
O14—C14—C15—N154.9 (6)Ba1i—Ba1—O1—Ba1iii93.85 (7)
N13—C14—C15—N15174.5 (4)O21—Ba1—O2—Ba1iii70.54 (12)
O14—C14—C15—C16175.1 (4)O11—Ba1—O2—Ba1iii120.71 (10)
N13—C14—C15—C165.5 (6)O2i—Ba1—O2—Ba1iii154.89 (11)
C16—C15—N15—O152.0 (6)O1i—Ba1—O2—Ba1iii161.48 (11)
C14—C15—N15—O15178.0 (3)O1—Ba1—O2—Ba1iii33.42 (8)
C12—N11—C16—N16179.2 (4)O4—Ba1—O2—Ba1iii19.30 (12)
C12—N11—C16—C150.7 (6)O3—Ba1—O2—Ba1iii45.87 (8)
N15—C15—C16—N161.9 (7)O3i—Ba1—O2—Ba1iii119.79 (10)
C14—C15—C16—N16178.1 (4)Ba1i—Ba1—O2—Ba1iii160.39 (8)
N15—C15—C16—N11177.9 (4)O21—Ba1—O3—Ba1iii65.45 (11)
C14—C15—C16—N112.0 (6)O11—Ba1—O3—Ba1iii165.39 (9)
C26—N21—C22—N22176.5 (4)O2i—Ba1—O3—Ba1iii127.9 (2)
C26—N21—C22—N234.6 (6)O1i—Ba1—O3—Ba1iii97.27 (8)
N21—C22—N22—C2213.8 (6)O1—Ba1—O3—Ba1iii30.38 (7)
N23—C22—N22—C221177.2 (4)O4—Ba1—O3—Ba1iii111.60 (10)
C22—N22—C221—C222119.2 (4)O2—Ba1—O3—Ba1iii43.50 (8)
C22—N22—C221—C223122.6 (4)O3i—Ba1—O3—Ba1iii27.77 (10)
N22—C221—C222—O2131.5 (5)O25ii—Ba1—O3—Ba1iii141.26 (7)
C223—C221—C222—O2188.2 (5)Ba1i—Ba1—O3—Ba1iii77.80 (9)
Symmetry codes: (i) x+2, y+1, z+1/2; (ii) y, x+1, z+1/4; (iii) x+2, y+1, z1/2; (iv) y+1, x, z1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N12—H12···O70.882.092.915 (5)156
N16—H16A···O14v0.882.072.890 (5)155
N16—H16B···O150.881.992.623 (5)128
N16—H16B···O6vi0.882.452.976 (5)119
N22—H22···O5vii0.882.052.891 (5)159
N26—H26A···O24v0.882.072.875 (5)152
N26—H26B···O250.882.002.644 (5)129
O1—H11W···O5vii0.842.553.379 (5)170
O1—H12W···O15iv0.841.862.702 (4)175
O1—H12W···N15iv0.842.573.321 (4)149
O2—H21W···O12iii0.841.912.738 (4)169
O2—H22W···O22iii0.841.912.752 (4)176
O3—H31W···O60.841.922.741 (4)167
O3—H32W···O12vii0.841.942.768 (4)171
O4—H41W···O25ii0.842.543.180 (5)134
O4—H41W···N25ii0.841.912.721 (5)161
O4—H42W···O12vii0.842.072.832 (4)151
O5—H51W···O4v0.842.002.842 (5)176
O5—H52W···O220.841.882.687 (5)160
O6—H61W···O22iii0.841.952.761 (4)163
O6—H62W···N15viii0.842.213.047 (6)176
O7—H71W···O110.842.102.832 (5)145
O7—H72W···O14viii0.842.223.055 (5)170
Symmetry codes: (ii) y, x+1, z+1/4; (iii) x+2, y+1, z1/2; (iv) y+1, x, z1/4; (v) x, y, z+1; (vi) y+1, x1, z+3/4; (vii) x, y, z1; (viii) y+1, x+1, z+1/4.

Experimental details

(I)(II)(III)(IV)
Crystal data
Chemical formulaC14H24CaN10O12·4(H2O)C14H26BaN10O13·H2OC18H28CaN10O12·4(H2O)C18H28N10O12Sr·4(H2O)
Mr636.58697.79688.65736.19
Crystal system, space groupTriclinic, P1Monoclinic, P21/cMonoclinic, C2Monoclinic, C2
Temperature (K)120120120120
a, b, c (Å)7.4540 (7), 7.6148 (11), 12.5939 (17)24.9613 (4), 6.9157 (1), 14.6427 (2)30.2259 (11), 6.4043 (2), 7.3667 (3)30.6420 (5), 6.4888 (1), 7.3733 (1)
α, β, γ (°)95.850 (6), 97.040 (8), 110.038 (8)90, 93.149 (1), 9090, 94.610 (2), 9090, 94.4319 (9), 90
V3)658.52 (14)2523.88 (6)1421.40 (9)1461.65 (4)
Z1422
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.331.660.321.94
Crystal size (mm)0.10 × 0.07 × 0.010.42 × 0.36 × 0.080.24 × 0.24 × 0.040.70 × 0.50 × 0.25
Data collection
DiffractometerKappa-CCD
diffractometer
Kappa-CCD
diffractometer
Kappa-CCD
diffractometer
Kappa-CCD
diffractometer
Absorption correctionMulti-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Tmin, Tmax0.963, 0.9980.548, 0.8810.867, 0.9900.331, 0.618
No. of measured, independent and
observed [I > 2σ(I)] reflections
5368, 2833, 1311 26202, 5709, 5255 9010, 3182, 2469 9899, 3314, 3291
Rint0.1030.0740.0730.062
(sin θ/λ)max1)0.6400.6490.6470.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.057, 0.150, 0.90 0.078, 0.208, 1.19 0.049, 0.096, 1.03 0.028, 0.069, 1.04
No. of reflections2833573931823314
No. of parameters188354206209
No. of restraints0011
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0574P)2]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0001P)2 + 84.2219P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0339P)2]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.030P)2 + 1.5757P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.39, 0.513.61, 4.210.30, 0.330.33, 0.46
Absolute structure??Flack (1983), 1412 Friedel pairsFlack (1983), 1486 Friedel pairs
Absolute structure parameter??0.08 (5)0.017 (4)


(V)(VI)(VII)(VIII)
Crystal data
Chemical formulaC16H28BaN10O14·3(H2O)C18H30N12O14SrC18H30BaN12O14C20H36CaN10O12·C20H38CaN10O13·3.123(H2O)
Mr775.45726.16775.871371.37
Crystal system, space groupTriclinic, P1Monoclinic, C2/cMonoclinic, C2/cMonoclinic, P21
Temperature (K)120120120120
a, b, c (Å)7.1387 (2), 7.4974 (2), 13.5644 (4)12.9517 (3), 7.7020 (2), 26.5416 (7)13.3918 (3), 7.4669 (2), 28.8211 (7)7.5557 (3), 13.9726 (6), 29.4179 (12)
α, β, γ (°)99.5040 (9), 94.308 (1), 99.6000 (16)90, 97.2770 (12), 9090, 103.131 (1), 9090, 91.803 (2), 90
V3)702.05 (3)2626.30 (11)2806.62 (12)3104.2 (2)
Z1442
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)1.512.151.510.28
Crystal size (mm)0.40 × 0.26 × 0.020.25 × 0.25 × 0.060.20 × 0.15 × 0.040.05 × 0.04 × 0.03
Data collection
DiffractometerKappa-CCD
diffractometer
Kappa-CCD
diffractometer
Kappa-CCD
diffractometer
Kappa-CCD
diffractometer
Absorption correctionMulti-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Tmin, Tmax0.625, 0.9700.616, 0.8820.753, 0.9420.967, 0.992
No. of measured, independent and
observed [I > 2σ(I)] reflections
10911, 5818, 5773 16348, 2982, 2369 7598, 3148, 2905 21417, 14077, 13181
Rint0.0380.0730.0460.027
(sin θ/λ)max1)0.6480.6490.6470.687
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.075, 1.01 0.049, 0.134, 1.05 0.034, 0.085, 1.24 0.037, 0.085, 1.05
No. of reflections58182982314814077
No. of parameters397205205888
No. of restraints30048
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0297P)2 + 0.7753P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0779P)2 + 5.4996P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2)P)2 + 16.8531P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0407P)2 + 0.4491P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.44, 0.931.43, 0.740.99, 0.840.40, 0.39
Absolute structureFlack (1983), 2609 Friedel pairs??Flack (1983), 5320 Friedel pairs
Absolute structure parameter0.006 (12)??0.085 (17)


(IX)
Crystal data
Chemical formulaC20H36BaN10O12S2·3(H2O)
Mr864.11
Crystal system, space groupTetragonal, P43
Temperature (K)120
a, b, c (Å)21.6978 (2), 21.6978 (2), 7.4057 (1)
α, β, γ (°)90, 90, 90
V3)3486.56 (7)
Z4
Radiation typeMo Kα
µ (mm1)1.34
Crystal size (mm)0.60 × 0.03 × 0.02
Data collection
DiffractometerKappa-CCD
diffractometer
Absorption correctionMulti-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Tmin, Tmax0.501, 0.974
No. of measured, independent and
observed [I > 2σ(I)] reflections
21371, 7394, 7035
Rint0.072
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.089, 1.05
No. of reflections7394
No. of parameters478
No. of restraints46
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0289P)2 + 4.0203P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.74, 0.71
Absolute structureFlack (1983), 3077 Friedel pairs
Absolute structure parameter0.022 (13)

Computer programs: Kappa-CCD server software (Nonius, 1997), DENZO-SMN (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 1997b), PLATON (Spek, 2003), SHELXL97 (Sheldrick, 1997a) and PRPKAPPA (Ferguson, 1999).

Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O2i0.882.122.962 (4)159
N6—H6A···O4ii0.882.012.818 (4)152
N6—H6B···O50.881.962.613 (4)130
O1—H1X···O122i0.941.762.698 (4)177
O1—H1Y···O5iii0.941.752.688 (4)172
O2—H2X···O4W0.941.802.733 (3)172
O2—H2Y···O30.941.702.635 (4)176
O3—H3X···O1220.941.782.710 (4)169
O3—H3Y···O1iv0.942.072.914 (4)149
O4W—H4X···O4v0.942.062.880 (4)145
O4W—H4X···N5v0.942.433.220 (4)141
O4W—H4Y···O122vi0.941.852.787 (4)172
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y, z; (iii) x, y1, z1; (iv) x, y+1, z; (v) x+1, y, z1; (vi) x+1, y+2, z+1.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
N16—H16A···O14i0.881.982.827 (13)161
N16—H16B···O150.881.972.608 (13)129
N22—H22···O3ii0.882.042.862 (10)156
N26—H26A···O24iii0.882.182.837 (12)131
N26—H26B···O250.881.942.607 (12)131
O1—H11C···O222iv0.881.862.721 (12)165
O1—H12D···O122ii0.961.822.722 (12)156
O2—H21C···O24v0.932.113.030 (11)168
O2—H21C···N25v0.932.362.918 (11)118
O2—H22D···O222iii0.901.942.731 (11)145
O3—H31C···O221iv0.921.882.796 (11)174
O3—H32D···O4iv1.002.243.024 (12)135
O4—H41C···O15vi0.921.762.667 (11)165
O4—H42D···O222iii0.912.092.996 (12)171
O5—H51C···O61.011.862.824(14158
O5—H51D···O122ii0.911.902.795 (12)170
O6—H61C···N15vii0.992.203.174 (12)172
O6—H62D···O1viii1.011.972.941 (13)160
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x, y1/2, z+1/2; (iv) x, y+1, z; (v) x+1, y+1/2, z+1/2; (vi) x, y, z+1; (vii) x, y1/2, z+1/2; (viii) x, y1, z.
Hydrogen-bond geometry (Å, º) for (III) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3i0.882.373.243 (3)168
O21—H21A···O20.822.042.846 (3)167
N6—H6A···O4ii0.881.912.781 (3)168
N6—H6B···O50.881.952.609 (3)130
O1—H11···O2i0.971.822.758 (3)162
O1—H12···O30.972.162.931 (3)136
O2—H21B···N5iii0.842.613.402 (3)157
O2—H21B···O5iii0.841.882.711 (3)175
O2—H22B···O23iv0.841.912.727 (3)164
O3—H31···O23i0.972.122.982 (3)147
O3—H32···O22v0.971.852.818 (3)174
Symmetry codes: (i) x+2, y, z; (ii) x, y, z+1; (iii) x+3/2, y1/2, z; (iv) x, y1, z; (v) x+2, y, z+1.
Hydrogen-bond geometry (Å, º) for (IV) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3i0.882.363.224 (3)166
O21—H21A···O20.822.012.812 (2)164
N6—H6A···O4ii0.881.922.790 (2)169
N6—H6B···O50.881.952.610 (2)130
O1—H11···O2i0.981.792.753 (2)167
O1—H12···O30.982.102.877 (3)135
O2—H21B···N5iii0.852.573.377 (3)158
O2—H21B···O5iii0.851.852.699 (2)173
O2—H22B···O23iv0.851.902.730 (2)163
O3—H31···O23i0.852.362.950 (4)127
O3—H31···O3i0.852.553.119 (4)126
O3—H32···O22v0.851.992.831 (2)171
Symmetry codes: (i) x+2, y, z; (ii) x, y, z+1; (iii) x+3/2, y1/2, z; (iv) x, y1, z; (v) x+2, y, z+1.
Hydrogen-bond geometry (Å, º) for (V) top
D—H···AD—HH···AD···AD—H···A
N12—H12···O70.882.252.989 (7)141
O13—H13···O60.851.932.772 (5)168
N16—H16A···O14i0.882.002.845 (7)161
N16—H16B···O150.881.972.620 (7)130
O23—H23···O70.852.072.885 (5)160
N26—H26A···O24ii0.882.042.873 (6)158
N26—H26B···O250.881.982.631 (6)130
O1—H1A···O11iii0.861.992.809 (4)158
O1—H1B···O22iv0.861.912.750 (5)164
O2—H2A···O15v0.881.812.691 (4)176
O2—H2A···N15v0.882.463.261 (6)152
O2—H2B···O22i0.881.992.849 (4)166
O3—H3A···O25vi0.881.922.793 (4)171
O3—H3B···O5i0.881.882.707 (5)155
O3—H3B···O51i0.881.962.831 (17)171
O4—H4A···O210.901.892.702 (5)149
O4—H4B···N15v0.902.163.012 (6)159
O4—H4B···O14v0.902.473.134 (4)131
O5—H5A···O120.951.792.695 (5)157
O5—H5B···O220.951.932.873 (6)175
O6—H6A···O12vii0.951.962.769 (6)141
O6—H6B···N25viii0.952.283.083 (8)142
O6—H6B···O24viii0.952.323.160 (6)147
O7—H7A···O3ix0.951.892.791 (4)157
O7—H7B···O220.952.032.935 (6)159
Symmetry codes: (i) x, y+1, z; (ii) x, y1, z; (iii) x+1, y, z; (iv) x+1, y+1, z; (v) x+1, y+1, z+1; (vi) x, y, z1; (vii) x1, y, z; (viii) x1, y1, z1; (ix) x1, y1, z.
Hydrogen-bond geometry (Å, º) for (VI) top
D—H···AD—HH···AD···AD—H···A
N21—H21···O23i0.882.132.928 (4)151
N21—H21···O2ii0.882.643.084 (4)112
N22—H22···N5iii0.882.263.041 (4)148
N6—H6A···O4iv0.882.032.841 (4)153
N6—H6B···O50.881.952.601 (4)130
O1—H1A···O220.931.982.901 (4)173
O1—H1B···O5v0.932.022.852 (4)148
O2—H2A···O22vi0.931.852.752 (4)162
O2—H2B···O22vii0.931.832.763 (4)176
Symmetry codes: (i) x+1/2, y1/2, z; (ii) x+3/2, y+1/2, z+1/2; (iii) x+3/2, y+5/2, z; (iv) x1/2, y1/2, z; (v) x, y+2, z+1/2; (vi) x, y1, z; (vii) x+3/2, y1/2, z+1/2.
Hydrogen-bond geometry (Å, º) for (VII) top
D—H···AD—HH···AD···AD—H···A
N21—H21···O23i0.882.052.827 (4)146
N22—H22···N5ii0.882.273.077 (4)152
N6—H6A···O4iii0.881.972.779 (4)151
N6—H6B···O50.881.942.597 (4)131
O1—H1A···O5iv0.901.942.839 (4)175
O1—H1B···O22v0.901.972.814 (4)156
O2—H2A···O220.901.952.826 (4)165
O2—H2B···O22vi0.901.902.779 (4)164
Symmetry codes: (i) x+1/2, y1/2, z; (ii) x+1/2, y+1/2, z; (iii) x, y+1, z; (iv) x+1/2, y+3/2, z+1/2; (v) x+1, y+1, z+1/2; (vi) x+1/2, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) for (VIII) top
D—H···AD—HH···AD···AD—H···A
N16—H16A···O14i0.882.132.997 (2)170
N16—H16B···O150.881.982.620 (2)128
N16—H16B···O4ii0.882.563.383 (2)156
N26—H26A···O24iii0.882.203.073 (2)175
N26—H26B···O250.882.002.640 (2)128
N32—H32···O120.882.162.989 (2)156
N36—H36A···O34iii0.882.032.830 (2)150
N36—H36B···O350.881.952.611 (2)131
N46—H46A···O44i0.882.042.871 (2)158
N46—H46B···O450.882.002.632 (2)128
N46—H46B···O11iv0.882.453.016 (2)123
O1—H1A···O422iii0.852.032.811 (2)154
O1—H1B···O8iii0.852.022.828 (2)160
O2—H2A···O1210.852.202.752 (2)122
O2—H2B···O60.852.042.869 (2)164
O3—H3A···O10v0.851.902.743 (2)174
O3—H3B···O122i0.851.992.777 (2)153
O4—H4A···O222iii0.852.062.902 (2)168
O4—H4B···O10vi0.851.902.750 (2)173
O5—H5A···O110.851.912.750 (2)169
O5—H5B···N35iv0.852.192.991 (2)157
O5—H5B···O34iv0.852.433.048 (2)130
O6—H6A···O3220.851.852.673 (2)161
O6—H6B···O422iii0.851.962.734 (2)152
O7—H7A···O45vii0.851.932.723 (2)155
O7—H7B···O35iv0.852.022.815 (2)155
O7—H7B···N35iv0.852.653.225 (2)126
O8—H8A···O2220.851.922.743 (2)163
O8—H8B···O122i0.851.842.680 (2)168
O9—H9A···O422iii0.951.792.730 (2)169
O9—H9B···O2220.952.133.074 (2)171
O9—H9B···O80.952.653.178 (2)116
O10—H10A···O140.892.112.947 (2)156
O10—H10A···N150.892.373.022 (2)130
O10—H10B···N25viii0.892.242.894 (2)130
O10—H10B···O24viii0.892.303.115 (2)152
O11—H11A···O3220.891.992.834 (2)159
O11—H11B···O44ix0.892.283.019 (2)140
O11—H11B···N45ix0.892.403.185 (2)148
O12—H12M···O70.892.273.017 (2)142
O12—H12M···O3210.892.403.086 (2)135
O12—H12N···O322i0.892.062.912 (2)161
Symmetry codes: (i) x+1, y, z; (ii) x, y+1/2, z+1; (iii) x1, y, z; (iv) x+2, y1/2, z+2; (v) x, y1/2, z+1; (vi) x1, y1/2, z+1; (vii) x+2, y+1/2, z+2; (viii) x2, y+1, z; (ix) x+1, y+1/2, z+2.
Hydrogen-bond geometry (Å, º) for (IX) top
D—H···AD—HH···AD···AD—H···A
N12—H12···O70.882.092.915 (5)156
N16—H16A···O14i0.882.072.890 (5)155
N16—H16B···O150.881.992.623 (5)128
N22—H22···O5ii0.882.052.891 (5)159
N26—H26A···O24i0.882.072.875 (5)152
N26—H26B···O250.882.002.644 (5)129
O1—H12W···O15iii0.841.862.702 (4)175
O2—H21W···O12iv0.841.912.738 (4)169
O2—H22W···O22iv0.841.912.752 (4)176
O3—H31W···O60.841.922.741 (4)167
O3—H32W···O12ii0.841.942.768 (4)171
O4—H41W···N25v0.841.912.721 (5)161
O4—H42W···O12ii0.842.072.832 (4)151
O5—H51W···O4i0.842.002.842 (5)176
O5—H52W···O220.841.882.687 (5)160
O6—H61W···O22iv0.841.952.761 (4)163
O6—H62W···N15vi0.842.213.047 (6)176
O7—H71W···O110.842.102.832 (5)145
O7—H72W···O14vi0.842.223.055 (5)170
Symmetry codes: (i) x, y, z+1; (ii) x, y, z1; (iii) y+1, x, z1/4; (iv) x+2, y+1, z1/2; (v) y, x+1, z+1/4; (vi) y+1, x+1, z+1/4.
 

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