Barium di-μ-hydroxo-bis[(nitrilo­triacetato)chromium(III)] hexahydrate

Visser, H.G.

doi:10.1107/S1600536806044631

Buy article online - an online subscription or single-article purchase is required to access this article.

Barium di-μ-hydroxo-bis[(nitrilotriacetato)chromium(III)] hexahydrate

H. G. Visser

The title compound, Ba[Cr₂(C₆H₆NO₆)₂(OH)₂]·6H₂O, is contains two discrete Cr(nta)OH units (nta³⁻ is nitrilotriacetate) in the asymmetric unit, each generating a centrosymmetric dimer with two hydroxo bridges. The ten-coordinate Ba²⁺ cation provides a link between dimeric units. Each Cr^III ion is in a distorted octahedral environment and coordinated by two bridging hydroxo O atoms, plus an N atom and three carboxylate O atoms of the nta³⁻ ligand. The important geometrical parameters are Cr—N = 2.0716 (19) and 2.0779 (19) Å, Cr—O = 1.9421 (17)–1.9900 (17) Å, and O—Cr—O = 162.85 (7)–176.90 (7)°.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044631/sj2140sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044631/sj2140Isup2.hkl Contains datablock I

CCDC reference: 630465

checkCIF report

Key indicators

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.003 Å
R factor = 0.024
wR factor = 0.055
Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.66 Ratio
PLAT354_ALERT_3_C Short   O-H Bond (0.82A)   O13    -   H13    ...       0.70 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.24 Ratio

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   4 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus and XPREP (Bruker, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

Barium di-µ-hydroxo-bis[(nitrilotriacetato)chromium(III)] trihydrate top

Crystal data top

Ba[Cr₂(C₆H₆NO₆)₂(OH)₂]·3H₂O	Z = 2
M_r = 759.69	F(000) = 752
Triclinic, P1	D_x = 2.149 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.0363 (13) Å	Cell parameters from 9163 reflections
b = 11.0609 (14) Å	θ = 3.0–28.2°
c = 11.6223 (14) Å	µ = 2.67 mm⁻¹
α = 66.513 (5)°	T = 100 K
β = 65.039 (6)°	Plate, purple
γ = 75.568 (6)°	0.39 × 0.14 × 0.07 mm
V = 1174.1 (3) Å³

Data collection top

Bruker X8 APEXII 4K KappaCCD area-detector diffractometer	5805 independent reflections
Graphite monochromator	5427 reflections with I > 2σ(I)
Detector resolution: 512 pixels mm^-1	R_int = 0.038
ω and φ scans	θ_max = 28.3°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −14→14
T_min = 0.423, T_max = 0.835	k = −14→14
22175 measured reflections	l = −15→15

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0217P)² + 1.0555P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.055	(Δ/σ)_max = 0.001
S = 1.02	Δρ_max = 0.57 e Å⁻³
5805 reflections	Δρ_min = −0.71 e Å⁻³
376 parameters

Special details top

Experimental. The intensity data were collected on a Bruker X8 Apex II 4 K Kappa CCD diffractometer using an exposure time of 3 s/frame. A total of 1865 frames were collected with a frame width of 0.5° covering up to θ = 28.28° with 99.6% completeness accomplished. IR, ν(C═O) 1624 cm^-1; UV–Vis (H₂O): λ_max 565.1, 410.2 nm.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cr1	−0.39768 (4)	0.41219 (3)	−0.06738 (4)	0.00630 (8)
Cr2	−0.43740 (4)	0.11764 (4)	0.46676 (4)	0.00674 (8)
C1	−0.3928 (2)	0.1308 (2)	0.0555 (2)	0.0087 (4)
H1A	−0.413	0.1129	0.152	0.01*
H1B	−0.357	0.0463	0.0371	0.01*
C2	−0.5214 (2)	0.1852 (2)	0.0248 (2)	0.0088 (4)
C3	−0.2057 (2)	0.2099 (2)	−0.1631 (2)	0.0089 (4)
H3A	−0.2395	0.1394	−0.1705	0.011*
H3B	−0.1119	0.1806	−0.1678	0.011*
C4	−0.2079 (2)	0.3354 (2)	−0.2804 (2)	0.0089 (4)
C5	−0.2041 (2)	0.2296 (2)	0.0411 (2)	0.0084 (4)
H5A	−0.1165	0.1783	0.0104	0.01*
H5B	−0.248	0.186	0.1393	0.01*
C6	−0.1806 (2)	0.3689 (2)	0.0144 (2)	0.0083 (4)
C7	−0.2152 (2)	0.1084 (2)	0.5371 (2)	0.0101 (5)
H7A	−0.2282	0.0264	0.6165	0.012*
H7B	−0.151	0.1579	0.5359	0.012*
C8	−0.1595 (2)	0.0734 (2)	0.4086 (2)	0.0094 (5)
C9	−0.4433 (2)	0.1786 (2)	0.6849 (2)	0.0082 (4)
H9A	−0.4323	0.247	0.7136	0.01*
H9B	−0.4258	0.0905	0.7479	0.01*
C10	−0.5867 (2)	0.1955 (2)	0.6886 (2)	0.0085 (4)
C11	−0.3269 (3)	0.3335 (2)	0.4619 (2)	0.0114 (5)
H11A	−0.2304	0.3458	0.4264	0.014*
H11B	−0.3764	0.3891	0.5197	0.014*
C12	−0.3747 (2)	0.3807 (2)	0.3447 (2)	0.0093 (5)
N1	−0.28964 (19)	0.22781 (18)	−0.02894 (19)	0.0067 (4)
N2	−0.34616 (19)	0.19114 (18)	0.54619 (18)	0.0071 (4)
O1	−0.61470 (17)	0.11670 (17)	0.07673 (18)	0.0137 (4)
O2	−0.52607 (16)	0.30753 (15)	−0.05513 (16)	0.0086 (3)
O3	−0.12844 (17)	0.33885 (17)	−0.39557 (16)	0.0125 (4)
O4	−0.29306 (16)	0.43220 (16)	−0.25546 (16)	0.0094 (3)
O5	−0.10158 (16)	0.38685 (16)	0.05482 (17)	0.0099 (3)
O6	−0.25133 (16)	0.46532 (15)	−0.04604 (16)	0.0079 (3)
O7	−0.03701 (17)	0.05735 (17)	0.34889 (17)	0.0136 (4)
O8	−0.24830 (16)	0.05872 (16)	0.37085 (16)	0.0095 (3)
O9	−0.68161 (17)	0.20985 (16)	0.78951 (17)	0.0115 (3)
O10	−0.59987 (16)	0.18816 (16)	0.58705 (16)	0.0093 (3)
O11	−0.36934 (18)	0.49713 (16)	0.27247 (17)	0.0145 (4)
O12	−0.41670 (17)	0.29344 (16)	0.32616 (16)	0.0093 (3)
O13	−0.48687 (17)	0.59203 (16)	−0.11739 (16)	0.0076 (3)
O14	−0.46761 (17)	−0.05648 (16)	0.60629 (16)	0.0081 (3)
Ba	−0.196707 (13)	0.656708 (12)	0.036813 (13)	0.00595 (4)
O15	−0.0751 (2)	0.5625 (2)	0.2259 (2)	0.0202 (4)
O16	−0.10151 (19)	0.89887 (18)	−0.0711 (2)	0.0138 (4)
O17	−0.07781 (19)	0.70074 (18)	−0.24391 (18)	0.0133 (4)
O18	−0.10769 (19)	0.91428 (19)	0.17540 (19)	0.0145 (4)
O19	−0.27699 (19)	0.74168 (18)	−0.34360 (19)	0.0126 (4)
O20	−0.1373 (2)	0.62050 (19)	−0.53863 (19)	0.0161 (4)
H15A	−0.029 (3)	0.494 (3)	0.241 (3)	0.024*
H15B	−0.102 (3)	0.579 (3)	0.290 (3)	0.024*
H16A	−0.051 (3)	0.922 (3)	−0.143 (3)	0.024*
H16B	−0.081 (3)	0.933 (3)	−0.035 (3)	0.024*
H17A	−0.041 (3)	0.766 (3)	−0.280 (3)	0.024*
H17B	−0.135 (3)	0.708 (3)	−0.272 (3)	0.024*
H18A	−0.160 (3)	0.866 (3)	0.198 (3)	0.024*
H18B	−0.145 (3)	0.948 (3)	0.233 (3)	0.024*
H19A	−0.246 (3)	0.713 (3)	−0.404 (3)	0.024*
H19B	−0.327 (3)	0.690 (3)	−0.278 (3)	0.024*
H20A	−0.064 (3)	0.640 (3)	−0.555 (3)	0.024*
H20B	−0.143 (3)	0.547 (3)	−0.495 (3)	0.024*
H13	−0.518 (3)	0.609 (3)	−0.164 (3)	0.019*
H14	−0.412 (3)	−0.105 (3)	0.613 (3)	0.019*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.00645 (18)	0.00598 (17)	0.00673 (17)	0.00014 (14)	−0.00322 (14)	−0.00195 (14)
Cr2	0.00705 (18)	0.00735 (17)	0.00653 (17)	−0.00109 (14)	−0.00310 (14)	−0.00211 (14)
C1	0.0085 (11)	0.0071 (10)	0.0087 (11)	−0.0003 (9)	−0.0034 (9)	−0.0010 (9)
C2	0.0105 (11)	0.0090 (11)	0.0077 (11)	0.0019 (9)	−0.0041 (9)	−0.0044 (9)
C3	0.0101 (11)	0.0074 (10)	0.0087 (11)	0.0013 (9)	−0.0028 (9)	−0.0043 (9)
C4	0.0084 (11)	0.0103 (11)	0.0115 (11)	−0.0027 (9)	−0.0051 (9)	−0.0044 (9)
C5	0.0111 (11)	0.0077 (10)	0.0105 (11)	0.0009 (9)	−0.0088 (9)	−0.0029 (9)
C6	0.0066 (11)	0.0103 (11)	0.0065 (10)	0.0008 (9)	0.0000 (9)	−0.0048 (9)
C7	0.0082 (11)	0.0132 (11)	0.0107 (11)	0.0005 (9)	−0.0049 (9)	−0.0052 (9)
C8	0.0103 (12)	0.0069 (10)	0.0085 (11)	−0.0018 (9)	−0.0027 (9)	−0.0005 (9)
C9	0.0078 (11)	0.0119 (11)	0.0059 (10)	−0.0037 (9)	−0.0017 (9)	−0.0032 (9)
C10	0.0108 (12)	0.0033 (10)	0.0100 (11)	−0.0009 (8)	−0.0035 (9)	−0.0012 (8)
C11	0.0174 (13)	0.0066 (10)	0.0114 (11)	−0.0045 (9)	−0.0087 (10)	0.0013 (9)
C12	0.0075 (11)	0.0126 (11)	0.0066 (10)	−0.0014 (9)	−0.0013 (9)	−0.0028 (9)
N1	0.0070 (9)	0.0069 (9)	0.0067 (9)	0.0000 (7)	−0.0032 (7)	−0.0024 (7)
N2	0.0073 (9)	0.0074 (9)	0.0055 (9)	−0.0010 (7)	−0.0024 (7)	−0.0008 (7)
O1	0.0113 (9)	0.0127 (8)	0.0175 (9)	−0.0041 (7)	−0.0070 (7)	−0.0017 (7)
O2	0.0104 (8)	0.0083 (8)	0.0090 (8)	0.0000 (6)	−0.0058 (7)	−0.0026 (6)
O3	0.0121 (9)	0.0158 (9)	0.0079 (8)	−0.0013 (7)	−0.0011 (7)	−0.0049 (7)
O4	0.0104 (8)	0.0076 (8)	0.0085 (8)	0.0014 (6)	−0.0036 (7)	−0.0022 (6)
O5	0.0088 (8)	0.0109 (8)	0.0135 (8)	−0.0006 (6)	−0.0060 (7)	−0.0058 (7)
O6	0.0070 (8)	0.0066 (7)	0.0108 (8)	−0.0005 (6)	−0.0046 (6)	−0.0023 (6)
O7	0.0084 (9)	0.0157 (9)	0.0146 (9)	−0.0019 (7)	−0.0017 (7)	−0.0054 (7)
O8	0.0080 (8)	0.0116 (8)	0.0098 (8)	−0.0013 (6)	−0.0025 (7)	−0.0052 (7)
O9	0.0102 (8)	0.0129 (8)	0.0113 (8)	−0.0018 (7)	−0.0007 (7)	−0.0071 (7)
O10	0.0083 (8)	0.0111 (8)	0.0097 (8)	−0.0009 (6)	−0.0033 (7)	−0.0049 (6)
O11	0.0182 (9)	0.0090 (8)	0.0130 (9)	−0.0040 (7)	−0.0076 (7)	0.0033 (7)
O12	0.0111 (8)	0.0093 (8)	0.0085 (8)	−0.0012 (6)	−0.0055 (7)	−0.0019 (6)
O13	0.0076 (8)	0.0093 (8)	0.0064 (8)	0.0006 (6)	−0.0043 (6)	−0.0021 (6)
O14	0.0077 (8)	0.0081 (8)	0.0094 (8)	0.0001 (6)	−0.0046 (7)	−0.0027 (6)
Ba	0.00643 (7)	0.00564 (7)	0.00633 (7)	−0.00056 (5)	−0.00270 (5)	−0.00216 (5)
O15	0.0202 (11)	0.0275 (11)	0.0156 (10)	0.0101 (9)	−0.0105 (8)	−0.0128 (9)
O16	0.0148 (10)	0.0119 (9)	0.0149 (9)	−0.0052 (7)	−0.0050 (8)	−0.0028 (7)
O17	0.0124 (9)	0.0164 (9)	0.0126 (9)	−0.0051 (7)	−0.0062 (7)	−0.0024 (7)
O18	0.0120 (9)	0.0172 (9)	0.0163 (9)	−0.0046 (7)	−0.0021 (8)	−0.0091 (8)
O19	0.0130 (9)	0.0118 (9)	0.0116 (9)	−0.0021 (7)	−0.0040 (7)	−0.0027 (7)
O20	0.0160 (10)	0.0150 (9)	0.0141 (9)	−0.0047 (8)	−0.0055 (8)	0.0001 (7)

Geometric parameters (Å, º) top

Cr1—O4	1.9421 (17)	C9—H9A	0.9900
Cr1—O13	1.9619 (16)	C9—H9B	0.9900
Cr1—O13ⁱ	1.9692 (17)	C10—O9	1.236 (3)
Cr1—O2	1.9708 (17)	C10—O10	1.284 (3)
Cr1—O6	1.9857 (16)	C11—N2	1.499 (3)
Cr1—N1	2.0716 (19)	C11—C12	1.520 (3)
Cr1—Cr1ⁱ	2.9292 (8)	C11—H11A	0.9900
Cr2—O14	1.9557 (17)	C11—H11B	0.9900
Cr2—O10	1.9581 (17)	C12—O11	1.225 (3)
Cr2—O14ⁱⁱ	1.9597 (17)	C12—O12	1.290 (3)
Cr2—O12	1.9690 (16)	O1—Baⁱ	3.0719 (17)
Cr2—O8	1.9900 (17)	O2—Baⁱ	2.9114 (16)
Cr2—N2	2.0779 (19)	O5—Ba	2.8603 (17)
Cr2—Cr2ⁱⁱ	2.9271 (8)	O5—Baⁱⁱⁱ	2.9770 (17)
C1—N1	1.495 (3)	O6—Ba	2.9195 (16)
C1—C2	1.528 (3)	O9—Ba^iv	2.6750 (17)
C1—H1A	0.9900	O11—Ba	2.7686 (17)
C1—H1B	0.9900	O13—Cr1ⁱ	1.9692 (17)
C2—O1	1.224 (3)	O13—H13	0.71 (3)
C2—O2	1.304 (3)	O14—Cr2ⁱⁱ	1.9597 (17)
C2—Baⁱ	3.379 (2)	O14—H14	0.72 (3)
C3—N1	1.504 (3)	Ba—O9^iv	2.6750 (17)
C3—C4	1.513 (3)	Ba—O16	2.7321 (18)
C3—H3A	0.9900	Ba—O15	2.7728 (19)
C3—H3B	0.9900	Ba—O17	2.8360 (19)
C4—O3	1.244 (3)	Ba—O2ⁱ	2.9114 (16)
C4—O4	1.276 (3)	Ba—O5ⁱⁱⁱ	2.9770 (17)
C5—N1	1.492 (3)	Ba—O1ⁱ	3.0719 (17)
C5—C6	1.512 (3)	Ba—C2ⁱ	3.379 (2)
C5—H5A	0.9900	O15—H15A	0.80 (3)
C5—H5B	0.9900	O15—H15B	0.76 (3)
C6—O5	1.236 (3)	O16—H16A	0.76 (3)
C6—O6	1.300 (3)	O16—H16B	0.79 (3)
C6—Ba	3.252 (2)	O17—H17A	0.79 (3)
C7—N2	1.492 (3)	O17—H17B	0.80 (3)
C7—C8	1.525 (3)	O18—H18A	0.78 (3)
C7—H7A	0.9900	O18—H18B	0.81 (3)
C7—H7B	0.9900	O19—H19A	0.79 (3)
C8—O7	1.236 (3)	O19—H19B	0.82 (3)
C8—O8	1.295 (3)	O20—H20A	0.81 (3)
C9—N2	1.484 (3)	O20—H20B	0.77 (3)
C9—C10	1.530 (3)

O4—Cr1—O13	91.01 (7)	C3—N1—Cr1	106.86 (13)
O4—Cr1—O13ⁱ	174.62 (7)	C9—N2—C7	115.37 (17)
O13—Cr1—O13ⁱ	83.66 (7)	C9—N2—C11	111.07 (18)
O4—Cr1—O2	93.26 (7)	C7—N2—C11	111.74 (18)
O13—Cr1—O2	101.03 (7)	C9—N2—Cr2	104.68 (14)
O13ⁱ—Cr1—O2	87.12 (7)	C7—N2—Cr2	105.42 (14)
O4—Cr1—O6	92.20 (7)	C11—N2—Cr2	107.88 (13)
O13—Cr1—O6	95.11 (7)	C2—O1—Baⁱ	93.69 (13)
O13ⁱ—Cr1—O6	88.97 (7)	C2—O2—Cr1	113.66 (14)
O2—Cr1—O6	162.85 (7)	C2—O2—Baⁱ	99.41 (13)
O4—Cr1—N1	84.85 (7)	Cr1—O2—Baⁱ	138.00 (7)
O13—Cr1—N1	175.21 (8)	C4—O4—Cr1	116.98 (14)
O13ⁱ—Cr1—N1	100.51 (7)	C6—O5—Ba	97.03 (13)
O2—Cr1—N1	81.64 (7)	C6—O5—Baⁱⁱⁱ	131.13 (15)
O6—Cr1—N1	82.68 (7)	Ba—O5—Baⁱⁱⁱ	111.65 (5)
O4—Cr1—Cr1ⁱ	132.93 (5)	C6—O6—Cr1	115.51 (14)
O13—Cr1—Cr1ⁱ	41.92 (5)	C6—O6—Ba	92.73 (13)
O13ⁱ—Cr1—Cr1ⁱ	41.73 (5)	Cr1—O6—Ba	141.73 (7)
O2—Cr1—Cr1ⁱ	95.41 (5)	C8—O8—Cr2	115.62 (15)
O6—Cr1—Cr1ⁱ	92.73 (5)	C10—O9—Ba^iv	148.92 (15)
N1—Cr1—Cr1ⁱ	142.19 (6)	C10—O10—Cr2	114.68 (15)
O14—Cr2—O10	87.52 (7)	C12—O11—Ba	139.58 (16)
O14—Cr2—O14ⁱⁱ	83.23 (7)	C12—O12—Cr2	116.91 (14)
O10—Cr2—O14ⁱⁱ	95.28 (7)	Cr1—O13—Cr1ⁱ	96.34 (7)
O14—Cr2—O12	176.90 (7)	Cr1—O13—H13	118 (3)
O10—Cr2—O12	90.82 (7)	Cr1ⁱ—O13—H13	118 (3)
O14ⁱⁱ—Cr2—O12	94.32 (7)	Cr2—O14—Cr2ⁱⁱ	96.77 (7)
O14—Cr2—O8	92.60 (7)	Cr2—O14—H14	120 (3)
O10—Cr2—O8	164.05 (7)	Cr2ⁱⁱ—O14—H14	107 (3)
O14ⁱⁱ—Cr2—O8	100.57 (7)	O9^iv—Ba—O16	69.80 (6)
O12—Cr2—O8	89.72 (7)	O9^iv—Ba—O11	71.19 (5)
O14—Cr2—N2	98.19 (7)	O16—Ba—O11	140.90 (6)
O10—Cr2—N2	81.71 (7)	O9^iv—Ba—O15	72.00 (6)
O14ⁱⁱ—Cr2—N2	176.58 (7)	O16—Ba—O15	92.89 (6)
O12—Cr2—N2	84.15 (7)	O11—Ba—O15	72.52 (6)
O8—Cr2—N2	82.49 (7)	O9^iv—Ba—O17	140.70 (5)
O14—Cr2—Cr2ⁱⁱ	41.67 (5)	O16—Ba—O17	75.71 (6)
O10—Cr2—Cr2ⁱⁱ	91.87 (5)	O11—Ba—O17	141.41 (6)
O14ⁱⁱ—Cr2—Cr2ⁱⁱ	41.56 (5)	O15—Ba—O17	128.97 (6)
O12—Cr2—Cr2ⁱⁱ	135.85 (5)	O9^iv—Ba—O5	136.07 (5)
O8—Cr2—Cr2ⁱⁱ	98.81 (5)	O16—Ba—O5	139.96 (5)
N2—Cr2—Cr2ⁱⁱ	139.78 (5)	O11—Ba—O5	72.08 (5)
N1—C1—C2	110.52 (17)	O15—Ba—O5	74.66 (6)
N1—C1—H1A	109.5	O17—Ba—O5	83.03 (5)
C2—C1—H1A	109.5	O9^iv—Ba—O2ⁱ	78.29 (5)
N1—C1—H1B	109.5	O16—Ba—O2ⁱ	109.21 (5)
C2—C1—H1B	109.5	O11—Ba—O2ⁱ	64.69 (5)
H1A—C1—H1B	108.1	O15—Ba—O2ⁱ	133.77 (5)
O1—C2—O2	123.2 (2)	O17—Ba—O2ⁱ	96.27 (5)
O1—C2—C1	120.5 (2)	O5—Ba—O2ⁱ	106.50 (5)
O2—C2—C1	116.2 (2)	O9^iv—Ba—O6	140.31 (5)
O1—C2—Baⁱ	65.12 (12)	O16—Ba—O6	140.22 (5)
O2—C2—Baⁱ	58.21 (11)	O11—Ba—O6	75.95 (5)
C1—C2—Baⁱ	172.15 (16)	O15—Ba—O6	118.26 (5)
N1—C3—C4	112.69 (18)	O17—Ba—O6	65.62 (5)
N1—C3—H3A	109.1	O5—Ba—O6	45.35 (4)
C4—C3—H3A	109.1	O2ⁱ—Ba—O6	67.78 (4)
N1—C3—H3B	109.1	O9^iv—Ba—O5ⁱⁱⁱ	116.20 (5)
C4—C3—H3B	109.1	O16—Ba—O5ⁱⁱⁱ	72.36 (5)
H3A—C3—H3B	107.8	O11—Ba—O5ⁱⁱⁱ	124.54 (5)
O3—C4—O4	123.5 (2)	O15—Ba—O5ⁱⁱⁱ	60.74 (5)
O3—C4—C3	118.8 (2)	O17—Ba—O5ⁱⁱⁱ	68.46 (5)
O4—C4—C3	117.7 (2)	O5—Ba—O5ⁱⁱⁱ	68.35 (5)
N1—C5—C6	112.08 (17)	O2ⁱ—Ba—O5ⁱⁱⁱ	164.08 (5)
N1—C5—H5A	109.2	O6—Ba—O5ⁱⁱⁱ	100.52 (4)
C6—C5—H5A	109.2	O9^iv—Ba—O1ⁱ	72.72 (5)
N1—C5—H5B	109.2	O16—Ba—O1ⁱ	66.82 (5)
C6—C5—H5B	109.2	O11—Ba—O1ⁱ	103.79 (5)
H5A—C5—H5B	107.9	O15—Ba—O1ⁱ	143.67 (6)
O5—C6—O6	123.0 (2)	O17—Ba—O1ⁱ	76.85 (5)
O5—C6—C5	120.0 (2)	O5—Ba—O1ⁱ	139.97 (5)
O6—C6—C5	117.0 (2)	O2ⁱ—Ba—O1ⁱ	43.54 (4)
O5—C6—Ba	60.80 (12)	O6—Ba—O1ⁱ	94.64 (5)
O6—C6—Ba	63.73 (12)	O5ⁱⁱⁱ—Ba—O1ⁱ	131.47 (5)
C5—C6—Ba	164.26 (16)	O9^iv—Ba—C6	140.87 (5)
N2—C7—C8	109.03 (18)	O16—Ba—C6	149.12 (6)
N2—C7—H7A	109.9	O11—Ba—C6	69.70 (6)
C8—C7—H7A	109.9	O15—Ba—C6	95.05 (6)
N2—C7—H7B	109.9	O17—Ba—C6	76.12 (6)
C8—C7—H7B	109.9	O5—Ba—C6	22.17 (5)
H7A—C7—H7B	108.3	O2ⁱ—Ba—C6	86.19 (5)
O7—C8—O8	123.8 (2)	O6—Ba—C6	23.54 (5)
O7—C8—C7	120.5 (2)	O5ⁱⁱⁱ—Ba—C6	85.73 (5)
O8—C8—C7	115.6 (2)	O1ⁱ—Ba—C6	118.05 (5)
N2—C9—C10	109.74 (18)	O9^iv—Ba—C2ⁱ	75.09 (5)
N2—C9—H9A	109.7	O16—Ba—C2ⁱ	87.60 (6)
C10—C9—H9A	109.7	O11—Ba—C2ⁱ	85.03 (5)
N2—C9—H9B	109.7	O15—Ba—C2ⁱ	144.64 (6)
C10—C9—H9B	109.7	O17—Ba—C2ⁱ	85.37 (5)
H9A—C9—H9B	108.2	O5—Ba—C2ⁱ	124.38 (5)
O9—C10—O10	124.2 (2)	O2ⁱ—Ba—C2ⁱ	22.38 (5)
O9—C10—C9	118.9 (2)	O6—Ba—C2ⁱ	80.55 (5)
O10—C10—C9	116.8 (2)	O5ⁱⁱⁱ—Ba—C2ⁱ	150.02 (5)
N2—C11—C12	113.35 (19)	O1ⁱ—Ba—C2ⁱ	21.19 (5)
N2—C11—H11A	108.9	C6—Ba—C2ⁱ	102.46 (6)
C12—C11—H11A	108.9	Ba—O15—H15A	126 (2)
N2—C11—H11B	108.9	Ba—O15—H15B	125 (3)
C12—C11—H11B	108.9	H15A—O15—H15B	104 (3)
H11A—C11—H11B	107.7	Ba—O16—H16A	122 (3)
O11—C12—O12	123.9 (2)	Ba—O16—H16B	127 (2)
O11—C12—C11	119.0 (2)	H16A—O16—H16B	101 (3)
O12—C12—C11	117.13 (19)	Ba—O17—H17A	109 (2)
C5—N1—C1	113.66 (17)	Ba—O17—H17B	109 (2)
C5—N1—C3	111.45 (18)	H17A—O17—H17B	110 (3)
C1—N1—C3	111.95 (18)	H18A—O18—H18B	99 (3)
C5—N1—Cr1	107.03 (13)	H19A—O19—H19B	109 (3)
C1—N1—Cr1	105.34 (13)	H20A—O20—H20B	109 (3)

N1—C1—C2—O1	174.9 (2)	O12—Cr2—O8—C8	92.42 (16)
N1—C1—C2—O2	−7.1 (3)	N2—Cr2—O8—C8	8.29 (15)
N1—C3—C4—O3	170.2 (2)	Cr2ⁱⁱ—Cr2—O8—C8	−131.08 (15)
N1—C3—C4—O4	−10.6 (3)	O10—C10—O9—Ba^iv	−127.6 (3)
N1—C5—C6—O5	−173.2 (2)	C9—C10—O9—Ba^iv	55.5 (4)
N1—C5—C6—O6	9.9 (3)	O9—C10—O10—Cr2	−163.92 (18)
N1—C5—C6—Ba	98.4 (5)	C9—C10—O10—Cr2	13.1 (2)
N2—C7—C8—O7	149.1 (2)	O14—Cr2—O10—C10	72.98 (16)
N2—C7—C8—O8	−32.7 (3)	O14ⁱⁱ—Cr2—O10—C10	155.95 (15)
N2—C9—C10—O9	−168.27 (19)	O12—Cr2—O10—C10	−109.64 (16)
N2—C9—C10—O10	14.6 (3)	O8—Cr2—O10—C10	−17.8 (3)
N2—C11—C12—O11	176.8 (2)	N2—Cr2—O10—C10	−25.68 (15)
N2—C11—C12—O12	−4.4 (3)	Cr2ⁱⁱ—Cr2—O10—C10	114.43 (15)
C6—C5—N1—C1	−138.0 (2)	O12—C12—O11—Ba	−86.3 (3)
C6—C5—N1—C3	94.4 (2)	C11—C12—O11—Ba	92.4 (3)
C6—C5—N1—Cr1	−22.1 (2)	O11—C12—O12—Cr2	−172.78 (19)
C2—C1—N1—C5	144.98 (19)	C11—C12—O12—Cr2	8.5 (3)
C2—C1—N1—C3	−87.7 (2)	O10—Cr2—O12—C12	74.23 (17)
C2—C1—N1—Cr1	28.1 (2)	O14ⁱⁱ—Cr2—O12—C12	169.58 (16)
C4—C3—N1—C5	−107.2 (2)	O8—Cr2—O12—C12	−89.83 (17)
C4—C3—N1—C1	124.3 (2)	N2—Cr2—O12—C12	−7.35 (17)
C4—C3—N1—Cr1	9.4 (2)	Cr2ⁱⁱ—Cr2—O12—C12	167.76 (13)
O4—Cr1—N1—C5	114.03 (15)	O4—Cr1—O13—Cr1ⁱ	179.31 (8)
O13ⁱ—Cr1—N1—C5	−66.44 (15)	O13ⁱ—Cr1—O13—Cr1ⁱ	0.0
O2—Cr1—N1—C5	−151.91 (15)	O2—Cr1—O13—Cr1ⁱ	85.80 (8)
O6—Cr1—N1—C5	21.13 (14)	O6—Cr1—O13—Cr1ⁱ	−88.39 (7)
Cr1ⁱ—Cr1—N1—C5	−63.85 (17)	O10—Cr2—O14—Cr2ⁱⁱ	95.62 (7)
O4—Cr1—N1—C1	−124.70 (14)	O14ⁱⁱ—Cr2—O14—Cr2ⁱⁱ	0.0
O13ⁱ—Cr1—N1—C1	54.84 (14)	O8—Cr2—O14—Cr2ⁱⁱ	−100.35 (8)
O2—Cr1—N1—C1	−30.63 (13)	N2—Cr2—O14—Cr2ⁱⁱ	176.87 (8)
O6—Cr1—N1—C1	142.41 (14)	C12—O11—Ba—O9^iv	−142.3 (2)
Cr1ⁱ—Cr1—N1—C1	57.42 (17)	C12—O11—Ba—O16	−138.2 (2)
O4—Cr1—N1—C3	−5.48 (14)	C12—O11—Ba—O15	−65.9 (2)
O13ⁱ—Cr1—N1—C3	174.06 (14)	C12—O11—Ba—O17	65.6 (3)
O2—Cr1—N1—C3	88.59 (14)	C12—O11—Ba—O5	13.2 (2)
O6—Cr1—N1—C3	−98.37 (14)	C12—O11—Ba—O2ⁱ	132.1 (3)
Cr1ⁱ—Cr1—N1—C3	176.64 (10)	C12—O11—Ba—O6	60.3 (2)
C10—C9—N2—C7	−147.12 (19)	C12—O11—Ba—O5ⁱⁱⁱ	−32.9 (3)
C10—C9—N2—C11	84.4 (2)	C12—O11—Ba—O1ⁱ	151.7 (2)
C10—C9—N2—Cr2	−31.7 (2)	C12—O11—Ba—C6	36.5 (2)
C8—C7—N2—C9	150.67 (19)	C12—O11—Ba—C2ⁱ	141.8 (2)
C8—C7—N2—C11	−81.2 (2)	C6—O5—Ba—O9^iv	114.54 (14)
C8—C7—N2—Cr2	35.7 (2)	Baⁱⁱⁱ—O5—Ba—O9^iv	−105.82 (7)
C12—C11—N2—C9	−115.6 (2)	C6—O5—Ba—O16	−127.95 (14)
C12—C11—N2—C7	114.0 (2)	Baⁱⁱⁱ—O5—Ba—O16	11.69 (10)
C12—C11—N2—Cr2	−1.4 (2)	C6—O5—Ba—O11	80.05 (14)
O14—Cr2—N2—C9	−55.31 (14)	Baⁱⁱⁱ—O5—Ba—O11	−140.31 (7)
O10—Cr2—N2—C9	30.95 (13)	C6—O5—Ba—O15	156.24 (15)
O12—Cr2—N2—C9	122.64 (14)	Baⁱⁱⁱ—O5—Ba—O15	−64.12 (6)
O8—Cr2—N2—C9	−146.87 (14)	C6—O5—Ba—O17	−70.09 (14)
Cr2ⁱⁱ—Cr2—N2—C9	−52.09 (17)	Baⁱⁱⁱ—O5—Ba—O17	69.55 (6)
O14—Cr2—N2—C7	66.82 (14)	C6—O5—Ba—O2ⁱ	24.41 (14)
O10—Cr2—N2—C7	153.08 (14)	Baⁱⁱⁱ—O5—Ba—O2ⁱ	164.05 (5)
O12—Cr2—N2—C7	−115.23 (14)	C6—O5—Ba—O6	−7.71 (13)
O8—Cr2—N2—C7	−24.74 (13)	Baⁱⁱⁱ—O5—Ba—O6	131.93 (9)
Cr2ⁱⁱ—Cr2—N2—C7	70.04 (16)	C6—O5—Ba—O5ⁱⁱⁱ	−139.64 (16)
O14—Cr2—N2—C11	−173.67 (14)	Baⁱⁱⁱ—O5—Ba—O5ⁱⁱⁱ	0.0
O10—Cr2—N2—C11	−87.41 (15)	C6—O5—Ba—O1ⁱ	−10.21 (17)
O12—Cr2—N2—C11	4.28 (15)	Baⁱⁱⁱ—O5—Ba—O1ⁱ	129.43 (6)
O8—Cr2—N2—C11	94.77 (15)	Baⁱⁱⁱ—O5—Ba—C6	139.64 (16)
Cr2ⁱⁱ—Cr2—N2—C11	−170.45 (11)	C6—O5—Ba—C2ⁱ	9.41 (16)
O2—C2—O1—Baⁱ	−4.0 (2)	Baⁱⁱⁱ—O5—Ba—C2ⁱ	149.05 (6)
C1—C2—O1—Baⁱ	173.85 (19)	C6—O6—Ba—O9^iv	−105.98 (14)
O1—C2—O2—Cr1	157.83 (19)	Cr1—O6—Ba—O9^iv	33.18 (15)
C1—C2—O2—Cr1	−20.2 (2)	C6—O6—Ba—O16	126.98 (13)
Baⁱ—C2—O2—Cr1	153.51 (14)	Cr1—O6—Ba—O16	−93.86 (13)
O1—C2—O2—Baⁱ	4.3 (3)	C6—O6—Ba—O11	−71.26 (13)
C1—C2—O2—Baⁱ	−173.66 (16)	Cr1—O6—Ba—O11	67.90 (12)
O4—Cr1—O2—C2	113.77 (16)	C6—O6—Ba—O15	−10.34 (14)
O13—Cr1—O2—C2	−154.57 (15)	Cr1—O6—Ba—O15	128.82 (11)
O13ⁱ—Cr1—O2—C2	−71.61 (16)	C6—O6—Ba—O17	112.36 (14)
O6—Cr1—O2—C2	5.4 (3)	Cr1—O6—Ba—O17	−108.47 (12)
N1—Cr1—O2—C2	29.47 (16)	C6—O6—Ba—O5	7.28 (12)
Cr1ⁱ—Cr1—O2—C2	−112.55 (15)	Cr1—O6—Ba—O5	146.44 (15)
O4—Cr1—O2—Baⁱ	−107.35 (11)	C6—O6—Ba—O2ⁱ	−139.30 (14)
O13—Cr1—O2—Baⁱ	−15.69 (12)	Cr1—O6—Ba—O2ⁱ	−0.14 (11)
O13ⁱ—Cr1—O2—Baⁱ	67.27 (11)	C6—O6—Ba—O5ⁱⁱⁱ	51.97 (13)
O6—Cr1—O2—Baⁱ	144.3 (2)	Cr1—O6—Ba—O5ⁱⁱⁱ	−168.87 (11)
N1—Cr1—O2—Baⁱ	168.35 (12)	C6—O6—Ba—O1ⁱ	−174.34 (13)
Cr1ⁱ—Cr1—O2—Baⁱ	26.33 (10)	Cr1—O6—Ba—O1ⁱ	−35.17 (12)
O3—C4—O4—Cr1	−175.03 (18)	Cr1—O6—Ba—C6	139.2 (2)
C3—C4—O4—Cr1	5.8 (3)	C6—O6—Ba—C2ⁱ	−158.46 (13)
O13—Cr1—O4—C4	177.64 (17)	Cr1—O6—Ba—C2ⁱ	−19.30 (11)
O2—Cr1—O4—C4	−81.25 (17)	O5—C6—Ba—O9^iv	−90.44 (15)
O6—Cr1—O4—C4	82.49 (17)	O6—C6—Ba—O9^iv	103.39 (14)
N1—Cr1—O4—C4	0.04 (17)	C5—C6—Ba—O9^iv	6.9 (6)
Cr1ⁱ—Cr1—O4—C4	178.27 (13)	O5—C6—Ba—O16	81.31 (17)
O6—C6—O5—Ba	14.8 (2)	O6—C6—Ba—O16	−84.86 (16)
C5—C6—O5—Ba	−161.90 (18)	C5—C6—Ba—O16	178.7 (5)
O6—C6—O5—Baⁱⁱⁱ	−112.2 (2)	O5—C6—Ba—O11	−92.21 (14)
C5—C6—O5—Baⁱⁱⁱ	71.1 (3)	O6—C6—Ba—O11	101.62 (13)
Ba—C6—O5—Baⁱⁱⁱ	−126.96 (17)	C5—C6—Ba—O11	5.2 (5)
O5—C6—O6—Cr1	−167.73 (18)	O5—C6—Ba—O15	−22.96 (14)
C5—C6—O6—Cr1	9.1 (3)	O6—C6—Ba—O15	170.87 (13)
Ba—C6—O6—Cr1	−153.33 (13)	C5—C6—Ba—O15	74.4 (5)
O5—C6—O6—Ba	−14.4 (2)	O5—C6—Ba—O17	105.98 (14)
C5—C6—O6—Ba	162.39 (18)	O6—C6—Ba—O17	−60.19 (13)
O4—Cr1—O6—C6	−102.15 (16)	C5—C6—Ba—O17	−156.6 (6)
O13—Cr1—O6—C6	166.64 (16)	O6—C6—Ba—O5	−166.2 (2)
O13ⁱ—Cr1—O6—C6	83.10 (16)	C5—C6—Ba—O5	97.4 (6)
O2—Cr1—O6—C6	6.3 (3)	O5—C6—Ba—O2ⁱ	−156.60 (14)
N1—Cr1—O6—C6	−17.63 (16)	O6—C6—Ba—O2ⁱ	37.23 (13)
Cr1ⁱ—Cr1—O6—C6	124.68 (15)	C5—C6—Ba—O2ⁱ	−59.2 (5)
O4—Cr1—O6—Ba	124.21 (12)	O5—C6—Ba—O6	166.2 (2)
O13—Cr1—O6—Ba	33.00 (12)	C5—C6—Ba—O6	−96.4 (6)
O13ⁱ—Cr1—O6—Ba	−50.53 (12)	O5—C6—Ba—O5ⁱⁱⁱ	37.13 (15)
O2—Cr1—O6—Ba	−127.3 (2)	O6—C6—Ba—O5ⁱⁱⁱ	−129.05 (13)
N1—Cr1—O6—Ba	−151.27 (13)	C5—C6—Ba—O5ⁱⁱⁱ	134.5 (5)
Cr1ⁱ—Cr1—O6—Ba	−8.96 (11)	O5—C6—Ba—O1ⁱ	172.57 (12)
O7—C8—O8—Cr2	−170.76 (18)	O6—C6—Ba—O1ⁱ	6.40 (14)
C7—C8—O8—Cr2	11.2 (2)	C5—C6—Ba—O1ⁱ	−90.0 (5)
O14—Cr2—O8—C8	−89.64 (16)	O5—C6—Ba—C2ⁱ	−172.06 (13)
O10—Cr2—O8—C8	0.4 (3)	O6—C6—Ba—C2ⁱ	21.77 (14)
O14ⁱⁱ—Cr2—O8—C8	−173.24 (15)	C5—C6—Ba—C2ⁱ	−74.7 (5)

Symmetry codes: (i) −x−1, −y+1, −z; (ii) −x−1, −y, −z+1; (iii) −x, −y+1, −z; (iv) −x−1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O15—H15A···O17ⁱⁱⁱ	0.80 (3)	2.18 (3)	2.955 (3)	164 (3)
O15—H15B···O20^v	0.76 (3)	2.08 (4)	2.822 (3)	169 (3)
O16—H16A···O7ⁱⁱⁱ	0.76 (3)	2.11 (3)	2.820 (3)	155 (3)
O16—H16B···O18^vi	0.79 (3)	2.56 (3)	3.015 (3)	119 (3)
O16—H16B···O18	0.79 (3)	2.26 (3)	2.909 (3)	140 (3)
O16—H16B···O18^vi	0.79 (3)	2.56 (3)	3.015 (3)	119 (3)
O17—H17A···O7ⁱⁱⁱ	0.79 (3)	2.05 (3)	2.835 (3)	172 (3)
O17—H17B···O19	0.80 (3)	1.96 (3)	2.759 (3)	175 (3)
O18—H18A···O9^iv	0.78 (3)	2.05 (4)	2.793 (3)	161 (3)
O18—H18B···O8^vii	0.81 (3)	2.16 (4)	2.967 (3)	174 (3)
O19—H19A···O20	0.79 (3)	2.00 (4)	2.784 (3)	168 (3)
O19—H19B···O13	0.82 (3)	2.08 (4)	2.884 (3)	168 (3)
O20—H20A···O3^viii	0.81 (3)	2.00 (3)	2.807 (3)	171 (3)
O20—H20B···O3	0.77 (3)	2.12 (3)	2.887 (3)	172 (3)
O20—H20B···O4	0.77 (3)	2.54 (3)	3.110 (3)	132 (3)
O13—H13···O12ⁱ	0.71 (3)	2.09 (3)	2.772 (2)	163 (3)
O14—H14···O19^ix	0.72 (3)	2.01 (3)	2.721 (2)	171 (4)

Symmetry codes: (i) −x−1, −y+1, −z; (iii) −x, −y+1, −z; (iv) −x−1, −y+1, −z+1; (v) x, y, z+1; (vi) −x, −y+2, −z; (vii) x, y+1, z; (viii) −x, −y+1, −z−1; (ix) x, y−1, z+1.

Distance of Cr and N from CCOO planes (Å) top

CCOO Plane	Cr distance	N distance
C1/C2/O1/O2	-0.060 (5)	-0.192 (6)
C3/C4/O3/O4	-0.354 (5)	0.188 (6)
C7/C8/O6/O7	0.010 (5)	-0.095 (6)
C9/C10/O8/O9	0.011 (5)	-0.495 (6)

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.

E-mail address*
Repeat e-mail address* (for error checking)

Format*	PDF (US $40)
	HTML (US $40)
	PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number (non-UK EC countries only)
Country*

Terms and conditions of use
Contact us

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page