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The title coordination polymers show different degrees of deprotonation of the disiloxane-di­carboxyl­ate bridging ligands: both contain tetra­gonally distorted trans-NiN4O2 octa­hedra.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989020002327/hb7892sup1.cif
Contains datablocks I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989020002327/hb7892Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989020002327/hb7892IIsup3.hkl
Contains datablock II

CCDC references: 1985068; 1985067

Key indicators

Structure: I
  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.009 Å
  • Disorder in main residue
  • R factor = 0.065
  • wR factor = 0.143
  • Data-to-parameter ratio = 24.0
Structure: II
  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](C-C) = 0.009 Å
  • Disorder in main residue
  • R factor = 0.050
  • wR factor = 0.115
  • Data-to-parameter ratio = 26.2

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level C PLAT220_ALERT_2_C NonSolvent Resd 1 C Ueq(max) / Ueq(min) Range 3.9 Ratio PLAT220_ALERT_2_C NonSolvent Resd 1 O Ueq(max) / Ueq(min) Range 3.2 Ratio PLAT222_ALERT_3_C NonSolvent Resd 1 H Uiso(max)/Uiso(min) Range 5.8 Ratio PLAT234_ALERT_4_C Large Hirshfeld Difference Si1 --C10 . 0.17 Ang. PLAT242_ALERT_2_C Low MainMol Ueq as Compared to Neighbors of Si1 Check PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.4 Note PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.0095 Ang. PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ...... 8.662 Check PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ...... 2.668 Check PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L= 0.595 24 Report
Alert level G PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 1 Info PLAT005_ALERT_5_G No Embedded Refinement Details Found in the CIF Please Do ! PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 2 Report PLAT230_ALERT_2_G Hirshfeld Test Diff for Si1 --O3 . 6.3 s.u. PLAT230_ALERT_2_G Hirshfeld Test Diff for Si1 --C10X . 7.3 s.u. PLAT300_ALERT_4_G Atom Site Occupancy of O3 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C10 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C10X Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C11 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C11X Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H10A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H10B Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H10C Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H10D Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H10E Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H10F Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H11A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H11B Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H11C Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H11D Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H11E Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H11F Constrained at 0.5 Check PLAT301_ALERT_3_G Main Residue Disorder ..............(Resd 1 ) 15% Note PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF . # 16 Check O3 -SI1 -O3 3.665 1.555 1.555 38.80 Deg. PLAT793_ALERT_4_G Model has Chirality at N1 (Centro SPGR) S Verify PLAT793_ALERT_4_G Model has Chirality at N2 (Centro SPGR) R Verify PLAT794_ALERT_5_G Tentative Bond Valency for Ni1 (II) . 2.07 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 6 Note PLAT870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed .. ! Info PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still 36% Note PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 1 Note PLAT931_ALERT_5_G CIFcalcFCF Twin Law ( 1 0 0) Est.d BASF 0.37 Check
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 10 ALERT level C = Check. Ensure it is not caused by an omission or oversight 32 ALERT level G = General information/check it is not something unexpected 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 9 ALERT type 3 Indicator that the structure quality may be low 22 ALERT type 4 Improvement, methodology, query or suggestion 5 ALERT type 5 Informative message, check
Datablock: II
Alert level B PLAT220_ALERT_2_B NonSolvent Resd 2 C Ueq(max) / Ueq(min) Range 6.5 Ratio PLAT934_ALERT_3_B Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 2 Check
Alert level C PLAT213_ALERT_2_C Atom C12 has ADP max/min Ratio ..... 3.1 prolat PLAT213_ALERT_2_C Atom C16 has ADP max/min Ratio ..... 3.6 prolat PLAT213_ALERT_2_C Atom C4 has ADP max/min Ratio ..... 3.1 prolat PLAT220_ALERT_2_C NonSolvent Resd 1 C Ueq(max) / Ueq(min) Range 4.9 Ratio PLAT222_ALERT_3_C NonSolvent Resd 1 H Uiso(max)/Uiso(min) Range 4.8 Ratio PLAT222_ALERT_3_C NonSolvent Resd 2 H Uiso(max)/Uiso(min) Range 5.7 Ratio PLAT234_ALERT_4_C Large Hirshfeld Difference N3 --C16 . 0.19 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference N4 --C13 . 0.18 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference C12 --C13_c . 0.19 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference C13 --C12_c . 0.19 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference Si1 --C10 . 0.18 Ang. PLAT241_ALERT_2_C High MainMol Ueq as Compared to Neighbors of C15 Check PLAT241_ALERT_2_C High MainMol Ueq as Compared to Neighbors of C16 Check PLAT242_ALERT_2_C Low MainMol Ueq as Compared to Neighbors of Ni2 Check PLAT242_ALERT_2_C Low MainMol Ueq as Compared to Neighbors of N3 Check PLAT242_ALERT_2_C Low MainMol Ueq as Compared to Neighbors of N4 Check PLAT242_ALERT_2_C Low MainMol Ueq as Compared to Neighbors of Si1 Check PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.3 Note PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.5 Note PLAT260_ALERT_2_C Large Average Ueq of Residue Including Cl1 0.134 Check PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.00867 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H2C ..O8 . 2.65 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 Note C22 H49 N4 Ni O5 Si2 PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ...... 2.834 Check PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L= 0.595 25 Report PLAT918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) . 1 Check
Alert level G PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 1 Info PLAT005_ALERT_5_G No Embedded Refinement Details Found in the CIF Please Do ! PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 6 Report PLAT244_ALERT_4_G Low Solvent Ueq as Compared to Neighbors of Cl1 Check PLAT300_ALERT_4_G Atom Site Occupancy of O6 Constrained at 0.25 Check PLAT300_ALERT_4_G Atom Site Occupancy of O6X Constrained at 0.25 Check PLAT300_ALERT_4_G Atom Site Occupancy of H5C Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of O3 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H2C Constrained at 0.5 Check PLAT301_ALERT_3_G Main Residue Disorder ..............(Resd 1 ) 3% Note PLAT301_ALERT_3_G Main Residue Disorder ..............(Resd 2 ) 3% Note PLAT396_ALERT_2_G Deviating Si-O-Si Angle From 150 for O3 137.4 Degree PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF . # 16 Check O3 -SI1 -O3 2.445 1.555 1.555 42.60 Deg. PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF . # 130 Check O6X -SI2 -O6X 2.654 1.555 1.555 13.00 Deg. PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF . # 131 Check O6X -SI2 -O6 1.555 1.555 2.654 13.00 Deg. PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF . # 132 Check O6X -SI2 -O6 2.654 1.555 2.654 17.00 Deg. PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle(s) in CIF . # 139 Check O6 -SI2 -O6 1.555 1.555 2.654 26.90 Deg. PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2 Note C22 H49 N4 Ni O5 Si2 PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 3 Note Cl O4 PLAT793_ALERT_4_G Model has Chirality at N1 (Centro SPGR) R Verify PLAT793_ALERT_4_G Model has Chirality at N2 (Centro SPGR) S Verify PLAT793_ALERT_4_G Model has Chirality at N3 (Centro SPGR) S Verify PLAT793_ALERT_4_G Model has Chirality at N4 (Centro SPGR) R Verify PLAT794_ALERT_5_G Tentative Bond Valency for Ni1 (II) . 2.08 Info PLAT794_ALERT_5_G Tentative Bond Valency for Ni2 (II) . 2.11 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 7 Note PLAT870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed .. ! Info PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 2 Note PLAT931_ALERT_5_G CIFcalcFCF Twin Law ( 1 0 0) Est.d BASF 0.33 Check
0 ALERT level A = Most likely a serious problem - resolve or explain 2 ALERT level B = A potentially serious problem, consider carefully 26 ALERT level C = Check. Ensure it is not caused by an omission or oversight 29 ALERT level G = General information/check it is not something unexpected 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 15 ALERT type 2 Indicator that the structure model may be wrong or deficient 11 ALERT type 3 Indicator that the structure quality may be low 25 ALERT type 4 Improvement, methodology, query or suggestion 6 ALERT type 5 Informative message, check

Computing details top

For both structures, data collection: CrysAlis PRO (Agilent, 2014); cell refinement: CrysAlis PRO (Agilent, 2014); data reduction: CrysAlis PRO (Agilent, 2014). Program(s) used to solve structure: SIR2008 (Burla et al., 2007) for (I); SHELXT (Sheldrick, 2015a) for (II). For both structures, program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: Mercury (Macrae et al., 2020); software used to prepare material for publication: publCIF (Westrip, 2010).

catena-Poly[[(1,4,8,11-tetraazacyclotetradecane-κ4N1,N4,N8,N11)nickel(II)]-µ-1,3-bis(3-carboxylatopropyl)tetramethyldisiloxane-κ2O:O'] (I) top
Crystal data top
[Ni(C10H24O5Si2)(C12H24N4)]F(000) = 608
Mr = 563.53Dx = 1.260 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 13.033 (5) ÅCell parameters from 468 reflections
b = 12.877 (10) Åθ = 2.2–23.0°
c = 9.028 (3) ŵ = 0.77 mm1
β = 101.31 (3)°T = 173 K
V = 1485.7 (13) Å3Plate, clear light colourless
Z = 20.25 × 0.25 × 0.05 mm
Data collection top
Agilent Xcalibur, Eos
diffractometer
3957 independent reflections
Radiation source: Enhance (Mo) X-ray Source2499 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
Detector resolution: 16.1593 pixels mm-1θmax = 25.0°, θmin = 2.3°
ω scansh = 1515
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2014)
k = 1515
Tmin = 0.694, Tmax = 1.000l = 109
3957 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.065H-atom parameters constrained
wR(F2) = 0.143 w = 1/[σ2(Fo2) + (0.0618P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max < 0.001
3957 reflectionsΔρmax = 0.56 e Å3
165 parametersΔρmin = 0.61 e Å3
6 restraints
Special details top

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

Refinement. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni11.0000000.5000000.5000000.0224 (3)
Si10.51530 (16)0.4465 (2)0.1590 (4)0.0810 (8)
O10.8723 (3)0.4020 (3)0.4131 (4)0.0278 (10)
O20.9375 (4)0.2757 (3)0.2920 (5)0.0546 (13)
O30.4991 (12)0.4662 (10)0.0400 (11)0.090 (4)0.5
N11.1059 (4)0.4111 (4)0.4113 (5)0.0313 (13)
H11.0689060.3484030.3683830.038*
N21.0173 (4)0.4173 (4)0.6987 (5)0.0302 (12)
H20.9748050.3542920.6775400.036*
C11.1301 (5)0.4718 (5)0.2850 (7)0.047 (2)
H1A1.1613360.4272430.2193190.057*
H1B1.1796200.5263090.3230160.057*
C20.9705 (5)0.4810 (5)0.8028 (7)0.050 (2)
H2A1.0186010.5354730.8457110.060*
H2B0.9555520.4383640.8846040.060*
C31.1239 (5)0.3849 (5)0.7630 (7)0.051 (2)
H3A1.1239290.3447480.8539310.061*
H3B1.1671990.4458110.7907580.061*
C41.1691 (6)0.3211 (6)0.6537 (9)0.056 (2)
H4A1.1186920.2675780.6141580.067*
H4B1.2308810.2863560.7090930.067*
C51.1991 (5)0.3767 (5)0.5216 (8)0.050 (2)
H5A1.2417880.4366260.5579670.061*
H5B1.2406230.3306620.4718420.061*
C60.8685 (5)0.3154 (5)0.3510 (7)0.0354 (16)
C70.7696 (5)0.2514 (5)0.3470 (8)0.0449 (18)
H7A0.7789860.2087180.4371870.054*
H7B0.7605440.2051560.2606040.054*
C80.6702 (5)0.3156 (5)0.3376 (7)0.0403 (18)
H8A0.6135220.2699780.3508860.048*
H8B0.6808610.3654960.4196800.048*
C90.6386 (4)0.3731 (5)0.1896 (8)0.0517 (19)
H9A0.6341540.3230190.1083490.062*
H9B0.6944020.4211660.1805780.062*
C10X0.4972 (14)0.5342 (14)0.313 (2)0.139 (5)0.5
H10A0.5045950.4956020.4055130.209*0.5
H10B0.4285900.5644430.2894550.209*0.5
H10C0.5489030.5881870.3243620.209*0.5
C110.3986 (16)0.369 (2)0.171 (7)0.139 (5)0.5
H11A0.3405880.4141110.1734860.209*0.5
H11B0.4122870.3273710.2612060.209*0.5
H11C0.3821820.3240190.0844040.209*0.5
C100.5355 (15)0.5612 (13)0.283 (2)0.139 (5)0.5
H10D0.5816260.6090010.2473710.209*0.5
H10E0.5658980.5399970.3842360.209*0.5
H10F0.4694600.5943670.2827390.209*0.5
C11X0.4087 (17)0.3521 (18)0.156 (7)0.139 (5)0.5
H11D0.3426130.3857300.1211760.209*0.5
H11E0.4114080.3254330.2558710.209*0.5
H11F0.4165370.2960060.0889760.209*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0285 (5)0.0157 (5)0.0236 (5)0.0026 (6)0.0068 (5)0.0002 (6)
Si10.0406 (13)0.0755 (19)0.119 (2)0.0021 (12)0.0034 (15)0.0400 (17)
O10.029 (2)0.019 (3)0.035 (3)0.003 (2)0.0052 (18)0.0074 (19)
O20.046 (3)0.031 (3)0.091 (4)0.006 (2)0.023 (3)0.033 (3)
O30.103 (8)0.105 (14)0.043 (9)0.010 (10)0.031 (9)0.010 (6)
N10.037 (3)0.014 (3)0.046 (3)0.002 (3)0.017 (3)0.012 (2)
N20.045 (3)0.025 (3)0.019 (3)0.013 (3)0.001 (2)0.005 (2)
C10.070 (5)0.028 (5)0.056 (5)0.014 (4)0.042 (4)0.013 (3)
C20.077 (6)0.039 (6)0.040 (4)0.013 (4)0.026 (4)0.003 (4)
C30.060 (5)0.046 (5)0.040 (4)0.002 (4)0.007 (4)0.023 (4)
C40.041 (4)0.029 (5)0.089 (6)0.009 (4)0.009 (4)0.018 (4)
C50.038 (4)0.029 (5)0.085 (6)0.006 (4)0.016 (4)0.008 (4)
C60.034 (4)0.025 (5)0.046 (4)0.002 (3)0.003 (3)0.003 (3)
C70.038 (4)0.022 (5)0.074 (5)0.001 (3)0.009 (3)0.008 (4)
C80.032 (4)0.039 (5)0.050 (4)0.002 (3)0.007 (3)0.001 (3)
C90.034 (4)0.067 (5)0.053 (4)0.009 (4)0.006 (4)0.011 (4)
C10X0.039 (6)0.077 (7)0.295 (14)0.005 (5)0.016 (7)0.004 (9)
C110.039 (6)0.077 (7)0.295 (14)0.005 (5)0.016 (7)0.004 (9)
C100.039 (6)0.077 (7)0.295 (14)0.005 (5)0.016 (7)0.004 (9)
C11X0.039 (6)0.077 (7)0.295 (14)0.005 (5)0.016 (7)0.004 (9)
Geometric parameters (Å, º) top
Ni1—O12.113 (4)C3—H3B0.9700
Ni1—O1i2.113 (4)C3—C41.491 (9)
Ni1—N12.071 (4)C4—H4A0.9700
Ni1—N1i2.071 (4)C4—H4B0.9700
Ni1—N22.060 (4)C4—C51.508 (9)
Ni1—N2i2.060 (4)C5—H5A0.9700
Si1—O31.785 (11)C5—H5B0.9700
Si1—O3ii1.541 (13)C6—C71.524 (9)
Si1—C91.838 (6)C7—H7A0.9700
Si1—C10X1.842 (7)C7—H7B0.9700
Si1—C111.842 (7)C7—C81.525 (8)
Si1—C101.842 (7)C8—H8A0.9700
Si1—C11X1.842 (7)C8—H8B0.9700
O1—C61.245 (7)C8—C91.512 (8)
O2—C61.242 (7)C9—H9A0.9700
O3—O3ii1.13 (2)C9—H9B0.9700
N1—H10.9800C10X—H10A0.9600
N1—C11.467 (7)C10X—H10B0.9600
N1—C51.479 (7)C10X—H10C0.9600
N2—H20.9800C11—H11A0.9600
N2—C21.467 (7)C11—H11B0.9600
N2—C31.459 (7)C11—H11C0.9600
C1—H1A0.9700C10—H10D0.9600
C1—H1B0.9700C10—H10E0.9600
C1—C2i1.519 (8)C10—H10F0.9600
C2—H2A0.9700C11X—H11D0.9600
C2—H2B0.9700C11X—H11E0.9600
C3—H3A0.9700C11X—H11F0.9600
O1i—Ni1—O1180.0N2—C3—C4111.3 (5)
N1—Ni1—O193.58 (17)H3A—C3—H3B108.0
N1i—Ni1—O186.42 (17)C4—C3—H3A109.4
N1—Ni1—O1i86.42 (17)C4—C3—H3B109.4
N1i—Ni1—O1i93.58 (17)C3—C4—H4A108.0
N1—Ni1—N1i180.0C3—C4—H4B108.0
N2i—Ni1—O192.40 (16)C3—C4—C5117.3 (6)
N2—Ni1—O1i92.40 (16)H4A—C4—H4B107.2
N2—Ni1—O187.60 (16)C5—C4—H4A108.0
N2i—Ni1—O1i87.60 (16)C5—C4—H4B108.0
N2—Ni1—N1i85.21 (19)N1—C5—C4111.6 (5)
N2i—Ni1—N1i94.79 (19)N1—C5—H5A109.3
N2—Ni1—N194.79 (19)N1—C5—H5B109.3
N2i—Ni1—N185.21 (19)C4—C5—H5A109.3
N2i—Ni1—N2180.0 (2)C4—C5—H5B109.3
O3ii—Si1—O338.8 (7)H5A—C5—H5B108.0
O3—Si1—C998.7 (5)O1—C6—C7117.0 (6)
O3ii—Si1—C9117.6 (6)O2—C6—O1126.5 (6)
O3ii—Si1—C10X93.6 (8)O2—C6—C7116.5 (6)
O3—Si1—C10X131.7 (9)C6—C7—H7A108.7
O3—Si1—C11102 (2)C6—C7—H7B108.7
O3ii—Si1—C11116.7 (16)C6—C7—C8114.4 (5)
O3—Si1—C10118.2 (9)H7A—C7—H7B107.6
O3ii—Si1—C1079.8 (9)C8—C7—H7A108.7
O3—Si1—C11X98 (2)C8—C7—H7B108.7
O3ii—Si1—C11X118.8 (18)C7—C8—H8A108.9
C9—Si1—C10X116.1 (7)C7—C8—H8B108.9
C9—Si1—C11114.8 (10)H8A—C8—H8B107.7
C9—Si1—C10107.7 (7)C9—C8—C7113.3 (5)
C9—Si1—C11X107.3 (9)C9—C8—H8A108.9
C11—Si1—C10X93.4 (18)C9—C8—H8B108.9
C11X—Si1—C10123.8 (18)Si1—C9—H9A107.9
C6—O1—Ni1131.4 (4)Si1—C9—H9B107.9
Si1ii—O3—Si1141.2 (7)C8—C9—Si1117.6 (4)
O3ii—O3—Si158.8 (11)C8—C9—H9A107.9
O3ii—O3—Si1ii82.4 (14)C8—C9—H9B107.9
Ni1—N1—H1107.2H9A—C9—H9B107.2
C1—N1—Ni1105.5 (4)Si1—C10X—H10A109.5
C1—N1—H1107.2Si1—C10X—H10B109.5
C1—N1—C5114.1 (5)Si1—C10X—H10C109.5
C5—N1—Ni1115.3 (4)H10A—C10X—H10B109.5
C5—N1—H1107.2H10A—C10X—H10C109.5
Ni1—N2—H2107.3H10B—C10X—H10C109.5
C2—N2—Ni1106.3 (4)Si1—C11—H11A109.5
C2—N2—H2107.3Si1—C11—H11B109.5
C3—N2—Ni1115.3 (4)Si1—C11—H11C109.5
C3—N2—H2107.3H11A—C11—H11B109.5
C3—N2—C2112.9 (5)H11A—C11—H11C109.5
N1—C1—H1A109.9H11B—C11—H11C109.5
N1—C1—H1B109.9Si1—C10—H10D109.5
N1—C1—C2i108.9 (5)Si1—C10—H10E109.5
H1A—C1—H1B108.3Si1—C10—H10F109.5
C2i—C1—H1A109.9H10D—C10—H10E109.5
C2i—C1—H1B109.9H10D—C10—H10F109.5
N2—C2—C1i108.3 (5)H10E—C10—H10F109.5
N2—C2—H2A110.0Si1—C11X—H11D109.5
N2—C2—H2B110.0Si1—C11X—H11E109.5
C1i—C2—H2A110.0Si1—C11X—H11F109.5
C1i—C2—H2B110.0H11D—C11X—H11E109.5
H2A—C2—H2B108.4H11D—C11X—H11F109.5
N2—C3—H3A109.4H11E—C11X—H11F109.5
N2—C3—H3B109.4
Ni1—O1—C6—O218.8 (10)C6—C7—C8—C967.1 (7)
Ni1—O1—C6—C7161.1 (4)C7—C8—C9—Si1176.0 (4)
Ni1—N1—C1—C2i41.9 (5)C9—Si1—O3—Si1ii123.8 (15)
Ni1—N1—C5—C453.8 (7)C9—Si1—O3—O3ii123.8 (15)
Ni1—N2—C2—C1i41.2 (5)C10X—Si1—O3—Si1ii13 (2)
Ni1—N2—C3—C457.1 (7)C10X—Si1—O3—O3ii13 (2)
O1—C6—C7—C831.8 (8)C10X—Si1—C9—C849.5 (9)
O2—C6—C7—C8148.4 (6)C11—Si1—O3—Si1ii118.5 (18)
O3ii—Si1—O3—Si1ii0.003 (1)C11—Si1—O3—O3ii118.5 (18)
O3—Si1—C9—C8165.0 (7)C11—Si1—C9—C858 (2)
O3ii—Si1—C9—C8159.0 (6)C10—Si1—O3—Si1ii8.3 (19)
N2—C3—C4—C572.9 (8)C10—Si1—O3—O3ii8.3 (19)
C1—N1—C5—C4176.2 (5)C10—Si1—C9—C871.5 (10)
C2—N2—C3—C4179.6 (5)C11X—Si1—O3—Si1ii127.1 (18)
C3—N2—C2—C1i168.6 (5)C11X—Si1—O3—O3ii127.1 (18)
C3—C4—C5—N171.1 (8)C11X—Si1—C9—C864 (2)
C5—N1—C1—C2i169.5 (5)
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O20.981.962.845 (6)150
N2—H2···O2iii0.982.072.883 (6)139
Symmetry code: (iii) x, y+1/2, z+1/2.
catena-Poly[[[(1,4,8,11-tetraazacyclotetradecane-κ4N1,N4,N8,N11)nickel(II)]-µ-4-({[(3-carboxypropyl)dimethylsilyl]oxy}dimethylsilyl)butanoato-κ2O:O'] perchlorate] (II) top
Crystal data top
[Ni(C10H25O5Si2)(C12H24N4)]ClO4Z = 2
Mr = 663.99F(000) = 708
Triclinic, P1Dx = 1.296 Mg m3
a = 9.3815 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.9009 (8) ÅCell parameters from 2033 reflections
c = 14.7604 (10) Åθ = 1.7–24.6°
α = 99.309 (5)°µ = 0.77 mm1
β = 100.343 (6)°T = 200 K
γ = 99.232 (6)°Block, clear light colourless
V = 1700.9 (2) Å30.45 × 0.35 × 0.30 mm
Data collection top
Agilent Xcalibur, Eos
diffractometer
9606 independent reflections
Radiation source: Enhance (Mo) X-ray Source5769 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.063
Detector resolution: 16.1593 pixels mm-1θmax = 25.0°, θmin = 2.0°
ω scansh = 1111
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2014)
k = 1515
Tmin = 0.889, Tmax = 1.000l = 1717
9606 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.050H-atom parameters constrained
wR(F2) = 0.115 w = 1/[σ2(Fo2) + (0.0451P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.002
9606 reflectionsΔρmax = 0.51 e Å3
367 parametersΔρmin = 0.44 e Å3
7 restraints
Special details top

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

Refinement. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.0000000.0000000.0000000.0241 (2)
Si10.3977 (2)0.55987 (11)0.05469 (15)0.0729 (6)
O10.1184 (3)0.1542 (2)0.0727 (2)0.0310 (8)
O20.0826 (3)0.1583 (2)0.2165 (2)0.0339 (8)
H2C0.0349500.1966530.2433670.051*0.5
O30.5535 (8)0.5084 (6)0.0332 (5)0.061 (3)0.5
N10.1859 (4)0.0236 (3)0.0499 (3)0.0408 (11)
H10.1571260.0876840.0998640.049*
N20.0809 (4)0.0725 (3)0.1075 (3)0.0390 (11)
H20.1280110.0149550.1616390.047*
C10.2858 (6)0.0494 (5)0.0295 (4)0.065 (2)
H1A0.3353370.0159690.0737020.078*
H1B0.3604800.0838400.0063360.078*
C20.1992 (7)0.1219 (4)0.0773 (4)0.0649 (19)
H2A0.1569440.1897710.0346190.078*
H2B0.2636740.1356050.1313690.078*
C30.0282 (7)0.1448 (4)0.1388 (4)0.0634 (18)
H3A0.0714510.2061810.0884460.076*
H3B0.0208550.1707240.1918010.076*
C40.1501 (7)0.0909 (4)0.1671 (4)0.068 (2)
H4A0.1044050.0251150.2119110.081*
H4B0.2059700.1371980.1994620.081*
C50.2570 (6)0.0641 (4)0.0893 (4)0.0608 (18)
H5A0.3399870.0432880.1134870.073*
H5B0.2947110.1271960.0399650.073*
C60.1332 (4)0.2035 (3)0.1537 (3)0.0254 (11)
C70.2146 (5)0.3171 (3)0.1832 (3)0.0378 (13)
H7A0.3033790.3194480.2293840.045*
H7B0.1533200.3588660.2140360.045*
C80.2580 (5)0.3700 (3)0.1066 (3)0.0363 (12)
H8A0.3166580.3277040.0738690.044*
H8B0.1695080.3717820.0617030.044*
C90.3463 (5)0.4842 (3)0.1431 (3)0.0477 (14)
H9A0.2891820.5241860.1792020.057*
H9B0.4362490.4808980.1858400.057*
C100.2275 (11)0.5710 (6)0.0258 (5)0.168 (4)
H10A0.1918650.5056350.0714070.252*
H10B0.1533860.5837860.0095800.252*
H10C0.2488720.6294170.0572380.252*
C110.5003 (7)0.6957 (4)0.1124 (5)0.102 (3)
H11A0.4425420.7302990.1509110.153*
H11B0.5921870.6909550.1508290.153*
H11C0.5194600.7365390.0654950.153*
Ni20.0000000.5000000.5000000.0281 (2)
Si20.35316 (15)0.04647 (10)0.52679 (11)0.0404 (4)
O40.0305 (3)0.3297 (2)0.47284 (19)0.0333 (8)
O50.0840 (3)0.2890 (2)0.3576 (2)0.0376 (9)
H5C0.0959500.2352760.3241180.056*0.5
N30.1442 (6)0.5206 (3)0.4129 (4)0.0621 (15)
H30.1438420.4494520.3774160.075*
N40.1844 (5)0.4870 (3)0.3968 (4)0.0675 (16)
H40.2078150.4128790.3619740.081*
C120.2937 (7)0.5585 (5)0.4771 (6)0.094 (3)
H12A0.3701620.5456050.4426640.113*
H12B0.3090770.6348090.5014740.113*
C130.3020 (7)0.5012 (5)0.4435 (7)0.111 (4)
H13A0.2951150.5768200.4675920.133*
H13B0.3959950.4747370.3995170.133*
C140.1635 (10)0.5587 (5)0.3256 (6)0.112 (3)
H14A0.1512660.6328810.3564240.134*
H14B0.2518650.5423540.2761300.134*
C150.0318 (15)0.5454 (6)0.2821 (5)0.136 (4)
H15A0.0353280.5829990.2301290.163*
H15B0.0401020.4700130.2565700.163*
C160.1145 (11)0.5851 (5)0.3474 (6)0.116 (4)
H16A0.1177740.6570980.3804210.139*
H16B0.1911320.5886320.3111030.139*
C170.0036 (5)0.2625 (3)0.4108 (3)0.0278 (11)
C180.0724 (5)0.1463 (3)0.3978 (3)0.0287 (12)
H18A0.1329970.1238120.3348280.034*
H18B0.0061930.1056100.4015450.034*
C190.1664 (5)0.1164 (3)0.4662 (3)0.0359 (12)
H19A0.1080870.1408130.5296650.043*
H19B0.2490450.1531880.4603480.043*
C200.2255 (5)0.0035 (3)0.4507 (3)0.0373 (13)
H20A0.2767180.0281120.3856480.045*
H20B0.1420640.0390910.4605460.045*
C210.2725 (6)0.0094 (4)0.6529 (4)0.0706 (18)
H21A0.1807660.0135400.6704840.106*
H21B0.2551620.0861530.6633820.106*
H21C0.3398760.0156530.6901110.106*
C220.3997 (6)0.1939 (4)0.5079 (5)0.084 (2)
H22A0.4454380.2224610.4431220.126*
H22B0.3112130.2213700.5239120.126*
H22C0.4667090.2146500.5467890.126*
O6X0.493 (3)0.013 (5)0.497 (6)0.037 (3)*0.25
O60.510 (3)0.021 (4)0.4772 (12)0.037 (3)*0.25
Cl10.38292 (17)0.21590 (12)0.21055 (12)0.0683 (5)
O70.3941 (6)0.2883 (5)0.2826 (4)0.194 (3)
O80.2362 (5)0.2323 (4)0.1955 (4)0.1227 (19)
O90.4112 (6)0.1102 (4)0.2279 (4)0.147 (2)
O100.4768 (6)0.2161 (4)0.1271 (4)0.137 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0254 (4)0.0202 (4)0.0226 (5)0.0021 (4)0.0072 (4)0.0040 (3)
Si10.1134 (15)0.0274 (8)0.0967 (15)0.0056 (9)0.0774 (14)0.0135 (8)
O10.0404 (19)0.0256 (16)0.0206 (19)0.0064 (14)0.0113 (15)0.0065 (14)
O20.051 (2)0.0206 (16)0.030 (2)0.0038 (14)0.0228 (17)0.0013 (14)
O30.085 (7)0.051 (4)0.069 (8)0.020 (5)0.056 (5)0.020 (5)
N10.033 (2)0.038 (2)0.041 (3)0.005 (2)0.016 (2)0.017 (2)
N20.052 (3)0.026 (2)0.031 (3)0.006 (2)0.001 (2)0.0044 (18)
C10.028 (3)0.065 (4)0.081 (5)0.019 (3)0.006 (3)0.032 (4)
C20.072 (4)0.048 (3)0.058 (4)0.024 (3)0.022 (4)0.009 (3)
C30.119 (5)0.027 (3)0.032 (3)0.010 (3)0.006 (4)0.003 (2)
C40.106 (5)0.045 (3)0.036 (4)0.041 (3)0.039 (4)0.009 (3)
C50.059 (4)0.060 (4)0.051 (4)0.023 (3)0.036 (3)0.018 (3)
C60.026 (3)0.025 (2)0.023 (3)0.000 (2)0.008 (2)0.002 (2)
C70.053 (3)0.027 (3)0.027 (3)0.010 (2)0.018 (3)0.004 (2)
C80.048 (3)0.025 (2)0.033 (3)0.001 (2)0.016 (3)0.002 (2)
C90.056 (3)0.028 (3)0.053 (4)0.010 (2)0.022 (3)0.004 (2)
C100.274 (12)0.096 (6)0.091 (7)0.042 (7)0.030 (7)0.047 (5)
C110.075 (5)0.042 (4)0.192 (8)0.006 (3)0.039 (5)0.034 (4)
Ni20.0285 (5)0.0228 (4)0.0292 (5)0.0009 (4)0.0125 (4)0.0067 (4)
Si20.0330 (8)0.0396 (8)0.0503 (10)0.0047 (7)0.0090 (7)0.0156 (7)
O40.0421 (19)0.0242 (16)0.0334 (19)0.0031 (14)0.0212 (16)0.0061 (14)
O50.053 (2)0.0263 (17)0.033 (2)0.0013 (15)0.0258 (18)0.0061 (14)
N30.099 (4)0.026 (2)0.073 (4)0.007 (3)0.064 (3)0.002 (3)
N40.056 (3)0.043 (3)0.080 (4)0.016 (3)0.019 (3)0.027 (3)
C120.049 (4)0.056 (4)0.167 (7)0.010 (3)0.066 (5)0.033 (4)
C130.039 (4)0.062 (5)0.188 (10)0.014 (4)0.027 (5)0.048 (5)
C140.164 (8)0.055 (4)0.088 (6)0.040 (5)0.055 (6)0.004 (4)
C150.313 (15)0.067 (5)0.049 (5)0.084 (8)0.047 (8)0.019 (4)
C160.238 (11)0.045 (4)0.088 (7)0.012 (6)0.122 (7)0.001 (4)
C170.028 (3)0.028 (2)0.024 (3)0.005 (2)0.003 (2)0.000 (2)
C180.033 (3)0.018 (2)0.036 (3)0.003 (2)0.014 (2)0.001 (2)
C190.038 (3)0.031 (3)0.041 (3)0.004 (2)0.017 (3)0.003 (2)
C200.034 (3)0.035 (3)0.041 (3)0.003 (2)0.011 (3)0.002 (2)
C210.079 (4)0.088 (4)0.045 (4)0.017 (4)0.011 (3)0.017 (3)
C220.082 (5)0.048 (3)0.116 (6)0.012 (3)0.023 (4)0.021 (4)
Cl10.0571 (10)0.0599 (10)0.0695 (12)0.0139 (8)0.0151 (10)0.0111 (9)
O70.137 (5)0.163 (5)0.202 (6)0.019 (4)0.037 (4)0.146 (5)
O80.077 (3)0.154 (5)0.144 (5)0.026 (3)0.017 (3)0.050 (4)
O90.176 (6)0.079 (4)0.158 (5)0.006 (4)0.005 (5)0.016 (3)
O100.117 (4)0.143 (4)0.115 (4)0.037 (3)0.050 (4)0.006 (4)
Geometric parameters (Å, º) top
Ni1—O12.125 (2)Ni2—N42.054 (4)
Ni1—O1i2.125 (2)Ni2—N4iii2.054 (4)
Ni1—N1i2.058 (3)Si2—C201.864 (5)
Ni1—N12.058 (3)Si2—C211.855 (5)
Ni1—N2i2.060 (4)Si2—C221.845 (5)
Ni1—N22.060 (4)Si2—O6Xiv1.570 (19)
Si1—O31.757 (8)Si2—O6X1.651 (19)
Si1—O3ii1.626 (7)Si2—O6iv1.66 (2)
Si1—C91.837 (5)Si2—O61.632 (16)
Si1—C101.852 (9)O4—C171.245 (4)
Si1—C111.845 (5)O5—H5C0.8199
O1—C61.232 (4)O5—C171.280 (5)
O2—H2C0.8200N3—H30.9800
O2—C61.291 (5)N3—C121.502 (8)
O3—O3ii1.234 (13)N3—C161.393 (9)
N1—H10.9800N4—H40.9800
N1—C11.481 (6)N4—C131.422 (8)
N1—C51.475 (6)N4—C141.527 (9)
N2—H20.9800C12—H12A0.9700
N2—C21.467 (6)C12—H12B0.9700
N2—C31.461 (6)C12—C13iii1.502 (10)
C1—H1A0.9700C13—H13A0.9700
C1—H1B0.9700C13—H13B0.9700
C1—C2i1.486 (7)C14—H14A0.9700
C2—H2B0.9700C14—H14B0.9700
C2—H2A0.9700C14—C151.512 (11)
C3—H3A0.9700C15—H15A0.9700
C3—H3B0.9700C15—H15B0.9700
C3—C41.516 (7)C15—C161.488 (11)
C4—H4A0.9700C16—H16A0.9700
C4—H4B0.9700C16—H16B0.9700
C4—C51.507 (7)C20—H20A0.9700
C5—H5A0.9700C20—H20B0.9700
C5—H5B0.9700C20—C191.521 (5)
C6—C71.496 (5)C19—H19A0.9700
C7—H7A0.9700C19—H19B0.9700
C7—H7B0.9700C19—C181.512 (6)
C7—C81.496 (6)C18—H18A0.9700
C8—H8A0.9700C18—H18B0.9700
C8—H8B0.9700C18—C171.501 (5)
C8—C91.529 (5)C21—H21A0.9600
C9—H9A0.9700C21—H21B0.9600
C9—H9B0.9700C21—H21C0.9600
C10—H10A0.9600C22—H22A0.9600
C10—H10B0.9600C22—H22B0.9600
C10—H10C0.9600C22—H22C0.9600
C11—H11A0.9600O6X—O6Xiv0.38 (7)
C11—H11B0.9600O6—O6iv0.77 (5)
C11—H11C0.9600Cl1—O71.329 (4)
Ni2—O4iii2.131 (2)Cl1—O81.421 (5)
Ni2—O42.131 (2)Cl1—O91.420 (5)
Ni2—N3iii2.043 (4)Cl1—O101.380 (5)
Ni2—N32.043 (4)
O1—Ni1—O1i180.0N3iii—Ni2—N485.7 (2)
N1i—Ni1—O188.17 (12)N4—Ni2—O4iii91.33 (14)
N1i—Ni1—O1i91.83 (12)N4—Ni2—O488.67 (14)
N1—Ni1—O1i88.17 (12)N4iii—Ni2—O491.33 (14)
N1—Ni1—O191.83 (12)N4iii—Ni2—O4iii88.67 (14)
N1i—Ni1—N1180.0N4—Ni2—N4iii180.0
N1i—Ni1—N285.82 (17)C21—Si2—C20111.6 (2)
N1—Ni1—N2i85.82 (17)C22—Si2—C20110.6 (2)
N1i—Ni1—N2i94.18 (17)C22—Si2—C21109.6 (3)
N1—Ni1—N294.18 (17)O6Xiv—Si2—C20113.4 (14)
N2—Ni1—O1i87.38 (12)O6X—Si2—C20102.5 (13)
N2i—Ni1—O187.38 (12)O6X—Si2—C21107 (3)
N2—Ni1—O192.62 (12)O6Xiv—Si2—C21107 (3)
N2i—Ni1—O1i92.62 (12)O6X—Si2—C22116 (2)
N2—Ni1—N2i180.0O6Xiv—Si2—C22104 (2)
O3ii—Si1—O342.6 (4)O6Xiv—Si2—O6X13 (3)
O3ii—Si1—C9115.6 (3)O6X—Si2—O6iv13 (3)
O3—Si1—C9100.2 (3)O6Xiv—Si2—O6iv17 (2)
O3—Si1—C10131.5 (4)O6iv—Si2—C20111.2 (17)
O3ii—Si1—C1089.4 (4)O6—Si2—C20103.5 (15)
O3ii—Si1—C11121.3 (4)O6—Si2—C21120.4 (6)
O3—Si1—C1195.7 (3)O6iv—Si2—C2194.3 (5)
C9—Si1—C10109.0 (3)O6—Si2—C22100.3 (19)
C9—Si1—C11110.1 (3)O6iv—Si2—C22118.5 (19)
C11—Si1—C10108.8 (3)O6—Si2—O6iv26.9 (17)
C6—O1—Ni1132.9 (3)C17—O4—Ni2133.8 (3)
C6—O2—H2C109.8C17—O5—H5C109.9
Si1ii—O3—Si1137.4 (4)Ni2—N3—H3106.9
O3ii—O3—Si163.0 (6)C12—N3—Ni2105.1 (4)
O3ii—O3—Si1ii74.4 (7)C12—N3—H3106.9
Ni1—N1—H1107.4C16—N3—Ni2117.3 (4)
C1—N1—Ni1105.0 (3)C16—N3—H3106.9
C1—N1—H1107.4C16—N3—C12113.2 (6)
C5—N1—Ni1116.2 (3)Ni2—N4—H4106.8
C5—N1—H1107.4C13—N4—Ni2106.5 (4)
C5—N1—C1113.1 (4)C13—N4—H4106.8
Ni1—N2—H2106.7C13—N4—C14115.0 (6)
C2—N2—Ni1105.7 (3)C14—N4—Ni2114.4 (4)
C2—N2—H2106.7C14—N4—H4106.8
C3—N2—Ni1116.1 (3)N3—C12—H12A109.9
C3—N2—H2106.7N3—C12—H12B109.9
C3—N2—C2114.2 (4)N3—C12—C13iii108.8 (5)
N1—C1—H1A109.7H12A—C12—H12B108.3
N1—C1—H1B109.7C13iii—C12—H12A109.9
N1—C1—C2i109.7 (4)C13iii—C12—H12B109.9
H1A—C1—H1B108.2N4—C13—C12iii109.6 (6)
C2i—C1—H1A109.7N4—C13—H13A109.8
C2i—C1—H1B109.7N4—C13—H13B109.8
N2—C2—C1i109.8 (4)C12iii—C13—H13A109.8
N2—C2—H2B109.7C12iii—C13—H13B109.8
N2—C2—H2A109.7H13A—C13—H13B108.2
C1i—C2—H2B109.7N4—C14—H14A109.0
C1i—C2—H2A109.7N4—C14—H14B109.0
H2B—C2—H2A108.2H14A—C14—H14B107.8
N2—C3—H3A109.1C15—C14—N4113.0 (6)
N2—C3—H3B109.1C15—C14—H14A109.0
N2—C3—C4112.3 (4)C15—C14—H14B109.0
H3A—C3—H3B107.9C14—C15—H15A108.5
C4—C3—H3A109.1C14—C15—H15B108.5
C4—C3—H3B109.1H15A—C15—H15B107.5
C3—C4—H4A108.1C16—C15—C14115.0 (6)
C3—C4—H4B108.1C16—C15—H15A108.5
H4A—C4—H4B107.3C16—C15—H15B108.5
C5—C4—C3116.7 (4)N3—C16—C15113.1 (7)
C5—C4—H4A108.1N3—C16—H16A109.0
C5—C4—H4B108.1N3—C16—H16B109.0
N1—C5—C4111.4 (4)C15—C16—H16A109.0
N1—C5—H5A109.4C15—C16—H16B109.0
N1—C5—H5B109.4H16A—C16—H16B107.8
C4—C5—H5A109.4Si2—C20—H20A108.3
C4—C5—H5B109.4Si2—C20—H20B108.3
H5A—C5—H5B108.0H20A—C20—H20B107.4
O1—C6—O2121.4 (4)C19—C20—Si2115.9 (3)
O1—C6—C7120.8 (4)C19—C20—H20A108.3
O2—C6—C7117.7 (4)C19—C20—H20B108.3
C6—C7—H7A108.3C20—C19—H19A109.0
C6—C7—H7B108.3C20—C19—H19B109.0
H7A—C7—H7B107.4H19A—C19—H19B107.8
C8—C7—C6116.0 (4)C18—C19—C20113.1 (3)
C8—C7—H7A108.3C18—C19—H19A109.0
C8—C7—H7B108.3C18—C19—H19B109.0
C7—C8—H8A109.0C19—C18—H18A108.1
C7—C8—H8B109.0C19—C18—H18B108.1
C7—C8—C9112.8 (4)H18A—C18—H18B107.3
H8A—C8—H8B107.8C17—C18—C19116.7 (3)
C9—C8—H8A109.0C17—C18—H18A108.1
C9—C8—H8B109.0C17—C18—H18B108.1
Si1—C9—H9A108.1O4—C17—O5121.9 (4)
Si1—C9—H9B108.1O4—C17—C18120.1 (4)
C8—C9—Si1116.8 (3)O5—C17—C18118.0 (3)
C8—C9—H9A108.1Si2—C21—H21A109.5
C8—C9—H9B108.1Si2—C21—H21B109.5
H9A—C9—H9B107.3Si2—C21—H21C109.5
Si1—C10—H10A109.5H21A—C21—H21B109.5
Si1—C10—H10B109.5H21A—C21—H21C109.5
Si1—C10—H10C109.5H21B—C21—H21C109.5
H10A—C10—H10B109.5Si2—C22—H22A109.5
H10A—C10—H10C109.5Si2—C22—H22B109.5
H10B—C10—H10C109.5Si2—C22—H22C109.5
Si1—C11—H11A109.5H22A—C22—H22B109.5
Si1—C11—H11B109.5H22A—C22—H22C109.5
Si1—C11—H11C109.5H22B—C22—H22C109.5
H11A—C11—H11B109.5Si2iv—O6X—Si2167 (3)
H11A—C11—H11C109.5O6Xiv—O6X—Si2iv96 (6)
H11B—C11—H11C109.5O6Xiv—O6X—Si271 (6)
O4—Ni2—O4iii180.00 (3)Si2—O6—Si2iv153.1 (17)
N3iii—Ni2—O4iii94.96 (13)O6iv—O6—Si278 (2)
N3—Ni2—O494.96 (13)O7—Cl1—O8110.3 (3)
N3iii—Ni2—O485.04 (13)O7—Cl1—O9112.0 (4)
N3—Ni2—O4iii85.04 (13)O7—Cl1—O10114.2 (4)
N3iii—Ni2—N3180.0O9—Cl1—O8105.3 (3)
N3iii—Ni2—N4iii94.3 (2)O10—Cl1—O8107.7 (4)
N3—Ni2—N494.3 (2)O10—Cl1—O9106.8 (3)
N3—Ni2—N4iii85.7 (2)
Ni1—O1—C6—O27.2 (6)Ni2—N4—C14—C1552.9 (7)
Ni1—O1—C6—C7174.5 (3)Si2—C20—C19—C18176.0 (3)
Ni1—N1—C1—C2i40.9 (4)N4—C14—C15—C1668.4 (9)
Ni1—N1—C5—C456.2 (5)C12—N3—C16—C15178.2 (6)
Ni1—N2—C2—C1i39.8 (4)C13—N4—C14—C15176.6 (6)
Ni1—N2—C3—C455.3 (5)C14—N4—C13—C12iii169.9 (5)
O1—C6—C7—C87.7 (6)C14—C15—C16—N371.7 (8)
O2—C6—C7—C8174.0 (4)C16—N3—C12—C13iii168.2 (5)
O3ii—Si1—O3—Si1ii0.001 (2)C20—Si2—O6X—Si2iv148 (28)
O3—Si1—C9—C881.0 (4)C20—Si2—O6X—O6Xiv148 (28)
O3ii—Si1—C9—C839.0 (5)C20—Si2—O6—Si2iv110 (7)
N2—C3—C4—C570.0 (6)C20—Si2—O6—O6iv110 (7)
C1—N1—C5—C4177.7 (4)C20—C19—C18—C17177.2 (4)
C2—N2—C3—C4178.7 (4)C19—C18—C17—O43.3 (6)
C3—N2—C2—C1i168.7 (4)C19—C18—C17—O5175.7 (4)
C3—C4—C5—N170.1 (5)C21—Si2—C20—C1952.0 (4)
C5—N1—C1—C2i168.6 (4)C21—Si2—O6X—Si2iv95 (29)
C6—C7—C8—C9177.5 (4)C21—Si2—O6X—O6Xiv95 (29)
C7—C8—C9—Si1176.9 (4)C21—Si2—O6—Si2iv15 (9)
C9—Si1—O3—Si1ii116.9 (7)C21—Si2—O6—O6iv15 (9)
C9—Si1—O3—O3ii116.9 (7)C22—Si2—C20—C19174.3 (4)
C10—Si1—O3—Si1ii10.0 (10)C22—Si2—O6X—Si2iv27 (30)
C10—Si1—O3—O3ii10.0 (10)C22—Si2—O6X—O6Xiv27 (30)
C10—Si1—C9—C859.7 (5)C22—Si2—O6—Si2iv135 (8)
C11—Si1—O3—Si1ii131.5 (8)C22—Si2—O6—O6iv135 (8)
C11—Si1—O3—O3ii131.5 (8)O6Xiv—Si2—C20—C1970 (4)
C11—Si1—C9—C8179.0 (4)O6X—Si2—C20—C1962 (3)
Ni2—O4—C17—O516.3 (6)O6Xiv—Si2—O6X—Si2iv0.01 (14)
Ni2—O4—C17—C18164.8 (3)O6iv—Si2—C20—C1951.9 (12)
Ni2—N3—C12—C13iii39.0 (6)O6—Si2—C20—C1979.0 (15)
Ni2—N3—C16—C1559.1 (7)O6iv—Si2—O6—Si2iv0.006 (14)
Ni2—N4—C13—C12iii42.1 (6)
Symmetry codes: (i) x, y, z; (ii) x1, y1, z; (iii) x, y1, z1; (iv) x+1, y, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O20.982.513.225 (5)130
N1—H1···O80.982.453.315 (6)147
N2—H2···O20.982.383.143 (4)134
N3—H3···O50.982.012.901 (5)150
N4—H4···O70.982.183.012 (6)142
O2—H2C···O50.821.842.456 (4)131
O2—H2C···O80.822.653.260 (5)133
O5—H5C···O20.821.702.456 (4)151
Selected geometrical parameters of the complex cations (Å, °) top
III
Ni1—N12.071 (4)Ni1—N12.058 (3)Ni2—N32.043 (4)
Ni1—N22.060 (4)Ni1—N22.060 (4)Ni2—N42.054 (4)
Ni1—O12.113 (4)Ni1—O12.125 (2)Ni2—O42.131 (2)
N1—Ni1—N2i85.21 (19)N1—Ni1—N2ii85.82 (17)N3—Ni2—N4iii85.7 (2)
N1—Ni1—N294.79 (19)N1—Ni1—N294.18 (17)N3—Ni2—N494.3 (2)
Symmetry codes: (i) -x + 2, -y + 1, -z + 1; (ii) -x, -y, -z; (iii) -x, -y - 1, -z -1.
 

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