The asymmetric unit of the title compound [Cu8ICu2II(CN)4(NCS)8(C6H8N2)7], consists of six crystallographically independent Cu atoms, four thiocyanate anions and two cyanide anions, as well as four 2,6-dimethylpyrazine ligands. Two of the six Cu atoms and one of the four 2,6-dimethylpyrazine ligands are located on centres of inversion. The ligand on a special position is therefore disordered due to symmetry. Altogether there are two copper(II) and eight copper(I) cations in the formula unit. The copper(II) cations are each coordinated by four N atoms within a slightly distorted square-planar coordination. The copper(I) cations, on the other hand, are coordinated by four ligands or anions within distorted tetrahedra. From this arrangement, a three-dimensional coordination network is formed.
Supporting information
CCDC reference: 604972
Key indicators
- Single-crystal X-ray study
- T = 220 K
- Mean (C-C) = 0.015 Å
- Disorder in main residue
- R factor = 0.059
- wR factor = 0.126
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.94 Ratio
| Author Response: Some of the atoms shows relatively large displacement parameters
because of some disorder which cannot be resolved successfully. In addition,
the data are of low quality because of the very low diffraction power of this
small crystal. I have used practically the maximum measuring time
of about 6 days and I also tried to get larger crystals but without any success
Therefore, there is nothing what I can do in addition.
However, I am absolutely sure that the structure model is correct.
I have everything explained in detail in the experiment part and I think
Michael Bolte the co-editor will take care of it.
|
Alert level B
PLAT220_ALERT_2_B Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.62 Ratio
| Author Response: Some of the atoms shows relatively large displacement parameters
because of some disorder which cannot be resolved successfully. In addition,
the data are of low quality because of the very low diffraction power of this
small crystal. I have used practically the maximum measuring time
of about 6 days and I also tried to get larger crystals but without any success
Therefore, there is nothing what I can do in addition.
However, I am absolutely sure that the structure model is correct.
I have everything explained in detail in the experiment part and I think
Michael Bolte the co-editor will take care of it.
|
PLAT341_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 16
Alert level C
ABSTM02_ALERT_3_C The ratio of Tmax/Tmin expected RT(exp) is > 1.10
Absorption corrections should be applied.
Tmin and Tmax expected: 0.788 0.912
RT(exp) = 1.158
RINTA01_ALERT_3_C The value of Rint is greater than 0.10
Rint given 0.106
PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11
PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 49 Perc.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT057_ALERT_3_C Correction for Absorption Required RT(exp) ... 1.17
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT213_ALERT_2_C Atom N31 has ADP max/min Ratio ............. 3.40 prolat
PLAT213_ALERT_2_C Atom C16 has ADP max/min Ratio ............. 3.90 prolat
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.09 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N31
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C34
PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc.
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 35.00 A 3
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.40 Deg.
C35 -C31 -H31 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 12.40 Deg.
C36 -C34 -H34 1.555 1.555 1.555
1 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
18 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
9 ALERT type 2 Indicator that the structure model may be wrong or deficient
8 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXTL.
Tetra-µ
2-cyano-
κ8C:
N-µ
2-2,5-dimethylpyrazine-
κ2N:
N'-
hexakis(2,5-dimethylpyrazine-
κN)octa-µ
2-thiocyanato-
κ16N:
S- decacopper(I,II)
top
Crystal data top
[Cu10(CN)4(NCS)8(C6H8N2)7] | Z = 1 |
Mr = 1961.13 | F(000) = 980 |
Triclinic, P1 | Dx = 1.749 Mg m−3 |
a = 10.2406 (7) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.2211 (12) Å | Cell parameters from 8000 reflections |
c = 14.7809 (14) Å | θ = 3–50° |
α = 97.837 (11)° | µ = 3.07 mm−1 |
β = 109.463 (10)° | T = 220 K |
γ = 92.057 (10)° | Plate, red |
V = 1862.1 (3) Å3 | 0.08 × 0.08 × 0.03 mm |
Data collection top
Stoe IPDS-1 diffractometer | 3143 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.107 |
Graphite monochromator | θmax = 25.0°, θmin = 2.3° |
φ scans | h = −12→12 |
11439 measured reflections | k = −15→15 |
6451 independent reflections | l = −17→17 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.059 | H-atom parameters constrained |
wR(F2) = 0.126 | w = 1/[σ2(Fo2) + (0.0393P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.89 | (Δ/σ)max < 0.001 |
6451 reflections | Δρmax = 0.85 e Å−3 |
463 parameters | Δρmin = −0.80 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0015 (3) |
Special details top
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cu1 | 1.32809 (12) | 0.82344 (8) | 0.86389 (9) | 0.0295 (3) | |
Cu2 | 1.0000 | 1.0000 | 1.0000 | 0.0280 (4) | |
Cu3 | 0.5000 | 0.5000 | 1.0000 | 0.0292 (4) | |
Cu4 | 0.81470 (12) | 0.63714 (9) | 0.84493 (10) | 0.0360 (4) | |
Cu5 | 0.75140 (13) | 0.76216 (9) | 0.68637 (10) | 0.0360 (4) | |
Cu6 | 1.25651 (14) | 0.64163 (10) | 0.69705 (13) | 0.0529 (5) | |
S1 | 0.6927 (3) | 0.58009 (18) | 0.6656 (2) | 0.0317 (6) | |
C61 | 0.5349 (9) | 0.5913 (6) | 0.6719 (7) | 0.023 (2) | |
N61 | 0.4274 (8) | 0.6012 (6) | 0.6781 (6) | 0.035 (2) | |
S2 | 0.7838 (2) | 0.83457 (17) | 0.84905 (18) | 0.0259 (6) | |
C62 | 0.6244 (10) | 0.8345 (6) | 0.8586 (7) | 0.022 (2) | |
N62 | 0.5159 (8) | 0.8331 (5) | 0.8665 (6) | 0.0241 (18) | |
S3 | 1.2838 (2) | 0.63054 (16) | 0.86398 (18) | 0.0242 (5) | |
C63 | 1.1246 (9) | 0.6344 (6) | 0.8662 (6) | 0.0174 (19) | |
N63 | 1.0104 (8) | 0.6367 (5) | 0.8639 (6) | 0.0265 (19) | |
S4 | 1.2072 (2) | 0.81454 (17) | 0.68200 (19) | 0.0283 (6) | |
C64 | 1.0432 (10) | 0.7994 (6) | 0.6749 (7) | 0.022 (2) | |
N64 | 0.9268 (9) | 0.7888 (6) | 0.6687 (6) | 0.032 (2) | |
N51 | 0.6187 (8) | 0.5499 (5) | 0.9367 (6) | 0.0278 (19) | |
C51 | 0.6969 (10) | 0.5838 (6) | 0.9038 (7) | 0.025 (2) | |
N52 | 1.1375 (8) | 0.9284 (5) | 0.9628 (6) | 0.030 (2) | |
C52 | 1.2154 (10) | 0.8876 (6) | 0.9283 (7) | 0.027 (2) | |
N1 | 0.3530 (9) | 0.8737 (6) | 0.4523 (7) | 0.040 (2) | |
C1 | 0.4034 (11) | 0.9251 (7) | 0.5433 (8) | 0.031 (2) | |
C2 | 0.5150 (10) | 0.8927 (7) | 0.6121 (8) | 0.032 (2) | |
H2 | 0.5524 | 0.9331 | 0.6738 | 0.038* | |
N2 | 0.5728 (8) | 0.8048 (6) | 0.5943 (7) | 0.035 (2) | |
C3 | 0.5165 (10) | 0.7517 (7) | 0.5041 (8) | 0.036 (3) | |
H3 | 0.5518 | 0.6895 | 0.4886 | 0.043* | |
C4 | 0.4092 (11) | 0.7855 (7) | 0.4337 (8) | 0.040 (3) | |
C5 | 0.3368 (12) | 1.0190 (7) | 0.5670 (9) | 0.049 (3) | |
H5A | 0.3019 | 1.0518 | 0.5098 | 0.073* | |
H5B | 0.4048 | 1.0661 | 0.6187 | 0.073* | |
H5C | 0.2603 | 1.0000 | 0.5880 | 0.073* | |
C6 | 0.3574 (13) | 0.7308 (10) | 0.3292 (9) | 0.068 (4) | |
H6A | 0.2657 | 0.7508 | 0.2955 | 0.102* | |
H6B | 0.3523 | 0.6573 | 0.3285 | 0.102* | |
H6C | 0.4210 | 0.7493 | 0.2969 | 0.102* | |
N11 | 0.3282 (9) | 0.2057 (5) | 0.7503 (6) | 0.033 (2) | |
C11 | 0.3219 (11) | 0.2994 (7) | 0.7260 (8) | 0.032 (2) | |
C12 | 0.3771 (10) | 0.3840 (7) | 0.7980 (7) | 0.030 (2) | |
H12 | 0.3777 | 0.4493 | 0.7796 | 0.036* | |
N12 | 0.4308 (8) | 0.3760 (5) | 0.8949 (6) | 0.0264 (19) | |
C13 | 0.4296 (10) | 0.2803 (6) | 0.9162 (7) | 0.028 (2) | |
H13 | 0.4609 | 0.2711 | 0.9817 | 0.034* | |
C14 | 0.3838 (11) | 0.1949 (7) | 0.8447 (8) | 0.034 (2) | |
C15 | 0.2525 (14) | 0.3118 (8) | 0.6233 (8) | 0.054 (3) | |
H15A | 0.2910 | 0.2679 | 0.5822 | 0.080* | |
H15B | 0.2676 | 0.3826 | 0.6160 | 0.080* | |
H15C | 0.1536 | 0.2930 | 0.6044 | 0.080* | |
C16 | 0.3918 (14) | 0.0884 (7) | 0.8685 (8) | 0.056 (4) | |
H16A | 0.3234 | 0.0421 | 0.8163 | 0.084* | |
H16B | 0.3731 | 0.0869 | 0.9285 | 0.084* | |
H16C | 0.4841 | 0.0671 | 0.8761 | 0.084* | |
N21 | 0.9976 (8) | 1.2235 (5) | 0.7660 (6) | 0.0292 (19) | |
C21 | 0.9937 (9) | 1.1217 (7) | 0.7428 (7) | 0.026 (2) | |
C22 | 0.9914 (9) | 1.0580 (6) | 0.8085 (7) | 0.028 (2) | |
H22 | 0.9925 | 0.9872 | 0.7904 | 0.033* | |
N22 | 0.9876 (8) | 1.0923 (5) | 0.8974 (6) | 0.0266 (19) | |
C23 | 0.9874 (10) | 1.1948 (6) | 0.9191 (7) | 0.029 (2) | |
H23 | 0.9834 | 1.2229 | 0.9800 | 0.035* | |
C24 | 0.9928 (10) | 1.2598 (6) | 0.8537 (7) | 0.026 (2) | |
C25 | 0.9993 (11) | 1.0791 (7) | 0.6442 (7) | 0.036 (3) | |
H25A | 0.9328 | 1.1104 | 0.5947 | 0.055* | |
H25B | 0.9766 | 1.0055 | 0.6315 | 0.055* | |
H25C | 1.0921 | 1.0940 | 0.6430 | 0.055* | |
C26 | 0.9936 (13) | 1.3729 (7) | 0.8803 (9) | 0.053 (3) | |
H26A | 1.0732 | 1.4070 | 0.8718 | 0.079* | |
H26B | 0.9993 | 1.3890 | 0.9476 | 0.079* | |
H26C | 0.9088 | 1.3961 | 0.8388 | 0.079* | |
N31 | 1.0976 (11) | 0.5584 (8) | 0.5851 (13) | 0.088 (5) | |
C31 | 1.0068 (14) | 0.4883 (10) | 0.5922 (15) | 0.071 (5) | |
H31 | 1.0088 | 0.4773 | 0.6542 | 0.086* | 0.50 |
C34 | 1.0924 (15) | 0.5700 (10) | 0.4908 (17) | 0.085 (6) | |
H34 | 1.1566 | 0.6178 | 0.4829 | 0.102* | 0.50 |
C35 | 1.001 (2) | 0.4688 (17) | 0.6646 (18) | 0.050 (7) | 0.50 |
H35A | 1.0892 | 0.4471 | 0.7024 | 0.075* | 0.50 |
H35B | 0.9281 | 0.4141 | 0.6513 | 0.075* | 0.50 |
H35C | 0.9797 | 0.5291 | 0.7009 | 0.075* | 0.50 |
C36 | 1.176 (2) | 0.6359 (14) | 0.4564 (17) | 0.045 (6) | 0.50 |
H36A | 1.1989 | 0.7022 | 0.4977 | 0.068* | 0.50 |
H36B | 1.1246 | 0.6446 | 0.3902 | 0.068* | 0.50 |
H36C | 1.2614 | 0.6048 | 0.4583 | 0.068* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0207 (7) | 0.0265 (6) | 0.0476 (9) | 0.0048 (5) | 0.0215 (6) | 0.0015 (6) |
Cu2 | 0.0384 (11) | 0.0196 (8) | 0.0432 (11) | 0.0163 (7) | 0.0317 (9) | 0.0139 (8) |
Cu3 | 0.0362 (11) | 0.0190 (8) | 0.0408 (11) | −0.0105 (7) | 0.0282 (9) | −0.0028 (8) |
Cu4 | 0.0211 (7) | 0.0486 (8) | 0.0504 (9) | 0.0040 (6) | 0.0225 (7) | 0.0218 (7) |
Cu5 | 0.0204 (7) | 0.0464 (8) | 0.0469 (9) | 0.0048 (6) | 0.0164 (6) | 0.0136 (7) |
Cu6 | 0.0365 (9) | 0.0406 (8) | 0.1032 (13) | 0.0157 (6) | 0.0456 (9) | 0.0251 (8) |
S1 | 0.0234 (14) | 0.0329 (14) | 0.0460 (17) | 0.0093 (11) | 0.0206 (13) | 0.0066 (12) |
C61 | 0.018 (5) | 0.019 (5) | 0.032 (6) | 0.003 (4) | 0.007 (4) | 0.010 (4) |
N61 | 0.025 (5) | 0.042 (5) | 0.042 (6) | 0.006 (4) | 0.016 (4) | 0.016 (4) |
S2 | 0.0147 (12) | 0.0260 (12) | 0.0407 (16) | 0.0007 (9) | 0.0148 (12) | 0.0043 (11) |
C62 | 0.029 (6) | 0.015 (4) | 0.027 (6) | 0.004 (4) | 0.015 (5) | 0.002 (4) |
N62 | 0.018 (4) | 0.024 (4) | 0.038 (5) | 0.005 (3) | 0.018 (4) | 0.006 (4) |
S3 | 0.0150 (13) | 0.0178 (11) | 0.0421 (16) | 0.0033 (9) | 0.0126 (11) | 0.0043 (10) |
C63 | 0.015 (5) | 0.014 (4) | 0.027 (6) | 0.000 (3) | 0.012 (4) | 0.005 (4) |
N63 | 0.022 (5) | 0.022 (4) | 0.043 (5) | 0.004 (3) | 0.017 (4) | 0.013 (4) |
S4 | 0.0221 (14) | 0.0272 (12) | 0.0423 (16) | 0.0026 (10) | 0.0176 (12) | 0.0111 (11) |
C64 | 0.023 (6) | 0.020 (5) | 0.028 (6) | 0.001 (4) | 0.013 (5) | 0.009 (4) |
N64 | 0.035 (5) | 0.036 (5) | 0.037 (5) | 0.012 (4) | 0.022 (4) | 0.020 (4) |
N51 | 0.026 (5) | 0.026 (4) | 0.035 (5) | −0.003 (3) | 0.014 (4) | 0.008 (4) |
C51 | 0.026 (5) | 0.021 (5) | 0.027 (6) | 0.000 (4) | 0.011 (5) | 0.002 (4) |
N52 | 0.043 (5) | 0.020 (4) | 0.038 (5) | 0.011 (4) | 0.025 (5) | 0.013 (4) |
C52 | 0.034 (6) | 0.022 (5) | 0.029 (6) | 0.008 (4) | 0.013 (5) | 0.009 (4) |
N1 | 0.030 (5) | 0.036 (5) | 0.051 (6) | 0.009 (4) | 0.009 (5) | 0.010 (5) |
C1 | 0.036 (6) | 0.027 (5) | 0.040 (7) | 0.001 (5) | 0.022 (5) | 0.011 (5) |
C2 | 0.030 (6) | 0.024 (5) | 0.046 (7) | 0.000 (4) | 0.019 (5) | 0.010 (5) |
N2 | 0.020 (5) | 0.036 (5) | 0.057 (6) | 0.009 (4) | 0.020 (5) | 0.017 (4) |
C3 | 0.028 (6) | 0.023 (5) | 0.055 (8) | 0.007 (4) | 0.013 (6) | 0.001 (5) |
C4 | 0.035 (7) | 0.032 (6) | 0.047 (8) | 0.005 (5) | 0.008 (6) | 0.000 (5) |
C5 | 0.063 (8) | 0.029 (6) | 0.069 (9) | 0.019 (5) | 0.042 (7) | 0.007 (5) |
C6 | 0.047 (8) | 0.076 (9) | 0.057 (9) | 0.029 (7) | −0.007 (7) | −0.017 (7) |
N11 | 0.036 (5) | 0.025 (4) | 0.036 (6) | 0.007 (4) | 0.010 (4) | 0.006 (4) |
C11 | 0.037 (6) | 0.026 (5) | 0.040 (7) | 0.012 (4) | 0.020 (5) | 0.010 (5) |
C12 | 0.034 (6) | 0.025 (5) | 0.041 (7) | 0.004 (4) | 0.023 (5) | 0.010 (5) |
N12 | 0.030 (5) | 0.020 (4) | 0.036 (5) | −0.001 (3) | 0.022 (4) | 0.001 (3) |
C13 | 0.034 (6) | 0.018 (5) | 0.037 (6) | −0.001 (4) | 0.018 (5) | 0.005 (4) |
C14 | 0.036 (6) | 0.024 (5) | 0.037 (7) | 0.001 (4) | 0.004 (5) | 0.008 (5) |
C15 | 0.081 (10) | 0.037 (6) | 0.053 (8) | 0.018 (6) | 0.033 (7) | 0.009 (6) |
C16 | 0.102 (11) | 0.012 (5) | 0.043 (7) | −0.010 (6) | 0.009 (7) | 0.011 (5) |
N21 | 0.034 (5) | 0.024 (4) | 0.030 (5) | 0.008 (4) | 0.009 (4) | 0.010 (4) |
C21 | 0.024 (5) | 0.030 (5) | 0.026 (6) | 0.001 (4) | 0.011 (5) | 0.007 (4) |
C22 | 0.027 (6) | 0.017 (5) | 0.042 (6) | 0.006 (4) | 0.017 (5) | −0.001 (4) |
N22 | 0.029 (5) | 0.014 (4) | 0.042 (5) | 0.007 (3) | 0.020 (4) | 0.001 (3) |
C23 | 0.031 (6) | 0.024 (5) | 0.038 (6) | 0.004 (4) | 0.017 (5) | 0.008 (4) |
C24 | 0.037 (6) | 0.018 (5) | 0.026 (6) | 0.006 (4) | 0.012 (5) | 0.008 (4) |
C25 | 0.036 (6) | 0.034 (6) | 0.042 (7) | 0.006 (5) | 0.014 (5) | 0.014 (5) |
C26 | 0.074 (9) | 0.022 (5) | 0.058 (8) | 0.013 (5) | 0.012 (7) | 0.018 (5) |
N31 | 0.030 (6) | 0.044 (6) | 0.203 (16) | 0.006 (5) | 0.048 (9) | 0.048 (8) |
C31 | 0.042 (9) | 0.062 (9) | 0.147 (16) | 0.031 (7) | 0.059 (10) | 0.063 (10) |
C34 | 0.035 (9) | 0.046 (8) | 0.18 (2) | 0.007 (7) | 0.039 (11) | 0.045 (11) |
C35 | 0.029 (14) | 0.047 (14) | 0.065 (18) | −0.018 (11) | 0.017 (13) | −0.018 (13) |
C36 | 0.070 (17) | 0.030 (11) | 0.058 (16) | 0.014 (11) | 0.048 (14) | 0.011 (11) |
Geometric parameters (Å, º) top
Cu1—C52 | 1.881 (9) | C6—H6A | 0.9700 |
Cu1—N62i | 1.910 (7) | C6—H6B | 0.9700 |
Cu1—S4 | 2.542 (3) | C6—H6C | 0.9700 |
Cu1—S3 | 2.574 (2) | N11—C11 | 1.334 (11) |
Cu2—N52ii | 1.910 (8) | N11—C14 | 1.350 (12) |
Cu2—N52 | 1.910 (8) | C11—C12 | 1.390 (13) |
Cu2—N22ii | 2.047 (7) | C11—C15 | 1.480 (14) |
Cu2—N22 | 2.047 (7) | C12—N12 | 1.372 (12) |
Cu3—N51iii | 1.912 (7) | C12—H12 | 0.9400 |
Cu3—N51 | 1.912 (7) | N12—C13 | 1.346 (10) |
Cu3—N12iii | 2.023 (7) | C13—C14 | 1.384 (12) |
Cu3—N12 | 2.023 (7) | C13—H13 | 0.9400 |
Cu4—C51 | 1.875 (9) | C14—C16 | 1.496 (12) |
Cu4—N63 | 1.929 (8) | C15—H15A | 0.9700 |
Cu4—S1 | 2.517 (3) | C15—H15B | 0.9700 |
Cu4—S2 | 2.636 (3) | C15—H15C | 0.9700 |
Cu4—Cu5 | 2.9609 (18) | C16—H16A | 0.9700 |
Cu5—N64 | 1.927 (8) | C16—H16B | 0.9700 |
Cu5—N2 | 2.035 (8) | C16—H16C | 0.9700 |
Cu5—S2 | 2.372 (3) | N21—C24 | 1.337 (11) |
Cu5—S1 | 2.413 (3) | N21—C21 | 1.339 (11) |
Cu6—N61i | 1.945 (8) | C21—C22 | 1.375 (12) |
Cu6—N31 | 2.044 (14) | C21—C25 | 1.509 (13) |
Cu6—S4 | 2.383 (3) | C22—N22 | 1.344 (11) |
Cu6—S3 | 2.414 (3) | C22—H22 | 0.9400 |
S1—C61 | 1.659 (9) | N22—C23 | 1.350 (10) |
C61—N61 | 1.145 (11) | C23—C24 | 1.391 (12) |
N61—Cu6iv | 1.945 (8) | C23—H23 | 0.9400 |
S2—C62 | 1.684 (9) | C24—C26 | 1.493 (12) |
C62—N62 | 1.155 (10) | C25—H25A | 0.9700 |
N62—Cu1iv | 1.910 (7) | C25—H25B | 0.9700 |
S3—C63 | 1.644 (8) | C25—H25C | 0.9700 |
C63—N63 | 1.160 (10) | C26—H26A | 0.9700 |
S4—C64 | 1.651 (9) | C26—H26B | 0.9700 |
C64—N64 | 1.166 (11) | C26—H26C | 0.9700 |
N51—C51 | 1.171 (10) | N31—C31 | 1.329 (14) |
N52—C52 | 1.190 (11) | N31—C34 | 1.41 (2) |
N1—C1 | 1.342 (13) | C31—C35 | 1.15 (3) |
N1—C4 | 1.355 (12) | C31—C34v | 1.41 (2) |
C1—C2 | 1.380 (13) | C31—H31 | 0.9400 |
C1—C5 | 1.493 (13) | C34—C31v | 1.41 (2) |
C2—N2 | 1.356 (11) | C34—C36 | 1.45 (2) |
C2—H2 | 0.9400 | C34—H34 | 0.9400 |
N2—C3 | 1.344 (13) | C35—H35A | 0.9700 |
C3—C4 | 1.374 (14) | C35—H35B | 0.9700 |
C3—H3 | 0.9400 | C35—H35C | 0.9700 |
C4—C6 | 1.521 (15) | C36—H36A | 0.9700 |
C5—H5A | 0.9700 | C36—H36B | 0.9700 |
C5—H5B | 0.9700 | C36—H36C | 0.9700 |
C5—H5C | 0.9700 | | |
| | | |
C52—Cu1—N62i | 139.8 (4) | C1—C5—H5C | 109.5 |
C52—Cu1—S4 | 108.5 (3) | H5A—C5—H5C | 109.5 |
N62i—Cu1—S4 | 98.3 (2) | H5B—C5—H5C | 109.5 |
C52—Cu1—S3 | 105.0 (3) | C4—C6—H6A | 109.5 |
N62i—Cu1—S3 | 101.8 (2) | C4—C6—H6B | 109.5 |
S4—Cu1—S3 | 95.25 (9) | H6A—C6—H6B | 109.5 |
N52ii—Cu2—N52 | 180.0 (5) | C4—C6—H6C | 109.5 |
N52ii—Cu2—N22ii | 89.7 (3) | H6A—C6—H6C | 109.5 |
N52—Cu2—N22ii | 90.3 (3) | H6B—C6—H6C | 109.5 |
N52ii—Cu2—N22 | 90.3 (3) | C11—N11—C14 | 119.4 (8) |
N52—Cu2—N22 | 89.7 (3) | N11—C11—C12 | 119.4 (9) |
N22ii—Cu2—N22 | 180.000 (3) | N11—C11—C15 | 119.5 (9) |
N51iii—Cu3—N51 | 180.000 (2) | C12—C11—C15 | 121.1 (8) |
N51iii—Cu3—N12iii | 90.9 (3) | N12—C12—C11 | 122.7 (8) |
N51—Cu3—N12iii | 89.1 (3) | N12—C12—H12 | 118.7 |
N51iii—Cu3—N12 | 89.1 (3) | C11—C12—H12 | 118.7 |
N51—Cu3—N12 | 90.9 (3) | C13—N12—C12 | 115.7 (8) |
N12iii—Cu3—N12 | 180.000 (1) | C13—N12—Cu3 | 121.7 (7) |
C51—Cu4—N63 | 135.0 (4) | C12—N12—Cu3 | 122.5 (6) |
C51—Cu4—S1 | 104.7 (3) | N12—C13—C14 | 122.1 (9) |
N63—Cu4—S1 | 105.2 (2) | N12—C13—H13 | 118.9 |
C51—Cu4—S2 | 107.5 (3) | C14—C13—H13 | 118.9 |
N63—Cu4—S2 | 100.6 (2) | N11—C14—C13 | 120.5 (8) |
S1—Cu4—S2 | 98.06 (9) | N11—C14—C16 | 117.6 (9) |
C51—Cu4—Cu5 | 129.7 (3) | C13—C14—C16 | 121.9 (9) |
N63—Cu4—Cu5 | 95.3 (2) | C11—C15—H15A | 109.5 |
S1—Cu4—Cu5 | 51.49 (6) | C11—C15—H15B | 109.5 |
S2—Cu4—Cu5 | 49.74 (6) | H15A—C15—H15B | 109.5 |
N64—Cu5—N2 | 120.8 (3) | C11—C15—H15C | 109.5 |
N64—Cu5—S2 | 105.9 (3) | H15A—C15—H15C | 109.5 |
N2—Cu5—S2 | 110.3 (3) | H15B—C15—H15C | 109.5 |
N64—Cu5—S1 | 110.4 (2) | C14—C16—H16A | 109.5 |
N2—Cu5—S1 | 100.2 (2) | C14—C16—H16B | 109.5 |
S2—Cu5—S1 | 108.83 (10) | H16A—C16—H16B | 109.5 |
N64—Cu5—Cu4 | 104.7 (2) | C14—C16—H16C | 109.5 |
N2—Cu5—Cu4 | 134.1 (2) | H16A—C16—H16C | 109.5 |
S2—Cu5—Cu4 | 57.99 (7) | H16B—C16—H16C | 109.5 |
S1—Cu5—Cu4 | 54.71 (8) | C24—N21—C21 | 117.2 (7) |
N61i—Cu6—N31 | 106.2 (4) | N21—C21—C22 | 121.0 (8) |
N61i—Cu6—S4 | 116.2 (2) | N21—C21—C25 | 118.1 (8) |
N31—Cu6—S4 | 103.4 (3) | C22—C21—C25 | 120.9 (8) |
N61i—Cu6—S3 | 106.7 (3) | N22—C22—C21 | 123.1 (8) |
N31—Cu6—S3 | 121.0 (4) | N22—C22—H22 | 118.4 |
S4—Cu6—S3 | 103.97 (10) | C21—C22—H22 | 118.4 |
C61—S1—Cu5 | 94.9 (3) | C22—N22—C23 | 115.5 (8) |
C61—S1—Cu4 | 94.1 (3) | C22—N22—Cu2 | 123.5 (6) |
Cu5—S1—Cu4 | 73.79 (8) | C23—N22—Cu2 | 120.7 (6) |
N61—C61—S1 | 178.2 (9) | N22—C23—C24 | 121.7 (9) |
C61—N61—Cu6iv | 170.5 (8) | N22—C23—H23 | 119.2 |
C62—S2—Cu5 | 106.4 (3) | C24—C23—H23 | 119.2 |
C62—S2—Cu4 | 98.7 (3) | N21—C24—C23 | 121.5 (8) |
Cu5—S2—Cu4 | 72.28 (8) | N21—C24—C26 | 118.2 (8) |
N62—C62—S2 | 178.6 (9) | C23—C24—C26 | 120.3 (8) |
C62—N62—Cu1iv | 173.3 (8) | C21—C25—H25A | 109.5 |
C63—S3—Cu6 | 103.6 (3) | C21—C25—H25B | 109.5 |
C63—S3—Cu1 | 96.5 (3) | H25A—C25—H25B | 109.5 |
Cu6—S3—Cu1 | 75.99 (8) | C21—C25—H25C | 109.5 |
N63—C63—S3 | 177.3 (9) | H25A—C25—H25C | 109.5 |
C63—N63—Cu4 | 173.8 (8) | H25B—C25—H25C | 109.5 |
C64—S4—Cu6 | 96.3 (3) | C24—C26—H26A | 109.5 |
C64—S4—Cu1 | 100.3 (3) | C24—C26—H26B | 109.5 |
Cu6—S4—Cu1 | 77.18 (9) | H26A—C26—H26B | 109.5 |
N64—C64—S4 | 179.2 (9) | C24—C26—H26C | 109.5 |
C64—N64—Cu5 | 167.3 (8) | H26A—C26—H26C | 109.5 |
C51—N51—Cu3 | 175.6 (8) | H26B—C26—H26C | 109.5 |
N51—C51—Cu4 | 177.0 (8) | C31—N31—C34 | 116.9 (14) |
C52—N52—Cu2 | 171.6 (8) | C31—N31—Cu6 | 126.6 (15) |
N52—C52—Cu1 | 175.4 (9) | C34—N31—Cu6 | 116.2 (9) |
C1—N1—C4 | 117.1 (9) | C35—C31—N31 | 125 (2) |
N1—C1—C2 | 120.7 (9) | C35—C31—C34v | 113.8 (17) |
N1—C1—C5 | 118.0 (10) | N31—C31—C34v | 121.6 (16) |
C2—C1—C5 | 121.3 (10) | C35—C31—H31 | 5.4 |
N2—C2—C1 | 122.6 (10) | N31—C31—H31 | 119.2 |
N2—C2—H2 | 118.7 | C34v—C31—H31 | 119.2 |
C1—C2—H2 | 118.7 | N31—C34—C31v | 121.5 (12) |
C3—N2—C2 | 115.8 (9) | N31—C34—C36 | 131.7 (18) |
C3—N2—Cu5 | 119.3 (6) | C31v—C34—C36 | 106.8 (19) |
C2—N2—Cu5 | 124.3 (7) | N31—C34—H34 | 119.3 |
N2—C3—C4 | 122.1 (9) | C31v—C34—H34 | 119.3 |
N2—C3—H3 | 118.9 | C36—C34—H34 | 12.4 |
C4—C3—H3 | 118.9 | C31—C35—H35A | 109.5 |
N1—C4—C3 | 121.5 (10) | C31—C35—H35B | 109.5 |
N1—C4—C6 | 116.8 (10) | C31—C35—H35C | 109.5 |
C3—C4—C6 | 121.4 (9) | C34—C36—H36A | 109.5 |
C1—C5—H5A | 109.5 | C34—C36—H36B | 109.5 |
C1—C5—H5B | 109.5 | C34—C36—H36C | 109.5 |
H5A—C5—H5B | 109.5 | | |
Symmetry codes: (i) x+1, y, z; (ii) −x+2, −y+2, −z+2; (iii) −x+1, −y+1, −z+2; (iv) x−1, y, z; (v) −x+2, −y+1, −z+1. |