#------------------------------------------------------------------------------
#$Date: 2019-11-02 06:03:31 +0200 (Sat, 02 Nov 2019) $
#$Revision: 220770 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/75/4127527.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4127527
loop_
_publ_author_name
'Song, Fangyuan'
'Al-Ameed, Karrar'
'Schilling, Mauro'
'Fox, Thomas'
'Luber, Sandra'
'Patzke, Greta R.'
_publ_section_title
;
 Mechanistically Driven Control over Cubane Oxo Cluster Catalysts.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8846
_journal_page_last               8857
_journal_paper_doi               10.1021/jacs.9b01356
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C48 H46 Co1.92 N8 Ni2.08 O14, 2(Cl O4)'
_chemical_formula_sum            'C48 H46 Cl2 Co1.94 N8 Ni2.06 O22'
_chemical_formula_weight         1393.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.903(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7499(14)
_cell_length_b                   12.1315(6)
_cell_length_c                   21.1640(12)
_cell_measurement_reflns_used    4646
_cell_measurement_temperature    183.05(10)
_cell_measurement_theta_max      28.2620
_cell_measurement_theta_min      3.1550
_cell_volume                     5254.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -90.00   5.00   0.50   50.00    --  -19.81 -57.00 150.00  190
  2  ω    -40.00  49.00   0.50   50.00    --  -19.81  57.00 -60.00  178
  3  ω     12.00  45.00   0.50   50.00    --   20.59 -38.00 -60.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0127327000
_diffrn_orient_matrix_UB_12      -0.0521762000
_diffrn_orient_matrix_UB_13      0.0148071000
_diffrn_orient_matrix_UB_21      -0.0311446000
_diffrn_orient_matrix_UB_22      -0.0156517000
_diffrn_orient_matrix_UB_23      -0.0029670000
_diffrn_orient_matrix_UB_31      -0.0082847000
_diffrn_orient_matrix_UB_32      -0.0212910000
_diffrn_orient_matrix_UB_33      -0.0340442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.523
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark purple'
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       prism
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.167
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6520
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0650P)²+18.9902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5013
_reflns_number_total             6520
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891349(2-coxni4-x-clo4final)
_cod_database_code               4127527
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H46 Cl2 Co4 N8 O22'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.533
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Co2, Ni2}
{Co1, Ni1}
3. Restrained distances
 O7-H7A
 0.86 with sigma of 0.02
 O7-H7B
 0.84 with sigma of 0.02
 O5-C23B \\sim O5-C23A
 with sigma of 0.002
 O6A-C23A \\sim O6B-C23B
 with sigma of 0.002
 C24B-C23B \\sim C24A-C23A
 with sigma of 0.002
 Cl1B-O8B \\sim Cl1B-O9B \\sim Cl1A-O11A \\sim Cl1B-O10B \\sim Cl1A-O10A \\sim
Cl1A-O8A \\sim Cl1A-O9A
 \\sim Cl1B-O11B
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
O8A \\sim O8B \\sim O9A \\sim O9B \\sim O10A \\sim O10B \\sim O11A \\sim O11B:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(Co2) = Uanis(Ni2)
Uanis(Co1) = Uanis(Ni1)
5. Rigid body (RIGU) restrains
 O5, O6A, O6B, C23A, C23B, C24A, C24B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 Cl1A, Cl1B, O8A, O8B, O9A, O9B, O10A, O10B, O11A, O11B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl1B)=Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(O11B)=1-FVAR(1)
 Sof(Cl1A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=FVAR(1)
 Sof(O6A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(2)
 Sof(O6B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=FVAR(2)
 Fixed Sof: Co1(0.49) Co2(0.47) Ni1(0.51) Ni2(0.53)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22)
7.b Idealised Me refined as rotating group:
 C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F)
7.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.759
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.55748(2) 0.31165(4) 0.32627(2) 0.03946(15) Uani 0.49 1 d . . P A 1
Co2 Co 0.55343(2) 0.11539(4) 0.22498(2) 0.03631(14) Uani 0.47 1 d . . P A 1
Ni1 Ni 0.55748(2) 0.31165(4) 0.32627(2) 0.03946(15) Uani 0.51 1 d . . P A 2
Ni2 Ni 0.55343(2) 0.11539(4) 0.22498(2) 0.03631(14) Uani 0.53 1 d . . P A 2
Cl1A Cl 0.70426(13) 0.66150(15) 0.34632(12) 0.0801(7) Uani 0.735(4) 1 d D U P B
1
Cl1B Cl 0.6956(2) 0.6594(3) 0.2971(3) 0.0533(15) Uani 0.265(4) 1 d D U P B 2
O1 O 0.54597(11) 0.2907(2) 0.22543(11) 0.0379(5) Uani 1 1 d . . . . .
O2 O 0.45452(12) 0.1360(2) 0.18046(11) 0.0361(5) Uani 1 1 d . . . . .
O3 O 0.58278(14) 0.4451(2) 0.18717(14) 0.0484(6) Uani 1 1 d . . . . .
H3 H 0.589487 0.486130 0.221621 0.20(4) Uiso 1 1 calc GR . . . .
O4 O 0.40828(15) 0.0840(3) 0.06295(12) 0.0527(8) Uani 1 1 d . . . . .
H4 H 0.416650 0.151125 0.061278 0.048(12) Uiso 1 1 calc GR . . . .
O5 O 0.57199(14) 0.3034(2) 0.42745(13) 0.0485(7) Uani 1 1 d D U . . .
O6A O 0.5224(10) 0.4506(13) 0.4381(7) 0.050(6) Uani 0.186(11) 1 d D U P A 1
O6B O 0.5739(3) 0.4817(4) 0.4568(3) 0.0817(19) Uani 0.814(11) 1 d D U P A 2
O7 O 0.54976(17) 0.4831(3) 0.3227(2) 0.0644(9) Uani 1 1 d D . . . .
H7A H 0.554(2) 0.495(3) 0.3629(13) 0.036(12) Uiso 1 1 d D . . . .
H7B H 0.580(3) 0.518(6) 0.319(4) 0.15(3) Uiso 1 1 d D . . . .
O8A O 0.7113(6) 0.6410(8) 0.4143(4) 0.182(4) Uani 0.735(4) 1 d D U P B 1
O8B O 0.6715(8) 0.6653(17) 0.2241(4) 0.106(5) Uani 0.265(4) 1 d D U P B 2
O9A O 0.6440(7) 0.611(2) 0.3074(8) 0.131(3) Uani 0.735(4) 1 d D U P B 1
O9B O 0.6386(19) 0.617(7) 0.297(3) 0.132(4) Uani 0.265(4) 1 d D U P B 2
O10A O 0.7013(11) 0.7754(4) 0.3356(8) 0.083(2) Uani 0.735(4) 1 d D U P B 1
O10B O 0.706(3) 0.7657(11) 0.325(2) 0.082(4) Uani 0.265(4) 1 d D U P B 2
O11A O 0.7536(7) 0.613(2) 0.3335(9) 0.122(3) Uani 0.735(4) 1 d D U P B 1
O11B O 0.7561(18) 0.606(6) 0.324(3) 0.119(4) Uani 0.265(4) 1 d D U P B 2
N1 N 0.65410(15) 0.3251(3) 0.33746(16) 0.0448(8) Uani 1 1 d . . . . .
N2 N 0.58192(16) 0.1602(3) 0.14944(15) 0.0441(7) Uani 1 1 d . . . . .
N3 N 0.52032(18) -0.0447(3) 0.18880(15) 0.0448(8) Uani 1 1 d . . . . .
N4 N 0.35428(16) 0.0668(3) 0.19838(15) 0.0448(7) Uani 1 1 d . . . . .
C1 C 0.7087(2) 0.3296(4) 0.3983(2) 0.0542(11) Uani 1 1 d . . . . .
H1 H 0.704674 0.326722 0.441114 0.065 Uiso 1 1 calc R . . . .
C2 C 0.7698(2) 0.3381(4) 0.4011(2) 0.0589(12) Uani 1 1 d . . . . .
H2 H 0.807432 0.340950 0.445035 0.071 Uiso 1 1 calc R . . . .
C3 C 0.7759(2) 0.3425(4) 0.3393(2) 0.0550(11) Uani 1 1 d . . . . .
H3A H 0.817815 0.347970 0.339965 0.066 Uiso 1 1 calc R . . . .
C4 C 0.71997(19) 0.3390(3) 0.2757(2) 0.0469(9) Uani 1 1 d . . . . .
H4A H 0.722923 0.341670 0.232302 0.056 Uiso 1 1 calc R . . . .
C5 C 0.65999(18) 0.3314(3) 0.27727(18) 0.0402(8) Uani 1 1 d . . . . .
C6 C 0.59461(18) 0.3350(3) 0.20972(18) 0.0407(8) Uani 1 1 d . . . . .
C7 C 0.59692(18) 0.2672(4) 0.14997(18) 0.0449(9) Uani 1 1 d . . . . .
C8 C 0.6120(2) 0.3128(4) 0.0993(2) 0.0613(13) Uani 1 1 d . . . . .
H8 H 0.621481 0.389229 0.100011 0.074 Uiso 1 1 calc R . . . .
C9 C 0.6132(3) 0.2448(5) 0.0473(2) 0.0762(17) Uani 1 1 d . . . . .
H9 H 0.624558 0.273857 0.012379 0.091 Uiso 1 1 calc R . . . .
C10 C 0.5977(3) 0.1344(5) 0.0463(2) 0.0713(15) Uani 1 1 d . . . . .
H10 H 0.597611 0.086675 0.010713 0.086 Uiso 1 1 calc R . . . .
C11 C 0.5825(2) 0.0956(4) 0.0981(2) 0.0551(11) Uani 1 1 d . . . . .
H11 H 0.571797 0.019838 0.097732 0.066 Uiso 1 1 calc R . . . .
C12 C 0.5562(3) -0.1371(4) 0.2032(2) 0.0579(12) Uani 1 1 d . . . . .
H12 H 0.601971 -0.132171 0.231595 0.069 Uiso 1 1 calc R . . . .
C13 C 0.5291(4) -0.2390(4) 0.1781(3) 0.0728(16) Uani 1 1 d . . . . .
H13 H 0.555844 -0.302900 0.188624 0.087 Uiso 1 1 calc R . . . .
C14 C 0.4626(4) -0.2469(4) 0.1377(3) 0.0770(17) Uani 1 1 d . . . . .
H14 H 0.442971 -0.316181 0.119762 0.092 Uiso 1 1 calc R . . . .
C15 C 0.4248(3) -0.1523(4) 0.1235(2) 0.0603(13) Uani 1 1 d . . . . .
H15 H 0.378722 -0.156042 0.096724 0.072 Uiso 1 1 calc R . . . .
C16 C 0.4551(2) -0.0525(3) 0.14897(17) 0.0459(9) Uani 1 1 d . . . . .
C17 C 0.41785(19) 0.0568(3) 0.13194(16) 0.0431(9) Uani 1 1 d . . . . .
C18 C 0.3521(2) 0.0463(3) 0.13491(18) 0.0466(9) Uani 1 1 d . . . . .
C19 C 0.2940(2) 0.0190(4) 0.0776(2) 0.0581(12) Uani 1 1 d . . . . .
H19 H 0.293340 0.004468 0.033177 0.070 Uiso 1 1 calc R . . . .
C20 C 0.2373(2) 0.0132(4) 0.0859(2) 0.0655(14) Uani 1 1 d . . . . .
H20 H 0.197195 -0.005787 0.047283 0.079 Uiso 1 1 calc R . . . .
C21 C 0.2392(2) 0.0351(4) 0.1501(3) 0.0618(12) Uani 1 1 d . . . . .
H21 H 0.200434 0.032643 0.156588 0.074 Uiso 1 1 calc R . . . .
C22 C 0.2988(2) 0.0609(4) 0.2058(2) 0.0518(10) Uani 1 1 d . . . . .
H22 H 0.300323 0.074938 0.250627 0.062 Uiso 1 1 calc R . . . .
C23A C 0.5503(11) 0.3633(14) 0.4636(8) 0.037(5) Uani 0.186(11) 1 d D U P A 1
C23B C 0.5713(3) 0.3828(5) 0.4683(3) 0.0531(17) Uani 0.814(11) 1 d D U P A 2
C24A C 0.556(3) 0.351(6) 0.5370(15) 0.059(11) Uani 0.186(11) 1 d D U P A 1
H24A H 0.574131 0.418666 0.563555 0.089 Uiso 0.186(11) 1 calc GR . P A 1
H24B H 0.585309 0.288940 0.560353 0.089 Uiso 0.186(11) 1 calc GR . P A 1
H24C H 0.512911 0.336588 0.534789 0.089 Uiso 0.186(11) 1 calc GR . P A 1
C24B C 0.5685(8) 0.3411(13) 0.5340(5) 0.068(3) Uani 0.814(11) 1 d D U P A 2
H24D H 0.549815 0.266768 0.525690 0.101 Uiso 0.814(11) 1 calc GR . P A 2
H24E H 0.541160 0.390435 0.546580 0.101 Uiso 0.814(11) 1 calc GR . P A 2
H24F H 0.612746 0.339067 0.572487 0.101 Uiso 0.814(11) 1 calc GR . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 -15 0 0.0852
30 -4 -20 0.1830
-16 -14 1 0.0661
16 12 -20 0.1270
0 1 27 0.2189
-26 5 24 0.2040
-26 0 27 0.2133
3 -3 -28 0.2219
-15 15 1 0.0958
29 0 0 0.1594
0 -17 0 0.0767
-6 0 29 0.2250
8 14 -16 0.1248
-28 5 1 0.1333
13 15 1 0.0836
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Co1 O1 80.83(11) . 2_655
O1 Co1 O2 76.58(10) 2_655 2_655
O1 Co1 O2 81.55(9) . 2_655
O1 Co1 O7 96.63(15) . .
O1 Co1 N1 77.26(11) . .
O5 Co1 O1 99.82(11) . 2_655
O5 Co1 O1 169.87(11) . .
O5 Co1 O2 88.74(10) . 2_655
O5 Co1 O7 93.45(15) . .
O5 Co1 N1 101.81(12) . .
O7 Co1 O1 92.50(12) . 2_655
O7 Co1 O2 169.07(11) . 2_655
O7 Co1 N1 89.68(14) . .
N1 Co1 O1 158.08(11) . 2_655
N1 Co1 O2 100.37(11) . 2_655
O2 Co2 O1 78.82(9) . .
O2 Co2 O1 80.62(9) 2_655 .
O2 Co2 O2 83.61(9) . 2_655
O2 Co2 N2 105.60(11) . .
O2 Co2 N3 78.33(12) . .
O2 Co2 N3 106.89(10) 2_655 .
O2 Co2 N4 156.91(12) . 2_655
N2 Co2 O1 77.96(12) . .
N2 Co2 O2 154.41(12) . 2_655
N2 Co2 N3 98.42(12) . .
N2 Co2 N4 97.31(13) . 2_655
N3 Co2 O1 154.91(11) . .
N4 Co2 O1 109.34(11) 2_655 .
N4 Co2 O2 76.76(11) 2_655 2_655
N4 Co2 N3 95.73(13) 2_655 .
O1 Ni1 O1 80.83(11) . 2_655
O1 Ni1 O2 76.58(10) 2_655 2_655
O1 Ni1 O2 81.55(9) . 2_655
O1 Ni1 O7 96.63(15) . .
O1 Ni1 N1 77.26(11) . .
O5 Ni1 O1 169.87(11) . .
O5 Ni1 O1 99.82(11) . 2_655
O5 Ni1 O2 88.74(10) . 2_655
O5 Ni1 O7 93.45(15) . .
O5 Ni1 N1 101.81(12) . .
O7 Ni1 O1 92.50(12) . 2_655
O7 Ni1 O2 169.07(11) . 2_655
O7 Ni1 N1 89.68(14) . .
N1 Ni1 O1 158.08(11) . 2_655
N1 Ni1 O2 100.37(11) . 2_655
O2 Ni2 O1 78.82(9) . .
O2 Ni2 O1 80.62(9) 2_655 .
O2 Ni2 O2 83.61(9) . 2_655
O2 Ni2 N2 105.60(11) . .
O2 Ni2 N3 106.89(10) 2_655 .
O2 Ni2 N3 78.33(12) . .
O2 Ni2 N4 156.91(12) . 2_655
N2 Ni2 O1 77.96(12) . .
N2 Ni2 O2 154.41(12) . 2_655
N2 Ni2 N3 98.42(12) . .
N2 Ni2 N4 97.31(13) . 2_655
N3 Ni2 O1 154.91(11) . .
N4 Ni2 O1 109.34(11) 2_655 .
N4 Ni2 O2 76.76(11) 2_655 2_655
N4 Ni2 N3 95.73(13) 2_655 .
O8A Cl1A O11A 112.6(9) . .
O9A Cl1A O8A 99.7(8) . .
O9A Cl1A O10A 112.2(15) . .
O9A Cl1A O11A 111.2(16) . .
O10A Cl1A O8A 108.6(6) . .
O10A Cl1A O11A 112.0(13) . .
O8B Cl1B O9B 96(2) . .
O10B Cl1B O8B 109.7(18) . .
O10B Cl1B O9B 109(4) . .
O10B Cl1B O11B 108(4) . .
O11B Cl1B O8B 108(2) . .
O11B Cl1B O9B 125(5) . .
Co1 O1 Co1 97.46(11) . 2_655
Co1 O1 Co2 98.86(10) . .
Co1 O1 Co2 100.86(10) 2_655 .
Ni1 O1 Ni2 98.86(10) . .
C6 O1 Co1 130.1(2) . 2_655
C6 O1 Co1 116.55(19) . .
C6 O1 Co2 108.1(2) . .
C6 O1 Ni1 116.55(19) . .
C6 O1 Ni2 108.1(2) . .
Co2 O2 Co1 96.90(10) 2_655 2_655
Co2 O2 Co1 103.60(10) . 2_655
Co2 O2 Co2 94.71(9) . 2_655
C17 O2 Co1 128.4(2) . 2_655
C17 O2 Co2 110.38(19) . 2_655
C17 O2 Co2 116.3(2) . .
C17 O2 Ni2 116.3(2) . .
C6 O3 H3 109.5 . .
C17 O4 H4 109.5 . .
C23A O5 Co1 131.9(7) . .
C23B O5 Ni1 128.6(4) . .
Co1 O7 H7A 99(3) . .
Co1 O7 H7B 117(6) . .
Ni1 O7 H7A 99(3) . .
Ni1 O7 H7B 117(6) . .
H7A O7 H7B 106(6) . .
C1 N1 Co1 126.2(3) . .
C1 N1 Ni1 126.2(3) . .
C5 N1 Co1 115.4(2) . .
C5 N1 Ni1 115.4(2) . .
C5 N1 C1 118.3(4) . .
C7 N2 Co2 114.7(2) . .
C7 N2 Ni2 114.7(2) . .
C7 N2 C11 118.6(3) . .
C11 N2 Co2 126.5(3) . .
C11 N2 Ni2 126.5(3) . .
C12 N3 Co2 127.1(3) . .
C12 N3 Ni2 127.1(3) . .
C12 N3 C16 118.4(4) . .
C16 N3 Co2 114.4(3) . .
C16 N3 Ni2 114.4(3) . .
C18 N4 Co2 114.3(3) . 2_655
C22 N4 Co2 126.8(3) . 2_655
C22 N4 C18 118.8(3) . .
N1 C1 H1 118.7 . .
N1 C1 C2 122.7(4) . .
C2 C1 H1 118.7 . .
C1 C2 H2 120.5 . .
C1 C2 C3 118.9(4) . .
C3 C2 H2 120.5 . .
C2 C3 H3A 120.3 . .
C2 C3 C4 119.3(4) . .
C4 C3 H3A 120.3 . .
C3 C4 H4A 120.9 . .
C5 C4 C3 118.3(4) . .
C5 C4 H4A 120.9 . .
N1 C5 C4 122.4(3) . .
N1 C5 C6 115.1(3) . .
C4 C5 C6 122.4(3) . .
O1 C6 O3 113.2(3) . .
O1 C6 C5 108.1(3) . .
O1 C6 C7 107.9(3) . .
O3 C6 C5 107.7(3) . .
O3 C6 C7 107.6(3) . .
C7 C6 C5 112.5(3) . .
N2 C7 C6 115.3(3) . .
N2 C7 C8 122.1(4) . .
C8 C7 C6 122.5(4) . .
C7 C8 H8 120.7 . .
C7 C8 C9 118.5(4) . .
C9 C8 H8 120.7 . .
C8 C9 H9 120.2 . .
C10 C9 C8 119.6(4) . .
C10 C9 H9 120.2 . .
C9 C10 H10 120.9 . .
C11 C10 C9 118.3(4) . .
C11 C10 H10 120.9 . .
N2 C11 C10 122.8(4) . .
N2 C11 H11 118.6 . .
C10 C11 H11 118.6 . .
N3 C12 H12 118.8 . .
N3 C12 C13 122.4(5) . .
C13 C12 H12 118.8 . .
C12 C13 H13 120.5 . .
C14 C13 C12 119.1(5) . .
C14 C13 H13 120.5 . .
C13 C14 H14 120.4 . .
C13 C14 C15 119.1(5) . .
C15 C14 H14 120.4 . .
C14 C15 H15 120.5 . .
C16 C15 C14 119.0(5) . .
C16 C15 H15 120.5 . .
N3 C16 C15 122.0(4) . .
N3 C16 C17 115.4(3) . .
C15 C16 C17 122.5(4) . .
O2 C17 O4 111.9(3) . .
O2 C17 C16 109.5(3) . .
O2 C17 C18 108.1(3) . .
O4 C17 C16 105.4(3) . .
O4 C17 C18 110.4(3) . .
C18 C17 C16 111.6(3) . .
N4 C18 C17 114.6(3) . .
N4 C18 C19 121.4(4) . .
C19 C18 C17 124.0(4) . .
C18 C19 H19 120.4 . .
C20 C19 C18 119.2(4) . .
C20 C19 H19 120.4 . .
C19 C20 H20 120.2 . .
C21 C20 C19 119.5(4) . .
C21 C20 H20 120.2 . .
C20 C21 H21 120.6 . .
C20 C21 C22 118.8(5) . .
C22 C21 H21 120.6 . .
N4 C22 C21 122.2(4) . .
N4 C22 H22 118.9 . .
C21 C22 H22 118.9 . .
O5 C23A C24A 132(2) . .
O6A C23A O5 118.6(11) . .
O6A C23A C24A 110(2) . .
O5 C23B C24B 112.5(7) . .
O6B C23B O5 125.2(6) . .
O6B C23B C24B 122.4(7) . .
C23A C24A H24A 109.5 . .
C23A C24A H24B 109.5 . .
C23A C24A H24C 109.5 . .
H24A C24A H24B 109.5 . .
H24A C24A H24C 109.5 . .
H24B C24A H24C 109.5 . .
C23B C24B H24D 109.5 . .
C23B C24B H24E 109.5 . .
C23B C24B H24F 109.5 . .
H24D C24B H24E 109.5 . .
H24D C24B H24F 109.5 . .
H24E C24B H24F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.049(2) .
Co1 O1 2.133(2) 2_655
Co1 O2 2.145(2) 2_655
Co1 O5 2.021(3) .
Co1 O7 2.086(4) .
Co1 N1 2.112(3) .
Co2 O1 2.134(3) .
Co2 O2 2.102(2) 2_655
Co2 O2 2.040(2) .
Co2 N2 2.044(3) .
Co2 N3 2.103(3) .
Co2 N4 2.100(3) 2_655
Ni1 O1 2.133(2) 2_655
Ni1 O1 2.049(2) .
Ni1 O2 2.145(2) 2_655
Ni1 O5 2.021(3) .
Ni1 O7 2.086(4) .
Ni1 N1 2.112(3) .
Ni2 O1 2.134(3) .
Ni2 O2 2.040(2) .
Ni2 O2 2.102(2) 2_655
Ni2 N2 2.044(3) .
Ni2 N3 2.103(3) .
Ni2 N4 2.100(3) 2_655
Cl1A O8A 1.398(5) .
Cl1A O9A 1.398(5) .
Cl1A O10A 1.398(5) .
Cl1A O11A 1.398(5) .
Cl1B O8B 1.398(5) .
Cl1B O9B 1.398(5) .
Cl1B O10B 1.398(5) .
Cl1B O11B 1.398(5) .
O1 C6 1.395(4) .
O2 C17 1.387(4) .
O3 H3 0.8400 .
O3 C6 1.404(5) .
O4 H4 0.8400 .
O4 C17 1.418(4) .
O5 C23A 1.300(5) .
O5 C23B 1.300(5) .
O6A C23A 1.231(7) .
O6B C23B 1.231(7) .
O7 H7A 0.826(19) .
O7 H7B 0.84(2) .
N1 C1 1.343(4) .
N1 C5 1.340(5) .
N2 C7 1.340(5) .
N2 C11 1.344(5) .
N3 C12 1.341(6) .
N3 C16 1.353(5) .
N4 C18 1.346(5) .
N4 C22 1.339(5) .
C1 H1 0.9500 .
C1 C2 1.371(6) .
C2 H2 0.9500 .
C2 C3 1.376(7) .
C3 H3A 0.9500 .
C3 C4 1.391(5) .
C4 H4A 0.9500 .
C4 C5 1.383(6) .
C5 C6 1.549(5) .
C6 C7 1.529(5) .
C7 C8 1.378(6) .
C8 H8 0.9500 .
C8 C9 1.385(7) .
C9 H9 0.9500 .
C9 C10 1.383(7) .
C10 H10 0.9500 .
C10 C11 1.369(6) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C12 C13 1.381(7) .
C13 H13 0.9500 .
C13 C14 1.377(9) .
C14 H14 0.9500 .
C14 C15 1.387(8) .
C15 H15 0.9500 .
C15 C16 1.380(6) .
C16 C17 1.530(6) .
C17 C18 1.529(6) .
C18 C19 1.389(5) .
C19 H19 0.9500 .
C19 C20 1.377(7) .
C20 H20 0.9500 .
C20 C21 1.367(7) .
C21 H21 0.9500 .
C21 C22 1.389(6) .
C22 H22 0.9500 .
C23A C24A 1.507(9) .
C23B C24B 1.507(9) .
C24A H24A 0.9800 .
C24A H24B 0.9800 .
C24A H24C 0.9800 .
C24B H24D 0.9800 .
C24B H24E 0.9800 .
C24B H24F 0.9800 .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
15.0004 -14.9904 0.0041 0.9732 -0.2326 0.1947
30.0068 -3.9995 -19.9843 0.2948 -0.8127 0.5169
-16.0002 -13.9932 0.9912 0.5411 0.7144 0.3967
16.0064 11.9904 -19.9879 -0.7178 -0.6269 0.2926
-0.0088 1.0051 26.9950 0.3472 -0.0956 -0.9404
-26.0081 5.0001 23.9854 -0.2369 0.6606 -0.7076
-26.0089 0.0035 26.9841 0.0682 0.7299 -0.7033
3.0091 -3.0040 -27.9938 -0.2195 0.0364 0.9921
-15.0007 14.9906 0.9957 -0.9584 0.2296 -0.2288
29.0002 0.0024 0.0120 0.3693 -0.9033 -0.2407
0.0003 -16.9905 -0.0024 0.8865 0.2659 0.3618
-6.0094 0.0056 28.9920 0.3525 0.1011 -0.9373
8.0050 13.9894 -15.9917 -0.8648 -0.4208 0.1803
-28.0006 4.9951 0.9889 -0.6025 0.7910 0.0920
12.9995 14.9928 1.0073 -0.6018 -0.6425 -0.4612
