#------------------------------------------------------------------------------
#$Date: 2020-05-05 15:46:01 +0300 (Tue, 05 May 2020) $
#$Revision: 251569 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/60/7126094.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_7126094
loop_
_publ_author_name
'Yu, You-Zhu'
'Guo, Yu-Hua'
'Zhang, Yan-Ru'
'Tian, Xiu-Juan'
'Zhang, Xian-Ming'
_publ_section_title
;
 Tetrahedral μ₄-chloride and in situ generated octahedral
 μ₆-sulfide templating Co₈ complexes with different
 distortions of the cube.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4236
_journal_page_last               4239
_journal_paper_doi               10.1039/d0cc01320j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C26 H54 Co8 N8 O12 S3'
_chemical_formula_sum            'C26 H48 Co8 K N8 O12 S2'
_chemical_formula_weight         1239.38
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-10
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2019-12-24 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.4577(3)
_cell_length_b                   13.4577(3)
_cell_length_c                   20.3224(4)
_cell_measurement_reflns_used    8110
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.66
_cell_volume                     3187.48(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13093
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.273
_diffrn_reflns_theta_min         2.014
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.301
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_description       block
_exptl_crystal_F_000             1869
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0371
_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)+(0.0909P)²+6.4853P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1628
_reflns_number_total             1766
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc01320j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7126094--7126095.cif.'
_cod_original_cell_volume        3187.48(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7126094
_shelx_shelxl_version_number     2014/7
_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   0.620
_shelx_estimated_absorpt_t_min   0.558
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H,H) groups, All N(H) groups 
2.a Ternary CH refined with riding coordinates: 
 N2(H2) 
2.b Secondary CH2 refined with riding coordinates: 
 C4(H4A,H4B), C2(H2A,H2B), C1(H1A,H1B), C3(H3A,H3B) 
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.86654(4) 0.47168(4) 0.28413(2) 0.0317(2) Uani 1 1 d . . . . .
Co2 Co 0.6667 0.3333 0.16986(4) 0.0348(2) Uani 1 3 d S T P . .
S1 S 0.6667 0.3333 -0.06788(9) 0.0686(6) Uani 1 3 d S T P . .
O2 O 0.8101(2) 0.4667(2) 0.19475(11) 0.0423(6) Uani 1 1 d . . . . .
O1 O 0.88107(19) 0.58656(19) 0.34849(11) 0.0373(5) Uani 1 1 d . . . . .
N1 N 0.6667 0.3333 0.0679(3) 0.0462(12) Uani 1 3 d S T P . .
N2 N 1.0225(3) 0.6164(3) 0.24474(14) 0.0436(7) Uani 1 1 d . . . . .
H2 H 1.0793 0.5939 0.2333 0.052 Uiso 1 1 calc R . . . .
C4 C 0.8922(3) 0.5445(3) 0.15116(18) 0.0462(8) Uani 1 1 d . . . . .
H4A H 0.8549 0.5671 0.1184 0.055 Uiso 1 1 calc R . . . .
H4B H 0.9286 0.5075 0.1285 0.055 Uiso 1 1 calc R . . . .
C5 C 0.6667 0.3333 0.0127(3) 0.0462(13) Uani 1 3 d S T P . .
C2 C 1.0642(3) 0.7014(4) 0.2975(2) 0.0552(10) Uani 1 1 d . . . . .
H2A H 1.1135 0.7770 0.2791 0.066 Uiso 1 1 calc R . . . .
H2B H 1.1094 0.6850 0.3281 0.066 Uiso 1 1 calc R . . . .
C1 C 0.9658(3) 0.7004(3) 0.33360(18) 0.0456(8) Uani 1 1 d . . . . .
H1A H 0.9937 0.7443 0.3740 0.055 Uiso 1 1 calc R . . . .
H1B H 0.9329 0.7359 0.3065 0.055 Uiso 1 1 calc R . . . .
C3 C 0.9812(5) 0.6481(4) 0.1858(2) 0.0650(13) Uani 1 1 d . . . . .
H3A H 1.0451 0.6922 0.1562 0.078 Uiso 1 1 calc R . . . .
H3B H 0.9493 0.6960 0.1984 0.078 Uiso 1 1 calc R . . . .
S2 S 0.6667 0.3333 0.3333 0.0272(3) Uani 1 6 d S T P . .
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
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
_geom_angle_publ_flag
O2 Co1 O1 122.06(11) . . ?
O2 Co1 N2 82.75(10) . . ?
O2 Co1 S2 95.04(7) . . ?
O1 Co1 O2 125.42(11) 17 . ?
O1 Co1 O1 112.47(3) 17 . ?
O1 Co1 N2 102.99(11) 17 . ?
O1 Co1 N2 82.44(10) . . ?
O1 Co1 S2 88.13(7) . . ?
O1 Co1 S2 88.62(7) 17 . ?
N2 Co1 S2 167.18(9) . . ?
O2 Co2 O2 113.41(6) . 2_655 ?
O2 Co2 O2 113.41(6) 3_665 2_655 ?
O2 Co2 O2 113.41(6) . 3_665 ?
O2 Co2 N1 105.17(7) . . ?
O2 Co2 N1 105.17(7) 2_655 . ?
O2 Co2 N1 105.17(7) 3_665 . ?
Co2 O2 Co1 117.72(12) . . ?
C4 O2 Co1 114.5(2) . . ?
C4 O2 Co2 125.4(2) . . ?
Co1 O1 Co1 106.12(11) 18_545 . ?
C1 O1 Co1 114.9(2) . . ?
C1 O1 Co1 127.7(2) . 18_545 ?
C5 N1 Co2 180.0 . . ?
C2 N2 Co1 104.6(2) . . ?
C2 N2 C3 115.1(3) . . ?
C3 N2 Co1 102.9(2) . . ?
O2 C4 C3 111.6(3) . . ?
N1 C5 S1 180.0 . . ?
N2 C2 C1 111.0(3) . . ?
O1 C1 C2 110.1(3) . . ?
N2 C3 C4 110.9(3) . . ?
Co1 S2 Co1 73.983(10) 2_655 16_655 ?
Co1 S2 Co1 73.983(10) . 17 ?
Co1 S2 Co1 73.981(10) 3_665 16_655 ?
Co1 S2 Co1 180.0 3_665 18_545 ?
Co1 S2 Co1 180.0 2_655 17 ?
Co1 S2 Co1 73.983(10) 2_655 18_545 ?
Co1 S2 Co1 180.0 . 16_655 ?
Co1 S2 Co1 106.018(10) 16_655 18_545 ?
Co1 S2 Co1 106.016(10) 17 16_655 ?
Co1 S2 Co1 106.018(10) 3_665 . ?
Co1 S2 Co1 73.982(10) . 18_545 ?
Co1 S2 Co1 106.019(10) 3_665 2_655 ?
Co1 S2 Co1 106.016(10) 17 18_545 ?
Co1 S2 Co1 106.018(10) . 2_655 ?
Co1 S2 Co1 73.982(10) 3_665 17 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 1.957(2) . ?
Co1 O1 1.959(2) . ?
Co1 O1 1.936(2) 17 ?
Co1 N2 2.180(3) . ?
Co1 S2 2.5872(4) . ?
Co2 O2 1.933(2) 2_655 ?
Co2 O2 1.933(2) 3_665 ?
Co2 O2 1.933(2) . ?
Co2 N1 2.071(5) . ?
S1 C5 1.638(7) . ?
O2 C4 1.395(4) . ?
O1 Co1 1.936(2) 18_545 ?
O1 C1 1.411(4) . ?
N1 C5 1.122(8) . ?
N2 C2 1.459(5) . ?
N2 C3 1.472(5) . ?
C4 C3 1.484(6) . ?
C2 C1 1.508(6) . ?
S2 Co1 2.5872(4) 3_665 ?
S2 Co1 2.5872(4) 18_545 ?
S2 Co1 2.5872(4) 16_655 ?
S2 Co1 2.5872(4) 2_655 ?
S2 Co1 2.5873(4) 17 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O2 C4 C3 -28.7(4) . . . . ?
Co1 O1 C1 C2 -32.1(4) . . . . ?
Co1 O1 C1 C2 -170.3(2) 18_545 . . . ?
Co1 N2 C2 C1 -36.6(4) . . . . ?
Co1 N2 C3 C4 -38.8(4) . . . . ?
Co2 O2 C4 C3 169.2(3) . . . . ?
O2 C4 C3 N2 46.8(5) . . . . ?
N2 C2 C1 O1 46.7(4) . . . . ?
C2 N2 C3 C4 -151.9(4) . . . . ?
C3 N2 C2 C1 75.6(4) . . . . ?
