Tetrahedral μ<sub>4</sub>-chloride and in situ generated octahedral μ<sub>6</sub>-sulfide templating Co<sub>8</sub> complexes with different distortions of the cube.
Yu, You-Zhu; Guo, Yu-Hua; Zhang, Yan-Ru; Tian, Xiu-Juan; Zhang, Xian-Ming; Chemical communications (Cambridge, England) 56 (2020) 4236–4239; doi:10.1039/d0cc01320j

data_7126095
_publ_section_title
;
 Tetrahedral \m<sub>4</sub>-chloride and in situ generated octahedral
 \m<sub>6</sub>-sulfide templating Co<sub>8</sub> 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 H51 Cl4 Co8 N5 O12'
_chemical_formula_sum            'C26 H51 Cl4 Co8 N5 O12'
_chemical_formula_weight         1238.95
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-23
_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                   14.8782(8)
_cell_length_b                   14.8782(8)
_cell_length_c                   16.9496(9)
_cell_measurement_reflns_used    7331
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.74
_cell_volume                     3249.3(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13610
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_min         1.985
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.288
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       block
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.899
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.361
_refine_ls_abs_structure_details
; 
 Flack x determined using 910 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.022(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1996
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.327
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0727P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.986
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                1900
_reflns_number_total             1996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01320j2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7126094--7126095.cif.'
_cod_original_cell_volume        3249.3(4)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               7126095
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H,H) groups 
2. Restrained distances 
 C3-C4 = C3'-C4' 
 1.53 with sigma of 0.01 
 C8-H8 
 0.97 with sigma of 0.01 
3. Uiso/Uaniso restraints and constraints 
Uanis(C3) = Uanis(C3') 
Uanis(C4) = Uanis(C4') 
4. Others 
 Sof(C3')=Sof(H3'A)=Sof(H3'B)=Sof(C4')=Sof(H4'A)=Sof(H4'B)=1-FVAR(1) 
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(1) 
 Fixed Sof: H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) H5A(0.5) H5B(0.5) 
 C6(0.5) H6A(0.5) H6B(0.5) 
5.a Secondary CH2 refined with riding coordinates: 
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C3'(H3'A,H3'B), C4'(H4'A, 
 H4'B), C5(H5A,H5B), C6(H6A,H6B) 
;
_shelx_res_checksum              98939
_olex2_submission_special_instructions 'No special instructions were received'