A single carbon atom controls the geometry and reactivity of Co<sup>II</sup>(N<sub>2</sub>S<sub>2</sub>) complexes.
Jana, Manish; Quiroz, Manuel; Darensbourg, Marcetta Y.; Chemical communications (Cambridge, England) 60 (2024) 1128–1131; doi:10.1039/d3cc05394f

data_7132485
_publ_section_title
;
 A single carbon atom controls the geometry and reactivity of
 Co<sup>II</sup>(N<sub>2</sub>S<sub>2</sub>) complexes.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1128
_journal_page_last               1131
_journal_paper_doi               10.1039/d3cc05394f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C54 H70 Co2 N6 O8 S4 W2, [+ solvents]'
_chemical_formula_sum            'C54 H70 Co2 N6 O8 S4 W2'
_chemical_formula_weight         1544.96
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive,Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2023-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.177(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5425(16)
_cell_length_b                   11.5431(8)
_cell_length_c                   24.7944(17)
_cell_measurement_reflns_used    9740
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      66.755
_cell_measurement_theta_min      3.981
_cell_volume                     6356.9(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            219133
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.981
_diffrn_reflns_theta_max         66.981
_diffrn_reflns_theta_min         2.121
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.185
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1278 before and 0.0772 after correction.
The Ratio of minimum to maximum transmission is 0.6500.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic greenish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       plate
_exptl_crystal_F_000             3064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF ETHER'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         11307
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+22.0312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9343
_reflns_number_total             11307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05394f2.cif
_cod_data_source_block           mj_co_dadtbz_wco4_0ma
_cod_depositor_comments
'Adding full bibliography for 7132482--7132485.cif.'
_cod_database_code               7132485
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.194
_shelx_estimated_absorpt_t_min   0.121
_olex2_refinement_description
;
1. Restrained distances
 C32B-C31B \\sim C32A-C31A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C34B) = Uanis(C34A)
Uanis(C35B) = Uanis(C35A)
Uanis(C36B) = Uanis(C36A)
Uanis(C25A) = Uanis(C25B)
Uanis(C31A) = Uanis(C31B)
Uanis(C32A) = Uanis(C32B)
Uanis(C31B) = Uanis(C51)
Uanis(C32B) = Uanis(C50)
Uanis(C27B) = Uanis(C27A)
Uanis(C26A) = Uanis(C26B)
3. Others
 Sof(H37A)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=
 Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C31B)=Sof(H31C)=Sof(H31D)=
 Sof(C36B)=Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(C34B)=Sof(H34B)=Sof(C32B)=
 Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(H37)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C31A)=Sof(H31A)=Sof(H31B)=
 Sof(C36A)=Sof(H36A)=Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C32A)=
 Sof(H32A)=Sof(H32B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C50(H50A,H50B), C13(H13A,H13B), C21(H21A,H21B), C42(H42A,
 H42B), C51(H51A,H51B), C20(H20A,H20B), C43(H43A,H43B), C11(H11A,H11B), C3(H3A,
 H3B), C2(H2A,H2B), C1(H1A,H1B), C41(H41A,H41B), C40(H40A,H40B), C10(H10A,H10B),
  C33(H33A,H33B), C31A(H31A,H31B), C31B(H31C,H31D), C32A(H32A,H32B), C32B(H32C,
 H32D)
4.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C9(H9), C37(H37), C37(H37A), C52(H52), C45(H45), C5(H5), C15(H15),
 C16(H16), C49(H49), C25A(H25A), C25B(H25B), C17(H17), C18(H18), C19(H19),
 C8(H8), C46(H46), C48(H48), C47(H47), C6(H6), C36A(H36A), C36B(H36B),
 C35A(H35A), C35B(H35B), C7(H7), C34A(H34A), C34B(H34B)
4.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C54(H54A,
 H54B,H54C), C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 254 electrons were 
found in a volume of 856\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.25[H20], 0.25[C3H7NO], 0.25[C3H7NO] per Unit Cell 
which account for 100 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24593
_shelx_hkl_checksum              53277
_shelx_fab_checksum              56862
_platon_squeeze_special_details
;
A solvent mask was calculated and 0 electrons were 
found in a volume of 32\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C3H7NO] per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'