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_7132484
_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         'C27 H33 Co N3 O5 S2 W, C4 H10 O'
_chemical_formula_sum            'C31 H43 Co N3 O6 S2 W'
_chemical_formula_weight         860.58
_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 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-12
_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                 105.716(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2062(12)
_cell_length_b                   14.5330(13)
_cell_length_c                   18.5933(17)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      25.054
_cell_measurement_theta_min      2.199
_cell_volume                     3435.1(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      110.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61741
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.055
_diffrn_reflns_theta_max         25.055
_diffrn_reflns_theta_min         2.276
_diffrn_source                   'sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.995
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1307 before and 0.0754 after correction.
The Ratio of minimum to maximum transmission is 0.6718.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic orangish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF ETHER'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.821
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6066
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+13.7919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5672
_reflns_number_total             6066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05394f2.cif
_cod_data_source_block           mj_co_dabz_w_co_4_1_0m
_cod_depositor_comments
'Adding full bibliography for 7132482--7132485.cif.'
_cod_database_code               7132484
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.502
_shelx_estimated_absorpt_t_min   0.240
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C6A \\sim N2-C6B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14B) = Uanis(C14A)
Uanis(C15B) = Uanis(C15A)
Uanis(C26B) = Uanis(C26A)
Uanis(C6A) = Uanis(C6B)
Uanis(C5A) = Uanis(C5B)
Uanis(C6B) = Uanis(C6A) = Uanis(C23)
Uanis(C5B) = Uanis(C5A) = Uanis(C24)
4. Others
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C14B)=Sof(H14C)=
 Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C26B)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=1-FVAR(1)
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C14A)=Sof(H14A)=
 Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C5B(H5BA,H5BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C7(H7A,H7B),
 C14A(H14A,H14B), C14B(H14C,H14D), C15A(H15A,H15B), C15B(H15C,H15D), C16(H16A,
 H16B), C23(H23A,H23B), C24(H24A,H24B), C29(HC,HD), C30(HE,HF)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22)
5.c Idealised Me refined as rotating group:
 C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C28(H,HA,HB), C31(HG,HH,HI)
;
_shelx_res_checksum              31101
_shelx_hkl_checksum              86599
_olex2_submission_special_instructions 'No special instructions were received'