Reversible Binding of Dinitrogen on a Thiolate-Bridged Cobalt-Ruthenium Complex Supported by a Flexible Bidentate Phosphine Ligand
Dong, Wenjing; Yang, Dawei; Mei, Tao; Wang, Baomin; Qu, Jingping; Dalton Transactions  (2022) –; doi:10.1039/D2DT01534J

data_7710430
_publ_section_title
;
 Reversible Binding of Dinitrogen on a Thiolate-Bridged Cobalt-Ruthenium
 Complex Supported by a Flexible Bidentate Phosphine Ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01534J
_journal_year                    2022
_chemical_formula_moiety
'C50 H53 Cl Co P2 Ru S3, C4 H10 O, C4 H8 O, C24 H20 B'
_chemical_formula_sum            'C82 H91 B Cl Co O2 P2 Ru S3'
_chemical_formula_weight         1472.92
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.809(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.460(3)
_cell_length_b                   30.325(6)
_cell_length_c                   21.269(4)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    233.0
_cell_measurement_theta_max      25.381
_cell_measurement_theta_min      2.232
_cell_volume                     7365(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      233.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1347
_diffrn_reflns_av_unetI/netI     0.0991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68494
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.036
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5126
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1615 before and 0.0856 after correction. The Ratio of minimum to maximum transmission is 0.6877. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       block
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.5126
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         12976
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0749
_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/[\s^2^(Fo^2^)+(0.0655P)^2^+19.5467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8025
_reflns_number_total             12976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01534j2.cif
_cod_data_source_block           1_CCDC2
_cod_original_cell_volume        7366(3)
_cod_database_code               7710430
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.861
_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
 C80-C79 = C81-C80 = C82-C81
 1.45 with sigma of 0.02
 O2-C82 \\sim O2-C79
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C82 \\sim C81 \\sim C80 \\sim C79: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O2, C79, C80, C81, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C76(H76a,
 H76b), C77(H77a,H77b), C79(H79a,H79b), C80(H80a,H80b), C81(H81a,H81b),
 C82(H82a,H82b)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C56(H56), C67(H67), C66(H66), C52(H52), C68(H68), C58(H58), C55(H55),
 C74(H74), C53(H53), C65(H65), C70(H70), C72(H72), C71(H71), C64(H64), C62(H62),
  C59(H59), C54(H54), C60(H60), C61(H61), C73(H73)
5.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C75(H75a,H75b,H75c), C78(H78a,H78b,H78c)
;
_shelx_res_checksum              10464
_olex2_submission_special_instructions 'No special instructions were received'