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_7710429
_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         'C40 H47 Cl Co P2 Ru S3, C H2 Cl2, C24 H20 B'
_chemical_formula_sum            'C65 H69 B Cl3 Co P2 Ru S3'
_chemical_formula_weight         1285.48
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-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             2021-11-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-03-24 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.051(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0693(10)
_cell_length_b                   27.421(2)
_cell_length_c                   18.1837(15)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      28.052
_cell_measurement_theta_min      2.239
_cell_volume                     5906.3(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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  0.0777
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64814
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         1.873
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1050 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.9147.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         14408
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0377P)^2^+8.7964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8880
_reflns_number_total             14408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01534j2.cif
_cod_data_source_block           1_CCDC1
_cod_original_cell_volume        5906.5(8)
_cod_database_code               7710429
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.831
_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. Rigid bond restraints
 P1, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C14(H14A,H14B), C12(H12A,H12B), C15(H15A,H15B), C11(H11A,
 H11B), C13(H13A,H13B), C65(H65A,H65B)
3.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C62(H62), C48(H48), C60(H60), C26(H26), C49(H49), C63(H63),
 C64(H64), C27(H27), C25(H25), C46(H46), C52(H52), C61(H61), C28(H28), C34(H34),
  C51(H51), C58(H58), C18(H18), C50(H50), C36(H36), C30(H30), C22(H22),
 C42(H42), C19(H19), C43(H43), C44(H44), C45(H45), C32(H32), C20(H20), C40(H40),
  C33(H33), C31(H31), C21(H21), C39(H39), C54(H54), C37(H37), C57(H57),
 C38(H38), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C),
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              65120
_olex2_submission_special_instructions 'No special instructions were received'