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_7710432
_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 Cl2 Co P2 Ru S3, C4 H8 O'
_chemical_formula_sum            'C44 H55 Cl2 Co O P2 Ru S3'
_chemical_formula_weight         988.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                94.842(2)
_cell_angle_beta                 105.592(2)
_cell_angle_gamma                93.863(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4855(10)
_cell_length_b                   12.5440(11)
_cell_length_c                   15.9637(14)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      28.087
_cell_measurement_theta_min      2.352
_cell_volume                     2197.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      295.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.1030
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35296
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.230
_diffrn_reflns_theta_min         1.997
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0898 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.9300.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6935
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         10702
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0460P)^2^+1.9417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6177
_reflns_number_total             10702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01534j2.cif
_cod_data_source_block           1_CCDC4
_cod_database_code               7710432
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.669
_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
 C42-C41 = C42-C43 = C43-C44
 1.45 with sigma of 0.02
 C43-C42
 1.45 with sigma of 0.02
 O1-C41 \\sim O1-C44
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C41 \\sim C44 \\sim C43 \\sim C42: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O1, C41, C44, C43, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C27(H27A,
 H27B), C28(H28A,H28B), C41(H41A,H41B), C44(H44A,H44B), C43(H43A,H43B),
 C42(H42A,H42B)
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), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
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)
;
_shelx_res_checksum              64503
_olex2_submission_special_instructions 'No special instructions were received'