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_7710428
_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 Cl2 Co P2 Ru S3'
_chemical_formula_sum            'C50 H53 Cl2 Co P2 Ru S3'
_chemical_formula_weight         1042.94
_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     iterative
_audit_creation_date             2021-11-29
_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                 104.1730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0207(7)
_cell_length_b                   24.9378(13)
_cell_length_c                   14.6486(7)
_cell_measurement_reflns_used    9740
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      26.898
_cell_measurement_theta_min      2.450
_cell_volume                     4611.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      220.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            60775
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.904
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'sealed tube'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5703
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1197 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.7651.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.5703
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         9928
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0253P)^2^+7.0054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8666
_reflns_number_total             9928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01534j2.cif
_cod_data_source_block           1
_cod_database_code               7710428
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.818
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 S1, Ru1
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.01
3. Others
 Sof(H14c)=Sof(H14d)=Sof(H11c)=Sof(H11d)=Sof(C13B)=Sof(H13c)=Sof(H13d)=
 Sof(C12B)=Sof(H12c)=Sof(H12d)=1-FVAR(1)
 Sof(H14a)=Sof(H14b)=Sof(H11a)=Sof(H11b)=Sof(C13A)=Sof(H13a)=Sof(H13b)=
 Sof(C12A)=Sof(H12a)=Sof(H12b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C14(H14c,H14d), C11(H11a,H11b), C11(H11c,H11d), C13A(H13a,
 H13b), C12A(H12a,H12b), C13B(H13c,H13d), C12B(H12c,H12d)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C34(H34), C20(H20), C38(H38), C19(H19), C44(H44),
 C26(H26), C32(H32), C22(H22), C18(H18), C28(H28), C24(H24), C37(H37), C25(H25),
  C36(H36), C35(H35), C23(H23), C29(H29), C43(H43), C40(H40), C31(H31),
 C48(H48), C50(H50), C46(H46), C30(H30), C42(H42), C41(H41), C47(H47), C49(H49)
4.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c), C7(H7a,H7b,H7c), C10(H10a,
 H10b,H10c)
;
_shelx_res_checksum              61926
_olex2_submission_special_instructions 'No special instructions were received'