Migratory Insertion and Hydrogenation of a Bridging Azide in Thiolate-Bridged Dicobalt Reaction Platform
Zhang, Yixin; Tong, Peng; Yang, Dawei; Li, Jianzhe; Wang, Baomin; Qu, Jingping; Chem. Commun.  (2017) –; doi:10.1039/C7CC05092E

data_7120535
_publ_section_title
;
 Migratory Insertion and Hydrogenation of a Bridging Azide in
 Thiolate-Bridged Dicobalt Reaction Platform
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05092E
_journal_year                    2017
_chemical_formula_sum            'C49.5 H61 B Cl Co2 I O S2'
_chemical_formula_weight         1027.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                83.6460(10)
_cell_angle_beta                 80.2610(10)
_cell_angle_gamma                86.086(2)
_cell_formula_units_Z            4
_cell_length_a                   8.8838(2)
_cell_length_b                   21.8060(6)
_cell_length_c                   25.6046(6)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.33
_cell_volume                     4852.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51619
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.956
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.220
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5426
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         17097
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0498P)^2^+8.3153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12932
_reflns_number_total             17097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc05092e2.cif
_cod_data_source_block           1_CCDC1
_cod_original_formula_sum        'C49.50 H61 B Cl Co2 I O S2'
_cod_database_code               7120535
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.623
_shelx_estimated_absorpt_t_max   0.734
_shelx_res_checksum              31476