Oxidative C-O bond cleavage of dihydroxybenzenes and conversion of coordinated cyanide to carbonyl by a luminescent Os(VI) cyanonitrido complex
Xiang, Jing; Zhu, Jiang; Zhou, Miaomiao; Liu, Lu-Lu; Wang, Li-Xin; Peng, Min; Hou, Bi-Shun; Yiu, Shek-Man; To, Wai-Pong; Che, Chi-Ming; LAU, Kai Chung; Lau, Tai-Chu; Chemical Communications  (2022) –; doi:10.1039/D2CC03002K

data_7130248
_publ_section_title
;
 Oxidative C-O bond cleavage of dihydroxybenzenes and conversion of
 coordinated cyanide to carbonyl by a luminescent Os(VI) cyanonitrido
 complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03002K
_journal_year                    2022
_chemical_formula_sum            'C47 H34 Cl2 N5 O6 Os P'
_chemical_formula_weight         1056.86
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-02-13 deposited with the CCDC.	2022-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.841(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9692(7)
_cell_length_b                   13.1008(5)
_cell_length_c                   23.5542(10)
_cell_measurement_reflns_used    5696
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.6780
_cell_measurement_theta_min      2.1760
_cell_volume                     4146.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.2684
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_av_unetI/netI     0.1199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.301
_exptl_absorpt_correction_T_max  1.243
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.184
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7314
_refine_ls_number_restraints     1656
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0546
_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^)+9.6467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4931
_reflns_number_total             7314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03002k2.cif
_cod_data_source_block           no2s
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130248
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.713
_shelx_res_checksum              67717