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_7130249
_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            'C39 H53 N7 O6 Os'
_chemical_formula_weight         906.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-02-13 deposited with the CCDC.	2022-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.4560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.5994(16)
_cell_length_b                   12.6388(5)
_cell_length_c                   26.0050(12)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.43
_cell_volume                     8882.2(7)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'Bruker Saint'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            66109
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'micro focus'
_exptl_absorpt_coefficient_mu    2.919
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.163
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         9119
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0411P)^2^+36.0169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7103
_reflns_number_total             9119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03002k2.cif
_cod_data_source_block           1_a_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7130249
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              48697
_shelx_fab_checksum              72016