Reaction of an osmium(VI) nitrido complex with enamines generated <i>in situ</i> from ketones and anilines.
Wang, Lei; Wang, Li-Xin; Liu, Zhao-Long; Xu, Fang; Qi, Rui-Yue; Man, Wai-Lun; Xiang, Jing; Liu, Ji-Yan; Lau, Tai-Chu; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14052–14058; doi:10.1039/d5dt01334h

data_7719553
_publ_section_title
;
 Reaction of an osmium(VI) nitrido complex with enamines generated <i>in
 situ</i> from ketones and anilines.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14052
_journal_page_last               14058
_journal_paper_doi               10.1039/d5dt01334h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C53.5 H43 N8 O5 Os P'
_chemical_formula_weight         1099.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-11-16 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.161(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3204(3)
_cell_length_b                   16.0179(4)
_cell_length_c                   23.9832(8)
_cell_measurement_reflns_used    9328
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.55
_cell_measurement_theta_min      3.35
_cell_volume                     4982.8(2)
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65163
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.543
_diffrn_reflns_theta_min         3.346
_diffrn_source                   'micro focus'
_exptl_absorpt_coefficient_mu    5.589
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6023
_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            purple
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.407
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         10171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+3.9887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9183
_reflns_number_total             10171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01334h2.cif
_cod_data_source_block           1_a_CCDC1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C53.50 H43 N8 O5 Os P'
_cod_database_code               7719553
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              35151