High-valent osmium iminoxolene complexes.
Gianino, Jacqueline; Erickson, Alexander N.; Markovitz, Sean J.; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8504–8515; doi:10.1039/d0dt01735c

data_7704636
_publ_section_title
;
 High-valent osmium iminoxolene complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8504
_journal_page_last               8515
_journal_paper_doi               10.1039/d0dt01735c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C26 H37 N O4 Os'
_chemical_formula_sum            'C26 H37 N O4 Os'
_chemical_formula_weight         617.76
_chemical_name_common            (^H^ap)OsO(pin)
_chemical_name_systematic
Oxo(pinacolato)(2-(phenylimido)-4,6-di-tert-butylphenoxo)-osmium(VI)
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1408(4)
_cell_length_b                   16.5112(6)
_cell_length_c                   15.0329(5)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.37
_cell_volume                     2499.90(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35684
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.613
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.132
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_recrystallization_method
'Crystals formed on vapor diffusion of acetonitrile into a solution of the compound in chloroform.'
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.5578
_refine_diff_density_max         2.848
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+2.4639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6459
_reflns_number_total             7245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01735c2.cif
_cod_data_source_block           ospin
_cod_depositor_comments
'Adding full bibliography for 7704635--7704640.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7704636
_shelx_estimated_absorpt_t_min   0.289
_shelx_estimated_absorpt_t_max   0.578
_shelxl_version_number           2013-4
_shelx_res_checksum              80775