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_7704640
_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         'C44 H52 N2 O7 Os'
_chemical_formula_sum            'C44 H52 N2 O7 Os'
_chemical_formula_weight         911.07
_chemical_name_common            (Egan)OsO
_chemical_name_systematic
(Oxo)(1,2-ethanedi-(2-(3,5-di-tert-butyl-2-oxyphenyl)amido)-benzoate)osmium(VI)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                105.229(2)
_cell_angle_beta                 104.4965(19)
_cell_angle_gamma                108.180(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0153(6)
_cell_length_b                   13.1218(7)
_cell_length_c                   14.0466(6)
_cell_measurement_reflns_used    9775
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.64
_cell_measurement_theta_min      2.50
_cell_volume                     2049.60(18)
_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-2013 (Sheldrick, 2013)'
_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 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.659
_diffrn_reflns_theta_min         1.612
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.162
_exptl_absorpt_correction_T_max  0.7802
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_type   numerical
_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    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_recrystallization_method
'Crystals were grown by vapor diffusion of methanol intoa benzene solution of the complex.'
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.7802
_exptl_transmission_factor_min   0.6140
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         12637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+0.7482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0332
_refine_ls_wR_factor_ref         0.0336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11999
_reflns_number_total             12637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01735c2.cif
_cod_data_source_block           eganoso
_cod_depositor_comments
'Adding full bibliography for 7704635--7704640.cif.'
_cod_original_cell_volume        2049.60(17)
_cod_database_code               7704640
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.703
_shelxl_version_number           2013-4
_shelx_res_checksum              93110