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_7704638
_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         'C40 H50 Cl2 N2 O2 Os, C D Cl3'
_chemical_formula_sum            'C41 H50 Cl5 D N2 O2 Os'
_chemical_formula_weight         972.29
_chemical_name_common
;
Os(^Ph^ap)~2~Cl~2~ . CDCl~3~
;
_chemical_name_systematic
'Cis-bis-(2-(phenylimido)-4,6-di-tert-butylphenoxo)dichloroosmium(VI) chloroform solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8082(7)
_cell_length_b                   40.829(2)
_cell_length_c                   12.5096(7)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.2465
_cell_measurement_theta_min      2.521
_cell_volume                     8584.9(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33267
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.244
_diffrn_reflns_theta_min         1.995
_exptl_absorpt_coefficient_mu    3.317
_exptl_absorpt_correction_T_max  0.745700
_exptl_absorpt_correction_T_min  0.664400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Square
_exptl_crystal_F_000             3904
_exptl_crystal_recrystallization_method
'Crystals were deposited from a solution of the material dissolvedin CDCl3.'
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.186
_exptl_transmission_factor_max   0.745700
_exptl_transmission_factor_min   0.664400
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2331 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0066P)^2^+7.1970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0322
_refine_ls_wR_factor_ref         0.0327
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5033
_reflns_number_total             5294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01735c2.cif
_cod_data_source_block           Final
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7704635--7704640.cif.
;
_cod_original_cell_volume        8584.8(8)
_cod_original_formula_sum        'C41 H50 D Cl5 N2 O2 Os'
_cod_database_code               7704638
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              5297