Optically active bis(aminophenols) and their metal complexes
Carbonel, Halen; Mikulski, Timothy D.; Nugraha, Kahargyan; Johnston, James; Wang, Yichun; Brown, Seth N.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02436A

data_7713820
_publ_section_title
;
 Optically active bis(aminophenols) and their metal complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02436A
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C46 H56 N2 O7 Os'
_chemical_formula_sum            'C46 H56 N2 O7 Os'
_chemical_formula_weight         939.12
_chemical_name_common            '(A,R,R)-(Bdan)OsO . (C,R,R)-(Bdan)OsO'
_chemical_name_systematic
'(A,R,R)-Oxo(2,3-butanediylbis(2-(2-oxy-3,5-di-tert-butylphenyl)amido)benzoate)osmium (C,R,R)-Oxo(2,3-butanediylbis(2-(2-oxy-3,5-di-tert-butylphenyl)amido)benzoate)osmium cocrystal'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8873(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7971(4)
_cell_length_b                   13.0573(4)
_cell_length_c                   25.7200(8)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.404
_cell_measurement_theta_min      3.801
_cell_volume                     4275.0(2)
_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 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            93554
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.520
_diffrn_reflns_theta_min         1.727
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.049
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6472
_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            'dark brown'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_recrystallization_method
'BdanH4 was metalated with OsO(OCH2CH2O) in benzene at 80 degC, and the crude material chromatogaphed on silica gel, eluting with 1:2 hexane:dichloromethane.  Crystals were deposited from a hexane solution of the eluate.'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.081
_exptl_transmission_factor_max   0.7536
_exptl_transmission_factor_min   0.6472
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 7282 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         16870
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0195
_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^)+(0.0271P)^2^+0.5870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                15998
_reflns_number_total             16870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02436a2.cif
_cod_data_source_block           pseudorac
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C92 H112 N4 O14 Os2'
_cod_original_formula_weight         1878.25
_cod_original_formula_moiety         'C46 H56 N2 O7 Os, C46 H56 N2 O7 Os'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7713820
_shelx_estimated_absorpt_t_min   0.531
_shelx_estimated_absorpt_t_max   0.640
_shelxl_version_number           2013-4
_shelx_res_checksum              88725