Asymmetric catalysis with a chiral-at-osmium complex.
Wang, Guanghui; Zhou, Zijun; Shen, Xiang; Ivlev, Sergei; Meggers, Eric; Chemical communications (Cambridge, England) 56 (2020) 7714–7717; doi:10.1039/d0cc03280h

data_7126701
_publ_section_title
;
 Asymmetric catalysis with a chiral-at-osmium complex.
;
_journal_issue                   56
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7714
_journal_page_last               7717
_journal_paper_doi               10.1039/d0cc03280h
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H29 N5 O2 Os, 2(F6 P)'
_chemical_formula_sum            'C36 H29 F12 N5 O2 Os P2'
_chemical_formula_weight         1043.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-01 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2495(3)
_cell_length_b                   10.7934(4)
_cell_length_c                   35.8310(11)
_cell_measurement_reflns_used    6883
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.94
_cell_measurement_theta_min      2.20
_cell_volume                     3577.1(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Diamond v4.5.3 (Brandenburg, 2018)'
_computing_publication_material  'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.3 mm diameter'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            60283
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.073
_diffrn_reflns_theta_min         2.203
_diffrn_source                   'microfocus X-ray tube'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.761
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6497
_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            yellow
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.062
_refine_diff_density_max         2.471
_refine_diff_density_min         -4.409
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Flack x determined using 4425 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         12430
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+9.8471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                11366
_reflns_number_total             12430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03280h2.cif
_cod_data_source_block           OsAux
_cod_depositor_comments
'Adding full bibliography for 7126701--7126702.cif.'
_cod_database_code               7126701
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.412
_shelx_estimated_absorpt_t_max   0.800
_shelx_res_checksum              69995