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_7126702
_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         'C29 H23 N5 O Os, 2(F6 P)'
_chemical_formula_sum            'C29 H23 F12 N5 O Os P2'
_chemical_formula_weight         937.66
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                70.816(2)
_cell_angle_beta                 78.674(2)
_cell_angle_gamma                76.497(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2056(8)
_cell_length_b                   15.5349(9)
_cell_length_c                   16.0807(9)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.63
_cell_volume                     3231.2(3)
_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 v4.6.2 (Brandenburg, 2020)'
_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 0.998
_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  0.0743
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            243051
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.363
_diffrn_reflns_theta_min         2.137
_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    4.149
_exptl_absorpt_correction_T_max  0.745687
_exptl_absorpt_correction_T_min  0.686536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.064
_refine_diff_density_max         2.307
_refine_diff_density_min         -1.936
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Flack x determined using 10334 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1814
_refine_ls_number_reflns         30785
_refine_ls_number_restraints     471
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+9.7390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                26058
_reflns_number_total             30785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03280h2.cif
_cod_data_source_block           Oslamb
_cod_depositor_comments
'Adding full bibliography for 7126701--7126702.cif.'
_cod_database_code               7126702
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.667
_shelx_estimated_absorpt_t_max   0.777
_shelx_res_checksum              83500
_shelx_fab_checksum              40753