Chiral Recognition and Dynamic Thermodynamic Resolution of Sulfoxides by Chiral Iridium(III) Complexes
Yao, Su-Yang; Chen, Xing-Yang; Ou, Yan-Ling; Ye, Bao-Hui; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.6b02494

data_4344999
_publ_section_title
;
 Chiral Recognition and Dynamic Thermodynamic Resolution of Sulfoxides by
 Chiral Iridium(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b02494
_journal_year                    2017
_chemical_formula_moiety         'C31 H27 Ir N2 O2 S'
_chemical_formula_sum            'C31 H27 Ir N2 O2 S'
_chemical_formula_weight         683.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.118(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7792(10)
_cell_length_b                   9.7493(6)
_cell_length_c                   16.6251(15)
_cell_measurement_reflns_used    1626
_cell_measurement_temperature    153
_cell_measurement_theta_max      54.96
_cell_measurement_theta_min      7.19
_cell_volume                     2555.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_av_unetI/netI     0.1002
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23252
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.222
_exptl_absorpt_coefficient_mu    5.338
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.073
_refine_diff_density_max         4.764
_refine_diff_density_min         -2.944
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0350P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5004
_reflns_number_total             5810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02494_si_002.cif
_cod_data_source_block           rac-3
_cod_database_code               4344999
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C24(H24), C27(H27), C25(H25), C2(H2), C9(H9), C20(H20), C22(H22),
 C16(H16), C10(H10), C15(H15), C21(H21), C26(H26), C3(H3), C13(H13), C5(H5),
 C4(H4), C8(H8), C19(H19), C14(H14)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'