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_4345001
_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_absolute_configuration ad
_chemical_formula_moiety         'C31 H27 Ir N2 O2 S'
_chemical_formula_sum            'C31 H28 Ir N2 O2 S'
_chemical_formula_weight         684.81
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.41597(13)
_cell_length_b                   15.5922(2)
_cell_length_c                   17.5922(3)
_cell_measurement_reflns_used    7826
_cell_measurement_temperature    150
_cell_measurement_theta_max      62.4760
_cell_measurement_theta_min      3.7680
_cell_volume                     2582.81(7)
_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      150
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.884
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15022
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.632
_diffrn_reflns_theta_min         3.788
_exptl_absorpt_coefficient_mu    11.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30129
_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    1.761
_exptl_crystal_description       plate
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.30129
_refine_diff_density_max         1.592
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 1710 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0222
_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^+4.1892P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.869
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4030
_reflns_number_total             4092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02494_si_002.cif
_cod_data_source_block           lambda-3
_cod_database_code               4345001
_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:
 C22(H22), C21(H21), C27(H27), C24(H24), C13(H13), C25(H25), C11(H11),
 C10(H10), C9(H9), C19(H19), C15(H15), C14(H14), C26(H26), C8(H8), C20(H20),
 C5(H5), C4(H4), C16(H16), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C30(H30a,H30b,H30c)
;
_olex2_submission_special_instructions 'No special instructions were received'