Asymmetric Synthesis of Enantiomerically Pure Mono- and Binuclear Bis(cyclometalated) Iridium(III) Complexes.
Yao, Su-Yang; Ou, Yan-Ling; Ye, Bao-Hui; Inorganic chemistry 55 (2016) 6018–6026; doi:10.1021/acs.inorgchem.6b00527

data_4347726
_publ_section_title
;
 Asymmetric Synthesis of Enantiomerically Pure Mono- and Binuclear
 Bis(cyclometalated) Iridium(III) Complexes.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6018
_journal_page_last               6026
_journal_paper_doi               10.1021/acs.inorgchem.6b00527
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C26 H22 Ir N4, F6 P'
_chemical_formula_sum            'C26 H22 F6 Ir N4 P'
_chemical_formula_weight         727.64
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.92212(13)
_cell_length_b                   8.92212(13)
_cell_length_c                   32.0341(8)
_cell_measurement_reflns_used    19102
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.9310
_cell_measurement_theta_min      2.7210
_cell_volume                     2550.05(8)
_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 0.851
_diffrn_measured_fraction_theta_max 0.997
_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  0.1043
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.851
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            43124
_diffrn_reflns_point_group_measured_fraction_full 0.843
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         61.164
_diffrn_reflns_theta_min         4.957
_exptl_absorpt_coefficient_mu    11.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00972
_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    1.895
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 1778 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.021(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+1.8612P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.835
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                3778
_reflns_number_total             3889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00527_si_002.cif
_cod_data_source_block           dp-cn
_cod_original_cell_volume        2550.05(10)
_cod_database_code               4347726
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H14(0.052) H13(0.041) H3(0.045) H2(0.041) H26A(0.068) H26B(0.068)
 H26C(0.068) H22(0.049) H5(0.056) H4(0.059) H20(0.061) H19(0.055) H16(0.055)
 H15(0.057) H8(0.056) H21(0.053) H11(0.055) H10(0.077) H24A(0.075) H24B(0.075)
 H24C(0.075) H9(0.071)
 Fixed X: H14(-0.1963) H13(0.0208) H3(0.5795) H2(0.4895) H26A(0.0846)
 H26B(0.0276) H26C(0.1896) H22(0.5398) H5(0.4256) H4(0.5514) H20(0.3402)
 H19(0.1329) H16(-0.0519) H15(-0.2355) H8(0.2813) H21(0.548) H11(0.2037)
 H10(0.1258) H24A(0.8432) H24B(0.803) H24C(0.8695) H9(0.1624)
 Fixed Y: H14(0.5374) H13(0.4244) H3(0.799) H2(0.5689) H26A(-0.2142) H26B(-
 0.1907) H26C(-0.2613) H22(0.221) H5(0.7233) H4(0.878) H20(0.3407) H19(0.4171)
 H16(0.4945) H15(0.5689) H8(0.5746) H21(0.2377) H11(0.108) H10(0.156)
 H24A(0.0913) H24B(-0.0148) H24C(0.1492) H9(0.3927)
 Fixed Z: H14(-0.0112) H13(-0.0355) H3(0.0316) H2(0.053) H26A(-0.0144)
 H26B(0.0325) H26C(0.024) H22(0.0797) H5(-0.0848) H4(-0.0375) H20(0.1868)
 H19(0.1489) H16(0.1075) H15(0.0606) H8(-0.1247) H21(0.1516) H11(-0.0672) H10(-
 0.135) H24A(-0.0289) H24B(0.0098) H24C(0.0178) H9(-0.1634)
;
_olex2_submission_special_instructions 'No special instructions were received'