Five-Coordinate Iridium(III) Complex with ΔΛ Chirality
Takimoto, Kazuyoshi; Watanabe, Yutaka; Yoshida, Jun; Sato, Hisako; Dalton Transactions  (2021) –; doi:10.1039/D1DT01960K

data_7708065
_publ_section_title
;
 Five-Coordinate Iridium(III) Complex with \D\L Chirality
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01960K
_journal_year                    2021
_chemical_formula_moiety         'C34 H32 Cl Ir N2'
_chemical_formula_sum            'C34 H32 Cl Ir N2'
_chemical_formula_weight         696.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-26 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                79.931(4)
_cell_angle_beta                 79.001(4)
_cell_angle_gamma                68.307(6)
_cell_formula_units_Z            2
_cell_length_a                   9.4178(6)
_cell_length_b                   11.1107(8)
_cell_length_c                   14.0254(6)
_cell_measurement_reflns_used    7445
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.4010
_cell_measurement_theta_min      3.2530
_cell_volume                     1329.82(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -46.00  37.00   0.50    0.05    --  -39.20  91.00-123.00  166
  2  \w    -35.00  36.00   0.50    0.05    --  -39.20  57.00-150.00  142
  3  \w    -68.00 -17.00   0.50    0.14    --  -94.50  30.00-180.00  102
  4  \w    -92.00 -10.00   0.50    0.05    --  -39.20 125.00-120.00  164
  5  \w    -91.00 -31.00   0.50    0.14    --  -94.50 125.00 -30.00  120
  6  \w    -69.00 -17.00   0.50    0.14    --  -94.50  30.00  60.00  104
  7  \w    -59.00 -19.00   0.50    0.05    --  -39.20 -77.00 150.00   80
  8  \w    -13.00  78.00   0.50    0.05    --   39.20 -91.00 123.00  182
  9  \w     77.00 144.00   0.50    0.14    --  109.49 -91.00 123.00  134
 10  \w     77.00 108.00   0.50    0.14    --  109.49 -94.00  60.00   62
 11  \w     42.00  99.00   0.50    0.14    --  109.49-125.00  90.00  114
 12  \w     30.00  74.00   0.50    0.14    --  109.49 -45.00  60.00   88
 13  \w     33.00  75.00   0.50    0.14    --  109.49 -45.00 120.00   84
 14  \w     32.00  68.00   0.50    0.14    --  109.49 -45.00 150.00   72
 15  \w     32.00  61.00   0.50    0.14    --  109.49 -45.00  90.00   58
 16  \w     77.00 173.00   0.50    0.14    --  109.49  30.00  90.00  192
 17  \w    140.00 177.00   0.50    0.14    --  109.49 125.00 -60.00   74
 18  \w    146.00 172.00   0.50    0.14    --  109.49 125.00-150.00   52
 19  \w    109.00 154.00   0.50    0.14    --  109.49  91.00-123.00   90
 20  \w     98.00 125.00   0.50    0.14    --  109.49 125.00 -30.00   54
 21  \w     93.00 118.00   0.50    0.14    --  109.49 125.00 -60.00   50
 22  \w     92.00 176.00   0.50    0.14    --  109.49 125.00  90.00  168
 23  \w     51.00  77.00   0.50    0.14    --  109.49 -45.00-120.00   52
 24  \w     53.00  79.00   0.50    0.14    --  109.49 -94.00 -90.00   52
 25  \w     40.00 116.00   0.50    0.14    --  109.49-125.00 -60.00  152
 26  \w     27.00  52.00   0.50    0.14    --  109.49 -30.00 -90.00   50
 27  \w     27.00  68.00   0.50    0.14    --  109.49 -30.00 -30.00   82
 28  \w     27.00  69.00   0.50    0.14    --  109.49 -30.00-120.00   84
 29  \w     32.00  68.00   0.50    0.14    --  109.49 -30.00-180.00   72
 30  \w     37.00  73.00   0.50    0.14    --  109.49 -45.00-180.00   72
 31  \w     32.00 117.00   0.50    0.14    --  109.49-125.00  30.00  170
 32  \w    -93.00 -66.00   0.50    0.14    --  -94.50 -45.00  30.00   54
 33  \w   -108.00 -83.00   0.50    0.05    --  -39.20-125.00  90.00   50
 34  \w   -115.00 -64.00   0.50    0.05    --  -39.20 -77.00 150.00  102
 35  \w   -124.00 -99.00   0.50    0.14    --  -94.50 -91.00 123.00   50
 36  \w   -172.00 -96.00   0.50    0.14    --  -94.50 -45.00  30.00  152
 37  \w   -108.00 -70.00   0.50    0.05    --  -39.20-125.00 -90.00   76
 38  \w   -110.00 -71.00   0.50    0.05    --  -39.20-125.00-120.00   78
 39  \w   -125.00-100.00   0.50    0.14    --  -94.50  91.00-123.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0414047000
_diffrn_orient_matrix_UB_12      0.0576279000
_diffrn_orient_matrix_UB_13      -0.1034411000
_diffrn_orient_matrix_UB_21      0.0712904000
_diffrn_orient_matrix_UB_22      0.1045488000
_diffrn_orient_matrix_UB_23      -0.0003535000
_diffrn_orient_matrix_UB_31      0.1574712000
_diffrn_orient_matrix_UB_32      -0.0911793000
_diffrn_orient_matrix_UB_33      -0.0445721000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13583
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.686
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.838
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+2.6299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4941
_reflns_number_total             5254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01960k2.cif
_cod_data_source_block           exp_73
_cod_database_code               7708065
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C34 H32 Ir N2 Cl'
_chemical_oxdiff_usercomment     YG129
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.281
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C32(H32A,H32B), C31(H31A,H31B), C13(H13A,
 H13B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C23(H23), C9(H9), C8(H8), C5(H5), C29(H29), C25(H25),
 C26(H26), C28(H28), C24(H24), C27(H27), C7(H7)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.754