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

data_7708066
_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
'C46 H40 Ir N4, Cl, 1.31(C H4 O), C0.69 H3.07 O0.69'
_chemical_formula_sum            'C48 H48.31 Cl Ir N4 O2'
_chemical_formula_weight         940.86
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.488(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3729(4)
_cell_length_b                   16.0231(3)
_cell_length_c                   17.1143(4)
_cell_measurement_reflns_used    35563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1160
_cell_measurement_theta_min      1.7560
_cell_volume                     4081.56(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0399883000
_diffrn_orient_matrix_UB_12      -0.0233200000
_diffrn_orient_matrix_UB_13      -0.0146633000
_diffrn_orient_matrix_UB_21      -0.0255415000
_diffrn_orient_matrix_UB_22      0.0373098000
_diffrn_orient_matrix_UB_23      -0.0039609000
_diffrn_orient_matrix_UB_31      0.0044439000
_diffrn_orient_matrix_UB_32      0.0048332000
_diffrn_orient_matrix_UB_33      -0.0400185000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.768
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.381
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             1897
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.166
_refine_diff_density_min         -2.012
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0256P)^2^+9.0291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8091
_reflns_number_total             9849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01960k2.cif
_cod_data_source_block           takimoto_autored
_cod_database_code               7708066
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Ir1Cl1N4C46H40
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.729
_reflns_odcompleteness_completeness 94.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.06
_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, All O(H) groups
2. Others
 Sof(O3)=Sof(H3)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=1-FVAR(1)
 Sof(O2)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C21(H21),
 C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C35(H35), C36(H36),
  C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3)
;
_shelx_res_checksum              82172
_shelx_hkl_checksum              72389
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.225
_oxdiff_exptl_absorpt_empirical_full_min 0.895