Effects of geometrical isomerism on emissive behaviour of heteroleptic cyclometalated Ir(III) complexes.
Jinsenji, Yoshiki; Takimoto, Kazuyoshi; Yoshida, Jun; Mori, Shigeki; Watanabe, Yutaka; Sato, Hisako; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8506–8511; doi:10.1039/d1dt00783a

data_7707494
_publ_section_title
;
 Effects of geometrical isomerism on emissive behaviour of heteroleptic
 cyclometalated Ir(III) complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8506
_journal_page_last               8511
_journal_paper_doi               10.1039/d1dt00783a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C39 H24 Ir N3 O2, 1.18(C H2 Cl2), 0.32(C6 H14)'
_chemical_formula_sum            'C42.1 H30.85 Cl2.36 Ir N3 O2'
_chemical_formula_weight         886.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-18 deposited with the CCDC.	2021-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.475(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.15927(16)
_cell_length_b                   27.4078(5)
_cell_length_c                   14.7784(3)
_cell_measurement_reflns_used    42025
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      2.04
_cell_volume                     3622.31(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62123
_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         2.049
_exptl_absorpt_coefficient_mu    3.901
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1750
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 7002 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         17491
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0448P)^2^+7.8015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                16041
_reflns_number_total             17491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00783a2.cif
_cod_data_source_block           shelxl_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7707490--7707494.cif.'
_cod_original_formula_sum        'C42.10 H30.85 Cl2.36 Ir N3 O2'
_cod_database_code               7707494
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.696
_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. Restrained distances
 Cl1-C79 = Cl2-C79
 1.78 with sigma of 0.02
 Cl3-C80 = Cl4-C80
 1.78 with sigma of 0.02
 Cl5-C87 = Cl6-C87
 1.78 with sigma of 0.02
 C81-C82 = C82-C83 = C83-C84 = C84-C85 = C85-C86
 1.55 with sigma of 0.02
 Cl1-Cl2
 2.85 with sigma of 0.04
 Cl3-Cl4
 2.85 with sigma of 0.04
 Cl5-Cl6
 2.85 with sigma of 0.04
 C81-C83 = C82-C84 = C83-C85 = C84-C86
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C79: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Cl3 \\sim Cl4 \\sim C80: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Cl5 \\sim Cl6 \\sim C87: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C79) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(Cl3) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(C80) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(Cl5) \\sim Ueq, Uanis(Cl6) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl1, Cl2, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, Cl4, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5, Cl6, C87
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C81, C82, C83, C84, C85, C86
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl5)=Sof(Cl6)=Sof(C87)=Sof(H87A)=Sof(H87B)=1-FVAR(1)
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C83)=
 Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C80(H80A,H80B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,
 H84B), C85(H85A,H85B), C87(H87A,H87B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37), C38(H38),
 C39(H39), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50), C51(H51),
  C52(H52), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C63(H63),
 C64(H64), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C75(H75), C76(H76),
  C77(H77), C78(H78)
6.c Idealised Me refined with riding coordinates:
 C81(H81A,H81B,H81C), C86(H86A,H86B,H86C)
;
_shelx_res_checksum              2328
_olex2_submission_special_instructions 'No special instructions were received'