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_7707492
_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, 1.22(C H2 Cl2), 0.28(C6 H14)'
_chemical_formula_sum            'C41.88 H30.3 Cl2.45 Ir N3 O2'
_chemical_formula_weight         886.58
_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                 102.392(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.15128(17)
_cell_length_b                   27.4566(6)
_cell_length_c                   14.7617(3)
_cell_measurement_reflns_used    36645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.21
_cell_measurement_theta_min      2.03
_cell_volume                     3622.66(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0638
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            62023
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.048
_exptl_absorpt_coefficient_mu    3.907
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.783
_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             1749
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 6509 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         17479
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0445P)^2^+2.1765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15485
_reflns_number_total             17479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00783a2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7707490--7707494.cif.'
_cod_original_formula_sum        'C41.88 H30.30 Cl2.45 Ir N3 O2'
_cod_database_code               7707492
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.859
_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
 Cl7-C88 = Cl8-C88
 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
 Cl7-Cl8
 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
C53 \\sim C54 \\sim C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
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
Cl7 \\sim Cl8 \\sim C88: 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(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
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(Cl7) \\sim Ueq, Uanis(Cl8) \\sim Ueq, Uanis(C88) \\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
 C53, C54, C59, C60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 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
 Cl7, Cl8, C88
 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
 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)]+1*[Sof(Cl5)+Sof(Cl6)+
 Sof(C87)+Sof(H87A)+Sof(H87B)]+1*[Sof(Cl7)+Sof(Cl8)+Sof(C88)+Sof(H88A)+
 Sof(H88B)]=1 with esd of 0.0005
 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)
 Sof(Cl5)=Sof(Cl6)=Sof(C87)=Sof(H87A)=Sof(H87B)=FVAR(2)
 Sof(Cl7)=Sof(Cl8)=Sof(C88)=Sof(H88A)=Sof(H88B)=FVAR(3)
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), C88(H88A,H88B)
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              70333
_olex2_submission_special_instructions 'No special instructions were received'