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_7707493
_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, C H2 Cl2'
_chemical_formula_sum            'C40 H26 Cl2 Ir N3 O2'
_chemical_formula_weight         843.74
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-09
_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                106.596(2)
_cell_angle_beta                 109.535(2)
_cell_angle_gamma                103.187(2)
_cell_formula_units_Z            4
_cell_length_a                   12.2740(2)
_cell_length_b                   16.9938(3)
_cell_length_c                   18.1515(5)
_cell_measurement_reflns_used    25933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.30
_cell_measurement_theta_min      1.80
_cell_volume                     3192.43(15)
_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 0.998
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54637
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.773
_exptl_absorpt_coefficient_mu    4.392
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.526
_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    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.052
_refine_diff_density_min         -2.091
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         15392
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0345P)^2^+6.3175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12083
_reflns_number_total             15392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00783a2.cif
_cod_data_source_block           shelxl_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7707490--7707494.cif.'
_cod_original_cell_volume        3192.42(13)
_cod_database_code               7707493
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.540
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Cl3, Cl13}
3. Restrained distances
 Cl1-C79 = Cl2-C79 = Cl11-C179 = Cl12-C179
 1.78 with sigma of 0.02
 Cl3-C80 = Cl4-C80 = Cl13-C180 = Cl14-C180
 1.78 with sigma of 0.02
 Cl1-Cl2 = Cl11-Cl12 = Cl3-Cl4 = Cl13-Cl14
 2.85 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C79 \\sim Cl11 \\sim Cl12 \\sim C179: 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 0.01 and sigma for terminal
atoms of 0.02
Cl13 \\sim Cl14 \\sim C180: 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, Uanis(Cl11)
\\sim Ueq, Uanis(Cl12) \\sim Ueq, Uanis(C179) \\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
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl13) \\sim Ueq, Uanis(Cl14) \\sim Ueq, Uanis(C180) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3) = Uanis(Cl13)
5. Rigid body (RIGU) restrains
 Cl1, Cl2, C79, Cl11, Cl12, C179
 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
 Cl13, Cl14, C180
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl11)=Sof(Cl12)=Sof(C179)=Sof(H17A)=Sof(H17B)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C79)=Sof(H79A)=Sof(H79B)=FVAR(1)
 Sof(Cl13)=Sof(Cl14)=Sof(C180)=Sof(H18A)=Sof(H18B)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl4)=Sof(C80)=Sof(H80A)=Sof(H80B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C179(H17A,H17B), C80(H80A,H80B), C180(H18A,H18B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C29(H29),
  C30(H30), C31(H31), C32(H32), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49),
  C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C60(H60), C61(H61),
 C62(H62), C68(H68), C69(H69), C70(H70), C71(H71), C75(H75), C76(H76), C77(H77),
  C78(H78)
;
_shelx_res_checksum              63199
_olex2_submission_special_instructions 'No special instructions were received'