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_7707491
_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                85.981(2)
_cell_angle_beta                 76.654(2)
_cell_angle_gamma                72.389(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4642(3)
_cell_length_b                   10.5088(2)
_cell_length_c                   15.5137(4)
_cell_measurement_reflns_used    23037
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.28
_cell_measurement_theta_min      2.03
_cell_volume                     1582.11(7)
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27014
_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         27.999
_diffrn_reflns_theta_min         2.033
_exptl_absorpt_coefficient_mu    4.432
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.767
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.759
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.8126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6931
_reflns_number_total             7631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00783a2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7707490--7707494.cif.'
_cod_original_cell_volume        1582.12(7)
_cod_database_code               7707491
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.843
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C40 \\sim Cl11 \\sim Cl12 \\sim C140: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(Cl11)
\\sim Ueq, Uanis(Cl12) \\sim Ueq, Uanis(C140) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Cl1, Cl2, C40, Cl11, Cl12, C140
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Cl1, Cl2, C40} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl11, Cl12, C140}
5. Others
 Sof(Cl11)=Sof(Cl12)=Sof(C140)=Sof(H14A)=Sof(H14B)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C140(H14A,H14B)
6.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)
;
_shelx_res_checksum              35868
_olex2_submission_special_instructions 'No special instructions were received'