Aggregation-induced emission of cyclometalated rhodium(III) and iridium(III) phenylpyridine complexes with ancillary 1,3-diketones
Kiseleva, Marina A.; Andrei, Churakov; Taydakov, Ilya V.; Metlin, Mikhail T.; Kozyukhin, Sergey; Bezzubov, Stanislav; Dalton Transactions  (2023) –; doi:10.1039/D3DT02651E

data_7714404
_publ_section_title
;
 Aggregation-induced emission of cyclometalated rhodium(III) and
 iridium(III) phenylpyridine complexes with ancillary 1,3-diketones
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02651E
_journal_year                    2023
_chemical_formula_moiety         'C32 H22 F3 Ir N2 O2'
_chemical_formula_sum            'C32 H22 F3 Ir N2 O2'
_chemical_formula_weight         715.71
_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     iterative
_audit_creation_date             2023-06-02
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-06-02 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                71.158(2)
_cell_angle_beta                 75.027(2)
_cell_angle_gamma                67.214(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4446(6)
_cell_length_b                   11.7077(6)
_cell_length_c                   13.0847(7)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.25
_cell_volume                     1511.82(14)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 'Bruker PHOTON III CMOS'
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17126
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.949
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.464
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0961 before and 0.0502 after correction.
The Ratio of minimum to maximum transmission is 0.6704.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.893
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5881
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0455P)^2^+2.0008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5347
_reflns_number_total             5881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02651e2.cif
_cod_data_source_block           ad4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7714404
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.616
_shelx_estimated_absorpt_t_min   0.427
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Ir1-C18 \\sim Ir1-C12
 with sigma of 0.01
 Ir1-N2 \\sim Ir1-N3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C23) = Uanis(C21) = Uanis(C22) =
Uanis(C17) = Uanis(C16) = Uanis(C15) = Uanis(C14) = Uanis(C13) = Uanis(C12)
Uanis(N3) = Uanis(C24) = Uanis(C33) = Uanis(C25) = Uanis(C32) = Uanis(C26) =
Uanis(N2) = Uanis(C28) = Uanis(C27) = Uanis(C31) = Uanis(C30) = Uanis(C29)
4. Others
 Fixed Sof: N3(0.5) C24(0.5) C23(0.5) C18(0.5) C19(0.5) H19(0.5) C20(0.5)
 H20(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5) C33(0.5) H33(0.5) C25(0.5)
 H25(0.5) C32(0.5) H32(0.5) C26(0.5) H26(0.5) N2(0.5) C28(0.5) H28(0.5)
 C27(0.5) H27(0.5) C31(0.5) H31(0.5) C30(0.5) H30(0.5) C29(0.5) C17(0.5)
 C12(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16(0.5)
 Fixed X: N3(0.285709) N2(0.3141)
 Fixed Y: N3(0.234819) N2(0.20825)
 Fixed Z: N3(0.137549) N2(0.13343)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C36(H36), C5(H5), C11(H11), C10(H10), C41(H41), C39(H39), C42(H42),
 C8(H8), C43(H43), C4(H4), C2(H2), C40(H40), C3(H3), C19(H19), C20(H20),
 C21(H21), C22(H22), C33(H33), C25(H25), C32(H32), C26(H26), C28(H28), C27(H27),
  C31(H31), C30(H30), C13(H13), C14(H14), C15(H15), C16(H16)
5.b Fitted hexagon refined as free rotating group:
 C23(C18,C19,C20,C21,C22), C17(C12,C13,C14,C15,C16)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75241
_shelx_fab_checksum              51721
_olex2_submission_special_instructions 'No special instructions were received'