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_7714407
_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 N2 O2 Rh'
_chemical_formula_sum            'C32 H22 F3 N2 O2 Rh'
_chemical_formula_weight         626.42
_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             2021-06-29
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-06-29 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                70.7650(10)
_cell_angle_beta                 72.2520(10)
_cell_angle_gamma                67.1520(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4135(4)
_cell_length_b                   11.8344(4)
_cell_length_c                   13.4479(5)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.24
_cell_volume                     1547.45(10)
_computing_cell_refinement       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker AXS, 2016)'
_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      150.0
_diffrn_detector                 'Bruker PHOTON III CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38065
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.552
_diffrn_reflns_theta_min         1.924
_diffrn_source                   'microfocus sealed X-ray tube'
_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    0.598
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0652 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.9081.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, hexane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.618
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0577P)^2^+2.1870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8052
_reflns_number_total             9430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02651e2.cif
_cod_data_source_block           mk42
_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               7714407
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.900
_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, All C(H,H) groups
2. Restrained distances
 F1-F3
 2.2 with sigma of 0.02
 F2-F3
 2.2 with sigma of 0.02
 F4-F6
 2.2 with sigma of 0.02
 F4-C23 \\sim F1-C23 \\sim F5-C23 \\sim F2-C23 \\sim F3-C23 \\sim F6-C23
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C27) = Uanis(C32) = Uanis(C36) = Uanis(C31) = Uanis(C35) = Uanis(C30) =
Uanis(C34) = Uanis(C29) = Uanis(C33) = Uanis(C28)
Uanis(F1) = Uanis(F4) = Uanis(F3) = Uanis(F6) = Uanis(F2) = Uanis(F5)
4. Others
 Fixed Sof: F6(0.5) F4(0.5) F5(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36(0.5) H32(0.5) H32A(0.5) C31(0.5) H31(0.5)
 C30(0.5) H30(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) F3(0.5) F2(0.5) F1(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C8(H8), C9(H9), C5(H5), C10(H10), C13(H13), C11(H11), C33(H33),
 C34(H34), C35(H35), C36(H36), C32(H32), C32(H32A), C2(H2), C4(H4), C31(H31),
 C14(H14), C16(H16), C30(H30), C22(H22), C19(H19), C3(H3), C15(H15), C20(H20),
 C28(H28), C21(H21), C29(H29)
5.b Fitted hexagon refined as free rotating group:
 C27(C33,C34,C35,C36,C32)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49924
_shelx_fab_checksum              39164
_olex2_submission_special_instructions 'No special instructions were received'