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_7714408
_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         'C30 H20 F3 Ir N2 O2 S'
_chemical_formula_sum            'C30 H20 F3 Ir N2 O2 S'
_chemical_formula_weight         721.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-28
_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                90
_cell_angle_beta                 113.797(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3589(12)
_cell_length_b                   20.2331(16)
_cell_length_c                   17.6076(15)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.35
_cell_volume                     5006.5(7)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON III CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0885
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            71238
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.353
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.473
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0807 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.8089. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.915
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, hexane'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         10933
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0176P)^2^+17.2872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8060
_reflns_number_total             10933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02651e2.cif
_cod_data_source_block           ad5
_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               7714408
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.584
_shelx_estimated_absorpt_t_min   0.379
_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
 C34-C33
 1.34 with sigma of 0.01
 C026-C025
 1.34 with sigma of 0.01
 C31-C005
 1.36 with sigma of 0.02
 C32-C0
 1.36 with sigma of 0.02
 C025-C005
 1.4 with sigma of 0.02
 C33-C32
 1.4 with sigma of 0.02
 C30-C28 = C32-C34
 2.28 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C32) = Uanis(C0) = Uanis(C33) = Uanis(C34) = Uanis(S0)
Uanis(C31) = Uanis(S004) = Uanis(C026) = Uanis(C025) = Uanis(C005)
Uanis(S004) = Uanis(C31) = Uanis(C005) = Uanis(C025) = Uanis(C026)
Uanis(S004) = Uanis(C026) = Uanis(C025) = Uanis(C005) = Uanis(C31)
4. Others
 Fixed Sof: S004(0.6) C005(0.6) H005(0.6) C31(0.6) C025(0.6) H025(0.6)
 C026(0.6) H026(0.6) C0(0.4) C32(0.4) H32(0.4) C33(0.4) H33(0.4) C34(0.4)
 H34(0.4) S0(0.4)
 Fixed X: C0(0.76246)
 Fixed Y: C0(0.601241)
 Fixed Z: C0(0.521091)
5.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C00M(H00M), C00R(H00R), C21(H21), C10(H10), C22(H22), C00Y(H00Y),
 C00Z(H00Z), C011(H011), C013(H013), C2(H2), C11(H11), C018(H018), C13(H13),
 C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C20(H20), C9(H9), C8(H8),
 C01H(H01H), C01I(H01I), C14(H14), C01M(H01M), C01Q(H01Q), C28(H28), C16(H16),
 C19(H19), C3(H3), C4(H4), C25(H25), C01X(H01X), C15(H15), C30(H30), C5(H5),
 C022(H022), C29(H29), C025(H025), C026(H026), C32(H32), C33(H33), C34(H34)
;
_shelx_res_checksum              19396
_olex2_submission_special_instructions 'No special instructions were received'