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_7714409
_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 H25 N2 O2 Rh'
_chemical_formula_sum            'C32 H25 N2 O2 Rh'
_chemical_formula_weight         572.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 100.002(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0427(11)
_cell_length_b                   23.901(2)
_cell_length_c                   12.1579(12)
_cell_measurement_reflns_used    3330
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      22.49
_cell_measurement_theta_min      2.41
_cell_volume                     2873.9(5)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_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 0.999
_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  0.1188
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29915
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.408
_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
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1033 before and 0.0736 after correction. The Ratio of minimum to maximum transmission is 0.8848. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, Hexane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0608P)^2^+5.4298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3413
_reflns_number_total             5057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02651e2.cif
_cod_data_source_block           mo_mk3_b_0m
_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_original_cell_volume        2874.0(5)
_cod_database_code               7714409
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.923
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C27) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29) =
Uanis(C33) = Uanis(C36) = Uanis(C34) = Uanis(C35)
3. Others
 Fixed Sof: H28(0.4) H28A(0.6) C32(0.4) H32(0.4) C31(0.4) H31(0.4) C30(0.4)
 H30(0.4) C29(0.4) H29(0.4) C33(0.6) H33(0.6) C36(0.6) H36(0.6) C34(0.6)
 H34(0.6) C35(0.6) H35(0.6)
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C5(H5), C2(H2), C3(H3), C22(H22), C13(H13), C4(H4), C11(H11),
 C8(H8), C9(H9), C21(H21), C10(H10), C16(H16), C20(H20), C28(H28), C28(H28A),
 C32(H32), C31(H31), C30(H30), C29(H29), C14(H14), C25(H25), C15(H15), C33(H33),
  C36(H36), C34(H34), C35(H35)
4.b Fitted hexagon refined as free rotating group:
 C28(C27,C32,C31,C30,C29)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              67904
_shelx_fab_checksum              99757
_olex2_submission_special_instructions 'No special instructions were received'