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_7714406
_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         'C37 H27 N2 O2 Rh, C0.5 H Cl'
_chemical_formula_sum            'C37.5 H28 Cl N2 O2 Rh'
_chemical_formula_weight         676.98
_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
_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                92.2610(10)
_cell_angle_beta                 93.1600(10)
_cell_angle_gamma                104.3880(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5699(2)
_cell_length_b                   11.7403(2)
_cell_length_c                   12.2502(2)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.32
_cell_volume                     1468.03(4)
_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
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18790
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.516
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0412 before and 0.0311 after correction. The Ratio of minimum to maximum transmission is 0.9061. 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    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             690
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, hexane'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.576
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8818
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+1.7410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8143
_reflns_number_total             8818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02651e2.cif
_cod_data_source_block           mk2b
_cod_original_formula_sum        'C37.50 H28 Cl N2 O2 Rh'
_cod_database_code               7714406
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.804
_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
 Cl1_$1-C38_$1 \\sim Cl1-C38_$1
 with sigma of 0.003
3. Others
 Fixed Sof: C38(0.5) H38A(0.5) H38B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C2(H2), C37(H37), C13(H13), C30(H30), C24(H24), C14(H14), C33(H33),
 C27(H27), C36(H36), C11(H11), C3(H3), C10(H10), C22(H22), C19(H19), C8(H8),
 C34(H34), C15(H15), C4(H4), C35(H35), C16(H16), C25(H25), C5(H5), C9(H9),
 C20(H20), C26(H26), C21(H21)
;
_shelx_res_checksum              5743
_olex2_submission_special_instructions 'No special instructions were received'