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_7714410
_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         'C44 H32 Cl2 N4 Rh2'
_chemical_formula_sum            'C44 H32 Cl2 N4 Rh2'
_chemical_formula_weight         893.45
_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     dual
_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                90
_cell_angle_beta                 95.936(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4265(12)
_cell_length_b                   13.9065(11)
_cell_length_c                   24.1630(18)
_cell_measurement_reflns_used    7857
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.22
_cell_volume                     4487.4(6)
_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    '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 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  0.0409
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44352
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.666
_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    0.886
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0668 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.8678.
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    1.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.175
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         9749
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0597P)^2^+21.8909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7246
_reflns_number_total             9749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02651e2.cif
_cod_data_source_block           mk3
_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               7714410
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.829
_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
 Rh2-N6 \\sim Rh2-N5
 with sigma of 0.02
 Rh2-C51 \\sim Rh2-C45
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(C17) = Uanis(C12) = Uanis(C24) = Uanis(C16) = Uanis(C28) =
Uanis(C15) = Uanis(C13) = Uanis(C25) = Uanis(C14) = Uanis(C27) = Uanis(C26) =
Uanis(N3) = Uanis(C33) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29) =
Uanis(C23) = Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C19) = Uanis(C18)
Uanis(N6) = Uanis(C45) = Uanis(C62) = Uanis(C56) = Uanis(C63) = Uanis(C61) =
Uanis(C46) = Uanis(C47) = Uanis(C65) = Uanis(C55) = Uanis(C59) = Uanis(C54) =
Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C48) = Uanis(C49) = Uanis(C50) =
Uanis(C57) = Uanis(C58) = Uanis(C64) = Uanis(C60) = Uanis(C66) = Uanis(N5)
4. Others
 Fixed Sof: N6(0.5) N2(0.5) C17(0.5) C45(0.5) C12(0.5) C24(0.5) C62(0.5)
 C16(0.5) H16(0.5) C28(0.5) H28(0.5) C56(0.5) C63(0.5) H63(0.5) C15(0.5)
 H15(0.5) C61(0.5) H61(0.5) C46(0.5) H46(0.5) C13(0.5) H13(0.5) C47(0.5)
 H47(0.5) C25(0.5) H25(0.5) C14(0.5) H14(0.5) C65(0.5) H65(0.5) C27(0.5)
 H27(0.5) C55(0.5) H55(0.5) C26(0.5) H26(0.5) C59(0.5) H59(0.5) C54(0.5)
 H54(0.5) N3(0.5) C33(0.5) H33(0.5) C32(0.5) H32(0.5) C31(0.5) H31(0.5)
 C30(0.5) H30(0.5) C29(0.5) C23(0.5) C22(0.5) H22(0.5) C21(0.5) H21(0.5)
 C20(0.5) H20(0.5) C19(0.5) H19(0.5) C18(0.5) C51(0.5) C52(0.5) H52(0.5)
 C53(0.5) H53(0.5) C48(0.5) H48(0.5) C49(0.5) H49(0.5) C50(0.5) C57(0.5)
 C58(0.5) H58(0.5) C64(0.5) H64(0.5) C60(0.5) H60(0.5) C66(0.5) H66(0.5) N5(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C35(H35), C11(H11), C5(H5), C2(H2), C16(H16),
 C36(H36), C44(H44), C28(H28), C63(H63), C15(H15), C37(H37), C10(H10), C43(H43),
  C61(H61), C46(H46), C41(H41), C42(H42), C9(H9), C38(H38), C13(H13), C47(H47),
 C25(H25), C14(H14), C65(H65), C27(H27), C55(H55), C26(H26), C59(H59), C54(H54),
  C33(H33), C32(H32), C31(H31), C30(H30), C22(H22), C21(H21), C20(H20),
 C19(H19), C52(H52), C53(H53), C48(H48), C49(H49), C58(H58), C64(H64), C60(H60),
  C66(H66)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53251
_shelx_fab_checksum              64678
_olex2_submission_special_instructions 'No special instructions were received'