Synthesis and luminescent properties of hetero-bimetallic and hetero-trimetallic Ru(II)/Au(I) or Ir(III)/Au(I) complexes.
Knighton, Richard C.; Pope, Simon J. A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4165–4174; doi:10.1039/d3dt03690a

data_7715108
_publ_section_title
;
 Synthesis and luminescent properties of hetero-bimetallic and
 hetero-trimetallic Ru(II)/Au(I) or Ir(III)/Au(I) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4165
_journal_page_last               4174
_journal_paper_doi               10.1039/d3dt03690a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C38 H36 Ir N6, B F4'
_chemical_formula_sum            'C38 H36 B F4 Ir N6'
_chemical_formula_weight         855.74
_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             2023-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-21 deposited with the CCDC.	2024-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                77.983(6)
_cell_angle_beta                 78.821(5)
_cell_angle_gamma                85.964(5)
_cell_formula_units_Z            2
_cell_length_a                   8.6524(4)
_cell_length_b                   12.6306(8)
_cell_length_c                   16.5547(10)
_cell_measurement_reflns_used    7955
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.4420
_cell_measurement_theta_min      2.6810
_cell_volume                     1735.11(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -94.00 -19.00   0.50    2.50    --  -47.32 128.00 100.00  150
  2  \w   -118.00 -65.00   0.50    2.50    --  -47.32-141.00-145.00  106
  3  \w   -102.00 -25.00   0.50    2.50    --  -47.32 141.00 -87.00  154
  4  \w     71.00 118.00   0.50    2.50    --   47.32 141.00 -87.00   94
  5  \w     25.00  94.00   0.50    2.50    --   47.32-128.00  25.00  138
  6  \w     31.00 102.00   0.50    2.50    --   47.32-141.00-145.00  142
  7  \w     31.00 124.00   0.50   12.00    --  100.00-141.00-145.00  186
  8  \w     80.00 172.00   0.50   12.00    --  100.00 128.00 100.00  184
  9  \w     28.00 114.00   0.50   12.00    --  100.00-128.00  25.00  172
 10  \w   -124.00 -30.00   0.50   12.00    -- -102.00 141.00 -87.00  188
 11  \w   -174.00 -74.00   0.50   12.00    -- -102.00-128.00  25.00  200
 12  \w   -114.00 -30.00   0.50   12.00    -- -102.00 128.00 100.00  168
 13  \w   -172.00 -65.00   0.50   12.00    -- -102.00-141.00-145.00  214
 14  \w    -24.00  26.00   0.50    2.50    --  -47.32  19.00 -90.00  100
 15  \w    -24.00  26.00   0.50    2.50    --  -47.32  19.00 -30.00  100
 16  \w   -118.00 -27.00   0.50    2.50    --  -47.32 -77.00  60.00  182
 17  \w    -24.00  26.00   0.50    2.50    --  -47.32  19.00   0.00  100
 18  \w   -118.00 -27.00   0.50    2.50    --  -47.32 -77.00-150.00  182
 19  \w     28.00 112.00   0.50   12.00    --  100.00-125.00   0.00  168
 20  \w     28.00 106.00   0.50   12.00    --  100.00 -94.00  90.00  156
 21  \w     28.00 112.00   0.50   12.00    --  100.00-125.00  60.00  168
 22  \w     71.00 172.00   0.50   12.00    --  100.00 141.00 -87.00  202
 23  \w     92.00 172.00   0.50   12.00    --  100.00  30.00  30.00  160
 24  \w     28.00 106.00   0.50   12.00    --  100.00 -94.00  60.00  156
 25  \w     28.00  73.00   0.50   12.00    --  100.00 -61.00 -90.00   90
 26  \w     92.00 172.00   0.50   12.00    --  100.00  30.00   0.00  160
 27  \w     80.00 106.00   0.50   12.00    --  100.00-103.00 -97.06   52
 28  \w     31.00 107.00   0.50   12.00    --  100.00 -77.00  60.00  152
 29  \w     30.00  66.00   0.50   12.00    --  100.00 -61.00   0.00   72
 30  \w     42.00  97.00   0.50   12.00    --  100.00 -94.00-150.00  110
 31  \w     30.00  85.00   0.50   12.00    --  100.00 -77.00-180.00  110
 32  \w     92.00 172.00   0.50   12.00    --  100.00  45.00 -90.00  160
 33  \w     58.00 106.00   0.50   12.00    --  100.00 -77.00-150.00   96
 34  \w     44.00  72.00   0.50   12.00    --  100.00 -61.00-120.00   56
 35  \w    -70.00 -43.00   0.50   12.00    -- -102.00  77.00-150.00   54
 36  \w    -61.00 -31.00   0.50   12.00    -- -102.00  61.00 150.00   60
 37  \w   -173.00-105.00   0.50   12.00    -- -102.00 -15.00-180.00  136
 38  \w    -68.00 -32.00   0.50   12.00    -- -102.00  61.00-120.00   72
 39  \w    -62.00 -30.00   0.50   12.00    -- -102.00  61.00 -30.00   64
 40  \w    -69.00 -44.00   0.50   12.00    -- -102.00  61.00 -90.00   50
 41  \w   -173.00 -93.00   0.50   12.00    -- -102.00 -45.00  90.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0039916000
_diffrn_orient_matrix_UB_12      0.1204162000
_diffrn_orient_matrix_UB_13      -0.0433974000
_diffrn_orient_matrix_UB_21      0.0262082000
_diffrn_orient_matrix_UB_22      -0.0325983000
_diffrn_orient_matrix_UB_23      -0.0864044000
_diffrn_orient_matrix_UB_31      -0.1796365000
_diffrn_orient_matrix_UB_32      0.0018663000
_diffrn_orient_matrix_UB_33      0.0044017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1101
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27371
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.055
_diffrn_reflns_theta_min         2.776
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.073
_refine_diff_density_min         -3.474
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1124P)^2^+4.9805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.2048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4473
_reflns_number_total             6455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03690a2.cif
_cod_data_source_block           2022ncs0201s
_cod_depositor_comments
'Adding full bibliography for 7715107--7715109.cif.'
_cod_database_code               7715108
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H36 F6 Ir N6 P'
_chemical_oxdiff_usercomment     RK-70
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.569
_reflns_odcompleteness_completeness 97.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00J(H00J), C00L(H00L), C00P(H00P), C00Q(H00Q),
 C00T(H00T), C00V(H00V), C00W(H00W), C012(H012), C016(H016), C018(H018)
2.b Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C), C014(H01D,H01E,H01F), C015(H01G,H01H,H01I), C017(H01J,
 H01K,H01L), C01A(H01M,H01N,H01O), C01B(H01P,H01Q,H01R), C01C(H01S,H01T,H01U),
 C01D(H01V,H01W,H01X)
;
_shelx_res_checksum              19761
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.974
_oxdiff_exptl_absorpt_empirical_full_min 0.330