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_7715109
_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         'C53 H45 Au N8 P Ru, 3(F6 P)'
_chemical_formula_sum            'C53 H45 Au F18 N8 P4 Ru'
_chemical_formula_weight         1557.88
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-18 deposited with the CCDC.	2024-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.515(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5010(3)
_cell_length_b                   21.5970(4)
_cell_length_c                   20.6880(5)
_cell_measurement_reflns_used    25124
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2620
_cell_measurement_theta_min      3.4090
_cell_volume                     5965.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5082
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.876
_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     71.00  97.00   1.00   41.86    --   10.51 178.00-150.00   26
  2  \w    -44.00  11.00   1.00   41.86    --  -11.44  77.00   0.00   55
  3  \w      0.00  29.00   1.00   41.86    --  -11.44  38.00 -30.00   29
  4  \w    -84.00 -17.00   1.00   41.86    --  -11.44 -38.00  90.00   67
  5  \w    -54.00  54.00   1.00   41.86    --  -11.44   0.00-180.00  108
  6  \w    -36.00  63.00   1.00   41.86    --  -11.44  38.00-120.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0341361000
_diffrn_orient_matrix_UB_12      -0.0156752000
_diffrn_orient_matrix_UB_13      0.0172746000
_diffrn_orient_matrix_UB_21      -0.0356781000
_diffrn_orient_matrix_UB_22      0.0238765000
_diffrn_orient_matrix_UB_23      -0.0082949000
_diffrn_orient_matrix_UB_31      -0.0195919000
_diffrn_orient_matrix_UB_32      -0.0162029000
_diffrn_orient_matrix_UB_33      -0.0288936000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62240
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.915
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.917
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_recrystallization_method MeCn/MeOH
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         15106
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+3.3783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10255
_reflns_number_total             15106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03690a2.cif
_cod_data_source_block           sjp2310
_cod_depositor_comments
'Adding full bibliography for 7715107--7715109.cif.'
_cod_database_code               7715109
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'c53 h46 n8 P4 F18  Au Ru '
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.347
_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. Restrained distances
 P004-F3 \\sim P004-F3A
 with sigma of 0.02
 P004-F5 \\sim P004-F5A
 with sigma of 0.02
 P004-F6 \\sim P004-F6A
 with sigma of 0.02
 P004-F9 \\sim P004-F9A
 with sigma of 0.02
 P005-F012 \\sim P005-F2
 with sigma of 0.02
 P005-F019 \\sim P005-F1
 with sigma of 0.02
 P005-F025 \\sim P005-F4
 with sigma of 0.02
 P005-F026 \\sim P005-F0
 with sigma of 0.02
 P006-F016 \\sim P006-F8
 with sigma of 0.02
 P006-F01R \\sim P006-F01S
 with sigma of 0.02
 P006-F028 \\sim P006-F7
 with sigma of 0.02
 P006-F02B \\sim P006-F02C
 with sigma of 0.02
 C65-C66 \\sim C64-C63
 with sigma of 0.02
 C60-C61 \\sim C69-C68
 with sigma of 0.02
 C61-C62 \\sim C68-C67
 with sigma of 0.02
 C66-C62 \\sim C63-C67
 with sigma of 0.02
 P46-C65 \\sim P46-C64
 with sigma of 0.04
 P46-C60 \\sim P46-C69
 with sigma of 0.04
 C65-C60 \\sim C64-C69
 with sigma of 0.04
 C65-C62 \\sim C64-C67
 with sigma of 0.04
 C60-C62 \\sim C69-C67
 with sigma of 0.04
 C61-C66 \\sim C68-C63
 with sigma of 0.04
3. Rigid bond restraints
 F6, P004, F9, F5, F00E, F00F, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F6 \\sim P004 \\sim F9 \\sim F5 \\sim F00E \\sim F00F \\sim F3: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F6) \\sim Ueq, Uanis(P004) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F5)
\\sim Ueq, Uanis(F00E) \\sim Ueq, Uanis(F00F) \\sim Ueq, Uanis(F3) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C65) = Uanis(C60) = Uanis(C61) = Uanis(C66) = Uanis(C62) = Uanis(C68) =
Uanis(C67) = Uanis(C63) = Uanis(C64) = Uanis(C69) = Uanis(C59)
5. Rigid body (RIGU) restrains
 F6, P004, F9, F5, F00E, F00F, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F9A)=Sof(F3A)=Sof(F6A)=Sof(F5A)=1-FVAR(1)
 Sof(F3)=Sof(F5)=Sof(F6)=Sof(F9)=FVAR(1)
 Sof(F0)=Sof(F1)=Sof(F2)=Sof(F4)=1-FVAR(2)
 Sof(F012)=Sof(F019)=Sof(F025)=Sof(F026)=FVAR(2)
 Sof(F02C)=Sof(F7)=Sof(F01S)=Sof(F8)=1-FVAR(3)
 Sof(F016)=Sof(F01R)=Sof(F028)=Sof(F02B)=FVAR(3)
 Sof(C68)=Sof(H68)=Sof(C67)=Sof(H67)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=
 Sof(C69)=Sof(H69)=1-FVAR(4)
 Sof(C65)=Sof(H65)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C66)=Sof(H66)=
 Sof(C62)=Sof(H62)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B)
7.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C27(H27), C40(H40), C3(H3), C24(H24), C5(H5), C41(H41), C9(H9),
 C54(H54), C49(H49), C52(H52), C21(H21), C23(H23), C12(H12), C4(H4), C50(H50),
 C55(H55), C11(H11), C10(H10), C28(H28), C48(H48), C6(H6), C30(H30), C15(H15),
 C22(H22), C34(H34), C58(H58), C33(H33), C17(H17), C16(H16), C56(H56), C18(H18),
  C51(H51), C29(H29), C57(H57), C65(H65), C60(H60), C61(H61), C66(H66),
 C62(H62), C68(H68), C67(H67), C63(H63), C69(H69)
7.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C)
;
_shelx_res_checksum              14315
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.851
_oxdiff_exptl_absorpt_empirical_full_min 0.667