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_7715107
_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         'C54 H52 Ir N10, 3(F6 P), 1.25[CH3OH]'
_chemical_formula_sum            'C55.25 H57 F18 Ir N10 O1.25 P3'
_chemical_formula_weight         1508.22
_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             2023-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-06 deposited with the CCDC.	2024-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                105.1570(10)
_cell_angle_beta                 108.1430(10)
_cell_angle_gamma                94.9750(10)
_cell_formula_units_Z            4
_cell_length_a                   16.5187(2)
_cell_length_b                   18.7439(3)
_cell_length_c                   22.3271(3)
_cell_measurement_reflns_used    52267
_cell_measurement_temperature    100.1(5)
_cell_measurement_theta_max      30.6870
_cell_measurement_theta_min      2.1990
_cell_volume                     6233.35(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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      100.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -86.00  -4.00   0.50   40.00    --  -10.52 -33.00  -3.00  164
  2  \w    -62.00  13.00   0.50   40.00    --   13.95 -33.00  -3.00  150
  3  \w      8.00  90.00   0.50   40.00    --   13.95  33.00 154.00  164
  4  \w    -56.00   1.00   0.50   40.00    --  -10.52 -57.00-120.00  114
  5  \w     21.00  68.00   0.50   40.00    --  -10.52  19.00 120.00   94
  6  \w    -64.00 -17.00   0.50   40.00    --   13.95 -19.00-120.00   94
  7  \w      3.00  62.00   0.50   40.00    --   13.95  57.00 150.00  118
  8  \w    -18.00  34.00   0.50   40.00    --   13.95 -77.00 -30.00  104
  9  \w    -18.00  34.00   0.50   40.00    --   13.95 -77.00-150.00  104
 10  \w      3.00  62.00   0.50   40.00    --   13.95  57.00-120.00  118
 11  \w      3.00  62.00   0.50   40.00    --   13.95  57.00  60.00  118
 12  \w      3.00  62.00   0.50   40.00    --   13.95  57.00   0.00  118
 13  \w    -18.00  34.00   0.50   40.00    --   13.95 -77.00  30.00  104
 14  \w     21.00  48.00   0.50   40.00    --   13.95  57.00 -30.00   54
 15  \w      4.00  62.00   0.50   40.00    --   13.95  57.00-150.00  116
 16  \w     25.00  50.00   0.50   40.00    --   13.95  33.00 154.00   50
 17  \w    -30.00   7.00   0.50   40.00    --  -10.52  77.00-150.00   74
 18  \w    -64.00 -17.00   0.50   40.00    --   13.95 -19.00  60.00   94
 19  \w    -18.00  34.00   0.50   40.00    --   13.95 -77.00 120.00  104
;
_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      0.0305989000
_diffrn_orient_matrix_UB_12      -0.0235515000
_diffrn_orient_matrix_UB_13      -0.0037521000
_diffrn_orient_matrix_UB_21      0.0177574000
_diffrn_orient_matrix_UB_22      0.0239182000
_diffrn_orient_matrix_UB_23      -0.0144592000
_diffrn_orient_matrix_UB_31      0.0293449000
_diffrn_orient_matrix_UB_32      0.0215354000
_diffrn_orient_matrix_UB_33      0.0317625000
_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  0.0801
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            170187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       plate
_exptl_crystal_F_000             3010
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.025
_refine_diff_density_max         3.767
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1628
_refine_ls_number_reflns         32144
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0503P)^2^+28.9405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22860
_reflns_number_total             32144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03690a2.cif
_cod_data_source_block           2022ncs0454s
_cod_depositor_comments
'Adding full bibliography for 7715107--7715109.cif.'
_cod_database_code               7715107
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C54 H52 F18 Ir N10 P3'
_chemical_oxdiff_usercomment     RK-130
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.768
_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
C03R \\sim C04K: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C03R) \\sim Ueq, Uanis(C04K) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Fixed Sof: P9(0.5) P8(0.5) F55(0.5) F53(0.5) F49(0.5) F51(0.5) F56(0.5)
 F54(0.5) F48(0.5) F57(0.5) F50(0.5) F52(0.5) F10(0.5) F13(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C02U(H02C,H02F), C02X(H02A,H02B), C03P(H03G,H03I), C04A(H04S,H04T)
4.b Aromatic/amide H refined with riding coordinates:
 C01N(H01N), C01P(H01P), C01T(H01T), C01V(H01V), C022(H022), C024(H024),
 C027(H027), C028(H028), C02D(H02D), C02E(H02E), C02J(H02J), C02K(H02K),
 C02M(H02M), C02N(H02N), C02O(H02O), C02R(H02R), C02S(H02S), C02Y(H02Y),
 C02Z(H02Z), C030(H030), C031(H031), C036(H036), C039(H039), C03A(H03Z),
 C03B(H03), C03C(H03C), C03E(H03E), C03F(H03F), C03H(H03H), C03I(H1),
 C03K(H03K), C03L(H03L), C03N(H2), C03Q(H03Q), C03T(H03T), C03U(H3), C03Z(H5),
 C040(H040), C041(H041), C045(H045), C048(H048), C049(H049), C04B(H04J),
 C04C(H04K), C04D(H04U), C04F(H04L), C04G(H04Y), C04I(H04Z)
4.c Idealised Me refined as rotating group:
 C035(H03S,H03U,H03V), C037(H03W,H03X,H03Y), C03M(H03A,H03B,H03D), C03S(H03J,
 H03M,H03N), C03V(H4,H,HA), C03X(H03O,H03P,H03R), C042(H04A,H04B,H04C),
 C043(H04D,H04E,H04F), C046(H04G,H04H,H04I), C04E(H04V,H04W,H04X), C04J(H04,HB,
 HC), C04K(H6,HD,HE), C04L(H7,HF,HG), C04M(H04M,H04N,H04O), C04N(H8,HH,HI),
 C04P(H04P,H04Q,H04R)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 107 electrons were 
found in a volume of 751\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
1.25[CH3OH] per Unit Cell 
which account for 90 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68728
_shelx_fab_checksum              807
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.704
_oxdiff_exptl_absorpt_empirical_full_min 0.436