Photoluminescent properties and molecular structures of dinuclear gold(I) complexes with bridged diphosphine ligands: near-unity phosphorescence from <sup>3</sup>XMMCT/<sup>3</sup>MC.
Osawa, Masahisa; Soma, Sakie; Hoshino, Mikio; Tanaka, Yuya; Akita, Munetaka; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15204–15212; doi:10.1039/d0dt03144e

data_7705612
_publ_section_title
;
 Photoluminescent properties and molecular structures of dinuclear gold(I)
 complexes with bridged diphosphine ligands: near-unity phosphorescence
 from <sup>3</sup>XMMCT/<sup>3</sup>MC.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15204
_journal_page_last               15212
_journal_paper_doi               10.1039/d0dt03144e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C42 H48 Au2 I2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H64 Au2 I2 O2 P2'
_chemical_formula_weight         1406.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-29
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-02 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.06858(18)
_cell_length_b                   17.0216(2)
_cell_length_c                   20.3878(2)
_cell_measurement_reflns_used    94419
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      31.1840
_cell_measurement_theta_min      3.2670
_cell_volume                     4882.26(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.920
_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    -33.00   8.00   0.50    0.22    --   -6.28 -55.00  82.00   82
  2  \w     -8.00  31.00   0.50    0.22    --    4.09  37.00 -90.00   78
  3  \w     43.00  69.00   0.50    0.22    --    4.09  37.00 -90.00   52
  4  \w    -17.00  38.00   0.50    0.22    --    4.09 -99.00  60.00  110
  5  \w     -8.00  75.00   0.50    0.22    --    4.09  37.00 120.00  166
  6  \w     -7.00  75.00   0.50    0.22    --    4.09  37.00   0.00  164
  7  \w    -20.00  60.00   0.50    0.22    --   -6.28  28.00 -93.82  160
  8  \w     15.00  61.00   0.50    0.22    --   -6.28  29.00 128.20   92
  9  \w    -20.00  67.00   0.50    0.22    --   -6.28  33.00-171.40  174
 10  \w    -20.00   8.00   0.50    0.22    --   -6.28  33.00  79.26   56
 11  \w     12.00  51.00   0.50    0.22    --   -6.28  33.00  79.26   78
 12  \w    -19.00   7.00   0.50    0.22    --   -6.28  29.00 128.20   52
 13  \w     41.00  67.00   0.50    0.22    --   -6.28  33.00  40.86   52
 14  \w    -16.00  27.00   0.50    0.22    --   -6.28 -99.00 120.00   86
 15  \w    -20.00  50.00   0.50    0.22    --   -6.28  33.00 -27.25  140
 16  \w    -20.00  25.00   0.50    0.22    --   -6.28  33.00  40.86   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0279555000
_diffrn_orient_matrix_UB_12      0.0244513000
_diffrn_orient_matrix_UB_13      0.0205268000
_diffrn_orient_matrix_UB_21      -0.0415065000
_diffrn_orient_matrix_UB_22      -0.0204608000
_diffrn_orient_matrix_UB_23      -0.0098912000
_diffrn_orient_matrix_UB_31      0.0061765000
_diffrn_orient_matrix_UB_32      -0.0268258000
_diffrn_orient_matrix_UB_33      0.0262894000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            142781
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.142
_diffrn_reflns_theta_min         3.228
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.370
_exptl_absorpt_correction_T_max  0.11000
_exptl_absorpt_correction_T_min  0.06600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.618
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 5535 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0107(12)
_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     531
_refine_ls_number_reflns         15766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0094P)^2^+2.6515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0302
_refine_ls_wR_factor_ref         0.0306
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                13220
_reflns_number_total             15766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03144e2.cif
_cod_data_source_block           191029_osawa_o
_cod_depositor_comments
'Adding full bibliography for 7705609--7705612.cif.'
_cod_database_code               7705612
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.404
_shelx_estimated_absorpt_t_min   0.320
_diffrn_oxdiff_digest_frames
;
01990ae10c785ef6b86217811ac83ab0ec000708cf1
;
_diffrn_oxdiff_digest_hkl
;
01e9186474fa6186d9572bd903aafbaea57f6a
;
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C34(H34), C37(H37), C40(H40), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C48(H48A,H48B), C44(H44A,H44B), C50(H50A,H50B), C45(H45A,
 H45B), C49(H49A,H49B), C47(H47A,H47B), C46(H46A,H46B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C12(H12), C11(H11), C9(H9), C17(H17), C3(H3), C6(H6), C16(H16),
 C21(H21), C27(H27), C4(H4), C28(H28), C22(H22), C23(H23), C10(H10), C30(H30),
 C15(H15), C5(H5), C29(H29), C14(H14)
2.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C33(H33A,H33B,
 H33C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C32(H32A,H32B,H32C), C42(H42A,
 H42B,H42C)
;
_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 1.314
_oxdiff_exptl_absorpt_empirical_full_min 0.852