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_7705610
_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 Br2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H64 Au2 Br2 O2 P2'
_chemical_formula_weight         1312.70
_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             2020-02-05
_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                   14.0829(7)
_cell_length_b                   16.7889(7)
_cell_length_c                   20.2432(8)
_cell_measurement_reflns_used    13845
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      29.7260
_cell_measurement_theta_min      3.3630
_cell_volume                     4786.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.803
_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    -14.00  11.00   0.50    6.81    --   -6.12  22.00  36.00   50
  2  \w     24.00  69.00   0.50    6.81    --   -6.12  22.00  36.00   90
  3  \w    -11.00  37.00   0.50    6.81    --    3.93 -99.00-120.00   96
  4  \w    -18.00   9.00   0.50    6.81    --   -6.12 -99.00-120.00   54
  5  \w    -18.00  27.00   0.50    6.81    --   -6.12 -99.00 -90.00   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      0.0459766000
_diffrn_orient_matrix_UB_12      0.0147628000
_diffrn_orient_matrix_UB_13      0.0071955000
_diffrn_orient_matrix_UB_21      0.0196647000
_diffrn_orient_matrix_UB_22      -0.0378687000
_diffrn_orient_matrix_UB_23      -0.0073720000
_diffrn_orient_matrix_UB_31      0.0056241000
_diffrn_orient_matrix_UB_32      0.0115485000
_diffrn_orient_matrix_UB_33      -0.0335202000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32230
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.751
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.827
_diffrn_reflns_theta_min         3.254
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.898
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (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    1.822
_exptl_crystal_description       plate
_exptl_crystal_F_000             2552
_exptl_crystal_recrystallization_method THF/hexane
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 3848 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         15027
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0202P)^2^+3.0517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.689
_reflns_number_gt                10052
_reflns_number_total             15027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03144e2.cif
_cod_data_source_block           20200205_osawa_lipraubr_thf
_cod_depositor_comments
'Adding full bibliography for 7705609--7705612.cif.'
_cod_database_code               7705610
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Au P O Br C H'
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.384
_diffrn_oxdiff_digest_frames
;
01f838a21f3714a53b5fa0bdd90fc216e40002562f3
;
_diffrn_oxdiff_digest_hkl
;
012643fde17a2f7dd772922ac84cc1c5af6cb1
;
_reflns_odcompleteness_completeness 99.63
_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. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(Au2) \\sim Ueq, Uanis(Au1) \\sim Ueq, Uanis(Br2)
\\sim Ueq, Uanis(P30) \\sim Ueq, Uanis(Br1) \\sim Ueq, Uanis(P11) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C34(H34), C40(H40), C37(H37), C31(H31)
3.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B), C45(H45A,H45B), C50(H50A,
 H50B), C48(H48A,H48B), C49(H49A,H49B), C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C12(H12), C9(H9), C17(H17), C16(H16), C3(H3), C11(H11), C28(H28),
 C4(H4), C27(H27), C21(H21), C10(H10), C22(H22), C14(H14), C23(H23), C30(H30),
 C15(H15), C29(H29), C6(H6), C5(H5)
3.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C33(H33A,H33B,
 H33C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C32(H32A,
 H32B,H32C)
;
_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 1.085
_oxdiff_exptl_absorpt_empirical_full_min 0.888