Near-white light emission from single crystals of cationic dinuclear gold(I) complexes with bridged diphosphine ligands.
Osawa, Masahisa; Soma, Sakie; Kobayashi, Hiroyuki; Tanaka, Yuya; Hoshino, Mikio; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt03785h

data_7712139
_publ_section_title
;
 Near-white light emission from single crystals of cationic dinuclear
 gold(I) complexes with bridged diphosphine ligands.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt03785h
_journal_year                    2023
_chemical_formula_moiety         'C42 H46 Au2 N2 P2, 2(B F4)'
_chemical_formula_sum            'C42 H46 Au2 B2 F8 N2 P2'
_chemical_formula_weight         1208.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-12-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-17 deposited with the CCDC.	2022-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.9142(12)
_cell_length_b                   24.8726(17)
_cell_length_c                   13.0916(6)
_cell_measurement_reflns_used    5791
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.5300
_cell_measurement_theta_min      3.5860
_cell_volume                     8763.9(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.972
_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     20.00 116.00   0.50    0.30    --   41.68  57.00   0.00  192
  2  \w     20.00  59.00   0.50    0.30    --   41.68  57.00 120.00   78
  3  \w    -38.00  28.00   0.50    0.30    --   41.68 -19.00 120.00  132
  4  \w     32.00  73.00   0.50    1.20    --  106.13 -61.00 150.00   82
  5  \w     32.00  73.00   0.50    1.20    --  106.13 -61.00  90.00   82
  6  \w     32.00  73.00   0.50    1.20    --  106.13 -61.00 -30.00   82
  7  \w    -24.00  39.00   0.50    0.30    --  -41.68  19.00-180.00  126
  8  \w    -87.00  -2.00   0.50    0.30    --  -41.68 109.00  -5.00  170
  9  \w    -69.00 -28.00   0.50    1.20    -- -102.00  61.00  30.00   82
 10  \w   -112.00 -28.00   0.50    1.20    -- -102.00 125.00  60.00  168
 11  \w    -69.00 -28.00   0.50    1.20    -- -102.00  61.00 150.00   82
 12  \w     32.00 109.00   0.50    1.20    --  106.13-113.00 167.00  154
 13  \w     30.00 107.00   0.50    1.20    --  106.13-109.00-102.00  154
 14  \w   -175.00 -73.00   0.50    1.20    -- -102.00 -22.00   2.00  204
;
_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      -0.0014980000
_diffrn_orient_matrix_UB_12      -0.0506656000
_diffrn_orient_matrix_UB_13      0.0677811000
_diffrn_orient_matrix_UB_21      -0.0166152000
_diffrn_orient_matrix_UB_22      -0.0337754000
_diffrn_orient_matrix_UB_23      -0.0923956000
_diffrn_orient_matrix_UB_31      0.0547348000
_diffrn_orient_matrix_UB_32      -0.0118051000
_diffrn_orient_matrix_UB_33      -0.0263710000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10347
_diffrn_reflns_point_group_measured_fraction_full 0.816
_diffrn_reflns_point_group_measured_fraction_max 0.780
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.292
_diffrn_reflns_theta_min         4.155
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.672
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.319
_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    1.832
_exptl_crystal_description       cube
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.914
_refine_diff_density_min         -2.672
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0605
_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^)+(0.1347P)^2^+55.5707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1673
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.535
_reflns_Friedel_fraction_full    0.613
_reflns_Friedel_fraction_max     0.570
_reflns_number_gt                3393
_reflns_number_total             4461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03785h2.cif
_cod_data_source_block           201215_osawa1
_cod_database_code               7712139
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.342
_diffrn_oxdiff_digest_frames
;
019ab0d7d8ec6cd93d2d7a9da059966eeb000499344
;
_diffrn_oxdiff_digest_hkl
;
013090e435e83d0b465a243049851be705cc0e
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 C17, Au1, N1, P1, C16, C13, C7, C1, C14, C12, C8, C2, C6, C15, C11, C1AA, C9,
 C3, C0AA, C5, C10, C1D, C4, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C7 \\sim Au1 \\sim N1 \\sim P1 \\sim C16 \\sim C13 \\sim C1 \\sim C17 \\sim C14
\\sim C12 \\sim C8 \\sim C2 \\sim C6 \\sim C15 \\sim C11 \\sim C1AA \\sim C9
\\sim C3 \\sim C0AA \\sim C5 \\sim C10 \\sim C1D \\sim C4 \\sim C2AA: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C17) \\sim Ueq, Uanis(Au1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(P1)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C1D) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C0AA(H0AA,H0AB)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C10(H10), C9(H9), C11(H11), C15(H15), C3(H3), C6(H6),
 C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C2AA(H2AA,H2AB,H2AC), C17(H17A,H17B,H17C), C1D(H1DA,H1DB,H1DC)
;
_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 1.985
_oxdiff_exptl_absorpt_empirical_full_min 0.502