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_7712140
_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         'C46 H54 Au2 N2 P2, 2(B F4), H2 O'
_chemical_formula_sum            'C46 H56 Au2 B2 F8 N2 O P2'
_chemical_formula_weight         1282.42
_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   mixed
_audit_creation_date             2020-09-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-19 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                   28.1116(8)
_cell_length_b                   23.6525(7)
_cell_length_c                   14.2329(5)
_cell_measurement_reflns_used    12087
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      74.8540
_cell_measurement_theta_min      3.6730
_cell_volume                     9463.6(5)
_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     13.00 116.00   0.50    0.05    --   42.05  77.00  30.00  206
  2  \w     32.00 138.00   0.50    0.15    --  106.13 -84.00  48.00  212
  3  \w     33.00 112.00   0.50    0.15    --  106.13-125.00 -90.00  158
  4  \w     32.00  73.00   0.50    0.15    --  106.13 -61.00-150.00   82
  5  \w     32.00  73.00   0.50    0.15    --  106.13 -61.00-120.00   82
  6  \w     20.00  72.00   0.50    0.05    --   42.05  57.00 150.00  104
  7  \w    -24.00  39.00   0.50    0.05    --  -42.05  19.00  90.00  126
  8  \w    -24.00  39.00   0.50    0.05    --  -42.05  19.00 150.00  126
  9  \w    -69.00 -28.00   0.50    0.15    -- -102.00  61.00 120.00   82
 10  \w    -69.00 -28.00   0.50    0.15    -- -102.00  61.00-120.00   82
 11  \w   -108.00 -26.00   0.50    0.15    -- -102.00 110.00-107.00  164
 12  \w    -88.00  -2.00   0.50    0.05    --  -42.05 110.00-107.00  172
 13  \w   -175.00 -79.00   0.50    0.15    -- -102.00 -41.00-120.00  192
;
_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      -0.0152412000
_diffrn_orient_matrix_UB_12      -0.0244864000
_diffrn_orient_matrix_UB_13      0.0956543000
_diffrn_orient_matrix_UB_21      0.0456934000
_diffrn_orient_matrix_UB_22      0.0235478000
_diffrn_orient_matrix_UB_23      0.0451248000
_diffrn_orient_matrix_UB_31      -0.0261068000
_diffrn_orient_matrix_UB_32      0.0555660000
_diffrn_orient_matrix_UB_33      0.0232054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11981
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.828
_diffrn_reflns_theta_min         3.951
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.718
_exptl_absorpt_correction_T_max  0.101
_exptl_absorpt_correction_T_min  0.090
_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    1.800
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 1744 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     424
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+77.5245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.842
_reflns_Friedel_fraction_max     0.768
_reflns_number_gt                4242
_reflns_number_total             4860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03785h2.cif
_cod_data_source_block           olex2_20200904_osawa_sample1
_cod_database_code               7712140
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.208
_shelx_estimated_absorpt_t_min   0.143
_diffrn_oxdiff_digest_frames
;
015373b225078a919f397dc6d6d662ea6100087e77c
;
_diffrn_oxdiff_digest_hkl
;
0141021d70e426dcea981a06ca20649187b679
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.84 with sigma of 0.0001
3. Rigid bond restraints
 Au1, P1, N1, C1, C13, C7, C22, C2, C6, C14, C12, C8, C23, C3, C16, C5, C15,
 C11, C19, C9, C4, C17, C18, C10, C21, C20, B1, F1, F4, F3, F2, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
P1 \\sim Au1 \\sim N1 \\sim C1 \\sim C13 \\sim C7 \\sim C22 \\sim C2 \\sim C6
\\sim C14 \\sim C12 \\sim C8 \\sim C23 \\sim C3 \\sim C16 \\sim C5 \\sim C15
\\sim C11 \\sim C19 \\sim C9 \\sim C4 \\sim C17 \\sim C18 \\sim C10 \\sim C21
\\sim C20 \\sim B1 \\sim F1 \\sim F4 \\sim F3 \\sim F2 \\sim O1: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(P1) \\sim Ueq, Uanis(Au1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C13) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C19(H19), C16(H16)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C9(H9), C10(H10), C6(H6), C15(H15), C11(H11), C3(H3),
 C5(H5), C4(H4)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C)
;
_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 2.232
_oxdiff_exptl_absorpt_empirical_full_min 0.606