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_7705609
_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 Cl2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H64 Au2 Cl2 O2 P2'
_chemical_formula_weight         1223.80
_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                   13.9885(6)
_cell_length_b                   16.7416(7)
_cell_length_c                   20.1362(7)
_cell_measurement_reflns_used    19778
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.0880
_cell_measurement_theta_min      3.4740
_cell_volume                     4715.7(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.820
_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    -25.00   9.00   0.50    0.13    --   -6.28 -90.00  22.00   68
  2  \w    -57.00 -32.00   0.50    0.13    --   -6.28 -67.00 -99.00   50
  3  \w      4.00  75.00   0.50    0.13    --    4.09  37.00-180.00  142
  4  \w     29.00  72.00   0.50    0.13    --    4.09  37.00 -60.00   86
  5  \w     -3.00  24.00   0.50    0.13    --    4.09  37.00 -60.00   54
;
_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      -0.0377961000
_diffrn_orient_matrix_UB_12      -0.0273952000
_diffrn_orient_matrix_UB_13      0.0057133000
_diffrn_orient_matrix_UB_21      -0.0082267000
_diffrn_orient_matrix_UB_22      0.0173744000
_diffrn_orient_matrix_UB_23      0.0316080000
_diffrn_orient_matrix_UB_31      -0.0328095000
_diffrn_orient_matrix_UB_32      0.0272364000
_diffrn_orient_matrix_UB_33      -0.0144516000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33517
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.930
_diffrn_reflns_theta_min         3.270
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.434
_exptl_absorpt_correction_T_max  0.200
_exptl_absorpt_correction_T_min  0.167
_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    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_recrystallization_method THF/hexane
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 4179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         14933
_refine_ls_number_restraints     703
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0244P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.714
_reflns_number_gt                10568
_reflns_number_total             14933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03144e2.cif
_cod_data_source_block           20200205_osawa_lipraucl_thf
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '93 (2)' was changed to
'93(2)' -- the value was reformatted.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705609--7705612.cif.
;
_cod_database_code               7705609
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Au Cl P C H'
_shelx_estimated_absorpt_t_max   0.296
_shelx_estimated_absorpt_t_min   0.248
_diffrn_oxdiff_digest_frames
;
01c2f47815ce9bd55ec7e3b97e6765c57c00068eb84
;
_diffrn_oxdiff_digest_hkl
;
01bd8c5d257860553e3693b06e87a41170412f
;
_reflns_odcompleteness_completeness 99.59
_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. Rigid bond restraints
 C3, Au2, Au1, P2, Cl2, Cl1, P1, C18, C25, C19, C7, C1, C13, C17, C26, C30,
 C24, C20, C12, C8, C2, C6, C14, C16, C40, C27, C29, C23, C37, C21, C11, C34,
 C9, C31, C5, C15, C42, C41, C28, C22, C38, C39, C10, C36, C35, C33, C32, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C3 \\sim Au2 \\sim Au1 \\sim P2 \\sim Cl2 \\sim Cl1 \\sim P1 \\sim C18 \\sim
C25 \\sim C19 \\sim C7 \\sim C1 \\sim C13 \\sim C17 \\sim C26 \\sim C30 \\sim
C24 \\sim C20 \\sim C12 \\sim C8 \\sim C2 \\sim C6 \\sim C14 \\sim C16 \\sim
C40 \\sim C27 \\sim C29 \\sim C23 \\sim C37 \\sim C21 \\sim C11 \\sim C34 \\sim
C9 \\sim C31 \\sim C5 \\sim C15 \\sim C42 \\sim C41 \\sim C28 \\sim C22 \\sim
C38 \\sim C39 \\sim C10 \\sim C36 \\sim C35 \\sim C33 \\sim C32 \\sim C4:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C5) \\sim Ueq, Uanis(Au2) \\sim Ueq, Uanis(Au1) \\sim Ueq, Uanis(P2)
\\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(P1) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 C34(H34), C40(H40), C37(H37), C31(H31)
4.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C49(H49A,H49B), C45(H45A,H45B), C48(H48A,H48B), C47(H47A,
 H47B), C46(H46A,H46B), C44(H44A,H44B), C43(H43A,H43B)
4.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C12(H12), C9(H9), C17(H17), C11(H11), C3(H3), C6(H6), C21(H21),
 C16(H16), C10(H10), C22(H22), C4(H4), C23(H23), C30(H30), C27(H27), C28(H28),
 C5(H5), C14(H14), C15(H15), C29(H29)
4.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C42(H42A,H42B,
 H42C), C41(H41A,H41B,H41C), C39(H39A,H39B,H39C), C33(H33A,H33B,H33C), 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 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.773