Synthesis, structural and photophysical properties of dimethylphosphino(perfluoro-)phenylene-based gold(I) dimers.
Müller, Felix; Wickemeyer, Lucas; Schwabedissen, Jan; Ertl, Martin; Neumann, Beate; Stammler, Hans-Georg; Monkowius, Uwe; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1955–1967; doi:10.1039/d1dt03658k

data_7709189
_publ_section_title
;
 Synthesis, structural and photophysical properties of
 dimethylphosphino(perfluoro-)phenylene-based gold(I) dimers.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1955
_journal_page_last               1967
_journal_paper_doi               10.1039/d1dt03658k
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C16 H20 Au2 P2, C H2 Cl2'
_chemical_formula_sum            'C17 H22 Au2 Cl2 P2'
_chemical_formula_weight         753.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-10-08 deposited with the CCDC.	2021-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                87.267(2)
_cell_angle_beta                 67.328(3)
_cell_angle_gamma                68.529(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1778(3)
_cell_length_b                   11.0554(3)
_cell_length_c                   11.4165(3)
_cell_measurement_reflns_used    39362
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.9280
_cell_measurement_theta_min      1.9380
_cell_volume                     988.78(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_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      6.00  95.00   1.00    5.04    --   26.03  57.00-150.00   89
  2  \w      6.00  95.00   1.00    5.04    --   26.03  57.00  90.00   89
  3  \w    -43.00  47.00   1.00    5.04    --   26.03 -57.00  60.00   90
  4  \w      1.00  98.00   1.00    5.04    --   26.03  38.00   0.00   97
  5  \w     -4.00  42.00   1.00    5.04    --   26.03  77.00-180.00   46
  6  \w     -4.00  42.00   1.00    5.04    --   26.03  77.00 -60.00   46
  7  \w    -47.00  70.00   1.00    5.04    --   26.03 -19.00-180.00  117
  8  \w    -15.00  68.00   1.00    5.04    --   26.03 -99.00   0.00   83
  9  \w      6.00  95.00   1.00    5.04    --   26.03  57.00 150.00   89
 10  \w     -4.00  42.00   1.00    5.04    --   26.03  77.00  30.00   46
 11  \w     37.00 103.00   1.00    5.04    --   26.03-178.00 -30.00   66
 12  \w    -15.00  68.00   1.00    5.04    --   26.03 -99.00-180.00   83
 13  \w      1.00  98.00   1.00    5.04    --   26.03  38.00 -30.00   97
 14  \w     39.00 102.00   1.00    5.04    --   26.03 178.00   0.00   63
 15  \w    -15.00  68.00   1.00    5.04    --   26.03 -99.00  60.00   83
 16  \w     -4.00  42.00   1.00    5.04    --   26.03  77.00-150.00   46
 17  \w    -42.00  56.00   1.00    5.04    --   26.03 -77.00-150.00   98
 18  \w    -47.00  99.00   1.00    5.04    --   26.03   0.00-180.00  146
 19  \w    -47.00  99.00   1.00    5.04    --   26.03   0.00-150.00  146
 20  \w    -47.00  99.00   1.00    5.04    --   26.03   0.00-120.00  146
 21  \w    -47.00  99.00   1.00    5.04    --   26.03   0.00 -90.00  146
 22  \w    -46.00  52.00   1.00    5.04    --   26.03 -38.00 -60.00   98
 23  \w    -47.00  99.00   1.00    5.04    --   26.03   0.00 -30.00  146
 24  \w    -47.00  95.00   1.00    5.04    --   26.03   0.00   0.00  142
 25  \w    -47.00  99.00   1.00    5.04    --   26.03   0.00 -60.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0096371000
_diffrn_orient_matrix_UB_12      -0.0477725000
_diffrn_orient_matrix_UB_13      -0.0446314000
_diffrn_orient_matrix_UB_21      0.0773861000
_diffrn_orient_matrix_UB_22      0.0049849000
_diffrn_orient_matrix_UB_23      -0.0424524000
_diffrn_orient_matrix_UB_31      0.0457963000
_diffrn_orient_matrix_UB_32      -0.0500301000
_diffrn_orient_matrix_UB_33      0.0281736000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60949
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.312
_diffrn_reflns_theta_min         1.945
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.248
_exptl_absorpt_correction_T_max  0.174
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.530
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.137
_refine_diff_density_max         2.171
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.00185(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0259P)^2^+3.4267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6448
_reflns_number_total             6669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03658k2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7709188--7709191.cif.'
_cod_original_cell_volume        988.78(5)
_cod_database_code               7709189
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H22Au2Cl2P2
_diffrn_oxdiff_digest_frames
;
018f4e1c27edb10c34a37f8f2b9fdfd79102544cfee
;
_diffrn_oxdiff_digest_hkl
;
01f65d96115106008c2b8cb39b3c2f439dd61c
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              36550
_shelx_hkl_checksum              45687
_olex2_date_sample_data_collection 2021-02-17
_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 2.157
_oxdiff_exptl_absorpt_empirical_full_min 0.586