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_7709191
_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         'C11 H15 F4 P Sn'
_chemical_formula_sum            'C11 H15 F4 P Sn'
_chemical_formula_weight         372.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-05
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6121)
;
_audit_update_record
;
2021-10-08 deposited with the CCDC.	2021-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.14600(10)
_cell_length_b                   7.16020(10)
_cell_length_c                   32.5086(3)
_cell_measurement_reflns_used    85916
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      40.3180
_cell_measurement_theta_min      3.1690
_cell_volume                     2783.23(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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     -7.00  44.00   1.00   20.00    --   36.51 -99.00  30.00   51
  2  \w     80.00 105.00   1.00   20.00    --   36.51  57.00-180.00   25
  3  \w    -31.00  54.00   1.00   20.00    --   36.51 -57.00 -90.00   85
  4  \w    -15.00  75.00   1.00   20.00    --   36.51 -99.00 -90.00   90
  5  \w     14.00  40.00   1.00   20.00    --   36.51  57.00-120.00   26
  6  \w     50.00  75.00   1.00   20.00    --   36.51 -99.00  30.00   25
  7  \w     20.00 103.00   1.00   20.00    --   36.51  57.00 -90.00   83
  8  \w     39.00 115.00   1.00   20.00    --   36.51 178.00-150.00   76
  9  \w     13.00 103.00   1.00   20.00    --   36.51  57.00  30.00   90
 10  \w     12.00  56.00   1.00   20.00    --   36.51  57.00-180.00   44
 11  \w    -23.00  51.00   1.00   20.00    --   36.51 -57.00 150.00   74
 12  \w     66.00  92.00   1.00   20.00    --   36.51  57.00-120.00   26
 13  \w     14.00  91.00   1.00   20.00    --   36.51  57.00 -30.00   77
 14  \w     45.00 109.00   1.00   20.00    --   36.51 178.00-180.00   64
 15  \w      6.00  61.00   1.00   20.00    --   36.51  19.00 150.00   55
 16  \w     66.00 109.00   1.00   20.00    --   36.51  19.00 150.00   43
 17  \w     22.00  75.00   1.00   20.00    --   36.51 -99.00-180.00   53
 18  \w     21.00 102.00   1.00   20.00    --   36.51  38.00-120.00   81
 19  \w     16.00  49.00   1.00   20.00    --   36.51  38.00-180.00   33
 20  \w     54.00 108.00   1.00   20.00    --   36.51  38.00-180.00   54
 21  \w     45.00 120.00   1.00   20.00    --   36.51-178.00 120.00   75
 22  \w    -41.00 -15.00   1.00   20.00    --  -36.82 -57.00  30.00   26
 23  \w    -95.00 -45.00   1.00   20.00    --  -36.82 -57.00  30.00   50
 24  \w    -42.00 -16.00   1.00   20.00    --  -36.82 -57.00 -60.00   26
 25  \w   -104.00 -68.00   1.00   20.00    --  -36.82 -57.00 -60.00   36
 26  \w   -103.00 -15.00   1.00   20.00    --  -36.82 -57.00   0.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0161707000
_diffrn_orient_matrix_UB_12      -0.0667588000
_diffrn_orient_matrix_UB_13      -0.0139151000
_diffrn_orient_matrix_UB_21      -0.0103159000
_diffrn_orient_matrix_UB_22      0.0660750000
_diffrn_orient_matrix_UB_23      -0.0164924000
_diffrn_orient_matrix_UB_31      0.0561184000
_diffrn_orient_matrix_UB_32      0.0314367000
_diffrn_orient_matrix_UB_33      0.0050946000
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            141539
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.971
_diffrn_reflns_theta_min         2.804
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020)
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    1.780
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.162
_refine_diff_density_min         -3.232
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.373
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         12229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.373
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0580
_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^)+11.3520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11463
_reflns_number_total             12229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03658k2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7709188--7709191.cif.'
_cod_database_code               7709191
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C88 H120 F32 P8 Sn8 '
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     40.15
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              22316
_shelx_hkl_checksum              20409
_olex2_date_sample_data_collection 2020-04-25
_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 1.293
_oxdiff_exptl_absorpt_empirical_full_min 0.763