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_7709188
_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 H19 P Sn'
_chemical_formula_sum            'C11 H19 P Sn'
_chemical_formula_weight         300.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-04
_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                90
_cell_angle_beta                 99.6724(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.78125(10)
_cell_length_b                   10.56152(12)
_cell_length_c                   16.2469(2)
_cell_measurement_reflns_used    53547
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      54.6650
_cell_measurement_theta_min      3.1850
_cell_volume                     1316.22(3)
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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    -66.00  21.00   1.00    4.00    --    2.00 -59.00 116.81   87
  2  \w    -37.00 -10.00   1.00    4.00    --   18.00 126.00 -71.21   27
  3  \w    -13.00  12.00   1.00    4.00    --   30.00 104.00-111.63   25
  4  \w    -33.00  54.00   1.00    4.00    --   35.08 -57.00 150.00   87
  5  \w    -32.00  53.00   1.00    4.00    --   35.08 -57.00   0.00   85
  6  \w    -32.00  62.00   1.00    4.00    --   35.08 -77.00-120.00   94
  7  \w      3.00  28.00   1.00    4.00    --   38.00  88.00 115.78   25
  8  \w     16.00  41.00   1.00    4.00    --   46.00  79.00 160.32   25
  9  \w     15.00  40.00   1.00    4.00    --   46.00  81.00  84.56   25
 10  \w     15.00  42.00   1.00    4.00    --   46.00  82.00 -31.62   27
 11  \w     15.00  40.00   1.00    4.00    --   46.00  82.00-126.74   25
 12  \w     15.00  40.00   1.00    4.00    --   46.00  82.00-168.77   25
 13  \w     15.00  40.00   1.00    4.00    --   46.00  82.00  24.87   25
 14  \w     15.00  41.00   1.00    4.00    --   46.00  82.00 -79.62   26
 15  \w     27.00  53.00   1.00    4.00    --   54.00  74.00-110.29   26
 16  \w     31.00  57.00   1.00   16.00    --   58.00  74.00  33.38   26
 17  \w     88.00 117.00   1.00   16.00    --   58.00  73.00 114.27   29
 18  \w     32.00  58.00   1.00   16.00    --   58.00  73.00 114.27   26
 19  \w     32.00  64.00   1.00   16.00    --   58.00  73.00 -80.21   32
 20  \w     31.00  68.00   1.00   16.00    --   58.00  74.00 156.04   37
 21  \w     68.00 105.00   1.00   16.00    --   58.00  73.00 -80.21   37
 22  \w     33.00  58.00   1.00   16.00    --   58.00  71.00  -4.14   25
 23  \w     36.00  62.00   1.00   16.00    --   62.00  72.00-172.13   26
 24  \w     37.00  63.00   1.00   16.00    --   62.00  70.00  89.45   26
 25  \w     40.00  68.00   1.00   16.00    --   66.00  73.00  53.91   28
 26  \w     41.00  67.00   1.00   16.00    --   66.00  71.00-108.04   26
 27  \w     42.00  68.00   1.00   16.00    --   66.00  68.00 -33.37   26
 28  \w     43.00  69.00   1.00   16.00    --   70.00  74.00 176.66   26
 29  \w     92.00 141.00   1.00   16.00    --   74.00  73.00-100.39   49
 30  \w     48.00  87.00   1.00   16.00    --   74.00  73.00-100.39   39
 31  \w     16.00 105.00   1.00   16.00    --   75.09 -94.00   0.00   89
 32  \w     85.00 132.00   1.00   16.00    --   75.09  67.00-173.27   47
 33  \w     52.00  79.00   1.00   16.00    --   75.09  67.00-173.27   27
 34  \w     50.00  79.00   1.00   16.00    --   75.09  72.00  -6.56   29
 35  \w     48.00 135.00   1.00   16.00    --   75.09  74.00 144.92   87
 36  \w    103.00 139.00   1.00   16.00    --   75.09 117.00 -97.00   36
 37  \w     51.00 143.00   1.00   16.00    --   75.09  69.00  50.93   92
 38  \w     55.00 130.00   1.00   16.00    --   75.09  61.00-120.00   75
 39  \w    114.00 143.00   1.00   16.00    --   75.09  67.00-150.01   29
 40  \w     52.00  78.00   1.00   16.00    --   75.09  67.00-150.01   26
 41  \w     81.00 120.00   1.00   16.00    --   75.09  68.00  14.14   39
 42  \w     65.00  90.00   1.00   16.00    --   75.09 -30.00 -90.00   25
 43  \w     13.00  50.00   1.00   16.00    --   75.09 -30.00 -90.00   37
 44  \w     51.00  77.00   1.00   16.00    --   75.09  68.00  14.14   26
 45  \w      6.00  94.00   1.00   16.00    --   75.09 -77.00  90.00   88
 46  \w     48.00  77.00   1.00   16.00    --   75.09  74.00 -74.95   29
 47  \w     84.00 113.00   1.00   16.00    --   75.09-125.00 -90.00   29
 48  \w      9.00  55.00   1.00   16.00    --   75.09-125.00 -90.00   46
 49  \w     91.00 143.00   1.00   16.00    --   75.09  65.00  83.08   52
 50  \w     53.00  80.00   1.00   16.00    --   75.09  65.00  83.08   27
 51  \w     85.00 139.00   1.00   16.00    --   75.09  70.00 -19.02   54
 52  \w     55.00  80.00   1.00   16.00    --   75.09  61.00 120.00   25
 53  \w     24.00  71.00   1.00   16.00    --   75.09-125.00  90.00   47
 54  \w     50.00  75.00   1.00   16.00    --   75.09  70.00 -19.02   25
 55  \w     11.00  83.00   1.00   16.00    --   75.09 -61.00-120.00   72
 56  \w     52.00 139.00   1.00   16.00    --   75.09  67.00 -53.54   87
 57  \w      6.00 104.00   1.00   16.00    --   75.09 -77.00-180.00   98
 58  \w     53.00 121.00   1.00   16.00    --   75.09  65.00 130.91   68
 59  \w    117.00 142.00   1.00   16.00    --   75.09  72.00  -6.56   25
;
_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      0.0682473000
_diffrn_orient_matrix_UB_12      0.0116040000
_diffrn_orient_matrix_UB_13      0.0339610000
_diffrn_orient_matrix_UB_21      -0.0613807000
_diffrn_orient_matrix_UB_22      0.0009687000
_diffrn_orient_matrix_UB_23      0.0277124000
_diffrn_orient_matrix_UB_31      0.0109974000
_diffrn_orient_matrix_UB_32      -0.0661488000
_diffrn_orient_matrix_UB_33      0.0063576000
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            156309
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         55.171
_diffrn_reflns_theta_min         2.543
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.023
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.234
_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    1.519
_exptl_crystal_description       cylindrically
_exptl_crystal_F_000             600
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.622
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.689
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         16781
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13305
_reflns_number_total             16781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03658k2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7709188--7709191.cif.'
_cod_database_code               7709188
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H19 P Sn'
_chemical_oxdiff_usercomment
'In situ grown. Ultrasonic at 200 K, at 240 polycrystalline material, at 289.0K seed, 1K/h to 127 K, 5 K/h to 240 and 360 K/h to 100K.'
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.366
_diffrn_oxdiff_digest_frames
;
0195b18319542829d022a10f7feba1a11f02528da1c
;
_diffrn_oxdiff_digest_hkl
;
011bd96a356f4cf6f8675a2a9944b603349161
;
_reflns_odcompleteness_completeness 96.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     55.56
_olex2_refinement_description
;
1. Restrained distances
 C9-H9D \\sim C9-H9C \\sim C9-H9F \\sim C9-H9B \\sim C9-H9E \\sim C9-H9A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uiso(H9C) = Uiso(H9F) = Uiso(H9B) = Uiso(H9E) = Uiso(H9A) = Uiso(H9D)
3. Others
 Sof(H9A)=Sof(H9B)=Sof(H9C)=1-FVAR(1)
 Sof(H9D)=Sof(H9E)=Sof(H9F)=FVAR(1)
;
_shelx_res_checksum              82915
_shelx_hkl_checksum              62273
_olex2_date_sample_data_collection 2020-11-03
_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 3.675
_oxdiff_exptl_absorpt_empirical_full_min 0.592