Coinage metal complexes of BN analogues of m-terphenyl ligands
Lamprecht, Anna; Lindl, Felix; Endres, Lukas; Krummenacher, Ivo; Braunschweig, Holger; Chemical Communications  (2023) –; doi:10.1039/D3CC03467D

data_7131916
_publ_section_title
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 Coinage metal complexes of BN analogues of m-terphenyl ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03467D
_journal_year                    2023
_chemical_formula_moiety         'C55 H64 Au B N P, C6 H6'
_chemical_formula_sum            'C61 H70 Au B N P'
_chemical_formula_weight         1055.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2x (K.Radacki, 2005-21)'
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.52780(10)
_cell_length_b                   11.60230(10)
_cell_length_c                   29.4589(2)
_cell_measurement_reflns_used    39264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8930
_cell_measurement_theta_min      2.9260
_cell_volume                     5140.59(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(11)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_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     19.00  59.00   0.50    0.05    --   58.61 -93.00 163.00   80
   2  \w    -58.00 -32.00   0.50    0.05    --  -60.19  93.00 -85.00   52
   3  \w    -76.00 -51.00   0.50    0.05    --  -69.72  93.00 -85.00   50
   4  \w     29.00  54.00   0.50    0.05    --   71.30 -93.00 163.00   50
   5  \w    -82.00 -57.00   0.50    0.05    --  -76.37  93.00 -85.00   50
   6  \w     40.00  65.00   0.50    0.05    --   82.31 -93.00 163.00   50
   7  \w     17.00  43.00   0.50    0.05    --    6.00  64.00 147.40   52
   8  \w     24.00  49.00   0.50    0.05    --   58.61 -95.00-120.00   50
   9  \w     29.00  54.00   0.50    0.05    --   71.30 -95.00-150.00   50
  10  \w     47.00  73.00   0.50    0.05    --   71.30 -95.00-120.00   52
  11  \w   -120.00 -88.00   0.50    0.05    --  -74.00 -45.00 -51.82   64
  12  \w   -121.00 -88.00   0.50    0.05    --  -74.00 -57.00  81.21   66
  13  \w   -121.00 -92.00   0.50    0.05    --  -74.00 -58.00-117.68   58
  14  \w   -127.00 -94.00   0.50    0.05    --  -79.50 -49.00 170.16   66
  15  \w   -123.00 -92.00   0.50    0.05    --  -79.50 -57.00-150.43   62
  16  \w   -120.00 -95.00   0.50    0.05    --  -79.50 -65.00 155.73   50
  17  \w   -128.00-102.00   0.50    0.05    --  -79.50-115.00-107.08   52
  18  \w   -119.00 -94.00   0.50    0.05    --  -79.50 -48.00-101.21   50
  19  \w     60.00  85.00   0.50    0.05    --   82.31 -95.00 -90.00   50
  20  \w     72.00  97.00   0.50    0.05    --   82.31-112.00 -90.00   50
  21  \w    100.00 130.00   0.50    0.05    --   85.25  63.00  19.44   60
  22  \w     50.00  76.00   0.50    0.05    --   85.25 -95.00  92.49   52
  23  \w     98.00 125.00   0.50    0.05    --   85.25  53.00 124.19   54
  24  \w     98.00 123.00   0.50    0.05    --   85.25  54.00 176.36   50
  25  \w    103.00 133.00   0.50    0.05    --   85.25 133.00-107.26   60
  26  \w     46.00  71.00   0.50    0.05    --   85.25 -83.00-156.61   50
  27  \w     53.00  95.00   0.50    0.05    --   85.25-104.00 -33.11   84
  28  \w     48.00  79.00   0.50    0.05    --   85.25 -82.00 -11.62   62
  29  \w     98.00 130.00   0.50    0.05    --   85.25  53.00 -51.97   64
  30  \w     59.00  88.00   0.50    0.05    --   85.25-106.00-168.26   58
  31  \w     77.00 133.00   0.50    0.05    --   85.25  11.00  59.92  112
  32  \w     63.00 102.00   0.50    0.05    --   85.25-130.00 179.63   78
  33  \w     48.00  97.00   0.50    0.05    --   85.25-112.00-117.86   98
  34  \w     47.00  85.00   0.50    0.05    --   85.25 -94.00 117.23   76
  35  \w     38.00  97.00   0.50    0.05    --   85.25-124.00 -34.12  118
  36  \w    100.00 134.00   0.50    0.05    --   85.25  52.00 -26.90   68
  37  \w     66.00  92.00   0.50    0.05    --   85.25-105.00  51.65   52
  38  \w     78.00 104.00   0.50    0.05    --   85.25  16.00 109.72   52
  39  \w     46.00  87.00   0.50    0.05    --   85.25 -90.00-128.07   82
  40  \w     59.00  86.00   0.50    0.05    --   85.25-108.00  41.62   54
  41  \w     61.00  87.00   0.50    0.05    --   85.25-139.00 -61.05   52
  42  \w    108.00 133.00   0.50    0.05    --   85.25  16.00 109.72   50
  43  \w    105.00 130.00   0.50    0.05    --   85.25 124.00  94.17   50
  44  \w     58.00  83.00   0.50    0.05    --   85.25 -82.00 -35.73   50
  45  \w     47.00  73.00   0.50    0.05    --   85.25 -94.00 165.66   52
  46  \w    102.00 128.00   0.50    0.05    --   85.25  55.00  75.18   52

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            58848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.238
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    5.955
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) 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            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.914
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         10519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0243P)^2^+6.4116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10000
_reflns_number_total             10519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03467d2.cif
_cod_data_source_block           2-AuPCy3
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7131916
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.512
_shelx_estimated_absorpt_t_max   0.716
_shelx_res_checksum              58005
_shelx_hkl_checksum              92623