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_7131912
_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         'C52 H58 B Cu N P, 2(C6 H6)'
_chemical_formula_sum            'C64 H70 B Cu N P'
_chemical_formula_weight         958.53
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9971(2)
_cell_length_b                   10.8689(2)
_cell_length_c                   28.2935(3)
_cell_measurement_reflns_used    20215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1620
_cell_measurement_theta_min      2.9220
_cell_volume                     5216.56(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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      100.01(11)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  96.00   0.50    1.73    --   50.00  52.00 -21.30   60
   2  \w     66.00  96.00   0.50    1.73    --   50.00  52.00  76.47   60
   3  \w     21.00  67.00   0.50    1.73    --   61.21 -95.00-150.00   92
   4  \w   -119.00 -84.00   0.50    1.73    --  -70.00 -36.00  66.23   70
   5  \w   -119.00 -83.00   0.50    1.73    --  -70.00 -35.00 103.31   72
   6  \w   -119.00 -89.00   0.50    1.73    --  -74.00 -56.00  89.67   60
   7  \w   -125.00 -94.00   0.50    1.73    --  -79.50 -55.00  66.61   62
   8  \w   -126.00 -95.00   0.50    1.73    --  -79.50 -50.00  -9.29   62
   9  \w   -126.00 -96.00   0.50    1.73    --  -79.50 -49.00 111.62   60
  10  \w   -122.00 -96.00   0.50    1.73    --  -79.50 -54.00-157.06   52
  11  \w    -90.00 -35.00   0.50    1.73    --  -79.50 108.00 -12.97  110
  12  \w    -90.00 -46.00   0.50    1.73    --  -79.50 132.00-133.84   88
  13  \w   -126.00-101.00   0.50    1.73    --  -79.50-123.00-107.05   50
  14  \w   -122.00 -97.00   0.50    1.73    --  -79.50 -65.00 -64.21   50
  15  \w   -123.00 -98.00   0.50    1.73    --  -79.50 -62.00-154.55   50
  16  \w     46.00  72.00   0.50    1.73    --   80.41 -95.00   0.00   52
  17  \w     97.00 122.00   0.50    1.73    --   83.50 128.00-110.82   50
  18  \w     98.00 124.00   0.50    1.73    --   83.50  57.00  80.76   52
  19  \w     62.00  89.00   0.50    1.73    --   83.50-114.00  82.54   54
  20  \w     41.00  92.00   0.50    1.73    --   83.50-102.00-163.93  102
  21  \w     63.00  95.00   0.50    1.73    --   83.50-110.00 -50.14   64
  22  \w     96.00 124.00   0.50    1.73    --   83.50 128.00  39.86   56
  23  \w     42.00 102.00   0.50    1.73    --   83.50-130.00-158.24  120
  24  \w     42.00  97.00   0.50    1.73    --   83.50-120.00  60.91  110
  25  \w     46.00  71.00   0.50    1.73    --   83.50 -86.00  85.16   50
  26  \w     70.00  97.00   0.50    1.73    --   83.50-114.00  32.83   54
  27  \w    100.00 125.00   0.50    1.73    --   83.50  47.00 108.37   50
  28  \w    100.00 125.00   0.50    1.73    --   83.50 120.00 168.23   50
  29  \w     97.00 122.00   0.50    1.73    --   83.50 125.00 -79.13   50
  30  \w     98.00 123.00   0.50    1.73    --   83.50  56.00 -68.84   50
  31  \w     44.00  69.00   0.50    1.73    --   83.50 -72.00  33.88   50
  32  \w    102.00 128.00   0.50    1.73    --   83.50  56.00 -44.80   52
  33  \w     45.00  92.00   0.50    1.73    --   83.50-101.00-142.64   94
  34  \w     52.00  79.00   0.50    1.73    --   83.50 -94.00 109.94   54
  35  \w     99.00 124.00   0.50    1.73    --   83.50  54.00 112.63   50
  36  \w    100.00 125.00   0.50    1.73    --   83.50  54.00 -53.45   50
  37  \w     44.00  70.00   0.50    1.73    --   83.50-136.00 174.61   52
  38  \w     44.00  95.00   0.50    1.73    --   83.50-107.00  -5.25  102
  39  \w     47.00  83.00   0.50    1.73    --   83.50 -93.00 -97.43   72
  40  \w     94.00 119.00   0.50    1.73    --   83.50 131.00-131.10   50

;
_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  0.0537
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53718
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.683
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.643
_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            'light colourless'
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.539
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0627P)^2^+7.2031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8398
_reflns_number_total             10705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03467d2.cif
_cod_data_source_block           1-CuPCy3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7131912
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.757
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              28967
_shelx_hkl_checksum              50519