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_7131914
_publ_section_title
;
 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 B Cu N P, C6 H6'
_chemical_formula_sum            'C61 H70 B Cu N P'
_chemical_formula_weight         922.50
_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                 104.0690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.52130(10)
_cell_length_b                   11.63020(10)
_cell_length_c                   29.0122(2)
_cell_measurement_reflns_used    98181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.3280
_cell_measurement_theta_min      2.9610
_cell_volume                     5080.07(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      100.00(10)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -20.00   6.00   0.50    1.85    --  -14.00  96.00 -10.85   52
   2  \w     58.00  88.00   0.50    1.85    --   42.00  52.00  40.52   60
   3  \w    -90.00 -57.00   0.50    1.85    --  -42.00 -45.00 159.83   66
   4  \w     62.00  93.00   0.50    1.85    --   46.00  51.00-163.99   62
   5  \w   -101.00 -70.00   0.50    1.85    --  -54.00 -50.00 -75.19   62
   6  \w   -105.00 -74.00   0.50    1.85    --  -58.00 -48.00-109.75   62
   7  \w     21.00  67.00   0.50    1.85    --   61.21 -95.00 150.00   92
   8  \w   -108.00 -78.00   0.50    1.85    --  -62.00 -51.00  93.55   60
   9  \w   -109.00 -78.00   0.50    1.85    --  -62.00 -48.00  40.55   62
  10  \w   -114.00 -86.00   0.50    1.85    --  -70.00 -60.00 162.14   56
  11  \w   -126.00 -92.00   0.50    1.85    --  -79.50-122.00-132.55   68
  12  \w   -122.00 -95.00   0.50    1.85    --  -79.50 -65.00 -10.33   54
  13  \w   -102.00 -34.00   0.50    1.85    --  -79.50 129.00-160.03  136
  14  \w   -100.00 -33.00   0.50    1.85    --  -79.50 123.00 -37.68  134
  15  \w   -101.00 -33.00   0.50    1.85    --  -79.50 126.00-144.58  136
  16  \w    -97.00 -33.00   0.50    1.85    --  -79.50 115.00  69.60  128
  17  \w   -128.00 -94.00   0.50    1.85    --  -79.50 -41.00-167.20   68
  18  \w   -122.00 -94.00   0.50    1.85    --  -79.50 -64.00-165.54   56
  19  \w    -97.00 -33.00   0.50    1.85    --  -79.50 115.00  13.35  128
  20  \w   -105.00 -34.00   0.50    1.85    --  -79.50 134.00 112.01  142
  21  \w   -123.00 -93.00   0.50    1.85    --  -79.50 -63.00  87.04   60
  22  \w   -126.00 -97.00   0.50    1.85    --  -79.50-113.00-104.85   58
  23  \w    -95.00 -35.00   0.50    1.85    --  -79.50 109.00 -42.42  120
  24  \w   -124.00 -84.00   0.50    1.85    --  -79.50-138.00-117.51   80
  25  \w    -87.00 -37.00   0.50    1.85    --  -79.50  99.00  73.63  100
  26  \w    -97.00 -33.00   0.50    1.85    --  -79.50 116.00-167.82  128
  27  \w   -124.00 -86.00   0.50    1.85    --  -79.50-135.00 -61.93   76
  28  \w   -122.00 -95.00   0.50    1.85    --  -79.50 -65.00 114.43   54
  29  \w    -95.00 -35.00   0.50    1.85    --  -79.50 109.00 147.43  120
  30  \w   -124.00 -85.00   0.50    1.85    --  -79.50-136.00-149.18   78
  31  \w   -122.00 -95.00   0.50    1.85    --  -79.50 -65.00 146.57   54
  32  \w   -126.00 -94.00   0.50    1.85    --  -79.50-118.00 115.31   64
  33  \w   -122.00 -95.00   0.50    1.85    --  -79.50 -65.00 -92.33   54
  34  \w    -90.00 -36.00   0.50    1.85    --  -79.50 103.00-146.13  108
  35  \w     40.00  86.00   0.50    1.85    --   80.41 -95.00 150.00   92
  36  \w     35.00  97.00   0.50    1.85    --   80.41-112.00 -30.00  124
  37  \w     35.00  97.00   0.50    1.85    --   80.41-112.00 -90.00  124
  38  \w     35.00  97.00   0.50    1.85    --   80.41-112.00  30.00  124
  39  \w     40.00  86.00   0.50    1.85    --   80.41 -95.00-180.00   92
  40  \w     35.00  97.00   0.50    1.85    --   80.41-112.00-180.00  124
  41  \w     40.00  86.00   0.50    1.85    --   80.41 -95.00  30.00   92
  42  \w     35.00  97.00   0.50    1.85    --   80.41-112.00-150.00  124
  43  \w     35.00  97.00   0.50    1.85    --   80.41-112.00 150.00  124
  44  \w     54.00 129.00   0.50    1.85    --   80.41  15.00  60.00  150
  45  \w     54.00 129.00   0.50    1.85    --   80.41  15.00  30.00  150
  46  \w     54.00 129.00   0.50    1.85    --   80.41  15.00-150.00  150
  47  \w     54.00 129.00   0.50    1.85    --   80.41  15.00   0.00  150
  48  \w     35.00  97.00   0.50    1.85    --   80.41-112.00 -60.00  124
  49  \w     40.00  86.00   0.50    1.85    --   80.41 -95.00 120.00   92
  50  \w     35.00  97.00   0.50    1.85    --   80.41-112.00  60.00  124
  51  \w     35.00  97.00   0.50    1.85    --   80.41-112.00-120.00  124
  52  \w     35.00  97.00   0.50    1.85    --   80.41-112.00 120.00  124
  53  \w     37.00  97.00   0.50    1.85    --   82.00-111.00  66.64  120
  54  \w     40.00  94.00   0.50    1.85    --   83.50-103.00 -17.67  108
  55  \w     43.00  89.00   0.50    1.85    --   83.50 -95.00-143.08   92
  56  \w     41.00  93.00   0.50    1.85    --   83.50-101.00  92.18  104
  57  \w     70.00 132.00   0.50    1.85    --   83.50  18.00 170.13  124
  58  \w     40.00 109.00   0.50    1.85    --   83.50-139.00 -73.13  138
  59  \w     37.00  97.00   0.50    1.85    --   83.50-115.00-101.97  120
  60  \w     38.00 102.00   0.50    1.85    --   83.50-131.00  94.50  128
  61  \w     76.00 133.00   0.50    1.85    --   83.50  21.00 -45.71  114
  62  \w     38.00 103.00   0.50    1.85    --   83.50-132.00 110.38  130
  63  \w     38.00 102.00   0.50    1.85    --   83.50-128.00 125.24  128
  64  \w     37.00 101.00   0.50    1.85    --   83.50-125.00 -24.09  128
  65  \w     91.00 128.00   0.50    1.85    --   83.50 138.00-115.18   74
  66  \w     38.00 102.00   0.50    1.85    --   83.50-131.00  32.28  128
  67  \w     99.00 131.00   0.50    1.85    --   83.50  45.00-133.26   64
  68  \w     44.00  87.00   0.50    1.85    --   83.50 -93.00-170.47   86
  69  \w    100.00 131.00   0.50    1.85    --   83.50  49.00-106.26   62
  70  \w     95.00 134.00   0.50    1.85    --   83.50  28.00-149.97   78
  71  \w     94.00 129.00   0.50    1.85    --   83.50 130.00-145.97   70
  72  \w     99.00 129.00   0.50    1.85    --   83.50  55.00 -47.27   60
  73  \w     94.00 134.00   0.50    1.85    --   83.50  27.00  79.07   80
  74  \w    100.00 126.00   0.50    1.85    --   83.50  64.00 110.61   52
  75  \w     19.00  46.00   0.50    1.85    --    6.00  63.00-110.31   54
  76  \w     28.00  54.00   0.50    1.85    --   14.00  61.00  94.66   52
  77  \w     32.00  60.00   0.50    1.85    --   18.00  59.00  -0.85   56
  78  \w     32.00  60.00   0.50    1.85    --   18.00  59.00 -60.20   56
  79  \w     32.00  60.00   0.50    1.85    --   18.00  59.00 143.92   56
  80  \w     50.00  80.00   0.50    1.85    --   34.00  52.00  18.00   60
  81  \w     58.00  88.00   0.50    1.85    --   42.00  52.00-117.03   60
  82  \w   -119.00 -88.00   0.50    1.85    --  -74.00 -57.00  95.11   62
  83  \w   -119.00 -88.00   0.50    1.85    --  -74.00 -58.00-132.70   62
  84  \w   -119.00 -88.00   0.50    1.85    --  -74.00 -58.00-159.69   62
  85  \w   -119.00 -88.00   0.50    1.85    --  -74.00 -58.00 136.16   62
  86  \w   -118.00 -88.00   0.50    1.85    --  -74.00 -59.00  88.31   60
  87  \w   -118.00 -88.00   0.50    1.85    --  -74.00 -60.00 146.03   60
  88  \w   -119.00 -88.00   0.50    1.85    --  -74.00 -57.00 -31.91   62
  89  \w   -119.00 -89.00   0.50    1.85    --  -74.00 -56.00-105.67   60
  90  \w   -118.00 -88.00   0.50    1.85    --  -74.00 -59.00  27.13   60
  91  \w   -119.00 -89.00   0.50    1.85    --  -74.00 -56.00 -16.58   60
  92  \w   -118.00 -88.00   0.50    1.85    --  -74.00 -61.00   3.88   60
  93  \w   -123.00 -92.00   0.50    1.85    --  -78.00 -57.00 172.91   62
  94  \w   -122.00 -92.00   0.50    1.85    --  -78.00 -59.00 128.79   60
  95  \w   -122.00 -91.00   0.50    1.85    --  -78.00 -61.00-115.21   62
  96  \w   -121.00 -91.00   0.50    1.85    --  -78.00 -62.00  50.71   60
  97  \w   -121.00 -91.00   0.50    1.85    --  -78.00 -62.00  42.28   60
  98  \w   -123.00 -93.00   0.50    1.85    --  -79.50 -61.00 -61.97   60
  99  \w   -123.00 -93.00   0.50    1.85    --  -79.50 -62.00 -37.02   60
 100  \w   -123.00 -93.00   0.50    1.85    --  -79.50 -63.00  66.01   60
 101  \w   -123.00 -84.00   0.50    1.85    --  -79.50-139.00-175.26   78
 102  \w   -123.00 -93.00   0.50    1.85    --  -79.50 -63.00  24.97   60
 103  \w   -126.00 -93.00   0.50    1.85    --  -79.50-121.00  60.33   66
 104  \w   -126.00 -93.00   0.50    1.85    --  -79.50-121.00  -6.01   66
 105  \w   -125.00 -98.00   0.50    1.85    --  -79.50-111.00 136.31   54
 106  \w   -123.00 -93.00   0.50    1.85    --  -79.50 -63.00 -83.19   60
 107  \w   -123.00 -93.00   0.50    1.85    --  -79.50 -63.00 163.65   60

;
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            203916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.708
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.922
_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            'clear colourless'
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         10479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0409P)^2^+3.2101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9492
_reflns_number_total             10479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03467d2.cif
_cod_data_source_block           2-CuPCy3
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7131914
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              3343
_shelx_hkl_checksum              25655