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_7131915
_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         'C74 H62 B2 Cu2 N2, C6 H6'
_chemical_formula_sum            'C80 H68 B2 Cu2 N2'
_chemical_formula_weight         1206.06
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-06
_audit_creation_method           'CIF-fill 1.3q (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                 117.9850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4246(2)
_cell_length_b                   11.86240(10)
_cell_length_c                   24.9377(2)
_cell_measurement_reflns_used    112677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2560
_cell_measurement_theta_min      3.5290
_cell_volume                     6119.23(10)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_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 0.989
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     19.00  46.00   0.50    0.05    --    6.00  63.00  66.09   54
  2  \w     32.00  60.00   0.50    0.05    --   18.00  58.00 100.73   56
  3  \w     32.00  60.00   0.50    0.05    --   18.00  59.00 138.49   56
  4  \w     46.00  76.00   0.50    0.05    --   30.00  52.00 -34.38   60
  5  \w     28.00  54.00   0.50    0.05    --   14.00  61.00 -52.68   52
  6  \w     33.00  60.00   0.50    0.05    --   18.00  54.00-103.49   54
  7  \w     54.00  84.00   0.50    0.05    --   38.00  52.00-160.24   60
  8  \w     32.00  60.00   0.50    0.05    --   18.00  58.00-171.61   56
  9  \w     58.00  89.00   0.50    0.05    --   42.00  50.00  50.51   62
 10  \w     54.00  85.00   0.50    0.05    --   38.00  50.00 130.19   62
 11  \w     54.00 129.00   0.50    0.05    --   80.41  15.00-120.00  150
 12  \w     97.00 127.00   0.50    0.05    --   83.50  61.00 -73.93   60
 13  \w     54.00 129.00   0.50    0.05    --   80.41  15.00-150.00  150
 14  \w     54.00 129.00   0.50    0.05    --   80.41  15.00   0.00  150
 15  \w     99.00 130.00   0.50    0.05    --   83.50  52.00  22.25   62
 16  \w     54.00 129.00   0.50    0.05    --   80.41  15.00  60.00  150
 17  \w     54.00 129.00   0.50    0.05    --   80.41  15.00 150.00  150
 18  \w     69.00 132.00   0.50    0.05    --   83.50  17.00 109.59  126
 19  \w     44.00  70.00   0.50    0.05    --   83.50 -72.00 127.40   52
 20  \w     37.00 102.00   0.50    0.05    --   83.50-129.00 147.98  130
 21  \w     37.00 102.00   0.50    0.05    --   83.50-129.00 134.41  130
 22  \w     39.00 106.00   0.50    0.05    --   83.50-136.00  57.64  134
 23  \w     20.00  87.00   0.50    0.05    --   61.21-126.00 -30.00  134
 24  \w     37.00 102.00   0.50    0.05    --   83.50-129.00 -93.59  130
 25  \w     40.00 109.00   0.50    0.05    --   83.50-140.00-152.44  138
 26  \w     35.00  97.00   0.50    0.05    --   80.41-112.00-120.00  124
 27  \w     35.00  97.00   0.50    0.05    --   80.41-112.00 -90.00  124
 28  \w     35.00  97.00   0.50    0.05    --   80.41-112.00 -60.00  124
 29  \w     35.00  97.00   0.50    0.05    --   80.41-112.00   0.00  124
 30  \w     35.00  97.00   0.50    0.05    --   80.41-112.00  30.00  124
 31  \w     35.00  97.00   0.50    0.05    --   80.41-112.00 150.00  124
 32  \w     35.00  97.00   0.50    0.05    --   80.41-112.00  90.00  124
 33  \w     35.00  97.00   0.50    0.05    --   80.41-112.00  60.00  124
 34  \w     42.00  91.00   0.50    0.05    --   83.50 -98.00  99.21   98
 35  \w     40.00  95.00   0.50    0.05    --   83.50-104.00  36.45  110
 36  \w     40.00  86.00   0.50    0.05    --   80.41 -95.00  60.00   92
 37  \w     35.00  97.00   0.50    0.05    --   80.41-112.00 -30.00  124
 38  \w     40.00  86.00   0.50    0.05    --   80.41 -95.00 -60.00   92
 39  \w     40.00  86.00   0.50    0.05    --   80.41 -95.00 -90.00   92
 40  \w     40.00  86.00   0.50    0.05    --   80.41 -95.00-150.00   92
 41  \w     35.00  97.00   0.50    0.05    --   80.41-112.00-180.00  124
 42  \w     38.00  95.00   0.50    0.05    --   83.50-110.00-151.01  114
 43  \w     45.00  80.00   0.50    0.05    --   82.00 -85.00 -47.83   70
 44  \w     46.00  77.00   0.50    0.05    --   83.50 -77.00 116.82   62
 45  \w     21.00  67.00   0.50    0.05    --   61.21 -95.00 120.00   92
 46  \w     40.00  86.00   0.50    0.05    --   80.41 -95.00 150.00   92
 47  \w    -86.00 -38.00   0.50    0.05    --  -79.50  98.00 169.68   96
 48  \w    -39.00 -13.00   0.50    0.05    --  -14.00 125.00  67.99   52
 49  \w   -108.00 -35.00   0.50    0.05    --  -79.50 139.00 127.31  146
 50  \w    -96.00 -34.00   0.50    0.05    --  -79.50 111.00  49.89  124
 51  \w    -90.00 -36.00   0.50    0.05    --  -79.50 103.00 -47.72  108
 52  \w   -106.00 -35.00   0.50    0.05    --  -79.50 136.00 -87.56  142
 53  \w    -97.00 -33.00   0.50    0.05    --  -79.50 114.00-124.73  128
 54  \w   -124.00 -56.00   0.50    0.05    --  -76.35 -15.00-120.00  136
 55  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -63.00 -49.53   60
 56  \w   -122.00 -94.00   0.50    0.05    --  -79.50 -64.00 -30.82   56
 57  \w   -121.00 -91.00   0.50    0.05    --  -78.00 -62.00-118.74   60
 58  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -62.00 -23.35   60
 59  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -62.00  15.74   60
 60  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -62.00  36.12   60
 61  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -62.00 114.65   60
 62  \w   -122.00 -94.00   0.50    0.05    --  -79.50 -64.00 155.97   56
 63  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -61.00 129.18   60
 64  \w   -122.00 -91.00   0.50    0.05    --  -78.00 -61.00  88.40   62
 65  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -61.00  56.27   60
 66  \w   -118.00 -88.00   0.50    0.05    --  -74.00 -61.00  14.45   60
 67  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -60.00 -40.15   60
 68  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -61.00 -10.74   60
 69  \w   -124.00 -93.00   0.50    0.05    --  -79.50 -59.00   2.62   62
 70  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -60.00  82.81   60
 71  \w   -118.00 -88.00   0.50    0.05    --  -74.00 -59.00 154.43   60
 72  \w   -118.00 -88.00   0.50    0.05    --  -74.00 -59.00  73.89   60
 73  \w   -119.00 -88.00   0.50    0.05    --  -74.00 -58.00 112.06   62
 74  \w   -123.00 -93.00   0.50    0.05    --  -79.50 -60.00 -99.41   60
 75  \w   -119.00 -88.00   0.50    0.05    --  -74.00 -57.00 -97.48   62
 76  \w   -122.00 -91.00   0.50    0.05    --  -78.00 -61.00-108.70   62
 77  \w   -122.00 -92.00   0.50    0.05    --  -78.00 -59.00-139.90   60
 78  \w   -124.00 -94.00   0.50    0.05    --  -79.50 -58.00-148.50   60
 79  \w   -119.00 -88.00   0.50    0.05    --  -74.00 -57.00-159.94   62
 80  \w   -122.00 -91.00   0.50    0.05    --  -78.00 -61.00-156.91   62
 81  \w   -123.00 -92.00   0.50    0.05    --  -78.00 -57.00 -72.86   62
 82  \w   -119.00 -89.00   0.50    0.05    --  -74.00 -56.00 -53.55   60
 83  \w   -125.00 -95.00   0.50    0.05    --  -79.50 -54.00-140.87   60
 84  \w   -120.00 -89.00   0.50    0.05    --  -74.00 -54.00 -47.96   62
 85  \w   -124.00 -94.00   0.50    0.05    --  -79.50 -57.00  65.34   60
 86  \w   -119.00 -89.00   0.50    0.05    --  -74.00 -56.00  95.65   60
 87  \w   -119.00 -89.00   0.50    0.05    --  -74.00 -55.00 125.62   60
 88  \w   -125.00 -94.00   0.50    0.05    --  -79.50 -53.00 160.02   62
 89  \w   -126.00 -95.00   0.50    0.05    --  -79.50 -51.00 163.53   62
 90  \w   -124.00 -93.00   0.50    0.05    --  -78.00 -52.00  84.81   62
 91  \w   -109.00 -78.00   0.50    0.05    --  -62.00 -50.00 127.94   62
 92  \w   -104.00 -74.00   0.50    0.05    --  -58.00 -51.00 166.71   60
 93  \w   -126.00 -96.00   0.50    0.05    --  -79.50 -49.00  34.09   60
 94  \w   -100.00 -69.00   0.50    0.05    --  -54.00 -52.00 -18.97   62
 95  \w   -108.00 -78.00   0.50    0.05    --  -62.00 -51.00 -35.61   60
 96  \w   -104.00 -74.00   0.50    0.05    --  -58.00 -51.00 -93.64   60
 97  \w   -128.00 -94.00   0.50    0.05    --  -79.50 -41.00 -44.83   68
 98  \w   -105.00 -74.00   0.50    0.05    --  -58.00 -48.00-117.76   62
 99  \w    -95.00 -60.00   0.50    0.05    --  -46.00 -38.00-178.08   70
 100  \w   -129.00 -92.00   0.50    0.05    --  -79.50 -33.00-143.39   74
 101  \w    -73.00 -42.00   0.50    0.05    --  -26.00 -47.00 -28.48   62
 102  \w   -128.00 -94.00   0.50    0.05    --  -79.50 -42.00  96.02   68
 103  \w   -127.00 -95.00   0.50    0.05    --  -79.50 -48.00 173.12   64
 104  \w   -123.00 -84.00   0.50    0.05    --  -79.50-139.00  35.25   78
 105  \w   -124.00 -86.00   0.50    0.05    --  -79.50-135.00 155.55   76
 106  \w   -124.00 -86.00   0.50    0.05    --  -79.50-135.00 -55.54   76
 107  \w   -126.00 -93.00   0.50    0.05    --  -79.50-120.00 -90.00   66
 108  \w   -126.00 -90.00   0.50    0.05    --  -79.50-126.00-171.98   72
 109  \w   -124.00 -84.00   0.50    0.05    --  -79.50-138.00-132.83   80
 110  \w   -125.00 -87.00   0.50    0.05    --  -79.50-132.00 -94.97   76
 111  \w   -125.00 -98.00   0.50    0.05    --  -79.50-111.00 -63.25   54
 112  \w   -126.00 -94.00   0.50    0.05    --  -79.50-118.00 -24.97   64
 113  \w   -126.00 -94.00   0.50    0.05    --  -79.50-119.00  30.64   64
 114  \w   -126.00 -94.00   0.50    0.05    --  -79.50-119.00  96.84   64
 115  \w   -126.00 -90.00   0.50    0.05    --  -79.50-126.00 122.36   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0298388000
_diffrn_orient_matrix_UB_12      0.1079686000
_diffrn_orient_matrix_UB_13      0.0106896000
_diffrn_orient_matrix_UB_21      0.0027256000
_diffrn_orient_matrix_UB_22      -0.0527038000
_diffrn_orient_matrix_UB_23      0.0576162000
_diffrn_orient_matrix_UB_31      0.0681385000
_diffrn_orient_matrix_UB_32      0.0494294000
_diffrn_orient_matrix_UB_33      0.0381954000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            248538
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.712
_diffrn_reflns_theta_min         3.554
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.579
_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    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_preparation
;
 Crystals were grown from saturated solution. For data collection the crystal 
 was immersed in a film of perfluoropolyether oil, mounted on a polyimide 
 loop and transferred to stream of cold nitrogen (Oxford Cryostream 800).
;
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         12578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0536P)^2^+3.7711P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11084
_reflns_number_total             12578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03467d2.cif
_cod_data_source_block           '[2-Cu]2'
_cod_original_cell_volume        6119.22(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7131915
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              94443
_shelx_hkl_checksum              68091