Stepwise and selective synthesis of chelating, multimetallic and mixed-metal π-diborene complexes.
Duwe, Dario; Saha, Koushik; Endres, Lukas; Brückner, Tobias; Dewhurst, Rian D.; Dietz, Maximilian; Radacki, Krzysztof; Fantuzzi, Felipe; Braunschweig, Holger; Chemical communications (Cambridge, England) 60 (2024) 1120–1123; doi:10.1039/d3cc05477b

data_7132496
_publ_section_title
;
 Stepwise and selective synthesis of chelating, multimetallic and
 mixed-metal &#x3c0;-diborene complexes.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1120
_journal_page_last               1123
_journal_paper_doi               10.1039/d3cc05477b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C51 H63 B2 Cl2 Cu2 N5'
_chemical_formula_sum            'C51 H63 B2 Cl2 Cu2 N5'
_chemical_formula_weight         965.66
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-01-27
_audit_creation_method           'CIF-fill 1.3q (K.Radacki, 2005-22)'
_audit_update_record
;
2023-08-23 deposited with the CCDC.	2023-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.1500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1438(2)
_cell_length_b                   11.81800(10)
_cell_length_c                   23.6127(2)
_cell_measurement_reflns_used    45797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.9330
_cell_measurement_theta_min      2.6260
_cell_volume                     4689.46(8)
_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 2014/5 (Sheldrick, 2014)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -126.00 -92.00   0.50    0.07    --  -79.50 -57.00 176.93   68
  2  \w   -120.00 -86.00   0.50    0.07    --  -74.00 -60.00 -88.02   68
  3  \w   -125.00 -91.00   0.50    0.07    --  -79.50 -60.00-108.84   68
  4  \w   -120.00 -86.00   0.50    0.07    --  -74.00 -59.00-104.13   68
  5  \w   -102.00 -67.00   0.50    0.07    --  -54.00 -52.00-179.03   70
  6  \w   -103.00 -68.00   0.50    0.07    --  -54.00 -50.00  29.92   70
  7  \w   -128.00 -93.00   0.50    0.07    --  -79.50 -50.00  39.52   70
  8  \w   -111.00 -76.00   0.50    0.07    --  -62.00 -50.00  82.29   70
  9  \w    -95.00 -60.00   0.50    0.07    --  -46.00 -47.00 142.43   70
 10  \w   -107.00 -72.00   0.50    0.07    --  -58.00 -50.00 117.90   70
 11  \w   -126.00 -88.00   0.50    0.07    --  -79.50-131.00 117.87   76
 12  \w   -126.00 -91.00   0.50    0.07    --  -79.50-124.00 -17.19   70
 13  \w   -126.00 -88.00   0.50    0.07    --  -79.50-130.00-130.58   76
 14  \w   -125.00 -94.00   0.50    0.07    --  -79.50-118.00-176.96   62
 15  \w    -92.00 -34.00   0.50    0.07    --  -79.50 108.00  62.91  116
 16  \w    -97.00 -33.00   0.50    0.07    --  -79.50 115.00 173.14  128
 17  \w    -97.00 -33.00   0.50    0.07    --  -79.50 115.00  -0.65  128
 18  \w    -97.00 -32.00   0.50    0.07    --  -78.00 114.00 -31.65  130
 19  \w    -97.00 -33.00   0.50    0.07    --  -79.50 115.00 -90.99  128
 20  \w     94.00 128.00   0.50    0.07    --   82.00  60.00 -28.86   68
 21  \w    103.00 135.00   0.50    0.07    --   85.25  42.00 -52.09   64
 22  \w     98.00 136.00   0.50    0.07    --   85.25  43.00-105.12   76
 23  \w     99.00 124.00   0.50    0.07    --   85.25  46.00 -70.02   50
 24  \w     81.00 111.00   0.50    0.07    --   82.28  15.00 -90.00   60
 25  \w    109.00 135.00   0.50    0.07    --   85.25  22.00 -61.55   52
 26  \w    102.00 129.00   0.50    0.07    --   82.28  15.00   0.00   54
 27  \w     72.00 112.00   0.50    0.07    --   82.28  15.00 120.00   80
 28  \w     97.00 122.00   0.50    0.07    --   85.25  56.00 146.95   50
 29  \w    104.00 137.00   0.50    0.07    --   85.25  37.00 162.33   66
 30  \w     46.00 133.00   0.50    0.07    --   82.28  15.00  30.00  174
 31  \w     97.00 129.00   0.50    0.07    --   82.28  15.00-120.00   64
 32  \w     48.00  75.00   0.50    0.07    --   85.25 -79.00 -83.02   54
 33  \w     35.00 101.00   0.50    0.07    --   82.00-128.00-147.62  132
 34  \w     52.00 107.00   0.50    0.07    --   85.25-138.00  12.17  110
 35  \w     41.00 101.00   0.50    0.07    --   85.25-126.00  33.09  120
 36  \w     38.00  99.00   0.50    0.07    --   85.25-127.00  78.38  122
 37  \w     39.00  65.00   0.50    0.07    --   85.25-125.00 166.78   52
 38  \w     39.00  70.00   0.50    0.07    --   85.25-139.00 157.63   62
 39  \w     75.00 101.00   0.50    0.07    --   85.25-139.00 157.63   52
 40  \w     48.00  97.00   0.50    0.07    --   85.25-116.00 155.64   98
 41  \w     37.00  93.00   0.50    0.07    --   82.28-112.00 120.00  112
 42  \w     37.00  62.00   0.50    0.07    --   82.28-112.00  90.00   50
 43  \w     47.00  92.00   0.50    0.07    --   82.28-112.00  30.00   90
 44  \w     37.00  93.00   0.50    0.07    --   82.28-112.00   0.00  112
 45  \w     38.00  85.00   0.50    0.07    --   85.25-120.00-138.16   94
 46  \w     37.00  69.00   0.50    0.07    --   82.28-112.00-120.00   64
 47  \w     41.00  67.00   0.50    0.07    --   85.25-109.00-109.66   52
 48  \w     45.00  92.00   0.50    0.07    --   85.25 -96.00-126.73   94
 49  \w     40.00  90.00   0.50    0.07    --   82.28 -95.00-180.00  100
 50  \w     40.00  90.00   0.50    0.07    --   82.28 -95.00 -90.00  100
 51  \w     50.00  92.00   0.50    0.07    --   85.25 -95.00-141.52   84
 52  \w     16.00  66.00   0.50    0.07    --   58.57 -95.00 -60.00  100
 53  \w     43.00  93.00   0.50    0.07    --   85.25-101.00  68.40  100
 54  \w     43.00  90.00   0.50    0.07    --   82.28 -95.00  90.00   94
 55  \w     56.00  93.00   0.50    0.07    --   85.25 -97.00 178.50   74
 56  \w     55.00  92.00   0.50    0.07    --   85.25 -95.00 161.25   74
 57  \w     46.00  71.00   0.50    0.07    --   85.25 -83.00 134.14   50
 58  \w    100.00 132.00   0.50    0.07    --   85.25 137.00 135.28   64
;
_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      0.0862556000
_diffrn_orient_matrix_UB_12      -0.0170236000
_diffrn_orient_matrix_UB_13      0.0045588000
_diffrn_orient_matrix_UB_21      0.0119363000
_diffrn_orient_matrix_UB_22      0.1292212000
_diffrn_orient_matrix_UB_23      0.0022534000
_diffrn_orient_matrix_UB_31      0.0286829000
_diffrn_orient_matrix_UB_32      -0.0030241000
_diffrn_orient_matrix_UB_33      0.0702480000
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            89216
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         2.629
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    2.473
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.593
_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            red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_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          0.310
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8530
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0566P)^2^+7.6209P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7458
_reflns_number_total             8530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05477b2.cif
_cod_data_source_block           DaDu055_DaDu_autored_a
_cod_depositor_comments
'Adding full bibliography for 7132494--7132501.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7132496
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.514
_shelx_estimated_absorpt_t_max   0.846
_shelx_res_checksum              40092
_shelx_hkl_checksum              2492