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_7132497
_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 H65 B2 Cl Cu N5'
_chemical_formula_sum            'C51 H65 B2 Cl Cu N5'
_chemical_formula_weight         868.69
_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             2023-01-26
_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                 101.3180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.70400(10)
_cell_length_b                   13.75780(10)
_cell_length_c                   24.4253(2)
_cell_measurement_reflns_used    50129
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.9780
_cell_measurement_theta_min      3.6650
_cell_volume                     4515.52(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     46.00  73.00   0.50    0.09    --   85.25-126.00-163.45   54
  2  \w     39.00  65.00   0.50    0.09    --   85.25-138.00-119.57   52
  3  \w     38.00  76.00   0.50    0.09    --   85.25-130.00 -52.62   76
  4  \w     72.00  98.00   0.50    0.09    --   85.25-117.00-132.49   52
  5  \w     40.00 101.00   0.50    0.09    --   85.25-125.00 -16.23  122
  6  \w     56.00  96.00   0.50    0.09    --   85.25-116.00 -61.33   80
  7  \w     65.00  99.00   0.50    0.09    --   85.25-128.00  65.99   68
  8  \w     46.00  72.00   0.50    0.09    --   85.25-140.00 140.24   52
  9  \w     50.00 100.00   0.50    0.09    --   85.25-126.00 147.75  100
 10  \w     71.00  97.00   0.50    0.09    --   85.25-115.00 100.10   52
 11  \w     40.00  66.00   0.50    0.09    --   85.25-115.00 100.10   52
 12  \w     24.00  53.00   0.50    0.09    --   58.57-103.00   3.00   58
 13  \w     40.00  84.00   0.50    0.09    --   85.25-110.00  -3.85   88
 14  \w     46.00  92.00   0.50    0.09    --   85.25-111.00-133.07   92
 15  \w     43.00  89.00   0.50    0.09    --   85.25-106.00-103.14   92
 16  \w     68.00  93.00   0.50    0.09    --   85.25-106.00   4.07   50
 17  \w     41.00  66.00   0.50    0.09    --   82.28-103.00   3.00   50
 18  \w     60.00  93.00   0.50    0.09    --   85.25 -98.00-108.27   66
 19  \w     31.00  56.00   0.50    0.09    --   71.34-103.00   3.00   50
 20  \w     65.00  91.00   0.50    0.09    --   85.25-100.00 131.57   52
 21  \w     41.00  66.00   0.50    0.09    --   85.25-103.00 144.98   50
 22  \w     44.00  93.00   0.50    0.09    --   85.25 -98.00 151.27   98
 23  \w     42.00  93.00   0.50    0.09    --   85.25 -97.00  98.14  102
 24  \w     40.00  66.00   0.50    0.09    --   82.28 -95.00 -30.00   52
 25  \w     55.00  93.00   0.50    0.09    --   85.25 -97.00-170.23   76
 26  \w     63.00  89.00   0.50    0.09    --   82.28 -95.00-180.00   52
 27  \w     63.00  89.00   0.50    0.09    --   82.28 -95.00-150.00   52
 28  \w     33.00  59.00   0.50    0.09    --   58.57 -95.00-180.00   52
 29  \w     64.00  90.00   0.50    0.09    --   82.28 -95.00  30.00   52
 30  \w     46.00  82.00   0.50    0.09    --   85.25 -87.00  40.43   72
 31  \w     31.00  57.00   0.50    0.09    --   71.34 -95.00  90.00   52
 32  \w     46.00  71.00   0.50    0.09    --   85.25 -87.00-125.09   50
 33  \w     46.00  71.00   0.50    0.09    --   85.25 -86.00 -72.47   50
 34  \w     54.00  80.00   0.50    0.09    --   85.25 -87.00  -2.45   52
 35  \w     65.00  91.00   0.50    0.09    --   85.25 -94.00 158.33   52
 36  \w     45.00  75.00   0.50    0.09    --   85.25 -75.00 132.63   60
 37  \w     46.00  71.00   0.50    0.09    --   85.25 -79.00  49.13   50
 38  \w     46.00  71.00   0.50    0.09    --   85.25 -77.00 -16.40   50
 39  \w     54.00  80.00   0.50    0.09    --   85.25 -79.00-164.81   52
 40  \w     98.00 130.00   0.50    0.09    --   85.25 122.00  14.00   64
 41  \w    103.00 129.00   0.50    0.09    --   85.25 117.00 175.69   52
 42  \w     75.00 123.00   0.50    0.09    --   85.25  11.00  -7.28   96
 43  \w     99.00 124.00   0.50    0.09    --   85.25  63.00 -80.10   50
 44  \w     98.00 127.00   0.50    0.09    --   85.25  59.00 -92.32   58
 45  \w     97.00 122.00   0.50    0.09    --   85.25  56.00-111.50   50
 46  \w    102.00 127.00   0.50    0.09    --   85.25  58.00  19.20   50
 47  \w     99.00 124.00   0.50    0.09    --   85.25  49.00  -4.68   50
 48  \w     98.00 125.00   0.50    0.09    --   85.25  58.00  13.41   54
 49  \w    108.00 134.00   0.50    0.09    --   85.25  52.00  47.32   52
 50  \w     97.00 122.00   0.50    0.09    --   85.25  59.00 173.00   50
 51  \w     90.00 135.00   0.50    0.09    --   85.25  19.00 162.26   90
 52  \w     99.00 133.00   0.50    0.09    --   85.25  48.00 161.82   68
 53  \w     47.00  73.00   0.50    0.09    --   82.28  15.00  30.00   52
 54  \w     61.00  91.00   0.50    0.09    --   82.28  15.00 -60.00   60
 55  \w     96.00 122.00   0.50    0.09    --   82.28  15.00 -60.00   52
 56  \w    105.00 131.00   0.50    0.09    --   85.25  40.00 -45.54   52
 57  \w    103.00 132.00   0.50    0.09    --   82.28  15.00   0.00   58
 58  \w     75.00 101.00   0.50    0.09    --   82.28  15.00  30.00   52
 59  \w     61.00 121.00   0.50    0.09    --   85.25  12.00  72.59  120
 60  \w     47.00  79.00   0.50    0.09    --   82.28  15.00   0.00   64
 61  \w     60.00 128.00   0.50    0.09    --   85.25  12.00 151.69  136
 62  \w     97.00 123.00   0.50    0.09    --   82.28  15.00-120.00   52
 63  \w    109.00 135.00   0.50    0.09    --   85.25  43.00-158.39   52
 64  \w    108.00 133.00   0.50    0.09    --   82.28  15.00-150.00   50
 65  \w    -97.00 -38.00   0.50    0.09    --  -79.50 115.00-169.99  118
 66  \w    -97.00 -33.00   0.50    0.09    --  -78.00 114.00 -14.88  128
 67  \w    -92.00 -36.00   0.50    0.09    --  -79.50 104.00 -80.51  112
 68  \w    -52.00 -15.00   0.50    0.09    --  -60.16 103.00 105.00   74
 69  \w    -86.00 -46.00   0.50    0.09    --  -76.35 103.00 105.00   80
 70  \w    -78.00 -53.00   0.50    0.09    --  -69.76 103.00 105.00   50
 71  \w   -123.00 -98.00   0.50    0.09    --  -79.50 -66.00  21.18   50
 72  \w   -124.00 -99.00   0.50    0.09    --  -79.50 -64.00 -82.87   50
 73  \w   -124.00 -93.00   0.50    0.09    --  -79.50 -60.00 -43.97   62
 74  \w   -110.00 -76.00   0.50    0.09    --  -62.00 -50.00-166.15   68
 75  \w   -123.00 -98.00   0.50    0.09    --  -79.50 -66.00  -9.36   50
 76  \w   -123.00 -93.00   0.50    0.09    --  -79.50 -62.00  46.39   60
 77  \w    -93.00 -59.00   0.50    0.09    --  -46.00 -51.00 133.48   68
 78  \w   -104.00 -73.00   0.50    0.09    --  -58.00 -50.00  84.74   62
 79  \w   -114.00 -80.00   0.50    0.09    --  -66.00 -50.00  56.21   68
 80  \w   -107.00 -81.00   0.50    0.09    --  -58.00 -50.00 -99.54   52
 81  \w   -123.00 -97.00   0.50    0.09    --  -79.50 -51.00  91.23   52
 82  \w   -128.00 -93.00   0.50    0.09    --  -79.50 -40.00 166.30   70
 83  \w   -125.00 -91.00   0.50    0.09    --  -79.50-131.00 103.39   68
;
_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      -0.0699535000
_diffrn_orient_matrix_UB_12      0.0431892000
_diffrn_orient_matrix_UB_13      0.0360017000
_diffrn_orient_matrix_UB_21      0.0876049000
_diffrn_orient_matrix_UB_22      0.0064670000
_diffrn_orient_matrix_UB_23      0.0501688000
_diffrn_orient_matrix_UB_31      0.0237623000
_diffrn_orient_matrix_UB_32      0.1030762000
_diffrn_orient_matrix_UB_33      -0.0181589000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            101889
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.328
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.721
_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    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_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          0.250
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+3.1056P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8348
_reflns_number_total             9291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05477b2.cif
_cod_data_source_block           DaDu052_DaDu_autored_a
_cod_depositor_comments
'Adding full bibliography for 7132494--7132501.cif.'
_cod_original_cell_volume        4515.51(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7132497
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.701
_shelx_estimated_absorpt_t_max   0.874
_shelx_res_checksum              68252
_shelx_hkl_checksum              83118