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_7132498
_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 Ag B2 Cl N5, 1.5(C6 H6)'
_chemical_formula_sum            'C60 H74 Ag B2 Cl N5'
_chemical_formula_weight         1030.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_audit_update_record
;
2023-08-23 deposited with the CCDC.	2023-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.88640(10)
_cell_length_b                   12.68250(10)
_cell_length_c                   36.1057(2)
_cell_measurement_reflns_used    58340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0810
_cell_measurement_theta_min      2.4510
_cell_volume                     10887.08(12)
_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      99.99(11)
_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):
 
   # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
 --------------------------------------------------------------------------
   1  \w    -31.00  -5.00   0.50    1.21    --  -10.00 113.00 145.04   52
   2  \w    -95.00 -60.00   0.50    1.21    --  -46.00 -49.00 -80.57   70
   3  \w   -102.00 -67.00   0.50    1.21    --  -54.00 -52.00 135.19   70
   4  \w   -104.00 -66.00   0.50    1.21    --  -54.00 -43.00-171.80   76
   5  \w     16.00  66.00   0.50    1.21    --   58.71 -95.00  90.00  100
   6  \w   -110.00 -75.00   0.50    1.21    --  -62.00 -51.00 159.87   70
   7  \w   -115.00 -80.00   0.50    1.21    --  -66.00 -47.00-101.45   70
   8  \w     29.00  79.00   0.50    1.21    --   71.32 -95.00 -90.00  100
   9  \w    -96.00 -28.00   0.50    1.21    --  -76.33 112.00   0.00  136
  10  \w   -100.00 -32.00   0.50    1.21    --  -79.50 113.00 -51.92  136
  11  \w    -99.00 -44.00   0.50    1.21    --  -79.50 122.00 160.79  110
  12  \w   -127.00-101.00   0.50    1.21    --  -79.50-120.00 -31.26   52
  13  \w   -126.00-100.00   0.50    1.21    --  -79.50 -52.00 140.22   52
  14  \w   -125.00 -97.00   0.50    1.21    --  -79.50-116.00 165.77   56
  15  \w   -119.00 -94.00   0.50    1.21    --  -79.50-119.00 -74.23   50
  16  \w   -126.00-101.00   0.50    1.21    --  -79.50-119.00 -91.06   50
  17  \w   -128.00-103.00   0.50    1.21    --  -79.50 -50.00-108.75   50
  18  \w   -102.00 -38.00   0.50    1.21    --  -79.50 127.00  67.19  128
  19  \w   -126.00 -98.00   0.50    1.21    --  -79.50-115.00-135.90   56
  20  \w   -121.00 -96.00   0.50    1.21    --  -79.50 -65.00-161.29   50
  21  \w     94.00 119.00   0.50    1.21    --   82.00  59.00  16.34   50
  22  \w     36.00  61.00   0.50    1.21    --   82.37-112.00 -60.00   50
  23  \w     40.00  66.00   0.50    1.21    --   82.37-112.00 -30.00   52
  24  \w     74.00 100.00   0.50    1.21    --   82.37-112.00  30.00   52
  25  \w     93.00 127.00   0.50    1.21    --   82.37  15.00-180.00   68
  26  \w    102.00 127.00   0.50    1.21    --   82.37  15.00  90.00   50
  27  \w     43.00  68.00   0.50    1.21    --   82.37 -95.00   0.00   50
  28  \w     75.00 100.00   0.50    1.21    --   82.37-112.00-180.00   50
  29  \w     35.00  61.00   0.50    1.21    --   82.37-112.00-120.00   52
  30  \w     75.00 100.00   0.50    1.21    --   82.37-112.00   0.00   50
  31  \w     36.00  62.00   0.50    1.21    --   82.37-112.00-180.00   52
  32  \w     74.00 100.00   0.50    1.21    --   82.37-112.00 -30.00   52
  33  \w     53.00  81.00   0.50    1.21    --   85.25 -85.00 -66.46   56
  34  \w     44.00  69.00   0.50    1.21    --   85.25 -73.00 175.98   50
  35  \w     37.00  83.00   0.50    1.21    --   85.25-125.00 130.27   92
  36  \w     38.00  64.00   0.50    1.21    --   85.25-134.00 -22.43   52
  37  \w     56.00  82.00   0.50    1.21    --   85.25 -90.00  18.04   52
  38  \w     43.00  68.00   0.50    1.21    --   85.25 -97.00 -60.61   50
  39  \w    101.00 135.00   0.50    1.21    --   85.25  36.00  13.72   68
  40  \w     72.00  98.00   0.50    1.21    --   85.25-105.00-174.53   52
  41  \w     39.00  64.00   0.50    1.21    --   85.25-105.00-174.53   50
  42  \w    102.00 128.00   0.50    1.21    --   85.25  58.00 158.10   52
  43  \w     59.00 101.00   0.50    1.21    --   85.25-118.00 155.96   84
  44  \w     38.00  63.00   0.50    1.21    --   85.25-119.00 -77.57   50
  45  \w     98.00 123.00   0.50    1.21    --   85.25  62.00  99.17   50
  46  \w     40.00  86.00   0.50    1.21    --   85.25-140.00  17.36   92
  47  \w     92.00 137.00   0.50    1.21    --   85.25  27.00 -13.38   90
  48  \w     39.00  76.00   0.50    1.21    --   85.25-138.00 -55.01   74
  49  \w     38.00  73.00   0.50    1.21    --   85.25-129.00  93.69   70
  50  \w     61.00  98.00   0.50    1.21    --   85.25-105.00-140.15   74
  51  \w    104.00 137.00   0.50    1.21    --   85.25  34.00-131.91   66
  52  \w    109.00 135.00   0.50    1.21    --   85.25  31.00  35.56   52
  53  \w     58.00  99.00   0.50    1.21    --   85.25-108.00  82.69   82
  54  \w     98.00 126.00   0.50    1.21    --   85.25  41.00 139.14   56
  55  \w     38.00  77.00   0.50    1.21    --   85.25-131.00   1.78   78
  56  \w    106.00 131.00   0.50    1.21    --   85.25  45.00 178.82   50
  57  \w     54.00  97.00   0.50    1.21    --   85.25-101.00-172.12   86
  58  \w    106.00 132.00   0.50    1.21    --   85.25  45.00  72.13   52
  59  \w    101.00 132.00   0.50    1.21    --   85.25 118.00-139.11   62
  60  \w     43.00  99.00   0.50    1.21    --   85.25-110.00 161.77  112
  61  \w     46.00  71.00   0.50    1.21    --   85.25 -81.00 147.53   50
  62  \w     43.00  99.00   0.50    1.21    --   85.25-107.00  53.38  112
  63  \w    104.00 130.00   0.50    1.21    --   85.25  30.00-143.51   52
  64  \w    110.00 136.00   0.50    1.21    --   85.25  43.00 107.35   52
  65  \w     99.00 125.00   0.50    1.21    --   85.25  51.00  83.22   52
  66  \w     40.00 109.00   0.50    1.21    --   85.25-140.00  59.93  138
  67  \w    102.00 127.00   0.50    1.21    --   85.25 115.00 -16.52   50
  68  \w     46.00  71.00   0.50    1.21    --   85.25 -74.00-130.81   50
  69  \w     36.00  95.00   0.50    1.21    --   85.25-119.00   9.26  118
  70  \w     43.00  99.00   0.50    1.21    --   85.25-106.00-108.64  112
  71  \w     61.00  96.00   0.50    1.21    --   85.25-103.00 -84.30   70
  72  \w     75.00 100.00   0.50    1.21    --   85.25-111.00 -44.56   50
  73  \w     72.00  99.00   0.50    1.21    --   85.25-106.00 107.11   54

;
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            112988
_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         75.496
_diffrn_reflns_theta_min         2.459
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    3.735
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.915
_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            yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         11200
_refine_ls_number_restraints     2056
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+22.7070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10438
_reflns_number_total             11200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05477b2.cif
_cod_data_source_block           DaDu008_DaDu_a
_cod_depositor_comments
'Adding full bibliography for 7132494--7132501.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7132498
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.807
_shelx_res_checksum              58542
_shelx_hkl_checksum              6244