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_7132495
_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         '2(C51 H65 Au B2 Br N5), C7 H8'
_chemical_formula_sum            'C109 H138 Au2 B4 Br2 N10'
_chemical_formula_weight         2185.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-07-13
_audit_creation_method           'CIF-fill 1.3e (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                 93.295(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.547(6)
_cell_length_b                   18.489(8)
_cell_length_c                   21.362(8)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.40
_cell_volume                     4947(4)
_computing_cell_refinement       'Saint+ ver. 8.40A (Bruker AXS)'
_computing_data_collection       'BIS 2011.8 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40A (Bruker AXS)'
_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                 CCD
_diffrn_detector_area_resol_mean 4.166
_diffrn_detector_type            Apex2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
;
 Sparks R.A., Computational Crystallography p1-18 (Clarendon Press, 1982)
;
_diffrn_orient_matrix_UB_11      -0,0721104
_diffrn_orient_matrix_UB_12      0,0171465
_diffrn_orient_matrix_UB_13      0,0110977
_diffrn_orient_matrix_UB_21      -0,0102706
_diffrn_orient_matrix_UB_22      -0,0455928
_diffrn_orient_matrix_UB_23      0,0241072
_diffrn_orient_matrix_UB_31      0,0326734
_diffrn_orient_matrix_UB_32      0,0235107
_diffrn_orient_matrix_UB_33      0,0386559
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73717
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.451
_diffrn_reflns_theta_max         25.451
_diffrn_reflns_theta_min         2.142
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Nonius FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.823
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_preparation
;
 Crystalls 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 
 700).
;
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.359
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.952
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         9121
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+12.8613P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7235
_reflns_number_total             9121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05477b2.cif
_cod_data_source_block           test_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7132494--7132501.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7132495
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
 Incident beam scaling, empirical absorption correction using spherical 
 harmonics, and outlier rejection was employed as implemented in SADABS. 
 Additional spherical absorption correction with mu*r value set to 0.2 was 
 applied.
;
_shelx_estimated_absorpt_t_min   0.338
_shelx_estimated_absorpt_t_max   0.476
_shelx_res_checksum              72967
_shelx_hkl_checksum              37877