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_7132499
_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_absolute_configuration unk
_chemical_formula_moiety         '2(C51 H65 Au B2 Cl2 Cu N5), 3(C6 H6)'
_chemical_formula_sum            'C120 H148 Au2 B4 Cl4 Cu2 N10'
_chemical_formula_weight         2436.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-07
_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                 101.525(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.642(9)
_cell_length_b                   11.768(3)
_cell_length_c                   26.907(7)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.46
_cell_volume                     11058(5)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40B (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                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_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      -0,0084934
_diffrn_orient_matrix_UB_12      0,0704414
_diffrn_orient_matrix_UB_13      -0,0198700
_diffrn_orient_matrix_UB_21      0,0014445
_diffrn_orient_matrix_UB_22      0,0432876
_diffrn_orient_matrix_UB_23      0,0323085
_diffrn_orient_matrix_UB_31      0,0273073
_diffrn_orient_matrix_UB_32      0,0196194
_diffrn_orient_matrix_UB_33      0,0000570
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89055
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.937
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             4968
_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          0.290
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.249(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1411
_refine_ls_number_reflns         19946
_refine_ls_number_restraints     499
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0261P)^2^+41.2401P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                19271
_reflns_number_total             19946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05477b2.cif
_cod_data_source_block           test_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7132494--7132501.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7132499
_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   0.460
_shelx_estimated_absorpt_t_max   0.700
_shelx_res_checksum              30612
_shelx_hkl_checksum              56516