Synthesis and fluxional behaviour of novel chloroborole dimers.
Zhang, Zuolun; Wang, Zheng; Haehnel, Martin; Eichhorn, Antonius; Edkins, Robert M.; Steffen, Andreas; Krueger, Anke; Lin, Zhenyang; Marder, Todd B.; Chemical communications (Cambridge, England) 52 (2016) 9707–9710; doi:10.1039/c6cc04831e

data_7124821
_publ_section_title
;
 Synthesis and fluxional behaviour of novel chloroborole dimers.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9707
_journal_page_last               9710
_journal_paper_doi               10.1039/c6cc04831e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C77 H66 B4 Cl6'
_chemical_formula_sum            'C77 H66 B4 Cl6'
_chemical_formula_weight         1247.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   iterative
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-30 deposited with the CCDC.
2016-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                68.0340(10)
_cell_angle_beta                 76.1090(10)
_cell_angle_gamma                68.5070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3724(3)
_cell_length_b                   16.2620(4)
_cell_length_c                   18.3411(5)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.60
_cell_volume                     3161.58(14)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            150442
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.206
_diffrn_source                   'rotating anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.793
_exptl_crystal_size_mid          0.610
_exptl_crystal_size_min          0.465
_refine_diff_density_max         0.982
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         12419
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0491P)^2^+2.1223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10609
_reflns_number_total             12419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04831e2.cif
_cod_data_source_block           MaHa066_multiscan2
_cod_database_code               7124821
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.866
_shelx_res_checksum              46367