Synthesis and reduction chemistry of mixed-Lewis-base-stabilised chloroborylenes
Arrowsmith, Merle; Schweizer, Julia I.; Heinz, Myron; Härterich, Marcel; Krummenacher, Ivo; Holthausen, Max C.; Braunschweig, Holger; Chemical Science 10 (2019) 5095–5103; doi:10.1039/C9SC01039D

data_1550854
_publ_section_title
;
 Synthesis and reduction chemistry of mixed-Lewis-base-stabilised
 chloroborylenes
;
_journal_issue                   19
_journal_name_full               'Chemical Science'
_journal_page_first              5095
_journal_page_last               5103
_journal_paper_doi               10.1039/C9SC01039D
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C40 H62 B Cl N2, C7 H8'
_chemical_formula_sum            'C47 H70 B Cl N2'
_chemical_formula_weight         709.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-25 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.624(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9399(13)
_cell_length_b                   14.8972(14)
_cell_length_c                   21.640(2)
_cell_measurement_reflns_used    4380
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.20
_cell_volume                     4124.3(7)
_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, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20660
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.071
_diffrn_reflns_theta_min         1.904
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8449
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SadAbs 2014/4 (Bruker AXS)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+4.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3003
_reflns_number_total             4085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01039d2.cif
_cod_data_source_block           final_a_CCDC3
_cod_original_cell_volume        4124.4(7)
_cod_database_code               1550854
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              79368