Group 13 BN dehydrocoupling reagents, similar to transition metal catalysts but with unique reactivity
Hansmann, Max M.; Melen, Rebecca L.; Wright, Dominic S.; Chemical Science 2 (2011) 1554–; doi:10.1039/c1sc00154j

data_1515606
_publ_section_title
;
 Group 13 BN dehydrocoupling reagents, similar to transition metal
 catalysts but with unique reactivity
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              1554
_journal_paper_doi               10.1039/c1sc00154j
_journal_volume                  2
_journal_year                    2011
_chemical_absolute_configuration
;
2879 Friedel pairs were averaged for the refinement
;
_chemical_formula_moiety         'C33 H105 B4 N9 Si12, C4 H8 O'
_chemical_formula_sum            'C37 H113 B4 N9 O Si12'
_chemical_formula_weight         1080.68
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   29.3467(5)
_cell_length_b                   29.3467(5)
_cell_length_c                   14.9405(4)
_cell_measurement_reflns_used    13468
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      1.00
_cell_volume                     11143.3(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20082
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3564
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4976
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      2.191
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.1235
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3072
_refine_ls_wR_factor_ref         0.3335
_reflns_number_gt                3446
_reflns_number_total             4976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00154j.txt
_cod_data_source_block           dw1117
_cod_original_sg_symbol_H-M      P6(3)
_cod_database_code               1515606