Geminal bis-borane formation by borane Lewis acid induced cyclopropyl rearrangement and its frustrated Lewis pair reaction with carbon dioxide.
Liu, Yun-Lin; Kehr, Gerald; Daniliuc, Constantin G.; Erker, Gerhard; Chemical science 8 (2017) 1097–1104; doi:10.1039/c6sc03468c

data_1544156
_publ_section_title
;
 Geminal bis-borane formation by borane Lewis acid induced cyclopropyl
 rearrangement and its frustrated Lewis pair reaction with carbon dioxide.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              1097
_journal_page_last               1104
_journal_paper_doi               10.1039/c6sc03468c
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C42 H35 B2 F20 O2 P'
_chemical_formula_weight         1004.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-08-01 deposited with the CCDC.
2016-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                89.016(3)
_cell_angle_beta                 87.552(3)
_cell_angle_gamma                73.104(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0179(3)
_cell_length_b                   11.2774(5)
_cell_length_c                   19.6359(11)
_cell_measurement_reflns_used    4122
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     2120.66(17)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.111
_diffrn_reflns_av_sigmaI/netI    0.1583
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            14903
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.9981
_exptl_absorpt_correction_T_min  0.9905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0022(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         7051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.2388
_refine_ls_R_factor_gt           0.1348
_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^)+(0.0000P)^2^+17.3742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2279
_refine_ls_wR_factor_ref         0.2746
_reflns_number_gt                3663
_reflns_number_total             7051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc03468c2.cif
_cod_data_source_block           erk8427
_cod_depositor_comments
;Adding full bibliography for 1544149--1544156.cif.

 Adding full bibliography for 1544149--1544156.cif.
;
_cod_original_cell_volume        2120.66(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1544156