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_1544155
_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            'C44 H39 B2 Cl4 F20 O2 P'
_chemical_formula_weight         1174.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-08-01 deposited with the CCDC.
2016-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8388(5)
_cell_length_b                   20.0253(6)
_cell_length_c                   18.7529(6)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.4973
_cell_measurement_theta_min      2.3101
_cell_volume                     4781.3(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;
APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)

;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            107562
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.29
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.630
_refine_diff_density_min         -1.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         10980
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0434P)^2^+6.0291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                8994
_reflns_number_total             10980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc03468c2.cif
_cod_data_source_block           erk8234
_cod_depositor_comments
;Adding full bibliography for 1544149--1544156.cif.

 Adding full bibliography for 1544149--1544156.cif.
;
_cod_database_code               1544155
_shelx_res_checksum              78784