Cyclopropane formation under frustrated Lewis pair conditions.
Krupski, Sergei; Kehr, Gerald; Daniliuc, Constantin G.; Erker, Gerhard; Chemical communications (Cambridge, England) 52 (2016) 2695–2697; doi:10.1039/c5cc09585a

data_7118202
_publ_section_title
;
 Cyclopropane formation under frustrated Lewis pair conditions.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2695
_journal_page_last               2697
_journal_paper_doi               10.1039/c5cc09585a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C25 H6 B F15 O'
_chemical_formula_weight         618.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2015-08-19 deposited with the CCDC.
2015-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                110.4140(10)
_cell_angle_beta                 100.0700(10)
_cell_angle_gamma                97.1110(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4516(4)
_cell_length_b                   12.1427(5)
_cell_length_c                   12.2399(4)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.5170
_cell_measurement_theta_min      2.5324
_cell_volume                     1269.99(9)
_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 (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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0473
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            51651
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_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    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.113
_platon_squeeze_details
;
 A badly disordered half toluene molecule was found in the asymmetrical unit 
 and could not be satisfactorily refined. The program SQUEEZE (A. L. Spek
 J. Appl. Cryst., 2003, 36, 7-13) was therefore used to remove mathematically
 the effect of the solvent. 
 The quoted formula and derived parameters are not included the squeezed
 solvent molecule.
;
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0465P)^2^+0.6325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                4788
_reflns_number_total             5853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc09585a2.cif
_cod_data_source_block           erk7976
_cod_depositor_comments
'Adding full bibliography for 7118199--7118202.cif.'
_cod_database_code               7118202
_shelx_res_checksum              92353