B(C6F5)3 promoted cyclisation of internal propargyl esters: structural characterisation of 1,3-dioxolium compounds
Max M. Hansmann; Rebecca L. Melen; Frank Rominger; A. Stephen K. Hashmi; Douglas W. Stephan; Chem.Commun. 50 (2014) 7243–; doi:10.1039/C4CC01370K

data_7114624
_publ_section_title
;
 B(C6F5)3 promoted cyclisation of internal propargyl esters: structural
 characterisation of 1,3-dioxolium compounds
;
_journal_name_full               Chem.Commun.
_journal_page_first              7243
_journal_paper_doi               10.1039/C4CC01370K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C32.5 H17 B Cl F15 O2'
_chemical_formula_weight         770.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.896(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.732(2)
_cell_length_b                   20.805(4)
_cell_length_c                   13.426(2)
_cell_measurement_reflns_used    5306
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      2.24
_cell_volume                     3118.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16881
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         1.824
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.9050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         4974
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0596P)^2^+0.4493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3703
_reflns_number_total             4974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01370k2.cif
_cod_data_source_block           mah30_compound_5
_cod_original_formula_sum        'C32.50 H17 B Cl F15 O2'
_cod_database_code               7114624
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.981