Synthesis, Structure, and Reaction of 1-Alkynyl(aryl)-λ3-bromanes
Masahito Ochiai; Yoshio Nishi; Satoru Goto; Motoo Shiro; Hermann J. Frohn; Journal of the American Chemical Society 125 (2003) 15304–15305; doi:10.1021/ja038777q

data_4114506
_publ_section_title
;
 Synthesis, Structure, and Reaction of 1-Alkynyl(aryl)-\l3-bromanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15304
_journal_page_last               15305
_journal_paper_doi               10.1021/ja038777q
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         '2(C13 H13 Br F3 +) , 2(B F4 -), C12 H24 O6'
_chemical_formula_sum            'C38 H50 B2 Br2 F14 O6'
_chemical_formula_weight         1050.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Wed Sep 24 08:58:42 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 92.31(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.295(9)
_cell_length_b                   17.76(1)
_cell_length_c                   12.43(1)
_cell_measurement_reflns_used    15145
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     2271(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXsan (MSC & Rigaku, 1999)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_refinement  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_solution    'PATTY (Beurskens, 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9954
_diffrn_measured_fraction_theta_max 0.9954
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18618
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1064.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4135
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.0046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                2604
_reflns_number_total             4135
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja038777qsi20030929_053457.cif
_cod_data_source_block           General
_cod_original_cell_volume        2270(3)
_cod_original_formula_sum        'C38 H50 B2 Br2 F14 O6 '
_cod_database_code               4114506