PhSeOTf???Et3N??3HF and PhSeSbF6???Et3N??3HF as new PhSe???F equivalents in the fluoroselenenylation of acetylenes
Poleschner, Helmut; Seppelt, Konrad; Journal of the Chemical Society, Perkin Transactions 1  (2002) 2668–; doi:10.1039/b207886b

data_7204515
_publ_section_title
;
 PhSeOTf???Et3N??3HF and PhSeSbF6???Et3N??3HF as new PhSe???F
 equivalents in the fluoroselenenylation of acetylenes
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2668
_journal_paper_doi               10.1039/b207886b
_journal_year                    2002
_chemical_formula_sum            'C17 H23 F Se'
_chemical_formula_weight         325.31
_chemical_melting_point          326.0(4)
_chemical_name_common            (E)-1-Fluoro-2-phenylseleno-cycloundecene
_chemical_name_systematic        (E)-1-Fluoro-2-phenylseleno-cycloundecene
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.415(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0991(15)
_cell_length_b                   6.3581(14)
_cell_length_c                   16.766(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    123(2)
_cell_volume                     756.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart CCD 1000 TM'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9687
_diffrn_reflns_theta_full        30.93
_diffrn_reflns_theta_max         30.93
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    2.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_process_details
'Equilibration of symmetry equivalent reflections'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.753
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_coef       0.003(4)
_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   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4699
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1146P)^2^+0.8778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                4447
_reflns_number_total             4699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207886b.txt
_cod_data_source_block           cy11se
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '52.5 - 53.3 C' was changed to
'326.0(4)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        756.8(3)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7204515