<i>endo</i>-Bicyclo[2.2.1]hept-2-ene-5,6-dimethylene bis(<i>p</i>-toluenesulfonate)
Xiao-Hong Ren; Lili Sun; Wu Li; Yu-Ping Guo; Fei Wang; Acta Crystallographica Section E 62 (2006) o3660–o3661; doi:10.1107/S1600536806029333

data_2210219
_publ_section_title
;
 <i>endo</i>-Bicyclo[2.2.1]hept-2-ene-5,6-dimethylene
 bis(<i>p</i>-toluenesulfonate)
;
_journal_coeditor_code           FB2010
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3660
_journal_page_last               o3661
_journal_paper_doi               10.1107/S1600536806029333
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H26 O6 S2'
_chemical_formula_moiety         'C23 H26 O6 S2'
_chemical_formula_sum            'C23 H26 O6 S2'
_chemical_formula_weight         462.56
_chemical_melting_point          359
_chemical_name_common
;
5,6-bis(endo-p-toluenesulfonyloxymethyl)-bicyclo[2.2.1]hept-2-ene
;
_chemical_name_systematic
;
endo-Bicyclo[2.2.1]hept-2-ene-5,6-dimethylene bis(p-toluenesulfonate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 115.424(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.139(2)
_cell_length_b                   13.186(2)
_cell_length_c                   13.626(2)
_cell_measurement_reflns_used    3103
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      23.06
_cell_measurement_theta_min      2.26
_cell_volume                     2294.4(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12673
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.9268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    76
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.5608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                2574
_reflns_number_total             4679
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fb2010.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2210219
_cod_database_fobs_code          2210219