3-(7,7-Dimethyl-2-oxobicyclo[2.2.1.]hept-1-ylmethanesulfonyloxy)-2-methyl-2-(toluene-4-sulfonyloxymethyl)propyl 4-chlorobenzoate
Linker, Manuela; Schürmann, Markus; Preut, Hans; Kreiser, Wolfgang; Acta Crystallographica Section E 58 (2002) o72–o73; doi:10.1107/S1600536801021420

data_2200847
_publ_section_title
;3-(7,7-Dimethyl-2-oxobicyclo[2.2.1.]hept-1-ylmethanesulfonyloxy)-2-methyl-2-(toluene-4-sulfonyloxymethyl)propyl
 4-chlorobenzoate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o72
_journal_page_last               o73
_journal_paper_doi               10.1107/S1600536801021420
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C29 H35 Cl O9 S2'
_chemical_formula_moiety         'C29 H35 Cl O9 S2'
_chemical_formula_sum            'C29 H35 Cl O9 S2'
_chemical_formula_weight         627.14
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.7225(14)
_cell_angle_beta                 85.0894(14)
_cell_angle_gamma                71.5179(14)
_cell_formula_units_Z            2
_cell_length_a                   8.5321(3)
_cell_length_b                   12.0941(4)
_cell_length_c                   16.6243(6)
_cell_measurement_reflns_used    15324
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.30
_cell_volume                     1535.38(9)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1997) and SCALEPACK
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2001)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full .973
_diffrn_measured_fraction_theta_max .973
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
323 frames via \w-rotation (\D\w=1\%) with 3 sets at
different \k-angles and two times 10 s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .043
_diffrn_reflns_av_sigmaI/netI    .1056
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15324
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.30
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          .6
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .35
_refine_diff_density_max         .153
_refine_diff_density_min         -.220
_refine_ls_abs_structure_details 'Flack (1983); 3632 Friedel pairs'
_refine_ls_abs_structure_Flack   -.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      .841
_refine_ls_R_factor_all          .1026
_refine_ls_R_factor_gt           .0379
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0209P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0682
_refine_ls_wR_factor_ref         .0782
_reflns_number_gt                5566
_reflns_number_total             10443
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6136.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2200847
_cod_database_fobs_code          2200847