A Cyclic Sulfate with a Seven-Membered Ring: 1,3,2-Dioxathiepane 2,2-Dioxide
Krüger, Carl; Kessler, Magnus; Six, Christian; Leitner, Walter; Acta Crystallographica Section C 54 (1998) 389–390; doi:10.1107/S010827019701634X

data_2007096
_publ_section_title
;
 A Cyclic Sulfate with a Seven-Membered Ring: 1,3,2-Dioxathiepane
 2,2-Dioxide
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              389
_journal_page_last               390
_journal_paper_doi               10.1107/S010827019701634X
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C4 H8 O4 S'
_chemical_formula_sum            'C4 H8 O4 S'
_chemical_formula_weight         152.16
_chemical_name_common            Tetramethylsulfate
_chemical_name_systematic
;
 1,3,2-Dioxathiepane, 2,2-dioxide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                92.328(8)
_cell_angle_beta                 96.772(11)
_cell_angle_gamma                99.011(11)
_cell_formula_units_Z            4
_cell_length_a                   6.4376(8)
_cell_length_b                   9.7440(9)
_cell_length_c                   10.8177(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.0
_cell_volume                     664.31(12)
_computing_data_collection       'CAD-4 Express Software (Enraf-Nonius, 1995)'
_computing_data_reduction        'DATAP (Coppens et al., 1965)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1983)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2940
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        9.1
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.019
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.047
_refine_ls_R_factor_all          0.081
_refine_ls_R_factor_obs          .042
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.1871P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.115
_refine_ls_wR_factor_obs         .096
_reflns_number_observed          1823
_reflns_number_total             2690
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            ka1250.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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.1871P] where P = (Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.1871P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2007096