1,5,7,11-Tetraoxaspiro[5.5]undecane, 3,9-Dimethylidene-1,5,7,11-tetraoxaspiro[5.5]undecane and 1,5-Dioxa-7,11-dithiaspiro[5.5]undecane
Bromley, Mark K.; Looney, Mark G.; Solomon, David H.; Gable, Robert W.; Helliwell, Madeleine; Hodge, Philip; Acta Crystallographica Section C 54 (1998) 1019–1023; doi:10.1107/S0108270198000274

data_2007472
_publ_section_title
;
 1,5,7,11-Tetraoxaspiro[5.5]undecane,
 3,9-Dimethylidene-1,5,7,11-tetraoxaspiro[5.5]undecane and
 1,5-Dioxa-7,11-dithiaspiro[5.5]undecane
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1019
_journal_page_last               1023
_journal_paper_doi               10.1107/S0108270198000274
_journal_volume                  54
_journal_year                    1998
_chemical_formula_sum            'C7 H12 O2 S2'
_chemical_formula_weight         192.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.478(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1062(12)
_cell_length_b                   8.404(2)
_cell_length_c                   17.721(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.0(10)
_cell_measurement_theta_max      17.1
_cell_measurement_theta_min      13.5
_cell_volume                     907.7(3)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCESS DATA (Gable et al., 1993)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL96
_computing_structure_refinement  'SHELXL96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 MachS'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2627
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   'Gaussian, integration (Sheldrick, 1976)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       blocke
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.180
_refine_ls_extinction_coef       0.048(3)
_refine_ls_extinction_method     SHELXL96
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.030
_refine_ls_R_factor_obs          .027
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.2508P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.074
_refine_ls_wR_factor_obs         .072
_reflns_number_observed          1633
_reflns_number_total             1783
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            os1000.cif
_cod_data_source_block           dhs_3
_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:

'_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^)+(0.0354P)^2^+0.2508P] 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^)+(0.0354P)^2^+0.2508P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2007472