Synthesis and structure of, and bonding in some derivatives of 2,6,9,10-tetraoxatricyclo[3.3.1.1^3,8^]decane
Simons, J.; Thomas, H. G.; Hall, S. R.; Raabe, G.; Acta Crystallographica Section B 57 (2001) 63–71; doi:10.1107/S0108768100013331

data_2103554
_publ_section_title
;
 Synthesis and structure of, and bonding in some derivatives of
 2,6,9,10-tetraoxatricyclo[3.3.1.1^3,8^]decane
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              63
_journal_page_last               71
_journal_paper_doi               10.1107/S0108768100013331
_journal_volume                  57
_journal_year                    2001
_chemical_formula_sum            'C15 H22 O9'
_chemical_formula_weight         346.33
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 104.508(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   10.858(3)
_cell_length_b                   14.1170(8)
_cell_length_c                   11.519(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.85
_cell_measurement_theta_min      10.19
_cell_volume                     1709.4(8)
_computing_data_reduction        'xtal DIFDAT SORTRF ADDREF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       '   \w/2\q'
_diffrn_radiation_monochromator  '  graphite'
_diffrn_radiation_source         '  Cu anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54179
_diffrn_reflns_av_R_equivalents  .05
_diffrn_reflns_av_sigmaI/netI    .041
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5250
_diffrn_reflns_reduction_process 'perpendicular monochr Lp'
_diffrn_reflns_theta_max         72.86
_diffrn_reflns_theta_min         4.21
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .959
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            '    colourless'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       '    irregular'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          .70
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .30
_refine_diff_density_max         .215
_refine_diff_density_min         -.255
_refine_ls_extinction_coef       128E2(3)
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.002
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .049
_refine_ls_R_factor_gt           .049
_refine_ls_shift/su_max          .014
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[3.52\s^2^(F^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .064
_refine_ls_wR_factor_ref         .064
_reflns_number_gt                3070
_reflns_number_total             3070
_reflns_threshold_expression     'Fsqd >  .00 sig(Fsqd)'
_cod_data_source_file            jz0010.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_hydrogen_treatment' value ' refall' changed to 'refall'
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:

'_refine_ls_hydrogen_treatment' value ' refall' changed to 'refall'
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_database_code               2103554
_cod_database_fobs_code          2103554