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_2103553
_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            'C14 H19 Cl O8'
_chemical_formula_weight         350.75
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 98.19(5)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   8.1170(10)
_cell_length_b                   8.5598(7)
_cell_length_c                   23.786(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      53.38
_cell_measurement_theta_min      29.05
_cell_volume                     1635.8(4)
_computing_data_reduction        'xtal 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         'fine-focus sealed tu'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  .013
_diffrn_reflns_av_sigmaI/netI    .014
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3274
_diffrn_reflns_theta_max         72.63
_diffrn_reflns_theta_min         3.75
_diffrn_standards_decay_%        9
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.431
_exptl_absorpt_correction_T_max  .999
_exptl_absorpt_correction_T_min  .810
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;A.C.T.North, D.C.Phillips, F.S.Matthews,
Acta Cryst. A24, 351-359 (1968). The Tmin/Tmax
values give below are relative values.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       irregular
_exptl_crystal_F_000             736
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .20
_refine_diff_density_max         .408
_refine_diff_density_min         -.498
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .058
_refine_ls_R_factor_gt           .058
_refine_ls_shift/su_max          .0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[3\s^2^(F^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .091
_refine_ls_wR_factor_ref         .091
_reflns_number_gt                3203
_reflns_number_total             3203
_reflns_threshold_expression     'Fsqd >  .00 sig(Fsqd)'
_cod_data_source_file            jz0010.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C14 H19 Cl1 O8'
_cod_database_code               2103553
_cod_database_fobs_code          2103553