3-<i>exo</i>-Chloro-8-oxabicyclo[3.2.1]oct-6-ene-2,4-diol chloroform 0.33-solvate
Tafeenko, Viktor A.; Aslanov, Leonid A.; Proskurnina, Marina V.; Sosonyuk, Sergei E.; Khlevin, Dmitrii A.; Acta Crystallographica Section E 65 (2009) o1580–; doi:10.1107/S1600536809021898

data_2222448
_publ_section_title
;
 3-<i>exo</i>-Chloro-8-oxabicyclo[3.2.1]oct-6-ene-2,4-diol chloroform
 0.33-solvate
;
_journal_coeditor_code           SI2178
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1580
_journal_paper_doi               10.1107/S1600536809021898
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C7 H9 Cl O3, 1/3(C H Cl3)'
_chemical_formula_moiety         '3(C7 H9 Cl O3), C H Cl3'
_chemical_formula_sum            'C7.33333 H9.33333 Cl2 O3'
_chemical_formula_weight         216.39
_chemical_melting_point          decomposition
_chemical_name_systematic
;
3-<i>exo</i>-Chloro-8-oxabicyclo[3.2.1]oct-6-ene-2,4-diol chloroform
0.33-solvate
;
_space_group_IT_number           160
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   18.687(5)
_cell_length_b                   18.687(5)
_cell_length_c                   6.8723(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      32
_cell_volume                     2078.3(9)
_computing_cell_refinement       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'XCAD-4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'Nonprofiled \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1832
_diffrn_reflns_theta_full        71.85
_diffrn_reflns_theta_max         71.85
_diffrn_reflns_theta_min         4.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.088
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          .07
_exptl_crystal_size_min          .06
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.511
_refine_ls_abs_structure_details 'Flack (1983), 481 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         987
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.021P)^2^+2.2041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                966
_reflns_number_total             987
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2178.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               2222448
_cod_database_fobs_code          2222448