Four Isomeric Dioxolane Derivatives of <small>D</small>-Camphorquinone
Clegg, W.; Golding, B. T.; King, B. J.; Maude, A. B.; Acta Crystallographica Section C 51 (1995) 1825–1829; doi:10.1107/S0108270195001788

data_2003918
_publ_section_title
;
 Four Isomeric Dioxolane Derivatives of <small>D</small>-Camphorquinone
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1825
_journal_page_last               1829
_journal_paper_doi               10.1107/S0108270195001788
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C13 H19 Cl O3'
_chemical_formula_weight         258.73
_chemical_name_systematic
;
 (1S,2R,4R,4'R)-4'-chloromethyl-4,7,7-trimethylbicyclo[2.2.1]heptane-
 2-spiro-2'-(1',3'-dioxolan)-3-one
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0866(14)
_cell_length_b                   7.813(2)
_cell_length_c                   23.956(4)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      12.38
_cell_measurement_theta_min      10.37
_cell_volume                     1326.4(5)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXL-93 and local programs'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1990)'
_diffrn_ambient_temperature      240(2)
_diffrn_measurement_device       'Stoe-Siemens diffractometer'
_diffrn_measurement_method
'\w/\q scans with on-line profile fitting (Clegg, 1981)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0177
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -08
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -09
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -028
_diffrn_reflns_number            3907
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .283
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .24
_refine_diff_density_max         .155
_refine_diff_density_min         -0.150
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .00(7)
_refine_ls_extinction_coef       .0068(11)
_refine_ls_extinction_method
'F~c~^*^ = kF~c~[1+0.001xF~c~^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment    'Isotropic H atoms refined with a riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_obs          .0285
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.0326P)^2^+0.2666P] where P =
 (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         .0806
_refine_ls_wR_factor_obs         .0714
_reflns_number_observed          2070
_reflns_number_total             2355
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1114.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      ' P 21 21 21'
_cod_database_code               2003918