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_2003917
_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,2S,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           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.90(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2200(13)
_cell_length_b                   7.6439(15)
_cell_length_c                   12.148(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      10.68
_cell_volume                     668.9(2)
_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  .0158
_diffrn_reflns_av_sigmaI/netI    0.0169
_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       14
_diffrn_reflns_limit_l_min       -014
_diffrn_reflns_number            4174
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .280
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             276
_exptl_crystal_size_max          .44
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .28
_refine_diff_density_max         .159
_refine_diff_density_min         -0.140
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -.03(6)
_refine_ls_extinction_coef       .023(3)
_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   1.091
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    'Isotropic H atoms refined with a riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2375
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.112
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_obs          .0284
_refine_ls_shift/esd_max         -0.001
_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^)+(0.0379P)^2^+0.1103P] where P =
 (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         .0776
_refine_ls_wR_factor_obs         .0756
_reflns_number_observed          2273
_reflns_number_total             2375
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1114.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2003917