(1<i>R</i>,4<i>S</i>)-({-})-3,3-Ethylenedioxy-1,7,7-trimethylbicyclo[2.2.1]heptan-2-one
Boyle, Grant A.; Govender, Thavendran; Kruger, Hendrik G.; Maguire, Glenn E. M.; Acta Crystallographica Section E 63 (2007) o3765–o3765; doi:10.1107/S1600536807038470

data_2214984
_publ_section_title
(1<i>R</i>,4<i>S</i>)-({-})-3,3-Ethylenedioxy-1,7,7-trimethylbicyclo[2.2.1]heptan-2-one
_journal_coeditor_code           BI2223
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3765
_journal_page_last               o3765
_journal_paper_doi               10.1107/S1600536807038470
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         'C12 H18 O3'
_chemical_formula_sum            'C12 H18 O3'
_chemical_formula_weight         210.26
_chemical_name_systematic
;
(1<i>R</i>,4<i>S</i>)-(-)-1,7,7-Trimethyl-3,3-ethylenedioxybicyclo-
[2.2.1]heptan-2-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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2169(8)
_cell_length_b                   11.8122(14)
_cell_length_c                   13.2986(15)
_cell_measurement_reflns_used    1017
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.82
_cell_volume                     1133.7(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics
;
SHELXTL and Mercury (Bruno <i>et al.</i>, 2002)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8262
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.181
_refine_ls_abs_structure_details
;
In the absence of significant anomalous scattering effects, Friedel
pairs have been merged as equivalent data.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.1693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                1469
_reflns_number_total             1589
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2223.cif
_cod_data_source_block           I
_cod_database_code               2214984
_cod_database_fobs_code          2214984