(±)-(3'aα,3'bα,6'aα,7'aα)- and (±)-(3'aα,3'bβ,6'aβ,7'aα)-2,3,3a,3b,4,5,6,6a,7,7a-decahydro-5,5-dimethylspiro[1,3-dioxane-2,5'-pentaleno[2,1-<i>b</i>]furan]-2'-one
Bats, Jan W.; Öhlinger, Stefan H.; Mulzer, Johann; Acta Crystallographica Section C 55 (1999) IUC9900111–; doi:10.1107/S0108270199098807

data_2008964
_publ_section_title
;(+-)-(3'a\a,3'b\a,6'a\a,7'a\a)- and
 (+-)-(3'a\a,3'b\b,6'a\b,7'a\a)-2,3,3a,3b,4,5,6,6a,7,7a-decahydro-5,5-dimethylspiro[1,3-dioxane-2,5'-pentaleno[2,1-<i>b</i>]furan]-2'-one
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900111
_journal_paper_doi               10.1107/S0108270199098807
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C15 H22 O4'
_chemical_formula_weight         266.33
_chemical_melting_point          358.0(10)
_chemical_name_systematic
;
(+-)-(3'a\a,3'b\a,6'a\a,7'a\a)-octahydro-5,5-dimethyl-spiro[1,3-dioxane-
2,5'(2'H)pentaleno[2,1-b]furan]-2'-one
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                88.370(11)
_cell_angle_beta                 86.483(7)
_cell_angle_gamma                70.162(11)
_cell_formula_units_Z            2
_cell_length_a                   5.6779(10)
_cell_length_b                   6.3017(11)
_cell_length_c                   20.480(3)
_cell_measurement_reflns_used    186
_cell_measurement_temperature    134(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     688.0(2)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'CIF in SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1996)'
_diffrn_ambient_temperature      134(2)
_diffrn_measured_fraction_theta_full 0.846
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       \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  0.038
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11957
_diffrn_reflns_theta_full        31.98
_diffrn_reflns_theta_max         30.6
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  540
_diffrn_standards_number         209
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   'numerical (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.217
_refine_ls_extinction_coef       0.019(7)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.557
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.557
_refine_ls_R_factor_all          0.045
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.06P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.125
_reflns_number_gt                3582
_reflns_number_total             4038
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qa0163.cif
_cod_data_source_block           I
_cod_original_cell_volume        687.98(19)
_cod_original_sg_symbol_H-M      ' P -1'
_cod_database_code               2008964