Octahydro-7a,8'-dimethylspiro[isobenzofuran-4(1<i>H</i>),4'(3'<i>H</i>)-[1<i>H</i>-7,9a]methanocyclohepta[<i>c</i>]pyran]-1',3,9'(3a<i>H</i>,4'a<i>H</i>)-trione
Shi, Hao; Pan, Yuan Jiang; Zhang, Xue Qin; Yu, Kai Bei; Acta Crystallographica Section E 57 (2001) o1007–o1009; doi:10.1107/S1600536801015847

data_2200717
_publ_section_title
Octahydro-7a,8'-dimethylspiro[isobenzofuran-4(1<i>H</i>),4'(3'<i>H</i>)-[1<i>H</i>-7,9a]methanocyclohepta[<i>c</i>]pyran]-1',3,9'(3a<i>H</i>,4'a<i>H</i>)-trione
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1007
_journal_page_last               o1009
_journal_paper_doi               10.1107/S1600536801015847
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C20 H26 O5'
_chemical_formula_moiety         'C20 H26 O5'
_chemical_formula_sum            'C20 H26 O5'
_chemical_formula_weight         346.41
_chemical_melting_point          570.0(10)
_chemical_name_common            'ludongnin B'
_chemical_name_systematic
;
spiro[isobenzofuran-4 (1H),4'(3'H)-[1H-7,9a]
methanocyclohepta[c]pyran]-1',3,9'(3aH,4'aH)-trione,
octahydro-7a,8'-dimethyl
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.62(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.569(2)
_cell_length_b                   9.397(2)
_cell_length_c                   12.310(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.21
_cell_measurement_theta_min      3.31
_cell_volume                     874.6(4)
_computing_cell_refinement       'XSCANS '
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'XSCANS '
_computing_molecular_graphics    'XP in SHELXTL/PC (Siemens, 1991)'
_computing_publication_material  SHELXTL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0226
_diffrn_reflns_av_sigmaI/netI    .0884
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2561
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        2.92
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             372
_exptl_crystal_size_max          .42
_exptl_crystal_size_mid          .34
_exptl_crystal_size_min          .14
_refine_diff_density_max         .243
_refine_diff_density_min         -.182
_refine_ls_abs_structure_details 'see text'
_refine_ls_extinction_coef       .017(4)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   .872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2291
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      .872
_refine_ls_R_factor_all          .1146
_refine_ls_R_factor_gt           .0529
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0602P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1283
_reflns_number_gt                1206
_reflns_number_total             2291
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6077.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '569-571K' was changed to '570.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '569-571K' was changed to '570.0(10)'
- the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2200717
_cod_database_fobs_code          2200717