A Novel Tricyclic Cyclobutanone Ketal
Britten, J. F.; Kassam, K.; Warkentin, J.; Acta Crystallographica Section C 53 (1997) 243–245; doi:10.1107/S0108270196013224

data_2005928
_publ_contact_author
;
      James F. Britten
      Department of Chemistry
      McMaster University
      1280 Main Street West
      Hamilton, Ont. L8S4M1
      Canada
;
_publ_section_title
;
 A Novel Tricyclic Cyclobutanone Ketal
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              243
_journal_page_last               245
_journal_paper_doi               10.1107/S0108270196013224
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C15 H22 O5'
_chemical_formula_sum            'C15 H22 O5'
_chemical_formula_weight         282.33
_chemical_name_systematic
;
    (+-)Methyl (1\a,1a\a,3a\a,6a\a,6b\a)-1a-ethenyl-octahydro-
6a-methoxy-2,2- dimethyl-3,6-dioxacyclobut[cd]indene-1-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.44(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.438(5)
_cell_length_b                   8.697(5)
_cell_length_c                   11.964(7)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.75
_cell_measurement_theta_min      9.90
_cell_volume                     1486.0(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control (MSC,1988)'
_computing_data_collection       'MSC/AFC Diffractometer Control (MSC,1988)'
_computing_data_reduction        'teXsan: PROCESS (MSC,1992)'
_computing_molecular_graphics    'SHELXTL: XP (Sheldrick,1995)'
_computing_publication_material  'SHELXTL: XL (Sheldrick,1995)'
_computing_structure_refinement  'SHELXTL: XL (Sheldrick,1995)'
_computing_structure_solution    'SAPI91 (Fan,1991)'
_diffrn_ambient_temperature      23.0
_diffrn_measurement_device       AFC6R
_diffrn_measurement_method       '2\q-\w scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.1374
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2578
_diffrn_reflns_reduction_process 'TEXSAN PROCESS (MSC,1992)'
_diffrn_reflns_theta_max         54.99
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        -0.54
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    none
_exptl_crystal_description       'fragment from a multiple crystal'
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.214
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_goodness_of_fit_obs   1.189
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         1806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_restrained_S_obs      1.189
_refine_ls_R_factor_all          0.1895
_refine_ls_R_factor_obs          0.0456
_refine_ls_shift/esd_max         0.015
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.4258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1644
_refine_ls_wR_factor_obs         0.1077
_reflns_number_observed          857
_reflns_number_total             1865
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cr1168.cif
_cod_data_source_block           C15H22O5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (22
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (37 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.4258P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.4258P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2005928