Product of a Novel Carbocyclic Enlargement in Aqueous Media: 9β-<i>tert</i>-Butoxy-4-(<i>E</i>)-ethylidene-8β-methyl-5-oxobicyclo[6.3.0]undecan-2β-carboxylic Acid Methyl Ester
Mague, J. T.; Li, C.-J.; Chen, D.-L.; Lu, Y.-Q.; Haberman, J. X.; Acta Crystallographica Section C 52 (1996) 2597–2599; doi:10.1107/S0108270196006270

data_2005547
_publ_section_title
;Product of a Novel Carbocyclic Enlargement in Aqueous Media:
 9\b-<i>tert</i>-Butoxy-4-(<i>E</i>)-ethylidene-8\b-methyl-5-oxobicyclo[6.3.0]undecan-2\b-carboxylic
 Acid Methyl Ester
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2597
_journal_page_last               2599
_journal_paper_doi               10.1107/S0108270196006270
_journal_volume                  52
_journal_year                    1996
_chemical_formula_structural     'C20 H32 O4'
_chemical_formula_sum            'C20 H32 O4'
_chemical_formula_weight         336.48
_chemical_name_systematic
;
9\b-tert-butoxy-4(E)-ethylidene-8\b-methyl-5-oxobicyclo[6.3.0]undean-2\b-
carboxylic Acid Methyl Ester
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   5.8088(3)
_cell_length_b                   17.976(2)
_cell_length_c                   18.213(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1901.8(3)
_computing_cell_refinement       CAD4
_computing_data_collection       'CAD4 (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCESS MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'CIF VAX MolEN (Fair, 1990)'
_computing_structure_refinement  'LSFM MolEN (Fair, 1990)'
_computing_structure_solution    'Direct methods (SIR88; Burla et al., 1989)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           'Mo K\a, graphite monochromated'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1948
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.1175
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.11
_refine_ls_abs_structure_details
;
?
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.006
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.076
_refine_ls_R_factor_obs          0.043
_refine_ls_shift/esd_max         0.087
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/[\s^2^(Fo^2^) + 0.0016 Fo^4^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.060
_reflns_number_observed          1475
_reflns_number_total             1948
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            sk1014.cif
_cod_data_source_block           1
_cod_depositor_comments
;
 Updating space group information and adding the symmetry operation list.

 Antanas Vaitkus,
 2018-06-18

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/[\s^2^(Fo^2^) + 0.0016
Fo^4^]' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/[\s^2^(Fo^2^) + 0.0016 Fo^4^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1901.8(5)
_cod_original_sg_symbol_H-M      'P 21 21 21                      '
_cod_database_code               2005547
_cod_database_fobs_code          2005547