Two 14-Membered Macrocycles with <i>trans</i>-<i>trans</i> and <i>trans</i>-<i>cis</i> Dienes. Trimethyl (2<i>E</i>,4<i>E</i>)-<i>cis</i>- and Trimethyl (2<i>Z</i>,4<i>E</i>)-<i>trans</i>-11,15-Dioxobicyclo[12.3.0]heptadeca-2,4-diene-7,7,14-tricarboxylate
Drouin, M.; Couturier, M.; Crevisy, C.; Dory, Y. L.; Deslongchamps, P.; Acta Crystallographica Section C 52 (1996) 2084–2087; doi:10.1107/S0108270195016817

data_2005292
_publ_section_title
;Two 14-Membered Macrocycles with <i>trans</i>-<i>trans</i> and
 <i>trans</i>-<i>cis</i> Dienes. Trimethyl (2<i>E</i>,4<i>E</i>)-<i>cis</i>-
 and Trimethyl
 (2<i>Z</i>,4<i>E</i>)-<i>trans</i>-11,15-Dioxobicyclo[12.3.0]heptadeca-2,4-diene-7,7,14-tricarboxylate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2084
_journal_page_last               2087
_journal_paper_doi               10.1107/S0108270195016817
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C23 H30 O8'
_chemical_formula_sum            'C23 H30 O8'
_chemical_formula_weight         434.47
_chemical_name_systematic
;
trimethyl(10E,12E)-cis-bicyclo[12.3.0]
heptadeca10,12-diene-4,17-dione-1,8,8-tricarboxylate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 107.567(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8355(4)
_cell_length_b                   8.2688(4)
_cell_length_c                   14.7126(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1140.74(10)
_computing_cell_refinement       'TRUANG NRCCAD'
_computing_data_collection       'DATCOL NRCCAD (Le Page, White & Gabe, 1986)'
_computing_data_reduction
'DATRD2 NRCVAX (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976) NRCVAX'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SOLVER NRCVAX '
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.010
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2499
_diffrn_reflns_reduction_process
;
Equivalent reflections grouped and averaged (Le Page & Gabe, 1979)
;
_diffrn_reflns_theta_max         71.66
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             464
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .25
_refine_diff_density_max         .176
_refine_diff_density_min         -.143
_refine_ls_extinction_coef       0.0107(12)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         2397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_obs          0.0413
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+( 0.0631P)^2^+0.0268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1121
_refine_ls_wR_factor_obs         0.1055
_reflns_number_observed          1978
_reflns_number_total             2397
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            pt1020.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:

'_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 'calc w = 1/[\s^2^(Fo^2^)+(
0.0631P)^2^+0.0268P] 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^)+( 0.0631P)^2^+0.0268P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1140.7(1)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2005292