Unique <i>trans</i>-<i>syn</i>-<i>cis</i> [6.6.7] Tricycle Derivative from Transannular Diels–Alder Contraction of a Model 15-Membered <i>trans</i>-<i>cis</i>-<i>cis</i> Macrocyclic Triene
Drouin, Marc; Hall, Dennis G.; Caillé, Alain-Sébastien; Pierre Deslongchamps; Acta Crystallographica Section C 53 (1997) 1490–1493; doi:10.1107/S0108270197005635

data_2006575
_publ_section_title
;
 Unique <i>trans</i>-<i>syn</i>-<i>cis</i> [6.6.7] Tricycle Derivative
 from Transannular Diels--Alder Contraction of a Model 15-Membered
 <i>trans</i>-<i>cis</i>-<i>cis</i> Macrocyclic Triene
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1490
_journal_page_last               1493
_journal_paper_doi               10.1107/S0108270197005635
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C24 H32 O9 '
_chemical_formula_sum            'C24 H32 O9'
_chemical_formula_weight         464.51
_chemical_name_systematic
;
5-Formyl-1,1,8,8-tetrakis(methoxycarbonyl)-(4E,11Z,13E)-
cyclopentadeca-4,11,13-triene
;
_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                74.196(4)
_cell_angle_beta                 78.952(4)
_cell_angle_gamma                73.558(4)
_cell_formula_units_Z            2
_cell_length_a                   6.9449(5)
_cell_length_b                   10.5817(5)
_cell_length_c                   17.8569(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      40.00
_cell_measurement_theta_min      30.00
_cell_volume                     1201.68(12)
_computing_cell_refinement       'NRCCAD TRUANG'
_computing_data_collection
;
NRCCAD DATCOL (Le Page, White & Gabe, 1986)
;
_computing_data_reduction
'NRCVAX DATRD2  (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics    'ORTEP in Xtal_GX (Johnson, 1995)'
_computing_publication_material  'NRCVAX TABLES'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       '\q/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Copper K\a    '
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  .011
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4975
_diffrn_reflns_reduction_process
;
Equivalent reflections grouped and averaged (Le Page & Gabe, 1979)
;
_diffrn_reflns_theta_max         69.57
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .81
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             496
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .10
_refine_diff_density_max         .22
_refine_diff_density_min         -.18
_refine_ls_extinction_coef       '0.27(7) x 10^-6^'
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_obs   1.41
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3057
_refine_ls_R_factor_all          .067
_refine_ls_R_factor_obs          .046
_refine_ls_shift/esd_max         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.0008F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .068
_refine_ls_wR_factor_obs         .061
_reflns_number_observed          3057
_reflns_number_total             4369
_reflns_observed_criterion       'Inet > 2.5\s(Inet)'
_cod_data_source_file            fg1245.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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 '1/[\s^2^(F) + 0.0008F^2^]' 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^(F) +
0.0008F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C24 H32 O9 '
_cod_database_code               2006575