14-Membered Macrocycles: Methyl <i>trans</i>-(10<i>E</i>)-5-Methyl-8-methylene-11,15-dioxobicyclo[12.3.0]heptadec-4-ene-14-carboxylate, (I), and Methyl <i>trans</i>-(2<i>E</i>,10<i>E</i>)-10-Methyl-7-methylene-4,17-dioxobicyclo[12.3.0]heptadeca-2,10-diene-1-carboxylate, (II)
Drouin, M.; Berthiaume, G.; Deslongchamps, P.; Acta Crystallographica Section C 52 (1996) 107–110; doi:10.1107/S0108270195010092

data_2004440
_publ_section_title
;14-Membered Macrocycles: Methyl
 <i>trans</i>-(10<i>E</i>)-5-Methyl-8-methylene-11,15-dioxobicyclo[12.3.0]heptadec-4-ene-14-carboxylate,
 (I), and Methyl
 <i>trans</i>-(2<i>E</i>,10<i>E</i>)-10-Methyl-7-methylene-4,17-dioxobicyclo[12.3.0]heptadeca-2,10-diene-1-carboxylate,
 (II)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              107
_journal_page_last               110
_journal_paper_doi               10.1107/S0108270195010092
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C21 H30 O4 '
_chemical_formula_sum            'C21 H30 O4'
_chemical_formula_weight         346.46
_chemical_name_systematic
;
Methyl(10E)-trans-bicyclo[12.3.0]heptadeca-7-ylidene-10-methyl-
10-ene-4,17-dione-1-carboxylate
;
_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                95.405(5)
_cell_angle_beta                 96.186(4)
_cell_angle_gamma                91.666(4)
_cell_formula_units_Z            2
_cell_length_a                   7.3972(3)
_cell_length_b                   9.7969(6)
_cell_length_c                   13.3883(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      15.0
_cell_volume                     959.55(9)
_computing_cell_refinement       'NRCCAD TRUANG'
_computing_data_collection       'NRCCAD DATCOL'
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    'NRCVAX ORTEP'
_computing_publication_material  'NRCVAX TABLES'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a~1~'
_diffrn_radiation_wavelength     .70930
_diffrn_reflns_av_R_equivalents  .009
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4818
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .08
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       irregular
_exptl_crystal_F_000             376.15
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .50
_refine_diff_density_max         .32
_refine_diff_density_min         -.20
_refine_ls_extinction_coef       4.5E4(2)
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_obs   1.68
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2690
_refine_ls_R_factor_all          .047
_refine_ls_R_factor_obs          .037
_refine_ls_shift/esd_max         .019
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(\s^2^(F) + 0.0009F^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .062
_refine_ls_wR_factor_obs         .060
_reflns_number_observed          2690
_reflns_number_total             3366
_reflns_observed_criterion       'Inet > 2.5\s(Inet)'
_cod_data_source_file            sz1039.cif
_cod_data_source_block           I
_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:

'_refine_ls_weighting_scheme' value 'w = 1/(\s^2^(F) + 0.0009F^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) +
0.0009F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C21 H30 O4 '
_cod_database_code               2004440