The Unusual Structure of a C-Arylated Gibberellin Bis-γ-lactone Formed from a Free Radical-Initiated Cyclization
Mander, L. N.; Sherburn, M. S.; Willis, A. C.; Acta Crystallographica Section C 53 (1997) 223–225; doi:10.1107/S010827019601147X

data_2005953
_publ_contact_author
;
      Dr Anthony C. Willis
      Research School of Chemistry
      Institute of Advanced Studies
      Australian National University
      Canberra, A.C.T.
      Australia    0200
;
_publ_section_title
;
 The Unusual Structure of a C-Arylated Gibberellin Bis-\g-lactone
 Formed from a Free Radical-Initiated Cyclization
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              223
_journal_page_last               225
_journal_paper_doi               10.1107/S010827019601147X
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C29 H30 O8, C2 H3 N'
_chemical_formula_sum            'C31 H33 N O8'
_chemical_formula_weight         547.61
_chemical_name_systematic
;
ent-13-acetoxy-2\b,3\a-dihydroxy-1\a-carboxy-10\a-phenyl-20-norgibberell-16-
ene-7,19-dioic acid 19,2-lactone 1',3-lactone 7-(methyl ester) acetonitrile
solvate
;
_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           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 92.21(1)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   8.350(2)
_cell_length_b                   12.570(2)
_cell_length_c                   12.945(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1357.7(4)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software
;
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1992)
;
_computing_data_reduction
;
Xtal DIFDAT ABSORB SORTRF ADDREF  (Hall & Stewart, 1990)
;
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement
;
Xtal CRYLSQ  (Hall, King & Stewart, 1995)
;
_computing_structure_solution
;
 shelxs86  (Sheldrick, 1985)
;
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Rigaku AFC6R'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  'equatorial graphite'
_diffrn_radiation_source         'Rigaku RU200B rotating Cu anode'
_diffrn_radiation_type           'Copper K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  .02
_diffrn_reflns_av_sigmaI/netI    .008
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2343
_diffrn_reflns_reduction_process equatorial_monochr_Lp
_diffrn_reflns_theta_max         60.59
_diffrn_reflns_theta_min         3.42
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.81
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         .309
_refine_diff_density_min         -.173
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       '8.1(13) \\times 10^4^ '
_refine_ls_extinction_method
;
equation 22 Larson (1970)
;
_refine_ls_goodness_of_fit_all   2.017
_refine_ls_goodness_of_fit_obs   2.017
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     361
_refine_ls_number_reflns         1741
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .053
_refine_ls_R_factor_obs          .053
_refine_ls_shift/esd_max         .018
_refine_ls_shift/esd_mean        .004
_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         .073
_refine_ls_wR_factor_obs         .073
_reflns_number_observed          1741
_reflns_number_total             1741
_reflns_observed_criterion       all
_cod_data_source_file            ta1104.cif
_cod_data_source_block           MS1
_cod_depositor_comments
;
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 '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_sg_symbol_Hall     P_2y1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2005953