Syn- and anticlinal isomers of 2a'-acetoxy-1,7'-diacetyl-7',7a'-dihydro-2-oxospiro[1<i>H</i>-indole-3(2<i>H</i>),2'(2a'<i>H</i>)-oxeto[3,2-<i>b</i>]indole]
Usman, Anwar; Razak, Ibrahim Abdul; Fun, Hoong-Kun; Chantrapromma, Suchada; Zhang, Yan; Xu, Jian-Hua; Acta Crystallographica Section C 58 (2002) o59–o62; doi:10.1107/S0108270101020820

data_2012515
_publ_section_title
;Syn- and anticlinal isomers of
 2a'-acetoxy-1,7'-diacetyl-7',7a'-dihydro-2-oxospiro[1<i>H</i>-indole-3(2<i>H</i>),2'(2a'<i>H</i>)-oxeto[3,2-<i>b</i>]indole]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o59
_journal_page_last               o62
_journal_paper_doi               10.1107/S0108270101020820
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C22 H18 N2 O6'
_chemical_formula_moiety         'C22 H18 N2 O6'
_chemical_formula_sum            'C22 H18 N2 O6'
_chemical_formula_weight         406.38
_chemical_melting_point          466
_chemical_name_systematic
;
syn-2a'-acetoxy-1,7'-diacetyl-7',7a'-dihydro-2-oxo-
spiro[1H-indole-3(2H),2'(2a'H)oxeto[2,3-b]indole]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.8970(10)
_cell_angle_beta                 89.8310(10)
_cell_angle_gamma                62.2010(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9350(4)
_cell_length_b                   9.1189(3)
_cell_length_c                   13.4690(6)
_cell_measurement_reflns_used    4055
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.60
_cell_volume                     933.64(7)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full .961
_diffrn_measured_fraction_theta_max .961
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0780
_diffrn_reflns_av_sigmaI/netI    .1443
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4475
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .107
_exptl_absorpt_correction_T_max  .9790
_exptl_absorpt_correction_T_min  .9606
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .32
_exptl_crystal_size_min          .20
_refine_diff_density_max         .560
_refine_diff_density_min         -.521
_refine_ls_extinction_coef       .058(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   .949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .949
_refine_ls_R_factor_all          .0917
_refine_ls_R_factor_gt           .0708
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0848P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1653
_refine_ls_wR_factor_ref         .1936
_reflns_number_gt                2252
_reflns_number_total             3160
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1545.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:

'_chemical_melting_point' value '466K' was changed to '466' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '466K' was changed to '466' - the
value should be numeric and without a unit
designator.

'_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 
;
_cod_database_code               2012515
_cod_database_fobs_code          2012515