#------------------------------------------------------------------------------
#$Date: 2019-09-11 18:44:08 +0200 (Wed 11 de Sep de 2019) $
#$Revision: 218197 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003398.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003398
loop_
_publ_author_name
'Pèpe, G.'
'Reboul, J.-P.'
'Brun, P.'
'Zylber, J.'
_publ_section_title
;
 3-Oxo-2-phenyl-3a,4,5,7a-tetrahydro-5,7a-epoxyisoindoline-4-carboxylic
 Acid in Two Crystalline Phases, Solvated with DMSO and Unsolvated
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              729
_journal_page_last               732
_journal_paper_doi               10.1107/S010827019401142X
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C15 H13 N1 O4'
_chemical_formula_structural     'C15 H13 N1 O4'
_chemical_formula_sum            'C15 H13 N O4'
_chemical_formula_weight         271.27
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-A 2ya'
_symmetry_space_group_name_H-M   'A 1 2/a 1'
_atom_type_scat_source
' International Tables for X-ray Crystallography (1974, Vol. IV, Table 2.2B)'
_cell_angle_alpha                90.00
_cell_angle_beta                 81.41(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.961(5)
_cell_length_b                   13.219(2)
_cell_length_c                   11.598(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      45
_cell_measurement_theta_min      15
_cell_volume                     2571.2(10)
_computing_cell_refinement       'CAD-4 Operations Manual'
_computing_data_collection
'CAD-4 Operations Manual (Enraf-Nonius, 1977)'
_computing_data_reduction        'program elaborated at CRMC2'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'Word 5.0 on Machintoch LC II'
_computing_structure_refinement  'SHELX76 (Sheldrick, 1976)'
_computing_structure_solution    'MULTAN80 (Main et al., 1980)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_sigmaI/netI    0.1928
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5489
_diffrn_reflns_reduction_process 'SDP system'
_diffrn_reflns_theta_max         45
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.76
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_meas      1.41(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         .25
_refine_diff_density_min         -.23
_refine_ls_goodness_of_fit_all   0.93
_refine_ls_goodness_of_fit_obs   0.93
_refine_ls_hydrogen_treatment
;
H-atom displacement parameters not refined
;
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .041
_refine_ls_R_factor_obs          .041
_refine_ls_shift/esd_max         .13
_refine_ls_shift/esd_mean        .13
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_all         .041
_refine_ls_wR_factor_obs         .041
_reflns_number_observed          2552
_reflns_number_total             5489
_reflns_observed_criterion       refl_obs_if_I_>_3.0_sigma(I)
_cod_data_source_file            pa1143.cif
_cod_data_source_block           pepe2
_cod_depositor_comments
;
 Changed the value of the '_atom_site_type_symbol' data item for hydrogen
 atoms from '?' to 'H'.

 Antanas Vaitkus,
 2019-09-11
;
_cod_original_cell_volume        2571.6(7)
_cod_original_sg_symbol_H-M      'A 2/a'
_cod_original_formula_sum        'C15 H13 N1 O4'
_cod_database_code               2003398
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,+y,-z
-x,-y,-z
1/2+x,-y,+z
x,1/2+y,1/2+z
1/2-x,1/2+y,1/2-z
-x,1/2-y,1/2-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_type_symbol
C1 -.0087(1) -.1955(1) -.4759(2) 3.0(1) Uani d C
C2 .0484(1) -.1829(2) -.4045(2) 3.6(1) Uani d C
C3 .1128(1) -.1198(2) -.4366(2) 3.2(1) Uani d C
C4 .1182(1) -.0656(1) -.5385(2) 3.2(1) Uani d C
C5 .0596(1) -.0742(1) -.6104(1) 2.5(1) Uani d C
C6 -.0043(1) -.1400(1) -.5801(1) 2.0(1) Uani d C
N7 -.0642(1) -.1524(1) -.6497(1) 2.0(1) Uani d N
C8 -.1442(1) -.1923(1) -.6012(1) 2.6(1) Uani d C
C9 -.1931(1) -.1682(1) -.6921(1) 1.7(1) Uani d C
C10 -.1348(1) -.1663(1) -.8076(1) 1.8(1) Uani d C
C11 -.0583(1) -.1360(1) -.7685(1) 2.2(1) Uani d O
O12 .0041(1) -.1060(1) -.8290(1) 3.0(1) Uani d C
C13 -.2709(1) -.2161(1) -.7113(2) 3.1(1) Uani d C
C14 -.3052(1) -.1531(2) -.7761(2) 3.0(1) Uani d C
C15 -.2512(1) -.0624(1) -.7945(1) 2.6(1) Uani d C
C16 -.1775(1) -.0947(1) -.8848(1) 2.6(1) Uani d C
C17 -.1285(1) -.0056(1) -.9375(1) 2.1(1) Uani d C
O18 -.0864(1) -.0294(1) -1.0369(1) 4.1(1) Uani d O
O19 -.1283(1) .0763(1) -.8954(1) 5.1(1) Uani d O
O20 -.2166(1) -.0624(1) -.6875(1) 2.2(1) Uani d O
H1 -.058(1) -.245(2) -.452(2) ? ? ? H
H2 .048(1) -.233(2) -.324(2) ? ? ? H
H3 .152(1) -.099(2) -.393(2) ? ? ? H
H4 .172(1) -.017(2) -.567(2) ? ? ? H
H5 .067(1) -.026(2) -.694(2) ? ? ? H
H6 -.172(1) -.159(2) -.533(2) ? ? ? H
H7 -.145(1) -.283(2) -.570(2) ? ? ? H
H8 -.126(1) -.227(2) -.847(2) ? ? ? H
H9 -.285(1) -.277(2) -.690(2) ? ? ? H
H10 -.356(1) -.176(2) -.811(2) ? ? ? H
H11 -.284(1) -.003(2) -.810(2) ? ? ? H
H12 -.191(1) -.135(2) -.949(2) ? ? ? H
H13 -.065(1) .013(2) -1.081(2) ? ? ? H
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
6 1 3
4 5 1
8 3 1
5 4 2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C11 C10 C9 102.4(3) yes
C11 C10 C16 120.9(4) yes
C16 C10 C9 102.5(3) yes
C10 C11 N7 108.9(4) yes
C10 C11 O12 128.3(4) yes
N7 C11 O12 122.7(4) yes
C14 C13 C9 106.9(5) yes
C13 C14 C15 105.9(5) yes
C14 C15 C16 106.6(4) yes
C14 C15 O20 101.2(4) yes
C16 C15 O20 100.8(3) yes
C10 C16 C15 100.1(3) yes
C10 C16 C17 115.5(4) yes
C15 C16 C17 113.1(4) yes
C16 C17 O18 111.4(4) yes
C16 C17 O19 125.3(4) yes
O18 C17 O19 123.4(4) yes
C1 C2 C3 120.7(6) yes
C2 C3 C4 119.7(6) yes
C3 C4 C5 120.7(5) yes
C4 C5 C6 119.8(4) yes
C1 C6 C5 118.8(4) yes
C1 C6 N7 119.0(4) yes
C5 C6 N7 122.2(4) yes
C9 C8 N7 103.4(4) yes
C10 C9 C8 105.7(4) yes
C10 C9 C13 109.9(4) yes
C10 C9 O20 98.8(3) yes
C13 C9 C8 127.9(4) yes
C13 C9 O20 99.7(3) yes
C8 C9 O20 111.3(4) yes
C11 N7 C6 127.3(4) yes
C11 N7 C8 111.1(4) yes
C6 N7 C8 121.6(4) yes
C15 O20 C9 96.5(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 1.375(4) yes
C1 C6 1.406(3) yes
C10 C9 1.542(3) yes
C10 C11 1.492(3) yes
C10 C16 1.554(3) yes
C11 N7 1.383(3) yes
C11 O12 1.244(3) yes
C13 C9 1.510(3) yes
C13 C14 1.314(4) yes
C14 C15 1.505(3) yes
C15 C16 1.565(3) yes
C15 O20 1.450(3) yes
C16 C17 1.517(3) yes
C17 O18 1.301(3) yes
C17 O19 1.188(3) yes
C2 C3 1.381(4) yes
C3 C4 1.374(4) yes
C4 C5 1.394(3) yes
C5 C6 1.393(3) yes
C6 N7 1.399(3) yes
C8 N7 1.486(3) yes
C8 C9 1.472(3) yes
C9 O20 1.453(3) yes
