A triclinic polymorph of methyl (3<i>R</i>,3'<i>S</i>)-1',1''-dimethyl-2,2''-dioxodispiro[indoline-3,2'-pyrrolidine-3',3''-indoline]-4'-carboxylate
Ganesh, G.; Yuvaraj, Panneer Selvam; Divakara, Chinthalapuri; Reddy, Boreddy S. R.; SubbiahPandi, A.; Acta Crystallographica Section E 68 (2012) o3468–o3469; doi:10.1107/S160053681204706X

data_2236997
_publ_section_title
;
 A triclinic polymorph of methyl
 (3<i>R</i>,3'<i>S</i>)-1',1''-dimethyl-2,2''-dioxodispiro[indoline-3,2'-pyrrolidine-3',3''-indoline]-4'-carboxylate
;
_journal_coeditor_code           PV2603
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3468
_journal_page_last               o3469
_journal_paper_doi               10.1107/S160053681204706X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C22 H21 N3 O4'
_chemical_formula_moiety         'C22 H21 N3 O4'
_chemical_formula_sum            'C22 H21 N3 O4'
_chemical_formula_weight         391.42
_chemical_name_systematic
;
Methyl (3<i>R</i>,3'<i>S</i>)-1',1''-dimethyl-2,2''-dioxodispiro[indoline-
3,2'-pyrrolidine-3',3''-indoline]-4'-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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.465(2)
_cell_angle_beta                 88.237(2)
_cell_angle_gamma                62.8420(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4418(3)
_cell_length_b                   10.0132(3)
_cell_length_c                   12.8861(4)
_cell_measurement_reflns_used    8469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.67
_cell_measurement_theta_min      2.39
_cell_volume                     985.68(6)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23829
_diffrn_reflns_theta_full        34.67
_diffrn_reflns_theta_max         34.67
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         8469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+0.0657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                5108
_reflns_number_total             8469
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2603.cif
_cod_data_source_block           I
_cod_original_cell_volume        985.68(5)
_cod_database_code               2236997
_cod_database_fobs_code          2236997