(<i>S</i>,<i>S</i>)-4''-Cyano-7,7''-dimethoxy-3',6'-dioxodispiro[indane-2,2'-piperazine-5',2''-indane]-4-carboxamide methanol solvate: interrupting the amide-to-amide hydrogen-bonded tape
Jagadish, Bhumasamudram; Carducci, Michael D.; Dawson, Alice; Nichol, Gary S.; Mash, Eugene A.; Acta Crystallographica Section C 64 (2008) o431–o433; doi:10.1107/S010827010802057X

data_2016737
_publ_section_title
;(<i>S</i>,<i>S</i>)-4''-Cyano-7,7''-dimethoxy-3',6'-dioxodispiro[indane-2,2'-piperazine-5',2''-indane]-4-carboxamide
 methanol solvate: interrupting the amide-to-amide hydrogen-bonded tape
;
_journal_coeditor_code           SK3252
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o431
_journal_page_last               o433
_journal_paper_doi               10.1107/S010827010802057X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C24 H22 N4 O5 , C H4 O'
_chemical_formula_moiety         'C24 H22 N4 O5 , C H4 O'
_chemical_formula_sum            'C25 H26 N4 O6'
_chemical_formula_weight         478.50
_chemical_melting_point          230
_chemical_name_systematic
;
4''-cyano-7,7''-dimethoxy-3',6'-dioxodispiro[indane-2,2'-piperazine-
5',2''-indane]-4-carboxamide methanol solvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6409(7)
_cell_length_b                   10.4629(8)
_cell_length_c                   25.5588(19)
_cell_measurement_reflns_used    4713
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.25
_cell_volume                     2578.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Version 2.0; Macrae
<i>et al.</i>,  2006)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2008) and local
programs
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20487
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.119
_refine_diff_density_min         -0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         2821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0341P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                2290
_reflns_number_total             2821
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3252.cif
_cod_data_source_block           I
_cod_database_code               2016737
_cod_database_fobs_code          2016737