A 1:2 complex of pyromellitic diimide and dimethyl sulfoxide
Bond, Andrew D.; Acta Crystallographica Section E 58 (2002) o194–o195; doi:10.1107/S1600536802001162

data_2200854
_publ_section_title
;
 A 1:2 complex of pyromellitic diimide and dimethyl sulfoxide
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o194
_journal_page_last               o195
_journal_paper_doi               10.1107/S1600536802001162
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C10 H4 N2 O4, 2C2 H6 O S'
_chemical_formula_moiety         'C10 H4 N2 O4, 2C2 H6 O S'
_chemical_formula_sum            'C14 H16 N2 O6 S2'
_chemical_formula_weight         372.41
_chemical_name_common
;
 pyromellitic diimide / dimethylsulfoxide (1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 114.533(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4152(11)
_cell_length_b                   5.3266(2)
_cell_length_c                   13.8046(12)
_cell_measurement_reflns_used    2650
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     830.49(11)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
 HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK
;
_computing_molecular_graphics
'XP (Sheldrick, 1993) and CAMERON (Watkin et al., 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full .990
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Thin-slice \w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .7107
_diffrn_reflns_av_R_equivalents  .0450
_diffrn_reflns_av_sigmaI/netI    .0646
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5086
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .354
_exptl_absorpt_correction_T_max  .958
_exptl_absorpt_correction_T_min  .879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          .23
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .12
_refine_diff_density_max         .272
_refine_diff_density_min         -.388
_refine_ls_extinction_coef       .038(4)
_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   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          .0752
_refine_ls_R_factor_gt           .0454
_refine_ls_shift/su_max          .010
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0453P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0981
_refine_ls_wR_factor_ref         .1075
_reflns_number_gt                1302
_reflns_number_total             1886
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6143.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2200854
_cod_database_fobs_code          2200854