Cyclic heterotetrameric and low-dimensional hydrogen-bonded polymeric structures in the morpholinium salts of ring-substituted benzoic acid analogues
Smith, Graham; Lynch, Daniel E.; Acta Crystallographica Section C 72 (2016) 105–111; doi:10.1107/S2053229615024821

data_2020393
_publ_section_title
;
 Cyclic heterotetrameric and low-dimensional hydrogen-bonded polymeric
 structures in the morpholinium salts of ring-substituted benzoic acid
 analogues
;
_journal_coeditor_code           KY3097
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              105
_journal_page_last               111
_journal_paper_doi               10.1107/S2053229615024821
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C4 H10 N O + , C7 H3 N2 O6 -'
_chemical_formula_moiety         'C4 H10 N O +, C7 H3 N2 O6 -'
_chemical_formula_sum            'C11 H13 N3 O7'
_chemical_formula_weight         299.24
_chemical_name_common            'Morpholinium 3,5-dinitrobenzoate'
_chemical_name_systematic
;
Tetrahydro-2<i>H</i>-1,4-oxazin-4-ium 3,5-dinitrobenzoate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.326(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.208(2)
_cell_length_b                   5.6443(4)
_cell_length_c                   23.9753(19)
_cell_measurement_reflns_used    1302
_cell_measurement_temperature    200.0(10)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      3.76
_cell_volume                     2572.3(5)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>, 1993)
;
_diffrn_ambient_temperature      200.0(10)
_diffrn_detector_area_resol_mean 16.077
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Gemini-S 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     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5493
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0425P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                1647
_reflns_number_total             2520
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ky3097sup1.cif
_cod_data_source_block           III
_cod_depositor_comments
'Adding full bibliography for 2020391--2020394.cif.'
_cod_original_cell_volume        2572.3(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2020393
_cod_database_fobs_code          2020393