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_2020392
_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 O7 -'
_chemical_formula_moiety         'C4 H10 N O +, C7 H3 N2 O7 -'
_chemical_formula_sum            'C11 H13 N3 O8'
_chemical_formula_weight         315.24
_chemical_name_common            'Morpholinium 3,5-dinitrosalicylate'
_chemical_name_systematic
;
Tetrahydro-2<i>H</i>-1,4-oxazin-4-ium 2-carboxy-4,6-dinitrophenolate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 101.060(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.8382(11)
_cell_length_b                   10.3220(7)
_cell_length_c                   14.5599(11)
_cell_measurement_reflns_used    1614
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      3.81
_cell_volume                     2631.1(3)
_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(2)
_diffrn_detector_area_resol_mean 16.077
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Gemini-S CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance(Mo) X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6502
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         3.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.214
_refine_ls_extinction_coef       0.0032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012)
;
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0396P)^2^+1.5569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                2054
_reflns_number_total             2574
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ky3097sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2020391--2020394.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2020392
_cod_database_fobs_code          2020392