Unusual crystal structure of <i>N</i>-substituted maleamic acid – very strong effect of intramolecular hydrogen bonds
Francis, Raju; Raghavaiah, Pallepogu; Pius, Kuruvilla; Acta Crystallographica Section B 70 (2014) 942–947; doi:10.1107/S2052520614018952

data_2105974
_publ_section_title
;
 Unusual crystal structure of <i>N</i>-substituted maleamic acid -- very
 strong effect of intramolecular hydrogen bonds
;
_journal_coeditor_code           EB5032
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              942
_journal_page_last               947
_journal_paper_doi               10.1107/S2052520614018952
_journal_volume                  70
_journal_year                    2014
_chemical_formula_sum            'C6 H7 N O5'
_chemical_formula_weight         173.12
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_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
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_cell_angle_beta                 104.2500(10)
_cell_angle_gamma                103.4720(10)
_cell_formula_units_Z            4
_cell_length_a                   8.1895(7)
_cell_length_b                   9.8902(9)
_cell_length_c                   10.6709(9)
_cell_measurement_reflns_used    5586
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     713.87(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
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_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.217
_refine_ls_extinction_coef       0.022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+0.1110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                2485
_reflns_number_total             2770
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            eb5032sup1.cif
_cod_data_source_block           tpr375
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               2105974
_cod_database_fobs_code          2105974