The crystal structure of Histidinium hydrogensquarate, C10H11N3O6
Kolev, Tsonko; Peeva, Martina I.; Bogdanov, Ivan P.; Ognyanov, Iliyan V.; Atanasov, Atanas G.; Tzvetkov, Nikolay T.; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 601–603; doi:10.1515/ncrs-2022-0181

data_8107164
_publ_section_title
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 The crystal structure of Histidinium hydrogensquarate, C10H11N3O6
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              601
_journal_page_last               603
_journal_paper_doi               10.1515/ncrs-2022-0181
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C6 H10.497 N3 O2, C4 H0.503 O4'
_chemical_formula_sum            'C10 H11 N3 O6'
_chemical_formula_weight         269.22
_chemical_melting_point          560
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.465(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4928(12)
_cell_length_b                   14.860(3)
_cell_length_c                   11.0593(18)
_cell_measurement_reflns_used    1360
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.8543
_cell_measurement_theta_min      2.3861
_cell_volume                     1161.0(4)
_computing_cell_refinement       'APEX2 (Bruker, 2011); SAINT (Bruker, 2009)'
_computing_data_collection       'GIS (Bruker)'
_computing_data_reduction        'SAINT (Bruker, 2009); XPREP (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 1.5-alpha [4]'
_computing_publication_material  'Olex2 1.5-alpha [4]'
_computing_structure_refinement  'ShelXL 2018/3 [5]'
_computing_structure_solution    'ShelXT  [5]'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7238
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.386
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.9821
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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'Sheldrick, G. M. (2008) SADABS. University of G\"ottingen, Germany.'
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_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0069(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 [6]'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2038
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.1119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1511
_reflns_number_total             2038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0181_suppl.cif
_cod_data_source_block           SQ_HIS
_cod_database_code               8107164
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
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1. Restrained distances
 O3-H3 \\sim O1-H1
 with sigma of 0.02
2. Others
 Sof(H1)=1-FVAR(1)
 Sof(H3)=FVAR(1)
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_shelx_res_checksum              207
_shelx_hkl_checksum              15415
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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