A whole zoo of hydrogen bonds in one crystal structure: tris(isonicotinium) hydrogensulfate sulfate monohydrate
Truong, Khai-Nghi; Lothmann, Niklas; Englert, Ulli; Acta Crystallographica Section C 73 (2017) 525–530; doi:10.1107/S2053229617008269

data_2020764
_publ_section_title
;
 A whole zoo of hydrogen bonds in one crystal structure:
 tris(isonicotinium) hydrogensulfate sulfate monohydrate
;
_journal_coeditor_code           YF3121
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              525
_journal_page_last               530
_journal_paper_doi               10.1107/S2053229617008269
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '3C6 H6 N O2 +, H O4 S -, O4 S 2-, H2 O'
_chemical_formula_moiety         '3(C6 H6 N O2 +), H O4 S -, O4 S 2-, H2 O'
_chemical_formula_sum            'C18 H21 N3 O15 S2'
_chemical_formula_weight         583.50
_chemical_name_common            'L-9 (H2SO4)'
_chemical_name_systematic
;
Tris(4-carboxypyridinium) hydrogensulfate sulfate monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.625(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.951(3)
_cell_length_b                   11.7885(18)
_cell_length_c                   20.891(4)
_cell_measurement_reflns_used    4228
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.39
_cell_volume                     4731.8(14)
_computing_cell_refinement
;
SMART (Bruker, 2001)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXS2013 (Sheldrick, 2008)
;
_computing_structure_solution
;
PLATON (Spek, 2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker D8 goniometer with APEX CCD detector'
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35239
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.188
_diffrn_reflns_theta_min         2.027
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.558
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6845
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+4.9842P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                5404
_reflns_number_total             6845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yf3121sup1.cif
_cod_data_source_block           I
_cod_database_code               2020764
_cod_database_fobs_code          2020764
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.921
_shelx_hkl_checksum              52152
_shelx_res_checksum              62171
_shelxl_version_number           20.13