A 16-connected three-dimensional hydrogen-bonding network in tetrakis(4-aminopyridinium) perylene-3,4,9,10-tetracarboxylate octahydrate
Zhang, Zhi-Hui; Wang, Jin-Long; Gao, Ning; He, Ming-Yang; Acta Crystallographica Section C 70 (2014) 668–671; doi:10.1107/S2053229614012947

data_2019585
_publ_section_title
;
 A 16-connected three-dimensional hydrogen-bonding network in
 tetrakis(4-aminopyridinium) perylene-3,4,9,10-tetracarboxylate
 octahydrate
;
_journal_coeditor_code           YF3064
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              668
_journal_page_last               671
_journal_paper_doi               10.1107/S2053229614012947
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '4C5 H7 N2 + , C24 H8 O8 4- , 8H2 O'
_chemical_formula_moiety         '4(C5 H7 N2 +), C24 H8 O8 4-, 8(H2 O)'
_chemical_formula_sum            'C44 H52 N8 O16'
_chemical_formula_weight         948.94
_chemical_name_systematic
;
Tetrakis(4-aminopyridinium) perylene-3,4,9,10-tetracarboxylate octahydrate
;
_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                 114.097(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.771(3)
_cell_length_b                   19.703(3)
_cell_length_c                   14.210(3)
_cell_measurement_reflns_used    1793
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.849
_cell_measurement_theta_min      2.498
_cell_volume                     4541.9(14)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2005)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0958
_diffrn_reflns_av_sigmaI/netI    0.1090
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14116
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7459.
_exptl_absorpt_correction_T_min  0.6117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0407P)^2^+0.0010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                2381
_reflns_number_total             4696
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yf3064sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019585.cif.'
_cod_original_cell_volume        4541.8(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2019585
_cod_database_fobs_code          2019585