The supramolecular architecture of tris(naphthalene-1,5-diaminium) bis(5-aminonaphthalen-1-aminium) octakis[hydrogen (5-carboxypyridin-3-yl)phosphonate]
Wilk, Magdalena; Janczak, Jan; Videnova-Adrabinska, Veneta; Acta Crystallographica Section C 68 (2012) o351–o354; doi:10.1107/S0108270112033781

data_2018609
_publ_section_title
;
 The supramolecular architecture of tris(naphthalene-1,5-diaminium)
 bis(5-aminonaphthalen-1-aminium) octakis[hydrogen
 (5-carboxypyridin-3-yl)phosphonate]
;
_journal_coeditor_code           EM3051
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o351
_journal_page_last               o354
_journal_paper_doi               10.1107/S0108270112033781
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'3C10 H12 N2 2+ , 2C10 H11 N2 + , 8C6 H5 N O5 P -'
_chemical_formula_moiety
'3(C10 H12 N2 2+), 2(C10 H11 N2 +), 8(C6 H5 N O5 P -)'
_chemical_formula_sum            'C98 H98 N18 O40 P8'
_chemical_formula_weight         2415.70
_chemical_name_systematic
;
tris(naphthalene-1,5-diaminium)
bis(5-aminonaphthalen-1-aminium) octakis[hydrogen
(5-carboxypyridin-3-yl)phosphonate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.306(3)
_cell_length_b                   26.675(5)
_cell_length_c                   14.436(3)
_cell_measurement_reflns_used    1252
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.41
_cell_volume                     5437(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type
'Kuma KM-4 diffractometer with a CCD area detector'
_diffrn_measurement_method       \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  0.0857
_diffrn_reflns_av_sigmaI/netI    0.1007
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71634
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.9167
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      1.47
_exptl_crystal_density_method    flotation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         13812
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                6933
_reflns_number_total             13812
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            em3051.cif
_cod_data_source_block           I
_cod_original_cell_volume        5437.2(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018609
_cod_database_fobs_code          2018609