Hydrogen bonding in 2,2',2''-(nitrilotrimethylene)tripyridinium hydrogenphosphate tetrakis(perchlorate) dihydrate and related compounds
Hazell, Alan; Acta Crystallographica Section E 62 (2006) o5941–o5943; doi:10.1107/S160053680605080X

data_2211486
_publ_section_title
;
 Hydrogen bonding in 2,2',2''-(nitrilotrimethylene)tripyridinium
 hydrogenphosphate tetrakis(perchlorate) dihydrate and related
 compounds
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o5941
_journal_page_last               o5943
_journal_paper_doi               10.1107/S160053680605080X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '2C18 H21 N4 3+, H1 O4 P 2-, 4Cl O4 -, 2H2 O'
_chemical_formula_moiety
'2(C18 H21 N4 3+), (H1 O4 P 2-), 4(Cl O4 -), 2(H2 O)'
_chemical_formula_sum            'C36 H47 Cl4 N8 O22 P'
_chemical_formula_weight         1116.64
_chemical_name_common            (H3tpa)2(HPO4)(ClO4)4,2H2O
_chemical_name_systematic
;
bis[2,2',2''-(nitrilotrimethylene)tripyridinium]
hydrogenphosphate tetrakis(perchlorate) dihydrate
;
_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_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 100.9880(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.1366(7)
_cell_length_b                   12.8104(6)
_cell_length_c                   23.8320(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      2.0
_cell_volume                     4836.1(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and KRYSTAL
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement
'modified ORFLS (Busing <i>et al.</i>,  1962) and KRYSTAL'
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999) and KRYSTAL (Hazell, 1995)
;
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            45366
_diffrn_reflns_reduction_process 45366
_diffrn_reflns_theta_full        29.8
_diffrn_reflns_theta_max         29.8
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2312.0
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.81(8)
_refine_diff_density_min         -1.12(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     644
_refine_ls_number_reflns         9018
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.053
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.00003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w= 1/{[\s~cs~(F^2^)+B +(1+A)F^2^]^1/2^- |F|}^2^, with A = 0.03, B = 0.5'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.051
_reflns_number_gt                9018
_reflns_number_total             13850
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            jh2046.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C36 H47 Cl4 N8 O22 P1'
_cod_database_code               2211486
_cod_database_fobs_code          2211486