Unusual solidification and phosphate binding to benzimidazole cations in the presence of water
Clifford, Sarah E.; Runowski, Marcin; Parthasarathy, Nalini; Besnard, Céline; Melich, Xavier; Williams, Alan F.; New Journal of Chemistry 36 (2012) 823–; doi:10.1039/c2nj20897k

data_7052856
_publ_section_title
;
 Unusual solidification and phosphate binding to benzimidazole cations in
 the presence of water
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              823
_journal_paper_doi               10.1039/c2nj20897k
_journal_volume                  36
_journal_year                    2012
_chemical_formula_moiety         'C19 H22 N4, 2(H2 O4 P)'
_chemical_formula_sum            'C19 H26 N4 O8 P2'
_chemical_formula_weight         500.39
_chemical_name_common
'1,5-bis(benzimidazolonium)pentane bis(dihydrogenophosphate)'
_chemical_name_systematic
'1,5-bis(benzimidazolonium)pentane bis(dihydrogenophosphate)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                99.752(8)
_cell_angle_beta                 98.148(8)
_cell_angle_gamma                115.368(8)
_cell_formula_units_Z            2
_cell_length_a                   9.6451(11)
_cell_length_b                   9.7718(11)
_cell_length_c                   13.5760(13)
_cell_measurement_reflns_used    19568
_cell_measurement_temperature    230
_cell_measurement_theta_max      31.59
_cell_measurement_theta_min      2.39
_cell_volume                     1106.0(2)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Sir2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      230
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21657
_diffrn_reflns_theta_full        30.053
_diffrn_reflns_theta_max         31.305
_diffrn_reflns_theta_min         2.387
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian Integration (Busing and Levy, 1957)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0613
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7078
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000486
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.63 1.62 0.357
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0613
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0613
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5522
_reflns_number_total             7093
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0550
_oxford_refine_ls_scale          0.36862(18)
_oxford_reflns_number_all        7078
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c2nj20897k.txt
_cod_data_source_block           4(H2PO4)2
_cod_database_code               7052856