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_7052857
_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         '2(C17 H18 N4), 0.5(H4 O2), 2(O4 S), 5(H2 O)'
_chemical_formula_sum            'C34 H48 N8 O14 S2'
_chemical_formula_weight         856.93
_chemical_name_common
'1,2-bis(benzimidazolonium)ethane sulphate trihydrate'
_chemical_name_systematic
'1,2-bis(benzimidazolonium)ethane sulphate trihydrate'
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9865(8)
_cell_length_b                   17.3680(10)
_cell_length_c                   15.8470(10)
_cell_measurement_reflns_used    17102
_cell_measurement_temperature    220
_cell_measurement_theta_max      28.301
_cell_measurement_theta_min      2.345
_cell_volume                     1916.5(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'STOE XAREA'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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      200
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      ' 145 frames, detector distance = 70 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17102
_diffrn_reflns_theta_full        28.301
_diffrn_reflns_theta_max         28.301
_diffrn_reflns_theta_min         2.345
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           35
_diffrn_source_power             1.93
_diffrn_source_voltage           55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated platelet'
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details 'Flack (1983), 4242 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.7020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.000677
_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:
343. 447. 230. 93.4
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0536
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0536
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                6656
_reflns_number_total             8995
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.35
_oxford_diffrn_Wilson_scale      0.10
_oxford_refine_ls_r_factor_ref   0.0388
_oxford_refine_ls_scale          4.08(2)
_oxford_reflns_number_all        7119
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c2nj20897k.txt
_cod_data_source_block           2(SO4)3H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P -2yac '
_cod_original_sg_symbol_H-M      'P 1 n 1 '
_cod_database_code               7052857