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_7052858
_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         'O4 H P, 2(O4 H2 P), 2(C19 H22 N4), 4(H2 O)'
_chemical_formula_sum            'C38 H57 N8 O16 P3'
_chemical_formula_weight         974.83
_chemical_name_common
;
Bis(1,5-bis(benzimidazolonium)pentane)
bis(dihydrogenophosphate)monohydrogenophosphate tetrahydrate
;
_chemical_name_systematic
;
Bis(1,5-bis(benzimidazolonium)pentane)
bis(dihydrogenophosphate)monohydrogenophosphate tetrahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-09-02
_audit_creation_method
;
Olex2 1.1-beta
(compiled 2011.08.21 svn.r1945, GUI svn.r3824)
;
_cell_angle_alpha                95.255(4)
_cell_angle_beta                 103.115(4)
_cell_angle_gamma                102.980(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8599(5)
_cell_length_b                   12.9049(8)
_cell_length_c                   18.8173(6)
_cell_measurement_reflns_used    13904
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      73.3434
_cell_measurement_theta_min      3.5522
_cell_volume                     2246.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
1 omega -71.00 42.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 77.0000 120.0000 113

2 omega -73.00 43.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 77.0000 -120.0000 116

3 omega -63.00 43.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 77.0000 0.0000 106

4 omega -63.00 -33.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 77.0000 -30.0000 30

5 omega -6.00 19.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 37.5615 98.0000 -179.0000 25

6 omega 69.00 95.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 37.5615 38.0000 60.0000 26

7 omega 68.00 94.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 37.5615 38.0000 -180.0000 26

8 omega 39.00 71.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -45.0000 -120.0000 32

9 omega 105.00 154.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 111.0000 -180.0000 49

10 omega 30.00 110.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -112.0000 174.0000 80

11 omega 57.00 129.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -77.0000 -180.0000 72

12 omega 75.00 122.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 77.0000 -120.0000 47

13 omega 31.00 59.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -45.0000 -180.0000 28

14 omega 34.00 60.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -45.0000 150.0000 26

15 omega 36.00 63.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -45.0000 -90.0000 27

16 omega 111.00 178.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 111.0000 150.0000 67

17 omega 109.00 158.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 111.0000 -150.0000 49

18 omega 32.00 76.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -45.0000 120.0000 44

19 omega 35.00 74.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -45.0000 60.0000 39

20 omega 27.00 174.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 0.0000 -150.0000 147

21 omega 62.00 101.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -111.0000 108.0000 39

22 omega 40.00 125.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 109.7499 -133.0000 32.0000 85

23 omega -122.00 -1.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 -77.0000 30.0000 121

24 omega -122.00 -1.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 -77.0000 90.0000 121

25 omega -122.00 -1.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 -77.0000 -90.0000 121

26 omega -74.00 46.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 77.0000 30.0000 120

27 omega -117.00 -6.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 -38.0000 -60.0000 111

28 omega -117.00 -86.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -37.5615 -38.0000 120.0000 31
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0666590000
_diffrn_orient_matrix_UB_12      -0.0967391000
_diffrn_orient_matrix_UB_13      -0.0047580000
_diffrn_orient_matrix_UB_21      -0.1402590000
_diffrn_orient_matrix_UB_22      -0.0749081000
_diffrn_orient_matrix_UB_23      0.0071754000
_diffrn_orient_matrix_UB_31      -0.0581588000
_diffrn_orient_matrix_UB_32      -0.0196225000
_diffrn_orient_matrix_UB_33      -0.0845899000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21035
_diffrn_reflns_theta_full        73.50
_diffrn_reflns_theta_max         73.50
_diffrn_reflns_theta_min         3.56
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.3915
_exptl_crystal_size_mid          0.1828
_exptl_crystal_size_min          0.0669
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0616P)^2^+0.9508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                8104
_reflns_number_total             8756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj20897k.txt
_cod_data_source_block           (4)2(HPO4)(H2PO4)2
_cod_database_code               7052858
_chemical_oxdiff_formula         'C38 H57 N8 O16 P3'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97