A mechanochemically synthesized covalent organic framework as a proton-conducting solid electrolyte
Shinde, Digambar Balaji; Aiyappa, Harshitha Barike; Bhadra, Mohitosh; Biswal, Bishnu P.; Wadge, Pritish; Kandambeth, Sharath; Garai, Bikash; Kundu, Tanay; Kurungot, Sreekumar; Banerjee, Rahul; Journal of Materials Chemistry A 4 (2016) 2682–; doi:10.1039/C5TA10521H

data_7236141
_publ_section_title
;
 A mechanochemically synthesized covalent organic framework as a
 proton-conducting solid electrolyte
;
_journal_issue                   7
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              2682
_journal_paper_doi               10.1039/C5TA10521H
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C10 H12 N4, 2(H2 O4 P)'
_chemical_formula_sum            'C10 H16 N4 O8 P2'
_chemical_formula_weight         382.21
_chemical_name_common
'2,2'-bipyridinium-5-amino5'-ammonium bis-dihydrogen Phosphate'
_chemical_name_systematic        BiPy-PA
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-30
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:34:12, GUI svn.r4372)
;
_audit_update_record
;
2015-02-03 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                73.441(9)
_cell_angle_beta                 85.209(8)
_cell_angle_gamma                83.669(9)
_cell_formula_units_Z            2
_cell_length_a                   8.6237(9)
_cell_length_b                   8.9142(10)
_cell_length_c                   10.2301(8)
_cell_measurement_reflns_used    3033
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.6480
_cell_measurement_theta_min      3.5080
_cell_volume                     748.09(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.8548
_diffrn_measurement_details
;
  1 omega   -2.00   89.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       19.9032   57.0000    0.0000 91

  2 omega   60.00   89.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       19.9032   57.0000 -150.0000 29

  3 omega  -11.00   91.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       19.9032   77.0000   60.0000 102

  4 omega  -20.00   63.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       19.9032  -99.0000 -150.0000 83

  5 omega  -41.00   17.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       19.9032  -57.0000  -90.0000 58

  6 omega  -56.00  -21.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -      -19.9032  -57.0000   90.0000 35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0180732000
_diffrn_orient_matrix_UB_12      0.0792417000
_diffrn_orient_matrix_UB_13      -0.0171584000
_diffrn_orient_matrix_UB_21      -0.0807248000
_diffrn_orient_matrix_UB_22      0.0256794000
_diffrn_orient_matrix_UB_23      -0.0041866000
_diffrn_orient_matrix_UB_31      -0.0050689000
_diffrn_orient_matrix_UB_32      -0.0030506000
_diffrn_orient_matrix_UB_33      0.0702569000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5795
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0410P)^2^+0.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                2877
_reflns_number_total             3425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ta10521h1.cif
_cod_data_source_block           BiPy-PA
_cod_original_cell_volume        748.10(13)
_cod_database_code               7236141
_chemical_oxdiff_formula         'C10 H5 O4 N2 P2'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H4 of C4, {H3A,H3B} of N3, H9 of C9, H2A of C2, H5 of C5, H10 of C10, H7 of
  C7, {H4A,H4B} of N4
 At 1.5 times of:
  H2B of O2, H1 of O1, H5A of O5, H6 of O6
2.a Rotating group:
 N4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C9(H9), C2(H2A), C5(H5), C10(H10)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2B), O1(H1), O5(H5A), O6(H6)
;