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_7236140
_publ_section_title
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 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, H O4 P, H2 O'
_chemical_formula_sum            'C10 H15 N4 O5 P'
_chemical_formula_weight         302.23
_chemical_name_common            BPY@PA
_chemical_name_systematic
'2,2'-bipyridinium-5,5'-diamino hydrogen Phosphate monohydreate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-31
_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                90.00
_cell_angle_beta                 100.972(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9672(5)
_cell_length_b                   4.22937(14)
_cell_length_c                   24.0975(8)
_cell_measurement_reflns_used    2682
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.0540
_cell_measurement_theta_min      3.9040
_cell_volume                     1297.42(8)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.8586
_diffrn_measurement_details
;
  1 omega   14.00   89.00   1.0000   26.3000
omega____ theta____ kappa____ phi______ frames
    -       19.9032   57.0000  -90.0000 75

  2 omega   51.00   97.00   1.0000   26.3000
omega____ theta____ kappa____ phi______ frames
    -       19.9032  178.0000   90.0000 46

  3 omega    3.00   44.00   1.0000   26.3000
omega____ theta____ kappa____ phi______ frames
    -       19.9032   57.0000  120.0000 41

  4 omega   -9.00   58.00   1.0000   26.3000
omega____ theta____ kappa____ phi______ frames
    -       19.9032  -99.0000 -180.0000 67
;
_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      0.0202217000
_diffrn_orient_matrix_UB_12      0.1472884000
_diffrn_orient_matrix_UB_13      0.0112288000
_diffrn_orient_matrix_UB_21      -0.0364425000
_diffrn_orient_matrix_UB_22      0.0002551000
_diffrn_orient_matrix_UB_23      0.0185416000
_diffrn_orient_matrix_UB_31      0.0369534000
_diffrn_orient_matrix_UB_32      -0.0801781000
_diffrn_orient_matrix_UB_33      0.0207279000
_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  0.0223
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            5075
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91424
_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    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.5281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                2480
_reflns_number_total             2944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ta10521h1.cif
_cod_data_source_block           BPY@PA
_cod_database_code               7236140
_chemical_oxdiff_formula         'C10 H15 N4 O5 P'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Sof: O5(0.5) O1(0.5) O4(0.5) O2(0.5) O6(0.5) O7(0.5) O8(0.5) O9(0.5)
;