Encapsulating Mobile Proton Carriers into Structural Defects in Coordination Polymer Crystals: High Anhydrous Proton Conduction and Fuel Cell Application.
Inukai, Munehiro; Horike, Satoshi; Itakura, Tomoya; Shinozaki, Ryota; Ogiwara, Naoki; Umeyama, Daiki; Nagarkar, Sanjog S.; Nishiyama, Yusuke; Malon, Michal; Hayashi, Akari; Ohhara, Takashi; Kiyanagi, Ryoji; Kitagawa, Susumu; Journal of the American Chemical Society 138 (2016) 8505–8511; doi:10.1021/jacs.6b03625

data_4130444
_publ_section_title
;
 Encapsulating Mobile Proton Carriers into Structural Defects in
 Coordination Polymer Crystals: High Anhydrous Proton Conduction and Fuel
 Cell Application.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8505
_journal_page_last               8511
_journal_paper_doi               10.1021/jacs.6b03625
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C2 H5 N3 O4 P Zn0.5'
_chemical_formula_weight         198.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.4676(18)
_cell_length_b                   9.549(2)
_cell_length_c                   15.570(3)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    77
_cell_measurement_theta_max      83.3
_cell_measurement_theta_min      6.6
_cell_volume                     1258.9(4)
_computing_cell_refinement       'STARGazer (Ohhara, 2009)'
_computing_data_collection       'STARGazer (Ohhara, 2009)'
_computing_data_reduction
'STARGazer (Ohhara, 2009) & Jana2006 (Petricek, Dusek & Palatinus, 2006)'
_computing_structure_refinement
'Jana2006 (Petricek, Dusek & Palatinus, 2006) & SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      77
_diffrn_detector_area_resol_mean '4 mm'
_diffrn_measured_fraction_theta_full 0.716
_diffrn_measured_fraction_theta_max 0.591
_diffrn_measurement_device_type
'single-crystal diffractometer SENJU at the BL18 in the MLF of the J-PARC'
_diffrn_measurement_method       'wavelength resolved TOF Laue'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     1.0
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.716
_diffrn_reflns_Laue_measured_fraction_max 0.591
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3661
_diffrn_reflns_point_group_measured_fraction_full 0.716
_diffrn_reflns_point_group_measured_fraction_max 0.591
_diffrn_reflns_theta_full        44.95
_diffrn_reflns_theta_max         83.3
_diffrn_reflns_theta_min         6.6
_diffrn_source                   J-PARC/MLF
_exptl_absorpt_coefficient_mu    0.31
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             430.8984
_exptl_crystal_size_max          2.0
_exptl_crystal_size_mid          2.0
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.355
_refine_ls_extinction_coef       0.6(2)
_refine_ls_extinction_method
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         1820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+31.2219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1806
_reflns_number_total             1820
_reflns_threshold_expression     'I > 3\s(I)'
_cod_data_source_file            ja6b03625_si_002.cif
_cod_data_source_block           neutron77K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C2 H5 N3 O4 P Zn0.50'
_cod_database_code               4130444
_shelxl_version_number           2014-3
_shelx_res_checksum              80763
_shelx_hkl_checksum              86061