Exploration of new water stable proton-conducting materials in an amino acid-templated metal phosphate system.
Shi, Jingyu; Wang, Kangcai; Li, Jing; Zeng, Hongmei; Zhang, Qinghua; Lin, Zhien; Dalton transactions (Cambridge, England : 2003) 47 (2018) 654–658; doi:10.1039/c7dt04125j

data_7044906
_publ_section_title
;
 Exploration of new water stable proton-conducting materials in an amino
 acid-templated metal phosphate system.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              654
_journal_page_last               658
_journal_paper_doi               10.1039/c7dt04125j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C3 H8 N O6 P Zn'
_chemical_formula_sum            'C3 H8 N O6 P Zn'
_chemical_formula_weight         250.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-02 deposited with the CCDC.
2017-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.663(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3358(3)
_cell_length_b                   5.14807(13)
_cell_length_c                   15.4325(4)
_cell_measurement_reflns_used    2127
_cell_measurement_temperature    296.65(10)
_cell_measurement_theta_max      72.0320
_cell_measurement_theta_min      5.7430
_cell_volume                     739.25(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.65(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000  150.0000 94

  2 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000 -120.0000 84

  3 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000 -120.0000 74

  4 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  -90.0000 94

  5 omega    7.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   19.0000 -120.0000 101

  6 omega   87.00  178.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 91

  7 omega   40.00   98.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

  8 omega  100.00  178.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 78

  9 omega   38.00   91.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 10 omega   91.00  176.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85

 11 omega   39.00  109.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 70

 12 omega   39.00  109.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 70

 13 omega   38.00   91.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 14 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  120.0000 84

 15 omega   22.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -123.0000   73.0000 67

 16 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -180.0000 94

 17 omega  -31.00   51.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000   60.0000 82

 18 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000   30.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1563148000
_diffrn_orient_matrix_UB_12      -0.0066559000
_diffrn_orient_matrix_UB_13      0.0405517000
_diffrn_orient_matrix_UB_21      0.0546060000
_diffrn_orient_matrix_UB_22      0.0269105000
_diffrn_orient_matrix_UB_23      -0.0911522000
_diffrn_orient_matrix_UB_31      -0.0015274000
_diffrn_orient_matrix_UB_32      0.2978587000
_diffrn_orient_matrix_UB_33      0.0090927000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4055
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         4.752
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0729P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1197
_reflns_number_total             1319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04125j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7044906--7044907.cif.'
_cod_original_cell_volume        739.25(3)
_cod_database_code               7044906
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'