Metal‒organic frameworks with a large breathing effect to host hydroxyl compounds for high anhydrous proton conductivity over a wide temperature range from subzero to 125 Â°C
Ye, Yingxiang; Wu, Xiuzhen; Yao, Zizhu; Wu, Ling; Cai, Zetao; Wang, Lihua; Ma, Xiuling; Chen, Qian-Huo; Zhang, Zhangjing; Xiang, Shengchang; J. Mater. Chem. A 4 (2016) 4062–4070; doi:10.1039/c5ta10765b

data_7227283
_publ_section_title
;
 Metal--organic frameworks with a large breathing effect to host hydroxyl
 compounds for high anhydrous proton conductivity over a wide temperature
 range from subzero to 125 \^A\%C
;
_journal_issue                   11
_journal_name_full               'J. Mater. Chem. A'
_journal_page_first              4062
_journal_page_last               4070
_journal_paper_doi               10.1039/c5ta10765b
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C10 H6 N3 O4 Zn1.5'
_chemical_formula_sum            'C10 H6 N3 O4 Zn1.5'
_chemical_formula_weight         330.23
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2015-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-12 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.775(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6854(5)
_cell_length_b                   19.7877(8)
_cell_length_c                   7.9849(5)
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.2880
_cell_measurement_theta_min      4.4250
_cell_volume                     1255.86(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details
;
  1 omega -117.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1999  -77.0000  -90.0000 108

  2 omega -117.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1999  -77.0000 -180.0000 108

  3 omega -101.00   -8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1999  135.0000  -56.0000 93

  4 omega   33.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615 -125.0000 -150.0000 88

  5 omega   94.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  125.0000  120.0000 84

  6 omega   30.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000   90.0000 61

  7 omega   81.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   45.0000 -120.0000 97

  8 omega   48.00  126.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615 -135.0000  146.0000 78

  9 omega   40.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000    0.0000 46

 10 omega   82.00  172.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   45.0000  120.0000 90

 11 omega   32.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -77.0000   30.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0818286000
_diffrn_orient_matrix_UB_12      0.0229067000
_diffrn_orient_matrix_UB_13      0.2012877000
_diffrn_orient_matrix_UB_21      -0.0594143000
_diffrn_orient_matrix_UB_22      0.0729129000
_diffrn_orient_matrix_UB_23      -0.0589394000
_diffrn_orient_matrix_UB_31      -0.1653852000
_diffrn_orient_matrix_UB_32      -0.0148486000
_diffrn_orient_matrix_UB_33      0.0211289000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7142
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.997
_diffrn_reflns_theta_min         4.469
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.845
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0577P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1803
_reflns_number_total             2401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ta10765b2.cif
_cod_data_source_block           FJU-31
_cod_original_cell_volume        1255.86(13)
_cod_original_formula_sum        'C10 H6 N3 O4 Zn1.50'
_cod_database_code               7227283
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.513
_reflns_odcompleteness_completeness 94.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.83
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C7(H7), C10(H10), C1(H1), C2(H2)
;
_shelx_res_checksum              825
_olex2_date_sample_data_collection 2015-06-23
_olex2_submission_special_instructions 'No special instructions were received'