#------------------------------------------------------------------------------
#$Date: 2016-12-19 12:49:07 +0200 (Mon, 19 Dec 2016) $
#$Revision: 189226 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/72/7227283.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7227283
loop_
_publ_author_name
'Ye, Yingxiang'
'Wu, Xiuzhen'
'Yao, Zizhu'
'Wu, Ling'
'Cai, Zetao'
'Wang, Lihua'
'Ma, Xiuling'
'Chen, Qian-Huo'
'Zhang, Zhangjing'
'Xiang, Shengchang'
_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 Â°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
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -117.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1999  -77.0000  -90.0000 108

#__ type_ start__ end____ width___ exp.time_
  2 omega -117.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1999  -77.0000 -180.0000 108

#__ type_ start__ end____ width___ exp.time_
  3 omega -101.00   -8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1999  135.0000  -56.0000 93

#__ type_ start__ end____ width___ exp.time_
  4 omega   33.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615 -125.0000 -150.0000 88

#__ type_ start__ end____ width___ exp.time_
  5 omega   94.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  125.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
  6 omega   30.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000   90.0000 61

#__ type_ start__ end____ width___ exp.time_
  7 omega   81.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   45.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
  8 omega   48.00  126.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615 -135.0000  146.0000 78

#__ type_ start__ end____ width___ exp.time_
  9 omega   40.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000    0.0000 46

#__ type_ start__ end____ width___ exp.time_
 10 omega   82.00  172.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   45.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
 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       'ω 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/[σ²(Fo²)+(0.0577P)²]
 where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_date_sample_data_collection 2015-06-23
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.0000 0.5000 0.5000 0.0364(2) Uani 1 2 d S T P . .
Zn2 Zn 0.72176(6) 0.48055(2) 0.03582(8) 0.03655(18) Uani 1 1 d . . . . .
O1 O 1.0241(4) 0.54365(15) 0.2665(5) 0.0501(8) Uani 1 1 d . . . . .
O4 O 0.8116(4) 0.39021(14) 0.0772(4) 0.0438(7) Uani 1 1 d . . . . .
O3 O 1.0393(4) 0.59369(14) 0.6229(5) 0.0482(8) Uani 1 1 d . . . . .
O2 O 0.8098(4) 0.56845(15) 0.0041(5) 0.0513(8) Uani 1 1 d . . . . .
N1 N 0.7414(4) 0.52400(17) 0.3983(5) 0.0404(8) Uani 1 1 d . . . . .
N2 N 0.6361(4) 0.50825(17) 0.2294(5) 0.0363(7) Uani 1 1 d . . . . .
N3 N 0.5160(4) 0.46660(18) -0.1996(5) 0.0431(9) Uani 1 1 d . . . . .
C8 C 0.8419(5) 0.2484(2) 0.1436(6) 0.0411(10) Uani 1 1 d . . . . .
H8 H 0.7477 0.2621 0.0421 0.049 Uiso 1 1 calc R . . . .
C9 C 0.8789(5) 0.18053(19) 0.1754(6) 0.0413(10) Uani 1 1 d . . . . .
H9 H 0.8079 0.1487 0.0958 0.050 Uiso 1 1 calc R . . . .
C7 C 1.0873(5) 0.2751(2) 0.4138(6) 0.0439(11) Uani 1 1 d . . . . .
H7 H 1.1569 0.3070 0.4944 0.053 Uiso 1 1 calc R . . . .
C10 C 1.1251(5) 0.2072(2) 0.4439(6) 0.0446(11) Uani 1 1 d . . . . .
H10 H 1.2206 0.1937 0.5440 0.054 Uiso 1 1 calc R . . . .
C5 C 0.9038(5) 0.37001(19) 0.2377(6) 0.0359(9) Uani 1 1 d . . . . .
C3 C 0.9367(5) 0.5855(2) 0.1486(7) 0.0425(10) Uani 1 1 d . . . . .
C6 C 0.9456(5) 0.29607(19) 0.2633(6) 0.0378(9) Uani 1 1 d . . . . .
C4 C 0.9790(5) 0.65890(19) 0.1748(6) 0.0375(9) Uani 1 1 d . . . . .
C1 C 0.3405(5) 0.4414(3) -0.4769(7) 0.0535(12) Uani 1 1 d . . . . .
H1 H 0.2960 0.4244 -0.5956 0.064 Uiso 1 1 calc R . . . .
C2 C 0.5051(5) 0.4349(3) -0.3506(7) 0.0606(15) Uani 1 1 d . . . . .
H2 H 0.5917 0.4126 -0.3682 0.073 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Zn1 O1 180.0 3_766 .
O3 Zn1 O1 89.78(13) 3_766 3_766
O3 Zn1 O1 90.22(13) 3_766 .
O3 Zn1 O1 89.78(13) . .
O3 Zn1 O1 90.22(13) . 3_766
O3 Zn1 O3 180.0 3_766 .
O3 Zn1 N1 94.17(12) . 3_766
O3 Zn1 N1 85.83(12) 3_766 3_766
O3 Zn1 N1 94.17(12) 3_766 .
O3 Zn1 N1 85.83(12) . .
N1 Zn1 O1 92.10(14) . .
N1 Zn1 O1 87.90(14) . 3_766
N1 Zn1 O1 92.10(14) 3_766 3_766
N1 Zn1 O1 87.90(14) 3_766 .
N1 Zn1 N1 180.00(7) . 3_766
O4 Zn2 O2 134.02(14) . .
O4 Zn2 N2 111.44(14) . .
O4 Zn2 N3 100.25(13) . .
O2 Zn2 N2 98.05(15) . .
O2 Zn2 N3 104.22(15) . .
N3 Zn2 N2 106.56(14) . .
C3 O1 Zn1 132.7(3) . .
C5 O4 Zn2 120.8(3) . .
C5 O3 Zn1 150.8(3) 3_766 .
C3 O2 Zn2 110.9(3) . .
N2 N1 Zn1 121.9(3) . .
C1 N1 Zn1 129.0(3) 3_665 .
C1 N1 N2 108.9(3) 3_665 .
N1 N2 Zn2 121.4(3) . .
N1 N2 N3 108.6(4) . 3_665
N3 N2 Zn2 126.8(3) 3_665 .
N2 N3 Zn2 123.5(3) 3_665 .
C2 N3 Zn2 128.4(3) . .
C2 N3 N2 108.1(3) . 3_665
C9 C8 H8 120.1 . .
C9 C8 C6 119.8(4) . .
C6 C8 H8 120.1 . .
C8 C9 H9 119.5 . .
C8 C9 C4 121.1(4) . 2_745
C4 C9 H9 119.5 2_745 .
C10 C7 H7 119.8 . .
C10 C7 C6 120.4(4) . .
C6 C7 H7 119.8 . .
C7 C10 H10 119.8 . .
C7 C10 C4 120.4(4) . 2_745
C4 C10 H10 119.8 2_745 .
O4 C5 C6 117.6(3) . .
O3 C5 O4 125.5(4) 3_766 .
O3 C5 C6 116.9(4) 3_766 .
O1 C3 O2 123.0(4) . .
O1 C3 C4 119.8(4) . .
O2 C3 C4 117.2(4) . .
C8 C6 C7 119.7(4) . .
C8 C6 C5 121.0(3) . .
C7 C6 C5 119.3(3) . .
C9 C4 C3 120.1(4) 2_755 .
C10 C4 C9 118.7(4) 2_755 2_755
C10 C4 C3 121.2(4) 2_755 .
N1 C1 H1 126.3 3_665 .
N1 C1 C2 107.4(4) 3_665 .
C2 C1 H1 126.3 . .
N3 C2 C1 107.0(4) . .
N3 C2 H2 126.5 . .
C1 C2 H2 126.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.141(4) .
Zn1 O1 2.141(4) 3_766
Zn1 O3 2.061(3) .
Zn1 O3 2.061(3) 3_766
Zn1 N1 2.112(3) .
Zn1 N1 2.112(3) 3_766
Zn2 O4 1.925(3) .
Zn2 O2 1.957(3) .
Zn2 N2 2.042(4) .
Zn2 N3 2.024(3) .
O1 C3 1.253(5) .
O4 C5 1.271(5) .
O3 C5 1.247(5) 3_766
O2 C3 1.278(6) .
N1 N2 1.326(5) .
N1 C1 1.316(6) 3_665
N2 N3 1.340(5) 3_665
N3 N2 1.340(5) 3_665
N3 C2 1.328(6) .
C8 H8 0.9300 .
C8 C9 1.380(5) .
C8 C6 1.386(6) .
C9 H9 0.9300 .
C9 C4 1.395(6) 2_745
C7 H7 0.9300 .
C7 C10 1.381(6) .
C7 C6 1.392(6) .
C10 H10 0.9300 .
C10 C4 1.392(6) 2_745
C5 O3 1.247(5) 3_766
C5 C6 1.501(5) .
C3 C4 1.493(5) .
C4 C9 1.395(6) 2_755
C4 C10 1.392(6) 2_755
C1 N1 1.316(6) 3_665
C1 H1 0.9300 .
C1 C2 1.384(6) .
C2 H2 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Zn1 O1 C3 O2 -86.2(6) . . . .
Zn1 O1 C3 C4 93.5(5) . . . .
Zn1 N1 N2 Zn2 -14.9(4) . . . .
Zn1 N1 N2 N3 -176.1(3) . . . 3_665
Zn2 O4 C5 O3 -8.6(6) . . . 3_766
Zn2 O4 C5 C6 170.2(3) . . . .
Zn2 O2 C3 O1 21.6(6) . . . .
Zn2 O2 C3 C4 -158.1(3) . . . .
Zn2 N3 C2 C1 -177.2(4) . . . .
O1 C3 C4 C9 3.7(7) . . . 2_755
O1 C3 C4 C10 -173.5(5) . . . 2_755
O4 C5 C6 C8 -24.7(7) . . . .
O4 C5 C6 C7 157.8(4) . . . .
O3 C5 C6 C8 154.2(5) 3_766 . . .
O3 C5 C6 C7 -23.4(6) 3_766 . . .
O2 C3 C4 C9 -176.6(5) . . . 2_755
O2 C3 C4 C10 6.1(7) . . . 2_755
N1 C1 C2 N3 -0.4(7) 3_665 . . .
N2 N3 C2 C1 0.3(6) 3_665 . . .
C9 C8 C6 C7 0.7(7) . . . .
C9 C8 C6 C5 -176.8(4) . . . .
C10 C7 C6 C8 0.1(8) . . . .
C10 C7 C6 C5 177.7(4) . . . .
C6 C8 C9 C4 -1.0(8) . . . 2_745
C6 C7 C10 C4 -0.7(8) . . . 2_745
C1 N1 N2 Zn2 161.2(3) 3_665 . . .
C1 N1 N2 N3 0.1(5) 3_665 . . 3_665
