#------------------------------------------------------------------------------
#$Date: 2016-12-19 12:49:07 +0200 (Mon, 19 Dec 2016) $
#$Revision: 189226 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/72/7227280.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_7227280
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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-29
_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                112.294(16)
_cell_angle_beta                 99.494(9)
_cell_angle_gamma                99.046(9)
_cell_formula_units_Z            2
_cell_length_a                   9.2142(6)
_cell_length_b                   11.1531(19)
_cell_length_c                   11.3582(19)
_cell_measurement_reflns_used    1538
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.0280
_cell_measurement_theta_min      4.3110
_cell_volume                     1033.8(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9456
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.440
_diffrn_reflns_theta_min         4.340
_exptl_absorpt_coefficient_mu    2.336
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.556
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0835
_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/[σ²(Fo²)+(0.1014P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2582
_reflns_number_total             4047
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ta10765b2.cif
_cod_data_source_block           FJU-31-Ch
_cod_original_formula_sum        'C10 H6 N3 O4 Zn1.50'
_cod_database_code               7227280
_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   0.800
_shelx_estimated_absorpt_t_min   0.652
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4(H4), C8(H8), C10(H10), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Zn2 Zn 0.18384(8) 0.61180(10) 0.11164(8) 0.0407(3) Uani 1 1 d . . . . .
Zn1 Zn 0.5000 0.5000 0.0000 0.0380(3) Uani 1 2 d S T P . .
O4 O 0.2805(6) 0.5946(7) 0.2657(5) 0.0655(16) Uani 1 1 d . . . . .
O2 O 0.2680(6) 0.7736(6) 0.0949(6) 0.0629(15) Uani 1 1 d . . . . .
N2 N 0.8443(5) 0.5505(6) 0.0537(5) 0.0369(11) Uani 1 1 d . . . . .
C7 C 0.5639(9) 0.4561(12) 0.3949(8) 0.076(3) Uani 1 1 d . . . . .
H7 H 0.6073 0.4264 0.3239 0.091 Uiso 1 1 calc R . . . .
O1 O 0.4607(7) 0.6908(7) 0.0429(7) 0.0741(17) Uani 1 1 d . . . . .
O3 O 0.4588(6) 0.5033(8) 0.1752(5) 0.0724(19) Uani 1 1 d . . . . .
C3 C 0.5669(10) 0.8937(10) -0.0314(11) 0.071(3) Uani 1 1 d . . . . .
H3 H 0.6115 0.8215 -0.0535 0.086 Uiso 1 1 calc R . . . .
N3 N 0.7302(6) 0.5959(7) 0.1010(6) 0.0484(14) Uani 1 1 d . . . . .
C4 C 0.3799(10) 0.9986(10) 0.0571(11) 0.077(3) Uani 1 1 d . . . . .
H4 H 0.2978 0.9975 0.0950 0.093 Uiso 1 1 calc R . . . .
C8 C 0.3853(10) 0.5660(13) 0.4948(9) 0.079(3) Uani 1 1 d . . . . .
H8 H 0.3083 0.6104 0.4919 0.095 Uiso 1 1 calc R . . . .
N1 N -0.0240(5) 0.6328(7) 0.1386(5) 0.0487(14) Uani 1 1 d . . . . .
C6 C 0.4493(7) 0.5220(9) 0.3898(7) 0.0538(19) Uani 1 1 d . . . . .
C2 C 0.4465(7) 0.8932(8) 0.0274(8) 0.0517(17) Uani 1 1 d . . . . .
C1 C 0.3898(8) 0.7754(8) 0.0577(8) 0.0547(18) Uani 1 1 d . . . . .
C5 C 0.3936(7) 0.5431(8) 0.2672(6) 0.0489(17) Uani 1 1 d . . . . .
C10 C -0.0616(10) 0.7221(11) 0.2353(9) 0.086(4) Uani 1 1 d . . . . .
H10 H 0.0063 0.7892 0.3098 0.104 Uiso 1 1 calc R . . . .
C9 C 0.7888(10) 0.7020(11) 0.2106(9) 0.082(3) Uani 1 1 d . . . . .
H9 H 0.7348 0.7546 0.2625 0.099 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
O4 Zn2 O2 115.8(3) . .
O4 Zn2 N2 113.2(3) . 2_665
O4 Zn2 N1 103.9(2) . .
O2 Zn2 N2 111.7(2) . 2_665
O2 Zn2 N1 103.2(3) . .
N2 Zn2 N1 107.9(2) 2_665 .
O1 Zn1 O1 180.0 2_665 .
O1 Zn1 N3 87.5(3) 2_665 2_665
O1 Zn1 N3 92.5(3) . 2_665
O1 Zn1 N3 87.5(3) . .
O1 Zn1 N3 92.5(3) 2_665 .
O3 Zn1 O1 88.0(3) 2_665 .
O3 Zn1 O1 92.0(3) 2_665 2_665
O3 Zn1 O1 88.0(3) . 2_665
O3 Zn1 O1 92.0(3) . .
O3 Zn1 O3 180.0 . 2_665
O3 Zn1 N3 88.4(2) . .
O3 Zn1 N3 88.4(2) 2_665 2_665
O3 Zn1 N3 91.6(2) 2_665 .
O3 Zn1 N3 91.6(2) . 2_665
N3 Zn1 N3 180.0 2_665 .
C5 O4 Zn2 121.1(5) . .
C1 O2 Zn2 115.3(5) . .
N3 N2 Zn2 124.2(4) . 2_665
N3 N2 N1 107.7(6) . 1_655
N1 N2 Zn2 128.1(4) 1_655 2_665
C6 C7 C8 120.5(7) . 2_666
C1 O1 Zn1 158.1(6) . .
C5 O3 Zn1 150.1(6) . .
C4 C3 C2 119.8(8) 2_675 .
N2 N3 Zn1 121.6(5) . .
C9 N3 Zn1 130.4(5) . .
C9 N3 N2 108.0(6) . .
C2 C4 C3 120.6(7) . 2_675
C6 C8 C7 119.7(8) . 2_666
N2 N1 Zn2 123.9(5) 1_455 .
C10 N1 Zn2 129.7(5) . .
C10 N1 N2 106.4(6) . 1_455
C7 C6 C5 119.6(6) . .
C8 C6 C7 119.8(7) . .
C8 C6 C5 120.6(7) . .
C3 C2 C1 119.7(7) . .
C4 C2 C3 119.6(7) . .
C4 C2 C1 120.7(7) . .
O2 C1 C2 115.9(7) . .
O1 C1 O2 125.2(7) . .
O1 C1 C2 118.9(7) . .
O4 C5 C6 115.9(6) . .
O3 C5 O4 126.2(6) . .
O3 C5 C6 117.8(6) . .
N1 C10 C9 109.6(7) . 1_455
N3 C9 C10 108.3(7) . 1_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn2 O4 1.920(5) .
Zn2 O2 1.939(5) .
Zn2 N2 1.996(6) 2_665
Zn2 N1 2.024(5) .
Zn1 O1 2.100(6) 2_665
Zn1 O1 2.100(6) .
Zn1 O3 2.075(5) .
Zn1 O3 2.075(5) 2_665
Zn1 N3 2.124(5) .
Zn1 N3 2.124(5) 2_665
O4 C5 1.267(9) .
O2 C1 1.262(9) .
N2 Zn2 1.996(6) 2_665
N2 N3 1.340(7) .
N2 N1 1.355(7) 1_655
C7 C8 1.388(11) 2_666
C7 C6 1.384(11) .
O1 C1 1.206(11) .
O3 C5 1.261(9) .
C3 C4 1.377(12) 2_675
C3 C2 1.386(10) .
N3 C9 1.305(10) .
C4 C3 1.377(12) 2_675
C4 C2 1.366(13) .
C8 C7 1.388(11) 2_666
C8 C6 1.374(11) .
N1 N2 1.355(7) 1_455
N1 C10 1.313(11) .
C6 C5 1.519(9) .
C2 C1 1.519(10) .
C10 C9 1.325(13) 1_455
C9 C10 1.325(13) 1_655
