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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/47/4104729.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_4104729
loop_
_publ_author_name
'Masaaki Sadakiyo'
'Teppei Yamada'
'Hiroshi Kitagawa'
_publ_section_title
;
 Rational Designs for Highly Proton-Conductive Metal-Organic Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9906
_journal_page_last               9907
_journal_paper_doi               10.1021/ja9040016
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C12 H24 N2 O19 Zn2 '
_chemical_formula_sum            'C12 H24 N2 O19 Zn2'
_chemical_formula_weight         631.08
_chemical_name_common            (NH4)2(adp)[Zn2(ox)3](H2O)3
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'by CrystalStructure 3.8.0'
_cell_angle_alpha                62.025(6)
_cell_angle_beta                 82.335(7)
_cell_angle_gamma                72.873(7)
_cell_formula_units_Z            1
_cell_length_a                   7.98580(10)
_cell_length_b                   9.1574(2)
_cell_length_c                   9.4523
_cell_measurement_reflns_used    1735
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     583.39(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4330
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    2.148
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       block
_exptl_crystal_F_000             322.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.29
_refine_diff_density_min         -1.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_hydrogen_treatment    none
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2497
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1138P)²+0.0638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                2315
_reflns_number_total             2497
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja9040016_si_002.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C12 H24 N2 O19 Zn2 '
_cod_database_code               4104729
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn(1) Zn 1.00796(6) -0.16815(5) 0.82516(5) 0.0144(2) Uani 1.00 1 d .
O(1) O 1.1597(3) -0.1752(3) 0.6298(3) 0.0172(6) Uani 1.00 1 d .
O(2) O 1.1646(3) -0.4029(3) 0.9860(3) 0.0178(6) Uani 1.00 1 d .
O(3) O 0.8567(3) -0.1133(3) 1.0033(3) 0.0173(6) Uani 1.00 1 d .
O(4) O 0.8497(3) -0.3274(3) 0.8586(3) 0.0175(6) Uani 1.00 1 d .
O(5) O 1.1494(3) -0.0281(3) 0.8566(3) 0.0188(6) Uani 1.00 1 d .
O(8) O 0.6077(4) 0.7957(4) 0.5414(4) 0.0287(7) Uani 1.00 1 d .
O(7) O 0.4629(4) 0.5919(4) 0.6418(5) 0.0346(8) Uani 1.00 1 d .
O(6) O 0.8467(3) 0.0362(3) 0.6384(3) 0.0164(5) Uani 1.00 1 d .
O(10) O 0.5061(8) 0.3805(8) 0.9970(8) 0.0315(15) Uani 0.50 1 d P
O(9) O 0.4455(5) 0.2232(5) 0.8438(6) 0.0613(15) Uani 1.00 1 d .
N(1) N 0.4840(4) 0.0564(4) 1.2311(4) 0.0220(7) Uani 1.00 1 d .
C(1) C 1.0911(4) -0.5216(4) 1.0366(4) 0.0138(7) Uani 1.00 1 d .
C(2) C 0.9153(4) -0.0247(4) 1.0424(4) 0.0135(7) Uani 1.00 1 d .
C(4) C 0.6082(6) 0.6464(5) 0.5872(5) 0.0255(9) Uani 1.00 1 d .
C(5) C 0.7677(6) 0.5055(5) 0.5937(6) 0.0292(10) Uani 1.00 1 d .
C(3) C 0.9098(4) 0.0603(4) 0.5035(4) 0.0143(7) Uani 1.00 1 d .
C(6) C 0.9222(6) 0.5718(6) 0.5011(6) 0.0275(9) Uani 1.00 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Zn Zn 0.284 1.430
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O(1) Zn(1) O(2) 92.49(11) yes . .
O(1) Zn(1) O(3) 169.33(12) yes . .
O(1) Zn(1) O(4) 101.92(14) yes . .
O(1) Zn(1) O(5) 92.34(13) yes . .
O(1) Zn(1) O(6) 80.29(10) yes . .
O(2) Zn(1) O(3) 95.04(11) yes . .
O(2) Zn(1) O(4) 80.30(12) yes . .
O(2) Zn(1) O(5) 93.20(13) yes . .
O(2) Zn(1) O(6) 167.34(16) yes . .
O(3) Zn(1) O(4) 86.82(14) yes . .
O(3) Zn(1) O(5) 79.72(13) yes . .
O(3) Zn(1) O(6) 93.59(11) yes . .
O(4) Zn(1) O(5) 164.51(12) yes . .
O(4) Zn(1) O(6) 90.96(12) yes . .
O(5) Zn(1) O(6) 97.45(12) yes . .
Zn(1) O(1) C(3) 113.0(2) yes . 2_756
Zn(1) O(2) C(1) 112.6(2) yes . .
Zn(1) O(3) C(2) 112.8(2) yes . .
Zn(1) O(4) C(1) 112.7(3) yes . 2_747
Zn(1) O(5) C(2) 113.9(2) yes . 2_757
Zn(1) O(6) C(3) 112.7(2) yes . .
O(2) C(1) O(4) 126.0(3) yes . 2_747
O(2) C(1) C(1) 117.3(2) yes . 2_747
O(4) C(1) C(1) 116.7(3) yes 2_747 2_747
O(3) C(2) O(5) 126.4(3) yes . 2_757
O(3) C(2) C(2) 116.9(3) yes . 2_757
O(5) C(2) C(2) 116.7(4) yes 2_757 2_757
O(8) C(4) O(7) 121.9(4) yes . .
O(8) C(4) C(5) 124.8(4) yes . .
O(7) C(4) C(5) 113.2(4) yes . .
C(4) C(5) C(6) 113.2(4) yes . .
O(1) C(3) O(6) 126.0(3) yes 2_756 .
O(1) C(3) C(3) 116.3(3) yes 2_756 2_756
O(6) C(3) C(3) 117.7(2) yes . 2_756
C(5) C(6) C(6) 112.4(4) yes . 2_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Zn(1) O(1) 2.086(3) yes .
Zn(1) O(2) 2.087(2) yes .
Zn(1) O(3) 2.107(3) yes .
Zn(1) O(4) 2.091(3) yes .
Zn(1) O(5) 2.076(4) yes .
Zn(1) O(6) 2.089(2) yes .
O(1) C(3) 1.266(4) yes 2_756
O(2) C(1) 1.252(5) yes .
O(3) C(2) 1.251(6) yes .
O(4) C(1) 1.254(3) yes 2_747
O(5) C(2) 1.252(5) yes 2_757
O(8) C(4) 1.224(6) yes .
O(7) C(4) 1.342(6) yes .
O(6) C(3) 1.248(5) yes .
C(1) C(1) 1.557(5) yes 2_747
C(2) C(2) 1.552(5) yes 2_757
C(4) C(5) 1.506(6) yes .
C(5) C(6) 1.520(7) yes .
C(3) C(3) 1.551(5) yes 2_756
C(6) C(6) 1.527(6) yes 2_766
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O(1) O(8) 3.524(4) 1_645
O(1) O(7) 2.688(4) 1_645
O(1) C(4) 3.527(5) 1_645
O(2) O(10) 2.842(6) 1_645
O(2) O(10) 2.729(8) 2_757
O(3) O(9) 2.839(5) 2_657
O(3) N(1) 3.503(5) 2_657
O(4) O(8) 3.329(5) 1_545
O(4) O(10) 3.054(7) 2_657
O(4) N(1) 2.951(4) 2_657
O(4) C(4) 3.538(7) 1_545
O(5) O(10) 3.390(6) 2_757
O(5) N(1) 2.904(4) 2_757
O(8) O(1) 3.524(4) 1_465
O(8) O(4) 3.329(5) 1_565
O(8) O(8) 3.375(4) 2_676
O(8) N(1) 2.845(4) 1_564
O(8) N(1) 2.953(6) 2_667
O(7) O(1) 2.688(4) 1_465
O(7) O(10) 2.993(8) .
O(7) O(10) 3.586(10) 2_667
O(7) O(9) 3.037(5) .
O(7) C(3) 3.506(4) 2_666
O(6) N(1) 2.946(4) 2_657
O(10) O(2) 2.842(6) 1_465
O(10) O(2) 2.729(8) 2_757
O(10) O(4) 3.054(7) 2_657
O(10) O(5) 3.390(6) 2_757
O(10) O(7) 2.993(8) .
O(10) O(7) 3.586(10) 2_667
O(10) O(10) 2.189(13) 2_667
O(10) O(9) 2.638(12) .
O(10) N(1) 2.789(7) .
O(10) C(1) 3.188(7) 1_465
O(9) O(3) 2.839(5) 2_657
O(9) O(7) 3.037(5) .
O(9) O(10) 2.638(12) .
O(9) N(1) 3.257(7) .
O(9) N(1) 2.850(7) 2_657
N(1) O(3) 3.503(5) 2_657
N(1) O(4) 2.951(4) 2_657
N(1) O(5) 2.904(4) 2_757
N(1) O(8) 2.845(4) 1_546
N(1) O(8) 2.953(6) 2_667
N(1) O(6) 2.946(4) 2_657
N(1) O(10) 2.789(7) .
N(1) O(9) 3.257(7) .
N(1) O(9) 2.850(7) 2_657
C(1) O(10) 3.188(7) 1_645
C(4) O(1) 3.527(5) 1_465
C(4) O(4) 3.538(7) 1_565
C(3) O(7) 3.506(4) 2_666
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_3
_geom_torsion_site_symmetry_4
O(1) Zn(1) O(2) C(1) -107.1(3) . . .
O(2) Zn(1) O(1) C(3) 169.7(3) . . 2_756
O(1) Zn(1) O(3) C(2) -41.3(7) . . .
O(3) Zn(1) O(1) C(3) -55.4(8) . . 2_756
O(1) Zn(1) O(4) C(1) 96.1(3) . . 2_747
O(4) Zn(1) O(1) C(3) 89.1(3) . . 2_756
O(1) Zn(1) O(5) C(2) 171.7(2) . . 2_757
O(5) Zn(1) O(1) C(3) -97.0(3) . . 2_756
O(1) Zn(1) O(6) C(3) -0.1(3) . . .
O(6) Zn(1) O(1) C(3) 0.2(3) . . 2_756
O(2) Zn(1) O(3) C(2) 93.4(2) . . .
O(3) Zn(1) O(2) C(1) 80.4(3) . . .
O(2) Zn(1) O(4) C(1) 5.6(3) . . 2_747
O(4) Zn(1) O(2) C(1) -5.4(3) . . .
O(2) Zn(1) O(5) C(2) -95.6(2) . . 2_757
O(5) Zn(1) O(2) C(1) 160.4(3) . . .
O(2) Zn(1) O(6) C(3) -56.0(6) . . .
O(6) Zn(1) O(2) C(1) -52.3(6) . . .
O(3) Zn(1) O(4) C(1) -90.1(3) . . 2_747
O(4) Zn(1) O(3) C(2) 173.4(2) . . .
O(3) Zn(1) O(5) C(2) -1.1(2) . . 2_757
O(5) Zn(1) O(3) C(2) 1.1(2) . . .
O(3) Zn(1) O(6) C(3) 171.1(3) . . .
O(6) Zn(1) O(3) C(2) -95.9(2) . . .
O(4) Zn(1) O(5) C(2) -31.1(5) . . 2_757
O(5) Zn(1) O(4) C(1) -60.5(5) . . 2_747
O(4) Zn(1) O(6) C(3) -102.1(3) . . .
O(6) Zn(1) O(4) C(1) 176.4(3) . . 2_747
O(5) Zn(1) O(6) C(3) 91.0(3) . . .
O(6) Zn(1) O(5) C(2) 91.2(2) . . 2_757
Zn(1) O(1) C(3) O(6) 179.9(2) . 2_756 2_756
Zn(1) O(1) C(3) C(3) -0.2(5) . 2_756 .
Zn(1) O(2) C(1) O(4) -175.2(3) . . 2_747
Zn(1) O(2) C(1) C(1) 4.6(5) . . 2_747
Zn(1) O(3) C(2) O(5) 179.1(2) . . 2_757
Zn(1) O(3) C(2) C(2) -0.9(3) . . 2_757
Zn(1) O(4) C(1) O(2) 175.4(3) . 2_747 2_747
Zn(1) O(4) C(1) C(1) -4.8(4) . 2_747 .
Zn(1) O(5) C(2) O(3) -179.1(2) . 2_757 2_757
Zn(1) O(5) C(2) C(2) 1.0(3) . 2_757 .
Zn(1) O(6) C(3) O(1) -179.8(3) . . 2_756
Zn(1) O(6) C(3) C(3) 0.1(4) . . 2_756
O(2) C(1) C(1) O(4) 0.2(5) . 2_747 .
O(4) C(1) C(1) O(2) -0.2(5) 2_747 2_747 2_747
O(3) C(2) C(2) O(5) -0.0(3) . 2_757 .
O(5) C(2) C(2) O(3) 0.0(3) 2_757 2_757 2_757
O(8) C(4) C(5) C(6) -13.8(8) . . .
O(7) C(4) C(5) C(6) 167.9(5) . . .
C(4) C(5) C(6) C(6) -175.9(5) . . 2_766
O(1) C(3) C(3) O(6) -0.1(5) 2_756 2_756 2_756
O(6) C(3) C(3) O(1) 0.1(5) . 2_756 .
