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#$Date: 2016-03-21 18:22:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178810 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/64/4106451.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_4106451
loop_
_publ_author_name
'Masaaki Sadakiyo'
'Teppei Yamada'
'Hiroshi Kitagawa'
_publ_contact_author_address
;
    Department of Chemistry
    Graduate School of Science
    Kyoto University
    Kitashirakawa-Oiwakecho
    Sakyo-ku, Kyoto, Japan
;
_publ_contact_author_email       sadakiyo@kuchem.kyoto-u.ac.jp
_publ_contact_author_fax         +81-92-642-2570
_publ_contact_author_name        'Masaaki Sadakiyo'
_publ_contact_author_phone       +81-92-642-2570
_publ_section_title
;
 Hydroxyl Group Recognition by Hydrogen-Bonding Donor and Acceptor Sites
 Embedded in a Layered Metal-Organic Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11050
_journal_page_last               11053
_journal_paper_doi               10.1021/ja203291n
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'N2 C4 H16 2+, Zn2 C6 O12 2-, 2(H2 O)'
_chemical_formula_sum            'C10 H18 N2 O14 Zn2'
_chemical_formula_weight         521.00
_chemical_name_common            {H3N(CH2)4NH3}[Zn2(ox)3](H2O)2
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.779(5)
_cell_angle_beta                 88.615(6)
_cell_angle_gamma                71.692(5)
_cell_formula_units_Z            1
_cell_length_a                   6.722(4)
_cell_length_b                   8.897(5)
_cell_length_c                   9.501(6)
_cell_measurement_temperature    100(2)
_cell_volume                     474.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'yadokari-XG (K. Wakita, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (A. Altomare, et.al. 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker SMART APEX CCD-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode with a mirror focusing unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4871
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    2.598
_exptl_absorpt_correction_T_max  0.8811
_exptl_absorpt_correction_T_min  0.6245
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_description       platelet
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0521P)²+1.4214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                1909
_reflns_number_total             2116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203291n_si_003.cif
_cod_data_source_block           dab_2h2o
_cod_database_code               4106451
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
Zn1 Zn 0.99526(6) 0.16569(5) 0.17820(5) 0.01807(16) Uani 1 1 d
O2 O 1.1917(4) 0.0776(3) 0.0364(3) 0.0206(5) Uani 1 1 d
O3 O 0.8201(4) 0.4020(3) -0.0180(3) 0.0210(5) Uani 1 1 d
O4 O 1.1811(4) -0.0603(3) 0.3848(3) 0.0194(5) Uani 1 1 d
O5 O 0.8148(4) 0.1951(3) 0.3512(3) 0.0205(5) Uani 1 1 d
O6 O 1.1625(4) 0.3246(3) 0.1777(3) 0.0227(5) Uani 1 1 d
O7 O 0.8239(4) 0.0300(3) 0.1320(3) 0.0199(5) Uani 1 1 d
O8 O 0.5086(5) -0.4502(4) 0.2238(3) 0.0282(6) Uani 1 1 d
C15 C 0.9316(6) -0.4316(5) 0.4203(4) 0.0218(7) Uani 1 1 d
C10 C 1.1070(5) -0.0744(4) 0.5102(4) 0.0161(6) Uani 1 1 d
N1 N 0.5772(5) -0.1980(4) 0.2906(4) 0.0214(6) Uani 1 1 d
C12 C 0.9010(5) 0.5230(5) -0.0569(4) 0.0176(7) Uani 1 1 d
C13 C 1.1062(5) 0.0135(4) -0.0265(4) 0.0176(7) Uani 1 1 d
C14 C 0.7209(6) -0.3216(5) 0.4454(4) 0.0220(7) Uani 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0253(2) 0.0160(2) 0.0162(2) -0.00919(17) 0.00460(16) -0.00893(17)
O2 0.0250(13) 0.0221(13) 0.0234(13) -0.0153(11) 0.0072(10) -0.0123(10)
O3 0.0273(13) 0.0177(12) 0.0202(12) -0.0079(10) 0.0011(10) -0.0119(10)
O4 0.0224(12) 0.0178(12) 0.0169(12) -0.0092(10) 0.0064(10) -0.0042(10)
O5 0.0235(13) 0.0180(12) 0.0183(12) -0.0093(10) 0.0039(10) -0.0039(10)
O6 0.0302(14) 0.0193(12) 0.0185(12) -0.0070(10) -0.0009(10) -0.0110(11)
O7 0.0256(13) 0.0199(12) 0.0214(12) -0.0128(10) 0.0098(10) -0.0122(10)
O8 0.0317(15) 0.0221(13) 0.0327(15) -0.0156(12) -0.0037(12) -0.0067(11)
C15 0.0211(17) 0.0254(18) 0.0207(18) -0.0127(16) 0.0054(14) -0.0076(15)
C10 0.0199(16) 0.0145(15) 0.0198(16) -0.0106(13) 0.0047(13) -0.0093(13)
N1 0.0212(15) 0.0222(15) 0.0197(15) -0.0089(13) 0.0039(12) -0.0078(12)
C12 0.0221(17) 0.0168(16) 0.0188(16) -0.0119(13) 0.0043(13) -0.0073(13)
C13 0.0219(17) 0.0117(14) 0.0168(16) -0.0046(13) 0.0033(13) -0.0061(13)
C14 0.0203(17) 0.0184(17) 0.0241(18) -0.0110(15) 0.0002(14) -0.0008(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O3 Zn1 O6 81.66(11) . .
O3 Zn1 O5 98.28(11) . .
O6 Zn1 O5 94.55(11) . .
O3 Zn1 O7 90.09(11) . .
O6 Zn1 O7 169.20(10) . .
O5 Zn1 O7 93.52(10) . .
O3 Zn1 O4 174.83(10) . .
O6 Zn1 O4 93.65(11) . .
O5 Zn1 O4 79.85(10) . .
O7 Zn1 O4 94.83(11) . .
O3 Zn1 O2 92.36(11) . .
O6 Zn1 O2 92.83(11) . .
O5 Zn1 O2 167.82(10) . .
O7 Zn1 O2 80.49(10) . .
O4 Zn1 O2 90.04(11) . .
C13 O2 Zn1 111.7(2) . .
C12 O3 Zn1 112.3(2) . .
C10 O4 Zn1 113.4(2) . .
C10 O5 Zn1 113.4(2) 2_756 .
C12 O6 Zn1 111.7(2) 2_765 .
C13 O7 Zn1 111.8(2) 2_755 .
C15 C15 C14 110.4(4) 2_746 .
O5 C10 O4 126.7(3) 2_756 .
O5 C10 C10 117.1(4) 2_756 2_756
O4 C10 C10 116.3(4) . 2_756
O6 C12 O3 126.2(3) 2_765 .
O6 C12 C12 117.5(4) 2_765 2_765
O3 C12 C12 116.2(4) . 2_765
O2 C13 O7 125.4(3) . 2_755
O2 C13 C13 117.8(4) . 2_755
O7 C13 C13 116.8(4) 2_755 2_755
N1 C14 C15 110.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 2.061(3) .
Zn1 O6 2.063(3) .
Zn1 O5 2.083(3) .
Zn1 O7 2.088(3) .
Zn1 O4 2.095(3) .
Zn1 O2 2.098(3) .
O2 C13 1.245(4) .
O3 C12 1.259(4) .
O4 C10 1.247(4) .
O5 C10 1.244(4) 2_756
O6 C12 1.255(4) 2_765
O7 C13 1.262(4) 2_755
C15 C15 1.516(7) 2_746
C15 C14 1.532(5) .
C10 O5 1.244(4) 2_756
C10 C10 1.563(7) 2_756
N1 C14 1.492(5) .
C12 O6 1.255(4) 2_765
C12 C12 1.559(7) 2_765
C13 O7 1.262(4) 2_755
C13 C13 1.555(7) 2_755
