#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:26:49 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178950 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/79/4117919.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_4117919
loop_
_publ_author_name
'Satoshi Horike'
'Daiki Umeyama'
'Munehiro Inukai'
'Tomoya Itakura'
'Susumu Kitagawa'
_publ_contact_author_address
;
Department of Synthetic Chemistry and Biological Chemistry
Graduate School of Engineering, Kyoto University
Katsura, Nishikyo-ku
Kyoto
615-8510
JAPAN
;
_publ_contact_author_email       KITAGAWA@SBCHEM.KYOTO-U.AC.JP
_publ_contact_author_name        'Susumu Kitagawa'
_publ_section_title
;
 Coordination-Network-Based Ionic Plastic Crystal for Anhydrous Proton
 Conductivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7612
_journal_page_last               7615
_journal_paper_doi               10.1021/ja301875x
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C6 H15 N4 O12 P3 Zn'
_chemical_formula_weight         493.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.064(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.009(2)
_cell_length_b                   21.830(5)
_cell_length_c                   9.235(2)
_cell_measurement_temperature    348(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3
_cell_volume                     1658.4(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      348(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13249
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.842
_exptl_absorpt_correction_T_max  0.7096
_exptl_absorpt_correction_T_min  0.7096
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0675
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1915
_reflns_number_gt                2595
_reflns_number_total             3739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301875x_si_002.cif
_cod_data_source_block           Zn(HPO4)2(H2PO4)_75C
_cod_original_cell_volume        1658.5(7)
_cod_database_code               4117919
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.02139(8) 0.33000(3) 0.61080(8) 0.0238(2) Uani 1 1 d . . .
P2 P -0.29870(18) 0.29628(7) 0.66818(17) 0.0208(3) Uani 1 1 d . . .
P3 P -0.2404(2) 0.39796(7) 0.29561(19) 0.0279(4) Uani 1 1 d . . .
P4 P 0.35117(19) 0.39350(7) 0.78709(18) 0.0246(4) Uani 1 1 d . . .
O5 O -0.3648(5) 0.2388(2) 0.5692(5) 0.0326(10) Uani 1 1 d . . .
O6 O 0.1771(5) 0.38518(19) 0.7646(5) 0.0299(10) Uani 1 1 d . . .
O7 O -0.3092(5) 0.2873(2) 0.8331(5) 0.0286(10) Uani 1 1 d . . .
H1 H -0.3919 0.3037 0.8308 0.043 Uiso 1 1 calc R . .
O8 O 0.4684(5) 0.3470(2) 0.8903(4) 0.0319(10) Uani 1 1 d . . .
O9 O -0.1177(5) 0.3036(2) 0.7115(5) 0.0303(10) Uani 1 1 d . . .
O10 O -0.3956(5) 0.3522(2) 0.5867(5) 0.0311(10) Uani 1 1 d . . .
O11 O 0.4137(6) 0.4568(2) 0.8646(6) 0.0468(13) Uani 1 1 d . . .
H21 H 0.3448 0.4830 0.8205 0.070 Uiso 1 1 calc R . .
N17 N 0.0782(7) 0.3059(3) 0.0403(6) 0.0386(14) Uani 1 1 d . . .
H6 H 0.0161 0.3057 -0.0593 0.046 Uiso 1 1 calc R . .
O13 O 0.3516(6) 0.3928(2) 0.6180(5) 0.0422(13) Uani 1 1 d . . .
H5 H 0.4201 0.3684 0.6164 0.063 Uiso 1 1 calc R . .
O14 O -0.2222(6) 0.4509(2) 0.2033(6) 0.0476(13) Uani 1 1 d . . .
N15 N 0.1569(8) 0.2997(3) 0.2893(7) 0.0444(16) Uani 1 1 d . . .
H7 H 0.1560 0.2950 0.3813 0.053 Uiso 1 1 calc R . .
O17 O -0.0843(6) 0.3728(3) 0.4143(5) 0.0487(14) Uani 1 1 d . . .
O15 O -0.3560(8) 0.4190(3) 0.3749(8) 0.0634(17) Uani 1 1 d . . .
H3 H -0.4251 0.3926 0.3617 0.095 Uiso 1 1 calc R . .
C19 C 0.2898(9) 0.3100(4) 0.2597(8) 0.0460(19) Uani 1 1 d . . .
H8 H 0.3963 0.3134 0.3349 0.055 Uiso 1 1 calc R . .
C20 C 0.2406(10) 0.3142(3) 0.1042(9) 0.0419(17) Uani 1 1 d . . .
H9 H 0.3055 0.3215 0.0494 0.050 Uiso 1 1 calc R . .
C21 C 0.0317(9) 0.2983(4) 0.1556(9) 0.0446(18) Uani 1 1 d . . .
H10 H -0.0752 0.2926 0.1432 0.053 Uiso 1 1 calc R . .
O16 O -0.3231(9) 0.3431(2) 0.1841(6) 0.071(2) Uani 1 1 d . . .
H4 H -0.3510 0.3537 0.0915 0.107 Uiso 1 1 calc R . .
N26 N 0.236(2) 0.5326(7) 0.1227(16) 0.040(3) Uiso 0.50 1 d P A 1
H11 H 0.2699 0.5469 0.0549 0.048 Uiso 0.50 1 calc PR A 1
C32 C 0.315(2) 0.4897(8) 0.248(2) 0.036(3) Uiso 0.50 1 d P A 1
H12 H 0.4157 0.4720 0.2695 0.043 Uiso 0.50 1 calc PR A 1
N25 N 0.084(2) 0.5064(10) 0.256(2) 0.063(5) Uiso 0.50 1 d P A 1
H13 H 0.0017 0.5011 0.2789 0.076 Uiso 0.50 1 calc PR A 1
C30 C 0.089(2) 0.5458(7) 0.137(2) 0.037(3) Uiso 0.50 1 d P A 1
H14 H 0.0110 0.5746 0.0793 0.044 Uiso 0.50 1 calc PR A 1
C31 C 0.229(4) 0.4786(14) 0.328(4) 0.081(8) Uiso 0.50 1 d P A 1
H15 H 0.2614 0.4553 0.4203 0.097 Uiso 0.50 1 calc PR A 1
N28 N 0.293(3) 0.5120(10) 0.189(3) 0.074(5) Uiso 0.50 1 d P B 2
H20 H 0.3785 0.5139 0.1693 0.089 Uiso 0.50 1 calc PR B 2
C34 C 0.158(4) 0.4833(13) 0.300(4) 0.076(8) Uiso 0.50 1 d P B 2
H16 H 0.1236 0.4602 0.3655 0.091 Uiso 0.50 1 calc PR B 2
N29 N 0.0757(16) 0.5344(7) 0.2148(19) 0.041(3) Uiso 0.50 1 d P B 2
H17 H -0.0080 0.5519 0.2188 0.050 Uiso 0.50 1 calc PR B 2
C33 C 0.270(5) 0.4735(15) 0.281(4) 0.103(11) Uiso 0.50 1 d P B 2
H18 H 0.3394 0.4408 0.3282 0.123 Uiso 0.50 1 calc PR B 2
C35 C 0.157(3) 0.5508(10) 0.122(2) 0.062(5) Uiso 0.50 1 d P B 2
H19 H 0.1298 0.5792 0.0406 0.074 Uiso 0.50 1 calc PR B 2
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'
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'
P P 0.1023 0.0942 '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'
H H 0.0000 0.0000 '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
O17 Zn1 O9 115.7(2) . .
O17 Zn1 O5 106.8(2) . 4_665
O9 Zn1 O5 111.29(19) . 4_665
O17 Zn1 O6 108.7(2) . .
O9 Zn1 O6 104.42(18) . .
O5 Zn1 O6 109.90(19) 4_665 .
O10 P2 O9 112.7(3) . .
O10 P2 O5 111.2(3) . .
O9 P2 O5 111.1(3) . .
O10 P2 O7 109.4(2) . .
O9 P2 O7 103.9(2) . .
O5 P2 O7 108.3(2) . .
O14 P3 O17 114.7(3) . .
O14 P3 O16 110.8(3) . .
O17 P3 O16 104.8(3) . .
O14 P3 O15 106.9(3) . .
O17 P3 O15 111.8(3) . .
O16 P3 O15 107.7(4) . .
O8 P4 O6 115.5(3) . .
O8 P4 O11 106.3(3) . .
O6 P4 O11 109.4(3) . .
O8 P4 O13 110.0(2) . .
O6 P4 O13 106.7(3) . .
O11 P4 O13 108.7(3) . .
P2 O5 Zn1 128.8(2) . 4_565
P4 O6 Zn1 125.0(2) . .
P2 O7 H1 109.5 . .
P2 O9 Zn1 138.0(3) . .
P4 O11 H21 109.5 . .
C21 N17 C20 108.2(6) . .
C21 N17 H6 125.9 . .
C20 N17 H6 125.9 . .
P4 O13 H5 109.5 . .
C21 N15 C19 108.2(6) . .
C21 N15 H7 125.9 . .
C19 N15 H7 125.9 . .
P3 O17 Zn1 146.4(3) . .
P3 O15 H3 109.5 . .
C20 C19 N15 107.4(7) . .
C20 C19 H8 126.3 . .
N15 C19 H8 126.3 . .
C19 C20 N17 106.9(6) . .
C19 C20 H9 126.6 . .
N17 C20 H9 126.6 . .
N15 C21 N17 109.3(7) . .
N15 C21 H10 125.3 . .
N17 C21 H10 125.3 . .
P3 O16 H4 109.5 . .
C30 N26 C32 103.6(12) . .
C30 N26 H11 128.2 . .
C32 N26 H11 128.2 . .
C31 C32 N26 111.5(18) . .
C31 C32 H12 124.3 . .
N26 C32 H12 124.3 . .
C31 N25 C30 109.5(19) . .
C31 N25 H13 125.3 . .
C30 N25 H13 125.3 . .
N25 C30 N26 105.9(14) . .
N25 C30 H14 127.1 . .
N26 C30 H14 127.1 . .
C32 C31 N25 109(2) . .
C32 C31 H15 125.7 . .
N25 C31 H15 125.7 . .
C33 N28 C35 110(2) . .
C33 N28 H20 125.2 . .
C35 N28 H20 125.2 . .
C33 C34 N29 112(3) . .
C33 C34 H16 124.1 . .
N29 C34 H16 124.1 . .
C35 N29 C34 105.4(18) . .
C35 N29 H17 127.3 . .
C34 N29 H17 127.3 . .
C34 C33 N28 113(3) . .
C34 C33 H18 123.7 . .
N28 C33 H18 123.7 . .
N29 C35 N28 99.4(17) . .
N29 C35 H19 130.3 . .
N28 C35 H19 130.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O17 1.914(4) .
Zn1 O9 1.928(4) .
Zn1 O5 1.944(4) 4_665
Zn1 O6 1.953(4) .
P2 O10 1.511(4) .
P2 O9 1.521(4) .
P2 O5 1.523(4) .
P2 O7 1.576(4) .
P3 O14 1.485(5) .
P3 O17 1.491(5) .
P3 O16 1.557(5) .
P3 O15 1.566(5) .
P4 O8 1.494(4) .
P4 O6 1.507(4) .
P4 O11 1.553(5) .
P4 O13 1.563(4) .
O5 Zn1 1.944(4) 4_565
O7 H1 0.8200 .
O11 H21 0.8200 .
N17 C21 1.305(9) .
N17 C20 1.348(9) .
N17 H6 0.8600 .
O13 H5 0.8200 .
N15 C21 1.290(9) .
N15 C19 1.351(9) .
N15 H7 0.8600 .
O15 H3 0.8200 .
C19 C20 1.323(10) .
C19 H8 0.9300 .
C20 H9 0.9300 .
C21 H10 0.9300 .
O16 H4 0.8200 .
N26 C30 1.41(2) .
N26 C32 1.43(2) .
N26 H11 0.8600 .
C32 C31 1.30(4) .
C32 H12 0.9300 .
N25 C31 1.34(4) .
N25 C30 1.41(2) .
N25 H13 0.8600 .
C30 H14 0.9300 .
C31 H15 0.9300 .
N28 C33 1.28(3) .
N28 C35 1.41(3) .
N28 H20 0.8600 .
C34 C33 1.11(4) .
C34 N29 1.39(3) .
C34 H16 0.9300 .
N29 C35 1.38(3) .
N29 H17 0.8600 .
C33 H18 0.9300 .
C35 H19 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_4
O10 P2 O5 Zn1 -110.3(4) . 4_565
O9 P2 O5 Zn1 123.3(3) . 4_565
O7 P2 O5 Zn1 9.9(4) . 4_565
O8 P4 O6 Zn1 -82.9(4) . .
O11 P4 O6 Zn1 157.1(3) . .
O13 P4 O6 Zn1 39.7(4) . .
O17 Zn1 O6 P4 -88.2(3) . .
O9 Zn1 O6 P4 147.8(3) . .
O5 Zn1 O6 P4 28.4(4) 4_665 .
O10 P2 O9 Zn1 -48.3(5) . .
O5 P2 O9 Zn1 77.2(5) . .
O7 P2 O9 Zn1 -166.5(4) . .
O17 Zn1 O9 P2 14.1(5) . .
O5 Zn1 O9 P2 -108.0(4) 4_665 .
O6 Zn1 O9 P2 133.5(4) . .
O14 P3 O17 Zn1 152.9(6) . .
O16 P3 O17 Zn1 -85.4(7) . .
O15 P3 O17 Zn1 31.0(8) . .
O9 Zn1 O17 P3 1.9(8) . .
O5 Zn1 O17 P3 126.4(6) 4_665 .
O6 Zn1 O17 P3 -115.1(6) . .
C21 N15 C19 C20 -0.4(9) . .
N15 C19 C20 N17 -0.6(9) . .
C21 N17 C20 C19 1.3(9) . .
C19 N15 C21 N17 1.2(9) . .
C20 N17 C21 N15 -1.6(9) . .
C30 N26 C32 C31 -0.4(19) . .
C31 N25 C30 N26 10(2) . .
C32 N26 C30 N25 -5.5(15) . .
N26 C32 C31 N25 6(3) . .
C30 N25 C31 C32 -10(3) . .
C33 C34 N29 C35 6(3) . .
N29 C34 C33 N28 1(4) . .
C35 N28 C33 C34 -7(4) . .
C34 N29 C35 N28 -9(2) . .
C33 N28 C35 N29 10(2) . .
