#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:13:47 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178890 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/19/4111952.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_4111952
loop_
_publ_author_name
'Yueh-Chun Liao'
'Yao-Chen Jiang'
'Sue-Lein Wang'
_publ_section_title
;
 Discrete Water Hexamers and Template-Assisted Molecular Recognition in an
 Elastic Zincophosphate Lattice
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12794
_journal_page_last               12795
_journal_paper_doi               10.1021/ja054357k
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C28 H54 N8 O24 P4 Zn3'
_chemical_formula_weight         1206.78
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.6840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0239(9)
_cell_length_b                   8.5826(5)
_cell_length_c                   36.299(2)
_cell_measurement_reflns_used    4289
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.28
_cell_volume                     4599.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14334
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       lamellar
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.968
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.394
_refine_ls_extinction_coef       0.00281(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0568P)²+9.2340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                4877
_reflns_number_total             5412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054357ksi20050701_065420.cif
_cod_data_source_block           TA-NTHU-3
_cod_original_cell_volume        4599.5(5)
_cod_database_code               4111952
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.63438(2) 0.33542(4) 0.243328(10) 0.01759(12) Uani 1 1 d .
Zn2 Zn 0.5000 -0.27148(6) 0.2500 0.02012(15) Uani 1 2 d S
P1 P 0.67316(5) -0.02587(9) 0.25719(2) 0.01642(18) Uani 1 1 d .
P2 P 0.46620(5) -0.52012(10) 0.19480(2) 0.01752(18) Uani 1 1 d .
O1 O 0.59955(17) -0.1278(3) 0.26929(7) 0.0292(6) Uani 1 1 d .
O2 O 0.66081(18) 0.1412(3) 0.27084(7) 0.0265(5) Uani 1 1 d .
O3 O 0.76523(16) -0.0872(3) 0.27830(7) 0.0252(5) Uani 1 1 d .
O4 O 0.66765(17) -0.0282(3) 0.21486(7) 0.0269(5) Uani 1 1 d .
O5 O 0.39655(17) -0.5200(3) 0.22040(7) 0.0267(5) Uani 1 1 d .
O6 O 0.51966(17) -0.3677(3) 0.20206(7) 0.0253(5) Uani 1 1 d .
O7 O 0.53051(16) -0.6605(3) 0.20072(7) 0.0230(5) Uani 1 1 d .
O8 O 0.41085(17) -0.5238(3) 0.15424(7) 0.0303(6) Uani 1 1 d .
O9 O 0.9785(2) 0.9534(4) 0.09794(8) 0.0471(8) Uani 1 1 d .
O10 O 0.8193(4) 0.3653(5) 0.03246(11) 0.0855(17) Uani 1 1 d .
O11 O 0.7762(3) 0.4836(4) 0.08019(9) 0.0503(8) Uani 1 1 d .
O12 O 0.8826(3) 1.1382(4) 0.07500(9) 0.0570(10) Uani 1 1 d .
N1 N 0.6034(2) -0.0254(4) 0.12539(8) 0.0262(6) Uani 1 1 d .
N2 N 0.6764(2) -0.2923(4) 0.17509(9) 0.0304(7) Uani 1 1 d .
N3 N 0.7547(2) 0.1607(4) 0.17062(9) 0.0299(7) Uani 1 1 d .
N4 N 0.4887(2) 0.0319(4) 0.18120(9) 0.0262(6) Uani 1 1 d .
C1 C 0.6059(3) -0.1883(5) 0.11311(10) 0.0342(8) Uani 1 1 d .
C2 C 0.6849(3) -0.2789(5) 0.13516(11) 0.0358(9) Uani 1 1 d .
C3 C 0.6676(3) 0.0727(5) 0.10998(10) 0.0320(8) Uani 1 1 d .
C4 C 0.6984(3) 0.2124(5) 0.13482(11) 0.0350(9) Uani 1 1 d .
C5 C 0.5109(3) 0.0387(5) 0.11557(11) 0.0330(8) Uani 1 1 d .
C6 C 0.4507(3) -0.0155(5) 0.14226(11) 0.0355(9) Uani 1 1 d .
C7 C 0.7876(3) 0.4837(5) 0.04834(12) 0.0412(10) Uani 1 1 d .
C8 C 0.7686(3) 0.6205(5) 0.02303(12) 0.0407(10) Uani 1 1 d .
C9 C 0.7640(5) 0.6066(6) -0.01548(14) 0.0603(15) Uani 1 1 d .
C10 C 0.7552(4) 0.7637(6) 0.03801(12) 0.0556(14) Uani 1 1 d .
C11 C 0.9409(3) 1.0410(5) 0.07122(10) 0.0356(9) Uani 1 1 d .
C12 C 0.9718(3) 1.0206(5) 0.03430(10) 0.0337(8) Uani 1 1 d .
C13 C 0.9263(17) 1.092(4) 0.0015(4) 0.046(6) Uani 0.58(7) 1 d P
C13' C 0.969(3) 1.144(2) 0.0099(7) 0.046(9) Uani 0.42(7) 1 d P
C14 C 1.043(2) 0.925(3) 0.0317(3) 0.053(7) Uani 0.65(6) 1 d P
C14' C 0.999(3) 0.875(3) 0.0243(8) 0.038(8) Uani 0.35(6) 1 d P
H1 H 0.7218 -0.3424 0.1856 0.050 Uiso 1 1 d .
H2 H 0.6307 -0.3522 0.1822 0.050 Uiso 1 1 d .
H3 H 0.6744 -0.2029 0.1833 0.050 Uiso 1 1 d .
H4 H 0.5446 0.0067 0.1854 0.050 Uiso 1 1 d .
H5 H 0.4564 -0.0165 0.1968 0.050 Uiso 1 1 d .
H6 H 0.4813 0.1243 0.1819 0.050 Uiso 1 1 d .
H7 H 0.7984 0.1157 0.1619 0.050 Uiso 1 1 d .
H8 H 0.7695 0.2380 0.1831 0.050 Uiso 1 1 d .
H9 H 0.7236 0.1028 0.1818 0.050 Uiso 1 1 d .
H10 H 0.5517 -0.2309 0.1170 0.050 Uiso 1 1 d .
H11 H 0.6082 -0.1816 0.0860 0.050 Uiso 1 1 d .
H12 H 0.7415 -0.2396 0.1304 0.050 Uiso 1 1 d .
H13 H 0.6865 -0.3633 0.1238 0.050 Uiso 1 1 d .
H14 H 0.5129 0.1484 0.1158 0.050 Uiso 1 1 d .
H15 H 0.4836 0.0089 0.0879 0.050 Uiso 1 1 d .
H16 H 0.4487 -0.1343 0.1424 0.050 Uiso 1 1 d .
H17 H 0.3923 0.0316 0.1313 0.050 Uiso 1 1 d .
H18 H 0.7206 0.0223 0.1083 0.050 Uiso 1 1 d .
H19 H 0.6392 0.1133 0.0839 0.050 Uiso 1 1 d .
H20 H 0.7288 0.2800 0.1200 0.050 Uiso 1 1 d .
H21 H 0.6533 0.2710 0.1408 0.050 Uiso 1 1 d .
H22 H 0.8362 0.2865 0.0460 0.050 Uiso 1 1 d .
H23 H 0.7639 0.5036 -0.0242 0.050 Uiso 1 1 d .
H24 H 0.7606 0.7871 0.0629 0.050 Uiso 1 1 d .
H25 H 0.8729 1.1455 0.0051 0.050 Uiso 1 1 d .
H26 H 1.0776 0.8621 0.0517 0.050 Uiso 1 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 0.0033 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'
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'
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
O5 Zn1 O3 111.08(10) 2_665 4_655
O5 Zn1 O2 104.65(11) 2_665 .
O3 Zn1 O2 113.62(11) 4_655 .
O5 Zn1 O7 105.47(11) 2_665 1_565
O3 Zn1 O7 103.67(10) 4_655 1_565
O2 Zn1 O7 118.13(10) . 1_565
O1 Zn2 O1 102.26(17) . 2_655
O1 Zn2 O6 110.13(10) . .
O1 Zn2 O6 100.05(11) 2_655 .
O1 Zn2 O6 100.05(11) . 2_655
O1 Zn2 O6 110.13(10) 2_655 2_655
O6 Zn2 O6 131.17(14) . 2_655
O1 Zn2 P2 136.94(8) . .
O1 Zn2 P2 101.00(8) 2_655 .
O6 Zn2 P2 29.66(7) . .
O6 Zn2 P2 105.19(7) 2_655 .
O1 Zn2 P2 101.00(8) . 2_655
O1 Zn2 P2 136.94(8) 2_655 2_655
O6 Zn2 P2 105.19(7) . 2_655
O6 Zn2 P2 29.66(7) 2_655 2_655
P2 Zn2 P2 85.53(3) . 2_655
O4 P1 O1 111.93(15) . .
O4 P1 O2 110.44(14) . .
O1 P1 O2 107.60(15) . .
O4 P1 O3 111.86(14) . .
O1 P1 O3 106.85(15) . .
O2 P1 O3 107.94(15) . .
O5 P2 O6 107.00(14) . .
O5 P2 O7 113.64(14) . .
O6 P2 O7 110.49(14) . .
O5 P2 O8 105.73(15) . .
O6 P2 O8 110.63(15) . .
O7 P2 O8 109.24(14) . .
O5 P2 Zn2 68.35(11) . .
O6 P2 Zn2 40.15(9) . .
O7 P2 Zn2 117.06(9) . .
O8 P2 Zn2 131.59(11) . .
P1 O1 Zn2 142.76(17) . .
P1 O2 Zn1 131.16(15) . .
P1 O3 Zn1 127.39(15) . 4_645
P2 O5 Zn1 134.15(16) . 2_645
P2 O6 Zn2 110.20(13) . .
P2 O7 Zn1 120.47(14) . 1_545
C3 N1 C1 112.0(3) . .
C3 N1 C5 110.5(3) . .
C1 N1 C5 110.9(3) . .
N1 C1 C2 112.9(3) . .
N2 C2 C1 110.8(3) . .
N1 C3 C4 112.1(3) . .
N3 C4 C3 110.3(3) . .
N1 C5 C6 112.2(3) . .
N4 C6 C5 110.9(3) . .
O11 C7 O10 123.8(4) . .
O11 C7 C8 123.5(4) . .
O10 C7 C8 112.8(4) . .
C10 C8 C9 119.4(4) . .
C10 C8 C7 119.2(4) . .
C9 C8 C7 121.5(4) . .
C10 C9 C8 119.5(4) 7_665 .
C8 C10 C9 121.1(4) . 7_665
O12 C11 O9 122.5(4) . .
O12 C11 C12 121.2(4) . .
O9 C11 C12 116.3(4) . .
C14 C12 C13' 110.2(16) . .
C14 C12 C14' 33.7(8) . .
C13' C12 C14' 120.0(9) . .
C14 C12 C13 118.2(6) . .
C13' C12 C13 33.3(9) . .
C14' C12 C13 107.2(17) . .
C14 C12 C11 120.3(5) . .
C13' C12 C11 120.4(6) . .
C14' C12 C11 119.5(7) . .
C13 C12 C11 121.5(5) . .
C13' C13 C14 91(3) . 5_775
C13' C13 C12 71.8(12) . .
C14 C13 C12 120.6(9) 5_775 .
C13' C13 C14' 62(2) . 5_775
C14 C13 C14' 29.5(7) 5_775 5_775
C12 C13 C14' 106.7(18) . 5_775
C13 C13' C12 74.9(16) . .
C13 C13' C14' 89(3) . 5_775
C12 C13' C14' 119.9(11) . 5_775
C13 C13' C14 59(2) . 5_775
C12 C13' C14 108(2) . 5_775
C14' C13' C14 29.8(11) 5_775 5_775
C14' C14 C12 74.0(16) . .
C14' C14 C13 92(3) . 5_775
C12 C14 C13 121.1(7) . 5_775
C14' C14 C13' 62(2) . 5_775
C12 C14 C13' 109.1(19) . 5_775
C13 C14 C13' 29.8(7) 5_775 5_775
C14 C14' C12 72.4(18) . .
C14 C14' C13' 88(3) . 5_775
C12 C14' C13' 119.9(12) . 5_775
C14 C14' C13 58(2) . 5_775
C12 C14' C13 106(2) . 5_775
C13' C14' C13 29.5(12) 5_775 5_775
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O5 1.927(2) 2_665
Zn1 O3 1.942(2) 4_655
Zn1 O2 1.946(2) .
Zn1 O7 1.983(2) 1_565
Zn2 O1 1.964(2) .
Zn2 O1 1.964(2) 2_655
Zn2 O6 1.997(2) .
Zn2 O6 1.997(2) 2_655
Zn2 P2 2.9067(9) .
Zn2 P2 2.9067(9) 2_655
P1 O4 1.524(2) .
P1 O1 1.537(2) .
P1 O2 1.539(2) .
P1 O3 1.544(2) .
P2 O5 1.523(2) .
P2 O6 1.532(2) .
P2 O7 1.534(2) .
P2 O8 1.551(2) .
O3 Zn1 1.942(2) 4_645
O5 Zn1 1.927(2) 2_645
O7 Zn1 1.983(2) 1_545
O9 C11 1.273(5) .
O10 C7 1.302(6) .
O11 C7 1.199(5) .
O12 C11 1.236(5) .
N1 C3 1.466(5) .
N1 C1 1.470(5) .
N1 C5 1.476(5) .
N2 C2 1.483(5) .
N3 C4 1.480(5) .
N4 C6 1.480(5) .
C1 C2 1.517(6) .
C3 C4 1.520(6) .
C5 C6 1.516(6) .
C7 C8 1.485(6) .
C8 C10 1.374(7) .
C8 C9 1.392(6) .
C9 C10 1.380(7) 7_665
C10 C9 1.380(7) 7_665
C11 C12 1.508(5) .
C12 C14 1.369(11) .
C12 C13' 1.377(13) .
C12 C14' 1.381(17) .
C12 C13 1.399(10) .
C13 C13' 0.80(2) .
C13 C14 1.376(13) 5_775
C13 C14' 1.62(3) 5_775
C13' C14' 1.42(2) 5_775
C13' C14 1.60(3) 5_775
C14 C14' 0.797(18) .
C14 C13 1.376(13) 5_775
C14 C13' 1.60(3) 5_775
C14' C13' 1.42(2) 5_775
C14' C13 1.62(3) 5_775
