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#$Date: 2016-03-26 17:03:07 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180370 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/39/7203964.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_7203964
loop_
_publ_author_name
'Liu, Wang'
'Liu, Yunling'
'Shi, Zhan'
'Pang, Wenqin'
_publ_section_title
;
 Hydrothermal synthesis and characterization of a new layered zinc
 phosphate intercalated with fully-protonated triethylenetetramine
 [Zn2(HPO4)3]2−[(C6N4H22)0.5]2+
;
_journal_issue                   6
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1451
_journal_paper_doi               10.1039/b000658k
_journal_volume                  10
_journal_year                    2000
_chemical_formula_sum            'C3 H14 N2 O12 P3 Zn2'
_chemical_formula_weight         493.81
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.723(2)
_cell_angle_beta                 101.258(2)
_cell_angle_gamma                115.785(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4876(8)
_cell_length_b                   8.2336(8)
_cell_length_c                   12.8592(13)
_cell_measurement_temperature    293(2)
_cell_volume                     674.51(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1669
_diffrn_reflns_av_sigmaI/netI    0.1152
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3323
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    3.980
_exptl_absorpt_correction_T_max  0.8899
_exptl_absorpt_correction_T_min  0.5033
_exptl_crystal_density_diffrn    2.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0596
_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)+(0.1079P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                1764
_reflns_number_total             1928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000658k.txt
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203964
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.16839(9) 0.60022(9) 0.68146(5) 0.0158(3) Uani 1 1 d . . .
Zn2 Zn 0.40687(9) 0.23218(8) 0.99672(5) 0.0161(3) Uani 1 1 d . . .
P1 P -0.2977(2) 0.3625(2) 0.53135(12) 0.0162(4) Uani 1 1 d . . .
P2 P 0.4269(2) 0.4324(2) 0.80586(11) 0.0142(4) Uani 1 1 d . . .
P3 P 0.8139(2) 0.2017(2) 1.08445(12) 0.0151(4) Uani 1 1 d . . .
O1 O -0.5053(6) 0.2506(7) 0.5499(3) 0.0339(12) Uani 1 1 d . . .
O2 O -0.2611(7) 0.5692(6) 0.5342(4) 0.0348(11) Uani 1 1 d . . .
H2 H -0.3511 0.5645 0.4840 0.080 Uiso 1 1 calc . . .
O3 O -0.1213(6) 0.3919(6) 0.6277(3) 0.0226(10) Uani 1 1 d . . .
O4 O 0.2277(8) 0.7926(6) 0.8057(4) 0.0307(11) Uani 1 1 d . . .
O5 O 0.2887(6) 0.7254(6) 0.5774(3) 0.0254(10) Uani 1 1 d . . .
O6 O 0.2719(7) 0.4265(6) 0.7076(3) 0.0261(10) Uani 1 1 d . . .
O7 O 0.5260(6) 0.3138(6) 0.7597(3) 0.0217(9) Uani 1 1 d . . .
H7 H 0.6087 0.3113 0.8109 0.080 Uiso 1 1 calc . . .
O8 O 0.3168(6) 0.3386(6) 0.8847(3) 0.0230(10) Uani 1 1 d . . .
O9 O 0.1859(6) -0.0222(6) 0.9616(3) 0.0229(10) Uani 1 1 d . . .
O10 O 0.3993(6) 0.3694(5) 1.1348(3) 0.0202(9) Uani 1 1 d . . .
O11 O 0.6727(6) 0.2434(6) 1.0042(3) 0.0235(10) Uani 1 1 d . . .
O12 O 1.0356(6) 0.3672(6) 1.0964(4) 0.0310(11) Uani 1 1 d . . .
H12 H 1.0399 0.4677 1.1194 0.080 Uiso 1 1 calc . . .
N1 N -0.1243(8) 0.2496(7) 0.8291(4) 0.0221(12) Uani 1 1 d . . .
H1A H -0.1961 0.2858 0.8656 0.080 Uiso 1 1 calc . . .
H1B H -0.1002 0.3094 0.7771 0.080 Uiso 1 1 calc . . .
H1C H -0.0042 0.2766 0.8756 0.080 Uiso 1 1 calc . . .
N2 N -0.1347(7) 0.0222(7) 0.6059(4) 0.0205(11) Uani 1 1 d . . .
H2A H -0.2628 -0.0492 0.5584 0.080 Uiso 1 1 calc . . .
H2B H -0.1050 0.1428 0.6160 0.080 Uiso 1 1 calc . . .
C1 C -0.2462(10) 0.0430(9) 0.7772(5) 0.0277(15) Uani 1 1 d . . .
H1D H -0.3782 0.0139 0.7276 0.080 Uiso 1 1 calc . . .
H1E H -0.2745 -0.0215 0.8339 0.080 Uiso 1 1 calc . . .
C2 C -0.1312(10) -0.0267(9) 0.7137(5) 0.0238(14) Uani 1 1 d . . .
H2C H 0.0117 0.0272 0.7583 0.080 Uiso 1 1 calc . . .
H2D H -0.1935 -0.1616 0.7002 0.080 Uiso 1 1 calc . . .
C3 C 0.0186(9) -0.0077(9) 0.5581(5) 0.0225(13) Uani 1 1 d . . .
H3A H 0.0035 -0.1305 0.5592 0.080 Uiso 1 1 calc . . .
H3B H 0.1585 0.0856 0.6016 0.080 Uiso 1 1 calc . . .
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
_geom_angle_publ_flag
O4 Zn1 O5 106.09(19) . . ?
O4 Zn1 O6 116.56(18) . . ?
O5 Zn1 O6 108.8(2) . . ?
O4 Zn1 O3 115.80(19) . . ?
O5 Zn1 O3 118.57(16) . . ?
O6 Zn1 O3 90.69(18) . . ?
O9 Zn2 O11 112.08(18) . . ?
O9 Zn2 O8 104.98(18) . . ?
O11 Zn2 O8 114.27(17) . . ?
O9 Zn2 O10 106.75(17) . . ?
O11 Zn2 O10 113.77(17) . . ?
O8 Zn2 O10 104.19(18) . . ?
O5 P1 O1 111.5(2) 2_566 . ?
O5 P1 O3 112.5(2) 2_566 . ?
O1 P1 O3 110.5(2) . . ?
O5 P1 O2 109.2(3) 2_566 . ?
O1 P1 O2 108.9(3) . . ?
O3 P1 O2 103.9(2) . . ?
O6 P2 O8 110.5(2) . . ?
O6 P2 O10 112.6(2) . 2_667 ?
O8 P2 O10 111.1(2) . 2_667 ?
O6 P2 O7 106.6(2) . . ?
O8 P2 O7 107.5(2) . . ?
O10 P2 O7 108.3(2) 2_667 . ?
O4 P3 O9 111.3(3) 2_667 2_657 ?
O4 P3 O11 112.7(3) 2_667 . ?
O9 P3 O11 113.2(3) 2_657 . ?
O4 P3 O12 110.3(3) 2_667 . ?
O9 P3 O12 106.8(2) 2_657 . ?
O11 P3 O12 101.9(2) . . ?
P1 O2 H2 109.5 . . ?
P1 O3 Zn1 128.1(2) . . ?
P3 O4 Zn1 135.1(3) 2_667 . ?
P1 O5 Zn1 127.6(3) 2_566 . ?
P2 O6 Zn1 131.8(2) . . ?
P2 O7 H7 109.5 . . ?
P2 O8 Zn2 129.6(2) . . ?
P3 O9 Zn2 128.6(3) 2_657 . ?
P2 O10 Zn2 120.1(2) 2_667 . ?
P3 O11 Zn2 132.9(3) . . ?
P3 O12 H12 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 N2 C2 111.3(5) . . ?
C3 N2 H2A 109.4 . . ?
C2 N2 H2A 109.4 . . ?
C3 N2 H2B 109.4 . . ?
C2 N2 H2B 109.4 . . ?
H2A N2 H2B 108.0 . . ?
N1 C1 C2 111.8(5) . . ?
N1 C1 H1D 109.3 . . ?
C2 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
C2 C1 H1E 109.3 . . ?
H1D C1 H1E 107.9 . . ?
N2 C2 C1 112.7(5) . . ?
N2 C2 H2C 109.0 . . ?
C1 C2 H2C 109.0 . . ?
N2 C2 H2D 109.0 . . ?
C1 C2 H2D 109.0 . . ?
H2C C2 H2D 107.8 . . ?
N2 C3 C3 109.1(6) . 2_556 ?
N2 C3 H3A 109.9 . . ?
C3 C3 H3A 109.9 2_556 . ?
N2 C3 H3B 109.9 . . ?
C3 C3 H3B 109.9 2_556 . ?
H3A C3 H3B 108.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.898(4) . ?
Zn1 O5 1.935(4) . ?
Zn1 O6 1.941(4) . ?
Zn1 O3 1.986(4) . ?
Zn2 O9 1.932(4) . ?
Zn2 O11 1.935(4) . ?
Zn2 O8 1.953(4) . ?
Zn2 O10 1.979(4) . ?
P1 O5 1.502(4) 2_566 ?
P1 O1 1.512(4) . ?
P1 O3 1.527(4) . ?
P1 O2 1.595(5) . ?
P2 O6 1.519(4) . ?
P2 O8 1.522(4) . ?
P2 O10 1.525(4) 2_667 ?
P2 O7 1.576(4) . ?
P3 O4 1.503(5) 2_667 ?
P3 O9 1.507(4) 2_657 ?
P3 O11 1.516(4) . ?
P3 O12 1.583(4) . ?
O2 H2 0.8200 . ?
O4 P3 1.503(5) 2_667 ?
O5 P1 1.502(4) 2_566 ?
O7 H7 0.8200 . ?
O9 P3 1.507(4) 2_657 ?
O10 P2 1.525(4) 2_667 ?
O12 H12 0.8200 . ?
N1 C1 1.496(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 C3 1.493(8) . ?
N2 C2 1.500(8) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
C1 C2 1.516(9) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C3 1.501(13) 2_556 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O1 0.82 2.26 2.905(7) 135.8 2_466
O2 H2 O2 0.82 2.56 3.129(10) 127.2 2_466
O2 H2 O6 0.82 2.65 3.100(7) 116.3 2_566
O7 H7 N1 0.82 2.25 2.892(6) 135.9 1_655
O7 H7 O11 0.82 2.63 3.345(6) 146.6 .
O12 H12 N1 0.82 2.08 2.885(7) 165.4 2_667
N1 H1A O11 0.89 2.20 2.947(6) 141.2 1_455
N1 H1A O7 0.89 2.38 2.892(6) 117.1 1_455
N1 H1B O3 0.89 2.13 3.000(6) 164.7 .
N1 H1C O8 0.89 2.20 2.962(6) 142.8 .
N2 H2A O1 0.90 1.89 2.754(6) 161.5 2_456
N2 H2B O3 0.90 2.09 2.970(7) 164.9 .
N2 H2B O6 0.90 2.63 3.220(7) 123.5 .
