#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:16:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180255 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/41/7114160.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_7114160
loop_
_publ_author_name
'Neeraj, S.'
'Cheetham, A. K.'
_publ_section_title
;
 Synthesis of open-framework zinc phosphates from organophosphorus amides
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1738
_journal_paper_doi               10.1039/b205557k
_journal_year                    2002
_chemical_formula_moiety         '[C2NH8][Zn3(PO4)(HPO4)2].H2O'
_chemical_formula_sum            'C2 H10 N O13 P3 Zn3'
_chemical_formula_weight         545.13
_chemical_name_common
;
Zinc Phosphate with N,N'dimethylamine
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.088(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6528(11)
_cell_length_b                   5.1909(4)
_cell_length_c                   21.1457(18)
_cell_measurement_temperature    293(2)
_cell_volume                     1383.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7705
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    5.575
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Long rod'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.0054(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0491P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                2604
_reflns_number_total             3171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205557k.txt
_cod_data_source_block           Compound_I
_cod_database_code               7114160
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.00597(3) 0.21510(8) 0.070543(18) 0.01404(12) Uani 1 1 d .
Zn2 Zn -0.00112(3) 0.73311(7) 0.172723(17) 0.01411(12) Uani 1 1 d .
Zn3 Zn 0.39935(3) -0.22196(8) 0.054651(18) 0.01604(13) Uani 1 1 d .
P1 P 0.13998(7) -0.26768(16) 0.05251(4) 0.01173(19) Uani 1 1 d .
P2 P -0.12672(7) 0.24183(16) 0.18659(4) 0.01230(19) Uani 1 1 d .
P3 P 0.47221(7) -0.29911(17) -0.08318(4) 0.0155(2) Uani 1 1 d .
O1 O 0.11566(19) 0.4457(5) 0.04952(11) 0.0216(5) Uani 1 1 d .
O2 O -0.11773(17) 0.1427(5) 0.01308(10) 0.0181(5) Uani 1 1 d .
O3 O -0.03717(18) 0.3747(5) 0.15073(10) 0.0174(5) Uani 1 1 d .
O4 O 0.06544(17) -0.1298(5) 0.09755(10) 0.0151(5) Uani 1 1 d .
O5 O 0.1017(2) 0.7963(5) 0.24236(11) 0.0221(6) Uani 1 1 d .
O6 O -0.12340(18) 0.9555(4) 0.17088(11) 0.0183(5) Uani 1 1 d .
O7 O 0.39430(19) -0.3291(6) -0.03265(12) 0.0289(6) Uani 1 1 d .
O8 O 0.43111(19) 0.1388(5) 0.06135(13) 0.0266(6) Uani 1 1 d .
O9 O 0.4950(2) -0.4393(5) 0.10692(11) 0.0230(6) Uani 1 1 d .
O10 O 0.25407(18) -0.2198(5) 0.07987(11) 0.0191(5) Uani 1 1 d .
O11 O -0.23193(18) 0.3622(5) 0.16567(12) 0.0240(6) Uani 1 1 d .
H10 H -0.2773 0.2495 0.1607 0.036 Uiso 1 1 calc R
O12 O 0.41077(18) -0.1499(5) -0.14023(11) 0.0233(6) Uani 1 1 d .
H9 H 0.3526 -0.2169 -0.1489 0.035 Uiso 1 1 calc R
O100 O 0.2666(3) -0.7694(6) -0.06258(17) 0.0483(9) Uani 1 1 d .
N1 N 0.2855(2) 0.0398(7) 0.19934(15) 0.0319(8) Uani 1 1 d .
H8 H 0.2743 -0.0263 0.1600 0.038 Uiso 1 1 calc R
H7 H 0.2401 -0.0377 0.2237 0.038 Uiso 1 1 calc R
C2 C 0.3947(4) -0.0187(11) 0.2247(2) 0.0511(14) Uani 1 1 d .
H6 H 0.4049 -0.2020 0.2257 0.077 Uiso 1 1 calc R
H5 H 0.4069 0.0492 0.2670 0.077 Uiso 1 1 calc R
H4 H 0.4435 0.0584 0.1981 0.077 Uiso 1 1 calc R
C1 C 0.2624(5) 0.3139(10) 0.1967(3) 0.0581(15) Uani 1 1 d .
H3 H 0.1902 0.3400 0.1799 0.087 Uiso 1 1 calc R
H2 H 0.3092 0.3975 0.1699 0.087 Uiso 1 1 calc R
H1 H 0.2726 0.3853 0.2387 0.087 Uiso 1 1 calc R
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
O1 Zn1 O2 122.63(10) . .
O1 Zn1 O4 111.28(10) . .
O2 Zn1 O4 105.56(10) . .
O1 Zn1 O3 101.26(10) . .
O2 Zn1 O3 110.25(10) . .
O4 Zn1 O3 104.56(9) . .
O5 Zn2 O6 113.84(10) . .
O5 Zn2 O3 118.36(11) . .
O6 Zn2 O3 113.19(10) . .
O5 Zn2 O4 104.30(10) . 1_565
O6 Zn2 O4 99.50(10) . 1_565
O3 Zn2 O4 104.78(9) . 1_565
O8 Zn3 O7 110.00(12) . .
O8 Zn3 O9 114.34(10) . .
O7 Zn3 O9 110.27(11) . .
O8 Zn3 O10 99.78(11) . .
O7 Zn3 O10 108.11(10) . .
O9 Zn3 O10 113.79(11) . .
O1 P1 O10 110.87(14) 1_545 .
O1 P1 O2 110.86(14) 1_545 3
O10 P1 O2 111.42(13) . 3
O1 P1 O4 109.94(13) 1_545 .
O10 P1 O4 107.11(13) . .
O2 P1 O4 106.47(13) 3 .
O11 P2 O6 112.49(14) . 1_545
O11 P2 O5 108.22(14) . 2_545
O6 P2 O5 112.70(14) 1_545 2_545
O11 P2 O3 109.41(14) . .
O6 P2 O3 106.67(13) 1_545 .
O5 P2 O3 107.19(14) 2_545 .
O8 P3 O9 110.75(15) 3_655 3_645
O8 P3 O7 113.37(15) 3_655 .
O9 P3 O7 110.68(16) 3_645 .
O8 P3 O12 107.01(14) 3_655 .
O9 P3 O12 108.47(14) 3_645 .
O7 P3 O12 106.28(15) . .
P1 O1 Zn1 138.66(16) 1_565 .
P1 O2 Zn1 124.06(14) 3 .
P2 O3 Zn2 117.57(13) . .
P2 O3 Zn1 119.12(13) . .
Zn2 O3 Zn1 121.14(11) . .
P1 O4 Zn2 129.73(14) . 1_545
P1 O4 Zn1 117.66(12) . .
Zn2 O4 Zn1 111.79(10) 1_545 .
P2 O5 Zn2 142.47(16) 2 .
P2 O6 Zn2 128.10(14) 1_565 .
P3 O7 Zn3 132.42(16) . .
P3 O8 Zn3 135.72(16) 3_655 .
P3 O9 Zn3 120.64(14) 3_645 .
P1 O10 Zn3 140.73(15) . .
C1 N1 C2 113.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.915(2) .
Zn1 O2 1.931(2) .
Zn1 O4 2.005(2) .
Zn1 O3 2.006(2) .
Zn2 O5 1.905(2) .
Zn2 O6 1.928(2) .
Zn2 O3 1.961(2) .
Zn2 O4 1.995(2) 1_565
Zn3 O8 1.918(3) .
Zn3 O7 1.924(3) .
Zn3 O9 1.929(2) .
Zn3 O10 1.959(2) .
P1 O1 1.520(2) 1_545
P1 O10 1.527(2) .
P1 O2 1.534(2) 3
P1 O4 1.571(2) .
P2 O11 1.501(2) .
P2 O6 1.524(2) 1_545
P2 O5 1.534(2) 2_545
P2 O3 1.577(2) .
P3 O8 1.517(3) 3_655
P3 O9 1.518(3) 3_645
P3 O7 1.525(3) .
P3 O12 1.579(2) .
O1 P1 1.520(2) 1_565
O2 P1 1.534(2) 3
O4 Zn2 1.995(2) 1_545
O5 P2 1.534(2) 2
O6 P2 1.524(2) 1_565
O8 P3 1.517(3) 3_655
O9 P3 1.518(3) 3_645
N1 C1 1.452(6) .
N1 C2 1.469(5) .
