#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:16:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180255 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/41/7114145.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_7114145
loop_
_publ_author_name
'Natarajan, Srinivasan'
_publ_section_title
;
 Synthesis of a layered zinc phosphate,
 [NH3(CH2)2NH2(CH2)3NH3][Zn2(PO4)(HPO4)2]·H2O, and its
 transformation to a extra-large pore three-dimensional zinc phosphate,
 [NH3(CH2)2NH2(CH2)3NH3][Zn3(PO4)(HPO4)3]
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              780
_journal_paper_doi               10.1039/b200293k
_journal_year                    2002
_chemical_formula_sum            'C5 H21 N3 O16 P4 Zn3'
_chemical_formula_weight         699.24
_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
_cell_angle_alpha                81.1140(10)
_cell_angle_beta                 83.6420(10)
_cell_angle_gamma                72.626(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4557(2)
_cell_length_b                   9.28440(10)
_cell_length_c                   13.8599(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1023.57(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  SHELXTL-PLUS
_computing_structure_solution    SHELXTL-PLUS
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4348
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    3.882
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.681841
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    2.269
_exptl_crystal_description       colorless
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_obs          0.0299
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0427P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0808
_refine_ls_wR_factor_obs         0.0752
_reflns_number_observed          2484
_reflns_number_total             2904
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b200293k.txt
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1023.57(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114145
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.29367(6) 0.91830(6) 0.51946(4) 0.0175(2) Uani 1 d .
Zn2 Zn 0.74556(6) 1.49370(6) -0.02699(4) 0.0160(2) Uani 1 d .
Zn3 Zn 0.63779(6) 0.88788(6) 0.12587(4) 0.0158(2) Uani 1 d .
P1 P 0.58114(14) 1.21710(13) 0.01996(8) 0.0141(3) Uani 1 d .
P2 P 0.58470(14) 0.86461(13) 0.36397(8) 0.0159(3) Uani 1 d .
P3 P 0.90460(14) 1.56629(13) 0.14874(8) 0.0154(3) Uani 1 d .
P4 P 0.01690(14) 1.20793(14) 0.42267(8) 0.0178(3) Uani 1 d .
O1 O 0.1668(4) 1.0703(4) 0.4238(2) 0.0295(8) Uani 1 d .
O2 O 0.4718(4) 0.7992(3) 0.4396(2) 0.0237(8) Uani 1 d .
O3 O 0.4033(4) 0.9820(3) 0.6163(2) 0.0226(7) Uani 1 d .
O4 O 0.1403(4) 0.8210(4) 0.6032(2) 0.0247(8) Uani 1 d .
O5 O 0.8141(4) 1.4767(4) 0.1035(2) 0.0287(8) Uani 1 d .
O6 O 0.9089(4) 1.5020(4) -0.1349(2) 0.0273(8) Uani 1 d .
O7 O 0.7098(4) 1.2965(3) -0.0300(2) 0.0227(7) Uani 1 d .
O8 O 0.5648(4) 1.6714(4) -0.0697(2) 0.0266(8) Uani 1 d .
O9 O 0.6642(4) 1.0918(3) 0.1018(2) 0.0199(7) Uani 1 d .
O10 O 0.8500(4) 0.7362(3) 0.1126(2) 0.0229(7) Uani 1 d .
O11 O 0.4689(4) 0.8557(4) 0.0581(2) 0.0248(8) Uani 1 d .
O12 O 0.5306(4) 0.8757(4) 0.2614(2) 0.0216(7) Uani 1 d .
O13 O 0.7678(4) 0.7538(4) 0.3695(2) 0.0281(8) Uani 1 d .
H20 H 0.7690(4) 0.6694(4) 0.3580(2) 0.042 Uiso 1 calc R
O14 O 0.8576(4) 1.5443(3) 0.2622(2) 0.0227(7) Uani 1 d .
H30 H 0.8847(4) 1.4533(3) 0.2829(2) 0.034 Uiso 1 calc R
O15 O 0.0579(4) 1.3336(4) 0.3493(3) 0.0319(9) Uani 1 d .
O16 O -0.0235(4) 1.2597(4) 0.5276(2) 0.0374(9) Uani 1 d .
H20' H 0.0562(4) 1.2812(4) 0.5438(2) 0.056 Uiso 1 calc R
N1 N 0.9045(5) 1.1629(4) 0.1865(3) 0.0260(10) Uani 1 d .
H1 H 0.8982(5) 1.2513(4) 0.1493(3) 0.039 Uiso 1 calc R
H2 H 0.8869(5) 1.1776(4) 0.2492(3) 0.039 Uiso 1 calc R
H3 H 0.8279(5) 1.1240(4) 0.1708(3) 0.039 Uiso 1 calc R
C1 C 1.0732(6) 1.0550(6) 0.1700(4) 0.0297(12) Uani 1 d .
H4 H 1.1575(6) 1.0968(6) 0.1866(4) 0.036 Uiso 1 calc R
H5 H 1.0936(6) 1.0387(6) 0.1017(4) 0.036 Uiso 1 calc R
C2 C 1.0802(6) 0.9046(5) 0.2346(4) 0.0251(11) Uani 1 d .
H6 H 1.0567(6) 0.9225(5) 0.3025(4) 0.030 Uiso 1 calc R
H7 H 0.9958(6) 0.8636(5) 0.2173(4) 0.030 Uiso 1 calc R
N2 N 1.2453(5) 0.7927(4) 0.2230(3) 0.0239(9) Uani 1 d .
H8 H 1.3227(5) 0.8337(4) 0.2370(3) 0.029 Uiso 1 calc R
H9 H 1.2651(5) 0.7768(4) 0.1598(3) 0.029 Uiso 1 calc R
C3 C 1.2665(6) 0.6428(5) 0.2847(3) 0.0244(11) Uani 1 d .
H10 H 1.1858(6) 0.5956(5) 0.2696(3) 0.029 Uiso 1 calc R
H11 H 1.2478(6) 0.6573(5) 0.3533(3) 0.029 Uiso 1 calc R
C4 C 1.4402(6) 0.5406(5) 0.2654(4) 0.0285(12) Uani 1 d .
H12 H 1.4606(6) 0.5343(5) 0.1958(4) 0.034 Uiso 1 calc R
H13 H 1.5194(6) 0.5864(5) 0.2844(4) 0.034 Uiso 1 calc R
C5 C 1.4699(6) 0.3822(6) 0.3193(4) 0.0323(13) Uani 1 d .
H14 H 1.5887(6) 0.3336(6) 0.3186(4) 0.039 Uiso 1 calc R
H15 H 1.4284(6) 0.3892(6) 0.3870(4) 0.039 Uiso 1 calc R
N3 N 1.3906(5) 0.2847(4) 0.2779(3) 0.0254(9) Uani 1 d .
H16 H 1.4130(5) 0.1931(4) 0.3131(3) 0.038 Uiso 1 calc R
H17 H 1.4300(5) 0.2754(4) 0.2162(3) 0.038 Uiso 1 calc R
H18 H 1.2811(5) 0.3270(4) 0.2797(3) 0.038 Uiso 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
O2 Zn1 O1 102.76(13) . .
O2 Zn1 O3 105.32(13) . .
O1 Zn1 O3 119.38(14) . .
O2 Zn1 O4 120.06(14) . .
O1 Zn1 O4 108.21(14) . .
O3 Zn1 O4 102.12(13) . .
O5 Zn2 O6 117.70(14) . .
O5 Zn2 O7 102.87(13) . .
O6 Zn2 O7 102.16(14) . .
O5 Zn2 O8 117.37(14) . .
O6 Zn2 O8 100.39(13) . .
O7 Zn2 O8 115.94(14) . .
O11 Zn3 O10 113.52(14) . .
O11 Zn3 O9 115.96(13) . .
O10 Zn3 O9 110.82(13) . .
O11 Zn3 O12 98.74(13) . .
O10 Zn3 O12 112.98(13) . .
O9 Zn3 O12 103.85(13) . .
O11 P1 O8 113.7(2) 2_675 2_685
O11 P1 O7 106.7(2) 2_675 .
O8 P1 O7 111.1(2) 2_685 .
O11 P1 O9 109.6(2) 2_675 .
O8 P1 O9 106.8(2) 2_685 .
O7 P1 O9 108.7(2) . .
O2 P2 O12 110.7(2) . .
O2 P2 O3 113.2(2) . 2_676
O12 P2 O3 110.7(2) . 2_676
O2 P2 O13 108.4(2) . .
O12 P2 O13 108.3(2) . .
O3 P2 O13 105.3(2) 2_676 .
O6 P3 O5 110.6(2) 2_785 .
O6 P3 O10 112.3(2) 2_785 1_565
O5 P3 O10 112.9(2) . 1_565
O6 P3 O14 106.7(2) 2_785 .
O5 P3 O14 105.9(2) . .
O10 P3 O14 108.0(2) 1_565 .
O1 P4 O15 107.7(2) . .
O1 P4 O4 113.8(2) . 2_576
O15 P4 O4 109.9(2) . 2_576
O1 P4 O16 109.6(2) . .
O15 P4 O16 110.2(2) . .
O4 P4 O16 105.7(2) 2_576 .
P4 O1 Zn1 138.0(2) . .
P2 O2 Zn1 124.6(2) . .
P2 O3 Zn1 134.0(2) 2_676 .
P4 O4 Zn1 129.2(2) 2_576 .
P3 O5 Zn2 132.0(2) . .
P3 O6 Zn2 134.3(2) 2_785 .
P1 O7 Zn2 134.5(2) . .
P1 O8 Zn2 136.2(2) 2_685 .
P1 O9 Zn3 124.5(2) . .
P3 O10 Zn3 131.3(2) 1_545 .
P1 O11 Zn3 150.0(2) 2_675 .
P2 O12 Zn3 135.9(2) . .
P2 O13 H20 109.47(13) . .
P3 O14 H30 109.47(12) . .
P4 O16 H20 109.47(13) . .
C1 N1 H1 109.5(2) . .
C1 N1 H2 109.5(3) . .
H1 N1 H2 109.5 . .
C1 N1 H3 109.5(3) . .
H1 N1 H3 109.5 . .
H2 N1 H3 109.5 . .
N1 C1 C2 108.3(4) . .
N1 C1 H4 110.0(3) . .
C2 C1 H4 110.0(3) . .
N1 C1 H5 110.0(3) . .
C2 C1 H5 110.0(3) . .
H4 C1 H5 108.4 . .
N2 C2 C1 111.2(4) . .
N2 C2 H6 109.4(2) . .
C1 C2 H6 109.4(3) . .
N2 C2 H7 109.4(2) . .
C1 C2 H7 109.4(3) . .
H6 C2 H7 108.0 . .
C2 N2 C3 115.5(4) . .
C2 N2 H8 108.4(2) . .
C3 N2 H8 108.4(2) . .
C2 N2 H9 108.4(2) . .
C3 N2 H9 108.4(2) . .
H8 N2 H9 107.5 . .
N2 C3 C4 109.8(4) . .
N2 C3 H10 109.7(2) . .
C4 C3 H10 109.7(3) . .
N2 C3 H11 109.7(2) . .
C4 C3 H11 109.7(3) . .
H10 C3 H11 108.2 . .
C5 C4 C3 113.7(4) . .
C5 C4 H12 108.8(3) . .
C3 C4 H12 108.8(3) . .
C5 C4 H13 108.8(3) . .
C3 C4 H13 108.8(3) . .
H12 C4 H13 107.7 . .
N3 C5 C4 114.2(4) . .
N3 C5 H14 108.7(2) . .
C4 C5 H14 108.7(3) . .
N3 C5 H15 108.7(2) . .
C4 C5 H15 108.7(3) . .
H14 C5 H15 107.6 . .
C5 N3 H16 109.5(2) . .
C5 N3 H17 109.5(2) . .
H16 N3 H17 109.5 . .
C5 N3 H18 109.5(2) . .
H16 N3 H18 109.5 . .
H17 N3 H18 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.932(3) .
Zn1 O1 1.932(3) .
Zn1 O3 1.964(3) .
Zn1 O4 1.971(3) .
Zn2 O5 1.928(3) .
Zn2 O6 1.929(3) .
Zn2 O7 1.950(3) .
Zn2 O8 1.949(3) .
Zn3 O11 1.910(3) .
Zn3 O10 1.932(3) .
Zn3 O9 1.945(3) .
Zn3 O12 1.996(3) .
P1 O11 1.518(3) 2_675
P1 O8 1.530(3) 2_685
P1 O7 1.537(3) .
P1 O9 1.553(3) .
P2 O2 1.519(3) .
P2 O12 1.520(3) .
P2 O3 1.526(3) 2_676
P2 O13 1.585(3) .
P3 O6 1.517(3) 2_785
P3 O5 1.523(3) .
P3 O10 1.524(3) 1_565
P3 O14 1.576(3) .
P4 O1 1.507(3) .
P4 O15 1.521(3) .
P4 O4 1.522(3) 2_576
P4 O16 1.572(3) .
O3 P2 1.526(3) 2_676
O4 P4 1.522(3) 2_576
O6 P3 1.517(3) 2_785
O8 P1 1.530(3) 2_685
O10 P3 1.524(3) 1_545
O11 P1 1.518(3) 2_675
O13 H20 0.82 .
O14 H30 0.82 .
O16 H20 0.82 .
N1 C1 1.495(6) .
N1 H1 0.89 .
N1 H2 0.89 .
N1 H3 0.89 .
C1 C2 1.526(6) .
C1 H4 0.97 .
C1 H5 0.97 .
C2 N2 1.480(6) .
C2 H6 0.97 .
C2 H7 0.97 .
N2 C3 1.489(6) .
N2 H8 0.90 .
N2 H9 0.90 .
C3 C4 1.512(6) .
C3 H10 0.97 .
C3 H11 0.97 .
C4 C5 1.504(7) .
C4 H12 0.97 .
C4 H13 0.97 .
C5 N3 1.486(6) .
C5 H14 0.97 .
C5 H15 0.97 .
N3 H16 0.89 .
N3 H17 0.89 .
N3 H18 0.89 .
