#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001408.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_4001408
loop_
_publ_author_name
'Chang, Wen-Ming'
'Cheng, Ming-Yu'
'Liao, Yueh-Chun'
'Chang, Ming-Chung'
'Wang, Sue-Lein'
_publ_section_title
;
 Template Effect of Chain-Type Polyamines on Pore Augmentation: Five
 Open-Framework Zinc Phosphates with 16-Ring Channels
;
_journal_issue                   25
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6114
_journal_paper_doi               10.1021/cm071462f
_journal_volume                  19
_journal_year                    2007
_chemical_formula_sum            'C4 H22 N3 O17.5 P4 Zn3'
_chemical_formula_weight         712.24
_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                109.0120(10)
_cell_angle_beta                 90.922(2)
_cell_angle_gamma                91.298(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4552(7)
_cell_length_b                   10.0614(8)
_cell_length_c                   12.8218(10)
_cell_measurement_reflns_used    6224
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      1.68
_cell_volume                     1030.68(14)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX 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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11962
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   none
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    2.295
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0296
_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)+(0.0461P)²+0.6604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                4303
_reflns_number_total             5106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071462f-file003.cif
_cod_data_source_block           fm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C4 H22 N3 O17.50 P4 Zn3'
_cod_database_code               4001408
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
Zn1 Zn 0.05299(4) 0.18217(4) 0.15604(3) 0.01820(10) Uani 1 1 d .
Zn2 Zn 0.25982(4) -0.00168(4) 0.54517(3) 0.01592(9) Uani 1 1 d .
Zn3 Zn 0.18587(4) 0.38327(4) 0.48538(3) 0.01797(10) Uani 1 1 d .
P1 P 0.01905(9) 0.48974(8) 0.30993(7) 0.01720(16) Uani 1 1 d .
P2 P 0.06043(9) 0.08686(8) 0.37536(6) 0.01519(16) Uani 1 1 d .
P3 P 0.50830(9) -0.25216(9) 0.44890(7) 0.01707(17) Uani 1 1 d .
P4 P 0.22787(9) 0.05194(9) -0.07087(7) 0.01842(17) Uani 1 1 d .
O1 O 0.1708(3) 0.4796(3) 0.3752(2) 0.0232(5) Uani 1 1 d .
O2 O -0.1285(3) 0.4772(2) 0.37356(19) 0.0246(5) Uani 1 1 d .
O3 O 0.0263(3) 0.6401(3) 0.2939(2) 0.0278(5) Uani 1 1 d .
O4 O 0.0137(3) 0.3831(3) 0.1941(2) 0.0291(5) Uani 1 1 d .
O5 O 0.1739(3) -0.0177(2) 0.40046(19) 0.0232(5) Uani 1 1 d .
O6 O 0.0493(3) 0.2208(2) 0.47667(19) 0.0227(5) Uani 1 1 d .
O7 O -0.1071(3) 0.0155(3) 0.34531(18) 0.0220(5) Uani 1 1 d .
O8 O 0.1257(3) 0.1223(3) 0.27649(19) 0.0255(5) Uani 1 1 d .
O9 O 0.4009(3) -0.3472(3) 0.3483(2) 0.0323(6) Uani 1 1 d .
O10 O 0.4042(3) -0.1551(3) 0.5354(2) 0.0287(5) Uani 1 1 d .
O11 O 0.6145(3) -0.1730(3) 0.39210(19) 0.0248(5) Uani 1 1 d .
O12 O 0.5934(3) -0.3453(3) 0.5021(2) 0.0278(5) Uani 1 1 d .
O13 O 0.2190(3) 0.1365(3) 0.05098(19) 0.0281(5) Uani 1 1 d .
O14 O 0.1564(3) -0.0996(3) -0.0988(2) 0.0273(5) Uani 1 1 d .
O15 O 0.1228(3) 0.1310(3) -0.1338(2) 0.0276(5) Uani 1 1 d .
O16 O 0.3975(3) 0.0412(3) -0.1082(2) 0.0294(6) Uani 1 1 d .
N1 N 0.3583(4) -0.2583(3) 0.7113(2) 0.0268(6) Uani 1 1 d .
N2 N 0.4071(3) -0.2479(3) 0.9555(2) 0.0248(6) Uani 1 1 d .
N3 N 0.3766(4) -0.1370(4) 1.2216(3) 0.0353(7) Uani 1 1 d .
C1 C 0.5087(4) -0.2846(4) 0.7643(3) 0.0288(8) Uani 1 1 d .
C2 C 0.4778(5) -0.3499(4) 0.8543(3) 0.0328(8) Uani 1 1 d .
C3 C 0.3486(6) -0.3214(4) 1.0336(4) 0.0464(11) Uani 1 1 d .
C4 C 0.2631(5) -0.2212(5) 1.1321(3) 0.0395(10) Uani 1 1 d .
OW1 O 0.3139(6) 0.3549(5) -0.1651(4) 0.0871(14) Uani 1 1 d .
OW2 O 0.060(3) 0.4500(12) -0.0059(13) 0.192(13) Uani 0.50 1 d P
H4 H 0.4773 -0.1733 0.9902 0.050 Uiso 1 1 d .
H10 H 0.3294 -0.4035 0.3639 0.050 Uiso 1 1 d .
H1 H 0.3787 -0.2217 0.6568 0.050 Uiso 1 1 d .
H5 H 0.3201 -0.2069 0.9446 0.050 Uiso 1 1 d .
H2 H 0.3113 -0.1931 0.7603 0.050 Uiso 1 1 d .
H6 H 0.4479 -0.0801 1.1959 0.050 Uiso 1 1 d .
H7 H 0.3213 -0.0667 1.2807 0.050 Uiso 1 1 d .
H3 H 0.2978 -0.3403 0.6897 0.050 Uiso 1 1 d .
H8 H 0.4233 -0.2132 1.2375 0.050 Uiso 1 1 d .
H9 H 0.0091 0.7192 0.3614 0.050 Uiso 1 1 d .
H11 H 0.1219 0.0825 -0.2068 0.050 Uiso 1 1 d .
H12 H 0.3678 0.3392 -0.2269 0.050 Uiso 1 1 d .
H13 H 0.2844 0.4409 -0.1418 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
O13 Zn1 O8 105.20(10) . .
O13 Zn1 O4 108.30(11) . .
O8 Zn1 O4 115.40(11) . .
O13 Zn1 O14 115.18(11) . 2
O8 Zn1 O14 111.82(10) . 2
O4 Zn1 O14 101.25(11) . 2
O5 Zn2 O11 111.16(10) . 2_656
O5 Zn2 O7 116.35(10) . 2_556
O11 Zn2 O7 108.36(10) 2_656 2_556
O5 Zn2 O10 110.52(10) . .
O11 Zn2 O10 106.07(11) 2_656 .
O7 Zn2 O10 103.66(10) 2_556 .
O12 Zn3 O6 112.03(10) 2_656 .
O12 Zn3 O1 106.30(10) 2_656 .
O6 Zn3 O1 121.56(10) . .
O12 Zn3 O2 107.08(11) 2_656 2_566
O6 Zn3 O2 103.10(10) . 2_566
O1 Zn3 O2 105.75(11) . 2_566
O4 P1 O2 111.57(14) . .
O4 P1 O1 112.17(14) . .
O2 P1 O1 110.94(14) . .
O4 P1 O3 105.74(14) . .
O2 P1 O3 109.41(14) . .
O1 P1 O3 106.72(13) . .
O8 P2 O6 110.85(14) . .
O8 P2 O5 107.29(14) . .
O6 P2 O5 110.56(13) . .
O8 P2 O7 109.74(13) . .
O6 P2 O7 109.22(13) . .
O5 P2 O7 109.15(13) . .
O12 P3 O10 107.87(15) . .
O12 P3 O11 115.38(14) . .
O10 P3 O11 112.87(14) . .
O12 P3 O9 109.38(15) . .
O10 P3 O9 109.57(15) . .
O11 P3 O9 101.53(13) . .
O16 P4 O13 110.97(14) . .
O16 P4 O14 108.06(14) . .
O13 P4 O14 112.75(15) . .
O16 P4 O15 111.93(15) . .
O13 P4 O15 105.89(14) . .
O14 P4 O15 107.22(13) . .
P1 O1 Zn3 125.39(13) . .
P1 O2 Zn3 124.07(13) . 2_566
P1 O3 H9 114.4 . .
P1 O4 Zn1 125.87(15) . .
P2 O5 Zn2 125.21(14) . .
P2 O6 Zn3 118.64(13) . .
P2 O7 Zn2 123.80(13) . 2_556
P2 O8 Zn1 139.91(14) . .
P3 O9 H10 116.2 . .
P3 O10 Zn2 137.45(16) . .
P3 O11 Zn2 129.97(15) . 2_656
P3 O12 Zn3 132.39(15) . 2_656
P4 O13 Zn1 134.88(15) . .
P4 O14 Zn1 132.18(15) . 2
P4 O15 H11 109.0 . .
C1 N1 H1 111.2 . .
C1 N1 H2 106.8 . .
H1 N1 H2 104.8 . .
C1 N1 H3 108.1 . .
H1 N1 H3 114.9 . .
H2 N1 H3 110.8 . .
C3 N2 C2 111.5(3) . .
C3 N2 H4 112.1 . .
C2 N2 H4 111.5 . .
C3 N2 H5 100.6 . .
C2 N2 H5 116.3 . .
H4 N2 H5 104.2 . .
C4 N3 H6 111.8 . .
C4 N3 H7 111.3 . .
H6 N3 H7 102.6 . .
C4 N3 H8 97.8 . .
H6 N3 H8 115.0 . .
H7 N3 H8 118.7 . .
N1 C1 C2 112.3(3) . .
N2 C2 C1 112.6(3) . .
N2 C3 C4 112.1(3) . .
N3 C4 C3 112.2(4) . .
H12 OW1 H13 110.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O13 1.919(2) .
Zn1 O8 1.928(2) .
Zn1 O4 1.957(2) .
Zn1 O14 1.964(2) 2
Zn2 O5 1.937(2) .
Zn2 O11 1.957(2) 2_656
Zn2 O7 1.959(2) 2_556
Zn2 O10 1.963(2) .
Zn3 O12 1.928(2) 2_656
Zn3 O6 1.951(2) .
Zn3 O1 1.960(2) .
Zn3 O2 1.970(2) 2_566
P1 O4 1.522(2) .
P1 O2 1.527(2) .
P1 O1 1.544(2) .
P1 O3 1.592(2) .
P2 O8 1.532(2) .
P2 O6 1.543(2) .
P2 O5 1.544(2) .
P2 O7 1.558(2) .
P3 O12 1.514(2) .
P3 O10 1.524(3) .
P3 O11 1.529(2) .
P3 O9 1.588(2) .
P4 O16 1.514(2) .
P4 O13 1.520(2) .
P4 O14 1.553(2) .
P4 O15 1.581(3) .
O2 Zn3 1.970(2) 2_566
O3 H9 0.9815 .
O7 Zn2 1.959(2) 2_556
O9 H10 0.8882 .
O11 Zn2 1.957(2) 2_656
O12 Zn3 1.928(2) 2_656
O14 Zn1 1.964(2) 2
O15 H11 0.9036 .
N1 C1 1.502(5) .
N1 H1 0.9065 .
N1 H2 0.8568 .
N1 H3 0.9203 .
N2 C3 1.509(5) .
N2 C2 1.510(5) .
N2 H4 0.9310 .
N2 H5 0.8827 .
N3 C4 1.500(5) .
N3 H6 0.9559 .
N3 H7 0.9853 .
N3 H8 0.9476 .
C1 C2 1.525(5) .
C3 C4 1.538(6) .
OW1 H12 0.8915 .
OW1 H13 0.8630 .
OW2 OW2 1.42(4) 2_565
