# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NTHU-11-cha
_database_code_depnum_ccdc_archive 'CCDC 848200'
_audit_update_record             
;
2011-10-11 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
#TrackingRef '7594_web_deposit_cif_file_0_Hsin-YauLin_1318347903.NTHU-11-cha.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         (NC6H14)2[Zn3(HPO3)3.5(HPO4)0.5]
_chemical_formula_sum            'C12 H32 N2 O12.5 P4 Zn3'
_chemical_formula_weight         724.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   32.4965(8)
_cell_length_b                   32.4965(8)
_cell_length_c                   13.1823(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12055.8(6)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9898
_cell_measurement_theta_min      3.70
_cell_measurement_theta_max      67.04

_exptl_crystal_description       Columnar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6552
_exptl_absorpt_coefficient_mu    5.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_T_max  0.9287
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30753
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         67.04
_reflns_number_total             4699
_reflns_number_gt                4441
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0336P)²+47.3262P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    const
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4699
_refine_ls_number_parameters     318
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.709795(11) 0.010914(10) 0.90866(2) 0.01737(9) Uani 1 1 d . . .
Zn2 Zn 0.663333(12) -0.108125(11) 0.35209(2) 0.02196(9) Uani 1 1 d . . .
Zn3 Zn 0.669399(12) -0.165791(11) 0.66545(2) 0.02112(9) Uani 1 1 d . . .
P1 P 0.66787(2) 0.04072(2) 0.72949(4) 0.01701(13) Uani 1 1 d . . .
P2 P 0.67762(2) -0.09229(2) 0.84354(4) 0.01782(13) Uani 1 1 d . . .
P3 P 0.59627(2) -0.14929(2) 0.54553(5) 0.02147(14) Uani 1 1 d . . .
P4 P 0.72527(2) -0.14534(2) 0.46583(4) 0.02116(14) Uani 1 1 d . . .
O1 O 0.68776(6) 0.04860(5) 0.83714(12) 0.0195(3) Uani 1 1 d . . .
O2 O 0.67822(6) -0.01631(6) 1.03648(11) 0.0190(3) Uani 1 1 d . . .
O3 O 0.69505(7) -0.04010(6) 0.31869(12) 0.0262(4) Uani 1 1 d . . .
O4 O 0.70989(6) -0.03897(6) 0.82737(12) 0.0206(3) Uani 1 1 d . . .
O5 O 0.69163(7) -0.11860(6) 0.76973(13) 0.0265(4) Uani 1 1 d . . .
O6 O 0.65461(7) -0.22763(6) 0.71359(13) 0.0278(4) Uani 1 1 d . . .
O7 O 0.61466(6) -0.18199(6) 0.57862(14) 0.0280(4) Uani 1 1 d . . .
O8 O 0.60798(6) -0.13232(6) 0.43697(13) 0.0266(4) Uani 1 1 d . . .
O9 O 0.77531(6) 0.05248(6) 0.95322(13) 0.0257(4) Uani 1 1 d . . .
O10 O 0.72498(6) -0.13217(6) 0.57657(13) 0.0277(4) Uani 1 1 d . . .
O11 O 0.71645(7) -0.11491(7) 0.39304(14) 0.0304(4) Uani 1 1 d . . .
O12 O 0.64010(7) -0.13512(6) 0.21758(13) 0.0322(4) Uani 1 1 d . . .
O13 O 0.6390(2) 0.0666(2) 0.7302(6) 0.029(2) Uani 0.248(7) 1 d P . .
O14 O 0.6261(2) -0.1085(2) 0.8200(4) 0.026(2) Uani 0.285(6) 1 d P . .
N1 N 0.70194(7) 0.12308(7) 0.97056(15) 0.0230(4) Uani 1 1 d . . .
C1 C 0.67680(8) 0.15090(8) 0.97598(19) 0.0227(5) Uani 1 1 d . . .
C2 C 0.69769(11) 0.18612(10) 1.0626(2) 0.0319(6) Uani 1 1 d . . .
C3 C 0.67346(13) 0.21586(12) 1.0698(3) 0.0483(8) Uani 1 1 d . . .
C4 C 0.67795(12) 0.24170(11) 0.9703(3) 0.0462(8) Uani 1 1 d . . .
C5 C 0.65822(11) 0.20699(11) 0.8827(3) 0.0410(7) Uani 1 1 d . . .
C6 C 0.68112(10) 0.17574(10) 0.8755(2) 0.0309(6) Uani 1 1 d . . .
N2 N 0.73271(8) -0.05616(8) 0.13853(16) 0.0295(5) Uani 1 1 d . . .
C7 C 0.78514(10) -0.02648(10) 0.1369(2) 0.0316(6) Uani 1 1 d . . .
C8 C 0.80547(10) -0.03351(11) 0.0395(2) 0.0350(6) Uani 1 1 d . . .
C9 C 0.85925(12) -0.00228(14) 0.0375(3) 0.0543(9) Uani 1 1 d . . .
C10 C 0.88121(12) -0.01218(16) 0.1307(3) 0.0636(11) Uani 1 1 d . . .
C11 C 0.86030(13) -0.00708(16) 0.2295(3) 0.0647(11) Uani 1 1 d . . .
C12 C 0.80606(12) -0.03710(15) 0.2286(2) 0.0524(9) Uani 1 1 d . . .
H1 H 0.6314 0.0514 0.7313 0.050 Uiso 0.75 1 d P . .
H2 H 0.6308 -0.1046 0.8268 0.050 Uiso 0.71 1 d P . .
H3 H 0.5505 -0.1750 0.5491 0.050 Uiso 1 1 d . . .
H4 H 0.7695 -0.1379 0.4540 0.050 Uiso 1 1 d . . .
H1A H 0.6906 0.1024 0.9294 0.080 Uiso 1 1 d . . .
H1C H 0.7338 0.1450 0.9566 0.080 Uiso 1 1 d . . .
H1B H 0.6997 0.1088 1.0315 0.080 Uiso 1 1 d . . .
H1D H 0.6425 0.1281 0.9909 0.080 Uiso 1 1 d . . .
H1E H 0.6861 0.2395 1.1285 0.080 Uiso 1 1 d . . .
H2A H 0.7205 -0.0496 0.0818 0.080 Uiso 1 1 d . . .
H2B H 0.7206 -0.0491 0.1907 0.080 Uiso 1 1 d . . .
H2C H 0.7233 -0.0918 0.1398 0.080 Uiso 1 1 d . . .
H2D H 0.6938 0.1693 1.1219 0.080 Uiso 1 1 d . . .
H2E H 0.7321 0.2076 1.0486 0.080 Uiso 1 1 d . . .
H3A H 0.6377 0.1922 1.0899 0.080 Uiso 1 1 d . . .
H4A H 0.7125 0.2647 0.9562 0.080 Uiso 1 1 d . . .
H4B H 0.6635 0.2628 0.9737 0.080 Uiso 1 1 d . . .
H5A H 0.6211 0.1875 0.8913 0.080 Uiso 1 1 d . . .
H5B H 0.6633 0.2234 0.8196 0.080 Uiso 1 1 d . . .
H6A H 0.7160 0.1975 0.8624 0.080 Uiso 1 1 d . . .
H6B H 0.6693 0.1551 0.8230 0.080 Uiso 1 1 d . . .
H7A H 0.7918 0.0081 0.1432 0.080 Uiso 1 1 d . . .
H8A H 0.7960 -0.0682 0.0302 0.080 Uiso 1 1 d . . .
H8B H 0.7908 -0.0243 -0.0203 0.080 Uiso 1 1 d . . .
H9A H 0.8699 -0.0095 -0.0322 0.080 Uiso 1 1 d . . .
H9B H 0.8706 0.0351 0.0369 0.080 Uiso 1 1 d . . .
H10A H 0.9179 0.0107 0.1288 0.080 Uiso 1 1 d . . .
H10B H 0.8718 -0.0495 0.1231 0.080 Uiso 1 1 d . . .
H11A H 0.8665 0.0282 0.2328 0.080 Uiso 1 1 d . . .
H11B H 0.8708 -0.0207 0.2905 0.080 Uiso 1 1 d . . .
H12A H 0.7930 -0.0340 0.2951 0.080 Uiso 1 1 d . . .
H12B H 0.7958 -0.0783 0.2270 0.080 Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O2 1.9408(16) . ?
Zn1 O1 1.9440(16) . ?
Zn1 O4 1.9445(16) . ?
Zn1 O9 1.9561(17) . ?
Zn2 O8 1.9213(18) . ?
Zn2 O11 1.9236(18) . ?
Zn2 O12 1.9548(18) . ?
Zn2 O3 1.9657(17) . ?
Zn3 O5 1.9120(16) . ?
Zn3 O6 1.9252(17) . ?
Zn3 O7 1.9533(18) . ?
Zn3 O10 1.9635(18) . ?
P1 O2 1.5148(16) 9_654 ?
P1 O3 1.5213(17) 5_545 ?
P1 O1 1.5268(16) . ?
P1 O13 1.541(7) . ?
P1 H1 1.3904 . ?
P2 O5 1.5081(17) . ?
P2 O6 1.5140(18) 16_646 ?
P2 O14 1.514(6) . ?
P2 O4 1.5264(17) . ?
P2 H2 1.3840 . ?
P3 O8 1.5123(18) . ?
P3 O9 1.5195(18) 9_654 ?
P3 O7 1.5202(18) . ?
P3 H3 1.2923 . ?
P4 O11 1.5048(18) . ?
P4 O12 1.5154(19) 16_645 ?
P4 O10 1.5225(18) . ?
P4 H4 1.3422 . ?
O2 P1 1.5149(16) 5_545 ?
O3 P1 1.5213(17) 9_654 ?
O6 P2 1.5139(18) 16_646 ?
O9 P3 1.5194(18) 5_545 ?
O12 P4 1.5153(19) 16_645 ?
O13 H1 0.4281 . ?
O14 H2 0.1665 . ?
N1 C1 1.493(3) . ?
N1 H1A 0.7962 . ?
N1 H1C 0.9358 . ?
N1 H1B 0.9122 . ?
C1 C2 1.516(4) . ?
C1 C6 1.520(4) . ?
C1 H1D 1.0021 . ?
C2 C3 1.524(4) . ?
C2 H2D 0.9253 . ?
C2 H2E 0.9957 . ?
C3 C4 1.524(5) . ?
C3 H1E 1.0212 . ?
C3 H3A 1.0575 . ?
C4 C5 1.514(5) . ?
C4 H4A 1.0073 . ?
C4 H4B 1.0073 . ?
C5 C6 1.533(4) . ?
C5 H5A 1.0511 . ?
C5 H5B 0.9574 . ?
C6 H6A 1.0067 . ?
C6 H6B 0.9051 . ?
N2 C7 1.480(3) . ?
N2 H2A 0.9201 . ?
N2 H2B 0.8779 . ?
N2 H2C 1.0397 . ?
C7 C12 1.509(4) . ?
C7 C8 1.513(4) . ?
C7 H7A 1.0360 . ?
C8 C9 1.520(4) . ?
C8 H8A 1.0165 . ?
C8 H8B 1.0395 . ?
C9 C10 1.534(5) . ?
C9 H9A 1.0492 . ?
C9 H9B 1.0786 . ?
C10 C11 1.515(6) . ?
C10 H10A 1.0435 . ?
C10 H10B 1.0971 . ?
C11 C12 1.530(5) . ?
C11 H11A 1.0610 . ?
C11 H11B 1.0539 . ?
C12 H12A 1.0009 . ?
C12 H12B 1.2074 . ?

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
O2 Zn1 O1 115.53(7) . . ?
O2 Zn1 O4 108.62(7) . . ?
O1 Zn1 O4 114.37(7) . . ?
O2 Zn1 O9 101.47(7) . . ?
O1 Zn1 O9 109.10(7) . . ?
O4 Zn1 O9 106.64(7) . . ?
O8 Zn2 O11 119.99(7) . . ?
O8 Zn2 O12 105.79(8) . . ?
O11 Zn2 O12 111.75(8) . . ?
O8 Zn2 O3 116.61(7) . . ?
O11 Zn2 O3 101.28(8) . . ?
O12 Zn2 O3 99.74(7) . . ?
O5 Zn3 O6 113.41(7) . . ?
O5 Zn3 O7 124.44(8) . . ?
O6 Zn3 O7 101.15(8) . . ?
O5 Zn3 O10 96.27(7) . . ?
O6 Zn3 O10 117.23(8) . . ?
O7 Zn3 O10 105.11(8) . . ?
O2 P1 O3 112.25(9) 9_654 5_545 ?
O2 P1 O1 112.06(9) 9_654 . ?
O3 P1 O1 111.59(9) 5_545 . ?
O2 P1 O13 113.9(3) 9_654 . ?
O3 P1 O13 103.4(3) 5_545 . ?
O1 P1 O13 103.0(3) . . ?
O2 P1 H1 98.7 9_654 . ?
O3 P1 H1 115.0 5_545 . ?
O1 P1 H1 106.5 . . ?
O13 P1 H1 15.7 . . ?
O5 P2 O6 113.24(10) . 16_646 ?
O5 P2 O14 105.4(2) . . ?
O6 P2 O14 106.0(2) 16_646 . ?
O5 P2 O4 108.82(10) . . ?
O6 P2 O4 111.00(9) 16_646 . ?
O14 P2 O4 112.3(2) . . ?
O5 P2 H2 109.5 . . ?
O6 P2 H2 104.4 16_646 . ?
O14 P2 H2 4.1 . . ?
O4 P2 H2 109.8 . . ?
O8 P3 O9 112.43(10) . 9_654 ?
O8 P3 O7 114.29(10) . . ?
O9 P3 O7 111.55(10) 9_654 . ?
O8 P3 H3 105.6 . . ?
O9 P3 H3 106.9 9_654 . ?
O7 P3 H3 105.4 . . ?
O11 P4 O12 113.82(11) . 16_645 ?
O11 P4 O10 113.37(11) . . ?
O12 P4 O10 111.18(10) 16_645 . ?
O11 P4 H4 110.3 . . ?
O12 P4 H4 104.7 16_645 . ?
O10 P4 H4 102.6 . . ?
P1 O1 Zn1 127.11(9) . . ?
P1 O2 Zn1 129.17(10) 5_545 . ?
P1 O3 Zn2 123.86(10) 9_654 . ?
P2 O4 Zn1 125.65(10) . . ?
P2 O5 Zn3 144.93(12) . . ?
P2 O6 Zn3 125.84(10) 16_646 . ?
P3 O7 Zn3 127.08(11) . . ?
P3 O8 Zn2 135.54(11) . . ?
P3 O9 Zn1 122.34(10) 5_545 . ?
P4 O10 Zn3 123.29(10) . . ?
P4 O11 Zn2 136.96(12) . . ?
P4 O12 Zn2 122.22(11) 16_645 . ?
P1 O13 H1 61.8 . . ?
P2 O14 H2 36.6 . . ?
C1 N1 H1A 112.4 . . ?
C1 N1 H1C 106.3 . . ?
H1A N1 H1C 112.2 . . ?
C1 N1 H1B 109.7 . . ?
H1A N1 H1B 106.6 . . ?
H1C N1 H1B 109.7 . . ?
N1 C1 C2 108.6(2) . . ?
N1 C1 C6 110.3(2) . . ?
C2 C1 C6 111.6(2) . . ?
N1 C1 H1D 107.7 . . ?
C2 C1 H1D 108.8 . . ?
C6 C1 H1D 109.7 . . ?
C1 C2 C3 110.3(2) . . ?
C1 C2 H2D 108.2 . . ?
C3 C2 H2D 111.2 . . ?
C1 C2 H2E 108.1 . . ?
C3 C2 H2E 108.8 . . ?
H2D C2 H2E 110.2 . . ?
C4 C3 C2 111.0(2) . . ?
C4 C3 H1E 110.2 . . ?
C2 C3 H1E 112.5 . . ?
C4 C3 H3A 112.6 . . ?
C2 C3 H3A 106.4 . . ?
H1E C3 H3A 103.8 . . ?
C5 C4 C3 110.9(3) . . ?
C5 C4 H4A 108.2 . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4B 111.9 . . ?
C3 C4 H4B 112.8 . . ?
H4A C4 H4B 103.2 . . ?
C4 C5 C6 112.1(2) . . ?
C4 C5 H5A 107.3 . . ?
C6 C5 H5A 113.5 . . ?
C4 C5 H5B 110.9 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 104.8 . . ?
C1 C6 C5 110.6(2) . . ?
C1 C6 H6A 107.2 . . ?
C5 C6 H6A 107.1 . . ?
C1 C6 H6B 112.4 . . ?
C5 C6 H6B 111.8 . . ?
H6A C6 H6B 107.5 . . ?
C7 N2 H2A 109.0 . . ?
C7 N2 H2B 111.2 . . ?
H2A N2 H2B 105.9 . . ?
C7 N2 H2C 109.1 . . ?
H2A N2 H2C 110.5 . . ?
H2B N2 H2C 111.0 . . ?
N2 C7 C12 110.0(2) . . ?
N2 C7 C8 111.2(2) . . ?
C12 C7 C8 111.4(3) . . ?
N2 C7 H7A 104.7 . . ?
C12 C7 H7A 108.1 . . ?
C8 C7 H7A 111.2 . . ?
C7 C8 C9 110.9(3) . . ?
C7 C8 H8A 110.9 . . ?
C9 C8 H8A 110.4 . . ?
C7 C8 H8B 107.6 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C9 C10 110.3(3) . . ?
C8 C9 H9A 105.3 . . ?
C10 C9 H9A 114.5 . . ?
C8 C9 H9B 112.6 . . ?
C10 C9 H9B 108.0 . . ?
H9A C9 H9B 106.3 . . ?
C11 C10 C9 112.6(3) . . ?
C11 C10 H10A 111.0 . . ?
C9 C10 H10A 108.5 . . ?
C11 C10 H10B 107.9 . . ?
C9 C10 H10B 104.9 . . ?
H10A C10 H10B 111.9 . . ?
C10 C11 C12 111.1(3) . . ?
C10 C11 H11A 107.5 . . ?
C12 C11 H11A 103.0 . . ?
C10 C11 H11B 110.7 . . ?
C12 C11 H11B 104.5 . . ?
H11A C11 H11B 119.7 . . ?
C7 C12 C11 111.6(3) . . ?
C7 C12 H12A 114.6 . . ?
C11 C12 H12A 109.9 . . ?
C7 C12 H12B 109.5 . . ?
C11 C12 H12B 107.4 . . ?
H12A C12 H12B 103.3 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        67.04
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.070
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NTHU-11-coa
_database_code_depnum_ccdc_archive 'CCDC 848202'
_audit_update_record             
;
2011-10-11 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
#TrackingRef '7596_web_deposit_cif_file_2_Hsin-YauLin_1318347903.NTHU-11-coa.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         (NC8H18)2[Zn3(HPO3)3.7(HPO4)0.3]
_chemical_formula_sum            'C16 H40 N2 O12.3 P4 Zn3'
_chemical_formula_weight         777.36

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   33.9287(3)
_cell_length_b                   33.9287(3)
_cell_length_c                   13.65790(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13616.0(2)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      2.04
_cell_measurement_theta_max      28.31

_exptl_crystal_description       Columnar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7128
_exptl_absorpt_coefficient_mu    2.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8370
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            60317
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         28.31
_reflns_number_total             7524
_reflns_number_gt                4896
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1037P)²+23.7947P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    const
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7524
_refine_ls_number_parameters     348
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1836
_refine_ls_wR_factor_gt          0.1464
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.130
_refine_ls_shift/su_mean         0.005

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 1.006652(19) 0.30051(2) 0.09770(4) 0.03235(16) Uani 1 1 d . . .
Zn2 Zn 1.10695(2) 0.33025(2) 0.30487(4) 0.04292(19) Uani 1 1 d . . .
Zn3 Zn 0.83190(2) 0.16510(2) 0.00337(4) 0.0499(2) Uani 1 1 d . . .
P1 P 1.04046(4) 0.36810(5) 0.27530(9) 0.0334(3) Uani 1 1 d . . .
P2 P 0.90458(5) 0.22890(5) 0.15465(9) 0.0375(3) Uani 1 1 d . . .
P3 P 1.07681(5) 0.26677(5) 0.11807(10) 0.0424(3) Uani 1 1 d . . .
P4 P 1.13322(5) 0.28230(5) 0.47078(9) 0.0420(3) Uani 1 1 d . . .
O1 O 0.98327(14) 0.30841(13) -0.0251(3) 0.0434(9) Uani 1 1 d . . .
O2 O 1.06646(15) 0.35342(17) 0.3415(3) 0.0562(11) Uani 1 1 d . . .
O3 O 1.04282(12) 0.35762(12) 0.1683(2) 0.0385(8) Uani 1 1 d . . .
O4 O 0.95576(12) 0.25302(13) 0.1690(3) 0.0462(9) Uani 1 1 d . . .
O5 O 0.78476(14) 0.13933(15) 0.0993(3) 0.0592(12) Uani 1 1 d . . .
O6 O 0.89151(13) 0.20926(15) 0.0535(3) 0.0568(12) Uani 1 1 d . . .
O7 O 1.07666(15) 0.27585(15) 0.2269(3) 0.0548(11) Uani 1 1 d . . .
O8 O 0.84103(15) 0.12340(16) -0.0757(3) 0.0637(12) Uani 1 1 d . . .
O9 O 1.05018(16) 0.28265(17) 0.0576(3) 0.0592(12) Uani 1 1 d . . .
O10 O 1.11948(16) 0.31562(17) 0.4347(3) 0.0616(12) Uani 1 1 d . . .
O11 O 1.17430(15) 0.28629(16) 0.4203(4) 0.0649(12) Uani 1 1 d . . .
O12 O 1.1366(2) 0.28284(18) 0.5803(3) 0.0761(15) Uani 1 1 d . . .
O13 O 0.8893(9) 0.2619(8) 0.1795(16) 0.127(11) Uani 0.335(17) 1 d P . .
H1 H 1.0582 0.4159 0.2846 0.050 Uiso 1 1 d . . .
H2 H 0.8903 0.2623 0.1771 0.050 Uiso 0.67 1 d P . .
H3 H 1.0613 0.2282 0.1251 0.050 Uiso 1 1 d . . .
H4 H 1.1017 0.2381 0.4502 0.050 Uiso 1 1 d . . .
N1 N 0.7006(5) 0.1097(3) -0.0264(6) 0.171(6) Uani 1 1 d . . .
C1 C 0.6889(4) 0.1402(3) -0.0256(5) 0.095(3) Uani 1 1 d . . .
C2 C 0.6788(3) 0.1552(3) -0.1224(6) 0.080(2) Uani 1 1 d . . .
C3 C 0.6549(5) 0.1829(5) -0.1235(11) 0.090(4) Uani 0.647(13) 1 d P . .
C3A C 0.6974(9) 0.2044(9) -0.157(2) 0.090(4) Uani 0.353(13) 1 d P . .
C4 C 0.6786(4) 0.2317(4) -0.1076(13) 0.155(6) Uani 1 1 d . . .
C5 C 0.7075(6) 0.2531(4) -0.0114(15) 0.171(7) Uani 1 1 d . . .
C6 C 0.7471(6) 0.2425(7) 0.0101(16) 0.204(8) Uani 1 1 d . . .
C7 C 0.7323(8) 0.2068(6) 0.0740(12) 0.193(9) Uani 1 1 d . . .
C8 C 0.6945(4) 0.1659(3) 0.0664(6) 0.091(3) Uani 1 1 d . . .
N2 N 1.1153(2) 0.3876(2) 0.5392(4) 0.0673(16) Uani 1 1 d . . .
C9 C 1.1396(5) 0.4365(3) 0.5358(8) 0.140(6) Uani 1 1 d . . .
C10 C 1.1593(6) 0.4589(4) 0.6267(9) 0.176(7) Uani 1 1 d . . .
C11 C 1.1793(8) 0.5091(6) 0.6300(16) 0.319(19) Uani 1 1 d . . .
C12 C 1.2271(6) 0.5381(6) 0.6054(13) 0.202(9) Uani 1 1 d . . .
C13 C 1.2438(6) 0.5347(8) 0.510(3) 0.285(15) Uani 1 1 d . . .
C14 C 1.2281(10) 0.5117(15) 0.4282(16) 0.266(16) Uani 1 1 d . . .
C15 C 1.1859(13) 0.4678(15) 0.416(2) 0.35(3) Uani 1 1 d . . .
C16 C 1.1482(9) 0.4586(8) 0.4485(17) 0.30(2) Uani 1 1 d . . .
H1B H 0.7108 0.1049 0.0294 0.080 Uiso 1 1 d . . .
H1C H 0.6901 0.0884 -0.0674 0.080 Uiso 1 1 d . . .
H1D H 0.7345 0.1302 -0.0593 0.080 Uiso 1 1 d . . .
H1A H 0.6552 0.1142 -0.0116 0.080 Uiso 1 1 d . . .
H2A H 0.6455 0.1393 -0.1311 0.080 Uiso 1 1 d . . .
H2B H 0.6889 0.1414 -0.1707 0.080 Uiso 1 1 d . . .
H3A H 0.6304 0.1696 -0.0723 0.080 Uiso 0.65 1 d P . .
H3B H 0.6372 0.1761 -0.1841 0.080 Uiso 0.65 1 d P . .
H3AA H 0.6908 0.2080 -0.2266 0.080 Uiso 0.35 1 d P . .
H3AB H 0.7300 0.2244 -0.1518 0.080 Uiso 0.35 1 d P . .
H4A H 0.6604 0.2455 -0.1181 0.080 Uiso 1 1 d . . .
H4B H 0.7029 0.2462 -0.1602 0.080 Uiso 1 1 d . . .
H5A H 0.6861 0.2418 0.0455 0.080 Uiso 1 1 d . . .
H5B H 0.7193 0.2869 -0.0078 0.080 Uiso 1 1 d . . .
H6A H 0.7763 0.2698 0.0285 0.080 Uiso 1 1 d . . .
H6B H 0.7558 0.2335 -0.0545 0.080 Uiso 1 1 d . . .
H7A H 0.7330 0.2208 0.1385 0.080 Uiso 1 1 d . . .
H7B H 0.7585 0.2008 0.0832 0.080 Uiso 1 1 d . . .
H8A H 0.6903 0.1465 0.1215 0.080 Uiso 1 1 d . . .
H8B H 0.6680 0.1715 0.0720 0.080 Uiso 1 1 d . . .
H2C H 1.1042 0.3753 0.4799 0.080 Uiso 1 1 d . . .
H2D H 1.1342 0.3772 0.5596 0.080 Uiso 1 1 d . . .
H2E H 1.0923 0.3782 0.5821 0.080 Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O1 1.931(3) . ?
Zn1 O9 1.935(4) . ?
Zn1 O4 1.935(3) . ?
Zn1 O3 1.953(3) . ?
Zn2 O11 1.910(5) 16_755 ?
Zn2 O7 1.924(4) . ?
Zn2 O10 1.945(4) . ?
Zn2 O2 1.959(4) . ?
Zn3 O5 1.909(4) . ?
Zn3 O8 1.924(5) . ?
Zn3 O12 1.940(5) 6_664 ?
Zn3 O6 1.942(4) . ?
P1 O2 1.511(4) . ?
P1 O1 1.514(4) 6_665 ?
P1 O3 1.515(3) . ?
P1 H1 1.4258 . ?
P2 O13 1.49(2) . ?
P2 O6 1.502(4) . ?
P2 O5 1.502(4) 13_655 ?
P2 O4 1.517(4) . ?
P2 H2 1.4681 . ?
P3 O9 1.509(4) . ?
P3 O8 1.509(5) 11_665 ?
P3 O7 1.518(4) . ?
P3 H3 1.1445 . ?
P4 O11 1.499(4) . ?
P4 O12 1.499(4) . ?
P4 O10 1.505(5) . ?
P4 H4 1.3667 . ?
O1 P1 1.514(4) 8_644 ?
O5 P2 1.502(4) 13_655 ?
O8 P3 1.509(5) 12_545 ?
O11 Zn2 1.910(5) 16_755 ?
O12 Zn3 1.939(5) 8_645 ?
O13 H2 0.0459 . ?
N1 C1 1.280(10) . ?
N1 H1B 0.8831 . ?
N1 H1C 0.8403 . ?
N1 H1D 1.0985 . ?
C1 C8 1.488(10) . ?
C1 C2 1.515(11) . ?
C1 H1A 1.0548 . ?
C2 C3 1.519(16) . ?
C2 C3A 1.54(3) . ?
C2 H2A 0.9858 . ?
C2 H2B 0.9644 . ?
C3 C3A 1.33(3) . ?
C3 C4 1.450(18) . ?
C3 H2A 1.3538 . ?
C3 H3A 1.0038 . ?
C3 H3B 0.9799 . ?
C3A C4 1.52(3) . ?
C3A H3AA 0.9939 . ?
C3A H3AB 0.9683 . ?
C3A H4B 1.3325 . ?
C4 C5 1.58(2) . ?
C4 H4A 0.9552 . ?
C4 H4B 1.0156 . ?
C5 C6 1.58(2) . ?
C5 H5A 1.0003 . ?
C5 H5B 1.0099 . ?
C6 C7 1.37(2) . ?
C6 H6A 0.9924 . ?
C6 H6B 1.0232 . ?
C7 C8 1.343(19) . ?
C7 H7A 0.9959 . ?
C7 H7B 1.0153 . ?
C8 H8A 0.9614 . ?
C8 H8B 1.0105 . ?
N2 C9 1.439(11) . ?
N2 H2C 0.9035 . ?
N2 H2D 0.9153 . ?
N2 H2E 0.8969 . ?
C9 C16 1.36(2) . ?
C9 C10 1.434(14) . ?
C10 C11 1.49(2) . ?
C11 C12 1.46(2) . ?
C12 C13 1.45(3) . ?
C13 C14 1.31(3) . ?
C14 C15 1.47(4) . ?
C15 C16 1.24(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
O1 Zn1 O9 103.21(17) . . ?
O1 Zn1 O4 107.18(16) . . ?
O9 Zn1 O4 112.6(2) . . ?
O1 Zn1 O3 112.91(15) . . ?
O9 Zn1 O3 104.55(18) . . ?
O4 Zn1 O3 115.73(15) . . ?
O11 Zn2 O7 115.78(19) 16_755 . ?
O11 Zn2 O10 112.7(2) 16_755 . ?
O7 Zn2 O10 109.89(19) . . ?
O11 Zn2 O2 105.8(2) 16_755 . ?
O7 Zn2 O2 112.41(19) . . ?
O10 Zn2 O2 98.98(17) . . ?
O5 Zn3 O8 117.0(2) . . ?
O5 Zn3 O12 104.6(2) . 6_664 ?
O8 Zn3 O12 105.8(2) . 6_664 ?
O5 Zn3 O6 114.98(17) . . ?
O8 Zn3 O6 106.05(19) . . ?
O12 Zn3 O6 107.6(2) 6_664 . ?
O2 P1 O1 112.8(2) . 6_665 ?
O2 P1 O3 113.1(2) . . ?
O1 P1 O3 111.5(2) 6_665 . ?
O2 P1 H1 109.7 . . ?
O1 P1 H1 100.8 6_665 . ?
O3 P1 H1 108.1 . . ?
O13 P2 O6 114.0(9) . . ?
O13 P2 O5 101.2(8) . 13_655 ?
O6 P2 O5 113.1(2) . 13_655 ?
O13 P2 O4 107.5(11) . . ?
O6 P2 O4 111.3(2) . . ?
O5 P2 O4 109.2(2) 13_655 . ?
O13 P2 H2 1.6 . . ?
O6 P2 H2 113.3 . . ?
O5 P2 H2 102.8 13_655 . ?
O4 P2 H2 106.6 . . ?
O9 P3 O8 111.9(3) . 11_665 ?
O9 P3 O7 113.6(2) . . ?
O8 P3 O7 114.4(3) 11_665 . ?
O9 P3 H3 116.1 . . ?
O8 P3 H3 103.6 11_665 . ?
O7 P3 H3 95.9 . . ?
O11 P4 O12 113.2(3) . . ?
O11 P4 O10 113.9(3) . . ?
O12 P4 O10 111.6(3) . . ?
O11 P4 H4 100.8 . . ?
O12 P4 H4 103.4 . . ?
O10 P4 H4 113.0 . . ?
P1 O1 Zn1 133.5(2) 8_644 . ?
P1 O2 Zn2 128.4(2) . . ?
P1 O3 Zn1 128.9(2) . . ?
P2 O4 Zn1 133.5(2) . . ?
P2 O5 Zn3 146.9(3) 13_655 . ?
P2 O6 Zn3 129.0(2) . . ?
P3 O7 Zn2 133.0(3) . . ?
P3 O8 Zn3 134.6(3) 12_545 . ?
P3 O9 Zn1 130.1(2) . . ?
P4 O10 Zn2 132.8(3) . . ?
P4 O11 Zn2 132.6(3) . 16_755 ?
P4 O12 Zn3 130.3(3) . 8_645 ?
P2 O13 H2 60.1 . . ?
C1 N1 H1B 116.6 . . ?
C1 N1 H1C 122.0 . . ?
H1B N1 H1C 117.0 . . ?
C1 N1 H1D 98.0 . . ?
H1B N1 H1D 95.1 . . ?
H1C N1 H1D 97.7 . . ?
N1 C1 C8 118.7(8) . . ?
N1 C1 C2 118.6(7) . . ?
C8 C1 C2 121.6(7) . . ?
N1 C1 H1A 88.4 . . ?
C8 C1 H1A 95.9 . . ?
C2 C1 H1A 96.1 . . ?
C1 C2 C3 119.8(9) . . ?
C1 C2 C3A 126.7(12) . . ?
C3 C2 C3A 51.7(12) . . ?
C1 C2 H2A 108.1 . . ?
C3 C2 H2A 61.1 . . ?
C3A C2 H2A 107.1 . . ?
C1 C2 H2B 103.9 . . ?
C3 C2 H2B 136.2 . . ?
C3A C2 H2B 105.1 . . ?
H2A C2 H2B 103.8 . . ?
C3A C3 C4 66.1(15) . . ?
C3A C3 C2 64.9(14) . . ?
C4 C3 C2 122.7(11) . . ?
C3A C3 H2A 99.8 . . ?
C4 C3 H2A 162.2 . . ?
C2 C3 H2A 39.6 . . ?
C3A C3 H3A 156.1 . . ?
C4 C3 H3A 105.8 . . ?
C2 C3 H3A 107.0 . . ?
H2A C3 H3A 82.6 . . ?
C3A C3 H3B 101.8 . . ?
C4 C3 H3B 108.7 . . ?
C2 C3 H3B 108.4 . . ?
H2A C3 H3B 84.0 . . ?
H3A C3 H3B 102.2 . . ?
C3 C3A C4 60.7(14) . . ?
C3 C3A C2 63.4(15) . . ?
C4 C3A C2 117(2) . . ?
C3 C3A H3AA 98.4 . . ?
C4 C3A H3AA 99.3 . . ?
C2 C3A H3AA 115.7 . . ?
C3 C3A H3AB 154.3 . . ?
C4 C3A H3AB 102.7 . . ?
C2 C3A H3AB 116.0 . . ?
H3AA C3A H3AB 103.9 . . ?
C3 C3A H4B 97.5 . . ?
C4 C3A H4B 41.0 . . ?
C2 C3A H4B 157.9 . . ?
H3AA C3A H4B 76.3 . . ?
H3AB C3A H4B 75.9 . . ?
C3 C4 C3A 53.3(12) . . ?
C3 C4 C5 120.8(12) . . ?
C3A C4 C5 107.4(13) . . ?
C3 C4 H4A 114.2 . . ?
C3A C4 H4A 143.3 . . ?
C5 C4 H4A 107.8 . . ?
C3 C4 H4B 107.4 . . ?
C3A C4 H4B 59.5 . . ?
C5 C4 H4B 101.5 . . ?
H4A C4 H4B 103.0 . . ?
C4 C5 C6 116.9(12) . . ?
C4 C5 H5A 107.8 . . ?
C6 C5 H5A 107.7 . . ?
C4 C5 H5B 111.5 . . ?
C6 C5 H5B 110.4 . . ?
H5A C5 H5B 101.2 . . ?
C7 C6 C5 109.9(19) . . ?
C7 C6 H6A 114.7 . . ?
C5 C6 H6A 113.6 . . ?
C7 C6 H6B 108.7 . . ?
C5 C6 H6B 108.1 . . ?
H6A C6 H6B 101.3 . . ?
C8 C7 C6 127.2(19) . . ?
C8 C7 H7A 110.1 . . ?
C6 C7 H7A 103.5 . . ?
C8 C7 H7B 106.2 . . ?
C6 C7 H7B 106.6 . . ?
H7A C7 H7B 99.9 . . ?
C7 C8 C1 116.6(11) . . ?
C7 C8 H8A 112.8 . . ?
C1 C8 H8A 109.2 . . ?
C7 C8 H8B 106.2 . . ?
C1 C8 H8B 108.0 . . ?
H8A C8 H8B 103.1 . . ?
C9 N2 H2C 111.7 . . ?
C9 N2 H2D 110.4 . . ?
H2C N2 H2D 107.8 . . ?
C9 N2 H2E 109.1 . . ?
H2C N2 H2E 109.4 . . ?
H2D N2 H2E 108.4 . . ?
C16 C9 C10 123.5(13) . . ?
C16 C9 N2 120.4(14) . . ?
C10 C9 N2 115.4(9) . . ?
C9 C10 C11 117.2(16) . . ?
C12 C11 C10 118.9(19) . . ?
C13 C12 C11 120.2(15) . . ?
C14 C13 C12 138.9(19) . . ?
C13 C14 C15 127(2) . . ?
C16 C15 C14 125(3) . . ?
C15 C16 C9 112(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.195
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NTHU-11-iba
_database_code_depnum_ccdc_archive 'CCDC 848203'
_audit_update_record             
;
2011-10-11 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
#TrackingRef '7597_web_deposit_cif_file_3_Hsin-YauLin_1318347903.NTHU-11-iba.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         (NC4H12)2[Zn3(HPO3)3(HPO4)1]
_chemical_formula_sum            'C8 H28 N2 O13 P4 Zn3'
_chemical_formula_weight         680.38

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   32.8755(9)
_cell_length_b                   32.8755(9)
_cell_length_c                   13.2082(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12362.9(7)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9858
_cell_measurement_theta_min      1.70
_cell_measurement_theta_max      28.36

_exptl_crystal_description       Columnar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6048
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7587
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            54091
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         28.36
_reflns_number_total             6863
_reflns_number_gt                5200
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0633P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    const
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6863
_refine_ls_number_parameters     192
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.1071
_refine_ls_wR_factor_gt          0.1005
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

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 0.325049(11) -0.041200(11) 0.08309(2) 0.03513(10) Uani 1 1 d . . .
Zn2 Zn 0.329267(14) 0.104490(12) 0.19568(3) 0.04562(11) Uani 1 1 d . . .
Zn3 Zn 0.496446(13) -0.005249(16) -0.16637(3) 0.05117(13) Uani 1 1 d . . .
P1 P 0.37212(3) 0.04136(2) 0.23795(5) 0.03348(16) Uani 1 1 d . . .
P2 P 0.42579(3) -0.01220(3) 0.01083(5) 0.04116(18) Uani 1 1 d D . .
P3 P 0.26400(3) 0.07719(3) 0.38644(6) 0.04128(18) Uani 1 1 d . . .
P4 P 0.27606(3) 0.12873(3) 0.03551(6) 0.0478(2) Uani 1 1 d . . .
O1 O 0.35230(7) -0.00955(7) 0.20982(14) 0.0405(5) Uani 1 1 d . . .
O2 O 0.35915(9) 0.06747(8) 0.16308(15) 0.0508(6) Uani 1 1 d . . .
O3 O 0.35938(7) 0.04682(7) 0.34633(14) 0.0390(4) Uani 1 1 d . . .
O4 O 0.37320(7) -0.04162(8) 0.00229(16) 0.0496(5) Uani 1 1 d . . .
O5 O 0.44674(9) -0.02873(10) -0.06897(17) 0.0643(7) Uani 1 1 d . . .
O6 O 0.44168(8) -0.01382(11) 0.11685(16) 0.0714(8) Uani 1 1 d . . .
O7 O 0.27318(8) 0.07076(8) 0.27700(15) 0.0501(5) Uani 1 1 d . . .
O8 O 0.28384(9) 0.12779(8) 0.41735(18) 0.0597(6) Uani 1 1 d . . .
O9 O 0.27826(8) 0.05083(8) 0.45822(15) 0.0499(5) Uani 1 1 d . . .
O10 O 0.30703(11) 0.10881(10) 0.06102(17) 0.0730(8) Uani 1 1 d . . .
O11 O 0.27542(10) 0.13629(12) -0.07610(19) 0.0876(10) Uani 1 1 d . . .
O12 O 0.28564(10) 0.17022(9) 0.0982(2) 0.0811(9) Uani 1 1 d . . .
O13 O 0.4275(2) 0.0672(2) 0.2371(5) 0.044(2) Uani 0.323(6) 1 d P . .
O14 O 0.44212(19) 0.03882(18) -0.0099(3) 0.0995(19) Uani 0.686(6) 1 d P . .
H1 H 0.4216 0.0643 0.2351 0.050 Uiso 0.68 1 d P . .
H2 H 0.4414 0.0354 0.0078 0.050 Uiso 0.31 1 d PD . .
H3 H 0.2156 0.0580 0.3895 0.050 Uiso 1 1 d . . .
H4 H 0.2295 0.0946 0.0687 0.050 Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.915(2) . ?
Zn1 O1 1.9379(19) . ?
Zn1 O3 1.9400(19) 8_544 ?
Zn1 O9 1.952(2) 8_544 ?
Zn2 O12 1.898(3) 13 ?
Zn2 O7 1.934(2) . ?
Zn2 O10 1.955(2) . ?
Zn2 O2 1.956(2) . ?
Zn3 O5 1.913(2) . ?
Zn3 O6 1.919(2) 10_655 ?
Zn3 O11 1.922(3) 18_544 ?
Zn3 O8 1.954(2) 6_554 ?
P1 O2 1.504(2) . ?
P1 O1 1.5078(19) . ?
P1 O3 1.5269(19) . ?
P1 O13 1.578(6) . ?
P1 H1 1.4097 . ?
P2 O5 1.502(2) . ?
P2 O6 1.505(2) . ?
P2 O4 1.505(2) . ?
P2 O14 1.509(5) . ?
P2 H2 1.3834 . ?
P3 O8 1.508(2) . ?
P3 O9 1.509(2) . ?
P3 O7 1.513(2) . ?
P3 H3 1.3872 . ?
P4 O12 1.489(3) . ?
P4 O11 1.497(3) . ?
P4 O10 1.498(3) . ?
P4 H4 1.4414 . ?
O3 Zn1 1.9402(19) 6 ?
O6 Zn3 1.919(2) 10_655 ?
O8 Zn3 1.954(2) 8_545 ?
O9 Zn1 1.952(2) 6 ?
O11 Zn3 1.922(3) 17_554 ?
O12 Zn2 1.898(3) 13 ?
O13 H1 0.1711 . ?
O14 H2 0.2551 . ?

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 O1 108.87(9) . . ?
O4 Zn1 O3 114.94(9) . 8_544 ?
O1 Zn1 O3 115.65(8) . 8_544 ?
O4 Zn1 O9 107.11(10) . 8_544 ?
O1 Zn1 O9 103.17(8) . 8_544 ?
O3 Zn1 O9 106.03(9) 8_544 8_544 ?
O12 Zn2 O7 122.92(11) 13 . ?
O12 Zn2 O10 110.74(14) 13 . ?
O7 Zn2 O10 105.25(11) . . ?
O12 Zn2 O2 102.59(11) 13 . ?
O7 Zn2 O2 113.39(9) . . ?
O10 Zn2 O2 99.64(9) . . ?
O5 Zn3 O6 117.04(10) . 10_655 ?
O5 Zn3 O11 99.99(12) . 18_544 ?
O6 Zn3 O11 113.41(14) 10_655 18_544 ?
O5 Zn3 O8 120.72(10) . 6_554 ?
O6 Zn3 O8 99.48(11) 10_655 6_554 ?
O11 Zn3 O8 106.32(11) 18_544 6_554 ?
O2 P1 O1 112.52(12) . . ?
O2 P1 O3 112.14(12) . . ?
O1 P1 O3 111.69(11) . . ?
O2 P1 O13 105.6(3) . . ?
O1 P1 O13 109.7(2) . . ?
O3 P1 O13 104.7(3) . . ?
O2 P1 H1 104.9 . . ?
O1 P1 H1 109.3 . . ?
O3 P1 H1 105.8 . . ?
O13 P1 H1 1.1 . . ?
O5 P2 O6 114.22(14) . . ?
O5 P2 O4 107.58(14) . . ?
O6 P2 O4 110.76(13) . . ?
O5 P2 O14 107.6(2) . . ?
O6 P2 O14 105.8(2) . . ?
O4 P2 O14 110.9(2) . . ?
O5 P2 H2 114.3 . . ?
O6 P2 H2 97.4 . . ?
O4 P2 H2 112.5 . . ?
O14 P2 H2 8.8 . . ?
O8 P3 O9 112.09(13) . . ?
O8 P3 O7 113.97(13) . . ?
O9 P3 O7 112.27(12) . . ?
O8 P3 H3 105.0 . . ?
O9 P3 H3 109.6 . . ?
O7 P3 H3 103.1 . . ?
O12 P4 O11 114.19(19) . . ?
O12 P4 O10 113.38(17) . . ?
O11 P4 O10 111.29(16) . . ?
O12 P4 H4 101.6 . . ?
O11 P4 H4 109.3 . . ?
O10 P4 H4 106.3 . . ?
P1 O1 Zn1 129.50(12) . . ?
P1 O2 Zn2 125.74(12) . . ?
P1 O3 Zn1 127.87(11) . 6 ?
P2 O4 Zn1 129.92(13) . . ?
P2 O5 Zn3 141.23(18) . . ?
P2 O6 Zn3 129.45(14) . 10_655 ?
P3 O7 Zn2 130.56(14) . . ?
P3 O8 Zn3 130.37(15) . 8_545 ?
P3 O9 Zn1 124.64(12) . 6 ?
P4 O10 Zn2 126.64(15) . . ?
P4 O11 Zn3 127.76(17) . 17_554 ?
P4 O12 Zn2 139.01(18) . 13 ?
P1 O13 H1 9.4 . . ?
P2 O14 H2 56.3 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.095

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.005 2266 544 ' '
2 0.333 0.667 0.288 2269 544 ' '
3 0.667 0.333 0.955 2269 544 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NTHU-11-pa
_database_code_depnum_ccdc_archive 'CCDC 848204'
_audit_update_record             
;
2011-10-11 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
#TrackingRef '7598_web_deposit_cif_file_4_Hsin-YauLin_1318347903.NTHU-11-pa.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         (NC5H14)2[Zn3(HPO3)3.5(HPO4)0.5]
_chemical_formula_sum            'C10 H18 N2 O12.5 P4 Zn3'
_chemical_formula_weight         686.32

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   33.1915(4)
_cell_length_b                   33.1915(4)
_cell_length_c                   13.3206(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12708.9(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9812
_cell_measurement_theta_min      1.68
_cell_measurement_theta_max      28.29

_exptl_crystal_description       Columnar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6084
_exptl_absorpt_coefficient_mu    2.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            56018
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         28.29
_reflns_number_total             7023
_reflns_number_gt                5494
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0690P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    const
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7023
_refine_ls_number_parameters     192
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.1045
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.299116(10) 0.008586(9) 0.909469(19) 0.04023(9) Uani 1 1 d . . .
Zn2 Zn 0.443504(12) 0.004768(14) 1.02748(2) 0.05856(12) Uani 1 1 d . . .
Zn3 Zn 0.164824(12) -0.164015(11) 0.66855(2) 0.05942(12) Uani 1 1 d . . .
P1 P 0.33840(2) -0.03546(2) 1.06240(4) 0.04224(15) Uani 1 1 d . . .
P2 P 0.22916(2) -0.09293(2) 0.84351(5) 0.04688(17) Uani 1 1 d . . .
P3 P 0.48074(2) 0.06899(3) 1.21944(5) 0.05183(17) Uani 1 1 d . . .
P4 P 0.52155(3) 0.05698(3) 0.86760(5) 0.0594(2) Uani 1 1 d . . .
O1 O 0.30722(6) -0.01643(6) 1.03397(12) 0.0468(4) Uani 1 1 d . . .
O2 O 0.37775(7) -0.02134(9) 0.98953(14) 0.0708(6) Uani 1 1 d . . .
O3 O 0.35537(6) -0.02377(6) 1.17061(12) 0.0466(4) Uani 1 1 d . . .
O4 O 0.25026(6) -0.04077(6) 0.83309(13) 0.0514(4) Uani 1 1 d . . .
O5 O 0.19108(7) -0.11587(7) 0.76747(15) 0.0713(6) Uani 1 1 d . . .
O6 O 0.21334(8) -0.10879(7) 0.95007(13) 0.0753(7) Uani 1 1 d . . .
O7 O 0.46698(7) 0.05930(7) 1.10986(13) 0.0620(5) Uani 1 1 d . . .
O8 O 0.51088(7) 0.04947(9) 1.25457(16) 0.0714(6) Uani 1 1 d . . .
O9 O 0.43943(7) 0.05510(8) 1.28790(13) 0.0591(5) Uani 1 1 d . . .
O10 O 0.47146(8) 0.02592(10) 0.89545(15) 0.0837(8) Uani 1 1 d . . .
O11 O 0.52940(9) 0.05716(9) 0.75663(16) 0.0920(8) Uani 1 1 d . . .
O12 O 0.55447(8) 0.04874(9) 0.9284(2) 0.0839(7) Uani 1 1 d . . .
O13 O 0.3095(5) -0.0873(5) 1.0601(13) 0.055(6) Uani 0.117(5) 1 d P . .
O14 O 0.2663(2) -0.1068(2) 0.8197(4) 0.0604(19) Uani 0.365(5) 1 d P . .
H1 H 0.3099 -0.0893 1.0594 0.050 Uiso 0.88 1 d P . .
H2 H 0.2652 -0.1078 0.8199 0.050 Uiso 0.63 1 d P . .
H3 H 0.5043 0.1109 1.2274 0.050 Uiso 1 1 d . . .
H4 H 0.5313 0.0993 0.8812 0.050 Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.9215(16) . ?
Zn1 O1 1.9327(17) . ?
Zn1 O3 1.9436(16) 8_544 ?
Zn1 O9 1.9490(19) 8_544 ?
Zn2 O12 1.903(3) 10_657 ?
Zn2 O7 1.918(2) . ?
Zn2 O10 1.948(2) . ?
Zn2 O2 1.969(2) . ?
Zn3 O5 1.9122(18) . ?
Zn3 O6 1.9157(19) 16_546 ?
Zn3 O8 1.939(2) 6_554 ?
Zn3 O11 1.947(3) 15_446 ?
P1 O13 1.493(15) . ?
P1 O2 1.502(2) . ?
P1 O1 1.5057(17) . ?
P1 O3 1.5255(16) . ?
P1 H1 1.5491 . ?
P2 O5 1.497(2) . ?
P2 O6 1.5138(18) . ?
P2 O4 1.5146(18) . ?
P2 O14 1.548(6) . ?
P2 H2 1.5375 . ?
P3 O8 1.512(2) . ?
P3 O9 1.514(2) . ?
P3 O7 1.5152(19) . ?
P3 H3 1.2125 . ?
P4 O12 1.491(2) . ?
P4 O10 1.500(2) . ?
P4 O11 1.501(2) . ?
P4 H4 1.2868 . ?
O3 Zn1 1.9436(16) 6 ?
O6 Zn3 1.9158(19) 16_546 ?
O8 Zn3 1.939(2) 8_545 ?
O9 Zn1 1.9491(19) 6 ?
O11 Zn3 1.947(3) 14_556 ?
O12 Zn2 1.903(3) 10_657 ?
O13 H1 0.0740 . ?
O14 H2 0.0346 . ?

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 O1 109.11(7) . . ?
O4 Zn1 O3 115.16(7) . 8_544 ?
O1 Zn1 O3 113.04(7) . 8_544 ?
O4 Zn1 O9 109.01(9) . 8_544 ?
O1 Zn1 O9 102.82(7) . 8_544 ?
O3 Zn1 O9 106.88(8) 8_544 8_544 ?
O12 Zn2 O7 121.13(9) 10_657 . ?
O12 Zn2 O10 112.46(12) 10_657 . ?
O7 Zn2 O10 106.32(10) . . ?
O12 Zn2 O2 102.53(11) 10_657 . ?
O7 Zn2 O2 113.59(9) . . ?
O10 Zn2 O2 98.64(8) . . ?
O5 Zn3 O6 115.89(8) . 16_546 ?
O5 Zn3 O8 119.76(9) . 6_554 ?
O6 Zn3 O8 101.94(9) 16_546 6_554 ?
O5 Zn3 O11 99.94(10) . 15_446 ?
O6 Zn3 O11 113.55(12) 16_546 15_446 ?
O8 Zn3 O11 105.80(10) 6_554 15_446 ?
O13 P1 O2 107.6(7) . . ?
O13 P1 O1 107.4(5) . . ?
O2 P1 O1 112.31(11) . . ?
O13 P1 O3 104.8(6) . . ?
O2 P1 O3 112.23(11) . . ?
O1 P1 O3 112.01(10) . . ?
O13 P1 H1 1.8 . . ?
O2 P1 H1 106.1 . . ?
O1 P1 H1 109.0 . . ?
O3 P1 H1 104.6 . . ?
O5 P2 O6 113.55(12) . . ?
O5 P2 O4 108.04(12) . . ?
O6 P2 O4 111.43(11) . . ?
O5 P2 O14 107.8(2) . . ?
O6 P2 O14 106.1(2) . . ?
O4 P2 O14 109.8(2) . . ?
O5 P2 H2 107.0 . . ?
O6 P2 H2 105.7 . . ?
O4 P2 H2 111.0 . . ?
O14 P2 H2 1.2 . . ?
O8 P3 O9 112.06(12) . . ?
O8 P3 O7 113.65(13) . . ?
O9 P3 O7 112.62(11) . . ?
O8 P3 H3 106.2 . . ?
O9 P3 H3 105.2 . . ?
O7 P3 H3 106.3 . . ?
O12 P4 O10 113.66(15) . . ?
O12 P4 O11 113.23(16) . . ?
O10 P4 O11 112.14(14) . . ?
O12 P4 H4 108.4 . . ?
O10 P4 H4 107.6 . . ?
O11 P4 H4 100.7 . . ?
P1 O1 Zn1 131.95(11) . . ?
P1 O2 Zn2 124.82(11) . . ?
P1 O3 Zn1 128.50(10) . 6 ?
P2 O4 Zn1 129.55(11) . . ?
P2 O5 Zn3 143.85(17) . . ?
P2 O6 Zn3 129.09(11) . 16_546 ?
P3 O7 Zn2 133.52(13) . . ?
P3 O8 Zn3 132.06(13) . 8_545 ?
P3 O9 Zn1 125.01(11) . 6 ?
P4 O10 Zn2 129.45(13) . . ?
P4 O11 Zn3 127.97(16) . 14_556 ?
P4 O12 Zn2 135.21(16) . 10_657 ?
P1 O13 H1 137.7 . . ?
P2 O14 H2 71.6 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.091

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.006 2432 495 ' '
2 0.333 0.667 0.787 2436 495 ' '
3 0.667 0.333 0.454 2436 495 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NTHU-11-ha
_database_code_depnum_ccdc_archive 'CCDC 848205'
_audit_update_record             
;
2011-10-11 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
#TrackingRef '7599_web_deposit_cif_file_5_Hsin-YauLin_1318347903.NTHU-11-ha.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         (NC6H16)2[Zn3(HPO3)3.7(HPO4)0.3]
_chemical_formula_sum            'C12 H36 N2 O12.3 P4 Zn3'
_chemical_formula_weight         725.29

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   33.2781(9)
_cell_length_b                   33.2781(9)
_cell_length_c                   13.5625(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13007.3(7)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9871
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      28.32

_exptl_crystal_description       Columnar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6624
_exptl_absorpt_coefficient_mu    2.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56676
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         28.32
_reflns_number_total             7189
_reflns_number_gt                5619
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0539P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    const
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7189
_refine_ls_number_parameters     192
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0850
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.002

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 0.340722(8) -0.034371(8) 0.754197(15) 0.03892(8) Uani 1 1 d . . .
Zn2 Zn 0.336855(12) 0.110466(10) 0.630373(17) 0.05644(10) Uani 1 1 d . . .
Zn3 Zn 0.170049(9) -0.168217(9) 0.997760(16) 0.05229(9) Uani 1 1 d . . .
P1 P 0.29793(2) 0.00495(2) 0.59915(3) 0.04154(13) Uani 1 1 d . . .
P2 P 0.239833(19) -0.105642(19) 0.82648(3) 0.04169(13) Uani 1 1 d . . .
P3 P 0.40202(2) 0.14648(2) 0.44576(4) 0.04979(15) Uani 1 1 d . . .
P4 P 0.38829(3) 0.18419(2) 0.80105(4) 0.05606(17) Uani 1 1 d . . .
O1 O 0.31473(5) -0.02739(5) 0.63204(10) 0.0484(4) Uani 1 1 d . . .
O2 O 0.31334(8) 0.04548(6) 0.66704(11) 0.0723(6) Uani 1 1 d . . .
O3 O 0.30913(5) 0.01878(5) 0.49160(9) 0.0461(3) Uani 1 1 d . . .
O4 O 0.29180(5) -0.08138(5) 0.83350(11) 0.0557(4) Uani 1 1 d . . .
O5 O 0.22033(6) -0.14141(6) 0.90693(11) 0.0652(5) Uani 1 1 d . . .
O6 O 0.22363(6) -0.12443(7) 0.72472(11) 0.0742(6) Uani 1 1 d . . .
O7 O 0.39299(6) 0.13362(6) 0.55454(11) 0.0623(4) Uani 1 1 d . . .
O8 O 0.38206(7) 0.17575(6) 0.41056(12) 0.0651(5) Uani 1 1 d . . .
O9 O 0.38819(7) 0.10488(6) 0.38063(11) 0.0633(5) Uani 1 1 d . . .
O10 O 0.35499(9) 0.13699(7) 0.76144(11) 0.0822(6) Uani 1 1 d . . .
O11 O 0.38223(7) 0.22167(7) 0.75592(16) 0.0798(6) Uani 1 1 d . . .
O12 O 0.38872(7) 0.18485(8) 0.91126(12) 0.0800(6) Uani 1 1 d . . .
O13 O 0.2498(17) -0.0137(18) 0.606(4) 0.05(2) Uani 0.030(5) 1 d P . .
O14 O 0.2239(3) -0.0712(3) 0.8476(6) 0.102(4) Uani 0.288(6) 1 d P . .
H1 H 0.2461 -0.0254 0.6033 0.050 Uiso 0.97 1 d P . .
H2 H 0.2250 -0.0710 0.8459 0.050 Uiso 0.71 1 d P . .
H3 H 0.4455 0.1686 0.4361 0.050 Uiso 1 1 d . . .
H4 H 0.4346 0.1977 0.7778 0.050 Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.9255(14) . ?
Zn1 O9 1.9343(16) 6 ?
Zn1 O1 1.9359(13) . ?
Zn1 O3 1.9530(14) 6 ?
Zn2 O11 1.905(2) 13_556 ?
Zn2 O7 1.9239(18) . ?
Zn2 O10 1.9418(16) . ?
Zn2 O2 1.9606(16) . ?
Zn3 O5 1.9028(15) . ?
Zn3 O6 1.9287(16) 16_546 ?
Zn3 O12 1.9385(19) 11_557 ?
Zn3 O8 1.9444(18) 8_545 ?
P1 O13 1.40(5) . ?
P1 O2 1.4963(17) . ?
P1 O1 1.5072(15) . ?
P1 O3 1.5187(13) . ?
P1 H1 1.5017 . ?
P2 O6 1.4997(15) . ?
P2 O5 1.5021(16) . ?
P2 O4 1.5018(16) . ?
P2 O14 1.509(9) . ?
P2 H2 1.4856 . ?
P3 O8 1.5051(18) . ?
P3 O9 1.5072(17) . ?
P3 O7 1.5236(16) . ?
P3 H3 1.2599 . ?
P4 O11 1.4907(19) . ?
P4 O12 1.4948(17) . ?
P4 O10 1.498(2) . ?
P4 H4 1.4085 . ?
O3 Zn1 1.9530(14) 8_544 ?
O6 Zn3 1.9288(16) 16_546 ?
O8 Zn3 1.9446(18) 6_554 ?
O9 Zn1 1.9347(16) 8_544 ?
O11 Zn2 1.905(2) 13_556 ?
O12 Zn3 1.9385(19) 12_557 ?
O13 H1 0.3488 . ?
O14 H2 0.0407 . ?

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 O9 110.02(8) . 6 ?
O4 Zn1 O1 109.18(6) . . ?
O9 Zn1 O1 104.55(6) 6 . ?
O4 Zn1 O3 112.39(6) . 6 ?
O9 Zn1 O3 107.74(7) 6 6 ?
O1 Zn1 O3 112.65(6) . 6 ?
O11 Zn2 O7 120.39(8) 13_556 . ?
O11 Zn2 O10 114.54(10) 13_556 . ?
O7 Zn2 O10 106.76(9) . . ?
O11 Zn2 O2 104.72(9) 13_556 . ?
O7 Zn2 O2 110.45(8) . . ?
O10 Zn2 O2 97.53(7) . . ?
O5 Zn3 O6 115.97(7) . 16_546 ?
O5 Zn3 O12 105.42(8) . 11_557 ?
O6 Zn3 O12 108.31(9) 16_546 11_557 ?
O5 Zn3 O8 118.42(7) . 8_545 ?
O6 Zn3 O8 101.44(8) 16_546 8_545 ?
O12 Zn3 O8 106.72(8) 11_557 8_545 ?
O13 P1 O2 99(2) . . ?
O13 P1 O1 114(2) . . ?
O2 P1 O1 112.29(9) . . ?
O13 P1 O3 105(2) . . ?
O2 P1 O3 113.35(9) . . ?
O1 P1 O3 112.22(8) . . ?
O13 P1 H1 13.2 . . ?
O2 P1 H1 110.1 . . ?
O1 P1 H1 102.7 . . ?
O3 P1 H1 105.4 . . ?
O6 P2 O5 114.54(11) . . ?
O6 P2 O4 111.09(9) . . ?
O5 P2 O4 107.76(10) . . ?
O6 P2 O14 107.5(3) . . ?
O5 P2 O14 106.7(3) . . ?
O4 P2 O14 109.0(4) . . ?
O6 P2 H2 107.3 . . ?
O5 P2 H2 107.9 . . ?
O4 P2 H2 108.1 . . ?
O14 P2 H2 1.3 . . ?
O8 P3 O9 112.19(10) . . ?
O8 P3 O7 113.57(10) . . ?
O9 P3 O7 112.51(10) . . ?
O8 P3 H3 109.8 . . ?
O9 P3 H3 102.1 . . ?
O7 P3 H3 105.8 . . ?
O11 P4 O12 113.73(13) . . ?
O11 P4 O10 113.05(12) . . ?
O12 P4 O10 111.76(11) . . ?
O11 P4 H4 103.0 . . ?
O12 P4 H4 102.6 . . ?
O10 P4 H4 111.9 . . ?
P1 O1 Zn1 133.35(9) . . ?
P1 O2 Zn2 127.31(9) . . ?
P1 O3 Zn1 129.50(9) . 8_544 ?
P2 O4 Zn1 132.84(9) . . ?
P2 O5 Zn3 140.53(13) . . ?
P2 O6 Zn3 133.24(10) . 16_546 ?
P3 O7 Zn2 130.23(11) . . ?
P3 O8 Zn3 133.88(11) . 6_554 ?
P3 O9 Zn1 127.73(9) . 8_544 ?
P4 O10 Zn2 134.74(12) . . ?
P4 O11 Zn2 132.89(13) . 13_556 ?
P4 O12 Zn3 129.20(12) . 12_557 ?
P1 O13 H1 99.8 . . ?
P2 O14 H2 53.4 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.082

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.005 2504 555 ' '
2 0.333 0.667 0.795 2508 555 ' '
3 0.667 0.333 0.462 2508 555 ' '
_platon_squeeze_details          
;
;


