# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_CCDC(1495889)
_database_code_depnum_ccdc_archive 'CCDC 1495889'
_audit_update_record             
;
2017-07-13 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Zinc diphosphonate ethelenediamine'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H18 N2 O15 P4 S0 Zn3'
_chemical_formula_weight         678.21

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   20.4135(8)
_cell_length_b                   8.9845(4)
_cell_length_c                   23.0411(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.499(3)
_cell_angle_gamma                90.00
_cell_volume                     4221.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3625
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      25.00

_exptl_crystal_description       'Block like'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2704
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5847
_exptl_absorpt_correction_T_max  0.7051
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8935
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3625
_reflns_number_gt                3029
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)'
_computing_publication_material  'PLATON (Spek, 2003)'

_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 > 2σ(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)+(0.0731P)²+151.0645P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3625
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.1805
_refine_ls_wR_factor_gt          0.1702
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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 0.60205(4) 0.47966(11) 0.03414(4) 0.0152(3) Uani 1 1 d . . .
Zn2 Zn 0.77694(5) 0.29030(12) 0.16755(4) 0.0192(3) Uani 1 1 d . . .
Zn3 Zn 0.84429(6) 0.76727(17) 0.12715(5) 0.0383(4) Uani 1 1 d . . .
P1 P 0.52630(10) 0.6320(3) -0.07565(9) 0.0159(5) Uani 1 1 d . . .
P2 P 0.63203(11) 0.4022(3) -0.09132(10) 0.0224(5) Uani 1 1 d . . .
P3 P 0.72135(10) 0.5631(3) 0.10848(9) 0.0143(5) Uani 1 1 d . . .
P4 P 0.78645(10) 0.6074(3) 0.22883(9) 0.0165(5) Uani 1 1 d . . .
O1 O 0.6626(3) 0.6200(7) 0.0712(2) 0.0153(12) Uani 1 1 d . . .
O2 O 0.6358(3) 0.3585(8) -0.0274(3) 0.0253(15) Uani 1 1 d . . .
O4 O 0.5485(3) 0.6255(7) -0.0114(2) 0.0160(12) Uani 1 1 d . . .
O5 O 0.7719(3) 0.6458(7) 0.2913(2) 0.0214(14) Uani 1 1 d . . .
O6 O 0.6455(3) 0.2647(10) -0.1283(3) 0.042(2) Uani 1 1 d . . .
O7 O 0.7183(3) 0.3959(7) 0.1119(2) 0.0175(13) Uani 1 1 d . . .
O8 O 0.8020(3) 0.4409(8) 0.2259(3) 0.0231(14) Uani 1 1 d . . .
O9 O 0.6755(3) 0.5338(10) -0.1025(3) 0.039(2) Uani 1 1 d . . .
O10 O 0.8403(3) 0.7063(8) 0.2077(3) 0.0260(15) Uani 1 1 d . . .
O11 O 0.7850(3) 0.6224(7) 0.0857(2) 0.0194(13) Uani 1 1 d . . .
O12 O 0.5619(3) 0.7555(8) -0.1077(3) 0.0315(16) Uani 1 1 d . . .
O13 O 0.7072(3) 0.7990(7) 0.1691(3) 0.0210(13) Uani 1 1 d . . .
H13 H 0.7024 0.8437 0.1997 0.031 Uiso 1 1 calc R . .
O14 O 0.5038(3) 0.3390(8) -0.0936(3) 0.0259(15) Uani 1 1 d . . .
C3 C 0.7126(4) 0.6430(10) 0.1804(3) 0.0148(17) Uani 1 1 d . . .
C4 C 0.6506(4) 0.5829(13) 0.2084(4) 0.029(2) Uani 1 1 d . . .
H4A H 0.6556 0.4781 0.2155 0.043 Uiso 1 1 calc R . .
H4B H 0.6132 0.5995 0.1826 0.043 Uiso 1 1 calc R . .
H4C H 0.6446 0.6335 0.2444 0.043 Uiso 1 1 calc R . .
C5 C 0.6681(8) 0.0280(17) 0.0568(9) 0.074(5) Uani 1 1 d . . .
H5A H 0.6717 0.1191 0.0346 0.089 Uiso 1 1 calc R . .
H5B H 0.6852 0.0423 0.0964 0.089 Uiso 1 1 calc R . .
C6 C 0.6016(16) -0.037(4) 0.0535(19) 0.24(3) Uani 1 1 d . . .
H6A H 0.5999 -0.1229 0.0281 0.286 Uiso 1 1 calc R . .
H6B H 0.5697 0.0358 0.0390 0.286 Uiso 1 1 calc R . .
N1 N 0.6946(19) -0.0968(19) 0.0295(8) 0.24(2) Uani 1 1 d . . .
H1A H 0.7375 -0.0840 0.0264 0.362 Uiso 1 1 calc R . .
H1B H 0.6756 -0.1074 -0.0058 0.362 Uiso 1 1 calc R . .
H1C H 0.6875 -0.1778 0.0505 0.362 Uiso 1 1 calc R . .
N2 N 0.5887(7) -0.080(2) 0.1142(7) 0.107(7) Uani 1 1 d . . .
H2A H 0.5489 -0.1200 0.1154 0.160 Uiso 1 1 calc R . .
H2B H 0.5911 -0.0001 0.1369 0.160 Uiso 1 1 calc R . .
H2C H 0.6185 -0.1465 0.1267 0.160 Uiso 1 1 calc R . .
O100 O 0.5856(7) 0.1592(16) 0.1690(8) 0.140(8) Uani 1 1 d . . .
C1 C 0.5471(4) 0.4576(10) -0.1111(4) 0.0185(18) Uani 1 1 d . . .
C2 C 0.5373(4) 0.4686(13) -0.1764(4) 0.028(2) Uani 1 1 d . . .
H2D H 0.5649 0.5458 -0.1906 0.042 Uiso 1 1 calc R . .
H2E H 0.4923 0.4917 -0.1863 0.042 Uiso 1 1 calc R . .
H2F H 0.5486 0.3754 -0.1937 0.042 Uiso 1 1 calc R . .
O3 O 0.4514(3) 0.6477(7) -0.0822(2) 0.0206(13) Uani 1 1 d . . .
H14 H 0.500(5) 0.327(11) -0.056(5) 0.02(3) Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.937(5) . ?
Zn1 O2 1.939(6) . ?
Zn1 O3 1.957(6) 5_665 ?
Zn1 O4 1.978(6) . ?
Zn2 O5 1.914(6) 4_645 ?
Zn2 O6 1.922(7) 7_655 ?
Zn2 O8 1.959(6) . ?
Zn2 O7 1.960(6) . ?
Zn3 O9 1.914(9) 7_665 ?
Zn3 O10 1.939(6) . ?
Zn3 O11 1.993(6) . ?
Zn3 O12 1.995(7) 7_665 ?
P1 O4 1.531(6) . ?
P1 O12 1.534(7) . ?
P1 O3 1.536(6) . ?
P1 C1 1.826(9) . ?
P2 O9 1.507(8) . ?
P2 O2 1.522(6) . ?
P2 O6 1.532(8) . ?
P2 C1 1.841(9) . ?
P3 O7 1.506(6) . ?
P3 O11 1.520(6) . ?
P3 O1 1.533(5) . ?
P3 C3 1.823(8) . ?
P4 O10 1.510(7) . ?
P4 O5 1.521(6) . ?
P4 O8 1.532(7) . ?
P4 C3 1.863(8) . ?
O5 Zn2 1.914(6) 4_655 ?
O6 Zn2 1.922(7) 7_655 ?
O9 Zn3 1.914(9) 7_665 ?
O12 Zn3 1.995(7) 7_665 ?
O13 C3 1.430(11) . ?
O14 C1 1.452(11) . ?
C3 C4 1.542(11) . ?
C5 N1 1.41(3) . ?
C5 C6 1.48(4) . ?
C6 N2 1.49(5) . ?
C1 C2 1.513(12) . ?
O3 Zn1 1.957(6) 5_665 ?

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 O2 116.6(3) . . ?
O1 Zn1 O3 119.5(2) . 5_665 ?
O2 Zn1 O3 108.1(3) . 5_665 ?
O1 Zn1 O4 97.4(2) . . ?
O2 Zn1 O4 101.0(2) . . ?
O3 Zn1 O4 112.2(2) 5_665 . ?
O5 Zn2 O6 121.1(3) 4_645 7_655 ?
O5 Zn2 O8 104.8(3) 4_645 . ?
O6 Zn2 O8 107.7(3) 7_655 . ?
O5 Zn2 O7 109.6(3) 4_645 . ?
O6 Zn2 O7 108.0(3) 7_655 . ?
O8 Zn2 O7 104.4(3) . . ?
O9 Zn3 O10 122.0(3) 7_665 . ?
O9 Zn3 O11 110.6(3) 7_665 . ?
O10 Zn3 O11 103.0(3) . . ?
O9 Zn3 O12 102.8(3) 7_665 7_665 ?
O10 Zn3 O12 105.5(3) . 7_665 ?
O11 Zn3 O12 113.2(3) . 7_665 ?
O4 P1 O12 111.5(4) . . ?
O4 P1 O3 110.5(3) . . ?
O12 P1 O3 112.2(4) . . ?
O4 P1 C1 109.6(4) . . ?
O12 P1 C1 106.3(4) . . ?
O3 P1 C1 106.6(4) . . ?
O9 P2 O2 111.2(4) . . ?
O9 P2 O6 114.6(5) . . ?
O2 P2 O6 109.1(4) . . ?
O9 P2 C1 107.5(4) . . ?
O2 P2 C1 108.4(4) . . ?
O6 P2 C1 105.7(4) . . ?
O7 P3 O11 114.0(4) . . ?
O7 P3 O1 109.2(3) . . ?
O11 P3 O1 110.4(3) . . ?
O7 P3 C3 109.8(4) . . ?
O11 P3 C3 107.2(3) . . ?
O1 P3 C3 105.8(4) . . ?
O10 P4 O5 110.3(4) . . ?
O10 P4 O8 113.9(4) . . ?
O5 P4 O8 108.2(4) . . ?
O10 P4 C3 106.7(4) . . ?
O5 P4 C3 110.0(4) . . ?
O8 P4 C3 107.7(4) . . ?
P3 O1 Zn1 119.9(4) . . ?
P2 O2 Zn1 123.9(4) . . ?
P1 O4 Zn1 132.2(4) . . ?
P4 O5 Zn2 138.6(4) . 4_655 ?
P2 O6 Zn2 129.8(5) . 7_655 ?
P3 O7 Zn2 119.4(3) . . ?
P4 O8 Zn2 131.1(4) . . ?
P2 O9 Zn3 131.7(4) . 7_665 ?
P4 O10 Zn3 122.5(3) . . ?
P3 O11 Zn3 125.0(3) . . ?
P1 O12 Zn3 120.9(4) . 7_665 ?
O13 C3 C4 111.2(7) . . ?
O13 C3 P3 103.3(5) . . ?
C4 C3 P3 110.9(6) . . ?
O13 C3 P4 109.4(5) . . ?
C4 C3 P4 110.3(6) . . ?
P3 C3 P4 111.6(4) . . ?
N1 C5 C6 91.9(19) . . ?
C5 C6 N2 104.7(17) . . ?
O14 C1 C2 105.5(7) . . ?
O14 C1 P1 110.5(5) . . ?
C2 C1 P1 111.4(7) . . ?
O14 C1 P2 108.1(6) . . ?
C2 C1 P2 110.2(6) . . ?
P1 C1 P2 110.9(5) . . ?
P1 O3 Zn1 117.9(3) . 5_665 ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         4.745
_refine_diff_density_min         -2.250
_refine_diff_density_rms         0.210

#####END#####
####################################################################### 
# 
# 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_CCDC(1495893)
_database_code_depnum_ccdc_archive 'CCDC 1495893'
_audit_update_record             
;
2017-07-13 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Zinc diphosphonate 1,3-diaminopropane'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H20 N2 O14 P4 Zn3'
_chemical_formula_weight         676.24

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

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

_cell_length_a                   18.1170(4)
_cell_length_b                   9.8448(3)
_cell_length_c                   10.7798(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1922.67(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1891
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      26.00

_exptl_crystal_description       'Block like'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1352
_exptl_absorpt_coefficient_mu    4.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_T_max  0.6376
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_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 SMART CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8219
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1891
_reflns_number_gt                1612
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.0627P)²+1.6341P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1891
_refine_ls_number_parameters     141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0768
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.68853(2) 0.00713(4) 0.32315(4) 0.01467(17) Uani 1 1 d . . .
Zn2 Zn 0.5000 -0.25265(6) 0.7500 0.01535(19) Uani 1 2 d S . .
P1 P 0.61590(5) -0.11989(10) 0.57815(9) 0.0128(2) Uani 1 1 d . . .
O2 O 0.62738(15) -0.0870(3) 0.4423(2) 0.0210(6) Uani 1 1 d . . .
O6 O 0.53538(13) -0.1612(3) 0.6001(3) 0.0198(6) Uani 1 1 d . . .
O7 O 0.75006(16) -0.2293(3) 0.5975(3) 0.0257(7) Uani 1 1 d . . .
C1 C 0.6734(2) -0.2678(4) 0.6169(4) 0.0148(8) Uani 1 1 d . . .
C2 C 0.6521(2) -0.3865(4) 0.5345(4) 0.0235(9) Uani 1 1 d . . .
H2A H 0.6014 -0.4100 0.5490 0.035 Uiso 1 1 calc R . .
H2B H 0.6829 -0.4631 0.5533 0.035 Uiso 1 1 calc R . .
H2C H 0.6585 -0.3615 0.4491 0.035 Uiso 1 1 calc R . .
C3 C 0.4566(3) -0.3253(5) 0.3388(4) 0.0322(11) Uani 1 1 d . . .
H3A H 0.4179 -0.3733 0.2946 0.039 Uiso 1 1 calc R . .
H3B H 0.4886 -0.3919 0.3774 0.039 Uiso 1 1 calc R . .
C4 C 0.5000 -0.2396(7) 0.2500 0.0306(15) Uani 1 2 d S . .
H4A H 0.4666 -0.1817 0.2038 0.037 Uiso 0.50 1 calc PR . .
H4B H 0.5334 -0.1817 0.2962 0.037 Uiso 0.50 1 calc PR . .
N1 N 0.4239(2) -0.2368(4) 0.4343(3) 0.0307(9) Uani 1 1 d . . .
H1A H 0.3979 -0.2870 0.4873 0.046 Uiso 1 1 calc R . .
H1B H 0.3943 -0.1763 0.3983 0.046 Uiso 1 1 calc R . .
H1C H 0.4596 -0.1937 0.4749 0.046 Uiso 1 1 calc R . .
P2 P 0.66611(5) -0.32043(10) 0.78015(9) 0.0127(2) Uani 1 1 d . . .
O1 O 0.63733(16) -0.0020(3) 0.6625(3) 0.0205(6) Uani 1 1 d . . .
O3 O 0.58520(14) -0.3561(3) 0.8049(3) 0.0201(6) Uani 1 1 d . . .
O4 O 0.69077(16) -0.2014(3) 0.8622(3) 0.0219(6) Uani 1 1 d . . .
O5 O 0.71313(15) -0.4442(3) 0.8004(3) 0.0209(6) Uani 1 1 d . . .
H7 H 0.768(3) -0.246(5) 0.533(6) 0.042(17) Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.902(3) 4_644 ?
Zn1 O2 1.933(3) . ?
Zn1 O4 1.959(3) 7 ?
Zn1 O1 1.965(3) 7 ?
Zn2 O3 1.942(3) 3_656 ?
Zn2 O3 1.942(3) . ?
Zn2 O6 1.958(3) 3_656 ?
Zn2 O6 1.958(3) . ?
P1 O2 1.515(3) . ?
P1 O1 1.525(3) . ?
P1 O6 1.533(3) . ?
P1 C1 1.839(4) . ?
O7 C1 1.455(5) . ?
O7 H7 0.79(6) . ?
C1 C2 1.517(5) . ?
C1 P2 1.839(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N1 1.473(6) . ?
C3 C4 1.498(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C3 1.498(6) 3_655 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
P2 O5 1.503(3) . ?
P2 O3 1.531(3) . ?
P2 O4 1.534(3) . ?
O1 Zn1 1.965(3) 7_556 ?
O4 Zn1 1.959(3) 7_556 ?
O5 Zn1 1.902(3) 4_645 ?

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
O5 Zn1 O2 117.80(12) 4_644 . ?
O5 Zn1 O4 109.04(12) 4_644 7 ?
O2 Zn1 O4 109.73(12) . 7 ?
O5 Zn1 O1 108.66(12) 4_644 7 ?
O2 Zn1 O1 107.61(12) . 7 ?
O4 Zn1 O1 102.96(11) 7 7 ?
O3 Zn2 O3 116.74(16) 3_656 . ?
O3 Zn2 O6 103.44(11) 3_656 3_656 ?
O3 Zn2 O6 104.46(11) . 3_656 ?
O3 Zn2 O6 104.46(11) 3_656 . ?
O3 Zn2 O6 103.44(11) . . ?
O6 Zn2 O6 125.27(18) 3_656 . ?
O2 P1 O1 112.29(16) . . ?
O2 P1 O6 109.67(15) . . ?
O1 P1 O6 110.65(17) . . ?
O2 P1 C1 108.11(17) . . ?
O1 P1 C1 108.86(16) . . ?
O6 P1 C1 107.09(16) . . ?
P1 O2 Zn1 145.46(18) . . ?
P1 O6 Zn2 124.12(16) . . ?
C1 O7 H7 118(4) . . ?
O7 C1 C2 111.1(3) . . ?
O7 C1 P1 107.6(2) . . ?
C2 C1 P1 109.4(3) . . ?
O7 C1 P2 106.2(3) . . ?
C2 C1 P2 109.0(3) . . ?
P1 C1 P2 113.5(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 109.0(4) . . ?
N1 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
N1 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C3 C4 C3 111.5(5) 3_655 . ?
C3 C4 H4A 109.3 3_655 . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 3_655 . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C3 N1 H1A 109.5 . . ?
C3 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C3 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
O5 P2 O3 109.36(16) . . ?
O5 P2 O4 111.75(17) . . ?
O3 P2 O4 110.70(16) . . ?
O5 P2 C1 109.05(17) . . ?
O3 P2 C1 107.46(16) . . ?
O4 P2 C1 108.41(16) . . ?
P1 O1 Zn1 128.77(16) . 7_556 ?
P2 O3 Zn2 126.01(16) . . ?
P2 O4 Zn1 127.99(17) . 7_556 ?
P2 O5 Zn1 144.46(19) . 4_645 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.125
####################################################################### 
# 
# 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_CCDC(1551493)
_database_code_depnum_ccdc_archive 'CCDC 1551493'
_audit_update_record             
;
2017-07-13 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Zinc diphosphonate dabco'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 N2 O14 P4 Zn3'
_chemical_formula_weight         712.27

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Aba2

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

_cell_length_a                   10.2729(3)
_cell_length_b                   18.1781(5)
_cell_length_c                   10.7119(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2000.36(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2147
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      28.28

_exptl_crystal_description       'Block like'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    3.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5042
_exptl_absorpt_correction_T_max  0.7967
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_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 SMART CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5141
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         28.28
_reflns_number_total             2147
_reflns_number_gt                2065
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.0559P)²+2.9264P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(1)
_refine_ls_number_reflns         2147
_refine_ls_number_parameters     150
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0929
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.000
_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 0.76815(5) 0.70953(3) 0.06559(6) 0.01233(14) Uani 1 1 d . . .
Zn2 Zn 1.0000 0.5000 -0.06123(8) 0.01233(17) Uani 1 2 d S . .
P1 P 0.86413(10) 0.63201(6) -0.18542(12) 0.0097(2) Uani 1 1 d . . .
P2 P 1.05813(10) 0.66198(6) 0.02668(12) 0.0094(2) Uani 1 1 d . . .
O1 O 1.1906(3) 0.69500(18) 0.0504(4) 0.0152(7) Uani 1 1 d . . .
O2 O 0.8370(4) 0.6527(2) -0.3189(3) 0.0182(7) Uani 1 1 d . . .
O3 O 0.9524(3) 0.6960(2) 0.1094(4) 0.0166(7) Uani 1 1 d . . .
O4 O 0.7566(3) 0.65698(19) -0.0955(3) 0.0160(7) Uani 1 1 d . . .
O5 O 1.0664(3) 0.57858(18) 0.0425(3) 0.0160(7) Uani 1 1 d . . .
O6 O 0.8820(3) 0.54878(17) -0.1756(4) 0.0170(7) Uani 1 1 d . . .
O7 O 0.9868(3) 0.7572(2) -0.1456(4) 0.0180(7) Uani 1 1 d . . .
H7 H 1.0509 0.7806 -0.1231 0.027 Uiso 1 1 calc R . .
N1 N 0.5826(4) 0.5498(2) 0.9270(5) 0.0215(9) Uani 1 1 d . . .
C1 C 1.0140(4) 0.6795(2) -0.1370(5) 0.0107(8) Uani 1 1 d . . .
C2 C 1.1288(4) 0.6579(3) -0.2195(5) 0.0174(10) Uani 1 1 d . . .
H2A H 1.1441 0.6060 -0.2122 0.026 Uiso 1 1 calc R . .
H2B H 1.2051 0.6842 -0.1933 0.026 Uiso 1 1 calc R . .
H2C H 1.1095 0.6698 -0.3048 0.026 Uiso 1 1 calc R . .
C3 C 0.6316(5) 0.4870(4) 1.0018(6) 0.0302(14) Uani 1 1 d . . .
H3A H 0.6338 0.4999 1.0896 0.036 Uiso 1 1 calc R . .
H3B H 0.7191 0.4741 0.9757 0.036 Uiso 1 1 calc R . .
C4 C 0.5604(6) 0.5244(4) 0.7962(6) 0.0348(15) Uani 1 1 d . . .
H4A H 0.6352 0.4970 0.7666 0.042 Uiso 1 1 calc R . .
H4B H 0.5473 0.5664 0.7416 0.042 Uiso 1 1 calc R . .
C5 C 0.4599(6) 0.5769(4) 0.9805(7) 0.0355(15) Uani 1 1 d . . .
H5A H 0.4202 0.6120 0.9241 0.043 Uiso 1 1 calc R . .
H5B H 0.4771 0.6016 1.0591 0.043 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.916(3) 4_465 ?
Zn1 O2 1.940(4) 7_645 ?
Zn1 O3 1.965(4) . ?
Zn1 O4 1.976(4) . ?
Zn2 O5 1.934(3) . ?
Zn2 O5 1.934(3) 2_765 ?
Zn2 O6 1.938(4) . ?
Zn2 O6 1.938(4) 2_765 ?
P1 O2 1.505(4) . ?
P1 O6 1.528(3) . ?
P1 O4 1.534(4) . ?
P1 C1 1.840(4) . ?
P2 O1 1.509(3) . ?
P2 O5 1.528(3) . ?
P2 O3 1.532(4) . ?
P2 C1 1.839(5) . ?
O1 Zn1 1.916(3) 4_565 ?
O2 Zn1 1.940(4) 7_644 ?
O7 C1 1.443(6) . ?
O7 H7 0.8200 . ?
N1 C5 1.469(8) . ?
N1 C3 1.483(8) . ?
N1 C4 1.492(8) . ?
C1 C2 1.525(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C5 1.512(9) 2_665 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C4 1.526(11) 2_665 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C3 1.512(9) 2_665 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?

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 O2 107.73(15) 4_465 7_645 ?
O1 Zn1 O3 122.26(14) 4_465 . ?
O2 Zn1 O3 108.52(16) 7_645 . ?
O1 Zn1 O4 109.80(16) 4_465 . ?
O2 Zn1 O4 105.44(15) 7_645 . ?
O3 Zn1 O4 101.87(15) . . ?
O5 Zn2 O5 109.9(2) . 2_765 ?
O5 Zn2 O6 104.22(14) . . ?
O5 Zn2 O6 118.70(15) 2_765 . ?
O5 Zn2 O6 118.70(15) . 2_765 ?
O5 Zn2 O6 104.22(14) 2_765 2_765 ?
O6 Zn2 O6 101.6(2) . 2_765 ?
O2 P1 O6 109.6(2) . . ?
O2 P1 O4 112.9(2) . . ?
O6 P1 O4 109.6(2) . . ?
O2 P1 C1 107.8(2) . . ?
O6 P1 C1 110.2(2) . . ?
O4 P1 C1 106.7(2) . . ?
O1 P2 O5 109.02(19) . . ?
O1 P2 O3 112.4(2) . . ?
O5 P2 O3 112.1(2) . . ?
O1 P2 C1 108.3(2) . . ?
O5 P2 C1 106.9(2) . . ?
O3 P2 C1 107.8(2) . . ?
P2 O1 Zn1 138.5(2) . 4_565 ?
P1 O2 Zn1 147.4(2) . 7_644 ?
P2 O3 Zn1 126.5(2) . . ?
P1 O4 Zn1 130.4(2) . . ?
P2 O5 Zn2 130.5(2) . . ?
P1 O6 Zn2 124.9(2) . . ?
C1 O7 H7 109.5 . . ?
C5 N1 C3 109.7(5) . . ?
C5 N1 C4 109.8(5) . . ?
C3 N1 C4 108.8(5) . . ?
O7 C1 C2 111.4(4) . . ?
O7 C1 P2 106.2(3) . . ?
C2 C1 P2 108.5(3) . . ?
O7 C1 P1 106.2(3) . . ?
C2 C1 P1 111.3(3) . . ?
P2 C1 P1 113.2(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C5 107.4(5) . 2_665 ?
N1 C3 H3A 110.2 . . ?
C5 C3 H3A 110.2 2_665 . ?
N1 C3 H3B 110.2 . . ?
C5 C3 H3B 110.2 2_665 . ?
H3A C3 H3B 108.5 . . ?
N1 C4 C4 107.7(3) . 2_665 ?
N1 C4 H4A 110.2 . . ?
C4 C4 H4A 110.2 2_665 . ?
N1 C4 H4B 110.2 . . ?
C4 C4 H4B 110.2 2_665 . ?
H4A C4 H4B 108.5 . . ?
N1 C5 C3 109.6(5) . 2_665 ?
N1 C5 H5A 109.8 . . ?
C3 C5 H5A 109.8 2_665 . ?
N1 C5 H5B 109.8 . . ?
C3 C5 H5B 109.8 2_665 . ?
H5A C5 H5B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.135

#####END#####
####################################################################### 
# 
# 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_CCDC(1495892)
_database_code_depnum_ccdc_archive 'CCDC 1495892'
_audit_update_record             
;
2017-07-13 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Zinc diphosphonate 1,2 diaminopropane'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H17 N3 O14 P4 Zn3'
_chemical_formula_weight         687.23

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

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

_cell_length_a                   18.1736(7)
_cell_length_b                   9.9376(6)
_cell_length_c                   10.3543(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1870.01(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2145
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.5

_exptl_crystal_description       'Block like'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    4.241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6301
_exptl_absorpt_correction_T_max  0.7278
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5840
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2145
_reflns_number_gt                1720
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.0397P)²+6.6994P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2145
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1147
_refine_ls_wR_factor_gt          0.1075
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
H7 H 0.263(6) 0.255(12) 0.480(12) 0.12(5) Uiso 1 1 d . . .
Zn1 Zn 0.19140(3) 0.50550(6) 0.68100(6) 0.01189(18) Uani 1 1 d . . .
Zn2 Zn 0.0000 0.24797(9) 0.2500 0.0117(2) Uani 1 2 d S . .
P1 P 0.16458(7) 0.18641(15) 0.21559(13) 0.0107(3) Uani 1 1 d . . .
P2 P 0.11550(7) 0.38345(15) 0.42719(13) 0.0118(3) Uani 1 1 d . . .
O1 O 0.21196(19) 0.0648(4) 0.1942(4) 0.0173(9) Uani 1 1 d . . .
O2 O 0.1244(2) 0.4061(4) 0.5714(4) 0.0155(8) Uani 1 1 d . . .
O3 O 0.1895(2) 0.3052(4) 0.1331(4) 0.0205(9) Uani 1 1 d . . .
O4 O 0.1410(2) 0.5043(4) 0.3485(4) 0.0164(8) Uani 1 1 d . . .
O5 O 0.08455(19) 0.1478(4) 0.1930(4) 0.0201(9) Uani 1 1 d . . .
O6 O 0.03542(19) 0.3493(4) 0.3977(4) 0.0179(9) Uani 1 1 d . . .
O7 O 0.2499(2) 0.2803(5) 0.3999(5) 0.0263(11) Uani 1 1 d . . .
C1 C 0.1563(3) 0.1235(6) 0.4693(6) 0.0202(13) Uani 1 1 d . . .
H1A H 0.1059 0.0971 0.4574 0.030 Uiso 1 1 calc R . .
H1B H 0.1639 0.1495 0.5576 0.030 Uiso 1 1 calc R . .
H1C H 0.1880 0.0494 0.4485 0.030 Uiso 1 1 calc R . .
C2 C 0.1732(3) 0.2385(6) 0.3836(5) 0.0134(11) Uani 1 1 d . . .
C3 C 0.0000 0.2388(12) 0.7500 0.077(5) Uani 1 2 d S . .
C4 C -0.0433(8) 0.1637(15) 0.6619(15) 0.097(5) Uani 1 1 d . . .
N1 N 0.0000 0.3837(8) 0.7500 0.041(2) Uani 1 2 d S . .
H1D H 0.0306 0.4135 0.8106 0.061 Uiso 0.50 1 calc PR . .
H1E H -0.0452 0.4135 0.7663 0.061 Uiso 0.50 1 calc PR . .
H1F H 0.0146 0.4135 0.6731 0.061 Uiso 0.50 1 calc PR . .
N2 N -0.0941(16) 0.206(3) 0.654(4) 0.60(5) Uani 1 1 d . . .
H2A H -0.1213 0.1583 0.5994 0.903 Uiso 1 1 calc R . .
H2B H -0.0897 0.2899 0.6252 0.903 Uiso 1 1 calc R . .
H2C H -0.1156 0.2069 0.7314 0.903 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.895(4) 2 ?
Zn1 O2 1.937(4) . ?
Zn1 O3 1.946(4) 8_566 ?
Zn1 O4 1.964(4) 8_566 ?
Zn2 O5 1.924(4) . ?
Zn2 O5 1.924(4) 4 ?
Zn2 O6 1.941(4) . ?
Zn2 O6 1.941(4) 4 ?
P1 O1 1.500(4) . ?
P1 O5 1.522(4) . ?
P1 O3 1.526(4) . ?
P1 C2 1.822(6) . ?
P2 O2 1.518(4) . ?
P2 O4 1.524(4) . ?
P2 O6 1.525(4) . ?
P2 C2 1.838(6) . ?
O1 Zn1 1.895(4) 2_554 ?
O3 Zn1 1.946(4) 8_565 ?
O4 Zn1 1.964(4) 8_565 ?
O7 C2 1.463(7) . ?
C1 C2 1.479(8) . ?
C3 C4 1.417(16) . ?
C3 C4 1.417(16) 4_556 ?
C3 N1 1.440(13) . ?
C4 N2 1.02(3) . ?

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 O2 115.93(17) 2 . ?
O1 Zn1 O3 113.06(17) 2 8_566 ?
O2 Zn1 O3 109.42(17) . 8_566 ?
O1 Zn1 O4 110.46(17) 2 8_566 ?
O2 Zn1 O4 101.50(16) . 8_566 ?
O3 Zn1 O4 105.36(17) 8_566 8_566 ?
O5 Zn2 O5 117.7(3) . 4 ?
O5 Zn2 O6 104.19(15) . . ?
O5 Zn2 O6 106.95(17) 4 . ?
O5 Zn2 O6 106.95(17) . 4 ?
O5 Zn2 O6 104.19(15) 4 4 ?
O6 Zn2 O6 117.5(3) . 4 ?
O1 P1 O5 108.8(2) . . ?
O1 P1 O3 111.8(2) . . ?
O5 P1 O3 113.1(2) . . ?
O1 P1 C2 108.7(2) . . ?
O5 P1 C2 107.5(2) . . ?
O3 P1 C2 106.8(2) . . ?
O2 P2 O4 112.1(2) . . ?
O2 P2 O6 109.3(2) . . ?
O4 P2 O6 111.1(2) . . ?
O2 P2 C2 107.3(2) . . ?
O4 P2 C2 108.2(2) . . ?
O6 P2 C2 108.7(2) . . ?
P1 O1 Zn1 147.1(3) . 2_554 ?
P2 O2 Zn1 135.9(2) . . ?
P1 O3 Zn1 127.6(2) . 8_565 ?
P2 O4 Zn1 125.1(2) . 8_565 ?
P1 O5 Zn2 125.9(2) . . ?
P2 O6 Zn2 126.1(2) . . ?
O7 C2 C1 110.4(5) . . ?
O7 C2 P1 105.8(4) . . ?
C1 C2 P1 109.6(4) . . ?
O7 C2 P2 107.0(4) . . ?
C1 C2 P2 109.8(4) . . ?
P1 C2 P2 114.1(3) . . ?
C4 C3 C4 116.4(14) . 4_556 ?
C4 C3 N1 121.8(7) . . ?
C4 C3 N1 121.8(7) 4_556 . ?
N2 C4 C3 110(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.196
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.164

#####END#####
####################################################################### 
# 
# 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_CCDC(1495891)
_database_code_depnum_ccdc_archive 'CCDC 1495891'
_audit_update_record             
;
2017-07-13 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Zinc diphosphonate diethelenetriamine'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H22 N3 O14 P4 Zn3'
_chemical_formula_weight         704.28

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   20.3473(5)
_cell_length_b                   9.1752(2)
_cell_length_c                   23.2486(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2540(10)
_cell_angle_gamma                90.00
_cell_volume                     4339.25(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3773
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      25.00

_exptl_crystal_description       'Rod like'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2824
_exptl_absorpt_coefficient_mu    3.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5283
_exptl_absorpt_correction_T_max  0.7112
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16188
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3773
_reflns_number_gt                3419
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.0638P)²+30.9297P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3773
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1104
_refine_ls_wR_factor_gt          0.1078
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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 0.22468(3) 0.71708(5) 0.32945(2) 0.02047(16) Uani 1 1 d . . .
Zn3 Zn 0.15758(3) 1.23839(6) 0.37335(2) 0.02561(17) Uani 1 1 d . . .
P1 P 0.28829(5) 0.90478(12) 0.22756(4) 0.0168(2) Uani 1 1 d . . .
P3 P 0.02817(5) 1.13540(12) 0.42849(5) 0.0186(2) Uani 1 1 d . . .
P4 P 0.13358(6) 0.91005(13) 0.40594(5) 0.0206(3) Uani 1 1 d . . .
O1 O 0.27321(17) 0.8580(4) 0.28790(13) 0.0300(8) Uani 1 1 d . . .
O3 O 0.14645(18) 0.7831(4) 0.36613(16) 0.0340(8) Uani 1 1 d . . .
O6 O 0.13821(17) 0.8613(4) 0.46886(14) 0.0297(8) Uani 1 1 d . . .
O16 O 0.17750(16) 1.0401(4) 0.39471(16) 0.0317(8) Uani 1 1 d . . .
O10 O 0.34514(16) 0.8194(4) 0.20300(15) 0.0349(9) Uani 1 1 d . . .
O13 O 0.21359(19) 0.7138(4) 0.16784(15) 0.0332(8) Uani 1 1 d . . .
H13 H 0.2082 0.6681 0.1977 0.050 Uiso 1 1 calc R . .
O14 O 0.00568(17) 0.8492(4) 0.40644(15) 0.0334(8) Uani 1 1 d . . .
H14 H 0.0145 0.7752 0.3884 0.050 Uiso 1 1 calc R . .
C1 C 0.2155(2) 0.8682(5) 0.18045(18) 0.0201(9) Uani 1 1 d . . .
C2 C 0.1523(2) 0.9212(7) 0.2069(2) 0.0374(13) Uani 1 1 d . . .
H2A H 0.1555 1.0238 0.2144 0.056 Uiso 1 1 calc R . .
H2B H 0.1453 0.8700 0.2423 0.056 Uiso 1 1 calc R . .
H2C H 0.1161 0.9031 0.1807 0.056 Uiso 1 1 calc R . .
C3 C 0.0490(2) 0.9655(5) 0.38980(19) 0.0223(9) Uani 1 1 d . . .
C4 C 0.0376(3) 0.9892(7) 0.3250(2) 0.0351(12) Uani 1 1 d . . .
H4A H 0.0651 1.0670 0.3122 0.053 Uiso 1 1 calc R . .
H4B H -0.0077 1.0140 0.3176 0.053 Uiso 1 1 calc R . .
H4C H 0.0480 0.9014 0.3047 0.053 Uiso 1 1 calc R . .
C5 C -0.0003(7) 0.5507(12) 0.3281(5) 0.104(4) Uani 1 1 d . . .
H5A H -0.0091 0.6494 0.3152 0.125 Uiso 1 1 calc R . .
H5B H 0.0176 0.4965 0.2963 0.125 Uiso 1 1 calc R . .
C6 C -0.0616(6) 0.4825(15) 0.3461(9) 0.155(8) Uani 1 1 d . . .
H6A H -0.0945 0.4895 0.3153 0.186 Uiso 1 1 calc R . .
H6B H -0.0542 0.3802 0.3544 0.186 Uiso 1 1 calc R . .
N1 N 0.0481(4) 0.5533(8) 0.3768(5) 0.099(3) Uani 1 1 d . . .
H1A H 0.0849 0.5965 0.3656 0.148 Uiso 1 1 calc R . .
H1B H 0.0571 0.4624 0.3878 0.148 Uiso 1 1 calc R . .
H1C H 0.0315 0.6024 0.4061 0.148 Uiso 1 1 calc R . .
N2 N -0.0851(6) 0.5566(14) 0.3973(9) 0.186(8) Uani 1 1 d . . .
N3 N -0.2040(4) 0.5984(9) 0.4622(4) 0.095(3) Uani 1 1 d . . .
H3A H -0.2185 0.6115 0.4977 0.143 Uiso 1 1 calc R . .
H3B H -0.2380 0.5960 0.4374 0.143 Uiso 1 1 calc R . .
H3C H -0.1774 0.6715 0.4532 0.143 Uiso 1 1 calc R . .
P2 P 0.22436(5) 0.94675(12) 0.10814(5) 0.0182(2) Uani 1 1 d . . .
O2 O 0.30139(17) 1.0688(4) 0.22707(14) 0.0276(7) Uani 1 1 d . . .
Zn2 Zn 0.10453(2) 0.97293(6) 0.53318(2) 0.02005(16) Uani 1 1 d . . .
O7 O 0.06477(16) 1.2577(4) 0.39836(15) 0.0290(8) Uani 1 1 d . . .
O4 O 0.22478(17) 1.1111(3) 0.11226(13) 0.0265(7) Uani 1 1 d . . .
O8 O -0.04622(15) 1.1525(4) 0.42362(14) 0.0249(7) Uani 1 1 d . . .
O5 O 0.28777(16) 0.8825(4) 0.08470(13) 0.0258(7) Uani 1 1 d . . .
O9 O 0.05078(15) 1.1200(3) 0.49103(13) 0.0230(7) Uani 1 1 d . . .
O11 O 0.16561(16) 0.8965(4) 0.07179(14) 0.0281(7) Uani 1 1 d . . .
C8 C -0.1693(7) 0.4656(12) 0.4596(6) 0.115(4) Uani 1 1 d . . .
H8A H -0.1329 0.4670 0.4872 0.138 Uiso 1 1 calc R . .
H8B H -0.1982 0.3858 0.4695 0.138 Uiso 1 1 calc R . .
C7 C -0.1457(9) 0.4440(17) 0.4052(6) 0.154(7) Uani 1 1 d . . .
H7A H -0.1800 0.4628 0.3765 0.184 Uiso 1 1 calc R . .
H7B H -0.1308 0.3444 0.4009 0.184 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.903(3) . ?
Zn1 O3 1.920(3) . ?
Zn1 O4 1.944(3) 4_545 ?
Zn1 O2 1.956(3) 4_545 ?
Zn3 O10 1.924(3) 4 ?
Zn3 O16 1.927(3) . ?
Zn3 O5 1.972(3) 4 ?
Zn3 O7 1.996(3) . ?
P1 O1 1.505(3) . ?
P1 O10 1.519(3) . ?
P1 O2 1.529(3) . ?
P1 C1 1.853(4) . ?
P3 O9 1.522(3) . ?
P3 O8 1.523(3) . ?
P3 O7 1.525(3) . ?
P3 C3 1.854(5) . ?
P4 O3 1.514(3) . ?
P4 O16 1.517(3) . ?
P4 O6 1.531(3) . ?
P4 C3 1.825(5) . ?
O6 Zn2 1.949(3) . ?
O10 Zn3 1.924(3) 4_545 ?
O13 C1 1.447(5) . ?
O13 H13 0.8200 . ?
O14 C3 1.443(5) . ?
O14 H14 0.8200 . ?
C1 C2 1.518(6) . ?
C1 P2 1.841(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.534(7) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.464(17) . ?
C5 N1 1.484(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N2 1.46(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 C7 1.62(2) . ?
N3 C8 1.410(12) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
P2 O4 1.511(3) . ?
P2 O11 1.520(3) . ?
P2 O5 1.530(3) . ?
O2 Zn1 1.956(3) 4 ?
Zn2 O11 1.933(3) 6_576 ?
Zn2 O8 1.948(3) 5_576 ?
Zn2 O9 1.982(3) . ?
O4 Zn1 1.944(3) 4 ?
O8 Zn2 1.948(3) 5_576 ?
O5 Zn3 1.972(3) 4_545 ?
O11 Zn2 1.933(3) 6_575 ?
C8 C7 1.376(18) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?

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 O3 117.08(16) . . ?
O1 Zn1 O4 114.91(15) . 4_545 ?
O3 Zn1 O4 106.23(16) . 4_545 ?
O1 Zn1 O2 105.51(15) . 4_545 ?
O3 Zn1 O2 107.61(15) . 4_545 ?
O4 Zn1 O2 104.59(14) 4_545 4_545 ?
O10 Zn3 O16 127.17(17) 4 . ?
O10 Zn3 O5 101.64(14) 4 4 ?
O16 Zn3 O5 113.11(15) . 4 ?
O10 Zn3 O7 103.07(15) 4 . ?
O16 Zn3 O7 101.75(14) . . ?
O5 Zn3 O7 108.88(14) 4 . ?
O1 P1 O10 112.1(2) . . ?
O1 P1 O2 109.07(19) . . ?
O10 P1 O2 111.8(2) . . ?
O1 P1 C1 108.8(2) . . ?
O10 P1 C1 106.83(19) . . ?
O2 P1 C1 108.1(2) . . ?
O9 P3 O8 111.08(18) . . ?
O9 P3 O7 111.5(2) . . ?
O8 P3 O7 112.60(19) . . ?
O9 P3 C3 108.52(19) . . ?
O8 P3 C3 106.8(2) . . ?
O7 P3 C3 106.05(19) . . ?
O3 P4 O16 112.9(2) . . ?
O3 P4 O6 110.6(2) . . ?
O16 P4 O6 111.7(2) . . ?
O3 P4 C3 105.3(2) . . ?
O16 P4 C3 107.6(2) . . ?
O6 P4 C3 108.4(2) . . ?
P1 O1 Zn1 141.8(2) . . ?
P4 O3 Zn1 132.1(2) . . ?
P4 O6 Zn2 124.3(2) . . ?
P4 O16 Zn3 131.7(2) . . ?
P1 O10 Zn3 122.6(2) . 4_545 ?
C1 O13 H13 109.5 . . ?
C3 O14 H14 109.5 . . ?
O13 C1 C2 112.1(4) . . ?
O13 C1 P2 101.6(3) . . ?
C2 C1 P2 110.2(3) . . ?
O13 C1 P1 108.4(3) . . ?
C2 C1 P1 112.1(3) . . ?
P2 C1 P1 112.1(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O14 C3 C4 106.7(4) . . ?
O14 C3 P4 108.5(3) . . ?
C4 C3 P4 111.3(3) . . ?
O14 C3 P3 110.1(3) . . ?
C4 C3 P3 109.0(3) . . ?
P4 C3 P3 111.1(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 110.2(10) . . ?
C6 C5 H5A 109.6 . . ?
N1 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
N1 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N2 C6 C5 109.2(12) . . ?
N2 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N2 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C5 N1 H1A 109.5 . . ?
C5 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C5 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C6 N2 C7 93.4(13) . . ?
C8 N3 H3A 109.5 . . ?
C8 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C8 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
O4 P2 O11 109.94(19) . . ?
O4 P2 O5 113.8(2) . . ?
O11 P2 O5 110.13(19) . . ?
O4 P2 C1 109.46(19) . . ?
O11 P2 C1 107.3(2) . . ?
O5 P2 C1 105.91(19) . . ?
P1 O2 Zn1 130.1(2) . 4 ?
O11 Zn2 O8 121.30(14) 6_576 5_576 ?
O11 Zn2 O6 116.65(15) 6_576 . ?
O8 Zn2 O6 108.27(15) 5_576 . ?
O11 Zn2 O9 98.63(14) 6_576 . ?
O8 Zn2 O9 108.76(13) 5_576 . ?
O6 Zn2 O9 100.24(13) . . ?
P3 O7 Zn3 122.9(2) . . ?
P2 O4 Zn1 123.08(19) . 4 ?
P3 O8 Zn2 121.07(19) . 5_576 ?
P2 O5 Zn3 123.59(18) . 4_545 ?
P3 O9 Zn2 133.44(19) . . ?
P2 O11 Zn2 124.1(2) . 6_575 ?
C7 C8 N3 110.4(12) . . ?
C7 C8 H8A 109.6 . . ?
N3 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
N3 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C8 C7 N2 107.1(14) . . ?
C8 C7 H7A 110.3 . . ?
N2 C7 H7A 110.3 . . ?
C8 C7 H7B 110.3 . . ?
N2 C7 H7B 110.3 . . ?
H7A C7 H7B 108.6 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.889
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.131

#####END#####
