# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Anne Richards'
_publ_contact_author_email       A.RICHARDS@TCU.EDU

_publ_section_title              
;
5-Pyrimidine phosphonic acid as a building block for
the synthesis of homo and hetero metal phosphonate polymers
;
loop_
_publ_author_name
'Anne Richards'
'Leslie A Lesikar'
'Jean-Luc Montchamp'
'Christian R Samanamu'
'Elena N Zamora'

# Attachment '4.CIF'

data_c:\pympox~1\pympoc~1\ar476xx
_database_code_depnum_ccdc_archive 'CCDC 681512'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (((PymPO3(H))2Cu2(H2O)4)(SO3CF3)2.H2O)n
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Cu2 F6 N4 O18 P2 S2'
_chemical_formula_weight         851.44

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.9181(15)
_cell_length_b                   11.6269(13)
_cell_length_c                   18.8112(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.025(6)
_cell_angle_gamma                90.00
_cell_volume                     2735.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    5133
_cell_measurement_theta_min      2.3345
_cell_measurement_theta_max      28.2825

_exptl_crystal_description       block
_exptl_crystal_colour            'pale blue'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1704
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9438
_exptl_absorpt_correction_T_max  0.9676
_exptl_absorpt_process_details   'SADABS: SAINT+, 2001'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(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 1000'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <0.01
_diffrn_reflns_number            15631
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         28.28
_reflns_number_total             6462
_reflns_number_gt                5004
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART v. 5.626'
_computing_cell_refinement       'Bruker SAINT+ v. 6.36a'
_computing_data_reduction        'Bruker SAINT+ v. 6.36a'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'

_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)+(0.0394P)²+2.0698P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6462
_refine_ls_number_parameters     409
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0812
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.042
_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
Cu1 Cu 0.23613(3) 0.07326(3) 0.48680(2) 0.01158(9) Uani 1 1 d . . .
Cu2 Cu 0.23860(3) 0.57023(3) 0.49833(2) 0.01126(9) Uani 1 1 d . . .
S2 S 0.12619(6) 0.73637(6) 0.62738(4) 0.01638(16) Uani 1 1 d . . .
P1 P 0.00311(6) 0.68963(6) 0.37363(4) 0.01011(15) Uani 1 1 d . . .
P2 P 0.53174(6) 0.80335(6) 0.41547(4) 0.01177(15) Uani 1 1 d . . .
F4 F 0.1433(2) 0.8013(3) 0.76387(16) 0.0727(9) Uani 1 1 d . . .
F5 F 0.29041(18) 0.8097(2) 0.75305(13) 0.0522(7) Uani 1 1 d . . .
F6 F 0.2269(2) 0.6467(3) 0.76674(14) 0.0682(8) Uani 1 1 d . . .
O1 O 0.09592(15) 0.61726(17) 0.42601(12) 0.0155(4) Uani 1 1 d . . .
O2 O 0.02080(16) 0.81335(16) 0.36126(12) 0.0157(4) Uani 1 1 d . . .
O3 O -0.05588(16) 0.62710(18) 0.29166(12) 0.0176(4) Uani 1 1 d D . .
O4 O 0.25390(17) 0.48908(18) 0.39043(13) 0.0219(5) Uani 1 1 d D . .
O5 O 0.38394(16) 0.52603(17) 0.57108(13) 0.0213(5) Uani 1 1 d D . .
H5B H 0.4021 0.4554 0.5792 0.026 Uiso 1 1 d RD . .
O6 O 0.62189(15) 0.86454(18) 0.48185(13) 0.0192(5) Uani 1 1 d . . .
O7 O 0.49270(19) 0.87921(19) 0.33961(13) 0.0265(5) Uani 1 1 d D . .
O8 O 0.54828(16) 0.68157(17) 0.40199(13) 0.0185(5) Uani 1 1 d . . .
O9 O 0.20360(19) 0.1685(2) 0.36842(13) 0.0283(5) Uani 1 1 d D . .
H9B H 0.1572 0.1606 0.3188 0.034 Uiso 1 1 d RD . .
O10 O 0.08639(15) 0.01222(17) 0.43950(13) 0.0204(5) Uani 1 1 d D . .
O11 O 0.26942(18) -0.00344(18) 0.60852(13) 0.0240(5) Uani 1 1 d D . .
O15 O 0.09962(18) 0.8540(2) 0.60074(16) 0.0330(6) Uani 1 1 d . . .
O16 O 0.03478(17) 0.66700(19) 0.61682(13) 0.0247(5) Uani 1 1 d . . .
O17 O 0.20029(19) 0.68339(19) 0.60322(14) 0.0277(5) Uani 1 1 d . . .
N1 N 0.18271(18) 0.42198(19) 0.52400(13) 0.0118(5) Uani 1 1 d . . .
N3 N 0.30057(18) 0.7186(2) 0.48138(14) 0.0126(5) Uani 1 1 d . . .
N4 N 0.29209(18) 0.92031(19) 0.46598(13) 0.0111(5) Uani 1 1 d . . .
N5 N 0.18309(18) 0.2186(2) 0.51954(14) 0.0119(5) Uani 1 1 d . . .
C1 C 0.1217(2) 0.4183(2) 0.56274(16) 0.0131(6) Uani 1 1 d . . .
H1 H 0.1006 0.4877 0.5773 0.016 Uiso 1 1 calc R . .
C2 C -0.0888(2) 0.6849(2) 0.41794(16) 0.0111(5) Uani 1 1 d . . .
C3 C 0.2103(2) 0.3215(2) 0.50367(17) 0.0123(6) Uani 1 1 d . . .
H3 H 0.2523 0.3239 0.4759 0.015 Uiso 1 1 calc R . .
C4 C 0.3815(2) 0.7147(2) 0.46048(17) 0.0138(6) Uani 1 1 d . . .
H4 H 0.4124 0.6433 0.4593 0.017 Uiso 1 1 calc R . .
C5 C 0.2601(2) 0.8213(2) 0.48400(17) 0.0122(5) Uani 1 1 d . . .
H5 H 0.2047 0.8241 0.4998 0.015 Uiso 1 1 calc R . .
C6 C 0.3717(2) 0.9159(2) 0.44375(16) 0.0109(5) Uani 1 1 d . . .
H6 H 0.3950 0.9845 0.4299 0.013 Uiso 1 1 calc R . .
C7 C -0.1230(2) 0.7842(2) 0.44052(16) 0.0123(6) Uani 1 1 d . . .
H7 H -0.1037 0.8559 0.4276 0.015 Uiso 1 1 calc R . .
C8 C 0.4203(2) 0.8131(2) 0.44068(16) 0.0115(5) Uani 1 1 d . . .
C10 C 0.2011(3) 0.7489(4) 0.7339(2) 0.0343(9) Uani 1 1 d . . .
S1 S 0.39745(6) 0.29464(7) 0.29264(5) 0.02049(17) Uani 1 1 d . . .
F1 F 0.4632(2) 0.1080(2) 0.24977(14) 0.0510(7) Uani 1 1 d . . .
F2 F 0.33938(18) 0.08103(18) 0.28673(15) 0.0466(6) Uani 1 1 d . . .
F3 F 0.49913(18) 0.11683(19) 0.37285(12) 0.0421(6) Uani 1 1 d . . .
O12 O 0.3760(2) 0.3158(2) 0.35966(15) 0.0313(6) Uani 1 1 d . . .
O13 O 0.49776(19) 0.3441(2) 0.30011(13) 0.0287(5) Uani 1 1 d . . .
O14 O 0.3102(2) 0.3101(2) 0.21632(16) 0.0407(7) Uani 1 1 d . . .
C9 C 0.4269(3) 0.1409(3) 0.29989(19) 0.0245(7) Uani 1 1 d . . .
O18 O 0.03738(16) 0.43320(17) 0.28048(12) 0.0219(5) Uani 1 1 d D . .
H3A H -0.0282 0.5625 0.2934 0.038(11) Uiso 1 1 d RD . .
H18B H 0.0176 0.3954 0.2377 0.043(12) Uiso 1 1 d RD . .
H18A H 0.0119 0.3812 0.3014 0.055(14) Uiso 1 1 d RD . .
H9A H 0.2658 0.1981 0.3783 0.09(2) Uiso 1 1 d RD . .
H10B H 0.0672 -0.0499 0.4105 0.034(11) Uiso 1 1 d RD . .
H10A H 0.0286 0.0498 0.4266 0.047(12) Uiso 1 1 d RD . .
H11B H 0.2198 -0.0441 0.6193 0.046(12) Uiso 1 1 d RD . .
H11A H 0.2939 0.0400 0.6525 0.075(16) Uiso 1 1 d RD . .
H4A H 0.1906 0.4728 0.3503 0.068(15) Uiso 1 1 d RD . .
H4B H 0.2852 0.4427 0.3695 0.055(13) Uiso 1 1 d RD . .
H5A H 0.4183 0.5732 0.6162 0.084(18) Uiso 1 1 d RD . .
H7A H 0.5153 0.8578 0.3091 0.073(17) Uiso 1 1 d RD . .


_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
Cu1 O6 1.9373(19) 3_666 ?
Cu1 O10 2.003(2) . ?
Cu1 N5 2.044(2) . ?
Cu1 N4 2.047(2) 1_545 ?
Cu1 O11 2.307(2) . ?
Cu1 O9 2.347(2) . ?
Cu2 O1 1.9294(19) . ?
Cu2 O5 1.949(2) . ?
Cu2 N3 2.015(2) . ?
Cu2 N1 2.035(2) . ?
Cu2 O4 2.331(2) . ?
S2 O17 1.436(2) . ?
S2 O16 1.445(2) . ?
S2 O15 1.447(2) . ?
S2 C10 1.814(4) . ?
P1 O1 1.493(2) . ?
P1 O2 1.495(2) . ?
P1 O3 1.572(2) . ?
P1 C2 1.808(3) . ?
P2 O8 1.474(2) . ?
P2 O6 1.505(2) . ?
P2 O7 1.559(2) . ?
P2 C8 1.814(3) . ?
F4 C10 1.317(4) . ?
F5 C10 1.335(4) . ?
F6 C10 1.314(5) . ?
O3 H3A 0.8379 . ?
O4 H4A 0.8935 . ?
O4 H4B 0.8872 . ?
O5 H5B 0.8527 . ?
O5 H5A 0.9448 . ?
O6 Cu1 1.9373(19) 3_666 ?
O7 H7A 0.8068 . ?
O9 H9B 0.8770 . ?
O9 H9A 0.8725 . ?
O10 H10B 0.8732 . ?
O10 H10A 0.8513 . ?
O11 H11B 0.9299 . ?
O11 H11A 0.8991 . ?
N1 C3 1.337(3) . ?
N1 C1 1.340(3) . ?
N3 C5 1.330(3) . ?
N3 C4 1.346(3) . ?
N4 C5 1.331(3) . ?
N4 C6 1.346(3) . ?
N4 Cu1 2.047(2) 1_565 ?
N5 C3 1.328(3) . ?
N5 C7 1.348(3) 3_566 ?
C1 C2 1.388(4) 3_566 ?
C1 H1 0.9400 . ?
C2 C7 1.386(4) . ?
C2 C1 1.388(4) 3_566 ?
C3 H3 0.9400 . ?
C4 C8 1.384(4) . ?
C4 H4 0.9400 . ?
C5 H5 0.9400 . ?
C6 C8 1.387(4) . ?
C6 H6 0.9400 . ?
C7 N5 1.348(3) 3_566 ?
C7 H7 0.9400 . ?
S1 O14 1.428(3) . ?
S1 O12 1.439(2) . ?
S1 O13 1.459(2) . ?
S1 C9 1.825(3) . ?
F1 C9 1.307(4) . ?
F2 C9 1.329(4) . ?
F3 C9 1.327(4) . ?
O18 H18B 0.8500 . ?
O18 H18A 0.8765 . ?

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
O6 Cu1 O10 172.35(9) 3_666 . ?
O6 Cu1 N5 93.13(9) 3_666 . ?
O10 Cu1 N5 89.07(9) . . ?
O6 Cu1 N4 87.68(9) 3_666 1_545 ?
O10 Cu1 N4 90.93(8) . 1_545 ?
N5 Cu1 N4 173.62(9) . 1_545 ?
O6 Cu1 O11 96.22(8) 3_666 . ?
O10 Cu1 O11 91.18(8) . . ?
N5 Cu1 O11 87.84(9) . . ?
N4 Cu1 O11 85.78(8) 1_545 . ?
O6 Cu1 O9 81.89(9) 3_666 . ?
O10 Cu1 O9 90.91(9) . . ?
N5 Cu1 O9 87.18(9) . . ?
N4 Cu1 O9 99.20(9) 1_545 . ?
O11 Cu1 O9 174.57(8) . . ?
O1 Cu2 O5 178.73(9) . . ?
O1 Cu2 N3 91.46(9) . . ?
O5 Cu2 N3 87.28(9) . . ?
O1 Cu2 N1 91.43(9) . . ?
O5 Cu2 N1 89.83(9) . . ?
N3 Cu2 N1 175.84(9) . . ?
O1 Cu2 O4 87.70(8) . . ?
O5 Cu2 O4 92.38(8) . . ?
N3 Cu2 O4 89.99(9) . . ?
N1 Cu2 O4 93.11(8) . . ?
O17 S2 O16 115.37(14) . . ?
O17 S2 O15 113.93(14) . . ?
O16 S2 O15 113.83(14) . . ?
O17 S2 C10 103.85(16) . . ?
O16 S2 C10 103.98(15) . . ?
O15 S2 C10 104.04(18) . . ?
O1 P1 O2 119.41(12) . . ?
O1 P1 O3 108.36(11) . . ?
O2 P1 O3 110.07(12) . . ?
O1 P1 C2 105.10(12) . . ?
O2 P1 C2 107.43(12) . . ?
O3 P1 C2 105.51(12) . . ?
O8 P2 O6 117.42(12) . . ?
O8 P2 O7 113.83(13) . . ?
O6 P2 O7 108.72(13) . . ?
O8 P2 C8 108.71(12) . . ?
O6 P2 C8 104.54(12) . . ?
O7 P2 C8 102.09(13) . . ?
P1 O1 Cu2 161.72(14) . . ?
P1 O3 H3A 110.0 . . ?
Cu2 O4 H4A 112.9 . . ?
Cu2 O4 H4B 152.0 . . ?
H4A O4 H4B 89.4 . . ?
Cu2 O5 H5B 120.9 . . ?
Cu2 O5 H5A 115.9 . . ?
H5B O5 H5A 113.9 . . ?
P2 O6 Cu1 142.82(13) . 3_666 ?
P2 O7 H7A 112.9 . . ?
Cu1 O9 H9B 134.9 . . ?
Cu1 O9 H9A 103.0 . . ?
H9B O9 H9A 117.8 . . ?
Cu1 O10 H10B 123.0 . . ?
Cu1 O10 H10A 127.8 . . ?
H10B O10 H10A 104.7 . . ?
Cu1 O11 H11B 124.6 . . ?
Cu1 O11 H11A 121.8 . . ?
H11B O11 H11A 95.9 . . ?
C3 N1 C1 117.2(2) . . ?
C3 N1 Cu2 119.00(18) . . ?
C1 N1 Cu2 123.76(19) . . ?
C5 N3 C4 117.6(2) . . ?
C5 N3 Cu2 123.00(18) . . ?
C4 N3 Cu2 119.23(18) . . ?
C5 N4 C6 117.3(2) . . ?
C5 N4 Cu1 120.32(18) . 1_565 ?
C6 N4 Cu1 121.78(18) . 1_565 ?
C3 N5 C7 117.1(2) . 3_566 ?
C3 N5 Cu1 120.04(18) . . ?
C7 N5 Cu1 122.83(18) 3_566 . ?
N1 C1 C2 122.1(2) . 3_566 ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 3_566 . ?
C7 C2 C1 116.3(2) . 3_566 ?
C7 C2 P1 121.6(2) . . ?
C1 C2 P1 122.0(2) 3_566 . ?
N5 C3 N1 125.2(3) . . ?
N5 C3 H3 117.4 . . ?
N1 C3 H3 117.4 . . ?
N3 C4 C8 121.7(3) . . ?
N3 C4 H4 119.1 . . ?
C8 C4 H4 119.1 . . ?
N3 C5 N4 124.9(3) . . ?
N3 C5 H5 117.5 . . ?
N4 C5 H5 117.5 . . ?
N4 C6 C8 121.9(2) . . ?
N4 C6 H6 119.0 . . ?
C8 C6 H6 119.0 . . ?
N5 C7 C2 122.1(3) 3_566 . ?
N5 C7 H7 118.9 3_566 . ?
C2 C7 H7 118.9 . . ?
C4 C8 C6 116.5(2) . . ?
C4 C8 P2 119.9(2) . . ?
C6 C8 P2 123.6(2) . . ?
F6 C10 F4 108.0(3) . . ?
F6 C10 F5 108.9(3) . . ?
F4 C10 F5 108.1(3) . . ?
F6 C10 S2 110.7(3) . . ?
F4 C10 S2 110.3(3) . . ?
F5 C10 S2 110.9(2) . . ?
O14 S1 O12 116.59(16) . . ?
O14 S1 O13 113.77(15) . . ?
O12 S1 O13 113.97(15) . . ?
O14 S1 C9 105.23(15) . . ?
O12 S1 C9 103.17(14) . . ?
O13 S1 C9 101.81(15) . . ?
F1 C9 F3 109.1(3) . . ?
F1 C9 F2 108.9(3) . . ?
F3 C9 F2 107.3(3) . . ?
F1 C9 S1 112.2(2) . . ?
F3 C9 S1 109.1(2) . . ?
F2 C9 S1 110.0(2) . . ?
H18B O18 H18A 92.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4B O12 0.89 2.00 2.854(3) 160.3 .
O4 H4A O18 0.89 2.01 2.883(3) 166.5 .
O3 H3A O18 0.84 1.83 2.655(3) 168.1 .

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.104

# Attachment '6.CIF'

data_c:\xray\finish~1\pympo\znpymp~1\ar458
_database_code_depnum_ccdc_archive 'CCDC 681514'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ((PymPO)Zn(H2O))
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 N4 O8 P2 Zn'
_chemical_formula_weight         419.53

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'
Cl Cl 0.1484 0.1585 '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   Pbca

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

_cell_length_a                   12.5436(14)
_cell_length_b                   7.0918(8)
_cell_length_c                   15.5908(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1386.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    1907
_cell_measurement_theta_min      2.6125
_cell_measurement_theta_max      27.923

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5874
_exptl_absorpt_correction_T_max  0.9798
_exptl_absorpt_process_details   'SADABS: SAINT+, 2001'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(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 1000'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <0.01
_diffrn_reflns_number            8009
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         28.29
_reflns_number_total             1683
_reflns_number_gt                1225
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART v. 5.626'
_computing_cell_refinement       'Bruker SAINT+ v. 6.36a'
_computing_data_reduction        'Bruker SAINT+ v. 6.36a'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'

_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)+(0.0367P)²+1.5917P] 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         1683
_refine_ls_number_parameters     118
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.031
_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 0.5000 0.0000 0.5000 0.01093(14) Uani 1 2 d S . .
P1 P 0.36105(6) 0.25306(10) 0.65525(4) 0.00968(17) Uani 1 1 d . . .
N1 N 0.43133(19) 0.2114(3) 0.40963(15) 0.0140(5) Uani 1 1 d . . .
N2 N 0.36515(19) -0.0209(3) 0.88376(16) 0.0141(5) Uani 1 1 d . . .
O1 O 0.43985(16) 0.1391(3) 0.60618(13) 0.0162(5) Uani 1 1 d . . .
O2 O 0.39177(16) 0.4671(3) 0.64886(13) 0.0137(4) Uani 1 1 d D . .
O3 O 0.24483(16) 0.2279(3) 0.63450(13) 0.0161(5) Uani 1 1 d . . .
O4 O 0.64090(17) 0.1521(3) 0.51276(14) 0.0166(5) Uani 1 1 d D . .
C1 C 0.4174(2) 0.1702(4) 0.32639(18) 0.0134(6) Uani 1 1 d . . .
H1 H 0.4341 0.0481 0.3071 0.016 Uiso 1 1 calc R . .
C2 C 0.3793(2) 0.1987(4) 0.76764(18) 0.0115(6) Uani 1 1 d . . .
C3 C 0.3548(2) 0.0216(4) 0.80067(19) 0.0136(6) Uani 1 1 d . . .
H3 H 0.3299 -0.0720 0.7630 0.016 Uiso 1 1 calc R . .
C4 C 0.4042(2) 0.1155(4) 0.93369(19) 0.0141(6) Uani 1 1 d . . .
H4 H 0.4135 0.0859 0.9920 0.017 Uiso 1 1 calc R . .
H4A H 0.641(3) 0.256(5) 0.550(3) 0.044(12) Uiso 1 1 d D . .
H4B H 0.675(3) 0.192(6) 0.466(2) 0.042(12) Uiso 1 1 d D . .
H2 H 0.340(2) 0.547(4) 0.645(3) 0.041(12) Uiso 1 1 d 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 2.0697(19) 5_656 ?
Zn1 O1 2.0697(19) . ?
Zn1 O4 2.080(2) . ?
Zn1 O4 2.080(2) 5_656 ?
Zn1 N1 2.230(2) 5_656 ?
Zn1 N1 2.230(2) . ?
P1 O1 1.488(2) . ?
P1 O3 1.504(2) . ?
P1 O2 1.569(2) . ?
P1 C2 1.809(3) . ?
N1 C4 1.328(4) 8_565 ?
N1 C1 1.342(4) . ?
N2 C4 1.334(4) . ?
N2 C3 1.336(4) . ?
O2 H2 0.865(10) . ?
O4 H4A 0.94(3) . ?
O4 H4B 0.89(3) . ?
C1 C2 1.390(4) 8_565 ?
C1 H1 0.9400 . ?
C2 C1 1.390(4) 8_566 ?
C2 C3 1.392(4) . ?
C3 H3 0.9400 . ?
C4 N1 1.328(4) 8_566 ?
C4 H4 0.9400 . ?

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 O1 180.00(6) 5_656 . ?
O1 Zn1 O4 90.80(8) 5_656 . ?
O1 Zn1 O4 89.20(8) . . ?
O1 Zn1 O4 89.20(8) 5_656 5_656 ?
O1 Zn1 O4 90.80(8) . 5_656 ?
O4 Zn1 O4 180.0 . 5_656 ?
O1 Zn1 N1 92.52(8) 5_656 5_656 ?
O1 Zn1 N1 87.48(8) . 5_656 ?
O4 Zn1 N1 87.71(8) . 5_656 ?
O4 Zn1 N1 92.29(8) 5_656 5_656 ?
O1 Zn1 N1 87.48(8) 5_656 . ?
O1 Zn1 N1 92.52(8) . . ?
O4 Zn1 N1 92.29(8) . . ?
O4 Zn1 N1 87.71(8) 5_656 . ?
N1 Zn1 N1 180.00(10) 5_656 . ?
O1 P1 O3 117.96(12) . . ?
O1 P1 O2 109.23(12) . . ?
O3 P1 O2 109.83(11) . . ?
O1 P1 C2 107.36(12) . . ?
O3 P1 C2 107.81(12) . . ?
O2 P1 C2 103.67(12) . . ?
C4 N1 C1 116.2(2) 8_565 . ?
C4 N1 Zn1 122.82(19) 8_565 . ?
C1 N1 Zn1 120.97(19) . . ?
C4 N2 C3 116.0(3) . . ?
P1 O1 Zn1 155.80(13) . . ?
P1 O2 H2 117(3) . . ?
Zn1 O4 H4A 118(2) . . ?
Zn1 O4 H4B 120(3) . . ?
H4A O4 H4B 104(4) . . ?
N1 C1 C2 122.4(3) . 8_565 ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 8_565 . ?
C1 C2 C3 115.8(3) 8_566 . ?
C1 C2 P1 122.7(2) 8_566 . ?
C3 C2 P1 121.5(2) . . ?
N2 C3 C2 122.7(3) . . ?
N2 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
N1 C4 N2 126.8(3) 8_566 . ?
N1 C4 H4 116.6 8_566 . ?
N2 C4 H4 116.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Zn1 N1 C4 -159.0(2) 5_656 . . 8_565 ?
O1 Zn1 N1 C4 21.0(2) . . . 8_565 ?
O4 Zn1 N1 C4 -68.3(2) . . . 8_565 ?
O4 Zn1 N1 C4 111.7(2) 5_656 . . 8_565 ?
N1 Zn1 N1 C4 127(100) 5_656 . . 8_565 ?
O1 Zn1 N1 C1 19.5(2) 5_656 . . . ?
O1 Zn1 N1 C1 -160.5(2) . . . . ?
O4 Zn1 N1 C1 110.2(2) . . . . ?
O4 Zn1 N1 C1 -69.8(2) 5_656 . . . ?
N1 Zn1 N1 C1 -55(100) 5_656 . . . ?
O3 P1 O1 Zn1 33.2(4) . . . . ?
O2 P1 O1 Zn1 -93.0(3) . . . . ?
C2 P1 O1 Zn1 155.2(3) . . . . ?
O1 Zn1 O1 P1 4(100) 5_656 . . . ?
O4 Zn1 O1 P1 127.0(3) . . . . ?
O4 Zn1 O1 P1 -53.0(3) 5_656 . . . ?
N1 Zn1 O1 P1 -145.3(3) 5_656 . . . ?
N1 Zn1 O1 P1 34.7(3) . . . . ?
C4 N1 C1 C2 1.5(4) 8_565 . . 8_565 ?
Zn1 N1 C1 C2 -177.1(2) . . . 8_565 ?
O1 P1 C2 C1 112.9(2) . . . 8_566 ?
O3 P1 C2 C1 -119.1(2) . . . 8_566 ?
O2 P1 C2 C1 -2.7(3) . . . 8_566 ?
O1 P1 C2 C3 -67.7(3) . . . . ?
O3 P1 C2 C3 60.4(3) . . . . ?
O2 P1 C2 C3 176.8(2) . . . . ?
C4 N2 C3 C2 -2.2(4) . . . . ?
C1 C2 C3 N2 1.1(4) 8_566 . . . ?
P1 C2 C3 N2 -178.4(2) . . . . ?
C3 N2 C4 N1 1.6(4) . . . 8_566 ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.106


