# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Zheng, Li-Min'

_publ_contact_author_name        'Zheng, Li-Min'
_publ_contact_author_email       lmzheng@netra.nju.edu.cn

_publ_section_title              
;
Three-dimensional Metal Phosphonodicarboxylates with
GIS-zeolite Topology: Syntheses, Structures and Magnetic Studies
;

# Attachment '- Co.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 779797'
#TrackingRef '- Co.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Co4 O25 P2'
_chemical_formula_weight         918.04

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'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/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                   27.543(3)
_cell_length_b                   7.4157(9)
_cell_length_c                   15.8568(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.3880(10)
_cell_angle_gamma                90.00
_cell_volume                     2704.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    5966
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      28.1815

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    2.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6925
_exptl_absorpt_correction_T_max  0.7779
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6994
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2644
_reflns_number_gt                2499
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0696P)^2^+5.6849P] where P=(Fo^2^+2Fc^2^)/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         2644
_refine_ls_number_parameters     213
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.1029
_refine_ls_wR_factor_gt          0.1013
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.055
_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
Co1 Co 0.194085(14) 0.39468(5) 0.19352(3) 0.01471(14) Uani 1 1 d . . .
Co2 Co 0.159731(15) 0.45812(5) 0.35187(3) 0.01778(15) Uani 1 1 d U . .
P1 P 0.32715(3) 0.30097(9) 0.26660(5) 0.01290(18) Uani 1 1 d . . .
O1 O 0.33496(9) 0.4154(3) 0.19561(14) 0.0184(4) Uani 1 1 d . . .
O2 O 0.28262(8) 0.3818(3) 0.28444(14) 0.0172(4) Uani 1 1 d . . .
O3 O 0.31321(8) 0.1046(3) 0.22884(14) 0.0155(4) Uani 1 1 d . . .
O4 O 0.57924(9) 0.1093(4) 0.72091(16) 0.0299(5) Uani 1 1 d . . .
O5 O 0.60896(9) 0.1755(3) 0.61876(15) 0.0252(5) Uani 1 1 d . . .
O6 O 0.36296(10) 0.1974(3) 0.56860(15) 0.0248(5) Uani 1 1 d . . .
O7 O 0.31433(8) 0.0676(3) 0.41795(15) 0.0196(4) Uani 1 1 d . . .
O1W O 0.20117(8) 0.2448(3) 0.32149(14) 0.0182(4) Uani 1 1 d . . .
H1WA H 0.2361 0.2260 0.3700 0.022 Uiso 1 1 d R . .
H1WB H 0.1819 0.1470 0.3034 0.022 Uiso 1 1 d R . .
O2W O 0.19141(9) 0.1797(3) 0.09597(16) 0.0258(5) Uani 1 1 d . . .
H2WB H 0.1605 0.1887 0.0374 0.031 Uiso 1 1 d R . .
H2WA H 0.1924 0.0813 0.1205 0.039 Uiso 1 1 d R . .
O3W O 0.24136(10) 0.5345(4) 0.47544(16) 0.0351(6) Uani 1 1 d . . .
H3WB H 0.2675 0.5003 0.4661 0.042 Uiso 1 1 d R . .
H3WA H 0.2468 0.4878 0.5268 0.042 Uiso 1 1 d R . .
O4W O 0.12321(10) 0.6866(3) 0.38042(18) 0.0333(5) Uani 1 1 d U . .
H4WB H 0.1055 0.7498 0.3278 0.040 Uiso 1 1 d R . .
H4WA H 0.1000 0.6528 0.3955 0.040 Uiso 1 1 d R . .
O5W O 0.5000 0.8504(9) 0.7500 0.0697(15) Uani 1 2 d S . .
H5WD H 0.5218 0.9149 0.7412 0.084 Uiso 0.50 1 d PR . .
H5WC H 0.4951 0.7498 0.7220 0.084 Uiso 0.50 1 d PR . .
O6W O 0.0473(5) 0.0291(12) 0.3052(8) 0.249(7) Uani 1 1 d . . .
H6WA H 0.0670 0.0663 0.3659 0.298 Uiso 1 1 d R . .
H6WB H 0.0615 0.1031 0.2848 0.298 Uiso 1 1 d R . .
C1 C 0.51029(12) 0.2134(4) 0.5536(2) 0.0187(6) Uani 1 1 d . . .
C2 C 0.46218(12) 0.1813(4) 0.5584(2) 0.0189(6) Uani 1 1 d . . .
H2 H 0.4676 0.1387 0.6182 0.023 Uiso 1 1 calc R . .
C3 C 0.40584(11) 0.2115(4) 0.4752(2) 0.0156(5) Uani 1 1 d . . .
C4 C 0.39710(11) 0.2848(4) 0.38628(19) 0.0146(5) Uani 1 1 d . . .
C5 C 0.44594(12) 0.3291(4) 0.3852(2) 0.0211(6) Uani 1 1 d . . .
H5 H 0.4410 0.3852 0.3285 0.025 Uiso 1 1 calc R . .
C6 C 0.50174(12) 0.2912(4) 0.4668(2) 0.0227(6) Uani 1 1 d . . .
H6 H 0.5336 0.3180 0.4633 0.027 Uiso 1 1 calc R . .
C7 C 0.57084(12) 0.1632(4) 0.6386(2) 0.0189(6) Uani 1 1 d . . .
C8 C 0.35717(12) 0.1548(4) 0.4870(2) 0.0166(5) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0107(2) 0.0184(2) 0.0148(2) -0.00052(13) 0.00688(17) 0.00020(13)
Co2 0.0154(2) 0.0240(3) 0.0157(2) -0.00128(14) 0.00970(18) -0.00343(14)
P1 0.0103(3) 0.0151(4) 0.0125(3) 0.0013(2) 0.0057(3) 0.0015(2)
O1 0.0200(10) 0.0180(10) 0.0180(9) 0.0044(8) 0.0110(8) 0.0025(8)
O2 0.0115(9) 0.0205(10) 0.0191(9) -0.0017(7) 0.0081(8) 0.0013(7)
O3 0.0144(9) 0.0178(10) 0.0147(9) 0.0007(7) 0.0083(8) 0.0007(7)
O4 0.0155(10) 0.0543(16) 0.0174(10) 0.0084(10) 0.0075(9) 0.0092(10)
O5 0.0135(9) 0.0387(13) 0.0232(10) 0.0084(9) 0.0099(8) 0.0060(9)
O6 0.0276(11) 0.0328(12) 0.0202(10) -0.0065(9) 0.0171(9) -0.0097(9)
O7 0.0150(9) 0.0268(10) 0.0175(9) -0.0035(8) 0.0092(8) -0.0048(8)
O1W 0.0144(9) 0.0170(10) 0.0202(10) 0.0008(8) 0.0077(8) -0.0014(7)
O2W 0.0218(10) 0.0274(11) 0.0221(10) 0.0003(8) 0.0083(9) 0.0055(9)
O3W 0.0274(12) 0.0585(18) 0.0186(11) -0.0036(10) 0.0121(10) -0.0114(11)
O4W 0.0324(13) 0.0410(13) 0.0339(12) 0.0098(10) 0.0228(11) 0.0081(10)
O5W 0.041(2) 0.111(4) 0.052(3) 0.000 0.022(2) 0.000
O6W 0.403(17) 0.149(7) 0.374(17) -0.140(9) 0.328(17) -0.112(8)
C1 0.0139(13) 0.0213(14) 0.0179(13) -0.0024(11) 0.0070(11) -0.0001(10)
C2 0.0163(13) 0.0244(15) 0.0153(12) 0.0010(11) 0.0082(11) -0.0010(11)
C3 0.0144(12) 0.0171(13) 0.0155(12) -0.0020(10) 0.0083(11) -0.0009(10)
C4 0.0110(12) 0.0163(13) 0.0145(12) 0.0002(10) 0.0057(10) 0.0012(10)
C5 0.0162(13) 0.0298(16) 0.0185(13) 0.0039(12) 0.0103(11) -0.0014(11)
C6 0.0128(13) 0.0328(17) 0.0238(14) 0.0033(12) 0.0109(12) -0.0020(11)
C7 0.0122(13) 0.0247(15) 0.0176(13) -0.0003(11) 0.0069(11) 0.0017(11)
C8 0.0148(13) 0.0194(13) 0.0154(12) 0.0029(10) 0.0081(11) 0.0007(10)

_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
Co1 O5 2.028(2) 8_455 ?
Co1 O2 2.0407(19) . ?
Co1 O3 2.0620(19) 4 ?
Co1 O7 2.091(2) 4 ?
Co1 O2W 2.194(2) . ?
Co1 O1W 2.2259(19) . ?
Co2 O6 2.044(2) 7_556 ?
Co2 O3W 2.090(2) . ?
Co2 O4 2.100(2) 8_455 ?
Co2 O3 2.103(2) 4 ?
Co2 O4W 2.142(2) . ?
Co2 O1W 2.154(2) . ?
P1 O1 1.517(2) . ?
P1 O2 1.5251(19) . ?
P1 O3 1.541(2) . ?
P1 C4 1.818(3) . ?
O3 Co1 2.0620(19) 4_545 ?
O3 Co2 2.1030(19) 4_545 ?
O4 C7 1.259(4) . ?
O4 Co2 2.100(2) 8_556 ?
O5 C7 1.254(3) . ?
O5 Co1 2.028(2) 8_556 ?
O6 C8 1.254(3) . ?
O6 Co2 2.044(2) 7_556 ?
O7 C8 1.260(4) . ?
O7 Co1 2.091(2) 4_545 ?
O1W H1WA 0.8492 . ?
O1W H1WB 0.8503 . ?
O2W H2WB 0.8494 . ?
O2W H2WA 0.8201 . ?
O3W H3WB 0.8507 . ?
O3W H3WA 0.8196 . ?
O4W H4WB 0.8399 . ?
O4W H4WA 0.8345 . ?
O5W H5WD 0.8364 . ?
O5W H5WC 0.8404 . ?
O6W H6WA 0.8500 . ?
O6W H6WB 0.8367 . ?
C1 C2 1.388(4) . ?
C1 C6 1.388(4) . ?
C1 C7 1.504(4) . ?
C2 C3 1.395(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.403(4) . ?
C3 C8 1.512(4) . ?
C4 C5 1.394(4) . ?
C5 C6 1.388(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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 Co1 O2 161.50(9) 8_455 . ?
O5 Co1 O3 94.68(8) 8_455 4 ?
O2 Co1 O3 94.86(8) . 4 ?
O5 Co1 O7 96.24(9) 8_455 4 ?
O2 Co1 O7 99.17(8) . 4 ?
O3 Co1 O7 92.28(8) 4 4 ?
O5 Co1 O2W 79.74(8) 8_455 . ?
O2 Co1 O2W 91.58(8) . . ?
O3 Co1 O2W 173.20(8) 4 . ?
O7 Co1 O2W 84.52(9) 4 . ?
O5 Co1 O1W 84.14(8) 8_455 . ?
O2 Co1 O1W 82.03(8) . . ?
O3 Co1 O1W 79.69(7) 4 . ?
O7 Co1 O1W 171.96(8) 4 . ?
O2W Co1 O1W 103.42(8) . . ?
O6 Co2 O3W 96.37(9) 7_556 . ?
O6 Co2 O4 87.76(9) 7_556 8_455 ?
O3W Co2 O4 175.84(9) . 8_455 ?
O6 Co2 O3 176.26(8) 7_556 4 ?
O3W Co2 O3 82.64(8) . 4 ?
O4 Co2 O3 93.21(8) 8_455 4 ?
O6 Co2 O4W 88.71(9) 7_556 . ?
O3W Co2 O4W 88.59(10) . . ?
O4 Co2 O4W 91.97(10) 8_455 . ?
O3 Co2 O4W 94.87(8) 4 . ?
O6 Co2 O1W 95.92(8) 7_556 . ?
O3W Co2 O1W 88.83(9) . . ?
O4 Co2 O1W 90.29(8) 8_455 . ?
O3 Co2 O1W 80.47(7) 4 . ?
O4W Co2 O1W 174.93(8) . . ?
O1 P1 O2 112.01(11) . . ?
O1 P1 O3 110.33(11) . . ?
O2 P1 O3 112.94(11) . . ?
O1 P1 C4 108.06(12) . . ?
O2 P1 C4 109.32(11) . . ?
O3 P1 C4 103.75(12) . . ?
P1 O2 Co1 131.12(12) . . ?
P1 O3 Co1 124.53(11) . 4_545 ?
P1 O3 Co2 128.96(12) . 4_545 ?
Co1 O3 Co2 99.03(8) 4_545 4_545 ?
C7 O4 Co2 126.34(19) . 8_556 ?
C7 O5 Co1 133.82(19) . 8_556 ?
C8 O6 Co2 125.9(2) . 7_556 ?
C8 O7 Co1 131.65(19) . 4_545 ?
Co2 O1W Co1 92.63(7) . . ?
Co2 O1W H1WA 113.1 . . ?
Co1 O1W H1WA 113.3 . . ?
Co2 O1W H1WB 113.1 . . ?
Co1 O1W H1WB 113.2 . . ?
H1WA O1W H1WB 110.5 . . ?
Co1 O2W H2WB 109.7 . . ?
Co1 O2W H2WA 109.4 . . ?
H2WB O2W H2WA 109.8 . . ?
Co2 O3W H3WB 109.5 . . ?
Co2 O3W H3WA 109.4 . . ?
H3WB O3W H3WA 109.7 . . ?
Co2 O4W H4WB 108.4 . . ?
Co2 O4W H4WA 110.2 . . ?
H4WB O4W H4WA 109.5 . . ?
H5WD O5W H5WC 110.0 . . ?
H6WA O6W H6WB 94.7 . . ?
C2 C1 C6 118.6(3) . . ?
C2 C1 C7 122.0(3) . . ?
C6 C1 C7 119.4(2) . . ?
C1 C2 C3 121.3(3) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C2 C3 C4 119.9(2) . . ?
C2 C3 C8 116.0(2) . . ?
C4 C3 C8 124.0(2) . . ?
C5 C4 C3 118.1(2) . . ?
C5 C4 P1 116.6(2) . . ?
C3 C4 P1 124.9(2) . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C1 C6 C5 120.4(3) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O5 C7 O4 125.6(3) . . ?
O5 C7 C1 115.2(2) . . ?
O4 C7 C1 119.2(2) . . ?
O6 C8 O7 123.5(3) . . ?
O6 C8 C3 116.1(2) . . ?
O7 C8 C3 120.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.121