# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Jonna Jokiniemi'
_publ_contact_author_email       JONNA.JOKINIEMI@JOENSUU.FI

_publ_section_title              
;
Synthesis of phenyl substituted bisphosphonates and
crystal structures and characterization of Cd complexes of
(dichloromethylene)bisphosphonic acid phenyl and alkyl ester derivatives
;
loop_
_publ_author_name
'Jonna Jokiniemi'
'Markku J Ahlgren'
'Harri Natkinniemi'
'Sirpa Peraniemi'
;
J.J.Vepsalainen
;

# Attachment 'Jokiniemi.cif'

data_I
_database_code_depnum_ccdc_archive 'CCDC 719961'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H24 Cd3 Cl4 O18 P4, 2H2O'
_chemical_formula_sum            'C15 H28 Cd3 Cl4 O20 P4'
_chemical_formula_weight         1131.25

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.6807(1)
_cell_length_b                   13.2318(2)
_cell_length_c                   19.3270(3)
_cell_angle_alpha                100.308(1)
_cell_angle_beta                 95.579(1)
_cell_angle_gamma                96.954(1)
_cell_volume                     1656.11(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    28696
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      26.00

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100
_exptl_absorpt_coefficient_mu    2.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4744
_exptl_absorpt_correction_T_max  0.8850
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker AXS, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28696
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6455
_reflns_number_gt                5912
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-200)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond v.3.0 (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0137P)²+3.6165P] 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         6455
_refine_ls_number_parameters     428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0197
_refine_ls_wR_factor_ref         0.0476
_refine_ls_wR_factor_gt          0.0461
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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
Cd1 Cd 0.5000 0.0000 0.0000 0.00975(6) Uani 1 2 d S . .
Cd2 Cd 0.02345(2) -0.125026(15) 0.179877(9) 0.00838(5) Uani 1 1 d . . .
Cd3 Cd 0.44205(3) 0.029624(15) 0.293786(9) 0.00941(5) Uani 1 1 d . . .
Cd4 Cd 0.0000 0.0000 0.5000 0.00870(6) Uani 1 2 d S . .
Cl1 Cl 0.57451(9) -0.29325(5) 0.01957(3) 0.01303(13) Uani 1 1 d . . .
Cl2 Cl 0.28187(9) -0.34526(5) 0.11445(3) 0.01399(13) Uani 1 1 d . . .
Cl3 Cl -0.11357(9) 0.25118(5) 0.40937(3) 0.01544(14) Uani 1 1 d . . .
Cl4 Cl 0.16287(9) 0.24178(5) 0.30200(3) 0.01482(13) Uani 1 1 d . . .
P1 P 0.18247(9) -0.20936(5) 0.01433(3) 0.00909(13) Uani 1 1 d . . .
P2 P 0.51930(9) -0.13437(5) 0.14244(3) 0.00736(13) Uani 1 1 d . . .
P3 P 0.28673(9) 0.18424(5) 0.43902(3) 0.00907(13) Uani 1 1 d . . .
P4 P -0.05342(9) 0.04644(5) 0.32797(3) 0.00783(13) Uani 1 1 d . . .
O1 O 0.2317(3) 0.08173(16) 0.03699(10) 0.0164(4) Uani 1 1 d . . .
H1A H 0.1700 0.1113 0.0074 0.025 Uiso 1 1 d R . .
H1B H 0.1516 0.0642 0.0657 0.025 Uiso 1 1 d R . .
O2 O 0.0733(3) -0.24558(15) 0.25051(10) 0.0152(4) Uani 1 1 d . . .
H2A H 0.1940 -0.2594 0.2559 0.023 Uiso 1 1 d R . .
H2B H 0.0306 -0.2298 0.2904 0.023 Uiso 1 1 d R . .
O3 O -0.0154(3) 0.03594(15) 0.14263(9) 0.0143(4) Uani 1 1 d . . .
H3A H 0.0121 0.0826 0.1800 0.022 Uiso 1 1 d R . .
H3B H -0.1421 0.0356 0.1328 0.022 Uiso 1 1 d R . .
O4 O 0.4984(3) -0.09368(15) 0.36367(9) 0.0131(4) Uani 1 1 d . . .
H4A H 0.5005 -0.1582 0.3497 0.020 Uiso 1 1 d R . .
H4B H 0.6040 -0.0699 0.3930 0.020 Uiso 1 1 d R . .
O5 O 0.4187(3) 0.11700(15) 0.19795(9) 0.0143(4) Uani 1 1 d . . .
H5 H 0.4091 0.0797 0.1568 0.021 Uiso 1 1 d R . .
O6 O 0.2716(3) -0.09219(15) 0.47759(9) 0.0146(4) Uani 1 1 d . . .
H6A H 0.3510 -0.0807 0.4469 0.022 Uiso 1 1 d R . .
H6B H 0.3507 -0.0940 0.5145 0.022 Uiso 1 1 d R . .
O7 O 0.5219(3) -0.27363(17) 0.27871(10) 0.0218(4) Uani 1 1 d . . .
H7A H 0.5174 -0.3392 0.2710 0.033 Uiso 1 1 d R . .
H7B H 0.5852 -0.2509 0.2473 0.033 Uiso 1 1 d R . .
O8 O -0.1090(7) -0.2775(4) 0.3705(2) 0.0199(10) Uani 0.55 1 d P . .
H8A H -0.1303 -0.2457 0.4108 0.030 Uiso 0.55 1 d PR . .
H8B H -0.2198 -0.2735 0.3458 0.030 Uiso 0.55 1 d PR . .
O8' O -0.0064(9) -0.2592(5) 0.3829(3) 0.0230(13) Uani 0.45 1 d P . .
H8A' H -0.1193 -0.2645 0.3996 0.035 Uiso 0.45 1 d PR . .
H8B' H 0.0791 -0.2177 0.4136 0.035 Uiso 0.45 1 d PR . .
O31 O 0.2061(3) 0.15403(14) 0.50323(9) 0.0107(4) Uani 1 1 d . . .
O11 O 0.2762(3) -0.14884(15) -0.03532(9) 0.0119(4) Uani 1 1 d . . .
O12 O 0.0431(3) -0.16026(15) 0.06197(9) 0.0125(4) Uani 1 1 d . . .
O13 O 0.0544(3) -0.31587(15) -0.02657(9) 0.0133(4) Uani 1 1 d . . .
O21 O 0.5782(3) -0.04501(14) 0.10552(9) 0.0100(4) Uani 1 1 d . . .
O22 O 0.3661(2) -0.10817(14) 0.19414(9) 0.0095(4) Uani 1 1 d . . .
O23 O 0.6973(2) -0.17540(14) 0.17745(9) 0.0102(4) Uani 1 1 d . . .
O32 O 0.4351(3) 0.12157(15) 0.40496(9) 0.0135(4) Uani 1 1 d . . .
O33 O 0.3811(3) 0.30318(15) 0.45488(10) 0.0180(4) Uani 1 1 d . . .
O41 O -0.1059(3) -0.00719(15) 0.38818(9) 0.0111(4) Uani 1 1 d . . .
O42 O 0.1038(2) -0.00162(14) 0.28564(9) 0.0105(4) Uani 1 1 d . . .
O43 O -0.2362(2) 0.05995(15) 0.28025(9) 0.0114(4) Uani 1 1 d . . .
C1 C 0.3884(4) -0.2447(2) 0.07226(13) 0.0097(5) Uani 1 1 d . . .
C2 C 0.0714(4) 0.1802(2) 0.37035(13) 0.0098(5) Uani 1 1 d . . .
C5 C 0.5404(5) 0.2140(3) 0.19677(18) 0.0312(8) Uani 1 1 d . . .
H5A H 0.4966 0.2697 0.2300 0.047 Uiso 1 1 calc R . .
H5B H 0.5239 0.2290 0.1488 0.047 Uiso 1 1 calc R . .
H5C H 0.6836 0.2095 0.2106 0.047 Uiso 1 1 calc R . .
C11 C 0.0980(4) -0.3790(2) -0.08826(14) 0.0138(6) Uani 1 1 d . . .
C12 C 0.0479(5) -0.3530(2) -0.15296(15) 0.0219(6) Uani 1 1 d . . .
H12 H -0.0071 -0.2907 -0.1559 0.026 Uiso 1 1 calc R . .
C13 C 0.0795(5) -0.4201(3) -0.21408(16) 0.0270(7) Uani 1 1 d . . .
H13 H 0.0464 -0.4035 -0.2593 0.032 Uiso 1 1 calc R . .
C14 C 0.1589(5) -0.5104(2) -0.20912(16) 0.0254(7) Uani 1 1 d . . .
H14 H 0.1822 -0.5552 -0.2509 0.030 Uiso 1 1 calc R . .
C15 C 0.2047(4) -0.5360(2) -0.14356(15) 0.0207(6) Uani 1 1 d . . .
H15 H 0.2581 -0.5986 -0.1404 0.025 Uiso 1 1 calc R . .
C16 C 0.1727(4) -0.4700(2) -0.08238(15) 0.0181(6) Uani 1 1 d . . .
H16 H 0.2019 -0.4874 -0.0372 0.022 Uiso 1 1 calc R . .
C21 C 0.4243(4) 0.3674(2) 0.52213(14) 0.0165(6) Uani 1 1 d . . .
C22 C 0.6003(5) 0.3632(3) 0.56380(16) 0.0263(7) Uani 1 1 d . . .
H22 H 0.6876 0.3145 0.5481 0.032 Uiso 1 1 calc R . .
C23 C 0.6503(6) 0.4294(3) 0.62838(17) 0.0394(9) Uani 1 1 d . . .
H23 H 0.7716 0.4260 0.6574 0.047 Uiso 1 1 calc R . .
C24 C 0.5261(7) 0.5001(3) 0.65086(19) 0.0448(11) Uani 1 1 d . . .
H24 H 0.5614 0.5459 0.6953 0.054 Uiso 1 1 calc R . .
C25 C 0.3499(8) 0.5048(3) 0.6091(2) 0.0519(12) Uani 1 1 d . . .
H25 H 0.2639 0.5542 0.6249 0.062 Uiso 1 1 calc R . .
C26 C 0.2957(6) 0.4371(3) 0.5430(2) 0.0336(8) Uani 1 1 d . . .
H26 H 0.1741 0.4397 0.5139 0.040 Uiso 1 1 calc R . .


_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
Cd1 O21 2.2560(17) . ?
Cd1 O21 2.2560(17) 2_655 ?
Cd1 O11 2.2775(18) 2_655 ?
Cd1 O11 2.2775(18) . ?
Cd1 O1 2.3099(18) . ?
Cd1 O1 2.3099(18) 2_655 ?
Cd2 O23 2.1932(16) 1_455 ?
Cd2 O22 2.2580(16) . ?
Cd2 O12 2.2629(17) . ?
Cd2 O2 2.3106(18) . ?
Cd2 O42 2.3480(17) . ?
Cd2 O3 2.4017(19) . ?
Cd3 O43 2.1882(17) 1_655 ?
Cd3 O42 2.2324(16) . ?
Cd3 O32 2.2796(18) . ?
Cd3 O4 2.3381(18) . ?
Cd3 O5 2.3550(18) . ?
Cd3 O22 2.3707(17) . ?
Cd4 O41 2.1892(17) 2_556 ?
Cd4 O41 2.1892(17) . ?
Cd4 O31 2.3046(18) 2_556 ?
Cd4 O31 2.3046(18) . ?
Cd4 O6 2.3380(18) . ?
Cd4 O6 2.3380(18) 2_556 ?
Cl1 C1 1.789(2) . ?
Cl2 C1 1.793(3) . ?
Cl3 C2 1.785(3) . ?
Cl4 C2 1.790(3) . ?
P1 O11 1.4916(19) . ?
P1 O12 1.4952(18) . ?
P1 O13 1.5878(19) . ?
P1 C1 1.846(3) . ?
P2 O23 1.5160(17) . ?
P2 O21 1.5185(19) . ?
P2 O22 1.5253(17) . ?
P2 C1 1.867(3) . ?
P3 O32 1.4946(19) . ?
P3 O31 1.4986(18) . ?
P3 O33 1.587(2) . ?
P3 C2 1.849(2) . ?
P4 O43 1.5054(17) . ?
P4 O41 1.5150(18) . ?
P4 O42 1.5229(18) . ?
P4 C2 1.868(3) . ?
O1 H1A 0.8502 . ?
O1 H1B 0.8503 . ?
O2 H2A 0.8488 . ?
O2 H2B 0.8484 . ?
O3 H3A 0.8508 . ?
O3 H3B 0.8488 . ?
O4 H4A 0.8501 . ?
O4 H4B 0.8500 . ?
O5 C5 1.439(4) . ?
O5 H5 0.8499 . ?
O6 H6A 0.8542 . ?
O6 H6B 0.8516 . ?
O7 H7A 0.8500 . ?
O7 H7B 0.8499 . ?
O8 H8A 0.8497 . ?
O8 H8B 0.8533 . ?
O8 H8A' 0.5722 . ?
O8' H8A 1.0468 . ?
O8' H8A' 0.8495 . ?
O8' H8B' 0.8501 . ?
O13 C11 1.405(3) . ?
O23 Cd2 2.1932(16) 1_655 ?
O33 C21 1.402(3) . ?
O43 Cd3 2.1882(16) 1_455 ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C11 C16 1.376(4) . ?
C11 C12 1.377(4) . ?
C12 C13 1.395(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.370(4) . ?
C21 C22 1.372(4) . ?
C22 C23 1.376(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.365(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.376(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.409(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

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
O21 Cd1 O21 180.00(12) . 2_655 ?
O21 Cd1 O11 89.93(6) . 2_655 ?
O21 Cd1 O11 90.07(6) 2_655 2_655 ?
O21 Cd1 O11 90.07(6) . . ?
O21 Cd1 O11 89.93(6) 2_655 . ?
O11 Cd1 O11 180.00(12) 2_655 . ?
O21 Cd1 O1 93.51(6) . . ?
O21 Cd1 O1 86.49(6) 2_655 . ?
O11 Cd1 O1 92.18(7) 2_655 . ?
O11 Cd1 O1 87.82(7) . . ?
O21 Cd1 O1 86.49(6) . 2_655 ?
O21 Cd1 O1 93.51(6) 2_655 2_655 ?
O11 Cd1 O1 87.82(7) 2_655 2_655 ?
O11 Cd1 O1 92.18(7) . 2_655 ?
O1 Cd1 O1 180.00(14) . 2_655 ?
O23 Cd2 O22 165.85(7) 1_455 . ?
O23 Cd2 O12 98.56(6) 1_455 . ?
O22 Cd2 O12 86.50(6) . . ?
O23 Cd2 O2 86.39(6) 1_455 . ?
O22 Cd2 O2 79.75(6) . . ?
O12 Cd2 O2 121.86(7) . . ?
O23 Cd2 O42 103.32(6) 1_455 . ?
O22 Cd2 O42 78.49(6) . . ?
O12 Cd2 O42 146.21(7) . . ?
O2 Cd2 O42 85.25(7) . . ?
O23 Cd2 O3 95.47(6) 1_455 . ?
O22 Cd2 O3 98.59(6) . . ?
O12 Cd2 O3 75.89(7) . . ?
O2 Cd2 O3 161.77(7) . . ?
O42 Cd2 O3 76.67(6) . . ?
O43 Cd3 O42 169.14(6) 1_655 . ?
O43 Cd3 O32 101.99(6) 1_655 . ?
O42 Cd3 O32 87.08(6) . . ?
O43 Cd3 O4 92.67(6) 1_655 . ?
O42 Cd3 O4 95.06(6) . . ?
O32 Cd3 O4 78.14(7) . . ?
O43 Cd3 O5 80.05(6) 1_655 . ?
O42 Cd3 O5 90.43(6) . . ?
O32 Cd3 O5 118.40(7) . . ?
O4 Cd3 O5 162.89(7) . . ?
O43 Cd3 O22 94.16(6) 1_655 . ?
O42 Cd3 O22 78.51(6) . . ?
O32 Cd3 O22 159.16(6) . . ?
O4 Cd3 O22 88.13(6) . . ?
O5 Cd3 O22 77.08(6) . . ?
O41 Cd4 O41 180.0 2_556 . ?
O41 Cd4 O31 90.33(6) 2_556 2_556 ?
O41 Cd4 O31 89.67(6) . 2_556 ?
O41 Cd4 O31 89.67(6) 2_556 . ?
O41 Cd4 O31 90.33(6) . . ?
O31 Cd4 O31 180.00(5) 2_556 . ?
O41 Cd4 O6 85.04(6) 2_556 . ?
O41 Cd4 O6 94.96(6) . . ?
O31 Cd4 O6 89.56(6) 2_556 . ?
O31 Cd4 O6 90.44(6) . . ?
O41 Cd4 O6 94.96(6) 2_556 2_556 ?
O41 Cd4 O6 85.04(6) . 2_556 ?
O31 Cd4 O6 90.44(6) 2_556 2_556 ?
O31 Cd4 O6 89.56(6) . 2_556 ?
O6 Cd4 O6 180.0 . 2_556 ?
O11 P1 O12 118.63(11) . . ?
O11 P1 O13 111.73(10) . . ?
O12 P1 O13 104.86(10) . . ?
O11 P1 C1 108.32(11) . . ?
O12 P1 C1 106.63(11) . . ?
O13 P1 C1 105.88(11) . . ?
O23 P2 O21 114.57(10) . . ?
O23 P2 O22 111.29(10) . . ?
O21 P2 O22 111.58(10) . . ?
O23 P2 C1 105.43(11) . . ?
O21 P2 C1 106.71(11) . . ?
O22 P2 C1 106.64(10) . . ?
O32 P3 O31 117.74(11) . . ?
O32 P3 O33 108.85(11) . . ?
O31 P3 O33 110.76(10) . . ?
O32 P3 C2 107.12(11) . . ?
O31 P3 C2 109.01(11) . . ?
O33 P3 C2 102.17(11) . . ?
O43 P4 O41 113.71(10) . . ?
O43 P4 O42 111.50(10) . . ?
O41 P4 O42 113.60(11) . . ?
O43 P4 C2 106.01(11) . . ?
O41 P4 C2 105.98(11) . . ?
O42 P4 C2 105.20(11) . . ?
Cd1 O1 H1A 116.7 . . ?
Cd1 O1 H1B 127.0 . . ?
H1A O1 H1B 109.7 . . ?
Cd2 O2 H2A 115.0 . . ?
Cd2 O2 H2B 112.3 . . ?
H2A O2 H2B 110.4 . . ?
Cd2 O3 H3A 105.8 . . ?
Cd2 O3 H3B 106.3 . . ?
H3A O3 H3B 101.8 . . ?
Cd3 O4 H4A 127.6 . . ?
Cd3 O4 H4B 108.1 . . ?
H4A O4 H4B 107.7 . . ?
C5 O5 Cd3 123.82(17) . . ?
C5 O5 H5 107.4 . . ?
Cd3 O5 H5 116.4 . . ?
Cd4 O6 H6A 123.0 . . ?
Cd4 O6 H6B 114.1 . . ?
H6A O6 H6B 104.6 . . ?
H7A O7 H7B 107.7 . . ?
H8A O8 H8B 100.0 . . ?
H8B O8 H8A' 107.4 . . ?
H8A O8' H8B' 94.2 . . ?
H8A' O8' H8B' 107.7 . . ?
P3 O31 Cd4 123.19(10) . . ?
P1 O11 Cd1 124.06(10) . . ?
P1 O12 Cd2 136.70(10) . . ?
C11 O13 P1 126.85(16) . . ?
P2 O21 Cd1 138.10(10) . . ?
P2 O22 Cd2 132.13(10) . . ?
P2 O22 Cd3 122.42(9) . . ?
Cd2 O22 Cd3 100.45(6) . . ?
P2 O23 Cd2 128.80(10) . 1_655 ?
P3 O32 Cd3 134.03(10) . . ?
C21 O33 P3 125.65(17) . . ?
P4 O41 Cd4 139.25(11) . . ?
P4 O42 Cd3 133.62(10) . . ?
P4 O42 Cd2 124.15(9) . . ?
Cd3 O42 Cd2 101.91(7) . . ?
P4 O43 Cd3 128.76(10) . 1_455 ?
Cl1 C1 Cl2 108.79(14) . . ?
Cl1 C1 P1 109.31(13) . . ?
Cl2 C1 P1 108.32(12) . . ?
Cl1 C1 P2 108.13(12) . . ?
Cl2 C1 P2 108.42(13) . . ?
P1 C1 P2 113.77(14) . . ?
Cl3 C2 Cl4 108.72(14) . . ?
Cl3 C2 P3 108.71(13) . . ?
Cl4 C2 P3 108.52(13) . . ?
Cl3 C2 P4 108.91(13) . . ?
Cl4 C2 P4 107.65(13) . . ?
P3 C2 P4 114.22(14) . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C16 C11 C12 122.1(3) . . ?
C16 C11 O13 118.5(2) . . ?
C12 C11 O13 119.2(3) . . ?
C11 C12 C13 118.5(3) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.3(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C11 C16 C15 118.9(3) . . ?
C11 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C26 C21 C22 121.5(3) . . ?
C26 C21 O33 119.2(3) . . ?
C22 C21 O33 119.2(3) . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.2(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.0(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.5(4) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C25 117.8(4) . . ?
C21 C26 H26 121.1 . . ?
C25 C26 H26 121.1 . . ?

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
O5 H5 O21 0.85 2.25 2.911(3) 134.7 .
O1 H1A O12 0.85 2.10 2.932(3) 166.2 2
O1 H1B O3 0.85 2.00 2.849(3) 173.0 .
O2 H2A O7 0.85 2.23 3.072(3) 172.2 .
O2 H2B O8 0.85 2.04 2.796(5) 148.4 .
O2 H2B O8' 0.85 1.93 2.696(6) 149.9 .
O3 H3B O21 0.85 2.01 2.771(2) 149.1 1_455
O4 H4A O7 0.85 1.89 2.670(3) 151.6 .
O4 H4B O41 0.85 2.03 2.712(2) 136.4 1_655
O6 H6A O4 0.85 1.96 2.790(2) 163.9 .
O6 H6B O32 0.85 2.12 2.963(2) 169.7 2_656
O7 H7B O23 0.85 1.97 2.807(3) 168.3 .
O8 H8A' O31 0.57 2.33 2.861(5) 155.4 2_556
O8 H8B O7 0.85 2.06 2.906(5) 174.5 1_455
O8' H8B' O6 0.85 2.09 2.929(6) 168.0 .

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.090

#===END===============================================================

data_II
_database_code_depnum_ccdc_archive 'CCDC 719962'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H16 Cd Cl2 O9 P2, H2O'
_chemical_formula_sum            'C13 H18 Cd Cl2 O10 P2'
_chemical_formula_weight         579.51

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   5.8432(1)
_cell_length_b                   9.2266(2)
_cell_length_c                   18.6853(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.103(1)
_cell_angle_gamma                90.00
_cell_volume                     1007.19(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    14021
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      26.00

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6969
_exptl_absorpt_correction_T_max  0.9262
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14021
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3935
_reflns_number_gt                3879
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius,1997-200)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond v.3.0 (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0200P)²+0.9000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.050(15)
_refine_ls_number_reflns         3935
_refine_ls_number_parameters     253
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0502
_refine_ls_wR_factor_gt          0.0499
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Cd1 Cd 0.78718(3) 0.22732(2) 0.517634(9) 0.00931(6) Uani 1 1 d . . .
Cl1 Cl 0.65639(11) 0.47742(7) 0.68228(4) 0.01396(14) Uani 1 1 d . . .
Cl2 Cl 0.19854(11) 0.59982(7) 0.69261(3) 0.01305(13) Uani 1 1 d . . .
P1 P 0.29875(11) 0.40286(7) 0.57195(3) 0.00831(14) Uani 1 1 d . . .
P2 P 0.27613(12) 0.29948(8) 0.73160(4) 0.01068(14) Uani 1 1 d . . .
O1 O 0.9248(3) 0.0794(2) 0.60849(11) 0.0135(4) Uani 1 1 d . . .
H1A H 0.8350 0.0065 0.6061 0.020 Uiso 1 1 d R . .
H1B H 0.9301 0.1318 0.6456 0.020 Uiso 1 1 d R . .
O2 O 1.1102(3) 0.1628(2) 0.45269(10) 0.0118(4) Uani 1 1 d . . .
H2A H 1.1100 0.0707 0.4491 0.018 Uiso 1 1 d R . .
H2B H 1.2243 0.1899 0.4784 0.018 Uiso 1 1 d R . .
O3 O 0.6960(3) 0.4094(2) 0.43482(11) 0.0140(4) Uani 1 1 d . . .
H3A H 0.5984 0.4687 0.4516 0.021 Uiso 1 1 d R . .
H3B H 0.8164 0.4609 0.4343 0.021 Uiso 1 1 d R . .
O4 O 0.7234(4) -0.1566(3) 0.65633(13) 0.0291(5) Uani 1 1 d . . .
H4A H 0.7596 -0.2191 0.6250 0.044 Uiso 1 1 d R . .
H4B H 0.6746 -0.1931 0.6934 0.044 Uiso 1 1 d R . .
O11 O 0.4282(3) 0.26355(18) 0.55642(10) 0.0105(4) Uani 1 1 d . . .
O12 O 0.3906(3) 0.5332(2) 0.53211(10) 0.0110(4) Uani 1 1 d . . .
O13 O 0.0405(3) 0.3882(2) 0.56698(10) 0.0099(4) Uani 1 1 d . . .
O21 O 0.4693(3) 0.1823(2) 0.72256(10) 0.0149(4) Uani 1 1 d . . .
O22 O 0.3224(3) 0.3665(2) 0.80895(10) 0.0145(4) Uani 1 1 d . . .
O23 O 0.0403(3) 0.2474(2) 0.72103(9) 0.0132(4) Uani 1 1 d . . .
C1 C 0.3601(5) 0.4416(3) 0.66900(15) 0.0109(5) Uani 1 1 d . . .
C11 C 0.4918(5) 0.0695(3) 0.77399(15) 0.0136(5) Uani 1 1 d . . .
C12 C 0.3267(5) -0.0373(3) 0.77796(16) 0.0186(6) Uani 1 1 d . . .
H12 H 0.1944 -0.0351 0.7476 0.022 Uiso 1 1 calc R . .
C13 C 0.3595(6) -0.1481(3) 0.82762(16) 0.0215(6) Uani 1 1 d . . .
H13 H 0.2482 -0.2225 0.8317 0.026 Uiso 1 1 calc R . .
C14 C 0.5540(6) -0.1502(4) 0.87114(17) 0.0238(7) Uani 1 1 d . . .
H14 H 0.5762 -0.2270 0.9045 0.029 Uiso 1 1 calc R . .
C15 C 0.7169(6) -0.0411(4) 0.86654(18) 0.0232(7) Uani 1 1 d . . .
H15 H 0.8489 -0.0427 0.8970 0.028 Uiso 1 1 calc R . .
C16 C 0.6862(5) 0.0712(3) 0.81684(16) 0.0193(6) Uani 1 1 d . . .
H16 H 0.7962 0.1464 0.8128 0.023 Uiso 1 1 calc R . .
C21 C 0.1555(5) 0.3590(3) 0.86244(15) 0.0152(6) Uani 1 1 d . . .
C22 C -0.0356(5) 0.4463(3) 0.85819(16) 0.0184(6) Uani 1 1 d . . .
H22 H -0.0568 0.5122 0.8195 0.022 Uiso 1 1 calc R . .
C23 C -0.1968(6) 0.4358(4) 0.91178(17) 0.0239(7) Uani 1 1 d . . .
H23 H -0.3312 0.4937 0.9094 0.029 Uiso 1 1 calc R . .
C24 C -0.1626(6) 0.3419(4) 0.96839(17) 0.0277(7) Uani 1 1 d . . .
H24 H -0.2721 0.3369 1.0052 0.033 Uiso 1 1 calc R . .
C25 C 0.1925(5) 0.2621(3) 0.91836(15) 0.0215(7) Uani 1 1 d . . .
H25 H 0.3250 0.2025 0.9201 0.026 Uiso 1 1 calc R . .
C26 C 0.0303(6) 0.2546(4) 0.97192(17) 0.0292(8) Uani 1 1 d . . .
H26 H 0.0521 0.1897 1.0109 0.035 Uiso 1 1 calc R . .


_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
Cd1 O11 2.2571(18) . ?
Cd1 O12 2.2613(19) 2_646 ?
Cd1 O13 2.2787(18) 1_655 ?
Cd1 O1 2.3109(19) . ?
Cd1 O3 2.338(2) . ?
Cd1 O2 2.3405(18) . ?
Cl1 C1 1.775(3) . ?
Cl2 C1 1.798(3) . ?
P1 O12 1.518(2) . ?
P1 O13 1.5162(19) . ?
P1 O11 1.5222(18) . ?
P1 C1 1.876(3) . ?
P2 O23 1.469(2) . ?
P2 O21 1.574(2) . ?
P2 O22 1.590(2) . ?
P2 C1 1.831(3) . ?
O1 H1A 0.8538 . ?
O1 H1B 0.8457 . ?
O2 H2A 0.8522 . ?
O2 H2B 0.8520 . ?
O3 H3A 0.8543 . ?
O3 H3B 0.8491 . ?
O4 H4A 0.8507 . ?
O4 H4B 0.8258 . ?
O12 Cd1 2.2614(18) 2_656 ?
O13 Cd1 2.2787(18) 1_455 ?
O21 C11 1.421(3) . ?
O22 C21 1.411(3) . ?
C11 C16 1.377(4) . ?
C11 C12 1.382(4) . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.401(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.378(4) . ?
C21 C25 1.389(4) . ?
C22 C23 1.391(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(5) . ?
C23 H23 0.9500 . ?
C24 C26 1.386(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

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
O11 Cd1 O12 80.04(7) . 2_646 ?
O11 Cd1 O13 111.96(6) . 1_655 ?
O12 Cd1 O13 166.41(6) 2_646 1_655 ?
O11 Cd1 O1 99.44(7) . . ?
O12 Cd1 O1 89.12(7) 2_646 . ?
O13 Cd1 O1 82.73(7) 1_655 . ?
O11 Cd1 O3 84.54(7) . . ?
O12 Cd1 O3 101.54(7) 2_646 . ?
O13 Cd1 O3 86.43(7) 1_655 . ?
O1 Cd1 O3 169.16(7) . . ?
O11 Cd1 O2 165.42(6) . . ?
O12 Cd1 O2 87.36(7) 2_646 . ?
O13 Cd1 O2 81.46(7) 1_655 . ?
O1 Cd1 O2 87.59(7) . . ?
O3 Cd1 O2 90.88(7) . . ?
O12 P1 O13 113.66(11) . . ?
O12 P1 O11 113.20(11) . . ?
O13 P1 O11 114.26(10) . . ?
O12 P1 C1 105.08(12) . . ?
O13 P1 C1 104.34(11) . . ?
O11 P1 C1 104.99(11) . . ?
O23 P2 O21 115.69(12) . . ?
O23 P2 O22 113.07(11) . . ?
O21 P2 O22 104.77(11) . . ?
O23 P2 C1 114.25(12) . . ?
O21 P2 C1 102.81(12) . . ?
O22 P2 C1 105.03(12) . . ?
Cd1 O1 H1A 102.8 . . ?
Cd1 O1 H1B 105.7 . . ?
H1A O1 H1B 120.4 . . ?
Cd1 O2 H2A 107.1 . . ?
Cd1 O2 H2B 105.2 . . ?
H2A O2 H2B 109.7 . . ?
Cd1 O3 H3A 111.3 . . ?
Cd1 O3 H3B 103.3 . . ?
H3A O3 H3B 101.8 . . ?
H4A O4 H4B 113.3 . . ?
P1 O11 Cd1 130.89(10) . . ?
P1 O12 Cd1 131.70(11) . 2_656 ?
P1 O13 Cd1 136.12(11) . 1_455 ?
C11 O21 P2 119.18(17) . . ?
C21 O22 P2 121.13(17) . . ?
Cl1 C1 Cl2 109.27(15) . . ?
Cl1 C1 P2 108.46(14) . . ?
Cl2 C1 P2 106.04(14) . . ?
Cl1 C1 P1 109.78(14) . . ?
Cl2 C1 P1 107.48(14) . . ?
P2 C1 P1 115.62(15) . . ?
C16 C11 C12 123.1(3) . . ?
C16 C11 O21 116.7(2) . . ?
C12 C11 O21 120.2(3) . . ?
C11 C12 C13 118.2(3) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.6(3) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C11 C16 C15 118.1(3) . . ?
C11 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
C22 C21 C25 122.3(3) . . ?
C22 C21 O22 120.0(3) . . ?
C25 C21 O22 117.7(3) . . ?
C21 C22 C23 118.5(3) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C26 120.5(3) . . ?
C23 C24 H24 119.8 . . ?
C26 C24 H24 119.8 . . ?
C21 C25 C26 118.3(3) . . ?
C21 C25 H25 120.8 . . ?
C26 C25 H25 120.8 . . ?
C24 C26 C25 120.1(3) . . ?
C24 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?

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
O1 H1A O4 0.85 1.90 2.639(3) 144.7 .
O1 H1B O23 0.85 1.87 2.688(3) 161.8 1_655
O2 H2A O13 0.85 1.92 2.705(3) 152.4 2_646
O2 H2B O11 0.85 1.98 2.817(3) 165.3 1_655
O3 H3A O12 0.85 2.04 2.814(3) 150.2 .
O3 H3B O1 0.85 2.04 2.845(3) 157.5 2_756
O4 H4A O2 0.85 1.98 2.819(3) 169.0 2_746

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.079

#===END===============================================================

data_III
_database_code_depnum_ccdc_archive 'CCDC 719963'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C3 H9 Cd1.50 Cl2 O8 P2, 0.5(C3 H6 O), 4.5(H2 O)'
_chemical_formula_sum            'C4.50 H21 Cd1.50 Cl2 O13 P2'
_chemical_formula_weight         584.65

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   31.2205(3)
_cell_length_b                   10.1546(1)
_cell_length_c                   11.6510(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.107(1)
_cell_angle_gamma                90.00
_cell_volume                     3597.51(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    27848
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      27.48

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2304
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5828
_exptl_absorpt_correction_T_max  0.7079
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27848
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4115
_reflns_number_gt                3746
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius,1997-200)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond v.3.0 (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0200P)²+12.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4115
_refine_ls_number_parameters     213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0592
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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
Cd1 Cd 0.2500 0.2500 0.0000 0.01072(7) Uani 1 2 d S . .
Cd2 Cd 0.250516(6) 0.127379(17) 0.358272(15) 0.01187(6) Uani 1 1 d . . .
Cl1 Cl 0.13189(2) -0.08914(6) 0.13473(6) 0.01655(13) Uani 1 1 d . . .
Cl2 Cl 0.13895(2) 0.02343(7) -0.08856(5) 0.01842(14) Uani 1 1 d . . .
P1 P 0.22016(2) -0.05242(6) 0.08618(5) 0.00938(13) Uani 1 1 d . . .
P2 P 0.16355(2) 0.18641(6) 0.12659(5) 0.01040(13) Uani 1 1 d . . .
O1 O 0.28273(6) 0.23569(17) 0.19672(15) 0.0133(4) Uani 1 1 d . . .
H1A H 0.2897 0.3274 0.2232 0.016 Uiso 1 1 calc R . .
H1B H 0.3113 0.1916 0.2008 0.016 Uiso 1 1 calc R . .
O2 O 0.32050(6) 0.04033(17) 0.41060(16) 0.0142(4) Uani 1 1 d . . .
H2A H 0.3348 0.0519 0.3584 0.021 Uiso 1 1 d R . .
H2B H 0.3193 -0.0424 0.4189 0.021 Uiso 1 1 d R . .
O3 O 0.36177(7) 0.0976(2) 0.23700(17) 0.0218(4) Uani 1 1 d . . .
H3A H 0.3886 0.1214 0.2621 0.033 Uiso 1 1 d R . .
H3B H 0.3630 0.0196 0.2101 0.033 Uiso 1 1 d R . .
O4 O 0.13567(7) 0.3583(2) 0.37575(17) 0.0212(4) Uani 1 1 d . . .
H4A H 0.1483 0.2949 0.3482 0.032 Uiso 1 1 d R . .
H4B H 0.1541 0.3813 0.4384 0.032 Uiso 1 1 d R . .
O5 O 0.05183(8) 0.3062(3) 0.4167(2) 0.0376(6) Uani 1 1 d . . .
H5A H 0.0789 0.3125 0.4168 0.056 Uiso 1 1 d R . .
H5B H 0.0490 0.3089 0.4877 0.056 Uiso 1 1 d R . .
O6 O 0.05177(7) 0.3269(2) 0.6654(2) 0.0333(5) Uani 1 1 d . . .
H6A H 0.0419 0.2578 0.6912 0.050 Uiso 1 1 d R . .
H6B H 0.0299 0.3764 0.6403 0.050 Uiso 1 1 d R . .
O7 O 0.0000 0.4792(3) 0.2500 0.0302(7) Uani 1 2 d S . .
H7 H 0.0189 0.4360 0.2985 0.045 Uiso 1 1 d R . .
O8 O 0.0000 0.1377(3) 0.7500 0.0425(9) Uani 1 2 d S . .
O11 O 0.24238(6) 0.02702(17) 0.00377(15) 0.0121(4) Uani 1 1 d . . .
O12 O 0.23941(6) -0.03736(17) 0.21695(15) 0.0122(4) Uani 1 1 d . . .
O13 O 0.21566(6) -0.19423(17) 0.04555(15) 0.0131(4) Uani 1 1 d . . .
O21 O 0.18471(6) 0.27458(17) 0.05155(15) 0.0134(4) Uani 1 1 d . . .
O22 O 0.18327(6) 0.18440(18) 0.25627(15) 0.0131(4) Uani 1 1 d . . .
O23 O 0.11377(6) 0.22210(19) 0.11281(16) 0.0162(4) Uani 1 1 d . . .
C1 C 0.16402(8) 0.0178(2) 0.0650(2) 0.0119(5) Uani 1 1 d . . .
C21 C 0.08527(11) 0.2712(4) 0.0048(3) 0.0306(7) Uani 1 1 d . . .
H21A H 0.0660 0.1996 -0.0353 0.037 Uiso 1 1 calc R . .
H21B H 0.1032 0.3039 -0.0494 0.037 Uiso 1 1 calc R . .
C22 C 0.05846(13) 0.3790(4) 0.0365(4) 0.0442(10) Uani 1 1 d . . .
H22A H 0.0427 0.3474 0.0948 0.066 Uiso 1 1 calc R . .
H22B H 0.0372 0.4089 -0.0341 0.066 Uiso 1 1 calc R . .
H22C H 0.0777 0.4524 0.0698 0.066 Uiso 1 1 calc R . .
C2 C 0.0000 0.0176(5) 0.7500 0.0329(11) Uani 1 2 d S . .
C3 C -0.02481(14) -0.0577(4) 0.8224(4) 0.0541(11) Uani 1 1 d . . .
H3C H -0.0354 0.0025 0.8757 0.081 Uiso 1 1 calc R . .
H3D H -0.0055 -0.1241 0.8687 0.081 Uiso 1 1 calc R . .
H3E H -0.0499 -0.1014 0.7708 0.081 Uiso 1 1 calc R . .


_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
Cd1 O21 2.2657(17) . ?
Cd1 O21 2.2657(17) 7 ?
Cd1 O11 2.2782(17) 7 ?
Cd1 O11 2.2782(17) . ?
Cd1 O1 2.2926(17) . ?
Cd1 O1 2.2927(17) 7 ?
Cd2 O22 2.2413(17) . ?
Cd2 O13 2.2617(17) 4 ?
Cd2 O2 2.3072(18) . ?
Cd2 O12 2.3175(17) . ?
Cd2 O11 2.3646(17) 6_556 ?
Cd2 O1 2.5734(17) . ?
Cl1 C1 1.793(2) . ?
Cl2 C1 1.784(2) . ?
P1 O13 1.5125(18) . ?
P1 O12 1.5135(17) . ?
P1 O11 1.5349(17) . ?
P1 C1 1.856(3) . ?
P2 O22 1.4968(18) . ?
P2 O21 1.5047(18) . ?
P2 O23 1.5685(19) . ?
P2 C1 1.858(3) . ?
O1 H1A 0.9900 . ?
O1 H1B 0.9900 . ?
O2 H2A 0.8414 . ?
O2 H2B 0.8477 . ?
O3 H3A 0.8560 . ?
O3 H3B 0.8554 . ?
O4 H4A 0.8541 . ?
O4 H4B 0.8536 . ?
O5 H5A 0.8468 . ?
O5 H5B 0.8525 . ?
O6 H6A 0.8481 . ?
O6 H6B 0.8448 . ?
O7 H7 0.8416 . ?
O8 C2 1.219(6) . ?
O11 Cd2 2.3647(17) 6 ?
O13 Cd2 2.2617(17) 4_545 ?
O23 C21 1.455(3) . ?
C21 C22 1.476(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C2 C3 1.481(5) 2_556 ?
C2 C3 1.481(5) . ?
C3 H3C 0.9800 . ?
C3 H3D 0.9800 . ?
C3 H3E 0.9800 . ?

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
O21 Cd1 O21 180.00(8) . 7 ?
O21 Cd1 O11 89.99(6) . 7 ?
O21 Cd1 O11 90.01(6) 7 7 ?
O21 Cd1 O11 90.01(6) . . ?
O21 Cd1 O11 89.99(6) 7 . ?
O11 Cd1 O11 180.0 7 . ?
O21 Cd1 O1 88.04(6) . . ?
O21 Cd1 O1 91.96(6) 7 . ?
O11 Cd1 O1 93.29(6) 7 . ?
O11 Cd1 O1 86.71(6) . . ?
O21 Cd1 O1 91.96(6) . 7 ?
O21 Cd1 O1 88.04(6) 7 7 ?
O11 Cd1 O1 86.70(6) 7 7 ?
O11 Cd1 O1 93.29(6) . 7 ?
O1 Cd1 O1 180.0 . 7 ?
O22 Cd2 O13 109.37(6) . 4 ?
O22 Cd2 O2 162.97(6) . . ?
O13 Cd2 O2 82.42(6) 4 . ?
O22 Cd2 O12 80.71(6) . . ?
O13 Cd2 O12 155.22(6) 4 . ?
O2 Cd2 O12 83.76(6) . . ?
O22 Cd2 O11 108.14(6) . 6_556 ?
O13 Cd2 O11 106.85(6) 4 6_556 ?
O2 Cd2 O11 78.80(6) . 6_556 ?
O12 Cd2 O11 90.44(6) . 6_556 ?
O22 Cd2 O1 88.64(6) . . ?
O13 Cd2 O1 78.70(6) 4 . ?
O2 Cd2 O1 81.56(6) . . ?
O12 Cd2 O1 79.00(6) . . ?
O11 Cd2 O1 158.60(6) 6_556 . ?
O13 P1 O12 113.50(10) . . ?
O13 P1 O11 109.13(10) . . ?
O12 P1 O11 116.36(10) . . ?
O13 P1 C1 107.85(11) . . ?
O12 P1 C1 104.04(10) . . ?
O11 P1 C1 105.18(10) . . ?
O22 P2 O21 117.41(11) . . ?
O22 P2 O23 106.12(10) . . ?
O21 P2 O23 111.00(10) . . ?
O22 P2 C1 109.88(11) . . ?
O21 P2 C1 106.31(10) . . ?
O23 P2 C1 105.54(11) . . ?
Cd1 O1 Cd2 126.78(7) . . ?
Cd1 O1 H1A 105.6 . . ?
Cd2 O1 H1A 105.6 . . ?
Cd1 O1 H1B 105.6 . . ?
Cd2 O1 H1B 105.6 . . ?
H1A O1 H1B 106.1 . . ?
Cd2 O2 H2A 112.5 . . ?
Cd2 O2 H2B 110.3 . . ?
H2A O2 H2B 105.3 . . ?
H3A O3 H3B 105.4 . . ?
H4A O4 H4B 104.4 . . ?
H5A O5 H5B 108.6 . . ?
H6A O6 H6B 106.6 . . ?
P1 O11 Cd1 126.75(10) . . ?
P1 O11 Cd2 103.73(9) . 6 ?
Cd1 O11 Cd2 128.06(7) . 6 ?
P1 O12 Cd2 138.54(10) . . ?
P1 O13 Cd2 127.43(10) . 4_545 ?
P2 O21 Cd1 128.93(10) . . ?
P2 O22 Cd2 131.31(10) . . ?
C21 O23 P2 124.40(18) . . ?
Cl2 C1 Cl1 108.09(13) . . ?
Cl2 C1 P1 109.40(13) . . ?
Cl1 C1 P1 108.37(13) . . ?
Cl2 C1 P2 108.55(13) . . ?
Cl1 C1 P2 109.20(13) . . ?
P1 C1 P2 113.12(13) . . ?
O23 C21 C22 107.9(3) . . ?
O23 C21 H21A 110.1 . . ?
C22 C21 H21A 110.1 . . ?
O23 C21 H21B 110.1 . . ?
C22 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C2 C3 121.1(2) . 2_556 ?
O8 C2 C3 121.1(2) . . ?
C3 C2 C3 117.8(5) 2_556 . ?
C2 C3 H3C 109.5 . . ?
C2 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
C2 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?

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
O1 H1B O3 0.99 1.81 2.784(3) 168.0 .
O1 H1A O12 0.99 1.87 2.668(2) 135.8 4
O2 H2A O3 0.84 1.86 2.696(3) 172.2 .
O2 H2B O21 0.85 1.90 2.745(2) 175.5 4_545
O3 H3A O6 0.86 1.94 2.788(3) 174.2 7_556
O3 H3B O4 0.86 1.93 2.772(3) 170.4 4_545
O4 H4A O22 0.85 2.03 2.864(3) 164.3 .
O4 H4B O2 0.85 1.93 2.754(3) 161.9 7_556
O5 H5A O4 0.85 1.99 2.815(3) 163.4 .
O5 H5B O6 0.85 2.06 2.906(3) 171.2 .
O6 H6A O8 0.85 2.02 2.828(3) 159.3 .
O7 H7 O5 0.84 2.01 2.837(3) 166.4 .
O6 H6B O7 0.84 2.28 2.861(3) 126.1 5_566

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.622
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.113


