# 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
'Susan Kunnas-Hiltunen'
'Markku Ahlgren'
'Matti Haukka'
'Jouko J Vepsalainen'

_publ_contact_author_name        'Susan Kunnas-Hiltunen'
_publ_contact_author_email       SUSAN.KUNNAS-HILTUNEN@UEF.FI

_publ_section_title              
;
Alkaline and Alkaline Earth Metal Complexes of
Dianhydride Derivatives of Clodronate and Their
Hydrolysis Products
;

# Attachment 'CIF_SKunnas-Hiltunen'

data_Structure(1)
_database_code_depnum_ccdc_archive 'CCDC 764807'
#TrackingRef 'CIF_SKunnas-Hiltunen'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C H10 Cl2 Na3 O11 P2'
_chemical_formula_sum            'C H10 Cl2 Na3 O11 P2'
_chemical_formula_weight         399.9

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'
Na Na 0.0362 0.0249 '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'

_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                   6.0326(12)
_cell_length_b                   9.6930(19)
_cell_length_c                   11.510(2)
_cell_angle_alpha                93.31(3)
_cell_angle_beta                 91.63(3)
_cell_angle_gamma                103.42(3)
_cell_volume                     653.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12304
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      28.23

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             402
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_publ_section_exptl_refinement   
;The highest peak is located 0.92 \%A from atom O13 and the deepest hole is
located 0.82 \%A from atom P1.
;

_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  'Nonius KappaCCD'
_diffrn_measurement_method       multi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12304
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.71
_diffrn_reflns_theta_max         28.23
_reflns_number_total             3132
_reflns_number_gt                2655
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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    'XP in SHELXTL v.5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0400P)^2^+2.1500P] 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         3132
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0936
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_restrained_S_all      0.940
_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
Cl1 Cl -0.13349(11) -0.00985(7) 0.65670(6) 0.01597(16) Uani 1 1 d . . .
Cl2 Cl 0.34706(11) -0.00356(7) 0.63268(6) 0.01534(15) Uani 1 1 d . . .
P1 P 0.10180(11) -0.14695(7) 0.82558(6) 0.01043(15) Uani 1 1 d . . .
P2 P 0.21293(11) 0.19125(7) 0.80820(6) 0.00997(15) Uani 1 1 d . . .
Na1 Na -0.2817(2) -0.42340(13) 0.62829(10) 0.0188(3) Uani 1 1 d . . .
Na2 Na 0.66140(18) 0.04306(11) 0.89341(10) 0.0138(2) Uani 1 1 d . . .
Na3 Na 0.51702(19) 0.32653(12) 1.05712(10) 0.0164(2) Uani 1 1 d . . .
O12 O 0.3160(3) -0.1263(2) 0.90204(17) 0.0125(4) Uani 1 1 d . . .
O11 O 0.0448(3) -0.2764(2) 0.74277(17) 0.0148(4) Uani 1 1 d . . .
O13 O -0.1059(3) -0.1341(2) 0.90169(17) 0.0129(4) Uani 1 1 d . . .
O21 O 0.4479(3) 0.2092(2) 0.86506(17) 0.0127(4) Uani 1 1 d . . .
O22 O 0.1967(3) 0.2920(2) 0.71443(17) 0.0135(4) Uani 1 1 d . . .
O23 O 0.0289(3) 0.1913(2) 0.89786(17) 0.0126(4) Uani 1 1 d . . .
O1 O 0.0372(4) -0.3209(2) 0.49740(19) 0.0226(5) Uani 1 1 d . . .
H1O H -0.0344 -0.2917 0.4425 0.034 Uiso 1 1 d R . .
H1P H 0.0942 -0.2508 0.5457 0.034 Uiso 1 1 d R . .
O2 O -0.4999(4) -0.3455(2) 0.47883(19) 0.0222(5) Uani 1 1 d . . .
H2O H -0.6444 -0.3224 0.4840 0.033 Uiso 1 1 d R . .
H2P H -0.4205 -0.3053 0.4201 0.033 Uiso 1 1 d R . .
O3 O -0.2084(3) -0.5985(2) 0.76028(18) 0.0166(4) Uani 1 1 d . . .
H3P H -0.3199 -0.6695 0.7821 0.025 Uiso 1 1 d R . .
H3O H -0.0956 -0.6350 0.7505 0.025 Uiso 1 1 d R . .
O4 O 0.6017(3) 0.4190(2) 1.25046(18) 0.0162(4) Uani 1 1 d . . .
H4O H 0.6581 0.5078 1.2568 0.024 Uiso 1 1 d R . .
H4P H 0.7128 0.3791 1.2763 0.024 Uiso 1 1 d R . .
O5 O 0.7588(3) 0.5306(2) 0.97672(18) 0.0177(4) Uani 1 1 d . . .
H5O H 0.8106 0.5106 0.9101 0.026 Uiso 1 1 d R . .
H5P H 0.8744 0.5947 1.0130 0.026 Uiso 1 1 d R . .
C1 C 0.1332(4) 0.0093(3) 0.7351(2) 0.0115(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
Cl1 0.0123(3) 0.0142(3) 0.0210(3) 0.0028(3) -0.0050(2) 0.0024(2)
Cl2 0.0145(3) 0.0148(3) 0.0173(3) 0.0010(2) 0.0039(2) 0.0041(2)
P1 0.0096(3) 0.0069(3) 0.0149(3) 0.0018(2) -0.0002(2) 0.0020(2)
P2 0.0092(3) 0.0065(3) 0.0143(3) 0.0019(2) 0.0004(2) 0.0017(2)
Na1 0.0179(6) 0.0192(6) 0.0193(6) 0.0042(5) -0.0005(4) 0.0035(5)
Na2 0.0108(5) 0.0104(5) 0.0204(6) 0.0021(4) 0.0004(4) 0.0026(4)
Na3 0.0194(6) 0.0115(5) 0.0192(6) 0.0005(4) -0.0025(4) 0.0063(4)
O12 0.0126(9) 0.0099(9) 0.0153(10) 0.0022(7) -0.0014(7) 0.0029(7)
O11 0.0152(10) 0.0099(9) 0.0190(10) -0.0012(8) -0.0012(8) 0.0033(7)
O13 0.0101(9) 0.0113(9) 0.0184(10) 0.0031(7) 0.0020(7) 0.0040(7)
O21 0.0115(9) 0.0105(9) 0.0165(10) 0.0012(7) -0.0016(7) 0.0039(7)
O22 0.0144(10) 0.0105(9) 0.0163(10) 0.0039(7) -0.0002(7) 0.0033(7)
O23 0.0106(9) 0.0106(9) 0.0165(10) 0.0023(7) 0.0018(7) 0.0017(7)
O1 0.0251(12) 0.0246(12) 0.0172(11) -0.0013(9) -0.0014(9) 0.0050(9)
O2 0.0248(11) 0.0229(11) 0.0213(11) 0.0073(9) 0.0030(9) 0.0088(9)
O3 0.0139(10) 0.0125(10) 0.0245(11) 0.0039(8) 0.0031(8) 0.0045(7)
O4 0.0170(10) 0.0088(9) 0.0227(11) 0.0010(8) -0.0002(8) 0.0030(7)
O5 0.0174(10) 0.0136(10) 0.0214(11) -0.0004(8) 0.0007(8) 0.0028(8)
C1 0.0074(12) 0.0121(12) 0.0153(13) 0.0016(10) -0.0028(10) 0.0029(9)

_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
Cl1 C1 1.788(3) . ?
Cl1 Na2 3.0893(15) 1_455 ?
Cl2 C1 1.792(3) . ?
P1 O11 1.498(2) . ?
P1 O12 1.510(2) . ?
P1 O13 1.574(2) . ?
P1 C1 1.864(3) . ?
P2 O21 1.512(2) . ?
P2 O22 1.513(2) . ?
P2 O23 1.537(2) . ?
P2 C1 1.861(3) . ?
P2 Na3 3.3830(18) . ?
Na1 O2 2.397(2) . ?
Na1 O4 2.421(2) 2_557 ?
Na1 O11 2.446(2) . ?
Na1 O3 2.448(2) . ?
Na1 O1 2.532(3) . ?
Na1 O2 2.548(3) 2_446 ?
Na1 Na1 3.886(3) 2_446 ?
Na1 Na3 4.065(2) 2_557 ?
Na2 O21 2.315(2) . ?
Na2 O23 2.343(2) 1_655 ?
Na2 O12 2.343(2) . ?
Na2 O12 2.434(2) 2_657 ?
Na2 O13 2.461(2) 1_655 ?
Na2 Cl1 3.0893(15) 1_655 ?
Na2 Na2 3.204(2) 2_657 ?
Na2 Na3 3.5308(18) . ?
Na2 Na3 3.5773(18) 2_657 ?
Na3 O4 2.347(2) . ?
Na3 O21 2.407(2) . ?
Na3 O5 2.418(2) . ?
Na3 O5 2.436(2) 2_667 ?
Na3 O12 2.447(2) 2_657 ?
Na3 O13 2.806(2) 2_557 ?
Na3 Na2 3.5774(18) 2_657 ?
Na3 Na3 3.728(2) 2_667 ?
Na3 Na1 4.065(2) 2_557 ?
O12 Na2 2.434(2) 2_657 ?
O12 Na3 2.447(2) 2_657 ?
O13 Na2 2.461(2) 1_455 ?
O13 Na3 2.806(2) 2_557 ?
O23 Na2 2.343(2) 1_455 ?
O1 H1O 0.8533 . ?
O1 H1P 0.8519 . ?
O2 Na1 2.548(3) 2_446 ?
O2 H2O 0.9512 . ?
O2 H2P 0.8944 . ?
O3 H3P 0.8962 . ?
O3 H3O 0.8439 . ?
O4 Na1 2.421(2) 2_557 ?
O4 H4O 0.8468 . ?
O4 H4P 0.8994 . ?
O5 Na3 2.436(2) 2_667 ?
O5 H5O 0.8645 . ?
O5 H5P 0.8940 . ?

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
C1 Cl1 Na2 87.15(10) . 1_455 ?
O11 P1 O12 116.92(11) . . ?
O11 P1 O13 111.69(11) . . ?
O12 P1 O13 110.19(11) . . ?
O11 P1 C1 106.49(12) . . ?
O12 P1 C1 107.85(12) . . ?
O13 P1 C1 102.55(11) . . ?
O21 P2 O22 115.18(11) . . ?
O21 P2 O23 112.37(11) . . ?
O22 P2 O23 111.24(11) . . ?
O21 P2 C1 106.99(12) . . ?
O22 P2 C1 106.03(12) . . ?
O23 P2 C1 104.11(12) . . ?
O21 P2 Na3 39.10(8) . . ?
O22 P2 Na3 117.89(9) . . ?
O23 P2 Na3 76.47(8) . . ?
C1 P2 Na3 132.72(9) . . ?
O2 Na1 O4 85.80(8) . 2_557 ?
O2 Na1 O11 126.22(9) . . ?
O4 Na1 O11 103.75(8) 2_557 . ?
O2 Na1 O3 153.05(9) . . ?
O4 Na1 O3 83.92(8) 2_557 . ?
O11 Na1 O3 80.52(8) . . ?
O2 Na1 O1 80.73(8) . . ?
O4 Na1 O1 155.66(9) 2_557 . ?
O11 Na1 O1 69.27(8) . . ?
O3 Na1 O1 116.51(8) . . ?
O2 Na1 O2 76.46(9) . 2_446 ?
O4 Na1 O2 90.91(8) 2_557 2_446 ?
O11 Na1 O2 153.19(9) . 2_446 ?
O3 Na1 O2 78.85(8) . 2_446 ?
O1 Na1 O2 105.38(9) . 2_446 ?
O2 Na1 Na1 39.61(6) . 2_446 ?
O4 Na1 Na1 88.01(7) 2_557 2_446 ?
O11 Na1 Na1 161.77(8) . 2_446 ?
O3 Na1 Na1 115.03(7) . 2_446 ?
O1 Na1 Na1 94.28(7) . 2_446 ?
O2 Na1 Na1 36.85(5) 2_446 2_446 ?
O2 Na1 Na3 108.64(7) . 2_557 ?
O4 Na1 Na3 30.96(5) 2_557 2_557 ?
O11 Na1 Na3 73.44(6) . 2_557 ?
O3 Na1 Na3 72.98(6) . 2_557 ?
O1 Na1 Na3 138.69(7) . 2_557 ?
O2 Na1 Na3 115.93(7) 2_446 2_557 ?
Na1 Na1 Na3 118.94(5) 2_446 2_557 ?
O21 Na2 O23 99.69(8) . 1_655 ?
O21 Na2 O12 87.46(8) . . ?
O23 Na2 O12 172.36(8) 1_655 . ?
O21 Na2 O12 85.63(8) . 2_657 ?
O23 Na2 O12 82.19(8) 1_655 2_657 ?
O12 Na2 O12 95.78(8) . 2_657 ?
O21 Na2 O13 174.07(8) . 1_655 ?
O23 Na2 O13 79.47(7) 1_655 1_655 ?
O12 Na2 O13 93.70(7) . 1_655 ?
O12 Na2 O13 100.03(8) 2_657 1_655 ?
O21 Na2 Cl1 106.17(7) . 1_655 ?
O23 Na2 Cl1 73.00(6) 1_655 1_655 ?
O12 Na2 Cl1 107.73(7) . 1_655 ?
O12 Na2 Cl1 153.89(6) 2_657 1_655 ?
O13 Na2 Cl1 67.93(6) 1_655 1_655 ?
O21 Na2 Na2 84.82(7) . 2_657 ?
O23 Na2 Na2 128.43(8) 1_655 2_657 ?
O12 Na2 Na2 49.10(6) . 2_657 ?
O12 Na2 Na2 46.68(6) 2_657 2_657 ?
O13 Na2 Na2 100.34(7) 1_655 2_657 ?
Cl1 Na2 Na2 154.80(6) 1_655 2_657 ?
O21 Na2 Na3 42.60(6) . . ?
O23 Na2 Na3 85.09(6) 1_655 . ?
O12 Na2 Na3 98.58(7) . . ?
O12 Na2 Na3 43.82(5) 2_657 . ?
O13 Na2 Na3 142.61(7) 1_655 . ?
Cl1 Na2 Na3 138.43(4) 1_655 . ?
Na2 Na2 Na3 63.96(5) 2_657 . ?
O21 Na2 Na3 130.22(6) . 2_657 ?
O23 Na2 Na3 129.88(7) 1_655 2_657 ?
O12 Na2 Na3 42.81(5) . 2_657 ?
O12 Na2 Na3 95.61(6) 2_657 2_657 ?
O13 Na2 Na3 51.43(5) 1_655 2_657 ?
Cl1 Na2 Na3 94.12(5) 1_655 2_657 ?
Na2 Na2 Na3 62.47(5) 2_657 2_657 ?
Na3 Na2 Na3 126.43(4) . 2_657 ?
O4 Na3 O21 173.42(8) . . ?
O4 Na3 O5 93.69(9) . . ?
O21 Na3 O5 89.63(8) . . ?
O4 Na3 O5 93.41(8) . 2_667 ?
O21 Na3 O5 92.77(8) . 2_667 ?
O5 Na3 O5 79.65(8) . 2_667 ?
O4 Na3 O12 90.04(8) . 2_657 ?
O21 Na3 O12 83.39(8) . 2_657 ?
O5 Na3 O12 117.80(8) . 2_657 ?
O5 Na3 O12 161.97(8) 2_667 2_657 ?
O4 Na3 O13 96.81(8) . 2_557 ?
O21 Na3 O13 82.21(8) . 2_557 ?
O5 Na3 O13 156.34(8) . 2_557 ?
O5 Na3 O13 78.61(7) 2_667 2_557 ?
O12 Na3 O13 83.41(7) 2_657 2_557 ?
O4 Na3 P2 160.33(7) . . ?
O21 Na3 P2 23.35(5) . . ?
O5 Na3 P2 97.05(7) . . ?
O5 Na3 P2 72.49(6) 2_667 . ?
O12 Na3 P2 99.37(6) 2_657 . ?
O13 Na3 P2 67.47(6) 2_557 . ?
O4 Na3 Na2 132.92(7) . . ?
O21 Na3 Na2 40.62(5) . . ?
O5 Na3 Na2 101.62(7) . . ?
O5 Na3 Na2 132.88(7) 2_667 . ?
O12 Na3 Na2 43.52(5) 2_657 . ?
O13 Na3 Na2 86.55(6) 2_557 . ?
P2 Na3 Na2 60.53(4) . . ?
O4 Na3 Na2 99.28(7) . 2_657 ?
O21 Na3 Na2 75.52(6) . 2_657 ?
O5 Na3 Na2 154.15(7) . 2_657 ?
O5 Na3 Na2 121.41(7) 2_667 2_657 ?
O12 Na3 Na2 40.58(5) 2_657 2_657 ?
O13 Na3 Na2 43.28(5) 2_557 2_657 ?
P2 Na3 Na2 77.69(4) . 2_657 ?
Na2 Na3 Na2 53.57(4) . 2_657 ?
O4 Na3 Na3 94.63(7) . 2_667 ?
O21 Na3 Na3 91.57(7) . 2_667 ?
O5 Na3 Na3 40.01(5) . 2_667 ?
O5 Na3 Na3 39.64(6) 2_667 2_667 ?
O12 Na3 Na3 157.51(8) 2_657 2_667 ?
O13 Na3 Na3 117.71(7) 2_557 2_667 ?
P2 Na3 Na3 83.28(5) . 2_667 ?
Na2 Na3 Na3 125.13(5) . 2_667 ?
Na2 Na3 Na3 157.55(6) 2_657 2_667 ?
O4 Na3 Na1 32.04(5) . 2_557 ?
O21 Na3 Na1 149.78(6) . 2_557 ?
O5 Na3 Na1 112.63(7) . 2_557 ?
O5 Na3 Na1 72.62(6) 2_667 2_557 ?
O12 Na3 Na1 102.27(6) 2_657 2_557 ?
O13 Na3 Na1 69.21(6) 2_557 2_557 ?
P2 Na3 Na1 128.35(4) . 2_557 ?
Na2 Na3 Na1 141.44(4) . 2_557 ?
Na2 Na3 Na1 89.48(5) 2_657 2_557 ?
Na3 Na3 Na1 93.12(5) 2_667 2_557 ?
P1 O12 Na2 128.75(11) . . ?
P1 O12 Na2 123.04(11) . 2_657 ?
Na2 O12 Na2 84.22(8) . 2_657 ?
P1 O12 Na3 121.17(11) . 2_657 ?
Na2 O12 Na3 96.61(8) . 2_657 ?
Na2 O12 Na3 92.66(8) 2_657 2_657 ?
P1 O11 Na1 139.69(12) . . ?
P1 O13 Na2 127.83(11) . 1_455 ?
P1 O13 Na3 132.60(11) . 2_557 ?
Na2 O13 Na3 85.28(7) 1_455 2_557 ?
P2 O21 Na2 130.13(12) . . ?
P2 O21 Na3 117.55(11) . . ?
Na2 O21 Na3 96.78(8) . . ?
P2 O23 Na2 127.40(11) . 1_455 ?
Na1 O1 H1O 102.1 . . ?
Na1 O1 H1P 93.4 . . ?
H1O O1 H1P 108.7 . . ?
Na1 O2 Na1 103.54(9) . 2_446 ?
Na1 O2 H2O 128.3 . . ?
Na1 O2 H2O 85.6 2_446 . ?
Na1 O2 H2P 115.6 . . ?
Na1 O2 H2P 99.3 2_446 . ?
H2O O2 H2P 112.6 . . ?
Na1 O3 H3P 122.2 . . ?
Na1 O3 H3O 119.8 . . ?
H3P O3 H3O 105.0 . . ?
Na3 O4 Na1 117.00(9) . 2_557 ?
Na3 O4 H4O 113.6 . . ?
Na1 O4 H4O 96.0 2_557 . ?
Na3 O4 H4P 105.1 . . ?
Na1 O4 H4P 119.0 2_557 . ?
H4O O4 H4P 105.5 . . ?
Na3 O5 Na3 100.35(8) . 2_667 ?
Na3 O5 H5O 113.2 . . ?
Na3 O5 H5O 107.7 2_667 . ?
Na3 O5 H5P 127.5 . . ?
Na3 O5 H5P 101.6 2_667 . ?
H5O O5 H5P 104.4 . . ?
Cl1 C1 Cl2 108.57(14) . . ?
Cl1 C1 P2 108.01(14) . . ?
Cl2 C1 P2 107.34(14) . . ?
Cl1 C1 P1 106.61(14) . . ?
Cl2 C1 P1 107.00(14) . . ?
P2 C1 P1 118.98(15) . . ?

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 H1O O22 0.85 2.03 2.843(3) 159.1 2_556
O1 H1P O11 0.85 2.32 2.830(3) 119.1 .
O1 H1P Cl2 0.85 2.65 3.463(3) 160.5 .
O2 H2O O1 0.95 1.93 2.869(3) 167.1 1_455
O2 H2P O22 0.89 2.07 2.914(3) 156.0 2_556
O3 H3P O21 0.90 1.92 2.799(3) 165.3 1_445
O3 H3O O22 0.84 2.09 2.931(3) 173.9 1_545
O4 H4O O22 0.85 1.94 2.784(3) 174.2 2_667
O4 H4P O11 0.90 1.96 2.799(3) 154.3 2_657
O5 H5O O3 0.86 1.96 2.756(3) 153.2 1_665
O5 H5P O23 0.89 2.20 2.973(3) 143.8 2_667

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        28.23
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.100

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

data_Structure(2)
_database_code_depnum_ccdc_archive 'CCDC 764808'
#TrackingRef 'CIF_SKunnas-Hiltunen'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H12 Ba Cl2 O11 P2'
_chemical_formula_sum            'C5 H12 Ba Cl2 O11 P2'
_chemical_formula_weight         518.33

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'
Ba Ba -0.3244 2.2819 '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/m'
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   15.7725(5)
_cell_length_b                   7.5324(2)
_cell_length_c                   14.5010(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.240(2)
_cell_angle_gamma                90.00
_cell_volume                     1517.73(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9039
_cell_measurement_theta_min      3.90
_cell_measurement_theta_max      27.45

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    3.228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4443
_exptl_absorpt_correction_T_max  0.7384
_exptl_absorpt_process_details   'XPREP in SHELXL v.5.1 (Bruker AXS, 1998)'

_publ_section_exptl_refinement   
;The H~2~O hydrogen atoms were located from the difference Fourier map but
constrained to ride on their parent atom, with U~iso~ = 1.5
U~eq~(parent atom).
Other hydrogen atoms were positioned geometrically and were also constrained
to ride on their parent atoms, with C---H = 0.98 \%A, and
U~iso~ = 1.5 U~eq~(parent atom).
The highest peak is located 0.99 \%A from atom H22B and the deepest hole is
located 0.80 \%A from atom Ba1.
;

_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       multi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9039
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.90
_diffrn_reflns_theta_max         27.45
_reflns_number_total             1853
_reflns_number_gt                1759
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in SHELXTL v.5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0090P)^2^+5.0000P] 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         1853
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0423
_refine_ls_wR_factor_gt          0.0415
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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
Ba1 Ba 0.289533(12) 0.0000 0.056857(13) 0.00817(6) Uani 1 2 d S . .
Cl1 Cl 0.03309(4) 0.19314(8) 0.38035(4) 0.01472(12) Uani 1 1 d . . .
P1 P 0.06598(5) 0.0000 0.22140(6) 0.00776(15) Uani 1 2 d S . .
P2 P -0.13263(5) 0.0000 0.21335(6) 0.00821(15) Uani 1 2 d S . .
O1 O 0.47972(15) 0.0000 0.18668(18) 0.0159(5) Uani 1 2 d S . .
H1 H 0.5097 -0.0931 0.1887 0.024 Uiso 1 1 d R . .
O2 O 0.12959(10) 0.2325(2) 0.01942(11) 0.0121(3) Uani 1 1 d . . .
H2A H 0.1178 0.2391 0.0698 0.018 Uiso 1 1 d R . .
H2B H 0.0794 0.1992 -0.0311 0.018 Uiso 1 1 d R . .
O11 O 0.04819(10) 0.1706(2) 0.16407(12) 0.0123(3) Uani 1 1 d . . .
O12 O 0.17584(14) 0.0000 0.32221(16) 0.0119(4) Uani 1 2 d S . .
O13 O 0.24535(16) 0.0000 0.21880(18) 0.0183(5) Uani 1 2 d S . .
O21 O -0.16168(10) -0.1683(2) 0.15380(12) 0.0125(3) Uani 1 1 d . . .
O22 O -0.16190(15) 0.0000 0.30779(17) 0.0132(5) Uani 1 2 d S . .
O23 O -0.32053(16) 0.0000 0.19486(18) 0.0168(5) Uani 1 2 d S . .
C1 C 0.0002(2) 0.0000 0.2992(2) 0.0090(6) Uani 1 2 d S . .
C11 C 0.2537(2) 0.0000 0.3057(2) 0.0117(6) Uani 1 2 d S . .
C12 C 0.3469(2) 0.0000 0.4043(3) 0.0208(7) Uani 1 2 d S . .
H12A H 0.3346 0.0000 0.4645 0.031 Uiso 1 2 d SR . .
H12B H 0.3838 0.1062 0.4067 0.031 Uiso 1 1 d R . .
C21 C -0.2571(2) 0.0000 0.2835(3) 0.0125(6) Uani 1 2 d S . .
C22 C -0.2694(2) 0.0000 0.3794(3) 0.0201(7) Uani 1 2 d S . .
H22A H -0.2061 0.0000 0.4417 0.030 Uiso 1 2 d SR . .
H22B H -0.3051 -0.1062 0.3797 0.030 Uiso 1 1 d R . .

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
Ba1 0.00750(9) 0.00665(10) 0.00993(9) 0.000 0.00377(7) 0.000
Cl1 0.0124(2) 0.0178(3) 0.0142(2) -0.0076(2) 0.0065(2) -0.0035(2)
P1 0.0066(3) 0.0083(4) 0.0085(3) 0.000 0.0037(3) 0.000
P2 0.0066(3) 0.0092(4) 0.0086(3) 0.000 0.0034(3) 0.000
O1 0.0118(11) 0.0071(11) 0.0257(12) 0.000 0.0065(10) 0.000
O2 0.0106(7) 0.0157(8) 0.0097(7) -0.0011(6) 0.0045(6) -0.0010(6)
O11 0.0131(7) 0.0104(8) 0.0142(7) 0.0028(6) 0.0073(6) 0.0016(6)
O12 0.0068(10) 0.0188(12) 0.0102(10) 0.000 0.0040(8) 0.000
O13 0.0159(11) 0.0266(14) 0.0147(11) 0.000 0.0090(9) 0.000
O21 0.0095(7) 0.0114(8) 0.0155(7) -0.0036(6) 0.0051(6) -0.0014(6)
O22 0.0079(10) 0.0210(12) 0.0117(10) 0.000 0.0056(8) 0.000
O23 0.0130(11) 0.0213(13) 0.0150(11) 0.000 0.0057(9) 0.000
C1 0.0101(14) 0.0081(14) 0.0080(13) 0.000 0.0038(11) 0.000
C11 0.0114(14) 0.0090(15) 0.0162(15) 0.000 0.0076(12) 0.000
C12 0.0110(15) 0.033(2) 0.0164(16) 0.000 0.0047(13) 0.000
C21 0.0119(14) 0.0085(15) 0.0187(15) 0.000 0.0086(13) 0.000
C22 0.0147(16) 0.031(2) 0.0188(16) 0.000 0.0118(14) 0.000

_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
Ba1 O1 2.683(2) . ?
Ba1 O13 2.747(2) . ?
Ba1 O21 2.7902(15) 3 ?
Ba1 O21 2.7902(15) 8_545 ?
Ba1 O2 2.8716(15) 4_545 ?
Ba1 O2 2.8716(15) 7 ?
Ba1 O2 2.9034(15) 6 ?
Ba1 O2 2.9034(15) . ?
Ba1 O21 3.0293(15) 2 ?
Ba1 O21 3.0293(15) 5 ?
Ba1 Ba1 4.06356(16) 7 ?
Cl1 C1 1.7867(17) . ?
P1 O11 1.4833(16) 6 ?
P1 O11 1.4833(16) . ?
P1 O12 1.656(2) . ?
P1 C1 1.859(3) . ?
P2 O21 1.4796(16) . ?
P2 O21 1.4796(16) 6 ?
P2 O22 1.639(2) . ?
P2 C1 1.863(3) . ?
O1 H1 0.8389 . ?
O2 H2A 0.8362 . ?
O2 H2B 0.8226 . ?
O12 C11 1.358(4) . ?
O13 C11 1.203(4) . ?
O22 C21 1.370(4) . ?
O23 C21 1.198(4) . ?
C1 Cl1 1.7867(17) 6 ?
C11 C12 1.489(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C21 C22 1.493(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 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
O1 Ba1 O13 92.97(7) . . ?
O1 Ba1 O21 72.32(3) . 3 ?
O13 Ba1 O21 71.97(4) . 3 ?
O1 Ba1 O21 72.32(3) . 8_545 ?
O13 Ba1 O21 71.97(4) . 8_545 ?
O21 Ba1 O21 127.10(6) 3 8_545 ?
O1 Ba1 O2 73.58(5) . 4_545 ?
O13 Ba1 O2 131.90(3) . 4_545 ?
O21 Ba1 O2 139.06(4) 3 4_545 ?
O21 Ba1 O2 59.93(4) 8_545 4_545 ?
O1 Ba1 O2 73.58(5) . 7 ?
O13 Ba1 O2 131.90(3) . 7 ?
O21 Ba1 O2 59.93(4) 3 7 ?
O21 Ba1 O2 139.06(4) 8_545 7 ?
O2 Ba1 O2 89.12(6) 4_545 7 ?
O1 Ba1 O2 135.66(4) . 6 ?
O13 Ba1 O2 67.08(5) . 6 ?
O21 Ba1 O2 129.97(4) 3 6 ?
O21 Ba1 O2 64.04(4) 8_545 6 ?
O2 Ba1 O2 90.56(4) 4_545 6 ?
O2 Ba1 O2 148.899(17) 7 6 ?
O1 Ba1 O2 135.66(4) . . ?
O13 Ba1 O2 67.08(5) . . ?
O21 Ba1 O2 64.04(4) 3 . ?
O21 Ba1 O2 129.97(4) 8_545 . ?
O2 Ba1 O2 148.899(17) 4_545 . ?
O2 Ba1 O2 90.56(4) 7 . ?
O2 Ba1 O2 74.20(6) 6 . ?
O1 Ba1 O21 134.22(5) . 2 ?
O13 Ba1 O21 123.01(5) . 2 ?
O21 Ba1 O21 140.91(4) 3 2 ?
O21 Ba1 O21 91.52(4) 8_545 2 ?
O2 Ba1 O21 61.51(4) 4_545 2 ?
O2 Ba1 O21 96.34(4) 7 2 ?
O2 Ba1 O21 56.91(4) 6 2 ?
O2 Ba1 O21 87.65(4) . 2 ?
O1 Ba1 O21 134.22(5) . 5 ?
O13 Ba1 O21 123.01(5) . 5 ?
O21 Ba1 O21 91.52(4) 3 5 ?
O21 Ba1 O21 140.91(4) 8_545 5 ?
O2 Ba1 O21 96.34(4) 4_545 5 ?
O2 Ba1 O21 61.51(4) 7 5 ?
O2 Ba1 O21 87.65(4) 6 5 ?
O2 Ba1 O21 56.91(4) . 5 ?
O21 Ba1 O21 49.49(6) 2 5 ?
O1 Ba1 Ba1 108.137(12) . 7 ?
O13 Ba1 Ba1 101.163(16) . 7 ?
O21 Ba1 Ba1 48.18(3) 3 7 ?
O21 Ba1 Ba1 173.11(3) 8_545 7 ?
O2 Ba1 Ba1 126.94(3) 4_545 7 ?
O2 Ba1 Ba1 45.60(3) 7 7 ?
O2 Ba1 Ba1 114.24(3) 6 7 ?
O2 Ba1 Ba1 44.96(3) . 7 ?
O21 Ba1 Ba1 92.79(3) 2 7 ?
O21 Ba1 Ba1 43.35(3) 5 7 ?
O11 P1 O11 120.07(13) 6 . ?
O11 P1 O12 109.64(7) 6 . ?
O11 P1 O12 109.64(7) . . ?
O11 P1 C1 109.16(7) 6 . ?
O11 P1 C1 109.16(7) . . ?
O12 P1 C1 96.63(12) . . ?
O21 P2 O21 117.97(13) . 6 ?
O21 P2 O22 110.84(7) . . ?
O21 P2 O22 110.84(7) 6 . ?
O21 P2 C1 109.25(7) . . ?
O21 P2 C1 109.25(7) 6 . ?
O22 P2 C1 96.55(12) . . ?
Ba1 O1 H1 116.7 . . ?
Ba1 O2 Ba1 89.44(4) 7 . ?
Ba1 O2 H2A 128.2 7 . ?
Ba1 O2 H2A 113.9 . . ?
Ba1 O2 H2B 106.7 7 . ?
Ba1 O2 H2B 111.5 . . ?
H2A O2 H2B 106.2 . . ?
C11 O12 P1 120.00(19) . . ?
C11 O13 Ba1 161.5(2) . . ?
P2 O21 Ba1 175.41(9) . 3_445 ?
P2 O21 Ba1 95.99(7) . 5 ?
Ba1 O21 Ba1 88.48(4) 3_445 5 ?
C21 O22 P2 119.5(2) . . ?
Cl1 C1 Cl1 109.02(15) . 6 ?
Cl1 C1 P1 109.17(11) . . ?
Cl1 C1 P1 109.17(11) 6 . ?
Cl1 C1 P2 108.91(11) . . ?
Cl1 C1 P2 108.91(11) 6 . ?
P1 C1 P2 111.62(15) . . ?
O13 C11 O12 121.6(3) . . ?
O13 C11 C12 125.1(3) . . ?
O12 C11 C12 113.2(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O23 C21 O22 122.3(3) . . ?
O23 C21 C22 126.0(3) . . ?
O22 C21 C22 111.7(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 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 H1 O11 0.84 1.97 2.7866(19) 165.4 3_545
O2 H2A O11 0.84 2.18 2.969(2) 156.8 .
O2 H2A O23 0.84 2.54 3.043(2) 120.2 3
O2 H2B O11 0.82 2.04 2.846(2) 168.2 2

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.096

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

data_structure(3)
_database_code_depnum_ccdc_archive 'CCDC 764809'
#TrackingRef 'CIF_SKunnas-Hiltunen'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C H10 Cl2 O11 P2 Sr2'
_chemical_formula_sum            'C H10 Cl2 O11 P2 Sr2'
_chemical_formula_weight         506.17

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'
Sr Sr -1.5307 3.2498 '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
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   5.7600(2)
_cell_length_b                   12.1202(3)
_cell_length_c                   18.0234(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.303(2)
_cell_angle_gamma                90.00
_cell_volume                     1252.87(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      26.00

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    9.243
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.2996
_exptl_absorpt_correction_T_max  0.8716
_exptl_absorpt_process_details   'XPREP in SHELXTL v.5.1 (Bruker AXS, 1998)'

_publ_section_exptl_refinement   
;The H~2~O hydrogen atoms were located from the difference Fourier map but
constrained to ride on their parent atom, with U~iso~ = 1.5
U~eq~(parent atom).
The highest peak is located 1.04 \%A from atom O5 and the deepest hole is
located 0.61 \%A from atom Sr2.
;

_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       multi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13434
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2448
_reflns_number_gt                2255
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in SHELXTL v.5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0300P)^2^+1.6000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2448
_refine_ls_number_parameters     164
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0599
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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
Sr1 Sr 0.25652(4) 0.33869(2) 0.215632(16) 0.01121(10) Uani 1 1 d . . .
Sr2 Sr 0.22182(5) 0.07536(2) 0.331556(16) 0.01346(11) Uani 1 1 d . . .
Cl1 Cl 1.07331(12) 0.13253(6) 0.10801(4) 0.01343(17) Uani 1 1 d . . .
Cl2 Cl 0.59153(12) 0.06551(6) 0.07392(4) 0.01425(17) Uani 1 1 d . . .
P1 P 0.75360(12) 0.14204(6) 0.22693(4) 0.01017(17) Uani 1 1 d . . .
P2 P 0.71713(13) 0.30460(6) 0.08663(4) 0.01106(17) Uani 1 1 d . . .
O1 O 0.3104(4) 0.29244(19) 0.36148(13) 0.0212(5) Uani 1 1 d . . .
H1A H 0.2051 0.3283 0.3904 0.032 Uiso 1 1 d R . .
H1B H 0.4551 0.3068 0.3850 0.032 Uiso 1 1 d R . .
O2 O 0.6628(4) 0.42191(17) 0.26608(13) 0.0165(5) Uani 1 1 d . . .
H2A H 0.7543 0.3709 0.2718 0.025 Uiso 1 1 d R . .
H2B H 0.6548 0.4477 0.3109 0.025 Uiso 1 1 d R . .
O3 O 0.6351(4) 0.05625(19) 0.39751(13) 0.0211(5) Uani 1 1 d . . .
H3A H 0.6651 -0.0093 0.4141 0.032 Uiso 1 1 d R . .
H3B H 0.6851 0.1084 0.4313 0.032 Uiso 1 1 d R . .
O4 O 0.1772(4) 0.1136(2) 0.47048(13) 0.0233(5) Uani 1 1 d . . .
H4A H 0.0429 0.1390 0.4762 0.035 Uiso 1 1 d R . .
H4B H 0.2700 0.1610 0.4944 0.035 Uiso 1 1 d R . .
O5 O -0.1027(5) 0.3636(2) 0.41525(15) 0.0314(6) Uani 1 1 d . . .
H5A H -0.0735 0.4293 0.4347 0.047 Uiso 1 1 d R . .
H5B H -0.1449 0.3183 0.4478 0.047 Uiso 1 1 d R . .
O11 O 0.5017(3) 0.16429(15) 0.23921(12) 0.0120(4) Uani 1 1 d . . .
O12 O 0.8393(3) 0.02603(16) 0.24494(12) 0.0124(4) Uani 1 1 d . . .
O13 O 0.9271(3) 0.22526(16) 0.26392(12) 0.0125(4) Uani 1 1 d . . .
O21 O 0.4687(4) 0.33128(16) 0.10108(13) 0.0153(5) Uani 1 1 d . . .
O22 O 0.7499(4) 0.29510(17) 0.00399(12) 0.0170(5) Uani 1 1 d . . .
O23 O 0.8955(3) 0.37930(16) 0.12867(12) 0.0135(4) Uani 1 1 d . . .
C1 C 0.7765(5) 0.1631(2) 0.12519(17) 0.0111(6) 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
Sr1 0.00833(15) 0.00839(16) 0.01708(18) -0.00137(10) 0.00208(11) 0.00013(9)
Sr2 0.01373(16) 0.01051(17) 0.01580(18) 0.00001(10) -0.00037(12) -0.00117(10)
Cl1 0.0096(3) 0.0129(4) 0.0180(4) -0.0008(3) 0.0025(3) 0.0009(2)
Cl2 0.0126(3) 0.0126(4) 0.0174(4) -0.0032(3) 0.0002(3) -0.0025(3)
P1 0.0095(4) 0.0077(4) 0.0134(4) 0.0007(3) 0.0020(3) 0.0000(3)
P2 0.0103(4) 0.0098(4) 0.0131(4) 0.0013(3) 0.0016(3) 0.0009(3)
O1 0.0237(12) 0.0180(12) 0.0220(13) -0.0044(9) 0.0026(10) -0.0039(9)
O2 0.0152(11) 0.0168(11) 0.0180(13) -0.0033(9) 0.0041(9) -0.0010(8)
O3 0.0283(12) 0.0161(11) 0.0178(13) -0.0011(9) -0.0041(10) 0.0032(9)
O4 0.0170(11) 0.0312(14) 0.0215(13) -0.0055(11) 0.0007(10) 0.0013(10)
O5 0.0530(17) 0.0180(13) 0.0244(15) 0.0034(10) 0.0101(12) 0.0036(11)
O11 0.0106(10) 0.0096(10) 0.0159(12) 0.0014(8) 0.0021(8) 0.0013(8)
O12 0.0129(10) 0.0065(10) 0.0177(12) 0.0023(8) 0.0014(8) 0.0004(8)
O13 0.0115(10) 0.0097(10) 0.0164(12) 0.0000(8) 0.0018(8) -0.0012(8)
O21 0.0117(10) 0.0140(11) 0.0203(12) 0.0047(9) 0.0021(9) 0.0030(8)
O22 0.0206(11) 0.0163(11) 0.0143(12) 0.0022(9) 0.0038(9) 0.0029(9)
O23 0.0146(11) 0.0081(10) 0.0179(12) -0.0006(8) 0.0014(9) -0.0005(8)
C1 0.0074(13) 0.0120(14) 0.0142(16) -0.0008(11) 0.0020(11) 0.0001(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
Sr1 O12 2.457(2) 2_655 ?
Sr1 O21 2.496(2) . ?
Sr1 O23 2.534(2) 1_455 ?
Sr1 O11 2.5557(19) . ?
Sr1 O13 2.560(2) 1_455 ?
Sr1 O2 2.632(2) . ?
Sr1 O1 2.678(2) . ?
Sr2 O3 2.571(2) . ?
Sr2 O4 2.583(2) . ?
Sr2 O23 2.590(2) 2_645 ?
Sr2 O12 2.648(2) 1_455 ?
Sr2 O11 2.651(2) . ?
Sr2 O2 2.686(2) 2_645 ?
Sr2 O13 2.699(2) 1_455 ?
Sr2 O1 2.724(2) . ?
Cl1 C1 1.804(3) . ?
Cl2 C1 1.791(3) . ?
P1 O11 1.512(2) . ?
P1 O12 1.515(2) . ?
P1 O13 1.529(2) . ?
P1 C1 1.868(3) . ?
P2 O21 1.513(2) . ?
P2 O23 1.518(2) . ?
P2 O22 1.523(2) . ?
P2 C1 1.870(3) . ?
O1 H1A 0.9411 . ?
O1 H1B 0.9158 . ?
O2 Sr2 2.686(2) 2_655 ?
O2 H2A 0.8133 . ?
O2 H2B 0.8714 . ?
O3 H3A 0.8603 . ?
O3 H3B 0.9062 . ?
O4 H4A 0.8481 . ?
O4 H4B 0.8709 . ?
O5 H5A 0.8798 . ?
O5 H5B 0.8547 . ?
O12 Sr1 2.457(2) 2_645 ?
O12 Sr2 2.648(2) 1_655 ?
O13 Sr1 2.5598(19) 1_655 ?
O13 Sr2 2.699(2) 1_655 ?
O23 Sr1 2.534(2) 1_655 ?
O23 Sr2 2.590(2) 2_655 ?

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
O12 Sr1 O21 114.37(7) 2_655 . ?
O12 Sr1 O23 78.81(7) 2_655 1_455 ?
O21 Sr1 O23 86.10(7) . 1_455 ?
O12 Sr1 O11 148.39(7) 2_655 . ?
O21 Sr1 O11 78.61(7) . . ?
O23 Sr1 O11 132.28(7) 1_455 . ?
O12 Sr1 O13 101.81(6) 2_655 1_455 ?
O21 Sr1 O13 134.18(7) . 1_455 ?
O23 Sr1 O13 73.92(7) 1_455 1_455 ?
O11 Sr1 O13 85.11(6) . 1_455 ?
O12 Sr1 O2 76.24(7) 2_655 . ?
O21 Sr1 O2 79.16(7) . . ?
O23 Sr1 O2 142.36(7) 1_455 . ?
O11 Sr1 O2 78.44(6) . . ?
O13 Sr1 O2 138.73(7) 1_455 . ?
O12 Sr1 O1 85.32(7) 2_655 . ?
O21 Sr1 O1 141.56(7) . . ?
O23 Sr1 O1 131.45(7) 1_455 . ?
O11 Sr1 O1 69.60(7) . . ?
O13 Sr1 O1 64.92(7) 1_455 . ?
O2 Sr1 O1 73.88(7) . . ?
O3 Sr2 O4 74.86(7) . . ?
O3 Sr2 O23 92.49(7) . 2_645 ?
O4 Sr2 O23 81.04(7) . 2_645 ?
O3 Sr2 O12 159.48(7) . 1_455 ?
O4 Sr2 O12 117.39(7) . 1_455 ?
O23 Sr2 O12 74.45(6) 2_645 1_455 ?
O3 Sr2 O11 74.70(7) . . ?
O4 Sr2 O11 131.04(7) . . ?
O23 Sr2 O11 137.42(6) 2_645 . ?
O12 Sr2 O11 104.05(6) 1_455 . ?
O3 Sr2 O2 88.04(7) . 2_645 ?
O4 Sr2 O2 144.32(7) . 2_645 ?
O23 Sr2 O2 68.45(7) 2_645 2_645 ?
O12 Sr2 O2 72.56(6) 1_455 2_645 ?
O11 Sr2 O2 70.64(6) . 2_645 ?
O3 Sr2 O13 141.83(7) . 1_455 ?
O4 Sr2 O13 101.68(7) . 1_455 ?
O23 Sr2 O13 124.98(6) 2_645 1_455 ?
O12 Sr2 O13 55.35(6) 1_455 1_455 ?
O11 Sr2 O13 80.58(6) . 1_455 ?
O2 Sr2 O13 110.71(6) 2_645 1_455 ?
O3 Sr2 O1 81.20(7) . . ?
O4 Sr2 O1 70.64(7) . . ?
O23 Sr2 O1 151.67(7) 2_645 . ?
O12 Sr2 O1 117.72(7) 1_455 . ?
O11 Sr2 O1 67.54(6) . . ?
O2 Sr2 O1 138.18(7) 2_645 . ?
O13 Sr2 O1 62.48(7) 1_455 . ?
O11 P1 O12 115.59(11) . . ?
O11 P1 O13 114.59(12) . . ?
O12 P1 O13 109.38(12) . . ?
O11 P1 C1 105.96(13) . . ?
O12 P1 C1 106.62(12) . . ?
O13 P1 C1 103.60(12) . . ?
O21 P2 O23 113.19(12) . . ?
O21 P2 O22 112.91(13) . . ?
O23 P2 O22 113.19(12) . . ?
O21 P2 C1 105.98(12) . . ?
O23 P2 C1 105.63(12) . . ?
O22 P2 C1 105.02(13) . . ?
Sr1 O1 Sr2 90.30(7) . . ?
Sr1 O1 H1A 115.1 . . ?
Sr2 O1 H1A 115.9 . . ?
Sr1 O1 H1B 115.6 . . ?
Sr2 O1 H1B 114.9 . . ?
H1A O1 H1B 105.2 . . ?
Sr1 O2 Sr2 107.76(8) . 2_655 ?
Sr1 O2 H2A 107.3 . . ?
Sr2 O2 H2A 114.4 2_655 . ?
Sr1 O2 H2B 109.7 . . ?
Sr2 O2 H2B 113.3 2_655 . ?
H2A O2 H2B 104.2 . . ?
Sr2 O3 H3A 113.0 . . ?
Sr2 O3 H3B 118.1 . . ?
H3A O3 H3B 111.6 . . ?
Sr2 O4 H4A 110.9 . . ?
Sr2 O4 H4B 119.1 . . ?
H4A O4 H4B 103.0 . . ?
H5A O5 H5B 111.3 . . ?
P1 O11 Sr1 130.25(11) . . ?
P1 O11 Sr2 131.83(11) . . ?
Sr1 O11 Sr2 94.70(6) . . ?
P1 O12 Sr1 147.35(12) . 2_645 ?
P1 O12 Sr2 98.83(10) . 1_655 ?
Sr1 O12 Sr2 103.59(7) 2_645 1_655 ?
P1 O13 Sr1 132.94(12) . 1_655 ?
P1 O13 Sr2 96.40(9) . 1_655 ?
Sr1 O13 Sr2 93.45(6) 1_655 1_655 ?
P2 O21 Sr1 133.89(13) . . ?
P2 O23 Sr1 132.19(11) . 1_655 ?
P2 O23 Sr2 120.23(11) . 2_655 ?
Sr1 O23 Sr2 103.13(7) 1_655 2_655 ?
Cl2 C1 Cl1 107.67(15) . . ?
Cl2 C1 P1 108.88(15) . . ?
Cl1 C1 P1 107.12(15) . . ?
Cl2 C1 P2 109.54(16) . . ?
Cl1 C1 P2 105.56(15) . . ?
P1 C1 P2 117.60(16) . . ?

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 O5 0.94 1.92 2.788(3) 152.9 .
O2 H2A O13 0.81 2.04 2.831(3) 164.9 .
O2 H2B O5 0.87 2.46 2.980(4) 119.1 1_655
O3 H3A O21 0.86 2.09 2.792(3) 138.4 2_645
O3 H3B O22 0.91 1.77 2.671(3) 172.2 4_566
O4 H4A O22 0.85 1.97 2.815(3) 171.7 4_466
O4 H4B O21 0.87 2.15 2.842(3) 136.4 4_566
O5 H5A Cl1 0.88 2.58 3.293(3) 138.6 2_655
O5 H5B O22 0.85 1.84 2.689(3) 170.0 4_466

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.107

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

data_structure(4)
_database_code_depnum_ccdc_archive 'CCDC 764810'
#TrackingRef 'CIF_SKunnas-Hiltunen'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H10 Cl2 K2 O9 P2'
_chemical_formula_sum            'C15 H10 Cl2 K2 O9 P2'
_chemical_formula_weight         545.27

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'
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'
K K 0.2009 0.2494 '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                   6.7201(2)
_cell_length_b                   10.4562(5)
_cell_length_c                   16.0580(8)
_cell_angle_alpha                72.827(2)
_cell_angle_beta                 84.164(3)
_cell_angle_gamma                71.395(3)
_cell_volume                     1021.67(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18759
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7411
_exptl_absorpt_correction_T_max  0.8273
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'

_publ_section_exptl_refinement   
;
The crystal structure was refined with two twin components (twin matrices
[0.998 0.002 0.002 0.999 -0.999 0.001 0.500 0.001 -0.999] and
1.000 0.000 0.000 0.993 -1.000 0.000 0.486 0.000 -1.000].
BASF values were refined to 0.02 and 0.05 respectively.
The hydrogen atoms were positioned geometrically and were also constrained
to ride on their parent atoms, with C---H = 0.95 \%A, and
U~iso~ = 1.2 U~eq~(parent atom).
The highest peak is located 1.89 \%A from atom K2 and the deepest hole is
located 0.85 \%A from atom K1.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4659
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.60
_reflns_number_total             4659
_reflns_number_gt                3566
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond v.3.1f (Brandenburg, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0418P)^2^+1.2831P] 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         4659
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
K1 K -0.30678(11) 0.62603(7) 0.47925(4) 0.01847(17) Uani 1 1 d . . .
K2 K 0.73440(11) 0.04036(7) 0.43531(5) 0.01859(16) Uani 1 1 d . . .
Cl1 Cl 0.50773(12) 0.16813(8) 0.22994(5) 0.02065(18) Uani 1 1 d . . .
Cl2 Cl 0.08992(13) 0.17989(8) 0.18693(5) 0.02199(19) Uani 1 1 d . . .
P1 P 0.15461(12) 0.23778(8) 0.35125(5) 0.01415(18) Uani 1 1 d . . .
P2 P 0.32880(12) -0.05856(8) 0.33285(5) 0.01398(18) Uani 1 1 d . . .
O11 O 0.3082(3) 0.1956(2) 0.42161(14) 0.0190(5) Uani 1 1 d . . .
O13 O -0.0646(3) 0.2369(2) 0.37162(15) 0.0229(5) Uani 1 1 d . . .
O12 O 0.1525(3) 0.3903(2) 0.28316(14) 0.0186(5) Uani 1 1 d . . .
O14 O 0.0342(3) 0.5194(2) 0.37771(14) 0.0198(5) Uani 1 1 d . . .
O21 O 0.5182(4) -0.1007(2) 0.38604(14) 0.0201(5) Uani 1 1 d . . .
O23 O 0.1316(3) -0.0834(2) 0.37435(15) 0.0206(5) Uani 1 1 d . . .
O22 O 0.3865(3) -0.1186(2) 0.24656(13) 0.0152(4) Uani 1 1 d . . .
O24 O 0.4928(4) -0.3457(2) 0.32499(14) 0.0203(5) Uani 1 1 d . . .
O9 O -0.2751(4) 0.3546(2) 0.49830(15) 0.0245(5) Uani 1 1 d . . .
C1 C 0.2685(5) 0.1313(3) 0.27392(19) 0.0142(6) Uani 1 1 d . . .
C11 C 0.0710(5) 0.5137(3) 0.3040(2) 0.0143(6) Uani 1 1 d . . .
C12 C 0.0305(5) 0.6358(3) 0.2250(2) 0.0152(6) Uani 1 1 d . . .
C13 C 0.0555(5) 0.6167(3) 0.1421(2) 0.0182(7) Uani 1 1 d . . .
H13 H 0.1087 0.5246 0.1353 0.022 Uiso 1 1 calc R . .
C14 C 0.0029(5) 0.7317(4) 0.0695(2) 0.0262(8) Uani 1 1 d . . .
H14 H 0.0198 0.7191 0.0127 0.031 Uiso 1 1 calc R . .
C15 C -0.0744(5) 0.8650(4) 0.0806(3) 0.0297(9) Uani 1 1 d . . .
H15 H -0.1152 0.9440 0.0311 0.036 Uiso 1 1 calc R . .
C16 C -0.0933(5) 0.8850(3) 0.1623(3) 0.0292(8) Uani 1 1 d . . .
H16 H -0.1425 0.9776 0.1684 0.035 Uiso 1 1 calc R . .
C17 C -0.0408(5) 0.7702(3) 0.2361(2) 0.0210(7) Uani 1 1 d . . .
H17 H -0.0533 0.7834 0.2927 0.025 Uiso 1 1 calc R . .
C21 C 0.4629(5) -0.2592(3) 0.2553(2) 0.0148(6) Uani 1 1 d . . .
C22 C 0.5021(5) -0.2911(3) 0.1697(2) 0.0155(6) Uani 1 1 d . . .
C23 C 0.5889(5) -0.4323(3) 0.1706(2) 0.0182(7) Uani 1 1 d . . .
H23 H 0.6180 -0.5039 0.2244 0.022 Uiso 1 1 calc R . .
C24 C 0.6319(5) -0.4665(4) 0.0921(2) 0.0234(7) Uani 1 1 d . . .
H24 H 0.6898 -0.5622 0.0921 0.028 Uiso 1 1 calc R . .
C25 C 0.5910(5) -0.3621(4) 0.0136(2) 0.0231(7) Uani 1 1 d . . .
H25 H 0.6226 -0.3862 -0.0399 0.028 Uiso 1 1 calc R . .
C26 C 0.5038(5) -0.2224(3) 0.0133(2) 0.0208(7) Uani 1 1 d . . .
H26 H 0.4746 -0.1510 -0.0405 0.025 Uiso 1 1 calc R . .
C27 C 0.4594(5) -0.1869(3) 0.0912(2) 0.0179(6) Uani 1 1 d . . .
H27 H 0.3997 -0.0912 0.0909 0.021 Uiso 1 1 calc R . .

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
K1 0.0232(4) 0.0117(3) 0.0182(4) -0.0064(3) -0.0030(3) 0.0006(3)
K2 0.0173(3) 0.0158(3) 0.0223(4) -0.0052(3) -0.0012(3) -0.0043(3)
Cl1 0.0221(4) 0.0171(4) 0.0218(4) -0.0070(3) 0.0066(3) -0.0055(3)
Cl2 0.0289(4) 0.0162(4) 0.0184(4) -0.0046(3) -0.0095(3) -0.0009(3)
P1 0.0178(4) 0.0090(3) 0.0146(4) -0.0047(3) 0.0003(3) -0.0016(3)
P2 0.0175(4) 0.0087(3) 0.0146(4) -0.0049(3) -0.0010(3) -0.0007(3)
O11 0.0259(12) 0.0119(10) 0.0177(11) -0.0072(9) -0.0043(9) 0.0002(9)
O13 0.0217(12) 0.0175(11) 0.0324(14) -0.0140(10) 0.0044(10) -0.0046(9)
O12 0.0292(12) 0.0079(10) 0.0161(11) -0.0029(8) 0.0028(9) -0.0032(9)
O14 0.0210(12) 0.0178(11) 0.0187(12) -0.0080(9) -0.0004(9) -0.0008(9)
O21 0.0283(13) 0.0104(10) 0.0208(12) -0.0049(9) -0.0082(10) -0.0021(9)
O23 0.0231(12) 0.0115(10) 0.0233(12) -0.0037(9) 0.0039(9) -0.0021(9)
O22 0.0212(11) 0.0097(10) 0.0143(11) -0.0071(8) 0.0000(9) -0.0006(9)
O24 0.0273(12) 0.0142(11) 0.0192(12) -0.0059(9) -0.0026(10) -0.0040(9)
O9 0.0295(13) 0.0153(11) 0.0253(13) -0.0060(10) 0.0071(10) -0.0042(10)
C1 0.0160(15) 0.0132(14) 0.0107(15) -0.0019(11) -0.0030(12) -0.0010(12)
C11 0.0113(14) 0.0114(14) 0.0198(17) -0.0072(12) 0.0002(12) -0.0004(11)
C12 0.0102(14) 0.0097(14) 0.0231(17) -0.0017(12) -0.0011(12) -0.0021(11)
C13 0.0145(15) 0.0161(15) 0.0226(17) -0.0038(13) -0.0007(13) -0.0041(12)
C14 0.0177(17) 0.0330(19) 0.0225(18) 0.0019(15) -0.0007(14) -0.0091(15)
C15 0.0166(17) 0.0232(18) 0.036(2) 0.0097(15) -0.0028(15) -0.0040(14)
C16 0.0165(17) 0.0123(16) 0.051(2) -0.0004(15) -0.0005(16) -0.0018(13)
C17 0.0162(16) 0.0150(15) 0.0314(19) -0.0082(13) 0.0005(14) -0.0028(13)
C21 0.0122(15) 0.0118(14) 0.0210(17) -0.0071(13) -0.0016(12) -0.0018(12)
C22 0.0128(15) 0.0162(14) 0.0198(16) -0.0094(12) 0.0002(12) -0.0036(12)
C23 0.0152(15) 0.0157(15) 0.0241(17) -0.0080(13) -0.0029(13) -0.0023(12)
C24 0.0207(17) 0.0204(16) 0.034(2) -0.0179(15) 0.0005(14) -0.0035(13)
C25 0.0183(17) 0.0338(19) 0.0232(18) -0.0180(15) 0.0035(14) -0.0079(14)
C26 0.0187(16) 0.0265(17) 0.0198(17) -0.0092(14) 0.0005(13) -0.0080(14)
C27 0.0190(16) 0.0161(15) 0.0204(16) -0.0071(12) -0.0010(13) -0.0057(13)

_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
K1 O9 2.703(2) . ?
K1 O21 2.734(2) 1_465 ?
K1 O9 2.746(3) 2_466 ?
K1 O11 2.784(2) 2_566 ?
K1 O14 2.799(2) . ?
K1 O14 2.821(2) 2_566 ?
K1 O24 2.834(2) 1_465 ?
K1 P2 3.7200(10) 1_465 ?
K1 P1 3.7770(10) 2_566 ?
K1 K1 4.1206(13) 2_566 ?
K1 K1 4.1367(14) 2_466 ?
K1 K2 4.2352(10) 2_566 ?
K2 O21 2.684(2) . ?
K2 O13 2.710(2) 1_655 ?
K2 O23 2.788(2) 1_655 ?
K2 O11 2.800(2) . ?
K2 O11 2.901(2) 2_656 ?
K2 O21 3.302(2) 2_656 ?
K2 Cl1 3.4789(11) . ?
K2 P1 3.7431(10) 2_656 ?
K2 P2 3.7578(11) 2_656 ?
K2 K2 3.7793(14) 2_656 ?
K2 P2 3.8628(10) . ?
K2 K2 4.0401(13) 2_756 ?
Cl1 C1 1.799(3) . ?
Cl2 C1 1.784(3) . ?
P1 O13 1.478(2) . ?
P1 O11 1.479(2) . ?
P1 O12 1.642(2) . ?
P1 C1 1.857(3) . ?
P1 K2 3.7431(10) 2_656 ?
P1 K1 3.7771(10) 2_566 ?
P2 O21 1.478(2) . ?
P2 O23 1.485(2) . ?
P2 O22 1.648(2) . ?
P2 C1 1.859(3) . ?
P2 K1 3.7201(10) 1_645 ?
P2 K2 3.7579(11) 2_656 ?
O11 K1 2.784(2) 2_566 ?
O11 K2 2.901(2) 2_656 ?
O13 K2 2.710(2) 1_455 ?
O12 C11 1.358(3) . ?
O14 C11 1.199(4) . ?
O14 K1 2.821(2) 2_566 ?
O21 K1 2.734(2) 1_645 ?
O21 K2 3.302(2) 2_656 ?
O23 K2 2.788(2) 1_455 ?
O22 C21 1.362(3) . ?
O24 C21 1.202(4) . ?
O24 K1 2.834(2) 1_645 ?
O9 K1 2.746(3) 2_466 ?
C11 C12 1.486(4) . ?
C12 C13 1.388(5) . ?
C12 C17 1.393(4) . ?
C13 C14 1.384(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.375(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.395(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C21 C22 1.487(4) . ?
C22 C27 1.386(4) . ?
C22 C23 1.399(4) . ?
C23 C24 1.389(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.386(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.386(4) . ?
C26 H26 0.9500 . ?
C27 H27 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
O9 K1 O21 145.82(7) . 1_465 ?
O9 K1 O9 81.22(7) . 2_466 ?
O21 K1 O9 79.99(7) 1_465 2_466 ?
O9 K1 O11 140.45(7) . 2_566 ?
O21 K1 O11 70.20(6) 1_465 2_566 ?
O9 K1 O11 96.43(7) 2_466 2_566 ?
O9 K1 O14 72.27(7) . . ?
O21 K1 O14 104.92(7) 1_465 . ?
O9 K1 O14 138.65(7) 2_466 . ?
O11 K1 O14 124.19(7) 2_566 . ?
O9 K1 O14 77.19(7) . 2_566 ?
O21 K1 O14 136.99(7) 1_465 2_566 ?
O9 K1 O14 119.02(7) 2_466 2_566 ?
O11 K1 O14 69.56(6) 2_566 2_566 ?
O14 K1 O14 85.70(7) . 2_566 ?
O9 K1 O24 79.74(7) . 1_465 ?
O21 K1 O24 66.60(6) 1_465 1_465 ?
O9 K1 O24 66.19(7) 2_466 1_465 ?
O11 K1 O24 135.46(6) 2_566 1_465 ?
O14 K1 O24 78.09(7) . 1_465 ?
O14 K1 O24 154.96(6) 2_566 1_465 ?
O9 K1 P2 126.76(6) . 1_465 ?
O21 K1 P2 19.88(5) 1_465 1_465 ?
O9 K1 P2 64.62(5) 2_466 1_465 ?
O11 K1 P2 85.43(5) 2_566 1_465 ?
O14 K1 P2 107.49(5) . 1_465 ?
O14 K1 P2 154.88(5) 2_566 1_465 ?
O24 K1 P2 50.05(4) 1_465 1_465 ?
O9 K1 P1 125.17(6) . 2_566 ?
O21 K1 P1 87.92(5) 1_465 2_566 ?
O9 K1 P1 108.21(5) 2_466 2_566 ?
O11 K1 P1 19.47(4) 2_566 2_566 ?
O14 K1 P1 112.94(5) . 2_566 ?
O14 K1 P1 50.45(5) 2_566 2_566 ?
O24 K1 P1 154.36(5) 1_465 2_566 ?
P2 K1 P1 104.44(2) 1_465 2_566 ?
O9 K1 K1 68.98(5) . 2_566 ?
O21 K1 K1 132.49(6) 1_465 2_566 ?
O9 K1 K1 147.37(6) 2_466 2_566 ?
O11 K1 K1 98.20(5) 2_566 2_566 ?
O14 K1 K1 43.06(5) . 2_566 ?
O14 K1 K1 42.65(5) 2_566 2_566 ?
O24 K1 K1 118.69(5) 1_465 2_566 ?
P2 K1 K1 145.49(3) 1_465 2_566 ?
P1 K1 K1 80.15(2) 2_566 2_566 ?
O9 K1 K1 41.00(5) . 2_466 ?
O21 K1 K1 115.16(5) 1_465 2_466 ?
O9 K1 K1 40.22(5) 2_466 2_466 ?
O11 K1 K1 125.33(6) 2_566 2_466 ?
O14 K1 K1 107.42(5) . 2_466 ?
O14 K1 K1 100.21(5) 2_566 2_466 ?
O24 K1 K1 67.40(5) 1_465 2_466 ?
P2 K1 K1 96.12(3) 1_465 2_466 ?
P1 K1 K1 125.72(3) 2_566 2_466 ?
K1 K1 K1 108.95(3) 2_566 2_466 ?
O9 K1 K2 135.37(6) . 2_566 ?
O21 K1 K2 51.21(5) 1_465 2_566 ?
O9 K1 K2 59.41(5) 2_466 2_566 ?
O11 K1 K2 40.81(5) 2_566 2_566 ?
O14 K1 K2 152.06(5) . 2_566 ?
O14 K1 K2 102.81(5) 2_566 2_566 ?
O24 K1 K2 100.39(5) 1_465 2_566 ?
P2 K1 K2 55.925(18) 1_465 2_566 ?
P1 K1 K2 58.646(17) 2_566 2_566 ?
K1 K1 K2 138.76(3) 2_566 2_566 ?
K1 K1 K2 97.31(2) 2_466 2_566 ?
O21 K2 O13 142.44(7) . 1_655 ?
O21 K2 O23 99.18(7) . 1_655 ?
O13 K2 O23 70.47(7) 1_655 1_655 ?
O21 K2 O11 70.44(6) . . ?
O13 K2 O11 104.05(7) 1_655 . ?
O23 K2 O11 155.93(7) 1_655 . ?
O21 K2 O11 69.12(6) . 2_656 ?
O13 K2 O11 146.73(7) 1_655 2_656 ?
O23 K2 O11 99.37(7) 1_655 2_656 ?
O11 K2 O11 96.97(6) . 2_656 ?
O21 K2 O21 102.46(6) . 2_656 ?
O13 K2 O21 107.22(6) 1_655 2_656 ?
O23 K2 O21 141.94(6) 1_655 2_656 ?
O11 K2 O21 62.03(6) . 2_656 ?
O11 K2 O21 60.92(6) 2_656 2_656 ?
O21 K2 Cl1 59.89(5) . . ?
O13 K2 Cl1 84.29(5) 1_655 . ?
O23 K2 Cl1 93.96(5) 1_655 . ?
O11 K2 Cl1 61.99(5) . . ?
O11 K2 Cl1 128.71(5) 2_656 . ?
O21 K2 Cl1 123.98(4) 2_656 . ?
O21 K2 P1 89.36(5) . 2_656 ?
O13 K2 P1 125.48(5) 1_655 2_656 ?
O23 K2 P1 89.99(5) 1_655 2_656 ?
O11 K2 P1 110.97(5) . 2_656 ?
O11 K2 P1 21.27(4) 2_656 2_656 ?
O21 K2 P1 59.59(4) 2_656 2_656 ?
Cl1 K2 P1 149.25(3) . 2_656 ?
O21 K2 P2 117.64(6) . 2_656 ?
O13 K2 P2 98.07(5) 1_655 2_656 ?
O23 K2 P2 119.20(5) 1_655 2_656 ?
O11 K2 P2 84.49(5) . 2_656 ?
O11 K2 P2 58.28(4) 2_656 2_656 ?
O21 K2 P2 23.02(4) 2_656 2_656 ?
Cl1 K2 P2 145.71(3) . 2_656 ?
P1 K2 P2 47.744(18) 2_656 2_656 ?
O21 K2 K2 58.56(5) . 2_656 ?
O13 K2 K2 145.25(6) 1_655 2_656 ?
O23 K2 K2 143.26(5) 1_655 2_656 ?
O11 K2 K2 49.64(5) . 2_656 ?
O11 K2 K2 47.33(5) 2_656 2_656 ?
O21 K2 K2 43.90(4) 2_656 2_656 ?
Cl1 K2 K2 97.59(3) . 2_656 ?
P1 K2 K2 63.24(2) 2_656 2_656 ?
P2 K2 K2 61.66(2) 2_656 2_656 ?
O21 K2 P2 15.91(4) . . ?
O13 K2 P2 131.87(6) 1_655 . ?
O23 K2 P2 108.02(5) 1_655 . ?
O11 K2 P2 57.30(5) . . ?
O11 K2 P2 81.28(5) 2_656 . ?
O21 K2 P2 100.98(4) 2_656 . ?
Cl1 K2 P2 47.586(19) . . ?
P1 K2 P2 102.34(2) 2_656 . ?
P2 K2 P2 120.56(2) 2_656 . ?
K2 K2 P2 58.90(2) 2_656 . ?
O21 K2 K2 138.94(5) . 2_756 ?
O13 K2 K2 66.48(5) 1_655 2_756 ?
O23 K2 K2 57.48(5) 1_655 2_756 ?
O11 K2 K2 143.28(5) . 2_756 ?
O11 K2 K2 81.22(5) 2_656 2_756 ?
O21 K2 K2 86.14(4) 2_656 2_756 ?
Cl1 K2 K2 143.94(3) . 2_756 ?
P1 K2 K2 60.32(2) 2_656 2_756 ?
P2 K2 K2 63.22(2) 2_656 2_756 ?
K2 K2 K2 118.46(3) 2_656 2_756 ?
P2 K2 K2 154.76(3) . 2_756 ?
C1 Cl1 K2 91.74(9) . . ?
O13 P1 O11 120.90(14) . . ?
O13 P1 O12 108.74(12) . . ?
O11 P1 O12 110.93(13) . . ?
O13 P1 C1 109.05(13) . . ?
O11 P1 C1 107.99(13) . . ?
O12 P1 C1 96.45(12) . . ?
O13 P1 K2 83.42(10) . 2_656 ?
O11 P1 K2 45.36(9) . 2_656 ?
O12 P1 K2 154.27(9) . 2_656 ?
C1 P1 K2 100.86(9) . 2_656 ?
O13 P1 K1 106.05(9) . 2_566 ?
O11 P1 K1 38.85(8) . 2_566 ?
O12 P1 K1 85.39(8) . 2_566 ?
C1 P1 K1 142.08(10) . 2_566 ?
K2 P1 K1 69.26(2) 2_656 2_566 ?
O21 P2 O23 120.17(14) . . ?
O21 P2 O22 110.34(12) . . ?
O23 P2 O22 110.21(12) . . ?
O21 P2 C1 108.45(13) . . ?
O23 P2 C1 107.97(13) . . ?
O22 P2 C1 97.18(12) . . ?
O21 P2 K1 38.98(8) . 1_645 ?
O23 P2 K1 96.35(9) . 1_645 ?
O22 P2 K1 94.43(7) . 1_645 ?
C1 P2 K1 147.30(10) . 1_645 ?
O21 P2 K2 60.91(9) . 2_656 ?
O23 P2 K2 67.11(9) . 2_656 ?
O22 P2 K2 162.23(8) . 2_656 ?
C1 P2 K2 100.31(9) . 2_656 ?
K1 P2 K2 68.99(2) 1_645 2_656 ?
O21 P2 K2 29.86(8) . . ?
O23 P2 K2 126.43(10) . . ?
O22 P2 K2 121.64(8) . . ?
C1 P2 K2 79.33(9) . . ?
K1 P2 K2 68.577(19) 1_645 . ?
K2 P2 K2 59.44(2) 2_656 . ?
P1 O11 K1 121.68(11) . 2_566 ?
P1 O11 K2 131.88(12) . . ?
K1 O11 K2 98.66(7) 2_566 . ?
P1 O11 K2 113.37(12) . 2_656 ?
K1 O11 K2 97.45(7) 2_566 2_656 ?
K2 O11 K2 83.03(6) . 2_656 ?
P1 O13 K2 136.63(12) . 1_455 ?
C11 O12 P1 123.0(2) . . ?
C11 O14 K1 138.97(19) . . ?
C11 O14 K1 126.28(19) . 2_566 ?
K1 O14 K1 94.30(7) . 2_566 ?
P2 O21 K2 134.23(12) . . ?
P2 O21 K1 121.14(12) . 1_645 ?
K2 O21 K1 104.13(7) . 1_645 ?
P2 O21 K2 96.07(11) . 2_656 ?
K2 O21 K2 77.54(6) . 2_656 ?
K1 O21 K2 88.59(6) 1_645 2_656 ?
P2 O23 K2 145.09(12) . 1_455 ?
C21 O22 P2 120.90(19) . . ?
C21 O24 K1 133.6(2) . 1_645 ?
K1 O9 K1 98.78(7) . 2_466 ?
Cl2 C1 Cl1 108.93(16) . . ?
Cl2 C1 P1 109.69(15) . . ?
Cl1 C1 P1 108.05(16) . . ?
Cl2 C1 P2 111.28(16) . . ?
Cl1 C1 P2 109.27(15) . . ?
P1 C1 P2 109.56(15) . . ?
O14 C11 O12 122.7(3) . . ?
O14 C11 C12 125.8(3) . . ?
O12 C11 C12 111.5(3) . . ?
C13 C12 C17 120.7(3) . . ?
C13 C12 C11 121.0(3) . . ?
C17 C12 C11 118.2(3) . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 119.2(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C12 C17 C16 118.4(3) . . ?
C12 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
O24 C21 O22 122.8(3) . . ?
O24 C21 C22 124.9(3) . . ?
O22 C21 C22 112.4(2) . . ?
C27 C22 C23 120.3(3) . . ?
C27 C22 C21 122.3(3) . . ?
C23 C22 C21 117.3(3) . . ?
C24 C23 C22 119.2(3) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.0(3) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C22 C27 C26 119.9(3) . . ?
C22 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.098