#------------------------------------------------------------------------------ #$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/89/4308954.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308954 loop_ _publ_author_name 'Mervi Kontturi' 'Elina Laurila' 'Riikka Mattsson' 'Sirpa Per\"aniemi' 'Jouko J. Veps\"al\"ainen' 'Markku Ahlgr\'en' _publ_contact_author_address ; Department of Chemistry University of Joensuu P.O. Box 111 FI-80101, Joensuu Finland ; _publ_contact_author_email mervi.kontturi@joensuu.fi _publ_contact_author_fax '358 13 2513390' _publ_contact_author_name 'Mervi Kontturi' _publ_contact_author_phone '358 13 2513377' _publ_section_title ; Structures of Bisphosphonate Metal Complexes: Zinc and Cadmium Complexes of Clodronate and Its Partial Ester Derivatives ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2400 _journal_page_last 2406 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C32 H80 Cd4 Cl8 O32 P8, 2(H2 O)' _chemical_formula_sum 'C32 H84 Cd4 Cl8 O34 P8' _chemical_formula_weight 1993.95 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.1647(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 13.9504(2) _cell_length_b 12.3418(2) _cell_length_c 21.0920(2) _cell_measurement_reflns_used 54179 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.00 _cell_measurement_theta_min 1.91 _cell_volume 3621.88(9) _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_collection 'collect (Nonius BV, 1997 - 2000)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 54179 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.91 _exptl_absorpt_coefficient_mu 1.709 _exptl_absorpt_correction_T_max 0.7836 _exptl_absorpt_correction_T_min 0.7836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'XPREP in SHELXTL v.5.1 (Bruker AXS, 1998)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_meas 1.79(2) _exptl_crystal_density_method 'flotation in cyclohexane/bromoform' _exptl_crystal_description cubic _exptl_crystal_F_000 1992 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.587 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.082 _refine_ls_extinction_coef 0.00096(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 399 _refine_ls_number_reflns 7102 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0239 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.0602 _reflns_number_gt 6391 _reflns_number_total 7102 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048329zsi20050201_035527_1.cif _[local]_cod_data_source_block Structure4 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 4308954 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 -0.024619(13) 0.367159(15) 0.027173(8) 0.01498(6) Uani 1 1 d . . . Cd2 Cd 0.226707(14) 0.400272(16) 0.209798(9) 0.01976(6) Uani 1 1 d . . . Cl1 Cl -0.14218(5) 0.23694(6) 0.16811(3) 0.02591(15) Uani 1 1 d . . . Cl2 Cl -0.01121(6) 0.25699(6) 0.28138(3) 0.02977(16) Uani 1 1 d . . . Cl3 Cl 0.30019(5) 0.57420(6) -0.06719(3) 0.02465(15) Uani 1 1 d . . . Cl4 Cl 0.41006(5) 0.56380(6) 0.05461(4) 0.02714(15) Uani 1 1 d . . . P1 P -0.02307(5) 0.43375(5) 0.18415(3) 0.01624(14) Uani 1 1 d . . . P2 P 0.06710(5) 0.21310(5) 0.15594(3) 0.01631(14) Uani 1 1 d . . . P3 P 0.21368(4) 0.46398(5) 0.04111(3) 0.01412(13) Uani 1 1 d . . . P4 P 0.24587(5) 0.71475(5) 0.03830(3) 0.01655(14) Uani 1 1 d . . . O1 O 0.04142(14) 0.31388(17) -0.06378(9) 0.0283(5) Uani 1 1 d . . . H1A H -0.0024 0.2945 -0.0917 0.042 Uiso 1 1 d R . . H1B H 0.0745 0.3654 -0.0776 0.042 Uiso 1 1 d R . . O2 O 0.28944(15) 0.57148(16) 0.21685(9) 0.0299(5) Uani 1 1 d . . . H2A H 0.2947 0.5980 0.1801 0.045 Uiso 1 1 d R . . H2B H 0.3106 0.6210 0.2455 0.045 Uiso 1 1 d R . . O3 O 0.37431(14) 0.31842(19) 0.22040(11) 0.0348(5) Uani 1 1 d . . . H3 H 0.3895 0.2716 0.2541 0.052 Uiso 1 1 d R . . O4 O 0.22002(16) 0.39722(16) 0.31771(9) 0.0295(5) Uani 1 1 d . . . H4 H 0.2225 0.3348 0.3405 0.044 Uiso 1 1 d R . . O5 O 0.08591(14) 0.69157(16) 0.17447(9) 0.0259(4) Uani 1 1 d . . . H5A H 0.0764 0.6254 0.1833 0.039 Uiso 1 1 d R . . H5B H 0.1338 0.6999 0.1533 0.039 Uiso 1 1 d R . . O11 O -0.05654(13) 0.45518(14) 0.11646(8) 0.0176(4) Uani 1 1 d . . . O12 O 0.07561(13) 0.47045(15) 0.20686(9) 0.0206(4) Uani 1 1 d . . . O13 O -0.09593(14) 0.48238(17) 0.23002(9) 0.0254(4) Uani 1 1 d . . . O21 O 0.05743(13) 0.24919(14) 0.08851(8) 0.0186(4) Uani 1 1 d . . . O22 O 0.16063(13) 0.23322(14) 0.19379(8) 0.0197(4) Uani 1 1 d . . . O23 O 0.04302(14) 0.08963(15) 0.16271(9) 0.0224(4) Uani 1 1 d . . . O31 O 0.11018(12) 0.49378(14) 0.02463(8) 0.0156(4) Uani 1 1 d . . . O32 O 0.24501(13) 0.43845(15) 0.10803(8) 0.0204(4) Uani 1 1 d . . . O33 O 0.23522(13) 0.36980(14) -0.00603(9) 0.0191(4) Uani 1 1 d . . . O41 O 0.15398(12) 0.73399(14) -0.00063(9) 0.0195(4) Uani 1 1 d . . . O42 O 0.24663(14) 0.71612(15) 0.10945(8) 0.0223(4) Uani 1 1 d . . . O43 O 0.32594(13) 0.79671(15) 0.01957(9) 0.0223(4) Uani 1 1 d . . . C1 C -0.02684(18) 0.2857(2) 0.19803(12) 0.0186(5) Uani 1 1 d . . . C2 C 0.29136(18) 0.5790(2) 0.01695(12) 0.0176(5) Uani 1 1 d . . . C3 C 0.4561(3) 0.3661(4) 0.1946(2) 0.0591(12) Uani 1 1 d . . . H3A H 0.4426 0.3777 0.1489 0.089 Uiso 1 1 calc R . . H3B H 0.5115 0.3176 0.2017 0.089 Uiso 1 1 calc R . . H3C H 0.4705 0.4357 0.2155 0.089 Uiso 1 1 calc R . . C4 C 0.1662(3) 0.4777(4) 0.34932(19) 0.0613(12) Uani 1 1 d . . . H4A H 0.1603 0.5432 0.3231 0.092 Uiso 1 1 calc R . . H4B H 0.1997 0.4952 0.3905 0.092 Uiso 1 1 calc R . . H4C H 0.1021 0.4494 0.3559 0.092 Uiso 1 1 calc R . . C11 C -0.1811(2) 0.5448(2) 0.20844(14) 0.0263(6) Uani 1 1 d . . . H11 H -0.1909 0.5401 0.1611 0.032 Uiso 1 1 calc R . . C12 C -0.1637(3) 0.6617(3) 0.22770(18) 0.0426(8) Uani 1 1 d . . . H12A H -0.1478 0.6657 0.2737 0.064 Uiso 1 1 calc R . . H12B H -0.2217 0.7043 0.2166 0.064 Uiso 1 1 calc R . . H12C H -0.1101 0.6908 0.2053 0.064 Uiso 1 1 calc R . . C13 C -0.2659(3) 0.4952(3) 0.2375(2) 0.0489(9) Uani 1 1 d . . . H13A H -0.2734 0.4198 0.2235 0.073 Uiso 1 1 calc R . . H13B H -0.3241 0.5360 0.2241 0.073 Uiso 1 1 calc R . . H13C H -0.2556 0.4974 0.2840 0.073 Uiso 1 1 calc R . . C21 C -0.00031(19) 0.0246(2) 0.10939(13) 0.0207(6) Uani 1 1 d . . . H21 H -0.0420 0.0718 0.0804 0.025 Uiso 1 1 calc R . . C22 C 0.0790(2) -0.0225(3) 0.07371(16) 0.0354(7) Uani 1 1 d . . . H22A H 0.1143 0.0361 0.0544 0.053 Uiso 1 1 calc R . . H22B H 0.0516 -0.0710 0.0403 0.053 Uiso 1 1 calc R . . H22C H 0.1230 -0.0635 0.1031 0.053 Uiso 1 1 calc R . . C23 C -0.0608(2) -0.0612(3) 0.13786(16) 0.0354(7) Uani 1 1 d . . . H23A H -0.0195 -0.1090 0.1650 0.053 Uiso 1 1 calc R . . H23B H -0.0940 -0.1038 0.1037 0.053 Uiso 1 1 calc R . . H23C H -0.1083 -0.0267 0.1633 0.053 Uiso 1 1 calc R . . C31 C 0.3202(2) 0.2994(2) 0.00232(14) 0.0234(6) Uani 1 1 d . . . H31 H 0.3758 0.3420 0.0218 0.028 Uiso 1 1 calc R . . C32 C 0.2981(2) 0.2076(2) 0.04564(16) 0.0346(7) Uani 1 1 d . . . H32A H 0.2846 0.2364 0.0874 0.052 Uiso 1 1 calc R . . H32B H 0.3534 0.1585 0.0504 0.052 Uiso 1 1 calc R . . H32C H 0.2418 0.1678 0.0274 0.052 Uiso 1 1 calc R . . C33 C 0.3416(3) 0.2639(3) -0.06359(16) 0.0405(8) Uani 1 1 d . . . H33A H 0.2869 0.2228 -0.0829 0.061 Uiso 1 1 calc R . . H33B H 0.3991 0.2182 -0.0611 0.061 Uiso 1 1 calc R . . H33C H 0.3526 0.3278 -0.0897 0.061 Uiso 1 1 calc R . . C41 C 0.3302(2) 0.8418(2) -0.04438(13) 0.0241(6) Uani 1 1 d . . . H41 H 0.2910 0.7958 -0.0755 0.029 Uiso 1 1 calc R . . C42 C 0.2894(3) 0.9544(3) -0.04489(18) 0.0444(9) Uani 1 1 d . . . H42A H 0.2215 0.9513 -0.0357 0.067 Uiso 1 1 calc R . . H42B H 0.2948 0.9871 -0.0868 0.067 Uiso 1 1 calc R . . H42C H 0.3251 0.9984 -0.0125 0.067 Uiso 1 1 calc R . . C43 C 0.4335(2) 0.8384(4) -0.05968(18) 0.0479(9) Uani 1 1 d . . . H43A H 0.4723 0.8820 -0.0286 0.072 Uiso 1 1 calc R . . H43B H 0.4394 0.8677 -0.1024 0.072 Uiso 1 1 calc R . . H43C H 0.4563 0.7633 -0.0580 0.072 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 Cd1 0.01725(10) 0.01381(10) 0.01347(10) 0.00072(7) -0.00171(7) 0.00110(7) Cd2 0.02222(11) 0.01898(11) 0.01733(10) 0.00112(7) -0.00371(8) 0.00016(7) Cl1 0.0212(3) 0.0260(4) 0.0306(4) 0.0007(3) 0.0022(3) -0.0055(3) Cl2 0.0426(4) 0.0319(4) 0.0150(3) 0.0062(3) 0.0035(3) 0.0006(3) Cl3 0.0346(4) 0.0221(3) 0.0180(3) -0.0024(3) 0.0073(3) -0.0034(3) Cl4 0.0158(3) 0.0279(4) 0.0367(4) 0.0014(3) -0.0047(3) -0.0008(3) P1 0.0185(3) 0.0161(3) 0.0140(3) -0.0009(2) 0.0011(2) 0.0016(3) P2 0.0204(3) 0.0132(3) 0.0148(3) 0.0020(2) -0.0022(3) 0.0012(2) P3 0.0149(3) 0.0133(3) 0.0138(3) 0.0003(2) -0.0013(2) 0.0009(2) P4 0.0180(3) 0.0150(3) 0.0165(3) -0.0020(3) 0.0003(3) -0.0022(3) O1 0.0232(10) 0.0369(12) 0.0251(10) -0.0146(9) 0.0037(8) -0.0073(9) O2 0.0457(13) 0.0223(11) 0.0197(10) -0.0010(8) -0.0105(9) -0.0109(9) O3 0.0245(11) 0.0407(13) 0.0387(12) 0.0136(10) -0.0010(9) 0.0069(9) O4 0.0477(13) 0.0228(11) 0.0173(10) 0.0016(8) -0.0021(9) 0.0059(9) O5 0.0281(10) 0.0207(10) 0.0290(11) 0.0009(8) 0.0030(8) -0.0009(8) O11 0.0219(9) 0.0174(9) 0.0136(8) -0.0007(7) 0.0010(7) 0.0032(7) O12 0.0207(9) 0.0177(9) 0.0228(9) -0.0016(8) -0.0026(7) 0.0001(7) O13 0.0280(10) 0.0312(11) 0.0173(9) -0.0029(8) 0.0042(8) 0.0093(9) O21 0.0225(9) 0.0180(9) 0.0150(9) 0.0038(7) 0.0002(7) 0.0055(7) O22 0.0227(9) 0.0146(9) 0.0208(9) 0.0017(7) -0.0056(7) 0.0009(7) O23 0.0341(11) 0.0136(9) 0.0185(9) 0.0010(7) -0.0046(8) -0.0030(8) O31 0.0160(9) 0.0140(9) 0.0166(9) 0.0029(7) -0.0013(7) 0.0007(7) O32 0.0223(9) 0.0243(10) 0.0140(9) 0.0031(7) -0.0029(7) -0.0001(8) O33 0.0204(9) 0.0152(9) 0.0213(9) -0.0030(7) -0.0017(7) 0.0033(7) O41 0.0178(9) 0.0154(9) 0.0249(10) -0.0005(7) -0.0012(7) -0.0003(7) O42 0.0290(10) 0.0210(10) 0.0170(9) -0.0039(8) 0.0020(8) -0.0032(8) O43 0.0229(10) 0.0207(10) 0.0230(10) 0.0010(8) -0.0015(8) -0.0073(8) C1 0.0209(13) 0.0207(14) 0.0138(12) 0.0023(10) 0.0000(10) -0.0021(10) C2 0.0172(12) 0.0209(14) 0.0145(12) -0.0004(10) -0.0004(10) 0.0000(10) C3 0.035(2) 0.096(4) 0.047(2) 0.028(2) 0.0057(17) 0.010(2) C4 0.089(3) 0.053(3) 0.041(2) -0.0048(19) 0.001(2) 0.013(2) C11 0.0233(14) 0.0293(16) 0.0269(15) -0.0030(12) 0.0059(12) 0.0066(12) C12 0.043(2) 0.0333(19) 0.053(2) -0.0081(16) 0.0128(17) 0.0069(15) C13 0.0348(19) 0.050(2) 0.064(2) -0.0086(19) 0.0226(18) -0.0041(16) C21 0.0250(14) 0.0162(13) 0.0202(13) -0.0026(10) -0.0041(11) 0.0001(11) C22 0.0338(17) 0.0359(18) 0.0371(18) -0.0081(14) 0.0065(14) 0.0017(14) C23 0.0388(18) 0.0237(16) 0.0442(19) -0.0040(14) 0.0074(15) -0.0085(13) C31 0.0212(13) 0.0171(14) 0.0322(15) -0.0019(11) 0.0041(11) 0.0058(11) C32 0.0379(17) 0.0220(16) 0.0452(19) 0.0058(14) 0.0121(15) 0.0102(13) C33 0.050(2) 0.0343(19) 0.0392(19) -0.0002(15) 0.0178(16) 0.0151(16) C41 0.0268(14) 0.0231(15) 0.0224(14) 0.0018(11) 0.0022(11) -0.0057(11) C42 0.061(2) 0.0280(18) 0.045(2) 0.0095(15) 0.0071(17) 0.0069(16) C43 0.0320(18) 0.064(3) 0.049(2) 0.0107(19) 0.0147(16) -0.0018(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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O41 98.82(7) . 3_565 ? O21 Cd1 O11 87.34(6) . . ? O41 Cd1 O11 105.96(7) 3_565 . ? O21 Cd1 O1 94.51(7) . . ? O41 Cd1 O1 89.79(7) 3_565 . ? O11 Cd1 O1 163.70(7) . . ? O21 Cd1 O31 171.97(6) . 3_565 ? O41 Cd1 O31 85.22(6) 3_565 3_565 ? O11 Cd1 O31 84.86(6) . 3_565 ? O1 Cd1 O31 92.44(7) . 3_565 ? O21 Cd1 O31 93.86(6) . . ? O41 Cd1 O31 163.67(6) 3_565 . ? O11 Cd1 O31 84.78(6) . . ? O1 Cd1 O31 78.94(6) . . ? O31 Cd1 O31 83.52(6) 3_565 . ? O32 Cd2 O22 97.02(7) . . ? O32 Cd2 O12 93.67(7) . . ? O22 Cd2 O12 88.64(6) . . ? O32 Cd2 O4 167.94(7) . . ? O22 Cd2 O4 95.02(7) . . ? O12 Cd2 O4 85.91(7) . . ? O32 Cd2 O2 78.32(7) . . ? O22 Cd2 O2 175.04(7) . . ? O12 Cd2 O2 89.97(7) . . ? O4 Cd2 O2 89.63(7) . . ? O32 Cd2 O3 91.27(7) . . ? O22 Cd2 O3 88.08(7) . . ? O12 Cd2 O3 174.37(7) . . ? O4 Cd2 O3 89.83(8) . . ? O2 Cd2 O3 93.68(8) . . ? O11 P1 O12 118.01(11) . . ? O11 P1 O13 110.46(10) . . ? O12 P1 O13 107.97(11) . . ? O11 P1 C1 108.39(11) . . ? O12 P1 C1 106.52(11) . . ? O13 P1 C1 104.62(12) . . ? O21 P2 O22 118.32(11) . . ? O21 P2 O23 111.89(10) . . ? O22 P2 O23 107.21(10) . . ? O21 P2 C1 107.07(11) . . ? O22 P2 C1 106.34(11) . . ? O23 P2 C1 105.10(11) . . ? O32 P3 O31 118.93(10) . . ? O32 P3 O33 112.87(11) . . ? O31 P3 O33 104.98(10) . . ? O32 P3 C2 106.45(11) . . ? O31 P3 C2 108.36(11) . . ? O33 P3 C2 104.27(11) . . ? O41 P4 O42 119.51(11) . . ? O41 P4 O43 110.86(10) . . ? O42 P4 O43 106.83(10) . . ? O41 P4 C2 107.78(11) . . ? O42 P4 C2 105.95(11) . . ? O43 P4 C2 104.89(11) . . ? Cd1 O1 H1A 110.4 . . ? Cd1 O1 H1B 109.6 . . ? H1A O1 H1B 110.7 . . ? Cd2 O2 H2A 110.7 . . ? Cd2 O2 H2B 141.4 . . ? H2A O2 H2B 107.9 . . ? C3 O3 Cd2 121.3(2) . . ? C3 O3 H3 113.8 . . ? Cd2 O3 H3 120.2 . . ? C4 O4 Cd2 120.7(2) . . ? C4 O4 H4 110.0 . . ? Cd2 O4 H4 122.6 . . ? H5A O5 H5B 112.3 . . ? P1 O11 Cd1 130.44(10) . . ? P1 O12 Cd2 136.32(11) . . ? C11 O13 P1 123.85(17) . . ? P2 O21 Cd1 139.82(11) . . ? P2 O22 Cd2 123.83(10) . . ? C21 O23 P2 122.53(16) . . ? P3 O31 Cd1 137.88(10) . 3_565 ? P3 O31 Cd1 124.34(10) . . ? Cd1 O31 Cd1 96.48(6) 3_565 . ? P3 O32 Cd2 156.32(12) . . ? C31 O33 P3 123.40(17) . . ? P4 O41 Cd1 134.15(11) . 3_565 ? C41 O43 P4 123.45(16) . . ? Cl1 C1 Cl2 108.79(14) . . ? Cl1 C1 P1 108.11(14) . . ? Cl2 C1 P1 110.32(14) . . ? Cl1 C1 P2 108.41(14) . . ? Cl2 C1 P2 109.44(14) . . ? P1 C1 P2 111.69(13) . . ? Cl3 C2 Cl4 107.94(13) . . ? Cl3 C2 P4 108.63(14) . . ? Cl4 C2 P4 107.91(13) . . ? Cl3 C2 P3 109.07(13) . . ? Cl4 C2 P3 109.45(14) . . ? P4 C2 P3 113.68(13) . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O13 C11 C13 107.8(3) . . ? O13 C11 C12 107.9(2) . . ? C13 C11 C12 113.2(3) . . ? O13 C11 H11 109.3 . . ? C13 C11 H11 109.3 . . ? C12 C11 H11 109.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O23 C21 C22 108.5(2) . . ? O23 C21 C23 106.8(2) . . ? C22 C21 C23 112.5(3) . . ? O23 C21 H21 109.7 . . ? C22 C21 H21 109.7 . . ? C23 C21 H21 109.7 . . ? 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 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O33 C31 C32 108.6(2) . . ? O33 C31 C33 105.8(2) . . ? C32 C31 C33 113.9(3) . . ? O33 C31 H31 109.5 . . ? C32 C31 H31 109.5 . . ? C33 C31 H31 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O43 C41 C43 106.9(2) . . ? O43 C41 C42 108.5(2) . . ? C43 C41 C42 113.2(3) . . ? O43 C41 H41 109.3 . . ? C43 C41 H41 109.3 . . ? C42 C41 H41 109.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? 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 2.2110(17) . ? Cd1 O41 2.2320(17) 3_565 ? Cd1 O11 2.2464(17) . ? Cd1 O1 2.2842(18) . ? Cd1 O31 2.3184(17) 3_565 ? Cd1 O31 2.4487(17) . ? Cd2 O32 2.2304(18) . ? Cd2 O22 2.2736(18) . ? Cd2 O12 2.2756(18) . ? Cd2 O4 2.2851(19) . ? Cd2 O2 2.288(2) . ? Cd2 O3 2.290(2) . ? Cl1 C1 1.789(3) . ? Cl2 C1 1.791(3) . ? Cl3 C2 1.789(3) . ? Cl4 C2 1.794(3) . ? P1 O11 1.4931(18) . ? P1 O12 1.4946(19) . ? P1 O13 1.5723(19) . ? P1 C1 1.852(3) . ? P2 O21 1.4871(18) . ? P2 O22 1.5001(19) . ? P2 O23 1.5692(19) . ? P2 C1 1.864(3) . ? P3 O32 1.4807(18) . ? P3 O31 1.5060(17) . ? P3 O33 1.5727(18) . ? P3 C2 1.879(3) . ? P4 O41 1.4903(18) . ? P4 O42 1.5001(19) . ? P4 O43 1.5783(19) . ? P4 C2 1.858(3) . ? O1 H1A 0.8522 . ? O1 H1B 0.8500 . ? O2 H2A 0.8499 . ? O2 H2B 0.8940 . ? O3 C3 1.426(4) . ? O3 H3 0.9282 . ? O4 C4 1.437(4) . ? O4 H4 0.9072 . ? O5 H5A 0.8499 . ? O5 H5B 0.8359 . ? O13 C11 1.460(3) . ? O23 C21 1.475(3) . ? O31 Cd1 2.3184(17) 3_565 ? O33 C31 1.470(3) . ? O41 Cd1 2.2320(17) 3_565 ? O43 C41 1.464(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C11 C13 1.502(4) . ? C11 C12 1.514(5) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.500(4) . ? C21 C23 1.506(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 C32 1.502(4) . ? C31 C33 1.508(4) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C43 1.500(4) . ? C41 C42 1.502(4) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? 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 O33 0.85 2.61 2.965(3) 106.3 . O1 H1A O5 0.85 2.03 2.830(3) 155.1 3_565 O1 H1B O11 0.85 2.37 3.072(3) 140.6 3_565 O2 H2A O42 0.85 2.16 2.912(3) 148.0 . O2 H2B O22 0.89 1.91 2.798(3) 172.7 2 O5 H5B O42 0.84 1.89 2.729(3) 176.8 . O3 H3 O5 0.93 1.81 2.738(3) 173.7 2_545 O5 H5A O12 0.85 1.98 2.819(3) 171.3 . O4 H4 O42 0.91 1.84 2.733(3) 168.3 2_545 _journal_paper_doi 10.1021/ic048329z