# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof Vadapalli Chandrasekhar' _publ_contact_author_email VC@IITK.AC.IN _publ_section_title ; Assembly of Tetra, Di and Mononuclear Molecular Cadmium Phosphonates using 2,4,6-Triisopropylphenylphosponic acid and Ancillary Ligands ; loop_ _publ_author_name 'Vadapalli Chandrasekhar' 'Ramamoorthy Boomishankar' 'Palani Sasikumar' data_1 _database_code_depnum_ccdc_archive 'CCDC 679265' # Attachment 'VCcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cadmiumphosphonate _chemical_melting_point 445.15 _chemical_formula_moiety 'C101 H132 Cd4 O29 P6' _chemical_formula_sum 'C101 H132 Cd4 O29 P6' _chemical_formula_weight 2445.49 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' 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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.572(5) _cell_length_b 14.766(5) _cell_length_c 16.186(5) _cell_angle_alpha 85.661(5) _cell_angle_beta 80.695(5) _cell_angle_gamma 72.648(5) _cell_volume 3054.1(18) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5370 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.01 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8515 _exptl_absorpt_correction_T_max 0.9215 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16894 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11234 _reflns_number_gt 9247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0674P)^2^+5.6504P] 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 11234 _refine_ls_number_parameters 701 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.3419(4) 0.6518(4) -0.2365(3) 0.0376(12) Uani 1 1 d . A . C2 C 0.4208(4) 0.5972(5) -0.2971(4) 0.0457(14) Uani 1 1 d . . . C3 C 0.4804(5) 0.6443(5) -0.3522(4) 0.0611(19) Uani 1 1 d . A . H3 H 0.5368 0.6073 -0.3897 0.073 Uiso 1 1 calc R . . C4 C 0.4629(5) 0.7388(6) -0.3555(5) 0.074(2) Uani 1 1 d . . . C5 C 0.3822(5) 0.7922(5) -0.2979(4) 0.0578(18) Uani 1 1 d . A . H5 H 0.3696 0.8591 -0.2989 0.069 Uiso 1 1 calc R . . C6 C 0.3198(4) 0.7518(4) -0.2394(4) 0.0422(14) Uani 1 1 d . . . C7 C 0.4462(4) 0.4907(5) -0.3046(4) 0.0487(15) Uani 1 1 d . . . H7 H 0.3870 0.4704 -0.2718 0.058 Uiso 1 1 calc R . . C8 C 0.4572(5) 0.4621(6) -0.3967(4) 0.066(2) Uani 1 1 d . . . H8A H 0.3956 0.4995 -0.4213 0.099 Uiso 1 1 calc R . . H8B H 0.4631 0.3944 -0.3982 0.099 Uiso 1 1 calc R . . H8C H 0.5198 0.4743 -0.4290 0.099 Uiso 1 1 calc R . . C9 C 0.5453(5) 0.4379(5) -0.2670(4) 0.0584(17) Uani 1 1 d . . . H9A H 0.6058 0.4518 -0.3012 0.088 Uiso 1 1 calc R . . H9B H 0.5546 0.3694 -0.2660 0.088 Uiso 1 1 calc R . . H9C H 0.5388 0.4586 -0.2098 0.088 Uiso 1 1 calc R . . C10A C 0.5262(10) 0.7769(9) -0.4319(8) 0.073(4) Uiso 0.70 1 d P A 1 C11A C 0.5829(11) 0.8356(10) -0.3859(8) 0.084(3) Uiso 0.70 1 d P A 1 C12A C 0.4605(10) 0.8393(9) -0.4887(8) 0.087(4) Uiso 0.70 1 d P A 1 C10B C 0.5326(16) 0.8019(15) -0.4060(13) 0.037(5) Uiso 0.30 1 d P A 2 C11B C 0.644(2) 0.770(2) -0.3829(18) 0.079(8) Uiso 0.30 1 d P A 2 C12B C 0.501(2) 0.896(2) -0.4083(18) 0.082(8) Uiso 0.30 1 d P A 2 C13 C 0.2309(4) 0.8178(4) -0.1819(4) 0.0460(15) Uani 1 1 d . A . H13 H 0.1799 0.7818 -0.1596 0.055 Uiso 1 1 calc R . . C14 C 0.1718(5) 0.9075(4) -0.2269(5) 0.0637(19) Uani 1 1 d . . . H14A H 0.1132 0.9445 -0.1877 0.096 Uiso 1 1 calc R A . H14B H 0.1452 0.8898 -0.2741 0.096 Uiso 1 1 calc R . . H14C H 0.2190 0.9458 -0.2475 0.096 Uiso 1 1 calc R . . C15 C 0.2707(6) 0.8442(5) -0.1076(5) 0.0629(18) Uani 1 1 d . . . H15A H 0.3099 0.7863 -0.0799 0.094 Uiso 1 1 calc R A . H15B H 0.2114 0.8790 -0.0678 0.094 Uiso 1 1 calc R . . H15C H 0.3164 0.8842 -0.1268 0.094 Uiso 1 1 calc R . . C16 C -0.0411(4) 0.7622(4) 0.2898(3) 0.0384(13) Uani 1 1 d . C . C17 C -0.1434(5) 0.7784(4) 0.3325(3) 0.0414(14) Uani 1 1 d . . . C18 C -0.1770(6) 0.8457(5) 0.3952(4) 0.060(2) Uani 1 1 d . C . H18 H -0.2452 0.8557 0.4256 0.073 Uiso 1 1 calc R . . C19 C -0.1153(7) 0.8985(4) 0.4152(4) 0.064(2) Uani 1 1 d . . . C20 C -0.0208(6) 0.8871(4) 0.3679(4) 0.060(2) Uani 1 1 d . C . H20 H 0.0201 0.9261 0.3782 0.072 Uiso 1 1 calc R . . C21 C 0.0197(5) 0.8209(4) 0.3044(3) 0.0408(14) Uani 1 1 d . . . C22 C -0.2211(5) 0.7309(4) 0.3131(4) 0.0484(15) Uani 1 1 d . . . H22 H -0.1952 0.7037 0.2563 0.058 Uiso 1 1 calc R . . C23 C -0.2278(5) 0.6493(5) 0.3741(4) 0.0591(18) Uani 1 1 d . . . H23A H -0.1576 0.6065 0.3769 0.089 Uiso 1 1 calc R . . H23B H -0.2708 0.6145 0.3552 0.089 Uiso 1 1 calc R . . H23C H -0.2594 0.6741 0.4298 0.089 Uiso 1 1 calc R . . C24 C -0.3307(5) 0.8009(6) 0.3100(4) 0.079(3) Uani 1 1 d . . . H24A H -0.3645 0.8189 0.3670 0.119 Uiso 1 1 calc R . . H24B H -0.3728 0.7705 0.2842 0.119 Uiso 1 1 calc R . . H24C H -0.3243 0.8577 0.2768 0.119 Uiso 1 1 calc R . . C26 C -0.1302(7) 0.9154(6) 0.5695(4) 0.071(2) Uani 1 1 d . . . C28 C 0.1238(5) 0.8196(4) 0.2516(4) 0.0491(16) Uani 1 1 d . C . H28 H 0.1407 0.7686 0.2099 0.059 Uiso 1 1 calc R . . C29 C 0.2137(6) 0.7968(5) 0.3031(5) 0.073(2) Uani 1 1 d . . . H29A H 0.2003 0.8466 0.3438 0.109 Uiso 1 1 calc R C . H29B H 0.2790 0.7938 0.2658 0.109 Uiso 1 1 calc R . . H29C H 0.2195 0.7355 0.3328 0.109 Uiso 1 1 calc R . . C30 C 0.1138(5) 0.9146(4) 0.2022(4) 0.0574(17) Uani 1 1 d . . . H30A H 0.0598 0.9248 0.1661 0.086 Uiso 1 1 calc R C . H30B H 0.1806 0.9127 0.1676 0.086 Uiso 1 1 calc R . . H30C H 0.0945 0.9665 0.2414 0.086 Uiso 1 1 calc R . . C31 C -0.2131(3) 0.7225(3) -0.0547(3) 0.0240(10) Uani 1 1 d . . . C32 C -0.2951(4) 0.7235(3) -0.0998(3) 0.0305(11) Uani 1 1 d . . . C33 C -0.3560(4) 0.8107(4) -0.1281(3) 0.0348(12) Uani 1 1 d . . . H33 H -0.4085 0.8112 -0.1606 0.042 Uiso 1 1 calc R . . C34 C -0.3430(4) 0.8963(3) -0.1109(3) 0.0331(11) Uani 1 1 d . . . C35 C -0.2659(4) 0.8941(3) -0.0629(3) 0.0299(11) Uani 1 1 d . . . H35 H -0.2567 0.9524 -0.0497 0.036 Uiso 1 1 calc R . . C36 C -0.2015(3) 0.8092(3) -0.0334(3) 0.0264(10) Uani 1 1 d . . . C37 C -0.3243(4) 0.6355(4) -0.1188(4) 0.0412(13) Uani 1 1 d . . . H37 H -0.2888 0.5815 -0.0828 0.049 Uiso 1 1 calc R . . C38 C -0.4404(5) 0.6487(5) -0.1000(5) 0.066(2) Uani 1 1 d . . . H38A H -0.4754 0.6916 -0.1425 0.098 Uiso 1 1 calc R . . H38B H -0.4674 0.6761 -0.0446 0.098 Uiso 1 1 calc R . . H38C H -0.4538 0.5871 -0.1006 0.098 Uiso 1 1 calc R . . C39 C -0.2860(5) 0.6093(5) -0.2090(4) 0.0586(18) Uani 1 1 d . . . H39A H -0.3187 0.6619 -0.2456 0.088 Uiso 1 1 calc R . . H39B H -0.3044 0.5524 -0.2199 0.088 Uiso 1 1 calc R . . H39C H -0.2101 0.5967 -0.2202 0.088 Uiso 1 1 calc R . . C40 C -0.4080(4) 0.9900(4) -0.1451(4) 0.0419(14) Uani 1 1 d . . . H40 H -0.4028 1.0417 -0.1111 0.050 Uiso 1 1 calc R . . C41 C -0.5220(5) 0.9951(5) -0.1372(5) 0.066(2) Uani 1 1 d . . . H41A H -0.5614 1.0576 -0.1572 0.100 Uiso 1 1 calc R . . H41B H -0.5489 0.9851 -0.0783 0.100 Uiso 1 1 calc R . . H41C H -0.5297 0.9458 -0.1708 0.100 Uiso 1 1 calc R . . C42 C -0.3649(6) 1.0077(5) -0.2350(4) 0.0603(18) Uani 1 1 d . . . H42A H -0.2934 1.0111 -0.2379 0.090 Uiso 1 1 calc R . . H42B H -0.4085 1.0678 -0.2561 0.090 Uiso 1 1 calc R . . H42C H -0.3649 0.9558 -0.2693 0.090 Uiso 1 1 calc R . . C43 C -0.1259(4) 0.8174(3) 0.0231(3) 0.0287(11) Uani 1 1 d . . . H43 H -0.0899 0.7516 0.0425 0.034 Uiso 1 1 calc R . . C44 C -0.1830(4) 0.8729(4) 0.1003(3) 0.0399(13) Uani 1 1 d . . . H44A H -0.2177 0.9384 0.0836 0.060 Uiso 1 1 calc R . . H44B H -0.1329 0.8729 0.1377 0.060 Uiso 1 1 calc R . . H44C H -0.2352 0.8434 0.1295 0.060 Uiso 1 1 calc R . . C45 C -0.0414(4) 0.8601(4) -0.0224(4) 0.0448(14) Uani 1 1 d . . . H45A H -0.0037 0.8219 -0.0708 0.067 Uiso 1 1 calc R . . H45B H 0.0075 0.8605 0.0159 0.067 Uiso 1 1 calc R . . H45C H -0.0740 0.9253 -0.0413 0.067 Uiso 1 1 calc R . . C46 C 0.3539(9) 0.6368(9) 0.0617(8) 0.053(3) Uani 0.70 1 d P B 1 C46A C 0.310(2) 0.674(2) 0.0823(18) 0.049(7) Uani 0.30 1 d P B 2 C47 C 0.0415(5) 0.2692(4) 0.2421(4) 0.0516(16) Uani 1 1 d . . . H47A H 0.0140 0.2585 0.1925 0.077 Uiso 1 1 calc R . . H47B H 0.0037 0.2469 0.2924 0.077 Uiso 1 1 calc R . . H47C H 0.1159 0.2343 0.2375 0.077 Uiso 1 1 calc R . . C25A C -0.1268(11) 0.9711(12) 0.4856(9) 0.031(4) Uani 0.40 1 d P C 1 C27A C -0.2384(16) 1.0388(15) 0.4820(13) 0.077(7) Uani 0.40 1 d P C 1 C25B C -0.1822(13) 0.9644(8) 0.4913(8) 0.054(3) Uani 0.60 1 d P C 2 C27B C -0.1642(10) 1.0642(7) 0.4681(7) 0.053(3) Uani 0.60 1 d P C 2 C1S C 0.4162(4) 0.2604(4) 0.8825(4) 0.0478(15) Uani 1 1 d . . . H1S1 H 0.4484 0.2844 0.9228 0.072 Uiso 1 1 calc R . . H1S2 H 0.4699 0.2300 0.8369 0.072 Uiso 1 1 calc R . . H1S3 H 0.3825 0.2139 0.9108 0.072 Uiso 1 1 calc R . . C2S C 0.2067(6) 0.6874(6) 0.5880(5) 0.083(3) Uani 1 1 d . . . H2S1 H 0.1787 0.7371 0.6295 0.125 Uiso 1 1 calc R . . H2S2 H 0.1758 0.7087 0.5366 0.125 Uiso 1 1 calc R . . H2S3 H 0.2826 0.6742 0.5754 0.125 Uiso 1 1 calc R . . C3S C 0.0406(10) 0.3350(8) 0.4732(7) 0.050(3) Uani 0.50 1 d P . . Cd1 Cd 0.12236(2) 0.61195(2) 0.02469(2) 0.02351(10) Uani 1 1 d . . . Cd2 Cd -0.05548(3) 0.48602(2) 0.15624(2) 0.02466(11) Uani 1 1 d . . . O1 O 0.2110(3) 0.6502(2) -0.0883(2) 0.0339(8) Uani 1 1 d . A . O2 O 0.3520(3) 0.5036(3) -0.1262(2) 0.0431(9) Uani 1 1 d . A . O3 O 0.1990(3) 0.5553(2) -0.2092(2) 0.0336(8) Uani 1 1 d . . . O4 O 0.0404(3) 0.6965(2) 0.1333(2) 0.0293(7) Uani 1 1 d . C . O5 O 0.1341(3) 0.6164(2) 0.2502(2) 0.0397(9) Uani 1 1 d . C . O6 O -0.0363(3) 0.5883(2) 0.2384(2) 0.0349(8) Uani 1 1 d . C . O7 O -0.0085(2) 0.6265(2) -0.05038(19) 0.0243(7) Uani 1 1 d . . . O8 O -0.1170(2) 0.5294(2) -0.07601(19) 0.0246(7) Uani 1 1 d . . . O9 O -0.1445(2) 0.5960(2) 0.06919(19) 0.0253(7) Uani 1 1 d . . . O10 O 0.2670(3) 0.5989(3) 0.0937(2) 0.0429(9) Uani 1 1 d . . . O11 O 0.0288(4) 0.3664(3) 0.2477(3) 0.0592(12) Uani 1 1 d . . . O1S O 0.3405(3) 0.3369(3) 0.8495(2) 0.0441(10) Uani 1 1 d . . . H1S H 0.2831 0.3464 0.8812 0.066 Uiso 1 1 calc R . . O2S O 0.1818(4) 0.6027(4) 0.6209(3) 0.0624(13) Uani 1 1 d . . . H2S H 0.1924 0.5933 0.6709 0.094 Uiso 1 1 calc R . . O3S O 0.0071(5) 0.4068(4) 0.4097(4) 0.0254(14) Uani 0.50 1 d P . . P1 P 0.26725(10) 0.58926(9) -0.16153(8) 0.0307(3) Uani 1 1 d . . . P2 P 0.02141(10) 0.66143(9) 0.22205(8) 0.0295(3) Uani 1 1 d . . . P3 P -0.11757(9) 0.61288(8) -0.02473(7) 0.0220(3) Uani 1 1 d . . . C4SA C 0.2190(13) 0.4886(15) 0.4284(9) 0.108(6) Uani 0.60 1 d P D 1 O4SA O 0.1328(5) 0.5249(5) 0.3876(4) 0.0476(17) Uani 0.60 1 d P D 1 C4SB C 0.160(3) 0.4123(17) 0.4212(15) 0.126(12) Uani 0.40 1 d P E 2 O4SB O 0.0909(10) 0.4745(10) 0.3681(8) 0.071(4) Uani 0.40 1 d P E 2 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 C1 0.022(3) 0.050(3) 0.038(3) 0.011(2) -0.003(2) -0.010(2) C2 0.025(3) 0.062(4) 0.045(3) 0.014(3) -0.007(2) -0.006(3) C3 0.033(3) 0.073(5) 0.061(4) 0.020(4) 0.008(3) -0.004(3) C4 0.035(4) 0.085(6) 0.087(5) 0.040(4) 0.002(4) -0.012(4) C5 0.036(3) 0.051(4) 0.081(5) 0.032(3) -0.007(3) -0.014(3) C6 0.025(3) 0.041(3) 0.056(4) 0.020(3) -0.006(2) -0.008(2) C7 0.033(3) 0.063(4) 0.042(3) -0.004(3) -0.001(3) -0.004(3) C8 0.052(4) 0.096(6) 0.041(4) -0.002(4) 0.008(3) -0.016(4) C9 0.042(4) 0.051(4) 0.072(4) -0.007(3) -0.013(3) 0.005(3) C13 0.033(3) 0.036(3) 0.066(4) 0.019(3) -0.005(3) -0.012(2) C14 0.045(4) 0.044(4) 0.089(5) 0.024(4) -0.007(4) -0.002(3) C15 0.067(5) 0.039(4) 0.085(5) 0.008(3) -0.015(4) -0.018(3) C16 0.052(3) 0.026(3) 0.030(3) -0.007(2) -0.019(3) 0.006(2) C17 0.051(4) 0.033(3) 0.030(3) -0.002(2) -0.015(3) 0.008(2) C18 0.088(5) 0.047(4) 0.026(3) -0.002(3) -0.003(3) 0.009(4) C19 0.120(7) 0.029(3) 0.031(3) -0.008(3) -0.024(4) 0.007(4) C20 0.103(6) 0.026(3) 0.046(4) -0.007(3) -0.038(4) 0.003(3) C21 0.059(4) 0.024(3) 0.041(3) -0.006(2) -0.027(3) -0.002(2) C22 0.041(3) 0.060(4) 0.032(3) -0.005(3) -0.008(3) 0.007(3) C23 0.044(4) 0.083(5) 0.048(4) -0.003(3) -0.003(3) -0.016(3) C24 0.052(4) 0.104(6) 0.056(4) -0.023(4) -0.012(3) 0.023(4) C26 0.093(6) 0.089(6) 0.038(4) -0.002(4) -0.002(4) -0.042(5) C28 0.050(4) 0.029(3) 0.074(4) -0.007(3) -0.035(3) -0.005(3) C29 0.079(5) 0.037(4) 0.112(6) -0.001(4) -0.068(5) -0.004(3) C30 0.054(4) 0.040(3) 0.081(5) -0.002(3) -0.026(4) -0.008(3) C31 0.022(2) 0.017(2) 0.030(2) 0.0021(18) -0.0045(19) -0.0017(18) C32 0.023(2) 0.027(3) 0.040(3) -0.003(2) -0.009(2) -0.004(2) C33 0.024(3) 0.033(3) 0.046(3) -0.001(2) -0.017(2) 0.000(2) C34 0.027(3) 0.029(3) 0.039(3) 0.006(2) -0.011(2) -0.002(2) C35 0.026(2) 0.018(2) 0.043(3) -0.001(2) -0.006(2) -0.0010(19) C36 0.021(2) 0.025(2) 0.031(3) 0.003(2) -0.0022(19) -0.0050(19) C37 0.030(3) 0.032(3) 0.065(4) -0.002(3) -0.021(3) -0.007(2) C38 0.041(4) 0.058(4) 0.108(6) -0.027(4) -0.008(4) -0.025(3) C39 0.057(4) 0.050(4) 0.073(5) -0.021(3) -0.015(3) -0.014(3) C40 0.042(3) 0.026(3) 0.055(4) 0.005(2) -0.021(3) 0.000(2) C41 0.036(3) 0.046(4) 0.110(6) 0.024(4) -0.021(4) -0.003(3) C42 0.067(4) 0.046(4) 0.073(5) 0.027(3) -0.025(4) -0.025(3) C43 0.026(3) 0.022(2) 0.037(3) 0.002(2) -0.011(2) -0.0031(19) C44 0.044(3) 0.033(3) 0.041(3) -0.003(2) -0.021(3) -0.001(2) C45 0.041(3) 0.047(3) 0.054(4) 0.004(3) -0.017(3) -0.020(3) C46 0.040(7) 0.078(9) 0.056(7) 0.014(6) -0.011(6) -0.042(6) C46A 0.034(15) 0.063(18) 0.050(15) -0.008(12) 0.004(12) -0.017(12) C47 0.064(4) 0.036(3) 0.043(3) 0.015(3) -0.002(3) -0.006(3) C25A 0.021(7) 0.053(10) 0.028(7) -0.019(6) 0.004(6) -0.024(7) C27A 0.064(12) 0.067(13) 0.095(15) -0.070(12) -0.018(11) 0.009(11) C25B 0.079(10) 0.039(7) 0.048(7) -0.010(5) -0.018(7) -0.016(8) C27B 0.060(7) 0.035(6) 0.063(7) -0.020(5) -0.012(6) -0.007(5) C1S 0.038(3) 0.042(3) 0.056(4) 0.005(3) -0.008(3) -0.001(3) C2S 0.062(5) 0.115(7) 0.081(5) 0.055(5) -0.032(4) -0.041(5) C3S 0.062(8) 0.047(7) 0.043(7) 0.033(5) -0.040(6) -0.012(6) Cd1 0.02335(19) 0.02094(18) 0.02739(19) 0.00048(13) -0.00638(14) -0.00705(13) Cd2 0.0274(2) 0.02296(18) 0.02251(18) 0.00166(13) -0.00457(14) -0.00573(14) O1 0.0331(19) 0.0329(19) 0.0369(19) 0.0045(15) -0.0026(16) -0.0141(15) O2 0.040(2) 0.041(2) 0.041(2) 0.0135(17) -0.0110(17) -0.0014(17) O3 0.0323(19) 0.0346(19) 0.0334(19) 0.0068(15) -0.0018(15) -0.0121(15) O4 0.0336(19) 0.0241(17) 0.0300(18) -0.0024(14) -0.0091(15) -0.0056(14) O5 0.043(2) 0.0286(19) 0.046(2) -0.0088(16) -0.0245(18) 0.0034(16) O6 0.047(2) 0.0306(19) 0.0270(18) -0.0041(15) -0.0042(16) -0.0105(16) O7 0.0223(16) 0.0220(16) 0.0289(17) 0.0044(13) -0.0072(13) -0.0065(13) O8 0.0233(16) 0.0207(16) 0.0291(17) 0.0005(13) -0.0047(13) -0.0050(13) O9 0.0243(17) 0.0212(16) 0.0288(17) 0.0035(13) -0.0059(14) -0.0043(13) O10 0.032(2) 0.048(2) 0.056(2) 0.0050(19) -0.0156(18) -0.0172(17) O11 0.077(3) 0.032(2) 0.081(3) 0.018(2) -0.051(3) -0.019(2) O1S 0.034(2) 0.039(2) 0.048(2) 0.0028(18) 0.0027(17) 0.0024(17) O2S 0.051(3) 0.086(3) 0.048(3) 0.034(2) -0.014(2) -0.022(2) O3S 0.036(4) 0.021(3) 0.018(3) 0.010(2) -0.012(3) -0.006(3) P1 0.0257(7) 0.0298(7) 0.0321(7) 0.0093(5) -0.0023(5) -0.0050(5) P2 0.0355(7) 0.0245(6) 0.0282(7) -0.0043(5) -0.0125(5) -0.0032(5) P3 0.0205(6) 0.0176(6) 0.0276(6) 0.0016(5) -0.0064(5) -0.0041(4) C4SA 0.100(12) 0.172(18) 0.074(10) 0.040(10) -0.040(9) -0.067(12) O4SA 0.039(4) 0.063(5) 0.045(4) 0.029(3) -0.018(3) -0.023(3) C4SB 0.23(3) 0.083(16) 0.096(17) 0.032(13) -0.13(2) -0.050(19) O4SB 0.071(8) 0.083(9) 0.068(8) 0.041(7) -0.034(7) -0.032(7) _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 C1 C6 1.416(8) . ? C1 C2 1.422(8) . ? C1 P1 1.828(5) . ? C2 C3 1.394(8) . ? C2 C7 1.516(9) . ? C3 C4 1.342(10) . ? C3 H3 0.9500 . ? C4 C5 1.399(10) . ? C4 C10A 1.556(14) . ? C4 C10B 1.61(2) . ? C5 C6 1.388(8) . ? C5 H5 0.9500 . ? C6 C13 1.532(8) . ? C7 C9 1.534(8) . ? C7 C8 1.553(8) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10A C12A 1.461(17) . ? C10A C11A 1.605(18) . ? C10B C12B 1.33(3) . ? C10B C11B 1.54(4) . ? C13 C15 1.515(9) . ? C13 C14 1.529(8) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.407(8) . ? C16 C21 1.417(8) . ? C16 P2 1.825(5) . ? C17 C18 1.400(8) . ? C17 C22 1.512(9) . ? C18 C19 1.388(11) . ? C18 H18 0.9500 . ? C19 C20 1.354(11) . ? C19 C25A 1.582(15) . ? C19 C25B 1.606(14) . ? C20 C21 1.400(8) . ? C20 H20 0.9500 . ? C21 C28 1.525(9) . ? C22 C23 1.513(9) . ? C22 C24 1.543(8) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 C25A 1.535(18) . ? C26 C25B 1.572(14) . ? C28 C29 1.530(8) . ? C28 C30 1.541(9) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.410(6) . ? C31 C32 1.422(6) . ? C31 P3 1.835(4) . ? C32 C33 1.397(7) . ? C32 C37 1.532(7) . ? C33 C34 1.381(7) . ? C33 H33 0.9500 . ? C34 C35 1.392(7) . ? C34 C40 1.520(7) . ? C35 C36 1.398(6) . ? C35 H35 0.9500 . ? C36 C43 1.516(7) . ? C37 C39 1.507(8) . ? C37 C38 1.512(8) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.512(8) . ? C40 C42 1.512(9) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.516(7) . ? C43 C45 1.531(7) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 O10 1.457(11) . ? C46A O10 1.39(3) . ? C47 O11 1.402(7) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C25A C27A 1.55(2) . ? C25B C27B 1.572(17) . ? C1S O1S 1.419(6) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S O2S 1.434(9) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S O3S 1.444(10) . ? Cd1 O1 2.157(3) . ? Cd1 O4 2.181(3) . ? Cd1 O8 2.204(3) 2_565 ? Cd1 O7 2.260(3) . ? Cd1 O10 2.365(4) . ? Cd2 O6 2.183(3) . ? Cd2 O3 2.233(3) 2_565 ? Cd2 O9 2.262(3) . ? Cd2 O7 2.353(3) 2_565 ? Cd2 O11 2.359(4) . ? Cd2 O8 2.442(3) 2_565 ? Cd2 P3 2.9979(14) 2_565 ? O1 P1 1.501(4) . ? O2 P1 1.577(4) . ? O3 P1 1.508(4) . ? O3 Cd2 2.233(3) 2_565 ? O4 P2 1.498(3) . ? O5 P2 1.600(4) . ? O6 P2 1.499(4) . ? O7 P3 1.539(3) . ? O7 Cd2 2.353(3) 2_565 ? O8 P3 1.535(3) . ? O8 Cd1 2.204(3) 2_565 ? O8 Cd2 2.442(3) 2_565 ? O9 P3 1.525(3) . ? O1S H1S 0.8400 . ? O2S H2S 0.8400 . ? P3 Cd2 2.9979(14) 2_565 ? C4SA O4SA 1.383(16) . ? C4SB O4SB 1.44(2) . ? 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 C6 C1 C2 119.4(5) . . ? C6 C1 P1 122.6(4) . . ? C2 C1 P1 117.9(4) . . ? C3 C2 C1 118.0(6) . . ? C3 C2 C7 117.6(6) . . ? C1 C2 C7 124.4(5) . . ? C4 C3 C2 123.9(6) . . ? C4 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? C3 C4 C5 117.5(6) . . ? C3 C4 C10A 114.7(8) . . ? C5 C4 C10A 127.2(8) . . ? C3 C4 C10B 129.7(9) . . ? C5 C4 C10B 111.9(10) . . ? C10A C4 C10B 22.2(8) . . ? C6 C5 C4 122.9(6) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C1 118.0(5) . . ? C5 C6 C13 118.3(5) . . ? C1 C6 C13 123.7(5) . . ? C2 C7 C9 111.4(5) . . ? C2 C7 C8 111.9(5) . . ? C9 C7 C8 110.2(5) . . ? C2 C7 H7 107.7 . . ? C9 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12A C10A C4 113.3(10) . . ? C12A C10A C11A 110.5(11) . . ? C4 C10A C11A 101.1(9) . . ? C12B C10B C11B 108(2) . . ? C12B C10B C4 123.0(19) . . ? C11B C10B C4 110.7(17) . . ? C15 C13 C14 110.0(5) . . ? C15 C13 C6 110.9(5) . . ? C14 C13 C6 113.4(5) . . ? C15 C13 H13 107.4 . . ? C14 C13 H13 107.4 . . ? C6 C13 H13 107.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.7(5) . . ? C17 C16 P2 122.3(4) . . ? C21 C16 P2 117.9(4) . . ? C18 C17 C16 117.8(6) . . ? C18 C17 C22 117.6(6) . . ? C16 C17 C22 124.5(5) . . ? C19 C18 C17 123.1(7) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C20 C19 C18 117.4(6) . . ? C20 C19 C25A 107.8(8) . . ? C18 C19 C25A 134.8(9) . . ? C20 C19 C25B 135.7(9) . . ? C18 C19 C25B 106.8(9) . . ? C25A C19 C25B 28.2(5) . . ? C19 C20 C21 123.4(7) . . ? C19 C20 H20 118.3 . . ? C21 C20 H20 118.3 . . ? C20 C21 C16 118.1(6) . . ? C20 C21 C28 118.3(6) . . ? C16 C21 C28 123.5(5) . . ? C17 C22 C23 111.6(5) . . ? C17 C22 C24 112.9(6) . . ? C23 C22 C24 110.3(6) . . ? C17 C22 H22 107.3 . . ? C23 C22 H22 107.3 . . ? C24 C22 H22 107.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25A C26 C25B 28.9(5) . . ? C21 C28 C29 113.0(6) . . ? C21 C28 C30 110.0(5) . . ? C29 C28 C30 111.1(5) . . ? C21 C28 H28 107.5 . . ? C29 C28 H28 107.5 . . ? C30 C28 H28 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 119.3(4) . . ? C36 C31 P3 117.5(3) . . ? C32 C31 P3 123.2(3) . . ? C33 C32 C31 118.6(4) . . ? C33 C32 C37 116.4(4) . . ? C31 C32 C37 125.0(4) . . ? C34 C33 C32 122.8(5) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C33 C34 C35 117.7(4) . . ? C33 C34 C40 121.6(5) . . ? C35 C34 C40 120.7(5) . . ? C34 C35 C36 122.4(5) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C31 118.9(4) . . ? C35 C36 C43 116.8(4) . . ? C31 C36 C43 124.2(4) . . ? C39 C37 C38 109.5(5) . . ? C39 C37 C32 110.6(5) . . ? C38 C37 C32 112.6(4) . . ? C39 C37 H37 108.0 . . ? C38 C37 H37 108.0 . . ? C32 C37 H37 108.0 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C42 110.7(5) . . ? C41 C40 C34 112.3(5) . . ? C42 C40 C34 110.8(5) . . ? C41 C40 H40 107.6 . . ? C42 C40 H40 107.6 . . ? C34 C40 H40 107.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C36 111.2(4) . . ? C44 C43 C45 110.6(4) . . ? C36 C43 C45 112.8(4) . . ? C44 C43 H43 107.3 . . ? C36 C43 H43 107.3 . . ? C45 C43 H43 107.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O11 C47 H47A 109.5 . . ? O11 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O11 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C26 C25A C27A 107.1(14) . . ? C26 C25A C19 106.6(11) . . ? C27A C25A C19 102.0(11) . . ? C26 C25B C27B 112.5(10) . . ? C26 C25B C19 103.7(9) . . ? C27B C25B C19 104.6(10) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O1 Cd1 O4 129.90(13) . . ? O1 Cd1 O8 129.73(12) . 2_565 ? O4 Cd1 O8 99.17(12) . 2_565 ? O1 Cd1 O7 87.74(12) . . ? O4 Cd1 O7 101.70(12) . . ? O8 Cd1 O7 92.83(11) 2_565 . ? O1 Cd1 O10 87.96(13) . . ? O4 Cd1 O10 81.38(13) . . ? O8 Cd1 O10 89.63(12) 2_565 . ? O7 Cd1 O10 175.69(12) . . ? O6 Cd2 O3 108.62(13) . 2_565 ? O6 Cd2 O9 95.48(12) . . ? O3 Cd2 O9 91.38(12) 2_565 . ? O6 Cd2 O7 152.26(12) . 2_565 ? O3 Cd2 O7 97.75(12) 2_565 2_565 ? O9 Cd2 O7 92.25(11) . 2_565 ? O6 Cd2 O11 86.91(14) . . ? O3 Cd2 O11 85.14(15) 2_565 . ? O9 Cd2 O11 176.27(13) . . ? O7 Cd2 O11 86.90(14) 2_565 . ? O6 Cd2 O8 91.59(12) . 2_565 ? O3 Cd2 O8 157.78(12) 2_565 2_565 ? O9 Cd2 O8 95.90(11) . 2_565 ? O7 Cd2 O8 61.09(10) 2_565 2_565 ? O11 Cd2 O8 86.87(14) . 2_565 ? O6 Cd2 P3 121.87(10) . 2_565 ? O3 Cd2 P3 127.63(9) 2_565 2_565 ? O9 Cd2 P3 96.53(8) . 2_565 ? O7 Cd2 P3 30.52(8) 2_565 2_565 ? O11 Cd2 P3 84.57(13) . 2_565 ? O8 Cd2 P3 30.67(7) 2_565 2_565 ? P1 O1 Cd1 128.2(2) . . ? P1 O3 Cd2 127.0(2) . 2_565 ? P2 O4 Cd1 127.25(19) . . ? P2 O6 Cd2 131.2(2) . . ? P3 O7 Cd1 131.16(18) . . ? P3 O7 Cd2 98.57(15) . 2_565 ? Cd1 O7 Cd2 107.13(12) . 2_565 ? P3 O8 Cd1 125.59(18) . 2_565 ? P3 O8 Cd2 95.10(15) . 2_565 ? Cd1 O8 Cd2 108.47(12) 2_565 2_565 ? P3 O9 Cd2 129.48(17) . . ? C46A O10 C46 29.9(9) . . ? C46A O10 Cd1 116.7(13) . . ? C46 O10 Cd1 125.2(5) . . ? C47 O11 Cd2 125.0(4) . . ? C1S O1S H1S 109.5 . . ? C2S O2S H2S 109.5 . . ? O1 P1 O3 115.4(2) . . ? O1 P1 O2 106.4(2) . . ? O3 P1 O2 111.5(2) . . ? O1 P1 C1 110.8(2) . . ? O3 P1 C1 107.4(2) . . ? O2 P1 C1 104.8(2) . . ? O4 P2 O6 117.17(19) . . ? O4 P2 O5 106.1(2) . . ? O6 P2 O5 108.0(2) . . ? O4 P2 C16 109.6(2) . . ? O6 P2 C16 110.6(2) . . ? O5 P2 C16 104.6(2) . . ? O9 P3 O8 112.57(18) . . ? O9 P3 O7 113.48(18) . . ? O8 P3 O7 104.93(17) . . ? O9 P3 C31 107.52(19) . . ? O8 P3 C31 110.89(19) . . ? O7 P3 C31 107.37(19) . . ? O9 P3 Cd2 133.93(13) . 2_565 ? O8 P3 Cd2 54.23(12) . 2_565 ? O7 P3 Cd2 50.91(12) . 2_565 ? C31 P3 Cd2 118.45(15) . 2_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 6.1(8) . . . . ? P1 C1 C2 C3 -177.6(4) . . . . ? C6 C1 C2 C7 -175.3(5) . . . . ? P1 C1 C2 C7 1.0(7) . . . . ? C1 C2 C3 C4 -5.0(10) . . . . ? C7 C2 C3 C4 176.4(7) . . . . ? C2 C3 C4 C5 2.4(12) . . . . ? C2 C3 C4 C10A -169.6(8) . . . . ? C2 C3 C4 C10B 171.0(12) . . . . ? C3 C4 C5 C6 -1.0(11) . . . . ? C10A C4 C5 C6 169.9(8) . . . . ? C10B C4 C5 C6 -171.5(10) . . . . ? C4 C5 C6 C1 2.3(10) . . . . ? C4 C5 C6 C13 -177.6(6) . . . . ? C2 C1 C6 C5 -4.9(8) . . . . ? P1 C1 C6 C5 179.0(5) . . . . ? C2 C1 C6 C13 175.0(5) . . . . ? P1 C1 C6 C13 -1.2(8) . . . . ? C3 C2 C7 C9 76.0(7) . . . . ? C1 C2 C7 C9 -102.5(7) . . . . ? C3 C2 C7 C8 -47.9(7) . . . . ? C1 C2 C7 C8 133.6(6) . . . . ? C3 C4 C10A C12A 116.4(11) . . . . ? C5 C4 C10A C12A -54.7(15) . . . . ? C10B C4 C10A C12A -106(3) . . . . ? C3 C4 C10A C11A -125.4(9) . . . . ? C5 C4 C10A C11A 63.5(12) . . . . ? C10B C4 C10A C11A 12(2) . . . . ? C3 C4 C10B C12B 174.8(19) . . . . ? C5 C4 C10B C12B -16(3) . . . . ? C10A C4 C10B C12B 122(4) . . . . ? C3 C4 C10B C11B -56(2) . . . . ? C5 C4 C10B C11B 113.1(17) . . . . ? C10A C4 C10B C11B -109(3) . . . . ? C5 C6 C13 C15 -83.0(7) . . . . ? C1 C6 C13 C15 97.1(7) . . . . ? C5 C6 C13 C14 41.4(8) . . . . ? C1 C6 C13 C14 -138.5(6) . . . . ? C21 C16 C17 C18 -7.1(7) . . . . ? P2 C16 C17 C18 167.6(4) . . . . ? C21 C16 C17 C22 170.5(5) . . . . ? P2 C16 C17 C22 -14.8(7) . . . . ? C16 C17 C18 C19 1.9(8) . . . . ? C22 C17 C18 C19 -175.9(5) . . . . ? C17 C18 C19 C20 3.8(9) . . . . ? C17 C18 C19 C25A -173.8(10) . . . . ? C17 C18 C19 C25B -178.6(6) . . . . ? C18 C19 C20 C21 -4.5(9) . . . . ? C25A C19 C20 C21 173.8(8) . . . . ? C25B C19 C20 C21 178.9(8) . . . . ? C19 C20 C21 C16 -0.6(8) . . . . ? C19 C20 C21 C28 175.9(5) . . . . ? C17 C16 C21 C20 6.6(7) . . . . ? P2 C16 C21 C20 -168.4(4) . . . . ? C17 C16 C21 C28 -169.8(5) . . . . ? P2 C16 C21 C28 15.3(7) . . . . ? C18 C17 C22 C23 -82.1(6) . . . . ? C16 C17 C22 C23 100.3(6) . . . . ? C18 C17 C22 C24 42.7(7) . . . . ? C16 C17 C22 C24 -134.9(6) . . . . ? C20 C21 C28 C29 61.6(7) . . . . ? C16 C21 C28 C29 -122.1(6) . . . . ? C20 C21 C28 C30 -63.2(6) . . . . ? C16 C21 C28 C30 113.1(6) . . . . ? C36 C31 C32 C33 5.7(7) . . . . ? P3 C31 C32 C33 -172.5(4) . . . . ? C36 C31 C32 C37 -173.0(5) . . . . ? P3 C31 C32 C37 8.7(7) . . . . ? C31 C32 C33 C34 -3.0(8) . . . . ? C37 C32 C33 C34 175.8(5) . . . . ? C32 C33 C34 C35 -0.3(8) . . . . ? C32 C33 C34 C40 177.9(5) . . . . ? C33 C34 C35 C36 1.1(8) . . . . ? C40 C34 C35 C36 -177.2(5) . . . . ? C34 C35 C36 C31 1.6(7) . . . . ? C34 C35 C36 C43 -175.9(5) . . . . ? C32 C31 C36 C35 -5.0(7) . . . . ? P3 C31 C36 C35 173.3(4) . . . . ? C32 C31 C36 C43 172.4(4) . . . . ? P3 C31 C36 C43 -9.3(6) . . . . ? C33 C32 C37 C39 77.1(6) . . . . ? C31 C32 C37 C39 -104.1(6) . . . . ? C33 C32 C37 C38 -45.7(7) . . . . ? C31 C32 C37 C38 133.1(6) . . . . ? C33 C34 C40 C41 43.8(8) . . . . ? C35 C34 C40 C41 -138.0(6) . . . . ? C33 C34 C40 C42 -80.6(7) . . . . ? C35 C34 C40 C42 97.6(6) . . . . ? C35 C36 C43 C44 58.4(6) . . . . ? C31 C36 C43 C44 -119.0(5) . . . . ? C35 C36 C43 C45 -66.5(6) . . . . ? C31 C36 C43 C45 116.0(5) . . . . ? C25B C26 C25A C27A 35.5(14) . . . . ? C25B C26 C25A C19 -73.1(16) . . . . ? C20 C19 C25A C26 -114.1(9) . . . . ? C18 C19 C25A C26 63.7(14) . . . . ? C25B C19 C25A C26 73.5(17) . . . . ? C20 C19 C25A C27A 133.7(13) . . . . ? C18 C19 C25A C27A -48.5(18) . . . . ? C25B C19 C25A C27A -38.7(17) . . . . ? C25A C26 C25B C27B -44.0(15) . . . . ? C25A C26 C25B C19 68.4(17) . . . . ? C20 C19 C25B C26 -77.8(12) . . . . ? C18 C19 C25B C26 105.3(9) . . . . ? C25A C19 C25B C26 -67.4(18) . . . . ? C20 C19 C25B C27B 40.1(14) . . . . ? C18 C19 C25B C27B -136.7(9) . . . . ? C25A C19 C25B C27B 50.6(17) . . . . ? O4 Cd1 O1 P1 179.4(2) . . . . ? O8 Cd1 O1 P1 14.5(3) 2_565 . . . ? O7 Cd1 O1 P1 -77.3(3) . . . . ? O10 Cd1 O1 P1 102.4(3) . . . . ? O1 Cd1 O4 P2 -150.5(2) . . . . ? O8 Cd1 O4 P2 17.8(3) 2_565 . . . ? O7 Cd1 O4 P2 112.6(2) . . . . ? O10 Cd1 O4 P2 -70.5(2) . . . . ? O3 Cd2 O6 P2 -157.4(3) 2_565 . . . ? O9 Cd2 O6 P2 -64.1(3) . . . . ? O7 Cd2 O6 P2 41.4(4) 2_565 . . . ? O11 Cd2 O6 P2 118.8(3) . . . . ? O8 Cd2 O6 P2 32.0(3) 2_565 . . . ? P3 Cd2 O6 P2 37.1(3) 2_565 . . . ? O1 Cd1 O7 P3 -179.9(2) . . . . ? O4 Cd1 O7 P3 -49.5(2) . . . . ? O8 Cd1 O7 P3 50.4(2) 2_565 . . . ? O10 Cd1 O7 P3 175.3(15) . . . . ? O1 Cd1 O7 Cd2 61.67(14) . . . 2_565 ? O4 Cd1 O7 Cd2 -167.99(12) . . . 2_565 ? O8 Cd1 O7 Cd2 -68.01(13) 2_565 . . 2_565 ? O10 Cd1 O7 Cd2 56.8(16) . . . 2_565 ? O6 Cd2 O9 P3 120.5(2) . . . . ? O3 Cd2 O9 P3 -130.6(2) 2_565 . . . ? O7 Cd2 O9 P3 -32.8(2) 2_565 . . . ? O11 Cd2 O9 P3 -110(2) . . . . ? O8 Cd2 O9 P3 28.3(2) 2_565 . . . ? P3 Cd2 O9 P3 -2.5(2) 2_565 . . . ? O1 Cd1 O10 C46A 49.3(12) . . . . ? O4 Cd1 O10 C46A -81.6(12) . . . . ? O8 Cd1 O10 C46A 179.1(12) 2_565 . . . ? O7 Cd1 O10 C46A 54(2) . . . . ? O1 Cd1 O10 C46 15.6(7) . . . . ? O4 Cd1 O10 C46 -115.2(7) . . . . ? O8 Cd1 O10 C46 145.4(7) 2_565 . . . ? O7 Cd1 O10 C46 20.5(19) . . . . ? O6 Cd2 O11 C47 174.1(5) . . . . ? O3 Cd2 O11 C47 65.1(5) 2_565 . . . ? O9 Cd2 O11 C47 44(2) . . . . ? O7 Cd2 O11 C47 -32.9(5) 2_565 . . . ? O8 Cd2 O11 C47 -94.1(5) 2_565 . . . ? P3 Cd2 O11 C47 -63.4(5) 2_565 . . . ? Cd1 O1 P1 O3 63.6(3) . . . . ? Cd1 O1 P1 O2 -60.6(3) . . . . ? Cd1 O1 P1 C1 -174.0(2) . . . . ? Cd2 O3 P1 O1 -35.8(3) 2_565 . . . ? Cd2 O3 P1 O2 85.7(3) 2_565 . . . ? Cd2 O3 P1 C1 -159.9(2) 2_565 . . . ? C6 C1 P1 O1 -20.4(5) . . . . ? C2 C1 P1 O1 163.4(4) . . . . ? C6 C1 P1 O3 106.5(5) . . . . ? C2 C1 P1 O3 -69.7(4) . . . . ? C6 C1 P1 O2 -134.8(5) . . . . ? C2 C1 P1 O2 49.0(5) . . . . ? Cd1 O4 P2 O6 -57.7(3) . . . . ? Cd1 O4 P2 O5 62.9(3) . . . . ? Cd1 O4 P2 C16 175.2(3) . . . . ? Cd2 O6 P2 O4 23.6(4) . . . . ? Cd2 O6 P2 O5 -96.0(3) . . . . ? Cd2 O6 P2 C16 150.2(3) . . . . ? C17 C16 P2 O4 114.4(4) . . . . ? C21 C16 P2 O4 -70.8(4) . . . . ? C17 C16 P2 O6 -16.3(5) . . . . ? C21 C16 P2 O6 158.5(4) . . . . ? C17 C16 P2 O5 -132.3(4) . . . . ? C21 C16 P2 O5 42.5(5) . . . . ? Cd2 O9 P3 O8 64.9(3) . . . . ? Cd2 O9 P3 O7 -54.1(3) . . . . ? Cd2 O9 P3 C31 -172.7(2) . . . . ? Cd2 O9 P3 Cd2 3.5(3) . . . 2_565 ? Cd1 O8 P3 O9 -11.7(3) 2_565 . . . ? Cd2 O8 P3 O9 -128.80(15) 2_565 . . . ? Cd1 O8 P3 O7 112.2(2) 2_565 . . . ? Cd2 O8 P3 O7 -4.92(17) 2_565 . . . ? Cd1 O8 P3 C31 -132.2(2) 2_565 . . . ? Cd2 O8 P3 C31 110.71(18) 2_565 . . . ? Cd1 O8 P3 Cd2 117.1(2) 2_565 . . 2_565 ? Cd1 O7 P3 O9 6.6(3) . . . . ? Cd2 O7 P3 O9 128.43(15) 2_565 . . . ? Cd1 O7 P3 O8 -116.7(2) . . . . ? Cd2 O7 P3 O8 5.14(17) 2_565 . . . ? Cd1 O7 P3 C31 125.3(2) . . . . ? Cd2 O7 P3 C31 -112.90(18) 2_565 . . . ? Cd1 O7 P3 Cd2 -121.8(3) . . . 2_565 ? C36 C31 P3 O9 75.6(4) . . . . ? C32 C31 P3 O9 -106.2(4) . . . . ? C36 C31 P3 O8 -161.0(3) . . . . ? C32 C31 P3 O8 17.3(5) . . . . ? C36 C31 P3 O7 -46.9(4) . . . . ? C32 C31 P3 O7 131.4(4) . . . . ? C36 C31 P3 Cd2 -101.3(4) . . . 2_565 ? C32 C31 P3 Cd2 76.9(4) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.209 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.114 #===END data_DMF4 _database_code_depnum_ccdc_archive 'CCDC 679266' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium phosphonate' _chemical_melting_point 459.15 _chemical_formula_moiety 'C102 H138 Cd4 N4 O22 P6' _chemical_formula_sum 'C102 H138 Cd4 N4 O22 P6' _chemical_formula_weight 2407.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.876(3) _cell_length_b 15.165(3) _cell_length_c 17.449(4) _cell_angle_alpha 69.26(3) _cell_angle_beta 75.11(3) _cell_angle_gamma 86.03(3) _cell_volume 3317.7(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2517 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 20.41 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8628 _exptl_absorpt_correction_T_max 0.9278 _exptl_absorpt_process_details SADABS _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 graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18821 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.1097 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12765 _reflns_number_gt 8017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1114P)^2^+0.0000P] 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 12765 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2216 _refine_ls_wR_factor_gt 0.1991 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.92261(5) 0.17199(4) 0.42308(4) 0.0464(2) Uani 1 1 d . . . Cd2 Cd 1.18081(4) 0.06558(4) 0.44936(3) 0.03011(17) Uani 1 1 d . . . P1 P 0.68501(17) 0.12985(16) 0.52852(14) 0.0416(5) Uani 1 1 d . . . P2 P 1.13855(17) 0.24996(14) 0.29464(14) 0.0408(5) Uani 1 1 d . . . P3 P 1.00252(14) 0.03100(12) 0.60028(12) 0.0272(4) Uani 1 1 d . . . O1 O 0.7805(4) 0.1817(4) 0.4977(4) 0.0506(15) Uani 1 1 d . . . O2 O 0.6317(5) 0.1567(5) 0.4531(4) 0.071(2) Uani 1 1 d . . . O3 O 0.6920(4) 0.0260(4) 0.5624(4) 0.0464(14) Uani 1 1 d . . . H2A H 0.6516 0.0013 0.5470 0.070 Uiso 1 1 calc R . . O4 O 1.0378(4) 0.2661(4) 0.3446(4) 0.0583(18) Uani 1 1 d . . . O5 O 1.1231(4) 0.1864(4) 0.2447(4) 0.0510(15) Uani 1 1 d . . . H5A H 1.0961 0.1348 0.2791 0.076 Uiso 1 1 calc R . . O6 O 1.2111(4) 0.2048(4) 0.3475(4) 0.0510(16) Uani 1 1 d . . . O7 O 1.0157(4) 0.1163(3) 0.5192(3) 0.0335(12) Uani 1 1 d . . . O8 O 0.9024(3) -0.0201(3) 0.6285(3) 0.0311(11) Uani 1 1 d . . . O9 O 1.0900(4) -0.0328(3) 0.5826(3) 0.0340(12) Uani 1 1 d . . . O10 O 0.8514(6) 0.2726(6) 0.3103(6) 0.094(3) Uani 1 1 d . . . O11 O 1.2578(4) 0.1275(4) 0.5223(4) 0.0493(15) Uani 1 1 d . . . N1 N 0.8864(7) 0.4095(7) 0.1977(6) 0.074(3) Uiso 1 1 d . . . N2 N 1.2679(6) 0.2303(6) 0.5843(5) 0.064(2) Uani 1 1 d . . . C1 C 0.6072(6) 0.1758(6) 0.6070(5) 0.041(2) Uani 1 1 d . . . C2 C 0.5650(6) 0.1195(6) 0.6925(6) 0.048(2) Uani 1 1 d . . . C3 C 0.5204(6) 0.1636(7) 0.7495(7) 0.058(3) Uani 1 1 d . . . H3 H 0.4953 0.1264 0.8074 0.069 Uiso 1 1 calc R . . C4 C 0.5115(6) 0.2630(7) 0.7236(6) 0.047(2) Uani 1 1 d . A . C5 C 0.5469(6) 0.3147(7) 0.6412(6) 0.051(2) Uani 1 1 d . . . H5 H 0.5385 0.3810 0.6240 0.062 Uiso 1 1 calc R . . C6 C 0.5952(6) 0.2770(6) 0.5796(6) 0.047(2) Uani 1 1 d . . . C7 C 0.5679(7) 0.0123(6) 0.7270(6) 0.052(2) Uani 1 1 d . . . H7 H 0.5740 -0.0114 0.6794 0.062 Uiso 1 1 calc R . . C8 C 0.4723(8) -0.0302(7) 0.7948(7) 0.076(3) Uani 1 1 d . . . H8A H 0.4756 -0.0991 0.8152 0.115 Uiso 1 1 calc R . . H8B H 0.4146 -0.0108 0.7705 0.115 Uiso 1 1 calc R . . H8C H 0.4655 -0.0078 0.8422 0.115 Uiso 1 1 calc R . . C9 C 0.6606(7) -0.0168(7) 0.7624(7) 0.068(3) Uani 1 1 d . . . H9A H 0.6639 -0.0858 0.7839 0.101 Uiso 1 1 calc R . . H9B H 0.6562 0.0070 0.8085 0.101 Uiso 1 1 calc R . . H9C H 0.7206 0.0097 0.7173 0.101 Uiso 1 1 calc R . . C10 C 0.4640(7) 0.3073(8) 0.7901(7) 0.066(3) Uani 1 1 d . . . C11A C 0.3761(14) 0.3642(14) 0.7705(13) 0.052(5) Uiso 0.50 1 d P A 1 C12A C 0.5413(16) 0.3330(17) 0.8236(15) 0.070(6) Uiso 0.50 1 d P A 1 C11B C 0.3517(16) 0.3160(17) 0.7974(14) 0.066(6) Uiso 0.50 1 d P A 2 C12B C 0.5335(16) 0.3866(17) 0.7876(15) 0.071(6) Uiso 0.50 1 d P A 2 C13 C 0.6255(8) 0.3395(6) 0.4896(6) 0.060(3) Uani 1 1 d . . . H13 H 0.6687 0.3028 0.4567 0.072 Uiso 1 1 calc R . . C14 C 0.5346(8) 0.3722(8) 0.4525(7) 0.081(4) Uani 1 1 d . . . H14A H 0.5570 0.4128 0.3930 0.121 Uiso 1 1 calc R . . H14B H 0.4907 0.4076 0.4844 0.121 Uiso 1 1 calc R . . H14C H 0.4980 0.3171 0.4564 0.121 Uiso 1 1 calc R . . C15 C 0.6870(8) 0.4275(7) 0.4785(7) 0.074(3) Uani 1 1 d . . . H15A H 0.7062 0.4670 0.4185 0.111 Uiso 1 1 calc R . . H15B H 0.7471 0.4067 0.4990 0.111 Uiso 1 1 calc R . . H15C H 0.6464 0.4639 0.5110 0.111 Uiso 1 1 calc R . . C16 C 1.1881(6) 0.3640(5) 0.2172(5) 0.042(2) Uani 1 1 d . . . C17 C 1.2341(7) 0.3788(7) 0.1322(6) 0.056(2) Uani 1 1 d . . . C18 C 1.2558(7) 0.4729(7) 0.0772(6) 0.057(2) Uani 1 1 d . . . H18 H 1.2850 0.4839 0.0189 0.068 Uiso 1 1 calc R . . C19 C 1.2373(8) 0.5484(7) 0.1025(6) 0.061(3) Uani 1 1 d . . . C20 C 1.1999(7) 0.5318(6) 0.1864(7) 0.060(3) Uani 1 1 d . . . H20 H 1.1898 0.5842 0.2051 0.072 Uiso 1 1 calc R . . C21 C 1.1754(6) 0.4423(6) 0.2465(5) 0.046(2) Uani 1 1 d . . . C22 C 1.2679(8) 0.3019(8) 0.0951(6) 0.072(3) Uani 1 1 d . . . H22 H 1.2575 0.2402 0.1432 0.087 Uiso 1 1 calc R . . C23 C 1.3790(10) 0.3125(9) 0.0511(9) 0.114(5) Uani 1 1 d . . . H23A H 1.3988 0.2611 0.0289 0.171 Uiso 1 1 calc R . . H23B H 1.4174 0.3099 0.0917 0.171 Uiso 1 1 calc R . . H23C H 1.3921 0.3731 0.0044 0.171 Uiso 1 1 calc R . . C24 C 1.2025(10) 0.2994(9) 0.0365(9) 0.099(4) Uiso 1 1 d . . . H24A H 1.2245 0.2489 0.0135 0.148 Uiso 1 1 calc R . . H24B H 1.2087 0.3601 -0.0101 0.148 Uiso 1 1 calc R . . H24C H 1.1327 0.2875 0.0688 0.148 Uiso 1 1 calc R . . C25 C 1.2562(9) 0.6486(8) 0.0404(8) 0.084(4) Uani 1 1 d . . . H25 H 1.2349 0.6917 0.0734 0.100 Uiso 1 1 calc R . . C26 C 1.1993(10) 0.6724(8) -0.0239(9) 0.110(5) Uani 1 1 d . . . H26A H 1.2140 0.7381 -0.0614 0.166 Uiso 1 1 calc R . . H26B H 1.1278 0.6643 0.0038 0.166 Uiso 1 1 calc R . . H26C H 1.2179 0.6307 -0.0571 0.166 Uiso 1 1 calc R . . C27 C 1.3648(11) 0.6644(9) 0.0020(10) 0.123(6) Uani 1 1 d . . . H27A H 1.4001 0.6495 0.0469 0.184 Uiso 1 1 calc R . . H27B H 1.3781 0.7305 -0.0347 0.184 Uiso 1 1 calc R . . H27C H 1.3879 0.6235 -0.0314 0.184 Uiso 1 1 calc R . . C28 C 1.1362(8) 0.4345(7) 0.3385(6) 0.060(3) Uani 1 1 d . . . H28 H 1.1286 0.3661 0.3745 0.072 Uiso 1 1 calc R . . C29 C 1.2117(9) 0.4805(8) 0.3646(7) 0.082(4) Uani 1 1 d . . . H29A H 1.1862 0.4753 0.4240 0.124 Uiso 1 1 calc R . . H29B H 1.2216 0.5473 0.3288 0.124 Uiso 1 1 calc R . . H29C H 1.2755 0.4485 0.3577 0.124 Uiso 1 1 calc R . . C30 C 1.0337(9) 0.4795(7) 0.3521(7) 0.074(3) Uani 1 1 d . . . H30A H 1.0092 0.4733 0.4117 0.111 Uiso 1 1 calc R . . H30B H 0.9868 0.4477 0.3364 0.111 Uiso 1 1 calc R . . H30C H 1.0397 0.5465 0.3167 0.111 Uiso 1 1 calc R . . C31 C 1.0167(5) 0.0718(5) 0.6828(5) 0.0340(17) Uani 1 1 d . . . C32 C 0.9740(6) 0.1596(5) 0.6872(5) 0.0376(18) Uani 1 1 d . . . C33 C 0.9975(6) 0.1980(6) 0.7408(5) 0.046(2) Uani 1 1 d . . . H33 H 0.9697 0.2568 0.7418 0.055 Uiso 1 1 calc R . . C34 C 1.0599(7) 0.1549(7) 0.7935(6) 0.060(3) Uani 1 1 d . B . C35 C 1.0939(7) 0.0672(7) 0.7929(6) 0.056(2) Uani 1 1 d . . . H35 H 1.1342 0.0347 0.8303 0.067 Uiso 1 1 calc R . . C36 C 1.0724(6) 0.0235(6) 0.7407(5) 0.042(2) Uani 1 1 d . . . C37 C 0.8999(6) 0.2091(6) 0.6364(5) 0.0410(19) Uani 1 1 d . . . H37 H 0.8809 0.1656 0.6107 0.049 Uiso 1 1 calc R . . C38 C 0.9464(6) 0.3006(5) 0.5637(6) 0.049(2) Uani 1 1 d . . . H38A H 0.8973 0.3305 0.5314 0.073 Uiso 1 1 calc R . . H38B H 1.0053 0.2849 0.5262 0.073 Uiso 1 1 calc R . . H38C H 0.9660 0.3441 0.5876 0.073 Uiso 1 1 calc R . . C39 C 0.8033(6) 0.2330(6) 0.6940(6) 0.054(2) Uani 1 1 d . . . H39A H 0.7565 0.2641 0.6597 0.081 Uiso 1 1 calc R . . H39B H 0.8204 0.2751 0.7204 0.081 Uiso 1 1 calc R . . H39C H 0.7723 0.1747 0.7382 0.081 Uiso 1 1 calc R . . C43 C 1.1069(7) -0.0763(6) 0.7556(6) 0.052(2) Uiso 1 1 d . . . H43 H 1.0778 -0.1018 0.7206 0.063 Uiso 1 1 calc R . . C44 C 1.2178(7) -0.0797(7) 0.7269(8) 0.077(3) Uani 1 1 d . . . H44A H 1.2377 -0.1453 0.7367 0.115 Uiso 1 1 calc R . . H44B H 1.2488 -0.0533 0.7589 0.115 Uiso 1 1 calc R . . H44C H 1.2397 -0.0427 0.6664 0.115 Uiso 1 1 calc R . . C45 C 1.0687(9) -0.1404(9) 0.8490(8) 0.093(4) Uiso 1 1 d . . . H45A H 1.0914 -0.2048 0.8560 0.139 Uiso 1 1 calc R . . H45B H 0.9956 -0.1406 0.8650 0.139 Uiso 1 1 calc R . . H45C H 1.0947 -0.1165 0.8852 0.139 Uiso 1 1 calc R . . C46 C 0.9082(10) 0.3206(9) 0.2419(7) 0.086(4) Uani 1 1 d . . . C47 C 0.8007(11) 0.4521(11) 0.2299(10) 0.120(5) Uiso 1 1 d . . . H47A H 0.7587 0.4049 0.2794 0.181 Uiso 1 1 calc R . . H47B H 0.7635 0.4788 0.1864 0.181 Uiso 1 1 calc R . . H47C H 0.8198 0.5025 0.2464 0.181 Uiso 1 1 calc R . . C48 C 0.9622(5) 0.4540(5) 0.1233(4) 0.101(4) Uani 1 1 d . . . H48A H 0.9422 0.5180 0.0944 0.152 Uiso 1 1 calc R . . H48B H 0.9720 0.4176 0.0855 0.152 Uiso 1 1 calc R . . H48C H 1.0247 0.4572 0.1387 0.152 Uiso 1 1 calc R . . C49 C 1.2317(5) 0.2015(5) 0.5354(4) 0.052(2) Uani 1 1 d R . . C50 C 1.2340(5) 0.3183(5) 0.5955(4) 0.086(4) Uiso 1 1 d R . . H50A H 1.2678 0.3308 0.6336 0.128 Uiso 1 1 d R . . H50B H 1.1617 0.3142 0.6199 0.128 Uiso 1 1 d R . . H50C H 1.2496 0.3695 0.5405 0.128 Uiso 1 1 d R . . C51 C 1.3350(8) 0.1760(9) 0.6309(8) 0.088(4) Uani 1 1 d . . . H51A H 1.3537 0.2105 0.6632 0.132 Uiso 1 1 calc R . . H51B H 1.3948 0.1643 0.5918 0.132 Uiso 1 1 calc R . . H51C H 1.3026 0.1157 0.6699 0.132 Uiso 1 1 calc R . . C40 C 1.0861(9) 0.2011(8) 0.8502(8) 0.080(3) Uiso 1 1 d . . . C41A C 1.0212(13) 0.1521(12) 0.9421(11) 0.082(5) Uiso 0.70 1 d P B 1 C42A C 1.0718(12) 0.3070(11) 0.8271(10) 0.075(4) Uiso 0.70 1 d P B 1 C41B C 1.178(3) 0.173(2) 0.867(2) 0.069(10) Uiso 0.30 1 d P B 2 C42B C 1.008(3) 0.240(3) 0.894(3) 0.084(11) Uiso 0.30 1 d P B 2 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 0.0444(4) 0.0356(4) 0.0588(4) -0.0279(3) 0.0036(3) 0.0024(3) Cd2 0.0304(3) 0.0258(3) 0.0397(3) -0.0199(2) -0.0075(2) 0.0050(2) P1 0.0455(13) 0.0452(13) 0.0454(13) -0.0274(11) -0.0201(11) 0.0235(11) P2 0.0480(13) 0.0306(11) 0.0425(12) -0.0160(10) -0.0061(10) 0.0074(10) P3 0.0302(10) 0.0241(9) 0.0334(10) -0.0190(8) -0.0076(8) 0.0080(8) O1 0.067(4) 0.038(3) 0.051(4) -0.028(3) -0.011(3) 0.025(3) O2 0.092(5) 0.092(5) 0.057(4) -0.052(4) -0.047(4) 0.063(4) O3 0.053(4) 0.038(3) 0.062(4) -0.032(3) -0.023(3) 0.027(3) O4 0.061(4) 0.044(3) 0.044(4) -0.009(3) 0.014(3) 0.025(3) O5 0.063(4) 0.047(3) 0.043(3) -0.023(3) 0.001(3) -0.010(3) O6 0.049(4) 0.034(3) 0.063(4) -0.005(3) -0.019(3) -0.004(3) O7 0.038(3) 0.027(3) 0.037(3) -0.015(2) -0.010(2) 0.015(2) O8 0.030(3) 0.038(3) 0.029(3) -0.020(2) -0.001(2) -0.003(2) O9 0.037(3) 0.030(3) 0.040(3) -0.018(2) -0.012(2) 0.017(2) O10 0.078(6) 0.098(6) 0.086(6) -0.014(5) -0.014(5) -0.002(5) O11 0.054(4) 0.050(4) 0.054(4) -0.028(3) -0.015(3) 0.000(3) N2 0.072(6) 0.060(5) 0.069(6) -0.029(5) -0.021(5) -0.014(4) C1 0.043(5) 0.043(5) 0.053(5) -0.034(4) -0.020(4) 0.018(4) C2 0.045(5) 0.054(5) 0.056(6) -0.034(5) -0.016(4) 0.020(4) C3 0.034(5) 0.079(7) 0.066(6) -0.035(6) -0.012(4) 0.012(5) C4 0.029(4) 0.068(6) 0.058(6) -0.041(5) -0.009(4) 0.014(4) C5 0.043(5) 0.057(6) 0.069(7) -0.042(5) -0.019(5) 0.031(4) C6 0.046(5) 0.048(5) 0.055(6) -0.028(4) -0.015(4) 0.022(4) C7 0.056(6) 0.055(6) 0.045(5) -0.019(5) -0.013(4) 0.005(5) C8 0.075(8) 0.058(6) 0.093(9) -0.027(6) -0.015(7) 0.005(6) C9 0.061(7) 0.071(7) 0.075(7) -0.029(6) -0.023(6) 0.015(5) C10 0.054(6) 0.090(8) 0.086(8) -0.071(7) -0.020(5) 0.028(5) C13 0.083(7) 0.035(5) 0.062(6) -0.023(5) -0.018(5) 0.034(5) C14 0.103(9) 0.075(7) 0.060(7) -0.016(6) -0.036(6) 0.048(7) C15 0.070(7) 0.067(7) 0.072(7) -0.020(6) -0.011(6) 0.035(6) C16 0.052(5) 0.036(4) 0.038(5) -0.014(4) -0.012(4) 0.010(4) C17 0.066(6) 0.048(5) 0.052(6) -0.019(5) -0.010(5) 0.006(5) C18 0.054(6) 0.073(7) 0.040(5) -0.018(5) -0.006(4) -0.004(5) C19 0.082(7) 0.049(6) 0.046(6) -0.003(5) -0.022(5) -0.013(5) C20 0.078(7) 0.041(5) 0.067(7) -0.022(5) -0.023(6) 0.003(5) C21 0.053(5) 0.038(5) 0.042(5) -0.010(4) -0.008(4) -0.004(4) C22 0.091(8) 0.068(7) 0.045(6) -0.024(5) 0.011(6) 0.007(6) C23 0.131(12) 0.090(10) 0.098(10) -0.043(8) 0.023(9) 0.003(9) C25 0.099(10) 0.058(7) 0.082(9) -0.006(6) -0.023(7) -0.027(7) C26 0.100(10) 0.072(8) 0.103(10) 0.034(7) -0.026(8) 0.020(7) C27 0.128(13) 0.081(9) 0.122(13) 0.016(9) -0.029(10) -0.041(9) C28 0.089(8) 0.042(5) 0.048(6) -0.016(5) -0.016(5) -0.003(5) C29 0.122(10) 0.065(7) 0.078(8) -0.031(6) -0.045(7) -0.002(7) C30 0.110(9) 0.042(5) 0.063(7) -0.026(5) 0.000(6) 0.008(6) C31 0.026(4) 0.036(4) 0.044(5) -0.025(4) 0.000(3) 0.000(3) C32 0.042(5) 0.034(4) 0.040(5) -0.025(4) 0.002(4) -0.003(4) C33 0.045(5) 0.049(5) 0.054(5) -0.036(5) -0.004(4) 0.000(4) C34 0.060(6) 0.073(7) 0.068(7) -0.049(6) -0.017(5) 0.000(5) C35 0.063(6) 0.069(6) 0.059(6) -0.039(5) -0.030(5) 0.007(5) C36 0.048(5) 0.039(5) 0.042(5) -0.018(4) -0.014(4) 0.008(4) C37 0.038(5) 0.040(4) 0.054(5) -0.029(4) -0.013(4) 0.012(4) C38 0.058(6) 0.026(4) 0.066(6) -0.026(4) -0.010(5) 0.013(4) C39 0.049(5) 0.056(6) 0.069(6) -0.044(5) -0.007(5) 0.021(4) C44 0.065(7) 0.072(7) 0.118(10) -0.046(7) -0.055(7) 0.038(6) C46 0.121(11) 0.079(8) 0.045(7) -0.006(6) -0.021(7) 0.002(8) C48 0.103(10) 0.095(10) 0.108(11) -0.032(9) -0.029(9) -0.011(8) C49 0.057(6) 0.054(6) 0.052(6) -0.032(5) -0.002(4) -0.019(5) C51 0.072(8) 0.106(10) 0.112(10) -0.056(8) -0.038(7) -0.008(7) _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 O4 2.068(6) . ? Cd1 O1 2.093(6) . ? Cd1 O9 2.169(5) 2_756 ? Cd1 O7 2.271(5) . ? Cd1 O10 2.417(8) . ? Cd2 O3 2.182(5) 2_756 ? Cd2 O6 2.208(5) . ? Cd2 O8 2.288(5) 2_756 ? Cd2 O11 2.308(6) . ? Cd2 O9 2.349(5) . ? Cd2 O7 2.512(5) . ? Cd2 P3 3.031(2) . ? P1 O1 1.464(6) . ? P1 O3 1.479(5) . ? P1 O2 1.589(6) . ? P1 C1 1.828(8) . ? P2 O4 1.500(6) . ? P2 O6 1.506(6) . ? P2 O5 1.565(6) . ? P2 C16 1.823(8) . ? P3 O8 1.516(5) . ? P3 O7 1.521(5) . ? P3 O9 1.537(5) . ? P3 C31 1.812(8) . ? O3 Cd2 2.182(5) 2_756 ? O3 H2A 0.8400 . ? O5 H5A 0.8400 . ? O8 Cd2 2.288(5) 2_756 ? O9 Cd1 2.169(5) 2_756 ? O10 C46 1.247(13) . ? O11 C49 1.234(8) . ? N1 C46 1.353(13) . ? N1 C47 1.398(15) . ? N1 C48 1.422(11) . ? N2 C49 1.299(10) . ? N2 C51 1.419(13) . ? N2 C50 1.446(10) . ? C1 C2 1.419(12) . ? C1 C6 1.448(11) . ? C2 C3 1.386(12) . ? C2 C7 1.521(12) . ? C3 C4 1.419(13) . ? C3 H3 0.9500 . ? C4 C5 1.347(13) . ? C4 C10 1.526(12) . ? C5 C6 1.394(11) . ? C5 H5 0.9500 . ? C6 C13 1.485(13) . ? C7 C8 1.532(13) . ? C7 C9 1.538(12) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12A 1.48(2) . ? C10 C11A 1.49(2) . ? C10 C11B 1.53(2) . ? C10 C12B 1.58(2) . ? C13 C14 1.537(13) . ? C13 C15 1.561(14) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.398(12) . ? C16 C21 1.434(11) . ? C17 C18 1.411(13) . ? C17 C22 1.518(13) . ? C18 C19 1.354(13) . ? C18 H18 0.9500 . ? C19 C20 1.357(13) . ? C19 C25 1.514(13) . ? C20 C21 1.390(12) . ? C20 H20 0.9500 . ? C21 C28 1.521(12) . ? C22 C23 1.526(16) . ? C22 C24 1.544(16) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.464(16) . ? C25 C27 1.481(16) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.533(14) . ? C28 C29 1.539(13) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.399(11) . ? C31 C32 1.438(10) . ? C32 C33 1.375(10) . ? C32 C37 1.515(11) . ? C33 C34 1.389(13) . ? C33 H33 0.9500 . ? C34 C35 1.384(13) . ? C34 C40 1.520(14) . ? C35 C36 1.397(11) . ? C35 H35 0.9500 . ? C36 C43 1.507(11) . ? C37 C38 1.551(11) . ? C37 C39 1.561(11) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C43 C44 1.495(13) . ? C43 C45 1.545(14) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C50 H50A 0.9801 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C40 C42B 1.38(4) . ? C40 C41B 1.39(3) . ? C40 C42A 1.523(19) . ? C40 C41A 1.56(2) . ? 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 O4 Cd1 O1 135.5(2) . . ? O4 Cd1 O9 122.6(2) . 2_756 ? O1 Cd1 O9 100.1(2) . 2_756 ? O4 Cd1 O7 88.9(2) . . ? O1 Cd1 O7 103.1(2) . . ? O9 Cd1 O7 91.45(18) 2_756 . ? O4 Cd1 O10 76.5(3) . . ? O1 Cd1 O10 82.5(3) . . ? O9 Cd1 O10 103.2(3) 2_756 . ? O7 Cd1 O10 163.3(2) . . ? O3 Cd2 O6 110.9(2) 2_756 . ? O3 Cd2 O8 97.03(19) 2_756 2_756 ? O6 Cd2 O8 89.04(19) . 2_756 ? O3 Cd2 O11 88.2(2) 2_756 . ? O6 Cd2 O11 85.9(2) . . ? O8 Cd2 O11 173.76(19) 2_756 . ? O3 Cd2 O9 96.75(19) 2_756 . ? O6 Cd2 O9 151.0(2) . . ? O8 Cd2 O9 96.37(17) 2_756 . ? O11 Cd2 O9 86.34(19) . . ? O3 Cd2 O7 156.54(19) 2_756 . ? O6 Cd2 O7 92.19(19) . . ? O8 Cd2 O7 87.25(16) 2_756 . ? O11 Cd2 O7 89.28(19) . . ? O9 Cd2 O7 59.81(15) . . ? O3 Cd2 P3 126.53(16) 2_756 . ? O6 Cd2 P3 121.45(16) . . ? O8 Cd2 P3 94.20(12) 2_756 . ? O11 Cd2 P3 85.34(15) . . ? O9 Cd2 P3 29.92(11) . . ? O7 Cd2 P3 30.02(11) . . ? O1 P1 O3 115.0(3) . . ? O1 P1 O2 108.7(4) . . ? O3 P1 O2 108.2(4) . . ? O1 P1 C1 106.3(4) . . ? O3 P1 C1 112.1(4) . . ? O2 P1 C1 106.2(3) . . ? O4 P2 O6 114.1(4) . . ? O4 P2 O5 107.7(4) . . ? O6 P2 O5 109.7(3) . . ? O4 P2 C16 107.3(3) . . ? O6 P2 C16 110.1(4) . . ? O5 P2 C16 107.6(4) . . ? O8 P3 O7 114.3(3) . . ? O8 P3 O9 112.2(3) . . ? O7 P3 O9 105.1(3) . . ? O8 P3 C31 108.9(3) . . ? O7 P3 C31 107.5(3) . . ? O9 P3 C31 108.7(3) . . ? O8 P3 Cd2 135.11(19) . . ? O7 P3 Cd2 55.76(18) . . ? O9 P3 Cd2 49.67(19) . . ? C31 P3 Cd2 115.8(2) . . ? P1 O1 Cd1 137.0(3) . . ? P1 O3 Cd2 131.1(4) . 2_756 ? P1 O3 H2A 109.5 . . ? Cd2 O3 H2A 100.7 2_756 . ? P2 O4 Cd1 130.5(3) . . ? P2 O5 H5A 109.5 . . ? P2 O6 Cd2 122.3(3) . . ? P3 O7 Cd1 132.2(3) . . ? P3 O7 Cd2 94.2(2) . . ? Cd1 O7 Cd2 108.93(19) . . ? P3 O8 Cd2 129.1(3) . 2_756 ? P3 O9 Cd1 125.6(3) . 2_756 ? P3 O9 Cd2 100.4(2) . . ? Cd1 O9 Cd2 108.1(2) 2_756 . ? C46 O10 Cd1 119.1(8) . . ? C49 O11 Cd2 122.8(5) . . ? C46 N1 C47 120.3(11) . . ? C46 N1 C48 113.5(9) . . ? C47 N1 C48 125.9(10) . . ? C49 N2 C51 122.4(8) . . ? C49 N2 C50 118.7(8) . . ? C51 N2 C50 118.8(8) . . ? C2 C1 C6 119.7(7) . . ? C2 C1 P1 123.9(6) . . ? C6 C1 P1 116.3(7) . . ? C3 C2 C1 118.8(8) . . ? C3 C2 C7 117.0(9) . . ? C1 C2 C7 124.1(7) . . ? C2 C3 C4 121.6(9) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 118.4(8) . . ? C5 C4 C10 122.7(9) . . ? C3 C4 C10 118.9(9) . . ? C4 C5 C6 124.1(9) . . ? C4 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C5 C6 C1 117.1(8) . . ? C5 C6 C13 119.8(8) . . ? C1 C6 C13 123.0(8) . . ? C2 C7 C8 111.2(8) . . ? C2 C7 C9 108.7(8) . . ? C8 C7 C9 111.2(8) . . ? C2 C7 H7 108.5 . . ? C8 C7 H7 108.5 . . ? C9 C7 H7 108.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12A C10 C11A 125.8(14) . . ? C12A C10 C4 110.4(11) . . ? C11A C10 C4 112.2(10) . . ? C12A C10 C11B 139.9(14) . . ? C11A C10 C11B 29.2(9) . . ? C4 C10 C11B 109.6(11) . . ? C12A C10 C12B 32.3(10) . . ? C11A C10 C12B 99.7(13) . . ? C4 C10 C12B 111.7(11) . . ? C11B C10 C12B 124.6(14) . . ? C6 C13 C14 111.4(9) . . ? C6 C13 C15 111.5(8) . . ? C14 C13 C15 109.4(8) . . ? C6 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.5(8) . . ? C17 C16 P2 123.9(7) . . ? C21 C16 P2 116.7(6) . . ? C16 C17 C18 117.4(8) . . ? C16 C17 C22 125.4(8) . . ? C18 C17 C22 117.1(9) . . ? C19 C18 C17 123.7(9) . . ? C19 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? C18 C19 C20 117.7(9) . . ? C18 C19 C25 121.9(10) . . ? C20 C19 C25 120.4(10) . . ? C19 C20 C21 123.6(9) . . ? C19 C20 H20 118.2 . . ? C21 C20 H20 118.2 . . ? C20 C21 C16 117.6(8) . . ? C20 C21 C28 117.7(8) . . ? C16 C21 C28 124.7(7) . . ? C17 C22 C23 111.4(10) . . ? C17 C22 C24 110.3(10) . . ? C23 C22 C24 112.7(10) . . ? C17 C22 H22 107.4 . . ? C23 C22 H22 107.4 . . ? C24 C22 H22 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 111.9(11) . . ? C26 C25 C19 113.5(10) . . ? C27 C25 C19 109.0(10) . . ? C26 C25 H25 107.4 . . ? C27 C25 H25 107.4 . . ? C19 C25 H25 107.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C30 110.6(8) . . ? C21 C28 C29 109.7(9) . . ? C30 C28 C29 111.3(9) . . ? C21 C28 H28 108.4 . . ? C30 C28 H28 108.4 . . ? C29 C28 H28 108.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.7(7) . . ? C36 C31 P3 122.5(6) . . ? C32 C31 P3 119.7(6) . . ? C33 C32 C31 119.8(8) . . ? C33 C32 C37 118.8(7) . . ? C31 C32 C37 121.3(7) . . ? C32 C33 C34 123.0(8) . . ? C32 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C35 C34 C33 116.1(8) . . ? C35 C34 C40 122.5(9) . . ? C33 C34 C40 121.3(9) . . ? C34 C35 C36 123.9(9) . . ? C34 C35 H35 118.0 . . ? C36 C35 H35 118.0 . . ? C35 C36 C31 118.9(7) . . ? C35 C36 C43 116.2(8) . . ? C31 C36 C43 124.8(7) . . ? C32 C37 C38 111.3(7) . . ? C32 C37 C39 111.2(7) . . ? C38 C37 C39 109.7(6) . . ? C32 C37 H37 108.2 . . ? C38 C37 H37 108.2 . . ? C39 C37 H37 108.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C44 C43 C36 111.5(8) . . ? C44 C43 C45 111.0(8) . . ? C36 C43 C45 111.8(8) . . ? C44 C43 H43 107.4 . . ? C36 C43 H43 107.4 . . ? C45 C43 H43 107.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O10 C46 N1 121.9(12) . . ? N1 C47 H47A 109.5 . . ? N1 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N1 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N1 C48 H48A 109.5 . . ? N1 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N1 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O11 C49 N2 122.3(7) . . ? N2 C50 H50A 109.4 . . ? N2 C50 H50B 109.7 . . ? H50A C50 H50B 109.5 . . ? N2 C50 H50C 109.3 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N2 C51 H51A 109.5 . . ? N2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C42B C40 C41B 129(2) . . ? C42B C40 C34 116.2(19) . . ? C41B C40 C34 112.0(18) . . ? C42B C40 C42A 56.8(18) . . ? C41B C40 C42A 113.0(18) . . ? C34 C40 C42A 117.2(11) . . ? C42B C40 C41A 53.3(18) . . ? C41B C40 C41A 96.8(18) . . ? C34 C40 C41A 108.1(10) . . ? C42A C40 C41A 107.6(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cd2 P3 O8 -87.9(3) 2_756 . . . ? O6 Cd2 P3 O8 105.6(3) . . . . ? O8 Cd2 P3 O8 14.1(4) 2_756 . . . ? O11 Cd2 P3 O8 -172.1(3) . . . . ? O9 Cd2 P3 O8 -81.4(4) . . . . ? O7 Cd2 P3 O8 91.2(4) . . . . ? O3 Cd2 P3 O7 -179.1(3) 2_756 . . . ? O6 Cd2 P3 O7 14.3(3) . . . . ? O8 Cd2 P3 O7 -77.1(3) 2_756 . . . ? O11 Cd2 P3 O7 96.7(3) . . . . ? O9 Cd2 P3 O7 -172.6(4) . . . . ? O3 Cd2 P3 O9 -6.5(3) 2_756 . . . ? O6 Cd2 P3 O9 -173.1(3) . . . . ? O8 Cd2 P3 O9 95.5(3) 2_756 . . . ? O11 Cd2 P3 O9 -90.8(3) . . . . ? O7 Cd2 P3 O9 172.6(4) . . . . ? O3 Cd2 P3 C31 86.7(3) 2_756 . . . ? O6 Cd2 P3 C31 -79.9(3) . . . . ? O8 Cd2 P3 C31 -171.3(3) 2_756 . . . ? O11 Cd2 P3 C31 2.4(3) . . . . ? O9 Cd2 P3 C31 93.2(4) . . . . ? O7 Cd2 P3 C31 -94.2(4) . . . . ? O3 P1 O1 Cd1 44.8(6) . . . . ? O2 P1 O1 Cd1 -76.6(5) . . . . ? C1 P1 O1 Cd1 169.5(5) . . . . ? O4 Cd1 O1 P1 151.9(5) . . . . ? O9 Cd1 O1 P1 -12.1(5) 2_756 . . . ? O7 Cd1 O1 P1 -106.0(5) . . . . ? O10 Cd1 O1 P1 90.1(6) . . . . ? O1 P1 O3 Cd2 -15.1(6) . . . 2_756 ? O2 P1 O3 Cd2 106.6(5) . . . 2_756 ? C1 P1 O3 Cd2 -136.7(4) . . . 2_756 ? O6 P2 O4 Cd1 -73.5(6) . . . . ? O5 P2 O4 Cd1 48.6(6) . . . . ? C16 P2 O4 Cd1 164.2(5) . . . . ? O1 Cd1 O4 P2 179.0(4) . . . . ? O9 Cd1 O4 P2 -19.8(6) 2_756 . . . ? O7 Cd1 O4 P2 71.2(5) . . . . ? O10 Cd1 O4 P2 -116.9(6) . . . . ? O4 P2 O6 Cd2 59.2(5) . . . . ? O5 P2 O6 Cd2 -61.8(5) . . . . ? C16 P2 O6 Cd2 180.0(4) . . . . ? O3 Cd2 O6 P2 130.7(4) 2_756 . . . ? O8 Cd2 O6 P2 33.6(4) 2_756 . . . ? O11 Cd2 O6 P2 -142.8(4) . . . . ? O9 Cd2 O6 P2 -67.9(6) . . . . ? O7 Cd2 O6 P2 -53.7(4) . . . . ? P3 Cd2 O6 P2 -60.8(5) . . . . ? O8 P3 O7 Cd1 -8.9(5) . . . . ? O9 P3 O7 Cd1 114.6(4) . . . . ? C31 P3 O7 Cd1 -129.8(4) . . . . ? Cd2 P3 O7 Cd1 120.4(4) . . . . ? O8 P3 O7 Cd2 -129.3(2) . . . . ? O9 P3 O7 Cd2 -5.8(3) . . . . ? C31 P3 O7 Cd2 109.8(3) . . . . ? O4 Cd1 O7 P3 -170.0(4) . . . . ? O1 Cd1 O7 P3 53.3(4) . . . . ? O9 Cd1 O7 P3 -47.4(4) 2_756 . . . ? O10 Cd1 O7 P3 161.3(7) . . . . ? O4 Cd1 O7 Cd2 -55.4(2) . . . . ? O1 Cd1 O7 Cd2 167.9(2) . . . . ? O9 Cd1 O7 Cd2 67.2(2) 2_756 . . . ? O10 Cd1 O7 Cd2 -84.1(8) . . . . ? O3 Cd2 O7 P3 1.9(6) 2_756 . . . ? O6 Cd2 O7 P3 -167.8(3) . . . . ? O8 Cd2 O7 P3 103.3(2) 2_756 . . . ? O11 Cd2 O7 P3 -81.9(3) . . . . ? O9 Cd2 O7 P3 4.3(2) . . . . ? O3 Cd2 O7 Cd1 -135.7(4) 2_756 . . . ? O6 Cd2 O7 Cd1 54.7(2) . . . . ? O8 Cd2 O7 Cd1 -34.3(2) 2_756 . . . ? O11 Cd2 O7 Cd1 140.5(2) . . . . ? O9 Cd2 O7 Cd1 -133.3(3) . . . . ? P3 Cd2 O7 Cd1 -137.6(3) . . . . ? O7 P3 O8 Cd2 46.8(4) . . . 2_756 ? O9 P3 O8 Cd2 -72.7(4) . . . 2_756 ? C31 P3 O8 Cd2 166.9(3) . . . 2_756 ? Cd2 P3 O8 Cd2 -18.3(5) . . . 2_756 ? O8 P3 O9 Cd1 9.7(4) . . . 2_756 ? O7 P3 O9 Cd1 -115.0(3) . . . 2_756 ? C31 P3 O9 Cd1 130.2(4) . . . 2_756 ? Cd2 P3 O9 Cd1 -121.4(4) . . . 2_756 ? O8 P3 O9 Cd2 131.1(2) . . . . ? O7 P3 O9 Cd2 6.3(3) . . . . ? C31 P3 O9 Cd2 -108.5(3) . . . . ? O3 Cd2 O9 P3 174.8(3) 2_756 . . . ? O6 Cd2 O9 P3 12.3(5) . . . . ? O8 Cd2 O9 P3 -87.3(3) 2_756 . . . ? O11 Cd2 O9 P3 87.0(3) . . . . ? O7 Cd2 O9 P3 -4.3(2) . . . . ? O3 Cd2 O9 Cd1 -52.2(2) 2_756 . . 2_756 ? O6 Cd2 O9 Cd1 145.3(3) . . . 2_756 ? O8 Cd2 O9 Cd1 45.7(2) 2_756 . . 2_756 ? O11 Cd2 O9 Cd1 -139.9(2) . . . 2_756 ? O7 Cd2 O9 Cd1 128.8(3) . . . 2_756 ? P3 Cd2 O9 Cd1 133.1(4) . . . 2_756 ? O4 Cd1 O10 C46 18.8(9) . . . . ? O1 Cd1 O10 C46 159.3(10) . . . . ? O9 Cd1 O10 C46 -102.1(9) 2_756 . . . ? O7 Cd1 O10 C46 48.4(15) . . . . ? O3 Cd2 O11 C49 165.2(6) 2_756 . . . ? O6 Cd2 O11 C49 54.1(6) . . . . ? O8 Cd2 O11 C49 18(2) 2_756 . . . ? O9 Cd2 O11 C49 -97.9(6) . . . . ? O7 Cd2 O11 C49 -38.1(6) . . . . ? P3 Cd2 O11 C49 -67.9(5) . . . . ? O1 P1 C1 C2 -121.7(7) . . . . ? O3 P1 C1 C2 4.8(8) . . . . ? O2 P1 C1 C2 122.7(7) . . . . ? O1 P1 C1 C6 54.0(7) . . . . ? O3 P1 C1 C6 -179.6(6) . . . . ? O2 P1 C1 C6 -61.6(7) . . . . ? C6 C1 C2 C3 -5.5(12) . . . . ? P1 C1 C2 C3 170.1(7) . . . . ? C6 C1 C2 C7 176.4(8) . . . . ? P1 C1 C2 C7 -8.1(12) . . . . ? C1 C2 C3 C4 3.4(13) . . . . ? C7 C2 C3 C4 -178.4(8) . . . . ? C2 C3 C4 C5 0.4(13) . . . . ? C2 C3 C4 C10 -178.4(8) . . . . ? C3 C4 C5 C6 -2.2(13) . . . . ? C10 C4 C5 C6 176.6(8) . . . . ? C4 C5 C6 C1 0.0(13) . . . . ? C4 C5 C6 C13 176.0(9) . . . . ? C2 C1 C6 C5 3.8(12) . . . . ? P1 C1 C6 C5 -172.0(6) . . . . ? C2 C1 C6 C13 -172.0(8) . . . . ? P1 C1 C6 C13 12.2(11) . . . . ? C3 C2 C7 C8 37.1(11) . . . . ? C1 C2 C7 C8 -144.8(9) . . . . ? C3 C2 C7 C9 -85.7(10) . . . . ? C1 C2 C7 C9 92.5(10) . . . . ? C5 C4 C10 C12A -87.0(15) . . . . ? C3 C4 C10 C12A 91.8(14) . . . . ? C5 C4 C10 C11A 58.6(14) . . . . ? C3 C4 C10 C11A -122.6(12) . . . . ? C5 C4 C10 C11B 89.8(14) . . . . ? C3 C4 C10 C11B -91.4(13) . . . . ? C5 C4 C10 C12B -52.4(15) . . . . ? C3 C4 C10 C12B 126.4(12) . . . . ? C5 C6 C13 C14 -70.8(11) . . . . ? C1 C6 C13 C14 104.9(10) . . . . ? C5 C6 C13 C15 51.7(11) . . . . ? C1 C6 C13 C15 -132.6(8) . . . . ? O4 P2 C16 C17 -135.0(8) . . . . ? O6 P2 C16 C17 100.2(8) . . . . ? O5 P2 C16 C17 -19.4(9) . . . . ? O4 P2 C16 C21 43.1(8) . . . . ? O6 P2 C16 C21 -81.7(7) . . . . ? O5 P2 C16 C21 158.7(6) . . . . ? C21 C16 C17 C18 -7.0(13) . . . . ? P2 C16 C17 C18 171.0(7) . . . . ? C21 C16 C17 C22 169.4(9) . . . . ? P2 C16 C17 C22 -12.6(15) . . . . ? C16 C17 C18 C19 2.0(15) . . . . ? C22 C17 C18 C19 -174.7(10) . . . . ? C17 C18 C19 C20 3.0(15) . . . . ? C17 C18 C19 C25 -176.3(10) . . . . ? C18 C19 C20 C21 -3.0(16) . . . . ? C25 C19 C20 C21 176.3(9) . . . . ? C19 C20 C21 C16 -1.9(15) . . . . ? C19 C20 C21 C28 178.8(10) . . . . ? C17 C16 C21 C20 7.0(13) . . . . ? P2 C16 C21 C20 -171.2(7) . . . . ? C17 C16 C21 C28 -173.7(9) . . . . ? P2 C16 C21 C28 8.1(12) . . . . ? C16 C17 C22 C23 -122.9(11) . . . . ? C18 C17 C22 C23 53.5(13) . . . . ? C16 C17 C22 C24 111.2(12) . . . . ? C18 C17 C22 C24 -72.4(12) . . . . ? C18 C19 C25 C26 59.5(16) . . . . ? C20 C19 C25 C26 -119.8(13) . . . . ? C18 C19 C25 C27 -65.9(14) . . . . ? C20 C19 C25 C27 114.8(13) . . . . ? C20 C21 C28 C30 67.0(11) . . . . ? C16 C21 C28 C30 -112.4(10) . . . . ? C20 C21 C28 C29 -56.2(11) . . . . ? C16 C21 C28 C29 124.5(9) . . . . ? O8 P3 C31 C36 99.5(7) . . . . ? O7 P3 C31 C36 -136.3(6) . . . . ? O9 P3 C31 C36 -23.0(7) . . . . ? Cd2 P3 C31 C36 -76.5(7) . . . . ? O8 P3 C31 C32 -83.9(6) . . . . ? O7 P3 C31 C32 40.4(7) . . . . ? O9 P3 C31 C32 153.6(6) . . . . ? Cd2 P3 C31 C32 100.2(6) . . . . ? C36 C31 C32 C33 7.0(11) . . . . ? P3 C31 C32 C33 -169.8(6) . . . . ? C36 C31 C32 C37 -170.6(7) . . . . ? P3 C31 C32 C37 12.6(10) . . . . ? C31 C32 C33 C34 -1.5(13) . . . . ? C37 C32 C33 C34 176.1(8) . . . . ? C32 C33 C34 C35 -3.4(14) . . . . ? C32 C33 C34 C40 178.4(9) . . . . ? C33 C34 C35 C36 2.8(15) . . . . ? C40 C34 C35 C36 -179.0(9) . . . . ? C34 C35 C36 C31 2.7(14) . . . . ? C34 C35 C36 C43 -173.7(9) . . . . ? C32 C31 C36 C35 -7.4(12) . . . . ? P3 C31 C36 C35 169.3(7) . . . . ? C32 C31 C36 C43 168.6(8) . . . . ? P3 C31 C36 C43 -14.7(12) . . . . ? C33 C32 C37 C38 72.9(9) . . . . ? C31 C32 C37 C38 -109.5(8) . . . . ? C33 C32 C37 C39 -49.7(10) . . . . ? C31 C32 C37 C39 127.8(8) . . . . ? C35 C36 C43 C44 -71.1(11) . . . . ? C31 C36 C43 C44 112.7(10) . . . . ? C35 C36 C43 C45 53.8(11) . . . . ? C31 C36 C43 C45 -122.3(10) . . . . ? Cd1 O10 C46 N1 -141.7(10) . . . . ? C47 N1 C46 O10 3.1(19) . . . . ? C48 N1 C46 O10 177.5(10) . . . . ? Cd2 O11 C49 N2 172.2(6) . . . . ? C51 N2 C49 O11 -4.5(14) . . . . ? C50 N2 C49 O11 179.4(5) . . . . ? C35 C34 C40 C42B -134(2) . . . . ? C33 C34 C40 C42B 44(2) . . . . ? C35 C34 C40 C41B 29(2) . . . . ? C33 C34 C40 C41B -152.8(18) . . . . ? C35 C34 C40 C42A 162.0(11) . . . . ? C33 C34 C40 C42A -19.9(16) . . . . ? C35 C34 C40 C41A -76.4(14) . . . . ? C33 C34 C40 C41A 101.7(12) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.522 _refine_diff_density_min -1.857 _refine_diff_density_rms 0.137 #===END data_DMF2 _database_code_depnum_ccdc_archive 'CCDC 679267' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium phosphonate' _chemical_melting_point 459.15 _chemical_formula_moiety 'C112 H136 Cd4 N8 O23 P6' _chemical_formula_sum 'C112 H136 Cd4 N8 O23 P6' _chemical_formula_weight 2597.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c _symmetry_space_group_name_HALL '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.0781(11) _cell_length_b 24.9027(18) _cell_length_c 17.1928(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.0370(10) _cell_angle_gamma 90.00 _cell_volume 6392.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9641 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.95 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2660 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8569 _exptl_absorpt_correction_T_max 0.8569 _exptl_absorpt_process_details SADABS _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 graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42173 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.29 _reflns_number_total 15780 _reflns_number_gt 12053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0684P)^2^+23.5896P] 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 15780 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.84746(2) 0.969516(13) 0.564685(19) 0.02121(9) Uani 1 1 d . . . Cd2 Cd 0.94274(2) 1.093248(13) 0.505673(18) 0.02024(9) Uani 1 1 d . . . P1 P 0.87224(8) 0.83484(5) 0.53370(8) 0.0243(3) Uani 1 1 d . . . P2 P 0.84949(9) 1.06737(6) 0.67389(7) 0.0267(3) Uani 1 1 d . . . P3 P 1.07365(8) 0.99903(5) 0.60733(6) 0.0179(2) Uani 1 1 d . . . O1 O 0.8221(2) 0.88672(14) 0.5377(2) 0.0336(8) Uani 1 1 d . . . O2 O 0.8863(2) 0.81106(15) 0.6203(2) 0.0317(8) Uani 1 1 d . . . H2 H 0.9098 0.7805 0.6200 0.047 Uiso 1 1 calc R . . O3 O 0.9620(2) 0.83883(15) 0.5053(2) 0.0317(8) Uani 1 1 d . . . O4 O 0.8395(2) 1.00735(16) 0.6802(2) 0.0339(8) Uani 1 1 d . . . O5 O 0.9436(2) 1.08602(15) 0.7197(2) 0.0302(8) Uani 1 1 d . . . H5 H 0.9851 1.0710 0.7001 0.045 Uiso 1 1 calc R . . O6 O 0.8419(2) 1.08554(18) 0.5901(2) 0.0370(9) Uani 1 1 d . . . O7 O 0.9998(2) 0.95689(13) 0.59213(18) 0.0231(7) Uani 1 1 d . . . O8 O 0.8645(2) 1.00998(13) 0.45504(18) 0.0236(7) Uani 1 1 d . . . O9 O 1.0354(2) 1.05590(12) 0.60713(17) 0.0195(6) Uani 1 1 d . . . O10 O 0.6925(2) 0.98472(16) 0.5473(2) 0.0357(9) Uani 1 1 d . . . N1 N 0.8405(3) 1.14671(17) 0.4320(3) 0.0306(10) Uani 1 1 d . . . N2 N 0.8755(3) 1.1980(2) 0.4219(3) 0.0426(12) Uani 1 1 d . . . H2A H 0.9310 1.2075 0.4389 0.051 Uiso 1 1 calc R . . N3 N 0.5846(3) 1.0022(2) 0.6225(3) 0.0454(13) Uani 1 1 d . . . C1 C 0.7682(3) 1.0997(2) 0.7285(3) 0.0297(11) Uani 1 1 d . . . C2 C 0.7111(4) 1.1412(2) 0.6962(3) 0.0361(13) Uani 1 1 d . . . C3 C 0.6436(4) 1.1597(3) 0.7384(4) 0.0420(14) Uani 1 1 d . . . C4 C 0.6321(4) 1.1378(3) 0.8112(4) 0.0410(14) Uani 1 1 d . . . C5 C 0.6912(4) 1.0983(2) 0.8433(3) 0.0350(12) Uani 1 1 d . . . C6 C 0.7589(4) 1.0794(2) 0.8032(3) 0.0312(11) Uani 1 1 d . . . C7 C 0.7205(4) 1.1693(3) 0.6194(4) 0.0506(17) Uani 1 1 d . . . H7 H 0.7338 1.1407 0.5817 0.061 Uiso 1 1 calc R . . C8 C 0.6377(6) 1.1985(4) 0.5810(5) 0.073(2) Uani 1 1 d . . . H8A H 0.5867 1.1738 0.5747 0.110 Uiso 1 1 calc R . . H8B H 0.6479 1.2119 0.5294 0.110 Uiso 1 1 calc R . . H8C H 0.6250 1.2288 0.6142 0.110 Uiso 1 1 calc R . . C9 C 0.7996(6) 1.2059(3) 0.6303(5) 0.068(2) Uiso 1 1 d . . . H9A H 0.8055 1.2236 0.5804 0.101 Uiso 1 1 calc R . . H9B H 0.8539 1.1851 0.6479 0.101 Uiso 1 1 calc R . . H9C H 0.7914 1.2331 0.6699 0.101 Uiso 1 1 calc R . . C10 C 0.5585(5) 1.1591(3) 0.8552(4) 0.0525(17) Uani 1 1 d . . . H10 H 0.5292 1.1895 0.8235 0.063 Uiso 1 1 calc R . . C11 C 0.5948(5) 1.1815(4) 0.9339(5) 0.080(3) Uani 1 1 d . . . H11A H 0.6396 1.2091 0.9277 0.119 Uiso 1 1 calc R . . H11B H 0.6226 1.1527 0.9676 0.119 Uiso 1 1 calc R . . H11C H 0.5459 1.1975 0.9581 0.119 Uiso 1 1 calc R . . C12 C 0.4883(5) 1.1177(4) 0.8591(5) 0.074(3) Uani 1 1 d . . . H12A H 0.4413 1.1323 0.8870 0.111 Uiso 1 1 calc R . . H12B H 0.5151 1.0861 0.8872 0.111 Uiso 1 1 calc R . . H12C H 0.4624 1.1073 0.8058 0.111 Uiso 1 1 calc R . . C13 C 0.8217(4) 1.0374(2) 0.8463(3) 0.0345(12) Uani 1 1 d . . . H13 H 0.8719 1.0315 0.8150 0.041 Uiso 1 1 calc R . . C14 C 0.7730(5) 0.9837(3) 0.8512(4) 0.0516(16) Uani 1 1 d . . . H14A H 0.8142 0.9574 0.8789 0.077 Uiso 1 1 calc R . . H14B H 0.7519 0.9707 0.7980 0.077 Uiso 1 1 calc R . . H14C H 0.7217 0.9888 0.8797 0.077 Uiso 1 1 calc R . . C15 C 0.8627(4) 1.0568(3) 0.9284(3) 0.0433(14) Uani 1 1 d . . . H15A H 0.9022 1.0289 0.9542 0.065 Uiso 1 1 calc R . . H15B H 0.8147 1.0642 0.9599 0.065 Uiso 1 1 calc R . . H15C H 0.8972 1.0897 0.9235 0.065 Uiso 1 1 calc R . . C16 C 0.7978(4) 0.7872(2) 0.4761(3) 0.0304(11) Uani 1 1 d . . . C17 C 0.7128(4) 0.7787(2) 0.4990(4) 0.0351(12) Uani 1 1 d . . . C18 C 0.6535(4) 0.7438(2) 0.4554(4) 0.0436(15) Uani 1 1 d . . . H18 H 0.5957 0.7389 0.4703 0.052 Uiso 1 1 calc R . . C19 C 0.6750(5) 0.7161(2) 0.3918(4) 0.0511(18) Uani 1 1 d . A . C20 C 0.7581(5) 0.7238(3) 0.3707(4) 0.0487(16) Uani 1 1 d . . . H20 H 0.7739 0.7044 0.3271 0.058 Uiso 1 1 calc R . . C21 C 0.8210(4) 0.7591(2) 0.4105(3) 0.0359(12) Uani 1 1 d . . . C22 C 0.6822(4) 0.8031(3) 0.5729(4) 0.0448(15) Uani 1 1 d . . . H22 H 0.7285 0.8297 0.5953 0.054 Uiso 1 1 calc R . . C23 C 0.5927(5) 0.8327(3) 0.5544(5) 0.069(2) Uani 1 1 d . . . H23A H 0.5979 0.8608 0.5154 0.104 Uiso 1 1 calc R . . H23B H 0.5771 0.8491 0.6025 0.104 Uiso 1 1 calc R . . H23C H 0.5458 0.8073 0.5334 0.104 Uiso 1 1 calc R . . C24 C 0.6781(5) 0.7588(3) 0.6340(4) 0.065(2) Uani 1 1 d . . . H24A H 0.7365 0.7411 0.6449 0.097 Uiso 1 1 calc R . . H24B H 0.6324 0.7324 0.6138 0.097 Uiso 1 1 calc R . . H24C H 0.6626 0.7746 0.6826 0.097 Uiso 1 1 calc R . . C25 C 0.6095(6) 0.6763(4) 0.3458(5) 0.074(2) Uiso 1 1 d . . . C26 C 0.5273(5) 0.7045(3) 0.3057(5) 0.063(2) Uani 1 1 d . A . C27A C 0.6111(9) 0.6254(4) 0.3875(9) 0.061(4) Uani 0.60 1 d P A 1 C27B C 0.6278(12) 0.6312(8) 0.3201(13) 0.065(6) Uani 0.40 1 d P A 2 C28 C 0.9121(5) 0.7620(3) 0.3811(3) 0.0441(15) Uani 1 1 d . . . H28 H 0.9370 0.7986 0.3941 0.053 Uiso 1 1 calc R . . C29 C 0.9092(5) 0.7541(3) 0.2924(4) 0.0588(18) Uiso 1 1 d . . . H29A H 0.9700 0.7567 0.2787 0.088 Uiso 1 1 calc R . . H29B H 0.8714 0.7818 0.2643 0.088 Uiso 1 1 calc R . . H29C H 0.8844 0.7186 0.2775 0.088 Uiso 1 1 calc R . . C30 C 0.9761(5) 0.7216(3) 0.4255(4) 0.0499(16) Uani 1 1 d . . . H30A H 1.0344 0.7238 0.4066 0.075 Uiso 1 1 calc R . . H30B H 0.9517 0.6853 0.4167 0.075 Uiso 1 1 calc R . . H30C H 0.9834 0.7298 0.4818 0.075 Uiso 1 1 calc R . . C31 C 1.1456(3) 0.98931(19) 0.7011(3) 0.0226(9) Uani 1 1 d . . . C32 C 1.1347(4) 0.9475(2) 0.7555(3) 0.0374(13) Uani 1 1 d . B . C33 C 1.1996(4) 0.9408(2) 0.8204(4) 0.0434(15) Uani 1 1 d . . . H33 H 1.1915 0.9134 0.8571 0.052 Uiso 1 1 calc R . . C34 C 1.2748(4) 0.9723(2) 0.8336(4) 0.0445(16) Uani 1 1 d . C . C35 C 1.2842(4) 1.0132(2) 0.7821(3) 0.0380(13) Uani 1 1 d . . . H35 H 1.3358 1.0355 0.7914 0.046 Uiso 1 1 calc R . . C36 C 1.2211(3) 1.0235(2) 0.7166(3) 0.0267(10) Uani 1 1 d . . . C37 C 1.0545(6) 0.9098(4) 0.7490(5) 0.075(3) Uani 1 1 d . . . C38A C 0.9861(10) 0.9198(6) 0.7859(11) 0.050(3) Uani 0.50 1 d P B 1 C39A C 1.0975(12) 0.8481(8) 0.7690(13) 0.041(5) Uani 0.50 1 d P B 1 C38B C 1.0033(9) 0.9273(5) 0.8352(9) 0.039(3) Uani 0.50 1 d P B 2 C39B C 1.0670(14) 0.8556(11) 0.7520(11) 0.057(7) Uani 0.50 1 d P B 2 C40 C 1.3445(6) 0.9620(3) 0.9065(5) 0.067(2) Uani 1 1 d . . . C41A C 1.4282(7) 0.9428(4) 0.8851(6) 0.056(2) Uiso 0.70 1 d P C 1 C41B C 1.368(2) 0.9040(14) 0.914(2) 0.084(9) Uiso 0.30 1 d P C 2 C42 C 1.3551(5) 1.0090(4) 0.9610(4) 0.061(2) Uani 1 1 d . C . C43 C 1.2370(3) 1.0723(2) 0.6667(3) 0.0276(10) Uani 1 1 d . . . H43 H 1.1885 1.0731 0.6207 0.033 Uiso 1 1 calc R . . C44 C 1.2293(4) 1.1231(2) 0.7142(3) 0.0388(13) Uani 1 1 d . . . H44A H 1.2397 1.1545 0.6823 0.058 Uiso 1 1 calc R . . H44B H 1.2741 1.1224 0.7613 0.058 Uiso 1 1 calc R . . H44C H 1.1693 1.1253 0.7296 0.058 Uiso 1 1 calc R . . C45 C 1.3272(4) 1.0697(3) 0.6352(3) 0.0371(13) Uani 1 1 d . . . H45A H 1.3346 1.1018 0.6039 0.056 Uiso 1 1 calc R . . H45B H 1.3288 1.0377 0.6022 0.056 Uiso 1 1 calc R . . H45C H 1.3759 1.0678 0.6793 0.056 Uiso 1 1 calc R . . C46 C 0.7016(5) 1.1009(3) 0.3993(5) 0.0580(19) Uani 1 1 d . . . H46A H 0.7366 1.0715 0.4263 0.087 Uiso 1 1 calc R . . H46B H 0.6803 1.0903 0.3450 0.087 Uiso 1 1 calc R . . H46C H 0.6502 1.1088 0.4266 0.087 Uiso 1 1 calc R . . C47 C 0.7577(4) 1.1485(3) 0.3994(4) 0.0445(15) Uani 1 1 d . . . C48 C 0.7354(5) 1.1976(3) 0.3678(4) 0.0576(19) Uani 1 1 d . . . H48 H 0.6790 1.2085 0.3407 0.069 Uiso 1 1 calc R . . C49 C 0.8158(5) 1.2299(3) 0.3841(4) 0.0523(17) Uani 1 1 d . . . C50 C 0.8355(6) 1.2864(3) 0.3649(7) 0.083(3) Uani 1 1 d . . . H50A H 0.8978 1.2948 0.3854 0.125 Uiso 1 1 calc R . . H50B H 0.7955 1.3105 0.3887 0.125 Uiso 1 1 calc R . . H50C H 0.8260 1.2912 0.3077 0.125 Uiso 1 1 calc R . . C51 C 0.6558(4) 0.9753(3) 0.6054(4) 0.0410(14) Uani 1 1 d . . . C52 C 0.5480(5) 1.0478(3) 0.5763(5) 0.0587(19) Uani 1 1 d . . . H52A H 0.4963 1.0620 0.5984 0.088 Uiso 1 1 calc R . . H52B H 0.5292 1.0364 0.5219 0.088 Uiso 1 1 calc R . . H52C H 0.5938 1.0758 0.5774 0.088 Uiso 1 1 calc R . . C53 C 0.5463(6) 0.9910(5) 0.6938(5) 0.093(4) Uani 1 1 d . . . H53A H 0.4948 1.0147 0.6964 0.139 Uiso 1 1 calc R . . H53B H 0.5915 0.9974 0.7396 0.139 Uiso 1 1 calc R . . H53C H 0.5267 0.9535 0.6936 0.139 Uiso 1 1 calc R . . C1S C 0.0531(5) 0.1612(2) 0.8682(3) 0.0434(15) Uani 1 1 d . . . C2S C 0.1884(6) 0.1396(3) 0.9567(5) 0.075(3) Uani 1 1 d . . . H2S1 H 0.2221 0.1072 0.9749 0.113 Uiso 1 1 calc R . . H2S2 H 0.1692 0.1582 1.0018 0.113 Uiso 1 1 calc R . . H2S3 H 0.2266 0.1635 0.9306 0.113 Uiso 1 1 calc R . . C3S C 0.0984(5) 0.0683(3) 0.8838(4) 0.0441(14) Uani 1 1 d . . . H3S1 H 0.1469 0.0478 0.9141 0.066 Uiso 1 1 calc R . . H3S2 H 0.0995 0.0626 0.8275 0.066 Uiso 1 1 calc R . . H3S3 H 0.0407 0.0563 0.8976 0.066 Uiso 1 1 calc R . . N1S N 0.1102(4) 0.1246(2) 0.9017(3) 0.0409(11) Uani 1 1 d . . . O1S O 0.7980(7) 0.8896(4) 0.7188(6) 0.057(3) Uani 0.50 1 d P . . O2S O 0.0585(4) 0.21001(19) 0.8818(3) 0.0587(13) 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 Cd1 0.02161(17) 0.01970(17) 0.02274(17) -0.00510(13) 0.00459(12) -0.00224(13) Cd2 0.01986(17) 0.02174(18) 0.01922(16) 0.00123(13) 0.00306(12) 0.00353(12) P1 0.0248(6) 0.0183(6) 0.0299(6) 0.0000(5) 0.0044(5) -0.0006(5) P2 0.0248(6) 0.0350(7) 0.0205(6) -0.0065(5) 0.0041(5) 0.0038(5) P3 0.0200(5) 0.0167(6) 0.0162(5) -0.0010(4) -0.0007(4) 0.0006(4) O1 0.0266(18) 0.0188(18) 0.054(2) -0.0079(16) 0.0023(17) -0.0062(14) O2 0.038(2) 0.030(2) 0.0271(18) -0.0014(15) 0.0068(15) -0.0034(16) O3 0.0297(19) 0.0272(19) 0.038(2) 0.0072(16) 0.0051(16) -0.0029(15) O4 0.032(2) 0.039(2) 0.0314(19) -0.0095(16) 0.0073(15) 0.0013(16) O5 0.0239(17) 0.040(2) 0.0265(17) -0.0099(15) 0.0024(14) 0.0071(15) O6 0.0256(19) 0.067(3) 0.0195(17) -0.0025(17) 0.0056(14) 0.0040(18) O7 0.0237(16) 0.0258(18) 0.0188(15) -0.0024(13) -0.0004(12) -0.0059(13) O8 0.0257(17) 0.0234(17) 0.0226(16) -0.0021(13) 0.0068(13) 0.0049(13) O9 0.0205(15) 0.0184(16) 0.0192(15) -0.0027(12) 0.0012(12) 0.0014(12) O10 0.0292(19) 0.044(2) 0.033(2) -0.0085(17) 0.0033(16) -0.0017(17) N1 0.036(2) 0.023(2) 0.033(2) 0.0058(18) 0.0054(19) 0.0136(18) N2 0.038(3) 0.036(3) 0.054(3) 0.009(2) 0.005(2) 0.004(2) N3 0.033(3) 0.061(4) 0.044(3) -0.005(3) 0.012(2) 0.011(2) C1 0.031(3) 0.034(3) 0.026(2) -0.005(2) 0.012(2) 0.007(2) C2 0.031(3) 0.042(3) 0.038(3) 0.003(2) 0.013(2) 0.012(2) C3 0.041(3) 0.043(3) 0.045(3) -0.009(3) 0.014(3) 0.009(3) C4 0.033(3) 0.048(4) 0.045(3) -0.010(3) 0.018(3) 0.003(3) C5 0.038(3) 0.038(3) 0.032(3) -0.005(2) 0.016(2) 0.000(2) C6 0.035(3) 0.031(3) 0.029(3) -0.004(2) 0.008(2) 0.000(2) C7 0.047(4) 0.056(4) 0.053(4) 0.015(3) 0.023(3) 0.028(3) C8 0.080(6) 0.078(6) 0.063(5) 0.034(4) 0.017(4) 0.022(5) C10 0.048(4) 0.059(4) 0.058(4) -0.004(3) 0.030(3) 0.011(3) C11 0.061(5) 0.084(6) 0.105(7) -0.057(5) 0.048(5) -0.009(4) C12 0.048(4) 0.092(6) 0.088(6) -0.042(5) 0.032(4) -0.013(4) C13 0.044(3) 0.034(3) 0.028(3) -0.002(2) 0.012(2) 0.002(2) C14 0.064(4) 0.034(3) 0.057(4) 0.003(3) 0.011(3) 0.000(3) C15 0.048(4) 0.053(4) 0.029(3) 0.003(3) 0.006(3) 0.007(3) C16 0.034(3) 0.019(2) 0.037(3) 0.003(2) -0.001(2) 0.000(2) C17 0.031(3) 0.023(3) 0.050(3) 0.002(2) 0.002(2) -0.006(2) C18 0.035(3) 0.027(3) 0.063(4) -0.001(3) -0.011(3) -0.007(2) C19 0.058(4) 0.023(3) 0.061(4) 0.001(3) -0.029(3) -0.003(3) C20 0.067(5) 0.034(3) 0.040(3) -0.003(3) -0.011(3) 0.005(3) C21 0.054(4) 0.019(3) 0.033(3) -0.005(2) -0.002(2) 0.004(2) C22 0.037(3) 0.045(4) 0.055(4) -0.009(3) 0.014(3) -0.014(3) C23 0.053(4) 0.063(5) 0.099(6) -0.007(5) 0.036(4) 0.007(4) C24 0.062(5) 0.077(6) 0.057(4) 0.000(4) 0.013(4) -0.011(4) C26 0.035(4) 0.079(5) 0.067(5) -0.021(4) -0.015(3) 0.002(3) C27A 0.068(8) 0.024(5) 0.083(9) -0.008(6) -0.021(7) -0.013(5) C27B 0.052(10) 0.048(11) 0.085(15) -0.045(11) -0.023(10) 0.017(8) C28 0.066(4) 0.033(3) 0.032(3) -0.010(2) 0.003(3) 0.007(3) C30 0.054(4) 0.060(4) 0.036(3) -0.002(3) 0.004(3) 0.013(3) C31 0.025(2) 0.017(2) 0.024(2) 0.0023(18) -0.0008(18) 0.0027(18) C32 0.043(3) 0.033(3) 0.033(3) 0.007(2) -0.006(2) -0.004(2) C33 0.056(4) 0.029(3) 0.039(3) 0.014(3) -0.012(3) -0.001(3) C34 0.053(4) 0.028(3) 0.044(3) 0.006(3) -0.024(3) 0.005(3) C35 0.039(3) 0.028(3) 0.042(3) -0.003(2) -0.011(2) -0.003(2) C36 0.029(3) 0.025(3) 0.024(2) -0.0011(19) -0.0060(19) 0.003(2) C37 0.073(5) 0.075(6) 0.066(5) 0.056(4) -0.033(4) -0.043(4) C38A 0.043(8) 0.036(7) 0.074(11) -0.004(8) 0.018(8) 0.007(6) C39A 0.041(10) 0.018(6) 0.060(12) 0.006(6) -0.008(7) -0.006(6) C38B 0.037(7) 0.037(7) 0.045(7) -0.011(6) 0.011(6) 0.001(5) C39B 0.062(14) 0.089(18) 0.028(8) -0.019(9) 0.028(9) -0.037(12) C40 0.076(5) 0.046(4) 0.065(5) 0.015(4) -0.043(4) 0.000(4) C42 0.062(5) 0.088(6) 0.030(3) 0.002(3) -0.012(3) -0.006(4) C43 0.023(2) 0.026(3) 0.034(3) 0.000(2) 0.002(2) -0.0003(19) C44 0.044(3) 0.032(3) 0.041(3) 0.003(2) 0.006(3) 0.003(2) C45 0.029(3) 0.043(3) 0.039(3) -0.004(3) 0.005(2) -0.001(2) C46 0.063(5) 0.044(4) 0.070(5) -0.011(3) 0.020(4) -0.005(3) C47 0.036(3) 0.050(4) 0.047(3) 0.005(3) 0.009(3) 0.010(3) C48 0.044(4) 0.063(5) 0.065(4) 0.023(4) 0.006(3) 0.025(3) C49 0.051(4) 0.039(4) 0.069(4) 0.020(3) 0.014(3) 0.013(3) C50 0.055(5) 0.050(5) 0.144(9) 0.042(5) 0.014(5) 0.005(4) C51 0.023(3) 0.052(4) 0.047(3) 0.000(3) 0.004(2) 0.000(2) C52 0.044(4) 0.059(5) 0.075(5) -0.004(4) 0.013(4) 0.017(3) C53 0.056(5) 0.173(11) 0.056(5) 0.027(6) 0.028(4) 0.029(6) C1S 0.068(4) 0.032(3) 0.032(3) -0.004(2) 0.011(3) -0.009(3) C2S 0.077(6) 0.064(5) 0.076(6) -0.022(4) -0.023(5) -0.003(4) C3S 0.057(4) 0.038(3) 0.034(3) 0.000(3) -0.003(3) -0.003(3) N1S 0.050(3) 0.039(3) 0.033(2) -0.008(2) 0.001(2) -0.005(2) O1S 0.058(6) 0.048(6) 0.065(6) -0.011(5) 0.005(5) 0.010(5) O2S 0.089(4) 0.038(3) 0.050(3) -0.003(2) 0.013(3) -0.012(2) _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 O1 2.136(3) . ? Cd1 O8 2.184(3) . ? Cd1 O4 2.217(4) . ? Cd1 O7 2.300(3) . ? Cd1 O10 2.345(4) . ? Cd1 P2 3.0738(13) . ? Cd2 O3 2.244(4) 3_776 ? Cd2 O6 2.252(4) . ? Cd2 O9 2.275(3) . ? Cd2 N1 2.282(4) . ? Cd2 O7 2.355(3) 3_776 ? Cd2 O8 2.482(3) . ? Cd2 P3 2.9971(12) 3_776 ? P1 O1 1.503(4) . ? P1 O3 1.505(4) . ? P1 O2 1.588(4) . ? P1 C16 1.826(5) . ? P2 O6 1.499(4) . ? P2 O4 1.508(4) . ? P2 O5 1.592(4) . ? P2 C1 1.831(5) . ? P3 O7 1.526(3) . ? P3 O9 1.529(3) . ? P3 O8 1.533(3) 3_776 ? P3 C31 1.829(5) . ? P3 Cd2 2.9971(12) 3_776 ? O2 H2 0.8400 . ? O3 Cd2 2.244(3) 3_776 ? O5 H5 0.8400 . ? O7 Cd2 2.355(3) 3_776 ? O8 P3 1.533(3) 3_776 ? O10 C51 1.230(7) . ? N1 C47 1.296(7) . ? N1 N2 1.402(7) . ? N2 C49 1.303(8) . ? N2 H2A 0.8800 . ? N3 C51 1.332(7) . ? N3 C52 1.450(9) . ? N3 C53 1.454(9) . ? C1 C6 1.406(7) . ? C1 C2 1.408(7) . ? C2 C3 1.408(7) . ? C2 C7 1.519(8) . ? C3 C4 1.398(9) . ? C4 C5 1.389(9) . ? C4 C10 1.524(8) . ? C5 C6 1.390(7) . ? C6 C13 1.530(8) . ? C7 C9 1.492(11) . ? C7 C8 1.515(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.486(10) . ? C10 C11 1.495(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.533(8) . ? C13 C15 1.538(8) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.408(8) . ? C16 C21 1.413(8) . ? C17 C18 1.390(8) . ? C17 C22 1.536(8) . ? C18 C19 1.370(10) . ? C18 H18 0.9500 . ? C19 C20 1.365(10) . ? C19 C25 1.538(11) . ? C20 C21 1.398(8) . ? C20 H20 0.9500 . ? C21 C28 1.530(9) . ? C22 C24 1.530(10) . ? C22 C23 1.533(10) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27B 1.251(17) . ? C25 C27A 1.454(15) . ? C25 C26 1.505(11) . ? C28 C30 1.523(9) . ? C28 C29 1.532(9) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.417(7) . ? C31 C32 1.423(7) . ? C32 C33 1.387(8) . ? C32 C37 1.523(9) . ? C33 C34 1.370(9) . ? C33 H33 0.9500 . ? C34 C35 1.372(8) . ? C34 C40 1.540(8) . ? C35 C36 1.393(7) . ? C35 H35 0.9500 . ? C36 C43 1.526(7) . ? C37 C38A 1.309(17) . ? C37 C39B 1.36(3) . ? C37 C39A 1.68(2) . ? C37 C38B 1.819(16) . ? C40 C41A 1.443(14) . ? C40 C41B 1.49(3) . ? C40 C42 1.496(11) . ? C43 C44 1.519(8) . ? C43 C45 1.536(7) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.455(9) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.363(9) . ? C48 C49 1.449(10) . ? C48 H48 0.9500 . ? C49 C50 1.484(10) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C1S O2S 1.239(7) . ? C1S N1S 1.329(8) . ? C2S N1S 1.454(9) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S N1S 1.439(8) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 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 Cd1 O8 107.29(14) . . ? O1 Cd1 O4 125.03(15) . . ? O8 Cd1 O4 127.23(14) . . ? O1 Cd1 O7 93.20(13) . . ? O8 Cd1 O7 90.32(12) . . ? O4 Cd1 O7 92.98(12) . . ? O1 Cd1 O10 89.04(14) . . ? O8 Cd1 O10 92.91(13) . . ? O4 Cd1 O10 82.40(13) . . ? O7 Cd1 O10 175.34(12) . . ? O1 Cd1 P2 152.12(11) . . ? O8 Cd1 P2 99.73(9) . . ? O4 Cd1 P2 27.50(11) . . ? O7 Cd1 P2 93.37(8) . . ? O10 Cd1 P2 82.79(10) . . ? O3 Cd2 O6 128.03(15) 3_776 . ? O3 Cd2 O9 92.34(12) 3_776 . ? O6 Cd2 O9 82.45(12) . . ? O3 Cd2 N1 84.50(15) 3_776 . ? O6 Cd2 N1 86.74(15) . . ? O9 Cd2 N1 163.48(13) . . ? O3 Cd2 O7 92.05(12) 3_776 3_776 ? O6 Cd2 O7 139.82(14) . 3_776 ? O9 Cd2 O7 94.75(11) . 3_776 ? N1 Cd2 O7 101.56(13) . 3_776 ? O3 Cd2 O8 151.48(12) 3_776 . ? O6 Cd2 O8 79.87(13) . . ? O9 Cd2 O8 97.93(11) . . ? N1 Cd2 O8 92.39(14) . . ? O7 Cd2 O8 60.73(11) 3_776 . ? O3 Cd2 P3 121.28(10) 3_776 3_776 ? O6 Cd2 P3 110.52(11) . 3_776 ? O9 Cd2 P3 99.77(8) . 3_776 ? N1 Cd2 P3 95.70(12) . 3_776 ? O7 Cd2 P3 30.21(8) 3_776 3_776 ? O8 Cd2 P3 30.70(7) . 3_776 ? O1 P1 O3 116.0(2) . . ? O1 P1 O2 106.2(2) . . ? O3 P1 O2 108.7(2) . . ? O1 P1 C16 108.0(2) . . ? O3 P1 C16 112.3(2) . . ? O2 P1 C16 104.9(2) . . ? O6 P2 O4 112.0(2) . . ? O6 P2 O5 109.3(2) . . ? O4 P2 O5 110.2(2) . . ? O6 P2 C1 113.2(2) . . ? O4 P2 C1 108.5(2) . . ? O5 P2 C1 103.4(2) . . ? O6 P2 Cd1 70.08(17) . . ? O4 P2 Cd1 42.76(14) . . ? O5 P2 Cd1 117.74(14) . . ? C1 P2 Cd1 135.32(18) . . ? O7 P3 O9 111.73(19) . . ? O7 P3 O8 106.28(19) . 3_776 ? O9 P3 O8 113.60(18) . 3_776 ? O7 P3 C31 112.9(2) . . ? O9 P3 C31 107.56(19) . . ? O8 P3 C31 104.7(2) 3_776 . ? O7 P3 Cd2 50.93(13) . 3_776 ? O9 P3 Cd2 135.38(12) . 3_776 ? O8 P3 Cd2 55.76(13) 3_776 3_776 ? C31 P3 Cd2 117.06(15) . 3_776 ? P1 O1 Cd1 139.8(2) . . ? P1 O2 H2 109.5 . . ? P1 O3 Cd2 133.8(2) . 3_776 ? P2 O4 Cd1 109.7(2) . . ? P2 O5 H5 109.5 . . ? P2 O6 Cd2 132.6(2) . . ? P3 O7 Cd1 128.7(2) . . ? P3 O7 Cd2 98.86(16) . 3_776 ? Cd1 O7 Cd2 112.50(13) . 3_776 ? P3 O8 Cd1 133.85(19) 3_776 . ? P3 O8 Cd2 93.55(16) 3_776 . ? Cd1 O8 Cd2 100.97(12) . . ? P3 O9 Cd2 124.85(17) . . ? C51 O10 Cd1 114.8(4) . . ? C47 N1 N2 105.8(5) . . ? C47 N1 Cd2 142.6(4) . . ? N2 N1 Cd2 111.3(3) . . ? C49 N2 N1 111.8(5) . . ? C49 N2 H2A 124.1 . . ? N1 N2 H2A 124.1 . . ? C51 N3 C52 122.0(6) . . ? C51 N3 C53 121.2(6) . . ? C52 N3 C53 116.5(6) . . ? C6 C1 C2 119.3(5) . . ? C6 C1 P2 118.1(4) . . ? C2 C1 P2 122.5(4) . . ? C3 C2 C1 118.9(5) . . ? C3 C2 C7 117.4(5) . . ? C1 C2 C7 123.7(5) . . ? C4 C3 C2 121.5(6) . . ? C5 C4 C3 118.6(5) . . ? C5 C4 C10 121.4(6) . . ? C3 C4 C10 119.9(6) . . ? C4 C5 C6 121.2(5) . . ? C5 C6 C1 120.4(5) . . ? C5 C6 C13 116.0(5) . . ? C1 C6 C13 123.6(5) . . ? C9 C7 C8 110.9(7) . . ? C9 C7 C2 110.0(6) . . ? C8 C7 C2 115.4(5) . . ? C9 C7 H7 106.7 . . ? C8 C7 H7 106.7 . . ? C2 C7 H7 106.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 113.0(6) . . ? C12 C10 C4 110.6(6) . . ? C11 C10 C4 112.4(6) . . ? C12 C10 H10 106.8 . . ? C11 C10 H10 106.8 . . ? C4 C10 H10 106.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 C14 110.8(5) . . ? C6 C13 C15 111.8(5) . . ? C14 C13 C15 110.9(5) . . ? C6 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.0(5) . . ? C17 C16 P1 117.4(4) . . ? C21 C16 P1 123.6(4) . . ? C18 C17 C16 119.1(6) . . ? C18 C17 C22 116.6(5) . . ? C16 C17 C22 124.2(5) . . ? C19 C18 C17 122.6(6) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C20 C19 C18 118.0(6) . . ? C20 C19 C25 120.2(7) . . ? C18 C19 C25 121.8(7) . . ? C19 C20 C21 123.0(6) . . ? C19 C20 H20 118.5 . . ? C21 C20 H20 118.5 . . ? C20 C21 C16 118.3(6) . . ? C20 C21 C28 116.6(5) . . ? C16 C21 C28 125.0(5) . . ? C24 C22 C23 111.7(6) . . ? C24 C22 C17 109.3(6) . . ? C23 C22 C17 112.1(6) . . ? C24 C22 H22 107.8 . . ? C23 C22 H22 107.8 . . ? C17 C22 H22 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27B C25 C27A 53.4(13) . . ? C27B C25 C26 117.7(11) . . ? C27A C25 C26 126.1(9) . . ? C27B C25 C19 127.0(11) . . ? C27A C25 C19 110.1(8) . . ? C26 C25 C19 111.3(7) . . ? C30 C28 C21 109.8(5) . . ? C30 C28 C29 110.0(5) . . ? C21 C28 C29 114.9(5) . . ? C30 C28 H28 107.3 . . ? C21 C28 H28 107.3 . . ? C29 C28 H28 107.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 118.7(4) . . ? C36 C31 P3 116.6(3) . . ? C32 C31 P3 124.6(4) . . ? C33 C32 C31 118.9(5) . . ? C33 C32 C37 116.6(5) . . ? C31 C32 C37 124.5(5) . . ? C34 C33 C32 122.6(5) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C33 C34 C35 118.4(5) . . ? C33 C34 C40 119.7(6) . . ? C35 C34 C40 121.9(6) . . ? C34 C35 C36 122.5(5) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C31 118.8(5) . . ? C35 C36 C43 117.2(5) . . ? C31 C36 C43 124.0(4) . . ? C38A C37 C39B 106.5(11) . . ? C38A C37 C32 121.2(11) . . ? C39B C37 C32 120.4(11) . . ? C38A C37 C39A 112.5(11) . . ? C39B C37 C39A 16.6(12) . . ? C32 C37 C39A 105.6(9) . . ? C38A C37 C38B 26.5(8) . . ? C39B C37 C38B 106.2(9) . . ? C32 C37 C38B 102.4(7) . . ? C39A C37 C38B 104.4(10) . . ? C41A C40 C41B 59.7(14) . . ? C41A C40 C42 113.4(7) . . ? C41B C40 C42 134.4(14) . . ? C41A C40 C34 111.7(8) . . ? C41B C40 C34 111.3(14) . . ? C42 C40 C34 112.4(6) . . ? C44 C43 C36 109.5(4) . . ? C44 C43 C45 111.3(4) . . ? C36 C43 C45 112.4(4) . . ? C44 C43 H43 107.8 . . ? C36 C43 H43 107.8 . . ? C45 C43 H43 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N1 C47 C48 111.8(6) . . ? N1 C47 C46 119.9(6) . . ? C48 C47 C46 128.3(7) . . ? C47 C48 C49 105.6(6) . . ? C47 C48 H48 127.2 . . ? C49 C48 H48 127.2 . . ? N2 C49 C48 105.0(6) . . ? N2 C49 C50 122.9(7) . . ? C48 C49 C50 132.1(6) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O10 C51 N3 123.4(6) . . ? N3 C52 H52A 109.5 . . ? N3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N3 C53 H53A 109.5 . . ? N3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O2S C1S N1S 124.8(6) . . ? N1S C2S H2S1 109.5 . . ? N1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N1S C3S H3S1 109.5 . . ? N1S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? N1S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C1S N1S C3S 121.4(5) . . ? C1S N1S C2S 121.5(6) . . ? C3S N1S C2S 117.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 P2 O6 -154.5(3) . . . . ? O8 Cd1 P2 O6 11.29(18) . . . . ? O4 Cd1 P2 O6 -167.8(3) . . . . ? O7 Cd1 P2 O6 102.19(17) . . . . ? O10 Cd1 P2 O6 -80.45(18) . . . . ? O1 Cd1 P2 O4 13.3(3) . . . . ? O8 Cd1 P2 O4 179.1(2) . . . . ? O7 Cd1 P2 O4 -90.0(2) . . . . ? O10 Cd1 P2 O4 87.4(2) . . . . ? O1 Cd1 P2 O5 103.6(3) . . . . ? O8 Cd1 P2 O5 -90.62(19) . . . . ? O4 Cd1 P2 O5 90.3(3) . . . . ? O7 Cd1 P2 O5 0.28(19) . . . . ? O10 Cd1 P2 O5 177.6(2) . . . . ? O1 Cd1 P2 C1 -51.3(3) . . . . ? O8 Cd1 P2 C1 114.5(3) . . . . ? O4 Cd1 P2 C1 -64.6(3) . . . . ? O7 Cd1 P2 C1 -154.6(3) . . . . ? O10 Cd1 P2 C1 22.8(3) . . . . ? O3 P1 O1 Cd1 -35.8(5) . . . . ? O2 P1 O1 Cd1 85.1(4) . . . . ? C16 P1 O1 Cd1 -162.8(4) . . . . ? O8 Cd1 O1 P1 90.8(4) . . . . ? O4 Cd1 O1 P1 -96.4(4) . . . . ? O7 Cd1 O1 P1 -0.5(4) . . . . ? O10 Cd1 O1 P1 -176.4(4) . . . . ? P2 Cd1 O1 P1 -103.9(4) . . . . ? O1 P1 O3 Cd2 18.2(4) . . . 3_776 ? O2 P1 O3 Cd2 -101.4(3) . . . 3_776 ? C16 P1 O3 Cd2 143.1(3) . . . 3_776 ? O6 P2 O4 Cd1 12.3(3) . . . . ? O5 P2 O4 Cd1 -109.5(2) . . . . ? C1 P2 O4 Cd1 138.0(2) . . . . ? O1 Cd1 O4 P2 -172.43(17) . . . . ? O8 Cd1 O4 P2 -1.1(3) . . . . ? O7 Cd1 O4 P2 91.6(2) . . . . ? O10 Cd1 O4 P2 -89.0(2) . . . . ? O4 P2 O6 Cd2 -86.8(4) . . . . ? O5 P2 O6 Cd2 35.6(4) . . . . ? C1 P2 O6 Cd2 150.2(3) . . . . ? Cd1 P2 O6 Cd2 -77.9(3) . . . . ? O3 Cd2 O6 P2 -82.8(4) 3_776 . . . ? O9 Cd2 O6 P2 4.3(3) . . . . ? N1 Cd2 O6 P2 -163.2(4) . . . . ? O7 Cd2 O6 P2 92.7(4) 3_776 . . . ? O8 Cd2 O6 P2 103.8(4) . . . . ? P3 Cd2 O6 P2 101.9(3) 3_776 . . . ? O9 P3 O7 Cd1 3.2(3) . . . . ? O8 P3 O7 Cd1 -121.3(2) 3_776 . . . ? C31 P3 O7 Cd1 124.5(2) . . . . ? Cd2 P3 O7 Cd1 -128.4(3) 3_776 . . . ? O9 P3 O7 Cd2 131.56(15) . . . 3_776 ? O8 P3 O7 Cd2 7.13(19) 3_776 . . 3_776 ? C31 P3 O7 Cd2 -107.08(19) . . . 3_776 ? O1 Cd1 O7 P3 171.2(2) . . . . ? O8 Cd1 O7 P3 63.9(2) . . . . ? O4 Cd1 O7 P3 -63.5(2) . . . . ? O10 Cd1 O7 P3 -70.1(17) . . . . ? P2 Cd1 O7 P3 -35.9(2) . . . . ? O1 Cd1 O7 Cd2 48.16(17) . . . 3_776 ? O8 Cd1 O7 Cd2 -59.18(15) . . . 3_776 ? O4 Cd1 O7 Cd2 173.51(16) . . . 3_776 ? O10 Cd1 O7 Cd2 166.8(15) . . . 3_776 ? P2 Cd1 O7 Cd2 -158.96(12) . . . 3_776 ? O1 Cd1 O8 P3 -55.4(3) . . . 3_776 ? O4 Cd1 O8 P3 132.0(3) . . . 3_776 ? O7 Cd1 O8 P3 38.1(3) . . . 3_776 ? O10 Cd1 O8 P3 -145.3(3) . . . 3_776 ? P2 Cd1 O8 P3 131.5(3) . . . 3_776 ? O1 Cd1 O8 Cd2 -161.27(12) . . . . ? O4 Cd1 O8 Cd2 26.17(19) . . . . ? O7 Cd1 O8 Cd2 -67.82(12) . . . . ? O10 Cd1 O8 Cd2 108.83(13) . . . . ? P2 Cd1 O8 Cd2 25.65(11) . . . . ? O3 Cd2 O8 P3 14.3(3) 3_776 . . 3_776 ? O6 Cd2 O8 P3 -176.59(17) . . . 3_776 ? O9 Cd2 O8 P3 -95.78(15) . . . 3_776 ? N1 Cd2 O8 P3 97.15(17) . . . 3_776 ? O7 Cd2 O8 P3 -4.77(13) 3_776 . . 3_776 ? O3 Cd2 O8 Cd1 150.2(2) 3_776 . . . ? O6 Cd2 O8 Cd1 -40.62(13) . . . . ? O9 Cd2 O8 Cd1 40.19(13) . . . . ? N1 Cd2 O8 Cd1 -126.88(15) . . . . ? O7 Cd2 O8 Cd1 131.20(16) 3_776 . . . ? P3 Cd2 O8 Cd1 136.0(2) 3_776 . . . ? O7 P3 O9 Cd2 -56.8(3) . . . . ? O8 P3 O9 Cd2 63.4(3) 3_776 . . . ? C31 P3 O9 Cd2 178.8(2) . . . . ? Cd2 P3 O9 Cd2 -1.0(3) 3_776 . . . ? O3 Cd2 O9 P3 -121.6(2) 3_776 . . . ? O6 Cd2 O9 P3 110.4(2) . . . . ? N1 Cd2 O9 P3 159.9(4) . . . . ? O7 Cd2 O9 P3 -29.3(2) 3_776 . . . ? O8 Cd2 O9 P3 31.8(2) . . . . ? P3 Cd2 O9 P3 0.7(2) 3_776 . . . ? O1 Cd1 O10 C51 84.4(4) . . . . ? O8 Cd1 O10 C51 -168.3(4) . . . . ? O4 Cd1 O10 C51 -41.1(4) . . . . ? O7 Cd1 O10 C51 -34.4(18) . . . . ? P2 Cd1 O10 C51 -68.8(4) . . . . ? O3 Cd2 N1 C47 179.0(7) 3_776 . . . ? O6 Cd2 N1 C47 -52.3(7) . . . . ? O9 Cd2 N1 C47 -101.4(8) . . . . ? O7 Cd2 N1 C47 88.0(7) 3_776 . . . ? O8 Cd2 N1 C47 27.4(7) . . . . ? P3 Cd2 N1 C47 58.0(7) 3_776 . . . ? O3 Cd2 N1 N2 -7.8(3) 3_776 . . . ? O6 Cd2 N1 N2 120.9(4) . . . . ? O9 Cd2 N1 N2 71.8(6) . . . . ? O7 Cd2 N1 N2 -98.8(3) 3_776 . . . ? O8 Cd2 N1 N2 -159.4(3) . . . . ? P3 Cd2 N1 N2 -128.8(3) 3_776 . . . ? C47 N1 N2 C49 -0.2(7) . . . . ? Cd2 N1 N2 C49 -175.9(5) . . . . ? O6 P2 C1 C6 169.6(4) . . . . ? O4 P2 C1 C6 44.7(5) . . . . ? O5 P2 C1 C6 -72.2(5) . . . . ? Cd1 P2 C1 C6 85.0(5) . . . . ? O6 P2 C1 C2 -6.1(6) . . . . ? O4 P2 C1 C2 -130.9(5) . . . . ? O5 P2 C1 C2 112.1(5) . . . . ? Cd1 P2 C1 C2 -90.6(5) . . . . ? C6 C1 C2 C3 -2.8(9) . . . . ? P2 C1 C2 C3 172.8(5) . . . . ? C6 C1 C2 C7 174.4(6) . . . . ? P2 C1 C2 C7 -9.9(9) . . . . ? C1 C2 C3 C4 0.0(9) . . . . ? C7 C2 C3 C4 -177.5(6) . . . . ? C2 C3 C4 C5 2.5(10) . . . . ? C2 C3 C4 C10 179.7(6) . . . . ? C3 C4 C5 C6 -2.1(9) . . . . ? C10 C4 C5 C6 -179.2(6) . . . . ? C4 C5 C6 C1 -0.8(9) . . . . ? C4 C5 C6 C13 177.8(5) . . . . ? C2 C1 C6 C5 3.3(8) . . . . ? P2 C1 C6 C5 -172.5(4) . . . . ? C2 C1 C6 C13 -175.3(5) . . . . ? P2 C1 C6 C13 8.9(7) . . . . ? C3 C2 C7 C9 103.9(7) . . . . ? C1 C2 C7 C9 -73.4(8) . . . . ? C3 C2 C7 C8 -22.4(10) . . . . ? C1 C2 C7 C8 160.3(7) . . . . ? C5 C4 C10 C12 -70.1(9) . . . . ? C3 C4 C10 C12 112.8(8) . . . . ? C5 C4 C10 C11 57.2(9) . . . . ? C3 C4 C10 C11 -119.9(8) . . . . ? C5 C6 C13 C14 70.7(6) . . . . ? C1 C6 C13 C14 -110.7(6) . . . . ? C5 C6 C13 C15 -53.6(7) . . . . ? C1 C6 C13 C15 125.0(6) . . . . ? O1 P1 C16 C17 -52.9(5) . . . . ? O3 P1 C16 C17 177.9(4) . . . . ? O2 P1 C16 C17 60.0(5) . . . . ? O1 P1 C16 C21 126.7(4) . . . . ? O3 P1 C16 C21 -2.4(5) . . . . ? O2 P1 C16 C21 -120.3(4) . . . . ? C21 C16 C17 C18 -1.3(8) . . . . ? P1 C16 C17 C18 178.4(4) . . . . ? C21 C16 C17 C22 174.8(5) . . . . ? P1 C16 C17 C22 -5.5(7) . . . . ? C16 C17 C18 C19 1.5(9) . . . . ? C22 C17 C18 C19 -174.8(6) . . . . ? C17 C18 C19 C20 -0.5(9) . . . . ? C17 C18 C19 C25 178.1(6) . . . . ? C18 C19 C20 C21 -0.9(9) . . . . ? C25 C19 C20 C21 -179.4(6) . . . . ? C19 C20 C21 C16 1.1(9) . . . . ? C19 C20 C21 C28 178.3(6) . . . . ? C17 C16 C21 C20 0.0(8) . . . . ? P1 C16 C21 C20 -179.6(4) . . . . ? C17 C16 C21 C28 -176.9(5) . . . . ? P1 C16 C21 C28 3.5(8) . . . . ? C18 C17 C22 C24 68.2(7) . . . . ? C16 C17 C22 C24 -107.9(6) . . . . ? C18 C17 C22 C23 -56.2(7) . . . . ? C16 C17 C22 C23 127.6(6) . . . . ? C20 C19 C25 C27B 40(2) . . . . ? C18 C19 C25 C27B -138.1(17) . . . . ? C20 C19 C25 C27A 99.1(10) . . . . ? C18 C19 C25 C27A -79.4(11) . . . . ? C20 C19 C25 C26 -116.3(8) . . . . ? C18 C19 C25 C26 65.2(9) . . . . ? C20 C21 C28 C30 -91.3(6) . . . . ? C16 C21 C28 C30 85.7(7) . . . . ? C20 C21 C28 C29 33.3(8) . . . . ? C16 C21 C28 C29 -149.8(6) . . . . ? O7 P3 C31 C36 174.1(4) . . . . ? O9 P3 C31 C36 -62.2(4) . . . . ? O8 P3 C31 C36 58.9(4) 3_776 . . . ? Cd2 P3 C31 C36 117.6(4) 3_776 . . . ? O7 P3 C31 C32 -0.6(5) . . . . ? O9 P3 C31 C32 123.1(5) . . . . ? O8 P3 C31 C32 -115.7(5) 3_776 . . . ? Cd2 P3 C31 C32 -57.0(5) 3_776 . . . ? C36 C31 C32 C33 -1.8(8) . . . . ? P3 C31 C32 C33 172.8(5) . . . . ? C36 C31 C32 C37 176.6(7) . . . . ? P3 C31 C32 C37 -8.9(9) . . . . ? C31 C32 C33 C34 -1.2(10) . . . . ? C37 C32 C33 C34 -179.7(8) . . . . ? C32 C33 C34 C35 2.6(10) . . . . ? C32 C33 C34 C40 -179.2(7) . . . . ? C33 C34 C35 C36 -1.0(10) . . . . ? C40 C34 C35 C36 -179.1(6) . . . . ? C34 C35 C36 C31 -1.9(9) . . . . ? C34 C35 C36 C43 176.4(6) . . . . ? C32 C31 C36 C35 3.3(8) . . . . ? P3 C31 C36 C35 -171.7(4) . . . . ? C32 C31 C36 C43 -175.0(5) . . . . ? P3 C31 C36 C43 10.0(7) . . . . ? C33 C32 C37 C38A 83.7(12) . . . . ? C31 C32 C37 C38A -94.6(11) . . . . ? C33 C32 C37 C39B -53.9(13) . . . . ? C31 C32 C37 C39B 127.7(11) . . . . ? C33 C32 C37 C39A -45.6(12) . . . . ? C31 C32 C37 C39A 136.1(10) . . . . ? C33 C32 C37 C38B 63.4(9) . . . . ? C31 C32 C37 C38B -114.9(7) . . . . ? C33 C34 C40 C41A 113.3(9) . . . . ? C35 C34 C40 C41A -68.6(9) . . . . ? C33 C34 C40 C41B 48.6(18) . . . . ? C35 C34 C40 C41B -133.3(16) . . . . ? C33 C34 C40 C42 -118.0(8) . . . . ? C35 C34 C40 C42 60.1(10) . . . . ? C35 C36 C43 C44 -66.1(6) . . . . ? C31 C36 C43 C44 112.2(5) . . . . ? C35 C36 C43 C45 58.1(6) . . . . ? C31 C36 C43 C45 -123.6(5) . . . . ? N2 N1 C47 C48 0.4(7) . . . . ? Cd2 N1 C47 C48 173.9(5) . . . . ? N2 N1 C47 C46 179.7(6) . . . . ? Cd2 N1 C47 C46 -6.9(10) . . . . ? N1 C47 C48 C49 -0.5(8) . . . . ? C46 C47 C48 C49 -179.7(7) . . . . ? N1 N2 C49 C48 -0.1(8) . . . . ? N1 N2 C49 C50 -179.4(7) . . . . ? C47 C48 C49 N2 0.3(8) . . . . ? C47 C48 C49 C50 179.5(9) . . . . ? Cd1 O10 C51 N3 147.9(5) . . . . ? C52 N3 C51 O10 -4.6(10) . . . . ? C53 N3 C51 O10 -177.2(7) . . . . ? O2S C1S N1S C3S 178.8(6) . . . . ? O2S C1S N1S C2S -2.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.788 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.157 #===END data_CD2(bipy)2 _database_code_depnum_ccdc_archive 'CCDC 679268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium phosphonate' _chemical_melting_point 513.15 _chemical_formula_moiety 'C82 H66 Cd2 N4 O14 P4' _chemical_formula_sum 'C82 H66 Cd2 N4 O14 P4' _chemical_formula_weight 1680.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c _symmetry_space_group_name_HALL '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.028(5) _cell_length_b 29.160(5) _cell_length_c 12.245(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 99.332(5) _cell_angle_gamma 90.000(5) _cell_volume 4238(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5377 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.90 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8831 _exptl_absorpt_correction_T_max 0.9390 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22173 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7454 _reflns_number_gt 6308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0670P)^2^+16.5673P] 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 7454 _refine_ls_number_parameters 520 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1523 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _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 0.46441(3) 1.011113(13) 0.16496(3) 0.02817(14) Uani 1 1 d . . . P1 P 0.31674(12) 0.96109(5) -0.05945(11) 0.0321(3) Uani 1 1 d . . . P2 P 0.59649(14) 0.90714(5) 0.17413(13) 0.0381(4) Uani 1 1 d . . . C1 C 0.2276(5) 0.9105(2) -0.0615(4) 0.0384(13) Uani 1 1 d U A . C2 C 0.1472(5) 0.9060(2) 0.0111(5) 0.0480(16) Uani 1 1 d U . . C3 C 0.0911(6) 0.8645(3) 0.0140(6) 0.076(2) Uani 1 1 d U A . H3 H 0.0407 0.8613 0.0637 0.091 Uiso 1 1 calc R . . C4 C 0.1063(8) 0.8280(3) -0.0529(6) 0.089(3) Uani 1 1 d U . . C5 C 0.1781(8) 0.8342(3) -0.1295(6) 0.080(3) Uani 1 1 d U A . H5 H 0.1859 0.8106 -0.1787 0.096 Uiso 1 1 calc R . . C6 C 0.2389(6) 0.8744(2) -0.1355(5) 0.0532(18) Uani 1 1 d U . . C7 C 0.1161(5) 0.9447(3) 0.0843(5) 0.0517(17) Uani 1 1 d . . . H7 H 0.1430 0.9733 0.0558 0.062 Uiso 1 1 calc R . . C8 C 0.1747(6) 0.9396(3) 0.2026(6) 0.072(2) Uani 1 1 d . . . H8A H 0.1485 0.9123 0.2340 0.108 Uiso 1 1 calc R . . H8B H 0.1582 0.9657 0.2448 0.108 Uiso 1 1 calc R . . H8C H 0.2546 0.9375 0.2040 0.108 Uiso 1 1 calc R . . C9 C -0.0119(5) 0.9492(3) 0.0779(7) 0.082(3) Uani 1 1 d . . . H9A H -0.0465 0.9530 0.0021 0.123 Uiso 1 1 calc R . . H9B H -0.0283 0.9754 0.1201 0.123 Uiso 1 1 calc R . . H9C H -0.0409 0.9221 0.1075 0.123 Uiso 1 1 calc R . . C10A C 0.0158(16) 0.7912(7) -0.0552(14) 0.084(5) Uani 0.60 1 d P A 1 C11A C 0.0805(17) 0.7540(7) 0.019(2) 0.085(6) Uani 0.60 1 d P A 1 C12A C -0.0411(12) 0.7763(5) -0.1610(12) 0.076(4) Uiso 0.60 1 d P A 1 C10B C 0.0726(17) 0.7727(7) -0.030(3) 0.052(6) Uani 0.40 1 d P A 2 C11B C 0.063(3) 0.7637(7) 0.090(2) 0.096(11) Uani 0.40 1 d P A 2 C12B C 0.135(2) 0.7377(9) -0.057(2) 0.083(6) Uiso 0.40 1 d P A 2 C13 C 0.3093(7) 0.8771(2) -0.2277(5) 0.063(2) Uani 1 1 d . A . H13 H 0.3399 0.9083 -0.2272 0.075 Uiso 1 1 calc R . . C14 C 0.4079(9) 0.8445(3) -0.2087(7) 0.085(3) Uani 1 1 d . . . H14A H 0.4512 0.8499 -0.1369 0.128 Uiso 1 1 calc R A . H14B H 0.4545 0.8493 -0.2643 0.128 Uiso 1 1 calc R . . H14C H 0.3807 0.8135 -0.2129 0.128 Uiso 1 1 calc R . . C15 C 0.2356(10) 0.8695(3) -0.3425(6) 0.102(4) Uani 1 1 d . . . H15A H 0.2791 0.8762 -0.3997 0.153 Uiso 1 1 calc R A . H15B H 0.1713 0.8895 -0.3500 0.153 Uiso 1 1 calc R . . H15C H 0.2108 0.8382 -0.3487 0.153 Uiso 1 1 calc R . . C16 C 0.6248(7) 0.8601(2) 0.2730(5) 0.0537(17) Uani 1 1 d U B . C17 C 0.7352(9) 0.8515(3) 0.3319(6) 0.080(2) Uani 1 1 d U B . C18 C 0.7459(11) 0.8154(3) 0.4077(6) 0.105(3) Uani 1 1 d U B . H18 H 0.8181 0.8091 0.4449 0.126 Uiso 1 1 calc R . . C19 C 0.6628(15) 0.7890(4) 0.4320(8) 0.128(4) Uani 1 1 d U . . C20 C 0.5553(11) 0.7982(3) 0.3736(8) 0.104(3) Uani 1 1 d U B . H20 H 0.4957 0.7801 0.3881 0.125 Uiso 1 1 calc R . . C21 C 0.5319(9) 0.8334(2) 0.2938(6) 0.070(2) Uani 1 1 d U . . C25A C 0.6382(16) 0.7409(6) 0.4964(11) 0.066(4) Uani 0.50 1 d P B 1 C25B C 0.7201(13) 0.7577(6) 0.5321(13) 0.062(4) Uani 0.50 1 d P B 2 C26 C 0.6933(9) 0.7055(3) 0.4644(9) 0.098(3) Uani 1 1 d . . . C27A C 0.675(3) 0.7536(8) 0.626(3) 0.068(7) Uani 0.50 1 d P B 1 C27B C 0.655(3) 0.7729(11) 0.625(3) 0.091(11) Uani 0.50 1 d P B 2 C28 C 0.4121(8) 0.8381(2) 0.2344(8) 0.076(3) Uani 1 1 d . B . H28 H 0.4037 0.8692 0.2035 0.092 Uiso 1 1 calc R . . C29 C 0.3223(10) 0.8319(3) 0.3099(10) 0.118(5) Uani 1 1 d . . . H29A H 0.3169 0.8000 0.3281 0.178 Uiso 1 1 calc R B . H29B H 0.2507 0.8424 0.2720 0.178 Uiso 1 1 calc R . . H29C H 0.3433 0.8493 0.3765 0.178 Uiso 1 1 calc R . . C30 C 0.3879(8) 0.8045(2) 0.1383(8) 0.081(3) Uani 1 1 d . . . H30A H 0.4435 0.8081 0.0908 0.122 Uiso 1 1 calc R B . H30B H 0.3145 0.8105 0.0970 0.122 Uiso 1 1 calc R . . H30C H 0.3905 0.7737 0.1664 0.122 Uiso 1 1 calc R . . N1 N 0.3410(5) 1.0633(2) 0.2213(4) 0.0526(14) Uani 1 1 d U . . N2 N 0.5331(5) 1.03599(17) 0.3435(4) 0.0453(12) Uani 1 1 d U . . O1 O 0.3197(3) 0.98853(14) 0.0452(3) 0.0421(10) Uani 1 1 d . . . O2 O 0.4358(3) 0.94505(12) -0.0709(3) 0.0341(9) Uani 1 1 d . . . O3 O 0.2668(3) 0.98947(13) -0.1625(3) 0.0413(9) Uani 1 1 d . . . O4 O 0.5227(3) 0.94177(12) 0.2188(3) 0.0397(10) Uani 1 1 d . . . O5 O 0.5332(4) 0.88358(13) 0.0666(3) 0.0441(10) Uani 1 1 d . . . O6 O 0.7040(4) 0.92781(14) 0.1469(4) 0.0490(11) Uani 1 1 d . . . C1SA C 0.0983(11) 0.9737(8) 0.6796(11) 0.071(6) Uani 0.50 1 d P . . O1SA O 0.0215(17) 0.9499(10) 0.7124(15) 0.199(12) Uani 0.50 1 d P . . C2SB C 0.022(3) 0.9889(13) 0.587(2) 0.192(18) Uani 0.50 1 d P . 2 O1SB O -0.0857(13) 1.0052(7) 0.5385(12) 0.155(8) Uani 0.50 1 d P . 2 C36 C 0.4678(6) 1.0628(2) 0.3936(5) 0.0520(15) Uani 1 1 d U . . C40 C 0.6294(7) 1.0214(2) 0.4006(5) 0.0579(17) Uani 1 1 d U . . H40 H 0.6764 1.0035 0.3648 0.069 Uiso 1 1 calc R . . C39 C 0.6634(7) 1.0316(3) 0.5119(5) 0.0649(19) Uani 1 1 d U . . H39 H 0.7313 1.0205 0.5500 0.078 Uiso 1 1 calc R . . C37 C 0.4963(7) 1.0741(3) 0.5048(6) 0.074(2) Uani 1 1 d U . . H37 H 0.4489 1.0924 0.5392 0.088 Uiso 1 1 calc R . . C31 C 0.2514(7) 1.0774(3) 0.1540(7) 0.076(2) Uani 1 1 d U . . H31 H 0.2373 1.0654 0.0827 0.091 Uiso 1 1 calc R . . C35 C 0.3644(7) 1.0785(3) 0.3248(6) 0.071(2) Uani 1 1 d U . . C32 C 0.1774(11) 1.1089(4) 0.1844(11) 0.118(4) Uiso 1 1 d U . . H32 H 0.1154 1.1196 0.1357 0.142 Uiso 1 1 calc R . . C34 C 0.2984(11) 1.1107(5) 0.3645(12) 0.130(4) Uiso 1 1 d U . . H34 H 0.3184 1.1228 0.4352 0.156 Uiso 1 1 calc R . . C33 C 0.2033(14) 1.1244(6) 0.2978(14) 0.159(5) Uiso 1 1 d U . . H33 H 0.1539 1.1442 0.3254 0.191 Uiso 1 1 calc R . . C38 C 0.5953(7) 1.0579(3) 0.5632(5) 0.074(2) Uani 1 1 d U . . H38 H 0.6156 1.0651 0.6378 0.088 Uiso 1 1 calc R . . C22 C 0.8419(9) 0.8768(4) 0.3132(11) 0.110(4) Uani 1 1 d . . . C23A C 0.9468(16) 0.8473(6) 0.2859(16) 0.096(5) Uiso 0.60 1 d P C 1 C24A C 0.9094(16) 0.8794(7) 0.4410(17) 0.110(6) Uiso 0.60 1 d P C 1 C23B C 0.888(2) 0.8404(9) 0.244(2) 0.082(6) Uiso 0.40 1 d P C 2 C24B C 0.889(3) 0.9156(11) 0.376(3) 0.113(9) Uiso 0.40 1 d P C 2 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 0.0363(2) 0.0322(2) 0.0180(2) -0.00812(15) 0.01048(15) -0.01222(16) P1 0.0373(8) 0.0330(8) 0.0283(7) -0.0125(6) 0.0124(6) -0.0137(6) P2 0.0564(10) 0.0235(7) 0.0407(8) -0.0068(6) 0.0268(7) -0.0009(6) C1 0.046(3) 0.045(3) 0.024(3) -0.007(2) 0.006(2) -0.023(3) C2 0.031(3) 0.078(4) 0.034(3) -0.001(3) 0.002(2) -0.026(3) C3 0.069(5) 0.108(6) 0.054(4) -0.009(4) 0.020(4) -0.062(5) C4 0.112(7) 0.103(6) 0.051(4) -0.015(4) 0.016(4) -0.086(6) C5 0.130(7) 0.067(5) 0.046(4) -0.019(4) 0.021(4) -0.069(5) C6 0.082(5) 0.051(4) 0.028(3) -0.009(3) 0.013(3) -0.038(3) C7 0.020(3) 0.095(5) 0.041(3) -0.005(3) 0.007(2) -0.008(3) C8 0.051(4) 0.122(7) 0.044(4) -0.017(4) 0.011(3) 0.030(4) C9 0.026(3) 0.129(8) 0.093(6) 0.038(6) 0.014(4) -0.002(4) C10A 0.087(12) 0.080(12) 0.075(10) 0.027(9) -0.014(9) -0.050(10) C11A 0.089(12) 0.037(11) 0.12(2) 0.004(11) -0.016(12) -0.014(9) C10B 0.040(11) 0.011(10) 0.10(2) 0.004(10) -0.019(11) -0.014(8) C11B 0.21(3) 0.025(11) 0.066(15) -0.003(10) 0.051(18) -0.038(14) C13 0.126(7) 0.036(4) 0.034(3) -0.020(3) 0.035(4) -0.035(4) C14 0.169(9) 0.042(4) 0.061(5) -0.014(4) 0.068(6) -0.013(5) C15 0.198(11) 0.079(6) 0.030(4) -0.021(4) 0.022(5) -0.070(7) C16 0.101(5) 0.024(3) 0.043(3) -0.003(3) 0.036(3) 0.013(3) C17 0.135(6) 0.050(4) 0.053(4) -0.011(3) 0.011(4) 0.047(4) C18 0.194(9) 0.093(6) 0.034(4) 0.000(4) 0.036(5) 0.086(6) C19 0.268(12) 0.087(7) 0.050(5) 0.028(5) 0.088(6) 0.084(7) C20 0.213(9) 0.045(4) 0.082(6) 0.014(4) 0.108(6) 0.026(6) C21 0.142(6) 0.024(3) 0.062(4) -0.003(3) 0.071(4) 0.010(4) C25A 0.100(13) 0.072(11) 0.030(7) 0.014(7) 0.024(8) -0.004(10) C25B 0.056(9) 0.072(10) 0.058(9) 0.027(8) 0.009(7) -0.021(8) C26 0.105(7) 0.050(5) 0.130(9) 0.043(6) -0.002(6) -0.021(5) C27A 0.100(19) 0.053(13) 0.045(12) 0.018(11) -0.003(11) -0.009(13) C27B 0.101(18) 0.12(3) 0.052(13) 0.06(2) 0.023(11) 0.01(2) C28 0.109(7) 0.029(4) 0.112(7) -0.004(4) 0.082(6) -0.001(4) C29 0.163(10) 0.044(5) 0.187(11) -0.007(6) 0.143(9) -0.020(5) C30 0.097(6) 0.035(4) 0.128(8) -0.017(4) 0.063(6) -0.017(4) N1 0.056(3) 0.057(3) 0.047(3) -0.030(3) 0.013(2) -0.010(3) N2 0.087(4) 0.031(3) 0.020(2) -0.005(2) 0.016(2) -0.013(2) O1 0.029(2) 0.058(3) 0.042(2) -0.030(2) 0.0124(17) -0.0188(18) O2 0.046(2) 0.0278(19) 0.034(2) -0.0064(16) 0.0214(17) -0.0125(16) O3 0.050(2) 0.037(2) 0.038(2) -0.0102(18) 0.0104(18) -0.0082(18) O4 0.058(3) 0.026(2) 0.043(2) -0.0084(17) 0.030(2) -0.0026(17) O5 0.064(3) 0.027(2) 0.048(2) -0.0157(18) 0.027(2) -0.0059(19) O6 0.052(3) 0.032(2) 0.070(3) -0.010(2) 0.032(2) 0.0001(19) C1SA 0.025(7) 0.161(18) 0.026(7) -0.016(8) -0.001(5) -0.025(8) O1SA 0.144(17) 0.33(3) 0.096(13) -0.113(17) -0.054(12) 0.062(19) C2SB 0.16(2) 0.28(4) 0.11(2) -0.08(2) -0.064(18) 0.16(3) O1SB 0.108(11) 0.28(2) 0.066(9) -0.020(11) -0.007(8) 0.124(13) C36 0.081(4) 0.049(4) 0.032(3) -0.019(3) 0.027(3) -0.028(3) C40 0.096(5) 0.052(4) 0.024(3) -0.005(3) 0.005(3) -0.013(3) C39 0.097(5) 0.069(5) 0.025(3) -0.001(3) 0.000(3) -0.035(4) C37 0.085(5) 0.102(6) 0.040(4) -0.047(4) 0.032(3) -0.051(4) C31 0.078(5) 0.069(5) 0.079(5) -0.048(4) 0.007(4) 0.020(4) C35 0.092(5) 0.069(5) 0.055(4) -0.042(4) 0.021(3) 0.002(4) C38 0.089(5) 0.111(6) 0.026(3) -0.028(4) 0.024(3) -0.071(4) C22 0.082(7) 0.085(7) 0.157(11) -0.002(7) -0.001(7) 0.026(6) _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 O1 2.187(4) . ? Cd1 O2 2.202(3) 3_675 ? Cd1 O4 2.206(4) . ? Cd1 N1 2.308(5) . ? Cd1 N2 2.324(5) . ? P1 O1 1.506(4) . ? P1 O2 1.534(4) . ? P1 O3 1.547(4) . ? P1 C1 1.821(5) . ? P2 O4 1.505(4) . ? P2 O6 1.512(4) . ? P2 O5 1.568(4) . ? P2 C16 1.824(6) . ? C1 C6 1.411(8) . ? C1 C2 1.421(8) . ? C2 C3 1.388(9) . ? C2 C7 1.524(10) . ? C3 C4 1.375(12) . ? C3 H3 0.9300 . ? C4 C5 1.386(11) . ? C4 C10A 1.525(15) . ? C4 C10B 1.70(2) . ? C5 C6 1.390(9) . ? C5 H5 0.9300 . ? C6 C13 1.519(9) . ? C7 C8 1.512(9) . ? C7 C9 1.534(8) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10A C12A 1.43(2) . ? C10A C11A 1.54(2) . ? C10B C12B 1.34(3) . ? C10B C11B 1.52(4) . ? C13 C14 1.510(12) . ? C13 C15 1.551(10) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C21 1.420(11) . ? C16 C17 1.427(12) . ? C17 C18 1.396(12) . ? C17 C22 1.530(15) . ? C18 C19 1.333(18) . ? C18 H18 0.9300 . ? C19 C20 1.399(18) . ? C19 C25B 1.592(18) . ? C19 C25A 1.659(19) . ? C20 C21 1.413(11) . ? C20 H20 0.9300 . ? C21 C28 1.511(13) . ? C25A C26 1.318(18) . ? C25A C27A 1.62(4) . ? C25B C27B 1.55(4) . ? C25B C26 1.74(2) . ? C28 C30 1.524(11) . ? C28 C29 1.542(10) . ? C28 H28 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 C31 1.312(10) . ? N1 C35 1.329(8) . ? N2 C40 1.323(9) . ? N2 C36 1.327(8) . ? O2 Cd1 2.202(3) 3_675 ? C1SA O1SA 1.27(3) . ? C1SA C2SB 1.41(3) . ? O1SA C2SB 1.91(5) . ? C2SB O1SB 1.41(2) . ? C2SB O1SB 1.84(4) 3_576 ? O1SB C2SB 1.84(4) 3_576 ? C36 C37 1.389(9) . ? C36 C35 1.458(11) . ? C40 C39 1.390(9) . ? C40 H40 0.9300 . ? C39 C38 1.349(12) . ? C39 H39 0.9300 . ? C37 C38 1.369(12) . ? C37 H37 0.9300 . ? C31 C32 1.372(13) . ? C31 H31 0.9300 . ? C35 C34 1.368(14) . ? C32 C33 1.446(18) . ? C32 H32 0.9300 . ? C34 C33 1.353(18) . ? C34 H34 0.9300 . ? C33 H33 0.9300 . ? C38 H38 0.9300 . ? C22 C24B 1.43(3) . ? C22 C23B 1.51(3) . ? C22 C23A 1.61(2) . ? C22 C24A 1.64(2) . ? 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 Cd1 O2 105.42(15) . 3_675 ? O1 Cd1 O4 95.99(16) . . ? O2 Cd1 O4 120.98(14) 3_675 . ? O1 Cd1 N1 85.34(17) . . ? O2 Cd1 N1 101.84(18) 3_675 . ? O4 Cd1 N1 134.72(18) . . ? O1 Cd1 N2 147.93(17) . . ? O2 Cd1 N2 99.78(15) 3_675 . ? O4 Cd1 N2 87.57(16) . . ? N1 Cd1 N2 70.2(2) . . ? O1 P1 O2 110.2(2) . . ? O1 P1 O3 111.2(2) . . ? O2 P1 O3 109.5(2) . . ? O1 P1 C1 112.0(2) . . ? O2 P1 C1 108.0(2) . . ? O3 P1 C1 105.8(2) . . ? O4 P2 O6 112.9(2) . . ? O4 P2 O5 111.4(2) . . ? O6 P2 O5 107.8(2) . . ? O4 P2 C16 108.7(2) . . ? O6 P2 C16 111.8(3) . . ? O5 P2 C16 103.9(3) . . ? C6 C1 C2 118.6(5) . . ? C6 C1 P1 119.7(4) . . ? C2 C1 P1 121.7(4) . . ? C3 C2 C1 118.7(6) . . ? C3 C2 C7 117.6(6) . . ? C1 C2 C7 123.7(6) . . ? C4 C3 C2 123.2(7) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C3 C4 C5 117.4(7) . . ? C3 C4 C10A 113.0(11) . . ? C5 C4 C10A 127.0(10) . . ? C3 C4 C10B 125.2(11) . . ? C5 C4 C10B 115.5(12) . . ? C10A C4 C10B 31.4(8) . . ? C4 C5 C6 122.5(7) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 119.3(6) . . ? C5 C6 C13 116.4(6) . . ? C1 C6 C13 124.2(5) . . ? C8 C7 C2 111.7(6) . . ? C8 C7 C9 111.4(6) . . ? C2 C7 C9 111.9(6) . . ? C8 C7 H7 107.2 . . ? C2 C7 H7 107.2 . . ? C9 C7 H7 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12A C10A C4 117.7(12) . . ? C12A C10A C11A 116.1(18) . . ? C4 C10A C11A 101.1(13) . . ? C12B C10B C11B 104(2) . . ? C12B C10B C4 121(2) . . ? C11B C10B C4 112.7(14) . . ? C14 C13 C6 111.8(6) . . ? C14 C13 C15 111.6(7) . . ? C6 C13 C15 111.1(7) . . ? C14 C13 H13 107.3 . . ? C6 C13 H13 107.3 . . ? C15 C13 H13 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 120.4(7) . . ? C21 C16 P2 117.7(6) . . ? C17 C16 P2 121.8(6) . . ? C18 C17 C16 116.6(10) . . ? C18 C17 C22 118.3(10) . . ? C16 C17 C22 125.0(8) . . ? C19 C18 C17 126.3(12) . . ? C19 C18 H18 116.9 . . ? C17 C18 H18 116.9 . . ? C18 C19 C20 116.1(9) . . ? C18 C19 C25B 104.8(13) . . ? C20 C19 C25B 138.8(13) . . ? C18 C19 C25A 142.4(14) . . ? C20 C19 C25A 100.6(13) . . ? C25B C19 C25A 40.4(7) . . ? C19 C20 C21 123.8(11) . . ? C19 C20 H20 118.1 . . ? C21 C20 H20 118.1 . . ? C20 C21 C16 116.7(10) . . ? C20 C21 C28 117.8(9) . . ? C16 C21 C28 125.4(7) . . ? C26 C25A C27A 113.4(16) . . ? C26 C25A C19 112.5(11) . . ? C27A C25A C19 103.3(15) . . ? C27B C25B C19 101.4(14) . . ? C27B C25B C26 121.8(17) . . ? C19 C25B C26 96.3(10) . . ? C25A C26 C25B 40.3(9) . . ? C21 C28 C30 111.2(6) . . ? C21 C28 C29 114.0(8) . . ? C30 C28 C29 108.8(7) . . ? C21 C28 H28 107.5 . . ? C30 C28 H28 107.5 . . ? C29 C28 H28 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 N1 C35 121.3(6) . . ? C31 N1 Cd1 121.4(4) . . ? C35 N1 Cd1 117.3(5) . . ? C40 N2 C36 118.6(6) . . ? C40 N2 Cd1 123.0(4) . . ? C36 N2 Cd1 118.2(5) . . ? P1 O1 Cd1 129.6(2) . . ? P1 O2 Cd1 117.8(2) . 3_675 ? P2 O4 Cd1 133.2(2) . . ? O1SA C1SA C2SB 91(2) . . ? C1SA O1SA C2SB 47.6(16) . . ? C1SA C2SB O1SB 151(3) . . ? C1SA C2SB O1SB 113.2(19) . 3_576 ? O1SB C2SB O1SB 95.4(18) . 3_576 ? C1SA C2SB O1SA 41.7(13) . . ? O1SB C2SB O1SA 115(3) . . ? O1SB C2SB O1SA 141.6(16) 3_576 . ? C2SB O1SB C2SB 84.6(18) . 3_576 ? N2 C36 C37 121.5(8) . . ? N2 C36 C35 115.6(5) . . ? C37 C36 C35 123.0(7) . . ? N2 C40 C39 122.8(8) . . ? N2 C40 H40 118.6 . . ? C39 C40 H40 118.6 . . ? C38 C39 C40 118.3(8) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? C38 C37 C36 119.1(7) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? N1 C31 C32 122.9(8) . . ? N1 C31 H31 118.6 . . ? C32 C31 H31 118.6 . . ? N1 C35 C34 121.5(10) . . ? N1 C35 C36 118.3(6) . . ? C34 C35 C36 120.0(8) . . ? C31 C32 C33 114.9(13) . . ? C31 C32 H32 122.5 . . ? C33 C32 H32 122.5 . . ? C33 C34 C35 118.1(14) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C34 C33 C32 121.1(16) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C39 C38 C37 119.7(6) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C24B C22 C23B 134.9(18) . . ? C24B C22 C17 124.7(16) . . ? C23B C22 C17 97.7(12) . . ? C24B C22 C23A 106.2(16) . . ? C23B C22 C23A 30.7(10) . . ? C17 C22 C23A 118.7(10) . . ? C24B C22 C24A 50.2(14) . . ? C23B C22 C24A 113.3(13) . . ? C17 C22 C24A 100.2(11) . . ? C23A C22 C24A 86.6(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.218 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.107 #===END data_Cd1 _database_code_depnum_ccdc_archive 'CCDC 679269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium phosphonate' _chemical_melting_point 445.15 _chemical_formula_moiety 'C50 H80 Cd N8 O6 P2' _chemical_formula_sum 'C50 H80 Cd N8 O6 P2' _chemical_formula_weight 1063.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.736(5) _cell_length_b 11.309(5) _cell_length_c 12.698(5) _cell_angle_alpha 65.732(5) _cell_angle_beta 75.580(5) _cell_angle_gamma 84.573(5) _cell_volume 1361.1(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2788 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.77 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 562 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9044 _exptl_absorpt_correction_T_max 0.9505 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9134 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6461 _reflns_number_gt 5766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0831P)^2^+0.0000P] 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 6461 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1353 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.2005(3) 0.5993(3) -0.2556(3) 0.0149(6) Uani 1 1 d . . . C2 C 0.1599(3) 0.7255(3) -0.3223(3) 0.0167(6) Uani 1 1 d . . . C3 C 0.1583(3) 0.7591(3) -0.4402(3) 0.0180(6) Uani 1 1 d . . . H3 H 0.1277 0.8424 -0.4833 0.022 Uiso 1 1 calc R . . C4 C 0.1995(3) 0.6763(3) -0.4982(3) 0.0173(6) Uani 1 1 d . . . C5 C 0.2460(3) 0.5562(3) -0.4336(3) 0.0181(6) Uani 1 1 d . . . H5 H 0.2768 0.4990 -0.4720 0.022 Uiso 1 1 calc R . . C6 C 0.2494(3) 0.5162(3) -0.3154(3) 0.0156(6) Uani 1 1 d . . . C7 C 0.1210(3) 0.8303(3) -0.2733(3) 0.0228(7) Uani 1 1 d . . . H7 H 0.1385 0.7955 -0.1922 0.027 Uiso 1 1 calc R . . C8 C 0.2011(5) 0.9529(4) -0.3479(5) 0.0562(14) Uani 1 1 d . . . H8A H 0.2926 0.9315 -0.3550 0.084 Uiso 1 1 calc R . . H8B H 0.1795 1.0144 -0.3098 0.084 Uiso 1 1 calc R . . H8C H 0.1829 0.9921 -0.4271 0.084 Uiso 1 1 calc R . . C9 C -0.0208(4) 0.8609(4) -0.2601(4) 0.0479(11) Uani 1 1 d . . . H9A H -0.0412 0.9278 -0.2282 0.072 Uiso 1 1 calc R . . H9B H -0.0711 0.7822 -0.2056 0.072 Uiso 1 1 calc R . . H9C H -0.0419 0.8924 -0.3378 0.072 Uiso 1 1 calc R . . C10 C 0.1961(3) 0.7149(3) -0.6269(3) 0.0212(6) Uani 1 1 d . . . H10 H 0.2430 0.6474 -0.6531 0.025 Uiso 1 1 calc R . . C11 C 0.0582(3) 0.7187(4) -0.6395(3) 0.0322(8) Uani 1 1 d . . . H11A H 0.0582 0.7433 -0.7230 0.048 Uiso 1 1 calc R . . H11B H 0.0094 0.7824 -0.6119 0.048 Uiso 1 1 calc R . . H11C H 0.0183 0.6328 -0.5916 0.048 Uiso 1 1 calc R . . C12 C 0.2625(3) 0.8448(3) -0.7077(3) 0.0266(7) Uani 1 1 d . . . H12A H 0.2585 0.8661 -0.7897 0.040 Uiso 1 1 calc R . . H12B H 0.3526 0.8397 -0.7027 0.040 Uiso 1 1 calc R . . H12C H 0.2192 0.9124 -0.6826 0.040 Uiso 1 1 calc R . . C13 C 0.3107(3) 0.3848(3) -0.2580(3) 0.0180(6) Uani 1 1 d . . . H13 H 0.3099 0.3711 -0.1748 0.022 Uiso 1 1 calc R . . C14 C 0.2345(3) 0.2743(3) -0.2516(3) 0.0260(7) Uani 1 1 d . . . H14A H 0.2764 0.1917 -0.2146 0.039 Uiso 1 1 calc R . . H14B H 0.2311 0.2870 -0.3319 0.039 Uiso 1 1 calc R . . H14C H 0.1469 0.2730 -0.2041 0.039 Uiso 1 1 calc R . . C15 C 0.4512(3) 0.3839(3) -0.3237(3) 0.0239(7) Uani 1 1 d . . . H15A H 0.4887 0.2990 -0.2856 0.036 Uiso 1 1 calc R . . H15B H 0.4998 0.4514 -0.3211 0.036 Uiso 1 1 calc R . . H15C H 0.4550 0.4007 -0.4066 0.036 Uiso 1 1 calc R . . C16 C 0.1541(3) 0.4508(3) 0.2389(3) 0.0264(7) Uani 1 1 d . . . H16A H 0.1762 0.5035 0.1532 0.040 Uiso 1 1 calc R . . H16B H 0.1157 0.5060 0.2809 0.040 Uiso 1 1 calc R . . H16C H 0.0924 0.3829 0.2562 0.040 Uiso 1 1 calc R . . C17 C 0.2730(3) 0.3896(3) 0.2790(3) 0.0185(6) Uani 1 1 d . . . C18 C 0.2833(3) 0.3067(3) 0.3953(3) 0.0206(6) Uani 1 1 d . . . H18 H 0.2154 0.2767 0.4647 0.025 Uiso 1 1 calc R . . C19 C 0.4115(3) 0.2783(3) 0.3876(3) 0.0187(6) Uani 1 1 d . . . C20 C 0.4841(3) 0.1967(3) 0.4796(3) 0.0247(7) Uani 1 1 d . . . H20A H 0.5758 0.1984 0.4419 0.037 Uiso 1 1 calc R . . H20B H 0.4518 0.1072 0.5162 0.037 Uiso 1 1 calc R . . H20C H 0.4720 0.2312 0.5406 0.037 Uiso 1 1 calc R . . C21 C 0.3578(3) 0.1784(3) 0.0836(4) 0.0306(8) Uani 1 1 d . . . H21A H 0.3262 0.2663 0.0706 0.046 Uiso 1 1 calc R . . H21B H 0.3246 0.1201 0.1667 0.046 Uiso 1 1 calc R . . H21C H 0.3282 0.1482 0.0317 0.046 Uiso 1 1 calc R . . C22 C 0.5000(3) 0.1792(3) 0.0560(3) 0.0239(7) Uani 1 1 d . . . C23 C 0.5868(3) 0.0774(3) 0.0608(3) 0.0249(7) Uani 1 1 d . . . H23 H 0.5664 -0.0104 0.0813 0.030 Uiso 1 1 calc R . . C24 C 0.7086(3) 0.1308(3) 0.0296(3) 0.0228(7) Uani 1 1 d . . . C25 C 0.8397(3) 0.0751(3) 0.0174(3) 0.0265(7) Uani 1 1 d . . . H25A H 0.9036 0.1432 -0.0064 0.040 Uiso 1 1 calc R . . H25B H 0.8546 0.0393 -0.0431 0.040 Uiso 1 1 calc R . . H25C H 0.8473 0.0059 0.0936 0.040 Uiso 1 1 calc R . . N1 N 0.3881(2) 0.4105(2) 0.2043(2) 0.0174(5) Uani 1 1 d . . . N2 N 0.4706(2) 0.3408(2) 0.2732(2) 0.0187(5) Uani 1 1 d . . . H2 H 0.5539 0.3373 0.2454 0.022 Uiso 1 1 calc R . . N3 N 0.5628(3) 0.2889(2) 0.0228(2) 0.0224(6) Uani 1 1 d . . . N4 N 0.6913(3) 0.2565(3) 0.0074(2) 0.0229(6) Uani 1 1 d . . . H4 H 0.7544 0.3121 -0.0143 0.028 Uiso 1 1 calc R . . O1 O 0.33026(19) 0.5165(2) -0.08332(19) 0.0202(5) Uani 1 1 d . . . O2 O 0.12844(19) 0.39662(19) -0.04347(19) 0.0186(4) Uani 1 1 d . . . H2A H 0.0520 0.4051 -0.0504 0.028 Uiso 1 1 calc R . . O3 O 0.1137(2) 0.6167(2) -0.03776(19) 0.0189(4) Uani 1 1 d . . . P1 P 0.19361(7) 0.53399(7) -0.09688(7) 0.01521(17) Uani 1 1 d . . . Cd1 Cd 0.5000 0.5000 0.0000 0.01228(10) Uani 1 2 d S . . 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 C1 0.0071(13) 0.0186(14) 0.0156(14) -0.0034(11) -0.0022(10) -0.0016(10) C2 0.0087(13) 0.0194(14) 0.0189(15) -0.0076(12) 0.0018(11) 0.0009(10) C3 0.0146(14) 0.0141(13) 0.0201(15) -0.0020(12) -0.0040(11) 0.0022(11) C4 0.0132(14) 0.0200(14) 0.0154(14) -0.0042(12) -0.0024(11) -0.0004(11) C5 0.0157(14) 0.0195(14) 0.0187(15) -0.0084(12) -0.0023(11) 0.0006(11) C6 0.0099(13) 0.0164(13) 0.0183(14) -0.0054(12) -0.0028(11) 0.0012(10) C7 0.0262(17) 0.0192(15) 0.0212(16) -0.0086(13) -0.0032(13) 0.0050(12) C8 0.055(3) 0.043(2) 0.072(3) -0.043(2) 0.026(2) -0.021(2) C9 0.031(2) 0.050(3) 0.074(3) -0.041(3) -0.010(2) 0.0143(19) C10 0.0172(15) 0.0273(16) 0.0171(15) -0.0077(13) -0.0045(12) 0.0050(12) C11 0.0252(18) 0.043(2) 0.0264(19) -0.0102(16) -0.0090(15) -0.0002(15) C12 0.0247(17) 0.0283(17) 0.0177(16) -0.0026(14) -0.0028(13) 0.0058(13) C13 0.0152(14) 0.0168(14) 0.0187(15) -0.0052(12) -0.0028(11) 0.0029(11) C14 0.0231(17) 0.0176(15) 0.0304(18) -0.0031(14) -0.0052(14) -0.0006(12) C15 0.0165(15) 0.0230(16) 0.0290(18) -0.0101(14) -0.0025(13) 0.0061(12) C16 0.0146(16) 0.0349(18) 0.0236(17) -0.0079(15) -0.0011(13) 0.0004(13) C17 0.0150(14) 0.0208(15) 0.0212(15) -0.0109(12) -0.0010(12) -0.0038(11) C18 0.0169(15) 0.0235(15) 0.0190(15) -0.0088(13) 0.0024(12) -0.0043(12) C19 0.0174(15) 0.0192(15) 0.0183(15) -0.0072(12) -0.0013(12) -0.0041(11) C20 0.0223(17) 0.0254(16) 0.0232(17) -0.0075(14) -0.0039(13) 0.0013(13) C21 0.0240(18) 0.0217(16) 0.043(2) -0.0100(16) -0.0076(15) 0.0007(13) C22 0.0267(18) 0.0211(15) 0.0240(17) -0.0089(13) -0.0050(13) -0.0028(13) C23 0.0228(17) 0.0214(16) 0.0286(18) -0.0083(14) -0.0052(14) -0.0015(12) C24 0.0226(17) 0.0243(16) 0.0237(16) -0.0125(14) -0.0051(13) 0.0032(12) C25 0.0238(17) 0.0254(17) 0.0294(18) -0.0118(15) -0.0044(14) 0.0030(13) N1 0.0133(12) 0.0189(12) 0.0168(13) -0.0055(10) 0.0002(10) -0.0022(9) N2 0.0096(12) 0.0262(14) 0.0165(13) -0.0073(11) 0.0019(9) -0.0005(10) N3 0.0195(14) 0.0198(13) 0.0232(14) -0.0075(11) 0.0013(11) -0.0007(10) N4 0.0160(13) 0.0250(14) 0.0266(15) -0.0103(12) -0.0019(11) -0.0024(10) O1 0.0098(10) 0.0306(12) 0.0173(11) -0.0065(9) -0.0029(8) -0.0008(8) O2 0.0105(10) 0.0197(10) 0.0194(11) -0.0037(9) -0.0001(8) -0.0001(8) O3 0.0119(10) 0.0252(11) 0.0189(11) -0.0095(9) 0.0003(8) -0.0034(8) P1 0.0078(4) 0.0205(4) 0.0149(4) -0.0054(3) -0.0012(3) -0.0006(3) Cd1 0.00824(15) 0.01337(16) 0.01406(16) -0.00476(11) -0.00172(10) -0.00030(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 C1 C2 1.420(4) . ? C1 C6 1.425(4) . ? C1 P1 1.824(3) . ? C2 C3 1.390(4) . ? C2 C7 1.533(4) . ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 C10 1.516(4) . ? C5 C6 1.388(4) . ? C5 H5 0.9500 . ? C6 C13 1.528(4) . ? C7 C9 1.511(5) . ? C7 C8 1.517(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.521(5) . ? C10 C11 1.523(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.521(4) . ? C13 C15 1.533(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.495(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N1 1.330(4) . ? C17 C18 1.414(4) . ? C18 C19 1.372(4) . ? C18 H18 0.9500 . ? C19 N2 1.339(4) . ? C19 C20 1.502(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.480(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.325(4) . ? C22 C23 1.402(5) . ? C23 C24 1.387(5) . ? C23 H23 0.9500 . ? C24 N4 1.334(4) . ? C24 C25 1.486(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? N1 N2 1.363(3) . ? N1 Cd1 2.391(3) . ? N2 H2 0.8800 . ? N3 N4 1.381(4) . ? N3 Cd1 2.337(3) . ? N4 H4 0.8800 . ? O1 P1 1.505(2) . ? O1 Cd1 2.282(2) . ? O2 P1 1.570(2) . ? O2 H2A 0.8400 . ? O3 P1 1.510(2) . ? Cd1 O1 2.282(2) 2_665 ? Cd1 N3 2.337(3) 2_665 ? Cd1 N1 2.391(3) 2_665 ? 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 C2 C1 C6 118.5(3) . . ? C2 C1 P1 124.6(2) . . ? C6 C1 P1 116.9(2) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C7 117.1(3) . . ? C1 C2 C7 123.9(3) . . ? C2 C3 C4 123.1(3) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C5 C4 C3 117.1(3) . . ? C5 C4 C10 120.8(3) . . ? C3 C4 C10 122.1(3) . . ? C6 C5 C4 122.7(3) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C1 119.4(3) . . ? C5 C6 C13 116.8(3) . . ? C1 C6 C13 123.8(3) . . ? C9 C7 C8 110.5(3) . . ? C9 C7 C2 112.4(3) . . ? C8 C7 C2 111.7(3) . . ? C9 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C2 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 C12 112.0(3) . . ? C4 C10 C11 110.8(3) . . ? C12 C10 C11 110.1(3) . . ? C4 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C6 111.6(2) . . ? C14 C13 C15 111.0(3) . . ? C6 C13 C15 110.8(3) . . ? C14 C13 H13 107.8 . . ? C6 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 110.4(3) . . ? N1 C17 C16 122.0(3) . . ? C18 C17 C16 127.6(3) . . ? C19 C18 C17 105.8(3) . . ? C19 C18 H18 127.1 . . ? C17 C18 H18 127.1 . . ? N2 C19 C18 106.2(3) . . ? N2 C19 C20 122.0(3) . . ? C18 C19 C20 131.8(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 110.4(3) . . ? N3 C22 C21 119.6(3) . . ? C23 C22 C21 130.0(3) . . ? C24 C23 C22 106.1(3) . . ? C24 C23 H23 126.9 . . ? C22 C23 H23 126.9 . . ? N4 C24 C23 106.3(3) . . ? N4 C24 C25 121.0(3) . . ? C23 C24 C25 132.7(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 N1 N2 104.7(2) . . ? C17 N1 Cd1 144.8(2) . . ? N2 N1 Cd1 109.98(17) . . ? C19 N2 N1 112.9(2) . . ? C19 N2 H2 123.5 . . ? N1 N2 H2 123.5 . . ? C22 N3 N4 105.3(3) . . ? C22 N3 Cd1 134.3(2) . . ? N4 N3 Cd1 120.30(19) . . ? C24 N4 N3 111.9(3) . . ? C24 N4 H4 124.0 . . ? N3 N4 H4 124.0 . . ? P1 O1 Cd1 158.65(14) . . ? P1 O2 H2A 109.5 . . ? O1 P1 O3 114.04(13) . . ? O1 P1 O2 108.57(12) . . ? O3 P1 O2 109.05(12) . . ? O1 P1 C1 106.95(13) . . ? O3 P1 C1 112.24(13) . . ? O2 P1 C1 105.59(12) . . ? O1 Cd1 O1 180.00(9) . 2_665 ? O1 Cd1 N3 81.31(9) . 2_665 ? O1 Cd1 N3 98.69(9) 2_665 2_665 ? O1 Cd1 N3 98.69(9) . . ? O1 Cd1 N3 81.31(9) 2_665 . ? N3 Cd1 N3 180.000(1) 2_665 . ? O1 Cd1 N1 81.44(8) . 2_665 ? O1 Cd1 N1 98.56(8) 2_665 2_665 ? N3 Cd1 N1 87.47(9) 2_665 2_665 ? N3 Cd1 N1 92.53(9) . 2_665 ? O1 Cd1 N1 98.56(8) . . ? O1 Cd1 N1 81.44(8) 2_665 . ? N3 Cd1 N1 92.53(9) 2_665 . ? N3 Cd1 N1 87.47(9) . . ? N1 Cd1 N1 180.000(1) 2_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 5.8(4) . . . . ? P1 C1 C2 C3 -173.7(2) . . . . ? C6 C1 C2 C7 -172.3(3) . . . . ? P1 C1 C2 C7 8.3(4) . . . . ? C1 C2 C3 C4 -2.5(4) . . . . ? C7 C2 C3 C4 175.6(3) . . . . ? C2 C3 C4 C5 -1.2(5) . . . . ? C2 C3 C4 C10 179.7(3) . . . . ? C3 C4 C5 C6 1.7(5) . . . . ? C10 C4 C5 C6 -179.2(3) . . . . ? C4 C5 C6 C1 1.6(4) . . . . ? C4 C5 C6 C13 -176.4(3) . . . . ? C2 C1 C6 C5 -5.4(4) . . . . ? P1 C1 C6 C5 174.1(2) . . . . ? C2 C1 C6 C13 172.6(3) . . . . ? P1 C1 C6 C13 -7.9(4) . . . . ? C3 C2 C7 C9 69.8(4) . . . . ? C1 C2 C7 C9 -112.1(4) . . . . ? C3 C2 C7 C8 -55.1(4) . . . . ? C1 C2 C7 C8 123.0(4) . . . . ? C5 C4 C10 C12 -127.0(3) . . . . ? C3 C4 C10 C12 52.1(4) . . . . ? C5 C4 C10 C11 109.7(3) . . . . ? C3 C4 C10 C11 -71.2(4) . . . . ? C5 C6 C13 C14 -64.5(4) . . . . ? C1 C6 C13 C14 117.5(3) . . . . ? C5 C6 C13 C15 59.8(3) . . . . ? C1 C6 C13 C15 -118.2(3) . . . . ? N1 C17 C18 C19 0.1(3) . . . . ? C16 C17 C18 C19 -178.8(3) . . . . ? C17 C18 C19 N2 -0.4(3) . . . . ? C17 C18 C19 C20 179.5(3) . . . . ? N3 C22 C23 C24 0.7(4) . . . . ? C21 C22 C23 C24 -178.1(3) . . . . ? C22 C23 C24 N4 -0.4(4) . . . . ? C22 C23 C24 C25 -179.7(4) . . . . ? C18 C17 N1 N2 0.2(3) . . . . ? C16 C17 N1 N2 179.2(3) . . . . ? C18 C17 N1 Cd1 170.1(2) . . . . ? C16 C17 N1 Cd1 -10.9(5) . . . . ? C18 C19 N2 N1 0.6(3) . . . . ? C20 C19 N2 N1 -179.4(3) . . . . ? C17 N1 N2 C19 -0.5(3) . . . . ? Cd1 N1 N2 C19 -174.30(19) . . . . ? C23 C22 N3 N4 -0.7(4) . . . . ? C21 C22 N3 N4 178.3(3) . . . . ? C23 C22 N3 Cd1 -176.5(2) . . . . ? C21 C22 N3 Cd1 2.5(5) . . . . ? C23 C24 N4 N3 0.0(4) . . . . ? C25 C24 N4 N3 179.4(3) . . . . ? C22 N3 N4 C24 0.4(4) . . . . ? Cd1 N3 N4 C24 177.0(2) . . . . ? Cd1 O1 P1 O3 28.8(4) . . . . ? Cd1 O1 P1 O2 -93.0(4) . . . . ? Cd1 O1 P1 C1 153.5(4) . . . . ? C2 C1 P1 O1 -113.3(3) . . . . ? C6 C1 P1 O1 67.2(2) . . . . ? C2 C1 P1 O3 12.5(3) . . . . ? C6 C1 P1 O3 -167.0(2) . . . . ? C2 C1 P1 O2 131.2(2) . . . . ? C6 C1 P1 O2 -48.3(2) . . . . ? P1 O1 Cd1 O1 -21(100) . . . 2_665 ? P1 O1 Cd1 N3 -61.0(4) . . . 2_665 ? P1 O1 Cd1 N3 119.0(4) . . . . ? P1 O1 Cd1 N1 -149.7(4) . . . 2_665 ? P1 O1 Cd1 N1 30.3(4) . . . . ? C22 N3 Cd1 O1 -40.5(3) . . . . ? N4 N3 Cd1 O1 144.2(2) . . . . ? C22 N3 Cd1 O1 139.5(3) . . . 2_665 ? N4 N3 Cd1 O1 -35.8(2) . . . 2_665 ? C22 N3 Cd1 N3 79(100) . . . 2_665 ? N4 N3 Cd1 N3 -96(100) . . . 2_665 ? C22 N3 Cd1 N1 -122.2(3) . . . 2_665 ? N4 N3 Cd1 N1 62.5(2) . . . 2_665 ? C22 N3 Cd1 N1 57.8(3) . . . . ? N4 N3 Cd1 N1 -117.5(2) . . . . ? C17 N1 Cd1 O1 -15.7(4) . . . . ? N2 N1 Cd1 O1 153.95(18) . . . . ? C17 N1 Cd1 O1 164.3(4) . . . 2_665 ? N2 N1 Cd1 O1 -26.05(18) . . . 2_665 ? C17 N1 Cd1 N3 65.9(4) . . . 2_665 ? N2 N1 Cd1 N3 -124.47(19) . . . 2_665 ? C17 N1 Cd1 N3 -114.1(4) . . . . ? N2 N1 Cd1 N3 55.53(19) . . . . ? C17 N1 Cd1 N1 127(100) . . . 2_665 ? N2 N1 Cd1 N1 -64(100) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.185 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.117 ##===END