# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 La N6 O10 P2' _chemical_formula_weight 1126.80 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' La La -0.2871 2.4523 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 13.2741(4) _cell_length_b 17.9504(8) _cell_length_c 21.7777(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.307(3) _cell_angle_gamma 90.00 _cell_volume 5157.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 174882 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and five \w scans with 2\% steps (469 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 174882 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_unetI/netI 0.0589 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9781 _reflns_number_gt 7431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Two nitrite ions (containing N1 and N5) are badly resolved; one of them (N5) was found to be disordered over two positions sharing one O atom, which were refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths, angles and displacement parameters for several nitrite ions: DFIX 1.24 0.005 N1 O1 DFIX 1.24 0.005 N1 O2 DFIX 2.05 0.005 O1 O2 DFIX 1.24 0.01 N5A O9A DFIX 1.24 0.01 N5A O10 DFIX 2.05 0.01 O9A O10 DFIX 1.24 0.01 N5B O9B DFIX 1.24 0.01 N5B O10 DFIX 2.05 0.01 O9B O10 ISOR 0.005 N1 O3 O4 O7 O8 N5A SIMU .005 .005 3. N1 O1 O2 SIMU .001 .001 3. N2 O3 O4 SIMU .005 .005 3. N3 O5 O6 SIMU .005 .005 3. N4 O7 O8 SIMU .005 .005 3. N5A N5B O9A O9B O10 The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0878P)^2^+10.8933P] 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 9781 _refine_ls_number_parameters 668 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.762 _refine_diff_density_min -2.052 _refine_diff_density_rms 0.143 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 La La 0.78848(2) 0.365306(18) 0.236028(14) 0.02761(13) Uani 1 1 d . . . P1 P 0.64379(11) 0.89772(9) 0.10617(7) 0.0325(3) Uani 1 1 d . . . P2 P 0.24098(10) 0.37171(8) 0.04974(6) 0.0267(3) Uani 1 1 d . . . O1 O 0.6940(7) 0.4336(4) 0.3153(3) 0.1139(19) Uani 1 1 d DU . . O2 O 0.7308(6) 0.5056(4) 0.2485(3) 0.0994(18) Uani 1 1 d DU . . O3 O 0.8238(6) 0.4272(5) 0.1336(4) 0.1123(15) Uani 1 1 d U . . O4 O 0.9463(5) 0.4025(5) 0.1830(4) 0.1135(15) Uani 1 1 d U . . O5 O 0.6085(3) 0.3887(2) 0.1705(2) 0.0437(10) Uani 1 1 d U . . O6 O 0.6852(4) 0.2944(3) 0.1442(2) 0.0674(13) Uani 1 1 d U . . O7 O 0.6309(5) 0.2890(4) 0.2728(3) 0.0867(15) Uani 1 1 d U . . O8 O 0.7670(5) 0.2587(3) 0.3172(3) 0.0765(14) Uani 1 1 d U . . O9A O 0.9288(10) 0.4560(5) 0.2880(6) 0.0851(19) Uani 0.498(7) 1 d PDU . . O9B O 0.8805(9) 0.4278(6) 0.3418(6) 0.0838(19) Uani 0.502(7) 1 d PDU . . O10 O 0.9572(4) 0.3429(3) 0.3094(3) 0.0754(14) Uani 1 1 d DU . . N1 N 0.6916(7) 0.4983(4) 0.2963(4) 0.107(2) Uani 1 1 d DU . . N2 N 0.9095(7) 0.4393(6) 0.1377(5) 0.1118(16) Uani 1 1 d U . . N3 N 0.6086(4) 0.3350(4) 0.1338(3) 0.0530(13) Uani 1 1 d U . . N4 N 0.6738(6) 0.2468(4) 0.3098(3) 0.0662(15) Uani 1 1 d U . . N5A N 0.9837(11) 0.4097(6) 0.3202(7) 0.080(2) Uani 0.498(7) 1 d PDU . . N5B N 0.9388(12) 0.3748(8) 0.3569(5) 0.084(2) Uani 0.502(7) 1 d PDU . . N6 N 0.8870(4) 0.2401(4) 0.1950(3) 0.0579(17) Uani 1 1 d . . . C1 C 0.9333(5) 0.1910(4) 0.2345(4) 0.058(2) Uani 1 1 d . . . H1 H 0.9374 0.2009 0.2766 0.069 Uiso 1 1 calc R . . C2 C 0.9756(6) 0.1255(5) 0.2149(6) 0.087(4) Uani 1 1 d . . . H2 H 1.0065 0.0917 0.2433 0.104 Uiso 1 1 calc R . . C3 C 0.9708(10) 0.1118(7) 0.1525(9) 0.135(7) Uani 1 1 d . . . H3 H 0.9992 0.0688 0.1379 0.162 Uiso 1 1 calc R . . C4 C 0.9241(10) 0.1617(10) 0.1129(8) 0.141(7) Uani 1 1 d . . . H4 H 0.9183 0.1527 0.0706 0.169 Uiso 1 1 calc R . . C5 C 0.8853(7) 0.2256(7) 0.1348(4) 0.093(4) Uani 1 1 d . . . H5 H 0.8564 0.2604 0.1065 0.112 Uiso 1 1 calc R . . C6 C 0.5322(4) 0.8653(3) 0.0593(3) 0.0339(13) Uani 1 1 d . . . C7 C 0.4404(5) 0.8579(4) 0.0848(3) 0.0412(15) Uani 1 1 d . . . H7 H 0.4349 0.8747 0.1247 0.049 Uiso 1 1 calc R . . C8 C 0.3581(5) 0.8257(4) 0.0508(3) 0.0468(16) Uani 1 1 d . . . H8 H 0.2976 0.8194 0.0680 0.056 Uiso 1 1 calc R . . C9 C 0.3658(5) 0.8025(4) -0.0096(3) 0.0429(15) Uani 1 1 d . . . H9 H 0.3101 0.7814 -0.0328 0.051 Uiso 1 1 calc R . . C10 C 0.4554(5) 0.8107(4) -0.0349(3) 0.0434(15) Uani 1 1 d . . . H10 H 0.4597 0.7956 -0.0754 0.052 Uiso 1 1 calc R . . C11 C 0.5392(5) 0.8411(3) -0.0008(3) 0.0378(14) Uani 1 1 d . . . H11 H 0.6002 0.8454 -0.0179 0.045 Uiso 1 1 calc R . . C12 C 0.6977(4) 0.8219(3) 0.1520(3) 0.0340(13) Uani 1 1 d . . . C13 C 0.6594(5) 0.7496(4) 0.1450(3) 0.0425(15) Uani 1 1 d . . . H13 H 0.6040 0.7396 0.1161 0.051 Uiso 1 1 calc R . . C14 C 0.7041(6) 0.6931(4) 0.1810(3) 0.0496(17) Uani 1 1 d . . . H14 H 0.6776 0.6452 0.1773 0.060 Uiso 1 1 calc R . . C15 C 0.7880(6) 0.7070(4) 0.2227(3) 0.0520(18) Uani 1 1 d . . . H15 H 0.8190 0.6681 0.2458 0.062 Uiso 1 1 calc R . . C16 C 0.8259(5) 0.7779(4) 0.2303(3) 0.0479(16) Uani 1 1 d . . . H16 H 0.8819 0.7870 0.2588 0.058 Uiso 1 1 calc R . . C17 C 0.7807(5) 0.8361(4) 0.1955(3) 0.0411(14) Uani 1 1 d . . . H17 H 0.8056 0.8843 0.2011 0.049 Uiso 1 1 calc R . . C18 C 0.7313(5) 0.9298(3) 0.0545(3) 0.0365(13) Uani 1 1 d . . . C19 C 0.6983(5) 0.9807(4) 0.0075(3) 0.0433(15) Uani 1 1 d . . . H19 H 0.6323 0.9990 0.0040 0.052 Uiso 1 1 calc R . . C20 C 0.7643(6) 1.0034(4) -0.0333(3) 0.0518(17) Uani 1 1 d . . . H20 H 0.7424 1.0372 -0.0643 0.062 Uiso 1 1 calc R . . C21 C 0.8613(6) 0.9770(4) -0.0291(3) 0.0510(17) Uani 1 1 d . . . H21 H 0.9047 0.9923 -0.0574 0.061 Uiso 1 1 calc R . . C22 C 0.8947(5) 0.9276(4) 0.0171(3) 0.0456(16) Uani 1 1 d . . . H22 H 0.9610 0.9101 0.0201 0.055 Uiso 1 1 calc R . . C23 C 0.8306(5) 0.9036(4) 0.0592(3) 0.0388(14) Uani 1 1 d . . . H23 H 0.8537 0.8703 0.0903 0.047 Uiso 1 1 calc R . . C24 C 0.6167(4) 0.9706(3) 0.1589(3) 0.0334(13) Uani 1 1 d . . . C25 C 0.5679(4) 0.9520(4) 0.2104(3) 0.0375(14) Uani 1 1 d . . . H25 H 0.5500 0.9028 0.2170 0.045 Uiso 1 1 calc R . . C26 C 0.5464(5) 1.0067(4) 0.2513(3) 0.0413(15) Uani 1 1 d . . . H26 H 0.5128 0.9946 0.2852 0.050 Uiso 1 1 calc R . . C27 C 0.5746(5) 1.0792(4) 0.2420(3) 0.0428(15) Uani 1 1 d . . . H27 H 0.5607 1.1157 0.2702 0.051 Uiso 1 1 calc R . . C28 C 0.6231(5) 1.0986(4) 0.1915(3) 0.0453(16) Uani 1 1 d . . . H28 H 0.6408 1.1480 0.1856 0.054 Uiso 1 1 calc R . . C29 C 0.6457(5) 1.0441(4) 0.1491(3) 0.0409(14) Uani 1 1 d . . . H29 H 0.6792 1.0566 0.1152 0.049 Uiso 1 1 calc R . . C30 C 0.1239(4) 0.3483(3) 0.0048(2) 0.0290(12) Uani 1 1 d . . . C31 C 0.0316(5) 0.3701(4) 0.0234(3) 0.0444(16) Uani 1 1 d . . . H31 H 0.0295 0.4004 0.0579 0.053 Uiso 1 1 calc R . . C32 C -0.0572(5) 0.3460(5) -0.0101(3) 0.0562(19) Uani 1 1 d . . . H32 H -0.1193 0.3604 0.0022 0.067 Uiso 1 1 calc R . . C33 C -0.0549(5) 0.3010(4) -0.0616(3) 0.0514(17) Uani 1 1 d . . . H33 H -0.1150 0.2845 -0.0833 0.062 Uiso 1 1 calc R . . C34 C 0.0373(5) 0.2807(4) -0.0805(3) 0.0436(15) Uani 1 1 d . . . H34 H 0.0393 0.2512 -0.1155 0.052 Uiso 1 1 calc R . . C35 C 0.1265(5) 0.3041(3) -0.0474(3) 0.0371(14) Uani 1 1 d . . . H35 H 0.1885 0.2902 -0.0601 0.045 Uiso 1 1 calc R . . C36 C 0.2255(4) 0.4505(3) 0.0983(3) 0.0305(12) Uani 1 1 d . . . C37 C 0.1764(5) 0.4423(3) 0.1508(3) 0.0373(14) Uani 1 1 d . . . H37 H 0.1513 0.3959 0.1606 0.045 Uiso 1 1 calc R . . C38 C 0.1646(5) 0.5029(4) 0.1887(3) 0.0454(16) Uani 1 1 d . . . H38 H 0.1313 0.4974 0.2238 0.055 Uiso 1 1 calc R . . C39 C 0.2017(5) 0.5702(4) 0.1745(3) 0.0463(16) Uani 1 1 d . . . H39 H 0.1936 0.6107 0.2002 0.056 Uiso 1 1 calc R . . C40 C 0.2513(5) 0.5799(4) 0.1227(3) 0.0439(15) Uani 1 1 d . . . H40 H 0.2768 0.6264 0.1138 0.053 Uiso 1 1 calc R . . C41 C 0.2631(5) 0.5197(3) 0.0839(3) 0.0378(14) Uani 1 1 d . . . H41 H 0.2958 0.5258 0.0486 0.045 Uiso 1 1 calc R . . C42 C 0.3332(4) 0.3939(3) -0.0017(2) 0.0300(12) Uani 1 1 d . . . C43 C 0.3043(5) 0.4403(3) -0.0523(3) 0.0366(13) Uani 1 1 d . . . H43 H 0.2378 0.4568 -0.0602 0.044 Uiso 1 1 calc R . . C44 C 0.3764(5) 0.4611(4) -0.0905(3) 0.0452(16) Uani 1 1 d . . . H44 H 0.3580 0.4920 -0.1241 0.054 Uiso 1 1 calc R . . C45 C 0.4742(5) 0.4366(4) -0.0792(3) 0.0481(17) Uani 1 1 d . . . H45 H 0.5219 0.4512 -0.1051 0.058 Uiso 1 1 calc R . . C46 C 0.5026(5) 0.3905(4) -0.0296(3) 0.0434(15) Uani 1 1 d . . . H46 H 0.5692 0.3738 -0.0226 0.052 Uiso 1 1 calc R . . C47 C 0.4331(4) 0.3691(3) 0.0097(3) 0.0335(13) Uani 1 1 d . . . H47 H 0.4527 0.3386 0.0434 0.040 Uiso 1 1 calc R . . C48 C 0.2830(4) 0.2952(3) 0.0985(2) 0.0269(11) Uani 1 1 d . . . C49 C 0.2380(4) 0.2253(3) 0.0903(3) 0.0318(12) Uani 1 1 d . . . H49 H 0.1830 0.2182 0.0606 0.038 Uiso 1 1 calc R . . C50 C 0.2760(5) 0.1660(3) 0.1270(3) 0.0374(13) Uani 1 1 d . . . H50 H 0.2456 0.1194 0.1224 0.045 Uiso 1 1 calc R . . C51 C 0.3588(5) 0.1764(4) 0.1703(3) 0.0389(14) Uani 1 1 d . . . H51 H 0.3843 0.1363 0.1941 0.047 Uiso 1 1 calc R . . C52 C 0.4041(4) 0.2449(4) 0.1787(3) 0.0373(14) Uani 1 1 d . . . H52 H 0.4604 0.2509 0.2077 0.045 Uiso 1 1 calc R . . C53 C 0.3653(4) 0.3054(3) 0.1436(2) 0.0320(12) Uani 1 1 d . . . H53 H 0.3940 0.3524 0.1501 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.02530(19) 0.0299(2) 0.02678(18) -0.00163(13) -0.00091(12) 0.00140(13) P1 0.0331(8) 0.0345(8) 0.0305(7) -0.0014(6) 0.0055(6) 0.0009(6) P2 0.0265(7) 0.0265(7) 0.0265(7) -0.0007(5) 0.0001(5) 0.0012(6) O1 0.133(4) 0.098(4) 0.116(4) -0.024(3) 0.035(3) -0.001(4) O2 0.125(4) 0.072(3) 0.096(4) -0.003(3) -0.008(3) 0.028(3) O3 0.079(2) 0.149(3) 0.112(3) 0.055(2) 0.022(2) -0.005(2) O4 0.080(2) 0.149(3) 0.114(3) 0.055(2) 0.023(2) -0.005(2) O5 0.036(2) 0.044(2) 0.048(2) 0.0005(18) -0.0088(18) 0.0060(18) O6 0.055(3) 0.071(3) 0.070(3) -0.030(2) -0.023(2) 0.017(2) O7 0.080(3) 0.092(3) 0.084(3) 0.036(2) -0.009(2) -0.019(2) O8 0.073(3) 0.078(3) 0.080(3) 0.036(2) 0.014(2) 0.010(2) O9A 0.080(4) 0.079(4) 0.089(4) -0.012(3) -0.026(3) 0.012(3) O9B 0.081(4) 0.080(4) 0.083(4) -0.015(3) -0.028(3) 0.023(3) O10 0.069(3) 0.072(3) 0.078(3) -0.009(2) -0.029(2) 0.020(2) N1 0.112(4) 0.092(3) 0.117(4) -0.014(3) 0.012(3) 0.016(3) N2 0.078(2) 0.148(3) 0.111(3) 0.055(2) 0.023(2) -0.005(3) N3 0.044(3) 0.058(3) 0.052(3) -0.009(2) -0.016(2) 0.011(2) N4 0.073(3) 0.059(3) 0.064(3) 0.022(3) -0.002(3) -0.006(3) N5A 0.075(3) 0.076(3) 0.082(3) -0.011(3) -0.023(3) 0.015(3) N5B 0.081(4) 0.078(4) 0.084(4) -0.012(3) -0.031(3) 0.021(3) N6 0.034(3) 0.069(4) 0.069(4) -0.033(3) 0.001(3) 0.004(3) C1 0.031(3) 0.036(4) 0.108(6) -0.009(4) 0.014(4) -0.002(3) C2 0.048(5) 0.042(5) 0.178(12) -0.003(6) 0.044(6) 0.002(4) C3 0.095(9) 0.097(9) 0.226(18) -0.096(11) 0.081(11) -0.001(7) C4 0.096(9) 0.168(14) 0.162(14) -0.110(12) 0.024(9) 0.032(9) C5 0.065(6) 0.140(10) 0.075(6) -0.058(6) 0.009(5) 0.030(6) C6 0.034(3) 0.036(3) 0.033(3) -0.004(2) 0.005(2) 0.003(2) C7 0.042(3) 0.051(4) 0.032(3) -0.005(3) 0.009(3) -0.009(3) C8 0.038(3) 0.061(4) 0.042(4) 0.000(3) 0.005(3) -0.004(3) C9 0.048(4) 0.041(4) 0.038(3) -0.002(3) -0.007(3) 0.000(3) C10 0.052(4) 0.048(4) 0.029(3) -0.005(3) 0.000(3) 0.011(3) C11 0.042(3) 0.039(3) 0.033(3) -0.002(3) 0.005(3) 0.004(3) C12 0.036(3) 0.035(3) 0.032(3) 0.000(2) 0.008(2) 0.005(2) C13 0.054(4) 0.043(4) 0.032(3) -0.004(3) 0.011(3) 0.002(3) C14 0.070(5) 0.039(4) 0.042(4) 0.001(3) 0.016(3) 0.003(3) C15 0.063(5) 0.055(5) 0.042(4) 0.012(3) 0.021(3) 0.021(4) C16 0.042(4) 0.060(5) 0.043(4) 0.007(3) 0.009(3) 0.010(3) C17 0.038(3) 0.042(4) 0.044(3) 0.000(3) 0.007(3) 0.004(3) C18 0.039(3) 0.037(3) 0.035(3) -0.003(3) 0.008(3) 0.000(3) C19 0.047(4) 0.043(4) 0.041(3) 0.001(3) 0.012(3) 0.004(3) C20 0.067(5) 0.049(4) 0.041(4) 0.005(3) 0.014(3) -0.005(4) C21 0.056(4) 0.056(4) 0.044(4) -0.008(3) 0.022(3) -0.017(3) C22 0.035(3) 0.058(4) 0.045(4) -0.006(3) 0.011(3) -0.010(3) C23 0.039(3) 0.043(4) 0.034(3) -0.006(3) 0.003(3) -0.002(3) C24 0.031(3) 0.038(3) 0.031(3) -0.004(2) 0.000(2) 0.005(2) C25 0.036(3) 0.037(3) 0.039(3) -0.002(3) 0.002(3) 0.001(3) C26 0.035(3) 0.054(4) 0.034(3) -0.006(3) -0.002(3) -0.002(3) C27 0.044(4) 0.047(4) 0.036(3) -0.010(3) -0.004(3) 0.012(3) C28 0.051(4) 0.034(3) 0.049(4) -0.004(3) -0.005(3) 0.007(3) C29 0.044(4) 0.039(4) 0.039(3) 0.001(3) 0.002(3) 0.001(3) C30 0.028(3) 0.031(3) 0.028(3) 0.002(2) -0.001(2) 0.003(2) C31 0.035(3) 0.059(4) 0.039(3) -0.004(3) 0.003(3) 0.000(3) C32 0.032(3) 0.088(6) 0.048(4) -0.010(4) -0.001(3) 0.011(3) C33 0.035(4) 0.068(5) 0.048(4) -0.004(3) -0.012(3) -0.001(3) C34 0.049(4) 0.043(4) 0.036(3) -0.010(3) -0.010(3) -0.005(3) C35 0.038(3) 0.037(3) 0.035(3) -0.006(3) -0.001(3) 0.006(3) C36 0.030(3) 0.027(3) 0.033(3) -0.005(2) -0.004(2) -0.001(2) C37 0.042(3) 0.032(3) 0.037(3) -0.007(3) 0.001(3) -0.001(3) C38 0.050(4) 0.049(4) 0.039(3) -0.009(3) 0.010(3) 0.004(3) C39 0.043(4) 0.044(4) 0.050(4) -0.015(3) 0.000(3) 0.006(3) C40 0.045(4) 0.031(3) 0.055(4) -0.008(3) -0.002(3) -0.004(3) C41 0.038(3) 0.032(3) 0.042(3) -0.004(3) 0.002(3) -0.001(3) C42 0.033(3) 0.029(3) 0.028(3) -0.002(2) 0.001(2) -0.002(2) C43 0.040(3) 0.033(3) 0.036(3) 0.002(3) 0.000(3) -0.002(3) C44 0.054(4) 0.045(4) 0.035(3) 0.013(3) 0.002(3) -0.010(3) C45 0.045(4) 0.062(4) 0.038(3) 0.012(3) 0.007(3) -0.014(3) C46 0.034(3) 0.052(4) 0.045(4) 0.005(3) 0.007(3) -0.004(3) C47 0.034(3) 0.035(3) 0.031(3) 0.003(2) 0.000(2) 0.001(2) C48 0.024(3) 0.029(3) 0.028(3) 0.000(2) 0.005(2) 0.003(2) C49 0.032(3) 0.035(3) 0.029(3) -0.002(2) 0.004(2) 0.000(2) C50 0.045(3) 0.030(3) 0.038(3) 0.004(3) 0.006(3) 0.005(3) C51 0.043(3) 0.039(4) 0.035(3) 0.010(3) 0.010(3) 0.010(3) C52 0.030(3) 0.050(4) 0.030(3) 0.009(3) -0.002(2) 0.003(3) C53 0.030(3) 0.036(3) 0.029(3) 0.002(2) 0.003(2) -0.002(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 La O1 2.556(7) . ? La O3 2.580(7) . ? La O4 2.589(7) . ? La O6 2.626(5) . ? La O9A 2.634(11) . ? La O10 2.635(5) . ? La O8 2.643(5) . ? La O2 2.655(6) . ? La O5 2.678(4) . ? La O7 2.694(6) . ? La O9B 2.727(11) . ? La N6 2.796(6) . ? P1 C12 1.791(6) . ? P1 C18 1.798(6) . ? P1 C6 1.801(6) . ? P1 C24 1.803(6) . ? P2 C48 1.788(5) . ? P2 C36 1.792(6) . ? P2 C42 1.793(6) . ? P2 C30 1.793(5) . ? O1 N1 1.231(5) . ? O2 N1 1.220(5) . ? O3 N2 1.152(10) . ? O4 N2 1.241(10) . ? O5 N3 1.253(7) . ? O6 N3 1.251(7) . ? O7 N4 1.203(8) . ? O8 N4 1.248(8) . ? O9A N5A 1.266(9) . ? O9B N5B 1.247(9) . ? O10 N5B 1.229(9) . ? O10 N5A 1.265(9) . ? N6 C1 1.334(10) . ? N6 C5 1.335(10) . ? C1 C2 1.390(11) . ? C1 H1 0.9300 . ? C2 C3 1.376(19) . ? C2 H2 0.9300 . ? C3 C4 1.35(2) . ? C3 H3 0.9300 . ? C4 C5 1.363(15) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.392(8) . ? C6 C7 1.400(8) . ? C7 C8 1.378(9) . ? C7 H7 0.9300 . ? C8 C9 1.394(9) . ? C8 H8 0.9300 . ? C9 C10 1.373(9) . ? C9 H9 0.9300 . ? C10 C11 1.381(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.395(8) . ? C12 C13 1.396(9) . ? C13 C14 1.376(9) . ? C13 H13 0.9300 . ? C14 C15 1.379(10) . ? C14 H14 0.9300 . ? C15 C16 1.373(10) . ? C15 H15 0.9300 . ? C16 C17 1.386(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.392(8) . ? C18 C19 1.407(9) . ? C19 C20 1.376(9) . ? C19 H19 0.9300 . ? C20 C21 1.366(10) . ? C20 H20 0.9300 . ? C21 C22 1.378(10) . ? C21 H21 0.9300 . ? C22 C23 1.385(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.394(8) . ? C24 C29 1.399(9) . ? C25 C26 1.377(9) . ? C25 H25 0.9300 . ? C26 C27 1.375(9) . ? C26 H26 0.9300 . ? C27 C28 1.377(9) . ? C27 H27 0.9300 . ? C28 C29 1.400(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.387(8) . ? C30 C35 1.391(8) . ? C31 C32 1.386(9) . ? C31 H31 0.9300 . ? C32 C33 1.386(10) . ? C32 H32 0.9300 . ? C33 C34 1.382(10) . ? C33 H33 0.9300 . ? C34 C35 1.383(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.384(8) . ? C36 C41 1.388(8) . ? C37 C38 1.385(9) . ? C37 H37 0.9300 . ? C38 C39 1.353(10) . ? C38 H38 0.9300 . ? C39 C40 1.378(10) . ? C39 H39 0.9300 . ? C40 C41 1.392(9) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.395(8) . ? C42 C43 1.400(8) . ? C43 C44 1.386(9) . ? C43 H43 0.9300 . ? C44 C45 1.368(9) . ? C44 H44 0.9300 . ? C45 C46 1.380(9) . ? C45 H45 0.9300 . ? C46 C47 1.381(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.393(8) . ? C48 C53 1.398(7) . ? C49 C50 1.390(8) . ? C49 H49 0.9300 . ? C50 C51 1.379(8) . ? C50 H50 0.9300 . ? C51 C52 1.372(9) . ? C51 H51 0.9300 . ? C52 C53 1.394(8) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La O3 121.8(3) . . ? O1 La O4 131.2(3) . . ? O3 La O4 43.2(2) . . ? O1 La O6 119.6(2) . . ? O3 La O6 71.3(2) . . ? O4 La O6 99.5(2) . . ? O1 La O9A 77.8(4) . . ? O3 La O9A 85.3(3) . . ? O4 La O9A 57.6(4) . . ? O6 La O9A 155.8(3) . . ? O1 La O10 96.4(2) . . ? O3 La O10 111.5(2) . . ? O4 La O10 68.5(2) . . ? O6 La O10 136.50(16) . . ? O9A La O10 47.17(19) . . ? O1 La O8 78.4(2) . . ? O3 La O8 159.0(3) . . ? O4 La O8 129.6(2) . . ? O6 La O8 94.2(2) . . ? O9A La O8 106.5(3) . . ? O10 La O8 68.3(2) . . ? O1 La O2 46.14(13) . . ? O3 La O2 76.3(3) . . ? O4 La O2 93.3(3) . . ? O6 La O2 113.93(19) . . ? O9A La O2 64.4(3) . . ? O10 La O2 108.6(2) . . ? O8 La O2 124.4(2) . . ? O1 La O5 79.0(2) . . ? O3 La O5 73.1(2) . . ? O4 La O5 116.1(2) . . ? O6 La O5 46.35(15) . . ? O9A La O5 132.8(2) . . ? O10 La O5 174.90(17) . . ? O8 La O5 108.32(17) . . ? O2 La O5 69.85(19) . . ? O1 La O7 65.7(2) . . ? O3 La O7 134.2(2) . . ? O4 La O7 163.1(3) . . ? O6 La O7 67.9(2) . . ? O9A La O7 136.2(4) . . ? O10 La O7 112.2(2) . . ? O8 La O7 44.64(18) . . ? O2 La O7 102.1(2) . . ? O5 La O7 64.00(16) . . ? O1 La O9B 55.9(3) . . ? O3 La O9B 116.5(4) . . ? O4 La O9B 87.7(4) . . ? O6 La O9B 172.1(4) . . ? O10 La O9B 43.83(18) . . ? O8 La O9B 78.7(3) . . ? O2 La O9B 68.3(2) . . ? O5 La O9B 132.6(2) . . ? O7 La O9B 104.4(3) . . ? O1 La N6 152.0(2) . . ? O3 La N6 86.2(3) . . ? O4 La N6 68.6(3) . . ? O6 La N6 65.81(16) . . ? O9A La N6 107.5(3) . . ? O10 La N6 71.02(17) . . ? O8 La N6 73.8(2) . . ? O2 La N6 161.0(2) . . ? O5 La N6 112.15(15) . . ? O7 La N6 95.3(2) . . ? O9B La N6 114.7(2) . . ? C12 P1 C18 110.2(3) . . ? C12 P1 C6 108.9(3) . . ? C18 P1 C6 107.2(3) . . ? C12 P1 C24 106.9(3) . . ? C18 P1 C24 110.8(3) . . ? C6 P1 C24 112.8(3) . . ? C48 P2 C36 107.7(3) . . ? C48 P2 C42 110.6(3) . . ? C36 P2 C42 108.9(3) . . ? C48 P2 C30 109.8(3) . . ? C36 P2 C30 111.0(3) . . ? C42 P2 C30 108.8(3) . . ? N1 O1 La 102.8(4) . . ? N1 O2 La 98.0(4) . . ? N2 O3 La 106.6(7) . . ? N2 O4 La 102.9(6) . . ? N3 O5 La 99.0(3) . . ? N3 O6 La 101.6(4) . . ? N4 O7 La 101.2(5) . . ? N4 O8 La 102.4(4) . . ? N5A O9A La 99.7(7) . . ? N5B O9B La 96.7(7) . . ? N5B O10 La 101.8(6) . . ? N5A O10 La 99.7(6) . . ? O2 N1 O1 113.0(6) . . ? O3 N2 O4 105.1(9) . . ? O6 N3 O5 113.0(5) . . ? O7 N4 O8 111.6(7) . . ? O10 N5A O9A 112.8(9) . . ? O10 N5B O9B 108.0(9) . . ? C1 N6 C5 117.5(8) . . ? C1 N6 La 121.6(5) . . ? C5 N6 La 120.9(6) . . ? N6 C1 C2 122.2(9) . . ? N6 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.6(11) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 118.7(10) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.1(14) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N6 C5 C4 122.7(13) . . ? N6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C11 C6 C7 119.7(6) . . ? C11 C6 P1 119.9(5) . . ? C7 C6 P1 120.2(4) . . ? C8 C7 C6 120.0(6) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.8(6) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 120.3(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.6(6) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C6 119.7(6) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C17 C12 C13 119.7(6) . . ? C17 C12 P1 118.5(5) . . ? C13 C12 P1 121.8(5) . . ? C14 C13 C12 119.5(6) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 120.6(7) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 120.4(6) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.1(7) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 119.7(6) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? C23 C18 C19 119.3(6) . . ? C23 C18 P1 121.2(5) . . ? C19 C18 P1 119.5(5) . . ? C20 C19 C18 119.5(6) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 121.1(7) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.8(6) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 120.7(6) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C18 119.5(6) . . ? C22 C23 H23 120.2 . . ? C18 C23 H23 120.2 . . ? C25 C24 C29 120.6(6) . . ? C25 C24 P1 118.8(5) . . ? C29 C24 P1 120.6(5) . . ? C26 C25 C24 119.8(6) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 120.1(6) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.9(6) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C29 120.3(6) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C24 C29 C28 118.3(6) . . ? C24 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C31 C30 C35 120.1(5) . . ? C31 C30 P2 121.0(4) . . ? C35 C30 P2 118.8(4) . . ? C32 C31 C30 119.1(6) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 121.0(7) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 119.6(6) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C35 C34 C33 120.0(6) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120.2(6) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C37 C36 C41 119.8(5) . . ? C37 C36 P2 119.9(4) . . ? C41 C36 P2 120.3(5) . . ? C36 C37 C38 120.1(6) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 119.9(6) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 121.1(6) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C39 C40 C41 119.7(6) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C36 C41 C40 119.3(6) . . ? C36 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C47 C42 C43 120.2(5) . . ? C47 C42 P2 121.3(4) . . ? C43 C42 P2 118.5(4) . . ? C44 C43 C42 119.0(6) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C45 C44 C43 120.6(6) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 120.4(6) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C47 120.6(6) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C46 C47 C42 119.2(5) . . ? C46 C47 H47 120.4 . . ? C42 C47 H47 120.4 . . ? C49 C48 C53 119.9(5) . . ? C49 C48 P2 121.0(4) . . ? C53 C48 P2 119.0(4) . . ? C50 C49 C48 119.5(5) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C51 C50 C49 120.0(6) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 121.2(6) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 119.6(5) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C48 119.8(5) . . ? C52 C53 H53 120.1 . . ? C48 C53 H53 120.1 . . ? _database_code_depnum_ccdc_archive 'CCDC 963095' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 Ce N6 O10 P2' _chemical_formula_weight 1128.01 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' Ce Ce -0.2486 2.6331 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 13.2645(5) _cell_length_b 17.9358(7) _cell_length_c 21.7448(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.433(2) _cell_angle_gamma 90.00 _cell_volume 5140.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 176769 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (536 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 176769 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_unetI/netI 0.0596 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9748 _reflns_number_gt 7415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Two nitrite ions (containing N1 and N5) are badly resolved; one of them (N5) was found to be disordered over two positions sharing one O atom, which were refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths, angles and displacement parameters for several nitrite ions: DFIX 1.24 0.005 N1 O1 DFIX 1.24 0.005 N1 O2 DFIX 2.05 0.005 O1 O2 DFIX 1.24 0.01 N5A O9A DFIX 1.24 0.01 N5A O10 DFIX 2.05 0.01 O9A O10 DFIX 1.24 0.01 N5B O9B DFIX 1.24 0.01 N5B O10 DFIX 2.05 0.01 O9B O10 ISOR 0.005 N1 O3 O4 O7 O8 N5A SIMU .005 .005 3. N1 O1 O2 SIMU .005 .005 3. N2 O3 O4 SIMU .005 .005 3. N3 O5 O6 SIMU .005 .005 3. N4 O7 O8 SIMU .005 .005 3. N5A N5B O9A O9B O10 The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0773P)^2^+15.6730P] 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 9748 _refine_ls_number_parameters 668 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.167 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.129 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 Ce Ce 0.78852(2) 0.365247(18) 0.236173(14) 0.02640(12) Uani 1 1 d . . . P1 P 0.64413(12) 0.89800(9) 0.10595(7) 0.0313(3) Uani 1 1 d . . . P2 P 0.24068(11) 0.37204(8) 0.04994(7) 0.0256(3) Uani 1 1 d . . . O1 O 0.6928(7) 0.4338(5) 0.3141(4) 0.122(2) Uani 1 1 d DU . . O2 O 0.7337(7) 0.5057(4) 0.2480(3) 0.108(2) Uani 1 1 d DU . . O3 O 0.8226(5) 0.4260(5) 0.1340(3) 0.0951(17) Uani 1 1 d U . . O4 O 0.9471(6) 0.4051(5) 0.1862(4) 0.1126(19) Uani 1 1 d U . . O5 O 0.6094(3) 0.3891(3) 0.1711(2) 0.0398(10) Uani 1 1 d U . . O6 O 0.6845(4) 0.2926(3) 0.1466(3) 0.0637(13) Uani 1 1 d U . . O7 O 0.6311(5) 0.2935(4) 0.2744(3) 0.0897(16) Uani 1 1 d U . . O8 O 0.7655(5) 0.2583(4) 0.3151(3) 0.0804(15) Uani 1 1 d U . . O9A O 0.9173(11) 0.4543(5) 0.2986(7) 0.097(2) Uani 0.511(8) 1 d PDU . . O9B O 0.8362(9) 0.3934(8) 0.3522(6) 0.096(2) Uani 0.489(8) 1 d PDU . . O10 O 0.9536(5) 0.3422(4) 0.3112(3) 0.0831(17) Uani 1 1 d DU . . N1 N 0.6915(8) 0.4984(5) 0.2943(5) 0.115(2) Uani 1 1 d DU . . N2 N 0.9091(6) 0.4381(6) 0.1383(4) 0.0895(19) Uani 1 1 d U . . N3 N 0.6082(4) 0.3350(4) 0.1356(3) 0.0504(13) Uani 1 1 d U . . N4 N 0.6725(6) 0.2487(4) 0.3087(4) 0.0710(16) Uani 1 1 d U . . N5A N 0.9805(11) 0.4081(6) 0.3232(8) 0.090(2) Uani 0.511(8) 1 d PDU . . N5B N 0.9257(10) 0.3719(10) 0.3586(6) 0.092(2) Uani 0.489(8) 1 d PDU . . N6 N 0.8872(4) 0.2411(4) 0.1952(3) 0.0532(17) Uani 1 1 d . . . C1 C 0.9330(5) 0.1915(4) 0.2341(4) 0.055(2) Uani 1 1 d . . . H1 H 0.9370 0.2008 0.2764 0.066 Uiso 1 1 calc R . . C2 C 0.9749(7) 0.1265(5) 0.2140(6) 0.082(3) Uani 1 1 d . . . H2 H 1.0067 0.0922 0.2419 0.098 Uiso 1 1 calc R . . C3 C 0.9674(10) 0.1146(7) 0.1508(9) 0.120(6) Uani 1 1 d . . . H3 H 0.9931 0.0709 0.1355 0.144 Uiso 1 1 calc R . . C4 C 0.9235(10) 0.1655(9) 0.1115(7) 0.121(5) Uani 1 1 d . . . H4 H 0.9191 0.1577 0.0690 0.146 Uiso 1 1 calc R . . C5 C 0.8857(7) 0.2281(6) 0.1344(4) 0.080(3) Uani 1 1 d . . . H5 H 0.8574 0.2639 0.1068 0.096 Uiso 1 1 calc R . . C6 C 0.5321(5) 0.8652(3) 0.0592(3) 0.0333(13) Uani 1 1 d . . . C7 C 0.4408(5) 0.8576(4) 0.0840(3) 0.0415(16) Uani 1 1 d . . . H7 H 0.4350 0.8745 0.1239 0.050 Uiso 1 1 calc R . . C8 C 0.3588(5) 0.8251(4) 0.0500(3) 0.0462(17) Uani 1 1 d . . . H8 H 0.2984 0.8185 0.0673 0.055 Uiso 1 1 calc R . . C9 C 0.3665(5) 0.8021(4) -0.0104(3) 0.0429(16) Uani 1 1 d . . . H9 H 0.3107 0.7810 -0.0338 0.051 Uiso 1 1 calc R . . C10 C 0.4555(5) 0.8103(4) -0.0355(3) 0.0442(17) Uani 1 1 d . . . H10 H 0.4599 0.7949 -0.0759 0.053 Uiso 1 1 calc R . . C11 C 0.5397(5) 0.8415(4) -0.0014(3) 0.0378(15) Uani 1 1 d . . . H11 H 0.6005 0.8465 -0.0186 0.045 Uiso 1 1 calc R . . C12 C 0.6989(5) 0.8225(3) 0.1518(3) 0.0327(13) Uani 1 1 d . . . C13 C 0.6602(5) 0.7497(4) 0.1450(3) 0.0413(16) Uani 1 1 d . . . H13 H 0.6044 0.7396 0.1163 0.050 Uiso 1 1 calc R . . C14 C 0.7059(6) 0.6935(4) 0.1813(3) 0.0507(19) Uani 1 1 d . . . H14 H 0.6801 0.6453 0.1775 0.061 Uiso 1 1 calc R . . C15 C 0.7892(6) 0.7080(5) 0.2231(3) 0.0497(19) Uani 1 1 d . . . H15 H 0.8202 0.6693 0.2467 0.060 Uiso 1 1 calc R . . C16 C 0.8270(5) 0.7789(4) 0.2303(3) 0.0462(17) Uani 1 1 d . . . H16 H 0.8833 0.7882 0.2587 0.055 Uiso 1 1 calc R . . C17 C 0.7815(5) 0.8362(4) 0.1955(3) 0.0404(15) Uani 1 1 d . . . H17 H 0.8062 0.8846 0.2012 0.048 Uiso 1 1 calc R . . C18 C 0.7310(5) 0.9301(4) 0.0539(3) 0.0344(14) Uani 1 1 d . . . C19 C 0.6980(5) 0.9814(4) 0.0073(3) 0.0424(16) Uani 1 1 d . . . H19 H 0.6321 0.9999 0.0040 0.051 Uiso 1 1 calc R . . C20 C 0.7638(6) 1.0043(4) -0.0337(3) 0.0485(18) Uani 1 1 d . . . H20 H 0.7421 1.0383 -0.0646 0.058 Uiso 1 1 calc R . . C21 C 0.8618(6) 0.9771(4) -0.0291(3) 0.0502(19) Uani 1 1 d . . . H21 H 0.9055 0.9925 -0.0573 0.060 Uiso 1 1 calc R . . C22 C 0.8948(5) 0.9275(4) 0.0169(3) 0.0474(17) Uani 1 1 d . . . H22 H 0.9610 0.9096 0.0198 0.057 Uiso 1 1 calc R . . C23 C 0.8303(5) 0.9039(4) 0.0590(3) 0.0379(15) Uani 1 1 d . . . H23 H 0.8533 0.8708 0.0904 0.045 Uiso 1 1 calc R . . C24 C 0.6168(5) 0.9711(3) 0.1582(3) 0.0327(13) Uani 1 1 d . . . C25 C 0.5676(5) 0.9526(4) 0.2095(3) 0.0357(14) Uani 1 1 d . . . H25 H 0.5492 0.9034 0.2159 0.043 Uiso 1 1 calc R . . C26 C 0.5459(5) 1.0074(4) 0.2510(3) 0.0418(16) Uani 1 1 d . . . H26 H 0.5121 0.9954 0.2849 0.050 Uiso 1 1 calc R . . C27 C 0.5747(5) 1.0798(4) 0.2415(3) 0.0419(16) Uani 1 1 d . . . H27 H 0.5608 1.1166 0.2696 0.050 Uiso 1 1 calc R . . C28 C 0.6236(5) 1.0988(4) 0.1913(3) 0.0443(17) Uani 1 1 d . . . H28 H 0.6421 1.1481 0.1856 0.053 Uiso 1 1 calc R . . C29 C 0.6455(5) 1.0447(4) 0.1489(3) 0.0383(15) Uani 1 1 d . . . H29 H 0.6788 1.0574 0.1149 0.046 Uiso 1 1 calc R . . C30 C 0.1238(4) 0.3482(3) 0.0051(3) 0.0281(12) Uani 1 1 d . . . C31 C 0.0312(5) 0.3707(4) 0.0233(3) 0.0424(16) Uani 1 1 d . . . H31 H 0.0291 0.4015 0.0576 0.051 Uiso 1 1 calc R . . C32 C -0.0583(5) 0.3467(5) -0.0104(4) 0.056(2) Uani 1 1 d . . . H32 H -0.1206 0.3613 0.0014 0.067 Uiso 1 1 calc R . . C33 C -0.0547(5) 0.3013(5) -0.0615(3) 0.0521(19) Uani 1 1 d . . . H33 H -0.1148 0.2844 -0.0831 0.063 Uiso 1 1 calc R . . C34 C 0.0368(5) 0.2809(4) -0.0806(3) 0.0421(16) Uani 1 1 d . . . H34 H 0.0385 0.2516 -0.1157 0.051 Uiso 1 1 calc R . . C35 C 0.1259(5) 0.3042(4) -0.0475(3) 0.0368(14) Uani 1 1 d . . . H35 H 0.1878 0.2904 -0.0603 0.044 Uiso 1 1 calc R . . C36 C 0.2260(4) 0.4513(3) 0.0985(3) 0.0292(13) Uani 1 1 d . . . C37 C 0.1758(5) 0.4424(4) 0.1509(3) 0.0368(14) Uani 1 1 d . . . H37 H 0.1504 0.3960 0.1603 0.044 Uiso 1 1 calc R . . C38 C 0.1638(5) 0.5029(4) 0.1889(3) 0.0447(17) Uani 1 1 d . . . H38 H 0.1296 0.4974 0.2237 0.054 Uiso 1 1 calc R . . C39 C 0.2025(5) 0.5707(4) 0.1751(3) 0.0463(18) Uani 1 1 d . . . H39 H 0.1953 0.6110 0.2011 0.056 Uiso 1 1 calc R . . C40 C 0.2521(5) 0.5802(4) 0.1229(3) 0.0425(16) Uani 1 1 d . . . H40 H 0.2777 0.6268 0.1139 0.051 Uiso 1 1 calc R . . C41 C 0.2635(5) 0.5201(3) 0.0843(3) 0.0352(14) Uani 1 1 d . . . H41 H 0.2963 0.5261 0.0490 0.042 Uiso 1 1 calc R . . C42 C 0.3326(4) 0.3938(3) -0.0014(3) 0.0282(12) Uani 1 1 d . . . C43 C 0.3035(5) 0.4404(3) -0.0525(3) 0.0351(14) Uani 1 1 d . . . H43 H 0.2368 0.4567 -0.0606 0.042 Uiso 1 1 calc R . . C44 C 0.3757(5) 0.4615(4) -0.0905(3) 0.0432(16) Uani 1 1 d . . . H44 H 0.3575 0.4929 -0.1240 0.052 Uiso 1 1 calc R . . C45 C 0.4739(5) 0.4364(4) -0.0793(3) 0.0474(18) Uani 1 1 d . . . H45 H 0.5216 0.4506 -0.1054 0.057 Uiso 1 1 calc R . . C46 C 0.5022(5) 0.3904(4) -0.0296(3) 0.0418(16) Uani 1 1 d . . . H46 H 0.5688 0.3736 -0.0224 0.050 Uiso 1 1 calc R . . C47 C 0.4324(4) 0.3692(3) 0.0097(3) 0.0319(13) Uani 1 1 d . . . H47 H 0.4521 0.3385 0.0434 0.038 Uiso 1 1 calc R . . C48 C 0.2829(4) 0.2950(3) 0.0989(2) 0.0257(12) Uani 1 1 d . . . C49 C 0.2367(4) 0.2251(3) 0.0909(3) 0.0302(13) Uani 1 1 d . . . H49 H 0.1811 0.2182 0.0614 0.036 Uiso 1 1 calc R . . C50 C 0.2750(5) 0.1664(3) 0.1274(3) 0.0356(14) Uani 1 1 d . . . H50 H 0.2441 0.1199 0.1231 0.043 Uiso 1 1 calc R . . C51 C 0.3588(5) 0.1761(4) 0.1703(3) 0.0383(15) Uani 1 1 d . . . H51 H 0.3853 0.1356 0.1934 0.046 Uiso 1 1 calc R . . C52 C 0.4032(5) 0.2447(4) 0.1793(3) 0.0365(15) Uani 1 1 d . . . H52 H 0.4590 0.2506 0.2088 0.044 Uiso 1 1 calc R . . C53 C 0.3652(4) 0.3056(4) 0.1443(3) 0.0327(13) Uani 1 1 d . . . H53 H 0.3940 0.3526 0.1510 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.02435(18) 0.0292(2) 0.02495(18) -0.00142(14) -0.00009(12) 0.00132(13) P1 0.0327(8) 0.0330(8) 0.0290(8) -0.0010(7) 0.0067(6) 0.0017(7) P2 0.0255(7) 0.0260(8) 0.0250(7) -0.0002(6) 0.0011(6) 0.0011(6) O1 0.145(5) 0.100(4) 0.123(4) -0.016(4) 0.028(4) 0.007(4) O2 0.139(5) 0.076(4) 0.105(4) -0.002(3) 0.000(4) 0.034(4) O3 0.073(3) 0.131(3) 0.083(3) 0.043(3) 0.015(3) -0.006(3) O4 0.082(3) 0.145(4) 0.112(3) 0.045(3) 0.021(3) -0.008(3) O5 0.034(2) 0.039(2) 0.044(2) -0.0017(18) -0.0063(18) 0.0044(18) O6 0.053(3) 0.069(3) 0.064(3) -0.030(2) -0.019(2) 0.017(2) O7 0.082(3) 0.096(3) 0.088(3) 0.037(3) -0.003(3) -0.015(3) O8 0.076(3) 0.081(3) 0.086(3) 0.039(2) 0.017(3) 0.013(3) O9A 0.091(4) 0.085(4) 0.106(4) -0.030(3) -0.033(4) 0.023(3) O9B 0.096(4) 0.087(4) 0.096(4) -0.028(3) -0.029(4) 0.031(3) O10 0.079(3) 0.074(3) 0.088(3) -0.021(3) -0.030(3) 0.027(3) N1 0.125(4) 0.095(4) 0.123(4) -0.008(4) 0.009(3) 0.020(3) N2 0.061(3) 0.133(4) 0.078(3) 0.043(3) 0.026(3) -0.013(3) N3 0.042(3) 0.057(3) 0.048(3) -0.010(2) -0.014(2) 0.010(2) N4 0.076(3) 0.064(3) 0.072(3) 0.026(3) 0.003(3) 0.000(3) N5A 0.086(4) 0.082(4) 0.094(4) -0.023(3) -0.026(3) 0.022(3) N5B 0.090(4) 0.082(4) 0.095(4) -0.026(4) -0.033(4) 0.027(4) N6 0.032(3) 0.063(4) 0.065(4) -0.031(3) 0.005(3) 0.005(3) C1 0.027(3) 0.038(4) 0.101(6) -0.013(4) 0.013(4) 0.002(3) C2 0.048(5) 0.047(5) 0.156(11) -0.011(6) 0.040(6) -0.007(4) C3 0.095(9) 0.087(9) 0.192(16) -0.077(10) 0.074(10) 0.001(7) C4 0.098(9) 0.142(13) 0.125(11) -0.080(10) 0.018(8) 0.031(9) C5 0.065(6) 0.108(8) 0.070(6) -0.046(6) 0.014(5) 0.021(5) C6 0.037(3) 0.033(3) 0.031(3) -0.001(3) 0.010(3) -0.001(3) C7 0.044(4) 0.050(4) 0.032(3) -0.002(3) 0.010(3) -0.005(3) C8 0.038(4) 0.056(5) 0.044(4) 0.001(3) 0.005(3) -0.006(3) C9 0.047(4) 0.042(4) 0.037(4) -0.005(3) -0.006(3) 0.002(3) C10 0.053(4) 0.047(4) 0.032(3) -0.005(3) -0.002(3) 0.011(3) C11 0.045(4) 0.040(4) 0.030(3) 0.001(3) 0.006(3) 0.006(3) C12 0.036(3) 0.035(3) 0.029(3) -0.001(3) 0.011(3) 0.005(3) C13 0.050(4) 0.043(4) 0.032(3) -0.006(3) 0.009(3) 0.002(3) C14 0.074(5) 0.037(4) 0.044(4) -0.002(3) 0.022(4) 0.001(4) C15 0.061(5) 0.055(5) 0.036(4) 0.010(3) 0.021(4) 0.021(4) C16 0.042(4) 0.060(5) 0.037(4) 0.008(3) 0.007(3) 0.012(4) C17 0.040(4) 0.042(4) 0.040(4) -0.002(3) 0.008(3) 0.006(3) C18 0.037(3) 0.036(3) 0.031(3) -0.006(3) 0.005(3) -0.003(3) C19 0.047(4) 0.045(4) 0.037(4) 0.004(3) 0.012(3) 0.000(3) C20 0.067(5) 0.042(4) 0.039(4) 0.000(3) 0.015(4) -0.008(4) C21 0.055(5) 0.053(5) 0.047(4) -0.010(4) 0.026(4) -0.020(4) C22 0.038(4) 0.056(4) 0.051(4) -0.008(4) 0.013(3) -0.013(3) C23 0.036(3) 0.043(4) 0.035(3) -0.004(3) 0.004(3) -0.003(3) C24 0.033(3) 0.035(3) 0.029(3) -0.002(3) 0.000(3) 0.005(3) C25 0.036(3) 0.040(4) 0.032(3) -0.004(3) 0.006(3) -0.005(3) C26 0.034(3) 0.054(4) 0.037(4) -0.008(3) 0.004(3) 0.003(3) C27 0.041(4) 0.047(4) 0.036(4) -0.013(3) -0.004(3) 0.014(3) C28 0.051(4) 0.031(4) 0.048(4) -0.005(3) -0.005(3) 0.007(3) C29 0.043(4) 0.035(4) 0.036(3) 0.001(3) 0.003(3) 0.003(3) C30 0.026(3) 0.032(3) 0.026(3) 0.003(2) 0.001(2) 0.001(2) C31 0.029(3) 0.060(5) 0.037(4) -0.010(3) 0.002(3) 0.005(3) C32 0.029(3) 0.089(6) 0.049(4) -0.008(4) -0.002(3) 0.010(4) C33 0.036(4) 0.073(5) 0.043(4) -0.007(4) -0.013(3) -0.008(4) C34 0.044(4) 0.046(4) 0.034(3) -0.006(3) -0.006(3) 0.003(3) C35 0.037(3) 0.036(4) 0.036(3) -0.004(3) 0.002(3) 0.006(3) C36 0.031(3) 0.025(3) 0.031(3) -0.005(2) -0.001(2) 0.003(2) C37 0.045(4) 0.034(3) 0.032(3) -0.003(3) 0.006(3) 0.003(3) C38 0.046(4) 0.048(4) 0.040(4) -0.010(3) 0.006(3) 0.006(3) C39 0.041(4) 0.044(4) 0.051(4) -0.019(3) -0.006(3) 0.010(3) C40 0.038(4) 0.030(3) 0.058(4) -0.010(3) 0.001(3) -0.004(3) C41 0.035(3) 0.034(3) 0.036(3) -0.004(3) 0.002(3) 0.000(3) C42 0.032(3) 0.028(3) 0.025(3) -0.002(2) 0.006(2) -0.002(2) C43 0.037(3) 0.033(3) 0.035(3) 0.005(3) 0.001(3) 0.000(3) C44 0.050(4) 0.048(4) 0.031(3) 0.012(3) 0.001(3) -0.012(3) C45 0.041(4) 0.065(5) 0.038(4) 0.013(3) 0.007(3) -0.013(3) C46 0.031(3) 0.055(4) 0.040(4) 0.008(3) 0.007(3) -0.003(3) C47 0.033(3) 0.034(3) 0.029(3) 0.004(3) 0.000(2) 0.002(3) C48 0.023(3) 0.029(3) 0.026(3) 0.003(2) 0.006(2) 0.001(2) C49 0.030(3) 0.033(3) 0.029(3) 0.001(3) 0.006(2) -0.001(3) C50 0.045(4) 0.027(3) 0.036(3) 0.004(3) 0.010(3) 0.000(3) C51 0.045(4) 0.038(4) 0.032(3) 0.012(3) 0.009(3) 0.011(3) C52 0.028(3) 0.049(4) 0.032(3) 0.008(3) 0.000(3) 0.001(3) C53 0.029(3) 0.038(3) 0.031(3) 0.003(3) 0.005(3) 0.000(3) _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 Ce O1 2.545(8) . ? Ce O3 2.559(6) . ? Ce O4 2.575(7) . ? Ce O9B 2.581(13) . ? Ce O6 2.606(5) . ? Ce O9A 2.607(12) . ? Ce O10 2.612(5) . ? Ce O8 2.615(6) . ? Ce O2 2.643(7) . ? Ce O5 2.660(4) . ? Ce O7 2.664(7) . ? Ce N6 2.781(6) . ? P1 C12 1.786(6) . ? P1 C18 1.798(6) . ? P1 C24 1.798(6) . ? P1 C6 1.802(6) . ? P2 C42 1.786(6) . ? P2 C30 1.789(6) . ? P2 C36 1.795(6) . ? P2 C48 1.794(6) . ? O1 N1 1.235(5) . ? O2 N1 1.213(5) . ? O3 N2 1.161(9) . ? O4 N2 1.253(10) . ? O5 N3 1.240(7) . ? O6 N3 1.268(7) . ? O7 N4 1.187(9) . ? O8 N4 1.237(9) . ? O9A N5A 1.256(9) . ? O9B N5B 1.242(9) . ? O10 N5B 1.251(9) . ? O10 N5A 1.253(9) . ? N6 C1 1.327(10) . ? N6 C5 1.338(10) . ? C1 C2 1.383(11) . ? C1 H1 0.9300 . ? C2 C3 1.384(18) . ? C2 H2 0.9300 . ? C3 C4 1.34(2) . ? C3 H3 0.9300 . ? C4 C5 1.348(15) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.387(9) . ? C6 C11 1.399(9) . ? C7 C8 1.373(9) . ? C7 H7 0.9300 . ? C8 C9 1.392(10) . ? C8 H8 0.9300 . ? C9 C10 1.363(10) . ? C9 H9 0.9300 . ? C10 C11 1.386(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.389(9) . ? C12 C13 1.405(9) . ? C13 C14 1.379(10) . ? C13 H13 0.9300 . ? C14 C15 1.375(11) . ? C14 H14 0.9300 . ? C15 C16 1.368(11) . ? C15 H15 0.9300 . ? C16 C17 1.377(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.391(9) . ? C18 C19 1.404(9) . ? C19 C20 1.377(9) . ? C19 H19 0.9300 . ? C20 C21 1.381(11) . ? C20 H20 0.9300 . ? C21 C22 1.373(11) . ? C21 H21 0.9300 . ? C22 C23 1.388(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.395(9) . ? C24 C25 1.394(9) . ? C25 C26 1.387(9) . ? C25 H25 0.9300 . ? C26 C27 1.375(10) . ? C26 H26 0.9300 . ? C27 C28 1.373(10) . ? C27 H27 0.9300 . ? C28 C29 1.392(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.392(8) . ? C30 C35 1.392(8) . ? C31 C32 1.391(9) . ? C31 H31 0.9300 . ? C32 C33 1.381(11) . ? C32 H32 0.9300 . ? C33 C34 1.376(10) . ? C33 H33 0.9300 . ? C34 C35 1.379(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.378(8) . ? C36 C37 1.391(9) . ? C37 C38 1.383(9) . ? C37 H37 0.9300 . ? C38 C39 1.366(10) . ? C38 H38 0.9300 . ? C39 C40 1.384(10) . ? C39 H39 0.9300 . ? C40 C41 1.387(9) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.392(8) . ? C42 C43 1.409(8) . ? C43 C44 1.387(9) . ? C43 H43 0.9300 . ? C44 C45 1.374(10) . ? C44 H44 0.9300 . ? C45 C46 1.379(9) . ? C45 H45 0.9300 . ? C46 C47 1.381(9) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.398(8) . ? C48 C53 1.400(8) . ? C49 C50 1.381(8) . ? C49 H49 0.9300 . ? C50 C51 1.379(9) . ? C50 H50 0.9300 . ? C51 C52 1.368(9) . ? C51 H51 0.9300 . ? C52 C53 1.394(9) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ce O3 121.4(3) . . ? O1 Ce O4 129.7(3) . . ? O3 Ce O4 44.2(2) . . ? O1 Ce O9B 48.8(3) . . ? O3 Ce O9B 135.8(4) . . ? O4 Ce O9B 103.6(4) . . ? O1 Ce O6 118.5(3) . . ? O3 Ce O6 72.3(2) . . ? O4 Ce O6 102.3(3) . . ? O9B Ce O6 151.5(4) . . ? O1 Ce O9A 72.8(4) . . ? O3 Ce O9A 91.2(4) . . ? O4 Ce O9A 62.0(4) . . ? O6 Ce O9A 163.1(4) . . ? O1 Ce O10 96.1(3) . . ? O3 Ce O10 113.1(2) . . ? O4 Ce O10 68.9(3) . . ? O9B Ce O10 47.5(2) . . ? O6 Ce O10 136.39(17) . . ? O9A Ce O10 46.9(2) . . ? O1 Ce O8 79.3(2) . . ? O3 Ce O8 158.0(3) . . ? O4 Ce O8 129.9(2) . . ? O9B Ce O8 62.3(4) . . ? O6 Ce O8 91.8(2) . . ? O9A Ce O8 103.1(3) . . ? O10 Ce O8 68.0(2) . . ? O1 Ce O2 46.45(13) . . ? O3 Ce O2 75.9(3) . . ? O4 Ce O2 91.3(3) . . ? O9B Ce O2 76.0(3) . . ? O6 Ce O2 114.9(2) . . ? O9A Ce O2 62.4(3) . . ? O10 Ce O2 108.1(2) . . ? O8 Ce O2 125.6(2) . . ? O1 Ce O5 78.1(2) . . ? O3 Ce O5 72.80(19) . . ? O4 Ce O5 117.0(2) . . ? O9B Ce O5 126.5(2) . . ? O6 Ce O5 46.89(15) . . ? O9A Ce O5 132.3(2) . . ? O10 Ce O5 173.52(19) . . ? O8 Ce O5 107.69(18) . . ? O2 Ce O5 70.1(2) . . ? O1 Ce O7 63.8(3) . . ? O3 Ce O7 134.2(2) . . ? O4 Ce O7 166.4(3) . . ? O9B Ce O7 84.5(4) . . ? O6 Ce O7 67.9(2) . . ? O9A Ce O7 128.6(4) . . ? O10 Ce O7 111.1(2) . . ? O8 Ce O7 44.5(2) . . ? O2 Ce O7 101.3(3) . . ? O5 Ce O7 63.84(17) . . ? C12 P1 C18 110.1(3) . . ? C12 P1 C24 107.3(3) . . ? C18 P1 C24 110.7(3) . . ? C12 P1 C6 109.0(3) . . ? C18 P1 C6 107.2(3) . . ? C24 P1 C6 112.5(3) . . ? C42 P2 C30 108.8(3) . . ? C42 P2 C36 108.7(3) . . ? C30 P2 C36 111.4(3) . . ? C42 P2 C48 110.4(3) . . ? C30 P2 C48 109.5(3) . . ? C36 P2 C48 108.0(3) . . ? N1 O1 Ce 102.2(5) . . ? N1 O2 Ce 97.8(5) . . ? N2 O3 Ce 106.2(6) . . ? N2 O4 Ce 102.1(6) . . ? N3 O5 Ce 98.9(3) . . ? N3 O6 Ce 100.7(4) . . ? N4 O7 Ce 101.5(6) . . ? N4 O8 Ce 102.5(5) . . ? N5A O9A Ce 100.6(7) . . ? N5B O9B Ce 100.1(8) . . ? N5B O10 N5A 62.0(11) . . ? N5B O10 Ce 98.2(6) . . ? N5A O10 Ce 100.4(6) . . ? O2 N1 O1 113.6(6) . . ? O3 N2 O4 106.3(8) . . ? O5 N3 O6 113.4(5) . . ? O7 N4 O8 111.2(7) . . ? O10 N5A O9A 111.9(10) . . ? O9B N5B O10 114.0(10) . . ? C1 N6 C5 117.9(7) . . ? C1 N6 Ce 122.0(5) . . ? C5 N6 Ce 120.0(6) . . ? N6 C1 C2 122.3(9) . . ? N6 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 117.2(11) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? C4 C3 C2 120.4(10) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.1(13) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N6 C5 C4 123.0(12) . . ? N6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C7 C6 C11 119.6(6) . . ? C7 C6 P1 120.9(5) . . ? C11 C6 P1 119.3(5) . . ? C8 C7 C6 120.4(6) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 119.8(7) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.8(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C6 119.1(6) . . ? C10 C11 H11 120.4 . . ? C6 C11 H11 120.4 . . ? C17 C12 C13 119.2(6) . . ? C17 C12 P1 119.2(5) . . ? C13 C12 P1 121.6(5) . . ? C14 C13 C12 119.1(7) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 120.7(7) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 120.5(7) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.9(7) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 120.5(7) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 119.7(6) . . ? C23 C18 P1 120.7(5) . . ? C19 C18 P1 119.7(5) . . ? C20 C19 C18 119.6(7) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.6(7) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 120.1(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.6(7) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 119.5(6) . . ? C22 C23 H23 120.2 . . ? C18 C23 H23 120.2 . . ? C29 C24 C25 120.1(6) . . ? C29 C24 P1 121.3(5) . . ? C25 C24 P1 118.5(5) . . ? C26 C25 C24 120.1(6) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 119.4(6) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C28 C27 C26 121.1(6) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.5(7) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C24 C29 C28 118.8(6) . . ? C24 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C31 C30 C35 119.9(6) . . ? C31 C30 P2 120.9(5) . . ? C35 C30 P2 119.1(5) . . ? C30 C31 C32 119.2(6) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 120.2(7) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.7(6) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.7(6) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C30 120.4(6) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? C41 C36 C37 120.3(5) . . ? C41 C36 P2 120.8(5) . . ? C37 C36 P2 119.0(5) . . ? C38 C37 C36 119.8(6) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C39 C38 C37 119.7(7) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 121.0(6) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 119.6(6) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C36 C41 C40 119.6(6) . . ? C36 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C47 C42 C43 119.7(5) . . ? C47 C42 P2 121.7(4) . . ? C43 C42 P2 118.5(5) . . ? C44 C43 C42 119.1(6) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C45 C44 C43 120.6(6) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 120.3(6) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 120.5(6) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C46 C47 C42 119.8(6) . . ? C46 C47 H47 120.1 . . ? C42 C47 H47 120.1 . . ? C49 C48 C53 120.4(5) . . ? C49 C48 P2 120.9(4) . . ? C53 C48 P2 118.7(4) . . ? C50 C49 C48 119.0(5) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C51 C50 C49 120.6(6) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C52 C51 C50 120.8(6) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 120.2(6) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C52 C53 C48 118.9(6) . . ? C52 C53 H53 120.5 . . ? C48 C53 H53 120.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 963096' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 Ag Ce N8 O12 P2' _chemical_formula_weight 1360.99 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3567(5) _cell_length_b 16.1781(9) _cell_length_c 17.3706(6) _cell_angle_alpha 97.503(4) _cell_angle_beta 97.694(4) _cell_angle_gamma 98.777(3) _cell_volume 2816.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 141359 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1370 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method '2 \f and 14 \w scans with 2\% steps (751 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 141359 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_unetI/netI 0.0905 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.68 _reflns_number_total 10682 _reflns_number_gt 7439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The Ag atom is disordered over two positions which were refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0609P)^2^] 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 10682 _refine_ls_number_parameters 749 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.390 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.120 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 Ce Ce 0.24853(3) 0.244593(17) 0.269575(17) 0.03578(11) Uani 1 1 d . . . Ag1 Ag 0.6916(2) 0.27355(9) 0.25584(9) 0.0503(4) Uani 0.868(12) 1 d P . . Ag2 Ag 0.752(4) 0.2652(14) 0.2625(6) 0.113(8) Uani 0.132(12) 1 d P . . P1 P 0.54754(11) 0.30180(7) 0.85853(7) 0.0289(3) Uani 1 1 d . . . P2 P 0.95842(11) 0.18483(7) 0.66498(7) 0.0288(3) Uani 1 1 d . . . O1 O 0.3763(4) 0.2813(3) 0.4159(2) 0.0611(11) Uani 1 1 d . . . O2 O 0.2860(5) 0.3779(2) 0.3762(3) 0.0673(12) Uani 1 1 d . . . O3 O 0.0334(4) 0.3088(3) 0.2426(3) 0.0592(11) Uani 1 1 d . . . O4 O 0.1927(4) 0.3767(2) 0.2035(2) 0.0593(11) Uani 1 1 d . . . O5 O 0.1511(6) 0.2044(4) 0.1148(4) 0.113(2) Uani 1 1 d . . . O6 O 0.2768(6) 0.1311(3) 0.1469(3) 0.0941(16) Uani 1 1 d . . . O7 O 0.2936(4) 0.1044(2) 0.3266(2) 0.0480(9) Uani 1 1 d . . . O8 O 0.4606(4) 0.1694(3) 0.2912(3) 0.0628(12) Uani 1 1 d . . . O9 O 0.0826(5) 0.2138(3) 0.3680(3) 0.0743(14) Uani 1 1 d . . . O10 O 0.0372(4) 0.1302(3) 0.2628(4) 0.0774(15) Uani 1 1 d . . . O11 O 0.4588(4) 0.3175(2) 0.2314(2) 0.0542(10) Uani 1 1 d . . . O12 O 0.6025(4) 0.4005(2) 0.1919(2) 0.0574(11) Uani 1 1 d . . . N1 N 0.3474(6) 0.3542(3) 0.4326(3) 0.0673(15) Uani 1 1 d . . . N2 N 0.0734(5) 0.3696(3) 0.2084(3) 0.0517(12) Uani 1 1 d . . . N3 N 0.2128(7) 0.1494(5) 0.0888(5) 0.099(3) Uani 1 1 d . . . N4 N 0.4143(4) 0.1081(3) 0.3201(3) 0.0428(11) Uani 1 1 d . . . N5 N -0.0016(6) 0.1508(4) 0.3239(5) 0.0777(19) Uani 1 1 d . . . N6 N 0.4846(5) 0.3824(3) 0.2003(3) 0.0520(12) Uani 1 1 d . . . N7 N 0.7573(5) 0.3507(3) 0.3711(3) 0.0458(11) Uani 1 1 d . . . N8 N 0.6930(4) 0.1854(3) 0.1499(3) 0.0412(10) Uani 1 1 d . . . C1 C 0.6793(6) 0.4048(3) 0.3961(4) 0.0501(14) Uani 1 1 d . . . H1 H 0.5998 0.4054 0.3644 0.060 Uiso 1 1 calc R . . C2 C 0.7116(6) 0.4594(4) 0.4666(3) 0.0489(14) Uani 1 1 d . . . H2 H 0.6570 0.4974 0.4809 0.059 Uiso 1 1 calc R . . C3 C 0.8269(6) 0.4560(4) 0.5149(3) 0.0513(14) Uani 1 1 d . . . H3 H 0.8495 0.4907 0.5635 0.062 Uiso 1 1 calc R . . C4 C 0.9079(6) 0.4016(4) 0.4914(3) 0.0531(15) Uani 1 1 d . . . H4 H 0.9864 0.3995 0.5234 0.064 Uiso 1 1 calc R . . C5 C 0.8718(6) 0.3495(3) 0.4190(4) 0.0516(15) Uani 1 1 d . . . H5 H 0.9274 0.3129 0.4029 0.062 Uiso 1 1 calc R . . C6 C 0.5817(5) 0.1606(3) 0.0986(3) 0.0450(13) Uani 1 1 d . . . H6 H 0.5063 0.1819 0.1089 0.054 Uiso 1 1 calc R . . C7 C 0.5747(6) 0.1041(4) 0.0301(4) 0.0552(16) Uani 1 1 d . . . H7 H 0.4959 0.0885 -0.0050 0.066 Uiso 1 1 calc R . . C8 C 0.6837(7) 0.0718(4) 0.0148(4) 0.0623(17) Uani 1 1 d . . . H8 H 0.6814 0.0333 -0.0303 0.075 Uiso 1 1 calc R . . C9 C 0.7992(7) 0.0986(4) 0.0693(4) 0.0589(16) Uani 1 1 d . . . H9 H 0.8762 0.0782 0.0609 0.071 Uiso 1 1 calc R . . C10 C 0.7984(6) 0.1546(4) 0.1346(3) 0.0487(14) Uani 1 1 d . . . H10 H 0.8764 0.1719 0.1702 0.058 Uiso 1 1 calc R . . C11 C 0.4338(4) 0.3520(3) 0.9108(3) 0.0305(10) Uani 1 1 d . . . C12 C 0.3884(5) 0.3190(3) 0.9745(3) 0.0385(12) Uani 1 1 d . . . H12 H 0.4069 0.2670 0.9859 0.046 Uiso 1 1 calc R . . C13 C 0.3159(5) 0.3638(3) 1.0203(3) 0.0431(13) Uani 1 1 d . . . H13 H 0.2858 0.3425 1.0631 0.052 Uiso 1 1 calc R . . C14 C 0.2880(5) 0.4408(3) 1.0023(3) 0.0452(13) Uani 1 1 d . . . H14 H 0.2402 0.4713 1.0338 0.054 Uiso 1 1 calc R . . C15 C 0.3298(5) 0.4726(3) 0.9387(4) 0.0463(14) Uani 1 1 d . . . H15 H 0.3087 0.5237 0.9266 0.056 Uiso 1 1 calc R . . C16 C 0.4029(5) 0.4287(3) 0.8928(3) 0.0365(11) Uani 1 1 d . . . H16 H 0.4317 0.4502 0.8498 0.044 Uiso 1 1 calc R . . C17 C 0.5496(4) 0.3368(3) 0.7647(3) 0.0300(10) Uani 1 1 d . . . C18 C 0.4907(5) 0.2819(3) 0.6968(3) 0.0359(11) Uani 1 1 d . . . H18 H 0.4562 0.2261 0.6999 0.043 Uiso 1 1 calc R . . C19 C 0.4825(5) 0.3098(3) 0.6233(3) 0.0408(12) Uani 1 1 d . . . H19 H 0.4416 0.2733 0.5778 0.049 Uiso 1 1 calc R . . C20 C 0.5362(5) 0.3923(3) 0.6200(3) 0.0433(13) Uani 1 1 d . . . H20 H 0.5313 0.4115 0.5717 0.052 Uiso 1 1 calc R . . C21 C 0.5974(5) 0.4472(3) 0.6874(3) 0.0423(13) Uani 1 1 d . . . H21 H 0.6345 0.5024 0.6837 0.051 Uiso 1 1 calc R . . C22 C 0.6039(5) 0.4209(3) 0.7596(3) 0.0368(12) Uani 1 1 d . . . H22 H 0.6437 0.4583 0.8047 0.044 Uiso 1 1 calc R . . C23 C 0.7083(4) 0.3297(3) 0.9177(3) 0.0292(10) Uani 1 1 d . . . C24 C 0.7203(5) 0.3185(3) 0.9968(3) 0.0363(12) Uani 1 1 d . . . H24 H 0.6463 0.2960 1.0170 0.044 Uiso 1 1 calc R . . C25 C 0.8414(5) 0.3410(3) 1.0449(3) 0.0380(12) Uani 1 1 d . . . H25 H 0.8485 0.3334 1.0974 0.046 Uiso 1 1 calc R . . C26 C 0.9519(5) 0.3744(3) 1.0156(3) 0.0423(13) Uani 1 1 d . . . H26 H 1.0332 0.3896 1.0484 0.051 Uiso 1 1 calc R . . C27 C 0.9421(5) 0.3855(4) 0.9378(3) 0.0482(14) Uani 1 1 d . . . H27 H 1.0167 0.4088 0.9184 0.058 Uiso 1 1 calc R . . C28 C 0.8204(5) 0.3618(3) 0.8876(3) 0.0416(12) Uani 1 1 d . . . H28 H 0.8146 0.3676 0.8348 0.050 Uiso 1 1 calc R . . C29 C 0.4983(4) 0.1893(3) 0.8421(3) 0.0297(10) Uani 1 1 d . . . C30 C 0.3649(5) 0.1538(3) 0.8299(3) 0.0382(12) Uani 1 1 d . . . H30 H 0.3018 0.1883 0.8360 0.046 Uiso 1 1 calc R . . C31 C 0.3261(5) 0.0675(3) 0.8087(3) 0.0441(13) Uani 1 1 d . . . H31 H 0.2369 0.0437 0.8007 0.053 Uiso 1 1 calc R . . C32 C 0.4208(5) 0.0160(3) 0.7992(3) 0.0398(12) Uani 1 1 d . . . H32 H 0.3947 -0.0421 0.7839 0.048 Uiso 1 1 calc R . . C33 C 0.5537(5) 0.0512(3) 0.8124(3) 0.0367(12) Uani 1 1 d . . . H33 H 0.6170 0.0168 0.8065 0.044 Uiso 1 1 calc R . . C34 C 0.5921(5) 0.1378(3) 0.8344(3) 0.0322(11) Uani 1 1 d . . . H34 H 0.6815 0.1614 0.8441 0.039 Uiso 1 1 calc R . . C35 C 0.7950(4) 0.1612(3) 0.6095(3) 0.0305(10) Uani 1 1 d . . . C36 C 0.6871(5) 0.1171(3) 0.6346(3) 0.0368(11) Uani 1 1 d . . . H36 H 0.6960 0.1006 0.6841 0.044 Uiso 1 1 calc R . . C37 C 0.5650(5) 0.0976(3) 0.5854(3) 0.0394(12) Uani 1 1 d . . . H37 H 0.4930 0.0669 0.6019 0.047 Uiso 1 1 calc R . . C38 C 0.5497(5) 0.1234(3) 0.5122(3) 0.0382(12) Uani 1 1 d . . . H38 H 0.4680 0.1100 0.4798 0.046 Uiso 1 1 calc R . . C39 C 0.6558(5) 0.1689(3) 0.4875(3) 0.0386(12) Uani 1 1 d . . . H39 H 0.6449 0.1877 0.4390 0.046 Uiso 1 1 calc R . . C40 C 0.7794(5) 0.1870(3) 0.5349(3) 0.0374(12) Uani 1 1 d . . . H40 H 0.8516 0.2162 0.5173 0.045 Uiso 1 1 calc R . . C41 C 1.0139(4) 0.2972(3) 0.6778(3) 0.0326(11) Uani 1 1 d . . . C42 C 0.9227(5) 0.3510(3) 0.6892(3) 0.0335(11) Uani 1 1 d . . . H42 H 0.8329 0.3291 0.6824 0.040 Uiso 1 1 calc R . . C43 C 0.9666(5) 0.4366(3) 0.7104(3) 0.0407(12) Uani 1 1 d . . . H43 H 0.9058 0.4723 0.7189 0.049 Uiso 1 1 calc R . . C44 C 1.0986(5) 0.4702(3) 0.7191(3) 0.0444(13) Uani 1 1 d . . . H44 H 1.1269 0.5282 0.7336 0.053 Uiso 1 1 calc R . . C45 C 1.1894(5) 0.4176(3) 0.7063(3) 0.0484(14) Uani 1 1 d . . . H45 H 1.2787 0.4404 0.7113 0.058 Uiso 1 1 calc R . . C46 C 1.1480(5) 0.3311(3) 0.6860(3) 0.0409(12) Uani 1 1 d . . . H46 H 1.2094 0.2958 0.6779 0.049 Uiso 1 1 calc R . . C47 C 1.0666(4) 0.1301(3) 0.6109(3) 0.0325(11) Uani 1 1 d . . . C48 C 1.0917(5) 0.0522(3) 0.6275(3) 0.0408(12) Uani 1 1 d . . . H48 H 1.0596 0.0304 0.6695 0.049 Uiso 1 1 calc R . . C49 C 1.1639(5) 0.0068(3) 0.5822(3) 0.0432(13) Uani 1 1 d . . . H49 H 1.1797 -0.0457 0.5934 0.052 Uiso 1 1 calc R . . C50 C 1.2123(5) 0.0387(3) 0.5207(3) 0.0401(12) Uani 1 1 d . . . H50 H 1.2619 0.0081 0.4906 0.048 Uiso 1 1 calc R . . C51 C 1.1876(5) 0.1173(4) 0.5029(3) 0.0431(13) Uani 1 1 d . . . H51 H 1.2205 0.1389 0.4609 0.052 Uiso 1 1 calc R . . C52 C 1.1145(5) 0.1622(3) 0.5477(3) 0.0389(12) Uani 1 1 d . . . H52 H 1.0970 0.2142 0.5359 0.047 Uiso 1 1 calc R . . C53 C 0.9623(4) 0.1532(3) 0.7605(3) 0.0302(10) Uani 1 1 d . . . C54 C 0.9111(5) 0.0702(3) 0.7682(3) 0.0367(11) Uani 1 1 d . . . H54 H 0.8668 0.0319 0.7247 0.044 Uiso 1 1 calc R . . C55 C 0.9280(5) 0.0460(4) 0.8430(3) 0.0469(14) Uani 1 1 d . . . H55 H 0.8945 -0.0091 0.8490 0.056 Uiso 1 1 calc R . . C56 C 0.9926(5) 0.1019(4) 0.9071(3) 0.0517(15) Uani 1 1 d . . . H56 H 1.0052 0.0843 0.9560 0.062 Uiso 1 1 calc R . . C57 C 1.0396(5) 0.1846(4) 0.8995(3) 0.0473(13) Uani 1 1 d . . . H57 H 1.0809 0.2232 0.9436 0.057 Uiso 1 1 calc R . . C58 C 1.0252(5) 0.2101(3) 0.8262(3) 0.0380(12) Uani 1 1 d . . . H58 H 1.0580 0.2656 0.8210 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.03528(17) 0.03084(17) 0.03953(19) 0.00684(12) 0.00200(12) 0.00268(12) Ag1 0.0730(8) 0.0384(6) 0.0394(5) 0.0042(3) 0.0110(4) 0.0086(5) Ag2 0.157(18) 0.103(7) 0.046(3) 0.015(4) 0.002(6) -0.067(9) P1 0.0292(6) 0.0281(6) 0.0300(7) 0.0049(5) 0.0053(5) 0.0058(5) P2 0.0251(6) 0.0284(6) 0.0315(7) 0.0029(5) 0.0039(5) 0.0018(5) O1 0.080(3) 0.059(3) 0.042(2) 0.004(2) -0.001(2) 0.015(2) O2 0.117(4) 0.036(2) 0.049(3) 0.0072(19) 0.018(3) 0.010(2) O3 0.052(2) 0.061(3) 0.068(3) 0.020(2) 0.002(2) 0.016(2) O4 0.062(3) 0.054(3) 0.064(3) 0.018(2) 0.006(2) 0.013(2) O5 0.108(5) 0.127(5) 0.089(4) -0.017(4) -0.007(4) 0.029(4) O6 0.105(4) 0.080(4) 0.091(4) 0.000(3) 0.021(3) 0.002(3) O7 0.046(2) 0.044(2) 0.056(3) 0.0128(18) 0.0083(18) 0.0096(17) O8 0.058(3) 0.059(3) 0.085(3) 0.031(2) 0.029(2) 0.020(2) O9 0.069(3) 0.090(4) 0.083(4) 0.046(3) 0.029(3) 0.033(3) O10 0.049(3) 0.054(3) 0.126(5) 0.026(3) -0.002(3) 0.003(2) O11 0.049(2) 0.050(2) 0.064(3) 0.020(2) 0.012(2) -0.0013(18) O12 0.056(3) 0.049(2) 0.069(3) 0.029(2) 0.009(2) -0.0014(19) N1 0.109(5) 0.041(3) 0.048(3) 0.001(2) -0.002(3) 0.017(3) N2 0.051(3) 0.048(3) 0.057(3) 0.014(2) 0.001(2) 0.016(2) N3 0.091(5) 0.097(5) 0.121(6) 0.067(5) -0.016(4) 0.038(4) N4 0.045(3) 0.045(3) 0.040(3) 0.009(2) 0.009(2) 0.013(2) N5 0.059(4) 0.075(5) 0.107(6) 0.044(4) 0.016(4) 0.007(3) N6 0.057(3) 0.040(3) 0.055(3) 0.016(2) 0.002(2) -0.004(2) N7 0.058(3) 0.041(3) 0.038(3) 0.009(2) 0.013(2) -0.002(2) N8 0.041(3) 0.035(2) 0.046(3) 0.012(2) 0.006(2) 0.000(2) C1 0.047(3) 0.050(3) 0.054(4) 0.007(3) 0.013(3) 0.004(3) C2 0.054(3) 0.055(4) 0.041(3) 0.012(3) 0.016(3) 0.008(3) C3 0.064(4) 0.049(3) 0.037(3) 0.007(3) 0.011(3) -0.003(3) C4 0.059(4) 0.048(4) 0.048(4) 0.013(3) 0.000(3) -0.004(3) C5 0.058(4) 0.040(3) 0.062(4) 0.019(3) 0.017(3) 0.009(3) C6 0.050(3) 0.043(3) 0.049(4) 0.024(3) 0.014(3) 0.010(3) C7 0.061(4) 0.044(3) 0.051(4) 0.017(3) -0.012(3) -0.010(3) C8 0.100(5) 0.053(4) 0.041(4) 0.012(3) 0.023(4) 0.020(4) C9 0.068(4) 0.066(4) 0.053(4) 0.022(3) 0.021(3) 0.022(3) C10 0.046(3) 0.051(4) 0.048(4) 0.015(3) 0.005(3) 0.001(3) C11 0.025(2) 0.033(3) 0.032(3) 0.003(2) 0.003(2) 0.004(2) C12 0.035(3) 0.044(3) 0.037(3) 0.008(2) 0.002(2) 0.011(2) C13 0.033(3) 0.058(4) 0.034(3) 0.002(3) 0.007(2) -0.001(2) C14 0.029(3) 0.045(3) 0.055(4) -0.012(3) 0.010(2) 0.002(2) C15 0.037(3) 0.033(3) 0.068(4) -0.001(3) 0.012(3) 0.008(2) C16 0.033(3) 0.031(3) 0.045(3) 0.004(2) 0.008(2) 0.006(2) C17 0.028(2) 0.026(2) 0.037(3) 0.005(2) 0.007(2) 0.0054(19) C18 0.035(3) 0.033(3) 0.041(3) 0.006(2) 0.007(2) 0.008(2) C19 0.045(3) 0.048(3) 0.031(3) 0.006(2) 0.009(2) 0.009(2) C20 0.042(3) 0.054(3) 0.041(3) 0.018(3) 0.014(2) 0.013(3) C21 0.036(3) 0.041(3) 0.055(4) 0.021(3) 0.015(3) 0.006(2) C22 0.035(3) 0.030(3) 0.047(3) 0.011(2) 0.009(2) 0.002(2) C23 0.030(2) 0.024(2) 0.032(3) 0.001(2) 0.004(2) 0.0047(19) C24 0.035(3) 0.028(3) 0.045(3) 0.013(2) 0.002(2) -0.002(2) C25 0.043(3) 0.032(3) 0.038(3) 0.010(2) -0.003(2) 0.003(2) C26 0.032(3) 0.040(3) 0.052(4) 0.003(3) -0.001(2) 0.007(2) C27 0.029(3) 0.059(4) 0.057(4) 0.006(3) 0.013(3) 0.005(2) C28 0.033(3) 0.054(3) 0.039(3) 0.005(2) 0.011(2) 0.007(2) C29 0.034(3) 0.028(2) 0.028(3) 0.005(2) 0.010(2) 0.002(2) C30 0.033(3) 0.038(3) 0.043(3) 0.010(2) 0.004(2) 0.002(2) C31 0.042(3) 0.041(3) 0.045(3) 0.010(3) 0.002(2) -0.005(2) C32 0.054(3) 0.026(3) 0.036(3) 0.004(2) 0.005(2) -0.001(2) C33 0.046(3) 0.033(3) 0.035(3) 0.008(2) 0.012(2) 0.013(2) C34 0.033(3) 0.033(3) 0.032(3) 0.006(2) 0.009(2) 0.003(2) C35 0.034(3) 0.021(2) 0.034(3) -0.002(2) 0.004(2) 0.0052(19) C36 0.033(3) 0.048(3) 0.032(3) 0.007(2) 0.010(2) 0.008(2) C37 0.026(3) 0.047(3) 0.043(3) 0.002(2) 0.010(2) 0.000(2) C38 0.028(3) 0.040(3) 0.043(3) 0.003(2) -0.004(2) 0.005(2) C39 0.040(3) 0.038(3) 0.037(3) 0.010(2) 0.000(2) 0.005(2) C40 0.039(3) 0.029(3) 0.045(3) 0.012(2) 0.006(2) 0.001(2) C41 0.032(3) 0.034(3) 0.031(3) 0.008(2) 0.006(2) 0.000(2) C42 0.030(2) 0.038(3) 0.033(3) 0.005(2) 0.005(2) 0.005(2) C43 0.046(3) 0.033(3) 0.045(3) 0.004(2) 0.013(2) 0.006(2) C44 0.053(3) 0.030(3) 0.045(3) 0.002(2) 0.005(3) -0.006(2) C45 0.037(3) 0.044(3) 0.057(4) 0.007(3) 0.003(3) -0.011(2) C46 0.030(3) 0.039(3) 0.052(3) 0.005(2) 0.007(2) 0.000(2) C47 0.029(2) 0.036(3) 0.031(3) 0.000(2) 0.004(2) 0.005(2) C48 0.037(3) 0.035(3) 0.051(3) 0.004(2) 0.013(2) 0.007(2) C49 0.042(3) 0.038(3) 0.052(4) 0.005(3) 0.014(3) 0.010(2) C50 0.029(3) 0.044(3) 0.043(3) -0.007(2) 0.006(2) 0.004(2) C51 0.034(3) 0.065(4) 0.033(3) 0.010(3) 0.009(2) 0.010(3) C52 0.038(3) 0.038(3) 0.042(3) 0.009(2) 0.007(2) 0.007(2) C53 0.025(2) 0.034(3) 0.031(3) 0.002(2) 0.006(2) 0.006(2) C54 0.030(3) 0.039(3) 0.042(3) 0.006(2) 0.010(2) 0.005(2) C55 0.044(3) 0.053(3) 0.053(4) 0.024(3) 0.018(3) 0.012(3) C56 0.044(3) 0.080(5) 0.041(3) 0.023(3) 0.013(3) 0.023(3) C57 0.049(3) 0.055(4) 0.036(3) 0.002(3) 0.004(3) 0.013(3) C58 0.034(3) 0.042(3) 0.038(3) 0.002(2) 0.008(2) 0.007(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 Ce O11 2.526(4) . ? Ce O2 2.596(4) . ? Ce O3 2.611(4) . ? Ce O10 2.621(5) . ? Ce O9 2.622(4) . ? Ce O1 2.651(4) . ? Ce O4 2.658(4) . ? Ce O7 2.670(3) . ? Ce O8 2.676(4) . ? Ce O5 2.700(6) . ? Ce O6 2.704(5) . ? Ag1 N7 2.180(5) . ? Ag1 N8 2.180(5) . ? Ag1 O11 2.613(4) . ? Ag1 O12 2.684(4) . ? Ag2 N8 2.157(11) . ? Ag2 N7 2.18(2) . ? P1 C29 1.788(5) . ? P1 C23 1.795(5) . ? P1 C17 1.796(5) . ? P1 C11 1.805(5) . ? P2 C35 1.792(5) . ? P2 C41 1.797(5) . ? P2 C53 1.797(5) . ? P2 C47 1.814(5) . ? O1 N1 1.267(6) . ? O2 N1 1.233(6) . ? O3 N2 1.260(6) . ? O4 N2 1.239(6) . ? O5 N3 1.245(8) . ? O6 N3 1.227(7) . ? O7 N4 1.262(5) . ? O8 N4 1.231(5) . ? O9 N5 1.316(8) . ? O10 N5 1.209(8) . ? O11 N6 1.251(5) . ? O12 N6 1.244(6) . ? N7 C1 1.348(7) . ? N7 C5 1.359(7) . ? N8 C10 1.311(7) . ? N8 C6 1.331(7) . ? C1 C2 1.381(8) . ? C1 H1 0.9300 . ? C2 C3 1.377(8) . ? C2 H2 0.9300 . ? C3 C4 1.367(8) . ? C3 H3 0.9300 . ? C4 C5 1.390(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.389(8) . ? C6 H6 0.9300 . ? C7 C8 1.357(9) . ? C7 H7 0.9300 . ? C8 C9 1.395(9) . ? C8 H8 0.9300 . ? C9 C10 1.358(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.390(6) . ? C11 C12 1.396(7) . ? C12 C13 1.377(7) . ? C12 H12 0.9300 . ? C13 C14 1.385(7) . ? C13 H13 0.9300 . ? C14 C15 1.371(8) . ? C14 H14 0.9300 . ? C15 C16 1.375(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.386(7) . ? C17 C22 1.410(6) . ? C18 C19 1.405(7) . ? C18 H18 0.9300 . ? C19 C20 1.377(7) . ? C19 H19 0.9300 . ? C20 C21 1.386(8) . ? C20 H20 0.9300 . ? C21 C22 1.371(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C28 1.393(6) . ? C23 C24 1.401(6) . ? C24 C25 1.380(6) . ? C24 H24 0.9300 . ? C25 C26 1.378(7) . ? C25 H25 0.9300 . ? C26 C27 1.380(7) . ? C26 H26 0.9300 . ? C27 C28 1.402(7) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.381(6) . ? C29 C30 1.389(6) . ? C30 C31 1.379(7) . ? C30 H30 0.9300 . ? C31 C32 1.393(7) . ? C31 H31 0.9300 . ? C32 C33 1.383(7) . ? C32 H32 0.9300 . ? C33 C34 1.385(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.384(6) . ? C35 C40 1.410(7) . ? C36 C37 1.396(7) . ? C36 H36 0.9300 . ? C37 C38 1.386(7) . ? C37 H37 0.9300 . ? C38 C39 1.376(7) . ? C38 H38 0.9300 . ? C39 C40 1.394(7) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C46 1.394(6) . ? C41 C42 1.394(6) . ? C42 C43 1.374(7) . ? C42 H42 0.9300 . ? C43 C44 1.373(7) . ? C43 H43 0.9300 . ? C44 C45 1.382(7) . ? C44 H44 0.9300 . ? C45 C46 1.383(7) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.384(6) . ? C47 C52 1.391(7) . ? C48 C49 1.375(7) . ? C48 H48 0.9300 . ? C49 C50 1.366(7) . ? C49 H49 0.9300 . ? C50 C51 1.400(7) . ? C50 H50 0.9300 . ? C51 C52 1.374(7) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C58 1.384(7) . ? C53 C54 1.396(6) . ? C54 C55 1.401(7) . ? C54 H54 0.9300 . ? C55 C56 1.363(8) . ? C55 H55 0.9300 . ? C56 C57 1.383(8) . ? C56 H56 0.9300 . ? C57 C58 1.385(7) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Ce O2 83.25(14) . . ? O11 Ce O3 118.62(13) . . ? O2 Ce O3 76.02(14) . . ? O11 Ce O10 158.64(17) . . ? O2 Ce O10 118.05(17) . . ? O3 Ce O10 68.97(13) . . ? O11 Ce O9 153.90(16) . . ? O2 Ce O9 72.96(16) . . ? O3 Ce O9 66.30(13) . . ? O10 Ce O9 46.71(18) . . ? O11 Ce O1 85.73(13) . . ? O2 Ce O1 46.80(13) . . ? O3 Ce O1 115.65(13) . . ? O10 Ce O1 109.63(17) . . ? O9 Ce O1 70.27(15) . . ? O11 Ce O4 72.09(12) . . ? O2 Ce O4 70.23(13) . . ? O3 Ce O4 46.54(13) . . ? O10 Ce O4 111.90(13) . . ? O9 Ce O4 108.44(13) . . ? O1 Ce O4 115.30(13) . . ? O11 Ce O7 109.41(11) . . ? O2 Ce O7 113.76(12) . . ? O3 Ce O7 131.89(12) . . ? O10 Ce O7 65.19(12) . . ? O9 Ce O7 72.07(12) . . ? O1 Ce O7 68.93(12) . . ? O4 Ce O7 175.73(12) . . ? O11 Ce O8 63.37(12) . . ? O2 Ce O8 107.61(15) . . ? O3 Ce O8 176.24(13) . . ? O10 Ce O8 108.01(13) . . ? O9 Ce O8 113.49(12) . . ? O1 Ce O8 67.22(14) . . ? O4 Ce O8 135.20(13) . . ? O7 Ce O8 46.05(11) . . ? O11 Ce O5 87.75(17) . . ? O2 Ce O5 136.66(18) . . ? O3 Ce O5 71.54(17) . . ? O10 Ce O5 75.6(2) . . ? O9 Ce O5 116.91(19) . . ? O1 Ce O5 172.08(16) . . ? O4 Ce O5 66.66(18) . . ? O7 Ce O5 109.23(17) . . ? O8 Ce O5 105.76(17) . . ? O11 Ce O6 79.39(15) . . ? O2 Ce O6 162.63(15) . . ? O3 Ce O6 112.25(16) . . ? O10 Ce O6 79.30(18) . . ? O9 Ce O6 124.12(17) . . ? O1 Ce O6 131.23(16) . . ? O4 Ce O6 103.74(16) . . ? O7 Ce O6 72.89(15) . . ? O8 Ce O6 64.55(17) . . ? O5 Ce O6 42.67(18) . . ? N7 Ag1 N8 160.33(19) . . ? N7 Ag1 O11 96.52(16) . . ? N8 Ag1 O11 103.15(17) . . ? N7 Ag1 O12 93.23(15) . . ? N8 Ag1 O12 100.29(15) . . ? O11 Ag1 O12 46.58(12) . . ? N8 Ag2 N7 165(3) . . ? C29 P1 C23 109.5(2) . . ? C29 P1 C17 108.2(2) . . ? C23 P1 C17 110.9(2) . . ? C29 P1 C11 110.6(2) . . ? C23 P1 C11 107.8(2) . . ? C17 P1 C11 109.8(2) . . ? C35 P2 C41 108.4(2) . . ? C35 P2 C53 111.9(2) . . ? C41 P2 C53 108.3(2) . . ? C35 P2 C47 108.7(2) . . ? C41 P2 C47 110.1(2) . . ? C53 P2 C47 109.4(2) . . ? N1 O1 Ce 98.1(3) . . ? N1 O2 Ce 101.8(3) . . ? N2 O3 Ce 101.2(3) . . ? N2 O4 Ce 99.4(3) . . ? N3 O5 Ce 105.4(5) . . ? N3 O6 Ce 105.8(5) . . ? N4 O7 Ce 99.6(3) . . ? N4 O8 Ce 100.3(3) . . ? N5 O9 Ce 99.4(4) . . ? N5 O10 Ce 102.8(5) . . ? N6 O11 Ce 132.5(3) . . ? N6 O11 Ag1 101.2(3) . . ? Ce O11 Ag1 126.17(15) . . ? N6 O12 Ag1 97.9(3) . . ? O2 N1 O1 113.0(5) . . ? O4 N2 O3 112.8(4) . . ? O6 N3 O5 105.4(8) . . ? O8 N4 O7 114.0(4) . . ? O10 N5 O9 110.8(6) . . ? O12 N6 O11 114.3(4) . . ? C1 N7 C5 117.5(5) . . ? C1 N7 Ag1 117.5(4) . . ? C5 N7 Ag1 125.0(4) . . ? C1 N7 Ag2 134.5(13) . . ? C5 N7 Ag2 107.8(13) . . ? C10 N8 C6 118.2(5) . . ? C10 N8 Ag2 105.5(14) . . ? C6 N8 Ag2 136.2(14) . . ? C10 N8 Ag1 122.9(4) . . ? C6 N8 Ag1 118.8(4) . . ? N7 C1 C2 123.3(5) . . ? N7 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.3(5) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C4 C3 C2 119.8(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.4(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N7 C5 C4 121.7(5) . . ? N7 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? N8 C6 C7 122.1(5) . . ? N8 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C8 C7 C6 119.5(6) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 117.4(6) . . ? C7 C8 H8 121.3 . . ? C9 C8 H8 121.3 . . ? C10 C9 C8 119.6(6) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N8 C10 C9 123.1(6) . . ? N8 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C16 C11 C12 119.9(4) . . ? C16 C11 P1 119.6(4) . . ? C12 C11 P1 120.1(3) . . ? C13 C12 C11 119.6(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 119.7(5) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.9(5) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.0(5) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C18 C17 C22 119.5(4) . . ? C18 C17 P1 119.6(3) . . ? C22 C17 P1 120.8(4) . . ? C17 C18 C19 120.6(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 118.7(5) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 121.1(5) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 120.6(5) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C17 119.5(5) . . ? C21 C22 H22 120.3 . . ? C17 C22 H22 120.3 . . ? C28 C23 C24 119.3(4) . . ? C28 C23 P1 122.4(4) . . ? C24 C23 P1 118.3(3) . . ? C25 C24 C23 120.3(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 120.4(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.1(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 120.4(5) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C23 C28 C27 119.5(5) . . ? C23 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C34 C29 C30 119.9(4) . . ? C34 C29 P1 119.8(3) . . ? C30 C29 P1 120.0(3) . . ? C31 C30 C29 120.0(5) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 119.9(5) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0(5) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 119.8(4) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C29 C34 C33 120.3(4) . . ? C29 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C36 C35 C40 119.4(4) . . ? C36 C35 P2 123.9(4) . . ? C40 C35 P2 116.7(4) . . ? C35 C36 C37 119.8(5) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 120.7(5) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 119.9(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.2(5) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C35 119.9(5) . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? C46 C41 C42 119.6(4) . . ? C46 C41 P2 121.0(4) . . ? C42 C41 P2 118.9(3) . . ? C43 C42 C41 119.5(4) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 121.0(5) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C43 C44 C45 119.8(5) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C46 120.3(5) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 119.7(5) . . ? C45 C46 H46 120.2 . . ? C41 C46 H46 120.2 . . ? C48 C47 C52 119.5(4) . . ? C48 C47 P2 120.0(4) . . ? C52 C47 P2 120.2(4) . . ? C49 C48 C47 120.4(5) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C50 C49 C48 120.2(5) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 120.3(5) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C52 C51 C50 119.5(5) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C47 120.1(5) . . ? C51 C52 H52 119.9 . . ? C47 C52 H52 119.9 . . ? C58 C53 C54 120.1(4) . . ? C58 C53 P2 119.3(4) . . ? C54 C53 P2 120.5(4) . . ? C53 C54 C55 118.5(5) . . ? C53 C54 H54 120.7 . . ? C55 C54 H54 120.7 . . ? C56 C55 C54 121.1(5) . . ? C56 C55 H55 119.4 . . ? C54 C55 H55 119.4 . . ? C55 C56 C57 120.1(5) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C56 C57 C58 119.9(5) . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C53 C58 C57 120.2(5) . . ? C53 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? _database_code_depnum_ccdc_archive 'CCDC 963097' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N6 O10 P2 Pr' _chemical_formula_weight 1128.80 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' Pr Pr -0.2180 2.8214 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 13.2497(4) _cell_length_b 17.9467(6) _cell_length_c 21.7355(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.6330(18) _cell_angle_gamma 90.00 _cell_volume 5133.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 193839 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (482 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 193839 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_unetI/netI 0.0320 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9732 _reflns_number_gt 8308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; The model found for the isomorphous Ce complex was used for the refinement. Two nitrite ions (containing N1 and N5) are badly resolved; one of them (N5) was found to be disordered over two positions sharing one O atom, which were refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths, angles and displacement parameters for several nitrite ions: DFIX 1.24 0.005 N1 O1 DFIX 1.24 0.005 N1 O2 DFIX 2.05 0.005 O1 O2 DFIX 1.24 0.01 N5A O9A DFIX 1.24 0.01 N5A O10 DFIX 2.05 0.01 O9A O10 DFIX 1.24 0.01 N5B O9B DFIX 1.24 0.01 N5B O10 DFIX 2.05 0.01 O9B O10 ISOR 0.005 N1 O4 O7 O8 N5A SIMU .005 .005 3. N1 O1 O2 SIMU .005 .005 3. N2 O3 O4 SIMU .005 .005 3. N3 O5 O6 SIMU .005 .005 3. N4 O7 O8 SIMU .005 .005 3. N5A N5B O9A O9B O10 The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0921P)^2^+21.7720P] 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 9732 _refine_ls_number_parameters 668 _refine_ls_number_restraints 171 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1575 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.310 _refine_diff_density_min -1.660 _refine_diff_density_rms 0.148 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 Pr Pr 0.78794(2) 0.365094(16) 0.236259(13) 0.02554(12) Uani 1 1 d . . . P1 P 0.64461(11) 0.89834(8) 0.10592(6) 0.0307(3) Uani 1 1 d . . . P2 P 0.24050(10) 0.37221(7) 0.05004(6) 0.0250(3) Uani 1 1 d . . . O1 O 0.6931(8) 0.4324(5) 0.3138(4) 0.140(2) Uani 1 1 d DU . . O2 O 0.7367(8) 0.5058(4) 0.2497(4) 0.124(2) Uani 1 1 d DU . . O3 O 0.8201(4) 0.4253(4) 0.1346(3) 0.0854(16) Uani 1 1 d U . . O4 O 0.9486(5) 0.4002(5) 0.1856(4) 0.0980(17) Uani 1 1 d U . . O5 O 0.6099(3) 0.3896(2) 0.1709(2) 0.0387(9) Uani 1 1 d U . . O6 O 0.6826(4) 0.2904(3) 0.1497(2) 0.0589(12) Uani 1 1 d U . . O7 O 0.6272(5) 0.3033(4) 0.2788(3) 0.0845(15) Uani 1 1 d U . . O8 O 0.7614(5) 0.2546(4) 0.3092(3) 0.0801(14) Uani 1 1 d U . . O9A O 0.9212(12) 0.4552(6) 0.2902(7) 0.0808(19) Uani 0.399(7) 1 d PDU . . O9B O 0.8202(7) 0.3838(6) 0.3537(5) 0.0785(18) Uani 0.601(7) 1 d PDU . . O10 O 0.9481(4) 0.3431(3) 0.3131(3) 0.0703(14) Uani 1 1 d DU . . N1 N 0.6896(9) 0.4968(5) 0.2936(5) 0.134(3) Uani 1 1 d DU . . N2 N 0.9087(5) 0.4348(5) 0.1390(4) 0.0791(17) Uani 1 1 d U . . N3 N 0.6077(4) 0.3339(3) 0.1366(3) 0.0479(12) Uani 1 1 d U . . N4 N 0.6685(6) 0.2507(4) 0.3073(3) 0.0673(15) Uani 1 1 d U . . N5A N 0.9775(13) 0.4092(6) 0.3219(8) 0.077(2) Uani 0.399(7) 1 d PDU . . N5B N 0.9132(8) 0.3689(7) 0.3611(5) 0.0783(19) Uani 0.601(7) 1 d PDU . . N6 N 0.8861(4) 0.2425(3) 0.1943(3) 0.0484(14) Uani 1 1 d . . . C1 C 0.9315(5) 0.1922(4) 0.2336(4) 0.0501(17) Uani 1 1 d . . . H1 H 0.9352 0.2010 0.2759 0.060 Uiso 1 1 calc R . . C2 C 0.9734(6) 0.1270(4) 0.2130(6) 0.078(3) Uani 1 1 d . . . H2 H 1.0042 0.0924 0.2409 0.093 Uiso 1 1 calc R . . C3 C 0.9679(10) 0.1153(7) 0.1501(8) 0.113(5) Uani 1 1 d . . . H3 H 0.9953 0.0722 0.1350 0.136 Uiso 1 1 calc R . . C4 C 0.9230(9) 0.1662(8) 0.1101(7) 0.111(5) Uani 1 1 d . . . H4 H 0.9178 0.1583 0.0676 0.133 Uiso 1 1 calc R . . C5 C 0.8850(6) 0.2302(6) 0.1338(4) 0.075(3) Uani 1 1 d . . . H5 H 0.8573 0.2665 0.1063 0.090 Uiso 1 1 calc R . . C6 C 0.5328(5) 0.8652(3) 0.0587(3) 0.0329(12) Uani 1 1 d . . . C7 C 0.4414(5) 0.8573(4) 0.0841(3) 0.0395(14) Uani 1 1 d . . . H7 H 0.4357 0.8738 0.1241 0.047 Uiso 1 1 calc R . . C8 C 0.3594(5) 0.8246(4) 0.0491(3) 0.0452(15) Uani 1 1 d . . . H8 H 0.2988 0.8178 0.0661 0.054 Uiso 1 1 calc R . . C9 C 0.3672(5) 0.8018(4) -0.0115(3) 0.0436(15) Uani 1 1 d . . . H9 H 0.3114 0.7807 -0.0351 0.052 Uiso 1 1 calc R . . C10 C 0.4566(5) 0.8104(4) -0.0363(3) 0.0418(14) Uani 1 1 d . . . H10 H 0.4613 0.7951 -0.0767 0.050 Uiso 1 1 calc R . . C11 C 0.5400(5) 0.8414(4) -0.0018(3) 0.0378(13) Uani 1 1 d . . . H11 H 0.6009 0.8464 -0.0188 0.045 Uiso 1 1 calc R . . C12 C 0.7000(4) 0.8229(3) 0.1524(3) 0.0336(12) Uani 1 1 d . . . C13 C 0.6616(5) 0.7505(3) 0.1448(3) 0.0398(14) Uani 1 1 d . . . H13 H 0.6060 0.7403 0.1158 0.048 Uiso 1 1 calc R . . C14 C 0.7084(6) 0.6941(4) 0.1815(3) 0.0471(16) Uani 1 1 d . . . H14 H 0.6830 0.6458 0.1775 0.056 Uiso 1 1 calc R . . C15 C 0.7914(5) 0.7087(4) 0.2236(3) 0.0480(17) Uani 1 1 d . . . H15 H 0.8224 0.6701 0.2474 0.058 Uiso 1 1 calc R . . C16 C 0.8297(5) 0.7811(4) 0.2309(3) 0.0467(16) Uani 1 1 d . . . H16 H 0.8864 0.7908 0.2592 0.056 Uiso 1 1 calc R . . C17 C 0.7829(5) 0.8378(4) 0.1960(3) 0.0390(13) Uani 1 1 d . . . H17 H 0.8068 0.8864 0.2016 0.047 Uiso 1 1 calc R . . C18 C 0.7318(5) 0.9310(3) 0.0541(3) 0.0343(12) Uani 1 1 d . . . C19 C 0.6985(5) 0.9820(4) 0.0074(3) 0.0421(14) Uani 1 1 d . . . H19 H 0.6325 1.0004 0.0042 0.050 Uiso 1 1 calc R . . C20 C 0.7641(6) 1.0050(4) -0.0339(3) 0.0471(16) Uani 1 1 d . . . H20 H 0.7423 1.0391 -0.0649 0.056 Uiso 1 1 calc R . . C21 C 0.8613(5) 0.9775(4) -0.0291(3) 0.0478(16) Uani 1 1 d . . . H21 H 0.9047 0.9928 -0.0573 0.057 Uiso 1 1 calc R . . C22 C 0.8958(5) 0.9278(4) 0.0166(3) 0.0460(15) Uani 1 1 d . . . H22 H 0.9621 0.9100 0.0193 0.055 Uiso 1 1 calc R . . C23 C 0.8308(5) 0.9041(4) 0.0589(3) 0.0374(13) Uani 1 1 d . . . H23 H 0.8535 0.8705 0.0901 0.045 Uiso 1 1 calc R . . C24 C 0.6167(4) 0.9713(3) 0.1579(3) 0.0328(12) Uani 1 1 d . . . C25 C 0.5669(4) 0.9526(4) 0.2092(3) 0.0369(13) Uani 1 1 d . . . H25 H 0.5486 0.9035 0.2157 0.044 Uiso 1 1 calc R . . C26 C 0.5451(5) 1.0075(4) 0.2502(3) 0.0410(14) Uani 1 1 d . . . H26 H 0.5108 0.9955 0.2839 0.049 Uiso 1 1 calc R . . C27 C 0.5743(5) 1.0805(4) 0.2412(3) 0.0401(14) Uani 1 1 d . . . H27 H 0.5598 1.1172 0.2691 0.048 Uiso 1 1 calc R . . C28 C 0.6243(5) 1.0992(4) 0.1914(3) 0.0423(14) Uani 1 1 d . . . H28 H 0.6434 1.1484 0.1859 0.051 Uiso 1 1 calc R . . C29 C 0.6464(5) 1.0449(3) 0.1493(3) 0.0388(13) Uani 1 1 d . . . H29 H 0.6807 1.0575 0.1157 0.047 Uiso 1 1 calc R . . C30 C 0.1234(4) 0.3488(3) 0.0047(2) 0.0280(11) Uani 1 1 d . . . C31 C 0.0302(5) 0.3714(4) 0.0226(3) 0.0426(15) Uani 1 1 d . . . H31 H 0.0279 0.4022 0.0569 0.051 Uiso 1 1 calc R . . C32 C -0.0586(5) 0.3472(5) -0.0113(3) 0.0540(18) Uani 1 1 d . . . H32 H -0.1210 0.3616 0.0005 0.065 Uiso 1 1 calc R . . C33 C -0.0558(5) 0.3021(4) -0.0624(3) 0.0496(17) Uani 1 1 d . . . H33 H -0.1160 0.2857 -0.0844 0.060 Uiso 1 1 calc R . . C34 C 0.0365(5) 0.2811(4) -0.0808(3) 0.0428(15) Uani 1 1 d . . . H34 H 0.0385 0.2514 -0.1157 0.051 Uiso 1 1 calc R . . C35 C 0.1252(4) 0.3044(3) -0.0475(3) 0.0349(12) Uani 1 1 d . . . H35 H 0.1872 0.2903 -0.0600 0.042 Uiso 1 1 calc R . . C36 C 0.2258(4) 0.4514(3) 0.0985(2) 0.0282(11) Uani 1 1 d . . . C37 C 0.1745(5) 0.4423(3) 0.1505(3) 0.0361(13) Uani 1 1 d . . . H37 H 0.1487 0.3960 0.1597 0.043 Uiso 1 1 calc R . . C38 C 0.1625(5) 0.5034(4) 0.1884(3) 0.0424(14) Uani 1 1 d . . . H38 H 0.1271 0.4983 0.2227 0.051 Uiso 1 1 calc R . . C39 C 0.2027(5) 0.5709(4) 0.1752(3) 0.0443(15) Uani 1 1 d . . . H39 H 0.1956 0.6112 0.2013 0.053 Uiso 1 1 calc R . . C40 C 0.2535(5) 0.5802(3) 0.1238(3) 0.0411(14) Uani 1 1 d . . . H40 H 0.2801 0.6265 0.1153 0.049 Uiso 1 1 calc R . . C41 C 0.2651(4) 0.5201(3) 0.0848(3) 0.0355(13) Uani 1 1 d . . . H41 H 0.2988 0.5261 0.0499 0.043 Uiso 1 1 calc R . . C42 C 0.3327(4) 0.3940(3) -0.0015(2) 0.0283(11) Uani 1 1 d . . . C43 C 0.3032(5) 0.4405(3) -0.0525(3) 0.0340(12) Uani 1 1 d . . . H43 H 0.2364 0.4570 -0.0605 0.041 Uiso 1 1 calc R . . C44 C 0.3752(5) 0.4614(4) -0.0907(3) 0.0419(14) Uani 1 1 d . . . H44 H 0.3571 0.4930 -0.1241 0.050 Uiso 1 1 calc R . . C45 C 0.4738(5) 0.4355(4) -0.0794(3) 0.0452(15) Uani 1 1 d . . . H45 H 0.5213 0.4492 -0.1056 0.054 Uiso 1 1 calc R . . C46 C 0.5023(5) 0.3896(4) -0.0296(3) 0.0426(14) Uani 1 1 d . . . H46 H 0.5688 0.3724 -0.0225 0.051 Uiso 1 1 calc R . . C47 C 0.4324(4) 0.3691(3) 0.0099(3) 0.0322(12) Uani 1 1 d . . . H47 H 0.4520 0.3387 0.0438 0.039 Uiso 1 1 calc R . . C48 C 0.2820(4) 0.2951(3) 0.0988(2) 0.0256(10) Uani 1 1 d . . . C49 C 0.2359(4) 0.2259(3) 0.0905(2) 0.0299(11) Uani 1 1 d . . . H49 H 0.1804 0.2193 0.0607 0.036 Uiso 1 1 calc R . . C50 C 0.2736(5) 0.1662(3) 0.1272(3) 0.0357(13) Uani 1 1 d . . . H50 H 0.2426 0.1198 0.1223 0.043 Uiso 1 1 calc R . . C51 C 0.3569(5) 0.1759(3) 0.1710(3) 0.0378(13) Uani 1 1 d . . . H51 H 0.3828 0.1356 0.1946 0.045 Uiso 1 1 calc R . . C52 C 0.4020(4) 0.2450(4) 0.1798(3) 0.0379(13) Uani 1 1 d . . . H52 H 0.4574 0.2512 0.2097 0.046 Uiso 1 1 calc R . . C53 C 0.3651(4) 0.3051(3) 0.1443(2) 0.0312(12) Uani 1 1 d . . . H53 H 0.3950 0.3518 0.1505 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr 0.02411(18) 0.02705(19) 0.02494(18) -0.00079(11) 0.00053(11) 0.00137(11) P1 0.0329(7) 0.0313(7) 0.0289(7) -0.0007(6) 0.0076(6) 0.0007(6) P2 0.0247(6) 0.0252(7) 0.0246(7) 0.0005(5) 0.0012(5) 0.0005(5) O1 0.169(5) 0.115(4) 0.137(5) -0.006(4) 0.030(4) 0.026(4) O2 0.164(5) 0.091(4) 0.116(5) 0.009(4) 0.010(4) 0.057(4) O3 0.055(3) 0.131(4) 0.071(3) 0.048(3) 0.015(2) -0.002(3) O4 0.068(3) 0.131(4) 0.097(3) 0.041(3) 0.022(2) -0.005(3) O5 0.0332(19) 0.035(2) 0.046(2) 0.0002(17) -0.0025(16) 0.0033(16) O6 0.049(2) 0.061(3) 0.062(2) -0.024(2) -0.015(2) 0.013(2) O7 0.076(3) 0.092(3) 0.084(3) 0.033(2) 0.006(2) -0.011(2) O8 0.075(3) 0.080(3) 0.089(3) 0.040(2) 0.025(2) 0.013(2) O9A 0.084(4) 0.074(4) 0.077(4) -0.016(3) -0.021(3) 0.010(3) O9B 0.085(3) 0.075(3) 0.070(3) -0.015(3) -0.017(3) 0.015(3) O10 0.073(3) 0.066(3) 0.065(3) -0.008(2) -0.024(2) 0.017(2) N1 0.150(4) 0.112(4) 0.140(4) 0.000(4) 0.013(4) 0.031(4) N2 0.052(3) 0.123(4) 0.067(3) 0.034(3) 0.025(3) -0.006(3) N3 0.039(2) 0.053(3) 0.048(3) -0.006(2) -0.010(2) 0.008(2) N4 0.071(3) 0.061(3) 0.072(3) 0.019(3) 0.017(3) 0.001(3) N5A 0.079(3) 0.073(3) 0.072(3) -0.014(3) -0.018(3) 0.012(3) N5B 0.084(4) 0.073(3) 0.070(3) -0.015(3) -0.023(3) 0.017(3) N6 0.033(3) 0.057(4) 0.055(3) -0.024(3) 0.005(2) 0.002(3) C1 0.028(3) 0.036(3) 0.087(5) -0.009(3) 0.009(3) -0.001(3) C2 0.048(5) 0.042(4) 0.150(10) -0.011(5) 0.041(6) 0.000(3) C3 0.090(8) 0.082(8) 0.180(14) -0.068(9) 0.069(9) -0.002(6) C4 0.089(8) 0.128(11) 0.118(10) -0.073(9) 0.022(7) 0.025(8) C5 0.057(5) 0.104(7) 0.066(5) -0.035(5) 0.015(4) 0.019(5) C6 0.036(3) 0.033(3) 0.030(3) -0.003(2) 0.007(2) 0.001(2) C7 0.042(3) 0.048(4) 0.030(3) -0.002(3) 0.008(3) -0.003(3) C8 0.038(3) 0.051(4) 0.047(4) -0.001(3) 0.004(3) -0.005(3) C9 0.048(4) 0.041(4) 0.039(3) -0.002(3) -0.007(3) 0.000(3) C10 0.053(4) 0.041(3) 0.031(3) -0.005(3) 0.001(3) 0.009(3) C11 0.044(3) 0.039(3) 0.031(3) -0.002(3) 0.008(2) 0.006(3) C12 0.040(3) 0.031(3) 0.031(3) 0.001(2) 0.009(2) 0.005(2) C13 0.051(4) 0.036(3) 0.034(3) -0.004(2) 0.013(3) 0.001(3) C14 0.070(5) 0.035(3) 0.040(3) 0.002(3) 0.019(3) 0.001(3) C15 0.063(4) 0.046(4) 0.038(3) 0.009(3) 0.019(3) 0.018(3) C16 0.043(4) 0.062(4) 0.037(3) 0.008(3) 0.011(3) 0.012(3) C17 0.042(3) 0.039(3) 0.037(3) -0.002(3) 0.009(3) 0.002(3) C18 0.040(3) 0.032(3) 0.032(3) -0.004(2) 0.008(2) -0.001(2) C19 0.044(3) 0.041(3) 0.043(3) 0.002(3) 0.013(3) 0.001(3) C20 0.060(4) 0.043(4) 0.040(3) 0.001(3) 0.016(3) -0.005(3) C21 0.052(4) 0.051(4) 0.045(4) -0.007(3) 0.022(3) -0.018(3) C22 0.038(3) 0.053(4) 0.049(4) -0.009(3) 0.013(3) -0.009(3) C23 0.038(3) 0.041(3) 0.034(3) -0.005(3) 0.007(2) -0.003(3) C24 0.034(3) 0.035(3) 0.029(3) -0.003(2) 0.001(2) 0.004(2) C25 0.036(3) 0.040(3) 0.035(3) -0.004(3) 0.007(2) -0.003(3) C26 0.037(3) 0.053(4) 0.033(3) -0.007(3) 0.005(2) 0.002(3) C27 0.041(3) 0.041(3) 0.037(3) -0.010(3) -0.004(3) 0.012(3) C28 0.048(4) 0.032(3) 0.045(3) -0.002(3) -0.003(3) 0.007(3) C29 0.043(3) 0.037(3) 0.036(3) 0.003(3) 0.003(3) 0.002(3) C30 0.026(3) 0.030(3) 0.027(3) 0.001(2) 0.001(2) 0.003(2) C31 0.029(3) 0.062(4) 0.036(3) -0.007(3) 0.002(2) 0.005(3) C32 0.027(3) 0.086(5) 0.048(4) -0.008(4) -0.001(3) 0.009(3) C33 0.036(3) 0.069(5) 0.041(3) -0.003(3) -0.008(3) -0.003(3) C34 0.042(3) 0.046(4) 0.037(3) -0.009(3) -0.007(3) 0.001(3) C35 0.034(3) 0.036(3) 0.035(3) -0.005(2) 0.001(2) 0.004(2) C36 0.027(3) 0.028(3) 0.029(3) -0.004(2) 0.000(2) 0.002(2) C37 0.043(3) 0.034(3) 0.031(3) -0.006(2) 0.005(2) 0.001(3) C38 0.049(4) 0.044(4) 0.036(3) -0.011(3) 0.009(3) 0.008(3) C39 0.039(3) 0.042(4) 0.048(4) -0.018(3) -0.007(3) 0.007(3) C40 0.041(3) 0.028(3) 0.054(4) -0.007(3) 0.001(3) -0.004(3) C41 0.035(3) 0.031(3) 0.040(3) -0.004(2) 0.003(2) 0.000(2) C42 0.033(3) 0.028(3) 0.024(2) -0.001(2) 0.003(2) -0.001(2) C43 0.036(3) 0.033(3) 0.032(3) 0.004(2) 0.001(2) -0.002(2) C44 0.050(4) 0.044(4) 0.031(3) 0.009(3) 0.002(3) -0.011(3) C45 0.039(3) 0.059(4) 0.038(3) 0.008(3) 0.006(3) -0.012(3) C46 0.031(3) 0.055(4) 0.043(3) 0.007(3) 0.009(3) 0.000(3) C47 0.032(3) 0.033(3) 0.031(3) 0.005(2) 0.003(2) 0.000(2) C48 0.025(2) 0.030(3) 0.022(2) 0.002(2) 0.0050(19) 0.001(2) C49 0.031(3) 0.030(3) 0.029(3) 0.000(2) 0.003(2) -0.001(2) C50 0.046(3) 0.026(3) 0.036(3) 0.002(2) 0.010(3) 0.002(2) C51 0.043(3) 0.036(3) 0.035(3) 0.011(2) 0.009(2) 0.009(3) C52 0.029(3) 0.051(4) 0.033(3) 0.011(3) 0.002(2) 0.002(3) C53 0.027(3) 0.037(3) 0.029(3) 0.005(2) 0.003(2) 0.000(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 Pr O1 2.524(9) . ? Pr O3 2.539(5) . ? Pr O9B 2.561(10) . ? Pr O9A 2.575(14) . ? Pr O10 2.575(5) . ? Pr O4 2.584(6) . ? Pr O6 2.584(5) . ? Pr O8 2.588(6) . ? Pr O2 2.640(8) . ? Pr O5 2.646(4) . ? Pr O7 2.659(6) . ? Pr N6 2.764(5) . ? P1 C12 1.795(6) . ? P1 C24 1.795(6) . ? P1 C18 1.802(6) . ? P1 C6 1.803(6) . ? P2 C30 1.789(5) . ? P2 C48 1.791(5) . ? P2 C42 1.794(5) . ? P2 C36 1.794(5) . ? O1 N1 1.236(5) . ? O2 N1 1.211(5) . ? O3 N2 1.178(9) . ? O4 N2 1.254(10) . ? O5 N3 1.245(7) . ? O6 N3 1.269(7) . ? O7 N4 1.223(9) . ? O8 N4 1.229(9) . ? O9A N5A 1.262(10) . ? O9B N5B 1.254(9) . ? O10 N5A 1.255(10) . ? O10 N5B 1.276(9) . ? N6 C5 1.332(10) . ? N6 C1 1.337(10) . ? C1 C2 1.390(10) . ? C1 H1 0.9300 . ? C2 C3 1.377(18) . ? C2 H2 0.9300 . ? C3 C4 1.35(2) . ? C3 H3 0.9300 . ? C4 C5 1.378(14) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.394(8) . ? C6 C11 1.397(8) . ? C7 C8 1.383(9) . ? C7 H7 0.9300 . ? C8 C9 1.395(9) . ? C8 H8 0.9300 . ? C9 C10 1.365(9) . ? C9 H9 0.9300 . ? C10 C11 1.378(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.392(9) . ? C12 C13 1.399(9) . ? C13 C14 1.389(9) . ? C13 H13 0.9300 . ? C14 C15 1.373(10) . ? C14 H14 0.9300 . ? C15 C16 1.398(10) . ? C15 H15 0.9300 . ? C16 C17 1.374(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.390(8) . ? C18 C19 1.400(9) . ? C19 C20 1.383(9) . ? C19 H19 0.9300 . ? C20 C21 1.373(10) . ? C20 H20 0.9300 . ? C21 C22 1.373(10) . ? C21 H21 0.9300 . ? C22 C23 1.399(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.397(9) . ? C24 C25 1.401(8) . ? C25 C26 1.382(8) . ? C25 H25 0.9300 . ? C26 C27 1.386(9) . ? C26 H26 0.9300 . ? C27 C28 1.373(9) . ? C27 H27 0.9300 . ? C28 C29 1.393(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.390(8) . ? C30 C31 1.397(8) . ? C31 C32 1.385(9) . ? C31 H31 0.9300 . ? C32 C33 1.378(10) . ? C32 H32 0.9300 . ? C33 C34 1.383(9) . ? C33 H33 0.9300 . ? C34 C35 1.372(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.385(8) . ? C36 C37 1.393(8) . ? C37 C38 1.392(8) . ? C37 H37 0.9300 . ? C38 C39 1.367(10) . ? C38 H38 0.9300 . ? C39 C40 1.380(10) . ? C39 H39 0.9300 . ? C40 C41 1.390(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.389(8) . ? C42 C43 1.407(8) . ? C43 C44 1.387(8) . ? C43 H43 0.9300 . ? C44 C45 1.381(9) . ? C44 H44 0.9300 . ? C45 C46 1.378(9) . ? C45 H45 0.9300 . ? C46 C47 1.383(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.386(8) . ? C48 C53 1.403(7) . ? C49 C50 1.392(8) . ? C49 H49 0.9300 . ? C50 C51 1.382(9) . ? C50 H50 0.9300 . ? C51 C52 1.381(9) . ? C51 H51 0.9300 . ? C52 C53 1.382(8) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pr O3 121.6(3) . . ? O1 Pr O9B 46.4(3) . . ? O3 Pr O9B 141.8(3) . . ? O1 Pr O9A 76.3(5) . . ? O3 Pr O9A 87.3(4) . . ? O9B Pr O9A 55.7(4) . . ? O1 Pr O10 94.4(3) . . ? O3 Pr O10 114.9(2) . . ? O9B Pr O10 48.98(19) . . ? O9A Pr O10 47.9(2) . . ? O1 Pr O4 131.8(3) . . ? O3 Pr O4 45.3(2) . . ? O9B Pr O4 110.0(3) . . ? O9A Pr O4 59.0(4) . . ? O10 Pr O4 69.9(2) . . ? O1 Pr O6 117.8(3) . . ? O3 Pr O6 73.6(2) . . ? O9B Pr O6 143.9(3) . . ? O9A Pr O6 160.3(4) . . ? O10 Pr O6 136.74(17) . . ? O4 Pr O6 102.6(2) . . ? O1 Pr O8 81.0(2) . . ? O3 Pr O8 155.1(3) . . ? O9B Pr O8 60.6(3) . . ? O9A Pr O8 109.7(3) . . ? O10 Pr O8 69.2(2) . . ? O4 Pr O8 128.6(2) . . ? O6 Pr O8 87.1(2) . . ? O1 Pr O2 46.70(14) . . ? O3 Pr O2 76.1(3) . . ? O9B Pr O2 77.3(3) . . ? O9A Pr O2 61.4(3) . . ? O10 Pr O2 106.1(3) . . ? O4 Pr O2 92.8(3) . . ? O6 Pr O2 116.9(2) . . ? O8 Pr O2 127.6(2) . . ? O1 Pr O5 78.3(3) . . ? O3 Pr O5 71.98(17) . . ? O9B Pr O5 123.3(2) . . ? O9A Pr O5 131.4(2) . . ? O10 Pr O5 172.14(16) . . ? O4 Pr O5 117.23(19) . . ? O6 Pr O5 47.34(14) . . ? O8 Pr O5 106.31(18) . . ? O2 Pr O5 71.1(2) . . ? O1 Pr O7 59.2(3) . . ? O3 Pr O7 134.5(2) . . ? O9B Pr O7 75.9(3) . . ? O9A Pr O7 129.7(4) . . ? O10 Pr O7 110.1(2) . . ? O4 Pr O7 168.9(3) . . ? O6 Pr O7 69.5(2) . . ? O8 Pr O7 45.3(2) . . ? O2 Pr O7 97.7(3) . . ? O5 Pr O7 63.67(17) . . ? O1 Pr N6 153.0(2) . . ? O3 Pr N6 85.3(2) . . ? O9B Pr N6 113.8(2) . . ? O9A Pr N6 109.0(3) . . ? O10 Pr N6 73.02(17) . . ? O4 Pr N6 67.1(2) . . ? O6 Pr N6 65.30(15) . . ? O8 Pr N6 72.2(2) . . ? O2 Pr N6 159.2(2) . . ? O5 Pr N6 112.31(15) . . ? O7 Pr N6 102.0(2) . . ? C12 P1 C24 107.2(3) . . ? C12 P1 C18 110.3(3) . . ? C24 P1 C18 110.4(3) . . ? C12 P1 C6 109.1(3) . . ? C24 P1 C6 112.5(3) . . ? C18 P1 C6 107.2(3) . . ? C30 P2 C48 109.4(2) . . ? C30 P2 C42 108.5(2) . . ? C48 P2 C42 110.7(2) . . ? C30 P2 C36 111.3(3) . . ? C48 P2 C36 108.1(2) . . ? C42 P2 C36 108.8(3) . . ? N1 O1 Pr 102.2(5) . . ? N1 O2 Pr 97.0(5) . . ? N2 O3 Pr 105.0(5) . . ? N2 O4 Pr 100.0(5) . . ? N3 O5 Pr 98.4(3) . . ? N3 O6 Pr 100.7(4) . . ? N4 O7 Pr 99.7(5) . . ? N4 O8 Pr 103.3(5) . . ? N5A O9A Pr 99.7(8) . . ? N5B O9B Pr 98.5(6) . . ? N5A O10 N5B 70.7(11) . . ? N5A O10 Pr 99.9(6) . . ? N5B O10 Pr 97.2(5) . . ? O2 N1 O1 113.8(6) . . ? O3 N2 O4 108.4(7) . . ? O5 N3 O6 113.4(5) . . ? O7 N4 O8 111.1(7) . . ? O10 N5A O9A 112.5(10) . . ? O9B N5B O10 114.6(9) . . ? C5 N6 C1 118.2(7) . . ? C5 N6 Pr 120.3(6) . . ? C1 N6 Pr 121.4(5) . . ? N6 C1 C2 121.9(9) . . ? N6 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 118.1(11) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C4 C3 C2 120.3(9) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 118.5(12) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N6 C5 C4 122.9(11) . . ? N6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C7 C6 C11 119.8(6) . . ? C7 C6 P1 120.2(5) . . ? C11 C6 P1 119.7(5) . . ? C8 C7 C6 119.3(6) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 120.3(6) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.6(6) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C6 119.9(6) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C17 C12 C13 120.5(6) . . ? C17 C12 P1 118.5(5) . . ? C13 C12 P1 121.0(5) . . ? C14 C13 C12 118.4(6) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 121.0(6) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C12 120.2(6) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C23 C18 C19 119.8(6) . . ? C23 C18 P1 120.5(5) . . ? C19 C18 P1 119.7(5) . . ? C20 C19 C18 119.9(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 119.8(7) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 121.3(6) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 119.7(6) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C18 C23 C22 119.5(6) . . ? C18 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C29 C24 C25 119.9(5) . . ? C29 C24 P1 121.6(5) . . ? C25 C24 P1 118.5(5) . . ? C26 C25 C24 119.8(6) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.0(6) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.8(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.3(6) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 119.4(6) . . ? C28 C29 H29 120.3 . . ? C24 C29 H29 120.3 . . ? C35 C30 C31 119.6(5) . . ? C35 C30 P2 119.3(4) . . ? C31 C30 P2 121.1(4) . . ? C32 C31 C30 119.0(6) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 120.9(6) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 120.1(6) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 119.7(6) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C30 120.8(6) . . ? C34 C35 H35 119.6 . . ? C30 C35 H35 119.6 . . ? C41 C36 C37 120.6(5) . . ? C41 C36 P2 120.7(4) . . ? C37 C36 P2 118.7(4) . . ? C38 C37 C36 119.2(6) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 120.0(6) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 121.0(6) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C41 119.9(6) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C36 C41 C40 119.3(6) . . ? C36 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C47 C42 C43 120.2(5) . . ? C47 C42 P2 121.4(4) . . ? C43 C42 P2 118.3(4) . . ? C44 C43 C42 119.0(6) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C45 C44 C43 120.3(6) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C46 C45 C44 120.6(6) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 120.2(6) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 C42 119.7(5) . . ? C46 C47 H47 120.2 . . ? C42 C47 H47 120.2 . . ? C49 C48 C53 120.3(5) . . ? C49 C48 P2 121.0(4) . . ? C53 C48 P2 118.7(4) . . ? C48 C49 C50 119.4(5) . . ? C48 C49 H49 120.3 . . ? C50 C49 H49 120.3 . . ? C51 C50 C49 120.2(6) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C52 C51 C50 120.4(5) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C53 120.3(5) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C52 C53 C48 119.4(5) . . ? C52 C53 H53 120.3 . . ? C48 C53 H53 120.3 . . ? _database_code_depnum_ccdc_archive 'CCDC 963098' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 N7 Nd O10 P2' _chemical_formula_weight 1211.23 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' Nd Nd -0.1943 3.0179 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4292(2) _cell_length_b 9.6856(3) _cell_length_c 15.8367(6) _cell_angle_alpha 76.145(2) _cell_angle_beta 75.304(2) _cell_angle_gamma 81.595(2) _cell_volume 1352.68(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 80560 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 617 _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method '2 \f and 14 \w scans with 2\% steps (771 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 80560 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_unetI/netI 0.0426 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8246 _reflns_number_gt 7975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All the nitrite ions, both coordinated and free, and the pyridine ligand, are disordered over two positions (sharing one N atom for one nitrite and one O atom for another one), which have been refined with occupancy parameters constrained to sum to unity (fixed to 0.5 for the free nitrite which is disordered around an inversion centre). This disorder did not disappear if the space group P1 was chosen instead of P-1. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for the free nitrite anion: DFIX 1.24 0.005 N4 O5 DFIX 1.24 0.005 N4 O6 SIMU .005 .005 1.5 N4 O5 O6 The two positions of the pyridine molecule, close to one another, were refined as idealized hexagons. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0430P)^2^+0.3134P] 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 8246 _refine_ls_number_parameters 436 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.765 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.086 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 Nd Nd 0.5000 0.5000 0.5000 0.02363(4) Uani 1 2 d S . . P1 P 0.93971(4) 0.84641(4) 0.86083(3) 0.02168(8) Uani 1 1 d . . . O1A O 0.3438(3) 0.6243(3) 0.61753(19) 0.0431(8) Uani 0.522(3) 1 d P . . O2A O 0.4602(4) 0.4402(3) 0.67077(18) 0.0525(10) Uani 0.522(3) 1 d P . . O1B O 0.3065(3) 0.4871(4) 0.64579(19) 0.0414(8) Uani 0.478(3) 1 d P . . O2B O 0.4968(4) 0.5783(4) 0.6407(2) 0.0511(10) Uani 0.478(3) 1 d P . . O3 O 0.25326(16) 0.60843(15) 0.45544(10) 0.0398(3) Uani 1 1 d . . . O4A O 0.3685(4) 0.7578(3) 0.4786(4) 0.0557(16) Uani 0.471(6) 1 d P . . O4B O 0.4271(4) 0.7397(3) 0.4092(2) 0.0446(11) Uani 0.529(6) 1 d P . . O5 O 0.4502(5) 0.5495(5) 0.9327(4) 0.0613(12) Uani 0.50 1 d PDU . . O6 O 0.5116(7) 0.4251(7) 1.0471(3) 0.0665(15) Uani 0.50 1 d PDU . . N1 N 0.3731(2) 0.54531(19) 0.68572(11) 0.0402(4) Uani 1 1 d . . . N2A N 0.2582(6) 0.7414(6) 0.4515(5) 0.0409(12) Uani 0.471(6) 1 d P . . N2B N 0.2946(6) 0.7245(5) 0.4159(3) 0.0379(9) Uani 0.529(6) 1 d P . . N4 N 0.5236(6) 0.5368(6) 0.9894(4) 0.0537(12) Uani 0.50 1 d PDU . . N3A N 0.3322(2) 0.3008(2) 0.5026(2) 0.0289(7) Uani 0.498(4) 1 d PG A 1 C1A C 0.3924(3) 0.1832(3) 0.4654(2) 0.0386(9) Uani 0.498(4) 1 d PG A 1 H1A H 0.4896 0.1791 0.4330 0.046 Uiso 0.498(4) 1 calc PR A 1 C2A C 0.3075(4) 0.0715(2) 0.4767(2) 0.0484(12) Uani 0.498(4) 1 d PG A 1 H2A H 0.3478 -0.0073 0.4518 0.058 Uiso 0.498(4) 1 calc PR A 1 C3A C 0.1623(4) 0.0775(3) 0.5251(2) 0.0543(15) Uani 0.498(4) 1 d PG A 1 H3A H 0.1054 0.0027 0.5327 0.065 Uiso 0.498(4) 1 calc PR A 1 C4A C 0.1020(2) 0.1951(3) 0.5624(2) 0.0502(14) Uani 0.498(4) 1 d PG A 1 H4A H 0.0049 0.1991 0.5948 0.060 Uiso 0.498(4) 1 calc PR A 1 C5A C 0.1869(3) 0.3068(3) 0.5511(2) 0.0379(10) Uani 0.498(4) 1 d PG A 1 H5A H 0.1466 0.3856 0.5760 0.045 Uiso 0.498(4) 1 calc PR A 1 N3B N 0.3074(2) 0.3078(2) 0.5475(2) 0.0279(7) Uani 0.502(4) 1 d PG A 2 C1B C 0.3374(2) 0.1788(2) 0.5197(2) 0.0369(10) Uani 0.502(4) 1 d PG A 2 H1B H 0.4320 0.1522 0.4896 0.044 Uiso 0.502(4) 1 calc PR A 2 C2B C 0.2260(3) 0.0895(2) 0.5368(2) 0.0416(11) Uani 0.502(4) 1 d PG A 2 H2B H 0.2461 0.0032 0.5182 0.050 Uiso 0.502(4) 1 calc PR A 2 C3B C 0.0847(3) 0.1293(3) 0.5818(2) 0.0410(11) Uani 0.502(4) 1 d PG A 2 H3B H 0.0101 0.0695 0.5933 0.049 Uiso 0.502(4) 1 calc PR A 2 C4B C 0.0547(2) 0.2582(3) 0.60962(19) 0.0362(9) Uani 0.502(4) 1 d PG A 2 H4B H -0.0399 0.2848 0.6397 0.043 Uiso 0.502(4) 1 calc PR A 2 C5B C 0.1660(2) 0.3475(2) 0.59246(19) 0.0314(8) Uani 0.502(4) 1 d PG A 2 H5B H 0.1460 0.4338 0.6111 0.038 Uiso 0.502(4) 1 calc PR A 2 C6 C 1.11742(17) 0.91271(16) 0.81579(10) 0.0241(3) Uani 1 1 d . . . C7 C 1.1345(2) 1.05762(18) 0.80097(13) 0.0325(4) Uani 1 1 d . . . H7 H 1.0532 1.1220 0.8148 0.039 Uiso 1 1 calc R . . C8 C 1.2740(2) 1.1055(2) 0.76537(15) 0.0395(4) Uani 1 1 d . . . H8 H 1.2857 1.2022 0.7549 0.047 Uiso 1 1 calc R . . C9 C 1.3950(2) 1.0097(2) 0.74553(14) 0.0377(4) Uani 1 1 d . . . H9 H 1.4878 1.0423 0.7213 0.045 Uiso 1 1 calc R . . C10 C 1.3786(2) 0.8654(2) 0.76168(16) 0.0405(4) Uani 1 1 d . . . H10 H 1.4606 0.8012 0.7490 0.049 Uiso 1 1 calc R . . C11 C 1.2403(2) 0.81623(19) 0.79682(14) 0.0340(4) Uani 1 1 d . . . H11 H 1.2294 0.7192 0.8077 0.041 Uiso 1 1 calc R . . C12 C 0.79935(17) 0.99146(17) 0.87433(11) 0.0255(3) Uani 1 1 d . . . C13 C 0.7581(2) 1.07723(19) 0.79844(13) 0.0329(4) Uani 1 1 d . . . H13 H 0.7992 1.0558 0.7426 0.039 Uiso 1 1 calc R . . C14 C 0.6556(2) 1.1946(2) 0.80654(16) 0.0406(4) Uani 1 1 d . . . H14 H 0.6287 1.2526 0.7561 0.049 Uiso 1 1 calc R . . C15 C 0.5935(2) 1.2249(2) 0.89037(16) 0.0410(5) Uani 1 1 d . . . H15 H 0.5252 1.3037 0.8957 0.049 Uiso 1 1 calc R . . C16 C 0.6320(2) 1.1394(2) 0.96576(15) 0.0380(4) Uani 1 1 d . . . H16 H 0.5885 1.1599 1.0215 0.046 Uiso 1 1 calc R . . C17 C 0.7360(2) 1.02249(19) 0.95852(13) 0.0316(3) Uani 1 1 d . . . H17 H 0.7632 0.9655 1.0092 0.038 Uiso 1 1 calc R . . C18 C 0.93962(18) 0.73340(16) 0.96900(10) 0.0243(3) Uani 1 1 d . . . C19 C 1.0613(2) 0.7206(2) 1.00606(12) 0.0331(4) Uani 1 1 d . . . H19 H 1.1463 0.7627 0.9727 0.040 Uiso 1 1 calc R . . C20 C 1.0549(3) 0.6443(2) 1.09355(13) 0.0398(4) Uani 1 1 d . . . H20 H 1.1359 0.6352 1.1186 0.048 Uiso 1 1 calc R . . C21 C 0.9279(2) 0.58219(19) 1.14313(12) 0.0367(4) Uani 1 1 d . . . H21 H 0.9229 0.5338 1.2020 0.044 Uiso 1 1 calc R . . C22 C 0.8087(2) 0.59170(19) 1.10566(13) 0.0355(4) Uani 1 1 d . . . H22 H 0.7248 0.5475 1.1388 0.043 Uiso 1 1 calc R . . C23 C 0.8137(2) 0.66700(19) 1.01879(12) 0.0317(3) Uani 1 1 d . . . H23 H 0.7332 0.6733 0.9937 0.038 Uiso 1 1 calc R . . C24 C 0.89942(18) 0.75543(16) 0.78401(11) 0.0246(3) Uani 1 1 d . . . C25 C 0.7669(2) 0.69186(19) 0.80734(13) 0.0321(3) Uani 1 1 d . . . H25 H 0.6997 0.7000 0.8606 0.038 Uiso 1 1 calc R . . C26 C 0.7360(2) 0.6165(2) 0.75066(16) 0.0424(5) Uani 1 1 d . . . H26 H 0.6493 0.5719 0.7668 0.051 Uiso 1 1 calc R . . C27 C 0.8343(3) 0.6079(3) 0.67017(17) 0.0503(6) Uani 1 1 d . . . H27 H 0.8133 0.5574 0.6324 0.060 Uiso 1 1 calc R . . C28 C 0.9636(2) 0.6740(2) 0.64565(14) 0.0439(5) Uani 1 1 d . . . H28 H 1.0281 0.6691 0.5910 0.053 Uiso 1 1 calc R . . C29 C 0.9974(2) 0.7478(2) 0.70241(12) 0.0310(3) Uani 1 1 d . . . H29 H 1.0846 0.7916 0.6861 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.02366(7) 0.02552(7) 0.02201(6) -0.00674(4) -0.00294(4) -0.00437(4) P1 0.02090(17) 0.02191(17) 0.02257(18) -0.00597(14) -0.00460(14) -0.00152(14) O1A 0.0427(16) 0.0478(16) 0.0348(14) -0.0136(12) -0.0054(11) 0.0102(12) O2A 0.073(2) 0.0506(18) 0.0243(13) -0.0039(11) -0.0095(13) 0.0149(16) O1B 0.0358(15) 0.0589(19) 0.0306(14) -0.0195(13) 0.0065(11) -0.0162(13) O2B 0.0451(18) 0.082(3) 0.0358(16) -0.0309(17) -0.0001(13) -0.0230(17) O3 0.0365(7) 0.0363(7) 0.0494(8) -0.0052(6) -0.0167(6) -0.0063(6) O4A 0.0349(18) 0.0307(15) 0.112(5) -0.0253(19) -0.030(2) 0.0038(13) O4B 0.0431(17) 0.0375(15) 0.053(2) 0.0113(13) -0.0224(16) -0.0160(12) O5 0.048(2) 0.055(2) 0.089(3) -0.025(2) -0.017(2) -0.0111(17) O6 0.061(4) 0.060(3) 0.072(4) -0.025(2) 0.013(3) -0.014(2) N1 0.0455(9) 0.0443(9) 0.0290(8) -0.0122(7) 0.0008(7) -0.0080(7) N2A 0.028(2) 0.035(2) 0.061(4) -0.012(2) -0.011(2) -0.0008(16) N2B 0.038(2) 0.0336(19) 0.041(2) 0.0013(17) -0.0162(18) -0.0039(16) N4 0.040(2) 0.047(3) 0.077(3) -0.032(2) 0.007(2) -0.0150(18) N3A 0.0273(15) 0.0288(14) 0.0321(18) -0.0026(13) -0.0105(14) -0.0072(11) C1A 0.042(2) 0.0324(18) 0.042(2) -0.0046(16) -0.0133(19) -0.0067(16) C2A 0.059(3) 0.0298(18) 0.064(3) -0.0051(18) -0.029(3) -0.0103(18) C3A 0.068(4) 0.044(2) 0.058(3) 0.015(2) -0.035(3) -0.033(2) C4A 0.043(2) 0.059(3) 0.051(3) 0.014(3) -0.023(2) -0.031(2) C5A 0.0270(18) 0.038(2) 0.044(2) 0.0082(17) -0.0120(17) -0.0105(15) N3B 0.0264(14) 0.0229(13) 0.0330(18) -0.0011(12) -0.0080(13) -0.0039(10) C1B 0.0330(19) 0.0253(16) 0.057(3) -0.0082(16) -0.0192(19) -0.0039(14) C2B 0.045(3) 0.0297(18) 0.056(3) -0.0044(17) -0.021(2) -0.0119(17) C3B 0.041(2) 0.039(2) 0.048(3) 0.0011(19) -0.021(2) -0.0195(18) C4B 0.0310(18) 0.0372(19) 0.039(2) 0.0027(16) -0.0109(15) -0.0107(15) C5B 0.0280(17) 0.0310(17) 0.0349(19) -0.0065(14) -0.0065(14) -0.0036(13) C6 0.0227(7) 0.0246(7) 0.0245(7) -0.0045(5) -0.0047(6) -0.0029(5) C7 0.0283(8) 0.0254(7) 0.0452(10) -0.0108(7) -0.0074(7) -0.0028(6) C8 0.0359(10) 0.0296(8) 0.0536(12) -0.0068(8) -0.0084(9) -0.0111(7) C9 0.0279(8) 0.0446(10) 0.0418(10) -0.0094(8) -0.0047(7) -0.0124(7) C10 0.0226(8) 0.0407(10) 0.0557(12) -0.0132(9) -0.0028(8) -0.0005(7) C11 0.0259(8) 0.0257(7) 0.0479(10) -0.0073(7) -0.0049(7) -0.0015(6) C12 0.0218(7) 0.0258(7) 0.0309(8) -0.0104(6) -0.0065(6) -0.0004(6) C13 0.0335(9) 0.0314(8) 0.0365(9) -0.0114(7) -0.0129(7) 0.0045(7) C14 0.0378(10) 0.0322(9) 0.0564(12) -0.0115(8) -0.0226(9) 0.0064(8) C15 0.0273(8) 0.0331(9) 0.0671(14) -0.0225(9) -0.0116(9) 0.0043(7) C16 0.0277(8) 0.0376(9) 0.0505(11) -0.0237(8) 0.0003(8) -0.0009(7) C17 0.0288(8) 0.0324(8) 0.0342(9) -0.0135(7) -0.0023(7) -0.0028(7) C18 0.0276(7) 0.0230(6) 0.0227(7) -0.0062(5) -0.0047(6) -0.0027(6) C19 0.0349(9) 0.0366(8) 0.0300(8) -0.0033(7) -0.0122(7) -0.0080(7) C20 0.0493(11) 0.0403(9) 0.0338(9) -0.0021(7) -0.0205(8) -0.0067(8) C21 0.0555(12) 0.0268(8) 0.0252(8) -0.0034(6) -0.0081(8) -0.0007(8) C22 0.0412(10) 0.0296(8) 0.0305(9) -0.0035(7) 0.0004(7) -0.0060(7) C23 0.0303(8) 0.0324(8) 0.0310(8) -0.0031(6) -0.0055(7) -0.0067(7) C24 0.0258(7) 0.0239(7) 0.0261(7) -0.0084(6) -0.0086(6) 0.0013(6) C25 0.0287(8) 0.0342(8) 0.0377(9) -0.0142(7) -0.0094(7) -0.0026(7) C26 0.0359(10) 0.0435(10) 0.0606(13) -0.0249(10) -0.0224(9) -0.0004(8) C27 0.0473(12) 0.0595(13) 0.0631(14) -0.0423(12) -0.0304(11) 0.0153(10) C28 0.0425(11) 0.0590(12) 0.0378(10) -0.0282(9) -0.0174(9) 0.0158(10) C29 0.0305(8) 0.0362(8) 0.0273(8) -0.0100(7) -0.0092(7) 0.0042(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 Nd O1A 2.499(3) . ? Nd O2B 2.512(3) . ? Nd O4B 2.523(3) . ? Nd O1B 2.543(3) . ? Nd O2A 2.567(3) . ? Nd O3 2.6034(14) . ? Nd O4A 2.606(3) . ? Nd N3B 2.6373(16) . ? Nd N3A 2.6547(17) . ? P1 C6 1.7938(16) . ? P1 C12 1.7966(16) . ? P1 C18 1.7984(16) . ? P1 C24 1.8019(16) . ? O1A N1 1.233(3) . ? O2A N1 1.241(3) . ? O1B N1 1.260(3) . ? O2B N1 1.245(4) . ? O3 N2B 1.214(5) . ? O3 N2A 1.282(6) . ? O4A N2A 1.264(6) . ? O4B N2B 1.254(6) . ? O5 N4 1.241(4) . ? O6 N4 1.237(4) . ? N3A C1A 1.3900 . ? N3A C5A 1.3900 . ? C1A C2A 1.3900 . ? C1A H1A 0.9300 . ? C2A C3A 1.3900 . ? C2A H2A 0.9300 . ? C3A C4A 1.3900 . ? C3A H3A 0.9300 . ? C4A C5A 1.3900 . ? C4A H4A 0.9300 . ? C5A H5A 0.9300 . ? N3B C1B 1.3900 . ? N3B C5B 1.3900 . ? C1B C2B 1.3900 . ? C1B H1B 0.9300 . ? C2B C3B 1.3900 . ? C2B H2B 0.9300 . ? C3B C4B 1.3900 . ? C3B H3B 0.9300 . ? C4B C5B 1.3900 . ? C4B H4B 0.9300 . ? C5B H5B 0.9300 . ? C6 C7 1.393(2) . ? C6 C11 1.395(2) . ? C7 C8 1.393(3) . ? C7 H7 0.9300 . ? C8 C9 1.382(3) . ? C8 H8 0.9300 . ? C9 C10 1.384(3) . ? C9 H9 0.9300 . ? C10 C11 1.387(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.396(2) . ? C12 C17 1.400(2) . ? C13 C14 1.388(3) . ? C13 H13 0.9300 . ? C14 C15 1.391(3) . ? C14 H14 0.9300 . ? C15 C16 1.379(3) . ? C15 H15 0.9300 . ? C16 C17 1.392(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.394(2) . ? C18 C23 1.397(2) . ? C19 C20 1.396(3) . ? C19 H19 0.9300 . ? C20 C21 1.386(3) . ? C20 H20 0.9300 . ? C21 C22 1.380(3) . ? C21 H21 0.9300 . ? C22 C23 1.387(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.396(2) . ? C24 C25 1.399(2) . ? C25 C26 1.390(2) . ? C25 H25 0.9300 . ? C26 C27 1.386(3) . ? C26 H26 0.9300 . ? C27 C28 1.384(4) . ? C27 H27 0.9300 . ? C28 C29 1.393(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Nd O1A 180.0 . 2_666 ? O1A Nd O2B 143.86(11) . 2_666 ? O1A Nd O2B 143.86(11) 2_666 . ? O2B Nd O2B 180.00(16) 2_666 . ? O1A Nd O4B 77.70(12) . . ? O1A Nd O4B 102.30(12) 2_666 . ? O2B Nd O4B 81.74(14) 2_666 . ? O2B Nd O4B 98.26(13) . . ? O1A Nd O4B 102.30(12) . 2_666 ? O1A Nd O4B 77.71(12) 2_666 2_666 ? O2B Nd O4B 98.26(14) 2_666 2_666 ? O2B Nd O4B 81.74(13) . 2_666 ? O4B Nd O4B 180.0 . 2_666 ? O1A Nd O1B 148.60(10) 2_666 . ? O2B Nd O1B 131.19(10) 2_666 . ? O2B Nd O1B 48.81(10) . . ? O4B Nd O1B 102.36(12) . . ? O4B Nd O1B 77.64(12) 2_666 . ? O1A Nd O1B 148.60(10) . 2_666 ? O2B Nd O1B 131.19(10) . 2_666 ? O4B Nd O1B 77.64(12) . 2_666 ? O4B Nd O1B 102.36(12) 2_666 2_666 ? O1B Nd O1B 180.0 . 2_666 ? O1A Nd O2A 48.13(9) . . ? O1A Nd O2A 131.87(9) 2_666 . ? O2B Nd O2A 148.70(12) 2_666 . ? O4B Nd O2A 124.59(12) . . ? O1B Nd O2A 144.13(11) 2_666 . ? O1A Nd O2A 131.87(9) . 2_666 ? O2B Nd O2A 148.70(12) . 2_666 ? O4B Nd O2A 124.59(12) 2_666 2_666 ? O1B Nd O2A 144.13(11) . 2_666 ? O2A Nd O2A 179.999(1) . 2_666 ? O1A Nd O3 109.49(8) . 2_666 ? O1A Nd O3 70.51(8) 2_666 2_666 ? O2B Nd O3 106.40(10) 2_666 2_666 ? O2B Nd O3 73.60(10) . 2_666 ? O4B Nd O3 131.77(7) . 2_666 ? O4B Nd O3 48.23(7) 2_666 2_666 ? O1B Nd O3 105.89(8) . 2_666 ? O1B Nd O3 74.11(8) 2_666 2_666 ? O2A Nd O3 70.27(9) . 2_666 ? O2A Nd O3 109.73(9) 2_666 2_666 ? O1A Nd O3 70.51(8) . . ? O1A Nd O3 109.49(8) 2_666 . ? O2B Nd O3 73.60(10) 2_666 . ? O2B Nd O3 106.40(10) . . ? O4B Nd O3 48.23(7) . . ? O4B Nd O3 131.77(7) 2_666 . ? O1B Nd O3 74.11(8) . . ? O1B Nd O3 105.89(8) 2_666 . ? O2A Nd O3 109.73(9) . . ? O2A Nd O3 70.27(9) 2_666 . ? O3 Nd O3 180.00(6) 2_666 . ? O1A Nd O4A 52.07(15) . . ? O1A Nd O4A 127.93(15) 2_666 . ? O2B Nd O4A 104.16(15) 2_666 . ? O2B Nd O4A 75.84(15) . . ? O4B Nd O4A 154.36(12) 2_666 . ? O1B Nd O4A 78.28(15) . . ? O1B Nd O4A 101.72(15) 2_666 . ? O2A Nd O4A 99.31(15) . . ? O2A Nd O4A 80.69(15) 2_666 . ? O3 Nd O4A 132.94(8) 2_666 . ? O3 Nd O4A 47.06(8) . . ? O1A Nd O4A 127.93(15) . 2_666 ? O1A Nd N3B 88.59(10) . . ? O1A Nd N3B 91.41(10) 2_666 . ? O2B Nd N3B 74.56(11) 2_666 . ? O2B Nd N3B 105.44(10) . . ? O4B Nd N3B 116.73(8) . . ? O4B Nd N3B 63.27(8) 2_666 . ? O1B Nd N3B 60.04(9) . . ? O1B Nd N3B 119.96(9) 2_666 . ? O2A Nd N3B 77.88(11) . . ? O2A Nd N3B 102.12(11) 2_666 . ? O3 Nd N3B 111.16(6) 2_666 . ? O3 Nd N3B 68.84(6) . . ? O4A Nd N3B 110.95(9) . . ? O4A Nd N3B 69.05(9) 2_666 . ? O1A Nd N3B 91.41(10) . 2_666 ? O1A Nd N3B 88.59(10) 2_666 2_666 ? O2B Nd N3B 105.44(10) 2_666 2_666 ? O2B Nd N3B 74.56(10) . 2_666 ? O4B Nd N3B 63.26(8) . 2_666 ? O4B Nd N3B 116.73(8) 2_666 2_666 ? O1B Nd N3B 119.96(9) . 2_666 ? O1B Nd N3B 60.04(9) 2_666 2_666 ? O2A Nd N3B 102.12(11) . 2_666 ? O2A Nd N3B 77.88(11) 2_666 2_666 ? O3 Nd N3B 68.84(6) 2_666 2_666 ? O3 Nd N3B 111.16(6) . 2_666 ? O4A Nd N3B 69.05(9) . 2_666 ? O4A Nd N3B 110.95(9) 2_666 2_666 ? N3B Nd N3B 180.0 . 2_666 ? O1A Nd N3A 102.07(10) . . ? O1A Nd N3A 77.93(10) 2_666 . ? O2B Nd N3A 59.30(11) 2_666 . ? O2B Nd N3A 120.70(11) . . ? O4B Nd N3A 112.24(8) . . ? O4B Nd N3A 67.76(8) 2_666 . ? O1B Nd N3A 74.92(9) . . ? O1B Nd N3A 105.08(9) 2_666 . ? O2A Nd N3A 92.37(11) . . ? O2A Nd N3A 87.64(11) 2_666 . ? O3 Nd N3A 112.41(6) 2_666 . ? O3 Nd N3A 67.59(6) . . ? O4A Nd N3A 113.80(9) . . ? O4A Nd N3A 66.20(9) 2_666 . ? N3B Nd N3A 164.69(7) 2_666 . ? O1A Nd N3A 77.93(10) . 2_666 ? O1A Nd N3A 102.07(10) 2_666 2_666 ? O2B Nd N3A 120.70(11) 2_666 2_666 ? O2B Nd N3A 59.30(11) . 2_666 ? O4B Nd N3A 67.76(8) . 2_666 ? O4B Nd N3A 112.24(8) 2_666 2_666 ? O1B Nd N3A 105.08(9) . 2_666 ? O1B Nd N3A 74.92(9) 2_666 2_666 ? O2A Nd N3A 87.63(11) . 2_666 ? O2A Nd N3A 92.36(11) 2_666 2_666 ? O3 Nd N3A 67.59(6) 2_666 2_666 ? O3 Nd N3A 112.41(6) . 2_666 ? O4A Nd N3A 66.19(9) . 2_666 ? O4A Nd N3A 113.80(9) 2_666 2_666 ? N3B Nd N3A 164.69(7) . 2_666 ? N3B Nd N3A 15.31(7) 2_666 2_666 ? N3A Nd N3A 180.0 . 2_666 ? C6 P1 C12 110.43(7) . . ? C6 P1 C18 108.35(8) . . ? C12 P1 C18 108.28(8) . . ? C6 P1 C24 109.36(8) . . ? C12 P1 C24 107.43(7) . . ? C18 P1 C24 112.99(7) . . ? N1 O1A Nd 101.09(17) . . ? N1 O2A Nd 97.45(17) . . ? N1 O1B Nd 98.07(17) . . ? N1 O2B Nd 100.08(19) . . ? N2B O3 Nd 96.3(2) . . ? N2A O3 Nd 101.3(3) . . ? N2A O4A Nd 101.7(3) . . ? N2B O4B Nd 99.1(3) . . ? O1A N1 O2A 113.3(2) . . ? O2B N1 O1B 113.0(2) . . ? O4A N2A O3 109.6(4) . . ? O3 N2B O4B 116.2(4) . . ? O6 N4 O5 114.8(4) . . ? C1A N3A C5A 120.0 . . ? C1A N3A Nd 120.66(12) . . ? C5A N3A Nd 118.90(12) . . ? C2A C1A N3A 120.0 . . ? C2A C1A H1A 120.0 . . ? N3A C1A H1A 120.0 . . ? C1A C2A C3A 120.0 . . ? C1A C2A H2A 120.0 . . ? C3A C2A H2A 120.0 . . ? C2A C3A C4A 120.0 . . ? C2A C3A H3A 120.0 . . ? C4A C3A H3A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A H4A 120.0 . . ? C5A C4A H4A 120.0 . . ? C4A C5A N3A 120.0 . . ? C4A C5A H5A 120.0 . . ? N3A C5A H5A 120.0 . . ? C1B N3B C5B 120.0 . . ? C1B N3B Nd 122.40(11) . . ? C5B N3B Nd 117.09(11) . . ? N3B C1B C2B 120.0 . . ? N3B C1B H1B 120.0 . . ? C2B C1B H1B 120.0 . . ? C1B C2B C3B 120.0 . . ? C1B C2B H2B 120.0 . . ? C3B C2B H2B 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C4B C5B N3B 120.0 . . ? C4B C5B H5B 120.0 . . ? N3B C5B H5B 120.0 . . ? C7 C6 C11 119.91(15) . . ? C7 C6 P1 121.15(12) . . ? C11 C6 P1 118.94(12) . . ? C8 C7 C6 119.60(16) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 120.26(17) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.22(18) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 120.16(18) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 119.84(16) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C13 C12 C17 120.11(15) . . ? C13 C12 P1 118.70(13) . . ? C17 C12 P1 121.14(13) . . ? C14 C13 C12 119.82(18) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.71(19) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.78(17) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.13(19) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 119.43(18) . . ? C16 C17 H17 120.3 . . ? C12 C17 H17 120.3 . . ? C19 C18 C23 119.82(16) . . ? C19 C18 P1 119.93(13) . . ? C23 C18 P1 120.08(13) . . ? C18 C19 C20 119.64(18) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 119.99(18) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.37(17) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.19(18) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 119.96(17) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C29 C24 C25 119.97(16) . . ? C29 C24 P1 121.25(13) . . ? C25 C24 P1 118.79(13) . . ? C26 C25 C24 119.78(18) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 120.0(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.40(18) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.30(19) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 119.49(18) . . ? C28 C29 H29 120.3 . . ? C24 C29 H29 120.3 . . ? _database_code_depnum_ccdc_archive 'CCDC 963099' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N6 Nd O10 P2' _chemical_formula_weight 1132.13 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' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 13.2408(2) _cell_length_b 17.9735(4) _cell_length_c 21.7067(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.8113(12) _cell_angle_gamma 90.00 _cell_volume 5129.38(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 191378 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2300 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and seven \w scans with 2\% steps (486 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 191378 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_unetI/netI 0.0246 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 30.51 _reflns_number_total 15604 _reflns_number_gt 13465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; The structure of the isomorphous Ce complex was used as a starting model, but the disorder of the two nitrite ions containing N1 and N5, which are very badly resolved, has been treated slightly differently. As in the Ce complex, the nitrite containing N5 was found to be disordered over two positions sharing the atom O10, but the nitrite ion containing N1 was also modeled with two positions. The positions A of the nitrite containing N1 and B of that containing N5 are incompatible, and the occupancy parameters, constrained to sum to unity, have been attributed accordingly. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths, angles and displacement parameters for atoms in the nitrite ions: DFIX 1.24 0.005 N1A O1A DFIX 1.24 0.005 N1A O2A DFIX 2.05 0.005 O1A O2A DFIX 1.24 0.005 N1B O1B DFIX 1.24 0.005 N1B O2B DFIX 2.05 0.005 O1B O2B DFIX 2.57 0.01 ND O2B DFIX 2.57 0.005 ND O9B DFIX 1.24 0.01 N5A O9A DFIX 1.24 0.01 N5A O10 DFIX 2.05 0.01 O9A O10 DFIX 1.24 0.01 N5B O9B DFIX 1.24 0.01 N5B O10 DFIX 2.05 0.01 O9B O10 ISOR 0.005 N1A O3 O4 O7 O8 N5A SIMU .005 .005 3. N1A O1A O2A N1B O1B O2B SIMU .005 .005 3. N2 O3 O4 SIMU .002 .002 3. N3 O5 O6 SIMU .005 .005 3. N4 O7 O8 SIMU .005 .005 3. N5A N5B O9A O9B O10 The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0583P)^2^+6.1907P] 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 15604 _refine_ls_number_parameters 695 _refine_ls_number_restraints 254 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.106 _refine_diff_density_min -1.186 _refine_diff_density_rms 0.088 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 Nd Nd 0.787803(10) 0.365264(7) 0.236507(6) 0.02638(5) Uani 1 1 d D . . P1 P 0.64499(6) 0.89863(4) 0.10554(3) 0.03153(14) Uani 1 1 d . . . P2 P 0.24047(5) 0.37268(4) 0.05029(3) 0.02612(12) Uani 1 1 d . . . O1A O 0.7057(3) 0.4909(3) 0.2595(3) 0.0564(10) Uani 0.595(3) 1 d PDU A 1 O2A O 0.8632(3) 0.4914(3) 0.2667(3) 0.0656(10) Uani 0.595(3) 1 d PDU A 1 N1A N 0.7842(4) 0.5274(3) 0.2711(3) 0.0648(11) Uani 0.595(3) 1 d PDU A 1 O1B O 0.6874(6) 0.4368(4) 0.3108(3) 0.0622(12) Uani 0.405(3) 1 d PDU A 2 O2B O 0.7374(7) 0.5042(4) 0.2446(3) 0.0624(14) Uani 0.405(3) 1 d PDU A 2 N1B N 0.6938(7) 0.5009(4) 0.2924(4) 0.0624(13) Uani 0.405(3) 1 d PDU A 2 O3 O 0.8177(2) 0.4235(2) 0.13407(15) 0.0744(8) Uani 1 1 d U A . O4 O 0.9499(3) 0.3986(3) 0.1868(2) 0.0936(10) Uani 1 1 d U A . O5 O 0.61067(16) 0.39008(13) 0.17066(11) 0.0397(4) Uani 1 1 d U A . O6 O 0.68199(19) 0.28925(15) 0.15134(12) 0.0518(5) Uani 1 1 d U A . O7 O 0.6263(3) 0.3090(2) 0.28068(17) 0.0839(9) Uani 1 1 d U A . O8 O 0.7577(3) 0.2514(2) 0.30432(18) 0.0842(9) Uani 1 1 d U A . O9A O 0.8138(4) 0.3838(3) 0.3548(2) 0.0595(10) Uani 0.595(3) 1 d PDU A . O9B O 0.8890(6) 0.4373(4) 0.3283(4) 0.0778(14) Uani 0.405(3) 1 d PDU A . O10 O 0.9467(2) 0.34133(17) 0.31377(14) 0.0638(7) Uani 1 1 d DU A . N2 N 0.9088(3) 0.4329(3) 0.14002(18) 0.0689(9) Uani 1 1 d U . . N3 N 0.6073(2) 0.33335(17) 0.13729(14) 0.0461(5) Uani 1 1 d U . . N4 N 0.6661(3) 0.25260(19) 0.30667(17) 0.0599(8) Uani 1 1 d U . . N5A N 0.9076(5) 0.3655(3) 0.3639(3) 0.0655(12) Uani 0.595(3) 1 d PDU . . N5B N 0.9754(6) 0.4063(5) 0.3282(5) 0.0750(15) Uani 0.405(3) 1 d PDU A . N6 N 0.8857(2) 0.24426(17) 0.19450(14) 0.0466(7) Uani 1 1 d . A . C1 C 0.9305(2) 0.19321(19) 0.2333(2) 0.0499(8) Uani 1 1 d . . . H1 H 0.9343 0.2016 0.2767 0.060 Uiso 1 1 calc R A . C2 C 0.9720(3) 0.1277(2) 0.2120(3) 0.0738(16) Uani 1 1 d . A . H2 H 1.0031 0.0921 0.2406 0.089 Uiso 1 1 calc R . . C3 C 0.9672(5) 0.1159(4) 0.1499(4) 0.106(3) Uani 1 1 d . . . H3 H 0.9934 0.0712 0.1346 0.127 Uiso 1 1 calc R A . C4 C 0.9238(5) 0.1696(4) 0.1087(3) 0.103(2) Uani 1 1 d . A . H4 H 0.9212 0.1629 0.0651 0.124 Uiso 1 1 calc R . . C5 C 0.8843(3) 0.2330(3) 0.1332(2) 0.0708(13) Uani 1 1 d . . . H5 H 0.8551 0.2701 0.1055 0.085 Uiso 1 1 calc R A . C6 C 0.5332(2) 0.86550(15) 0.05841(13) 0.0333(5) Uani 1 1 d . . . C7 C 0.4416(3) 0.85741(19) 0.08327(15) 0.0409(7) Uani 1 1 d . . . H7 H 0.4355 0.8743 0.1241 0.049 Uiso 1 1 calc R . . C8 C 0.3592(3) 0.8245(2) 0.04789(16) 0.0466(7) Uani 1 1 d . . . H8 H 0.2971 0.8178 0.0650 0.056 Uiso 1 1 calc R . . C9 C 0.3672(3) 0.80148(19) -0.01218(16) 0.0447(7) Uani 1 1 d . . . H9 H 0.3102 0.7796 -0.0362 0.054 Uiso 1 1 calc R . . C10 C 0.4569(3) 0.81010(18) -0.03719(14) 0.0423(7) Uani 1 1 d . . . H10 H 0.4616 0.7947 -0.0786 0.051 Uiso 1 1 calc R . . C11 C 0.5407(2) 0.84126(19) -0.00221(14) 0.0390(6) Uani 1 1 d . . . H11 H 0.6032 0.8462 -0.0193 0.047 Uiso 1 1 calc R . . C12 C 0.7007(2) 0.82335(16) 0.15208(13) 0.0340(5) Uani 1 1 d . . . C13 C 0.6634(3) 0.75090(18) 0.14490(14) 0.0406(6) Uani 1 1 d . . . H13 H 0.6065 0.7402 0.1153 0.049 Uiso 1 1 calc R . . C14 C 0.7105(3) 0.69478(19) 0.18151(16) 0.0477(8) Uani 1 1 d . . . H14 H 0.6849 0.6454 0.1773 0.057 Uiso 1 1 calc R . . C15 C 0.7942(3) 0.7097(2) 0.22401(16) 0.0474(8) Uani 1 1 d . . . H15 H 0.8262 0.6705 0.2483 0.057 Uiso 1 1 calc R . . C16 C 0.8319(3) 0.7816(2) 0.23153(15) 0.0452(7) Uani 1 1 d . . . H16 H 0.8897 0.7916 0.2606 0.054 Uiso 1 1 calc R . . C17 C 0.7840(2) 0.83884(19) 0.19607(14) 0.0395(6) Uani 1 1 d . . . H17 H 0.8079 0.8885 0.2018 0.047 Uiso 1 1 calc R . . C18 C 0.7322(2) 0.93105(17) 0.05412(14) 0.0357(6) Uani 1 1 d . . . C19 C 0.6984(3) 0.98199(19) 0.00718(16) 0.0442(7) Uani 1 1 d . . . H19 H 0.6309 1.0008 0.0040 0.053 Uiso 1 1 calc R . . C20 C 0.7634(3) 1.0048(2) -0.03452(16) 0.0498(8) Uani 1 1 d . . . H20 H 0.7406 1.0391 -0.0664 0.060 Uiso 1 1 calc R . . C21 C 0.8617(3) 0.9776(2) -0.02978(17) 0.0498(8) Uani 1 1 d . . . H21 H 0.9059 0.9933 -0.0586 0.060 Uiso 1 1 calc R . . C22 C 0.8961(3) 0.9280(2) 0.01618(17) 0.0478(8) Uani 1 1 d . . . H22 H 0.9639 0.9099 0.0191 0.057 Uiso 1 1 calc R . . C23 C 0.8317(2) 0.90413(19) 0.05862(15) 0.0402(6) Uani 1 1 d . . . H23 H 0.8553 0.8698 0.0904 0.048 Uiso 1 1 calc R . . C24 C 0.6170(2) 0.97143(16) 0.15763(13) 0.0334(5) Uani 1 1 d . . . C25 C 0.5662(2) 0.95272(18) 0.20847(14) 0.0373(6) Uani 1 1 d . . . H25 H 0.5473 0.9026 0.2149 0.045 Uiso 1 1 calc R . . C26 C 0.5436(2) 1.00808(19) 0.24952(15) 0.0414(6) Uani 1 1 d . . . H26 H 0.5076 0.9960 0.2835 0.050 Uiso 1 1 calc R . . C27 C 0.5734(3) 1.08053(19) 0.24092(15) 0.0429(7) Uani 1 1 d . . . H27 H 0.5588 1.1179 0.2695 0.052 Uiso 1 1 calc R . . C28 C 0.6245(3) 1.09930(18) 0.19098(16) 0.0439(7) Uani 1 1 d . . . H28 H 0.6443 1.1494 0.1853 0.053 Uiso 1 1 calc R . . C29 C 0.6469(2) 1.04468(17) 0.14896(14) 0.0388(6) Uani 1 1 d . . . H29 H 0.6821 1.0573 0.1148 0.047 Uiso 1 1 calc R . . C30 C 0.1230(2) 0.34939(16) 0.00484(12) 0.0302(5) Uani 1 1 d . . . C31 C 0.0300(2) 0.3722(2) 0.02268(15) 0.0418(7) Uani 1 1 d . . . H31 H 0.0279 0.4034 0.0578 0.050 Uiso 1 1 calc R . . C32 C -0.0595(3) 0.3486(3) -0.01179(18) 0.0538(9) Uani 1 1 d . . . H32 H -0.1233 0.3640 -0.0002 0.065 Uiso 1 1 calc R . . C33 C -0.0563(3) 0.3030(2) -0.06290(17) 0.0512(8) Uani 1 1 d . . . H33 H -0.1180 0.2862 -0.0855 0.061 Uiso 1 1 calc R . . C34 C 0.0355(2) 0.28160(19) -0.08126(15) 0.0429(7) Uani 1 1 d . . . H34 H 0.0371 0.2510 -0.1168 0.051 Uiso 1 1 calc R . . C35 C 0.1255(2) 0.30484(17) -0.04764(14) 0.0365(6) Uani 1 1 d . . . H35 H 0.1889 0.2904 -0.0603 0.044 Uiso 1 1 calc R . . C36 C 0.2259(2) 0.45165(15) 0.09889(12) 0.0300(5) Uani 1 1 d . . . C37 C 0.1743(2) 0.44266(17) 0.15052(14) 0.0373(6) Uani 1 1 d . . . H37 H 0.1477 0.3954 0.1598 0.045 Uiso 1 1 calc R . . C38 C 0.1620(3) 0.50384(19) 0.18851(15) 0.0435(7) Uani 1 1 d . . . H38 H 0.1254 0.4987 0.2234 0.052 Uiso 1 1 calc R . . C39 C 0.2030(3) 0.57172(19) 0.17537(16) 0.0444(7) Uani 1 1 d . . . H39 H 0.1956 0.6129 0.2019 0.053 Uiso 1 1 calc R . . C40 C 0.2547(2) 0.58057(18) 0.12412(17) 0.0428(7) Uani 1 1 d . . . H40 H 0.2826 0.6276 0.1155 0.051 Uiso 1 1 calc R . . C41 C 0.2656(2) 0.52041(16) 0.08526(14) 0.0363(6) Uani 1 1 d . . . H41 H 0.3001 0.5263 0.0496 0.044 Uiso 1 1 calc R . . C42 C 0.3325(2) 0.39394(15) -0.00137(12) 0.0289(5) Uani 1 1 d . . . C43 C 0.3033(2) 0.44030(16) -0.05246(13) 0.0356(6) Uani 1 1 d . . . H43 H 0.2352 0.4575 -0.0605 0.043 Uiso 1 1 calc R . . C44 C 0.3743(3) 0.46078(19) -0.09100(14) 0.0428(7) Uani 1 1 d . . . H44 H 0.3553 0.4927 -0.1253 0.051 Uiso 1 1 calc R . . C45 C 0.4734(3) 0.4349(2) -0.07970(16) 0.0467(8) Uani 1 1 d . . . H45 H 0.5217 0.4487 -0.1067 0.056 Uiso 1 1 calc R . . C46 C 0.5023(2) 0.3892(2) -0.02947(16) 0.0435(7) Uani 1 1 d . . . H46 H 0.5704 0.3719 -0.0220 0.052 Uiso 1 1 calc R . . C47 C 0.4324(2) 0.36869(16) 0.01012(14) 0.0338(6) Uani 1 1 d . . . H47 H 0.4525 0.3376 0.0448 0.041 Uiso 1 1 calc R . . C48 C 0.28196(19) 0.29549(14) 0.09923(12) 0.0274(5) Uani 1 1 d . . . C49 C 0.2352(2) 0.22606(15) 0.09065(13) 0.0320(5) Uani 1 1 d . . . H49 H 0.1784 0.2195 0.0600 0.038 Uiso 1 1 calc R . . C50 C 0.2728(2) 0.16644(17) 0.12750(14) 0.0384(6) Uani 1 1 d . . . H50 H 0.2411 0.1191 0.1223 0.046 Uiso 1 1 calc R . . C51 C 0.3560(2) 0.17596(18) 0.17157(14) 0.0402(6) Uani 1 1 d . . . H51 H 0.3819 0.1348 0.1959 0.048 Uiso 1 1 calc R . . C52 C 0.4021(2) 0.24497(19) 0.18060(14) 0.0384(6) Uani 1 1 d . . . H52 H 0.4593 0.2510 0.2110 0.046 Uiso 1 1 calc R . . C53 C 0.3645(2) 0.30522(16) 0.14514(13) 0.0327(5) Uani 1 1 d . . . H53 H 0.3946 0.3529 0.1520 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.02456(7) 0.02802(8) 0.02622(7) -0.00019(5) 0.00158(5) 0.00160(4) P1 0.0342(3) 0.0322(3) 0.0291(3) -0.0003(3) 0.0076(3) 0.0005(3) P2 0.0260(3) 0.0269(3) 0.0252(3) 0.0002(2) 0.0022(2) 0.0008(2) O1A 0.046(2) 0.052(2) 0.070(2) -0.0130(19) 0.0037(19) 0.0069(16) O2A 0.068(2) 0.0530(19) 0.078(2) -0.0161(18) 0.0167(19) -0.0125(17) N1A 0.066(2) 0.052(2) 0.076(2) -0.0106(19) 0.006(2) -0.0017(18) O1B 0.063(2) 0.060(2) 0.068(3) -0.022(2) 0.025(2) -0.007(2) O2B 0.064(3) 0.050(2) 0.071(3) -0.012(2) -0.003(2) 0.003(2) N1B 0.056(3) 0.057(2) 0.074(3) -0.024(2) 0.011(2) 0.003(2) O3 0.0528(14) 0.110(2) 0.0618(15) 0.0361(15) 0.0120(12) -0.0012(15) O4 0.0572(16) 0.127(2) 0.100(2) 0.046(2) 0.0233(16) -0.0042(17) O5 0.0333(9) 0.0380(9) 0.0462(10) 0.0004(8) -0.0017(8) 0.0022(8) O6 0.0444(10) 0.0539(11) 0.0536(11) -0.0149(9) -0.0089(9) 0.0082(9) O7 0.0659(17) 0.103(2) 0.0825(19) 0.0345(17) 0.0064(15) -0.0094(16) O8 0.0727(17) 0.0818(18) 0.105(2) 0.0550(16) 0.0407(16) 0.0272(15) O9A 0.068(2) 0.059(2) 0.050(2) -0.0126(17) -0.0021(18) 0.0085(18) O9B 0.078(3) 0.071(3) 0.078(3) -0.022(2) -0.018(2) 0.017(2) O10 0.0628(15) 0.0587(14) 0.0624(15) -0.0076(13) -0.0230(13) 0.0161(13) N2 0.0485(16) 0.101(2) 0.0613(18) 0.0224(18) 0.0244(14) -0.0066(17) N3 0.0391(11) 0.0497(12) 0.0467(11) -0.0054(10) -0.0060(9) 0.0037(10) N4 0.073(2) 0.0470(16) 0.0629(18) 0.0015(14) 0.0215(16) -0.0021(15) N5A 0.072(2) 0.061(2) 0.058(2) -0.0126(19) -0.015(2) 0.0171(19) N5B 0.071(3) 0.071(3) 0.076(3) -0.024(3) -0.021(3) 0.016(2) N6 0.0325(12) 0.0538(16) 0.0532(16) -0.0176(13) 0.0035(11) 0.0044(11) C1 0.0313(14) 0.0385(16) 0.081(3) -0.0065(16) 0.0104(15) -0.0003(12) C2 0.044(2) 0.0416(19) 0.141(5) -0.004(2) 0.034(3) 0.0051(15) C3 0.084(4) 0.077(4) 0.168(7) -0.060(4) 0.059(4) 0.003(3) C4 0.091(4) 0.117(5) 0.106(5) -0.057(4) 0.028(3) 0.025(4) C5 0.059(2) 0.096(3) 0.058(2) -0.032(2) 0.0125(19) 0.018(2) C6 0.0368(14) 0.0335(13) 0.0301(13) -0.0007(10) 0.0055(11) 0.0009(10) C7 0.0402(15) 0.0505(18) 0.0330(14) -0.0029(12) 0.0084(12) -0.0051(13) C8 0.0407(16) 0.0527(19) 0.0463(17) -0.0020(15) 0.0052(13) -0.0068(14) C9 0.0462(17) 0.0413(16) 0.0440(17) -0.0037(13) -0.0051(13) 0.0001(13) C10 0.0510(18) 0.0428(16) 0.0322(14) -0.0057(12) 0.0012(12) 0.0074(13) C11 0.0438(16) 0.0430(15) 0.0311(13) -0.0037(12) 0.0079(12) 0.0048(13) C12 0.0388(14) 0.0326(13) 0.0319(13) -0.0004(10) 0.0094(11) 0.0035(11) C13 0.0529(18) 0.0372(15) 0.0330(14) -0.0014(11) 0.0098(13) 0.0003(13) C14 0.069(2) 0.0352(15) 0.0414(16) 0.0023(13) 0.0176(16) 0.0045(15) C15 0.059(2) 0.0476(18) 0.0388(16) 0.0081(13) 0.0189(15) 0.0185(15) C16 0.0421(16) 0.0552(19) 0.0388(15) 0.0044(14) 0.0076(13) 0.0119(14) C17 0.0410(15) 0.0399(15) 0.0378(15) -0.0003(12) 0.0057(12) 0.0037(12) C18 0.0394(14) 0.0352(13) 0.0340(13) -0.0008(11) 0.0100(11) -0.0015(11) C19 0.0479(17) 0.0437(16) 0.0430(16) 0.0065(13) 0.0135(14) 0.0023(13) C20 0.065(2) 0.0456(18) 0.0422(17) 0.0043(14) 0.0192(16) -0.0051(16) C21 0.055(2) 0.0534(19) 0.0451(17) -0.0050(15) 0.0214(15) -0.0159(16) C22 0.0389(16) 0.057(2) 0.0504(18) -0.0079(16) 0.0159(14) -0.0089(14) C23 0.0388(15) 0.0438(16) 0.0391(15) -0.0048(13) 0.0096(12) -0.0032(12) C24 0.0341(13) 0.0338(13) 0.0320(13) -0.0024(10) 0.0028(10) 0.0026(10) C25 0.0396(14) 0.0387(14) 0.0342(13) -0.0039(11) 0.0070(11) -0.0031(11) C26 0.0396(15) 0.0493(17) 0.0360(14) -0.0083(13) 0.0077(12) 0.0012(13) C27 0.0442(16) 0.0420(16) 0.0408(16) -0.0100(13) -0.0026(13) 0.0101(13) C28 0.0518(18) 0.0329(14) 0.0452(17) -0.0017(13) -0.0021(14) 0.0050(13) C29 0.0432(15) 0.0360(14) 0.0371(14) 0.0024(12) 0.0041(12) 0.0014(12) C30 0.0284(12) 0.0339(12) 0.0275(12) 0.0006(10) 0.0001(9) 0.0015(10) C31 0.0292(13) 0.060(2) 0.0354(15) -0.0072(13) 0.0019(11) 0.0070(12) C32 0.0285(14) 0.084(3) 0.0477(19) -0.0089(18) -0.0013(13) 0.0050(16) C33 0.0352(15) 0.069(2) 0.0458(18) -0.0074(17) -0.0082(13) -0.0014(15) C34 0.0424(16) 0.0478(17) 0.0357(14) -0.0076(13) -0.0071(12) 0.0007(13) C35 0.0344(13) 0.0399(14) 0.0344(13) -0.0056(11) 0.0012(11) 0.0024(11) C36 0.0292(12) 0.0291(12) 0.0309(12) -0.0032(10) 0.0003(9) 0.0026(9) C37 0.0439(15) 0.0349(14) 0.0340(13) -0.0040(11) 0.0086(12) 0.0011(11) C38 0.0478(17) 0.0460(17) 0.0376(15) -0.0094(13) 0.0084(13) 0.0075(13) C39 0.0431(16) 0.0413(16) 0.0475(17) -0.0159(14) -0.0003(13) 0.0062(13) C40 0.0409(15) 0.0319(14) 0.0547(19) -0.0083(13) 0.0025(14) -0.0023(11) C41 0.0364(14) 0.0319(13) 0.0401(14) -0.0035(11) 0.0030(11) -0.0017(11) C42 0.0311(12) 0.0282(12) 0.0275(11) 0.0002(9) 0.0043(9) -0.0011(9) C43 0.0377(14) 0.0353(14) 0.0332(13) 0.0054(11) 0.0015(11) -0.0006(11) C44 0.0483(17) 0.0460(17) 0.0334(14) 0.0113(13) 0.0025(12) -0.0078(13) C45 0.0427(16) 0.059(2) 0.0394(16) 0.0093(15) 0.0103(13) -0.0121(15) C46 0.0311(14) 0.0556(19) 0.0450(17) 0.0080(15) 0.0099(12) -0.0005(13) C47 0.0317(13) 0.0364(14) 0.0334(13) 0.0057(10) 0.0046(10) 0.0008(10) C48 0.0272(11) 0.0287(11) 0.0267(11) 0.0014(9) 0.0047(9) 0.0017(9) C49 0.0351(13) 0.0317(12) 0.0293(12) -0.0004(10) 0.0045(10) -0.0015(10) C50 0.0485(16) 0.0301(13) 0.0377(14) 0.0037(11) 0.0098(12) 0.0006(12) C51 0.0430(15) 0.0405(15) 0.0381(15) 0.0115(12) 0.0092(12) 0.0111(12) C52 0.0322(13) 0.0487(16) 0.0334(14) 0.0087(12) 0.0005(11) 0.0040(12) C53 0.0293(12) 0.0367(13) 0.0319(13) 0.0040(11) 0.0031(10) -0.0017(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 Nd O3 2.530(3) . ? Nd O2A 2.533(5) . ? Nd O1B 2.554(6) . ? Nd O10 2.567(3) . ? Nd O9A 2.571(5) . ? Nd O6 2.575(2) . ? Nd O8 2.579(3) . ? Nd O1A 2.581(5) . ? Nd O4 2.585(3) . ? Nd O2B 2.596(7) . ? Nd O5 2.636(2) . ? Nd O7 2.646(3) . ? Nd O9B 2.609(4) . ? Nd N6 2.743(3) . ? P1 C12 1.794(3) . ? P1 C18 1.796(3) . ? P1 C24 1.797(3) . ? P1 C6 1.798(3) . ? P2 C30 1.790(3) . ? P2 C42 1.792(3) . ? P2 C36 1.793(3) . ? P2 C48 1.793(3) . ? O1A N1A 1.230(5) . ? O2A N1A 1.243(4) . ? O1B N1B 1.227(5) . ? O2B N1B 1.247(5) . ? O3 N2 1.210(4) . ? O4 N2 1.256(5) . ? O5 N3 1.248(4) . ? O6 N3 1.276(4) . ? O7 N4 1.246(5) . ? O8 N4 1.220(5) . ? O9A N5A 1.277(6) . ? O9B N5B 1.273(8) . ? O10 N5B 1.255(8) . ? O10 N5A 1.333(6) . ? N6 C1 1.335(5) . ? N6 C5 1.344(5) . ? C1 C2 1.400(5) . ? C1 H1 0.9500 . ? C2 C3 1.360(10) . ? C2 H2 0.9500 . ? C3 C4 1.393(11) . ? C3 H3 0.9500 . ? C4 C5 1.386(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.392(4) . ? C6 C11 1.401(4) . ? C7 C8 1.389(5) . ? C7 H7 0.9500 . ? C8 C9 1.384(5) . ? C8 H8 0.9500 . ? C9 C10 1.373(5) . ? C9 H9 0.9500 . ? C10 C11 1.386(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.395(4) . ? C12 C17 1.399(4) . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.382(5) . ? C14 H14 0.9500 . ? C15 C16 1.387(5) . ? C15 H15 0.9500 . ? C16 C17 1.392(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.395(4) . ? C18 C19 1.403(4) . ? C19 C20 1.383(5) . ? C19 H19 0.9500 . ? C20 C21 1.382(6) . ? C20 H20 0.9500 . ? C21 C22 1.375(5) . ? C21 H21 0.9500 . ? C22 C23 1.395(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.394(4) . ? C24 C25 1.400(4) . ? C25 C26 1.392(4) . ? C25 H25 0.9500 . ? C26 C27 1.380(5) . ? C26 H26 0.9500 . ? C27 C28 1.386(5) . ? C27 H27 0.9500 . ? C28 C29 1.396(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.395(4) . ? C30 C35 1.396(4) . ? C31 C32 1.391(5) . ? C31 H31 0.9500 . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C33 C34 1.378(5) . ? C33 H33 0.9500 . ? C34 C35 1.386(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.389(4) . ? C36 C37 1.389(4) . ? C37 C38 1.396(4) . ? C37 H37 0.9500 . ? C38 C39 1.379(5) . ? C38 H38 0.9500 . ? C39 C40 1.383(5) . ? C39 H39 0.9500 . ? C40 C41 1.389(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.393(4) . ? C42 C43 1.404(4) . ? C43 C44 1.381(4) . ? C43 H43 0.9500 . ? C44 C45 1.385(5) . ? C44 H44 0.9500 . ? C45 C46 1.382(5) . ? C45 H45 0.9500 . ? C46 C47 1.385(4) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.396(4) . ? C48 C53 1.400(4) . ? C49 C50 1.394(4) . ? C49 H49 0.9500 . ? C50 C51 1.381(5) . ? C50 H50 0.9500 . ? C51 C52 1.386(5) . ? C51 H51 0.9500 . ? C52 C53 1.386(4) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd O2A 76.07(16) . . ? O3 Nd O1B 119.59(17) . . ? O2A Nd O1B 66.74(17) . . ? O3 Nd O10 116.23(11) . . ? O2A Nd O10 73.35(13) . . ? O1B Nd O10 96.87(19) . . ? O3 Nd O9A 143.84(15) . . ? O2A Nd O9A 67.89(18) . . ? O10 Nd O9A 50.73(12) . . ? O3 Nd O6 73.56(11) . . ? O2A Nd O6 145.59(14) . . ? O1B Nd O6 116.13(18) . . ? O10 Nd O6 135.57(8) . . ? O9A Nd O6 141.49(14) . . ? O3 Nd O8 151.68(14) . . ? O2A Nd O8 130.21(16) . . ? O1B Nd O8 84.93(16) . . ? O10 Nd O8 70.39(12) . . ? O9A Nd O8 62.89(16) . . ? O6 Nd O8 83.17(12) . . ? O3 Nd O1A 85.50(17) . . ? O2A Nd O1A 47.83(10) . . ? O10 Nd O1A 110.60(13) . . ? O9A Nd O1A 72.72(18) . . ? O6 Nd O1A 113.40(12) . . ? O8 Nd O1A 119.12(16) . . ? O3 Nd O4 46.62(11) . . ? O2A Nd O4 65.08(15) . . ? O1B Nd O4 131.82(18) . . ? O10 Nd O4 69.79(12) . . ? O9A Nd O4 111.55(15) . . ? O6 Nd O4 103.38(13) . . ? O8 Nd O4 127.92(12) . . ? O1A Nd O4 105.51(16) . . ? O3 Nd O2B 74.33(17) . . ? O1B Nd O2B 46.87(13) . . ? O10 Nd O2B 108.3(2) . . ? O6 Nd O2B 115.9(2) . . ? O8 Nd O2B 131.78(16) . . ? O4 Nd O2B 92.2(2) . . ? O3 Nd O5 71.06(9) . . ? O2A Nd O5 106.68(12) . . ? O1B Nd O5 76.16(18) . . ? O10 Nd O5 172.07(9) . . ? O9A Nd O5 121.64(11) . . ? O6 Nd O5 47.72(7) . . ? O8 Nd O5 104.83(10) . . ? O1A Nd O5 65.70(12) . . ? O4 Nd O5 117.65(10) . . ? O2B Nd O5 69.8(2) . . ? O3 Nd O7 133.92(10) . . ? O2A Nd O7 124.00(14) . . ? O1B Nd O7 57.32(17) . . ? O10 Nd O7 109.53(11) . . ? O9A Nd O7 72.89(15) . . ? O6 Nd O7 70.32(11) . . ? O8 Nd O7 45.87(11) . . ? O1A Nd O7 83.52(15) . . ? O4 Nd O7 170.69(15) . . ? O2B Nd O7 96.8(2) . . ? O5 Nd O7 63.63(9) . . ? O3 Nd O9B 110.3(2) . . ? O1B Nd O9B 61.8(2) . . ? O10 Nd O9B 43.72(15) . . ? O6 Nd O9B 176.1(2) . . ? O8 Nd O9B 93.3(2) . . ? O4 Nd O9B 80.0(2) . . ? O2B Nd O9B 65.4(3) . . ? O5 Nd O9B 132.33(15) . . ? O7 Nd O9B 106.1(2) . . ? O3 Nd N6 84.62(11) . . ? O2A Nd N6 127.48(11) . . ? O1B Nd N6 155.59(16) . . ? O10 Nd N6 72.61(9) . . ? O9A Nd N6 114.97(12) . . ? O6 Nd N6 65.11(8) . . ? O8 Nd N6 70.85(11) . . ? O1A Nd N6 169.99(16) . . ? O4 Nd N6 66.20(13) . . ? O2B Nd N6 157.01(17) . . ? O5 Nd N6 112.29(8) . . ? O7 Nd N6 104.58(12) . . ? O9B Nd N6 115.29(15) . . ? C12 P1 C18 110.05(14) . . ? C12 P1 C24 107.25(13) . . ? C18 P1 C24 110.54(14) . . ? C12 P1 C6 109.05(14) . . ? C18 P1 C6 107.49(14) . . ? C24 P1 C6 112.45(13) . . ? C30 P2 C42 108.42(13) . . ? C30 P2 C36 111.24(13) . . ? C42 P2 C36 109.15(13) . . ? C30 P2 C48 109.31(13) . . ? C42 P2 C48 110.63(12) . . ? C36 P2 C48 108.09(12) . . ? N1A O1A Nd 98.1(3) . . ? N1A O2A Nd 100.2(3) . . ? O1A N1A O2A 113.9(5) . . ? N1B O1B Nd 101.9(4) . . ? N1B O2B Nd 99.1(4) . . ? O1B N1B O2B 111.8(5) . . ? N2 O3 Nd 102.8(2) . . ? N2 O4 Nd 98.6(2) . . ? N3 O5 Nd 98.32(17) . . ? N3 O6 Nd 100.50(19) . . ? N4 O7 Nd 99.1(3) . . ? N4 O8 Nd 103.4(2) . . ? N5A O9A Nd 97.7(4) . . ? N5B O9B Nd 99.3(5) . . ? N5B O10 Nd 102.0(4) . . ? N5A O10 Nd 96.4(3) . . ? O3 N2 O4 110.4(3) . . ? O5 N3 O6 113.3(3) . . ? O8 N4 O7 111.3(3) . . ? O9A N5A O10 114.9(5) . . ? O10 N5B O9B 99.3(7) . . ? C1 N6 C5 118.3(4) . . ? C1 N6 Nd 121.8(2) . . ? C5 N6 Nd 119.8(3) . . ? N6 C1 C2 122.2(4) . . ? N6 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.0(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.0(6) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N6 C5 C4 122.8(6) . . ? N6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C7 C6 C11 119.6(3) . . ? C7 C6 P1 120.7(2) . . ? C11 C6 P1 119.5(2) . . ? C8 C7 C6 119.5(3) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 120.4(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 119.9(3) . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? C13 C12 C17 120.1(3) . . ? C13 C12 P1 121.6(2) . . ? C17 C12 P1 118.2(2) . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.6(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C12 120.0(3) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C23 C18 C19 119.6(3) . . ? C23 C18 P1 121.0(2) . . ? C19 C18 P1 119.3(2) . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 119.6(3) . . ? C18 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C29 C24 C25 120.3(3) . . ? C29 C24 P1 121.3(2) . . ? C25 C24 P1 118.4(2) . . ? C26 C25 C24 119.5(3) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 C25 120.1(3) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.6(3) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 120.1(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 119.4(3) . . ? C24 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C31 C30 C35 120.2(3) . . ? C31 C30 P2 121.1(2) . . ? C35 C30 P2 118.7(2) . . ? C32 C31 C30 119.0(3) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.6(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.8(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C30 120.0(3) . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C41 C36 C37 120.7(3) . . ? C41 C36 P2 120.6(2) . . ? C37 C36 P2 118.7(2) . . ? C36 C37 C38 119.2(3) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 119.9(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.8(3) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C39 C40 C41 119.7(3) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C36 C41 C40 119.6(3) . . ? C36 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C47 C42 C43 120.1(3) . . ? C47 C42 P2 121.3(2) . . ? C43 C42 P2 118.5(2) . . ? C44 C43 C42 119.6(3) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 120.1(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 120.3(3) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C42 119.5(3) . . ? C46 C47 H47 120.3 . . ? C42 C47 H47 120.3 . . ? C49 C48 C53 120.2(2) . . ? C49 C48 P2 120.8(2) . . ? C53 C48 P2 118.9(2) . . ? C50 C49 C48 119.2(3) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C51 C50 C49 120.2(3) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C50 C51 C52 120.7(3) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C51 C52 C53 119.8(3) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C52 C53 C48 119.8(3) . . ? C52 C53 H53 120.1 . . ? C48 C53 H53 120.1 . . ? _database_code_depnum_ccdc_archive 'CCDC 963100' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N6 Nd O10 P2' _chemical_formula_weight 1132.13 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' Nd Nd -0.1943 3.0179 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0031(4) _cell_length_b 12.8890(7) _cell_length_c 21.3346(11) _cell_angle_alpha 87.813(2) _cell_angle_beta 77.576(3) _cell_angle_gamma 68.306(3) _cell_volume 2493.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 159280 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 30.51 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method '2 \f and 13 \w scans with 2\% steps (745 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 159280 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_unetI/netI 0.0660 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.51 _reflns_number_total 15217 _reflns_number_gt 12029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Atom N5 is disordered over two positions which were refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for the disordered ones (SIMU .01 .01 1.2 N5A N5B). The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0267P)^2^] 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 15217 _refine_ls_number_parameters 659 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.561 _refine_diff_density_min -1.045 _refine_diff_density_rms 0.110 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 Nd Nd 0.243341(11) 0.463170(9) 0.275703(5) 0.02442(3) Uani 1 1 d . . . P1 P 0.20069(5) 0.16782(4) 0.98238(2) 0.02539(10) Uani 1 1 d . . . P2 P 0.29738(5) 0.90272(4) 0.41122(2) 0.02566(10) Uani 1 1 d . . . O1 O 0.36495(18) 0.46674(14) 0.36917(7) 0.0440(4) Uani 1 1 d . . . O2 O 0.38460(19) 0.58113(14) 0.29788(8) 0.0475(4) Uani 1 1 d . . . O3 O 0.04638(19) 0.60854(14) 0.35765(8) 0.0497(4) Uani 1 1 d . . . O4 O 0.08090(17) 0.44258(15) 0.38200(7) 0.0423(4) Uani 1 1 d . . . O5 O 0.48909(16) 0.29238(13) 0.26966(7) 0.0402(4) Uani 1 1 d . . . O6 O 0.29644(17) 0.25553(13) 0.29452(7) 0.0374(3) Uani 1 1 d . . . O7 O 0.44713(16) 0.45231(13) 0.17109(7) 0.0368(3) Uani 1 1 d . . . O8 O 0.29977(15) 0.37503(12) 0.16212(6) 0.0319(3) Uani 1 1 d . . . O9 O 0.13623(19) 0.62570(14) 0.21891(8) 0.0514(4) Uani 1 1 d . . . O10 O 0.0942(2) 0.74669(16) 0.15012(10) 0.0684(6) Uani 1 1 d . . . N1 N 0.4162(2) 0.54111(18) 0.35063(10) 0.0475(5) Uani 1 1 d . . . N2 N 0.0106(2) 0.5443(2) 0.39811(10) 0.0516(5) Uani 1 1 d . . . N3 N 0.4357(2) 0.21863(16) 0.28648(8) 0.0415(4) Uani 1 1 d . . . N4 N 0.40996(19) 0.39842(15) 0.13473(8) 0.0352(4) Uani 1 1 d . . . N5A N 0.1333(4) 0.6522(3) 0.16379(15) 0.0538(12) Uani 0.800(10) 1 d PU . . N5B N 0.1653(13) 0.6873(13) 0.1910(8) 0.053(4) Uani 0.200(10) 1 d PU . . N6 N 0.00778(17) 0.42860(14) 0.25152(7) 0.0279(4) Uani 1 1 d . . . C1 C -0.0721(2) 0.37831(18) 0.29066(10) 0.0335(5) Uani 1 1 d . . . H1 H -0.0429 0.3499 0.3294 0.040 Uiso 1 1 calc R . . C2 C -0.1947(2) 0.3660(2) 0.27723(11) 0.0412(5) Uani 1 1 d . . . H2 H -0.2490 0.3312 0.3067 0.049 Uiso 1 1 calc R . . C3 C -0.2375(2) 0.40412(19) 0.22118(11) 0.0400(5) Uani 1 1 d . . . H3 H -0.3219 0.3968 0.2113 0.048 Uiso 1 1 calc R . . C4 C -0.1549(2) 0.45360(19) 0.17923(11) 0.0365(5) Uani 1 1 d . . . H4 H -0.1798 0.4791 0.1394 0.044 Uiso 1 1 calc R . . C5 C -0.0350(2) 0.46508(18) 0.19662(9) 0.0308(4) Uani 1 1 d . . . H5 H 0.0198 0.5007 0.1681 0.037 Uiso 1 1 calc R . . C6 C 0.3337(2) 0.22668(17) 0.94550(11) 0.0334(5) Uani 1 1 d . . . C7 C 0.3412(2) 0.2484(2) 0.88024(12) 0.0445(6) Uani 1 1 d . . . H7 H 0.2793 0.2302 0.8581 0.053 Uiso 1 1 calc R . . C8 C 0.4378(3) 0.2960(2) 0.84767(15) 0.0613(8) Uani 1 1 d . . . H8 H 0.4417 0.3116 0.8036 0.074 Uiso 1 1 calc R . . C9 C 0.5274(3) 0.3202(2) 0.8798(2) 0.0739(10) Uani 1 1 d . . . H9 H 0.5935 0.3534 0.8577 0.089 Uiso 1 1 calc R . . C10 C 0.5248(3) 0.2979(2) 0.94307(19) 0.0670(9) Uani 1 1 d . . . H10 H 0.5904 0.3141 0.9638 0.080 Uiso 1 1 calc R . . C11 C 0.4250(2) 0.25074(19) 0.97822(14) 0.0476(6) Uani 1 1 d . . . H11 H 0.4210 0.2363 1.0224 0.057 Uiso 1 1 calc R . . C12 C 0.2219(2) 0.05687(16) 0.92838(9) 0.0248(4) Uani 1 1 d . . . C13 C 0.1040(2) 0.05168(17) 0.90575(9) 0.0275(4) Uani 1 1 d . . . H13 H 0.0076 0.1058 0.9203 0.033 Uiso 1 1 calc R . . C14 C 0.1286(2) -0.03334(18) 0.86172(9) 0.0316(4) Uani 1 1 d . . . H14 H 0.0489 -0.0365 0.8454 0.038 Uiso 1 1 calc R . . C15 C 0.2677(2) -0.11342(18) 0.84131(9) 0.0314(4) Uani 1 1 d . . . H15 H 0.2828 -0.1718 0.8116 0.038 Uiso 1 1 calc R . . C16 C 0.3859(2) -0.10907(17) 0.86407(9) 0.0307(4) Uani 1 1 d . . . H16 H 0.4815 -0.1645 0.8500 0.037 Uiso 1 1 calc R . . C17 C 0.3637(2) -0.02383(17) 0.90719(9) 0.0301(4) Uani 1 1 d . . . H17 H 0.4443 -0.0199 0.9224 0.036 Uiso 1 1 calc R . . C18 C 0.2259(2) 0.11511(17) 1.05977(9) 0.0272(4) Uani 1 1 d . . . C19 C 0.2540(2) 0.00306(17) 1.07246(9) 0.0289(4) Uani 1 1 d . . . H19 H 0.2675 -0.0488 1.0390 0.035 Uiso 1 1 calc R . . C20 C 0.2620(2) -0.03223(18) 1.13437(10) 0.0337(5) Uani 1 1 d . . . H20 H 0.2805 -0.1084 1.1434 0.040 Uiso 1 1 calc R . . C21 C 0.2433(2) 0.04301(19) 1.18269(10) 0.0361(5) Uani 1 1 d . . . H21 H 0.2497 0.0182 1.2248 0.043 Uiso 1 1 calc R . . C22 C 0.2156(2) 0.15365(19) 1.17045(10) 0.0377(5) Uani 1 1 d . . . H22 H 0.2037 0.2048 1.2040 0.045 Uiso 1 1 calc R . . C23 C 0.2051(2) 0.19089(19) 1.10915(10) 0.0372(5) Uani 1 1 d . . . H23 H 0.1837 0.2677 1.1009 0.045 Uiso 1 1 calc R . . C24 C 0.0192(2) 0.27244(16) 0.99465(9) 0.0265(4) Uani 1 1 d . . . C25 C -0.0115(2) 0.37285(18) 0.96513(11) 0.0392(5) Uani 1 1 d . . . H25 H 0.0654 0.3890 0.9372 0.047 Uiso 1 1 calc R . . C26 C -0.1556(3) 0.4509(2) 0.97615(13) 0.0470(6) Uani 1 1 d . . . H26 H -0.1769 0.5198 0.9553 0.056 Uiso 1 1 calc R . . C27 C -0.2662(2) 0.42837(19) 1.01685(11) 0.0413(5) Uani 1 1 d . . . H27 H -0.3642 0.4817 1.0242 0.050 Uiso 1 1 calc R . . C28 C -0.2362(3) 0.3288(2) 1.04719(11) 0.0470(6) Uani 1 1 d . . . H28 H -0.3134 0.3138 1.0757 0.056 Uiso 1 1 calc R . . C29 C -0.0947(2) 0.2507(2) 1.03634(10) 0.0408(5) Uani 1 1 d . . . H29 H -0.0744 0.1819 1.0573 0.049 Uiso 1 1 calc R . . C30 C 0.1510(2) 0.94562(17) 0.36822(9) 0.0279(4) Uani 1 1 d . . . C31 C 0.1537(3) 0.8715(2) 0.32127(10) 0.0375(5) Uani 1 1 d . . . H31 H 0.2333 0.8016 0.3115 0.045 Uiso 1 1 calc R . . C32 C 0.0395(3) 0.9010(2) 0.28911(11) 0.0501(7) Uani 1 1 d . . . H32 H 0.0394 0.8506 0.2577 0.060 Uiso 1 1 calc R . . C33 C -0.0737(3) 1.0031(3) 0.30269(11) 0.0526(7) Uani 1 1 d . . . H33 H -0.1507 1.0234 0.2798 0.063 Uiso 1 1 calc R . . C34 C -0.0779(3) 1.0767(2) 0.34867(12) 0.0466(6) Uani 1 1 d . . . H34 H -0.1574 1.1468 0.3577 0.056 Uiso 1 1 calc R . . C35 C 0.0356(2) 1.04776(19) 0.38200(10) 0.0365(5) Uani 1 1 d . . . H35 H 0.0336 1.0979 0.4140 0.044 Uiso 1 1 calc R . . C36 C 0.4723(2) 0.84978(17) 0.35417(9) 0.0278(4) Uani 1 1 d . . . C37 C 0.5167(2) 0.9233(2) 0.31298(10) 0.0394(5) Uani 1 1 d . . . H37 H 0.4535 0.9995 0.3133 0.047 Uiso 1 1 calc R . . C38 C 0.6542(3) 0.8840(2) 0.27151(11) 0.0456(6) Uani 1 1 d . . . H38 H 0.6851 0.9336 0.2432 0.055 Uiso 1 1 calc R . . C39 C 0.7461(2) 0.7739(2) 0.27107(11) 0.0440(6) Uani 1 1 d . . . H39 H 0.8415 0.7484 0.2437 0.053 Uiso 1 1 calc R . . C40 C 0.7003(2) 0.7008(2) 0.31003(11) 0.0430(5) Uani 1 1 d . . . H40 H 0.7632 0.6245 0.3087 0.052 Uiso 1 1 calc R . . C41 C 0.5624(2) 0.73800(19) 0.35132(10) 0.0353(5) Uani 1 1 d . . . H41 H 0.5301 0.6869 0.3775 0.042 Uiso 1 1 calc R . . C42 C 0.2822(2) 0.79256(17) 0.46310(9) 0.0277(4) Uani 1 1 d . . . C43 C 0.1674(2) 0.75438(18) 0.46673(9) 0.0318(4) Uani 1 1 d . . . H43 H 0.0931 0.7889 0.4431 0.038 Uiso 1 1 calc R . . C44 C 0.1619(3) 0.66560(19) 0.50505(10) 0.0385(5) Uani 1 1 d . . . H44 H 0.0838 0.6394 0.5077 0.046 Uiso 1 1 calc R . . C45 C 0.2699(3) 0.6158(2) 0.53915(10) 0.0420(5) Uani 1 1 d . . . H45 H 0.2662 0.5547 0.5649 0.050 Uiso 1 1 calc R . . C46 C 0.3839(2) 0.6536(2) 0.53642(10) 0.0410(5) Uani 1 1 d . . . H46 H 0.4575 0.6189 0.5603 0.049 Uiso 1 1 calc R . . C47 C 0.3900(2) 0.74226(19) 0.49864(10) 0.0355(5) Uani 1 1 d . . . H47 H 0.4675 0.7689 0.4969 0.043 Uiso 1 1 calc R . . C48 C 0.2841(2) 1.02184(17) 0.45715(9) 0.0276(4) Uani 1 1 d . . . C49 C 0.2732(2) 1.01951(19) 0.52291(9) 0.0357(5) Uani 1 1 d . . . H49 H 0.2785 0.9526 0.5443 0.043 Uiso 1 1 calc R . . C50 C 0.2547(3) 1.1143(2) 0.55771(10) 0.0428(6) Uani 1 1 d . . . H50 H 0.2475 1.1119 0.6028 0.051 Uiso 1 1 calc R . . C51 C 0.2467(2) 1.21212(19) 0.52716(10) 0.0379(5) Uani 1 1 d . . . H51 H 0.2334 1.2770 0.5513 0.046 Uiso 1 1 calc R . . C52 C 0.2581(3) 1.2156(2) 0.46192(11) 0.0416(5) Uani 1 1 d . . . H52 H 0.2540 1.2827 0.4409 0.050 Uiso 1 1 calc R . . C53 C 0.2756(3) 1.12159(19) 0.42648(10) 0.0396(5) Uani 1 1 d . . . H53 H 0.2818 1.1248 0.3814 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.02269(5) 0.02383(6) 0.02620(6) 0.00000(4) -0.00580(4) -0.00760(4) P1 0.0244(2) 0.0224(3) 0.0285(2) 0.0006(2) -0.0076(2) -0.0066(2) P2 0.0259(2) 0.0276(3) 0.0230(2) 0.0025(2) -0.00455(19) -0.0100(2) O1 0.0469(9) 0.0465(10) 0.0419(9) 0.0011(7) -0.0221(7) -0.0140(8) O2 0.0540(10) 0.0452(11) 0.0559(10) 0.0037(8) -0.0202(8) -0.0281(9) O3 0.0494(10) 0.0404(10) 0.0446(10) -0.0073(8) -0.0049(8) -0.0019(8) O4 0.0427(9) 0.0526(11) 0.0309(8) -0.0019(7) -0.0017(7) -0.0198(9) O5 0.0329(8) 0.0323(9) 0.0478(9) 0.0016(7) -0.0039(7) -0.0061(7) O6 0.0462(9) 0.0357(9) 0.0331(8) 0.0063(7) -0.0087(7) -0.0188(8) O7 0.0305(8) 0.0398(9) 0.0435(8) 0.0079(7) -0.0078(7) -0.0178(7) O8 0.0297(7) 0.0356(9) 0.0300(7) -0.0013(6) 0.0001(6) -0.0149(7) O9 0.0619(12) 0.0347(10) 0.0478(10) 0.0094(8) -0.0191(9) -0.0037(9) O10 0.0942(16) 0.0386(12) 0.0696(13) 0.0231(10) -0.0388(12) -0.0118(11) N1 0.0415(11) 0.0513(14) 0.0534(13) -0.0086(10) -0.0184(10) -0.0159(10) N2 0.0412(12) 0.0634(16) 0.0397(11) -0.0100(11) -0.0034(9) -0.0094(11) N3 0.0497(12) 0.0323(11) 0.0332(10) 0.0016(8) -0.0038(9) -0.0076(9) N4 0.0295(9) 0.0366(11) 0.0367(10) 0.0048(8) -0.0028(8) -0.0119(8) N5A 0.080(2) 0.0391(18) 0.0342(17) 0.0052(13) -0.0081(15) -0.0155(15) N5B 0.052(6) 0.057(7) 0.061(7) 0.019(6) -0.016(5) -0.031(5) N6 0.0258(8) 0.0293(9) 0.0286(8) 0.0003(7) -0.0045(7) -0.0110(7) C1 0.0328(11) 0.0351(12) 0.0331(11) 0.0061(9) -0.0070(9) -0.0138(10) C2 0.0322(11) 0.0419(14) 0.0536(14) 0.0061(11) -0.0049(10) -0.0210(11) C3 0.0280(11) 0.0384(13) 0.0580(14) 0.0019(11) -0.0147(10) -0.0142(10) C4 0.0341(11) 0.0369(13) 0.0425(12) 0.0045(10) -0.0173(10) -0.0129(10) C5 0.0287(10) 0.0341(12) 0.0318(10) 0.0037(9) -0.0087(8) -0.0130(9) C6 0.0256(10) 0.0218(11) 0.0505(13) 0.0000(9) -0.0070(9) -0.0066(8) C7 0.0354(12) 0.0394(14) 0.0525(14) 0.0117(11) -0.0017(11) -0.0119(11) C8 0.0390(14) 0.0438(16) 0.087(2) 0.0241(15) 0.0061(14) -0.0117(12) C9 0.0426(16) 0.0236(14) 0.139(3) 0.0149(17) 0.0042(18) -0.0082(12) C10 0.0321(13) 0.0285(14) 0.143(3) -0.0162(17) -0.0250(17) -0.0090(11) C11 0.0332(12) 0.0257(12) 0.0825(18) -0.0105(12) -0.0186(12) -0.0046(10) C12 0.0247(9) 0.0244(10) 0.0242(9) 0.0010(7) -0.0052(7) -0.0077(8) C13 0.0239(9) 0.0291(11) 0.0276(9) 0.0039(8) -0.0060(8) -0.0076(8) C14 0.0299(10) 0.0371(12) 0.0288(10) -0.0003(9) -0.0059(8) -0.0136(9) C15 0.0367(11) 0.0295(11) 0.0282(10) -0.0024(8) -0.0034(8) -0.0143(10) C16 0.0255(10) 0.0278(11) 0.0327(10) -0.0031(8) -0.0037(8) -0.0040(8) C17 0.0238(10) 0.0310(11) 0.0335(10) -0.0009(9) -0.0079(8) -0.0068(9) C18 0.0264(10) 0.0264(11) 0.0284(10) -0.0004(8) -0.0098(8) -0.0069(8) C19 0.0252(10) 0.0256(11) 0.0334(10) -0.0021(8) -0.0062(8) -0.0061(8) C20 0.0326(11) 0.0292(12) 0.0356(11) 0.0077(9) -0.0089(9) -0.0068(9) C21 0.0322(11) 0.0423(14) 0.0314(11) 0.0053(10) -0.0104(9) -0.0097(10) C22 0.0435(13) 0.0393(13) 0.0308(11) -0.0033(9) -0.0122(9) -0.0130(11) C23 0.0444(13) 0.0294(12) 0.0383(12) -0.0008(9) -0.0142(10) -0.0112(10) C24 0.0259(9) 0.0238(10) 0.0266(9) -0.0029(8) -0.0077(8) -0.0041(8) C25 0.0334(12) 0.0297(12) 0.0518(13) 0.0090(10) -0.0109(10) -0.0085(10) C26 0.0435(13) 0.0269(13) 0.0695(17) 0.0079(11) -0.0239(12) -0.0058(11) C27 0.0303(11) 0.0328(13) 0.0525(14) -0.0150(10) -0.0150(10) 0.0027(10) C28 0.0324(12) 0.0500(16) 0.0443(13) -0.0005(11) 0.0004(10) -0.0036(11) C29 0.0317(11) 0.0412(14) 0.0375(12) 0.0095(10) -0.0032(9) -0.0030(10) C30 0.0290(10) 0.0327(12) 0.0233(9) 0.0055(8) -0.0054(8) -0.0136(9) C31 0.0458(13) 0.0391(13) 0.0325(11) 0.0029(9) -0.0107(10) -0.0202(11) C32 0.0627(17) 0.0669(19) 0.0387(13) 0.0091(12) -0.0211(12) -0.0396(16) C33 0.0499(15) 0.083(2) 0.0395(13) 0.0227(14) -0.0226(12) -0.0352(16) C34 0.0328(12) 0.0532(16) 0.0480(14) 0.0199(12) -0.0112(10) -0.0098(11) C35 0.0336(11) 0.0385(13) 0.0353(11) 0.0059(10) -0.0067(9) -0.0119(10) C36 0.0268(10) 0.0317(11) 0.0253(9) -0.0004(8) -0.0041(8) -0.0121(9) C37 0.0365(12) 0.0374(13) 0.0395(12) 0.0050(10) 0.0015(10) -0.0139(10) C38 0.0416(13) 0.0541(17) 0.0401(13) 0.0036(11) 0.0043(10) -0.0238(13) C39 0.0312(12) 0.0590(17) 0.0369(12) -0.0108(11) 0.0031(9) -0.0157(12) C40 0.0373(12) 0.0414(14) 0.0390(12) -0.0086(10) -0.0013(10) -0.0045(11) C41 0.0353(11) 0.0349(13) 0.0330(11) -0.0007(9) -0.0028(9) -0.0121(10) C42 0.0281(10) 0.0273(11) 0.0241(9) 0.0016(8) -0.0019(8) -0.0082(9) C43 0.0327(11) 0.0351(12) 0.0275(10) 0.0032(9) -0.0054(8) -0.0132(10) C44 0.0441(13) 0.0355(13) 0.0365(12) 0.0043(10) -0.0013(10) -0.0200(11) C45 0.0519(14) 0.0338(13) 0.0335(12) 0.0079(10) -0.0013(10) -0.0132(11) C46 0.0402(13) 0.0413(14) 0.0334(11) 0.0101(10) -0.0088(10) -0.0062(11) C47 0.0323(11) 0.0408(13) 0.0322(11) 0.0062(9) -0.0073(9) -0.0125(10) C48 0.0288(10) 0.0308(11) 0.0241(9) -0.0002(8) -0.0053(8) -0.0120(9) C49 0.0431(12) 0.0383(13) 0.0285(10) 0.0033(9) -0.0056(9) -0.0197(11) C50 0.0509(14) 0.0527(16) 0.0269(11) -0.0063(10) -0.0060(10) -0.0223(13) C51 0.0334(11) 0.0395(13) 0.0403(12) -0.0110(10) -0.0064(9) -0.0124(10) C52 0.0494(14) 0.0361(13) 0.0415(12) 0.0010(10) -0.0117(10) -0.0172(11) C53 0.0572(15) 0.0360(13) 0.0275(11) 0.0017(9) -0.0080(10) -0.0201(12) _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 Nd O9 2.3896(16) . ? Nd O2 2.5421(15) . ? Nd O3 2.5471(16) . ? Nd O4 2.5575(14) . ? Nd O1 2.5595(14) . ? Nd O6 2.5622(14) . ? Nd O8 2.5745(14) . ? Nd O5 2.6058(15) . ? Nd O7 2.6480(14) . ? Nd N6 2.7081(15) . ? P1 C24 1.787(2) . ? P1 C12 1.793(2) . ? P1 C6 1.7931(19) . ? P1 C18 1.7940(19) . ? P2 C42 1.7976(19) . ? P2 C30 1.798(2) . ? P2 C48 1.801(2) . ? P2 C36 1.8088(19) . ? O1 N1 1.259(2) . ? O2 N1 1.273(2) . ? O3 N2 1.261(3) . ? O4 N2 1.257(3) . ? O5 N3 1.259(2) . ? O6 N3 1.269(2) . ? O7 N4 1.256(2) . ? O8 N4 1.266(2) . ? O9 N5B 1.064(11) . ? O9 N5A 1.215(3) . ? O10 N5A 1.179(3) . ? O10 N5B 1.290(14) . ? N6 C5 1.342(2) . ? N6 C1 1.346(2) . ? C1 C2 1.382(3) . ? C1 H1 0.9500 . ? C2 C3 1.369(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C11 1.385(3) . ? C6 C7 1.401(3) . ? C7 C8 1.382(3) . ? C7 H7 0.9500 . ? C8 C9 1.364(4) . ? C8 H8 0.9500 . ? C9 C10 1.365(4) . ? C9 H9 0.9500 . ? C10 C11 1.422(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.391(3) . ? C12 C17 1.403(3) . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 C15 1.379(3) . ? C14 H14 0.9500 . ? C15 C16 1.391(3) . ? C15 H15 0.9500 . ? C16 C17 1.383(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.393(3) . ? C18 C19 1.393(3) . ? C19 C20 1.390(3) . ? C19 H19 0.9500 . ? C20 C21 1.377(3) . ? C20 H20 0.9500 . ? C21 C22 1.374(3) . ? C21 H21 0.9500 . ? C22 C23 1.388(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.376(3) . ? C24 C29 1.396(3) . ? C25 C26 1.394(3) . ? C25 H25 0.9500 . ? C26 C27 1.366(3) . ? C26 H26 0.9500 . ? C27 C28 1.376(3) . ? C27 H27 0.9500 . ? C28 C29 1.376(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C35 1.383(3) . ? C30 C31 1.399(3) . ? C31 C32 1.385(3) . ? C31 H31 0.9500 . ? C32 C33 1.373(4) . ? C32 H32 0.9500 . ? C33 C34 1.374(4) . ? C33 H33 0.9500 . ? C34 C35 1.395(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.384(3) . ? C36 C37 1.396(3) . ? C37 C38 1.388(3) . ? C37 H37 0.9500 . ? C38 C39 1.375(3) . ? C38 H38 0.9500 . ? C39 C40 1.373(3) . ? C39 H39 0.9500 . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.394(3) . ? C42 C47 1.399(3) . ? C43 C44 1.392(3) . ? C43 H43 0.9500 . ? C44 C45 1.378(3) . ? C44 H44 0.9500 . ? C45 C46 1.386(3) . ? C45 H45 0.9500 . ? C46 C47 1.385(3) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.384(3) . ? C48 C53 1.403(3) . ? C49 C50 1.386(3) . ? C49 H49 0.9500 . ? C50 C51 1.381(3) . ? C50 H50 0.9500 . ? C51 C52 1.372(3) . ? C51 H51 0.9500 . ? C52 C53 1.388(3) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Nd O2 79.76(6) . . ? O9 Nd O3 72.66(6) . . ? O2 Nd O3 79.06(6) . . ? O9 Nd O4 115.40(6) . . ? O2 Nd O4 108.17(5) . . ? O3 Nd O4 48.59(5) . . ? O9 Nd O1 122.87(6) . . ? O2 Nd O1 48.79(5) . . ? O3 Nd O1 74.50(5) . . ? O4 Nd O1 69.74(5) . . ? O9 Nd O6 149.33(6) . . ? O2 Nd O6 128.75(5) . . ? O3 Nd O6 118.98(5) . . ? O4 Nd O6 70.42(5) . . ? O1 Nd O6 87.73(5) . . ? O9 Nd O8 79.62(5) . . ? O2 Nd O8 119.19(5) . . ? O3 Nd O8 143.45(5) . . ? O4 Nd O8 132.34(5) . . ? O1 Nd O8 141.85(5) . . ? O6 Nd O8 76.07(4) . . ? O9 Nd O5 140.92(5) . . ? O2 Nd O5 86.01(5) . . ? O3 Nd O5 139.73(5) . . ? O4 Nd O5 103.59(5) . . ? O1 Nd O5 67.64(5) . . ? O6 Nd O5 48.11(5) . . ? O8 Nd O5 76.02(5) . . ? O9 Nd O7 74.68(5) . . ? O2 Nd O7 71.99(5) . . ? O3 Nd O7 139.42(5) . . ? O4 Nd O7 169.90(5) . . ? O1 Nd O7 104.79(5) . . ? O6 Nd O7 101.36(5) . . ? O8 Nd O7 47.47(4) . . ? O5 Nd O7 66.31(5) . . ? O9 Nd N6 78.59(6) . . ? O2 Nd N6 155.06(5) . . ? O3 Nd N6 82.80(5) . . ? O4 Nd N6 70.84(5) . . ? O1 Nd N6 140.35(5) . . ? O6 Nd N6 75.30(5) . . ? O8 Nd N6 68.53(4) . . ? O5 Nd N6 118.75(5) . . ? O7 Nd N6 113.48(5) . . ? C24 P1 C12 111.25(9) . . ? C24 P1 C6 109.97(9) . . ? C12 P1 C6 106.19(9) . . ? C24 P1 C18 106.53(9) . . ? C12 P1 C18 110.21(9) . . ? C6 P1 C18 112.76(9) . . ? C42 P2 C30 109.64(9) . . ? C42 P2 C48 110.69(9) . . ? C30 P2 C48 108.52(10) . . ? C42 P2 C36 108.48(9) . . ? C30 P2 C36 108.99(9) . . ? C48 P2 C36 110.49(9) . . ? N1 O1 Nd 99.04(12) . . ? N1 O2 Nd 99.48(12) . . ? N2 O3 Nd 99.37(14) . . ? N2 O4 Nd 98.99(12) . . ? N3 O5 Nd 98.49(12) . . ? N3 O6 Nd 100.33(11) . . ? N4 O7 Nd 98.08(10) . . ? N4 O8 Nd 101.47(11) . . ? N5B O9 Nd 140.5(7) . . ? N5A O9 Nd 138.75(19) . . ? O1 N1 O2 112.67(17) . . ? O4 N2 O3 113.05(18) . . ? O5 N3 O6 112.92(17) . . ? O7 N4 O8 112.98(16) . . ? O10 N5A O9 121.6(4) . . ? O9 N5B O10 124.9(13) . . ? C5 N6 C1 116.60(16) . . ? C5 N6 Nd 118.17(11) . . ? C1 N6 Nd 125.23(13) . . ? N6 C1 C2 123.11(19) . . ? N6 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.63(19) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 118.43(19) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 118.63(19) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N6 C5 C4 123.57(18) . . ? N6 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C11 C6 C7 120.5(2) . . ? C11 C6 P1 123.36(18) . . ? C7 C6 P1 116.14(16) . . ? C8 C7 C6 120.7(2) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 118.9(3) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 121.8(3) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 117.4(3) . . ? C6 C11 H11 121.3 . . ? C10 C11 H11 121.3 . . ? C13 C12 C17 120.13(18) . . ? C13 C12 P1 121.95(15) . . ? C17 C12 P1 117.88(14) . . ? C14 C13 C12 119.26(19) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C15 C14 C13 120.70(19) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.29(19) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.77(19) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C12 119.85(18) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C23 C18 C19 119.91(18) . . ? C23 C18 P1 118.28(15) . . ? C19 C18 P1 121.62(15) . . ? C20 C19 C18 119.51(19) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.15(19) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.58(19) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.2(2) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 119.7(2) . . ? C22 C23 H23 120.2 . . ? C18 C23 H23 120.2 . . ? C25 C24 C29 119.28(19) . . ? C25 C24 P1 122.64(16) . . ? C29 C24 P1 118.08(15) . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 120.2(2) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 120.1(2) . . ? C28 C29 H29 119.9 . . ? C24 C29 H29 119.9 . . ? C35 C30 C31 120.2(2) . . ? C35 C30 P2 121.41(16) . . ? C31 C30 P2 118.40(17) . . ? C32 C31 C30 119.5(2) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C33 C32 C31 119.8(2) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 121.4(2) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C35 119.5(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C30 C35 C34 119.6(2) . . ? C30 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C41 C36 C37 119.88(19) . . ? C41 C36 P2 120.88(14) . . ? C37 C36 P2 119.24(16) . . ? C38 C37 C36 119.3(2) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C39 C38 C37 120.5(2) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 120.2(2) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120.3(2) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C36 C41 C40 119.75(19) . . ? C36 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C47 119.75(18) . . ? C43 C42 P2 120.94(15) . . ? C47 C42 P2 119.28(15) . . ? C44 C43 C42 119.79(19) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 119.9(2) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.9(2) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C47 C46 C45 119.6(2) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C42 120.0(2) . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? C49 C48 C53 118.92(19) . . ? C49 C48 P2 121.48(15) . . ? C53 C48 P2 119.49(15) . . ? C48 C49 C50 120.4(2) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 120.4(2) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C50 119.9(2) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 120.4(2) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C52 C53 C48 120.0(2) . . ? C52 C53 H53 120.0 . . ? C48 C53 H53 120.0 . . ? _database_code_depnum_ccdc_archive 'CCDC 963101' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 Ag N8 O12 P2 Pr' _chemical_formula_weight 1361.78 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.9249(10) _cell_length_b 10.8245(5) _cell_length_c 20.8700(8) _cell_angle_alpha 90.00 _cell_angle_beta 127.881(2) _cell_angle_gamma 90.00 _cell_volume 5692.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 100289 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (539 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 100289 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.0424 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8682 _reflns_number_gt 6727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; The structure of the isomorphous Nd complex was used as a starting model for the refinement. The three nitrite ions are disordered: two of them (containing N1 and N2) have two components nearly orthogonal to one another while only one O atom is disordered over two positions in the third (N3). The occupancy parameters of all these positions have been refined to values very close to 0.5, then fixed to this value to allow for the mixing of the different positions and their symmetry equivalents (some positions are mutually incompatible). All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some bond lengths and displacement parameters in the disordered parts: DFIX 1.24 0.005 N2A O3A DFIX 1.24 0.005 N2A O4A DFIX 1.24 0.005 N2B O3B DFIX 1.24 0.005 N2B O4B DFIX 1.24 0.005 N3 O5A DFIX 1.24 0.005 N3 O5B DFIX 1.24 0.005 N3 O6 SIMU .01 .01 1.5 N2A N2B. The H atoms were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0507P)^2^+0.2461P] 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 8682 _refine_ls_number_parameters 425 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.941 _refine_diff_density_min -1.742 _refine_diff_density_rms 0.095 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 Pr Pr 0.0000 0.188144(18) 0.2500 0.03238(7) Uani 1 2 d S . . Ag Ag 0.0000 -0.21975(4) 0.2500 0.06706(12) Uani 1 2 d S . . P1 P 0.27037(2) 0.09213(6) 0.34928(4) 0.03058(13) Uani 1 1 d . . . O1A O 0.07593(15) 0.3323(3) 0.3492(2) 0.0480(9) Uani 0.50 1 d P A 1 O2A O 0.05926(17) 0.3240(4) 0.2345(3) 0.0560(11) Uani 0.50 1 d P A 1 O3A O -0.00946(19) 0.2379(5) 0.3632(3) 0.0637(12) Uani 0.50 1 d PD A 1 O4A O 0.0410(2) 0.0906(5) 0.3901(3) 0.0555(13) Uani 0.50 1 d PD A 1 N2A N 0.0202(3) 0.1567(8) 0.4127(5) 0.065(2) Uani 0.50 1 d PDU A 1 O1B O 0.04235(16) 0.4035(4) 0.2760(2) 0.0490(9) Uani 0.50 1 d P A 2 O2B O 0.09614(14) 0.2557(5) 0.3090(3) 0.0544(10) Uani 0.50 1 d P A 2 O3B O 0.05641(16) 0.2612(4) 0.4040(2) 0.0546(10) Uani 0.50 1 d PD B 2 O4B O 0.0137(2) 0.0979(6) 0.3797(3) 0.0575(14) Uani 0.50 1 d PD B 2 N2B N 0.0440(3) 0.1784(6) 0.4307(4) 0.0545(18) Uani 0.50 1 d PDU B 2 O5A O -0.04411(16) -0.0100(4) 0.2232(3) 0.0555(12) Uani 0.50 1 d PD A 3 O5B O -0.07360(16) 0.0534(3) 0.2102(2) 0.0448(9) Uani 0.50 1 d PD A 4 O6 O -0.10983(11) -0.1344(3) 0.18443(15) 0.0870(9) Uani 1 1 d D A . N1 N 0.08853(10) 0.3718(3) 0.30552(17) 0.0561(6) Uani 1 1 d . . . N3 N -0.08395(15) -0.0532(3) 0.1973(2) 0.0797(10) Uani 1 1 d D . . N4 N 0.01445(9) -0.2889(2) 0.36177(14) 0.0443(5) Uani 1 1 d . A . C1 C 0.00647(14) -0.2096(3) 0.4023(2) 0.0543(8) Uani 1 1 d . . . H1 H -0.0035 -0.1292 0.3829 0.065 Uiso 1 1 calc R A . C2 C 0.01220(14) -0.2404(4) 0.4710(2) 0.0676(9) Uani 1 1 d . A . H2 H 0.0047 -0.1831 0.4959 0.081 Uiso 1 1 calc R . . C3 C 0.02874(14) -0.3546(5) 0.5019(2) 0.0788(12) Uani 1 1 d . . . H3 H 0.0339 -0.3759 0.5494 0.095 Uiso 1 1 calc R A . C4 C 0.03808(13) -0.4400(4) 0.4633(3) 0.0808(13) Uani 1 1 d . A . H4 H 0.0499 -0.5191 0.4844 0.097 Uiso 1 1 calc R . . C5 C 0.02930(11) -0.4046(3) 0.3903(2) 0.0592(8) Uani 1 1 d . . . H5 H 0.0339 -0.4622 0.3620 0.071 Uiso 1 1 calc R A . C6 C 0.32014(9) 0.0956(2) 0.33425(14) 0.0325(5) Uani 1 1 d . . . C7 C 0.33666(9) 0.2057(2) 0.32240(15) 0.0383(5) Uani 1 1 d . . . H7 H 0.3257 0.2807 0.3293 0.046 Uiso 1 1 calc R . . C8 C 0.36972(10) 0.2035(3) 0.30024(17) 0.0458(6) Uani 1 1 d . . . H8 H 0.3811 0.2772 0.2925 0.055 Uiso 1 1 calc R . . C9 C 0.38575(9) 0.0920(3) 0.28963(16) 0.0447(6) Uani 1 1 d . . . H9 H 0.4072 0.0911 0.2735 0.054 Uiso 1 1 calc R . . C10 C 0.37030(11) -0.0183(3) 0.30279(18) 0.0436(6) Uani 1 1 d . . . H10 H 0.3819 -0.0929 0.2965 0.052 Uiso 1 1 calc R . . C11 C 0.33766(11) -0.0175(2) 0.32528(17) 0.0400(6) Uani 1 1 d . . . H11 H 0.3273 -0.0915 0.3345 0.048 Uiso 1 1 calc R . . C12 C 0.20679(9) 0.0727(2) 0.25192(14) 0.0332(5) Uani 1 1 d . . . C13 C 0.20328(10) 0.0708(2) 0.18196(15) 0.0407(6) Uani 1 1 d . . . H13 H 0.2335 0.0825 0.1856 0.049 Uiso 1 1 calc R . . C14 C 0.15452(11) 0.0515(3) 0.10688(17) 0.0476(6) Uani 1 1 d . . . H14 H 0.1522 0.0497 0.0602 0.057 Uiso 1 1 calc R . . C15 C 0.10964(12) 0.0349(3) 0.10127(18) 0.0502(7) Uani 1 1 d . . . H15 H 0.0771 0.0209 0.0509 0.060 Uiso 1 1 calc R . . C16 C 0.11282(11) 0.0390(3) 0.17062(19) 0.0477(7) Uani 1 1 d . . . H16 H 0.0822 0.0304 0.1663 0.057 Uiso 1 1 calc R . . C17 C 0.16108(10) 0.0558(2) 0.24594(16) 0.0401(6) Uani 1 1 d . . . H17 H 0.1632 0.0558 0.2924 0.048 Uiso 1 1 calc R . . C18 C 0.27207(10) 0.2308(2) 0.39828(15) 0.0335(5) Uani 1 1 d . . . C19 C 0.22515(10) 0.2892(2) 0.37247(17) 0.0411(6) Uani 1 1 d . . . H19 H 0.1930 0.2634 0.3250 0.049 Uiso 1 1 calc R . . C20 C 0.22627(11) 0.3853(3) 0.41699(18) 0.0464(6) Uani 1 1 d . . . H20 H 0.1949 0.4241 0.3996 0.056 Uiso 1 1 calc R . . C21 C 0.27432(12) 0.4236(2) 0.48769(17) 0.0451(6) Uani 1 1 d . . . H21 H 0.2751 0.4872 0.5184 0.054 Uiso 1 1 calc R . . C22 C 0.32138(11) 0.3673(3) 0.51288(16) 0.0451(6) Uani 1 1 d . . . H22 H 0.3536 0.3941 0.5599 0.054 Uiso 1 1 calc R . . C23 C 0.32033(10) 0.2719(2) 0.46822(16) 0.0398(5) Uani 1 1 d . . . H23 H 0.3518 0.2349 0.4848 0.048 Uiso 1 1 calc R . . C24 C 0.28397(9) -0.0395(2) 0.41215(14) 0.0313(5) Uani 1 1 d . . . C25 C 0.32885(10) -0.0387(2) 0.49357(16) 0.0386(5) Uani 1 1 d . . . H25 H 0.3502 0.0313 0.5158 0.046 Uiso 1 1 calc R . . C26 C 0.34146(10) -0.1429(3) 0.54107(16) 0.0424(6) Uani 1 1 d . . . H26 H 0.3713 -0.1426 0.5953 0.051 Uiso 1 1 calc R . . C27 C 0.30993(11) -0.2471(3) 0.50825(16) 0.0437(6) Uani 1 1 d . . . H27 H 0.3188 -0.3169 0.5403 0.052 Uiso 1 1 calc R . . C28 C 0.26554(12) -0.2477(2) 0.42844(17) 0.0451(6) Uani 1 1 d . . . H28 H 0.2443 -0.3179 0.4070 0.054 Uiso 1 1 calc R . . C29 C 0.25187(10) -0.1446(2) 0.37914(15) 0.0392(5) Uani 1 1 d . . . H29 H 0.2218 -0.1457 0.3251 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr 0.02974(10) 0.03897(12) 0.03372(11) 0.000 0.02217(8) 0.000 Ag 0.05180(19) 0.1028(3) 0.0546(2) 0.000 0.03678(17) 0.000 P1 0.0332(3) 0.0305(3) 0.0331(3) -0.0013(2) 0.0229(3) -0.0018(2) O1A 0.041(2) 0.050(2) 0.044(2) -0.0024(17) 0.0213(18) -0.0081(16) O2A 0.054(2) 0.070(3) 0.058(3) -0.003(2) 0.041(2) -0.017(2) O3A 0.073(3) 0.084(3) 0.051(3) 0.007(2) 0.047(2) 0.020(3) O4A 0.066(3) 0.060(3) 0.050(3) 0.006(2) 0.040(3) 0.007(3) N2A 0.073(5) 0.083(5) 0.052(4) 0.000(4) 0.045(4) -0.002(4) O1B 0.053(2) 0.044(2) 0.054(2) -0.0004(18) 0.034(2) -0.0070(18) O2B 0.0324(18) 0.072(3) 0.060(3) 0.011(2) 0.0293(19) -0.0003(19) O3B 0.048(2) 0.073(3) 0.038(2) -0.003(2) 0.0243(18) -0.015(2) O4B 0.060(4) 0.063(4) 0.049(3) 0.012(3) 0.033(3) -0.005(3) N2B 0.057(4) 0.073(4) 0.042(3) 0.005(3) 0.034(3) 0.000(3) O5A 0.038(2) 0.050(3) 0.082(3) -0.006(2) 0.038(2) -0.0086(19) O5B 0.042(2) 0.048(2) 0.044(2) 0.0043(18) 0.0266(18) -0.0034(19) O6 0.0977(19) 0.104(2) 0.0668(15) -0.0282(15) 0.0546(15) -0.0670(18) N1 0.0455(14) 0.0618(18) 0.0584(16) 0.0044(14) 0.0306(13) -0.0089(13) N3 0.123(3) 0.078(2) 0.077(2) -0.0233(18) 0.081(2) -0.040(2) N4 0.0418(12) 0.0430(14) 0.0480(13) -0.0019(10) 0.0274(11) -0.0033(10) C1 0.066(2) 0.0462(18) 0.061(2) -0.0099(14) 0.0440(17) -0.0148(14) C2 0.071(2) 0.078(3) 0.058(2) -0.0140(19) 0.0422(19) -0.0291(19) C3 0.056(2) 0.111(3) 0.055(2) 0.016(2) 0.0268(17) -0.013(2) C4 0.0458(18) 0.067(2) 0.111(3) 0.045(2) 0.039(2) 0.0075(17) C5 0.0394(15) 0.0494(19) 0.084(2) 0.0002(17) 0.0353(16) -0.0013(13) C6 0.0325(11) 0.0362(13) 0.0312(12) 0.0006(10) 0.0207(10) -0.0008(9) C7 0.0355(12) 0.0399(14) 0.0420(14) 0.0037(11) 0.0250(11) 0.0021(10) C8 0.0418(14) 0.0524(17) 0.0504(16) 0.0039(13) 0.0320(13) -0.0058(12) C9 0.0320(12) 0.0669(19) 0.0396(14) 0.0022(13) 0.0243(11) 0.0002(12) C10 0.0434(15) 0.0477(16) 0.0472(16) -0.0055(12) 0.0315(13) -0.0006(12) C11 0.0422(14) 0.0379(14) 0.0462(15) -0.0016(11) 0.0303(13) -0.0017(11) C12 0.0335(11) 0.0312(12) 0.0350(12) -0.0004(10) 0.0211(10) 0.0010(9) C13 0.0417(13) 0.0439(15) 0.0380(13) 0.0028(11) 0.0252(12) 0.0038(12) C14 0.0507(16) 0.0513(17) 0.0351(14) 0.0003(12) 0.0234(13) 0.0040(13) C15 0.0408(15) 0.0488(16) 0.0392(15) -0.0009(13) 0.0134(12) 0.0041(13) C16 0.0350(13) 0.0474(16) 0.0527(17) -0.0056(13) 0.0228(13) -0.0029(12) C17 0.0390(13) 0.0427(15) 0.0429(14) -0.0038(12) 0.0274(12) -0.0027(11) C18 0.0428(13) 0.0293(11) 0.0343(12) 0.0001(10) 0.0267(11) -0.0019(10) C19 0.0405(13) 0.0374(14) 0.0475(15) -0.0036(11) 0.0281(12) -0.0017(11) C20 0.0507(15) 0.0386(15) 0.0630(18) -0.0074(13) 0.0416(15) -0.0011(12) C21 0.0669(17) 0.0328(14) 0.0558(16) -0.0059(12) 0.0479(15) -0.0066(13) C22 0.0538(16) 0.0369(14) 0.0409(14) -0.0031(12) 0.0272(13) -0.0064(13) C23 0.0427(13) 0.0334(12) 0.0409(14) 0.0006(11) 0.0245(12) -0.0011(11) C24 0.0346(12) 0.0295(12) 0.0363(12) 0.0008(9) 0.0250(11) 0.0014(9) C25 0.0349(12) 0.0374(13) 0.0413(14) 0.0021(11) 0.0222(11) -0.0036(10) C26 0.0366(12) 0.0476(15) 0.0389(13) 0.0074(12) 0.0211(11) 0.0005(11) C27 0.0522(16) 0.0375(15) 0.0495(16) 0.0087(12) 0.0354(14) 0.0038(12) C28 0.0603(17) 0.0331(15) 0.0479(16) -0.0038(12) 0.0362(14) -0.0109(12) C29 0.0457(14) 0.0366(13) 0.0350(13) -0.0043(11) 0.0245(11) -0.0071(11) _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 Pr O5A 2.435(4) . ? Pr O5A 2.435(4) 2 ? Pr O5B 2.437(4) 2 ? Pr O5B 2.438(4) . ? Pr O1A 2.537(4) . ? Pr O1A 2.537(4) 2 ? Pr O2A 2.569(4) . ? Pr O2A 2.569(4) 2 ? Pr O1B 2.580(4) 2 ? Pr O1B 2.580(4) . ? Pr O4A 2.585(5) 2 ? Pr O4A 2.585(5) . ? Pr O2B 2.614(4) . ? Pr O2B 2.614(4) 2 ? Pr O3A 2.616(4) . ? Pr O3A 2.616(4) 2 ? Pr O4B 2.650(6) 2 ? Pr O4B 2.650(6) . ? Pr O3B 2.662(4) 2 ? Pr O3B 2.662(4) . ? Ag N4 2.212(2) . ? Ag O5A 2.546(4) . ? P1 C12 1.797(2) . ? P1 C18 1.798(3) . ? P1 C6 1.799(2) . ? P1 C24 1.801(2) . ? O1A N1 1.275(4) . ? O2A N1 1.280(5) . ? O3A N2A 1.239(5) . ? O4A N2A 1.248(5) . ? O1B N1 1.247(5) . ? O2B N1 1.274(5) . ? O3B N2B 1.242(4) . ? O4B N2B 1.252(5) . ? O5A N3 1.133(4) . ? O5B N3 1.185(4) . ? O6 N3 1.120(3) . ? N4 C1 1.335(4) . ? N4 C5 1.341(4) . ? C1 C2 1.372(5) . ? C1 H1 0.9300 . ? C2 C3 1.343(6) . ? C2 H2 0.9300 . ? C3 C4 1.374(6) . ? C3 H3 0.9300 . ? C4 C5 1.421(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.386(3) . ? C6 C11 1.405(3) . ? C7 C8 1.389(3) . ? C7 H7 0.9300 . ? C8 C9 1.381(4) . ? C8 H8 0.9300 . ? C9 C10 1.383(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.394(3) . ? C12 C17 1.398(3) . ? C13 C14 1.388(4) . ? C13 H13 0.9300 . ? C14 C15 1.376(4) . ? C14 H14 0.9300 . ? C15 C16 1.388(4) . ? C15 H15 0.9300 . ? C16 C17 1.380(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.393(3) . ? C18 C19 1.394(3) . ? C19 C20 1.380(4) . ? C19 H19 0.9300 . ? C20 C21 1.387(4) . ? C20 H20 0.9300 . ? C21 C22 1.391(4) . ? C21 H21 0.9300 . ? C22 C23 1.378(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.397(4) . ? C24 C29 1.396(3) . ? C25 C26 1.388(4) . ? C25 H25 0.9300 . ? C26 C27 1.381(4) . ? C26 H26 0.9300 . ? C27 C28 1.373(4) . ? C27 H27 0.9300 . ? C28 C29 1.394(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5A Pr O5B 81.46(15) . 2 ? O5A Pr O1A 149.03(15) . . ? O5A Pr O1A 103.10(14) 2 . ? O5B Pr O1A 81.48(13) 2 . ? O5B Pr O1A 152.21(13) . . ? O5A Pr O1A 103.10(14) . 2 ? O5A Pr O1A 149.03(15) 2 2 ? O5B Pr O1A 152.21(13) 2 2 ? O5B Pr O1A 81.48(13) . 2 ? O5A Pr O2A 147.36(15) . . ? O5A Pr O2A 99.56(14) 2 . ? O5B Pr O2A 75.83(14) 2 . ? O5B Pr O2A 158.41(14) . . ? O1A Pr O2A 87.35(13) 2 . ? O5A Pr O2A 99.56(14) . 2 ? O5A Pr O2A 147.36(15) 2 2 ? O5B Pr O2A 158.41(14) 2 2 ? O2A Pr O2A 110.2(2) . 2 ? O5A Pr O1B 126.38(14) . 2 ? O5A Pr O1B 177.11(13) 2 2 ? O5B Pr O1B 152.07(13) 2 2 ? O5B Pr O1B 101.42(12) . 2 ? O5A Pr O1B 177.11(13) . . ? O5A Pr O1B 126.38(14) 2 . ? O5B Pr O1B 101.42(12) 2 . ? O5B Pr O1B 152.07(13) . . ? O1A Pr O4A 137.78(15) . 2 ? O2A Pr O4A 118.46(17) 2 2 ? O1B Pr O4A 107.19(16) 2 2 ? O1B Pr O4A 116.27(14) . 2 ? O1A Pr O4A 137.78(15) 2 . ? O2A Pr O4A 118.46(17) . . ? O1B Pr O4A 116.27(14) 2 . ? O1B Pr O4A 107.19(16) . . ? O4A Pr O4A 131.8(2) 2 . ? N4 Ag N4 140.43(12) . 2 ? N4 Ag O5A 105.20(13) . . ? N4 Ag O5A 109.96(14) 2 . ? C12 P1 C18 111.06(11) . . ? C12 P1 C6 108.11(11) . . ? C18 P1 C6 111.12(11) . . ? C12 P1 C24 109.33(11) . . ? C18 P1 C24 109.67(11) . . ? C6 P1 C24 107.46(11) . . ? N1 O1A Pr 100.7(2) . . ? N1 O2A Pr 99.0(2) . . ? N2A O3A Pr 98.9(4) . . ? N2A O4A Pr 100.1(4) . . ? O3A N2A O4A 113.8(6) . . ? N1 O1B Pr 99.4(2) . . ? N1 O2B Pr 97.0(2) . . ? N2B O3B Pr 99.3(4) . . ? N2B O4B Pr 99.7(4) . . ? O3B N2B O4B 114.4(5) . . ? N3 O5A Pr 142.6(4) . . ? N3 O5A Ag 92.5(3) . . ? Pr O5A Ag 124.82(15) . . ? N3 O5B Pr 137.4(3) . . ? O1B N1 O2B 115.2(3) . . ? O1A N1 O2A 111.5(3) . . ? O6 N3 O5A 152.2(5) . . ? O6 N3 O5B 151.7(4) . . ? C1 N4 C5 118.2(3) . . ? C1 N4 Ag 116.9(2) . . ? C5 N4 Ag 124.9(2) . . ? N4 C1 C2 123.5(3) . . ? N4 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N4 C5 C4 120.7(3) . . ? N4 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C7 C6 C11 119.9(2) . . ? C7 C6 P1 121.51(18) . . ? C11 C6 P1 118.14(18) . . ? C6 C7 C8 119.7(2) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 120.0(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.7(2) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 119.8(3) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C6 119.8(2) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C13 C12 C17 119.8(2) . . ? C13 C12 P1 119.63(18) . . ? C17 C12 P1 120.59(18) . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.1(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C12 119.5(2) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? C23 C18 C19 119.6(2) . . ? C23 C18 P1 119.36(19) . . ? C19 C18 P1 120.59(19) . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 119.8(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C18 120.0(2) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C25 C24 C29 119.9(2) . . ? C25 C24 P1 119.33(18) . . ? C29 C24 P1 120.62(18) . . ? C26 C25 C24 119.7(2) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 C25 120.4(2) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.9(2) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C24 119.0(2) . . ? C28 C29 H29 120.5 . . ? C24 C29 H29 120.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 963102' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 Ag N8 Nd O12 P2' _chemical_formula_weight 1365.11 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.8726(10) _cell_length_b 10.8359(3) _cell_length_c 20.8434(7) _cell_angle_alpha 90.00 _cell_angle_beta 127.829(2) _cell_angle_gamma 90.00 _cell_volume 5685.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 64608 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2748 _exptl_absorpt_coefficient_mu 1.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and two \w scans with 2\% steps (348 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 64608 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8658 _reflns_number_gt 7081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The three nitrite ions are disordered: two of them (containing N1 and N2) have two components nearly orthogonal to one another while only one O atom is disordered over two positions in the third (N3). The occupancy parameters of all these positions have been refined to values very close to 0.5, then fixed to this value to allow for the mixing of the different positions and their symmetry equivalents (some positions are mutually incompatible). All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some bond lengths and displacement parameters in the disordered parts: DFIX 1.24 0.005 N2A O3A DFIX 1.24 0.005 N2A O4A DFIX 1.24 0.005 N2B O3B DFIX 1.24 0.005 N2B O4B DFIX 1.24 0.005 N3 O5A DFIX 1.24 0.005 N3 O5B DFIX 1.24 0.005 N3 O6 SIMU .01 .01 1.5 N2A N2B. The H atoms were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0450P)^2^+1.0341P] 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 8658 _refine_ls_number_parameters 425 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.618 _refine_diff_density_min -1.950 _refine_diff_density_rms 0.083 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 Nd Nd 0.0000 0.188509(15) 0.2500 0.03218(6) Uani 1 2 d S . . Ag Ag 0.0000 -0.21628(4) 0.2500 0.06548(10) Uani 1 2 d S . . P1 P 0.27036(2) 0.09196(5) 0.34907(3) 0.03094(12) Uani 1 1 d . . . O1A O 0.07555(13) 0.3309(3) 0.3491(2) 0.0462(8) Uani 0.50 1 d P A 1 O2A O 0.05846(15) 0.3232(3) 0.2337(2) 0.0530(9) Uani 0.50 1 d P A 1 O3A O -0.01036(17) 0.2376(4) 0.3614(2) 0.0620(11) Uani 0.50 1 d PD A 1 O4A O 0.0408(2) 0.0910(5) 0.3896(3) 0.0541(12) Uani 0.50 1 d PD A 1 N2A N 0.0194(3) 0.1567(7) 0.4114(4) 0.0650(18) Uani 0.50 1 d PDU A 1 O1B O 0.04202(14) 0.4028(3) 0.2757(2) 0.0485(8) Uani 0.50 1 d P A 2 O2B O 0.09582(13) 0.2552(4) 0.3095(2) 0.0544(9) Uani 0.50 1 d P A 2 O3B O 0.05630(15) 0.2603(4) 0.4031(2) 0.0551(9) Uani 0.50 1 d PD B 2 O4B O 0.0134(2) 0.0965(5) 0.3786(3) 0.0573(13) Uani 0.50 1 d PD B 2 N2B N 0.0438(3) 0.1769(5) 0.4298(3) 0.0538(15) Uani 0.50 1 d PDU B 2 O5A O -0.04406(15) -0.0084(3) 0.2235(3) 0.0548(11) Uani 0.50 1 d PD A 3 O5B O -0.07371(14) 0.0548(3) 0.2099(2) 0.0428(8) Uani 0.50 1 d PD A 4 O6 O -0.10995(10) -0.1319(3) 0.18405(14) 0.0879(8) Uani 1 1 d D A . N1 N 0.08816(9) 0.3701(2) 0.30530(15) 0.0551(6) Uani 1 1 d . . . N3 N -0.08393(14) -0.0516(3) 0.19701(19) 0.0788(9) Uani 1 1 d D . . N4 N 0.01450(9) -0.2875(2) 0.36163(14) 0.0455(5) Uani 1 1 d . A . C1 C 0.00681(13) -0.2097(3) 0.4028(2) 0.0564(7) Uani 1 1 d . . . H1 H -0.0031 -0.1291 0.3838 0.068 Uiso 1 1 calc R A . C2 C 0.01271(14) -0.2415(4) 0.4716(2) 0.0721(9) Uani 1 1 d . A . H2 H 0.0057 -0.1845 0.4974 0.087 Uiso 1 1 calc R . . C3 C 0.02880(13) -0.3568(5) 0.5013(2) 0.0832(12) Uani 1 1 d . . . H3 H 0.0337 -0.3795 0.5485 0.100 Uiso 1 1 calc R A . C4 C 0.03802(12) -0.4410(4) 0.4618(3) 0.0861(14) Uani 1 1 d . A . H4 H 0.0500 -0.5202 0.4824 0.103 Uiso 1 1 calc R . . C5 C 0.02879(10) -0.4041(3) 0.3888(2) 0.0591(8) Uani 1 1 d . . . H5 H 0.0327 -0.4611 0.3594 0.071 Uiso 1 1 calc R A . C6 C 0.32014(8) 0.0951(2) 0.33408(13) 0.0332(4) Uani 1 1 d . . . C7 C 0.33669(9) 0.2054(2) 0.32228(14) 0.0389(5) Uani 1 1 d . . . H7 H 0.3259 0.2804 0.3296 0.047 Uiso 1 1 calc R . . C8 C 0.36950(10) 0.2030(2) 0.29947(16) 0.0460(6) Uani 1 1 d . . . H8 H 0.3805 0.2767 0.2911 0.055 Uiso 1 1 calc R . . C9 C 0.38581(9) 0.0921(3) 0.28926(15) 0.0449(6) Uani 1 1 d . . . H9 H 0.4074 0.0914 0.2732 0.054 Uiso 1 1 calc R . . C10 C 0.37053(10) -0.0182(2) 0.30260(17) 0.0447(6) Uani 1 1 d . . . H10 H 0.3822 -0.0926 0.2964 0.054 Uiso 1 1 calc R . . C11 C 0.33771(10) -0.0175(2) 0.32521(16) 0.0408(5) Uani 1 1 d . . . H11 H 0.3274 -0.0915 0.3344 0.049 Uiso 1 1 calc R . . C12 C 0.20680(8) 0.0726(2) 0.25171(13) 0.0344(4) Uani 1 1 d . . . C13 C 0.20325(9) 0.0708(2) 0.18168(14) 0.0402(5) Uani 1 1 d . . . H13 H 0.2335 0.0825 0.1851 0.048 Uiso 1 1 calc R . . C14 C 0.15427(10) 0.0513(2) 0.10663(16) 0.0479(6) Uani 1 1 d . . . H14 H 0.1518 0.0496 0.0598 0.058 Uiso 1 1 calc R . . C15 C 0.10939(10) 0.0346(2) 0.10123(17) 0.0504(6) Uani 1 1 d . . . H15 H 0.0769 0.0204 0.0509 0.061 Uiso 1 1 calc R . . C16 C 0.11251(10) 0.0387(2) 0.17057(17) 0.0483(6) Uani 1 1 d . . . H16 H 0.0819 0.0296 0.1663 0.058 Uiso 1 1 calc R . . C17 C 0.16100(9) 0.0562(2) 0.24612(15) 0.0415(5) Uani 1 1 d . . . H17 H 0.1632 0.0572 0.2927 0.050 Uiso 1 1 calc R . . C18 C 0.27200(9) 0.2302(2) 0.39812(14) 0.0338(4) Uani 1 1 d . . . C19 C 0.22506(10) 0.2887(2) 0.37220(16) 0.0419(5) Uani 1 1 d . . . H19 H 0.1928 0.2629 0.3248 0.050 Uiso 1 1 calc R . . C20 C 0.22634(10) 0.3853(2) 0.41692(17) 0.0462(6) Uani 1 1 d . . . H20 H 0.1950 0.4243 0.3995 0.055 Uiso 1 1 calc R . . C21 C 0.27427(11) 0.4238(2) 0.48750(16) 0.0456(6) Uani 1 1 d . . . H21 H 0.2750 0.4874 0.5181 0.055 Uiso 1 1 calc R . . C22 C 0.32132(10) 0.3675(2) 0.51275(15) 0.0442(6) Uani 1 1 d . . . H22 H 0.3535 0.3944 0.5598 0.053 Uiso 1 1 calc R . . C23 C 0.32037(10) 0.2719(2) 0.46812(15) 0.0405(5) Uani 1 1 d . . . H23 H 0.3520 0.2352 0.4847 0.049 Uiso 1 1 calc R . . C24 C 0.28398(8) -0.0397(2) 0.41212(14) 0.0323(4) Uani 1 1 d . . . C25 C 0.32890(9) -0.0391(2) 0.49373(15) 0.0388(5) Uani 1 1 d . . . H25 H 0.3502 0.0309 0.5161 0.047 Uiso 1 1 calc R . . C26 C 0.34157(9) -0.1429(2) 0.54113(15) 0.0434(5) Uani 1 1 d . . . H26 H 0.3715 -0.1428 0.5954 0.052 Uiso 1 1 calc R . . C27 C 0.30984(10) -0.2467(2) 0.50802(16) 0.0448(6) Uani 1 1 d . . . H27 H 0.3187 -0.3164 0.5401 0.054 Uiso 1 1 calc R . . C28 C 0.26542(11) -0.2480(2) 0.42825(16) 0.0462(6) Uani 1 1 d . . . H28 H 0.2441 -0.3180 0.4067 0.055 Uiso 1 1 calc R . . C29 C 0.25211(10) -0.1446(2) 0.37942(15) 0.0416(5) Uani 1 1 d . . . H29 H 0.2221 -0.1456 0.3253 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.02920(9) 0.03826(10) 0.03394(10) 0.000 0.02184(7) 0.000 Ag 0.05155(18) 0.0971(3) 0.0561(2) 0.000 0.03723(16) 0.000 P1 0.0328(3) 0.0314(3) 0.0337(3) -0.0017(2) 0.0230(2) -0.0020(2) O1A 0.0403(17) 0.0477(19) 0.0414(19) -0.0022(15) 0.0205(16) -0.0058(14) O2A 0.051(2) 0.065(2) 0.056(2) -0.0028(18) 0.0393(19) -0.0164(17) O3A 0.071(3) 0.082(3) 0.052(2) 0.006(2) 0.047(2) 0.015(2) O4A 0.066(3) 0.056(3) 0.049(3) 0.005(2) 0.040(3) 0.004(2) N2A 0.072(5) 0.083(5) 0.055(4) -0.001(4) 0.047(4) -0.008(4) O1B 0.051(2) 0.0443(19) 0.053(2) 0.0013(16) 0.0334(18) -0.0029(16) O2B 0.0342(17) 0.066(3) 0.065(2) 0.010(2) 0.0316(18) -0.0023(17) O3B 0.051(2) 0.074(3) 0.0352(18) -0.0029(18) 0.0236(17) -0.0157(19) O4B 0.060(3) 0.065(3) 0.047(3) 0.013(2) 0.033(3) -0.005(3) N2B 0.056(4) 0.068(4) 0.045(3) 0.003(2) 0.035(3) -0.001(3) O5A 0.038(2) 0.049(2) 0.079(3) -0.0068(18) 0.037(2) -0.0054(16) O5B 0.0420(18) 0.0457(19) 0.0441(19) 0.0017(16) 0.0282(16) -0.0045(16) O6 0.0997(18) 0.1048(19) 0.0649(14) -0.0288(14) 0.0533(14) -0.0688(16) N1 0.0446(12) 0.0606(15) 0.0585(15) 0.0028(12) 0.0308(11) -0.0097(11) N3 0.118(3) 0.079(2) 0.078(2) -0.0249(16) 0.080(2) -0.0441(19) N4 0.0430(11) 0.0434(11) 0.0498(13) -0.0022(9) 0.0284(10) -0.0030(9) C1 0.0695(19) 0.0460(15) 0.0645(19) -0.0100(13) 0.0465(17) -0.0145(13) C2 0.080(2) 0.083(2) 0.061(2) -0.0183(18) 0.0475(19) -0.0352(19) C3 0.0558(19) 0.120(3) 0.057(2) 0.021(2) 0.0257(17) -0.013(2) C4 0.0469(17) 0.074(2) 0.116(3) 0.051(2) 0.039(2) 0.0080(16) C5 0.0400(13) 0.0486(16) 0.083(2) 0.0025(15) 0.0348(14) -0.0007(11) C6 0.0309(10) 0.0383(11) 0.0323(11) 0.0015(9) 0.0204(9) -0.0003(8) C7 0.0363(11) 0.0412(13) 0.0423(13) 0.0037(10) 0.0257(10) 0.0020(9) C8 0.0422(13) 0.0516(15) 0.0516(15) 0.0064(11) 0.0325(12) -0.0046(10) C9 0.0342(11) 0.0648(16) 0.0420(13) 0.0029(12) 0.0266(11) -0.0004(11) C10 0.0426(13) 0.0501(14) 0.0479(15) -0.0051(11) 0.0311(12) 0.0004(10) C11 0.0427(13) 0.0392(12) 0.0476(15) -0.0025(10) 0.0312(12) -0.0028(9) C12 0.0342(10) 0.0347(11) 0.0344(11) -0.0005(9) 0.0211(9) 0.0008(8) C13 0.0400(12) 0.0431(13) 0.0386(12) 0.0018(10) 0.0246(10) 0.0036(10) C14 0.0509(14) 0.0504(14) 0.0364(13) 0.0003(11) 0.0236(12) 0.0054(12) C15 0.0399(13) 0.0493(14) 0.0417(14) -0.0027(11) 0.0146(11) 0.0029(11) C16 0.0358(12) 0.0507(14) 0.0518(16) -0.0052(12) 0.0236(12) -0.0020(11) C17 0.0391(12) 0.0456(13) 0.0439(13) -0.0054(11) 0.0276(11) -0.0039(10) C18 0.0402(11) 0.0313(10) 0.0348(11) 0.0008(9) 0.0256(10) -0.0014(9) C19 0.0400(12) 0.0400(12) 0.0459(14) -0.0041(10) 0.0264(11) -0.0011(9) C20 0.0505(14) 0.0386(13) 0.0616(16) -0.0050(11) 0.0405(13) -0.0003(10) C21 0.0649(16) 0.0333(12) 0.0563(15) -0.0075(11) 0.0461(14) -0.0090(11) C22 0.0522(14) 0.0393(13) 0.0386(13) -0.0045(10) 0.0265(11) -0.0089(11) C23 0.0436(12) 0.0352(11) 0.0410(13) 0.0012(10) 0.0252(11) -0.0018(10) C24 0.0352(11) 0.0312(10) 0.0372(12) 0.0006(9) 0.0257(10) 0.0003(8) C25 0.0348(11) 0.0380(12) 0.0423(13) 0.0020(10) 0.0230(10) -0.0037(9) C26 0.0375(11) 0.0476(13) 0.0410(13) 0.0082(11) 0.0219(10) 0.0014(10) C27 0.0524(14) 0.0391(13) 0.0511(15) 0.0095(11) 0.0359(13) 0.0044(11) C28 0.0600(15) 0.0354(13) 0.0481(15) -0.0034(11) 0.0357(13) -0.0097(11) C29 0.0475(13) 0.0393(12) 0.0377(12) -0.0039(10) 0.0258(11) -0.0059(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 Nd O5A 2.425(3) 2 ? Nd O5A 2.425(3) . ? Nd O5B 2.431(3) 2 ? Nd O5B 2.431(3) . ? Nd O1A 2.519(3) 2 ? Nd O1A 2.519(3) . ? Nd O2A 2.548(3) 2 ? Nd O2A 2.548(3) . ? Nd O1B 2.567(3) . ? Nd O1B 2.567(3) 2 ? Nd O4A 2.574(5) . ? Nd O4A 2.574(5) 2 ? Nd O3A 2.592(4) 2 ? Nd O3A 2.592(4) . ? Nd O2B 2.596(3) 2 ? Nd O2B 2.596(3) . ? Nd O4B 2.637(5) 2 ? Nd O4B 2.637(5) . ? Nd O3B 2.643(4) . ? Nd O3B 2.643(4) 2 ? Ag N4 2.214(2) 2 ? Ag N4 2.214(2) . ? Ag O5A 2.530(4) . ? Ag O5A 2.530(4) 2 ? P1 C12 1.795(2) . ? P1 C6 1.796(2) . ? P1 C18 1.796(2) . ? P1 C24 1.803(2) . ? O1A N1 1.274(4) . ? O2A N1 1.283(4) . ? O3A N2A 1.242(5) . ? O4A N2A 1.249(5) . ? O1B N1 1.248(4) . ? O2B N1 1.261(5) . ? O3B N2B 1.246(4) . ? O4B N2B 1.252(5) . ? O5A N3 1.130(4) . ? O5B N3 1.183(3) . ? O6 N3 1.115(3) . ? N4 C1 1.328(4) . ? N4 C5 1.345(3) . ? C1 C2 1.372(4) . ? C1 H1 0.9300 . ? C2 C3 1.349(6) . ? C2 H2 0.9300 . ? C3 C4 1.377(6) . ? C3 H3 0.9300 . ? C4 C5 1.418(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.389(3) . ? C6 C11 1.401(3) . ? C7 C8 1.389(3) . ? C7 H7 0.9300 . ? C8 C9 1.377(4) . ? C8 H8 0.9300 . ? C9 C10 1.382(4) . ? C9 H9 0.9300 . ? C10 C11 1.386(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.393(3) . ? C12 C17 1.403(3) . ? C13 C14 1.390(3) . ? C13 H13 0.9300 . ? C14 C15 1.376(4) . ? C14 H14 0.9300 . ? C15 C16 1.388(4) . ? C15 H15 0.9300 . ? C16 C17 1.385(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.393(3) . ? C18 C23 1.397(3) . ? C19 C20 1.386(3) . ? C19 H19 0.9300 . ? C20 C21 1.384(4) . ? C20 H20 0.9300 . ? C21 C22 1.389(4) . ? C21 H21 0.9300 . ? C22 C23 1.381(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.393(3) . ? C24 C25 1.399(3) . ? C25 C26 1.385(3) . ? C25 H25 0.9300 . ? C26 C27 1.381(4) . ? C26 H26 0.9300 . ? C27 C28 1.372(3) . ? C27 H27 0.9300 . ? C28 C29 1.393(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5A Nd O5A 56.70(18) . 2 ? O5A Nd O5B 81.75(13) 2 . ? O5B Nd O5B 106.83(17) . 2 ? O5A Nd O1A 102.91(13) . 2 ? O5A Nd O1A 148.75(14) 2 2 ? O5B Nd O1A 81.19(12) . 2 ? O5B Nd O1A 152.05(12) 2 2 ? O5A Nd O1A 148.75(14) . . ? O5A Nd O1A 102.91(13) 2 . ? O5B Nd O1A 152.06(12) . . ? O5B Nd O1A 81.19(12) 2 . ? O1A Nd O1A 104.44(16) 2 . ? O5A Nd O2A 99.55(13) . 2 ? O5A Nd O2A 147.40(14) 2 2 ? O5B Nd O2A 75.86(12) . 2 ? O5B Nd O2A 158.01(13) 2 2 ? O1A Nd O2A 87.10(12) . 2 ? O5A Nd O2A 147.40(14) . . ? O5A Nd O2A 99.54(13) 2 . ? O5B Nd O2A 158.01(13) . . ? O5B Nd O2A 75.85(12) 2 . ? O1A Nd O2A 87.11(12) 2 . ? O1A Nd O2A 49.35(12) . . ? O2A Nd O2A 110.10(18) 2 . ? O5A Nd O1B 126.39(13) . 2 ? O5A Nd O1B 176.90(11) 2 2 ? O5B Nd O1B 101.36(11) . 2 ? O5B Nd O1B 151.79(12) 2 2 ? O1A Nd O1B 74.40(12) . 2 ? O2A Nd O1B 77.55(12) . 2 ? O5A Nd O1B 176.90(11) . . ? O5A Nd O1B 126.39(13) 2 . ? O5B Nd O1B 151.79(12) . . ? O5B Nd O1B 101.35(11) 2 . ? O1A Nd O1B 74.40(12) 2 . ? O2A Nd O1B 77.55(12) 2 . ? O1B Nd O1B 50.52(16) 2 . ? O5A Nd O4A 63.95(16) . 2 ? O5A Nd O4A 73.57(17) 2 2 ? O5B Nd O4A 69.83(13) . 2 ? O5B Nd O4A 81.71(15) 2 2 ? O1A Nd O4A 76.03(15) 2 2 ? O1A Nd O4A 138.08(14) . 2 ? O2A Nd O4A 118.77(16) 2 2 ? O2A Nd O4A 89.35(14) . 2 ? O1B Nd O4A 107.31(15) 2 2 ? O1B Nd O4A 116.38(13) . 2 ? O5A Nd O4A 73.57(17) . . ? O5A Nd O4A 63.95(16) 2 . ? O5B Nd O4A 81.71(15) . . ? O5B Nd O4A 69.83(13) 2 . ? O1A Nd O4A 138.08(14) 2 . ? O1A Nd O4A 76.03(15) . . ? O2A Nd O4A 89.35(14) 2 . ? O2A Nd O4A 118.77(16) . . ? O1B Nd O4A 116.39(13) 2 . ? O1B Nd O4A 107.31(15) . . ? O4A Nd O4A 131.6(2) 2 . ? N4 Ag N4 139.23(11) 2 . ? N4 Ag O5A 110.52(13) 2 . ? N4 Ag O5A 105.65(13) . . ? N4 Ag O5A 105.65(13) 2 2 ? N4 Ag O5A 110.52(13) . 2 ? O5A Ag O5A 54.16(15) . 2 ? C12 P1 C6 108.08(10) . . ? C12 P1 C18 111.09(10) . . ? C6 P1 C18 111.29(10) . . ? C12 P1 C24 109.37(10) . . ? C6 P1 C24 107.35(10) . . ? C18 P1 C24 109.57(10) . . ? N1 O1A Nd 100.4(2) . . ? N1 O2A Nd 98.7(2) . . ? N2A O3A Nd 99.0(3) . . ? N2A O4A Nd 99.7(4) . . ? O3A N2A O4A 113.7(5) . . ? N1 O1B Nd 98.7(2) . . ? N1 O2B Nd 96.9(2) . . ? N2B O3B Nd 99.2(3) . . ? N2B O4B Nd 99.3(4) . . ? O3B N2B O4B 114.6(5) . . ? N3 O5A Nd 142.7(3) . . ? N3 O5A Ag 92.6(3) . . ? Nd O5A Ag 124.57(15) . . ? N3 O5B Nd 137.1(3) . . ? O1B N1 O2B 115.7(3) . . ? O1A N1 O2A 111.6(3) . . ? O6 N3 O5A 152.6(5) . . ? O6 N3 O5B 151.1(4) . . ? C1 N4 C5 118.3(3) . . ? C1 N4 Ag 117.06(19) . . ? C5 N4 Ag 124.6(2) . . ? N4 C1 C2 123.7(3) . . ? N4 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N4 C5 C4 120.7(3) . . ? N4 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C11 120.0(2) . . ? C7 C6 P1 121.27(17) . . ? C11 C6 P1 118.29(17) . . ? C6 C7 C8 119.5(2) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 120.3(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.7(2) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 119.8(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C6 119.7(2) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C13 C12 C17 120.0(2) . . ? C13 C12 P1 119.76(16) . . ? C17 C12 P1 120.26(18) . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C12 119.4(2) . . ? C16 C17 H17 120.3 . . ? C12 C17 H17 120.3 . . ? C19 C18 C23 119.5(2) . . ? C19 C18 P1 120.61(18) . . ? C23 C18 P1 119.49(17) . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.0(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 120.0(2) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C29 C24 C25 119.6(2) . . ? C29 C24 P1 120.79(17) . . ? C25 C24 P1 119.48(17) . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.6(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.2(2) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C24 C29 C28 119.7(2) . . ? C24 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? _database_code_depnum_ccdc_archive 'CCDC 963103' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N6 O10 P2 Sm' _chemical_formula_weight 1138.24 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 17.8243(8) _cell_length_b 13.6518(3) _cell_length_c 22.0678(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.511(2) _cell_angle_gamma 90.00 _cell_volume 5061.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 175865 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 28.70 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and five \w scans with 2\% steps (478 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 175865 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_unetI/netI 0.1040 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 28.70 _reflns_number_total 13075 _reflns_number_gt 8465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0176P)^2^] 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 13075 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.658 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.102 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 Sm Sm 0.274318(9) 0.829327(11) 0.244685(6) 0.02729(5) Uani 1 1 d . . . P1 P 0.15933(4) 0.38417(5) 0.06257(3) 0.02447(16) Uani 1 1 d . . . P2 P 0.36018(4) 0.36886(6) 0.39874(3) 0.02967(17) Uani 1 1 d . . . O1 O 0.27702(13) 0.72648(16) 0.33912(9) 0.0435(5) Uani 1 1 d . . . O2 O 0.25458(12) 0.65041(15) 0.25153(10) 0.0423(5) Uani 1 1 d . . . O3 O 0.19382(13) 0.7778(2) 0.13100(10) 0.0567(7) Uani 1 1 d . . . O4 O 0.20338(14) 0.9287(2) 0.14693(11) 0.0564(7) Uani 1 1 d . . . O5 O 0.35226(12) 0.98339(15) 0.25378(10) 0.0433(5) Uani 1 1 d . . . O6 O 0.35325(12) 0.92925(18) 0.34348(9) 0.0477(6) Uani 1 1 d . . . O7 O 0.13134(11) 0.80051(17) 0.23663(9) 0.0422(5) Uani 1 1 d . . . O8 O 0.17979(14) 0.93355(18) 0.28049(10) 0.0506(6) Uani 1 1 d . . . O9 O 0.41468(11) 0.76711(16) 0.28314(10) 0.0444(5) Uani 1 1 d . . . O10 O 0.36365(12) 0.78114(17) 0.18267(9) 0.0451(6) Uani 1 1 d . . . N1 N 0.26149(16) 0.6449(2) 0.31080(13) 0.0475(7) Uani 1 1 d . . . N2 N 0.17711(17) 0.8610(3) 0.10717(13) 0.0633(10) Uani 1 1 d . . . N3 N 0.37656(16) 0.9960(2) 0.31387(13) 0.0510(7) Uani 1 1 d . . . N4 N 0.11978(17) 0.8787(2) 0.26206(12) 0.0502(8) Uani 1 1 d . . . N5 N 0.42450(15) 0.7563(2) 0.22908(14) 0.0483(7) Uani 1 1 d . . . N6 N 0.01756(19) 0.6044(2) 0.31898(12) 0.0577(8) Uani 1 1 d . . . C1 C 0.0856(2) 0.6354(3) 0.36008(19) 0.0627(11) Uani 1 1 d . . . H1 H 0.1260 0.6527 0.3442 0.075 Uiso 1 1 calc R . . C2 C 0.1005(2) 0.6438(3) 0.42660(18) 0.0613(10) Uani 1 1 d . . . H2 H 0.1493 0.6659 0.4541 0.074 Uiso 1 1 calc R . . C3 C 0.0409(2) 0.6184(3) 0.44944(15) 0.0532(9) Uani 1 1 d . . . H3 H 0.0481 0.6233 0.4931 0.064 Uiso 1 1 calc R . . C4 C -0.0291(2) 0.5857(2) 0.40741(15) 0.0467(8) Uani 1 1 d . . . H4 H -0.0704 0.5673 0.4219 0.056 Uiso 1 1 calc R . . C5 C -0.0379(2) 0.5803(2) 0.34399(14) 0.0458(8) Uani 1 1 d . . . H5 H -0.0864 0.5580 0.3161 0.055 Uiso 1 1 calc R . . C6 C 0.10635(15) 0.2987(2) 0.00134(11) 0.0254(6) Uani 1 1 d . . . C7 C 0.03900(15) 0.3301(2) -0.04836(12) 0.0300(6) Uani 1 1 d . . . H7 H 0.0219 0.3946 -0.0495 0.036 Uiso 1 1 calc R . . C8 C -0.00219(17) 0.2654(2) -0.09576(13) 0.0359(7) Uani 1 1 d . . . H8 H -0.0476 0.2859 -0.1285 0.043 Uiso 1 1 calc R . . C9 C 0.02398(18) 0.1707(2) -0.09449(14) 0.0391(7) Uani 1 1 d . . . H9 H -0.0040 0.1273 -0.1266 0.047 Uiso 1 1 calc R . . C10 C 0.09125(18) 0.1388(2) -0.04636(14) 0.0407(8) Uani 1 1 d . . . H10 H 0.1088 0.0747 -0.0464 0.049 Uiso 1 1 calc R . . C11 C 0.13247(16) 0.2028(2) 0.00209(13) 0.0314(7) Uani 1 1 d . . . H11 H 0.1775 0.1815 0.0350 0.038 Uiso 1 1 calc R . . C12 C 0.24293(15) 0.3219(2) 0.11779(11) 0.0269(6) Uani 1 1 d . . . C13 C 0.22898(17) 0.2579(2) 0.16233(12) 0.0342(7) Uani 1 1 d . . . H13 H 0.1784 0.2535 0.1655 0.041 Uiso 1 1 calc R . . C14 C 0.28998(19) 0.2014(2) 0.20141(14) 0.0457(8) Uani 1 1 d . . . H14 H 0.2804 0.1574 0.2301 0.055 Uiso 1 1 calc R . . C15 C 0.36581(19) 0.2105(3) 0.19776(14) 0.0466(9) Uani 1 1 d . . . H15 H 0.4070 0.1727 0.2245 0.056 Uiso 1 1 calc R . . C16 C 0.38097(18) 0.2747(3) 0.15508(14) 0.0459(9) Uani 1 1 d . . . H16 H 0.4323 0.2808 0.1536 0.055 Uiso 1 1 calc R . . C17 C 0.31922(16) 0.3303(2) 0.11406(12) 0.0350(7) Uani 1 1 d . . . H17 H 0.3288 0.3727 0.0845 0.042 Uiso 1 1 calc R . . C18 C 0.09610(15) 0.4268(2) 0.10545(11) 0.0255(6) Uani 1 1 d . . . C19 C 0.12594(16) 0.4943(2) 0.15545(11) 0.0286(6) Uani 1 1 d . . . H19 H 0.1779 0.5171 0.1659 0.034 Uiso 1 1 calc R . . C20 C 0.07795(16) 0.5270(2) 0.18942(12) 0.0338(7) Uani 1 1 d . . . H20 H 0.0971 0.5733 0.2219 0.041 Uiso 1 1 calc R . . C21 C 0.00165(17) 0.4908(2) 0.17498(13) 0.0353(7) Uani 1 1 d . . . H21 H -0.0306 0.5130 0.1977 0.042 Uiso 1 1 calc R . . C22 C -0.02705(16) 0.4220(2) 0.12730(13) 0.0348(7) Uani 1 1 d . . . H22 H -0.0781 0.3971 0.1186 0.042 Uiso 1 1 calc R . . C23 C 0.01946(15) 0.3894(2) 0.09206(12) 0.0293(6) Uani 1 1 d . . . H23 H -0.0003 0.3431 0.0598 0.035 Uiso 1 1 calc R . . C24 C 0.19324(15) 0.4819(2) 0.02349(12) 0.0264(6) Uani 1 1 d . . . C25 C 0.21841(16) 0.4566(2) -0.02815(12) 0.0333(7) Uani 1 1 d . . . H25 H 0.2148 0.3920 -0.0422 0.040 Uiso 1 1 calc R . . C26 C 0.24838(16) 0.5274(2) -0.05791(13) 0.0362(7) Uani 1 1 d . . . H26 H 0.2654 0.5103 -0.0920 0.043 Uiso 1 1 calc R . . C27 C 0.25348(17) 0.6234(2) -0.03785(13) 0.0388(8) Uani 1 1 d . . . H27 H 0.2736 0.6709 -0.0584 0.047 Uiso 1 1 calc R . . C28 C 0.22856(18) 0.6488(2) 0.01298(13) 0.0423(8) Uani 1 1 d . . . H28 H 0.2320 0.7135 0.0267 0.051 Uiso 1 1 calc R . . C29 C 0.19851(17) 0.5778(2) 0.04347(13) 0.0359(7) Uani 1 1 d . . . H29 H 0.1818 0.5951 0.0777 0.043 Uiso 1 1 calc R . . C30 C 0.26400(16) 0.3157(2) 0.35921(12) 0.0315(7) Uani 1 1 d . . . C31 C 0.19945(17) 0.3785(2) 0.33600(13) 0.0355(7) Uani 1 1 d . . . H31 H 0.2068 0.4457 0.3417 0.043 Uiso 1 1 calc R . . C32 C 0.12434(18) 0.3415(3) 0.30443(13) 0.0416(8) Uani 1 1 d . . . H32 H 0.0811 0.3836 0.2891 0.050 Uiso 1 1 calc R . . C33 C 0.1140(2) 0.2418(3) 0.29587(13) 0.0471(9) Uani 1 1 d . . . H33 H 0.0635 0.2169 0.2744 0.057 Uiso 1 1 calc R . . C34 C 0.17770(19) 0.1782(3) 0.31886(14) 0.0448(8) Uani 1 1 d . . . H34 H 0.1702 0.1110 0.3130 0.054 Uiso 1 1 calc R . . C35 C 0.25258(18) 0.2157(2) 0.35060(13) 0.0369(7) Uani 1 1 d . . . H35 H 0.2956 0.1734 0.3663 0.044 Uiso 1 1 calc R . . C36 C 0.39858(16) 0.4232(2) 0.34131(12) 0.0297(6) Uani 1 1 d . . . C37 C 0.34892(17) 0.4504(2) 0.28078(13) 0.0340(7) Uani 1 1 d . . . H37 H 0.2945 0.4385 0.2684 0.041 Uiso 1 1 calc R . . C38 C 0.38131(17) 0.4957(2) 0.23866(13) 0.0369(7) Uani 1 1 d . . . H38 H 0.3481 0.5154 0.1983 0.044 Uiso 1 1 calc R . . C39 C 0.46124(17) 0.5113(2) 0.25601(13) 0.0374(7) Uani 1 1 d . . . H39 H 0.4821 0.5406 0.2271 0.045 Uiso 1 1 calc R . . C40 C 0.51103(18) 0.4844(3) 0.31551(14) 0.0513(9) Uani 1 1 d . . . H40 H 0.5656 0.4949 0.3270 0.062 Uiso 1 1 calc R . . C41 C 0.47907(18) 0.4409(3) 0.35894(14) 0.0483(9) Uani 1 1 d . . . H41 H 0.5124 0.4239 0.3999 0.058 Uiso 1 1 calc R . . C42 C 0.34718(16) 0.4591(2) 0.45340(12) 0.0297(6) Uani 1 1 d . . . C43 C 0.37150(16) 0.5554(2) 0.45256(12) 0.0311(7) Uani 1 1 d . . . H43 H 0.3960 0.5745 0.4233 0.037 Uiso 1 1 calc R . . C44 C 0.35948(16) 0.6233(2) 0.49495(13) 0.0362(7) Uani 1 1 d . . . H44 H 0.3756 0.6879 0.4940 0.043 Uiso 1 1 calc R . . C45 C 0.32340(16) 0.5949(2) 0.53887(13) 0.0370(7) Uani 1 1 d . . . H45 H 0.3161 0.6404 0.5678 0.044 Uiso 1 1 calc R . . C46 C 0.29798(17) 0.4988(2) 0.53985(13) 0.0372(7) Uani 1 1 d . . . H46 H 0.2736 0.4799 0.5692 0.045 Uiso 1 1 calc R . . C47 C 0.30921(16) 0.4315(2) 0.49681(13) 0.0353(7) Uani 1 1 d . . . H47 H 0.2914 0.3675 0.4968 0.042 Uiso 1 1 calc R . . C48 C 0.42901(16) 0.2764(2) 0.44231(13) 0.0328(7) Uani 1 1 d . . . C49 C 0.45704(19) 0.2084(2) 0.40795(14) 0.0481(9) Uani 1 1 d . . . H49 H 0.4412 0.2122 0.3634 0.058 Uiso 1 1 calc R . . C50 C 0.5086(2) 0.1352(3) 0.44046(15) 0.0524(9) Uani 1 1 d . . . H50 H 0.5271 0.0896 0.4175 0.063 Uiso 1 1 calc R . . C51 C 0.53263(18) 0.1292(2) 0.50657(15) 0.0451(8) Uani 1 1 d . . . H51 H 0.5669 0.0794 0.5279 0.054 Uiso 1 1 calc R . . C52 C 0.50610(18) 0.1966(2) 0.54086(14) 0.0427(8) Uani 1 1 d . . . H52 H 0.5229 0.1928 0.5855 0.051 Uiso 1 1 calc R . . C53 C 0.45470(17) 0.2700(2) 0.50959(13) 0.0383(7) Uani 1 1 d . . . H53 H 0.4370 0.3155 0.5331 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.02799(8) 0.02788(9) 0.02461(7) -0.00144(7) 0.00694(5) 0.00034(7) P1 0.0247(4) 0.0238(4) 0.0252(3) 0.0004(3) 0.0087(3) -0.0005(3) P2 0.0321(4) 0.0277(4) 0.0287(4) 0.0011(3) 0.0096(3) 0.0003(3) O1 0.0540(14) 0.0387(14) 0.0386(12) 0.0089(10) 0.0165(10) 0.0036(12) O2 0.0403(13) 0.0315(13) 0.0541(13) -0.0071(10) 0.0146(11) -0.0023(10) O3 0.0392(14) 0.093(2) 0.0363(13) -0.0250(14) 0.0100(11) -0.0038(15) O4 0.0498(15) 0.0709(19) 0.0422(13) 0.0214(13) 0.0070(12) 0.0039(14) O5 0.0494(14) 0.0339(13) 0.0469(13) 0.0002(10) 0.0166(11) -0.0051(11) O6 0.0474(14) 0.0592(17) 0.0324(11) -0.0105(11) 0.0079(10) -0.0065(12) O7 0.0327(12) 0.0505(15) 0.0445(12) -0.0049(11) 0.0143(10) 0.0009(11) O8 0.0579(16) 0.0500(16) 0.0417(12) -0.0097(11) 0.0138(12) 0.0146(13) O9 0.0319(12) 0.0480(15) 0.0498(13) 0.0037(11) 0.0090(10) 0.0051(11) O10 0.0356(13) 0.0587(16) 0.0423(12) 0.0013(11) 0.0149(11) 0.0072(12) N1 0.0504(18) 0.0354(17) 0.0594(18) 0.0085(14) 0.0221(15) 0.0007(14) N2 0.0381(18) 0.116(3) 0.0348(17) 0.007(2) 0.0108(14) -0.005(2) N3 0.0513(18) 0.0438(19) 0.0560(18) -0.0134(15) 0.0152(15) -0.0075(15) N4 0.0464(18) 0.063(2) 0.0424(16) 0.0026(15) 0.0168(14) 0.0134(17) N5 0.0382(17) 0.0415(18) 0.0671(19) 0.0032(15) 0.0200(15) 0.0028(14) N6 0.066(2) 0.069(2) 0.0420(16) -0.0020(15) 0.0229(16) -0.0043(18) C1 0.057(3) 0.061(3) 0.085(3) 0.002(2) 0.043(2) 0.000(2) C2 0.048(2) 0.041(2) 0.073(3) -0.0110(19) -0.010(2) 0.0010(18) C3 0.069(3) 0.051(2) 0.0350(18) -0.0068(16) 0.0108(18) 0.005(2) C4 0.060(2) 0.039(2) 0.0464(19) 0.0017(16) 0.0241(18) 0.0056(18) C5 0.048(2) 0.039(2) 0.0425(18) -0.0046(15) 0.0039(16) -0.0009(17) C6 0.0256(15) 0.0261(16) 0.0266(13) -0.0020(12) 0.0113(12) -0.0027(12) C7 0.0332(16) 0.0213(16) 0.0352(14) 0.0021(13) 0.0110(13) 0.0000(13) C8 0.0357(17) 0.0383(19) 0.0306(15) -0.0001(14) 0.0071(13) -0.0064(15) C9 0.0468(19) 0.0322(19) 0.0384(16) -0.0090(14) 0.0143(15) -0.0095(16) C10 0.046(2) 0.0287(18) 0.0507(19) -0.0077(15) 0.0200(16) 0.0012(15) C11 0.0300(16) 0.0312(17) 0.0339(15) 0.0012(13) 0.0120(13) 0.0015(14) C12 0.0272(15) 0.0262(16) 0.0264(13) 0.0005(12) 0.0079(11) 0.0037(13) C13 0.0361(17) 0.0336(18) 0.0340(15) 0.0053(14) 0.0131(14) 0.0050(14) C14 0.056(2) 0.045(2) 0.0372(17) 0.0112(15) 0.0179(16) 0.0165(18) C15 0.042(2) 0.057(2) 0.0341(16) -0.0001(16) 0.0038(15) 0.0200(18) C16 0.0303(18) 0.062(3) 0.0416(18) -0.0037(17) 0.0073(15) 0.0118(17) C17 0.0301(16) 0.043(2) 0.0308(14) -0.0001(14) 0.0090(12) 0.0035(15) C18 0.0270(15) 0.0288(16) 0.0222(13) 0.0040(12) 0.0103(12) 0.0022(13) C19 0.0261(15) 0.0316(17) 0.0273(14) 0.0043(12) 0.0079(12) -0.0014(13) C20 0.0375(18) 0.0389(19) 0.0258(14) -0.0008(13) 0.0116(13) 0.0006(15) C21 0.0440(19) 0.0358(19) 0.0329(16) 0.0043(14) 0.0219(14) 0.0056(15) C22 0.0282(16) 0.041(2) 0.0380(16) 0.0068(14) 0.0151(14) -0.0023(14) C23 0.0277(16) 0.0301(17) 0.0302(14) -0.0006(12) 0.0099(12) -0.0012(13) C24 0.0262(15) 0.0245(16) 0.0279(14) 0.0011(12) 0.0081(12) 0.0013(13) C25 0.0375(17) 0.0303(18) 0.0339(15) -0.0020(13) 0.0144(14) -0.0003(14) C26 0.0350(17) 0.044(2) 0.0331(16) 0.0008(14) 0.0156(14) -0.0044(15) C27 0.0408(19) 0.035(2) 0.0391(17) 0.0085(14) 0.0116(15) -0.0088(15) C28 0.057(2) 0.0271(18) 0.0431(17) 0.0004(14) 0.0173(16) -0.0122(16) C29 0.0456(19) 0.0313(18) 0.0320(15) 0.0003(13) 0.0147(14) -0.0054(15) C30 0.0381(17) 0.0310(17) 0.0261(13) 0.0031(12) 0.0117(13) -0.0033(14) C31 0.0374(18) 0.0326(19) 0.0357(16) 0.0056(14) 0.0111(14) -0.0053(15) C32 0.0350(18) 0.054(2) 0.0355(16) 0.0105(16) 0.0108(14) -0.0015(17) C33 0.044(2) 0.067(3) 0.0295(16) -0.0027(17) 0.0110(15) -0.0226(19) C34 0.052(2) 0.042(2) 0.0393(17) -0.0032(16) 0.0143(16) -0.0155(18) C35 0.046(2) 0.0316(19) 0.0344(16) 0.0029(14) 0.0159(15) 0.0002(15) C36 0.0298(16) 0.0269(17) 0.0310(15) -0.0010(12) 0.0085(13) 0.0012(13) C37 0.0320(17) 0.0314(18) 0.0371(16) 0.0010(13) 0.0095(14) -0.0026(14) C38 0.0407(18) 0.0384(19) 0.0294(15) 0.0027(13) 0.0087(14) 0.0030(15) C39 0.0425(19) 0.0371(19) 0.0387(16) 0.0003(14) 0.0215(15) 0.0009(16) C40 0.0308(18) 0.075(3) 0.0475(19) 0.0137(18) 0.0130(16) -0.0048(18) C41 0.038(2) 0.065(3) 0.0376(17) 0.0124(17) 0.0066(15) 0.0030(18) C42 0.0292(16) 0.0285(17) 0.0296(14) -0.0004(12) 0.0076(13) -0.0001(13) C43 0.0268(16) 0.0326(18) 0.0308(14) 0.0032(13) 0.0056(13) 0.0005(13) C44 0.0319(17) 0.0271(18) 0.0430(17) -0.0022(14) 0.0038(14) -0.0023(14) C45 0.0297(17) 0.0389(19) 0.0386(16) -0.0076(14) 0.0063(14) 0.0066(15) C46 0.0323(17) 0.044(2) 0.0392(16) -0.0037(15) 0.0164(14) -0.0005(15) C47 0.0365(17) 0.0287(18) 0.0421(17) 0.0009(14) 0.0151(15) -0.0036(14) C48 0.0310(16) 0.0301(18) 0.0337(15) 0.0042(13) 0.0060(13) 0.0008(14) C49 0.057(2) 0.045(2) 0.0307(16) -0.0043(15) 0.0001(15) 0.0155(18) C50 0.055(2) 0.041(2) 0.051(2) -0.0106(17) 0.0036(17) 0.0137(18) C51 0.0378(19) 0.036(2) 0.053(2) 0.0123(16) 0.0032(16) -0.0008(16) C52 0.0403(19) 0.050(2) 0.0360(16) 0.0151(15) 0.0102(14) 0.0043(17) C53 0.0348(18) 0.044(2) 0.0376(16) 0.0067(15) 0.0146(14) 0.0018(15) _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 Sm O2 2.480(2) . ? Sm O5 2.491(2) . ? Sm O1 2.4998(19) . ? Sm O4 2.504(2) . ? Sm O9 2.5065(19) . ? Sm O10 2.5093(18) . ? Sm O8 2.525(2) . ? Sm O7 2.5255(19) . ? Sm O3 2.538(2) . ? Sm O6 2.558(2) . ? P1 C12 1.793(3) . ? P1 C18 1.794(2) . ? P1 C6 1.796(3) . ? P1 C24 1.799(3) . ? P2 C36 1.790(3) . ? P2 C42 1.792(3) . ? P2 C30 1.797(3) . ? P2 C48 1.799(3) . ? O1 N1 1.262(3) . ? O2 N1 1.274(3) . ? O3 N2 1.245(4) . ? O4 N2 1.252(4) . ? O5 N3 1.262(3) . ? O6 N3 1.270(3) . ? O7 N4 1.254(3) . ? O8 N4 1.257(3) . ? O9 N5 1.271(3) . ? O10 N5 1.264(3) . ? N6 C1 1.318(4) . ? N6 C5 1.325(4) . ? C1 C2 1.406(5) . ? C1 H1 0.9300 . ? C2 C3 1.364(5) . ? C2 H2 0.9300 . ? C3 C4 1.357(4) . ? C3 H3 0.9300 . ? C4 C5 1.357(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.388(4) . ? C6 C7 1.396(4) . ? C7 C8 1.378(4) . ? C7 H7 0.9300 . ? C8 C9 1.371(4) . ? C8 H8 0.9300 . ? C9 C10 1.380(4) . ? C9 H9 0.9300 . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.394(3) . ? C12 C13 1.398(3) . ? C13 C14 1.376(4) . ? C13 H13 0.9300 . ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C15 C16 1.378(4) . ? C15 H15 0.9300 . ? C16 C17 1.394(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.394(3) . ? C18 C19 1.399(4) . ? C19 C20 1.386(3) . ? C19 H19 0.9300 . ? C20 C21 1.381(4) . ? C20 H20 0.9300 . ? C21 C22 1.375(4) . ? C21 H21 0.9300 . ? C22 C23 1.386(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.374(4) . ? C24 C25 1.400(3) . ? C25 C26 1.373(4) . ? C25 H25 0.9300 . ? C26 C27 1.376(4) . ? C26 H26 0.9300 . ? C27 C28 1.382(4) . ? C27 H27 0.9300 . ? C28 C29 1.385(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.383(4) . ? C30 C31 1.388(4) . ? C31 C32 1.382(4) . ? C31 H31 0.9300 . ? C32 C33 1.379(4) . ? C32 H32 0.9300 . ? C33 C34 1.384(4) . ? C33 H33 0.9300 . ? C34 C35 1.382(4) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.377(4) . ? C36 C37 1.384(4) . ? C37 C38 1.392(4) . ? C37 H37 0.9300 . ? C38 C39 1.363(4) . ? C38 H38 0.9300 . ? C39 C40 1.367(4) . ? C39 H39 0.9300 . ? C40 C41 1.400(4) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.387(4) . ? C42 C47 1.396(3) . ? C43 C44 1.383(4) . ? C43 H43 0.9300 . ? C44 C45 1.385(4) . ? C44 H44 0.9300 . ? C45 C46 1.391(4) . ? C45 H45 0.9300 . ? C46 C47 1.383(4) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.392(4) . ? C48 C53 1.403(4) . ? C49 C50 1.385(4) . ? C49 H49 0.9300 . ? C50 C51 1.379(4) . ? C50 H50 0.9300 . ? C51 C52 1.372(4) . ? C51 H51 0.9300 . ? C52 C53 1.377(4) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sm O5 155.97(7) . . ? O2 Sm O1 50.18(7) . . ? O5 Sm O1 123.50(7) . . ? O2 Sm O4 123.03(8) . . ? O5 Sm O4 73.71(8) . . ? O1 Sm O4 152.37(7) . . ? O2 Sm O9 77.96(7) . . ? O5 Sm O9 78.00(7) . . ? O1 Sm O9 77.78(7) . . ? O4 Sm O9 129.42(7) . . ? O2 Sm O10 84.48(7) . . ? O5 Sm O10 80.03(7) . . ? O1 Sm O10 117.93(7) . . ? O4 Sm O10 84.38(7) . . ? O9 Sm O10 49.63(6) . . ? O2 Sm O8 114.38(7) . . ? O5 Sm O8 84.93(8) . . ? O1 Sm O8 83.38(7) . . ? O4 Sm O8 76.50(7) . . ? O9 Sm O8 141.25(7) . . ? O10 Sm O8 158.37(8) . . ? O2 Sm O7 71.97(7) . . ? O5 Sm O7 131.27(7) . . ? O1 Sm O7 73.10(7) . . ? O4 Sm O7 79.42(7) . . ? O9 Sm O7 147.21(7) . . ? O10 Sm O7 136.89(7) . . ? O8 Sm O7 49.21(7) . . ? O2 Sm O3 75.08(8) . . ? O5 Sm O3 115.42(8) . . ? O1 Sm O3 121.04(8) . . ? O4 Sm O3 48.89(9) . . ? O9 Sm O3 114.31(7) . . ? O10 Sm O3 68.93(7) . . ? O8 Sm O3 104.44(7) . . ? O7 Sm O3 70.32(7) . . ? O2 Sm O6 121.48(7) . . ? O5 Sm O6 49.31(7) . . ? O1 Sm O6 74.75(7) . . ? O4 Sm O6 114.89(9) . . ? O9 Sm O6 71.91(7) . . ? O10 Sm O6 109.64(7) . . ? O8 Sm O6 70.57(7) . . ? O7 Sm O6 113.44(7) . . ? O3 Sm O6 163.43(9) . . ? C12 P1 C18 108.74(11) . . ? C12 P1 C6 108.19(13) . . ? C18 P1 C6 110.03(12) . . ? C12 P1 C24 109.95(12) . . ? C18 P1 C24 112.53(12) . . ? C6 P1 C24 107.31(12) . . ? C36 P2 C42 110.98(13) . . ? C36 P2 C30 110.62(12) . . ? C42 P2 C30 106.71(13) . . ? C36 P2 C48 108.38(13) . . ? C42 P2 C48 109.92(13) . . ? C30 P2 C48 110.23(14) . . ? N1 O1 Sm 98.22(16) . . ? N1 O2 Sm 98.84(17) . . ? N2 O3 Sm 98.1(2) . . ? N2 O4 Sm 99.6(2) . . ? N3 O5 Sm 100.76(17) . . ? N3 O6 Sm 97.22(16) . . ? N4 O7 Sm 98.55(18) . . ? N4 O8 Sm 98.49(17) . . ? N5 O9 Sm 99.01(16) . . ? N5 O10 Sm 99.06(16) . . ? O1 N1 O2 112.7(2) . . ? O3 N2 O4 113.3(3) . . ? O5 N3 O6 112.7(3) . . ? O7 N4 O8 113.7(2) . . ? O10 N5 O9 112.3(2) . . ? C1 N6 C5 115.8(3) . . ? N6 C1 C2 123.6(3) . . ? N6 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 117.8(3) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N6 C5 C4 124.8(3) . . ? N6 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? C11 C6 C7 119.7(2) . . ? C11 C6 P1 120.9(2) . . ? C7 C6 P1 119.3(2) . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C6 119.7(3) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C17 C12 C13 119.9(3) . . ? C17 C12 P1 121.8(2) . . ? C13 C12 P1 118.1(2) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.9(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C12 C17 C16 119.4(3) . . ? C12 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C23 C18 C19 119.7(2) . . ? C23 C18 P1 120.9(2) . . ? C19 C18 P1 119.3(2) . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.6(3) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 119.4(3) . . ? C22 C23 H23 120.3 . . ? C18 C23 H23 120.3 . . ? C29 C24 C25 119.3(3) . . ? C29 C24 P1 123.4(2) . . ? C25 C24 P1 117.2(2) . . ? C26 C25 C24 119.8(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.7(3) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 119.7(3) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C29 120.0(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 120.4(3) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C35 C30 C31 119.5(3) . . ? C35 C30 P2 122.6(2) . . ? C31 C30 P2 117.9(2) . . ? C32 C31 C30 120.3(3) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C31 119.5(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 120.9(3) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 119.3(3) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C30 120.5(3) . . ? C34 C35 H35 119.7 . . ? C30 C35 H35 119.7 . . ? C41 C36 C37 119.7(3) . . ? C41 C36 P2 118.8(2) . . ? C37 C36 P2 121.5(2) . . ? C36 C37 C38 119.3(3) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 120.7(3) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C40 120.7(3) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 119.3(3) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C36 C41 C40 120.3(3) . . ? C36 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C47 119.3(3) . . ? C43 C42 P2 122.1(2) . . ? C47 C42 P2 118.6(2) . . ? C44 C43 C42 120.4(3) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 119.9(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C47 C46 C45 119.6(3) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C42 120.5(3) . . ? C46 C47 H47 119.8 . . ? C42 C47 H47 119.8 . . ? C49 C48 C53 119.1(3) . . ? C49 C48 P2 118.8(2) . . ? C53 C48 P2 122.2(2) . . ? C50 C49 C48 119.7(3) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C51 C50 C49 120.6(3) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C52 C51 C50 120.1(3) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 120.4(3) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C52 C53 C48 120.2(3) . . ? C52 C53 H53 119.9 . . ? C48 C53 H53 119.9 . . ? _database_code_depnum_ccdc_archive 'CCDC 963104' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N6 O10 P2 Yb' _chemical_formula_weight 1160.93 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 17.7881(5) _cell_length_b 13.6149(4) _cell_length_c 21.9841(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.6818(17) _cell_angle_gamma 90.00 _cell_volume 5013.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 172017 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 30.51 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2340 _exptl_absorpt_coefficient_mu 1.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.741 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (594 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 172017 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_unetI/netI 0.0476 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 30.51 _reflns_number_total 15284 _reflns_number_gt 11714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0298P)^2^] 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 15284 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.496 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.136 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 Yb Yb 0.273528(5) 0.830179(6) 0.244558(4) 0.02472(3) Uani 1 1 d . . . P1 P 0.16038(3) 0.38388(3) 0.06378(2) 0.02254(10) Uani 1 1 d . . . P2 P 0.35944(3) 0.36928(4) 0.39909(2) 0.02714(11) Uani 1 1 d . . . O1 O 0.27580(9) 0.73440(11) 0.33736(7) 0.0400(4) Uani 1 1 d . . . O2 O 0.25568(10) 0.65697(11) 0.25045(7) 0.0391(4) Uani 1 1 d . . . O3 O 0.19496(10) 0.77400(14) 0.13438(7) 0.0481(4) Uani 1 1 d . . . O4 O 0.20615(10) 0.92556(13) 0.15021(7) 0.0479(4) Uani 1 1 d . . . O5 O 0.34925(9) 0.97592(10) 0.25149(7) 0.0392(4) Uani 1 1 d . . . O6 O 0.35262(10) 0.92632(12) 0.34269(7) 0.0436(4) Uani 1 1 d . . . O7 O 0.13551(9) 0.80471(12) 0.23671(7) 0.0404(4) Uani 1 1 d . . . O8 O 0.18679(10) 0.93675(12) 0.27899(7) 0.0464(4) Uani 1 1 d . . . O9 O 0.40876(9) 0.76747(11) 0.28468(7) 0.0385(3) Uani 1 1 d . . . O10 O 0.35897(9) 0.78512(11) 0.18407(7) 0.0387(3) Uani 1 1 d . . . N1 N 0.26168(12) 0.65202(14) 0.30950(10) 0.0438(5) Uani 1 1 d . . . N2 N 0.17844(12) 0.8571(2) 0.10973(9) 0.0532(6) Uani 1 1 d . . . N3 N 0.37498(12) 0.99199(15) 0.31208(10) 0.0471(5) Uani 1 1 d . . . N4 N 0.12508(13) 0.88359(17) 0.26198(9) 0.0484(5) Uani 1 1 d . . . N5 N 0.41923(11) 0.75806(13) 0.23088(9) 0.0402(4) Uani 1 1 d . . . N6 N 0.01829(15) 0.60580(17) 0.31986(9) 0.0560(6) Uani 1 1 d . . . C1 C 0.08677(18) 0.6371(2) 0.36149(16) 0.0635(8) Uani 1 1 d . . . H1 H 0.1274 0.6552 0.3460 0.076 Uiso 1 1 calc R . . C2 C 0.10059(17) 0.64394(19) 0.42850(15) 0.0598(8) Uani 1 1 d . . . H2 H 0.1495 0.6656 0.4567 0.072 Uiso 1 1 calc R . . C3 C 0.04118(17) 0.61839(18) 0.45045(11) 0.0509(7) Uani 1 1 d . . . H3 H 0.0482 0.6227 0.4942 0.061 Uiso 1 1 calc R . . C4 C -0.02882(15) 0.58634(17) 0.40793(11) 0.0448(6) Uani 1 1 d . . . H4 H -0.0705 0.5681 0.4222 0.054 Uiso 1 1 calc R . . C5 C -0.03750(15) 0.58120(17) 0.34439(11) 0.0444(6) Uani 1 1 d . . . H5 H -0.0861 0.5588 0.3160 0.053 Uiso 1 1 calc R . . C6 C 0.10665(12) 0.29857(14) 0.00254(9) 0.0242(4) Uani 1 1 d . . . C7 C 0.03892(12) 0.33029(14) -0.04731(9) 0.0301(4) Uani 1 1 d . . . H7 H 0.0222 0.3952 -0.0483 0.036 Uiso 1 1 calc R . . C8 C -0.00329(13) 0.26597(15) -0.09502(9) 0.0335(5) Uani 1 1 d . . . H8 H -0.0493 0.2868 -0.1275 0.040 Uiso 1 1 calc R . . C9 C 0.02316(14) 0.17003(15) -0.09440(10) 0.0365(5) Uani 1 1 d . . . H9 H -0.0052 0.1266 -0.1266 0.044 Uiso 1 1 calc R . . C10 C 0.09136(14) 0.13860(16) -0.04622(10) 0.0375(5) Uani 1 1 d . . . H10 H 0.1094 0.0746 -0.0466 0.045 Uiso 1 1 calc R . . C11 C 0.13307(12) 0.20261(14) 0.00287(9) 0.0297(4) Uani 1 1 d . . . H11 H 0.1784 0.1812 0.0357 0.036 Uiso 1 1 calc R . . C12 C 0.24409(12) 0.32109(13) 0.11935(9) 0.0266(4) Uani 1 1 d . . . C13 C 0.23010(13) 0.25670(15) 0.16346(9) 0.0348(5) Uani 1 1 d . . . H13 H 0.1795 0.2520 0.1668 0.042 Uiso 1 1 calc R . . C14 C 0.29210(16) 0.19964(18) 0.20243(11) 0.0452(6) Uani 1 1 d . . . H14 H 0.2826 0.1546 0.2308 0.054 Uiso 1 1 calc R . . C15 C 0.36752(15) 0.2093(2) 0.19935(10) 0.0481(6) Uani 1 1 d . . . H15 H 0.4091 0.1716 0.2262 0.058 Uiso 1 1 calc R . . C16 C 0.38214(14) 0.27457(18) 0.15672(10) 0.0443(6) Uani 1 1 d . . . H16 H 0.4336 0.2813 0.1555 0.053 Uiso 1 1 calc R . . C17 C 0.32038(12) 0.33036(15) 0.11558(10) 0.0345(5) Uani 1 1 d . . . H17 H 0.3299 0.3732 0.0860 0.041 Uiso 1 1 calc R . . C18 C 0.09735(11) 0.42670(13) 0.10695(8) 0.0243(4) Uani 1 1 d . . . C19 C 0.12689(12) 0.49610(14) 0.15667(8) 0.0272(4) Uani 1 1 d . . . H19 H 0.1787 0.5199 0.1670 0.033 Uiso 1 1 calc R . . C20 C 0.07829(13) 0.52869(15) 0.19017(9) 0.0312(4) Uani 1 1 d . . . H20 H 0.0971 0.5757 0.2224 0.037 Uiso 1 1 calc R . . C21 C 0.00200(13) 0.49182(15) 0.17607(9) 0.0324(5) Uani 1 1 d . . . H21 H -0.0304 0.5144 0.1987 0.039 Uiso 1 1 calc R . . C22 C -0.02656(12) 0.42126(15) 0.12842(9) 0.0334(5) Uani 1 1 d . . . H22 H -0.0776 0.3956 0.1198 0.040 Uiso 1 1 calc R . . C23 C 0.02037(12) 0.38879(14) 0.09358(9) 0.0277(4) Uani 1 1 d . . . H23 H 0.0008 0.3419 0.0613 0.033 Uiso 1 1 calc R . . C24 C 0.19429(11) 0.48136(13) 0.02422(8) 0.0253(4) Uani 1 1 d . . . C25 C 0.21824(12) 0.45557(15) -0.02801(9) 0.0317(4) Uani 1 1 d . . . H25 H 0.2141 0.3908 -0.0421 0.038 Uiso 1 1 calc R . . C26 C 0.24808(13) 0.52641(16) -0.05869(9) 0.0354(5) Uani 1 1 d . . . H26 H 0.2643 0.5090 -0.0932 0.042 Uiso 1 1 calc R . . C27 C 0.25386(13) 0.62252(16) -0.03844(10) 0.0381(5) Uani 1 1 d . . . H27 H 0.2736 0.6701 -0.0595 0.046 Uiso 1 1 calc R . . C28 C 0.23027(15) 0.64845(16) 0.01338(11) 0.0413(6) Uani 1 1 d . . . H28 H 0.2348 0.7134 0.0273 0.050 Uiso 1 1 calc R . . C29 C 0.20004(13) 0.57828(15) 0.04453(10) 0.0340(5) Uani 1 1 d . . . H29 H 0.1837 0.5961 0.0789 0.041 Uiso 1 1 calc R . . C30 C 0.26256(13) 0.31687(14) 0.35922(9) 0.0298(4) Uani 1 1 d . . . C31 C 0.19789(13) 0.38095(16) 0.33654(9) 0.0342(5) Uani 1 1 d . . . H31 H 0.2054 0.4483 0.3430 0.041 Uiso 1 1 calc R . . C32 C 0.12244(14) 0.34382(17) 0.30436(10) 0.0403(5) Uani 1 1 d . . . H32 H 0.0791 0.3861 0.2888 0.048 Uiso 1 1 calc R . . C33 C 0.11173(15) 0.24328(19) 0.29546(10) 0.0441(6) Uani 1 1 d . . . H33 H 0.0610 0.2184 0.2741 0.053 Uiso 1 1 calc R . . C34 C 0.17533(16) 0.18010(17) 0.31783(11) 0.0431(6) Uani 1 1 d . . . H34 H 0.1675 0.1128 0.3114 0.052 Uiso 1 1 calc R . . C35 C 0.25111(14) 0.21648(15) 0.35003(10) 0.0352(5) Uani 1 1 d . . . H35 H 0.2941 0.1737 0.3654 0.042 Uiso 1 1 calc R . . C36 C 0.39770(12) 0.42347(14) 0.34122(9) 0.0275(4) Uani 1 1 d . . . C37 C 0.34749(13) 0.45359(15) 0.28098(9) 0.0321(4) Uani 1 1 d . . . H37 H 0.2927 0.4440 0.2690 0.039 Uiso 1 1 calc R . . C38 C 0.37981(13) 0.49799(15) 0.23894(9) 0.0354(5) Uani 1 1 d . . . H38 H 0.3461 0.5195 0.1989 0.042 Uiso 1 1 calc R . . C39 C 0.46023(13) 0.51087(15) 0.25500(10) 0.0349(5) Uani 1 1 d . . . H39 H 0.4811 0.5398 0.2258 0.042 Uiso 1 1 calc R . . C40 C 0.51065(14) 0.48057(19) 0.31504(11) 0.0469(6) Uani 1 1 d . . . H40 H 0.5655 0.4892 0.3264 0.056 Uiso 1 1 calc R . . C41 C 0.47929(14) 0.4377(2) 0.35778(11) 0.0468(6) Uani 1 1 d . . . H41 H 0.5132 0.4181 0.3982 0.056 Uiso 1 1 calc R . . C42 C 0.34649(12) 0.45996(14) 0.45402(9) 0.0281(4) Uani 1 1 d . . . C43 C 0.37030(12) 0.55705(15) 0.45211(9) 0.0299(4) Uani 1 1 d . . . H43 H 0.3940 0.5764 0.4223 0.036 Uiso 1 1 calc R . . C44 C 0.35831(12) 0.62448(15) 0.49505(10) 0.0340(5) Uani 1 1 d . . . H44 H 0.3738 0.6895 0.4938 0.041 Uiso 1 1 calc R . . C45 C 0.32331(12) 0.59593(16) 0.54000(10) 0.0341(5) Uani 1 1 d . . . H45 H 0.3162 0.6416 0.5691 0.041 Uiso 1 1 calc R . . C46 C 0.29904(13) 0.49998(16) 0.54167(10) 0.0360(5) Uani 1 1 d . . . H46 H 0.2754 0.4809 0.5717 0.043 Uiso 1 1 calc R . . C47 C 0.31005(12) 0.43207(15) 0.49831(10) 0.0335(5) Uani 1 1 d . . . H47 H 0.2930 0.3676 0.4989 0.040 Uiso 1 1 calc R . . C48 C 0.42845(12) 0.27641(14) 0.44289(9) 0.0301(4) Uani 1 1 d . . . C49 C 0.45480(15) 0.20671(17) 0.40835(10) 0.0438(6) Uani 1 1 d . . . H49 H 0.4383 0.2101 0.3635 0.053 Uiso 1 1 calc R . . C50 C 0.50548(15) 0.13258(18) 0.44071(12) 0.0492(6) Uani 1 1 d . . . H50 H 0.5218 0.0849 0.4175 0.059 Uiso 1 1 calc R . . C51 C 0.53213(14) 0.12875(16) 0.50728(11) 0.0410(5) Uani 1 1 d . . . H51 H 0.5667 0.0790 0.5288 0.049 Uiso 1 1 calc R . . C52 C 0.50773(14) 0.19834(17) 0.54205(11) 0.0401(5) Uani 1 1 d . . . H52 H 0.5262 0.1958 0.5870 0.048 Uiso 1 1 calc R . . C53 C 0.45564(13) 0.27223(16) 0.51014(9) 0.0339(5) Uani 1 1 d . . . H53 H 0.4389 0.3190 0.5336 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb 0.02477(5) 0.02618(5) 0.02227(4) -0.00122(3) 0.00668(3) 0.00158(4) P1 0.0219(2) 0.0220(2) 0.0241(2) 0.00044(18) 0.00835(19) -0.00028(19) P2 0.0285(3) 0.0262(3) 0.0255(2) 0.0010(2) 0.0074(2) 0.0004(2) O1 0.0452(10) 0.0385(9) 0.0371(8) 0.0033(7) 0.0149(7) 0.0032(7) O2 0.0368(9) 0.0318(9) 0.0478(10) -0.0062(6) 0.0133(8) -0.0023(7) O3 0.0359(10) 0.0721(12) 0.0366(8) -0.0173(9) 0.0127(7) -0.0038(9) O4 0.0422(10) 0.0622(11) 0.0369(8) 0.0133(8) 0.0102(7) 0.0032(9) O5 0.0452(10) 0.0326(8) 0.0410(8) 0.0009(7) 0.0159(7) -0.0026(7) O6 0.0476(10) 0.0492(10) 0.0312(8) -0.0061(7) 0.0096(7) 0.0004(8) O7 0.0359(9) 0.0500(9) 0.0380(8) -0.0003(7) 0.0161(7) 0.0060(8) O8 0.0495(11) 0.0474(10) 0.0395(8) -0.0069(7) 0.0114(8) 0.0141(9) O9 0.0330(9) 0.0411(9) 0.0387(8) 0.0027(7) 0.0084(7) 0.0039(7) O10 0.0329(9) 0.0460(9) 0.0375(8) 0.0001(7) 0.0124(7) 0.0057(7) N1 0.0442(12) 0.0359(11) 0.0541(12) 0.0064(9) 0.0201(10) -0.0012(9) N2 0.0346(12) 0.0952(18) 0.0286(10) 0.0028(11) 0.0092(9) -0.0040(12) N3 0.0467(12) 0.0412(11) 0.0509(12) -0.0137(10) 0.0131(10) -0.0077(10) N4 0.0425(13) 0.0672(15) 0.0394(11) 0.0045(10) 0.0189(10) 0.0156(11) N5 0.0307(10) 0.0370(10) 0.0525(12) 0.0019(9) 0.0134(9) 0.0057(8) N6 0.0720(17) 0.0623(14) 0.0384(11) -0.0040(10) 0.0248(11) -0.0006(13) C1 0.0576(19) 0.0551(16) 0.094(2) 0.0052(16) 0.0467(18) 0.0015(15) C2 0.0427(16) 0.0427(14) 0.0713(19) -0.0103(13) -0.0107(14) 0.0023(12) C3 0.0685(19) 0.0444(14) 0.0353(12) -0.0004(11) 0.0115(13) 0.0095(14) C4 0.0519(16) 0.0382(13) 0.0485(13) 0.0013(11) 0.0224(12) 0.0035(12) C5 0.0451(15) 0.0413(13) 0.0401(12) -0.0051(10) 0.0056(11) 0.0010(11) C6 0.0251(10) 0.0228(9) 0.0263(9) -0.0017(7) 0.0107(8) -0.0018(8) C7 0.0313(11) 0.0269(10) 0.0301(10) 0.0009(8) 0.0079(8) -0.0021(9) C8 0.0311(11) 0.0369(12) 0.0295(10) 0.0004(9) 0.0062(9) -0.0062(9) C9 0.0410(13) 0.0331(11) 0.0356(11) -0.0082(9) 0.0132(10) -0.0108(10) C10 0.0420(13) 0.0263(10) 0.0466(12) -0.0080(9) 0.0183(11) 0.0009(10) C11 0.0279(11) 0.0283(10) 0.0340(10) -0.0009(8) 0.0121(9) 0.0024(9) C12 0.0253(10) 0.0285(10) 0.0248(9) 0.0006(8) 0.0068(8) 0.0032(8) C13 0.0350(12) 0.0350(12) 0.0356(11) 0.0051(9) 0.0135(9) 0.0070(10) C14 0.0557(16) 0.0447(13) 0.0359(12) 0.0151(10) 0.0164(11) 0.0192(12) C15 0.0466(15) 0.0595(16) 0.0329(11) 0.0041(11) 0.0067(11) 0.0280(13) C16 0.0279(12) 0.0623(16) 0.0407(12) -0.0031(11) 0.0087(10) 0.0109(11) C17 0.0267(11) 0.0429(12) 0.0332(10) 0.0007(9) 0.0092(9) 0.0034(10) C18 0.0255(10) 0.0240(9) 0.0240(9) 0.0017(7) 0.0090(8) 0.0015(8) C19 0.0267(10) 0.0301(10) 0.0245(9) 0.0016(8) 0.0083(8) -0.0004(8) C20 0.0365(12) 0.0322(11) 0.0262(9) -0.0005(8) 0.0124(9) 0.0025(9) C21 0.0352(12) 0.0343(11) 0.0328(10) 0.0025(9) 0.0182(9) 0.0055(9) C22 0.0254(11) 0.0383(12) 0.0394(11) 0.0059(9) 0.0148(9) -0.0009(9) C23 0.0273(10) 0.0264(10) 0.0305(9) -0.0016(8) 0.0111(8) -0.0015(8) C24 0.0248(10) 0.0256(10) 0.0248(9) 0.0017(7) 0.0076(8) -0.0001(8) C25 0.0354(12) 0.0317(11) 0.0301(10) -0.0021(8) 0.0139(9) -0.0036(9) C26 0.0364(12) 0.0436(13) 0.0297(10) 0.0030(9) 0.0158(9) -0.0049(10) C27 0.0385(13) 0.0404(13) 0.0358(11) 0.0084(10) 0.0131(10) -0.0124(10) C28 0.0572(16) 0.0277(11) 0.0427(12) 0.0011(9) 0.0217(12) -0.0096(11) C29 0.0427(13) 0.0287(11) 0.0331(10) 0.0002(8) 0.0161(9) -0.0022(10) C30 0.0327(11) 0.0331(11) 0.0239(9) 0.0016(8) 0.0098(8) -0.0056(9) C31 0.0338(12) 0.0340(11) 0.0341(10) 0.0065(9) 0.0106(9) -0.0015(10) C32 0.0326(12) 0.0535(15) 0.0314(11) 0.0109(10) 0.0063(9) -0.0021(11) C33 0.0433(14) 0.0578(16) 0.0295(11) -0.0034(10) 0.0100(10) -0.0208(12) C34 0.0542(16) 0.0359(13) 0.0401(12) -0.0055(10) 0.0171(12) -0.0147(11) C35 0.0406(13) 0.0307(11) 0.0335(10) 0.0028(9) 0.0114(10) -0.0031(10) C36 0.0282(10) 0.0270(10) 0.0276(9) 0.0016(8) 0.0098(8) 0.0017(8) C37 0.0299(11) 0.0341(11) 0.0313(10) 0.0004(8) 0.0089(8) -0.0004(9) C38 0.0394(13) 0.0368(12) 0.0281(10) 0.0043(9) 0.0089(9) 0.0026(10) C39 0.0402(13) 0.0354(11) 0.0327(10) 0.0023(9) 0.0171(9) 0.0005(10) C40 0.0273(12) 0.0689(17) 0.0447(13) 0.0143(12) 0.0127(10) 0.0016(12) C41 0.0306(12) 0.0726(17) 0.0354(11) 0.0167(12) 0.0088(10) 0.0031(12) C42 0.0256(10) 0.0297(10) 0.0283(9) -0.0024(8) 0.0080(8) 0.0006(8) C43 0.0278(11) 0.0311(10) 0.0281(9) 0.0024(8) 0.0058(8) 0.0010(9) C44 0.0300(11) 0.0283(11) 0.0382(11) -0.0023(9) 0.0042(9) 0.0012(9) C45 0.0275(11) 0.0370(12) 0.0344(10) -0.0062(9) 0.0061(9) 0.0056(9) C46 0.0342(12) 0.0420(12) 0.0338(10) -0.0037(9) 0.0141(9) -0.0010(10) C47 0.0334(12) 0.0294(11) 0.0399(11) -0.0025(9) 0.0152(10) -0.0024(9) C48 0.0328(11) 0.0266(10) 0.0281(9) 0.0020(8) 0.0067(8) 0.0005(9) C49 0.0505(15) 0.0438(13) 0.0281(10) -0.0035(10) 0.0014(10) 0.0145(12) C50 0.0547(16) 0.0378(13) 0.0488(14) -0.0079(11) 0.0089(12) 0.0138(12) C51 0.0352(13) 0.0320(12) 0.0500(13) 0.0122(10) 0.0067(11) 0.0025(10) C52 0.0356(13) 0.0478(13) 0.0332(11) 0.0120(10) 0.0068(10) 0.0006(11) C53 0.0324(12) 0.0393(12) 0.0301(10) 0.0039(9) 0.0108(9) 0.0011(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 Yb O5 2.3741(14) . ? Yb O2 2.3888(15) . ? Yb O4 2.3980(15) . ? Yb O1 2.4102(14) . ? Yb O10 2.4117(14) . ? Yb O8 2.4177(15) . ? Yb O9 2.4215(15) . ? Yb O7 2.4274(16) . ? Yb O3 2.4748(15) . ? Yb O6 2.5104(14) . ? P1 C6 1.7912(19) . ? P1 C18 1.7929(18) . ? P1 C12 1.7930(19) . ? P1 C24 1.7986(18) . ? P2 C36 1.7914(19) . ? P2 C42 1.7953(19) . ? P2 C30 1.797(2) . ? P2 C48 1.799(2) . ? O1 N1 1.262(2) . ? O2 N1 1.268(2) . ? O3 N2 1.246(3) . ? O4 N2 1.269(3) . ? O5 N3 1.273(2) . ? O6 N3 1.261(2) . ? O7 N4 1.251(2) . ? O8 N4 1.262(3) . ? O9 N5 1.264(2) . ? O10 N5 1.265(2) . ? N6 C5 1.322(3) . ? N6 C1 1.324(4) . ? C1 C2 1.413(4) . ? C1 H1 0.9300 . ? C2 C3 1.347(4) . ? C2 H2 0.9300 . ? C3 C4 1.353(3) . ? C3 H3 0.9300 . ? C4 C5 1.355(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.388(3) . ? C6 C7 1.396(3) . ? C7 C8 1.379(3) . ? C7 H7 0.9300 . ? C8 C9 1.387(3) . ? C8 H8 0.9300 . ? C9 C10 1.382(3) . ? C9 H9 0.9300 . ? C10 C11 1.391(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.391(3) . ? C12 C17 1.393(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9300 . ? C14 C15 1.372(3) . ? C14 H14 0.9300 . ? C15 C16 1.378(3) . ? C15 H15 0.9300 . ? C16 C17 1.390(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.399(3) . ? C18 C19 1.406(3) . ? C19 C20 1.384(3) . ? C19 H19 0.9300 . ? C20 C21 1.381(3) . ? C20 H20 0.9300 . ? C21 C22 1.386(3) . ? C21 H21 0.9300 . ? C22 C23 1.382(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.386(3) . ? C24 C25 1.397(2) . ? C25 C26 1.381(3) . ? C25 H25 0.9300 . ? C26 C27 1.375(3) . ? C26 H26 0.9300 . ? C27 C28 1.386(3) . ? C27 H27 0.9300 . ? C28 C29 1.385(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.387(3) . ? C30 C31 1.395(3) . ? C31 C32 1.385(3) . ? C31 H31 0.9300 . ? C32 C33 1.387(3) . ? C32 H32 0.9300 . ? C33 C34 1.374(3) . ? C33 H33 0.9300 . ? C34 C35 1.386(3) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.386(3) . ? C36 C37 1.387(3) . ? C37 C38 1.381(3) . ? C37 H37 0.9300 . ? C38 C39 1.365(3) . ? C38 H38 0.9300 . ? C39 C40 1.385(3) . ? C39 H39 0.9300 . ? C40 C41 1.374(3) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.392(3) . ? C42 C43 1.393(3) . ? C43 C44 1.384(3) . ? C43 H43 0.9300 . ? C44 C45 1.389(3) . ? C44 H44 0.9300 . ? C45 C46 1.380(3) . ? C45 H45 0.9300 . ? C46 C47 1.388(3) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.392(3) . ? C48 C53 1.393(3) . ? C49 C50 1.380(3) . ? C49 H49 0.9300 . ? C50 C51 1.379(3) . ? C50 H50 0.9300 . ? C51 C52 1.376(3) . ? C51 H51 0.9300 . ? C52 C53 1.387(3) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Yb O2 154.75(5) . . ? O5 Yb O4 73.17(5) . . ? O2 Yb O4 123.00(6) . . ? O5 Yb O1 123.40(5) . . ? O2 Yb O1 52.02(5) . . ? O4 Yb O1 152.40(6) . . ? O5 Yb O10 78.38(5) . . ? O2 Yb O10 84.19(6) . . ? O4 Yb O10 83.40(5) . . ? O1 Yb O10 119.68(5) . . ? O5 Yb O8 83.48(5) . . ? O2 Yb O8 117.71(6) . . ? O4 Yb O8 76.11(5) . . ? O1 Yb O8 83.70(5) . . ? O10 Yb O8 155.84(5) . . ? O5 Yb O9 78.39(5) . . ? O2 Yb O9 76.47(5) . . ? O4 Yb O9 130.68(5) . . ? O1 Yb O9 76.67(5) . . ? O10 Yb O9 51.54(5) . . ? O8 Yb O9 139.28(5) . . ? O5 Yb O7 131.48(5) . . ? O2 Yb O7 73.33(6) . . ? O4 Yb O7 79.45(5) . . ? O1 Yb O7 73.21(5) . . ? O10 Yb O7 137.28(5) . . ? O8 Yb O7 51.04(6) . . ? O9 Yb O7 146.34(5) . . ? O5 Yb O3 116.25(6) . . ? O2 Yb O3 72.93(6) . . ? O4 Yb O3 50.79(6) . . ? O1 Yb O3 120.28(6) . . ? O10 Yb O3 68.58(5) . . ? O8 Yb O3 106.40(5) . . ? O9 Yb O3 114.32(5) . . ? O7 Yb O3 70.25(5) . . ? O5 Yb O6 50.76(5) . . ? O2 Yb O6 120.96(5) . . ? O4 Yb O6 115.67(6) . . ? O1 Yb O6 73.14(5) . . ? O10 Yb O6 109.37(5) . . ? O8 Yb O6 69.52(5) . . ? O9 Yb O6 70.75(5) . . ? O7 Yb O6 113.34(5) . . ? O3 Yb O6 166.05(6) . . ? C6 P1 C18 109.77(9) . . ? C6 P1 C12 108.26(9) . . ? C18 P1 C12 108.56(9) . . ? C6 P1 C24 107.22(8) . . ? C18 P1 C24 112.79(9) . . ? C12 P1 C24 110.15(9) . . ? C36 P2 C42 111.10(9) . . ? C36 P2 C30 110.39(9) . . ? C42 P2 C30 106.37(9) . . ? C36 P2 C48 108.40(9) . . ? C42 P2 C48 110.01(9) . . ? C30 P2 C48 110.57(10) . . ? N1 O1 Yb 97.25(12) . . ? N1 O2 Yb 98.11(11) . . ? N2 O3 Yb 96.78(13) . . ? N2 O4 Yb 99.88(14) . . ? N3 O5 Yb 101.95(12) . . ? N3 O6 Yb 95.58(11) . . ? N4 O7 Yb 98.25(13) . . ? N4 O8 Yb 98.41(12) . . ? N5 O9 Yb 97.83(11) . . ? N5 O10 Yb 98.28(11) . . ? O1 N1 O2 112.58(17) . . ? O3 N2 O4 112.53(18) . . ? O6 N3 O5 111.68(17) . . ? O7 N4 O8 112.30(18) . . ? O9 N5 O10 112.34(17) . . ? C5 N6 C1 116.2(2) . . ? N6 C1 C2 122.6(3) . . ? N6 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N6 C5 C4 124.5(2) . . ? N6 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C11 C6 C7 119.77(18) . . ? C11 C6 P1 120.83(15) . . ? C7 C6 P1 119.36(14) . . ? C8 C7 C6 120.38(19) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 119.6(2) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.42(19) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.1(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C6 C11 C10 119.6(2) . . ? C6 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C17 120.35(19) . . ? C13 C12 P1 118.24(16) . . ? C17 C12 P1 121.23(15) . . ? C14 C13 C12 119.5(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.2(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 120.4(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 119.0(2) . . ? C16 C17 H17 120.5 . . ? C12 C17 H17 120.5 . . ? C23 C18 C19 119.64(17) . . ? C23 C18 P1 120.74(14) . . ? C19 C18 P1 119.56(15) . . ? C20 C19 C18 119.48(18) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 120.46(19) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.27(18) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.31(19) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 119.79(18) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? C29 C24 C25 119.61(18) . . ? C29 C24 P1 123.18(14) . . ? C25 C24 P1 117.17(14) . . ? C26 C25 C24 119.97(19) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.36(19) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 119.89(19) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 120.4(2) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C24 119.76(19) . . ? C28 C29 H29 120.1 . . ? C24 C29 H29 120.1 . . ? C35 C30 C31 120.1(2) . . ? C35 C30 P2 122.14(17) . . ? C31 C30 P2 117.76(15) . . ? C32 C31 C30 119.7(2) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.7(2) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 120.7(2) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 120.1(2) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C30 119.8(2) . . ? C34 C35 H35 120.1 . . ? C30 C35 H35 120.1 . . ? C41 C36 C37 119.36(18) . . ? C41 C36 P2 119.06(15) . . ? C37 C36 P2 121.56(16) . . ? C38 C37 C36 119.3(2) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 121.29(19) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 119.62(19) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 119.8(2) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C36 120.7(2) . . ? C40 C41 H41 119.7 . . ? C36 C41 H41 119.7 . . ? C47 C42 C43 119.86(18) . . ? C47 C42 P2 118.58(15) . . ? C43 C42 P2 121.54(15) . . ? C44 C43 C42 119.38(19) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 120.58(19) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 120.20(19) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 119.62(19) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C46 C47 C42 120.34(19) . . ? C46 C47 H47 119.8 . . ? C42 C47 H47 119.8 . . ? C49 C48 C53 119.40(19) . . ? C49 C48 P2 118.79(15) . . ? C53 C48 P2 121.81(16) . . ? C50 C49 C48 119.9(2) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C51 C50 C49 120.4(2) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C50 120.2(2) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 120.0(2) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C52 C53 C48 120.0(2) . . ? C52 C53 H53 120.0 . . ? C48 C53 H53 120.0 . . ? _database_code_depnum_ccdc_archive 'CCDC 963105' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N6 O10 P2 Y' _chemical_formula_weight 1076.80 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 17.8054(7) _cell_length_b 13.6258(6) _cell_length_c 22.0104(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.628(2) _cell_angle_gamma 90.00 _cell_volume 5029.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 164062 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 28.70 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.682 _exptl_absorpt_correction_T_max 0.868 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (532 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 164062 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_unetI/netI 0.0748 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.70 _reflns_number_total 12979 _reflns_number_gt 8570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; The structure of the isomorphous Yb complex was used as a starting point for refinement. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0388P)^2^] 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 12979 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.348 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.068 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 Y Y 0.273754(11) 0.829865(14) 0.244695(8) 0.02610(6) Uani 1 1 d . . . P1 P 0.15999(3) 0.38394(4) 0.06338(2) 0.02342(11) Uani 1 1 d . . . P2 P 0.35967(3) 0.36904(4) 0.39908(2) 0.02831(12) Uani 1 1 d . . . O1 O 0.27608(9) 0.73179(11) 0.33776(7) 0.0416(4) Uani 1 1 d . . . O2 O 0.25510(8) 0.65458(10) 0.25081(7) 0.0409(4) Uani 1 1 d . . . O3 O 0.19479(9) 0.77484(15) 0.13368(7) 0.0520(4) Uani 1 1 d . . . O4 O 0.20517(9) 0.92697(13) 0.14926(7) 0.0517(4) Uani 1 1 d . . . O5 O 0.35055(9) 0.97860(10) 0.25225(7) 0.0413(4) Uani 1 1 d . . . O6 O 0.35270(9) 0.92724(12) 0.34284(6) 0.0440(4) Uani 1 1 d . . . O7 O 0.13387(8) 0.80316(12) 0.23687(7) 0.0437(4) Uani 1 1 d . . . O8 O 0.18499(10) 0.93591(12) 0.27942(7) 0.0487(4) Uani 1 1 d . . . O9 O 0.41058(8) 0.76709(11) 0.28439(7) 0.0407(4) Uani 1 1 d . . . O10 O 0.36043(8) 0.78426(11) 0.18384(7) 0.0413(4) Uani 1 1 d . . . N1 N 0.26135(11) 0.65000(14) 0.30974(10) 0.0454(5) Uani 1 1 d . . . N2 N 0.17819(11) 0.8586(2) 0.10903(9) 0.0567(6) Uani 1 1 d . . . N3 N 0.37517(11) 0.99303(14) 0.31273(10) 0.0483(5) Uani 1 1 d . . . N4 N 0.12317(12) 0.88171(17) 0.26201(9) 0.0506(5) Uani 1 1 d . . . N5 N 0.42084(10) 0.75743(14) 0.23057(9) 0.0432(5) Uani 1 1 d . . . N6 N 0.01795(13) 0.60519(16) 0.31970(9) 0.0578(6) Uani 1 1 d . . . C1 C 0.08680(16) 0.6364(2) 0.36118(14) 0.0627(7) Uani 1 1 d . . . H1 H 0.1273 0.6541 0.3455 0.075 Uiso 1 1 calc R . . C2 C 0.10092(15) 0.64371(18) 0.42758(14) 0.0606(7) Uani 1 1 d . . . H2 H 0.1499 0.6654 0.4555 0.073 Uiso 1 1 calc R . . C3 C 0.04120(16) 0.61825(18) 0.45031(11) 0.0535(7) Uani 1 1 d . . . H3 H 0.0484 0.6226 0.4941 0.064 Uiso 1 1 calc R . . C4 C -0.02899(14) 0.58647(16) 0.40773(11) 0.0455(6) Uani 1 1 d . . . H4 H -0.0708 0.5687 0.4218 0.055 Uiso 1 1 calc R . . C5 C -0.03726(14) 0.58099(17) 0.34430(11) 0.0462(6) Uani 1 1 d . . . H5 H -0.0857 0.5584 0.3161 0.055 Uiso 1 1 calc R . . C6 C 0.10662(10) 0.29886(14) 0.00227(8) 0.0247(4) Uani 1 1 d . . . C7 C 0.03876(11) 0.33056(15) -0.04776(9) 0.0301(4) Uani 1 1 d . . . H7 H 0.0218 0.3953 -0.0489 0.036 Uiso 1 1 calc R . . C8 C -0.00282(12) 0.26572(15) -0.09517(9) 0.0338(5) Uani 1 1 d . . . H8 H -0.0486 0.2862 -0.1277 0.041 Uiso 1 1 calc R . . C9 C 0.02356(12) 0.17038(16) -0.09432(10) 0.0373(5) Uani 1 1 d . . . H9 H -0.0047 0.1268 -0.1264 0.045 Uiso 1 1 calc R . . C10 C 0.09143(12) 0.13907(16) -0.04630(10) 0.0382(5) Uani 1 1 d . . . H10 H 0.1095 0.0751 -0.0467 0.046 Uiso 1 1 calc R . . C11 C 0.13286(11) 0.20302(15) 0.00267(9) 0.0310(5) Uani 1 1 d . . . H11 H 0.1780 0.1816 0.0356 0.037 Uiso 1 1 calc R . . C12 C 0.24364(11) 0.32170(14) 0.11866(9) 0.0273(4) Uani 1 1 d . . . C13 C 0.22982(12) 0.25733(15) 0.16323(9) 0.0355(5) Uani 1 1 d . . . H13 H 0.1793 0.2528 0.1667 0.043 Uiso 1 1 calc R . . C14 C 0.29185(14) 0.20024(17) 0.20221(10) 0.0453(6) Uani 1 1 d . . . H14 H 0.2825 0.1555 0.2308 0.054 Uiso 1 1 calc R . . C15 C 0.36678(14) 0.20987(18) 0.19860(10) 0.0483(6) Uani 1 1 d . . . H15 H 0.4082 0.1719 0.2253 0.058 Uiso 1 1 calc R . . C16 C 0.38191(12) 0.27459(18) 0.15624(10) 0.0453(6) Uani 1 1 d . . . H16 H 0.4333 0.2813 0.1550 0.054 Uiso 1 1 calc R . . C17 C 0.31998(11) 0.32989(16) 0.11537(9) 0.0343(5) Uani 1 1 d . . . H17 H 0.3296 0.3725 0.0858 0.041 Uiso 1 1 calc R . . C18 C 0.09699(10) 0.42661(14) 0.10669(8) 0.0240(4) Uani 1 1 d . . . C19 C 0.12654(11) 0.49534(14) 0.15629(8) 0.0279(4) Uani 1 1 d . . . H19 H 0.1784 0.5188 0.1666 0.033 Uiso 1 1 calc R . . C20 C 0.07807(12) 0.52812(15) 0.18988(9) 0.0318(5) Uani 1 1 d . . . H20 H 0.0970 0.5750 0.2221 0.038 Uiso 1 1 calc R . . C21 C 0.00171(11) 0.49145(15) 0.17570(9) 0.0335(5) Uani 1 1 d . . . H21 H -0.0307 0.5141 0.1982 0.040 Uiso 1 1 calc R . . C22 C -0.02656(11) 0.42140(15) 0.12823(9) 0.0336(5) Uani 1 1 d . . . H22 H -0.0774 0.3956 0.1197 0.040 Uiso 1 1 calc R . . C23 C 0.02019(11) 0.38933(14) 0.09324(9) 0.0280(4) Uani 1 1 d . . . H23 H 0.0005 0.3429 0.0608 0.034 Uiso 1 1 calc R . . C24 C 0.19380(10) 0.48152(14) 0.02402(8) 0.0247(4) Uani 1 1 d . . . C25 C 0.21853(11) 0.45623(15) -0.02780(9) 0.0313(5) Uani 1 1 d . . . H25 H 0.2149 0.3914 -0.0417 0.038 Uiso 1 1 calc R . . C26 C 0.24828(12) 0.52671(16) -0.05850(9) 0.0372(5) Uani 1 1 d . . . H26 H 0.2646 0.5095 -0.0930 0.045 Uiso 1 1 calc R . . C27 C 0.25384(12) 0.62280(17) -0.03791(10) 0.0399(5) Uani 1 1 d . . . H27 H 0.2741 0.6705 -0.0584 0.048 Uiso 1 1 calc R . . C28 C 0.22936(13) 0.64802(16) 0.01299(10) 0.0418(5) Uani 1 1 d . . . H28 H 0.2331 0.7130 0.0266 0.050 Uiso 1 1 calc R . . C29 C 0.19928(12) 0.57840(15) 0.04418(9) 0.0350(5) Uani 1 1 d . . . H29 H 0.1828 0.5964 0.0785 0.042 Uiso 1 1 calc R . . C30 C 0.26316(11) 0.31693(14) 0.35952(9) 0.0291(4) Uani 1 1 d . . . C31 C 0.19804(12) 0.38021(16) 0.33650(9) 0.0361(5) Uani 1 1 d . . . H31 H 0.2052 0.4475 0.3427 0.043 Uiso 1 1 calc R . . C32 C 0.12330(13) 0.34310(17) 0.30464(9) 0.0407(5) Uani 1 1 d . . . H32 H 0.0801 0.3854 0.2891 0.049 Uiso 1 1 calc R . . C33 C 0.11234(13) 0.24273(18) 0.29564(9) 0.0440(6) Uani 1 1 d . . . H33 H 0.0617 0.2179 0.2742 0.053 Uiso 1 1 calc R . . C34 C 0.17591(14) 0.17962(17) 0.31811(10) 0.0442(6) Uani 1 1 d . . . H34 H 0.1682 0.1124 0.3117 0.053 Uiso 1 1 calc R . . C35 C 0.25176(13) 0.21639(16) 0.35038(9) 0.0369(5) Uani 1 1 d . . . H35 H 0.2948 0.1737 0.3658 0.044 Uiso 1 1 calc R . . C36 C 0.39789(11) 0.42320(14) 0.34139(8) 0.0285(4) Uani 1 1 d . . . C37 C 0.34808(12) 0.45206(15) 0.28106(9) 0.0328(5) Uani 1 1 d . . . H37 H 0.2934 0.4412 0.2689 0.039 Uiso 1 1 calc R . . C38 C 0.38007(12) 0.49725(15) 0.23885(9) 0.0369(5) Uani 1 1 d . . . H38 H 0.3465 0.5183 0.1987 0.044 Uiso 1 1 calc R . . C39 C 0.46104(12) 0.51119(15) 0.25575(9) 0.0362(5) Uani 1 1 d . . . H39 H 0.4820 0.5406 0.2268 0.043 Uiso 1 1 calc R . . C40 C 0.51101(13) 0.48180(18) 0.31529(10) 0.0485(6) Uani 1 1 d . . . H40 H 0.5658 0.4911 0.3267 0.058 Uiso 1 1 calc R . . C41 C 0.47967(12) 0.43848(18) 0.35811(10) 0.0460(6) Uani 1 1 d . . . H41 H 0.5135 0.4193 0.3986 0.055 Uiso 1 1 calc R . . C42 C 0.34658(11) 0.45988(15) 0.45387(8) 0.0286(4) Uani 1 1 d . . . C43 C 0.37064(11) 0.55651(15) 0.45232(9) 0.0303(4) Uani 1 1 d . . . H43 H 0.3948 0.5758 0.4227 0.036 Uiso 1 1 calc R . . C44 C 0.35846(11) 0.62404(16) 0.49512(9) 0.0352(5) Uani 1 1 d . . . H44 H 0.3739 0.6890 0.4939 0.042 Uiso 1 1 calc R . . C45 C 0.32340(11) 0.59526(16) 0.53966(9) 0.0362(5) Uani 1 1 d . . . H45 H 0.3166 0.6406 0.5690 0.043 Uiso 1 1 calc R . . C46 C 0.29853(12) 0.49956(16) 0.54080(9) 0.0363(5) Uani 1 1 d . . . H46 H 0.2745 0.4807 0.5705 0.044 Uiso 1 1 calc R . . C47 C 0.30932(11) 0.43215(16) 0.49792(9) 0.0347(5) Uani 1 1 d . . . H47 H 0.2918 0.3679 0.4982 0.042 Uiso 1 1 calc R . . C48 C 0.42873(11) 0.27625(15) 0.44276(9) 0.0308(5) Uani 1 1 d . . . C49 C 0.45537(13) 0.20683(17) 0.40842(10) 0.0462(6) Uani 1 1 d . . . H49 H 0.4388 0.2100 0.3636 0.055 Uiso 1 1 calc R . . C50 C 0.50638(14) 0.13330(18) 0.44073(11) 0.0516(6) Uani 1 1 d . . . H50 H 0.5236 0.0865 0.4176 0.062 Uiso 1 1 calc R . . C51 C 0.53188(12) 0.12885(17) 0.50699(10) 0.0429(6) Uani 1 1 d . . . H51 H 0.5660 0.0788 0.5285 0.051 Uiso 1 1 calc R . . C52 C 0.50721(12) 0.19790(17) 0.54146(10) 0.0414(5) Uani 1 1 d . . . H52 H 0.5255 0.1953 0.5863 0.050 Uiso 1 1 calc R . . C53 C 0.45522(12) 0.27155(16) 0.50985(9) 0.0358(5) Uani 1 1 d . . . H53 H 0.4380 0.3178 0.5334 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.02665(10) 0.02736(11) 0.02301(10) -0.00150(8) 0.00663(7) 0.00115(8) P1 0.0230(2) 0.0229(3) 0.0246(2) 0.0005(2) 0.00824(19) 0.0000(2) P2 0.0309(3) 0.0267(3) 0.0263(3) 0.0014(2) 0.0083(2) 0.0007(2) O1 0.0495(9) 0.0386(10) 0.0376(8) 0.0054(7) 0.0157(7) 0.0031(8) O2 0.0400(8) 0.0344(9) 0.0483(10) -0.0059(7) 0.0149(7) -0.0024(7) O3 0.0381(9) 0.0795(14) 0.0384(9) -0.0203(9) 0.0129(7) -0.0053(9) O4 0.0462(9) 0.0669(12) 0.0375(9) 0.0167(9) 0.0081(7) 0.0039(9) O5 0.0490(9) 0.0337(9) 0.0418(9) -0.0007(7) 0.0160(7) -0.0044(7) O6 0.0484(9) 0.0497(10) 0.0315(8) -0.0079(7) 0.0101(7) -0.0040(8) O7 0.0345(8) 0.0553(11) 0.0431(9) -0.0036(8) 0.0154(7) 0.0031(7) O8 0.0557(10) 0.0481(10) 0.0404(8) -0.0077(8) 0.0134(7) 0.0148(9) O9 0.0337(8) 0.0437(10) 0.0407(9) 0.0017(7) 0.0072(7) 0.0040(7) O10 0.0371(8) 0.0489(10) 0.0394(8) -0.0017(7) 0.0145(7) 0.0051(7) N1 0.0442(11) 0.0395(13) 0.0544(13) 0.0066(10) 0.0188(10) 0.0010(9) N2 0.0357(11) 0.104(2) 0.0298(11) 0.0022(13) 0.0106(9) -0.0059(12) N3 0.0477(12) 0.0401(13) 0.0558(13) -0.0138(10) 0.0158(10) -0.0077(10) N4 0.0451(12) 0.0686(16) 0.0401(11) 0.0021(11) 0.0169(9) 0.0170(12) N5 0.0336(10) 0.0399(12) 0.0558(12) 0.0017(9) 0.0146(9) 0.0045(9) N6 0.0715(15) 0.0644(15) 0.0426(11) -0.0039(10) 0.0257(11) 0.0010(12) C1 0.0565(17) 0.0564(18) 0.088(2) 0.0013(15) 0.0408(16) -0.0020(14) C2 0.0442(15) 0.0429(16) 0.0739(19) -0.0119(14) -0.0077(13) -0.0001(12) C3 0.0751(18) 0.0459(16) 0.0338(13) -0.0048(11) 0.0109(12) 0.0083(14) C4 0.0561(15) 0.0372(14) 0.0499(14) -0.0014(11) 0.0266(12) 0.0034(12) C5 0.0431(13) 0.0423(15) 0.0447(13) -0.0046(11) 0.0037(11) 0.0026(11) C6 0.0253(9) 0.0239(11) 0.0268(10) -0.0008(8) 0.0112(8) -0.0020(8) C7 0.0328(11) 0.0252(11) 0.0313(10) 0.0016(9) 0.0092(8) 0.0004(9) C8 0.0327(11) 0.0363(13) 0.0288(10) -0.0007(9) 0.0057(9) -0.0071(10) C9 0.0453(13) 0.0334(13) 0.0340(11) -0.0091(10) 0.0143(10) -0.0121(10) C10 0.0449(13) 0.0263(12) 0.0464(13) -0.0054(10) 0.0193(11) 0.0016(10) C11 0.0290(10) 0.0312(12) 0.0341(11) -0.0016(9) 0.0120(9) 0.0014(9) C12 0.0266(10) 0.0264(11) 0.0273(10) -0.0008(8) 0.0071(8) 0.0036(8) C13 0.0366(11) 0.0356(13) 0.0355(11) 0.0071(10) 0.0136(9) 0.0068(10) C14 0.0571(15) 0.0438(15) 0.0365(12) 0.0121(10) 0.0177(11) 0.0171(12) C15 0.0460(14) 0.0575(17) 0.0343(12) 0.0036(11) 0.0039(10) 0.0266(12) C16 0.0301(11) 0.0641(17) 0.0397(12) -0.0025(12) 0.0092(10) 0.0127(11) C17 0.0284(10) 0.0417(13) 0.0314(11) 0.0000(9) 0.0082(8) 0.0018(10) C18 0.0252(9) 0.0243(11) 0.0237(9) 0.0040(8) 0.0098(8) 0.0029(8) C19 0.0276(10) 0.0304(12) 0.0256(10) 0.0025(8) 0.0088(8) -0.0007(9) C20 0.0410(12) 0.0308(12) 0.0246(10) -0.0001(9) 0.0120(9) 0.0035(9) C21 0.0344(11) 0.0365(13) 0.0354(11) 0.0046(9) 0.0195(9) 0.0065(10) C22 0.0268(10) 0.0375(13) 0.0380(11) 0.0049(10) 0.0130(9) -0.0010(9) C23 0.0270(10) 0.0269(11) 0.0301(10) -0.0002(8) 0.0097(8) -0.0012(8) C24 0.0231(9) 0.0247(11) 0.0256(9) 0.0022(8) 0.0074(8) -0.0019(8) C25 0.0338(11) 0.0294(12) 0.0326(10) -0.0016(9) 0.0137(9) -0.0051(9) C26 0.0380(12) 0.0445(14) 0.0322(11) 0.0020(10) 0.0159(9) -0.0056(10) C27 0.0418(12) 0.0412(14) 0.0360(11) 0.0089(10) 0.0122(10) -0.0121(11) C28 0.0573(14) 0.0258(12) 0.0433(13) 0.0000(10) 0.0182(11) -0.0104(10) C29 0.0458(12) 0.0278(12) 0.0348(11) -0.0009(9) 0.0182(9) -0.0036(10) C30 0.0346(11) 0.0290(12) 0.0239(9) 0.0015(8) 0.0099(8) -0.0038(9) C31 0.0384(12) 0.0347(13) 0.0345(11) 0.0057(10) 0.0114(9) -0.0025(10) C32 0.0354(12) 0.0514(16) 0.0331(11) 0.0083(10) 0.0087(9) -0.0028(11) C33 0.0428(13) 0.0589(17) 0.0294(11) -0.0022(11) 0.0107(10) -0.0186(12) C34 0.0569(15) 0.0384(14) 0.0390(12) -0.0059(10) 0.0183(11) -0.0176(12) C35 0.0453(13) 0.0328(13) 0.0329(11) 0.0022(9) 0.0137(10) -0.0033(10) C36 0.0310(10) 0.0255(11) 0.0295(10) 0.0016(8) 0.0108(8) 0.0019(9) C37 0.0315(11) 0.0344(12) 0.0313(11) 0.0034(9) 0.0087(9) 0.0009(9) C38 0.0390(12) 0.0385(13) 0.0315(11) 0.0044(9) 0.0099(9) 0.0021(10) C39 0.0412(12) 0.0371(13) 0.0343(11) 0.0003(9) 0.0181(10) -0.0012(10) C40 0.0300(12) 0.0704(18) 0.0461(13) 0.0129(12) 0.0141(10) 0.0018(11) C41 0.0307(11) 0.0695(18) 0.0340(12) 0.0176(11) 0.0059(9) 0.0042(11) C42 0.0286(10) 0.0294(12) 0.0257(10) -0.0009(8) 0.0064(8) 0.0017(9) C43 0.0284(10) 0.0307(12) 0.0294(10) 0.0015(9) 0.0067(8) -0.0002(9) C44 0.0328(11) 0.0283(12) 0.0387(12) -0.0012(9) 0.0044(9) 0.0010(9) C45 0.0309(11) 0.0385(14) 0.0333(11) -0.0065(10) 0.0031(9) 0.0073(10) C46 0.0324(11) 0.0428(14) 0.0359(11) -0.0021(10) 0.0143(9) -0.0004(10) C47 0.0341(11) 0.0307(12) 0.0413(12) -0.0002(10) 0.0152(9) -0.0030(9) C48 0.0327(11) 0.0268(12) 0.0302(11) 0.0024(9) 0.0071(8) 0.0013(9) C49 0.0549(14) 0.0412(14) 0.0327(12) -0.0017(10) 0.0019(10) 0.0150(12) C50 0.0573(15) 0.0405(15) 0.0486(14) -0.0081(11) 0.0067(12) 0.0145(12) C51 0.0355(12) 0.0348(14) 0.0499(14) 0.0112(11) 0.0031(10) 0.0032(10) C52 0.0373(12) 0.0497(15) 0.0350(12) 0.0122(11) 0.0094(10) 0.0016(11) C53 0.0358(11) 0.0406(14) 0.0315(11) 0.0053(9) 0.0120(9) 0.0021(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 Y O5 2.4191(14) . ? Y O2 2.4213(14) . ? Y O1 2.4344(14) . ? Y O4 2.4355(14) . ? Y O10 2.4395(13) . ? Y O8 2.4456(14) . ? Y O9 2.4495(13) . ? Y O7 2.4652(14) . ? Y O3 2.4902(14) . ? Y O6 2.5226(14) . ? P1 C6 1.7882(18) . ? P1 C12 1.7890(18) . ? P1 C18 1.7953(17) . ? P1 C24 1.7976(18) . ? P2 C36 1.7891(19) . ? P2 C30 1.7916(19) . ? P2 C42 1.7971(19) . ? P2 C48 1.800(2) . ? O1 N1 1.258(2) . ? O2 N1 1.266(2) . ? O3 N2 1.256(3) . ? O4 N2 1.263(3) . ? O5 N3 1.269(2) . ? O6 N3 1.257(2) . ? O7 N4 1.249(2) . ? O8 N4 1.273(2) . ? O9 N5 1.265(2) . ? O10 N5 1.267(2) . ? N6 C5 1.314(3) . ? N6 C1 1.329(3) . ? C1 C2 1.401(4) . ? C1 H1 0.9300 . ? C2 C3 1.363(4) . ? C2 H2 0.9300 . ? C3 C4 1.357(3) . ? C3 H3 0.9300 . ? C4 C5 1.356(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.386(3) . ? C6 C7 1.402(3) . ? C7 C8 1.378(3) . ? C7 H7 0.9300 . ? C8 C9 1.379(3) . ? C8 H8 0.9300 . ? C9 C10 1.379(3) . ? C9 H9 0.9300 . ? C10 C11 1.390(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.390(3) . ? C12 C13 1.398(3) . ? C13 C14 1.387(3) . ? C13 H13 0.9300 . ? C14 C15 1.369(3) . ? C14 H14 0.9300 . ? C15 C16 1.374(3) . ? C15 H15 0.9300 . ? C16 C17 1.388(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.394(2) . ? C18 C19 1.400(3) . ? C19 C20 1.385(3) . ? C19 H19 0.9300 . ? C20 C21 1.382(3) . ? C20 H20 0.9300 . ? C21 C22 1.379(3) . ? C21 H21 0.9300 . ? C22 C23 1.381(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.386(3) . ? C24 C25 1.397(2) . ? C25 C26 1.378(3) . ? C25 H25 0.9300 . ? C26 C27 1.378(3) . ? C26 H26 0.9300 . ? C27 C28 1.375(3) . ? C27 H27 0.9300 . ? C28 C29 1.380(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.390(3) . ? C30 C31 1.396(3) . ? C31 C32 1.375(3) . ? C31 H31 0.9300 . ? C32 C33 1.386(3) . ? C32 H32 0.9300 . ? C33 C34 1.374(3) . ? C33 H33 0.9300 . ? C34 C35 1.391(3) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.383(3) . ? C36 C41 1.392(3) . ? C37 C38 1.386(3) . ? C37 H37 0.9300 . ? C38 C39 1.376(3) . ? C38 H38 0.9300 . ? C39 C40 1.373(3) . ? C39 H39 0.9300 . ? C40 C41 1.379(3) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.389(3) . ? C42 C47 1.398(3) . ? C43 C44 1.385(3) . ? C43 H43 0.9300 . ? C44 C45 1.384(3) . ? C44 H44 0.9300 . ? C45 C46 1.380(3) . ? C45 H45 0.9300 . ? C46 C47 1.376(3) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.390(3) . ? C48 C53 1.393(3) . ? C49 C50 1.379(3) . ? C49 H49 0.9300 . ? C50 C51 1.375(3) . ? C50 H50 0.9300 . ? C51 C52 1.370(3) . ? C51 H51 0.9300 . ? C52 C53 1.384(3) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Y O2 155.16(5) . . ? O5 Y O1 123.54(5) . . ? O2 Y O1 51.37(5) . . ? O5 Y O4 73.27(5) . . ? O2 Y O4 123.06(5) . . ? O1 Y O4 152.36(5) . . ? O5 Y O10 78.69(5) . . ? O2 Y O10 84.44(5) . . ? O1 Y O10 119.15(5) . . ? O4 Y O10 83.75(5) . . ? O5 Y O8 83.87(5) . . ? O2 Y O8 116.76(6) . . ? O1 Y O8 83.77(5) . . ? O4 Y O8 76.06(5) . . ? O10 Y O8 156.42(5) . . ? O5 Y O9 78.26(5) . . ? O2 Y O9 76.95(5) . . ? O1 Y O9 76.96(5) . . ? O4 Y O9 130.38(5) . . ? O10 Y O9 50.96(5) . . ? O8 Y O9 139.86(5) . . ? O5 Y O7 131.53(5) . . ? O2 Y O7 72.79(5) . . ? O1 Y O7 73.08(5) . . ? O4 Y O7 79.50(5) . . ? O10 Y O7 137.28(5) . . ? O8 Y O7 50.60(5) . . ? O9 Y O7 146.49(5) . . ? O5 Y O3 116.07(6) . . ? O2 Y O3 73.43(6) . . ? O1 Y O3 120.32(6) . . ? O4 Y O3 50.43(6) . . ? O10 Y O3 68.73(5) . . ? O8 Y O3 105.87(5) . . ? O9 Y O3 114.26(5) . . ? O7 Y O3 70.29(5) . . ? O5 Y O6 50.28(5) . . ? O2 Y O6 121.24(5) . . ? O1 Y O6 73.80(5) . . ? O4 Y O6 115.25(6) . . ? O10 Y O6 109.32(5) . . ? O8 Y O6 69.78(5) . . ? O9 Y O6 71.15(5) . . ? O7 Y O6 113.38(5) . . ? O3 Y O6 165.28(6) . . ? C6 P1 C12 108.36(9) . . ? C6 P1 C18 109.90(8) . . ? C12 P1 C18 108.56(8) . . ? C6 P1 C24 107.24(8) . . ? C12 P1 C24 109.96(8) . . ? C18 P1 C24 112.73(9) . . ? C36 P2 C30 110.49(9) . . ? C36 P2 C42 110.99(9) . . ? C30 P2 C42 106.24(9) . . ? C36 P2 C48 108.32(9) . . ? C30 P2 C48 110.66(9) . . ? C42 P2 C48 110.16(9) . . ? N1 O1 Y 97.58(11) . . ? N1 O2 Y 98.00(12) . . ? N2 O3 Y 97.10(13) . . ? N2 O4 Y 99.59(14) . . ? N3 O5 Y 100.96(12) . . ? N3 O6 Y 96.20(11) . . ? N4 O7 Y 98.24(13) . . ? N4 O8 Y 98.48(12) . . ? N5 O9 Y 98.14(11) . . ? N5 O10 Y 98.56(11) . . ? O1 N1 O2 113.01(17) . . ? O3 N2 O4 112.85(18) . . ? O6 N3 O5 112.55(17) . . ? O7 N4 O8 112.68(17) . . ? O9 N5 O10 112.34(16) . . ? C5 N6 C1 116.3(2) . . ? N6 C1 C2 122.7(2) . . ? N6 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.4(2) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C4 C3 C2 118.6(2) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C5 C4 C3 119.0(2) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N6 C5 C4 125.0(2) . . ? N6 C5 H5 117.5 . . ? C4 C5 H5 117.5 . . ? C11 C6 C7 119.67(17) . . ? C11 C6 P1 120.88(14) . . ? C7 C6 P1 119.41(15) . . ? C8 C7 C6 119.95(19) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.99(19) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.57(19) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.0(2) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C6 C11 C10 119.74(19) . . ? C6 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C17 C12 C13 119.52(17) . . ? C17 C12 P1 122.13(15) . . ? C13 C12 P1 118.17(14) . . ? C14 C13 C12 119.65(19) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 121.2(2) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C17 119.6(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C12 120.0(2) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C23 C18 C19 119.61(16) . . ? C23 C18 P1 120.83(14) . . ? C19 C18 P1 119.51(14) . . ? C20 C19 C18 119.58(17) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.31(18) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 120.15(18) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.42(18) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 119.88(18) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? C29 C24 C25 119.27(17) . . ? C29 C24 P1 123.32(14) . . ? C25 C24 P1 117.36(14) . . ? C26 C25 C24 120.46(19) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 119.84(19) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 119.86(19) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 121.0(2) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C24 119.53(19) . . ? C28 C29 H29 120.2 . . ? C24 C29 H29 120.2 . . ? C35 C30 C31 119.54(18) . . ? C35 C30 P2 122.05(16) . . ? C31 C30 P2 118.40(15) . . ? C32 C31 C30 120.1(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.1(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.4(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.0(2) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C30 C35 C34 119.9(2) . . ? C30 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C41 119.18(17) . . ? C37 C36 P2 121.64(14) . . ? C41 C36 P2 119.17(14) . . ? C36 C37 C38 119.62(18) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 120.61(18) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C40 C39 C38 120.13(19) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 119.72(19) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C36 120.72(18) . . ? C40 C41 H41 119.6 . . ? C36 C41 H41 119.6 . . ? C43 C42 C47 119.70(18) . . ? C43 C42 P2 121.73(14) . . ? C47 C42 P2 118.55(15) . . ? C44 C43 C42 119.55(18) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 120.3(2) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C46 C45 C44 120.3(2) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C47 C46 C45 119.91(19) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C42 120.2(2) . . ? C46 C47 H47 119.9 . . ? C42 C47 H47 119.9 . . ? C49 C48 C53 119.31(19) . . ? C49 C48 P2 118.95(15) . . ? C53 C48 P2 121.73(16) . . ? C50 C49 C48 120.0(2) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C51 C50 C49 120.3(2) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C50 120.2(2) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 120.3(2) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C52 C53 C48 119.8(2) . . ? C52 C53 H53 120.1 . . ? C48 C53 H53 120.1 . . ? _database_code_depnum_ccdc_archive 'CCDC 963106' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 Ag N8 O12 P2 Sm' _chemical_formula_weight 1371.22 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1729(5) _cell_length_b 11.6627(5) _cell_length_c 24.7799(9) _cell_angle_alpha 95.368(3) _cell_angle_beta 93.817(3) _cell_angle_gamma 103.994(2) _cell_volume 2828.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 155212 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1378 _exptl_absorpt_coefficient_mu 1.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.823 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method '2 \f and 13 \w scans with 2\% steps (826 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 155212 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_unetI/netI 0.0678 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 30.51 _reflns_number_total 17283 _reflns_number_gt 12818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The Ag atom is disordered over two positions which were refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0313P)^2^] 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 17283 _refine_ls_number_parameters 749 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.082 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.098 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 Sm Sm 0.290823(11) 0.509412(9) 0.262786(4) 0.02818(4) Uani 1 1 d . . . Ag1 Ag -0.2400(12) 0.5221(3) 0.2456(2) 0.0596(9) Uani 0.51(2) 1 d P . . Ag2 Ag -0.2741(3) 0.5167(3) 0.24022(13) 0.0431(4) Uani 0.49(2) 1 d P . . P1 P 0.71616(5) 0.84985(5) 0.02128(2) 0.02735(12) Uani 1 1 d . . . P2 P 0.77797(5) 0.15882(5) 0.48375(2) 0.02439(11) Uani 1 1 d . . . O1 O 0.17514(16) 0.54030(15) 0.17253(7) 0.0433(4) Uani 1 1 d . . . O2 O 0.12225(17) 0.36607(14) 0.19437(7) 0.0439(4) Uani 1 1 d . . . O3 O 0.16920(17) 0.34631(15) 0.31701(7) 0.0469(4) Uani 1 1 d . . . O4 O 0.32058(17) 0.30098(14) 0.27276(7) 0.0450(4) Uani 1 1 d . . . O5 O 0.36134(18) 0.58762(16) 0.36241(7) 0.0500(4) Uani 1 1 d . . . O6 O 0.51780(17) 0.54948(16) 0.31894(8) 0.0523(5) Uani 1 1 d . . . O7 O 0.3761(2) 0.71471(16) 0.25834(9) 0.0676(6) Uani 1 1 d . . . O8 O 0.4084(3) 0.87195(19) 0.22227(11) 0.0917(8) Uani 1 1 d . . . O9 O 0.08661(16) 0.55959(14) 0.28440(6) 0.0402(4) Uani 1 1 d . . . O10 O -0.05513(17) 0.60779(16) 0.33537(7) 0.0474(4) Uani 1 1 d . . . O11 O 0.46644(18) 0.48924(17) 0.20499(8) 0.0535(5) Uani 1 1 d . . . O12 O 0.57731(19) 0.4387(2) 0.14263(8) 0.0638(6) Uani 1 1 d . . . N1 N 0.1062(2) 0.4355(2) 0.15979(9) 0.0487(5) Uani 1 1 d . . . N2 N 0.2257(2) 0.26623(18) 0.30203(9) 0.0426(5) Uani 1 1 d . . . N3 N 0.4841(2) 0.58766(18) 0.36389(9) 0.0443(5) Uani 1 1 d . . . N4 N 0.3862(4) 0.7766(3) 0.22537(13) 0.0968(11) Uani 1 1 d . . . N5 N 0.0601(2) 0.59359(18) 0.33266(8) 0.0418(5) Uani 1 1 d . . . N6 N 0.4651(3) 0.4444(2) 0.15804(10) 0.0599(6) Uani 1 1 d . . . N7 N -0.1821(2) 0.70361(17) 0.22651(8) 0.0381(4) Uani 1 1 d . . . N8 N -0.27009(19) 0.33798(16) 0.26090(8) 0.0352(4) Uani 1 1 d . . . C1 C -0.2657(3) 0.7715(2) 0.21408(9) 0.0432(6) Uani 1 1 d . . . H1 H -0.3590 0.7378 0.2097 0.052 Uiso 1 1 calc R . . C2 C -0.2177(3) 0.8907(2) 0.20744(10) 0.0559(8) Uani 1 1 d . . . H2 H -0.2780 0.9359 0.1983 0.067 Uiso 1 1 calc R . . C3 C -0.0809(4) 0.9408(2) 0.21443(11) 0.0671(9) Uani 1 1 d . . . H3 H -0.0467 1.0209 0.2108 0.081 Uiso 1 1 calc R . . C4 C 0.0045(3) 0.8714(3) 0.22682(11) 0.0607(8) Uani 1 1 d . . . H4 H 0.0980 0.9038 0.2317 0.073 Uiso 1 1 calc R . . C5 C -0.0485(3) 0.7534(2) 0.23206(10) 0.0465(6) Uani 1 1 d . . . H5 H 0.0108 0.7065 0.2398 0.056 Uiso 1 1 calc R . . C6 C -0.3898(2) 0.2577(2) 0.25536(10) 0.0428(6) Uani 1 1 d . . . H6 H -0.4671 0.2796 0.2425 0.051 Uiso 1 1 calc R . . C7 C -0.4025(3) 0.1427(2) 0.26817(11) 0.0527(7) Uani 1 1 d . . . H7 H -0.4869 0.0882 0.2642 0.063 Uiso 1 1 calc R . . C8 C -0.2881(3) 0.1109(2) 0.28678(10) 0.0556(8) Uani 1 1 d . . . H8 H -0.2939 0.0342 0.2957 0.067 Uiso 1 1 calc R . . C9 C -0.1651(3) 0.1928(2) 0.29206(10) 0.0486(6) Uani 1 1 d . . . H9 H -0.0863 0.1724 0.3043 0.058 Uiso 1 1 calc R . . C10 C -0.1597(2) 0.3047(2) 0.27905(9) 0.0390(5) Uani 1 1 d . . . H10 H -0.0760 0.3602 0.2830 0.047 Uiso 1 1 calc R . . C11 C 0.5519(2) 0.75392(19) 0.02802(9) 0.0306(5) Uani 1 1 d . . . C12 C 0.5041(2) 0.7442(2) 0.07889(10) 0.0380(5) Uani 1 1 d . . . H12 H 0.5472 0.7989 0.1083 0.046 Uiso 1 1 calc R . . C13 C 0.3928(2) 0.6537(2) 0.08626(11) 0.0458(6) Uani 1 1 d . . . H13 H 0.3609 0.6473 0.1204 0.055 Uiso 1 1 calc R . . C14 C 0.3295(2) 0.5727(2) 0.04221(12) 0.0492(7) Uani 1 1 d . . . H14 H 0.2570 0.5098 0.0471 0.059 Uiso 1 1 calc R . . C15 C 0.3731(2) 0.5848(2) -0.00873(11) 0.0460(6) Uani 1 1 d . . . H15 H 0.3271 0.5320 -0.0383 0.055 Uiso 1 1 calc R . . C16 C 0.4846(2) 0.67449(19) -0.01659(10) 0.0362(5) Uani 1 1 d . . . H16 H 0.5144 0.6818 -0.0511 0.043 Uiso 1 1 calc R . . C17 C 0.7439(2) 0.98309(19) 0.06761(8) 0.0288(4) Uani 1 1 d . . . C18 C 0.6360(2) 1.0343(2) 0.07694(9) 0.0393(5) Uani 1 1 d . . . H18 H 0.5485 0.9956 0.0619 0.047 Uiso 1 1 calc R . . C19 C 0.6590(3) 1.1428(2) 0.10867(10) 0.0451(6) Uani 1 1 d . . . H19 H 0.5867 1.1764 0.1154 0.054 Uiso 1 1 calc R . . C20 C 0.7891(3) 1.2008(2) 0.13032(9) 0.0424(6) Uani 1 1 d . . . H20 H 0.8047 1.2745 0.1509 0.051 Uiso 1 1 calc R . . C21 C 0.8968(2) 1.1498(2) 0.12145(9) 0.0389(5) Uani 1 1 d . . . H21 H 0.9843 1.1886 0.1365 0.047 Uiso 1 1 calc R . . C22 C 0.8737(2) 1.04081(19) 0.09017(9) 0.0322(5) Uani 1 1 d . . . H22 H 0.9457 1.0064 0.0843 0.039 Uiso 1 1 calc R . . C23 C 0.8394(2) 0.76804(18) 0.03767(9) 0.0298(5) Uani 1 1 d . . . C24 C 0.8237(2) 0.7034(2) 0.08221(9) 0.0379(5) Uani 1 1 d . . . H24 H 0.7514 0.7046 0.1031 0.045 Uiso 1 1 calc R . . C25 C 0.9143(3) 0.6376(2) 0.09561(10) 0.0425(6) Uani 1 1 d . . . H25 H 0.9035 0.5950 0.1256 0.051 Uiso 1 1 calc R . . C26 C 1.0204(2) 0.6351(2) 0.06460(11) 0.0464(6) Uani 1 1 d . . . H26 H 1.0818 0.5909 0.0737 0.056 Uiso 1 1 calc R . . C27 C 1.0364(3) 0.6972(3) 0.02029(13) 0.0594(8) Uani 1 1 d . . . H27 H 1.1075 0.6935 -0.0010 0.071 Uiso 1 1 calc R . . C28 C 0.9471(2) 0.7660(2) 0.00678(11) 0.0459(6) Uani 1 1 d . . . H28 H 0.9599 0.8100 -0.0227 0.055 Uiso 1 1 calc R . . C29 C 0.7289(2) 0.89079(19) -0.04650(8) 0.0291(4) Uani 1 1 d . . . C30 C 0.7320(2) 1.0077(2) -0.05582(9) 0.0352(5) Uani 1 1 d . . . H30 H 0.7348 1.0651 -0.0268 0.042 Uiso 1 1 calc R . . C31 C 0.7309(2) 1.0377(2) -0.10876(10) 0.0416(6) Uani 1 1 d . . . H31 H 0.7337 1.1155 -0.1151 0.050 Uiso 1 1 calc R . . C32 C 0.7258(2) 0.9523(2) -0.15195(10) 0.0426(6) Uani 1 1 d . . . H32 H 0.7222 0.9724 -0.1874 0.051 Uiso 1 1 calc R . . C33 C 0.7259(2) 0.8376(2) -0.14276(10) 0.0400(6) Uani 1 1 d . . . H33 H 0.7244 0.7809 -0.1720 0.048 Uiso 1 1 calc R . . C34 C 0.7281(2) 0.8066(2) -0.09063(9) 0.0354(5) Uani 1 1 d . . . H34 H 0.7292 0.7292 -0.0847 0.042 Uiso 1 1 calc R . . C35 C 0.64478(19) 0.23167(17) 0.46818(8) 0.0264(4) Uani 1 1 d . . . C36 C 0.5599(2) 0.25965(18) 0.50638(9) 0.0291(4) Uani 1 1 d . . . H36 H 0.5642 0.2336 0.5406 0.035 Uiso 1 1 calc R . . C37 C 0.4690(2) 0.32640(19) 0.49338(9) 0.0320(5) Uani 1 1 d . . . H37 H 0.4133 0.3462 0.5191 0.038 Uiso 1 1 calc R . . C38 C 0.4611(2) 0.36349(19) 0.44207(9) 0.0326(5) Uani 1 1 d . . . H38 H 0.4003 0.4086 0.4336 0.039 Uiso 1 1 calc R . . C39 C 0.5428(2) 0.3341(2) 0.40335(9) 0.0348(5) Uani 1 1 d . . . H39 H 0.5363 0.3586 0.3688 0.042 Uiso 1 1 calc R . . C40 C 0.6342(2) 0.26816(18) 0.41628(9) 0.0309(5) Uani 1 1 d . . . H40 H 0.6890 0.2479 0.3903 0.037 Uiso 1 1 calc R . . C41 C 0.75842(19) 0.09549(18) 0.54690(8) 0.0265(4) Uani 1 1 d . . . C42 C 0.7543(2) 0.16663(19) 0.59543(9) 0.0300(5) Uani 1 1 d . . . H42 H 0.7591 0.2472 0.5950 0.036 Uiso 1 1 calc R . . C43 C 0.7430(2) 0.1164(2) 0.64361(9) 0.0348(5) Uani 1 1 d . . . H43 H 0.7396 0.1634 0.6757 0.042 Uiso 1 1 calc R . . C44 C 0.7366(2) -0.0030(2) 0.64473(9) 0.0379(5) Uani 1 1 d . . . H44 H 0.7286 -0.0359 0.6775 0.045 Uiso 1 1 calc R . . C45 C 0.7421(2) -0.0739(2) 0.59738(9) 0.0359(5) Uani 1 1 d . . . H45 H 0.7394 -0.1540 0.5984 0.043 Uiso 1 1 calc R . . C46 C 0.7516(2) -0.02535(18) 0.54817(9) 0.0304(5) Uani 1 1 d . . . H46 H 0.7534 -0.0732 0.5162 0.036 Uiso 1 1 calc R . . C47 C 0.9393(2) 0.26616(18) 0.48723(9) 0.0271(4) Uani 1 1 d . . . C48 C 1.0185(2) 0.30437(19) 0.53652(9) 0.0330(5) Uani 1 1 d . . . H48 H 0.9922 0.2694 0.5676 0.040 Uiso 1 1 calc R . . C49 C 1.1369(2) 0.3947(2) 0.53927(10) 0.0396(5) Uani 1 1 d . . . H49 H 1.1903 0.4199 0.5722 0.048 Uiso 1 1 calc R . . C50 C 1.1755(2) 0.44723(19) 0.49312(9) 0.0345(5) Uani 1 1 d . . . H50 H 1.2542 0.5085 0.4952 0.041 Uiso 1 1 calc R . . C51 C 1.0979(2) 0.4092(2) 0.44413(10) 0.0392(5) Uani 1 1 d . . . H51 H 1.1244 0.4447 0.4132 0.047 Uiso 1 1 calc R . . C52 C 0.9809(2) 0.3185(2) 0.44083(9) 0.0376(5) Uani 1 1 d . . . H52 H 0.9297 0.2921 0.4075 0.045 Uiso 1 1 calc R . . C53 C 0.7670(2) 0.04107(17) 0.43050(8) 0.0270(4) Uani 1 1 d . . . C54 C 0.8843(2) 0.0094(2) 0.41556(9) 0.0342(5) Uani 1 1 d . . . H54 H 0.9695 0.0559 0.4297 0.041 Uiso 1 1 calc R . . C55 C 0.8738(2) -0.0916(2) 0.37962(9) 0.0378(5) Uani 1 1 d . . . H55 H 0.9519 -0.1130 0.3696 0.045 Uiso 1 1 calc R . . C56 C 0.7467(2) -0.1607(2) 0.35866(9) 0.0371(5) Uani 1 1 d . . . H56 H 0.7398 -0.2294 0.3352 0.045 Uiso 1 1 calc R . . C57 C 0.6296(2) -0.12845(19) 0.37234(9) 0.0351(5) Uani 1 1 d . . . H57 H 0.5447 -0.1742 0.3574 0.042 Uiso 1 1 calc R . . C58 C 0.6394(2) -0.02806(18) 0.40824(9) 0.0303(5) Uani 1 1 d . . . H58 H 0.5610 -0.0064 0.4176 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.03171(7) 0.02586(6) 0.02789(6) 0.00428(4) 0.00288(4) 0.00844(4) Ag1 0.102(2) 0.0293(4) 0.0470(8) 0.0102(4) 0.0171(12) 0.0114(9) Ag2 0.0526(10) 0.0359(5) 0.0400(5) 0.0046(3) 0.0011(5) 0.0103(4) P1 0.0265(3) 0.0281(3) 0.0270(3) 0.0022(2) 0.0012(2) 0.0067(2) P2 0.0256(3) 0.0228(3) 0.0249(3) 0.0028(2) 0.0025(2) 0.0062(2) O1 0.0484(10) 0.0434(10) 0.0376(9) 0.0113(8) 0.0018(8) 0.0086(8) O2 0.0536(10) 0.0363(9) 0.0374(10) 0.0031(8) -0.0069(8) 0.0062(8) O3 0.0582(11) 0.0445(10) 0.0472(10) 0.0151(8) 0.0211(9) 0.0221(9) O4 0.0485(10) 0.0407(10) 0.0539(11) 0.0132(8) 0.0154(9) 0.0208(8) O5 0.0539(11) 0.0569(12) 0.0376(10) -0.0028(8) -0.0036(8) 0.0159(9) O6 0.0380(10) 0.0587(12) 0.0602(13) 0.0070(10) -0.0054(9) 0.0150(9) O7 0.0921(16) 0.0357(11) 0.0654(14) 0.0198(10) -0.0187(12) -0.0008(10) O8 0.123(2) 0.0389(13) 0.103(2) 0.0273(13) -0.0244(16) 0.0019(13) O9 0.0462(9) 0.0428(10) 0.0372(9) 0.0053(8) 0.0102(8) 0.0200(8) O10 0.0422(10) 0.0673(13) 0.0364(10) 0.0016(9) 0.0070(8) 0.0216(9) O11 0.0622(12) 0.0592(12) 0.0453(11) 0.0082(9) 0.0170(9) 0.0229(10) O12 0.0482(11) 0.1000(17) 0.0450(11) -0.0114(11) 0.0089(9) 0.0279(11) N1 0.0573(14) 0.0480(14) 0.0368(12) 0.0053(10) -0.0070(10) 0.0081(11) N2 0.0488(12) 0.0362(11) 0.0451(13) 0.0123(10) 0.0039(10) 0.0126(10) N3 0.0551(14) 0.0344(11) 0.0407(12) 0.0056(10) -0.0065(10) 0.0084(10) N4 0.131(3) 0.0576(19) 0.076(2) 0.0245(17) -0.0343(19) -0.0194(19) N5 0.0457(12) 0.0428(12) 0.0343(11) 0.0001(9) 0.0002(9) 0.0085(9) N6 0.0812(18) 0.0533(15) 0.0460(15) 0.0024(12) -0.0033(13) 0.0220(13) N7 0.0489(12) 0.0346(11) 0.0313(11) 0.0061(8) 0.0019(9) 0.0109(9) N8 0.0375(11) 0.0310(10) 0.0364(11) 0.0018(8) 0.0049(8) 0.0074(8) C1 0.0515(15) 0.0542(16) 0.0277(12) 0.0015(11) 0.0012(11) 0.0226(13) C2 0.098(2) 0.0426(16) 0.0351(14) 0.0010(12) -0.0047(15) 0.0372(16) C3 0.114(3) 0.0348(15) 0.0430(17) 0.0092(13) -0.0086(17) 0.0032(17) C4 0.0641(19) 0.064(2) 0.0435(16) 0.0191(15) -0.0056(14) -0.0066(15) C5 0.0528(16) 0.0491(16) 0.0405(15) 0.0131(12) 0.0014(12) 0.0160(13) C6 0.0358(13) 0.0475(15) 0.0445(15) -0.0012(12) 0.0068(11) 0.0108(11) C7 0.0572(17) 0.0408(15) 0.0500(17) -0.0042(13) 0.0220(14) -0.0082(13) C8 0.100(2) 0.0355(15) 0.0382(15) 0.0114(12) 0.0262(15) 0.0231(16) C9 0.0635(18) 0.0544(17) 0.0365(14) 0.0064(12) 0.0059(12) 0.0302(15) C10 0.0346(12) 0.0455(14) 0.0335(13) -0.0003(11) 0.0023(10) 0.0056(11) C11 0.0284(11) 0.0314(12) 0.0322(12) 0.0072(9) 0.0004(9) 0.0072(9) C12 0.0319(12) 0.0461(14) 0.0363(13) 0.0072(11) 0.0025(10) 0.0095(10) C13 0.0390(13) 0.0495(16) 0.0559(17) 0.0234(14) 0.0181(12) 0.0141(12) C14 0.0327(13) 0.0341(14) 0.083(2) 0.0132(14) 0.0189(13) 0.0064(10) C15 0.0312(12) 0.0381(14) 0.0640(18) -0.0055(12) 0.0028(12) 0.0041(10) C16 0.0332(12) 0.0356(13) 0.0387(13) -0.0007(10) 0.0042(10) 0.0084(10) C17 0.0311(11) 0.0308(11) 0.0250(11) 0.0035(9) 0.0017(9) 0.0085(9) C18 0.0367(12) 0.0445(14) 0.0377(13) -0.0024(11) 0.0019(10) 0.0152(11) C19 0.0475(15) 0.0465(15) 0.0463(15) 0.0010(12) 0.0077(12) 0.0224(12) C20 0.0584(16) 0.0367(13) 0.0320(13) -0.0018(11) 0.0079(11) 0.0126(12) C21 0.0391(13) 0.0379(13) 0.0356(13) 0.0024(10) 0.0055(10) 0.0020(10) C22 0.0325(11) 0.0328(12) 0.0315(12) 0.0043(10) 0.0059(9) 0.0075(9) C23 0.0288(11) 0.0281(11) 0.0318(11) 0.0011(9) -0.0014(9) 0.0079(9) C24 0.0467(14) 0.0438(14) 0.0293(12) 0.0035(10) 0.0051(10) 0.0229(11) C25 0.0544(15) 0.0427(14) 0.0355(13) 0.0072(11) 0.0003(11) 0.0217(12) C26 0.0380(14) 0.0470(15) 0.0600(17) 0.0120(13) 0.0018(12) 0.0203(12) C27 0.0365(14) 0.069(2) 0.087(2) 0.0360(17) 0.0241(14) 0.0267(13) C28 0.0363(13) 0.0511(15) 0.0576(17) 0.0240(13) 0.0123(12) 0.0159(11) C29 0.0252(10) 0.0340(12) 0.0289(11) 0.0052(9) 0.0025(8) 0.0081(9) C30 0.0376(12) 0.0352(13) 0.0359(13) 0.0054(10) 0.0049(10) 0.0143(10) C31 0.0450(14) 0.0431(14) 0.0425(14) 0.0167(12) 0.0087(11) 0.0168(11) C32 0.0377(13) 0.0616(17) 0.0304(13) 0.0128(12) 0.0061(10) 0.0123(12) C33 0.0381(13) 0.0496(15) 0.0305(12) -0.0012(11) 0.0049(10) 0.0091(11) C34 0.0343(12) 0.0361(13) 0.0359(13) 0.0028(10) 0.0066(10) 0.0086(10) C35 0.0264(10) 0.0221(10) 0.0295(11) 0.0010(8) -0.0001(8) 0.0053(8) C36 0.0262(10) 0.0290(11) 0.0307(11) 0.0039(9) 0.0023(9) 0.0041(8) C37 0.0269(11) 0.0309(12) 0.0385(13) -0.0007(10) 0.0035(9) 0.0094(9) C38 0.0321(11) 0.0305(12) 0.0376(13) 0.0043(10) 0.0027(9) 0.0125(9) C39 0.0404(13) 0.0380(13) 0.0302(12) 0.0075(10) 0.0034(10) 0.0166(10) C40 0.0364(12) 0.0318(12) 0.0275(11) 0.0019(9) 0.0067(9) 0.0140(9) C41 0.0227(10) 0.0276(11) 0.0289(11) 0.0060(9) 0.0028(8) 0.0047(8) C42 0.0288(11) 0.0303(11) 0.0307(12) 0.0021(9) 0.0023(9) 0.0074(9) C43 0.0330(12) 0.0428(14) 0.0285(12) 0.0023(10) 0.0048(9) 0.0094(10) C44 0.0375(13) 0.0445(14) 0.0313(12) 0.0142(11) 0.0033(10) 0.0060(10) C45 0.0371(12) 0.0297(12) 0.0400(13) 0.0100(10) 0.0007(10) 0.0051(10) C46 0.0311(11) 0.0282(11) 0.0311(12) 0.0029(9) 0.0020(9) 0.0063(9) C47 0.0263(10) 0.0250(11) 0.0295(11) 0.0026(9) 0.0022(8) 0.0059(8) C48 0.0326(12) 0.0363(12) 0.0280(11) 0.0045(10) 0.0049(9) 0.0040(9) C49 0.0327(12) 0.0441(14) 0.0361(13) -0.0025(11) 0.0009(10) 0.0013(10) C50 0.0294(11) 0.0282(12) 0.0453(14) 0.0016(10) 0.0117(10) 0.0048(9) C51 0.0370(13) 0.0411(14) 0.0412(14) 0.0142(11) 0.0113(11) 0.0074(10) C52 0.0371(13) 0.0428(14) 0.0301(12) 0.0081(10) 0.0027(10) 0.0032(10) C53 0.0310(11) 0.0242(10) 0.0274(11) 0.0050(9) 0.0036(9) 0.0087(8) C54 0.0349(12) 0.0358(12) 0.0340(12) 0.0033(10) 0.0049(9) 0.0127(10) C55 0.0439(14) 0.0378(13) 0.0384(13) 0.0047(11) 0.0106(11) 0.0210(11) C56 0.0563(15) 0.0279(12) 0.0295(12) 0.0018(10) 0.0099(11) 0.0139(11) C57 0.0420(13) 0.0269(11) 0.0339(12) 0.0008(10) 0.0028(10) 0.0052(10) C58 0.0326(11) 0.0260(11) 0.0331(12) 0.0041(9) 0.0058(9) 0.0080(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm O7 2.3569(18) . ? Sm O9 2.3712(14) . ? Sm O11 2.4040(17) . ? Sm O2 2.5112(16) . ? Sm O6 2.5328(17) . ? Sm O5 2.5430(17) . ? Sm O3 2.5527(16) . ? Sm O4 2.5535(15) . ? Sm O1 2.5539(16) . ? Ag1 N7 2.162(3) . ? Ag1 N8 2.168(3) . ? Ag2 N8 2.201(3) . ? Ag2 N7 2.222(3) . ? P1 C29 1.793(2) . ? P1 C17 1.795(2) . ? P1 C23 1.798(2) . ? P1 C11 1.800(2) . ? P2 C53 1.791(2) . ? P2 C41 1.795(2) . ? P2 C47 1.798(2) . ? P2 C35 1.8042(19) . ? O1 N1 1.253(3) . ? O2 N1 1.261(2) . ? O3 N2 1.250(2) . ? O4 N2 1.258(2) . ? O5 N3 1.247(3) . ? O6 N3 1.260(3) . ? O7 N4 1.133(3) . ? O8 N4 1.091(3) . ? O9 N5 1.291(2) . ? O10 N5 1.228(2) . ? O11 N6 1.228(3) . ? O12 N6 1.242(3) . ? N7 C1 1.334(3) . ? N7 C5 1.335(3) . ? N8 C6 1.335(3) . ? N8 C10 1.338(3) . ? C1 C2 1.387(4) . ? C1 H1 0.9300 . ? C2 C3 1.365(4) . ? C2 H2 0.9300 . ? C3 C4 1.362(4) . ? C3 H3 0.9300 . ? C4 C5 1.373(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.384(4) . ? C6 H6 0.9300 . ? C7 C8 1.369(4) . ? C7 H7 0.9300 . ? C8 C9 1.368(4) . ? C8 H8 0.9300 . ? C9 C10 1.362(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.386(3) . ? C11 C16 1.396(3) . ? C12 C13 1.384(3) . ? C12 H12 0.9300 . ? C13 C14 1.384(4) . ? C13 H13 0.9300 . ? C14 C15 1.374(3) . ? C14 H14 0.9300 . ? C15 C16 1.383(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.383(3) . ? C17 C18 1.392(3) . ? C18 C19 1.386(3) . ? C18 H18 0.9300 . ? C19 C20 1.379(3) . ? C19 H19 0.9300 . ? C20 C21 1.389(3) . ? C20 H20 0.9300 . ? C21 C22 1.385(3) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C28 1.381(3) . ? C23 C24 1.391(3) . ? C24 C25 1.377(3) . ? C24 H24 0.9300 . ? C25 C26 1.370(3) . ? C25 H25 0.9300 . ? C26 C27 1.368(4) . ? C26 H26 0.9300 . ? C27 C28 1.394(3) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.398(3) . ? C29 C34 1.398(3) . ? C30 C31 1.389(3) . ? C30 H30 0.9300 . ? C31 C32 1.381(3) . ? C31 H31 0.9300 . ? C32 C33 1.379(3) . ? C32 H32 0.9300 . ? C33 C34 1.374(3) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.391(3) . ? C35 C40 1.397(3) . ? C36 C37 1.386(3) . ? C36 H36 0.9300 . ? C37 C38 1.384(3) . ? C37 H37 0.9300 . ? C38 C39 1.382(3) . ? C38 H38 0.9300 . ? C39 C40 1.383(3) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C46 1.398(3) . ? C41 C42 1.405(3) . ? C42 C43 1.377(3) . ? C42 H42 0.9300 . ? C43 C44 1.382(3) . ? C43 H43 0.9300 . ? C44 C45 1.383(3) . ? C44 H44 0.9300 . ? C45 C46 1.392(3) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.391(3) . ? C47 C52 1.394(3) . ? C48 C49 1.388(3) . ? C48 H48 0.9300 . ? C49 C50 1.383(3) . ? C49 H49 0.9300 . ? C50 C51 1.377(3) . ? C50 H50 0.9300 . ? C51 C52 1.380(3) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.394(3) . ? C53 C58 1.398(3) . ? C54 C55 1.387(3) . ? C54 H54 0.9300 . ? C55 C56 1.386(3) . ? C55 H55 0.9300 . ? C56 C57 1.386(3) . ? C56 H56 0.9300 . ? C57 C58 1.382(3) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sm O9 85.28(7) . . ? O7 Sm O11 84.19(7) . . ? O9 Sm O11 154.82(6) . . ? O7 Sm O2 126.40(6) . . ? O9 Sm O2 79.53(6) . . ? O11 Sm O2 88.49(6) . . ? O7 Sm O6 78.76(6) . . ? O9 Sm O6 129.99(6) . . ? O11 Sm O6 69.83(6) . . ? O2 Sm O6 145.82(6) . . ? O7 Sm O5 77.99(7) . . ? O9 Sm O5 81.83(6) . . ? O11 Sm O5 118.01(6) . . ? O2 Sm O5 147.38(6) . . ? O6 Sm O5 48.66(6) . . ? O7 Sm O3 147.39(7) . . ? O9 Sm O3 74.20(5) . . ? O11 Sm O3 124.08(6) . . ? O2 Sm O3 75.02(6) . . ? O6 Sm O3 95.12(6) . . ? O5 Sm O3 74.26(6) . . ? O7 Sm O4 152.59(7) . . ? O9 Sm O4 120.26(5) . . ? O11 Sm O4 75.81(6) . . ? O2 Sm O4 72.25(5) . . ? O6 Sm O4 76.86(6) . . ? O5 Sm O4 94.91(6) . . ? O3 Sm O4 48.30(5) . . ? O7 Sm O1 77.34(6) . . ? O9 Sm O1 74.27(5) . . ? O11 Sm O1 81.13(6) . . ? O2 Sm O1 49.08(5) . . ? O6 Sm O1 143.89(6) . . ? O5 Sm O1 146.76(6) . . ? O3 Sm O1 119.30(6) . . ? O4 Sm O1 116.95(6) . . ? N7 Ag1 N8 171.8(5) . . ? N8 Ag2 N7 154.92(17) . . ? C29 P1 C17 108.41(10) . . ? C29 P1 C23 110.35(10) . . ? C17 P1 C23 110.48(10) . . ? C29 P1 C11 111.35(10) . . ? C17 P1 C11 109.77(10) . . ? C23 P1 C11 106.48(10) . . ? C53 P2 C41 108.33(9) . . ? C53 P2 C47 110.47(9) . . ? C41 P2 C47 110.12(10) . . ? C53 P2 C35 108.04(9) . . ? C41 P2 C35 111.33(9) . . ? C47 P2 C35 108.53(9) . . ? N1 O1 Sm 97.72(13) . . ? N1 O2 Sm 99.59(13) . . ? N2 O3 Sm 99.40(13) . . ? N2 O4 Sm 99.14(12) . . ? N3 O5 Sm 99.10(14) . . ? N3 O6 Sm 99.21(13) . . ? N4 O7 Sm 136.4(2) . . ? N5 O9 Sm 125.11(13) . . ? N6 O11 Sm 133.51(18) . . ? O1 N1 O2 113.61(19) . . ? O3 N2 O4 112.81(18) . . ? O5 N3 O6 113.02(19) . . ? O8 N4 O7 138.4(4) . . ? O10 N5 O9 114.58(18) . . ? O11 N6 O12 116.1(2) . . ? C1 N7 C5 118.0(2) . . ? C1 N7 Ag1 126.7(4) . . ? C5 N7 Ag1 115.0(4) . . ? C1 N7 Ag2 117.97(19) . . ? C5 N7 Ag2 123.94(18) . . ? C6 N8 C10 118.2(2) . . ? C6 N8 Ag1 125.1(4) . . ? C10 N8 Ag1 116.6(4) . . ? C6 N8 Ag2 115.99(17) . . ? C10 N8 Ag2 125.79(17) . . ? N7 C1 C2 122.0(3) . . ? N7 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.2(2) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N7 C5 C4 122.4(2) . . ? N7 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N8 C6 C7 122.1(2) . . ? N8 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 118.6(2) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 119.4(2) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 119.0(2) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N8 C10 C9 122.7(2) . . ? N8 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C12 C11 C16 119.9(2) . . ? C12 C11 P1 120.11(17) . . ? C16 C11 P1 119.02(17) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.3(2) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 120.5(2) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.8(2) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 119.0(2) . . ? C15 C16 H16 120.5 . . ? C11 C16 H16 120.5 . . ? C22 C17 C18 119.8(2) . . ? C22 C17 P1 120.31(16) . . ? C18 C17 P1 119.66(17) . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 119.9(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.2(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 119.8(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C17 C22 C21 120.2(2) . . ? C17 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C28 C23 C24 119.4(2) . . ? C28 C23 P1 121.92(17) . . ? C24 C23 P1 118.66(16) . . ? C25 C24 C23 120.6(2) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 120.3(2) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 120.6(2) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C23 C28 C27 119.3(2) . . ? C23 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C30 C29 C34 119.3(2) . . ? C30 C29 P1 119.30(16) . . ? C34 C29 P1 121.28(16) . . ? C31 C30 C29 119.6(2) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C30 120.2(2) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C29 120.3(2) . . ? C33 C34 H34 119.9 . . ? C29 C34 H34 119.9 . . ? C36 C35 C40 119.39(18) . . ? C36 C35 P2 122.96(16) . . ? C40 C35 P2 117.49(15) . . ? C37 C36 C35 120.0(2) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 119.9(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 120.7(2) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C40 119.6(2) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C39 C40 C35 120.42(19) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? C46 C41 C42 119.51(19) . . ? C46 C41 P2 119.63(16) . . ? C42 C41 P2 120.83(15) . . ? C43 C42 C41 119.7(2) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.7(2) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C45 120.4(2) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 119.9(2) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 119.9(2) . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C48 C47 C52 119.3(2) . . ? C48 C47 P2 120.79(16) . . ? C52 C47 P2 119.70(16) . . ? C49 C48 C47 120.0(2) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C48 120.0(2) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C51 C50 C49 120.3(2) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C50 C51 C52 120.1(2) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C51 C52 C47 120.3(2) . . ? C51 C52 H52 119.9 . . ? C47 C52 H52 119.9 . . ? C54 C53 C58 119.69(19) . . ? C54 C53 P2 120.28(16) . . ? C58 C53 P2 119.63(15) . . ? C55 C54 C53 120.0(2) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C56 C55 C54 119.8(2) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C55 C56 C57 120.6(2) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C58 C57 C56 119.8(2) . . ? C58 C57 H57 120.1 . . ? C56 C57 H57 120.1 . . ? C57 C58 C53 120.12(19) . . ? C57 C58 H58 119.9 . . ? C53 C58 H58 119.9 . . ? _database_code_depnum_ccdc_archive 'CCDC 963107' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_14 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 Ag N8 O12 P2 Y' _chemical_formula_weight 1309.78 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1741(3) _cell_length_b 11.6470(5) _cell_length_c 24.6852(12) _cell_angle_alpha 95.277(2) _cell_angle_beta 94.020(3) _cell_angle_gamma 103.847(3) _cell_volume 2815.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 163001 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.798 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method '2 \f and 14 \w scans with 2\% steps (782 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 163001 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_unetI/netI 0.0711 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 30.51 _reflns_number_total 17198 _reflns_number_gt 11391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; The structure of the isomorphous Sm complex was used as a starting model. The Ag atom is disordered over two positions which were refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0334P)^2^] 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 17198 _refine_ls_number_parameters 749 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.917 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.070 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 Y Y 0.290976(18) 0.510264(16) 0.262798(7) 0.02817(5) Uani 1 1 d . . . Ag1 Ag -0.2513(8) 0.5208(2) 0.24391(14) 0.0701(6) Uani 0.510(15) 1 d P . . Ag2 Ag -0.28224(17) 0.51547(19) 0.23954(9) 0.0418(4) Uani 0.490(15) 1 d P . . P1 P 0.71666(5) 0.85211(4) 0.021544(19) 0.02824(11) Uani 1 1 d . . . P2 P 0.77753(5) 0.15822(4) 0.484128(18) 0.02520(10) Uani 1 1 d . . . O1 O 0.17847(14) 0.54236(13) 0.17462(5) 0.0412(3) Uani 1 1 d . . . O2 O 0.12716(14) 0.36842(12) 0.19684(6) 0.0425(4) Uani 1 1 d . . . O3 O 0.17355(15) 0.35216(14) 0.31677(6) 0.0466(4) Uani 1 1 d . . . O4 O 0.32599(15) 0.30894(13) 0.27274(6) 0.0460(4) Uani 1 1 d . . . O5 O 0.35710(16) 0.58783(14) 0.36021(6) 0.0509(4) Uani 1 1 d . . . O6 O 0.51300(15) 0.54832(15) 0.31693(7) 0.0517(4) Uani 1 1 d . . . O7 O 0.37506(19) 0.71084(14) 0.25904(7) 0.0678(6) Uani 1 1 d . . . O8 O 0.4112(2) 0.87186(15) 0.22457(8) 0.0730(6) Uani 1 1 d . . . O9 O 0.09245(13) 0.56029(12) 0.28343(5) 0.0376(3) Uani 1 1 d . . . O10 O -0.05199(15) 0.60591(14) 0.33373(6) 0.0467(4) Uani 1 1 d . . . O11 O 0.46074(16) 0.49214(14) 0.20563(6) 0.0516(4) Uani 1 1 d . . . O12 O 0.56760(17) 0.43838(17) 0.14235(6) 0.0608(5) Uani 1 1 d . . . N1 N 0.10909(19) 0.43742(17) 0.16162(7) 0.0475(5) Uani 1 1 d . . . N2 N 0.23314(19) 0.27331(16) 0.30265(7) 0.0414(4) Uani 1 1 d . . . N3 N 0.4804(2) 0.58847(16) 0.36208(8) 0.0449(5) Uani 1 1 d . . . N4 N 0.3829(3) 0.7717(2) 0.22529(10) 0.0900(10) Uani 1 1 d . . . N5 N 0.06438(18) 0.59387(16) 0.33170(7) 0.0413(4) Uani 1 1 d . . . N6 N 0.4555(2) 0.44447(18) 0.15836(8) 0.0593(6) Uani 1 1 d . . . N7 N -0.18614(18) 0.70237(15) 0.22577(7) 0.0391(4) Uani 1 1 d . . . N8 N -0.27125(17) 0.33819(14) 0.26082(6) 0.0359(4) Uani 1 1 d . . . C1 C -0.2672(2) 0.7731(2) 0.21388(8) 0.0435(5) Uani 1 1 d . . . H1 H -0.3608 0.7417 0.2099 0.052 Uiso 1 1 calc R . . C2 C -0.2166(3) 0.8913(2) 0.20731(9) 0.0576(7) Uani 1 1 d . . . H2 H -0.2752 0.9385 0.1986 0.069 Uiso 1 1 calc R . . C3 C -0.0783(3) 0.9385(2) 0.21381(10) 0.0664(8) Uani 1 1 d . . . H3 H -0.0422 1.0184 0.2103 0.080 Uiso 1 1 calc R . . C4 C 0.0053(3) 0.8666(2) 0.22548(9) 0.0603(7) Uani 1 1 d . . . H4 H 0.0991 0.8966 0.2298 0.072 Uiso 1 1 calc R . . C5 C -0.0519(2) 0.7481(2) 0.23078(8) 0.0468(5) Uani 1 1 d . . . H5 H 0.0052 0.6988 0.2381 0.056 Uiso 1 1 calc R . . C6 C -0.3886(2) 0.2545(2) 0.25650(9) 0.0444(5) Uani 1 1 d . . . H6 H -0.4684 0.2735 0.2441 0.053 Uiso 1 1 calc R . . C7 C -0.3948(3) 0.1408(2) 0.26982(9) 0.0528(7) Uani 1 1 d . . . H7 H -0.4776 0.0843 0.2667 0.063 Uiso 1 1 calc R . . C8 C -0.2764(3) 0.1124(2) 0.28787(9) 0.0556(7) Uani 1 1 d . . . H8 H -0.2780 0.0365 0.2971 0.067 Uiso 1 1 calc R . . C9 C -0.1566(2) 0.1980(2) 0.29193(8) 0.0477(6) Uani 1 1 d . . . H9 H -0.0754 0.1809 0.3040 0.057 Uiso 1 1 calc R . . C10 C -0.1574(2) 0.30838(19) 0.27808(8) 0.0399(5) Uani 1 1 d . . . H10 H -0.0752 0.3656 0.2807 0.048 Uiso 1 1 calc R . . C11 C 0.55236(18) 0.75724(17) 0.02845(7) 0.0302(4) Uani 1 1 d . . . C12 C 0.5043(2) 0.74827(19) 0.07975(8) 0.0386(5) Uani 1 1 d . . . H12 H 0.5471 0.8034 0.1092 0.046 Uiso 1 1 calc R . . C13 C 0.3931(2) 0.6577(2) 0.08714(10) 0.0468(5) Uani 1 1 d . . . H13 H 0.3605 0.6521 0.1213 0.056 Uiso 1 1 calc R . . C14 C 0.3311(2) 0.5754(2) 0.04310(11) 0.0506(6) Uani 1 1 d . . . H14 H 0.2592 0.5123 0.0483 0.061 Uiso 1 1 calc R . . C15 C 0.3744(2) 0.58588(19) -0.00815(10) 0.0471(6) Uani 1 1 d . . . H15 H 0.3288 0.5324 -0.0377 0.056 Uiso 1 1 calc R . . C16 C 0.48568(19) 0.67595(18) -0.01585(8) 0.0365(5) Uani 1 1 d . . . H16 H 0.5159 0.6823 -0.0504 0.044 Uiso 1 1 calc R . . C17 C 0.74513(18) 0.98557(16) 0.06768(7) 0.0298(4) Uani 1 1 d . . . C18 C 0.6383(2) 1.03825(19) 0.07699(8) 0.0398(5) Uani 1 1 d . . . H18 H 0.5507 1.0000 0.0618 0.048 Uiso 1 1 calc R . . C19 C 0.6610(2) 1.1467(2) 0.10849(9) 0.0453(5) Uani 1 1 d . . . H19 H 0.5891 1.1812 0.1148 0.054 Uiso 1 1 calc R . . C20 C 0.7925(2) 1.2039(2) 0.13072(8) 0.0441(5) Uani 1 1 d . . . H20 H 0.8087 1.2775 0.1515 0.053 Uiso 1 1 calc R . . C21 C 0.8992(2) 1.15197(18) 0.12201(8) 0.0392(5) Uani 1 1 d . . . H21 H 0.9866 1.1905 0.1373 0.047 Uiso 1 1 calc R . . C22 C 0.87646(19) 1.04237(17) 0.09056(7) 0.0333(4) Uani 1 1 d . . . H22 H 0.9482 1.0073 0.0849 0.040 Uiso 1 1 calc R . . C23 C 0.83931(18) 0.76878(16) 0.03797(7) 0.0308(4) Uani 1 1 d . . . C24 C 0.8210(2) 0.70138(18) 0.08198(8) 0.0385(5) Uani 1 1 d . . . H24 H 0.7474 0.7012 0.1023 0.046 Uiso 1 1 calc R . . C25 C 0.9116(2) 0.63506(19) 0.09549(8) 0.0429(5) Uani 1 1 d . . . H25 H 0.9001 0.5914 0.1253 0.051 Uiso 1 1 calc R . . C26 C 1.0185(2) 0.6338(2) 0.06491(10) 0.0492(6) Uani 1 1 d . . . H26 H 1.0793 0.5887 0.0739 0.059 Uiso 1 1 calc R . . C27 C 1.0366(2) 0.6986(2) 0.02096(12) 0.0614(7) Uani 1 1 d . . . H27 H 1.1086 0.6960 0.0000 0.074 Uiso 1 1 calc R . . C28 C 0.9483(2) 0.7675(2) 0.00772(10) 0.0476(6) Uani 1 1 d . . . H28 H 0.9622 0.8129 -0.0214 0.057 Uiso 1 1 calc R . . C29 C 0.72926(18) 0.89248(17) -0.04661(7) 0.0297(4) Uani 1 1 d . . . C30 C 0.7305(2) 1.00848(18) -0.05666(8) 0.0365(5) Uani 1 1 d . . . H30 H 0.7326 1.0661 -0.0277 0.044 Uiso 1 1 calc R . . C31 C 0.7286(2) 1.0382(2) -0.10994(9) 0.0431(5) Uani 1 1 d . . . H31 H 0.7305 1.1158 -0.1166 0.052 Uiso 1 1 calc R . . C32 C 0.7238(2) 0.9520(2) -0.15290(8) 0.0422(5) Uani 1 1 d . . . H32 H 0.7195 0.9714 -0.1886 0.051 Uiso 1 1 calc R . . C33 C 0.7255(2) 0.8376(2) -0.14332(8) 0.0392(5) Uani 1 1 d . . . H33 H 0.7245 0.7808 -0.1725 0.047 Uiso 1 1 calc R . . C34 C 0.72853(19) 0.80700(18) -0.09054(8) 0.0355(4) Uani 1 1 d . . . H34 H 0.7301 0.7298 -0.0842 0.043 Uiso 1 1 calc R . . C35 C 0.64492(17) 0.23163(15) 0.46840(7) 0.0263(4) Uani 1 1 d . . . C36 C 0.55989(18) 0.25936(16) 0.50663(7) 0.0298(4) Uani 1 1 d . . . H36 H 0.5641 0.2329 0.5410 0.036 Uiso 1 1 calc R . . C37 C 0.46861(18) 0.32657(17) 0.49348(8) 0.0331(4) Uani 1 1 d . . . H37 H 0.4122 0.3455 0.5191 0.040 Uiso 1 1 calc R . . C38 C 0.46155(19) 0.36534(17) 0.44234(8) 0.0329(4) Uani 1 1 d . . . H38 H 0.4011 0.4111 0.4339 0.039 Uiso 1 1 calc R . . C39 C 0.54393(19) 0.33644(17) 0.40353(8) 0.0340(4) Uani 1 1 d . . . H39 H 0.5379 0.3617 0.3690 0.041 Uiso 1 1 calc R . . C40 C 0.63528(19) 0.26979(17) 0.41649(7) 0.0320(4) Uani 1 1 d . . . H40 H 0.6906 0.2503 0.3905 0.038 Uiso 1 1 calc R . . C41 C 0.75780(17) 0.09413(16) 0.54748(7) 0.0272(4) Uani 1 1 d . . . C42 C 0.75423(17) 0.16514(17) 0.59603(7) 0.0295(4) Uani 1 1 d . . . H42 H 0.7592 0.2458 0.5956 0.035 Uiso 1 1 calc R . . C43 C 0.74330(19) 0.11472(18) 0.64482(8) 0.0354(5) Uani 1 1 d . . . H43 H 0.7395 0.1614 0.6771 0.042 Uiso 1 1 calc R . . C44 C 0.73804(19) -0.00482(19) 0.64555(8) 0.0380(5) Uani 1 1 d . . . H44 H 0.7313 -0.0379 0.6784 0.046 Uiso 1 1 calc R . . C45 C 0.74264(19) -0.07595(18) 0.59781(8) 0.0370(5) Uani 1 1 d . . . H45 H 0.7393 -0.1562 0.5987 0.044 Uiso 1 1 calc R . . C46 C 0.75218(18) -0.02640(16) 0.54877(8) 0.0310(4) Uani 1 1 d . . . H46 H 0.7548 -0.0738 0.5166 0.037 Uiso 1 1 calc R . . C47 C 0.93953(17) 0.26532(16) 0.48772(7) 0.0270(4) Uani 1 1 d . . . C48 C 1.01692(18) 0.30570(17) 0.53734(8) 0.0337(4) Uani 1 1 d . . . H48 H 0.9904 0.2717 0.5687 0.040 Uiso 1 1 calc R . . C49 C 1.13395(19) 0.39686(18) 0.54001(8) 0.0379(5) Uani 1 1 d . . . H49 H 1.1856 0.4243 0.5733 0.045 Uiso 1 1 calc R . . C50 C 1.17432(19) 0.44714(17) 0.49350(8) 0.0351(4) Uani 1 1 d . . . H50 H 1.2527 0.5085 0.4956 0.042 Uiso 1 1 calc R . . C51 C 1.0984(2) 0.40635(19) 0.44392(8) 0.0398(5) Uani 1 1 d . . . H51 H 1.1258 0.4405 0.4127 0.048 Uiso 1 1 calc R . . C52 C 0.9817(2) 0.31504(18) 0.44049(8) 0.0374(5) Uani 1 1 d . . . H52 H 0.9316 0.2868 0.4069 0.045 Uiso 1 1 calc R . . C53 C 0.76637(18) 0.03999(16) 0.43077(7) 0.0266(4) Uani 1 1 d . . . C54 C 0.8831(2) 0.00759(18) 0.41623(8) 0.0344(4) Uani 1 1 d . . . H54 H 0.9684 0.0533 0.4307 0.041 Uiso 1 1 calc R . . C55 C 0.8716(2) -0.09392(18) 0.37978(8) 0.0390(5) Uani 1 1 d . . . H55 H 0.9494 -0.1158 0.3698 0.047 Uiso 1 1 calc R . . C56 C 0.7449(2) -0.16182(17) 0.35856(8) 0.0379(5) Uani 1 1 d . . . H56 H 0.7376 -0.2308 0.3351 0.046 Uiso 1 1 calc R . . C57 C 0.6288(2) -0.12824(17) 0.37182(7) 0.0348(4) Uani 1 1 d . . . H57 H 0.5440 -0.1736 0.3566 0.042 Uiso 1 1 calc R . . C58 C 0.63816(19) -0.02708(16) 0.40777(7) 0.0305(4) Uani 1 1 d . . . H58 H 0.5601 -0.0041 0.4165 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.03117(10) 0.02549(10) 0.02847(10) 0.00508(7) 0.00260(7) 0.00750(7) Ag1 0.1271(16) 0.0315(4) 0.0528(6) 0.0120(4) 0.0254(9) 0.0143(8) Ag2 0.0469(11) 0.0379(4) 0.0399(4) 0.0039(3) 0.0011(4) 0.0105(2) P1 0.0281(3) 0.0290(3) 0.0273(2) 0.00275(19) 0.00148(19) 0.00687(19) P2 0.0262(2) 0.0242(2) 0.0252(2) 0.00230(17) 0.00217(18) 0.00639(18) O1 0.0479(9) 0.0412(9) 0.0352(8) 0.0125(6) 0.0019(6) 0.0098(7) O2 0.0522(9) 0.0360(8) 0.0358(8) 0.0032(6) -0.0039(6) 0.0065(7) O3 0.0591(10) 0.0457(9) 0.0446(9) 0.0172(7) 0.0208(7) 0.0222(8) O4 0.0487(9) 0.0438(9) 0.0546(9) 0.0153(7) 0.0155(7) 0.0223(7) O5 0.0508(10) 0.0604(11) 0.0386(8) -0.0037(7) -0.0065(7) 0.0147(8) O6 0.0411(9) 0.0610(11) 0.0535(10) 0.0064(8) -0.0036(7) 0.0161(8) O7 0.0901(14) 0.0336(9) 0.0684(12) 0.0197(8) -0.0231(10) -0.0031(9) O8 0.0964(15) 0.0353(10) 0.0805(13) 0.0232(9) -0.0104(11) 0.0019(9) O9 0.0434(8) 0.0398(8) 0.0330(7) 0.0028(6) 0.0052(6) 0.0170(6) O10 0.0423(9) 0.0631(10) 0.0382(8) 0.0016(7) 0.0091(7) 0.0199(8) O11 0.0617(10) 0.0547(10) 0.0425(9) 0.0070(7) 0.0146(7) 0.0191(8) O12 0.0466(10) 0.0921(14) 0.0458(9) -0.0095(9) 0.0095(7) 0.0261(9) N1 0.0541(12) 0.0508(12) 0.0345(10) 0.0050(8) -0.0027(8) 0.0091(9) N2 0.0496(11) 0.0344(10) 0.0419(10) 0.0099(8) 0.0033(8) 0.0119(8) N3 0.0531(12) 0.0332(10) 0.0446(11) 0.0061(8) -0.0081(9) 0.0060(8) N4 0.133(2) 0.0473(15) 0.0672(16) 0.0212(12) -0.0258(15) -0.0178(15) N5 0.0425(10) 0.0460(11) 0.0339(9) -0.0001(8) 0.0031(8) 0.0101(8) N6 0.0760(15) 0.0503(13) 0.0485(12) -0.0015(10) -0.0054(11) 0.0155(11) N7 0.0485(11) 0.0389(10) 0.0321(9) 0.0066(7) 0.0038(8) 0.0141(8) N8 0.0390(10) 0.0307(9) 0.0369(9) 0.0013(7) 0.0053(7) 0.0069(7) C1 0.0560(14) 0.0511(14) 0.0267(10) 0.0023(9) 0.0022(9) 0.0212(11) C2 0.100(2) 0.0505(15) 0.0312(12) 0.0017(10) -0.0070(12) 0.0413(14) C3 0.107(2) 0.0373(14) 0.0435(14) 0.0094(11) -0.0140(14) 0.0006(14) C4 0.0623(16) 0.0656(17) 0.0434(13) 0.0188(12) -0.0048(12) -0.0048(14) C5 0.0541(14) 0.0522(14) 0.0384(12) 0.0127(10) 0.0006(10) 0.0197(11) C6 0.0325(11) 0.0511(14) 0.0470(13) -0.0044(10) 0.0058(9) 0.0083(10) C7 0.0593(16) 0.0406(13) 0.0490(14) -0.0039(10) 0.0223(11) -0.0078(11) C8 0.098(2) 0.0361(13) 0.0399(13) 0.0097(10) 0.0249(13) 0.0231(13) C9 0.0582(15) 0.0569(15) 0.0341(11) 0.0050(10) 0.0040(10) 0.0264(12) C10 0.0364(12) 0.0412(12) 0.0376(11) -0.0018(9) 0.0037(9) 0.0031(9) C11 0.0262(10) 0.0311(10) 0.0338(10) 0.0069(8) 0.0015(7) 0.0070(7) C12 0.0344(11) 0.0451(12) 0.0369(11) 0.0088(9) 0.0047(8) 0.0093(9) C13 0.0440(13) 0.0484(14) 0.0542(14) 0.0205(11) 0.0170(10) 0.0147(10) C14 0.0329(12) 0.0359(12) 0.0860(18) 0.0137(12) 0.0207(11) 0.0075(9) C15 0.0330(12) 0.0405(13) 0.0628(15) -0.0051(11) 0.0040(10) 0.0036(9) C16 0.0331(11) 0.0377(11) 0.0377(11) 0.0012(8) 0.0031(8) 0.0085(8) C17 0.0307(10) 0.0305(10) 0.0268(9) 0.0034(7) 0.0033(7) 0.0045(8) C18 0.0375(11) 0.0442(12) 0.0383(11) 0.0008(9) 0.0005(9) 0.0134(9) C19 0.0498(13) 0.0506(14) 0.0418(12) 0.0012(10) 0.0098(10) 0.0247(11) C20 0.0596(14) 0.0376(12) 0.0334(11) -0.0015(9) 0.0075(10) 0.0096(10) C21 0.0405(12) 0.0364(11) 0.0358(11) 0.0012(9) 0.0043(9) 0.0009(9) C22 0.0340(10) 0.0355(11) 0.0309(10) 0.0047(8) 0.0070(8) 0.0079(8) C23 0.0280(10) 0.0281(10) 0.0340(10) 0.0008(8) -0.0033(8) 0.0055(8) C24 0.0494(13) 0.0413(12) 0.0292(10) 0.0027(8) 0.0048(9) 0.0201(10) C25 0.0528(13) 0.0448(13) 0.0355(11) 0.0080(9) 0.0011(10) 0.0204(10) C26 0.0407(13) 0.0485(14) 0.0643(15) 0.0140(11) 0.0008(11) 0.0210(10) C27 0.0399(13) 0.0739(18) 0.0872(19) 0.0380(15) 0.0254(13) 0.0302(12) C28 0.0337(12) 0.0544(14) 0.0613(15) 0.0270(11) 0.0115(10) 0.0137(10) C29 0.0257(9) 0.0319(10) 0.0314(10) 0.0026(8) 0.0039(7) 0.0070(7) C30 0.0391(11) 0.0368(11) 0.0348(11) 0.0040(8) 0.0057(8) 0.0110(9) C31 0.0490(13) 0.0436(13) 0.0431(12) 0.0132(10) 0.0100(10) 0.0190(10) C32 0.0387(12) 0.0584(15) 0.0314(11) 0.0117(10) 0.0061(9) 0.0126(10) C33 0.0341(11) 0.0487(13) 0.0343(11) 0.0011(9) 0.0076(8) 0.0090(9) C34 0.0359(11) 0.0355(11) 0.0351(11) 0.0030(8) 0.0080(8) 0.0080(8) C35 0.0276(9) 0.0228(9) 0.0282(9) 0.0013(7) 0.0003(7) 0.0065(7) C36 0.0283(10) 0.0320(10) 0.0292(9) 0.0056(8) 0.0028(7) 0.0065(8) C37 0.0283(10) 0.0334(10) 0.0385(11) 0.0019(8) 0.0051(8) 0.0095(8) C38 0.0308(10) 0.0314(10) 0.0389(11) 0.0057(8) 0.0018(8) 0.0122(8) C39 0.0385(11) 0.0360(11) 0.0309(10) 0.0076(8) 0.0021(8) 0.0146(9) C40 0.0365(11) 0.0329(10) 0.0297(10) 0.0033(8) 0.0073(8) 0.0137(8) C41 0.0233(9) 0.0289(10) 0.0292(9) 0.0047(7) 0.0016(7) 0.0062(7) C42 0.0277(10) 0.0305(10) 0.0303(9) 0.0029(7) 0.0022(7) 0.0075(8) C43 0.0331(11) 0.0430(12) 0.0297(10) 0.0036(8) 0.0037(8) 0.0091(9) C44 0.0365(11) 0.0446(12) 0.0323(10) 0.0136(9) 0.0035(8) 0.0054(9) C45 0.0370(11) 0.0315(11) 0.0408(11) 0.0112(9) 0.0011(9) 0.0035(8) C46 0.0306(10) 0.0301(10) 0.0316(10) 0.0028(8) 0.0017(8) 0.0064(8) C47 0.0244(9) 0.0265(9) 0.0307(9) 0.0035(7) 0.0035(7) 0.0071(7) C48 0.0313(10) 0.0384(11) 0.0297(10) 0.0062(8) 0.0042(8) 0.0043(8) C49 0.0328(11) 0.0424(12) 0.0328(10) -0.0023(9) 0.0015(8) 0.0015(9) C50 0.0298(10) 0.0285(10) 0.0459(12) 0.0012(8) 0.0116(8) 0.0043(8) C51 0.0386(12) 0.0426(12) 0.0397(11) 0.0150(9) 0.0115(9) 0.0070(9) C52 0.0356(11) 0.0451(12) 0.0289(10) 0.0079(9) 0.0021(8) 0.0038(9) C53 0.0317(10) 0.0262(9) 0.0238(9) 0.0033(7) 0.0040(7) 0.0101(7) C54 0.0326(10) 0.0365(11) 0.0358(10) 0.0008(8) 0.0030(8) 0.0129(8) C55 0.0446(12) 0.0404(12) 0.0387(11) 0.0036(9) 0.0107(9) 0.0219(9) C56 0.0571(14) 0.0283(10) 0.0299(10) 0.0026(8) 0.0083(9) 0.0126(9) C57 0.0404(11) 0.0275(10) 0.0328(10) 0.0021(8) 0.0023(8) 0.0022(8) C58 0.0312(10) 0.0292(10) 0.0316(10) 0.0048(8) 0.0052(8) 0.0075(8) _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 Y O7 2.3005(15) . ? Y O9 2.3089(14) . ? Y O11 2.3410(15) . ? Y O2 2.4424(13) . ? Y O6 2.4644(14) . ? Y O5 2.4766(14) . ? Y O4 2.4857(15) . ? Y O1 2.4886(13) . ? Y O3 2.4929(14) . ? Ag1 N7 2.159(3) . ? Ag1 N8 2.169(3) . ? Ag2 N8 2.203(3) . ? Ag2 N7 2.230(3) . ? P1 C17 1.7916(19) . ? P1 C29 1.7930(18) . ? P1 C11 1.7985(18) . ? P1 C23 1.801(2) . ? P2 C53 1.7930(18) . ? P2 C41 1.7973(18) . ? P2 C35 1.8006(19) . ? P2 C47 1.8043(17) . ? O1 N1 1.256(2) . ? O2 N1 1.270(2) . ? O3 N2 1.253(2) . ? O4 N2 1.256(2) . ? O5 N3 1.251(2) . ? O6 N3 1.265(2) . ? O7 N4 1.137(3) . ? O8 N4 1.135(3) . ? O9 N5 1.292(2) . ? O10 N5 1.229(2) . ? O11 N6 1.237(2) . ? O12 N6 1.249(3) . ? N7 C5 1.334(3) . ? N7 C1 1.334(3) . ? N8 C6 1.339(2) . ? N8 C10 1.340(3) . ? C1 C2 1.378(3) . ? C1 H1 0.9300 . ? C2 C3 1.374(4) . ? C2 H2 0.9300 . ? C3 C4 1.362(4) . ? C3 H3 0.9300 . ? C4 C5 1.386(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.381(3) . ? C6 H6 0.9300 . ? C7 C8 1.379(4) . ? C7 H7 0.9300 . ? C8 C9 1.368(3) . ? C8 H8 0.9300 . ? C9 C10 1.362(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.393(3) . ? C11 C16 1.397(3) . ? C12 C13 1.386(3) . ? C12 H12 0.9300 . ? C13 C14 1.386(3) . ? C13 H13 0.9300 . ? C14 C15 1.375(3) . ? C14 H14 0.9300 . ? C15 C16 1.385(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.392(3) . ? C17 C22 1.394(3) . ? C18 C19 1.382(3) . ? C18 H18 0.9300 . ? C19 C20 1.392(3) . ? C19 H19 0.9300 . ? C20 C21 1.384(3) . ? C20 H20 0.9300 . ? C21 C22 1.392(3) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C28 1.382(3) . ? C23 C24 1.395(3) . ? C24 C25 1.380(3) . ? C24 H24 0.9300 . ? C25 C26 1.368(3) . ? C25 H25 0.9300 . ? C26 C27 1.376(3) . ? C26 H26 0.9300 . ? C27 C28 1.383(3) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.393(3) . ? C29 C34 1.401(3) . ? C30 C31 1.390(3) . ? C30 H30 0.9300 . ? C31 C32 1.381(3) . ? C31 H31 0.9300 . ? C32 C33 1.378(3) . ? C32 H32 0.9300 . ? C33 C34 1.382(3) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.391(3) . ? C35 C40 1.399(2) . ? C36 C37 1.390(3) . ? C36 H36 0.9300 . ? C37 C38 1.382(3) . ? C37 H37 0.9300 . ? C38 C39 1.386(3) . ? C38 H38 0.9300 . ? C39 C40 1.385(3) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C46 1.395(3) . ? C41 C42 1.400(3) . ? C42 C43 1.388(3) . ? C42 H42 0.9300 . ? C43 C44 1.382(3) . ? C43 H43 0.9300 . ? C44 C45 1.387(3) . ? C44 H44 0.9300 . ? C45 C46 1.388(3) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.387(2) . ? C47 C52 1.398(2) . ? C48 C49 1.386(2) . ? C48 H48 0.9300 . ? C49 C50 1.380(3) . ? C49 H49 0.9300 . ? C50 C51 1.380(3) . ? C50 H50 0.9300 . ? C51 C52 1.383(3) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.390(3) . ? C53 C58 1.400(2) . ? C54 C55 1.394(3) . ? C54 H54 0.9300 . ? C55 C56 1.380(3) . ? C55 H55 0.9300 . ? C56 C57 1.381(3) . ? C56 H56 0.9300 . ? C57 C58 1.388(3) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Y O9 85.16(6) . . ? O7 Y O11 83.71(7) . . ? O9 Y O11 153.78(5) . . ? O7 Y O2 127.77(5) . . ? O9 Y O2 79.77(5) . . ? O11 Y O2 88.47(5) . . ? O7 Y O6 78.38(6) . . ? O9 Y O6 130.67(5) . . ? O11 Y O6 69.73(6) . . ? O2 Y O6 144.82(6) . . ? O7 Y O5 77.29(6) . . ? O9 Y O5 81.15(5) . . ? O11 Y O5 119.13(5) . . ? O2 Y O5 146.51(5) . . ? O6 Y O5 50.03(5) . . ? O7 Y O4 150.97(6) . . ? O9 Y O4 121.81(5) . . ? O11 Y O4 75.50(5) . . ? O2 Y O4 72.34(5) . . ? O6 Y O4 75.54(5) . . ? O5 Y O4 95.23(5) . . ? O7 Y O1 77.36(5) . . ? O9 Y O1 73.90(5) . . ? O11 Y O1 80.52(5) . . ? O2 Y O1 50.44(5) . . ? O6 Y O1 143.26(5) . . ? O5 Y O1 145.60(5) . . ? O4 Y O1 117.92(5) . . ? O7 Y O3 146.68(6) . . ? O9 Y O3 74.47(5) . . ? O11 Y O3 124.99(5) . . ? O2 Y O3 74.73(5) . . ? O6 Y O3 95.04(5) . . ? O5 Y O3 73.77(5) . . ? O4 Y O3 49.53(5) . . ? O1 Y O3 120.07(5) . . ? N7 Ag1 N8 167.7(4) . . ? N8 Ag2 N7 152.09(10) . . ? C17 P1 C29 108.39(9) . . ? C17 P1 C11 109.73(9) . . ? C29 P1 C11 111.38(8) . . ? C17 P1 C23 110.81(9) . . ? C29 P1 C23 110.16(9) . . ? C11 P1 C23 106.38(9) . . ? C53 P2 C41 107.97(8) . . ? C53 P2 C35 108.18(8) . . ? C41 P2 C35 111.42(9) . . ? C53 P2 C47 110.43(8) . . ? C41 P2 C47 110.24(8) . . ? C35 P2 C47 108.58(8) . . ? N1 O1 Y 97.55(11) . . ? N1 O2 Y 99.43(11) . . ? N2 O3 Y 98.74(11) . . ? N2 O4 Y 99.03(12) . . ? N3 O5 Y 98.74(12) . . ? N3 O6 Y 98.89(12) . . ? N4 O7 Y 134.88(17) . . ? N5 O9 Y 125.61(12) . . ? N6 O11 Y 132.04(15) . . ? O1 N1 O2 112.58(15) . . ? O3 N2 O4 112.49(17) . . ? O5 N3 O6 112.30(16) . . ? O8 N4 O7 134.2(3) . . ? O10 N5 O9 114.39(15) . . ? O11 N6 O12 115.07(19) . . ? C5 N7 C1 118.41(19) . . ? C5 N7 Ag1 115.4(3) . . ? C1 N7 Ag1 126.0(3) . . ? C5 N7 Ag2 123.28(16) . . ? C1 N7 Ag2 118.26(15) . . ? C6 N8 C10 117.90(19) . . ? C6 N8 Ag1 125.0(3) . . ? C10 N8 Ag1 117.1(3) . . ? C6 N8 Ag2 116.84(15) . . ? C10 N8 Ag2 125.25(14) . . ? N7 C1 C2 122.1(2) . . ? N7 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.1(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N7 C5 C4 122.3(2) . . ? N7 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N8 C6 C7 122.1(2) . . ? N8 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 119.0(2) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C9 C8 C7 118.8(2) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C10 C9 C8 119.3(2) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N8 C10 C9 122.92(19) . . ? N8 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C12 C11 C16 119.56(17) . . ? C12 C11 P1 120.24(14) . . ? C16 C11 P1 119.04(15) . . ? C13 C12 C11 120.30(19) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.3(2) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 120.89(19) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 119.76(19) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C18 C17 C22 119.80(18) . . ? C18 C17 P1 120.00(14) . . ? C22 C17 P1 119.96(16) . . ? C19 C18 C17 120.72(19) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 119.3(2) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.36(19) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 119.4(2) . . ? C21 C22 H22 120.3 . . ? C17 C22 H22 120.3 . . ? C28 C23 C24 119.37(19) . . ? C28 C23 P1 122.16(15) . . ? C24 C23 P1 118.46(15) . . ? C25 C24 C23 120.3(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.5(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C23 C28 C27 119.7(2) . . ? C23 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C34 119.38(17) . . ? C30 C29 P1 119.63(15) . . ? C34 C29 P1 120.85(15) . . ? C31 C30 C29 120.09(19) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.55(19) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 120.3(2) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C29 119.9(2) . . ? C33 C34 H34 120.1 . . ? C29 C34 H34 120.1 . . ? C36 C35 C40 119.32(17) . . ? C36 C35 P2 122.92(14) . . ? C40 C35 P2 117.58(14) . . ? C37 C36 C35 120.00(17) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.12(18) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.45(19) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 119.64(18) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C35 120.45(18) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? C46 C41 C42 119.61(17) . . ? C46 C41 P2 119.71(14) . . ? C42 C41 P2 120.62(14) . . ? C43 C42 C41 119.76(18) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C42 120.05(19) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.75(18) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C44 C45 C46 119.51(19) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C46 C41 120.31(18) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C48 C47 C52 119.76(16) . . ? C48 C47 P2 120.81(13) . . ? C52 C47 P2 119.22(14) . . ? C49 C48 C47 119.80(17) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C50 C49 C48 120.36(18) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 120.04(17) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C52 120.34(18) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C47 119.68(18) . . ? C51 C52 H52 120.2 . . ? C47 C52 H52 120.2 . . ? C54 C53 C58 120.17(17) . . ? C54 C53 P2 120.22(14) . . ? C58 C53 P2 119.30(14) . . ? C53 C54 C55 119.60(18) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C56 C55 C54 120.01(19) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.54(19) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C56 C57 C58 120.30(18) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C57 C58 C53 119.33(18) . . ? C57 C58 H58 120.3 . . ? C53 C58 H58 120.3 . . ? _database_code_depnum_ccdc_archive 'CCDC 963108'