# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email creutz@mit.edu _publ_contact_author_name 'Christopher Cummins' loop_ _publ_author_name 'Ivo Krummenacher' 'Sid Creutz' 'Christopher Cummins' 'Christopher Clough' data_09262 _database_code_depnum_ccdc_archive 'CCDC 789234' #TrackingRef '2139_web_deposit_cif_file_0_SidCreutz_1281723785.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; (THT)AuP(Ph2CCO)3Nb(N[CH2tBu]Ar)3 2.5.THF ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H118 Au N3 Nb O5.50 P S' _chemical_formula_weight 1742.83 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 26.964(4) _cell_length_b 14.146(2) _cell_length_c 24.947(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.938(2) _cell_angle_gamma 90.00 _cell_volume 8483(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9010 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 31.35 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3616 _exptl_absorpt_coefficient_mu 1.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4724 _exptl_absorpt_correction_T_max 0.5077 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 221113 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 29.57 _reflns_number_total 23816 _reflns_number_gt 19101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.3.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+34.2332P] 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 23816 _refine_ls_number_parameters 1006 _refine_ls_number_restraints 186 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.597862(5) 0.079214(9) 1.293978(6) 0.01623(4) Uani 1 1 d . . . Nb1 Nb 0.785873(11) -0.07957(2) 1.270182(12) 0.01309(6) Uani 1 1 d . . . P1 P 0.67049(3) 0.01400(6) 1.28341(4) 0.01391(15) Uani 1 1 d . . . S1 S 0.52723(3) 0.16830(6) 1.29864(4) 0.02163(17) Uani 1 1 d . . . O1 O 0.71665(9) -0.00020(16) 1.21044(10) 0.0160(4) Uani 1 1 d . . . N1 N 0.77280(11) -0.1677(2) 1.20073(13) 0.0170(5) Uani 1 1 d . . . C1 C 0.46501(16) 0.1018(3) 1.2874(2) 0.0309(9) Uani 1 1 d . . . H1A H 0.4367 0.1027 1.2447 0.037 Uiso 1 1 calc R . . H1B H 0.4742 0.0354 1.3008 0.037 Uiso 1 1 calc R . . O2 O 0.72408(9) -0.14481(16) 1.28625(11) 0.0170(4) Uani 1 1 d . . . N2 N 0.83989(11) 0.0076(2) 1.25837(12) 0.0162(5) Uani 1 1 d . . . C2 C 0.44507(17) 0.1557(3) 1.3268(2) 0.0359(10) Uani 1 1 d . . . H2A H 0.4297 0.2179 1.3087 0.043 Uiso 1 1 calc R . . H2B H 0.4157 0.1196 1.3313 0.043 Uiso 1 1 calc R . . O3 O 0.78144(9) 0.01829(16) 1.33164(10) 0.0164(4) Uani 1 1 d . . . N3 N 0.84242(11) -0.16004(19) 1.33735(12) 0.0163(5) Uani 1 1 d . . . C3 C 0.49525(18) 0.1687(4) 1.3875(2) 0.0369(10) Uani 1 1 d . . . H3A H 0.5031 0.1093 1.4109 0.044 Uiso 1 1 calc R . . H3B H 0.4878 0.2190 1.4105 0.044 Uiso 1 1 calc R . . C4 C 0.54504(16) 0.1958(3) 1.37730(18) 0.0286(8) Uani 1 1 d . . . H4A H 0.5783 0.1596 1.4048 0.034 Uiso 1 1 calc R . . H4B H 0.5532 0.2641 1.3852 0.034 Uiso 1 1 calc R . . C11 C 0.80428(14) -0.2541(2) 1.20948(16) 0.0208(7) Uani 1 1 d . . . C12 C 0.79583(15) -0.3294(3) 1.24046(17) 0.0230(7) Uani 1 1 d . . . H12 H 0.7702 -0.3227 1.2566 0.028 Uiso 1 1 calc R . . C13 C 0.82462(17) -0.4146(3) 1.2481(2) 0.0310(8) Uani 1 1 d . . . C14 C 0.86197(17) -0.4224(3) 1.2237(2) 0.0348(9) Uani 1 1 d . . . H14 H 0.8816 -0.4800 1.2285 0.042 Uiso 1 1 calc R . . C15 C 0.87112(16) -0.3486(3) 1.19290(19) 0.0316(9) Uani 1 1 d . . . C16 C 0.84210(14) -0.2638(3) 1.18596(17) 0.0253(7) Uani 1 1 d . . . H16 H 0.8482 -0.2125 1.1651 0.030 Uiso 1 1 calc R . . C17 C 0.73645(14) -0.1492(2) 1.13583(15) 0.0187(6) Uani 1 1 d . . . H17A H 0.7606 -0.1467 1.1155 0.022 Uiso 1 1 calc R . . H17B H 0.7201 -0.0855 1.1324 0.022 Uiso 1 1 calc R . . C18 C 0.68821(14) -0.2183(3) 1.09988(16) 0.0215(7) Uani 1 1 d . . . C21 C 0.85869(13) -0.0122(2) 1.21353(16) 0.0184(6) Uani 1 1 d . . . C22 C 0.91246(14) -0.0465(3) 1.23112(17) 0.0230(7) Uani 1 1 d . . . H22 H 0.9362 -0.0590 1.2724 0.028 Uiso 1 1 calc R . . C23 C 0.93139(16) -0.0623(3) 1.18829(19) 0.0288(8) Uani 1 1 d . . . C24 C 0.89599(17) -0.0442(3) 1.12797(19) 0.0290(8) Uani 1 1 d . . . H24 H 0.9088 -0.0554 1.0988 0.035 Uiso 1 1 calc R . . C25 C 0.84229(15) -0.0102(3) 1.10945(16) 0.0225(7) Uani 1 1 d . . . C26 C 0.82408(14) 0.0056(2) 1.15324(16) 0.0196(6) Uani 1 1 d . . . H26 H 0.7875 0.0287 1.1414 0.023 Uiso 1 1 calc R . . C27 C 0.87058(13) 0.0884(2) 1.29661(15) 0.0188(6) Uani 1 1 d . . . H27A H 0.9105 0.0712 1.3165 0.023 Uiso 1 1 calc R . . H27B H 0.8588 0.0943 1.3287 0.023 Uiso 1 1 calc R . . C28 C 0.86584(14) 0.1885(2) 1.26839(16) 0.0199(7) Uani 1 1 d . . . C31 C 0.90088(13) -0.1532(2) 1.35372(15) 0.0190(6) Uani 1 1 d . . . C32 C 0.92779(14) -0.2271(3) 1.34004(17) 0.0244(7) Uani 1 1 d . . . H32 H 0.9074 -0.2817 1.3198 0.029 Uiso 1 1 calc R . . C33 C 0.98459(15) -0.2207(3) 1.35603(17) 0.0267(8) Uani 1 1 d . . . C34 C 1.01356(15) -0.1396(3) 1.38499(17) 0.0284(8) Uani 1 1 d . . . H34 H 1.0519 -0.1342 1.3948 0.034 Uiso 1 1 calc R . . C35 C 0.98763(14) -0.0660(3) 1.39988(16) 0.0243(7) Uani 1 1 d . . . C36 C 0.93137(13) -0.0744(3) 1.38467(15) 0.0194(6) Uani 1 1 d . . . H36 H 0.9135 -0.0256 1.3956 0.023 Uiso 1 1 calc R . . C37 C 0.83133(14) -0.2379(2) 1.37071(15) 0.0198(6) Uani 1 1 d . . . H37A H 0.8495 -0.2957 1.3657 0.024 Uiso 1 1 calc R . . H37B H 0.7907 -0.2499 1.3509 0.024 Uiso 1 1 calc R . . C38 C 0.85001(14) -0.2250(3) 1.43902(16) 0.0230(7) Uani 1 1 d . . . C40 C 0.66705(13) 0.0129(2) 1.20738(14) 0.0151(6) Uani 1 1 d . . . C41 C 0.62206(13) 0.0624(2) 1.09982(15) 0.0184(6) Uani 1 1 d . . . C42 C 0.57573(15) 0.0478(3) 1.04364(16) 0.0249(7) Uani 1 1 d . . . H42 H 0.5428 0.0212 1.0422 0.030 Uiso 1 1 calc R . . C43 C 0.57712(17) 0.0714(3) 0.99042(17) 0.0313(9) Uani 1 1 d . . . H43 H 0.5452 0.0617 0.9530 0.038 Uiso 1 1 calc R . . C44 C 0.62485(18) 0.1089(4) 0.99164(19) 0.0367(10) Uani 1 1 d . . . H44 H 0.6263 0.1229 0.9552 0.044 Uiso 1 1 calc R . . C45 C 0.67072(17) 0.1259(3) 1.0465(2) 0.0349(9) Uani 1 1 d . . . H45 H 0.7032 0.1534 1.0475 0.042 Uiso 1 1 calc R . . C46 C 0.66945(15) 0.1031(3) 1.09995(17) 0.0253(8) Uani 1 1 d . . . H46 H 0.7012 0.1152 1.1371 0.030 Uiso 1 1 calc R . . C50 C 0.61998(13) 0.0371(2) 1.15641(15) 0.0167(6) Uani 1 1 d . . . C51 C 0.56470(13) 0.0330(2) 1.15566(14) 0.0166(6) Uani 1 1 d . . . C52 C 0.54863(14) -0.0471(3) 1.17683(16) 0.0202(7) Uani 1 1 d . . . H52 H 0.5732 -0.0996 1.1911 0.024 Uiso 1 1 calc R . . C53 C 0.49736(15) -0.0514(3) 1.17741(17) 0.0239(7) Uani 1 1 d . . . H53 H 0.4878 -0.1056 1.1932 0.029 Uiso 1 1 calc R . . C54 C 0.46022(14) 0.0232(3) 1.15503(16) 0.0241(7) Uani 1 1 d . . . H54 H 0.4249 0.0198 1.1548 0.029 Uiso 1 1 calc R . . C55 C 0.47492(14) 0.1032(3) 1.13284(17) 0.0235(7) Uani 1 1 d . . . H55 H 0.4496 0.1544 1.1173 0.028 Uiso 1 1 calc R . . C56 C 0.52674(14) 0.1082(3) 1.13337(16) 0.0214(7) Uani 1 1 d . . . H56 H 0.5365 0.1632 1.1185 0.026 Uiso 1 1 calc R . . C60 C 0.68871(12) -0.1108(2) 1.30498(14) 0.0154(6) Uani 1 1 d . . . C61 C 0.67346(13) -0.2673(2) 1.34126(15) 0.0180(6) Uani 1 1 d . . . C62 C 0.67239(14) -0.3103(3) 1.39169(17) 0.0228(7) Uani 1 1 d . . . H62 H 0.6639 -0.2734 1.4183 0.027 Uiso 1 1 calc R . . C63 C 0.68364(15) -0.4065(3) 1.40294(19) 0.0271(8) Uani 1 1 d . . . H63 H 0.6832 -0.4343 1.4374 0.033 Uiso 1 1 calc R . . C64 C 0.69544(16) -0.4618(3) 1.3644(2) 0.0314(9) Uani 1 1 d . . . H64 H 0.7045 -0.5267 1.3730 0.038 Uiso 1 1 calc R . . C65 C 0.69393(16) -0.4212(3) 1.3130(2) 0.0299(8) Uani 1 1 d . . . H65 H 0.7000 -0.4594 1.2852 0.036 Uiso 1 1 calc R . . C66 C 0.68357(14) -0.3254(3) 1.30181(17) 0.0226(7) Uani 1 1 d . . . H66 H 0.6833 -0.2986 1.2668 0.027 Uiso 1 1 calc R . . C70 C 0.66386(13) -0.1638(2) 1.33169(14) 0.0159(6) Uani 1 1 d . . . C71 C 0.62959(13) -0.1217(2) 1.35908(15) 0.0174(6) Uani 1 1 d . . . C72 C 0.57433(14) -0.1516(3) 1.33934(17) 0.0223(7) Uani 1 1 d . . . H72 H 0.5575 -0.1919 1.3053 0.027 Uiso 1 1 calc R . . C73 C 0.54412(16) -0.1225(3) 1.36920(19) 0.0300(8) Uani 1 1 d . . . H73 H 0.5066 -0.1424 1.3552 0.036 Uiso 1 1 calc R . . C74 C 0.56859(18) -0.0647(3) 1.41944(19) 0.0340(9) Uani 1 1 d . . . H74 H 0.5481 -0.0460 1.4402 0.041 Uiso 1 1 calc R . . C75 C 0.62285(18) -0.0344(3) 1.43916(18) 0.0310(9) Uani 1 1 d . . . H75 H 0.6395 0.0058 1.4733 0.037 Uiso 1 1 calc R . . C76 C 0.65314(15) -0.0626(3) 1.40911(16) 0.0230(7) Uani 1 1 d . . . H76 H 0.6903 -0.0413 1.4229 0.028 Uiso 1 1 calc R . . C80 C 0.73909(12) 0.0735(2) 1.32402(14) 0.0148(6) Uani 1 1 d . . . C81 C 0.79648(14) 0.2067(2) 1.38917(15) 0.0188(6) Uani 1 1 d . . . C82 C 0.80214(15) 0.3057(3) 1.39498(17) 0.0233(7) Uani 1 1 d . . . H82 H 0.7718 0.3448 1.3699 0.028 Uiso 1 1 calc R . . C83 C 0.85133(17) 0.3474(3) 1.43675(19) 0.0306(8) Uani 1 1 d . . . H83 H 0.8541 0.4143 1.4400 0.037 Uiso 1 1 calc R . . C84 C 0.89621(17) 0.2918(3) 1.47354(18) 0.0335(9) Uani 1 1 d . . . H84 H 0.9297 0.3202 1.5021 0.040 Uiso 1 1 calc R . . C85 C 0.89171(16) 0.1939(3) 1.46816(17) 0.0306(8) Uani 1 1 d . . . H85 H 0.9226 0.1555 1.4927 0.037 Uiso 1 1 calc R . . C86 C 0.84257(14) 0.1517(3) 1.42728(16) 0.0228(7) Uani 1 1 d . . . H86 H 0.8400 0.0847 1.4250 0.027 Uiso 1 1 calc R . . C90 C 0.74329(13) 0.1636(2) 1.34565(15) 0.0162(6) Uani 1 1 d . . . C91 C 0.69332(13) 0.2264(2) 1.32085(15) 0.0177(6) Uani 1 1 d . . . C92 C 0.66656(14) 0.2450(2) 1.25917(16) 0.0203(7) Uani 1 1 d . . . H92 H 0.6798 0.2161 1.2337 0.024 Uiso 1 1 calc R . . C93 C 0.62047(15) 0.3055(3) 1.23419(17) 0.0245(7) Uani 1 1 d . . . H93 H 0.6023 0.3168 1.1921 0.029 Uiso 1 1 calc R . . C94 C 0.60161(15) 0.3486(3) 1.27149(19) 0.0268(8) Uani 1 1 d . . . H94 H 0.5704 0.3897 1.2550 0.032 Uiso 1 1 calc R . . C95 C 0.62835(15) 0.3318(3) 1.33264(17) 0.0237(7) Uani 1 1 d . . . H95 H 0.6155 0.3621 1.3580 0.028 Uiso 1 1 calc R . . C96 C 0.67366(14) 0.2712(2) 1.35762(16) 0.0203(7) Uani 1 1 d . . . H96 H 0.6914 0.2601 1.3997 0.024 Uiso 1 1 calc R . . C131 C 0.8143(2) -0.4958(3) 1.2813(3) 0.0497(13) Uani 1 1 d . . . H13A H 0.7812 -0.5309 1.2536 0.075 Uiso 1 1 calc R . . H13B H 0.8083 -0.4709 1.3146 0.075 Uiso 1 1 calc R . . H13C H 0.8466 -0.5381 1.2972 0.075 Uiso 1 1 calc R . . C151 C 0.91155(19) -0.3584(4) 1.1660(2) 0.0434(11) Uani 1 1 d . . . H15A H 0.9394 -0.4067 1.1882 0.065 Uiso 1 1 calc R . . H15B H 0.9301 -0.2977 1.1688 0.065 Uiso 1 1 calc R . . H15C H 0.8911 -0.3771 1.1237 0.065 Uiso 1 1 calc R . . C181 C 0.70720(18) -0.3144(3) 1.08682(19) 0.0328(9) Uani 1 1 d . . . H18A H 0.7257 -0.3505 1.1243 0.049 Uiso 1 1 calc R . . H18B H 0.7332 -0.3042 1.0698 0.049 Uiso 1 1 calc R . . H18C H 0.6748 -0.3497 1.0580 0.049 Uiso 1 1 calc R . . C182 C 0.65221(17) -0.2327(3) 1.13217(18) 0.0341(9) Uani 1 1 d . . . H18D H 0.6202 -0.2726 1.1075 0.051 Uiso 1 1 calc R . . H18E H 0.6390 -0.1713 1.1387 0.051 Uiso 1 1 calc R . . H18F H 0.6743 -0.2635 1.1710 0.051 Uiso 1 1 calc R . . C183 C 0.65372(17) -0.1702(3) 1.03903(17) 0.0299(8) Uani 1 1 d . . . H18G H 0.6772 -0.1592 1.0190 0.045 Uiso 1 1 calc R . . H18H H 0.6396 -0.1096 1.0454 0.045 Uiso 1 1 calc R . . H18I H 0.6224 -0.2110 1.0138 0.045 Uiso 1 1 calc R . . C231 C 0.98996(18) -0.0997(4) 1.2082(2) 0.0416(11) Uani 1 1 d . . . H23A H 0.9904 -0.1412 1.1770 0.062 Uiso 1 1 calc R . . H23B H 1.0019 -0.1353 1.2457 0.062 Uiso 1 1 calc R . . H23C H 1.0154 -0.0466 1.2148 0.062 Uiso 1 1 calc R . . C251 C 0.80433(18) 0.0109(3) 1.04421(18) 0.0323(9) Uani 1 1 d . . . H25A H 0.8021 0.0794 1.0378 0.048 Uiso 1 1 calc R . . H25B H 0.7671 -0.0142 1.0335 0.048 Uiso 1 1 calc R . . H25C H 0.8191 -0.0188 1.0190 0.048 Uiso 1 1 calc R . . C281 C 0.80488(15) 0.2174(3) 1.23250(19) 0.0287(8) Uani 1 1 d . . . H28A H 0.8028 0.2816 1.2170 0.043 Uiso 1 1 calc R . . H28B H 0.7866 0.2154 1.2587 0.043 Uiso 1 1 calc R . . H28C H 0.7861 0.1735 1.1988 0.043 Uiso 1 1 calc R . . C282 C 0.89542(16) 0.2553(3) 1.32227(18) 0.0266(8) Uani 1 1 d . . . H28D H 0.8963 0.3193 1.3077 0.040 Uiso 1 1 calc R . . H28E H 0.9335 0.2331 1.3469 0.040 Uiso 1 1 calc R . . H28F H 0.8753 0.2560 1.3465 0.040 Uiso 1 1 calc R . . C283 C 0.89639(16) 0.1971(3) 1.22948(18) 0.0266(8) Uani 1 1 d . . . H28G H 0.8759 0.1622 1.1919 0.040 Uiso 1 1 calc R . . H28H H 0.9339 0.1707 1.2513 0.040 Uiso 1 1 calc R . . H28I H 0.8989 0.2638 1.2204 0.040 Uiso 1 1 calc R . . C331 C 1.01373(18) -0.3018(4) 1.3419(2) 0.0443(12) Uani 1 1 d . . . H33A H 1.0078 -0.3604 1.3591 0.066 Uiso 1 1 calc R . . H33B H 1.0537 -0.2885 1.3593 0.066 Uiso 1 1 calc R . . H33C H 0.9986 -0.3087 1.2983 0.066 Uiso 1 1 calc R . . C351 C 1.01955(16) 0.0218(3) 1.43166(19) 0.0334(9) Uani 1 1 d . . . H35A H 1.0576 0.0042 1.4604 0.050 Uiso 1 1 calc R . . H35B H 1.0010 0.0519 1.4531 0.050 Uiso 1 1 calc R . . H35C H 1.0207 0.0660 1.4020 0.050 Uiso 1 1 calc R . . C381 C 0.91324(16) -0.2248(3) 1.47773(18) 0.0341(9) Uani 1 1 d . . . H38A H 0.9289 -0.1666 1.4703 0.051 Uiso 1 1 calc R . . H38B H 0.9294 -0.2796 1.4674 0.051 Uiso 1 1 calc R . . H38C H 0.9219 -0.2280 1.5203 0.051 Uiso 1 1 calc R . . C382 C 0.8246(2) -0.1358(3) 1.44989(19) 0.0391(10) Uani 1 1 d . . . H38D H 0.8353 -0.1299 1.4929 0.059 Uiso 1 1 calc R . . H38E H 0.7840 -0.1392 1.4272 0.059 Uiso 1 1 calc R . . H38F H 0.8381 -0.0807 1.4366 0.059 Uiso 1 1 calc R . . C383 C 0.82768(17) -0.3119(3) 1.45786(19) 0.0335(9) Uani 1 1 d . . . H38G H 0.8374 -0.3074 1.5007 0.050 Uiso 1 1 calc R . . H38H H 0.8442 -0.3692 1.4507 0.050 Uiso 1 1 calc R . . H38I H 0.7871 -0.3147 1.4342 0.050 Uiso 1 1 calc R . . O1S O 0.4268(3) 0.5560(4) 0.8946(3) 0.108(2) Uani 1 1 d DU . . C1S C 0.3664(4) 0.5380(6) 0.8765(5) 0.122(3) Uani 1 1 d DU . . H1S1 H 0.3454 0.5276 0.8326 0.146 Uiso 1 1 calc R . . H1S2 H 0.3618 0.4820 0.8976 0.146 Uiso 1 1 calc R . . C2S C 0.3475(3) 0.6235(7) 0.8942(3) 0.092(2) Uani 1 1 d DU . . H2S1 H 0.3177 0.6091 0.9059 0.110 Uiso 1 1 calc R . . H2S2 H 0.3333 0.6704 0.8612 0.110 Uiso 1 1 calc R . . C3S C 0.3996(3) 0.6596(5) 0.9478(3) 0.0774(19) Uani 1 1 d DU . . H3S1 H 0.4030 0.7289 0.9448 0.093 Uiso 1 1 calc R . . H3S2 H 0.3978 0.6457 0.9857 0.093 Uiso 1 1 calc R . . C4S C 0.4457(3) 0.6133(8) 0.9471(4) 0.110(3) Uani 1 1 d DU . . H4S1 H 0.4645 0.5735 0.9835 0.132 Uiso 1 1 calc R . . H4S2 H 0.4728 0.6606 0.9471 0.132 Uiso 1 1 calc R . . O1T O 0.7362(2) 0.4259(5) 1.0363(3) 0.1027(19) Uani 1 1 d DU . . C1T C 0.7494(3) 0.3386(7) 1.0120(3) 0.109(3) Uani 1 1 d DU . . H1T1 H 0.7210 0.2893 1.0049 0.131 Uiso 1 1 calc R . . H1T2 H 0.7505 0.3519 0.9736 0.131 Uiso 1 1 calc R . . C2T C 0.8044(3) 0.3073(5) 1.0581(3) 0.0801(19) Uani 1 1 d DU . . H2T1 H 0.8260 0.2759 1.0399 0.096 Uiso 1 1 calc R . . H2T2 H 0.8012 0.2642 1.0877 0.096 Uiso 1 1 calc R . . C3T C 0.8299(2) 0.4009(6) 1.0862(4) 0.083(2) Uani 1 1 d DU . . H3T1 H 0.8573 0.3916 1.1288 0.100 Uiso 1 1 calc R . . H3T2 H 0.8492 0.4293 1.0646 0.100 Uiso 1 1 calc R . . C4T C 0.7858(3) 0.4624(6) 1.0825(5) 0.108(3) Uani 1 1 d DU . . H4T1 H 0.7838 0.4630 1.1211 0.129 Uiso 1 1 calc R . . H4T2 H 0.7923 0.5277 1.0729 0.129 Uiso 1 1 calc R . . O1R O 0.9482(5) -0.4768(9) 1.4954(7) 0.103(4) Uani 0.50 1 d PDU A -1 C1R C 1.0014(8) -0.4673(13) 1.5526(7) 0.089(5) Uani 0.50 1 d PDU A -1 H1R1 H 1.0178 -0.4036 1.5562 0.106 Uiso 0.50 1 calc PR A -1 H1R2 H 0.9955 -0.4799 1.5883 0.106 Uiso 0.50 1 calc PR A -1 C2R C 1.0348(11) -0.537(2) 1.5454(8) 0.081(5) Uani 0.50 1 d PDU A -1 H2R1 H 1.0279 -0.5997 1.5579 0.097 Uiso 0.50 1 calc PR A -1 H2R2 H 1.0748 -0.5210 1.5679 0.097 Uiso 0.50 1 calc PR A -1 C3R C 1.0142(7) -0.5314(18) 1.4764(7) 0.090(5) Uani 0.50 1 d PDU A -1 H3R1 H 1.0439 -0.5024 1.4688 0.108 Uiso 0.50 1 calc PR A -1 H3R2 H 1.0084 -0.5967 1.4603 0.108 Uiso 0.50 1 calc PR A -1 C4R C 0.9645(11) -0.480(3) 1.4443(9) 0.100(7) Uani 0.50 1 d PDU A -1 H4R1 H 0.9371 -0.5142 1.4086 0.120 Uiso 0.50 1 calc PR A -1 H4R2 H 0.9712 -0.4160 1.4325 0.120 Uiso 0.50 1 calc PR A -1 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 Au1 0.01229(6) 0.01728(6) 0.01974(6) -0.00076(5) 0.00780(4) 0.00126(4) Nb1 0.01097(12) 0.01234(12) 0.01611(13) -0.00124(10) 0.00627(10) -0.00012(9) P1 0.0120(3) 0.0139(4) 0.0158(4) -0.0001(3) 0.0062(3) 0.0004(3) S1 0.0167(4) 0.0221(4) 0.0272(4) -0.0020(3) 0.0109(3) 0.0022(3) O1 0.0130(10) 0.0181(11) 0.0170(11) 0.0002(9) 0.0070(8) 0.0013(8) N1 0.0151(12) 0.0159(13) 0.0202(13) -0.0016(11) 0.0083(11) -0.0013(10) C1 0.0203(17) 0.030(2) 0.042(2) -0.0046(17) 0.0142(16) -0.0047(14) O2 0.0143(10) 0.0161(11) 0.0222(11) 0.0001(9) 0.0097(9) 0.0006(8) N2 0.0135(12) 0.0164(13) 0.0194(13) -0.0022(10) 0.0080(10) -0.0016(10) C2 0.0264(19) 0.041(2) 0.048(3) -0.007(2) 0.0231(19) 0.0001(17) O3 0.0131(10) 0.0167(11) 0.0188(11) -0.0008(9) 0.0065(9) 0.0007(8) N3 0.0142(12) 0.0150(13) 0.0196(13) -0.0027(10) 0.0076(10) -0.0002(10) C3 0.035(2) 0.045(3) 0.040(2) -0.007(2) 0.0247(19) -0.0045(19) C4 0.0254(18) 0.031(2) 0.031(2) -0.0051(16) 0.0137(16) 0.0011(15) C11 0.0180(15) 0.0189(16) 0.0244(17) -0.0066(13) 0.0086(13) -0.0016(12) C12 0.0211(16) 0.0192(17) 0.0282(18) -0.0047(14) 0.0106(14) -0.0004(13) C13 0.0281(19) 0.0202(18) 0.043(2) -0.0059(17) 0.0146(17) 0.0028(14) C14 0.029(2) 0.026(2) 0.046(2) -0.0090(18) 0.0136(18) 0.0073(16) C15 0.0224(18) 0.036(2) 0.037(2) -0.0124(18) 0.0135(16) 0.0044(15) C16 0.0203(16) 0.0295(19) 0.0280(18) -0.0071(15) 0.0125(14) -0.0007(14) C17 0.0202(15) 0.0178(16) 0.0187(15) -0.0026(12) 0.0094(12) -0.0031(12) C18 0.0195(15) 0.0227(17) 0.0211(16) -0.0047(13) 0.0083(13) -0.0038(13) C21 0.0165(14) 0.0180(15) 0.0245(16) -0.0027(13) 0.0128(13) -0.0040(12) C22 0.0189(16) 0.0250(18) 0.0262(18) -0.0044(14) 0.0112(14) -0.0015(13) C23 0.0222(17) 0.032(2) 0.038(2) -0.0068(17) 0.0192(16) -0.0011(14) C24 0.033(2) 0.031(2) 0.034(2) -0.0062(17) 0.0252(17) -0.0029(16) C25 0.0272(17) 0.0207(17) 0.0231(17) -0.0035(13) 0.0146(14) -0.0048(13) C26 0.0194(15) 0.0169(16) 0.0253(17) -0.0018(13) 0.0127(13) -0.0038(12) C27 0.0161(14) 0.0193(16) 0.0221(16) -0.0024(13) 0.0096(12) -0.0038(12) C28 0.0177(15) 0.0178(16) 0.0265(17) -0.0014(13) 0.0119(13) -0.0033(12) C31 0.0142(14) 0.0215(17) 0.0218(16) 0.0010(13) 0.0086(12) 0.0018(12) C32 0.0165(15) 0.0284(19) 0.0272(18) -0.0011(15) 0.0089(13) 0.0029(13) C33 0.0207(16) 0.036(2) 0.0234(17) 0.0007(15) 0.0100(14) 0.0060(15) C34 0.0147(15) 0.043(2) 0.0258(18) 0.0025(16) 0.0078(14) 0.0010(15) C35 0.0171(15) 0.033(2) 0.0195(16) 0.0015(14) 0.0054(13) -0.0046(13) C36 0.0158(14) 0.0216(16) 0.0201(15) 0.0008(13) 0.0075(12) -0.0006(12) C37 0.0168(14) 0.0150(15) 0.0244(16) 0.0028(13) 0.0066(13) 0.0004(11) C38 0.0203(16) 0.0203(17) 0.0248(17) 0.0045(14) 0.0072(13) 0.0000(13) C40 0.0137(13) 0.0144(14) 0.0169(14) -0.0005(11) 0.0068(11) -0.0006(11) C41 0.0152(14) 0.0216(17) 0.0175(15) 0.0001(12) 0.0067(12) 0.0018(12) C42 0.0205(16) 0.0301(19) 0.0210(17) -0.0017(14) 0.0066(13) -0.0002(14) C43 0.0288(19) 0.042(2) 0.0178(17) 0.0014(16) 0.0061(14) 0.0059(17) C44 0.037(2) 0.050(3) 0.026(2) 0.0134(19) 0.0165(17) 0.0101(19) C45 0.0272(19) 0.045(3) 0.036(2) 0.0159(19) 0.0180(17) 0.0044(17) C46 0.0177(16) 0.031(2) 0.0231(17) 0.0073(15) 0.0057(13) -0.0005(13) C50 0.0134(14) 0.0177(15) 0.0184(15) -0.0002(12) 0.0068(12) -0.0010(11) C51 0.0118(13) 0.0205(16) 0.0149(14) -0.0026(12) 0.0037(11) 0.0001(11) C52 0.0153(14) 0.0207(16) 0.0219(16) -0.0017(13) 0.0062(12) -0.0012(12) C53 0.0202(16) 0.0260(18) 0.0252(18) -0.0012(14) 0.0101(14) -0.0060(13) C54 0.0142(15) 0.035(2) 0.0241(17) -0.0067(15) 0.0092(13) -0.0058(13) C55 0.0160(15) 0.0255(18) 0.0253(17) -0.0042(14) 0.0060(13) 0.0016(13) C56 0.0164(15) 0.0222(17) 0.0251(17) 0.0005(14) 0.0090(13) -0.0008(12) C60 0.0118(13) 0.0156(14) 0.0154(14) 0.0003(12) 0.0032(11) 0.0000(11) C61 0.0121(13) 0.0179(16) 0.0229(16) 0.0013(13) 0.0070(12) -0.0008(11) C62 0.0175(15) 0.0222(17) 0.0283(18) 0.0040(14) 0.0099(14) 0.0007(12) C63 0.0212(17) 0.0220(18) 0.036(2) 0.0080(15) 0.0116(15) -0.0013(13) C64 0.0223(17) 0.0142(17) 0.057(3) 0.0042(17) 0.0178(18) -0.0001(13) C65 0.0251(18) 0.0196(17) 0.048(2) -0.0088(17) 0.0186(17) -0.0034(14) C66 0.0171(15) 0.0224(17) 0.0279(18) -0.0009(14) 0.0098(13) -0.0024(12) C70 0.0143(14) 0.0172(15) 0.0160(14) -0.0002(12) 0.0066(11) -0.0012(11) C71 0.0179(15) 0.0165(15) 0.0197(15) 0.0064(12) 0.0103(12) 0.0040(12) C72 0.0181(15) 0.0252(18) 0.0251(17) 0.0050(14) 0.0110(13) 0.0018(13) C73 0.0244(18) 0.035(2) 0.036(2) 0.0096(17) 0.0184(16) 0.0060(15) C74 0.038(2) 0.041(2) 0.033(2) 0.0101(18) 0.0249(18) 0.0176(18) C75 0.042(2) 0.030(2) 0.0229(18) 0.0001(16) 0.0165(17) 0.0098(17) C76 0.0255(17) 0.0230(18) 0.0214(16) 0.0028(13) 0.0114(14) 0.0020(13) C80 0.0144(13) 0.0168(15) 0.0138(13) 0.0013(12) 0.0071(11) 0.0017(11) C81 0.0191(15) 0.0185(16) 0.0209(16) -0.0041(13) 0.0108(13) -0.0019(12) C82 0.0213(16) 0.0187(17) 0.0324(19) -0.0075(14) 0.0142(15) -0.0023(13) C83 0.0304(19) 0.025(2) 0.038(2) -0.0129(17) 0.0169(17) -0.0104(15) C84 0.0260(19) 0.041(2) 0.027(2) -0.0124(17) 0.0068(16) -0.0137(17) C85 0.0234(18) 0.039(2) 0.0214(18) -0.0007(16) 0.0030(14) -0.0025(16) C86 0.0225(16) 0.0222(17) 0.0211(16) -0.0027(14) 0.0077(13) -0.0015(13) C90 0.0150(14) 0.0168(15) 0.0178(15) 0.0003(12) 0.0084(12) 0.0004(11) C91 0.0165(14) 0.0120(14) 0.0249(16) -0.0044(12) 0.0096(13) -0.0021(11) C92 0.0204(15) 0.0177(16) 0.0248(17) -0.0001(13) 0.0121(13) 0.0002(12) C93 0.0217(16) 0.0233(18) 0.0265(18) 0.0049(14) 0.0093(14) 0.0037(13) C94 0.0181(16) 0.0206(18) 0.040(2) 0.0041(16) 0.0118(15) 0.0037(13) C95 0.0224(16) 0.0208(17) 0.0324(19) -0.0048(14) 0.0164(15) 0.0004(13) C96 0.0203(15) 0.0197(16) 0.0224(16) -0.0022(13) 0.0111(13) -0.0002(12) C131 0.053(3) 0.021(2) 0.084(4) 0.011(2) 0.038(3) 0.0118(19) C151 0.034(2) 0.051(3) 0.052(3) -0.014(2) 0.025(2) 0.009(2) C181 0.033(2) 0.024(2) 0.032(2) -0.0100(16) 0.0069(17) -0.0032(16) C182 0.0265(19) 0.050(3) 0.0260(19) -0.0084(18) 0.0125(16) -0.0162(18) C183 0.033(2) 0.029(2) 0.0228(18) -0.0039(15) 0.0081(15) -0.0018(16) C231 0.025(2) 0.055(3) 0.051(3) -0.007(2) 0.022(2) 0.0073(19) C251 0.039(2) 0.037(2) 0.0242(19) -0.0023(17) 0.0171(17) -0.0018(17) C281 0.0218(17) 0.0215(18) 0.042(2) 0.0012(16) 0.0133(16) -0.0005(14) C282 0.0274(18) 0.0201(18) 0.035(2) -0.0068(15) 0.0167(16) -0.0078(14) C283 0.0299(19) 0.0237(18) 0.032(2) -0.0008(15) 0.0191(16) -0.0077(14) C331 0.028(2) 0.062(3) 0.044(3) -0.008(2) 0.0169(19) 0.015(2) C351 0.0219(18) 0.040(2) 0.034(2) -0.0023(18) 0.0082(16) -0.0123(16) C381 0.0259(19) 0.041(2) 0.0253(19) 0.0080(17) 0.0027(15) -0.0068(17) C382 0.060(3) 0.034(2) 0.026(2) 0.0044(17) 0.022(2) 0.013(2) C383 0.0264(19) 0.037(2) 0.031(2) 0.0112(17) 0.0074(16) -0.0073(16) O1S 0.121(5) 0.092(4) 0.095(4) 0.000(3) 0.035(4) 0.034(4) C1S 0.180(8) 0.070(5) 0.146(8) -0.024(5) 0.101(7) -0.051(6) C2S 0.077(4) 0.148(7) 0.069(4) 0.003(5) 0.049(4) -0.007(5) C3S 0.077(4) 0.072(5) 0.086(5) 0.001(4) 0.040(4) 0.011(4) C4S 0.091(5) 0.138(8) 0.099(6) -0.022(5) 0.041(5) 0.039(5) O1T 0.061(3) 0.151(6) 0.076(4) -0.006(3) 0.013(3) 0.000(3) C1T 0.065(4) 0.238(9) 0.039(3) -0.071(5) 0.035(3) -0.064(5) C2T 0.097(5) 0.089(5) 0.078(5) -0.018(4) 0.060(4) -0.017(4) C3T 0.040(3) 0.105(6) 0.091(5) -0.039(4) 0.018(3) 0.013(3) C4T 0.047(4) 0.102(6) 0.142(8) -0.032(6) 0.016(4) 0.004(4) O1R 0.091(7) 0.078(7) 0.156(11) -0.002(8) 0.070(7) 0.000(6) C1R 0.095(12) 0.043(8) 0.130(10) 0.019(10) 0.053(9) 0.016(8) C2R 0.078(10) 0.078(12) 0.109(8) -0.022(10) 0.061(8) -0.007(8) C3R 0.047(8) 0.108(13) 0.099(9) 0.036(10) 0.019(8) -0.005(8) C4R 0.057(10) 0.100(18) 0.136(9) -0.015(13) 0.036(8) 0.005(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 Au1 P1 2.2855(8) . ? Au1 S1 2.3302(9) . ? Nb1 N3 2.028(3) . ? Nb1 N2 2.029(3) . ? Nb1 N1 2.032(3) . ? Nb1 O2 2.096(2) . ? Nb1 O1 2.108(2) . ? Nb1 O3 2.109(2) . ? P1 C60 1.847(3) . ? P1 C40 1.856(3) . ? P1 C80 1.860(3) . ? S1 C1 1.831(4) . ? S1 C4 1.838(4) . ? O1 C40 1.318(4) . ? N1 C11 1.447(4) . ? N1 C17 1.488(4) . ? C1 C2 1.524(6) . ? O2 C60 1.328(4) . ? N2 C21 1.449(4) . ? N2 C27 1.478(4) . ? C2 C3 1.516(6) . ? O3 C80 1.324(4) . ? N3 C31 1.441(4) . ? N3 C37 1.490(4) . ? C3 C4 1.524(6) . ? C11 C12 1.393(5) . ? C11 C16 1.395(5) . ? C12 C13 1.400(5) . ? C13 C14 1.396(6) . ? C13 C131 1.514(6) . ? C14 C15 1.384(7) . ? C15 C16 1.400(5) . ? C15 C151 1.523(6) . ? C17 C18 1.547(5) . ? C18 C182 1.530(5) . ? C18 C183 1.534(5) . ? C18 C181 1.539(5) . ? C21 C26 1.387(5) . ? C21 C22 1.398(5) . ? C22 C23 1.395(5) . ? C23 C24 1.393(6) . ? C23 C231 1.520(5) . ? C24 C25 1.391(5) . ? C25 C26 1.404(5) . ? C25 C251 1.509(5) . ? C27 C28 1.561(5) . ? C28 C281 1.529(5) . ? C28 C283 1.536(5) . ? C28 C282 1.537(5) . ? C31 C36 1.393(5) . ? C31 C32 1.400(5) . ? C32 C33 1.400(5) . ? C33 C34 1.392(6) . ? C33 C331 1.519(6) . ? C34 C35 1.395(6) . ? C35 C36 1.392(5) . ? C35 C351 1.514(5) . ? C37 C38 1.554(5) . ? C38 C382 1.518(6) . ? C38 C381 1.532(5) . ? C38 C383 1.533(5) . ? C40 C50 1.372(4) . ? C41 C46 1.400(5) . ? C41 C42 1.408(5) . ? C41 C50 1.482(5) . ? C42 C43 1.386(5) . ? C43 C44 1.379(6) . ? C44 C45 1.389(6) . ? C45 C46 1.387(5) . ? C50 C51 1.483(4) . ? C51 C52 1.400(5) . ? C51 C56 1.404(5) . ? C52 C53 1.390(5) . ? C53 C54 1.386(5) . ? C54 C55 1.394(5) . ? C55 C56 1.393(5) . ? C60 C70 1.363(4) . ? C61 C66 1.400(5) . ? C61 C62 1.409(5) . ? C61 C70 1.487(5) . ? C62 C63 1.395(5) . ? C63 C64 1.383(6) . ? C64 C65 1.390(6) . ? C65 C66 1.387(5) . ? C70 C71 1.499(4) . ? C71 C76 1.394(5) . ? C71 C72 1.406(5) . ? C72 C73 1.392(5) . ? C73 C74 1.388(6) . ? C74 C75 1.384(6) . ? C75 C76 1.394(5) . ? C80 C90 1.369(5) . ? C81 C82 1.408(5) . ? C81 C86 1.408(5) . ? C81 C90 1.482(5) . ? C82 C83 1.393(5) . ? C83 C84 1.386(6) . ? C84 C85 1.391(6) . ? C85 C86 1.388(5) . ? C90 C91 1.494(4) . ? C91 C92 1.397(5) . ? C91 C96 1.402(5) . ? C92 C93 1.401(5) . ? C93 C94 1.388(5) . ? C94 C95 1.381(6) . ? C95 C96 1.388(5) . ? O1S C4S 1.424(9) . ? O1S C1S 1.503(10) . ? C1S C2S 1.458(10) . ? C2S C3S 1.524(9) . ? C3S C4S 1.412(9) . ? O1T C4T 1.409(8) . ? O1T C1T 1.488(9) . ? C1T C2T 1.476(9) . ? C2T C3T 1.510(9) . ? C3T C4T 1.440(8) . ? O1R C1R 1.502(13) . ? O1R C4R 1.527(14) . ? C1R C2R 1.397(14) . ? C2R C3R 1.552(16) . ? C3R C4R 1.415(13) . ? 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 P1 Au1 S1 170.57(3) . . ? N3 Nb1 N2 98.09(11) . . ? N3 Nb1 N1 97.76(11) . . ? N2 Nb1 N1 96.19(11) . . ? N3 Nb1 O2 87.71(10) . . ? N2 Nb1 O2 168.63(10) . . ? N1 Nb1 O2 92.69(10) . . ? N3 Nb1 O1 167.52(10) . . ? N2 Nb1 O1 92.15(10) . . ? N1 Nb1 O1 88.17(10) . . ? O2 Nb1 O1 81.01(9) . . ? N3 Nb1 O3 92.11(10) . . ? N2 Nb1 O3 89.28(10) . . ? N1 Nb1 O3 167.91(10) . . ? O2 Nb1 O3 80.69(9) . . ? O1 Nb1 O3 80.84(9) . . ? C60 P1 C40 99.99(15) . . ? C60 P1 C80 101.91(14) . . ? C40 P1 C80 97.90(14) . . ? C60 P1 Au1 118.75(11) . . ? C40 P1 Au1 118.19(10) . . ? C80 P1 Au1 116.56(10) . . ? C1 S1 C4 92.93(19) . . ? C1 S1 Au1 115.29(14) . . ? C4 S1 Au1 110.10(13) . . ? C40 O1 Nb1 131.8(2) . . ? C11 N1 C17 111.4(3) . . ? C11 N1 Nb1 121.8(2) . . ? C17 N1 Nb1 126.5(2) . . ? C2 C1 S1 102.2(3) . . ? C60 O2 Nb1 131.9(2) . . ? C21 N2 C27 111.0(3) . . ? C21 N2 Nb1 121.3(2) . . ? C27 N2 Nb1 127.2(2) . . ? C3 C2 C1 106.8(3) . . ? C80 O3 Nb1 127.7(2) . . ? C31 N3 C37 111.2(3) . . ? C31 N3 Nb1 120.9(2) . . ? C37 N3 Nb1 127.6(2) . . ? C2 C3 C4 108.6(3) . . ? C3 C4 S1 107.5(3) . . ? C12 C11 C16 119.5(3) . . ? C12 C11 N1 119.8(3) . . ? C16 C11 N1 120.7(3) . . ? C11 C12 C13 120.9(4) . . ? C14 C13 C12 118.3(4) . . ? C14 C13 C131 121.8(4) . . ? C12 C13 C131 119.9(4) . . ? C15 C14 C13 121.9(4) . . ? C14 C15 C16 119.0(4) . . ? C14 C15 C151 121.3(4) . . ? C16 C15 C151 119.7(4) . . ? C11 C16 C15 120.4(4) . . ? N1 C17 C18 119.1(3) . . ? C182 C18 C183 109.6(3) . . ? C182 C18 C181 110.2(3) . . ? C183 C18 C181 107.1(3) . . ? C182 C18 C17 110.3(3) . . ? C183 C18 C17 105.5(3) . . ? C181 C18 C17 114.0(3) . . ? C26 C21 C22 119.7(3) . . ? C26 C21 N2 120.2(3) . . ? C22 C21 N2 120.0(3) . . ? C23 C22 C21 120.2(4) . . ? C24 C23 C22 119.2(3) . . ? C24 C23 C231 121.3(4) . . ? C22 C23 C231 119.5(4) . . ? C25 C24 C23 121.6(3) . . ? C24 C25 C26 118.3(3) . . ? C24 C25 C251 121.5(3) . . ? C26 C25 C251 120.2(3) . . ? C21 C26 C25 121.0(3) . . ? N2 C27 C28 120.2(3) . . ? C281 C28 C283 110.5(3) . . ? C281 C28 C282 110.0(3) . . ? C283 C28 C282 106.8(3) . . ? C281 C28 C27 110.7(3) . . ? C283 C28 C27 113.5(3) . . ? C282 C28 C27 105.0(3) . . ? C36 C31 C32 119.5(3) . . ? C36 C31 N3 120.4(3) . . ? C32 C31 N3 120.1(3) . . ? C33 C32 C31 120.2(4) . . ? C34 C33 C32 119.0(4) . . ? C34 C33 C331 121.0(4) . . ? C32 C33 C331 120.0(4) . . ? C33 C34 C35 121.5(3) . . ? C36 C35 C34 118.7(3) . . ? C36 C35 C351 120.2(4) . . ? C34 C35 C351 121.1(3) . . ? C35 C36 C31 121.1(3) . . ? N3 C37 C38 118.6(3) . . ? C382 C38 C381 110.4(4) . . ? C382 C38 C383 109.9(4) . . ? C381 C38 C383 106.7(3) . . ? C382 C38 C37 110.2(3) . . ? C381 C38 C37 114.0(3) . . ? C383 C38 C37 105.4(3) . . ? O1 C40 C50 125.2(3) . . ? O1 C40 P1 111.3(2) . . ? C50 C40 P1 122.8(2) . . ? C46 C41 C42 117.4(3) . . ? C46 C41 C50 121.7(3) . . ? C42 C41 C50 120.9(3) . . ? C43 C42 C41 121.4(4) . . ? C44 C43 C42 120.1(4) . . ? C43 C44 C45 119.6(4) . . ? C46 C45 C44 120.6(4) . . ? C45 C46 C41 120.9(3) . . ? C40 C50 C41 121.7(3) . . ? C40 C50 C51 120.3(3) . . ? C41 C50 C51 118.0(3) . . ? C52 C51 C56 117.9(3) . . ? C52 C51 C50 120.5(3) . . ? C56 C51 C50 121.6(3) . . ? C53 C52 C51 121.2(3) . . ? C54 C53 C52 120.2(3) . . ? C53 C54 C55 119.6(3) . . ? C56 C55 C54 120.1(3) . . ? C55 C56 C51 120.9(3) . . ? O2 C60 C70 124.3(3) . . ? O2 C60 P1 112.5(2) . . ? C70 C60 P1 122.9(2) . . ? C66 C61 C62 117.6(3) . . ? C66 C61 C70 122.7(3) . . ? C62 C61 C70 119.7(3) . . ? C63 C62 C61 120.7(4) . . ? C64 C63 C62 120.6(4) . . ? C63 C64 C65 119.2(4) . . ? C66 C65 C64 120.5(4) . . ? C65 C66 C61 121.2(4) . . ? C60 C70 C61 122.1(3) . . ? C60 C70 C71 123.1(3) . . ? C61 C70 C71 114.6(3) . . ? C76 C71 C72 118.3(3) . . ? C76 C71 C70 121.4(3) . . ? C72 C71 C70 119.7(3) . . ? C73 C72 C71 120.6(4) . . ? C74 C73 C72 120.2(4) . . ? C75 C74 C73 119.8(4) . . ? C74 C75 C76 120.2(4) . . ? C71 C76 C75 120.9(4) . . ? O3 C80 C90 125.5(3) . . ? O3 C80 P1 113.1(2) . . ? C90 C80 P1 121.4(2) . . ? C82 C81 C86 117.3(3) . . ? C82 C81 C90 120.5(3) . . ? C86 C81 C90 122.1(3) . . ? C83 C82 C81 121.3(4) . . ? C84 C83 C82 120.3(4) . . ? C83 C84 C85 119.3(4) . . ? C86 C85 C84 120.7(4) . . ? C85 C86 C81 121.0(4) . . ? C80 C90 C81 123.5(3) . . ? C80 C90 C91 119.5(3) . . ? C81 C90 C91 116.8(3) . . ? C92 C91 C96 118.4(3) . . ? C92 C91 C90 119.1(3) . . ? C96 C91 C90 122.4(3) . . ? C91 C92 C93 121.1(3) . . ? C94 C93 C92 119.4(3) . . ? C95 C94 C93 119.9(3) . . ? C94 C95 C96 121.0(3) . . ? C95 C96 C91 120.2(3) . . ? C4S O1S C1S 105.1(7) . . ? C2S C1S O1S 104.4(6) . . ? C1S C2S C3S 103.5(7) . . ? C4S C3S C2S 107.6(6) . . ? C3S C4S O1S 109.0(7) . . ? C4T O1T C1T 108.9(5) . . ? C2T C1T O1T 105.8(5) . . ? C1T C2T C3T 100.6(6) . . ? C4T C3T C2T 108.2(6) . . ? O1T C4T C3T 106.3(6) . . ? C1R O1R C4R 106.4(13) . . ? C2R C1R O1R 102.1(14) . . ? C1R C2R C3R 100.5(12) . . ? C4R C3R C2R 115.1(11) . . ? C3R C4R O1R 95.6(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.068 _refine_diff_density_min -1.347 _refine_diff_density_rms 0.120 data_09451 _database_code_depnum_ccdc_archive 'CCDC 789235' #TrackingRef '2140_web_deposit_cif_file_0_SidCreutz_1281724091.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (py)AuP(C[CPh2]O)3Nb(N[Np]Ar)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H115 Au N4 Nb O5.50 P' _chemical_formula_weight 1733.77 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/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 27.017(2) _cell_length_b 14.1228(13) _cell_length_c 24.657(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.1100(10) _cell_angle_gamma 90.00 _cell_volume 8448.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 1.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6971 _exptl_absorpt_correction_T_max 0.7591 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 159360 _diffrn_reflns_av_R_equivalents 0.1102 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 27.10 _reflns_number_total 18630 _reflns_number_gt 13842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18630 _refine_ls_number_parameters 993 _refine_ls_number_restraints 1251 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.500 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.605424(8) 0.929878(15) 3.806643(10) 0.01884(8) Uani 1 1 d U . . Nb1 Nb 0.788107(18) 1.08174(3) 3.77352(2) 0.01380(11) Uani 1 1 d U . . P1 P 0.67297(5) 0.98991(10) 3.78738(6) 0.0154(3) Uani 1 1 d U . . O3 O 0.78300(13) 0.9836(2) 3.83449(16) 0.0155(8) Uani 1 1 d U . . O2 O 0.71878(13) 1.0051(3) 3.71313(16) 0.0167(8) Uani 1 1 d U . . N5 N 0.77678(17) 1.1708(3) 3.7044(2) 0.0172(9) Uani 1 1 d U . . O1 O 0.72710(13) 1.1481(2) 3.79083(16) 0.0162(8) Uani 1 1 d U . . N1 N 0.84137(17) 0.9941(3) 3.7606(2) 0.0163(9) Uani 1 1 d U . . N4 N 0.54908(18) 0.8698(3) 3.8337(2) 0.0250(11) Uani 1 1 d U . . C70 C 0.7405(2) 0.9284(4) 3.8267(2) 0.0147(10) Uani 1 1 d U . . C16 C 0.9127(2) 1.0477(4) 3.7308(3) 0.0210(12) Uani 1 1 d U . . H16 H 0.9365 1.0611 3.7719 0.025 Uiso 1 1 calc R . . N3 N 0.84427(16) 1.1616(3) 3.8410(2) 0.0154(9) Uani 1 1 d U . . C11 C 0.8594(2) 1.0129(4) 3.7147(2) 0.0168(11) Uani 1 1 d U . . C711 C 0.7965(2) 0.7929(4) 3.8908(3) 0.0198(12) Uani 1 1 d U . . C81 C 0.6227(2) 0.9682(4) 3.6604(2) 0.0175(11) Uani 1 1 d U . . C56 C 0.8454(2) 1.2676(4) 3.6883(3) 0.0250(13) Uani 1 1 d U . . H56 H 0.8512 1.2165 3.6667 0.030 Uiso 1 1 calc R . . C21 C 0.8719(2) 0.9126(4) 3.7990(3) 0.0188(12) Uani 1 1 d U . . H21A H 0.8600 0.9065 3.8315 0.023 Uiso 1 1 calc R . . H21B H 0.9114 0.9299 3.8186 0.023 Uiso 1 1 calc R . . C15 C 0.9307(2) 1.0627(4) 3.6864(3) 0.0257(13) Uani 1 1 d U . . C821 C 0.6245(2) 0.9429(4) 3.6025(3) 0.0208(12) Uani 1 1 d U . . C410 C 0.8505(2) 1.2253(4) 3.9434(3) 0.0214(12) Uani 1 1 d U . . C80 C 0.6694(2) 0.9920(4) 3.7109(2) 0.0158(11) Uani 1 1 d U . . C210 C 0.8673(2) 0.8124(4) 3.7704(3) 0.0202(12) Uani 1 1 d U . . C812 C 0.5505(2) 1.0505(4) 3.6804(3) 0.0238(13) Uani 1 1 d U . . H812 H 0.5745 1.1034 3.6949 0.029 Uiso 1 1 calc R . . C61 C 0.7414(2) 1.1528(4) 3.6393(2) 0.0197(12) Uani 1 1 d U . . H61A H 0.7243 1.0896 3.6358 0.024 Uiso 1 1 calc R . . H61B H 0.7657 1.1490 3.6188 0.024 Uiso 1 1 calc R . . C213 C 0.8979(2) 0.8044(4) 3.7307(3) 0.0248(13) Uani 1 1 d U . . H21X H 0.8809 0.8470 3.6959 0.037 Uiso 1 1 calc R . . H21Y H 0.8957 0.7390 3.7164 0.037 Uiso 1 1 calc R . . H21Z H 0.9367 0.8219 3.7544 0.037 Uiso 1 1 calc R . . C51 C 0.8081(2) 1.2568(4) 3.7128(3) 0.0196(12) Uani 1 1 d U . . C721 C 0.6938(2) 0.7769(4) 3.8229(3) 0.0180(11) Uani 1 1 d U . . C52 C 0.8008(2) 1.3321(4) 3.7452(3) 0.0215(12) Uani 1 1 d U . . H52 H 0.7756 1.3252 3.7622 0.026 Uiso 1 1 calc R . . C211 C 0.8067(2) 0.7838(4) 3.7349(3) 0.0268(13) Uani 1 1 d U . . H21D H 0.7884 0.8273 3.7009 0.040 Uiso 1 1 calc R . . H21E H 0.7884 0.7866 3.7615 0.040 Uiso 1 1 calc R . . H21F H 0.8045 0.7191 3.7196 0.040 Uiso 1 1 calc R . . C813 C 0.4992(2) 1.0545(4) 3.6800(3) 0.0269(14) Uani 1 1 d U . . H813 H 0.4886 1.1093 3.6947 0.032 Uiso 1 1 calc R . . C811 C 0.5677(2) 0.9702(4) 3.6601(2) 0.0190(12) Uani 1 1 d U . . C712 C 0.8423(2) 0.8471(4) 3.9290(3) 0.0224(12) Uani 1 1 d U . . H712 H 0.8402 0.9143 3.9272 0.027 Uiso 1 1 calc R . . C71 C 0.7437(2) 0.8385(4) 3.8478(2) 0.0175(11) Uani 1 1 d U . . C13 C 0.8425(2) 1.0092(4) 3.6096(3) 0.0222(12) Uani 1 1 d U . . C610 C 0.6948(2) 1.2235(4) 3.6037(3) 0.0245(13) Uani 1 1 d U . . C12 C 0.8252(2) 0.9946(4) 3.6547(3) 0.0182(11) Uani 1 1 d U . . H12 H 0.7891 0.9714 3.6438 0.022 Uiso 1 1 calc R . . C41 C 0.8328(2) 1.2396(4) 3.8754(2) 0.0196(12) Uani 1 1 d U . . H41A H 0.7927 1.2518 3.8557 0.024 Uiso 1 1 calc R . . H41B H 0.8511 1.2977 3.8707 0.024 Uiso 1 1 calc R . . C36 C 0.9325(2) 1.0762(4) 3.8867(3) 0.0204(12) Uani 1 1 d U . . H36 H 0.9150 1.0271 3.8980 0.024 Uiso 1 1 calc R . . C916 C 0.6529(2) 1.0761(4) 3.9160(3) 0.0246(13) Uani 1 1 d U . . H916 H 0.6907 1.0582 3.9330 0.030 Uiso 1 1 calc R . . C921 C 0.6755(2) 1.2724(4) 3.8451(3) 0.0190(12) Uani 1 1 d U . . C31 C 0.9023(2) 1.1553(4) 3.8564(2) 0.0186(12) Uani 1 1 d U . . C823 C 0.5799(3) 0.9361(5) 3.4925(3) 0.0361(16) Uani 1 1 d U . . H823 H 0.5488 0.9483 3.4552 0.043 Uiso 1 1 calc R . . C35 C 0.9883(2) 1.0680(4) 3.9006(3) 0.0230(12) Uani 1 1 d U . . C91 C 0.6664(2) 1.1689(4) 3.8360(2) 0.0180(11) Uani 1 1 d U . . C911 C 0.6305(2) 1.1287(4) 3.8629(3) 0.0205(12) Uani 1 1 d U . . C725 C 0.6268(2) 0.6750(4) 3.8338(3) 0.0267(13) Uani 1 1 d U . . H725 H 0.6131 0.6451 3.8590 0.032 Uiso 1 1 calc R . . C713 C 0.8905(2) 0.8033(5) 3.9692(3) 0.0290(14) Uani 1 1 d U . . H713 H 0.9213 0.8409 3.9942 0.035 Uiso 1 1 calc R . . C212 C 0.8962(2) 0.7456(4) 3.8240(3) 0.0246(13) Uani 1 1 d U . . H21G H 0.9349 0.7647 3.8467 0.037 Uiso 1 1 calc R . . H21H H 0.8945 0.6807 3.8093 0.037 Uiso 1 1 calc R . . H21I H 0.8779 0.7487 3.8505 0.037 Uiso 1 1 calc R . . C723 C 0.6199(2) 0.7038(4) 3.7354(3) 0.0242(13) Uani 1 1 d U . . H723 H 0.6017 0.6942 3.6930 0.029 Uiso 1 1 calc R . . C922 C 0.6728(2) 1.3173(4) 3.8946(3) 0.0245(13) Uani 1 1 d U . . H922 H 0.6634 1.2811 3.9212 0.029 Uiso 1 1 calc R . . C53 C 0.8292(2) 1.4164(4) 3.7532(3) 0.0285(14) Uani 1 1 d U . . C926 C 0.6871(2) 1.3300(4) 3.8053(3) 0.0243(13) Uani 1 1 d U . . H926 H 0.6880 1.3027 3.7706 0.029 Uiso 1 1 calc R . . C90 C 0.6912(2) 1.1149(4) 3.8095(2) 0.0165(11) Uani 1 1 d U . . C923 C 0.6834(2) 1.4122(4) 3.9056(3) 0.0308(15) Uani 1 1 d U . . H923 H 0.6822 1.4402 3.9400 0.037 Uiso 1 1 calc R . . C726 C 0.6736(2) 0.7319(4) 3.8598(3) 0.0218(12) Uani 1 1 d U . . H726 H 0.6918 0.7401 3.9024 0.026 Uiso 1 1 calc R . . C14 C 0.8957(2) 1.0434(4) 3.6267(3) 0.0252(13) Uani 1 1 d U . . H14 H 0.9082 1.0537 3.5967 0.030 Uiso 1 1 calc R . . C816 C 0.5304(2) 0.8947(4) 3.6379(3) 0.0231(13) Uani 1 1 d U . . H816 H 0.5407 0.8397 3.6231 0.028 Uiso 1 1 calc R . . C716 C 0.8014(2) 0.6941(4) 3.8953(3) 0.0240(13) Uani 1 1 d U . . H716 H 0.7712 0.6560 3.8696 0.029 Uiso 1 1 calc R . . C54 C 0.8657(3) 1.4251(4) 3.7277(3) 0.0337(15) Uani 1 1 d U . . H54 H 0.8854 1.4827 3.7327 0.040 Uiso 1 1 calc R . . C822 C 0.5790(2) 0.9611(5) 3.5470(3) 0.0285(14) Uani 1 1 d U . . H822 H 0.5472 0.9908 3.5464 0.034 Uiso 1 1 calc R . . C32 C 0.9287(2) 1.2296(4) 3.8426(3) 0.0223(12) Uani 1 1 d U . . H32 H 0.9085 1.2846 3.8230 0.027 Uiso 1 1 calc R . . C551 C 0.9139(3) 1.3623(5) 3.6670(3) 0.0445(19) Uani 1 1 d U . . H55A H 0.9297 1.4261 3.6748 0.067 Uiso 1 1 calc R . . H55B H 0.8942 1.3518 3.6233 0.067 Uiso 1 1 calc R . . H55C H 0.9435 1.3155 3.6848 0.067 Uiso 1 1 calc R . . C815 C 0.4791(2) 0.8989(4) 3.6369(3) 0.0287(14) Uani 1 1 d U . . H815 H 0.4545 0.8468 3.6219 0.034 Uiso 1 1 calc R . . C33 C 0.9849(2) 1.2233(5) 3.8576(3) 0.0267(13) Uani 1 1 d U . . C34 C 1.0136(2) 1.1424(5) 3.8850(3) 0.0263(13) Uani 1 1 d U . . H34 H 1.0514 1.1372 3.8935 0.032 Uiso 1 1 calc R . . C722 C 0.6666(2) 0.7605(4) 3.7604(3) 0.0207(12) Uani 1 1 d U . . H722 H 0.6803 0.7888 3.7348 0.025 Uiso 1 1 calc R . . C55 C 0.8741(2) 1.3519(5) 3.6949(3) 0.0308(15) Uani 1 1 d U . . C714 C 0.8943(2) 0.7052(5) 3.9735(3) 0.0304(14) Uani 1 1 d U . . H714 H 0.9273 0.6757 4.0016 0.036 Uiso 1 1 calc R . . C611 C 0.7152(3) 1.3181(4) 3.5896(3) 0.0318(15) Uani 1 1 d U . . H61X H 0.6835 1.3593 3.5670 0.048 Uiso 1 1 calc R . . H61Y H 0.7351 1.3059 3.5653 0.048 Uiso 1 1 calc R . . H61Z H 0.7399 1.3491 3.6274 0.048 Uiso 1 1 calc R . . C724 C 0.5999(2) 0.6612(4) 3.7720(3) 0.0272(14) Uani 1 1 d U . . H724 H 0.5678 0.6228 3.7549 0.033 Uiso 1 1 calc R . . C531 C 0.8209(3) 1.4975(4) 3.7893(3) 0.0405(17) Uani 1 1 d U . . H53A H 0.8443 1.5511 3.7901 0.061 Uiso 1 1 calc R . . H53B H 0.8311 1.4763 3.8307 0.061 Uiso 1 1 calc R . . H53C H 0.7822 1.5172 3.7704 0.061 Uiso 1 1 calc R . . C814 C 0.4631(2) 0.9793(5) 3.6581(3) 0.0278(14) Uani 1 1 d U . . H814 H 0.4278 0.9822 3.6575 0.033 Uiso 1 1 calc R . . C413 C 0.9131(2) 1.2245(5) 3.9825(3) 0.0317(15) Uani 1 1 d U . . H41X H 0.9292 1.1697 3.9717 0.048 Uiso 1 1 calc R . . H41Y H 0.9210 1.2204 4.0252 0.048 Uiso 1 1 calc R . . H41Z H 0.9291 1.2828 3.9756 0.048 Uiso 1 1 calc R . . C912 C 0.5746(2) 1.1545(4) 3.8392(3) 0.0268(14) Uani 1 1 d U . . H912 H 0.5585 1.1913 3.8033 0.032 Uiso 1 1 calc R . . C826 C 0.6705(2) 0.8987(4) 3.6017(3) 0.0258(13) Uani 1 1 d U . . H826 H 0.7017 0.8849 3.6387 0.031 Uiso 1 1 calc R . . C131 C 0.8044(3) 0.9880(5) 3.5447(3) 0.0323(15) Uani 1 1 d U . . H13A H 0.7691 0.9650 3.5418 0.048 Uiso 1 1 calc R . . H13B H 0.8210 0.9395 3.5295 0.048 Uiso 1 1 calc R . . H13C H 0.7983 1.0458 3.5206 0.048 Uiso 1 1 calc R . . C925 C 0.6970(2) 1.4257(4) 3.8163(3) 0.0314(15) Uani 1 1 d U . . H925 H 0.7047 1.4634 3.7890 0.038 Uiso 1 1 calc R . . C914 C 0.5657(3) 1.0736(5) 3.9206(3) 0.0378(16) Uani 1 1 d U . . H914 H 0.5437 1.0542 3.9399 0.045 Uiso 1 1 calc R . . C351 C 1.0197(2) 0.9803(5) 3.9314(3) 0.0338(15) Uani 1 1 d U . . H35A H 1.0582 0.9866 3.9383 0.051 Uiso 1 1 calc R . . H35B H 1.0031 0.9251 3.9057 0.051 Uiso 1 1 calc R . . H35C H 1.0183 0.9722 3.9701 0.051 Uiso 1 1 calc R . . C715 C 0.8492(2) 0.6510(4) 3.9363(3) 0.0291(14) Uani 1 1 d U . . H715 H 0.8513 0.5839 3.9390 0.035 Uiso 1 1 calc R . . C1 C 0.5680(3) 0.8358(5) 3.8900(3) 0.0356(16) Uani 1 1 d U . . H1 H 0.6064 0.8395 3.9158 0.043 Uiso 1 1 calc R . . C825 C 0.6710(3) 0.8748(5) 3.5476(3) 0.0325(15) Uani 1 1 d U . . H825 H 0.7026 0.8450 3.5477 0.039 Uiso 1 1 calc R . . C412 C 0.8280(2) 1.3108(5) 3.9636(3) 0.0326(15) Uani 1 1 d U . . H41D H 0.7879 1.3140 3.9397 0.049 Uiso 1 1 calc R . . H41E H 0.8449 1.3688 3.9575 0.049 Uiso 1 1 calc R . . H41F H 0.8369 1.3043 4.0065 0.049 Uiso 1 1 calc R . . C5 C 0.4957(2) 0.8640(5) 3.7977(3) 0.0363(16) Uani 1 1 d U . . H5 H 0.4817 0.8885 3.7579 0.044 Uiso 1 1 calc R . . C913 C 0.5426(2) 1.1264(5) 3.8680(3) 0.0352(16) Uani 1 1 d U . . H913 H 0.5047 1.1435 3.8513 0.042 Uiso 1 1 calc R . . C151 C 0.9889(2) 1.0998(5) 3.7048(3) 0.0370(16) Uani 1 1 d U . . H15A H 0.9955 1.1055 3.6690 0.056 Uiso 1 1 calc R . . H15B H 1.0157 1.0556 3.7335 0.056 Uiso 1 1 calc R . . H15C H 0.9929 1.1620 3.7239 0.056 Uiso 1 1 calc R . . C411 C 0.8254(3) 1.1339(5) 3.9539(3) 0.0416(18) Uani 1 1 d U . . H41G H 0.7855 1.1345 3.9290 0.062 Uiso 1 1 calc R . . H41H H 0.8333 1.1294 3.9966 0.062 Uiso 1 1 calc R . . H41I H 0.8415 1.0793 3.9430 0.062 Uiso 1 1 calc R . . C613 C 0.6594(3) 1.1758(5) 3.5435(3) 0.0420(18) Uani 1 1 d U . . H61D H 0.6457 1.1152 3.5508 0.063 Uiso 1 1 calc R . . H61E H 0.6815 1.1648 3.5216 0.063 Uiso 1 1 calc R . . H61F H 0.6281 1.2168 3.5194 0.063 Uiso 1 1 calc R . . C331 C 1.0132(3) 1.3053(5) 3.8428(3) 0.0382(17) Uani 1 1 d U . . H33A H 1.0524 1.2905 3.8568 0.057 Uiso 1 1 calc R . . H33B H 1.0095 1.3627 3.8630 0.057 Uiso 1 1 calc R . . H33C H 0.9961 1.3155 3.7990 0.057 Uiso 1 1 calc R . . C824 C 0.6257(3) 0.8940(5) 3.4932(3) 0.0388(16) Uani 1 1 d U . . H824 H 0.6265 0.8778 3.4562 0.047 Uiso 1 1 calc R . . C612 C 0.6602(3) 1.2416(5) 3.6381(3) 0.0389(17) Uani 1 1 d U . . H61G H 0.6475 1.1810 3.6468 0.058 Uiso 1 1 calc R . . H61H H 0.6282 1.2808 3.6134 0.058 Uiso 1 1 calc R . . H61I H 0.6827 1.2744 3.6761 0.058 Uiso 1 1 calc R . . C2 C 0.5340(3) 0.7957(5) 3.9119(4) 0.0409(17) Uani 1 1 d U . . H2 H 0.5486 0.7755 3.9527 0.049 Uiso 1 1 calc R . . C915 C 0.6205(3) 1.0492(5) 3.9447(3) 0.0321(15) Uani 1 1 d U . . H915 H 0.6365 1.0138 3.9812 0.039 Uiso 1 1 calc R . . C924 C 0.6960(2) 1.4676(5) 3.8669(3) 0.0370(16) Uani 1 1 d U . . H924 H 0.7037 1.5331 3.8748 0.044 Uiso 1 1 calc R . . C4 C 0.4591(3) 0.8219(6) 3.8175(4) 0.048(2) Uani 1 1 d U . . H4 H 0.4207 0.8188 3.7917 0.058 Uiso 1 1 calc R . . C3 C 0.48067(12) 0.7854(2) 3.87567(14) 0.0473(19) Uani 1 1 d U . . H3 H 0.4575 0.7533 3.8895 0.057 Uiso 1 1 calc R . . O1SC O 0.75199(12) 0.7011(2) 3.52310(14) 0.078(3) Uani 0.669(10) 1 d PRDU A 1 C4SC C 0.80536(12) 0.7072(2) 3.56310(14) 0.039(3) Uani 0.669(10) 1 d PRDU A 1 H4S1 H 0.8096 0.7550 3.5942 0.046 Uiso 0.669(10) 1 calc PR A 1 H4S2 H 0.8273 0.7282 3.5421 0.046 Uiso 0.669(10) 1 calc PR A 1 C3SC C 0.74189(12) 0.6184(2) 3.50501(14) 0.058(4) Uani 0.669(10) 1 d PRDU A 1 H3S1 H 0.7332 0.6142 3.4617 0.070 Uiso 0.669(10) 1 calc PR A 1 H3S2 H 0.7103 0.5931 3.5108 0.070 Uiso 0.669(10) 1 calc PR A 1 C2SC C 0.79980(12) 0.5588(2) 3.54742(14) 0.094(6) Uani 0.669(10) 1 d PRDU A 1 H2S1 H 0.7912 0.4976 3.5610 0.112 Uiso 0.669(10) 1 calc PR A 1 H2S2 H 0.8213 0.5463 3.5245 0.112 Uiso 0.669(10) 1 calc PR A 1 C1SC C 0.82682(12) 0.6137(2) 3.59309(14) 0.065(4) Uani 0.669(10) 1 d PRDU A 1 H1S1 H 0.8672 0.6080 3.6076 0.078 Uiso 0.669(10) 1 calc PR A 1 H1S2 H 0.8172 0.6019 3.6269 0.078 Uiso 0.669(10) 1 calc PR A 1 O1SD O 0.73664(12) 0.5638(2) 3.54020(14) 0.034(4) Uani 0.331(10) 1 d PRDU A 2 C1SD C 0.78913(12) 0.5320(2) 3.59040(14) 0.054(5) Uani 0.331(10) 1 d PRDU A 2 H3S3 H 0.7947 0.4629 3.5891 0.065 Uiso 0.331(10) 1 calc PR A 2 H3S4 H 0.7916 0.5497 3.6304 0.065 Uiso 0.331(10) 1 calc PR A 2 C2SD C 0.83035(12) 0.5903(2) 3.57430(14) 0.116(8) Uani 0.331(10) 1 d PRDU A 2 H1S3 H 0.8647 0.6056 3.6106 0.139 Uiso 0.331(10) 1 calc PR A 2 H1S4 H 0.8394 0.5570 3.5445 0.139 Uiso 0.331(10) 1 calc PR A 2 C3SD C 0.79825(12) 0.6701(2) 3.54980(14) 0.116(8) Uani 0.331(10) 1 d PRDU A 2 H2S3 H 0.8012 0.7111 3.5836 0.139 Uiso 0.331(10) 1 calc PR A 2 H2S4 H 0.8146 0.7053 3.5269 0.139 Uiso 0.331(10) 1 calc PR A 2 C4SD C 0.74559(12) 0.6578(2) 3.51395(14) 0.054(5) Uani 0.331(10) 1 d PRDU A 2 H4S3 H 0.7385 0.6512 3.4712 0.065 Uiso 0.331(10) 1 calc PR A 2 H4S4 H 0.7227 0.7095 3.5179 0.065 Uiso 0.331(10) 1 calc PR A 2 O1SA O 0.57463(12) 0.6055(2) 3.58616(14) 0.096(4) Uani 0.661(11) 1 d PRDU B 1 C1SA C 0.61403(12) 0.6486(2) 3.57127(14) 0.085(5) Uani 0.661(11) 1 d PRDU B 1 H1SY H 0.6101 0.6235 3.5321 0.103 Uiso 0.661(11) 1 calc PR B 1 H1SZ H 0.6073 0.7176 3.5668 0.103 Uiso 0.661(11) 1 calc PR B 1 C2SA C 0.66182(12) 0.6337(2) 3.61065(14) 0.125(8) Uani 0.661(11) 1 d PRDU B 1 H2SX H 0.6755 0.6914 3.6356 0.150 Uiso 0.661(11) 1 calc PR B 1 H2SY H 0.6858 0.6220 3.5905 0.150 Uiso 0.661(11) 1 calc PR B 1 C3SA C 0.66663(12) 0.5579(2) 3.64835(14) 0.107(6) Uani 0.661(11) 1 d PRDU B 1 H3SX H 0.6765 0.5784 3.6902 0.129 Uiso 0.661(11) 1 calc PR B 1 H3SY H 0.6937 0.5104 3.6484 0.129 Uiso 0.661(11) 1 calc PR B 1 C4SA C 0.59773(12) 0.5151(2) 3.61126(14) 0.094(6) Uani 0.661(11) 1 d PRDU B 1 H4SX H 0.5926 0.4671 3.5800 0.113 Uiso 0.661(11) 1 calc PR B 1 H4SY H 0.5840 0.4907 3.6397 0.113 Uiso 0.661(11) 1 calc PR B 1 O1SB O 0.61552(12) 0.5843(2) 3.55051(14) 0.099(7) Uani 0.339(11) 1 d PRDU B 2 C1SB C 0.66182(12) 0.6337(2) 3.61066(14) 0.078(7) Uani 0.339(11) 1 d PRDU B 2 H2S5 H 0.6888 0.6647 3.5994 0.093 Uiso 0.339(11) 1 calc PR B 2 H2S6 H 0.6435 0.6844 3.6228 0.093 Uiso 0.339(11) 1 calc PR B 2 C2SB C 0.68602(12) 0.5880(2) 3.65230(14) 0.079(7) Uani 0.339(11) 1 d PRDU B 2 H1S7 H 0.6994 0.6256 3.6900 0.095 Uiso 0.339(11) 1 calc PR B 2 H1S8 H 0.7176 0.5561 3.6498 0.095 Uiso 0.339(11) 1 calc PR B 2 C3SB C 0.63873(12) 0.5129(2) 3.64750(14) 0.079(7) Uani 0.339(11) 1 d PRDU B 2 H3S5 H 0.6530 0.4472 3.6552 0.095 Uiso 0.339(11) 1 calc PR B 2 H3S6 H 0.6227 0.5290 3.6755 0.095 Uiso 0.339(11) 1 calc PR B 2 C4SB C 0.59462(12) 0.5281(2) 3.57750(14) 0.085(7) Uani 0.339(11) 1 d PRDU B 2 H4S5 H 0.5853 0.4662 3.5566 0.102 Uiso 0.339(11) 1 calc PR B 2 H4S6 H 0.5603 0.5562 3.5756 0.102 Uiso 0.339(11) 1 calc PR B 2 O1S O 0.94651(12) 1.0254(2) 3.49946(14) 0.068(3) Uani 0.50 1 d PRDU C -1 C4S C 0.96469(12) 1.0755(2) 3.44467(14) 0.146(11) Uani 0.50 1 d PRDU C -1 H4S7 H 0.9863 1.1349 3.4575 0.175 Uiso 0.50 1 calc PR D -1 H4S8 H 0.9337 1.0815 3.4038 0.175 Uiso 0.50 1 calc PR E -1 C3S C 1.01025(12) 0.9581(2) 3.45743(14) 0.052(3) Uani 0.50 1 d PRDU C -1 H3S7 H 0.9879 0.9004 3.4408 0.063 Uiso 0.50 1 calc PR F -1 H3S8 H 1.0390 0.9642 3.4430 0.063 Uiso 0.50 1 calc PR G -1 C2S C 1.03909(12) 0.9688(2) 3.54492(14) 0.052(3) Uani 0.50 1 d PRDU C -1 H2S7 H 1.0389 0.9081 3.5649 0.063 Uiso 0.50 1 calc PR H -1 H2S8 H 1.0759 0.9987 3.5644 0.063 Uiso 0.50 1 calc PR I -1 C1S C 0.99032(12) 1.0381(2) 3.53841(14) 0.105(7) Uani 0.50 1 d PRDU C -1 H1S5 H 0.9872 1.0361 3.5769 0.126 Uiso 0.50 1 calc PR J -1 H1S6 H 1.0016 1.1032 3.5340 0.126 Uiso 0.50 1 calc PR K -1 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 Au1 0.01476(11) 0.01912(13) 0.02390(13) 0.00041(10) 0.00967(9) -0.00073(8) Nb1 0.0123(2) 0.0140(3) 0.0145(3) 0.00072(19) 0.00537(19) 0.00016(18) P1 0.0134(6) 0.0149(7) 0.0173(8) -0.0001(6) 0.0063(6) -0.0001(5) O3 0.0141(17) 0.017(2) 0.014(2) 0.0021(15) 0.0050(15) 0.0008(14) O2 0.0123(17) 0.019(2) 0.018(2) -0.0006(16) 0.0054(15) -0.0004(14) N5 0.018(2) 0.017(2) 0.017(2) 0.0018(19) 0.0084(19) 0.0012(18) O1 0.0146(17) 0.016(2) 0.019(2) 0.0000(16) 0.0079(16) -0.0005(14) N1 0.014(2) 0.017(2) 0.016(2) 0.0021(19) 0.0058(19) 0.0005(17) N4 0.021(2) 0.019(3) 0.040(3) 0.000(2) 0.018(2) -0.001(2) C70 0.014(2) 0.015(3) 0.016(3) -0.002(2) 0.008(2) 0.000(2) C16 0.017(3) 0.024(3) 0.022(3) 0.000(2) 0.008(2) 0.001(2) N3 0.015(2) 0.015(2) 0.016(2) 0.0010(18) 0.0066(18) -0.0005(17) C11 0.017(2) 0.015(3) 0.018(3) 0.003(2) 0.008(2) 0.003(2) C711 0.019(3) 0.023(3) 0.021(3) 0.003(2) 0.012(2) 0.001(2) C81 0.016(2) 0.014(3) 0.020(3) 0.001(2) 0.005(2) 0.001(2) C56 0.020(3) 0.030(3) 0.022(3) 0.008(3) 0.007(2) 0.002(2) C21 0.019(3) 0.018(3) 0.021(3) 0.003(2) 0.010(2) 0.003(2) C15 0.024(3) 0.025(3) 0.033(3) 0.002(3) 0.017(3) 0.001(2) C821 0.019(3) 0.022(3) 0.018(3) -0.001(2) 0.005(2) -0.006(2) C410 0.021(3) 0.023(3) 0.020(3) -0.003(2) 0.009(2) 0.001(2) C80 0.016(2) 0.012(3) 0.019(3) 0.001(2) 0.007(2) 0.003(2) C210 0.020(3) 0.019(3) 0.023(3) 0.000(2) 0.011(2) 0.004(2) C812 0.019(3) 0.025(3) 0.023(3) 0.001(3) 0.005(2) 0.003(2) C61 0.024(3) 0.018(3) 0.016(3) 0.001(2) 0.008(2) 0.000(2) C213 0.027(3) 0.022(3) 0.027(3) 0.002(3) 0.014(3) 0.007(2) C51 0.018(3) 0.019(3) 0.018(3) 0.008(2) 0.005(2) 0.003(2) C721 0.017(2) 0.013(3) 0.026(3) 0.004(2) 0.011(2) 0.004(2) C52 0.021(3) 0.017(3) 0.024(3) 0.003(2) 0.007(2) 0.002(2) C211 0.024(3) 0.023(3) 0.033(4) -0.001(3) 0.013(3) -0.001(2) C813 0.017(3) 0.032(4) 0.028(3) 0.000(3) 0.006(3) 0.006(2) C811 0.016(2) 0.021(3) 0.017(3) 0.004(2) 0.004(2) 0.002(2) C712 0.023(3) 0.025(3) 0.020(3) 0.003(2) 0.010(2) 0.002(2) C71 0.016(2) 0.020(3) 0.018(3) -0.001(2) 0.009(2) 0.002(2) C13 0.028(3) 0.021(3) 0.019(3) 0.003(2) 0.011(2) 0.005(2) C610 0.024(3) 0.025(3) 0.022(3) 0.004(3) 0.008(2) 0.001(2) C12 0.017(2) 0.012(3) 0.024(3) 0.000(2) 0.007(2) 0.001(2) C41 0.017(3) 0.015(3) 0.024(3) -0.003(2) 0.006(2) 0.000(2) C36 0.020(3) 0.022(3) 0.017(3) -0.003(2) 0.006(2) 0.000(2) C916 0.021(3) 0.032(4) 0.020(3) -0.006(3) 0.008(2) -0.006(2) C921 0.011(2) 0.022(3) 0.022(3) 0.000(2) 0.006(2) 0.003(2) C31 0.014(2) 0.024(3) 0.017(3) -0.005(2) 0.005(2) -0.002(2) C823 0.037(3) 0.045(4) 0.020(3) -0.003(3) 0.006(3) -0.006(3) C35 0.019(3) 0.030(3) 0.016(3) -0.005(3) 0.004(2) 0.004(2) C91 0.018(3) 0.019(3) 0.016(3) -0.002(2) 0.007(2) 0.000(2) C911 0.021(3) 0.022(3) 0.022(3) -0.007(2) 0.013(2) -0.004(2) C725 0.026(3) 0.022(3) 0.036(4) 0.005(3) 0.017(3) -0.002(2) C713 0.027(3) 0.040(4) 0.016(3) 0.004(3) 0.005(2) 0.007(3) C212 0.026(3) 0.019(3) 0.030(3) 0.005(3) 0.013(3) 0.006(2) C723 0.026(3) 0.019(3) 0.027(3) -0.002(3) 0.011(3) -0.002(2) C922 0.021(3) 0.026(3) 0.027(3) -0.006(3) 0.010(3) -0.001(2) C53 0.028(3) 0.022(3) 0.029(4) 0.005(3) 0.007(3) -0.002(2) C926 0.020(3) 0.023(3) 0.030(3) 0.002(3) 0.011(3) 0.004(2) C90 0.013(2) 0.018(3) 0.017(3) -0.001(2) 0.005(2) 0.000(2) C923 0.020(3) 0.031(4) 0.040(4) -0.011(3) 0.012(3) 0.001(2) C726 0.023(3) 0.018(3) 0.024(3) 0.004(2) 0.010(2) 0.001(2) C14 0.029(3) 0.027(3) 0.027(3) 0.006(3) 0.020(3) 0.004(2) C816 0.016(3) 0.019(3) 0.029(3) 0.000(3) 0.005(2) 0.000(2) C716 0.021(3) 0.022(3) 0.031(4) 0.004(3) 0.013(3) 0.000(2) C54 0.029(3) 0.023(3) 0.040(4) 0.009(3) 0.007(3) -0.007(3) C822 0.025(3) 0.034(4) 0.022(3) -0.001(3) 0.007(3) -0.003(3) C32 0.020(3) 0.026(3) 0.020(3) 0.000(3) 0.009(2) -0.001(2) C551 0.036(4) 0.054(5) 0.050(5) 0.015(4) 0.025(4) -0.008(3) C815 0.018(3) 0.028(3) 0.032(4) 0.007(3) 0.004(3) -0.003(2) C33 0.022(3) 0.038(4) 0.020(3) -0.003(3) 0.010(2) -0.009(3) C34 0.016(3) 0.042(4) 0.020(3) -0.006(3) 0.006(2) -0.002(2) C722 0.020(3) 0.022(3) 0.023(3) 0.000(2) 0.013(2) 0.000(2) C55 0.022(3) 0.037(4) 0.033(4) 0.013(3) 0.013(3) -0.001(3) C714 0.026(3) 0.035(4) 0.025(4) 0.008(3) 0.007(3) 0.011(3) C611 0.033(3) 0.026(3) 0.031(4) 0.012(3) 0.008(3) 0.005(3) C724 0.024(3) 0.023(3) 0.035(4) 0.000(3) 0.012(3) -0.006(2) C531 0.048(4) 0.018(3) 0.050(5) -0.002(3) 0.016(4) -0.006(3) C814 0.016(3) 0.036(4) 0.029(4) 0.006(3) 0.008(3) 0.005(2) C413 0.030(3) 0.038(4) 0.023(3) -0.007(3) 0.007(3) 0.004(3) C912 0.021(3) 0.029(4) 0.029(4) -0.007(3) 0.010(3) 0.002(2) C826 0.024(3) 0.027(3) 0.023(3) -0.005(3) 0.007(3) -0.002(2) C131 0.038(4) 0.039(4) 0.022(3) 0.004(3) 0.016(3) 0.002(3) C925 0.027(3) 0.021(3) 0.046(4) 0.009(3) 0.017(3) 0.004(3) C914 0.035(3) 0.046(4) 0.043(4) -0.013(3) 0.027(3) -0.014(3) C351 0.027(3) 0.041(4) 0.029(4) 0.000(3) 0.008(3) 0.010(3) C715 0.032(3) 0.024(3) 0.036(4) 0.013(3) 0.019(3) 0.011(3) C1 0.031(3) 0.035(4) 0.047(4) 0.016(3) 0.023(3) 0.006(3) C825 0.035(3) 0.035(4) 0.032(4) -0.012(3) 0.019(3) -0.001(3) C412 0.027(3) 0.039(4) 0.028(4) -0.011(3) 0.008(3) 0.006(3) C5 0.023(3) 0.045(4) 0.040(4) -0.007(3) 0.013(3) -0.005(3) C913 0.022(3) 0.044(4) 0.044(4) -0.011(3) 0.019(3) -0.006(3) C151 0.027(3) 0.052(5) 0.039(4) 0.002(3) 0.020(3) -0.006(3) C411 0.062(5) 0.042(4) 0.024(4) -0.006(3) 0.022(4) -0.022(4) C613 0.049(4) 0.030(4) 0.027(4) 0.006(3) -0.002(3) -0.005(3) C331 0.028(3) 0.053(5) 0.036(4) 0.001(3) 0.017(3) -0.016(3) C824 0.047(4) 0.048(4) 0.025(4) -0.012(3) 0.019(3) -0.014(3) C612 0.024(3) 0.053(5) 0.041(4) 0.017(3) 0.016(3) 0.015(3) C2 0.040(4) 0.041(4) 0.053(5) 0.015(4) 0.031(3) 0.007(3) C915 0.036(3) 0.037(4) 0.025(3) -0.004(3) 0.015(3) -0.013(3) C924 0.025(3) 0.021(3) 0.060(5) -0.008(3) 0.015(3) 0.002(3) C4 0.022(3) 0.063(5) 0.061(5) -0.007(4) 0.019(3) -0.011(3) C3 0.050(4) 0.042(5) 0.070(5) 0.000(4) 0.045(4) -0.007(4) O1SC 0.066(6) 0.083(7) 0.062(7) -0.016(5) 0.008(5) 0.012(5) C4SC 0.034(5) 0.046(6) 0.038(6) -0.001(5) 0.018(5) -0.002(5) C3SC 0.053(7) 0.079(9) 0.030(7) -0.026(7) 0.007(5) -0.019(6) C2SC 0.110(12) 0.053(8) 0.078(11) -0.010(7) 0.005(9) 0.010(8) C1SC 0.047(7) 0.067(8) 0.052(8) 0.027(6) -0.003(5) -0.024(6) O1SD 0.033(7) 0.041(8) 0.017(7) 0.005(6) 0.001(5) -0.005(6) C1SD 0.035(7) 0.097(12) 0.024(9) 0.009(8) 0.008(6) -0.006(8) C2SD 0.052(8) 0.127(14) 0.118(15) 0.048(12) -0.009(10) -0.028(10) C3SD 0.052(8) 0.127(14) 0.118(15) 0.048(12) -0.009(10) -0.028(10) C4SD 0.035(7) 0.097(12) 0.024(9) 0.009(8) 0.008(6) -0.006(8) O1SA 0.076(7) 0.070(7) 0.124(10) 0.005(7) 0.027(6) -0.009(6) C1SA 0.132(12) 0.067(10) 0.043(9) 0.004(7) 0.026(8) -0.035(10) C2SA 0.109(11) 0.163(18) 0.107(16) -0.003(12) 0.052(11) -0.042(13) C3SA 0.121(11) 0.103(13) 0.074(12) -0.013(9) 0.021(9) 0.064(11) C4SA 0.169(14) 0.029(7) 0.127(16) -0.001(8) 0.105(12) -0.008(8) O1SB 0.164(18) 0.085(15) 0.047(10) -0.011(9) 0.046(10) 0.013(13) C1SB 0.116(18) 0.081(16) 0.063(14) -0.016(11) 0.065(12) 0.018(12) C2SB 0.112(14) 0.062(13) 0.071(11) -0.011(9) 0.046(9) 0.014(11) C3SB 0.112(14) 0.062(13) 0.071(11) -0.011(9) 0.046(9) 0.014(11) C4SB 0.091(15) 0.11(2) 0.080(15) -0.028(14) 0.058(11) 0.013(12) O1S 0.083(8) 0.026(6) 0.101(11) -0.007(6) 0.045(7) -0.011(6) C4S 0.055(13) 0.29(3) 0.092(16) 0.019(17) 0.035(12) 0.063(18) C3S 0.060(7) 0.040(7) 0.068(8) 0.016(6) 0.038(6) -0.023(5) C2S 0.060(7) 0.040(7) 0.068(8) 0.016(6) 0.038(6) -0.023(5) C1S 0.102(13) 0.12(2) 0.127(14) -0.013(13) 0.081(12) 0.015(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N4 2.092(5) . ? Au1 P1 2.2446(14) . ? Nb1 N1 2.027(4) . ? Nb1 N3 2.030(5) . ? Nb1 N5 2.031(4) . ? Nb1 O3 2.093(4) . ? Nb1 O1 2.097(3) . ? Nb1 O2 2.107(4) . ? P1 C80 1.845(6) . ? P1 C90 1.850(6) . ? P1 C70 1.863(5) . ? O3 C70 1.330(6) . ? O2 C80 1.325(6) . ? N5 C51 1.442(7) . ? N5 C61 1.485(7) . ? O1 C90 1.328(6) . ? N1 C11 1.442(7) . ? N1 C21 1.487(7) . ? N4 C5 1.322(7) . ? N4 C1 1.341(8) . ? C70 C71 1.360(7) . ? C16 C15 1.396(8) . ? C16 C11 1.403(7) . ? N3 C31 1.443(6) . ? N3 C41 1.503(7) . ? C11 C12 1.380(8) . ? C711 C716 1.401(8) . ? C711 C712 1.406(8) . ? C711 C71 1.496(7) . ? C81 C80 1.369(7) . ? C81 C811 1.483(7) . ? C81 C821 1.492(8) . ? C56 C51 1.391(8) . ? C56 C55 1.392(8) . ? C21 C210 1.562(8) . ? C15 C14 1.382(9) . ? C15 C151 1.523(8) . ? C821 C826 1.399(8) . ? C821 C822 1.404(8) . ? C410 C412 1.530(8) . ? C410 C411 1.531(8) . ? C410 C413 1.534(8) . ? C410 C41 1.542(8) . ? C210 C212 1.529(8) . ? C210 C211 1.534(8) . ? C210 C213 1.539(7) . ? C812 C813 1.382(8) . ? C812 C811 1.400(8) . ? C61 C610 1.543(8) . ? C51 C52 1.394(8) . ? C721 C726 1.401(7) . ? C721 C722 1.405(8) . ? C721 C71 1.492(7) . ? C52 C53 1.382(8) . ? C813 C814 1.380(8) . ? C811 C816 1.402(8) . ? C712 C713 1.387(8) . ? C13 C14 1.395(8) . ? C13 C12 1.397(7) . ? C13 C131 1.503(8) . ? C610 C613 1.524(9) . ? C610 C612 1.535(8) . ? C610 C611 1.542(8) . ? C36 C31 1.391(8) . ? C36 C35 1.394(7) . ? C916 C911 1.391(8) . ? C916 C915 1.399(8) . ? C921 C922 1.406(8) . ? C921 C926 1.412(8) . ? C921 C91 1.482(8) . ? C31 C32 1.393(8) . ? C823 C824 1.365(9) . ? C823 C822 1.399(9) . ? C35 C34 1.397(8) . ? C35 C351 1.505(8) . ? C91 C90 1.358(7) . ? C91 C911 1.506(7) . ? C911 C912 1.408(7) . ? C725 C724 1.384(9) . ? C725 C726 1.394(8) . ? C713 C714 1.390(9) . ? C723 C724 1.377(8) . ? C723 C722 1.389(8) . ? C922 C923 1.372(8) . ? C53 C54 1.390(9) . ? C53 C531 1.527(9) . ? C926 C925 1.381(8) . ? C923 C924 1.386(10) . ? C816 C815 1.379(8) . ? C716 C715 1.384(8) . ? C54 C55 1.391(9) . ? C32 C33 1.398(8) . ? C551 C55 1.516(8) . ? C815 C814 1.395(9) . ? C33 C34 1.379(9) . ? C33 C331 1.519(8) . ? C714 C715 1.389(9) . ? C912 C913 1.396(8) . ? C826 C825 1.381(8) . ? C925 C924 1.391(9) . ? C914 C915 1.375(9) . ? C914 C913 1.384(10) . ? C1 C2 1.374(8) . ? C825 C824 1.389(9) . ? C5 C4 1.411(9) . ? C2 C3 1.328(8) . ? C4 C3 1.388(9) . ? O1SC C3SC 1.2371 . ? O1SC C4SC 1.3445 . ? C4SC C1SC 1.4996 . ? C3SC C2SC 1.6762 . ? C2SC C1SC 1.2958 . ? O1SD C1SD 1.4831 . ? O1SD C4SD 1.5416 . ? C1SD C2SD 1.5697 . ? C2SD C3SD 1.3879 . ? C3SD C4SD 1.3148 . ? O1SA C1SA 1.4078 . ? O1SA C4SA 1.4356 . ? C1SA C2SA 1.2453 . ? C2SA C3SA 1.3858 . ? C3SA C4SA 1.7796 . ? O1SB C4SB 1.3125 . ? O1SB C1SB 1.6179 . ? C1SB C2SB 1.1432 . ? C2SB C3SB 1.6243 . ? C3SB C4SB 1.6231 . ? O1S C1S 1.1640 . ? O1S C4S 1.7754 . ? C4S C3S 2.0055 . ? C3S C2S 1.9504 . ? C2S C1S 1.5918 . ? 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 N4 Au1 P1 173.86(15) . . ? N1 Nb1 N3 98.16(18) . . ? N1 Nb1 N5 95.84(17) . . ? N3 Nb1 N5 97.22(18) . . ? N1 Nb1 O3 89.08(16) . . ? N3 Nb1 O3 92.37(16) . . ? N5 Nb1 O3 168.47(16) . . ? N1 Nb1 O1 168.82(16) . . ? N3 Nb1 O1 87.47(15) . . ? N5 Nb1 O1 93.01(15) . . ? O3 Nb1 O1 81.00(14) . . ? N1 Nb1 O2 92.69(16) . . ? N3 Nb1 O2 167.35(15) . . ? N5 Nb1 O2 88.05(16) . . ? O3 Nb1 O2 81.30(14) . . ? O1 Nb1 O2 80.76(14) . . ? C80 P1 C90 100.0(2) . . ? C80 P1 C70 98.0(2) . . ? C90 P1 C70 102.6(2) . . ? C80 P1 Au1 122.72(17) . . ? C90 P1 Au1 115.73(17) . . ? C70 P1 Au1 114.52(17) . . ? C70 O3 Nb1 127.6(3) . . ? C80 O2 Nb1 131.8(3) . . ? C51 N5 C61 111.0(4) . . ? C51 N5 Nb1 122.6(3) . . ? C61 N5 Nb1 126.0(3) . . ? C90 O1 Nb1 132.2(3) . . ? C11 N1 C21 111.0(4) . . ? C11 N1 Nb1 121.3(3) . . ? C21 N1 Nb1 127.3(3) . . ? C5 N4 C1 118.6(5) . . ? C5 N4 Au1 123.0(5) . . ? C1 N4 Au1 118.5(4) . . ? O3 C70 C71 126.0(5) . . ? O3 C70 P1 112.7(4) . . ? C71 C70 P1 121.2(4) . . ? C15 C16 C11 119.9(5) . . ? C31 N3 C41 111.5(4) . . ? C31 N3 Nb1 120.9(3) . . ? C41 N3 Nb1 127.2(3) . . ? C12 C11 C16 119.3(5) . . ? C12 C11 N1 120.6(5) . . ? C16 C11 N1 120.1(5) . . ? C716 C711 C712 117.7(5) . . ? C716 C711 C71 120.7(5) . . ? C712 C711 C71 121.6(5) . . ? C80 C81 C811 121.3(5) . . ? C80 C81 C821 121.6(5) . . ? C811 C81 C821 117.1(5) . . ? C51 C56 C55 121.1(6) . . ? N1 C21 C210 120.2(5) . . ? C14 C15 C16 119.6(5) . . ? C14 C15 C151 121.2(5) . . ? C16 C15 C151 119.2(6) . . ? C826 C821 C822 118.0(5) . . ? C826 C821 C81 121.6(5) . . ? C822 C821 C81 120.4(5) . . ? C412 C410 C411 110.0(5) . . ? C412 C410 C413 106.7(5) . . ? C411 C410 C413 109.6(5) . . ? C412 C410 C41 105.8(5) . . ? C411 C410 C41 110.3(5) . . ? C413 C410 C41 114.3(5) . . ? O2 C80 C81 125.4(5) . . ? O2 C80 P1 111.2(4) . . ? C81 C80 P1 122.6(4) . . ? C212 C210 C211 110.0(5) . . ? C212 C210 C213 107.0(4) . . ? C211 C210 C213 110.8(5) . . ? C212 C210 C21 105.1(5) . . ? C211 C210 C21 110.4(4) . . ? C213 C210 C21 113.4(5) . . ? C813 C812 C811 121.3(6) . . ? N5 C61 C610 118.7(5) . . ? C56 C51 C52 118.5(5) . . ? C56 C51 N5 121.3(5) . . ? C52 C51 N5 120.2(5) . . ? C726 C721 C722 118.2(5) . . ? C726 C721 C71 122.4(5) . . ? C722 C721 C71 119.3(5) . . ? C53 C52 C51 122.0(5) . . ? C814 C813 C812 120.3(6) . . ? C812 C811 C816 117.5(5) . . ? C812 C811 C81 120.3(5) . . ? C816 C811 C81 122.2(5) . . ? C713 C712 C711 120.5(6) . . ? C70 C71 C721 119.5(5) . . ? C70 C71 C711 123.5(5) . . ? C721 C71 C711 116.7(5) . . ? C14 C13 C12 118.1(5) . . ? C14 C13 C131 121.5(5) . . ? C12 C13 C131 120.4(5) . . ? C613 C610 C612 109.7(5) . . ? C613 C610 C611 107.3(5) . . ? C612 C610 C611 110.3(5) . . ? C613 C610 C61 105.8(5) . . ? C612 C610 C61 109.6(5) . . ? C611 C610 C61 114.0(5) . . ? C11 C12 C13 121.6(5) . . ? N3 C41 C410 118.4(4) . . ? C31 C36 C35 121.0(5) . . ? C911 C916 C915 120.7(6) . . ? C922 C921 C926 117.1(5) . . ? C922 C921 C91 120.5(5) . . ? C926 C921 C91 122.4(5) . . ? C36 C31 C32 119.5(5) . . ? C36 C31 N3 120.3(5) . . ? C32 C31 N3 120.2(5) . . ? C824 C823 C822 119.7(6) . . ? C36 C35 C34 118.5(5) . . ? C36 C35 C351 120.1(6) . . ? C34 C35 C351 121.4(5) . . ? C90 C91 C921 122.8(5) . . ? C90 C91 C911 123.4(5) . . ? C921 C91 C911 113.6(4) . . ? C916 C911 C912 118.2(5) . . ? C916 C911 C91 121.3(5) . . ? C912 C911 C91 120.0(5) . . ? C724 C725 C726 121.2(6) . . ? C712 C713 C714 121.0(6) . . ? C724 C723 C722 120.2(6) . . ? C923 C922 C921 121.7(6) . . ? C52 C53 C54 118.1(6) . . ? C52 C53 C531 121.1(6) . . ? C54 C53 C531 120.8(6) . . ? C925 C926 C921 120.7(6) . . ? O1 C90 C91 124.0(5) . . ? O1 C90 P1 112.0(4) . . ? C91 C90 P1 123.6(4) . . ? C922 C923 C924 120.6(6) . . ? C725 C726 C721 119.7(6) . . ? C15 C14 C13 121.4(5) . . ? C815 C816 C811 121.2(6) . . ? C715 C716 C711 121.4(6) . . ? C53 C54 C55 121.9(6) . . ? C823 C822 C821 120.9(6) . . ? C31 C32 C33 120.0(6) . . ? C816 C815 C814 120.2(6) . . ? C34 C33 C32 119.6(6) . . ? C34 C33 C331 121.0(5) . . ? C32 C33 C331 119.4(6) . . ? C33 C34 C35 121.3(5) . . ? C723 C722 C721 121.1(5) . . ? C54 C55 C56 118.5(6) . . ? C54 C55 C551 121.5(6) . . ? C56 C55 C551 120.0(6) . . ? C715 C714 C713 119.0(6) . . ? C723 C724 C725 119.5(6) . . ? C813 C814 C815 119.5(5) . . ? C913 C912 C911 120.5(6) . . ? C825 C826 C821 120.6(6) . . ? C926 C925 C924 120.9(6) . . ? C915 C914 C913 119.7(6) . . ? C716 C715 C714 120.4(6) . . ? N4 C1 C2 122.5(6) . . ? C826 C825 C824 120.3(6) . . ? N4 C5 C4 121.2(7) . . ? C914 C913 C912 120.3(6) . . ? C823 C824 C825 120.5(6) . . ? C3 C2 C1 119.8(6) . . ? C914 C915 C916 120.6(6) . . ? C923 C924 C925 118.9(6) . . ? C3 C4 C5 118.3(6) . . ? C2 C3 C4 119.4(5) . . ? C3SC O1SC C4SC 108.7 . . ? O1SC C4SC C1SC 111.2 . . ? O1SC C3SC C2SC 104.6 . . ? C1SC C2SC C3SC 104.8 . . ? C2SC C1SC C4SC 98.7 . . ? C1SD O1SD C4SD 110.0 . . ? O1SD C1SD C2SD 98.9 . . ? C3SD C2SD C1SD 99.2 . . ? C4SD C3SD C2SD 118.0 . . ? C3SD C4SD O1SD 98.9 . . ? C1SA O1SA C4SA 105.1 . . ? C2SA C1SA O1SA 111.5 . . ? C1SA C2SA C3SA 114.4 . . ? C2SA C3SA C4SA 98.6 . . ? O1SA C4SA C3SA 94.5 . . ? C4SB O1SB C1SB 97.3 . . ? C2SB C1SB O1SB 119.1 . . ? C1SB C2SB C3SB 100.5 . . ? C4SB C3SB C2SB 100.2 . . ? O1SB C4SB C3SB 109.9 . . ? C1S O1S C4S 92.6 . . ? O1S C4S C3S 84.7 . . ? C2S C3S C4S 91.6 . . ? C1S C2S C3S 91.5 . . ? O1S C1S C2S 119.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.731 _refine_diff_density_min -1.346 _refine_diff_density_rms 0.110 # Attachment '2141_web_deposit_cif_file_1_SidCreutz_1281724091.cif' data_10096 _database_code_depnum_ccdc_archive 'CCDC 789236' #TrackingRef '2141_web_deposit_cif_file_1_SidCreutz_1281724091.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (pyr)AgP(C[CPh2]O)3Nb(N[Np]Ar)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H115 Ag N4 Nb O5.50 P' _chemical_formula_weight 1644.67 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' Nb Nb -2.0727 0.6215 '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 ? _symmetry_space_group_name_H-M P21/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 27.086(2) _cell_length_b 14.0697(11) _cell_length_c 24.790(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.3960(10) _cell_angle_gamma 90.00 _cell_volume 8462.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8262 _exptl_absorpt_correction_T_max 0.8609 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 35973 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 29.53 _reflns_number_total 21967 _reflns_number_gt 13833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21967 _refine_ls_number_parameters 1077 _refine_ls_number_restraints 1236 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.212035(11) 1.083586(19) -0.271892(12) 0.01427(7) Uani 1 1 d U . . Ag1 Ag 0.401630(10) 0.930466(18) -0.301227(12) 0.02549(8) Uani 1 1 d U . . P1 P 0.32791(3) 0.99012(6) -0.28440(4) 0.01567(16) Uani 1 1 d U . . O1 O 0.21743(8) 0.98342(14) -0.33169(9) 0.0162(4) Uani 1 1 d U . . O2 O 0.27287(8) 1.15025(14) -0.28920(9) 0.0177(5) Uani 1 1 d U . . O3 O 0.28158(8) 1.00760(14) -0.21058(9) 0.0167(4) Uani 1 1 d U . . C16 C 0.08686(13) 1.0504(2) -0.23121(15) 0.0215(7) Uani 1 1 d U . . H16 H 0.0633 1.0630 -0.2724 0.026 Uiso 1 1 calc R . . N1 N 0.22298(10) 1.17370(17) -0.20330(11) 0.0166(5) Uani 1 1 d U . . N4 N 0.45674(11) 0.8646(2) -0.33191(14) 0.0272(7) Uani 1 1 d U . . C900 C 0.26039(12) 0.9298(2) -0.32381(13) 0.0162(6) Uani 1 1 d U . . C21 C 0.12851(13) 0.9135(2) -0.29756(14) 0.0186(6) Uani 1 1 d U . . H21A H 0.1403 0.9073 -0.3299 0.022 Uiso 1 1 calc R . . H21B H 0.0889 0.9303 -0.3174 0.022 Uiso 1 1 calc R . . N3 N 0.15584(10) 1.16322(17) -0.34000(11) 0.0164(5) Uani 1 1 d U . . N2 N 0.15867(10) 0.99628(17) -0.25957(11) 0.0171(5) Uani 1 1 d U . . C220 C 0.14013(13) 1.0156(2) -0.21445(14) 0.0177(6) Uani 1 1 d U . . C52 C 0.06774(13) 1.0772(2) -0.38618(14) 0.0198(7) Uani 1 1 d U . . H52 H 0.0855 1.0277 -0.3970 0.024 Uiso 1 1 calc R . . C801 C 0.37723(12) 0.9689(2) -0.15827(14) 0.0182(6) Uani 1 1 d U . . C911 C 0.20535(13) 0.7927(2) -0.38800(14) 0.0191(7) Uani 1 1 d U . . C32 C 0.15451(13) 1.2717(2) -0.18884(15) 0.0244(7) Uani 1 1 d U . . H32 H 0.1483 1.2208 -0.1674 0.029 Uiso 1 1 calc R . . C724 C 0.31793(14) 1.4097(2) -0.40683(16) 0.0274(8) Uani 1 1 d U . . H724 H 0.3195 1.4362 -0.4413 0.033 Uiso 1 1 calc R . . C36 C 0.20015(13) 1.3350(2) -0.24448(14) 0.0229(7) Uani 1 1 d U . . H36 H 0.2257 1.3274 -0.2608 0.028 Uiso 1 1 calc R . . C701 C 0.33380(12) 1.1675(2) -0.33396(13) 0.0177(6) Uani 1 1 d U . . C51 C 0.09792(12) 1.1564(2) -0.35595(13) 0.0183(6) Uani 1 1 d U . . C901 C 0.25759(13) 0.8387(2) -0.34525(14) 0.0179(6) Uani 1 1 d U . . C223 C 0.10301(14) 0.8050(2) -0.22999(16) 0.0264(8) Uani 1 1 d U . . H22A H 0.0644 0.8235 -0.2534 0.040 Uiso 1 1 calc R . . H22B H 0.1204 0.8466 -0.1948 0.040 Uiso 1 1 calc R . . H22C H 0.1049 0.7390 -0.2166 0.040 Uiso 1 1 calc R . . C53 C 0.01213(14) 1.0687(2) -0.40099(15) 0.0254(7) Uani 1 1 d U . . C55 C 0.01526(14) 1.2250(3) -0.35769(15) 0.0270(8) Uani 1 1 d U . . C31 C 0.19166(13) 1.2600(2) -0.21282(14) 0.0202(7) Uani 1 1 d U . . C721 C 0.32510(12) 1.2715(2) -0.34440(14) 0.0188(6) Uani 1 1 d U . . C35 C 0.17205(15) 1.4208(2) -0.25266(17) 0.0301(8) Uani 1 1 d U . . C22 C 0.13335(13) 0.8143(2) -0.26930(15) 0.0205(7) Uani 1 1 d U . . C821 C 0.37576(13) 0.9462(2) -0.10021(14) 0.0217(7) Uani 1 1 d U . . C15 C 0.06822(14) 1.0667(2) -0.18810(17) 0.0273(8) Uani 1 1 d U . . C926 C 0.33548(13) 0.7624(2) -0.25796(15) 0.0207(7) Uani 1 1 d U . . H926 H 0.3215 0.7903 -0.2326 0.025 Uiso 1 1 calc R . . C13 C 0.15621(14) 1.0128(2) -0.10998(15) 0.0232(7) Uani 1 1 d U . . C924 C 0.40247(14) 0.6640(2) -0.26965(17) 0.0292(8) Uani 1 1 d U . . H924 H 0.4345 0.6253 -0.2527 0.035 Uiso 1 1 calc R . . C711 C 0.36862(13) 1.1242(2) -0.36004(14) 0.0194(7) Uani 1 1 d U . . C722 C 0.30420(14) 1.4281(2) -0.31924(17) 0.0291(8) Uani 1 1 d U . . H722 H 0.2966 1.4678 -0.2928 0.035 Uiso 1 1 calc R . . C42 C 0.30546(13) 1.2282(2) -0.10364(14) 0.0231(7) Uani 1 1 d U . . C800 C 0.33050(12) 0.9933(2) -0.20871(14) 0.0170(6) Uani 1 1 d U . . C62 C 0.15016(13) 1.2254(2) -0.44178(15) 0.0236(7) Uani 1 1 d U . . C222 C 0.10426(14) 0.7461(2) -0.32276(15) 0.0250(7) Uani 1 1 d U . . H22D H 0.0654 0.7641 -0.3450 0.038 Uiso 1 1 calc R . . H22E H 0.1069 0.6809 -0.3078 0.038 Uiso 1 1 calc R . . H22F H 0.1220 0.7498 -0.3496 0.038 Uiso 1 1 calc R . . C816 C 0.44894(14) 1.0450(2) -0.18180(15) 0.0256(7) Uani 1 1 d U . . H816 H 0.4254 1.0985 -0.1970 0.031 Uiso 1 1 calc R . . C61 C 0.16709(13) 1.2404(2) -0.37393(14) 0.0192(7) Uani 1 1 d U . . H61A H 0.2072 1.2533 -0.3537 0.023 Uiso 1 1 calc R . . H61B H 0.1483 1.2985 -0.3699 0.023 Uiso 1 1 calc R . . C56 C 0.07104(13) 1.2306(2) -0.34234(15) 0.0239(7) Uani 1 1 d U . . H56 H 0.0912 1.2856 -0.3223 0.029 Uiso 1 1 calc R . . C916 C 0.20127(14) 0.6931(2) -0.39245(16) 0.0242(7) Uani 1 1 d U . . H916 H 0.2317 0.6553 -0.3666 0.029 Uiso 1 1 calc R . . C725 C 0.32802(13) 1.3133(2) -0.39467(15) 0.0229(7) Uani 1 1 d U . . H725 H 0.3370 1.2750 -0.4206 0.027 Uiso 1 1 calc R . . C221 C 0.19393(14) 0.7856(2) -0.23399(17) 0.0300(8) Uani 1 1 d U . . H22G H 0.2124 0.7914 -0.2600 0.045 Uiso 1 1 calc R . . H22H H 0.1962 0.7196 -0.2204 0.045 Uiso 1 1 calc R . . H22I H 0.2120 0.8273 -0.1990 0.045 Uiso 1 1 calc R . . C14 C 0.10345(14) 1.0479(2) -0.12750(16) 0.0274(8) Uani 1 1 d U . . H14 H 0.0909 1.0594 -0.0978 0.033 Uiso 1 1 calc R . . C700 C 0.30879(12) 1.1156(2) -0.30669(13) 0.0164(6) Uani 1 1 d U . . C41 C 0.25896(13) 1.1568(2) -0.13796(14) 0.0209(7) Uani 1 1 d U . . H41A H 0.2759 1.0933 -0.1339 0.025 Uiso 1 1 calc R . . H41B H 0.2350 1.1541 -0.1174 0.025 Uiso 1 1 calc R . . C925 C 0.38248(14) 0.7061(2) -0.23278(16) 0.0254(7) Uani 1 1 d U . . H925 H 0.4008 0.6965 -0.1905 0.030 Uiso 1 1 calc R . . C812 C 0.46852(13) 0.8914(2) -0.13577(15) 0.0259(7) Uani 1 1 d U . . H812 H 0.4586 0.8382 -0.1191 0.031 Uiso 1 1 calc R . . C12 C 0.17445(13) 0.9967(2) -0.15393(14) 0.0192(6) Uani 1 1 d U . . H12 H 0.2105 0.9726 -0.1424 0.023 Uiso 1 1 calc R . . C921 C 0.30832(13) 0.7788(2) -0.32016(14) 0.0188(6) Uani 1 1 d U . . C915 C 0.15363(15) 0.6492(3) -0.43388(16) 0.0307(8) Uani 1 1 d U . . H915 H 0.1518 0.5818 -0.4365 0.037 Uiso 1 1 calc R . . C712 C 0.34484(15) 1.0680(2) -0.41204(15) 0.0266(8) Uani 1 1 d U . . H712 H 0.3074 1.0492 -0.4273 0.032 Uiso 1 1 calc R . . C54 C -0.01347(14) 1.1429(3) -0.38594(15) 0.0276(8) Uani 1 1 d U . . H54 H -0.0513 1.1374 -0.3951 0.033 Uiso 1 1 calc R . . C726 C 0.31363(13) 1.3314(2) -0.30669(15) 0.0229(7) Uani 1 1 d U . . H726 H 0.3122 1.3060 -0.2719 0.027 Uiso 1 1 calc R . . C824 C 0.37439(17) 0.9038(3) 0.00937(17) 0.0410(10) Uani 1 1 d U . . H824 H 0.3735 0.8909 0.0465 0.049 Uiso 1 1 calc R . . C912 C 0.15938(14) 0.8454(2) -0.42660(14) 0.0242(7) Uani 1 1 d U . . H912 H 0.1610 0.9128 -0.4250 0.029 Uiso 1 1 calc R . . C822 C 0.33016(14) 0.9041(2) -0.09872(15) 0.0275(8) Uani 1 1 d U . . H822 H 0.2990 0.8893 -0.1355 0.033 Uiso 1 1 calc R . . C811 C 0.43144(13) 0.9677(2) -0.15904(14) 0.0203(7) Uani 1 1 d U . . C423 C 0.28560(15) 1.3233(2) -0.08977(16) 0.0312(8) Uani 1 1 d U . . H42A H 0.2636 1.3113 -0.0680 0.047 Uiso 1 1 calc R . . H42B H 0.2630 1.3565 -0.1276 0.047 Uiso 1 1 calc R . . H42C H 0.3175 1.3626 -0.0649 0.047 Uiso 1 1 calc R . . C825 C 0.42068(17) 0.9431(3) 0.00898(17) 0.0375(9) Uani 1 1 d U . . H825 H 0.4522 0.9556 0.0459 0.045 Uiso 1 1 calc R . . C815 C 0.49959(14) 1.0453(3) -0.18269(16) 0.0320(8) Uani 1 1 d U . . H815 H 0.5101 1.0983 -0.1991 0.038 Uiso 1 1 calc R . . C826 C 0.42139(15) 0.9644(3) -0.04493(15) 0.0292(8) Uani 1 1 d U . . H826 H 0.4535 0.9921 -0.0446 0.035 Uiso 1 1 calc R . . C913 C 0.11161(15) 0.8012(3) -0.46706(16) 0.0300(8) Uani 1 1 d U . . H913 H 0.0806 0.8385 -0.4920 0.036 Uiso 1 1 calc R . . C922 C 0.32906(13) 0.7354(2) -0.35654(15) 0.0239(7) Uani 1 1 d U . . H922 H 0.3112 0.7449 -0.3989 0.029 Uiso 1 1 calc R . . C623 C 0.17514(17) 1.1349(3) -0.45121(16) 0.0374(9) Uani 1 1 d U . . H62A H 0.1601 1.0805 -0.4388 0.056 Uiso 1 1 calc R . . H62B H 0.2152 1.1369 -0.4271 0.056 Uiso 1 1 calc R . . H62C H 0.1664 1.1286 -0.4939 0.056 Uiso 1 1 calc R . . C422 C 0.33925(15) 1.2450(3) -0.13821(17) 0.0369(9) Uani 1 1 d U . . H42D H 0.3160 1.2750 -0.1770 0.055 Uiso 1 1 calc R . . H42E H 0.3530 1.1840 -0.1452 0.055 Uiso 1 1 calc R . . H42F H 0.3705 1.2866 -0.1147 0.055 Uiso 1 1 calc R . . C33 C 0.12610(14) 1.3574(3) -0.19584(16) 0.0300(8) Uani 1 1 d U . . C34 C 0.13554(15) 1.4305(3) -0.22762(18) 0.0337(9) Uani 1 1 d U . . H34 H 0.1165 1.4889 -0.2324 0.040 Uiso 1 1 calc R . . C531 C -0.01948(15) 0.9805(3) -0.43225(17) 0.0331(9) Uani 1 1 d U . . H53A H -0.0579 0.9867 -0.4393 0.050 Uiso 1 1 calc R . . H53B H -0.0029 0.9248 -0.4068 0.050 Uiso 1 1 calc R . . H53C H -0.0181 0.9727 -0.4709 0.050 Uiso 1 1 calc R . . C131 C 0.19471(15) 0.9913(3) -0.04454(15) 0.0320(8) Uani 1 1 d U . . H13A H 0.2301 0.9684 -0.0414 0.048 Uiso 1 1 calc R . . H13B H 0.1782 0.9423 -0.0295 0.048 Uiso 1 1 calc R . . H13C H 0.2007 1.0492 -0.0205 0.048 Uiso 1 1 calc R . . C723 C 0.30575(14) 1.4669(2) -0.36950(18) 0.0309(8) Uani 1 1 d U . . H723 H 0.2985 1.5326 -0.3782 0.037 Uiso 1 1 calc R . . C622 C 0.08746(14) 1.2256(3) -0.48100(15) 0.0314(8) Uani 1 1 d U . . H62D H 0.0711 1.1713 -0.4701 0.047 Uiso 1 1 calc R . . H62E H 0.0795 1.2207 -0.5235 0.047 Uiso 1 1 calc R . . H62F H 0.0718 1.2847 -0.4744 0.047 Uiso 1 1 calc R . . C716 C 0.42392(14) 1.1499(2) -0.33938(17) 0.0282(8) Uani 1 1 d U . . H716 H 0.4411 1.1879 -0.3042 0.034 Uiso 1 1 calc R . . C814 C 0.53501(14) 0.9694(3) -0.15997(17) 0.0338(9) Uani 1 1 d U . . H814 H 0.5699 0.9700 -0.1603 0.041 Uiso 1 1 calc R . . C5 C 0.43502(15) 0.8293(3) -0.38796(19) 0.0342(9) Uani 1 1 d U . . H5 H 0.3964 0.8352 -0.4119 0.041 Uiso 1 1 calc R . . C3 C 0.52085(17) 0.7761(3) -0.3785(2) 0.0477(11) Uani 1 1 d U . . H3 H 0.5428 0.7455 -0.3944 0.057 Uiso 1 1 calc R . . C621 C 0.17276(15) 1.3116(3) -0.46114(17) 0.0346(9) Uani 1 1 d U . . H62G H 0.1560 1.3697 -0.4549 0.052 Uiso 1 1 calc R . . H62H H 0.1640 1.3057 -0.5039 0.052 Uiso 1 1 calc R . . H62I H 0.2128 1.3147 -0.4371 0.052 Uiso 1 1 calc R . . C551 C -0.01376(15) 1.3064(3) -0.34393(18) 0.0421(10) Uani 1 1 d U . . H55A H 0.0126 1.3579 -0.3245 0.063 Uiso 1 1 calc R . . H55B H -0.0290 1.2843 -0.3169 0.063 Uiso 1 1 calc R . . H55C H -0.0437 1.3297 -0.3815 0.063 Uiso 1 1 calc R . . C923 C 0.37574(14) 0.6784(2) -0.33081(17) 0.0292(8) Uani 1 1 d U . . H923 H 0.3894 0.6489 -0.3559 0.035 Uiso 1 1 calc R . . C914 C 0.10869(15) 0.7031(3) -0.47146(16) 0.0326(9) Uani 1 1 d U . . H914 H 0.0761 0.6730 -0.5000 0.039 Uiso 1 1 calc R . . C715 C 0.45417(16) 1.1212(3) -0.36915(18) 0.0363(9) Uani 1 1 d U . . H715 H 0.4917 1.1398 -0.3544 0.044 Uiso 1 1 calc R . . C823 C 0.32908(16) 0.8832(3) -0.04446(17) 0.0377(9) Uani 1 1 d U . . H823 H 0.2973 0.8548 -0.0443 0.045 Uiso 1 1 calc R . . C713 C 0.37588(17) 1.0394(3) -0.44171(17) 0.0348(9) Uani 1 1 d U . . H713 H 0.3592 1.0014 -0.4770 0.042 Uiso 1 1 calc R . . C813 C 0.51925(14) 0.8923(3) -0.13673(17) 0.0322(9) Uani 1 1 d U . . H813 H 0.5434 0.8396 -0.1213 0.039 Uiso 1 1 calc R . . C4 C 0.46543(16) 0.7851(3) -0.4129(2) 0.0389(10) Uani 1 1 d U . . H4 H 0.4482 0.7616 -0.4530 0.047 Uiso 1 1 calc R . . C714 C 0.42972(17) 1.0654(3) -0.42054(18) 0.0402(10) Uani 1 1 d U . . H714 H 0.4505 1.0454 -0.4409 0.048 Uiso 1 1 calc R . . C151 C 0.01080(15) 1.1047(3) -0.20671(19) 0.0420(10) Uani 1 1 d U . . H15A H 0.0045 1.1124 -0.1710 0.063 Uiso 1 1 calc R . . H15B H -0.0162 1.0600 -0.2347 0.063 Uiso 1 1 calc R . . H15C H 0.0069 1.1664 -0.2266 0.063 Uiso 1 1 calc R . . C421 C 0.34188(17) 1.1803(3) -0.04294(16) 0.0404(10) Uani 1 1 d U . . H42G H 0.3202 1.1694 -0.0208 0.061 Uiso 1 1 calc R . . H42H H 0.3732 1.2217 -0.0193 0.061 Uiso 1 1 calc R . . H42I H 0.3555 1.1194 -0.0502 0.061 Uiso 1 1 calc R . . C331 C 0.08620(17) 1.3688(3) -0.1693(2) 0.0447(11) Uani 1 1 d U . . H33A H 0.0856 1.3104 -0.1480 0.067 Uiso 1 1 calc R . . H33B H 0.0493 1.3813 -0.2015 0.067 Uiso 1 1 calc R . . H33C H 0.0978 1.4221 -0.1409 0.067 Uiso 1 1 calc R . . C351 C 0.18251(18) 1.5009(3) -0.2870(2) 0.0453(11) Uani 1 1 d U . . H35A H 0.1592 1.5553 -0.2890 0.068 Uiso 1 1 calc R . . H35B H 0.1738 1.4795 -0.3279 0.068 Uiso 1 1 calc R . . H35C H 0.2214 1.5197 -0.2663 0.068 Uiso 1 1 calc R . . C1 C 0.51109(15) 0.8556(3) -0.29952(18) 0.0354(9) Uani 1 1 d U . . H1 H 0.5275 0.8809 -0.2598 0.042 Uiso 1 1 calc R . . C2 C 0.54488(17) 0.8117(3) -0.3205(2) 0.0494(12) Uani 1 1 d U . . H2 H 0.5834 0.8062 -0.2958 0.059 Uiso 1 1 calc R . . O1S1 O 0.4269(3) 0.6089(4) -0.0870(3) 0.090(2) Uani 0.728(10) 1 d PDU A 1 C1S1 C 0.3822(5) 0.6522(7) -0.0804(4) 0.107(3) Uani 0.728(10) 1 d PDU A 1 H1S1 H 0.3840 0.7219 -0.0844 0.128 Uiso 0.728(10) 1 calc PR A 1 H1S2 H 0.3858 0.6385 -0.0396 0.128 Uiso 0.728(10) 1 calc PR A 1 C1S2 C 0.3267(5) 0.6158(10) -0.1274(6) 0.139(5) Uani 0.728(10) 1 d PDU A 1 H1S3 H 0.3029 0.5962 -0.1085 0.167 Uiso 0.728(10) 1 calc PR A 1 H1S4 H 0.3073 0.6648 -0.1583 0.167 Uiso 0.728(10) 1 calc PR A 1 C1S3 C 0.3411(5) 0.5395(9) -0.1517(5) 0.113(4) Uani 0.728(10) 1 d PDU A 1 H1S5 H 0.3376 0.5544 -0.1923 0.135 Uiso 0.728(10) 1 calc PR A 1 H1S6 H 0.3182 0.4832 -0.1543 0.135 Uiso 0.728(10) 1 calc PR A 1 C1S4 C 0.4046(5) 0.5226(8) -0.1041(7) 0.121(4) Uani 0.728(10) 1 d PDU A 1 H1S7 H 0.4069 0.4860 -0.0690 0.145 Uiso 0.728(10) 1 calc PR A 1 H1S8 H 0.4242 0.4870 -0.1232 0.145 Uiso 0.728(10) 1 calc PR A 1 O1SA O 0.3716(12) 0.5123(15) -0.1421(10) 0.126(8) Uani 0.272(10) 1 d PDU A 2 C1SA C 0.3473(11) 0.579(2) -0.1189(12) 0.104(6) Uani 0.272(10) 1 d PDU A 2 H1S9 H 0.3163 0.5491 -0.1145 0.125 Uiso 0.272(10) 1 calc PR A 2 H1SX H 0.3324 0.6329 -0.1474 0.125 Uiso 0.272(10) 1 calc PR A 2 C1SB C 0.3898(13) 0.6173(15) -0.0570(11) 0.135(9) Uani 0.272(10) 1 d PDU A 2 H1SY H 0.3913 0.6875 -0.0582 0.161 Uiso 0.272(10) 1 calc PR A 2 H1SZ H 0.3784 0.5991 -0.0255 0.161 Uiso 0.272(10) 1 calc PR A 2 C1SC C 0.4421(10) 0.5792(18) -0.0429(13) 0.108(7) Uani 0.272(10) 1 d PDU A 2 H1SA H 0.4607 0.5546 -0.0012 0.129 Uiso 0.272(10) 1 calc PR A 2 H1SB H 0.4663 0.6251 -0.0499 0.129 Uiso 0.272(10) 1 calc PR A 2 C1SD C 0.4214(13) 0.498(2) -0.0910(15) 0.143(11) Uani 0.272(10) 1 d PDU A 2 H1SC H 0.4503 0.4860 -0.1045 0.171 Uiso 0.272(10) 1 calc PR A 2 H1SD H 0.4180 0.4389 -0.0710 0.171 Uiso 0.272(10) 1 calc PR A 2 O2S1 O 0.2620(2) 0.9277(4) -0.5387(3) 0.060(2) Uani 0.560(9) 1 d PDU B 1 C2S1 C 0.2132(3) 0.9589(7) -0.5855(5) 0.060(3) Uani 0.560(9) 1 d PDU B 1 H2S1 H 0.2139 0.9493 -0.6247 0.072 Uiso 0.560(9) 1 calc PR B 1 H2S2 H 0.2074 1.0273 -0.5808 0.072 Uiso 0.560(9) 1 calc PR B 1 C2S2 C 0.1687(4) 0.9006(8) -0.5819(5) 0.047(3) Uani 0.560(9) 1 d PDU B 1 H2S3 H 0.1372 0.8914 -0.6220 0.057 Uiso 0.560(9) 1 calc PR B 1 H2S4 H 0.1554 0.9291 -0.5542 0.057 Uiso 0.560(9) 1 calc PR B 1 C2S3 C 0.2003(5) 0.8067(7) -0.5565(6) 0.062(3) Uani 0.560(9) 1 d PDU B 1 H2S5 H 0.1832 0.7684 -0.5359 0.074 Uiso 0.560(9) 1 calc PR B 1 H2S6 H 0.2032 0.7680 -0.5884 0.074 Uiso 0.560(9) 1 calc PR B 1 C2S4 C 0.2552(5) 0.8459(8) -0.5130(6) 0.060(4) Uani 0.560(9) 1 d PDU B 1 H2S7 H 0.2555 0.8595 -0.4737 0.072 Uiso 0.560(9) 1 calc PR B 1 H2S8 H 0.2850 0.8001 -0.5068 0.072 Uiso 0.560(9) 1 calc PR B 1 O2SA O 0.2452(4) 0.7930(8) -0.5232(5) 0.076(3) Uani 0.440(9) 1 d PDU B 2 C2SA C 0.2531(8) 0.8874(12) -0.5077(8) 0.075(5) Uani 0.440(9) 1 d PDU B 2 H2S9 H 0.2865 0.9111 -0.5101 0.089 Uiso 0.440(9) 1 calc PR B 2 H2SX H 0.2583 0.8959 -0.4658 0.089 Uiso 0.440(9) 1 calc PR B 2 C2SB C 0.2029(7) 0.9422(9) -0.5508(6) 0.075(4) Uani 0.440(9) 1 d PDU B 2 H2SY H 0.1781 0.9570 -0.5322 0.090 Uiso 0.440(9) 1 calc PR B 2 H2SZ H 0.2136 1.0021 -0.5637 0.090 Uiso 0.440(9) 1 calc PR B 2 C2SC C 0.1765(7) 0.8769(11) -0.6014(7) 0.070(4) Uani 0.440(9) 1 d PDU B 2 H2SA H 0.1932 0.8810 -0.6297 0.084 Uiso 0.440(9) 1 calc PR B 2 H2SB H 0.1364 0.8885 -0.6236 0.084 Uiso 0.440(9) 1 calc PR B 2 C2SD C 0.1889(3) 0.7826(5) -0.5686(4) 0.062(4) Uani 0.440(9) 1 d PDU B 2 H2SC H 0.1638 0.7712 -0.5501 0.074 Uiso 0.440(9) 1 calc PR B 2 H2SD H 0.1854 0.7295 -0.5963 0.074 Uiso 0.440(9) 1 calc PR B 2 O1X O -0.0532(3) 0.5221(5) -0.5003(4) 0.115(4) Uani 0.50 1 d PRDU B -1 C1X C -0.0379(3) 0.5260(5) -0.5481(4) 0.103(6) Uani 0.50 1 d PRDU B -1 H1X1 H -0.0332 0.5925 -0.5580 0.124 Uiso 0.50 1 calc PR B -1 H1X2 H -0.0657 0.4943 -0.5847 0.124 Uiso 0.50 1 calc PR B -1 C2X C 0.0201(3) 0.4693(5) -0.5210(4) 0.127(6) Uani 0.50 1 d PRDU B -1 H2X1 H 0.0480 0.5020 -0.5299 0.153 Uiso 0.50 1 calc PR B -1 H2X2 H 0.0156 0.4029 -0.5357 0.153 Uiso 0.50 1 calc PR B -1 C3X C 0.0347(3) 0.4748(5) -0.4501(4) 0.101(5) Uani 0.50 1 d PRDU B -1 H3X1 H 0.0302 0.4125 -0.4342 0.121 Uiso 0.50 1 calc PR B -1 H3X2 H 0.0723 0.4995 -0.4254 0.121 Uiso 0.50 1 calc PR B -1 C4X C -0.0031(3) 0.5350(5) -0.4541(4) 0.066(3) Uani 0.50 1 d PRDU B -1 H4X1 H 0.0097 0.5997 -0.4574 0.079 Uiso 0.50 1 calc PR B -1 H4X2 H -0.0068 0.5324 -0.4162 0.079 Uiso 0.50 1 calc PR B -1 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 Nb1 0.01195(14) 0.01336(14) 0.01401(13) -0.00085(11) 0.00261(11) 0.00006(10) Ag1 0.02020(14) 0.02449(14) 0.03283(15) 0.00076(11) 0.01274(12) 0.00486(10) P1 0.0134(4) 0.0144(4) 0.0156(4) 0.0003(3) 0.0031(3) 0.0010(3) O1 0.0135(11) 0.0145(11) 0.0172(11) -0.0016(9) 0.0037(9) 0.0006(8) O2 0.0169(11) 0.0150(11) 0.0189(11) 0.0010(9) 0.0057(9) 0.0019(9) O3 0.0134(11) 0.0165(11) 0.0174(11) -0.0001(9) 0.0043(9) 0.0003(8) C16 0.0186(17) 0.0221(17) 0.0219(17) -0.0024(14) 0.0072(14) -0.0010(13) N1 0.0149(13) 0.0157(13) 0.0159(13) -0.0030(10) 0.0039(11) -0.0003(10) N4 0.0220(15) 0.0203(15) 0.0399(18) -0.0018(13) 0.0144(14) 0.0011(12) C900 0.0135(15) 0.0188(16) 0.0141(14) 0.0001(12) 0.0041(12) 0.0018(12) C21 0.0150(16) 0.0174(15) 0.0203(16) -0.0031(13) 0.0050(13) -0.0024(12) N3 0.0133(13) 0.0150(13) 0.0169(13) 0.0001(10) 0.0031(11) -0.0002(10) N2 0.0142(13) 0.0155(13) 0.0178(13) -0.0019(11) 0.0037(11) -0.0015(10) C220 0.0195(16) 0.0134(15) 0.0211(16) -0.0022(12) 0.0099(13) -0.0048(12) C52 0.0177(16) 0.0206(16) 0.0158(15) 0.0027(13) 0.0028(13) -0.0006(12) C801 0.0150(15) 0.0174(16) 0.0161(15) -0.0008(12) 0.0015(12) -0.0009(12) C911 0.0183(16) 0.0217(16) 0.0157(15) -0.0050(13) 0.0062(13) 0.0001(12) C32 0.0207(17) 0.0271(18) 0.0226(17) -0.0075(14) 0.0072(14) -0.0038(14) C724 0.0228(18) 0.0253(18) 0.0312(19) 0.0074(15) 0.0094(16) -0.0019(14) C36 0.0232(18) 0.0179(16) 0.0232(17) -0.0051(13) 0.0061(14) -0.0010(13) C701 0.0158(16) 0.0182(15) 0.0143(15) -0.0003(12) 0.0025(12) -0.0003(12) C51 0.0137(15) 0.0212(16) 0.0143(15) 0.0019(13) 0.0012(12) 0.0008(12) C901 0.0186(16) 0.0162(15) 0.0172(15) -0.0013(12) 0.0064(13) -0.0002(12) C223 0.0298(19) 0.0180(17) 0.033(2) -0.0005(15) 0.0152(16) -0.0074(14) C53 0.0243(18) 0.0313(19) 0.0159(16) 0.0020(14) 0.0047(14) -0.0055(14) C55 0.0188(17) 0.038(2) 0.0218(18) 0.0000(15) 0.0062(15) 0.0046(15) C31 0.0151(16) 0.0182(16) 0.0201(16) -0.0075(13) 0.0013(13) -0.0017(12) C721 0.0129(15) 0.0190(16) 0.0210(16) 0.0000(13) 0.0042(13) -0.0021(12) C35 0.029(2) 0.0166(17) 0.036(2) -0.0057(15) 0.0067(16) 0.0014(14) C22 0.0188(16) 0.0155(16) 0.0264(17) -0.0008(13) 0.0094(14) -0.0014(12) C821 0.0205(17) 0.0210(17) 0.0177(15) 0.0029(13) 0.0032(13) 0.0044(13) C15 0.0215(18) 0.0284(19) 0.0338(19) -0.0039(16) 0.0139(15) -0.0008(14) C926 0.0234(17) 0.0166(16) 0.0220(16) 0.0007(13) 0.0100(14) -0.0001(13) C13 0.0268(18) 0.0208(17) 0.0219(17) -0.0039(14) 0.0108(14) -0.0051(14) C924 0.0226(19) 0.0219(18) 0.041(2) 0.0028(16) 0.0122(16) 0.0050(14) C711 0.0198(16) 0.0174(16) 0.0199(16) 0.0060(13) 0.0078(14) 0.0039(12) C722 0.0244(19) 0.0196(17) 0.042(2) -0.0084(16) 0.0137(17) -0.0053(14) C42 0.0217(18) 0.0230(17) 0.0178(16) -0.0044(14) 0.0026(14) -0.0029(13) C800 0.0155(15) 0.0145(15) 0.0180(15) 0.0004(12) 0.0047(12) -0.0026(12) C62 0.0218(17) 0.0217(17) 0.0218(17) 0.0057(14) 0.0048(14) -0.0008(13) C222 0.0238(18) 0.0185(17) 0.0313(19) -0.0039(14) 0.0109(15) -0.0047(13) C816 0.0164(17) 0.0277(18) 0.0229(17) 0.0007(14) 0.0000(14) -0.0012(14) C61 0.0156(16) 0.0155(16) 0.0216(16) 0.0025(13) 0.0039(13) 0.0001(12) C56 0.0201(17) 0.0253(18) 0.0217(17) -0.0040(14) 0.0051(14) 0.0021(13) C916 0.0253(18) 0.0189(16) 0.0281(18) -0.0048(14) 0.0118(15) -0.0008(13) C725 0.0205(17) 0.0230(17) 0.0238(17) 0.0043(14) 0.0087(14) 0.0009(13) C221 0.0245(19) 0.0218(18) 0.037(2) 0.0018(16) 0.0078(16) -0.0005(14) C14 0.0307(19) 0.0281(19) 0.0295(18) -0.0094(15) 0.0191(16) -0.0044(15) C700 0.0126(15) 0.0154(15) 0.0164(15) -0.0004(12) 0.0021(12) 0.0010(11) C41 0.0246(17) 0.0192(16) 0.0156(15) -0.0036(13) 0.0059(13) -0.0014(13) C925 0.0247(18) 0.0211(18) 0.0264(18) 0.0038(14) 0.0078(15) 0.0031(14) C812 0.0199(17) 0.0234(18) 0.0271(18) -0.0027(15) 0.0039(15) 0.0007(13) C12 0.0190(16) 0.0136(15) 0.0232(16) -0.0043(13) 0.0075(13) -0.0033(12) C921 0.0185(16) 0.0118(15) 0.0235(16) -0.0025(13) 0.0071(13) -0.0014(12) C915 0.036(2) 0.0240(19) 0.035(2) -0.0138(16) 0.0174(17) -0.0083(15) C712 0.0282(19) 0.0263(19) 0.0227(17) 0.0025(14) 0.0090(15) 0.0060(15) C54 0.0131(17) 0.046(2) 0.0201(17) 0.0022(16) 0.0038(14) 0.0006(15) C726 0.0194(17) 0.0216(17) 0.0259(18) 0.0000(14) 0.0086(14) -0.0040(13) C824 0.047(3) 0.053(3) 0.0228(19) 0.0153(18) 0.0161(18) 0.018(2) C912 0.0259(18) 0.0233(18) 0.0201(17) -0.0047(14) 0.0072(14) -0.0034(14) C822 0.0242(18) 0.033(2) 0.0216(17) 0.0099(15) 0.0067(15) 0.0037(15) C811 0.0161(16) 0.0224(17) 0.0166(16) -0.0018(13) 0.0020(13) -0.0010(13) C423 0.032(2) 0.0240(18) 0.029(2) -0.0068(15) 0.0061(16) -0.0032(15) C825 0.039(2) 0.044(2) 0.0186(18) 0.0022(17) 0.0029(17) 0.0117(18) C815 0.0202(19) 0.042(2) 0.0276(19) 0.0019(17) 0.0047(16) -0.0085(16) C826 0.0242(19) 0.033(2) 0.0199(17) -0.0001(15) 0.0008(15) 0.0013(15) C913 0.0244(19) 0.035(2) 0.0200(18) -0.0020(16) 0.0006(15) -0.0053(15) C922 0.0249(18) 0.0218(17) 0.0236(17) -0.0040(14) 0.0095(15) 0.0000(14) C623 0.050(3) 0.035(2) 0.0241(19) 0.0056(17) 0.0141(18) 0.0148(19) C422 0.022(2) 0.052(3) 0.032(2) -0.0125(19) 0.0080(17) -0.0147(18) C33 0.0242(19) 0.032(2) 0.030(2) -0.0143(16) 0.0091(16) 0.0026(15) C34 0.025(2) 0.0230(19) 0.044(2) -0.0093(17) 0.0074(17) 0.0046(15) C531 0.0234(19) 0.040(2) 0.028(2) -0.0047(17) 0.0048(16) -0.0144(16) C131 0.041(2) 0.033(2) 0.0207(17) 0.0005(16) 0.0130(16) -0.0004(17) C723 0.0255(19) 0.0165(17) 0.047(2) 0.0068(16) 0.0126(18) -0.0017(14) C622 0.030(2) 0.032(2) 0.0224(18) 0.0042(16) 0.0028(15) -0.0055(16) C716 0.0240(18) 0.0274(19) 0.033(2) 0.0067(16) 0.0121(16) 0.0027(15) C814 0.0125(17) 0.053(2) 0.031(2) -0.0114(18) 0.0051(15) -0.0045(16) C5 0.025(2) 0.027(2) 0.049(2) -0.0057(18) 0.0149(18) -0.0014(15) C3 0.035(2) 0.051(3) 0.065(3) -0.012(2) 0.030(2) 0.005(2) C621 0.029(2) 0.038(2) 0.028(2) 0.0111(17) 0.0058(17) -0.0075(17) C551 0.024(2) 0.061(3) 0.038(2) -0.006(2) 0.0109(18) 0.0152(19) C923 0.0277(19) 0.0236(19) 0.038(2) -0.0071(16) 0.0166(17) 0.0043(15) C914 0.028(2) 0.039(2) 0.0242(19) -0.0122(17) 0.0056(16) -0.0125(16) C715 0.026(2) 0.041(2) 0.045(2) 0.0082(19) 0.0186(18) 0.0063(17) C823 0.035(2) 0.046(2) 0.035(2) 0.0190(19) 0.0178(18) 0.0076(18) C713 0.047(2) 0.034(2) 0.0226(18) 0.0019(16) 0.0152(17) 0.0139(18) C813 0.0203(18) 0.032(2) 0.034(2) -0.0071(16) 0.0025(16) 0.0062(15) C4 0.035(2) 0.033(2) 0.049(3) -0.0118(19) 0.0196(19) -0.0025(18) C714 0.041(2) 0.051(3) 0.039(2) 0.0130(19) 0.027(2) 0.019(2) C151 0.030(2) 0.055(3) 0.046(2) -0.008(2) 0.0215(19) 0.0029(19) C421 0.043(2) 0.035(2) 0.0236(19) -0.0062(17) -0.0035(17) 0.0033(18) C331 0.039(2) 0.049(3) 0.050(3) -0.013(2) 0.022(2) 0.006(2) C351 0.048(3) 0.024(2) 0.061(3) 0.004(2) 0.021(2) 0.0044(19) C1 0.026(2) 0.036(2) 0.040(2) 0.0033(18) 0.0104(17) 0.0021(16) C2 0.024(2) 0.063(3) 0.057(3) -0.004(2) 0.014(2) 0.009(2) O1S1 0.081(4) 0.072(4) 0.083(5) 0.007(3) 0.007(3) -0.006(3) C1S1 0.215(9) 0.068(5) 0.059(5) 0.020(4) 0.081(6) 0.050(6) C1S2 0.116(7) 0.167(11) 0.169(10) 0.120(8) 0.094(7) 0.074(7) C1S3 0.114(8) 0.112(9) 0.076(7) 0.025(6) 0.011(6) -0.071(7) C1S4 0.110(8) 0.049(5) 0.156(11) 0.025(6) 0.015(7) 0.024(5) O1SA 0.163(17) 0.072(10) 0.102(12) 0.019(9) 0.024(11) 0.060(11) C1SA 0.130(12) 0.120(15) 0.097(12) 0.038(11) 0.082(10) 0.029(11) C1SB 0.158(15) 0.153(18) 0.113(15) -0.015(13) 0.079(13) 0.028(14) C1SC 0.163(13) 0.071(13) 0.099(14) 0.011(10) 0.067(11) 0.034(12) C1SD 0.145(16) 0.094(16) 0.130(17) -0.015(13) 0.008(13) 0.051(13) O2S1 0.035(3) 0.082(5) 0.048(4) 0.018(3) 0.005(3) -0.013(3) C2S1 0.030(4) 0.072(6) 0.065(6) 0.022(5) 0.009(4) -0.012(4) C2S2 0.035(4) 0.058(6) 0.053(7) 0.004(5) 0.022(4) -0.011(4) C2S3 0.076(7) 0.042(5) 0.058(7) -0.006(5) 0.021(6) -0.017(5) C2S4 0.080(7) 0.036(6) 0.030(6) -0.002(5) -0.006(5) 0.005(6) O2SA 0.060(6) 0.078(7) 0.062(6) -0.016(5) 0.002(5) 0.009(5) C2SA 0.084(9) 0.089(10) 0.035(7) -0.023(9) 0.012(6) -0.035(8) C2SB 0.110(10) 0.057(6) 0.072(8) -0.002(6) 0.054(7) -0.005(6) C2SC 0.064(9) 0.079(9) 0.053(8) 0.000(6) 0.013(6) -0.002(7) C2SD 0.045(7) 0.072(7) 0.054(8) 0.001(6) 0.008(6) -0.019(6) O1X 0.094(6) 0.078(6) 0.189(10) -0.023(7) 0.077(6) -0.005(5) C1X 0.093(11) 0.091(13) 0.112(7) -0.065(9) 0.034(7) -0.025(9) C2X 0.155(13) 0.089(14) 0.191(13) 0.016(11) 0.125(12) 0.008(10) C3X 0.076(8) 0.084(12) 0.182(11) 0.048(11) 0.092(8) 0.022(8) C4X 0.070(6) 0.031(6) 0.120(8) 0.005(6) 0.064(6) 0.000(5) _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 Nb1 N2 2.021(3) . ? Nb1 N3 2.034(2) . ? Nb1 N1 2.034(2) . ? Nb1 O1 2.097(2) . ? Nb1 O2 2.099(2) . ? Nb1 O3 2.111(2) . ? Ag1 N4 2.162(3) . ? Ag1 P1 2.3678(9) . ? P1 C800 1.847(3) . ? P1 C900 1.852(3) . ? P1 C700 1.854(3) . ? O1 C900 1.326(3) . ? O2 C700 1.322(4) . ? O3 C800 1.321(4) . ? C16 C15 1.389(5) . ? C16 C220 1.400(4) . ? N1 C31 1.440(4) . ? N1 C41 1.492(4) . ? N4 C1 1.333(4) . ? N4 C5 1.340(5) . ? C900 C901 1.377(4) . ? C21 N2 1.492(4) . ? C21 C22 1.541(4) . ? N3 C51 1.441(4) . ? N3 C61 1.486(4) . ? N2 C220 1.441(4) . ? C220 C12 1.395(4) . ? C52 C53 1.388(4) . ? C52 C51 1.389(4) . ? C801 C800 1.370(4) . ? C801 C811 1.477(4) . ? C801 C821 1.492(4) . ? C911 C912 1.399(4) . ? C911 C916 1.405(4) . ? C911 C901 1.487(4) . ? C32 C31 1.387(5) . ? C32 C33 1.399(5) . ? C724 C723 1.373(5) . ? C724 C725 1.389(4) . ? C36 C35 1.393(4) . ? C36 C31 1.394(5) . ? C701 C700 1.362(4) . ? C701 C721 1.487(4) . ? C701 C711 1.490(4) . ? C51 C56 1.397(4) . ? C901 C921 1.491(4) . ? C223 C22 1.534(5) . ? C53 C54 1.393(5) . ? C53 C531 1.511(5) . ? C55 C56 1.387(4) . ? C55 C54 1.395(5) . ? C55 C551 1.511(5) . ? C721 C726 1.392(4) . ? C721 C725 1.412(4) . ? C35 C34 1.388(5) . ? C35 C351 1.513(5) . ? C22 C221 1.531(4) . ? C22 C222 1.539(4) . ? C821 C822 1.385(5) . ? C821 C826 1.402(4) . ? C15 C14 1.401(5) . ? C15 C151 1.510(5) . ? C926 C925 1.390(4) . ? C926 C921 1.401(4) . ? C13 C14 1.387(5) . ? C13 C12 1.400(4) . ? C13 C131 1.519(5) . ? C924 C923 1.374(5) . ? C924 C925 1.386(5) . ? C711 C716 1.398(5) . ? C711 C712 1.401(5) . ? C722 C723 1.378(5) . ? C722 C726 1.393(5) . ? C42 C422 1.525(5) . ? C42 C423 1.536(5) . ? C42 C421 1.540(5) . ? C42 C41 1.539(4) . ? C62 C623 1.508(5) . ? C62 C621 1.528(5) . ? C62 C622 1.537(5) . ? C62 C61 1.548(4) . ? C816 C815 1.382(5) . ? C816 C811 1.401(5) . ? C916 C915 1.387(5) . ? C812 C813 1.385(5) . ? C812 C811 1.407(4) . ? C921 C922 1.397(4) . ? C915 C914 1.384(5) . ? C712 C713 1.400(5) . ? C824 C825 1.374(6) . ? C824 C823 1.384(5) . ? C912 C913 1.383(4) . ? C822 C823 1.390(5) . ? C825 C826 1.378(5) . ? C815 C814 1.378(5) . ? C913 C914 1.384(5) . ? C922 C923 1.390(4) . ? C33 C34 1.386(5) . ? C33 C331 1.503(5) . ? C716 C715 1.384(5) . ? C814 C813 1.381(5) . ? C5 C4 1.378(5) . ? C3 C4 1.363(5) . ? C3 C2 1.382(6) . ? C715 C714 1.389(6) . ? C713 C714 1.362(5) . ? C1 C2 1.384(5) . ? O1S1 C1S4 1.338(11) . ? O1S1 C1S1 1.427(11) . ? C1S1 C1S2 1.524(12) . ? C1S2 C1S3 1.370(11) . ? C1S3 C1S4 1.614(12) . ? O1SA C1SD 1.396(17) . ? O1SA C1SA 1.409(16) . ? C1SA C1SB 1.547(16) . ? C1SB C1SC 1.41(2) . ? C1SC C1SD 1.569(17) . ? O2S1 C2S4 1.366(12) . ? O2S1 C2S1 1.387(9) . ? C2S1 C2S2 1.493(12) . ? C2S2 C2S3 1.548(16) . ? C2S3 C2S4 1.500(13) . ? O2SA C2SA 1.373(13) . ? O2SA C2SD 1.445(11) . ? C2SA C2SB 1.516(17) . ? C2SB C2SC 1.46(2) . ? C2SC C2SD 1.513(16) . ? O1X C4X 1.3439 . ? O1X C1X 1.4197 . ? C1X C2X 1.6179 . ? C2X C3X 1.6226 . ? C3X C4X 1.2983 . ? 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 N2 Nb1 N3 97.98(10) . . ? N2 Nb1 N1 95.78(10) . . ? N3 Nb1 N1 97.34(10) . . ? N2 Nb1 O1 88.72(9) . . ? N3 Nb1 O1 92.58(9) . . ? N1 Nb1 O1 168.42(9) . . ? N2 Nb1 O2 168.97(9) . . ? N3 Nb1 O2 87.13(9) . . ? N1 Nb1 O2 93.24(9) . . ? O1 Nb1 O2 81.26(8) . . ? N2 Nb1 O3 93.01(9) . . ? N3 Nb1 O3 167.30(9) . . ? N1 Nb1 O3 87.82(9) . . ? O1 Nb1 O3 81.28(8) . . ? O2 Nb1 O3 80.98(8) . . ? N4 Ag1 P1 169.13(8) . . ? C800 P1 C900 97.44(14) . . ? C800 P1 C700 99.17(14) . . ? C900 P1 C700 101.53(13) . . ? C800 P1 Ag1 122.23(10) . . ? C900 P1 Ag1 117.19(10) . . ? C700 P1 Ag1 115.52(10) . . ? C900 O1 Nb1 127.63(18) . . ? C700 O2 Nb1 131.42(19) . . ? C800 O3 Nb1 131.53(19) . . ? C15 C16 C220 120.6(3) . . ? C31 N1 C41 111.4(2) . . ? C31 N1 Nb1 122.17(19) . . ? C41 N1 Nb1 126.19(19) . . ? C1 N4 C5 116.6(3) . . ? C1 N4 Ag1 125.4(3) . . ? C5 N4 Ag1 118.0(2) . . ? O1 C900 C901 125.4(3) . . ? O1 C900 P1 114.4(2) . . ? C901 C900 P1 120.2(2) . . ? N2 C21 C22 120.5(3) . . ? C51 N3 C61 111.4(2) . . ? C51 N3 Nb1 120.87(19) . . ? C61 N3 Nb1 127.33(19) . . ? C220 N2 C21 110.8(2) . . ? C220 N2 Nb1 121.45(19) . . ? C21 N2 Nb1 127.4(2) . . ? C12 C220 C16 119.5(3) . . ? C12 C220 N2 120.2(3) . . ? C16 C220 N2 120.3(3) . . ? C53 C52 C51 121.4(3) . . ? C800 C801 C811 120.8(3) . . ? C800 C801 C821 121.6(3) . . ? C811 C801 C821 117.6(3) . . ? C912 C911 C916 117.4(3) . . ? C912 C911 C901 122.2(3) . . ? C916 C911 C901 120.4(3) . . ? C31 C32 C33 120.8(3) . . ? C723 C724 C725 120.6(3) . . ? C35 C36 C31 121.4(3) . . ? C700 C701 C721 122.5(3) . . ? C700 C701 C711 123.2(3) . . ? C721 C701 C711 114.1(3) . . ? C52 C51 C56 119.0(3) . . ? C52 C51 N3 120.6(3) . . ? C56 C51 N3 120.3(3) . . ? C900 C901 C911 123.5(3) . . ? C900 C901 C921 118.8(3) . . ? C911 C901 C921 117.4(3) . . ? C52 C53 C54 118.4(3) . . ? C52 C53 C531 120.5(3) . . ? C54 C53 C531 121.1(3) . . ? C56 C55 C54 118.8(3) . . ? C56 C55 C551 120.5(3) . . ? C54 C55 C551 120.7(3) . . ? C32 C31 C36 119.0(3) . . ? C32 C31 N1 121.1(3) . . ? C36 C31 N1 119.9(3) . . ? C726 C721 C725 117.2(3) . . ? C726 C721 C701 123.0(3) . . ? C725 C721 C701 119.8(3) . . ? C34 C35 C36 118.2(4) . . ? C34 C35 C351 121.8(3) . . ? C36 C35 C351 120.0(3) . . ? C221 C22 C223 110.8(3) . . ? C221 C22 C222 109.6(3) . . ? C223 C22 C222 106.3(3) . . ? C221 C22 C21 110.6(3) . . ? C223 C22 C21 113.8(3) . . ? C222 C22 C21 105.4(3) . . ? C822 C821 C826 117.5(3) . . ? C822 C821 C801 121.6(3) . . ? C826 C821 C801 120.9(3) . . ? C16 C15 C14 119.1(3) . . ? C16 C15 C151 120.0(3) . . ? C14 C15 C151 120.8(3) . . ? C925 C926 C921 121.1(3) . . ? C14 C13 C12 119.0(3) . . ? C14 C13 C131 121.9(3) . . ? C12 C13 C131 119.1(3) . . ? C923 C924 C925 119.7(3) . . ? C716 C711 C712 117.6(3) . . ? C716 C711 C701 121.1(3) . . ? C712 C711 C701 120.6(3) . . ? C723 C722 C726 120.8(3) . . ? C422 C42 C423 110.4(3) . . ? C422 C42 C421 109.4(3) . . ? C423 C42 C421 107.4(3) . . ? C422 C42 C41 109.8(3) . . ? C423 C42 C41 114.2(3) . . ? C421 C42 C41 105.4(3) . . ? O3 C800 C801 125.2(3) . . ? O3 C800 P1 112.6(2) . . ? C801 C800 P1 121.6(2) . . ? C623 C62 C621 110.6(3) . . ? C623 C62 C622 110.4(3) . . ? C621 C62 C622 106.5(3) . . ? C623 C62 C61 110.3(3) . . ? C621 C62 C61 105.5(3) . . ? C622 C62 C61 113.4(3) . . ? C815 C816 C811 121.7(3) . . ? N3 C61 C62 118.7(3) . . ? C55 C56 C51 120.8(3) . . ? C915 C916 C911 121.1(3) . . ? C724 C725 C721 121.0(3) . . ? C13 C14 C15 121.3(3) . . ? O2 C700 C701 124.5(3) . . ? O2 C700 P1 113.7(2) . . ? C701 C700 P1 121.5(2) . . ? N1 C41 C42 118.4(3) . . ? C924 C925 C926 119.7(3) . . ? C813 C812 C811 121.2(3) . . ? C220 C12 C13 120.6(3) . . ? C922 C921 C926 118.3(3) . . ? C922 C921 C901 122.5(3) . . ? C926 C921 C901 119.2(3) . . ? C914 C915 C916 120.3(3) . . ? C713 C712 C711 120.5(3) . . ? C53 C54 C55 121.5(3) . . ? C722 C726 C721 121.0(3) . . ? C825 C824 C823 119.9(4) . . ? C913 C912 C911 121.3(3) . . ? C821 C822 C823 121.3(3) . . ? C816 C811 C812 116.8(3) . . ? C816 C811 C801 120.9(3) . . ? C812 C811 C801 122.4(3) . . ? C824 C825 C826 120.0(4) . . ? C814 C815 C816 120.4(4) . . ? C825 C826 C821 121.5(4) . . ? C912 C913 C914 120.5(3) . . ? C923 C922 C921 120.0(3) . . ? C34 C33 C32 118.7(3) . . ? C34 C33 C331 121.3(3) . . ? C32 C33 C331 120.0(4) . . ? C33 C34 C35 121.9(3) . . ? C724 C723 C722 119.4(3) . . ? C715 C716 C711 121.4(4) . . ? C815 C814 C813 119.4(3) . . ? N4 C5 C4 123.9(4) . . ? C4 C3 C2 119.7(4) . . ? C924 C923 C922 121.1(3) . . ? C915 C914 C913 119.4(3) . . ? C716 C715 C714 120.0(4) . . ? C824 C823 C822 119.9(4) . . ? C714 C713 C712 120.7(4) . . ? C814 C813 C812 120.5(3) . . ? C3 C4 C5 118.2(4) . . ? C713 C714 C715 119.8(4) . . ? N4 C1 C2 123.6(4) . . ? C3 C2 C1 118.0(4) . . ? C1S4 O1S1 C1S1 98.0(9) . . ? O1S1 C1S1 C1S2 111.6(7) . . ? C1S3 C1S2 C1S1 102.9(7) . . ? C1S2 C1S3 C1S4 102.3(8) . . ? O1S1 C1S4 C1S3 106.4(7) . . ? C1SD O1SA C1SA 99.6(17) . . ? O1SA C1SA C1SB 111.1(15) . . ? C1SC C1SB C1SA 109.7(14) . . ? C1SB C1SC C1SD 96.3(13) . . ? O1SA C1SD C1SC 117.1(16) . . ? C2S4 O2S1 C2S1 112.3(7) . . ? O2S1 C2S1 C2S2 105.7(7) . . ? C2S1 C2S2 C2S3 100.2(8) . . ? C2S4 C2S3 C2S2 99.8(7) . . ? O2S1 C2S4 C2S3 105.7(8) . . ? C2SA O2SA C2SD 107.2(11) . . ? O2SA C2SA C2SB 108.4(11) . . ? C2SC C2SB C2SA 103.2(10) . . ? C2SB C2SC C2SD 100.5(10) . . ? O2SA C2SD C2SC 103.6(9) . . ? C4X O1X C1X 98.4 . . ? O1X C1X C2X 103.0 . . ? C1X C2X C3X 98.6 . . ? C4X C3X C2X 98.3 . . ? C3X C4X O1X 116.1 . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.438 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.103 data_10219 _database_code_depnum_ccdc_archive 'CCDC 789237' #TrackingRef '2142_web_deposit_cif_file_0_SidCreutz_1281724789.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Rh(eta(6)-Ph,eta(2)-Ph'-P(C[CPh2]O)3Nb(N[Np]Ar)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92.5 H122 N3 Nb O5 P Rh' _chemical_formula_weight 1582.75 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.3525(16) _cell_length_b 15.0941(10) _cell_length_c 25.0969(17) _cell_angle_alpha 90.00 _cell_angle_beta 115.1470(10) _cell_angle_gamma 90.00 _cell_volume 8007.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9580 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.98 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3388 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7842 _exptl_absorpt_correction_T_max 0.8828 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 214390 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 30.03 _reflns_number_total 23398 _reflns_number_gt 18910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+14.4919P] 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 23398 _refine_ls_number_parameters 985 _refine_ls_number_restraints 280 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.818667(8) 0.946732(11) 0.249893(7) 0.01444(4) Uani 1 1 d . . . Nb1 Nb 0.992240(9) 0.741718(12) 0.206115(8) 0.01202(5) Uani 1 1 d . . . P1 P 0.86737(3) 0.85585(4) 0.21656(2) 0.01278(10) Uani 1 1 d . . . O3 O 0.89515(7) 0.72260(10) 0.16515(7) 0.0147(3) Uani 1 1 d . . . O1 O 0.96327(8) 0.87690(10) 0.18730(7) 0.0155(3) Uani 1 1 d . . . O2 O 0.97028(7) 0.75663(10) 0.27969(7) 0.0149(3) Uani 1 1 d . . . C8 C 0.92031(10) 0.79427(13) 0.28131(10) 0.0140(4) Uani 1 1 d . . . N3 N 0.99433(9) 0.72674(12) 0.12674(8) 0.0150(3) Uani 1 1 d . . . N1 N 1.08005(9) 0.79307(12) 0.24956(8) 0.0147(3) Uani 1 1 d . . . C7 C 0.92146(10) 0.92240(14) 0.19815(9) 0.0139(4) Uani 1 1 d . . . N2 N 1.01242(9) 0.61398(12) 0.23313(8) 0.0141(3) Uani 1 1 d . . . C9 C 0.84452(10) 0.76733(14) 0.16033(9) 0.0138(4) Uani 1 1 d . . . C423 C 0.96312(13) 0.42776(16) 0.25624(12) 0.0259(5) Uani 1 1 d . . . H42A H 0.9380 0.3838 0.2657 0.039 Uiso 1 1 calc R . . H42B H 1.0055 0.4040 0.2662 0.039 Uiso 1 1 calc R . . H42C H 0.9424 0.4414 0.2141 0.039 Uiso 1 1 calc R . . C816 C 0.78009(11) 0.82694(15) 0.27582(10) 0.0172(4) Uani 1 1 d . . . H816 H 0.7745 0.7973 0.2405 0.021 Uiso 1 1 calc R . . C711 C 0.86745(11) 1.04627(14) 0.22045(10) 0.0166(4) Uani 1 1 d . . . C41 C 1.01898(11) 0.57780(14) 0.29064(10) 0.0159(4) Uani 1 1 d . . . H41A H 1.0205 0.6287 0.3161 0.019 Uiso 1 1 calc R . . H41B H 1.0605 0.5477 0.3092 0.019 Uiso 1 1 calc R . . C31 C 1.03261(11) 0.55051(14) 0.20161(10) 0.0161(4) Uani 1 1 d . . . C911 C 0.73220(10) 0.81197(14) 0.11329(10) 0.0152(4) Uani 1 1 d . . . C21 C 1.09986(11) 0.88611(14) 0.24828(10) 0.0166(4) Uani 1 1 d . . . H21A H 1.0638 0.9179 0.2177 0.020 Uiso 1 1 calc R . . H21B H 1.1345 0.8856 0.2354 0.020 Uiso 1 1 calc R . . C61 C 0.94261(11) 0.69088(14) 0.07266(10) 0.0163(4) Uani 1 1 d . . . H61A H 0.9107 0.6646 0.0842 0.020 Uiso 1 1 calc R . . H61B H 0.9605 0.6418 0.0583 0.020 Uiso 1 1 calc R . . C220 C 1.12245(11) 0.94086(15) 0.30568(10) 0.0186(4) Uani 1 1 d . . . C80 C 0.90097(10) 0.79408(14) 0.32589(10) 0.0144(4) Uani 1 1 d . . . C712 C 0.88837(12) 1.06541(15) 0.28178(11) 0.0196(4) Uani 1 1 d . . . H712 H 0.9323 1.0660 0.3073 0.024 Uiso 1 1 calc R . . C12 C 1.13812(11) 0.70192(15) 0.33709(10) 0.0171(4) Uani 1 1 d . . . H12 H 1.1051 0.7118 0.3490 0.021 Uiso 1 1 calc R . . C32 C 1.09570(11) 0.52219(15) 0.22501(11) 0.0190(4) Uani 1 1 d . . . H32 H 1.1252 0.5447 0.2618 0.023 Uiso 1 1 calc R . . C912 C 0.68339(11) 0.79239(15) 0.12971(10) 0.0183(4) Uani 1 1 d . . . H912 H 0.6831 0.7369 0.1474 0.022 Uiso 1 1 calc R . . C90 C 0.78379(11) 0.74715(14) 0.12236(10) 0.0150(4) Uani 1 1 d . . . C811 C 0.84309(11) 0.84534(15) 0.31990(10) 0.0161(4) Uani 1 1 d . . . C926 C 0.80684(12) 0.59422(15) 0.09378(11) 0.0186(4) Uani 1 1 d . . . H926 H 0.8458 0.5928 0.1280 0.022 Uiso 1 1 calc R . . C821 C 0.93345(11) 0.74362(14) 0.38140(10) 0.0157(4) Uani 1 1 d . . . C825 C 0.92578(12) 0.65688(17) 0.45977(11) 0.0228(5) Uani 1 1 d . . . H825 H 0.9006 0.6309 0.4769 0.027 Uiso 1 1 calc R . . C70 C 0.91358(11) 1.01280(14) 0.19784(10) 0.0163(4) Uani 1 1 d . . . C51 C 1.05141(11) 0.74222(15) 0.11945(10) 0.0159(4) Uani 1 1 d . . . C16 C 1.18180(11) 0.72416(16) 0.26698(11) 0.0197(4) Uani 1 1 d . . . H16 H 1.1784 0.7479 0.2307 0.024 Uiso 1 1 calc R . . C11 C 1.13327(10) 0.73834(14) 0.28443(10) 0.0154(4) Uani 1 1 d . . . C36 C 0.98976(12) 0.51632(15) 0.14771(10) 0.0184(4) Uani 1 1 d . . . H36 H 0.9467 0.5343 0.1321 0.022 Uiso 1 1 calc R . . C721 C 0.94998(11) 1.07699(15) 0.18069(10) 0.0180(4) Uani 1 1 d . . . C420 C 0.96847(11) 0.51253(15) 0.29175(11) 0.0180(4) Uani 1 1 d . . . C714 C 0.77832(12) 1.08634(16) 0.26637(12) 0.0231(5) Uani 1 1 d . . . H714 H 0.7485 1.0939 0.2825 0.028 Uiso 1 1 calc R . . C716 C 0.80136(11) 1.05747(14) 0.18244(11) 0.0188(4) Uani 1 1 d . . . H716 H 0.7872 1.0507 0.1411 0.023 Uiso 1 1 calc R . . C916 C 0.73007(11) 0.89251(15) 0.08508(10) 0.0180(4) Uani 1 1 d . . . H916 H 0.7622 0.9063 0.0727 0.022 Uiso 1 1 calc R . . C822 C 0.99928(11) 0.73319(16) 0.40920(10) 0.0189(4) Uani 1 1 d . . . H822 H 1.0248 0.7590 0.3922 0.023 Uiso 1 1 calc R . . C914 C 0.63471(12) 0.93397(16) 0.09342(11) 0.0217(5) Uani 1 1 d . . . H914 H 0.6023 0.9759 0.0877 0.026 Uiso 1 1 calc R . . C34 C 1.07225(13) 0.42936(16) 0.14040(12) 0.0239(5) Uani 1 1 d . . . H34 H 1.0859 0.3887 0.1193 0.029 Uiso 1 1 calc R . . C35 C 1.00892(13) 0.45620(15) 0.11631(11) 0.0221(5) Uani 1 1 d . . . C56 C 1.08579(11) 0.67082(15) 0.11219(10) 0.0190(4) Uani 1 1 d . . . H56 H 1.0707 0.6121 0.1111 0.023 Uiso 1 1 calc R . . C223 C 1.07415(12) 0.93574(17) 0.33205(11) 0.0218(5) Uani 1 1 d . . . H22A H 1.0716 0.8747 0.3441 0.033 Uiso 1 1 calc R . . H22B H 1.0326 0.9544 0.3025 0.033 Uiso 1 1 calc R . . H22C H 1.0874 0.9749 0.3664 0.033 Uiso 1 1 calc R . . C915 C 0.68134(11) 0.95302(16) 0.07493(11) 0.0209(5) Uani 1 1 d . . . H915 H 0.6802 1.0073 0.0553 0.025 Uiso 1 1 calc R . . C715 C 0.75722(12) 1.07827(16) 0.20506(11) 0.0217(5) Uani 1 1 d . . . H715 H 0.7139 1.0867 0.1794 0.026 Uiso 1 1 calc R . . C53 C 1.12915(12) 0.84408(17) 0.11389(11) 0.0227(5) Uani 1 1 d . . . C921 C 0.76682(11) 0.66832(15) 0.08325(10) 0.0167(4) Uani 1 1 d . . . C713 C 0.84354(13) 1.08332(16) 0.30400(11) 0.0225(5) Uani 1 1 d . . . H713 H 0.8574 1.0935 0.3450 0.027 Uiso 1 1 calc R . . C812 C 0.84713(12) 0.89264(16) 0.37158(11) 0.0208(5) Uani 1 1 d . . . H812 H 0.8876 0.9064 0.4017 0.025 Uiso 1 1 calc R . . C620 C 0.90711(11) 0.75355(15) 0.01975(10) 0.0183(4) Uani 1 1 d . . . C222 C 1.18859(12) 0.91429(18) 0.35143(11) 0.0244(5) Uani 1 1 d . . . H22D H 1.2040 0.9585 0.3830 0.037 Uiso 1 1 calc R . . H22E H 1.2176 0.9111 0.3325 0.037 Uiso 1 1 calc R . . H22F H 1.1864 0.8563 0.3680 0.037 Uiso 1 1 calc R . . C826 C 0.89719(11) 0.70461(16) 0.40784(10) 0.0191(4) Uani 1 1 d . . . H826 H 0.8525 0.7111 0.3899 0.023 Uiso 1 1 calc R . . C623 C 0.88058(13) 0.83379(17) 0.03882(11) 0.0261(5) Uani 1 1 d . . . H62A H 0.9154 0.8671 0.0688 0.039 Uiso 1 1 calc R . . H62B H 0.8514 0.8138 0.0551 0.039 Uiso 1 1 calc R . . H62C H 0.8579 0.8720 0.0047 0.039 Uiso 1 1 calc R . . C922 C 0.70887(12) 0.66582(17) 0.03317(11) 0.0217(5) Uani 1 1 d . . . H922 H 0.6803 0.7141 0.0253 0.026 Uiso 1 1 calc R . . C726 C 0.97844(12) 1.05217(15) 0.14354(11) 0.0212(5) Uani 1 1 d . . . H726 H 0.9740 0.9930 0.1294 0.025 Uiso 1 1 calc R . . C54 C 1.16338(12) 0.77198(18) 0.10789(12) 0.0244(5) Uani 1 1 d . . . H54 H 1.2019 0.7821 0.1047 0.029 Uiso 1 1 calc R . . C913 C 0.63545(12) 0.85302(17) 0.12044(11) 0.0221(5) Uani 1 1 d . . . H913 H 0.6030 0.8393 0.1325 0.027 Uiso 1 1 calc R . . C422 C 0.90365(12) 0.55711(17) 0.27027(12) 0.0235(5) Uani 1 1 d . . . H42D H 0.8909 0.5789 0.2300 0.035 Uiso 1 1 calc R . . H42E H 0.9061 0.6069 0.2962 0.035 Uiso 1 1 calc R . . H42F H 0.8725 0.5141 0.2708 0.035 Uiso 1 1 calc R . . C52 C 1.07318(12) 0.82841(15) 0.11954(10) 0.0191(4) Uani 1 1 d . . . H52 H 1.0495 0.8771 0.1235 0.023 Uiso 1 1 calc R . . C925 C 0.79020(12) 0.52323(15) 0.05491(11) 0.0215(5) Uani 1 1 d . . . H925 H 0.8182 0.4744 0.0626 0.026 Uiso 1 1 calc R . . C531 C 1.15182(15) 0.93808(18) 0.11425(14) 0.0316(6) Uani 1 1 d . . . H53A H 1.1425 0.9736 0.1423 0.047 Uiso 1 1 calc R . . H53B H 1.1301 0.9636 0.0748 0.047 Uiso 1 1 calc R . . H53C H 1.1976 0.9379 0.1259 0.047 Uiso 1 1 calc R . . C724 C 1.02015(13) 1.19930(17) 0.14741(13) 0.0277(5) Uani 1 1 d . . . H724 H 1.0443 1.2402 0.1366 0.033 Uiso 1 1 calc R . . C15 C 1.23512(12) 0.67559(17) 0.30227(12) 0.0234(5) Uani 1 1 d . . . C622 C 0.85224(13) 0.69834(18) -0.02467(11) 0.0261(5) Uani 1 1 d . . . H62D H 0.8286 0.7339 -0.0599 0.039 Uiso 1 1 calc R . . H62E H 0.8240 0.6805 -0.0068 0.039 Uiso 1 1 calc R . . H62F H 0.8692 0.6454 -0.0355 0.039 Uiso 1 1 calc R . . C14 C 1.23876(12) 0.63901(17) 0.35463(12) 0.0238(5) Uani 1 1 d . . . H14 H 1.2749 0.6051 0.3785 0.029 Uiso 1 1 calc R . . C13 C 1.19031(12) 0.65130(16) 0.37272(11) 0.0207(4) Uani 1 1 d . . . C33 C 1.11563(12) 0.46087(16) 0.19447(12) 0.0230(5) Uani 1 1 d . . . C551 C 1.17957(14) 0.60800(19) 0.09972(14) 0.0304(6) Uani 1 1 d . . . H55A H 1.2224 0.6093 0.1315 0.046 Uiso 1 1 calc R . . H55B H 1.1818 0.6123 0.0617 0.046 Uiso 1 1 calc R . . H55C H 1.1588 0.5524 0.1015 0.046 Uiso 1 1 calc R . . C823 C 1.02772(12) 0.68549(18) 0.46141(11) 0.0246(5) Uani 1 1 d . . . H823 H 1.0724 0.6792 0.4798 0.030 Uiso 1 1 calc R . . C55 C 1.14207(12) 0.68524(17) 0.10657(11) 0.0216(5) Uani 1 1 d . . . C621 C 0.94805(13) 0.78485(19) -0.01091(12) 0.0275(5) Uani 1 1 d . . . H62G H 0.9691 0.7337 -0.0188 0.041 Uiso 1 1 calc R . . H62H H 0.9800 0.8268 0.0146 0.041 Uiso 1 1 calc R . . H62I H 0.9212 0.8140 -0.0481 0.041 Uiso 1 1 calc R . . C351 C 0.96188(15) 0.42142(19) 0.05745(12) 0.0310(6) Uani 1 1 d . . . H35A H 0.9807 0.4233 0.0292 0.047 Uiso 1 1 calc R . . H35B H 0.9237 0.4583 0.0430 0.047 Uiso 1 1 calc R . . H35C H 0.9507 0.3602 0.0620 0.047 Uiso 1 1 calc R . . C815 C 0.72607(12) 0.85315(17) 0.28499(11) 0.0222(5) Uani 1 1 d . . . H815 H 0.6848 0.8397 0.2560 0.027 Uiso 1 1 calc R . . C722 C 0.95690(13) 1.16588(16) 0.19985(11) 0.0234(5) Uani 1 1 d . . . H722 H 0.9374 1.1852 0.2242 0.028 Uiso 1 1 calc R . . C924 C 0.73326(14) 0.52273(17) 0.00518(11) 0.0260(5) Uani 1 1 d . . . H924 H 0.7224 0.4742 -0.0214 0.031 Uiso 1 1 calc R . . C824 C 0.99123(13) 0.64692(17) 0.48685(11) 0.0258(5) Uani 1 1 d . . . H824 H 1.0108 0.6141 0.5224 0.031 Uiso 1 1 calc R . . C725 C 1.01279(13) 1.11218(16) 0.12711(12) 0.0253(5) Uani 1 1 d . . . H725 H 1.0315 1.0939 0.1019 0.030 Uiso 1 1 calc R . . C814 C 0.73298(13) 0.89709(19) 0.33464(12) 0.0265(5) Uani 1 1 d . . . H814 H 0.6967 0.9138 0.3402 0.032 Uiso 1 1 calc R . . C723 C 0.99187(14) 1.22562(17) 0.18349(13) 0.0298(6) Uani 1 1 d . . . H723 H 0.9964 1.2850 0.1972 0.036 Uiso 1 1 calc R . . C421 C 0.99159(14) 0.48762(18) 0.35712(12) 0.0271(5) Uani 1 1 d . . . H42G H 0.9626 0.4442 0.3614 0.041 Uiso 1 1 calc R . . H42H H 0.9928 0.5408 0.3800 0.041 Uiso 1 1 calc R . . H42I H 1.0341 0.4620 0.3716 0.041 Uiso 1 1 calc R . . C331 C 1.18400(14) 0.4311(2) 0.22069(15) 0.0359(7) Uani 1 1 d . . . H33A H 1.1920 0.3920 0.2543 0.054 Uiso 1 1 calc R . . H33B H 1.2117 0.4830 0.2339 0.054 Uiso 1 1 calc R . . H33C H 1.1925 0.3990 0.1909 0.054 Uiso 1 1 calc R . . C221 C 1.12626(15) 1.03698(17) 0.28745(12) 0.0309(6) Uani 1 1 d . . . H22G H 1.0840 1.0573 0.2604 0.046 Uiso 1 1 calc R . . H22H H 1.1546 1.0402 0.2678 0.046 Uiso 1 1 calc R . . H22I H 1.1427 1.0748 0.3225 0.046 Uiso 1 1 calc R . . C813 C 0.79449(13) 0.91812(18) 0.37827(11) 0.0252(5) Uani 1 1 d . . . H813 H 0.7989 0.9502 0.4124 0.030 Uiso 1 1 calc R . . C923 C 0.69235(14) 0.59386(18) -0.00539(11) 0.0273(5) Uani 1 1 d . . . H923 H 0.6529 0.5936 -0.0391 0.033 Uiso 1 1 calc R . . C131 C 1.19518(14) 0.6142(2) 0.43020(12) 0.0311(6) Uani 1 1 d . . . H13A H 1.2104 0.6604 0.4605 0.047 Uiso 1 1 calc R . . H13B H 1.2249 0.5644 0.4421 0.047 Uiso 1 1 calc R . . H13C H 1.1535 0.5936 0.4254 0.047 Uiso 1 1 calc R . . C151 C 1.28861(14) 0.6633(2) 0.28436(15) 0.0357(7) Uani 1 1 d . . . H15A H 1.2717 0.6627 0.2413 0.054 Uiso 1 1 calc R . . H15B H 1.3101 0.6070 0.3001 0.054 Uiso 1 1 calc R . . H15C H 1.3188 0.7122 0.3000 0.054 Uiso 1 1 calc R . . O1S O 1.24661(13) 0.87205(18) -0.04386(11) 0.0511(7) Uani 1 1 d DU . . C11S C 1.2383(2) 0.7835(2) -0.0653(2) 0.0542(10) Uani 1 1 d DU . . H11A H 1.2795 0.7527 -0.0517 0.065 Uiso 1 1 calc R . . H11B H 1.2176 0.7827 -0.1089 0.065 Uiso 1 1 calc R . . C12S C 1.1967(2) 0.7397(2) -0.0406(2) 0.0539(10) Uani 1 1 d DU . . H12A H 1.1714 0.6913 -0.0665 0.065 Uiso 1 1 calc R . . H12B H 1.2222 0.7156 -0.0007 0.065 Uiso 1 1 calc R . . C13S C 1.15552(16) 0.8136(2) -0.03858(15) 0.0410(7) Uani 1 1 d DU . . H13D H 1.1411 0.8039 -0.0072 0.049 Uiso 1 1 calc R . . H13E H 1.1181 0.8201 -0.0768 0.049 Uiso 1 1 calc R . . C14S C 1.1977(2) 0.8930(3) -0.02561(19) 0.0557(10) Uani 1 1 d DU . . H14A H 1.1733 0.9452 -0.0474 0.067 Uiso 1 1 calc R . . H14B H 1.2163 0.9065 0.0170 0.067 Uiso 1 1 calc R . . O2S O 0.9737(3) 1.0584(4) 0.4261(2) 0.0555(14) Uani 0.50 1 d PDU A -1 C21S C 0.9732(4) 1.1051(5) 0.4753(3) 0.0496(17) Uani 0.50 1 d PDU A -1 H21C H 0.9347 1.1418 0.4638 0.060 Uiso 0.50 1 calc PR A -1 H21D H 1.0110 1.1432 0.4940 0.060 Uiso 0.50 1 calc PR A -1 C22S C 0.9739(4) 1.0291(6) 0.5157(4) 0.053(2) Uani 0.50 1 d PDU A -1 H22J H 0.9938 1.0482 0.5574 0.063 Uiso 0.50 1 calc PR A -1 H22K H 0.9304 1.0085 0.5060 0.063 Uiso 0.50 1 calc PR A -1 C23S C 1.0113(4) 0.9581(6) 0.5052(4) 0.0522(18) Uani 0.50 1 d PDU A -1 H23A H 0.9892 0.9004 0.4993 0.063 Uiso 0.50 1 calc PR A -1 H23B H 1.0535 0.9528 0.5388 0.063 Uiso 0.50 1 calc PR A -1 C24S C 1.0175(4) 0.9865(5) 0.4495(4) 0.0525(19) Uani 0.50 1 d PDU A -1 H24A H 1.0612 1.0062 0.4589 0.063 Uiso 0.50 1 calc PR A -1 H24B H 1.0066 0.9370 0.4210 0.063 Uiso 0.50 1 calc PR A -1 O3S O 1.1591(4) 1.1769(6) 0.4211(4) 0.106(3) Uani 0.491(6) 1 d PDU B 1 C31S C 1.1674(2) 1.2512(3) 0.3915(2) 0.128(5) Uani 0.491(6) 1 d PDU B 1 H31A H 1.1930 1.2393 0.3694 0.154 Uiso 0.491(6) 1 calc PR B 1 H31B H 1.1831 1.3042 0.4168 0.154 Uiso 0.491(6) 1 calc PR B 1 C32S C 1.0916(2) 1.2519(3) 0.3509(2) 0.115(5) Uani 0.491(6) 1 d PRDU B 1 H32A H 1.0781 1.3069 0.3272 0.138 Uiso 0.491(6) 1 calc PR B 1 H32B H 1.0782 1.2000 0.3243 0.138 Uiso 0.491(6) 1 calc PR B 1 C33S C 1.0694(2) 1.2480(3) 0.3910(2) 0.153(6) Uani 0.491(6) 1 d PRDU B 1 H33D H 1.0229 1.2401 0.3713 0.184 Uiso 0.491(6) 1 calc PR B 1 H33E H 1.0781 1.3049 0.4128 0.184 Uiso 0.491(6) 1 calc PR B 1 C34S C 1.0954(2) 1.1802(3) 0.4303(2) 0.096(3) Uani 0.491(6) 1 d PRDU B 1 H34A H 1.0706 1.1247 0.4182 0.116 Uiso 0.491(6) 1 calc PR B 1 H34B H 1.1029 1.1962 0.4710 0.116 Uiso 0.491(6) 1 calc PR B 1 C41P C 1.1680(2) 1.3802(3) 0.3665(2) 0.067(3) Uani 0.509(6) 1 d PRDU B 2 H41C H 1.1360 1.4252 0.3619 0.101 Uiso 0.509(6) 1 calc PR B 2 H41D H 1.1972 1.4032 0.3511 0.101 Uiso 0.509(6) 1 calc PR B 2 H41E H 1.1916 1.3657 0.4083 0.101 Uiso 0.509(6) 1 calc PR B 2 C42P C 1.1361(2) 1.2981(3) 0.3330(2) 0.093(3) Uani 0.509(6) 1 d PRDU B 2 H42J H 1.1146 1.3146 0.2909 0.111 Uiso 0.509(6) 1 calc PR B 2 H42K H 1.1699 1.2555 0.3368 0.111 Uiso 0.509(6) 1 calc PR B 2 C43P C 1.0946(2) 1.2549(3) 0.3459(2) 0.167(7) Uani 0.509(6) 1 d PRDU B 2 H43A H 1.0775 1.2044 0.3184 0.200 Uiso 0.509(6) 1 calc PR B 2 H43B H 1.0590 1.2948 0.3407 0.200 Uiso 0.509(6) 1 calc PR B 2 C44P C 1.1281(2) 1.2161(3) 0.4169(2) 0.106(4) Uani 0.509(6) 1 d PRDU B 2 H44A H 1.1405 1.2624 0.4477 0.127 Uiso 0.509(6) 1 calc PR B 2 H44B H 1.1619 1.1714 0.4252 0.127 Uiso 0.509(6) 1 calc PR B 2 C45P C 1.0404(2) 1.1659(3) 0.3926(2) 0.280(15) Uani 0.509(6) 1 d PRDU B 2 H45A H 1.0146 1.1788 0.3509 0.421 Uiso 0.509(6) 1 calc PR B 2 H45B H 1.0209 1.1928 0.4164 0.421 Uiso 0.509(6) 1 calc PR B 2 H45C H 1.0432 1.1016 0.3986 0.421 Uiso 0.509(6) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01630(8) 0.01395(8) 0.01393(8) -0.00139(6) 0.00726(6) 0.00261(6) Nb1 0.01380(9) 0.01127(8) 0.01226(9) -0.00043(6) 0.00675(7) 0.00056(6) P1 0.0153(2) 0.0117(2) 0.0122(2) -0.00089(18) 0.0068(2) 0.00086(18) O3 0.0147(7) 0.0145(7) 0.0156(7) -0.0023(5) 0.0070(6) 0.0011(5) O1 0.0183(8) 0.0138(7) 0.0173(8) -0.0004(6) 0.0102(6) 0.0013(6) O2 0.0149(7) 0.0161(7) 0.0150(7) 0.0004(6) 0.0076(6) 0.0020(6) C8 0.0153(10) 0.0110(9) 0.0151(10) -0.0002(7) 0.0058(8) 0.0008(7) N3 0.0157(9) 0.0156(8) 0.0152(9) -0.0011(7) 0.0079(7) 0.0001(7) N1 0.0168(9) 0.0142(8) 0.0142(8) 0.0001(6) 0.0076(7) -0.0004(7) C7 0.0152(10) 0.0132(9) 0.0133(9) -0.0002(7) 0.0060(8) -0.0001(7) N2 0.0148(8) 0.0145(8) 0.0149(9) -0.0012(6) 0.0080(7) 0.0000(6) C9 0.0174(10) 0.0134(9) 0.0127(9) -0.0007(7) 0.0084(8) 0.0010(7) C423 0.0340(14) 0.0194(11) 0.0315(14) -0.0056(10) 0.0210(12) -0.0068(10) C816 0.0180(10) 0.0194(10) 0.0150(10) 0.0001(8) 0.0079(9) -0.0004(8) C711 0.0196(10) 0.0118(9) 0.0189(10) -0.0011(7) 0.0088(9) -0.0001(7) C41 0.0179(10) 0.0155(9) 0.0158(10) 0.0019(7) 0.0087(8) 0.0009(8) C31 0.0211(11) 0.0117(9) 0.0197(11) 0.0010(8) 0.0128(9) 0.0011(8) C911 0.0154(10) 0.0155(9) 0.0130(9) -0.0012(7) 0.0044(8) 0.0002(7) C21 0.0191(10) 0.0157(10) 0.0160(10) -0.0005(8) 0.0084(9) -0.0033(8) C61 0.0203(11) 0.0151(9) 0.0144(10) -0.0018(7) 0.0083(9) 0.0003(8) C220 0.0223(11) 0.0168(10) 0.0173(10) -0.0030(8) 0.0089(9) -0.0043(8) C80 0.0155(10) 0.0140(9) 0.0146(10) -0.0002(7) 0.0071(8) 0.0011(7) C712 0.0218(11) 0.0152(10) 0.0199(11) -0.0038(8) 0.0070(9) 0.0000(8) C12 0.0167(10) 0.0175(10) 0.0174(10) -0.0022(8) 0.0074(9) -0.0010(8) C32 0.0205(11) 0.0162(10) 0.0230(11) -0.0002(8) 0.0119(9) 0.0007(8) C912 0.0192(11) 0.0182(10) 0.0181(11) 0.0030(8) 0.0084(9) 0.0008(8) C90 0.0177(10) 0.0144(9) 0.0137(9) 0.0005(7) 0.0074(8) 0.0010(7) C811 0.0172(10) 0.0178(10) 0.0149(10) 0.0002(8) 0.0084(8) 0.0026(8) C926 0.0221(11) 0.0167(10) 0.0194(11) -0.0013(8) 0.0112(9) -0.0027(8) C821 0.0179(10) 0.0165(10) 0.0129(9) -0.0014(7) 0.0066(8) 0.0009(8) C825 0.0289(13) 0.0246(12) 0.0171(11) 0.0011(9) 0.0117(10) -0.0048(9) C70 0.0196(10) 0.0137(9) 0.0171(10) -0.0012(7) 0.0093(9) 0.0001(8) C51 0.0185(10) 0.0184(10) 0.0128(9) -0.0008(7) 0.0086(8) -0.0005(8) C16 0.0197(11) 0.0212(11) 0.0207(11) -0.0022(8) 0.0111(9) -0.0001(8) C11 0.0132(10) 0.0153(9) 0.0156(10) -0.0024(7) 0.0043(8) -0.0013(7) C36 0.0232(11) 0.0150(10) 0.0189(11) 0.0005(8) 0.0108(9) 0.0010(8) C721 0.0192(11) 0.0148(10) 0.0203(11) 0.0014(8) 0.0087(9) 0.0012(8) C420 0.0212(11) 0.0161(10) 0.0216(11) -0.0006(8) 0.0137(9) -0.0030(8) C714 0.0263(12) 0.0167(10) 0.0301(13) -0.0036(9) 0.0155(11) 0.0049(9) C716 0.0234(11) 0.0143(10) 0.0178(11) 0.0017(8) 0.0080(9) 0.0021(8) C916 0.0174(10) 0.0195(10) 0.0167(10) 0.0003(8) 0.0068(9) -0.0005(8) C822 0.0186(11) 0.0222(11) 0.0165(10) -0.0007(8) 0.0080(9) 0.0004(8) C914 0.0183(11) 0.0200(11) 0.0241(12) 0.0003(9) 0.0063(9) 0.0032(8) C34 0.0359(14) 0.0152(10) 0.0308(13) -0.0014(9) 0.0241(12) 0.0018(9) C35 0.0318(13) 0.0152(10) 0.0243(12) -0.0021(8) 0.0166(11) -0.0032(9) C56 0.0225(11) 0.0184(10) 0.0187(11) -0.0003(8) 0.0113(9) 0.0002(8) C223 0.0222(11) 0.0242(11) 0.0212(11) -0.0061(9) 0.0113(10) -0.0022(9) C915 0.0200(11) 0.0177(10) 0.0216(11) 0.0039(8) 0.0055(9) 0.0015(8) C715 0.0208(11) 0.0174(10) 0.0263(12) 0.0026(9) 0.0095(10) 0.0066(8) C53 0.0278(12) 0.0231(11) 0.0213(12) -0.0015(9) 0.0145(10) -0.0059(9) C921 0.0192(10) 0.0175(10) 0.0150(10) -0.0012(8) 0.0088(9) -0.0020(8) C713 0.0324(13) 0.0165(10) 0.0199(11) -0.0053(8) 0.0125(10) 0.0031(9) C812 0.0233(12) 0.0228(11) 0.0168(11) -0.0019(8) 0.0089(9) 0.0046(9) C620 0.0223(11) 0.0195(10) 0.0135(10) 0.0020(8) 0.0080(9) 0.0010(8) C222 0.0215(12) 0.0310(13) 0.0206(12) -0.0071(10) 0.0090(10) -0.0047(10) C826 0.0195(11) 0.0215(11) 0.0163(10) -0.0014(8) 0.0075(9) -0.0014(8) C623 0.0336(14) 0.0240(12) 0.0206(12) 0.0030(9) 0.0114(11) 0.0088(10) C922 0.0219(11) 0.0249(11) 0.0173(11) -0.0021(9) 0.0072(9) -0.0024(9) C726 0.0272(12) 0.0144(10) 0.0254(12) 0.0020(8) 0.0145(10) 0.0019(8) C54 0.0243(12) 0.0294(13) 0.0261(13) -0.0008(10) 0.0171(11) -0.0041(10) C913 0.0183(11) 0.0255(12) 0.0249(12) 0.0020(9) 0.0114(10) 0.0022(9) C422 0.0200(11) 0.0240(12) 0.0292(13) -0.0009(9) 0.0132(10) -0.0032(9) C52 0.0259(12) 0.0175(10) 0.0157(10) -0.0008(8) 0.0106(9) -0.0004(8) C925 0.0315(13) 0.0148(10) 0.0251(12) -0.0020(8) 0.0188(11) -0.0040(9) C531 0.0384(15) 0.0263(13) 0.0393(16) -0.0029(11) 0.0253(13) -0.0113(11) C724 0.0318(14) 0.0197(11) 0.0352(14) 0.0025(10) 0.0177(12) -0.0048(10) C15 0.0196(11) 0.0226(11) 0.0292(13) -0.0044(9) 0.0115(10) 0.0012(9) C622 0.0287(13) 0.0289(13) 0.0157(11) 0.0012(9) 0.0048(10) -0.0030(10) C14 0.0188(11) 0.0224(11) 0.0253(12) -0.0002(9) 0.0045(10) 0.0042(9) C13 0.0201(11) 0.0199(11) 0.0190(11) -0.0003(8) 0.0052(9) 0.0007(8) C33 0.0251(12) 0.0176(10) 0.0334(14) 0.0007(9) 0.0191(11) 0.0029(9) C551 0.0303(14) 0.0307(13) 0.0401(16) 0.0002(11) 0.0246(13) 0.0046(11) C823 0.0208(12) 0.0289(13) 0.0194(12) 0.0016(9) 0.0039(10) 0.0020(9) C55 0.0241(12) 0.0249(12) 0.0204(11) 0.0005(9) 0.0139(10) 0.0022(9) C621 0.0301(14) 0.0347(14) 0.0212(12) 0.0077(10) 0.0142(11) 0.0008(11) C351 0.0433(16) 0.0252(13) 0.0244(13) -0.0082(10) 0.0142(12) -0.0016(11) C815 0.0183(11) 0.0280(12) 0.0223(12) 0.0025(9) 0.0104(10) 0.0035(9) C722 0.0315(13) 0.0172(11) 0.0253(12) -0.0027(9) 0.0158(11) -0.0015(9) C924 0.0417(15) 0.0216(11) 0.0197(12) -0.0066(9) 0.0178(11) -0.0104(10) C824 0.0292(13) 0.0261(12) 0.0177(11) 0.0055(9) 0.0057(10) 0.0009(10) C725 0.0308(13) 0.0197(11) 0.0326(14) 0.0037(10) 0.0206(12) 0.0008(9) C814 0.0244(12) 0.0371(14) 0.0242(13) 0.0034(10) 0.0163(11) 0.0101(10) C723 0.0421(16) 0.0161(11) 0.0348(15) -0.0046(10) 0.0197(13) -0.0067(10) C421 0.0334(14) 0.0269(12) 0.0242(13) 0.0059(10) 0.0153(11) -0.0039(10) C331 0.0300(14) 0.0332(15) 0.0513(19) -0.0022(13) 0.0238(14) 0.0107(11) C221 0.0452(17) 0.0202(12) 0.0252(13) -0.0038(10) 0.0130(12) -0.0115(11) C813 0.0302(13) 0.0307(13) 0.0190(11) -0.0011(9) 0.0145(10) 0.0086(10) C923 0.0309(14) 0.0314(13) 0.0163(11) -0.0053(10) 0.0068(10) -0.0088(11) C131 0.0327(15) 0.0332(14) 0.0220(13) 0.0074(10) 0.0065(11) 0.0060(11) C151 0.0267(14) 0.0399(16) 0.0472(18) 0.0041(13) 0.0222(13) 0.0115(12) O1S 0.0666(17) 0.0502(14) 0.0433(14) -0.0029(11) 0.0298(13) -0.0244(13) C11S 0.076(3) 0.0401(18) 0.065(3) 0.0130(17) 0.048(2) 0.0101(18) C12S 0.068(3) 0.0337(17) 0.067(3) 0.0149(17) 0.036(2) -0.0009(16) C13S 0.0427(18) 0.0477(18) 0.0292(15) 0.0092(13) 0.0119(14) 0.0001(14) C14S 0.085(3) 0.0415(19) 0.051(2) -0.0112(16) 0.039(2) -0.0149(19) O2S 0.053(3) 0.065(3) 0.038(3) -0.016(2) 0.009(2) 0.007(3) C21S 0.042(4) 0.053(4) 0.048(4) -0.019(3) 0.013(3) 0.007(3) C22S 0.046(5) 0.069(5) 0.053(5) -0.024(4) 0.030(5) -0.008(4) C23S 0.045(5) 0.068(5) 0.043(4) -0.009(4) 0.018(4) 0.000(4) C24S 0.048(4) 0.061(5) 0.058(5) -0.021(4) 0.031(4) 0.003(3) O3S 0.107(6) 0.083(6) 0.101(6) -0.013(5) 0.019(5) 0.011(5) C31S 0.125(8) 0.117(10) 0.129(11) -0.022(8) 0.041(8) -0.042(9) C32S 0.158(9) 0.107(9) 0.056(6) -0.017(5) 0.021(6) 0.092(8) C33S 0.156(10) 0.167(13) 0.153(12) 0.004(10) 0.082(10) 0.059(10) C34S 0.098(8) 0.079(7) 0.106(8) -0.053(5) 0.039(7) -0.009(6) C41P 0.053(5) 0.076(6) 0.064(6) 0.011(4) 0.016(4) 0.016(4) C42P 0.048(5) 0.116(9) 0.101(8) -0.038(6) 0.019(5) 0.001(5) C43P 0.172(14) 0.124(12) 0.166(12) 0.040(11) 0.035(11) -0.023(10) C44P 0.106(9) 0.078(7) 0.110(8) -0.021(6) 0.023(7) 0.051(6) C45P 0.27(2) 0.21(2) 0.37(4) 0.01(3) 0.14(2) -0.11(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 Rh1 P1 2.1643(6) . ? Rh1 C711 2.195(2) . ? Rh1 C811 2.214(2) . ? Rh1 C816 2.237(2) . ? Rh1 C716 2.290(2) . ? Rh1 C712 2.322(2) . ? Rh1 C713 2.400(2) . ? Rh1 C714 2.415(2) . ? Rh1 C715 2.428(2) . ? Nb1 N1 2.0235(19) . ? Nb1 N3 2.0260(19) . ? Nb1 N2 2.0316(18) . ? Nb1 O3 2.0735(16) . ? Nb1 O2 2.1280(16) . ? Nb1 O1 2.1383(15) . ? P1 C7 1.820(2) . ? P1 C8 1.824(2) . ? P1 C9 1.850(2) . ? O3 C9 1.322(3) . ? O1 C7 1.313(3) . ? O2 C8 1.314(3) . ? C8 C80 1.373(3) . ? N3 C51 1.440(3) . ? N3 C61 1.483(3) . ? N1 C11 1.438(3) . ? N1 C21 1.483(3) . ? C7 C70 1.376(3) . ? N2 C31 1.443(3) . ? N2 C41 1.489(3) . ? C9 C90 1.365(3) . ? C423 C420 1.534(3) . ? C816 C815 1.431(3) . ? C816 C811 1.443(3) . ? C711 C712 1.432(3) . ? C711 C716 1.439(3) . ? C711 C70 1.502(3) . ? C41 C420 1.546(3) . ? C31 C36 1.395(3) . ? C31 C32 1.401(3) . ? C911 C916 1.397(3) . ? C911 C912 1.398(3) . ? C911 C90 1.492(3) . ? C21 C220 1.546(3) . ? C61 C620 1.552(3) . ? C220 C223 1.533(3) . ? C220 C221 1.535(3) . ? C220 C222 1.535(4) . ? C80 C821 1.483(3) . ? C80 C811 1.508(3) . ? C712 C713 1.406(3) . ? C12 C11 1.391(3) . ? C12 C13 1.394(3) . ? C32 C33 1.401(3) . ? C912 C913 1.387(3) . ? C90 C921 1.485(3) . ? C811 C812 1.448(3) . ? C926 C925 1.389(3) . ? C926 C921 1.409(3) . ? C821 C822 1.401(3) . ? C821 C826 1.408(3) . ? C825 C826 1.387(3) . ? C825 C824 1.392(4) . ? C70 C721 1.469(3) . ? C51 C52 1.396(3) . ? C51 C56 1.401(3) . ? C16 C15 1.391(3) . ? C16 C11 1.394(3) . ? C36 C35 1.394(3) . ? C721 C726 1.406(3) . ? C721 C722 1.411(3) . ? C420 C422 1.530(3) . ? C420 C421 1.540(3) . ? C714 C715 1.407(4) . ? C714 C713 1.411(4) . ? C716 C715 1.407(3) . ? C916 C915 1.396(3) . ? C822 C823 1.392(3) . ? C914 C915 1.383(4) . ? C914 C913 1.394(3) . ? C34 C33 1.388(4) . ? C34 C35 1.399(4) . ? C35 C351 1.512(4) . ? C56 C55 1.397(3) . ? C53 C52 1.394(3) . ? C53 C54 1.396(4) . ? C53 C531 1.513(3) . ? C921 C922 1.402(3) . ? C812 C813 1.365(3) . ? C620 C623 1.527(3) . ? C620 C621 1.535(3) . ? C620 C622 1.538(3) . ? C922 C923 1.396(3) . ? C726 C725 1.384(3) . ? C54 C55 1.396(4) . ? C925 C924 1.384(4) . ? C724 C723 1.386(4) . ? C724 C725 1.394(4) . ? C15 C14 1.394(4) . ? C15 C151 1.508(4) . ? C14 C13 1.399(4) . ? C13 C131 1.506(4) . ? C33 C331 1.514(4) . ? C551 C55 1.511(4) . ? C823 C824 1.391(4) . ? C815 C814 1.359(4) . ? C722 C723 1.390(4) . ? C924 C923 1.386(4) . ? C814 C813 1.424(4) . ? O1S C11S 1.424(4) . ? O1S C14S 1.436(5) . ? C11S C12S 1.509(5) . ? C12S C13S 1.488(5) . ? C13S C14S 1.496(5) . ? O2S C21S 1.426(7) . ? O2S C24S 1.435(8) . ? C21S C22S 1.527(11) . ? C22S C23S 1.475(10) . ? C23S C24S 1.528(10) . ? O3S C31S 1.403(9) . ? O3S C34S 1.598(9) . ? C31S C32S 1.6256 . ? C32S C33S 1.3171 . ? C33S C34S 1.3703 . ? C41P C42P 1.5051 . ? C42P C43P 1.3171 . ? C43P C44P 1.7172 . ? C44P C45P 2.0204 . ? 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 P1 Rh1 C711 82.56(6) . . ? P1 Rh1 C811 82.43(6) . . ? C711 Rh1 C811 138.14(8) . . ? P1 Rh1 C816 86.72(6) . . ? C711 Rh1 C816 169.19(8) . . ? C811 Rh1 C816 37.83(8) . . ? P1 Rh1 C716 97.68(6) . . ? C711 Rh1 C716 37.35(8) . . ? C811 Rh1 C716 175.11(9) . . ? C816 Rh1 C716 147.03(8) . . ? P1 Rh1 C712 102.45(6) . . ? C711 Rh1 C712 36.84(8) . . ? C811 Rh1 C712 110.69(8) . . ? C816 Rh1 C712 146.45(8) . . ? C716 Rh1 C712 64.49(9) . . ? P1 Rh1 C713 136.26(7) . . ? C711 Rh1 C713 64.34(9) . . ? C811 Rh1 C713 103.06(8) . . ? C816 Rh1 C713 124.08(9) . . ? C716 Rh1 C713 73.47(8) . . ? C712 Rh1 C713 34.59(8) . . ? P1 Rh1 C714 157.94(7) . . ? C711 Rh1 C714 75.90(8) . . ? C811 Rh1 C714 117.06(9) . . ? C816 Rh1 C714 114.89(9) . . ? C716 Rh1 C714 61.99(9) . . ? C712 Rh1 C714 62.30(9) . . ? C713 Rh1 C714 34.08(9) . . ? P1 Rh1 C715 130.04(6) . . ? C711 Rh1 C715 64.74(8) . . ? C811 Rh1 C715 146.63(8) . . ? C816 Rh1 C715 124.34(8) . . ? C716 Rh1 C715 34.56(8) . . ? C712 Rh1 C715 73.65(9) . . ? C713 Rh1 C715 60.86(9) . . ? C714 Rh1 C715 33.79(9) . . ? N1 Nb1 N3 97.48(8) . . ? N1 Nb1 N2 98.37(7) . . ? N3 Nb1 N2 97.07(7) . . ? N1 Nb1 O3 164.72(7) . . ? N3 Nb1 O3 88.57(7) . . ? N2 Nb1 O3 94.76(7) . . ? N1 Nb1 O2 93.13(7) . . ? N3 Nb1 O2 168.65(7) . . ? N2 Nb1 O2 85.30(7) . . ? O3 Nb1 O2 80.15(6) . . ? N1 Nb1 O1 84.64(7) . . ? N3 Nb1 O1 91.54(7) . . ? N2 Nb1 O1 170.41(7) . . ? O3 Nb1 O1 81.18(6) . . ? O2 Nb1 O1 85.44(6) . . ? C7 P1 C8 103.10(10) . . ? C7 P1 C9 102.20(10) . . ? C8 P1 C9 100.26(10) . . ? C7 P1 Rh1 106.48(7) . . ? C8 P1 Rh1 104.31(7) . . ? C9 P1 Rh1 136.39(7) . . ? C9 O3 Nb1 136.17(14) . . ? C7 O1 Nb1 130.27(14) . . ? C8 O2 Nb1 128.11(14) . . ? O2 C8 C80 128.9(2) . . ? O2 C8 P1 117.88(16) . . ? C80 C8 P1 113.20(16) . . ? C51 N3 C61 112.39(17) . . ? C51 N3 Nb1 121.15(14) . . ? C61 N3 Nb1 126.15(14) . . ? C11 N1 C21 111.12(17) . . ? C11 N1 Nb1 121.57(14) . . ? C21 N1 Nb1 127.23(14) . . ? O1 C7 C70 128.8(2) . . ? O1 C7 P1 114.91(15) . . ? C70 C7 P1 116.28(17) . . ? C31 N2 C41 111.40(17) . . ? C31 N2 Nb1 122.04(14) . . ? C41 N2 Nb1 125.82(14) . . ? O3 C9 C90 124.99(19) . . ? O3 C9 P1 110.02(15) . . ? C90 C9 P1 124.83(16) . . ? C815 C816 C811 120.3(2) . . ? C815 C816 Rh1 108.36(16) . . ? C811 C816 Rh1 70.24(13) . . ? C712 C711 C716 118.0(2) . . ? C712 C711 C70 120.1(2) . . ? C716 C711 C70 121.9(2) . . ? C712 C711 Rh1 76.42(14) . . ? C716 C711 Rh1 74.91(13) . . ? C70 C711 Rh1 117.07(14) . . ? N2 C41 C420 119.09(19) . . ? C36 C31 C32 119.1(2) . . ? C36 C31 N2 120.7(2) . . ? C32 C31 N2 120.2(2) . . ? C916 C911 C912 118.4(2) . . ? C916 C911 C90 120.0(2) . . ? C912 C911 C90 121.5(2) . . ? N1 C21 C220 118.16(18) . . ? N3 C61 C620 119.44(18) . . ? C223 C220 C221 108.8(2) . . ? C223 C220 C222 110.8(2) . . ? C221 C220 C222 107.6(2) . . ? C223 C220 C21 110.67(19) . . ? C221 C220 C21 105.51(19) . . ? C222 C220 C21 113.2(2) . . ? C8 C80 C821 123.5(2) . . ? C8 C80 C811 120.58(19) . . ? C821 C80 C811 115.86(19) . . ? C713 C712 C711 119.6(2) . . ? C713 C712 Rh1 75.75(14) . . ? C711 C712 Rh1 66.74(12) . . ? C11 C12 C13 121.5(2) . . ? C31 C32 C33 120.4(2) . . ? C913 C912 C911 120.8(2) . . ? C9 C90 C921 123.1(2) . . ? C9 C90 C911 119.47(19) . . ? C921 C90 C911 116.94(19) . . ? C816 C811 C812 116.0(2) . . ? C816 C811 C80 123.79(19) . . ? C812 C811 C80 116.7(2) . . ? C816 C811 Rh1 71.93(13) . . ? C812 C811 Rh1 105.47(15) . . ? C80 C811 Rh1 110.57(14) . . ? C925 C926 C921 121.0(2) . . ? C822 C821 C826 118.1(2) . . ? C822 C821 C80 122.7(2) . . ? C826 C821 C80 119.2(2) . . ? C826 C825 C824 120.3(2) . . ? C7 C70 C721 124.3(2) . . ? C7 C70 C711 116.5(2) . . ? C721 C70 C711 119.08(19) . . ? C52 C51 C56 119.2(2) . . ? C52 C51 N3 120.5(2) . . ? C56 C51 N3 120.3(2) . . ? C15 C16 C11 120.5(2) . . ? C12 C11 C16 119.3(2) . . ? C12 C11 N1 120.4(2) . . ? C16 C11 N1 120.3(2) . . ? C35 C36 C31 121.2(2) . . ? C726 C721 C722 117.5(2) . . ? C726 C721 C70 120.9(2) . . ? C722 C721 C70 121.6(2) . . ? C422 C420 C423 109.8(2) . . ? C422 C420 C421 109.2(2) . . ? C423 C420 C421 108.7(2) . . ? C422 C420 C41 111.19(19) . . ? C423 C420 C41 113.30(19) . . ? C421 C420 C41 104.48(19) . . ? C715 C714 C713 120.4(2) . . ? C715 C714 Rh1 73.62(13) . . ? C713 C714 Rh1 72.40(13) . . ? C715 C716 C711 121.5(2) . . ? C715 C716 Rh1 78.11(14) . . ? C711 C716 Rh1 67.74(12) . . ? C915 C916 C911 120.8(2) . . ? C823 C822 C821 120.7(2) . . ? C915 C914 C913 119.8(2) . . ? C33 C34 C35 121.5(2) . . ? C36 C35 C34 118.6(2) . . ? C36 C35 C351 120.2(2) . . ? C34 C35 C351 121.2(2) . . ? C55 C56 C51 120.6(2) . . ? C914 C915 C916 120.0(2) . . ? C716 C715 C714 119.0(2) . . ? C716 C715 Rh1 67.33(13) . . ? C714 C715 Rh1 72.59(14) . . ? C52 C53 C54 118.9(2) . . ? C52 C53 C531 120.0(2) . . ? C54 C53 C531 121.1(2) . . ? C922 C921 C926 117.2(2) . . ? C922 C921 C90 119.9(2) . . ? C926 C921 C90 122.9(2) . . ? C712 C713 C714 121.0(2) . . ? C712 C713 Rh1 69.66(13) . . ? C714 C713 Rh1 73.52(14) . . ? C813 C812 C811 122.0(2) . . ? C623 C620 C621 109.6(2) . . ? C623 C620 C622 109.5(2) . . ? C621 C620 C622 107.9(2) . . ? C623 C620 C61 110.83(19) . . ? C621 C620 C61 113.4(2) . . ? C622 C620 C61 105.52(19) . . ? C825 C826 C821 120.9(2) . . ? C923 C922 C921 121.3(2) . . ? C725 C726 C721 121.4(2) . . ? C53 C54 C55 121.3(2) . . ? C912 C913 C914 120.2(2) . . ? C53 C52 C51 121.0(2) . . ? C924 C925 C926 120.8(2) . . ? C723 C724 C725 119.3(2) . . ? C16 C15 C14 119.2(2) . . ? C16 C15 C151 120.4(2) . . ? C14 C15 C151 120.4(2) . . ? C15 C14 C13 121.3(2) . . ? C12 C13 C14 118.1(2) . . ? C12 C13 C131 120.5(2) . . ? C14 C13 C131 121.3(2) . . ? C34 C33 C32 119.1(2) . . ? C34 C33 C331 121.4(2) . . ? C32 C33 C331 119.5(2) . . ? C824 C823 C822 120.5(2) . . ? C54 C55 C56 119.0(2) . . ? C54 C55 C551 120.6(2) . . ? C56 C55 C551 120.5(2) . . ? C814 C815 C816 120.9(2) . . ? C723 C722 C721 120.8(2) . . ? C925 C924 C923 119.2(2) . . ? C823 C824 C825 119.4(2) . . ? C726 C725 C724 120.4(2) . . ? C815 C814 C813 120.1(2) . . ? C724 C723 C722 120.6(2) . . ? C812 C813 C814 120.7(2) . . ? C924 C923 C922 120.3(2) . . ? C11S O1S C14S 109.1(3) . . ? O1S C11S C12S 105.3(3) . . ? C13S C12S C11S 102.9(3) . . ? C12S C13S C14S 103.4(3) . . ? O1S C14S C13S 107.1(3) . . ? C21S O2S C24S 106.6(5) . . ? O2S C21S C22S 101.7(6) . . ? C23S C22S C21S 105.5(8) . . ? C22S C23S C24S 104.6(7) . . ? O2S C24S C23S 105.0(6) . . ? C31S O3S C34S 113.4(5) . . ? O3S C31S C32S 88.8(4) . . ? C33S C32S C31S 101.4 . . ? C32S C33S C34S 112.6 . . ? C33S C34S O3S 94.4(3) . . ? C43P C42P C41P 120.8 . . ? C42P C43P C44P 111.4 . . ? C43P C44P C45P 81.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.450 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.097 # Attachment '2143_web_deposit_cif_file_1_SidCreutz_1281724789.cif' data_10216 _database_code_depnum_ccdc_archive 'CCDC 789238' #TrackingRef '2143_web_deposit_cif_file_1_SidCreutz_1281724789.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (py)CuP(C[CPh2]O)3Nb(N[Np]Ar)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H115 Cu N4 Nb O5.50 P' _chemical_formula_weight 1600.34 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 27.065(3) _cell_length_b 14.0252(16) _cell_length_c 24.972(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.777(2) _cell_angle_gamma 90.00 _cell_volume 8462.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9207 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 30.94 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8371 _exptl_absorpt_correction_T_max 0.8741 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 229224 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.03 _reflns_number_total 24729 _reflns_number_gt 19030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+10.3130P] 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 24729 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 366 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.287122(7) 0.582017(12) 0.271825(8) 0.01322(5) Uani 1 1 d . . . Cu1 Cu 0.105415(12) 0.43299(2) 0.303099(14) 0.02482(7) Uani 1 1 d . . . P1 P 0.17146(2) 0.48825(4) 0.28492(2) 0.01399(10) Uani 1 1 d . . . O1 O 0.21737(6) 0.50529(10) 0.21143(7) 0.0159(3) Uani 1 1 d . . . O2 O 0.22661(6) 0.64886(10) 0.28923(7) 0.0159(3) Uani 1 1 d . . . O3 O 0.28246(6) 0.48181(10) 0.33175(7) 0.0160(3) Uani 1 1 d . . . N1 N 0.27463(7) 0.67122(12) 0.20261(8) 0.0164(3) Uani 1 1 d . . . N2 N 0.34375(7) 0.66246(12) 0.33921(8) 0.0163(3) Uani 1 1 d . . . N3 N 0.34078(7) 0.49453(12) 0.25940(8) 0.0160(3) Uani 1 1 d . . . N4 N 0.05422(8) 0.37372(14) 0.32728(9) 0.0228(4) Uani 1 1 d . . . C5 C 0.19079(8) 0.61356(14) 0.30660(9) 0.0153(4) Uani 1 1 d . . . C6 C 0.23959(8) 0.42818(14) 0.32437(9) 0.0152(4) Uani 1 1 d . . . C7 C 0.16839(8) 0.49000(14) 0.20941(9) 0.0149(4) Uani 1 1 d . . . C18 C 0.19004(10) 0.72436(16) 0.10379(10) 0.0220(4) Uani 1 1 d . . . C16 C 0.29753(9) 0.83329(15) 0.24333(10) 0.0215(4) Uani 1 1 d . . . H16 H 0.2723 0.8258 0.2600 0.026 Uiso 1 1 calc R . . C13 C 0.37160(11) 0.85490(19) 0.19447(12) 0.0296(5) Uani 1 1 d . . . C11 C 0.30574(9) 0.75802(15) 0.21170(10) 0.0187(4) Uani 1 1 d . . . C14 C 0.36246(11) 0.92890(18) 0.22595(13) 0.0326(6) Uani 1 1 d . . . H14 H 0.3817 0.9874 0.2306 0.039 Uiso 1 1 calc R . . C151 C 0.31574(14) 0.99995(19) 0.28530(17) 0.0443(8) Uani 1 1 d . . . H15A H 0.3485 1.0410 0.3028 0.066 Uiso 1 1 calc R . . H15B H 0.3084 0.9734 0.3173 0.066 Uiso 1 1 calc R . . H15C H 0.2838 1.0375 0.2579 0.066 Uiso 1 1 calc R . . C12 C 0.34299(10) 0.76883(17) 0.18758(11) 0.0240(5) Uani 1 1 d . . . H12 H 0.3490 0.7175 0.1664 0.029 Uiso 1 1 calc R . . C131 C 0.41134(13) 0.8660(2) 0.16737(15) 0.0422(7) Uani 1 1 d . . . H13A H 0.3910 0.8880 0.1258 0.063 Uiso 1 1 calc R . . H13B H 0.4288 0.8044 0.1681 0.063 Uiso 1 1 calc R . . H13C H 0.4399 0.9127 0.1906 0.063 Uiso 1 1 calc R . . C182 C 0.15627(11) 0.7396(2) 0.13816(13) 0.0361(6) Uani 1 1 d . . . H18A H 0.1250 0.7819 0.1151 0.054 Uiso 1 1 calc R . . H18B H 0.1797 0.7686 0.1772 0.054 Uiso 1 1 calc R . . H18C H 0.1424 0.6781 0.1443 0.054 Uiso 1 1 calc R . . C183 C 0.15386(12) 0.6765(2) 0.04317(12) 0.0360(6) Uani 1 1 d . . . H18D H 0.1394 0.6162 0.0500 0.054 Uiso 1 1 calc R . . H18E H 0.1762 0.6642 0.0220 0.054 Uiso 1 1 calc R . . H18F H 0.1230 0.7188 0.0189 0.054 Uiso 1 1 calc R . . C17 C 0.23798(9) 0.65384(15) 0.13811(10) 0.0193(4) Uani 1 1 d . . . H17A H 0.2216 0.5896 0.1344 0.023 Uiso 1 1 calc R . . H17B H 0.2615 0.6520 0.1172 0.023 Uiso 1 1 calc R . . C181 C 0.20910(11) 0.82063(18) 0.09028(12) 0.0303(5) Uani 1 1 d . . . H18G H 0.1767 0.8582 0.0639 0.046 Uiso 1 1 calc R . . H18H H 0.2327 0.8097 0.0705 0.046 Uiso 1 1 calc R . . H18I H 0.2301 0.8554 0.1279 0.046 Uiso 1 1 calc R . . C15 C 0.32579(11) 0.91939(16) 0.25091(13) 0.0288(5) Uani 1 1 d . . . C21 C 0.40185(9) 0.65559(15) 0.35479(10) 0.0178(4) Uani 1 1 d . . . C23 C 0.48485(10) 0.72420(19) 0.35634(11) 0.0273(5) Uani 1 1 d . . . C251 C 0.52029(11) 0.4803(2) 0.43212(13) 0.0329(6) Uani 1 1 d . . . H25A H 0.5049 0.4546 0.4579 0.049 Uiso 1 1 calc R . . H25B H 0.5593 0.4971 0.4567 0.049 Uiso 1 1 calc R . . H25C H 0.5175 0.4322 0.4024 0.049 Uiso 1 1 calc R . . C22 C 0.42856(9) 0.73005(17) 0.34091(11) 0.0229(4) Uani 1 1 d . . . H22 H 0.4082 0.7851 0.3208 0.027 Uiso 1 1 calc R . . C27 C 0.33284(9) 0.74009(15) 0.37273(10) 0.0188(4) Uani 1 1 d . . . H27A H 0.2925 0.7527 0.3529 0.023 Uiso 1 1 calc R . . H27B H 0.3513 0.7984 0.3683 0.023 Uiso 1 1 calc R . . C26 C 0.43252(9) 0.57645(15) 0.38582(10) 0.0183(4) Uani 1 1 d . . . H26 H 0.4150 0.5273 0.3972 0.022 Uiso 1 1 calc R . . C231 C 0.51354(12) 0.8059(2) 0.34212(15) 0.0423(7) Uani 1 1 d . . . H23A H 0.5281 0.8506 0.3759 0.063 Uiso 1 1 calc R . . H23B H 0.4870 0.8389 0.3060 0.063 Uiso 1 1 calc R . . H23C H 0.5441 0.7810 0.3353 0.063 Uiso 1 1 calc R . . C28 C 0.35097(10) 0.72555(16) 0.44076(10) 0.0223(4) Uani 1 1 d . . . C282 C 0.32832(11) 0.81254(19) 0.46026(12) 0.0318(6) Uani 1 1 d . . . H28A H 0.3373 0.8064 0.5027 0.048 Uiso 1 1 calc R . . H28B H 0.2881 0.8158 0.4361 0.048 Uiso 1 1 calc R . . H28C H 0.3452 0.8708 0.4543 0.048 Uiso 1 1 calc R . . C281 C 0.32546(14) 0.6348(2) 0.45069(12) 0.0364(6) Uani 1 1 d . . . H28D H 0.3390 0.5798 0.4370 0.055 Uiso 1 1 calc R . . H28E H 0.2851 0.6383 0.4280 0.055 Uiso 1 1 calc R . . H28F H 0.3358 0.6278 0.4935 0.055 Uiso 1 1 calc R . . C25 C 0.48832(10) 0.56819(18) 0.40034(11) 0.0246(5) Uani 1 1 d . . . C283 C 0.41374(11) 0.7247(2) 0.47966(12) 0.0312(5) Uani 1 1 d . . . H28G H 0.4220 0.7263 0.5221 0.047 Uiso 1 1 calc R . . H28H H 0.4301 0.7807 0.4703 0.047 Uiso 1 1 calc R . . H28I H 0.4293 0.6667 0.4715 0.047 Uiso 1 1 calc R . . C24 C 0.51389(10) 0.6426(2) 0.38523(11) 0.0279(5) Uani 1 1 d . . . H24 H 0.5520 0.6375 0.3949 0.033 Uiso 1 1 calc R . . C33 C 0.34208(10) 0.51165(16) 0.11030(11) 0.0226(4) Uani 1 1 d . . . C37 C 0.37148(9) 0.41268(14) 0.29780(10) 0.0176(4) Uani 1 1 d . . . H37A H 0.3597 0.4066 0.3298 0.021 Uiso 1 1 calc R . . H37B H 0.4112 0.4300 0.3176 0.021 Uiso 1 1 calc R . . C31 C 0.35897(9) 0.51454(14) 0.21459(10) 0.0174(4) Uani 1 1 d . . . C382 C 0.39626(10) 0.24488(16) 0.32343(12) 0.0256(5) Uani 1 1 d . . . H38A H 0.3757 0.2429 0.3472 0.038 Uiso 1 1 calc R . . H38B H 0.4339 0.2680 0.3485 0.038 Uiso 1 1 calc R . . H38C H 0.3979 0.1807 0.3088 0.038 Uiso 1 1 calc R . . C36 C 0.41253(9) 0.54905(16) 0.23155(11) 0.0219(4) Uani 1 1 d . . . H36 H 0.4365 0.5615 0.2726 0.026 Uiso 1 1 calc R . . C32 C 0.32442(9) 0.49604(15) 0.15439(10) 0.0196(4) Uani 1 1 d . . . H32 H 0.2882 0.4724 0.1430 0.024 Uiso 1 1 calc R . . C35 C 0.43082(10) 0.56519(18) 0.18823(12) 0.0264(5) Uani 1 1 d . . . C351 C 0.48891(12) 0.6032(2) 0.20720(15) 0.0405(7) Uani 1 1 d . . . H35A H 0.5141 0.5499 0.2127 0.061 Uiso 1 1 calc R . . H35B H 0.5013 0.6383 0.2450 0.061 Uiso 1 1 calc R . . H35C H 0.4888 0.6460 0.1761 0.061 Uiso 1 1 calc R . . C381 C 0.39713(11) 0.30351(17) 0.23069(12) 0.0264(5) Uani 1 1 d . . . H38D H 0.3980 0.2364 0.2202 0.040 Uiso 1 1 calc R . . H38E H 0.4351 0.3273 0.2531 0.040 Uiso 1 1 calc R . . H38F H 0.3777 0.3411 0.1940 0.040 Uiso 1 1 calc R . . C38 C 0.36677(9) 0.31258(15) 0.26963(10) 0.0200(4) Uani 1 1 d . . . C383 C 0.30610(10) 0.28348(17) 0.23437(12) 0.0279(5) Uani 1 1 d . . . H38G H 0.2880 0.2869 0.2606 0.042 Uiso 1 1 calc R . . H38H H 0.3039 0.2181 0.2196 0.042 Uiso 1 1 calc R . . H38I H 0.2875 0.3268 0.2003 0.042 Uiso 1 1 calc R . . C331 C 0.30410(12) 0.4900(2) 0.04560(11) 0.0311(5) Uani 1 1 d . . . H33A H 0.2905 0.5499 0.0235 0.047 Uiso 1 1 calc R . . H33B H 0.2727 0.4521 0.0430 0.047 Uiso 1 1 calc R . . H33C H 0.3243 0.4541 0.0281 0.047 Uiso 1 1 calc R . . C34 C 0.39553(11) 0.54649(18) 0.12816(12) 0.0269(5) Uani 1 1 d . . . H34 H 0.4081 0.5577 0.0988 0.032 Uiso 1 1 calc R . . C42 C 0.03844(14) 0.2941(2) 0.40275(15) 0.0385(6) Uani 1 1 d . . . H42 H 0.0531 0.2693 0.4423 0.046 Uiso 1 1 calc R . . C43 C -0.01715(15) 0.2872(2) 0.36474(17) 0.0471(8) Uani 1 1 d . . . H43 H -0.0416 0.2577 0.3776 0.057 Uiso 1 1 calc R . . C41 C 0.07248(11) 0.33743(18) 0.38258(12) 0.0291(5) Uani 1 1 d . . . H41 H 0.1109 0.3419 0.4092 0.035 Uiso 1 1 calc R . . C45 C 0.00004(11) 0.3668(2) 0.29059(13) 0.0342(6) Uani 1 1 d . . . H45 H -0.0138 0.3922 0.2512 0.041 Uiso 1 1 calc R . . C44 C -0.03673(12) 0.3236(3) 0.30805(16) 0.0459(8) Uani 1 1 d . . . H44 H -0.0750 0.3194 0.2809 0.055 Uiso 1 1 calc R . . C50 C 0.16530(8) 0.66517(14) 0.33361(9) 0.0160(4) Uani 1 1 d . . . C521 C 0.13049(9) 0.62101(15) 0.35938(10) 0.0181(4) Uani 1 1 d . . . C522 C 0.15451(10) 0.56663(16) 0.41187(11) 0.0237(5) Uani 1 1 d . . . H522 H 0.1921 0.5475 0.4271 0.028 Uiso 1 1 calc R . . C526 C 0.07443(10) 0.64600(17) 0.33746(11) 0.0237(5) Uani 1 1 d . . . H526 H 0.0570 0.6825 0.3017 0.028 Uiso 1 1 calc R . . C511 C 0.17492(9) 0.76900(15) 0.34560(10) 0.0178(4) Uani 1 1 d . . . C512 C 0.17276(9) 0.80915(16) 0.39628(11) 0.0213(4) Uani 1 1 d . . . H512 H 0.1635 0.7699 0.4215 0.026 Uiso 1 1 calc R . . C525 C 0.04414(11) 0.61801(19) 0.36742(13) 0.0305(5) Uani 1 1 d . . . H525 H 0.0062 0.6348 0.3516 0.037 Uiso 1 1 calc R . . C514 C 0.19694(10) 0.96415(17) 0.37341(13) 0.0292(5) Uani 1 1 d . . . H514 H 0.2058 1.0293 0.3835 0.035 Uiso 1 1 calc R . . C515 C 0.19681(11) 0.92693(17) 0.32203(13) 0.0283(5) Uani 1 1 d . . . H515 H 0.2040 0.9676 0.2959 0.034 Uiso 1 1 calc R . . C524 C 0.06892(12) 0.5660(2) 0.41998(13) 0.0341(6) Uani 1 1 d . . . H524 H 0.0482 0.5482 0.4406 0.041 Uiso 1 1 calc R . . C513 C 0.18395(10) 0.90539(16) 0.40999(12) 0.0256(5) Uani 1 1 d . . . H513 H 0.1827 0.9310 0.4446 0.031 Uiso 1 1 calc R . . C523 C 0.12408(12) 0.53986(19) 0.44245(12) 0.0308(5) Uani 1 1 d . . . H523 H 0.1412 0.5039 0.4785 0.037 Uiso 1 1 calc R . . C516 C 0.18623(9) 0.83038(16) 0.30809(11) 0.0217(4) Uani 1 1 d . . . H516 H 0.1867 0.8059 0.2728 0.026 Uiso 1 1 calc R . . C60 C 0.24265(9) 0.33715(14) 0.34603(9) 0.0165(4) Uani 1 1 d . . . C612 C 0.29989(10) 0.19148(16) 0.39295(11) 0.0236(5) Uani 1 1 d . . . H612 H 0.2696 0.1532 0.3670 0.028 Uiso 1 1 calc R . . C626 C 0.16282(9) 0.26233(15) 0.25939(10) 0.0204(4) Uani 1 1 d . . . H626 H 0.1754 0.2922 0.2337 0.025 Uiso 1 1 calc R . . C624 C 0.09776(10) 0.15925(16) 0.27196(12) 0.0256(5) Uani 1 1 d . . . H624 H 0.0658 0.1198 0.2555 0.031 Uiso 1 1 calc R . . C622 C 0.17296(10) 0.23020(15) 0.35830(11) 0.0214(4) Uani 1 1 d . . . H622 H 0.1921 0.2383 0.4006 0.026 Uiso 1 1 calc R . . C613 C 0.34780(11) 0.14764(18) 0.43429(12) 0.0290(5) Uani 1 1 d . . . H613 H 0.3497 0.0800 0.4369 0.035 Uiso 1 1 calc R . . C625 C 0.11580(10) 0.20455(16) 0.23458(11) 0.0242(5) Uani 1 1 d . . . H625 H 0.0963 0.1963 0.1923 0.029 Uiso 1 1 calc R . . C614 C 0.39305(11) 0.2021(2) 0.47202(12) 0.0316(6) Uani 1 1 d . . . H614 H 0.4259 0.1721 0.5004 0.038 Uiso 1 1 calc R . . C615 C 0.38957(11) 0.3008(2) 0.46770(11) 0.0299(5) Uani 1 1 d . . . H615 H 0.4206 0.3385 0.4928 0.036 Uiso 1 1 calc R . . C611 C 0.29504(9) 0.29128(15) 0.38855(10) 0.0186(4) Uani 1 1 d . . . C623 C 0.12652(10) 0.17187(16) 0.33348(12) 0.0245(5) Uani 1 1 d . . . H623 H 0.1143 0.1402 0.3590 0.029 Uiso 1 1 calc R . . C616 C 0.34112(10) 0.34508(17) 0.42701(10) 0.0227(4) Uani 1 1 d . . . H616 H 0.3392 0.4127 0.4253 0.027 Uiso 1 1 calc R . . C621 C 0.19183(9) 0.27712(14) 0.32145(10) 0.0176(4) Uani 1 1 d . . . C70 C 0.12175(8) 0.46393(14) 0.15910(9) 0.0162(4) Uani 1 1 d . . . C726 C 0.17020(10) 0.39560(18) 0.10245(12) 0.0271(5) Uani 1 1 d . . . H726 H 0.2014 0.3821 0.1396 0.033 Uiso 1 1 calc R . . C721 C 0.12372(9) 0.43849(15) 0.10236(10) 0.0190(4) Uani 1 1 d . . . C716 C 0.02877(9) 0.38923(16) 0.13328(10) 0.0214(4) Uani 1 1 d . . . H716 H 0.0392 0.3349 0.1181 0.026 Uiso 1 1 calc R . . C715 C -0.02374(10) 0.39321(17) 0.13031(11) 0.0250(5) Uani 1 1 d . . . H715 H -0.0488 0.3417 0.1131 0.030 Uiso 1 1 calc R . . C713 C -0.00278(10) 0.54689(18) 0.17783(11) 0.0258(5) Uani 1 1 d . . . H713 H -0.0134 0.6007 0.1933 0.031 Uiso 1 1 calc R . . C714 C -0.03973(10) 0.47213(19) 0.15233(11) 0.0268(5) Uani 1 1 d . . . H714 H -0.0757 0.4750 0.1500 0.032 Uiso 1 1 calc R . . C712 C 0.04974(9) 0.54310(16) 0.18068(10) 0.0205(4) Uani 1 1 d . . . H712 H 0.0745 0.5949 0.1980 0.025 Uiso 1 1 calc R . . C725 C 0.17183(12) 0.3722(2) 0.04910(13) 0.0378(7) Uani 1 1 d . . . H725 H 0.2040 0.3433 0.0501 0.045 Uiso 1 1 calc R . . C711 C 0.06680(9) 0.46465(15) 0.15858(9) 0.0173(4) Uani 1 1 d . . . C722 C 0.07811(10) 0.45529(18) 0.04631(11) 0.0264(5) Uani 1 1 d . . . H722 H 0.0456 0.4834 0.0448 0.032 Uiso 1 1 calc R . . C724 C 0.12683(14) 0.3908(2) -0.00525(13) 0.0415(7) Uani 1 1 d . . . H724 H 0.1283 0.3757 -0.0416 0.050 Uiso 1 1 calc R . . C723 C 0.07981(13) 0.4314(2) -0.00680(12) 0.0358(6) Uani 1 1 d . . . H723 H 0.0486 0.4431 -0.0442 0.043 Uiso 1 1 calc R . . O1S O 0.06831(15) 0.1036(3) 0.09037(18) 0.0927(11) Uani 1 1 d DU . . C11S C 0.1064(3) 0.1454(4) 0.0732(3) 0.0959(17) Uani 1 1 d DU . . H11A H 0.1034 0.2158 0.0725 0.115 Uiso 1 1 calc R . . H11B H 0.0997 0.1231 0.0329 0.115 Uiso 1 1 calc R . . C12S C 0.1615(3) 0.1145(6) 0.1189(3) 0.122(2) Uani 1 1 d DU . . H12A H 0.1847 0.0951 0.0993 0.146 Uiso 1 1 calc R . . H12B H 0.1803 0.1677 0.1468 0.146 Uiso 1 1 calc R . . C13S C 0.1541(3) 0.0342(5) 0.1518(3) 0.121(2) Uani 1 1 d DU . . H13D H 0.1633 0.0516 0.1937 0.145 Uiso 1 1 calc R . . H13E H 0.1764 -0.0217 0.1517 0.145 Uiso 1 1 calc R . . C14S C 0.0931(3) 0.0166(4) 0.1149(4) 0.128(3) Uani 1 1 d DU . . H14A H 0.0868 -0.0298 0.0826 0.154 Uiso 1 1 calc R . . H14B H 0.0770 -0.0096 0.1405 0.154 Uiso 1 1 calc R . . O2S O 0.23628(17) 0.4276(4) 0.5371(2) 0.0608(15) Uani 0.594(7) 1 d PDU A 1 C21S C 0.2850(2) 0.4604(5) 0.5848(3) 0.064(2) Uani 0.594(7) 1 d PDU A 1 H21A H 0.2836 0.4506 0.6233 0.076 Uiso 0.594(7) 1 calc PR A 1 H21B H 0.2901 0.5292 0.5801 0.076 Uiso 0.594(7) 1 calc PR A 1 C22S C 0.3314(2) 0.4038(5) 0.5835(4) 0.0466(15) Uani 0.594(7) 1 d PDU A 1 H22A H 0.3619 0.3946 0.6243 0.056 Uiso 0.594(7) 1 calc PR A 1 H22B H 0.3461 0.4348 0.5580 0.056 Uiso 0.594(7) 1 calc PR A 1 C23S C 0.3034(4) 0.3109(5) 0.5568(4) 0.058(2) Uani 0.594(7) 1 d PDU A 1 H23D H 0.3015 0.2685 0.5875 0.070 Uiso 0.594(7) 1 calc PR A 1 H23E H 0.3222 0.2772 0.5363 0.070 Uiso 0.594(7) 1 calc PR A 1 C24S C 0.2469(4) 0.3453(6) 0.5128(4) 0.065(3) Uani 0.594(7) 1 d PDU A 1 H24A H 0.2461 0.3594 0.4736 0.077 Uiso 0.594(7) 1 calc PR A 1 H24B H 0.2186 0.2961 0.5068 0.077 Uiso 0.594(7) 1 calc PR A 1 O2P O 0.2572(3) 0.2843(6) 0.5194(3) 0.0545(19) Uani 0.406(7) 1 d PDU A 2 C21P C 0.2463(5) 0.3803(8) 0.5060(6) 0.061(3) Uani 0.406(7) 1 d PDU A 2 H21C H 0.2122 0.3985 0.5088 0.073 Uiso 0.406(7) 1 calc PR A 2 H21D H 0.2404 0.3927 0.4646 0.073 Uiso 0.406(7) 1 calc PR A 2 C22P C 0.2946(5) 0.4386(7) 0.5498(5) 0.073(3) Uani 0.406(7) 1 d PDU A 2 H22C H 0.3187 0.4592 0.5317 0.088 Uiso 0.406(7) 1 calc PR A 2 H22D H 0.2817 0.4957 0.5632 0.088 Uiso 0.406(7) 1 calc PR A 2 C23P C 0.3240(5) 0.3724(8) 0.6001(5) 0.059(3) Uani 0.406(7) 1 d PDU A 2 H23F H 0.3092 0.3753 0.6298 0.070 Uiso 0.406(7) 1 calc PR A 2 H23G H 0.3643 0.3856 0.6204 0.070 Uiso 0.406(7) 1 calc PR A 2 C24P C 0.3116(5) 0.2780(7) 0.5678(5) 0.055(3) Uani 0.406(7) 1 d PDU A 2 H24C H 0.3388 0.2647 0.5524 0.066 Uiso 0.406(7) 1 calc PR A 2 H24D H 0.3134 0.2259 0.5954 0.066 Uiso 0.406(7) 1 calc PR A 2 O3S O 0.5521(4) 1.0459(7) 0.5106(5) 0.159(4) Uani 0.50 1 d PGDU B -1 C31S C 0.5100(4) 1.0203(6) 0.4530(4) 0.112(4) Uani 0.50 1 d PGDU B -1 H31A H 0.4953 1.0781 0.4280 0.134 Uiso 0.50 1 calc PR B -1 H31B H 0.5253 0.9774 0.4327 0.134 Uiso 0.50 1 calc PR B -1 C32S C 0.4672(4) 0.9734(6) 0.4608(4) 0.086(3) Uani 0.50 1 d PGDU B -1 H32A H 0.4620 0.9080 0.4442 0.104 Uiso 0.50 1 calc PR B -1 H32B H 0.4320 1.0086 0.4395 0.104 Uiso 0.50 1 calc PR B -1 C33S C 0.4828(5) 0.9700(6) 0.5232(4) 0.101(3) Uani 0.50 1 d PGDU B -1 H33D H 0.4851 0.9030 0.5365 0.121 Uiso 0.50 1 calc PR B -1 H33E H 0.4550 1.0036 0.5318 0.121 Uiso 0.50 1 calc PR B -1 C34S C 0.5352(5) 1.0148(7) 0.5540(3) 0.119(4) Uani 0.50 1 d PGDU B -1 H34A H 0.5626 0.9693 0.5820 0.143 Uiso 0.50 1 calc PR B -1 H34B H 0.5326 1.0699 0.5773 0.143 Uiso 0.50 1 calc PR B -1 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 Nb1 0.01127(8) 0.01278(8) 0.01469(9) 0.00104(6) 0.00504(7) -0.00001(6) Cu1 0.02168(15) 0.02588(14) 0.03185(17) -0.00007(11) 0.01643(13) -0.00530(11) P1 0.0127(2) 0.0139(2) 0.0147(2) -0.00066(17) 0.00557(19) -0.00099(17) O1 0.0135(7) 0.0179(7) 0.0158(7) -0.0009(5) 0.0062(6) -0.0012(5) O2 0.0140(7) 0.0148(6) 0.0188(7) 0.0000(5) 0.0073(6) 0.0002(5) O3 0.0125(7) 0.0158(6) 0.0177(7) 0.0014(5) 0.0052(6) -0.0015(5) N1 0.0148(8) 0.0165(8) 0.0176(9) 0.0021(6) 0.0070(7) 0.0005(6) N2 0.0149(8) 0.0134(7) 0.0200(9) 0.0003(6) 0.0073(7) -0.0006(6) N3 0.0137(8) 0.0163(8) 0.0177(8) 0.0012(6) 0.0068(7) 0.0011(6) N4 0.0194(9) 0.0215(9) 0.0299(11) -0.0005(7) 0.0131(8) -0.0019(7) C5 0.0135(9) 0.0143(8) 0.0152(9) 0.0008(7) 0.0039(7) 0.0002(7) C6 0.0134(9) 0.0164(9) 0.0155(9) -0.0006(7) 0.0062(8) 0.0001(7) C7 0.0144(9) 0.0135(8) 0.0166(9) -0.0003(7) 0.0070(8) 0.0005(7) C18 0.0213(11) 0.0227(10) 0.0194(11) 0.0060(8) 0.0070(9) 0.0042(8) C16 0.0201(10) 0.0182(10) 0.0249(11) 0.0042(8) 0.0091(9) 0.0002(8) C13 0.0233(12) 0.0339(13) 0.0306(13) 0.0122(10) 0.0113(10) -0.0024(9) C11 0.0157(10) 0.0183(9) 0.0201(10) 0.0062(7) 0.0063(8) 0.0009(7) C14 0.0278(13) 0.0239(12) 0.0410(15) 0.0098(10) 0.0109(11) -0.0057(9) C151 0.0477(18) 0.0183(11) 0.072(2) -0.0071(12) 0.0316(17) -0.0091(11) C12 0.0203(11) 0.0259(11) 0.0258(12) 0.0080(9) 0.0104(9) 0.0015(8) C131 0.0309(15) 0.0504(18) 0.0503(18) 0.0146(14) 0.0227(14) -0.0053(12) C182 0.0243(13) 0.0519(17) 0.0337(14) 0.0155(12) 0.0145(11) 0.0165(11) C183 0.0385(15) 0.0316(13) 0.0227(13) 0.0055(10) 0.0004(11) -0.0013(11) C17 0.0218(10) 0.0183(9) 0.0173(10) 0.0041(7) 0.0084(8) 0.0023(8) C181 0.0334(14) 0.0240(11) 0.0288(13) 0.0093(9) 0.0097(11) 0.0047(9) C15 0.0277(12) 0.0178(10) 0.0378(14) 0.0043(9) 0.0120(11) -0.0025(9) C21 0.0138(9) 0.0203(9) 0.0171(10) -0.0010(7) 0.0051(8) -0.0012(7) C23 0.0199(11) 0.0383(13) 0.0235(12) 0.0002(10) 0.0095(9) -0.0077(9) C251 0.0233(12) 0.0391(14) 0.0311(14) 0.0026(11) 0.0076(11) 0.0123(10) C22 0.0182(10) 0.0250(11) 0.0232(11) 0.0020(8) 0.0074(9) -0.0036(8) C27 0.0148(9) 0.0163(9) 0.0213(10) -0.0025(7) 0.0046(8) 0.0002(7) C26 0.0173(10) 0.0206(10) 0.0155(10) -0.0009(7) 0.0059(8) 0.0007(7) C231 0.0263(14) 0.0585(19) 0.0420(17) 0.0090(14) 0.0155(13) -0.0145(13) C28 0.0202(11) 0.0213(10) 0.0211(11) -0.0043(8) 0.0054(9) 0.0003(8) C282 0.0241(12) 0.0344(13) 0.0297(13) -0.0098(10) 0.0059(10) 0.0067(10) C281 0.0529(18) 0.0337(14) 0.0242(13) -0.0058(10) 0.0188(13) -0.0138(12) C25 0.0191(11) 0.0326(12) 0.0186(11) -0.0013(9) 0.0055(9) 0.0048(9) C283 0.0232(12) 0.0383(14) 0.0233(12) -0.0059(10) 0.0027(10) 0.0071(10) C24 0.0138(10) 0.0450(14) 0.0234(12) -0.0020(10) 0.0070(9) -0.0009(9) C33 0.0255(11) 0.0223(10) 0.0225(11) 0.0043(8) 0.0129(9) 0.0044(8) C37 0.0159(9) 0.0165(9) 0.0200(10) 0.0022(7) 0.0080(8) 0.0028(7) C31 0.0164(10) 0.0155(9) 0.0221(10) 0.0017(7) 0.0101(8) 0.0023(7) C382 0.0253(12) 0.0191(10) 0.0340(13) 0.0064(9) 0.0150(10) 0.0065(8) C36 0.0182(10) 0.0234(10) 0.0236(11) 0.0013(8) 0.0091(9) -0.0002(8) C32 0.0188(10) 0.0162(9) 0.0245(11) 0.0025(8) 0.0103(9) 0.0019(7) C35 0.0204(11) 0.0301(12) 0.0334(13) 0.0051(9) 0.0162(10) -0.0001(9) C351 0.0253(14) 0.0559(18) 0.0460(17) 0.0066(14) 0.0212(13) -0.0062(12) C381 0.0308(13) 0.0218(11) 0.0314(13) 0.0016(9) 0.0182(11) 0.0070(9) C38 0.0169(10) 0.0173(9) 0.0262(11) 0.0003(8) 0.0100(9) 0.0020(7) C383 0.0224(12) 0.0212(11) 0.0367(14) -0.0012(9) 0.0101(10) 0.0002(8) C331 0.0358(14) 0.0376(14) 0.0225(12) 0.0043(10) 0.0153(11) 0.0022(11) C34 0.0280(12) 0.0304(12) 0.0306(13) 0.0080(10) 0.0204(11) 0.0035(9) C42 0.0516(18) 0.0304(13) 0.0450(17) 0.0070(12) 0.0320(15) 0.0016(12) C43 0.0496(19) 0.0431(17) 0.068(2) -0.0099(15) 0.0437(18) -0.0162(14) C41 0.0266(12) 0.0263(12) 0.0362(14) 0.0036(10) 0.0156(11) 0.0034(9) C45 0.0228(12) 0.0469(16) 0.0310(14) -0.0014(11) 0.0105(11) -0.0007(11) C44 0.0226(14) 0.063(2) 0.053(2) -0.0116(16) 0.0175(14) -0.0129(13) C50 0.0146(9) 0.0157(9) 0.0156(9) -0.0001(7) 0.0048(8) -0.0002(7) C521 0.0200(10) 0.0172(9) 0.0186(10) -0.0039(7) 0.0099(8) -0.0025(7) C522 0.0247(11) 0.0247(11) 0.0210(11) -0.0024(8) 0.0099(9) -0.0041(8) C526 0.0212(11) 0.0253(11) 0.0266(12) -0.0034(9) 0.0124(9) -0.0015(8) C511 0.0143(9) 0.0168(9) 0.0203(10) -0.0011(7) 0.0060(8) 0.0016(7) C512 0.0187(10) 0.0208(10) 0.0234(11) -0.0036(8) 0.0085(9) -0.0002(8) C525 0.0235(12) 0.0345(13) 0.0393(15) -0.0065(11) 0.0193(11) -0.0051(10) C514 0.0243(12) 0.0163(10) 0.0448(15) -0.0035(9) 0.0136(11) 0.0015(8) C515 0.0263(12) 0.0189(10) 0.0399(14) 0.0054(9) 0.0151(11) 0.0024(8) C524 0.0366(15) 0.0399(14) 0.0359(15) -0.0077(11) 0.0253(13) -0.0135(11) C513 0.0206(11) 0.0211(10) 0.0326(13) -0.0079(9) 0.0098(10) 0.0008(8) C523 0.0384(15) 0.0329(13) 0.0237(12) -0.0018(10) 0.0163(11) -0.0094(11) C516 0.0193(10) 0.0196(10) 0.0259(11) 0.0015(8) 0.0099(9) 0.0022(8) C60 0.0153(9) 0.0166(9) 0.0171(10) 0.0002(7) 0.0069(8) -0.0007(7) C612 0.0237(11) 0.0196(10) 0.0297(12) 0.0050(8) 0.0139(10) 0.0028(8) C626 0.0229(11) 0.0172(9) 0.0231(11) -0.0005(8) 0.0120(9) -0.0029(8) C624 0.0217(11) 0.0202(10) 0.0345(13) -0.0021(9) 0.0123(10) -0.0055(8) C622 0.0223(11) 0.0186(9) 0.0251(11) 0.0030(8) 0.0123(9) 0.0004(8) C613 0.0306(13) 0.0244(11) 0.0339(14) 0.0113(10) 0.0163(11) 0.0100(9) C625 0.0236(11) 0.0223(10) 0.0249(12) -0.0018(8) 0.0096(9) -0.0041(8) C614 0.0274(13) 0.0374(14) 0.0243(12) 0.0104(10) 0.0067(10) 0.0121(10) C615 0.0240(12) 0.0379(13) 0.0199(12) 0.0028(10) 0.0028(10) 0.0040(10) C611 0.0185(10) 0.0193(9) 0.0184(10) 0.0042(7) 0.0087(8) 0.0021(7) C623 0.0261(12) 0.0200(10) 0.0326(13) 0.0025(9) 0.0178(10) -0.0027(8) C616 0.0218(11) 0.0238(10) 0.0188(11) 0.0024(8) 0.0059(9) 0.0016(8) C621 0.0171(10) 0.0133(8) 0.0231(11) 0.0015(7) 0.0099(8) 0.0002(7) C70 0.0139(9) 0.0168(9) 0.0171(10) -0.0010(7) 0.0064(8) -0.0001(7) C726 0.0216(11) 0.0325(12) 0.0264(12) -0.0108(9) 0.0099(10) -0.0023(9) C721 0.0179(10) 0.0205(10) 0.0176(10) -0.0032(7) 0.0071(8) -0.0035(7) C716 0.0176(10) 0.0210(10) 0.0214(11) -0.0012(8) 0.0051(9) -0.0007(8) C715 0.0174(11) 0.0261(11) 0.0265(12) 0.0016(9) 0.0055(9) -0.0037(8) C713 0.0195(11) 0.0292(11) 0.0271(12) -0.0012(9) 0.0091(9) 0.0058(9) C714 0.0131(10) 0.0369(13) 0.0284(12) 0.0035(10) 0.0075(9) 0.0024(9) C712 0.0143(10) 0.0220(10) 0.0214(11) -0.0021(8) 0.0046(8) 0.0008(7) C725 0.0318(14) 0.0513(17) 0.0362(15) -0.0205(13) 0.0205(12) -0.0071(12) C711 0.0129(9) 0.0201(9) 0.0157(10) -0.0001(7) 0.0036(8) -0.0006(7) C722 0.0233(12) 0.0327(12) 0.0193(11) 0.0000(9) 0.0060(9) -0.0013(9) C724 0.0467(18) 0.0568(18) 0.0272(14) -0.0185(13) 0.0222(13) -0.0165(14) C723 0.0364(15) 0.0469(16) 0.0179(12) -0.0046(10) 0.0067(11) -0.0087(12) O1S 0.078(2) 0.080(2) 0.107(3) 0.003(2) 0.030(2) -0.0028(19) C11S 0.145(5) 0.085(4) 0.079(3) -0.008(3) 0.070(4) -0.024(3) C12S 0.108(4) 0.169(7) 0.113(5) -0.036(5) 0.071(4) -0.007(5) C13S 0.139(5) 0.126(5) 0.084(4) -0.010(3) 0.040(4) 0.084(4) C14S 0.143(5) 0.055(3) 0.189(8) 0.011(4) 0.078(5) 0.004(3) O2S 0.034(2) 0.095(4) 0.044(3) -0.012(2) 0.0090(18) 0.010(2) C21S 0.038(3) 0.080(5) 0.064(4) -0.031(4) 0.015(3) 0.011(3) C22S 0.034(3) 0.051(4) 0.060(4) 0.004(3) 0.025(3) 0.006(3) C23S 0.083(6) 0.044(4) 0.059(5) 0.008(3) 0.042(4) 0.010(3) C24S 0.097(6) 0.040(4) 0.028(4) -0.005(3) 0.003(3) -0.011(4) O2P 0.050(4) 0.067(4) 0.035(3) 0.006(3) 0.009(3) -0.009(3) C21P 0.068(6) 0.068(7) 0.028(5) 0.013(6) 0.006(4) 0.021(6) C22P 0.106(9) 0.044(4) 0.054(6) 0.002(4) 0.022(6) 0.001(5) C23P 0.046(5) 0.066(6) 0.053(6) 0.000(4) 0.013(4) -0.008(5) C24P 0.047(5) 0.055(6) 0.047(6) 0.007(5) 0.008(4) 0.001(5) O3S 0.143(7) 0.173(8) 0.159(8) 0.023(7) 0.067(6) -0.062(6) C31S 0.142(8) 0.080(7) 0.149(6) -0.005(7) 0.098(6) -0.050(6) C32S 0.100(6) 0.047(4) 0.146(6) 0.040(5) 0.085(5) 0.004(4) C33S 0.167(7) 0.046(4) 0.152(7) -0.058(5) 0.127(6) -0.028(5) C34S 0.113(8) 0.123(9) 0.148(6) 0.001(7) 0.082(6) 0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N3 2.0291(17) . ? Nb1 N2 2.0322(18) . ? Nb1 N1 2.0348(18) . ? Nb1 O2 2.0956(15) . ? Nb1 O3 2.0976(15) . ? Nb1 O1 2.1051(15) . ? Cu1 N4 1.931(2) . ? Cu1 P1 2.1757(6) . ? P1 C5 1.844(2) . ? P1 C7 1.850(2) . ? P1 C6 1.856(2) . ? O1 C7 1.321(2) . ? O2 C5 1.323(3) . ? O3 C6 1.324(2) . ? N1 C11 1.439(3) . ? N1 C17 1.483(3) . ? N2 C21 1.443(3) . ? N2 C27 1.482(3) . ? N3 C31 1.439(3) . ? N3 C37 1.487(3) . ? N4 C45 1.337(3) . ? N4 C41 1.340(3) . ? C5 C50 1.369(3) . ? C6 C60 1.374(3) . ? C7 C70 1.370(3) . ? C18 C182 1.525(4) . ? C18 C181 1.536(3) . ? C18 C183 1.538(4) . ? C18 C17 1.547(3) . ? C16 C11 1.395(3) . ? C16 C15 1.396(3) . ? C13 C14 1.390(4) . ? C13 C12 1.402(3) . ? C13 C131 1.515(4) . ? C11 C12 1.396(3) . ? C14 C15 1.396(4) . ? C151 C15 1.516(4) . ? C21 C26 1.394(3) . ? C21 C22 1.400(3) . ? C23 C24 1.392(4) . ? C23 C22 1.395(3) . ? C23 C231 1.513(4) . ? C251 C25 1.509(3) . ? C27 C28 1.555(3) . ? C26 C25 1.390(3) . ? C28 C281 1.521(4) . ? C28 C283 1.531(3) . ? C28 C282 1.540(3) . ? C25 C24 1.395(4) . ? C33 C34 1.396(3) . ? C33 C32 1.401(3) . ? C33 C331 1.504(4) . ? C37 C38 1.550(3) . ? C31 C32 1.391(3) . ? C31 C36 1.401(3) . ? C382 C38 1.542(3) . ? C36 C35 1.396(3) . ? C35 C34 1.393(4) . ? C35 C351 1.520(4) . ? C381 C38 1.535(3) . ? C38 C383 1.528(3) . ? C42 C43 1.374(5) . ? C42 C41 1.375(4) . ? C43 C44 1.367(5) . ? C45 C44 1.393(4) . ? C50 C511 1.486(3) . ? C50 C521 1.494(3) . ? C521 C522 1.398(3) . ? C521 C526 1.406(3) . ? C522 C523 1.403(3) . ? C526 C525 1.393(3) . ? C511 C516 1.404(3) . ? C511 C512 1.410(3) . ? C512 C513 1.392(3) . ? C525 C524 1.382(4) . ? C514 C515 1.384(4) . ? C514 C513 1.388(4) . ? C515 C516 1.395(3) . ? C524 C523 1.387(4) . ? C60 C611 1.482(3) . ? C60 C621 1.489(3) . ? C612 C613 1.385(3) . ? C612 C611 1.405(3) . ? C626 C625 1.396(3) . ? C626 C621 1.402(3) . ? C624 C623 1.385(4) . ? C624 C625 1.387(3) . ? C622 C623 1.390(3) . ? C622 C621 1.401(3) . ? C613 C614 1.389(4) . ? C614 C615 1.389(4) . ? C615 C616 1.392(3) . ? C611 C616 1.403(3) . ? C70 C711 1.481(3) . ? C70 C721 1.485(3) . ? C726 C725 1.392(4) . ? C726 C721 1.394(3) . ? C721 C722 1.408(3) . ? C716 C715 1.390(3) . ? C716 C711 1.411(3) . ? C715 C714 1.389(4) . ? C713 C714 1.390(4) . ? C713 C712 1.392(3) . ? C712 C711 1.399(3) . ? C725 C724 1.380(4) . ? C722 C723 1.388(4) . ? C724 C723 1.379(5) . ? O1S C14S 1.393(6) . ? O1S C11S 1.411(6) . ? C11S C12S 1.477(8) . ? C12S C13S 1.460(9) . ? C13S C14S 1.506(8) . ? O2S C24S 1.392(9) . ? O2S C21S 1.397(7) . ? C21S C22S 1.499(8) . ? C22S C23S 1.504(9) . ? C23S C24S 1.505(10) . ? O2P C21P 1.387(10) . ? O2P C24P 1.424(10) . ? C21P C22P 1.513(12) . ? C22P C23P 1.473(11) . ? C23P C24P 1.508(12) . ? O3S C31S 1.4200 . ? O3S C34S 1.4200 . ? C31S C32S 1.4200 . ? C32S C33S 1.4200 . ? C33S C34S 1.4200 . ? 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 N3 Nb1 N2 97.91(7) . . ? N3 Nb1 N1 95.64(7) . . ? N2 Nb1 N1 97.86(7) . . ? N3 Nb1 O2 169.22(6) . . ? N2 Nb1 O2 87.03(6) . . ? N1 Nb1 O2 93.14(6) . . ? N3 Nb1 O3 88.92(6) . . ? N2 Nb1 O3 92.67(6) . . ? N1 Nb1 O3 167.82(6) . . ? O2 Nb1 O3 81.26(6) . . ? N3 Nb1 O1 93.10(6) . . ? N2 Nb1 O1 167.28(7) . . ? N1 Nb1 O1 87.34(6) . . ? O2 Nb1 O1 81.07(6) . . ? O3 Nb1 O1 81.13(6) . . ? N4 Cu1 P1 172.43(6) . . ? C5 P1 C7 99.39(9) . . ? C5 P1 C6 101.20(9) . . ? C7 P1 C6 97.16(9) . . ? C5 P1 Cu1 115.43(7) . . ? C7 P1 Cu1 123.62(7) . . ? C6 P1 Cu1 116.15(7) . . ? C7 O1 Nb1 132.13(13) . . ? C5 O2 Nb1 131.06(12) . . ? C6 O3 Nb1 127.72(13) . . ? C11 N1 C17 111.60(17) . . ? C11 N1 Nb1 121.65(14) . . ? C17 N1 Nb1 126.55(13) . . ? C21 N2 C27 111.53(16) . . ? C21 N2 Nb1 120.66(14) . . ? C27 N2 Nb1 127.43(13) . . ? C31 N3 C37 111.40(16) . . ? C31 N3 Nb1 121.35(13) . . ? C37 N3 Nb1 126.79(14) . . ? C45 N4 C41 117.4(2) . . ? C45 N4 Cu1 122.47(19) . . ? C41 N4 Cu1 120.16(17) . . ? O2 C5 C50 124.73(18) . . ? O2 C5 P1 114.40(14) . . ? C50 C5 P1 120.61(16) . . ? O3 C6 C60 125.40(19) . . ? O3 C6 P1 114.50(14) . . ? C60 C6 P1 120.00(16) . . ? O1 C7 C70 124.92(19) . . ? O1 C7 P1 112.32(14) . . ? C70 C7 P1 122.07(16) . . ? C182 C18 C181 110.3(2) . . ? C182 C18 C183 109.7(2) . . ? C181 C18 C183 107.2(2) . . ? C182 C18 C17 110.08(19) . . ? C181 C18 C17 113.8(2) . . ? C183 C18 C17 105.65(19) . . ? C11 C16 C15 120.9(2) . . ? C14 C13 C12 118.9(2) . . ? C14 C13 C131 121.3(2) . . ? C12 C13 C131 119.8(3) . . ? C16 C11 C12 119.5(2) . . ? C16 C11 N1 119.90(19) . . ? C12 C11 N1 120.6(2) . . ? C13 C14 C15 121.6(2) . . ? C11 C12 C13 120.5(2) . . ? N1 C17 C18 118.72(18) . . ? C14 C15 C16 118.6(2) . . ? C14 C15 C151 121.8(2) . . ? C16 C15 C151 119.6(2) . . ? C26 C21 C22 119.2(2) . . ? C26 C21 N2 120.47(19) . . ? C22 C21 N2 120.34(19) . . ? C24 C23 C22 118.9(2) . . ? C24 C23 C231 121.0(2) . . ? C22 C23 C231 120.2(2) . . ? C23 C22 C21 120.6(2) . . ? N2 C27 C28 118.41(17) . . ? C25 C26 C21 121.1(2) . . ? C281 C28 C283 110.2(2) . . ? C281 C28 C282 109.7(2) . . ? C283 C28 C282 106.95(19) . . ? C281 C28 C27 110.18(19) . . ? C283 C28 C27 114.1(2) . . ? C282 C28 C27 105.49(19) . . ? C26 C25 C24 118.7(2) . . ? C26 C25 C251 120.2(2) . . ? C24 C25 C251 121.1(2) . . ? C23 C24 C25 121.5(2) . . ? C34 C33 C32 118.4(2) . . ? C34 C33 C331 121.5(2) . . ? C32 C33 C331 120.2(2) . . ? N3 C37 C38 119.93(18) . . ? C32 C31 C36 119.4(2) . . ? C32 C31 N3 120.34(19) . . ? C36 C31 N3 120.2(2) . . ? C35 C36 C31 120.1(2) . . ? C31 C32 C33 121.3(2) . . ? C34 C35 C36 119.6(2) . . ? C34 C35 C351 120.9(2) . . ? C36 C35 C351 119.6(2) . . ? C383 C38 C381 110.8(2) . . ? C383 C38 C382 109.74(19) . . ? C381 C38 C382 106.63(18) . . ? C383 C38 C37 110.54(18) . . ? C381 C38 C37 113.86(18) . . ? C382 C38 C37 104.94(18) . . ? C35 C34 C33 121.3(2) . . ? C43 C42 C41 119.0(3) . . ? C44 C43 C42 118.8(3) . . ? N4 C41 C42 123.3(3) . . ? N4 C45 C44 122.3(3) . . ? C43 C44 C45 119.2(3) . . ? C5 C50 C511 122.41(19) . . ? C5 C50 C521 123.27(18) . . ? C511 C50 C521 114.00(18) . . ? C522 C521 C526 117.7(2) . . ? C522 C521 C50 120.9(2) . . ? C526 C521 C50 120.6(2) . . ? C521 C522 C523 121.2(2) . . ? C525 C526 C521 120.9(2) . . ? C516 C511 C512 117.6(2) . . ? C516 C511 C50 122.5(2) . . ? C512 C511 C50 119.9(2) . . ? C513 C512 C511 121.0(2) . . ? C524 C525 C526 120.5(2) . . ? C515 C514 C513 119.4(2) . . ? C514 C515 C516 120.8(2) . . ? C525 C524 C523 119.8(2) . . ? C514 C513 C512 120.4(2) . . ? C524 C523 C522 119.9(3) . . ? C515 C516 C511 120.7(2) . . ? C6 C60 C611 123.63(19) . . ? C6 C60 C621 118.84(19) . . ? C611 C60 C621 117.26(18) . . ? C613 C612 C611 121.6(2) . . ? C625 C626 C621 121.4(2) . . ? C623 C624 C625 119.7(2) . . ? C623 C622 C621 120.5(2) . . ? C612 C613 C614 120.3(2) . . ? C624 C625 C626 119.6(2) . . ? C615 C614 C613 119.1(2) . . ? C614 C615 C616 120.7(2) . . ? C616 C611 C612 117.3(2) . . ? C616 C611 C60 121.71(19) . . ? C612 C611 C60 120.9(2) . . ? C624 C623 C622 120.9(2) . . ? C615 C616 C611 120.9(2) . . ? C622 C621 C626 117.9(2) . . ? C622 C621 C60 122.5(2) . . ? C626 C621 C60 119.52(19) . . ? C7 C70 C711 120.86(19) . . ? C7 C70 C721 121.64(19) . . ? C711 C70 C721 117.44(18) . . ? C725 C726 C721 121.2(2) . . ? C726 C721 C722 117.4(2) . . ? C726 C721 C70 121.5(2) . . ? C722 C721 C70 121.1(2) . . ? C715 C716 C711 121.0(2) . . ? C714 C715 C716 120.3(2) . . ? C714 C713 C712 120.2(2) . . ? C715 C714 C713 119.6(2) . . ? C713 C712 C711 121.4(2) . . ? C724 C725 C726 120.2(3) . . ? C712 C711 C716 117.5(2) . . ? C712 C711 C70 120.68(19) . . ? C716 C711 C70 121.71(19) . . ? C723 C722 C721 121.2(2) . . ? C723 C724 C725 120.0(3) . . ? C724 C723 C722 120.0(3) . . ? C14S O1S C11S 103.0(5) . . ? O1S C11S C12S 105.4(5) . . ? C13S C12S C11S 108.3(5) . . ? C12S C13S C14S 100.0(5) . . ? O1S C14S C13S 107.7(5) . . ? C24S O2S C21S 110.1(5) . . ? O2S C21S C22S 106.6(5) . . ? C21S C22S C23S 102.0(6) . . ? C22S C23S C24S 100.9(5) . . ? O2S C24S C23S 106.8(6) . . ? C21P O2P C24P 107.0(8) . . ? O2P C21P C22P 109.2(8) . . ? C23P C22P C21P 103.5(8) . . ? C22P C23P C24P 101.2(8) . . ? O2P C24P C23P 107.2(8) . . ? C31S O3S C34S 108.0 . . ? C32S C31S O3S 108.0 . . ? C31S C32S C33S 108.0 . . ? C32S C33S C34S 108.0 . . ? C33S C34S O3S 108.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.718 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.089 data_r3 _database_code_depnum_ccdc_archive 'CCDC 789473' #TrackingRef '2155_web_deposit_cif_file_0_SidCreutz_1281986427.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Na(thf)6][(Ar[Np]N)3Nb(OC[CPh2])3P]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C105 H138 N3 Na Nb O9 P' _chemical_formula_weight 1733.05 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.736(2) _cell_length_b 17.736(2) _cell_length_c 51.913(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14143(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9835 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.26 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5568 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9518 _exptl_absorpt_correction_T_max 0.9856 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 94854 _diffrn_reflns_av_R_equivalents 0.1119 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -69 _diffrn_reflns_limit_l_max 69 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 28.37 _reflns_number_total 7872 _reflns_number_gt 5983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+43.9684P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7872 _refine_ls_number_parameters 416 _refine_ls_number_restraints 270 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.6667 0.3333 0.069293(6) 0.01726(9) Uani 1 3 d S . . P1 P 0.6667 0.3333 0.138867(19) 0.0232(2) Uani 1 3 d S . . O1 O 0.58627(10) 0.23975(10) 0.09503(3) 0.0220(3) Uani 1 1 d . . . N1 N 0.55587(11) 0.30888(11) 0.04961(3) 0.0185(4) Uani 1 1 d . . . C1 C 0.58200(15) 0.23790(15) 0.12063(4) 0.0227(4) Uani 1 1 d D A . C2 C 0.51923(16) 0.16820(15) 0.13398(4) 0.0245(5) Uani 1 1 d DU . . C31 C 0.5155(4) 0.1732(4) 0.16260(12) 0.0265(14) Uani 0.617(14) 1 d PDU A 1 C32 C 0.4637(5) 0.2025(5) 0.17374(13) 0.0327(13) Uani 0.617(14) 1 d PDU A 1 H32 H 0.4318 0.2202 0.1631 0.039 Uiso 0.617(14) 1 calc PR A 1 C33 C 0.4582(5) 0.2062(6) 0.20033(13) 0.0416(15) Uani 0.617(14) 1 d PDU A 1 H33 H 0.4194 0.2220 0.2080 0.050 Uiso 0.617(14) 1 calc PR A 1 C34 C 0.5109(9) 0.1863(9) 0.21574(19) 0.0475(14) Uani 0.617(14) 1 d PDU A 1 H34 H 0.5131 0.1956 0.2338 0.057 Uiso 0.617(14) 1 calc PR A 1 C35 C 0.5591(6) 0.1538(6) 0.20503(12) 0.0444(16) Uani 0.617(14) 1 d PDU A 1 H35 H 0.5911 0.1363 0.2157 0.053 Uiso 0.617(14) 1 calc PR A 1 C36 C 0.5609(6) 0.1468(6) 0.17850(11) 0.0378(15) Uani 0.617(14) 1 d PDU A 1 H36 H 0.5938 0.1234 0.1711 0.045 Uiso 0.617(14) 1 calc PR A 1 C31A C 0.5125(6) 0.1730(7) 0.16287(18) 0.030(2) Uani 0.383(14) 1 d PDU A 2 C32A C 0.4929(9) 0.2307(9) 0.1754(2) 0.039(2) Uani 0.383(14) 1 d PDU A 2 H32A H 0.4806 0.2681 0.1654 0.046 Uiso 0.383(14) 1 calc PR A 2 C33A C 0.4910(10) 0.2350(9) 0.2020(2) 0.049(2) Uani 0.383(14) 1 d PDU A 2 H33A H 0.4840 0.2792 0.2100 0.058 Uiso 0.383(14) 1 calc PR A 2 C34A C 0.4993(16) 0.1747(13) 0.2169(3) 0.0475(14) Uani 0.383(14) 1 d PDU A 2 H34A H 0.4893 0.1716 0.2350 0.057 Uiso 0.383(14) 1 calc PR A 2 C35A C 0.5220(9) 0.1197(9) 0.20528(18) 0.043(2) Uani 0.383(14) 1 d PDU A 2 H35A H 0.5355 0.0834 0.2154 0.052 Uiso 0.383(14) 1 calc PR A 2 C36A C 0.5253(9) 0.1171(8) 0.17883(18) 0.039(2) Uani 0.383(14) 1 d PDU A 2 H36A H 0.5367 0.0753 0.1711 0.047 Uiso 0.383(14) 1 calc PR A 2 C181 C 0.3739(2) 0.3037(2) 0.05152(6) 0.0425(7) Uani 1 1 d . . . H18A H 0.3232 0.3031 0.0592 0.064 Uiso 1 1 calc R . . H18B H 0.3606 0.2832 0.0337 0.064 Uiso 1 1 calc R . . H18C H 0.4236 0.3632 0.0518 0.064 Uiso 1 1 calc R . . C21 C 0.45159(15) 0.08673(15) 0.12181(4) 0.0233(5) Uani 1 1 d . A . C12 C 0.58260(15) 0.44494(15) 0.02887(4) 0.0232(5) Uani 1 1 d . . . H12 H 0.5892 0.4705 0.0454 0.028 Uiso 1 1 calc R . . C17 C 0.46827(14) 0.23203(15) 0.05383(4) 0.0230(5) Uani 1 1 d . . . H17A H 0.4760 0.1898 0.0643 0.028 Uiso 1 1 calc R . . H17B H 0.4458 0.2046 0.0368 0.028 Uiso 1 1 calc R . . C11 C 0.56002(14) 0.35716(15) 0.02703(4) 0.0223(4) Uani 1 1 d . . . C182 C 0.42123(16) 0.27726(17) 0.09449(5) 0.0297(5) Uani 1 1 d . . . H18D H 0.3748 0.2844 0.1022 0.045 Uiso 1 1 calc R . . H18E H 0.4755 0.3335 0.0943 0.045 Uiso 1 1 calc R . . H18F H 0.4295 0.2353 0.1046 0.045 Uiso 1 1 calc R . . C16 C 0.54466(14) 0.31911(15) 0.00249(4) 0.0215(4) Uani 1 1 d . . . H16 H 0.5275 0.2593 0.0009 0.026 Uiso 1 1 calc R . . C151 C 0.53670(18) 0.32399(18) -0.04574(5) 0.0318(5) Uani 1 1 d . . . H15A H 0.5627 0.2866 -0.0464 0.048 Uiso 1 1 calc R . . H15B H 0.5623 0.3683 -0.0593 0.048 Uiso 1 1 calc R . . H15C H 0.4737 0.2886 -0.0484 0.048 Uiso 1 1 calc R . . C15 C 0.55435(16) 0.36805(16) -0.01959(4) 0.0257(5) Uani 1 1 d . . . C26 C 0.37163(17) 0.03347(18) 0.13410(5) 0.0337(6) Uani 1 1 d . . . H26 H 0.3607 0.0505 0.1504 0.040 Uiso 1 1 calc R A . C183 C 0.31594(16) 0.15170(18) 0.06726(5) 0.0354(6) Uani 1 1 d . . . H18G H 0.3294 0.1128 0.0772 0.053 Uiso 1 1 calc R . . H18H H 0.3005 0.1300 0.0496 0.053 Uiso 1 1 calc R . . H18I H 0.2669 0.1536 0.0753 0.053 Uiso 1 1 calc R . . C13 C 0.59553(15) 0.49534(15) 0.00701(5) 0.0253(5) Uani 1 1 d . . . C22 C 0.46504(17) 0.05732(16) 0.09815(5) 0.0300(5) Uani 1 1 d . . . H22 H 0.5188 0.0910 0.0894 0.036 Uiso 1 1 calc R A . C24 C 0.32194(17) -0.07018(17) 0.09940(5) 0.0328(6) Uani 1 1 d . . . H24 H 0.2777 -0.1220 0.0916 0.039 Uiso 1 1 calc R A . C18 C 0.39615(16) 0.24390(17) 0.06687(5) 0.0274(5) Uani 1 1 d . . . C131 C 0.62858(17) 0.59205(16) 0.00937(5) 0.0297(5) Uani 1 1 d . . . H13A H 0.6320 0.6077 0.0276 0.045 Uiso 1 1 calc R . . H13B H 0.5886 0.6063 0.0005 0.045 Uiso 1 1 calc R . . H13C H 0.6865 0.6247 0.0016 0.045 Uiso 1 1 calc R . . C14 C 0.58094(16) 0.45652(16) -0.01722(5) 0.0270(5) Uani 1 1 d . . . H14 H 0.5891 0.4904 -0.0322 0.032 Uiso 1 1 calc R . . C23 C 0.40155(18) -0.01995(17) 0.08723(5) 0.0340(6) Uani 1 1 d . A . H23 H 0.4126 -0.0387 0.0713 0.041 Uiso 1 1 calc R . . C25 C 0.30832(18) -0.04339(19) 0.12304(6) 0.0396(6) Uani 1 1 d . A . H25 H 0.2549 -0.0781 0.1318 0.047 Uiso 1 1 calc R . . Na1 Na 0.0000 0.0000 0.0000 0.0214(4) Uani 1 6 d S . . Na2 Na 0.3333 -0.3333 0.1667 0.0290(5) Uani 1 6 d S . . O1T O 0.09139(13) -0.03448(13) 0.02537(3) 0.0375(4) Uani 1 1 d . . . O1S O 0.43002(13) -0.21163(13) 0.14017(4) 0.0383(4) Uani 1 1 d . . . C4T C 0.15902(19) -0.0452(2) 0.01358(6) 0.0387(6) Uani 1 1 d . . . H4T1 H 0.2157 0.0095 0.0146 0.046 Uiso 1 1 calc R . . H4T2 H 0.1453 -0.0622 -0.0047 0.046 Uiso 1 1 calc R . . C1S C 0.4665(2) -0.2157(2) 0.11600(6) 0.0486(8) Uani 1 1 d . . . H1S1 H 0.4220 -0.2340 0.1022 0.058 Uiso 1 1 calc R . . H1S2 H 0.4866 -0.2586 0.1169 0.058 Uiso 1 1 calc R . . C1T C 0.0732(2) -0.0726(2) 0.05031(5) 0.0413(7) Uani 1 1 d . . . H1T1 H 0.0133 -0.1231 0.0509 0.050 Uiso 1 1 calc R . . H1T2 H 0.0783 -0.0296 0.0634 0.050 Uiso 1 1 calc R . . C2T C 0.1386(2) -0.1016(2) 0.05572(6) 0.0437(7) Uani 1 1 d . . . H2T1 H 0.1905 -0.0557 0.0648 0.052 Uiso 1 1 calc R . . H2T2 H 0.1125 -0.1555 0.0661 0.052 Uiso 1 1 calc R . . C4S C 0.4705(2) -0.12225(19) 0.14805(7) 0.0469(7) Uani 1 1 d . . . H4S1 H 0.4768 -0.1174 0.1670 0.056 Uiso 1 1 calc R . . H4S2 H 0.4354 -0.0960 0.1425 0.056 Uiso 1 1 calc R . . C3T C 0.1614(2) -0.1173(2) 0.02898(6) 0.0437(7) Uani 1 1 d . . . H3T1 H 0.1180 -0.1756 0.0225 0.052 Uiso 1 1 calc R . . H3T2 H 0.2200 -0.1113 0.0285 0.052 Uiso 1 1 calc R . . C3S C 0.5588(2) -0.0772(2) 0.13518(7) 0.0509(8) Uani 1 1 d . . . H3S1 H 0.5789 -0.0149 0.1321 0.061 Uiso 1 1 calc R . . H3S2 H 0.6026 -0.0822 0.1457 0.061 Uiso 1 1 calc R . . C2S C 0.5423(2) -0.1262(2) 0.11013(7) 0.0592(9) Uani 1 1 d . . . H2S1 H 0.5941 -0.1296 0.1048 0.071 Uiso 1 1 calc R . . H2S2 H 0.5272 -0.0977 0.0963 0.071 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 Nb1 0.01830(12) 0.01830(12) 0.01519(16) 0.000 0.000 0.00915(6) P1 0.0263(3) 0.0263(3) 0.0169(5) 0.000 0.000 0.01316(16) O1 0.0241(8) 0.0230(8) 0.0165(7) 0.0024(6) -0.0004(6) 0.0098(7) N1 0.0181(9) 0.0182(9) 0.0193(9) 0.0000(7) 0.0012(7) 0.0091(7) C1 0.0251(11) 0.0271(12) 0.0183(10) 0.0009(8) -0.0006(8) 0.0148(10) C2 0.0283(12) 0.0276(12) 0.0203(10) 0.0025(9) 0.0015(9) 0.0161(10) C31 0.028(3) 0.029(3) 0.022(2) 0.007(3) 0.006(3) 0.014(3) C32 0.031(3) 0.046(4) 0.0251(19) 0.006(2) 0.005(2) 0.022(3) C33 0.038(3) 0.065(4) 0.029(2) 0.004(3) 0.011(2) 0.032(3) C34 0.057(4) 0.078(3) 0.0197(14) 0.0093(17) 0.0118(17) 0.044(3) C35 0.055(4) 0.075(5) 0.022(2) 0.001(3) -0.004(3) 0.046(4) C36 0.047(4) 0.062(4) 0.0215(18) 0.002(3) 0.002(2) 0.040(3) C31A 0.034(6) 0.035(6) 0.020(3) 0.003(4) 0.001(5) 0.017(4) C32A 0.047(6) 0.048(5) 0.028(3) 0.009(3) 0.017(4) 0.030(4) C33A 0.065(7) 0.067(6) 0.030(3) 0.004(4) 0.018(5) 0.044(5) C34A 0.057(4) 0.078(3) 0.0197(14) 0.0093(17) 0.0118(17) 0.044(3) C35A 0.052(6) 0.062(6) 0.023(3) 0.010(4) 0.001(4) 0.033(4) C36A 0.051(6) 0.046(5) 0.024(3) 0.003(3) -0.004(4) 0.026(4) C181 0.0395(16) 0.0576(19) 0.0427(16) 0.0183(14) 0.0128(12) 0.0336(15) C21 0.0248(11) 0.0242(11) 0.0231(11) 0.0080(9) 0.0027(9) 0.0138(10) C12 0.0217(11) 0.0246(11) 0.0241(11) -0.0017(9) -0.0016(8) 0.0122(9) C17 0.0205(11) 0.0241(11) 0.0222(11) 0.0019(8) 0.0017(8) 0.0096(9) C11 0.0201(10) 0.0258(11) 0.0232(11) 0.0037(9) 0.0016(8) 0.0133(9) C182 0.0274(12) 0.0336(13) 0.0295(13) -0.0018(10) 0.0054(10) 0.0162(11) C16 0.0208(11) 0.0239(11) 0.0203(10) 0.0011(8) 0.0007(8) 0.0115(9) C151 0.0405(15) 0.0395(14) 0.0210(11) 0.0026(10) -0.0003(10) 0.0243(12) C15 0.0251(12) 0.0338(13) 0.0221(11) 0.0014(9) 0.0001(9) 0.0178(10) C26 0.0342(14) 0.0367(14) 0.0261(12) 0.0065(10) 0.0076(10) 0.0147(12) C183 0.0227(12) 0.0409(15) 0.0341(14) -0.0013(11) 0.0044(10) 0.0096(11) C13 0.0209(11) 0.0236(11) 0.0318(12) 0.0020(9) -0.0004(9) 0.0114(9) C22 0.0289(13) 0.0279(12) 0.0315(13) 0.0079(10) 0.0085(10) 0.0130(11) C24 0.0298(13) 0.0240(12) 0.0372(14) 0.0049(10) -0.0012(11) 0.0080(10) C18 0.0229(11) 0.0319(13) 0.0280(12) 0.0038(10) 0.0047(9) 0.0140(10) C131 0.0306(13) 0.0236(12) 0.0354(13) 0.0031(10) -0.0021(10) 0.0138(10) C14 0.0262(12) 0.0315(13) 0.0253(11) 0.0069(9) 0.0015(9) 0.0161(10) C23 0.0374(14) 0.0271(13) 0.0346(14) 0.0034(10) 0.0041(11) 0.0139(11) C25 0.0292(14) 0.0370(15) 0.0414(15) 0.0098(12) 0.0077(11) 0.0083(12) Na1 0.0221(7) 0.0221(7) 0.0200(10) 0.000 0.000 0.0110(3) Na2 0.0287(8) 0.0287(8) 0.0298(12) 0.000 0.000 0.0143(4) O1T 0.0452(11) 0.0525(12) 0.0289(9) 0.0067(8) 0.0008(8) 0.0351(10) O1S 0.0403(11) 0.0336(10) 0.0374(10) 0.0028(8) 0.0070(8) 0.0157(9) C4T 0.0337(14) 0.0446(16) 0.0410(15) 0.0050(12) 0.0027(12) 0.0219(13) C1S 0.0462(18) 0.0532(19) 0.0378(16) 0.0007(14) 0.0092(13) 0.0185(15) C1T 0.0511(18) 0.0527(18) 0.0281(13) 0.0062(12) -0.0009(12) 0.0319(15) C2T 0.0463(17) 0.0412(16) 0.0428(16) 0.0083(13) -0.0109(13) 0.0214(14) C4S 0.0449(17) 0.0339(15) 0.0558(19) 0.0030(13) 0.0111(14) 0.0151(14) C3T 0.0468(17) 0.0464(17) 0.0490(17) 0.0064(13) -0.0032(13) 0.0315(15) C3S 0.0430(17) 0.0420(17) 0.055(2) 0.0083(14) 0.0099(15) 0.0120(14) C2S 0.059(2) 0.053(2) 0.059(2) 0.0077(17) 0.0242(17) 0.0237(18) _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 Nb1 O1 2.0507(15) 2_655 ? Nb1 O1 2.0508(15) 3_665 ? Nb1 O1 2.0508(15) . ? Nb1 N1 2.0596(18) 2_655 ? Nb1 N1 2.0597(18) . ? Nb1 N1 2.0597(18) 3_665 ? P1 C1 1.864(2) . ? P1 C1 1.864(2) 2_655 ? P1 C1 1.864(2) 3_665 ? O1 C1 1.331(3) . ? N1 C11 1.432(3) . ? N1 C17 1.484(3) . ? C1 C2 1.368(3) . ? C2 C21 1.481(3) . ? C2 C31 1.492(7) . ? C2 C31A 1.510(10) . ? C31 C36 1.387(7) . ? C31 C32 1.390(7) . ? C32 C33 1.388(7) . ? C33 C34 1.403(10) . ? C34 C35 1.365(9) . ? C35 C36 1.385(7) . ? C31A C32A 1.394(11) . ? C31A C36A 1.395(11) . ? C32A C33A 1.384(11) . ? C33A C34A 1.388(12) . ? C34A C35A 1.368(12) . ? C35A C36A 1.376(10) . ? C181 C18 1.528(4) . ? C21 C22 1.401(3) . ? C21 C26 1.404(3) . ? C12 C13 1.391(3) . ? C12 C11 1.404(3) . ? C17 C18 1.552(3) . ? C11 C16 1.403(3) . ? C182 C18 1.530(3) . ? C16 C15 1.396(3) . ? C151 C15 1.519(3) . ? C15 C14 1.400(3) . ? C26 C25 1.385(4) . ? C183 C18 1.540(4) . ? C13 C14 1.395(3) . ? C13 C131 1.515(3) . ? C22 C23 1.387(4) . ? C24 C25 1.380(4) . ? C24 C23 1.389(4) . ? Na1 O1T 2.3931(18) . ? Na1 O1T 2.3931(18) 11 ? Na1 O1T 2.3931(18) 2 ? Na1 O1T 2.3931(18) 10 ? Na1 O1T 2.3931(18) 12 ? Na1 O1T 2.3931(18) 3 ? Na2 O1S 2.4062(19) 14 ? Na2 O1S 2.4063(19) 13_545 ? Na2 O1S 2.4063(19) 15_445 ? Na2 O1S 2.4063(19) . ? Na2 O1S 2.4064(19) 2_545 ? Na2 O1S 2.4064(19) 3_655 ? O1T C1T 1.421(3) . ? O1T C4T 1.441(3) . ? O1S C1S 1.430(3) . ? O1S C4S 1.434(4) . ? C4T C3T 1.526(4) . ? C1S C2S 1.513(5) . ? C1T C2T 1.512(4) . ? C2T C3T 1.510(4) . ? C4S C3S 1.511(4) . ? C3S C2S 1.508(5) . ? 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 Nb1 O1 82.16(6) 2_655 3_665 ? O1 Nb1 O1 82.16(6) 2_655 . ? O1 Nb1 O1 82.16(6) 3_665 . ? O1 Nb1 N1 87.06(7) 2_655 2_655 ? O1 Nb1 N1 168.47(7) 3_665 2_655 ? O1 Nb1 N1 92.35(7) . 2_655 ? O1 Nb1 N1 168.47(7) 2_655 . ? O1 Nb1 N1 92.35(7) 3_665 . ? O1 Nb1 N1 87.06(7) . . ? N1 Nb1 N1 97.51(6) 2_655 . ? O1 Nb1 N1 92.35(7) 2_655 3_665 ? O1 Nb1 N1 87.06(7) 3_665 3_665 ? O1 Nb1 N1 168.46(7) . 3_665 ? N1 Nb1 N1 97.51(6) 2_655 3_665 ? N1 Nb1 N1 97.51(6) . 3_665 ? C1 P1 C1 96.49(10) . 2_655 ? C1 P1 C1 96.49(10) . 3_665 ? C1 P1 C1 96.49(10) 2_655 3_665 ? C1 O1 Nb1 132.73(14) . . ? C11 N1 C17 112.81(17) . . ? C11 N1 Nb1 121.46(14) . . ? C17 N1 Nb1 124.79(14) . . ? O1 C1 C2 122.6(2) . . ? O1 C1 P1 118.35(16) . . ? C2 C1 P1 119.03(17) . . ? C1 C2 C21 124.2(2) . . ? C1 C2 C31 119.4(3) . . ? C21 C2 C31 116.4(3) . . ? C1 C2 C31A 120.2(4) . . ? C21 C2 C31A 115.5(4) . . ? C31 C2 C31A 2.0(7) . . ? C36 C31 C32 118.9(6) . . ? C36 C31 C2 121.5(6) . . ? C32 C31 C2 119.5(6) . . ? C33 C32 C31 120.4(6) . . ? C32 C33 C34 119.0(7) . . ? C35 C34 C33 120.7(8) . . ? C34 C35 C36 119.4(6) . . ? C35 C36 C31 121.2(6) . . ? C32A C31A C36A 115.7(9) . . ? C32A C31A C2 124.0(9) . . ? C36A C31A C2 120.3(9) . . ? C33A C32A C31A 121.8(10) . . ? C32A C33A C34A 120.0(11) . . ? C35A C34A C33A 119.0(13) . . ? C34A C35A C36A 119.8(10) . . ? C35A C36A C31A 123.0(9) . . ? C22 C21 C26 116.8(2) . . ? C22 C21 C2 122.1(2) . . ? C26 C21 C2 121.0(2) . . ? C13 C12 C11 121.4(2) . . ? N1 C17 C18 119.70(19) . . ? C16 C11 C12 118.3(2) . . ? C16 C11 N1 121.1(2) . . ? C12 C11 N1 120.6(2) . . ? C15 C16 C11 120.8(2) . . ? C16 C15 C14 119.5(2) . . ? C16 C15 C151 119.0(2) . . ? C14 C15 C151 121.5(2) . . ? C25 C26 C21 121.5(2) . . ? C12 C13 C14 119.2(2) . . ? C12 C13 C131 120.5(2) . . ? C14 C13 C131 120.2(2) . . ? C23 C22 C21 121.4(2) . . ? C25 C24 C23 118.7(2) . . ? C181 C18 C182 110.3(2) . . ? C181 C18 C183 108.8(2) . . ? C182 C18 C183 109.5(2) . . ? C181 C18 C17 112.5(2) . . ? C182 C18 C17 111.2(2) . . ? C183 C18 C17 104.4(2) . . ? C13 C14 C15 120.5(2) . . ? C22 C23 C24 120.7(3) . . ? C24 C25 C26 120.8(2) . . ? O1T Na1 O1T 87.38(6) . 11 ? O1T Na1 O1T 92.62(6) . 2 ? O1T Na1 O1T 180.00(12) 11 2 ? O1T Na1 O1T 180.0 . 10 ? O1T Na1 O1T 92.62(6) 11 10 ? O1T Na1 O1T 87.38(6) 2 10 ? O1T Na1 O1T 87.38(6) . 12 ? O1T Na1 O1T 92.62(6) 11 12 ? O1T Na1 O1T 87.38(6) 2 12 ? O1T Na1 O1T 92.62(6) 10 12 ? O1T Na1 O1T 92.62(6) . 3 ? O1T Na1 O1T 87.38(6) 11 3 ? O1T Na1 O1T 92.62(6) 2 3 ? O1T Na1 O1T 87.38(6) 10 3 ? O1T Na1 O1T 180.00(17) 12 3 ? O1S Na2 O1S 90.57(7) 14 13_545 ? O1S Na2 O1S 90.57(7) 14 15_445 ? O1S Na2 O1S 90.57(7) 13_545 15_445 ? O1S Na2 O1S 89.43(7) 14 . ? O1S Na2 O1S 180.00(8) 13_545 . ? O1S Na2 O1S 89.43(7) 15_445 . ? O1S Na2 O1S 179.996(1) 14 2_545 ? O1S Na2 O1S 89.43(7) 13_545 2_545 ? O1S Na2 O1S 89.43(7) 15_445 2_545 ? O1S Na2 O1S 90.56(7) . 2_545 ? O1S Na2 O1S 89.44(7) 14 3_655 ? O1S Na2 O1S 89.44(7) 13_545 3_655 ? O1S Na2 O1S 179.994(1) 15_445 3_655 ? O1S Na2 O1S 90.57(7) . 3_655 ? O1S Na2 O1S 90.56(7) 2_545 3_655 ? C1T O1T C4T 109.2(2) . . ? C1T O1T Na1 126.98(17) . . ? C4T O1T Na1 120.99(15) . . ? C1S O1S C4S 108.5(2) . . ? C1S O1S Na2 126.41(18) . . ? C4S O1S Na2 124.53(17) . . ? O1T C4T C3T 105.2(2) . . ? O1S C1S C2S 108.1(3) . . ? O1T C1T C2T 107.5(2) . . ? C3T C2T C1T 102.3(2) . . ? O1S C4S C3S 105.8(3) . . ? C2T C3T C4T 101.8(2) . . ? C2S C3S C4S 103.1(3) . . ? C3S C2S C1S 104.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.838 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.073 # Attachment '2156_web_deposit_cif_file_1_SidCreutz_1281986427.cif' data_09043 _database_code_depnum_ccdc_archive 'CCDC 789474' #TrackingRef '2156_web_deposit_cif_file_1_SidCreutz_1281986427.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(Ar[Np]N)3Nb(OC[CPh2])2P][Na(thf)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74.75 H97 N3 Na Nb O3 P' _chemical_formula_weight 1232.42 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 23.715(2) _cell_length_b 16.1639(13) _cell_length_c 19.4189(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.0020(10) _cell_angle_gamma 90.00 _cell_volume 7118.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9305 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 29.51 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2630 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9175 _exptl_absorpt_correction_T_max 0.9808 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 109340 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13042 _reflns_number_gt 10072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+10.2114P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13042 _refine_ls_number_parameters 892 _refine_ls_number_restraints 395 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 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 Nb1 Nb 0.265352(11) 0.076409(17) 0.342707(13) 0.02293(9) Uani 1 1 d . A . Na1 Na 0.13310(6) -0.03638(9) 0.32225(7) 0.0451(4) Uani 1 1 d . A . P1 P 0.20064(3) 0.08896(5) 0.20694(4) 0.02421(18) Uani 1 1 d . . . C1 C 0.20654(13) -0.0248(2) 0.22335(15) 0.0260(6) Uani 1 1 d . A . O1S O 0.04686(11) -0.09888(16) 0.27793(13) 0.0434(6) Uani 1 1 d . . . N1 N 0.26779(11) 0.02301(18) 0.43873(12) 0.0308(6) Uani 1 1 d . . . C1S C 0.02714(19) -0.1287(3) 0.2049(2) 0.0556(11) Uani 1 1 d . . . H1S1 H 0.0544 -0.1107 0.1777 0.067 Uiso 1 1 calc R . . H1S2 H 0.0251 -0.1899 0.2040 0.067 Uiso 1 1 calc R . . N2 N 0.28168(12) 0.19799(18) 0.35615(15) 0.0357(7) Uani 1 1 d . . . C2S C -0.0304(2) -0.0936(4) 0.1743(2) 0.0780(16) Uani 1 1 d . . . H2S1 H -0.0547 -0.1296 0.1357 0.094 Uiso 1 1 calc R . . H2S2 H -0.0274 -0.0382 0.1538 0.094 Uiso 1 1 calc R . . N3 N 0.34137(12) 0.04953(18) 0.31764(16) 0.0380(7) Uani 1 1 d . . . C3S C -0.05654(17) -0.0876(3) 0.2354(2) 0.0518(10) Uani 1 1 d . . . H3S1 H -0.0781 -0.1388 0.2399 0.062 Uiso 1 1 calc R . . H3S2 H -0.0838 -0.0399 0.2291 0.062 Uiso 1 1 calc R . . C4S C -0.00336(16) -0.0756(2) 0.30030(18) 0.0397(8) Uani 1 1 d . . . H4S1 H -0.0002 -0.0172 0.3161 0.048 Uiso 1 1 calc R . . H4S2 H -0.0064 -0.1109 0.3407 0.048 Uiso 1 1 calc R . . C11 C 0.21933(13) -0.0150(2) 0.45622(15) 0.0299(7) Uani 1 1 d . A . C12 C 0.18429(14) 0.0302(2) 0.48939(16) 0.0336(7) Uani 1 1 d . . . H12 H 0.1928 0.0869 0.5004 0.040 Uiso 1 1 calc R A . C13 C 0.13689(14) -0.0069(2) 0.50669(17) 0.0363(8) Uani 1 1 d . A . C14 C 0.12305(15) -0.0887(2) 0.48638(17) 0.0380(8) Uani 1 1 d . . . H14 H 0.0896 -0.1135 0.4956 0.046 Uiso 1 1 calc R A . C15 C 0.15695(15) -0.1354(2) 0.45286(17) 0.0366(8) Uani 1 1 d . A . C16 C 0.20600(15) -0.0979(2) 0.43939(16) 0.0350(8) Uani 1 1 d . . . H16 H 0.2305 -0.1295 0.4184 0.042 Uiso 1 1 calc R A . C17 C 0.32641(18) -0.0214(3) 0.4774(2) 0.0248(10) Uani 0.707(5) 1 d PDU A 1 H17A H 0.3198 -0.0818 0.4714 0.030 Uiso 0.707(5) 1 calc PR A 1 H17B H 0.3559 -0.0062 0.4526 0.030 Uiso 0.707(5) 1 calc PR A 1 C18 C 0.3532(4) -0.0033(5) 0.5583(4) 0.0292(19) Uani 0.707(5) 1 d PDU A 1 C182 C 0.3185(6) -0.0464(8) 0.6043(7) 0.033(2) Uani 0.707(5) 1 d PDU A 1 H18A H 0.3369 -0.0336 0.6553 0.050 Uiso 0.707(5) 1 calc PR A 1 H18B H 0.3190 -0.1064 0.5971 0.050 Uiso 0.707(5) 1 calc PR A 1 H18C H 0.2777 -0.0267 0.5897 0.050 Uiso 0.707(5) 1 calc PR A 1 C183 C 0.4155(2) -0.0383(4) 0.5799(3) 0.0425(14) Uani 0.707(5) 1 d PDU A 1 H18D H 0.4342 -0.0281 0.6313 0.064 Uiso 0.707(5) 1 calc PR A 1 H18E H 0.4384 -0.0114 0.5517 0.064 Uiso 0.707(5) 1 calc PR A 1 H18F H 0.4139 -0.0980 0.5707 0.064 Uiso 0.707(5) 1 calc PR A 1 C181 C 0.3546(2) 0.0899(3) 0.5732(2) 0.0373(13) Uani 0.707(5) 1 d PDU A 1 H18G H 0.3718 0.0998 0.6249 0.056 Uiso 0.707(5) 1 calc PR A 1 H18H H 0.3144 0.1120 0.5576 0.056 Uiso 0.707(5) 1 calc PR A 1 H18I H 0.3786 0.1176 0.5466 0.056 Uiso 0.707(5) 1 calc PR A 1 C17A C 0.3098(4) 0.0684(7) 0.5040(5) 0.030(3) Uani 0.293(5) 1 d PDU A 2 H17C H 0.3364 0.1052 0.4870 0.036 Uiso 0.293(5) 1 calc PR A 2 H17D H 0.2863 0.1034 0.5273 0.036 Uiso 0.293(5) 1 calc PR A 2 C18A C 0.3471(8) 0.0069(11) 0.5599(10) 0.035(5) Uani 0.293(5) 1 d PDU A 2 C186 C 0.3102(14) -0.038(2) 0.6019(18) 0.050(7) Uani 0.293(5) 1 d PDU A 2 H18J H 0.2917 0.0024 0.6259 0.075 Uiso 0.293(5) 1 calc PR A 2 H18K H 0.3359 -0.0748 0.6381 0.075 Uiso 0.293(5) 1 calc PR A 2 H18L H 0.2795 -0.0714 0.5685 0.075 Uiso 0.293(5) 1 calc PR A 2 C185 C 0.3758(6) -0.0573(8) 0.5239(7) 0.048(3) Uani 0.293(5) 1 d PDU A 2 H18M H 0.3451 -0.0907 0.4908 0.071 Uiso 0.293(5) 1 calc PR A 2 H18N H 0.4013 -0.0932 0.5607 0.071 Uiso 0.293(5) 1 calc PR A 2 H18O H 0.3993 -0.0294 0.4970 0.071 Uiso 0.293(5) 1 calc PR A 2 C184 C 0.3943(6) 0.0594(9) 0.6128(6) 0.054(4) Uani 0.293(5) 1 d PDU A 2 H18P H 0.3752 0.1002 0.6358 0.082 Uiso 0.293(5) 1 calc PR A 2 H18Q H 0.4182 0.0880 0.5867 0.082 Uiso 0.293(5) 1 calc PR A 2 H18R H 0.4197 0.0235 0.6497 0.082 Uiso 0.293(5) 1 calc PR A 2 C21 C 0.28377(14) 0.2372(2) 0.42323(17) 0.0315(7) Uani 1 1 d . A . C22 C 0.33420(15) 0.2794(2) 0.46337(19) 0.0382(8) Uani 1 1 d . . . H22 H 0.3682 0.2808 0.4470 0.046 Uiso 1 1 calc R A . C23 C 0.33479(16) 0.3193(2) 0.52686(19) 0.0418(9) Uani 1 1 d . A . C24 C 0.28510(16) 0.3153(2) 0.55088(17) 0.0388(8) Uani 1 1 d . . . H24 H 0.2858 0.3415 0.5949 0.047 Uiso 1 1 calc R A . C25 C 0.23440(15) 0.2738(2) 0.51182(16) 0.0323(7) Uani 1 1 d . A . C26 C 0.23446(14) 0.23508(19) 0.44777(16) 0.0298(7) Uani 1 1 d . . . H26 H 0.2001 0.2068 0.4204 0.036 Uiso 1 1 calc R A . C27 C 0.29578(17) 0.2547(2) 0.30334(19) 0.0429(9) Uani 1 1 d . A . H27A H 0.2974 0.2212 0.2613 0.051 Uiso 1 1 calc R . . H27B H 0.3359 0.2768 0.3256 0.051 Uiso 1 1 calc R . . C28 C 0.25475(19) 0.3287(2) 0.27494(19) 0.0463(10) Uani 1 1 d . . . C31 C 0.38897(14) 0.1088(2) 0.3340(2) 0.0378(8) Uani 1 1 d . A . C32 C 0.42086(16) 0.1243(2) 0.4044(2) 0.0411(8) Uani 1 1 d . . . H32 H 0.4120 0.0936 0.4416 0.049 Uiso 1 1 calc R A . C33 C 0.46561(16) 0.1835(2) 0.4231(2) 0.0451(9) Uani 1 1 d . A . C34 C 0.47789(16) 0.2280(3) 0.3682(2) 0.0513(10) Uani 1 1 d . . . H34 H 0.5078 0.2692 0.3798 0.062 Uiso 1 1 calc R A . C35 C 0.44702(18) 0.2133(3) 0.2960(2) 0.0594(12) Uani 1 1 d . A . C36 C 0.40314(17) 0.1529(3) 0.2796(2) 0.0542(11) Uani 1 1 d . . . H36 H 0.3826 0.1416 0.2306 0.065 Uiso 1 1 calc R A . C37 C 0.34461(17) -0.0129(3) 0.2575(2) 0.0290(10) Uani 0.775(5) 1 d PDU A 1 H37A H 0.3044 -0.0344 0.2345 0.035 Uiso 0.775(5) 1 calc PR A 1 H37B H 0.3570 0.0177 0.2202 0.035 Uiso 0.775(5) 1 calc PR A 1 C38 C 0.3865(3) -0.0875(5) 0.2819(5) 0.0390(17) Uani 0.775(5) 1 d PDU A 1 C383 C 0.4508(3) -0.0541(7) 0.3061(5) 0.090(4) Uani 0.775(5) 1 d PDU A 1 H38A H 0.4580 -0.0209 0.2673 0.136 Uiso 0.775(5) 1 calc PR A 1 H38B H 0.4784 -0.1007 0.3172 0.136 Uiso 0.775(5) 1 calc PR A 1 H38C H 0.4565 -0.0197 0.3492 0.136 Uiso 0.775(5) 1 calc PR A 1 C382 C 0.3650(2) -0.1417(3) 0.3343(3) 0.0498(14) Uani 0.775(5) 1 d PDU A 1 H38D H 0.3240 -0.1579 0.3117 0.075 Uiso 0.775(5) 1 calc PR A 1 H38E H 0.3678 -0.1104 0.3784 0.075 Uiso 0.775(5) 1 calc PR A 1 H38F H 0.3897 -0.1914 0.3463 0.075 Uiso 0.775(5) 1 calc PR A 1 C381 C 0.3803(2) -0.1386(3) 0.2136(3) 0.0494(14) Uani 0.775(5) 1 d PDU A 1 H38G H 0.3946 -0.1063 0.1794 0.074 Uiso 0.775(5) 1 calc PR A 1 H38H H 0.3387 -0.1527 0.1916 0.074 Uiso 0.775(5) 1 calc PR A 1 H38I H 0.4035 -0.1895 0.2260 0.074 Uiso 0.775(5) 1 calc PR A 1 C37A C 0.3648(6) -0.0292(9) 0.3400(7) 0.031(3) Uani 0.225(5) 1 d PDU A 2 H37C H 0.3341 -0.0656 0.3489 0.037 Uiso 0.225(5) 1 calc PR A 2 H37D H 0.3978 -0.0249 0.3850 0.037 Uiso 0.225(5) 1 calc PR A 2 C38A C 0.3867(11) -0.0640(13) 0.2789(11) 0.038(5) Uani 0.225(5) 1 d PDU A 2 C386 C 0.3499(7) -0.0327(11) 0.2055(7) 0.043(4) Uani 0.225(5) 1 d PDU A 2 H38J H 0.3487 0.0279 0.2061 0.064 Uiso 0.225(5) 1 calc PR A 2 H38K H 0.3098 -0.0547 0.1948 0.064 Uiso 0.225(5) 1 calc PR A 2 H38L H 0.3677 -0.0512 0.1686 0.064 Uiso 0.225(5) 1 calc PR A 2 C385 C 0.3889(7) -0.1592(10) 0.2813(9) 0.048(4) Uani 0.225(5) 1 d PDU A 2 H38M H 0.4113 -0.1774 0.3297 0.071 Uiso 0.225(5) 1 calc PR A 2 H38N H 0.4080 -0.1796 0.2463 0.071 Uiso 0.225(5) 1 calc PR A 2 H38O H 0.3487 -0.1812 0.2696 0.071 Uiso 0.225(5) 1 calc PR A 2 C384 C 0.4508(9) -0.0630(17) 0.3232(12) 0.032(5) Uani 0.225(5) 1 d PDU A 2 H38P H 0.4565 -0.1006 0.3643 0.048 Uiso 0.225(5) 1 calc PR A 2 H38Q H 0.4620 -0.0068 0.3408 0.048 Uiso 0.225(5) 1 calc PR A 2 H38R H 0.4754 -0.0810 0.2933 0.048 Uiso 0.225(5) 1 calc PR A 2 C41 C 0.20172(13) -0.1762(2) 0.19106(16) 0.0285(7) Uani 1 1 d . A . C42 C 0.20318(15) -0.2088(2) 0.25830(17) 0.0351(8) Uani 1 1 d . . . H42 H 0.1980 -0.1727 0.2945 0.042 Uiso 1 1 calc R . . C43 C 0.21203(16) -0.2928(2) 0.27366(19) 0.0422(8) Uani 1 1 d . . . H43 H 0.2135 -0.3127 0.3202 0.051 Uiso 1 1 calc R . . C44 C 0.21870(16) -0.3477(2) 0.2219(2) 0.0450(9) Uani 1 1 d . . . H44 H 0.2250 -0.4049 0.2324 0.054 Uiso 1 1 calc R . . C45 C 0.21598(17) -0.3174(2) 0.1549(2) 0.0463(9) Uani 1 1 d . . . H45 H 0.2196 -0.3544 0.1184 0.056 Uiso 1 1 calc R . . C46 C 0.20806(16) -0.2333(2) 0.13967(18) 0.0384(8) Uani 1 1 d . . . H46 H 0.2069 -0.2142 0.0930 0.046 Uiso 1 1 calc R . . C51 C 0.12439(14) -0.09420(19) 0.04727(16) 0.0302(7) Uani 1 1 d . . . H51 H 0.0982 -0.1262 0.0653 0.036 Uiso 1 1 calc R . . C52 C 0.10979(16) -0.0773(2) -0.02581(16) 0.0359(8) Uani 1 1 d . . . H52 H 0.0736 -0.0969 -0.0572 0.043 Uiso 1 1 calc R . . C53 C 0.14779(18) -0.0320(2) -0.05310(17) 0.0419(9) Uani 1 1 d . . . H53 H 0.1381 -0.0211 -0.1033 0.050 Uiso 1 1 calc R . . C54 C 0.19997(18) -0.0025(2) -0.00712(18) 0.0444(9) Uani 1 1 d . . . H54 H 0.2260 0.0293 -0.0256 0.053 Uiso 1 1 calc R . . C55 C 0.21450(15) -0.0195(2) 0.06648(17) 0.0364(8) Uani 1 1 d . . . H55 H 0.2507 0.0005 0.0976 0.044 Uiso 1 1 calc R . . C56 C 0.17691(13) -0.06508(19) 0.09498(15) 0.0269(7) Uani 1 1 d . A . C61 C 0.04513(13) 0.13594(18) 0.27149(15) 0.0244(6) Uani 1 1 d . A . C62 C 0.06069(14) 0.14353(19) 0.34664(16) 0.0283(7) Uani 1 1 d . . . H62 H 0.1012 0.1444 0.3737 0.034 Uiso 1 1 calc R . . C63 C 0.01775(15) 0.1498(2) 0.38213(17) 0.0335(7) Uani 1 1 d . . . H63 H 0.0295 0.1547 0.4331 0.040 Uiso 1 1 calc R . . C64 C -0.04130(15) 0.1490(2) 0.34523(18) 0.0365(8) Uani 1 1 d . . . H64 H -0.0702 0.1530 0.3702 0.044 Uiso 1 1 calc R . . C65 C -0.05789(15) 0.1422(2) 0.27095(18) 0.0369(8) Uani 1 1 d . . . H65 H -0.0985 0.1419 0.2446 0.044 Uiso 1 1 calc R . . C66 C -0.01584(14) 0.1358(2) 0.23480(16) 0.0296(7) Uani 1 1 d . . . H66 H -0.0283 0.1311 0.1838 0.036 Uiso 1 1 calc R . . C151 C 0.14100(18) -0.2240(2) 0.4312(2) 0.0490(10) Uani 1 1 d . . . H15A H 0.1171 -0.2259 0.3807 0.074 Uiso 1 1 calc R A . H15B H 0.1184 -0.2473 0.4616 0.074 Uiso 1 1 calc R . . H15C H 0.1771 -0.2563 0.4374 0.074 Uiso 1 1 calc R . . C231 C 0.38945(19) 0.3684(3) 0.5676(2) 0.0646(13) Uani 1 1 d . . . H23A H 0.4195 0.3305 0.5961 0.097 Uiso 1 1 calc R A . H23B H 0.3788 0.4082 0.5998 0.097 Uiso 1 1 calc R . . H23C H 0.4051 0.3981 0.5332 0.097 Uiso 1 1 calc R . . C251 C 0.17994(16) 0.2720(2) 0.53658(19) 0.0421(9) Uani 1 1 d . . . H25A H 0.1842 0.2292 0.5735 0.063 Uiso 1 1 calc R A . H25B H 0.1455 0.2595 0.4956 0.063 Uiso 1 1 calc R . . H25C H 0.1746 0.3260 0.5567 0.063 Uiso 1 1 calc R . . C281 C 0.2588(2) 0.3985(2) 0.3311(2) 0.0591(12) Uani 1 1 d . A . H28A H 0.2353 0.4460 0.3076 0.089 Uiso 1 1 calc R . . H28B H 0.3000 0.4154 0.3513 0.089 Uiso 1 1 calc R . . H28C H 0.2436 0.3782 0.3698 0.089 Uiso 1 1 calc R . . C282 C 0.2762(2) 0.3656(3) 0.2136(2) 0.0640(13) Uani 1 1 d . A . H28D H 0.2757 0.3226 0.1779 0.096 Uiso 1 1 calc R . . H28E H 0.3164 0.3867 0.2334 0.096 Uiso 1 1 calc R . . H28F H 0.2500 0.4110 0.1906 0.096 Uiso 1 1 calc R . . C283 C 0.19060(18) 0.3022(2) 0.2446(2) 0.0480(10) Uani 1 1 d . A . H28G H 0.1665 0.3502 0.2236 0.072 Uiso 1 1 calc R . . H28H H 0.1766 0.2791 0.2833 0.072 Uiso 1 1 calc R . . H28I H 0.1874 0.2601 0.2073 0.072 Uiso 1 1 calc R . . C331 C 0.4995(2) 0.1987(3) 0.5005(2) 0.0677(13) Uani 1 1 d . . . H33A H 0.5342 0.2326 0.5028 0.101 Uiso 1 1 calc R A . H33B H 0.5120 0.1457 0.5247 0.101 Uiso 1 1 calc R . . H33C H 0.4742 0.2278 0.5246 0.101 Uiso 1 1 calc R . . C351 C 0.4601(3) 0.2628(4) 0.2352(3) 0.096(2) Uani 1 1 d . . . H35A H 0.4929 0.2371 0.2222 0.144 Uiso 1 1 calc R A . H35B H 0.4706 0.3197 0.2514 0.144 Uiso 1 1 calc R . . H35C H 0.4250 0.2633 0.1932 0.144 Uiso 1 1 calc R . . O2 O 0.17207(9) 0.09273(13) 0.32975(10) 0.0260(5) Uani 1 1 d . . . O1 O 0.22956(9) -0.03827(13) 0.29520(10) 0.0272(5) Uani 1 1 d . . . C4 C 0.08852(13) 0.12557(18) 0.22997(14) 0.0226(6) Uani 1 1 d . . . C70 C 0.06590(13) 0.14231(18) 0.15065(15) 0.0231(6) Uani 1 1 d . A . C71 C 0.06389(13) 0.08238(19) 0.09856(15) 0.0264(6) Uani 1 1 d . . . H71 H 0.0770 0.0278 0.1130 0.032 Uiso 1 1 calc R A . C74 C 0.02359(14) 0.2401(2) 0.05471(16) 0.0295(7) Uani 1 1 d . A . H74 H 0.0097 0.2943 0.0400 0.035 Uiso 1 1 calc R . . C73 C 0.02230(13) 0.1799(2) 0.00355(16) 0.0295(7) Uani 1 1 d . . . H73 H 0.0074 0.1925 -0.0463 0.035 Uiso 1 1 calc R A . C75 C 0.04510(14) 0.22141(19) 0.12729(15) 0.0278(7) Uani 1 1 d . . . H75 H 0.0457 0.2632 0.1619 0.033 Uiso 1 1 calc R A . C3 C 0.14628(13) 0.10476(18) 0.25873(14) 0.0229(6) Uani 1 1 d . A . C2 C 0.19410(13) -0.08643(19) 0.17341(15) 0.0255(6) Uani 1 1 d . . . C72 C 0.04289(14) 0.1014(2) 0.02564(16) 0.0303(7) Uani 1 1 d . A . H72 H 0.0427 0.0601 -0.0092 0.036 Uiso 1 1 calc R . . C131 C 0.10216(17) 0.0399(2) 0.5482(2) 0.0524(10) Uani 1 1 d . . . H13A H 0.0599 0.0323 0.5248 0.079 Uiso 1 1 calc R A . H13B H 0.1119 0.0989 0.5491 0.079 Uiso 1 1 calc R . . H13C H 0.1122 0.0188 0.5976 0.079 Uiso 1 1 calc R . . C1T C 0.3158(2) -0.3082(2) 0.49915(19) 0.119(6) Uani 0.443(11) 1 d PRDU B 1 H1T1 H 0.3148 -0.3060 0.5492 0.179 Uiso 0.443(11) 1 calc PR B 1 H1T2 H 0.2764 -0.3221 0.4677 0.179 Uiso 0.443(11) 1 calc PR B 1 H1T3 H 0.3278 -0.2542 0.4853 0.179 Uiso 0.443(11) 1 calc PR B 1 C2T C 0.3568(2) -0.3696(3) 0.49222(19) 0.101(5) Uani 0.443(11) 1 d PRDU B 1 H2T1 H 0.3450 -0.4224 0.5099 0.121 Uiso 0.443(11) 1 calc PR B 1 H2T2 H 0.3957 -0.3545 0.5255 0.121 Uiso 0.443(11) 1 calc PR B 1 C3T C 0.3660(2) -0.3872(2) 0.4173(2) 0.122(6) Uani 0.443(11) 1 d PRDU B 1 H3T1 H 0.3754 -0.3341 0.3978 0.146 Uiso 0.443(11) 1 calc PR B 1 H3T2 H 0.3281 -0.4069 0.3846 0.146 Uiso 0.443(11) 1 calc PR B 1 C4T C 0.4177(2) -0.4549(2) 0.41461(19) 0.138(7) Uani 0.443(11) 1 d PRDU B 1 H4T1 H 0.4538 -0.4402 0.4535 0.166 Uiso 0.443(11) 1 calc PR B 1 H4T2 H 0.4048 -0.5098 0.4268 0.166 Uiso 0.443(11) 1 calc PR B 1 C5T C 0.4363(2) -0.4653(2) 0.34123(19) 0.224(16) Uani 0.443(11) 1 d PRDU B 1 H5T1 H 0.4666 -0.5083 0.3480 0.337 Uiso 0.443(11) 1 calc PR B 1 H5T2 H 0.4520 -0.4128 0.3295 0.337 Uiso 0.443(11) 1 calc PR B 1 H5T3 H 0.4017 -0.4812 0.3018 0.337 Uiso 0.443(11) 1 calc PR B 1 C1X C 0.3303(2) -0.3295(2) 0.48155(19) 0.142(12) Uani 0.307(11) 1 d PRDU B 2 H1X1 H 0.2880 -0.3313 0.4763 0.213 Uiso 0.307(11) 1 calc PR B 2 H1X2 H 0.3415 -0.2731 0.4723 0.213 Uiso 0.307(11) 1 calc PR B 2 H1X3 H 0.3525 -0.3458 0.5306 0.213 Uiso 0.307(11) 1 calc PR B 2 C2X C 0.3441(2) -0.3876(2) 0.4289(2) 0.132(10) Uani 0.307(11) 1 d PRDU B 2 H2X1 H 0.3279 -0.4410 0.4394 0.158 Uiso 0.307(11) 1 calc PR B 2 H2X2 H 0.3172 -0.3695 0.3821 0.158 Uiso 0.307(11) 1 calc PR B 2 C3X C 0.3946(2) -0.4108(3) 0.41155(19) 0.103(8) Uani 0.307(11) 1 d PRDU B 2 H3X1 H 0.4142 -0.4517 0.4488 0.124 Uiso 0.307(11) 1 calc PR B 2 H3X2 H 0.4202 -0.3611 0.4214 0.124 Uiso 0.307(11) 1 calc PR B 2 C4X C 0.4015(2) -0.4471(2) 0.3387(2) 0.130(9) Uani 0.307(11) 1 d PRDU B 2 H4X1 H 0.3725 -0.4925 0.3236 0.156 Uiso 0.307(11) 1 calc PR B 2 H4X2 H 0.3894 -0.4031 0.3018 0.156 Uiso 0.307(11) 1 calc PR B 2 C5X C 0.4595(2) -0.4796(3) 0.33495(19) 0.25(2) Uani 0.307(11) 1 d PRDU B 2 H5X1 H 0.4555 -0.5001 0.2863 0.381 Uiso 0.307(11) 1 calc PR B 2 H5X2 H 0.4723 -0.5248 0.3696 0.381 Uiso 0.307(11) 1 calc PR B 2 H5X3 H 0.4889 -0.4351 0.3466 0.381 Uiso 0.307(11) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.02118(15) 0.03293(16) 0.01390(13) -0.00093(11) 0.00392(10) -0.00480(11) Na1 0.0358(8) 0.0504(9) 0.0414(8) 0.0130(6) -0.0009(6) -0.0121(6) P1 0.0236(4) 0.0335(4) 0.0152(4) 0.0004(3) 0.0051(3) -0.0020(3) C1 0.0202(15) 0.0394(18) 0.0174(14) -0.0008(12) 0.0041(11) 0.0007(13) O1S 0.0360(14) 0.0460(15) 0.0429(14) -0.0085(11) 0.0035(11) -0.0092(11) N1 0.0233(14) 0.0492(17) 0.0166(12) 0.0043(11) 0.0005(10) -0.0102(12) C1S 0.059(3) 0.060(3) 0.047(2) -0.017(2) 0.014(2) -0.007(2) N2 0.0355(16) 0.0374(16) 0.0418(16) -0.0164(13) 0.0232(13) -0.0126(12) C2S 0.068(3) 0.115(4) 0.039(2) -0.020(3) -0.004(2) 0.031(3) N3 0.0232(14) 0.0352(16) 0.0551(18) 0.0075(13) 0.0107(13) 0.0003(12) C3S 0.037(2) 0.069(3) 0.045(2) 0.0086(19) 0.0052(17) -0.0100(19) C4S 0.046(2) 0.040(2) 0.0331(18) 0.0024(15) 0.0119(16) -0.0124(17) C11 0.0252(16) 0.045(2) 0.0157(14) 0.0083(13) -0.0005(12) -0.0060(14) C12 0.0312(18) 0.0385(19) 0.0274(16) 0.0125(14) 0.0030(14) -0.0033(14) C13 0.0268(17) 0.049(2) 0.0310(17) 0.0153(15) 0.0058(14) 0.0036(15) C14 0.0294(18) 0.052(2) 0.0311(17) 0.0176(15) 0.0069(14) -0.0070(16) C15 0.0374(19) 0.045(2) 0.0228(16) 0.0113(14) 0.0018(14) -0.0091(16) C16 0.0316(18) 0.053(2) 0.0186(15) -0.0007(14) 0.0036(13) -0.0061(15) C17 0.021(2) 0.032(2) 0.020(2) -0.0004(17) 0.0045(16) -0.0010(18) C18 0.029(4) 0.039(4) 0.018(4) 0.004(3) 0.005(3) 0.001(3) C182 0.028(4) 0.049(5) 0.023(5) 0.007(3) 0.007(3) 0.003(3) C183 0.026(3) 0.067(4) 0.029(3) 0.005(2) -0.001(2) 0.001(2) C181 0.038(3) 0.050(3) 0.021(2) -0.007(2) 0.004(2) -0.011(2) C17A 0.025(5) 0.047(6) 0.016(5) -0.002(4) 0.002(4) -0.004(4) C18A 0.009(7) 0.068(12) 0.023(9) 0.002(7) -0.002(6) 0.007(6) C186 0.056(16) 0.073(17) 0.014(11) 0.011(10) -0.001(9) -0.023(12) C185 0.049(8) 0.051(7) 0.042(7) 0.024(5) 0.012(6) 0.012(6) C184 0.038(7) 0.089(10) 0.027(6) 0.010(6) -0.005(5) -0.018(7) C21 0.0332(18) 0.0302(17) 0.0341(17) -0.0074(14) 0.0144(14) -0.0018(14) C22 0.0283(18) 0.041(2) 0.046(2) -0.0073(16) 0.0106(15) -0.0039(15) C23 0.038(2) 0.039(2) 0.041(2) -0.0095(16) 0.0002(16) -0.0033(16) C24 0.043(2) 0.042(2) 0.0265(17) -0.0079(15) 0.0024(15) 0.0037(16) C25 0.0372(19) 0.0327(18) 0.0270(16) -0.0021(13) 0.0092(14) 0.0035(14) C26 0.0296(17) 0.0318(17) 0.0279(16) -0.0073(13) 0.0082(13) -0.0035(13) C27 0.052(2) 0.044(2) 0.045(2) -0.0173(17) 0.0323(18) -0.0190(18) C28 0.071(3) 0.041(2) 0.039(2) -0.0118(16) 0.0360(19) -0.0219(19) C31 0.0224(17) 0.040(2) 0.052(2) 0.0073(16) 0.0110(15) 0.0011(14) C32 0.044(2) 0.037(2) 0.051(2) 0.0001(16) 0.0281(18) -0.0006(16) C33 0.037(2) 0.047(2) 0.053(2) -0.0032(18) 0.0160(18) -0.0007(17) C34 0.0273(19) 0.053(2) 0.072(3) 0.008(2) 0.0111(19) -0.0075(17) C35 0.037(2) 0.069(3) 0.068(3) 0.022(2) 0.008(2) -0.014(2) C36 0.036(2) 0.063(3) 0.055(2) 0.020(2) -0.0005(18) -0.0127(19) C37 0.023(2) 0.044(2) 0.022(2) -0.0039(17) 0.0083(16) 0.0019(18) C38 0.024(3) 0.051(4) 0.038(3) -0.012(3) 0.003(2) 0.011(3) C383 0.024(3) 0.124(9) 0.108(8) -0.082(6) -0.004(4) 0.016(4) C382 0.053(3) 0.045(3) 0.049(3) 0.000(2) 0.012(2) 0.017(2) C381 0.042(3) 0.061(3) 0.043(3) -0.021(2) 0.008(2) 0.007(2) C37A 0.026(7) 0.041(8) 0.027(6) 0.001(6) 0.012(6) -0.003(6) C38A 0.046(10) 0.051(10) 0.020(8) -0.011(8) 0.013(7) 0.005(10) C386 0.032(8) 0.065(11) 0.033(7) 0.012(7) 0.012(6) 0.009(7) C385 0.042(9) 0.047(8) 0.048(10) 0.000(7) 0.005(8) 0.009(7) C384 0.038(8) 0.037(10) 0.028(8) 0.023(8) 0.019(6) 0.009(7) C41 0.0220(16) 0.0340(18) 0.0262(16) -0.0013(13) 0.0017(12) 0.0033(13) C42 0.0381(19) 0.0384(19) 0.0284(17) -0.0030(14) 0.0091(14) -0.0003(15) C43 0.044(2) 0.043(2) 0.0359(19) 0.0029(16) 0.0061(16) 0.0005(17) C44 0.044(2) 0.037(2) 0.051(2) 0.0054(17) 0.0092(18) 0.0119(17) C45 0.053(2) 0.040(2) 0.044(2) -0.0055(17) 0.0117(18) 0.0185(18) C46 0.042(2) 0.044(2) 0.0279(17) 0.0006(15) 0.0083(15) 0.0124(16) C51 0.0340(18) 0.0292(17) 0.0242(16) -0.0038(12) 0.0037(13) 0.0024(13) C52 0.043(2) 0.0349(18) 0.0217(16) -0.0073(14) -0.0037(14) 0.0079(15) C53 0.064(3) 0.039(2) 0.0181(16) -0.0014(14) 0.0060(16) 0.0088(18) C54 0.062(3) 0.048(2) 0.0264(17) -0.0002(15) 0.0181(17) -0.0067(19) C55 0.0368(19) 0.047(2) 0.0246(16) -0.0068(14) 0.0084(14) -0.0081(16) C56 0.0272(16) 0.0318(17) 0.0201(15) -0.0038(12) 0.0045(12) 0.0043(13) C61 0.0282(16) 0.0224(15) 0.0227(15) 0.0004(11) 0.0076(12) -0.0004(12) C62 0.0293(17) 0.0320(17) 0.0229(15) -0.0014(12) 0.0065(13) 0.0009(13) C63 0.044(2) 0.0350(18) 0.0235(16) -0.0010(13) 0.0137(14) 0.0026(15) C64 0.040(2) 0.040(2) 0.0357(18) 0.0049(15) 0.0205(16) 0.0052(15) C65 0.0284(18) 0.048(2) 0.0348(18) 0.0065(15) 0.0100(14) 0.0045(15) C66 0.0309(17) 0.0369(18) 0.0213(15) 0.0017(13) 0.0080(13) 0.0014(14) C151 0.053(2) 0.051(2) 0.044(2) 0.0056(18) 0.0144(18) -0.0169(19) C231 0.050(3) 0.078(3) 0.059(3) -0.025(2) 0.005(2) -0.019(2) C251 0.046(2) 0.051(2) 0.0338(18) -0.0095(16) 0.0189(16) 0.0030(17) C281 0.104(4) 0.034(2) 0.049(2) -0.0059(17) 0.039(2) -0.009(2) C282 0.092(3) 0.066(3) 0.048(2) -0.009(2) 0.042(2) -0.035(3) C283 0.067(3) 0.039(2) 0.049(2) -0.0017(17) 0.033(2) -0.0088(19) C331 0.082(3) 0.065(3) 0.056(3) -0.016(2) 0.019(2) -0.022(3) C351 0.086(4) 0.107(5) 0.084(4) 0.034(3) 0.008(3) -0.052(3) O2 0.0263(11) 0.0359(12) 0.0149(10) 0.0012(8) 0.0045(8) -0.0008(9) O1 0.0284(11) 0.0352(12) 0.0147(10) -0.0010(8) 0.0010(8) 0.0006(9) C4 0.0262(16) 0.0245(15) 0.0165(14) -0.0015(11) 0.0055(12) -0.0016(12) C70 0.0223(15) 0.0275(16) 0.0201(14) 0.0007(12) 0.0070(12) -0.0001(12) C71 0.0293(16) 0.0253(16) 0.0227(15) -0.0007(12) 0.0047(12) -0.0004(13) C74 0.0326(17) 0.0302(17) 0.0260(16) 0.0057(13) 0.0092(13) 0.0038(14) C73 0.0289(17) 0.0387(19) 0.0188(15) 0.0026(13) 0.0035(12) -0.0032(14) C75 0.0361(18) 0.0267(16) 0.0217(15) -0.0014(12) 0.0104(13) 0.0023(13) C3 0.0256(16) 0.0262(15) 0.0178(14) -0.0021(11) 0.0077(12) -0.0035(12) C2 0.0209(15) 0.0348(18) 0.0197(14) -0.0015(12) 0.0043(12) 0.0004(13) C72 0.0377(18) 0.0311(17) 0.0194(15) -0.0053(12) 0.0040(13) -0.0030(14) C131 0.044(2) 0.059(3) 0.059(3) 0.017(2) 0.024(2) 0.0100(19) C1T 0.101(12) 0.102(12) 0.140(15) 0.042(11) 0.012(11) -0.008(9) C2T 0.082(9) 0.111(11) 0.086(9) 0.033(8) -0.013(7) -0.030(7) C3T 0.083(13) 0.143(16) 0.116(12) 0.000(11) -0.010(9) -0.052(9) C4T 0.118(14) 0.160(17) 0.130(14) 0.023(12) 0.026(11) -0.041(11) C5T 0.15(2) 0.34(4) 0.19(2) -0.13(3) 0.057(18) -0.10(2) C1X 0.13(2) 0.13(2) 0.12(2) 0.005(17) -0.035(17) 0.01(2) C2X 0.111(15) 0.116(19) 0.12(2) -0.001(14) -0.038(13) 0.006(15) C3X 0.060(12) 0.108(17) 0.104(14) 0.018(11) -0.035(9) -0.060(11) C4X 0.095(15) 0.15(2) 0.111(16) -0.001(14) -0.019(12) -0.062(14) C5X 0.111(19) 0.37(6) 0.29(5) -0.13(4) 0.07(2) -0.11(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 Nb1 N2 2.005(3) . ? Nb1 N1 2.040(2) . ? Nb1 N3 2.047(3) . ? Nb1 O1 2.133(2) . ? Nb1 O2 2.168(2) . ? Nb1 P1 2.6421(8) . ? Nb1 Na1 3.5483(14) . ? Na1 O1S 2.217(3) . ? Na1 O2 2.270(2) . ? Na1 O1 2.493(3) . ? Na1 C16 2.617(3) . ? Na1 C3 2.655(3) . ? Na1 C11 2.821(3) . ? Na1 C15 2.911(3) . ? Na1 C1 2.952(3) . ? P1 C1 1.864(3) . ? P1 C3 1.870(3) . ? C1 O1 1.359(3) . ? C1 C2 1.362(4) . ? O1S C4S 1.432(4) . ? O1S C1S 1.440(4) . ? N1 C11 1.429(4) . ? N1 C17 1.550(5) . ? N1 C17A 1.550(10) . ? C1S C2S 1.435(6) . ? N2 C21 1.436(4) . ? N2 C27 1.485(4) . ? C2S C3S 1.496(6) . ? N3 C37A 1.405(14) . ? N3 C31 1.444(4) . ? N3 C37 1.563(5) . ? C3S C4S 1.512(5) . ? C11 C16 1.393(5) . ? C11 C12 1.397(5) . ? C12 C13 1.399(4) . ? C13 C14 1.392(5) . ? C13 C131 1.513(5) . ? C14 C15 1.394(5) . ? C15 C16 1.403(5) . ? C15 C151 1.509(5) . ? C17 C18 1.540(8) . ? C18 C183 1.522(9) . ? C18 C181 1.533(8) . ? C18 C182 1.546(7) . ? C17A C18A 1.546(16) . ? C18A C185 1.517(17) . ? C18A C184 1.535(17) . ? C18A C186 1.545(15) . ? C21 C26 1.386(4) . ? C21 C22 1.399(5) . ? C22 C23 1.388(5) . ? C23 C24 1.390(5) . ? C23 C231 1.529(5) . ? C24 C25 1.392(5) . ? C25 C26 1.393(4) . ? C25 C251 1.504(5) . ? C27 C28 1.538(6) . ? C28 C283 1.523(6) . ? C28 C282 1.545(5) . ? C28 C281 1.552(5) . ? C31 C32 1.378(5) . ? C31 C36 1.395(5) . ? C32 C33 1.395(5) . ? C33 C34 1.385(5) . ? C33 C331 1.504(6) . ? C34 C35 1.399(6) . ? C35 C36 1.394(5) . ? C35 C351 1.531(6) . ? C37 C38 1.546(7) . ? C38 C381 1.533(9) . ? C38 C382 1.539(9) . ? C38 C383 1.554(10) . ? C37A C38A 1.535(18) . ? C38A C384 1.51(2) . ? C38A C386 1.52(2) . ? C38A C385 1.540(18) . ? C41 C42 1.399(4) . ? C41 C46 1.399(4) . ? C41 C2 1.490(4) . ? C42 C43 1.392(5) . ? C43 C44 1.384(5) . ? C44 C45 1.374(5) . ? C45 C46 1.392(5) . ? C51 C52 1.386(4) . ? C51 C56 1.399(4) . ? C52 C53 1.382(5) . ? C53 C54 1.382(5) . ? C54 C55 1.396(4) . ? C55 C56 1.390(4) . ? C56 C2 1.497(4) . ? C61 C62 1.402(4) . ? C61 C66 1.413(4) . ? C61 C4 1.491(4) . ? C62 C63 1.390(4) . ? C63 C64 1.374(5) . ? C64 C65 1.384(5) . ? C65 C66 1.381(4) . ? O2 C3 1.349(3) . ? C4 C3 1.362(4) . ? C4 C70 1.500(4) . ? C70 C71 1.391(4) . ? C70 C75 1.397(4) . ? C71 C72 1.391(4) . ? C74 C73 1.384(4) . ? C74 C75 1.385(4) . ? C73 C72 1.383(4) . ? C1T C2T 1.4243 . ? C2T C3T 1.5577 . ? C3T C4T 1.6562 . ? C4T C5T 1.6192 . ? C1X C2X 1.4942 . ? C2X C3X 1.3867 . ? C3X C4X 1.5843 . ? C4X C5X 1.4936 . ? 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 N2 Nb1 N1 110.05(11) . . ? N2 Nb1 N3 95.11(11) . . ? N1 Nb1 N3 109.63(11) . . ? N2 Nb1 O1 160.95(10) . . ? N1 Nb1 O1 85.93(9) . . ? N3 Nb1 O1 88.82(10) . . ? N2 Nb1 O2 92.72(10) . . ? N1 Nb1 O2 85.00(9) . . ? N3 Nb1 O2 159.72(10) . . ? O1 Nb1 O2 78.00(8) . . ? N2 Nb1 P1 95.07(9) . . ? N1 Nb1 P1 142.89(7) . . ? N3 Nb1 P1 94.24(9) . . ? O1 Nb1 P1 66.02(5) . . ? O2 Nb1 P1 66.40(5) . . ? N2 Nb1 Na1 130.46(8) . . ? N1 Nb1 Na1 70.91(7) . . ? N3 Nb1 Na1 132.50(9) . . ? O1 Nb1 Na1 43.79(6) . . ? O2 Nb1 Na1 37.91(6) . . ? P1 Nb1 Na1 72.02(3) . . ? O1S Na1 O2 139.11(11) . . ? O1S Na1 O1 135.39(11) . . ? O2 Na1 O1 69.10(8) . . ? O1S Na1 C16 117.66(11) . . ? O2 Na1 C16 98.06(10) . . ? O1 Na1 C16 76.40(9) . . ? O1S Na1 C3 115.58(11) . . ? O2 Na1 C3 30.54(8) . . ? O1 Na1 C3 70.89(9) . . ? C16 Na1 C3 126.33(11) . . ? O1S Na1 C11 138.72(11) . . ? O2 Na1 C11 69.91(9) . . ? O1 Na1 C11 74.53(8) . . ? C16 Na1 C11 29.37(10) . . ? C3 Na1 C11 99.86(10) . . ? O1S Na1 C15 90.57(10) . . ? O2 Na1 C15 118.54(10) . . ? O1 Na1 C15 102.73(10) . . ? C16 Na1 C15 28.77(10) . . ? C3 Na1 C15 149.08(11) . . ? C11 Na1 C15 50.21(9) . . ? O1S Na1 C1 115.42(10) . . ? O2 Na1 C1 71.13(9) . . ? O1 Na1 C1 27.27(7) . . ? C16 Na1 C1 102.95(10) . . ? C3 Na1 C1 58.06(9) . . ? C11 Na1 C1 100.70(9) . . ? C15 Na1 C1 126.91(11) . . ? O1S Na1 Nb1 164.26(9) . . ? O2 Na1 Nb1 35.94(6) . . ? O1 Na1 Nb1 36.31(5) . . ? C16 Na1 Nb1 76.13(8) . . ? C3 Na1 Nb1 52.42(7) . . ? C11 Na1 Nb1 56.99(6) . . ? C15 Na1 Nb1 104.17(8) . . ? C1 Na1 Nb1 50.93(6) . . ? C1 P1 C3 94.12(13) . . ? C1 P1 Nb1 76.17(9) . . ? C3 P1 Nb1 76.37(9) . . ? O1 C1 C2 123.5(3) . . ? O1 C1 P1 108.8(2) . . ? C2 C1 P1 127.6(2) . . ? O1 C1 Na1 57.19(14) . . ? C2 C1 Na1 111.8(2) . . ? P1 C1 Na1 98.33(12) . . ? C4S O1S C1S 109.1(3) . . ? C4S O1S Na1 121.2(2) . . ? C1S O1S Na1 122.1(2) . . ? C11 N1 C17 110.8(3) . . ? C11 N1 C17A 112.3(4) . . ? C17 N1 C17A 63.4(4) . . ? C11 N1 Nb1 126.11(19) . . ? C17 N1 Nb1 114.9(2) . . ? C17A N1 Nb1 112.8(4) . . ? C2S C1S O1S 105.8(3) . . ? C21 N2 C27 113.5(3) . . ? C21 N2 Nb1 120.3(2) . . ? C27 N2 Nb1 126.1(2) . . ? C1S C2S C3S 105.1(4) . . ? C37A N3 C31 108.7(6) . . ? C37A N3 C37 62.9(5) . . ? C31 N3 C37 112.8(3) . . ? C37A N3 Nb1 114.5(5) . . ? C31 N3 Nb1 119.6(2) . . ? C37 N3 Nb1 123.7(2) . . ? C2S C3S C4S 103.4(3) . . ? O1S C4S C3S 106.2(3) . . ? C16 C11 C12 119.1(3) . . ? C16 C11 N1 120.1(3) . . ? C12 C11 N1 120.8(3) . . ? C16 C11 Na1 67.19(17) . . ? C12 C11 Na1 96.9(2) . . ? N1 C11 Na1 104.48(17) . . ? C11 C12 C13 120.9(3) . . ? C14 C13 C12 118.6(3) . . ? C14 C13 C131 120.4(3) . . ? C12 C13 C131 121.0(3) . . ? C13 C14 C15 121.7(3) . . ? C14 C15 C16 118.4(3) . . ? C14 C15 C151 120.8(3) . . ? C16 C15 C151 120.8(3) . . ? C14 C15 Na1 96.8(2) . . ? C16 C15 Na1 63.91(17) . . ? C151 C15 Na1 108.1(2) . . ? C11 C16 C15 121.0(3) . . ? C11 C16 Na1 83.44(19) . . ? C15 C16 Na1 87.3(2) . . ? C18 C17 N1 116.7(4) . . ? C183 C18 C181 110.3(6) . . ? C183 C18 C17 106.8(5) . . ? C181 C18 C17 111.1(5) . . ? C183 C18 C182 108.0(7) . . ? C181 C18 C182 108.7(7) . . ? C17 C18 C182 112.0(8) . . ? C18A C17A N1 111.6(10) . . ? C185 C18A C184 110.5(13) . . ? C185 C18A C186 108.6(17) . . ? C184 C18A C186 108.9(17) . . ? C185 C18A C17A 111.0(13) . . ? C184 C18A C17A 105.6(12) . . ? C186 C18A C17A 112.2(17) . . ? C26 C21 C22 119.3(3) . . ? C26 C21 N2 119.5(3) . . ? C22 C21 N2 121.2(3) . . ? C23 C22 C21 120.4(3) . . ? C22 C23 C24 119.2(3) . . ? C22 C23 C231 119.2(3) . . ? C24 C23 C231 121.6(3) . . ? C23 C24 C25 121.4(3) . . ? C24 C25 C26 118.5(3) . . ? C24 C25 C251 121.4(3) . . ? C26 C25 C251 120.1(3) . . ? C21 C26 C25 121.2(3) . . ? N2 C27 C28 118.8(3) . . ? C283 C28 C27 112.1(3) . . ? C283 C28 C282 109.1(3) . . ? C27 C28 C282 105.1(3) . . ? C283 C28 C281 109.0(3) . . ? C27 C28 C281 114.2(3) . . ? C282 C28 C281 107.1(3) . . ? C32 C31 C36 118.4(3) . . ? C32 C31 N3 120.4(3) . . ? C36 C31 N3 121.2(3) . . ? C31 C32 C33 122.5(3) . . ? C34 C33 C32 118.1(4) . . ? C34 C33 C331 120.9(4) . . ? C32 C33 C331 121.0(4) . . ? C33 C34 C35 121.1(4) . . ? C36 C35 C34 119.1(4) . . ? C36 C35 C351 119.7(4) . . ? C34 C35 C351 121.3(4) . . ? C35 C36 C31 120.8(4) . . ? C38 C37 N3 116.2(4) . . ? C381 C38 C382 107.3(6) . . ? C381 C38 C37 105.3(6) . . ? C382 C38 C37 109.8(5) . . ? C381 C38 C383 106.7(6) . . ? C382 C38 C383 118.9(7) . . ? C37 C38 C383 108.0(7) . . ? N3 C37A C38A 106.6(11) . . ? C384 C38A C386 137.2(18) . . ? C384 C38A C37A 93.8(17) . . ? C386 C38A C37A 111.8(15) . . ? C384 C38A C385 88.5(15) . . ? C386 C38A C385 111.5(17) . . ? C37A C38A C385 111.0(15) . . ? C42 C41 C46 116.0(3) . . ? C42 C41 C2 123.4(3) . . ? C46 C41 C2 120.6(3) . . ? C43 C42 C41 121.9(3) . . ? C44 C43 C42 120.7(3) . . ? C45 C44 C43 118.5(3) . . ? C44 C45 C46 121.0(3) . . ? C45 C46 C41 121.9(3) . . ? C52 C51 C56 121.3(3) . . ? C53 C52 C51 120.1(3) . . ? C54 C53 C52 119.7(3) . . ? C53 C54 C55 120.0(3) . . ? C56 C55 C54 121.1(3) . . ? C55 C56 C51 117.7(3) . . ? C55 C56 C2 120.8(3) . . ? C51 C56 C2 121.4(3) . . ? C62 C61 C66 116.4(3) . . ? C62 C61 C4 124.0(3) . . ? C66 C61 C4 119.6(3) . . ? C63 C62 C61 121.0(3) . . ? C64 C63 C62 121.6(3) . . ? C63 C64 C65 118.7(3) . . ? C66 C65 C64 120.6(3) . . ? C65 C66 C61 121.9(3) . . ? C3 O2 Nb1 106.16(16) . . ? C3 O2 Na1 90.72(16) . . ? Nb1 O2 Na1 106.15(9) . . ? C1 O1 Nb1 107.09(18) . . ? C1 O1 Na1 95.54(16) . . ? Nb1 O1 Na1 99.90(9) . . ? C3 C4 C61 125.2(3) . . ? C3 C4 C70 118.7(2) . . ? C61 C4 C70 116.0(2) . . ? C71 C70 C75 117.9(3) . . ? C71 C70 C4 123.2(3) . . ? C75 C70 C4 119.0(3) . . ? C72 C71 C70 120.8(3) . . ? C73 C74 C75 120.1(3) . . ? C72 C73 C74 119.4(3) . . ? C74 C75 C70 121.3(3) . . ? O2 C3 C4 123.8(2) . . ? O2 C3 P1 110.6(2) . . ? C4 C3 P1 125.6(2) . . ? O2 C3 Na1 58.74(14) . . ? C4 C3 Na1 99.32(19) . . ? P1 C3 Na1 109.02(13) . . ? C1 C2 C41 124.3(3) . . ? C1 C2 C56 119.6(3) . . ? C41 C2 C56 115.9(2) . . ? C73 C72 C71 120.5(3) . . ? C1T C2T C3T 120.1 . . ? C2T C3T C4T 117.2 . . ? C5T C4T C3T 119.5 . . ? C3X C2X C1X 135.5 . . ? C2X C3X C4X 129.7 . . ? C5X C4X C3X 120.70(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.009 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.071