# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Joseph Schmidt' _publ_contact_author_email JOSEPH.SCHMIDT@UTOLEDO.EDU _publ_section_title ; Mono-Anionic Acetophenone Imine Ligands: Synthesis, Ortho-Lithiation and First Examples of Group V Metal Complexes ; loop_ _publ_author_name 'Joseph Schmidt' 'John F. Beck' 'Abdollah Neshat' 'Cheryl L. Seambos' # Attachment 'Schmidt_Dalton_ciffiles.txt' data_(2)2Nb(N-2,6-iPr2C6H3)Cl_(16) _database_code_depnum_ccdc_archive 'CCDC 722163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H62 Cl N3 Nb O4.50' _chemical_formula_weight 929.41 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.557(1) _cell_length_b 12.424(2) _cell_length_c 21.471(3) _cell_angle_alpha 106.767(3) _cell_angle_beta 91.047(3) _cell_angle_gamma 101.570(3) _cell_volume 2383.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 175(2) _cell_measurement_reflns_used 6448 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.15 _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.541 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 175(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 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25946 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 28.46 _reflns_number_total 11698 _reflns_number_gt 7098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1396P)^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 11698 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2340 _refine_ls_wR_factor_gt 0.2050 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.86558(4) 0.00182(4) 0.740250(18) 0.03831(15) Uani 1 1 d . . . Cl1 Cl 1.03060(12) -0.03100(12) 0.65809(5) 0.0525(3) Uani 1 1 d . . . O1 O 1.0962(5) 0.1723(4) 0.8835(2) 0.0822(14) Uani 1 1 d . . . O2 O 1.1916(5) 0.1358(4) 0.97212(19) 0.0806(13) Uani 1 1 d . . . O3 O 0.6910(4) -0.0418(4) 0.88876(16) 0.0744(13) Uani 1 1 d . . . O4 O 0.4556(4) -0.0826(5) 0.91201(18) 0.0882(16) Uani 1 1 d . . . N1 N 0.9088(4) 0.1527(4) 0.77270(19) 0.0510(10) Uani 1 1 d . . . N2 N 0.6947(4) -0.0002(4) 0.66088(17) 0.0431(9) Uani 1 1 d . . . N3 N 0.8357(4) -0.2113(3) 0.72475(18) 0.0431(9) Uani 1 1 d . . . C1 C 0.9546(7) 0.2721(5) 0.8041(3) 0.0645(16) Uani 1 1 d . . . C2 C 1.0591(9) 0.3389(6) 0.7773(4) 0.093(2) Uani 1 1 d . . . C3 C 1.1055(11) 0.4538(7) 0.8095(5) 0.115(3) Uani 1 1 d . . . H3A H 1.1747 0.4992 0.7926 0.138 Uiso 1 1 calc R . . C4 C 1.0492(12) 0.5024(7) 0.8675(6) 0.118(4) Uani 1 1 d . . . H4A H 1.0843 0.5798 0.8896 0.142 Uiso 1 1 calc R . . C5 C 0.9440(11) 0.4403(7) 0.8931(4) 0.104(3) Uani 1 1 d . . . H5A H 0.9049 0.4765 0.9308 0.125 Uiso 1 1 calc R . . C6 C 0.8948(9) 0.3224(6) 0.8628(4) 0.083(2) Uani 1 1 d . . . C7 C 1.1206(10) 0.2843(7) 0.7129(5) 0.109(3) Uani 1 1 d . . . H7A H 1.0522 0.2130 0.6898 0.131 Uiso 1 1 calc R . . C8 C 1.1457(14) 0.3595(10) 0.6666(6) 0.175(6) Uani 1 1 d . . . H8A H 1.1834 0.3190 0.6277 0.263 Uiso 1 1 calc R . . H8B H 1.2129 0.4300 0.6880 0.263 Uiso 1 1 calc R . . H8C H 1.0566 0.3764 0.6554 0.263 Uiso 1 1 calc R . . C9 C 1.2536(11) 0.2523(8) 0.7311(6) 0.141(4) Uani 1 1 d . . . H9A H 1.2323 0.2040 0.7589 0.212 Uiso 1 1 calc R . . H9B H 1.3229 0.3207 0.7538 0.212 Uiso 1 1 calc R . . H9C H 1.2917 0.2116 0.6924 0.212 Uiso 1 1 calc R . . C10 C 0.7826(10) 0.2499(7) 0.8918(3) 0.099(3) Uani 1 1 d . . . H10A H 0.7932 0.1700 0.8746 0.118 Uiso 1 1 calc R . . C11 C 0.6336(11) 0.2538(9) 0.8669(5) 0.139(4) Uani 1 1 d . . . H11A H 0.5623 0.2077 0.8849 0.208 Uiso 1 1 calc R . . H11B H 0.6231 0.2243 0.8202 0.208 Uiso 1 1 calc R . . H11C H 0.6217 0.3319 0.8801 0.208 Uiso 1 1 calc R . . C12 C 0.7975(14) 0.2798(9) 0.9653(4) 0.153(5) Uani 1 1 d . . . H12A H 0.8920 0.2763 0.9794 0.229 Uiso 1 1 calc R . . H12B H 0.7278 0.2260 0.9791 0.229 Uiso 1 1 calc R . . H12C H 0.7822 0.3562 0.9842 0.229 Uiso 1 1 calc R . . C13 C 0.6451(5) -0.0282(5) 0.7769(2) 0.0473(12) Uani 1 1 d . . . C14 C 0.6034(5) -0.0462(6) 0.8356(2) 0.0573(14) Uani 1 1 d . . . C15 C 0.4625(5) -0.0704(6) 0.8507(2) 0.0634(16) Uani 1 1 d . . . C16 C 0.3504(5) -0.0764(6) 0.8092(3) 0.0666(17) Uani 1 1 d . . . H16A H 0.2561 -0.0928 0.8197 0.080 Uiso 1 1 calc R . . C17 C 0.3842(5) -0.0565(5) 0.7497(2) 0.0572(14) Uani 1 1 d . . . H17A H 0.3112 -0.0574 0.7202 0.069 Uiso 1 1 calc R . . C18 C 0.5258(5) -0.0355(5) 0.7344(2) 0.0453(11) Uani 1 1 d . . . C19 C 0.5993(6) -0.0793(8) 0.9326(3) 0.096(3) Uani 1 1 d . . . H19A H 0.6245 -0.0270 0.9764 0.115 Uiso 1 1 calc R . . H19B H 0.6090 -0.1553 0.9331 0.115 Uiso 1 1 calc R . . C20 C 0.5604(5) -0.0176(5) 0.6722(2) 0.0482(12) Uani 1 1 d . . . C21 C 0.4438(6) -0.0189(6) 0.6236(3) 0.0710(18) Uani 1 1 d . . . H21A H 0.4854 -0.0074 0.5850 0.107 Uiso 1 1 calc R . . H21B H 0.3948 0.0416 0.6424 0.107 Uiso 1 1 calc R . . H21C H 0.3770 -0.0918 0.6124 0.107 Uiso 1 1 calc R . . C22 C 0.7377(5) 0.0405(4) 0.6060(2) 0.0457(11) Uani 1 1 d . . . C23 C 0.7696(5) -0.0361(5) 0.5487(2) 0.0474(11) Uani 1 1 d . . . C24 C 0.8218(6) 0.0095(5) 0.4995(2) 0.0568(14) Uani 1 1 d . . . H24A H 0.8431 -0.0398 0.4610 0.068 Uiso 1 1 calc R . . C25 C 0.8427(7) 0.1239(6) 0.5058(3) 0.0675(16) Uani 1 1 d . . . H25A H 0.8819 0.1521 0.4728 0.081 Uiso 1 1 calc R . . C26 C 0.8057(8) 0.1978(6) 0.5611(3) 0.0745(18) Uani 1 1 d . . . H26A H 0.8168 0.2754 0.5644 0.089 Uiso 1 1 calc R . . C27 C 0.7511(7) 0.1573(5) 0.6129(2) 0.0615(15) Uani 1 1 d . . . C28 C 0.7455(6) -0.1633(5) 0.5384(2) 0.0594(14) Uani 1 1 d . . . H28A H 0.7351 -0.1783 0.5801 0.071 Uiso 1 1 calc R . . H28B H 0.8286 -0.1906 0.5202 0.071 Uiso 1 1 calc R . . C29 C 0.6119(10) -0.2294(7) 0.4924(5) 0.113(3) Uani 1 1 d . . . H29A H 0.6009 -0.3103 0.4865 0.170 Uiso 1 1 calc R . . H29B H 0.6221 -0.2150 0.4510 0.170 Uiso 1 1 calc R . . H29C H 0.5291 -0.2043 0.5110 0.170 Uiso 1 1 calc R . . C30 C 0.7053(11) 0.2368(6) 0.6721(3) 0.099(3) Uani 1 1 d . . . H30A H 0.6245 0.1922 0.6869 0.119 Uiso 1 1 calc R . . H30B H 0.7830 0.2589 0.7061 0.119 Uiso 1 1 calc R . . C31 C 0.6670(16) 0.3358(8) 0.6690(5) 0.163(6) Uani 1 1 d . . . H31A H 0.6409 0.3760 0.7110 0.245 Uiso 1 1 calc R . . H31B H 0.5870 0.3168 0.6373 0.245 Uiso 1 1 calc R . . H31C H 0.7464 0.3840 0.6566 0.245 Uiso 1 1 calc R . . C32 C 0.9670(4) -0.0255(4) 0.8254(2) 0.0400(10) Uani 1 1 d . . . C33 C 1.0529(5) 0.0569(4) 0.8768(2) 0.0487(11) Uani 1 1 d . . . C34 C 1.1115(5) 0.0347(5) 0.9304(2) 0.0550(13) Uani 1 1 d . . . C35 C 1.0872(6) -0.0715(6) 0.9370(2) 0.0623(15) Uani 1 1 d . . . H35A H 1.1240 -0.0859 0.9735 0.075 Uiso 1 1 calc R . . C36 C 1.0048(6) -0.1581(5) 0.8868(2) 0.0544(13) Uani 1 1 d . . . H36A H 0.9858 -0.2329 0.8895 0.065 Uiso 1 1 calc R . . C37 C 0.9488(5) -0.1371(4) 0.8319(2) 0.0439(11) Uani 1 1 d . . . C38 C 1.1990(9) 0.2193(6) 0.9382(4) 0.099(3) Uani 1 1 d . . . H38A H 1.2942 0.2371 0.9239 0.119 Uiso 1 1 calc R . . H38B H 1.1781 0.2896 0.9666 0.119 Uiso 1 1 calc R . . C39 C 0.8760(5) -0.2346(4) 0.7762(2) 0.0466(11) Uani 1 1 d . . . C40 C 0.8584(9) -0.3563(5) 0.7795(3) 0.088(2) Uani 1 1 d . . . H40A H 0.8096 -0.4091 0.7396 0.132 Uiso 1 1 calc R . . H40B H 0.8034 -0.3648 0.8154 0.132 Uiso 1 1 calc R . . H40C H 0.9510 -0.3722 0.7857 0.132 Uiso 1 1 calc R . . C41 C 0.7882(6) -0.3068(4) 0.6659(2) 0.0524(12) Uani 1 1 d . A . C42 C 0.6415(7) -0.3525(5) 0.6482(3) 0.0706(17) Uani 1 1 d . . . C43 C 0.6015(9) -0.4403(7) 0.5903(4) 0.094(2) Uani 1 1 d . A . H43A H 0.5048 -0.4717 0.5777 0.113 Uiso 1 1 calc R . . C44 C 0.7002(11) -0.4809(7) 0.5521(4) 0.101(3) Uani 1 1 d . . . H44A H 0.6708 -0.5380 0.5126 0.122 Uiso 1 1 calc R A . C45 C 0.8453(9) -0.4394(6) 0.5704(3) 0.089(2) Uani 1 1 d . A . H45A H 0.9121 -0.4704 0.5439 0.107 Uiso 1 1 calc R . . C46 C 0.8909(6) -0.3522(5) 0.6280(3) 0.0609(14) Uani 1 1 d . . . C47 C 0.5302(7) -0.3139(7) 0.6912(5) 0.103(3) Uani 1 1 d . A 1 H47A H 0.4534 -0.3058 0.6638 0.124 Uiso 1 1 calc R A 1 H47B H 0.5718 -0.2377 0.7201 0.124 Uiso 1 1 calc R A 1 C47 C 0.5301 -0.3140 0.6912 0.104 Uani 0.00 1 d P A 2 C48 C 0.460(6) -0.399(5) 0.705(3) 0.30(5) Uani 0.50 1 d P A 2 H48A H 0.3805 -0.3776 0.7292 0.447 Uiso 0.50 1 calc PR A 2 H48B H 0.5204 -0.4244 0.7319 0.447 Uiso 0.50 1 calc PR A 2 H48C H 0.4243 -0.4604 0.6662 0.447 Uiso 0.50 1 calc PR A 2 C48A C 0.465(5) -0.386(2) 0.732(2) 0.163(16) Uani 0.50 1 d P A 1 H48D H 0.3764 -0.4352 0.7103 0.244 Uiso 0.50 1 calc PR A 1 H48E H 0.4465 -0.3370 0.7734 0.244 Uiso 0.50 1 calc PR A 1 H48F H 0.5294 -0.4321 0.7392 0.244 Uiso 0.50 1 calc PR A 1 C49 C 1.0489(6) -0.3127(6) 0.6503(3) 0.0765(18) Uani 1 1 d . A . H49A H 1.0699 -0.2294 0.6675 0.092 Uiso 1 1 calc R . . H49B H 1.0657 -0.3423 0.6863 0.092 Uiso 1 1 calc R . . C50 C 1.1553(9) -0.3456(8) 0.6012(4) 0.110(3) Uani 1 1 d . . . H50A H 1.2508 -0.3162 0.6219 0.165 Uiso 1 1 calc R A . H50B H 1.1446 -0.3135 0.5661 0.165 Uiso 1 1 calc R . . H50C H 1.1384 -0.4279 0.5842 0.165 Uiso 1 1 calc R . . O9 O 0.5000 0.5000 1.0000 0.159(4) Uiso 1 2 d S . . C98 C 0.532(2) 0.5532(16) 0.9662(9) 0.100(5) Uiso 0.50 1 d P B 2 H98C H 0.6304 0.5489 0.9580 0.120 Uiso 0.50 1 calc PR B 2 H98D H 0.5345 0.6321 0.9916 0.120 Uiso 0.50 1 calc PR B 2 C98A C 0.437(3) 0.5095(18) 0.9426(12) 0.122(6) Uiso 0.50 1 d P B 1 H98A H 0.4259 0.4370 0.9084 0.146 Uiso 0.50 1 calc PR B 1 H98B H 0.3426 0.5255 0.9504 0.146 Uiso 0.50 1 calc PR B 1 C99 C 0.453(3) 0.537(3) 0.8972(15) 0.169(11) Uiso 0.50 1 d P B 2 H99D H 0.3811 0.4666 0.8852 0.253 Uiso 0.50 1 calc PR B 2 H99E H 0.5215 0.5330 0.8649 0.253 Uiso 0.50 1 calc PR B 2 H99F H 0.4086 0.6005 0.8998 0.253 Uiso 0.50 1 calc PR B 2 C99A C 0.521(3) 0.598(3) 0.9222(18) 0.183(12) Uiso 0.50 1 d P B 1 H99A H 0.4758 0.6019 0.8829 0.275 Uiso 0.50 1 calc PR B 1 H99B H 0.6142 0.5812 0.9139 0.275 Uiso 0.50 1 calc PR B 1 H99C H 0.5307 0.6696 0.9557 0.275 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 0.0285(2) 0.0595(3) 0.0256(2) 0.00542(17) -0.00499(14) 0.01764(17) Cl1 0.0376(6) 0.0839(9) 0.0316(6) 0.0098(6) 0.0033(4) 0.0142(6) O1 0.105(3) 0.071(3) 0.052(2) -0.009(2) -0.051(2) 0.022(2) O2 0.087(3) 0.097(3) 0.040(2) -0.002(2) -0.035(2) 0.014(2) O3 0.0414(19) 0.164(4) 0.0296(18) 0.034(2) 0.0037(14) 0.040(2) O4 0.045(2) 0.195(5) 0.037(2) 0.044(3) 0.0128(16) 0.040(3) N1 0.052(2) 0.067(3) 0.034(2) 0.006(2) -0.0128(17) 0.027(2) N2 0.039(2) 0.070(3) 0.0222(17) 0.0111(17) -0.0034(14) 0.0207(19) N3 0.0350(19) 0.058(2) 0.032(2) 0.0061(18) -0.0055(15) 0.0122(17) C1 0.073(4) 0.063(3) 0.051(3) -0.002(3) -0.023(3) 0.030(3) C2 0.097(6) 0.065(4) 0.094(6) 0.001(4) -0.021(4) 0.004(4) C3 0.128(8) 0.074(5) 0.116(8) -0.002(5) -0.035(6) 0.007(5) C4 0.144(9) 0.065(5) 0.127(9) 0.001(5) -0.065(7) 0.026(5) C5 0.137(8) 0.085(5) 0.081(6) -0.014(4) -0.023(5) 0.063(6) C6 0.099(5) 0.070(4) 0.069(4) -0.011(3) -0.024(4) 0.044(4) C7 0.101(7) 0.083(5) 0.119(8) 0.013(5) -0.003(5) -0.007(5) C8 0.197(13) 0.135(9) 0.166(12) 0.057(9) 0.012(10) -0.045(9) C9 0.114(8) 0.094(6) 0.189(12) 0.008(7) 0.004(8) 0.011(6) C10 0.128(7) 0.107(6) 0.052(4) -0.019(4) -0.006(4) 0.068(5) C11 0.121(8) 0.145(8) 0.134(9) -0.017(7) 0.015(7) 0.076(7) C12 0.242(14) 0.155(9) 0.062(5) -0.007(6) 0.017(7) 0.101(9) C13 0.032(2) 0.080(3) 0.028(2) 0.003(2) -0.0038(17) 0.025(2) C14 0.040(3) 0.109(4) 0.029(2) 0.016(3) 0.0006(19) 0.037(3) C15 0.046(3) 0.123(5) 0.024(2) 0.016(3) 0.0032(19) 0.035(3) C16 0.037(3) 0.130(5) 0.038(3) 0.020(3) 0.006(2) 0.035(3) C17 0.038(2) 0.105(4) 0.026(2) 0.008(3) -0.0056(18) 0.029(3) C18 0.036(2) 0.073(3) 0.026(2) 0.007(2) -0.0034(17) 0.022(2) C19 0.051(3) 0.217(9) 0.035(3) 0.049(4) 0.007(2) 0.045(4) C20 0.036(2) 0.083(3) 0.028(2) 0.012(2) -0.0056(17) 0.025(2) C21 0.048(3) 0.137(6) 0.036(3) 0.026(3) -0.012(2) 0.037(3) C22 0.041(2) 0.067(3) 0.030(2) 0.013(2) -0.0052(18) 0.018(2) C23 0.040(2) 0.074(3) 0.026(2) 0.011(2) -0.0061(18) 0.012(2) C24 0.057(3) 0.085(4) 0.027(2) 0.013(3) -0.005(2) 0.016(3) C25 0.071(4) 0.095(5) 0.040(3) 0.028(3) -0.004(3) 0.016(3) C26 0.102(5) 0.076(4) 0.052(4) 0.030(3) -0.010(3) 0.021(4) C27 0.082(4) 0.076(4) 0.032(3) 0.014(3) -0.007(2) 0.034(3) C28 0.071(4) 0.070(3) 0.027(2) 0.004(2) -0.008(2) 0.009(3) C29 0.111(6) 0.092(5) 0.106(7) 0.012(5) -0.049(5) -0.018(5) C30 0.172(8) 0.097(5) 0.047(4) 0.013(4) -0.001(4) 0.082(6) C31 0.315(17) 0.111(7) 0.105(8) 0.037(6) 0.076(9) 0.128(10) C32 0.033(2) 0.058(3) 0.025(2) 0.0026(19) -0.0013(16) 0.016(2) C33 0.047(3) 0.062(3) 0.033(2) 0.001(2) -0.0105(19) 0.021(2) C34 0.050(3) 0.082(4) 0.026(2) 0.000(2) -0.009(2) 0.022(3) C35 0.058(3) 0.107(5) 0.025(2) 0.021(3) -0.004(2) 0.024(3) C36 0.060(3) 0.077(4) 0.029(2) 0.018(2) 0.000(2) 0.015(3) C37 0.034(2) 0.071(3) 0.026(2) 0.012(2) 0.0003(17) 0.012(2) C38 0.119(6) 0.089(5) 0.069(5) 0.002(4) -0.065(4) 0.016(4) C39 0.044(3) 0.057(3) 0.037(3) 0.015(2) -0.0015(19) 0.006(2) C40 0.127(6) 0.071(4) 0.059(4) 0.028(3) -0.023(4) -0.004(4) C41 0.051(3) 0.056(3) 0.041(3) 0.009(2) -0.016(2) 0.000(2) C42 0.057(3) 0.066(4) 0.079(4) 0.017(3) -0.027(3) -0.001(3) C43 0.084(5) 0.088(5) 0.087(6) 0.015(4) -0.055(4) -0.017(4) C44 0.124(7) 0.091(5) 0.055(4) -0.004(4) -0.043(4) -0.011(5) C45 0.098(5) 0.090(5) 0.048(4) -0.011(3) -0.008(3) -0.002(4) C46 0.067(4) 0.063(3) 0.036(3) -0.005(2) -0.009(2) 0.008(3) C47 0.038(4) 0.080(5) 0.162(9) 0.006(5) -0.020(4) -0.006(3) C47 0.039 0.080 0.162 0.005 -0.020 -0.005 C48 0.19(5) 0.28(5) 0.46(12) 0.11(6) 0.22(7) 0.11(4) C48A 0.21(4) 0.067(11) 0.20(3) 0.033(14) 0.15(3) 0.009(15) C49 0.058(4) 0.080(4) 0.069(4) -0.010(3) 0.000(3) 0.013(3) C50 0.101(6) 0.130(7) 0.086(6) 0.006(5) 0.007(5) 0.035(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 N1 1.760(4) . ? Nb1 C32 2.196(4) . ? Nb1 C13 2.261(4) . ? Nb1 N2 2.330(3) . ? Nb1 Cl1 2.3895(12) . ? Nb1 N3 2.528(4) . ? O1 C33 1.374(7) . ? O1 C38 1.420(7) . ? O2 C34 1.381(7) . ? O2 C38 1.420(8) . ? O3 C14 1.384(5) . ? O3 C19 1.411(7) . ? O4 C15 1.368(6) . ? O4 C19 1.424(7) . ? N1 C1 1.413(7) . ? N2 C20 1.297(6) . ? N2 C22 1.447(6) . ? N3 C39 1.291(6) . ? N3 C41 1.452(6) . ? C1 C2 1.409(10) . ? C1 C6 1.420(9) . ? C2 C3 1.371(10) . ? C2 C7 1.538(12) . ? C3 C4 1.387(14) . ? C4 C5 1.364(13) . ? C5 C6 1.398(11) . ? C6 C10 1.521(11) . ? C7 C9 1.483(13) . ? C7 C8 1.540(14) . ? C10 C12 1.509(11) . ? C10 C11 1.527(12) . ? C13 C14 1.394(6) . ? C13 C18 1.420(6) . ? C14 C15 1.385(7) . ? C15 C16 1.358(7) . ? C16 C17 1.401(7) . ? C17 C18 1.391(6) . ? C18 C20 1.448(6) . ? C20 C21 1.507(6) . ? C22 C27 1.394(8) . ? C22 C23 1.402(7) . ? C23 C24 1.392(7) . ? C23 C28 1.499(8) . ? C24 C25 1.361(8) . ? C25 C26 1.376(9) . ? C26 C27 1.416(8) . ? C27 C30 1.501(8) . ? C28 C29 1.531(9) . ? C30 C31 1.371(10) . ? C32 C33 1.386(6) . ? C32 C37 1.409(7) . ? C33 C34 1.391(7) . ? C34 C35 1.343(8) . ? C35 C36 1.378(8) . ? C36 C37 1.398(6) . ? C37 C39 1.475(7) . ? C39 C40 1.510(8) . ? C41 C46 1.389(8) . ? C41 C42 1.403(8) . ? C42 C43 1.384(10) . ? C42 C47 1.483(7) . ? C42 C47 1.483(11) . ? C43 C44 1.340(12) . ? C44 C45 1.385(11) . ? C45 C46 1.382(8) . ? C46 C49 1.514(8) . ? C47 C48A 1.49(3) . ? C47 C48 1.25(5) . ? C49 C50 1.508(10) . ? O9 C98 1.123(19) . ? O9 C98 1.123(19) 2_667 ? O9 C98A 1.41(2) . ? O9 C98A 1.41(2) 2_667 ? C98 C99 1.59(4) . ? C98A C99A 1.40(3) . ? 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 N1 Nb1 C32 93.65(17) . . ? N1 Nb1 C13 97.64(19) . . ? C32 Nb1 C13 92.49(16) . . ? N1 Nb1 N2 94.66(16) . . ? C32 Nb1 N2 161.94(15) . . ? C13 Nb1 N2 70.54(15) . . ? N1 Nb1 Cl1 101.96(14) . . ? C32 Nb1 Cl1 104.92(11) . . ? C13 Nb1 Cl1 152.71(13) . . ? N2 Nb1 Cl1 88.99(9) . . ? N1 Nb1 N3 163.72(15) . . ? C32 Nb1 N3 70.10(15) . . ? C13 Nb1 N3 82.52(16) . . ? N2 Nb1 N3 100.68(13) . . ? Cl1 Nb1 N3 83.87(9) . . ? C33 O1 C38 106.7(5) . . ? C34 O2 C38 105.7(4) . . ? C14 O3 C19 106.2(4) . . ? C15 O4 C19 104.9(4) . . ? C1 N1 Nb1 173.3(3) . . ? C20 N2 C22 119.1(4) . . ? C20 N2 Nb1 119.2(3) . . ? C22 N2 Nb1 120.5(3) . . ? C39 N3 C41 117.8(4) . . ? C39 N3 Nb1 113.5(3) . . ? C41 N3 Nb1 128.7(3) . . ? C2 C1 N1 119.7(6) . . ? C2 C1 C6 121.1(6) . . ? N1 C1 C6 119.2(6) . . ? C3 C2 C1 118.9(9) . . ? C3 C2 C7 120.3(9) . . ? C1 C2 C7 120.8(6) . . ? C2 C3 C4 119.9(10) . . ? C5 C4 C3 122.2(8) . . ? C4 C5 C6 120.1(8) . . ? C5 C6 C1 117.7(8) . . ? C5 C6 C10 121.3(7) . . ? C1 C6 C10 121.0(6) . . ? C9 C7 C2 106.3(9) . . ? C9 C7 C8 112.4(10) . . ? C2 C7 C8 114.9(8) . . ? C12 C10 C6 115.1(8) . . ? C12 C10 C11 111.5(8) . . ? C6 C10 C11 109.1(8) . . ? C14 C13 C18 112.0(4) . . ? C14 C13 Nb1 130.2(3) . . ? C18 C13 Nb1 117.8(3) . . ? O3 C14 C15 108.0(4) . . ? O3 C14 C13 127.6(4) . . ? C15 C14 C13 124.5(4) . . ? C16 C15 O4 126.8(5) . . ? C16 C15 C14 122.3(5) . . ? O4 C15 C14 110.9(4) . . ? C15 C16 C17 116.6(5) . . ? C18 C17 C16 120.6(4) . . ? C17 C18 C13 124.1(4) . . ? C17 C18 C20 120.6(4) . . ? C13 C18 C20 115.4(4) . . ? O3 C19 O4 108.5(4) . . ? N2 C20 C18 117.1(4) . . ? N2 C20 C21 122.3(4) . . ? C18 C20 C21 120.6(4) . . ? C27 C22 C23 121.9(4) . . ? C27 C22 N2 118.1(4) . . ? C23 C22 N2 119.9(4) . . ? C24 C23 C22 117.4(5) . . ? C24 C23 C28 119.9(5) . . ? C22 C23 C28 122.6(4) . . ? C25 C24 C23 122.3(5) . . ? C24 C25 C26 119.8(5) . . ? C25 C26 C27 121.0(6) . . ? C22 C27 C26 117.5(5) . . ? C22 C27 C30 121.5(5) . . ? C26 C27 C30 121.0(6) . . ? C23 C28 C29 111.9(5) . . ? C31 C30 C27 120.6(6) . . ? C33 C32 C37 112.4(4) . . ? C33 C32 Nb1 127.3(4) . . ? C37 C32 Nb1 120.3(3) . . ? O1 C33 C32 126.6(4) . . ? O1 C33 C34 108.7(4) . . ? C32 C33 C34 124.7(5) . . ? C35 C34 O2 128.6(5) . . ? C35 C34 C33 121.9(5) . . ? O2 C34 C33 109.5(5) . . ? C34 C35 C36 116.3(5) . . ? C35 C36 C37 122.2(5) . . ? C36 C37 C32 122.4(5) . . ? C36 C37 C39 119.7(5) . . ? C32 C37 C39 117.7(4) . . ? O2 C38 O1 107.6(6) . . ? N3 C39 C37 117.4(4) . . ? N3 C39 C40 122.6(5) . . ? C37 C39 C40 119.9(4) . . ? C46 C41 C42 120.9(5) . . ? C46 C41 N3 118.6(4) . . ? C42 C41 N3 120.5(5) . . ? C43 C42 C41 118.3(7) . . ? C43 C42 C47 119.6(6) . . ? C41 C42 C47 122.0(5) . . ? C43 C42 C47 119.6(6) . . ? C41 C42 C47 122.0(6) . . ? C47 C42 C47 0.1(4) . . ? C44 C43 C42 120.9(7) . . ? C43 C44 C45 121.2(7) . . ? C46 C45 C44 120.1(7) . . ? C45 C46 C41 118.4(6) . . ? C45 C46 C49 120.1(6) . . ? C41 C46 C49 121.4(5) . . ? C42 C47 C48A 118.7(15) . . ? C48 C47 C42 108(2) . . ? C50 C49 C46 118.2(6) . . ? C98 O9 C98 180.000(14) . 2_667 ? C98 O9 C98A 44.8(11) . . ? C98 O9 C98A 135.2(11) 2_667 . ? C98 O9 C98A 135.2(11) . 2_667 ? C98 O9 C98A 44.8(11) 2_667 2_667 ? C98A O9 C98A 180.000(14) . 2_667 ? O9 C98 C99 126(2) . . ? C99A C98A O9 111(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.599 _refine_diff_density_min -2.484 _refine_diff_density_rms 0.131 data_(3)2Nb(N-2,6-iPr2C6H3)Cl_(17) _database_code_depnum_ccdc_archive 'CCDC 722164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H49 Cl N3 Nb O4' _chemical_formula_weight 836.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4669(6) _cell_length_b 12.2295(5) _cell_length_c 25.2702(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.7740(10) _cell_angle_gamma 90.00 _cell_volume 4101.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 5648 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.25 _exptl_crystal_description red _exptl_crystal_colour block _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45419 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.29 _reflns_number_total 10183 _reflns_number_gt 7393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^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 10183 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _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 0.698645(14) 0.800808(15) 0.364364(7) 0.01461(6) Uani 1 1 d . . . Cl1 Cl 0.56537(4) 0.92287(4) 0.37559(2) 0.02340(12) Uani 1 1 d . . . O1 O 0.83049(13) 0.58593(13) 0.29848(6) 0.0299(4) Uani 1 1 d . . . O2 O 0.92695(14) 0.43667(14) 0.32950(7) 0.0353(4) Uani 1 1 d . . . O3 O 0.79779(13) 0.90704(14) 0.25052(6) 0.0319(4) Uani 1 1 d . . . O4 O 0.79236(15) 0.84870(17) 0.16335(7) 0.0414(5) Uani 1 1 d . . . N1 N 0.80090(14) 0.89208(14) 0.36608(7) 0.0182(4) Uani 1 1 d . . . N2 N 0.72385(13) 0.77485(14) 0.45786(7) 0.0171(4) Uani 1 1 d . . . N3 N 0.56128(14) 0.66627(15) 0.33658(7) 0.0196(4) Uani 1 1 d . . . C1 C 0.88093(17) 0.96421(18) 0.36236(8) 0.0221(5) Uani 1 1 d . . . C2 C 0.97296(18) 0.92279(19) 0.35103(8) 0.0239(5) Uani 1 1 d . . . C3 C 1.04991(19) 0.9964(2) 0.34798(9) 0.0323(6) Uani 1 1 d . . . H3A H 1.1117 0.9706 0.3415 0.039 Uiso 1 1 calc R . . C4 C 1.0369(2) 1.1082(2) 0.35437(10) 0.0375(7) Uani 1 1 d . . . H4A H 1.0891 1.1564 0.3513 0.045 Uiso 1 1 calc R . . C5 C 0.9471(2) 1.1470(2) 0.36524(11) 0.0372(6) Uani 1 1 d . . . H5A H 0.9389 1.2219 0.3693 0.045 Uiso 1 1 calc R . . C6 C 0.8678(2) 1.07729(19) 0.37030(10) 0.0312(6) Uani 1 1 d . . . C7 C 0.98635(18) 0.8005(2) 0.34396(10) 0.0277(5) Uani 1 1 d . . . H7A H 0.9189 0.7688 0.3342 0.033 Uiso 1 1 calc R . . C8 C 1.0448(2) 0.7715(2) 0.29911(11) 0.0406(7) Uani 1 1 d . . . H8A H 1.0130 0.8051 0.2662 0.061 Uiso 1 1 calc R . . H8B H 1.0453 0.6936 0.2946 0.061 Uiso 1 1 calc R . . H8C H 1.1127 0.7976 0.3083 0.061 Uiso 1 1 calc R . . C9 C 1.0344(2) 0.7488(2) 0.39736(11) 0.0368(6) Uani 1 1 d . . . H9A H 0.9958 0.7680 0.4246 0.055 Uiso 1 1 calc R . . H9B H 1.1021 0.7754 0.4074 0.055 Uiso 1 1 calc R . . H9C H 1.0354 0.6708 0.3936 0.055 Uiso 1 1 calc R . . C10 C 0.7686(2) 1.1212(2) 0.38240(13) 0.0461(8) Uani 1 1 d . . . H10A H 0.7305 1.0589 0.3928 0.055 Uiso 1 1 calc R . . C11 C 0.7086(3) 1.1691(4) 0.33236(16) 0.0897(15) Uani 1 1 d . . . H11A H 0.6457 1.1964 0.3400 0.135 Uiso 1 1 calc R . . H11B H 0.6960 1.1137 0.3051 0.135 Uiso 1 1 calc R . . H11C H 0.7458 1.2280 0.3199 0.135 Uiso 1 1 calc R . . C12 C 0.7780(3) 1.2040(3) 0.42756(15) 0.0623(9) Uani 1 1 d . . . H12A H 0.8154 1.1725 0.4597 0.093 Uiso 1 1 calc R . . H12B H 0.7120 1.2243 0.4337 0.093 Uiso 1 1 calc R . . H12C H 0.8126 1.2677 0.4179 0.093 Uiso 1 1 calc R . . C13 C 0.79067(16) 0.64776(16) 0.38590(8) 0.0173(4) Uani 1 1 d . . . C14 C 0.83318(17) 0.57713(18) 0.35355(9) 0.0208(5) Uani 1 1 d . . . C15 C 0.89230(18) 0.48741(18) 0.37159(9) 0.0253(5) Uani 1 1 d . . . C16 C 0.91429(18) 0.45995(19) 0.42455(10) 0.0281(5) Uani 1 1 d . . . H16A H 0.9542 0.3998 0.4365 0.034 Uiso 1 1 calc R . . C17 C 0.87333(17) 0.52748(18) 0.45986(9) 0.0239(5) Uani 1 1 d . . . H17A H 0.8857 0.5119 0.4964 0.029 Uiso 1 1 calc R . . C18 C 0.81439(16) 0.61763(17) 0.44140(8) 0.0192(4) Uani 1 1 d . . . C19 C 0.8700(2) 0.4870(2) 0.28254(10) 0.0375(6) Uani 1 1 d . . . H19A H 0.9131 0.5010 0.2562 0.045 Uiso 1 1 calc R . . H19B H 0.8157 0.4391 0.2665 0.045 Uiso 1 1 calc R . . C20 C 0.77680(16) 0.69221(17) 0.47883(8) 0.0193(4) Uani 1 1 d . . . C21 C 0.8020(2) 0.67530(19) 0.53841(9) 0.0284(5) Uani 1 1 d . . . H21A H 0.7708 0.7316 0.5564 0.043 Uiso 1 1 calc R . . H21B H 0.8737 0.6783 0.5495 0.043 Uiso 1 1 calc R . . H21C H 0.7775 0.6052 0.5474 0.043 Uiso 1 1 calc R . . C22 C 0.69819(16) 0.85874(17) 0.49398(8) 0.0175(4) Uani 1 1 d . . . C23 C 0.60432(16) 0.85627(17) 0.51023(8) 0.0189(4) Uani 1 1 d . . . C24 C 0.58078(18) 0.93981(18) 0.54354(8) 0.0230(5) Uani 1 1 d . . . H24A H 0.5185 0.9397 0.5548 0.028 Uiso 1 1 calc R . . C25 C 0.64857(19) 1.02266(19) 0.56007(9) 0.0278(5) Uani 1 1 d . . . H25A H 0.6313 1.0789 0.5815 0.033 Uiso 1 1 calc R . . C26 C 0.74169(19) 1.02163(19) 0.54468(9) 0.0276(5) Uani 1 1 d . . . H26A H 0.7871 1.0775 0.5562 0.033 Uiso 1 1 calc R . . C27 C 0.76984(17) 0.93891(18) 0.51215(9) 0.0222(5) Uani 1 1 d . . . C28 C 0.53031(18) 0.76641(19) 0.49346(9) 0.0250(5) Uani 1 1 d . . . H28A H 0.5580 0.7160 0.4708 0.038 Uiso 1 1 calc R . . H28B H 0.4690 0.7969 0.4741 0.038 Uiso 1 1 calc R . . H28C H 0.5164 0.7288 0.5247 0.038 Uiso 1 1 calc R . . C29 C 0.87583(17) 0.9367(2) 0.49979(9) 0.0291(5) Uani 1 1 d . . . H29A H 0.8832 0.8752 0.4771 0.044 Uiso 1 1 calc R . . H29B H 0.9231 0.9305 0.5327 0.044 Uiso 1 1 calc R . . H29C H 0.8885 1.0030 0.4817 0.044 Uiso 1 1 calc R . . C30 C 0.68544(17) 0.76600(18) 0.27797(8) 0.0210(5) Uani 1 1 d . . . C31 C 0.73537(17) 0.81712(18) 0.24166(9) 0.0230(5) Uani 1 1 d . . . C32 C 0.7325(2) 0.7827(2) 0.18871(9) 0.0314(6) Uani 1 1 d . . . C33 C 0.6790(2) 0.6938(2) 0.16846(10) 0.0433(7) Uani 1 1 d . . . H33A H 0.6788 0.6699 0.1335 0.052 Uiso 1 1 calc R . . C34 C 0.6241(2) 0.6401(2) 0.20277(10) 0.0377(6) Uani 1 1 d . . . H34A H 0.5854 0.5795 0.1903 0.045 Uiso 1 1 calc R . . C35 C 0.62600(18) 0.67539(19) 0.25538(9) 0.0250(5) Uani 1 1 d . . . C36 C 0.8198(2) 0.9376(2) 0.19948(9) 0.0359(6) Uani 1 1 d . . . H36A H 0.8910 0.9535 0.2022 0.043 Uiso 1 1 calc R . . H36B H 0.7820 1.0026 0.1865 0.043 Uiso 1 1 calc R . . C37 C 0.56040(17) 0.62440(19) 0.28939(9) 0.0247(5) Uani 1 1 d . . . C38 C 0.4939(2) 0.5293(2) 0.26848(11) 0.0398(7) Uani 1 1 d . . . H38A H 0.4562 0.5061 0.2955 0.060 Uiso 1 1 calc R . . H38B H 0.5349 0.4699 0.2598 0.060 Uiso 1 1 calc R . . H38C H 0.4484 0.5513 0.2368 0.060 Uiso 1 1 calc R . . C39 C 0.48297(17) 0.63566(18) 0.36598(9) 0.0210(5) Uani 1 1 d . . . C40 C 0.49578(18) 0.54896(19) 0.40287(10) 0.0278(5) Uani 1 1 d . . . C41 C 0.4193(2) 0.5300(2) 0.43271(10) 0.0352(6) Uani 1 1 d . . . H41A H 0.4265 0.4733 0.4576 0.042 Uiso 1 1 calc R . . C42 C 0.3338(2) 0.5930(2) 0.42618(11) 0.0390(7) Uani 1 1 d . . . H42A H 0.2855 0.5814 0.4479 0.047 Uiso 1 1 calc R . . C43 C 0.31953(19) 0.6731(2) 0.38767(10) 0.0332(6) Uani 1 1 d . . . H43A H 0.2601 0.7134 0.3825 0.040 Uiso 1 1 calc R . . C44 C 0.39263(18) 0.69508(19) 0.35605(9) 0.0259(5) Uani 1 1 d . . . C45 C 0.5872(2) 0.4761(2) 0.40952(12) 0.0389(6) Uani 1 1 d . . . H45A H 0.6318 0.5004 0.3860 0.058 Uiso 1 1 calc R . . H45B H 0.5667 0.4022 0.4007 0.058 Uiso 1 1 calc R . . H45C H 0.6214 0.4793 0.4461 0.058 Uiso 1 1 calc R . . C46 C 0.36987(19) 0.7771(2) 0.31108(10) 0.0350(6) Uani 1 1 d . . . H46A H 0.4271 0.7838 0.2933 0.053 Uiso 1 1 calc R . . H46B H 0.3553 0.8468 0.3255 0.053 Uiso 1 1 calc R . . H46C H 0.3126 0.7528 0.2858 0.053 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 0.01651(10) 0.01493(9) 0.01245(9) -0.00092(7) 0.00264(7) 0.00081(8) Cl1 0.0249(3) 0.0232(3) 0.0227(3) 0.0003(2) 0.0056(2) 0.0078(2) O1 0.0427(11) 0.0287(9) 0.0196(8) -0.0056(7) 0.0095(7) 0.0118(8) O2 0.0444(11) 0.0300(9) 0.0330(10) -0.0072(7) 0.0109(8) 0.0141(8) O3 0.0422(11) 0.0377(10) 0.0177(8) 0.0003(7) 0.0106(7) -0.0156(8) O4 0.0515(12) 0.0575(12) 0.0182(9) -0.0033(8) 0.0143(8) -0.0160(10) N1 0.0229(10) 0.0167(9) 0.0147(8) -0.0009(7) 0.0023(7) 0.0003(8) N2 0.0186(9) 0.0187(9) 0.0145(8) -0.0009(7) 0.0037(7) 0.0012(7) N3 0.0196(10) 0.0200(9) 0.0188(9) -0.0014(7) 0.0020(7) -0.0019(7) C1 0.0258(12) 0.0242(11) 0.0151(10) 0.0018(8) 0.0002(9) -0.0081(10) C2 0.0256(13) 0.0309(13) 0.0146(10) 0.0024(9) 0.0022(9) -0.0067(10) C3 0.0273(14) 0.0459(16) 0.0240(12) 0.0010(11) 0.0050(10) -0.0112(12) C4 0.0457(17) 0.0383(15) 0.0276(13) 0.0014(11) 0.0032(12) -0.0260(13) C5 0.0475(17) 0.0260(13) 0.0374(15) -0.0006(11) 0.0056(13) -0.0149(13) C6 0.0376(15) 0.0231(12) 0.0315(13) -0.0009(10) 0.0018(11) -0.0088(11) C7 0.0200(12) 0.0333(13) 0.0308(12) 0.0006(11) 0.0075(10) -0.0034(11) C8 0.0372(16) 0.0430(16) 0.0460(17) 0.0006(13) 0.0193(13) 0.0016(13) C9 0.0277(14) 0.0383(15) 0.0440(16) 0.0090(12) 0.0046(12) -0.0038(12) C10 0.0421(17) 0.0195(13) 0.077(2) -0.0055(13) 0.0116(15) -0.0033(12) C11 0.069(3) 0.119(4) 0.069(3) -0.019(2) -0.021(2) 0.031(3) C12 0.073(3) 0.0432(19) 0.074(2) -0.0023(17) 0.022(2) 0.0095(18) C13 0.0182(11) 0.0150(10) 0.0186(10) -0.0005(8) 0.0026(8) -0.0009(9) C14 0.0211(12) 0.0210(11) 0.0202(11) -0.0010(9) 0.0032(9) -0.0002(9) C15 0.0252(13) 0.0195(11) 0.0321(13) -0.0081(9) 0.0072(10) 0.0037(10) C16 0.0277(13) 0.0201(11) 0.0356(14) 0.0001(10) 0.0030(11) 0.0075(10) C17 0.0267(13) 0.0207(11) 0.0237(12) 0.0028(9) 0.0020(10) 0.0032(10) C18 0.0184(11) 0.0183(10) 0.0207(11) -0.0010(8) 0.0029(9) -0.0011(9) C19 0.0460(17) 0.0352(15) 0.0319(14) -0.0116(11) 0.0080(12) 0.0134(13) C20 0.0196(11) 0.0206(11) 0.0178(10) 0.0017(9) 0.0033(8) 0.0002(9) C21 0.0365(14) 0.0308(13) 0.0176(11) 0.0025(9) 0.0036(10) 0.0118(11) C22 0.0220(12) 0.0175(10) 0.0126(10) 0.0002(8) 0.0020(8) 0.0030(9) C23 0.0232(12) 0.0195(11) 0.0139(10) 0.0022(8) 0.0024(9) 0.0047(9) C24 0.0250(12) 0.0281(12) 0.0166(10) 0.0003(9) 0.0055(9) 0.0076(10) C25 0.0388(15) 0.0239(12) 0.0204(11) -0.0051(9) 0.0039(10) 0.0077(11) C26 0.0331(14) 0.0249(12) 0.0234(12) -0.0063(9) 0.0010(10) -0.0045(10) C27 0.0240(12) 0.0252(12) 0.0169(11) -0.0001(9) 0.0024(9) 0.0005(9) C28 0.0247(13) 0.0259(12) 0.0256(12) 0.0005(9) 0.0074(10) -0.0006(10) C29 0.0257(13) 0.0377(14) 0.0240(12) -0.0049(10) 0.0045(10) -0.0073(11) C30 0.0205(12) 0.0249(11) 0.0173(11) -0.0026(8) 0.0028(9) 0.0014(9) C31 0.0240(12) 0.0272(12) 0.0177(11) -0.0021(9) 0.0029(9) -0.0027(10) C32 0.0326(14) 0.0451(16) 0.0180(11) -0.0018(10) 0.0082(10) -0.0030(12) C33 0.0509(18) 0.0601(19) 0.0201(12) -0.0164(13) 0.0097(12) -0.0146(15) C34 0.0427(16) 0.0452(16) 0.0258(13) -0.0157(12) 0.0071(12) -0.0138(13) C35 0.0256(13) 0.0306(13) 0.0179(11) -0.0070(9) 0.0011(9) -0.0035(10) C36 0.0465(17) 0.0436(16) 0.0198(12) 0.0037(11) 0.0116(11) -0.0087(13) C37 0.0235(12) 0.0260(12) 0.0238(12) -0.0052(9) 0.0018(9) -0.0032(10) C38 0.0444(17) 0.0421(16) 0.0333(14) -0.0140(12) 0.0076(12) -0.0169(13) C39 0.0204(12) 0.0218(11) 0.0203(11) -0.0038(9) 0.0019(9) -0.0057(9) C40 0.0287(13) 0.0243(12) 0.0294(13) 0.0008(10) 0.0018(10) -0.0081(10) C41 0.0412(16) 0.0315(14) 0.0327(14) 0.0043(11) 0.0053(12) -0.0139(12) C42 0.0338(15) 0.0467(16) 0.0396(15) -0.0034(13) 0.0151(12) -0.0169(13) C43 0.0204(13) 0.0396(15) 0.0398(15) -0.0044(11) 0.0056(11) -0.0059(11) C44 0.0240(12) 0.0258(12) 0.0271(12) -0.0044(10) 0.0019(9) -0.0034(10) C45 0.0360(15) 0.0297(14) 0.0502(17) 0.0117(12) 0.0047(13) -0.0001(12) C46 0.0244(14) 0.0427(16) 0.0355(14) 0.0038(11) -0.0017(11) 0.0011(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N1 1.7674(18) . ? Nb1 C30 2.202(2) . ? Nb1 C13 2.260(2) . ? Nb1 N2 2.3508(17) . ? Nb1 Cl1 2.3881(6) . ? Nb1 N3 2.4862(18) . ? O1 C14 1.390(3) . ? O1 C19 1.408(3) . ? O2 C15 1.379(3) . ? O2 C19 1.437(3) . ? O3 C31 1.379(3) . ? O3 C36 1.422(3) . ? O4 C32 1.373(3) . ? O4 C36 1.428(3) . ? N1 C1 1.408(3) . ? N2 C20 1.297(3) . ? N2 C22 1.453(3) . ? N3 C37 1.296(3) . ? N3 C39 1.439(3) . ? C1 C6 1.413(3) . ? C1 C2 1.412(3) . ? C2 C3 1.385(3) . ? C2 C7 1.521(3) . ? C3 C4 1.391(4) . ? C4 C5 1.371(4) . ? C5 C6 1.389(3) . ? C6 C10 1.518(4) . ? C7 C8 1.527(3) . ? C7 C9 1.530(3) . ? C10 C11 1.499(5) . ? C10 C12 1.515(4) . ? C13 C14 1.379(3) . ? C13 C18 1.433(3) . ? C14 C15 1.386(3) . ? C15 C16 1.363(3) . ? C16 C17 1.396(3) . ? C17 C18 1.392(3) . ? C18 C20 1.465(3) . ? C20 C21 1.501(3) . ? C22 C23 1.394(3) . ? C22 C27 1.398(3) . ? C23 C24 1.394(3) . ? C23 C28 1.496(3) . ? C24 C25 1.380(3) . ? C25 C26 1.375(3) . ? C26 C27 1.396(3) . ? C27 C29 1.512(3) . ? C30 C31 1.376(3) . ? C30 C35 1.428(3) . ? C31 C32 1.397(3) . ? C32 C33 1.356(4) . ? C33 C34 1.395(4) . ? C34 C35 1.394(3) . ? C35 C37 1.472(3) . ? C37 C38 1.508(3) . ? C39 C44 1.403(3) . ? C39 C40 1.403(3) . ? C40 C41 1.395(3) . ? C40 C45 1.506(4) . ? C41 C42 1.373(4) . ? C42 C43 1.371(4) . ? C43 C44 1.395(3) . ? C44 C46 1.507(3) . ? 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 N1 Nb1 C30 94.47(8) . . ? N1 Nb1 C13 97.13(8) . . ? C30 Nb1 C13 91.57(8) . . ? N1 Nb1 N2 94.68(7) . . ? C30 Nb1 N2 160.75(7) . . ? C13 Nb1 N2 70.51(7) . . ? N1 Nb1 Cl1 101.56(6) . . ? C30 Nb1 Cl1 107.63(6) . . ? C13 Nb1 Cl1 151.84(6) . . ? N2 Nb1 Cl1 87.03(4) . . ? N1 Nb1 N3 164.61(7) . . ? C30 Nb1 N3 70.18(7) . . ? C13 Nb1 N3 82.60(7) . . ? N2 Nb1 N3 99.67(6) . . ? Cl1 Nb1 N3 84.78(5) . . ? C14 O1 C19 105.84(18) . . ? C15 O2 C19 103.94(18) . . ? C31 O3 C36 106.13(17) . . ? C32 O4 C36 104.94(18) . . ? C1 N1 Nb1 174.83(15) . . ? C20 N2 C22 117.80(17) . . ? C20 N2 Nb1 119.43(14) . . ? C22 N2 Nb1 121.78(13) . . ? C37 N3 C39 118.64(19) . . ? C37 N3 Nb1 114.30(15) . . ? C39 N3 Nb1 127.00(13) . . ? N1 C1 C6 119.2(2) . . ? N1 C1 C2 119.8(2) . . ? C6 C1 C2 121.0(2) . . ? C3 C2 C1 117.9(2) . . ? C3 C2 C7 121.9(2) . . ? C1 C2 C7 120.1(2) . . ? C2 C3 C4 121.5(3) . . ? C5 C4 C3 119.7(2) . . ? C4 C5 C6 121.6(2) . . ? C5 C6 C1 118.1(2) . . ? C5 C6 C10 121.2(2) . . ? C1 C6 C10 120.7(2) . . ? C2 C7 C8 113.7(2) . . ? C2 C7 C9 110.1(2) . . ? C8 C7 C9 111.4(2) . . ? C11 C10 C12 109.8(3) . . ? C11 C10 C6 109.6(3) . . ? C12 C10 C6 115.1(3) . . ? C14 C13 C18 111.92(19) . . ? C14 C13 Nb1 129.94(16) . . ? C18 C13 Nb1 118.09(14) . . ? C13 C14 C15 125.0(2) . . ? C13 C14 O1 127.03(19) . . ? C15 C14 O1 107.84(19) . . ? C16 C15 O2 126.9(2) . . ? C16 C15 C14 122.3(2) . . ? O2 C15 C14 110.7(2) . . ? C15 C16 C17 116.0(2) . . ? C18 C17 C16 121.3(2) . . ? C17 C18 C13 123.5(2) . . ? C17 C18 C20 121.12(19) . . ? C13 C18 C20 115.33(18) . . ? O1 C19 O2 107.85(19) . . ? N2 C20 C18 116.60(18) . . ? N2 C20 C21 122.15(19) . . ? C18 C20 C21 121.21(19) . . ? C23 C22 C27 121.90(19) . . ? C23 C22 N2 119.59(19) . . ? C27 C22 N2 118.50(19) . . ? C24 C23 C22 118.2(2) . . ? C24 C23 C28 120.0(2) . . ? C22 C23 C28 121.76(19) . . ? C25 C24 C23 120.9(2) . . ? C26 C25 C24 119.7(2) . . ? C25 C26 C27 121.7(2) . . ? C26 C27 C22 117.4(2) . . ? C26 C27 C29 119.7(2) . . ? C22 C27 C29 122.9(2) . . ? C31 C30 C35 112.96(19) . . ? C31 C30 Nb1 127.36(16) . . ? C35 C30 Nb1 119.46(16) . . ? O3 C31 C30 127.4(2) . . ? O3 C31 C32 108.2(2) . . ? C30 C31 C32 124.4(2) . . ? C33 C32 O4 127.7(2) . . ? C33 C32 C31 121.9(2) . . ? O4 C32 C31 110.3(2) . . ? C32 C33 C34 116.6(2) . . ? C35 C34 C33 121.4(2) . . ? C34 C35 C30 122.7(2) . . ? C34 C35 C37 120.7(2) . . ? C30 C35 C37 116.53(19) . . ? O3 C36 O4 107.96(19) . . ? N3 C37 C35 117.2(2) . . ? N3 C37 C38 122.6(2) . . ? C35 C37 C38 120.1(2) . . ? C44 C39 C40 121.0(2) . . ? C44 C39 N3 117.5(2) . . ? C40 C39 N3 121.4(2) . . ? C41 C40 C39 117.8(2) . . ? C41 C40 C45 120.4(2) . . ? C39 C40 C45 121.8(2) . . ? C42 C41 C40 121.5(2) . . ? C41 C42 C43 120.0(2) . . ? C42 C43 C44 121.1(3) . . ? C43 C44 C39 118.2(2) . . ? C43 C44 C46 119.1(2) . . ? C39 C44 C46 122.6(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.569 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.086 data_(4)2Nb(N-2,6-iPr2C6H3)Cl_(18) _database_code_depnum_ccdc_archive 'CCDC 722165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H49 Cl N3 Nb O4' _chemical_formula_weight 740.16 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' Cl Cl 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.678(1) _cell_length_b 11.2151(7) _cell_length_c 36.896(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7314.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 8960 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.02 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78495 _diffrn_reflns_av_R_equivalents 0.1337 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9101 _reflns_number_gt 5430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^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 9101 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 0.544346(14) 0.62730(2) 0.112772(7) 0.01566(7) Uani 1 1 d . . . Cl1 Cl 0.59384(4) 0.42934(6) 0.09786(2) 0.02351(17) Uani 1 1 d . . . O1 O 0.34654(12) 0.5749(2) 0.09510(6) 0.0349(6) Uani 1 1 d . . . O2 O 0.27573(12) 0.5660(2) 0.04223(6) 0.0383(6) Uani 1 1 d . . . O3 O 0.42273(13) 0.85160(18) 0.05792(6) 0.0339(6) Uani 1 1 d . . . O4 O 0.44189(16) 1.0505(2) 0.04719(7) 0.0502(8) Uani 1 1 d . . . N1 N 0.47299(13) 0.5909(2) 0.14486(6) 0.0190(5) Uani 1 1 d . . . N2 N 0.62130(13) 0.6753(2) 0.05903(6) 0.0171(5) Uani 1 1 d . . . N3 N 0.60878(13) 0.7312(2) 0.15897(7) 0.0218(6) Uani 1 1 d . . . C1 C 0.41499(16) 0.5658(3) 0.16963(8) 0.0204(6) Uani 1 1 d . . . C2 C 0.39272(17) 0.4469(3) 0.17554(8) 0.0238(7) Uani 1 1 d . . . C3 C 0.33532(19) 0.4257(3) 0.20054(9) 0.0321(8) Uani 1 1 d . . . H3A H 0.3201 0.3477 0.2050 0.039 Uiso 1 1 calc R . . C4 C 0.30059(19) 0.5178(3) 0.21880(9) 0.0347(8) Uani 1 1 d . . . H4A H 0.2621 0.5017 0.2353 0.042 Uiso 1 1 calc R . . C5 C 0.32293(18) 0.6342(3) 0.21268(9) 0.0319(8) Uani 1 1 d . . . H5A H 0.2988 0.6955 0.2251 0.038 Uiso 1 1 calc R . . C6 C 0.38031(17) 0.6621(3) 0.18848(8) 0.0235(7) Uani 1 1 d . . . C7 C 0.42933(18) 0.3441(3) 0.15536(9) 0.0283(8) Uani 1 1 d . . . H7A H 0.4669 0.3782 0.1388 0.034 Uiso 1 1 calc R . . C8 C 0.3728(3) 0.2763(4) 0.13265(14) 0.0785(17) Uani 1 1 d . . . H8A H 0.3980 0.2122 0.1203 0.118 Uiso 1 1 calc R . . H8B H 0.3505 0.3291 0.1152 0.118 Uiso 1 1 calc R . . H8C H 0.3339 0.2444 0.1480 0.118 Uiso 1 1 calc R . . C9 C 0.4703(3) 0.2606(4) 0.18020(12) 0.0840(18) Uani 1 1 d . . . H9A H 0.5064 0.3045 0.1943 0.126 Uiso 1 1 calc R . . H9B H 0.4961 0.2012 0.1661 0.126 Uiso 1 1 calc R . . H9C H 0.4346 0.2227 0.1961 0.126 Uiso 1 1 calc R . . C10 C 0.40424(19) 0.7896(3) 0.18133(9) 0.0289(8) Uani 1 1 d . . . H10A H 0.4559 0.7872 0.1717 0.035 Uiso 1 1 calc R . . C11 C 0.3538(2) 0.8451(3) 0.15210(10) 0.0378(9) Uani 1 1 d . . . H11A H 0.3541 0.7952 0.1309 0.057 Uiso 1 1 calc R . . H11B H 0.3727 0.9227 0.1459 0.057 Uiso 1 1 calc R . . H11C H 0.3031 0.8520 0.1611 0.057 Uiso 1 1 calc R . . C12 C 0.4055(2) 0.8677(3) 0.21541(10) 0.0455(10) Uani 1 1 d . . . H12A H 0.4381 0.8322 0.2332 0.068 Uiso 1 1 calc R . . H12B H 0.3553 0.8741 0.2251 0.068 Uiso 1 1 calc R . . H12C H 0.4240 0.9456 0.2093 0.068 Uiso 1 1 calc R . . C13 C 0.46968(15) 0.6211(3) 0.06614(8) 0.0192(6) Uani 1 1 d . . . C14 C 0.39354(17) 0.5956(3) 0.06566(8) 0.0234(7) Uani 1 1 d . . . C15 C 0.35098(17) 0.5909(3) 0.03413(9) 0.0274(7) Uani 1 1 d . . . C16 C 0.38131(18) 0.6083(3) 0.00076(9) 0.0278(7) Uani 1 1 d . . . H16A H 0.3523 0.6037 -0.0202 0.033 Uiso 1 1 calc R . . C17 C 0.45874(18) 0.6336(3) -0.00020(8) 0.0258(6) Uani 1 1 d . . . H17A H 0.4821 0.6453 -0.0225 0.031 Uiso 1 1 calc R . . C18 C 0.50185(16) 0.6419(2) 0.03122(8) 0.0198(6) Uani 1 1 d . . . C19 C 0.27250(19) 0.5691(4) 0.08111(10) 0.0487(11) Uani 1 1 d . . . H19A H 0.2438 0.6381 0.0890 0.058 Uiso 1 1 calc R . . H19B H 0.2473 0.4981 0.0901 0.058 Uiso 1 1 calc R . . C20 C 0.58300(17) 0.6764(2) 0.02932(8) 0.0202(6) Uani 1 1 d . . . C21 C 0.61116(19) 0.7140(3) -0.00754(8) 0.0298(8) Uani 1 1 d . . . H21A H 0.6639 0.7340 -0.0060 0.045 Uiso 1 1 calc R . . H21B H 0.5831 0.7822 -0.0157 0.045 Uiso 1 1 calc R . . H21C H 0.6044 0.6496 -0.0244 0.045 Uiso 1 1 calc R . . C22 C 0.70356(16) 0.7115(3) 0.05998(8) 0.0217(7) Uani 1 1 d . . . C23 C 0.70823(19) 0.8474(3) 0.05783(10) 0.0337(8) Uani 1 1 d . . . H23A H 0.6767 0.8819 0.0763 0.051 Uiso 1 1 calc R . . H23B H 0.6912 0.8735 0.0344 0.051 Uiso 1 1 calc R . . H23C H 0.7596 0.8722 0.0615 0.051 Uiso 1 1 calc R . . C24 C 0.75342(18) 0.6502(3) 0.03117(9) 0.0289(8) Uani 1 1 d . . . H24A H 0.7369 0.6736 0.0074 0.043 Uiso 1 1 calc R . . H24B H 0.7492 0.5653 0.0336 0.043 Uiso 1 1 calc R . . H24C H 0.8052 0.6736 0.0346 0.043 Uiso 1 1 calc R . . C25 C 0.73397(18) 0.6710(3) 0.09667(9) 0.0351(8) Uani 1 1 d . . . H25A H 0.7047 0.7070 0.1157 0.053 Uiso 1 1 calc R . . H25B H 0.7859 0.6949 0.0990 0.053 Uiso 1 1 calc R . . H25C H 0.7304 0.5858 0.0984 0.053 Uiso 1 1 calc R . . C26 C 0.52242(16) 0.8260(3) 0.10535(8) 0.0189(6) Uani 1 1 d . . . C27 C 0.48135(17) 0.8919(3) 0.08013(8) 0.0238(7) Uani 1 1 d . . . C28 C 0.4896(2) 1.0131(3) 0.07394(9) 0.0313(8) Uani 1 1 d . . . C29 C 0.5378(2) 1.0827(3) 0.09384(10) 0.0333(8) Uani 1 1 d . . . H29A H 0.5450 1.1632 0.0888 0.040 Uiso 1 1 calc R . . C30 C 0.57517(18) 1.0256(3) 0.12196(9) 0.0282(8) Uani 1 1 d . . . H30A H 0.6060 1.0698 0.1373 0.034 Uiso 1 1 calc R . . C31 C 0.56736(16) 0.9028(2) 0.12764(8) 0.0198(6) Uani 1 1 d . . . C32 C 0.4113(2) 0.9429(3) 0.03196(10) 0.0417(10) Uani 1 1 d . . . H32A H 0.3578 0.9525 0.0270 0.050 Uiso 1 1 calc R . . H32B H 0.4369 0.9233 0.0095 0.050 Uiso 1 1 calc R . . C33 C 0.60458(16) 0.8467(3) 0.15881(8) 0.0224(7) Uani 1 1 d . . . C34 C 0.6316(2) 0.9296(3) 0.18847(10) 0.0381(9) Uani 1 1 d . . . H34A H 0.6551 0.8838 0.2074 0.057 Uiso 1 1 calc R . . H34B H 0.5893 0.9726 0.1982 0.057 Uiso 1 1 calc R . . H34C H 0.6676 0.9849 0.1786 0.057 Uiso 1 1 calc R . . C35 C 0.64344(19) 0.6627(3) 0.19020(8) 0.0276(7) Uani 1 1 d . . . C36 C 0.72513(19) 0.7038(3) 0.19823(10) 0.0383(9) Uani 1 1 d . . . H36A H 0.7248 0.7863 0.2052 0.057 Uiso 1 1 calc R . . H36B H 0.7556 0.6940 0.1769 0.057 Uiso 1 1 calc R . . H36C H 0.7457 0.6567 0.2176 0.057 Uiso 1 1 calc R . . C37 C 0.5913(2) 0.6708(3) 0.22355(9) 0.0408(9) Uani 1 1 d . . . H37A H 0.5414 0.6441 0.2171 0.061 Uiso 1 1 calc R . . H37B H 0.5889 0.7519 0.2317 0.061 Uiso 1 1 calc R . . H37C H 0.6109 0.6213 0.2426 0.061 Uiso 1 1 calc R . . C38 C 0.6480(2) 0.5316(3) 0.17968(9) 0.0336(8) Uani 1 1 d . . . H38A H 0.5981 0.5021 0.1746 0.050 Uiso 1 1 calc R . . H38B H 0.6696 0.4868 0.1993 0.050 Uiso 1 1 calc R . . H38C H 0.6790 0.5231 0.1585 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.01566(12) 0.01380(11) 0.01753(12) 0.00018(11) 0.00058(12) 0.00070(11) Cl1 0.0275(4) 0.0167(3) 0.0263(4) 0.0010(3) 0.0043(3) 0.0044(3) O1 0.0191(11) 0.0575(16) 0.0280(13) -0.0050(12) -0.0001(10) -0.0116(11) O2 0.0235(12) 0.0554(16) 0.0361(15) -0.0090(12) -0.0064(11) -0.0060(12) O3 0.0431(14) 0.0210(12) 0.0377(14) -0.0027(10) -0.0195(12) 0.0085(10) O4 0.078(2) 0.0241(13) 0.0488(17) 0.0052(12) -0.0242(15) 0.0123(13) N1 0.0199(13) 0.0174(12) 0.0196(13) -0.0017(10) 0.0005(10) -0.0003(10) N2 0.0180(12) 0.0101(11) 0.0231(14) 0.0012(10) 0.0041(11) -0.0004(10) N3 0.0180(13) 0.0254(14) 0.0220(14) -0.0001(11) -0.0027(11) 0.0031(11) C1 0.0192(15) 0.0258(16) 0.0161(15) -0.0011(13) 0.0013(12) -0.0008(13) C2 0.0227(16) 0.0269(17) 0.0219(16) -0.0013(13) 0.0006(13) -0.0046(13) C3 0.0330(19) 0.0346(19) 0.0288(19) 0.0009(15) 0.0067(15) -0.0104(16) C4 0.0258(18) 0.049(2) 0.0295(19) -0.0018(17) 0.0113(15) -0.0059(16) C5 0.0251(17) 0.042(2) 0.0289(18) -0.0087(17) 0.0085(14) 0.0017(16) C6 0.0226(16) 0.0265(16) 0.0214(16) -0.0024(13) 0.0029(13) -0.0015(13) C7 0.0283(17) 0.0248(17) 0.0316(19) -0.0015(14) 0.0083(15) -0.0048(13) C8 0.058(3) 0.078(4) 0.099(4) -0.061(3) -0.018(3) 0.012(3) C9 0.122(5) 0.083(4) 0.047(3) 0.004(3) 0.005(3) 0.063(3) C10 0.0250(17) 0.0280(17) 0.0338(19) -0.0078(15) 0.0072(15) 0.0022(14) C11 0.038(2) 0.035(2) 0.040(2) 0.0015(16) 0.0058(17) 0.0056(16) C12 0.049(2) 0.037(2) 0.050(2) -0.0183(19) 0.0072(19) -0.0025(19) C13 0.0183(15) 0.0162(13) 0.0229(15) -0.0009(13) -0.0032(11) 0.0015(12) C14 0.0261(16) 0.0228(16) 0.0213(16) -0.0034(12) -0.0003(13) -0.0011(13) C15 0.0216(16) 0.0280(17) 0.0325(19) -0.0071(14) -0.0069(14) 0.0019(13) C16 0.0314(17) 0.0243(17) 0.0277(17) -0.0041(13) -0.0125(14) 0.0043(14) C17 0.0332(17) 0.0214(15) 0.0226(15) 0.0013(13) -0.0010(14) 0.0045(16) C18 0.0237(16) 0.0132(14) 0.0225(16) 0.0016(12) -0.0003(13) 0.0050(12) C19 0.0202(18) 0.083(3) 0.043(2) -0.008(2) -0.0013(17) -0.006(2) C20 0.0259(17) 0.0131(14) 0.0217(17) 0.0015(12) 0.0031(13) 0.0048(12) C21 0.036(2) 0.0278(17) 0.0255(18) 0.0060(14) 0.0043(15) 0.0040(15) C22 0.0166(15) 0.0193(15) 0.0291(18) -0.0002(13) 0.0062(13) -0.0011(12) C23 0.0273(18) 0.0224(18) 0.052(2) -0.0064(15) 0.0147(17) -0.0053(14) C24 0.0262(17) 0.0251(19) 0.0353(19) 0.0004(14) 0.0074(15) 0.0039(14) C25 0.0189(16) 0.052(2) 0.035(2) -0.0035(18) 0.0020(15) -0.0080(16) C26 0.0170(14) 0.0196(14) 0.0202(17) -0.0022(12) 0.0025(11) 0.0021(12) C27 0.0288(16) 0.0193(16) 0.0234(16) -0.0013(13) -0.0014(13) 0.0067(13) C28 0.042(2) 0.0199(16) 0.0319(19) 0.0026(14) -0.0013(16) 0.0091(15) C29 0.045(2) 0.0144(14) 0.040(2) -0.0008(14) 0.0049(18) -0.0011(15) C30 0.0243(16) 0.0217(16) 0.038(2) -0.0072(14) 0.0043(14) -0.0041(14) C31 0.0169(14) 0.0155(14) 0.0270(16) -0.0032(12) 0.0017(12) 0.0009(11) C32 0.058(2) 0.0287(19) 0.038(2) 0.0014(16) -0.0188(19) 0.0166(18) C33 0.0169(15) 0.0239(16) 0.0262(17) -0.0075(13) -0.0016(13) 0.0005(12) C34 0.038(2) 0.0342(19) 0.042(2) -0.0164(17) -0.0124(18) 0.0006(17) C35 0.0301(18) 0.0327(18) 0.0200(17) 0.0023(13) -0.0076(14) 0.0033(14) C36 0.033(2) 0.046(2) 0.036(2) -0.0023(17) -0.0166(17) 0.0068(18) C37 0.051(2) 0.049(2) 0.0224(19) 0.0043(17) -0.0039(17) 0.0046(19) C38 0.040(2) 0.0326(19) 0.0284(19) 0.0036(15) -0.0070(16) 0.0078(16) _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 N1 1.777(2) . ? Nb1 C13 2.170(3) . ? Nb1 C26 2.278(3) . ? Nb1 N3 2.358(2) . ? Nb1 Cl1 2.4489(7) . ? Nb1 N2 2.464(2) . ? O1 C14 1.387(4) . ? O1 C19 1.408(4) . ? O2 C15 1.392(4) . ? O2 C19 1.436(4) . ? O3 C27 1.396(4) . ? O3 C32 1.417(4) . ? O4 C28 1.364(4) . ? O4 C32 1.437(4) . ? N1 C1 1.402(4) . ? N2 C20 1.289(4) . ? N2 C22 1.510(4) . ? N3 C33 1.298(4) . ? N3 C35 1.514(4) . ? C1 C2 1.407(4) . ? C1 C6 1.423(4) . ? C2 C3 1.392(4) . ? C2 C7 1.518(4) . ? C3 C4 1.378(5) . ? C4 C5 1.382(5) . ? C5 C6 1.387(4) . ? C6 C10 1.514(4) . ? C7 C9 1.496(5) . ? C7 C8 1.510(5) . ? C10 C11 1.531(5) . ? C10 C12 1.532(4) . ? C13 C14 1.376(4) . ? C13 C18 1.427(4) . ? C14 C15 1.386(4) . ? C15 C16 1.357(4) . ? C16 C17 1.399(4) . ? C17 C18 1.390(4) . ? C18 C20 1.488(4) . ? C20 C21 1.508(4) . ? C22 C25 1.526(5) . ? C22 C23 1.529(4) . ? C22 C24 1.542(4) . ? C26 C27 1.393(4) . ? C26 C31 1.431(4) . ? C27 C28 1.387(4) . ? C28 C29 1.368(5) . ? C29 C30 1.387(5) . ? C30 C31 1.400(4) . ? C31 C33 1.467(4) . ? C33 C34 1.513(4) . ? C35 C38 1.523(4) . ? C35 C37 1.541(5) . ? C35 C36 1.545(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 N1 Nb1 C13 95.12(11) . . ? N1 Nb1 C26 100.60(10) . . ? C13 Nb1 C26 80.36(10) . . ? N1 Nb1 N3 88.56(10) . . ? C13 Nb1 N3 151.99(9) . . ? C26 Nb1 N3 71.68(9) . . ? N1 Nb1 Cl1 101.24(8) . . ? C13 Nb1 Cl1 90.59(8) . . ? C26 Nb1 Cl1 157.00(7) . . ? N3 Nb1 Cl1 115.96(6) . . ? N1 Nb1 N2 167.94(9) . . ? C13 Nb1 N2 72.82(9) . . ? C26 Nb1 N2 77.50(9) . . ? N3 Nb1 N2 101.94(8) . . ? Cl1 Nb1 N2 79.64(6) . . ? C14 O1 C19 106.1(3) . . ? C15 O2 C19 104.3(2) . . ? C27 O3 C32 105.6(2) . . ? C28 O4 C32 105.0(2) . . ? C1 N1 Nb1 177.8(2) . . ? C20 N2 C22 121.5(2) . . ? C20 N2 Nb1 113.37(19) . . ? C22 N2 Nb1 124.87(18) . . ? C33 N3 C35 122.2(3) . . ? C33 N3 Nb1 117.6(2) . . ? C35 N3 Nb1 119.65(18) . . ? N1 C1 C2 119.7(3) . . ? N1 C1 C6 118.7(3) . . ? C2 C1 C6 121.5(3) . . ? C3 C2 C1 118.0(3) . . ? C3 C2 C7 120.4(3) . . ? C1 C2 C7 121.6(3) . . ? C4 C3 C2 121.4(3) . . ? C3 C4 C5 120.1(3) . . ? C4 C5 C6 121.8(3) . . ? C5 C6 C1 117.3(3) . . ? C5 C6 C10 121.9(3) . . ? C1 C6 C10 120.7(3) . . ? C9 C7 C8 110.2(4) . . ? C9 C7 C2 112.4(3) . . ? C8 C7 C2 111.9(3) . . ? C6 C10 C11 110.1(3) . . ? C6 C10 C12 113.6(3) . . ? C11 C10 C12 110.8(3) . . ? C14 C13 C18 114.3(3) . . ? C14 C13 Nb1 127.7(2) . . ? C18 C13 Nb1 117.92(19) . . ? C13 C14 C15 123.3(3) . . ? C13 C14 O1 127.6(3) . . ? C15 C14 O1 109.0(3) . . ? C16 C15 C14 122.8(3) . . ? C16 C15 O2 127.0(3) . . ? C14 C15 O2 110.3(3) . . ? C15 C16 C17 116.0(3) . . ? C18 C17 C16 121.9(3) . . ? C17 C18 C13 121.6(3) . . ? C17 C18 C20 120.4(3) . . ? C13 C18 C20 118.0(3) . . ? O1 C19 O2 109.3(3) . . ? N2 C20 C18 117.7(3) . . ? N2 C20 C21 126.6(3) . . ? C18 C20 C21 115.7(3) . . ? N2 C22 C25 106.3(2) . . ? N2 C22 C23 108.6(2) . . ? C25 C22 C23 108.9(3) . . ? N2 C22 C24 114.5(2) . . ? C25 C22 C24 106.1(3) . . ? C23 C22 C24 112.2(3) . . ? C27 C26 C31 110.7(3) . . ? C27 C26 Nb1 133.5(2) . . ? C31 C26 Nb1 115.2(2) . . ? C28 C27 C26 125.1(3) . . ? C28 C27 O3 107.4(3) . . ? C26 C27 O3 127.4(3) . . ? O4 C28 C29 126.7(3) . . ? O4 C28 C27 110.8(3) . . ? C29 C28 C27 122.4(3) . . ? C28 C29 C30 115.8(3) . . ? C29 C30 C31 121.3(3) . . ? C30 C31 C26 124.1(3) . . ? C30 C31 C33 119.7(3) . . ? C26 C31 C33 116.2(3) . . ? O3 C32 O4 106.8(3) . . ? N3 C33 C31 117.2(3) . . ? N3 C33 C34 126.3(3) . . ? C31 C33 C34 116.5(3) . . ? N3 C35 C38 108.5(2) . . ? N3 C35 C37 109.6(3) . . ? C38 C35 C37 107.0(3) . . ? N3 C35 C36 111.9(3) . . ? C38 C35 C36 106.8(3) . . ? C37 C35 C36 112.9(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.511 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.146 data_(1)2Nb(N-2,6-Me2C6H3)Cl_(20) _database_code_depnum_ccdc_archive 'CCDC 722166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H134 Cl2 N6 Nb2 O10' _chemical_formula_weight 1932.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/n _symmetry_Int_Tables_number 14 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 24.0051(8) _cell_length_b 18.6894(6) _cell_length_c 24.3056(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.790(1) _cell_angle_gamma 90.00 _cell_volume 9977.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 7661 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 24.93 _exptl_crystal_description plate _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.939 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112567 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 28.32 _reflns_number_total 24814 _reflns_number_gt 15458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^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 24814 _refine_ls_number_parameters 1153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.720462(12) 0.658950(14) 0.238587(12) 0.02035(8) Uani 1 1 d . . . Nb2 Nb 0.211368(13) 0.031941(15) 0.230339(13) 0.02301(8) Uani 1 1 d . . . Cl1 Cl 0.81379(4) 0.71995(5) 0.29645(4) 0.0330(2) Uani 1 1 d . . . Cl2 Cl 0.30514(4) -0.02993(5) 0.28351(4) 0.0360(2) Uani 1 1 d . . . N1 N 0.68368(12) 0.66455(14) 0.28831(12) 0.0260(6) Uani 1 1 d . . . N2 N 0.77596(11) 0.55373(14) 0.28517(11) 0.0223(6) Uani 1 1 d . . . N3 N 0.75274(12) 0.69237(14) 0.15454(11) 0.0236(6) Uani 1 1 d . . . N4 N 0.17570(12) 0.02628(14) 0.28102(12) 0.0282(6) Uani 1 1 d . . . N5 N 0.24248(12) 0.00010(14) 0.14316(12) 0.0255(6) Uani 1 1 d . . . N6 N 0.26185(12) 0.14040(13) 0.27151(11) 0.0243(6) Uani 1 1 d . . . O1 O 0.58445(12) 0.61306(13) 0.09994(11) 0.0472(7) Uani 1 1 d . . . O2 O 0.53762(12) 0.50585(14) 0.06048(11) 0.0498(8) Uani 1 1 d . . . O3 O 0.57205(12) 0.73154(16) 0.21426(14) 0.0532(8) Uani 1 1 d . . . O4 O 0.51303(12) 0.82121(15) 0.15428(14) 0.0521(8) Uani 1 1 d . . . O5 O 0.06355(12) -0.03921(15) 0.20590(13) 0.0477(7) Uani 1 1 d . . . O6 O 0.00983(11) -0.13756(15) 0.15490(12) 0.0454(7) Uani 1 1 d . . . O7 O 0.07253(12) 0.06588(14) 0.08911(12) 0.0477(7) Uani 1 1 d . . . O8 O 0.01761(12) 0.16802(15) 0.04786(12) 0.0509(8) Uani 1 1 d . . . O9 O 0.03884(16) 0.41838(17) 0.07546(16) 0.0708(10) Uani 1 1 d . . . O10 O 0.46162(14) 0.71336(16) -0.03648(14) 0.0577(8) Uani 1 1 d . . . C1 C 0.65224(17) 0.6777(2) 0.32479(16) 0.0368(9) Uani 1 1 d . . . C2 C 0.6626(2) 0.7411(2) 0.3580(2) 0.0518(11) Uani 1 1 d . . . C3 C 0.6316(3) 0.7528(3) 0.3948(2) 0.0730(16) Uani 1 1 d . . . H3A H 0.6386 0.7948 0.4171 0.088 Uiso 1 1 calc R . . C4 C 0.5918(3) 0.7048(4) 0.3989(3) 0.0881(19) Uani 1 1 d . . . H4A H 0.5718 0.7136 0.4239 0.106 Uiso 1 1 calc R . . C5 C 0.5807(2) 0.6420(4) 0.3655(2) 0.0763(17) Uani 1 1 d . . . H5A H 0.5529 0.6091 0.3685 0.092 Uiso 1 1 calc R . . C6 C 0.61015(18) 0.6269(2) 0.32769(19) 0.0493(11) Uani 1 1 d . . . C7 C 0.7061(3) 0.7960(2) 0.3536(2) 0.0691(15) Uani 1 1 d . . . H7A H 0.7231 0.7795 0.3262 0.104 Uiso 1 1 calc R . . H7B H 0.7383 0.8033 0.3926 0.104 Uiso 1 1 calc R . . H7C H 0.6849 0.8402 0.3392 0.104 Uiso 1 1 calc R . . C8 C 0.5966(2) 0.5611(3) 0.2887(2) 0.0668(14) Uani 1 1 d . . . H8A H 0.5672 0.5322 0.2959 0.100 Uiso 1 1 calc R . . H8B H 0.6333 0.5341 0.2982 0.100 Uiso 1 1 calc R . . H8C H 0.5806 0.5750 0.2472 0.100 Uiso 1 1 calc R . . C9 C 0.67047(14) 0.56197(16) 0.18754(14) 0.0242(7) Uani 1 1 d . . . C10 C 0.61777(15) 0.55700(18) 0.13570(15) 0.0294(8) Uani 1 1 d . . . C11 C 0.58886(16) 0.4933(2) 0.11090(15) 0.0350(9) Uani 1 1 d . . . C12 C 0.61030(17) 0.42799(19) 0.13600(16) 0.0376(9) Uani 1 1 d . . . H12A H 0.5905 0.3856 0.1192 0.045 Uiso 1 1 calc R . . C13 C 0.66338(16) 0.42884(18) 0.18806(16) 0.0338(8) Uani 1 1 d . . . H13A H 0.6797 0.3859 0.2070 0.041 Uiso 1 1 calc R . . C14 C 0.69291(15) 0.49326(17) 0.21263(14) 0.0260(7) Uani 1 1 d . . . C15 C 0.54007(19) 0.5802(2) 0.04856(18) 0.0531(12) Uani 1 1 d . . . H15A H 0.5506 0.5865 0.0143 0.064 Uiso 1 1 calc R . . H15B H 0.5006 0.6020 0.0392 0.064 Uiso 1 1 calc R . . C16 C 0.74943(14) 0.49261(17) 0.26590(14) 0.0249(7) Uani 1 1 d . . . C17 C 0.77401(16) 0.42205(18) 0.29645(16) 0.0365(9) Uani 1 1 d . . . H17A H 0.8115 0.4301 0.3308 0.055 Uiso 1 1 calc R . . H17B H 0.7813 0.3907 0.2688 0.055 Uiso 1 1 calc R . . H17C H 0.7449 0.4006 0.3092 0.055 Uiso 1 1 calc R . . C18 C 0.83251(14) 0.55303(17) 0.33898(15) 0.0272(7) Uani 1 1 d . . . C19 C 0.88766(16) 0.54809(18) 0.33301(17) 0.0355(9) Uani 1 1 d . . . C20 C 0.94059(17) 0.5465(2) 0.3855(2) 0.0493(11) Uani 1 1 d . . . H20A H 0.9779 0.5429 0.3826 0.059 Uiso 1 1 calc R . . C21 C 0.9396(2) 0.5499(2) 0.4411(2) 0.0540(13) Uani 1 1 d . . . H21A H 0.9758 0.5490 0.4753 0.065 Uiso 1 1 calc R . . C22 C 0.88523(19) 0.5547(2) 0.44636(17) 0.0450(10) Uani 1 1 d . . . H22A H 0.8848 0.5566 0.4844 0.054 Uiso 1 1 calc R . . C23 C 0.83022(17) 0.55694(18) 0.39569(15) 0.0344(9) Uani 1 1 d . . . C24 C 0.89132(17) 0.5418(2) 0.27240(19) 0.0446(10) Uani 1 1 d . . . H24A H 0.8525 0.5580 0.2415 0.053 Uiso 1 1 calc R . . C25 C 0.9016(3) 0.4643(3) 0.2587(2) 0.0705(15) Uani 1 1 d . . . H25A H 0.8699 0.4347 0.2608 0.106 Uiso 1 1 calc R . . H25B H 0.9403 0.4481 0.2875 0.106 Uiso 1 1 calc R . . H25C H 0.9010 0.4615 0.2190 0.106 Uiso 1 1 calc R . . C26 C 0.9420(2) 0.5876(3) 0.2680(3) 0.0809(18) Uani 1 1 d . . . H26A H 0.9359 0.6367 0.2758 0.121 Uiso 1 1 calc R . . H26B H 0.9414 0.5834 0.2284 0.121 Uiso 1 1 calc R . . H26C H 0.9806 0.5716 0.2971 0.121 Uiso 1 1 calc R . . C27 C 0.77134(18) 0.5625(2) 0.40451(15) 0.0375(9) Uani 1 1 d . . . H27A H 0.7380 0.5688 0.3648 0.045 Uiso 1 1 calc R . . C28 C 0.7715(2) 0.6270(2) 0.44280(18) 0.0528(11) Uani 1 1 d . . . H28A H 0.7793 0.6696 0.4250 0.079 Uiso 1 1 calc R . . H28B H 0.8027 0.6211 0.4825 0.079 Uiso 1 1 calc R . . H28C H 0.7326 0.6309 0.4451 0.079 Uiso 1 1 calc R . . C29 C 0.7587(2) 0.4937(2) 0.43249(19) 0.0583(13) Uani 1 1 d . . . H29A H 0.7581 0.4535 0.4078 0.087 Uiso 1 1 calc R . . H29B H 0.7199 0.4978 0.4351 0.087 Uiso 1 1 calc R . . H29C H 0.7900 0.4872 0.4720 0.087 Uiso 1 1 calc R . . C30 C 0.65139(15) 0.72989(17) 0.17398(15) 0.0268(7) Uani 1 1 d . . . C31 C 0.59866(15) 0.75489(18) 0.17683(16) 0.0319(8) Uani 1 1 d . . . C32 C 0.56112(15) 0.8077(2) 0.13965(18) 0.0377(9) Uani 1 1 d . . . C33 C 0.57315(17) 0.8386(2) 0.09442(17) 0.0406(9) Uani 1 1 d . . . H33A H 0.5485 0.8741 0.0698 0.049 Uiso 1 1 calc R . . C34 C 0.62449(16) 0.81340(19) 0.08745(16) 0.0357(9) Uani 1 1 d . . . H34A H 0.6339 0.8320 0.0567 0.043 Uiso 1 1 calc R . . C35 C 0.66231(14) 0.76123(16) 0.12515(14) 0.0246(7) Uani 1 1 d . . . C36 C 0.5254(2) 0.7808(3) 0.2083(3) 0.0677(15) Uani 1 1 d . . . H36A H 0.5383 0.8124 0.2428 0.081 Uiso 1 1 calc R . . H36B H 0.4891 0.7556 0.2057 0.081 Uiso 1 1 calc R . . C37 C 0.71515(15) 0.73559(17) 0.11541(14) 0.0266(7) Uani 1 1 d . . . C38 C 0.72262(17) 0.7598(2) 0.05968(15) 0.0373(9) Uani 1 1 d . . . H38A H 0.7590 0.7392 0.0590 0.056 Uiso 1 1 calc R . . H38B H 0.7256 0.8110 0.0597 0.056 Uiso 1 1 calc R . . H38C H 0.6881 0.7446 0.0247 0.056 Uiso 1 1 calc R . . C39 C 0.80577(15) 0.67109(18) 0.14406(15) 0.0279(7) Uani 1 1 d . . . C40 C 0.85598(16) 0.71742(19) 0.15873(16) 0.0315(8) Uani 1 1 d . . . C41 C 0.90214(18) 0.6970(2) 0.14092(18) 0.0434(10) Uani 1 1 d . . . H41A H 0.9357 0.7269 0.1499 0.052 Uiso 1 1 calc R . . C42 C 0.89973(19) 0.6345(2) 0.1107(2) 0.0503(11) Uani 1 1 d . . . H42A H 0.9306 0.6231 0.0984 0.060 Uiso 1 1 calc R . . C43 C 0.85109(19) 0.5886(2) 0.09850(19) 0.0488(11) Uani 1 1 d . . . H43A H 0.8505 0.5453 0.0794 0.059 Uiso 1 1 calc R . . C44 C 0.80296(16) 0.60563(19) 0.11426(16) 0.0335(8) Uani 1 1 d . . . C45 C 0.86140(16) 0.78861(19) 0.19067(17) 0.0349(8) Uani 1 1 d . . . H45A H 0.8264 0.7935 0.2014 0.042 Uiso 1 1 calc R . . C46 C 0.86018(18) 0.8512(2) 0.1493(2) 0.0488(11) Uani 1 1 d . . . H46A H 0.8236 0.8489 0.1132 0.073 Uiso 1 1 calc R . . H46B H 0.8950 0.8484 0.1394 0.073 Uiso 1 1 calc R . . H46C H 0.8612 0.8956 0.1696 0.073 Uiso 1 1 calc R . . C47 C 0.91921(17) 0.7932(2) 0.24815(18) 0.0472(10) Uani 1 1 d . . . H47A H 0.9201 0.7543 0.2743 0.071 Uiso 1 1 calc R . . H47B H 0.9199 0.8378 0.2680 0.071 Uiso 1 1 calc R . . H47C H 0.9541 0.7903 0.2384 0.071 Uiso 1 1 calc R . . C48 C 0.74832(19) 0.5576(2) 0.09599(19) 0.0457(10) Uani 1 1 d . . . H48A H 0.7264 0.5702 0.1210 0.055 Uiso 1 1 calc R . . C49 C 0.7048(2) 0.5692(3) 0.0307(2) 0.0786(17) Uani 1 1 d . . . H49A H 0.6943 0.6189 0.0242 0.118 Uiso 1 1 calc R . . H49B H 0.6685 0.5414 0.0220 0.118 Uiso 1 1 calc R . . H49C H 0.7240 0.5544 0.0048 0.118 Uiso 1 1 calc R . . C50 C 0.7644(2) 0.4784(2) 0.1062(2) 0.0591(12) Uani 1 1 d . . . H50A H 0.7914 0.4709 0.1475 0.089 Uiso 1 1 calc R . . H50B H 0.7841 0.4636 0.0806 0.089 Uiso 1 1 calc R . . H50C H 0.7280 0.4510 0.0970 0.089 Uiso 1 1 calc R . . C51 C 0.14227(16) 0.01250(19) 0.31547(15) 0.0315(8) Uani 1 1 d . . . C52 C 0.09789(18) 0.0612(2) 0.31540(18) 0.0436(10) Uani 1 1 d . . . C53 C 0.0646(2) 0.0438(3) 0.3490(2) 0.0617(13) Uani 1 1 d . . . H53A H 0.0356 0.0759 0.3503 0.074 Uiso 1 1 calc R . . C54 C 0.0734(2) -0.0191(3) 0.3800(2) 0.0681(15) Uani 1 1 d . . . H54A H 0.0499 -0.0299 0.4014 0.082 Uiso 1 1 calc R . . C55 C 0.1171(2) -0.0663(3) 0.3794(2) 0.0599(13) Uani 1 1 d . . . H55A H 0.1230 -0.1088 0.4008 0.072 Uiso 1 1 calc R . . C56 C 0.15213(18) -0.0520(2) 0.34782(17) 0.0409(9) Uani 1 1 d . . . C57 C 0.0855(2) 0.1282(2) 0.2792(2) 0.0573(12) Uani 1 1 d . . . H57A H 0.1130 0.1314 0.2596 0.086 Uiso 1 1 calc R . . H57B H 0.0911 0.1687 0.3051 0.086 Uiso 1 1 calc R . . H57C H 0.0443 0.1275 0.2495 0.086 Uiso 1 1 calc R . . C58 C 0.1996(2) -0.1040(2) 0.3467(2) 0.0587(12) Uani 1 1 d . . . H58A H 0.2195 -0.0847 0.3227 0.088 Uiso 1 1 calc R . . H58B H 0.1806 -0.1486 0.3298 0.088 Uiso 1 1 calc R . . H58C H 0.2292 -0.1118 0.3870 0.088 Uiso 1 1 calc R . . C59 C 0.14430(14) -0.04163(17) 0.16768(14) 0.0267(7) Uani 1 1 d . . . C60 C 0.09249(15) -0.06692(18) 0.17171(15) 0.0306(8) Uani 1 1 d . . . C61 C 0.05794(15) -0.12464(19) 0.13921(16) 0.0325(8) Uani 1 1 d . . . C62 C 0.07119(16) -0.15909(19) 0.09687(16) 0.0344(8) Uani 1 1 d . . . H62A H 0.0484 -0.1977 0.0752 0.041 Uiso 1 1 calc R . . C63 C 0.12152(15) -0.13260(18) 0.08788(15) 0.0311(8) Uani 1 1 d . . . H63A H 0.1319 -0.1536 0.0586 0.037 Uiso 1 1 calc R . . C64 C 0.15635(14) -0.07610(17) 0.12128(14) 0.0252(7) Uani 1 1 d . . . C65 C 0.02159(19) -0.0922(2) 0.2065(2) 0.0567(12) Uani 1 1 d . . . H65A H -0.0159 -0.0700 0.2041 0.068 Uiso 1 1 calc R . . H65B H 0.0386 -0.1200 0.2432 0.068 Uiso 1 1 calc R . . C66 C 0.20670(15) -0.04796(17) 0.10777(14) 0.0263(7) Uani 1 1 d . . . C67 C 0.21218(16) -0.0750(2) 0.05207(15) 0.0371(9) Uani 1 1 d . . . H67A H 0.2465 -0.0529 0.0482 0.056 Uiso 1 1 calc R . . H67B H 0.1758 -0.0636 0.0175 0.056 Uiso 1 1 calc R . . H67C H 0.2178 -0.1260 0.0548 0.056 Uiso 1 1 calc R . . C68 C 0.29193(15) 0.02497(18) 0.12829(14) 0.0283(7) Uani 1 1 d . . . C69 C 0.28618(16) 0.09189(19) 0.10033(15) 0.0328(8) Uani 1 1 d . . . C70 C 0.33195(18) 0.1149(2) 0.08340(16) 0.0399(9) Uani 1 1 d . . . H70A H 0.3287 0.1595 0.0653 0.048 Uiso 1 1 calc R . . C71 C 0.38223(18) 0.0728(2) 0.09289(17) 0.0426(10) Uani 1 1 d . . . H71A H 0.4122 0.0884 0.0807 0.051 Uiso 1 1 calc R . . C72 C 0.38746(17) 0.0075(2) 0.12066(17) 0.0420(9) Uani 1 1 d . . . H72A H 0.4215 -0.0205 0.1270 0.050 Uiso 1 1 calc R . . C73 C 0.34360(16) -0.01838(19) 0.13978(16) 0.0332(8) Uani 1 1 d . . . C74 C 0.22918(19) 0.1365(2) 0.08551(18) 0.0418(9) Uani 1 1 d . . . H74A H 0.2121 0.1232 0.1145 0.050 Uiso 1 1 calc R . . C75 C 0.1814(2) 0.1188(3) 0.0235(2) 0.0602(13) Uani 1 1 d . . . H75A H 0.1744 0.0681 0.0203 0.090 Uiso 1 1 calc R . . H75B H 0.1953 0.1341 -0.0065 0.090 Uiso 1 1 calc R . . H75C H 0.1441 0.1430 0.0175 0.090 Uiso 1 1 calc R . . C76 C 0.2411(2) 0.2173(2) 0.0921(2) 0.0646(14) Uani 1 1 d . . . H76A H 0.2711 0.2275 0.1317 0.097 Uiso 1 1 calc R . . H76B H 0.2040 0.2419 0.0861 0.097 Uiso 1 1 calc R . . H76C H 0.2556 0.2331 0.0627 0.097 Uiso 1 1 calc R . . C77 C 0.35359(17) -0.0917(2) 0.16967(17) 0.0390(9) Uani 1 1 d . . . H77A H 0.3180 -0.1031 0.1783 0.047 Uiso 1 1 calc R . . C78 C 0.35988(19) -0.1501(2) 0.1281(2) 0.0520(11) Uani 1 1 d . . . H78A H 0.3243 -0.1502 0.0910 0.078 Uiso 1 1 calc R . . H78B H 0.3641 -0.1959 0.1472 0.078 Uiso 1 1 calc R . . H78C H 0.3952 -0.1406 0.1200 0.078 Uiso 1 1 calc R . . C79 C 0.41014(17) -0.0932(2) 0.22899(19) 0.0516(11) Uani 1 1 d . . . H79A H 0.4065 -0.0572 0.2555 0.077 Uiso 1 1 calc R . . H79B H 0.4457 -0.0839 0.2213 0.077 Uiso 1 1 calc R . . H79C H 0.4137 -0.1394 0.2474 0.077 Uiso 1 1 calc R . . C80 C 0.15525(15) 0.12351(18) 0.17610(15) 0.0273(7) Uani 1 1 d . . . C81 C 0.10183(16) 0.12417(19) 0.12460(16) 0.0327(8) Uani 1 1 d . . . C82 C 0.06837(17) 0.1848(2) 0.09920(16) 0.0383(9) Uani 1 1 d . . . C83 C 0.08461(18) 0.2515(2) 0.12314(18) 0.0430(10) Uani 1 1 d . . . H83A H 0.0611 0.2918 0.1065 0.052 Uiso 1 1 calc R . . C84 C 0.13899(18) 0.2550(2) 0.17449(17) 0.0396(9) Uani 1 1 d . . . H84A H 0.1529 0.2991 0.1923 0.048 Uiso 1 1 calc R . . C85 C 0.17270(15) 0.19381(18) 0.19949(15) 0.0293(8) Uani 1 1 d . . . C86 C 0.0219(2) 0.0929(2) 0.04049(19) 0.0559(12) Uani 1 1 d . . . H86A H -0.0149 0.0696 0.0387 0.067 Uiso 1 1 calc R . . H86B H 0.0262 0.0834 0.0032 0.067 Uiso 1 1 calc R . . C87 C 0.23049(16) 0.19914(18) 0.25260(15) 0.0299(8) Uani 1 1 d . . . C88 C 0.25199(19) 0.27162(19) 0.28053(18) 0.0427(10) Uani 1 1 d . . . H88A H 0.2902 0.2666 0.3146 0.064 Uiso 1 1 calc R . . H88B H 0.2224 0.2917 0.2934 0.064 Uiso 1 1 calc R . . H88C H 0.2571 0.3027 0.2514 0.064 Uiso 1 1 calc R . . C89 C 0.31716(15) 0.14360(17) 0.32657(15) 0.0284(7) Uani 1 1 d . . . C90 C 0.31630(17) 0.14065(18) 0.38397(15) 0.0331(8) Uani 1 1 d . . . C91 C 0.37173(19) 0.14536(19) 0.43373(17) 0.0418(10) Uani 1 1 d . . . H91A H 0.3719 0.1439 0.4720 0.050 Uiso 1 1 calc R . . C92 C 0.42590(18) 0.1521(2) 0.42796(18) 0.0434(10) Uani 1 1 d . . . H92A H 0.4623 0.1551 0.4618 0.052 Uiso 1 1 calc R . . C93 C 0.42564(17) 0.1545(2) 0.37122(17) 0.0397(9) Uani 1 1 d . . . H93A H 0.4624 0.1590 0.3673 0.048 Uiso 1 1 calc R . . C94 C 0.37169(16) 0.15012(18) 0.31941(16) 0.0327(8) Uani 1 1 d . . . C95 C 0.25880(18) 0.1351(2) 0.39470(17) 0.0419(9) Uani 1 1 d . . . H95A H 0.2246 0.1283 0.3557 0.050 Uiso 1 1 calc R . . C96 C 0.2472(2) 0.2034(3) 0.4231(2) 0.0647(14) Uani 1 1 d . . . H96A H 0.2458 0.2436 0.3979 0.097 Uiso 1 1 calc R . . H96B H 0.2795 0.2101 0.4621 0.097 Uiso 1 1 calc R . . H96C H 0.2092 0.1993 0.4271 0.097 Uiso 1 1 calc R . . C97 C 0.2607(2) 0.0707(2) 0.43448(18) 0.0571(12) Uani 1 1 d . . . H97A H 0.2680 0.0278 0.4166 0.086 Uiso 1 1 calc R . . H97B H 0.2224 0.0667 0.4381 0.086 Uiso 1 1 calc R . . H97C H 0.2928 0.0772 0.4736 0.086 Uiso 1 1 calc R . . C98 C 0.37414(16) 0.1553(2) 0.25844(17) 0.0372(9) Uani 1 1 d . . . H98A H 0.3351 0.1392 0.2279 0.045 Uiso 1 1 calc R . . C99 C 0.4241(2) 0.1094(3) 0.2545(2) 0.0606(13) Uani 1 1 d . . . H99A H 0.4179 0.0605 0.2627 0.091 Uiso 1 1 calc R . . H99B H 0.4628 0.1256 0.2834 0.091 Uiso 1 1 calc R . . H99C H 0.4234 0.1129 0.2148 0.091 Uiso 1 1 calc R . . C100 C 0.3848(3) 0.2323(2) 0.2449(2) 0.0756(16) Uani 1 1 d . . . H10A H 0.3530 0.2621 0.2468 0.113 Uiso 1 1 calc R . . H10B H 0.3846 0.2350 0.2054 0.113 Uiso 1 1 calc R . . H10C H 0.4234 0.2484 0.2740 0.113 Uiso 1 1 calc R . . C101 C 0.0100(4) 0.4632(3) 0.1014(3) 0.105(3) Uani 1 1 d . . . H10K H -0.0086 0.5030 0.0747 0.126 Uiso 1 1 calc R . . H10L H 0.0395 0.4821 0.1390 0.126 Uiso 1 1 calc R . . C102 C -0.0364(3) 0.4228(4) 0.1123(3) 0.107(2) Uani 1 1 d . . . H10O H -0.0566 0.4536 0.1300 0.161 Uiso 1 1 calc R . . H10P H -0.0177 0.3838 0.1391 0.161 Uiso 1 1 calc R . . H10Q H -0.0656 0.4043 0.0749 0.161 Uiso 1 1 calc R . . C103 C 0.0839(3) 0.4540(4) 0.0621(3) 0.106(3) Uani 1 1 d . . . H10M H 0.1110 0.4800 0.0973 0.127 Uiso 1 1 calc R . . H10N H 0.0648 0.4880 0.0299 0.127 Uiso 1 1 calc R . . C104 C 0.1182(3) 0.4024(5) 0.0444(3) 0.128(3) Uani 1 1 d . . . H10R H 0.1486 0.4267 0.0352 0.192 Uiso 1 1 calc R . . H10S H 0.0913 0.3769 0.0095 0.192 Uiso 1 1 calc R . . H10T H 0.1376 0.3693 0.0767 0.192 Uiso 1 1 calc R . . C105 C 0.4136(3) 0.7455(3) -0.0261(3) 0.0807(17) Uani 1 1 d . . . H10I H 0.3812 0.7585 -0.0642 0.097 Uiso 1 1 calc R . . H10J H 0.4281 0.7888 -0.0026 0.097 Uiso 1 1 calc R . . C106 C 0.3903(4) 0.6953(4) 0.0064(4) 0.152(4) Uani 1 1 d . . . H10U H 0.3575 0.7174 0.0132 0.228 Uiso 1 1 calc R . . H10V H 0.4224 0.6830 0.0442 0.228 Uiso 1 1 calc R . . H10W H 0.3757 0.6527 -0.0172 0.228 Uiso 1 1 calc R . . C107 C 0.4863(2) 0.7589(2) -0.0673(2) 0.0621(13) Uani 1 1 d . . . H10D H 0.5017 0.8021 -0.0440 0.075 Uiso 1 1 calc R . . H10E H 0.4547 0.7724 -0.1057 0.075 Uiso 1 1 calc R . . C108 C 0.5363(2) 0.7224(3) -0.0770(3) 0.0794(16) Uani 1 1 d . . . H10F H 0.5526 0.7538 -0.0981 0.119 Uiso 1 1 calc R . . H10G H 0.5209 0.6798 -0.1004 0.119 Uiso 1 1 calc R . . H10H H 0.5678 0.7097 -0.0389 0.119 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 0.02116(14) 0.01666(14) 0.02167(14) 0.00152(11) 0.00702(11) -0.00037(11) Nb2 0.02481(16) 0.02002(15) 0.02474(15) -0.00078(12) 0.01056(12) -0.00043(12) Cl1 0.0301(4) 0.0325(5) 0.0297(4) -0.0002(4) 0.0051(4) -0.0102(4) Cl2 0.0325(5) 0.0390(5) 0.0320(4) 0.0011(4) 0.0082(4) 0.0085(4) N1 0.0295(15) 0.0223(14) 0.0287(14) 0.0030(12) 0.0144(12) 0.0001(12) N2 0.0227(14) 0.0230(14) 0.0197(13) 0.0012(11) 0.0070(11) 0.0016(11) N3 0.0260(14) 0.0212(14) 0.0234(14) 0.0008(11) 0.0096(12) -0.0008(11) N4 0.0313(15) 0.0267(15) 0.0279(14) -0.0033(12) 0.0133(12) -0.0015(12) N5 0.0264(15) 0.0246(14) 0.0261(14) 0.0037(12) 0.0113(12) 0.0011(12) N6 0.0250(14) 0.0109(12) 0.0232(13) -0.0031(10) -0.0046(11) 0.0007(10) O1 0.0436(16) 0.0282(14) 0.0392(15) 0.0041(11) -0.0152(12) -0.0006(12) O2 0.0495(17) 0.0367(15) 0.0349(15) 0.0009(12) -0.0124(13) -0.0145(13) O3 0.0371(16) 0.0622(19) 0.071(2) 0.0258(16) 0.0327(15) 0.0198(14) O4 0.0309(15) 0.0509(17) 0.069(2) 0.0077(15) 0.0147(14) 0.0183(13) O5 0.0386(15) 0.0536(17) 0.0629(18) -0.0196(15) 0.0330(14) -0.0174(13) O6 0.0321(14) 0.0502(17) 0.0558(17) -0.0119(14) 0.0199(13) -0.0134(12) O7 0.0429(16) 0.0372(15) 0.0403(15) -0.0031(12) -0.0068(12) 0.0044(12) O8 0.0434(16) 0.0458(17) 0.0438(16) 0.0004(13) -0.0030(13) 0.0110(13) O9 0.075(2) 0.0442(19) 0.074(2) 0.0015(17) 0.0100(19) -0.0063(18) O10 0.057(2) 0.0459(18) 0.065(2) -0.0009(16) 0.0188(16) 0.0116(15) C1 0.036(2) 0.044(2) 0.0324(19) 0.0058(17) 0.0167(17) 0.0091(17) C2 0.066(3) 0.049(3) 0.050(3) -0.002(2) 0.033(2) 0.010(2) C3 0.080(4) 0.088(4) 0.068(3) -0.010(3) 0.048(3) 0.018(3) C4 0.082(4) 0.131(6) 0.079(4) -0.006(4) 0.061(4) 0.015(4) C5 0.059(3) 0.113(5) 0.079(4) 0.017(4) 0.051(3) 0.000(3) C6 0.037(2) 0.063(3) 0.054(3) 0.010(2) 0.024(2) -0.003(2) C7 0.106(4) 0.039(3) 0.077(3) -0.024(2) 0.053(3) -0.006(3) C8 0.045(3) 0.067(3) 0.096(4) 0.004(3) 0.036(3) -0.022(2) C9 0.0269(17) 0.0191(16) 0.0246(16) 0.0008(13) 0.0082(14) -0.0022(13) C10 0.0296(18) 0.0254(17) 0.0271(17) 0.0009(14) 0.0052(15) -0.0010(14) C11 0.035(2) 0.036(2) 0.0243(17) -0.0008(15) 0.0028(15) -0.0087(16) C12 0.045(2) 0.0237(18) 0.0337(19) -0.0007(15) 0.0049(17) -0.0099(16) C13 0.039(2) 0.0202(17) 0.0350(19) 0.0005(15) 0.0077(16) -0.0029(15) C14 0.0304(18) 0.0202(16) 0.0261(17) -0.0022(13) 0.0101(14) -0.0041(14) C15 0.053(3) 0.035(2) 0.038(2) 0.0018(18) -0.0165(19) -0.0055(19) C16 0.0264(17) 0.0202(16) 0.0277(17) 0.0016(13) 0.0103(14) 0.0012(13) C17 0.036(2) 0.0251(18) 0.037(2) 0.0051(15) 0.0035(17) 0.0031(15) C18 0.0224(17) 0.0186(16) 0.0309(18) 0.0064(14) 0.0006(14) -0.0005(13) C19 0.0289(19) 0.0223(17) 0.046(2) 0.0101(16) 0.0051(17) 0.0005(14) C20 0.027(2) 0.034(2) 0.069(3) 0.013(2) 0.001(2) 0.0031(16) C21 0.044(3) 0.034(2) 0.050(3) 0.008(2) -0.017(2) 0.0035(19) C22 0.053(3) 0.034(2) 0.0290(19) 0.0045(16) -0.0028(18) 0.0003(19) C23 0.044(2) 0.0231(17) 0.0257(17) 0.0043(14) 0.0027(16) -0.0060(16) C24 0.027(2) 0.053(3) 0.055(3) 0.019(2) 0.0175(18) 0.0110(18) C25 0.095(4) 0.064(3) 0.069(3) 0.007(3) 0.051(3) 0.014(3) C26 0.048(3) 0.094(4) 0.105(4) 0.051(4) 0.035(3) 0.010(3) C27 0.050(2) 0.039(2) 0.0210(17) 0.0052(15) 0.0111(16) -0.0057(18) C28 0.066(3) 0.053(3) 0.039(2) 0.000(2) 0.022(2) -0.001(2) C29 0.083(3) 0.049(3) 0.046(3) 0.006(2) 0.029(2) -0.015(2) C30 0.0256(17) 0.0210(16) 0.0315(18) -0.0002(14) 0.0090(15) 0.0005(13) C31 0.0266(18) 0.0288(18) 0.039(2) 0.0057(16) 0.0120(16) 0.0013(15) C32 0.0211(18) 0.031(2) 0.053(2) -0.0006(18) 0.0067(17) 0.0042(15) C33 0.033(2) 0.032(2) 0.043(2) 0.0061(18) 0.0008(17) 0.0086(17) C34 0.035(2) 0.0318(19) 0.0315(19) 0.0076(16) 0.0044(16) 0.0023(16) C35 0.0248(17) 0.0207(16) 0.0223(16) -0.0018(13) 0.0034(14) -0.0037(13) C36 0.046(3) 0.064(3) 0.110(4) 0.031(3) 0.049(3) 0.024(2) C37 0.0317(18) 0.0232(17) 0.0219(16) 0.0000(13) 0.0077(14) -0.0042(14) C38 0.039(2) 0.042(2) 0.0280(18) 0.0110(16) 0.0108(17) 0.0009(17) C39 0.0280(18) 0.0298(18) 0.0280(17) 0.0049(14) 0.0134(15) 0.0042(14) C40 0.0305(19) 0.0314(19) 0.0347(19) 0.0070(15) 0.0153(16) 0.0018(15) C41 0.039(2) 0.047(2) 0.052(2) 0.001(2) 0.027(2) -0.0026(18) C42 0.045(2) 0.056(3) 0.063(3) -0.006(2) 0.035(2) 0.007(2) C43 0.055(3) 0.043(2) 0.060(3) -0.011(2) 0.036(2) 0.002(2) C44 0.038(2) 0.0324(19) 0.0357(19) -0.0018(16) 0.0208(17) -0.0009(16) C45 0.0300(19) 0.033(2) 0.047(2) 0.0003(17) 0.0211(17) -0.0045(15) C46 0.041(2) 0.035(2) 0.067(3) 0.006(2) 0.018(2) -0.0049(18) C47 0.036(2) 0.053(3) 0.053(3) -0.004(2) 0.020(2) -0.0078(19) C48 0.055(3) 0.035(2) 0.056(3) -0.0188(19) 0.032(2) -0.0061(19) C49 0.072(4) 0.049(3) 0.088(4) -0.015(3) 0.005(3) -0.011(3) C50 0.078(3) 0.041(3) 0.064(3) -0.008(2) 0.034(3) -0.010(2) C51 0.037(2) 0.0336(19) 0.0295(18) -0.0060(15) 0.0191(16) -0.0088(16) C52 0.045(2) 0.053(3) 0.042(2) -0.0052(19) 0.0255(19) -0.004(2) C53 0.053(3) 0.088(4) 0.055(3) -0.005(3) 0.033(2) 0.002(3) C54 0.064(3) 0.099(4) 0.059(3) 0.003(3) 0.043(3) -0.020(3) C55 0.069(3) 0.065(3) 0.053(3) 0.006(2) 0.032(3) -0.018(3) C56 0.050(2) 0.039(2) 0.037(2) 0.0016(17) 0.0212(19) -0.0090(19) C57 0.055(3) 0.059(3) 0.069(3) 0.006(2) 0.038(3) 0.020(2) C58 0.087(4) 0.031(2) 0.068(3) 0.014(2) 0.042(3) 0.005(2) C59 0.0255(17) 0.0247(17) 0.0283(17) 0.0001(14) 0.0093(14) -0.0001(13) C60 0.0283(18) 0.0318(19) 0.0324(18) -0.0030(15) 0.0129(15) -0.0022(15) C61 0.0238(18) 0.0310(19) 0.038(2) 0.0024(16) 0.0077(16) -0.0029(15) C62 0.036(2) 0.0270(18) 0.0334(19) -0.0018(16) 0.0063(16) -0.0055(16) C63 0.0328(19) 0.0288(18) 0.0293(18) -0.0029(15) 0.0101(15) 0.0004(15) C64 0.0252(17) 0.0225(16) 0.0238(16) 0.0031(13) 0.0057(14) 0.0014(13) C65 0.046(3) 0.056(3) 0.083(3) -0.022(3) 0.041(3) -0.020(2) C66 0.0307(18) 0.0254(17) 0.0226(16) 0.0027(13) 0.0103(14) 0.0048(14) C67 0.036(2) 0.043(2) 0.0322(19) -0.0068(17) 0.0140(17) -0.0033(17) C68 0.0308(18) 0.0300(18) 0.0251(17) -0.0044(14) 0.0123(15) -0.0048(15) C69 0.043(2) 0.0281(18) 0.0307(18) -0.0006(15) 0.0184(17) -0.0037(16) C70 0.049(2) 0.038(2) 0.036(2) 0.0038(17) 0.0208(19) -0.0074(18) C71 0.040(2) 0.057(3) 0.038(2) 0.0022(19) 0.0227(18) -0.013(2) C72 0.030(2) 0.055(3) 0.044(2) -0.003(2) 0.0188(18) -0.0050(18) C73 0.0316(19) 0.036(2) 0.0331(19) -0.0015(16) 0.0139(16) -0.0037(16) C74 0.055(3) 0.039(2) 0.044(2) 0.0103(18) 0.033(2) 0.0081(19) C75 0.053(3) 0.059(3) 0.062(3) 0.008(2) 0.017(2) 0.017(2) C76 0.099(4) 0.034(2) 0.082(3) 0.010(2) 0.057(3) 0.007(2) C77 0.033(2) 0.040(2) 0.049(2) 0.0061(18) 0.0219(18) 0.0030(17) C78 0.045(2) 0.043(2) 0.070(3) 0.000(2) 0.025(2) 0.004(2) C79 0.034(2) 0.065(3) 0.054(3) 0.014(2) 0.015(2) 0.007(2) C80 0.0292(18) 0.0269(17) 0.0308(18) -0.0011(14) 0.0174(15) -0.0010(14) C81 0.034(2) 0.0279(18) 0.0331(19) -0.0004(15) 0.0103(16) 0.0017(15) C82 0.035(2) 0.043(2) 0.034(2) 0.0045(17) 0.0110(17) 0.0077(17) C83 0.042(2) 0.035(2) 0.047(2) 0.0064(18) 0.0127(19) 0.0125(18) C84 0.049(2) 0.0264(19) 0.045(2) 0.0018(17) 0.020(2) 0.0064(17) C85 0.0319(19) 0.0241(17) 0.0337(19) 0.0026(15) 0.0150(16) 0.0023(14) C86 0.052(3) 0.049(3) 0.043(2) -0.003(2) -0.006(2) 0.013(2) C87 0.036(2) 0.0267(18) 0.0310(18) -0.0004(14) 0.0174(16) -0.0041(15) C88 0.049(2) 0.0230(18) 0.052(2) -0.0020(17) 0.016(2) -0.0005(17) C89 0.0312(18) 0.0191(16) 0.0291(18) -0.0040(13) 0.0061(15) -0.0033(14) C90 0.043(2) 0.0265(18) 0.0277(18) -0.0015(14) 0.0117(16) -0.0053(16) C91 0.055(3) 0.030(2) 0.0300(19) -0.0014(16) 0.0059(18) -0.0030(18) C92 0.041(2) 0.037(2) 0.039(2) 0.0004(18) 0.0018(18) -0.0042(18) C93 0.031(2) 0.036(2) 0.043(2) 0.0004(18) 0.0050(17) -0.0020(16) C94 0.0335(19) 0.0248(18) 0.0337(19) -0.0035(15) 0.0072(16) -0.0054(15) C95 0.049(2) 0.046(2) 0.032(2) -0.0070(17) 0.0179(18) -0.0058(19) C96 0.076(4) 0.065(3) 0.068(3) -0.012(3) 0.044(3) -0.001(3) C97 0.064(3) 0.066(3) 0.038(2) 0.008(2) 0.017(2) -0.015(2) C98 0.0297(19) 0.042(2) 0.039(2) -0.0057(17) 0.0123(16) -0.0045(17) C99 0.052(3) 0.078(3) 0.054(3) -0.017(2) 0.024(2) 0.010(2) C100 0.131(5) 0.048(3) 0.064(3) 0.008(2) 0.055(3) 0.000(3) C101 0.143(7) 0.063(4) 0.067(4) 0.001(3) -0.002(4) 0.020(4) C102 0.092(5) 0.127(6) 0.087(5) -0.022(4) 0.019(4) 0.033(5) C103 0.116(6) 0.097(5) 0.057(4) 0.025(3) -0.015(4) -0.051(4) C104 0.123(6) 0.174(9) 0.101(6) -0.001(6) 0.059(5) -0.053(6) C105 0.081(4) 0.087(4) 0.078(4) 0.010(3) 0.036(3) 0.040(3) C106 0.157(8) 0.146(7) 0.222(10) 0.064(7) 0.148(8) 0.056(6) C107 0.075(3) 0.045(3) 0.055(3) 0.000(2) 0.015(3) 0.004(2) C108 0.062(3) 0.072(4) 0.110(5) -0.007(3) 0.040(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N1 1.764(3) . ? Nb1 C30 2.207(3) . ? Nb1 C9 2.250(3) . ? Nb1 N2 2.389(3) . ? Nb1 Cl1 2.3989(8) . ? Nb1 N3 2.538(3) . ? Nb2 N4 1.764(3) . ? Nb2 C59 2.196(3) . ? Nb2 C80 2.247(3) . ? Nb2 N6 2.367(2) . ? Nb2 Cl2 2.3933(9) . ? Nb2 N5 2.584(3) . ? N1 C1 1.399(4) . ? N2 C16 1.300(4) . ? N2 C18 1.456(4) . ? N3 C37 1.296(4) . ? N3 C39 1.451(4) . ? N4 C51 1.397(4) . ? N5 C66 1.299(4) . ? N5 C68 1.450(4) . ? N6 C87 1.305(4) . ? N6 C89 1.457(4) . ? O1 C10 1.390(4) . ? O1 C15 1.414(4) . ? O2 C11 1.362(4) . ? O2 C15 1.425(4) . ? O3 C31 1.377(4) . ? O3 C36 1.411(5) . ? O4 C32 1.361(4) . ? O4 C36 1.439(5) . ? O5 C60 1.381(4) . ? O5 C65 1.417(4) . ? O6 C61 1.376(4) . ? O6 C65 1.444(5) . ? O7 C81 1.392(4) . ? O7 C86 1.404(4) . ? O8 C82 1.383(4) . ? O8 C86 1.423(5) . ? O9 C101 1.388(7) . ? O9 C103 1.415(7) . ? O10 C105 1.409(6) . ? O10 C107 1.411(6) . ? C1 C2 1.398(6) . ? C1 C6 1.409(5) . ? C2 C3 1.393(6) . ? C2 C7 1.497(6) . ? C3 C4 1.343(8) . ? C4 C5 1.390(8) . ? C5 C6 1.397(6) . ? C6 C8 1.506(6) . ? C9 C10 1.382(4) . ? C9 C14 1.431(4) . ? C10 C11 1.388(5) . ? C11 C12 1.368(5) . ? C12 C13 1.387(5) . ? C13 C14 1.402(4) . ? C14 C16 1.449(4) . ? C16 C17 1.512(4) . ? C18 C19 1.392(5) . ? C18 C23 1.403(5) . ? C19 C20 1.391(5) . ? C19 C24 1.515(5) . ? C20 C21 1.361(6) . ? C21 C22 1.365(6) . ? C22 C23 1.397(5) . ? C23 C27 1.516(5) . ? C24 C26 1.526(6) . ? C24 C25 1.528(6) . ? C27 C28 1.522(5) . ? C27 C29 1.540(5) . ? C30 C31 1.377(5) . ? C30 C35 1.439(5) . ? C31 C32 1.396(5) . ? C32 C33 1.371(5) . ? C33 C34 1.392(5) . ? C34 C35 1.394(4) . ? C35 C37 1.462(5) . ? C37 C38 1.506(5) . ? C39 C40 1.408(5) . ? C39 C44 1.409(5) . ? C40 C41 1.395(5) . ? C40 C45 1.519(5) . ? C41 C42 1.369(6) . ? C42 C43 1.382(6) . ? C43 C44 1.393(5) . ? C44 C48 1.501(5) . ? C45 C47 1.523(5) . ? C45 C46 1.535(5) . ? C48 C49 1.523(6) . ? C48 C50 1.524(6) . ? C51 C52 1.400(5) . ? C51 C56 1.406(5) . ? C52 C53 1.392(6) . ? C52 C57 1.490(6) . ? C53 C54 1.365(7) . ? C54 C55 1.374(7) . ? C55 C56 1.375(6) . ? C56 C58 1.507(6) . ? C59 C60 1.370(5) . ? C59 C64 1.426(4) . ? C60 C61 1.395(5) . ? C61 C62 1.356(5) . ? C62 C63 1.402(5) . ? C63 C64 1.388(4) . ? C64 C66 1.471(5) . ? C66 C67 1.500(4) . ? C68 C69 1.403(5) . ? C68 C73 1.412(5) . ? C69 C70 1.388(5) . ? C69 C74 1.516(5) . ? C70 C71 1.380(5) . ? C71 C72 1.376(6) . ? C72 C73 1.397(5) . ? C73 C77 1.524(5) . ? C74 C75 1.517(6) . ? C74 C76 1.534(5) . ? C77 C79 1.531(5) . ? C77 C78 1.535(5) . ? C80 C81 1.384(5) . ? C80 C85 1.426(5) . ? C81 C82 1.383(5) . ? C82 C83 1.364(5) . ? C83 C84 1.397(5) . ? C84 C85 1.391(5) . ? C85 C87 1.468(5) . ? C87 C88 1.510(5) . ? C89 C94 1.394(5) . ? C89 C90 1.404(5) . ? C90 C91 1.394(5) . ? C90 C95 1.508(5) . ? C91 C92 1.369(6) . ? C92 C93 1.377(5) . ? C93 C94 1.398(5) . ? C94 C98 1.510(5) . ? C95 C96 1.529(6) . ? C95 C97 1.533(5) . ? C98 C99 1.510(5) . ? C98 C100 1.520(6) . ? C101 C102 1.456(9) . ? C103 C104 1.441(9) . ? C105 C106 1.476(8) . ? C107 C108 1.480(7) . ? 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 N1 Nb1 C30 90.68(12) . . ? N1 Nb1 C9 97.04(12) . . ? C30 Nb1 C9 90.63(12) . . ? N1 Nb1 N2 93.54(10) . . ? C30 Nb1 N2 161.24(10) . . ? C9 Nb1 N2 70.72(10) . . ? N1 Nb1 Cl1 100.21(9) . . ? C30 Nb1 Cl1 112.80(9) . . ? C9 Nb1 Cl1 150.49(9) . . ? N2 Nb1 Cl1 84.43(6) . . ? N1 Nb1 N3 159.48(10) . . ? C30 Nb1 N3 70.44(11) . . ? C9 Nb1 N3 91.29(10) . . ? N2 Nb1 N3 106.92(9) . . ? Cl1 Nb1 N3 80.72(6) . . ? N4 Nb2 C59 91.15(12) . . ? N4 Nb2 C80 96.34(12) . . ? C59 Nb2 C80 88.38(12) . . ? N4 Nb2 N6 93.79(11) . . ? C59 Nb2 N6 159.48(10) . . ? C80 Nb2 N6 71.29(10) . . ? N4 Nb2 Cl2 102.11(9) . . ? C59 Nb2 Cl2 109.79(9) . . ? C80 Nb2 Cl2 153.58(9) . . ? N6 Nb2 Cl2 88.62(6) . . ? N4 Nb2 N5 160.19(11) . . ? C59 Nb2 N5 70.17(11) . . ? C80 Nb2 N5 89.86(10) . . ? N6 Nb2 N5 106.02(9) . . ? Cl2 Nb2 N5 79.13(6) . . ? C1 N1 Nb1 172.7(2) . . ? C16 N2 C18 117.4(3) . . ? C16 N2 Nb1 117.0(2) . . ? C18 N2 Nb1 124.94(19) . . ? C37 N3 C39 116.3(3) . . ? C37 N3 Nb1 113.3(2) . . ? C39 N3 Nb1 130.41(19) . . ? C51 N4 Nb2 170.7(2) . . ? C66 N5 C68 116.5(3) . . ? C66 N5 Nb2 111.7(2) . . ? C68 N5 Nb2 131.8(2) . . ? C87 N6 C89 118.1(3) . . ? C87 N6 Nb2 116.6(2) . . ? C89 N6 Nb2 123.02(18) . . ? C10 O1 C15 105.3(3) . . ? C11 O2 C15 104.8(3) . . ? C31 O3 C36 106.6(3) . . ? C32 O4 C36 104.9(3) . . ? C60 O5 C65 106.0(3) . . ? C61 O6 C65 104.2(3) . . ? C81 O7 C86 106.8(3) . . ? C82 O8 C86 104.8(3) . . ? C101 O9 C103 112.8(5) . . ? C105 O10 C107 112.7(4) . . ? C2 C1 N1 119.9(4) . . ? C2 C1 C6 120.5(4) . . ? N1 C1 C6 119.6(4) . . ? C3 C2 C1 119.1(5) . . ? C3 C2 C7 120.5(4) . . ? C1 C2 C7 120.4(4) . . ? C4 C3 C2 121.6(5) . . ? C3 C4 C5 119.7(5) . . ? C4 C5 C6 121.6(5) . . ? C5 C6 C1 117.5(5) . . ? C5 C6 C8 122.7(4) . . ? C1 C6 C8 119.8(4) . . ? C10 C9 C14 112.2(3) . . ? C10 C9 Nb1 130.2(2) . . ? C14 C9 Nb1 117.6(2) . . ? C9 C10 C11 124.5(3) . . ? C9 C10 O1 127.1(3) . . ? C11 C10 O1 108.3(3) . . ? O2 C11 C12 126.6(3) . . ? O2 C11 C10 110.8(3) . . ? C12 C11 C10 122.6(3) . . ? C11 C12 C13 116.0(3) . . ? C12 C13 C14 121.2(3) . . ? C13 C14 C9 123.4(3) . . ? C13 C14 C16 120.2(3) . . ? C9 C14 C16 116.4(3) . . ? O1 C15 O2 108.8(3) . . ? N2 C16 C14 117.4(3) . . ? N2 C16 C17 123.5(3) . . ? C14 C16 C17 119.0(3) . . ? C19 C18 C23 121.4(3) . . ? C19 C18 N2 119.2(3) . . ? C23 C18 N2 119.3(3) . . ? C20 C19 C18 117.4(4) . . ? C20 C19 C24 120.0(4) . . ? C18 C19 C24 122.5(3) . . ? C21 C20 C19 122.3(4) . . ? C20 C21 C22 119.8(4) . . ? C21 C22 C23 121.2(4) . . ? C22 C23 C18 117.8(4) . . ? C22 C23 C27 118.8(3) . . ? C18 C23 C27 123.4(3) . . ? C19 C24 C26 112.6(4) . . ? C19 C24 C25 111.3(3) . . ? C26 C24 C25 108.2(4) . . ? C23 C27 C28 111.6(3) . . ? C23 C27 C29 111.5(3) . . ? C28 C27 C29 110.0(3) . . ? C31 C30 C35 112.4(3) . . ? C31 C30 Nb1 127.6(3) . . ? C35 C30 Nb1 119.8(2) . . ? C30 C31 O3 127.4(3) . . ? C30 C31 C32 125.0(3) . . ? O3 C31 C32 107.6(3) . . ? O4 C32 C33 127.4(3) . . ? O4 C32 C31 110.8(3) . . ? C33 C32 C31 121.8(3) . . ? C32 C33 C34 116.1(3) . . ? C33 C34 C35 122.0(4) . . ? C34 C35 C30 122.7(3) . . ? C34 C35 C37 120.0(3) . . ? C30 C35 C37 117.3(3) . . ? O3 C36 O4 107.4(3) . . ? N3 C37 C35 118.6(3) . . ? N3 C37 C38 123.2(3) . . ? C35 C37 C38 118.2(3) . . ? C40 C39 C44 121.5(3) . . ? C40 C39 N3 120.6(3) . . ? C44 C39 N3 117.7(3) . . ? C41 C40 C39 117.3(3) . . ? C41 C40 C45 118.9(3) . . ? C39 C40 C45 123.8(3) . . ? C42 C41 C40 122.2(4) . . ? C41 C42 C43 119.6(4) . . ? C42 C43 C44 121.5(4) . . ? C43 C44 C39 117.8(3) . . ? C43 C44 C48 120.3(3) . . ? C39 C44 C48 121.7(3) . . ? C40 C45 C47 112.1(3) . . ? C40 C45 C46 111.0(3) . . ? C47 C45 C46 109.1(3) . . ? C44 C48 C49 112.0(4) . . ? C44 C48 C50 113.4(4) . . ? C49 C48 C50 109.3(3) . . ? N4 C51 C52 120.0(3) . . ? N4 C51 C56 119.0(3) . . ? C52 C51 C56 120.9(3) . . ? C53 C52 C51 117.7(4) . . ? C53 C52 C57 121.2(4) . . ? C51 C52 C57 121.1(3) . . ? C54 C53 C52 121.8(5) . . ? C53 C54 C55 119.7(4) . . ? C54 C55 C56 121.5(5) . . ? C55 C56 C51 118.4(4) . . ? C55 C56 C58 121.5(4) . . ? C51 C56 C58 120.0(3) . . ? C60 C59 C64 112.4(3) . . ? C60 C59 Nb2 126.8(3) . . ? C64 C59 Nb2 120.4(2) . . ? C59 C60 O5 127.2(3) . . ? C59 C60 C61 125.1(3) . . ? O5 C60 C61 107.6(3) . . ? C62 C61 O6 127.4(3) . . ? C62 C61 C60 121.9(3) . . ? O6 C61 C60 110.6(3) . . ? C61 C62 C63 115.5(3) . . ? C64 C63 C62 122.1(3) . . ? C63 C64 C59 122.7(3) . . ? C63 C64 C66 119.8(3) . . ? C59 C64 C66 117.5(3) . . ? O5 C65 O6 107.0(3) . . ? N5 C66 C64 118.8(3) . . ? N5 C66 C67 123.7(3) . . ? C64 C66 C67 117.4(3) . . ? C69 C68 C73 120.9(3) . . ? C69 C68 N5 118.4(3) . . ? C73 C68 N5 120.6(3) . . ? C70 C69 C68 119.0(3) . . ? C70 C69 C74 120.4(3) . . ? C68 C69 C74 120.5(3) . . ? C71 C70 C69 121.2(4) . . ? C72 C71 C70 119.2(4) . . ? C71 C72 C73 122.6(4) . . ? C72 C73 C68 117.1(3) . . ? C72 C73 C77 118.3(3) . . ? C68 C73 C77 124.5(3) . . ? C69 C74 C75 111.4(3) . . ? C69 C74 C76 113.8(4) . . ? C75 C74 C76 110.7(4) . . ? C73 C77 C79 112.0(3) . . ? C73 C77 C78 111.3(3) . . ? C79 C77 C78 108.8(3) . . ? C81 C80 C85 111.6(3) . . ? C81 C80 Nb2 130.9(2) . . ? C85 C80 Nb2 117.2(2) . . ? C82 C81 C80 124.8(3) . . ? C82 C81 O7 107.9(3) . . ? C80 C81 O7 127.3(3) . . ? C83 C82 C81 123.0(3) . . ? C83 C82 O8 126.1(3) . . ? C81 C82 O8 111.0(3) . . ? C82 C83 C84 115.3(3) . . ? C85 C84 C83 121.4(4) . . ? C84 C85 C80 123.9(3) . . ? C84 C85 C87 120.3(3) . . ? C80 C85 C87 115.8(3) . . ? O7 C86 O8 109.3(3) . . ? N6 C87 C85 117.3(3) . . ? N6 C87 C88 123.5(3) . . ? C85 C87 C88 119.1(3) . . ? C94 C89 C90 121.2(3) . . ? C94 C89 N6 116.3(3) . . ? C90 C89 N6 122.5(3) . . ? C91 C90 C89 117.9(3) . . ? C91 C90 C95 118.3(3) . . ? C89 C90 C95 123.8(3) . . ? C92 C91 C90 122.1(4) . . ? C91 C92 C93 119.0(4) . . ? C92 C93 C94 121.9(4) . . ? C89 C94 C93 117.9(3) . . ? C89 C94 C98 122.6(3) . . ? C93 C94 C98 119.5(3) . . ? C90 C95 C96 111.4(3) . . ? C90 C95 C97 111.6(3) . . ? C96 C95 C97 109.6(3) . . ? C99 C98 C94 111.9(3) . . ? C99 C98 C100 108.5(4) . . ? C94 C98 C100 110.5(3) . . ? O9 C101 C102 109.2(5) . . ? O9 C103 C104 109.6(6) . . ? O10 C105 C106 109.8(5) . . ? O10 C107 C108 110.4(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.848 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.091 data_(1)2Ta(N-2,6-iPr2C6H3)Cl_(23) _database_code_depnum_ccdc_archive 'CCDC 722167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H81 Cl N3 O4 Ta' _chemical_formula_weight 1220.76 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.5332(8) _cell_length_b 14.7874(6) _cell_length_c 39.729(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.180(1) _cell_angle_gamma 90.00 _cell_volume 11908.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 5660 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.05 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5056 _exptl_absorpt_coefficient_mu 1.941 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66517 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 28.32 _reflns_number_total 14845 _reflns_number_gt 12324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+58.6716P] 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 14845 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.009 _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 Ta1 Ta 0.842254(7) 0.012409(9) 0.871921(3) 0.01727(5) Uani 1 1 d . . . Cl1 Cl 0.88480(4) 0.10952(6) 0.91737(2) 0.02632(18) Uani 1 1 d . . . O1 O 0.72982(14) -0.0470(2) 0.79118(7) 0.0324(6) Uani 1 1 d . . . O2 O 0.65909(15) -0.1652(2) 0.77601(7) 0.0381(7) Uani 1 1 d . . . O3 O 0.90375(14) 0.0713(2) 0.79455(7) 0.0339(6) Uani 1 1 d . . . O4 O 0.85489(19) 0.1278(3) 0.74295(8) 0.0579(11) Uani 1 1 d . . . N1 N 0.91602(14) -0.02396(19) 0.85748(7) 0.0201(6) Uani 1 1 d . . . N2 N 0.84462(14) -0.10401(19) 0.91273(7) 0.0191(6) Uani 1 1 d . . . N3 N 0.73777(14) 0.0960(2) 0.87784(7) 0.0209(6) Uani 1 1 d . . . C1 C 0.97180(17) -0.0442(2) 0.84292(9) 0.0219(7) Uani 1 1 d . A . C2 C 1.03055(19) 0.0058(3) 0.85264(10) 0.0304(8) Uani 1 1 d . . . C3 C 1.0845(2) -0.0157(3) 0.83711(11) 0.0388(10) Uani 1 1 d . . . H3A H 1.1234 0.0168 0.8429 0.047 Uiso 1 1 calc R . . C4 C 1.0818(2) -0.0836(3) 0.81343(12) 0.0409(11) Uani 1 1 d . . . H4A H 1.1187 -0.0967 0.8034 0.049 Uiso 1 1 calc R . . C5 C 1.0248(2) -0.1323(3) 0.80449(11) 0.0377(10) Uani 1 1 d . A . H5A H 1.0236 -0.1785 0.7885 0.045 Uiso 1 1 calc R . . C6 C 0.9689(2) -0.1141(3) 0.81887(10) 0.0295(8) Uani 1 1 d . . . C7 C 1.0340(2) 0.0788(3) 0.87920(12) 0.0393(10) Uani 1 1 d . . . H7A H 1.0034 0.0624 0.8948 0.047 Uiso 1 1 calc R . . C8 C 1.1025(2) 0.0915(4) 0.90074(12) 0.0479(12) Uani 1 1 d . . . H8A H 1.1171 0.0352 0.9114 0.072 Uiso 1 1 calc R . . H8B H 1.1001 0.1364 0.9179 0.072 Uiso 1 1 calc R . . H8C H 1.1332 0.1107 0.8863 0.072 Uiso 1 1 calc R . . C9 C 1.0104(3) 0.1674(4) 0.86242(15) 0.0573(14) Uani 1 1 d . . . H9A H 0.9677 0.1590 0.8490 0.086 Uiso 1 1 calc R . . H9B H 1.0409 0.1871 0.8480 0.086 Uiso 1 1 calc R . . H9C H 1.0078 0.2121 0.8796 0.086 Uiso 1 1 calc R . . C10 C 0.9063(2) -0.1672(4) 0.80817(12) 0.0504(14) Uani 1 1 d . A 1 H10A H 0.8749 -0.1567 0.8239 0.060 Uiso 1 1 calc R A 1 C10A C 0.9060 -0.1668 0.8083 0.049 Uani 0.00 1 d P A 2 C11 C 0.8754(3) -0.1499(4) 0.77291(18) 0.079(2) Uani 1 1 d . . . H11A H 0.8621 -0.0877 0.7706 0.119 Uiso 1 1 calc R A 1 H11B H 0.8375 -0.1881 0.7672 0.119 Uiso 1 1 calc R A 1 H11C H 0.9065 -0.1625 0.7578 0.119 Uiso 1 1 calc R A 1 C12B C 0.8968(8) -0.2509(9) 0.8189(3) 0.080(5) Uani 0.50 1 d P A 2 H12D H 0.8614 -0.2513 0.8320 0.120 Uiso 0.50 1 calc PR A 2 H12E H 0.9365 -0.2719 0.8328 0.120 Uiso 0.50 1 calc PR A 2 H12F H 0.8860 -0.2900 0.7995 0.120 Uiso 0.50 1 calc PR A 2 C12 C 0.9289(6) -0.2773(7) 0.8085(3) 0.042(3) Uani 0.50 1 d P A 1 H12A H 0.8906 -0.3143 0.8020 0.064 Uiso 0.50 1 calc PR A 1 H12B H 0.9499 -0.2938 0.8311 0.064 Uiso 0.50 1 calc PR A 1 H12C H 0.9592 -0.2863 0.7927 0.064 Uiso 0.50 1 calc PR A 1 C13 C 0.77407(16) -0.0988(2) 0.84989(9) 0.0190(7) Uani 1 1 d . . . C14 C 0.73428(18) -0.1064(2) 0.81844(9) 0.0240(7) Uani 1 1 d . . . C15 C 0.69213(19) -0.1785(3) 0.80832(10) 0.0287(8) Uani 1 1 d . . . C16 C 0.6872(2) -0.2517(3) 0.82876(11) 0.0344(9) Uani 1 1 d . . . H16A H 0.6592 -0.3000 0.8218 0.041 Uiso 1 1 calc R . . C17 C 0.72689(19) -0.2494(3) 0.86063(10) 0.0288(8) Uani 1 1 d . . . H17A H 0.7261 -0.2979 0.8754 0.035 Uiso 1 1 calc R . . C18 C 0.76785(17) -0.1758(2) 0.87084(9) 0.0224(7) Uani 1 1 d . . . C19 C 0.6727(2) -0.0725(3) 0.76881(11) 0.0441(11) Uani 1 1 d . . . H19A H 0.6796 -0.0663 0.7453 0.053 Uiso 1 1 calc R . . H19B H 0.6358 -0.0344 0.7722 0.053 Uiso 1 1 calc R . . C20 C 0.80814(17) -0.1744(2) 0.90483(9) 0.0221(7) Uani 1 1 d . . . C21 C 0.8044(2) -0.2531(3) 0.92855(10) 0.0311(9) Uani 1 1 d . . . H21A H 0.8331 -0.2422 0.9497 0.047 Uiso 1 1 calc R . . H21B H 0.8179 -0.3073 0.9183 0.047 Uiso 1 1 calc R . . H21C H 0.7599 -0.2599 0.9327 0.047 Uiso 1 1 calc R . . C22 C 0.89241(17) -0.1079(2) 0.94436(9) 0.0221(7) Uani 1 1 d . . . C23 C 0.87675(18) -0.0726(3) 0.97473(9) 0.0245(7) Uani 1 1 d . . . C24 C 0.9234(2) -0.0796(3) 1.00413(10) 0.0318(9) Uani 1 1 d . . . H24A H 0.9138 -0.0560 1.0245 0.038 Uiso 1 1 calc R . . C25 C 0.9834(2) -0.1204(3) 1.00381(10) 0.0365(10) Uani 1 1 d . . . H25A H 1.0140 -0.1242 1.0237 0.044 Uiso 1 1 calc R . . C26 C 0.99785(19) -0.1559(3) 0.97370(11) 0.0323(9) Uani 1 1 d . . . H26A H 1.0383 -0.1841 0.9737 0.039 Uiso 1 1 calc R . . C27 C 0.95341(18) -0.1506(2) 0.94337(9) 0.0239(7) Uani 1 1 d . . . C28 C 0.97285(19) -0.1923(3) 0.91135(10) 0.0279(8) Uani 1 1 d . . . H28A H 0.9426 -0.1696 0.8916 0.033 Uiso 1 1 calc R . . C29 C 0.9675(2) -0.2957(3) 0.91179(12) 0.0384(10) Uani 1 1 d . . . H29A H 0.9234 -0.3128 0.9143 0.058 Uiso 1 1 calc R . . H29B H 0.9980 -0.3194 0.9306 0.058 Uiso 1 1 calc R . . H29C H 0.9777 -0.3198 0.8908 0.058 Uiso 1 1 calc R . . C30 C 1.0430(2) -0.1662(3) 0.90702(12) 0.0395(10) Uani 1 1 d . . . H30A H 1.0468 -0.1015 0.9066 0.059 Uiso 1 1 calc R . . H30B H 1.0528 -0.1908 0.8860 0.059 Uiso 1 1 calc R . . H30C H 1.0736 -0.1899 0.9257 0.059 Uiso 1 1 calc R . . C31 C 0.8102(2) -0.0309(3) 0.97755(10) 0.0328(9) Uani 1 1 d . . . H31A H 0.7856 -0.0226 0.9545 0.039 Uiso 1 1 calc R . . C32 C 0.8180(2) 0.0615(3) 0.99523(11) 0.0407(10) Uani 1 1 d . . . H32A H 0.8429 0.1009 0.9829 0.061 Uiso 1 1 calc R . . H32B H 0.8408 0.0542 1.0181 0.061 Uiso 1 1 calc R . . H32C H 0.7752 0.0872 0.9957 0.061 Uiso 1 1 calc R . . C33 C 0.7698(2) -0.0935(4) 0.99754(13) 0.0509(13) Uani 1 1 d . . . H33A H 0.7641 -0.1513 0.9865 0.076 Uiso 1 1 calc R . . H33B H 0.7273 -0.0669 0.9982 0.076 Uiso 1 1 calc R . . H33C H 0.7927 -0.1011 1.0204 0.076 Uiso 1 1 calc R . . C34 C 0.81067(18) 0.0940(2) 0.82607(9) 0.0235(7) Uani 1 1 d . . . C35 C 0.8417(2) 0.1012(3) 0.79781(10) 0.0278(8) Uani 1 1 d . . . C36 C 0.8138(3) 0.1375(3) 0.76685(11) 0.0443(12) Uani 1 1 d . . . C37 C 0.7517(3) 0.1720(4) 0.76173(12) 0.0572(16) Uani 1 1 d . . . H37A H 0.7324 0.1948 0.7407 0.069 Uiso 1 1 calc R . . C38 C 0.7184(2) 0.1715(3) 0.78969(11) 0.0453(12) Uani 1 1 d . . . H38A H 0.6764 0.1968 0.7876 0.054 Uiso 1 1 calc R . . C39 C 0.7465(2) 0.1339(3) 0.82064(9) 0.0286(8) Uani 1 1 d . . . C40 C 0.9156(2) 0.0985(3) 0.76187(11) 0.0416(11) Uani 1 1 d . . . H40A H 0.9330 0.0482 0.7504 0.050 Uiso 1 1 calc R . . H40B H 0.9476 0.1473 0.7640 0.050 Uiso 1 1 calc R . . C41 C 0.71052(19) 0.1350(3) 0.84996(10) 0.0276(8) Uani 1 1 d . . . C42 C 0.6455(2) 0.1841(3) 0.84579(11) 0.0400(11) Uani 1 1 d . . . H42A H 0.6271 0.1794 0.8665 0.060 Uiso 1 1 calc R . . H42B H 0.6156 0.1575 0.8274 0.060 Uiso 1 1 calc R . . H42C H 0.6522 0.2466 0.8409 0.060 Uiso 1 1 calc R . . C43 C 0.70657(17) 0.1102(2) 0.90779(9) 0.0225(7) Uani 1 1 d . . . C44 C 0.66330(17) 0.0446(3) 0.91714(10) 0.0251(7) Uani 1 1 d . . . C45 C 0.63175(18) 0.0619(3) 0.94488(10) 0.0276(8) Uani 1 1 d . . . H45A H 0.6029 0.0190 0.9513 0.033 Uiso 1 1 calc R . . C46 C 0.64224(19) 0.1413(3) 0.96308(10) 0.0293(8) Uani 1 1 d . . . H46A H 0.6205 0.1518 0.9815 0.035 Uiso 1 1 calc R . . C47 C 0.68504(19) 0.2048(3) 0.95390(10) 0.0274(8) Uani 1 1 d . . . H47A H 0.6925 0.2576 0.9666 0.033 Uiso 1 1 calc R . . C48 C 0.71763(17) 0.1922(2) 0.92595(9) 0.0237(7) Uani 1 1 d . . . C49 C 0.76070(19) 0.2685(3) 0.91621(10) 0.0274(8) Uani 1 1 d . . . H49A H 0.7831 0.2471 0.8977 0.033 Uiso 1 1 calc R . . C50 C 0.8133(2) 0.2980(3) 0.94606(11) 0.0353(9) Uani 1 1 d . . . H50A H 0.8401 0.2470 0.9543 0.053 Uiso 1 1 calc R . . H50B H 0.7922 0.3215 0.9641 0.053 Uiso 1 1 calc R . . H50C H 0.8406 0.3441 0.9385 0.053 Uiso 1 1 calc R . . C51 C 0.7195(2) 0.3525(3) 0.90354(12) 0.0384(10) Uani 1 1 d . . . H51A H 0.6863 0.3359 0.8847 0.058 Uiso 1 1 calc R . . H51B H 0.7478 0.3978 0.8963 0.058 Uiso 1 1 calc R . . H51C H 0.6987 0.3760 0.9217 0.058 Uiso 1 1 calc R . . C52 C 0.6490(2) -0.0421(3) 0.89664(11) 0.0329(9) Uani 1 1 d . . . H52A H 0.6887 -0.0563 0.8868 0.040 Uiso 1 1 calc R . . C53 C 0.6358(2) -0.1231(3) 0.91822(13) 0.0453(11) Uani 1 1 d . . . H53A H 0.6715 -0.1299 0.9368 0.068 Uiso 1 1 calc R . . H53B H 0.6321 -0.1767 0.9044 0.068 Uiso 1 1 calc R . . H53C H 0.5954 -0.1137 0.9270 0.068 Uiso 1 1 calc R . . C54 C 0.5930(3) -0.0312(4) 0.86713(15) 0.0679(17) Uani 1 1 d . . . H54A H 0.6017 0.0198 0.8535 0.102 Uiso 1 1 calc R . . H54B H 0.5525 -0.0215 0.8758 0.102 Uiso 1 1 calc R . . H54C H 0.5893 -0.0849 0.8534 0.102 Uiso 1 1 calc R . . C84 C 0.4455(8) 0.1203(10) 1.0002(4) 0.056(4) Uiso 0.50 1 d P B -1 H84A H 0.4203 0.1726 0.9997 0.067 Uiso 0.50 1 calc PR B -1 C85 C 0.4258(7) 0.0317(9) 0.9779(3) 0.069(3) Uiso 0.50 1 d P B -1 H85A H 0.3826 0.0272 0.9632 0.083 Uiso 0.50 1 d P C -1 C86 C 0.5239(6) -0.0419(8) 1.0016(3) 0.053(3) Uiso 0.50 1 d P B -1 C87 C 0.5707(9) -0.1074(12) 1.0073(5) 0.078(5) Uiso 0.50 1 d P B -1 H87A H 0.5572 -0.1586 0.9931 0.116 Uiso 0.50 1 calc PR B -1 H87B H 0.5764 -0.1254 1.0308 0.116 Uiso 0.50 1 calc PR B -1 H87C H 0.6117 -0.0844 1.0021 0.116 Uiso 0.50 1 calc PR B -1 C88 C 0.5037(6) 0.1073(8) 1.0197(3) 0.059(3) Uiso 0.50 1 d P B -1 H88A H 0.5207 0.1548 1.0337 0.071 Uiso 0.50 1 calc PR B -1 C89 C 0.5374(3) 0.0374(4) 1.02075(15) 0.0590(14) Uiso 1 1 d . B -1 H89A H 0.5765 0.0376 1.0362 0.071 Uiso 1 1 calc R B -1 C90 C 0.6860(8) 0.0426(12) 0.6567(4) 0.093(5) Uiso 0.50 1 d P D 1 H90A H 0.6931 0.1022 0.6508 0.111 Uiso 0.50 1 calc PR D 1 C91 C 0.7231(8) -0.0966(11) 0.6839(4) 0.090(4) Uiso 0.50 1 d P D 1 H91A H 0.7524 -0.1345 0.6975 0.108 Uiso 0.50 1 calc PR D 1 C92 C 0.6311(6) -0.0899(8) 0.6400(3) 0.054(3) Uiso 0.50 1 d P D 1 C93 C 0.6369(5) -0.1639(8) 0.6466(3) 0.050(2) Uiso 0.50 1 d P E 2 H93A H 0.6360 -0.2266 0.6482 0.060 Uiso 0.50 1 calc PR E 2 C94 C 0.5984(5) -0.0246(7) 0.6201(3) 0.050(2) Uiso 0.50 1 d P E 2 H94A H 0.5723 0.0117 0.6043 0.060 Uiso 0.50 1 calc PR E 2 C95 C 0.6887(5) -0.0265(7) 0.6669(3) 0.045(2) Uiso 0.50 1 d P E 2 C96 C 0.7352(5) 0.0098(6) 0.6858(3) 0.116(3) Uiso 1 1 d . D 1 H96A H 0.7652 0.0427 0.7011 0.139 Uiso 0.50 1 calc PR D 1 C97 C 0.5855(4) -0.1236(5) 0.6197(2) 0.089(2) Uiso 1 1 d . D 1 H97A H 0.5909 -0.1881 0.6193 0.134 Uiso 0.50 1 calc PR D 1 H97B H 0.5864 -0.0997 0.5973 0.134 Uiso 0.50 1 calc PR D 1 H97C H 0.5441 -0.1093 0.6266 0.134 Uiso 0.50 1 calc PR D 1 C98 C 0.6787(3) -0.1283(4) 0.66604(16) 0.0657(16) Uiso 1 1 d . D 1 H98A H 0.6733 -0.1899 0.6693 0.079 Uiso 0.50 1 calc PR D 1 C99 C 0.6430(3) 0.0117(4) 0.64066(18) 0.0692(17) Uiso 1 1 d . D 1 H99A H 0.6130 0.0489 0.6271 0.083 Uiso 0.50 1 calc PR D 1 C96A C 0.7370 0.0113 0.6867 0.112 Uiso 0.00 1 d P E 2 H96B H 0.7223 0.0670 0.6953 0.169 Uiso 0.50 1 calc PR E 2 H96C H 0.7722 0.0235 0.6740 0.169 Uiso 0.50 1 calc PR E 2 H96D H 0.7527 -0.0284 0.7053 0.169 Uiso 0.50 1 calc PR E 2 C97A C 0.5843 -0.1249 0.6192 0.088 Uiso 0.00 1 d P E 2 H97D H 0.5511 -0.1557 0.6051 0.106 Uiso 0.50 1 calc PR E 2 C98A C 0.6789 -0.1295 0.6664 0.066 Uiso 0.00 1 d P E 2 H98B H 0.7065 -0.1653 0.6818 0.079 Uiso 0.50 1 calc PR E 2 C99A C 0.6427 0.0131 0.6406 0.069 Uiso 0.00 1 d P E 2 H99B H 0.6458 0.0755 0.6383 0.083 Uiso 0.50 1 calc PR E 2 C1T C 0.4926(5) -0.0837(7) 0.7652(2) 0.036(2) Uiso 0.50 1 d P F -1 C2T C 0.4943(7) 0.0047(9) 0.7692(4) 0.067(3) Uiso 0.50 1 d P F -1 H2TA H 0.4849 0.0302 0.7893 0.080 Uiso 0.50 1 calc PR F -1 C3T C 0.5108(7) 0.0621(9) 0.7423(4) 0.072(4) Uiso 0.50 1 d P F -1 H3TA H 0.5122 0.1248 0.7442 0.087 Uiso 0.50 1 calc PR F -1 C4T C 0.5242(7) 0.0178(9) 0.7135(4) 0.072(3) Uiso 0.50 1 d P F -1 H4TA H 0.5350 0.0534 0.6959 0.086 Uiso 0.50 1 calc PR F -1 C5T C 0.5231(6) -0.0709(9) 0.7089(3) 0.068(3) Uiso 0.50 1 d P F -1 H5TA H 0.5330 -0.0964 0.6889 0.081 Uiso 0.50 1 calc PR F -1 C6T C 0.4761(7) -0.1498(9) 0.7913(3) 0.074(4) Uiso 0.50 1 d P F -1 H6TA H 0.4672 -0.1175 0.8110 0.110 Uiso 0.50 1 calc PR F -1 H6TB H 0.5127 -0.1900 0.7977 0.110 Uiso 0.50 1 calc PR F -1 H6TC H 0.4379 -0.1841 0.7818 0.110 Uiso 0.50 1 calc PR F -1 C7T C 0.5069(5) -0.1231(8) 0.7345(3) 0.045(2) Uiso 0.50 1 d P F -1 H7TA H 0.5051 -0.1856 0.7319 0.054 Uiso 0.50 1 calc PR F -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 Ta1 0.01616(7) 0.01888(7) 0.01674(7) 0.00055(5) 0.00254(5) -0.00050(5) Cl1 0.0245(4) 0.0308(5) 0.0224(4) -0.0062(3) 0.0001(3) -0.0001(3) O1 0.0323(15) 0.0424(16) 0.0193(13) 0.0024(11) -0.0058(11) -0.0076(12) O2 0.0353(16) 0.0512(19) 0.0237(14) -0.0087(13) -0.0077(12) -0.0091(14) O3 0.0333(15) 0.0464(17) 0.0253(14) 0.0098(12) 0.0147(12) 0.0052(13) O4 0.076(3) 0.071(2) 0.0342(18) 0.0271(17) 0.0328(18) 0.038(2) N1 0.0160(13) 0.0230(15) 0.0219(14) -0.0017(11) 0.0053(11) 0.0001(11) N2 0.0159(14) 0.0244(15) 0.0170(14) 0.0024(11) 0.0022(11) 0.0009(11) N3 0.0187(14) 0.0242(15) 0.0205(15) -0.0033(11) 0.0048(12) 0.0033(11) C1 0.0216(17) 0.0241(17) 0.0211(17) 0.0046(13) 0.0062(14) 0.0005(14) C2 0.0250(18) 0.034(2) 0.033(2) -0.0019(16) 0.0079(16) -0.0054(16) C3 0.0232(19) 0.055(3) 0.040(2) -0.001(2) 0.0108(17) -0.0087(19) C4 0.027(2) 0.061(3) 0.039(2) 0.001(2) 0.0168(19) 0.004(2) C5 0.039(2) 0.041(2) 0.037(2) -0.0075(18) 0.0190(19) 0.0034(19) C6 0.031(2) 0.032(2) 0.028(2) -0.0043(16) 0.0135(16) -0.0051(16) C7 0.030(2) 0.043(2) 0.048(3) -0.011(2) 0.016(2) -0.0152(19) C8 0.041(3) 0.060(3) 0.043(3) -0.005(2) 0.009(2) -0.023(2) C9 0.047(3) 0.053(3) 0.069(4) -0.012(3) 0.001(3) -0.008(2) C10 0.048(3) 0.066(3) 0.045(3) -0.033(2) 0.032(2) -0.032(2) C10A 0.050 0.061 0.044 -0.030 0.029 -0.032 C11 0.059(4) 0.053(3) 0.109(6) 0.021(3) -0.035(4) -0.025(3) C12B 0.107(13) 0.068(9) 0.055(8) 0.011(7) -0.017(8) -0.054(9) C12 0.050(6) 0.028(5) 0.054(7) -0.008(4) 0.022(5) -0.004(4) C13 0.0154(16) 0.0232(17) 0.0191(16) -0.0015(13) 0.0050(13) 0.0020(13) C14 0.0230(18) 0.0288(19) 0.0209(18) -0.0023(14) 0.0051(14) 0.0024(14) C15 0.0241(19) 0.039(2) 0.0223(19) -0.0093(16) 0.0002(15) -0.0034(16) C16 0.035(2) 0.031(2) 0.036(2) -0.0077(17) 0.0033(18) -0.0127(17) C17 0.029(2) 0.031(2) 0.027(2) 0.0001(15) 0.0043(16) -0.0075(16) C18 0.0173(17) 0.0233(18) 0.0270(19) 0.0001(14) 0.0046(14) -0.0006(13) C19 0.042(3) 0.058(3) 0.027(2) 0.002(2) -0.0100(19) -0.014(2) C20 0.0182(17) 0.0253(18) 0.0239(18) 0.0028(14) 0.0064(14) 0.0019(13) C21 0.033(2) 0.031(2) 0.028(2) 0.0088(16) 0.0001(16) -0.0059(16) C22 0.0203(17) 0.0227(17) 0.0225(18) 0.0049(13) 0.0005(14) -0.0028(13) C23 0.0224(18) 0.032(2) 0.0181(17) 0.0004(14) 0.0003(14) -0.0010(14) C24 0.034(2) 0.040(2) 0.0190(18) -0.0011(16) -0.0030(16) 0.0014(17) C25 0.036(2) 0.043(2) 0.025(2) 0.0018(17) -0.0126(17) -0.0009(19) C26 0.0216(19) 0.035(2) 0.037(2) 0.0038(17) -0.0037(16) 0.0050(16) C27 0.0215(18) 0.0233(18) 0.0256(19) 0.0031(14) 0.0000(14) 0.0009(14) C28 0.0248(19) 0.035(2) 0.0241(19) 0.0060(15) 0.0036(15) 0.0063(16) C29 0.041(3) 0.035(2) 0.040(2) -0.0018(18) 0.011(2) 0.0061(19) C30 0.026(2) 0.050(3) 0.043(3) 0.013(2) 0.0089(18) 0.0101(19) C31 0.028(2) 0.048(3) 0.0217(19) -0.0007(17) 0.0024(15) 0.0053(17) C32 0.045(3) 0.050(3) 0.028(2) -0.0033(19) 0.0070(19) 0.014(2) C33 0.040(3) 0.072(4) 0.043(3) -0.004(2) 0.016(2) -0.009(2) C34 0.0256(19) 0.0239(18) 0.0209(17) 0.0005(13) 0.0036(14) 0.0014(14) C35 0.034(2) 0.0256(19) 0.0250(19) 0.0042(14) 0.0094(16) 0.0041(15) C36 0.065(3) 0.047(3) 0.026(2) 0.0143(19) 0.019(2) 0.023(2) C37 0.071(4) 0.080(4) 0.024(2) 0.023(2) 0.014(2) 0.046(3) C38 0.053(3) 0.059(3) 0.025(2) 0.011(2) 0.008(2) 0.034(2) C39 0.037(2) 0.028(2) 0.0205(18) 0.0020(14) 0.0046(16) 0.0132(16) C40 0.052(3) 0.045(3) 0.032(2) 0.0105(19) 0.022(2) 0.001(2) C41 0.0256(19) 0.032(2) 0.0241(19) -0.0028(15) -0.0004(15) 0.0078(15) C42 0.038(2) 0.057(3) 0.023(2) 0.0013(19) 0.0009(18) 0.023(2) C43 0.0165(16) 0.032(2) 0.0191(17) -0.0015(14) 0.0044(13) 0.0055(14) C44 0.0179(17) 0.0301(19) 0.0270(19) -0.0001(15) 0.0029(14) 0.0032(14) C45 0.0200(18) 0.035(2) 0.029(2) 0.0036(16) 0.0068(15) 0.0027(15) C46 0.028(2) 0.038(2) 0.0237(19) 0.0006(16) 0.0080(15) 0.0094(16) C47 0.029(2) 0.0278(19) 0.0255(19) -0.0048(15) 0.0049(15) 0.0063(15) C48 0.0190(17) 0.0293(19) 0.0234(18) -0.0005(14) 0.0050(14) 0.0055(14) C49 0.0264(19) 0.030(2) 0.028(2) -0.0047(15) 0.0104(16) 0.0009(15) C50 0.034(2) 0.035(2) 0.038(2) -0.0140(18) 0.0083(18) -0.0035(17) C51 0.042(3) 0.033(2) 0.042(3) 0.0039(18) 0.013(2) 0.0043(19) C52 0.026(2) 0.036(2) 0.038(2) -0.0084(18) 0.0086(17) -0.0074(16) C53 0.043(3) 0.038(3) 0.057(3) -0.007(2) 0.013(2) -0.009(2) C54 0.077(4) 0.061(4) 0.055(3) -0.014(3) -0.020(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 1.786(3) . ? Ta1 C34 2.195(4) . ? Ta1 C13 2.245(3) . ? Ta1 N2 2.360(3) . ? Ta1 Cl1 2.3627(9) . ? Ta1 N3 2.519(3) . ? O1 C14 1.385(4) . ? O1 C19 1.406(5) . ? O2 C15 1.367(5) . ? O2 C19 1.435(6) . ? O3 C35 1.374(5) . ? O3 C40 1.417(5) . ? O4 C36 1.374(5) . ? O4 C40 1.418(6) . ? N1 C1 1.396(4) . ? N2 C20 1.292(5) . ? N2 C22 1.467(4) . ? N3 C41 1.294(5) . ? N3 C43 1.454(4) . ? C1 C6 1.401(5) . ? C1 C2 1.415(5) . ? C2 C3 1.388(6) . ? C2 C7 1.504(6) . ? C3 C4 1.371(6) . ? C4 C5 1.373(6) . ? C5 C6 1.387(5) . ? C6 C10 1.510(6) . ? C6 C10A 1.511(4) . ? C7 C9 1.513(7) . ? C7 C8 1.537(6) . ? C10 C11 1.465(8) . ? C10 C12 1.693(11) . ? C10A C12B 1.336(12) . ? C10A C11 1.467(6) . ? C13 C14 1.384(5) . ? C13 C18 1.428(5) . ? C14 C15 1.392(5) . ? C15 C16 1.367(6) . ? C16 C17 1.393(6) . ? C17 C18 1.395(5) . ? C18 C20 1.467(5) . ? C20 C21 1.506(5) . ? C22 C23 1.399(5) . ? C22 C27 1.408(5) . ? C23 C24 1.392(5) . ? C23 C31 1.520(5) . ? C24 C25 1.372(6) . ? C25 C26 1.381(6) . ? C26 C27 1.393(5) . ? C27 C28 1.524(5) . ? C28 C30 1.528(6) . ? C28 C29 1.533(6) . ? C31 C32 1.533(6) . ? C31 C33 1.545(6) . ? C34 C35 1.381(5) . ? C34 C39 1.429(5) . ? C35 C36 1.380(6) . ? C36 C37 1.359(7) . ? C37 C38 1.394(6) . ? C38 C39 1.388(5) . ? C39 C41 1.476(5) . ? C41 C42 1.506(5) . ? C43 C44 1.404(5) . ? C43 C48 1.411(5) . ? C44 C45 1.388(5) . ? C44 C52 1.523(6) . ? C45 C46 1.377(6) . ? C46 C47 1.375(6) . ? C47 C48 1.397(5) . ? C48 C49 1.520(5) . ? C49 C50 1.535(5) . ? C49 C51 1.542(6) . ? C52 C54 1.514(7) . ? C52 C53 1.522(6) . ? C84 C88 1.329(18) . ? C84 C85 1.60(2) . ? C86 C87 1.36(2) . ? C86 C89 1.400(12) . ? C88 C89 1.241(12) . ? C90 C99 1.103(16) . ? C90 C96 1.491(19) . ? C91 C98 1.161(16) . ? C91 C96 1.592(17) . ? C92 C97 1.240(12) . ? C92 C98 1.423(13) . ? C92 C99 1.522(13) . ? C93 C98A 1.185(11) . ? C93 C97A 1.520(11) . ? C94 C99A 1.251(11) . ? C94 C97A 1.511(10) . ? C95 C96A 1.291(10) . ? C95 C99A 1.420(10) . ? C95 C98A 1.535(10) . ? C1T C2T 1.316(16) . ? C1T C7T 1.425(11) . ? C1T C6T 1.501(16) . ? C2T C3T 1.449(17) . ? C3T C4T 1.382(19) . ? C4T C5T 1.324(18) . ? C5T C7T 1.361(16) . ? 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 N1 Ta1 C34 93.01(13) . . ? N1 Ta1 C13 99.34(12) . . ? C34 Ta1 C13 89.76(13) . . ? N1 Ta1 N2 94.33(12) . . ? C34 Ta1 N2 160.41(12) . . ? C13 Ta1 N2 71.13(11) . . ? N1 Ta1 Cl1 101.50(10) . . ? C34 Ta1 Cl1 108.93(10) . . ? C13 Ta1 Cl1 151.02(9) . . ? N2 Ta1 Cl1 87.35(7) . . ? N1 Ta1 N3 162.98(12) . . ? C34 Ta1 N3 70.39(12) . . ? C13 Ta1 N3 84.74(11) . . ? N2 Ta1 N3 102.61(10) . . ? Cl1 Ta1 N3 81.20(7) . . ? C14 O1 C19 105.6(3) . . ? C15 O2 C19 104.0(3) . . ? C35 O3 C40 107.0(3) . . ? C36 O4 C40 104.5(3) . . ? C1 N1 Ta1 172.7(3) . . ? C20 N2 C22 117.3(3) . . ? C20 N2 Ta1 118.3(2) . . ? C22 N2 Ta1 123.7(2) . . ? C41 N3 C43 116.7(3) . . ? C41 N3 Ta1 113.4(2) . . ? C43 N3 Ta1 129.8(2) . . ? N1 C1 C6 119.5(3) . . ? N1 C1 C2 119.6(3) . . ? C6 C1 C2 120.8(3) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 C7 121.6(4) . . ? C1 C2 C7 120.7(3) . . ? C4 C3 C2 121.7(4) . . ? C3 C4 C5 120.0(4) . . ? C4 C5 C6 121.2(4) . . ? C5 C6 C1 118.5(4) . . ? C5 C6 C10 120.4(4) . . ? C1 C6 C10 121.1(3) . . ? C5 C6 C10A 120.8(3) . . ? C1 C6 C10A 120.7(3) . . ? C10 C6 C10A 0.39(19) . . ? C2 C7 C9 109.7(4) . . ? C2 C7 C8 114.5(4) . . ? C9 C7 C8 109.9(4) . . ? C11 C10 C6 113.4(4) . . ? C11 C10 C12 104.7(6) . . ? C6 C10 C12 106.1(5) . . ? C12B C10A C11 113.7(6) . . ? C12B C10A C6 123.4(7) . . ? C11 C10A C6 113.2(3) . . ? C10 C11 C10A 0.4(2) . . ? C14 C13 C18 111.5(3) . . ? C14 C13 Ta1 130.7(3) . . ? C18 C13 Ta1 117.7(2) . . ? C13 C14 O1 127.6(3) . . ? C13 C14 C15 125.0(4) . . ? O1 C14 C15 107.4(3) . . ? O2 C15 C16 126.8(4) . . ? O2 C15 C14 110.7(4) . . ? C16 C15 C14 122.5(4) . . ? C15 C16 C17 115.6(4) . . ? C16 C17 C18 121.5(4) . . ? C17 C18 C13 123.9(3) . . ? C17 C18 C20 120.2(3) . . ? C13 C18 C20 115.8(3) . . ? O1 C19 O2 107.4(3) . . ? N2 C20 C18 117.0(3) . . ? N2 C20 C21 123.8(3) . . ? C18 C20 C21 119.2(3) . . ? C23 C22 C27 121.3(3) . . ? C23 C22 N2 120.7(3) . . ? C27 C22 N2 118.0(3) . . ? C24 C23 C22 118.3(3) . . ? C24 C23 C31 118.4(3) . . ? C22 C23 C31 123.2(3) . . ? C25 C24 C23 121.5(4) . . ? C24 C25 C26 119.5(4) . . ? C25 C26 C27 121.7(4) . . ? C26 C27 C22 117.7(3) . . ? C26 C27 C28 118.5(3) . . ? C22 C27 C28 123.9(3) . . ? C27 C28 C30 111.7(3) . . ? C27 C28 C29 111.5(3) . . ? C30 C28 C29 108.9(3) . . ? C23 C31 C32 111.5(3) . . ? C23 C31 C33 111.0(4) . . ? C32 C31 C33 108.9(4) . . ? C35 C34 C39 112.3(3) . . ? C35 C34 Ta1 127.1(3) . . ? C39 C34 Ta1 119.7(3) . . ? O3 C35 C36 107.5(3) . . ? O3 C35 C34 127.4(3) . . ? C36 C35 C34 125.1(4) . . ? C37 C36 O4 126.9(4) . . ? C37 C36 C35 121.7(4) . . ? O4 C36 C35 111.2(4) . . ? C36 C37 C38 116.5(4) . . ? C39 C38 C37 121.3(4) . . ? C38 C39 C34 122.9(4) . . ? C38 C39 C41 120.3(4) . . ? C34 C39 C41 116.8(3) . . ? O3 C40 O4 107.9(3) . . ? N3 C41 C39 117.9(3) . . ? N3 C41 C42 124.3(3) . . ? C39 C41 C42 117.7(3) . . ? C44 C43 C48 121.0(3) . . ? C44 C43 N3 119.8(3) . . ? C48 C43 N3 119.1(3) . . ? C45 C44 C43 118.5(4) . . ? C45 C44 C52 120.3(3) . . ? C43 C44 C52 121.1(3) . . ? C46 C45 C44 121.3(4) . . ? C47 C46 C45 119.7(4) . . ? C46 C47 C48 121.8(4) . . ? C47 C48 C43 117.5(3) . . ? C47 C48 C49 118.4(3) . . ? C43 C48 C49 124.1(3) . . ? C48 C49 C50 112.4(3) . . ? C48 C49 C51 111.7(3) . . ? C50 C49 C51 107.7(3) . . ? C54 C52 C53 109.8(4) . . ? C54 C52 C44 112.4(4) . . ? C53 C52 C44 113.4(4) . . ? C88 C84 C85 109.2(12) . . ? C87 C86 C89 115.6(12) . . ? C89 C88 C84 125.8(12) . . ? C88 C89 C86 128.1(9) . . ? C99 C90 C96 134.0(17) . . ? C98 C91 C96 122.0(14) . . ? C97 C92 C98 132.3(10) . . ? C97 C92 C99 120.7(10) . . ? C98 C92 C99 106.9(8) . . ? C98A C93 C97A 132.1(9) . . ? C99A C94 C97A 124.7(8) . . ? C96A C95 C99A 128.7(8) . . ? C96A C95 C98A 121.7(7) . . ? C99A C95 C98A 109.2(6) . . ? C90 C96 C91 101.7(11) . . ? C91 C98 C92 131.7(11) . . ? C90 C99 C92 122.1(12) . . ? C94 C97A C93 104.1(6) . . ? C93 C98A C95 121.0(7) . . ? C94 C99A C95 128.7(6) . . ? C2T C1T C7T 120.3(10) . . ? C2T C1T C6T 124.6(11) . . ? C7T C1T C6T 115.2(9) . . ? C1T C2T C3T 119.8(12) . . ? C4T C3T C2T 115.7(13) . . ? C5T C4T C3T 125.6(14) . . ? C4T C5T C7T 117.4(14) . . ? C5T C7T C1T 121.1(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.692 _refine_diff_density_min -1.670 _refine_diff_density_rms 0.117 data_(2)2Ta(N-2,6-iPr2C6H3)Cl_(24) _database_code_depnum_ccdc_archive 'CCDC 722168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H62 Cl N3 O4.50 Ta' _chemical_formula_weight 1017.45 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5748(5) _cell_length_b 12.4236(6) _cell_length_c 21.464(1) _cell_angle_alpha 106.673(1) _cell_angle_beta 91.012(1) _cell_angle_gamma 101.091(1) _cell_volume 2393.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6388 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.00 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 2.400 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27256 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11859 _reflns_number_gt 9593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+2.7365P] 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 11859 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Ta1 Ta 0.363235(18) 0.500188(16) 0.240129(9) 0.03335(6) Uani 1 1 d . . . Cl1 Cl 0.52665(12) 0.46528(12) 0.15822(6) 0.0484(3) Uani 1 1 d . . . O1 O 0.6001(5) 0.6695(3) 0.3802(2) 0.0730(13) Uani 1 1 d . . . O2 O 0.6912(5) 0.6328(4) 0.47008(19) 0.0747(13) Uani 1 1 d . . . O3 O 0.1920(4) 0.4581(4) 0.38875(16) 0.0651(12) Uani 1 1 d . . . O4 O -0.0429(4) 0.4169(5) 0.41196(19) 0.0803(15) Uani 1 1 d . . . N1 N 0.4067(4) 0.6527(4) 0.27270(19) 0.0459(10) Uani 1 1 d . . . N2 N 0.3345(4) 0.2888(3) 0.22533(18) 0.0383(8) Uani 1 1 d . . . N3 N 0.1947(4) 0.4959(3) 0.16031(17) 0.0383(8) Uani 1 1 d . . . C1 C 0.4519(6) 0.7703(5) 0.3034(3) 0.0569(14) Uani 1 1 d . . . C2 C 0.5543(8) 0.8368(6) 0.2765(4) 0.0777(19) Uani 1 1 d . . . C3 C 0.6015(10) 0.9511(6) 0.3094(5) 0.102(3) Uani 1 1 d . . . H3A H 0.6712 0.9952 0.2922 0.122 Uiso 1 1 calc R . . C4 C 0.5486(11) 1.0021(7) 0.3670(5) 0.106(3) Uani 1 1 d . . . H4A H 0.5818 1.0797 0.3883 0.127 Uiso 1 1 calc R . . C5 C 0.4464(11) 0.9376(7) 0.3930(4) 0.102(3) Uani 1 1 d . . . H5A H 0.4103 0.9726 0.4319 0.123 Uiso 1 1 calc R . . C6 C 0.3955(8) 0.8211(5) 0.3622(3) 0.0722(18) Uani 1 1 d . . . C7 C 0.6139(9) 0.7821(7) 0.2125(4) 0.097(3) Uani 1 1 d . . . H7A H 0.5462 0.7108 0.1899 0.116 Uiso 1 1 calc R . . C8 C 0.7520(11) 0.7501(9) 0.2300(6) 0.137(4) Uani 1 1 d . . . H8A H 0.7334 0.7017 0.2579 0.206 Uiso 1 1 calc R . . H8B H 0.8204 0.8186 0.2522 0.206 Uiso 1 1 calc R . . H8C H 0.7893 0.7098 0.1908 0.206 Uiso 1 1 calc R . . C9 C 0.6356(14) 0.8580(9) 0.1662(6) 0.159(5) Uani 1 1 d . . . H9A H 0.5463 0.8763 0.1565 0.238 Uiso 1 1 calc R . . H9B H 0.6703 0.8172 0.1264 0.238 Uiso 1 1 calc R . . H9C H 0.7037 0.9275 0.1867 0.238 Uiso 1 1 calc R . . C10 C 0.2836(9) 0.7503(7) 0.3916(3) 0.093(3) Uani 1 1 d . . . H10A H 0.2949 0.6706 0.3745 0.111 Uiso 1 1 calc R . . C11 C 0.1325(10) 0.7525(8) 0.3672(5) 0.123(3) Uani 1 1 d . . . H11A H 0.1245 0.7301 0.3204 0.184 Uiso 1 1 calc R . . H11B H 0.1149 0.8286 0.3840 0.184 Uiso 1 1 calc R . . H11C H 0.0637 0.7000 0.3820 0.184 Uiso 1 1 calc R . . C12 C 0.2975(14) 0.7794(9) 0.4660(4) 0.140(4) Uani 1 1 d . . . H12A H 0.3925 0.7775 0.4802 0.210 Uiso 1 1 calc R . . H12B H 0.2299 0.7241 0.4794 0.210 Uiso 1 1 calc R . . H12C H 0.2789 0.8547 0.4851 0.210 Uiso 1 1 calc R . . C13 C 0.4690(5) 0.4729(4) 0.3240(2) 0.0384(10) Uani 1 1 d . . . C14 C 0.5556(5) 0.5553(4) 0.3747(2) 0.0458(11) Uani 1 1 d . . . C15 C 0.6118(5) 0.5329(5) 0.4287(2) 0.0514(13) Uani 1 1 d . . . C16 C 0.5862(6) 0.4296(6) 0.4370(2) 0.0595(15) Uani 1 1 d . . . H16A H 0.6215 0.4167 0.4743 0.071 Uiso 1 1 calc R . . C17 C 0.5037(6) 0.3412(5) 0.3871(2) 0.0517(13) Uani 1 1 d . . . H17A H 0.4845 0.2670 0.3907 0.062 Uiso 1 1 calc R . . C18 C 0.4488(5) 0.3617(4) 0.3315(2) 0.0409(10) Uani 1 1 d . . . C19 C 0.6986(8) 0.7169(6) 0.4360(3) 0.087(2) Uani 1 1 d . . . H19A H 0.6744 0.7862 0.4639 0.105 Uiso 1 1 calc R . . H19B H 0.7945 0.7362 0.4230 0.105 Uiso 1 1 calc R . . C20 C 0.3741(5) 0.2650(4) 0.2764(2) 0.0429(10) Uani 1 1 d . . . C21 C 0.3547(8) 0.1453(5) 0.2810(3) 0.0755(19) Uani 1 1 d . . . H21A H 0.3041 0.0925 0.2417 0.113 Uiso 1 1 calc R . . H21B H 0.3011 0.1392 0.3176 0.113 Uiso 1 1 calc R . . H21C H 0.4464 0.1274 0.2865 0.113 Uiso 1 1 calc R . . C22 C 0.2866(5) 0.1938(4) 0.1667(2) 0.0461(11) Uani 1 1 d . . . C23 C 0.1413(6) 0.1487(5) 0.1495(3) 0.0618(15) Uani 1 1 d . . . C24 C 0.1021(8) 0.0603(6) 0.0908(4) 0.083(2) Uani 1 1 d . . . H24A H 0.0058 0.0297 0.0783 0.100 Uiso 1 1 calc R . . C25 C 0.1993(10) 0.0190(6) 0.0523(3) 0.089(2) Uani 1 1 d . . . H25A H 0.1699 -0.0378 0.0130 0.107 Uiso 1 1 calc R . . C26 C 0.3450(9) 0.0605(6) 0.0708(3) 0.083(2) Uani 1 1 d . . . H26A H 0.4119 0.0291 0.0444 0.100 Uiso 1 1 calc R . . C27 C 0.3904(6) 0.1488(5) 0.1286(3) 0.0552(13) Uani 1 1 d . . . C28 C 0.0287(6) 0.1854(6) 0.1930(4) 0.090(3) Uani 1 1 d . . . H28A H 0.0702 0.2574 0.2256 0.108 Uiso 1 1 calc R . . H28B H -0.0459 0.1998 0.1672 0.108 Uiso 1 1 calc R . . C29 C -0.0369(14) 0.1021(10) 0.2268(7) 0.192(7) Uani 1 1 d . . . H29A H -0.1080 0.1323 0.2535 0.287 Uiso 1 1 calc R . . H29B H 0.0353 0.0891 0.2537 0.287 Uiso 1 1 calc R . . H29C H -0.0806 0.0310 0.1951 0.287 Uiso 1 1 calc R . . C30 C 0.5466(6) 0.1853(6) 0.1500(3) 0.0729(18) Uani 1 1 d . . . H30A H 0.5679 0.2683 0.1679 0.088 Uiso 1 1 calc R . . H30B H 0.5628 0.1544 0.1856 0.088 Uiso 1 1 calc R . . C31 C 0.6520(9) 0.1540(8) 0.1024(4) 0.102(3) Uani 1 1 d . . . H31A H 0.7465 0.1822 0.1236 0.154 Uiso 1 1 calc R . . H31B H 0.6427 0.1875 0.0678 0.154 Uiso 1 1 calc R . . H31C H 0.6354 0.0720 0.0847 0.154 Uiso 1 1 calc R . . C32 C 0.1455(4) 0.4702(4) 0.2767(2) 0.0395(10) Uani 1 1 d . . . C33 C 0.1044(5) 0.4523(5) 0.3351(2) 0.0487(12) Uani 1 1 d . . . C34 C -0.0360(5) 0.4290(6) 0.3503(2) 0.0583(15) Uani 1 1 d . . . C35 C -0.1499(5) 0.4223(6) 0.3088(3) 0.0597(15) Uani 1 1 d . . . H35A H -0.2436 0.4074 0.3198 0.072 Uiso 1 1 calc R . . C36 C -0.1162(5) 0.4394(5) 0.2488(3) 0.0563(14) Uani 1 1 d . . . H36A H -0.1892 0.4353 0.2185 0.068 Uiso 1 1 calc R . . C37 C 0.0255(5) 0.4627(4) 0.2339(2) 0.0404(10) Uani 1 1 d . . . C38 C 0.1007(6) 0.4241(8) 0.4335(3) 0.091(3) Uani 1 1 d . . . H38A H 0.1240 0.4794 0.4763 0.109 Uiso 1 1 calc R . . H38B H 0.1129 0.3500 0.4365 0.109 Uiso 1 1 calc R . . C39 C 0.0607(5) 0.4794(4) 0.1718(2) 0.0433(11) Uani 1 1 d . . . C40 C -0.0555(6) 0.4781(6) 0.1230(3) 0.0640(17) Uani 1 1 d . . . H40A H -0.0138 0.4905 0.0846 0.096 Uiso 1 1 calc R . . H40B H -0.1060 0.5379 0.1419 0.096 Uiso 1 1 calc R . . H40C H -0.1207 0.4051 0.1114 0.096 Uiso 1 1 calc R . . C41 C 0.2388(5) 0.5369(4) 0.1051(2) 0.0423(11) Uani 1 1 d . . . C42 C 0.2699(5) 0.4607(5) 0.0482(2) 0.0453(11) Uani 1 1 d . . . C43 C 0.3221(6) 0.5069(5) -0.0014(2) 0.0532(13) Uani 1 1 d . . . H43A H 0.3460 0.4584 -0.0396 0.064 Uiso 1 1 calc R . . C44 C 0.3383(6) 0.6202(6) 0.0051(3) 0.0626(15) Uani 1 1 d . . . H44A H 0.3753 0.6493 -0.0280 0.075 Uiso 1 1 calc R . . C45 C 0.2996(7) 0.6929(5) 0.0608(3) 0.0664(16) Uani 1 1 d . . . H45A H 0.3078 0.7701 0.0639 0.080 Uiso 1 1 calc R . . C46 C 0.2491(7) 0.6543(5) 0.1122(3) 0.0571(14) Uani 1 1 d . . . C47 C 0.2474(6) 0.3344(5) 0.0378(2) 0.0556(13) Uani 1 1 d . . . H47A H 0.2367 0.3192 0.0796 0.067 Uiso 1 1 calc R . . H47B H 0.3308 0.3073 0.0198 0.067 Uiso 1 1 calc R . . C48 C 0.1143(9) 0.2677(7) -0.0086(4) 0.104(3) Uani 1 1 d . . . H48A H 0.1037 0.1871 -0.0140 0.156 Uiso 1 1 calc R . . H48B H 0.1252 0.2814 -0.0503 0.156 Uiso 1 1 calc R . . H48C H 0.0311 0.2932 0.0094 0.156 Uiso 1 1 calc R . . C49 C 0.2045(10) 0.7337(6) 0.1718(3) 0.086(2) Uani 1 1 d . . . H49A H 0.1229 0.6899 0.1860 0.103 Uiso 1 1 calc R . . H49B H 0.2814 0.7528 0.2056 0.103 Uiso 1 1 calc R . . C50 C 0.1688(15) 0.8359(8) 0.1707(5) 0.152(5) Uani 1 1 d . . . H50A H 0.1427 0.8745 0.2130 0.229 Uiso 1 1 calc R . . H50B H 0.0897 0.8203 0.1390 0.229 Uiso 1 1 calc R . . H50C H 0.2491 0.8838 0.1592 0.229 Uiso 1 1 calc R . . C97 C 0.023(4) 1.094(3) 0.419(2) 0.211(17) Uiso 0.50 1 d P A 1 H97D H -0.0259 1.0969 0.3804 0.317 Uiso 0.50 1 calc PR A 1 H97E H 0.1132 1.0736 0.4091 0.317 Uiso 0.50 1 calc PR A 1 H97F H 0.0375 1.1678 0.4514 0.317 Uiso 0.50 1 calc PR A 1 C97A C -0.048(4) 1.044(3) 0.4026(16) 0.177(12) Uiso 0.50 1 d P B 2 H97A H 0.0008 1.0988 0.3825 0.266 Uiso 0.50 1 calc PR B 2 H97B H -0.1420 1.0575 0.4114 0.266 Uiso 0.50 1 calc PR B 2 H97C H -0.0547 0.9678 0.3738 0.266 Uiso 0.50 1 calc PR B 2 C98A C 0.031(2) 1.0556(17) 0.4631(9) 0.100(5) Uiso 0.50 1 d P B 2 H98C H 0.1265 1.0469 0.4517 0.120 Uiso 0.50 1 calc PR B 2 H98D H 0.0394 1.1350 0.4889 0.120 Uiso 0.50 1 calc PR B 2 C98 C -0.067(3) 1.005(2) 0.4458(12) 0.129(7) Uiso 0.50 1 d P A 1 H98A H -0.1593 1.0245 0.4556 0.155 Uiso 0.50 1 calc PR A 1 H98B H -0.0836 0.9300 0.4132 0.155 Uiso 0.50 1 calc PR A 1 O9 O 0.0000 1.0000 0.5000 0.165(4) Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.02531(9) 0.04715(11) 0.02733(9) 0.00797(7) -0.00137(6) 0.01181(7) Cl1 0.0364(6) 0.0734(8) 0.0327(6) 0.0118(5) 0.0069(5) 0.0107(6) O1 0.088(3) 0.056(2) 0.060(3) 0.0001(19) -0.043(2) 0.008(2) O2 0.082(3) 0.086(3) 0.045(2) 0.007(2) -0.032(2) 0.012(2) O3 0.0381(18) 0.138(4) 0.0279(17) 0.031(2) 0.0047(14) 0.027(2) O4 0.044(2) 0.166(5) 0.043(2) 0.042(3) 0.0136(17) 0.032(3) N1 0.046(2) 0.054(2) 0.036(2) 0.0071(18) -0.0076(17) 0.0174(19) N2 0.0311(18) 0.045(2) 0.037(2) 0.0103(17) -0.0013(15) 0.0076(16) N3 0.0361(19) 0.054(2) 0.0255(18) 0.0083(16) -0.0029(15) 0.0157(17) C1 0.066(4) 0.048(3) 0.050(3) 0.003(2) -0.020(3) 0.016(3) C2 0.078(5) 0.060(4) 0.082(5) 0.010(4) -0.013(4) 0.002(3) C3 0.112(7) 0.055(4) 0.117(7) 0.009(4) -0.026(6) -0.003(4) C4 0.134(8) 0.049(4) 0.116(7) 0.000(5) -0.053(6) 0.018(5) C5 0.131(8) 0.071(5) 0.088(6) -0.017(4) -0.034(5) 0.047(5) C6 0.087(5) 0.058(4) 0.066(4) 0.000(3) -0.014(4) 0.031(3) C7 0.093(6) 0.071(5) 0.110(7) 0.023(5) 0.003(5) -0.015(4) C8 0.104(8) 0.104(7) 0.180(11) 0.018(7) 0.019(8) 0.004(6) C9 0.189(12) 0.123(9) 0.148(10) 0.063(8) 0.006(9) -0.046(8) C10 0.118(6) 0.093(5) 0.059(4) -0.015(4) 0.001(4) 0.059(5) C11 0.100(7) 0.117(7) 0.138(9) 0.001(6) 0.018(6) 0.048(6) C12 0.225(13) 0.126(8) 0.058(5) -0.011(5) 0.015(6) 0.071(8) C13 0.031(2) 0.056(3) 0.030(2) 0.011(2) 0.0020(17) 0.014(2) C14 0.045(3) 0.055(3) 0.032(2) 0.003(2) -0.006(2) 0.015(2) C15 0.045(3) 0.074(4) 0.030(2) 0.005(2) -0.006(2) 0.018(3) C16 0.054(3) 0.095(5) 0.031(3) 0.020(3) -0.001(2) 0.018(3) C17 0.049(3) 0.076(4) 0.036(3) 0.025(3) 0.005(2) 0.013(3) C18 0.034(2) 0.061(3) 0.029(2) 0.012(2) 0.0029(18) 0.013(2) C19 0.097(5) 0.078(5) 0.067(4) 0.002(4) -0.051(4) 0.004(4) C20 0.038(2) 0.047(3) 0.045(3) 0.018(2) 0.003(2) 0.007(2) C21 0.099(5) 0.060(4) 0.064(4) 0.025(3) -0.012(4) 0.000(4) C22 0.043(3) 0.049(3) 0.040(3) 0.010(2) -0.011(2) 0.002(2) C23 0.049(3) 0.050(3) 0.077(4) 0.017(3) -0.026(3) -0.006(2) C24 0.072(4) 0.072(4) 0.086(5) 0.014(4) -0.044(4) -0.012(4) C25 0.114(7) 0.075(5) 0.051(4) -0.002(3) -0.033(4) -0.010(5) C26 0.101(6) 0.078(5) 0.050(4) -0.004(3) 0.001(4) 0.004(4) C27 0.059(3) 0.052(3) 0.041(3) 0.000(2) -0.006(2) 0.001(3) C28 0.035(3) 0.065(4) 0.151(8) 0.012(4) -0.014(4) -0.002(3) C29 0.185(12) 0.124(9) 0.291(18) 0.086(11) 0.159(13) 0.042(8) C30 0.056(3) 0.070(4) 0.072(4) -0.011(3) 0.009(3) 0.011(3) C31 0.094(6) 0.118(7) 0.087(6) 0.006(5) 0.015(5) 0.038(5) C32 0.028(2) 0.061(3) 0.028(2) 0.004(2) 0.0015(17) 0.018(2) C33 0.032(2) 0.084(4) 0.030(2) 0.010(2) -0.0004(18) 0.023(2) C34 0.038(3) 0.109(5) 0.034(3) 0.022(3) 0.011(2) 0.029(3) C35 0.030(2) 0.108(5) 0.042(3) 0.020(3) 0.010(2) 0.018(3) C36 0.036(3) 0.090(4) 0.041(3) 0.013(3) -0.003(2) 0.020(3) C37 0.031(2) 0.059(3) 0.032(2) 0.009(2) -0.0030(18) 0.018(2) C38 0.043(3) 0.200(9) 0.042(3) 0.046(4) 0.011(3) 0.039(4) C39 0.035(2) 0.064(3) 0.033(2) 0.013(2) -0.0046(18) 0.019(2) C40 0.041(3) 0.121(5) 0.039(3) 0.032(3) -0.004(2) 0.025(3) C41 0.040(2) 0.056(3) 0.032(2) 0.013(2) -0.0046(19) 0.011(2) C42 0.040(2) 0.065(3) 0.028(2) 0.011(2) -0.0052(19) 0.009(2) C43 0.050(3) 0.076(4) 0.032(3) 0.015(2) -0.003(2) 0.011(3) C44 0.064(4) 0.086(4) 0.041(3) 0.031(3) 0.003(3) 0.003(3) C45 0.088(5) 0.061(4) 0.054(4) 0.026(3) -0.009(3) 0.012(3) C46 0.073(4) 0.066(4) 0.037(3) 0.016(2) -0.005(3) 0.024(3) C47 0.067(4) 0.061(3) 0.031(3) 0.006(2) -0.003(2) 0.007(3) C48 0.110(6) 0.083(5) 0.094(6) 0.013(4) -0.050(5) -0.020(5) C49 0.140(7) 0.080(5) 0.052(4) 0.019(3) 0.001(4) 0.061(5) C50 0.297(16) 0.095(6) 0.112(7) 0.054(6) 0.079(9) 0.112(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 1.783(4) . ? Ta1 C13 2.191(4) . ? Ta1 C32 2.243(4) . ? Ta1 N3 2.315(3) . ? Ta1 Cl1 2.3765(11) . ? Ta1 N2 2.513(4) . ? O1 C14 1.370(7) . ? O1 C19 1.419(6) . ? O2 C15 1.374(7) . ? O2 C19 1.429(8) . ? O3 C33 1.389(5) . ? O3 C38 1.408(7) . ? O4 C34 1.375(6) . ? O4 C38 1.421(7) . ? N1 C1 1.396(7) . ? N2 C20 1.283(6) . ? N2 C22 1.451(6) . ? N3 C39 1.299(6) . ? N3 C41 1.457(6) . ? C1 C2 1.400(10) . ? C1 C6 1.408(9) . ? C2 C3 1.373(10) . ? C2 C7 1.522(11) . ? C3 C4 1.373(13) . ? C4 C5 1.372(13) . ? C5 C6 1.392(10) . ? C6 C10 1.516(11) . ? C7 C8 1.522(13) . ? C7 C9 1.547(12) . ? C10 C12 1.531(11) . ? C10 C11 1.538(11) . ? C13 C14 1.387(7) . ? C13 C18 1.414(7) . ? C14 C15 1.388(7) . ? C15 C16 1.325(8) . ? C16 C17 1.393(8) . ? C17 C18 1.402(6) . ? C18 C20 1.476(7) . ? C20 C21 1.494(7) . ? C22 C23 1.397(7) . ? C22 C27 1.397(8) . ? C23 C24 1.402(9) . ? C23 C28 1.491(10) . ? C24 C25 1.333(11) . ? C25 C26 1.399(11) . ? C26 C27 1.395(8) . ? C27 C30 1.500(8) . ? C28 C29 1.480(13) . ? C30 C31 1.474(9) . ? C32 C33 1.385(7) . ? C32 C37 1.430(6) . ? C33 C34 1.385(7) . ? C34 C35 1.371(7) . ? C35 C36 1.396(7) . ? C36 C37 1.395(7) . ? C37 C39 1.443(7) . ? C39 C40 1.510(6) . ? C41 C42 1.391(7) . ? C41 C46 1.406(7) . ? C42 C43 1.405(7) . ? C42 C47 1.491(7) . ? C43 C44 1.352(8) . ? C44 C45 1.381(9) . ? C45 C46 1.383(8) . ? C46 C49 1.500(8) . ? C47 C48 1.543(8) . ? C49 C50 1.383(9) . ? C97 C98 1.52(4) . ? C97A C98A 1.45(4) . ? C98A O9 1.20(2) . ? C98 O9 1.34(3) . ? O9 C98A 1.20(2) 2_576 ? O9 C98 1.34(3) 2_576 ? 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 N1 Ta1 C13 93.53(18) . . ? N1 Ta1 C32 98.15(18) . . ? C13 Ta1 C32 93.66(16) . . ? N1 Ta1 N3 95.60(15) . . ? C13 Ta1 N3 163.11(15) . . ? C32 Ta1 N3 71.01(15) . . ? N1 Ta1 Cl1 102.25(14) . . ? C13 Ta1 Cl1 103.45(11) . . ? C32 Ta1 Cl1 152.33(12) . . ? N3 Ta1 Cl1 88.46(9) . . ? N1 Ta1 N2 163.58(15) . . ? C13 Ta1 N2 70.10(15) . . ? C32 Ta1 N2 82.05(15) . . ? N3 Ta1 N2 99.94(13) . . ? Cl1 Ta1 N2 83.56(9) . . ? C14 O1 C19 106.5(5) . . ? C15 O2 C19 105.7(4) . . ? C33 O3 C38 106.2(4) . . ? C34 O4 C38 104.9(4) . . ? C1 N1 Ta1 173.4(3) . . ? C20 N2 C22 117.6(4) . . ? C20 N2 Ta1 113.9(3) . . ? C22 N2 Ta1 128.4(3) . . ? C39 N3 C41 119.5(4) . . ? C39 N3 Ta1 118.9(3) . . ? C41 N3 Ta1 120.2(3) . . ? N1 C1 C2 120.3(6) . . ? N1 C1 C6 119.5(6) . . ? C2 C1 C6 120.2(6) . . ? C3 C2 C1 119.0(8) . . ? C3 C2 C7 120.9(8) . . ? C1 C2 C7 120.1(6) . . ? C4 C3 C2 121.7(9) . . ? C5 C4 C3 119.6(8) . . ? C4 C5 C6 121.3(9) . . ? C5 C6 C1 118.2(8) . . ? C5 C6 C10 121.0(7) . . ? C1 C6 C10 120.8(6) . . ? C2 C7 C8 106.9(8) . . ? C2 C7 C9 114.1(8) . . ? C8 C7 C9 112.2(9) . . ? C6 C10 C12 115.8(8) . . ? C6 C10 C11 110.8(7) . . ? C12 C10 C11 110.8(8) . . ? C14 C13 C18 112.7(4) . . ? C14 C13 Ta1 127.2(4) . . ? C18 C13 Ta1 120.1(3) . . ? O1 C14 C13 126.7(4) . . ? O1 C14 C15 109.2(4) . . ? C13 C14 C15 124.1(5) . . ? C16 C15 O2 127.5(5) . . ? C16 C15 C14 122.8(5) . . ? O2 C15 C14 109.6(5) . . ? C15 C16 C17 116.5(5) . . ? C16 C17 C18 121.4(5) . . ? C17 C18 C13 122.3(5) . . ? C17 C18 C20 120.3(5) . . ? C13 C18 C20 117.3(4) . . ? O1 C19 O2 107.7(5) . . ? N2 C20 C18 117.3(4) . . ? N2 C20 C21 123.3(5) . . ? C18 C20 C21 119.3(4) . . ? C23 C22 C27 121.3(5) . . ? C23 C22 N2 120.8(5) . . ? C27 C22 N2 117.9(4) . . ? C22 C23 C24 117.9(6) . . ? C22 C23 C28 122.5(5) . . ? C24 C23 C28 119.4(6) . . ? C25 C24 C23 121.7(6) . . ? C24 C25 C26 120.5(6) . . ? C27 C26 C25 120.2(7) . . ? C26 C27 C22 118.1(6) . . ? C26 C27 C30 119.3(6) . . ? C22 C27 C30 122.4(5) . . ? C29 C28 C23 114.9(7) . . ? C31 C30 C27 119.5(6) . . ? C33 C32 C37 112.0(4) . . ? C33 C32 Ta1 130.2(3) . . ? C37 C32 Ta1 117.7(3) . . ? C34 C33 C32 124.3(4) . . ? C34 C33 O3 108.1(4) . . ? C32 C33 O3 127.6(4) . . ? C35 C34 O4 126.1(5) . . ? C35 C34 C33 123.0(5) . . ? O4 C34 C33 110.8(4) . . ? C34 C35 C36 115.8(5) . . ? C37 C36 C35 120.7(5) . . ? C36 C37 C32 124.2(4) . . ? C36 C37 C39 120.9(4) . . ? C32 C37 C39 114.9(4) . . ? O3 C38 O4 109.1(5) . . ? N3 C39 C37 117.4(4) . . ? N3 C39 C40 122.2(4) . . ? C37 C39 C40 120.4(4) . . ? C42 C41 C46 122.4(5) . . ? C42 C41 N3 119.9(4) . . ? C46 C41 N3 117.6(4) . . ? C41 C42 C43 117.2(5) . . ? C41 C42 C47 123.0(4) . . ? C43 C42 C47 119.8(5) . . ? C44 C43 C42 121.6(5) . . ? C43 C44 C45 119.9(5) . . ? C44 C45 C46 122.0(6) . . ? C45 C46 C41 116.8(5) . . ? C45 C46 C49 121.3(6) . . ? C41 C46 C49 121.9(5) . . ? C42 C47 C48 112.1(5) . . ? C50 C49 C46 121.6(6) . . ? O9 C98A C97A 127(3) . . ? O9 C98 C97 110(3) . . ? C98A O9 C98A 180.0(15) . 2_576 ? C98A O9 C98 47.1(12) . . ? C98A O9 C98 132.9(12) 2_576 . ? C98A O9 C98 132.9(12) . 2_576 ? C98A O9 C98 47.1(12) 2_576 2_576 ? C98 O9 C98 180.000(12) . 2_576 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.659 _refine_diff_density_min -1.672 _refine_diff_density_rms 0.118