# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 894039' #TrackingRef '12900_web_deposit_cif_file_0_LidijaAndros_1343389594.ccdc_deposit1.cif' _audit_creation_date 2012-05-24T16:43:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_formula_sum 'C56 H46 N8 Ni O22.50 Ta' _chemical_formula_weight 1430.67 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0511(4) _cell_length_b 14.9625(5) _cell_length_c 16.2348(5) _cell_angle_alpha 76.487(3) _cell_angle_beta 86.836(3) _cell_angle_gamma 72.440(3) _cell_volume 2713.33(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16714 _cell_measurement_theta_min 3.7371 _cell_measurement_theta_max 32.6271 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_description polyhedron _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1438 _exptl_special_details ? #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.457 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.86511 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.3426 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_ub_11 -0.0188867663 _diffrn_orient_matrix_ub_12 0.0405181828 _diffrn_orient_matrix_ub_13 0.0184622843 _diffrn_orient_matrix_ub_21 0.0345983218 _diffrn_orient_matrix_ub_22 -0.0267855273 _diffrn_orient_matrix_ub_23 0.0367063281 _diffrn_orient_matrix_ub_31 0.0476515942 _diffrn_orient_matrix_ub_32 0.0158032193 _diffrn_orient_matrix_ub_33 -0.0181752462 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_number 29028 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.965 _reflns_number_total 15253 _reflns_number_gt 12398 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0228P)^2^+23.7529P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 15253 _refine_ls_number_parameters 826 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.746 _refine_diff_density_min -2.344 _refine_diff_density_rms 0.16 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1960(5) 0.6904(4) 0.9143(4) 0.0226(12) Uani 1 1 d . . . H1 H 0.2157 0.748 0.9114 0.027 Uiso 1 1 calc R . . C2 C 0.2675(5) 0.6039(5) 0.9618(4) 0.0255(12) Uani 1 1 d . . . H2 H 0.3339 0.6032 0.9912 0.031 Uiso 1 1 calc R . . C3 C 0.2418(5) 0.5207(5) 0.9659(4) 0.0254(12) Uani 1 1 d . . . H3 H 0.2912 0.4614 0.9969 0.031 Uiso 1 1 calc R . . C4 C 0.1409(5) 0.5227(4) 0.9237(4) 0.0227(11) Uani 1 1 d . . . C5 C 0.1045(6) 0.4397(4) 0.9262(4) 0.0299(14) Uani 1 1 d . . . H5 H 0.1524 0.378 0.9541 0.036 Uiso 1 1 calc R . . C6 C 0.0022(6) 0.4476(5) 0.8893(4) 0.0301(14) Uani 1 1 d . . . H6 H -0.0205 0.3914 0.8919 0.036 Uiso 1 1 calc R . . C7 C -0.0714(5) 0.5394(4) 0.8468(4) 0.0227(12) Uani 1 1 d . . . C8 C -0.1817(5) 0.5534(5) 0.8111(4) 0.0276(13) Uani 1 1 d . . . H8 H -0.2115 0.5005 0.8161 0.033 Uiso 1 1 calc R . . C9 C -0.2443(5) 0.6427(5) 0.7699(4) 0.0289(13) Uani 1 1 d . . . H9 H -0.3191 0.653 0.7468 0.035 Uiso 1 1 calc R . . C10 C -0.1987(5) 0.7193(5) 0.7614(4) 0.0259(12) Uani 1 1 d . . . H10 H -0.2428 0.7807 0.73 0.031 Uiso 1 1 calc R . . C11 C -0.0338(5) 0.6209(4) 0.8386(3) 0.0191(11) Uani 1 1 d . . . C12 C 0.0726(5) 0.6127(4) 0.8790(3) 0.0177(10) Uani 1 1 d . . . C22 C 0.1945(6) 0.7164(5) 0.6808(4) 0.0310(14) Uani 1 1 d . . . H22 H 0.2334 0.6802 0.7328 0.037 Uiso 1 1 calc R . . C21 C 0.2513(7) 0.7037(6) 0.6050(5) 0.0413(18) Uani 1 1 d . . . H21 H 0.3279 0.6611 0.6058 0.05 Uiso 1 1 calc R . . C20 C 0.1955(8) 0.7531(6) 0.5302(5) 0.045(2) Uani 1 1 d . . . H20 H 0.2326 0.7442 0.4783 0.054 Uiso 1 1 calc R . . C19 C 0.0824(8) 0.8176(6) 0.5295(4) 0.0411(19) Uani 1 1 d . . . C18 C 0.0185(10) 0.8712(7) 0.4555(5) 0.056(3) Uani 1 1 d . . . H18 H 0.0506 0.8628 0.402 0.068 Uiso 1 1 calc R . . C17 C -0.0882(11) 0.9346(7) 0.4583(5) 0.063(3) Uani 1 1 d . . . H17 H -0.1304 0.9685 0.4071 0.076 Uiso 1 1 calc R . . C16 C -0.1382(8) 0.9513(6) 0.5370(5) 0.051(2) Uani 1 1 d . . . C15 C -0.2450(8) 1.0223(6) 0.5453(6) 0.058(3) Uani 1 1 d . . . H15 H -0.2895 1.0612 0.4963 0.07 Uiso 1 1 calc R . . C14 C -0.2821(7) 1.0341(6) 0.6212(7) 0.056(3) Uani 1 1 d . . . H14 H -0.3538 1.0811 0.6266 0.068 Uiso 1 1 calc R . . C13 C -0.2168(6) 0.9779(5) 0.6938(5) 0.0398(18) Uani 1 1 d . . . H13 H -0.2453 0.988 0.7476 0.048 Uiso 1 1 calc R . . C23 C -0.0765(6) 0.8971(5) 0.6124(4) 0.0326(15) Uani 1 1 d . . . C24 C 0.0335(6) 0.8285(5) 0.6085(4) 0.0313(15) Uani 1 1 d . . . C25 C 0.1744(5) 0.9277(5) 0.7600(4) 0.0278(13) Uani 1 1 d . . . H25 H 0.2178 0.8838 0.7277 0.033 Uiso 1 1 calc R . . C26 C 0.2151(6) 1.0044(5) 0.7660(4) 0.0364(17) Uani 1 1 d . . . H26 H 0.2848 1.0112 0.7386 0.044 Uiso 1 1 calc R . . C27 C 0.1547(6) 1.0690(5) 0.8109(5) 0.0365(17) Uani 1 1 d . . . H27 H 0.1816 1.1212 0.8155 0.044 Uiso 1 1 calc R . . C28 C 0.0503(6) 1.0573(4) 0.8508(5) 0.0327(15) Uani 1 1 d . . . C29 C -0.0202(6) 1.1212(5) 0.9002(6) 0.043(2) Uani 1 1 d . . . H29 H 0.001 1.1758 0.9055 0.052 Uiso 1 1 calc R . . C30 C -0.1157(6) 1.1041(5) 0.9390(6) 0.045(2) Uani 1 1 d . . . H30 H -0.162 1.148 0.9702 0.053 Uiso 1 1 calc R . . C31 C -0.1493(6) 1.0211(5) 0.9343(5) 0.0347(15) Uani 1 1 d . . . C32 C -0.2454(6) 0.9983(6) 0.9769(5) 0.0401(17) Uani 1 1 d . . . H32 H -0.2934 1.0391 1.01 0.048 Uiso 1 1 calc R . . C33 C -0.2684(6) 0.9166(6) 0.9699(5) 0.0394(17) Uani 1 1 d . . . H33 H -0.3328 0.9 0.9986 0.047 Uiso 1 1 calc R . . C34 C -0.1971(5) 0.8568(5) 0.9204(4) 0.0302(14) Uani 1 1 d . . . H34 H -0.2141 0.7999 0.9165 0.036 Uiso 1 1 calc R . . C35 C -0.0826(5) 0.9588(4) 0.8857(4) 0.0253(12) Uani 1 1 d . . . C36 C 0.0175(5) 0.9772(4) 0.8432(4) 0.0253(13) Uani 1 1 d . . . C37 C 0.6509(10) 0.5180(14) 0.5450(8) 0.143(8) Uani 1 1 d . . . H37 H 0.5941 0.5309 0.5871 0.171 Uiso 1 1 calc R . . C38 C 0.6187(12) 0.5617(14) 0.4599(8) 0.135(7) Uani 1 1 d . . . H38 H 0.5409 0.6001 0.4448 0.162 Uiso 1 1 calc R . . C39 C 0.6992(10) 0.5483(8) 0.4003(6) 0.074(3) Uani 1 1 d . . . H39 H 0.6784 0.5766 0.3424 0.089 Uiso 1 1 calc R . . C40 C 0.8121(9) 0.4937(6) 0.4224(5) 0.051(2) Uani 1 1 d . . . C41 C 0.9038(11) 0.4781(7) 0.3640(5) 0.059(3) Uani 1 1 d . . . H41 H 0.8883 0.5092 0.3059 0.071 Uiso 1 1 calc R . . C42 C 1.0106(11) 0.4215(8) 0.3876(5) 0.065(3) Uani 1 1 d . . . H42 H 1.0694 0.4132 0.3462 0.078 Uiso 1 1 calc R . . C43 C 1.0397(9) 0.3708(6) 0.4777(5) 0.047(2) Uani 1 1 d . . . C44 C 1.1478(10) 0.3122(7) 0.5056(7) 0.066(3) Uani 1 1 d . . . H44 H 1.2093 0.3025 0.4663 0.079 Uiso 1 1 calc R . . C45 C 1.1693(8) 0.2668(6) 0.5902(7) 0.055(2) Uani 1 1 d . . . H45 H 1.2441 0.2248 0.6096 0.066 Uiso 1 1 calc R . . C46 C 1.0785(6) 0.2846(5) 0.6457(5) 0.0390(17) Uani 1 1 d . . . H46 H 1.0909 0.2559 0.7044 0.047 Uiso 1 1 calc R . . C47 C 0.9518(7) 0.3868(5) 0.5339(4) 0.0355(16) Uani 1 1 d . . . C48 C 0.8373(7) 0.4462(6) 0.5093(5) 0.045(2) Uani 1 1 d . . . C49 C 0.4898(6) 0.4850(5) 1.2399(4) 0.0344(16) Uani 1 1 d . . . C50 C 0.4898(5) 0.4840(5) 1.1465(4) 0.0279(13) Uani 1 1 d . . . C51 C 0.5580(5) 0.7383(4) 0.9748(4) 0.0224(11) Uani 1 1 d . . . C52 C 0.4245(5) 0.7781(4) 0.9658(4) 0.0198(11) Uani 1 1 d . . . C53 C 0.5719(6) 0.8357(5) 1.1548(4) 0.0339(15) Uani 1 1 d . . . C54 C 0.6578(6) 0.7392(5) 1.1965(5) 0.0382(17) Uani 1 1 d . . . C55 C 0.2707(7) 0.7403(5) 1.2656(4) 0.0360(16) Uani 1 1 d . . . C56 C 0.2281(6) 0.6807(5) 1.2154(4) 0.0261(13) Uani 1 1 d . . . N1 N 0.1013(4) 0.6954(3) 0.8728(3) 0.0179(9) Uani 1 1 d . . . N2 N -0.0957(4) 0.7116(3) 0.7951(3) 0.0186(9) Uani 1 1 d . . . N4 N 0.0887(4) 0.7771(4) 0.6832(3) 0.0252(11) Uani 1 1 d . . . N3 N -0.1163(5) 0.9107(4) 0.6901(4) 0.0300(12) Uani 1 1 d . . . N5 N 0.0786(4) 0.9131(4) 0.7971(3) 0.0232(10) Uani 1 1 d . . . N6 N -0.1072(4) 0.8778(4) 0.8791(3) 0.0243(10) Uani 1 1 d . . . N7 N 0.7571(7) 0.4593(9) 0.5703(5) 0.092(4) Uani 1 1 d . . . N8 N 0.9744(5) 0.3416(4) 0.6172(4) 0.0330(13) Uani 1 1 d . . . H8A H 0.9173 0.3506 0.6535 0.04 Uiso 1 1 calc R . . O1 O 0.4819(4) 0.5685(3) 1.2541(3) 0.0316(10) Uani 1 1 d . . . O2 O 0.4957(4) 0.5657(3) 1.0998(3) 0.0252(9) Uani 1 1 d . . . O3 O 0.4844(5) 0.4158(4) 1.1228(3) 0.0393(12) Uani 1 1 d . . . O4 O 0.4998(6) 0.4118(4) 1.2956(3) 0.0511(15) Uani 1 1 d . . . O5 O 0.5910(3) 0.6938(3) 1.0510(3) 0.0278(9) Uani 1 1 d . . . O6 O 0.3718(3) 0.7564(3) 1.0363(2) 0.0210(8) Uani 1 1 d . . . O7 O 0.6190(4) 0.7516(3) 0.9141(3) 0.0350(11) Uani 1 1 d . . . O8 O 0.3747(4) 0.8253(3) 0.8992(3) 0.0306(10) Uani 1 1 d . . . O9 O 0.4800(4) 0.8276(3) 1.1256(3) 0.0290(10) Uani 1 1 d . . . O10 O 0.6103(4) 0.6698(3) 1.2095(3) 0.0358(11) Uani 1 1 d . . . O11 O 0.7569(5) 0.7305(4) 1.2158(4) 0.0562(17) Uani 1 1 d . . . O12 O 0.5920(5) 0.9131(4) 1.1527(3) 0.0411(12) Uani 1 1 d . . . O13 O 0.2973(4) 0.6575(3) 1.1565(3) 0.0244(9) Uani 1 1 d . . . O14 O 0.3691(4) 0.7529(4) 1.2374(3) 0.0357(11) Uani 1 1 d . . . O15 O 0.2150(6) 0.7713(5) 1.3225(4) 0.065(2) Uani 1 1 d . . . O16 O 0.1365(4) 0.6607(3) 1.2320(3) 0.0297(10) Uani 1 1 d . . . O17 O 0.4242(5) 0.7692(4) 0.7424(3) 0.0400(12) Uani 1 1 d D . . O18 O 0.5608(5) 0.9337(5) 0.7929(4) 0.0496(14) Uani 1 1 d D . . Ni1 Ni -0.00751(6) 0.81304(5) 0.78900(5) 0.01935(15) Uani 1 1 d . . . Ta1 Ta 0.46193(2) 0.686457(19) 1.146979(16) 0.02155(7) Uani 1 1 d . . . O19A O 0.5 1 0.5 0.030(4) Uani 0.5 2 d SP . . O19B O 0.5420(17) 0.943(2) 0.4940(13) 0.066(10) Uani 0.25 1 d P . . O23 O 0.5110(14) 0.7661(10) 0.3771(10) 0.077(4) Uani 0.5 1 d P . . O24 O 0.5560(17) 0.8556(14) 0.5700(12) 0.098(5) Uiso 0.5 1 d P . . O20A O 0.5726(11) 0.9279(9) 0.3557(8) 0.055(2) Uiso 0.510(10) 1 d P . . O20B O 0.6072(11) 0.8996(9) 0.4261(9) 0.055(2) Uiso 0.490(10) 1 d P . . O21A O 0.4538(9) 0.8747(8) 0.6088(7) 0.0336(18) Uiso 0.462(10) 1 d P . . O21B O 0.5501(10) 0.8789(8) 0.6564(7) 0.0336(18) Uiso 0.424(10) 1 d P . . O21C O 0.448(3) 0.840(3) 0.562(2) 0.0336(18) Uiso 0.125(10) 1 d P . . O22B O 0.6455(12) 0.7904(10) 0.6008(9) 0.074(3) Uiso 0.560(11) 1 d P . . O22A O 0.5565(15) 0.7254(12) 0.5555(11) 0.074(3) Uiso 0.440(11) 1 d P . . H17A H 0.471(9) 0.709(4) 0.748(7) 0.111 Uiso 1 1 d D . . H17B H 0.413(10) 0.786(8) 0.793(4) 0.111 Uiso 1 1 d D . . H18A H 0.515(9) 0.977(6) 0.821(7) 0.111 Uiso 1 1 d D . . H18B H 0.558(10) 0.873(3) 0.815(7) 0.111 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(3) 0.026(3) 0.024(3) -0.005(2) -0.004(2) -0.011(2) C2 0.020(3) 0.031(3) 0.023(3) -0.005(2) -0.002(2) -0.005(2) C3 0.024(3) 0.026(3) 0.022(3) -0.005(2) -0.002(2) -0.001(2) C4 0.022(3) 0.023(3) 0.021(3) -0.006(2) 0.004(2) -0.003(2) C5 0.036(3) 0.017(3) 0.035(3) -0.005(2) 0.004(3) -0.007(3) C6 0.037(4) 0.021(3) 0.035(3) -0.008(3) 0.004(3) -0.013(3) C7 0.023(3) 0.025(3) 0.024(3) -0.011(2) 0.008(2) -0.011(2) C8 0.023(3) 0.032(3) 0.036(3) -0.015(3) 0.008(3) -0.015(3) C9 0.025(3) 0.035(4) 0.032(3) -0.010(3) -0.001(3) -0.015(3) C10 0.021(3) 0.033(3) 0.026(3) -0.005(2) -0.004(2) -0.011(3) C11 0.017(2) 0.023(3) 0.019(2) -0.006(2) 0.004(2) -0.007(2) C12 0.021(3) 0.014(3) 0.020(3) -0.007(2) 0.001(2) -0.006(2) C22 0.034(3) 0.040(4) 0.026(3) -0.012(3) 0.003(3) -0.018(3) C21 0.044(4) 0.057(5) 0.039(4) -0.024(4) 0.015(3) -0.032(4) C20 0.065(5) 0.069(5) 0.029(4) -0.026(4) 0.020(3) -0.052(5) C19 0.067(5) 0.051(5) 0.028(3) -0.016(3) 0.007(3) -0.047(4) C18 0.096(8) 0.066(6) 0.028(4) 0.001(4) -0.005(4) -0.063(6) C17 0.110(8) 0.072(6) 0.026(4) 0.014(4) -0.030(5) -0.067(7) C16 0.062(5) 0.050(5) 0.045(4) 0.024(4) -0.035(4) -0.043(4) C15 0.059(5) 0.048(5) 0.064(6) 0.032(4) -0.043(5) -0.037(4) C14 0.034(4) 0.040(5) 0.084(7) 0.024(4) -0.030(4) -0.017(4) C13 0.024(3) 0.033(4) 0.055(5) 0.010(3) -0.010(3) -0.011(3) C23 0.040(4) 0.034(4) 0.030(3) 0.006(3) -0.015(3) -0.027(3) C24 0.045(4) 0.037(4) 0.021(3) -0.001(3) -0.006(3) -0.029(3) C25 0.026(3) 0.033(3) 0.023(3) 0.005(2) -0.004(2) -0.016(3) C26 0.035(4) 0.041(4) 0.034(4) 0.009(3) -0.012(3) -0.024(3) C27 0.036(4) 0.024(3) 0.050(4) 0.006(3) -0.020(3) -0.017(3) C28 0.026(3) 0.018(3) 0.052(4) -0.002(3) -0.017(3) -0.004(3) C29 0.036(4) 0.018(3) 0.077(6) -0.017(3) -0.022(4) -0.002(3) C30 0.028(3) 0.030(4) 0.077(6) -0.031(4) -0.012(4) 0.005(3) C31 0.024(3) 0.027(3) 0.052(4) -0.015(3) -0.009(3) 0.000(3) C32 0.027(3) 0.040(4) 0.053(5) -0.025(4) -0.003(3) 0.002(3) C33 0.028(3) 0.049(5) 0.043(4) -0.017(3) 0.007(3) -0.011(3) C34 0.026(3) 0.034(4) 0.034(3) -0.012(3) 0.002(3) -0.012(3) C35 0.019(3) 0.020(3) 0.037(3) -0.009(2) -0.007(2) -0.001(2) C36 0.023(3) 0.011(3) 0.039(3) 0.000(2) -0.012(2) -0.004(2) C37 0.041(6) 0.25(2) 0.057(7) 0.051(10) -0.005(5) 0.004(9) C38 0.066(8) 0.24(2) 0.053(7) 0.024(10) -0.024(6) -0.013(10) C39 0.089(8) 0.091(8) 0.035(5) 0.020(5) -0.030(5) -0.036(7) C40 0.078(6) 0.052(5) 0.032(4) 0.003(3) -0.012(4) -0.041(5) C41 0.117(9) 0.058(6) 0.022(4) -0.007(4) 0.000(5) -0.057(6) C42 0.111(9) 0.073(7) 0.029(4) -0.020(4) 0.032(5) -0.053(7) C43 0.085(6) 0.036(4) 0.035(4) -0.021(3) 0.011(4) -0.031(4) C44 0.081(7) 0.056(6) 0.068(7) -0.036(5) 0.039(6) -0.023(6) C45 0.046(5) 0.039(5) 0.087(7) -0.028(5) 0.009(5) -0.014(4) C46 0.040(4) 0.036(4) 0.047(4) -0.008(3) -0.005(3) -0.021(3) C47 0.053(4) 0.039(4) 0.026(3) -0.006(3) 0.001(3) -0.033(4) C48 0.055(5) 0.058(5) 0.026(3) 0.006(3) -0.009(3) -0.032(4) C49 0.036(4) 0.032(4) 0.035(4) 0.006(3) -0.016(3) -0.016(3) C50 0.022(3) 0.030(3) 0.033(3) 0.002(3) -0.001(2) -0.016(3) C51 0.019(3) 0.018(3) 0.033(3) -0.007(2) 0.001(2) -0.007(2) C52 0.020(3) 0.017(3) 0.023(3) -0.003(2) 0.000(2) -0.008(2) C53 0.043(4) 0.040(4) 0.023(3) 0.004(3) -0.003(3) -0.027(3) C54 0.040(4) 0.040(4) 0.040(4) 0.001(3) -0.014(3) -0.024(3) C55 0.048(4) 0.045(4) 0.027(3) -0.009(3) 0.007(3) -0.031(4) C56 0.034(3) 0.029(3) 0.016(3) 0.001(2) -0.003(2) -0.014(3) N1 0.018(2) 0.019(2) 0.019(2) -0.0047(17) -0.0006(17) -0.0070(18) N2 0.015(2) 0.026(3) 0.016(2) -0.0075(18) 0.0003(17) -0.0048(19) N4 0.028(3) 0.033(3) 0.020(2) -0.004(2) -0.001(2) -0.019(2) N3 0.028(3) 0.027(3) 0.034(3) 0.008(2) -0.013(2) -0.016(2) N5 0.024(2) 0.020(2) 0.025(2) 0.0013(19) -0.007(2) -0.010(2) N6 0.020(2) 0.021(3) 0.032(3) -0.006(2) -0.003(2) -0.007(2) N7 0.034(4) 0.170(10) 0.033(4) 0.025(5) -0.004(3) -0.007(5) N8 0.032(3) 0.042(3) 0.030(3) -0.005(2) 0.001(2) -0.021(3) O1 0.042(3) 0.029(2) 0.028(2) 0.0033(18) -0.012(2) -0.021(2) O2 0.024(2) 0.019(2) 0.031(2) 0.0008(17) -0.0003(17) -0.0099(17) O3 0.048(3) 0.032(3) 0.044(3) -0.007(2) 0.004(2) -0.022(2) O4 0.082(4) 0.033(3) 0.038(3) 0.012(2) -0.015(3) -0.030(3) O5 0.0166(19) 0.023(2) 0.039(3) 0.0022(18) -0.0031(18) -0.0043(17) O6 0.0174(18) 0.023(2) 0.0198(19) -0.0031(15) -0.0011(15) -0.0035(16) O7 0.024(2) 0.038(3) 0.048(3) -0.018(2) 0.018(2) -0.015(2) O8 0.032(2) 0.033(2) 0.023(2) 0.0020(18) -0.0047(18) -0.010(2) O9 0.033(2) 0.025(2) 0.030(2) -0.0018(18) -0.0020(19) -0.0142(19) O10 0.038(3) 0.033(3) 0.036(3) 0.010(2) -0.019(2) -0.020(2) O11 0.042(3) 0.058(4) 0.070(4) 0.008(3) -0.025(3) -0.030(3) O12 0.047(3) 0.035(3) 0.051(3) -0.009(2) 0.000(2) -0.027(2) O13 0.026(2) 0.031(2) 0.021(2) -0.0071(17) -0.0001(16) -0.0156(19) O14 0.043(3) 0.046(3) 0.031(2) -0.013(2) 0.005(2) -0.029(2) O15 0.090(5) 0.103(5) 0.043(3) -0.048(4) 0.038(3) -0.072(4) O16 0.031(2) 0.036(3) 0.026(2) -0.0050(19) 0.0050(18) -0.017(2) O17 0.045(3) 0.030(3) 0.041(3) -0.003(2) 0.002(2) -0.009(2) O18 0.053(3) 0.055(4) 0.045(3) -0.010(3) 0.018(3) -0.026(3) Ni1 0.0191(3) 0.0188(4) 0.0206(3) -0.0015(3) -0.0026(3) -0.0081(3) Ta1 0.02319(12) 0.02233(12) 0.02027(11) 0.00195(8) -0.00622(8) -0.01247(9) O19A 0.010(6) 0.017(7) 0.073(12) -0.043(8) 0.005(7) 0.007(5) O19B 0.023(11) 0.11(2) 0.042(13) 0.076(14) -0.045(10) -0.052(14) O23 0.090(11) 0.054(8) 0.084(11) -0.018(7) -0.030(9) -0.010(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.331(7) . ? C1 C2 1.396(8) . ? C1 H1 0.95 . ? C2 C3 1.357(9) . ? C2 H2 0.95 . ? C3 C4 1.417(8) . ? C3 H3 0.95 . ? C4 C12 1.399(8) . ? C4 C5 1.429(8) . ? C5 C6 1.362(9) . ? C5 H5 0.95 . ? C6 C7 1.428(9) . ? C6 H6 0.95 . ? C7 C11 1.401(8) . ? C7 C8 1.416(8) . ? C8 C9 1.354(9) . ? C8 H8 0.95 . ? C9 C10 1.390(8) . ? C9 H9 0.95 . ? C10 N2 1.346(7) . ? C10 H10 0.95 . ? C11 N2 1.376(7) . ? C11 C12 1.432(7) . ? C12 N1 1.362(7) . ? C22 N4 1.328(9) . ? C22 C21 1.399(9) . ? C22 H22 0.95 . ? C21 C20 1.358(11) . ? C21 H21 0.95 . ? C20 C19 1.412(12) . ? C20 H20 0.95 . ? C19 C18 1.399(12) . ? C19 C24 1.405(10) . ? C18 C17 1.354(15) . ? C18 H18 0.95 . ? C17 C16 1.424(14) . ? C17 H17 0.95 . ? C16 C23 1.408(9) . ? C16 C15 1.423(14) . ? C15 C14 1.320(14) . ? C15 H15 0.95 . ? C14 C13 1.398(10) . ? C14 H14 0.95 . ? C13 N3 1.330(9) . ? C13 H13 0.95 . ? C23 N3 1.363(9) . ? C23 C24 1.420(11) . ? C24 N4 1.360(8) . ? C25 N5 1.326(8) . ? C25 C26 1.401(9) . ? C25 H25 0.95 . ? C26 C27 1.358(11) . ? C26 H26 0.95 . ? C27 C28 1.422(10) . ? C27 H27 0.95 . ? C28 C36 1.402(8) . ? C28 C29 1.439(11) . ? C29 C30 1.345(11) . ? C29 H29 0.95 . ? C30 C31 1.437(10) . ? C30 H30 0.95 . ? C31 C35 1.401(9) . ? C31 C32 1.405(11) . ? C32 C33 1.362(10) . ? C32 H32 0.95 . ? C33 C34 1.407(10) . ? C33 H33 0.95 . ? C34 N6 1.322(8) . ? C34 H34 0.95 . ? C35 N6 1.359(7) . ? C35 C36 1.424(9) . ? C36 N5 1.368(8) . ? C37 N7 1.337(13) . ? C37 C38 1.405(15) . ? C37 H37 0.95 . ? C38 C39 1.336(17) . ? C38 H38 0.95 . ? C39 C40 1.377(14) . ? C39 H39 0.95 . ? C40 C41 1.416(14) . ? C40 C48 1.426(10) . ? C41 C42 1.329(15) . ? C41 H41 0.95 . ? C42 C43 1.488(12) . ? C42 H42 0.95 . ? C43 C47 1.362(11) . ? C43 C44 1.364(14) . ? C44 C45 1.383(14) . ? C44 H44 0.95 . ? C45 C46 1.381(12) . ? C45 H45 0.95 . ? C46 N8 1.322(9) . ? C46 H46 0.95 . ? C47 N8 1.365(8) . ? C47 C48 1.417(11) . ? C48 N7 1.350(11) . ? C49 O4 1.226(8) . ? C49 O1 1.298(8) . ? C49 C50 1.520(10) . ? C50 O3 1.192(8) . ? C50 O2 1.299(7) . ? C51 O7 1.211(7) . ? C51 O5 1.281(7) . ? C51 C52 1.540(8) . ? C52 O8 1.219(7) . ? C52 O6 1.301(7) . ? C53 O12 1.245(8) . ? C53 O9 1.277(8) . ? C53 C54 1.528(10) . ? C54 O11 1.212(8) . ? C54 O10 1.302(8) . ? C55 O15 1.210(9) . ? C55 O14 1.299(8) . ? C55 C56 1.544(9) . ? C56 O16 1.229(7) . ? C56 O13 1.274(7) . ? N1 Ni1 2.087(5) . ? N2 Ni1 2.083(5) . ? N4 Ni1 2.103(5) . ? N3 Ni1 2.100(5) . ? N5 Ni1 2.093(5) . ? N6 Ni1 2.071(5) . ? N8 H8A 0.88 . ? O1 Ta1 2.134(4) . ? O2 Ta1 2.046(4) . ? O5 Ta1 2.148(4) . ? O6 Ta1 2.038(4) . ? O9 Ta1 2.134(4) . ? O10 Ta1 2.025(4) . ? O13 Ta1 2.145(4) . ? O14 Ta1 2.055(5) . ? O17 H17A 0.90(2) . ? O17 H17B 0.90(2) . ? O18 H18A 0.90(2) . ? O18 H18B 0.91(2) . ? O19A O19B 0.87(3) 2_676 ? O19B O19B 1.74(7) 2_676 ? 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 C1 C2 122.5(5) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.7(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.8(6) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C12 C4 C3 116.8(5) . . ? C12 C4 C5 119.1(5) . . ? C3 C4 C5 124.0(6) . . ? C6 C5 C4 121.1(6) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 120.6(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C11 C7 C8 117.2(6) . . ? C11 C7 C6 119.2(5) . . ? C8 C7 C6 123.6(5) . . ? C9 C8 C7 119.6(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.7(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 123.8(6) . . ? N2 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? N2 C11 C7 123.5(5) . . ? N2 C11 C12 116.6(5) . . ? C7 C11 C12 119.8(5) . . ? N1 C12 C4 123.0(5) . . ? N1 C12 C11 117.1(5) . . ? C4 C12 C11 119.9(5) . . ? N4 C22 C21 122.8(7) . . ? N4 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C20 C21 C22 119.2(8) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C20 C19 120.1(7) . . ? C21 C20 H20 120 . . ? C19 C20 H20 120 . . ? C18 C19 C24 119.2(9) . . ? C18 C19 C20 123.9(8) . . ? C24 C19 C20 116.9(7) . . ? C17 C18 C19 121.5(8) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C17 C16 121.1(8) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C23 C16 C15 116.8(8) . . ? C23 C16 C17 118.5(9) . . ? C15 C16 C17 124.7(8) . . ? C14 C15 C16 120.0(7) . . ? C14 C15 H15 120 . . ? C16 C15 H15 120 . . ? C15 C14 C13 120.6(9) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N3 C13 C14 122.3(9) . . ? N3 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? N3 C23 C16 122.3(8) . . ? N3 C23 C24 117.9(5) . . ? C16 C23 C24 119.8(7) . . ? N4 C24 C19 122.7(7) . . ? N4 C24 C23 117.4(6) . . ? C19 C24 C23 119.9(6) . . ? N5 C25 C26 123.4(7) . . ? N5 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C27 C26 C25 119.9(6) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 118.8(6) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C36 C28 C27 117.5(7) . . ? C36 C28 C29 119.0(6) . . ? C27 C28 C29 123.5(6) . . ? C30 C29 C28 120.6(6) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 121.5(7) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C35 C31 C32 117.9(6) . . ? C35 C31 C30 118.7(7) . . ? C32 C31 C30 123.4(7) . . ? C33 C32 C31 118.9(7) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 120.2(7) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? N6 C34 C33 121.7(6) . . ? N6 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? N6 C35 C31 122.4(6) . . ? N6 C35 C36 117.5(6) . . ? C31 C35 C36 120.1(6) . . ? N5 C36 C28 123.1(6) . . ? N5 C36 C35 116.8(5) . . ? C28 C36 C35 120.1(6) . . ? N7 C37 C38 123.7(12) . . ? N7 C37 H37 118.2 . . ? C38 C37 H37 118.2 . . ? C39 C38 C37 118.9(12) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 120.4(9) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C41 124.2(8) . . ? C39 C40 C48 117.8(9) . . ? C41 C40 C48 117.9(9) . . ? C42 C41 C40 122.3(8) . . ? C42 C41 H41 118.8 . . ? C40 C41 H41 118.8 . . ? C41 C42 C43 121.1(9) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C47 C43 C44 119.8(8) . . ? C47 C43 C42 116.4(9) . . ? C44 C43 C42 123.7(9) . . ? C43 C44 C45 121.0(9) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 117.8(9) . . ? C46 C45 H45 121.1 . . ? C44 C45 H45 121.1 . . ? N8 C46 C45 120.2(8) . . ? N8 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C43 C47 N8 118.5(7) . . ? C43 C47 C48 122.8(7) . . ? N8 C47 C48 118.7(7) . . ? N7 C48 C47 118.2(7) . . ? N7 C48 C40 122.4(8) . . ? C47 C48 C40 119.4(8) . . ? O4 C49 O1 124.1(7) . . ? O4 C49 C50 121.8(7) . . ? O1 C49 C50 114.1(5) . . ? O3 C50 O2 127.2(6) . . ? O3 C50 C49 122.3(6) . . ? O2 C50 C49 110.6(6) . . ? O7 C51 O5 127.5(6) . . ? O7 C51 C52 120.5(5) . . ? O5 C51 C52 112.0(5) . . ? O8 C52 O6 124.2(5) . . ? O8 C52 C51 122.9(5) . . ? O6 C52 C51 112.9(5) . . ? O12 C53 O9 125.4(7) . . ? O12 C53 C54 121.2(6) . . ? O9 C53 C54 113.4(6) . . ? O11 C54 O10 125.3(7) . . ? O11 C54 C53 123.1(6) . . ? O10 C54 C53 111.5(6) . . ? O15 C55 O14 126.5(6) . . ? O15 C55 C56 122.0(6) . . ? O14 C55 C56 111.5(6) . . ? O16 C56 O13 125.9(6) . . ? O16 C56 C55 121.9(6) . . ? O13 C56 C55 112.3(5) . . ? C1 N1 C12 118.2(5) . . ? C1 N1 Ni1 128.9(4) . . ? C12 N1 Ni1 112.8(3) . . ? C10 N2 C11 116.1(5) . . ? C10 N2 Ni1 131.1(4) . . ? C11 N2 Ni1 112.8(3) . . ? C22 N4 C24 118.3(6) . . ? C22 N4 Ni1 128.9(4) . . ? C24 N4 Ni1 112.7(5) . . ? C13 N3 C23 118.1(6) . . ? C13 N3 Ni1 129.5(5) . . ? C23 N3 Ni1 112.3(4) . . ? C25 N5 C36 117.3(5) . . ? C25 N5 Ni1 130.6(5) . . ? C36 N5 Ni1 111.9(4) . . ? C34 N6 C35 118.9(6) . . ? C34 N6 Ni1 128.1(4) . . ? C35 N6 Ni1 112.5(4) . . ? C37 N7 C48 116.6(8) . . ? C46 N8 C47 122.7(7) . . ? C46 N8 H8A 118.7 . . ? C47 N8 H8A 118.7 . . ? C49 O1 Ta1 117.5(4) . . ? C50 O2 Ta1 122.0(4) . . ? C51 O5 Ta1 119.0(4) . . ? C52 O6 Ta1 121.6(3) . . ? C53 O9 Ta1 117.5(4) . . ? C54 O10 Ta1 120.5(4) . . ? C56 O13 Ta1 119.8(4) . . ? C55 O14 Ta1 122.5(4) . . ? H17A O17 H17B 111(5) . . ? H18A O18 H18B 113(5) . . ? N6 Ni1 N2 95.29(18) . . ? N6 Ni1 N1 97.27(19) . . ? N2 Ni1 N1 79.66(17) . . ? N6 Ni1 N5 79.7(2) . . ? N2 Ni1 N5 173.77(19) . . ? N1 Ni1 N5 97.16(18) . . ? N6 Ni1 N3 91.8(2) . . ? N2 Ni1 N3 92.12(18) . . ? N1 Ni1 N3 168.3(2) . . ? N5 Ni1 N3 91.77(19) . . ? N6 Ni1 N4 168.0(2) . . ? N2 Ni1 N4 93.14(18) . . ? N1 Ni1 N4 92.6(2) . . ? N5 Ni1 N4 92.4(2) . . ? N3 Ni1 N4 79.4(2) . . ? O10 Ta1 O6 142.31(17) . . ? O10 Ta1 O2 104.58(19) . . ? O6 Ta1 O2 85.30(16) . . ? O10 Ta1 O14 88.7(2) . . ? O6 Ta1 O14 105.17(18) . . ? O2 Ta1 O14 143.09(17) . . ? O10 Ta1 O9 74.79(18) . . ? O6 Ta1 O9 76.71(16) . . ? O2 Ta1 O9 144.84(17) . . ? O14 Ta1 O9 71.62(18) . . ? O10 Ta1 O1 72.05(17) . . ? O6 Ta1 O1 144.51(16) . . ? O2 Ta1 O1 73.83(17) . . ? O14 Ta1 O1 78.0(2) . . ? O9 Ta1 O1 135.03(17) . . ? O10 Ta1 O13 145.35(17) . . ? O6 Ta1 O13 72.05(16) . . ? O2 Ta1 O13 77.02(16) . . ? O14 Ta1 O13 73.08(17) . . ? O9 Ta1 O13 123.74(17) . . ? O1 Ta1 O13 75.42(16) . . ? O10 Ta1 O5 74.49(19) . . ? O6 Ta1 O5 74.20(16) . . ? O2 Ta1 O5 72.39(16) . . ? O14 Ta1 O5 144.39(17) . . ? O9 Ta1 O5 73.73(17) . . ? O1 Ta1 O5 123.58(18) . . ? O13 Ta1 O5 135.71(16) . . ? data_2 _database_code_depnum_ccdc_archive 'CCDC 894040' #TrackingRef '12901_web_deposit_cif_file_1_LidijaAndros_1343389594.ccdc_deposit2.cif' _audit_creation_date 2012-05-24T15:26:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_formula_sum 'C42 H41 N6 Ni O21 Ta' _chemical_formula_weight 1205.47 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6629(3) _cell_length_b 13.5404(4) _cell_length_c 16.0209(4) _cell_angle_alpha 65.972(3) _cell_angle_beta 80.640(2) _cell_angle_gamma 76.627(2) _cell_volume 2241.45(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10224 _cell_measurement_theta_min 4.1586 _cell_measurement_theta_max 28.9454 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_special_details ? #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.62928 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.3426 _diffrn_orient_matrix_ub_11 0.0270431 _diffrn_orient_matrix_ub_12 -0.0470266 _diffrn_orient_matrix_ub_13 -0.0098947 _diffrn_orient_matrix_ub_21 0.0288297 _diffrn_orient_matrix_ub_22 0.033683 _diffrn_orient_matrix_ub_23 -0.0406562 _diffrn_orient_matrix_ub_31 0.0486681 _diffrn_orient_matrix_ub_32 -0.0075895 _diffrn_orient_matrix_ub_33 0.0247569 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.053 _diffrn_reflns_number 17383 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 29.01 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.846 _reflns_number_total 10082 _reflns_number_gt 8902 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0308P)^2^+0.9132P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10082 _refine_ls_number_parameters 703 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.332 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.119 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6638(3) 0.8975(3) 0.5856(2) 0.0173(7) Uani 1 1 d . . . H1 H 0.6246 0.97 0.5702 0.021 Uiso 1 1 calc R . . C2 C 0.6557(3) 0.8428(3) 0.5299(2) 0.0223(8) Uani 1 1 d . . . H2 H 0.6132 0.8791 0.478 0.027 Uiso 1 1 calc R . . C3 C 0.7106(3) 0.7358(3) 0.5521(2) 0.0221(8) Uani 1 1 d . . . H3 H 0.7045 0.6981 0.5162 0.027 Uiso 1 1 calc R . . C4 C 0.7767(3) 0.6826(3) 0.6300(2) 0.0190(7) Uani 1 1 d . . . C5 C 0.8390(3) 0.5720(3) 0.6575(3) 0.0244(8) Uani 1 1 d . . . H5 H 0.8341 0.5303 0.6247 0.029 Uiso 1 1 calc R . . C6 C 0.9054(3) 0.5263(3) 0.7306(3) 0.0251(8) Uani 1 1 d . . . H6 H 0.9439 0.4534 0.7481 0.03 Uiso 1 1 calc R . . C7 C 0.9170(3) 0.5894(3) 0.7813(2) 0.0192(7) Uani 1 1 d . . . C8 C 0.9898(3) 0.5487(3) 0.8541(2) 0.0198(7) Uani 1 1 d . . . H8 H 1.0304 0.4765 0.8738 0.024 Uiso 1 1 calc R . . C9 C 1.0007(3) 0.6159(3) 0.8961(2) 0.0210(8) Uani 1 1 d . . . H9 H 1.0505 0.5904 0.9433 0.025 Uiso 1 1 calc R . . C10 C 0.9359(3) 0.7235(3) 0.8669(2) 0.0181(7) Uani 1 1 d . . . H10 H 0.9433 0.7685 0.896 0.022 Uiso 1 1 calc R . . C11 C 0.8554(3) 0.6971(3) 0.7566(2) 0.0142(7) Uani 1 1 d . . . C12 C 0.7826(3) 0.7452(3) 0.6806(2) 0.0144(6) Uani 1 1 d . . . C13 C 0.8613(3) 1.0225(3) 0.8525(2) 0.0190(7) Uani 1 1 d . . . H13 H 0.9136 1.046 0.801 0.023 Uiso 1 1 calc R . . C14 C 0.8683(3) 1.0490(3) 0.9272(2) 0.0211(7) Uani 1 1 d . . . H14 H 0.9237 1.0898 0.9248 0.025 Uiso 1 1 calc R . . C15 C 0.7927(3) 1.0140(3) 1.0039(2) 0.0204(7) Uani 1 1 d . . . H15 H 0.7971 1.0304 1.0542 0.025 Uiso 1 1 calc R . . C16 C 0.7091(3) 0.9538(3) 1.0061(2) 0.0156(7) Uani 1 1 d . . . C17 C 0.6266(3) 0.9142(3) 1.0827(2) 0.0182(7) Uani 1 1 d . . . H17 H 0.6291 0.9264 1.1354 0.022 Uiso 1 1 calc R . . C18 C 0.5451(3) 0.8596(3) 1.0801(2) 0.0180(7) Uani 1 1 d . . . H18 H 0.4917 0.8357 1.1307 0.022 Uiso 1 1 calc R . . C19 C 0.5393(3) 0.8379(3) 1.0005(2) 0.0142(6) Uani 1 1 d . . . C20 C 0.4566(3) 0.7802(3) 0.9941(2) 0.0175(7) Uani 1 1 d . . . H20 H 0.4007 0.755 1.0424 0.021 Uiso 1 1 calc R . . C21 C 0.4600(3) 0.7620(3) 0.9159(2) 0.0192(7) Uani 1 1 d . . . H21 H 0.4066 0.7236 0.9109 0.023 Uiso 1 1 calc R . . C22 C 0.5438(3) 0.8008(3) 0.8435(2) 0.0187(7) Uani 1 1 d . . . H22 H 0.5453 0.787 0.791 0.022 Uiso 1 1 calc R . . C23 C 0.6204(3) 0.8739(3) 0.9250(2) 0.0136(6) Uani 1 1 d . . . C24 C 0.7064(3) 0.9325(3) 0.9273(2) 0.0132(6) Uani 1 1 d . . . C25 C 0.5380(3) 1.1042(3) 0.6892(2) 0.0177(7) Uani 1 1 d . . . H25 H 0.494 1.0598 0.738 0.021 Uiso 1 1 calc R . . C26 C 0.4803(3) 1.2061(3) 0.6312(2) 0.0214(8) Uani 1 1 d . . . H26 H 0.3998 1.229 0.6423 0.026 Uiso 1 1 calc R . . C27 C 0.5425(3) 1.2721(3) 0.5579(2) 0.0216(8) Uani 1 1 d . . . H27 H 0.5046 1.3396 0.5184 0.026 Uiso 1 1 calc R . . C28 C 0.6642(3) 1.2370(3) 0.5430(2) 0.0171(7) Uani 1 1 d . . . C29 C 0.7374(3) 1.3000(3) 0.4692(2) 0.0224(8) Uani 1 1 d . . . H29 H 0.7038 1.3676 0.4271 0.027 Uiso 1 1 calc R . . C30 C 0.8552(3) 1.2627(3) 0.4598(2) 0.0229(8) Uani 1 1 d . . . H30 H 0.9009 1.3051 0.4111 0.027 Uiso 1 1 calc R . . C31 C 0.9104(3) 1.1598(3) 0.5230(2) 0.0178(7) Uani 1 1 d . . . C32 C 1.0332(3) 1.1191(3) 0.5206(2) 0.0219(8) Uani 1 1 d . . . H32 H 1.0834 1.1597 0.4748 0.026 Uiso 1 1 calc R . . C33 C 1.0785(3) 1.0206(3) 0.5850(2) 0.0220(8) Uani 1 1 d . . . H33 H 1.1596 0.9943 0.5847 0.026 Uiso 1 1 calc R . . C34 C 1.0008(3) 0.9595(3) 0.6519(2) 0.0194(7) Uani 1 1 d . . . H34 H 1.0316 0.8909 0.6943 0.023 Uiso 1 1 calc R . . C35 C 0.8406(3) 1.0947(3) 0.5947(2) 0.0146(7) Uani 1 1 d . . . C36 C 0.7155(3) 1.1346(3) 0.6051(2) 0.0131(6) Uani 1 1 d . . . C37 C 0.2680(3) 0.4259(3) 0.7797(2) 0.0171(7) Uani 1 1 d . . . C38 C 0.2848(3) 0.4007(3) 0.8817(2) 0.0141(6) Uani 1 1 d . . . C39 C 0.2853(3) 0.7492(3) 0.7649(2) 0.0199(7) Uani 1 1 d . . . C40 C 0.3647(3) 0.7849(3) 0.6747(2) 0.0220(8) Uani 1 1 d . . . C41 C 0.6245(3) 0.4492(3) 0.6497(2) 0.0196(7) Uani 1 1 d . . . C42 C 0.6175(3) 0.3521(3) 0.7423(2) 0.0202(7) Uani 1 1 d . . . N1 N 0.7250(2) 0.8507(2) 0.65964(18) 0.0137(6) Uani 1 1 d . . . N2 N 0.8643(2) 0.7639(2) 0.79951(18) 0.0141(6) Uani 1 1 d . . . N3 N 0.7831(2) 0.9653(2) 0.85216(18) 0.0145(6) Uani 1 1 d . . . N4 N 0.6214(2) 0.8568(2) 0.84698(17) 0.0141(6) Uani 1 1 d . . . N5 N 0.6530(2) 1.0679(2) 0.67772(18) 0.0139(6) Uani 1 1 d . . . N6 N 0.8855(2) 0.9954(2) 0.65725(18) 0.0153(6) Uani 1 1 d . . . Ni1 Ni 0.75545(3) 0.91784(3) 0.74947(3) 0.01245(9) Uani 1 1 d . . . O1 O 0.5582(2) 0.5595(2) 0.83385(18) 0.0194(5) Uani 1 1 d . . . O2 O 0.3302(2) 0.4954(2) 0.72209(15) 0.0184(5) Uani 1 1 d . . . O3 O 0.2002(2) 0.3834(2) 0.76074(16) 0.0247(6) Uani 1 1 d . . . O4 O 0.22372(19) 0.3460(2) 0.94401(15) 0.0197(5) Uani 1 1 d . . . O5 O 0.36664(19) 0.44579(18) 0.88906(14) 0.0142(5) Uani 1 1 d . . . O6 O 0.3116(2) 0.6456(2) 0.81207(16) 0.0205(5) Uani 1 1 d . . . O7 O 0.2102(2) 0.8159(2) 0.78718(18) 0.0274(6) Uani 1 1 d . . . O8 O 0.3561(2) 0.8782(2) 0.61915(19) 0.0330(7) Uani 1 1 d . . . O9 O 0.4413(2) 0.7006(2) 0.66809(16) 0.0215(5) Uani 1 1 d . . . O10 O 0.5590(2) 0.5398(2) 0.65274(15) 0.0180(5) Uani 1 1 d . . . O11 O 0.6862(2) 0.4407(2) 0.58350(17) 0.0292(6) Uani 1 1 d . . . O12 O 0.6778(2) 0.2618(2) 0.75591(18) 0.0288(6) Uani 1 1 d . . . O13 O 0.5408(2) 0.3804(2) 0.80020(15) 0.0189(5) Uani 1 1 d . . . O14 O 0.9128(3) 0.2544(3) 0.6810(3) 0.0526(9) Uani 1 1 d D . . O15 O 0.8089(3) 0.5682(3) 0.4285(2) 0.0489(9) Uani 1 1 d D . . O16 O 0.9620(2) 0.7538(2) 0.0593(2) 0.0308(6) Uani 1 1 d D . . O17 O 0.9026(3) 0.8031(3) 0.2185(2) 0.0398(7) Uani 1 1 d D . . O18 O 0.7179(3) 0.9652(3) 0.2526(3) 0.0457(8) Uani 1 1 d D . . O19 O 0.6948(2) 0.5015(3) 0.95335(18) 0.0285(6) Uani 1 1 d D . . O20 O 0.1870(2) 0.7048(3) 0.9893(2) 0.0324(7) Uani 1 1 d D . . O21 O 0.9998(5) 0.6123(6) 0.4724(4) 0.130(2) Uani 1 1 d G . . Ta1 Ta 0.455969(12) 0.545141(12) 0.769344(9) 0.01493(5) Uani 1 1 d . . . H11 H 0.595(5) 0.541(6) 0.871(4) 0.09(2) Uiso 1 1 d . . . H14A H 0.835(2) 0.260(4) 0.701(3) 0.074(19) Uiso 1 1 d D . . H14B H 0.911(3) 0.311(3) 0.6268(18) 0.028(12) Uiso 1 1 d D . . H15A H 0.822(8) 0.509(4) 0.478(3) 0.17(4) Uiso 1 1 d D . . H15B H 0.803(4) 0.568(4) 0.3765(18) 0.051(15) Uiso 1 1 d D . . H16A H 0.898(3) 0.733(4) 0.054(3) 0.059(16) Uiso 1 1 d D . . H16B H 0.959(3) 0.767(3) 0.1090(18) 0.017(10) Uiso 1 1 d D . . H17A H 0.866(5) 0.745(4) 0.236(4) 0.11(3) Uiso 1 1 d D . . H17B H 0.961(4) 0.782(4) 0.257(3) 0.08(2) Uiso 1 1 d D . . H18A H 0.789(2) 0.926(3) 0.246(3) 0.047(14) Uiso 1 1 d D . . H18B H 0.724(5) 1.031(3) 0.249(5) 0.14(3) Uiso 1 1 d D . . H19A H 0.733(3) 0.4329(19) 0.970(3) 0.035(13) Uiso 1 1 d D . . H19B H 0.664(5) 0.527(4) 0.996(3) 0.10(2) Uiso 1 1 d D . . H20A H 0.116(3) 0.716(5) 1.018(3) 0.075(19) Uiso 1 1 d D . . H20B H 0.186(4) 0.735(4) 0.9284(13) 0.070(18) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0149(16) 0.0182(19) 0.0172(16) -0.0049(14) -0.0002(13) -0.0040(13) C2 0.0206(18) 0.031(2) 0.0172(17) -0.0092(16) -0.0040(14) -0.0056(16) C3 0.0218(18) 0.028(2) 0.0228(18) -0.0128(16) -0.0024(14) -0.0104(16) C4 0.0176(17) 0.021(2) 0.0219(17) -0.0097(15) 0.0017(14) -0.0095(14) C5 0.0241(19) 0.023(2) 0.032(2) -0.0151(17) -0.0016(16) -0.0063(16) C6 0.0261(19) 0.017(2) 0.033(2) -0.0118(17) -0.0030(16) -0.0009(15) C7 0.0179(17) 0.0183(19) 0.0205(17) -0.0065(15) 0.0029(14) -0.0068(14) C8 0.0157(16) 0.0148(18) 0.0229(18) -0.0022(15) -0.0022(14) -0.0005(14) C9 0.0187(17) 0.024(2) 0.0163(17) -0.0016(15) -0.0049(13) -0.0041(15) C10 0.0184(17) 0.0197(19) 0.0141(16) -0.0036(14) -0.0010(13) -0.0053(14) C11 0.0137(15) 0.0155(18) 0.0130(15) -0.0052(13) 0.0029(12) -0.0052(13) C12 0.0129(15) 0.0153(18) 0.0156(16) -0.0062(14) 0.0037(12) -0.0068(13) C13 0.0159(16) 0.0196(19) 0.0203(17) -0.0060(15) -0.0013(13) -0.0042(14) C14 0.0228(18) 0.0188(19) 0.0257(19) -0.0089(16) -0.0026(15) -0.0103(15) C15 0.0219(18) 0.023(2) 0.0194(17) -0.0113(16) -0.0012(14) -0.0051(15) C16 0.0182(16) 0.0144(17) 0.0137(15) -0.0052(13) -0.0018(13) -0.0023(13) C17 0.0225(17) 0.0214(19) 0.0125(16) -0.0101(14) 0.0006(13) -0.0020(14) C18 0.0190(17) 0.0177(19) 0.0140(16) -0.0041(14) 0.0024(13) -0.0035(14) C19 0.0134(15) 0.0129(17) 0.0134(15) -0.0030(13) -0.0004(12) -0.0012(13) C20 0.0171(16) 0.0156(18) 0.0156(16) -0.0017(14) -0.0013(13) -0.0032(13) C21 0.0167(16) 0.022(2) 0.0192(17) -0.0056(15) -0.0023(13) -0.0078(14) C22 0.0197(17) 0.022(2) 0.0165(16) -0.0081(15) -0.0019(13) -0.0062(14) C23 0.0150(15) 0.0097(16) 0.0151(15) -0.0034(13) -0.0024(12) -0.0021(12) C24 0.0131(15) 0.0106(16) 0.0146(15) -0.0044(13) -0.0015(12) -0.0005(12) C25 0.0159(16) 0.0214(19) 0.0180(17) -0.0097(15) -0.0008(13) -0.0042(14) C26 0.0200(17) 0.023(2) 0.0223(18) -0.0110(16) -0.0060(14) 0.0008(15) C27 0.0267(19) 0.0164(19) 0.0213(18) -0.0064(15) -0.0134(15) 0.0032(15) C28 0.0229(17) 0.0145(18) 0.0165(16) -0.0066(14) -0.0042(13) -0.0052(14) C29 0.037(2) 0.0148(19) 0.0126(16) 0.0006(14) -0.0084(15) -0.0062(16) C30 0.034(2) 0.021(2) 0.0140(17) -0.0027(15) 0.0013(15) -0.0146(16) C31 0.0225(17) 0.0201(19) 0.0142(16) -0.0077(14) -0.0007(13) -0.0087(14) C32 0.0222(18) 0.029(2) 0.0176(17) -0.0100(16) 0.0059(14) -0.0135(16) C33 0.0135(16) 0.029(2) 0.0240(18) -0.0104(16) 0.0023(14) -0.0065(15) C34 0.0151(16) 0.023(2) 0.0200(17) -0.0095(15) 0.0006(13) -0.0022(14) C35 0.0200(16) 0.0155(18) 0.0104(15) -0.0063(13) 0.0002(12) -0.0057(13) C36 0.0191(16) 0.0139(17) 0.0087(14) -0.0060(13) -0.0029(12) -0.0031(13) C37 0.0168(16) 0.0152(18) 0.0192(17) -0.0063(14) -0.0025(13) -0.0023(13) C38 0.0133(15) 0.0113(17) 0.0156(16) -0.0053(13) -0.0005(12) 0.0018(13) C39 0.0163(16) 0.024(2) 0.0229(18) -0.0098(16) -0.0061(14) -0.0047(15) C40 0.0196(17) 0.019(2) 0.0265(19) -0.0055(16) -0.0079(15) -0.0041(15) C41 0.0263(18) 0.0171(19) 0.0166(17) -0.0050(15) 0.0003(14) -0.0101(15) C42 0.0166(17) 0.0177(19) 0.0259(19) -0.0067(15) -0.0017(14) -0.0053(14) N1 0.0122(13) 0.0165(15) 0.0126(13) -0.0053(11) 0.0001(10) -0.0046(11) N2 0.0154(13) 0.0133(15) 0.0117(13) -0.0027(11) -0.0006(10) -0.0034(11) N3 0.0162(13) 0.0118(15) 0.0150(13) -0.0046(11) -0.0020(11) -0.0022(11) N4 0.0140(13) 0.0170(15) 0.0112(13) -0.0045(11) -0.0005(10) -0.0049(11) N5 0.0143(13) 0.0138(15) 0.0136(13) -0.0051(11) -0.0010(10) -0.0030(11) N6 0.0156(13) 0.0189(16) 0.0131(13) -0.0069(12) 0.0023(11) -0.0075(11) Ni1 0.0132(2) 0.0128(2) 0.01046(19) -0.00353(17) -0.00035(15) -0.00299(16) O1 0.0195(12) 0.0203(14) 0.0192(13) -0.0078(11) -0.0022(10) -0.0042(10) O2 0.0241(12) 0.0180(13) 0.0121(11) -0.0027(10) -0.0009(9) -0.0081(10) O3 0.0279(14) 0.0300(16) 0.0197(13) -0.0072(12) -0.0005(11) -0.0172(12) O4 0.0168(12) 0.0210(14) 0.0161(12) -0.0024(10) 0.0006(9) -0.0039(10) O5 0.0161(11) 0.0105(12) 0.0142(11) -0.0034(9) -0.0027(9) -0.0004(9) O6 0.0224(12) 0.0133(13) 0.0199(12) -0.0019(10) -0.0015(10) -0.0005(10) O7 0.0279(14) 0.0219(15) 0.0304(14) -0.0112(12) -0.0061(11) 0.0040(11) O8 0.0337(15) 0.0161(15) 0.0369(16) 0.0011(13) -0.0037(13) -0.0021(12) O9 0.0223(13) 0.0137(13) 0.0225(13) -0.0017(11) -0.0018(10) -0.0016(10) O10 0.0258(13) 0.0132(13) 0.0148(11) -0.0045(10) 0.0029(10) -0.0077(10) O11 0.0439(16) 0.0274(16) 0.0188(13) -0.0119(12) 0.0132(12) -0.0162(13) O12 0.0305(15) 0.0234(16) 0.0301(15) -0.0123(12) 0.0044(12) -0.0013(12) O13 0.0213(12) 0.0165(13) 0.0139(11) -0.0031(10) 0.0034(9) -0.0022(10) O14 0.0363(19) 0.076(3) 0.053(2) -0.034(2) 0.0141(17) -0.0193(19) O15 0.081(3) 0.061(3) 0.0180(15) -0.0133(16) 0.0013(16) -0.046(2) O16 0.0230(14) 0.0343(18) 0.0395(17) -0.0187(14) 0.0056(12) -0.0107(12) O17 0.0438(19) 0.0329(19) 0.050(2) -0.0229(16) 0.0079(16) -0.0167(15) O18 0.0301(17) 0.045(2) 0.076(2) -0.037(2) -0.0100(16) -0.0034(15) O19 0.0268(15) 0.0376(19) 0.0246(14) -0.0171(14) -0.0070(12) 0.0006(13) O20 0.0227(14) 0.046(2) 0.0306(16) -0.0185(15) 0.0001(12) -0.0040(13) O21 0.111(4) 0.178(7) 0.106(4) -0.047(4) 0.014(3) -0.064(5) Ta1 0.01670(7) 0.01431(8) 0.01293(7) -0.00339(5) -0.00154(5) -0.00445(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.332(4) . ? C1 C2 1.397(5) . ? C1 H1 0.93 . ? C2 C3 1.365(5) . ? C2 H2 0.93 . ? C3 C4 1.413(5) . ? C3 H3 0.93 . ? C4 C12 1.410(4) . ? C4 C5 1.424(5) . ? C5 C6 1.356(5) . ? C5 H5 0.93 . ? C6 C7 1.435(5) . ? C6 H6 0.93 . ? C7 C11 1.392(5) . ? C7 C8 1.402(5) . ? C8 C9 1.369(5) . ? C8 H8 0.93 . ? C9 C10 1.402(5) . ? C9 H9 0.93 . ? C10 N2 1.327(4) . ? C10 H10 0.93 . ? C11 N2 1.369(4) . ? C11 C12 1.435(4) . ? C12 N1 1.358(4) . ? C13 N3 1.328(4) . ? C13 C14 1.400(5) . ? C13 H13 0.93 . ? C14 C15 1.370(5) . ? C14 H14 0.93 . ? C15 C16 1.396(5) . ? C15 H15 0.93 . ? C16 C24 1.412(4) . ? C16 C17 1.427(5) . ? C17 C18 1.347(5) . ? C17 H17 0.93 . ? C18 C19 1.435(4) . ? C18 H18 0.93 . ? C19 C23 1.399(4) . ? C19 C20 1.414(4) . ? C20 C21 1.364(5) . ? C20 H20 0.93 . ? C21 C22 1.395(5) . ? C21 H21 0.93 . ? C22 N4 1.329(4) . ? C22 H22 0.93 . ? C23 N4 1.359(4) . ? C23 C24 1.428(4) . ? C24 N3 1.359(4) . ? C25 N5 1.327(4) . ? C25 C26 1.397(5) . ? C25 H25 0.93 . ? C26 C27 1.369(5) . ? C26 H26 0.93 . ? C27 C28 1.402(5) . ? C27 H27 0.93 . ? C28 C36 1.399(5) . ? C28 C29 1.429(5) . ? C29 C30 1.356(5) . ? C29 H29 0.93 . ? C30 C31 1.424(5) . ? C30 H30 0.93 . ? C31 C35 1.401(4) . ? C31 C32 1.410(5) . ? C32 C33 1.362(5) . ? C32 H32 0.93 . ? C33 C34 1.401(5) . ? C33 H33 0.93 . ? C34 N6 1.321(4) . ? C34 H34 0.93 . ? C35 N6 1.354(4) . ? C35 C36 1.442(4) . ? C36 N5 1.369(4) . ? C37 O3 1.217(4) . ? C37 O2 1.286(4) . ? C37 C38 1.563(4) . ? C38 O4 1.210(4) . ? C38 O5 1.289(4) . ? C39 O7 1.227(4) . ? C39 O6 1.283(4) . ? C39 C40 1.543(5) . ? C40 O8 1.205(4) . ? C40 O9 1.307(4) . ? C41 O11 1.213(4) . ? C41 O10 1.301(4) . ? C41 C42 1.536(5) . ? C42 O12 1.213(4) . ? C42 O13 1.292(4) . ? N1 Ni1 2.098(3) . ? N2 Ni1 2.084(3) . ? N3 Ni1 2.087(3) . ? N4 Ni1 2.078(3) . ? N5 Ni1 2.073(3) . ? N6 Ni1 2.081(3) . ? O1 Ta1 1.789(3) . ? O1 H11 0.72(6) . ? O2 Ta1 2.101(2) . ? O5 Ta1 2.114(2) . ? O6 Ta1 2.116(2) . ? O9 Ta1 2.058(2) . ? O10 Ta1 2.068(2) . ? O13 Ta1 2.107(2) . ? O14 H14A 0.906(19) . ? O14 H14B 0.894(18) . ? O15 H15A 0.87(2) . ? O15 H15B 0.851(19) . ? O16 H16A 0.890(19) . ? O16 H16B 0.877(18) . ? O17 H17A 0.90(2) . ? O17 H17B 0.919(19) . ? O18 H18A 0.898(19) . ? O18 H18B 0.89(2) . ? O19 H19A 0.882(18) . ? O19 H19B 0.870(19) . ? O20 H20A 0.892(19) . ? O20 H20B 0.891(19) . ? 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 C1 C2 123.1(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C12 C4 C3 117.0(3) . . ? C12 C4 C5 119.4(3) . . ? C3 C4 C5 123.6(3) . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C11 C7 C8 117.6(3) . . ? C11 C7 C6 119.1(3) . . ? C8 C7 C6 123.2(3) . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.0(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 122.8(3) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 122.8(3) . . ? N2 C11 C12 116.6(3) . . ? C7 C11 C12 120.5(3) . . ? N1 C12 C4 123.2(3) . . ? N1 C12 C11 117.8(3) . . ? C4 C12 C11 119.0(3) . . ? N3 C13 C14 122.7(3) . . ? N3 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C24 117.4(3) . . ? C15 C16 C17 123.7(3) . . ? C24 C16 C17 118.9(3) . . ? C18 C17 C16 121.3(3) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 121.0(3) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C23 C19 C20 117.4(3) . . ? C23 C19 C18 119.0(3) . . ? C20 C19 C18 123.6(3) . . ? C21 C20 C19 119.0(3) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120 . . ? C22 C21 H21 120 . . ? N4 C22 C21 122.3(3) . . ? N4 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? N4 C23 C19 122.9(3) . . ? N4 C23 C24 117.0(3) . . ? C19 C23 C24 120.1(3) . . ? N3 C24 C16 122.7(3) . . ? N3 C24 C23 117.6(3) . . ? C16 C24 C23 119.7(3) . . ? N5 C25 C26 122.8(3) . . ? N5 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C27 C26 C25 119.8(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.3(3) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C36 C28 C27 117.3(3) . . ? C36 C28 C29 118.9(3) . . ? C27 C28 C29 123.8(3) . . ? C30 C29 C28 121.0(3) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 121.4(3) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C35 C31 C32 116.5(3) . . ? C35 C31 C30 119.1(3) . . ? C32 C31 C30 124.4(3) . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 118.8(3) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? N6 C34 C33 122.7(3) . . ? N6 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? N6 C35 C31 123.0(3) . . ? N6 C35 C36 117.4(3) . . ? C31 C35 C36 119.6(3) . . ? N5 C36 C28 123.4(3) . . ? N5 C36 C35 116.6(3) . . ? C28 C36 C35 120.1(3) . . ? O3 C37 O2 126.0(3) . . ? O3 C37 C38 121.0(3) . . ? O2 C37 C38 113.0(3) . . ? O4 C38 O5 126.4(3) . . ? O4 C38 C37 121.1(3) . . ? O5 C38 C37 112.5(3) . . ? O7 C39 O6 126.4(3) . . ? O7 C39 C40 121.7(3) . . ? O6 C39 C40 111.8(3) . . ? O8 C40 O9 125.6(4) . . ? O8 C40 C39 123.8(3) . . ? O9 C40 C39 110.6(3) . . ? O11 C41 O10 125.4(3) . . ? O11 C41 C42 122.9(3) . . ? O10 C41 C42 111.7(3) . . ? O12 C42 O13 126.6(3) . . ? O12 C42 C41 122.3(3) . . ? O13 C42 C41 111.2(3) . . ? C1 N1 C12 117.7(3) . . ? C1 N1 Ni1 129.8(2) . . ? C12 N1 Ni1 112.4(2) . . ? C10 N2 C11 117.9(3) . . ? C10 N2 Ni1 128.9(2) . . ? C11 N2 Ni1 113.1(2) . . ? C13 N3 C24 118.1(3) . . ? C13 N3 Ni1 129.4(2) . . ? C24 N3 Ni1 112.4(2) . . ? C22 N4 C23 118.3(3) . . ? C22 N4 Ni1 128.6(2) . . ? C23 N4 Ni1 113.0(2) . . ? C25 N5 C36 117.4(3) . . ? C25 N5 Ni1 129.8(2) . . ? C36 N5 Ni1 112.8(2) . . ? C34 N6 C35 118.5(3) . . ? C34 N6 Ni1 128.8(2) . . ? C35 N6 Ni1 112.6(2) . . ? N5 Ni1 N4 95.93(11) . . ? N5 Ni1 N6 80.24(11) . . ? N4 Ni1 N6 172.78(11) . . ? N5 Ni1 N2 169.90(10) . . ? N4 Ni1 N2 89.68(11) . . ? N6 Ni1 N2 95.04(11) . . ? N5 Ni1 N3 94.20(10) . . ? N4 Ni1 N3 79.93(10) . . ? N6 Ni1 N3 94.19(10) . . ? N2 Ni1 N3 95.04(10) . . ? N5 Ni1 N1 91.35(10) . . ? N4 Ni1 N1 94.79(10) . . ? N6 Ni1 N1 91.43(10) . . ? N2 Ni1 N1 79.79(10) . . ? N3 Ni1 N1 172.69(11) . . ? Ta1 O1 H11 155(5) . . ? C37 O2 Ta1 119.6(2) . . ? C38 O5 Ta1 119.54(19) . . ? C39 O6 Ta1 121.3(2) . . ? C40 O9 Ta1 123.2(2) . . ? C41 O10 Ta1 122.3(2) . . ? C42 O13 Ta1 121.5(2) . . ? H14A O14 H14B 102(3) . . ? H15A O15 H15B 124(5) . . ? H16A O16 H16B 114(3) . . ? H17A O17 H17B 107(4) . . ? H18A O18 H18B 111(4) . . ? H19A O19 H19B 119(4) . . ? H20A O20 H20B 113(4) . . ? O1 Ta1 O9 97.54(11) . . ? O1 Ta1 O10 102.75(10) . . ? O9 Ta1 O10 70.21(9) . . ? O1 Ta1 O2 166.34(10) . . ? O9 Ta1 O2 95.62(9) . . ? O10 Ta1 O2 85.11(9) . . ? O1 Ta1 O13 89.26(10) . . ? O9 Ta1 O13 143.26(9) . . ? O10 Ta1 O13 73.07(9) . . ? O2 Ta1 O13 82.31(9) . . ? O1 Ta1 O5 92.38(10) . . ? O9 Ta1 O5 142.78(9) . . ? O10 Ta1 O5 141.77(9) . . ? O2 Ta1 O5 74.85(8) . . ? O13 Ta1 O5 72.23(9) . . ? O1 Ta1 O6 93.95(10) . . ? O9 Ta1 O6 72.90(9) . . ? O10 Ta1 O6 141.05(9) . . ? O2 Ta1 O6 86.47(9) . . ? O13 Ta1 O6 142.87(9) . . ? O5 Ta1 O6 70.69(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.3(5) . . . . ? C1 C2 C3 C4 -1.3(5) . . . . ? C2 C3 C4 C12 -0.5(5) . . . . ? C2 C3 C4 C5 -178.6(3) . . . . ? C12 C4 C5 C6 -1.1(5) . . . . ? C3 C4 C5 C6 177.1(3) . . . . ? C4 C5 C6 C7 -1.4(6) . . . . ? C5 C6 C7 C11 2.4(5) . . . . ? C5 C6 C7 C8 -176.2(3) . . . . ? C11 C7 C8 C9 -1.9(5) . . . . ? C6 C7 C8 C9 176.7(3) . . . . ? C7 C8 C9 C10 1.8(5) . . . . ? C8 C9 C10 N2 -0.4(5) . . . . ? C8 C7 C11 N2 0.6(5) . . . . ? C6 C7 C11 N2 -178.0(3) . . . . ? C8 C7 C11 C12 177.8(3) . . . . ? C6 C7 C11 C12 -0.8(5) . . . . ? C3 C4 C12 N1 2.4(5) . . . . ? C5 C4 C12 N1 -179.3(3) . . . . ? C3 C4 C12 C11 -175.7(3) . . . . ? C5 C4 C12 C11 2.6(5) . . . . ? N2 C11 C12 N1 -2.5(4) . . . . ? C7 C11 C12 N1 -179.8(3) . . . . ? N2 C11 C12 C4 175.7(3) . . . . ? C7 C11 C12 C4 -1.6(5) . . . . ? N3 C13 C14 C15 0.6(5) . . . . ? C13 C14 C15 C16 -0.7(5) . . . . ? C14 C15 C16 C24 -0.5(5) . . . . ? C14 C15 C16 C17 -179.8(3) . . . . ? C15 C16 C17 C18 177.8(3) . . . . ? C24 C16 C17 C18 -1.6(5) . . . . ? C16 C17 C18 C19 0.9(5) . . . . ? C17 C18 C19 C23 0.3(5) . . . . ? C17 C18 C19 C20 179.4(3) . . . . ? C23 C19 C20 C21 0.4(5) . . . . ? C18 C19 C20 C21 -178.7(3) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? C20 C21 C22 N4 -0.6(5) . . . . ? C20 C19 C23 N4 0.8(5) . . . . ? C18 C19 C23 N4 179.9(3) . . . . ? C20 C19 C23 C24 -179.9(3) . . . . ? C18 C19 C23 C24 -0.7(5) . . . . ? C15 C16 C24 N3 1.9(5) . . . . ? C17 C16 C24 N3 -178.7(3) . . . . ? C15 C16 C24 C23 -178.2(3) . . . . ? C17 C16 C24 C23 1.2(5) . . . . ? N4 C23 C24 N3 -0.7(4) . . . . ? C19 C23 C24 N3 179.8(3) . . . . ? N4 C23 C24 C16 179.4(3) . . . . ? C19 C23 C24 C16 -0.1(5) . . . . ? N5 C25 C26 C27 1.1(5) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C36 0.0(5) . . . . ? C26 C27 C28 C29 -179.3(3) . . . . ? C36 C28 C29 C30 -1.0(5) . . . . ? C27 C28 C29 C30 178.3(3) . . . . ? C28 C29 C30 C31 -0.2(5) . . . . ? C29 C30 C31 C35 1.9(5) . . . . ? C29 C30 C31 C32 -176.0(3) . . . . ? C35 C31 C32 C33 0.8(5) . . . . ? C30 C31 C32 C33 178.7(3) . . . . ? C31 C32 C33 C34 1.7(5) . . . . ? C32 C33 C34 N6 -2.6(5) . . . . ? C32 C31 C35 N6 -2.7(5) . . . . ? C30 C31 C35 N6 179.3(3) . . . . ? C32 C31 C35 C36 175.8(3) . . . . ? C30 C31 C35 C36 -2.2(5) . . . . ? C27 C28 C36 N5 0.9(5) . . . . ? C29 C28 C36 N5 -179.8(3) . . . . ? C27 C28 C36 C35 -178.7(3) . . . . ? C29 C28 C36 C35 0.6(5) . . . . ? N6 C35 C36 N5 -0.1(4) . . . . ? C31 C35 C36 N5 -178.7(3) . . . . ? N6 C35 C36 C28 179.6(3) . . . . ? C31 C35 C36 C28 1.0(5) . . . . ? O3 C37 C38 O4 -6.5(5) . . . . ? O2 C37 C38 O4 172.3(3) . . . . ? O3 C37 C38 O5 174.8(3) . . . . ? O2 C37 C38 O5 -6.5(4) . . . . ? O7 C39 C40 O8 -2.9(5) . . . . ? O6 C39 C40 O8 179.6(3) . . . . ? O7 C39 C40 O9 176.9(3) . . . . ? O6 C39 C40 O9 -0.6(4) . . . . ? O11 C41 C42 O12 3.4(5) . . . . ? O10 C41 C42 O12 -175.1(3) . . . . ? O11 C41 C42 O13 -176.2(3) . . . . ? O10 C41 C42 O13 5.2(4) . . . . ? C2 C1 N1 C12 0.6(5) . . . . ? C2 C1 N1 Ni1 177.1(2) . . . . ? C4 C12 N1 C1 -2.4(5) . . . . ? C11 C12 N1 C1 175.7(3) . . . . ? C4 C12 N1 Ni1 -179.6(2) . . . . ? C11 C12 N1 Ni1 -1.5(3) . . . . ? C9 C10 N2 C11 -0.8(5) . . . . ? C9 C10 N2 Ni1 177.2(2) . . . . ? C7 C11 N2 C10 0.7(5) . . . . ? C12 C11 N2 C10 -176.6(3) . . . . ? C7 C11 N2 Ni1 -177.6(2) . . . . ? C12 C11 N2 Ni1 5.1(3) . . . . ? C14 C13 N3 C24 0.7(5) . . . . ? C14 C13 N3 Ni1 179.4(3) . . . . ? C16 C24 N3 C13 -2.0(5) . . . . ? C23 C24 N3 C13 178.1(3) . . . . ? C16 C24 N3 Ni1 179.1(2) . . . . ? C23 C24 N3 Ni1 -0.8(4) . . . . ? C21 C22 N4 C23 1.7(5) . . . . ? C21 C22 N4 Ni1 178.1(3) . . . . ? C19 C23 N4 C22 -1.8(5) . . . . ? C24 C23 N4 C22 178.8(3) . . . . ? C19 C23 N4 Ni1 -178.7(3) . . . . ? C24 C23 N4 Ni1 1.9(4) . . . . ? C26 C25 N5 C36 -0.3(5) . . . . ? C26 C25 N5 Ni1 -176.1(2) . . . . ? C28 C36 N5 C25 -0.7(4) . . . . ? C35 C36 N5 C25 178.9(3) . . . . ? C28 C36 N5 Ni1 175.8(2) . . . . ? C35 C36 N5 Ni1 -4.6(3) . . . . ? C33 C34 N6 C35 0.8(5) . . . . ? C33 C34 N6 Ni1 179.3(2) . . . . ? C31 C35 N6 C34 1.9(5) . . . . ? C36 C35 N6 C34 -176.6(3) . . . . ? C31 C35 N6 Ni1 -176.8(2) . . . . ? C36 C35 N6 Ni1 4.7(3) . . . . ? C25 N5 Ni1 N4 -4.8(3) . . . . ? C36 N5 Ni1 N4 179.2(2) . . . . ? C25 N5 Ni1 N6 -178.6(3) . . . . ? C36 N5 Ni1 N6 5.4(2) . . . . ? C25 N5 Ni1 N2 118.6(6) . . . . ? C36 N5 Ni1 N2 -57.4(7) . . . . ? C25 N5 Ni1 N3 -85.1(3) . . . . ? C36 N5 Ni1 N3 98.9(2) . . . . ? C25 N5 Ni1 N1 90.1(3) . . . . ? C36 N5 Ni1 N1 -85.8(2) . . . . ? C22 N4 Ni1 N5 88.5(3) . . . . ? C23 N4 Ni1 N5 -95.0(2) . . . . ? C22 N4 Ni1 N6 146.0(8) . . . . ? C23 N4 Ni1 N6 -37.4(9) . . . . ? C22 N4 Ni1 N2 -83.1(3) . . . . ? C23 N4 Ni1 N2 93.5(2) . . . . ? C22 N4 Ni1 N3 -178.3(3) . . . . ? C23 N4 Ni1 N3 -1.7(2) . . . . ? C22 N4 Ni1 N1 -3.3(3) . . . . ? C23 N4 Ni1 N1 173.2(2) . . . . ? C34 N6 Ni1 N5 176.1(3) . . . . ? C35 N6 Ni1 N5 -5.4(2) . . . . ? C34 N6 Ni1 N4 117.7(8) . . . . ? C35 N6 Ni1 N4 -63.8(9) . . . . ? C34 N6 Ni1 N2 -12.9(3) . . . . ? C35 N6 Ni1 N2 165.6(2) . . . . ? C34 N6 Ni1 N3 82.5(3) . . . . ? C35 N6 Ni1 N3 -99.0(2) . . . . ? C34 N6 Ni1 N1 -92.8(3) . . . . ? C35 N6 Ni1 N1 85.7(2) . . . . ? C10 N2 Ni1 N5 148.5(5) . . . . ? C11 N2 Ni1 N5 -33.4(7) . . . . ? C10 N2 Ni1 N4 -87.6(3) . . . . ? C11 N2 Ni1 N4 90.5(2) . . . . ? C10 N2 Ni1 N6 86.9(3) . . . . ? C11 N2 Ni1 N6 -95.0(2) . . . . ? C10 N2 Ni1 N3 -7.8(3) . . . . ? C11 N2 Ni1 N3 170.3(2) . . . . ? C10 N2 Ni1 N1 177.4(3) . . . . ? C11 N2 Ni1 N1 -4.5(2) . . . . ? C13 N3 Ni1 N5 -82.1(3) . . . . ? C24 N3 Ni1 N5 96.6(2) . . . . ? C13 N3 Ni1 N4 -177.4(3) . . . . ? C24 N3 Ni1 N4 1.3(2) . . . . ? C13 N3 Ni1 N6 -1.6(3) . . . . ? C24 N3 Ni1 N6 177.1(2) . . . . ? C13 N3 Ni1 N2 93.8(3) . . . . ? C24 N3 Ni1 N2 -87.4(2) . . . . ? C13 N3 Ni1 N1 138.6(7) . . . . ? C24 N3 Ni1 N1 -42.7(9) . . . . ? C1 N1 Ni1 N5 1.6(3) . . . . ? C12 N1 Ni1 N5 178.3(2) . . . . ? C1 N1 Ni1 N4 97.7(3) . . . . ? C12 N1 Ni1 N4 -85.6(2) . . . . ? C1 N1 Ni1 N6 -78.7(3) . . . . ? C12 N1 Ni1 N6 98.0(2) . . . . ? C1 N1 Ni1 N2 -173.5(3) . . . . ? C12 N1 Ni1 N2 3.2(2) . . . . ? C1 N1 Ni1 N3 141.0(8) . . . . ? C12 N1 Ni1 N3 -42.3(9) . . . . ? O3 C37 O2 Ta1 -173.1(3) . . . . ? C38 C37 O2 Ta1 8.2(4) . . . . ? O4 C38 O5 Ta1 -176.8(3) . . . . ? C37 C38 O5 Ta1 1.9(3) . . . . ? O7 C39 O6 Ta1 -173.5(3) . . . . ? C40 C39 O6 Ta1 3.8(4) . . . . ? O8 C40 O9 Ta1 176.7(3) . . . . ? C39 C40 O9 Ta1 -3.1(4) . . . . ? O11 C41 O10 Ta1 179.6(3) . . . . ? C42 C41 O10 Ta1 -1.9(4) . . . . ? O12 C42 O13 Ta1 173.8(3) . . . . ? C41 C42 O13 Ta1 -6.6(4) . . . . ? C40 O9 Ta1 O1 -88.0(3) . . . . ? C40 O9 Ta1 O10 171.1(3) . . . . ? C40 O9 Ta1 O2 88.4(3) . . . . ? C40 O9 Ta1 O13 173.1(2) . . . . ? C40 O9 Ta1 O5 16.1(3) . . . . ? C40 O9 Ta1 O6 3.8(2) . . . . ? C41 O10 Ta1 O1 84.3(3) . . . . ? C41 O10 Ta1 O9 177.8(3) . . . . ? C41 O10 Ta1 O2 -84.4(2) . . . . ? C41 O10 Ta1 O13 -1.0(2) . . . . ? C41 O10 Ta1 O5 -26.6(3) . . . . ? C41 O10 Ta1 O6 -162.6(2) . . . . ? C37 O2 Ta1 O1 15.5(6) . . . . ? C37 O2 Ta1 O9 -149.1(3) . . . . ? C37 O2 Ta1 O10 141.4(3) . . . . ? C37 O2 Ta1 O13 67.9(3) . . . . ? C37 O2 Ta1 O5 -5.7(2) . . . . ? C37 O2 Ta1 O6 -76.7(3) . . . . ? C42 O13 Ta1 O1 -99.0(2) . . . . ? C42 O13 Ta1 O9 2.6(3) . . . . ? C42 O13 Ta1 O10 4.5(2) . . . . ? C42 O13 Ta1 O2 91.7(2) . . . . ? C42 O13 Ta1 O5 168.2(3) . . . . ? C42 O13 Ta1 O6 165.4(2) . . . . ? C38 O5 Ta1 O1 -173.6(2) . . . . ? C38 O5 Ta1 O9 80.7(3) . . . . ? C38 O5 Ta1 O10 -59.4(3) . . . . ? C38 O5 Ta1 O2 1.5(2) . . . . ? C38 O5 Ta1 O13 -85.1(2) . . . . ? C38 O5 Ta1 O6 93.1(2) . . . . ? C39 O6 Ta1 O1 92.5(2) . . . . ? C39 O6 Ta1 O9 -4.2(2) . . . . ? C39 O6 Ta1 O10 -23.4(3) . . . . ? C39 O6 Ta1 O2 -101.2(2) . . . . ? C39 O6 Ta1 O13 -173.5(2) . . . . ? C39 O6 Ta1 O5 -176.3(3) . . . . ? data_3 _database_code_depnum_ccdc_archive 'CCDC 894041' #TrackingRef '12902_web_deposit_cif_file_2_LidijaAndros_1343389594.ccdc_deposit3.cif' _audit_creation_date 2012-05-24T16:01:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H31 N6 Ni O14 Ta' _chemical_formula_weight 1107.41 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5314(6) _cell_length_b 12.6938(6) _cell_length_c 15.6130(8) _cell_angle_alpha 108.324(4) _cell_angle_beta 92.332(4) _cell_angle_gamma 109.013(4) _cell_volume 2024.90(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13312 _cell_measurement_theta_min 4.1672 _cell_measurement_theta_max 32.5191 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.61679 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.3426 _diffrn_orient_matrix_ub_11 0.0346998641 _diffrn_orient_matrix_ub_12 -0.0231907575 _diffrn_orient_matrix_ub_13 0.0227187795 _diffrn_orient_matrix_ub_21 -0.0087446082 _diffrn_orient_matrix_ub_22 0.0356578866 _diffrn_orient_matrix_ub_23 0.0431962265 _diffrn_orient_matrix_ub_31 -0.0553797166 _diffrn_orient_matrix_ub_32 -0.046802142 _diffrn_orient_matrix_ub_33 -0.0011470077 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_number 43552 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 32.6 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.916 _reflns_number_total 13543 _reflns_number_gt 9568 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 13543 _refine_ls_number_parameters 604 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.053 _refine_ls_wR_factor_gt 0.0502 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.117 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0457(2) 0.6851(2) 0.33714(16) 0.0432(5) Uani 1 1 d . . . H1 H 1.0591 0.6959 0.2816 0.052 Uiso 1 1 calc R . . C2 C 1.1470(2) 0.7323(2) 0.40696(17) 0.0469(6) Uani 1 1 d . . . H2 H 1.2258 0.7729 0.3977 0.056 Uiso 1 1 calc R . . C3 C 1.1292(2) 0.71824(19) 0.48889(17) 0.0441(6) Uani 1 1 d . . . H3 H 1.1957 0.7501 0.5365 0.053 Uiso 1 1 calc R . . C4 C 1.0100(2) 0.65530(18) 0.50097(14) 0.0374(5) Uani 1 1 d . . . C5 C 0.9821(2) 0.6331(2) 0.58403(16) 0.0476(6) Uani 1 1 d . . . H5 H 1.0448 0.6651 0.6342 0.057 Uiso 1 1 calc R . . C6 C 0.8677(3) 0.5673(2) 0.59071(16) 0.0500(6) Uani 1 1 d . . . H6 H 0.8528 0.5541 0.6452 0.06 Uiso 1 1 calc R . . C7 C 0.7684(2) 0.51719(19) 0.51573(15) 0.0404(5) Uani 1 1 d . . . C8 C 0.6481(2) 0.4435(2) 0.51730(18) 0.0504(6) Uani 1 1 d . . . H8 H 0.6295 0.4241 0.5691 0.06 Uiso 1 1 calc R . . C9 C 0.5589(2) 0.4007(2) 0.44250(19) 0.0503(6) Uani 1 1 d . . . H9 H 0.4793 0.351 0.4427 0.06 Uiso 1 1 calc R . . C10 C 0.5874(2) 0.43147(19) 0.36563(17) 0.0429(5) Uani 1 1 d . . . H10 H 0.5249 0.4027 0.3157 0.051 Uiso 1 1 calc R . . C11 C 0.79050(19) 0.54093(17) 0.43473(14) 0.0324(4) Uani 1 1 d . . . C12 C 0.91287(19) 0.60987(17) 0.42708(14) 0.0319(4) Uani 1 1 d . . . C13 C 0.5070(2) 0.5181(2) 0.15196(16) 0.0452(6) Uani 1 1 d . . . H13 H 0.5157 0.5936 0.1911 0.054 Uiso 1 1 calc R . . C14 C 0.4039(2) 0.4571(3) 0.08411(18) 0.0564(7) Uani 1 1 d . . . H14 H 0.3461 0.4919 0.0772 0.068 Uiso 1 1 calc R . . C15 C 0.3886(2) 0.3465(3) 0.02809(18) 0.0615(8) Uani 1 1 d . . . H15 H 0.3187 0.3039 -0.0168 0.074 Uiso 1 1 calc R . . C16 C 0.4777(2) 0.2950(2) 0.03714(16) 0.0499(6) Uani 1 1 d . . . C17 C 0.4712(3) 0.1796(2) -0.01958(18) 0.0654(8) Uani 1 1 d . . . H17 H 0.4033 0.1328 -0.0656 0.078 Uiso 1 1 calc R . . C18 C 0.5605(3) 0.1371(2) -0.00810(18) 0.0619(8) Uani 1 1 d . . . H18 H 0.5528 0.0613 -0.0459 0.074 Uiso 1 1 calc R . . C19 C 0.6683(2) 0.20623(19) 0.06150(16) 0.0453(6) Uani 1 1 d . . . C20 C 0.7679(3) 0.1700(2) 0.07315(18) 0.0548(7) Uani 1 1 d . . . H20 H 0.7654 0.0952 0.0369 0.066 Uiso 1 1 calc R . . C21 C 0.8694(3) 0.2448(2) 0.13801(18) 0.0519(6) Uani 1 1 d . . . H21 H 0.9362 0.2214 0.1465 0.062 Uiso 1 1 calc R . . C22 C 0.8712(2) 0.3562(2) 0.19097(16) 0.0417(5) Uani 1 1 d . . . H22 H 0.9409 0.4066 0.2345 0.05 Uiso 1 1 calc R . . C23 C 0.6772(2) 0.31939(18) 0.11777(14) 0.0365(5) Uani 1 1 d . . . C24 C 0.58012(19) 0.36402(19) 0.10683(14) 0.0367(5) Uani 1 1 d . . . C25 C 0.8949(2) 0.5984(2) 0.09155(15) 0.0416(5) Uani 1 1 d . . . H25 H 0.8942 0.5211 0.0758 0.05 Uiso 1 1 calc R . . C26 C 0.9480(2) 0.6648(2) 0.03805(16) 0.0479(6) Uani 1 1 d . . . H26 H 0.981 0.6318 -0.0126 0.058 Uiso 1 1 calc R . . C27 C 0.9515(2) 0.7788(2) 0.06047(16) 0.0445(6) Uani 1 1 d . . . H27 H 0.9891 0.8251 0.0265 0.053 Uiso 1 1 calc R . . C28 C 0.89747(19) 0.82532(19) 0.13534(15) 0.0368(5) Uani 1 1 d . . . C29 C 0.8889(2) 0.9414(2) 0.16026(18) 0.0465(6) Uani 1 1 d . . . H29 H 0.9247 0.991 0.1281 0.056 Uiso 1 1 calc R . . C30 C 0.8298(2) 0.9790(2) 0.22934(18) 0.0487(6) Uani 1 1 d . . . H30 H 0.8244 1.0539 0.2435 0.058 Uiso 1 1 calc R . . C31 C 0.7750(2) 0.90668(19) 0.28185(15) 0.0396(5) Uani 1 1 d . . . C32 C 0.7099(2) 0.9400(2) 0.35410(16) 0.0477(6) Uani 1 1 d . . . H32 H 0.7034 1.0148 0.3721 0.057 Uiso 1 1 calc R . . C33 C 0.6567(2) 0.8631(2) 0.39751(17) 0.0515(6) Uani 1 1 d . . . H33 H 0.6114 0.8837 0.4438 0.062 Uiso 1 1 calc R . . C34 C 0.6707(2) 0.7533(2) 0.37171(16) 0.0436(5) Uani 1 1 d . . . H34 H 0.6346 0.7017 0.4023 0.052 Uiso 1 1 calc R . . C35 C 0.78336(18) 0.79354(17) 0.26006(14) 0.0327(5) Uani 1 1 d . . . C36 C 0.84495(17) 0.75240(17) 0.18495(13) 0.0309(4) Uani 1 1 d . . . C43 C 0.1082(2) -0.0105(2) 0.38892(18) 0.0551(7) Uani 1 1 d . . . H43A H 0.1626 -0.0163 0.4349 0.066 Uiso 1 1 calc R . . H43B H 0.0267 -0.0701 0.3813 0.066 Uiso 1 1 calc R . . C44 C 0.0985(3) 0.1093(2) 0.4213(2) 0.0706(8) Uani 1 1 d . . . H44A H 0.1793 0.1687 0.4302 0.106 Uiso 1 1 calc R . . H44B H 0.0666 0.1215 0.478 0.106 Uiso 1 1 calc R . . H44C H 0.0435 0.1149 0.3765 0.106 Uiso 1 1 calc R . . C37 C 0.5606(2) 0.11715(19) 0.29575(16) 0.0393(5) Uani 1 1 d . . . C38 C 0.5134(2) 0.11924(18) 0.38755(15) 0.0367(5) Uani 1 1 d . . . C39 C 0.3336(2) -0.2315(2) 0.23193(18) 0.0501(6) Uani 1 1 d . . . C40 C 0.2584(2) -0.2560(2) 0.14079(17) 0.0475(6) Uani 1 1 d . . . C41 C 0.2100(2) 0.1201(2) 0.14005(19) 0.0548(7) Uani 1 1 d . . . C42 C 0.2754(2) 0.2185(2) 0.23052(18) 0.0493(6) Uani 1 1 d . . . N1 N 0.93128(15) 0.62586(14) 0.34565(11) 0.0333(4) Uani 1 1 d . . . N2 N 0.70004(15) 0.50010(14) 0.36070(12) 0.0345(4) Uani 1 1 d . . . N3 N 0.59415(16) 0.47439(16) 0.16397(12) 0.0381(4) Uani 1 1 d . . . N4 N 0.77811(16) 0.39443(15) 0.18267(12) 0.0343(4) Uani 1 1 d . . . N5 N 0.84507(15) 0.63992(15) 0.16409(11) 0.0329(4) Uani 1 1 d . . . N6 N 0.73336(16) 0.71847(15) 0.30548(11) 0.0348(4) Uani 1 1 d . . . Ni1 Ni 0.76313(2) 0.55676(2) 0.253500(17) 0.03134(6) Uani 1 1 d . . . O1 O 0.15485(13) -0.03458(13) 0.30477(10) 0.0422(4) Uani 1 1 d . . . O2 O 0.47072(14) 0.05927(14) 0.22563(10) 0.0445(4) Uani 1 1 d . . . O3 O 0.66800(15) 0.16406(16) 0.29148(13) 0.0597(5) Uani 1 1 d . . . O5 O 0.39355(13) 0.08218(12) 0.37934(9) 0.0373(3) Uani 1 1 d . . . O4 O 0.58431(15) 0.15407(16) 0.45798(11) 0.0558(5) Uani 1 1 d . . . O6 O 0.35465(16) -0.12507(14) 0.28712(11) 0.0539(4) Uani 1 1 d . . . O7 O 0.3642(2) -0.30676(17) 0.24866(15) 0.0801(6) Uani 1 1 d . . . O9 O 0.23613(15) -0.16131(14) 0.13952(11) 0.0501(4) Uani 1 1 d . . . O8 O 0.2232(2) -0.35034(16) 0.07952(14) 0.0744(6) Uani 1 1 d . . . O10 O 0.21781(16) 0.01859(14) 0.13691(11) 0.0518(4) Uani 1 1 d . . . O11 O 0.1560(2) 0.13384(19) 0.07945(16) 0.0995(8) Uani 1 1 d . . . O13 O 0.31315(16) 0.17696(13) 0.28752(11) 0.0514(4) Uani 1 1 d . . . O12 O 0.2901(2) 0.32212(16) 0.24550(14) 0.0728(6) Uani 1 1 d . . . O14 O 0.1569(2) 0.4557(2) 0.19702(17) 0.0753(6) Uani 1 1 d D . . Ta1 Ta 0.293181(8) -0.004882(8) 0.247926(6) 0.03532(3) Uani 1 1 d . . . H14A H 0.215(3) 0.5264(19) 0.210(3) 0.120(16) Uiso 1 1 d D . . H14B H 0.200(3) 0.409(3) 0.199(3) 0.126(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0360(12) 0.0485(13) 0.0400(13) 0.0144(11) 0.0034(10) 0.0098(10) C2 0.0324(12) 0.0448(13) 0.0518(15) 0.0106(12) -0.0017(11) 0.0059(10) C3 0.0359(12) 0.0388(12) 0.0467(14) 0.0041(11) -0.0097(10) 0.0117(10) C4 0.0447(13) 0.0318(10) 0.0321(11) 0.0025(9) -0.0038(10) 0.0184(9) C5 0.0607(16) 0.0490(14) 0.0316(12) 0.0072(11) -0.0047(11) 0.0257(12) C6 0.0721(18) 0.0549(15) 0.0336(13) 0.0187(12) 0.0100(12) 0.0328(13) C7 0.0516(14) 0.0396(12) 0.0375(12) 0.0138(10) 0.0130(11) 0.0247(10) C8 0.0657(17) 0.0485(14) 0.0483(15) 0.0232(12) 0.0243(13) 0.0269(12) C9 0.0471(15) 0.0413(13) 0.0657(18) 0.0203(13) 0.0248(13) 0.0163(11) C10 0.0364(12) 0.0386(12) 0.0483(14) 0.0099(11) 0.0070(11) 0.0116(10) C11 0.0381(12) 0.0286(10) 0.0318(11) 0.0075(9) 0.0058(9) 0.0161(8) C12 0.0358(11) 0.0307(10) 0.0286(11) 0.0049(9) 0.0017(9) 0.0167(9) C13 0.0335(12) 0.0577(14) 0.0446(14) 0.0156(12) 0.0022(10) 0.0190(10) C14 0.0363(13) 0.085(2) 0.0507(16) 0.0260(15) 0.0006(12) 0.0237(13) C15 0.0327(13) 0.089(2) 0.0463(15) 0.0195(15) -0.0079(11) 0.0063(13) C16 0.0385(13) 0.0562(15) 0.0368(13) 0.0095(12) 0.0010(10) 0.0008(11) C17 0.0548(17) 0.0597(17) 0.0436(15) -0.0019(13) -0.0066(13) -0.0071(14) C18 0.075(2) 0.0366(13) 0.0440(15) -0.0032(12) 0.0130(14) -0.0024(13) C19 0.0593(16) 0.0341(11) 0.0353(12) 0.0089(10) 0.0154(11) 0.0096(11) C20 0.082(2) 0.0389(13) 0.0496(15) 0.0143(12) 0.0285(15) 0.0281(13) C21 0.0709(18) 0.0545(15) 0.0524(16) 0.0264(13) 0.0259(14) 0.0412(14) C22 0.0470(13) 0.0449(13) 0.0396(13) 0.0170(11) 0.0099(10) 0.0219(10) C23 0.0412(12) 0.0335(11) 0.0297(11) 0.0091(9) 0.0070(9) 0.0084(9) C24 0.0327(11) 0.0398(12) 0.0296(11) 0.0084(9) 0.0036(9) 0.0063(9) C25 0.0427(13) 0.0464(13) 0.0343(12) 0.0085(10) 0.0056(10) 0.0195(10) C26 0.0464(14) 0.0677(16) 0.0360(13) 0.0183(12) 0.0144(11) 0.0272(12) C27 0.0348(12) 0.0629(15) 0.0431(14) 0.0282(12) 0.0068(10) 0.0170(11) C28 0.0279(11) 0.0454(12) 0.0362(12) 0.0150(10) 0.0000(9) 0.0117(9) C29 0.0429(14) 0.0472(13) 0.0535(15) 0.0261(12) 0.0049(12) 0.0137(11) C30 0.0519(14) 0.0371(12) 0.0578(16) 0.0167(12) 0.0003(12) 0.0174(11) C31 0.0388(12) 0.0384(11) 0.0378(12) 0.0064(10) -0.0040(10) 0.0167(9) C32 0.0557(15) 0.0439(13) 0.0435(14) 0.0043(11) 0.0018(12) 0.0289(11) C33 0.0584(16) 0.0623(16) 0.0375(13) 0.0076(12) 0.0117(12) 0.0351(13) C34 0.0486(14) 0.0476(13) 0.0350(12) 0.0113(11) 0.0102(11) 0.0202(11) C35 0.0295(11) 0.0344(10) 0.0295(11) 0.0065(9) -0.0022(8) 0.0107(8) C36 0.0251(10) 0.0372(11) 0.0267(10) 0.0077(9) -0.0033(8) 0.0105(8) C43 0.0522(16) 0.0555(15) 0.0512(16) 0.0100(13) 0.0110(13) 0.0189(12) C44 0.077(2) 0.0659(18) 0.0660(19) 0.0045(16) 0.0112(16) 0.0394(16) C37 0.0339(12) 0.0405(12) 0.0456(13) 0.0155(11) 0.0058(10) 0.0156(10) C38 0.0340(12) 0.0313(10) 0.0408(13) 0.0093(10) -0.0015(10) 0.0107(9) C39 0.0514(15) 0.0431(13) 0.0541(16) 0.0112(12) 0.0060(12) 0.0207(11) C40 0.0475(14) 0.0423(13) 0.0448(14) 0.0060(11) 0.0054(11) 0.0151(11) C41 0.0532(16) 0.0540(15) 0.0587(17) 0.0296(14) -0.0054(13) 0.0130(12) C42 0.0493(15) 0.0447(14) 0.0561(16) 0.0179(12) 0.0043(12) 0.0199(11) N1 0.0301(9) 0.0341(9) 0.0300(9) 0.0066(8) 0.0004(7) 0.0090(7) N2 0.0313(9) 0.0334(9) 0.0363(10) 0.0085(8) 0.0049(8) 0.0119(7) N3 0.0319(10) 0.0437(10) 0.0339(10) 0.0086(8) 0.0004(8) 0.0125(8) N4 0.0353(10) 0.0349(9) 0.0325(10) 0.0103(8) 0.0041(8) 0.0139(7) N5 0.0341(9) 0.0372(9) 0.0252(9) 0.0059(7) 0.0024(7) 0.0148(7) N6 0.0370(10) 0.0375(9) 0.0275(9) 0.0066(8) 0.0037(8) 0.0152(8) Ni1 0.03011(14) 0.03227(13) 0.02779(14) 0.00575(11) 0.00072(11) 0.01119(11) O1 0.0355(8) 0.0452(9) 0.0402(9) 0.0072(7) 0.0031(7) 0.0148(7) O2 0.0383(9) 0.0558(10) 0.0357(9) 0.0138(8) 0.0088(7) 0.0137(7) O3 0.0350(10) 0.0762(12) 0.0666(12) 0.0303(10) 0.0106(9) 0.0125(9) O5 0.0336(8) 0.0407(8) 0.0301(8) 0.0051(7) 0.0006(6) 0.0113(6) O4 0.0440(10) 0.0695(11) 0.0423(10) 0.0144(9) -0.0096(8) 0.0121(8) O6 0.0719(12) 0.0428(9) 0.0428(10) 0.0044(8) -0.0109(9) 0.0277(8) O7 0.1094(17) 0.0564(11) 0.0779(14) 0.0117(11) -0.0100(13) 0.0482(12) O9 0.0592(11) 0.0434(9) 0.0387(9) 0.0013(7) -0.0089(8) 0.0211(8) O8 0.0948(15) 0.0432(10) 0.0654(13) -0.0067(10) -0.0101(11) 0.0265(10) O10 0.0656(11) 0.0443(9) 0.0387(9) 0.0096(8) -0.0104(8) 0.0177(8) O11 0.125(2) 0.0750(14) 0.0913(17) 0.0421(13) -0.0441(15) 0.0209(13) O13 0.0633(11) 0.0385(9) 0.0464(10) 0.0066(8) -0.0099(8) 0.0204(8) O12 0.0965(16) 0.0480(11) 0.0802(14) 0.0256(11) 0.0015(12) 0.0320(10) O14 0.0679(14) 0.0867(16) 0.0922(17) 0.0471(15) 0.0290(13) 0.0368(14) Ta1 0.03400(5) 0.03513(5) 0.03198(5) 0.00610(4) -0.00133(3) 0.01230(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.325(3) . ? C1 C2 1.393(3) . ? C1 H1 0.93 . ? C2 C3 1.360(3) . ? C2 H2 0.93 . ? C3 C4 1.401(3) . ? C3 H3 0.93 . ? C4 C12 1.405(3) . ? C4 C5 1.439(3) . ? C5 C6 1.340(3) . ? C5 H5 0.93 . ? C6 C7 1.426(3) . ? C6 H6 0.93 . ? C7 C8 1.404(3) . ? C7 C11 1.404(3) . ? C8 C9 1.363(4) . ? C8 H8 0.93 . ? C9 C10 1.394(3) . ? C9 H9 0.93 . ? C10 N2 1.329(3) . ? C10 H10 0.93 . ? C11 N2 1.366(3) . ? C11 C12 1.430(3) . ? C12 N1 1.363(3) . ? C13 N3 1.330(3) . ? C13 C14 1.384(3) . ? C13 H13 0.93 . ? C14 C15 1.350(4) . ? C14 H14 0.93 . ? C15 C16 1.410(4) . ? C15 H15 0.93 . ? C16 C24 1.403(3) . ? C16 C17 1.430(4) . ? C17 C18 1.338(4) . ? C17 H17 0.93 . ? C18 C19 1.441(4) . ? C18 H18 0.93 . ? C19 C20 1.394(4) . ? C19 C23 1.396(3) . ? C20 C21 1.368(4) . ? C20 H20 0.93 . ? C21 C22 1.388(3) . ? C21 H21 0.93 . ? C22 N4 1.331(3) . ? C22 H22 0.93 . ? C23 N4 1.365(3) . ? C23 C24 1.436(3) . ? C24 N3 1.356(3) . ? C25 N5 1.329(3) . ? C25 C26 1.390(3) . ? C25 H25 0.93 . ? C26 C27 1.365(3) . ? C26 H26 0.93 . ? C27 C28 1.403(3) . ? C27 H27 0.93 . ? C28 C36 1.395(3) . ? C28 C29 1.439(3) . ? C29 C30 1.343(3) . ? C29 H29 0.93 . ? C30 C31 1.433(3) . ? C30 H30 0.93 . ? C31 C35 1.405(3) . ? C31 C32 1.411(3) . ? C32 C33 1.360(3) . ? C32 H32 0.93 . ? C33 C34 1.390(3) . ? C33 H33 0.93 . ? C34 N6 1.330(3) . ? C34 H34 0.93 . ? C35 N6 1.358(3) . ? C35 C36 1.441(3) . ? C36 N5 1.361(2) . ? C43 O1 1.422(3) . ? C43 C44 1.487(4) . ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? C44 H44A 0.96 . ? C44 H44B 0.96 . ? C44 H44C 0.96 . ? C37 O3 1.202(3) . ? C37 O2 1.311(3) . ? C37 C38 1.549(3) . ? C38 O4 1.208(2) . ? C38 O5 1.293(2) . ? C39 O7 1.214(3) . ? C39 O6 1.290(3) . ? C39 C40 1.523(3) . ? C40 O8 1.202(3) . ? C40 O9 1.314(3) . ? C41 O11 1.200(3) . ? C41 O10 1.306(3) . ? C41 C42 1.522(4) . ? C42 O12 1.213(3) . ? C42 O13 1.293(3) . ? N1 Ni1 2.1144(16) . ? N2 Ni1 2.0888(18) . ? N3 Ni1 2.0918(17) . ? N4 Ni1 2.0769(17) . ? N5 Ni1 2.0832(17) . ? N6 Ni1 2.1033(17) . ? O1 Ta1 1.8461(15) . ? O2 Ta1 2.0312(15) . ? O5 Ta1 2.0780(14) . ? O6 Ta1 2.1120(16) . ? O9 Ta1 2.0458(15) . ? O10 Ta1 2.0542(16) . ? O13 Ta1 2.1232(15) . ? O14 H14A 0.881(18) . ? O14 H14B 0.899(18) . ? 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 C1 C2 123.5(2) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.2(2) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C12 117.9(2) . . ? C3 C4 C5 123.8(2) . . ? C12 C4 C5 118.3(2) . . ? C6 C5 C4 121.5(2) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 121.2(2) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C11 117.1(2) . . ? C8 C7 C6 123.8(2) . . ? C11 C7 C6 119.1(2) . . ? C9 C8 C7 119.6(2) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.8(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 122.8(2) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 123.1(2) . . ? N2 C11 C12 117.16(19) . . ? C7 C11 C12 119.76(19) . . ? N1 C12 C4 122.20(19) . . ? N1 C12 C11 117.71(18) . . ? C4 C12 C11 120.1(2) . . ? N3 C13 C14 123.3(2) . . ? N3 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C15 C14 C13 119.0(2) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C24 C16 C15 116.6(2) . . ? C24 C16 C17 118.5(2) . . ? C15 C16 C17 124.8(2) . . ? C18 C17 C16 121.6(2) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 121.5(2) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C23 117.6(2) . . ? C20 C19 C18 124.1(2) . . ? C23 C19 C18 118.2(2) . . ? C21 C20 C19 119.8(2) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 119.0(2) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N4 C22 C21 123.3(2) . . ? N4 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N4 C23 C19 122.9(2) . . ? N4 C23 C24 116.62(18) . . ? C19 C23 C24 120.4(2) . . ? N3 C24 C16 122.7(2) . . ? N3 C24 C23 117.50(18) . . ? C16 C24 C23 119.8(2) . . ? N5 C25 C26 123.2(2) . . ? N5 C25 H25 118.4 . . ? C26 C25 H25 118.4 . . ? C27 C26 C25 119.4(2) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 119.2(2) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C36 C28 C27 117.7(2) . . ? C36 C28 C29 119.0(2) . . ? C27 C28 C29 123.2(2) . . ? C30 C29 C28 120.8(2) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 121.7(2) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C35 C31 C32 116.7(2) . . ? C35 C31 C30 118.9(2) . . ? C32 C31 C30 124.5(2) . . ? C33 C32 C31 120.1(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 119.1(2) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? N6 C34 C33 123.2(2) . . ? N6 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? N6 C35 C31 123.0(2) . . ? N6 C35 C36 117.51(18) . . ? C31 C35 C36 119.5(2) . . ? N5 C36 C28 122.90(19) . . ? N5 C36 C35 116.94(18) . . ? C28 C36 C35 120.13(19) . . ? O1 C43 C44 112.4(2) . . ? O1 C43 H43A 109.1 . . ? C44 C43 H43A 109.1 . . ? O1 C43 H43B 109.1 . . ? C44 C43 H43B 109.1 . . ? H43A C43 H43B 107.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O3 C37 O2 125.2(2) . . ? O3 C37 C38 122.5(2) . . ? O2 C37 C38 112.25(18) . . ? O4 C38 O5 125.6(2) . . ? O4 C38 C37 121.6(2) . . ? O5 C38 C37 112.78(18) . . ? O7 C39 O6 126.3(2) . . ? O7 C39 C40 122.2(2) . . ? O6 C39 C40 111.4(2) . . ? O8 C40 O9 125.3(2) . . ? O8 C40 C39 123.8(2) . . ? O9 C40 C39 110.8(2) . . ? O11 C41 O10 124.1(3) . . ? O11 C41 C42 123.9(3) . . ? O10 C41 C42 112.0(2) . . ? O12 C42 O13 125.4(2) . . ? O12 C42 C41 123.4(2) . . ? O13 C42 C41 111.2(2) . . ? C1 N1 C12 117.76(18) . . ? C1 N1 Ni1 130.10(15) . . ? C12 N1 Ni1 112.04(13) . . ? C10 N2 C11 117.59(19) . . ? C10 N2 Ni1 129.26(15) . . ? C11 N2 Ni1 113.16(13) . . ? C13 N3 C24 117.84(18) . . ? C13 N3 Ni1 129.27(16) . . ? C24 N3 Ni1 112.68(14) . . ? C22 N4 C23 117.31(19) . . ? C22 N4 Ni1 129.35(15) . . ? C23 N4 Ni1 113.33(14) . . ? C25 N5 C36 117.51(19) . . ? C25 N5 Ni1 129.27(15) . . ? C36 N5 Ni1 113.22(13) . . ? C34 N6 C35 117.85(19) . . ? C34 N6 Ni1 129.68(16) . . ? C35 N6 Ni1 112.42(13) . . ? N4 Ni1 N5 95.02(7) . . ? N4 Ni1 N2 92.02(7) . . ? N5 Ni1 N2 170.23(6) . . ? N4 Ni1 N3 79.82(7) . . ? N5 Ni1 N3 90.70(7) . . ? N2 Ni1 N3 97.22(7) . . ? N4 Ni1 N6 170.96(7) . . ? N5 Ni1 N6 79.79(7) . . ? N2 Ni1 N6 94.07(7) . . ? N3 Ni1 N6 92.76(7) . . ? N4 Ni1 N1 96.50(7) . . ? N5 Ni1 N1 92.93(7) . . ? N2 Ni1 N1 79.52(7) . . ? N3 Ni1 N1 175.05(7) . . ? N6 Ni1 N1 91.19(6) . . ? C43 O1 Ta1 146.05(15) . . ? C37 O2 Ta1 119.17(14) . . ? C38 O5 Ta1 117.44(13) . . ? C39 O6 Ta1 121.66(15) . . ? C40 O9 Ta1 123.50(15) . . ? C41 O10 Ta1 122.54(15) . . ? C42 O13 Ta1 121.08(15) . . ? H14A O14 H14B 103(3) . . ? O1 Ta1 O2 162.29(6) . . ? O1 Ta1 O9 98.36(7) . . ? O2 Ta1 O9 97.30(7) . . ? O1 Ta1 O10 98.89(7) . . ? O2 Ta1 O10 94.03(7) . . ? O9 Ta1 O10 70.75(6) . . ? O1 Ta1 O5 85.50(6) . . ? O2 Ta1 O5 76.96(6) . . ? O9 Ta1 O5 144.00(6) . . ? O10 Ta1 O5 144.34(6) . . ? O1 Ta1 O6 93.02(7) . . ? O2 Ta1 O6 83.84(7) . . ? O9 Ta1 O6 72.57(6) . . ? O10 Ta1 O6 142.66(6) . . ? O5 Ta1 O6 71.49(6) . . ? O1 Ta1 O13 90.00(7) . . ? O2 Ta1 O13 82.25(7) . . ? O9 Ta1 O13 143.48(7) . . ? O10 Ta1 O13 72.86(6) . . ? O5 Ta1 O13 71.77(6) . . ? O6 Ta1 O13 142.76(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.4(4) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C2 C3 C4 C12 -0.5(3) . . . . ? C2 C3 C4 C5 178.5(2) . . . . ? C3 C4 C5 C6 -176.6(2) . . . . ? C12 C4 C5 C6 2.4(3) . . . . ? C4 C5 C6 C7 -0.5(4) . . . . ? C5 C6 C7 C8 177.2(2) . . . . ? C5 C6 C7 C11 -2.2(3) . . . . ? C11 C7 C8 C9 -1.2(3) . . . . ? C6 C7 C8 C9 179.4(2) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C8 C9 C10 N2 1.3(4) . . . . ? C8 C7 C11 N2 2.9(3) . . . . ? C6 C7 C11 N2 -177.69(19) . . . . ? C8 C7 C11 C12 -176.48(19) . . . . ? C6 C7 C11 C12 3.0(3) . . . . ? C3 C4 C12 N1 -0.4(3) . . . . ? C5 C4 C12 N1 -179.46(19) . . . . ? C3 C4 C12 C11 177.49(18) . . . . ? C5 C4 C12 C11 -1.6(3) . . . . ? N2 C11 C12 N1 -2.5(3) . . . . ? C7 C11 C12 N1 176.91(18) . . . . ? N2 C11 C12 C4 179.54(17) . . . . ? C7 C11 C12 C4 -1.1(3) . . . . ? N3 C13 C14 C15 1.5(4) . . . . ? C13 C14 C15 C16 -1.5(4) . . . . ? C14 C15 C16 C24 0.5(4) . . . . ? C14 C15 C16 C17 -178.9(3) . . . . ? C24 C16 C17 C18 -0.6(4) . . . . ? C15 C16 C17 C18 178.8(3) . . . . ? C16 C17 C18 C19 -0.6(4) . . . . ? C17 C18 C19 C20 -175.9(3) . . . . ? C17 C18 C19 C23 0.5(4) . . . . ? C23 C19 C20 C21 0.0(4) . . . . ? C18 C19 C20 C21 176.3(2) . . . . ? C19 C20 C21 C22 -0.2(4) . . . . ? C20 C21 C22 N4 0.6(4) . . . . ? C20 C19 C23 N4 0.0(3) . . . . ? C18 C19 C23 N4 -176.6(2) . . . . ? C20 C19 C23 C24 177.5(2) . . . . ? C18 C19 C23 C24 0.9(3) . . . . ? C15 C16 C24 N3 0.6(4) . . . . ? C17 C16 C24 N3 -180.0(2) . . . . ? C15 C16 C24 C23 -177.5(2) . . . . ? C17 C16 C24 C23 2.0(3) . . . . ? N4 C23 C24 N3 -2.6(3) . . . . ? C19 C23 C24 N3 179.7(2) . . . . ? N4 C23 C24 C16 175.5(2) . . . . ? C19 C23 C24 C16 -2.1(3) . . . . ? N5 C25 C26 C27 0.8(3) . . . . ? C25 C26 C27 C28 -2.1(3) . . . . ? C26 C27 C28 C36 1.5(3) . . . . ? C26 C27 C28 C29 -175.6(2) . . . . ? C36 C28 C29 C30 -1.0(3) . . . . ? C27 C28 C29 C30 176.1(2) . . . . ? C28 C29 C30 C31 1.1(3) . . . . ? C29 C30 C31 C35 -0.1(3) . . . . ? C29 C30 C31 C32 -178.9(2) . . . . ? C35 C31 C32 C33 -1.5(3) . . . . ? C30 C31 C32 C33 177.3(2) . . . . ? C31 C32 C33 C34 2.1(4) . . . . ? C32 C33 C34 N6 -0.6(4) . . . . ? C32 C31 C35 N6 -0.6(3) . . . . ? C30 C31 C35 N6 -179.43(19) . . . . ? C32 C31 C35 C36 177.92(18) . . . . ? C30 C31 C35 C36 -0.9(3) . . . . ? C27 C28 C36 N5 0.5(3) . . . . ? C29 C28 C36 N5 177.70(18) . . . . ? C27 C28 C36 C35 -177.27(18) . . . . ? C29 C28 C36 C35 -0.1(3) . . . . ? N6 C35 C36 N5 1.7(3) . . . . ? C31 C35 C36 N5 -176.90(17) . . . . ? N6 C35 C36 C28 179.61(18) . . . . ? C31 C35 C36 C28 1.0(3) . . . . ? O3 C37 C38 O4 -10.2(3) . . . . ? O2 C37 C38 O4 169.8(2) . . . . ? O3 C37 C38 O5 168.8(2) . . . . ? O2 C37 C38 O5 -11.2(3) . . . . ? O7 C39 C40 O8 0.6(4) . . . . ? O6 C39 C40 O8 -177.1(2) . . . . ? O7 C39 C40 O9 179.5(3) . . . . ? O6 C39 C40 O9 1.8(3) . . . . ? O11 C41 C42 O12 -8.2(5) . . . . ? O10 C41 C42 O12 172.9(2) . . . . ? O11 C41 C42 O13 172.3(3) . . . . ? O10 C41 C42 O13 -6.6(3) . . . . ? C2 C1 N1 C12 -0.5(3) . . . . ? C2 C1 N1 Ni1 175.54(17) . . . . ? C4 C12 N1 C1 0.9(3) . . . . ? C11 C12 N1 C1 -177.03(18) . . . . ? C4 C12 N1 Ni1 -175.83(15) . . . . ? C11 C12 N1 Ni1 6.2(2) . . . . ? C9 C10 N2 C11 0.2(3) . . . . ? C9 C10 N2 Ni1 179.87(16) . . . . ? C7 C11 N2 C10 -2.4(3) . . . . ? C12 C11 N2 C10 176.99(18) . . . . ? C7 C11 N2 Ni1 177.93(15) . . . . ? C12 C11 N2 Ni1 -2.7(2) . . . . ? C14 C13 N3 C24 -0.4(4) . . . . ? C14 C13 N3 Ni1 173.89(18) . . . . ? C16 C24 N3 C13 -0.7(3) . . . . ? C23 C24 N3 C13 177.5(2) . . . . ? C16 C24 N3 Ni1 -175.88(17) . . . . ? C23 C24 N3 Ni1 2.2(2) . . . . ? C21 C22 N4 C23 -0.6(3) . . . . ? C21 C22 N4 Ni1 -179.31(17) . . . . ? C19 C23 N4 C22 0.4(3) . . . . ? C24 C23 N4 C22 -177.25(19) . . . . ? C19 C23 N4 Ni1 179.25(17) . . . . ? C24 C23 N4 Ni1 1.6(2) . . . . ? C26 C25 N5 C36 1.2(3) . . . . ? C26 C25 N5 Ni1 -179.28(16) . . . . ? C28 C36 N5 C25 -1.9(3) . . . . ? C35 C36 N5 C25 176.00(17) . . . . ? C28 C36 N5 Ni1 178.57(15) . . . . ? C35 C36 N5 Ni1 -3.6(2) . . . . ? C33 C34 N6 C35 -1.4(3) . . . . ? C33 C34 N6 Ni1 -178.52(17) . . . . ? C31 C35 N6 C34 2.0(3) . . . . ? C36 C35 N6 C34 -176.53(18) . . . . ? C31 C35 N6 Ni1 179.61(15) . . . . ? C36 C35 N6 Ni1 1.1(2) . . . . ? C22 N4 Ni1 N5 88.54(19) . . . . ? C23 N4 Ni1 N5 -90.17(15) . . . . ? C22 N4 Ni1 N2 -84.67(19) . . . . ? C23 N4 Ni1 N2 96.62(15) . . . . ? C22 N4 Ni1 N3 178.4(2) . . . . ? C23 N4 Ni1 N3 -0.35(14) . . . . ? C22 N4 Ni1 N6 143.1(4) . . . . ? C23 N4 Ni1 N6 -35.6(5) . . . . ? C22 N4 Ni1 N1 -5.0(2) . . . . ? C23 N4 Ni1 N1 176.30(14) . . . . ? C25 N5 Ni1 N4 -3.85(18) . . . . ? C36 N5 Ni1 N4 175.67(13) . . . . ? C25 N5 Ni1 N2 132.0(4) . . . . ? C36 N5 Ni1 N2 -48.5(4) . . . . ? C25 N5 Ni1 N3 -83.69(18) . . . . ? C36 N5 Ni1 N3 95.82(13) . . . . ? C25 N5 Ni1 N6 -176.37(18) . . . . ? C36 N5 Ni1 N6 3.14(13) . . . . ? C25 N5 Ni1 N1 92.94(18) . . . . ? C36 N5 Ni1 N1 -87.54(13) . . . . ? C10 N2 Ni1 N4 -78.87(18) . . . . ? C11 N2 Ni1 N4 100.79(14) . . . . ? C10 N2 Ni1 N5 145.1(3) . . . . ? C11 N2 Ni1 N5 -35.3(5) . . . . ? C10 N2 Ni1 N3 1.12(19) . . . . ? C11 N2 Ni1 N3 -179.22(13) . . . . ? C10 N2 Ni1 N6 94.43(18) . . . . ? C11 N2 Ni1 N6 -85.91(14) . . . . ? C10 N2 Ni1 N1 -175.11(19) . . . . ? C11 N2 Ni1 N1 4.55(13) . . . . ? C13 N3 Ni1 N4 -175.6(2) . . . . ? C24 N3 Ni1 N4 -1.02(15) . . . . ? C13 N3 Ni1 N5 -80.6(2) . . . . ? C24 N3 Ni1 N5 93.96(15) . . . . ? C13 N3 Ni1 N2 93.7(2) . . . . ? C24 N3 Ni1 N2 -91.78(15) . . . . ? C13 N3 Ni1 N6 -0.8(2) . . . . ? C24 N3 Ni1 N6 173.77(15) . . . . ? C13 N3 Ni1 N1 142.2(7) . . . . ? C24 N3 Ni1 N1 -43.3(9) . . . . ? C34 N6 Ni1 N4 119.5(4) . . . . ? C35 N6 Ni1 N4 -57.8(5) . . . . ? C34 N6 Ni1 N5 175.00(19) . . . . ? C35 N6 Ni1 N5 -2.25(13) . . . . ? C34 N6 Ni1 N2 -12.66(19) . . . . ? C35 N6 Ni1 N2 170.09(13) . . . . ? C34 N6 Ni1 N3 84.78(19) . . . . ? C35 N6 Ni1 N3 -92.47(14) . . . . ? C34 N6 Ni1 N1 -92.24(19) . . . . ? C35 N6 Ni1 N1 90.51(14) . . . . ? C1 N1 Ni1 N4 87.15(19) . . . . ? C12 N1 Ni1 N4 -96.62(14) . . . . ? C1 N1 Ni1 N5 -8.24(19) . . . . ? C12 N1 Ni1 N5 167.99(13) . . . . ? C1 N1 Ni1 N2 178.00(19) . . . . ? C12 N1 Ni1 N2 -5.76(13) . . . . ? C1 N1 Ni1 N3 128.9(8) . . . . ? C12 N1 Ni1 N3 -54.9(8) . . . . ? C1 N1 Ni1 N6 -88.08(19) . . . . ? C12 N1 Ni1 N6 88.15(14) . . . . ? C44 C43 O1 Ta1 75.0(3) . . . . ? O3 C37 O2 Ta1 -176.16(18) . . . . ? C38 C37 O2 Ta1 3.8(2) . . . . ? O4 C38 O5 Ta1 -167.63(18) . . . . ? C37 C38 O5 Ta1 13.4(2) . . . . ? O7 C39 O6 Ta1 -179.3(2) . . . . ? C40 C39 O6 Ta1 -1.7(3) . . . . ? O8 C40 O9 Ta1 177.7(2) . . . . ? C39 C40 O9 Ta1 -1.2(3) . . . . ? O11 C41 O10 Ta1 -172.5(2) . . . . ? C42 C41 O10 Ta1 6.4(3) . . . . ? O12 C42 O13 Ta1 -175.1(2) . . . . ? C41 C42 O13 Ta1 4.4(3) . . . . ? C43 O1 Ta1 O2 0.6(4) . . . . ? C43 O1 Ta1 O9 152.6(3) . . . . ? C43 O1 Ta1 O10 -135.7(3) . . . . ? C43 O1 Ta1 O5 8.6(3) . . . . ? C43 O1 Ta1 O6 79.8(3) . . . . ? C43 O1 Ta1 O13 -63.1(3) . . . . ? C37 O2 Ta1 O1 10.3(3) . . . . ? C37 O2 Ta1 O9 -141.77(16) . . . . ? C37 O2 Ta1 O10 147.15(16) . . . . ? C37 O2 Ta1 O5 2.09(15) . . . . ? C37 O2 Ta1 O6 -70.29(16) . . . . ? C37 O2 Ta1 O13 75.07(16) . . . . ? C40 O9 Ta1 O1 -90.22(19) . . . . ? C40 O9 Ta1 O2 81.50(19) . . . . ? C40 O9 Ta1 O10 173.2(2) . . . . ? C40 O9 Ta1 O5 3.7(2) . . . . ? C40 O9 Ta1 O6 0.34(18) . . . . ? C40 O9 Ta1 O13 168.32(16) . . . . ? C41 O10 Ta1 O1 83.9(2) . . . . ? C41 O10 Ta1 O2 -83.9(2) . . . . ? C41 O10 Ta1 O9 179.7(2) . . . . ? C41 O10 Ta1 O5 -10.8(3) . . . . ? C41 O10 Ta1 O6 -169.06(17) . . . . ? C41 O10 Ta1 O13 -3.34(19) . . . . ? C38 O5 Ta1 O1 173.37(15) . . . . ? C38 O5 Ta1 O2 -9.12(14) . . . . ? C38 O5 Ta1 O9 75.33(18) . . . . ? C38 O5 Ta1 O10 -87.63(17) . . . . ? C38 O5 Ta1 O6 78.66(15) . . . . ? C38 O5 Ta1 O13 -95.14(15) . . . . ? C39 O6 Ta1 O1 98.69(19) . . . . ? C39 O6 Ta1 O2 -98.79(19) . . . . ? C39 O6 Ta1 O9 0.87(18) . . . . ? C39 O6 Ta1 O10 -10.2(2) . . . . ? C39 O6 Ta1 O5 -177.1(2) . . . . ? C39 O6 Ta1 O13 -167.32(17) . . . . ? C42 O13 Ta1 O1 -100.39(19) . . . . ? C42 O13 Ta1 O2 95.58(19) . . . . ? C42 O13 Ta1 O9 3.8(2) . . . . ? C42 O13 Ta1 O10 -1.09(18) . . . . ? C42 O13 Ta1 O5 174.3(2) . . . . ? C42 O13 Ta1 O6 164.60(17) . . . . ? data_4 _database_code_depnum_ccdc_archive 'CCDC 894042' #TrackingRef '12903_web_deposit_cif_file_3_LidijaAndros_1343389594.ccdc_deposit4.cif' _audit_creation_date 2012-05-24T16:10:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C43 H29 N6 Ni O14 Ta' _chemical_formula_weight 1093.38 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4776(2) _cell_length_b 12.6662(2) _cell_length_c 15.53000(10) _cell_angle_alpha 110.1450(10) _cell_angle_beta 90.8670(10) _cell_angle_gamma 109.593(2) _cell_volume 1974.97(5) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 41359 _cell_measurement_theta_min 2.1087 _cell_measurement_theta_max 32.326 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.77732 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.3801 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_number 61331 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 32.4 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.916 _reflns_number_total 12970 _reflns_number_gt 12171 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0183P)^2^+1.0807P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 12970 _refine_ls_number_parameters 594 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0446 _refine_ls_wR_factor_gt 0.0433 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.537 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.58498(14) 0.44088(14) 0.86612(12) 0.0228(3) Uani 1 1 d . . . H1 H 0.5217 0.415 0.8172 0.027 Uiso 1 1 calc R . . C2 C 0.55683(16) 0.40367(14) 0.94099(12) 0.0259(3) Uani 1 1 d . . . H2 H 0.4765 0.3529 0.9407 0.031 Uiso 1 1 calc R . . C3 C 0.64810(17) 0.44244(15) 1.01442(12) 0.0270(3) Uani 1 1 d . . . H3 H 0.6301 0.4185 1.0645 0.032 Uiso 1 1 calc R . . C4 C 0.76938(16) 0.51882(14) 1.01353(11) 0.0227(3) Uani 1 1 d . . . C5 C 0.87077(18) 0.56499(16) 1.08774(11) 0.0286(3) Uani 1 1 d . . . H5 H 0.8567 0.5465 1.1405 0.034 Uiso 1 1 calc R . . C6 C 0.98634(17) 0.63501(16) 1.08179(11) 0.0281(3) Uani 1 1 d . . . H6 H 1.0504 0.6648 1.131 0.034 Uiso 1 1 calc R . . C7 C 1.01211(15) 0.66432(14) 1.00077(11) 0.0225(3) Uani 1 1 d . . . C8 C 1.13233(15) 0.73019(15) 0.98922(12) 0.0264(3) Uani 1 1 d . . . H8 H 1.1997 0.7589 1.0357 0.032 Uiso 1 1 calc R . . C9 C 1.14938(15) 0.75177(16) 0.90870(12) 0.0284(3) Uani 1 1 d . . . H9 H 1.2283 0.7958 0.9001 0.034 Uiso 1 1 calc R . . C10 C 1.04639(15) 0.70671(15) 0.83957(12) 0.0255(3) Uani 1 1 d . . . H10 H 1.0589 0.7221 0.7854 0.031 Uiso 1 1 calc R . . C11 C 0.91417(14) 0.62171(13) 0.92773(10) 0.0182(3) Uani 1 1 d . . . C12 C 0.79051(14) 0.54942(13) 0.93472(10) 0.0183(3) Uani 1 1 d . . . C13 C 0.89454(15) 0.60065(15) 0.58810(11) 0.0224(3) Uani 1 1 d . . . H13 H 0.8935 0.5226 0.5727 0.027 Uiso 1 1 calc R . . C14 C 0.94657(16) 0.66416(16) 0.53148(11) 0.0254(3) Uani 1 1 d . . . H14 H 0.9772 0.6278 0.4787 0.03 Uiso 1 1 calc R . . C15 C 0.95193(15) 0.78039(16) 0.55460(11) 0.0237(3) Uani 1 1 d . . . H15 H 0.9897 0.825 0.5193 0.028 Uiso 1 1 calc R . . C16 C 0.89981(13) 0.83182(14) 0.63227(10) 0.0196(3) Uani 1 1 d . . . C17 C 0.89264(15) 0.94962(15) 0.65777(12) 0.0247(3) Uani 1 1 d . . . H17 H 0.9295 0.9979 0.6248 0.03 Uiso 1 1 calc R . . C18 C 0.83311(16) 0.99151(15) 0.72907(12) 0.0257(3) Uani 1 1 d . . . H18 H 0.8288 1.0676 0.7438 0.031 Uiso 1 1 calc R . . C19 C 0.77653(14) 0.91964(14) 0.78228(11) 0.0205(3) Uani 1 1 d . . . C20 C 0.70925(16) 0.95606(15) 0.85467(11) 0.0252(3) Uani 1 1 d . . . H20 H 0.7018 1.0312 0.8717 0.03 Uiso 1 1 calc R . . C21 C 0.65473(17) 0.88068(16) 0.90009(11) 0.0270(3) Uani 1 1 d . . . H21 H 0.6083 0.903 0.947 0.032 Uiso 1 1 calc R . . C22 C 0.67014(16) 0.76927(15) 0.87460(11) 0.0245(3) Uani 1 1 d . . . H22 H 0.6344 0.7192 0.9065 0.029 Uiso 1 1 calc R . . C23 C 0.78496(13) 0.80547(13) 0.76042(10) 0.0172(2) Uani 1 1 d . . . C24 C 0.84681(13) 0.76067(13) 0.68400(10) 0.0164(2) Uani 1 1 d . . . C25 C 0.50739(15) 0.52196(17) 0.65234(12) 0.0267(3) Uani 1 1 d . . . H25 H 0.5151 0.5989 0.6921 0.032 Uiso 1 1 calc R . . C26 C 0.40352(16) 0.4557(2) 0.58257(13) 0.0341(4) Uani 1 1 d . . . H26 H 0.3444 0.4886 0.5756 0.041 Uiso 1 1 calc R . . C27 C 0.39059(17) 0.3417(2) 0.52486(13) 0.0369(4) Uani 1 1 d . . . H27 H 0.3216 0.296 0.4788 0.044 Uiso 1 1 calc R . . C28 C 0.48177(16) 0.29330(17) 0.53513(12) 0.0303(4) Uani 1 1 d . . . C29 C 0.47688(19) 0.17540(18) 0.47747(13) 0.0393(5) Uani 1 1 d . . . H29 H 0.4095 0.1259 0.4305 0.047 Uiso 1 1 calc R . . C30 C 0.5680(2) 0.13500(16) 0.49001(13) 0.0366(4) Uani 1 1 d . . . H30 H 0.562 0.0579 0.4517 0.044 Uiso 1 1 calc R . . C31 C 0.67447(17) 0.20846(14) 0.56132(11) 0.0273(3) Uani 1 1 d . . . C32 C 0.77468(19) 0.17340(15) 0.57529(13) 0.0317(4) Uani 1 1 d . . . H32 H 0.7731 0.097 0.5394 0.038 Uiso 1 1 calc R . . C33 C 0.87456(18) 0.25228(16) 0.64194(13) 0.0299(4) Uani 1 1 d . . . H33 H 0.9416 0.23 0.6517 0.036 Uiso 1 1 calc R . . C34 C 0.87513(16) 0.36728(15) 0.69560(11) 0.0236(3) Uani 1 1 d . . . H34 H 0.9438 0.4205 0.7405 0.028 Uiso 1 1 calc R . . C35 C 0.68213(15) 0.32478(13) 0.61857(10) 0.0210(3) Uani 1 1 d . . . C36 C 0.58368(14) 0.36703(14) 0.60612(11) 0.0219(3) Uani 1 1 d . . . C37 C 0.55762(14) 0.12838(14) 0.79878(11) 0.0208(3) Uani 1 1 d . . . C38 C 0.50890(14) 0.12783(13) 0.89201(10) 0.0187(3) Uani 1 1 d . . . C39 C 0.33546(17) -0.22479(15) 0.73062(13) 0.0286(3) Uani 1 1 d . . . C40 C 0.25027(16) -0.25580(15) 0.64198(12) 0.0267(3) Uani 1 1 d . . . C41 C 0.21467(17) 0.12442(16) 0.64014(13) 0.0297(3) Uani 1 1 d . . . C42 C 0.27067(16) 0.22502(15) 0.73574(12) 0.0265(3) Uani 1 1 d . . . C43 C 0.10240(19) 0.0240(2) 0.89177(14) 0.0384(4) Uani 1 1 d . . . H43A H 0.0186 -0.0276 0.8905 0.058 Uiso 1 1 calc R . . H43B H 0.1028 0.1017 0.8963 0.058 Uiso 1 1 calc R . . H43C H 0.1552 0.033 0.9444 0.058 Uiso 1 1 calc R . . N1 N 0.69897(12) 0.51193(11) 0.86251(9) 0.0187(2) Uani 1 1 d . . . N2 N 0.93130(12) 0.64283(11) 0.84780(9) 0.0191(2) Uani 1 1 d . . . N3 N 0.84651(12) 0.64704(11) 0.66293(8) 0.0182(2) Uani 1 1 d . . . N4 N 0.73345(12) 0.73174(11) 0.80700(9) 0.0191(2) Uani 1 1 d . . . N5 N 0.59551(12) 0.47956(12) 0.66417(9) 0.0212(2) Uani 1 1 d . . . N6 N 0.78134(12) 0.40283(11) 0.68470(9) 0.0192(2) Uani 1 1 d . . . Ni1 Ni 0.763869(17) 0.568539(16) 0.755127(13) 0.01638(4) Uani 1 1 d . . . O1 O 0.14737(11) -0.02756(11) 0.80968(8) 0.0259(2) Uani 1 1 d . . . O2 O 0.46641(11) 0.07486(11) 0.72849(8) 0.0249(2) Uani 1 1 d . . . O3 O 0.66692(11) 0.17377(12) 0.79459(9) 0.0305(3) Uani 1 1 d . . . O4 O 0.57999(11) 0.15986(11) 0.96198(8) 0.0274(2) Uani 1 1 d . . . O5 O 0.38794(10) 0.09225(10) 0.88405(7) 0.0198(2) Uani 1 1 d . . . O6 O 0.35970(13) -0.11427(11) 0.78623(9) 0.0322(3) Uani 1 1 d . . . O7 O 0.37004(16) -0.29809(13) 0.74576(11) 0.0470(4) Uani 1 1 d . . . O8 O 0.21394(15) -0.35361(12) 0.58033(10) 0.0431(4) Uani 1 1 d . . . O9 O 0.22343(12) -0.16238(11) 0.64321(9) 0.0301(3) Uani 1 1 d . . . O10 O 0.22328(12) 0.02277(11) 0.63725(8) 0.0294(3) Uani 1 1 d . . . O11 O 0.16819(18) 0.13827(15) 0.57690(11) 0.0535(4) Uani 1 1 d . . . O12 O 0.28820(15) 0.33054(12) 0.75112(10) 0.0397(3) Uani 1 1 d . . . O13 O 0.29752(12) 0.18283(11) 0.79501(8) 0.0282(2) Uani 1 1 d . . . O14 O 0.16175(15) 0.46565(15) 0.70453(12) 0.0418(3) Uani 1 1 d D . . Ta1 Ta 0.288387(5) 0.001128(5) 0.751143(4) 0.01859(2) Uani 1 1 d . . . H14A H 0.222(2) 0.5338(19) 0.706(2) 0.081(11) Uiso 1 1 d D . . H14B H 0.202(3) 0.416(2) 0.707(2) 0.068(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0193(7) 0.0194(6) 0.0273(8) 0.0061(6) 0.0046(6) 0.0067(5) C2 0.0254(7) 0.0194(7) 0.0329(9) 0.0095(6) 0.0116(7) 0.0082(6) C3 0.0343(9) 0.0247(7) 0.0286(8) 0.0141(6) 0.0143(7) 0.0139(7) C4 0.0284(8) 0.0223(7) 0.0213(7) 0.0093(6) 0.0066(6) 0.0128(6) C5 0.0387(9) 0.0333(9) 0.0182(7) 0.0112(6) 0.0044(7) 0.0167(7) C6 0.0337(9) 0.0316(8) 0.0186(7) 0.0074(6) -0.0029(6) 0.0137(7) C7 0.0239(7) 0.0221(7) 0.0189(7) 0.0037(6) -0.0020(6) 0.0095(6) C8 0.0213(7) 0.0250(7) 0.0259(8) 0.0036(6) -0.0058(6) 0.0062(6) C9 0.0178(7) 0.0284(8) 0.0308(9) 0.0080(7) -0.0014(6) 0.0017(6) C10 0.0205(7) 0.0273(8) 0.0246(8) 0.0101(6) 0.0017(6) 0.0035(6) C11 0.0188(6) 0.0177(6) 0.0169(6) 0.0041(5) 0.0006(5) 0.0075(5) C12 0.0201(6) 0.0176(6) 0.0183(6) 0.0058(5) 0.0037(5) 0.0090(5) C13 0.0228(7) 0.0252(7) 0.0182(7) 0.0045(6) 0.0032(6) 0.0112(6) C14 0.0251(7) 0.0354(8) 0.0189(7) 0.0096(6) 0.0070(6) 0.0154(7) C15 0.0194(7) 0.0349(8) 0.0219(7) 0.0149(6) 0.0055(6) 0.0117(6) C16 0.0157(6) 0.0246(7) 0.0193(7) 0.0098(6) 0.0001(5) 0.0067(5) C17 0.0242(7) 0.0253(7) 0.0283(8) 0.0150(6) 0.0033(6) 0.0084(6) C18 0.0281(8) 0.0218(7) 0.0301(8) 0.0118(6) 0.0028(6) 0.0103(6) C19 0.0216(7) 0.0200(6) 0.0191(7) 0.0057(5) 0.0001(5) 0.0085(5) C20 0.0300(8) 0.0245(7) 0.0210(7) 0.0032(6) 0.0017(6) 0.0153(6) C21 0.0319(8) 0.0315(8) 0.0196(7) 0.0065(6) 0.0079(6) 0.0171(7) C22 0.0273(8) 0.0277(8) 0.0201(7) 0.0092(6) 0.0071(6) 0.0115(6) C23 0.0163(6) 0.0185(6) 0.0148(6) 0.0040(5) -0.0003(5) 0.0062(5) C24 0.0145(6) 0.0192(6) 0.0141(6) 0.0050(5) -0.0007(5) 0.0056(5) C25 0.0202(7) 0.0360(9) 0.0258(8) 0.0126(7) 0.0021(6) 0.0113(6) C26 0.0198(7) 0.0536(12) 0.0308(9) 0.0201(9) 0.0002(7) 0.0114(8) C27 0.0198(8) 0.0521(12) 0.0268(9) 0.0136(8) -0.0064(7) -0.0002(7) C28 0.0240(8) 0.0330(9) 0.0213(8) 0.0077(7) -0.0018(6) -0.0023(6) C29 0.0359(10) 0.0321(9) 0.0249(9) 0.0011(7) -0.0039(7) -0.0079(8) C30 0.0448(11) 0.0209(8) 0.0250(8) -0.0003(6) 0.0074(8) -0.0022(7) C31 0.0361(9) 0.0184(7) 0.0213(7) 0.0058(6) 0.0089(7) 0.0038(6) C32 0.0493(11) 0.0207(7) 0.0280(8) 0.0088(6) 0.0179(8) 0.0158(7) C33 0.0400(10) 0.0304(8) 0.0316(9) 0.0168(7) 0.0172(8) 0.0216(7) C34 0.0260(7) 0.0260(7) 0.0230(7) 0.0113(6) 0.0065(6) 0.0124(6) C35 0.0241(7) 0.0172(6) 0.0177(7) 0.0056(5) 0.0038(5) 0.0035(5) C36 0.0202(7) 0.0228(7) 0.0173(7) 0.0064(5) 0.0013(5) 0.0023(5) C37 0.0205(7) 0.0206(6) 0.0226(7) 0.0085(6) 0.0030(6) 0.0085(5) C38 0.0189(6) 0.0161(6) 0.0194(7) 0.0052(5) 0.0012(5) 0.0059(5) C39 0.0299(8) 0.0231(7) 0.0315(9) 0.0086(7) -0.0002(7) 0.0098(6) C40 0.0270(8) 0.0226(7) 0.0265(8) 0.0050(6) 0.0007(6) 0.0083(6) C41 0.0293(8) 0.0298(8) 0.0289(8) 0.0147(7) -0.0042(7) 0.0058(7) C42 0.0254(8) 0.0266(8) 0.0296(8) 0.0114(7) 0.0010(6) 0.0112(6) C43 0.0288(9) 0.0492(11) 0.0310(9) 0.0077(8) 0.0053(7) 0.0141(8) N1 0.0177(5) 0.0174(5) 0.0197(6) 0.0054(5) 0.0026(5) 0.0063(4) N2 0.0179(6) 0.0195(6) 0.0171(6) 0.0053(5) 0.0004(4) 0.0050(4) N3 0.0174(5) 0.0204(6) 0.0149(5) 0.0045(4) 0.0007(4) 0.0069(4) N4 0.0212(6) 0.0194(6) 0.0157(5) 0.0049(5) 0.0022(5) 0.0077(5) N5 0.0179(6) 0.0232(6) 0.0200(6) 0.0070(5) -0.0002(5) 0.0057(5) N6 0.0210(6) 0.0190(5) 0.0178(6) 0.0065(5) 0.0030(5) 0.0077(5) Ni1 0.01579(8) 0.01648(8) 0.01508(8) 0.00440(6) 0.00035(6) 0.00524(6) O1 0.0186(5) 0.0298(6) 0.0254(6) 0.0080(5) 0.0002(4) 0.0063(4) O2 0.0239(5) 0.0307(6) 0.0179(5) 0.0084(4) 0.0023(4) 0.0077(5) O3 0.0211(5) 0.0378(7) 0.0342(7) 0.0168(6) 0.0072(5) 0.0089(5) O4 0.0211(5) 0.0339(6) 0.0229(6) 0.0085(5) -0.0038(4) 0.0070(5) O5 0.0165(5) 0.0246(5) 0.0165(5) 0.0058(4) 0.0006(4) 0.0072(4) O6 0.0414(7) 0.0222(6) 0.0287(6) 0.0039(5) -0.0117(5) 0.0125(5) O7 0.0599(10) 0.0302(7) 0.0502(9) 0.0073(6) -0.0119(8) 0.0243(7) O8 0.0542(9) 0.0249(6) 0.0384(8) -0.0027(6) -0.0093(7) 0.0157(6) O9 0.0354(7) 0.0227(5) 0.0255(6) 0.0002(5) -0.0096(5) 0.0118(5) O10 0.0382(7) 0.0251(6) 0.0208(5) 0.0072(5) -0.0072(5) 0.0084(5) O11 0.0700(11) 0.0435(9) 0.0448(9) 0.0241(7) -0.0218(8) 0.0111(8) O12 0.0521(9) 0.0277(6) 0.0431(8) 0.0143(6) -0.0004(7) 0.0184(6) O13 0.0373(7) 0.0232(5) 0.0246(6) 0.0060(5) -0.0034(5) 0.0147(5) O14 0.0385(8) 0.0508(9) 0.0533(9) 0.0331(8) 0.0176(7) 0.0226(7) Ta1 0.01794(3) 0.01788(3) 0.01720(3) 0.00480(2) -0.00217(2) 0.00511(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3312(19) . ? C1 C2 1.402(2) . ? C1 H1 0.93 . ? C2 C3 1.368(3) . ? C2 H2 0.93 . ? C3 C4 1.407(2) . ? C3 H3 0.93 . ? C4 C12 1.407(2) . ? C4 C5 1.436(2) . ? C5 C6 1.351(3) . ? C5 H5 0.93 . ? C6 C7 1.438(2) . ? C6 H6 0.93 . ? C7 C8 1.404(2) . ? C7 C11 1.405(2) . ? C8 C9 1.372(2) . ? C8 H8 0.93 . ? C9 C10 1.401(2) . ? C9 H9 0.93 . ? C10 N2 1.332(2) . ? C10 H10 0.93 . ? C11 N2 1.3608(19) . ? C11 C12 1.437(2) . ? C12 N1 1.3601(19) . ? C13 N3 1.3289(19) . ? C13 C14 1.399(2) . ? C13 H13 0.93 . ? C14 C15 1.369(2) . ? C14 H14 0.93 . ? C15 C16 1.407(2) . ? C15 H15 0.93 . ? C16 C24 1.405(2) . ? C16 C17 1.437(2) . ? C17 C18 1.355(2) . ? C17 H17 0.93 . ? C18 C19 1.439(2) . ? C18 H18 0.93 . ? C19 C23 1.404(2) . ? C19 C20 1.408(2) . ? C20 C21 1.370(2) . ? C20 H20 0.93 . ? C21 C22 1.401(2) . ? C21 H21 0.93 . ? C22 N4 1.329(2) . ? C22 H22 0.93 . ? C23 N4 1.3612(19) . ? C23 C24 1.437(2) . ? C24 N3 1.3605(18) . ? C25 N5 1.331(2) . ? C25 C26 1.401(2) . ? C25 H25 0.93 . ? C26 C27 1.368(3) . ? C26 H26 0.93 . ? C27 C28 1.410(3) . ? C27 H27 0.93 . ? C28 C36 1.405(2) . ? C28 C29 1.434(3) . ? C29 C30 1.348(3) . ? C29 H29 0.93 . ? C30 C31 1.439(3) . ? C30 H30 0.93 . ? C31 C32 1.403(3) . ? C31 C35 1.406(2) . ? C32 C33 1.367(3) . ? C32 H32 0.93 . ? C33 C34 1.405(2) . ? C33 H33 0.93 . ? C34 N6 1.328(2) . ? C34 H34 0.93 . ? C35 N6 1.356(2) . ? C35 C36 1.439(2) . ? C36 N5 1.358(2) . ? C37 O3 1.2054(19) . ? C37 O2 1.3140(19) . ? C37 C38 1.561(2) . ? C38 O4 1.2076(18) . ? C38 O5 1.2972(18) . ? C39 O7 1.212(2) . ? C39 O6 1.297(2) . ? C39 C40 1.528(2) . ? C40 O8 1.204(2) . ? C40 O9 1.313(2) . ? C41 O11 1.202(2) . ? C41 O10 1.310(2) . ? C41 C42 1.536(2) . ? C42 O12 1.218(2) . ? C42 O13 1.292(2) . ? C43 O1 1.411(2) . ? C43 H43A 0.96 . ? C43 H43B 0.96 . ? C43 H43C 0.96 . ? N1 Ni1 2.0863(13) . ? N2 Ni1 2.1025(13) . ? N3 Ni1 2.0802(13) . ? N4 Ni1 2.0952(13) . ? N5 Ni1 2.0880(13) . ? N6 Ni1 2.0855(13) . ? O1 Ta1 1.8590(12) . ? O2 Ta1 2.0345(12) . ? O5 Ta1 2.0740(10) . ? O6 Ta1 2.1073(12) . ? O9 Ta1 2.0469(12) . ? O10 Ta1 2.0478(12) . ? O13 Ta1 2.1279(12) . ? O14 H14A 0.896(17) . ? O14 H14B 0.904(17) . ? 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 C1 C2 122.43(15) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.70(15) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.46(15) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C12 C4 C3 117.21(15) . . ? C12 C4 C5 119.35(15) . . ? C3 C4 C5 123.44(15) . . ? C6 C5 C4 120.83(15) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.20(15) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C11 117.81(15) . . ? C8 C7 C6 123.04(15) . . ? C11 C7 C6 119.10(15) . . ? C9 C8 C7 119.34(15) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.17(15) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 123.09(15) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N2 C11 C7 122.77(14) . . ? N2 C11 C12 117.38(13) . . ? C7 C11 C12 119.82(14) . . ? N1 C12 C4 123.03(14) . . ? N1 C12 C11 117.32(13) . . ? C4 C12 C11 119.64(14) . . ? N3 C13 C14 122.87(15) . . ? N3 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 119.31(15) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.46(15) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C24 C16 C15 117.44(14) . . ? C24 C16 C17 119.10(14) . . ? C15 C16 C17 123.38(14) . . ? C18 C17 C16 121.13(15) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.79(15) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C23 C19 C20 117.23(14) . . ? C23 C19 C18 119.27(14) . . ? C20 C19 C18 123.48(14) . . ? C21 C20 C19 119.92(15) . . ? C21 C20 H20 120 . . ? C19 C20 H20 120 . . ? C20 C21 C22 118.79(15) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N4 C22 C21 123.16(15) . . ? N4 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N4 C23 C19 122.90(13) . . ? N4 C23 C24 117.29(13) . . ? C19 C23 C24 119.78(13) . . ? N3 C24 C16 122.80(13) . . ? N3 C24 C23 117.26(13) . . ? C16 C24 C23 119.88(13) . . ? N5 C25 C26 122.82(17) . . ? N5 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C27 C26 C25 118.87(18) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 120.10(16) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C36 C28 C27 117.05(17) . . ? C36 C28 C29 118.85(18) . . ? C27 C28 C29 124.10(17) . . ? C30 C29 C28 121.24(17) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 121.47(17) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C35 117.31(16) . . ? C32 C31 C30 124.08(17) . . ? C35 C31 C30 118.55(18) . . ? C33 C32 C31 119.59(16) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 119.41(17) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? N6 C34 C33 122.50(16) . . ? N6 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? N6 C35 C31 122.96(16) . . ? N6 C35 C36 117.08(13) . . ? C31 C35 C36 119.92(15) . . ? N5 C36 C28 122.76(16) . . ? N5 C36 C35 117.27(13) . . ? C28 C36 C35 119.96(15) . . ? O3 C37 O2 125.71(15) . . ? O3 C37 C38 122.23(14) . . ? O2 C37 C38 112.06(13) . . ? O4 C38 O5 126.30(14) . . ? O4 C38 C37 121.45(14) . . ? O5 C38 C37 112.24(12) . . ? O7 C39 O6 126.24(17) . . ? O7 C39 C40 122.52(16) . . ? O6 C39 C40 111.18(14) . . ? O8 C40 O9 125.78(17) . . ? O8 C40 C39 123.35(16) . . ? O9 C40 C39 110.87(14) . . ? O11 C41 O10 124.96(18) . . ? O11 C41 C42 123.69(17) . . ? O10 C41 C42 111.34(14) . . ? O12 C42 O13 125.72(17) . . ? O12 C42 C41 122.97(16) . . ? O13 C42 C41 111.30(14) . . ? O1 C43 H43A 109.5 . . ? O1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C1 N1 C12 118.14(13) . . ? C1 N1 Ni1 128.75(11) . . ? C12 N1 Ni1 113.00(10) . . ? C10 N2 C11 117.81(13) . . ? C10 N2 Ni1 129.79(11) . . ? C11 N2 Ni1 112.39(10) . . ? C13 N3 C24 118.04(13) . . ? C13 N3 Ni1 129.07(11) . . ? C24 N3 Ni1 112.87(9) . . ? C22 N4 C23 117.96(13) . . ? C22 N4 Ni1 129.63(11) . . ? C23 N4 Ni1 112.38(9) . . ? C25 N5 C36 118.38(14) . . ? C25 N5 Ni1 128.69(12) . . ? C36 N5 Ni1 112.71(10) . . ? C34 N6 C35 118.23(14) . . ? C34 N6 Ni1 128.77(11) . . ? C35 N6 Ni1 112.99(10) . . ? N3 Ni1 N6 94.90(5) . . ? N3 Ni1 N1 171.76(5) . . ? N6 Ni1 N1 90.35(5) . . ? N3 Ni1 N5 90.29(5) . . ? N6 Ni1 N5 79.88(5) . . ? N1 Ni1 N5 96.90(5) . . ? N3 Ni1 N4 80.04(5) . . ? N6 Ni1 N4 171.53(5) . . ? N1 Ni1 N4 95.47(5) . . ? N5 Ni1 N4 93.29(5) . . ? N3 Ni1 N2 93.28(5) . . ? N6 Ni1 N2 95.92(5) . . ? N1 Ni1 N2 79.84(5) . . ? N5 Ni1 N2 174.72(5) . . ? N4 Ni1 N2 91.17(5) . . ? C43 O1 Ta1 141.13(12) . . ? C37 O2 Ta1 119.07(10) . . ? C38 O5 Ta1 117.37(9) . . ? C39 O6 Ta1 121.72(11) . . ? C40 O9 Ta1 123.46(11) . . ? C41 O10 Ta1 122.91(11) . . ? C42 O13 Ta1 120.58(11) . . ? H14A O14 H14B 105(2) . . ? O1 Ta1 O2 161.35(5) . . ? O1 Ta1 O9 95.60(5) . . ? O2 Ta1 O9 102.19(5) . . ? O1 Ta1 O10 101.83(5) . . ? O2 Ta1 O10 89.31(5) . . ? O9 Ta1 O10 71.05(5) . . ? O1 Ta1 O5 85.46(5) . . ? O2 Ta1 O5 76.90(4) . . ? O9 Ta1 O5 143.87(5) . . ? O10 Ta1 O5 144.14(5) . . ? O1 Ta1 O6 96.80(6) . . ? O2 Ta1 O6 83.35(5) . . ? O9 Ta1 O6 72.76(5) . . ? O10 Ta1 O6 140.53(5) . . ? O5 Ta1 O6 71.26(5) . . ? O1 Ta1 O13 86.30(5) . . ? O2 Ta1 O13 82.66(5) . . ? O9 Ta1 O13 143.77(5) . . ? O10 Ta1 O13 73.16(5) . . ? O5 Ta1 O13 72.35(4) . . ? O6 Ta1 O13 143.09(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.1(2) . . . . ? C1 C2 C3 C4 -0.3(2) . . . . ? C2 C3 C4 C12 -1.2(2) . . . . ? C2 C3 C4 C5 179.37(16) . . . . ? C12 C4 C5 C6 -1.5(2) . . . . ? C3 C4 C5 C6 177.92(16) . . . . ? C4 C5 C6 C7 -0.8(3) . . . . ? C5 C6 C7 C8 -175.79(17) . . . . ? C5 C6 C7 C11 1.7(2) . . . . ? C11 C7 C8 C9 0.9(2) . . . . ? C6 C7 C8 C9 178.41(16) . . . . ? C7 C8 C9 C10 -0.5(3) . . . . ? C8 C9 C10 N2 -0.2(3) . . . . ? C8 C7 C11 N2 -0.7(2) . . . . ? C6 C7 C11 N2 -178.31(14) . . . . ? C8 C7 C11 C12 177.32(14) . . . . ? C6 C7 C11 C12 -0.3(2) . . . . ? C3 C4 C12 N1 2.2(2) . . . . ? C5 C4 C12 N1 -178.37(14) . . . . ? C3 C4 C12 C11 -176.60(14) . . . . ? C5 C4 C12 C11 2.8(2) . . . . ? N2 C11 C12 N1 -2.7(2) . . . . ? C7 C11 C12 N1 179.17(13) . . . . ? N2 C11 C12 C4 176.18(13) . . . . ? C7 C11 C12 C4 -2.0(2) . . . . ? N3 C13 C14 C15 1.8(2) . . . . ? C13 C14 C15 C16 -3.0(2) . . . . ? C14 C15 C16 C24 1.5(2) . . . . ? C14 C15 C16 C17 -175.18(15) . . . . ? C24 C16 C17 C18 -1.7(2) . . . . ? C15 C16 C17 C18 174.93(16) . . . . ? C16 C17 C18 C19 0.8(3) . . . . ? C17 C18 C19 C23 0.9(2) . . . . ? C17 C18 C19 C20 -177.41(16) . . . . ? C23 C19 C20 C21 -0.4(2) . . . . ? C18 C19 C20 C21 177.90(16) . . . . ? C19 C20 C21 C22 1.6(3) . . . . ? C20 C21 C22 N4 -1.3(3) . . . . ? C20 C19 C23 N4 -1.3(2) . . . . ? C18 C19 C23 N4 -179.63(14) . . . . ? C20 C19 C23 C24 176.75(14) . . . . ? C18 C19 C23 C24 -1.6(2) . . . . ? C15 C16 C24 N3 1.3(2) . . . . ? C17 C16 C24 N3 178.14(14) . . . . ? C15 C16 C24 C23 -175.94(13) . . . . ? C17 C16 C24 C23 0.9(2) . . . . ? N4 C23 C24 N3 1.45(19) . . . . ? C19 C23 C24 N3 -176.65(13) . . . . ? N4 C23 C24 C16 178.87(13) . . . . ? C19 C23 C24 C16 0.8(2) . . . . ? N5 C25 C26 C27 1.1(3) . . . . ? C25 C26 C27 C28 -0.9(3) . . . . ? C26 C27 C28 C36 0.0(3) . . . . ? C26 C27 C28 C29 -179.37(18) . . . . ? C36 C28 C29 C30 -0.3(3) . . . . ? C27 C28 C29 C30 179.04(19) . . . . ? C28 C29 C30 C31 -0.4(3) . . . . ? C29 C30 C31 C32 -177.27(18) . . . . ? C29 C30 C31 C35 0.0(3) . . . . ? C35 C31 C32 C33 -0.7(2) . . . . ? C30 C31 C32 C33 176.63(16) . . . . ? C31 C32 C33 C34 0.1(3) . . . . ? C32 C33 C34 N6 0.5(3) . . . . ? C32 C31 C35 N6 0.6(2) . . . . ? C30 C31 C35 N6 -176.80(15) . . . . ? C32 C31 C35 C36 178.51(14) . . . . ? C30 C31 C35 C36 1.1(2) . . . . ? C27 C28 C36 N5 0.9(2) . . . . ? C29 C28 C36 N5 -179.69(16) . . . . ? C27 C28 C36 C35 -178.03(15) . . . . ? C29 C28 C36 C35 1.4(2) . . . . ? N6 C35 C36 N5 -2.8(2) . . . . ? C31 C35 C36 N5 179.24(14) . . . . ? N6 C35 C36 C28 176.22(14) . . . . ? C31 C35 C36 C28 -1.8(2) . . . . ? O3 C37 C38 O4 -9.1(2) . . . . ? O2 C37 C38 O4 171.05(14) . . . . ? O3 C37 C38 O5 169.68(14) . . . . ? O2 C37 C38 O5 -10.17(18) . . . . ? O7 C39 C40 O8 -1.8(3) . . . . ? O6 C39 C40 O8 -179.25(18) . . . . ? O7 C39 C40 O9 178.21(19) . . . . ? O6 C39 C40 O9 0.7(2) . . . . ? O11 C41 C42 O12 -10.6(3) . . . . ? O10 C41 C42 O12 170.00(17) . . . . ? O11 C41 C42 O13 170.5(2) . . . . ? O10 C41 C42 O13 -8.9(2) . . . . ? C2 C1 N1 C12 -0.2(2) . . . . ? C2 C1 N1 Ni1 175.59(11) . . . . ? C4 C12 N1 C1 -1.5(2) . . . . ? C11 C12 N1 C1 177.34(13) . . . . ? C4 C12 N1 Ni1 -177.94(11) . . . . ? C11 C12 N1 Ni1 0.90(16) . . . . ? C9 C10 N2 C11 0.4(2) . . . . ? C9 C10 N2 Ni1 179.18(13) . . . . ? C7 C11 N2 C10 0.0(2) . . . . ? C12 C11 N2 C10 -178.04(14) . . . . ? C7 C11 N2 Ni1 -178.91(12) . . . . ? C12 C11 N2 Ni1 3.02(16) . . . . ? C14 C13 N3 C24 1.0(2) . . . . ? C14 C13 N3 Ni1 179.37(12) . . . . ? C16 C24 N3 C13 -2.5(2) . . . . ? C23 C24 N3 C13 174.80(13) . . . . ? C16 C24 N3 Ni1 178.80(11) . . . . ? C23 C24 N3 Ni1 -3.86(16) . . . . ? C21 C22 N4 C23 -0.3(2) . . . . ? C21 C22 N4 Ni1 -178.09(12) . . . . ? C19 C23 N4 C22 1.6(2) . . . . ? C24 C23 N4 C22 -176.44(14) . . . . ? C19 C23 N4 Ni1 179.75(11) . . . . ? C24 C23 N4 Ni1 1.71(16) . . . . ? C26 C25 N5 C36 -0.2(2) . . . . ? C26 C25 N5 Ni1 173.98(13) . . . . ? C28 C36 N5 C25 -0.8(2) . . . . ? C35 C36 N5 C25 178.13(14) . . . . ? C28 C36 N5 Ni1 -175.88(12) . . . . ? C35 C36 N5 Ni1 3.08(17) . . . . ? C33 C34 N6 C35 -0.5(2) . . . . ? C33 C34 N6 Ni1 -179.26(12) . . . . ? C31 C35 N6 C34 -0.1(2) . . . . ? C36 C35 N6 C34 -177.99(13) . . . . ? C31 C35 N6 Ni1 178.88(12) . . . . ? C36 C35 N6 Ni1 0.95(17) . . . . ? C13 N3 Ni1 N6 -1.71(14) . . . . ? C24 N3 Ni1 N6 176.77(10) . . . . ? C13 N3 Ni1 N1 127.7(3) . . . . ? C24 N3 Ni1 N1 -53.9(4) . . . . ? C13 N3 Ni1 N5 -81.57(14) . . . . ? C24 N3 Ni1 N5 96.90(10) . . . . ? C13 N3 Ni1 N4 -174.86(14) . . . . ? C24 N3 Ni1 N4 3.61(10) . . . . ? C13 N3 Ni1 N2 94.53(13) . . . . ? C24 N3 Ni1 N2 -87.00(10) . . . . ? C34 N6 Ni1 N3 89.90(13) . . . . ? C35 N6 Ni1 N3 -88.90(11) . . . . ? C34 N6 Ni1 N1 -83.74(13) . . . . ? C35 N6 Ni1 N1 97.46(11) . . . . ? C34 N6 Ni1 N5 179.32(14) . . . . ? C35 N6 Ni1 N5 0.52(10) . . . . ? C34 N6 Ni1 N4 142.8(3) . . . . ? C35 N6 Ni1 N4 -36.0(4) . . . . ? C34 N6 Ni1 N2 -3.92(14) . . . . ? C35 N6 Ni1 N2 177.28(10) . . . . ? C1 N1 Ni1 N3 150.9(3) . . . . ? C12 N1 Ni1 N3 -33.1(4) . . . . ? C1 N1 Ni1 N6 -79.49(13) . . . . ? C12 N1 Ni1 N6 96.49(10) . . . . ? C1 N1 Ni1 N5 0.36(13) . . . . ? C12 N1 Ni1 N5 176.33(10) . . . . ? C1 N1 Ni1 N4 94.35(13) . . . . ? C12 N1 Ni1 N4 -89.68(10) . . . . ? C1 N1 Ni1 N2 -175.44(14) . . . . ? C12 N1 Ni1 N2 0.53(10) . . . . ? C25 N5 Ni1 N3 -81.45(14) . . . . ? C36 N5 Ni1 N3 92.98(11) . . . . ? C25 N5 Ni1 N6 -176.37(15) . . . . ? C36 N5 Ni1 N6 -1.94(10) . . . . ? C25 N5 Ni1 N1 94.51(14) . . . . ? C36 N5 Ni1 N1 -91.06(11) . . . . ? C25 N5 Ni1 N4 -1.41(14) . . . . ? C36 N5 Ni1 N4 173.01(11) . . . . ? C25 N5 Ni1 N2 146.1(5) . . . . ? C36 N5 Ni1 N2 -39.5(6) . . . . ? C22 N4 Ni1 N3 175.03(15) . . . . ? C23 N4 Ni1 N3 -2.85(10) . . . . ? C22 N4 Ni1 N6 121.3(3) . . . . ? C23 N4 Ni1 N6 -56.6(4) . . . . ? C22 N4 Ni1 N1 -11.94(15) . . . . ? C23 N4 Ni1 N1 170.18(10) . . . . ? C22 N4 Ni1 N5 85.32(14) . . . . ? C23 N4 Ni1 N5 -92.57(10) . . . . ? C22 N4 Ni1 N2 -91.84(14) . . . . ? C23 N4 Ni1 N2 90.27(10) . . . . ? C10 N2 Ni1 N3 -5.27(15) . . . . ? C11 N2 Ni1 N3 173.52(10) . . . . ? C10 N2 Ni1 N6 90.01(14) . . . . ? C11 N2 Ni1 N6 -91.21(10) . . . . ? C10 N2 Ni1 N1 179.30(15) . . . . ? C11 N2 Ni1 N1 -1.92(10) . . . . ? C10 N2 Ni1 N5 127.1(5) . . . . ? C11 N2 Ni1 N5 -54.1(6) . . . . ? C10 N2 Ni1 N4 -85.35(14) . . . . ? C11 N2 Ni1 N4 93.43(10) . . . . ? O3 C37 O2 Ta1 178.74(13) . . . . ? C38 C37 O2 Ta1 -1.41(16) . . . . ? O4 C38 O5 Ta1 -164.31(13) . . . . ? C37 C38 O5 Ta1 16.98(15) . . . . ? O7 C39 O6 Ta1 -178.30(17) . . . . ? C40 C39 O6 Ta1 -0.9(2) . . . . ? O8 C40 O9 Ta1 179.72(15) . . . . ? C39 C40 O9 Ta1 -0.2(2) . . . . ? O11 C41 O10 Ta1 -173.97(17) . . . . ? C42 C41 O10 Ta1 5.4(2) . . . . ? O12 C42 O13 Ta1 -169.91(15) . . . . ? C41 C42 O13 Ta1 8.98(19) . . . . ? C43 O1 Ta1 O2 11.0(3) . . . . ? C43 O1 Ta1 O9 173.6(2) . . . . ? C43 O1 Ta1 O10 -114.6(2) . . . . ? C43 O1 Ta1 O5 29.8(2) . . . . ? C43 O1 Ta1 O6 100.3(2) . . . . ? C43 O1 Ta1 O13 -42.7(2) . . . . ? C37 O2 Ta1 O1 27.0(2) . . . . ? C37 O2 Ta1 O9 -135.28(11) . . . . ? C37 O2 Ta1 O10 154.29(12) . . . . ? C37 O2 Ta1 O5 7.67(11) . . . . ? C37 O2 Ta1 O6 -64.57(12) . . . . ? C37 O2 Ta1 O13 81.18(12) . . . . ? C40 O9 Ta1 O1 -95.55(14) . . . . ? C40 O9 Ta1 O2 78.84(14) . . . . ? C40 O9 Ta1 O10 163.84(15) . . . . ? C40 O9 Ta1 O5 -5.58(19) . . . . ? C40 O9 Ta1 O6 -0.15(13) . . . . ? C40 O9 Ta1 O13 173.06(12) . . . . ? C41 O10 Ta1 O1 81.50(14) . . . . ? C41 O10 Ta1 O2 -83.44(14) . . . . ? C41 O10 Ta1 O9 173.42(15) . . . . ? C41 O10 Ta1 O5 -17.24(18) . . . . ? C41 O10 Ta1 O6 -162.09(13) . . . . ? C41 O10 Ta1 O13 -0.90(13) . . . . ? C38 O5 Ta1 O1 172.01(11) . . . . ? C38 O5 Ta1 O2 -14.09(10) . . . . ? C38 O5 Ta1 O9 78.72(13) . . . . ? C38 O5 Ta1 O10 -84.02(13) . . . . ? C38 O5 Ta1 O6 73.25(11) . . . . ? C38 O5 Ta1 O13 -100.43(11) . . . . ? C39 O6 Ta1 O1 94.42(15) . . . . ? C39 O6 Ta1 O2 -104.36(15) . . . . ? C39 O6 Ta1 O9 0.64(14) . . . . ? C39 O6 Ta1 O10 -23.60(19) . . . . ? C39 O6 Ta1 O5 177.26(15) . . . . ? C39 O6 Ta1 O13 -172.68(12) . . . . ? C42 O13 Ta1 O1 -108.64(13) . . . . ? C42 O13 Ta1 O2 86.42(13) . . . . ? C42 O13 Ta1 O9 -14.21(18) . . . . ? C42 O13 Ta1 O10 -5.09(13) . . . . ? C42 O13 Ta1 O5 164.95(14) . . . . ? C42 O13 Ta1 O6 154.95(12) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF