Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Pavica Planinic' 'Nevenka Brnicevic' 'Gerald Giester' 'Marijana Juric' 'Branko Kaitner' 'Damir Pajic' 'Berislav Peric' 'Kreso Zadro' _publ_contact_author_name 'Pavica Planinic' _publ_contact_author_address ; Division of Material Chemistry Rudjer Boskovic Institute Bijenicka 54 Zagreb 10002 CROATIA ; _publ_contact_author_email PLANINIC@IRB.HR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Supramolecular motifs and pseudo-polymorphism within the compounds containing [M(bpy)3]2+ entities: [M(bpy)3]2[NbO(C2O4)3]Cl.nH2O (M = Fe2+, Co2+, Ni2+, Cu2+ and Zn2+; bpy = 2,2'-bipyridine; n = 11, 12). ; #=============================================================================== data_I _database_code_depnum_ccdc_archive 'CCDC 648552' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H24 Fe N6), C6 Nb O13, 12(H2 O), Cl' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural '2(C30 H24 Fe N6), C6 Nb O13, 12(H2 O), Cl' _chemical_formula_sum 'C66 H72 Cl Fe2 N12 Nb O25' _chemical_formula_iupac ? _chemical_formula_weight 1673.42 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 14.9750(10) _cell_length_b 21.708(2) _cell_length_c 22.351(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7265.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 22167 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 30.53 _cell_special_details ; ? ; _exptl_crystal_description polyhedral _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 0.674 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.93 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(3) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius-Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 22167 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 30.53 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 22167 # number of observed reflections (> n sig(I)) _reflns_number_gt 15502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software (Nonius, 1998)' _computing_cell_refinement 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(8) # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ad _refine_ls_number_reflns 22167 _refine_ls_number_parameters 1036 _refine_ls_number_restraints 39 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.843 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.066 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Fe1 Fe Uani 0.36326(2) 0.32896(1) 0.00031(1) 1.000 0.0219(1) . . N1 N Uani 0.25998(13) 0.33413(10) 0.05479(9) 1.000 0.0237(6) . . N2 N Uani 0.29379(14) 0.39284(9) -0.04259(9) 1.000 0.0232(6) . . N3 N Uani 0.43444(14) 0.38990(10) 0.04498(9) 1.000 0.0252(6) . . N4 N Uani 0.46654(13) 0.33399(9) -0.05389(9) 1.000 0.0240(6) . . N5 N Uani 0.41622(14) 0.25815(9) 0.04352(9) 1.000 0.0259(6) . . N6 N Uani 0.30409(14) 0.26201(10) -0.04415(9) 1.000 0.0261(7) . . C1 C Uani 0.24986(18) 0.30568(13) 0.10813(11) 1.000 0.0299(8) . . C2 C Uani 0.17676(18) 0.31410(13) 0.14413(12) 1.000 0.0357(9) . . C3 C Uani 0.10879(19) 0.35168(14) 0.12553(13) 1.000 0.0398(9) . . C4 C Uani 0.11677(18) 0.38086(13) 0.07047(13) 1.000 0.0363(9) . . C5 C Uani 0.19302(17) 0.37192(11) 0.03680(11) 1.000 0.0252(8) . . C6 C Uani 0.21150(17) 0.40375(11) -0.02017(11) 1.000 0.0252(7) . . C7 C Uani 0.15044(18) 0.44157(12) -0.04916(11) 1.000 0.0318(8) . . C8 C Uani 0.1736(2) 0.46859(13) -0.10262(12) 1.000 0.0365(9) . . C9 C Uani 0.25724(19) 0.45835(13) -0.12539(12) 1.000 0.0348(9) . . C10 C Uani 0.31570(18) 0.42003(12) -0.09469(11) 1.000 0.0311(8) . . C11 C Uani 0.41491(18) 0.41582(12) 0.09799(11) 1.000 0.0322(8) . . C12 C Uani 0.4732(2) 0.45367(13) 0.12845(13) 1.000 0.0364(9) . . C13 C Uani 0.55485(19) 0.46654(13) 0.10452(13) 1.000 0.0360(9) . . C14 C Uani 0.57588(18) 0.44232(13) 0.04852(13) 1.000 0.0345(9) . . C15 C Uani 0.51484(16) 0.40395(11) 0.02061(11) 1.000 0.0260(7) . . C16 C Uani 0.53192(17) 0.37299(12) -0.03722(11) 1.000 0.0277(8) . . C17 C Uani 0.60816(19) 0.38289(13) -0.07171(13) 1.000 0.0377(9) . . C18 C Uani 0.6163(2) 0.35164(14) -0.12565(13) 1.000 0.0429(10) . . C19 C Uani 0.5487(2) 0.31184(13) -0.14330(13) 1.000 0.0383(9) . . C20 C Uani 0.47670(18) 0.30328(13) -0.10640(12) 1.000 0.0313(8) . . C21 C Uani 0.47722(18) 0.25921(13) 0.08762(12) 1.000 0.0348(9) . . C22 C Uani 0.50455(19) 0.20653(14) 0.11792(13) 1.000 0.0389(10) . . C23 C Uani 0.4687(2) 0.15084(14) 0.10239(13) 1.000 0.0423(10) . . C24 C Uani 0.4070(2) 0.14825(13) 0.05669(13) 1.000 0.0410(10) . . C25 C Uani 0.38264(18) 0.20240(12) 0.02739(11) 1.000 0.0289(8) . . C26 C Uani 0.32002(18) 0.20456(12) -0.02274(12) 1.000 0.0301(8) . . C27 C Uani 0.2830(2) 0.15283(13) -0.04961(13) 1.000 0.0403(10) . . C28 C Uani 0.2314(2) 0.15850(13) -0.09961(13) 1.000 0.0404(10) . . C29 C Uani 0.21556(19) 0.21656(14) -0.12204(13) 1.000 0.0373(9) . . C30 C Uani 0.25123(18) 0.26724(13) -0.09268(12) 1.000 0.0317(8) . . Fe2 Fe Uani 0.36176(2) 0.67205(2) 0.02636(1) 1.000 0.0225(1) . . N7 N Uani 0.46842(13) 0.66666(10) 0.07786(9) 1.000 0.0249(6) . . N8 N Uani 0.43131(14) 0.61212(9) -0.02115(9) 1.000 0.0249(6) . . N9 N Uani 0.29621(14) 0.60714(10) 0.06908(9) 1.000 0.0253(6) . . N10 N Uani 0.25734(14) 0.66696(10) -0.02678(9) 1.000 0.0278(6) . . N11 N Uani 0.30434(14) 0.73864(10) 0.07298(9) 1.000 0.0271(7) . . N12 N Uani 0.41323(15) 0.74317(10) -0.01621(9) 1.000 0.0264(7) . . C31 C Uani 0.47955(18) 0.69374(13) 0.13146(12) 1.000 0.0332(8) . . C32 C Uani 0.5556(2) 0.68427(13) 0.16542(13) 1.000 0.0406(10) . . C33 C Uani 0.6229(2) 0.64830(14) 0.14381(14) 1.000 0.0446(10) . . C34 C Uani 0.61348(19) 0.62124(14) 0.08810(14) 1.000 0.0403(10) . . C35 C Uani 0.53510(17) 0.63117(12) 0.05669(11) 1.000 0.0273(8) . . C36 C Uani 0.51541(17) 0.60221(11) -0.00155(12) 1.000 0.0275(8) . . C37 C Uani 0.5767(2) 0.56768(13) -0.03410(13) 1.000 0.0377(9) . . C38 C Uani 0.5510(2) 0.54253(14) -0.08787(14) 1.000 0.0447(11) . . C39 C Uani 0.4651(2) 0.55038(14) -0.10718(13) 1.000 0.0438(10) . . C40 C Uani 0.4064(2) 0.58543(12) -0.07325(12) 1.000 0.0339(9) . . C41 C Uani 0.31993(18) 0.57899(12) 0.12054(11) 1.000 0.0315(8) . . C42 C Uani 0.2649(2) 0.53765(13) 0.15007(13) 1.000 0.0371(9) . . C43 C Uani 0.1838(2) 0.52289(13) 0.12535(13) 1.000 0.0406(10) . . C44 C Uani 0.1590(2) 0.54977(13) 0.07255(13) 1.000 0.0386(9) . . C45 C Uani 0.21556(17) 0.59232(12) 0.04494(11) 1.000 0.0276(8) . . C46 C Uani 0.19457(17) 0.62573(12) -0.01022(11) 1.000 0.0294(8) . . C47 C Uani 0.11845(19) 0.61558(14) -0.04498(13) 1.000 0.0407(10) . . C48 C Uani 0.1076(2) 0.64741(15) -0.09752(14) 1.000 0.0471(11) . . C49 C Uani 0.1711(2) 0.68894(14) -0.11433(13) 1.000 0.0420(10) . . C50 C Uani 0.2447(2) 0.69842(13) -0.07847(12) 1.000 0.0349(9) . . C51 C Uani 0.24850(18) 0.73274(13) 0.12033(12) 1.000 0.0330(8) . . C52 C Uani 0.2130(2) 0.78257(14) 0.15019(13) 1.000 0.0417(10) . . C53 C Uani 0.2331(2) 0.84145(14) 0.13085(14) 1.000 0.0442(10) . . C54 C Uani 0.2893(2) 0.84846(13) 0.08280(13) 1.000 0.0395(9) . . C55 C Uani 0.32429(17) 0.79666(12) 0.05456(12) 1.000 0.0291(8) . . C56 C Uani 0.38511(17) 0.79868(12) 0.00333(12) 1.000 0.0282(8) . . C57 C Uani 0.4102(2) 0.85310(13) -0.02482(13) 1.000 0.0369(9) . . C58 C Uani 0.4666(2) 0.85025(14) -0.07400(13) 1.000 0.0387(10) . . C59 C Uani 0.49553(19) 0.79413(13) -0.09364(13) 1.000 0.0359(9) . . C60 C Uani 0.46903(19) 0.74189(13) -0.06369(12) 1.000 0.0334(9) . . Nb1 Nb Uani 0.84019(1) 0.48731(1) 0.20338(1) 1.000 0.0288(1) . . O1 O Uani 0.82279(13) 0.40922(8) 0.20630(9) 1.000 0.0418(6) . . O2 O Uani 0.77325(11) 0.50359(9) 0.12168(8) 1.000 0.0340(6) . . O3 O Uani 0.93795(11) 0.48106(10) 0.13122(8) 1.000 0.0352(6) . . O4 O Uani 0.77947(12) 0.51394(10) 0.02235(8) 1.000 0.0377(6) . . O5 O Uani 0.96375(11) 0.49054(10) 0.03329(8) 1.000 0.0362(6) . . O6 O Uani 0.82489(12) 0.49678(9) 0.29774(8) 1.000 0.0409(6) . . O7 O Uani 0.71288(12) 0.52486(9) 0.21970(8) 1.000 0.0366(6) . . O8 O Uani 0.73900(14) 0.52566(11) 0.37387(9) 1.000 0.0488(8) . . O9 O Uani 0.62299(14) 0.57234(10) 0.28464(9) 1.000 0.0448(7) . . O10 O Uani 0.96858(12) 0.48304(9) 0.24172(8) 1.000 0.0340(6) . . O11 O Uani 0.88960(12) 0.58322(8) 0.20506(9) 1.000 0.0359(6) . . O12 O Uani 1.09189(14) 0.53415(11) 0.26676(10) 1.000 0.0525(8) . . O13 O Uani 1.01179(16) 0.63974(11) 0.22034(10) 1.000 0.0576(8) . . C61 C Uani 0.81360(16) 0.50433(11) 0.07070(11) 1.000 0.0266(8) . . C62 C Uani 0.91456(16) 0.49087(12) 0.07738(12) 1.000 0.0276(8) . . C63 C Uani 0.75390(18) 0.52005(14) 0.32080(12) 1.000 0.0342(8) . . C64 C Uani 0.68870(18) 0.54158(13) 0.27248(12) 1.000 0.0328(8) . . C65 C Uani 1.01590(19) 0.53227(14) 0.24578(12) 1.000 0.0351(9) . . C66 C Uani 0.9707(2) 0.59095(14) 0.22218(11) 1.000 0.0364(9) . . O14 O Uani 0.91138(16) 0.29190(10) 0.21349(12) 1.000 0.0557(9) . . O15 O Uani 1.05405(16) 0.30596(12) 0.29143(14) 1.000 0.0637(9) . . O16 O Uani 1.1572(2) 0.40845(14) 0.27216(19) 1.000 0.0993(16) . . O17 O Uani 0.82234(17) 0.71020(11) 0.19651(12) 1.000 0.0616(9) . . O18 O Uani 0.69974(15) 0.69904(11) 0.29049(12) 1.000 0.0533(8) . . O19 O Uani 0.44361(16) 0.57204(11) 0.24538(13) 1.000 0.0587(9) . . O20 O Uani 0.40198(18) 0.30255(11) 0.22050(13) 1.000 0.0655(10) . . O21 O Uani 0.5789(2) 0.29509(18) 0.24909(16) 1.000 0.1077(16) . . O22 O Uani 0.65091(17) 0.18162(13) 0.24142(16) 1.000 0.0798(13) . . O23 O Uani 0.82863(15) 0.17656(13) 0.22069(14) 1.000 0.0684(10) . . O24 O Uani 0.5654(2) 0.41290(14) 0.30913(15) 1.000 0.0863(12) . . O25 O Uani 0.56765(15) 0.48975(12) 0.41217(10) 1.000 0.0527(8) . . Cl1 Cl Uani 0.36084(6) 0.43770(4) 0.26786(4) 1.000 0.0518(3) . . H1 H Uiso 0.29460 0.27910 0.12100 1.000 0.0360 calc R H2 H Uiso 0.17340 0.29440 0.18100 1.000 0.0430 calc R H3 H Uiso 0.05840 0.35750 0.14920 1.000 0.0480 calc R H4 H Uiso 0.07120 0.40610 0.05640 1.000 0.0440 calc R H7 H Uiso 0.09440 0.44860 -0.03260 1.000 0.0380 calc R H8 H Uiso 0.13310 0.49340 -0.12300 1.000 0.0440 calc R H9 H Uiso 0.27470 0.47690 -0.16100 1.000 0.0420 calc R H10 H Uiso 0.37210 0.41290 -0.11070 1.000 0.0370 calc R H11 H Uiso 0.35940 0.40780 0.11490 1.000 0.0390 calc R H12 H Uiso 0.45680 0.47040 0.16520 1.000 0.0440 calc R H13 H Uiso 0.59560 0.49090 0.12510 1.000 0.0430 calc R H14 H Uiso 0.63000 0.45170 0.03020 1.000 0.0410 calc R H17 H Uiso 0.65250 0.40980 -0.05890 1.000 0.0450 calc R H18 H Uiso 0.66640 0.35730 -0.14960 1.000 0.0510 calc R H19 H Uiso 0.55230 0.29120 -0.17970 1.000 0.0460 calc R H20 H Uiso 0.43290 0.27530 -0.11780 1.000 0.0380 calc R H21 H Uiso 0.50220 0.29680 0.09840 1.000 0.0420 calc R H22 H Uiso 0.54670 0.20910 0.14840 1.000 0.0470 calc R H23 H Uiso 0.48570 0.11520 0.12240 1.000 0.0510 calc R H24 H Uiso 0.38200 0.11080 0.04550 1.000 0.0490 calc R H27 H Uiso 0.29360 0.11400 -0.03340 1.000 0.0480 calc R H28 H Uiso 0.20740 0.12390 -0.11810 1.000 0.0480 calc R H29 H Uiso 0.18140 0.22180 -0.15640 1.000 0.0450 calc R H30 H Uiso 0.23810 0.30640 -0.10710 1.000 0.0380 calc R H31 H Uiso 0.43500 0.71950 0.14610 1.000 0.0400 calc R H32 H Uiso 0.56070 0.70240 0.20300 1.000 0.0490 calc R H33 H Uiso 0.67450 0.64200 0.16620 1.000 0.0540 calc R H34 H Uiso 0.65870 0.59700 0.07210 1.000 0.0480 calc R H37 H Uiso 0.63430 0.56170 -0.01970 1.000 0.0450 calc R H38 H Uiso 0.59160 0.52040 -0.11090 1.000 0.0540 calc R H39 H Uiso 0.44620 0.53240 -0.14280 1.000 0.0520 calc R H40 H Uiso 0.34810 0.59070 -0.08670 1.000 0.0410 calc R H41 H Uiso 0.37560 0.58770 0.13690 1.000 0.0380 calc R H42 H Uiso 0.28270 0.52010 0.18610 1.000 0.0450 calc R H43 H Uiso 0.14610 0.49500 0.14430 1.000 0.0490 calc R H44 H Uiso 0.10460 0.53970 0.05510 1.000 0.0460 calc R H47 H Uiso 0.07540 0.58740 -0.03260 1.000 0.0490 calc R H48 H Uiso 0.05760 0.64070 -0.12130 1.000 0.0560 calc R H49 H Uiso 0.16480 0.71080 -0.14990 1.000 0.0500 calc R H50 H Uiso 0.28710 0.72730 -0.09010 1.000 0.0420 calc R H51 H Uiso 0.23350 0.69330 0.13320 1.000 0.0400 calc R H52 H Uiso 0.17600 0.77660 0.18310 1.000 0.0500 calc R H53 H Uiso 0.20890 0.87560 0.15000 1.000 0.0530 calc R H54 H Uiso 0.30390 0.88770 0.06920 1.000 0.0470 calc R H57 H Uiso 0.38940 0.89090 -0.01090 1.000 0.0440 calc R H58 H Uiso 0.48450 0.88610 -0.09330 1.000 0.0470 calc R H59 H Uiso 0.53270 0.79130 -0.12690 1.000 0.0430 calc R H60 H Uiso 0.49050 0.70400 -0.07670 1.000 0.0400 calc R H141 H Uiso 0.8884(19) 0.3253(8) 0.2039(16) 1.000 0.0670 . . H142 H Uiso 0.9577(15) 0.3003(14) 0.2320(15) 1.000 0.0670 . . H151 H Uiso 1.0850(19) 0.2742(8) 0.2940(19) 1.000 0.0760 . . H152 H Uiso 1.0883(18) 0.3355(9) 0.2959(19) 1.000 0.0760 . . H161 H Uiso 1.123(2) 0.432(2) 0.2533(19) 1.000 0.1190 . . H162 H Uiso 1.2052(17) 0.408(2) 0.2532(19) 1.000 0.1190 . . H171 H Uiso 0.846(2) 0.6756(9) 0.1946(15) 1.000 0.0740 . . H172 H Uiso 0.798(2) 0.7110(15) 0.2300(9) 1.000 0.0740 . . H181 H Uiso 0.6657(17) 0.6684(8) 0.2908(17) 1.000 0.0640 . . H182 H Uiso 0.6658(17) 0.7293(8) 0.2857(16) 1.000 0.0640 . . H191 H Uiso 0.4970(9) 0.5726(15) 0.2550(16) 1.000 0.0700 . . H192 H Uiso 0.4226(19) 0.5397(11) 0.2596(16) 1.000 0.0700 . . H201 H Uiso 0.384(2) 0.3336(12) 0.2390(15) 1.000 0.0790 . . H202 H Uiso 0.4542(11) 0.2976(16) 0.2320(17) 1.000 0.0790 . . H211 H Uiso 0.593(4) 0.2608(8) 0.2638(12) 1.000 0.1290 . . H212 H Uiso 0.5730(18) 0.3189(7) 0.2775(9) 1.000 0.1290 . . H221 H Uiso 0.630(2) 0.1569(17) 0.2169(17) 1.000 0.0960 . . H222 H Uiso 0.7056(8) 0.1746(19) 0.2416(18) 1.000 0.0960 . . H231 H Uiso 0.857(2) 0.2096(9) 0.2155(19) 1.000 0.0820 . . H232 H Uiso 0.8643(19) 0.1526(12) 0.2365(17) 1.000 0.0820 . . H241 H Uiso 0.523(2) 0.4394(16) 0.3006(19) 1.000 0.1030 . . H242 H Uiso 0.589(3) 0.4305(18) 0.3394(14) 1.000 0.1030 . . H251 H Uiso 0.560(2) 0.4919(16) 0.4489(5) 1.000 0.0630 . . H252 H Uiso 0.6141(15) 0.5097(14) 0.4053(12) 1.000 0.0630 . . 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 Fe1 0.0200(2) 0.0218(2) 0.0240(2) 0.0012(1) 0.0007(1) 0.0002(1) N1 0.0214(10) 0.0248(11) 0.0248(10) 0.0023(9) 0.0001(8) -0.0033(9) N2 0.0235(11) 0.0212(10) 0.0250(11) 0.0026(8) 0.0022(8) -0.0013(9) N3 0.0244(11) 0.0256(11) 0.0257(11) -0.0001(9) 0.0019(9) 0.0000(9) N4 0.0236(10) 0.0244(11) 0.0241(10) 0.0013(9) 0.0029(8) 0.0016(9) N5 0.0236(11) 0.0266(11) 0.0276(11) 0.0032(9) 0.0021(9) 0.0026(9) N6 0.0226(11) 0.0278(12) 0.0278(11) -0.0005(9) 0.0019(9) 0.0003(9) C1 0.0292(14) 0.0316(14) 0.0289(14) 0.0078(11) 0.0025(11) -0.0007(11) C2 0.0355(16) 0.0421(17) 0.0296(14) 0.0077(12) 0.0071(12) -0.0014(12) C3 0.0298(15) 0.0512(18) 0.0384(16) 0.0081(14) 0.0156(13) 0.0035(13) C4 0.0254(14) 0.0395(16) 0.0441(16) 0.0082(13) 0.0074(12) 0.0055(12) C5 0.0230(13) 0.0240(13) 0.0286(13) 0.0031(10) 0.0004(10) 0.0003(10) C6 0.0248(13) 0.0237(12) 0.0271(13) 0.0008(10) 0.0024(10) 0.0006(10) C7 0.0269(14) 0.0344(14) 0.0341(14) 0.0044(11) 0.0004(11) 0.0073(12) C8 0.0395(16) 0.0368(16) 0.0331(14) 0.0076(12) -0.0031(12) 0.0095(12) C9 0.0414(17) 0.0335(15) 0.0295(14) 0.0099(12) 0.0031(12) 0.0026(13) C10 0.0301(14) 0.0322(14) 0.0309(14) 0.0052(11) 0.0053(11) -0.0022(11) C11 0.0302(14) 0.0379(15) 0.0286(14) -0.0049(12) 0.0046(11) -0.0028(12) C12 0.0399(17) 0.0340(15) 0.0354(15) -0.0085(12) 0.0009(13) -0.0038(13) C13 0.0337(15) 0.0311(15) 0.0432(16) -0.0064(12) -0.0082(13) -0.0020(12) C14 0.0274(15) 0.0324(15) 0.0437(16) -0.0025(13) -0.0004(12) -0.0058(12) C15 0.0211(13) 0.0245(12) 0.0323(13) 0.0035(11) 0.0008(10) 0.0009(10) C16 0.0246(13) 0.0288(14) 0.0297(14) 0.0031(11) 0.0023(11) 0.0025(11) C17 0.0275(14) 0.0389(16) 0.0467(17) -0.0001(13) 0.0094(13) -0.0025(12) C18 0.0364(17) 0.0498(18) 0.0424(17) -0.0012(14) 0.0204(14) 0.0025(14) C19 0.0392(16) 0.0413(17) 0.0343(15) -0.0035(13) 0.0084(13) 0.0072(13) C20 0.0287(14) 0.0322(14) 0.0331(15) -0.0039(11) -0.0007(11) 0.0054(12) C21 0.0294(14) 0.0376(16) 0.0373(16) 0.0054(13) -0.0028(12) 0.0005(12) C22 0.0316(15) 0.0469(19) 0.0381(16) 0.0109(14) -0.0049(12) 0.0071(13) C23 0.0497(19) 0.0377(17) 0.0396(17) 0.0126(13) 0.0041(14) 0.0145(14) C24 0.056(2) 0.0268(14) 0.0403(17) 0.0023(12) -0.0003(15) 0.0047(14) C25 0.0325(14) 0.0245(13) 0.0298(13) 0.0012(11) 0.0024(11) 0.0048(11) C26 0.0330(15) 0.0242(13) 0.0330(14) -0.0002(11) 0.0045(11) 0.0000(10) C27 0.0500(19) 0.0268(15) 0.0441(17) -0.0026(12) 0.0012(14) -0.0026(13) C28 0.0442(18) 0.0352(17) 0.0417(17) -0.0141(13) 0.0072(14) -0.0121(13) C29 0.0335(15) 0.0458(18) 0.0327(15) -0.0099(13) -0.0024(12) -0.0055(13) C30 0.0300(14) 0.0318(15) 0.0332(15) -0.0015(12) -0.0029(11) -0.0026(12) Fe2 0.0230(2) 0.0228(2) 0.0216(2) -0.0008(1) -0.0013(1) 0.0005(2) N7 0.0251(11) 0.0262(11) 0.0235(10) 0.0013(9) -0.0028(8) -0.0033(9) N8 0.0300(12) 0.0229(10) 0.0217(10) 0.0007(8) 0.0002(9) 0.0025(9) N9 0.0246(11) 0.0258(11) 0.0256(11) -0.0018(9) -0.0004(9) 0.0005(9) N10 0.0278(11) 0.0294(11) 0.0261(10) -0.0019(9) -0.0053(9) 0.0043(10) N11 0.0257(11) 0.0297(12) 0.0260(11) -0.0006(9) -0.0011(9) 0.0013(9) N12 0.0253(11) 0.0276(11) 0.0263(12) 0.0001(9) -0.0007(9) -0.0003(9) C31 0.0329(15) 0.0360(15) 0.0308(14) -0.0022(12) -0.0055(12) -0.0051(12) C32 0.0461(18) 0.0411(17) 0.0347(16) 0.0003(13) -0.0156(13) -0.0107(14) C33 0.0368(17) 0.0468(17) 0.0503(18) 0.0063(15) -0.0216(14) -0.0070(14) C34 0.0281(15) 0.0386(16) 0.0541(19) 0.0016(14) -0.0096(13) -0.0027(12) C35 0.0233(13) 0.0265(13) 0.0322(14) 0.0043(11) -0.0013(11) -0.0026(10) C36 0.0274(14) 0.0257(13) 0.0293(13) 0.0038(11) 0.0045(11) 0.0019(10) C37 0.0339(16) 0.0377(16) 0.0414(16) 0.0039(13) 0.0085(13) 0.0065(13) C38 0.0486(19) 0.0421(18) 0.0434(18) -0.0013(14) 0.0161(15) 0.0119(14) C39 0.065(2) 0.0364(17) 0.0299(15) -0.0074(13) 0.0074(15) 0.0067(15) C40 0.0405(16) 0.0324(15) 0.0289(14) -0.0054(12) -0.0010(12) 0.0045(12) C41 0.0318(15) 0.0316(14) 0.0310(14) 0.0044(11) -0.0034(11) 0.0018(11) C42 0.0447(18) 0.0355(15) 0.0312(14) 0.0085(12) 0.0026(13) -0.0027(13) C43 0.0456(18) 0.0346(16) 0.0417(16) 0.0029(13) 0.0123(13) -0.0101(13) C44 0.0327(15) 0.0403(16) 0.0427(16) -0.0077(13) 0.0039(13) -0.0078(13) C45 0.0242(13) 0.0278(13) 0.0307(14) -0.0063(11) 0.0012(10) -0.0030(11) C46 0.0229(13) 0.0357(15) 0.0297(14) -0.0061(11) -0.0010(10) 0.0036(11) C47 0.0299(16) 0.0462(18) 0.0461(17) -0.0044(14) -0.0104(13) -0.0025(13) C48 0.0431(18) 0.056(2) 0.0423(17) -0.0102(15) -0.0218(14) 0.0096(16) C49 0.0513(19) 0.0419(17) 0.0328(15) -0.0033(12) -0.0156(14) 0.0103(15) C50 0.0398(16) 0.0350(15) 0.0299(14) 0.0019(12) -0.0074(12) 0.0078(13) C51 0.0339(15) 0.0346(15) 0.0305(14) -0.0010(12) 0.0060(12) 0.0020(12) C52 0.0445(18) 0.0467(19) 0.0339(16) -0.0080(13) 0.0101(13) 0.0037(14) C53 0.0468(18) 0.0384(18) 0.0474(18) -0.0134(14) 0.0099(15) 0.0109(14) C54 0.0481(18) 0.0269(14) 0.0434(17) -0.0037(13) 0.0009(14) 0.0048(13) C55 0.0291(14) 0.0254(13) 0.0327(14) -0.0012(11) -0.0051(11) 0.0015(11) C56 0.0281(14) 0.0283(13) 0.0281(13) 0.0007(11) -0.0037(11) -0.0006(10) C57 0.0465(17) 0.0270(14) 0.0373(16) 0.0026(12) -0.0032(14) -0.0050(13) C58 0.0471(18) 0.0338(16) 0.0353(16) 0.0088(12) -0.0032(14) -0.0081(13) C59 0.0324(15) 0.0411(17) 0.0343(15) 0.0043(13) 0.0042(12) -0.0023(13) C60 0.0362(16) 0.0364(16) 0.0277(14) 0.0031(12) 0.0042(12) 0.0058(12) Nb1 0.0244(1) 0.0341(1) 0.0278(1) 0.0016(1) -0.0042(1) 0.0050(1) O1 0.0429(12) 0.0349(10) 0.0477(11) 0.0024(9) -0.0079(10) 0.0009(8) O2 0.0220(9) 0.0505(12) 0.0295(10) 0.0015(8) -0.0008(8) 0.0059(8) O3 0.0241(9) 0.0507(12) 0.0307(10) -0.0012(9) -0.0035(8) 0.0096(9) O4 0.0283(10) 0.0547(12) 0.0301(10) 0.0040(10) -0.0057(8) 0.0010(9) O5 0.0229(9) 0.0515(12) 0.0341(10) -0.0018(9) 0.0005(8) 0.0060(9) O6 0.0327(10) 0.0650(14) 0.0251(9) 0.0096(9) -0.0040(8) 0.0112(9) O7 0.0267(10) 0.0559(13) 0.0271(10) 0.0016(9) -0.0036(7) 0.0095(9) O8 0.0391(12) 0.0782(17) 0.0292(11) -0.0040(11) -0.0005(9) -0.0035(11) O9 0.0388(12) 0.0549(13) 0.0408(12) -0.0026(10) 0.0034(9) 0.0126(10) O10 0.0279(9) 0.0403(11) 0.0339(10) 0.0034(9) -0.0071(8) 0.0072(9) O11 0.0363(11) 0.0334(10) 0.0380(10) 0.0030(9) -0.0091(9) 0.0019(8) O12 0.0305(11) 0.0800(17) 0.0470(13) 0.0137(12) -0.0120(10) -0.0076(11) O13 0.0642(16) 0.0565(14) 0.0522(14) 0.0121(11) -0.0187(12) -0.0210(12) C61 0.0226(11) 0.0270(14) 0.0303(14) -0.0024(10) -0.0023(10) 0.0004(10) C62 0.0226(12) 0.0263(13) 0.0340(14) -0.0059(12) -0.0029(11) -0.0011(11) C63 0.0288(14) 0.0418(16) 0.0321(14) 0.0004(13) -0.0020(11) -0.0059(13) C64 0.0286(14) 0.0350(15) 0.0347(15) 0.0013(12) -0.0006(11) -0.0031(11) C65 0.0303(15) 0.0512(18) 0.0239(13) 0.0039(12) -0.0002(11) 0.0009(13) C66 0.0421(17) 0.0457(17) 0.0215(13) 0.0007(12) -0.0044(12) -0.0057(14) O14 0.0541(15) 0.0457(13) 0.0674(17) -0.0004(12) -0.0014(12) 0.0139(11) O15 0.0599(16) 0.0534(15) 0.0779(18) 0.0133(15) -0.0066(15) 0.0002(12) O16 0.0623(19) 0.0655(19) 0.170(4) -0.0121(19) 0.030(2) 0.0054(16) O17 0.0523(15) 0.0511(14) 0.0813(19) -0.0009(13) 0.0036(14) 0.0101(11) O18 0.0465(13) 0.0524(13) 0.0611(14) -0.0096(13) -0.0092(12) -0.0005(11) O19 0.0433(14) 0.0490(14) 0.0839(19) 0.0057(13) -0.0149(13) -0.0015(11) O20 0.0677(17) 0.0449(14) 0.084(2) -0.0148(13) -0.0140(15) 0.0058(13) O21 0.072(2) 0.125(3) 0.126(3) -0.072(2) -0.015(2) 0.022(2) O22 0.0404(14) 0.0700(19) 0.129(3) 0.0322(17) -0.0001(16) -0.0047(13) O23 0.0429(14) 0.0653(16) 0.097(2) 0.0211(16) -0.0083(13) 0.0115(12) O24 0.089(2) 0.086(2) 0.084(2) -0.0220(18) -0.0159(17) -0.0004(17) O25 0.0483(13) 0.0690(16) 0.0408(12) -0.0089(12) 0.0060(10) -0.0125(12) Cl1 0.0611(5) 0.0478(4) 0.0466(4) 0.0006(3) 0.0041(4) 0.0066(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O7 2.1052(18) . . no Nb1 O10 2.1071(18) . . no Nb1 O11 2.2100(18) . . no Nb1 O3 2.1825(18) . . no Nb1 O1 1.7162(18) . . no Nb1 O2 2.1129(18) . . no Nb1 O6 2.1314(18) . . no Fe1 N4 1.968(2) . . no Fe1 N1 1.972(2) . . no Fe1 N2 1.981(2) . . no Fe1 N3 1.971(2) . . no Fe1 N5 1.981(2) . . no Fe1 N6 1.971(2) . . no Fe2 N7 1.972(2) . . no Fe2 N8 1.976(2) . . no Fe2 N9 1.965(2) . . no Fe2 N10 1.967(2) . . no Fe2 N11 1.979(2) . . no Fe2 N12 1.971(2) . . no O2 C61 1.290(3) . . no O3 C62 1.271(3) . . no O4 C61 1.214(3) . . no O5 C62 1.230(3) . . no O6 C63 1.285(3) . . no O7 C64 1.286(3) . . no O8 C63 1.213(3) . . no O9 C64 1.220(3) . . no O10 C65 1.286(4) . . no O11 C66 1.284(3) . . no O12 C65 1.232(4) . . no O13 C66 1.226(4) . . no O14 H142 0.83(3) . . no O14 H141 0.83(2) . . no O15 H151 0.83(2) . . no O15 H152 0.83(2) . . no N1 C5 1.357(3) . . no N1 C1 1.351(3) . . no N2 C10 1.346(3) . . no N2 C6 1.351(3) . . no N3 C15 1.356(3) . . no N3 C11 1.344(3) . . no N4 C20 1.358(3) . . no N4 C16 1.347(3) . . no N5 C21 1.344(3) . . no N5 C25 1.359(3) . . no N6 C30 1.348(3) . . no N6 C26 1.357(3) . . no O16 H161 0.84(4) . . no O16 H162 0.83(3) . . no N7 C35 1.347(3) . . no N7 C31 1.345(3) . . no N8 C40 1.353(3) . . no N8 C36 1.351(3) . . no N9 C41 1.350(3) . . no N9 C45 1.361(3) . . no N10 C50 1.355(3) . . no N10 C46 1.350(3) . . no N11 C55 1.358(3) . . no N11 C51 1.355(3) . . no N12 C60 1.351(3) . . no N12 C56 1.349(3) . . no O17 H171 0.83(2) . . no O17 H172 0.83(2) . . no O18 H182 0.84(2) . . no O18 H181 0.84(2) . . no O19 H192 0.83(3) . . no O19 H191 0.828(17) . . no O20 H202 0.83(2) . . no O20 H201 0.84(3) . . no C1 C2 1.371(4) . . no C2 C3 1.369(4) . . no C3 C4 1.389(4) . . no C4 C5 1.381(4) . . no C5 C6 1.475(3) . . no C6 C7 1.389(4) . . no C7 C8 1.376(4) . . no C8 C9 1.370(4) . . no C9 C10 1.389(4) . . no C11 C12 1.379(4) . . no C12 C13 1.364(4) . . no C13 C14 1.394(4) . . no C14 C15 1.385(4) . . no C15 C16 1.479(3) . . no C16 C17 1.394(4) . . no C17 C18 1.389(4) . . no C18 C19 1.388(4) . . no C19 C20 1.370(4) . . no C21 C22 1.391(4) . . no C22 C23 1.368(4) . . no C23 C24 1.379(4) . . no C24 C25 1.394(4) . . no C25 C26 1.462(4) . . no C26 C27 1.389(4) . . no C27 C28 1.364(4) . . no C28 C29 1.377(4) . . no C29 C30 1.388(4) . . no C1 H1 0.9298 . . no C2 H2 0.9298 . . no C3 H3 0.9302 . . no C4 H4 0.9299 . . no C7 H7 0.9298 . . no C8 H8 0.9303 . . no C9 H9 0.9295 . . no C10 H10 0.9302 . . no C11 H11 0.9296 . . no C12 H12 0.9311 . . no C13 H13 0.9293 . . no C14 H14 0.9306 . . no C17 H17 0.9296 . . no C18 H18 0.9298 . . no C19 H19 0.9304 . . no C20 H20 0.9295 . . no C21 H21 0.9294 . . no O21 H212 0.824(19) . . no O21 H211 0.84(3) . . no C22 H22 0.9304 . . no C23 H23 0.9292 . . no C24 H24 0.9293 . . no C27 H27 0.9311 . . no C28 H28 0.9296 . . no C29 H29 0.9297 . . no C30 H30 0.9302 . . no C31 C32 1.384(4) . . no C32 C33 1.363(4) . . no C33 C34 1.384(4) . . no C34 C35 1.385(4) . . no C35 C36 1.475(4) . . no C36 C37 1.391(4) . . no C37 C38 1.375(4) . . no C38 C39 1.368(4) . . no C39 C40 1.388(4) . . no C41 C42 1.386(4) . . no C42 C43 1.372(4) . . no C43 C44 1.368(4) . . no C44 C45 1.397(4) . . no C45 C46 1.465(4) . . no C46 C47 1.397(4) . . no C47 C48 1.372(4) . . no C48 C49 1.363(4) . . no C49 C50 1.378(4) . . no C51 C52 1.378(4) . . no C52 C53 1.382(4) . . no C53 C54 1.373(4) . . no C54 C55 1.392(4) . . no C55 C56 1.464(4) . . no C56 C57 1.390(4) . . no C57 C58 1.388(4) . . no C58 C59 1.366(4) . . no C59 C60 1.375(4) . . no O22 H221 0.83(4) . . no O22 H222 0.833(14) . . no C31 H31 0.9300 . . no C32 H32 0.9307 . . no C33 H33 0.9307 . . no C34 H34 0.9292 . . no C37 H37 0.9298 . . no C38 H38 0.9303 . . no C39 H39 0.9307 . . no C40 H40 0.9304 . . no C41 H41 0.9298 . . no C42 H42 0.9299 . . no C43 H43 0.9299 . . no C44 H44 0.9293 . . no C47 H47 0.9308 . . no C48 H48 0.9297 . . no C49 H49 0.9307 . . no C50 H50 0.9294 . . no C51 H51 0.9307 . . no C52 H52 0.9300 . . no C53 H53 0.9296 . . no C54 H54 0.9305 . . no C57 H57 0.9312 . . no C58 H58 0.9293 . . no C59 H59 0.9307 . . no C60 H60 0.9298 . . no C61 C62 1.547(3) . . no C63 C64 1.529(4) . . no C65 C66 1.536(4) . . no O23 H231 0.84(2) . . no O23 H232 0.83(3) . . no O24 H241 0.88(3) . . no O24 H242 0.85(4) . . no O25 H251 0.830(12) . . no O25 H252 0.83(3) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O10 142.35(7) . . . no O2 Nb1 O11 90.91(7) . . . no O3 Nb1 O6 144.03(7) . . . no O3 Nb1 O7 139.43(7) . . . no O3 Nb1 O10 71.68(7) . . . no O3 Nb1 O11 81.17(8) . . . no O6 Nb1 O7 72.17(7) . . . no O6 Nb1 O10 72.54(7) . . . no O6 Nb1 O11 85.89(7) . . . no O7 Nb1 O10 140.61(7) . . . no O7 Nb1 O11 86.30(7) . . . no O10 Nb1 O11 74.27(7) . . . no O1 Nb1 O6 92.37(9) . . . no O1 Nb1 O7 103.79(8) . . . no O1 Nb1 O10 94.57(8) . . . no O1 Nb1 O11 168.72(8) . . . no O2 Nb1 O3 71.94(6) . . . no O2 Nb1 O6 142.01(7) . . . no O2 Nb1 O7 69.84(7) . . . no O1 Nb1 O3 93.93(9) . . . no O1 Nb1 O2 97.24(9) . . . no N1 Fe1 N3 94.19(9) . . . no N1 Fe1 N4 173.55(9) . . . no N1 Fe1 N6 90.04(9) . . . no N2 Fe1 N3 93.40(9) . . . no N1 Fe1 N5 93.28(9) . . . no N1 Fe1 N2 81.21(9) . . . no N4 Fe1 N5 91.64(8) . . . no N4 Fe1 N6 94.81(8) . . . no N5 Fe1 N6 81.59(9) . . . no N3 Fe1 N6 173.54(9) . . . no N2 Fe1 N5 171.62(9) . . . no N2 Fe1 N6 92.07(9) . . . no N2 Fe1 N4 94.35(8) . . . no N3 Fe1 N5 93.29(9) . . . no N3 Fe1 N4 81.34(8) . . . no N7 Fe2 N8 81.24(9) . . . no N11 Fe2 N12 81.48(9) . . . no N8 Fe2 N10 93.30(9) . . . no N8 Fe2 N11 173.24(9) . . . no N7 Fe2 N9 94.50(9) . . . no N7 Fe2 N10 173.23(9) . . . no N7 Fe2 N11 95.04(9) . . . no N7 Fe2 N12 90.66(9) . . . no N8 Fe2 N9 93.00(9) . . . no N10 Fe2 N12 93.64(9) . . . no N9 Fe2 N10 81.72(9) . . . no N9 Fe2 N11 92.92(9) . . . no N8 Fe2 N12 92.88(9) . . . no N10 Fe2 N11 90.78(9) . . . no N9 Fe2 N12 172.71(9) . . . no Nb1 O2 C61 122.91(15) . . . no Nb1 O3 C62 120.29(15) . . . no Nb1 O6 C63 121.59(17) . . . no Nb1 O7 C64 121.54(17) . . . no Nb1 O10 C65 119.68(17) . . . no Nb1 O11 C66 116.41(17) . . . no H141 O14 H142 107(3) . . . no H151 O15 H152 107(2) . . . no Fe1 N1 C5 115.55(16) . . . no Fe1 N1 C1 127.36(17) . . . no C1 N1 C5 117.1(2) . . . no Fe1 N2 C6 114.97(16) . . . no Fe1 N2 C10 126.70(17) . . . no C6 N2 C10 117.8(2) . . . no Fe1 N3 C15 115.32(16) . . . no Fe1 N3 C11 127.60(18) . . . no C11 N3 C15 117.0(2) . . . no Fe1 N4 C16 115.85(16) . . . no Fe1 N4 C20 126.35(17) . . . no C16 N4 C20 117.8(2) . . . no Fe1 N5 C25 114.42(16) . . . no Fe1 N5 C21 128.05(18) . . . no C21 N5 C25 117.5(2) . . . no Fe1 N6 C26 114.89(17) . . . no C26 N6 C30 117.7(2) . . . no Fe1 N6 C30 127.43(18) . . . no H161 O16 H162 106(4) . . . no Fe2 N7 C31 126.47(17) . . . no C31 N7 C35 118.1(2) . . . no Fe2 N7 C35 115.42(16) . . . no Fe2 N8 C40 126.80(18) . . . no C36 N8 C40 117.9(2) . . . no Fe2 N8 C36 114.96(16) . . . no C41 N9 C45 117.7(2) . . . no Fe2 N9 C45 114.84(16) . . . no Fe2 N9 C41 127.39(18) . . . no C46 N10 C50 118.1(2) . . . no Fe2 N10 C50 126.69(18) . . . no Fe2 N10 C46 115.18(16) . . . no Fe2 N11 C55 114.98(17) . . . no C51 N11 C55 117.4(2) . . . no Fe2 N11 C51 127.63(18) . . . no Fe2 N12 C56 114.92(17) . . . no C56 N12 C60 117.8(2) . . . no Fe2 N12 C60 127.24(18) . . . no H171 O17 H172 105(3) . . . no H181 O18 H182 105(2) . . . no H191 O19 H192 106(3) . . . no H201 O20 H202 105(3) . . . no N1 C1 C2 123.1(2) . . . no C1 C2 C3 119.7(3) . . . no C2 C3 C4 118.5(3) . . . no C3 C4 C5 119.3(3) . . . no N1 C5 C6 113.6(2) . . . no C4 C5 C6 124.0(2) . . . no N1 C5 C4 122.3(2) . . . no N2 C6 C5 114.2(2) . . . no C5 C6 C7 123.8(2) . . . no N2 C6 C7 122.1(2) . . . no C6 C7 C8 119.4(2) . . . no C7 C8 C9 119.0(3) . . . no C8 C9 C10 119.3(3) . . . no N2 C10 C9 122.4(2) . . . no N3 C11 C12 123.2(2) . . . no C11 C12 C13 119.8(3) . . . no C12 C13 C14 118.5(3) . . . no C13 C14 C15 118.8(2) . . . no C14 C15 C16 123.6(2) . . . no N3 C15 C16 113.7(2) . . . no N3 C15 C14 122.7(2) . . . no N4 C16 C17 122.6(2) . . . no N4 C16 C15 113.7(2) . . . no C15 C16 C17 123.7(2) . . . no C16 C17 C18 118.5(3) . . . no C17 C18 C19 119.1(3) . . . no C18 C19 C20 119.2(3) . . . no N4 C20 C19 122.8(2) . . . no N5 C21 C22 122.9(3) . . . no C21 C22 C23 119.2(3) . . . no C22 C23 C24 119.2(3) . . . no C23 C24 C25 119.3(3) . . . no C24 C25 C26 123.7(2) . . . no N5 C25 C24 122.0(2) . . . no N5 C25 C26 114.3(2) . . . no N6 C26 C25 114.4(2) . . . no C25 C26 C27 124.2(2) . . . no N6 C26 C27 121.4(2) . . . no C26 C27 C28 120.5(3) . . . no C27 C28 C29 118.6(3) . . . no C28 C29 C30 119.2(3) . . . no N6 C30 C29 122.7(3) . . . no N1 C1 H1 118.41 . . . no C2 C1 H1 118.46 . . . no C1 C2 H2 120.14 . . . no C3 C2 H2 120.20 . . . no C4 C3 H3 120.78 . . . no C2 C3 H3 120.75 . . . no C5 C4 H4 120.34 . . . no C3 C4 H4 120.34 . . . no C8 C7 H7 120.22 . . . no C6 C7 H7 120.36 . . . no C9 C8 H8 120.53 . . . no C7 C8 H8 120.52 . . . no C8 C9 H9 120.33 . . . no C10 C9 H9 120.34 . . . no C9 C10 H10 118.81 . . . no N2 C10 H10 118.76 . . . no N3 C11 H11 118.34 . . . no C12 C11 H11 118.49 . . . no C13 C12 H12 120.18 . . . no C11 C12 H12 120.07 . . . no C12 C13 H13 120.75 . . . no C14 C13 H13 120.72 . . . no C13 C14 H14 120.63 . . . no C15 C14 H14 120.54 . . . no C18 C17 H17 120.78 . . . no C16 C17 H17 120.76 . . . no C17 C18 H18 120.40 . . . no C19 C18 H18 120.47 . . . no C18 C19 H19 120.40 . . . no C20 C19 H19 120.44 . . . no C19 C20 H20 118.61 . . . no N4 C20 H20 118.59 . . . no C22 C21 H21 118.51 . . . no N5 C21 H21 118.60 . . . no H211 O21 H212 106(2) . . . no C21 C22 H22 120.46 . . . no C23 C22 H22 120.34 . . . no C24 C23 H23 120.42 . . . no C22 C23 H23 120.42 . . . no C25 C24 H24 120.38 . . . no C23 C24 H24 120.34 . . . no C28 C27 H27 119.80 . . . no C26 C27 H27 119.71 . . . no C27 C28 H28 120.68 . . . no C29 C28 H28 120.74 . . . no C30 C29 H29 120.35 . . . no C28 C29 H29 120.50 . . . no N6 C30 H30 118.69 . . . no C29 C30 H30 118.64 . . . no N7 C31 C32 121.7(2) . . . no C31 C32 C33 119.9(3) . . . no C32 C33 C34 119.1(3) . . . no C33 C34 C35 118.5(3) . . . no C34 C35 C36 123.4(2) . . . no N7 C35 C36 113.9(2) . . . no N7 C35 C34 122.6(2) . . . no N8 C36 C35 113.9(2) . . . no N8 C36 C37 122.1(2) . . . no C35 C36 C37 124.0(2) . . . no C36 C37 C38 119.1(3) . . . no C37 C38 C39 119.3(3) . . . no C38 C39 C40 119.4(3) . . . no N8 C40 C39 122.0(3) . . . no N9 C41 C42 122.9(2) . . . no C41 C42 C43 119.1(3) . . . no C42 C43 C44 119.2(3) . . . no C43 C44 C45 119.9(3) . . . no C44 C45 C46 124.7(2) . . . no N9 C45 C46 114.0(2) . . . no N9 C45 C44 121.3(2) . . . no N10 C46 C47 121.4(2) . . . no C45 C46 C47 124.4(2) . . . no N10 C46 C45 114.2(2) . . . no C46 C47 C48 119.6(3) . . . no C47 C48 C49 119.1(3) . . . no C48 C49 C50 119.8(3) . . . no N10 C50 C49 122.2(3) . . . no N11 C51 C52 122.8(3) . . . no C51 C52 C53 119.4(3) . . . no C52 C53 C54 118.7(3) . . . no C53 C54 C55 119.7(3) . . . no C54 C55 C56 124.4(2) . . . no N11 C55 C56 113.7(2) . . . no N11 C55 C54 121.9(2) . . . no C55 C56 C57 123.2(2) . . . no N12 C56 C57 121.9(2) . . . no N12 C56 C55 114.9(2) . . . no C56 C57 C58 119.0(3) . . . no C57 C58 C59 119.2(3) . . . no C58 C59 C60 119.2(3) . . . no N12 C60 C59 122.9(3) . . . no H221 O22 H222 105(4) . . . no N7 C31 H31 119.17 . . . no C32 C31 H31 119.12 . . . no C31 C32 H32 119.98 . . . no C33 C32 H32 120.08 . . . no C34 C33 H33 120.40 . . . no C32 C33 H33 120.49 . . . no C33 C34 H34 120.82 . . . no C35 C34 H34 120.72 . . . no C38 C37 H37 120.45 . . . no C36 C37 H37 120.43 . . . no C37 C38 H38 120.38 . . . no C39 C38 H38 120.30 . . . no C38 C39 H39 120.25 . . . no C40 C39 H39 120.31 . . . no C39 C40 H40 119.02 . . . no N8 C40 H40 118.95 . . . no N9 C41 H41 118.62 . . . no C42 C41 H41 118.53 . . . no C43 C42 H42 120.45 . . . no C41 C42 H42 120.49 . . . no C42 C43 H43 120.40 . . . no C44 C43 H43 120.39 . . . no C45 C44 H44 120.11 . . . no C43 C44 H44 119.98 . . . no C46 C47 H47 120.23 . . . no C48 C47 H47 120.22 . . . no C49 C48 H48 120.52 . . . no C47 C48 H48 120.38 . . . no C50 C49 H49 120.11 . . . no C48 C49 H49 120.13 . . . no C49 C50 H50 118.97 . . . no N10 C50 H50 118.87 . . . no C52 C51 H51 118.65 . . . no N11 C51 H51 118.51 . . . no C51 C52 H52 120.24 . . . no C53 C52 H52 120.39 . . . no C54 C53 H53 120.72 . . . no C52 C53 H53 120.56 . . . no C55 C54 H54 120.20 . . . no C53 C54 H54 120.07 . . . no C58 C57 H57 120.50 . . . no C56 C57 H57 120.48 . . . no C59 C58 H58 120.42 . . . no C57 C58 H58 120.39 . . . no C58 C59 H59 120.36 . . . no C60 C59 H59 120.46 . . . no N12 C60 H60 118.54 . . . no C59 C60 H60 118.52 . . . no O4 C61 C62 122.0(2) . . . no O2 C61 O4 126.3(2) . . . no O2 C61 C62 111.7(2) . . . no O3 C62 C61 113.1(2) . . . no O5 C62 C61 120.6(2) . . . no O3 C62 O5 126.3(2) . . . no O6 C63 O8 125.7(3) . . . no O8 C63 C64 122.9(3) . . . no O6 C63 C64 111.4(2) . . . no O7 C64 O9 125.9(3) . . . no O9 C64 C63 121.7(2) . . . no O7 C64 C63 112.4(2) . . . no O10 C65 C66 115.0(2) . . . no O12 C65 C66 120.7(3) . . . no O10 C65 O12 124.3(3) . . . no O13 C66 C65 120.5(3) . . . no O11 C66 O13 125.3(3) . . . no O11 C66 C65 114.3(2) . . . no H231 O23 H232 106(3) . . . no H241 O24 H242 100(4) . . . no H251 O25 H252 106(3) . . . no 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 O11 Nb1 O2 C61 78.86(19) . . . . no O1 Nb1 O3 C62 98.4(2) . . . . no O2 Nb1 O3 C62 2.00(19) . . . . no O6 Nb1 O3 C62 -162.14(18) . . . . no O7 Nb1 O3 C62 -18.3(3) . . . . no O10 Nb1 O3 C62 -168.1(2) . . . . no O11 Nb1 O3 C62 -91.9(2) . . . . no O1 Nb1 O6 C63 -105.4(2) . . . . no O2 Nb1 O6 C63 -0.4(3) . . . . no O3 Nb1 O6 C63 154.6(2) . . . . no O7 Nb1 O6 C63 -1.7(2) . . . . no O10 Nb1 O6 C63 160.6(2) . . . . no O11 Nb1 O6 C63 85.8(2) . . . . no O1 Nb1 O7 C64 95.3(2) . . . . no O2 Nb1 O7 C64 -171.9(2) . . . . no O3 Nb1 O7 C64 -151.43(19) . . . . no O6 Nb1 O7 C64 7.3(2) . . . . no O10 Nb1 O7 C64 -20.1(3) . . . . no O11 Nb1 O7 C64 -79.6(2) . . . . no O1 Nb1 O10 C65 174.95(19) . . . . no O2 Nb1 O10 C65 66.9(2) . . . . no O3 Nb1 O10 C65 82.31(19) . . . . no O6 Nb1 O10 C65 -94.00(19) . . . . no O7 Nb1 O10 C65 -66.7(2) . . . . no O11 Nb1 O10 C65 -3.40(18) . . . . no O2 Nb1 O11 C66 -139.13(18) . . . . no O1 Nb1 O2 C61 -93.3(2) . . . . no O3 Nb1 O2 C61 -1.55(18) . . . . no O6 Nb1 O2 C61 163.34(17) . . . . no O7 Nb1 O2 C61 164.6(2) . . . . no O10 Nb1 O2 C61 13.9(3) . . . . no O10 Nb1 O11 C66 5.77(17) . . . . no O3 Nb1 O11 C66 -67.57(18) . . . . no O6 Nb1 O11 C66 78.78(18) . . . . no O7 Nb1 O11 C66 151.14(19) . . . . no N2 Fe1 N1 C5 4.38(17) . . . . no N3 Fe1 N1 C1 -81.0(2) . . . . no N3 Fe1 N1 C5 97.18(18) . . . . no N2 Fe1 N1 C1 -173.8(2) . . . . no N1 Fe1 N2 C6 -6.63(17) . . . . no N1 Fe1 N2 C10 -178.0(2) . . . . no N3 Fe1 N2 C6 -100.36(18) . . . . no N5 Fe1 N1 C1 12.5(2) . . . . no N5 Fe1 N1 C5 -169.28(18) . . . . no N6 Fe1 N1 C1 94.1(2) . . . . no N6 Fe1 N1 C5 -87.70(18) . . . . no N6 Fe1 N2 C10 -88.2(2) . . . . no N1 Fe1 N3 C11 7.4(2) . . . . no N1 Fe1 N3 C15 -177.08(18) . . . . no N2 Fe1 N3 C11 88.8(2) . . . . no N2 Fe1 N3 C15 -95.66(18) . . . . no N4 Fe1 N3 C11 -177.3(2) . . . . no N4 Fe1 N3 C15 -1.77(17) . . . . no N5 Fe1 N3 C11 -86.2(2) . . . . no N5 Fe1 N3 C15 89.39(18) . . . . no N2 Fe1 N4 C16 92.72(18) . . . . no N2 Fe1 N4 C20 -85.7(2) . . . . no N3 Fe1 N2 C10 88.3(2) . . . . no N4 Fe1 N2 C6 178.08(17) . . . . no N4 Fe1 N2 C10 6.8(2) . . . . no N6 Fe1 N2 C6 83.09(18) . . . . no N5 Fe1 N4 C16 -93.15(18) . . . . no N5 Fe1 N4 C20 88.5(2) . . . . no N6 Fe1 N4 C16 -174.84(18) . . . . no N6 Fe1 N4 C20 6.8(2) . . . . no N1 Fe1 N5 C21 -93.2(2) . . . . no N1 Fe1 N5 C25 83.73(18) . . . . no N3 Fe1 N5 C21 1.2(2) . . . . no N3 Fe1 N5 C25 178.13(18) . . . . no N4 Fe1 N5 C21 82.6(2) . . . . no N4 Fe1 N5 C25 -100.45(18) . . . . no N6 Fe1 N5 C21 177.2(2) . . . . no N6 Fe1 N5 C25 -5.83(18) . . . . no N1 Fe1 N6 C26 -88.24(19) . . . . no N1 Fe1 N6 C30 92.2(2) . . . . no N2 Fe1 N6 C26 -169.44(18) . . . . no N2 Fe1 N6 C30 11.0(2) . . . . no N4 Fe1 N6 C26 96.01(19) . . . . no N4 Fe1 N6 C30 -83.5(2) . . . . no N5 Fe1 N6 C26 5.06(18) . . . . no N5 Fe1 N6 C30 -174.5(2) . . . . no N3 Fe1 N4 C20 -178.4(2) . . . . no N3 Fe1 N4 C16 -0.07(17) . . . . no N11 Fe2 N7 C35 -170.47(18) . . . . no N11 Fe2 N7 C31 10.8(2) . . . . no N7 Fe2 N8 C36 -6.85(17) . . . . no N7 Fe2 N8 C40 179.9(2) . . . . no N9 Fe2 N8 C36 -100.95(18) . . . . no N9 Fe2 N8 C40 85.9(2) . . . . no N10 Fe2 N8 C36 177.19(18) . . . . no N12 Fe2 N7 C31 92.3(2) . . . . no N12 Fe2 N7 C35 -88.96(19) . . . . no N11 Fe2 N12 C60 -178.7(2) . . . . no N12 Fe2 N8 C40 -89.8(2) . . . . no N7 Fe2 N9 C41 7.8(2) . . . . no N7 Fe2 N9 C45 -176.32(18) . . . . no N8 Fe2 N9 C41 89.2(2) . . . . no N8 Fe2 N9 C45 -94.88(18) . . . . no N10 Fe2 N9 C41 -177.9(2) . . . . no N10 Fe2 N9 C45 -1.98(18) . . . . no N11 Fe2 N9 C41 -87.5(2) . . . . no N11 Fe2 N9 C45 88.39(18) . . . . no N8 Fe2 N10 C46 93.39(18) . . . . no N8 Fe2 N10 C50 -83.8(2) . . . . no N9 Fe2 N10 C46 0.83(18) . . . . no N9 Fe2 N10 C50 -176.3(2) . . . . no N11 Fe2 N10 C46 -92.00(19) . . . . no N11 Fe2 N10 C50 90.9(2) . . . . no N8 Fe2 N7 C31 -174.9(2) . . . . no N8 Fe2 N7 C35 3.85(18) . . . . no N9 Fe2 N7 C31 -82.5(2) . . . . no N9 Fe2 N7 C35 96.20(19) . . . . no N9 Fe2 N11 C55 -174.16(18) . . . . no N10 Fe2 N11 C51 87.6(2) . . . . no N10 Fe2 N11 C55 -92.42(18) . . . . no N12 Fe2 N11 C51 -178.8(2) . . . . no N12 Fe2 N11 C55 1.15(18) . . . . no N7 Fe2 N12 C56 -97.09(19) . . . . no N7 Fe2 N12 C60 86.4(2) . . . . no N8 Fe2 N12 C56 -178.36(19) . . . . no N8 Fe2 N12 C60 5.1(2) . . . . no N10 Fe2 N12 C56 88.15(19) . . . . no N10 Fe2 N12 C60 -88.4(2) . . . . no N11 Fe2 N12 C56 -2.09(18) . . . . no N12 Fe2 N10 C46 -173.52(18) . . . . no N12 Fe2 N10 C50 9.4(2) . . . . no N7 Fe2 N11 C51 -88.9(2) . . . . no N7 Fe2 N11 C55 91.06(18) . . . . no N9 Fe2 N11 C51 5.9(2) . . . . no N12 Fe2 N8 C36 83.37(18) . . . . no N10 Fe2 N8 C40 4.0(2) . . . . no Nb1 O2 C61 O4 -179.3(2) . . . . no Nb1 O2 C61 C62 1.0(3) . . . . no Nb1 O3 C62 O5 177.7(2) . . . . no Nb1 O3 C62 C61 -2.1(3) . . . . no Nb1 O6 C63 O8 178.1(2) . . . . no Nb1 O6 C63 C64 -2.9(3) . . . . no Nb1 O7 C64 O9 167.6(2) . . . . no Nb1 O7 C64 C63 -10.8(3) . . . . no Nb1 O10 C65 C66 1.0(3) . . . . no Nb1 O10 C65 O12 -179.1(2) . . . . no Nb1 O11 C66 O13 172.5(2) . . . . no Nb1 O11 C66 C65 -7.0(3) . . . . no C1 N1 C5 C4 -0.9(4) . . . . no C1 N1 C5 C6 176.8(2) . . . . no C5 N1 C1 C2 -0.9(4) . . . . no Fe1 N1 C1 C2 177.3(2) . . . . no Fe1 N1 C5 C4 -179.3(2) . . . . no Fe1 N1 C5 C6 -1.6(3) . . . . no Fe1 N2 C6 C7 -172.10(19) . . . . no C6 N2 C10 C9 0.1(4) . . . . no Fe1 N2 C10 C9 171.2(2) . . . . no C10 N2 C6 C7 0.0(4) . . . . no Fe1 N2 C6 C5 7.6(3) . . . . no C10 N2 C6 C5 179.7(2) . . . . no Fe1 N3 C11 C12 173.6(2) . . . . no C11 N3 C15 C16 179.2(2) . . . . no Fe1 N3 C15 C14 -175.1(2) . . . . no C15 N3 C11 C12 -2.0(4) . . . . no C11 N3 C15 C14 1.0(4) . . . . no Fe1 N3 C15 C16 3.1(3) . . . . no Fe1 N4 C16 C15 1.7(3) . . . . no C16 N4 C20 C19 -2.0(4) . . . . no Fe1 N4 C16 C17 -178.2(2) . . . . no C20 N4 C16 C15 -179.8(2) . . . . no C20 N4 C16 C17 0.3(4) . . . . no Fe1 N4 C20 C19 176.3(2) . . . . no Fe1 N5 C21 C22 174.9(2) . . . . no C21 N5 C25 C26 -177.2(2) . . . . no Fe1 N5 C25 C24 -174.6(2) . . . . no C25 N5 C21 C22 -2.0(4) . . . . no C21 N5 C25 C24 2.7(4) . . . . no Fe1 N5 C25 C26 5.6(3) . . . . no C30 N6 C26 C27 -0.3(4) . . . . no Fe1 N6 C30 C29 177.4(2) . . . . no C30 N6 C26 C25 176.1(2) . . . . no Fe1 N6 C26 C25 -3.5(3) . . . . no Fe1 N6 C26 C27 -179.8(2) . . . . no C26 N6 C30 C29 -2.1(4) . . . . no C31 N7 C35 C34 0.6(4) . . . . no C35 N7 C31 C32 -2.2(4) . . . . no C31 N7 C35 C36 178.4(2) . . . . no Fe2 N7 C35 C36 -0.5(3) . . . . no Fe2 N7 C31 C32 176.6(2) . . . . no Fe2 N7 C35 C34 -178.2(2) . . . . no C36 N8 C40 C39 -2.0(4) . . . . no Fe2 N8 C36 C37 -171.6(2) . . . . no C40 N8 C36 C37 2.3(4) . . . . no Fe2 N8 C36 C35 8.4(3) . . . . no C40 N8 C36 C35 -177.7(2) . . . . no Fe2 N8 C40 C39 171.0(2) . . . . no Fe2 N9 C45 C44 -175.9(2) . . . . no Fe2 N9 C41 C42 173.8(2) . . . . no C41 N9 C45 C46 179.0(2) . . . . no Fe2 N9 C45 C46 2.7(3) . . . . no C41 N9 C45 C44 0.4(4) . . . . no C45 N9 C41 C42 -2.0(4) . . . . no C50 N10 C46 C47 -0.2(4) . . . . no Fe2 N10 C50 C49 176.2(2) . . . . no C50 N10 C46 C45 177.8(2) . . . . no Fe2 N10 C46 C45 0.4(3) . . . . no C46 N10 C50 C49 -0.8(4) . . . . no Fe2 N10 C46 C47 -177.6(2) . . . . no Fe2 N11 C55 C54 -179.9(2) . . . . no C51 N11 C55 C56 179.9(2) . . . . no Fe2 N11 C55 C56 -0.1(3) . . . . no C51 N11 C55 C54 0.0(4) . . . . no C55 N11 C51 C52 -0.8(4) . . . . no Fe2 N11 C51 C52 179.1(2) . . . . no C60 N12 C56 C57 1.6(4) . . . . no C56 N12 C60 C59 -2.2(4) . . . . no Fe2 N12 C56 C55 2.6(3) . . . . no C60 N12 C56 C55 179.5(2) . . . . no Fe2 N12 C60 C59 174.3(2) . . . . no Fe2 N12 C56 C57 -175.3(2) . . . . no N1 C1 C2 C3 1.7(4) . . . . no C1 C2 C3 C4 -0.7(4) . . . . no C2 C3 C4 C5 -1.0(4) . . . . no C3 C4 C5 C6 -175.6(3) . . . . no C3 C4 C5 N1 1.8(4) . . . . no N1 C5 C6 N2 -3.9(3) . . . . no C4 C5 C6 C7 -6.6(4) . . . . no C4 C5 C6 N2 173.7(2) . . . . no N1 C5 C6 C7 175.7(2) . . . . no N2 C6 C7 C8 0.5(4) . . . . no C5 C6 C7 C8 -179.1(2) . . . . no C6 C7 C8 C9 -1.2(4) . . . . no C7 C8 C9 C10 1.4(4) . . . . no C8 C9 C10 N2 -0.8(4) . . . . no N3 C11 C12 C13 0.4(4) . . . . no C11 C12 C13 C14 2.0(4) . . . . no C12 C13 C14 C15 -2.9(4) . . . . no C13 C14 C15 C16 -176.6(2) . . . . no C13 C14 C15 N3 1.4(4) . . . . no C14 C15 C16 C17 -5.1(4) . . . . no N3 C15 C16 C17 176.8(2) . . . . no N3 C15 C16 N4 -3.2(3) . . . . no C14 C15 C16 N4 175.0(2) . . . . no C15 C16 C17 C18 -179.3(3) . . . . no N4 C16 C17 C18 0.7(4) . . . . no C16 C17 C18 C19 0.0(4) . . . . no C17 C18 C19 C20 -1.6(4) . . . . no C18 C19 C20 N4 2.6(4) . . . . no N5 C21 C22 C23 0.4(4) . . . . no C21 C22 C23 C24 0.6(4) . . . . no C22 C23 C24 C25 0.0(4) . . . . no C23 C24 C25 C26 178.1(3) . . . . no C23 C24 C25 N5 -1.7(4) . . . . no N5 C25 C26 C27 174.8(3) . . . . no C24 C25 C26 N6 178.8(3) . . . . no C24 C25 C26 C27 -5.0(4) . . . . no N5 C25 C26 N6 -1.4(3) . . . . no C25 C26 C27 C28 -174.1(3) . . . . no N6 C26 C27 C28 1.9(4) . . . . no C26 C27 C28 C29 -1.2(4) . . . . no C27 C28 C29 C30 -1.0(4) . . . . no C28 C29 C30 N6 2.8(4) . . . . no N7 C31 C32 C33 2.2(4) . . . . no C31 C32 C33 C34 -0.6(4) . . . . no C32 C33 C34 C35 -0.9(4) . . . . no C33 C34 C35 C36 -176.7(3) . . . . no C33 C34 C35 N7 0.9(4) . . . . no C34 C35 C36 C37 -7.5(4) . . . . no N7 C35 C36 N8 -5.2(3) . . . . no N7 C35 C36 C37 174.8(2) . . . . no C34 C35 C36 N8 172.5(2) . . . . no N8 C36 C37 C38 -0.3(4) . . . . no C35 C36 C37 C38 179.7(3) . . . . no C36 C37 C38 C39 -2.1(4) . . . . no C37 C38 C39 C40 2.3(4) . . . . no C38 C39 C40 N8 -0.3(4) . . . . no N9 C41 C42 C43 2.1(4) . . . . no C41 C42 C43 C44 -0.6(4) . . . . no C42 C43 C44 C45 -0.9(4) . . . . no C43 C44 C45 C46 -177.5(3) . . . . no C43 C44 C45 N9 1.0(4) . . . . no N9 C45 C46 C47 175.9(3) . . . . no C44 C45 C46 C47 -5.6(4) . . . . no N9 C45 C46 N10 -2.0(3) . . . . no C44 C45 C46 N10 176.6(2) . . . . no N10 C46 C47 C48 1.0(4) . . . . no C45 C46 C47 C48 -176.8(3) . . . . no C46 C47 C48 C49 -0.8(5) . . . . no C47 C48 C49 C50 -0.2(5) . . . . no C48 C49 C50 N10 1.0(4) . . . . no N11 C51 C52 C53 1.3(4) . . . . no C51 C52 C53 C54 -1.0(4) . . . . no C52 C53 C54 C55 0.3(4) . . . . no C53 C54 C55 C56 -179.6(3) . . . . no C53 C54 C55 N11 0.2(4) . . . . no C54 C55 C56 C57 -4.0(4) . . . . no C54 C55 C56 N12 178.2(3) . . . . no N11 C55 C56 N12 -1.7(3) . . . . no N11 C55 C56 C57 176.2(2) . . . . no N12 C56 C57 C58 -0.8(4) . . . . no C55 C56 C57 C58 -178.5(3) . . . . no C56 C57 C58 C59 0.4(4) . . . . no C57 C58 C59 C60 -0.9(4) . . . . no C58 C59 C60 N12 1.8(4) . . . . no O2 C61 C62 O5 -179.1(2) . . . . no O4 C61 C62 O3 -179.0(2) . . . . no O4 C61 C62 O5 1.2(4) . . . . no O2 C61 C62 O3 0.8(3) . . . . no O8 C63 C64 O7 -172.5(3) . . . . no O6 C63 C64 O9 -170.0(3) . . . . no O8 C63 C64 O9 9.1(5) . . . . no O6 C63 C64 O7 8.4(3) . . . . no O10 C65 C66 O11 4.1(3) . . . . no O12 C65 C66 O13 4.7(4) . . . . no O10 C65 C66 O13 -175.3(2) . . . . no O12 C65 C66 O11 -175.8(2) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O14 H141 O1 0.83(2) 2.07(2) 2.876(3) 163(3) . no O14 H142 O15 0.83(3) 1.97(3) 2.774(4) 165(3) . no O15 H151 O17 0.83(2) 1.98(2) 2.797(4) 169(2) 4_745 no O15 H152 O16 0.83(2) 1.96(2) 2.743(4) 157(4) . no O16 H161 O10 0.84(4) 2.58(3) 3.326(4) 150(3) . no O16 H161 O12 0.84(4) 2.29(4) 2.901(4) 131(4) . no O16 H162 Cl1 0.83(3) 2.44(3) 3.116(3) 139(4) 1_655 no O17 H171 O11 0.83(2) 2.12(2) 2.941(3) 168(3) . no O17 H172 O18 0.83(2) 2.02(3) 2.800(4) 157(3) . no O18 H181 O9 0.84(2) 2.186(19) 2.984(3) 159(2) . no O18 H182 O20 0.84(2) 1.89(2) 2.726(3) 174(2) 4_655 no O19 H191 O9 0.828(17) 2.000(17) 2.826(3) 176(3) . no O19 H192 Cl1 0.83(3) 2.41(2) 3.208(3) 162(3) . no O20 H201 Cl1 0.84(3) 2.38(3) 3.179(3) 162(3) . no O20 H202 O21 0.83(2) 1.907(18) 2.730(4) 171(3) . no O21 H211 O22 0.84(3) 1.99(3) 2.694(5) 141(3) . no O21 H212 O24 0.824(19) 2.163(16) 2.895(5) 148.2(17) . no O22 H221 O19 0.83(4) 2.31(4) 2.784(4) 117(3) 4_645 no O22 H222 O23 0.833(14) 1.901(16) 2.704(3) 161(4) . no O23 H231 O14 0.84(2) 1.96(2) 2.798(4) 171(3) . no O23 H232 O13 0.83(3) 2.11(3) 2.844(3) 148(2) 4_745 no O24 H241 Cl1 0.88(3) 2.54(3) 3.244(3) 138(3) . no O24 H242 O25 0.85(4) 2.10(3) 2.844(4) 146(4) . no O25 H251 O5 0.830(12) 1.957(14) 2.781(3) 172(3) 2_665 no O25 H252 O8 0.83(3) 2.03(2) 2.815(3) 157(3) . no C1 H1 N5 0.9300 2.5500 3.059(3) 114.00 . no C4 H4 O5 0.9300 2.4900 3.407(3) 168.00 1_455 no C9 H9 O12 0.9300 2.5800 3.308(4) 136.00 2_664 no C10 H10 N4 0.9300 2.5600 3.070(3) 115.00 . no C11 H11 N1 0.9300 2.5600 3.076(3) 115.00 . no C12 H12 Cl1 0.9300 2.8000 3.558(3) 139.00 . no C20 H20 N6 0.9300 2.5500 3.069(3) 115.00 . no C21 H21 N3 0.9300 2.5600 3.061(4) 114.00 . no C30 H30 N2 0.9300 2.5100 3.016(3) 114.00 . no C31 H31 N11 0.9300 2.5800 3.089(3) 115.00 . no C37 H37 O4 0.9300 2.5900 3.489(4) 164.00 . no C38 H38 O6 0.9300 2.4200 3.274(4) 152.00 2_664 no C39 H39 O12 0.9300 2.5500 3.469(4) 170.00 2_664 no C40 H40 N10 0.9300 2.5300 3.032(4) 114.00 . no C41 H41 N7 0.9300 2.5700 3.078(3) 115.00 . no C42 H42 Cl1 0.9300 2.8100 3.702(3) 160.00 . no C44 H44 O5 0.9300 2.4100 3.312(3) 163.00 1_455 no C50 H50 N12 0.9300 2.5300 3.041(4) 115.00 . no C51 H51 N9 0.9300 2.5400 3.043(4) 114.00 . no C59 H59 O13 0.9300 2.5900 3.184(4) 122.00 3_465 no C60 H60 N8 0.9300 2.5100 3.026(3) 115.00 . no #=============================================================================== data_II _database_code_depnum_ccdc_archive 'CCDC 648553' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C30 H24 Co N6), C6 Nb O13, Cl0.34 0.66(H2 O), Cl0.42 0.58(H2 O), Cl0.24 0.76(H2 O), 0.5(H2 O), 0.5(H2 O), 0.4(H2 O), 0.6(H2 O), 7(H2 O) ; _chemical_formula_structural ; 2(C30 H24 Co N6), C6 Nb O13, Cl0.34 0.66(H2 O), Cl0.42 0.58(H2 O), Cl0.24 0.76(H2 O), 0.5(H2 O), 0.5(H2 O), 0.4(H2 O), 0.6(H2 O), 7(H2 O) ; _chemical_formula_sum 'C66 H70 Cl Co2 N12 Nb O24' _chemical_formula_iupac ? _chemical_formula_weight 1661.56 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 23.548(3) _cell_length_b 13.6310(10) _cell_length_c 22.812(2) _cell_angle_alpha 90 _cell_angle_beta 101.040(10) _cell_angle_gamma 90 _cell_volume 7186.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 34461 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 28.31 _cell_special_details ; ? ; _exptl_crystal_description needle _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3416.0 _exptl_absorpt_coefficient_mu 0.753 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.96 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(3) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius-Kappa CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 34461 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 28.31 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 17763 # number of observed reflections (> n sig(I)) _reflns_number_gt 12012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software (Nonius, 1998)' _computing_cell_refinement 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0505P)^2^+9.2572P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 17763 _refine_ls_number_parameters 976 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.304 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.073 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Co1 Co Uani 0.08457(2) 0.33339(3) 0.26166(2) 1.000 0.0308(1) . . N1 N Uani 0.08505(11) 0.2008(2) 0.21337(11) 1.000 0.0346(8) . . N2 N Uani 0.15497(11) 0.2548(2) 0.31320(11) 1.000 0.0350(8) . . N3 N Uani 0.14012(11) 0.4096(2) 0.21351(12) 1.000 0.0379(9) . . N4 N Uani 0.10057(11) 0.4677(2) 0.30868(12) 1.000 0.0356(8) . . N5 N Uani 0.00495(11) 0.38545(19) 0.21066(11) 1.000 0.0312(8) . . N6 N Uani 0.02197(11) 0.27670(19) 0.30858(11) 1.000 0.0314(8) . . C1 C Uani 0.04997(15) 0.1796(3) 0.16086(15) 1.000 0.0435(11) . . C2 C Uani 0.05361(16) 0.0932(3) 0.13089(16) 1.000 0.0464(11) . . C3 C Uani 0.09354(17) 0.0247(3) 0.15584(17) 1.000 0.0493(12) . . C4 C Uani 0.12942(16) 0.0442(3) 0.20962(17) 1.000 0.0448(11) . . C5 C Uani 0.12497(13) 0.1337(2) 0.23742(14) 1.000 0.0336(10) . . C6 C Uani 0.16315(13) 0.1631(3) 0.29360(14) 1.000 0.0348(10) . . C7 C Uani 0.20576(15) 0.1025(3) 0.32519(16) 1.000 0.0474(11) . . C8 C Uani 0.24012(16) 0.1361(3) 0.37692(18) 1.000 0.0548(14) . . C9 C Uani 0.23141(15) 0.2291(3) 0.39680(17) 1.000 0.0517(13) . . C10 C Uani 0.18887(14) 0.2860(3) 0.36376(15) 1.000 0.0429(11) . . C11 C Uani 0.15841(16) 0.3766(3) 0.16516(16) 1.000 0.0502(12) . . C12 C Uani 0.19080(17) 0.4334(4) 0.13341(18) 1.000 0.0596(14) . . C13 C Uani 0.20458(17) 0.5267(4) 0.1516(2) 1.000 0.0619(16) . . C14 C Uani 0.18729(15) 0.5616(3) 0.20250(18) 1.000 0.0523(11) . . C15 C Uani 0.15560(13) 0.5007(3) 0.23301(15) 1.000 0.0398(11) . . C16 C Uani 0.13565(13) 0.5318(2) 0.28791(15) 1.000 0.0376(10) . . C17 C Uani 0.15226(16) 0.6195(3) 0.31782(18) 1.000 0.0503(12) . . C18 C Uani 0.13210(18) 0.6410(3) 0.36890(18) 1.000 0.0567(14) . . C19 C Uani 0.09573(16) 0.5770(3) 0.38945(17) 1.000 0.0488(12) . . C20 C Uani 0.08075(14) 0.4917(3) 0.35806(15) 1.000 0.0408(11) . . C21 C Uani -0.00097(14) 0.4392(2) 0.16097(15) 1.000 0.0385(10) . . C22 C Uani -0.05396(15) 0.4613(3) 0.12586(15) 1.000 0.0412(11) . . C23 C Uani -0.10332(14) 0.4280(3) 0.14323(15) 1.000 0.0396(10) . . C24 C Uani -0.09796(13) 0.3739(3) 0.19514(14) 1.000 0.0370(10) . . C25 C Uani -0.04339(13) 0.3537(2) 0.22840(13) 1.000 0.0310(9) . . C26 C Uani -0.03387(13) 0.2962(2) 0.28420(13) 1.000 0.0315(9) . . C27 C Uani -0.07884(15) 0.2648(3) 0.31106(15) 1.000 0.0399(11) . . C28 C Uani -0.06603(16) 0.2110(3) 0.36362(15) 1.000 0.0440(11) . . C29 C Uani -0.01001(16) 0.1904(3) 0.38772(14) 1.000 0.0412(11) . . C30 C Uani 0.03282(15) 0.2239(2) 0.35917(14) 1.000 0.0381(10) . . Co2 Co Uani 0.41803(2) 0.24516(3) 0.22326(2) 1.000 0.0304(1) . . N7 N Uani 0.40782(11) 0.3741(2) 0.16975(12) 1.000 0.0337(8) . . N8 N Uani 0.37829(11) 0.3441(2) 0.27470(12) 1.000 0.0366(9) . . N9 N Uani 0.33674(11) 0.1849(2) 0.18563(12) 1.000 0.0353(8) . . N10 N Uani 0.41121(11) 0.1236(2) 0.28053(12) 1.000 0.0377(8) . . N11 N Uani 0.46388(11) 0.16720(19) 0.16650(11) 1.000 0.0328(8) . . N12 N Uani 0.50451(11) 0.28010(19) 0.26005(11) 1.000 0.0329(8) . . C31 C Uani 0.42600(15) 0.3865(3) 0.11781(15) 1.000 0.0424(11) . . C32 C Uani 0.41522(17) 0.4694(3) 0.08410(18) 1.000 0.0543(12) . . C33 C Uani 0.38449(19) 0.5436(3) 0.1039(2) 1.000 0.0628(16) . . C34 C Uani 0.36556(17) 0.5327(3) 0.15726(19) 1.000 0.0535(14) . . C35 C Uani 0.37767(13) 0.4467(2) 0.18944(15) 1.000 0.0362(10) . . C36 C Uani 0.35939(13) 0.4287(2) 0.24684(15) 1.000 0.0367(10) . . C37 C Uani 0.32512(15) 0.4935(3) 0.27204(17) 1.000 0.0462(11) . . C38 C Uani 0.31130(16) 0.4713(3) 0.32683(18) 1.000 0.0543(14) . . C39 C Uani 0.33201(16) 0.3882(3) 0.35539(17) 1.000 0.0510(14) . . C40 C Uani 0.36544(15) 0.3256(3) 0.32837(15) 1.000 0.0464(11) . . C41 C Uani 0.30222(14) 0.2175(3) 0.13568(15) 1.000 0.0428(11) . . C42 C Uani 0.25282(15) 0.1679(3) 0.10869(16) 1.000 0.0496(13) . . C43 C Uani 0.23906(16) 0.0814(3) 0.13396(17) 1.000 0.0545(14) . . C44 C Uani 0.27346(15) 0.0485(3) 0.18577(17) 1.000 0.0479(11) . . C45 C Uani 0.32200(13) 0.1019(2) 0.21100(15) 1.000 0.0356(10) . . C46 C Uani 0.36135(13) 0.0734(2) 0.26739(15) 1.000 0.0354(10) . . C47 C Uani 0.34742(16) 0.0009(3) 0.30553(17) 1.000 0.0463(11) . . C48 C Uani 0.38543(17) -0.0189(3) 0.35848(18) 1.000 0.0541(12) . . C49 C Uani 0.43624(17) 0.0328(3) 0.37181(18) 1.000 0.0550(14) . . C50 C Uani 0.44833(16) 0.1024(3) 0.33164(17) 1.000 0.0493(11) . . C51 C Uani 0.44104(15) 0.1111(2) 0.11976(15) 1.000 0.0402(11) . . C52 C Uani 0.47417(16) 0.0622(3) 0.08531(16) 1.000 0.0462(11) . . C53 C Uani 0.53350(16) 0.0711(3) 0.09998(16) 1.000 0.0474(12) . . C54 C Uani 0.55743(15) 0.1292(3) 0.14752(15) 1.000 0.0425(11) . . C55 C Uani 0.52202(13) 0.1771(2) 0.18009(14) 1.000 0.0333(9) . . C56 C Uani 0.54436(13) 0.2427(2) 0.23115(13) 1.000 0.0330(9) . . C57 C Uani 0.60278(14) 0.2649(3) 0.24882(15) 1.000 0.0415(11) . . C58 C Uani 0.61976(15) 0.3264(3) 0.29678(16) 1.000 0.0484(11) . . C59 C Uani 0.57939(15) 0.3638(3) 0.32649(16) 1.000 0.0446(11) . . C60 C Uani 0.52261(15) 0.3398(3) 0.30694(15) 1.000 0.0402(11) . . Nb1 Nb Uani 0.34305(1) 0.69679(2) 0.50261(1) 1.000 0.0334(1) . . O1 O Uani 0.33307(10) 0.73852(18) 0.57098(10) 1.000 0.0426(8) . . O2 O Uani 0.42996(9) 0.65696(17) 0.53207(11) 1.000 0.0429(8) . . O3 O Uani 0.39501(10) 0.81136(17) 0.47877(10) 1.000 0.0425(8) . . O4 O Uani 0.52259(11) 0.7022(2) 0.55108(13) 1.000 0.0604(10) . . O5 O Uani 0.48426(12) 0.8692(2) 0.48016(14) 1.000 0.0661(11) . . O6 O Uani 0.25596(10) 0.63786(19) 0.48912(11) 1.000 0.0469(8) . . O7 O Uani 0.34999(10) 0.54383(17) 0.51173(11) 1.000 0.0429(8) . . O8 O Uani 0.20126(12) 0.5041(2) 0.48744(15) 1.000 0.0767(11) . . O9 O Uani 0.30623(13) 0.3984(2) 0.49772(12) 1.000 0.0579(10) . . O10 O Uani 0.28659(10) 0.80676(18) 0.45853(10) 1.000 0.0427(8) . . O11 O Uani 0.32985(9) 0.66421(17) 0.40645(10) 1.000 0.0388(7) . . O12 O Uani 0.24296(12) 0.8705(2) 0.37147(12) 1.000 0.0597(10) . . O13 O Uani 0.28818(10) 0.71594(19) 0.31574(10) 1.000 0.0469(8) . . C61 C Uani 0.47213(14) 0.7159(3) 0.52879(15) 1.000 0.0406(11) . . C62 C Uani 0.45100(16) 0.8086(3) 0.49279(15) 1.000 0.0426(11) . . C63 C Uani 0.24828(15) 0.5456(3) 0.49105(16) 1.000 0.0488(13) . . C64 C Uani 0.30497(15) 0.4875(3) 0.50045(14) 1.000 0.0418(11) . . C65 C Uani 0.27300(14) 0.8089(3) 0.40130(15) 1.000 0.0390(10) . . C66 C Uani 0.29856(13) 0.7229(3) 0.37042(15) 1.000 0.0369(10) . . O19 O Uani -0.00025(9) 0.40481(13) 0.46913(7) 0.659(7) 0.0627(7) . . Cl2 Cl Uani -0.00025(9) 0.40481(13) 0.46913(7) 0.341(7) 0.0627(7) . . O20 O Uani 0.04716(8) 0.0697(2) 0.53366(8) 0.580(8) 0.0970(12) . . Cl3 Cl Uani 0.04716(8) 0.0697(2) 0.53366(8) 0.420(8) 0.0970(12) . . O25 O Uani 0.03986(13) 0.7586(2) 0.46793(12) 0.761(8) 0.0960(11) . . Cl1 Cl Uani 0.03986(13) 0.7586(2) 0.46793(12) 0.239(8) 0.0960(11) . . O162 O Uani 0.2122(3) -0.0286(5) 0.4926(3) 0.600 0.083(3) . . O161 O Uani 0.2397(4) -0.0669(7) 0.5255(4) 0.400 0.076(4) . . O211 O Uani 0.1284(3) 0.8717(10) 0.5200(4) 0.500 0.144(5) . . O212 O Uani 0.1640(5) 0.7926(10) 0.5148(5) 0.500 0.145(6) . . O14 O Uani 0.37312(13) 0.2257(2) 0.48771(17) 1.000 0.0801(13) . . O15 O Uani 0.27898(17) 0.1268(3) 0.53195(17) 1.000 0.0942(16) . . O17 O Uani 0.13727(19) 0.1390(3) 0.47672(17) 1.000 0.1089(18) . . O18 O Uani 0.13122(16) 0.3396(3) 0.49167(19) 1.000 0.0991(17) . . O22 O Uani 0.14326(17) 0.6330(4) 0.55397(19) 1.000 0.1122(19) . . O23 O Uani 0.21817(10) 0.84651(19) 0.23605(11) 1.000 0.0479(8) . . O24 O Uani 0.23688(14) 0.7680(3) 0.12964(13) 1.000 0.0779(13) . . H1 H Uiso 0.02220 0.22540 0.14430 1.000 0.0520 calc R H2 H Uiso 0.02940 0.08150 0.09430 1.000 0.0560 calc R H3 H Uiso 0.09640 -0.03470 0.13650 1.000 0.0590 calc R H4 H Uiso 0.15640 -0.00210 0.22720 1.000 0.0540 calc R H7 H Uiso 0.21100 0.03950 0.31140 1.000 0.0570 calc R H8 H Uiso 0.26890 0.09630 0.39820 1.000 0.0660 calc R H9 H Uiso 0.25390 0.25290 0.43190 1.000 0.0620 calc R H10 H Uiso 0.18330 0.34920 0.37710 1.000 0.0520 calc R H11 H Uiso 0.14900 0.31290 0.15230 1.000 0.0600 calc R H12 H Uiso 0.20300 0.40800 0.10000 1.000 0.0710 calc R H13 H Uiso 0.22540 0.56660 0.13030 1.000 0.0740 calc R H14 H Uiso 0.19680 0.62500 0.21600 1.000 0.0630 calc R H17 H Uiso 0.17670 0.66290 0.30330 1.000 0.0600 calc R H18 H Uiso 0.14310 0.69900 0.38950 1.000 0.0680 calc R H19 H Uiso 0.08150 0.59070 0.42390 1.000 0.0590 calc R H20 H Uiso 0.05560 0.44860 0.37180 1.000 0.0490 calc R H21 H Uiso 0.03220 0.46290 0.14940 1.000 0.0460 calc R H22 H Uiso -0.05620 0.49800 0.09110 1.000 0.0500 calc R H23 H Uiso -0.13960 0.44160 0.12040 1.000 0.0480 calc R H24 H Uiso -0.13080 0.35100 0.20780 1.000 0.0440 calc R H27 H Uiso -0.11700 0.27970 0.29410 1.000 0.0480 calc R H28 H Uiso -0.09560 0.18930 0.38220 1.000 0.0530 calc R H29 H Uiso -0.00070 0.15430 0.42290 1.000 0.0490 calc R H30 H Uiso 0.07110 0.20920 0.37580 1.000 0.0460 calc R H31 H Uiso 0.44690 0.33630 0.10430 1.000 0.0510 calc R H32 H Uiso 0.42850 0.47550 0.04840 1.000 0.0650 calc R H33 H Uiso 0.37640 0.60080 0.08160 1.000 0.0750 calc R H34 H Uiso 0.34490 0.58270 0.17140 1.000 0.0640 calc R H37 H Uiso 0.31170 0.55100 0.25230 1.000 0.0560 calc R H38 H Uiso 0.28790 0.51340 0.34390 1.000 0.0650 calc R H39 H Uiso 0.32390 0.37320 0.39270 1.000 0.0620 calc R H40 H Uiso 0.37960 0.26850 0.34820 1.000 0.0560 calc R H41 H Uiso 0.31190 0.27560 0.11860 1.000 0.0510 calc R H42 H Uiso 0.22940 0.19240 0.07430 1.000 0.0590 calc R H43 H Uiso 0.20680 0.04550 0.11610 1.000 0.0660 calc R H44 H Uiso 0.26420 -0.00900 0.20370 1.000 0.0570 calc R H47 H Uiso 0.31290 -0.03380 0.29550 1.000 0.0550 calc R H48 H Uiso 0.37660 -0.06650 0.38460 1.000 0.0650 calc R H49 H Uiso 0.46220 0.02130 0.40730 1.000 0.0660 calc R H50 H Uiso 0.48340 0.13570 0.34030 1.000 0.0590 calc R H51 H Uiso 0.40100 0.10490 0.11000 1.000 0.0480 calc R H52 H Uiso 0.45690 0.02410 0.05300 1.000 0.0550 calc R H53 H Uiso 0.55700 0.03820 0.07800 1.000 0.0570 calc R H54 H Uiso 0.59740 0.13620 0.15780 1.000 0.0510 calc R H57 H Uiso 0.62990 0.23860 0.22850 1.000 0.0500 calc R H58 H Uiso 0.65860 0.34260 0.30900 1.000 0.0580 calc R H59 H Uiso 0.59040 0.40470 0.35930 1.000 0.0540 calc R H60 H Uiso 0.49520 0.36590 0.32690 1.000 0.0480 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0299(2) 0.0321(2) 0.0308(2) 0.0009(2) 0.0066(2) 0.0002(2) N1 0.0346(14) 0.0371(15) 0.0320(13) 0.0001(12) 0.0058(11) -0.0004(12) N2 0.0297(13) 0.0404(16) 0.0344(14) 0.0029(12) 0.0049(11) -0.0014(12) N3 0.0318(14) 0.0454(17) 0.0387(15) 0.0050(13) 0.0120(12) 0.0026(12) N4 0.0321(13) 0.0339(15) 0.0404(15) 0.0005(12) 0.0063(11) 0.0007(11) N5 0.0331(13) 0.0290(14) 0.0320(13) 0.0018(11) 0.0079(11) 0.0019(11) N6 0.0344(13) 0.0309(14) 0.0293(13) -0.0005(11) 0.0070(10) 0.0001(11) C1 0.0406(18) 0.050(2) 0.0379(18) -0.0049(16) 0.0023(14) 0.0014(16) C2 0.051(2) 0.046(2) 0.0421(19) -0.0128(17) 0.0089(16) -0.0083(17) C3 0.062(2) 0.037(2) 0.053(2) -0.0110(17) 0.0211(19) -0.0071(18) C4 0.049(2) 0.0348(19) 0.054(2) 0.0032(16) 0.0187(17) 0.0026(16) C5 0.0308(15) 0.0347(18) 0.0379(17) 0.0037(14) 0.0135(13) 0.0005(13) C6 0.0297(15) 0.0397(19) 0.0365(17) 0.0078(14) 0.0103(13) 0.0034(14) C7 0.0428(19) 0.051(2) 0.049(2) 0.0095(18) 0.0106(16) 0.0118(17) C8 0.0369(19) 0.073(3) 0.052(2) 0.017(2) 0.0023(17) 0.0113(19) C9 0.0349(18) 0.073(3) 0.043(2) 0.0116(19) -0.0027(15) -0.0086(18) C10 0.0380(18) 0.050(2) 0.0385(18) 0.0006(16) 0.0016(14) -0.0063(16) C11 0.051(2) 0.055(2) 0.049(2) 0.0044(18) 0.0204(17) 0.0016(18) C12 0.047(2) 0.087(3) 0.050(2) 0.015(2) 0.0225(18) 0.006(2) C13 0.043(2) 0.078(3) 0.067(3) 0.028(2) 0.0167(19) -0.004(2) C14 0.0393(19) 0.057(2) 0.061(2) 0.017(2) 0.0106(17) -0.0032(18) C15 0.0281(16) 0.042(2) 0.0479(19) 0.0116(16) 0.0039(14) 0.0006(14) C16 0.0280(15) 0.0358(18) 0.0467(19) 0.0057(15) 0.0014(14) 0.0008(14) C17 0.045(2) 0.040(2) 0.062(2) 0.0063(18) 0.0006(18) -0.0096(17) C18 0.064(3) 0.042(2) 0.057(2) -0.0101(19) -0.006(2) -0.0020(19) C19 0.048(2) 0.047(2) 0.049(2) -0.0109(18) 0.0031(17) 0.0046(18) C20 0.0372(17) 0.042(2) 0.0440(19) -0.0053(16) 0.0101(15) -0.0001(15) C21 0.0389(17) 0.0378(19) 0.0393(18) 0.0062(15) 0.0088(14) 0.0005(15) C22 0.048(2) 0.0380(19) 0.0373(18) 0.0062(15) 0.0074(15) 0.0066(16) C23 0.0367(17) 0.0401(19) 0.0391(18) 0.0007(15) 0.0001(14) 0.0078(15) C24 0.0299(16) 0.0398(19) 0.0418(18) -0.0006(15) 0.0079(13) 0.0002(14) C25 0.0337(16) 0.0294(17) 0.0304(15) -0.0027(13) 0.0075(12) -0.0006(13) C26 0.0343(16) 0.0289(16) 0.0320(15) -0.0039(13) 0.0079(12) -0.0014(13) C27 0.0362(17) 0.046(2) 0.0389(18) 0.0002(15) 0.0107(14) -0.0066(15) C28 0.052(2) 0.046(2) 0.0371(18) 0.0011(16) 0.0164(16) -0.0105(17) C29 0.057(2) 0.0385(19) 0.0301(16) 0.0015(14) 0.0133(15) -0.0027(16) C30 0.0441(18) 0.0386(19) 0.0318(16) 0.0006(14) 0.0078(14) -0.0001(15) Co2 0.0281(2) 0.0291(2) 0.0342(2) 0.0023(2) 0.0067(2) 0.0012(2) N7 0.0316(13) 0.0325(15) 0.0375(14) 0.0035(12) 0.0079(11) 0.0005(11) N8 0.0342(14) 0.0388(16) 0.0372(15) -0.0007(12) 0.0082(11) 0.0022(12) N9 0.0296(13) 0.0361(16) 0.0398(15) 0.0023(12) 0.0059(11) 0.0012(11) N10 0.0334(14) 0.0361(15) 0.0436(15) 0.0081(13) 0.0075(12) 0.0025(12) N11 0.0330(13) 0.0286(14) 0.0364(14) 0.0008(11) 0.0058(11) 0.0022(11) N12 0.0342(13) 0.0312(14) 0.0334(14) 0.0014(11) 0.0067(11) 0.0005(11) C31 0.0438(19) 0.043(2) 0.0430(19) 0.0074(16) 0.0146(15) 0.0005(16) C32 0.061(2) 0.052(2) 0.054(2) 0.0208(19) 0.0214(19) 0.004(2) C33 0.072(3) 0.043(2) 0.077(3) 0.031(2) 0.023(2) 0.012(2) C34 0.061(2) 0.033(2) 0.071(3) 0.0091(19) 0.024(2) 0.0088(18) C35 0.0307(16) 0.0304(17) 0.0470(19) 0.0006(14) 0.0061(14) 0.0019(13) C36 0.0290(16) 0.0372(19) 0.0430(18) -0.0055(15) 0.0050(13) -0.0003(14) C37 0.0412(19) 0.041(2) 0.056(2) -0.0117(17) 0.0080(16) 0.0030(16) C38 0.048(2) 0.058(3) 0.061(2) -0.024(2) 0.0210(18) -0.0004(19) C39 0.048(2) 0.066(3) 0.043(2) -0.0136(19) 0.0191(17) -0.006(2) C40 0.045(2) 0.056(2) 0.0394(19) 0.0000(17) 0.0111(15) 0.0007(17) C41 0.0364(17) 0.049(2) 0.0419(19) 0.0059(16) 0.0051(14) 0.0026(16) C42 0.0374(18) 0.069(3) 0.0409(19) -0.0034(19) 0.0039(15) 0.0011(18) C43 0.041(2) 0.077(3) 0.046(2) -0.011(2) 0.0096(17) -0.018(2) C44 0.0424(19) 0.053(2) 0.050(2) -0.0041(18) 0.0130(16) -0.0132(17) C45 0.0317(16) 0.0370(19) 0.0411(18) -0.0032(14) 0.0145(14) -0.0009(14) C46 0.0321(16) 0.0312(17) 0.0449(18) 0.0006(14) 0.0126(14) 0.0038(13) C47 0.0441(19) 0.042(2) 0.056(2) 0.0082(17) 0.0176(17) -0.0039(16) C48 0.058(2) 0.047(2) 0.061(2) 0.0215(19) 0.0209(19) 0.0033(19) C49 0.053(2) 0.056(3) 0.054(2) 0.021(2) 0.0056(18) 0.0086(19) C50 0.0407(19) 0.048(2) 0.056(2) 0.0173(18) 0.0014(16) 0.0024(17) C51 0.0420(18) 0.0358(19) 0.0428(19) -0.0044(15) 0.0083(15) -0.0024(15) C52 0.059(2) 0.038(2) 0.0425(19) -0.0079(16) 0.0123(17) -0.0040(17) C53 0.053(2) 0.045(2) 0.048(2) -0.0013(17) 0.0192(17) 0.0091(18) C54 0.0370(18) 0.048(2) 0.0445(19) -0.0011(17) 0.0125(15) 0.0043(16) C55 0.0364(16) 0.0299(17) 0.0344(16) 0.0054(13) 0.0086(13) 0.0024(13) C56 0.0334(16) 0.0329(17) 0.0329(16) 0.0070(13) 0.0067(13) 0.0012(13) C57 0.0310(16) 0.051(2) 0.0426(19) 0.0068(16) 0.0071(14) -0.0019(15) C58 0.0370(18) 0.059(2) 0.045(2) 0.0062(18) -0.0028(15) -0.0108(17) C59 0.046(2) 0.046(2) 0.0379(18) -0.0025(16) -0.0015(15) -0.0034(17) C60 0.0413(18) 0.043(2) 0.0363(17) -0.0043(15) 0.0072(14) 0.0003(15) Nb1 0.0330(2) 0.0330(2) 0.0336(2) 0.0025(1) 0.0049(1) -0.0013(1) O1 0.0443(13) 0.0460(14) 0.0380(12) 0.0014(11) 0.0094(10) -0.0024(11) O2 0.0344(12) 0.0376(13) 0.0553(15) 0.0095(11) 0.0052(10) -0.0038(10) O3 0.0434(13) 0.0368(13) 0.0463(13) 0.0088(11) 0.0061(10) -0.0059(11) O4 0.0373(14) 0.0659(19) 0.0734(19) 0.0159(15) -0.0011(13) -0.0079(13) O5 0.0551(17) 0.0587(18) 0.084(2) 0.0230(16) 0.0122(15) -0.0212(14) O6 0.0351(12) 0.0479(16) 0.0561(15) 0.0068(12) 0.0050(11) -0.0060(11) O7 0.0386(12) 0.0370(13) 0.0515(14) 0.0060(11) 0.0050(11) -0.0046(10) O8 0.0425(15) 0.077(2) 0.103(2) 0.0269(19) -0.0054(15) -0.0218(15) O9 0.0767(19) 0.0402(16) 0.0614(17) -0.0027(13) 0.0246(14) -0.0149(14) O10 0.0437(13) 0.0443(14) 0.0406(13) 0.0017(11) 0.0096(10) 0.0103(11) O11 0.0400(12) 0.0385(13) 0.0355(12) 0.0013(10) 0.0015(10) 0.0070(10) O12 0.0570(16) 0.0641(19) 0.0583(16) 0.0185(14) 0.0122(13) 0.0257(14) O13 0.0490(14) 0.0573(16) 0.0346(13) 0.0085(11) 0.0084(11) 0.0047(12) C61 0.0353(18) 0.047(2) 0.0391(18) -0.0007(16) 0.0064(14) -0.0055(15) C62 0.048(2) 0.041(2) 0.0386(18) 0.0002(15) 0.0081(15) -0.0061(17) C63 0.0392(19) 0.064(3) 0.0403(19) 0.0076(18) 0.0007(15) -0.0129(18) C64 0.052(2) 0.043(2) 0.0308(17) 0.0023(15) 0.0086(15) -0.0124(17) C65 0.0319(16) 0.0404(19) 0.0464(19) 0.0092(16) 0.0120(14) 0.0060(15) C66 0.0281(15) 0.0409(19) 0.0419(19) 0.0052(15) 0.0073(13) -0.0034(14) O19 0.0975(16) 0.0435(11) 0.0420(10) 0.0051(7) 0.0008(9) -0.0052(9) Cl2 0.0975(16) 0.0435(11) 0.0420(10) 0.0051(7) 0.0008(9) -0.0052(9) O20 0.0668(13) 0.173(3) 0.0518(12) 0.0159(13) 0.0127(9) -0.0304(14) Cl3 0.0668(13) 0.173(3) 0.0518(12) 0.0159(13) 0.0127(9) -0.0304(14) O25 0.123(2) 0.096(2) 0.0837(19) -0.0389(15) 0.0569(16) -0.0361(17) Cl1 0.123(2) 0.096(2) 0.0837(19) -0.0389(15) 0.0569(16) -0.0361(17) O162 0.067(4) 0.085(5) 0.099(5) -0.022(4) 0.023(3) 0.003(3) O161 0.073(6) 0.078(7) 0.089(7) -0.034(5) 0.047(5) -0.011(5) O211 0.047(4) 0.255(13) 0.123(7) 0.119(8) 0.000(4) -0.017(6) O212 0.109(8) 0.193(12) 0.139(9) -0.047(8) 0.041(7) -0.041(8) O14 0.0535(18) 0.072(2) 0.113(3) 0.021(2) 0.0116(17) -0.0093(16) O15 0.112(3) 0.091(3) 0.087(2) -0.003(2) 0.038(2) 0.002(2) O17 0.119(3) 0.136(4) 0.080(2) 0.028(2) 0.040(2) 0.054(3) O18 0.087(3) 0.090(3) 0.121(3) -0.012(2) 0.022(2) -0.037(2) O22 0.088(3) 0.140(4) 0.107(3) 0.001(3) 0.015(2) 0.010(3) O23 0.0426(13) 0.0503(15) 0.0495(14) 0.0071(12) 0.0054(11) 0.0041(12) O24 0.0678(19) 0.119(3) 0.0516(17) -0.0106(18) 0.0233(15) -0.0122(19) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O7 2.099(2) . . no Nb1 O10 2.125(2) . . no Nb1 O11 2.201(2) . . no Nb1 O3 2.118(2) . . no Nb1 O1 1.718(2) . . no Nb1 O2 2.100(2) . . no Nb1 O6 2.169(2) . . no Co1 N4 2.119(3) . . no Co1 N1 2.118(3) . . no Co1 N2 2.129(3) . . no Co1 N3 2.132(3) . . no Co1 N5 2.130(3) . . no Co1 N6 2.126(3) . . no Co2 N7 2.127(3) . . no Co2 N8 2.120(3) . . no Co2 N9 2.109(3) . . no Co2 N10 2.135(3) . . no Co2 N11 2.123(3) . . no Co2 N12 2.103(3) . . no O2 C61 1.291(4) . . no O3 C62 1.296(4) . . no O4 C61 1.214(4) . . no O5 C62 1.210(5) . . no O6 C63 1.273(5) . . no O7 C64 1.294(4) . . no O8 C63 1.232(5) . . no O9 C64 1.217(5) . . no O10 C65 1.284(4) . . no O11 C66 1.275(4) . . no O12 C65 1.218(5) . . no O13 C66 1.228(4) . . no N1 C1 1.350(4) . . no N1 C5 1.350(4) . . no N2 C6 1.354(5) . . no N2 C10 1.340(4) . . no N3 C11 1.337(5) . . no N3 C15 1.346(5) . . no N4 C16 1.349(4) . . no N4 C20 1.340(4) . . no N5 C21 1.334(4) . . no N5 C25 1.350(4) . . no N6 C26 1.352(4) . . no N6 C30 1.343(4) . . no N7 C31 1.345(4) . . no N7 C35 1.344(4) . . no N8 C36 1.350(4) . . no N8 C40 1.340(4) . . no N9 C41 1.342(4) . . no N9 C45 1.346(4) . . no N10 C50 1.348(5) . . no N10 C46 1.342(4) . . no N11 C51 1.338(4) . . no N11 C55 1.351(4) . . no N12 C60 1.347(4) . . no N12 C56 1.346(4) . . no O211 O212 1.385(17) . . no C1 C2 1.373(6) . . no C2 C3 1.369(6) . . no C3 C4 1.376(5) . . no C4 C5 1.388(5) . . no C5 C6 1.473(4) . . no C6 C7 1.390(5) . . no C7 C8 1.375(5) . . no C8 C9 1.375(6) . . no C9 C10 1.373(5) . . no C11 C12 1.385(6) . . no C12 C13 1.358(8) . . no C13 C14 1.386(6) . . no C14 C15 1.389(5) . . no C15 C16 1.481(5) . . no C16 C17 1.395(5) . . no C17 C18 1.372(6) . . no C18 C19 1.367(6) . . no C19 C20 1.376(6) . . no C21 C22 1.381(5) . . no C22 C23 1.375(5) . . no C23 C24 1.380(5) . . no C24 C25 1.389(4) . . no C25 C26 1.475(4) . . no C26 C27 1.389(5) . . no C27 C28 1.389(5) . . no C28 C29 1.358(5) . . no C29 C30 1.379(5) . . no C1 H1 0.9303 . . no C2 H2 0.9300 . . no C3 H3 0.9307 . . no C4 H4 0.9302 . . no C7 H7 0.9309 . . no C8 H8 0.9291 . . no C9 H9 0.9297 . . no C10 H10 0.9313 . . no C11 H11 0.9296 . . no C12 H12 0.9312 . . no C13 H13 0.9292 . . no C14 H14 0.9303 . . no C17 H17 0.9295 . . no C18 H18 0.9308 . . no C19 H19 0.9304 . . no C20 H20 0.9302 . . no C21 H21 0.9290 . . no C22 H22 0.9305 . . no C23 H23 0.9301 . . no C24 H24 0.9297 . . no C27 H27 0.9302 . . no C28 H28 0.9301 . . no C29 H29 0.9311 . . no C30 H30 0.9304 . . no C31 C32 1.363(6) . . no C32 C33 1.370(6) . . no C33 C34 1.382(6) . . no C34 C35 1.384(5) . . no C35 C36 1.475(5) . . no C36 C37 1.393(5) . . no C37 C38 1.384(6) . . no C38 C39 1.350(6) . . no C39 C40 1.383(5) . . no C41 C42 1.384(5) . . no C42 C43 1.378(6) . . no C43 C44 1.374(5) . . no C44 C45 1.384(5) . . no C45 C46 1.486(5) . . no C46 C47 1.397(5) . . no C47 C48 1.385(6) . . no C48 C49 1.372(6) . . no C49 C50 1.386(6) . . no C51 C52 1.380(5) . . no C52 C53 1.378(5) . . no C53 C54 1.374(5) . . no C54 C55 1.382(5) . . no C55 C56 1.483(4) . . no C56 C57 1.391(5) . . no C57 C58 1.376(5) . . no C58 C59 1.367(5) . . no C59 C60 1.366(5) . . no C31 H31 0.9293 . . no C32 H32 0.9303 . . no C33 H33 0.9305 . . no C34 H34 0.9302 . . no C37 H37 0.9287 . . no C38 H38 0.9310 . . no C39 H39 0.9300 . . no C40 H40 0.9294 . . no C41 H41 0.9300 . . no C42 H42 0.9303 . . no C43 H43 0.9295 . . no C44 H44 0.9291 . . no C47 H47 0.9304 . . no C48 H48 0.9310 . . no C49 H49 0.9296 . . no C50 H50 0.9298 . . no C51 H51 0.9302 . . no C52 H52 0.9293 . . no C53 H53 0.9301 . . no C54 H54 0.9303 . . no C57 H57 0.9298 . . no C58 H58 0.9302 . . no C59 H59 0.9295 . . no C60 H60 0.9290 . . no C61 C62 1.537(5) . . no C63 C64 1.532(5) . . no C65 C66 1.548(5) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O10 144.81(9) . . . no O2 Nb1 O11 102.11(9) . . . no O3 Nb1 O6 144.45(9) . . . no O3 Nb1 O7 136.07(9) . . . no O3 Nb1 O10 72.43(9) . . . no O3 Nb1 O11 82.60(9) . . . no O6 Nb1 O7 72.52(10) . . . no O6 Nb1 O10 72.85(9) . . . no O6 Nb1 O11 80.48(9) . . . no O7 Nb1 O10 141.05(9) . . . no O7 Nb1 O11 83.79(9) . . . no O10 Nb1 O11 73.41(9) . . . no O1 Nb1 O6 87.79(10) . . . no O1 Nb1 O7 105.10(11) . . . no O1 Nb1 O10 90.81(10) . . . no O1 Nb1 O11 162.51(10) . . . no O2 Nb1 O3 72.38(9) . . . no O2 Nb1 O6 141.90(9) . . . no O2 Nb1 O7 70.05(9) . . . no O1 Nb1 O3 100.09(10) . . . no O1 Nb1 O2 95.13(10) . . . no N1 Co1 N3 94.75(10) . . . no N1 Co1 N4 169.29(10) . . . no N1 Co1 N6 91.43(10) . . . no N2 Co1 N3 92.29(10) . . . no N1 Co1 N5 95.28(10) . . . no N1 Co1 N2 77.10(10) . . . no N4 Co1 N5 92.36(10) . . . no N4 Co1 N6 97.61(10) . . . no N5 Co1 N6 76.90(10) . . . no N3 Co1 N6 171.60(10) . . . no N2 Co1 N5 168.59(10) . . . no N2 Co1 N6 94.63(10) . . . no N2 Co1 N4 96.38(10) . . . no N3 Co1 N5 96.83(10) . . . no N3 Co1 N4 76.86(10) . . . no N7 Co2 N8 77.21(10) . . . no N11 Co2 N12 77.88(10) . . . no N8 Co2 N10 93.56(10) . . . no N8 Co2 N11 170.48(10) . . . no N7 Co2 N9 95.41(10) . . . no N7 Co2 N10 168.22(10) . . . no N7 Co2 N11 94.50(10) . . . no N7 Co2 N12 92.08(10) . . . no N8 Co2 N9 90.61(10) . . . no N10 Co2 N12 96.44(10) . . . no N9 Co2 N10 77.17(10) . . . no N9 Co2 N11 94.87(10) . . . no N8 Co2 N12 97.55(10) . . . no N10 Co2 N11 95.24(10) . . . no N9 Co2 N12 169.98(10) . . . no Nb1 O2 C61 122.3(2) . . . no Nb1 O3 C62 121.7(2) . . . no Nb1 O6 C63 119.9(2) . . . no Nb1 O7 C64 121.6(2) . . . no Nb1 O10 C65 120.6(2) . . . no Nb1 O11 C66 118.0(2) . . . no Co1 N1 C1 125.5(2) . . . no Co1 N1 C5 116.1(2) . . . no C1 N1 C5 118.4(3) . . . no Co1 N2 C6 115.3(2) . . . no C6 N2 C10 118.6(3) . . . no Co1 N2 C10 126.0(2) . . . no C11 N3 C15 118.3(3) . . . no Co1 N3 C15 115.7(2) . . . no Co1 N3 C11 126.0(2) . . . no Co1 N4 C16 116.3(2) . . . no Co1 N4 C20 125.4(2) . . . no C16 N4 C20 118.2(3) . . . no Co1 N5 C25 115.72(19) . . . no Co1 N5 C21 125.8(2) . . . no C21 N5 C25 118.3(3) . . . no Co1 N6 C26 115.78(19) . . . no C26 N6 C30 118.0(3) . . . no Co1 N6 C30 126.3(2) . . . no C31 N7 C35 118.6(3) . . . no Co2 N7 C31 126.1(2) . . . no Co2 N7 C35 115.2(2) . . . no Co2 N8 C40 125.9(2) . . . no C36 N8 C40 118.6(3) . . . no Co2 N8 C36 115.1(2) . . . no Co2 N9 C41 124.9(2) . . . no C41 N9 C45 118.6(3) . . . no Co2 N9 C45 116.2(2) . . . no C46 N10 C50 118.6(3) . . . no Co2 N10 C50 125.7(2) . . . no Co2 N10 C46 115.1(2) . . . no Co2 N11 C55 114.9(2) . . . no Co2 N11 C51 126.7(2) . . . no C51 N11 C55 118.3(3) . . . no Co2 N12 C56 115.6(2) . . . no C56 N12 C60 118.3(3) . . . no Co2 N12 C60 126.1(2) . . . no N1 C1 C2 122.7(3) . . . no C1 C2 C3 118.8(3) . . . no C2 C3 C4 119.6(4) . . . no C3 C4 C5 119.3(4) . . . no C4 C5 C6 123.3(3) . . . no N1 C5 C6 115.5(3) . . . no N1 C5 C4 121.2(3) . . . no N2 C6 C7 120.8(3) . . . no C5 C6 C7 123.3(3) . . . no N2 C6 C5 115.9(3) . . . no C6 C7 C8 119.7(4) . . . no C7 C8 C9 119.3(4) . . . no C8 C9 C10 118.6(4) . . . no N2 C10 C9 123.0(4) . . . no N3 C11 C12 122.7(4) . . . no C11 C12 C13 119.2(4) . . . no C12 C13 C14 119.1(4) . . . no C13 C14 C15 119.1(4) . . . no C14 C15 C16 122.7(3) . . . no N3 C15 C16 115.7(3) . . . no N3 C15 C14 121.6(3) . . . no N4 C16 C17 121.1(3) . . . no N4 C16 C15 115.2(3) . . . no C15 C16 C17 123.7(3) . . . no C16 C17 C18 119.2(4) . . . no C17 C18 C19 119.8(4) . . . no C18 C19 C20 118.4(4) . . . no N4 C20 C19 123.2(3) . . . no N5 C21 C22 123.3(3) . . . no C21 C22 C23 118.7(3) . . . no C22 C23 C24 118.7(3) . . . no C23 C24 C25 119.8(3) . . . no C24 C25 C26 123.3(3) . . . no N5 C25 C24 121.2(3) . . . no N5 C25 C26 115.6(3) . . . no N6 C26 C27 121.4(3) . . . no N6 C26 C25 115.8(3) . . . no C25 C26 C27 122.8(3) . . . no C26 C27 C28 119.1(3) . . . no C27 C28 C29 119.5(3) . . . no C28 C29 C30 118.8(3) . . . no N6 C30 C29 123.2(3) . . . no C2 C1 H1 118.66 . . . no N1 C1 H1 118.68 . . . no C1 C2 H2 120.54 . . . no C3 C2 H2 120.68 . . . no C4 C3 H3 120.20 . . . no C2 C3 H3 120.16 . . . no C5 C4 H4 120.29 . . . no C3 C4 H4 120.37 . . . no C6 C7 H7 120.16 . . . no C8 C7 H7 120.19 . . . no C9 C8 H8 120.40 . . . no C7 C8 H8 120.28 . . . no C10 C9 H9 120.74 . . . no C8 C9 H9 120.63 . . . no C9 C10 H10 118.49 . . . no N2 C10 H10 118.48 . . . no N3 C11 H11 118.67 . . . no C12 C11 H11 118.63 . . . no C13 C12 H12 120.35 . . . no C11 C12 H12 120.49 . . . no C14 C13 H13 120.41 . . . no C12 C13 H13 120.50 . . . no C13 C14 H14 120.36 . . . no C15 C14 H14 120.51 . . . no C18 C17 H17 120.36 . . . no C16 C17 H17 120.39 . . . no C19 C18 H18 120.07 . . . no C17 C18 H18 120.15 . . . no C20 C19 H19 120.76 . . . no C18 C19 H19 120.82 . . . no N4 C20 H20 118.42 . . . no C19 C20 H20 118.35 . . . no C22 C21 H21 118.35 . . . no N5 C21 H21 118.39 . . . no C21 C22 H22 120.60 . . . no C23 C22 H22 120.66 . . . no C22 C23 H23 120.62 . . . no C24 C23 H23 120.68 . . . no C25 C24 H24 120.09 . . . no C23 C24 H24 120.07 . . . no C26 C27 H27 120.45 . . . no C28 C27 H27 120.49 . . . no C29 C28 H28 120.25 . . . no C27 C28 H28 120.24 . . . no C28 C29 H29 120.56 . . . no C30 C29 H29 120.62 . . . no C29 C30 H30 118.37 . . . no N6 C30 H30 118.43 . . . no N7 C31 C32 123.0(4) . . . no C31 C32 C33 118.6(4) . . . no C32 C33 C34 119.4(4) . . . no C33 C34 C35 119.3(4) . . . no C34 C35 C36 123.1(3) . . . no N7 C35 C34 121.0(3) . . . no N7 C35 C36 115.9(3) . . . no N8 C36 C37 120.8(3) . . . no C35 C36 C37 123.5(3) . . . no N8 C36 C35 115.7(3) . . . no C36 C37 C38 119.3(4) . . . no C37 C38 C39 119.6(4) . . . no C38 C39 C40 119.1(4) . . . no N8 C40 C39 122.6(4) . . . no N9 C41 C42 122.5(3) . . . no C41 C42 C43 118.5(3) . . . no C42 C43 C44 119.5(4) . . . no C43 C44 C45 119.3(4) . . . no C44 C45 C46 123.4(3) . . . no N9 C45 C44 121.6(3) . . . no N9 C45 C46 115.0(3) . . . no C45 C46 C47 122.9(3) . . . no N10 C46 C47 121.4(3) . . . no N10 C46 C45 115.7(3) . . . no C46 C47 C48 119.4(4) . . . no C47 C48 C49 118.9(4) . . . no C48 C49 C50 119.1(4) . . . no N10 C50 C49 122.5(4) . . . no N11 C51 C52 123.0(3) . . . no C51 C52 C53 118.5(3) . . . no C52 C53 C54 119.1(4) . . . no C53 C54 C55 119.9(3) . . . no N11 C55 C56 115.6(3) . . . no N11 C55 C54 121.2(3) . . . no C54 C55 C56 123.2(3) . . . no C55 C56 C57 122.8(3) . . . no N12 C56 C57 121.3(3) . . . no N12 C56 C55 115.9(3) . . . no C56 C57 C58 118.9(3) . . . no C57 C58 C59 119.9(3) . . . no C58 C59 C60 118.6(3) . . . no N12 C60 C59 123.0(3) . . . no C32 C31 H31 118.46 . . . no N7 C31 H31 118.53 . . . no C33 C32 H32 120.67 . . . no C31 C32 H32 120.69 . . . no C32 C33 H33 120.28 . . . no C34 C33 H33 120.31 . . . no C33 C34 H34 120.33 . . . no C35 C34 H34 120.34 . . . no C38 C37 H37 120.36 . . . no C36 C37 H37 120.36 . . . no C37 C38 H38 120.22 . . . no C39 C38 H38 120.21 . . . no C38 C39 H39 120.49 . . . no C40 C39 H39 120.42 . . . no C39 C40 H40 118.78 . . . no N8 C40 H40 118.65 . . . no N9 C41 H41 118.71 . . . no C42 C41 H41 118.83 . . . no C43 C42 H42 120.73 . . . no C41 C42 H42 120.79 . . . no C42 C43 H43 120.33 . . . no C44 C43 H43 120.20 . . . no C43 C44 H44 120.31 . . . no C45 C44 H44 120.35 . . . no C46 C47 H47 120.33 . . . no C48 C47 H47 120.24 . . . no C49 C48 H48 120.56 . . . no C47 C48 H48 120.51 . . . no C50 C49 H49 120.48 . . . no C48 C49 H49 120.44 . . . no N10 C50 H50 118.79 . . . no C49 C50 H50 118.70 . . . no N11 C51 H51 118.48 . . . no C52 C51 H51 118.51 . . . no C53 C52 H52 120.74 . . . no C51 C52 H52 120.81 . . . no C52 C53 H53 120.45 . . . no C54 C53 H53 120.47 . . . no C53 C54 H54 120.03 . . . no C55 C54 H54 120.09 . . . no C58 C57 H57 120.58 . . . no C56 C57 H57 120.48 . . . no C59 C58 H58 120.00 . . . no C57 C58 H58 120.16 . . . no C58 C59 H59 120.64 . . . no C60 C59 H59 120.75 . . . no C59 C60 H60 118.48 . . . no N12 C60 H60 118.48 . . . no O2 C61 O4 125.6(4) . . . no O2 C61 C62 111.6(3) . . . no O4 C61 C62 122.8(3) . . . no O3 C62 O5 126.5(4) . . . no O3 C62 C61 111.4(3) . . . no O5 C62 C61 122.0(3) . . . no O6 C63 O8 125.7(4) . . . no O6 C63 C64 113.0(3) . . . no O8 C63 C64 121.3(4) . . . no O7 C64 O9 125.1(3) . . . no O7 C64 C63 112.3(3) . . . no O9 C64 C63 122.6(3) . . . no O10 C65 O12 126.1(4) . . . no O10 C65 C66 113.8(3) . . . no O12 C65 C66 120.2(3) . . . no O11 C66 O13 125.8(3) . . . no O11 C66 C65 114.1(3) . . . no O13 C66 C65 120.1(3) . . . no 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 O11 Nb1 O2 C61 84.4(3) . . . . no O1 Nb1 O3 C62 90.2(3) . . . . no O2 Nb1 O3 C62 -2.0(2) . . . . no O6 Nb1 O3 C62 -169.3(2) . . . . no O7 Nb1 O3 C62 -34.3(3) . . . . no O10 Nb1 O3 C62 177.8(3) . . . . no O11 Nb1 O3 C62 -107.3(3) . . . . no O1 Nb1 O6 C63 -108.2(3) . . . . no O2 Nb1 O6 C63 -12.7(3) . . . . no O3 Nb1 O6 C63 147.5(2) . . . . no O7 Nb1 O6 C63 -1.6(2) . . . . no O10 Nb1 O6 C63 160.3(3) . . . . no O11 Nb1 O6 C63 84.9(3) . . . . no O1 Nb1 O7 C64 89.4(3) . . . . no O2 Nb1 O7 C64 179.4(3) . . . . no O3 Nb1 O7 C64 -147.8(2) . . . . no O6 Nb1 O7 C64 6.7(2) . . . . no O10 Nb1 O7 C64 -21.5(3) . . . . no O11 Nb1 O7 C64 -75.3(2) . . . . no O1 Nb1 O10 C65 -175.3(3) . . . . no O2 Nb1 O10 C65 84.6(3) . . . . no O3 Nb1 O10 C65 84.4(3) . . . . no O6 Nb1 O10 C65 -87.9(3) . . . . no O7 Nb1 O10 C65 -59.7(3) . . . . no O11 Nb1 O10 C65 -3.0(2) . . . . no O2 Nb1 O11 C66 -141.7(2) . . . . no O1 Nb1 O2 C61 -92.7(3) . . . . no O3 Nb1 O2 C61 6.3(2) . . . . no O6 Nb1 O2 C61 174.4(2) . . . . no O7 Nb1 O2 C61 163.1(3) . . . . no O10 Nb1 O2 C61 6.1(3) . . . . no O10 Nb1 O11 C66 2.2(2) . . . . no O3 Nb1 O11 C66 -71.6(2) . . . . no O6 Nb1 O11 C66 77.0(2) . . . . no O7 Nb1 O11 C66 150.3(2) . . . . no N2 Co1 N1 C5 2.3(2) . . . . no N3 Co1 N1 C1 -85.1(3) . . . . no N3 Co1 N1 C5 93.5(2) . . . . no N2 Co1 N1 C1 -176.4(3) . . . . no N1 Co1 N2 C6 -3.4(2) . . . . no N1 Co1 N2 C10 -179.8(3) . . . . no N3 Co1 N2 C6 -97.8(2) . . . . no N5 Co1 N1 C1 12.2(3) . . . . no N5 Co1 N1 C5 -169.2(2) . . . . no N6 Co1 N1 C1 89.2(3) . . . . no N6 Co1 N1 C5 -92.2(2) . . . . no N6 Co1 N2 C10 -89.3(3) . . . . no N1 Co1 N3 C11 7.3(3) . . . . no N1 Co1 N3 C15 -175.6(2) . . . . no N2 Co1 N3 C11 84.5(3) . . . . no N2 Co1 N3 C15 -98.4(2) . . . . no N4 Co1 N3 C11 -179.5(3) . . . . no N4 Co1 N3 C15 -2.4(2) . . . . no N5 Co1 N3 C11 -88.6(3) . . . . no N5 Co1 N3 C15 88.5(2) . . . . no N2 Co1 N4 C16 90.4(2) . . . . no N2 Co1 N4 C20 -86.7(3) . . . . no N3 Co1 N2 C10 85.9(3) . . . . no N4 Co1 N2 C6 -174.8(2) . . . . no N4 Co1 N2 C10 8.9(3) . . . . no N6 Co1 N2 C6 87.0(2) . . . . no N5 Co1 N4 C16 -96.9(2) . . . . no N5 Co1 N4 C20 85.9(3) . . . . no N6 Co1 N4 C16 -174.0(2) . . . . no N6 Co1 N4 C20 8.8(3) . . . . no N1 Co1 N5 C21 -88.8(3) . . . . no N1 Co1 N5 C25 85.6(2) . . . . no N3 Co1 N5 C21 6.7(3) . . . . no N3 Co1 N5 C25 -179.0(2) . . . . no N4 Co1 N5 C21 83.7(3) . . . . no N4 Co1 N5 C25 -101.9(2) . . . . no N6 Co1 N5 C21 -179.0(3) . . . . no N6 Co1 N5 C25 -4.6(2) . . . . no N1 Co1 N6 C26 -92.8(2) . . . . no N1 Co1 N6 C30 86.9(2) . . . . no N2 Co1 N6 C26 -170.0(2) . . . . no N2 Co1 N6 C30 9.7(3) . . . . no N4 Co1 N6 C26 92.9(2) . . . . no N4 Co1 N6 C30 -87.4(3) . . . . no N5 Co1 N6 C26 2.3(2) . . . . no N5 Co1 N6 C30 -178.1(3) . . . . no N3 Co1 N4 C20 -177.6(3) . . . . no N3 Co1 N4 C16 -0.5(2) . . . . no N11 Co2 N7 C35 178.1(2) . . . . no N11 Co2 N7 C31 1.6(3) . . . . no N7 Co2 N8 C36 8.9(2) . . . . no N7 Co2 N8 C40 -178.4(3) . . . . no N9 Co2 N8 C36 -86.5(2) . . . . no N9 Co2 N8 C40 86.2(3) . . . . no N10 Co2 N8 C36 -163.7(2) . . . . no N12 Co2 N7 C31 79.6(3) . . . . no N12 Co2 N7 C35 -103.9(2) . . . . no N11 Co2 N12 C60 178.4(3) . . . . no N12 Co2 N8 C40 -88.0(3) . . . . no N7 Co2 N9 C41 12.3(3) . . . . no N7 Co2 N9 C45 -174.5(2) . . . . no N8 Co2 N9 C41 89.5(3) . . . . no N8 Co2 N9 C45 -97.3(2) . . . . no N10 Co2 N9 C41 -176.9(3) . . . . no N10 Co2 N9 C45 -3.8(2) . . . . no N11 Co2 N9 C41 -82.7(3) . . . . no N11 Co2 N9 C45 90.5(2) . . . . no N8 Co2 N10 C46 87.6(2) . . . . no N8 Co2 N10 C50 -83.1(3) . . . . no N9 Co2 N10 C46 -2.3(2) . . . . no N9 Co2 N10 C50 -173.0(3) . . . . no N11 Co2 N10 C46 -96.1(2) . . . . no N11 Co2 N10 C50 93.2(3) . . . . no N8 Co2 N7 C31 176.9(3) . . . . no N8 Co2 N7 C35 -6.6(2) . . . . no N9 Co2 N7 C31 -93.7(3) . . . . no N9 Co2 N7 C35 82.8(2) . . . . no N9 Co2 N11 C55 -173.3(2) . . . . no N10 Co2 N11 C51 84.5(3) . . . . no N10 Co2 N11 C55 -95.7(2) . . . . no N12 Co2 N11 C51 180.0(3) . . . . no N12 Co2 N11 C55 -0.3(2) . . . . no N7 Co2 N12 C56 -91.8(2) . . . . no N7 Co2 N12 C60 84.2(3) . . . . no N8 Co2 N12 C56 -169.2(2) . . . . no N8 Co2 N12 C60 6.9(3) . . . . no N10 Co2 N12 C56 96.3(2) . . . . no N10 Co2 N12 C60 -87.6(3) . . . . no N11 Co2 N12 C56 2.3(2) . . . . no N12 Co2 N10 C46 -174.4(2) . . . . no N12 Co2 N10 C50 14.9(3) . . . . no N7 Co2 N11 C51 -88.9(3) . . . . no N7 Co2 N11 C55 90.9(2) . . . . no N9 Co2 N11 C51 7.0(3) . . . . no N12 Co2 N8 C36 99.3(2) . . . . no N10 Co2 N8 C40 9.0(3) . . . . no Nb1 O2 C61 O4 170.9(3) . . . . no Nb1 O2 C61 C62 -8.8(4) . . . . no Nb1 O3 C62 O5 178.4(3) . . . . no Nb1 O3 C62 C61 -1.5(4) . . . . no Nb1 O6 C63 O8 175.7(3) . . . . no Nb1 O6 C63 C64 -2.6(4) . . . . no Nb1 O7 C64 O9 170.6(3) . . . . no Nb1 O7 C64 C63 -9.8(4) . . . . no Nb1 O10 C65 C66 3.2(4) . . . . no Nb1 O10 C65 O12 -177.0(3) . . . . no Nb1 O11 C66 O13 178.4(3) . . . . no Nb1 O11 C66 C65 -1.4(4) . . . . no C1 N1 C5 C4 -1.1(5) . . . . no C1 N1 C5 C6 177.9(3) . . . . no C5 N1 C1 C2 -0.5(5) . . . . no Co1 N1 C1 C2 178.0(3) . . . . no Co1 N1 C5 C4 -179.8(3) . . . . no Co1 N1 C5 C6 -0.8(3) . . . . no Co1 N2 C6 C7 -176.6(3) . . . . no C6 N2 C10 C9 -0.3(5) . . . . no Co1 N2 C10 C9 175.9(3) . . . . no C10 N2 C6 C7 0.0(5) . . . . no Co1 N2 C6 C5 4.1(4) . . . . no C10 N2 C6 C5 -179.3(3) . . . . no Co1 N3 C11 C12 174.8(3) . . . . no C11 N3 C15 C16 -178.0(3) . . . . no Co1 N3 C15 C14 -174.1(3) . . . . no C15 N3 C11 C12 -2.3(5) . . . . no C11 N3 C15 C14 3.2(5) . . . . no Co1 N3 C15 C16 4.7(4) . . . . no Co1 N4 C16 C15 3.0(4) . . . . no C16 N4 C20 C19 -1.9(5) . . . . no Co1 N4 C16 C17 -175.6(3) . . . . no C20 N4 C16 C15 -179.7(3) . . . . no C20 N4 C16 C17 1.8(5) . . . . no Co1 N4 C20 C19 175.2(3) . . . . no Co1 N5 C21 C22 172.2(3) . . . . no C21 N5 C25 C26 -179.0(3) . . . . no Co1 N5 C25 C24 -173.1(2) . . . . no C25 N5 C21 C22 -2.1(5) . . . . no C21 N5 C25 C24 1.7(4) . . . . no Co1 N5 C25 C26 6.2(3) . . . . no C30 N6 C26 C27 1.4(4) . . . . no Co1 N6 C30 C29 179.2(3) . . . . no C30 N6 C26 C25 -179.5(3) . . . . no Co1 N6 C26 C25 0.2(3) . . . . no Co1 N6 C26 C27 -178.8(2) . . . . no C26 N6 C30 C29 -1.2(4) . . . . no C31 N7 C35 C34 -0.2(5) . . . . no C35 N7 C31 C32 -0.1(5) . . . . no C31 N7 C35 C36 -179.6(3) . . . . no Co2 N7 C35 C36 3.7(4) . . . . no Co2 N7 C31 C32 176.3(3) . . . . no Co2 N7 C35 C34 -176.9(3) . . . . no C36 N8 C40 C39 2.2(5) . . . . no Co2 N8 C36 C37 170.5(3) . . . . no C40 N8 C36 C37 -2.8(5) . . . . no Co2 N8 C36 C35 -9.8(3) . . . . no C40 N8 C36 C35 176.9(3) . . . . no Co2 N8 C40 C39 -170.3(3) . . . . no Co2 N9 C45 C44 -171.5(3) . . . . no Co2 N9 C41 C42 171.6(3) . . . . no C41 N9 C45 C46 -177.7(3) . . . . no Co2 N9 C45 C46 8.8(3) . . . . no C41 N9 C45 C44 2.1(5) . . . . no C45 N9 C41 C42 -1.4(5) . . . . no C50 N10 C46 C47 0.4(5) . . . . no Co2 N10 C50 C49 168.6(3) . . . . no C50 N10 C46 C45 178.9(3) . . . . no Co2 N10 C46 C45 7.4(3) . . . . no C46 N10 C50 C49 -1.8(5) . . . . no Co2 N10 C46 C47 -171.1(3) . . . . no Co2 N11 C55 C54 178.9(3) . . . . no C51 N11 C55 C56 178.1(3) . . . . no Co2 N11 C55 C56 -1.6(3) . . . . no C51 N11 C55 C54 -1.3(4) . . . . no C55 N11 C51 C52 0.7(5) . . . . no Co2 N11 C51 C52 -179.5(3) . . . . no C60 N12 C56 C57 -0.2(5) . . . . no C56 N12 C60 C59 -0.2(5) . . . . no Co2 N12 C56 C55 -3.9(3) . . . . no C60 N12 C56 C55 179.7(3) . . . . no Co2 N12 C60 C59 -176.2(3) . . . . no Co2 N12 C56 C57 176.2(2) . . . . no N1 C1 C2 C3 1.5(6) . . . . no C1 C2 C3 C4 -0.8(6) . . . . no C2 C3 C4 C5 -0.7(6) . . . . no C3 C4 C5 C6 -177.2(3) . . . . no C3 C4 C5 N1 1.8(5) . . . . no N1 C5 C6 N2 -2.2(4) . . . . no C4 C5 C6 C7 -2.5(5) . . . . no C4 C5 C6 N2 176.8(3) . . . . no N1 C5 C6 C7 178.5(3) . . . . no N2 C6 C7 C8 -0.1(5) . . . . no C5 C6 C7 C8 179.1(3) . . . . no C6 C7 C8 C9 0.5(6) . . . . no C7 C8 C9 C10 -0.7(6) . . . . no C8 C9 C10 N2 0.6(6) . . . . no N3 C11 C12 C13 -0.3(6) . . . . no C11 C12 C13 C14 1.9(6) . . . . no C12 C13 C14 C15 -1.0(6) . . . . no C13 C14 C15 C16 179.7(3) . . . . no C13 C14 C15 N3 -1.6(5) . . . . no C14 C15 C16 C17 -7.8(5) . . . . no N3 C15 C16 C17 173.5(3) . . . . no N3 C15 C16 N4 -5.1(4) . . . . no C14 C15 C16 N4 173.7(3) . . . . no C15 C16 C17 C18 -179.0(3) . . . . no N4 C16 C17 C18 -0.6(5) . . . . no C16 C17 C18 C19 -0.6(6) . . . . no C17 C18 C19 C20 0.5(6) . . . . no C18 C19 C20 N4 0.8(6) . . . . no N5 C21 C22 C23 1.2(5) . . . . no C21 C22 C23 C24 0.1(6) . . . . no C22 C23 C24 C25 -0.4(6) . . . . no C23 C24 C25 C26 -179.8(3) . . . . no C23 C24 C25 N5 -0.5(5) . . . . no N5 C25 C26 C27 174.8(3) . . . . no C24 C25 C26 N6 175.0(3) . . . . no C24 C25 C26 C27 -5.9(5) . . . . no N5 C25 C26 N6 -4.3(4) . . . . no C25 C26 C27 C28 -180.0(3) . . . . no N6 C26 C27 C28 -1.0(5) . . . . no C26 C27 C28 C29 0.2(6) . . . . no C27 C28 C29 C30 0.1(6) . . . . no C28 C29 C30 N6 0.4(5) . . . . no N7 C31 C32 C33 0.0(6) . . . . no C31 C32 C33 C34 0.3(6) . . . . no C32 C33 C34 C35 -0.5(6) . . . . no C33 C34 C35 C36 179.8(4) . . . . no C33 C34 C35 N7 0.4(6) . . . . no C34 C35 C36 C37 4.4(5) . . . . no N7 C35 C36 N8 4.1(4) . . . . no N7 C35 C36 C37 -176.2(3) . . . . no C34 C35 C36 N8 -175.3(3) . . . . no N8 C36 C37 C38 1.2(5) . . . . no C35 C36 C37 C38 -178.5(3) . . . . no C36 C37 C38 C39 1.1(6) . . . . no C37 C38 C39 C40 -1.7(6) . . . . no C38 C39 C40 N8 0.1(6) . . . . no N9 C41 C42 C43 -0.6(6) . . . . no C41 C42 C43 C44 1.9(6) . . . . no C42 C43 C44 C45 -1.3(6) . . . . no C43 C44 C45 C46 179.0(3) . . . . no C43 C44 C45 N9 -0.7(5) . . . . no N9 C45 C46 C47 167.7(3) . . . . no C44 C45 C46 C47 -12.0(5) . . . . no N9 C45 C46 N10 -10.8(4) . . . . no C44 C45 C46 N10 169.5(3) . . . . no N10 C46 C47 C48 0.9(5) . . . . no C45 C46 C47 C48 -177.5(3) . . . . no C46 C47 C48 C49 -0.7(6) . . . . no C47 C48 C49 C50 -0.8(6) . . . . no C48 C49 C50 N10 2.1(6) . . . . no N11 C51 C52 C53 0.4(5) . . . . no C51 C52 C53 C54 -1.0(6) . . . . no C52 C53 C54 C55 0.5(6) . . . . no C53 C54 C55 C56 -178.7(3) . . . . no C53 C54 C55 N11 0.7(5) . . . . no C54 C55 C56 C57 3.0(5) . . . . no C54 C55 C56 N12 -176.9(3) . . . . no N11 C55 C56 N12 3.7(4) . . . . no N11 C55 C56 C57 -176.5(3) . . . . no N12 C56 C57 C58 -0.1(5) . . . . no C55 C56 C57 C58 -179.9(3) . . . . no C56 C57 C58 C59 0.6(6) . . . . no C57 C58 C59 C60 -0.9(6) . . . . no C58 C59 C60 N12 0.7(6) . . . . no O2 C61 C62 O5 -173.6(3) . . . . no O4 C61 C62 O3 -173.4(3) . . . . no O4 C61 C62 O5 6.7(6) . . . . no O2 C61 C62 O3 6.3(4) . . . . no O8 C63 C64 O7 -170.6(3) . . . . no O6 C63 C64 O9 -172.7(3) . . . . no O8 C63 C64 O9 9.0(5) . . . . no O6 C63 C64 O7 7.7(4) . . . . no O10 C65 C66 O11 -1.1(4) . . . . no O12 C65 C66 O13 -0.7(5) . . . . no O10 C65 C66 O13 179.2(3) . . . . no O12 C65 C66 O11 179.1(3) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C4 H4 O23 0.9300 2.5100 3.393(5) 158.00 1_545 no C27 H27 O23 0.9300 2.5200 3.437(4) 168.00 2_545 no C33 H33 O1 0.9300 2.4100 3.241(5) 149.00 4_564 no C38 H38 O11 0.9300 2.5900 3.178(5) 122.00 . no C39 H39 O9 0.9300 2.5300 3.418(5) 159.00 . no C41 H41 O15 0.9300 2.3900 3.148(5) 139.00 4_554 no C44 H44 O23 0.9300 2.4300 3.341(5) 167.00 1_545 no C52 H52 O2 0.9300 2.5700 3.317(5) 138.00 4_554 no C54 H54 O11 0.9300 2.4900 3.169(4) 130.00 2_645 no C57 H57 O13 0.9300 2.3600 3.264(4) 163.00 2_645 no #=============================================================================== data_III _database_code_depnum_ccdc_archive 'CCDC 648554' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H24 Co N6), C6 Nb O13, 12(H2 O), Cl' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural '2(C30 H24 Co N6), C6 Nb O13, 12(H2 O), Cl' _chemical_formula_sum 'C66 H72 Cl Co2 N12 Nb O25' _chemical_formula_iupac ? _chemical_formula_weight 1679.58 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 15.1030(10) _cell_length_b 22.075(2) _cell_length_c 22.386(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7463.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 22725 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 30.51 _cell_special_details ; ? ; _exptl_crystal_description polyhedral _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.712 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.93 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(3) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius-Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 22725 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 22725 # number of observed reflections (> n sig(I)) _reflns_number_gt 16932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software (Nonius, 1998)' _computing_cell_refinement 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0646P)^2^+2.0458P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(10) # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ad _refine_ls_number_reflns 22725 _refine_ls_number_parameters 1033 _refine_ls_number_restraints 44 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.311 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.070 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Co1 Co Uani 0.36323(3) 0.33020(2) -0.00085(2) 1.000 0.0277(1) . . N1 N Uani 0.25044(16) 0.33848(12) 0.05528(11) 1.000 0.0297(8) . . N2 N Uani 0.28544(17) 0.39636(12) -0.04624(11) 1.000 0.0296(7) . . N3 N Uani 0.44205(17) 0.39359(12) 0.04704(12) 1.000 0.0307(8) . . N4 N Uani 0.47591(17) 0.33926(12) -0.05568(12) 1.000 0.0328(8) . . N5 N Uani 0.41390(18) 0.25160(13) 0.04254(12) 1.000 0.0347(8) . . N6 N Uani 0.30131(19) 0.25778(12) -0.04860(12) 1.000 0.0340(8) . . C1 C Uani 0.2391(2) 0.31103(17) 0.10865(15) 1.000 0.0388(10) . . C2 C Uani 0.1658(3) 0.31970(17) 0.14325(16) 1.000 0.0446(11) . . C3 C Uani 0.0991(3) 0.35623(19) 0.12229(19) 1.000 0.0530(12) . . C4 C Uani 0.1087(2) 0.38431(18) 0.06704(18) 1.000 0.0469(11) . . C5 C Uani 0.1855(2) 0.37516(15) 0.03509(14) 1.000 0.0310(9) . . C6 C Uani 0.2041(2) 0.40528(13) -0.02294(14) 1.000 0.0298(9) . . C7 C Uani 0.1422(2) 0.44094(16) -0.05218(15) 1.000 0.0406(10) . . C8 C Uani 0.1644(3) 0.46740(17) -0.10634(16) 1.000 0.0433(11) . . C9 C Uani 0.2464(3) 0.45816(16) -0.12952(16) 1.000 0.0429(11) . . C10 C Uani 0.3052(2) 0.42177(15) -0.09838(14) 1.000 0.0356(10) . . C11 C Uani 0.4221(2) 0.41831(16) 0.09969(15) 1.000 0.0380(10) . . C12 C Uani 0.4795(3) 0.45684(17) 0.13012(17) 1.000 0.0424(11) . . C13 C Uani 0.5585(3) 0.47039(17) 0.10547(18) 1.000 0.0452(11) . . C14 C Uani 0.5807(2) 0.44628(16) 0.04927(16) 1.000 0.0412(11) . . C15 C Uani 0.5207(2) 0.40713(14) 0.02185(15) 1.000 0.0313(9) . . C16 C Uani 0.5398(2) 0.37741(15) -0.03655(14) 1.000 0.0328(9) . . C17 C Uani 0.6171(2) 0.38690(18) -0.06879(18) 1.000 0.0477(12) . . C18 C Uani 0.6284(3) 0.35644(19) -0.12217(19) 1.000 0.0543(12) . . C19 C Uani 0.5636(3) 0.31816(19) -0.14257(17) 1.000 0.0527(14) . . C20 C Uani 0.4882(3) 0.30963(18) -0.10806(16) 1.000 0.0424(11) . . C21 C Uani 0.4730(2) 0.25123(18) 0.08753(17) 1.000 0.0440(12) . . C22 C Uani 0.4968(3) 0.1978(2) 0.11757(18) 1.000 0.0510(14) . . C23 C Uani 0.4568(3) 0.14396(19) 0.10103(18) 1.000 0.0497(12) . . C24 C Uani 0.3971(3) 0.14425(17) 0.05459(17) 1.000 0.0468(11) . . C25 C Uani 0.3779(2) 0.19837(14) 0.02536(15) 1.000 0.0340(9) . . C26 C Uani 0.3167(2) 0.20160(14) -0.02643(15) 1.000 0.0346(10) . . C27 C Uani 0.2790(3) 0.15156(16) -0.05258(17) 1.000 0.0458(11) . . C28 C Uani 0.2271(3) 0.15725(18) -0.10234(17) 1.000 0.0477(12) . . C29 C Uani 0.2115(2) 0.21434(18) -0.12563(16) 1.000 0.0437(11) . . C30 C Uani 0.2491(2) 0.26310(16) -0.09684(16) 1.000 0.0391(11) . . Co2 Co Uani 0.36137(3) 0.67053(2) 0.02860(2) 1.000 0.0283(1) . . N7 N Uani 0.47963(18) 0.66338(12) 0.07840(12) 1.000 0.0330(8) . . N8 N Uani 0.43713(18) 0.60760(12) -0.02170(12) 1.000 0.0314(8) . . N9 N Uani 0.28917(17) 0.60379(12) 0.07455(12) 1.000 0.0312(8) . . N10 N Uani 0.24693(19) 0.66109(13) -0.02564(13) 1.000 0.0368(8) . . N11 N Uani 0.30422(18) 0.74439(13) 0.07672(13) 1.000 0.0350(8) . . N12 N Uani 0.4107(2) 0.74745(12) -0.01751(12) 1.000 0.0340(8) . . C31 C Uani 0.4945(3) 0.68999(18) 0.13143(17) 1.000 0.0463(11) . . C32 C Uani 0.5740(3) 0.6825(2) 0.16162(19) 1.000 0.0570(16) . . C33 C Uani 0.6383(3) 0.6482(2) 0.1376(2) 1.000 0.0623(17) . . C34 C Uani 0.6250(3) 0.62095(19) 0.0823(2) 1.000 0.0543(14) . . C35 C Uani 0.5441(2) 0.62884(16) 0.05446(15) 1.000 0.0356(10) . . C36 C Uani 0.5217(2) 0.59987(15) -0.00371(15) 1.000 0.0340(9) . . C37 C Uani 0.5822(3) 0.56723(18) -0.03719(17) 1.000 0.0482(11) . . C38 C Uani 0.5560(3) 0.5418(2) -0.09000(19) 1.000 0.0567(16) . . C39 C Uani 0.4701(3) 0.54719(19) -0.10795(17) 1.000 0.0576(13) . . C40 C Uani 0.4119(3) 0.58148(16) -0.07353(16) 1.000 0.0448(11) . . C41 C Uani 0.3132(2) 0.57776(15) 0.12619(15) 1.000 0.0379(10) . . C42 C Uani 0.2601(3) 0.53566(17) 0.15593(17) 1.000 0.0460(11) . . C43 C Uani 0.1816(3) 0.51983(18) 0.13108(18) 1.000 0.0500(12) . . C44 C Uani 0.1566(3) 0.54540(18) 0.07765(17) 1.000 0.0473(11) . . C45 C Uani 0.2107(2) 0.58891(15) 0.04999(15) 1.000 0.0348(10) . . C46 C Uani 0.1879(2) 0.61917(16) -0.00618(16) 1.000 0.0364(10) . . C47 C Uani 0.1119(3) 0.6067(2) -0.03960(19) 1.000 0.0520(12) . . C48 C Uani 0.0973(3) 0.6361(2) -0.0922(2) 1.000 0.0610(16) . . C49 C Uani 0.1572(3) 0.6775(2) -0.11198(18) 1.000 0.0597(16) . . C50 C Uani 0.2318(3) 0.68954(18) -0.07759(17) 1.000 0.0483(12) . . C51 C Uani 0.2502(2) 0.74006(17) 0.12434(16) 1.000 0.0429(11) . . C52 C Uani 0.2146(3) 0.7899(2) 0.15296(18) 1.000 0.0543(14) . . C53 C Uani 0.2362(3) 0.84722(19) 0.13160(19) 1.000 0.0527(12) . . C54 C Uani 0.2903(3) 0.85193(17) 0.08278(18) 1.000 0.0464(11) . . C55 C Uani 0.3243(2) 0.80004(15) 0.05588(15) 1.000 0.0347(10) . . C56 C Uani 0.3829(2) 0.80126(14) 0.00340(14) 1.000 0.0331(9) . . C57 C Uani 0.4073(3) 0.85500(16) -0.02521(18) 1.000 0.0456(11) . . C58 C Uani 0.4615(3) 0.85232(18) -0.07491(17) 1.000 0.0501(14) . . C59 C Uani 0.4900(3) 0.79751(19) -0.09594(17) 1.000 0.0461(11) . . C60 C Uani 0.4644(3) 0.74634(17) -0.06547(16) 1.000 0.0422(11) . . Nb1 Nb Uani 0.84193(2) 0.48783(1) 0.20016(1) 1.000 0.0299(1) . . O1 O Uani 0.82436(16) 0.41078(11) 0.20227(12) 1.000 0.0450(8) . . O2 O Uani 0.77505(13) 0.50375(12) 0.11829(10) 1.000 0.0366(7) . . O3 O Uani 0.93904(13) 0.48326(11) 0.12825(10) 1.000 0.0352(7) . . O4 O Uani 0.78100(14) 0.51150(12) 0.01892(9) 1.000 0.0397(7) . . O5 O Uani 0.96389(14) 0.49239(12) 0.03005(10) 1.000 0.0382(7) . . O6 O Uani 0.82513(14) 0.49504(11) 0.29482(10) 1.000 0.0411(7) . . O7 O Uani 0.71600(15) 0.52575(12) 0.21621(10) 1.000 0.0416(8) . . O8 O Uani 0.73809(17) 0.52266(14) 0.36996(11) 1.000 0.0515(9) . . O9 O Uani 0.62908(19) 0.57417(14) 0.28069(12) 1.000 0.0575(10) . . O10 O Uani 0.96871(14) 0.48330(11) 0.23858(10) 1.000 0.0360(7) . . O11 O Uani 0.89032(15) 0.58226(10) 0.20501(11) 1.000 0.0379(7) . . O12 O Uani 1.08987(17) 0.53295(13) 0.26719(12) 1.000 0.0521(9) . . O13 O Uani 1.0097(2) 0.63866(13) 0.22330(13) 1.000 0.0607(11) . . C61 C Uani 0.81525(19) 0.50377(14) 0.06775(14) 1.000 0.0297(9) . . C62 C Uani 0.91481(19) 0.49207(14) 0.07389(14) 1.000 0.0302(9) . . C63 C Uani 0.7548(2) 0.51798(18) 0.31731(14) 1.000 0.0387(10) . . C64 C Uani 0.6926(2) 0.54234(17) 0.26858(16) 1.000 0.0386(10) . . C65 C Uani 1.0154(2) 0.53147(16) 0.24583(14) 1.000 0.0353(10) . . C66 C Uani 0.9694(2) 0.59009(16) 0.22331(15) 1.000 0.0396(11) . . O14 O Uani 0.9196(2) 0.29661(15) 0.21044(16) 1.000 0.0667(11) . . O15 O Uani 1.0613(2) 0.30772(15) 0.29294(15) 1.000 0.0671(11) . . O16 O Uani 1.1617(3) 0.41109(19) 0.2773(2) 1.000 0.105(2) . . O17 O Uani 0.8244(2) 0.70997(16) 0.20320(18) 1.000 0.0735(13) . . O18 O Uani 0.7005(2) 0.70268(16) 0.29307(15) 1.000 0.0661(11) . . O19 O Uani 0.4475(2) 0.57177(14) 0.24631(17) 1.000 0.0661(11) . . O20 O Uani 0.4078(3) 0.30310(16) 0.21639(18) 1.000 0.0830(16) . . O21 O Uani 0.5762(2) 0.28434(18) 0.2608(2) 1.000 0.0843(14) . . O22 O Uani 0.65605(19) 0.17516(14) 0.23666(17) 1.000 0.0672(13) . . O23 O Uani 0.8361(2) 0.18536(16) 0.2233(2) 1.000 0.0857(14) . . O24 O Uani 0.5705(3) 0.4113(2) 0.3034(2) 1.000 0.117(2) . . O25 O Uani 0.56969(18) 0.48795(16) 0.40869(12) 1.000 0.0534(9) . . Cl1 Cl Uani 0.36478(9) 0.43526(6) 0.26540(5) 1.000 0.0723(4) . . H1 H Uiso 0.28310 0.28510 0.12240 1.000 0.0470 calc R H2 H Uiso 0.16120 0.30120 0.18040 1.000 0.0530 calc R H3 H Uiso 0.04810 0.36210 0.14480 1.000 0.0640 calc R H4 H Uiso 0.06390 0.40890 0.05190 1.000 0.0560 calc R H7 H Uiso 0.08640 0.44700 -0.03570 1.000 0.0490 calc R H8 H Uiso 0.12350 0.49130 -0.12660 1.000 0.0520 calc R H9 H Uiso 0.26270 0.47590 -0.16550 1.000 0.0510 calc R H10 H Uiso 0.36090 0.41480 -0.11470 1.000 0.0430 calc R H11 H Uiso 0.36760 0.40940 0.11680 1.000 0.0460 calc R H12 H Uiso 0.46350 0.47300 0.16690 1.000 0.0510 calc R H13 H Uiso 0.59810 0.49550 0.12550 1.000 0.0540 calc R H14 H Uiso 0.63400 0.45620 0.03090 1.000 0.0490 calc R H17 H Uiso 0.66040 0.41320 -0.05470 1.000 0.0570 calc R H18 H Uiso 0.67990 0.36190 -0.14430 1.000 0.0650 calc R H19 H Uiso 0.57010 0.29820 -0.17890 1.000 0.0630 calc R H20 H Uiso 0.44490 0.28280 -0.12130 1.000 0.0510 calc R H21 H Uiso 0.49890 0.28760 0.09910 1.000 0.0530 calc R H22 H Uiso 0.53860 0.19860 0.14800 1.000 0.0610 calc R H23 H Uiso 0.47010 0.10810 0.12100 1.000 0.0590 calc R H24 H Uiso 0.36970 0.10850 0.04280 1.000 0.0560 calc R H27 H Uiso 0.28890 0.11340 -0.03630 1.000 0.0550 calc R H28 H Uiso 0.20260 0.12320 -0.12030 1.000 0.0570 calc R H29 H Uiso 0.17670 0.21960 -0.15950 1.000 0.0520 calc R H30 H Uiso 0.23780 0.30170 -0.11160 1.000 0.0470 calc R H31 H Uiso 0.45050 0.71400 0.14830 1.000 0.0560 calc R H32 H Uiso 0.58270 0.70120 0.19840 1.000 0.0690 calc R H33 H Uiso 0.69150 0.64260 0.15780 1.000 0.0750 calc R H34 H Uiso 0.66940 0.59800 0.06450 1.000 0.0650 calc R H37 H Uiso 0.64020 0.56270 -0.02390 1.000 0.0580 calc R H38 H Uiso 0.59660 0.52090 -0.11350 1.000 0.0680 calc R H39 H Uiso 0.45070 0.52830 -0.14270 1.000 0.0690 calc R H40 H Uiso 0.35400 0.58650 -0.08660 1.000 0.0530 calc R H41 H Uiso 0.36760 0.58820 0.14290 1.000 0.0460 calc R H42 H Uiso 0.27830 0.51880 0.19200 1.000 0.0550 calc R H43 H Uiso 0.14490 0.49190 0.15000 1.000 0.0600 calc R H44 H Uiso 0.10360 0.53380 0.05970 1.000 0.0570 calc R H47 H Uiso 0.07120 0.57820 -0.02590 1.000 0.0620 calc R H48 H Uiso 0.04660 0.62800 -0.11450 1.000 0.0730 calc R H49 H Uiso 0.14850 0.69740 -0.14810 1.000 0.0720 calc R H50 H Uiso 0.27240 0.71820 -0.09100 1.000 0.0580 calc R H51 H Uiso 0.23620 0.70170 0.13870 1.000 0.0520 calc R H52 H Uiso 0.17720 0.78520 0.18560 1.000 0.0650 calc R H53 H Uiso 0.21420 0.88180 0.15020 1.000 0.0630 calc R H54 H Uiso 0.30450 0.88990 0.06750 1.000 0.0560 calc R H57 H Uiso 0.38730 0.89210 -0.01100 1.000 0.0550 calc R H58 H Uiso 0.47860 0.88780 -0.09410 1.000 0.0600 calc R H59 H Uiso 0.52550 0.79490 -0.12980 1.000 0.0560 calc R H60 H Uiso 0.48520 0.70900 -0.07870 1.000 0.0510 calc R H141 H Uiso 0.885(2) 0.3256(14) 0.2070(19) 1.000 0.0800 . . H142 H Uiso 0.954(2) 0.305(2) 0.2390(15) 1.000 0.0800 . . H151 H Uiso 1.069(3) 0.2826(16) 0.3202(16) 1.000 0.0810 . . H152 H Uiso 1.099(3) 0.3349(15) 0.299(2) 1.000 0.0810 . . H161 H Uiso 1.126(4) 0.436(2) 0.2611(18) 1.000 0.1260 . . H162 H Uiso 1.195(3) 0.401(3) 0.2490(16) 1.000 0.1260 . . H171 H Uiso 0.859(3) 0.6801(16) 0.2057(17) 1.000 0.0880 . . H172 H Uiso 0.805(3) 0.713(2) 0.2384(9) 1.000 0.0880 . . H181 H Uiso 0.665(2) 0.6741(12) 0.290(2) 1.000 0.0790 . . H182 H Uiso 0.6789(19) 0.7316(13) 0.2741(17) 1.000 0.0790 . . H191 H Uiso 0.5028(7) 0.569(2) 0.245(2) 1.000 0.0790 . . H192 H Uiso 0.431(3) 0.5397(14) 0.263(2) 1.000 0.0790 . . H201 H Uiso 0.384(4) 0.327(2) 0.2405(17) 1.000 0.1000 . . H202 H Uiso 0.4389(16) 0.2803(11) 0.2368(18) 1.000 0.1000 . . H211 H Uiso 0.6219(19) 0.2645(16) 0.265(3) 1.000 0.1010 . . H212 H Uiso 0.590(3) 0.3207(8) 0.267(2) 1.000 0.1010 . . H221 H Uiso 0.6120(19) 0.1527(18) 0.237(2) 1.000 0.0800 . . H222 H Uiso 0.688(2) 0.164(2) 0.2089(16) 1.000 0.0800 . . H231 H Uiso 0.859(3) 0.2198(10) 0.225(2) 1.000 0.1030 . . H232 H Uiso 0.874(3) 0.1615(17) 0.237(3) 1.000 0.1030 . . H241 H Uiso 0.53320 0.44090 0.29660 1.000 0.1400 . . H242 H Uiso 0.595(4) 0.424(2) 0.335(2) 1.000 0.1400 . . H251 H Uiso 0.568(2) 0.485(2) 0.4460(5) 1.000 0.0640 . . H252 H Uiso 0.6223(12) 0.497(2) 0.4006(15) 1.000 0.0640 . . 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 Co1 0.0251(2) 0.0278(2) 0.0301(2) 0.0007(2) -0.0004(2) -0.0003(2) N1 0.0269(12) 0.0318(14) 0.0304(13) 0.0044(10) -0.0008(10) -0.0029(11) N2 0.0257(12) 0.0292(13) 0.0338(13) 0.0042(11) 0.0009(10) 0.0002(10) N3 0.0274(13) 0.0312(14) 0.0336(14) -0.0002(11) 0.0016(10) -0.0021(11) N4 0.0307(13) 0.0362(15) 0.0314(13) -0.0015(11) 0.0029(11) 0.0030(11) N5 0.0311(14) 0.0369(15) 0.0361(15) 0.0042(12) -0.0005(11) 0.0020(11) N6 0.0372(15) 0.0311(14) 0.0336(14) -0.0005(11) -0.0010(11) -0.0004(12) C1 0.0403(18) 0.0419(19) 0.0342(17) 0.0104(14) 0.0014(14) -0.0009(15) C2 0.051(2) 0.047(2) 0.0358(17) 0.0105(15) 0.0106(16) -0.0052(17) C3 0.046(2) 0.058(2) 0.055(2) 0.012(2) 0.0230(19) 0.0045(19) C4 0.0367(19) 0.048(2) 0.056(2) 0.0153(18) 0.0111(17) 0.0081(16) C5 0.0287(15) 0.0329(16) 0.0315(16) 0.0025(13) 0.0015(12) -0.0016(12) C6 0.0320(16) 0.0247(14) 0.0326(15) 0.0036(12) -0.0013(13) -0.0010(12) C7 0.0338(18) 0.0460(19) 0.0419(17) 0.0049(15) 0.0018(15) 0.0087(15) C8 0.0436(19) 0.047(2) 0.0393(18) 0.0101(15) -0.0078(16) 0.0100(16) C9 0.053(2) 0.0406(19) 0.0351(17) 0.0111(15) 0.0041(16) 0.0012(17) C10 0.0361(17) 0.0380(18) 0.0326(16) 0.0057(14) 0.0056(13) -0.0018(14) C11 0.0367(17) 0.0425(19) 0.0349(17) -0.0053(14) 0.0096(14) -0.0052(14) C12 0.048(2) 0.0406(19) 0.0387(18) -0.0091(16) -0.0030(16) 0.0004(16) C13 0.046(2) 0.0376(19) 0.052(2) -0.0086(16) -0.0139(17) 0.0005(15) C14 0.0267(16) 0.045(2) 0.052(2) -0.0026(17) 0.0012(15) -0.0039(14) C15 0.0255(15) 0.0295(15) 0.0389(17) 0.0013(13) 0.0016(13) 0.0028(12) C16 0.0308(16) 0.0343(17) 0.0332(16) 0.0029(13) 0.0039(13) 0.0037(13) C17 0.039(2) 0.048(2) 0.056(2) 0.0027(18) 0.0128(17) -0.0037(16) C18 0.050(2) 0.059(2) 0.054(2) -0.0004(19) 0.029(2) 0.005(2) C19 0.064(3) 0.055(2) 0.039(2) -0.0010(17) 0.0158(18) 0.014(2) C20 0.046(2) 0.047(2) 0.0343(18) -0.0054(15) 0.0042(15) 0.0084(16) C21 0.043(2) 0.046(2) 0.043(2) 0.0042(16) -0.0067(16) 0.0040(16) C22 0.047(2) 0.063(3) 0.043(2) 0.0141(19) -0.0063(17) 0.019(2) C23 0.059(2) 0.045(2) 0.045(2) 0.0111(17) 0.0069(18) 0.0139(19) C24 0.060(2) 0.0333(18) 0.047(2) 0.0051(16) 0.0051(18) 0.0059(17) C25 0.0376(17) 0.0296(15) 0.0347(16) 0.0008(13) 0.0048(14) 0.0054(13) C26 0.0394(18) 0.0270(15) 0.0375(17) -0.0024(13) 0.0053(14) 0.0016(13) C27 0.060(2) 0.0275(17) 0.050(2) -0.0050(15) 0.0067(18) -0.0029(16) C28 0.052(2) 0.044(2) 0.047(2) -0.0144(17) 0.0024(17) -0.0125(17) C29 0.0409(19) 0.055(2) 0.0351(18) -0.0072(16) -0.0013(15) -0.0089(17) C30 0.0401(18) 0.0364(18) 0.0408(19) -0.0008(14) -0.0034(15) -0.0023(15) Co2 0.0295(2) 0.0270(2) 0.0284(2) -0.0010(2) -0.0010(2) 0.0002(2) N7 0.0338(14) 0.0351(15) 0.0300(13) 0.0000(11) -0.0017(11) -0.0054(12) N8 0.0360(14) 0.0297(13) 0.0286(13) -0.0033(11) -0.0014(11) 0.0034(11) N9 0.0302(13) 0.0306(14) 0.0328(14) 0.0011(11) 0.0000(11) 0.0001(11) N10 0.0381(15) 0.0347(15) 0.0375(14) -0.0027(12) -0.0096(12) 0.0067(12) N11 0.0345(14) 0.0345(15) 0.0359(15) -0.0026(12) 0.0008(12) 0.0002(12) N12 0.0391(15) 0.0308(13) 0.0320(14) 0.0003(11) 0.0036(11) 0.0010(11) C31 0.053(2) 0.049(2) 0.0369(18) -0.0033(16) -0.0072(16) -0.0130(17) C32 0.068(3) 0.056(3) 0.047(2) 0.0008(19) -0.027(2) -0.011(2) C33 0.053(3) 0.062(3) 0.072(3) 0.005(2) -0.034(2) -0.009(2) C34 0.040(2) 0.052(2) 0.071(3) 0.005(2) -0.017(2) 0.0011(17) C35 0.0316(16) 0.0354(17) 0.0399(18) 0.0048(14) -0.0026(14) -0.0037(14) C36 0.0333(16) 0.0327(16) 0.0360(17) 0.0069(14) 0.0037(14) 0.0028(13) C37 0.0385(19) 0.054(2) 0.052(2) 0.0035(19) 0.0118(17) 0.0131(17) C38 0.064(3) 0.057(3) 0.049(2) 0.0006(19) 0.021(2) 0.018(2) C39 0.093(3) 0.048(2) 0.0318(18) -0.0088(17) 0.005(2) 0.015(2) C40 0.055(2) 0.041(2) 0.0383(18) -0.0098(15) -0.0036(16) 0.0110(17) C41 0.0396(18) 0.0373(18) 0.0369(17) 0.0038(14) -0.0043(14) -0.0003(14) C42 0.052(2) 0.046(2) 0.0399(19) 0.0110(16) 0.0084(17) -0.0037(17) C43 0.052(2) 0.047(2) 0.051(2) 0.0012(18) 0.0122(17) -0.0127(18) C44 0.0359(18) 0.055(2) 0.051(2) -0.0097(17) 0.0058(17) -0.0121(17) C45 0.0288(16) 0.0334(17) 0.0423(18) -0.0083(14) -0.0011(13) -0.0020(13) C46 0.0302(16) 0.0388(17) 0.0401(18) -0.0036(15) -0.0034(14) 0.0037(13) C47 0.038(2) 0.057(2) 0.061(2) -0.006(2) -0.0123(18) -0.0054(18) C48 0.054(2) 0.070(3) 0.059(3) -0.014(2) -0.027(2) 0.006(2) C49 0.073(3) 0.062(3) 0.044(2) -0.0045(19) -0.025(2) 0.021(2) C50 0.061(2) 0.041(2) 0.043(2) 0.0032(16) -0.0131(18) 0.0092(18) C51 0.048(2) 0.0403(19) 0.0405(19) -0.0019(15) 0.0102(16) 0.0041(16) C52 0.057(2) 0.060(3) 0.046(2) -0.0087(19) 0.0140(19) 0.007(2) C53 0.057(2) 0.044(2) 0.057(2) -0.0117(18) 0.009(2) 0.0135(18) C54 0.054(2) 0.0331(18) 0.052(2) -0.0042(16) 0.0002(18) 0.0065(16) C55 0.0361(17) 0.0304(16) 0.0375(17) -0.0011(13) -0.0061(13) 0.0033(13) C56 0.0365(17) 0.0303(15) 0.0324(15) 0.0003(13) -0.0052(13) -0.0007(13) C57 0.060(2) 0.0299(17) 0.047(2) 0.0067(16) -0.0035(19) -0.0023(16) C58 0.073(3) 0.0362(19) 0.041(2) 0.0100(16) 0.0004(19) -0.0098(19) C59 0.050(2) 0.054(2) 0.0344(19) 0.0055(17) 0.0021(16) -0.0036(18) C60 0.053(2) 0.040(2) 0.0335(18) 0.0027(15) 0.0070(16) 0.0057(17) Nb1 0.0247(1) 0.0355(1) 0.0294(1) 0.0024(1) -0.0033(1) 0.0028(1) O1 0.0462(14) 0.0378(13) 0.0511(14) 0.0031(12) -0.0064(12) -0.0061(10) O2 0.0244(10) 0.0551(16) 0.0304(11) 0.0008(10) -0.0017(9) 0.0042(10) O3 0.0242(10) 0.0500(13) 0.0314(11) -0.0012(11) -0.0023(8) 0.0066(10) O4 0.0286(11) 0.0594(15) 0.0312(11) 0.0029(11) -0.0059(9) 0.0025(11) O5 0.0259(10) 0.0539(14) 0.0349(11) -0.0006(11) 0.0022(9) 0.0049(10) O6 0.0339(11) 0.0610(16) 0.0283(10) 0.0080(11) -0.0030(9) 0.0091(10) O7 0.0276(11) 0.0652(17) 0.0320(12) 0.0017(11) -0.0020(9) 0.0085(11) O8 0.0409(13) 0.082(2) 0.0315(13) 0.0008(13) 0.0015(11) -0.0054(14) O9 0.0480(15) 0.078(2) 0.0465(15) -0.0053(14) 0.0052(12) 0.0235(15) O10 0.0293(11) 0.0414(12) 0.0372(12) 0.0040(11) -0.0045(9) 0.0052(10) O11 0.0414(13) 0.0338(12) 0.0386(12) 0.0031(10) -0.0055(11) 0.0027(9) O12 0.0352(13) 0.0743(19) 0.0469(15) 0.0115(13) -0.0130(12) -0.0095(12) O13 0.070(2) 0.0530(17) 0.0591(18) 0.0135(14) -0.0220(15) -0.0229(15) C61 0.0259(13) 0.0325(17) 0.0306(15) -0.0002(12) -0.0009(11) 0.0005(12) C62 0.0280(14) 0.0276(15) 0.0351(16) -0.0025(13) -0.0015(12) 0.0004(12) C63 0.0320(16) 0.051(2) 0.0331(17) 0.0029(15) -0.0012(12) -0.0053(16) C64 0.0316(16) 0.047(2) 0.0372(18) -0.0008(16) -0.0005(14) 0.0003(15) C65 0.0313(16) 0.052(2) 0.0226(14) 0.0062(13) -0.0013(12) -0.0016(14) C66 0.046(2) 0.047(2) 0.0257(15) -0.0004(14) -0.0070(14) -0.0046(16) O14 0.064(2) 0.0602(19) 0.076(2) -0.0009(17) 0.0031(17) 0.0165(15) O15 0.077(2) 0.0594(19) 0.065(2) 0.0157(17) -0.0006(17) -0.0068(16) O16 0.065(2) 0.075(3) 0.175(5) -0.004(3) 0.024(3) 0.005(2) O17 0.0515(18) 0.070(2) 0.099(3) -0.008(2) 0.0003(19) 0.0145(15) O18 0.0632(19) 0.071(2) 0.064(2) -0.0083(17) -0.0184(16) -0.0015(16) O19 0.0584(18) 0.0538(18) 0.086(2) 0.0021(17) -0.0172(18) 0.0072(15) O20 0.096(3) 0.059(2) 0.094(3) -0.0148(19) -0.023(2) 0.0204(19) O21 0.072(2) 0.081(2) 0.100(3) -0.015(2) -0.004(2) 0.0108(19) O22 0.0389(15) 0.0626(19) 0.100(3) 0.0219(18) 0.0033(16) -0.0073(15) O23 0.057(2) 0.068(2) 0.132(3) 0.024(2) -0.016(2) 0.0133(17) O24 0.121(4) 0.129(4) 0.100(3) -0.018(3) -0.010(3) -0.008(3) O25 0.0450(14) 0.0736(19) 0.0416(14) -0.0065(15) 0.0060(11) -0.0102(15) Cl1 0.0795(8) 0.0721(7) 0.0654(7) 0.0042(6) 0.0085(6) 0.0141(6) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O7 2.109(2) . . no Nb1 O10 2.102(2) . . no Nb1 O11 2.212(2) . . no Nb1 O3 2.180(2) . . no Nb1 O1 1.722(2) . . no Nb1 O2 2.122(2) . . no Nb1 O6 2.140(2) . . no Co1 N4 2.108(3) . . no Co1 N1 2.125(2) . . no Co1 N2 2.132(3) . . no Co1 N3 2.127(3) . . no Co1 N5 2.131(3) . . no Co1 N6 2.138(3) . . no Co2 N7 2.111(3) . . no Co2 N8 2.123(3) . . no Co2 N9 2.102(3) . . no Co2 N10 2.123(3) . . no Co2 N11 2.136(3) . . no Co2 N12 2.122(3) . . no O2 C61 1.284(4) . . no O3 C62 1.286(4) . . no O4 C61 1.221(4) . . no O5 C62 1.230(4) . . no O6 C63 1.280(4) . . no O7 C64 1.278(4) . . no O8 C63 1.210(4) . . no O9 C64 1.220(4) . . no O10 C65 1.286(4) . . no O11 C66 1.274(4) . . no O12 C65 1.223(4) . . no O13 C66 1.233(4) . . no O14 H142 0.84(3) . . no O14 H141 0.83(3) . . no O15 H151 0.83(4) . . no O15 H152 0.84(4) . . no N1 C5 1.350(4) . . no N1 C1 1.351(4) . . no N2 C10 1.329(4) . . no N2 C6 1.349(4) . . no N3 C15 1.348(4) . . no N3 C11 1.333(4) . . no N4 C20 1.355(5) . . no N4 C16 1.351(4) . . no N5 C21 1.346(4) . . no N5 C25 1.351(4) . . no N6 C30 1.342(4) . . no N6 C26 1.356(4) . . no O16 H161 0.85(5) . . no O16 H162 0.84(4) . . no N7 C35 1.348(4) . . no N7 C31 1.343(5) . . no N8 C40 1.351(5) . . no N8 C36 1.350(4) . . no N9 C41 1.341(4) . . no N9 C45 1.347(4) . . no N10 C50 1.341(5) . . no N10 C46 1.357(4) . . no N11 C55 1.349(4) . . no N11 C51 1.346(4) . . no N12 C60 1.346(5) . . no N12 C56 1.344(4) . . no O17 H171 0.84(4) . . no O17 H172 0.84(2) . . no O18 H182 0.83(3) . . no O18 H181 0.83(3) . . no O19 H192 0.84(4) . . no O19 H191 0.838(11) . . no O20 H202 0.83(3) . . no O20 H201 0.84(5) . . no C1 C2 1.365(5) . . no C2 C3 1.373(6) . . no C3 C4 1.391(6) . . no C4 C5 1.378(5) . . no C5 C6 1.486(4) . . no C6 C7 1.386(4) . . no C7 C8 1.387(5) . . no C8 C9 1.358(6) . . no C9 C10 1.386(5) . . no C11 C12 1.393(5) . . no C12 C13 1.348(6) . . no C13 C14 1.407(5) . . no C14 C15 1.395(5) . . no C15 C16 1.491(5) . . no C16 C17 1.388(5) . . no C17 C18 1.382(6) . . no C18 C19 1.371(6) . . no C19 C20 1.389(6) . . no C21 C22 1.405(6) . . no C22 C23 1.384(6) . . no C23 C24 1.376(6) . . no C24 C25 1.393(5) . . no C25 C26 1.484(5) . . no C26 C27 1.374(5) . . no C27 C28 1.368(6) . . no C28 C29 1.384(6) . . no C29 C30 1.377(5) . . no C1 H1 0.9295 . . no C2 H2 0.9291 . . no C3 H3 0.9295 . . no C4 H4 0.9313 . . no C7 H7 0.9296 . . no C8 H8 0.9304 . . no C9 H9 0.9288 . . no C10 H10 0.9300 . . no C11 H11 0.9289 . . no C12 H12 0.9293 . . no C13 H13 0.9306 . . no C14 H14 0.9301 . . no C17 H17 0.9296 . . no C18 H18 0.9300 . . no C19 H19 0.9302 . . no C20 H20 0.9308 . . no C21 H21 0.9299 . . no O21 H212 0.84(2) . . no O21 H211 0.82(3) . . no C22 H22 0.9289 . . no C23 H23 0.9310 . . no C24 H24 0.9294 . . no C27 H27 0.9299 . . no C28 H28 0.9293 . . no C29 H29 0.9298 . . no C30 H30 0.9297 . . no C31 C32 1.388(6) . . no C32 C33 1.344(6) . . no C33 C34 1.391(6) . . no C34 C35 1.383(5) . . no C35 C36 1.490(5) . . no C36 C37 1.384(5) . . no C37 C38 1.367(6) . . no C38 C39 1.363(6) . . no C39 C40 1.393(6) . . no C41 C42 1.397(5) . . no C42 C43 1.355(6) . . no C43 C44 1.375(6) . . no C44 C45 1.405(5) . . no C45 C46 1.465(5) . . no C46 C47 1.398(5) . . no C47 C48 1.363(6) . . no C48 C49 1.360(6) . . no C49 C50 1.390(6) . . no C51 C52 1.382(6) . . no C52 C53 1.392(6) . . no C53 C54 1.369(6) . . no C54 C55 1.392(5) . . no C55 C56 1.471(4) . . no C56 C57 1.398(5) . . no C57 C58 1.383(6) . . no C58 C59 1.368(6) . . no C59 C60 1.375(6) . . no O22 H221 0.83(3) . . no O22 H222 0.82(3) . . no C31 H31 0.9301 . . no C32 H32 0.9304 . . no C33 H33 0.9302 . . no C34 H34 0.9301 . . no C37 H37 0.9305 . . no C38 H38 0.9304 . . no C39 H39 0.9300 . . no C40 H40 0.9287 . . no C41 H41 0.9317 . . no C42 H42 0.9306 . . no C43 H43 0.9310 . . no C44 H44 0.9315 . . no C47 H47 0.9315 . . no C48 H48 0.9314 . . no C49 H49 0.9295 . . no C50 H50 0.9308 . . no C51 H51 0.9301 . . no C52 H52 0.9294 . . no C53 H53 0.9308 . . no C54 H54 0.9304 . . no C57 H57 0.9291 . . no C58 H58 0.9299 . . no C59 H59 0.9302 . . no C60 H60 0.9305 . . no C61 C62 1.532(4) . . no C63 C64 1.537(5) . . no C65 C66 1.553(5) . . no O23 H231 0.84(3) . . no O23 H232 0.84(5) . . no O24 H241 0.8761 . . no O24 H242 0.85(5) . . no O25 H251 0.838(12) . . no O25 H252 0.84(2) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O10 142.67(8) . . . no O2 Nb1 O11 92.50(9) . . . no O3 Nb1 O6 144.52(8) . . . no O3 Nb1 O7 138.68(9) . . . no O3 Nb1 O10 71.76(8) . . . no O3 Nb1 O11 81.81(9) . . . no O6 Nb1 O7 72.23(8) . . . no O6 Nb1 O10 72.92(8) . . . no O6 Nb1 O11 85.44(9) . . . no O7 Nb1 O10 140.43(9) . . . no O7 Nb1 O11 85.15(9) . . . no O10 Nb1 O11 73.96(9) . . . no O1 Nb1 O6 91.60(11) . . . no O1 Nb1 O7 104.38(11) . . . no O1 Nb1 O10 94.71(11) . . . no O1 Nb1 O11 168.67(10) . . . no O2 Nb1 O3 71.95(8) . . . no O2 Nb1 O6 141.85(8) . . . no O2 Nb1 O7 69.64(8) . . . no O1 Nb1 O3 94.49(11) . . . no O1 Nb1 O2 96.55(11) . . . no N1 Co1 N3 95.40(10) . . . no N1 Co1 N4 169.60(10) . . . no N1 Co1 N6 90.54(10) . . . no N2 Co1 N3 95.62(10) . . . no N1 Co1 N5 95.08(10) . . . no N1 Co1 N2 77.36(10) . . . no N4 Co1 N5 93.03(10) . . . no N4 Co1 N6 97.64(11) . . . no N5 Co1 N6 77.07(10) . . . no N3 Co1 N6 171.30(11) . . . no N2 Co1 N5 166.66(10) . . . no N2 Co1 N6 91.88(10) . . . no N2 Co1 N4 95.87(10) . . . no N3 Co1 N5 96.03(10) . . . no N3 Co1 N4 77.24(10) . . . no N7 Co2 N8 77.01(10) . . . no N11 Co2 N12 77.08(11) . . . no N8 Co2 N10 94.08(11) . . . no N8 Co2 N11 169.94(11) . . . no N7 Co2 N9 97.36(10) . . . no N7 Co2 N10 169.61(11) . . . no N7 Co2 N11 97.62(11) . . . no N7 Co2 N12 91.12(11) . . . no N8 Co2 N9 94.62(10) . . . no N10 Co2 N12 94.94(11) . . . no N9 Co2 N10 77.80(11) . . . no N9 Co2 N11 94.51(11) . . . no N8 Co2 N12 94.38(11) . . . no N10 Co2 N11 91.97(11) . . . no N9 Co2 N12 168.81(11) . . . no Nb1 O2 C61 122.41(18) . . . no Nb1 O3 C62 120.03(18) . . . no Nb1 O6 C63 121.2(2) . . . no Nb1 O7 C64 121.3(2) . . . no Nb1 O10 C65 120.8(2) . . . no Nb1 O11 C66 117.0(2) . . . no H141 O14 H142 107(4) . . . no H151 O15 H152 105(4) . . . no Co1 N1 C5 115.9(2) . . . no Co1 N1 C1 125.9(2) . . . no C1 N1 C5 118.2(3) . . . no Co1 N2 C6 114.7(2) . . . no Co1 N2 C10 125.7(2) . . . no C6 N2 C10 118.9(3) . . . no Co1 N3 C15 115.3(2) . . . no Co1 N3 C11 126.0(2) . . . no C11 N3 C15 118.6(3) . . . no Co1 N4 C16 116.8(2) . . . no Co1 N4 C20 124.7(2) . . . no C16 N4 C20 118.5(3) . . . no Co1 N5 C25 115.7(2) . . . no Co1 N5 C21 125.8(2) . . . no C21 N5 C25 118.4(3) . . . no Co1 N6 C26 115.2(2) . . . no C26 N6 C30 118.4(3) . . . no Co1 N6 C30 126.4(2) . . . no H161 O16 H162 103(5) . . . no Co2 N7 C31 125.1(3) . . . no C31 N7 C35 118.6(3) . . . no Co2 N7 C35 116.3(2) . . . no Co2 N8 C40 125.7(2) . . . no C36 N8 C40 118.0(3) . . . no Co2 N8 C36 115.8(2) . . . no C41 N9 C45 119.0(3) . . . no Co2 N9 C45 115.3(2) . . . no Co2 N9 C41 125.6(2) . . . no C46 N10 C50 119.1(3) . . . no Co2 N10 C50 126.1(3) . . . no Co2 N10 C46 114.7(2) . . . no Co2 N11 C55 115.5(2) . . . no C51 N11 C55 118.4(3) . . . no Co2 N11 C51 126.2(2) . . . no Co2 N12 C56 115.4(2) . . . no C56 N12 C60 118.8(3) . . . no Co2 N12 C60 125.8(2) . . . no H171 O17 H172 102(4) . . . no H181 O18 H182 107(3) . . . no H191 O19 H192 105(4) . . . no H201 O20 H202 106(4) . . . no N1 C1 C2 122.8(3) . . . no C1 C2 C3 118.9(3) . . . no C2 C3 C4 119.3(4) . . . no C3 C4 C5 119.0(3) . . . no N1 C5 C6 115.1(3) . . . no C4 C5 C6 123.2(3) . . . no N1 C5 C4 121.7(3) . . . no N2 C6 C5 116.4(3) . . . no C5 C6 C7 122.6(3) . . . no N2 C6 C7 121.0(3) . . . no C6 C7 C8 119.3(3) . . . no C7 C8 C9 119.4(4) . . . no C8 C9 C10 118.6(3) . . . no N2 C10 C9 122.9(3) . . . no N3 C11 C12 122.8(3) . . . no C11 C12 C13 119.1(4) . . . no C12 C13 C14 119.5(4) . . . no C13 C14 C15 118.3(3) . . . no C14 C15 C16 122.2(3) . . . no N3 C15 C16 116.1(3) . . . no N3 C15 C14 121.7(3) . . . no N4 C16 C17 122.0(3) . . . no N4 C16 C15 114.5(3) . . . no C15 C16 C17 123.5(3) . . . no C16 C17 C18 118.7(3) . . . no C17 C18 C19 120.0(4) . . . no C18 C19 C20 118.9(4) . . . no N4 C20 C19 121.9(4) . . . no N5 C21 C22 122.2(4) . . . no C21 C22 C23 118.8(4) . . . no C22 C23 C24 119.0(4) . . . no C23 C24 C25 119.7(4) . . . no C24 C25 C26 122.5(3) . . . no N5 C25 C24 121.9(3) . . . no N5 C25 C26 115.6(3) . . . no N6 C26 C25 115.9(3) . . . no C25 C26 C27 123.5(3) . . . no N6 C26 C27 120.6(3) . . . no C26 C27 C28 120.7(3) . . . no C27 C28 C29 119.2(4) . . . no C28 C29 C30 117.7(3) . . . no N6 C30 C29 123.4(3) . . . no N1 C1 H1 118.59 . . . no C2 C1 H1 118.58 . . . no C1 C2 H2 120.47 . . . no C3 C2 H2 120.61 . . . no C4 C3 H3 120.42 . . . no C2 C3 H3 120.30 . . . no C5 C4 H4 120.55 . . . no C3 C4 H4 120.50 . . . no C8 C7 H7 120.36 . . . no C6 C7 H7 120.37 . . . no C9 C8 H8 120.29 . . . no C7 C8 H8 120.30 . . . no C8 C9 H9 120.64 . . . no C10 C9 H9 120.72 . . . no C9 C10 H10 118.56 . . . no N2 C10 H10 118.58 . . . no N3 C11 H11 118.56 . . . no C12 C11 H11 118.64 . . . no C13 C12 H12 120.51 . . . no C11 C12 H12 120.40 . . . no C12 C13 H13 120.25 . . . no C14 C13 H13 120.21 . . . no C13 C14 H14 120.84 . . . no C15 C14 H14 120.91 . . . no C18 C17 H17 120.69 . . . no C16 C17 H17 120.62 . . . no C17 C18 H18 120.06 . . . no C19 C18 H18 119.96 . . . no C18 C19 H19 120.51 . . . no C20 C19 H19 120.57 . . . no C19 C20 H20 119.03 . . . no N4 C20 H20 119.10 . . . no C22 C21 H21 118.95 . . . no N5 C21 H21 118.83 . . . no H211 O21 H212 106(4) . . . no C21 C22 H22 120.60 . . . no C23 C22 H22 120.62 . . . no C24 C23 H23 120.53 . . . no C22 C23 H23 120.51 . . . no C25 C24 H24 120.15 . . . no C23 C24 H24 120.15 . . . no C28 C27 H27 119.63 . . . no C26 C27 H27 119.65 . . . no C27 C28 H28 120.41 . . . no C29 C28 H28 120.38 . . . no C30 C29 H29 121.14 . . . no C28 C29 H29 121.14 . . . no N6 C30 H30 118.29 . . . no C29 C30 H30 118.32 . . . no N7 C31 C32 121.5(4) . . . no C31 C32 C33 119.8(4) . . . no C32 C33 C34 119.7(4) . . . no C33 C34 C35 118.3(4) . . . no C34 C35 C36 122.7(3) . . . no N7 C35 C36 115.2(3) . . . no N7 C35 C34 122.0(3) . . . no N8 C36 C35 114.9(3) . . . no N8 C36 C37 121.9(3) . . . no C35 C36 C37 123.2(3) . . . no C36 C37 C38 119.4(4) . . . no C37 C38 C39 119.6(4) . . . no C38 C39 C40 119.0(4) . . . no N8 C40 C39 122.0(4) . . . no N9 C41 C42 122.7(3) . . . no C41 C42 C43 118.6(4) . . . no C42 C43 C44 119.4(4) . . . no C43 C44 C45 120.3(4) . . . no C44 C45 C46 123.6(3) . . . no N9 C45 C46 116.5(3) . . . no N9 C45 C44 119.9(3) . . . no N10 C46 C47 120.1(3) . . . no C45 C46 C47 124.3(3) . . . no N10 C46 C45 115.6(3) . . . no C46 C47 C48 120.1(4) . . . no C47 C48 C49 119.6(4) . . . no C48 C49 C50 119.2(4) . . . no N10 C50 C49 121.9(4) . . . no N11 C51 C52 123.1(3) . . . no C51 C52 C53 118.3(4) . . . no C52 C53 C54 118.9(4) . . . no C53 C54 C55 120.2(4) . . . no C54 C55 C56 123.5(3) . . . no N11 C55 C56 115.4(3) . . . no N11 C55 C54 121.1(3) . . . no C55 C56 C57 122.7(3) . . . no N12 C56 C57 120.6(3) . . . no N12 C56 C55 116.7(3) . . . no C56 C57 C58 119.3(3) . . . no C57 C58 C59 120.1(4) . . . no C58 C59 C60 117.9(4) . . . no N12 C60 C59 123.4(4) . . . no H221 O22 H222 107(4) . . . no N7 C31 H31 119.24 . . . no C32 C31 H31 119.23 . . . no C31 C32 H32 120.02 . . . no C33 C32 H32 120.14 . . . no C34 C33 H33 119.99 . . . no C32 C33 H33 120.30 . . . no C33 C34 H34 120.85 . . . no C35 C34 H34 120.84 . . . no C38 C37 H37 120.32 . . . no C36 C37 H37 120.28 . . . no C37 C38 H38 120.12 . . . no C39 C38 H38 120.25 . . . no C38 C39 H39 120.48 . . . no C40 C39 H39 120.51 . . . no C39 C40 H40 119.00 . . . no N8 C40 H40 119.04 . . . no N9 C41 H41 118.61 . . . no C42 C41 H41 118.66 . . . no C43 C42 H42 120.75 . . . no C41 C42 H42 120.68 . . . no C42 C43 H43 120.32 . . . no C44 C43 H43 120.26 . . . no C45 C44 H44 119.84 . . . no C43 C44 H44 119.88 . . . no C46 C47 H47 119.92 . . . no C48 C47 H47 119.96 . . . no C49 C48 H48 120.09 . . . no C47 C48 H48 120.32 . . . no C50 C49 H49 120.39 . . . no C48 C49 H49 120.45 . . . no C49 C50 H50 119.03 . . . no N10 C50 H50 119.06 . . . no C52 C51 H51 118.43 . . . no N11 C51 H51 118.44 . . . no C51 C52 H52 120.80 . . . no C53 C52 H52 120.94 . . . no C54 C53 H53 120.53 . . . no C52 C53 H53 120.55 . . . no C55 C54 H54 119.81 . . . no C53 C54 H54 119.98 . . . no C58 C57 H57 120.38 . . . no C56 C57 H57 120.37 . . . no C59 C58 H58 119.91 . . . no C57 C58 H58 120.01 . . . no C58 C59 H59 121.11 . . . no C60 C59 H59 121.02 . . . no N12 C60 H60 118.26 . . . no C59 C60 H60 118.35 . . . no O4 C61 C62 121.3(3) . . . no O2 C61 O4 126.1(3) . . . no O2 C61 C62 112.7(3) . . . no O3 C62 C61 113.0(3) . . . no O5 C62 C61 121.3(3) . . . no O3 C62 O5 125.8(3) . . . no O6 C63 O8 126.2(3) . . . no O8 C63 C64 122.3(3) . . . no O6 C63 C64 111.5(3) . . . no O7 C64 O9 125.9(3) . . . no O9 C64 C63 121.6(3) . . . no O7 C64 C63 112.5(3) . . . no O10 C65 C66 113.8(3) . . . no O12 C65 C66 121.1(3) . . . no O10 C65 O12 125.2(3) . . . no O13 C66 C65 120.3(3) . . . no O11 C66 O13 125.5(3) . . . no O11 C66 C65 114.2(3) . . . no H231 O23 H232 106(4) . . . no H241 O24 H242 100.33 . . . no H251 O25 H252 105(3) . . . no 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 O11 Nb1 O2 C61 80.7(3) . . . . no O1 Nb1 O3 C62 96.2(2) . . . . no O2 Nb1 O3 C62 0.7(2) . . . . no O6 Nb1 O3 C62 -164.7(2) . . . . no O7 Nb1 O3 C62 -21.7(3) . . . . no O10 Nb1 O3 C62 -170.4(3) . . . . no O11 Nb1 O3 C62 -94.6(2) . . . . no O1 Nb1 O6 C63 -106.1(3) . . . . no O2 Nb1 O6 C63 -3.4(3) . . . . no O3 Nb1 O6 C63 153.8(2) . . . . no O7 Nb1 O6 C63 -1.5(3) . . . . no O10 Nb1 O6 C63 159.4(3) . . . . no O11 Nb1 O6 C63 84.8(3) . . . . no O1 Nb1 O7 C64 96.0(3) . . . . no O2 Nb1 O7 C64 -172.3(3) . . . . no O3 Nb1 O7 C64 -149.6(2) . . . . no O6 Nb1 O7 C64 9.0(3) . . . . no O10 Nb1 O7 C64 -20.4(3) . . . . no O11 Nb1 O7 C64 -77.8(3) . . . . no O1 Nb1 O10 C65 177.8(2) . . . . no O2 Nb1 O10 C65 70.5(3) . . . . no O3 Nb1 O10 C65 84.6(2) . . . . no O6 Nb1 O10 C65 -92.0(2) . . . . no O7 Nb1 O10 C65 -62.8(3) . . . . no O11 Nb1 O10 C65 -1.9(2) . . . . no O2 Nb1 O11 C66 -139.9(2) . . . . no O1 Nb1 O2 C61 -92.5(3) . . . . no O3 Nb1 O2 C61 0.1(2) . . . . no O6 Nb1 O2 C61 166.5(2) . . . . no O7 Nb1 O2 C61 164.6(3) . . . . no O10 Nb1 O2 C61 14.2(3) . . . . no O10 Nb1 O11 C66 4.7(2) . . . . no O3 Nb1 O11 C66 -68.6(2) . . . . no O6 Nb1 O11 C66 78.2(2) . . . . no O7 Nb1 O11 C66 150.8(2) . . . . no N2 Co1 N1 C5 4.4(2) . . . . no N3 Co1 N1 C1 -80.4(3) . . . . no N3 Co1 N1 C5 99.0(2) . . . . no N2 Co1 N1 C1 -174.9(3) . . . . no N1 Co1 N2 C6 -7.1(2) . . . . no N1 Co1 N2 C10 -177.0(3) . . . . no N3 Co1 N2 C6 -101.3(2) . . . . no N5 Co1 N1 C1 16.2(3) . . . . no N5 Co1 N1 C5 -164.5(2) . . . . no N6 Co1 N1 C1 93.3(3) . . . . no N6 Co1 N1 C5 -87.4(2) . . . . no N6 Co1 N2 C10 -86.9(3) . . . . no N1 Co1 N3 C11 9.3(3) . . . . no N1 Co1 N3 C15 -173.7(2) . . . . no N2 Co1 N3 C11 87.1(3) . . . . no N2 Co1 N3 C15 -95.9(2) . . . . no N4 Co1 N3 C11 -178.2(3) . . . . no N4 Co1 N3 C15 -1.1(2) . . . . no N5 Co1 N3 C11 -86.4(3) . . . . no N5 Co1 N3 C15 90.6(2) . . . . no N2 Co1 N4 C16 94.6(2) . . . . no N2 Co1 N4 C20 -85.5(3) . . . . no N3 Co1 N2 C10 88.7(3) . . . . no N4 Co1 N2 C6 -179.1(2) . . . . no N4 Co1 N2 C10 11.0(3) . . . . no N6 Co1 N2 C6 83.1(2) . . . . no N5 Co1 N4 C16 -95.3(2) . . . . no N5 Co1 N4 C20 84.6(3) . . . . no N6 Co1 N4 C16 -172.7(2) . . . . no N6 Co1 N4 C20 7.2(3) . . . . no N1 Co1 N5 C21 -92.7(3) . . . . no N1 Co1 N5 C25 82.5(2) . . . . no N3 Co1 N5 C21 3.3(3) . . . . no N3 Co1 N5 C25 178.4(2) . . . . no N4 Co1 N5 C21 80.8(3) . . . . no N4 Co1 N5 C25 -104.1(2) . . . . no N6 Co1 N5 C21 177.9(3) . . . . no N6 Co1 N5 C25 -6.9(2) . . . . no N1 Co1 N6 C26 -89.7(2) . . . . no N1 Co1 N6 C30 89.4(3) . . . . no N2 Co1 N6 C26 -167.1(2) . . . . no N2 Co1 N6 C30 12.0(3) . . . . no N4 Co1 N6 C26 96.7(2) . . . . no N4 Co1 N6 C30 -84.1(3) . . . . no N5 Co1 N6 C26 5.4(2) . . . . no N5 Co1 N6 C30 -175.5(3) . . . . no N3 Co1 N4 C20 -179.9(3) . . . . no N3 Co1 N4 C16 0.2(2) . . . . no N11 Co2 N7 C35 -166.9(2) . . . . no N11 Co2 N7 C31 13.6(3) . . . . no N7 Co2 N8 C36 -7.8(2) . . . . no N7 Co2 N8 C40 -178.6(3) . . . . no N9 Co2 N8 C36 -104.3(2) . . . . no N9 Co2 N8 C40 84.9(3) . . . . no N10 Co2 N8 C36 177.7(2) . . . . no N12 Co2 N7 C31 90.7(3) . . . . no N12 Co2 N7 C35 -89.8(2) . . . . no N11 Co2 N12 C60 -179.6(3) . . . . no N12 Co2 N8 C40 -88.5(3) . . . . no N7 Co2 N9 C41 11.4(3) . . . . no N7 Co2 N9 C45 -171.5(2) . . . . no N8 Co2 N9 C41 88.9(3) . . . . no N8 Co2 N9 C45 -94.1(2) . . . . no N10 Co2 N9 C41 -177.9(3) . . . . no N10 Co2 N9 C45 -0.9(2) . . . . no N11 Co2 N9 C41 -86.9(3) . . . . no N11 Co2 N9 C45 90.2(2) . . . . no N8 Co2 N10 C46 93.1(2) . . . . no N8 Co2 N10 C50 -82.6(3) . . . . no N9 Co2 N10 C46 -0.8(2) . . . . no N9 Co2 N10 C50 -176.5(3) . . . . no N11 Co2 N10 C46 -95.0(2) . . . . no N11 Co2 N10 C50 89.3(3) . . . . no N8 Co2 N7 C31 -175.1(3) . . . . no N8 Co2 N7 C35 4.4(2) . . . . no N9 Co2 N7 C31 -82.0(3) . . . . no N9 Co2 N7 C35 97.5(2) . . . . no N9 Co2 N11 C55 -171.7(2) . . . . no N10 Co2 N11 C51 85.2(3) . . . . no N10 Co2 N11 C55 -93.8(2) . . . . no N12 Co2 N11 C51 179.8(3) . . . . no N12 Co2 N11 C55 0.8(2) . . . . no N7 Co2 N12 C56 -98.8(2) . . . . no N7 Co2 N12 C60 82.8(3) . . . . no N8 Co2 N12 C56 -175.8(2) . . . . no N8 Co2 N12 C60 5.8(3) . . . . no N10 Co2 N12 C56 89.7(2) . . . . no N10 Co2 N12 C60 -88.7(3) . . . . no N11 Co2 N12 C56 -1.2(2) . . . . no N12 Co2 N10 C46 -172.2(2) . . . . no N12 Co2 N10 C50 12.2(3) . . . . no N7 Co2 N11 C51 -90.8(3) . . . . no N7 Co2 N11 C55 90.2(2) . . . . no N9 Co2 N11 C51 7.3(3) . . . . no N12 Co2 N8 C36 82.4(2) . . . . no N10 Co2 N8 C40 6.8(3) . . . . no Nb1 O2 C61 O4 178.6(3) . . . . no Nb1 O2 C61 C62 -0.8(4) . . . . no Nb1 O3 C62 O5 177.7(3) . . . . no Nb1 O3 C62 C61 -1.3(3) . . . . no Nb1 O6 C63 O8 178.0(3) . . . . no Nb1 O6 C63 C64 -4.3(4) . . . . no Nb1 O7 C64 O9 165.9(3) . . . . no Nb1 O7 C64 C63 -13.6(4) . . . . no Nb1 O10 C65 C66 -0.6(3) . . . . no Nb1 O10 C65 O12 -179.3(3) . . . . no Nb1 O11 C66 O13 172.6(3) . . . . no Nb1 O11 C66 C65 -6.3(4) . . . . no C1 N1 C5 C4 -0.9(5) . . . . no C1 N1 C5 C6 178.1(3) . . . . no C5 N1 C1 C2 -1.2(5) . . . . no Co1 N1 C1 C2 178.1(3) . . . . no Co1 N1 C5 C4 179.8(3) . . . . no Co1 N1 C5 C6 -1.3(3) . . . . no Co1 N2 C6 C7 -171.5(2) . . . . no C6 N2 C10 C9 1.3(5) . . . . no Co1 N2 C10 C9 170.9(3) . . . . no C10 N2 C6 C7 -0.9(4) . . . . no Co1 N2 C6 C5 8.6(3) . . . . no C10 N2 C6 C5 179.3(3) . . . . no Co1 N3 C11 C12 176.1(3) . . . . no C11 N3 C15 C16 179.1(3) . . . . no Co1 N3 C15 C14 -177.6(2) . . . . no C15 N3 C11 C12 -0.9(5) . . . . no C11 N3 C15 C14 -0.4(5) . . . . no Co1 N3 C15 C16 1.9(4) . . . . no Co1 N4 C16 C15 0.7(4) . . . . no C16 N4 C20 C19 -0.9(5) . . . . no Co1 N4 C16 C17 179.8(3) . . . . no C20 N4 C16 C15 -179.2(3) . . . . no C20 N4 C16 C17 -0.1(5) . . . . no Co1 N4 C20 C19 179.2(3) . . . . no Co1 N5 C21 C22 173.8(3) . . . . no C21 N5 C25 C26 -177.1(3) . . . . no Co1 N5 C25 C24 -172.5(3) . . . . no C25 N5 C21 C22 -1.2(5) . . . . no C21 N5 C25 C24 3.1(5) . . . . no Co1 N5 C25 C26 7.4(4) . . . . no C30 N6 C26 C27 -0.5(5) . . . . no Co1 N6 C30 C29 179.8(2) . . . . no C30 N6 C26 C25 177.5(3) . . . . no Co1 N6 C26 C25 -3.3(4) . . . . no Co1 N6 C26 C27 178.7(3) . . . . no C26 N6 C30 C29 -1.1(5) . . . . no C31 N7 C35 C34 -1.1(5) . . . . no C35 N7 C31 C32 -0.1(5) . . . . no C31 N7 C35 C36 178.7(3) . . . . no Co2 N7 C35 C36 -0.8(4) . . . . no Co2 N7 C31 C32 179.4(3) . . . . no Co2 N7 C35 C34 179.4(3) . . . . no C36 N8 C40 C39 0.3(5) . . . . no Co2 N8 C36 C37 -170.5(3) . . . . no C40 N8 C36 C37 1.1(5) . . . . no Co2 N8 C36 C35 9.7(4) . . . . no C40 N8 C36 C35 -178.7(3) . . . . no Co2 N8 C40 C39 171.0(3) . . . . no Co2 N9 C45 C44 -179.1(3) . . . . no Co2 N9 C41 C42 176.9(3) . . . . no C41 N9 C45 C46 179.6(3) . . . . no Co2 N9 C45 C46 2.3(4) . . . . no C41 N9 C45 C44 -1.8(5) . . . . no C45 N9 C41 C42 -0.1(5) . . . . no C50 N10 C46 C47 -0.9(5) . . . . no Co2 N10 C50 C49 175.8(3) . . . . no C50 N10 C46 C45 178.2(3) . . . . no Co2 N10 C46 C45 2.2(4) . . . . no C46 N10 C50 C49 0.3(6) . . . . no Co2 N10 C46 C47 -176.9(3) . . . . no Co2 N11 C55 C54 179.1(3) . . . . no C51 N11 C55 C56 -179.4(3) . . . . no Co2 N11 C55 C56 -0.3(4) . . . . no C51 N11 C55 C54 0.1(5) . . . . no C55 N11 C51 C52 -0.2(5) . . . . no Co2 N11 C51 C52 -179.2(3) . . . . no C60 N12 C56 C57 1.8(5) . . . . no C56 N12 C60 C59 -2.6(6) . . . . no Co2 N12 C56 C55 1.5(4) . . . . no C60 N12 C56 C55 180.0(3) . . . . no Co2 N12 C60 C59 175.8(3) . . . . no Co2 N12 C56 C57 -176.7(3) . . . . no N1 C1 C2 C3 2.3(6) . . . . no C1 C2 C3 C4 -1.3(6) . . . . no C2 C3 C4 C5 -0.7(6) . . . . no C3 C4 C5 C6 -177.0(3) . . . . no C3 C4 C5 N1 1.8(5) . . . . no N1 C5 C6 N2 -4.9(4) . . . . no C4 C5 C6 C7 -5.9(5) . . . . no C4 C5 C6 N2 174.0(3) . . . . no N1 C5 C6 C7 175.3(3) . . . . no N2 C6 C7 C8 0.4(5) . . . . no C5 C6 C7 C8 -179.8(3) . . . . no C6 C7 C8 C9 -0.4(5) . . . . no C7 C8 C9 C10 0.7(5) . . . . no C8 C9 C10 N2 -1.3(5) . . . . no N3 C11 C12 C13 0.5(6) . . . . no C11 C12 C13 C14 1.1(6) . . . . no C12 C13 C14 C15 -2.2(5) . . . . no C13 C14 C15 C16 -177.6(3) . . . . no C13 C14 C15 N3 1.9(5) . . . . no C14 C15 C16 C17 -1.3(5) . . . . no N3 C15 C16 C17 179.2(3) . . . . no N3 C15 C16 N4 -1.7(4) . . . . no C14 C15 C16 N4 177.8(3) . . . . no C15 C16 C17 C18 179.3(3) . . . . no N4 C16 C17 C18 0.3(5) . . . . no C16 C17 C18 C19 0.6(6) . . . . no C17 C18 C19 C20 -1.6(6) . . . . no C18 C19 C20 N4 1.8(6) . . . . no N5 C21 C22 C23 -1.3(6) . . . . no C21 C22 C23 C24 1.9(6) . . . . no C22 C23 C24 C25 -0.2(6) . . . . no C23 C24 C25 C26 177.7(4) . . . . no C23 C24 C25 N5 -2.4(6) . . . . no N5 C25 C26 C27 175.3(3) . . . . no C24 C25 C26 N6 177.1(3) . . . . no C24 C25 C26 C27 -4.9(5) . . . . no N5 C25 C26 N6 -2.7(4) . . . . no C25 C26 C27 C28 -176.2(4) . . . . no N6 C26 C27 C28 1.7(6) . . . . no C26 C27 C28 C29 -1.2(6) . . . . no C27 C28 C29 C30 -0.4(6) . . . . no C28 C29 C30 N6 1.6(5) . . . . no N7 C31 C32 C33 0.3(6) . . . . no C31 C32 C33 C34 0.7(7) . . . . no C32 C33 C34 C35 -1.8(6) . . . . no C33 C34 C35 C36 -177.7(4) . . . . no C33 C34 C35 N7 2.1(6) . . . . no C34 C35 C36 C37 -5.9(6) . . . . no N7 C35 C36 N8 -5.9(4) . . . . no N7 C35 C36 C37 174.3(3) . . . . no C34 C35 C36 N8 173.9(3) . . . . no N8 C36 C37 C38 -0.2(6) . . . . no C35 C36 C37 C38 179.6(4) . . . . no C36 C37 C38 C39 -2.2(6) . . . . no C37 C38 C39 C40 3.5(6) . . . . no C38 C39 C40 N8 -2.6(6) . . . . no N9 C41 C42 C43 1.0(6) . . . . no C41 C42 C43 C44 0.1(6) . . . . no C42 C43 C44 C45 -1.9(6) . . . . no C43 C44 C45 C46 -178.6(4) . . . . no C43 C44 C45 N9 2.8(6) . . . . no N9 C45 C46 C47 176.1(3) . . . . no C44 C45 C46 C47 -2.5(6) . . . . no N9 C45 C46 N10 -3.0(4) . . . . no C44 C45 C46 N10 178.4(3) . . . . no N10 C46 C47 C48 0.8(6) . . . . no C45 C46 C47 C48 -178.3(4) . . . . no C46 C47 C48 C49 0.1(7) . . . . no C47 C48 C49 C50 -0.8(7) . . . . no C48 C49 C50 N10 0.6(6) . . . . no N11 C51 C52 C53 -0.4(6) . . . . no C51 C52 C53 C54 1.1(6) . . . . no C52 C53 C54 C55 -1.2(6) . . . . no C53 C54 C55 C56 -179.9(4) . . . . no C53 C54 C55 N11 0.7(6) . . . . no C54 C55 C56 C57 -2.1(5) . . . . no C54 C55 C56 N12 179.8(3) . . . . no N11 C55 C56 N12 -0.8(4) . . . . no N11 C55 C56 C57 177.4(3) . . . . no N12 C56 C57 C58 -0.9(6) . . . . no C55 C56 C57 C58 -179.0(4) . . . . no C56 C57 C58 C59 0.6(6) . . . . no C57 C58 C59 C60 -1.2(6) . . . . no C58 C59 C60 N12 2.3(6) . . . . no O2 C61 C62 O5 -177.8(3) . . . . no O4 C61 C62 O3 -178.1(3) . . . . no O4 C61 C62 O5 2.8(5) . . . . no O2 C61 C62 O3 1.3(4) . . . . no O8 C63 C64 O7 -171.1(4) . . . . no O6 C63 C64 O9 -168.4(3) . . . . no O8 C63 C64 O9 9.4(6) . . . . no O6 C63 C64 O7 11.2(4) . . . . no O10 C65 C66 O11 4.7(4) . . . . no O12 C65 C66 O13 4.5(5) . . . . no O10 C65 C66 O13 -174.3(3) . . . . no O12 C65 C66 O11 -176.6(3) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O14 H141 O1 0.83(3) 2.09(3) 2.908(4) 167(3) . no O14 H142 O15 0.84(3) 2.02(3) 2.837(5) 162(4) . no O15 H151 O17 0.83(4) 2.33(4) 2.765(5) 113(3) 4_745 no O15 H152 O16 0.84(4) 1.99(4) 2.762(5) 153(4) . no O16 H161 O12 0.85(5) 2.21(5) 2.909(5) 139(4) . no O16 H162 Cl1 0.84(4) 2.70(5) 3.125(5) 113(4) 1_655 no O17 H171 O11 0.84(4) 2.21(4) 2.990(4) 154(4) . no O17 H171 O13 0.84(4) 2.48(4) 3.242(4) 150(4) . no O17 H172 O18 0.84(2) 2.01(4) 2.752(5) 146(4) . no O18 H181 O9 0.83(3) 2.28(3) 3.048(5) 154(3) . no O18 H182 O20 0.83(3) 2.06(3) 2.763(5) 142(3) 4_655 no O19 H191 O9 0.838(11) 2.07(2) 2.849(4) 154(4) . no O19 H192 Cl1 0.84(4) 2.51(3) 3.290(3) 155(4) . no O20 H201 Cl1 0.84(5) 2.47(4) 3.184(4) 144(4) . no O20 H202 O21 0.83(3) 2.14(3) 2.762(6) 132(2) . no O21 H211 O22 0.82(3) 2.14(4) 2.749(5) 131(4) . no O21 H212 O24 0.84(2) 2.18(2) 2.962(6) 155(4) . no O22 H221 O19 0.83(3) 2.03(4) 2.793(4) 152(3) 4_645 no O22 H222 O23 0.82(3) 2.31(3) 2.745(4) 114(3) . no O23 H231 O14 0.84(3) 1.95(3) 2.776(5) 167(4) . no O23 H232 O13 0.84(5) 2.03(5) 2.813(5) 155(4) 4_745 no O24 H241 Cl1 0.8800 2.6400 3.265(5) 129.00 . no O24 H242 O25 0.85(5) 2.21(5) 2.902(5) 140(5) . no O25 H251 O5 0.838(12) 2.005(17) 2.798(4) 157(4) 2_665 no O25 H252 O8 0.84(2) 1.96(2) 2.794(4) 171(3) . no C4 H4 O5 0.9300 2.4300 3.341(4) 165.00 1_455 no C7 H7 O5 0.9300 2.5700 3.454(4) 160.00 1_455 no C12 H12 Cl1 0.9300 2.7900 3.521(4) 136.00 . no C14 H14 O4 0.9300 2.5500 3.419(4) 156.00 . no C31 H31 O21 0.9300 2.5900 3.361(6) 140.00 4_655 no C37 H37 O4 0.9300 2.5900 3.479(5) 160.00 . no C38 H38 O6 0.9300 2.3900 3.245(5) 152.00 2_664 no C39 H39 O12 0.9300 2.5000 3.430(5) 173.00 2_664 no C42 H42 Cl1 0.9300 2.7900 3.663(4) 156.00 . no C44 H44 O5 0.9300 2.3900 3.313(5) 169.00 1_455 no C59 H59 O13 0.9300 2.5700 3.194(5) 125.00 3_465 no #=============================================================================== data_IV _database_code_depnum_ccdc_archive 'CCDC 648555' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H24 N6 Ni), C6 Nb O13, 11(H2 O), Cl' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural '(C30 H24 N6 Ni)2, (C6 Nb O13), 11(H2 O), Cl' _chemical_formula_sum 'C66 H70 Cl N12 Nb Ni2 O24' _chemical_formula_iupac ? _chemical_formula_weight 1661.12 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Nb Nb -2.0727 0.6215 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 23.875(3) _cell_length_b 13.2650(10) _cell_length_c 23.115(2) _cell_angle_alpha 90 _cell_angle_beta 101.690(10) _cell_angle_gamma 90 _cell_volume 7168.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 42694 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 30.55 _cell_special_details ; ? ; _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.802 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.96 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(3) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius-Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 42694 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_sigmaI/netI 0.1526 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 30.55 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 21837 # number of observed reflections (> n sig(I)) _reflns_number_gt 10419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software (Nonius, 1998)' _computing_cell_refinement 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0538P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 21837 _refine_ls_number_parameters 1033 _refine_ls_number_restraints 47 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1674 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.428 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.089 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ni1 Ni Uani 0.08143(2) 0.33909(3) 0.25734(2) 1.000 0.0250(1) . . N1 N Uani 0.07883(11) 0.2089(2) 0.20675(11) 1.000 0.0278(9) . . N2 N Uani 0.14895(11) 0.2569(2) 0.30683(11) 1.000 0.0259(9) . . N3 N Uani 0.13542(12) 0.4159(2) 0.21111(12) 1.000 0.0296(10) . . N4 N Uani 0.09881(11) 0.4706(2) 0.30689(11) 1.000 0.0271(9) . . N5 N Uani 0.00536(11) 0.3950(2) 0.20708(11) 1.000 0.0258(9) . . N6 N Uani 0.02156(11) 0.28367(19) 0.30359(11) 1.000 0.0242(9) . . C1 C Uani 0.04451(15) 0.1916(3) 0.15387(14) 1.000 0.0341(11) . . C2 C Uani 0.04825(16) 0.1067(3) 0.12158(16) 1.000 0.0383(12) . . C3 C Uani 0.08783(16) 0.0350(3) 0.14354(16) 1.000 0.0395(14) . . C4 C Uani 0.12323(15) 0.0502(3) 0.19803(16) 1.000 0.0349(12) . . C5 C Uani 0.11866(14) 0.1389(3) 0.22827(14) 1.000 0.0268(11) . . C6 C Uani 0.15647(14) 0.1642(3) 0.28549(14) 1.000 0.0266(11) . . C7 C Uani 0.19743(15) 0.0989(3) 0.31550(15) 1.000 0.0356(12) . . C8 C Uani 0.23092(16) 0.1281(3) 0.36844(17) 1.000 0.0408(14) . . C9 C Uani 0.22306(15) 0.2217(3) 0.39042(16) 1.000 0.0384(14) . . C10 C Uani 0.18199(14) 0.2842(3) 0.35888(15) 1.000 0.0323(12) . . C11 C Uani 0.15189(16) 0.3847(3) 0.16222(16) 1.000 0.0395(12) . . C12 C Uani 0.18432(17) 0.4419(3) 0.13174(17) 1.000 0.0465(16) . . C13 C Uani 0.20032(17) 0.5375(3) 0.15278(17) 1.000 0.0487(16) . . C14 C Uani 0.18422(16) 0.5704(3) 0.20393(16) 1.000 0.0396(12) . . C15 C Uani 0.15232(14) 0.5077(3) 0.23244(15) 1.000 0.0280(11) . . C16 C Uani 0.13396(14) 0.5371(2) 0.28760(14) 1.000 0.0271(11) . . C17 C Uani 0.15122(15) 0.6251(3) 0.31823(16) 1.000 0.0371(12) . . C18 C Uani 0.13196(17) 0.6454(3) 0.36940(17) 1.000 0.0409(14) . . C19 C Uani 0.09607(16) 0.5782(3) 0.38905(16) 1.000 0.0371(12) . . C20 C Uani 0.08039(15) 0.4921(3) 0.35669(15) 1.000 0.0336(12) . . C21 C Uani -0.00059(15) 0.4476(3) 0.15640(14) 1.000 0.0306(11) . . C22 C Uani -0.05321(15) 0.4686(3) 0.12075(15) 1.000 0.0329(11) . . C23 C Uani -0.10163(15) 0.4379(3) 0.13866(15) 1.000 0.0333(12) . . C24 C Uani -0.09707(15) 0.3862(3) 0.19106(15) 1.000 0.0325(12) . . C25 C Uani -0.04276(14) 0.3645(2) 0.22454(14) 1.000 0.0258(11) . . C26 C Uani -0.03365(14) 0.3067(2) 0.28016(14) 1.000 0.0263(11) . . C27 C Uani -0.07784(15) 0.2790(3) 0.30761(15) 1.000 0.0315(11) . . C28 C Uani -0.06531(16) 0.2267(3) 0.36032(15) 1.000 0.0363(12) . . C29 C Uani -0.00948(16) 0.2026(3) 0.38385(15) 1.000 0.0337(11) . . C30 C Uani 0.03263(15) 0.2312(2) 0.35456(14) 1.000 0.0303(11) . . Ni2 Ni Uani 0.41723(2) 0.24401(3) 0.21521(2) 1.000 0.0271(1) . . N7 N Uani 0.41148(12) 0.3799(2) 0.16966(12) 1.000 0.0292(9) . . N8 N Uani 0.37692(12) 0.3354(2) 0.26844(12) 1.000 0.0338(10) . . N9 N Uani 0.33723(12) 0.1952(2) 0.17039(12) 1.000 0.0309(10) . . N10 N Uani 0.40632(12) 0.1162(2) 0.26367(13) 1.000 0.0341(10) . . N11 N Uani 0.46373(11) 0.1697(2) 0.16123(12) 1.000 0.0275(9) . . N12 N Uani 0.50046(12) 0.2760(2) 0.25887(12) 1.000 0.0269(9) . . C31 C Uani 0.43304(15) 0.3997(3) 0.12175(15) 1.000 0.0360(12) . . C32 C Uani 0.42449(17) 0.4895(3) 0.09173(17) 1.000 0.0459(16) . . C33 C Uani 0.39107(19) 0.5618(3) 0.11165(18) 1.000 0.0543(16) . . C34 C Uani 0.36880(18) 0.5428(3) 0.16071(18) 1.000 0.0475(16) . . C35 C Uani 0.38000(15) 0.4515(3) 0.18986(16) 1.000 0.0330(12) . . C36 C Uani 0.35910(14) 0.4254(3) 0.24393(16) 1.000 0.0318(12) . . C37 C Uani 0.32473(16) 0.4879(3) 0.26942(18) 1.000 0.0445(14) . . C38 C Uani 0.30883(18) 0.4592(3) 0.3206(2) 1.000 0.0531(17) . . C39 C Uani 0.32864(18) 0.3701(4) 0.34701(19) 1.000 0.0526(17) . . C40 C Uani 0.36217(17) 0.3096(3) 0.31959(16) 1.000 0.0441(16) . . C41 C Uani 0.30537(15) 0.2357(3) 0.12136(16) 1.000 0.0383(12) . . C42 C Uani 0.25283(16) 0.1958(3) 0.09408(17) 1.000 0.0467(14) . . C43 C Uani 0.23294(17) 0.1114(4) 0.11746(18) 1.000 0.0530(16) . . C44 C Uani 0.26506(17) 0.0692(3) 0.16791(18) 1.000 0.0480(16) . . C45 C Uani 0.31682(15) 0.1132(3) 0.19410(16) 1.000 0.0325(12) . . C46 C Uani 0.35392(15) 0.0746(3) 0.24945(16) 1.000 0.0332(12) . . C47 C Uani 0.33567(17) 0.0025(3) 0.28488(18) 1.000 0.0432(14) . . C48 C Uani 0.37199(18) -0.0269(3) 0.33639(18) 1.000 0.0475(16) . . C49 C Uani 0.42523(18) 0.0143(3) 0.35101(18) 1.000 0.0479(17) . . C50 C Uani 0.44065(17) 0.0848(3) 0.31295(18) 1.000 0.0459(16) . . C51 C Uani 0.44322(15) 0.1146(3) 0.11319(15) 1.000 0.0338(12) . . C52 C Uani 0.47714(17) 0.0645(3) 0.08183(16) 1.000 0.0383(14) . . C53 C Uani 0.53548(16) 0.0717(3) 0.09963(16) 1.000 0.0404(12) . . C54 C Uani 0.55774(15) 0.1295(3) 0.14812(15) 1.000 0.0358(12) . . C55 C Uani 0.52116(14) 0.1782(2) 0.17838(14) 1.000 0.0265(11) . . C56 C Uani 0.54134(14) 0.2424(2) 0.23131(14) 1.000 0.0273(11) . . C57 C Uani 0.59830(15) 0.2675(3) 0.25119(15) 1.000 0.0331(12) . . C58 C Uani 0.61352(16) 0.3270(3) 0.30125(16) 1.000 0.0394(12) . . C59 C Uani 0.57225(16) 0.3586(3) 0.33013(16) 1.000 0.0396(12) . . C60 C Uani 0.51632(16) 0.3325(3) 0.30736(15) 1.000 0.0357(12) . . Nb1 Nb Uani 0.33809(1) 0.68712(2) 0.49766(1) 1.000 0.0274(1) . . O1 O Uani 0.32721(10) 0.72690(18) 0.56515(10) 1.000 0.0354(8) . . O2 O Uani 0.42563(10) 0.65697(18) 0.52723(10) 1.000 0.0352(8) . . O3 O Uani 0.38537(10) 0.81482(17) 0.47618(10) 1.000 0.0345(8) . . O4 O Uani 0.51501(11) 0.7140(2) 0.54770(13) 1.000 0.0546(11) . . O5 O Uani 0.47093(12) 0.8778(2) 0.47195(12) 1.000 0.0547(11) . . O6 O Uani 0.25561(10) 0.6140(2) 0.48129(10) 1.000 0.0391(9) . . O7 O Uani 0.35212(10) 0.53124(17) 0.50661(10) 1.000 0.0352(8) . . O8 O Uani 0.20815(12) 0.4692(2) 0.46926(15) 1.000 0.0768(13) . . O9 O Uani 0.31588(12) 0.3758(2) 0.49108(12) 1.000 0.0503(10) . . O10 O Uani 0.27777(10) 0.79315(18) 0.45340(10) 1.000 0.0337(8) . . O11 O Uani 0.33017(10) 0.65812(17) 0.40248(10) 1.000 0.0312(8) . . O12 O Uani 0.23354(11) 0.8557(2) 0.36661(11) 1.000 0.0459(9) . . O13 O Uani 0.29159(10) 0.71495(19) 0.31235(10) 1.000 0.0384(9) . . C61 C Uani 0.46505(16) 0.7225(3) 0.52440(16) 1.000 0.0357(12) . . C62 C Uani 0.44083(16) 0.8148(3) 0.48746(15) 1.000 0.0331(12) . . C63 C Uani 0.25221(16) 0.5178(3) 0.47952(16) 1.000 0.0412(14) . . C64 C Uani 0.31066(16) 0.4663(3) 0.49308(15) 1.000 0.0356(12) . . C65 C Uani 0.26643(14) 0.7974(3) 0.39675(15) 1.000 0.0308(11) . . C66 C Uani 0.29845(14) 0.7178(3) 0.36670(16) 1.000 0.0288(11) . . O17 O Uani 0.12710(13) 0.1408(3) 0.47958(14) 1.000 0.0651(12) . . O18 O Uani 0.12089(16) 0.3459(3) 0.49393(19) 1.000 0.0823(14) . . O19 O Uani 0.00835(14) 0.4138(2) 0.46689(11) 1.000 0.0481(10) . . O20 O Uani 0.03906(16) 0.0692(4) 0.52945(16) 1.000 0.123(2) . . O14 O Uani 0.38809(15) 0.2039(2) 0.4881(2) 1.000 0.0982(16) . . O15 O Uani 0.33017(12) 0.0238(2) 0.46549(15) 1.000 0.0634(12) . . O16 O Uani 0.2318(2) 0.0456(4) 0.5113(2) 1.000 0.115(2) . . O21 O Uani 0.1887(2) 0.8582(4) 0.5136(2) 1.000 0.123(2) . . O22 O Uani 0.1531(2) 0.6108(3) 0.55390(16) 1.000 0.0997(17) . . O23 O Uani 0.21521(11) 0.8562(2) 0.23655(11) 1.000 0.0404(9) . . O24 O Uani 0.24067(15) 0.7866(4) 0.13278(13) 1.000 0.0866(16) . . Cl1 Cl Uani 0.06206(5) 0.76155(9) 0.48422(5) 1.000 0.0602(4) . . H1 H Uiso 0.01710 0.23960 0.13870 1.000 0.0410 calc R H2 H Uiso 0.02410 0.09780 0.08500 1.000 0.0460 calc R H3 H Uiso 0.09100 -0.02330 0.12210 1.000 0.0470 calc R H4 H Uiso 0.14980 0.00140 0.21420 1.000 0.0420 calc R H7 H Uiso 0.20230 0.03560 0.29990 1.000 0.0430 calc R H8 H Uiso 0.25860 0.08480 0.38910 1.000 0.0490 calc R H9 H Uiso 0.24520 0.24280 0.42620 1.000 0.0460 calc R H10 H Uiso 0.17680 0.34770 0.37400 1.000 0.0390 calc R H11 H Uiso 0.14080 0.32060 0.14800 1.000 0.0470 calc R H12 H Uiso 0.19520 0.41710 0.09800 1.000 0.0560 calc R H13 H Uiso 0.22150 0.57900 0.13290 1.000 0.0580 calc R H14 H Uiso 0.19480 0.63420 0.21900 1.000 0.0480 calc R H17 H Uiso 0.17550 0.67000 0.30450 1.000 0.0440 calc R H18 H Uiso 0.14320 0.70420 0.39050 1.000 0.0490 calc R H19 H Uiso 0.08270 0.59070 0.42350 1.000 0.0450 calc R H20 H Uiso 0.05600 0.44680 0.36980 1.000 0.0400 calc R H21 H Uiso 0.03220 0.47080 0.14480 1.000 0.0370 calc R H22 H Uiso -0.05560 0.50310 0.08530 1.000 0.0390 calc R H23 H Uiso -0.13740 0.45180 0.11560 1.000 0.0400 calc R H24 H Uiso -0.12970 0.36600 0.20410 1.000 0.0390 calc R H27 H Uiso -0.11550 0.29540 0.29070 1.000 0.0380 calc R H28 H Uiso -0.09430 0.20820 0.37960 1.000 0.0430 calc R H29 H Uiso -0.00020 0.16720 0.41920 1.000 0.0400 calc R H30 H Uiso 0.07030 0.21370 0.37060 1.000 0.0360 calc R H31 H Uiso 0.45480 0.35030 0.10820 1.000 0.0430 calc R H32 H Uiso 0.44070 0.50140 0.05900 1.000 0.0550 calc R H33 H Uiso 0.38380 0.62290 0.09180 1.000 0.0650 calc R H34 H Uiso 0.34630 0.59090 0.17440 1.000 0.0570 calc R H37 H Uiso 0.31240 0.54920 0.25190 1.000 0.0540 calc R H38 H Uiso 0.28470 0.49990 0.33740 1.000 0.0640 calc R H39 H Uiso 0.31960 0.35080 0.38270 1.000 0.0630 calc R H40 H Uiso 0.37510 0.24860 0.33710 1.000 0.0530 calc R H41 H Uiso 0.31900 0.29250 0.10510 1.000 0.0460 calc R H42 H Uiso 0.23150 0.22590 0.06040 1.000 0.0560 calc R H43 H Uiso 0.19820 0.08290 0.09950 1.000 0.0640 calc R H44 H Uiso 0.25220 0.01180 0.18430 1.000 0.0580 calc R H47 H Uiso 0.29940 -0.02580 0.27410 1.000 0.0520 calc R H48 H Uiso 0.36020 -0.07450 0.36100 1.000 0.0570 calc R H49 H Uiso 0.45040 -0.00430 0.38550 1.000 0.0580 calc R H50 H Uiso 0.47730 0.11180 0.32250 1.000 0.0550 calc R H51 H Uiso 0.40380 0.11020 0.10050 1.000 0.0410 calc R H52 H Uiso 0.46100 0.02620 0.04900 1.000 0.0460 calc R H53 H Uiso 0.55950 0.03790 0.07920 1.000 0.0490 calc R H54 H Uiso 0.59710 0.13590 0.16060 1.000 0.0430 calc R H57 H Uiso 0.62600 0.24470 0.23120 1.000 0.0400 calc R H58 H Uiso 0.65150 0.34510 0.31500 1.000 0.0470 calc R H59 H Uiso 0.58170 0.39680 0.36440 1.000 0.0470 calc R H60 H Uiso 0.48810 0.35530 0.32670 1.000 0.0430 calc R H171 H Uiso 0.1604(8) 0.120(3) 0.4848(19) 1.000 0.0780 . . H172 H Uiso 0.1178(13) 0.138(4) 0.5123(8) 0.500 0.0780 . . H173 H Uiso 0.130(2) 0.2019(19) 0.489(4) 0.500 0.0780 . . H181 H Uiso 0.1396(18) 0.386(3) 0.477(2) 1.000 0.0990 . . H182 H Uiso 0.129(4) 0.2886(18) 0.483(4) 0.500 0.0990 . . H183 H Uiso 0.0866(7) 0.357(7) 0.478(4) 0.500 0.0990 . . H191 H Uiso -0.0094(14) 0.369(2) 0.4817(16) 1.000 0.0580 . . H192 H Uiso 0.0428(6) 0.402(5) 0.482(3) 0.500 0.0580 . . H193 H Uiso 0.010(3) 0.463(3) 0.490(2) 0.500 0.0580 . . H201 H Uiso 0.0126(5) 0.1105(11) 0.5335(12) 1.000 0.1470 . . H202 H Uiso 0.0221(8) 0.0132(9) 0.5258(13) 0.500 0.1470 . . H203 H Uiso 0.062(3) 0.105(3) 0.515(5) 0.500 0.1470 . . H141 H Uiso 0.3709(18) 0.258(2) 0.489(3) 1.000 0.1180 . . H142 H Uiso 0.4203(11) 0.220(4) 0.482(3) 1.000 0.1180 . . H151 H Uiso 0.3523(14) 0.0744(17) 0.473(2) 1.000 0.0760 . . H152 H Uiso 0.3533(13) -0.0255(17) 0.472(2) 1.000 0.0760 . . H161 H Uiso 0.2665(9) 0.043(4) 0.508(3) 1.000 0.1370 . . H162 H Uiso 0.223(2) -0.0162(15) 0.513(3) 1.000 0.1370 . . H211 H Uiso 0.1638(18) 0.811(3) 0.513(3) 1.000 0.1470 . . H212 H Uiso 0.2128(18) 0.829(2) 0.497(3) 1.000 0.1470 . . H221 H Uiso 0.129(2) 0.651(4) 0.5324(18) 1.000 0.1200 . . H222 H Uiso 0.168(2) 0.581(4) 0.5279(16) 1.000 0.1200 . . H231 H Uiso 0.2331(14) 0.822(2) 0.2645(9) 1.000 0.0490 . . H232 H Uiso 0.2269(15) 0.836(3) 0.2069(8) 1.000 0.0490 . . H241 H Uiso 0.2664(13) 0.790(4) 0.1127(17) 1.000 0.1040 . . H242 H Uiso 0.2121(12) 0.812(4) 0.1107(17) 1.000 0.1040 . . 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 Ni1 0.0266(2) 0.0245(2) 0.0237(2) -0.0011(2) 0.0046(2) 0.0002(2) N1 0.0283(16) 0.0301(17) 0.0239(15) -0.0011(13) 0.0026(12) -0.0023(13) N2 0.0249(15) 0.0266(16) 0.0252(15) -0.0039(13) 0.0030(12) -0.0022(13) N3 0.0293(17) 0.0354(18) 0.0246(15) 0.0003(13) 0.0064(13) 0.0003(14) N4 0.0288(16) 0.0264(16) 0.0265(16) -0.0016(13) 0.0068(13) 0.0003(13) N5 0.0294(16) 0.0246(15) 0.0229(15) 0.0003(12) 0.0043(12) 0.0021(13) N6 0.0286(16) 0.0199(14) 0.0235(15) -0.0022(12) 0.0037(12) -0.0009(12) C1 0.035(2) 0.037(2) 0.0274(19) -0.0022(17) -0.0003(16) 0.0050(17) C2 0.044(2) 0.042(2) 0.028(2) -0.0121(18) 0.0049(17) -0.006(2) C3 0.051(3) 0.031(2) 0.037(2) -0.0129(18) 0.0098(19) -0.0008(19) C4 0.037(2) 0.028(2) 0.040(2) -0.0031(17) 0.0084(18) 0.0050(17) C5 0.0237(19) 0.0265(19) 0.0310(19) 0.0012(15) 0.0072(15) 0.0002(15) C6 0.0243(18) 0.0270(19) 0.0293(18) 0.0013(16) 0.0075(15) 0.0003(15) C7 0.035(2) 0.034(2) 0.038(2) 0.0030(18) 0.0082(18) 0.0060(17) C8 0.031(2) 0.049(3) 0.041(2) 0.008(2) 0.0039(18) 0.0085(19) C9 0.032(2) 0.052(3) 0.029(2) 0.0051(19) 0.0011(17) -0.0055(19) C10 0.029(2) 0.035(2) 0.032(2) -0.0035(17) 0.0040(16) -0.0034(17) C11 0.040(2) 0.046(2) 0.035(2) -0.0085(19) 0.0138(18) -0.0013(19) C12 0.048(3) 0.065(3) 0.031(2) 0.006(2) 0.0187(19) 0.003(2) C13 0.042(2) 0.062(3) 0.046(3) 0.011(2) 0.018(2) -0.007(2) C14 0.040(2) 0.038(2) 0.041(2) 0.0045(19) 0.0085(19) -0.0067(19) C15 0.0243(18) 0.029(2) 0.0310(19) 0.0066(16) 0.0061(15) 0.0027(16) C16 0.0246(19) 0.0247(19) 0.0305(19) 0.0016(16) 0.0020(15) 0.0008(15) C17 0.038(2) 0.028(2) 0.044(2) -0.0017(18) 0.0056(18) -0.0077(17) C18 0.047(3) 0.029(2) 0.042(2) -0.0097(18) -0.002(2) -0.0007(19) C19 0.042(2) 0.037(2) 0.032(2) -0.0083(18) 0.0067(18) 0.0044(19) C20 0.036(2) 0.033(2) 0.033(2) -0.0008(17) 0.0102(17) 0.0006(17) C21 0.038(2) 0.028(2) 0.0279(19) 0.0013(16) 0.0115(16) 0.0003(17) C22 0.044(2) 0.030(2) 0.0234(18) 0.0063(16) 0.0035(17) 0.0062(17) C23 0.032(2) 0.036(2) 0.028(2) 0.0018(17) -0.0028(16) 0.0034(17) C24 0.032(2) 0.033(2) 0.032(2) -0.0020(17) 0.0055(16) -0.0002(17) C25 0.031(2) 0.0234(18) 0.0237(18) -0.0028(14) 0.0070(15) -0.0015(15) C26 0.032(2) 0.0221(18) 0.0243(17) -0.0042(15) 0.0043(15) -0.0011(16) C27 0.0265(19) 0.039(2) 0.0292(19) 0.0018(17) 0.0061(16) -0.0035(16) C28 0.038(2) 0.040(2) 0.034(2) 0.0008(18) 0.0150(18) -0.0087(18) C29 0.046(2) 0.028(2) 0.0280(19) 0.0007(16) 0.0100(17) 0.0004(18) C30 0.032(2) 0.0266(19) 0.031(2) 0.0020(16) 0.0035(16) 0.0028(16) Ni2 0.0257(2) 0.0255(2) 0.0304(2) 0.0026(2) 0.0067(2) 0.0006(2) N7 0.0289(16) 0.0273(16) 0.0303(16) 0.0021(13) 0.0035(13) -0.0009(13) N8 0.0305(17) 0.0381(19) 0.0340(17) -0.0018(15) 0.0091(14) -0.0011(14) N9 0.0270(16) 0.0325(18) 0.0335(17) -0.0025(14) 0.0066(13) 0.0016(14) N10 0.0285(17) 0.0340(18) 0.0406(18) 0.0063(15) 0.0088(14) 0.0004(14) N11 0.0251(16) 0.0232(16) 0.0333(16) -0.0016(13) 0.0037(13) -0.0036(13) N12 0.0285(16) 0.0282(16) 0.0243(15) 0.0030(13) 0.0063(13) 0.0016(13) C31 0.036(2) 0.035(2) 0.037(2) 0.0054(18) 0.0072(17) -0.0019(18) C32 0.055(3) 0.041(3) 0.041(2) 0.013(2) 0.008(2) -0.003(2) C33 0.074(3) 0.036(2) 0.048(3) 0.014(2) 0.001(2) 0.009(2) C34 0.057(3) 0.037(2) 0.047(3) -0.001(2) 0.007(2) 0.013(2) C35 0.031(2) 0.027(2) 0.039(2) -0.0016(17) 0.0025(17) 0.0024(17) C36 0.026(2) 0.027(2) 0.041(2) -0.0041(17) 0.0036(17) -0.0009(16) C37 0.039(2) 0.038(2) 0.057(3) -0.013(2) 0.011(2) 0.0040(19) C38 0.047(3) 0.051(3) 0.067(3) -0.028(2) 0.025(2) -0.004(2) C39 0.054(3) 0.065(3) 0.046(3) -0.012(2) 0.027(2) -0.014(2) C40 0.050(3) 0.048(3) 0.039(2) 0.001(2) 0.020(2) -0.001(2) C41 0.033(2) 0.040(2) 0.041(2) -0.0015(19) 0.0055(18) 0.0004(18) C42 0.034(2) 0.065(3) 0.038(2) -0.002(2) -0.0001(18) 0.001(2) C43 0.035(2) 0.077(3) 0.047(3) -0.010(2) 0.008(2) -0.017(2) C44 0.041(2) 0.052(3) 0.054(3) -0.004(2) 0.017(2) -0.019(2) C45 0.027(2) 0.034(2) 0.040(2) -0.0037(18) 0.0154(17) -0.0040(17) C46 0.036(2) 0.026(2) 0.041(2) -0.0023(17) 0.0159(18) 0.0014(17) C47 0.044(2) 0.033(2) 0.058(3) -0.002(2) 0.023(2) -0.0055(19) C48 0.060(3) 0.033(2) 0.056(3) 0.013(2) 0.027(2) 0.002(2) C49 0.045(3) 0.047(3) 0.053(3) 0.025(2) 0.013(2) 0.006(2) C50 0.034(2) 0.044(3) 0.059(3) 0.018(2) 0.008(2) 0.0001(19) C51 0.029(2) 0.035(2) 0.037(2) -0.0027(18) 0.0059(17) -0.0058(17) C52 0.051(3) 0.032(2) 0.033(2) -0.0063(17) 0.0114(19) -0.0036(19) C53 0.042(2) 0.043(2) 0.041(2) -0.0074(19) 0.0200(19) 0.0018(19) C54 0.028(2) 0.043(2) 0.038(2) 0.0027(18) 0.0103(17) 0.0018(17) C55 0.0267(19) 0.0251(19) 0.0287(18) 0.0067(15) 0.0081(15) 0.0005(15) C56 0.0292(19) 0.0284(19) 0.0237(18) 0.0071(15) 0.0038(15) -0.0019(16) C57 0.028(2) 0.040(2) 0.031(2) 0.0073(17) 0.0052(16) -0.0006(17) C58 0.032(2) 0.044(2) 0.038(2) 0.0078(19) -0.0027(18) -0.0064(19) C59 0.043(2) 0.038(2) 0.033(2) -0.0016(18) -0.0036(19) -0.0049(19) C60 0.038(2) 0.040(2) 0.029(2) -0.0008(17) 0.0068(17) 0.0035(18) Nb1 0.0257(2) 0.0285(2) 0.0269(2) 0.0000(1) 0.0029(1) 0.0013(1) O1 0.0349(14) 0.0424(15) 0.0283(13) -0.0013(11) 0.0051(11) 0.0024(12) O2 0.0255(13) 0.0311(14) 0.0473(16) 0.0096(12) 0.0035(12) -0.0020(11) O3 0.0329(14) 0.0286(14) 0.0407(14) 0.0060(12) 0.0042(11) 0.0019(12) O4 0.0297(16) 0.0580(19) 0.071(2) 0.0202(16) -0.0018(14) -0.0062(14) O5 0.0493(18) 0.0455(17) 0.071(2) 0.0180(15) 0.0160(15) -0.0090(15) O6 0.0277(14) 0.0432(16) 0.0454(16) 0.0028(13) 0.0052(12) -0.0014(12) O7 0.0323(14) 0.0266(14) 0.0450(15) 0.0041(12) 0.0037(12) -0.0023(11) O8 0.0412(18) 0.070(2) 0.106(3) 0.031(2) -0.0163(18) -0.0278(17) O9 0.065(2) 0.0296(16) 0.0554(18) -0.0005(14) 0.0104(15) -0.0109(14) O10 0.0330(14) 0.0379(15) 0.0293(14) -0.0014(11) 0.0040(11) 0.0102(11) O11 0.0319(14) 0.0325(14) 0.0288(13) -0.0012(11) 0.0054(11) 0.0087(11) O12 0.0448(17) 0.0499(17) 0.0395(15) 0.0044(13) 0.0003(13) 0.0224(14) O13 0.0420(16) 0.0456(16) 0.0285(14) 0.0038(12) 0.0094(12) 0.0064(13) C61 0.032(2) 0.039(2) 0.036(2) 0.0016(18) 0.0065(18) -0.0024(18) C62 0.040(2) 0.028(2) 0.032(2) 0.0003(17) 0.0089(17) -0.0018(18) C63 0.034(2) 0.052(3) 0.034(2) 0.011(2) -0.0016(18) -0.012(2) C64 0.042(2) 0.038(2) 0.027(2) 0.0037(18) 0.0072(17) -0.005(2) C65 0.0235(19) 0.036(2) 0.033(2) 0.0001(17) 0.0059(16) -0.0040(16) C66 0.0256(19) 0.029(2) 0.031(2) 0.0002(16) 0.0041(16) -0.0040(16) O17 0.062(2) 0.072(2) 0.061(2) -0.0043(19) 0.0115(17) -0.0015(18) O18 0.063(2) 0.069(2) 0.119(3) 0.005(2) 0.028(2) -0.016(2) O19 0.068(2) 0.0399(17) 0.0324(16) 0.0051(13) 0.0009(15) -0.0032(16) O20 0.089(3) 0.234(5) 0.050(2) -0.003(3) 0.026(2) -0.050(3) O14 0.056(2) 0.054(2) 0.195(4) 0.020(3) 0.050(3) -0.0031(18) O15 0.051(2) 0.053(2) 0.079(2) 0.0038(19) -0.0035(18) 0.0067(15) O16 0.122(4) 0.143(4) 0.099(3) 0.031(3) 0.070(3) 0.060(3) O21 0.095(4) 0.187(5) 0.096(3) -0.032(3) 0.044(3) 0.027(3) O22 0.103(3) 0.098(3) 0.095(3) 0.009(3) 0.013(3) 0.027(2) O23 0.0411(16) 0.0407(16) 0.0375(15) 0.0063(13) 0.0032(13) 0.0063(13) O24 0.055(2) 0.159(4) 0.049(2) -0.011(2) 0.0182(17) -0.005(3) Cl1 0.0729(8) 0.0571(7) 0.0544(7) -0.0031(6) 0.0222(6) 0.0116(6) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O7 2.098(2) . . no Nb1 O10 2.122(2) . . no Nb1 O11 2.203(2) . . no Nb1 O3 2.149(2) . . no Nb1 O1 1.716(2) . . no Nb1 O2 2.102(2) . . no Nb1 O6 2.159(3) . . no Ni1 N4 2.082(3) . . no Ni1 N1 2.079(3) . . no Ni1 N2 2.085(3) . . no Ni1 N3 2.098(3) . . no Ni1 N5 2.084(3) . . no Ni1 N6 2.085(3) . . no Ni2 N7 2.078(3) . . no Ni2 N8 2.095(3) . . no Ni2 N9 2.083(3) . . no Ni2 N10 2.077(3) . . no Ni2 N11 2.079(3) . . no Ni2 N12 2.082(3) . . no O2 C61 1.293(5) . . no O3 C62 1.297(5) . . no O4 C61 1.211(5) . . no O5 C62 1.203(5) . . no O6 C63 1.279(5) . . no O7 C64 1.302(5) . . no O8 C63 1.216(5) . . no O9 C64 1.209(5) . . no O10 C65 1.284(4) . . no O11 C66 1.277(4) . . no O12 C65 1.216(4) . . no O13 C66 1.234(4) . . no O17 H172 0.83(2) . . no O17 H173 0.84(4) . . no O17 H171 0.83(2) . . no O18 H183 0.84(5) . . no O18 H182 0.84(5) . . no O18 H181 0.84(4) . . no N1 C5 1.350(5) . . no N1 C1 1.346(4) . . no N2 C10 1.348(4) . . no N2 C6 1.350(5) . . no N3 C11 1.335(5) . . no N3 C15 1.345(5) . . no N4 C20 1.344(4) . . no N4 C16 1.354(4) . . no N5 C21 1.346(4) . . no N5 C25 1.354(4) . . no N6 C26 1.355(4) . . no N6 C30 1.348(4) . . no O19 H193 0.84(4) . . no O19 H191 0.84(3) . . no O19 H192 0.84(4) . . no N7 C35 1.352(5) . . no N7 C31 1.338(4) . . no N8 C36 1.353(5) . . no N8 C40 1.345(5) . . no N9 C45 1.353(5) . . no N9 C41 1.343(5) . . no N10 C46 1.346(5) . . no N10 C50 1.328(5) . . no N11 C55 1.353(4) . . no N11 C51 1.337(4) . . no N12 C56 1.345(4) . . no N12 C60 1.338(5) . . no O20 H203 0.84(7) . . no O20 H201 0.856(15) . . no O20 H202 0.842(15) . . no O14 H142 0.84(3) . . no O14 H141 0.83(3) . . no O15 H152 0.85(3) . . no O15 H151 0.85(3) . . no O16 H162 0.85(2) . . no O16 H161 0.85(3) . . no C1 C2 1.364(5) . . no C2 C3 1.364(6) . . no C3 C4 1.382(5) . . no C4 C5 1.384(5) . . no C5 C6 1.481(5) . . no C6 C7 1.383(5) . . no C7 C8 1.375(5) . . no C8 C9 1.369(6) . . no C9 C10 1.375(5) . . no C11 C12 1.376(6) . . no C12 C13 1.384(6) . . no C13 C14 1.386(5) . . no C14 C15 1.382(5) . . no C15 C16 1.482(5) . . no C16 C17 1.384(5) . . no C17 C18 1.380(5) . . no C18 C19 1.376(6) . . no C19 C20 1.375(5) . . no C21 C22 1.384(5) . . no C22 C23 1.367(5) . . no C23 C24 1.377(5) . . no C24 C25 1.399(5) . . no C25 C26 1.475(4) . . no C26 C27 1.386(5) . . no C27 C28 1.381(5) . . no C28 C29 1.372(5) . . no C29 C30 1.374(5) . . no C1 H1 0.9293 . . no C2 H2 0.9294 . . no C3 H3 0.9298 . . no C4 H4 0.9301 . . no C7 H7 0.9304 . . no C8 H8 0.9310 . . no C9 H9 0.9298 . . no C10 H10 0.9298 . . no C11 H11 0.9305 . . no C12 H12 0.9306 . . no C13 H13 0.9296 . . no C14 H14 0.9304 . . no C17 H17 0.9306 . . no C18 H18 0.9302 . . no C19 H19 0.9309 . . no C20 H20 0.9293 . . no C21 H21 0.9298 . . no O21 H211 0.86(4) . . no O21 H212 0.85(5) . . no C22 H22 0.9302 . . no C23 H23 0.9290 . . no C24 H24 0.9299 . . no C27 H27 0.9307 . . no C28 H28 0.9289 . . no C29 H29 0.9295 . . no C30 H30 0.9301 . . no C31 C32 1.373(6) . . no C32 C33 1.385(6) . . no C33 C34 1.370(6) . . no C34 C35 1.385(6) . . no C35 C36 1.478(5) . . no C36 C37 1.380(5) . . no C37 C38 1.368(6) . . no C38 C39 1.370(7) . . no C39 C40 1.376(6) . . no C41 C42 1.390(5) . . no C42 C43 1.369(6) . . no C43 C44 1.378(6) . . no C44 C45 1.390(6) . . no C45 C46 1.491(5) . . no C46 C47 1.386(6) . . no C47 C48 1.380(6) . . no C48 C49 1.362(6) . . no C49 C50 1.384(6) . . no C51 C52 1.364(5) . . no C52 C53 1.373(6) . . no C53 C54 1.373(5) . . no C54 C55 1.385(5) . . no C55 C56 1.488(4) . . no C56 C57 1.385(5) . . no C57 C58 1.387(5) . . no C58 C59 1.363(5) . . no C59 C60 1.377(5) . . no O22 H222 0.86(4) . . no O22 H221 0.86(5) . . no C31 H31 0.9292 . . no C32 H32 0.9304 . . no C33 H33 0.9302 . . no C34 H34 0.9299 . . no C37 H37 0.9293 . . no C38 H38 0.9300 . . no C39 H39 0.9300 . . no C40 H40 0.9291 . . no C41 H41 0.9297 . . no C42 H42 0.9296 . . no C43 H43 0.9293 . . no C44 H44 0.9299 . . no C47 H47 0.9303 . . no C48 H48 0.9308 . . no C49 H49 0.9292 . . no C50 H50 0.9297 . . no C51 H51 0.9292 . . no C52 H52 0.9295 . . no C53 H53 0.9288 . . no C54 H54 0.9293 . . no C57 H57 0.9307 . . no C58 H58 0.9296 . . no C59 H59 0.9288 . . no C60 H60 0.9313 . . no C61 C62 1.537(5) . . no C63 C64 1.528(6) . . no C65 C66 1.548(5) . . no O23 H231 0.83(2) . . no O23 H232 0.84(3) . . no O24 H241 0.84(3) . . no O24 H242 0.84(4) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O10 144.70(9) . . . no O2 Nb1 O11 99.79(9) . . . no O3 Nb1 O6 144.79(9) . . . no O3 Nb1 O7 135.96(9) . . . no O3 Nb1 O10 72.73(9) . . . no O3 Nb1 O11 81.36(9) . . . no O6 Nb1 O7 72.31(10) . . . no O6 Nb1 O10 72.98(10) . . . no O6 Nb1 O11 81.71(9) . . . no O7 Nb1 O10 141.26(9) . . . no O7 Nb1 O11 84.61(9) . . . no O10 Nb1 O11 73.85(9) . . . no O1 Nb1 O6 89.81(10) . . . no O1 Nb1 O7 105.30(10) . . . no O1 Nb1 O10 91.23(10) . . . no O1 Nb1 O11 164.44(10) . . . no O2 Nb1 O3 71.99(9) . . . no O2 Nb1 O6 141.56(10) . . . no O2 Nb1 O7 69.64(9) . . . no O1 Nb1 O3 98.69(10) . . . no O1 Nb1 O2 94.97(10) . . . no N1 Ni1 N3 93.92(10) . . . no N1 Ni1 N4 170.10(11) . . . no N1 Ni1 N6 92.87(10) . . . no N2 Ni1 N3 92.69(11) . . . no N1 Ni1 N5 93.37(10) . . . no N1 Ni1 N2 78.81(10) . . . no N4 Ni1 N5 93.59(10) . . . no N4 Ni1 N6 95.41(10) . . . no N5 Ni1 N6 78.51(10) . . . no N3 Ni1 N6 171.33(11) . . . no N2 Ni1 N5 168.92(11) . . . no N2 Ni1 N6 93.92(10) . . . no N2 Ni1 N4 95.19(10) . . . no N3 Ni1 N5 95.70(11) . . . no N3 Ni1 N4 78.39(10) . . . no N7 Ni2 N8 78.73(11) . . . no N11 Ni2 N12 79.30(11) . . . no N8 Ni2 N10 91.88(11) . . . no N8 Ni2 N11 172.52(11) . . . no N7 Ni2 N9 93.31(11) . . . no N7 Ni2 N10 168.11(12) . . . no N7 Ni2 N11 95.49(11) . . . no N7 Ni2 N12 91.57(11) . . . no N8 Ni2 N9 89.31(11) . . . no N10 Ni2 N12 96.70(11) . . . no N9 Ni2 N10 79.16(11) . . . no N9 Ni2 N11 95.82(11) . . . no N8 Ni2 N12 95.99(11) . . . no N10 Ni2 N11 94.43(11) . . . no N9 Ni2 N12 173.41(11) . . . no Nb1 O2 C61 122.8(2) . . . no Nb1 O3 C62 121.1(2) . . . no Nb1 O6 C63 120.3(2) . . . no Nb1 O7 C64 122.0(2) . . . no Nb1 O10 C65 120.2(2) . . . no Nb1 O11 C66 117.3(2) . . . no H171 O17 H172 106(4) . . . no H171 O17 H173 105(5) . . . no H172 O17 H173 80(7) . . . no H181 O18 H182 105(7) . . . no H181 O18 H183 104(6) . . . no H182 O18 H183 107(9) . . . no Ni1 N1 C5 115.2(2) . . . no Ni1 N1 C1 126.5(2) . . . no C1 N1 C5 118.1(3) . . . no Ni1 N2 C6 114.9(2) . . . no Ni1 N2 C10 126.6(2) . . . no C6 N2 C10 118.3(3) . . . no Ni1 N3 C15 115.0(2) . . . no Ni1 N3 C11 126.7(2) . . . no C11 N3 C15 118.2(3) . . . no Ni1 N4 C16 115.6(2) . . . no Ni1 N4 C20 125.9(2) . . . no C16 N4 C20 118.4(3) . . . no C21 N5 C25 117.9(3) . . . no Ni1 N5 C25 115.1(2) . . . no Ni1 N5 C21 126.6(2) . . . no Ni1 N6 C30 126.7(2) . . . no Ni1 N6 C26 115.4(2) . . . no C26 N6 C30 117.9(3) . . . no H191 O19 H192 103(5) . . . no H192 O19 H193 88(6) . . . no H191 O19 H193 105(4) . . . no Ni2 N7 C31 126.3(2) . . . no C31 N7 C35 118.8(3) . . . no Ni2 N7 C35 114.8(2) . . . no Ni2 N8 C40 127.1(2) . . . no Ni2 N8 C36 114.1(2) . . . no C36 N8 C40 118.5(3) . . . no C41 N9 C45 118.4(3) . . . no Ni2 N9 C41 127.0(2) . . . no Ni2 N9 C45 114.7(2) . . . no Ni2 N10 C46 114.5(2) . . . no C46 N10 C50 117.5(3) . . . no Ni2 N10 C50 126.5(3) . . . no Ni2 N11 C55 114.7(2) . . . no C51 N11 C55 117.9(3) . . . no Ni2 N11 C51 127.4(2) . . . no C56 N12 C60 118.2(3) . . . no Ni2 N12 C60 126.9(2) . . . no Ni2 N12 C56 114.6(2) . . . no H201 O20 H203 104(4) . . . no H201 O20 H202 103.0(17) . . . no H202 O20 H203 143(6) . . . no H141 O14 H142 105(5) . . . no H151 O15 H152 103(3) . . . no H161 O16 H162 103(5) . . . no N1 C1 C2 122.8(3) . . . no C1 C2 C3 119.3(3) . . . no C2 C3 C4 119.1(4) . . . no C3 C4 C5 119.2(3) . . . no C4 C5 C6 123.2(3) . . . no N1 C5 C6 115.5(3) . . . no N1 C5 C4 121.4(3) . . . no N2 C6 C7 121.3(3) . . . no N2 C6 C5 115.5(3) . . . no C5 C6 C7 123.2(3) . . . no C6 C7 C8 119.6(4) . . . no C7 C8 C9 119.2(4) . . . no C8 C9 C10 119.1(3) . . . no N2 C10 C9 122.5(3) . . . no N3 C11 C12 123.7(4) . . . no C11 C12 C13 118.0(4) . . . no C12 C13 C14 118.9(4) . . . no C13 C14 C15 119.5(4) . . . no N3 C15 C14 121.6(3) . . . no N3 C15 C16 115.8(3) . . . no C14 C15 C16 122.7(3) . . . no N4 C16 C17 121.4(3) . . . no N4 C16 C15 115.0(3) . . . no C15 C16 C17 123.6(3) . . . no C16 C17 C18 119.1(3) . . . no C17 C18 C19 119.7(4) . . . no C18 C19 C20 118.5(3) . . . no N4 C20 C19 122.8(3) . . . no N5 C21 C22 123.1(3) . . . no C21 C22 C23 118.8(3) . . . no C22 C23 C24 119.6(3) . . . no C23 C24 C25 119.2(3) . . . no C24 C25 C26 123.1(3) . . . no N5 C25 C24 121.4(3) . . . no N5 C25 C26 115.5(3) . . . no N6 C26 C25 115.2(3) . . . no C25 C26 C27 123.1(3) . . . no N6 C26 C27 121.8(3) . . . no C26 C27 C28 119.2(3) . . . no C27 C28 C29 119.1(3) . . . no C28 C29 C30 119.3(3) . . . no N6 C30 C29 122.7(3) . . . no C2 C1 H1 118.58 . . . no N1 C1 H1 118.58 . . . no C3 C2 H2 120.35 . . . no C1 C2 H2 120.36 . . . no C2 C3 H3 120.44 . . . no C4 C3 H3 120.42 . . . no C5 C4 H4 120.39 . . . no C3 C4 H4 120.40 . . . no C6 C7 H7 120.13 . . . no C8 C7 H7 120.23 . . . no C9 C8 H8 120.38 . . . no C7 C8 H8 120.47 . . . no C10 C9 H9 120.39 . . . no C8 C9 H9 120.48 . . . no C9 C10 H10 118.81 . . . no N2 C10 H10 118.72 . . . no N3 C11 H11 118.08 . . . no C12 C11 H11 118.19 . . . no C13 C12 H12 120.96 . . . no C11 C12 H12 121.05 . . . no C14 C13 H13 120.53 . . . no C12 C13 H13 120.53 . . . no C13 C14 H14 120.31 . . . no C15 C14 H14 120.20 . . . no C18 C17 H17 120.42 . . . no C16 C17 H17 120.45 . . . no C17 C18 H18 120.15 . . . no C19 C18 H18 120.20 . . . no C20 C19 H19 120.70 . . . no C18 C19 H19 120.76 . . . no C19 C20 H20 118.64 . . . no N4 C20 H20 118.53 . . . no H211 O21 H212 101(4) . . . no N5 C21 H21 118.42 . . . no C22 C21 H21 118.52 . . . no C21 C22 H22 120.65 . . . no C23 C22 H22 120.59 . . . no C22 C23 H23 120.18 . . . no C24 C23 H23 120.22 . . . no C25 C24 H24 120.33 . . . no C23 C24 H24 120.43 . . . no C28 C27 H27 120.40 . . . no C26 C27 H27 120.39 . . . no C29 C28 H28 120.46 . . . no C27 C28 H28 120.44 . . . no C28 C29 H29 120.38 . . . no C30 C29 H29 120.31 . . . no N6 C30 H30 118.68 . . . no C29 C30 H30 118.65 . . . no N7 C31 C32 123.1(3) . . . no C31 C32 C33 118.0(4) . . . no C32 C33 C34 119.6(4) . . . no C33 C34 C35 119.6(4) . . . no N7 C35 C34 120.8(3) . . . no N7 C35 C36 115.7(3) . . . no C34 C35 C36 123.5(4) . . . no N8 C36 C37 121.0(3) . . . no N8 C36 C35 115.4(3) . . . no C35 C36 C37 123.5(4) . . . no C36 C37 C38 119.7(4) . . . no C37 C38 C39 119.6(4) . . . no C38 C39 C40 118.6(4) . . . no N8 C40 C39 122.5(4) . . . no N9 C41 C42 122.4(3) . . . no C41 C42 C43 119.1(4) . . . no C42 C43 C44 119.2(4) . . . no C43 C44 C45 119.4(4) . . . no N9 C45 C46 115.1(3) . . . no N9 C45 C44 121.5(3) . . . no C44 C45 C46 123.4(4) . . . no N10 C46 C45 115.5(3) . . . no C45 C46 C47 122.7(3) . . . no N10 C46 C47 121.8(3) . . . no C46 C47 C48 119.2(4) . . . no C47 C48 C49 119.5(4) . . . no C48 C49 C50 117.9(4) . . . no N10 C50 C49 124.0(4) . . . no N11 C51 C52 123.4(3) . . . no C51 C52 C53 118.8(3) . . . no C52 C53 C54 119.0(4) . . . no C53 C54 C55 119.6(3) . . . no N11 C55 C54 121.3(3) . . . no N11 C55 C56 115.4(3) . . . no C54 C55 C56 123.4(3) . . . no C55 C56 C57 122.9(3) . . . no N12 C56 C55 115.7(3) . . . no N12 C56 C57 121.4(3) . . . no C56 C57 C58 119.2(3) . . . no C57 C58 C59 119.4(4) . . . no C58 C59 C60 118.5(3) . . . no N12 C60 C59 123.3(3) . . . no H221 O22 H222 102(4) . . . no C32 C31 H31 118.53 . . . no N7 C31 H31 118.40 . . . no C31 C32 H32 120.96 . . . no C33 C32 H32 121.03 . . . no C32 C33 H33 120.13 . . . no C34 C33 H33 120.25 . . . no C33 C34 H34 120.22 . . . no C35 C34 H34 120.15 . . . no C38 C37 H37 120.11 . . . no C36 C37 H37 120.20 . . . no C37 C38 H38 120.24 . . . no C39 C38 H38 120.13 . . . no C38 C39 H39 120.77 . . . no C40 C39 H39 120.63 . . . no C39 C40 H40 118.71 . . . no N8 C40 H40 118.79 . . . no C42 C41 H41 118.88 . . . no N9 C41 H41 118.73 . . . no C43 C42 H42 120.45 . . . no C41 C42 H42 120.49 . . . no C44 C43 H43 120.40 . . . no C42 C43 H43 120.38 . . . no C45 C44 H44 120.29 . . . no C43 C44 H44 120.29 . . . no C46 C47 H47 120.49 . . . no C48 C47 H47 120.35 . . . no C47 C48 H48 120.28 . . . no C49 C48 H48 120.21 . . . no C50 C49 H49 121.05 . . . no C48 C49 H49 121.01 . . . no N10 C50 H50 118.06 . . . no C49 C50 H50 117.92 . . . no C52 C51 H51 118.30 . . . no N11 C51 H51 118.28 . . . no C53 C52 H52 120.67 . . . no C51 C52 H52 120.50 . . . no C54 C53 H53 120.52 . . . no C52 C53 H53 120.48 . . . no C53 C54 H54 120.28 . . . no C55 C54 H54 120.15 . . . no C58 C57 H57 120.45 . . . no C56 C57 H57 120.39 . . . no C59 C58 H58 120.32 . . . no C57 C58 H58 120.32 . . . no C58 C59 H59 120.70 . . . no C60 C59 H59 120.83 . . . no C59 C60 H60 118.35 . . . no N12 C60 H60 118.34 . . . no O2 C61 O4 125.2(4) . . . no O2 C61 C62 111.6(3) . . . no O4 C61 C62 123.2(4) . . . no O5 C62 C61 122.6(3) . . . no O3 C62 O5 126.0(4) . . . no O3 C62 C61 111.5(3) . . . no O6 C63 C64 113.0(3) . . . no O6 C63 O8 125.6(4) . . . no O8 C63 C64 121.4(4) . . . no O7 C64 C63 111.8(3) . . . no O7 C64 O9 126.0(4) . . . no O9 C64 C63 122.2(4) . . . no O10 C65 C66 114.0(3) . . . no O12 C65 C66 119.8(3) . . . no O10 C65 O12 126.2(3) . . . no O13 C66 C65 120.1(3) . . . no O11 C66 O13 125.4(3) . . . no O11 C66 C65 114.5(3) . . . no H231 O23 H232 105(3) . . . no H241 O24 H242 104(4) . . . no 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 O11 Nb1 O2 C61 82.4(3) . . . . no O1 Nb1 O3 C62 95.1(3) . . . . no O2 Nb1 O3 C62 2.7(2) . . . . no O6 Nb1 O3 C62 -162.7(2) . . . . no O7 Nb1 O3 C62 -27.7(3) . . . . no O10 Nb1 O3 C62 -176.3(3) . . . . no O11 Nb1 O3 C62 -100.6(2) . . . . no O1 Nb1 O6 C63 -111.6(3) . . . . no O2 Nb1 O6 C63 -13.8(3) . . . . no O3 Nb1 O6 C63 143.5(2) . . . . no O7 Nb1 O6 C63 -5.4(2) . . . . no O10 Nb1 O6 C63 157.1(3) . . . . no O11 Nb1 O6 C63 81.6(2) . . . . no O1 Nb1 O7 C64 92.4(3) . . . . no O2 Nb1 O7 C64 -177.9(3) . . . . no O3 Nb1 O7 C64 -147.1(2) . . . . no O6 Nb1 O7 C64 7.6(2) . . . . no O10 Nb1 O7 C64 -19.7(3) . . . . no O11 Nb1 O7 C64 -75.4(2) . . . . no O1 Nb1 O10 C65 -178.9(3) . . . . no O2 Nb1 O10 C65 80.8(3) . . . . no O3 Nb1 O10 C65 82.4(3) . . . . no O6 Nb1 O10 C65 -89.4(3) . . . . no O7 Nb1 O10 C65 -62.2(3) . . . . no O11 Nb1 O10 C65 -3.4(2) . . . . no O2 Nb1 O11 C66 -140.0(2) . . . . no O1 Nb1 O2 C61 -92.6(3) . . . . no O3 Nb1 O2 C61 4.9(2) . . . . no O6 Nb1 O2 C61 171.4(2) . . . . no O7 Nb1 O2 C61 162.9(3) . . . . no O10 Nb1 O2 C61 6.6(3) . . . . no O10 Nb1 O11 C66 4.3(2) . . . . no O3 Nb1 O11 C66 -70.1(2) . . . . no O6 Nb1 O11 C66 78.9(2) . . . . no O7 Nb1 O11 C66 151.8(3) . . . . no N2 Ni1 N1 C5 0.1(2) . . . . no N3 Ni1 N1 C1 -83.1(3) . . . . no N3 Ni1 N1 C5 92.1(2) . . . . no N2 Ni1 N1 C1 -175.0(3) . . . . no N1 Ni1 N2 C6 -2.6(2) . . . . no N1 Ni1 N2 C10 -177.4(3) . . . . no N3 Ni1 N2 C6 -96.1(2) . . . . no N5 Ni1 N1 C1 12.9(3) . . . . no N5 Ni1 N1 C5 -172.0(2) . . . . no N6 Ni1 N1 C1 91.5(3) . . . . no N6 Ni1 N1 C5 -93.3(2) . . . . no N6 Ni1 N2 C10 -85.3(3) . . . . no N1 Ni1 N3 C11 7.2(3) . . . . no N1 Ni1 N3 C15 -176.0(2) . . . . no N2 Ni1 N3 C11 86.2(3) . . . . no N2 Ni1 N3 C15 -97.1(2) . . . . no N4 Ni1 N3 C11 -179.1(3) . . . . no N4 Ni1 N3 C15 -2.3(2) . . . . no N5 Ni1 N3 C11 -86.6(3) . . . . no N5 Ni1 N3 C15 90.2(2) . . . . no N2 Ni1 N4 C16 91.3(2) . . . . no N2 Ni1 N4 C20 -85.7(3) . . . . no N3 Ni1 N2 C10 89.1(3) . . . . no N4 Ni1 N2 C6 -174.6(2) . . . . no N4 Ni1 N2 C10 10.5(3) . . . . no N6 Ni1 N2 C6 89.6(2) . . . . no N5 Ni1 N4 C16 -95.5(2) . . . . no N5 Ni1 N4 C20 87.6(3) . . . . no N6 Ni1 N4 C16 -174.3(2) . . . . no N6 Ni1 N4 C20 8.8(3) . . . . no N1 Ni1 N5 C21 -84.3(3) . . . . no N1 Ni1 N5 C25 87.7(2) . . . . no N3 Ni1 N5 C21 10.0(3) . . . . no N3 Ni1 N5 C25 -178.0(2) . . . . no N4 Ni1 N5 C21 88.7(3) . . . . no N4 Ni1 N5 C25 -99.3(2) . . . . no N6 Ni1 N5 C21 -176.5(3) . . . . no N6 Ni1 N5 C25 -4.5(2) . . . . no N1 Ni1 N6 C26 -91.6(2) . . . . no N1 Ni1 N6 C30 90.8(2) . . . . no N2 Ni1 N6 C26 -170.6(2) . . . . no N2 Ni1 N6 C30 11.8(3) . . . . no N4 Ni1 N6 C26 93.8(2) . . . . no N4 Ni1 N6 C30 -83.8(2) . . . . no N5 Ni1 N6 C26 1.3(2) . . . . no N5 Ni1 N6 C30 -176.4(3) . . . . no N3 Ni1 N4 C20 -177.3(3) . . . . no N3 Ni1 N4 C16 -0.4(2) . . . . no N11 Ni2 N7 C35 176.5(2) . . . . no N11 Ni2 N7 C31 0.3(3) . . . . no N7 Ni2 N8 C36 10.3(2) . . . . no N7 Ni2 N8 C40 -177.3(3) . . . . no N9 Ni2 N8 C36 -83.2(2) . . . . no N9 Ni2 N8 C40 89.2(3) . . . . no N10 Ni2 N8 C36 -162.3(2) . . . . no N12 Ni2 N7 C31 79.7(3) . . . . no N12 Ni2 N7 C35 -104.1(3) . . . . no N11 Ni2 N12 C60 178.1(3) . . . . no N12 Ni2 N8 C40 -86.9(3) . . . . no N7 Ni2 N9 C41 12.9(3) . . . . no N7 Ni2 N9 C45 -167.8(2) . . . . no N8 Ni2 N9 C41 91.6(3) . . . . no N8 Ni2 N9 C45 -89.1(3) . . . . no N10 Ni2 N9 C41 -176.4(3) . . . . no N10 Ni2 N9 C45 2.9(2) . . . . no N11 Ni2 N9 C41 -82.9(3) . . . . no N11 Ni2 N9 C45 96.3(3) . . . . no N8 Ni2 N10 C46 80.6(3) . . . . no N8 Ni2 N10 C50 -85.4(3) . . . . no N9 Ni2 N10 C46 -8.3(2) . . . . no N9 Ni2 N10 C50 -174.3(3) . . . . no N11 Ni2 N10 C46 -103.4(3) . . . . no N11 Ni2 N10 C50 90.6(3) . . . . no N8 Ni2 N7 C31 175.5(3) . . . . no N8 Ni2 N7 C35 -8.3(2) . . . . no N9 Ni2 N7 C31 -95.9(3) . . . . no N9 Ni2 N7 C35 80.4(3) . . . . no N9 Ni2 N11 C55 -176.4(2) . . . . no N10 Ni2 N11 C51 82.0(3) . . . . no N10 Ni2 N11 C55 -96.9(2) . . . . no N12 Ni2 N11 C51 178.0(3) . . . . no N12 Ni2 N11 C55 -0.9(2) . . . . no N7 Ni2 N12 C56 -91.0(2) . . . . no N7 Ni2 N12 C60 82.9(3) . . . . no N8 Ni2 N12 C56 -169.8(2) . . . . no N8 Ni2 N12 C60 4.0(3) . . . . no N10 Ni2 N12 C56 97.6(2) . . . . no N10 Ni2 N12 C60 -88.6(3) . . . . no N11 Ni2 N12 C56 4.3(2) . . . . no N12 Ni2 N10 C46 176.9(2) . . . . no N12 Ni2 N10 C50 10.9(3) . . . . no N7 Ni2 N11 C51 -91.4(3) . . . . no N7 Ni2 N11 C55 89.7(2) . . . . no N9 Ni2 N11 C51 2.5(3) . . . . no N12 Ni2 N8 C36 100.7(2) . . . . no N10 Ni2 N8 C40 10.0(3) . . . . no Nb1 O2 C61 O4 169.6(3) . . . . no Nb1 O2 C61 C62 -10.2(4) . . . . no Nb1 O3 C62 O5 172.1(3) . . . . no Nb1 O3 C62 C61 -8.2(4) . . . . no Nb1 O6 C63 O8 -178.1(3) . . . . no Nb1 O6 C63 C64 3.0(4) . . . . no Nb1 O7 C64 O9 171.8(3) . . . . no Nb1 O7 C64 C63 -8.4(4) . . . . no Nb1 O10 C65 C66 2.1(4) . . . . no Nb1 O10 C65 O12 -178.7(3) . . . . no Nb1 O11 C66 O13 176.4(3) . . . . no Nb1 O11 C66 C65 -4.6(4) . . . . no C1 N1 C5 C4 -2.0(5) . . . . no C5 N1 C1 C2 0.2(5) . . . . no C1 N1 C5 C6 177.8(3) . . . . no Ni1 N1 C5 C6 2.2(4) . . . . no Ni1 N1 C1 C2 175.3(3) . . . . no Ni1 N1 C5 C4 -177.6(3) . . . . no Ni1 N2 C10 C9 175.3(3) . . . . no C10 N2 C6 C7 -0.9(5) . . . . no C6 N2 C10 C9 0.6(5) . . . . no Ni1 N2 C6 C5 4.5(4) . . . . no C10 N2 C6 C5 179.8(3) . . . . no Ni1 N2 C6 C7 -176.2(3) . . . . no C11 N3 C15 C16 -178.5(3) . . . . no Ni1 N3 C11 C12 175.4(3) . . . . no C11 N3 C15 C14 2.2(5) . . . . no Ni1 N3 C15 C14 -174.8(3) . . . . no C15 N3 C11 C12 -1.3(5) . . . . no Ni1 N3 C15 C16 4.5(4) . . . . no C16 N4 C20 C19 -0.5(5) . . . . no C20 N4 C16 C15 180.0(3) . . . . no Ni1 N4 C16 C15 2.8(4) . . . . no Ni1 N4 C16 C17 -176.7(3) . . . . no Ni1 N4 C20 C19 176.3(3) . . . . no C20 N4 C16 C17 0.5(5) . . . . no Ni1 N5 C21 C22 169.6(3) . . . . no C25 N5 C21 C22 -2.3(5) . . . . no C21 N5 C25 C26 179.7(3) . . . . no Ni1 N5 C25 C24 -172.4(2) . . . . no C21 N5 C25 C24 0.3(5) . . . . no Ni1 N5 C25 C26 6.9(3) . . . . no C30 N6 C26 C27 0.9(4) . . . . no C30 N6 C26 C25 179.8(2) . . . . no Ni1 N6 C30 C29 176.1(2) . . . . no Ni1 N6 C26 C25 1.9(3) . . . . no Ni1 N6 C26 C27 -176.9(2) . . . . no C26 N6 C30 C29 -1.5(4) . . . . no C35 N7 C31 C32 -0.3(5) . . . . no C31 N7 C35 C36 -178.2(3) . . . . no Ni2 N7 C31 C32 175.8(3) . . . . no C31 N7 C35 C34 1.8(5) . . . . no Ni2 N7 C35 C36 5.2(4) . . . . no Ni2 N7 C35 C34 -174.8(3) . . . . no Ni2 N8 C36 C37 170.6(3) . . . . no C36 N8 C40 C39 1.6(6) . . . . no C40 N8 C36 C37 -2.5(5) . . . . no Ni2 N8 C36 C35 -10.7(4) . . . . no Ni2 N8 C40 C39 -170.5(3) . . . . no C40 N8 C36 C35 176.2(3) . . . . no Ni2 N9 C45 C44 -177.4(3) . . . . no Ni2 N9 C45 C46 2.4(4) . . . . no Ni2 N9 C41 C42 178.6(3) . . . . no C41 N9 C45 C44 1.9(5) . . . . no C41 N9 C45 C46 -178.3(3) . . . . no C45 N9 C41 C42 -0.7(5) . . . . no Ni2 N10 C50 C49 163.9(3) . . . . no C50 N10 C46 C47 0.8(5) . . . . no Ni2 N10 C46 C45 12.0(4) . . . . no C50 N10 C46 C45 179.4(3) . . . . no C46 N10 C50 C49 -1.8(6) . . . . no Ni2 N10 C46 C47 -166.6(3) . . . . no Ni2 N11 C55 C54 177.4(2) . . . . no C51 N11 C55 C56 178.6(3) . . . . no Ni2 N11 C55 C56 -2.4(3) . . . . no Ni2 N11 C51 C52 -176.9(3) . . . . no C55 N11 C51 C52 2.0(5) . . . . no C51 N11 C55 C54 -1.6(5) . . . . no C60 N12 C56 C57 -1.8(5) . . . . no Ni2 N12 C56 C55 -6.8(3) . . . . no C56 N12 C60 C59 0.6(5) . . . . no Ni2 N12 C56 C57 172.6(3) . . . . no C60 N12 C56 C55 178.8(3) . . . . no Ni2 N12 C60 C59 -173.1(3) . . . . no N1 C1 C2 C3 0.8(6) . . . . no C1 C2 C3 C4 0.0(6) . . . . no C2 C3 C4 C5 -1.7(6) . . . . no C3 C4 C5 C6 -177.0(3) . . . . no C3 C4 C5 N1 2.7(5) . . . . no N1 C5 C6 C7 176.3(3) . . . . no C4 C5 C6 N2 175.3(3) . . . . no C4 C5 C6 C7 -4.0(6) . . . . no N1 C5 C6 N2 -4.4(4) . . . . no C5 C6 C7 C8 179.9(3) . . . . no N2 C6 C7 C8 0.7(5) . . . . no C6 C7 C8 C9 -0.1(6) . . . . no C7 C8 C9 C10 -0.2(6) . . . . no C8 C9 C10 N2 0.0(5) . . . . no N3 C11 C12 C13 -0.6(6) . . . . no C11 C12 C13 C14 1.4(6) . . . . no C12 C13 C14 C15 -0.5(6) . . . . no C13 C14 C15 C16 179.4(3) . . . . no C13 C14 C15 N3 -1.4(6) . . . . no N3 C15 C16 N4 -4.8(4) . . . . no N3 C15 C16 C17 174.7(3) . . . . no C14 C15 C16 C17 -6.1(5) . . . . no C14 C15 C16 N4 174.5(3) . . . . no C15 C16 C17 C18 -179.7(3) . . . . no N4 C16 C17 C18 -0.2(5) . . . . no C16 C17 C18 C19 0.0(6) . . . . no C17 C18 C19 C20 0.0(6) . . . . no C18 C19 C20 N4 0.3(6) . . . . no N5 C21 C22 C23 2.5(6) . . . . no C21 C22 C23 C24 -0.7(6) . . . . no C22 C23 C24 C25 -1.1(6) . . . . no C23 C24 C25 C26 -177.9(3) . . . . no C23 C24 C25 N5 1.3(5) . . . . no N5 C25 C26 C27 173.0(3) . . . . no C24 C25 C26 C27 -7.7(5) . . . . no N5 C25 C26 N6 -5.9(4) . . . . no C24 C25 C26 N6 173.4(3) . . . . no C25 C26 C27 C28 -178.6(3) . . . . no N6 C26 C27 C28 0.1(5) . . . . no C26 C27 C28 C29 -0.7(6) . . . . no C27 C28 C29 C30 0.2(6) . . . . no C28 C29 C30 N6 1.0(5) . . . . no N7 C31 C32 C33 -1.2(6) . . . . no C31 C32 C33 C34 1.3(6) . . . . no C32 C33 C34 C35 0.0(6) . . . . no C33 C34 C35 N7 -1.6(6) . . . . no C33 C34 C35 C36 178.4(4) . . . . no C34 C35 C36 C37 2.4(6) . . . . no N7 C35 C36 N8 3.7(5) . . . . no C34 C35 C36 N8 -176.3(4) . . . . no N7 C35 C36 C37 -177.6(3) . . . . no N8 C36 C37 C38 0.7(6) . . . . no C35 C36 C37 C38 -177.9(4) . . . . no C36 C37 C38 C39 2.0(6) . . . . no C37 C38 C39 C40 -2.9(7) . . . . no C38 C39 C40 N8 1.1(6) . . . . no N9 C41 C42 C43 -0.8(6) . . . . no C41 C42 C43 C44 1.0(6) . . . . no C42 C43 C44 C45 0.2(6) . . . . no C43 C44 C45 C46 178.5(4) . . . . no C43 C44 C45 N9 -1.7(6) . . . . no C44 C45 C46 N10 170.1(4) . . . . no N9 C45 C46 C47 169.0(4) . . . . no C44 C45 C46 C47 -11.3(6) . . . . no N9 C45 C46 N10 -9.6(5) . . . . no N10 C46 C47 C48 0.5(6) . . . . no C45 C46 C47 C48 -178.0(4) . . . . no C46 C47 C48 C49 -0.9(6) . . . . no C47 C48 C49 C50 0.0(6) . . . . no C48 C49 C50 N10 1.4(6) . . . . no N11 C51 C52 C53 -1.0(6) . . . . no C51 C52 C53 C54 -0.4(6) . . . . no C52 C53 C54 C55 0.7(6) . . . . no C53 C54 C55 C56 -180.0(3) . . . . no C53 C54 C55 N11 0.2(5) . . . . no N11 C55 C56 N12 6.2(4) . . . . no N11 C55 C56 C57 -173.2(3) . . . . no C54 C55 C56 N12 -173.7(3) . . . . no C54 C55 C56 C57 7.0(5) . . . . no C55 C56 C57 C58 -179.4(3) . . . . no N12 C56 C57 C58 1.2(5) . . . . no C56 C57 C58 C59 0.7(6) . . . . no C57 C58 C59 C60 -1.9(6) . . . . no C58 C59 C60 N12 1.3(6) . . . . no O4 C61 C62 O5 11.2(6) . . . . no O2 C61 C62 O3 11.3(4) . . . . no O4 C61 C62 O3 -168.5(3) . . . . no O2 C61 C62 O5 -169.0(3) . . . . no O8 C63 C64 O7 -175.8(3) . . . . no O8 C63 C64 O9 4.1(6) . . . . no O6 C63 C64 O9 -176.9(3) . . . . no O6 C63 C64 O7 3.2(4) . . . . no O10 C65 C66 O13 -179.2(3) . . . . no O12 C65 C66 O11 -177.5(3) . . . . no O12 C65 C66 O13 1.6(5) . . . . no O10 C65 C66 O11 1.7(5) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O14 H141 O9 0.83(3) 2.05(4) 2.868(4) 170(4) . no O14 H142 O4 0.84(3) 2.01(4) 2.828(5) 164(6) 3_666 no O15 H151 O14 0.85(3) 1.92(3) 2.757(4) 168(3) . no O15 H152 O3 0.85(3) 2.25(2) 3.058(4) 160(3) 1_545 no O16 H161 O15 0.85(3) 1.99(4) 2.780(6) 155(6) . no O16 H162 O21 0.85(2) 1.86(3) 2.695(7) 168(5) 1_545 no O17 H171 O16 0.83(2) 1.96(3) 2.764(6) 165(4) . no O17 H172 O20 0.83(2) 2.20(4) 2.762(5) 125(3) . no O17 H173 O18 0.84(4) 1.93(3) 2.748(6) 166(8) . no O18 H181 O8 0.84(4) 2.01(4) 2.797(5) 155(4) . no O18 H182 O17 0.84(5) 1.96(3) 2.748(6) 156(8) . no O18 H183 O19 0.84(5) 1.98(4) 2.782(5) 159(7) . no O19 H191 Cl1 0.84(3) 2.37(3) 3.207(3) 176(3) 3_566 no O19 H192 O18 0.84(4) 1.97(3) 2.782(5) 161(7) . no O19 H193 O19 0.84(4) 2.01(5) 2.825(4) 164(7) 3_566 no O20 H201 Cl1 0.856(15) 2.435(15) 3.265(5) 164(2) 3_566 no O20 H202 O20 0.842(15) 2.05(2) 2.770(6) 143(2) 3_556 no O20 H203 O17 0.84(7) 1.96(8) 2.762(5) 160(6) . no O21 H211 Cl1 0.86(4) 2.47(5) 3.227(5) 147(5) . no O21 H212 O10 0.85(5) 2.07(5) 2.899(5) 166(3) . no O22 H221 Cl1 0.86(5) 2.29(5) 3.146(4) 174(4) . no O22 H222 O6 0.86(4) 2.58(5) 3.236(5) 135(4) . no O22 H222 O8 0.86(4) 2.34(5) 3.182(5) 168(5) . no O23 H231 O12 0.83(2) 2.40(2) 2.949(4) 124(2) . no O23 H231 O13 0.83(2) 2.14(3) 2.935(4) 160(2) . no O23 H232 O24 0.84(3) 1.92(2) 2.751(4) 171(3) . no O24 H241 O1 0.84(3) 2.00(3) 2.838(4) 171(5) 4_564 no O24 H242 O22 0.84(4) 2.00(4) 2.829(6) 170(4) 4_564 no C4 H4 O23 0.9300 2.4700 3.383(5) 168.00 1_545 no C8 H8 O15 0.9300 2.3400 3.226(5) 159.00 . no C12 H12 O16 0.9300 2.3900 3.216(6) 147.00 4_554 no C19 H19 Cl1 0.9300 2.7600 3.484(4) 135.00 . no C27 H27 O23 0.9300 2.4700 3.390(5) 169.00 2_545 no C33 H33 O1 0.9300 2.4200 3.267(5) 152.00 4_564 no C39 H39 O9 0.9300 2.5500 3.406(5) 154.00 . no C47 H47 O23 0.9300 2.5600 3.462(5) 164.00 1_545 no C49 H49 O5 0.9300 2.5100 3.324(5) 147.00 1_545 no C52 H52 O2 0.9300 2.5900 3.333(5) 137.00 4_554 no C54 H54 O11 0.9300 2.5000 3.153(4) 127.00 2_645 no C57 H57 O13 0.9300 2.4200 3.335(4) 169.00 2_645 no #=============================================================================== data_V _database_code_depnum_ccdc_archive 'CCDC 648556' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H24 N6 Ni), C6 Nb O13, 12(H2 O), Cl' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural '2(C30 H24 N6 Ni), C6 Nb O13, 12(H2 O), Cl' _chemical_formula_sum 'C66 H72 Cl N12 Nb Ni2 O25' _chemical_formula_iupac ? _chemical_formula_weight 1679.14 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Nb Nb -2.0727 0.6215 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 15.0580(10) _cell_length_b 22.039(2) _cell_length_c 22.398(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7433.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 22608 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 30.49 _cell_special_details ; ? ; _exptl_crystal_description polyhedral _exptl_crystal_colour 'dark pink' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 0.775 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.93 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(3) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius-Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 22608 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 30.49 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 22608 # number of observed reflections (> n sig(I)) _reflns_number_gt 16952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software (Nonius, 1998)' _computing_cell_refinement 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(9) # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ad _refine_ls_number_reflns 22608 _refine_ls_number_parameters 1033 _refine_ls_number_restraints 43 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.487 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.074 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ni1 Ni Uani 0.36274(2) 0.32974(2) -0.00035(2) 1.000 0.0257(1) . . N1 N Uani 0.25272(16) 0.33763(12) 0.05557(11) 1.000 0.0280(7) . . N2 N Uani 0.28761(16) 0.39551(11) -0.04523(11) 1.000 0.0274(7) . . N3 N Uani 0.43981(17) 0.39182(12) 0.04698(11) 1.000 0.0294(7) . . N4 N Uani 0.47262(17) 0.33695(12) -0.05511(11) 1.000 0.0312(8) . . N5 N Uani 0.41404(17) 0.25313(12) 0.04374(11) 1.000 0.0305(8) . . N6 N Uani 0.30240(18) 0.25948(11) -0.04763(12) 1.000 0.0311(8) . . C1 C Uani 0.2417(2) 0.31022(16) 0.10887(15) 1.000 0.0363(10) . . C2 C Uani 0.1685(2) 0.31944(17) 0.14368(16) 1.000 0.0427(11) . . C3 C Uani 0.1021(3) 0.35657(19) 0.12401(17) 1.000 0.0497(12) . . C4 C Uani 0.1116(2) 0.38405(17) 0.06807(17) 1.000 0.0434(11) . . C5 C Uani 0.1879(2) 0.37455(14) 0.03609(14) 1.000 0.0296(8) . . C6 C Uani 0.2065(2) 0.40510(13) -0.02178(14) 1.000 0.0287(8) . . C7 C Uani 0.1445(2) 0.44116(16) -0.05077(15) 1.000 0.0381(10) . . C8 C Uani 0.1670(2) 0.46736(16) -0.10534(15) 1.000 0.0409(10) . . C9 C Uani 0.2501(3) 0.45777(16) -0.12834(16) 1.000 0.0421(11) . . C10 C Uani 0.3080(2) 0.42109(15) -0.09742(14) 1.000 0.0340(9) . . C11 C Uani 0.4202(2) 0.41773(15) 0.09936(14) 1.000 0.0357(10) . . C12 C Uani 0.4776(2) 0.45529(16) 0.12917(16) 1.000 0.0406(11) . . C13 C Uani 0.5578(3) 0.46880(16) 0.10515(17) 1.000 0.0428(11) . . C14 C Uani 0.5795(2) 0.44412(16) 0.04900(17) 1.000 0.0404(11) . . C15 C Uani 0.51848(19) 0.40543(13) 0.02170(14) 1.000 0.0281(8) . . C16 C Uani 0.5371(2) 0.37554(14) -0.03656(14) 1.000 0.0326(9) . . C17 C Uani 0.6142(2) 0.38563(18) -0.06941(17) 1.000 0.0455(11) . . C18 C Uani 0.6255(3) 0.35451(19) -0.12253(18) 1.000 0.0520(12) . . C19 C Uani 0.5594(3) 0.31592(19) -0.14325(17) 1.000 0.0495(11) . . C20 C Uani 0.4841(2) 0.30756(17) -0.10749(15) 1.000 0.0390(10) . . C21 C Uani 0.4727(2) 0.25312(17) 0.08848(16) 1.000 0.0407(11) . . C22 C Uani 0.4981(3) 0.20019(19) 0.11818(18) 1.000 0.0497(14) . . C23 C Uani 0.4597(3) 0.14589(19) 0.10169(17) 1.000 0.0487(12) . . C24 C Uani 0.4000(3) 0.14614(17) 0.05482(17) 1.000 0.0459(11) . . C25 C Uani 0.3793(2) 0.19995(14) 0.02601(14) 1.000 0.0330(9) . . C26 C Uani 0.3176(2) 0.20288(14) -0.02522(15) 1.000 0.0332(9) . . C27 C Uani 0.2805(3) 0.15220(16) -0.05198(17) 1.000 0.0435(11) . . C28 C Uani 0.2279(3) 0.15795(17) -0.10166(17) 1.000 0.0450(11) . . C29 C Uani 0.2123(2) 0.21518(18) -0.12432(16) 1.000 0.0440(11) . . C30 C Uani 0.2501(2) 0.26422(16) -0.09545(15) 1.000 0.0369(10) . . Ni2 Ni Uani 0.36217(2) 0.67103(2) 0.02738(2) 1.000 0.0263(1) . . N7 N Uani 0.47724(17) 0.66452(12) 0.07798(11) 1.000 0.0305(8) . . N8 N Uani 0.43604(17) 0.60902(11) -0.02253(11) 1.000 0.0294(7) . . N9 N Uani 0.29203(17) 0.60479(12) 0.07310(12) 1.000 0.0300(8) . . N10 N Uani 0.24995(18) 0.66269(12) -0.02650(13) 1.000 0.0346(8) . . N11 N Uani 0.30551(18) 0.74292(12) 0.07573(12) 1.000 0.0322(8) . . N12 N Uani 0.41220(19) 0.74621(12) -0.01838(12) 1.000 0.0321(8) . . C31 C Uani 0.4913(2) 0.69061(17) 0.13107(16) 1.000 0.0400(10) . . C32 C Uani 0.5695(3) 0.68275(18) 0.16256(18) 1.000 0.0507(12) . . C33 C Uani 0.6354(3) 0.6478(2) 0.1385(2) 1.000 0.0593(14) . . C34 C Uani 0.6214(3) 0.62026(18) 0.08406(19) 1.000 0.0495(11) . . C35 C Uani 0.5416(2) 0.62959(15) 0.05474(15) 1.000 0.0331(9) . . C36 C Uani 0.5203(2) 0.59995(14) -0.00388(15) 1.000 0.0319(9) . . C37 C Uani 0.5804(3) 0.56708(18) -0.03607(17) 1.000 0.0458(11) . . C38 C Uani 0.5549(3) 0.54169(19) -0.08978(18) 1.000 0.0527(12) . . C39 C Uani 0.4689(3) 0.54785(19) -0.10806(16) 1.000 0.0551(13) . . C40 C Uani 0.4115(3) 0.58266(15) -0.07437(15) 1.000 0.0405(10) . . C41 C Uani 0.3164(2) 0.57885(15) 0.12448(15) 1.000 0.0359(10) . . C42 C Uani 0.2616(3) 0.53725(17) 0.15479(16) 1.000 0.0445(11) . . C43 C Uani 0.1826(3) 0.52179(18) 0.12988(19) 1.000 0.0500(12) . . C44 C Uani 0.1579(3) 0.54757(17) 0.07580(17) 1.000 0.0464(11) . . C45 C Uani 0.2129(2) 0.58988(14) 0.04839(15) 1.000 0.0330(9) . . C46 C Uani 0.1910(2) 0.62114(15) -0.00773(15) 1.000 0.0349(9) . . C47 C Uani 0.1141(3) 0.60940(19) -0.04124(18) 1.000 0.0500(12) . . C48 C Uani 0.1001(3) 0.6387(2) -0.09388(19) 1.000 0.0583(14) . . C49 C Uani 0.1611(3) 0.6803(2) -0.11257(17) 1.000 0.0580(15) . . C50 C Uani 0.2355(3) 0.69168(17) -0.07893(17) 1.000 0.0449(11) . . C51 C Uani 0.2515(2) 0.73830(17) 0.12310(15) 1.000 0.0400(11) . . C52 C Uani 0.2145(3) 0.78808(18) 0.15111(18) 1.000 0.0490(12) . . C53 C Uani 0.2350(3) 0.84542(18) 0.12986(19) 1.000 0.0517(12) . . C54 C Uani 0.2904(3) 0.85073(17) 0.08185(17) 1.000 0.0455(11) . . C55 C Uani 0.3248(2) 0.79891(14) 0.05479(15) 1.000 0.0330(9) . . C56 C Uani 0.3842(2) 0.80038(14) 0.00216(14) 1.000 0.0320(9) . . C57 C Uani 0.4088(3) 0.85386(16) -0.02537(17) 1.000 0.0438(11) . . C58 C Uani 0.4633(3) 0.85121(18) -0.07553(17) 1.000 0.0485(13) . . C59 C Uani 0.4919(3) 0.79608(18) -0.09612(16) 1.000 0.0433(11) . . C60 C Uani 0.4659(2) 0.74508(16) -0.06613(15) 1.000 0.0385(11) . . Nb1 Nb Uani 0.84210(2) 0.48828(1) 0.20084(1) 1.000 0.0296(1) . . O1 O Uani 0.82403(16) 0.41117(10) 0.20347(12) 1.000 0.0433(7) . . O2 O Uani 0.77480(13) 0.50389(12) 0.11920(10) 1.000 0.0367(7) . . O3 O Uani 0.93927(13) 0.48381(12) 0.12901(10) 1.000 0.0357(7) . . O4 O Uani 0.78034(14) 0.51212(12) 0.01992(10) 1.000 0.0399(7) . . O5 O Uani 0.96431(14) 0.49301(12) 0.03082(10) 1.000 0.0383(7) . . O6 O Uani 0.82542(15) 0.49574(11) 0.29530(10) 1.000 0.0423(7) . . O7 O Uani 0.71590(15) 0.52607(12) 0.21685(10) 1.000 0.0419(8) . . O8 O Uani 0.73916(17) 0.52413(15) 0.37050(11) 1.000 0.0515(9) . . O9 O Uani 0.62891(19) 0.57534(14) 0.28184(12) 1.000 0.0549(9) . . O10 O Uani 0.96916(14) 0.48350(11) 0.23893(10) 1.000 0.0358(6) . . O11 O Uani 0.89007(15) 0.58280(10) 0.20503(11) 1.000 0.0389(7) . . O12 O Uani 1.09051(17) 0.53436(14) 0.26777(13) 1.000 0.0557(9) . . O13 O Uani 1.0094(2) 0.63937(13) 0.22358(13) 1.000 0.0598(10) . . C61 C Uani 0.81454(18) 0.50430(14) 0.06856(13) 1.000 0.0288(8) . . C62 C Uani 0.91490(18) 0.49291(13) 0.07492(14) 1.000 0.0285(8) . . C63 C Uani 0.7553(2) 0.51935(17) 0.31800(14) 1.000 0.0364(9) . . C64 C Uani 0.6923(2) 0.54334(16) 0.26946(16) 1.000 0.0379(10) . . C65 C Uani 1.0159(2) 0.53216(17) 0.24575(14) 1.000 0.0370(10) . . C66 C Uani 0.9698(2) 0.59120(16) 0.22363(14) 1.000 0.0382(10) . . O14 O Uani 0.9164(2) 0.29542(15) 0.21127(16) 1.000 0.0678(11) . . O15 O Uani 1.0595(2) 0.30844(14) 0.29222(15) 1.000 0.0600(10) . . O16 O Uani 1.1599(3) 0.4113(2) 0.2759(2) 1.000 0.106(2) . . O17 O Uani 0.8236(2) 0.71028(16) 0.20034(17) 1.000 0.0713(11) . . O18 O Uani 0.7014(2) 0.70206(16) 0.29282(16) 1.000 0.0646(11) . . O19 O Uani 0.4476(2) 0.57107(14) 0.24564(17) 1.000 0.0661(11) . . O20 O Uani 0.4053(3) 0.30217(16) 0.21908(16) 1.000 0.0743(11) . . O21 O Uani 0.5759(3) 0.2825(2) 0.25944(19) 1.000 0.0887(16) . . O22 O Uani 0.65395(19) 0.17418(14) 0.23486(19) 1.000 0.0732(13) . . O23 O Uani 0.8330(2) 0.18283(18) 0.2232(2) 1.000 0.0880(14) . . O24 O Uani 0.5619(4) 0.4192(3) 0.3057(2) 1.000 0.222(4) . . O25 O Uani 0.57041(18) 0.48945(16) 0.40987(12) 1.000 0.0554(9) . . Cl1 Cl Uani 0.36161(10) 0.43566(6) 0.26556(6) 1.000 0.0742(4) . . H1 H Uiso 0.28570 0.28400 0.12250 1.000 0.0440 calc R H2 H Uiso 0.16400 0.30050 0.18070 1.000 0.0510 calc R H3 H Uiso 0.05180 0.36340 0.14720 1.000 0.0600 calc R H4 H Uiso 0.06660 0.40850 0.05280 1.000 0.0520 calc R H7 H Uiso 0.08880 0.44770 -0.03400 1.000 0.0460 calc R H8 H Uiso 0.12610 0.49110 -0.12590 1.000 0.0490 calc R H9 H Uiso 0.26700 0.47570 -0.16420 1.000 0.0510 calc R H10 H Uiso 0.36380 0.41380 -0.11360 1.000 0.0410 calc R H11 H Uiso 0.36510 0.40990 0.11640 1.000 0.0430 calc R H12 H Uiso 0.46150 0.47150 0.16590 1.000 0.0490 calc R H13 H Uiso 0.59760 0.49380 0.12530 1.000 0.0510 calc R H14 H Uiso 0.63320 0.45340 0.03060 1.000 0.0490 calc R H17 H Uiso 0.65720 0.41270 -0.05590 1.000 0.0540 calc R H18 H Uiso 0.67740 0.35950 -0.14440 1.000 0.0620 calc R H19 H Uiso 0.56500 0.29620 -0.17980 1.000 0.0600 calc R H20 H Uiso 0.44030 0.28080 -0.12030 1.000 0.0470 calc R H21 H Uiso 0.49760 0.28980 0.10030 1.000 0.0490 calc R H22 H Uiso 0.54010 0.20150 0.14860 1.000 0.0600 calc R H23 H Uiso 0.47360 0.11010 0.12160 1.000 0.0580 calc R H24 H Uiso 0.37370 0.11010 0.04260 1.000 0.0550 calc R H27 H Uiso 0.29140 0.11390 -0.03610 1.000 0.0520 calc R H28 H Uiso 0.20320 0.12390 -0.11970 1.000 0.0540 calc R H29 H Uiso 0.17740 0.22060 -0.15810 1.000 0.0530 calc R H30 H Uiso 0.23820 0.30280 -0.11020 1.000 0.0440 calc R H31 H Uiso 0.44700 0.71490 0.14740 1.000 0.0480 calc R H32 H Uiso 0.57710 0.70100 0.19960 1.000 0.0610 calc R H33 H Uiso 0.68900 0.64280 0.15850 1.000 0.0710 calc R H34 H Uiso 0.66490 0.59570 0.06720 1.000 0.0590 calc R H37 H Uiso 0.63800 0.56180 -0.02200 1.000 0.0550 calc R H38 H Uiso 0.59570 0.52070 -0.11310 1.000 0.0630 calc R H39 H Uiso 0.44920 0.52890 -0.14270 1.000 0.0660 calc R H40 H Uiso 0.35360 0.58820 -0.08790 1.000 0.0490 calc R H41 H Uiso 0.37140 0.58860 0.14080 1.000 0.0430 calc R H42 H Uiso 0.27910 0.52070 0.19110 1.000 0.0530 calc R H43 H Uiso 0.14540 0.49420 0.14880 1.000 0.0600 calc R H44 H Uiso 0.10450 0.53650 0.05790 1.000 0.0560 calc R H47 H Uiso 0.07260 0.58150 -0.02740 1.000 0.0600 calc R H48 H Uiso 0.04990 0.63050 -0.11670 1.000 0.0700 calc R H49 H Uiso 0.15230 0.70110 -0.14820 1.000 0.0700 calc R H50 H Uiso 0.27680 0.71990 -0.09240 1.000 0.0540 calc R H51 H Uiso 0.23840 0.69990 0.13780 1.000 0.0480 calc R H52 H Uiso 0.17650 0.78320 0.18350 1.000 0.0590 calc R H53 H Uiso 0.21140 0.87980 0.14800 1.000 0.0620 calc R H54 H Uiso 0.30520 0.88890 0.06730 1.000 0.0550 calc R H57 H Uiso 0.38920 0.89100 -0.01070 1.000 0.0520 calc R H58 H Uiso 0.48030 0.88670 -0.09490 1.000 0.0580 calc R H59 H Uiso 0.52800 0.79340 -0.12970 1.000 0.0520 calc R H60 H Uiso 0.48650 0.70770 -0.07950 1.000 0.0460 calc R H141 H Uiso 0.880(3) 0.3228(16) 0.2024(19) 1.000 0.0810 . . H142 H Uiso 0.935(3) 0.304(2) 0.2451(12) 1.000 0.0810 . . H151 H Uiso 1.087(3) 0.2789(11) 0.306(2) 1.000 0.0720 . . H152 H Uiso 1.088(3) 0.3392(10) 0.302(2) 1.000 0.0720 . . H161 H Uiso 1.126(4) 0.435(2) 0.2563(17) 1.000 0.1280 . . H162 H Uiso 1.202(3) 0.406(3) 0.252(2) 1.000 0.1280 . . H171 H Uiso 0.844(3) 0.6749(10) 0.200(2) 1.000 0.0850 . . H172 H Uiso 0.824(4) 0.720(2) 0.2368(8) 1.000 0.0850 . . H181 H Uiso 0.664(2) 0.6743(13) 0.297(2) 1.000 0.0780 . . H182 H Uiso 0.673(2) 0.7325(11) 0.281(2) 1.000 0.0780 . . H191 H Uiso 0.5029(8) 0.5729(19) 0.248(2) 1.000 0.0790 . . H192 H Uiso 0.433(3) 0.5372(11) 0.2595(19) 1.000 0.0790 . . H201 H Uiso 0.378(3) 0.3305(17) 0.2356(18) 1.000 0.0890 . . H202 H Uiso 0.434(2) 0.2860(13) 0.2463(15) 1.000 0.0890 . . H211 H Uiso 0.6076(17) 0.2592(16) 0.2783(14) 1.000 0.1070 . . H212 H Uiso 0.581(4) 0.3169(10) 0.274(3) 1.000 0.1070 . . H221 H Uiso 0.619(2) 0.1453(14) 0.240(3) 1.000 0.0880 . . H222 H Uiso 0.7038(13) 0.1593(18) 0.231(3) 1.000 0.0880 . . H231 H Uiso 0.864(3) 0.2108(12) 0.2075(19) 1.000 0.1060 . . H232 H Uiso 0.864(3) 0.1514(12) 0.219(3) 1.000 0.1060 . . H241 H Uiso 0.52040 0.44370 0.30060 1.000 0.2670 . . H242 H Uiso 0.575(6) 0.422(4) 0.3419(14) 1.000 0.2670 . . H251 H Uiso 0.562(2) 0.5091(18) 0.4418(12) 1.000 0.0670 . . H252 H Uiso 0.6226(13) 0.4997(19) 0.4005(17) 1.000 0.0670 . . 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 Ni1 0.0240(2) 0.0256(2) 0.0276(2) 0.0013(2) 0.0005(1) 0.0002(1) N1 0.0254(12) 0.0296(13) 0.0289(12) 0.0031(10) 0.0010(10) -0.0025(10) N2 0.0252(12) 0.0270(12) 0.0299(12) 0.0030(10) 0.0034(10) -0.0012(10) N3 0.0268(12) 0.0318(13) 0.0295(13) 0.0007(11) 0.0014(10) 0.0007(10) N4 0.0284(12) 0.0348(14) 0.0305(13) -0.0009(11) 0.0026(10) 0.0026(11) N5 0.0272(12) 0.0334(14) 0.0309(13) 0.0042(11) 0.0009(10) 0.0022(10) N6 0.0338(13) 0.0254(13) 0.0341(14) 0.0011(11) -0.0006(11) 0.0004(11) C1 0.0380(17) 0.0371(17) 0.0339(16) 0.0099(14) 0.0007(14) -0.0002(14) C2 0.0441(19) 0.045(2) 0.0391(17) 0.0121(15) 0.0094(15) -0.0024(16) C3 0.044(2) 0.057(2) 0.048(2) 0.0094(18) 0.0221(17) 0.0041(18) C4 0.0353(18) 0.045(2) 0.050(2) 0.0137(16) 0.0087(15) 0.0070(15) C5 0.0282(14) 0.0297(15) 0.0309(15) 0.0030(12) 0.0016(12) -0.0026(12) C6 0.0295(15) 0.0256(14) 0.0310(15) 0.0011(12) -0.0001(12) -0.0006(12) C7 0.0356(17) 0.0401(17) 0.0386(16) 0.0070(14) -0.0023(14) 0.0080(15) C8 0.0421(18) 0.0456(19) 0.0349(16) 0.0091(14) -0.0026(15) 0.0118(15) C9 0.054(2) 0.0373(18) 0.0351(17) 0.0113(15) 0.0042(16) 0.0036(16) C10 0.0325(15) 0.0370(17) 0.0326(16) 0.0054(13) 0.0042(13) -0.0036(13) C11 0.0353(16) 0.0398(18) 0.0321(16) -0.0037(13) 0.0058(13) -0.0052(14) C12 0.048(2) 0.0391(18) 0.0348(17) -0.0066(15) -0.0038(15) -0.0024(16) C13 0.048(2) 0.0343(18) 0.046(2) -0.0083(15) -0.0103(16) -0.0004(15) C14 0.0292(16) 0.0440(19) 0.048(2) -0.0028(16) -0.0027(14) -0.0033(14) C15 0.0247(14) 0.0240(14) 0.0356(15) 0.0011(12) 0.0015(12) 0.0026(11) C16 0.0302(15) 0.0327(16) 0.0348(16) 0.0022(13) 0.0037(13) 0.0064(13) C17 0.0366(18) 0.049(2) 0.051(2) 0.0010(17) 0.0123(16) -0.0031(16) C18 0.044(2) 0.061(2) 0.051(2) 0.0003(19) 0.0257(18) 0.0033(19) C19 0.055(2) 0.053(2) 0.0405(19) 0.0022(17) 0.0176(17) 0.0136(18) C20 0.0394(18) 0.0440(19) 0.0336(17) -0.0078(14) 0.0033(14) 0.0080(15) C21 0.0395(18) 0.044(2) 0.0387(18) 0.0066(15) -0.0083(15) 0.0047(15) C22 0.046(2) 0.059(3) 0.044(2) 0.0123(19) -0.0028(17) 0.0174(19) C23 0.057(2) 0.046(2) 0.043(2) 0.0137(17) 0.0048(17) 0.0162(19) C24 0.059(2) 0.0317(17) 0.047(2) 0.0049(16) 0.0026(18) 0.0051(17) C25 0.0402(17) 0.0267(14) 0.0321(15) 0.0027(12) 0.0044(13) 0.0069(13) C26 0.0361(17) 0.0287(15) 0.0347(16) 0.0003(13) 0.0037(13) 0.0012(12) C27 0.058(2) 0.0255(16) 0.047(2) -0.0032(15) 0.0048(17) -0.0023(15) C28 0.053(2) 0.038(2) 0.0441(19) -0.0119(15) 0.0042(16) -0.0106(16) C29 0.0378(18) 0.055(2) 0.0391(19) -0.0117(17) -0.0014(15) -0.0086(16) C30 0.0388(17) 0.0352(17) 0.0368(17) 0.0000(14) -0.0037(14) -0.0004(14) Ni2 0.0285(2) 0.0250(2) 0.0255(2) -0.0005(1) -0.0016(2) 0.0006(2) N7 0.0323(13) 0.0313(14) 0.0280(12) 0.0015(11) -0.0022(10) -0.0026(11) N8 0.0357(14) 0.0270(12) 0.0254(12) -0.0034(10) -0.0009(10) 0.0047(10) N9 0.0291(13) 0.0297(13) 0.0313(13) 0.0004(11) -0.0004(10) 0.0009(11) N10 0.0356(14) 0.0335(14) 0.0347(13) -0.0021(11) -0.0107(11) 0.0072(11) N11 0.0337(13) 0.0309(14) 0.0319(14) 0.0011(11) 0.0004(11) 0.0010(11) N12 0.0360(14) 0.0282(12) 0.0320(14) -0.0004(11) 0.0020(11) 0.0009(11) C31 0.0406(18) 0.0436(19) 0.0358(17) -0.0038(15) -0.0057(14) -0.0111(15) C32 0.060(2) 0.047(2) 0.045(2) 0.0024(17) -0.0248(18) -0.0089(18) C33 0.051(2) 0.061(2) 0.066(3) 0.007(2) -0.032(2) -0.007(2) C34 0.0395(19) 0.048(2) 0.061(2) 0.0048(18) -0.0132(18) 0.0004(16) C35 0.0290(15) 0.0325(16) 0.0379(17) 0.0049(13) -0.0019(13) -0.0042(13) C36 0.0326(15) 0.0305(15) 0.0327(15) 0.0050(13) 0.0037(13) 0.0041(12) C37 0.0413(19) 0.048(2) 0.048(2) 0.0041(17) 0.0095(16) 0.0121(16) C38 0.060(2) 0.056(2) 0.042(2) -0.0006(18) 0.0184(18) 0.019(2) C39 0.092(3) 0.045(2) 0.0282(17) -0.0108(16) 0.006(2) 0.016(2) C40 0.052(2) 0.0342(17) 0.0353(17) -0.0051(14) -0.0023(15) 0.0112(15) C41 0.0359(17) 0.0350(17) 0.0368(17) 0.0070(14) -0.0019(13) -0.0008(13) C42 0.054(2) 0.0421(19) 0.0373(18) 0.0109(15) 0.0027(16) -0.0039(17) C43 0.050(2) 0.045(2) 0.055(2) 0.0092(18) 0.0144(18) -0.0095(17) C44 0.0381(18) 0.051(2) 0.050(2) -0.0069(17) 0.0037(17) -0.0091(17) C45 0.0294(15) 0.0293(15) 0.0403(17) -0.0057(13) -0.0025(13) -0.0002(12) C46 0.0289(15) 0.0379(17) 0.0380(17) -0.0048(14) -0.0035(13) 0.0038(13) C47 0.039(2) 0.053(2) 0.058(2) -0.0104(19) -0.0131(17) 0.0002(17) C48 0.054(2) 0.068(3) 0.053(2) -0.013(2) -0.029(2) 0.008(2) C49 0.073(3) 0.061(3) 0.0399(19) -0.0034(18) -0.026(2) 0.025(2) C50 0.052(2) 0.0399(19) 0.0428(19) 0.0038(16) -0.0114(17) 0.0062(16) C51 0.0456(19) 0.0387(18) 0.0356(18) -0.0017(14) 0.0089(15) 0.0027(15) C52 0.047(2) 0.053(2) 0.047(2) -0.0122(18) 0.0120(17) 0.0070(18) C53 0.059(2) 0.041(2) 0.055(2) -0.0099(18) 0.011(2) 0.0134(18) C54 0.052(2) 0.0336(17) 0.051(2) -0.0084(16) 0.0018(18) 0.0043(16) C55 0.0322(16) 0.0300(15) 0.0368(16) -0.0021(13) -0.0038(13) 0.0039(12) C56 0.0366(16) 0.0293(15) 0.0302(14) 0.0004(12) -0.0056(13) -0.0003(12) C57 0.058(2) 0.0286(16) 0.0447(19) 0.0018(15) -0.0029(18) -0.0048(16) C58 0.068(3) 0.0376(19) 0.0398(19) 0.0101(16) 0.0011(18) -0.0104(18) C59 0.045(2) 0.049(2) 0.0358(18) 0.0054(16) 0.0057(15) -0.0021(17) C60 0.048(2) 0.0363(18) 0.0313(17) 0.0023(14) 0.0029(14) 0.0057(15) Nb1 0.0247(1) 0.0354(1) 0.0286(1) 0.0019(1) -0.0031(1) 0.0034(1) O1 0.0435(13) 0.0366(12) 0.0497(13) 0.0054(11) -0.0082(12) -0.0030(10) O2 0.0236(9) 0.0583(16) 0.0281(10) 0.0023(10) -0.0012(8) 0.0055(10) O3 0.0234(10) 0.0516(13) 0.0320(11) -0.0012(11) -0.0036(8) 0.0062(10) O4 0.0287(10) 0.0576(14) 0.0335(11) 0.0029(12) -0.0063(9) 0.0027(11) O5 0.0274(10) 0.0531(14) 0.0344(11) -0.0002(11) 0.0017(9) 0.0049(10) O6 0.0378(11) 0.0608(16) 0.0283(10) 0.0109(11) -0.0043(9) 0.0075(11) O7 0.0305(11) 0.0651(17) 0.0302(11) 0.0021(11) -0.0019(9) 0.0092(11) O8 0.0398(13) 0.083(2) 0.0316(12) -0.0035(13) 0.0007(11) -0.0050(13) O9 0.0472(15) 0.0722(19) 0.0452(14) -0.0066(13) 0.0032(12) 0.0201(14) O10 0.0304(10) 0.0403(12) 0.0368(11) 0.0042(10) -0.0048(9) 0.0051(10) O11 0.0422(13) 0.0341(11) 0.0403(12) 0.0021(10) -0.0069(11) 0.0017(9) O12 0.0339(13) 0.086(2) 0.0473(15) 0.0125(14) -0.0133(12) -0.0119(13) O13 0.0704(19) 0.0506(16) 0.0584(17) 0.0106(14) -0.0222(15) -0.0230(14) C61 0.0252(12) 0.0304(16) 0.0308(15) -0.0014(12) -0.0009(11) 0.0011(11) C62 0.0242(12) 0.0260(14) 0.0353(15) -0.0036(12) -0.0004(12) 0.0003(11) C63 0.0308(15) 0.0471(19) 0.0313(15) 0.0027(14) -0.0011(12) -0.0049(14) C64 0.0299(15) 0.0452(19) 0.0385(17) 0.0018(15) -0.0010(14) -0.0002(14) C65 0.0315(16) 0.056(2) 0.0235(14) 0.0074(14) -0.0024(12) -0.0016(15) C66 0.0451(19) 0.0443(19) 0.0253(15) 0.0019(14) -0.0048(14) -0.0043(15) O14 0.074(2) 0.0575(18) 0.072(2) -0.0002(17) 0.0044(18) 0.0227(16) O15 0.0665(19) 0.0530(16) 0.0606(19) 0.0122(16) 0.0012(15) -0.0031(14) O16 0.072(3) 0.082(3) 0.165(5) -0.002(3) 0.032(3) 0.013(2) O17 0.0589(19) 0.065(2) 0.090(2) -0.0078(19) 0.000(2) 0.0116(15) O18 0.0584(18) 0.071(2) 0.0643(19) -0.0063(18) -0.0175(16) -0.0009(15) O19 0.0583(18) 0.0539(17) 0.086(2) 0.0056(17) -0.0197(18) 0.0042(15) O20 0.083(2) 0.0578(19) 0.082(2) -0.0122(18) -0.0157(19) 0.0175(18) O21 0.072(2) 0.097(3) 0.097(3) -0.021(2) -0.001(2) 0.014(2) O22 0.0370(14) 0.0645(19) 0.118(3) 0.032(2) -0.0028(18) -0.0072(15) O23 0.057(2) 0.079(2) 0.128(3) 0.021(2) -0.010(2) 0.0208(18) O24 0.263(8) 0.322(10) 0.082(4) -0.064(5) 0.027(4) -0.201(8) O25 0.0461(14) 0.080(2) 0.0401(14) -0.0077(15) 0.0065(12) -0.0121(15) Cl1 0.0861(9) 0.0689(7) 0.0675(7) 0.0043(6) 0.0092(7) 0.0132(7) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O7 2.106(2) . . no Nb1 O10 2.098(2) . . no Nb1 O11 2.207(2) . . no Nb1 O3 2.177(2) . . no Nb1 O1 1.722(2) . . no Nb1 O2 2.119(2) . . no Nb1 O6 2.137(2) . . no Ni1 N4 2.066(3) . . no Ni1 N1 2.084(2) . . no Ni1 N2 2.096(2) . . no Ni1 N3 2.084(3) . . no Ni1 N5 2.103(3) . . no Ni1 N6 2.084(3) . . no Ni2 N7 2.075(3) . . no Ni2 N8 2.087(3) . . no Ni2 N9 2.073(3) . . no Ni2 N10 2.085(3) . . no Ni2 N11 2.100(3) . . no Ni2 N12 2.089(3) . . no O2 C61 1.282(4) . . no O3 C62 1.282(4) . . no O4 C61 1.217(4) . . no O5 C62 1.237(4) . . no O6 C63 1.282(4) . . no O7 C64 1.288(4) . . no O8 C63 1.205(4) . . no O9 C64 1.219(4) . . no O10 C65 1.292(4) . . no O11 C66 1.284(4) . . no O12 C65 1.228(4) . . no O13 C66 1.218(4) . . no O14 H142 0.83(3) . . no O14 H141 0.84(4) . . no O15 H151 0.83(3) . . no O15 H152 0.83(3) . . no N1 C5 1.344(4) . . no N1 C1 1.348(4) . . no N2 C10 1.334(4) . . no N2 C6 1.346(4) . . no N3 C15 1.347(4) . . no N3 C11 1.338(4) . . no N4 C20 1.351(4) . . no N4 C16 1.356(4) . . no N5 C21 1.336(4) . . no N5 C25 1.344(4) . . no N6 C30 1.334(4) . . no N6 C26 1.364(4) . . no O16 H161 0.85(5) . . no O16 H162 0.84(5) . . no N7 C35 1.343(4) . . no N7 C31 1.338(4) . . no N8 C40 1.350(4) . . no N8 C36 1.351(4) . . no N9 C41 1.336(4) . . no N9 C45 1.354(4) . . no N10 C50 1.355(5) . . no N10 C46 1.343(4) . . no N11 C55 1.352(4) . . no N11 C51 1.341(4) . . no N12 C60 1.341(4) . . no N12 C56 1.347(4) . . no O17 H171 0.84(3) . . no O17 H172 0.84(2) . . no O18 H182 0.84(3) . . no O18 H181 0.84(3) . . no O19 H192 0.84(3) . . no O19 H191 0.835(13) . . no O20 H202 0.83(3) . . no O20 H201 0.83(4) . . no C1 C2 1.365(5) . . no C2 C3 1.365(5) . . no C3 C4 1.399(5) . . no C4 C5 1.370(4) . . no C5 C6 1.487(4) . . no C6 C7 1.387(4) . . no C7 C8 1.394(5) . . no C8 C9 1.370(5) . . no C9 C10 1.376(5) . . no C11 C12 1.370(5) . . no C12 C13 1.355(5) . . no C13 C14 1.409(5) . . no C14 C15 1.395(4) . . no C15 C16 1.488(4) . . no C16 C17 1.392(4) . . no C17 C18 1.384(6) . . no C18 C19 1.389(6) . . no C19 C20 1.400(5) . . no C21 C22 1.396(6) . . no C22 C23 1.380(6) . . no C23 C24 1.382(6) . . no C24 C25 1.386(5) . . no C25 C26 1.478(4) . . no C26 C27 1.385(5) . . no C27 C28 1.372(6) . . no C28 C29 1.380(5) . . no C29 C30 1.382(5) . . no C1 H1 0.9306 . . no C2 H2 0.9308 . . no C3 H3 0.9307 . . no C4 H4 0.9309 . . no C7 H7 0.9302 . . no C8 H8 0.9301 . . no C9 H9 0.9306 . . no C10 H10 0.9291 . . no C11 H11 0.9294 . . no C12 H12 0.9291 . . no C13 H13 0.9308 . . no C14 H14 0.9303 . . no C17 H17 0.9310 . . no C18 H18 0.9289 . . no C19 H19 0.9307 . . no C20 H20 0.9301 . . no C21 H21 0.9296 . . no O21 H212 0.83(4) . . no O21 H211 0.82(3) . . no C22 H22 0.9301 . . no C23 H23 0.9300 . . no C24 H24 0.9288 . . no C27 H27 0.9306 . . no C28 H28 0.9299 . . no C29 H29 0.9289 . . no C30 H30 0.9296 . . no C31 C32 1.384(5) . . no C32 C33 1.367(6) . . no C33 C34 1.378(6) . . no C34 C35 1.385(5) . . no C35 C36 1.501(5) . . no C36 C37 1.365(5) . . no C37 C38 1.381(6) . . no C38 C39 1.365(6) . . no C39 C40 1.380(6) . . no C41 C42 1.408(5) . . no C42 C43 1.357(6) . . no C43 C44 1.389(6) . . no C44 C45 1.390(5) . . no C45 C46 1.471(5) . . no C46 C47 1.404(5) . . no C47 C48 1.361(6) . . no C48 C49 1.364(6) . . no C49 C50 1.373(6) . . no C51 C52 1.381(5) . . no C52 C53 1.385(6) . . no C53 C54 1.366(6) . . no C54 C55 1.393(5) . . no C55 C56 1.480(4) . . no C56 C57 1.381(5) . . no C57 C58 1.393(6) . . no C58 C59 1.369(6) . . no C59 C60 1.367(5) . . no O22 H221 0.83(3) . . no O22 H222 0.82(2) . . no C31 H31 0.9302 . . no C32 H32 0.9291 . . no C33 H33 0.9296 . . no C34 H34 0.9299 . . no C37 H37 0.9301 . . no C38 H38 0.9297 . . no C39 H39 0.9297 . . no C40 H40 0.9311 . . no C41 H41 0.9304 . . no C42 H42 0.9295 . . no C43 H43 0.9290 . . no C44 H44 0.9310 . . no C47 H47 0.9299 . . no C48 H48 0.9302 . . no C49 H49 0.9298 . . no C50 H50 0.9298 . . no C51 H51 0.9293 . . no C52 H52 0.9302 . . no C53 H53 0.9303 . . no C54 H54 0.9293 . . no C57 H57 0.9301 . . no C58 H58 0.9303 . . no C59 H59 0.9299 . . no C60 H60 0.9298 . . no C61 C62 1.539(4) . . no C63 C64 1.537(5) . . no C65 C66 1.556(5) . . no O23 H231 0.85(4) . . no O23 H232 0.84(3) . . no O24 H241 0.8337 . . no O24 H242 0.84(4) . . no O25 H251 0.85(3) . . no O25 H252 0.84(2) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O10 142.70(8) . . . no O2 Nb1 O11 92.29(9) . . . no O3 Nb1 O6 144.51(8) . . . no O3 Nb1 O7 138.62(9) . . . no O3 Nb1 O10 71.65(8) . . . no O3 Nb1 O11 81.61(9) . . . no O6 Nb1 O7 72.23(9) . . . no O6 Nb1 O10 73.04(9) . . . no O6 Nb1 O11 85.62(9) . . . no O7 Nb1 O10 140.70(9) . . . no O7 Nb1 O11 85.11(9) . . . no O10 Nb1 O11 74.43(9) . . . no O1 Nb1 O6 91.35(11) . . . no O1 Nb1 O7 104.00(11) . . . no O1 Nb1 O10 94.63(11) . . . no O1 Nb1 O11 169.05(10) . . . no O2 Nb1 O3 72.00(8) . . . no O2 Nb1 O6 141.79(8) . . . no O2 Nb1 O7 69.58(8) . . . no O1 Nb1 O3 94.98(11) . . . no O1 Nb1 O2 96.56(11) . . . no N1 Ni1 N3 94.72(10) . . . no N1 Ni1 N4 170.78(11) . . . no N1 Ni1 N6 91.19(10) . . . no N2 Ni1 N3 95.19(10) . . . no N1 Ni1 N5 94.41(10) . . . no N1 Ni1 N2 78.55(10) . . . no N4 Ni1 N5 92.66(10) . . . no N4 Ni1 N6 96.01(10) . . . no N5 Ni1 N6 78.60(10) . . . no N3 Ni1 N6 171.48(10) . . . no N2 Ni1 N5 168.21(10) . . . no N2 Ni1 N6 91.99(10) . . . no N2 Ni1 N4 95.41(10) . . . no N3 Ni1 N5 94.80(10) . . . no N3 Ni1 N4 78.78(10) . . . no N7 Ni2 N8 78.60(10) . . . no N11 Ni2 N12 78.53(11) . . . no N8 Ni2 N10 93.69(10) . . . no N8 Ni2 N11 170.68(10) . . . no N7 Ni2 N9 96.14(10) . . . no N7 Ni2 N10 170.68(10) . . . no N7 Ni2 N11 96.30(10) . . . no N7 Ni2 N12 91.24(11) . . . no N8 Ni2 N9 94.31(10) . . . no N10 Ni2 N12 94.49(11) . . . no N9 Ni2 N10 79.10(11) . . . no N9 Ni2 N11 93.99(10) . . . no N8 Ni2 N12 93.69(10) . . . no N10 Ni2 N11 92.05(11) . . . no N9 Ni2 N12 170.05(11) . . . no Nb1 O2 C61 122.77(18) . . . no Nb1 O3 C62 119.94(17) . . . no Nb1 O6 C63 121.4(2) . . . no Nb1 O7 C64 121.4(2) . . . no Nb1 O10 C65 120.2(2) . . . no Nb1 O11 C66 117.1(2) . . . no H141 O14 H142 106(4) . . . no H151 O15 H152 107(4) . . . no Ni1 N1 C5 115.7(2) . . . no Ni1 N1 C1 126.3(2) . . . no C1 N1 C5 118.0(3) . . . no Ni1 N2 C6 114.28(19) . . . no Ni1 N2 C10 126.1(2) . . . no C6 N2 C10 119.0(3) . . . no Ni1 N3 C15 115.0(2) . . . no Ni1 N3 C11 127.1(2) . . . no C11 N3 C15 117.9(3) . . . no Ni1 N4 C16 116.1(2) . . . no Ni1 N4 C20 125.5(2) . . . no C16 N4 C20 118.4(3) . . . no Ni1 N5 C25 114.7(2) . . . no Ni1 N5 C21 126.5(2) . . . no C21 N5 C25 118.6(3) . . . no Ni1 N6 C26 114.8(2) . . . no C26 N6 C30 117.8(3) . . . no Ni1 N6 C30 127.4(2) . . . no H161 O16 H162 102(5) . . . no Ni2 N7 C31 126.0(2) . . . no C31 N7 C35 118.5(3) . . . no Ni2 N7 C35 115.5(2) . . . no Ni2 N8 C40 126.6(2) . . . no C36 N8 C40 117.4(3) . . . no Ni2 N8 C36 115.6(2) . . . no C41 N9 C45 119.3(3) . . . no Ni2 N9 C45 114.7(2) . . . no Ni2 N9 C41 125.9(2) . . . no C46 N10 C50 119.1(3) . . . no Ni2 N10 C50 126.2(3) . . . no Ni2 N10 C46 114.5(2) . . . no Ni2 N11 C55 115.0(2) . . . no C51 N11 C55 118.3(3) . . . no Ni2 N11 C51 126.7(2) . . . no Ni2 N12 C56 115.0(2) . . . no C56 N12 C60 118.5(3) . . . no Ni2 N12 C60 126.4(2) . . . no H171 O17 H172 104(4) . . . no H181 O18 H182 106(3) . . . no H191 O19 H192 106(4) . . . no H201 O20 H202 105(4) . . . no N1 C1 C2 122.6(3) . . . no C1 C2 C3 119.8(3) . . . no C2 C3 C4 118.3(4) . . . no C3 C4 C5 119.2(3) . . . no N1 C5 C6 114.9(3) . . . no C4 C5 C6 123.0(3) . . . no N1 C5 C4 122.1(3) . . . no N2 C6 C5 116.1(3) . . . no C5 C6 C7 122.7(3) . . . no N2 C6 C7 121.2(3) . . . no C6 C7 C8 119.0(3) . . . no C7 C8 C9 119.2(3) . . . no C8 C9 C10 118.7(3) . . . no N2 C10 C9 122.9(3) . . . no N3 C11 C12 123.1(3) . . . no C11 C12 C13 120.1(3) . . . no C12 C13 C14 118.5(3) . . . no C13 C14 C15 118.3(3) . . . no C14 C15 C16 122.1(3) . . . no N3 C15 C16 115.8(3) . . . no N3 C15 C14 122.1(3) . . . no N4 C16 C17 122.4(3) . . . no N4 C16 C15 114.3(3) . . . no C15 C16 C17 123.3(3) . . . no C16 C17 C18 118.5(3) . . . no C17 C18 C19 120.2(4) . . . no C18 C19 C20 118.0(4) . . . no N4 C20 C19 122.5(3) . . . no N5 C21 C22 122.6(3) . . . no C21 C22 C23 118.8(4) . . . no C22 C23 C24 118.2(4) . . . no C23 C24 C25 120.2(4) . . . no C24 C25 C26 122.7(3) . . . no N5 C25 C24 121.4(3) . . . no N5 C25 C26 115.9(3) . . . no N6 C26 C25 115.5(3) . . . no C25 C26 C27 123.7(3) . . . no N6 C26 C27 120.7(3) . . . no C26 C27 C28 120.6(3) . . . no C27 C28 C29 118.8(3) . . . no C28 C29 C30 118.2(3) . . . no N6 C30 C29 123.9(3) . . . no N1 C1 H1 118.75 . . . no C2 C1 H1 118.67 . . . no C1 C2 H2 120.05 . . . no C3 C2 H2 120.20 . . . no C4 C3 H3 120.87 . . . no C2 C3 H3 120.86 . . . no C5 C4 H4 120.45 . . . no C3 C4 H4 120.35 . . . no C8 C7 H7 120.61 . . . no C6 C7 H7 120.43 . . . no C9 C8 H8 120.37 . . . no C7 C8 H8 120.42 . . . no C8 C9 H9 120.59 . . . no C10 C9 H9 120.70 . . . no C9 C10 H10 118.58 . . . no N2 C10 H10 118.49 . . . no N3 C11 H11 118.55 . . . no C12 C11 H11 118.37 . . . no C13 C12 H12 119.97 . . . no C11 C12 H12 119.94 . . . no C12 C13 H13 120.75 . . . no C14 C13 H13 120.80 . . . no C13 C14 H14 120.81 . . . no C15 C14 H14 120.85 . . . no C18 C17 H17 120.77 . . . no C16 C17 H17 120.70 . . . no C17 C18 H18 119.88 . . . no C19 C18 H18 119.95 . . . no C18 C19 H19 120.99 . . . no C20 C19 H19 121.00 . . . no C19 C20 H20 118.76 . . . no N4 C20 H20 118.75 . . . no C22 C21 H21 118.71 . . . no N5 C21 H21 118.70 . . . no H211 O21 H212 109(5) . . . no C21 C22 H22 120.62 . . . no C23 C22 H22 120.54 . . . no C24 C23 H23 120.93 . . . no C22 C23 H23 120.87 . . . no C25 C24 H24 119.92 . . . no C23 C24 H24 119.85 . . . no C28 C27 H27 119.72 . . . no C26 C27 H27 119.66 . . . no C27 C28 H28 120.59 . . . no C29 C28 H28 120.65 . . . no C30 C29 H29 120.90 . . . no C28 C29 H29 120.90 . . . no N6 C30 H30 118.09 . . . no C29 C30 H30 118.01 . . . no N7 C31 C32 122.3(3) . . . no C31 C32 C33 119.2(4) . . . no C32 C33 C34 119.1(4) . . . no C33 C34 C35 119.1(4) . . . no C34 C35 C36 122.4(3) . . . no N7 C35 C36 115.7(3) . . . no N7 C35 C34 121.9(3) . . . no N8 C36 C35 114.0(3) . . . no N8 C36 C37 122.5(3) . . . no C35 C36 C37 123.5(3) . . . no C36 C37 C38 119.4(4) . . . no C37 C38 C39 119.0(4) . . . no C38 C39 C40 119.0(4) . . . no N8 C40 C39 122.6(4) . . . no N9 C41 C42 122.2(3) . . . no C41 C42 C43 118.6(3) . . . no C42 C43 C44 119.4(4) . . . no C43 C44 C45 120.0(4) . . . no C44 C45 C46 123.9(3) . . . no N9 C45 C46 115.7(3) . . . no N9 C45 C44 120.4(3) . . . no N10 C46 C47 120.2(3) . . . no C45 C46 C47 123.7(3) . . . no N10 C46 C45 116.0(3) . . . no C46 C47 C48 120.2(4) . . . no C47 C48 C49 118.7(4) . . . no C48 C49 C50 120.3(4) . . . no N10 C50 C49 121.4(4) . . . no N11 C51 C52 123.0(3) . . . no C51 C52 C53 118.6(4) . . . no C52 C53 C54 119.0(4) . . . no C53 C54 C55 120.0(3) . . . no C54 C55 C56 123.6(3) . . . no N11 C55 C56 115.2(3) . . . no N11 C55 C54 121.2(3) . . . no C55 C56 C57 122.4(3) . . . no N12 C56 C57 121.3(3) . . . no N12 C56 C55 116.2(3) . . . no C56 C57 C58 118.9(3) . . . no C57 C58 C59 119.6(4) . . . no C58 C59 C60 118.3(4) . . . no N12 C60 C59 123.3(3) . . . no H221 O22 H222 107(3) . . . no N7 C31 H31 118.91 . . . no C32 C31 H31 118.81 . . . no C31 C32 H32 120.39 . . . no C33 C32 H32 120.44 . . . no C34 C33 H33 120.46 . . . no C32 C33 H33 120.47 . . . no C33 C34 H34 120.52 . . . no C35 C34 H34 120.34 . . . no C38 C37 H37 120.24 . . . no C36 C37 H37 120.37 . . . no C37 C38 H38 120.48 . . . no C39 C38 H38 120.53 . . . no C38 C39 H39 120.55 . . . no C40 C39 H39 120.41 . . . no C39 C40 H40 118.77 . . . no N8 C40 H40 118.68 . . . no N9 C41 H41 118.94 . . . no C42 C41 H41 118.86 . . . no C43 C42 H42 120.64 . . . no C41 C42 H42 120.75 . . . no C42 C43 H43 120.35 . . . no C44 C43 H43 120.28 . . . no C45 C44 H44 120.01 . . . no C43 C44 H44 119.98 . . . no C46 C47 H47 119.86 . . . no C48 C47 H47 119.90 . . . no C49 C48 H48 120.62 . . . no C47 C48 H48 120.65 . . . no C50 C49 H49 119.81 . . . no C48 C49 H49 119.93 . . . no C49 C50 H50 119.33 . . . no N10 C50 H50 119.30 . . . no C52 C51 H51 118.48 . . . no N11 C51 H51 118.58 . . . no C51 C52 H52 120.70 . . . no C53 C52 H52 120.70 . . . no C54 C53 H53 120.48 . . . no C52 C53 H53 120.52 . . . no C55 C54 H54 120.03 . . . no C53 C54 H54 120.01 . . . no C58 C57 H57 120.59 . . . no C56 C57 H57 120.55 . . . no C59 C58 H58 120.16 . . . no C57 C58 H58 120.21 . . . no C58 C59 H59 120.84 . . . no C60 C59 H59 120.85 . . . no N12 C60 H60 118.32 . . . no C59 C60 H60 118.35 . . . no O4 C61 C62 121.4(3) . . . no O2 C61 O4 126.5(3) . . . no O2 C61 C62 112.0(2) . . . no O3 C62 C61 113.2(2) . . . no O5 C62 C61 121.1(3) . . . no O3 C62 O5 125.7(3) . . . no O6 C63 O8 126.0(3) . . . no O8 C63 C64 122.4(3) . . . no O6 C63 C64 111.6(3) . . . no O7 C64 O9 126.5(3) . . . no O9 C64 C63 121.4(3) . . . no O7 C64 C63 112.0(3) . . . no O10 C65 C66 114.4(3) . . . no O12 C65 C66 120.2(3) . . . no O10 C65 O12 125.4(3) . . . no O13 C66 C65 120.7(3) . . . no O11 C66 O13 125.7(3) . . . no O11 C66 C65 113.6(3) . . . no H231 O23 H232 104(4) . . . no H241 O24 H242 105.17 . . . no H251 O25 H252 102(3) . . . no 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 O11 Nb1 O2 C61 80.2(3) . . . . no O1 Nb1 O3 C62 96.5(2) . . . . no O2 Nb1 O3 C62 1.2(2) . . . . no O6 Nb1 O3 C62 -164.1(2) . . . . no O7 Nb1 O3 C62 -21.3(3) . . . . no O10 Nb1 O3 C62 -170.2(3) . . . . no O11 Nb1 O3 C62 -94.0(2) . . . . no O1 Nb1 O6 C63 -106.7(3) . . . . no O2 Nb1 O6 C63 -4.3(3) . . . . no O3 Nb1 O6 C63 152.8(2) . . . . no O7 Nb1 O6 C63 -2.4(2) . . . . no O10 Nb1 O6 C63 158.9(3) . . . . no O11 Nb1 O6 C63 83.9(3) . . . . no O1 Nb1 O7 C64 96.3(3) . . . . no O2 Nb1 O7 C64 -171.9(3) . . . . no O3 Nb1 O7 C64 -149.0(2) . . . . no O6 Nb1 O7 C64 9.4(2) . . . . no O10 Nb1 O7 C64 -19.6(3) . . . . no O11 Nb1 O7 C64 -77.6(3) . . . . no O1 Nb1 O10 C65 177.9(2) . . . . no O2 Nb1 O10 C65 70.8(3) . . . . no O3 Nb1 O10 C65 84.2(2) . . . . no O6 Nb1 O10 C65 -92.1(2) . . . . no O7 Nb1 O10 C65 -63.3(3) . . . . no O11 Nb1 O10 C65 -2.0(2) . . . . no O2 Nb1 O11 C66 -140.4(2) . . . . no O1 Nb1 O2 C61 -93.4(3) . . . . no O3 Nb1 O2 C61 -0.2(2) . . . . no O6 Nb1 O2 C61 166.0(2) . . . . no O7 Nb1 O2 C61 164.1(3) . . . . no O10 Nb1 O2 C61 13.2(3) . . . . no O10 Nb1 O11 C66 4.2(2) . . . . no O3 Nb1 O11 C66 -69.0(2) . . . . no O6 Nb1 O11 C66 77.8(2) . . . . no O7 Nb1 O11 C66 150.3(2) . . . . no N2 Ni1 N1 C5 4.4(2) . . . . no N3 Ni1 N1 C1 -80.2(3) . . . . no N3 Ni1 N1 C5 98.7(2) . . . . no N2 Ni1 N1 C1 -174.6(3) . . . . no N1 Ni1 N2 C6 -6.8(2) . . . . no N1 Ni1 N2 C10 -177.2(3) . . . . no N3 Ni1 N2 C6 -100.6(2) . . . . no N5 Ni1 N1 C1 15.0(3) . . . . no N5 Ni1 N1 C5 -166.1(2) . . . . no N6 Ni1 N1 C1 93.6(3) . . . . no N6 Ni1 N1 C5 -87.4(2) . . . . no N6 Ni1 N2 C10 -86.4(3) . . . . no N1 Ni1 N3 C11 7.6(3) . . . . no N1 Ni1 N3 C15 -174.0(2) . . . . no N2 Ni1 N3 C11 86.5(3) . . . . no N2 Ni1 N3 C15 -95.1(2) . . . . no N4 Ni1 N3 C11 -179.0(3) . . . . no N4 Ni1 N3 C15 -0.6(2) . . . . no N5 Ni1 N3 C11 -87.2(3) . . . . no N5 Ni1 N3 C15 91.1(2) . . . . no N2 Ni1 N4 C16 93.7(2) . . . . no N2 Ni1 N4 C20 -85.0(3) . . . . no N3 Ni1 N2 C10 89.1(3) . . . . no N4 Ni1 N2 C6 -179.8(2) . . . . no N4 Ni1 N2 C10 9.9(3) . . . . no N6 Ni1 N2 C6 84.0(2) . . . . no N5 Ni1 N4 C16 -94.9(2) . . . . no N5 Ni1 N4 C20 86.4(3) . . . . no N6 Ni1 N4 C16 -173.7(2) . . . . no N6 Ni1 N4 C20 7.6(3) . . . . no N1 Ni1 N5 C21 -92.1(3) . . . . no N1 Ni1 N5 C25 84.2(2) . . . . no N3 Ni1 N5 C21 3.0(3) . . . . no N3 Ni1 N5 C25 179.3(2) . . . . no N4 Ni1 N5 C21 82.0(3) . . . . no N4 Ni1 N5 C25 -101.7(2) . . . . no N6 Ni1 N5 C21 177.6(3) . . . . no N6 Ni1 N5 C25 -6.1(2) . . . . no N1 Ni1 N6 C26 -88.7(2) . . . . no N1 Ni1 N6 C30 89.6(3) . . . . no N2 Ni1 N6 C26 -167.3(2) . . . . no N2 Ni1 N6 C30 11.0(3) . . . . no N4 Ni1 N6 C26 97.0(2) . . . . no N4 Ni1 N6 C30 -84.7(3) . . . . no N5 Ni1 N6 C26 5.5(2) . . . . no N5 Ni1 N6 C30 -176.2(3) . . . . no N3 Ni1 N4 C20 -179.2(3) . . . . no N3 Ni1 N4 C16 -0.5(2) . . . . no N11 Ni2 N7 C35 -168.3(2) . . . . no N11 Ni2 N7 C31 13.2(3) . . . . no N7 Ni2 N8 C36 -6.7(2) . . . . no N7 Ni2 N8 C40 -179.1(3) . . . . no N9 Ni2 N8 C36 -102.2(2) . . . . no N9 Ni2 N8 C40 85.5(3) . . . . no N10 Ni2 N8 C36 178.5(2) . . . . no N12 Ni2 N7 C31 91.8(3) . . . . no N12 Ni2 N7 C35 -89.7(2) . . . . no N11 Ni2 N12 C60 -179.7(3) . . . . no N12 Ni2 N8 C40 -88.5(3) . . . . no N7 Ni2 N9 C41 10.4(3) . . . . no N7 Ni2 N9 C45 -172.8(2) . . . . no N8 Ni2 N9 C41 89.3(3) . . . . no N8 Ni2 N9 C45 -93.8(2) . . . . no N10 Ni2 N9 C41 -177.7(3) . . . . no N10 Ni2 N9 C45 -0.9(2) . . . . no N11 Ni2 N9 C41 -86.4(3) . . . . no N11 Ni2 N9 C45 90.5(2) . . . . no N8 Ni2 N10 C46 93.0(2) . . . . no N8 Ni2 N10 C50 -82.3(3) . . . . no N9 Ni2 N10 C46 -0.7(2) . . . . no N9 Ni2 N10 C50 -176.0(3) . . . . no N11 Ni2 N10 C46 -94.4(2) . . . . no N11 Ni2 N10 C50 90.4(3) . . . . no N8 Ni2 N7 C31 -174.7(3) . . . . no N8 Ni2 N7 C35 3.8(2) . . . . no N9 Ni2 N7 C31 -81.5(3) . . . . no N9 Ni2 N7 C35 97.0(2) . . . . no N9 Ni2 N11 C55 -171.7(2) . . . . no N10 Ni2 N11 C51 85.6(3) . . . . no N10 Ni2 N11 C55 -92.5(2) . . . . no N12 Ni2 N11 C51 179.8(3) . . . . no N12 Ni2 N11 C55 1.7(2) . . . . no N7 Ni2 N12 C56 -98.1(2) . . . . no N7 Ni2 N12 C60 84.2(3) . . . . no N8 Ni2 N12 C56 -176.7(2) . . . . no N8 Ni2 N12 C60 5.5(3) . . . . no N10 Ni2 N12 C56 89.3(2) . . . . no N10 Ni2 N12 C60 -88.5(3) . . . . no N11 Ni2 N12 C56 -1.9(2) . . . . no N12 Ni2 N10 C46 -173.0(2) . . . . no N12 Ni2 N10 C50 11.7(3) . . . . no N7 Ni2 N11 C51 -90.3(3) . . . . no N7 Ni2 N11 C55 91.7(2) . . . . no N9 Ni2 N11 C51 6.4(3) . . . . no N12 Ni2 N8 C36 83.8(2) . . . . no N10 Ni2 N8 C40 6.2(3) . . . . no Nb1 O2 C61 O4 179.0(3) . . . . no Nb1 O2 C61 C62 -0.6(4) . . . . no Nb1 O3 C62 O5 178.1(2) . . . . no Nb1 O3 C62 C61 -1.9(3) . . . . no Nb1 O6 C63 O8 178.1(3) . . . . no Nb1 O6 C63 C64 -3.4(4) . . . . no Nb1 O7 C64 O9 165.6(3) . . . . no Nb1 O7 C64 C63 -13.7(4) . . . . no Nb1 O10 C65 C66 -0.1(3) . . . . no Nb1 O10 C65 O12 179.6(3) . . . . no Nb1 O11 C66 O13 172.9(3) . . . . no Nb1 O11 C66 C65 -5.4(3) . . . . no C1 N1 C5 C4 -1.1(5) . . . . no C1 N1 C5 C6 177.6(3) . . . . no C5 N1 C1 C2 -1.1(5) . . . . no Ni1 N1 C1 C2 177.8(3) . . . . no Ni1 N1 C5 C4 179.9(3) . . . . no Ni1 N1 C5 C6 -1.5(3) . . . . no Ni1 N2 C6 C7 -171.4(2) . . . . no C6 N2 C10 C9 0.9(5) . . . . no Ni1 N2 C10 C9 170.9(3) . . . . no C10 N2 C6 C7 -0.3(4) . . . . no Ni1 N2 C6 C5 8.1(3) . . . . no C10 N2 C6 C5 179.2(3) . . . . no Ni1 N3 C11 C12 175.7(2) . . . . no C11 N3 C15 C16 -179.9(3) . . . . no Ni1 N3 C15 C14 -177.1(2) . . . . no C15 N3 C11 C12 -2.6(5) . . . . no C11 N3 C15 C14 1.4(4) . . . . no Ni1 N3 C15 C16 1.6(3) . . . . no Ni1 N4 C16 C15 1.5(3) . . . . no C16 N4 C20 C19 -0.6(5) . . . . no Ni1 N4 C16 C17 -179.0(3) . . . . no C20 N4 C16 C15 -179.7(3) . . . . no C20 N4 C16 C17 -0.2(5) . . . . no Ni1 N4 C20 C19 178.2(3) . . . . no Ni1 N5 C21 C22 175.0(3) . . . . no C21 N5 C25 C26 -177.7(3) . . . . no Ni1 N5 C25 C24 -173.7(3) . . . . no C25 N5 C21 C22 -1.2(5) . . . . no C21 N5 C25 C24 3.0(5) . . . . no Ni1 N5 C25 C26 5.7(3) . . . . no C30 N6 C26 C27 0.8(5) . . . . no Ni1 N6 C30 C29 -179.9(2) . . . . no C30 N6 C26 C25 177.3(3) . . . . no Ni1 N6 C26 C25 -4.3(3) . . . . no Ni1 N6 C26 C27 179.2(3) . . . . no C26 N6 C30 C29 -1.6(5) . . . . no C31 N7 C35 C34 -0.2(5) . . . . no C35 N7 C31 C32 0.0(5) . . . . no C31 N7 C35 C36 177.9(3) . . . . no Ni2 N7 C35 C36 -0.7(4) . . . . no Ni2 N7 C31 C32 178.4(3) . . . . no Ni2 N7 C35 C34 -178.9(3) . . . . no C36 N8 C40 C39 -0.3(5) . . . . no Ni2 N8 C36 C37 -171.3(3) . . . . no C40 N8 C36 C37 1.8(5) . . . . no Ni2 N8 C36 C35 8.2(3) . . . . no C40 N8 C36 C35 -178.7(3) . . . . no Ni2 N8 C40 C39 171.9(3) . . . . no Ni2 N9 C45 C44 -177.8(3) . . . . no Ni2 N9 C41 C42 175.3(3) . . . . no C41 N9 C45 C46 179.3(3) . . . . no Ni2 N9 C45 C46 2.2(4) . . . . no C41 N9 C45 C44 -0.7(5) . . . . no C45 N9 C41 C42 -1.4(5) . . . . no C50 N10 C46 C47 -2.0(5) . . . . no Ni2 N10 C50 C49 176.4(3) . . . . no C50 N10 C46 C45 177.7(3) . . . . no Ni2 N10 C46 C45 2.1(4) . . . . no C46 N10 C50 C49 1.3(5) . . . . no Ni2 N10 C46 C47 -177.6(3) . . . . no Ni2 N11 C55 C54 178.8(3) . . . . no C51 N11 C55 C56 -179.5(3) . . . . no Ni2 N11 C55 C56 -1.3(3) . . . . no C51 N11 C55 C54 0.6(5) . . . . no C55 N11 C51 C52 0.4(5) . . . . no Ni2 N11 C51 C52 -177.6(3) . . . . no C60 N12 C56 C57 0.8(5) . . . . no C56 N12 C60 C59 -1.8(5) . . . . no Ni2 N12 C56 C55 1.8(4) . . . . no C60 N12 C56 C55 179.8(3) . . . . no Ni2 N12 C60 C59 175.9(3) . . . . no Ni2 N12 C56 C57 -177.2(3) . . . . no N1 C1 C2 C3 1.6(5) . . . . no C1 C2 C3 C4 0.2(6) . . . . no C2 C3 C4 C5 -2.2(6) . . . . no C3 C4 C5 C6 -175.8(3) . . . . no C3 C4 C5 N1 2.8(5) . . . . no N1 C5 C6 N2 -4.5(4) . . . . no C4 C5 C6 C7 -6.3(5) . . . . no C4 C5 C6 N2 174.1(3) . . . . no N1 C5 C6 C7 175.1(3) . . . . no N2 C6 C7 C8 0.5(5) . . . . no C5 C6 C7 C8 -179.0(3) . . . . no C6 C7 C8 C9 -1.2(5) . . . . no C7 C8 C9 C10 1.7(5) . . . . no C8 C9 C10 N2 -1.6(5) . . . . no N3 C11 C12 C13 1.4(5) . . . . no C11 C12 C13 C14 0.9(5) . . . . no C12 C13 C14 C15 -2.0(5) . . . . no C13 C14 C15 C16 -177.8(3) . . . . no C13 C14 C15 N3 0.8(5) . . . . no C14 C15 C16 C17 -2.9(5) . . . . no N3 C15 C16 C17 178.4(3) . . . . no N3 C15 C16 N4 -2.0(4) . . . . no C14 C15 C16 N4 176.7(3) . . . . no C15 C16 C17 C18 178.8(3) . . . . no N4 C16 C17 C18 -0.7(5) . . . . no C16 C17 C18 C19 2.4(6) . . . . no C17 C18 C19 C20 -3.0(6) . . . . no C18 C19 C20 N4 2.2(6) . . . . no N5 C21 C22 C23 -1.5(6) . . . . no C21 C22 C23 C24 2.4(6) . . . . no C22 C23 C24 C25 -0.6(6) . . . . no C23 C24 C25 C26 178.6(3) . . . . no C23 C24 C25 N5 -2.1(6) . . . . no N5 C25 C26 C27 175.4(3) . . . . no C24 C25 C26 N6 178.4(3) . . . . no C24 C25 C26 C27 -5.2(5) . . . . no N5 C25 C26 N6 -1.0(4) . . . . no C25 C26 C27 C28 -176.1(4) . . . . no N6 C26 C27 C28 0.2(6) . . . . no C26 C27 C28 C29 -0.3(6) . . . . no C27 C28 C29 C30 -0.5(6) . . . . no C28 C29 C30 N6 1.5(5) . . . . no N7 C31 C32 C33 0.9(6) . . . . no C31 C32 C33 C34 -1.4(6) . . . . no C32 C33 C34 C35 1.1(6) . . . . no C33 C34 C35 C36 -178.4(4) . . . . no C33 C34 C35 N7 -0.3(6) . . . . no C34 C35 C36 C37 -7.4(5) . . . . no N7 C35 C36 N8 -5.0(4) . . . . no N7 C35 C36 C37 174.5(3) . . . . no C34 C35 C36 N8 173.2(3) . . . . no N8 C36 C37 C38 -0.2(6) . . . . no C35 C36 C37 C38 -179.7(3) . . . . no C36 C37 C38 C39 -2.9(6) . . . . no C37 C38 C39 C40 4.3(6) . . . . no C38 C39 C40 N8 -2.8(6) . . . . no N9 C41 C42 C43 2.0(5) . . . . no C41 C42 C43 C44 -0.5(6) . . . . no C42 C43 C44 C45 -1.5(6) . . . . no C43 C44 C45 C46 -177.8(3) . . . . no C43 C44 C45 N9 2.2(5) . . . . no N9 C45 C46 C47 176.8(3) . . . . no C44 C45 C46 C47 -3.3(5) . . . . no N9 C45 C46 N10 -2.9(4) . . . . no C44 C45 C46 N10 177.1(3) . . . . no N10 C46 C47 C48 2.0(6) . . . . no C45 C46 C47 C48 -177.6(4) . . . . no C46 C47 C48 C49 -1.3(6) . . . . no C47 C48 C49 C50 0.7(7) . . . . no C48 C49 C50 N10 -0.6(6) . . . . no N11 C51 C52 C53 -0.9(6) . . . . no C51 C52 C53 C54 0.5(6) . . . . no C52 C53 C54 C55 0.5(6) . . . . no C53 C54 C55 C56 179.1(4) . . . . no C53 C54 C55 N11 -1.0(6) . . . . no C54 C55 C56 C57 -1.5(5) . . . . no C54 C55 C56 N12 179.6(3) . . . . no N11 C55 C56 N12 -0.3(4) . . . . no N11 C55 C56 C57 178.6(3) . . . . no N12 C56 C57 C58 0.3(6) . . . . no C55 C56 C57 C58 -178.5(3) . . . . no C56 C57 C58 C59 -0.6(6) . . . . no C57 C58 C59 C60 -0.3(6) . . . . no C58 C59 C60 N12 1.6(6) . . . . no O2 C61 C62 O5 -178.4(3) . . . . no O4 C61 C62 O3 -178.0(3) . . . . no O4 C61 C62 O5 2.0(5) . . . . no O2 C61 C62 O3 1.6(4) . . . . no O8 C63 C64 O7 -170.9(3) . . . . no O6 C63 C64 O9 -168.8(3) . . . . no O8 C63 C64 O9 9.9(6) . . . . no O6 C63 C64 O7 10.5(4) . . . . no O10 C65 C66 O11 3.7(4) . . . . no O12 C65 C66 O13 5.7(5) . . . . no O10 C65 C66 O13 -174.6(3) . . . . no O12 C65 C66 O11 -176.0(3) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O14 H141 O1 0.84(4) 2.12(4) 2.911(4) 157(4) . no O14 H142 O15 0.83(3) 2.15(4) 2.831(5) 139(4) . no O15 H151 O17 0.83(3) 2.03(4) 2.794(5) 153(4) 4_745 no O15 H152 O16 0.83(3) 2.01(3) 2.749(5) 148(4) . no O16 H161 O12 0.85(5) 2.27(5) 2.912(5) 132(4) . no O16 H162 Cl1 0.84(5) 2.51(5) 3.093(5) 128(4) 1_655 no O17 H171 O11 0.84(3) 2.15(3) 2.984(4) 176(4) . no O17 H172 O18 0.84(2) 2.27(5) 2.777(5) 119(5) . no O18 H181 O9 0.84(3) 2.27(3) 3.009(5) 147(3) . no O18 H182 O20 0.84(3) 1.94(3) 2.742(5) 161(4) 4_655 no O19 H191 O9 0.835(13) 2.04(2) 2.850(4) 162(4) . no O19 H192 Cl1 0.84(3) 2.49(3) 3.284(3) 159(4) . no O20 H201 Cl1 0.83(4) 2.43(4) 3.189(4) 153(4) . no O20 H202 O21 0.83(3) 2.16(3) 2.758(6) 129(3) . no O21 H211 O22 0.82(3) 2.22(3) 2.717(5) 119(3) . no O21 H212 O24 0.83(4) 2.38(3) 3.193(8) 167(6) . no O22 H221 O19 0.83(3) 1.95(3) 2.774(4) 172(3) 4_645 no O22 H222 O23 0.82(2) 2.02(2) 2.716(4) 142(4) . no O23 H231 O14 0.85(4) 2.03(3) 2.794(5) 150(4) . no O23 H232 O13 0.84(3) 2.32(5) 2.823(5) 119(4) 4_745 no O24 H241 Cl1 0.8300 2.5200 3.168(6) 135.00 . no O24 H242 O25 0.84(4) 2.13(6) 2.803(6) 138(8) . no O25 H251 O5 0.85(3) 2.03(3) 2.786(4) 148(4) 2_665 no O25 H252 O8 0.84(2) 1.96(2) 2.796(4) 174(4) . no C4 H4 O5 0.9300 2.4700 3.374(4) 165.00 1_455 no C7 H7 O5 0.9300 2.5700 3.465(4) 161.00 1_455 no C12 H12 Cl1 0.9300 2.8100 3.545(4) 137.00 . no C14 H14 O4 0.9300 2.5800 3.438(4) 154.00 . no C30 H30 N2 0.9300 2.6200 3.155(4) 118.00 . no C31 H31 O21 0.9300 2.5900 3.338(6) 138.00 4_655 no C37 H37 O4 0.9300 2.5800 3.479(5) 162.00 . no C38 H38 O6 0.9300 2.4000 3.249(5) 152.00 2_664 no C39 H39 O12 0.9300 2.5100 3.438(5) 172.00 2_664 no C42 H42 Cl1 0.9300 2.8000 3.666(4) 155.00 . no C44 H44 O5 0.9300 2.4000 3.310(5) 167.00 1_455 no C59 H59 O13 0.9300 2.5900 3.201(5) 124.00 3_465 no #=============================================================================== data_VI _database_code_depnum_ccdc_archive 'CCDC 648557' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H24 Cu N6), C6 Nb O13, 12(H2 O), Cl' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural '2(C30 H24 Cu N6), C6 Nb O13, 12(H2 O), Cl' _chemical_formula_sum 'C66 H72 Cl Cu2 N12 Nb O25' _chemical_formula_iupac ? _chemical_formula_weight 1688.80 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 15.0350(10) _cell_length_b 22.267(2) _cell_length_c 22.538(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7545.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 15.4 _cell_special_details ; ? ; _exptl_crystal_description polyhedral _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 0.828 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type none # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW1100 updated by STOE' _diffrn_measurement_method 'omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 4 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 10.9 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 17810 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.05 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 16364 # number of observed reflections (> n sig(I)) _reflns_number_gt 9976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1995)' _computing_cell_refinement 'STADI4 (STOE, 1995)' _computing_data_reduction 'X-RED (STOE, 1995)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0827P)^2^+0.4229P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(13) # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ad _refine_ls_number_reflns 16364 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 46 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.850 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.070 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cu1 Cu Uani 0.63665(4) 0.66897(3) 0.99943(3) 1.000 0.0431(2) . . N1 N Uani 0.7476(3) 0.6598(2) 0.94654(19) 1.000 0.0450(14) . . N2 N Uani 0.7141(3) 0.6024(2) 1.0481(2) 1.000 0.0480(16) . . N3 N Uani 0.5583(3) 0.6080(2) 0.9500(2) 1.000 0.0483(17) . . N4 N Uani 0.5260(3) 0.6614(2) 1.0514(2) 1.000 0.0483(16) . . N5 N Uani 0.5860(4) 0.7496(2) 0.9556(2) 1.000 0.0630(17) . . N6 N Uani 0.6978(4) 0.7422(2) 1.0474(2) 1.000 0.0607(17) . . C1 C Uani 0.7586(4) 0.6871(3) 0.8940(3) 1.000 0.061(2) . . C2 C Uani 0.8313(5) 0.6789(3) 0.8600(3) 1.000 0.068(2) . . C3 C Uani 0.8982(5) 0.6422(3) 0.8804(3) 1.000 0.079(3) . . C4 C Uani 0.8881(4) 0.6149(3) 0.9352(3) 1.000 0.066(2) . . C5 C Uani 0.8132(3) 0.6238(2) 0.9665(2) 1.000 0.0460(17) . . C6 C Uani 0.7936(4) 0.5934(2) 1.0241(2) 1.000 0.0457(17) . . C7 C Uani 0.8566(4) 0.5572(3) 1.0528(3) 1.000 0.061(2) . . C8 C Uani 0.8333(5) 0.5312(3) 1.1060(3) 1.000 0.076(3) . . C9 C Uani 0.7535(5) 0.5417(3) 1.1308(3) 1.000 0.069(3) . . C10 C Uani 0.6948(4) 0.5782(3) 1.1001(3) 1.000 0.059(2) . . C11 C Uani 0.5782(4) 0.5821(3) 0.8972(3) 1.000 0.063(2) . . C12 C Uani 0.5206(5) 0.5450(3) 0.8689(3) 1.000 0.070(3) . . C13 C Uani 0.4429(5) 0.5319(3) 0.8918(3) 1.000 0.070(3) . . C14 C Uani 0.4202(4) 0.5561(3) 0.9475(3) 1.000 0.063(2) . . C15 C Uani 0.4798(3) 0.5949(2) 0.9751(3) 1.000 0.0460(17) . . C16 C Uani 0.4621(4) 0.6236(3) 1.0330(3) 1.000 0.0533(19) . . C17 C Uani 0.3857(5) 0.6139(3) 1.0655(3) 1.000 0.076(3) . . C18 C Uani 0.3738(6) 0.6461(4) 1.1177(3) 1.000 0.086(3) . . C19 C Uani 0.4393(5) 0.6825(3) 1.1376(3) 1.000 0.078(3) . . C20 C Uani 0.5155(5) 0.6903(3) 1.1031(3) 1.000 0.065(2) . . C21 C Uani 0.5298(5) 0.7510(3) 0.9099(3) 1.000 0.078(3) . . C22 C Uani 0.5080(6) 0.8057(4) 0.8811(4) 1.000 0.088(3) . . C23 C Uani 0.5454(6) 0.8571(4) 0.8992(4) 1.000 0.085(3) . . C24 C Uani 0.6031(5) 0.8560(3) 0.9461(3) 1.000 0.075(3) . . C25 C Uani 0.6219(4) 0.8021(3) 0.9751(3) 1.000 0.0563(19) . . C26 C Uani 0.6815(4) 0.7979(2) 1.0264(3) 1.000 0.0537(19) . . C27 C Uani 0.7168(6) 0.8485(3) 1.0537(3) 1.000 0.077(3) . . C28 C Uani 0.7685(5) 0.8413(3) 1.1038(3) 1.000 0.079(3) . . C29 C Uani 0.7854(5) 0.7848(3) 1.1239(3) 1.000 0.074(3) . . C30 C Uani 0.7488(5) 0.7375(3) 1.0951(3) 1.000 0.072(3) . . Cu2 Cu Uani 0.63899(4) 0.33019(3) 0.97113(3) 1.000 0.0449(2) . . N7 N Uani 0.5216(3) 0.3399(2) 0.92372(19) 1.000 0.0487(17) . . N8 N Uani 0.5610(3) 0.3943(2) 1.0245(2) 1.000 0.0510(16) . . N9 N Uani 0.7102(3) 0.3942(2) 0.9256(2) 1.000 0.0507(17) . . N10 N Uani 0.7509(3) 0.3381(2) 1.0252(2) 1.000 0.0603(17) . . N11 N Uani 0.6987(3) 0.2543(2) 0.9192(2) 1.000 0.0597(17) . . N12 N Uani 0.5918(4) 0.2530(2) 1.0130(2) 1.000 0.0570(19) . . C31 C Uani 0.5076(5) 0.3134(3) 0.8710(3) 1.000 0.069(2) . . C32 C Uani 0.4288(6) 0.3203(3) 0.8404(3) 1.000 0.085(3) . . C33 C Uani 0.3635(6) 0.3552(4) 0.8648(4) 1.000 0.087(3) . . C34 C Uani 0.3775(5) 0.3831(3) 0.9185(4) 1.000 0.080(3) . . C35 C Uani 0.4571(4) 0.3742(3) 0.9468(3) 1.000 0.0513(17) . . C36 C Uani 0.4791(4) 0.4030(2) 1.0059(3) 1.000 0.0513(19) . . C37 C Uani 0.4182(5) 0.4352(3) 1.0370(3) 1.000 0.076(3) . . C38 C Uani 0.4444(6) 0.4610(3) 1.0906(3) 1.000 0.083(3) . . C39 C Uani 0.5285(7) 0.4553(3) 1.1085(3) 1.000 0.090(4) . . C40 C Uani 0.5861(5) 0.4205(3) 1.0766(3) 1.000 0.070(3) . . C41 C Uani 0.6873(4) 0.4204(3) 0.8743(3) 1.000 0.061(2) . . C42 C Uani 0.7402(5) 0.4606(3) 0.8451(3) 1.000 0.070(3) . . C43 C Uani 0.8195(5) 0.4770(3) 0.8696(3) 1.000 0.079(3) . . C44 C Uani 0.8448(5) 0.4507(3) 0.9237(3) 1.000 0.072(2) . . C45 C Uani 0.7885(4) 0.4092(3) 0.9504(3) 1.000 0.0520(19) . . C46 C Uani 0.8106(4) 0.3778(3) 1.0064(3) 1.000 0.0540(19) . . C47 C Uani 0.8855(5) 0.3896(3) 1.0389(4) 1.000 0.079(3) . . C48 C Uani 0.8999(7) 0.3610(5) 1.0920(4) 1.000 0.101(4) . . C49 C Uani 0.8397(7) 0.3185(4) 1.1103(3) 1.000 0.093(3) . . C50 C Uani 0.7653(5) 0.3081(3) 1.0769(3) 1.000 0.076(3) . . C51 C Uani 0.7526(5) 0.2567(3) 0.8716(3) 1.000 0.078(3) . . C52 C Uani 0.7886(6) 0.2088(4) 0.8450(4) 1.000 0.090(3) . . C53 C Uani 0.7670(6) 0.1524(4) 0.8672(4) 1.000 0.090(3) . . C54 C Uani 0.7128(6) 0.1483(3) 0.9150(3) 1.000 0.081(3) . . C55 C Uani 0.6796(4) 0.2003(3) 0.9413(3) 1.000 0.058(2) . . C56 C Uani 0.6213(4) 0.1999(2) 0.9947(3) 1.000 0.0523(19) . . C57 C Uani 0.5964(5) 0.1482(3) 1.0231(3) 1.000 0.072(3) . . C58 C Uani 0.5437(6) 0.1506(3) 1.0729(3) 1.000 0.080(3) . . C59 C Uani 0.5153(5) 0.2040(4) 1.0921(3) 1.000 0.073(3) . . C60 C Uani 0.5384(5) 0.2555(3) 1.0616(3) 1.000 0.070(3) . . Nb1 Nb Uani 0.15692(3) 0.50994(2) 0.79940(2) 1.000 0.0453(1) . . O1 O Uani 0.1708(3) 0.58637(18) 0.7958(2) 1.000 0.0753(16) . . O2 O Uani 0.2245(2) 0.4968(2) 0.88088(16) 1.000 0.0529(13) . . O3 O Uani 0.0600(2) 0.51412(19) 0.87050(16) 1.000 0.0545(13) . . O4 O Uani 0.2185(2) 0.4898(2) 0.97945(16) 1.000 0.0599(14) . . O5 O Uani 0.0357(2) 0.5073(2) 0.96814(19) 1.000 0.0621(13) . . O6 O Uani 0.1731(2) 0.49918(19) 0.70564(17) 1.000 0.0633(14) . . O7 O Uani 0.2854(3) 0.4762(2) 0.78471(17) 1.000 0.0657(16) . . O8 O Uani 0.2621(3) 0.4738(3) 0.63159(19) 1.000 0.082(2) . . O9 O Uani 0.3749(4) 0.4294(3) 0.7200(2) 1.000 0.114(3) . . O10 O Uani 0.0298(2) 0.51037(19) 0.76153(17) 1.000 0.0570(14) . . O11 O Uani 0.1137(3) 0.41547(17) 0.79680(19) 1.000 0.0617(14) . . O12 O Uani -0.0877(3) 0.4579(3) 0.7320(2) 1.000 0.094(2) . . O13 O Uani 0.0004(4) 0.3557(3) 0.7762(3) 1.000 0.109(3) . . C61 C Uani 0.1838(3) 0.4971(2) 0.9311(2) 1.000 0.0437(17) . . C62 C Uani 0.0836(3) 0.5067(2) 0.9249(2) 1.000 0.0457(16) . . C63 C Uani 0.2460(4) 0.4786(3) 0.6839(3) 1.000 0.060(2) . . C64 C Uani 0.3099(4) 0.4595(3) 0.7322(3) 1.000 0.068(3) . . C65 C Uani -0.0123(4) 0.4613(3) 0.7543(3) 1.000 0.061(2) . . C66 C Uani 0.0358(5) 0.4057(3) 0.7773(3) 1.000 0.067(3) . . O14 O Uani 0.0818(4) 0.7038(2) 0.7916(3) 1.000 0.097(2) . . O15 O Uani -0.0574(5) 0.6893(3) 0.7070(4) 1.000 0.128(3) . . O16 O Uani -0.1516(6) 0.5857(3) 0.7290(5) 1.000 0.177(5) . . O17 O Uani 0.1775(5) 0.2844(3) 0.7986(4) 1.000 0.124(3) . . O18 O Uani 0.2977(5) 0.2976(3) 0.7063(4) 1.000 0.129(3) . . O19 O Uani 0.5581(4) 0.4318(3) 0.7520(3) 1.000 0.110(3) . . O20 O Uani 0.6094(6) 0.7010(4) 0.7757(3) 1.000 0.142(3) . . O21 O Uani 0.4326(5) 0.7181(3) 0.7411(4) 1.000 0.142(4) . . O22 O Uani 0.3460(3) 0.8253(2) 0.7617(3) 1.000 0.099(2) . . O23 O Uani 0.1651(4) 0.8156(3) 0.7763(4) 1.000 0.117(3) . . O24 O Uani 0.4398(9) 0.5900(4) 0.6972(4) 1.000 0.289(9) . . O25 O Uani 0.4308(3) 0.5150(3) 0.5893(2) 1.000 0.0877(19) . . Cl1 Cl Uani 0.6464(2) 0.56724(12) 0.73655(12) 1.000 0.1265(10) . . H1 H Uiso 0.71420 0.71280 0.88050 1.000 0.0720 calc R H2 H Uiso 0.83610 0.69770 0.82340 1.000 0.0810 calc R H3 H Uiso 0.94910 0.63580 0.85780 1.000 0.0950 calc R H4 H Uiso 0.93300 0.59050 0.95020 1.000 0.0800 calc R H7 H Uiso 0.91260 0.55090 1.03630 1.000 0.0740 calc R H8 H Uiso 0.87340 0.50590 1.12500 1.000 0.0910 calc R H9 H Uiso 0.73830 0.52500 1.16720 1.000 0.0830 calc R H10 H Uiso 0.63950 0.58600 1.11670 1.000 0.0710 calc R H11 H Uiso 0.63310 0.59000 0.87980 1.000 0.0760 calc R H12 H Uiso 0.53660 0.52860 0.83250 1.000 0.0840 calc R H13 H Uiso 0.40350 0.50700 0.87160 1.000 0.0840 calc R H14 H Uiso 0.36640 0.54630 0.96550 1.000 0.0750 calc R H17 H Uiso 0.34310 0.58650 1.05270 1.000 0.0910 calc R H18 H Uiso 0.32110 0.64250 1.13900 1.000 0.1030 calc R H19 H Uiso 0.43360 0.70220 1.17380 1.000 0.0940 calc R H20 H Uiso 0.56000 0.71610 1.11620 1.000 0.0790 calc R H21 H Uiso 0.50440 0.71540 0.89660 1.000 0.0940 calc R H22 H Uiso 0.46780 0.80590 0.84980 1.000 0.1060 calc R H23 H Uiso 0.53240 0.89310 0.88020 1.000 0.1020 calc R H24 H Uiso 0.62990 0.89140 0.95870 1.000 0.0900 calc R H27 H Uiso 0.70580 0.88660 1.03850 1.000 0.0920 calc R H28 H Uiso 0.79140 0.87460 1.12350 1.000 0.0940 calc R H29 H Uiso 0.82160 0.77880 1.15690 1.000 0.0880 calc R H30 H Uiso 0.76020 0.69930 1.10980 1.000 0.0860 calc R H31 H Uiso 0.55220 0.28960 0.85480 1.000 0.0820 calc R H32 H Uiso 0.42030 0.30170 0.80390 1.000 0.1020 calc R H33 H Uiso 0.30960 0.36010 0.84510 1.000 0.1040 calc R H34 H Uiso 0.33390 0.40740 0.93520 1.000 0.0960 calc R H37 H Uiso 0.36050 0.43990 1.02290 1.000 0.0920 calc R H38 H Uiso 0.40350 0.48200 1.11370 1.000 0.1000 calc R H39 H Uiso 0.54790 0.47490 1.14250 1.000 0.1080 calc R H40 H Uiso 0.64350 0.41450 1.09080 1.000 0.0840 calc R H41 H Uiso 0.63260 0.41060 0.85760 1.000 0.0730 calc R H42 H Uiso 0.72240 0.47670 0.80890 1.000 0.0840 calc R H43 H Uiso 0.85590 0.50500 0.85100 1.000 0.0940 calc R H44 H Uiso 0.89850 0.46090 0.94150 1.000 0.0860 calc R H47 H Uiso 0.92700 0.41710 1.02490 1.000 0.0950 calc R H48 H Uiso 0.94930 0.37020 1.11510 1.000 0.1210 calc R H49 H Uiso 0.84940 0.29690 1.14500 1.000 0.1110 calc R H50 H Uiso 0.72370 0.28010 1.08990 1.000 0.0920 calc R H51 H Uiso 0.76570 0.29440 0.85610 1.000 0.0930 calc R H52 H Uiso 0.82680 0.21310 0.81280 1.000 0.1070 calc R H53 H Uiso 0.78940 0.11780 0.84950 1.000 0.1080 calc R H54 H Uiso 0.69780 0.11080 0.93030 1.000 0.0970 calc R H57 H Uiso 0.61530 0.11130 1.00870 1.000 0.0870 calc R H58 H Uiso 0.52820 0.11560 1.09300 1.000 0.0960 calc R H59 H Uiso 0.48000 0.20650 1.12590 1.000 0.0870 calc R H60 H Uiso 0.51710 0.29250 1.07460 1.000 0.0840 calc R H141 H Uiso 0.104(5) 0.6697(16) 0.798(4) 1.000 0.1170 . . H142 H Uiso 0.049(3) 0.698(3) 0.7618(17) 1.000 0.1170 . . H151 H Uiso -0.103(4) 0.709(2) 0.717(5) 1.000 0.1530 . . H152 H Uiso -0.070(2) 0.6535(14) 0.716(5) 1.000 0.1530 . . H161 H Uiso -0.12680 0.55210 0.73970 1.000 0.2120 . . H162 H Uiso -0.2054(5) 0.5795(11) 0.738(3) 1.000 0.2120 . . H171 H Uiso 0.151(4) 0.317(2) 0.789(4) 1.000 0.1490 . . H172 H Uiso 0.208(6) 0.277(4) 0.768(3) 1.000 0.1490 . . H181 H Uiso 0.327(4) 0.3300(7) 0.712(4) 1.000 0.1550 . . H182 H Uiso 0.33490 0.27130 0.72220 1.000 0.1550 . . H191 H Uiso 0.506(2) 0.436(4) 0.740(4) 1.000 0.1320 . . H192 H Uiso 0.581(5) 0.4662(15) 0.744(4) 1.000 0.1320 . . H201 H Uiso 0.621(5) 0.6681(11) 0.759(3) 1.000 0.1710 . . H202 H Uiso 0.561(3) 0.7112(13) 0.761(4) 1.000 0.1710 . . H211 H Uiso 0.3804(17) 0.7301(10) 0.738(6) 1.000 0.1710 . . H212 H Uiso 0.42440 0.67850 0.73590 1.000 0.1710 . . H221 H Uiso 0.367(4) 0.8578(19) 0.749(4) 1.000 0.1190 . . H222 H Uiso 0.293(2) 0.833(3) 0.770(4) 1.000 0.1190 . . H231 H Uiso 0.130(4) 0.7870(12) 0.785(4) 1.000 0.1400 . . H232 H Uiso 0.133(3) 0.8462(15) 0.777(5) 1.000 0.1400 . . H241 H Uiso 0.50050 0.58660 0.70370 1.000 0.3470 . . H242 H Uiso 0.4416(10) 0.5937(7) 0.6604(5) 1.000 0.3470 . . H251 H Uiso 0.434(4) 0.504(4) 0.5540(12) 1.000 0.1050 . . H252 H Uiso 0.3774(15) 0.5109(19) 0.599(3) 1.000 0.1050 . . 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 Cu1 0.0431(3) 0.0433(3) 0.0428(3) 0.0008(3) 0.0009(3) -0.0014(3) N1 0.046(2) 0.045(3) 0.044(2) 0.006(2) 0.0002(19) -0.004(2) N2 0.044(2) 0.049(3) 0.051(3) 0.009(2) 0.003(2) 0.000(2) N3 0.048(3) 0.049(3) 0.048(3) 0.003(2) 0.003(2) -0.002(2) N4 0.044(2) 0.053(3) 0.048(3) -0.001(2) -0.002(2) -0.002(2) N5 0.076(3) 0.054(3) 0.059(3) 0.002(2) 0.007(3) -0.003(3) N6 0.073(3) 0.049(3) 0.060(3) 0.009(2) 0.009(3) 0.004(3) C1 0.068(4) 0.063(4) 0.051(3) 0.013(3) 0.001(3) 0.007(3) C2 0.084(5) 0.068(4) 0.051(3) 0.019(3) 0.012(3) -0.002(4) C3 0.073(4) 0.084(5) 0.080(5) 0.018(4) 0.037(4) 0.005(4) C4 0.056(4) 0.069(4) 0.074(4) 0.011(4) 0.013(3) 0.017(3) C5 0.046(3) 0.045(3) 0.047(3) -0.003(3) -0.003(3) 0.006(2) C6 0.047(3) 0.042(3) 0.048(3) 0.005(2) -0.002(3) 0.001(2) C7 0.058(4) 0.069(4) 0.057(3) 0.007(3) 0.005(3) 0.017(3) C8 0.079(5) 0.092(5) 0.056(4) 0.016(3) -0.008(4) 0.025(4) C9 0.084(5) 0.070(4) 0.053(4) 0.022(3) 0.008(4) 0.006(4) C10 0.060(4) 0.063(4) 0.055(4) 0.006(3) 0.012(3) 0.002(3) C11 0.056(4) 0.072(4) 0.061(4) -0.002(3) 0.019(3) -0.009(3) C12 0.078(5) 0.071(4) 0.060(4) -0.016(3) -0.001(4) -0.005(4) C13 0.083(5) 0.064(4) 0.063(4) -0.018(3) -0.012(4) -0.003(3) C14 0.042(3) 0.065(4) 0.081(5) 0.000(3) -0.002(3) -0.010(3) C15 0.040(3) 0.041(3) 0.057(3) 0.002(3) 0.002(3) 0.003(2) C16 0.049(3) 0.048(3) 0.063(4) 0.005(3) -0.004(3) 0.005(3) C17 0.066(4) 0.080(5) 0.081(5) -0.001(4) 0.027(4) -0.014(4) C18 0.083(5) 0.097(5) 0.077(5) 0.005(4) 0.034(4) 0.002(5) C19 0.095(6) 0.083(5) 0.057(4) -0.002(4) 0.012(4) 0.012(4) C20 0.071(4) 0.069(4) 0.056(4) -0.007(3) 0.003(3) 0.005(3) C21 0.080(5) 0.074(5) 0.081(5) -0.005(4) -0.009(4) 0.003(4) C22 0.090(5) 0.096(6) 0.079(5) 0.020(5) -0.010(4) 0.021(5) C23 0.114(6) 0.069(5) 0.073(5) 0.000(4) -0.002(5) 0.024(5) C24 0.102(6) 0.055(4) 0.067(4) -0.001(3) 0.004(4) 0.006(4) C25 0.072(4) 0.047(3) 0.050(3) 0.003(3) 0.013(3) 0.006(3) C26 0.061(4) 0.040(3) 0.060(3) -0.001(3) 0.011(3) 0.003(2) C27 0.105(6) 0.043(4) 0.082(5) -0.010(3) 0.004(4) -0.001(4) C28 0.097(6) 0.070(5) 0.069(5) -0.015(4) 0.012(4) -0.015(4) C29 0.083(5) 0.082(5) 0.056(4) -0.004(4) 0.006(4) -0.001(4) C30 0.093(5) 0.053(4) 0.070(5) 0.004(3) 0.009(4) -0.001(4) Cu2 0.0513(4) 0.0422(3) 0.0411(3) 0.0013(3) -0.0017(3) -0.0020(3) N7 0.054(3) 0.049(3) 0.043(3) -0.004(2) 0.004(2) -0.002(2) N8 0.060(3) 0.052(3) 0.041(2) -0.003(2) -0.001(2) 0.008(2) N9 0.047(3) 0.053(3) 0.052(3) 0.001(2) -0.002(2) -0.002(2) N10 0.064(3) 0.059(3) 0.058(3) 0.000(3) -0.009(2) 0.002(3) N11 0.069(3) 0.050(3) 0.060(3) 0.006(2) -0.008(3) -0.005(2) N12 0.067(3) 0.045(3) 0.059(4) 0.001(2) 0.001(2) 0.000(2) C31 0.075(4) 0.073(4) 0.058(4) -0.001(3) -0.006(3) -0.017(3) C32 0.114(6) 0.071(5) 0.071(5) -0.004(4) -0.022(5) -0.014(5) C33 0.082(5) 0.090(5) 0.089(5) -0.001(4) -0.036(5) -0.017(5) C34 0.064(4) 0.079(5) 0.098(5) 0.000(4) -0.022(4) 0.007(4) C35 0.048(3) 0.052(3) 0.054(3) 0.007(3) 0.000(3) -0.003(3) C36 0.056(4) 0.046(3) 0.052(3) 0.004(3) 0.008(3) 0.007(3) C37 0.075(4) 0.082(5) 0.072(5) 0.002(4) 0.020(4) 0.023(4) C38 0.105(6) 0.080(5) 0.065(5) -0.004(4) 0.030(4) 0.027(4) C39 0.160(9) 0.071(5) 0.040(4) -0.012(3) 0.008(5) 0.027(5) C40 0.091(5) 0.063(4) 0.057(4) -0.003(3) -0.009(4) 0.011(4) C41 0.052(3) 0.071(4) 0.061(4) -0.002(3) -0.005(3) -0.004(3) C42 0.081(5) 0.074(4) 0.054(4) 0.010(3) 0.008(4) -0.004(4) C43 0.091(5) 0.073(4) 0.072(4) 0.010(4) 0.019(4) -0.018(4) C44 0.060(4) 0.078(4) 0.078(4) -0.011(4) 0.007(4) -0.014(4) C45 0.042(3) 0.055(3) 0.059(4) -0.008(3) 0.001(3) -0.007(3) C46 0.051(3) 0.055(3) 0.056(4) -0.014(3) -0.004(3) 0.001(3) C47 0.070(4) 0.079(5) 0.088(5) -0.011(4) -0.018(4) -0.005(4) C48 0.112(7) 0.109(7) 0.081(6) -0.020(5) -0.053(5) 0.016(6) C49 0.131(7) 0.080(5) 0.067(4) -0.002(4) -0.039(5) 0.034(5) C50 0.105(6) 0.064(4) 0.060(4) 0.004(4) -0.013(4) 0.003(4) C51 0.089(5) 0.068(5) 0.077(5) 0.005(4) 0.005(4) -0.008(4) C52 0.094(6) 0.099(6) 0.076(5) -0.006(5) 0.017(4) 0.012(5) C53 0.122(7) 0.060(5) 0.088(6) -0.013(4) 0.025(5) 0.016(4) C54 0.109(6) 0.053(4) 0.080(5) -0.005(4) 0.000(5) 0.009(4) C55 0.063(4) 0.047(3) 0.064(4) 0.006(3) -0.010(3) 0.000(3) C56 0.067(4) 0.038(3) 0.052(3) 0.001(3) -0.019(3) 0.002(3) C57 0.099(5) 0.045(3) 0.072(5) 0.008(3) -0.001(4) 0.001(3) C58 0.133(7) 0.050(4) 0.057(4) 0.004(3) 0.007(4) -0.013(4) C59 0.076(5) 0.085(5) 0.057(4) 0.002(4) 0.003(3) 0.000(4) C60 0.097(5) 0.057(4) 0.057(4) 0.017(3) 0.008(4) 0.004(4) Nb1 0.0405(2) 0.0519(3) 0.0435(2) 0.0031(2) -0.0065(2) 0.0035(2) O1 0.091(3) 0.054(2) 0.081(3) 0.005(2) -0.010(3) 0.003(2) O2 0.0356(16) 0.080(3) 0.043(2) 0.008(2) -0.0040(16) 0.009(2) O3 0.0405(18) 0.075(3) 0.048(2) -0.001(2) -0.0109(16) 0.0108(19) O4 0.0447(19) 0.088(3) 0.047(2) 0.005(2) -0.0058(17) 0.006(2) O5 0.0402(18) 0.091(3) 0.055(2) -0.001(2) 0.0013(19) 0.012(2) O6 0.056(2) 0.085(3) 0.049(2) 0.014(2) -0.0090(19) 0.005(2) O7 0.046(2) 0.105(4) 0.046(2) 0.000(2) -0.0024(18) 0.012(2) O8 0.068(3) 0.136(5) 0.043(3) -0.007(3) 0.003(2) -0.006(3) O9 0.083(4) 0.179(6) 0.081(4) -0.020(4) 0.002(3) 0.059(4) O10 0.049(2) 0.066(3) 0.056(2) 0.008(2) -0.0120(18) 0.015(2) O11 0.072(3) 0.055(2) 0.058(2) 0.013(2) -0.009(2) 0.0050(19) O12 0.061(3) 0.149(5) 0.073(3) 0.019(3) -0.022(3) -0.025(3) O13 0.147(5) 0.088(4) 0.091(4) 0.015(3) -0.036(4) -0.048(4) C61 0.047(3) 0.041(3) 0.043(3) -0.002(2) -0.006(2) 0.002(2) C62 0.040(2) 0.045(3) 0.052(3) -0.011(3) -0.001(3) 0.003(2) C63 0.052(3) 0.077(4) 0.050(4) -0.008(3) -0.002(3) -0.008(3) C64 0.055(4) 0.098(5) 0.052(4) 0.001(4) -0.002(3) 0.008(3) C65 0.049(4) 0.095(5) 0.039(3) 0.010(3) -0.001(3) -0.014(3) C66 0.081(5) 0.076(5) 0.045(3) 0.002(3) -0.010(3) -0.016(4) O14 0.097(4) 0.088(4) 0.107(4) -0.003(3) 0.009(3) 0.017(3) O15 0.138(6) 0.104(4) 0.142(6) 0.027(5) 0.007(5) 0.002(4) O16 0.147(7) 0.119(5) 0.265(11) -0.005(6) 0.062(8) 0.003(5) O17 0.106(5) 0.106(4) 0.161(6) 0.009(5) 0.008(5) 0.017(4) O18 0.117(5) 0.138(5) 0.133(5) -0.025(5) -0.026(5) -0.007(4) O19 0.093(4) 0.092(4) 0.146(6) -0.001(4) -0.029(4) 0.017(3) O20 0.190(7) 0.137(5) 0.100(5) -0.029(4) -0.044(5) 0.088(5) O21 0.121(6) 0.137(6) 0.168(7) -0.013(5) 0.001(6) 0.012(5) O22 0.066(3) 0.096(4) 0.136(5) 0.029(4) 0.000(3) -0.005(3) O23 0.079(4) 0.103(4) 0.170(6) 0.015(5) -0.010(4) 0.021(3) O24 0.315(16) 0.386(19) 0.167(10) -0.021(11) -0.038(11) -0.184(15) O25 0.084(3) 0.116(4) 0.063(3) -0.016(3) 0.009(2) -0.007(3) Cl1 0.154(2) 0.1173(17) 0.1083(17) 0.0091(14) 0.0111(18) 0.0329(18) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O7 2.099(5) . . no Nb1 O10 2.093(3) . . no Nb1 O11 2.202(4) . . no Nb1 O3 2.168(3) . . no Nb1 O1 1.717(4) . . no Nb1 O2 2.119(4) . . no Nb1 O6 2.141(4) . . no Cu1 N4 2.042(5) . . no Cu1 N1 2.060(4) . . no Cu1 N2 2.181(5) . . no Cu1 N3 2.115(5) . . no Cu1 N5 2.186(5) . . no Cu1 N6 2.162(5) . . no Cu2 N7 2.075(4) . . no Cu2 N8 2.205(5) . . no Cu2 N9 2.057(5) . . no Cu2 N10 2.085(5) . . no Cu2 N11 2.243(5) . . no Cu2 N12 2.085(5) . . no O2 C61 1.287(6) . . no O3 C62 1.287(6) . . no O4 C61 1.219(6) . . no O5 C62 1.212(6) . . no O6 C63 1.285(7) . . no O7 C64 1.294(8) . . no O8 C63 1.208(8) . . no O9 C64 1.217(9) . . no O10 C65 1.273(8) . . no O11 C66 1.270(9) . . no O12 C65 1.242(8) . . no O13 C66 1.234(9) . . no O14 H142 0.84(4) . . no O14 H141 0.84(5) . . no O15 H151 0.85(7) . . no O15 H152 0.84(5) . . no N1 C5 1.348(6) . . no N1 C1 1.341(8) . . no N2 C10 1.322(8) . . no N2 C6 1.327(7) . . no N3 C15 1.341(7) . . no N3 C11 1.356(8) . . no N4 C20 1.340(8) . . no N4 C16 1.343(8) . . no N5 C21 1.333(9) . . no N5 C25 1.361(8) . . no N6 C30 1.325(9) . . no N6 C26 1.350(7) . . no O16 H161 0.8700 . . no O16 H162 0.85(2) . . no N7 C35 1.340(8) . . no N7 C31 1.343(8) . . no N8 C40 1.364(8) . . no N8 C36 1.315(8) . . no N9 C41 1.340(8) . . no N9 C45 1.345(8) . . no N10 C50 1.361(8) . . no N10 C46 1.329(8) . . no N11 C55 1.333(8) . . no N11 C51 1.346(8) . . no N12 C60 1.359(9) . . no N12 C56 1.329(7) . . no O17 H171 0.86(5) . . no O17 H172 0.84(8) . . no O18 H182 0.8855 . . no O18 H181 0.86(4) . . no O19 H192 0.86(5) . . no O19 H191 0.83(4) . . no O20 H202 0.83(5) . . no O20 H201 0.84(4) . . no C1 C2 1.347(10) . . no C2 C3 1.375(10) . . no C3 C4 1.385(10) . . no C4 C5 1.344(8) . . no C5 C6 1.493(6) . . no C6 C7 1.402(8) . . no C7 C8 1.377(10) . . no C8 C9 1.344(10) . . no C9 C10 1.385(10) . . no C11 C12 1.356(10) . . no C12 C13 1.310(10) . . no C13 C14 1.408(10) . . no C14 C15 1.392(8) . . no C15 C16 1.477(9) . . no C16 C17 1.379(10) . . no C17 C18 1.389(10) . . no C18 C19 1.352(11) . . no C19 C20 1.396(10) . . no C21 C22 1.419(11) . . no C22 C23 1.339(13) . . no C23 C24 1.368(11) . . no C24 C25 1.396(9) . . no C25 C26 1.466(9) . . no C26 C27 1.389(9) . . no C27 C28 1.380(10) . . no C28 C29 1.361(10) . . no C29 C30 1.354(10) . . no C1 H1 0.9304 . . no C2 H2 0.9278 . . no C3 H3 0.9303 . . no C4 H4 0.9302 . . no C7 H7 0.9311 . . no C8 H8 0.9296 . . no C9 H9 0.9293 . . no C10 H10 0.9281 . . no C11 H11 0.9306 . . no C12 H12 0.9297 . . no C13 H13 0.9304 . . no C14 H14 0.9309 . . no C17 H17 0.9304 . . no C18 H18 0.9299 . . no C19 H19 0.9303 . . no C20 H20 0.9300 . . no C21 H21 0.9296 . . no O21 H212 0.8980 . . no O21 H211 0.83(3) . . no C22 H22 0.9290 . . no C23 H23 0.9296 . . no C24 H24 0.9297 . . no C27 H27 0.9298 . . no C28 H28 0.9303 . . no C29 H29 0.9313 . . no C30 H30 0.9288 . . no C31 C32 1.380(11) . . no C32 C33 1.368(12) . . no C33 C34 1.377(12) . . no C34 C35 1.371(10) . . no C35 C36 1.515(9) . . no C36 C37 1.358(9) . . no C37 C38 1.395(10) . . no C38 C39 1.333(13) . . no C39 C40 1.367(11) . . no C41 C42 1.366(10) . . no C42 C43 1.364(10) . . no C43 C44 1.405(10) . . no C44 C45 1.390(10) . . no C45 C46 1.481(9) . . no C46 C47 1.369(10) . . no C47 C48 1.373(13) . . no C48 C49 1.373(14) . . no C49 C50 1.368(12) . . no C51 C52 1.338(11) . . no C52 C53 1.390(13) . . no C53 C54 1.354(12) . . no C54 C55 1.393(10) . . no C55 C56 1.489(9) . . no C56 C57 1.369(9) . . no C57 C58 1.375(10) . . no C58 C59 1.336(11) . . no C59 C60 1.381(11) . . no O22 H221 0.84(5) . . no O22 H222 0.84(4) . . no C31 H31 0.9294 . . no C32 H32 0.9298 . . no C33 H33 0.9305 . . no C34 H34 0.9296 . . no C37 H37 0.9298 . . no C38 H38 0.9316 . . no C39 H39 0.9288 . . no C40 H40 0.9301 . . no C41 H41 0.9304 . . no C42 H42 0.9305 . . no C43 H43 0.9295 . . no C44 H44 0.9297 . . no C47 H47 0.9294 . . no C48 H48 0.9299 . . no C49 H49 0.9296 . . no C50 H50 0.9305 . . no C51 H51 0.9303 . . no C52 H52 0.9304 . . no C53 H53 0.9307 . . no C54 H54 0.9311 . . no C57 H57 0.9280 . . no C58 H58 0.9311 . . no C59 H59 0.9301 . . no C60 H60 0.9312 . . no C61 C62 1.528(6) . . no C63 C64 1.513(9) . . no C65 C66 1.525(10) . . no O23 H231 0.85(5) . . no O23 H232 0.84(4) . . no O24 H241 0.9274 . . no O24 H242 0.834(14) . . no O25 H251 0.83(3) . . no O25 H252 0.84(3) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O10 142.36(14) . . . no O2 Nb1 O11 91.87(16) . . . no O3 Nb1 O6 144.18(12) . . . no O3 Nb1 O7 138.64(14) . . . no O3 Nb1 O10 71.79(13) . . . no O3 Nb1 O11 82.09(16) . . . no O6 Nb1 O7 72.52(14) . . . no O6 Nb1 O10 72.65(13) . . . no O6 Nb1 O11 84.28(16) . . . no O7 Nb1 O10 141.05(15) . . . no O7 Nb1 O11 85.73(17) . . . no O10 Nb1 O11 73.99(16) . . . no O1 Nb1 O6 92.89(19) . . . no O1 Nb1 O7 103.62(19) . . . no O1 Nb1 O10 95.00(19) . . . no O1 Nb1 O11 168.98(19) . . . no O2 Nb1 O3 71.80(12) . . . no O2 Nb1 O6 141.77(13) . . . no O2 Nb1 O7 69.27(14) . . . no O1 Nb1 O3 94.25(19) . . . no O1 Nb1 O2 96.87(19) . . . no N1 Cu1 N3 94.74(18) . . . no N1 Cu1 N4 169.57(18) . . . no N1 Cu1 N6 91.13(19) . . . no N2 Cu1 N3 97.24(17) . . . no N1 Cu1 N5 95.85(19) . . . no N1 Cu1 N2 77.96(17) . . . no N4 Cu1 N5 92.48(19) . . . no N4 Cu1 N6 97.00(19) . . . no N5 Cu1 N6 75.80(18) . . . no N3 Cu1 N6 169.95(19) . . . no N2 Cu1 N5 166.28(19) . . . no N2 Cu1 N6 91.95(18) . . . no N2 Cu1 N4 95.19(17) . . . no N3 Cu1 N5 95.46(18) . . . no N3 Cu1 N4 78.19(18) . . . no N7 Cu2 N8 76.17(17) . . . no N11 Cu2 N12 75.60(18) . . . no N8 Cu2 N10 93.19(17) . . . no N8 Cu2 N11 170.21(17) . . . no N7 Cu2 N9 96.53(18) . . . no N7 Cu2 N10 168.19(18) . . . no N7 Cu2 N11 98.64(17) . . . no N7 Cu2 N12 91.7(2) . . . no N8 Cu2 N9 95.76(17) . . . no N10 Cu2 N12 94.6(2) . . . no N9 Cu2 N10 79.22(18) . . . no N9 Cu2 N11 93.06(17) . . . no N8 Cu2 N12 96.08(18) . . . no N10 Cu2 N11 92.62(17) . . . no N9 Cu2 N12 166.9(2) . . . no Nb1 O2 C61 122.3(3) . . . no Nb1 O3 C62 120.9(3) . . . no Nb1 O6 C63 120.9(4) . . . no Nb1 O7 C64 120.6(4) . . . no Nb1 O10 C65 120.2(4) . . . no Nb1 O11 C66 116.4(4) . . . no H141 O14 H142 103(7) . . . no H151 O15 H152 104(5) . . . no Cu1 N1 C5 117.3(3) . . . no Cu1 N1 C1 124.5(4) . . . no C1 N1 C5 118.3(5) . . . no Cu1 N2 C6 112.2(3) . . . no Cu1 N2 C10 127.3(4) . . . no C6 N2 C10 119.8(5) . . . no Cu1 N3 C15 114.1(4) . . . no Cu1 N3 C11 127.8(4) . . . no C11 N3 C15 118.2(5) . . . no Cu1 N4 C16 117.2(4) . . . no Cu1 N4 C20 123.7(4) . . . no C16 N4 C20 119.0(5) . . . no Cu1 N5 C25 114.9(4) . . . no Cu1 N5 C21 126.1(4) . . . no C21 N5 C25 118.8(5) . . . no Cu1 N6 C26 116.1(4) . . . no C26 N6 C30 117.5(5) . . . no Cu1 N6 C30 126.3(4) . . . no H161 O16 H162 101.72 . . . no Cu2 N7 C31 122.9(4) . . . no C31 N7 C35 118.7(5) . . . no Cu2 N7 C35 118.4(4) . . . no Cu2 N8 C40 126.8(4) . . . no C36 N8 C40 118.1(5) . . . no Cu2 N8 C36 114.8(4) . . . no C41 N9 C45 118.4(5) . . . no Cu2 N9 C45 114.9(4) . . . no Cu2 N9 C41 126.8(4) . . . no C46 N10 C50 119.5(5) . . . no Cu2 N10 C50 126.0(4) . . . no Cu2 N10 C46 114.5(4) . . . no Cu2 N11 C55 113.5(4) . . . no C51 N11 C55 117.6(5) . . . no Cu2 N11 C51 128.8(4) . . . no Cu2 N12 C56 118.7(4) . . . no C56 N12 C60 118.9(5) . . . no Cu2 N12 C60 122.1(4) . . . no H171 O17 H172 102(8) . . . no H181 O18 H182 99.89 . . . no H191 O19 H192 102(8) . . . no H201 O20 H202 104(6) . . . no N1 C1 C2 122.7(6) . . . no C1 C2 C3 118.9(6) . . . no C2 C3 C4 118.6(6) . . . no C3 C4 C5 119.7(6) . . . no N1 C5 C6 114.5(4) . . . no C4 C5 C6 123.7(5) . . . no N1 C5 C4 121.7(5) . . . no N2 C6 C5 117.6(4) . . . no C5 C6 C7 121.9(5) . . . no N2 C6 C7 120.5(5) . . . no C6 C7 C8 118.1(6) . . . no C7 C8 C9 121.1(6) . . . no C8 C9 C10 117.6(6) . . . no N2 C10 C9 122.8(6) . . . no N3 C11 C12 122.1(6) . . . no C11 C12 C13 121.3(6) . . . no C12 C13 C14 118.8(6) . . . no C13 C14 C15 118.7(6) . . . no C14 C15 C16 123.2(5) . . . no N3 C15 C16 115.9(5) . . . no N3 C15 C14 120.9(6) . . . no N4 C16 C17 122.0(6) . . . no N4 C16 C15 114.5(5) . . . no C15 C16 C17 123.5(6) . . . no C16 C17 C18 118.4(7) . . . no C17 C18 C19 119.8(7) . . . no C18 C19 C20 119.2(6) . . . no N4 C20 C19 121.4(6) . . . no N5 C21 C22 121.4(6) . . . no C21 C22 C23 119.8(8) . . . no C22 C23 C24 119.1(8) . . . no C23 C24 C25 120.4(7) . . . no C24 C25 C26 123.2(6) . . . no N5 C25 C24 120.5(6) . . . no N5 C25 C26 116.3(5) . . . no N6 C26 C25 116.5(5) . . . no C25 C26 C27 122.1(5) . . . no N6 C26 C27 121.4(6) . . . no C26 C27 C28 118.9(6) . . . no C27 C28 C29 119.0(6) . . . no C28 C29 C30 118.9(7) . . . no N6 C30 C29 124.3(6) . . . no N1 C1 H1 118.62 . . . no C2 C1 H1 118.65 . . . no C1 C2 H2 120.50 . . . no C3 C2 H2 120.56 . . . no C4 C3 H3 120.75 . . . no C2 C3 H3 120.64 . . . no C5 C4 H4 120.24 . . . no C3 C4 H4 120.06 . . . no C8 C7 H7 120.97 . . . no C6 C7 H7 120.89 . . . no C9 C8 H8 119.52 . . . no C7 C8 H8 119.40 . . . no C8 C9 H9 121.13 . . . no C10 C9 H9 121.28 . . . no C9 C10 H10 118.64 . . . no N2 C10 H10 118.53 . . . no N3 C11 H11 119.02 . . . no C12 C11 H11 118.90 . . . no C13 C12 H12 119.40 . . . no C11 C12 H12 119.28 . . . no C12 C13 H13 120.51 . . . no C14 C13 H13 120.66 . . . no C13 C14 H14 120.63 . . . no C15 C14 H14 120.68 . . . no C18 C17 H17 120.82 . . . no C16 C17 H17 120.75 . . . no C17 C18 H18 120.16 . . . no C19 C18 H18 120.07 . . . no C18 C19 H19 120.43 . . . no C20 C19 H19 120.37 . . . no C19 C20 H20 119.38 . . . no N4 C20 H20 119.20 . . . no C22 C21 H21 119.32 . . . no N5 C21 H21 119.33 . . . no H211 O21 H212 100.07 . . . no C21 C22 H22 120.13 . . . no C23 C22 H22 120.04 . . . no C24 C23 H23 120.32 . . . no C22 C23 H23 120.56 . . . no C25 C24 H24 119.89 . . . no C23 C24 H24 119.72 . . . no C28 C27 H27 120.51 . . . no C26 C27 H27 120.59 . . . no C27 C28 H28 120.42 . . . no C29 C28 H28 120.58 . . . no C30 C29 H29 120.58 . . . no C28 C29 H29 120.50 . . . no N6 C30 H30 117.95 . . . no C29 C30 H30 117.80 . . . no N7 C31 C32 121.9(6) . . . no C31 C32 C33 118.6(7) . . . no C32 C33 C34 120.0(8) . . . no C33 C34 C35 118.5(7) . . . no C34 C35 C36 122.6(6) . . . no N7 C35 C36 115.1(5) . . . no N7 C35 C34 122.3(6) . . . no N8 C36 C35 115.0(5) . . . no N8 C36 C37 123.0(6) . . . no C35 C36 C37 122.0(6) . . . no C36 C37 C38 118.3(7) . . . no C37 C38 C39 119.4(7) . . . no C38 C39 C40 119.7(7) . . . no N8 C40 C39 121.3(7) . . . no N9 C41 C42 123.5(6) . . . no C41 C42 C43 119.3(6) . . . no C42 C43 C44 118.5(6) . . . no C43 C44 C45 119.2(7) . . . no C44 C45 C46 123.1(6) . . . no N9 C45 C46 115.7(5) . . . no N9 C45 C44 121.2(6) . . . no N10 C46 C47 120.8(6) . . . no C45 C46 C47 123.4(6) . . . no N10 C46 C45 115.7(5) . . . no C46 C47 C48 120.5(7) . . . no C47 C48 C49 118.5(9) . . . no C48 C49 C50 119.4(7) . . . no N10 C50 C49 121.2(6) . . . no N11 C51 C52 124.7(7) . . . no C51 C52 C53 117.7(8) . . . no C52 C53 C54 119.2(8) . . . no C53 C54 C55 119.9(7) . . . no C54 C55 C56 123.4(6) . . . no N11 C55 C56 115.7(5) . . . no N11 C55 C54 120.9(6) . . . no C55 C56 C57 122.9(5) . . . no N12 C56 C57 120.8(6) . . . no N12 C56 C55 116.2(5) . . . no C56 C57 C58 120.4(6) . . . no C57 C58 C59 118.9(7) . . . no C58 C59 C60 119.8(7) . . . no N12 C60 C59 121.0(6) . . . no H221 O22 H222 105(6) . . . no N7 C31 H31 119.01 . . . no C32 C31 H31 119.13 . . . no C31 C32 H32 120.71 . . . no C33 C32 H32 120.68 . . . no C34 C33 H33 119.99 . . . no C32 C33 H33 120.00 . . . no C33 C34 H34 120.72 . . . no C35 C34 H34 120.76 . . . no C38 C37 H37 120.88 . . . no C36 C37 H37 120.81 . . . no C37 C38 H38 120.30 . . . no C39 C38 H38 120.31 . . . no C38 C39 H39 120.18 . . . no C40 C39 H39 120.10 . . . no C39 C40 H40 119.24 . . . no N8 C40 H40 119.43 . . . no N9 C41 H41 118.30 . . . no C42 C41 H41 118.25 . . . no C43 C42 H42 120.22 . . . no C41 C42 H42 120.49 . . . no C42 C43 H43 120.78 . . . no C44 C43 H43 120.77 . . . no C45 C44 H44 120.29 . . . no C43 C44 H44 120.51 . . . no C46 C47 H47 119.81 . . . no C48 C47 H47 119.72 . . . no C49 C48 H48 120.68 . . . no C47 C48 H48 120.79 . . . no C50 C49 H49 120.24 . . . no C48 C49 H49 120.39 . . . no C49 C50 H50 119.33 . . . no N10 C50 H50 119.46 . . . no C52 C51 H51 117.74 . . . no N11 C51 H51 117.56 . . . no C51 C52 H52 121.14 . . . no C53 C52 H52 121.19 . . . no C54 C53 H53 120.20 . . . no C52 C53 H53 120.60 . . . no C55 C54 H54 120.06 . . . no C53 C54 H54 120.06 . . . no C58 C57 H57 119.76 . . . no C56 C57 H57 119.81 . . . no C59 C58 H58 120.50 . . . no C57 C58 H58 120.59 . . . no C58 C59 H59 120.07 . . . no C60 C59 H59 120.09 . . . no N12 C60 H60 119.53 . . . no C59 C60 H60 119.43 . . . no O4 C61 C62 121.5(4) . . . no O2 C61 O4 125.6(4) . . . no O2 C61 C62 112.9(4) . . . no O3 C62 C61 112.1(4) . . . no O5 C62 C61 120.9(4) . . . no O3 C62 O5 126.9(4) . . . no O6 C63 O8 125.1(6) . . . no O8 C63 C64 123.4(6) . . . no O6 C63 C64 111.6(5) . . . no O7 C64 O9 126.4(6) . . . no O9 C64 C63 120.2(6) . . . no O7 C64 C63 113.4(5) . . . no O10 C65 C66 114.7(5) . . . no O12 C65 C66 121.4(6) . . . no O10 C65 O12 123.9(6) . . . no O13 C66 C65 121.4(7) . . . no O11 C66 O13 124.0(7) . . . no O11 C66 C65 114.6(6) . . . no H231 O23 H232 104(5) . . . no H241 O24 H242 97.66 . . . no H251 O25 H252 106(6) . . . no 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 O11 Nb1 O2 C61 -81.2(4) . . . . no O1 Nb1 O3 C62 -96.8(4) . . . . no O2 Nb1 O3 C62 -0.9(4) . . . . no O6 Nb1 O3 C62 162.3(3) . . . . no O7 Nb1 O3 C62 19.5(5) . . . . no O10 Nb1 O3 C62 169.4(4) . . . . no O11 Nb1 O3 C62 93.7(4) . . . . no O1 Nb1 O6 C63 103.9(5) . . . . no O2 Nb1 O6 C63 -1.0(6) . . . . no O3 Nb1 O6 C63 -154.8(4) . . . . no O7 Nb1 O6 C63 0.5(4) . . . . no O10 Nb1 O6 C63 -161.8(5) . . . . no O11 Nb1 O6 C63 -86.8(5) . . . . no O1 Nb1 O7 C64 -96.0(5) . . . . no O2 Nb1 O7 C64 171.7(5) . . . . no O3 Nb1 O7 C64 151.0(4) . . . . no O6 Nb1 O7 C64 -7.2(4) . . . . no O10 Nb1 O7 C64 20.3(6) . . . . no O11 Nb1 O7 C64 78.1(5) . . . . no O1 Nb1 O10 C65 -179.6(5) . . . . no O2 Nb1 O10 C65 -71.6(5) . . . . no O3 Nb1 O10 C65 -86.8(4) . . . . no O6 Nb1 O10 C65 88.9(4) . . . . no O7 Nb1 O10 C65 61.4(5) . . . . no O11 Nb1 O10 C65 0.0(4) . . . . no O2 Nb1 O11 C66 141.9(4) . . . . no O1 Nb1 O2 C61 92.1(4) . . . . no O3 Nb1 O2 C61 -0.2(4) . . . . no O6 Nb1 O2 C61 -164.3(3) . . . . no O7 Nb1 O2 C61 -165.9(4) . . . . no O10 Nb1 O2 C61 -15.4(6) . . . . no O10 Nb1 O11 C66 -2.7(4) . . . . no O3 Nb1 O11 C66 70.5(4) . . . . no O6 Nb1 O11 C66 -76.3(4) . . . . no O7 Nb1 O11 C66 -149.1(5) . . . . no N2 Cu1 N1 C5 -4.2(4) . . . . no N3 Cu1 N1 C1 79.3(5) . . . . no N3 Cu1 N1 C5 -100.7(4) . . . . no N2 Cu1 N1 C1 175.7(5) . . . . no N1 Cu1 N2 C6 5.6(3) . . . . no N1 Cu1 N2 C10 176.2(5) . . . . no N3 Cu1 N2 C6 98.9(4) . . . . no N5 Cu1 N1 C1 -16.7(5) . . . . no N5 Cu1 N1 C5 163.4(4) . . . . no N6 Cu1 N1 C1 -92.5(5) . . . . no N6 Cu1 N1 C5 87.5(4) . . . . no N6 Cu1 N2 C10 85.4(5) . . . . no N1 Cu1 N3 C11 -8.5(5) . . . . no N1 Cu1 N3 C15 172.1(4) . . . . no N2 Cu1 N3 C11 -86.9(5) . . . . no N2 Cu1 N3 C15 93.7(4) . . . . no N4 Cu1 N3 C11 179.3(5) . . . . no N4 Cu1 N3 C15 -0.1(4) . . . . no N5 Cu1 N3 C11 87.9(5) . . . . no N5 Cu1 N3 C15 -91.5(4) . . . . no N2 Cu1 N4 C16 -94.5(4) . . . . no N2 Cu1 N4 C20 83.2(5) . . . . no N3 Cu1 N2 C10 -90.5(5) . . . . no N4 Cu1 N2 C6 177.6(4) . . . . no N4 Cu1 N2 C10 -11.8(5) . . . . no N6 Cu1 N2 C6 -85.2(4) . . . . no N5 Cu1 N4 C16 96.9(4) . . . . no N5 Cu1 N4 C20 -85.4(5) . . . . no N6 Cu1 N4 C16 172.9(4) . . . . no N6 Cu1 N4 C20 -9.4(5) . . . . no N1 Cu1 N5 C21 90.6(6) . . . . no N1 Cu1 N5 C25 -84.1(4) . . . . no N3 Cu1 N5 C21 -4.8(6) . . . . no N3 Cu1 N5 C25 -179.5(4) . . . . no N4 Cu1 N5 C21 -83.1(6) . . . . no N4 Cu1 N5 C25 102.2(5) . . . . no N6 Cu1 N5 C21 -179.7(6) . . . . no N6 Cu1 N5 C25 5.6(4) . . . . no N1 Cu1 N6 C26 91.7(5) . . . . no N1 Cu1 N6 C30 -88.7(6) . . . . no N2 Cu1 N6 C26 169.7(5) . . . . no N2 Cu1 N6 C30 -10.7(6) . . . . no N4 Cu1 N6 C26 -94.9(5) . . . . no N4 Cu1 N6 C30 84.8(6) . . . . no N5 Cu1 N6 C26 -4.1(4) . . . . no N5 Cu1 N6 C30 175.6(6) . . . . no N3 Cu1 N4 C20 179.5(5) . . . . no N3 Cu1 N4 C16 1.8(4) . . . . no N11 Cu2 N7 C35 167.9(4) . . . . no N11 Cu2 N7 C31 -12.2(5) . . . . no N7 Cu2 N8 C36 6.4(4) . . . . no N7 Cu2 N8 C40 179.8(5) . . . . no N9 Cu2 N8 C36 101.8(4) . . . . no N9 Cu2 N8 C40 -84.9(5) . . . . no N10 Cu2 N8 C36 -178.8(4) . . . . no N12 Cu2 N7 C31 -87.9(5) . . . . no N12 Cu2 N7 C35 92.2(4) . . . . no N11 Cu2 N12 C60 178.8(6) . . . . no N12 Cu2 N8 C40 89.5(5) . . . . no N7 Cu2 N9 C41 -12.8(5) . . . . no N7 Cu2 N9 C45 169.0(4) . . . . no N8 Cu2 N9 C41 -89.4(5) . . . . no N8 Cu2 N9 C45 92.3(4) . . . . no N10 Cu2 N9 C41 178.4(5) . . . . no N10 Cu2 N9 C45 0.1(4) . . . . no N11 Cu2 N9 C41 86.3(5) . . . . no N11 Cu2 N9 C45 -92.0(4) . . . . no N8 Cu2 N10 C46 -95.0(4) . . . . no N8 Cu2 N10 C50 83.1(5) . . . . no N9 Cu2 N10 C46 0.3(4) . . . . no N9 Cu2 N10 C50 178.3(5) . . . . no N11 Cu2 N10 C46 92.9(4) . . . . no N11 Cu2 N10 C50 -89.0(5) . . . . no N8 Cu2 N7 C31 176.3(5) . . . . no N8 Cu2 N7 C35 -3.6(4) . . . . no N9 Cu2 N7 C31 81.9(5) . . . . no N9 Cu2 N7 C35 -98.0(4) . . . . no N9 Cu2 N11 C55 170.2(4) . . . . no N10 Cu2 N11 C51 -86.2(5) . . . . no N10 Cu2 N11 C55 90.8(4) . . . . no N12 Cu2 N11 C51 179.8(6) . . . . no N12 Cu2 N11 C55 -3.2(4) . . . . no N7 Cu2 N12 C56 103.4(5) . . . . no N7 Cu2 N12 C60 -82.7(5) . . . . no N8 Cu2 N12 C56 179.6(5) . . . . no N8 Cu2 N12 C60 -6.4(5) . . . . no N10 Cu2 N12 C56 -86.7(5) . . . . no N10 Cu2 N12 C60 87.3(5) . . . . no N11 Cu2 N12 C56 4.9(5) . . . . no N12 Cu2 N10 C46 168.6(4) . . . . no N12 Cu2 N10 C50 -13.3(5) . . . . no N7 Cu2 N11 C51 90.3(5) . . . . no N7 Cu2 N11 C55 -92.7(4) . . . . no N9 Cu2 N11 C51 -6.8(5) . . . . no N12 Cu2 N8 C36 -83.8(4) . . . . no N10 Cu2 N8 C40 -5.4(5) . . . . no Nb1 O2 C61 O4 179.9(4) . . . . no Nb1 O2 C61 C62 1.0(6) . . . . no Nb1 O3 C62 O5 -179.0(4) . . . . no Nb1 O3 C62 C61 1.6(5) . . . . no Nb1 O6 C63 O8 -176.3(6) . . . . no Nb1 O6 C63 C64 4.9(7) . . . . no Nb1 O7 C64 O9 -165.3(6) . . . . no Nb1 O7 C64 C63 11.8(7) . . . . no Nb1 O10 C65 C66 2.3(7) . . . . no Nb1 O10 C65 O12 -179.7(5) . . . . no Nb1 O11 C66 O13 -175.8(6) . . . . no Nb1 O11 C66 C65 4.6(7) . . . . no C1 N1 C5 C4 -0.1(8) . . . . no C1 N1 C5 C6 -177.6(5) . . . . no C5 N1 C1 C2 1.6(9) . . . . no Cu1 N1 C1 C2 -178.4(5) . . . . no Cu1 N1 C5 C4 179.9(4) . . . . no Cu1 N1 C5 C6 2.4(5) . . . . no Cu1 N2 C6 C7 172.9(4) . . . . no C6 N2 C10 C9 -2.0(9) . . . . no Cu1 N2 C10 C9 -171.9(5) . . . . no C10 N2 C6 C7 1.6(8) . . . . no Cu1 N2 C6 C5 -6.2(5) . . . . no C10 N2 C6 C5 -177.6(5) . . . . no Cu1 N3 C11 C12 -177.8(5) . . . . no C11 N3 C15 C16 179.1(5) . . . . no Cu1 N3 C15 C14 179.1(4) . . . . no C15 N3 C11 C12 1.6(9) . . . . no C11 N3 C15 C14 -0.4(8) . . . . no Cu1 N3 C15 C16 -1.4(6) . . . . no Cu1 N4 C16 C15 -3.1(7) . . . . no C16 N4 C20 C19 -0.9(9) . . . . no Cu1 N4 C16 C17 178.3(5) . . . . no C20 N4 C16 C15 179.1(5) . . . . no C20 N4 C16 C17 0.4(9) . . . . no Cu1 N4 C20 C19 -178.5(5) . . . . no Cu1 N5 C21 C22 -173.7(6) . . . . no C21 N5 C25 C26 178.6(6) . . . . no Cu1 N5 C25 C24 172.4(5) . . . . no C25 N5 C21 C22 0.8(10) . . . . no C21 N5 C25 C24 -2.7(9) . . . . no Cu1 N5 C25 C26 -6.3(7) . . . . no C30 N6 C26 C27 0.0(10) . . . . no Cu1 N6 C30 C29 -179.7(6) . . . . no C30 N6 C26 C25 -177.5(6) . . . . no Cu1 N6 C26 C25 2.1(7) . . . . no Cu1 N6 C26 C27 179.7(5) . . . . no C26 N6 C30 C29 0.0(10) . . . . no C31 N7 C35 C34 0.0(9) . . . . no C35 N7 C31 C32 -0.4(9) . . . . no C31 N7 C35 C36 -179.2(5) . . . . no Cu2 N7 C35 C36 0.8(7) . . . . no Cu2 N7 C31 C32 179.7(5) . . . . no Cu2 N7 C35 C34 180.0(5) . . . . no C36 N8 C40 C39 -0.6(9) . . . . no Cu2 N8 C36 C37 172.0(5) . . . . no C40 N8 C36 C37 -2.0(8) . . . . no Cu2 N8 C36 C35 -7.9(6) . . . . no C40 N8 C36 C35 178.1(5) . . . . no Cu2 N8 C40 C39 -173.8(5) . . . . no Cu2 N9 C45 C44 178.3(5) . . . . no Cu2 N9 C41 C42 -176.7(5) . . . . no C41 N9 C45 C46 -178.9(6) . . . . no Cu2 N9 C45 C46 -0.4(7) . . . . no C41 N9 C45 C44 -0.2(9) . . . . no C45 N9 C41 C42 1.5(9) . . . . no C50 N10 C46 C47 -1.2(9) . . . . no Cu2 N10 C50 C49 -177.3(6) . . . . no C50 N10 C46 C45 -178.8(6) . . . . no Cu2 N10 C46 C45 -0.5(7) . . . . no C46 N10 C50 C49 0.7(10) . . . . no Cu2 N10 C46 C47 177.1(5) . . . . no Cu2 N11 C55 C54 -178.8(5) . . . . no C51 N11 C55 C56 178.8(6) . . . . no Cu2 N11 C55 C56 1.4(7) . . . . no C51 N11 C55 C54 -1.5(9) . . . . no C55 N11 C51 C52 -0.2(10) . . . . no Cu2 N11 C51 C52 176.7(6) . . . . no C60 N12 C56 C57 1.9(10) . . . . no C56 N12 C60 C59 0.5(10) . . . . no Cu2 N12 C56 C55 -5.8(7) . . . . no C60 N12 C56 C55 -179.9(6) . . . . no Cu2 N12 C60 C59 -173.4(5) . . . . no Cu2 N12 C56 C57 176.1(5) . . . . no N1 C1 C2 C3 -1.6(10) . . . . no C1 C2 C3 C4 0.2(10) . . . . no C2 C3 C4 C5 1.3(10) . . . . no C3 C4 C5 C6 176.0(5) . . . . no C3 C4 C5 N1 -1.3(9) . . . . no N1 C5 C6 N2 2.9(6) . . . . no C4 C5 C6 C7 6.2(8) . . . . no C4 C5 C6 N2 -174.7(5) . . . . no N1 C5 C6 C7 -176.2(5) . . . . no N2 C6 C7 C8 0.4(9) . . . . no C5 C6 C7 C8 179.5(5) . . . . no C6 C7 C8 C9 -2.1(10) . . . . no C7 C8 C9 C10 1.8(10) . . . . no C8 C9 C10 N2 0.3(10) . . . . no N3 C11 C12 C13 -0.8(11) . . . . no C11 C12 C13 C14 -1.3(11) . . . . no C12 C13 C14 C15 2.4(10) . . . . no C13 C14 C15 C16 179.0(6) . . . . no C13 C14 C15 N3 -1.6(9) . . . . no C14 C15 C16 C17 1.1(10) . . . . no N3 C15 C16 C17 -178.4(6) . . . . no N3 C15 C16 N4 2.9(8) . . . . no C14 C15 C16 N4 -177.6(5) . . . . no C15 C16 C17 C18 -176.2(6) . . . . no N4 C16 C17 C18 2.4(10) . . . . no C16 C17 C18 C19 -4.8(11) . . . . no C17 C18 C19 C20 4.4(11) . . . . no C18 C19 C20 N4 -1.6(11) . . . . no N5 C21 C22 C23 1.1(12) . . . . no C21 C22 C23 C24 -1.1(13) . . . . no C22 C23 C24 C25 -0.7(12) . . . . no C23 C24 C25 C26 -178.6(7) . . . . no C23 C24 C25 N5 2.7(11) . . . . no N5 C25 C26 C27 -174.7(6) . . . . no C24 C25 C26 N6 -175.9(6) . . . . no C24 C25 C26 C27 6.7(10) . . . . no N5 C25 C26 N6 2.8(8) . . . . no C25 C26 C27 C28 176.5(7) . . . . no N6 C26 C27 C28 -0.9(11) . . . . no C26 C27 C28 C29 1.9(11) . . . . no C27 C28 C29 C30 -1.9(11) . . . . no C28 C29 C30 N6 1.0(11) . . . . no N7 C31 C32 C33 0.0(11) . . . . no C31 C32 C33 C34 0.7(12) . . . . no C32 C33 C34 C35 -1.0(12) . . . . no C33 C34 C35 C36 179.8(7) . . . . no C33 C34 C35 N7 0.7(11) . . . . no C34 C35 C36 C37 5.9(10) . . . . no N7 C35 C36 N8 5.0(8) . . . . no N7 C35 C36 C37 -174.9(6) . . . . no C34 C35 C36 N8 -174.2(6) . . . . no N8 C36 C37 C38 1.1(9) . . . . no C35 C36 C37 C38 -179.0(6) . . . . no C36 C37 C38 C39 2.5(10) . . . . no C37 C38 C39 C40 -5.0(10) . . . . no C38 C39 C40 N8 4.2(10) . . . . no N9 C41 C42 C43 -2.2(10) . . . . no C41 C42 C43 C44 1.4(10) . . . . no C42 C43 C44 C45 -0.1(10) . . . . no C43 C44 C45 C46 178.1(6) . . . . no C43 C44 C45 N9 -0.5(10) . . . . no N9 C45 C46 C47 -176.9(6) . . . . no C44 C45 C46 C47 4.4(11) . . . . no N9 C45 C46 N10 0.7(8) . . . . no C44 C45 C46 N10 -178.0(6) . . . . no N10 C46 C47 C48 -0.7(11) . . . . no C45 C46 C47 C48 176.7(8) . . . . no C46 C47 C48 C49 2.9(13) . . . . no C47 C48 C49 C50 -3.3(14) . . . . no C48 C49 C50 N10 1.5(12) . . . . no N11 C51 C52 C53 1.7(13) . . . . no C51 C52 C53 C54 -1.5(13) . . . . no C52 C53 C54 C55 -0.1(13) . . . . no C53 C54 C55 C56 -178.6(7) . . . . no C53 C54 C55 N11 1.6(11) . . . . no C54 C55 C56 C57 1.0(10) . . . . no C54 C55 C56 N12 -177.1(7) . . . . no N11 C55 C56 N12 2.7(8) . . . . no N11 C55 C56 C57 -179.2(6) . . . . no N12 C56 C57 C58 -3.1(11) . . . . no C55 C56 C57 C58 178.8(7) . . . . no C56 C57 C58 C59 1.8(12) . . . . no C57 C58 C59 C60 0.6(12) . . . . no C58 C59 C60 N12 -1.8(11) . . . . no O2 C61 C62 O5 179.0(5) . . . . no O4 C61 C62 O3 179.4(5) . . . . no O4 C61 C62 O5 0.0(7) . . . . no O2 C61 C62 O3 -1.6(6) . . . . no O8 C63 C64 O7 170.7(7) . . . . no O6 C63 C64 O9 166.9(6) . . . . no O8 C63 C64 O9 -11.9(11) . . . . no O6 C63 C64 O7 -10.4(8) . . . . no O10 C65 C66 O11 -4.6(9) . . . . no O12 C65 C66 O13 -2.2(11) . . . . no O10 C65 C66 O13 175.8(6) . . . . no O12 C65 C66 O11 177.4(6) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O14 H141 O1 0.84(5) 2.11(5) 2.939(6) 168(8) . no O14 H142 O15 0.84(4) 2.03(4) 2.850(10) 164(4) . no O15 H151 O17 0.85(7) 2.05(5) 2.786(10) 146(8) 4_556 no O15 H152 O16 0.84(5) 1.97(3) 2.752(10) 154(5) . no O16 H161 O10 0.8700 2.5800 3.285(9) 139.00 . no O16 H161 O12 0.8700 2.1900 3.004(10) 157.00 . no O16 H162 Cl1 0.85(2) 2.245(9) 3.070(9) 165(6) 1_455 no O17 H171 O11 0.86(5) 2.27(5) 3.072(8) 156(6) . no O17 H171 O13 0.86(5) 2.44(6) 3.141(10) 140(5) . no O17 H172 O18 0.84(8) 1.99(8) 2.771(12) 153(8) . no O18 H181 O9 0.86(4) 2.34(2) 3.171(9) 166(6) . no O18 H182 O20 0.8900 1.7800 2.597(11) 153.00 4_646 no O19 H191 O9 0.83(4) 2.03(4) 2.848(8) 168(8) . no O19 H192 Cl1 0.86(5) 2.46(4) 3.314(7) 172(8) . no O20 H201 Cl1 0.84(4) 2.33(3) 3.156(9) 166(6) . no O20 H202 O21 0.83(5) 1.99(5) 2.796(12) 164(5) . no O21 H211 O22 0.83(3) 2.25(4) 2.758(8) 120(3) . no O21 H212 O24 0.9000 2.1700 3.021(11) 159.00 . no O22 H221 O19 0.84(5) 2.00(5) 2.793(8) 158(7) 4_656 no O22 H222 O23 0.84(4) 1.97(3) 2.748(8) 155(7) . no O23 H231 O14 0.85(5) 2.00(3) 2.808(8) 160(6) . no O23 H232 O12 0.84(4) 2.59(4) 3.381(9) 159(6) 4_556 no O23 H232 O13 0.84(4) 2.35(7) 2.896(9) 124(7) 4_556 no O24 H241 Cl1 0.9300 2.3500 3.270(13) 169.00 . no O24 H242 O25 0.834(14) 2.380(15) 2.953(10) 126.5(15) . no O25 H251 O5 0.83(3) 2.00(3) 2.821(6) 166(5) 2_564 no O25 H252 O8 0.84(3) 2.06(4) 2.861(7) 161(4) . no C4 H4 O5 0.9300 2.4500 3.349(7) 164.00 1_655 no C7 H7 O5 0.9300 2.5900 3.482(7) 160.00 1_655 no C14 H14 O4 0.9300 2.5700 3.449(7) 157.00 . no C37 H37 O4 0.9300 2.6000 3.489(8) 161.00 . no C38 H38 O6 0.9300 2.4100 3.260(8) 152.00 2_565 no C39 H39 O12 0.9300 2.5800 3.504(9) 172.00 2_565 no C44 H44 O5 0.9300 2.3800 3.291(8) 165.00 1_655 no C60 H60 N8 0.9300 2.6200 3.220(8) 123.00 . no #=============================================================================== data_VII _database_code_depnum_ccdc_archive 'CCDC 648558' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H24 N6 Zn), C6 Nb O13, 11(H2 O), Cl' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural '(C30 H24 N6 Zn)2, (C6 Nb O13), 11(H2 O), Cl' _chemical_formula_sum 'C66 H70 Cl N12 Nb O24 Zn2' _chemical_formula_iupac ? _chemical_formula_weight 1674.44 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 24.070(2) _cell_length_b 13.3320(10) _cell_length_c 23.168(2) _cell_angle_alpha 90 _cell_angle_beta 102.190(10) _cell_angle_gamma 90 _cell_volume 7267.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 43343 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 30.52 _cell_special_details ; ? ; _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.933 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.95 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(3) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius-Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 43343 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 30.52 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 22113 # number of observed reflections (> n sig(I)) _reflns_number_gt 14954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software (Nonius, 1998)' _computing_cell_refinement 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0492P)^2^+2.3516P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 22113 _refine_ls_number_parameters 1033 _refine_ls_number_restraints 48 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.770 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.068 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Zn1 Zn Uani 0.08114(1) 0.34285(2) 0.25597(1) 1.000 0.0279(1) . . N1 N Uani 0.08119(7) 0.21023(13) 0.20373(8) 1.000 0.0298(5) . . N2 N Uani 0.14948(7) 0.25454(13) 0.30681(8) 1.000 0.0295(5) . . N3 N Uani 0.13587(8) 0.42617(14) 0.20955(8) 1.000 0.0331(5) . . N4 N Uani 0.10066(7) 0.47669(13) 0.30689(8) 1.000 0.0294(5) . . N5 N Uani 0.00183(7) 0.39624(13) 0.20423(7) 1.000 0.0292(5) . . N6 N Uani 0.01905(7) 0.28669(13) 0.30274(7) 1.000 0.0286(5) . . C1 C Uani 0.04645(10) 0.19292(18) 0.15105(10) 1.000 0.0368(7) . . C2 C Uani 0.04881(10) 0.10656(18) 0.11947(10) 1.000 0.0407(7) . . C3 C Uani 0.08759(11) 0.03363(18) 0.14272(10) 1.000 0.0415(7) . . C4 C Uani 0.12301(10) 0.04961(17) 0.19724(10) 1.000 0.0364(7) . . C5 C Uani 0.11942(8) 0.13948(16) 0.22652(9) 1.000 0.0278(6) . . C6 C Uani 0.15730(8) 0.16398(16) 0.28428(9) 1.000 0.0288(6) . . C7 C Uani 0.19823(9) 0.09831(18) 0.31381(10) 1.000 0.0385(7) . . C8 C Uani 0.23180(10) 0.1260(2) 0.36691(11) 1.000 0.0440(8) . . C9 C Uani 0.22393(10) 0.2189(2) 0.39020(10) 1.000 0.0415(8) . . C10 C Uani 0.18254(9) 0.28068(19) 0.35903(9) 1.000 0.0356(7) . . C11 C Uani 0.15155(11) 0.3970(2) 0.16008(11) 1.000 0.0462(8) . . C12 C Uani 0.18388(12) 0.4561(2) 0.13110(12) 1.000 0.0520(9) . . C13 C Uani 0.20057(11) 0.5487(2) 0.15366(12) 1.000 0.0514(9) . . C14 C Uani 0.18550(10) 0.57962(19) 0.20537(11) 1.000 0.0420(8) . . C15 C Uani 0.15329(9) 0.51602(16) 0.23258(9) 1.000 0.0307(6) . . C16 C Uani 0.13534(8) 0.54327(16) 0.28826(9) 1.000 0.0295(6) . . C17 C Uani 0.15231(10) 0.63034(18) 0.31939(11) 1.000 0.0389(7) . . C18 C Uani 0.13326(11) 0.65008(19) 0.37038(11) 1.000 0.0431(8) . . C19 C Uani 0.09751(10) 0.58295(19) 0.38915(11) 1.000 0.0408(8) . . C20 C Uani 0.08228(10) 0.49762(18) 0.35631(10) 1.000 0.0356(7) . . C21 C Uani -0.00469(10) 0.44760(17) 0.15339(10) 1.000 0.0348(7) . . C22 C Uani -0.05697(10) 0.47004(17) 0.11867(10) 1.000 0.0363(7) . . C23 C Uani -0.10521(10) 0.44020(18) 0.13716(10) 1.000 0.0363(7) . . C24 C Uani -0.09937(9) 0.38839(17) 0.18986(10) 1.000 0.0343(7) . . C25 C Uani -0.04541(9) 0.36705(15) 0.22263(9) 1.000 0.0273(6) . . C26 C Uani -0.03560(9) 0.30966(15) 0.27878(9) 1.000 0.0279(6) . . C27 C Uani -0.07963(10) 0.28137(18) 0.30556(10) 1.000 0.0350(7) . . C28 C Uani -0.06687(10) 0.22855(18) 0.35854(10) 1.000 0.0380(7) . . C29 C Uani -0.01142(10) 0.20421(17) 0.38227(10) 1.000 0.0366(7) . . C30 C Uani 0.03031(10) 0.23427(16) 0.35336(9) 1.000 0.0335(7) . . Zn2 Zn Uani 0.41868(1) 0.24450(2) 0.21590(1) 1.000 0.0310(1) . . N7 N Uani 0.41052(8) 0.38514(14) 0.17065(8) 1.000 0.0341(6) . . N8 N Uani 0.37932(8) 0.34156(16) 0.27173(9) 1.000 0.0401(6) . . N9 N Uani 0.33621(8) 0.19293(14) 0.17012(9) 1.000 0.0352(6) . . N10 N Uani 0.40436(8) 0.11547(15) 0.26587(9) 1.000 0.0381(6) . . N11 N Uani 0.46698(7) 0.17199(13) 0.16042(8) 1.000 0.0310(5) . . N12 N Uani 0.50459(7) 0.27392(14) 0.26029(8) 1.000 0.0317(5) . . C31 C Uani 0.43214(10) 0.40562(19) 0.12308(10) 1.000 0.0408(7) . . C32 C Uani 0.42478(12) 0.4966(2) 0.09419(12) 1.000 0.0516(9) . . C33 C Uani 0.39323(15) 0.5681(2) 0.11510(14) 1.000 0.0656(10) . . C34 C Uani 0.37041(13) 0.5485(2) 0.16391(14) 1.000 0.0572(10) . . C35 C Uani 0.38023(10) 0.45560(18) 0.19163(11) 1.000 0.0388(7) . . C36 C Uani 0.35968(9) 0.42930(18) 0.24560(11) 1.000 0.0398(7) . . C37 C Uani 0.32345(12) 0.4892(2) 0.26918(14) 1.000 0.0571(10) . . C38 C Uani 0.30745(13) 0.4612(3) 0.32028(16) 1.000 0.0655(11) . . C39 C Uani 0.32847(13) 0.3739(3) 0.34809(14) 1.000 0.0619(11) . . C40 C Uani 0.36431(12) 0.3160(2) 0.32227(12) 1.000 0.0528(9) . . C41 C Uani 0.30440(10) 0.2322(2) 0.12066(11) 1.000 0.0428(8) . . C42 C Uani 0.25208(11) 0.1945(2) 0.09398(12) 1.000 0.0522(9) . . C43 C Uani 0.23165(12) 0.1126(3) 0.11849(13) 1.000 0.0601(10) . . C44 C Uani 0.26399(11) 0.0707(2) 0.16959(12) 1.000 0.0530(9) . . C45 C Uani 0.31577(9) 0.11334(18) 0.19490(11) 1.000 0.0362(7) . . C46 C Uani 0.35229(9) 0.07539(17) 0.25080(10) 1.000 0.0349(7) . . C47 C Uani 0.33399(11) 0.00379(19) 0.28641(12) 1.000 0.0449(8) . . C48 C Uani 0.36996(12) -0.0250(2) 0.33808(12) 1.000 0.0501(9) . . C49 C Uani 0.42330(12) 0.0154(2) 0.35333(13) 1.000 0.0522(9) . . C50 C Uani 0.43894(11) 0.0850(2) 0.31588(12) 1.000 0.0506(9) . . C51 C Uani 0.44634(10) 0.11520(18) 0.11258(11) 1.000 0.0384(7) . . C52 C Uani 0.48042(11) 0.06396(19) 0.08188(11) 1.000 0.0433(8) . . C53 C Uani 0.53827(11) 0.0718(2) 0.10073(11) 1.000 0.0447(8) . . C54 C Uani 0.56046(10) 0.13052(19) 0.14910(11) 1.000 0.0407(8) . . C55 C Uani 0.52369(9) 0.18024(16) 0.17815(9) 1.000 0.0303(6) . . C56 C Uani 0.54431(9) 0.24417(16) 0.23111(9) 1.000 0.0306(6) . . C57 C Uani 0.60065(9) 0.27257(19) 0.24952(10) 1.000 0.0377(7) . . C58 C Uani 0.61649(11) 0.33177(19) 0.29947(11) 1.000 0.0427(8) . . C59 C Uani 0.57598(11) 0.36149(19) 0.32972(11) 1.000 0.0422(8) . . C60 C Uani 0.52039(10) 0.33099(19) 0.30862(10) 1.000 0.0393(7) . . Nb1 Nb Uani 0.33811(1) 0.68536(1) 0.49882(1) 1.000 0.0282(1) . . O1 O Uani 0.32710(7) 0.72426(13) 0.56603(7) 1.000 0.0383(5) . . O2 O Uani 0.42525(6) 0.65684(12) 0.52852(7) 1.000 0.0366(5) . . O3 O Uani 0.38415(7) 0.81348(11) 0.47735(7) 1.000 0.0379(5) . . O4 O Uani 0.51426(7) 0.71417(15) 0.54785(9) 1.000 0.0574(7) . . O5 O Uani 0.46942(8) 0.87753(15) 0.47337(9) 1.000 0.0596(7) . . O6 O Uani 0.25650(6) 0.61139(13) 0.48210(7) 1.000 0.0412(5) . . O7 O Uani 0.35290(6) 0.52996(12) 0.50787(7) 1.000 0.0373(5) . . O8 O Uani 0.20986(9) 0.46654(19) 0.47003(12) 1.000 0.0866(9) . . O9 O Uani 0.31791(9) 0.37500(14) 0.49244(9) 1.000 0.0550(7) . . O10 O Uani 0.27770(6) 0.79030(12) 0.45471(7) 1.000 0.0359(5) . . O11 O Uani 0.32991(6) 0.65718(11) 0.40375(6) 1.000 0.0327(5) . . O12 O Uani 0.23461(7) 0.85519(13) 0.36811(7) 1.000 0.0457(6) . . O13 O Uani 0.29210(7) 0.71651(13) 0.31383(7) 1.000 0.0398(5) . . C61 C Uani 0.46398(10) 0.72200(18) 0.52491(10) 1.000 0.0363(7) . . C62 C Uani 0.43920(10) 0.81395(18) 0.48830(10) 1.000 0.0378(7) . . C63 C Uani 0.25358(10) 0.5154(2) 0.48022(11) 1.000 0.0462(8) . . C64 C Uani 0.31212(10) 0.46539(19) 0.49411(10) 1.000 0.0383(8) . . C65 C Uani 0.26689(9) 0.79589(17) 0.39793(9) 1.000 0.0314(6) . . C66 C Uani 0.29867(9) 0.71701(16) 0.36782(9) 1.000 0.0295(6) . . O17 O Uani 0.12517(10) 0.1476(2) 0.48067(12) 1.000 0.0786(10) . . O18 O Uani 0.12001(11) 0.34906(19) 0.49007(16) 1.000 0.0906(12) . . O19 O Uani 0.00875(9) 0.41673(14) 0.46596(8) 1.000 0.0518(6) . . O20 O Uani 0.03630(11) 0.0767(2) 0.52770(12) 1.000 0.0886(11) . . O14 O Uani 0.39118(11) 0.20370(19) 0.49120(17) 1.000 0.0984(12) . . O15 O Uani 0.33028(8) 0.02623(16) 0.46757(10) 1.000 0.0574(7) . . O16 O Uani 0.22926(13) 0.0493(2) 0.50851(13) 1.000 0.0871(11) . . O21 O Uani 0.19025(11) 0.8576(2) 0.51450(12) 1.000 0.0800(10) . . O22 O Uani 0.15430(11) 0.60725(19) 0.55345(10) 1.000 0.0718(9) . . O23 O Uani 0.21587(7) 0.85769(13) 0.23841(7) 1.000 0.0402(5) . . O24 O Uani 0.24152(10) 0.7980(2) 0.13377(9) 1.000 0.0751(9) . . Cl1 Cl Uani 0.06331(3) 0.75991(5) 0.48659(3) 1.000 0.0484(2) . . H1 H Uiso 0.01980 0.24150 0.13540 1.000 0.0440 calc R H2 H Uiso 0.02460 0.09740 0.08290 1.000 0.0490 calc R H3 H Uiso 0.08990 -0.02550 0.12210 1.000 0.0500 calc R H4 H Uiso 0.14900 0.00070 0.21410 1.000 0.0440 calc R H7 H Uiso 0.20290 0.03580 0.29770 1.000 0.0460 calc R H8 H Uiso 0.25950 0.08270 0.38700 1.000 0.0530 calc R H9 H Uiso 0.24610 0.23920 0.42620 1.000 0.0500 calc R H10 H Uiso 0.17710 0.34330 0.37470 1.000 0.0430 calc R H11 H Uiso 0.14010 0.33420 0.14460 1.000 0.0550 calc R H12 H Uiso 0.19420 0.43340 0.09690 1.000 0.0630 calc R H13 H Uiso 0.22180 0.59050 0.13450 1.000 0.0620 calc R H14 H Uiso 0.19680 0.64210 0.22160 1.000 0.0500 calc R H17 H Uiso 0.17640 0.67530 0.30610 1.000 0.0470 calc R H18 H Uiso 0.14450 0.70820 0.39180 1.000 0.0520 calc R H19 H Uiso 0.08400 0.59500 0.42320 1.000 0.0490 calc R H20 H Uiso 0.05810 0.45220 0.36900 1.000 0.0430 calc R H21 H Uiso 0.02770 0.46900 0.14110 1.000 0.0420 calc R H22 H Uiso -0.05970 0.50470 0.08340 1.000 0.0440 calc R H23 H Uiso -0.14110 0.45460 0.11460 1.000 0.0440 calc R H24 H Uiso -0.13140 0.36800 0.20320 1.000 0.0410 calc R H27 H Uiso -0.11710 0.29750 0.28840 1.000 0.0420 calc R H28 H Uiso -0.09560 0.21000 0.37760 1.000 0.0460 calc R H29 H Uiso -0.00210 0.16800 0.41730 1.000 0.0440 calc R H30 H Uiso 0.06790 0.21750 0.36960 1.000 0.0400 calc R H31 H Uiso 0.45310 0.35610 0.10900 1.000 0.0490 calc R H32 H Uiso 0.44070 0.50890 0.06160 1.000 0.0620 calc R H33 H Uiso 0.38710 0.63010 0.09640 1.000 0.0790 calc R H34 H Uiso 0.34880 0.59680 0.17810 1.000 0.0690 calc R H37 H Uiso 0.30980 0.54870 0.25040 1.000 0.0690 calc R H38 H Uiso 0.28250 0.50100 0.33600 1.000 0.0790 calc R H39 H Uiso 0.31890 0.35430 0.38330 1.000 0.0740 calc R H40 H Uiso 0.37860 0.25670 0.34080 1.000 0.0630 calc R H41 H Uiso 0.31840 0.28740 0.10370 1.000 0.0510 calc R H42 H Uiso 0.23100 0.22410 0.06000 1.000 0.0630 calc R H43 H Uiso 0.19650 0.08530 0.10110 1.000 0.0720 calc R H44 H Uiso 0.25100 0.01460 0.18660 1.000 0.0640 calc R H47 H Uiso 0.29790 -0.02420 0.27540 1.000 0.0540 calc R H48 H Uiso 0.35800 -0.07190 0.36260 1.000 0.0600 calc R H49 H Uiso 0.44820 -0.00370 0.38800 1.000 0.0630 calc R H50 H Uiso 0.47530 0.11220 0.32580 1.000 0.0610 calc R H51 H Uiso 0.40710 0.11040 0.09970 1.000 0.0460 calc R H52 H Uiso 0.46470 0.02500 0.04920 1.000 0.0520 calc R H53 H Uiso 0.56240 0.03760 0.08100 1.000 0.0540 calc R H54 H Uiso 0.59960 0.13680 0.16210 1.000 0.0490 calc R H57 H Uiso 0.62760 0.25210 0.22850 1.000 0.0450 calc R H58 H Uiso 0.65420 0.35120 0.31240 1.000 0.0510 calc R H59 H Uiso 0.58560 0.40100 0.36340 1.000 0.0510 calc R H60 H Uiso 0.49280 0.35100 0.32890 1.000 0.0470 calc R H171 H Uiso 0.1582(7) 0.124(3) 0.4875(15) 1.000 0.0940 . . H172 H Uiso 0.1120(9) 0.131(4) 0.5103(8) 0.500 0.0940 . . H173 H Uiso 0.1295(19) 0.2061(8) 0.4949(15) 0.500 0.0940 . . H181 H Uiso 0.1426(14) 0.386(2) 0.4784(17) 1.000 0.1090 . . H182 H Uiso 0.123(3) 0.2923(7) 0.4754(16) 0.500 0.1090 . . H183 H Uiso 0.0919(18) 0.385(3) 0.492(4) 0.500 0.1090 . . H191 H Uiso -0.0114(10) 0.3752(17) 0.4781(13) 1.000 0.0620 . . H192 H Uiso 0.0417(7) 0.394(3) 0.475(3) 0.500 0.0620 . . H193 H Uiso 0.011(2) 0.466(2) 0.488(2) 0.500 0.0620 . . H201 H Uiso 0.0093(5) 0.1131(9) 0.5315(11) 1.000 0.1060 . . H202 H Uiso 0.0236(8) 0.0170(9) 0.5228(14) 0.500 0.1060 . . H203 H Uiso 0.0599(19) 0.115(2) 0.516(3) 0.500 0.1060 . . H141 H Uiso 0.3762(15) 0.2606(15) 0.492(2) 1.000 0.1180 . . H142 H Uiso 0.4232(9) 0.217(3) 0.484(2) 1.000 0.1180 . . H151 H Uiso 0.3534(10) 0.0736(13) 0.4748(14) 1.000 0.0690 . . H152 H Uiso 0.3499(10) -0.0256(12) 0.4791(14) 1.000 0.0690 . . H161 H Uiso 0.2622(8) 0.049(3) 0.5019(18) 1.000 0.1050 . . H162 H Uiso 0.2210(15) -0.0121(11) 0.5099(19) 1.000 0.1050 . . H211 H Uiso 0.1562(6) 0.838(3) 0.5059(16) 1.000 0.0960 . . H212 H Uiso 0.2055(12) 0.827(3) 0.4900(13) 1.000 0.0960 . . H221 H Uiso 0.1291(12) 0.648(2) 0.5373(13) 1.000 0.0860 . . H222 H Uiso 0.1647(14) 0.579(2) 0.5255(10) 1.000 0.0860 . . H231 H Uiso 0.2333(10) 0.8264(18) 0.2678(6) 1.000 0.0480 . . H232 H Uiso 0.2315(10) 0.8405(19) 0.2111(7) 1.000 0.0480 . . H241 H Uiso 0.2662(10) 0.784(3) 0.1143(12) 1.000 0.0900 . . H242 H Uiso 0.2138(9) 0.819(3) 0.1085(11) 1.000 0.0900 . . 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 Zn1 0.0286(1) 0.0270(1) 0.0277(1) -0.0025(1) 0.0051(1) 0.0000(1) N1 0.0297(9) 0.0292(9) 0.0285(9) -0.0041(7) 0.0019(7) 0.0006(7) N2 0.0265(8) 0.0316(9) 0.0288(9) -0.0026(7) 0.0025(7) -0.0014(7) N3 0.0335(9) 0.0383(10) 0.0292(9) -0.0029(8) 0.0104(7) -0.0025(8) N4 0.0304(9) 0.0280(9) 0.0298(9) -0.0020(7) 0.0067(7) -0.0014(7) N5 0.0321(9) 0.0265(9) 0.0289(9) 0.0016(7) 0.0062(7) 0.0018(7) N6 0.0318(9) 0.0251(9) 0.0282(9) 0.0008(7) 0.0046(7) -0.0007(7) C1 0.0368(12) 0.0395(13) 0.0303(11) -0.0043(10) -0.0013(9) 0.0047(10) C2 0.0458(13) 0.0428(14) 0.0303(11) -0.0082(10) 0.0005(10) -0.0033(11) C3 0.0525(14) 0.0337(12) 0.0378(12) -0.0119(10) 0.0086(11) -0.0012(11) C4 0.0405(12) 0.0292(11) 0.0395(12) -0.0025(10) 0.0085(10) 0.0051(10) C5 0.0267(10) 0.0278(11) 0.0295(10) -0.0008(8) 0.0072(8) -0.0006(8) C6 0.0248(10) 0.0321(11) 0.0299(10) 0.0014(9) 0.0068(8) 0.0003(8) C7 0.0347(12) 0.0358(13) 0.0440(13) 0.0007(10) 0.0059(10) 0.0068(10) C8 0.0325(12) 0.0524(16) 0.0430(14) 0.0097(12) -0.0011(10) 0.0062(11) C9 0.0322(12) 0.0581(16) 0.0303(11) 0.0010(11) -0.0019(9) -0.0071(11) C10 0.0335(11) 0.0416(13) 0.0297(11) -0.0034(10) 0.0024(9) -0.0027(10) C11 0.0505(15) 0.0528(16) 0.0390(13) -0.0081(12) 0.0181(11) -0.0039(12) C12 0.0519(15) 0.071(2) 0.0385(13) -0.0025(13) 0.0216(12) -0.0033(14) C13 0.0468(15) 0.0634(18) 0.0477(15) 0.0122(13) 0.0186(12) -0.0077(13) C14 0.0399(13) 0.0405(14) 0.0467(14) 0.0051(11) 0.0114(11) -0.0021(11) C15 0.0260(10) 0.0324(11) 0.0326(11) 0.0033(9) 0.0034(8) 0.0021(9) C16 0.0264(10) 0.0289(11) 0.0321(11) -0.0005(9) 0.0036(8) 0.0013(8) C17 0.0394(12) 0.0315(12) 0.0436(13) -0.0018(10) 0.0039(10) -0.0062(10) C18 0.0488(14) 0.0337(12) 0.0430(14) -0.0106(11) 0.0010(11) -0.0014(11) C19 0.0436(13) 0.0423(14) 0.0368(12) -0.0103(10) 0.0095(10) 0.0038(11) C20 0.0382(12) 0.0365(12) 0.0338(11) -0.0038(10) 0.0117(9) 0.0008(10) C21 0.0364(12) 0.0360(12) 0.0330(11) 0.0053(9) 0.0094(9) 0.0021(10) C22 0.0452(13) 0.0332(12) 0.0291(11) 0.0046(9) 0.0048(10) 0.0052(10) C23 0.0345(12) 0.0390(13) 0.0312(11) 0.0003(10) -0.0024(9) 0.0052(10) C24 0.0303(11) 0.0377(12) 0.0344(11) 0.0005(10) 0.0055(9) -0.0002(9) C25 0.0297(10) 0.0249(10) 0.0275(10) -0.0009(8) 0.0068(8) 0.0002(8) C26 0.0305(10) 0.0258(10) 0.0260(10) -0.0021(8) 0.0031(8) -0.0010(8) C27 0.0319(11) 0.0397(12) 0.0342(12) 0.0016(10) 0.0090(9) -0.0030(9) C28 0.0411(13) 0.0414(13) 0.0340(12) -0.0004(10) 0.0138(10) -0.0060(10) C29 0.0486(14) 0.0338(12) 0.0275(11) 0.0029(9) 0.0084(10) -0.0002(10) C30 0.0365(11) 0.0328(12) 0.0298(11) 0.0033(9) 0.0041(9) 0.0019(9) Zn2 0.0277(1) 0.0289(1) 0.0367(1) 0.0042(1) 0.0075(1) 0.0004(1) N7 0.0338(10) 0.0283(9) 0.0381(10) 0.0016(8) 0.0028(8) -0.0010(8) N8 0.0357(10) 0.0431(12) 0.0431(11) -0.0052(9) 0.0123(9) 0.0006(9) N9 0.0305(9) 0.0344(10) 0.0410(11) 0.0002(8) 0.0086(8) -0.0003(8) N10 0.0305(10) 0.0386(11) 0.0462(11) 0.0109(9) 0.0104(8) 0.0011(8) N11 0.0290(9) 0.0291(9) 0.0352(9) 0.0002(8) 0.0073(7) -0.0018(7) N12 0.0297(9) 0.0350(10) 0.0299(9) 0.0026(8) 0.0053(7) -0.0002(8) C31 0.0443(13) 0.0388(13) 0.0369(12) 0.0070(10) 0.0029(10) -0.0043(11) C32 0.0630(17) 0.0442(15) 0.0418(14) 0.0142(12) -0.0020(12) -0.0070(13) C33 0.089(2) 0.0420(16) 0.0568(18) 0.0178(14) -0.0047(17) 0.0025(16) C34 0.0660(18) 0.0359(14) 0.0619(18) -0.0005(13) -0.0039(14) 0.0149(13) C35 0.0344(12) 0.0322(12) 0.0449(13) -0.0038(10) -0.0030(10) 0.0000(10) C36 0.0304(11) 0.0340(12) 0.0517(14) -0.0121(11) 0.0012(10) 0.0003(9) C37 0.0484(15) 0.0471(16) 0.074(2) -0.0226(15) 0.0089(14) 0.0046(13) C38 0.0543(17) 0.064(2) 0.085(2) -0.0366(18) 0.0298(16) -0.0037(15) C39 0.0610(18) 0.073(2) 0.0599(18) -0.0248(16) 0.0313(15) -0.0191(16) C40 0.0550(16) 0.0568(17) 0.0513(16) -0.0052(13) 0.0220(13) -0.0040(14) C41 0.0361(12) 0.0485(15) 0.0424(13) 0.0017(11) 0.0054(10) -0.0009(11) C42 0.0394(14) 0.071(2) 0.0430(14) -0.0050(14) 0.0015(11) -0.0029(13) C43 0.0432(15) 0.081(2) 0.0536(17) -0.0104(16) 0.0049(13) -0.0232(15) C44 0.0473(15) 0.0573(17) 0.0554(16) -0.0040(14) 0.0131(13) -0.0196(13) C45 0.0311(11) 0.0355(12) 0.0449(13) -0.0060(10) 0.0143(10) -0.0028(9) C46 0.0338(11) 0.0300(11) 0.0453(13) -0.0021(10) 0.0184(10) -0.0006(9) C47 0.0480(14) 0.0356(13) 0.0571(16) -0.0009(12) 0.0249(12) -0.0069(11) C48 0.0651(18) 0.0380(14) 0.0549(16) 0.0100(12) 0.0299(14) 0.0013(13) C49 0.0536(16) 0.0506(16) 0.0541(16) 0.0214(13) 0.0152(13) 0.0076(13) C50 0.0386(13) 0.0552(17) 0.0575(16) 0.0217(13) 0.0090(12) 0.0002(12) C51 0.0364(12) 0.0342(12) 0.0437(13) -0.0038(10) 0.0066(10) -0.0070(10) C52 0.0515(15) 0.0382(13) 0.0408(13) -0.0065(11) 0.0111(11) -0.0065(11) C53 0.0473(14) 0.0458(14) 0.0450(14) -0.0032(12) 0.0191(11) 0.0026(12) C54 0.0335(12) 0.0488(15) 0.0418(13) 0.0006(11) 0.0123(10) -0.0003(11) C55 0.0302(10) 0.0300(11) 0.0313(11) 0.0052(9) 0.0078(8) -0.0017(9) C56 0.0307(10) 0.0311(11) 0.0292(10) 0.0074(9) 0.0048(8) -0.0012(9) C57 0.0291(11) 0.0477(14) 0.0358(12) 0.0067(10) 0.0057(9) -0.0032(10) C58 0.0366(12) 0.0486(15) 0.0384(13) 0.0058(11) -0.0022(10) -0.0088(11) C59 0.0460(14) 0.0434(14) 0.0323(12) 0.0019(10) -0.0030(10) -0.0036(11) C60 0.0385(12) 0.0444(14) 0.0340(12) -0.0003(10) 0.0052(10) 0.0015(10) Nb1 0.0261(1) 0.0305(1) 0.0268(1) 0.0003(1) 0.0028(1) 0.0023(1) O1 0.0371(8) 0.0471(10) 0.0299(8) -0.0018(7) 0.0053(7) 0.0007(7) O2 0.0268(8) 0.0329(8) 0.0479(9) 0.0110(7) 0.0027(7) -0.0013(6) O3 0.0372(9) 0.0298(8) 0.0444(9) 0.0049(7) 0.0035(7) 0.0012(7) O4 0.0298(9) 0.0613(12) 0.0759(14) 0.0226(11) -0.0005(9) -0.0077(8) O5 0.0529(11) 0.0494(11) 0.0762(14) 0.0216(10) 0.0129(10) -0.0136(9) O6 0.0266(8) 0.0501(11) 0.0455(9) 0.0013(8) 0.0042(7) -0.0017(7) O7 0.0314(8) 0.0320(8) 0.0462(9) 0.0043(7) 0.0027(7) -0.0020(7) O8 0.0456(12) 0.0784(16) 0.119(2) 0.0403(15) -0.0205(12) -0.0296(11) O9 0.0664(12) 0.0350(10) 0.0618(12) 0.0010(9) 0.0095(10) -0.0127(9) O10 0.0357(8) 0.0413(9) 0.0296(8) -0.0022(7) 0.0044(6) 0.0131(7) O11 0.0339(8) 0.0336(8) 0.0303(8) -0.0015(6) 0.0058(6) 0.0078(6) O12 0.0453(10) 0.0476(10) 0.0407(9) 0.0039(8) 0.0013(8) 0.0200(8) O13 0.0434(9) 0.0476(10) 0.0297(8) 0.0040(7) 0.0104(7) 0.0078(8) C61 0.0318(11) 0.0369(12) 0.0391(12) 0.0036(10) 0.0052(9) -0.0006(10) C62 0.0428(13) 0.0332(12) 0.0370(12) 0.0008(10) 0.0073(10) -0.0034(10) C63 0.0346(12) 0.0573(17) 0.0420(14) 0.0140(12) -0.0028(10) -0.0131(12) C64 0.0424(13) 0.0396(14) 0.0329(12) 0.0026(10) 0.0077(10) -0.0106(11) C65 0.0254(10) 0.0348(12) 0.0331(11) -0.0012(9) 0.0043(8) 0.0021(9) C66 0.0260(10) 0.0312(11) 0.0314(11) 0.0009(9) 0.0065(8) -0.0011(8) O17 0.0618(14) 0.0760(17) 0.0960(19) -0.0036(14) 0.0122(13) 0.0021(12) O18 0.0650(16) 0.0652(15) 0.150(3) 0.0036(17) 0.0418(17) -0.0157(12) O19 0.0670(12) 0.0418(10) 0.0434(10) 0.0059(8) 0.0047(10) -0.0010(10) O20 0.0865(18) 0.107(2) 0.0784(17) 0.0091(16) 0.0312(14) 0.0078(16) O14 0.0574(15) 0.0616(15) 0.186(3) 0.0151(18) 0.0480(18) -0.0087(12) O15 0.0452(11) 0.0519(12) 0.0688(13) 0.0073(11) -0.0025(10) 0.0037(9) O16 0.105(2) 0.0789(17) 0.0995(18) 0.0232(16) 0.0717(17) 0.0275(15) O21 0.0730(16) 0.0916(19) 0.0861(18) -0.0196(14) 0.0408(14) -0.0005(14) O22 0.0753(16) 0.0715(16) 0.0643(14) 0.0071(12) 0.0049(12) 0.0216(12) O23 0.0387(9) 0.0463(10) 0.0341(9) 0.0035(8) 0.0045(7) 0.0056(8) O24 0.0539(13) 0.127(2) 0.0471(12) -0.0173(13) 0.0165(10) -0.0013(14) Cl1 0.0554(4) 0.0471(4) 0.0453(3) -0.0032(3) 0.0166(3) 0.0085(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O7 2.1052(16) . . no Nb1 O10 2.1186(16) . . no Nb1 O11 2.2018(14) . . no Nb1 O3 2.1507(16) . . no Nb1 O1 1.7141(16) . . no Nb1 O2 2.0994(15) . . no Nb1 O6 2.1588(16) . . no Zn1 N4 2.1360(18) . . no Zn1 N1 2.1428(18) . . no Zn1 N2 2.1591(18) . . no Zn1 N3 2.1736(19) . . no Zn1 N5 2.1496(17) . . no Zn1 N6 2.1569(17) . . no Zn2 N7 2.1369(19) . . no Zn2 N8 2.182(2) . . no Zn2 N9 2.156(2) . . no Zn2 N10 2.142(2) . . no Zn2 N11 2.1376(18) . . no Zn2 N12 2.1423(18) . . no O2 C61 1.290(3) . . no O3 C62 1.296(3) . . no O4 C61 1.219(3) . . no O5 C62 1.214(3) . . no O6 C63 1.282(3) . . no O7 C64 1.294(3) . . no O8 C63 1.218(3) . . no O9 C64 1.215(3) . . no O10 C65 1.288(3) . . no O11 C66 1.277(3) . . no O12 C65 1.216(3) . . no O13 C66 1.227(3) . . no O17 H172 0.84(2) . . no O17 H173 0.845(17) . . no O17 H171 0.84(2) . . no O18 H183 0.84(5) . . no O18 H182 0.84(2) . . no O18 H181 0.82(3) . . no N1 C5 1.345(3) . . no N1 C1 1.346(3) . . no N2 C10 1.346(3) . . no N2 C6 1.344(3) . . no N3 C11 1.338(3) . . no N3 C15 1.342(3) . . no N4 C20 1.341(3) . . no N4 C16 1.350(3) . . no N5 C21 1.343(3) . . no N5 C25 1.353(3) . . no N6 C26 1.351(3) . . no N6 C30 1.343(3) . . no O19 H193 0.83(4) . . no O19 H191 0.82(2) . . no O19 H192 0.83(3) . . no N7 C35 1.342(3) . . no N7 C31 1.343(3) . . no N8 C36 1.356(3) . . no N8 C40 1.340(3) . . no N9 C45 1.348(3) . . no N9 C41 1.343(3) . . no N10 C46 1.339(3) . . no N10 C50 1.339(3) . . no N11 C55 1.344(3) . . no N11 C51 1.348(3) . . no N12 C56 1.342(3) . . no N12 C60 1.341(3) . . no O20 H203 0.85(4) . . no O20 H201 0.831(13) . . no O20 H202 0.852(14) . . no O14 H142 0.84(3) . . no O14 H141 0.84(2) . . no O15 H152 0.85(2) . . no O15 H151 0.84(2) . . no O16 H162 0.845(17) . . no O16 H161 0.84(2) . . no C1 C2 1.372(3) . . no C2 C3 1.376(3) . . no C3 C4 1.383(3) . . no C4 C5 1.389(3) . . no C5 C6 1.488(3) . . no C6 C7 1.386(3) . . no C7 C8 1.372(3) . . no C8 C9 1.380(4) . . no C9 C10 1.374(3) . . no C11 C12 1.378(4) . . no C12 C13 1.368(4) . . no C13 C14 1.386(4) . . no C14 C15 1.387(3) . . no C15 C16 1.489(3) . . no C16 C17 1.382(3) . . no C17 C18 1.380(4) . . no C18 C19 1.374(4) . . no C19 C20 1.375(3) . . no C21 C22 1.376(3) . . no C22 C23 1.378(3) . . no C23 C24 1.384(3) . . no C24 C25 1.389(3) . . no C25 C26 1.485(3) . . no C26 C27 1.389(3) . . no C27 C28 1.392(3) . . no C28 C29 1.371(3) . . no C29 C30 1.379(3) . . no C1 H1 0.9296 . . no C2 H2 0.9294 . . no C3 H3 0.9295 . . no C4 H4 0.9306 . . no C7 H7 0.9296 . . no C8 H8 0.9292 . . no C9 H9 0.9304 . . no C10 H10 0.9306 . . no C11 H11 0.9294 . . no C12 H12 0.9296 . . no C13 H13 0.9298 . . no C14 H14 0.9306 . . no C17 H17 0.9304 . . no C18 H18 0.9291 . . no C19 H19 0.9286 . . no C20 H20 0.9296 . . no C21 H21 0.9295 . . no O21 H211 0.84(2) . . no O21 H212 0.84(3) . . no C22 H22 0.9289 . . no C23 H23 0.9304 . . no C24 H24 0.9297 . . no C27 H27 0.9308 . . no C28 H28 0.9292 . . no C29 H29 0.9301 . . no C30 H30 0.9308 . . no C31 C32 1.379(4) . . no C32 C33 1.370(4) . . no C33 C34 1.382(5) . . no C34 C35 1.392(4) . . no C35 C36 1.481(3) . . no C36 C37 1.378(4) . . no C37 C38 1.372(5) . . no C38 C39 1.374(5) . . no C39 C40 1.384(4) . . no C41 C42 1.376(4) . . no C42 C43 1.369(5) . . no C43 C44 1.389(4) . . no C44 C45 1.383(4) . . no C45 C46 1.492(3) . . no C46 C47 1.393(3) . . no C47 C48 1.376(4) . . no C48 C49 1.368(4) . . no C49 C50 1.376(4) . . no C51 C52 1.375(4) . . no C52 C53 1.373(4) . . no C53 C54 1.379(4) . . no C54 C55 1.388(3) . . no C55 C56 1.490(3) . . no C56 C57 1.386(3) . . no C57 C58 1.386(3) . . no C58 C59 1.374(4) . . no C59 C60 1.385(4) . . no O22 H222 0.83(3) . . no O22 H221 0.84(3) . . no C31 H31 0.9308 . . no C32 H32 0.9306 . . no C33 H33 0.9304 . . no C34 H34 0.9303 . . no C37 H37 0.9307 . . no C38 H38 0.9312 . . no C39 H39 0.9307 . . no C40 H40 0.9302 . . no C41 H41 0.9303 . . no C42 H42 0.9297 . . no C43 H43 0.9309 . . no C44 H44 0.9298 . . no C47 H47 0.9302 . . no C48 H48 0.9304 . . no C49 H49 0.9306 . . no C50 H50 0.9302 . . no C51 H51 0.9307 . . no C52 H52 0.9302 . . no C53 H53 0.9308 . . no C54 H54 0.9303 . . no C57 H57 0.9305 . . no C58 H58 0.9305 . . no C59 H59 0.9293 . . no C60 H60 0.9299 . . no C61 C62 1.538(3) . . no C63 C64 1.530(4) . . no C65 C66 1.550(3) . . no O23 H231 0.833(18) . . no O23 H232 0.83(2) . . no O24 H241 0.84(3) . . no O24 H242 0.84(3) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O10 144.50(6) . . . no O2 Nb1 O11 99.75(6) . . . no O3 Nb1 O6 144.59(6) . . . no O3 Nb1 O7 136.07(6) . . . no O3 Nb1 O10 72.46(6) . . . no O3 Nb1 O11 81.14(6) . . . no O6 Nb1 O7 72.34(6) . . . no O6 Nb1 O10 73.10(6) . . . no O6 Nb1 O11 81.75(6) . . . no O7 Nb1 O10 141.47(6) . . . no O7 Nb1 O11 84.79(6) . . . no O10 Nb1 O11 73.90(6) . . . no O1 Nb1 O6 89.53(7) . . . no O1 Nb1 O7 105.22(7) . . . no O1 Nb1 O10 90.94(7) . . . no O1 Nb1 O11 164.15(7) . . . no O2 Nb1 O3 72.05(6) . . . no O2 Nb1 O6 141.66(6) . . . no O2 Nb1 O7 69.69(6) . . . no O1 Nb1 O3 98.97(7) . . . no O1 Nb1 O2 95.31(7) . . . no N1 Zn1 N3 93.99(7) . . . no N1 Zn1 N4 167.15(7) . . . no N1 Zn1 N6 94.61(7) . . . no N2 Zn1 N3 94.42(7) . . . no N1 Zn1 N5 93.71(7) . . . no N1 Zn1 N2 76.52(7) . . . no N4 Zn1 N5 95.58(7) . . . no N4 Zn1 N6 96.17(7) . . . no N5 Zn1 N6 76.54(6) . . . no N3 Zn1 N6 169.31(7) . . . no N2 Zn1 N5 165.78(7) . . . no N2 Zn1 N6 93.76(7) . . . no N2 Zn1 N4 95.78(7) . . . no N3 Zn1 N5 96.58(7) . . . no N3 Zn1 N4 76.16(7) . . . no N7 Zn2 N8 76.35(8) . . . no N11 Zn2 N12 77.24(7) . . . no N8 Zn2 N10 90.93(8) . . . no N8 Zn2 N11 169.69(7) . . . no N7 Zn2 N9 93.37(7) . . . no N7 Zn2 N10 164.02(8) . . . no N7 Zn2 N11 96.15(7) . . . no N7 Zn2 N12 93.11(7) . . . no N8 Zn2 N9 90.62(8) . . . no N10 Zn2 N12 97.86(7) . . . no N9 Zn2 N10 76.89(8) . . . no N9 Zn2 N11 96.96(7) . . . no N8 Zn2 N12 95.90(7) . . . no N10 Zn2 N11 97.58(7) . . . no N9 Zn2 N12 171.73(7) . . . no Nb1 O2 C61 122.85(15) . . . no Nb1 O3 C62 120.94(14) . . . no Nb1 O6 C63 120.23(15) . . . no Nb1 O7 C64 121.79(15) . . . no Nb1 O10 C65 120.06(14) . . . no Nb1 O11 C66 117.49(13) . . . no H171 O17 H172 105(3) . . . no H171 O17 H173 104(4) . . . no H172 O17 H173 88(4) . . . no H181 O18 H182 107(5) . . . no H181 O18 H183 106(4) . . . no H182 O18 H183 133(6) . . . no Zn1 N1 C5 116.03(14) . . . no Zn1 N1 C1 125.40(15) . . . no C1 N1 C5 118.57(19) . . . no Zn1 N2 C6 115.53(14) . . . no Zn1 N2 C10 125.94(15) . . . no C6 N2 C10 118.48(19) . . . no Zn1 N3 C15 115.51(14) . . . no Zn1 N3 C11 125.83(16) . . . no C11 N3 C15 118.6(2) . . . no Zn1 N4 C16 116.83(14) . . . no Zn1 N4 C20 124.86(15) . . . no C16 N4 C20 118.28(19) . . . no C21 N5 C25 118.21(18) . . . no Zn1 N5 C25 115.82(13) . . . no Zn1 N5 C21 125.70(15) . . . no Zn1 N6 C30 125.88(15) . . . no Zn1 N6 C26 115.65(13) . . . no C26 N6 C30 118.46(18) . . . no H191 O19 H192 106(3) . . . no H192 O19 H193 102(5) . . . no H191 O19 H193 107(4) . . . no Zn2 N7 C31 124.74(16) . . . no C31 N7 C35 119.3(2) . . . no Zn2 N7 C35 115.93(15) . . . no Zn2 N8 C40 126.72(18) . . . no Zn2 N8 C36 113.65(16) . . . no C36 N8 C40 118.5(2) . . . no C41 N9 C45 118.5(2) . . . no Zn2 N9 C41 126.54(16) . . . no Zn2 N9 C45 114.99(16) . . . no Zn2 N10 C46 115.35(15) . . . no C46 N10 C50 118.8(2) . . . no Zn2 N10 C50 124.74(17) . . . no Zn2 N11 C55 115.17(14) . . . no C51 N11 C55 118.13(19) . . . no Zn2 N11 C51 126.57(15) . . . no C56 N12 C60 118.80(19) . . . no Zn2 N12 C60 125.43(15) . . . no Zn2 N12 C56 114.97(14) . . . no H201 O20 H203 106(3) . . . no H201 O20 H202 107.1(16) . . . no H202 O20 H203 140(4) . . . no H141 O14 H142 103(4) . . . no H151 O15 H152 105(2) . . . no H161 O16 H162 104(4) . . . no N1 C1 C2 122.7(2) . . . no C1 C2 C3 119.0(2) . . . no C2 C3 C4 119.0(2) . . . no C3 C4 C5 119.3(2) . . . no C4 C5 C6 122.64(19) . . . no N1 C5 C6 115.95(18) . . . no N1 C5 C4 121.41(19) . . . no N2 C6 C7 121.26(19) . . . no N2 C6 C5 115.91(18) . . . no C5 C6 C7 122.83(19) . . . no C6 C7 C8 119.7(2) . . . no C7 C8 C9 119.3(2) . . . no C8 C9 C10 118.5(2) . . . no N2 C10 C9 122.9(2) . . . no N3 C11 C12 122.8(2) . . . no C11 C12 C13 118.7(3) . . . no C12 C13 C14 119.3(2) . . . no C13 C14 C15 119.0(2) . . . no N3 C15 C14 121.5(2) . . . no N3 C15 C16 116.02(19) . . . no C14 C15 C16 122.5(2) . . . no N4 C16 C17 121.3(2) . . . no N4 C16 C15 115.37(18) . . . no C15 C16 C17 123.3(2) . . . no C16 C17 C18 119.5(2) . . . no C17 C18 C19 119.4(2) . . . no C18 C19 C20 118.4(2) . . . no N4 C20 C19 123.2(2) . . . no N5 C21 C22 123.2(2) . . . no C21 C22 C23 118.8(2) . . . no C22 C23 C24 118.9(2) . . . no C23 C24 C25 119.6(2) . . . no C24 C25 C26 122.8(2) . . . no N5 C25 C24 121.34(19) . . . no N5 C25 C26 115.82(18) . . . no N6 C26 C25 115.97(19) . . . no C25 C26 C27 122.4(2) . . . no N6 C26 C27 121.59(19) . . . no C26 C27 C28 119.0(2) . . . no C27 C28 C29 119.2(2) . . . no C28 C29 C30 118.9(2) . . . no N6 C30 C29 122.8(2) . . . no C2 C1 H1 118.66 . . . no N1 C1 H1 118.67 . . . no C3 C2 H2 120.45 . . . no C1 C2 H2 120.52 . . . no C2 C3 H3 120.48 . . . no C4 C3 H3 120.52 . . . no C5 C4 H4 120.35 . . . no C3 C4 H4 120.37 . . . no C6 C7 H7 120.12 . . . no C8 C7 H7 120.19 . . . no C9 C8 H8 120.33 . . . no C7 C8 H8 120.42 . . . no C10 C9 H9 120.77 . . . no C8 C9 H9 120.76 . . . no C9 C10 H10 118.61 . . . no N2 C10 H10 118.54 . . . no N3 C11 H11 118.56 . . . no C12 C11 H11 118.63 . . . no C13 C12 H12 120.65 . . . no C11 C12 H12 120.62 . . . no C14 C13 H13 120.33 . . . no C12 C13 H13 120.35 . . . no C13 C14 H14 120.53 . . . no C15 C14 H14 120.48 . . . no C18 C17 H17 120.23 . . . no C16 C17 H17 120.30 . . . no C17 C18 H18 120.30 . . . no C19 C18 H18 120.35 . . . no C20 C19 H19 120.87 . . . no C18 C19 H19 120.74 . . . no C19 C20 H20 118.40 . . . no N4 C20 H20 118.42 . . . no H211 O21 H212 103(3) . . . no N5 C21 H21 118.36 . . . no C22 C21 H21 118.49 . . . no C21 C22 H22 120.57 . . . no C23 C22 H22 120.61 . . . no C22 C23 H23 120.60 . . . no C24 C23 H23 120.53 . . . no C25 C24 H24 120.26 . . . no C23 C24 H24 120.15 . . . no C28 C27 H27 120.47 . . . no C26 C27 H27 120.57 . . . no C29 C28 H28 120.38 . . . no C27 C28 H28 120.39 . . . no C28 C29 H29 120.52 . . . no C30 C29 H29 120.55 . . . no N6 C30 H30 118.54 . . . no C29 C30 H30 118.64 . . . no N7 C31 C32 123.0(2) . . . no C31 C32 C33 117.7(3) . . . no C32 C33 C34 120.2(3) . . . no C33 C34 C35 119.2(3) . . . no N7 C35 C34 120.5(2) . . . no N7 C35 C36 116.4(2) . . . no C34 C35 C36 123.1(2) . . . no N8 C36 C37 120.9(2) . . . no N8 C36 C35 115.7(2) . . . no C35 C36 C37 123.4(2) . . . no C36 C37 C38 120.1(3) . . . no C37 C38 C39 119.5(3) . . . no C38 C39 C40 118.1(3) . . . no N8 C40 C39 122.9(3) . . . no N9 C41 C42 123.0(2) . . . no C41 C42 C43 118.7(3) . . . no C42 C43 C44 119.2(3) . . . no C43 C44 C45 119.3(3) . . . no N9 C45 C46 115.8(2) . . . no N9 C45 C44 121.4(2) . . . no C44 C45 C46 122.8(2) . . . no N10 C46 C45 116.0(2) . . . no C45 C46 C47 123.0(2) . . . no N10 C46 C47 121.0(2) . . . no C46 C47 C48 119.2(2) . . . no C47 C48 C49 119.9(3) . . . no C48 C49 C50 118.0(3) . . . no N10 C50 C49 123.2(3) . . . no N11 C51 C52 123.2(2) . . . no C51 C52 C53 118.3(2) . . . no C52 C53 C54 119.7(2) . . . no C53 C54 C55 119.2(2) . . . no N11 C55 C54 121.5(2) . . . no N11 C55 C56 116.01(19) . . . no C54 C55 C56 122.5(2) . . . no C55 C56 C57 123.0(2) . . . no N12 C56 C55 115.78(19) . . . no N12 C56 C57 121.3(2) . . . no C56 C57 C58 119.4(2) . . . no C57 C58 C59 119.4(2) . . . no C58 C59 C60 118.2(2) . . . no N12 C60 C59 123.0(2) . . . no H221 O22 H222 105(3) . . . no C32 C31 H31 118.52 . . . no N7 C31 H31 118.44 . . . no C31 C32 H32 121.08 . . . no C33 C32 H32 121.23 . . . no C32 C33 H33 119.93 . . . no C34 C33 H33 119.83 . . . no C33 C34 H34 120.44 . . . no C35 C34 H34 120.39 . . . no C38 C37 H37 119.98 . . . no C36 C37 H37 119.95 . . . no C37 C38 H38 120.28 . . . no C39 C38 H38 120.22 . . . no C38 C39 H39 120.93 . . . no C40 C39 H39 120.96 . . . no C39 C40 H40 118.55 . . . no N8 C40 H40 118.53 . . . no C42 C41 H41 118.57 . . . no N9 C41 H41 118.47 . . . no C43 C42 H42 120.67 . . . no C41 C42 H42 120.64 . . . no C44 C43 H43 120.40 . . . no C42 C43 H43 120.36 . . . no C45 C44 H44 120.31 . . . no C43 C44 H44 120.43 . . . no C46 C47 H47 120.42 . . . no C48 C47 H47 120.42 . . . no C47 C48 H48 119.99 . . . no C49 C48 H48 120.09 . . . no C50 C49 H49 121.11 . . . no C48 C49 H49 120.89 . . . no N10 C50 H50 118.43 . . . no C49 C50 H50 118.39 . . . no C52 C51 H51 118.41 . . . no N11 C51 H51 118.38 . . . no C53 C52 H52 120.83 . . . no C51 C52 H52 120.91 . . . no C54 C53 H53 120.16 . . . no C52 C53 H53 120.19 . . . no C53 C54 H54 120.41 . . . no C55 C54 H54 120.38 . . . no C58 C57 H57 120.31 . . . no C56 C57 H57 120.26 . . . no C59 C58 H58 120.31 . . . no C57 C58 H58 120.33 . . . no C58 C59 H59 120.93 . . . no C60 C59 H59 120.90 . . . no C59 C60 H60 118.50 . . . no N12 C60 H60 118.55 . . . no O2 C61 O4 125.4(2) . . . no O2 C61 C62 111.8(2) . . . no O4 C61 C62 122.9(2) . . . no O5 C62 C61 121.9(2) . . . no O3 C62 O5 126.7(2) . . . no O3 C62 C61 111.5(2) . . . no O6 C63 C64 112.7(2) . . . no O6 C63 O8 125.4(2) . . . no O8 C63 C64 121.8(2) . . . no O7 C64 C63 112.3(2) . . . no O7 C64 O9 125.6(2) . . . no O9 C64 C63 122.2(2) . . . no O10 C65 C66 114.07(18) . . . no O12 C65 C66 120.14(18) . . . no O10 C65 O12 125.8(2) . . . no O13 C66 C65 119.52(19) . . . no O11 C66 O13 126.3(2) . . . no O11 C66 C65 114.15(17) . . . no H231 O23 H232 105(2) . . . no H241 O24 H242 104(3) . . . no 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 O11 Nb1 O2 C61 81.08(17) . . . . no O1 Nb1 O3 C62 95.99(17) . . . . no O2 Nb1 O3 C62 3.28(16) . . . . no O6 Nb1 O3 C62 -162.02(15) . . . . no O7 Nb1 O3 C62 -27.2(2) . . . . no O10 Nb1 O3 C62 -175.87(17) . . . . no O11 Nb1 O3 C62 -100.05(16) . . . . no O1 Nb1 O6 C63 -111.68(18) . . . . no O2 Nb1 O6 C63 -13.7(2) . . . . no O3 Nb1 O6 C63 143.40(16) . . . . no O7 Nb1 O6 C63 -5.52(17) . . . . no O10 Nb1 O6 C63 157.20(18) . . . . no O11 Nb1 O6 C63 81.61(17) . . . . no O1 Nb1 O7 C64 92.23(17) . . . . no O2 Nb1 O7 C64 -177.68(18) . . . . no O3 Nb1 O7 C64 -146.75(15) . . . . no O6 Nb1 O7 C64 7.72(16) . . . . no O10 Nb1 O7 C64 -19.4(2) . . . . no O11 Nb1 O7 C64 -75.26(17) . . . . no O1 Nb1 O10 C65 -179.84(17) . . . . no O2 Nb1 O10 C65 79.66(19) . . . . no O3 Nb1 O10 C65 81.05(16) . . . . no O6 Nb1 O10 C65 -90.62(16) . . . . no O7 Nb1 O10 C65 -63.59(19) . . . . no O11 Nb1 O10 C65 -4.54(15) . . . . no O2 Nb1 O11 C66 -138.89(15) . . . . no O1 Nb1 O2 C61 -93.94(17) . . . . no O3 Nb1 O2 C61 3.79(16) . . . . no O6 Nb1 O2 C61 170.08(15) . . . . no O7 Nb1 O2 C61 161.77(18) . . . . no O10 Nb1 O2 C61 5.2(2) . . . . no O10 Nb1 O11 C66 5.22(15) . . . . no O3 Nb1 O11 C66 -68.97(15) . . . . no O6 Nb1 O11 C66 79.92(15) . . . . no O7 Nb1 O11 C66 152.78(15) . . . . no N2 Zn1 N1 C5 1.92(14) . . . . no N3 Zn1 N1 C1 -84.65(18) . . . . no N3 Zn1 N1 C5 95.52(15) . . . . no N2 Zn1 N1 C1 -178.24(19) . . . . no N1 Zn1 N2 C6 -2.34(14) . . . . no N1 Zn1 N2 C10 -179.64(19) . . . . no N3 Zn1 N2 C6 -95.39(15) . . . . no N5 Zn1 N1 C1 12.22(19) . . . . no N5 Zn1 N1 C5 -167.62(15) . . . . no N6 Zn1 N1 C1 89.00(18) . . . . no N6 Zn1 N1 C5 -90.84(15) . . . . no N6 Zn1 N2 C10 -85.79(18) . . . . no N1 Zn1 N3 C11 9.2(2) . . . . no N1 Zn1 N3 C15 -173.05(16) . . . . no N2 Zn1 N3 C11 86.0(2) . . . . no N2 Zn1 N3 C15 -96.29(16) . . . . no N4 Zn1 N3 C11 -179.1(2) . . . . no N4 Zn1 N3 C15 -1.41(15) . . . . no N5 Zn1 N3 C11 -85.0(2) . . . . no N5 Zn1 N3 C15 92.74(16) . . . . no N2 Zn1 N4 C16 92.33(15) . . . . no N2 Zn1 N4 C20 -85.84(18) . . . . no N3 Zn1 N2 C10 87.31(18) . . . . no N4 Zn1 N2 C6 -171.89(15) . . . . no N4 Zn1 N2 C10 10.81(18) . . . . no N6 Zn1 N2 C6 91.51(15) . . . . no N5 Zn1 N4 C16 -96.23(15) . . . . no N5 Zn1 N4 C20 85.60(18) . . . . no N6 Zn1 N4 C16 -173.24(15) . . . . no N6 Zn1 N4 C20 8.59(19) . . . . no N1 Zn1 N5 C21 -83.02(18) . . . . no N1 Zn1 N5 C25 90.84(15) . . . . no N3 Zn1 N5 C21 11.43(18) . . . . no N3 Zn1 N5 C25 -174.70(14) . . . . no N4 Zn1 N5 C21 88.09(18) . . . . no N4 Zn1 N5 C25 -98.05(15) . . . . no N6 Zn1 N5 C21 -176.88(18) . . . . no N6 Zn1 N5 C25 -3.02(14) . . . . no N1 Zn1 N6 C26 -92.35(15) . . . . no N1 Zn1 N6 C30 89.48(17) . . . . no N2 Zn1 N6 C26 -169.11(14) . . . . no N2 Zn1 N6 C30 12.72(17) . . . . no N4 Zn1 N6 C26 94.65(15) . . . . no N4 Zn1 N6 C30 -83.52(17) . . . . no N5 Zn1 N6 C26 0.37(14) . . . . no N5 Zn1 N6 C30 -177.81(18) . . . . no N3 Zn1 N4 C20 -178.98(19) . . . . no N3 Zn1 N4 C16 -0.81(15) . . . . no N11 Zn2 N7 C35 178.50(17) . . . . no N11 Zn2 N7 C31 0.1(2) . . . . no N7 Zn2 N8 C36 12.54(16) . . . . no N7 Zn2 N8 C40 179.9(2) . . . . no N9 Zn2 N8 C36 -80.77(17) . . . . no N9 Zn2 N8 C40 86.6(2) . . . . no N10 Zn2 N8 C36 -157.67(17) . . . . no N12 Zn2 N7 C31 77.60(19) . . . . no N12 Zn2 N7 C35 -104.01(17) . . . . no N11 Zn2 N12 C60 175.8(2) . . . . no N12 Zn2 N8 C40 -88.3(2) . . . . no N7 Zn2 N9 C41 15.6(2) . . . . no N7 Zn2 N9 C45 -164.25(17) . . . . no N8 Zn2 N9 C41 92.0(2) . . . . no N8 Zn2 N9 C45 -87.89(17) . . . . no N10 Zn2 N9 C41 -177.2(2) . . . . no N10 Zn2 N9 C45 2.93(16) . . . . no N11 Zn2 N9 C41 -81.0(2) . . . . no N11 Zn2 N9 C45 99.13(17) . . . . no N8 Zn2 N10 C46 82.66(17) . . . . no N8 Zn2 N10 C50 -84.8(2) . . . . no N9 Zn2 N10 C46 -7.76(16) . . . . no N9 Zn2 N10 C50 -175.3(2) . . . . no N11 Zn2 N10 C46 -103.18(17) . . . . no N11 Zn2 N10 C50 89.3(2) . . . . no N8 Zn2 N7 C31 172.9(2) . . . . no N8 Zn2 N7 C35 -8.70(17) . . . . no N9 Zn2 N7 C31 -97.27(19) . . . . no N9 Zn2 N7 C35 81.12(17) . . . . no N9 Zn2 N11 C55 -174.89(15) . . . . no N10 Zn2 N11 C51 78.50(19) . . . . no N10 Zn2 N11 C55 -97.26(15) . . . . no N12 Zn2 N11 C51 174.9(2) . . . . no N12 Zn2 N11 C55 -0.87(15) . . . . no N7 Zn2 N12 C56 -89.41(16) . . . . no N7 Zn2 N12 C60 80.15(19) . . . . no N8 Zn2 N12 C56 -166.00(16) . . . . no N8 Zn2 N12 C60 3.6(2) . . . . no N10 Zn2 N12 C56 102.23(16) . . . . no N10 Zn2 N12 C60 -88.21(19) . . . . no N11 Zn2 N12 C56 6.19(15) . . . . no N12 Zn2 N10 C46 178.75(16) . . . . no N12 Zn2 N10 C50 11.3(2) . . . . no N7 Zn2 N11 C51 -93.30(19) . . . . no N7 Zn2 N11 C55 90.94(15) . . . . no N9 Zn2 N11 C51 0.87(19) . . . . no N12 Zn2 N8 C36 104.33(16) . . . . no N10 Zn2 N8 C40 9.7(2) . . . . no Nb1 O2 C61 O4 170.38(19) . . . . no Nb1 O2 C61 C62 -8.8(3) . . . . no Nb1 O3 C62 O5 172.7(2) . . . . no Nb1 O3 C62 C61 -8.2(2) . . . . no Nb1 O6 C63 O8 -178.5(2) . . . . no Nb1 O6 C63 C64 3.1(3) . . . . no Nb1 O7 C64 O9 172.17(19) . . . . no Nb1 O7 C64 C63 -8.5(3) . . . . no Nb1 O10 C65 C66 3.4(2) . . . . no Nb1 O10 C65 O12 -177.40(18) . . . . no Nb1 O11 C66 O13 175.15(18) . . . . no Nb1 O11 C66 C65 -5.1(2) . . . . no C1 N1 C5 C4 -0.8(3) . . . . no C1 N1 C5 C6 178.85(19) . . . . no C5 N1 C1 C2 -0.6(3) . . . . no Zn1 N1 C1 C2 179.55(18) . . . . no Zn1 N1 C5 C4 179.03(16) . . . . no Zn1 N1 C5 C6 -1.3(2) . . . . no Zn1 N2 C6 C7 -177.35(16) . . . . no C6 N2 C10 C9 0.1(3) . . . . no Zn1 N2 C10 C9 177.33(17) . . . . no C10 N2 C6 C7 0.2(3) . . . . no Zn1 N2 C6 C5 2.4(2) . . . . no C10 N2 C6 C5 179.93(19) . . . . no Zn1 N3 C11 C12 176.3(2) . . . . no C11 N3 C15 C16 -178.9(2) . . . . no Zn1 N3 C15 C14 -176.01(17) . . . . no C15 N3 C11 C12 -1.3(4) . . . . no C11 N3 C15 C14 1.9(3) . . . . no Zn1 N3 C15 C16 3.2(2) . . . . no Zn1 N4 C16 C15 2.7(2) . . . . no C16 N4 C20 C19 -0.7(3) . . . . no Zn1 N4 C16 C17 -177.47(17) . . . . no C20 N4 C16 C15 -179.01(19) . . . . no C20 N4 C16 C17 0.8(3) . . . . no Zn1 N4 C20 C19 177.46(18) . . . . no Zn1 N5 C21 C22 172.36(17) . . . . no C21 N5 C25 C26 179.40(18) . . . . no Zn1 N5 C25 C24 -173.72(16) . . . . no C25 N5 C21 C22 -1.4(3) . . . . no C21 N5 C25 C24 0.6(3) . . . . no Zn1 N5 C25 C26 5.1(2) . . . . no C30 N6 C26 C27 0.7(3) . . . . no Zn1 N6 C30 C29 177.19(16) . . . . no C30 N6 C26 C25 -179.58(18) . . . . no Zn1 N6 C26 C25 2.1(2) . . . . no Zn1 N6 C26 C27 -177.60(16) . . . . no C26 N6 C30 C29 -0.9(3) . . . . no C31 N7 C35 C34 1.1(4) . . . . no C35 N7 C31 C32 0.0(4) . . . . no C31 N7 C35 C36 -177.6(2) . . . . no Zn2 N7 C35 C36 3.9(3) . . . . no Zn2 N7 C31 C32 178.35(19) . . . . no Zn2 N7 C35 C34 -177.4(2) . . . . no C36 N8 C40 C39 1.8(4) . . . . no Zn2 N8 C36 C37 166.1(2) . . . . no C40 N8 C36 C37 -2.3(4) . . . . no Zn2 N8 C36 C35 -14.6(3) . . . . no C40 N8 C36 C35 176.9(2) . . . . no Zn2 N8 C40 C39 -165.1(2) . . . . no Zn2 N9 C45 C44 -178.44(19) . . . . no Zn2 N9 C41 C42 179.76(19) . . . . no C41 N9 C45 C46 -178.1(2) . . . . no Zn2 N9 C45 C46 1.8(3) . . . . no C41 N9 C45 C44 1.7(3) . . . . no C45 N9 C41 C42 -0.4(4) . . . . no C50 N10 C46 C47 0.4(3) . . . . no Zn2 N10 C50 C49 166.0(2) . . . . no C50 N10 C46 C45 179.4(2) . . . . no Zn2 N10 C46 C45 11.1(3) . . . . no C46 N10 C50 C49 -1.1(4) . . . . no Zn2 N10 C46 C47 -167.90(18) . . . . no Zn2 N11 C55 C54 174.92(17) . . . . no C51 N11 C55 C56 179.78(19) . . . . no Zn2 N11 C55 C56 -4.1(2) . . . . no C51 N11 C55 C54 -1.2(3) . . . . no C55 N11 C51 C52 1.3(3) . . . . no Zn2 N11 C51 C52 -174.35(18) . . . . no C60 N12 C56 C57 -1.0(3) . . . . no C56 N12 C60 C59 0.5(3) . . . . no Zn2 N12 C56 C55 -10.2(2) . . . . no C60 N12 C56 C55 179.5(2) . . . . no Zn2 N12 C60 C59 -168.69(18) . . . . no Zn2 N12 C56 C57 169.32(17) . . . . no N1 C1 C2 C3 1.0(4) . . . . no C1 C2 C3 C4 0.0(4) . . . . no C2 C3 C4 C5 -1.4(4) . . . . no C3 C4 C5 C6 -177.8(2) . . . . no C3 C4 C5 N1 1.8(3) . . . . no N1 C5 C6 N2 -0.8(3) . . . . no C4 C5 C6 C7 -1.3(3) . . . . no C4 C5 C6 N2 178.9(2) . . . . no N1 C5 C6 C7 179.0(2) . . . . no N2 C6 C7 C8 -0.4(3) . . . . no C5 C6 C7 C8 179.9(2) . . . . no C6 C7 C8 C9 0.4(4) . . . . no C7 C8 C9 C10 -0.1(4) . . . . no C8 C9 C10 N2 -0.1(4) . . . . no N3 C11 C12 C13 -0.2(4) . . . . no C11 C12 C13 C14 1.2(4) . . . . no C12 C13 C14 C15 -0.7(4) . . . . no C13 C14 C15 C16 179.9(2) . . . . no C13 C14 C15 N3 -0.9(4) . . . . no C14 C15 C16 C17 -4.5(3) . . . . no N3 C15 C16 C17 176.2(2) . . . . no N3 C15 C16 N4 -3.9(3) . . . . no C14 C15 C16 N4 175.3(2) . . . . no C15 C16 C17 C18 179.5(2) . . . . no N4 C16 C17 C18 -0.3(3) . . . . no C16 C17 C18 C19 -0.3(4) . . . . no C17 C18 C19 C20 0.4(4) . . . . no C18 C19 C20 N4 0.1(4) . . . . no N5 C21 C22 C23 1.2(3) . . . . no C21 C22 C23 C24 -0.3(3) . . . . no C22 C23 C24 C25 -0.4(3) . . . . no C23 C24 C25 C26 -178.4(2) . . . . no C23 C24 C25 N5 0.3(3) . . . . no N5 C25 C26 C27 174.9(2) . . . . no C24 C25 C26 N6 174.0(2) . . . . no C24 C25 C26 C27 -6.3(3) . . . . no N5 C25 C26 N6 -4.8(3) . . . . no C25 C26 C27 C28 -179.3(2) . . . . no N6 C26 C27 C28 0.4(3) . . . . no C26 C27 C28 C29 -1.2(3) . . . . no C27 C28 C29 C30 1.0(3) . . . . no C28 C29 C30 N6 0.1(3) . . . . no N7 C31 C32 C33 -0.9(4) . . . . no C31 C32 C33 C34 0.6(5) . . . . no C32 C33 C34 C35 0.4(5) . . . . no C33 C34 C35 C36 177.3(3) . . . . no C33 C34 C35 N7 -1.3(4) . . . . no C34 C35 C36 C37 8.0(4) . . . . no N7 C35 C36 N8 7.4(3) . . . . no N7 C35 C36 C37 -173.3(2) . . . . no C34 C35 C36 N8 -171.2(2) . . . . no N8 C36 C37 C38 1.0(4) . . . . no C35 C36 C37 C38 -178.2(3) . . . . no C36 C37 C38 C39 0.9(5) . . . . no C37 C38 C39 C40 -1.5(5) . . . . no C38 C39 C40 N8 0.2(5) . . . . no N9 C41 C42 C43 -0.7(4) . . . . no C41 C42 C43 C44 0.5(4) . . . . no C42 C43 C44 C45 0.7(4) . . . . no C43 C44 C45 C46 177.9(3) . . . . no C43 C44 C45 N9 -1.9(4) . . . . no N9 C45 C46 C47 170.4(2) . . . . no C44 C45 C46 C47 -9.4(4) . . . . no N9 C45 C46 N10 -8.7(3) . . . . no C44 C45 C46 N10 171.6(2) . . . . no N10 C46 C47 C48 0.7(4) . . . . no C45 C46 C47 C48 -178.3(2) . . . . no C46 C47 C48 C49 -1.1(4) . . . . no C47 C48 C49 C50 0.5(4) . . . . no C48 C49 C50 N10 0.7(4) . . . . no N11 C51 C52 C53 -0.5(4) . . . . no C51 C52 C53 C54 -0.4(4) . . . . no C52 C53 C54 C55 0.4(4) . . . . no C53 C54 C55 C56 179.3(2) . . . . no C53 C54 C55 N11 0.4(4) . . . . no C54 C55 C56 C57 11.1(3) . . . . no C54 C55 C56 N12 -169.4(2) . . . . no N11 C55 C56 N12 9.6(3) . . . . no N11 C55 C56 C57 -169.9(2) . . . . no N12 C56 C57 C58 0.9(3) . . . . no C55 C56 C57 C58 -179.7(2) . . . . no C56 C57 C58 C59 -0.2(4) . . . . no C57 C58 C59 C60 -0.3(4) . . . . no C58 C59 C60 N12 0.1(4) . . . . no O2 C61 C62 O5 -170.4(2) . . . . no O4 C61 C62 O3 -168.7(2) . . . . no O4 C61 C62 O5 10.4(4) . . . . no O2 C61 C62 O3 10.5(3) . . . . no O8 C63 C64 O7 -175.2(2) . . . . no O6 C63 C64 O9 -177.4(2) . . . . no O8 C63 C64 O9 4.2(4) . . . . no O6 C63 C64 O7 3.2(3) . . . . no O10 C65 C66 O11 1.3(3) . . . . no O12 C65 C66 O13 1.8(3) . . . . no O10 C65 C66 O13 -179.0(2) . . . . no O12 C65 C66 O11 -178.0(2) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O14 H141 O9 0.84(2) 2.07(3) 2.889(3) 163(3) . no O14 H142 O4 0.84(3) 2.03(3) 2.840(3) 162(4) 3_666 no O15 H151 O14 0.84(2) 1.96(2) 2.776(3) 166(2) . no O15 H152 O3 0.85(2) 2.302(17) 3.107(3) 159(3) 1_545 no O16 H161 O15 0.84(2) 1.99(3) 2.807(4) 165(4) . no O16 H162 O21 0.845(17) 1.90(2) 2.736(4) 170(4) 1_545 no O17 H171 O16 0.84(2) 1.95(3) 2.780(4) 170(3) . no O17 H172 O20 0.84(2) 2.08(3) 2.764(4) 138(2) . no O17 H173 O18 0.845(17) 1.920(12) 2.700(4) 153(3) . no O18 H181 O8 0.82(3) 1.99(3) 2.788(4) 165(4) . no O18 H182 O17 0.84(2) 1.933(10) 2.700(4) 151(4) . no O18 H183 O19 0.84(5) 2.01(5) 2.769(4) 150(7) . no O19 H191 Cl1 0.82(2) 2.43(2) 3.251(2) 174(2) 3_566 no O19 H192 O18 0.83(3) 1.94(3) 2.769(4) 175(6) . no O19 H193 O19 0.83(4) 2.01(4) 2.806(3) 163(5) 3_566 no O20 H201 Cl1 0.831(13) 2.406(13) 3.204(3) 162(2) 3_566 no O20 H202 O20 0.852(14) 2.07(2) 2.817(4) 146(2) 3_556 no O20 H203 O17 0.85(4) 1.97(5) 2.764(4) 156(4) . no O21 H211 Cl1 0.84(2) 2.42(2) 3.258(3) 172(3) . no O21 H212 O10 0.84(3) 2.13(3) 2.896(3) 151(3) . no O22 H221 Cl1 0.84(3) 2.31(3) 3.147(3) 176(3) . no O22 H222 O8 0.83(3) 2.38(3) 3.184(4) 162(2) . no O23 H231 O12 0.833(18) 2.349(15) 2.943(2) 129(2) . no O23 H231 O13 0.833(18) 2.16(2) 2.934(2) 155.5(19) . no O23 H232 O24 0.83(2) 1.942(18) 2.743(3) 161(2) . no O24 H241 O1 0.84(3) 2.03(3) 2.857(3) 170(4) 4_564 no O24 H242 O22 0.84(3) 1.97(3) 2.796(3) 170(4) 4_564 no C4 H4 O23 0.9300 2.4800 3.399(3) 168.00 1_545 no C8 H8 O15 0.9300 2.3700 3.239(3) 156.00 . no C12 H12 O16 0.9300 2.3900 3.252(4) 155.00 4_554 no C19 H19 Cl1 0.9300 2.7500 3.482(3) 137.00 . no C27 H27 O23 0.9300 2.4600 3.379(3) 169.00 2_545 no C33 H33 O1 0.9300 2.4300 3.275(3) 150.00 4_564 no C39 H39 O9 0.9300 2.5500 3.407(4) 154.00 . no C47 H47 O23 0.9300 2.5300 3.432(3) 164.00 1_545 no C49 H49 O5 0.9300 2.5000 3.323(4) 147.00 1_545 no C54 H54 O11 0.9300 2.5200 3.155(3) 125.00 2_645 no C57 H57 O13 0.9300 2.3900 3.313(3) 170.00 2_645 no #===END