# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1649 data_global _publ_contact_author ; Prof. Maurizio Lanfranchi Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universit\`a degli Studi di Parma Viale delle Scienze 78 I-43100 Parma Italy ; _publ_contact_letter ; Date April 22, 1999 Re: Paper submitted to Dalton Communications 9/05424C we are sending you the CIF files of the structures inserted in the paper submitted to Dalton Communications. The cif- files were already deposited to the CCDC (115090 and 115091). Yours Sincerely Maurizio Lanfranchi ; _publ_contact_author_phone '[int.code]521 905 424' _publ_contact_author_fax '[int.code]521 905 557' _publ_contact_author_email 'chimic4@ipruniv.cce.unipr.it' _publ_requested_journal 'Dalton Communications' _publ_requested_coeditor_name ? _publ_section_title ; A novel lithium compound [(Li(H2O)(bdmpza))4 = lithium, aquo bis(3,5-dimethylpyrazol-1-yl)acetate], a precursor of a new type of monoanionic "scorpionate" ligand. ; loop_ _publ_author_name ; A. Otero J. Fernandez-Baeza J. Tejeda A. Antinolo F. Carrillo-Hermosilla E. Diez-Barra A. Lara-Sanchez M. Fernandez-Lopez M. Lanfranchi M. A. Pellinghelli ; _publ_author_address ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universit`a degli Studi di Parma Centro di Studio per la Strutturistica Diffrattometrica del CNR Viale delle Scienze 78 I-43100 Parma Italy ; #-------------------------- data section of block ---------------------- data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H68 Li4 N16 O12' _chemical_formula_weight 1088.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.355(8) _cell_length_b 8.966(3) _cell_length_c 25.515(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.28(2) _cell_angle_gamma 90.00 _cell_volume 5704(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 20 _cell_measurement_theta_max 39 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED diffractometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5486 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 70.05 _reflns_number_total 5365 _reflns_number_gt 3909 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00034(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5365 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1760 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.943 _refine_ls_shift/su_mean 0.018 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.47537(14) 0.2347(4) 0.66765(16) 0.0521(8) Uani 1 d . . . O1 O 0.54468(6) 0.26068(18) 0.72538(7) 0.0605(4) Uani 1 d . . . O2 O 0.58229(6) 0.32436(19) 0.81801(7) 0.0605(4) Uani 1 d . . . C1 C 0.62356(7) 0.4032(2) 0.75616(9) 0.0470(4) Uani 1 d . . . H1 H 0.6049 0.4776 0.7265 0.046(5) Uiso 1 calc R . . C2 C 0.57940(8) 0.3204(2) 0.76830(9) 0.0486(4) Uani 1 d . . . N1A N 0.65233(7) 0.63618(18) 0.80589(8) 0.0523(4) Uani 1 d . . . N2A N 0.66095(6) 0.48615(19) 0.80554(7) 0.0496(4) Uani 1 d . . . C1A C 0.69800(9) 0.4374(3) 0.85663(10) 0.0581(5) Uani 1 d . . . C2A C 0.71484(9) 0.5614(3) 0.89119(11) 0.0624(6) Uani 1 d . . . H2A H 0.7405 0.5646 0.9289 0.073(8) Uiso 1 calc R . . C3A C 0.68557(8) 0.6817(3) 0.85824(10) 0.0577(5) Uani 1 d . . . C4A C 0.71410(12) 0.2779(3) 0.86976(14) 0.0825(8) Uani 1 d . . . H4A1 H 0.6841 0.2210 0.8690 0.124 Uiso 1 calc R . . H4A2 H 0.7430 0.2708 0.9072 0.124 Uiso 1 calc R . . H4A3 H 0.7255 0.2394 0.8415 0.124 Uiso 1 calc R . . C5A C 0.68693(12) 0.8423(3) 0.87498(13) 0.0784(8) Uani 1 d . . . H5A1 H 0.7158 0.8919 0.8700 0.118 Uiso 1 calc R . . H5A2 H 0.6923 0.8488 0.9145 0.118 Uiso 1 calc R . . H5A3 H 0.6536 0.8890 0.8511 0.118 Uiso 1 calc R . . N1B N 0.65092(7) 0.15359(19) 0.73810(8) 0.0548(4) Uani 1 d . . . N2B N 0.65087(7) 0.30510(19) 0.73183(7) 0.0499(4) Uani 1 d . . . C1B C 0.67659(9) 0.3466(3) 0.69863(10) 0.0567(5) Uani 1 d . . . C2B C 0.69385(10) 0.2167(3) 0.68334(11) 0.0675(6) Uani 1 d . . . H2B H 0.7131 0.2077 0.6608 0.078(8) Uiso 1 calc R . . C3B C 0.67684(9) 0.1007(3) 0.70819(10) 0.0579(5) Uani 1 d . . . C4B C 0.68156(11) 0.5055(3) 0.68447(12) 0.0754(7) Uani 1 d . . . H4B1 H 0.6467 0.5511 0.6690 0.113 Uiso 1 calc R . . H4B2 H 0.6967 0.5103 0.6566 0.113 Uiso 1 calc R . . H4B3 H 0.7045 0.5574 0.7187 0.113 Uiso 1 calc R . . C5B C 0.68234(12) -0.0635(3) 0.70245(14) 0.0800(8) Uani 1 d . . . H5B1 H 0.6801 -0.1137 0.7346 0.120 Uiso 1 calc R . . H5B2 H 0.7164 -0.0845 0.7015 0.120 Uiso 1 calc R . . H5B3 H 0.6540 -0.0980 0.6675 0.120 Uiso 1 calc R . . Li2 Li 0.57438(14) 0.7376(4) 0.76087(15) 0.0518(7) Uani 1 d . . . O1' O 0.53305(7) 0.64490(19) 0.68904(7) 0.0639(4) Uani 1 d . . . O2' O 0.45321(7) 0.71857(19) 0.68393(6) 0.0635(4) Uani 1 d . . . C1' C 0.45379(8) 0.5651(2) 0.61002(8) 0.0469(4) Uani 1 d . . . H1' H 0.4318 0.4909 0.6186 0.054(6) Uiso 1 calc R . . C2' C 0.48299(9) 0.6529(2) 0.66615(8) 0.0503(5) Uani 1 d . . . N1A' N 0.48779(7) 0.32837(18) 0.59625(7) 0.0497(4) Uani 1 d . . . N2A' N 0.48873(7) 0.48076(18) 0.59111(7) 0.0469(4) Uani 1 d . . . C1A' C 0.52904(9) 0.5264(2) 0.57676(9) 0.0529(5) Uani 1 d . . . C2A' C 0.55386(9) 0.3988(3) 0.57071(10) 0.0585(5) Uani 1 d . . . H2A' H 0.5824 0.3928 0.5600 0.071(8) Uiso 1 calc R . . C3A' C 0.52786(9) 0.2795(2) 0.58374(9) 0.0545(5) Uani 1 d . . . C4A' C 0.54083(11) 0.6857(3) 0.56982(11) 0.0669(6) Uani 1 d . . . H4A4 H 0.5084 0.7350 0.5449 0.100 Uiso 1 calc R . . H4A5 H 0.5667 0.6910 0.5534 0.100 Uiso 1 calc R . . H4A6 H 0.5550 0.7338 0.6067 0.100 Uiso 1 calc R . . C5A' C 0.53944(11) 0.1164(3) 0.58424(12) 0.0700(7) Uani 1 d . . . H5A4 H 0.5510 0.0786 0.6227 0.105 Uiso 1 calc R . . H5A5 H 0.5672 0.1010 0.5710 0.105 Uiso 1 calc R . . H5A6 H 0.5076 0.0649 0.5594 0.105 Uiso 1 calc R . . N1B' N 0.42361(7) 0.8088(2) 0.56291(8) 0.0562(4) Uani 1 d . . . N2B' N 0.41598(7) 0.65907(19) 0.56470(7) 0.0503(4) Uani 1 d . . . C1B' C 0.37016(9) 0.6127(3) 0.52130(10) 0.0603(5) Uani 1 d . . . C2B' C 0.34755(10) 0.7383(3) 0.48987(11) 0.0696(7) Uani 1 d . . . H2B' H 0.3158 0.7432 0.4568 0.089(10) Uiso 1 calc R . . C3B' C 0.38134(10) 0.8568(3) 0.51703(10) 0.0624(6) Uani 1 d . . . C4B' C 0.35240(12) 0.4541(3) 0.51309(14) 0.0836(8) Uani 1 d . . . H4B4 H 0.3789 0.3941 0.5074 0.125 Uiso 1 calc R . . H4B5 H 0.3189 0.4461 0.4800 0.125 Uiso 1 calc R . . H4B6 H 0.3480 0.4198 0.5465 0.125 Uiso 1 calc R . . C5B' C 0.37536(14) 1.0186(3) 0.50261(15) 0.0907(9) Uani 1 d . . . H5B4 H 0.3495 1.0616 0.5146 0.136 Uiso 1 calc R . . H5B5 H 0.3634 1.0308 0.4618 0.136 Uiso 1 calc R . . H5B6 H 0.4093 1.0676 0.5221 0.136 Uiso 1 calc R . . O1W O 0.46253(8) 0.0226(2) 0.66006(9) 0.0731(5) Uani 1 d . . . H1W1 H 0.4478(15) -0.012(5) 0.6864(16) 0.116(13) Uiso 1 d . . . H2W1 H 0.4539(16) -0.043(5) 0.6291(18) 0.125(14) Uiso 1 d . . . O2W O 0.57418(8) 0.94965(19) 0.74801(9) 0.0700(5) Uani 1 d . . . H1W2 H 0.5984(12) 1.030(3) 0.7453(12) 0.081(8) Uiso 1 d . . . H2W2 H 0.545(2) 0.969(6) 0.713(2) 0.17(2) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0535(17) 0.0460(17) 0.0600(19) -0.0014(14) 0.0264(15) -0.0033(14) O1 0.0495(7) 0.0625(9) 0.0690(9) -0.0100(7) 0.0239(7) -0.0081(7) O2 0.0631(9) 0.0611(9) 0.0681(9) -0.0083(7) 0.0378(8) -0.0113(7) C1 0.0460(9) 0.0411(9) 0.0568(11) 0.0013(8) 0.0241(8) 0.0003(8) C2 0.0465(10) 0.0403(9) 0.0639(12) -0.0033(8) 0.0277(9) 0.0005(8) N1A 0.0518(9) 0.0397(9) 0.0678(11) -0.0015(7) 0.0269(8) -0.0003(7) N2A 0.0469(8) 0.0407(8) 0.0607(10) 0.0003(7) 0.0216(7) -0.0016(7) C1A 0.0513(11) 0.0504(11) 0.0709(13) 0.0035(10) 0.0233(10) -0.0020(9) C2A 0.0541(11) 0.0601(13) 0.0661(13) -0.0019(10) 0.0175(10) -0.0057(10) C3A 0.0505(11) 0.0522(12) 0.0719(13) -0.0096(10) 0.0267(10) -0.0060(9) C4A 0.0786(17) 0.0589(15) 0.0897(19) 0.0124(13) 0.0140(15) 0.0091(12) C5A 0.0760(16) 0.0597(15) 0.0911(18) -0.0202(13) 0.0258(14) -0.0067(12) N1B 0.0583(10) 0.0414(9) 0.0722(11) 0.0015(8) 0.0345(9) 0.0028(7) N2B 0.0528(9) 0.0420(8) 0.0625(10) 0.0002(7) 0.0312(8) -0.0015(7) C1B 0.0546(11) 0.0599(13) 0.0641(12) 0.0016(10) 0.0330(10) -0.0060(9) C2B 0.0641(13) 0.0774(16) 0.0739(15) -0.0102(12) 0.0413(12) -0.0047(12) C3B 0.0538(11) 0.0542(12) 0.0695(13) -0.0068(10) 0.0294(10) 0.0035(9) C4B 0.0838(17) 0.0667(15) 0.0860(17) 0.0112(13) 0.0455(15) -0.0128(13) C5B 0.0785(17) 0.0618(15) 0.103(2) -0.0130(14) 0.0401(15) 0.0121(13) Li2 0.0552(18) 0.0460(17) 0.0565(18) -0.0005(14) 0.0251(15) 0.0032(14) O1' 0.0652(9) 0.0631(10) 0.0564(8) -0.0079(7) 0.0178(7) 0.0093(7) O2' 0.0799(10) 0.0614(10) 0.0585(9) -0.0032(7) 0.0377(8) 0.0108(8) C1' 0.0531(10) 0.0411(10) 0.0498(10) 0.0011(8) 0.0243(8) 0.0030(8) C2' 0.0642(12) 0.0403(10) 0.0482(10) 0.0045(8) 0.0251(9) 0.0063(8) N1A' 0.0603(10) 0.0396(8) 0.0544(9) 0.0007(7) 0.0288(8) 0.0035(7) N2A' 0.0559(9) 0.0402(8) 0.0491(8) 0.0010(6) 0.0262(7) 0.0027(7) C1A' 0.0597(11) 0.0518(12) 0.0516(10) -0.0004(9) 0.0275(9) -0.0024(9) C2A' 0.0600(12) 0.0625(13) 0.0630(12) -0.0021(10) 0.0352(10) 0.0033(10) C3A' 0.0631(12) 0.0519(12) 0.0530(11) -0.0009(9) 0.0286(9) 0.0077(9) C4A' 0.0743(15) 0.0589(13) 0.0755(15) 0.0067(11) 0.0387(12) -0.0074(11) C5A' 0.0832(16) 0.0543(13) 0.0785(16) 0.0008(11) 0.0392(14) 0.0153(12) N1B' 0.0598(10) 0.0458(9) 0.0611(10) 0.0045(8) 0.0229(8) 0.0033(8) N2B' 0.0537(9) 0.0443(9) 0.0507(9) 0.0013(7) 0.0194(7) 0.0016(7) C1B' 0.0538(11) 0.0613(13) 0.0624(12) -0.0093(10) 0.0205(10) 0.0026(10) C2B' 0.0590(13) 0.0729(16) 0.0659(14) 0.0000(12) 0.0145(11) 0.0135(11) C3B' 0.0643(13) 0.0587(13) 0.0620(13) 0.0098(10) 0.0237(11) 0.0140(11) C4B' 0.0719(16) 0.0657(16) 0.101(2) -0.0212(15) 0.0233(15) -0.0061(13) C5B' 0.092(2) 0.0678(17) 0.105(2) 0.0289(16) 0.0333(17) 0.0246(15) O1W 0.0984(13) 0.0488(9) 0.0781(12) -0.0056(8) 0.0423(11) -0.0139(9) O2W 0.0702(10) 0.0482(9) 0.0970(13) 0.0148(8) 0.0398(10) 0.0015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O1 1.877(4) . ? Li1 O1W 1.929(4) . ? Li1 O2 1.934(4) 2_656 ? Li1 N1A' 2.156(4) . ? Li1 C2 2.742(4) 2_656 ? O1 C2 1.238(3) . ? O2 C2 1.238(3) . ? O2 Li1 1.934(4) 2_656 ? C1 N2B 1.449(2) . ? C1 N2A 1.458(3) . ? C1 C2 1.554(3) . ? C1 H1 0.9800 . ? C2 Li1 2.742(4) 2_656 ? N1A C3A 1.334(3) . ? N1A N2A 1.366(2) . ? N1A Li2 2.163(4) . ? N2A C1A 1.353(3) . ? C1A C2A 1.375(3) . ? C1A C4A 1.493(4) . ? C2A C3A 1.399(3) . ? C2A H2A 0.9300 . ? C3A C5A 1.498(3) . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C4A H4A3 0.9600 . ? C5A H5A1 0.9600 . ? C5A H5A2 0.9600 . ? C5A H5A3 0.9600 . ? N1B C3B 1.325(3) . ? N1B N2B 1.368(2) . ? N2B C1B 1.357(3) . ? C1B C2B 1.373(3) . ? C1B C4B 1.489(3) . ? C2B C3B 1.393(4) . ? C2B H2B 0.9300 . ? C3B C5B 1.494(3) . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? C5B H5B1 0.9600 . ? C5B H5B2 0.9600 . ? C5B H5B3 0.9600 . ? Li2 O2' 1.859(4) 2_656 ? Li2 O1' 1.904(4) . ? Li2 O2W 1.929(4) . ? Li2 C2' 2.775(4) . ? O1' C2' 1.250(3) . ? O2' C2' 1.233(3) . ? O2' Li2 1.859(4) 2_656 ? C1' N2A' 1.448(2) . ? C1' N2B' 1.461(3) . ? C1' C2' 1.539(3) . ? C1' H1' 0.9800 . ? N1A' C3A' 1.335(3) . ? N1A' N2A' 1.374(2) . ? N2A' C1A' 1.360(3) . ? C1A' C2A' 1.371(3) . ? C1A' C4A' 1.491(3) . ? C2A' C3A' 1.398(3) . ? C2A' H2A' 0.9300 . ? C3A' C5A' 1.495(3) . ? C4A' H4A4 0.9600 . ? C4A' H4A5 0.9600 . ? C4A' H4A6 0.9600 . ? C5A' H5A4 0.9600 . ? C5A' H5A5 0.9600 . ? C5A' H5A6 0.9600 . ? N1B' C3B' 1.334(3) . ? N1B' N2B' 1.362(3) . ? N2B' C1B' 1.352(3) . ? C1B' C2B' 1.374(4) . ? C1B' C4B' 1.490(4) . ? C2B' C3B' 1.392(4) . ? C2B' H2B' 0.9300 . ? C3B' C5B' 1.489(4) . ? C4B' H4B4 0.9600 . ? C4B' H4B5 0.9600 . ? C4B' H4B6 0.9600 . ? C5B' H5B4 0.9600 . ? C5B' H5B5 0.9600 . ? C5B' H5B6 0.9600 . ? O1W H1W1 0.97(4) . ? O1W H2W1 0.94(5) . ? O2W H1W2 1.00(3) . ? O2W H2W2 0.93(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 O1W 106.52(19) . . ? O1 Li1 O2 116.1(2) . 2_656 ? O1W Li1 O2 107.43(18) . 2_656 ? O1 Li1 N1A' 98.96(17) . . ? O1W Li1 N1A' 112.61(19) . . ? O2 Li1 N1A' 114.97(18) 2_656 . ? O1 Li1 C2 96.93(16) . 2_656 ? O1W Li1 C2 102.39(16) . 2_656 ? O2 Li1 C2 23.52(8) 2_656 2_656 ? N1A' Li1 C2 135.15(17) . 2_656 ? C2 O1 Li1 155.20(18) . . ? C2 O2 Li1 117.92(18) . 2_656 ? N2B C1 N2A 112.20(15) . . ? N2B C1 C2 112.05(16) . . ? N2A C1 C2 113.45(16) . . ? N2B C1 H1 106.2 . . ? N2A C1 H1 106.2 . . ? C2 C1 H1 106.2 . . ? O1 C2 O2 128.38(19) . . ? O1 C2 C1 114.01(18) . . ? O2 C2 C1 117.59(18) . . ? O1 C2 Li1 89.85(14) . 2_656 ? O2 C2 Li1 38.56(12) . 2_656 ? C1 C2 Li1 155.90(16) . 2_656 ? C3A N1A N2A 105.02(17) . . ? C3A N1A Li2 121.36(17) . . ? N2A N1A Li2 123.07(16) . . ? C1A N2A N1A 112.01(18) . . ? C1A N2A C1 130.47(18) . . ? N1A N2A C1 116.48(16) . . ? N2A C1A C2A 106.1(2) . . ? N2A C1A C4A 124.1(2) . . ? C2A C1A C4A 129.8(2) . . ? C1A C2A C3A 106.3(2) . . ? C1A C2A H2A 126.9 . . ? C3A C2A H2A 126.9 . . ? N1A C3A C2A 110.6(2) . . ? N1A C3A C5A 120.4(2) . . ? C2A C3A C5A 129.0(2) . . ? C1A C4A H4A1 109.5 . . ? C1A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C1A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C3A C5A H5A1 109.5 . . ? C3A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C3A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C3B N1B N2B 105.26(17) . . ? C1B N2B N1B 111.70(17) . . ? C1B N2B C1 126.29(18) . . ? N1B N2B C1 121.94(16) . . ? N2B C1B C2B 105.8(2) . . ? N2B C1B C4B 122.4(2) . . ? C2B C1B C4B 131.8(2) . . ? C1B C2B C3B 106.6(2) . . ? C1B C2B H2B 126.7 . . ? C3B C2B H2B 126.7 . . ? N1B C3B C2B 110.7(2) . . ? N1B C3B C5B 120.6(2) . . ? C2B C3B C5B 128.7(2) . . ? C1B C4B H4B1 109.5 . . ? C1B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C1B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C3B C5B H5B1 109.5 . . ? C3B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C3B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? O2' Li2 O1' 115.1(2) 2_656 . ? O2' Li2 O2W 104.24(18) 2_656 . ? O1' Li2 O2W 107.92(19) . . ? O2' Li2 N1A 100.23(17) 2_656 . ? O1' Li2 N1A 113.14(18) . . ? O2W Li2 N1A 115.98(19) . . ? O2' Li2 C2' 97.68(16) 2_656 . ? O1' Li2 C2' 22.51(8) . . ? O2W Li2 C2' 100.56(16) . . ? N1A Li2 C2' 133.28(16) . . ? C2' O1' Li2 121.84(18) . . ? C2' O2' Li2 149.10(19) . 2_656 ? N2A' C1' N2B' 112.77(15) . . ? N2A' C1' C2' 114.58(16) . . ? N2B' C1' C2' 111.66(16) . . ? N2A' C1' H1' 105.6 . . ? N2B' C1' H1' 105.7 . . ? C2' C1' H1' 105.7 . . ? O2' C2' O1' 128.2(2) . . ? O2' C2' C1' 114.71(19) . . ? O1' C2' C1' 117.08(18) . . ? O2' C2' Li2 92.50(15) . . ? O1' C2' Li2 35.65(12) . . ? C1' C2' Li2 152.59(15) . . ? C3A' N1A' N2A' 104.71(17) . . ? C3A' N1A' Li1 120.29(17) . . ? N2A' N1A' Li1 118.92(15) . . ? C1A' N2A' N1A' 111.97(16) . . ? C1A' N2A' C1' 130.68(17) . . ? N1A' N2A' C1' 116.52(15) . . ? N2A' C1A' C2A' 105.84(19) . . ? N2A' C1A' C4A' 124.0(2) . . ? C2A' C1A' C4A' 130.1(2) . . ? C1A' C2A' C3A' 106.72(19) . . ? C1A' C2A' H2A' 126.6 . . ? C3A' C2A' H2A' 126.6 . . ? N1A' C3A' C2A' 110.73(19) . . ? N1A' C3A' C5A' 120.7(2) . . ? C2A' C3A' C5A' 128.6(2) . . ? C1A' C4A' H4A4 109.5 . . ? C1A' C4A' H4A5 109.5 . . ? H4A4 C4A' H4A5 109.5 . . ? C1A' C4A' H4A6 109.5 . . ? H4A4 C4A' H4A6 109.5 . . ? H4A5 C4A' H4A6 109.5 . . ? C3A' C5A' H5A4 109.5 . . ? C3A' C5A' H5A5 109.5 . . ? H5A4 C5A' H5A5 109.5 . . ? C3A' C5A' H5A6 109.5 . . ? H5A4 C5A' H5A6 109.5 . . ? H5A5 C5A' H5A6 109.5 . . ? C3B' N1B' N2B' 104.95(18) . . ? C1B' N2B' N1B' 112.26(18) . . ? C1B' N2B' C1' 125.94(18) . . ? N1B' N2B' C1' 121.79(16) . . ? N2B' C1B' C2B' 105.6(2) . . ? N2B' C1B' C4B' 123.2(2) . . ? C2B' C1B' C4B' 131.2(2) . . ? C1B' C2B' C3B' 106.7(2) . . ? C1B' C2B' H2B' 126.6 . . ? C3B' C2B' H2B' 126.6 . . ? N1B' C3B' C2B' 110.4(2) . . ? N1B' C3B' C5B' 119.9(2) . . ? C2B' C3B' C5B' 129.6(2) . . ? C1B' C4B' H4B4 109.5 . . ? C1B' C4B' H4B5 109.5 . . ? H4B4 C4B' H4B5 109.5 . . ? C1B' C4B' H4B6 109.5 . . ? H4B4 C4B' H4B6 109.5 . . ? H4B5 C4B' H4B6 109.5 . . ? C3B' C5B' H5B4 109.5 . . ? C3B' C5B' H5B5 109.5 . . ? H5B4 C5B' H5B5 109.5 . . ? C3B' C5B' H5B6 109.5 . . ? H5B4 C5B' H5B6 109.5 . . ? H5B5 C5B' H5B6 109.5 . . ? Li1 O1W H1W1 111(2) . . ? Li1 O1W H2W1 133(3) . . ? H1W1 O1W H2W1 111(3) . . ? Li2 O2W H1W2 139.9(17) . . ? Li2 O2W H2W2 106(4) . . ? H1W2 O2W H2W2 98(4) . . ? _diffrn_measured_fraction_theta_max 0.465 _diffrn_reflns_theta_full 70.05 _diffrn_measured_fraction_theta_full 0.465 _refine_diff_density_max 0.313 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.059 #=END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C21 H23 Cl2 N4 Nb O2, C H2 Cl2' _chemical_formula_sum 'C22 H25 Cl4 N4 Nb O2' _chemical_formula_weight 612.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.242(7) _cell_length_b 8.024(3) _cell_length_c 34.146(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.30(2) _cell_angle_gamma 90.00 _cell_volume 5271(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 10 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW 1100 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7787 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7677 _reflns_number_gt 4042 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7677 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.245 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb Nb 0.413093(19) 0.14328(5) 0.141752(10) 0.03038(12) Uani 1 d . . . Cl1 Cl 0.29161(6) 0.19621(17) 0.12939(4) 0.0492(3) Uani 1 d . . . Cl2 Cl 0.41524(7) -0.02061(17) 0.19974(3) 0.0536(3) Uani 1 d . . . O1 O 0.42909(15) 0.2092(4) 0.08320(8) 0.0350(7) Uani 1 d . . . O2 O 0.4499(2) 0.1551(4) 0.02088(8) 0.0535(9) Uani 1 d . . . N1A N 0.38963(17) -0.1171(4) 0.11098(9) 0.0334(8) Uani 1 d . . . N2A N 0.43054(18) -0.1645(4) 0.08006(9) 0.0319(8) Uani 1 d . . . C1A C 0.4147(2) -0.3203(5) 0.06735(13) 0.0387(10) Uani 1 d . . . C2A C 0.3621(3) -0.3740(6) 0.09044(14) 0.0457(11) Uani 1 d . . . H2A H 0.3399 -0.4768 0.0889 0.055 Uiso 1 calc R . . C3A C 0.3480(2) -0.2465(6) 0.11658(13) 0.0394(10) Uani 1 d . . . C4A C 0.4511(3) -0.4050(7) 0.03497(17) 0.0621(16) Uani 1 d . . . H4A1 H 0.4472 -0.3384 0.0117 0.093 Uiso 1 calc R . . H4A2 H 0.4303 -0.5120 0.0302 0.093 Uiso 1 calc R . . H4A3 H 0.4993 -0.4191 0.0421 0.093 Uiso 1 calc R . . C5A C 0.2931(3) -0.2476(7) 0.14776(15) 0.0546(14) Uani 1 d . . . H5A1 H 0.3137 -0.2831 0.1722 0.082 Uiso 1 calc R . . H5A2 H 0.2565 -0.3229 0.1402 0.082 Uiso 1 calc R . . H5A3 H 0.2745 -0.1374 0.1506 0.082 Uiso 1 calc R . . N1B N 0.52190(18) 0.0461(5) 0.13254(10) 0.0349(8) Uani 1 d . . . N2B N 0.53735(17) -0.0321(5) 0.09811(10) 0.0334(8) Uani 1 d . . . C1B C 0.6030(2) -0.0908(7) 0.09932(14) 0.0447(12) Uani 1 d . . . C2B C 0.6303(2) -0.0482(7) 0.13526(14) 0.0488(13) Uani 1 d . . . H2B H 0.6749 -0.0721 0.1446 0.059 Uiso 1 calc R . . C3B C 0.5801(2) 0.0357(6) 0.15499(13) 0.0404(11) Uani 1 d . . . C4B C 0.6348(3) -0.1835(9) 0.06570(17) 0.077(2) Uani 1 d . . . H4B1 H 0.6116 -0.2885 0.0622 0.115 Uiso 1 calc R . . H4B2 H 0.6833 -0.2024 0.0714 0.115 Uiso 1 calc R . . H4B3 H 0.6298 -0.1185 0.0422 0.115 Uiso 1 calc R . . C5B C 0.5859(3) 0.1100(8) 0.19522(14) 0.0602(15) Uani 1 d . . . H5B1 H 0.5656 0.2192 0.1950 0.090 Uiso 1 calc R . . H5B2 H 0.6341 0.1179 0.2030 0.090 Uiso 1 calc R . . H5B3 H 0.5620 0.0405 0.2134 0.090 Uiso 1 calc R . . C1 C 0.4849(2) -0.0516(5) 0.06752(11) 0.0300(9) Uani 1 d . . . H1 H 0.5069 -0.1004 0.0446 0.036 Uiso 1 calc R . . C2 C 0.4523(2) 0.1174(5) 0.05518(12) 0.0329(9) Uani 1 d . . . C3 C 0.4632(2) 0.3637(6) 0.15409(12) 0.0364(9) Uani 1 d . . . C4 C 0.4133(2) 0.3463(6) 0.17847(11) 0.0342(9) Uani 1 d . . . C5 C 0.5193(3) 0.4804(7) 0.14204(15) 0.0559(14) Uani 1 d . . . H5A H 0.5057 0.5930 0.1476 0.084 Uiso 1 calc R . . H5B H 0.5268 0.4686 0.1145 0.084 Uiso 1 calc R . . H5C H 0.5615 0.4547 0.1563 0.084 Uiso 1 calc R . . C6 C 0.3808(2) 0.4247(6) 0.21256(12) 0.0389(10) Uani 1 d . . . C7 C 0.4120(3) 0.5610(7) 0.23104(15) 0.0531(13) Uani 1 d . . . H7 H 0.4524 0.6064 0.2210 0.064 Uiso 1 calc R . . C8 C 0.3836(4) 0.6296(8) 0.26421(17) 0.0708(18) Uani 1 d . . . H8 H 0.4050 0.7197 0.2766 0.085 Uiso 1 calc R . . C9 C 0.3236(4) 0.5642(9) 0.27868(17) 0.075(2) Uani 1 d . . . H9 H 0.3047 0.6094 0.3011 0.090 Uiso 1 calc R . . C10 C 0.2914(3) 0.4330(10) 0.26033(17) 0.0739(19) Uani 1 d . . . H10 H 0.2503 0.3902 0.2700 0.089 Uiso 1 calc R . . C11 C 0.3203(3) 0.3646(8) 0.22755(15) 0.0562(14) Uani 1 d . . . H11 H 0.2982 0.2753 0.2152 0.067 Uiso 1 calc R . . Cl4 Cl 0.2288(2) 0.0243(6) 0.00479(11) 0.2070(17) Uani 1 d . . . Cl3 Cl 0.1616(3) -0.1823(6) 0.05910(13) 0.2232(19) Uani 1 d . . . C12 C 0.2410(6) -0.0861(15) 0.0446(3) 0.167(5) Uani 1 d . . . H12A H 0.2585 -0.0148 0.0655 0.200 Uiso 1 calc R . . H12B H 0.2756 -0.1715 0.0399 0.200 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb 0.03363(19) 0.0325(2) 0.02535(18) -0.00113(18) 0.00799(13) 0.00219(19) Cl1 0.0337(6) 0.0590(8) 0.0550(7) -0.0061(6) 0.0042(5) 0.0078(5) Cl2 0.0783(9) 0.0509(8) 0.0321(6) 0.0084(5) 0.0108(6) -0.0023(7) O1 0.0479(17) 0.0307(15) 0.0267(14) 0.0034(12) 0.0080(12) 0.0116(14) O2 0.085(3) 0.051(2) 0.0255(15) 0.0044(16) 0.0097(15) 0.0191(19) N1A 0.0370(18) 0.036(2) 0.0280(17) 0.0006(15) 0.0103(14) -0.0006(16) N2A 0.0390(18) 0.032(2) 0.0247(16) -0.0014(15) 0.0059(13) 0.0033(16) C1A 0.051(3) 0.027(2) 0.038(2) -0.0020(18) 0.002(2) 0.0023(19) C2A 0.059(3) 0.031(3) 0.048(3) 0.000(2) 0.007(2) -0.009(2) C3A 0.038(2) 0.039(3) 0.041(2) 0.004(2) 0.0042(19) -0.003(2) C4A 0.078(4) 0.039(3) 0.070(4) -0.017(3) 0.024(3) -0.002(3) C5A 0.056(3) 0.052(3) 0.056(3) -0.001(3) 0.020(2) -0.013(3) N1B 0.0378(19) 0.042(2) 0.0251(17) -0.0015(16) 0.0033(14) 0.0056(17) N2B 0.0319(18) 0.038(2) 0.0307(17) -0.0007(16) 0.0069(14) 0.0066(16) C1B 0.030(2) 0.057(3) 0.047(3) 0.003(2) 0.0070(19) 0.009(2) C2B 0.035(2) 0.063(4) 0.048(3) 0.001(3) -0.004(2) 0.008(2) C3B 0.038(2) 0.046(3) 0.037(2) 0.003(2) -0.0053(19) 0.001(2) C4B 0.048(3) 0.122(6) 0.060(3) -0.021(4) 0.006(3) 0.041(4) C5B 0.064(3) 0.075(4) 0.040(3) -0.010(3) -0.019(2) 0.004(3) C1 0.034(2) 0.032(2) 0.0249(19) -0.0012(17) 0.0090(16) 0.0038(18) C2 0.033(2) 0.036(3) 0.030(2) 0.0006(18) 0.0066(16) 0.0006(18) C3 0.041(2) 0.040(2) 0.0278(19) -0.001(2) 0.0033(16) 0.004(2) C4 0.041(2) 0.034(2) 0.0278(19) 0.0041(19) 0.0037(16) 0.006(2) C5 0.056(3) 0.066(4) 0.046(3) -0.001(3) 0.009(2) -0.019(3) C6 0.047(3) 0.039(3) 0.032(2) 0.000(2) 0.0079(19) 0.007(2) C7 0.068(4) 0.047(3) 0.045(3) -0.005(2) 0.009(2) 0.011(3) C8 0.099(5) 0.061(4) 0.052(3) -0.024(3) 0.005(3) 0.024(4) C9 0.090(5) 0.092(5) 0.045(3) -0.010(3) 0.018(3) 0.049(4) C10 0.066(4) 0.100(5) 0.057(4) -0.005(4) 0.028(3) 0.015(4) C11 0.056(3) 0.068(4) 0.044(3) -0.008(3) 0.018(2) -0.001(3) Cl4 0.193(4) 0.263(5) 0.167(3) -0.022(3) 0.049(3) -0.014(3) Cl3 0.272(5) 0.194(4) 0.204(4) 0.062(3) 0.010(4) 0.004(4) C12 0.222(13) 0.153(10) 0.122(9) -0.014(8) -0.096(9) 0.077(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb C4 2.055(4) . ? Nb C3 2.053(5) . ? Nb O1 2.098(3) . ? Nb N1B 2.263(3) . ? Nb Cl2 2.3767(13) . ? Nb N1A 2.377(4) . ? Nb Cl1 2.4037(14) . ? O1 C2 1.295(5) . ? O2 C2 1.209(5) . ? N1A C3A 1.328(5) . ? N1A N2A 1.384(4) . ? N2A C1A 1.356(5) . ? N2A C1 1.456(5) . ? C1A C2A 1.367(6) . ? C1A C4A 1.486(6) . ? C2A C3A 1.388(6) . ? C2A H2A 0.9300 . ? C3A C5A 1.516(6) . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C4A H4A3 0.9600 . ? C5A H5A1 0.9600 . ? C5A H5A2 0.9600 . ? C5A H5A3 0.9600 . ? N1B C3B 1.345(5) . ? N1B N2B 1.371(5) . ? N2B C1B 1.348(5) . ? N2B C1 1.444(5) . ? C1B C2B 1.367(7) . ? C1B C4B 1.509(7) . ? C2B C3B 1.367(6) . ? C2B H2B 0.9300 . ? C3B C5B 1.499(6) . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? C5B H5B1 0.9600 . ? C5B H5B2 0.9600 . ? C5B H5B3 0.9600 . ? C1 C2 1.548(6) . ? C1 H1 0.9800 . ? C3 C4 1.293(5) . ? C3 C5 1.495(6) . ? C4 C6 1.475(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C11 1.370(7) . ? C6 C7 1.392(7) . ? C7 C8 1.383(7) . ? C7 H7 0.9300 . ? C8 C9 1.370(9) . ? C8 H8 0.9300 . ? C9 C10 1.367(10) . ? C9 H9 0.9300 . ? C10 C11 1.375(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? Cl4 C12 1.634(10) . ? Cl3 C12 1.792(13) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Nb C3 36.68(15) . . ? C4 Nb O1 112.54(14) . . ? C3 Nb O1 84.26(14) . . ? C4 Nb N1B 111.68(15) . . ? C3 Nb N1B 83.92(16) . . ? O1 Nb N1B 78.36(12) . . ? C4 Nb Cl2 86.02(12) . . ? C3 Nb Cl2 107.85(12) . . ? O1 Nb Cl2 158.99(9) . . ? N1B Nb Cl2 85.78(10) . . ? C4 Nb N1A 164.52(14) . . ? C3 Nb N1A 158.63(14) . . ? O1 Nb N1A 80.26(12) . . ? N1B Nb N1A 78.62(13) . . ? Cl2 Nb N1A 83.20(9) . . ? C4 Nb Cl1 87.43(12) . . ? C3 Nb Cl1 109.51(13) . . ? O1 Nb Cl1 87.21(9) . . ? N1B Nb Cl1 159.33(9) . . ? Cl2 Nb Cl1 104.03(5) . . ? N1A Nb Cl1 84.46(9) . . ? C2 O1 Nb 128.4(3) . . ? C3A N1A N2A 104.5(3) . . ? C3A N1A Nb 137.1(3) . . ? N2A N1A Nb 118.2(2) . . ? C1A N2A N1A 111.7(3) . . ? C1A N2A C1 129.6(3) . . ? N1A N2A C1 118.6(3) . . ? N2A C1A C2A 105.6(4) . . ? N2A C1A C4A 123.6(4) . . ? C2A C1A C4A 130.7(4) . . ? C3A C2A C1A 107.3(4) . . ? C3A C2A H2A 126.4 . . ? C1A C2A H2A 126.4 . . ? N1A C3A C2A 110.9(4) . . ? N1A C3A C5A 122.5(4) . . ? C2A C3A C5A 126.6(4) . . ? C1A C4A H4A1 109.5 . . ? C1A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C1A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C3A C5A H5A1 109.5 . . ? C3A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C3A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C3B N1B N2B 105.5(3) . . ? C3B N1B Nb 134.7(3) . . ? N2B N1B Nb 119.7(3) . . ? C1B N2B N1B 110.8(4) . . ? C1B N2B C1 128.6(4) . . ? N1B N2B C1 120.5(3) . . ? N2B C1B C2B 106.3(4) . . ? N2B C1B C4B 123.0(4) . . ? C2B C1B C4B 130.7(4) . . ? C1B C2B C3B 107.7(4) . . ? C1B C2B H2B 126.1 . . ? C3B C2B H2B 126.1 . . ? N1B C3B C2B 109.7(4) . . ? N1B C3B C5B 122.8(4) . . ? C2B C3B C5B 127.5(4) . . ? C1B C4B H4B1 109.5 . . ? C1B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C1B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C3B C5B H5B1 109.5 . . ? C3B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C3B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? N2A C1 N2B 110.5(3) . . ? N2A C1 C2 109.6(3) . . ? N2B C1 C2 112.0(3) . . ? N2A C1 H1 108.2 . . ? N2B C1 H1 108.2 . . ? C2 C1 H1 108.2 . . ? O2 C2 O1 124.5(4) . . ? O2 C2 C1 119.3(4) . . ? O1 C2 C1 116.2(3) . . ? C4 C3 C5 142.9(5) . . ? C4 C3 Nb 71.8(3) . . ? C5 C3 Nb 145.3(3) . . ? C3 C4 C6 142.8(5) . . ? C3 C4 Nb 71.6(3) . . ? C6 C4 Nb 145.6(3) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 118.0(4) . . ? C11 C6 C4 121.6(5) . . ? C7 C6 C4 120.5(4) . . ? C8 C7 C6 120.6(5) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 119.7(6) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 119.6(6) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C6 C11 C10 121.7(6) . . ? C6 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? Cl4 C12 Cl3 110.9(6) . . ? Cl4 C12 H12A 109.5 . . ? Cl3 C12 H12A 109.5 . . ? Cl4 C12 H12B 109.5 . . ? Cl3 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.468 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.468 _refine_diff_density_max 0.995 _refine_diff_density_min -1.299 _refine_diff_density_rms 0.124 #=END