# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- Structure.cif' _audit_creation_method SHELXL-97 _publ_contact_author_name 'Prof. Samar K. Das' _publ_contact_author_address ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; _publ_contact_author_email skdsc@uohyd.ernet.in _publ_contact_author_phone '91 40 23011007' _publ_contact_author_fax ? loop_ _publ_author_name _publ_author_address 'Monima Sarma' ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; 'Tanmay Chatterjee' ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; S.K.Das ; School of Chemistry University of Hyderabad Hyderabad 500 046, India ; data_Co-TDE-Cl2-Mo6 _database_code_depnum_ccdc_archive 'CCDC 776418' #TrackingRef '- Structure.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H32 Cl2 Co N4), Mo6 O19' _chemical_formula_sum 'C32 H64 Cl4 Co2 Mo6 N8 O19' _chemical_formula_weight 1700.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7302(8) _cell_length_b 11.3642(8) _cell_length_c 11.7568(9) _cell_angle_alpha 107.9180(10) _cell_angle_beta 101.7540(10) _cell_angle_gamma 95.4500(10) _cell_volume 1316.22(17) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5308 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.01 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 838 _exptl_absorpt_coefficient_mu 2.273 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6592 _exptl_absorpt_correction_T_max 0.7721 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12640 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4620 _reflns_number_gt 3980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.2951P] 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 4620 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1550(4) 0.2733(4) 1.0072(4) 0.0419(10) Uani 1 1 d . . . H1A H 1.2326 0.3342 1.0529 0.050 Uiso 1 1 calc R . . H1B H 1.1790 0.1907 0.9809 0.050 Uiso 1 1 calc R . . C2 C 1.0600(4) 0.2757(4) 1.0879(4) 0.0399(10) Uani 1 1 d . . . H2A H 1.0798 0.2215 1.1363 0.048 Uiso 1 1 calc R . . H2B H 1.0678 0.3604 1.1443 0.048 Uiso 1 1 calc R . . C3 C 0.8325(4) 0.2267(4) 1.0602(4) 0.0377(9) Uani 1 1 d . . . C4 C 0.6962(4) 0.1911(4) 0.9845(4) 0.0448(11) Uani 1 1 d . . . H4A H 0.6715 0.2635 0.9642 0.054 Uiso 1 1 calc R . . H4B H 0.6416 0.1730 1.0355 0.054 Uiso 1 1 calc R . . C5 C 0.6667(4) 0.0798(4) 0.8651(4) 0.0405(10) Uani 1 1 d . . . C6 C 0.7178(5) 0.0280(4) 0.6549(4) 0.0497(11) Uani 1 1 d . . . H6A H 0.6270 0.0012 0.6131 0.060 Uiso 1 1 calc R . . H6B H 0.7548 -0.0452 0.6610 0.060 Uiso 1 1 calc R . . C7 C 0.7873(5) 0.0920(5) 0.5846(4) 0.0503(12) Uani 1 1 d . . . H7A H 0.8134 0.0293 0.5210 0.060 Uiso 1 1 calc R . . H7B H 0.7287 0.1355 0.5445 0.060 Uiso 1 1 calc R . . C8 C 0.9735(5) 0.2432(4) 0.6223(4) 0.0469(11) Uani 1 1 d . . . C9 C 1.0842(5) 0.3427(5) 0.7053(4) 0.0521(12) Uani 1 1 d . . . H9A H 1.0495 0.4175 0.7408 0.063 Uiso 1 1 calc R . . H9B H 1.1381 0.3627 0.6546 0.063 Uiso 1 1 calc R . . C10 C 1.1714(4) 0.3152(5) 0.8110(4) 0.0479(11) Uani 1 1 d . . . C11 C 0.8500(5) 0.2585(5) 1.1962(4) 0.0530(12) Uani 1 1 d . . . H11A H 0.8479 0.1829 1.2165 0.080 Uiso 1 1 calc R . . H11B H 0.7818 0.3009 1.2211 0.080 Uiso 1 1 calc R . . H11C H 0.9317 0.3122 1.2384 0.080 Uiso 1 1 calc R . . C12 C 0.7144(5) -0.0338(4) 0.8907(5) 0.0508(12) Uani 1 1 d . . . H12A H 0.7011 -0.1016 0.8142 0.076 Uiso 1 1 calc R . . H12B H 0.6675 -0.0592 0.9429 0.076 Uiso 1 1 calc R . . H12C H 0.8049 -0.0124 0.9309 0.076 Uiso 1 1 calc R . . C13 C 0.5208(4) 0.0483(5) 0.8082(5) 0.0574(13) Uani 1 1 d . . . H13A H 0.4917 0.1183 0.7880 0.086 Uiso 1 1 calc R . . H13B H 0.4772 0.0305 0.8662 0.086 Uiso 1 1 calc R . . H13C H 0.5022 -0.0239 0.7347 0.086 Uiso 1 1 calc R . . C14 C 0.9499(6) 0.2239(6) 0.4872(4) 0.0745(17) Uani 1 1 d . . . H14A H 1.0067 0.1708 0.4524 0.112 Uiso 1 1 calc R . . H14B H 0.9661 0.3035 0.4758 0.112 Uiso 1 1 calc R . . H14C H 0.8619 0.1851 0.4470 0.112 Uiso 1 1 calc R . . C15 C 1.2822(5) 0.4254(5) 0.8767(5) 0.0695(16) Uani 1 1 d . . . H15A H 1.2481 0.5003 0.9095 0.104 Uiso 1 1 calc R . . H15B H 1.3302 0.4367 0.8191 0.104 Uiso 1 1 calc R . . H15C H 1.3381 0.4087 0.9427 0.104 Uiso 1 1 calc R . . C16 C 1.2246(5) 0.1953(5) 0.7614(5) 0.0648(15) Uani 1 1 d . . . H16A H 1.2778 0.1782 0.8287 0.097 Uiso 1 1 calc R . . H16B H 1.2752 0.2054 0.7055 0.097 Uiso 1 1 calc R . . H16C H 1.1543 0.1267 0.7189 0.097 Uiso 1 1 calc R . . H1 H 1.071(4) 0.373(4) 0.926(4) 0.027(11) Uiso 1 1 d . . . H3 H 0.697(4) 0.174(4) 0.760(4) 0.050(15) Uiso 1 1 d . . . N1 N 1.0906(3) 0.3041(3) 0.8992(3) 0.0334(8) Uani 1 1 d . . . N2 N 0.9265(3) 0.2328(3) 1.0097(3) 0.0314(7) Uani 1 1 d . . . N3 N 0.7336(3) 0.1202(3) 0.7787(3) 0.0348(8) Uani 1 1 d . . . N4 N 0.9016(3) 0.1822(3) 0.6666(3) 0.0373(8) Uani 1 1 d . . . O1 O 0.5151(4) 0.8146(3) 0.4145(3) 0.0648(10) Uani 1 1 d . . . O2 O 0.6885(3) 0.6680(3) 0.4977(3) 0.0458(7) Uani 1 1 d . . . O3 O 0.5155(3) 0.7402(3) 0.6246(3) 0.0447(7) Uani 1 1 d . . . O4 O 0.5107(3) 0.6982(3) 0.8486(3) 0.0569(9) Uani 1 1 d . . . O5 O 0.3259(3) 0.5701(3) 0.6267(3) 0.0447(7) Uani 1 1 d . . . O6 O 0.5000 0.5000 0.5000 0.0292(8) Uani 1 2 d S . . O7 O 0.1147(3) 0.4572(3) 0.4152(3) 0.0602(9) Uani 1 1 d . . . O8 O 0.3132(3) 0.3870(3) 0.2986(2) 0.0434(7) Uani 1 1 d . . . O9 O 0.3273(3) 0.6299(3) 0.4277(3) 0.0461(7) Uani 1 1 d . . . O10 O 0.4964(3) 0.5551(3) 0.2967(3) 0.0452(7) Uani 1 1 d . . . Cl1 Cl 0.98871(13) 0.02202(13) 0.81470(12) 0.0631(3) Uani 1 1 d . . . Cl2 Cl 0.84068(11) 0.39245(11) 0.86083(10) 0.0469(3) Uani 1 1 d . . . Co1 Co 0.91453(5) 0.20738(5) 0.83829(4) 0.02873(13) Uani 1 1 d . . . Mo1 Mo 0.51182(4) 0.68103(4) 0.44896(4) 0.04223(12) Uani 1 1 d . . . Mo2 Mo 0.50303(4) 0.61636(4) 0.70081(3) 0.03873(11) Uani 1 1 d . . . Mo3 Mo 0.27627(3) 0.47471(4) 0.44735(3) 0.04033(12) Uani 1 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 C1 0.034(2) 0.053(3) 0.041(2) 0.022(2) 0.0044(19) 0.005(2) C2 0.040(2) 0.049(3) 0.031(2) 0.0182(19) 0.0042(18) 0.002(2) C3 0.045(2) 0.040(2) 0.034(2) 0.0158(18) 0.0174(19) 0.0112(19) C4 0.042(2) 0.056(3) 0.043(2) 0.019(2) 0.019(2) 0.010(2) C5 0.033(2) 0.047(3) 0.044(2) 0.019(2) 0.0123(19) 0.0017(19) C6 0.053(3) 0.047(3) 0.040(3) 0.008(2) 0.004(2) 0.004(2) C7 0.061(3) 0.058(3) 0.025(2) 0.007(2) 0.006(2) 0.014(2) C8 0.067(3) 0.051(3) 0.032(2) 0.019(2) 0.022(2) 0.014(2) C9 0.074(3) 0.051(3) 0.044(3) 0.022(2) 0.034(2) 0.009(2) C10 0.047(3) 0.058(3) 0.044(3) 0.019(2) 0.025(2) 0.003(2) C11 0.061(3) 0.069(3) 0.034(2) 0.019(2) 0.020(2) 0.011(3) C12 0.051(3) 0.044(3) 0.061(3) 0.026(2) 0.011(2) 0.004(2) C13 0.041(3) 0.065(3) 0.067(3) 0.028(3) 0.009(2) 0.003(2) C14 0.102(5) 0.093(4) 0.033(3) 0.028(3) 0.023(3) 0.005(4) C15 0.058(3) 0.083(4) 0.069(4) 0.027(3) 0.029(3) -0.008(3) C16 0.062(3) 0.074(4) 0.074(4) 0.025(3) 0.044(3) 0.026(3) N1 0.0353(19) 0.037(2) 0.0343(18) 0.0154(16) 0.0144(15) 0.0116(16) N2 0.0358(18) 0.0341(18) 0.0256(16) 0.0118(14) 0.0073(14) 0.0066(14) N3 0.0369(19) 0.0327(19) 0.0331(18) 0.0106(15) 0.0053(15) 0.0059(16) N4 0.047(2) 0.040(2) 0.0261(17) 0.0095(15) 0.0112(15) 0.0125(16) O1 0.089(3) 0.050(2) 0.067(2) 0.0327(18) 0.024(2) 0.0098(19) O2 0.0420(17) 0.0487(18) 0.0463(17) 0.0171(14) 0.0133(14) -0.0044(14) O3 0.0525(19) 0.0368(16) 0.0416(17) 0.0076(13) 0.0147(14) 0.0043(14) O4 0.057(2) 0.071(2) 0.0330(16) 0.0012(15) 0.0181(15) 0.0019(17) O5 0.0376(16) 0.060(2) 0.0360(16) 0.0117(14) 0.0167(13) 0.0079(14) O6 0.0293(19) 0.035(2) 0.0227(18) 0.0080(15) 0.0084(15) 0.0021(16) O7 0.0320(17) 0.085(3) 0.057(2) 0.0166(19) 0.0085(15) 0.0068(17) O8 0.0354(16) 0.0566(19) 0.0288(15) 0.0063(13) 0.0032(12) 0.0007(14) O9 0.0432(17) 0.0531(19) 0.0444(17) 0.0196(15) 0.0074(14) 0.0155(15) O10 0.0558(19) 0.0549(19) 0.0309(15) 0.0202(14) 0.0158(14) 0.0066(15) Cl1 0.0660(8) 0.0642(8) 0.0643(8) 0.0245(7) 0.0209(7) 0.0151(7) Cl2 0.0534(7) 0.0463(6) 0.0434(6) 0.0175(5) 0.0111(5) 0.0125(5) Co1 0.0340(3) 0.0313(3) 0.0236(3) 0.0111(2) 0.0089(2) 0.0080(2) Mo1 0.0518(2) 0.0392(2) 0.0419(2) 0.01957(17) 0.01612(18) 0.00714(18) Mo2 0.0398(2) 0.0465(2) 0.02544(19) 0.00503(16) 0.01156(15) 0.00210(17) Mo3 0.0288(2) 0.0542(3) 0.0345(2) 0.01091(17) 0.00781(15) 0.00390(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.474(5) . ? C1 C2 1.524(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.480(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.277(5) . ? C3 C4 1.493(6) . ? C3 C11 1.494(5) . ? C4 C5 1.524(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.509(5) . ? C5 C12 1.524(6) . ? C5 C13 1.532(6) . ? C6 N3 1.475(5) . ? C6 C7 1.512(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.469(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.277(5) . ? C8 C9 1.496(7) . ? C8 C14 1.498(6) . ? C9 C10 1.529(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.506(5) . ? C10 C16 1.522(7) . ? C10 C15 1.526(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 Co1 1.965(3) . ? N1 H1 0.82(4) . ? N2 Co1 1.921(3) . ? N3 Co1 1.973(3) . ? N3 H3 0.82(5) . ? N4 Co1 1.923(3) . ? O1 Mo1 1.686(3) . ? O2 Mo1 1.899(3) . ? O2 Mo3 1.963(3) 2_666 ? O3 Mo2 1.895(3) . ? O3 Mo1 1.956(3) . ? O4 Mo2 1.680(3) . ? O5 Mo2 1.871(3) . ? O5 Mo3 1.983(3) . ? O6 Mo1 2.3129(4) 2_666 ? O6 Mo1 2.3130(4) . ? O6 Mo2 2.3158(4) 2_666 ? O6 Mo2 2.3159(4) . ? O6 Mo3 2.3200(4) 2_666 ? O6 Mo3 2.3201(4) . ? O7 Mo3 1.676(3) . ? O8 Mo3 1.869(3) . ? O8 Mo2 1.974(3) 2_666 ? O9 Mo3 1.893(3) . ? O9 Mo1 1.952(3) . ? O10 Mo1 1.881(3) . ? O10 Mo2 1.959(3) 2_666 ? Cl1 Co1 2.2796(15) . ? Cl2 Co1 2.2762(12) . ? Mo2 O10 1.959(3) 2_666 ? Mo2 O8 1.974(3) 2_666 ? Mo3 O2 1.963(3) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 107.5(3) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 109.9(3) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 120.8(4) . . ? N2 C3 C11 123.2(4) . . ? C4 C3 C11 116.0(4) . . ? C3 C4 C5 117.2(4) . . ? C3 C4 H4A 108.0 . . ? C5 C4 H4A 108.0 . . ? C3 C4 H4B 108.0 . . ? C5 C4 H4B 108.0 . . ? H4A C4 H4B 107.3 . . ? N3 C5 C4 106.7(3) . . ? N3 C5 C12 111.7(4) . . ? C4 C5 C12 110.1(4) . . ? N3 C5 C13 109.2(4) . . ? C4 C5 C13 109.6(4) . . ? C12 C5 C13 109.5(4) . . ? N3 C6 C7 107.0(4) . . ? N3 C6 H6A 110.3 . . ? C7 C6 H6A 110.3 . . ? N3 C6 H6B 110.3 . . ? C7 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? N4 C7 C6 111.4(3) . . ? N4 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? N4 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C9 120.7(4) . . ? N4 C8 C14 122.9(5) . . ? C9 C8 C14 116.3(4) . . ? C8 C9 C10 118.2(4) . . ? C8 C9 H9A 107.8 . . ? C10 C9 H9A 107.8 . . ? C8 C9 H9B 107.8 . . ? C10 C9 H9B 107.8 . . ? H9A C9 H9B 107.1 . . ? N1 C10 C16 111.6(4) . . ? N1 C10 C15 109.2(4) . . ? C16 C10 C15 109.9(4) . . ? N1 C10 C9 107.0(4) . . ? C16 C10 C9 110.2(4) . . ? C15 C10 C9 108.8(4) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 C10 116.2(3) . . ? C1 N1 Co1 107.7(2) . . ? C10 N1 Co1 120.8(3) . . ? C1 N1 H1 107(3) . . ? C10 N1 H1 106(3) . . ? Co1 N1 H1 97(3) . . ? C3 N2 C2 119.5(3) . . ? C3 N2 Co1 126.6(3) . . ? C2 N2 Co1 113.5(2) . . ? C6 N3 C5 117.0(3) . . ? C6 N3 Co1 108.2(3) . . ? C5 N3 Co1 120.1(3) . . ? C6 N3 H3 100(3) . . ? C5 N3 H3 108(3) . . ? Co1 N3 H3 101(3) . . ? C8 N4 C7 119.9(4) . . ? C8 N4 Co1 126.6(3) . . ? C7 N4 Co1 113.2(3) . . ? Mo1 O2 Mo3 116.20(14) . 2_666 ? Mo2 O3 Mo1 116.82(14) . . ? Mo2 O5 Mo3 116.48(14) . . ? Mo1 O6 Mo1 180.0 2_666 . ? Mo1 O6 Mo2 90.234(15) 2_666 2_666 ? Mo1 O6 Mo2 89.767(14) . 2_666 ? Mo1 O6 Mo2 89.766(15) 2_666 . ? Mo1 O6 Mo2 90.232(14) . . ? Mo2 O6 Mo2 180.0 2_666 . ? Mo1 O6 Mo3 89.901(14) 2_666 2_666 ? Mo1 O6 Mo3 90.100(14) . 2_666 ? Mo2 O6 Mo3 89.981(13) 2_666 2_666 ? Mo2 O6 Mo3 90.021(13) . 2_666 ? Mo1 O6 Mo3 90.101(14) 2_666 . ? Mo1 O6 Mo3 89.898(14) . . ? Mo2 O6 Mo3 90.019(13) 2_666 . ? Mo2 O6 Mo3 89.979(13) . . ? Mo3 O6 Mo3 179.998(1) 2_666 . ? Mo3 O8 Mo2 117.06(13) . 2_666 ? Mo3 O9 Mo1 116.68(14) . . ? Mo1 O10 Mo2 116.58(14) . 2_666 ? N2 Co1 N4 179.70(14) . . ? N2 Co1 N1 83.93(13) . . ? N4 Co1 N1 96.29(14) . . ? N2 Co1 N3 95.89(14) . . ? N4 Co1 N3 83.88(15) . . ? N1 Co1 N3 176.42(15) . . ? N2 Co1 Cl2 89.66(10) . . ? N4 Co1 Cl2 90.14(11) . . ? N1 Co1 Cl2 87.81(11) . . ? N3 Co1 Cl2 88.62(11) . . ? N2 Co1 Cl1 90.64(10) . . ? N4 Co1 Cl1 89.56(11) . . ? N1 Co1 Cl1 92.14(11) . . ? N3 Co1 Cl1 91.43(11) . . ? Cl2 Co1 Cl1 179.68(5) . . ? O1 Mo1 O10 104.01(15) . . ? O1 Mo1 O2 104.39(16) . . ? O10 Mo1 O2 89.85(13) . . ? O1 Mo1 O9 101.93(16) . . ? O10 Mo1 O9 87.38(13) . . ? O2 Mo1 O9 153.42(13) . . ? O1 Mo1 O3 102.52(15) . . ? O10 Mo1 O3 153.27(12) . . ? O2 Mo1 O3 86.73(13) . . ? O9 Mo1 O3 84.01(12) . . ? O1 Mo1 O6 177.54(13) . . ? O10 Mo1 O6 77.44(9) . . ? O2 Mo1 O6 77.52(9) . . ? O9 Mo1 O6 76.07(9) . . ? O3 Mo1 O6 75.94(9) . . ? O4 Mo2 O5 104.17(14) . . ? O4 Mo2 O3 104.34(16) . . ? O5 Mo2 O3 90.71(13) . . ? O4 Mo2 O10 102.57(15) . 2_666 ? O5 Mo2 O10 87.95(14) . 2_666 ? O3 Mo2 O10 152.54(12) . 2_666 ? O4 Mo2 O8 102.42(14) . 2_666 ? O5 Mo2 O8 153.23(12) . 2_666 ? O3 Mo2 O8 85.60(13) . 2_666 ? O10 Mo2 O8 83.40(13) 2_666 2_666 ? O4 Mo2 O6 177.56(13) . . ? O5 Mo2 O6 77.78(9) . . ? O3 Mo2 O6 76.98(9) . . ? O10 Mo2 O6 75.93(8) 2_666 . ? O8 Mo2 O6 75.55(8) 2_666 . ? O7 Mo3 O8 104.71(14) . . ? O7 Mo3 O9 103.85(16) . . ? O8 Mo3 O9 90.95(13) . . ? O7 Mo3 O2 102.80(15) . 2_666 ? O8 Mo3 O2 87.81(13) . 2_666 ? O9 Mo3 O2 152.73(12) . 2_666 ? O7 Mo3 O5 102.26(14) . . ? O8 Mo3 O5 152.86(12) . . ? O9 Mo3 O5 85.53(13) . . ? O2 Mo3 O5 83.31(13) 2_666 . ? O7 Mo3 O6 177.70(11) . . ? O8 Mo3 O6 77.37(8) . . ? O9 Mo3 O6 76.99(9) . . ? O2 Mo3 O6 76.16(8) 2_666 . ? O5 Mo3 O6 75.62(8) . . ? 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 C15 H15B O10 0.96 2.53 3.463(6) 164.1 2_766 C14 H14B O7 0.96 2.61 3.460(7) 148.2 1_655 C13 H13C O3 0.96 2.63 3.491(6) 149.9 1_545 C12 H12A O3 0.96 2.69 3.498(6) 142.6 1_545 C11 H11B O5 0.96 2.50 3.391(5) 154.8 2_667 C11 H11C O7 0.96 2.55 3.467(6) 159.6 1_656 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.848 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.094 #END******************************************************** data_Ni-TDE-W6 _database_code_depnum_ccdc_archive 'CCDC 776419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C16 H30 N4 Ni, O19 W6, C2 H6 O S, C H2 Cl2 ; _chemical_formula_sum 'C19 H38 Cl2 N4 Ni O20 S W6' _chemical_formula_weight 1907.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.1285(13) _cell_length_b 16.4933(12) _cell_length_c 12.8503(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.5540(10) _cell_angle_gamma 90.00 _cell_volume 3817.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5848 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.02 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 18.761 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1533 _exptl_absorpt_correction_T_max 0.2118 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36003 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6669 _reflns_number_gt 6206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+29.8497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6669 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 0.027 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7671(5) 0.2820(5) 0.1869(7) 0.020(2) Uani 1 1 d . . . H1A H 0.7393 0.2329 0.1680 0.025 Uiso 1 1 calc R . . H1B H 0.8044 0.2699 0.2451 0.025 Uiso 1 1 calc R . . C2 C 0.8035(5) 0.3123(5) 0.0953(7) 0.0166(19) Uani 1 1 d . . . H2A H 0.8442 0.2770 0.0821 0.020 Uiso 1 1 calc R . . H2B H 0.7680 0.3142 0.0329 0.020 Uiso 1 1 calc R . . C3 C 0.8920(5) 0.4186(5) 0.0932(7) 0.0158(19) Uani 1 1 d . . . C4 C 0.9221(5) 0.5010(5) 0.1178(7) 0.018(2) Uani 1 1 d . . . H4A H 0.9153 0.5323 0.0535 0.022 Uiso 1 1 calc R . . H4B H 0.9752 0.4955 0.1368 0.022 Uiso 1 1 calc R . . C5 C 0.8916(5) 0.5521(5) 0.2038(7) 0.018(2) Uani 1 1 d . . . C6 C 0.7715(5) 0.6156(5) 0.2356(7) 0.020(2) Uani 1 1 d . . . H6A H 0.7767 0.6684 0.2039 0.024 Uiso 1 1 calc R . . H6B H 0.7944 0.6178 0.3075 0.024 Uiso 1 1 calc R . . C7 C 0.6914(5) 0.5943(5) 0.2328(8) 0.021(2) Uani 1 1 d . . . H7A H 0.6687 0.6261 0.2840 0.025 Uiso 1 1 calc R . . H7B H 0.6656 0.6056 0.1640 0.025 Uiso 1 1 calc R . . C8 C 0.6323(5) 0.4800(5) 0.3025(6) 0.0151(19) Uani 1 1 d . . . C9 C 0.6245(5) 0.3923(5) 0.3275(7) 0.018(2) Uani 1 1 d . . . H9A H 0.5835 0.3711 0.2803 0.021 Uiso 1 1 calc R . . H9B H 0.6101 0.3888 0.3978 0.021 Uiso 1 1 calc R . . C10 C 0.6901(5) 0.3358(6) 0.3224(7) 0.021(2) Uani 1 1 d . . . C11 C 0.9364(5) 0.3689(6) 0.0245(8) 0.027(2) Uani 1 1 d . . . H11A H 0.9629 0.3274 0.0657 0.041 Uiso 1 1 calc R . . H11B H 0.9711 0.4033 -0.0055 0.041 Uiso 1 1 calc R . . H11C H 0.9036 0.3443 -0.0304 0.041 Uiso 1 1 calc R . . C12 C 0.9114(5) 0.5144(6) 0.3120(7) 0.026(2) Uani 1 1 d . . . H12A H 0.8902 0.5462 0.3636 0.039 Uiso 1 1 calc R . . H12B H 0.9645 0.5130 0.3283 0.039 Uiso 1 1 calc R . . H12C H 0.8922 0.4602 0.3122 0.039 Uiso 1 1 calc R . . C13 C 0.9230(5) 0.6369(6) 0.2003(9) 0.028(2) Uani 1 1 d . . . H13A H 0.9063 0.6614 0.1340 0.042 Uiso 1 1 calc R . . H13B H 0.9763 0.6343 0.2090 0.042 Uiso 1 1 calc R . . H13C H 0.9065 0.6687 0.2557 0.042 Uiso 1 1 calc R . . C14 C 0.5705(5) 0.5331(6) 0.3327(8) 0.026(2) Uani 1 1 d . . . H14A H 0.5890 0.5668 0.3908 0.039 Uiso 1 1 calc R . . H14B H 0.5310 0.4997 0.3522 0.039 Uiso 1 1 calc R . . H14C H 0.5523 0.5666 0.2742 0.039 Uiso 1 1 calc R . . C15 C 0.6626(5) 0.2489(6) 0.3350(8) 0.026(2) Uani 1 1 d . . . H15A H 0.6283 0.2347 0.2752 0.039 Uiso 1 1 calc R . . H15B H 0.6382 0.2452 0.3973 0.039 Uiso 1 1 calc R . . H15C H 0.7041 0.2123 0.3402 0.039 Uiso 1 1 calc R . . C16 C 0.7523(5) 0.3550(6) 0.4102(7) 0.024(2) Uani 1 1 d . . . H16A H 0.7955 0.3236 0.4002 0.035 Uiso 1 1 calc R . . H16B H 0.7361 0.3416 0.4766 0.035 Uiso 1 1 calc R . . H16C H 0.7641 0.4116 0.4086 0.035 Uiso 1 1 calc R . . C17 C 0.0149(6) 0.3432(6) 0.4328(8) 0.029(2) Uani 1 1 d . . . H17A H 0.0383 0.3935 0.4153 0.035 Uiso 1 1 calc R . . H17B H 0.0535 0.3062 0.4616 0.035 Uiso 1 1 calc R . . C18 C 0.4992(5) 0.6171(6) 0.0496(8) 0.027(2) Uani 1 1 d . . . H18A H 0.4880 0.6477 0.1094 0.040 Uiso 1 1 calc R . . H18B H 0.5509 0.6028 0.0579 0.040 Uiso 1 1 calc R . . H18C H 0.4696 0.5687 0.0438 0.040 Uiso 1 1 calc R . . C19 C 0.5303(6) 0.7651(6) -0.0226(8) 0.034(3) Uani 1 1 d . . . H19A H 0.5315 0.8023 -0.0799 0.051 Uiso 1 1 calc R . . H19B H 0.5801 0.7497 0.0034 0.051 Uiso 1 1 calc R . . H19C H 0.5072 0.7907 0.0324 0.051 Uiso 1 1 calc R . . Cl1 Cl -0.04639(15) 0.36250(17) 0.5279(2) 0.0370(6) Uani 1 1 d . . . Cl2 Cl -0.03279(15) 0.30074(17) 0.3183(2) 0.0374(6) Uani 1 1 d . . . N1 N 0.7161(4) 0.3468(4) 0.2172(5) 0.0126(15) Uani 1 1 d . . . N2 N 0.8308(4) 0.3935(4) 0.1235(5) 0.0130(15) Uani 1 1 d . . . N3 N 0.8081(4) 0.5532(4) 0.1772(6) 0.0140(16) Uani 1 1 d . . . N4 N 0.6865(4) 0.5075(4) 0.2568(5) 0.0119(15) Uani 1 1 d . . . Ni1 Ni 0.76167(6) 0.44992(6) 0.19746(8) 0.0108(2) Uani 1 1 d . . . O1 O 0.8883(3) 0.7011(4) 0.9205(5) 0.0206(14) Uani 1 1 d . . . O2 O 0.7750(3) 0.5864(3) 0.9527(4) 0.0136(13) Uani 1 1 d . . . O3 O 0.7359(3) 0.7110(3) 0.8276(4) 0.0128(12) Uani 1 1 d . . . O4 O 0.6346(3) 0.6057(3) 0.8717(4) 0.0121(12) Uani 1 1 d . . . O5 O 0.8379(3) 0.6681(3) 0.7049(4) 0.0141(13) Uani 1 1 d . . . O6 O 0.7359(3) 0.5630(3) 0.7496(4) 0.0095(12) Uani 1 1 d . . . O7 O 0.5855(3) 0.7438(4) 0.7478(5) 0.0167(13) Uani 1 1 d . . . O8 O 0.6975(3) 0.6877(3) 0.6257(4) 0.0132(12) Uani 1 1 d . . . O9 O 0.5959(3) 0.5816(3) 0.6695(4) 0.0122(12) Uani 1 1 d . . . O10 O 0.8046(3) 0.6507(4) 0.4842(5) 0.0223(15) Uani 1 1 d . . . O11 O 0.6968(3) 0.5387(3) 0.5466(4) 0.0134(13) Uani 1 1 d . . . O12 O 0.5844(3) 0.4240(4) 0.5781(5) 0.0191(14) Uani 1 1 d . . . O13 O 0.8372(3) 0.5204(3) 0.6274(4) 0.0135(13) Uani 1 1 d . . . O14 O 0.6335(3) 0.4573(3) 0.7938(4) 0.0128(12) Uani 1 1 d . . . O15 O 0.7352(3) 0.4150(3) 0.6720(5) 0.0160(13) Uani 1 1 d . . . O16 O 0.8854(3) 0.3823(4) 0.7495(5) 0.0221(15) Uani 1 1 d . . . O17 O 0.7736(3) 0.4382(3) 0.8731(4) 0.0138(13) Uani 1 1 d . . . O18 O 0.8766(3) 0.5437(4) 0.8301(4) 0.0150(13) Uani 1 1 d . . . O19 O 0.6683(3) 0.4763(4) 1.0153(5) 0.0206(14) Uani 1 1 d . . . O20 O 0.3990(3) 0.7020(4) -0.0679(5) 0.0268(15) Uani 1 1 d . . . S1 S 0.47872(13) 0.67711(15) -0.06660(19) 0.0238(5) Uani 1 1 d . . . W1 W 0.774466(19) 0.61411(2) 0.59584(3) 0.01357(9) Uani 1 1 d . . . W2 W 0.648272(19) 0.48246(2) 0.65047(3) 0.01221(9) Uani 1 1 d . . . W3 W 0.648878(19) 0.66677(2) 0.74859(3) 0.01219(8) Uani 1 1 d . . . W4 W 0.696202(19) 0.51132(2) 0.90118(3) 0.01237(9) Uani 1 1 d . . . W5 W 0.823285(19) 0.64379(2) 0.84734(3) 0.01285(9) Uani 1 1 d . . . W6 W 0.822678(19) 0.45916(2) 0.74969(3) 0.01410(9) Uani 1 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 C1 0.029(5) 0.005(4) 0.029(5) -0.008(4) 0.009(4) 0.003(4) C2 0.015(5) 0.016(5) 0.020(5) -0.010(4) 0.005(4) 0.000(4) C3 0.016(5) 0.018(5) 0.014(4) 0.008(4) 0.003(4) 0.004(4) C4 0.011(5) 0.019(5) 0.027(5) 0.001(4) 0.007(4) 0.002(4) C5 0.012(5) 0.012(5) 0.030(5) 0.006(4) 0.001(4) -0.001(4) C6 0.028(5) 0.006(4) 0.026(5) 0.001(4) 0.000(4) -0.004(4) C7 0.020(5) 0.013(5) 0.030(5) -0.002(4) 0.003(4) 0.003(4) C8 0.016(5) 0.020(5) 0.009(4) 0.001(4) 0.001(3) 0.005(4) C9 0.016(5) 0.024(5) 0.013(4) -0.003(4) 0.004(4) 0.002(4) C10 0.026(5) 0.016(5) 0.021(5) -0.005(4) 0.009(4) -0.002(4) C11 0.025(6) 0.026(6) 0.032(6) 0.002(5) 0.008(5) 0.004(5) C12 0.021(5) 0.029(6) 0.026(5) 0.000(4) -0.011(4) 0.001(4) C13 0.014(5) 0.018(5) 0.050(7) 0.004(5) -0.003(5) -0.003(4) C14 0.018(5) 0.027(6) 0.035(6) 0.005(5) 0.014(4) 0.001(4) C15 0.030(6) 0.021(5) 0.029(5) 0.010(4) 0.019(4) 0.005(4) C16 0.016(5) 0.030(6) 0.023(5) 0.002(4) -0.005(4) 0.003(4) C17 0.027(6) 0.028(6) 0.029(6) 0.003(5) -0.006(4) 0.007(5) C18 0.018(5) 0.016(5) 0.045(6) 0.020(5) 0.000(4) 0.003(4) C19 0.040(7) 0.033(6) 0.027(6) 0.007(5) -0.006(5) -0.019(5) Cl1 0.0336(15) 0.0418(16) 0.0356(15) -0.0050(12) 0.0033(12) -0.0053(13) Cl2 0.0347(15) 0.0332(15) 0.0415(16) -0.0085(12) -0.0075(12) 0.0140(12) N1 0.012(4) 0.007(4) 0.020(4) -0.003(3) 0.009(3) -0.006(3) N2 0.009(4) 0.012(4) 0.018(4) -0.004(3) 0.001(3) 0.005(3) N3 0.011(4) 0.008(4) 0.023(4) -0.001(3) 0.002(3) -0.002(3) N4 0.012(4) 0.010(4) 0.013(4) 0.001(3) 0.001(3) 0.007(3) Ni1 0.0100(5) 0.0080(5) 0.0147(5) -0.0003(4) 0.0022(4) 0.0005(4) O1 0.015(3) 0.026(4) 0.020(3) -0.001(3) -0.004(3) -0.007(3) O2 0.013(3) 0.013(3) 0.014(3) -0.001(2) 0.001(2) -0.004(2) O3 0.012(3) 0.010(3) 0.016(3) -0.001(2) 0.001(2) 0.000(2) O4 0.012(3) 0.011(3) 0.013(3) -0.004(2) 0.000(2) 0.000(2) O5 0.010(3) 0.015(3) 0.018(3) 0.001(3) 0.001(2) 0.000(2) O6 0.007(3) 0.010(3) 0.012(3) -0.001(2) 0.002(2) 0.002(2) O7 0.015(3) 0.012(3) 0.022(3) -0.003(3) 0.001(3) 0.001(3) O8 0.016(3) 0.011(3) 0.012(3) 0.003(2) 0.002(2) -0.001(2) O9 0.008(3) 0.012(3) 0.015(3) -0.005(2) -0.004(2) -0.001(2) O10 0.020(4) 0.027(4) 0.020(3) -0.002(3) 0.004(3) -0.003(3) O11 0.014(3) 0.014(3) 0.012(3) -0.004(2) -0.002(2) -0.006(2) O12 0.015(3) 0.019(3) 0.022(3) -0.011(3) -0.002(3) -0.005(3) O13 0.016(3) 0.009(3) 0.016(3) -0.002(2) 0.003(2) 0.001(2) O14 0.013(3) 0.010(3) 0.016(3) 0.003(2) 0.003(2) -0.001(2) O15 0.017(3) 0.007(3) 0.025(3) -0.006(3) 0.004(3) 0.003(2) O16 0.014(3) 0.017(4) 0.035(4) 0.002(3) 0.002(3) 0.006(3) O17 0.012(3) 0.010(3) 0.019(3) 0.006(2) 0.001(2) 0.003(2) O18 0.009(3) 0.017(3) 0.018(3) -0.003(3) -0.004(2) -0.001(3) O19 0.018(3) 0.021(4) 0.023(3) 0.001(3) 0.002(3) -0.001(3) O20 0.022(4) 0.032(4) 0.026(4) -0.006(3) -0.002(3) -0.001(3) S1 0.0198(13) 0.0273(14) 0.0241(13) -0.0028(10) 0.0019(10) -0.0006(10) W1 0.01271(18) 0.01543(19) 0.01284(18) 0.00147(14) 0.00268(14) -0.00186(14) W2 0.01071(18) 0.01162(18) 0.01408(18) -0.00257(14) 0.00054(13) -0.00160(14) W3 0.01148(18) 0.00984(18) 0.01503(18) -0.00010(14) 0.00053(14) 0.00106(14) W4 0.01272(18) 0.01247(18) 0.01182(17) 0.00164(14) 0.00099(13) -0.00148(14) W5 0.01070(18) 0.01215(19) 0.01517(18) -0.00050(14) -0.00086(14) -0.00273(14) W6 0.01101(18) 0.01171(19) 0.01952(19) -0.00005(14) 0.00147(14) 0.00180(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.494(10) . ? C1 C2 1.498(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.460(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.285(11) . ? C3 C4 1.485(12) . ? C3 C11 1.503(12) . ? C4 C5 1.542(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.512(11) . ? C5 C13 1.513(12) . ? C5 C12 1.529(12) . ? C6 N3 1.476(11) . ? C6 C7 1.490(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.470(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.284(11) . ? C8 C9 1.492(12) . ? C8 C14 1.507(12) . ? C9 C10 1.518(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.492(11) . ? C10 C15 1.532(13) . ? C10 C16 1.533(13) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 Cl2 1.764(10) . ? C17 Cl1 1.771(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 S1 1.795(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 S1 1.784(10) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? N1 Ni1 1.920(7) . ? N2 Ni1 1.900(7) . ? N3 Ni1 1.930(7) . ? N4 Ni1 1.891(7) . ? O1 W5 1.707(6) . ? O2 W5 1.941(5) . ? O2 W4 1.948(5) . ? O3 W3 1.920(5) . ? O3 W5 1.926(5) . ? O4 W3 1.918(5) . ? O4 W4 1.927(6) . ? O5 W5 1.921(6) . ? O5 W1 1.927(6) . ? O6 W4 2.314(5) . ? O6 W6 2.326(5) . ? O6 W5 2.326(5) . ? O6 W3 2.326(5) . ? O6 W1 2.329(5) . ? O6 W2 2.334(5) . ? O7 W3 1.711(6) . ? O8 W1 1.920(6) . ? O8 W3 1.925(5) . ? O9 W2 1.921(6) . ? O9 W3 1.925(5) . ? O10 W1 1.702(6) . ? O11 W2 1.919(5) . ? O11 W1 1.931(5) . ? O12 W2 1.699(6) . ? O13 W6 1.912(6) . ? O13 W1 1.934(6) . ? O14 W4 1.906(6) . ? O14 W2 1.936(5) . ? O15 W6 1.919(6) . ? O15 W2 1.923(6) . ? O16 W6 1.702(6) . ? O17 W4 1.916(5) . ? O17 W6 1.936(5) . ? O18 W6 1.933(6) . ? O18 W5 1.939(6) . ? O19 W4 1.706(6) . ? O20 S1 1.501(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 107.9(7) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 106.2(7) . . ? N2 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? N2 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? N2 C3 C4 122.6(8) . . ? N2 C3 C11 122.8(8) . . ? C4 C3 C11 114.5(7) . . ? C3 C4 C5 120.0(7) . . ? C3 C4 H4A 107.3 . . ? C5 C4 H4A 107.3 . . ? C3 C4 H4B 107.3 . . ? C5 C4 H4B 107.3 . . ? H4A C4 H4B 106.9 . . ? N3 C5 C13 110.7(7) . . ? N3 C5 C12 109.6(7) . . ? C13 C5 C12 110.6(8) . . ? N3 C5 C4 106.0(7) . . ? C13 C5 C4 108.5(7) . . ? C12 C5 C4 111.3(7) . . ? N3 C6 C7 108.5(7) . . ? N3 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? N3 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N4 C7 C6 107.9(7) . . ? N4 C7 H7A 110.1 . . ? C6 C7 H7A 110.1 . . ? N4 C7 H7B 110.1 . . ? C6 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? N4 C8 C9 122.5(8) . . ? N4 C8 C14 122.9(8) . . ? C9 C8 C14 114.6(7) . . ? C8 C9 C10 119.5(7) . . ? C8 C9 H9A 107.5 . . ? C10 C9 H9A 107.5 . . ? C8 C9 H9B 107.5 . . ? C10 C9 H9B 107.5 . . ? H9A C9 H9B 107.0 . . ? N1 C10 C9 107.1(7) . . ? N1 C10 C15 110.4(7) . . ? C9 C10 C15 107.7(7) . . ? N1 C10 C16 111.1(7) . . ? C9 C10 C16 110.8(7) . . ? C15 C10 C16 109.7(8) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl2 C17 Cl1 111.2(6) . . ? Cl2 C17 H17A 109.4 . . ? Cl1 C17 H17A 109.4 . . ? Cl2 C17 H17B 109.4 . . ? Cl1 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? S1 C18 H18A 109.5 . . ? S1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? S1 C19 H19A 109.5 . . ? S1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? S1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C10 N1 C1 114.7(7) . . ? C10 N1 Ni1 114.4(5) . . ? C1 N1 Ni1 108.1(5) . . ? C3 N2 C2 120.0(7) . . ? C3 N2 Ni1 129.5(6) . . ? C2 N2 Ni1 110.4(5) . . ? C6 N3 C5 112.9(7) . . ? C6 N3 Ni1 108.6(5) . . ? C5 N3 Ni1 113.6(5) . . ? C8 N4 C7 120.5(7) . . ? C8 N4 Ni1 129.2(6) . . ? C7 N4 Ni1 109.9(5) . . ? N4 Ni1 N2 173.8(3) . . ? N4 Ni1 N1 92.9(3) . . ? N2 Ni1 N1 87.2(3) . . ? N4 Ni1 N3 87.5(3) . . ? N2 Ni1 N3 92.4(3) . . ? N1 Ni1 N3 179.6(3) . . ? W5 O2 W4 116.4(3) . . ? W3 O3 W5 117.7(3) . . ? W3 O4 W4 117.2(3) . . ? W5 O5 W1 117.5(3) . . ? W4 O6 W6 90.21(19) . . ? W4 O6 W5 90.84(19) . . ? W6 O6 W5 90.13(18) . . ? W4 O6 W3 90.02(18) . . ? W6 O6 W3 179.7(3) . . ? W5 O6 W3 90.07(19) . . ? W4 O6 W1 179.2(3) . . ? W6 O6 W1 89.88(18) . . ? W5 O6 W1 89.91(18) . . ? W3 O6 W1 89.88(19) . . ? W4 O6 W2 89.57(18) . . ? W6 O6 W2 89.96(19) . . ? W5 O6 W2 179.6(3) . . ? W3 O6 W2 89.84(18) . . ? W1 O6 W2 89.68(18) . . ? W1 O8 W3 117.5(3) . . ? W2 O9 W3 117.7(3) . . ? W2 O11 W1 117.3(3) . . ? W6 O13 W1 117.5(3) . . ? W4 O14 W2 116.9(3) . . ? W6 O15 W2 118.1(3) . . ? W4 O17 W6 117.2(3) . . ? W6 O18 W5 116.6(3) . . ? O20 S1 C19 104.5(5) . . ? O20 S1 C18 105.5(4) . . ? C19 S1 C18 97.7(5) . . ? O10 W1 O8 104.8(3) . . ? O10 W1 O5 103.1(3) . . ? O8 W1 O5 87.1(2) . . ? O10 W1 O11 104.1(3) . . ? O8 W1 O11 87.3(2) . . ? O5 W1 O11 152.7(2) . . ? O10 W1 O13 102.8(3) . . ? O8 W1 O13 152.4(2) . . ? O5 W1 O13 85.9(2) . . ? O11 W1 O13 86.8(2) . . ? O10 W1 O6 178.8(3) . . ? O8 W1 O6 76.3(2) . . ? O5 W1 O6 76.2(2) . . ? O11 W1 O6 76.5(2) . . ? O13 W1 O6 76.1(2) . . ? O12 W2 O11 103.4(3) . . ? O12 W2 O9 103.7(3) . . ? O11 W2 O9 87.1(2) . . ? O12 W2 O15 104.3(3) . . ? O11 W2 O15 86.9(2) . . ? O9 W2 O15 152.0(2) . . ? O12 W2 O14 103.8(3) . . ? O11 W2 O14 152.8(2) . . ? O9 W2 O14 86.4(2) . . ? O15 W2 O14 86.5(2) . . ? O12 W2 O6 179.9(3) . . ? O11 W2 O6 76.6(2) . . ? O9 W2 O6 76.2(2) . . ? O15 W2 O6 75.9(2) . . ? O14 W2 O6 76.2(2) . . ? O7 W3 O4 103.9(3) . . ? O7 W3 O3 103.4(3) . . ? O4 W3 O3 86.7(2) . . ? O7 W3 O9 104.1(3) . . ? O4 W3 O9 86.9(2) . . ? O3 W3 O9 152.5(2) . . ? O7 W3 O8 103.4(3) . . ? O4 W3 O8 152.6(2) . . ? O3 W3 O8 86.6(2) . . ? O9 W3 O8 86.9(2) . . ? O7 W3 O6 179.5(2) . . ? O4 W3 O6 76.3(2) . . ? O3 W3 O6 76.2(2) . . ? O9 W3 O6 76.3(2) . . ? O8 W3 O6 76.3(2) . . ? O19 W4 O14 104.6(3) . . ? O19 W4 O17 104.1(3) . . ? O14 W4 O17 87.6(2) . . ? O19 W4 O4 102.7(3) . . ? O14 W4 O4 87.2(2) . . ? O17 W4 O4 153.1(2) . . ? O19 W4 O2 101.6(3) . . ? O14 W4 O2 153.8(2) . . ? O17 W4 O2 86.6(2) . . ? O4 W4 O2 86.5(2) . . ? O19 W4 O6 177.9(3) . . ? O14 W4 O6 77.3(2) . . ? O17 W4 O6 76.6(2) . . ? O4 W4 O6 76.5(2) . . ? O2 W4 O6 76.5(2) . . ? O1 W5 O5 104.3(3) . . ? O1 W5 O3 105.0(3) . . ? O5 W5 O3 87.4(2) . . ? O1 W5 O18 102.3(3) . . ? O5 W5 O18 86.8(2) . . ? O3 W5 O18 152.7(2) . . ? O1 W5 O2 103.0(3) . . ? O5 W5 O2 152.7(2) . . ? O3 W5 O2 86.7(2) . . ? O18 W5 O2 86.3(2) . . ? O1 W5 O6 178.7(3) . . ? O5 W5 O6 76.4(2) . . ? O3 W5 O6 76.1(2) . . ? O18 W5 O6 76.6(2) . . ? O2 W5 O6 76.3(2) . . ? O16 W6 O13 103.7(3) . . ? O16 W6 O15 103.2(3) . . ? O13 W6 O15 87.5(2) . . ? O16 W6 O18 103.9(3) . . ? O13 W6 O18 87.1(2) . . ? O15 W6 O18 152.8(2) . . ? O16 W6 O17 103.7(3) . . ? O13 W6 O17 152.5(2) . . ? O15 W6 O17 85.9(2) . . ? O18 W6 O17 86.7(2) . . ? O16 W6 O6 179.3(3) . . ? O13 W6 O6 76.6(2) . . ? O15 W6 O6 76.1(2) . . ? O18 W6 O6 76.7(2) . . ? O17 W6 O6 76.0(2) . . ? 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 C14 H14B O9 0.96 2.65 3.558(11) 158.2 3_666 C13 H13B O16 0.96 2.52 3.475(11) 173.3 3_766 C9 H9B O12 0.97 2.48 3.422(10) 162.5 . C6 H6B O10 0.97 2.32 3.235(11) 156.7 . C1 H1A O15 0.97 2.44 3.302(10) 147.8 4_565 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.314 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.212 #END******************************************************* data_Zn-TDE-Cl-W6 _database_code_depnum_ccdc_archive 'CCDC 776420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H32 Cl N4 Zn), O19 W6' _chemical_formula_sum 'C32 H64 Cl2 N8 O19 W6 Zn2' _chemical_formula_weight 2169.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.799(3) _cell_length_b 11.888(2) _cell_length_c 18.130(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.842(3) _cell_angle_gamma 90.00 _cell_volume 2960.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6024 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.48 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 12.555 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2109 _exptl_absorpt_correction_T_max 0.3666 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27908 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5219 _reflns_number_gt 4529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^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 5219 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8883(5) 0.6575(6) 0.6788(4) 0.0524(19) Uani 1 1 d . . . H1A H 0.9466 0.6869 0.6733 0.063 Uiso 1 1 calc R . . H1B H 0.9077 0.6101 0.7257 0.063 Uiso 1 1 calc R . . C2 C 0.8253(6) 0.7544(6) 0.6875(4) 0.058(2) Uani 1 1 d . . . H2A H 0.8604 0.7969 0.7352 0.070 Uiso 1 1 calc R . . H2B H 0.8097 0.8046 0.6423 0.070 Uiso 1 1 calc R . . C3 C 0.6877(6) 0.7634(6) 0.7259(4) 0.0555(19) Uani 1 1 d . . . C4 C 0.6017(6) 0.7135(8) 0.7368(5) 0.078(3) Uani 1 1 d . . . H4A H 0.5704 0.7731 0.7551 0.094 Uiso 1 1 calc R . . H4B H 0.6258 0.6593 0.7797 0.094 Uiso 1 1 calc R . . C5 C 0.5217(6) 0.6542(7) 0.6668(5) 0.068(2) Uani 1 1 d . . . C6 C 0.5867(6) 0.4559(7) 0.6979(5) 0.062(2) Uani 1 1 d . . . H6A H 0.5275 0.4273 0.7023 0.074 Uiso 1 1 calc R . . H6B H 0.6305 0.4789 0.7504 0.074 Uiso 1 1 calc R . . C7 C 0.6336(6) 0.3650(6) 0.6669(5) 0.059(2) Uani 1 1 d . . . H7A H 0.6538 0.3038 0.7049 0.071 Uiso 1 1 calc R . . H7B H 0.5869 0.3356 0.6175 0.071 Uiso 1 1 calc R . . C8 C 0.7952(6) 0.3512(6) 0.6668(4) 0.0486(18) Uani 1 1 d . . . C9 C 0.8838(5) 0.3984(6) 0.6570(4) 0.056(2) Uani 1 1 d . . . H9A H 0.9195 0.3349 0.6478 0.067 Uiso 1 1 calc R . . H9B H 0.9240 0.4299 0.7081 0.067 Uiso 1 1 calc R . . C10 C 0.8793(5) 0.4865(6) 0.5947(4) 0.0502(18) Uani 1 1 d . . . C11 C 0.7132(6) 0.8812(7) 0.7577(5) 0.077(3) Uani 1 1 d . . . H11A H 0.7731 0.9037 0.7530 0.115 Uiso 1 1 calc R . . H11B H 0.7205 0.8831 0.8126 0.115 Uiso 1 1 calc R . . H11C H 0.6621 0.9318 0.7277 0.115 Uiso 1 1 calc R . . C12 C 0.4843(6) 0.7348(8) 0.5964(6) 0.086(3) Uani 1 1 d . . . H12A H 0.5378 0.7593 0.5825 0.129 Uiso 1 1 calc R . . H12B H 0.4546 0.7987 0.6106 0.129 Uiso 1 1 calc R . . H12C H 0.4372 0.6969 0.5519 0.129 Uiso 1 1 calc R . . C13 C 0.4366(7) 0.6213(8) 0.6932(6) 0.095(3) Uani 1 1 d . . . H13A H 0.3935 0.5707 0.6549 0.143 Uiso 1 1 calc R . . H13B H 0.4016 0.6878 0.6967 0.143 Uiso 1 1 calc R . . H13C H 0.4623 0.5852 0.7441 0.143 Uiso 1 1 calc R . . C14 C 0.8053(7) 0.2320(7) 0.6957(6) 0.087(3) Uani 1 1 d . . . H14A H 0.7756 0.2242 0.7343 0.130 Uiso 1 1 calc R . . H14B H 0.8731 0.2129 0.7196 0.130 Uiso 1 1 calc R . . H14C H 0.7738 0.1826 0.6517 0.130 Uiso 1 1 calc R . . C15 C 0.9843(5) 0.5117(7) 0.6004(5) 0.070(2) Uani 1 1 d . . . H15A H 0.9839 0.5765 0.5688 0.104 Uiso 1 1 calc R . . H15B H 1.0091 0.4481 0.5813 0.104 Uiso 1 1 calc R . . H15C H 1.0249 0.5261 0.6548 0.104 Uiso 1 1 calc R . . C16 C 0.8175(6) 0.4426(7) 0.5111(4) 0.067(2) Uani 1 1 d . . . H16A H 0.7513 0.4329 0.5069 0.100 Uiso 1 1 calc R . . H16B H 0.8430 0.3717 0.5024 0.100 Uiso 1 1 calc R . . H16C H 0.8196 0.4957 0.4719 0.100 Uiso 1 1 calc R . . Cl1 Cl 0.61148(14) 0.61706(18) 0.48023(11) 0.0637(5) Uani 1 1 d . . . H1 H 0.829(4) 0.633(5) 0.579(3) 0.021(19) Uiso 1 1 d . . . H3 H 0.520(3) 0.527(4) 0.603(3) 0.005(13) Uiso 1 1 d . . . N1 N 0.8322(5) 0.5918(6) 0.6085(4) 0.0500(17) Uani 1 1 d . . . N2 N 0.7350(4) 0.7083(5) 0.6919(3) 0.0513(15) Uani 1 1 d . . . N3 N 0.5635(4) 0.5540(5) 0.6433(4) 0.0484(15) Uani 1 1 d . . . N4 N 0.7195(4) 0.4100(5) 0.6530(3) 0.0497(15) Uani 1 1 d . . . O1 O 0.9095(4) 0.4961(4) 0.1830(3) 0.0575(13) Uani 1 1 d . . . O2 O 0.8462(3) 0.4162(4) 0.0220(3) 0.0500(12) Uani 1 1 d . . . O3 O 0.7606(4) 0.3268(5) -0.1344(3) 0.0738(17) Uani 1 1 d . . . O4 O 0.9329(3) 0.4221(4) -0.1470(3) 0.0499(12) Uani 1 1 d . . . O5 O 0.9567(3) 0.2845(4) -0.0267(3) 0.0508(12) Uani 1 1 d . . . O6 O 1.1107(3) 0.3675(4) -0.0478(3) 0.0517(12) Uani 1 1 d . . . O7 O 1.1438(4) 0.2093(5) 0.0760(3) 0.0780(17) Uani 1 1 d . . . O8 O 1.1773(3) 0.4451(4) 0.0981(3) 0.0549(13) Uani 1 1 d . . . O9 O 1.0237(3) 0.3621(4) 0.1209(3) 0.0496(12) Uani 1 1 d . . . O10 O 1.0000 0.5000 0.0000 0.0398(15) Uani 1 2 d S . . W1 W 0.94657(2) 0.49714(2) 0.104767(16) 0.04507(10) Uani 1 1 d . . . W2 W 0.86214(2) 0.39910(3) -0.077723(17) 0.04856(10) Uani 1 1 d . . . W3 W 1.08315(2) 0.33222(2) 0.044843(17) 0.04831(10) Uani 1 1 d . . . Zn1 Zn 0.68964(6) 0.57387(7) 0.61266(5) 0.0456(2) Uani 1 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 C1 0.048(4) 0.055(5) 0.049(4) -0.002(4) 0.013(4) 0.005(4) C2 0.068(5) 0.054(5) 0.052(5) -0.003(4) 0.022(4) -0.006(4) C3 0.059(5) 0.050(5) 0.056(5) 0.000(4) 0.019(4) 0.014(4) C4 0.091(7) 0.078(6) 0.090(7) -0.018(5) 0.061(6) 0.001(5) C5 0.063(5) 0.065(6) 0.095(7) 0.005(5) 0.050(5) 0.018(5) C6 0.054(5) 0.067(5) 0.072(5) 0.022(4) 0.032(4) 0.001(4) C7 0.064(5) 0.047(5) 0.067(5) 0.022(4) 0.025(4) 0.002(4) C8 0.063(5) 0.044(4) 0.037(4) 0.002(3) 0.017(4) 0.012(4) C9 0.056(5) 0.060(5) 0.047(4) 0.001(4) 0.015(4) 0.022(4) C10 0.052(4) 0.056(5) 0.047(4) -0.001(4) 0.024(4) 0.009(4) C11 0.077(6) 0.064(6) 0.089(6) -0.016(5) 0.030(5) 0.026(5) C12 0.073(6) 0.075(6) 0.118(8) 0.018(6) 0.045(6) 0.032(5) C13 0.083(7) 0.092(7) 0.144(10) -0.001(7) 0.080(7) 0.012(6) C14 0.096(7) 0.050(5) 0.121(8) 0.012(5) 0.048(6) 0.030(5) C15 0.054(5) 0.099(7) 0.062(5) 0.011(5) 0.029(4) 0.007(5) C16 0.079(6) 0.078(6) 0.046(5) -0.004(4) 0.025(4) 0.016(5) Cl1 0.0538(11) 0.0761(14) 0.0546(12) 0.0146(10) 0.0126(9) 0.0078(10) N1 0.055(4) 0.055(4) 0.042(4) 0.013(3) 0.020(3) 0.010(3) N2 0.053(4) 0.047(4) 0.056(4) -0.002(3) 0.022(3) 0.001(3) N3 0.047(4) 0.056(4) 0.046(4) 0.006(3) 0.022(3) -0.001(3) N4 0.052(4) 0.045(4) 0.049(4) 0.004(3) 0.014(3) 0.013(3) O1 0.073(3) 0.059(3) 0.047(3) 0.000(2) 0.031(3) -0.004(3) O2 0.044(3) 0.051(3) 0.052(3) 0.002(2) 0.014(2) -0.008(2) O3 0.061(4) 0.085(4) 0.062(3) -0.015(3) 0.008(3) -0.026(3) O4 0.055(3) 0.052(3) 0.038(3) -0.005(2) 0.013(2) -0.010(2) O5 0.062(3) 0.033(2) 0.058(3) -0.001(2) 0.023(2) -0.006(2) O6 0.060(3) 0.049(3) 0.047(3) 0.004(2) 0.021(2) 0.007(3) O7 0.091(4) 0.066(4) 0.081(4) 0.019(3) 0.037(3) 0.020(3) O8 0.049(3) 0.058(3) 0.049(3) 0.006(2) 0.008(2) -0.003(3) O9 0.055(3) 0.046(3) 0.044(3) 0.012(2) 0.015(2) 0.001(2) O10 0.046(4) 0.024(3) 0.042(4) 0.003(3) 0.008(3) 0.000(3) W1 0.05094(19) 0.04571(18) 0.03979(17) 0.00231(13) 0.01828(14) -0.00314(14) W2 0.04639(18) 0.0517(2) 0.04273(18) -0.00219(14) 0.01094(14) -0.01246(14) W3 0.0545(2) 0.04110(18) 0.04890(19) 0.00936(13) 0.01874(15) 0.00630(14) Zn1 0.0445(5) 0.0450(5) 0.0495(5) 0.0052(4) 0.0201(4) 0.0053(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.462(9) . ? C1 C2 1.526(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.474(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.273(8) . ? C3 C4 1.481(11) . ? C3 C11 1.507(10) . ? C4 C5 1.546(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.476(9) . ? C5 C12 1.525(11) . ? C5 C13 1.553(10) . ? C6 N3 1.485(9) . ? C6 C7 1.502(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.483(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.264(8) . ? C8 C9 1.497(10) . ? C8 C14 1.498(10) . ? C9 C10 1.524(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.498(9) . ? C10 C16 1.541(10) . ? C10 C15 1.547(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Cl1 Zn1 2.302(2) . ? N1 Zn1 2.150(6) . ? N1 H1 0.71(5) . ? N2 Zn1 2.086(6) . ? N3 Zn1 2.151(6) . ? N3 H3 0.83(5) . ? N4 Zn1 2.070(6) . ? O1 W1 1.701(5) . ? O2 W2 1.919(5) . ? O2 W1 1.929(4) . ? O3 W2 1.704(5) . ? O4 W1 1.917(4) 3_765 ? O4 W2 1.930(4) . ? O5 W3 1.923(5) . ? O5 W2 1.926(5) . ? O6 W3 1.917(4) . ? O6 W1 1.929(5) 3_765 ? O7 W3 1.698(5) . ? O8 W3 1.917(5) . ? O8 W2 1.935(5) 3_765 ? O9 W3 1.924(4) . ? O9 W1 1.929(5) . ? O10 W1 2.3135(4) . ? O10 W1 2.3135(4) 3_765 ? O10 W3 2.3257(4) 3_765 ? O10 W3 2.3257(4) . ? O10 W2 2.3339(4) . ? O10 W2 2.3340(4) 3_765 ? W1 O4 1.917(4) 3_765 ? W1 O6 1.929(5) 3_765 ? W2 O8 1.935(5) 3_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108.8(6) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 109.1(6) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N2 C3 C4 120.8(7) . . ? N2 C3 C11 123.9(7) . . ? C4 C3 C11 115.3(7) . . ? C3 C4 C5 120.5(7) . . ? C3 C4 H4A 107.2 . . ? C5 C4 H4A 107.2 . . ? C3 C4 H4B 107.2 . . ? C5 C4 H4B 107.2 . . ? H4A C4 H4B 106.8 . . ? N3 C5 C12 109.0(7) . . ? N3 C5 C4 109.2(7) . . ? C12 C5 C4 109.2(8) . . ? N3 C5 C13 111.1(7) . . ? C12 C5 C13 109.4(7) . . ? C4 C5 C13 108.9(7) . . ? N3 C6 C7 109.9(6) . . ? N3 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? N3 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N4 C7 C6 110.4(6) . . ? N4 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? N4 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N4 C8 C9 121.4(7) . . ? N4 C8 C14 123.9(7) . . ? C9 C8 C14 114.7(7) . . ? C8 C9 C10 123.2(6) . . ? C8 C9 H9A 106.5 . . ? C10 C9 H9A 106.5 . . ? C8 C9 H9B 106.5 . . ? C10 C9 H9B 106.5 . . ? H9A C9 H9B 106.5 . . ? N1 C10 C9 110.2(6) . . ? N1 C10 C16 107.7(6) . . ? C9 C10 C16 110.0(6) . . ? N1 C10 C15 110.2(6) . . ? C9 C10 C15 108.5(6) . . ? C16 C10 C15 110.3(6) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 C10 116.3(6) . . ? C1 N1 Zn1 105.6(4) . . ? C10 N1 Zn1 116.5(5) . . ? C1 N1 H1 99(5) . . ? C10 N1 H1 111(5) . . ? Zn1 N1 H1 107(5) . . ? C3 N2 C2 120.6(6) . . ? C3 N2 Zn1 129.4(5) . . ? C2 N2 Zn1 108.2(4) . . ? C5 N3 C6 117.4(6) . . ? C5 N3 Zn1 118.9(5) . . ? C6 N3 Zn1 104.5(4) . . ? C5 N3 H3 107(3) . . ? C6 N3 H3 102(3) . . ? Zn1 N3 H3 106(3) . . ? C8 N4 C7 121.3(6) . . ? C8 N4 Zn1 130.3(5) . . ? C7 N4 Zn1 108.4(4) . . ? W2 O2 W1 117.2(2) . . ? W1 O4 W2 117.4(2) 3_765 . ? W3 O5 W2 117.8(2) . . ? W3 O6 W1 117.2(2) . 3_765 ? W3 O8 W2 117.6(2) . 3_765 ? W3 O9 W1 116.6(2) . . ? W1 O10 W1 180.0 . 3_765 ? W1 O10 W3 90.094(12) . 3_765 ? W1 O10 W3 89.906(12) 3_765 3_765 ? W1 O10 W3 89.909(12) . . ? W1 O10 W3 90.091(12) 3_765 . ? W3 O10 W3 180.0 3_765 . ? W1 O10 W2 89.951(15) . . ? W1 O10 W2 90.050(15) 3_765 . ? W3 O10 W2 89.982(15) 3_765 . ? W3 O10 W2 90.018(16) . . ? W1 O10 W2 90.051(15) . 3_765 ? W1 O10 W2 89.948(15) 3_765 3_765 ? W3 O10 W2 90.016(15) 3_765 3_765 ? W3 O10 W2 89.983(15) . 3_765 ? W2 O10 W2 180.0 . 3_765 ? O1 W1 O4 102.2(2) . 3_765 ? O1 W1 O9 103.0(2) . . ? O4 W1 O9 86.9(2) 3_765 . ? O1 W1 O6 103.8(2) . 3_765 ? O4 W1 O6 87.4(2) 3_765 3_765 ? O9 W1 O6 153.25(19) . 3_765 ? O1 W1 O2 104.6(2) . . ? O4 W1 O2 153.23(19) 3_765 . ? O9 W1 O2 86.77(19) . . ? O6 W1 O2 86.7(2) 3_765 . ? O1 W1 O10 178.83(17) . . ? O4 W1 O10 76.63(13) 3_765 . ? O9 W1 O10 76.85(13) . . ? O6 W1 O10 76.40(13) 3_765 . ? O2 W1 O10 76.60(13) . . ? O3 W2 O2 103.4(2) . . ? O3 W2 O5 104.6(2) . . ? O2 W2 O5 86.82(19) . . ? O3 W2 O4 104.4(2) . . ? O2 W2 O4 152.15(19) . . ? O5 W2 O4 86.52(19) . . ? O3 W2 O8 103.4(2) . 3_765 ? O2 W2 O8 86.8(2) . 3_765 ? O5 W2 O8 151.94(19) . 3_765 ? O4 W2 O8 86.4(2) . 3_765 ? O3 W2 O10 179.3(2) . . ? O2 W2 O10 76.27(13) . . ? O5 W2 O10 75.98(13) . . ? O4 W2 O10 75.88(13) . . ? O8 W2 O10 75.96(14) 3_765 . ? O7 W3 O8 103.9(3) . . ? O7 W3 O6 102.8(2) . . ? O8 W3 O6 86.4(2) . . ? O7 W3 O5 103.4(2) . . ? O8 W3 O5 152.73(19) . . ? O6 W3 O5 86.8(2) . . ? O7 W3 O9 104.2(2) . . ? O8 W3 O9 87.1(2) . . ? O6 W3 O9 152.9(2) . . ? O5 W3 O9 87.03(19) . . ? O7 W3 O10 179.04(19) . . ? O8 W3 O10 76.50(14) . . ? O6 W3 O10 76.31(14) . . ? O5 W3 O10 76.23(13) . . ? O9 W3 O10 76.64(13) . . ? N4 Zn1 N2 120.4(2) . . ? N4 Zn1 N1 91.3(2) . . ? N2 Zn1 N1 83.1(2) . . ? N4 Zn1 N3 84.1(2) . . ? N2 Zn1 N3 89.6(2) . . ? N1 Zn1 N3 168.0(2) . . ? N4 Zn1 Cl1 122.47(17) . . ? N2 Zn1 Cl1 117.10(17) . . ? N1 Zn1 Cl1 93.44(18) . . ? N3 Zn1 Cl1 98.43(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 N2 N3 N4 32.8(2) . . . . ? 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 C9 H9B O1 0.97 2.67 3.569(9) 154.5 3_766 C16 H16B O5 0.96 2.69 3.613(9) 162.2 4_566 N3 H3 Cl1 0.83(5) 2.61(5) 3.397(7) 157(4) 3_666 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.598 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.160 #END******************************************************