# Copyright The Royal Society of Chemistry, 1998 # ref. 8/02148A data_global _audit_creation_date ? _audit_creation_method 'CIFmaker on Quansan personal computer' _audit_update_record ? _publ_contact_author ; Dr. Corrado Rizzoli Universita di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale delle Scienze 78 I-43100 Parma Italy ; _publ_contact_author_phone '[039]521 905 449' _publ_contact_author_fax '[039]521 905 556' _publ_contact_author_email 'rizzoli@at@ipruniv.cce.unipr.it' _publ_section_title ; Molybdenum-carbon functionalitiessupported by a quadridentate Schiff base ligand: the reactivity of [trans-dichloro{N,N`-o- phenylenebis(salicylideneiminato)}-molybdenum(IV)] ; _jounal_name_full 'J.C.S., Dalton Transactions' ######## Please note: paper submitted, not published ########### loop_ _publ_author_name _publ_author_address 'Euro Solari' ; Institut de Chemie Minerale et Analytique Universite de Lausanne BCH CH-1015 Lausanne Switzerland ; 'Cristiano Maltese' ; Institut de Chemie Minerale et Analytique Universite de Lausanne BCH CH-1015 Lausanne Switzerland ; 'Mario Latronico' ; Dipartimento di Ingegneria e Fisica dell Ambiente Universita della Basilicata I-85100 Potenza Switzerland ; 'Carlo Floriani(*)' ; Institut de Chemie Minerale et Analytique Universite de Lausanne BCH CH-1015 Lausanne Switzerland ; 'Angiola Chiesi-Villa' ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universita di Parma Viale delle Scienze 78 I-43100 Parma Italy ; 'Corrado Rizzoli' ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale delle Scienze 78 Universita di Parma I-43100 Parma Italy ; _publ_section_references ; North, A.C.T, Phillips, D.C, Mathews, F.S. (1968) Acta Cryst., A, Cryst. Phys., Diffr., Theor. Gen. Crystallogr., A24, 351-359 TEXSAN - TEXRAY Structure Analysis Package, Molecular Structure Corporation (1985). Sheldrick, G.M. (1976). SHELX76, Programs for the solution of crystal structures. Univ. of Cambridge, England Sheldrick, G.M. (1993). SHELXL93, Program for the crystal structure refinement. Univ. of Gottingen, Germany ; _publ_section_explt_prep ; ? ; _publ_section_explt_refinement ; ? ; ######################################################################## ###### #### Complex 2 Crystallographic Data data_COMPLEX_2 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40H54Cl2MoN2O3' _chemical_formula_weight 777.72 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mo' 'Mo' -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.648(3) _cell_length_b 15.105(5) _cell_length_c 11.149(3) _cell_angle_alpha 108.48(3) _cell_angle_beta 105.37(2) _cell_angle_gamma 63.91(2) _cell_volume 1936.3(10) _cell_formula_units_Z 2.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 133 _cell_measurement_theta_min 44.1 _cell_measurement_theta_max 47.9 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.3339 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 816.0 _exptl_absorpt_coefficient_mu 4.4083 _exptl_absorpt_correction_type 'North et al. 1968' _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 133 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuKa _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 7543 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 70.16 _reflns_number_total 7218 _reflns_number_observed 4910 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN Software' _computing_cell_refinement 'TEXSAN Software' _computing_data_reduction 'TEXSAN Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 702 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs 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^)+( 0.0634P)^2^+4.9838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6516 _refine_ls_number_parameters 430 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_obs 0.0507 _refine_ls_wR_factor_all 0.1426 _refine_ls_wR_factor_obs 0.1284 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_obs 1.118 _refine_ls_restrained_S_all 1.159 _refine_ls_restrained_S_obs 1.114 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # #label x/a y/b z/c Ueq tmf typ . att R MO1 -0.08107(3) 0.39250(3) -0.31837(4) 0.0230(2) aniso Mo . . 1.84 CL1 -0.2411(1) 0.5136(1) -0.2217(1) 0.0298(5) aniso Cl . . 1.84 CL2 0.0785(1) 0.2697(1) -0.4141(1) 0.0324(5) aniso Cl . . 1.99 O1 -0.0674(3) 0.3030(3) -0.2187(3) 0.0254(15) aniso O . . 1.88 O2 -0.1692(3) 0.3735(2) -0.4838(3) 0.0259(15) aniso O . . 1.88 O3 0.4349(4) 0.0475(4) -0.3449(5) 0.0546(25) aniso O . . 2.09 N1 0.0353(3) 0.4362(3) -0.1699(4) 0.0227(17) aniso N . . 1.64 N2 -0.0800(3) 0.5183(3) -0.3652(4) 0.0223(16) aniso N . . 1.53 C1 0.0201(4) 0.2496(4) -0.1454(4) 0.0216(19) aniso C . . 1.83 C2 0.0317(4) 0.1553(4) -0.1342(5) 0.0244(20) aniso C . . 2.23 C3 0.1195(4) 0.1095(4) -0.0445(5) 0.0283(20) aniso C . . 2.91 C4 0.1953(4) 0.1514(4) 0.0305(5) 0.0323(23) aniso C . . 1.75 C5 0.1842(4) 0.2413(4) 0.0134(5) 0.0313(26) aniso C . . 2.46 C6 0.0983(4) 0.2915(4) -0.0742(5) 0.0264(22) aniso C . . 1.61 C7 0.0993(4) 0.3820(4) -0.0868(5) 0.0256(22) aniso C . . 2.69 C8 0.0528(4) 0.5213(4) -0.1762(5) 0.0227(21) aniso C . . 1.70 C9 0.1247(4) 0.5617(4) -0.0868(5) 0.0273(21) aniso C . . 1.63 C10 0.1381(5) 0.6408(4) -0.1065(5) 0.0333(25) aniso C . . 1.67 C11 0.0814(4) 0.6810(4) -0.2114(5) 0.0306(22) aniso C . . 1.47 C12 0.0104(4) 0.6420(4) -0.3003(5) 0.0295(23) aniso C . . 1.71 C13 -0.0050(4) 0.5623(4) -0.2826(5) 0.0226(19) aniso C . . 1.97 C14 -0.1502(4) 0.5616(4) -0.4551(5) 0.0232(21) aniso C . . 1.58 C15 -0.2334(4) 0.5306(4) -0.5413(5) 0.0256(21) aniso C . . 1.47 C16 -0.3061(4) 0.5952(4) -0.6212(5) 0.0242(19) aniso C . . 1.65 C17 -0.3921(4) 0.5760(4) -0.7055(5) 0.0252(20) aniso C . . 1.91 C18 -0.4044(4) 0.4880(4) -0.7085(5) 0.0255(22) aniso C . . 1.81 C19 -0.3329(4) 0.4176(4) -0.6349(5) 0.0234(19) aniso C . . 1.56 C20 -0.2461(4) 0.4399(4) -0.5515(5) 0.0227(18) aniso C . . 2.18 C21 -0.0442(4) 0.1020(4) -0.2187(5) 0.0282(22) aniso C . . 1.58 C22 -0.1617(4) 0.1612(4) -0.1905(6) 0.0370(26) aniso C . . 2.43 C23 -0.0417(6) 0.0913(5) -0.3598(6) 0.0478(31) aniso C . . 2.31 C24 -0.0072(5) -0.0055(4) -0.2024(7) 0.0461(30) aniso C . . 2.93 C25 0.2892(5) 0.0976(5) 0.1262(7) 0.0442(26) aniso C . . 3.86 C26A 0.3055(15) -0.0060(13) 0.1183(17) 0.0249(21) iso C . . 1.78 C27A 0.3977(12) 0.1037(11) 0.1141(14) 0.0311(21) iso C . . 2.32 C28A 0.2627(16) 0.1665(15) 0.2688(19) 0.0327(24) iso C . . 1.81 C26B 0.3478(12) -0.0218(11) 0.0531(14) 0.0338(25) iso C . . 2.12 C27B 0.3763(11) 0.1386(11) 0.1745(14) 0.0274(21) iso C . . 1.73 C28B 0.2404(13) 0.0912(13) 0.2315(16) 0.0342(23) iso C . . 1.93 C29 -0.4717(4) 0.6500(4) -0.7901(5) 0.0432(30) aniso C . . 2.91 C30 -0.5148(4) 0.7584(4) -0.7082(5) 0.0417(29) aniso C . . 2.34 C31 -0.5705(4) 0.6231(4) -0.8646(5) 0.0433(25) aniso C . . 1.92 C32 -0.4064(4) 0.6468(4) -0.8874(5) 0.0487(29) aniso C . . 1.84 C33 -0.3522(4) 0.3231(4) -0.6413(5) 0.0515(33) aniso C . . 1.73 C34 -0.2529(5) 0.2268(4) -0.6848(6) 0.0831(53) aniso C . . 3.40 C35 -0.4542(5) 0.3164(5) -0.7374(7) 0.0330(31) aniso C . . 0.00 C36 -0.3696(5) 0.3266(5) -0.5096(6) 0.0463(35) aniso C . . 0.00 C37 0.3517(5) 0.1006(5) -0.2633(7) 0.0377(33) aniso C . . 0.00 C38 0.2847(5) 0.0372(5) -0.2972(7) 0.0407(36) aniso C . . 0.00 C39 0.2906(6) -0.0067(5) -0.4379(7) 0.0476(39) aniso C . . 0.00 C40 0.4024(8) -0.0241(8) -0.4466(8) 0.0818(63) aniso C . . 0.00 H3 0.13170(0) 0.04240(0) -0.03500(0) 0.0500(0) iso H . C3 1.00 H5 0.23620(0) 0.27080(0) 0.06430(0) 0.0500(0) iso H . C5 1.00 H7 0.15540(0) 0.40440(0) -0.03850(0) 0.0500(0) iso H . C7 1.00 H9 0.16060(0) 0.53430(0) -0.00570(0) 0.0500(0) iso H . C9 1.00 H10 0.18480(0) 0.66580(0) -0.04760(0) 0.0500(0) iso H . C10 1.00 H11 0.09370(0) 0.73590(0) -0.21540(0) 0.0500(0) iso H . C11 1.00 H12 -0.02740(0) 0.66500(0) -0.37270(0) 0.0500(0) iso H . C12 1.00 H14 -0.13970(0) 0.61130(0) -0.48390(0) 0.0500(0) iso H . C14 1.00 H16 -0.29340(0) 0.64890(0) -0.62510(0) 0.0500(0) iso H . C16 1.00 H18 -0.46230(0) 0.47380(0) -0.76130(0) 0.0500(0) iso H . C18 1.00 H221 -0.21550(0) 0.13040(0) -0.24010(0) 0.0500(0) iso H . C22 1.00 H222 -0.19780(0) 0.23440(0) -0.19500(0) 0.0500(0) iso H . C22 1.00 H223 -0.17200(0) 0.16350(0) -0.09880(0) 0.0500(0) iso H . C22 1.00 H231 0.02240(0) 0.05970(0) -0.39080(0) 0.0500(0) iso H . C23 1.00 H232 -0.07600(0) 0.15800(0) -0.38920(0) 0.0500(0) iso H . C23 1.00 H233 -0.09710(0) 0.05730(0) -0.41710(0) 0.0500(0) iso H . C23 1.00 H241 0.06590(0) -0.03910(0) -0.21390(0) 0.0500(0) iso H . C24 1.00 H242 -0.06800(0) -0.03510(0) -0.26050(0) 0.0500(0) iso H . C24 1.00 H243 -0.01520(0) -0.00160(0) -0.11900(0) 0.0500(0) iso H . C24 1.00 H301 -0.55840(0) 0.75930(0) -0.64390(0) 0.0500(0) iso H . C30 1.00 H302 -0.56650(0) 0.80590(0) -0.76210(0) 0.0500(0) iso H . C30 1.00 H303 -0.44260(0) 0.78400(0) -0.66430(0) 0.0500(0) iso H . C30 1.00 H311 -0.55000(0) 0.55930(0) -0.93070(0) 0.0500(0) iso H . C31 1.00 H312 -0.61780(0) 0.62340(0) -0.81510(0) 0.0500(0) iso H . C31 1.00 H313 -0.62170(0) 0.67290(0) -0.92140(0) 0.0500(0) iso H . C31 1.00 H321 -0.33660(0) 0.65610(0) -0.85240(0) 0.0500(0) iso H . C32 1.00 H322 -0.45700(0) 0.69660(0) -0.95210(0) 0.0500(0) iso H . C32 1.00 H323 -0.37850(0) 0.57540(0) -0.94130(0) 0.0500(0) iso H . C32 1.00 H341 -0.18550(0) 0.22630(0) -0.62840(0) 0.0500(0) iso H . C34 1.00 H342 -0.24970(0) 0.22530(0) -0.77530(0) 0.0500(0) iso H . C34 1.00 H343 -0.26760(0) 0.16540(0) -0.68270(0) 0.0500(0) iso H . C34 1.00 H351 -0.51950(0) 0.37380(0) -0.70570(0) 0.0500(0) iso H . C35 1.00 H352 -0.46130(0) 0.24740(0) -0.73940(0) 0.0500(0) iso H . C35 1.00 H353 -0.43990(0) 0.30760(0) -0.82850(0) 0.0500(0) iso H . C35 1.00 H361 -0.43160(0) 0.38310(0) -0.48400(0) 0.0500(0) iso H . C36 1.00 H362 -0.30480(0) 0.33200(0) -0.42970(0) 0.0500(0) iso H . C36 1.00 H363 -0.38230(0) 0.26760(0) -0.51930(0) 0.0500(0) iso H . C36 1.00 H371 0.30580(0) 0.15510(0) -0.29360(0) 0.0500(0) iso H . C37 1.00 H372 0.39200(0) 0.10920(0) -0.17610(0) 0.0500(0) iso H . C37 1.00 H381 0.20630(0) 0.07960(0) -0.28710(0) 0.0500(0) iso H . C38 1.00 H382 0.32580(0) -0.02140(0) -0.25110(0) 0.0500(0) iso H . C38 1.00 H391 0.28210(0) -0.06570(0) -0.46440(0) 0.0500(0) iso H . C39 1.00 H392 0.23300(0) 0.04650(0) -0.50150(0) 0.0500(0) iso H . C39 1.00 H401 0.46920(0) -0.11110(0) -0.44570(0) 0.0500(0) iso H . C40 1.00 H402 0.40800(0) -0.02050(0) -0.52850(0) 0.0500(0) iso H . C40 1.00 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 #label U11 U22 U33 U23 U13 U12 MO1 0.0214(2) 0.0224(2) 0.0233(2) 0.0094(2) -0.0021(1) -0.0070(2) CL1 0.0226(6) 0.0305(6) 0.0303(7) 0.0088(5) 0.0034(5) -0.0040(5) CL2 0.0276(6) 0.0320(7) 0.0320(7) 0.0125(5) 0.0052(5) -0.0027(5) O1 0.0212(17) 0.0267(18) 0.0286(19) 0.0123(15) -0.0022(14) -0.0089(14) O2 0.0253(18) 0.0199(16) 0.0283(19) 0.0084(14) 0.0009(15) -0.0049(14) O3 0.0473(27) 0.0585(30) 0.0614(32) 0.0024(25) 0.0106(23) -0.0299(24) N1 0.0216(20) 0.0263(21) 0.0206(21) 0.0050(17) -0.0008(16) -0.0122(17) N2 0.0190(19) 0.0231(20) 0.0216(21) 0.0054(17) 0.0003(16) -0.0066(16) C1 0.0185(23) 0.0274(24) 0.0176(23) 0.0076(19) 0.0010(18) -0.0070(20) C2 0.0169(23) 0.0238(24) 0.0264(26) 0.0051(21) 0.0056(19) -0.0015(19) C3 0.0188(24) 0.0280(26) 0.0357(30) 0.0175(23) 0.0008(21) -0.0018(20) C4 0.0256(27) 0.0342(29) 0.0352(31) 0.0135(25) -0.0016(23) -0.0096(23) C5 0.0228(26) 0.0359(29) 0.0320(29) 0.0159(24) -0.0055(22) -0.0084(23) C6 0.0199(24) 0.0281(26) 0.0306(28) 0.0096(22) 0.0027(21) -0.0073(21) C7 0.0200(23) 0.0339(27) 0.0205(25) 0.0107(21) -0.0052(19) -0.0099(21) C8 0.0191(23) 0.0205(23) 0.0278(26) 0.0048(20) 0.0012(19) -0.0089(19) C9 0.0218(25) 0.0279(26) 0.0278(28) 0.0079(22) 0.0009(21) -0.0061(21) C10 0.0317(29) 0.0378(30) 0.0316(30) 0.0058(24) -0.0001(23) -0.0186(25) C11 0.0292(27) 0.0331(28) 0.0317(30) 0.0093(24) 0.0000(23) -0.0152(23) C12 0.0309(28) 0.0333(28) 0.0257(27) 0.0120(23) -0.0013(22) -0.0134(23) C13 0.0189(23) 0.0169(22) 0.0273(26) 0.0026(19) 0.0046(19) -0.0035(19) C14 0.0235(24) 0.0208(23) 0.0240(26) 0.0087(20) 0.0027(20) -0.0054(19) C15 0.0237(25) 0.0237(25) 0.0286(27) 0.0052(21) 0.0077(21) -0.0067(20) C16 0.0210(24) 0.0213(24) 0.0273(27) 0.0088(20) 0.0024(20) -0.0040(20) C17 0.0237(25) 0.0205(23) 0.0244(26) 0.0046(20) 0.0044(20) -0.0024(20) C18 0.0212(24) 0.0226(24) 0.0259(26) 0.0038(20) 0.0000(20) -0.0056(20) C19 0.0236(24) 0.0191(23) 0.0254(26) 0.0060(20) 0.0057(20) -0.0047(19) C20 0.0187(23) 0.0219(23) 0.0218(25) 0.0084(20) 0.0008(19) -0.0018(19) C21 0.0246(26) 0.0234(25) 0.0355(30) 0.0077(22) 0.0036(22) -0.0080(21) C22 0.0251(28) 0.0295(28) 0.0543(38) 0.0041(26) 0.0082(26) -0.0112(23) C23 0.0559(41) 0.0606(42) 0.0313(33) 0.0017(30) 0.0048(29) -0.0334(36) C24 0.0435(36) 0.0259(29) 0.0579(43) 0.0063(28) -0.0043(31) -0.0126(27) C25 0.0307(31) 0.0545(39) 0.0488(39) 0.0347(33) -0.0073(27) -0.0097(28) C29 0.0218(24) 0.0261(25) 0.0232(26) 0.0079(21) -0.0021(20) -0.0076(20) C30 0.0330(29) 0.0216(25) 0.0305(29) 0.0071(22) 0.0069(23) -0.0014(22) C31 0.0301(28) 0.0304(28) 0.0317(30) 0.0093(24) -0.0026(23) -0.0091(23) C32 0.0262(27) 0.0452(33) 0.0282(29) 0.0149(25) 0.0042(22) -0.0078(25) C33 0.0247(26) 0.0232(25) 0.0335(29) 0.0097(22) -0.0006(22) -0.0091(21) C34 0.0358(30) 0.0240(26) 0.0404(33) 0.0057(23) 0.0028(25) -0.0122(24) C35 0.0330(31) 0.0389(33) 0.0607(42) 0.0221(31) -0.0114(29) -0.0196(27) C36 0.0463(35) 0.0380(32) 0.0483(38) 0.0109(28) 0.0220(30) -0.0138(28) C37 0.0377(33) 0.0324(31) 0.0502(39) 0.0041(28) 0.0100(29) -0.0066(26) C38 0.0407(36) 0.0525(39) 0.0540(42) 0.0088(33) 0.0180(31) -0.0152(31) C39 0.0476(39) 0.0497(39) 0.0563(44) 0.0061(33) 0.0026(33) -0.0250(33) C40 0.0818(63) 0.1246(85) 0.0507(49) -0.0136(51) 0.0203(44) -0.0642(63) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MO1 CL1 2.400(1) yes MO1 CL2 2.397(1) yes MO1 O1 1.928(5) yes MO1 O2 1.929(3) yes MO1 N1 2.129(4) yes MO1 N2 2.131(5) yes O1 C1 1.341(5) yes O2 C20 1.346(6) yes O3 C37 1.430(9) yes O3 C40 1.42(1) yes N1 C7 1.309(7) yes N1 C8 1.432(9) yes N2 C13 1.431(7) yes N2 C14 1.306(7) yes C1 C2 1.405(9) yes C1 C6 1.413(8) yes C2 C3 1.410(7) yes C2 C21 1.531(8) yes C3 C4 1.397(8) yes C4 C5 1.37(1) yes C4 C25 1.533(8) yes C5 C6 1.408(7) yes C6 C7 1.42(1) yes C8 C9 1.397(8) yes C8 C13 1.398(8) yes C9 C10 1.37(1) yes C10 C11 1.376(8) yes C11 C12 1.375(8) yes C12 C13 1.39(1) yes C14 C15 1.427(8) yes C15 C16 1.400(8) yes C15 C20 1.42(1) yes C16 C17 1.374(7) yes C17 C18 1.40(1) yes C17 C29 1.541(8) yes C18 C19 1.404(8) yes C19 C20 1.396(8) yes C19 C33 1.54(1) yes C21 C22 1.516(7) yes C21 C23 1.538(9) yes C21 C24 1.530(9) yes C25 C26A 1.46(2) yes C25 C27A 1.57(2) yes C25 C28A 1.63(2) yes C25 C26B 1.64(1) yes C25 C27B 1.48(1) yes C25 C28B 1.54(2) yes C29 C30 1.533(7) yes C29 C31 1.532(8) yes C29 C32 1.55(1) yes C33 C34 1.535(7) yes C33 C35 1.536(8) yes C33 C36 1.53(1) yes C37 C38 1.50(1) yes C38 C39 1.51(1) yes C39 C40 1.45(1) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 MO1 N2 76.4(2) yes O2 MO1 N2 85.9(2) yes O2 MO1 N1 160.0(2) yes O1 MO1 N2 160.4(2) yes O1 MO1 N1 86.1(2) yes O1 MO1 O2 112.7(2) yes CL2 MO1 N2 95.5(2) yes CL2 MO1 N1 84.4(2) yes CL2 MO1 O2 88.4(1) yes CL2 MO1 O1 91.4(2) yes CL1 MO1 N2 85.3(1) yes CL1 MO1 N1 95.8(1) yes CL1 MO1 O2 91.7(1) yes CL1 MO1 O1 87.8(1) yes CL1 MO1 CL2 179.2(1) yes MO1 O1 C1 130.7(4) yes MO1 O2 C20 131.9(3) yes C37 O3 C40 108.5(7) yes MO1 N1 C8 116.2(3) yes MO1 N1 C7 123.2(4) yes C7 N1 C8 120.1(5) yes MO1 N2 C14 123.6(4) yes MO1 N2 C13 116.3(3) yes C13 N2 C14 119.8(5) yes O1 C1 C6 119.2(5) yes O1 C1 C2 120.7(5) yes C2 C1 C6 120.0(5) yes C1 C2 C21 121.9(5) yes C1 C2 C3 117.0(5) yes C3 C2 C21 121.0(5) yes C2 C3 C4 123.9(5) yes C3 C4 C25 121.4(6) yes C3 C4 C5 117.5(5) yes C5 C4 C25 121.1(6) yes C4 C5 C6 121.6(6) yes C1 C6 C5 119.8(5) yes C5 C6 C7 115.8(5) yes C1 C6 C7 124.3(5) yes N1 C7 C6 127.2(5) yes N1 C8 C13 115.7(5) yes N1 C8 C9 124.4(5) yes C9 C8 C13 119.9(6) yes C8 C9 C10 118.9(5) yes C9 C10 C11 121.2(6) yes C10 C11 C12 120.6(6) yes C11 C12 C13 119.4(5) yes C8 C13 C12 120.0(5) yes N2 C13 C12 124.6(5) yes N2 C13 C8 115.4(5) yes N2 C14 C15 126.9(5) yes C14 C15 C20 124.7(5) yes C14 C15 C16 116.3(5) yes C16 C15 C20 118.9(5) yes C15 C16 C17 122.2(6) yes C16 C17 C29 120.7(5) yes C16 C17 C18 116.9(5) yes C18 C17 C29 122.4(5) yes C17 C18 C19 124.4(6) yes C18 C19 C33 121.7(5) yes C18 C19 C20 116.6(5) yes C20 C19 C33 121.6(5) yes C15 C20 C19 120.8(5) yes O2 C20 C19 120.7(5) yes O2 C20 C15 118.4(5) yes C2 C21 C24 112.9(5) yes C2 C21 C23 109.0(5) yes C2 C21 C22 111.2(5) yes C23 C21 C24 106.2(5) yes C22 C21 C24 108.0(5) yes C22 C21 C23 109.4(5) yes C4 C25 C28B 109.4(9) yes C4 C25 C27B 114.2(8) yes C4 C25 C26B 107.8(7) yes C4 C25 C28A 106.8(9) yes C4 C25 C27A 108.5(8) yes C4 C25 C26A 115.9(9) yes C27B C25 C28B 114(1) yes C26B C25 C28B 103(1) yes C26B C25 C27B 107(1) yes C27A C25 C28A 104(1) yes C26A C25 C28A 109(1) yes C26A C25 C27A 111(1) yes C17 C29 C32 108.1(5) yes C17 C29 C31 113.0(5) yes C17 C29 C30 110.3(4) yes C31 C29 C32 108.5(4) yes C30 C29 C32 108.3(5) yes C30 C29 C31 108.6(5) yes C19 C33 C36 109.6(5) yes C19 C33 C35 112.0(5) yes C19 C33 C34 110.1(5) yes C35 C33 C36 108.1(6) yes C34 C33 C36 109.9(5) yes C34 C33 C35 107.1(5) yes O3 C37 C38 105.2(6) yes C37 C38 C39 101.7(6) yes C38 C39 C40 102.7(7) yes O3 C40 C39 107.9(7) yes _refine_diff_density_max 0.978 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.107 #=END ######################################################################## ###### #### Complex 4 Crystallographic Data data_COMPLEX_4 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C47H47MoN2O2' _chemical_formula_weight 767.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mo' 'Mo' -0.0483 2.7339 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/N' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.188(2) _cell_length_b 30.228(4) _cell_length_c 13.615(2) _cell_angle_alpha 90.00(0) _cell_angle_beta 103.99(2) _cell_angle_gamma 90.00(0) _cell_volume 3669.2(11) _cell_formula_units_Z 4.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 133 _cell_measurement_theta_min 40.1 _cell_measurement_theta_max 52.9 _exptl_crystal_description elongated_prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.3900 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 1604.0 _exptl_absorpt_coefficient_mu 3.2828 _exptl_absorpt_correction_type 'North et al. 1968' _exptl_absorpt_correction_T_min 0.643 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 133 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuKa _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.2 _diffrn_reflns_number 7267 _diffrn_reflns_av_R_equivalents 0.1630 _diffrn_reflns_av_sigmaI/netI 0.1107 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 70.11 _reflns_number_total 6818 _reflns_number_observed 4104 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN Software' _computing_cell_refinement 'TEXSAN Software' _computing_data_reduction 'TEXSAN Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 859 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs 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^)+( 0.1052P)^2^+7.7431P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5959 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1430 _refine_ls_R_factor_obs 0.0676 _refine_ls_wR_factor_all 0.1956 _refine_ls_wR_factor_obs 0.1728 _refine_ls_goodness_of_fit_all 1.101 _refine_ls_goodness_of_fit_obs 1.187 _refine_ls_restrained_S_all 1.476 _refine_ls_restrained_S_obs 1.187 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # #label x/a y/b z/c Ueq tmf typ . att R MO1 -0.18641(6) 0.14494(2) 0.15588(4) 0.0207(2) aniso Mo . . 1.51 O1 -0.0463(6) 0.1788(2) 0.0992(4) 0.0285(17) aniso O . . 2.21 O2 -0.2556(6) 0.1983(2) 0.2092(4) 0.0289(15) aniso O . . 1.80 N1 -0.2732(7) 0.1156(2) 0.0268(4) 0.0222(19) aniso N . . 1.85 N2 -0.3667(7) 0.1170(2) 0.1870(4) 0.0248(20) aniso N . . 2.36 C1 0.0115(9) 0.1681(2) 0.0192(5) 0.0284(26) aniso C . . 1.71 C2 0.1491(9) 0.1866(3) 0.0165(6) 0.0358(27) aniso C . . 2.35 C3 0.2171(10) 0.1753(3) -0.0601(7) 0.0427(31) aniso C . . 1.92 C4 0.1493(10) 0.1458(3) -0.1334(7) 0.0428(30) aniso C . . 2.05 C5 0.0114(9) 0.1287(3) -0.1317(6) 0.0351(28) aniso C . . 3.08 C6 -0.0637(8) 0.1392(2) -0.0569(5) 0.0271(21) aniso C . . 1.85 C7 -0.2188(8) 0.1190(2) -0.0691(5) 0.0239(23) aniso C . . 1.66 C8 -0.4074(8) 0.0924(2) 0.0190(5) 0.0272(24) aniso C . . 1.94 C9 -0.4849(9) 0.0679(2) -0.0628(6) 0.0310(26) aniso C . . 2.15 C10 -0.6202(10) 0.0483(3) -0.0619(6) 0.0395(30) aniso C . . 2.18 C11 -0.6794(10) 0.0532(3) 0.0227(7) 0.0408(31) aniso C . . 2.44 C12 -0.6025(9) 0.0761(3) 0.1076(6) 0.0352(28) aniso C . . 2.03 C13 -0.4633(8) 0.0950(3) 0.1076(5) 0.0272(24) aniso C . . 1.79 C14 -0.4196(8) 0.1292(2) 0.2789(5) 0.0266(23) aniso C . . 2.36 C15 -0.4727(8) 0.1760(2) 0.2636(5) 0.0261(23) aniso C . . 2.95 C16 -0.6127(10) 0.1886(3) 0.2829(6) 0.0359(28) aniso C . . 1.53 C17 -0.6576(10) 0.2321(3) 0.2735(6) 0.0396(30) aniso C . . 4.38 C18 -0.5727(10) 0.2642(3) 0.2411(6) 0.0373(28) aniso C . . 2.05 C19 -0.4372(9) 0.2516(3) 0.2172(6) 0.0330(25) aniso C . . 2.30 C20 -0.3912(8) 0.2081(2) 0.2282(5) 0.0249(22) aniso C . . 2.47 C21 -0.3351(8) 0.1409(2) -0.1573(5) 0.0245(23) aniso C . . 1.62 C22 -0.4027(8) 0.1818(2) -0.1476(5) 0.0228(21) aniso C . . 2.14 C23 -0.4979(8) 0.2013(2) -0.2308(5) 0.0255(21) aniso C . . 1.83 C24 -0.5272(9) 0.1818(3) -0.3264(6) 0.0319(27) aniso C . . 1.65 C25 -0.4630(9) 0.1414(3) -0.3357(5) 0.0332(25) aniso C . . 2.91 C26 -0.3677(9) 0.1203(2) -0.2531(6) 0.0295(25) aniso C . . 2.42 C27 -0.3715(9) 0.2069(2) -0.0491(6) 0.0312(27) aniso C . . 1.91 C28 -0.6250(12) 0.2051(3) -0.4159(6) 0.0476(31) aniso C . . 3.64 C29 -0.3129(10) 0.0754(3) -0.2758(6) 0.0383(30) aniso C . . 3.68 C31 -0.3002(9) 0.1167(3) 0.3756(6) 0.0319(24) aniso C . . 2.20 C32 -0.2348(9) 0.1456(3) 0.4552(6) 0.0345(25) aniso C . . 2.11 C33 -0.1194(10) 0.1305(3) 0.5327(6) 0.0380(29) aniso C . . 3.30 C34 -0.0696(10) 0.0868(3) 0.5403(5) 0.0363(26) aniso C . . 4.30 C35 -0.1423(10) 0.0578(3) 0.4666(6) 0.0358(28) aniso C . . 3.56 C36 -0.2560(9) 0.0717(2) 0.3853(5) 0.0296(25) aniso C . . 2.41 C37 -0.2774(10) 0.1945(3) 0.4615(6) 0.0383(27) aniso C . . 2.63 C38 0.0623(11) 0.0722(3) 0.6224(7) 0.0447(29) aniso C . . 1.86 C39 -0.3275(10) 0.0369(3) 0.3129(6) 0.0371(27) aniso C . . 2.74 C41 -0.0207(8) 0.1033(2) 0.2456(5) 0.0227(22) aniso C . . 1.94 C42 0.0745(8) 0.1247(2) 0.3284(5) 0.0226(20) aniso C . . 1.58 C43 0.1890(9) 0.1027(3) 0.3921(6) 0.0307(23) aniso C . . 1.51 C44 0.2219(9) 0.0584(3) 0.3745(6) 0.0308(26) aniso C . . 1.86 C45 0.1322(9) 0.0378(2) 0.2897(5) 0.0285(25) aniso C . . 1.58 C46 0.0118(8) 0.0591(2) 0.2243(5) 0.0261(24) aniso C . . 1.95 C47 0.0537(9) 0.1729(3) 0.3513(6) 0.0342(26) aniso C . . 2.28 C48 0.3522(9) 0.0352(3) 0.4440(7) 0.0385(30) aniso C . . 1.98 C49 -0.0682(10) 0.0342(3) 0.1334(6) 0.0364(30) aniso C . . 1.73 H2 0.19500(0) 0.20650(0) 0.06040(0) 0.0500(0) iso H . C2 1.00 H3 0.32130(0) 0.19290(0) -0.05370(0) 0.0500(0) iso H . C3 1.00 H4 0.19910(0) 0.13740(0) -0.20350(0) 0.0500(0) iso H . C4 1.00 H5 -0.03090(0) 0.10960(0) -0.17760(0) 0.0500(0) iso H . C5 1.00 H7 -0.20620(0) 0.08300(0) -0.09120(0) 0.0500(0) iso H . C7 1.00 H9 -0.43520(0) 0.06110(0) -0.11380(0) 0.0500(0) iso H . C9 1.00 H10 -0.66090(0) 0.03870(0) -0.13230(0) 0.0500(0) iso H . C10 1.00 H11 -0.73200(0) 0.04230(0) 0.03370(0) 0.0500(0) iso H . C11 1.00 H12 -0.62870(0) 0.07840(0) 0.17990(0) 0.0500(0) iso H . C12 1.00 H14 -0.51400(0) 0.11280(0) 0.28620(0) 0.0500(0) iso H . C14 1.00 H16 -0.67910(0) 0.16670(0) 0.31360(0) 0.0500(0) iso H . C16 1.00 H17 -0.75210(0) 0.23830(0) 0.27500(0) 0.0500(0) iso H . C17 1.00 H18 -0.60850(0) 0.29760(0) 0.23980(0) 0.0500(0) iso H . C18 1.00 H19 -0.38830(0) 0.27570(0) 0.19930(0) 0.0500(0) iso H . C19 1.00 H23 -0.55270(0) 0.22970(0) -0.21770(0) 0.0500(0) iso H . C23 1.00 H25 -0.47930(0) 0.12910(0) -0.38720(0) 0.0500(0) iso H . C25 1.00 H271 -0.29200(0) 0.19150(0) -0.00200(0) 0.0500(0) iso H . C27 1.00 H272 -0.44710(0) 0.20820(0) -0.03640(0) 0.0500(0) iso H . C27 1.00 H273 -0.35020(0) 0.22720(0) -0.07110(0) 0.0500(0) iso H . C27 1.00 H281 -0.65140(0) 0.23390(0) -0.39690(0) 0.0500(0) iso H . C28 1.00 H282 -0.72000(0) 0.18770(0) -0.43450(0) 0.0500(0) iso H . C28 1.00 H283 -0.57950(0) 0.20770(0) -0.46450(0) 0.0500(0) iso H . C28 1.00 H291 -0.25620(0) 0.06020(0) -0.22620(0) 0.0500(0) iso H . C29 1.00 H292 -0.27610(0) 0.07620(0) -0.33560(0) 0.0500(0) iso H . C29 1.00 H293 -0.40900(0) 0.05400(0) -0.32100(0) 0.0500(0) iso H . C29 1.00 H33 -0.08480(0) 0.14960(0) 0.57810(0) 0.0500(0) iso H . C33 1.00 H35 -0.11000(0) 0.02840(0) 0.47650(0) 0.0500(0) iso H . C35 1.00 H371 -0.36520(0) 0.20440(0) 0.39630(0) 0.0500(0) iso H . C37 1.00 H372 -0.20000(0) 0.21320(0) 0.44820(0) 0.0500(0) iso H . C37 1.00 H373 -0.28810(0) 0.20870(0) 0.50990(0) 0.0500(0) iso H . C37 1.00 H381 0.10920(0) 0.09240(0) 0.67730(0) 0.0500(0) iso H . C38 1.00 H382 0.14070(0) 0.06700(0) 0.59650(0) 0.0500(0) iso H . C38 1.00 H383 0.03960(0) 0.04740(0) 0.66320(0) 0.0500(0) iso H . C38 1.00 H391 -0.39990(0) 0.04100(0) 0.27750(0) 0.0500(0) iso H . C39 1.00 H392 -0.34870(0) 0.00790(0) 0.33150(0) 0.0500(0) iso H . C39 1.00 H393 -0.28080(0) 0.02610(0) 0.27260(0) 0.0500(0) iso H . C39 1.00 H43 0.25120(0) 0.11590(0) 0.46050(0) 0.0500(0) iso H . C43 1.00 H45 0.14440(0) 0.01100(0) 0.26720(0) 0.0500(0) iso H . C45 1.00 H471 -0.00490(0) 0.18390(0) 0.30480(0) 0.0500(0) iso H . C47 1.00 H472 0.14110(0) 0.18700(0) 0.35440(0) 0.0500(0) iso H . C47 1.00 H473 0.04990(0) 0.17580(0) 0.42600(0) 0.0500(0) iso H . C47 1.00 H481 0.38890(0) 0.04800(0) 0.50350(0) 0.0500(0) iso H . C48 1.00 H482 0.41640(0) 0.02840(0) 0.40560(0) 0.0500(0) iso H . C48 1.00 H483 0.30710(0) 0.00880(0) 0.44660(0) 0.0500(0) iso H . C48 1.00 H491 -0.16380(0) 0.04010(0) 0.09530(0) 0.0500(0) iso H . C49 1.00 H492 -0.07040(0) -0.00020(0) 0.15990(0) 0.0500(0) iso H . C49 1.00 H493 -0.02260(0) 0.03080(0) 0.09370(0) 0.0500(0) iso H . C49 1.00 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 #label U11 U22 U33 U23 U13 U12 MO1 0.0259(3) 0.0175(3) 0.0189(3) -0.0006(2) 0.0055(2) 0.0003(3) O1 0.0364(30) 0.0268(27) 0.0213(25) -0.0050(20) 0.0052(22) -0.0061(22) O2 0.0329(29) 0.0276(27) 0.0268(26) -0.0054(21) 0.0083(22) -0.0065(23) N1 0.0293(32) 0.0192(28) 0.0175(27) -0.0015(22) 0.0046(24) -0.0027(25) N2 0.0328(34) 0.0225(30) 0.0193(28) -0.0028(23) 0.0066(25) 0.0064(26) C1 0.0349(43) 0.0284(39) 0.0221(36) 0.0000(29) 0.0070(32) -0.0045(33) C2 0.0362(45) 0.0436(49) 0.0258(38) 0.0061(34) 0.0036(33) -0.0112(38) C3 0.0308(46) 0.0492(55) 0.0503(53) 0.0027(43) 0.0144(39) -0.0030(39) C4 0.0398(46) 0.0495(52) 0.0451(47) 0.0029(44) 0.0223(38) -0.0006(44) C5 0.0367(45) 0.0380(43) 0.0368(43) -0.0056(35) 0.0206(36) 0.0086(36) C6 0.0259(36) 0.0233(37) 0.0318(37) -0.0012(30) 0.0064(30) 0.0060(30) C7 0.0256(37) 0.0194(35) 0.0276(36) -0.0033(28) 0.0081(30) 0.0010(28) C8 0.0329(41) 0.0206(36) 0.0260(37) -0.0016(28) 0.0033(31) -0.0041(30) C9 0.0419(46) 0.0209(36) 0.0317(39) -0.0008(30) 0.0117(34) -0.0043(33) C10 0.0407(49) 0.0403(49) 0.0341(43) -0.0025(36) 0.0026(37) -0.0129(39) C11 0.0382(48) 0.0355(47) 0.0492(50) 0.0026(38) 0.0116(39) -0.0137(38) C12 0.0303(43) 0.0395(47) 0.0360(43) -0.0007(36) 0.0084(35) -0.0106(36) C13 0.0310(41) 0.0323(40) 0.0181(33) -0.0002(29) 0.0056(30) 0.0001(33) C14 0.0301(40) 0.0289(38) 0.0255(36) -0.0011(29) 0.0160(31) 0.0002(32) C15 0.0237(38) 0.0275(39) 0.0299(37) -0.0016(30) 0.0119(30) 0.0095(30) C16 0.0404(47) 0.0334(44) 0.0358(44) -0.0009(35) 0.0132(37) 0.0049(37) C17 0.0454(51) 0.0401(48) 0.0349(43) -0.0021(36) 0.0130(38) 0.0240(40) C18 0.0491(52) 0.0353(45) 0.0259(39) -0.0019(33) 0.0057(36) 0.0041(39) C19 0.0466(48) 0.0238(39) 0.0302(39) -0.0010(31) 0.0125(35) 0.0064(34) C20 0.0289(39) 0.0248(38) 0.0227(34) -0.0002(28) 0.0094(29) 0.0096(31) C21 0.0243(36) 0.0228(34) 0.0261(33) 0.0024(31) 0.0058(28) -0.0041(30) C22 0.0203(36) 0.0236(35) 0.0219(34) -0.0006(27) 0.0001(27) -0.0060(28) C23 0.0283(38) 0.0191(34) 0.0280(36) -0.0032(28) 0.0044(30) -0.0031(29) C24 0.0318(42) 0.0333(43) 0.0279(39) -0.0044(33) 0.0017(32) -0.0027(34) C25 0.0408(44) 0.0305(40) 0.0267(36) -0.0119(33) 0.0048(32) 0.0027(36) C26 0.0414(46) 0.0239(40) 0.0265(37) -0.0040(29) 0.0145(34) 0.0025(33) C27 0.0388(45) 0.0232(38) 0.0308(40) -0.0043(31) 0.0071(33) 0.0014(33) C28 0.0748(68) 0.0368(49) 0.0248(41) -0.0018(36) -0.0001(42) 0.0162(46) C29 0.0577(55) 0.0313(44) 0.0215(37) -0.0060(32) 0.0008(36) 0.0112(39) C31 0.0429(47) 0.0306(41) 0.0257(37) -0.0011(30) 0.0151(36) 0.0036(35) C32 0.0375(43) 0.0402(45) 0.0281(37) 0.0085(36) 0.0124(32) 0.0066(40) C33 0.0563(55) 0.0359(45) 0.0213(37) -0.0061(32) 0.0086(36) 0.0062(40) C34 0.0551(54) 0.0362(46) 0.0174(34) 0.0060(32) 0.0083(35) 0.0188(40) C35 0.0524(52) 0.0356(44) 0.0250(38) 0.0027(33) 0.0206(37) 0.0119(39) C36 0.0388(44) 0.0292(41) 0.0247(36) 0.0056(31) 0.0149(33) 0.0005(34) C37 0.0549(55) 0.0326(44) 0.0254(39) -0.0055(33) 0.0054(37) 0.0038(39) C38 0.0549(57) 0.0437(54) 0.0374(46) 0.0041(39) 0.0148(42) 0.0137(44) C39 0.0565(56) 0.0265(41) 0.0272(38) 0.0034(31) 0.0084(38) 0.0104(38) C41 0.0243(37) 0.0193(35) 0.0252(34) 0.0028(27) 0.0073(29) 0.0062(28) C42 0.0258(36) 0.0204(34) 0.0207(33) 0.0008(27) 0.0037(28) 0.0037(29) C43 0.0355(43) 0.0280(40) 0.0271(37) 0.0017(31) 0.0043(32) 0.0023(33) C44 0.0354(44) 0.0281(39) 0.0303(39) 0.0031(31) 0.0106(33) 0.0086(33) C45 0.0333(42) 0.0231(37) 0.0286(38) -0.0019(30) 0.0063(32) 0.0022(31) C46 0.0309(40) 0.0181(34) 0.0291(37) 0.0019(29) 0.0069(31) 0.0046(30) C47 0.0375(46) 0.0253(40) 0.0347(42) -0.0056(33) -0.0014(35) 0.0020(34) C48 0.0325(45) 0.0383(47) 0.0415(46) 0.0033(38) 0.0030(37) 0.0098(37) C49 0.0437(50) 0.0291(41) 0.0365(44) -0.0063(34) 0.0097(38) -0.0012(36) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MO1 O1 1.944(6) yes MO1 O2 1.938(6) yes MO1 N1 1.958(5) yes MO1 N2 1.994(7) yes MO1 C41 2.120(6) yes O1 C1 1.36(1) yes O2 C20 1.36(1) yes N1 C7 1.51(1) yes N1 C8 1.40(1) yes N2 C13 1.391(9) yes N2 C14 1.49(1) yes C1 C2 1.39(1) yes C1 C6 1.403(9) yes C2 C3 1.38(1) yes C3 C4 1.37(1) yes C4 C5 1.37(1) yes C5 C6 1.40(1) yes C6 C7 1.52(1) yes C7 C21 1.550(9) yes C8 C9 1.383(9) yes C8 C13 1.42(1) yes C9 C10 1.38(1) yes C10 C11 1.40(1) yes C11 C12 1.39(1) yes C12 C13 1.40(1) yes C14 C15 1.495(9) yes C14 C31 1.54(1) yes C15 C16 1.43(1) yes C15 C20 1.38(1) yes C16 C17 1.37(1) yes C17 C18 1.38(1) yes C18 C19 1.41(1) yes C19 C20 1.38(1) yes C21 C22 1.404(9) yes C21 C26 1.41(1) yes C22 C23 1.384(9) yes C22 C27 1.51(1) yes C23 C24 1.39(1) yes C24 C25 1.38(1) yes C24 C28 1.50(1) yes C25 C26 1.40(1) yes C26 C29 1.51(1) yes C31 C32 1.41(1) yes C31 C36 1.42(1) yes C32 C33 1.38(1) yes C32 C37 1.54(1) yes C33 C34 1.39(1) yes C34 C35 1.38(1) yes C34 C38 1.50(1) yes C35 C36 1.39(1) yes C36 C39 1.48(1) yes C41 C42 1.406(9) yes C41 C46 1.414(9) yes C42 C43 1.36(1) yes C42 C47 1.51(1) yes C43 C44 1.41(1) yes C44 C45 1.39(1) yes C44 C48 1.51(1) yes C45 C46 1.398(9) yes C46 C49 1.48(1) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N2 MO1 C41 98.3(2) yes N1 MO1 C41 109.2(3) yes N1 MO1 N2 79.6(3) yes O2 MO1 C41 122.2(2) yes O2 MO1 N2 84.7(3) yes O2 MO1 N1 127.9(2) yes O1 MO1 C41 95.1(3) yes O1 MO1 N2 166.2(2) yes O1 MO1 N1 92.7(2) yes O1 MO1 O2 91.1(3) yes MO1 O1 C1 128.1(5) yes MO1 O2 C20 130.4(5) yes MO1 N1 C8 117.1(4) yes MO1 N1 C7 126.7(4) yes C7 N1 C8 116.0(5) yes MO1 N2 C14 121.9(4) yes MO1 N2 C13 116.4(5) yes C13 N2 C14 119.6(6) yes O1 C1 C6 121.4(7) yes O1 C1 C2 117.3(6) yes C2 C1 C6 121.3(7) yes C1 C2 C3 120.0(8) yes C2 C3 C4 120.1(9) yes C3 C4 C5 119.4(9) yes C4 C5 C6 123.1(8) yes C1 C6 C5 116.0(7) yes C5 C6 C7 116.3(6) yes C1 C6 C7 127.7(6) yes N1 C7 C6 115.4(5) yes C6 C7 C21 111.4(5) yes N1 C7 C21 112.9(6) yes N1 C8 C13 113.6(6) yes N1 C8 C9 127.0(7) yes C9 C8 C13 119.4(7) yes C8 C9 C10 120.8(7) yes C9 C10 C11 119.6(8) yes C10 C11 C12 121.3(9) yes C11 C12 C13 119.0(8) yes C8 C13 C12 119.6(6) yes N2 C13 C12 127.3(6) yes N2 C13 C8 113.1(6) yes N2 C14 C31 110.2(6) yes N2 C14 C15 106.2(5) yes C15 C14 C31 119.4(6) yes C14 C15 C20 121.8(6) yes C14 C15 C16 120.4(6) yes C16 C15 C20 117.8(6) yes C15 C16 C17 120.2(8) yes C16 C17 C18 121.4(9) yes C17 C18 C19 118.7(8) yes C18 C19 C20 119.8(8) yes C15 C20 C19 122.0(7) yes O2 C20 C19 117.2(7) yes O2 C20 C15 120.7(6) yes C7 C21 C26 118.7(6) yes C7 C21 C22 122.8(6) yes C22 C21 C26 118.4(6) yes C21 C22 C27 122.3(6) yes C21 C22 C23 120.3(6) yes C23 C22 C27 117.4(6) yes C22 C23 C24 121.7(6) yes C23 C24 C28 120.1(7) yes C23 C24 C25 118.1(7) yes C25 C24 C28 121.8(7) yes C24 C25 C26 121.9(7) yes C21 C26 C25 119.6(6) yes C25 C26 C29 114.9(7) yes C21 C26 C29 125.5(7) yes C14 C31 C36 116.3(6) yes C14 C31 C32 126.0(7) yes C32 C31 C36 117.7(7) yes C31 C32 C37 124.9(7) yes C31 C32 C33 119.3(8) yes C33 C32 C37 115.8(7) yes C32 C33 C34 123.2(8) yes C33 C34 C38 121.7(8) yes C33 C34 C35 117.2(8) yes C35 C34 C38 121.1(8) yes C34 C35 C36 121.8(8) yes C31 C36 C35 120.5(6) yes C35 C36 C39 116.2(7) yes C31 C36 C39 123.3(7) yes MO1 C41 C46 126.9(5) yes MO1 C41 C42 114.2(4) yes C42 C41 C46 118.5(6) yes C41 C42 C47 121.6(6) yes C41 C42 C43 121.3(6) yes C43 C42 C47 117.1(7) yes C42 C43 C44 121.4(7) yes C43 C44 C48 120.5(8) yes C43 C44 C45 117.3(8) yes C45 C44 C48 122.2(7) yes C44 C45 C46 122.7(6) yes C41 C46 C45 118.6(6) yes C45 C46 C49 117.0(6) yes C41 C46 C49 124.3(6) yes _refine_diff_density_max 1.321 _refine_diff_density_min -1.571 _refine_diff_density_rms 0.141 #=END ######################################################################## ###### #### Complex 5 Crystallographic Data data_COMPLEX_5 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C76H64Mo2N4O6' _chemical_formula_weight 1321.24 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mo' 'Mo' -0.0483 2.7339 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'PBCN' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 24.185(4) _cell_length_b 14.435(2) _cell_length_c 17.044(2) _cell_angle_alpha 90.00(0) _cell_angle_beta 90.00(0) _cell_angle_gamma 90.00(0) _cell_volume 5950.2(15) _cell_formula_units_Z 4.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 133 _cell_measurement_theta_min 44.0 _cell_measurement_theta_max 49.9 _exptl_crystal_description irregular_prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.4749 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 2720.0 _exptl_absorpt_coefficient_mu 3.9850 _exptl_absorpt_correction_type 'North et al. 1968' _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 133 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuKa _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.3 _diffrn_reflns_number 5631 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 70.11 _reflns_number_total 5631 _reflns_number_observed 3303 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN Software' _computing_cell_refinement 'TEXSAN Software' _computing_data_reduction 'TEXSAN Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 712 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs 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^)+( 0.0513P)^2^+6.1205P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4919 _refine_ls_number_parameters 412 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1109 _refine_ls_R_factor_obs 0.0420 _refine_ls_wR_factor_all 0.1209 _refine_ls_wR_factor_obs 0.1047 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.140 _refine_ls_restrained_S_all 1.252 _refine_ls_restrained_S_obs 1.135 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # #label x/a y/b z/c Ueq tmf typ . att R MO1 -0.03797(1) 0.19678(2) 0.69836(2) 0.0148(1) aniso Mo . . 1.36 O1 -0.0581(1) 0.2849(2) 0.6119(2) 0.0202(10) aniso O . . 1.78 O2 0.1191(1) 0.1705(2) 0.7942(2) 0.0221(10) aniso O . . 1.54 O3A -0.1754(5) -0.1009(9) 0.6036(8) 0.0195(13) iso O . . 1.66 O3B -0.2692(8) -0.0849(14) 0.6464(11) 0.0163(11) iso O . . 2.71 O3C -0.2096(8) -0.2161(15) 0.6887(13) 0.0163(10) iso O . . 2.71 N1 -0.0492(2) 0.0929(3) 0.6036(2) 0.0218(16) aniso N . . 1.91 N2 0.0349(2) 0.1161(2) 0.6939(2) 0.0310(19) aniso N . . 2.30 C1 -0.0935(2) 0.2738(4) 0.5537(3) 0.0378(21) aniso C . . 3.64 C2 -0.1153(2) 0.3533(4) 0.5188(4) 0.0316(20) aniso C . . 3.33 C3 -0.1518(2) 0.3495(5) 0.4580(4) 0.0249(16) aniso C . . 2.16 C4 -0.1688(2) 0.2634(5) 0.4289(4) 0.0243(17) aniso C . . 1.36 C5 -0.1455(2) 0.1839(5) 0.4585(3) 0.0201(14) aniso C . . 1.49 C6 -0.1077(2) 0.1869(4) 0.5214(3) 0.0301(16) aniso C . . 2.02 C7 -0.0817(2) 0.1016(4) 0.5437(3) 0.0356(19) aniso C . . 3.25 C8 -0.0216(2) 0.0098(4) 0.6218(3) 0.0335(18) aniso C . . 2.97 C9 -0.0354(2) -0.0795(4) 0.5951(4) 0.0247(14) aniso C . . 1.91 C10 -0.0038(3) -0.1536(4) 0.6197(4) 0.0180(14) aniso C . . 2.38 C11 0.0418(3) -0.1412(4) 0.6681(4) 0.0175(14) aniso C . . 1.63 C12 0.0555(2) -0.0538(4) 0.6955(4) 0.0201(15) aniso C . . 2.88 C13 0.0227(2) 0.0216(3) 0.6729(3) 0.0260(16) aniso C . . 2.48 C14 0.0775(2) 0.1501(3) 0.6373(3) 0.0350(19) aniso C . . 2.85 C15 0.1340(2) 0.1181(3) 0.6620(3) 0.0418(23) aniso C . . 3.69 C16 0.1696(2) 0.0762(4) 0.6093(3) 0.0346(19) aniso C . . 2.13 C17 0.2216(2) 0.0459(4) 0.6311(4) 0.0225(14) aniso C . . 2.34 C18 0.2384(2) 0.0596(5) 0.7075(4) 0.0174(15) aniso C . . 2.30 C19 0.2037(2) 0.1009(4) 0.7608(4) 0.0199(14) aniso C . . 2.02 C20 0.1512(2) 0.1315(4) 0.7396(3) 0.0199(13) aniso C . . 2.02 C21 0.0748(2) 0.2540(3) 0.6391(3) 0.0208(15) aniso C . . 2.42 C22 0.0491(2) 0.2936(3) 0.7012(3) 0.0302(16) aniso C . . 2.67 C31 0.1047(2) 0.3029(4) 0.5754(3) 0.0394(19) aniso C . . 2.86 C32 0.1616(2) 0.3157(4) 0.5785(4) 0.0392(21) aniso C . . 2.59 C33 0.1893(3) 0.3614(4) 0.5192(4) 0.0292(17) aniso C . . 1.77 C34 0.1599(3) 0.3950(5) 0.4559(4) 0.0212(14) aniso C . . 2.27 C35 0.1035(3) 0.3828(5) 0.4515(4) 0.0233(16) aniso C . . 2.02 C36 0.0757(2) 0.3384(4) 0.5117(4) 0.0308(18) aniso C . . 2.63 C41 0.0561(2) 0.3968(3) 0.7071(3) 0.0371(19) aniso C . . 4.12 C42 0.0265(2) 0.4586(4) 0.6611(3) 0.0286(15) aniso C . . 3.85 C43 0.0395(3) 0.5526(4) 0.6628(4) 0.0229(15) aniso C . . 1.77 C44 0.0803(3) 0.5851(4) 0.7121(4) 0.0459(35) aniso C . . 0.00 C45 0.1097(2) 0.5243(4) 0.7580(3) 0.0243(26) aniso C . . 0.00 C46 0.0974(2) 0.4306(4) 0.7558(3) 0.0217(25) aniso C . . 0.00 C51A -0.2322(5) -0.1049(16) 0.5860(11) 0.0554(61) iso C . . 0.00 C52A -0.2611(7) -0.1553(13) 0.6537(10) 0.0607(47) iso C . . 0.00 C53A -0.2143(7) -0.1793(20) 0.7110(11) 0.0662(60) iso C . . 0.00 C54A -0.1619(8) -0.1720(13) 0.6590(11) 0.0733(60) iso C . . 0.00 C51B -0.2618(15) -0.1605(21) 0.6991(21) 0.0704(96) iso C . . 0.00 C52B -0.1986(15) -0.1652(49) 0.7086(28) 0.106(19) iso C . . 0.00 C53B -0.1766(13) -0.1236(26) 0.6312(22) 0.0496(82) iso C . . 0.00 C54B -0.2256(10) -0.0742(26) 0.5916(17) 0.0540(96) iso C . . 0.00 C51C -0.1687(13) -0.1451(21) 0.6845(17) 0.0544(86) iso C . . 0.00 C52C -0.1706(10) -0.1366(24) 0.5945(17) 0.0400(70) iso C . . 0.00 C53C -0.2318(10) -0.1348(23) 0.5708(18) 0.0486(92) iso C . . 0.00 C54C -0.2544(10) -0.1974(22) 0.6363(15) 0.0492(71) iso C . . 0.00 H2 -0.16630(0) 0.39910(0) 0.43150(0) 0.0500(0) iso H . C3 1.00 H3 -0.11350(0) 0.40620(0) 0.53420(0) 0.0500(0) iso H . C2 1.00 H4 -0.20060(0) 0.26650(0) 0.39200(0) 0.0500(0) iso H . C4 1.00 H5 -0.15510(0) 0.12800(0) 0.43400(0) 0.0500(0) iso H . C5 1.00 H7 -0.09020(0) 0.03630(0) 0.50500(0) 0.0500(0) iso H . C7 1.00 H9 -0.06550(0) -0.09230(0) 0.55040(0) 0.0500(0) iso H . C9 1.00 H10 -0.01220(0) -0.21060(0) 0.59740(0) 0.0500(0) iso H . C10 1.00 H11 0.06210(0) -0.19650(0) 0.68400(0) 0.0500(0) iso H . C11 1.00 H12 0.08060(0) -0.04680(0) 0.73360(0) 0.0500(0) iso H . C12 1.00 H14 0.06600(0) 0.12560(0) 0.58730(0) 0.0500(0) iso H . C14 1.00 H16 0.15700(0) 0.07220(0) 0.55990(0) 0.0500(0) iso H . C16 1.00 H17 0.23870(0) 0.01860(0) 0.58590(0) 0.0500(0) iso H . C17 1.00 H18 0.26810(0) 0.05660(0) 0.72880(0) 0.0500(0) iso H . C18 1.00 H19 0.21500(0) 0.10850(0) 0.80920(0) 0.0500(0) iso H . C19 1.00 H32 0.18380(0) 0.29260(0) 0.62170(0) 0.0500(0) iso H . C32 1.00 H33 0.22860(0) 0.36770(0) 0.52470(0) 0.0500(0) iso H . C33 1.00 H34 0.17680(0) 0.42360(0) 0.41290(0) 0.0500(0) iso H . C34 1.00 H35 0.08340(0) 0.40460(0) 0.40760(0) 0.0500(0) iso H . C35 1.00 H36 0.03830(0) 0.31750(0) 0.51190(0) 0.0500(0) iso H . C36 1.00 H42 -0.00120(0) 0.43650(0) 0.62260(0) 0.0500(0) iso H . C42 1.00 H43 0.01860(0) 0.59300(0) 0.63110(0) 0.0500(0) iso H . C43 1.00 H44 0.08440(0) 0.64060(0) 0.71340(0) 0.0500(0) iso H . C44 1.00 H45 0.13920(0) 0.55250(0) 0.79050(0) 0.0500(0) iso H . C45 1.00 H46 0.11290(0) 0.38670(0) 0.78700(0) 0.0500(0) iso H . C46 1.00 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 #label U11 U22 U33 U23 U13 U12 MO1 0.0141(2) 0.0132(2) 0.0170(2) -0.0005(2) -0.0012(2) 0.0005(2) O1 0.0214(17) 0.0180(19) 0.0213(19) 0.0016(14) -0.0055(14) 0.0002(14) O2 0.0178(16) 0.0254(18) 0.0230(19) 0.0001(15) -0.0017(15) 0.0019(14) N1 0.0171(22) 0.0213(21) 0.0202(22) -0.0037(18) -0.0004(16) -0.0022(17) N2 0.0178(18) 0.0092(17) 0.0220(20) 0.0006(16) 0.0015(20) 0.0028(16) C1 0.0171(24) 0.0284(29) 0.0199(27) -0.0002(22) -0.0018(20) 0.0036(21) C2 0.0275(29) 0.0367(35) 0.0289(32) 0.0046(26) -0.0055(26) 0.0081(26) C3 0.0269(30) 0.0509(42) 0.0340(35) 0.0151(31) -0.0046(27) 0.0109(29) C4 0.0261(30) 0.0595(43) 0.0279(32) 0.0022(30) -0.0099(25) 0.0038(30) C5 0.0218(27) 0.0461(39) 0.0270(30) -0.0088(28) -0.0082(23) 0.0018(26) C6 0.0195(24) 0.0371(32) 0.0181(25) -0.0033(24) 0.0006(21) -0.0005(25) C7 0.0253(26) 0.0257(29) 0.0220(28) -0.0028(23) 0.0008(22) -0.0007(23) C8 0.0197(23) 0.0188(25) 0.0218(26) -0.0029(21) 0.0026(21) -0.0012(20) C9 0.0317(28) 0.0256(27) 0.0328(29) -0.0070(24) 0.0029(26) -0.0054(26) C10 0.0445(35) 0.0204(27) 0.0417(37) -0.0102(27) 0.0066(30) -0.0034(26) C11 0.0376(32) 0.0182(27) 0.0446(35) -0.0010(25) 0.0110(31) 0.0022(25) C12 0.0231(24) 0.0182(24) 0.0327(29) -0.0001(25) 0.0037(25) 0.0013(20) C13 0.0222(24) 0.0124(23) 0.0195(25) -0.0041(19) 0.0022(20) -0.0017(19) C14 0.0189(24) 0.0139(23) 0.0198(27) 0.0005(20) 0.0023(21) -0.0015(20) C15 0.0129(23) 0.0143(24) 0.0329(30) 0.0038(21) -0.0016(21) -0.0016(19) C16 0.0186(25) 0.0266(30) 0.0328(31) -0.0069(25) 0.0052(23) 0.0017(21) C17 0.0257(29) 0.0316(33) 0.0478(38) -0.0070(29) 0.0090(28) 0.0051(25) C18 0.0185(28) 0.0488(39) 0.0583(44) 0.0048(36) -0.0011(27) 0.0079(27) C19 0.0247(28) 0.0410(35) 0.0380(35) 0.0035(30) -0.0077(26) -0.0005(27) C20 0.0159(24) 0.0181(25) 0.0335(31) 0.0023(23) 0.0014(23) 0.0022(20) C21 0.0144(22) 0.0126(24) 0.0254(28) 0.0012(20) -0.0029(20) -0.0017(19) C22 0.0182(23) 0.0149(23) 0.0265(25) 0.0026(23) 0.0006(20) -0.0020(18) C31 0.0282(26) 0.0133(21) 0.0210(25) -0.0015(22) 0.0023(20) -0.0035(22) C32 0.0280(28) 0.0287(32) 0.0339(32) 0.0052(26) -0.0049(24) -0.0115(25) C33 0.0317(32) 0.0401(37) 0.0389(37) 0.0029(29) 0.0055(29) -0.0110(28) C34 0.0369(34) 0.0452(40) 0.0359(35) 0.0094(31) 0.0109(28) -0.0101(30) C35 0.0380(35) 0.0497(41) 0.0297(34) 0.0140(30) -0.0035(28) -0.0019(31) C36 0.0231(27) 0.0372(32) 0.0273(31) 0.0053(25) 0.0014(23) -0.0003(25) C41 0.0232(24) 0.0161(24) 0.0242(28) -0.0014(22) 0.0068(21) -0.0040(19) C42 0.0242(28) 0.0189(25) 0.0268(28) 0.0031(21) 0.0066(22) -0.0008(21) C43 0.0326(29) 0.0200(26) 0.0398(32) 0.0066(24) 0.0058(28) 0.0048(25) C44 0.0459(35) 0.0183(27) 0.0471(40) -0.0033(27) 0.0183(30) -0.0078(26) C45 0.0243(26) 0.0278(29) 0.0335(31) -0.0082(25) 0.0073(24) -0.0134(23) C46 0.0217(25) 0.0198(25) 0.0272(28) -0.0009(22) 0.0042(21) -0.0032(21) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MO1 MO1` 2.5440(5) yes MO1 O1 2.007(3) yes MO1 O2` 2.003(3) yes MO1 N1 2.220(4) yes MO1 N2 2.114(4) yes MO1 N2` 2.176(3) yes MO1 C22 2.528(5) yes MO1 C22` 2.226(5) yes MO1` O2 2.003(3) yes MO1` N2 2.176(3) yes MO1` N2` 2.114(4) yes MO1` C22 2.226(5) yes MO1` C22` 2.528(5) yes O1 C1 1.320(6) yes O2 C20 1.336(6) yes O3A C51A 1.41(1) yes O3A C54A 1.43(2) yes O3B C51B 1.42(3) yes O3B C54B 1.42(3) yes O3C C51C 1.43(3) yes O3C C54C 1.43(3) yes N1 C7 1.295(6) yes N1 C8 1.407(7) yes N2 C13 1.441(5) yes N2 C14 1.494(6) yes C1 C2 1.396(8) yes C1 C6 1.412(8) yes C2 C3 1.362(9) yes C3 C4 1.40(1) yes C4 C5 1.37(1) yes C5 C6 1.410(7) yes C6 C7 1.434(8) yes C8 C9 1.407(8) yes C8 C13 1.391(7) yes C9 C10 1.380(9) yes C10 C11 1.39(1) yes C11 C12 1.385(8) yes C12 C13 1.401(7) yes C14 C15 1.503(7) yes C14 C21 1.502(6) yes C15 C16 1.383(7) yes C15 C20 1.400(7) yes C16 C17 1.382(7) yes C17 C18 1.38(0) yes C18 C19 1.373(9) yes C19 C20 1.392(7) yes C21 C22 1.354(7) yes C21 C31 1.483(7) yes C22 C41 1.503(6) yes C31 C32 1.390(7) yes C31 C36 1.390(8) yes C32 C33 1.380(9) yes C33 C34 1.38(1) yes C34 C35 1.38(1) yes C35 C36 1.384(9) yes C41 C42 1.387(7) yes C41 C46 1.387(7) yes C42 C43 1.393(8) yes C43 C44 1.38(1) yes C44 C45 1.374(8) yes C45 C46 1.385(8) yes C51A C52A 1.53(2) yes C52A C53A 1.53(2) yes C53A C54A 1.55(2) yes C51B C52B 1.54(5) yes C52B C53B 1.54(6) yes C53B C54B 1.54(4) yes C51C C52C 1.54(4) yes C52C C53C 1.53(3) yes C53C C54C 1.54(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C22 MO1 C22` 74.9(2) yes N2` MO1 C22` 72.0(2) yes N2` MO1 C22 104.6(2) yes N2 MO1 C22` 118.3(2) yes N2 MO1 C22 67.1(1) yes N2 MO1 N2` 73.0(1) yes N1 MO1 C22` 165.6(2) yes N1 MO1 C22 119.3(2) yes N1 MO1 N2` 104.9(1) yes N1 MO1 N2 72.8(2) yes O2` MO1 C22` 87.2(2) yes O2` MO1 C22 156.9(1) yes O2` MO1 N2` 83.0(1) yes O2` MO1 N2 135.6(1) yes O2` MO1 N1 78.4(1) yes O1 MO1 C22` 97.9(1) yes O1 MO1 C22 82.3(1) yes O1 MO1 N2` 165.3(1) yes O1 MO1 N2 121.7(1) yes O1 MO1 N1 82.2(1) yes O1 MO1 O2` 85.9(1) yes MO1` MO1 C22` 63.6(1) yes MO1` MO1 C22 52.1(1) yes MO1` MO1 N2` 52.5(1) yes MO1` MO1 N2 54.8(1) yes MO1` MO1 N1 126.3(1) yes MO1` MO1 O2` 131.6(1) yes MO1` MO1 O1 133.1(1) yes MO1 MO1` C22` 52.1(1) yes MO1 MO1` C22 63.6(1) yes MO1 MO1` N2` 54.8(1) yes MO1 MO1` N2 52.5(1) yes MO1 MO1` O2 131.6(1) yes C22 MO1` C22` 74.9(2) yes N2` MO1` C22` 67.1(1) yes N2` MO1` C22 118.3(2) yes N2 MO1` C22` 104.6(2) yes N2 MO1` C22 72.0(2) yes N2 MO1` N2` 73.0(1) yes O2 MO1` C22` 156.9(1) yes O2 MO1` C22 87.2(2) yes O2 MO1` N2` 135.6(1) yes O2 MO1` N2 83.0(1) yes MO1 O1 C1 129.2(3) yes MO1` O2 C20 133.9(3) yes C51A O3A C54A 109(1) yes C51B O3B C54B 114(2) yes C51C O3C C54C 111(2) yes MO1 N1 C8 110.9(3) yes MO1 N1 C7 125.6(4) yes C7 N1 C8 123.0(4) yes MO1 N2 MO1` 72.7(1) yes MO1` N2 C14 110.2(3) yes MO1` N2 C13 136.3(3) yes MO1 N2 C14 114.7(3) yes MO1 N2 C13 111.1(3) yes C13 N2 C14 107.0(3) yes MO1 N2` MO1` 72.7(1) yes O1 C1 C6 123.9(5) yes O1 C1 C2 117.7(5) yes C2 C1 C6 118.2(5) yes C1 C2 C3 122.4(6) yes C2 C3 C4 119.7(6) yes C3 C4 C5 119.4(5) yes C4 C5 C6 121.3(6) yes C1 C6 C5 118.8(5) yes C5 C6 C7 117.4(5) yes C1 C6 C7 123.6(5) yes N1 C7 C6 124.0(5) yes N1 C8 C13 113.5(5) yes N1 C8 C9 126.7(5) yes C9 C8 C13 119.8(5) yes C8 C9 C10 118.7(5) yes C9 C10 C11 121.4(5) yes C10 C11 C12 120.5(6) yes C11 C12 C13 118.7(5) yes C8 C13 C12 120.9(5) yes N2 C13 C12 123.5(4) yes N2 C13 C8 115.4(4) yes N2 C14 C21 106.6(4) yes N2 C14 C15 110.2(4) yes C15 C14 C21 109.9(4) yes C14 C15 C20 119.5(4) yes C14 C15 C16 121.2(4) yes C16 C15 C20 119.3(4) yes C15 C16 C17 122.0(5) yes C16 C17 C18 118.5(5) yes C17 C18 C19 120.5(5) yes C18 C19 C20 121.6(6) yes C15 C20 C19 118.2(5) yes O2 C20 C19 118.9(5) yes O2 C20 C15 122.9(4) yes C14 C21 C31 116.1(4) yes C14 C21 C22 117.2(4) yes C22 C21 C31 126.5(4) yes MO1` C22 C21 113.1(3) yes MO1 C22 C21 97.7(3) yes MO1 C22 MO1` 64.3(1) yes C21 C22 C41 114.8(4) yes MO1` C22 C41 125.8(3) yes MO1 C22 C41 130.0(3) yes MO1 C22` MO1` 64.3(1) yes C21 C31 C36 120.1(4) yes C21 C31 C32 121.2(5) yes C32 C31 C36 118.7(5) yes C31 C32 C33 121.1(5) yes C32 C33 C34 119.4(6) yes C33 C34 C35 120.5(6) yes C34 C35 C36 120.0(6) yes C31 C36 C35 120.3(5) yes C22 C41 C46 118.0(4) yes C22 C41 C42 122.8(4) yes C42 C41 C46 118.9(4) yes C41 C42 C43 119.9(5) yes C42 C43 C44 120.4(5) yes C43 C44 C45 120.0(6) yes C44 C45 C46 119.8(5) yes C41 C46 C45 120.9(5) yes O3A C51A C52A 108(1) yes C51A C52A C53A 104(1) yes C52A C53A C54A 103(1) yes O3A C54A C53A 104(1) yes O3B C51B C52B 103(3) yes C51B C52B C53B 104(3) yes C52B C53B C54B 107(3) yes O3B C54B C53B 104(2) yes O3C C51C C52C 95(2) yes C51C C52C C53C 107(2) yes C52C C53C C54C 98(2) yes O3C C54C C53C 107(2) yes _refine_diff_density_max 0.464 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.106