# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1209 data_global #======================================================================= # 1. SUBMISSION DETAILS _publ_contact_author ; Gotthelf Wolmersh\"auser Fachbereich Chemie Universit\"at Kaiserslautern Erwin-Schr\"odinger-Str. 67663 Kaiserslautern Deutschland ; _publ_contact_author_phone '0631 205 2468' _publ_contact_author_fax '0631 205 2187' _publ_contact_author_email wolmersh@chemie.uni-kl.de _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ? #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Superamidines 1. Synthesis of some very bulky N,N'-disubstituted amidines and initial studies of their coordination chemistry ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Rene T. Boere' ; Department of Chemistry University of Lethbridge Lethbridge Alberta T1K 3M4 Canada ; 'Vicki Klassen' ; Department of Chemistry University of Lethbridge Lethbridge Alberta T1K 3M4 Canada ; 'Wolmersh\"auser, Gotthelf' ; Fachbereich Chemie Universit\"at Kaiserslautern Erwin-Schr\"odinger-Str. 67663 Kaiserslautern Deutschland ; #======================================================================= # 4. RESULTS data_9619 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 N2' _chemical_formula_weight 378.58 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.9260(10) _cell_length_b 20.1330(10) _cell_length_c 16.671(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5009.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 10.498 _cell_measurement_theta_max 21.136 _exptl_crystal_description 'transparent prisms' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.058 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9717 _exptl_absorpt_correction_T_max 0.9829 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method 'Phi oscillation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8778 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max -1 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4945 _reflns_number_gt 2679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.028(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(3) _refine_ls_number_reflns 4945 _refine_ls_number_parameters 406 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.808 _refine_ls_shift/su_max 0.753 _refine_ls_shift/su_mean 0.065 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.48703(11) 0.24030(8) 0.14388(10) 0.0718(4) Uani 1 d . . . N2 N 0.38110(11) 0.20448(9) 0.23124(10) 0.0713(4) Uani 1 d D . . H3 H 0.426(4) 0.208(4) 0.272(3) 0.25(3) Uiso 1 d D . . C1 C 0.40303(13) 0.22286(10) 0.15686(12) 0.0694(5) Uani 1 d . . . C2 C 0.33509(19) 0.22386(19) 0.09124(16) 0.0936(8) Uani 1 d . . . H2A H 0.280(3) 0.238(2) 0.103(2) 0.145(14) Uiso 1 d . . . H2B H 0.323(4) 0.176(3) 0.072(4) 0.194(19) Uiso 1 d . . . H2C H 0.360(3) 0.244(2) 0.040(3) 0.148(12) Uiso 1 d . . . C9 C 0.51641(14) 0.26380(12) 0.06739(12) 0.0783(6) Uani 1 d . . . C10 C 0.55280(16) 0.21905(17) 0.01222(15) 0.0958(8) Uani 1 d . . . C11 C 0.5607(2) 0.1464(2) 0.0291(3) 0.1239(11) Uani 1 d . . . H11 H 0.5381(19) 0.1348(15) 0.073(2) 0.099(9) Uiso 1 d . . . C12 C 0.5023(5) 0.1042(4) -0.0268(8) 0.207(4) Uani 1 d . . . H12A H 0.511(5) 0.053(4) -0.016(5) 0.24(3) Uiso 1 d . . . H12B H 0.533(4) 0.114(3) -0.077(4) 0.18(3) Uiso 1 d . . . H12C H 0.435(4) 0.126(3) -0.011(4) 0.21(2) Uiso 1 d . . . C13 C 0.6564(4) 0.1219(4) 0.0263(5) 0.1557(18) Uani 1 d . . . H13A H 0.676(5) 0.115(4) -0.023(5) 0.23(3) Uiso 1 d . . . H13B H 0.658(4) 0.080(3) 0.058(4) 0.20(3) Uiso 1 d . . . H13C H 0.698(3) 0.152(2) 0.055(3) 0.157(15) Uiso 1 d . . . C14 C 0.5831(2) 0.2450(3) -0.06150(19) 0.1235(12) Uani 1 d . . . H14 H 0.601(3) 0.199(3) -0.106(3) 0.180(16) Uiso 1 d . . . C15 C 0.5787(2) 0.3114(3) -0.0779(2) 0.1332(15) Uani 1 d . . . H15 H 0.595(2) 0.3349(19) -0.130(3) 0.140(11) Uiso 1 d . . . C16 C 0.5449(2) 0.3531(3) -0.0237(3) 0.1252(14) Uani 1 d . . . H16 H 0.537(2) 0.394(2) -0.034(3) 0.141(15) Uiso 1 d . . . C17 C 0.51283(18) 0.33213(15) 0.05038(15) 0.0975(8) Uani 1 d . . . C18 C 0.4752(3) 0.38184(17) 0.1100(3) 0.1254(11) Uani 1 d . . . H18 H 0.471(3) 0.358(3) 0.157(4) 0.21(2) Uiso 1 d . . . C19 C 0.5445(5) 0.4338(3) 0.1354(5) 0.183(2) Uani 1 d . . . H19A H 0.508(5) 0.466(3) 0.194(4) 0.23(2) Uiso 1 d . . . H19B H 0.571(5) 0.452(3) 0.085(5) 0.22(3) Uiso 1 d . . . H19C H 0.595(4) 0.407(3) 0.181(4) 0.21(2) Uiso 1 d . . . C20 C 0.3926(5) 0.4172(4) 0.0771(6) 0.203(3) Uani 1 d . . . H20A H 0.348(3) 0.460(3) 0.117(3) 0.190(17) Uiso 1 d . . . H20B H 0.351(4) 0.388(3) 0.058(3) 0.165(17) Uiso 1 d . . . H20C H 0.431(9) 0.467(8) 0.019(12) 0.45(8) Uiso 1 d . . . C21 C 0.29478(14) 0.17989(11) 0.25197(13) 0.0767(5) Uani 1 d . . . C22 C 0.23453(16) 0.22153(15) 0.29160(14) 0.0906(7) Uani 1 d . . . C23 C 0.2593(3) 0.29356(17) 0.30889(16) 0.1076(9) Uani 1 d . . . H23 H 0.325(3) 0.302(2) 0.306(3) 0.152(14) Uiso 1 d . . . C24 C 0.2212(6) 0.3404(3) 0.2486(3) 0.178(3) Uani 1 d . . . H24A H 0.237(5) 0.322(4) 0.190(6) 0.28(4) Uiso 1 d . . . H24B H 0.257(5) 0.391(6) 0.267(6) 0.29(3) Uiso 1 d . . . H24C H 0.152(2) 0.3350(15) 0.2652(19) 0.100(9) Uiso 1 d . . . C25 C 0.2408(4) 0.3163(3) 0.3939(2) 0.1404(16) Uani 1 d . . . H25A H 0.255(5) 0.282(4) 0.436(5) 0.25(3) Uiso 1 d . . . H25B H 0.179(4) 0.317(3) 0.398(3) 0.180(19) Uiso 1 d . . . H25C H 0.259(2) 0.370(2) 0.413(3) 0.142(12) Uiso 1 d . . . C26 C 0.1522(2) 0.1945(3) 0.3157(2) 0.1222(12) Uani 1 d . . . H26 H 0.115(3) 0.2194(19) 0.344(2) 0.131(11) Uiso 1 d . . . C27 C 0.1305(2) 0.1304(3) 0.2995(2) 0.1279(12) Uani 1 d . . . H27 H 0.073(3) 0.1046(18) 0.316(2) 0.132(10) Uiso 1 d . . . C28 C 0.1888(2) 0.0907(2) 0.2609(3) 0.1242(11) Uani 1 d . . . H28 H 0.175(3) 0.043(3) 0.261(3) 0.177(16) Uiso 1 d . . . C29 C 0.27314(16) 0.11391(14) 0.23658(19) 0.0985(7) Uani 1 d . . . C30 C 0.3378(2) 0.06686(16) 0.1967(3) 0.1315(12) Uani 1 d . . . H30 H 0.389(2) 0.0990(19) 0.172(2) 0.134(11) Uiso 1 d . . . C31 C 0.2980(5) 0.0278(3) 0.1285(5) 0.181(2) Uani 1 d . . . H31A H 0.362(4) -0.006(3) 0.092(4) 0.22(2) Uiso 1 d . . . H31B H 0.280(3) 0.059(2) 0.088(3) 0.130(14) Uiso 1 d . . . H31C H 0.249(3) -0.002(3) 0.153(3) 0.156(14) Uiso 1 d . . . C32 C 0.3752(4) 0.0176(3) 0.2621(6) 0.188(3) Uani 1 d . . . H32A H 0.417(6) -0.013(4) 0.221(5) 0.27(3) Uiso 1 d . . . H32B H 0.322(5) -0.015(4) 0.270(5) 0.26(3) Uiso 1 d . . . H32C H 0.417(5) 0.056(4) 0.292(5) 0.25(3) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0671(9) 0.0838(10) 0.0645(9) 0.0067(7) 0.0009(7) -0.0108(7) N2 0.0682(9) 0.0781(10) 0.0677(9) 0.0009(8) 0.0036(7) -0.0080(7) C1 0.0688(12) 0.0727(11) 0.0669(11) -0.0011(9) -0.0040(8) -0.0098(8) C2 0.0705(14) 0.134(2) 0.0761(14) 0.0041(14) -0.0102(11) -0.0155(15) C9 0.0671(11) 0.1022(15) 0.0657(11) 0.0102(10) -0.0040(9) -0.0148(10) C10 0.0756(13) 0.134(2) 0.0781(14) -0.0058(14) 0.0065(10) -0.0117(13) C11 0.119(3) 0.133(3) 0.120(2) -0.024(2) 0.031(2) -0.0007(19) C12 0.142(4) 0.155(5) 0.325(12) -0.054(6) -0.043(7) -0.002(4) C13 0.129(3) 0.178(5) 0.160(4) -0.033(4) -0.017(3) 0.031(3) C14 0.0890(18) 0.203(4) 0.0783(15) -0.005(2) 0.0097(12) -0.018(2) C15 0.095(2) 0.217(5) 0.088(2) 0.046(3) -0.0013(16) -0.028(2) C16 0.101(2) 0.163(4) 0.112(3) 0.064(3) -0.0074(19) -0.022(2) C17 0.0898(16) 0.1126(19) 0.0901(15) 0.0285(14) -0.0054(12) -0.0180(14) C18 0.144(3) 0.0915(19) 0.141(3) 0.0235(19) 0.007(2) -0.0077(17) C19 0.207(5) 0.150(4) 0.191(6) -0.018(4) -0.030(5) -0.048(4) C20 0.146(4) 0.150(4) 0.314(10) -0.025(5) -0.038(5) 0.029(3) C21 0.0684(12) 0.0851(14) 0.0765(12) 0.0090(10) 0.0053(10) -0.0035(10) C22 0.0876(15) 0.111(2) 0.0730(13) 0.0137(12) 0.0120(11) 0.0142(13) C23 0.128(2) 0.110(2) 0.0843(15) -0.0107(14) 0.0123(14) 0.0295(18) C24 0.286(9) 0.121(3) 0.125(3) 0.001(3) -0.041(4) 0.050(4) C25 0.138(3) 0.191(5) 0.092(2) -0.027(2) 0.0008(18) 0.041(3) C26 0.0872(19) 0.175(4) 0.104(2) 0.028(2) 0.0268(16) 0.024(2) C27 0.0836(19) 0.175(4) 0.125(2) 0.029(3) 0.0181(17) -0.023(2) C28 0.095(2) 0.129(3) 0.149(3) 0.027(2) 0.008(2) -0.0343(19) C29 0.0811(14) 0.0913(17) 0.1232(19) 0.0098(15) 0.0121(14) -0.0172(12) C30 0.107(2) 0.0812(18) 0.206(4) -0.020(2) 0.019(2) -0.0145(16) C31 0.201(5) 0.123(4) 0.218(6) -0.038(4) 0.016(5) -0.029(4) C32 0.139(3) 0.124(3) 0.300(8) -0.026(4) -0.028(5) 0.012(3) _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 N1 C1 1.320(2) . ? N1 C9 1.429(3) . ? N2 C1 1.335(3) . ? N2 C21 1.423(3) . ? C1 C2 1.492(3) . ? C9 C10 1.397(4) . ? C9 C17 1.406(4) . ? C10 C14 1.410(5) . ? C10 C11 1.493(5) . ? C11 C13 1.512(6) . ? C11 C12 1.534(8) . ? C14 C15 1.366(6) . ? C15 C16 1.333(7) . ? C16 C17 1.391(5) . ? C17 C18 1.518(5) . ? C18 C20 1.525(7) . ? C18 C19 1.532(6) . ? C21 C22 1.396(3) . ? C21 C29 1.391(4) . ? C22 C26 1.403(5) . ? C22 C23 1.524(5) . ? C23 C24 1.491(5) . ? C23 C25 1.515(4) . ? C26 C27 1.358(6) . ? C27 C28 1.345(6) . ? C28 C29 1.403(4) . ? C29 C30 1.508(5) . ? C30 C31 1.503(8) . ? C30 C32 1.577(9) . ? 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 C1 N1 C9 121.72(16) . . ? C1 N2 C21 122.96(17) . . ? N1 C1 N2 117.32(17) . . ? N1 C1 C2 121.46(19) . . ? N2 C1 C2 121.22(19) . . ? C10 C9 C17 120.9(2) . . ? C10 C9 N1 119.6(2) . . ? C17 C9 N1 119.5(2) . . ? C14 C10 C9 117.4(3) . . ? C14 C10 C11 120.1(3) . . ? C9 C10 C11 122.5(2) . . ? C10 C11 C13 112.9(4) . . ? C10 C11 C12 112.5(5) . . ? C13 C11 C12 109.7(5) . . ? C15 C14 C10 121.4(4) . . ? C16 C15 C14 120.0(3) . . ? C15 C16 C17 122.7(5) . . ? C16 C17 C9 117.6(4) . . ? C16 C17 C18 120.5(4) . . ? C9 C17 C18 121.8(2) . . ? C17 C18 C20 111.8(5) . . ? C17 C18 C19 112.4(4) . . ? C20 C18 C19 109.1(5) . . ? C22 C21 C29 120.7(2) . . ? C22 C21 N2 119.3(2) . . ? C29 C21 N2 119.8(2) . . ? C26 C22 C21 117.8(3) . . ? C26 C22 C23 121.9(3) . . ? C21 C22 C23 120.3(2) . . ? C24 C23 C25 111.7(4) . . ? C24 C23 C22 112.4(4) . . ? C25 C23 C22 114.8(4) . . ? C27 C26 C22 121.3(4) . . ? C28 C27 C26 120.4(3) . . ? C27 C28 C29 121.4(4) . . ? C28 C29 C21 118.2(3) . . ? C28 C29 C30 119.5(3) . . ? C21 C29 C30 122.2(2) . . ? C29 C30 C31 114.1(4) . . ? C29 C30 C32 108.4(4) . . ? C31 C30 C32 109.5(5) . . ? _diffrn_measured_fraction_theta_max 0.441 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.441 _refine_diff_density_max 0.079 _refine_diff_density_min -0.067 _refine_diff_density_rms 0.018 # ==== END data_9620 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H42 N2 O' _chemical_formula_weight 470.68 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.269(2) _cell_length_b 10.1220(10) _cell_length_c 17.899(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.717(9) _cell_angle_gamma 90.00 _cell_volume 2930.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 26 _exptl_crystal_description 'transparent blocks' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9750 _exptl_absorpt_correction_T_max 0.9812 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method 'Phi oscillation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20572 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5646 _reflns_number_gt 4212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+0.1669P] 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 5646 _refine_ls_number_parameters 484 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1728 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.179 _refine_ls_shift/su_mean 0.018 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.75028(8) 0.33052(11) 0.24685(7) 0.0591(3) Uani 1 d D . . H1 H 0.7687(11) 0.4051(16) 0.2795(12) 0.083(5) Uiso 1 d D . . N2 N 0.75913(8) 0.45085(11) 0.14047(7) 0.0576(3) Uani 1 d . . . O1 O 0.70437(13) -0.08741(18) -0.05017(12) 0.1257(6) Uani 1 d . . . C1 C 0.74676(8) 0.33894(13) 0.16923(8) 0.0517(3) Uani 1 d . . . C2 C 0.73187(8) 0.22025(13) 0.11489(8) 0.0534(3) Uani 1 d . . . C3 C 0.68433(11) 0.23361(18) 0.02722(10) 0.0677(4) Uani 1 d . . . H3 H 0.6539(12) 0.319(2) 0.0014(12) 0.084(5) Uiso 1 d . . . C4 C 0.67518(13) 0.1284(2) -0.02576(12) 0.0838(5) Uani 1 d . . . H4 H 0.6399(14) 0.139(2) -0.0901(16) 0.102(6) Uiso 1 d . . . C5 C 0.71372(13) 0.00923(19) 0.00718(12) 0.0815(5) Uani 1 d . . . C6 C 0.7580(4) -0.1981(3) -0.0216(3) 0.1554(16) Uani 1 d . . . H6A H 0.814(3) -0.162(5) 0.004(3) 0.21(2) Uiso 1 d . . . H6B H 0.744(2) -0.253(3) -0.075(2) 0.161(11) Uiso 1 d . . . H6C H 0.754(2) -0.256(4) 0.026(3) 0.172(13) Uiso 1 d . . . C7 C 0.75944(12) -0.00692(17) 0.09404(13) 0.0766(5) Uani 1 d . . . H7 H 0.7832(13) -0.093(2) 0.1174(14) 0.096(6) Uiso 1 d . . . C8 C 0.76818(10) 0.09874(15) 0.14727(11) 0.0638(4) Uani 1 d . . . H8 H 0.8006(11) 0.0862(18) 0.2081(13) 0.076(5) Uiso 1 d . . . C9 C 0.73222(10) 0.22365(13) 0.28786(9) 0.0581(4) Uani 1 d . . . C10 C 0.79499(11) 0.18787(16) 0.36850(9) 0.0713(4) Uani 1 d . . . C11 C 0.87777(14) 0.2572(3) 0.40639(12) 0.0930(6) Uani 1 d . . . H11 H 0.8924(14) 0.281(2) 0.3625(16) 0.100(7) Uiso 1 d . . . C12 C 0.8736(2) 0.3915(4) 0.4459(2) 0.1244(10) Uani 1 d . . . H12A H 0.825(3) 0.454(4) 0.400(3) 0.191(16) Uiso 1 d . . . H12B H 0.926(2) 0.434(3) 0.469(2) 0.155(12) Uiso 1 d . . . H12C H 0.8682(17) 0.359(3) 0.496(2) 0.123(9) Uiso 1 d . . . C13 C 0.9491(3) 0.1688(6) 0.4680(2) 0.1494(15) Uani 1 d . . . H13A H 0.940(2) 0.164(4) 0.517(3) 0.179(15) Uiso 1 d . . . H13B H 0.999(2) 0.219(3) 0.483(2) 0.128(10) Uiso 1 d . . . H13C H 0.958(3) 0.051(6) 0.432(4) 0.25(2) Uiso 1 d . . . C14 C 0.77545(19) 0.0898(2) 0.41280(13) 0.0958(7) Uani 1 d . . . H14 H 0.8202(15) 0.067(2) 0.4671(17) 0.110(7) Uiso 1 d . . . C15 C 0.69822(19) 0.0314(2) 0.37856(16) 0.0976(7) Uani 1 d . . . H15 H 0.6836(14) -0.037(2) 0.4123(15) 0.108(7) Uiso 1 d . . . C16 C 0.63935(16) 0.06735(17) 0.30051(14) 0.0843(5) Uani 1 d . . . H16 H 0.5837(16) 0.016(3) 0.2770(16) 0.118(8) Uiso 1 d . . . C17 C 0.65330(11) 0.16456(14) 0.25294(10) 0.0652(4) Uani 1 d . . . C18 C 0.58174(11) 0.20664(17) 0.16984(12) 0.0729(4) Uani 1 d . . . H18 H 0.6048(10) 0.2657(16) 0.1420(10) 0.063(4) Uiso 1 d . . . C19 C 0.5439(2) 0.0893(3) 0.1083(2) 0.1141(8) Uani 1 d . . . H19A H 0.591(2) 0.024(4) 0.109(2) 0.153(11) Uiso 1 d . . . H19B H 0.494(3) 0.125(4) 0.046(3) 0.186(14) Uiso 1 d . . . H19C H 0.5206(18) 0.048(3) 0.1365(19) 0.122(10) Uiso 1 d . . . C20 C 0.5179(2) 0.2850(4) 0.1852(2) 0.1197(10) Uani 1 d . . . H20A H 0.492(2) 0.229(3) 0.212(2) 0.146(10) Uiso 1 d . . . H20B H 0.472(2) 0.321(3) 0.129(2) 0.158(11) Uiso 1 d . . . H20C H 0.545(2) 0.360(4) 0.228(2) 0.158(14) Uiso 1 d . . . C21 C 0.78085(10) 0.56540(13) 0.19283(9) 0.0606(4) Uani 1 d . . . C22 C 0.71913(12) 0.64466(15) 0.19619(11) 0.0732(4) Uani 1 d . . . C23 C 0.62908(14) 0.6085(2) 0.14442(16) 0.0896(6) Uani 1 d . . . H23 H 0.6236(13) 0.521(2) 0.1423(13) 0.094(6) Uiso 1 d . . . C24 C 0.5736(3) 0.6584(4) 0.1815(4) 0.1613(16) Uani 1 d . . . H24A H 0.604(2) 0.578(4) 0.240(2) 0.165(12) Uiso 1 d . . . H24B H 0.506(2) 0.611(3) 0.141(2) 0.154(11) Uiso 1 d . . . H24C H 0.569(4) 0.769(7) 0.174(4) 0.29(3) Uiso 1 d . . . C25 C 0.5973(3) 0.6510(6) 0.0527(3) 0.1524(14) Uani 1 d . . . H25A H 0.597(3) 0.758(6) 0.051(3) 0.208(19) Uiso 1 d . . . H25B H 0.538(3) 0.634(4) 0.016(3) 0.167(13) Uiso 1 d . . . H25C H 0.629(6) 0.650(9) 0.021(5) 0.34(4) Uiso 1 d . . . C26 C 0.7453(2) 0.75952(19) 0.24699(16) 0.0972(7) Uani 1 d . . . H26 H 0.6991(17) 0.817(3) 0.2459(17) 0.121(8) Uiso 1 d . . . C27 C 0.8273(2) 0.7923(2) 0.29156(16) 0.1060(8) Uani 1 d . . . H27 H 0.8475(17) 0.872(3) 0.3301(19) 0.132(8) Uiso 1 d . . . C28 C 0.88614(19) 0.7147(2) 0.28740(15) 0.0987(7) Uani 1 d . . . H28 H 0.949(2) 0.744(3) 0.321(2) 0.138(9) Uiso 1 d . . . C29 C 0.86508(12) 0.59958(17) 0.23859(11) 0.0768(5) Uani 1 d . . . C30 C 0.93103(13) 0.5140(3) 0.23317(15) 0.0960(6) Uani 1 d . . . H30 H 0.9159(17) 0.412(3) 0.2281(18) 0.130(9) Uiso 1 d . . . C31 C 0.9477(4) 0.5589(5) 0.1639(3) 0.1559(15) Uani 1 d . . . H31A H 0.900(3) 0.586(5) 0.109(3) 0.199(19) Uiso 1 d . . . H31B H 0.995(3) 0.513(5) 0.162(3) 0.196(15) Uiso 1 d . . . H31C H 0.9894(14) 0.634(3) 0.2022(16) 0.094(7) Uiso 1 d . . . C32 C 1.0099(2) 0.4980(7) 0.3172(3) 0.1515(14) Uani 1 d . . . H32A H 1.019(3) 0.607(7) 0.306(4) 0.23(2) Uiso 1 d . . . H32B H 1.043(4) 0.433(6) 0.298(4) 0.25(2) Uiso 1 d . . . H32C H 1.000(3) 0.475(5) 0.364(3) 0.191(17) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0816(8) 0.0502(6) 0.0523(6) -0.0009(5) 0.0368(6) -0.0028(5) N2 0.0725(7) 0.0522(6) 0.0575(6) 0.0004(5) 0.0381(6) -0.0010(5) O1 0.1721(16) 0.1051(12) 0.1297(13) -0.0677(10) 0.0952(13) -0.0445(11) C1 0.0549(7) 0.0539(7) 0.0509(7) 0.0007(5) 0.0284(5) 0.0032(5) C2 0.0583(7) 0.0550(7) 0.0557(7) -0.0042(5) 0.0338(6) -0.0042(6) C3 0.0760(9) 0.0739(10) 0.0571(8) -0.0029(7) 0.0342(7) -0.0040(8) C4 0.0980(13) 0.0934(13) 0.0615(10) -0.0198(9) 0.0384(9) -0.0225(10) C5 0.1013(12) 0.0751(11) 0.0901(12) -0.0337(9) 0.0630(10) -0.0300(10) C6 0.273(5) 0.0766(15) 0.197(4) -0.056(2) 0.177(4) -0.036(2) C7 0.0971(12) 0.0576(9) 0.0946(12) -0.0124(8) 0.0610(10) -0.0043(8) C8 0.0747(9) 0.0586(8) 0.0677(9) -0.0037(6) 0.0412(8) 0.0031(7) C9 0.0842(9) 0.0489(7) 0.0544(7) 0.0050(5) 0.0433(7) 0.0110(6) C10 0.0944(11) 0.0713(9) 0.0563(8) 0.0073(7) 0.0419(8) 0.0230(8) C11 0.0926(13) 0.1247(17) 0.0596(9) -0.0004(10) 0.0337(9) 0.0235(12) C12 0.113(2) 0.153(3) 0.1047(19) -0.050(2) 0.0483(17) -0.023(2) C13 0.104(2) 0.228(5) 0.100(2) 0.036(2) 0.0339(17) 0.049(3) C14 0.149(2) 0.0858(13) 0.0665(11) 0.0287(9) 0.0613(12) 0.0460(14) C15 0.156(2) 0.0667(10) 0.1064(15) 0.0224(10) 0.0919(16) 0.0139(12) C16 0.1255(16) 0.0577(9) 0.1024(14) 0.0096(9) 0.0805(13) 0.0017(10) C17 0.0892(10) 0.0510(7) 0.0758(9) 0.0020(6) 0.0555(8) 0.0028(7) C18 0.0745(10) 0.0704(9) 0.0842(11) 0.0048(8) 0.0457(9) -0.0003(8) C19 0.1088(18) 0.0972(17) 0.113(2) -0.0095(14) 0.0317(16) -0.0199(15) C20 0.1162(19) 0.143(2) 0.137(2) 0.042(2) 0.090(2) 0.0467(19) C21 0.0870(10) 0.0478(7) 0.0598(8) 0.0010(6) 0.0449(7) -0.0016(6) C22 0.1100(13) 0.0515(8) 0.0831(10) 0.0088(7) 0.0658(10) 0.0078(8) C23 0.0993(13) 0.0671(11) 0.1296(17) 0.0184(11) 0.0761(13) 0.0191(10) C24 0.162(3) 0.134(3) 0.260(5) -0.006(3) 0.159(4) 0.018(2) C25 0.112(2) 0.192(4) 0.134(3) 0.057(3) 0.041(2) 0.004(2) C26 0.165(2) 0.0551(9) 0.1104(15) 0.0025(10) 0.0971(17) 0.0124(12) C27 0.171(3) 0.0628(11) 0.1001(15) -0.0202(10) 0.0767(17) -0.0225(14) C28 0.1323(19) 0.0715(12) 0.0915(13) -0.0210(10) 0.0515(13) -0.0238(12) C29 0.0942(12) 0.0642(9) 0.0748(10) -0.0084(7) 0.0416(9) -0.0132(8) C30 0.0789(11) 0.0963(14) 0.1053(15) -0.0225(12) 0.0365(11) -0.0110(10) C31 0.192(4) 0.179(4) 0.138(3) -0.001(3) 0.111(3) 0.040(4) C32 0.105(2) 0.208(5) 0.130(3) 0.002(3) 0.0446(19) 0.015(2) _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 N1 C1 1.3633(17) . ? N1 C9 1.4294(17) . ? N2 C1 1.3066(17) . ? N2 C21 1.4262(17) . ? O1 C5 1.370(2) . ? O1 C6 1.418(5) . ? C1 C2 1.4890(18) . ? C2 C8 1.390(2) . ? C2 C3 1.403(2) . ? C3 C4 1.383(2) . ? C4 C5 1.383(3) . ? C5 C7 1.391(3) . ? C7 C8 1.391(2) . ? C9 C17 1.410(2) . ? C9 C10 1.411(2) . ? C10 C14 1.416(3) . ? C10 C11 1.512(3) . ? C11 C13 1.543(4) . ? C11 C12 1.552(4) . ? C14 C15 1.383(4) . ? C15 C16 1.358(3) . ? C16 C17 1.400(2) . ? C17 C18 1.515(3) . ? C18 C20 1.536(3) . ? C18 C19 1.547(3) . ? C21 C22 1.408(2) . ? C21 C29 1.409(2) . ? C22 C26 1.415(3) . ? C22 C23 1.510(3) . ? C23 C24 1.532(3) . ? C23 C25 1.527(4) . ? C26 C27 1.370(4) . ? C27 C28 1.362(4) . ? C28 C29 1.398(3) . ? C29 C30 1.523(3) . ? C30 C31 1.478(5) . ? C30 C32 1.533(4) . ? 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 C1 N1 C9 131.14(12) . . ? C1 N2 C21 119.49(11) . . ? C5 O1 C6 118.0(3) . . ? N2 C1 N1 121.38(12) . . ? N2 C1 C2 117.04(11) . . ? N1 C1 C2 121.53(11) . . ? C8 C2 C3 118.62(13) . . ? C8 C2 C1 122.34(12) . . ? C3 C2 C1 118.88(13) . . ? C4 C3 C2 120.49(17) . . ? C3 C4 C5 120.26(17) . . ? O1 C5 C4 116.24(19) . . ? O1 C5 C7 123.7(2) . . ? C4 C5 C7 120.08(15) . . ? C5 C7 C8 119.55(17) . . ? C2 C8 C7 120.96(16) . . ? C17 C9 C10 121.44(14) . . ? C17 C9 N1 121.73(13) . . ? C10 C9 N1 116.60(14) . . ? C9 C10 C14 117.15(19) . . ? C9 C10 C11 120.50(16) . . ? C14 C10 C11 122.29(18) . . ? C10 C11 C13 112.8(3) . . ? C10 C11 C12 111.10(19) . . ? C13 C11 C12 112.8(3) . . ? C15 C14 C10 121.51(19) . . ? C16 C15 C14 119.87(18) . . ? C15 C16 C17 122.2(2) . . ? C16 C17 C9 117.79(17) . . ? C16 C17 C18 118.47(17) . . ? C9 C17 C18 123.61(13) . . ? C17 C18 C20 110.48(19) . . ? C17 C18 C19 112.25(17) . . ? C20 C18 C19 113.5(3) . . ? C22 C21 C29 120.99(15) . . ? C22 C21 N2 120.51(15) . . ? C29 C21 N2 118.46(13) . . ? C21 C22 C26 117.3(2) . . ? C21 C22 C23 120.07(15) . . ? C26 C22 C23 122.64(19) . . ? C22 C23 C24 113.9(3) . . ? C22 C23 C25 110.6(2) . . ? C24 C23 C25 112.1(3) . . ? C27 C26 C22 121.6(2) . . ? C28 C27 C26 120.4(2) . . ? C27 C28 C29 121.3(2) . . ? C28 C29 C21 118.45(19) . . ? C28 C29 C30 121.17(19) . . ? C21 C29 C30 120.37(15) . . ? C31 C30 C29 110.9(3) . . ? C31 C30 C32 112.9(3) . . ? C29 C30 C32 114.1(3) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.191 _refine_diff_density_min -0.162 _refine_diff_density_rms 0.025 # ==== END data_9624 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H38 Mo N2 O3' _chemical_formula_weight 558.55 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.8448(11) _cell_length_b 19.285(2) _cell_length_c 14.3146(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.993(8) _cell_angle_gamma 90.00 _cell_volume 2928.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent blocks' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type 'empirical (DIFABS V09.0)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.93 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method 'Phi oscillation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61104 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8322 _reflns_number_gt 5618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.5573P] 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 8322 _refine_ls_number_parameters 468 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.981 _refine_ls_shift/su_mean 0.044 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.81698(2) 0.107651(11) 0.537446(15) 0.06098(9) Uani 1 d . . . N1 N 0.7449(2) 0.27451(10) 0.65784(14) 0.0577(4) Uani 1 d D . . H1 H 0.761(2) 0.2455(12) 0.6140(15) 0.054(6) Uiso 1 d D . . N2 N 0.79763(19) 0.18599(11) 0.77117(14) 0.0599(5) Uani 1 d . . . C1 C 0.7695(2) 0.24953(13) 0.74849(15) 0.0548(5) Uani 1 d . . . C2 C 0.7663(4) 0.29983(19) 0.8289(2) 0.0759(8) Uani 1 d . . . H2A H 0.690(5) 0.317(3) 0.827(4) 0.154(19) Uiso 1 d . . . H2B H 0.803(6) 0.345(3) 0.813(4) 0.17(2) Uiso 1 d . . . H2C H 0.790(4) 0.281(2) 0.889(3) 0.117(14) Uiso 1 d . . . C9 C 0.7217(2) 0.34579(12) 0.63123(16) 0.0573(5) Uani 1 d . . . C10 C 0.6017(3) 0.37407(14) 0.63117(18) 0.0638(6) Uani 1 d . . . C11 C 0.4933(3) 0.33039(17) 0.6504(2) 0.0743(7) Uani 1 d . . . H11 H 0.530(3) 0.2919(17) 0.690(2) 0.083(9) Uiso 1 d . . . C12 C 0.4130(5) 0.3678(4) 0.7118(4) 0.1142(15) Uani 1 d . . . H12A H 0.458(5) 0.392(2) 0.777(4) 0.135(17) Uiso 1 d . . . H12B H 0.351(5) 0.337(3) 0.720(4) 0.141(19) Uiso 1 d . . . H12C H 0.368(6) 0.402(3) 0.671(5) 0.16(3) Uiso 1 d . . . C13 C 0.4125(5) 0.3041(3) 0.5585(4) 0.1070(13) Uani 1 d . . . H13A H 0.334(5) 0.274(3) 0.572(4) 0.141(16) Uiso 1 d . . . H13B H 0.455(5) 0.284(3) 0.512(4) 0.144(18) Uiso 1 d . . . H13C H 0.377(4) 0.341(2) 0.522(3) 0.106(15) Uiso 1 d . . . C14 C 0.5840(3) 0.44467(16) 0.6088(2) 0.0803(8) Uani 1 d . . . H14 H 0.508(3) 0.4657(17) 0.609(2) 0.080(9) Uiso 1 d . . . C15 C 0.6789(4) 0.48412(17) 0.5862(3) 0.0892(10) Uani 1 d . . . H15 H 0.668(3) 0.531(2) 0.571(3) 0.104(11) Uiso 1 d . . . C16 C 0.7930(4) 0.45457(17) 0.5826(3) 0.0841(9) Uani 1 d . . . H16 H 0.854(3) 0.4793(17) 0.563(2) 0.074(8) Uiso 1 d . . . C17 C 0.8177(3) 0.38472(14) 0.6051(2) 0.0675(6) Uani 1 d . . . C18 C 0.9458(3) 0.3532(2) 0.6033(3) 0.0873(9) Uani 1 d . . . H18 H 0.940(4) 0.303(2) 0.602(3) 0.130(16) Uiso 1 d . . . C19 C 1.0369(5) 0.3692(5) 0.6973(6) 0.166(3) Uani 1 d . . . H19A H 1.097(5) 0.349(3) 0.702(4) 0.124(17) Uiso 1 d . . . H19B H 1.047(9) 0.377(5) 0.837(7) 0.27(4) Uiso 1 d . . . H19C H 1.058(4) 0.416(2) 0.658(3) 0.106(14) Uiso 1 d . . . C20 C 0.9954(9) 0.3713(7) 0.5154(7) 0.188(5) Uani 1 d . . . H20A H 0.914(7) 0.333(5) 0.462(6) 0.21(3) Uiso 1 d . . . H20B H 1.072(6) 0.341(3) 0.512(4) 0.155(19) Uiso 1 d . . . H20C H 0.955(7) 0.391(3) 0.472(5) 0.15(3) Uiso 1 d . . . C21 C 0.8110(2) 0.13206(13) 0.70912(17) 0.0560(5) Uani 1 d . . . C22 C 0.9346(2) 0.10961(13) 0.70433(19) 0.0619(5) Uani 1 d . . . C23 C 1.0489(3) 0.14974(16) 0.7569(2) 0.0721(7) Uani 1 d . . . H23 H 1.018(3) 0.1919(18) 0.767(2) 0.078(9) Uiso 1 d . . . C24 C 1.0979(5) 0.1152(3) 0.8524(4) 0.1105(15) Uani 1 d . . . H24A H 1.168(5) 0.149(3) 0.896(3) 0.135(15) Uiso 1 d . . . H24B H 1.127(4) 0.068(3) 0.836(3) 0.129(16) Uiso 1 d . . . H24C H 1.026(6) 0.106(3) 0.890(4) 0.17(2) Uiso 1 d . . . C25 C 1.1529(4) 0.1593(3) 0.7010(4) 0.1121(14) Uani 1 d . . . H25A H 1.218(4) 0.186(2) 0.743(3) 0.116(13) Uiso 1 d . . . H25B H 1.125(5) 0.183(3) 0.636(4) 0.15(2) Uiso 1 d . . . H25C H 1.184(6) 0.112(3) 0.683(5) 0.16(2) Uiso 1 d . . . C26 C 0.9498(3) 0.04426(14) 0.6618(2) 0.0717(7) Uani 1 d . . . H26 H 1.032(3) 0.0308(15) 0.660(2) 0.068(8) Uiso 1 d . . . C27 C 0.8458(3) 0.00258(15) 0.6246(2) 0.0757(7) Uani 1 d . . . H27 H 0.859(3) -0.0377(17) 0.595(2) 0.076(9) Uiso 1 d . . . C28 C 0.7228(3) 0.02605(14) 0.6252(2) 0.0690(6) Uani 1 d . . . H28 H 0.651(3) -0.0024(16) 0.591(2) 0.069(8) Uiso 1 d . . . C29 C 0.7026(2) 0.09145(13) 0.66291(18) 0.0599(5) Uani 1 d . . . C30 C 0.5705(3) 0.11688(17) 0.6665(2) 0.0705(7) Uani 1 d . . . H30 H 0.578(3) 0.1683(16) 0.662(2) 0.065(7) Uiso 1 d . . . C31 C 0.5375(4) 0.0957(4) 0.7619(3) 0.1089(15) Uani 1 d . . . H31A H 0.456(5) 0.119(2) 0.766(3) 0.131(16) Uiso 1 d . . . H31B H 0.607(4) 0.1136(18) 0.816(3) 0.097(12) Uiso 1 d . . . H31C H 0.535(4) 0.042(3) 0.763(4) 0.133(17) Uiso 1 d . . . C32 C 0.4693(3) 0.0920(3) 0.5827(3) 0.0948(11) Uani 1 d . . . H32A H 0.399(5) 0.112(2) 0.587(3) 0.107(14) Uiso 1 d . . . H32B H 0.457(4) 0.042(3) 0.592(3) 0.122(15) Uiso 1 d . . . H32C H 0.497(4) 0.1013(18) 0.522(3) 0.098(12) Uiso 1 d . . . C33 C 0.9489(4) 0.1546(3) 0.4862(3) 0.1098(14) Uani 1 d . . . C34 C 0.6995(4) 0.17602(18) 0.4681(2) 0.0873(9) Uani 1 d . . . C35 C 0.7787(3) 0.05717(15) 0.4167(2) 0.0688(6) Uani 1 d . . . O33 O 1.0263(4) 0.1803(3) 0.4549(3) 0.185(2) Uani 1 d . . . O34 O 0.6276(4) 0.21435(16) 0.4259(2) 0.1380(13) Uani 1 d . . . O35 O 0.7559(2) 0.02635(13) 0.34620(16) 0.0909(6) Uani 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 Mo1 0.06602(14) 0.05781(12) 0.06009(13) -0.00321(9) 0.01537(9) 0.00287(9) N1 0.0661(11) 0.0546(10) 0.0499(9) -0.0033(8) 0.0068(8) 0.0075(9) N2 0.0605(11) 0.0653(11) 0.0512(10) 0.0032(8) 0.0052(8) 0.0116(9) C1 0.0479(10) 0.0640(12) 0.0494(10) -0.0024(9) 0.0034(9) 0.0088(9) C2 0.087(2) 0.0815(19) 0.0536(14) -0.0093(13) 0.0016(14) 0.0217(16) C9 0.0628(13) 0.0549(11) 0.0488(11) -0.0040(9) -0.0013(10) 0.0043(10) C10 0.0630(13) 0.0657(13) 0.0559(12) -0.0057(10) -0.0035(11) 0.0085(11) C11 0.0599(14) 0.0806(18) 0.0783(17) -0.0053(15) 0.0048(13) 0.0087(13) C12 0.087(3) 0.139(4) 0.122(4) -0.038(3) 0.036(3) -0.006(3) C13 0.097(3) 0.123(4) 0.095(3) -0.025(3) 0.005(2) -0.031(3) C14 0.0811(19) 0.0658(16) 0.0841(19) -0.0013(14) -0.0060(16) 0.0188(15) C15 0.101(2) 0.0591(16) 0.095(2) 0.0081(15) -0.0077(19) 0.0073(16) C16 0.091(2) 0.0677(17) 0.086(2) 0.0096(15) -0.0008(17) -0.0150(16) C17 0.0671(15) 0.0681(15) 0.0617(13) -0.0017(11) 0.0002(12) -0.0043(12) C18 0.0683(17) 0.088(2) 0.106(3) 0.0072(19) 0.0185(17) -0.0025(16) C19 0.079(3) 0.233(9) 0.165(6) -0.013(6) -0.024(4) 0.026(4) C20 0.146(6) 0.288(12) 0.154(7) 0.070(8) 0.083(6) 0.070(8) C21 0.0549(12) 0.0555(11) 0.0552(11) 0.0064(9) 0.0060(10) 0.0051(9) C22 0.0565(12) 0.0581(12) 0.0693(14) 0.0042(11) 0.0088(11) 0.0078(10) C23 0.0561(13) 0.0670(15) 0.0884(19) -0.0026(14) 0.0037(13) 0.0030(11) C24 0.105(3) 0.111(3) 0.095(3) 0.006(2) -0.025(2) -0.023(3) C25 0.0661(19) 0.141(4) 0.128(4) -0.009(3) 0.018(2) -0.023(2) C26 0.0624(14) 0.0627(14) 0.0880(18) -0.0008(13) 0.0109(13) 0.0140(11) C27 0.0844(18) 0.0543(13) 0.0850(19) -0.0013(13) 0.0099(15) 0.0084(13) C28 0.0690(15) 0.0599(13) 0.0735(16) 0.0046(12) 0.0042(13) -0.0053(12) C29 0.0571(12) 0.0618(13) 0.0588(12) 0.0078(10) 0.0074(10) 0.0008(10) C30 0.0553(13) 0.0813(18) 0.0739(16) 0.0084(13) 0.0112(12) 0.0007(12) C31 0.073(2) 0.168(5) 0.092(3) 0.025(3) 0.032(2) 0.011(3) C32 0.0593(17) 0.118(3) 0.100(3) 0.006(2) 0.0008(17) -0.0062(18) C33 0.117(3) 0.140(4) 0.080(2) -0.018(2) 0.037(2) -0.051(3) C34 0.129(3) 0.0727(17) 0.0585(14) 0.0030(13) 0.0155(16) 0.0282(18) C35 0.0679(15) 0.0704(15) 0.0680(15) -0.0087(12) 0.0142(12) 0.0064(12) O33 0.189(4) 0.259(5) 0.130(3) -0.027(3) 0.083(3) -0.124(4) O34 0.202(3) 0.112(2) 0.0857(16) 0.0130(15) -0.002(2) 0.071(2) O35 0.0959(15) 0.0970(16) 0.0784(13) -0.0261(12) 0.0153(11) 0.0021(12) _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 Mo1 C35 1.952(3) . ? Mo1 C34 1.955(3) . ? Mo1 C33 1.959(4) . ? Mo1 C27 2.366(3) . ? Mo1 C28 2.373(3) . ? Mo1 C26 2.382(3) . ? Mo1 C29 2.405(3) . ? Mo1 C22 2.464(3) . ? Mo1 C21 2.516(2) . ? N1 C1 1.358(3) . ? N1 C9 1.435(3) . ? N2 C1 1.288(3) . ? N2 C21 1.395(3) . ? C1 C2 1.511(4) . ? C9 C17 1.396(4) . ? C9 C10 1.410(4) . ? C10 C14 1.403(4) . ? C10 C11 1.517(4) . ? C11 C13 1.509(5) . ? C11 C12 1.539(5) . ? C14 C15 1.371(5) . ? C15 C16 1.373(5) . ? C16 C17 1.398(4) . ? C17 C18 1.522(5) . ? C18 C20 1.509(8) . ? C18 C19 1.526(8) . ? C21 C22 1.424(3) . ? C21 C29 1.452(4) . ? C22 C26 1.424(4) . ? C22 C23 1.521(4) . ? C23 C24 1.514(5) . ? C23 C25 1.525(5) . ? C26 C27 1.398(4) . ? C27 C28 1.410(4) . ? C28 C29 1.407(4) . ? C29 C30 1.526(4) . ? C30 C32 1.525(5) . ? C30 C31 1.537(5) . ? C33 O33 1.143(4) . ? C34 O34 1.150(4) . ? C35 O35 1.152(3) . ? 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 C35 Mo1 C34 83.72(12) . . ? C35 Mo1 C33 86.34(14) . . ? C34 Mo1 C33 87.0(2) . . ? C35 Mo1 C27 91.15(12) . . ? C34 Mo1 C27 147.78(15) . . ? C33 Mo1 C27 124.49(18) . . ? C35 Mo1 C28 95.88(11) . . ? C34 Mo1 C28 114.16(14) . . ? C33 Mo1 C28 158.82(17) . . ? C27 Mo1 C28 34.62(10) . . ? C35 Mo1 C26 112.98(11) . . ? C34 Mo1 C26 162.71(11) . . ? C33 Mo1 C26 98.15(16) . . ? C27 Mo1 C26 34.24(10) . . ? C28 Mo1 C26 61.57(10) . . ? C35 Mo1 C29 123.26(11) . . ? C34 Mo1 C29 94.81(12) . . ? C33 Mo1 C29 150.38(13) . . ? C27 Mo1 C29 61.78(10) . . ? C28 Mo1 C29 34.23(9) . . ? C26 Mo1 C29 72.60(10) . . ? C35 Mo1 C22 146.98(10) . . ? C34 Mo1 C22 129.30(11) . . ? C33 Mo1 C22 94.88(14) . . ? C27 Mo1 C22 61.12(10) . . ? C28 Mo1 C22 71.92(9) . . ? C26 Mo1 C22 34.13(9) . . ? C29 Mo1 C22 61.40(8) . . ? C35 Mo1 C21 156.10(11) . . ? C34 Mo1 C21 102.89(10) . . ? C33 Mo1 C21 116.65(12) . . ? C27 Mo1 C21 70.90(10) . . ? C28 Mo1 C21 60.37(9) . . ? C26 Mo1 C21 60.03(9) . . ? C29 Mo1 C21 34.23(8) . . ? C22 Mo1 C21 33.20(8) . . ? C1 N1 C9 125.6(2) . . ? C1 N2 C21 126.8(2) . . ? N2 C1 N1 124.6(2) . . ? N2 C1 C2 117.4(2) . . ? N1 C1 C2 118.0(2) . . ? C17 C9 C10 122.1(2) . . ? C17 C9 N1 119.1(2) . . ? C10 C9 N1 118.8(2) . . ? C14 C10 C9 117.2(3) . . ? C14 C10 C11 120.4(3) . . ? C9 C10 C11 122.3(2) . . ? C13 C11 C10 111.1(3) . . ? C13 C11 C12 111.1(4) . . ? C10 C11 C12 113.3(3) . . ? C15 C14 C10 121.3(3) . . ? C14 C15 C16 120.3(3) . . ? C15 C16 C17 121.5(3) . . ? C9 C17 C16 117.5(3) . . ? C9 C17 C18 121.6(3) . . ? C16 C17 C18 120.9(3) . . ? C20 C18 C19 114.2(6) . . ? C20 C18 C17 114.0(5) . . ? C19 C18 C17 109.3(4) . . ? N2 C21 C22 118.7(2) . . ? N2 C21 C29 120.7(2) . . ? C22 C21 C29 119.7(2) . . ? N2 C21 Mo1 142.06(16) . . ? C22 C21 Mo1 71.37(15) . . ? C29 C21 Mo1 68.71(14) . . ? C26 C22 C21 118.9(2) . . ? C26 C22 C23 120.4(2) . . ? C21 C22 C23 120.0(2) . . ? C26 C22 Mo1 69.80(16) . . ? C21 C22 Mo1 75.43(14) . . ? C23 C22 Mo1 133.80(19) . . ? C24 C23 C22 108.7(3) . . ? C24 C23 C25 111.6(4) . . ? C22 C23 C25 114.7(3) . . ? C27 C26 C22 121.0(3) . . ? C27 C26 Mo1 72.24(17) . . ? C22 C26 Mo1 76.07(15) . . ? C26 C27 C28 120.2(3) . . ? C26 C27 Mo1 73.52(17) . . ? C28 C27 Mo1 72.98(16) . . ? C29 C28 C27 120.9(3) . . ? C29 C28 Mo1 74.14(15) . . ? C27 C28 Mo1 72.40(17) . . ? C28 C29 C21 118.9(2) . . ? C28 C29 C30 121.5(2) . . ? C21 C29 C30 119.2(2) . . ? C28 C29 Mo1 71.63(16) . . ? C21 C29 Mo1 77.07(14) . . ? C30 C29 Mo1 128.09(17) . . ? C29 C30 C32 113.6(3) . . ? C29 C30 C31 109.7(3) . . ? C32 C30 C31 110.6(3) . . ? O33 C33 Mo1 178.1(5) . . ? O34 C34 Mo1 177.6(4) . . ? O35 C35 Mo1 178.9(3) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.250 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.050 # ==== END data_9627 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H42 Mo N2 O3' _chemical_formula_weight 634.65 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinc _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7485(12) _cell_length_b 10.5118(13) _cell_length_c 18.577(3) _cell_angle_alpha 73.567(11) _cell_angle_beta 80.949(11) _cell_angle_gamma 64.730(10) _cell_volume 1649.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 27.1 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type 'empirical (DIFABS V09.0)' _exptl_absorpt_correction_T_min 0.19 _exptl_absorpt_correction_T_max 0.88 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method 'Phi rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17169 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0567 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6303 _reflns_number_gt 4774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6303 _refine_ls_number_parameters 539 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 2.532 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.46449(3) 0.24019(3) 0.364686(16) 0.04760(13) Uani 1 d . . . C1 C 0.0834(3) 0.5658(3) 0.25823(15) 0.0357(6) Uani 1 d . . . C2 C -0.0485(3) 0.6937(3) 0.22083(16) 0.0412(6) Uani 1 d . . . C3 C -0.0875(4) 0.8281(4) 0.2355(2) 0.0589(9) Uani 1 d . . . H3 H -0.023(5) 0.828(4) 0.268(2) 0.080(13) Uiso 1 d . . . C4 C -0.2076(5) 0.9484(4) 0.2018(3) 0.0729(11) Uani 1 d . . . H4 H -0.229(5) 1.033(5) 0.213(3) 0.097(16) Uiso 1 d . . . C5 C -0.2970(4) 0.9414(4) 0.1535(2) 0.0616(9) Uani 1 d . . . C6 C -0.4287(7) 1.0758(7) 0.1158(4) 0.0945(18) Uani 1 d . . . H6A H -0.460(5) 1.075(5) 0.068(3) 0.093(16) Uiso 1 d . . . H6B H -0.412(7) 1.173(8) 0.104(4) 0.15(2) Uiso 1 d . . . H6C H -0.492(6) 1.084(6) 0.144(3) 0.09(2) Uiso 1 d . . . C7 C -0.2612(4) 0.8081(4) 0.1402(2) 0.0625(10) Uani 1 d . . . H7 H -0.314(4) 0.796(4) 0.107(2) 0.064(11) Uiso 1 d . . . C8 C -0.1385(4) 0.6855(4) 0.1724(2) 0.0539(8) Uani 1 d . . . H8 H -0.124(4) 0.599(4) 0.164(2) 0.062(11) Uiso 1 d . . . C9 C 0.1750(3) 0.4535(3) 0.14606(16) 0.0406(6) Uani 1 d . . . C10 C 0.2121(3) 0.5550(3) 0.08826(17) 0.0468(7) Uani 1 d . . . C11 C 0.2411(4) 0.6778(4) 0.0998(2) 0.0567(8) Uani 1 d . . . H11 H 0.220(4) 0.686(4) 0.147(2) 0.049(9) Uiso 1 d . . . C12 C 0.4059(5) 0.6593(6) 0.0803(4) 0.0818(14) Uani 1 d . . . H12A H 0.474(6) 0.574(6) 0.102(3) 0.117(19) Uiso 1 d . . . H12B H 0.425(4) 0.740(4) 0.089(2) 0.064(11) Uiso 1 d . . . H12C H 0.421(5) 0.665(4) 0.032(3) 0.067(13) Uiso 1 d . . . C13 C 0.1336(6) 0.8260(5) 0.0555(3) 0.0773(12) Uani 1 d . . . H13A H 0.163(5) 0.828(5) 0.000(3) 0.088(14) Uiso 1 d . . . H13B H 0.157(6) 0.900(6) 0.059(3) 0.12(2) Uiso 1 d . . . H13C H 0.032(5) 0.846(5) 0.069(3) 0.084(14) Uiso 1 d . . . C14 C 0.2249(4) 0.5397(5) 0.0149(2) 0.0637(10) Uani 1 d . . . H14 H 0.251(4) 0.608(4) -0.025(2) 0.061(10) Uiso 1 d . . . C15 C 0.2040(5) 0.4285(5) 0.0002(2) 0.0732(12) Uani 1 d . . . H15 H 0.213(5) 0.434(5) -0.055(3) 0.091(14) Uiso 1 d . . . C16 C 0.1688(4) 0.3297(5) 0.0572(2) 0.0657(11) Uani 1 d . . . H16 H 0.160(4) 0.250(4) 0.051(2) 0.065(11) Uiso 1 d . . . C17 C 0.1535(4) 0.3392(3) 0.13182(19) 0.0515(8) Uani 1 d . . . C18 C 0.1115(5) 0.2312(4) 0.1946(3) 0.0681(10) Uani 1 d . . . H18 H 0.168(4) 0.207(4) 0.237(2) 0.060(10) Uiso 1 d . . . C19 C 0.1571(11) 0.0837(7) 0.1768(6) 0.122(2) Uani 1 d . . . H19A H 0.124(7) 0.040(7) 0.223(4) 0.13(3) Uiso 1 d . . . H19B H 0.254(7) 0.036(6) 0.175(3) 0.10(2) Uiso 1 d . . . H19C H 0.105(15) 0.101(16) 0.123(8) 0.39(8) Uiso 1 d . . . C20 C -0.0546(7) 0.2907(7) 0.2168(4) 0.0983(17) Uani 1 d . . . H20A H -0.107(4) 0.287(4) 0.172(2) 0.065(11) Uiso 1 d . . . H20B H -0.093(5) 0.390(5) 0.235(3) 0.095(15) Uiso 1 d . . . H20C H -0.071(8) 0.215(8) 0.251(4) 0.15(3) Uiso 1 d . . . C21 C 0.2237(3) 0.4557(3) 0.37117(16) 0.0426(7) Uani 1 d . . . C22 C 0.2044(4) 0.3300(4) 0.41624(17) 0.0498(7) Uani 1 d . . . C23 C 0.0651(4) 0.3046(5) 0.4077(2) 0.0608(9) Uani 1 d . . . H23 H 0.044(3) 0.335(3) 0.3582(19) 0.041(8) Uiso 1 d . . . C24 C -0.0693(8) 0.3967(11) 0.4513(4) 0.107(2) Uani 1 d . . . H24A H -0.153(6) 0.373(5) 0.448(3) 0.099(15) Uiso 1 d . . . H24B H -0.088(7) 0.491(7) 0.437(4) 0.12(2) Uiso 1 d . . . H24C H -0.043(7) 0.334(7) 0.501(4) 0.14(3) Uiso 1 d . . . C25 C 0.0907(9) 0.1447(8) 0.4298(4) 0.102(2) Uani 1 d . . . H25A H 0.086(6) 0.127(6) 0.481(4) 0.108(19) Uiso 1 d . . . H25B H 0.167(12) 0.096(11) 0.405(6) 0.25(5) Uiso 1 d . . . H25C H 0.000(7) 0.137(6) 0.418(3) 0.119(18) Uiso 1 d . . . C26 C 0.3038(5) 0.2396(5) 0.4757(2) 0.0628(10) Uani 1 d . . . H26 H 0.304(5) 0.162(5) 0.502(3) 0.083(14) Uiso 1 d . . . C27 C 0.4209(5) 0.2701(4) 0.4896(2) 0.0657(10) Uani 1 d . . . H27 H 0.491(5) 0.203(5) 0.532(3) 0.083(12) Uiso 1 d . . . C28 C 0.4467(4) 0.3917(4) 0.4415(2) 0.0552(8) Uani 1 d . . . H28 H 0.515(4) 0.421(4) 0.451(2) 0.064(11) Uiso 1 d . . . C29 C 0.3508(4) 0.4832(3) 0.38237(17) 0.0457(7) Uani 1 d . . . C30 C 0.3712(4) 0.6184(4) 0.3347(2) 0.0528(8) Uani 1 d . . . H30 H 0.340(3) 0.633(3) 0.2915(17) 0.034(8) Uiso 1 d . . . C31 C 0.5338(6) 0.6035(6) 0.3216(4) 0.0781(13) Uani 1 d . . . H31A H 0.575(5) 0.601(5) 0.369(3) 0.094(16) Uiso 1 d . . . H31B H 0.540(4) 0.681(5) 0.289(2) 0.074(13) Uiso 1 d . . . H31C H 0.593(5) 0.535(5) 0.298(2) 0.076(14) Uiso 1 d . . . C32 C 0.2749(6) 0.7451(5) 0.3696(3) 0.0698(11) Uani 1 d . . . H32A H 0.178(5) 0.757(4) 0.377(2) 0.068(12) Uiso 1 d . . . H32B H 0.278(5) 0.819(5) 0.340(3) 0.081(14) Uiso 1 d . . . H32C H 0.312(5) 0.722(5) 0.426(3) 0.099(15) Uiso 1 d . . . C41 C 0.4564(4) 0.0782(4) 0.3369(2) 0.0664(10) Uani 1 d . . . C42 C 0.5296(4) 0.3015(4) 0.2607(2) 0.0575(9) Uani 1 d . . . C43 C 0.6805(5) 0.1167(4) 0.3757(2) 0.0665(10) Uani 1 d . . . N1 N 0.1669(3) 0.4573(3) 0.22353(13) 0.0410(5) Uani 1 d D . . H1 H 0.241(3) 0.380(2) 0.2488(15) 0.038(8) Uiso 1 d D . . N2 N 0.1101(3) 0.5648(3) 0.32468(14) 0.0431(6) Uani 1 d . . . O41 O 0.4553(4) -0.0208(4) 0.3208(2) 0.1048(12) Uani 1 d . . . O42 O 0.5732(3) 0.3378(3) 0.19996(17) 0.0870(9) Uani 1 d . . . O43 O 0.8086(3) 0.0420(4) 0.3810(2) 0.0979(10) Uani 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 Mo1 0.05738(19) 0.04323(17) 0.04840(19) 0.00176(11) -0.01895(12) -0.02844(13) C1 0.0374(14) 0.0437(15) 0.0342(15) -0.0129(12) 0.0008(11) -0.0226(12) C2 0.0387(15) 0.0469(16) 0.0384(16) -0.0128(13) -0.0013(12) -0.0164(13) C3 0.0535(19) 0.0536(19) 0.071(2) -0.0223(18) -0.0144(17) -0.0140(16) C4 0.069(3) 0.050(2) 0.093(3) -0.022(2) -0.016(2) -0.0101(19) C5 0.0444(18) 0.061(2) 0.060(2) -0.0098(18) -0.0021(16) -0.0069(16) C6 0.063(3) 0.083(4) 0.096(4) -0.006(3) -0.017(3) 0.004(3) C7 0.0471(19) 0.078(3) 0.059(2) -0.022(2) -0.0131(16) -0.0154(18) C8 0.0499(18) 0.061(2) 0.053(2) -0.0189(17) -0.0102(15) -0.0183(16) C9 0.0391(15) 0.0455(15) 0.0360(15) -0.0139(12) -0.0088(11) -0.0111(13) C10 0.0436(16) 0.0532(17) 0.0383(17) -0.0128(14) -0.0053(12) -0.0122(14) C11 0.062(2) 0.062(2) 0.045(2) -0.0046(16) 0.0021(16) -0.0309(18) C12 0.066(3) 0.079(3) 0.087(4) 0.015(3) -0.011(2) -0.036(2) C13 0.074(3) 0.064(3) 0.079(3) -0.007(2) 0.006(2) -0.024(2) C14 0.060(2) 0.079(3) 0.041(2) -0.0164(19) 0.0022(16) -0.017(2) C15 0.070(2) 0.096(3) 0.047(2) -0.034(2) -0.0070(18) -0.015(2) C16 0.062(2) 0.070(2) 0.072(3) -0.043(2) -0.0172(19) -0.0122(19) C17 0.0496(17) 0.0512(17) 0.056(2) -0.0193(16) -0.0170(14) -0.0141(15) C18 0.085(3) 0.060(2) 0.075(3) -0.012(2) -0.025(2) -0.039(2) C19 0.132(6) 0.073(4) 0.176(8) -0.037(4) -0.001(6) -0.053(4) C20 0.097(4) 0.103(4) 0.103(4) -0.008(4) -0.004(3) -0.060(3) C21 0.0561(17) 0.0507(16) 0.0319(15) -0.0096(13) -0.0049(12) -0.0310(14) C22 0.0639(19) 0.0634(19) 0.0351(16) -0.0070(14) -0.0064(14) -0.0394(16) C23 0.072(2) 0.090(3) 0.0420(19) -0.0067(18) -0.0019(17) -0.058(2) C24 0.089(4) 0.164(7) 0.104(5) -0.045(5) 0.021(3) -0.087(5) C25 0.137(5) 0.114(4) 0.097(4) 0.009(4) -0.026(4) -0.103(4) C26 0.094(3) 0.069(2) 0.0394(18) 0.0055(17) -0.0133(18) -0.055(2) C27 0.088(3) 0.073(2) 0.0436(19) 0.0067(17) -0.0268(18) -0.045(2) C28 0.067(2) 0.062(2) 0.050(2) -0.0061(16) -0.0206(16) -0.0365(18) C29 0.0594(18) 0.0495(17) 0.0402(16) -0.0087(13) -0.0098(13) -0.0318(15) C30 0.070(2) 0.0540(18) 0.0468(19) -0.0049(15) -0.0105(16) -0.0387(17) C31 0.081(3) 0.074(3) 0.099(4) -0.021(3) 0.009(3) -0.054(3) C32 0.084(3) 0.055(2) 0.082(3) -0.012(2) -0.008(2) -0.040(2) C41 0.070(2) 0.056(2) 0.080(3) -0.0024(19) -0.0172(19) -0.0360(19) C42 0.058(2) 0.0427(17) 0.064(2) -0.0025(16) -0.0155(17) -0.0143(15) C43 0.074(2) 0.057(2) 0.071(2) 0.0081(18) -0.028(2) -0.0346(19) N1 0.0455(14) 0.0416(13) 0.0354(13) -0.0075(11) -0.0113(10) -0.0150(11) N2 0.0507(14) 0.0482(13) 0.0370(14) -0.0123(11) -0.0056(10) -0.0236(12) O41 0.120(3) 0.078(2) 0.151(3) -0.050(2) 0.009(2) -0.064(2) O42 0.086(2) 0.0807(19) 0.0644(19) 0.0020(15) 0.0059(15) -0.0213(16) O43 0.0681(18) 0.094(2) 0.115(3) 0.0055(19) -0.0404(17) -0.0239(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 Mo1 C43 1.953(4) . ? Mo1 C41 1.948(4) . ? Mo1 C42 1.952(4) . ? Mo1 C28 2.361(4) . ? Mo1 C27 2.377(4) . ? Mo1 C26 2.386(4) . ? Mo1 C29 2.410(3) . ? Mo1 C22 2.437(3) . ? Mo1 C21 2.486(3) . ? C1 N2 1.297(4) . ? C1 N1 1.355(4) . ? C1 C2 1.490(4) . ? C2 C8 1.393(4) . ? C2 C3 1.394(5) . ? C3 C4 1.371(5) . ? C4 C5 1.382(6) . ? C5 C7 1.377(6) . ? C5 C6 1.520(6) . ? C7 C8 1.387(5) . ? C9 C17 1.403(4) . ? C9 C10 1.408(4) . ? C9 N1 1.440(4) . ? C10 C14 1.397(5) . ? C10 C11 1.510(5) . ? C11 C13 1.534(6) . ? C11 C12 1.530(6) . ? C14 C15 1.373(6) . ? C15 C16 1.374(6) . ? C16 C17 1.397(5) . ? C17 C18 1.522(5) . ? C18 C20 1.501(7) . ? C18 C19 1.537(7) . ? C21 N2 1.394(4) . ? C21 C22 1.420(4) . ? C21 C29 1.444(4) . ? C22 C26 1.421(5) . ? C22 C23 1.530(4) . ? C23 C25 1.530(7) . ? C23 C24 1.529(8) . ? C26 C27 1.388(5) . ? C27 C28 1.433(5) . ? C28 C29 1.401(4) . ? C29 C30 1.522(4) . ? C30 C31 1.511(6) . ? C30 C32 1.519(6) . ? C41 O41 1.167(5) . ? C42 O42 1.159(4) . ? C43 O43 1.159(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C43 Mo1 C41 84.43(16) . . ? C43 Mo1 C42 83.09(15) . . ? C41 Mo1 C42 87.37(16) . . ? C43 Mo1 C28 97.20(15) . . ? C41 Mo1 C28 158.67(15) . . ? C42 Mo1 C28 113.95(14) . . ? C43 Mo1 C27 94.80(16) . . ? C41 Mo1 C27 123.52(15) . . ? C42 Mo1 C27 148.81(15) . . ? C28 Mo1 C27 35.20(12) . . ? C43 Mo1 C26 117.22(15) . . ? C41 Mo1 C26 98.43(16) . . ? C42 Mo1 C26 159.22(14) . . ? C28 Mo1 C26 61.84(13) . . ? C27 Mo1 C26 33.88(13) . . ? C43 Mo1 C29 123.12(13) . . ? C41 Mo1 C29 152.34(14) . . ? C42 Mo1 C29 93.29(12) . . ? C28 Mo1 C29 34.13(11) . . ? C27 Mo1 C29 61.84(12) . . ? C26 Mo1 C29 72.38(12) . . ? C43 Mo1 C22 151.35(14) . . ? C41 Mo1 C22 95.99(14) . . ? C42 Mo1 C22 125.57(12) . . ? C28 Mo1 C22 72.47(12) . . ? C27 Mo1 C22 61.11(12) . . ? C26 Mo1 C22 34.25(12) . . ? C29 Mo1 C22 61.46(11) . . ? C43 Mo1 C21 157.06(14) . . ? C41 Mo1 C21 118.39(13) . . ? C42 Mo1 C21 99.31(12) . . ? C28 Mo1 C21 60.83(11) . . ? C27 Mo1 C21 71.30(12) . . ? C26 Mo1 C21 60.37(12) . . ? C29 Mo1 C21 34.27(10) . . ? C22 Mo1 C21 33.51(10) . . ? N2 C1 N1 123.3(2) . . ? N2 C1 C2 116.4(2) . . ? N1 C1 C2 120.3(2) . . ? C8 C2 C3 117.6(3) . . ? C8 C2 C1 123.1(3) . . ? C3 C2 C1 119.3(3) . . ? C4 C3 C2 121.0(4) . . ? C3 C4 C5 121.8(4) . . ? C7 C5 C4 117.4(3) . . ? C7 C5 C6 121.2(4) . . ? C4 C5 C6 121.3(4) . . ? C5 C7 C8 121.8(4) . . ? C2 C8 C7 120.4(3) . . ? C17 C9 C10 122.1(3) . . ? C17 C9 N1 116.8(3) . . ? C10 C9 N1 120.9(3) . . ? C14 C10 C9 117.5(3) . . ? C14 C10 C11 117.7(3) . . ? C9 C10 C11 124.9(3) . . ? C10 C11 C13 112.0(4) . . ? C10 C11 C12 112.4(4) . . ? C13 C11 C12 109.9(3) . . ? C15 C14 C10 121.1(4) . . ? C14 C15 C16 120.8(4) . . ? C15 C16 C17 121.1(4) . . ? C16 C17 C9 117.5(3) . . ? C16 C17 C18 120.8(3) . . ? C9 C17 C18 121.6(3) . . ? C20 C18 C17 112.1(4) . . ? C20 C18 C19 109.3(5) . . ? C17 C18 C19 113.8(5) . . ? N2 C21 C22 121.1(3) . . ? N2 C21 C29 118.4(3) . . ? C22 C21 C29 119.7(3) . . ? N2 C21 Mo1 140.1(2) . . ? C22 C21 Mo1 71.36(18) . . ? C29 C21 Mo1 69.96(18) . . ? C21 C22 C26 119.2(3) . . ? C21 C22 C23 119.9(3) . . ? C26 C22 C23 120.3(3) . . ? C21 C22 Mo1 75.13(18) . . ? C26 C22 Mo1 70.9(2) . . ? C23 C22 Mo1 132.6(2) . . ? C25 C23 C24 112.7(5) . . ? C25 C23 C22 113.7(4) . . ? C24 C23 C22 108.3(4) . . ? C27 C26 C22 121.3(3) . . ? C27 C26 Mo1 72.7(2) . . ? C22 C26 Mo1 74.9(2) . . ? C26 C27 C28 119.7(3) . . ? C26 C27 Mo1 73.4(2) . . ? C28 C27 Mo1 71.8(2) . . ? C29 C28 C27 120.5(3) . . ? C29 C28 Mo1 74.85(19) . . ? C27 C28 Mo1 73.0(2) . . ? C28 C29 C21 119.4(3) . . ? C28 C29 C30 120.5(3) . . ? C21 C29 C30 119.9(3) . . ? C28 C29 Mo1 71.0(2) . . ? C21 C29 Mo1 75.77(18) . . ? C30 C29 Mo1 129.2(2) . . ? C31 C30 C29 114.9(3) . . ? C31 C30 C32 110.7(4) . . ? C29 C30 C32 109.0(3) . . ? O41 C41 Mo1 178.3(4) . . ? O42 C42 Mo1 177.3(3) . . ? O43 C43 Mo1 178.4(4) . . ? C1 N1 C9 130.4(2) . . ? C1 N2 C21 126.7(2) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.585 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.068 # ==== END data_9630 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H38 Mo N2 O5' _chemical_formula_weight 614.57 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.9975(10) _cell_length_b 21.7750(18) _cell_length_c 14.5403(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.524(7) _cell_angle_gamma 90.00 _cell_volume 3239.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description 'transparent blocks' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type 'empirical (DIFABS V09.0)' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.90 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method 'Phi rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25416 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6135 _reflns_number_gt 4678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SIR92 (Giacovazzo et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.2443P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6135 _refine_ls_number_parameters 505 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.338 _refine_ls_shift/su_mean 0.012 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.01480(2) 0.137466(10) 0.660705(17) 0.07123(12) Uani 1 d . . . N1 N 0.22791(18) 0.10210(8) 0.74942(14) 0.0587(4) Uani 1 d . . . N2 N 0.1749(2) 0.02818(10) 0.84105(16) 0.0678(5) Uani 1 d D . . H3 H 0.094(2) 0.0402(14) 0.805(2) 0.085(9) Uiso 1 d D . . C1 C 0.2648(2) 0.05929(10) 0.81647(17) 0.0583(5) Uani 1 d . . . C2 C 0.4044(3) 0.04112(15) 0.8715(3) 0.0738(7) Uani 1 d . . . H2A H 0.414(4) -0.001(2) 0.868(3) 0.117(13) Uiso 1 d . . . H2B H 0.434(4) 0.0462(18) 0.938(3) 0.114(13) Uiso 1 d . . . H2C H 0.466(3) 0.0599(18) 0.848(2) 0.101(11) Uiso 1 d . . . C9 C 0.3324(2) 0.13444(11) 0.73082(19) 0.0648(6) Uani 1 d . . . C10 C 0.3767(3) 0.11258(13) 0.6574(2) 0.0729(6) Uani 1 d . . . C11 C 0.3205(4) 0.05592(15) 0.5963(2) 0.0845(8) Uani 1 d . . . H11 H 0.248(3) 0.0428(13) 0.607(2) 0.075(8) Uiso 1 d . . . C12 C 0.2712(7) 0.0703(3) 0.4857(3) 0.1175(14) Uani 1 d . . . H12A H 0.224(4) 0.037(2) 0.448(3) 0.114(13) Uiso 1 d . . . H12B H 0.346(5) 0.076(2) 0.467(4) 0.139(17) Uiso 1 d . . . H12C H 0.205(6) 0.106(3) 0.464(4) 0.17(2) Uiso 1 d . . . C13 C 0.4176(7) 0.0028(3) 0.6211(5) 0.1250(15) Uani 1 d . . . H13A H 0.371(4) -0.034(2) 0.579(3) 0.134(15) Uiso 1 d . . . H13B H 0.455(5) -0.010(2) 0.686(4) 0.148(19) Uiso 1 d . . . H13C H 0.484(8) 0.008(4) 0.610(6) 0.22(4) Uiso 1 d . . . C14 C 0.4783(4) 0.14477(17) 0.6433(3) 0.0906(9) Uani 1 d . . . H14 H 0.507(5) 0.125(2) 0.600(4) 0.131(15) Uiso 1 d . . . C15 C 0.5323(4) 0.19553(18) 0.6961(3) 0.0990(11) Uani 1 d . . . H15 H 0.598(4) 0.2129(17) 0.687(3) 0.107(11) Uiso 1 d . . . C16 C 0.4870(3) 0.21722(16) 0.7663(3) 0.0901(9) Uani 1 d . . . H16 H 0.525(3) 0.2531(16) 0.803(2) 0.093(9) Uiso 1 d . . . C17 C 0.3863(3) 0.18747(12) 0.7860(2) 0.0727(6) Uani 1 d . . . C18 C 0.3427(3) 0.21165(14) 0.8665(2) 0.0826(8) Uani 1 d . . . H18 H 0.266(3) 0.1874(16) 0.866(2) 0.097(10) Uiso 1 d . . . C19 C 0.2974(6) 0.2788(2) 0.8480(5) 0.1230(15) Uani 1 d . . . H19A H 0.371(5) 0.306(2) 0.854(3) 0.135(16) Uiso 1 d . . . H19B H 0.273(5) 0.286(2) 0.898(4) 0.133(17) Uiso 1 d . . . H19C H 0.223(5) 0.285(2) 0.783(4) 0.137(16) Uiso 1 d . . . C20 C 0.4482(5) 0.2050(2) 0.9690(3) 0.1050(11) Uani 1 d . . . H20A H 0.413(4) 0.2110(18) 1.020(3) 0.117(13) Uiso 1 d . . . H20B H 0.523(4) 0.229(2) 0.969(3) 0.124(14) Uiso 1 d . . . H20C H 0.479(4) 0.161(2) 0.986(3) 0.117(13) Uiso 1 d . . . C21 C 0.2038(2) -0.01668(11) 0.91883(19) 0.0638(6) Uani 1 d . . . C22 C 0.2314(2) 0.00410(12) 1.0160(2) 0.0691(6) Uani 1 d . . . C23 C 0.2253(3) 0.07188(14) 1.0393(3) 0.0796(7) Uani 1 d . . . H23 H 0.240(3) 0.0946(15) 0.993(2) 0.085(9) Uiso 1 d . . . C24 C 0.3221(7) 0.0919(3) 1.1387(5) 0.1327(18) Uani 1 d . . . H24A H 0.317(4) 0.139(2) 1.143(3) 0.130(15) Uiso 1 d . . . H24B H 0.402(5) 0.085(2) 1.136(4) 0.15(2) Uiso 1 d . . . H24C H 0.313(7) 0.071(3) 1.186(5) 0.20(4) Uiso 1 d . . . C25 C 0.0852(5) 0.0883(2) 1.0240(7) 0.138(2) Uani 1 d . . . H25A H 0.050(6) 0.133(3) 1.024(4) 0.16(2) Uiso 1 d . . . H25B H 0.099(4) 0.0750(18) 1.097(3) 0.103(13) Uiso 1 d . . . H25C H 0.020(9) 0.070(4) 0.978(7) 0.29(5) Uiso 1 d . . . C26 C 0.2591(3) -0.04034(16) 1.0903(2) 0.0793(7) Uani 1 d . . . H26 H 0.278(3) -0.0272(15) 1.151(3) 0.088(9) Uiso 1 d . . . C27 C 0.2589(3) -0.10167(16) 1.0686(2) 0.0836(8) Uani 1 d . . . H27 H 0.280(3) -0.1319(14) 1.117(2) 0.085(9) Uiso 1 d . . . C28 C 0.2311(3) -0.12102(14) 0.9730(3) 0.0808(8) Uani 1 d . . . H28 H 0.231(3) -0.1653(17) 0.959(2) 0.097(10) Uiso 1 d . . . C29 C 0.2025(2) -0.07903(12) 0.8956(2) 0.0695(6) Uani 1 d . . . C30 C 0.1688(3) -0.10113(15) 0.7905(2) 0.0828(8) Uani 1 d . . . H30 H 0.167(3) -0.0694(16) 0.753(2) 0.089(10) Uiso 1 d . . . C31 C 0.0319(6) -0.1294(3) 0.7516(4) 0.1320(17) Uani 1 d . . . H31A H 0.011(5) -0.146(2) 0.689(4) 0.144(18) Uiso 1 d . . . H31B H -0.029(8) -0.090(3) 0.756(6) 0.22(3) Uiso 1 d . . . H31C H 0.034(6) -0.167(3) 0.797(5) 0.20(3) Uiso 1 d . . . C32 C 0.2679(7) -0.1459(4) 0.7795(5) 0.144(2) Uani 1 d . . . H32A H 0.248(5) -0.154(2) 0.714(4) 0.148(18) Uiso 1 d . . . H32B H 0.223(12) -0.186(6) 0.788(9) 0.39(8) Uiso 1 d . . . H32C H 0.343(6) -0.131(2) 0.802(4) 0.13(2) Uiso 1 d . . . C41 C -0.1531(4) 0.17605(18) 0.5839(3) 0.1046(10) Uani 1 d . . . C42 C 0.0077(3) 0.18724(17) 0.7793(3) 0.0973(9) Uani 1 d . . . C43 C 0.1011(3) 0.20723(16) 0.6061(3) 0.0957(9) Uani 1 d . . . C44 C -0.0155(3) 0.08736(16) 0.5350(2) 0.0884(8) Uani 1 d . . . C45 C -0.0981(3) 0.07472(16) 0.6934(2) 0.0849(8) Uani 1 d . . . O41 O -0.2521(3) 0.19817(17) 0.5387(3) 0.1560(13) Uani 1 d . . . O42 O -0.0102(3) 0.21421(16) 0.8403(2) 0.1369(11) Uani 1 d . . . O43 O 0.1368(3) 0.24558(14) 0.5698(2) 0.1386(11) Uani 1 d . . . O44 O -0.0495(3) 0.06206(15) 0.46143(19) 0.1275(10) Uani 1 d . . . O45 O -0.1749(3) 0.04244(16) 0.7047(2) 0.1224(9) Uani 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 Mo1 0.06863(17) 0.06819(17) 0.07116(17) 0.00566(10) 0.01890(11) 0.00871(10) N1 0.0606(10) 0.0547(10) 0.0609(10) 0.0031(9) 0.0223(8) 0.0006(8) N2 0.0562(11) 0.0665(11) 0.0784(13) 0.0194(10) 0.0219(10) 0.0027(9) C1 0.0587(12) 0.0547(11) 0.0625(12) 0.0015(10) 0.0233(10) 0.0005(9) C2 0.0584(14) 0.0794(18) 0.0832(18) 0.0212(15) 0.0254(13) 0.0053(12) C9 0.0656(13) 0.0595(12) 0.0683(13) 0.0101(11) 0.0234(11) -0.0002(10) C10 0.0798(16) 0.0719(14) 0.0710(15) 0.0107(13) 0.0324(13) 0.0004(13) C11 0.101(2) 0.0821(18) 0.0821(18) -0.0011(15) 0.0475(17) -0.0023(16) C12 0.148(4) 0.123(3) 0.084(2) -0.012(2) 0.047(2) -0.016(3) C13 0.154(4) 0.100(3) 0.130(4) -0.006(3) 0.062(4) 0.027(3) C14 0.095(2) 0.099(2) 0.090(2) 0.0167(18) 0.0479(18) -0.0047(18) C15 0.089(2) 0.103(2) 0.109(2) 0.024(2) 0.0416(19) -0.0190(19) C16 0.088(2) 0.0745(18) 0.100(2) 0.0102(17) 0.0255(17) -0.0191(15) C17 0.0732(15) 0.0603(13) 0.0796(16) 0.0062(12) 0.0220(12) -0.0030(11) C18 0.0809(18) 0.0694(15) 0.0919(19) -0.0141(14) 0.0249(15) -0.0054(14) C19 0.142(4) 0.081(2) 0.146(4) -0.017(3) 0.052(4) 0.010(3) C20 0.103(3) 0.118(3) 0.088(2) -0.021(2) 0.027(2) -0.010(2) C21 0.0544(12) 0.0657(13) 0.0731(14) 0.0118(11) 0.0256(10) 0.0002(10) C22 0.0553(12) 0.0759(15) 0.0793(16) 0.0054(13) 0.0284(11) 0.0008(11) C23 0.0683(15) 0.0796(17) 0.097(2) 0.0015(16) 0.0373(15) -0.0003(13) C24 0.134(4) 0.119(4) 0.121(4) -0.036(3) 0.018(3) 0.001(3) C25 0.095(3) 0.101(3) 0.233(7) -0.025(4) 0.079(4) 0.011(2) C26 0.0682(15) 0.100(2) 0.0716(16) 0.0130(16) 0.0283(13) 0.0011(14) C27 0.0740(17) 0.090(2) 0.0875(19) 0.0321(18) 0.0303(14) 0.0073(14) C28 0.0760(17) 0.0693(17) 0.100(2) 0.0204(16) 0.0359(15) 0.0071(13) C29 0.0618(13) 0.0675(14) 0.0807(16) 0.0096(12) 0.0279(12) 0.0026(11) C30 0.091(2) 0.0719(17) 0.0863(19) 0.0040(15) 0.0328(15) -0.0017(14) C31 0.117(3) 0.164(5) 0.103(3) -0.025(3) 0.027(2) -0.038(3) C32 0.124(4) 0.176(6) 0.128(4) -0.048(4) 0.043(3) 0.030(4) C41 0.094(2) 0.106(2) 0.103(2) 0.012(2) 0.0230(18) 0.0199(19) C42 0.093(2) 0.092(2) 0.100(2) -0.0030(19) 0.0278(18) 0.0136(17) C43 0.098(2) 0.0822(19) 0.093(2) 0.0144(18) 0.0199(17) 0.0098(17) C44 0.0901(19) 0.092(2) 0.0763(18) 0.0089(16) 0.0224(14) -0.0029(16) C45 0.0750(17) 0.102(2) 0.0724(16) 0.0011(15) 0.0210(13) 0.0039(16) O41 0.1030(19) 0.168(3) 0.164(3) 0.034(2) 0.0101(19) 0.059(2) O42 0.163(3) 0.130(2) 0.127(2) -0.0347(18) 0.064(2) 0.0223(19) O43 0.156(3) 0.1025(18) 0.146(2) 0.0535(19) 0.041(2) -0.0098(17) O44 0.153(2) 0.139(2) 0.0779(15) -0.0195(15) 0.0273(15) -0.0155(19) O45 0.1067(18) 0.157(2) 0.1097(18) -0.0051(17) 0.0466(15) -0.0409(18) _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 Mo1 C41 1.962(3) . ? Mo1 C45 2.016(4) . ? Mo1 C44 2.049(4) . ? Mo1 C42 2.062(4) . ? Mo1 C43 2.095(4) . ? Mo1 N1 2.3519(19) . ? N1 C1 1.302(3) . ? N1 C9 1.455(3) . ? N2 C1 1.351(3) . ? N2 C21 1.439(3) . ? C1 C2 1.500(3) . ? C9 C17 1.407(4) . ? C9 C10 1.409(4) . ? C10 C14 1.396(4) . ? C10 C11 1.514(4) . ? C11 C13 1.525(6) . ? C11 C12 1.528(5) . ? C14 C15 1.352(6) . ? C15 C16 1.373(6) . ? C16 C17 1.400(4) . ? C17 C18 1.514(4) . ? C18 C20 1.523(5) . ? C18 C19 1.536(5) . ? C21 C29 1.398(4) . ? C21 C22 1.406(4) . ? C22 C26 1.398(4) . ? C22 C23 1.521(4) . ? C23 C25 1.516(5) . ? C23 C24 1.511(6) . ? C26 C27 1.372(5) . ? C27 C28 1.375(5) . ? C28 C29 1.394(4) . ? C29 C30 1.513(4) . ? C30 C32 1.513(6) . ? C30 C31 1.530(6) . ? C41 O41 1.151(4) . ? C42 O42 1.140(4) . ? C43 O43 1.133(4) . ? C44 O44 1.137(4) . ? C45 O45 1.156(4) . ? 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 C41 Mo1 C45 83.80(15) . . ? C41 Mo1 C44 84.80(15) . . ? C45 Mo1 C44 86.38(13) . . ? C41 Mo1 C42 86.24(15) . . ? C45 Mo1 C42 86.78(14) . . ? C44 Mo1 C42 169.26(14) . . ? C41 Mo1 C43 86.35(15) . . ? C45 Mo1 C43 169.71(12) . . ? C44 Mo1 C43 89.77(14) . . ? C42 Mo1 C43 95.56(15) . . ? C41 Mo1 N1 173.10(13) . . ? C45 Mo1 N1 102.99(10) . . ? C44 Mo1 N1 96.77(10) . . ? C42 Mo1 N1 92.82(10) . . ? C43 Mo1 N1 86.93(10) . . ? C1 N1 C9 115.80(19) . . ? C1 N1 Mo1 128.28(15) . . ? C9 N1 Mo1 115.83(14) . . ? C1 N2 C21 125.2(2) . . ? N1 C1 N2 120.0(2) . . ? N1 C1 C2 124.4(2) . . ? N2 C1 C2 115.6(2) . . ? C17 C9 C10 121.2(2) . . ? C17 C9 N1 119.2(2) . . ? C10 C9 N1 119.6(2) . . ? C14 C10 C9 117.3(3) . . ? C14 C10 C11 120.0(3) . . ? C9 C10 C11 122.7(2) . . ? C10 C11 C13 112.3(4) . . ? C10 C11 C12 111.2(3) . . ? C13 C11 C12 110.6(4) . . ? C15 C14 C10 122.4(3) . . ? C14 C15 C16 120.0(3) . . ? C15 C16 C17 121.5(3) . . ? C16 C17 C9 117.6(3) . . ? C16 C17 C18 119.7(3) . . ? C9 C17 C18 122.7(2) . . ? C17 C18 C20 112.4(3) . . ? C17 C18 C19 111.7(4) . . ? C20 C18 C19 110.1(4) . . ? C29 C21 C22 122.3(2) . . ? C29 C21 N2 119.3(2) . . ? C22 C21 N2 118.4(2) . . ? C26 C22 C21 117.3(3) . . ? C26 C22 C23 120.9(3) . . ? C21 C22 C23 121.7(2) . . ? C25 C23 C24 113.2(5) . . ? C25 C23 C22 108.7(3) . . ? C24 C23 C22 114.8(3) . . ? C27 C26 C22 121.0(3) . . ? C28 C27 C26 120.8(3) . . ? C27 C28 C29 121.1(3) . . ? C28 C29 C21 117.5(3) . . ? C28 C29 C30 120.4(3) . . ? C21 C29 C30 122.0(2) . . ? C32 C30 C29 113.1(4) . . ? C32 C30 C31 110.5(5) . . ? C29 C30 C31 110.2(3) . . ? O41 C41 Mo1 179.4(4) . . ? O42 C42 Mo1 172.7(3) . . ? O43 C43 Mo1 173.7(3) . . ? O44 C44 Mo1 170.6(3) . . ? O45 C45 Mo1 172.1(3) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.286 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.042 # ==== END data_9811 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H42 N2' _chemical_formula_weight 454.68 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.409(2) _cell_length_b 9.9850(10) _cell_length_c 17.6590(10) _cell_angle_alpha 90.00 _cell_angle_beta 117.130(10) _cell_angle_gamma 90.00 _cell_volume 2888.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 9.564 _cell_measurement_theta_max 25.052 _exptl_crystal_description 'transparent blocks' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9581 _exptl_absorpt_correction_T_max 0.9741 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.46 _diffrn_reflns_number 6226 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5026 _reflns_number_gt 2454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.0762P)^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 5026 _refine_ls_number_parameters 480 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.24957(12) 0.17971(19) 0.25205(12) 0.0584(5) Uani 1 d D . . H1 H 0.2296(17) 0.106(2) 0.2194(17) 0.065(10) Uiso 0.72 d PD . . N2 N 0.23888(12) 0.0604(2) 0.35854(12) 0.0606(5) Uani 1 d D . . H2 H 0.228(5) 0.058(8) 0.405(3) 0.07(2) Uiso 0.28 d PD . . C1 C 0.25091(12) 0.1746(2) 0.32872(14) 0.0529(6) Uani 1 d . . . C2 C 0.26349(13) 0.2943(2) 0.38297(14) 0.0532(6) Uani 1 d . . . C3 C 0.30815(17) 0.2827(3) 0.47113(17) 0.0713(7) Uani 1 d . . . H3 H 0.3329(15) 0.190(3) 0.4943(16) 0.091(9) Uiso 1 d . . . C4 C 0.3155(2) 0.3923(4) 0.5227(2) 0.0872(9) Uani 1 d . . . H4 H 0.3465(15) 0.378(3) 0.5817(18) 0.087(9) Uiso 1 d . . . C5 C 0.27981(19) 0.5134(3) 0.4898(2) 0.0819(9) Uani 1 d . . . C6 C 0.2865(4) 0.6312(5) 0.5475(4) 0.1289(17) Uani 1 d . . . H6A H 0.296(3) 0.597(5) 0.603(4) 0.22(3) Uiso 1 d . . . H6B H 0.234(4) 0.683(6) 0.529(4) 0.24(3) Uiso 1 d . . . H6C H 0.326(3) 0.684(5) 0.558(3) 0.20(2) Uiso 1 d . . . C7 C 0.23698(18) 0.5255(3) 0.4028(2) 0.0766(8) Uani 1 d . . . H7 H 0.2069(15) 0.609(3) 0.3755(15) 0.078(8) Uiso 1 d . . . C8 C 0.22871(16) 0.4178(2) 0.34972(18) 0.0646(7) Uani 1 d . . . H8 H 0.1949(12) 0.429(2) 0.2867(14) 0.058(6) Uiso 1 d . . . C9 C 0.26608(16) 0.2885(2) 0.21028(14) 0.0576(6) Uani 1 d . . . C10 C 0.34337(17) 0.3483(2) 0.24347(15) 0.0634(6) Uani 1 d . . . C11 C 0.41471(16) 0.3033(3) 0.32548(17) 0.0703(7) Uani 1 d . . . H11 H 0.3960(14) 0.243(2) 0.3550(15) 0.075(8) Uiso 1 d . . . C12 C 0.4556(3) 0.4188(4) 0.3874(3) 0.1156(13) Uani 1 d . . . H12A H 0.502(2) 0.383(4) 0.445(3) 0.143(13) Uiso 1 d . . . H12B H 0.416(3) 0.482(5) 0.389(3) 0.166(19) Uiso 1 d . . . H12C H 0.481(2) 0.473(4) 0.355(2) 0.124(13) Uiso 1 d . . . C13 C 0.4744(3) 0.2204(5) 0.3067(3) 0.1066(12) Uani 1 d . . . H13A H 0.519(2) 0.187(4) 0.360(2) 0.139(14) Uiso 1 d . . . H13B H 0.496(2) 0.284(4) 0.282(2) 0.147(16) Uiso 1 d . . . H13C H 0.446(3) 0.138(4) 0.265(3) 0.170(18) Uiso 1 d . . . C14 C 0.3558(2) 0.4472(3) 0.1954(2) 0.0808(8) Uani 1 d . . . H14 H 0.4127(17) 0.492(3) 0.2170(16) 0.094(9) Uiso 1 d . . . C15 C 0.2958(3) 0.4840(3) 0.1177(3) 0.0969(11) Uani 1 d . . . H15 H 0.3108(18) 0.551(3) 0.0884(19) 0.115(11) Uiso 1 d . . . C16 C 0.2209(3) 0.4240(3) 0.0853(2) 0.0899(9) Uani 1 d . . . H16 H 0.1777(15) 0.442(3) 0.0282(18) 0.084(8) Uiso 1 d . . . C17 C 0.20342(17) 0.3239(3) 0.13014(15) 0.0679(7) Uani 1 d . . . C18 C 0.12220(19) 0.2529(4) 0.09407(19) 0.0896(9) Uani 1 d . . . H18 H 0.1068(19) 0.237(3) 0.143(2) 0.127(12) Uiso 1 d . . . C19 C 0.0504(3) 0.3369(8) 0.0330(3) 0.1534(19) Uani 1 d . . . H19A H -0.006(3) 0.276(5) 0.015(3) 0.19(2) Uiso 1 d . . . H19B H 0.057(3) 0.345(4) -0.025(3) 0.176(17) Uiso 1 d . . . H19C H 0.057(3) 0.432(6) 0.076(4) 0.24(3) Uiso 1 d . . . C20 C 0.1264(3) 0.1168(5) 0.0537(3) 0.1311(16) Uani 1 d . . . H20A H 0.076(3) 0.079(4) 0.034(3) 0.148(16) Uiso 1 d . . . H20B H 0.175(3) 0.065(5) 0.103(3) 0.20(2) Uiso 1 d . . . H20C H 0.116(2) 0.196(4) -0.011(2) 0.148(13) Uiso 1 d . . . C21 C 0.21838(17) -0.0565(2) 0.30610(15) 0.0655(7) Uani 1 d . . . C22 C 0.2805(2) -0.1343(3) 0.30349(17) 0.0752(7) Uani 1 d . . . C23 C 0.3685(2) -0.0993(3) 0.3585(2) 0.0867(9) Uani 1 d . . . H23 H 0.3729(14) -0.006(3) 0.3632(15) 0.072(8) Uiso 1 d . . . C24 C 0.3977(3) -0.1453(6) 0.4504(3) 0.1342(16) Uani 1 d . . . H24A H 0.458(3) -0.123(4) 0.487(3) 0.157(15) Uiso 1 d . . . H24B H 0.391(3) -0.252(5) 0.445(3) 0.21(2) Uiso 1 d . . . H24C H 0.357(3) -0.123(5) 0.471(3) 0.18(2) Uiso 1 d . . . C25 C 0.4289(4) -0.1515(7) 0.3274(5) 0.1490(18) Uani 1 d . . . H25A H 0.489(3) -0.116(5) 0.378(3) 0.21(2) Uiso 1 d . . . H25B H 0.405(2) -0.091(4) 0.271(2) 0.145(16) Uiso 1 d . . . H25C H 0.423(4) -0.250(7) 0.327(4) 0.24(3) Uiso 1 d . . . C26 C 0.2566(3) -0.2474(3) 0.2505(2) 0.0992(10) Uani 1 d . . . H26 H 0.3050(17) -0.299(3) 0.2548(17) 0.098(10) Uiso 1 d . . . C27 C 0.1759(4) -0.2798(4) 0.2035(3) 0.1174(15) Uani 1 d . . . H27 H 0.159(2) -0.351(4) 0.169(2) 0.135(14) Uiso 1 d . . . C28 C 0.1158(3) -0.2039(4) 0.2080(2) 0.1052(11) Uani 1 d . . . H28 H 0.056(2) -0.232(3) 0.171(2) 0.124(12) Uiso 1 d . . . C29 C 0.1359(2) -0.0908(3) 0.25851(18) 0.0835(8) Uani 1 d . . . C30 C 0.0697(2) -0.0070(4) 0.2644(3) 0.1067(11) Uani 1 d . . . H30 H 0.0859(19) 0.093(4) 0.278(2) 0.129(12) Uiso 1 d . . . C31 C 0.0531(6) -0.0595(8) 0.3343(5) 0.174(2) Uani 1 d . . . H31A H 0.006(2) -0.138(4) 0.292(3) 0.142(14) Uiso 1 d . . . H31B H 0.013(3) -0.027(6) 0.337(3) 0.19(3) Uiso 1 d . . . H31C H 0.109(5) -0.067(8) 0.394(5) 0.30(4) Uiso 1 d . . . C32 C -0.0075(3) 0.0065(9) 0.1806(5) 0.161(2) Uani 1 d . . . H32A H -0.045(4) 0.067(6) 0.191(4) 0.24(3) Uiso 1 d . . . H32B H -0.030(3) -0.108(6) 0.175(4) 0.23(3) Uiso 1 d . . . H32C H 0.003(3) 0.027(6) 0.134(3) 0.21(3) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0784(13) 0.0478(12) 0.0521(11) -0.0032(10) 0.0325(10) -0.0062(10) N2 0.0785(14) 0.0499(12) 0.0611(12) -0.0023(11) 0.0385(11) -0.0056(10) C1 0.0510(13) 0.0530(14) 0.0555(13) -0.0023(12) 0.0249(11) 0.0032(11) C2 0.0565(14) 0.0547(15) 0.0563(14) -0.0061(12) 0.0325(12) -0.0075(11) C3 0.0843(18) 0.0717(18) 0.0624(17) -0.0064(15) 0.0374(14) -0.0107(15) C4 0.102(2) 0.103(3) 0.0619(19) -0.0219(19) 0.0418(18) -0.030(2) C5 0.101(2) 0.072(2) 0.099(2) -0.0294(18) 0.069(2) -0.0292(17) C6 0.175(5) 0.106(3) 0.150(4) -0.077(3) 0.111(4) -0.057(3) C7 0.088(2) 0.0603(18) 0.100(2) -0.0127(18) 0.0586(19) -0.0024(15) C8 0.0726(16) 0.0605(16) 0.0661(17) -0.0084(14) 0.0363(14) -0.0014(13) C9 0.0806(17) 0.0460(13) 0.0567(14) 0.0014(12) 0.0406(14) 0.0069(12) C10 0.0883(18) 0.0492(14) 0.0685(16) -0.0003(13) 0.0495(15) -0.0006(13) C11 0.0742(17) 0.0663(17) 0.0769(18) -0.0007(15) 0.0400(16) -0.0044(14) C12 0.118(3) 0.094(3) 0.105(3) -0.013(2) 0.025(3) -0.015(3) C13 0.099(3) 0.122(3) 0.119(3) 0.021(3) 0.067(3) 0.031(3) C14 0.108(2) 0.0641(17) 0.091(2) 0.0036(17) 0.064(2) -0.0045(18) C15 0.157(4) 0.063(2) 0.101(3) 0.0144(19) 0.085(3) 0.006(2) C16 0.132(3) 0.080(2) 0.0598(19) 0.0192(17) 0.045(2) 0.030(2) C17 0.0891(19) 0.0645(16) 0.0545(15) 0.0057(14) 0.0365(15) 0.0197(15) C18 0.079(2) 0.113(2) 0.0667(18) -0.0021(19) 0.0246(16) 0.0173(19) C19 0.105(3) 0.221(6) 0.116(3) 0.027(4) 0.034(3) 0.046(4) C20 0.110(3) 0.143(4) 0.127(4) -0.053(3) 0.042(3) -0.028(3) C21 0.095(2) 0.0467(14) 0.0673(15) 0.0015(13) 0.0480(15) -0.0048(14) C22 0.110(2) 0.0506(15) 0.0815(18) 0.0076(14) 0.0585(18) 0.0059(15) C23 0.108(3) 0.064(2) 0.112(2) 0.0144(18) 0.071(2) 0.0196(18) C24 0.110(3) 0.161(5) 0.117(3) 0.043(3) 0.039(3) -0.001(3) C25 0.158(5) 0.141(5) 0.196(6) 0.011(5) 0.123(5) 0.037(4) C26 0.155(4) 0.059(2) 0.105(3) 0.002(2) 0.079(3) 0.016(2) C27 0.195(5) 0.063(2) 0.099(3) -0.019(2) 0.070(3) -0.024(3) C28 0.132(3) 0.074(2) 0.099(2) -0.020(2) 0.044(2) -0.025(2) C29 0.104(2) 0.0647(18) 0.0792(18) -0.0133(15) 0.0398(17) -0.0201(17) C30 0.086(2) 0.102(3) 0.122(3) -0.035(2) 0.039(2) -0.022(2) C31 0.202(7) 0.214(6) 0.151(5) -0.028(5) 0.119(5) 0.010(6) C32 0.108(4) 0.208(7) 0.153(5) -0.010(5) 0.047(4) 0.003(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 N1 C1 1.344(3) . ? N1 C9 1.422(3) . ? N2 C1 1.317(3) . ? N2 C21 1.429(3) . ? C1 C2 1.483(3) . ? C2 C8 1.390(3) . ? C2 C3 1.395(3) . ? C3 C4 1.390(4) . ? C4 C5 1.373(4) . ? C5 C7 1.375(4) . ? C5 C6 1.524(4) . ? C7 C8 1.388(3) . ? C9 C10 1.401(3) . ? C9 C17 1.403(3) . ? C10 C14 1.387(4) . ? C10 C11 1.513(4) . ? C11 C12 1.529(4) . ? C11 C13 1.528(4) . ? C14 C15 1.363(5) . ? C15 C16 1.366(5) . ? C16 C17 1.401(4) . ? C17 C18 1.509(4) . ? C18 C19 1.521(5) . ? C18 C20 1.553(5) . ? C21 C22 1.400(4) . ? C21 C29 1.403(4) . ? C22 C26 1.403(4) . ? C22 C23 1.503(4) . ? C23 C24 1.529(5) . ? C23 C25 1.537(5) . ? C26 C27 1.370(5) . ? C27 C28 1.372(6) . ? C28 C29 1.380(4) . ? C29 C30 1.519(4) . ? C30 C31 1.496(7) . ? C30 C32 1.520(6) . ? 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 C1 N1 C9 129.9(2) . . ? C1 N2 C21 119.40(18) . . ? N2 C1 N1 120.4(2) . . ? N2 C1 C2 116.43(19) . . ? N1 C1 C2 123.1(2) . . ? C8 C2 C3 118.0(2) . . ? C8 C2 C1 122.4(2) . . ? C3 C2 C1 119.5(2) . . ? C4 C3 C2 119.8(3) . . ? C5 C4 C3 122.1(3) . . ? C4 C5 C7 118.0(3) . . ? C4 C5 C6 121.3(4) . . ? C7 C5 C6 120.6(4) . . ? C5 C7 C8 121.1(3) . . ? C7 C8 C2 121.0(3) . . ? C10 C9 C17 121.7(2) . . ? C10 C9 N1 121.7(2) . . ? C17 C9 N1 116.4(2) . . ? C14 C10 C9 117.8(3) . . ? C14 C10 C11 118.9(3) . . ? C9 C10 C11 123.1(2) . . ? C10 C11 C12 112.9(3) . . ? C10 C11 C13 110.5(3) . . ? C12 C11 C13 113.2(3) . . ? C15 C14 C10 121.6(3) . . ? C14 C15 C16 120.3(3) . . ? C15 C16 C17 121.6(3) . . ? C16 C17 C9 117.1(3) . . ? C16 C17 C18 122.4(3) . . ? C9 C17 C18 120.5(2) . . ? C17 C18 C19 114.4(4) . . ? C17 C18 C20 111.0(3) . . ? C19 C18 C20 111.5(4) . . ? C22 C21 C29 121.5(3) . . ? C22 C21 N2 119.7(2) . . ? C29 C21 N2 118.8(2) . . ? C26 C22 C21 117.1(3) . . ? C26 C22 C23 122.4(3) . . ? C21 C22 C23 120.4(2) . . ? C22 C23 C24 111.6(3) . . ? C22 C23 C25 115.6(4) . . ? C24 C23 C25 108.5(4) . . ? C27 C26 C22 121.2(4) . . ? C28 C27 C26 120.9(4) . . ? C27 C28 C29 120.3(4) . . ? C28 C29 C21 119.0(3) . . ? C28 C29 C30 120.6(3) . . ? C21 C29 C30 120.5(2) . . ? C31 C30 C32 112.5(5) . . ? C31 C30 C29 109.6(4) . . ? C32 C30 C29 113.9(4) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.157 _refine_diff_density_min -0.127 _refine_diff_density_rms 0.032 # ==== END