Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Juan Flores' _publ_contact_author_address ; Departamento de Quimica Inorganica Universidad de Alcala Campus Universitario Alcala de Henares Madrid 28871 SPAIN ; _publ_contact_author_email JUANC.FLORES@UAH.ES _publ_section_title ; Dendronized Scorpionate Complexes of Molybdenum in Low and High Oxidation States ; _publ_requested_category FM loop_ _publ_author_name 'Juan Flores' 'Ernesto de Jesus' 'Pilar Gomez-Sal' 'Alba M. Ortiz' 'Alberto Sanchez-Mendez' data_13 _database_code_depnum_ccdc_archive 'CCDC 652159' _audit_creation_date 2007-05-17T18:35:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H22 Mo1 N4 O4' _chemical_formula_sum 'C22 H22 Mo N4 O4' _chemical_formula_weight 502.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 12.651(5) _cell_length_b 12.999(5) _cell_length_c 13.437(5) _cell_angle_alpha 90 _cell_angle_beta 96.271(5) _cell_angle_gamma 90 _cell_volume 2196.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 253 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 20.809 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -5 -2 1 0.168 0 3 -4 0.092 2 -1 2 0.235 -1 8 5 0.038 0 -3 -2 0.167 -1 12 9 0.102 3 -8 4 0.187 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1094 _diffrn_reflns_av_unetI/netI 0.0479 _diffrn_reflns_number 42259 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 5053 _reflns_number_gt 4008 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.3255P] 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_number_reflns 5053 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.388 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.128 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.801751(16) 0.321460(15) -0.071067(15) 0.01900(8) Uani 1 1 d . . . N1 N 0.72518(16) 0.45114(15) 0.01556(15) 0.0206(4) Uani 1 1 d . . . N2 N 0.64487(16) 0.43611(14) 0.07709(15) 0.0191(4) Uani 1 1 d . . . N3 N 0.64610(16) 0.24249(15) -0.03756(15) 0.0205(4) Uani 1 1 d . . . N4 N 0.59372(16) 0.25906(15) 0.04615(14) 0.0198(4) Uani 1 1 d . . . O1 O 0.96648(18) 0.2300(2) 0.10242(17) 0.0512(6) Uani 1 1 d . . . O2 O 0.70590(17) 0.39946(18) -0.28750(15) 0.0436(5) Uani 1 1 d . . . O3 O 1.00642(16) 0.43100(18) -0.12979(17) 0.0440(5) Uani 1 1 d . . . O4 O 0.89048(17) 0.13950(16) -0.18930(16) 0.0404(5) Uani 1 1 d . . . C1 C 0.7296(2) 0.55361(18) 0.00300(18) 0.0227(5) Uani 1 1 d . . . C2 C 0.6556(2) 0.6032(2) 0.05783(19) 0.0258(5) Uani 1 1 d . . . C3 C 0.60306(19) 0.52759(18) 0.10418(18) 0.0216(5) Uani 1 1 d . . . C4 C 0.8013(3) 0.6029(2) -0.0646(2) 0.0337(6) Uani 1 1 d . . . C5 C 0.5164(2) 0.5364(2) 0.1718(2) 0.0293(6) Uani 1 1 d . . . C6 C 0.5880(2) 0.16959(18) -0.08979(18) 0.0229(5) Uani 1 1 d . . . C7 C 0.5017(2) 0.1390(2) -0.0390(2) 0.0262(5) Uani 1 1 d . . . C8 C 0.5069(2) 0.19660(19) 0.04679(19) 0.0240(5) Uani 1 1 d . . . C9 C 0.6137(3) 0.1294(3) -0.1893(2) 0.0350(7) Uani 1 1 d . . . C10 C 0.4362(3) 0.1958(3) 0.1289(3) 0.0396(7) Uani 1 1 d . . . C11 C 0.6274(2) 0.33669(18) 0.12205(18) 0.0211(5) Uani 1 1 d . . . C12 C 0.7202(3) 0.3035(2) 0.2007(2) 0.0319(6) Uani 1 1 d . . . C13 C 0.7196(2) 0.36795(19) 0.29449(19) 0.0251(5) Uani 1 1 d . . . C14 C 0.7698(2) 0.4633(2) 0.3038(2) 0.0349(6) Uani 1 1 d . . . C15 C 0.7593(3) 0.5237(2) 0.3883(3) 0.0454(9) Uani 1 1 d . . . C16 C 0.7026(3) 0.4896(3) 0.4628(2) 0.0468(8) Uani 1 1 d . . . C17 C 0.6545(3) 0.3955(3) 0.4551(2) 0.0444(8) Uani 1 1 d . . . C18 C 0.6626(3) 0.3344(2) 0.3715(2) 0.0340(6) Uani 1 1 d . . . C21 C 0.9007(2) 0.2638(2) 0.0461(2) 0.0302(6) Uani 1 1 d . . . C22 C 0.7325(2) 0.37383(19) -0.2072(2) 0.0253(5) Uani 1 1 d . . . C23 C 0.9297(2) 0.3930(2) -0.1050(2) 0.0283(6) Uani 1 1 d . . . C24 C 0.8551(2) 0.2066(2) -0.1449(2) 0.0275(6) Uani 1 1 d . . . H121 H 0.789(3) 0.313(3) 0.172(3) 0.059(11) Uiso 1 1 d . . . H53 H 0.538(3) 0.509(3) 0.239(3) 0.046(9) Uiso 1 1 d . . . H11 H 0.569(2) 0.3472(19) 0.158(2) 0.014(6) Uiso 1 1 d . . . H14 H 0.807(3) 0.482(2) 0.255(2) 0.034(8) Uiso 1 1 d . . . H17 H 0.613(3) 0.372(3) 0.510(3) 0.056(10) Uiso 1 1 d . . . H51 H 0.453(3) 0.497(3) 0.148(3) 0.060(11) Uiso 1 1 d . . . H7 H 0.452(2) 0.091(2) -0.060(2) 0.027(7) Uiso 1 1 d . . . H122 H 0.715(3) 0.231(3) 0.215(3) 0.049(10) Uiso 1 1 d . . . H92 H 0.683(3) 0.098(3) -0.181(3) 0.060(11) Uiso 1 1 d . . . H42 H 0.775(3) 0.582(3) -0.139(3) 0.063(11) Uiso 1 1 d . . . H18 H 0.628(2) 0.267(3) 0.368(2) 0.041(9) Uiso 1 1 d . . . H102 H 0.404(3) 0.265(3) 0.141(3) 0.057(11) Uiso 1 1 d . . . H3 H 0.639(2) 0.672(2) 0.056(2) 0.031(8) Uiso 1 1 d . . . H41 H 0.873(3) 0.581(3) -0.056(3) 0.055(11) Uiso 1 1 d . . . H103 H 0.472(3) 0.182(3) 0.189(4) 0.066(13) Uiso 1 1 d . . . H15 H 0.798(3) 0.578(4) 0.394(4) 0.084(14) Uiso 1 1 d . . . H43 H 0.796(3) 0.674(4) -0.061(3) 0.077(16) Uiso 1 1 d . . . H93 H 0.560(3) 0.089(3) -0.221(3) 0.057(11) Uiso 1 1 d . . . H91 H 0.637(3) 0.177(3) -0.231(3) 0.049(11) Uiso 1 1 d . . . H52 H 0.498(3) 0.598(3) 0.180(3) 0.057(11) Uiso 1 1 d . . . H101 H 0.380(3) 0.155(3) 0.111(3) 0.063(12) Uiso 1 1 d . . . H16 H 0.698(3) 0.534(4) 0.537(4) 0.092(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02156(12) 0.02049(12) 0.01568(12) -0.00014(8) 0.00537(8) 0.00166(8) N1 0.0245(10) 0.0214(10) 0.0164(10) -0.0005(8) 0.0039(8) -0.0001(8) N2 0.0219(10) 0.0179(10) 0.0178(10) -0.0010(8) 0.0039(8) 0.0012(8) N3 0.0257(11) 0.0204(10) 0.0161(10) -0.0007(8) 0.0059(8) 0.0016(8) N4 0.0270(10) 0.0193(10) 0.0143(10) -0.0018(8) 0.0077(8) 0.0001(8) O1 0.0412(13) 0.0739(17) 0.0368(13) 0.0077(12) -0.0044(10) 0.0164(12) O2 0.0477(13) 0.0590(14) 0.0240(11) 0.0106(10) 0.0031(9) 0.0102(11) O3 0.0321(11) 0.0552(14) 0.0463(13) 0.0059(11) 0.0113(10) -0.0098(10) O4 0.0527(13) 0.0308(10) 0.0412(12) -0.0069(9) 0.0207(10) 0.0082(10) C1 0.0256(12) 0.0220(12) 0.0203(12) 0.0007(10) 0.0012(10) -0.0006(10) C2 0.0346(14) 0.0160(12) 0.0267(14) -0.0004(10) 0.0034(11) 0.0037(11) C3 0.0242(12) 0.0222(12) 0.0178(12) -0.0014(9) 0.0004(10) 0.0047(10) C4 0.0449(18) 0.0243(14) 0.0342(16) 0.0017(12) 0.0148(13) -0.0038(13) C5 0.0319(15) 0.0266(14) 0.0308(15) -0.0030(12) 0.0102(12) 0.0059(12) C6 0.0287(13) 0.0209(12) 0.0188(12) -0.0019(9) 0.0015(10) 0.0007(10) C7 0.0269(13) 0.0248(13) 0.0267(14) -0.0005(11) 0.0026(11) -0.0051(11) C8 0.0257(13) 0.0216(13) 0.0255(13) 0.0031(10) 0.0062(11) -0.0009(10) C9 0.0424(18) 0.0392(17) 0.0246(15) -0.0125(13) 0.0092(13) -0.0070(15) C10 0.0424(18) 0.0443(19) 0.0351(18) -0.0022(14) 0.0188(15) -0.0105(15) C11 0.0280(13) 0.0198(12) 0.0161(12) -0.0013(9) 0.0055(10) 0.0002(10) C12 0.0461(17) 0.0291(15) 0.0195(13) -0.0021(11) -0.0012(12) 0.0132(12) C13 0.0313(14) 0.0236(13) 0.0199(13) -0.0003(10) -0.0005(10) 0.0054(10) C14 0.0339(15) 0.0350(15) 0.0341(16) 0.0121(13) -0.0043(13) -0.0046(12) C15 0.060(2) 0.0201(14) 0.049(2) -0.0024(13) -0.0285(17) -0.0066(14) C16 0.066(2) 0.0405(18) 0.0306(16) -0.0131(14) -0.0078(15) 0.0139(16) C17 0.0511(19) 0.060(2) 0.0226(15) -0.0059(14) 0.0078(14) 0.0012(16) C18 0.0466(17) 0.0335(16) 0.0214(14) -0.0008(11) 0.0012(12) -0.0094(13) C21 0.0328(14) 0.0344(15) 0.0246(14) 0.0013(11) 0.0084(12) 0.0015(12) C22 0.0251(12) 0.0254(13) 0.0270(14) -0.0024(10) 0.0105(11) 0.0023(10) C23 0.0291(14) 0.0316(14) 0.0242(13) 0.0009(11) 0.0034(11) 0.0018(11) C24 0.0306(14) 0.0289(13) 0.0238(13) 0.0033(11) 0.0076(11) 0.0008(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C24 1.954(3) . ? Mo1 C23 1.963(3) . ? Mo1 C21 2.044(3) . ? Mo1 C22 2.056(3) . ? Mo1 N3 2.308(2) . ? Mo1 N1 2.320(2) . ? N1 C1 1.344(3) . ? N1 N2 1.392(3) . ? N2 C3 1.367(3) . ? N2 C11 1.454(3) . ? N3 C6 1.348(3) . ? N3 N4 1.383(3) . ? N4 C8 1.366(3) . ? N4 C11 1.465(3) . ? O1 C21 1.149(3) . ? O2 C22 1.144(3) . ? O3 C23 1.170(3) . ? O4 C24 1.172(3) . ? C1 C2 1.409(4) . ? C1 C4 1.496(4) . ? C2 C3 1.373(4) . ? C3 C5 1.503(4) . ? C6 C7 1.407(4) . ? C6 C9 1.505(4) . ? C7 C8 1.370(4) . ? C8 C10 1.495(4) . ? C11 C12 1.552(4) . ? C12 C13 1.514(4) . ? C13 C14 1.392(4) . ? C13 C18 1.394(4) . ? C14 C15 1.398(5) . ? C15 C16 1.368(5) . ? C16 C17 1.364(5) . ? C17 C18 1.389(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 C24 Mo1 C23 84.51(11) . . ? C24 Mo1 C21 83.95(11) . . ? C23 Mo1 C21 84.35(11) . . ? C24 Mo1 C22 86.47(11) . . ? C23 Mo1 C22 85.33(11) . . ? C21 Mo1 C22 166.53(10) . . ? C24 Mo1 N3 96.24(9) . . ? C23 Mo1 N3 176.96(9) . . ? C21 Mo1 N3 98.65(9) . . ? C22 Mo1 N3 91.77(9) . . ? C24 Mo1 N1 175.37(9) . . ? C23 Mo1 N1 99.94(9) . . ? C21 Mo1 N1 97.70(9) . . ? C22 Mo1 N1 92.58(9) . . ? N3 Mo1 N1 79.25(7) . . ? C1 N1 N2 104.88(19) . . ? C1 N1 Mo1 129.16(16) . . ? N2 N1 Mo1 124.60(14) . . ? C3 N2 N1 111.40(18) . . ? C3 N2 C11 125.6(2) . . ? N1 N2 C11 121.70(18) . . ? C6 N3 N4 104.49(19) . . ? C6 N3 Mo1 129.74(16) . . ? N4 N3 Mo1 125.73(15) . . ? C8 N4 N3 111.67(19) . . ? C8 N4 C11 125.3(2) . . ? N3 N4 C11 123.00(19) . . ? N1 C1 C2 110.4(2) . . ? N1 C1 C4 122.5(2) . . ? C2 C1 C4 127.1(2) . . ? C3 C2 C1 107.0(2) . . ? N2 C3 C2 106.3(2) . . ? N2 C3 C5 123.8(2) . . ? C2 C3 C5 129.8(2) . . ? N3 C6 C7 110.7(2) . . ? N3 C6 C9 123.2(2) . . ? C7 C6 C9 126.0(2) . . ? C8 C7 C6 106.6(2) . . ? N4 C8 C7 106.5(2) . . ? N4 C8 C10 123.7(2) . . ? C7 C8 C10 129.7(3) . . ? N2 C11 N4 111.65(19) . . ? N2 C11 C12 113.1(2) . . ? N4 C11 C12 115.1(2) . . ? C13 C12 C11 109.9(2) . . ? C14 C13 C18 118.7(3) . . ? C14 C13 C12 121.6(3) . . ? C18 C13 C12 119.7(3) . . ? C13 C14 C15 119.3(3) . . ? C16 C15 C14 121.1(3) . . ? C17 C16 C15 120.0(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C13 120.7(3) . . ? O1 C21 Mo1 170.4(2) . . ? O2 C22 Mo1 171.2(2) . . ? O3 C23 Mo1 175.8(2) . . ? O4 C24 Mo1 177.6(2) . . ? # Attachment 'Compound_15.cif' # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-06-25 at 19:26:21 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : import dreduc struct sortav data_15 _database_code_depnum_ccdc_archive 'CCDC 652160' _audit_creation_date 2007-06-25T19:26:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H31 Mo1 N5 O3' _chemical_formula_sum 'C29 H31 Mo N5 O3' _chemical_formula_weight 593.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.280(5) _cell_length_b 12.284(5) _cell_length_c 19.122(5) _cell_angle_alpha 83.470(5) _cell_angle_beta 89.970(5) _cell_angle_gamma 89.760(5) _cell_volume 2865.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 20.29 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 1 4 0.158 3 -2 -5 0.114 3 -1 0 0.068 -3 1 0 0.125 0 -2 -1 0.03 0 1 0 0.064 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1312 _diffrn_reflns_av_unetI/netI 0.194 _diffrn_reflns_number 25236 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 13133 _reflns_number_gt 5790 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0925P)^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_number_reflns 13133 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1869 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.224 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0.079 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.365 _refine_diff_density_min -1.777 _refine_diff_density_rms 0.153 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.0612(6) 0.3331(7) 0.9606(4) 0.0384(19) Uani 1 1 d . . . C1B C 0.4382(6) 0.3334(6) 0.4603(4) 0.0334(17) Uani 1 1 d . . . C2A C 0.0354(6) 0.3631(7) 1.0275(4) 0.0376(19) Uani 1 1 d . . . H2A H -0.0291 0.3956 1.0402 0.045 Uiso 1 1 calc R . . C2B C 0.4635(6) 0.3629(7) 0.5269(4) 0.0369(19) Uani 1 1 d . . . H2B H 0.5277 0.3955 0.5395 0.044 Uiso 1 1 calc R . . C3A C 0.1228(6) 0.3356(7) 1.0704(4) 0.0328(18) Uani 1 1 d . . . C3B C 0.3777(6) 0.3357(6) 0.5700(4) 0.0333(17) Uani 1 1 d . . . C4A C -0.0067(6) 0.3501(8) 0.8959(4) 0.046(2) Uani 1 1 d . . . H4A1 H 0.0315 0.3228 0.8577 0.069 Uiso 1 1 calc R . . H4A2 H -0.0213 0.4269 0.8844 0.069 Uiso 1 1 calc R . . H4A3 H -0.0742 0.3115 0.9039 0.069 Uiso 1 1 calc R . . C4B C 0.5060(6) 0.3496(9) 0.3949(4) 0.051(2) Uani 1 1 d . . . H4B1 H 0.4678 0.3219 0.3569 0.076 Uiso 1 1 calc R . . H4B2 H 0.5738 0.311 0.4029 0.076 Uiso 1 1 calc R . . H4B3 H 0.52 0.4263 0.383 0.076 Uiso 1 1 calc R . . C5A C 0.1411(6) 0.3478(7) 1.1458(4) 0.042(2) Uani 1 1 d . . . H5A1 H 0.2117 0.3195 1.1597 0.063 Uiso 1 1 calc R . . H5A2 H 0.0863 0.308 1.1738 0.063 Uiso 1 1 calc R . . H5A3 H 0.1371 0.424 1.1527 0.063 Uiso 1 1 calc R . . C5B C 0.3588(7) 0.3484(8) 0.6462(4) 0.045(2) Uani 1 1 d . . . H5B1 H 0.2882 0.3206 0.66 0.067 Uiso 1 1 calc R . . H5B2 H 0.3627 0.4245 0.6529 0.067 Uiso 1 1 calc R . . H5B3 H 0.4136 0.3082 0.6743 0.067 Uiso 1 1 calc R . . C6A C 0.3504(6) -0.0018(7) 0.9875(4) 0.0340(18) Uani 1 1 d . . . C6B C 0.1500(6) -0.0018(7) 0.4864(4) 0.0356(18) Uani 1 1 d . . . C7A C 0.3790(6) -0.0301(6) 1.0576(4) 0.0334(17) Uani 1 1 d . . . H7A H 0.4018 -0.0986 1.0782 0.04 Uiso 1 1 calc R . . C7B C 0.1201(6) -0.0302(7) 0.5571(4) 0.0371(18) Uani 1 1 d . . . H7B H 0.0962 -0.0982 0.5777 0.045 Uiso 1 1 calc R . . C8A C 0.3670(6) 0.0643(6) 1.0910(4) 0.0341(18) Uani 1 1 d . . . C8B C 0.1335(6) 0.0634(6) 0.5899(4) 0.0286(16) Uani 1 1 d . . . C9A C 0.3511(7) -0.0746(6) 0.9280(5) 0.043(2) Uani 1 1 d . . . H9A1 H 0.3276 -0.0328 0.8852 0.065 Uiso 1 1 calc R . . H9A2 H 0.3027 -0.1351 0.9394 0.065 Uiso 1 1 calc R . . H9A3 H 0.4236 -0.1017 0.922 0.065 Uiso 1 1 calc R . . C9B C 0.1486(7) -0.0760(7) 0.4288(4) 0.043(2) Uani 1 1 d . . . H9B1 H 0.1724 -0.036 0.3855 0.064 Uiso 1 1 calc R . . H9B2 H 0.0759 -0.1022 0.4232 0.064 Uiso 1 1 calc R . . H9B3 H 0.1966 -0.1371 0.4411 0.064 Uiso 1 1 calc R . . C10A C 0.3899(7) 0.0837(8) 1.1658(4) 0.045(2) Uani 1 1 d . . . H10A H 0.372 0.1581 1.1721 0.068 Uiso 1 1 calc R . . H10B H 0.4657 0.0706 1.1759 0.068 Uiso 1 1 calc R . . H10C H 0.3467 0.0349 1.1971 0.068 Uiso 1 1 calc R . . C10B C 0.1092(7) 0.0819(8) 0.6648(4) 0.046(2) Uani 1 1 d . . . H10D H 0.127 0.156 0.6717 0.069 Uiso 1 1 calc R . . H10E H 0.1517 0.0322 0.6962 0.069 Uiso 1 1 calc R . . H10F H 0.0332 0.0695 0.6743 0.069 Uiso 1 1 calc R . . C11A C 0.3106(5) 0.2601(6) 1.0502(4) 0.0271(16) Uani 1 1 d . . . C11B C 0.1901(5) 0.2593(6) 0.5498(4) 0.0276(17) Uani 1 1 d . . . H11B H 0.1859 0.2638 0.6006 0.033 Uiso 1 1 calc R . . C12A C 0.3946(6) 0.3406(7) 1.0151(4) 0.0336(18) Uani 1 1 d . . . C12B C 0.1053(6) 0.3409(7) 0.5154(4) 0.0310(17) Uani 1 1 d . . . C13A C 0.3627(6) 0.4596(7) 1.0200(4) 0.0344(18) Uani 1 1 d . . . C13B C 0.1379(6) 0.4599(6) 0.5201(4) 0.0306(17) Uani 1 1 d . . . C14A C 0.3804(6) 0.5094(7) 1.0813(4) 0.0394(19) Uani 1 1 d . . . H14A H 0.4168 0.4712 1.1191 0.047 Uiso 1 1 calc R . . C14B C 0.1197(6) 0.5093(7) 0.5819(4) 0.0378(19) Uani 1 1 d . . . H14B H 0.0844 0.4709 0.62 0.045 Uiso 1 1 calc R . . C15A C 0.3431(7) 0.6173(7) 1.0860(5) 0.045(2) Uani 1 1 d . . . H15A H 0.3559 0.6501 1.1267 0.054 Uiso 1 1 calc R . . C15B C 0.1549(7) 0.6164(7) 0.5855(4) 0.045(2) Uani 1 1 d . . . H15B H 0.1407 0.6495 0.6259 0.054 Uiso 1 1 calc R . . C16A C 0.2880(7) 0.6744(7) 1.0306(5) 0.045(2) Uani 1 1 d . . . H16A H 0.2607 0.744 1.0349 0.054 Uiso 1 1 calc R . . C16B C 0.2109(7) 0.6749(7) 0.5298(5) 0.049(2) Uani 1 1 d . . . H16B H 0.238 0.7444 0.5341 0.059 Uiso 1 1 calc R . . C17A C 0.2728(6) 0.6270(7) 0.9670(4) 0.0388(19) Uani 1 1 d . . . H17A H 0.2391 0.6666 0.9285 0.047 Uiso 1 1 calc R . . C17B C 0.2254(7) 0.6267(7) 0.4670(4) 0.041(2) Uani 1 1 d . . . H17B H 0.2583 0.6662 0.4283 0.05 Uiso 1 1 calc R . . C18A C 0.3094(6) 0.5197(7) 0.9630(4) 0.0347(18) Uani 1 1 d . . . H18A H 0.2982 0.4876 0.9219 0.042 Uiso 1 1 calc R . . C18B C 0.1905(6) 0.5196(7) 0.4630(4) 0.0370(19) Uani 1 1 d . . . H18B H 0.2022 0.4875 0.4219 0.044 Uiso 1 1 calc R . . C21A C 0.3613(7) 0.3089(7) 0.8459(4) 0.0355(19) Uani 1 1 d . . . C21B C 0.1387(6) 0.3074(7) 0.3465(4) 0.0326(18) Uani 1 1 d . . . C22A C 0.3187(6) 0.1240(6) 0.8040(4) 0.0315(17) Uani 1 1 d . . . C22B C 0.3251(6) 0.2742(7) 0.2928(4) 0.0364(18) Uani 1 1 d . . . C23A C 0.1735(6) 0.2749(7) 0.7931(4) 0.0355(18) Uani 1 1 d . . . C23B C 0.1827(6) 0.1241(7) 0.3039(4) 0.0361(18) Uani 1 1 d . . . C24A C 0.0324(7) 0.0250(7) 0.9017(4) 0.0382(19) Uani 1 1 d . . . C24B C 0.4661(7) 0.0251(8) 0.4011(4) 0.045(2) Uani 1 1 d . . . C25A C -0.0639(9) -0.0471(9) 0.9065(5) 0.074(3) Uani 1 1 d . . . H25A H -0.0647 -0.0889 0.8671 0.111 Uiso 1 1 calc R . . H25B H -0.1288 -0.0033 0.9062 0.111 Uiso 1 1 calc R . . H25C H -0.0606 -0.0959 0.9494 0.111 Uiso 1 1 calc R . . C25B C 0.5648(9) -0.0458(10) 0.4066(6) 0.076(4) Uani 1 1 d . . . H25D H 0.6223 -0.0101 0.379 0.114 Uiso 1 1 calc R . . H25E H 0.5485 -0.1145 0.3896 0.114 Uiso 1 1 calc R . . H25F H 0.5873 -0.0586 0.455 0.114 Uiso 1 1 calc R . . C31A C 0.2579(8) 0.5937(8) 0.7762(4) 0.050(2) Uani 1 1 d . . . H31A H 0.265 0.5178 0.7812 0.06 Uiso 1 1 calc R . . C31B C 0.2426(8) 0.5926(8) 0.2756(5) 0.053(3) Uani 1 1 d . . . H31B H 0.2358 0.5168 0.2798 0.063 Uiso 1 1 calc R . . C32A C 0.1536(8) 0.6409(9) 0.7736(5) 0.056(3) Uani 1 1 d . . . H32A H 0.092 0.597 0.7748 0.067 Uiso 1 1 calc R . . C32B C 0.1531(8) 0.6568(11) 0.2715(5) 0.065(3) Uani 1 1 d . . . H32B H 0.0842 0.6256 0.2718 0.078 Uiso 1 1 calc R . . C33A C 0.1438(8) 0.7524(10) 0.7692(6) 0.064(3) Uani 1 1 d . . . H33A H 0.0749 0.7844 0.7679 0.077 Uiso 1 1 calc R . . C33B C 0.1645(11) 0.7718(12) 0.2667(6) 0.084(4) Uani 1 1 d . . . H33B H 0.1031 0.8167 0.2637 0.101 Uiso 1 1 calc R . . C34A C 0.2340(11) 0.8175(9) 0.7666(7) 0.082(4) Uani 1 1 d . . . H34A H 0.227 0.8931 0.765 0.098 Uiso 1 1 calc R . . C34B C 0.2698(11) 0.8187(10) 0.2666(6) 0.083(4) Uani 1 1 d . . . H34B H 0.2779 0.8942 0.2649 0.1 Uiso 1 1 calc R . . C35A C 0.3385(9) 0.7681(13) 0.7665(6) 0.084(4) Uani 1 1 d . . . H35A H 0.4009 0.8109 0.763 0.101 Uiso 1 1 calc R . . C35B C 0.3591(8) 0.7520(10) 0.2691(6) 0.069(3) Uani 1 1 d . . . H35B H 0.4288 0.7816 0.2677 0.083 Uiso 1 1 calc R . . C36A C 0.3458(8) 0.6544(11) 0.7716(5) 0.061(3) Uani 1 1 d . . . H36A H 0.4139 0.6211 0.7718 0.074 Uiso 1 1 calc R . . C36B C 0.3446(7) 0.6399(8) 0.2737(5) 0.048(2) Uani 1 1 d . . . H36B H 0.4057 0.5946 0.2755 0.058 Uiso 1 1 calc R . . N1A N 0.1614(4) 0.2884(5) 0.9610(3) 0.0274(13) Uani 1 1 d . . . N1B N 0.3391(5) 0.2886(5) 0.4610(3) 0.0297(14) Uani 1 1 d . . . N2A N 0.1974(4) 0.2890(5) 1.0290(3) 0.0255(13) Uani 1 1 d . . . N2B N 0.3019(4) 0.2882(5) 0.5288(3) 0.0244(13) Uani 1 1 d . . . N3A N 0.3205(5) 0.1066(5) 0.9750(3) 0.0296(14) Uani 1 1 d . . . N3B N 0.1796(5) 0.1056(5) 0.4751(3) 0.0311(14) Uani 1 1 d . . . N4A N 0.3303(4) 0.1438(5) 1.0398(3) 0.0264(13) Uani 1 1 d . . . N4B N 0.1695(4) 0.1451(5) 0.5400(3) 0.0295(14) Uani 1 1 d . . . N5A N 0.1071(5) 0.0807(5) 0.8959(3) 0.0337(15) Uani 1 1 d . . . N5B N 0.3925(5) 0.0791(6) 0.3969(3) 0.0387(16) Uani 1 1 d . . . O1A O 0.4266(5) 0.3702(5) 0.8205(3) 0.0474(15) Uani 1 1 d . . . O1B O 0.0733(5) 0.3695(5) 0.3202(3) 0.0507(16) Uani 1 1 d . . . O2A O 0.3675(5) 0.0843(5) 0.7606(3) 0.0502(16) Uani 1 1 d . . . O2B O 0.3693(5) 0.3205(6) 0.2404(3) 0.0504(16) Uani 1 1 d . . . O3A O 0.1309(5) 0.3205(5) 0.7401(3) 0.0457(15) Uani 1 1 d . . . O3B O 0.1328(5) 0.0848(5) 0.2604(3) 0.0531(16) Uani 1 1 d . . . Mo1 Mo 0.24651(5) 0.20139(5) 0.87366(3) 0.02682(18) Uani 1 1 d . . . Mo2 Mo 0.25356(5) 0.20143(5) 0.37363(3) 0.02736(19) Uani 1 1 d . . . H1A H 0.313(5) 0.253(5) 1.101(3) 0.014(16) Uiso 1 1 d . . . H12A H 0.465(6) 0.332(6) 1.043(4) 0.026(19) Uiso 1 1 d . . . H12B H 0.091(4) 0.332(5) 0.464(3) 0.005(14) Uiso 1 1 d . . . H3A H 0.403(5) 0.339(6) 0.965(4) 0.023(18) Uiso 1 1 d . . . H3B H 0.041(6) 0.324(6) 0.533(4) 0.021(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.027(4) 0.047(5) 0.040(5) -0.004(4) 0.005(3) 0.002(4) C1B 0.034(4) 0.036(5) 0.031(4) -0.002(3) 0.001(3) -0.005(3) C2A 0.031(4) 0.043(5) 0.037(4) 0.002(4) 0.005(3) 0.016(4) C2B 0.032(4) 0.036(5) 0.043(5) -0.009(4) -0.007(3) -0.006(4) C3A 0.025(4) 0.036(5) 0.038(5) -0.008(4) 0.002(3) 0.003(3) C3B 0.029(4) 0.029(4) 0.041(5) -0.001(3) 0.000(3) -0.002(3) C4A 0.022(4) 0.067(6) 0.049(5) -0.009(5) -0.008(3) 0.010(4) C4B 0.028(4) 0.086(7) 0.039(5) -0.010(5) 0.009(3) -0.006(4) C5A 0.036(4) 0.046(5) 0.043(5) -0.002(4) 0.014(4) 0.010(4) C5B 0.041(5) 0.055(6) 0.040(5) -0.014(4) -0.011(4) -0.004(4) C6A 0.028(4) 0.040(5) 0.035(4) -0.008(4) 0.001(3) -0.002(3) C6B 0.033(4) 0.034(5) 0.041(5) -0.008(4) -0.001(3) 0.004(3) C7A 0.045(5) 0.021(4) 0.033(4) -0.001(3) -0.005(3) 0.012(3) C7B 0.035(4) 0.033(5) 0.043(5) -0.001(4) 0.003(3) -0.002(3) C8A 0.031(4) 0.026(4) 0.045(5) -0.003(4) 0.000(3) 0.002(3) C8B 0.025(4) 0.033(4) 0.026(4) 0.002(3) 0.002(3) -0.003(3) C9A 0.055(5) 0.020(4) 0.056(6) -0.008(4) 0.002(4) 0.001(4) C9B 0.053(5) 0.026(4) 0.051(5) -0.013(4) 0.003(4) -0.001(4) C10A 0.051(5) 0.055(6) 0.027(4) 0.006(4) -0.005(4) 0.017(4) C10B 0.050(5) 0.048(6) 0.038(5) 0.005(4) 0.003(4) -0.009(4) C11A 0.022(4) 0.032(4) 0.025(4) 0.005(3) -0.001(3) 0.007(3) C11B 0.021(3) 0.034(4) 0.028(4) -0.008(3) -0.003(3) -0.002(3) C12A 0.019(4) 0.048(5) 0.036(5) -0.015(4) 0.000(3) 0.000(3) C12B 0.017(4) 0.038(5) 0.039(5) -0.010(4) 0.002(3) 0.001(3) C13A 0.026(4) 0.039(5) 0.038(4) -0.003(4) 0.010(3) -0.001(3) C13B 0.023(4) 0.030(4) 0.040(4) -0.008(3) -0.001(3) 0.003(3) C14A 0.037(4) 0.043(5) 0.037(5) 0.003(4) -0.002(3) -0.008(4) C14B 0.034(4) 0.039(5) 0.038(5) 0.003(4) 0.005(3) 0.006(4) C15A 0.058(6) 0.032(5) 0.047(5) -0.009(4) 0.003(4) -0.008(4) C15B 0.059(6) 0.039(5) 0.040(5) -0.014(4) -0.001(4) 0.015(4) C16A 0.041(5) 0.029(5) 0.064(6) 0.000(4) 0.014(4) 0.004(4) C16B 0.046(5) 0.026(5) 0.074(7) -0.005(4) -0.005(5) 0.004(4) C17A 0.039(5) 0.033(5) 0.045(5) -0.004(4) -0.002(4) 0.001(4) C17B 0.044(5) 0.036(5) 0.042(5) 0.004(4) 0.000(4) 0.000(4) C18A 0.032(4) 0.042(5) 0.031(4) -0.004(4) 0.002(3) 0.003(4) C18B 0.035(4) 0.038(5) 0.037(5) -0.001(4) -0.007(3) 0.004(4) C21A 0.045(5) 0.045(5) 0.018(4) -0.010(4) 0.000(3) 0.019(4) C21B 0.028(4) 0.043(5) 0.028(4) -0.011(4) 0.007(3) -0.011(4) C22A 0.035(4) 0.032(4) 0.029(4) -0.008(3) 0.003(3) -0.002(3) C22B 0.030(4) 0.039(5) 0.040(5) 0.001(4) -0.006(3) 0.010(4) C23A 0.030(4) 0.036(5) 0.041(5) -0.006(4) 0.004(3) -0.001(3) C23B 0.038(4) 0.037(5) 0.033(4) 0.001(4) 0.012(3) 0.004(4) C24A 0.040(5) 0.037(5) 0.039(5) -0.009(4) -0.003(4) -0.010(4) C24B 0.044(5) 0.047(5) 0.044(5) -0.006(4) 0.002(4) 0.016(4) C25A 0.081(8) 0.080(8) 0.060(7) 0.000(6) -0.004(5) -0.058(7) C25B 0.071(7) 0.089(9) 0.066(7) -0.007(6) -0.004(5) 0.057(7) C31A 0.055(6) 0.050(6) 0.042(5) 0.002(4) -0.003(4) 0.014(5) C31B 0.062(6) 0.055(6) 0.041(5) -0.007(5) 0.014(4) -0.023(5) C32A 0.050(6) 0.068(7) 0.048(6) 0.002(5) -0.003(4) -0.003(5) C32B 0.031(5) 0.108(11) 0.057(7) -0.007(6) 0.008(4) -0.002(6) C33A 0.043(6) 0.067(8) 0.083(8) -0.018(6) -0.004(5) 0.014(5) C33B 0.090(9) 0.095(10) 0.064(7) 0.008(7) 0.019(6) 0.056(8) C34A 0.105(10) 0.040(7) 0.102(9) -0.015(6) -0.038(8) 0.008(7) C34B 0.103(10) 0.056(8) 0.092(9) -0.016(7) 0.044(8) -0.017(7) C35A 0.048(6) 0.120(12) 0.080(8) 0.009(8) -0.018(6) -0.035(7) C35B 0.047(6) 0.079(9) 0.084(8) -0.024(7) 0.022(5) -0.009(6) C36A 0.032(5) 0.095(10) 0.056(6) -0.009(6) -0.001(4) 0.001(6) C36B 0.042(5) 0.057(7) 0.046(5) -0.003(5) -0.004(4) 0.005(5) N1A 0.019(3) 0.037(4) 0.026(3) -0.005(3) -0.001(2) 0.004(3) N1B 0.027(3) 0.038(4) 0.025(3) -0.005(3) 0.002(2) 0.000(3) N2A 0.022(3) 0.028(3) 0.028(3) -0.008(3) -0.001(2) 0.001(2) N2B 0.022(3) 0.026(3) 0.025(3) -0.001(3) -0.005(2) 0.000(2) N3A 0.032(3) 0.019(3) 0.038(4) -0.007(3) -0.001(3) 0.004(3) N3B 0.026(3) 0.027(4) 0.040(4) -0.002(3) 0.002(3) 0.000(3) N4A 0.024(3) 0.025(3) 0.030(3) -0.001(3) -0.001(2) 0.005(2) N4B 0.023(3) 0.029(3) 0.037(4) -0.006(3) 0.000(2) -0.004(3) N5A 0.036(4) 0.036(4) 0.030(3) -0.006(3) 0.000(3) -0.002(3) N5B 0.035(4) 0.040(4) 0.041(4) -0.002(3) 0.003(3) 0.012(3) O1A 0.038(3) 0.053(4) 0.050(4) 0.000(3) 0.013(3) -0.016(3) O1B 0.044(3) 0.055(4) 0.052(4) -0.002(3) -0.007(3) 0.025(3) O2A 0.058(4) 0.051(4) 0.042(4) -0.008(3) 0.011(3) 0.012(3) O2B 0.042(3) 0.069(5) 0.038(3) -0.001(3) 0.007(3) 0.000(3) O3A 0.044(3) 0.055(4) 0.035(3) 0.003(3) 0.000(3) 0.007(3) O3B 0.063(4) 0.049(4) 0.048(4) -0.006(3) -0.013(3) -0.002(3) Mo1 0.0244(3) 0.0266(4) 0.0295(4) -0.0035(3) 0.0011(3) 0.0005(3) Mo2 0.0242(3) 0.0278(4) 0.0301(4) -0.0035(3) 0.0002(3) 0.0039(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1A N1A 1.346(9) . ? C1A C2A 1.406(11) . ? C1A C4A 1.487(11) . ? C1B N1B 1.337(9) . ? C1B C2B 1.400(10) . ? C1B C4B 1.496(10) . ? C2A C3A 1.369(10) . ? C2B C3B 1.356(11) . ? C3A N2A 1.376(9) . ? C3A C5A 1.483(11) . ? C3B N2B 1.391(9) . ? C3B C5B 1.501(11) . ? C6A N3A 1.375(10) . ? C6A C7A 1.390(10) . ? C6A C9A 1.526(10) . ? C6B N3B 1.363(10) . ? C6B C7B 1.406(11) . ? C6B C9B 1.509(10) . ? C7A C8A 1.393(10) . ? C7B C8B 1.381(11) . ? C8A N4A 1.376(9) . ? C8A C10A 1.504(11) . ? C8B N4B 1.379(9) . ? C8B C10B 1.505(10) . ? C11A N2A 1.479(8) . ? C11A N4A 1.484(9) . ? C11A C12A 1.533(11) . ? C11B N4B 1.460(9) . ? C11B N2B 1.465(8) . ? C11B C12B 1.537(10) . ? C12A C13A 1.525(11) . ? C12B C13B 1.530(11) . ? C13A C14A 1.399(11) . ? C13A C18A 1.405(11) . ? C13B C18B 1.403(11) . ? C13B C14B 1.406(10) . ? C14A C15A 1.414(12) . ? C14B C15B 1.396(12) . ? C15A C16A 1.378(12) . ? C15B C16B 1.398(13) . ? C16A C17A 1.419(12) . ? C16B C17B 1.409(12) . ? C17A C18A 1.401(11) . ? C17B C18B 1.396(11) . ? C21A O1A 1.169(10) . ? C21A Mo1 1.967(9) . ? C21B O1B 1.178(9) . ? C21B Mo2 1.946(8) . ? C22A O2A 1.174(8) . ? C22A Mo1 1.934(7) . ? C22B O2B 1.222(10) . ? C22B Mo2 1.911(9) . ? C23A O3A 1.218(9) . ? C23A Mo1 1.916(8) . ? C23B O3B 1.180(9) . ? C23B Mo2 1.933(9) . ? C24A N5A 1.145(9) . ? C24A C25A 1.476(12) . ? C24B N5B 1.116(9) . ? C24B C25B 1.487(12) . ? C31A C36A 1.312(13) . ? C31A C32A 1.402(12) . ? C31B C32B 1.347(14) . ? C31B C36B 1.381(12) . ? C32A C33A 1.368(15) . ? C32B C33B 1.413(17) . ? C33A C34A 1.366(16) . ? C33B C34B 1.418(18) . ? C34A C35A 1.416(17) . ? C34B C35B 1.364(16) . ? C35A C36A 1.392(17) . ? C35B C36B 1.383(15) . ? N1A N2A 1.373(8) . ? N1A Mo1 2.328(6) . ? N1B N2B 1.374(8) . ? N1B Mo2 2.336(6) . ? N3A N4A 1.374(8) . ? N3A Mo1 2.327(6) . ? N3B N4B 1.389(8) . ? N3B Mo2 2.337(6) . ? N5A Mo1 2.278(7) . ? N5B Mo2 2.279(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 N1A C1A C2A 110.4(7) . . ? N1A C1A C4A 122.3(7) . . ? C2A C1A C4A 127.3(7) . . ? N1B C1B C2B 110.1(6) . . ? N1B C1B C4B 122.1(7) . . ? C2B C1B C4B 127.7(7) . . ? C3A C2A C1A 107.4(7) . . ? C3B C2B C1B 107.9(7) . . ? C2A C3A N2A 105.3(6) . . ? C2A C3A C5A 131.1(7) . . ? N2A C3A C5A 123.6(6) . . ? C2B C3B N2B 105.6(7) . . ? C2B C3B C5B 131.5(7) . . ? N2B C3B C5B 122.9(7) . . ? N3A C6A C7A 111.5(6) . . ? N3A C6A C9A 120.6(7) . . ? C7A C6A C9A 127.9(7) . . ? N3B C6B C7B 110.7(7) . . ? N3B C6B C9B 122.8(7) . . ? C7B C6B C9B 126.4(7) . . ? C6A C7A C8A 106.6(7) . . ? C8B C7B C6B 106.0(7) . . ? N4A C8A C7A 105.5(6) . . ? N4A C8A C10A 124.1(7) . . ? C7A C8A C10A 130.3(7) . . ? N4B C8B C7B 107.7(6) . . ? N4B C8B C10B 123.1(7) . . ? C7B C8B C10B 129.2(7) . . ? N2A C11A N4A 108.5(6) . . ? N2A C11A C12A 113.1(6) . . ? N4A C11A C12A 114.6(6) . . ? N4B C11B N2B 109.8(6) . . ? N4B C11B C12B 114.5(6) . . ? N2B C11B C12B 113.0(6) . . ? C13A C12A C11A 112.1(6) . . ? C13B C12B C11B 112.1(6) . . ? C14A C13A C18A 118.7(7) . . ? C14A C13A C12A 121.6(7) . . ? C18A C13A C12A 119.5(7) . . ? C18B C13B C14B 119.3(7) . . ? C18B C13B C12B 119.8(7) . . ? C14B C13B C12B 120.9(7) . . ? C13A C14A C15A 120.4(8) . . ? C15B C14B C13B 119.5(8) . . ? C16A C15A C14A 120.4(8) . . ? C14B C15B C16B 121.6(8) . . ? C15A C16A C17A 120.2(8) . . ? C15B C16B C17B 118.8(8) . . ? C18A C17A C16A 118.9(8) . . ? C18B C17B C16B 119.9(8) . . ? C17A C18A C13A 121.3(7) . . ? C17B C18B C13B 120.9(8) . . ? O1A C21A Mo1 171.2(6) . . ? O1B C21B Mo2 170.2(6) . . ? O2A C22A Mo1 174.7(7) . . ? O2B C22B Mo2 178.9(7) . . ? O3A C23A Mo1 177.1(6) . . ? O3B C23B Mo2 173.9(7) . . ? N5A C24A C25A 178.0(9) . . ? N5B C24B C25B 179.4(11) . . ? C36A C31A C32A 121.3(10) . . ? C32B C31B C36B 119.8(10) . . ? C33A C32A C31A 119.1(10) . . ? C31B C32B C33B 119.6(10) . . ? C34A C33A C32A 120.8(10) . . ? C32B C33B C34B 119.8(10) . . ? C33A C34A C35A 119.1(11) . . ? C35B C34B C33B 119.3(11) . . ? C36A C35A C34A 118.8(11) . . ? C34B C35B C36B 119.1(10) . . ? C31A C36A C35A 120.9(10) . . ? C31B C36B C35B 122.3(10) . . ? C1A N1A N2A 104.7(5) . . ? C1A N1A Mo1 128.6(5) . . ? N2A N1A Mo1 126.0(4) . . ? C1B N1B N2B 105.6(5) . . ? C1B N1B Mo2 128.8(5) . . ? N2B N1B Mo2 124.9(4) . . ? N1A N2A C3A 112.3(5) . . ? N1A N2A C11A 122.4(5) . . ? C3A N2A C11A 124.5(6) . . ? N1B N2B C3B 110.8(6) . . ? N1B N2B C11B 123.0(5) . . ? C3B N2B C11B 125.4(6) . . ? N4A N3A C6A 103.5(6) . . ? N4A N3A Mo1 126.9(4) . . ? C6A N3A Mo1 129.1(5) . . ? C6B N3B N4B 105.3(6) . . ? C6B N3B Mo2 128.7(5) . . ? N4B N3B Mo2 125.6(5) . . ? N3A N4A C8A 112.9(6) . . ? N3A N4A C11A 122.0(6) . . ? C8A N4A C11A 125.0(6) . . ? C8B N4B N3B 110.3(6) . . ? C8B N4B C11B 127.1(6) . . ? N3B N4B C11B 122.6(6) . . ? C24A N5A Mo1 173.6(6) . . ? C24B N5B Mo2 171.6(7) . . ? C23A Mo1 C22A 83.3(3) . . ? C23A Mo1 C21A 83.0(3) . . ? C22A Mo1 C21A 81.6(3) . . ? C23A Mo1 N5A 92.0(3) . . ? C22A Mo1 N5A 96.4(3) . . ? C21A Mo1 N5A 174.8(3) . . ? C23A Mo1 N3A 175.0(3) . . ? C22A Mo1 N3A 99.1(3) . . ? C21A Mo1 N3A 101.7(3) . . ? N5A Mo1 N3A 83.4(2) . . ? C23A Mo1 N1A 98.9(3) . . ? C22A Mo1 N1A 177.6(3) . . ? C21A Mo1 N1A 99.6(2) . . ? N5A Mo1 N1A 82.6(2) . . ? N3A Mo1 N1A 78.6(2) . . ? C22B Mo2 C23B 82.6(3) . . ? C22B Mo2 C21B 83.1(3) . . ? C23B Mo2 C21B 81.7(3) . . ? C22B Mo2 N5B 92.9(3) . . ? C23B Mo2 N5B 96.2(3) . . ? C21B Mo2 N5B 175.7(3) . . ? C22B Mo2 N1B 99.2(3) . . ? C23B Mo2 N1B 177.8(3) . . ? C21B Mo2 N1B 99.8(3) . . ? N5B Mo2 N1B 82.5(2) . . ? C22B Mo2 N3B 175.3(3) . . ? C23B Mo2 N3B 98.9(3) . . ? C21B Mo2 N3B 101.4(3) . . ? N5B Mo2 N3B 82.6(2) . . ? N1B Mo2 N3B 79.2(2) . . ?