# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'John Errington' _publ_contact_author_name 'John Errington' _publ_contact_author_address ; Bedson Building Newcastle upon Tyne NE1 7RU ; _publ_contact_author_email John.Errington@ncl.ac.uk # Attachment '- TiMo5.cif' data_rje253_salt_of_3 _database_code_depnum_ccdc_archive 'CCDC 832952' #TrackingRef '- TiMo5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C16 H36 N +,C H3 Mo5 O19 Ti 3-' _chemical_formula_sum 'C49 H111 Mo5 N3 O19 Ti' _chemical_formula_weight 1574.01 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' Ti Ti 0.2776 0.4457 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.4619(7) _cell_length_b 18.6123(7) _cell_length_c 27.2737(9) _cell_angle_alpha 90.00 _cell_angle_beta 113.343(2) _cell_angle_gamma 90.00 _cell_volume 13731.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 42495 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.69 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6480 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 0.665 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48667 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12093 _reflns_number_gt 11036 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0240P)^2^+192.2561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12093 _refine_ls_number_parameters 756 _refine_ls_number_restraints 261 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1389 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 1.273 _refine_ls_restrained_S_all 1.266 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.23780(3) 0.36347(4) 0.52153(3) 0.02334(16) Uani 0.50 1 d P A 1 Mo1 Mo 0.23780(3) 0.36347(4) 0.52153(3) 0.02334(16) Uani 0.50 1 d P A 2 Mo2 Mo 0.335276(19) 0.26782(3) 0.53819(2) 0.02560(14) Uani 1 1 d . . . Mo3 Mo 0.25234(2) 0.20958(3) 0.58219(2) 0.02607(14) Uani 1 1 d . . . Ti2 Ti 0.08215(3) 0.25035(5) 0.77724(3) 0.0395(2) Uani 0.50 1 d P . 1 Mo4 Mo 0.08215(3) 0.25035(5) 0.77724(3) 0.0395(2) Uani 0.50 1 d P . 2 Mo5 Mo -0.00508(2) 0.34041(3) 0.68767(3) 0.03745(16) Uani 1 1 d . . . Mo6 Mo -0.00560(3) 0.16360(4) 0.68726(3) 0.0544(2) Uani 1 1 d . . . O1 O 0.25787(17) 0.1795(2) 0.64291(17) 0.0327(10) Uani 1 1 d . . . O2 O 0.18469(15) 0.2026(2) 0.53887(16) 0.0265(9) Uani 1 1 d . . . O3 O 0.32400(14) 0.2324(2) 0.59686(15) 0.0241(9) Uani 1 1 d . . . O4 O 0.39719(15) 0.2817(3) 0.56216(17) 0.0331(10) Uani 1 1 d . . . O5 O 0.30965(15) 0.3582(2) 0.54578(16) 0.0268(9) Uani 1 1 d . . . O6 O 0.23564(15) 0.3756(2) 0.45039(16) 0.0266(9) Uani 1 1 d . . . O7 O 0.22842(17) 0.4495(2) 0.54113(19) 0.0363(11) Uani 1 1 d . . . O8 O 0.17145(15) 0.3276(2) 0.48999(17) 0.0273(9) Uani 1 1 d . . . O9 O 0.24556(16) 0.3107(2) 0.58660(17) 0.0287(10) Uani 1 1 d . . . O10 O 0.2500 0.2500 0.5000 0.0234(12) Uani 1 2 d S . . O12 O 0.06347(18) 0.3240(3) 0.7222(2) 0.0426(12) Uani 1 1 d . . . O15 O 0.0000 0.3969(4) 0.7500 0.052(2) Uani 1 2 d S . . O16 O -0.0087(2) 0.2511(3) 0.6489(2) 0.0501(14) Uani 1 1 d . . . O17 O -0.0718(2) 0.1793(4) 0.6778(2) 0.070(2) Uani 1 1 d . . . O19 O 0.0000 0.1078(4) 0.7500 0.069(3) Uani 1 2 d S . . O20 O 0.0629(2) 0.1801(3) 0.7210(2) 0.0518(14) Uani 1 1 d . . . O21 O 0.0000 0.2520(3) 0.7500 0.0304(14) Uani 1 2 d S . . C1 C 0.2060(6) 0.4752(10) 0.5782(8) 0.062(5) Uani 0.50 1 d P A 1 H1A H 0.2073 0.5278 0.5799 0.093 Uiso 0.50 1 calc PR A 1 H1B H 0.2244 0.4554 0.6139 0.093 Uiso 0.50 1 calc PR A 1 H1C H 0.1715 0.4593 0.5652 0.093 Uiso 0.50 1 calc PR A 1 C2 C 0.1975(7) 0.2446(11) 0.8398(9) 0.081(7) Uani 0.50 1 d P . 1 H2A H 0.2203 0.2525 0.8221 0.121 Uiso 0.50 1 calc PR . 1 H2B H 0.2026 0.1963 0.8553 0.121 Uiso 0.50 1 calc PR . 1 H2C H 0.2038 0.2804 0.8681 0.121 Uiso 0.50 1 calc PR . 1 N1 N -0.0661(2) 0.7282(4) 0.4390(2) 0.0482(16) Uani 1 1 d D . . C3 C -0.0792(3) 0.8037(4) 0.4498(3) 0.0490(19) Uani 1 1 d DU . . H3A H -0.1152 0.8058 0.4410 0.059 Uiso 1 1 calc R . . H3B H -0.0619 0.8139 0.4884 0.059 Uiso 1 1 calc R . . C4 C -0.0663(4) 0.8617(5) 0.4190(4) 0.068(3) Uani 1 1 d DU B . H4A H -0.0300 0.8662 0.4322 0.082 Uiso 1 1 calc R . . H4B H -0.0791 0.8482 0.3807 0.082 Uiso 1 1 calc R . . C5 C -0.0880(4) 0.9322(5) 0.4248(6) 0.095(4) Uani 1 1 d DU . . H5A H -0.0808 0.9672 0.4015 0.114 Uiso 0.66(2) 1 calc PR B 1 H5B H -0.1244 0.9262 0.4103 0.114 Uiso 0.66(2) 1 calc PR B 1 H5C H -0.1235 0.9319 0.4007 0.114 Uiso 0.34(2) 1 calc PR B 2 H5D H -0.0860 0.9355 0.4618 0.114 Uiso 0.34(2) 1 calc PR B 2 C6 C -0.0737(10) 0.9627(11) 0.4744(8) 0.144(11) Uani 0.66(2) 1 d PDU B 1 H6A H -0.0922 1.0074 0.4717 0.215 Uiso 0.66(2) 1 calc PR B 1 H6B H -0.0382 0.9733 0.4885 0.215 Uiso 0.66(2) 1 calc PR B 1 H6C H -0.0805 0.9294 0.4985 0.215 Uiso 0.66(2) 1 calc PR B 1 C6X C -0.0669(13) 0.9939(12) 0.4142(15) 0.099(13) Uiso 0.34(2) 1 d PDU B 2 H6X1 H -0.0844 1.0363 0.4191 0.148 Uiso 0.34(2) 1 calc PR B 2 H6X2 H -0.0695 0.9925 0.3772 0.148 Uiso 0.34(2) 1 calc PR B 2 H6X3 H -0.0321 0.9965 0.4386 0.148 Uiso 0.34(2) 1 calc PR B 2 C7 C -0.0112(3) 0.7221(6) 0.4516(3) 0.060(2) Uani 1 1 d DU . . H7A H -0.0045 0.6731 0.4421 0.072 Uiso 1 1 calc R . . H7B H -0.0030 0.7562 0.4285 0.072 Uiso 1 1 calc R . . C8 C 0.0231(3) 0.7364(7) 0.5087(3) 0.075(3) Uani 1 1 d DU C . H8A H 0.0164 0.7849 0.5192 0.090 Uiso 1 1 calc R . . H8B H 0.0169 0.7009 0.5322 0.090 Uiso 1 1 calc R . . C9 C 0.0761(4) 0.7320(8) 0.5159(5) 0.095(4) Uani 1 1 d DU . . H9A H 0.0824 0.6828 0.5063 0.114 Uiso 0.68(2) 1 calc PR C 1 H9B H 0.0811 0.7653 0.4902 0.114 Uiso 0.68(2) 1 calc PR C 1 H9C H 0.0968 0.7270 0.5545 0.114 Uiso 0.32(2) 1 calc PR C 2 H9D H 0.0806 0.6879 0.4980 0.114 Uiso 0.32(2) 1 calc PR C 2 C10 C 0.1118(6) 0.7477(14) 0.5671(7) 0.130(10) Uani 0.68(2) 1 d PDU C 1 H10A H 0.1449 0.7419 0.5673 0.195 Uiso 0.68(2) 1 calc PR C 1 H10B H 0.1078 0.7149 0.5932 0.195 Uiso 0.68(2) 1 calc PR C 1 H10C H 0.1075 0.7974 0.5765 0.195 Uiso 0.68(2) 1 calc PR C 1 C10X C 0.0935(12) 0.7903(19) 0.4963(17) 0.116(15) Uani 0.32(2) 1 d PDU C 2 H10D H 0.1283 0.7826 0.5028 0.173 Uiso 0.32(2) 1 calc PR C 2 H10E H 0.0903 0.8342 0.5145 0.173 Uiso 0.32(2) 1 calc PR C 2 H10F H 0.0741 0.7950 0.4578 0.173 Uiso 0.32(2) 1 calc PR C 2 C11 C -0.0935(3) 0.7078(5) 0.3806(3) 0.053(2) Uani 1 1 d DU . . H11A H -0.0806 0.7373 0.3588 0.064 Uiso 1 1 calc R . . H11B H -0.0862 0.6569 0.3761 0.064 Uiso 1 1 calc R . . C12 C -0.1490(3) 0.7173(6) 0.3594(3) 0.066(3) Uani 1 1 d DU D . H12A H -0.1612 0.6988 0.3859 0.080 Uiso 1 1 calc R . . H12B H -0.1571 0.7691 0.3540 0.080 Uiso 1 1 calc R . . C13 C -0.1742(4) 0.6784(8) 0.3076(4) 0.104(4) Uani 1 1 d DU . . H13A H -0.1618 0.6981 0.2816 0.125 Uiso 0.55(2) 1 calc PR D 1 H13B H -0.1641 0.6273 0.3134 0.125 Uiso 0.55(2) 1 calc PR D 1 H13C H -0.2001 0.7095 0.2821 0.125 Uiso 0.45(2) 1 calc PR D 2 H13D H -0.1500 0.6667 0.2920 0.125 Uiso 0.45(2) 1 calc PR D 2 C14 C -0.2247(5) 0.6808(12) 0.2848(7) 0.081(7) Uani 0.55(2) 1 d PDU D 1 H14A H -0.2367 0.6542 0.2511 0.121 Uiso 0.55(2) 1 calc PR D 1 H14B H -0.2356 0.7309 0.2780 0.121 Uiso 0.55(2) 1 calc PR D 1 H14C H -0.2379 0.6590 0.3091 0.121 Uiso 0.55(2) 1 calc PR D 1 C14X C -0.1962(10) 0.6135(12) 0.3165(10) 0.106(10) Uani 0.45(2) 1 d PDU D 2 H14D H -0.2123 0.5879 0.2825 0.159 Uiso 0.45(2) 1 calc PR D 2 H14E H -0.2208 0.6253 0.3310 0.159 Uiso 0.45(2) 1 calc PR D 2 H14F H -0.1704 0.5830 0.3418 0.159 Uiso 0.45(2) 1 calc PR D 2 C15 C -0.0808(3) 0.6784(4) 0.4747(3) 0.053(2) Uani 1 1 d . . . H15A H -0.0637 0.6946 0.5121 0.063 Uiso 1 1 calc R . . H15B H -0.1168 0.6832 0.4649 0.063 Uiso 1 1 calc R . . C16 C -0.0691(4) 0.6002(5) 0.4718(4) 0.073(3) Uani 1 1 d . . . H16A H -0.0912 0.5808 0.4366 0.088 Uiso 1 1 calc R . . H16B H -0.0346 0.5957 0.4746 0.088 Uiso 1 1 calc R . . C17 C -0.0750(5) 0.5567(6) 0.5152(6) 0.100(5) Uani 1 1 d . . . H17A H -0.0533 0.5777 0.5500 0.120 Uiso 1 1 calc R . . H17B H -0.1095 0.5620 0.5119 0.120 Uiso 1 1 calc R . . C18 C -0.0640(5) 0.4804(7) 0.5162(5) 0.109(5) Uani 1 1 d . . . H18A H -0.0693 0.4575 0.5459 0.164 Uiso 1 1 calc R . . H18B H -0.0295 0.4739 0.5210 0.164 Uiso 1 1 calc R . . H18C H -0.0858 0.4583 0.4825 0.164 Uiso 1 1 calc R . . O13 O -0.0113(3) 0.4018(4) 0.6398(3) 0.074(2) Uani 1 1 d . . . O11 O 0.1471(2) 0.2515(5) 0.8011(3) 0.087(2) Uani 1 1 d . . . N2 N -0.1276(2) -0.0268(3) 0.6712(2) 0.0380(14) Uani 1 1 d D . . C19 C -0.1305(3) 0.0263(4) 0.7123(3) 0.0463(19) Uani 1 1 d D . . H19A H -0.1111 0.0069 0.7484 0.056 Uiso 1 1 calc R . . H19B H -0.1147 0.0719 0.7088 0.056 Uiso 1 1 calc R . . C20 C -0.1822(3) 0.0428(5) 0.7081(4) 0.063(2) Uani 1 1 d D . . H20A H -0.1997 -0.0027 0.7076 0.076 Uiso 1 1 calc R . . H20B H -0.2006 0.0683 0.6741 0.076 Uiso 1 1 calc R . . C21 C -0.1810(4) 0.0891(5) 0.7548(4) 0.070(3) Uani 1 1 d D . . H21A H -0.1650 0.0620 0.7885 0.084 Uiso 1 1 calc R . . H21B H -0.1610 0.1328 0.7571 0.084 Uiso 1 1 calc R . . C22 C -0.2321(5) 0.1106(7) 0.7483(5) 0.105(4) Uani 1 1 d D . . H22A H -0.2302 0.1404 0.7787 0.157 Uiso 1 1 calc R . . H22B H -0.2516 0.0674 0.7468 0.157 Uiso 1 1 calc R . . H22C H -0.2478 0.1380 0.7151 0.157 Uiso 1 1 calc R . . C23 C -0.1576(3) -0.0015(4) 0.6146(3) 0.0398(16) Uani 1 1 d DU . . H23A H -0.1550 -0.0383 0.5896 0.048 Uiso 1 1 calc R . . H23B H -0.1927 0.0013 0.6095 0.048 Uiso 1 1 calc R . . C24 C -0.1428(3) 0.0703(4) 0.5994(3) 0.054(2) Uani 1 1 d DU E . H24A H -0.1078 0.0687 0.6040 0.065 Uiso 1 1 calc R . . H24B H -0.1465 0.1084 0.6228 0.065 Uiso 1 1 calc R . . C25 C -0.1755(4) 0.0868(6) 0.5417(4) 0.096(4) Uani 1 1 d DU . . H25A H -0.2104 0.0822 0.5372 0.115 Uiso 0.569(19) 1 calc PR E 1 H25B H -0.1701 0.1376 0.5346 0.115 Uiso 0.569(19) 1 calc PR E 1 H25C H -0.1807 0.0418 0.5208 0.115 Uiso 0.431(19) 1 calc PR E 2 H25D H -0.2081 0.1028 0.5400 0.115 Uiso 0.431(19) 1 calc PR E 2 C26 C -0.1685(10) 0.0433(11) 0.5022(7) 0.125(10) Uani 0.569(19) 1 d PDU E 1 H26A H -0.1916 0.0583 0.4666 0.187 Uiso 0.569(19) 1 calc PR E 1 H26B H -0.1745 -0.0072 0.5079 0.187 Uiso 0.569(19) 1 calc PR E 1 H26C H -0.1345 0.0488 0.5048 0.187 Uiso 0.569(19) 1 calc PR E 1 C26X C -0.1563(12) 0.1416(15) 0.5162(10) 0.112(12) Uani 0.431(19) 1 d PDU E 2 H26D H -0.1798 0.1488 0.4793 0.168 Uiso 0.431(19) 1 calc PR E 2 H26E H -0.1245 0.1257 0.5165 0.168 Uiso 0.431(19) 1 calc PR E 2 H26F H -0.1518 0.1869 0.5359 0.168 Uiso 0.431(19) 1 calc PR E 2 C27 C -0.0733(3) -0.0335(4) 0.6812(3) 0.0399(17) Uani 1 1 d . . . H27A H -0.0599 0.0155 0.6820 0.048 Uiso 1 1 calc R . . H27B H -0.0558 -0.0548 0.7171 0.048 Uiso 1 1 calc R . . C28 C -0.0612(3) -0.0775(5) 0.6416(3) 0.049(2) Uani 1 1 d . . . H28A H -0.0733 -0.0524 0.6067 0.059 Uiso 1 1 calc R . . H28B H -0.0782 -0.1245 0.6364 0.059 Uiso 1 1 calc R . . C29 C -0.0058(3) -0.0895(5) 0.6611(4) 0.056(2) Uani 1 1 d . . . H29A H 0.0112 -0.0424 0.6698 0.067 Uiso 1 1 calc R . . H29B H 0.0055 -0.1183 0.6943 0.067 Uiso 1 1 calc R . . C30 C 0.0089(4) -0.1277(7) 0.6203(4) 0.090(4) Uani 1 1 d . . . H30A H 0.0448 -0.1347 0.6352 0.135 Uiso 1 1 calc R . . H30B H -0.0010 -0.0985 0.5878 0.135 Uiso 1 1 calc R . . H30C H -0.0076 -0.1745 0.6117 0.135 Uiso 1 1 calc R . . C31 C -0.1487(3) -0.0995(4) 0.6766(3) 0.0434(18) Uani 1 1 d . . . H31A H -0.1844 -0.0931 0.6678 0.052 Uiso 1 1 calc R . . H31B H -0.1457 -0.1318 0.6492 0.052 Uiso 1 1 calc R . . C32 C -0.1264(3) -0.1374(4) 0.7298(3) 0.047(2) Uani 1 1 d . . . H32A H -0.0909 -0.1465 0.7388 0.057 Uiso 1 1 calc R . . H32B H -0.1291 -0.1063 0.7580 0.057 Uiso 1 1 calc R . . C33 C -0.1523(4) -0.2075(5) 0.7281(4) 0.069(3) Uani 1 1 d . . . H33A H -0.1880 -0.1978 0.7175 0.083 Uiso 1 1 calc R . . H33B H -0.1488 -0.2383 0.7002 0.083 Uiso 1 1 calc R . . C34 C -0.1336(4) -0.2481(5) 0.7798(4) 0.075(3) Uani 1 1 d . . . H34A H -0.1528 -0.2923 0.7757 0.112 Uiso 1 1 calc R . . H34B H -0.1370 -0.2182 0.8078 0.112 Uiso 1 1 calc R . . H34C H -0.0987 -0.2602 0.7898 0.112 Uiso 1 1 calc R . . O14 O -0.07169(19) 0.3227(4) 0.6773(2) 0.0652(18) Uani 1 1 d . . . O18 O -0.0107(3) 0.0995(4) 0.6415(3) 0.089(3) Uani 1 1 d . . . N3 N 0.1478(2) 0.4964(3) 0.3367(3) 0.0447(16) Uani 1 1 d D . . C35 C 0.1277(3) 0.4261(4) 0.3488(4) 0.053(2) Uani 1 1 d DU . . H35A H 0.1355 0.3870 0.3288 0.063 Uiso 1 1 calc R . . H35B H 0.1452 0.4155 0.3873 0.063 Uiso 1 1 calc R . . C36 C 0.0727(3) 0.4251(5) 0.3350(4) 0.065(3) Uani 1 1 d DU F . H36A H 0.0545 0.4373 0.2969 0.078 Uiso 1 1 calc R . . H36B H 0.0644 0.4615 0.3567 0.078 Uiso 1 1 calc R . . C37 C 0.0570(3) 0.3511(6) 0.3461(5) 0.088(4) Uani 1 1 d DU . . H37A H 0.0673 0.3156 0.3255 0.105 Uiso 0.59(2) 1 calc PR F 1 H37B H 0.0756 0.3403 0.3844 0.105 Uiso 0.59(2) 1 calc PR F 1 H37C H 0.0791 0.3370 0.3828 0.105 Uiso 0.41(2) 1 calc PR F 2 H37D H 0.0231 0.3550 0.3451 0.105 Uiso 0.41(2) 1 calc PR F 2 C38 C 0.0062(6) 0.3403(14) 0.3341(12) 0.150(13) Uani 0.59(2) 1 d PDU F 1 H38A H 0.0010 0.2910 0.3432 0.224 Uiso 0.59(2) 1 calc PR F 1 H38B H -0.0129 0.3485 0.2959 0.224 Uiso 0.59(2) 1 calc PR F 1 H38C H -0.0047 0.3740 0.3548 0.224 Uiso 0.59(2) 1 calc PR F 1 C38X C 0.0573(9) 0.2954(11) 0.3110(9) 0.071(8) Uiso 0.41(2) 1 d PDU F 2 H38D H 0.0473 0.2502 0.3223 0.107 Uiso 0.41(2) 1 calc PR F 2 H38E H 0.0907 0.2903 0.3117 0.107 Uiso 0.41(2) 1 calc PR F 2 H38F H 0.0341 0.3071 0.2746 0.107 Uiso 0.41(2) 1 calc PR F 2 C39 C 0.1417(3) 0.5560(5) 0.3715(3) 0.060(2) Uani 1 1 d DU . . H39A H 0.1513 0.6018 0.3598 0.072 Uiso 1 1 calc R . . H39B H 0.1061 0.5596 0.3646 0.072 Uiso 1 1 calc R . . C40 C 0.1703(4) 0.5493(6) 0.4311(4) 0.078(3) Uani 1 1 d DU G . H40A H 0.2057 0.5413 0.4389 0.094 Uiso 1 1 calc R . . H40B H 0.1580 0.5075 0.4447 0.094 Uiso 1 1 calc R . . C41 C 0.1644(6) 0.6182(8) 0.4594(5) 0.117(5) Uani 1 1 d DU . . H41A H 0.1287 0.6286 0.4475 0.140 Uiso 0.68(2) 1 calc PR G 1 H41B H 0.1775 0.6088 0.4983 0.140 Uiso 0.68(2) 1 calc PR G 1 H41C H 0.1727 0.6594 0.4416 0.140 Uiso 0.32(2) 1 calc PR G 2 H41D H 0.1290 0.6228 0.4528 0.140 Uiso 0.32(2) 1 calc PR G 2 C42 C 0.1878(9) 0.6794(9) 0.4507(8) 0.131(9) Uani 0.68(2) 1 d PDU G 1 H42A H 0.1812 0.7205 0.4694 0.197 Uiso 0.68(2) 1 calc PR G 1 H42B H 0.1751 0.6897 0.4124 0.197 Uiso 0.68(2) 1 calc PR G 1 H42C H 0.2235 0.6710 0.4643 0.197 Uiso 0.68(2) 1 calc PR G 1 C42X C 0.1920(15) 0.626(2) 0.5152(9) 0.14(2) Uani 0.32(2) 1 d PDU G 2 H42D H 0.1840 0.6717 0.5273 0.207 Uiso 0.32(2) 1 calc PR G 2 H42E H 0.2274 0.6241 0.5228 0.207 Uiso 0.32(2) 1 calc PR G 2 H42F H 0.1837 0.5863 0.5341 0.207 Uiso 0.32(2) 1 calc PR G 2 C43 C 0.2017(3) 0.4834(4) 0.3482(3) 0.0438(18) Uani 1 1 d . . . H43A H 0.2182 0.4661 0.3854 0.053 Uiso 1 1 calc R . . H43B H 0.2038 0.4445 0.3245 0.053 Uiso 1 1 calc R . . C44 C 0.2298(3) 0.5476(5) 0.3412(4) 0.059(2) Uani 1 1 d . . . H44A H 0.2269 0.5878 0.3636 0.070 Uiso 1 1 calc R . . H44B H 0.2153 0.5634 0.3034 0.070 Uiso 1 1 calc R . . C45 C 0.2839(4) 0.5296(6) 0.3568(5) 0.082(3) Uani 1 1 d . . . H45A H 0.2985 0.5160 0.3950 0.098 Uiso 1 1 calc R . . H45B H 0.2863 0.4874 0.3359 0.098 Uiso 1 1 calc R . . C46 C 0.3135(4) 0.5899(8) 0.3480(6) 0.112(5) Uani 1 1 d . . . H46A H 0.3479 0.5745 0.3586 0.168 Uiso 1 1 calc R . . H46B H 0.3122 0.6315 0.3695 0.168 Uiso 1 1 calc R . . H46C H 0.2996 0.6032 0.3101 0.168 Uiso 1 1 calc R . . C47 C 0.1194(3) 0.5192(4) 0.2790(3) 0.052(2) Uani 1 1 d . . . H47A H 0.0846 0.5282 0.2735 0.063 Uiso 1 1 calc R . . H47B H 0.1334 0.5652 0.2731 0.063 Uiso 1 1 calc R . . C48 C 0.1199(4) 0.4664(5) 0.2377(3) 0.061(2) Uani 1 1 d . . . H48A H 0.1100 0.4183 0.2454 0.073 Uiso 1 1 calc R . . H48B H 0.1537 0.4627 0.2384 0.073 Uiso 1 1 calc R . . C49 C 0.0844(5) 0.4914(6) 0.1832(4) 0.089(4) Uani 1 1 d . . . H49A H 0.0922 0.5416 0.1774 0.107 Uiso 1 1 calc R . . H49B H 0.0502 0.4901 0.1815 0.107 Uiso 1 1 calc R . . C50 C 0.0881(6) 0.4433(7) 0.1393(4) 0.119(5) Uani 1 1 d . . . H50A H 0.0647 0.4602 0.1044 0.179 Uiso 1 1 calc R . . H50B H 0.0801 0.3937 0.1449 0.179 Uiso 1 1 calc R . . H50C H 0.1218 0.4454 0.1406 0.179 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0226(4) 0.0255(4) 0.0221(4) -0.0071(3) 0.0091(3) 0.0003(3) Mo1 0.0226(4) 0.0255(4) 0.0221(4) -0.0071(3) 0.0091(3) 0.0003(3) Mo2 0.0174(2) 0.0335(3) 0.0258(3) -0.0069(2) 0.0084(2) -0.0010(2) Mo3 0.0263(3) 0.0332(3) 0.0208(3) -0.0001(2) 0.0115(2) 0.0020(2) Ti2 0.0244(4) 0.0557(6) 0.0391(5) 0.0009(4) 0.0134(4) 0.0079(4) Mo4 0.0244(4) 0.0557(6) 0.0391(5) 0.0009(4) 0.0134(4) 0.0079(4) Mo5 0.0492(4) 0.0312(3) 0.0406(4) 0.0122(3) 0.0269(3) 0.0063(3) Mo6 0.0941(6) 0.0330(4) 0.0629(5) -0.0204(3) 0.0597(5) -0.0217(4) O1 0.041(3) 0.037(3) 0.024(2) -0.0011(19) 0.016(2) 0.001(2) O2 0.025(2) 0.035(2) 0.021(2) -0.0080(18) 0.0108(18) -0.0021(18) O3 0.021(2) 0.031(2) 0.018(2) -0.0047(17) 0.0059(16) 0.0021(17) O4 0.023(2) 0.045(3) 0.031(2) -0.009(2) 0.0116(19) -0.003(2) O5 0.024(2) 0.028(2) 0.027(2) -0.0063(18) 0.0092(18) -0.0032(18) O6 0.028(2) 0.027(2) 0.024(2) -0.0027(18) 0.0098(18) 0.0029(18) O7 0.036(3) 0.026(2) 0.044(3) -0.011(2) 0.012(2) 0.002(2) O8 0.020(2) 0.032(2) 0.029(2) -0.0037(19) 0.0084(18) 0.0019(18) O9 0.032(2) 0.029(2) 0.029(2) -0.0090(19) 0.0171(19) 0.0035(19) O10 0.021(3) 0.029(3) 0.023(3) -0.002(2) 0.011(2) 0.000(2) O12 0.044(3) 0.033(3) 0.065(3) -0.002(2) 0.036(3) -0.004(2) O15 0.062(5) 0.021(4) 0.094(6) 0.000 0.055(5) 0.000 O16 0.058(3) 0.064(4) 0.035(3) -0.005(3) 0.026(3) -0.012(3) O17 0.070(4) 0.089(5) 0.064(4) -0.047(4) 0.040(3) -0.042(4) O19 0.114(8) 0.023(4) 0.113(8) 0.000 0.093(7) 0.000 O20 0.069(4) 0.034(3) 0.072(4) 0.000(3) 0.049(3) 0.009(3) O21 0.044(4) 0.022(3) 0.033(3) 0.000 0.022(3) 0.000 C1 0.044(10) 0.064(12) 0.074(12) -0.027(10) 0.019(9) 0.004(8) C2 0.042(10) 0.069(13) 0.113(18) -0.025(12) 0.012(11) 0.003(9) N1 0.049(4) 0.063(4) 0.049(4) 0.000(3) 0.038(3) 0.005(3) C3 0.045(4) 0.061(5) 0.055(5) -0.007(4) 0.033(4) 0.001(4) C4 0.060(6) 0.065(5) 0.093(7) 0.002(5) 0.045(5) -0.009(5) C5 0.087(8) 0.062(6) 0.149(11) 0.000(7) 0.060(8) -0.010(6) C6 0.20(3) 0.067(13) 0.141(16) -0.005(12) 0.050(18) 0.038(15) C7 0.050(4) 0.092(7) 0.054(5) 0.004(5) 0.039(4) 0.009(5) C8 0.061(5) 0.119(9) 0.055(5) -0.002(6) 0.035(4) 0.014(6) C9 0.059(5) 0.125(10) 0.098(8) -0.006(8) 0.029(5) 0.009(7) C10 0.072(9) 0.22(3) 0.088(12) -0.019(15) 0.016(8) 0.008(14) C10X 0.07(2) 0.16(3) 0.11(3) 0.00(3) 0.03(2) -0.02(2) C11 0.053(4) 0.069(6) 0.052(5) -0.004(4) 0.036(4) -0.001(4) C12 0.052(5) 0.096(7) 0.062(5) -0.018(5) 0.035(4) -0.017(5) C13 0.082(7) 0.150(12) 0.070(7) -0.033(7) 0.019(6) -0.018(8) C14 0.072(8) 0.103(17) 0.066(12) -0.034(11) 0.024(8) 0.000(11) C14X 0.080(18) 0.15(2) 0.10(2) -0.079(16) 0.053(15) -0.046(17) C15 0.073(6) 0.057(5) 0.051(5) -0.006(4) 0.048(5) 0.007(4) C16 0.099(8) 0.066(6) 0.085(7) 0.014(5) 0.069(7) 0.016(6) C17 0.158(12) 0.063(7) 0.133(11) 0.029(7) 0.115(10) 0.034(7) C18 0.128(11) 0.120(11) 0.106(10) 0.047(9) 0.075(9) 0.047(9) O13 0.091(5) 0.067(4) 0.084(5) 0.044(4) 0.055(4) 0.024(4) O11 0.035(3) 0.152(7) 0.074(5) 0.005(5) 0.023(3) 0.020(4) N2 0.051(4) 0.032(3) 0.027(3) -0.007(2) 0.011(3) -0.010(3) C19 0.064(5) 0.042(4) 0.035(4) -0.014(3) 0.022(4) -0.014(4) C20 0.075(6) 0.064(6) 0.058(6) -0.023(5) 0.035(5) -0.011(5) C21 0.089(7) 0.068(6) 0.076(7) -0.027(5) 0.058(6) -0.025(5) C22 0.126(11) 0.112(10) 0.110(10) -0.034(8) 0.085(9) -0.005(9) C23 0.046(4) 0.040(4) 0.030(4) -0.009(3) 0.011(3) -0.006(3) C24 0.060(5) 0.047(5) 0.044(4) 0.003(4) 0.009(4) -0.015(4) C25 0.098(8) 0.091(8) 0.063(6) 0.030(5) -0.007(6) -0.028(7) C26 0.21(3) 0.103(16) 0.040(8) 0.018(9) 0.026(12) -0.061(16) C26X 0.16(3) 0.09(2) 0.077(16) 0.031(14) 0.033(18) -0.025(18) C27 0.038(4) 0.043(4) 0.030(4) -0.006(3) 0.005(3) -0.006(3) C28 0.044(4) 0.053(5) 0.040(4) -0.014(4) 0.005(4) -0.003(4) C29 0.044(5) 0.056(5) 0.056(5) -0.014(4) 0.008(4) -0.002(4) C30 0.048(6) 0.129(11) 0.083(8) -0.029(7) 0.016(5) 0.013(6) C31 0.059(5) 0.029(4) 0.038(4) -0.013(3) 0.015(4) -0.019(3) C32 0.071(5) 0.039(4) 0.028(4) -0.005(3) 0.016(4) -0.015(4) C33 0.098(8) 0.046(5) 0.062(6) -0.002(4) 0.031(6) -0.024(5) C34 0.114(9) 0.044(5) 0.065(6) 0.006(5) 0.034(6) -0.011(5) O14 0.035(3) 0.106(5) 0.056(4) 0.042(4) 0.020(3) 0.019(3) O18 0.129(6) 0.076(5) 0.109(6) -0.057(4) 0.096(5) -0.050(5) N3 0.045(4) 0.038(4) 0.054(4) 0.015(3) 0.022(3) 0.017(3) C35 0.048(4) 0.051(5) 0.060(5) 0.023(4) 0.022(4) 0.015(4) C36 0.048(5) 0.076(6) 0.073(6) 0.032(5) 0.027(5) 0.016(4) C37 0.048(5) 0.096(8) 0.112(9) 0.038(7) 0.023(6) 0.003(5) C38 0.050(9) 0.16(2) 0.22(3) 0.10(2) 0.030(15) -0.001(12) C39 0.066(6) 0.050(5) 0.075(5) 0.002(4) 0.039(5) 0.021(4) C40 0.094(8) 0.080(7) 0.072(6) 0.001(5) 0.044(6) 0.022(6) C41 0.139(12) 0.136(10) 0.088(8) -0.033(8) 0.059(8) 0.038(10) C42 0.19(2) 0.079(10) 0.084(14) -0.015(11) 0.015(14) 0.044(11) C42X 0.13(3) 0.17(4) 0.104(16) -0.05(2) 0.04(2) 0.06(3) C43 0.046(4) 0.041(4) 0.047(4) 0.010(3) 0.022(4) 0.017(4) C44 0.056(5) 0.053(5) 0.066(6) 0.016(4) 0.022(5) 0.006(4) C45 0.065(7) 0.073(7) 0.123(10) -0.005(7) 0.053(7) -0.007(5) C46 0.073(8) 0.122(11) 0.136(12) 0.027(10) 0.038(8) -0.023(8) C47 0.055(5) 0.037(4) 0.061(5) 0.021(4) 0.019(4) 0.014(4) C48 0.067(6) 0.054(5) 0.053(5) 0.016(4) 0.015(4) 0.016(5) C49 0.125(10) 0.057(6) 0.060(6) 0.013(5) 0.009(6) -0.005(6) C50 0.189(15) 0.091(9) 0.053(7) 0.005(6) 0.022(8) -0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O5 1.954(4) . ? Ti1 O6 1.929(4) . ? Ti1 O7 1.744(4) . ? Ti1 O8 1.917(4) . ? Ti1 O9 1.961(4) . ? Ti1 O10 2.2586(7) . ? Mo2 O2 2.022(4) 7_556 ? Mo2 O3 1.878(4) . ? Mo2 O4 1.696(4) . ? Mo2 O5 1.888(4) . ? Mo2 O8 1.914(4) 7_556 ? Mo2 O10 2.3309(5) . ? Mo3 O1 1.693(4) . ? Mo3 O2 1.876(4) . ? Mo3 O3 2.032(4) . ? Mo3 O6 1.918(4) 7_556 ? Mo3 O9 1.901(4) . ? Mo3 O10 2.3396(5) . ? Ti2 O12 1.945(5) . ? Ti2 O17 1.908(6) 2_556 ? Ti2 O20 1.922(6) . ? Ti2 O21 2.2330(8) . ? Ti2 O11 1.761(6) . ? Ti2 O14 1.936(6) 2_556 ? Mo5 O12 1.884(5) . ? Mo5 O15 1.953(4) . ? Mo5 O16 1.950(6) . ? Mo5 O21 2.328(4) . ? Mo5 O13 1.690(6) . ? Mo5 O14 1.897(5) . ? Mo6 O16 1.919(6) . ? Mo6 O17 1.885(6) . ? Mo6 O19 1.952(4) . ? Mo6 O20 1.882(6) . ? Mo6 O21 2.332(4) . ? Mo6 O18 1.691(6) . ? O2 Mo2 2.022(4) 7_556 ? O6 Mo3 1.918(4) 7_556 ? O7 C1 1.490(17) . ? O8 Mo2 1.914(4) 7_556 ? O10 Ti1 2.2586(7) 7_556 ? O10 Mo1 2.2586(7) 7_556 ? O10 Mo2 2.3309(5) 7_556 ? O10 Mo3 2.3396(5) 7_556 ? O15 Mo5 1.953(4) 2_556 ? O17 Ti2 1.908(6) 2_556 ? O17 Mo4 1.908(6) 2_556 ? O19 Mo6 1.952(4) 2_556 ? O21 Ti2 2.2330(8) 2_556 ? O21 Mo4 2.2330(8) 2_556 ? O21 Mo5 2.328(4) 2_556 ? O21 Mo6 2.332(4) 2_556 ? C1 H1A 0.980 . ? C1 H1B 0.980 . ? C1 H1C 0.980 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C2 O11 1.447(19) . ? N1 C3 1.518(9) . ? N1 C7 1.520(8) . ? N1 C11 1.520(9) . ? N1 C15 1.525(10) . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C3 C4 1.506(10) . ? C4 H4A 0.990 . ? C4 H4B 0.990 . ? C4 C5 1.495(11) . ? C5 H5A 0.990 . ? C5 H5B 0.990 . ? C5 H5C 0.990 . ? C5 H5D 0.990 . ? C5 C6 1.372(15) . ? C5 C6X 1.391(17) . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C6X H6X1 0.980 . ? C6X H6X2 0.980 . ? C6X H6X3 0.980 . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C7 C8 1.505(10) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C8 C9 1.496(11) . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 H9C 0.990 . ? C9 H9D 0.990 . ? C9 C10 1.406(14) . ? C9 C10X 1.393(17) . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C10X H10D 0.980 . ? C10X H10E 0.980 . ? C10X H10F 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 C12 1.512(10) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.496(11) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 H13C 0.990 . ? C13 H13D 0.990 . ? C13 C14 1.365(14) . ? C13 C14X 1.434(16) . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C14X H14D 0.980 . ? C14X H14E 0.980 . ? C14X H14F 0.980 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.504(12) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.501(13) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.456(15) . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? N2 C19 1.522(8) . ? N2 C23 1.518(8) . ? N2 C27 1.518(9) . ? N2 C31 1.521(9) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.512(10) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.528(10) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.499(13) . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 C24 1.512(9) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C24 C25 1.515(11) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C25 H25C 0.990 . ? C25 H25D 0.990 . ? C25 C26 1.428(17) . ? C25 C26X 1.468(17) . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? C26X H26D 0.980 . ? C26X H26E 0.980 . ? C26X H26F 0.980 . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C27 C28 1.508(10) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C28 C29 1.519(11) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C29 C30 1.519(13) . ? C30 H30A 0.980 . ? C30 H30B 0.980 . ? C30 H30C 0.980 . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C31 C32 1.509(10) . ? C32 H32A 0.990 . ? C32 H32B 0.990 . ? C32 C33 1.503(11) . ? C33 H33A 0.990 . ? C33 H33B 0.990 . ? C33 C34 1.500(12) . ? C34 H34A 0.980 . ? C34 H34B 0.980 . ? C34 H34C 0.980 . ? O14 Ti2 1.936(6) 2_556 ? O14 Mo4 1.936(6) 2_556 ? N3 C35 1.524(9) . ? N3 C39 1.516(9) . ? N3 C43 1.512(9) . ? N3 C47 1.521(10) . ? C35 H35A 0.990 . ? C35 H35B 0.990 . ? C35 C36 1.512(10) . ? C36 H36A 0.990 . ? C36 H36B 0.990 . ? C36 C37 1.519(12) . ? C37 H37A 0.990 . ? C37 H37B 0.990 . ? C37 H37C 0.990 . ? C37 H37D 0.990 . ? C37 C38 1.414(15) . ? C37 C38X 1.413(17) . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? C38X H38D 0.980 . ? C38X H38E 0.980 . ? C38X H38F 0.980 . ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? C39 C40 1.511(11) . ? C40 H40A 0.990 . ? C40 H40B 0.990 . ? C40 C41 1.540(13) . ? C41 H41A 0.990 . ? C41 H41B 0.990 . ? C41 H41C 0.990 . ? C41 H41D 0.990 . ? C41 C42 1.401(17) . ? C41 C42X 1.421(19) . ? C42 H42A 0.980 . ? C42 H42B 0.980 . ? C42 H42C 0.980 . ? C42X H42D 0.980 . ? C42X H42E 0.980 . ? C42X H42F 0.980 . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C43 C44 1.510(11) . ? C44 H44A 0.990 . ? C44 H44B 0.990 . ? C44 C45 1.514(13) . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C45 C46 1.498(14) . ? C46 H46A 0.980 . ? C46 H46B 0.980 . ? C46 H46C 0.980 . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C47 C48 1.500(12) . ? C48 H48A 0.990 . ? C48 H48B 0.990 . ? C48 C49 1.512(12) . ? C49 H49A 0.990 . ? C49 H49B 0.990 . ? C49 C50 1.532(16) . ? C50 H50A 0.980 . ? C50 H50B 0.980 . ? C50 H50C 0.980 . ? 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 O5 Ti1 O6 86.90(17) . . ? O5 Ti1 O7 103.0(2) . . ? O5 Ti1 O8 155.46(18) . . ? O5 Ti1 O9 86.92(18) . . ? O5 Ti1 O10 77.19(12) . . ? O6 Ti1 O7 104.8(2) . . ? O6 Ti1 O8 88.16(18) . . ? O6 Ti1 O9 156.11(17) . . ? O6 Ti1 O10 78.05(12) . . ? O7 Ti1 O8 101.5(2) . . ? O7 Ti1 O9 99.1(2) . . ? O7 Ti1 O10 177.17(17) . . ? O8 Ti1 O9 87.95(18) . . ? O8 Ti1 O10 78.27(13) . . ? O9 Ti1 O10 78.08(12) . . ? O2 Mo2 O3 154.77(17) 7_556 . ? O2 Mo2 O4 100.64(19) 7_556 . ? O2 Mo2 O5 84.65(17) 7_556 . ? O2 Mo2 O8 83.94(17) 7_556 7_556 ? O2 Mo2 O10 75.88(11) 7_556 . ? O3 Mo2 O4 104.57(19) . . ? O3 Mo2 O5 90.32(18) . . ? O3 Mo2 O8 89.52(18) . 7_556 ? O3 Mo2 O10 78.90(12) . . ? O4 Mo2 O5 103.7(2) . . ? O4 Mo2 O8 102.8(2) . 7_556 ? O4 Mo2 O10 176.48(15) . . ? O5 Mo2 O8 152.65(17) . 7_556 ? O5 Mo2 O10 76.63(12) . . ? O8 Mo2 O10 76.51(12) 7_556 . ? O1 Mo3 O2 105.1(2) . . ? O1 Mo3 O3 100.76(19) . . ? O1 Mo3 O6 102.5(2) . 7_556 ? O1 Mo3 O9 103.7(2) . . ? O1 Mo3 O10 176.42(16) . . ? O2 Mo3 O3 154.18(17) . . ? O2 Mo3 O6 89.75(18) . 7_556 ? O2 Mo3 O9 89.82(18) . . ? O2 Mo3 O10 78.36(12) . . ? O3 Mo3 O6 84.02(17) . 7_556 ? O3 Mo3 O9 84.68(17) . . ? O3 Mo3 O10 75.82(11) . . ? O6 Mo3 O9 152.97(18) 7_556 . ? O6 Mo3 O10 76.25(13) 7_556 . ? O9 Mo3 O10 77.19(13) . . ? O12 Ti2 O17 156.3(2) . 2_556 ? O12 Ti2 O20 87.7(2) . . ? O12 Ti2 O21 78.20(18) . . ? O12 Ti2 O11 102.1(3) . . ? O12 Ti2 O14 86.3(3) . 2_556 ? O17 Ti2 O20 88.3(3) 2_556 . ? O17 Ti2 O21 78.1(2) 2_556 . ? O17 Ti2 O11 101.5(3) 2_556 . ? O17 Ti2 O14 87.9(3) 2_556 2_556 ? O20 Ti2 O21 78.8(2) . . ? O20 Ti2 O11 103.7(3) . . ? O20 Ti2 O14 155.9(2) . 2_556 ? O21 Ti2 O11 177.5(3) . . ? O21 Ti2 O14 77.11(19) . 2_556 ? O11 Ti2 O14 100.4(3) . 2_556 ? O12 Mo5 O15 87.41(16) . . ? O12 Mo5 O16 87.2(2) . . ? O12 Mo5 O21 76.97(15) . . ? O12 Mo5 O13 105.2(3) . . ? O12 Mo5 O14 152.5(2) . . ? O15 Mo5 O16 154.1(2) . . ? O15 Mo5 O21 77.54(19) . . ? O15 Mo5 O13 104.8(3) . . ? O15 Mo5 O14 86.6(2) . . ? O16 Mo5 O21 76.57(18) . . ? O16 Mo5 O13 101.0(3) . . ? O16 Mo5 O14 86.6(3) . . ? O21 Mo5 O13 176.8(3) . . ? O21 Mo5 O14 75.50(17) . . ? O13 Mo5 O14 102.3(3) . . ? O16 Mo6 O17 88.3(3) . . ? O16 Mo6 O19 154.1(2) . . ? O16 Mo6 O20 86.4(2) . . ? O16 Mo6 O21 77.04(19) . . ? O16 Mo6 O18 103.0(3) . . ? O17 Mo6 O19 85.7(2) . . ? O17 Mo6 O20 153.1(2) . . ? O17 Mo6 O21 76.08(17) . . ? O17 Mo6 O18 103.0(3) . . ? O19 Mo6 O20 87.53(18) . . ? O19 Mo6 O21 77.0(2) . . ? O19 Mo6 O18 102.9(3) . . ? O20 Mo6 O21 77.04(15) . . ? O20 Mo6 O18 103.9(3) . . ? O21 Mo6 O18 179.0(3) . . ? Mo2 O2 Mo3 115.8(2) 7_556 . ? Mo2 O3 Mo3 115.25(19) . . ? Ti1 O5 Mo2 115.7(2) . . ? Ti1 O6 Mo3 115.5(2) . 7_556 ? Ti1 O7 C1 132.1(8) . . ? Ti1 O8 Mo2 115.4(2) . 7_556 ? Ti1 O9 Mo3 114.6(2) . . ? Ti1 O10 Mo1 180.0 . 7_556 ? Ti1 O10 Mo2 90.30(2) . . ? Ti1 O10 Mo2 90.29(2) 7_556 7_556 ? Ti1 O10 Mo2 89.71(2) . 7_556 ? Ti1 O10 Mo2 89.70(2) 7_556 . ? Ti1 O10 Mo3 89.93(2) . . ? Ti1 O10 Mo3 89.93(2) 7_556 7_556 ? Ti1 O10 Mo3 90.07(2) . 7_556 ? Ti1 O10 Mo3 90.07(2) 7_556 . ? Mo1 O10 Mo2 90.29(2) 7_556 7_556 ? Mo1 O10 Mo2 89.70(2) 7_556 . ? Mo1 O10 Mo3 89.93(2) 7_556 7_556 ? Mo1 O10 Mo3 90.07(2) 7_556 . ? Mo2 O10 Mo2 180.0 . 7_556 ? Mo2 O10 Mo3 90.018(19) . . ? Mo2 O10 Mo3 90.016(19) 7_556 7_556 ? Mo2 O10 Mo3 89.982(19) . 7_556 ? Mo2 O10 Mo3 89.984(19) 7_556 . ? Mo3 O10 Mo3 180.0 . 7_556 ? Ti2 O12 Mo5 114.8(2) . . ? Mo5 O15 Mo5 114.9(3) . 2_556 ? Mo5 O16 Mo6 116.5(2) . . ? Ti2 O17 Mo6 116.1(3) 2_556 . ? Mo4 O17 Mo6 116.1(3) 2_556 . ? Mo6 O19 Mo6 115.7(4) . 2_556 ? Ti2 O20 Mo6 114.9(2) . . ? Ti2 O21 Mo4 178.4(3) . 2_556 ? Ti2 O21 Mo5 90.01(11) . . ? Ti2 O21 Mo5 91.10(11) 2_556 . ? Ti2 O21 Mo5 90.01(11) 2_556 2_556 ? Ti2 O21 Mo5 91.10(11) . 2_556 ? Ti2 O21 Mo6 89.23(11) . . ? Ti2 O21 Mo6 89.65(11) 2_556 . ? Ti2 O21 Mo6 89.23(11) 2_556 2_556 ? Ti2 O21 Mo6 89.65(11) . 2_556 ? Mo4 O21 Mo5 91.10(11) 2_556 . ? Mo4 O21 Mo5 90.01(11) 2_556 2_556 ? Mo4 O21 Mo6 89.65(11) 2_556 . ? Mo4 O21 Mo6 89.23(11) 2_556 2_556 ? Mo5 O21 Mo5 90.0(2) . 2_556 ? Mo5 O21 Mo6 89.85(2) . . ? Mo5 O21 Mo6 179.65(10) 2_556 . ? Mo5 O21 Mo6 179.65(10) . 2_556 ? Mo5 O21 Mo6 89.85(2) 2_556 2_556 ? Mo6 O21 Mo6 90.3(2) . 2_556 ? O7 C1 H1A 109.5 . . ? O7 C1 H1B 109.5 . . ? O7 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2A C2 O11 109.5 . . ? H2B C2 H2C 109.5 . . ? H2B C2 O11 109.5 . . ? H2C C2 O11 109.5 . . ? C3 N1 C7 110.8(6) . . ? C3 N1 C11 111.4(6) . . ? C3 N1 C15 106.3(5) . . ? C7 N1 C11 107.2(5) . . ? C7 N1 C15 110.8(6) . . ? C11 N1 C15 110.4(6) . . ? N1 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? N1 C3 C4 114.4(6) . . ? H3A C3 H3B 107.6 . . ? H3A C3 C4 108.6 . . ? H3B C3 C4 108.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 C5 110.8(8) . . ? H4A C4 H4B 108.1 . . ? H4A C4 C5 109.5 . . ? H4B C4 C5 109.5 . . ? C4 C5 H5A 107.5 . . ? C4 C5 H5B 107.5 . . ? C4 C5 H5C 108.0 . . ? C4 C5 H5D 108.0 . . ? C4 C5 C6 119.4(13) . . ? C4 C5 C6X 117.3(16) . . ? H5A C5 H5B 107.0 . . ? H5A C5 C6 107.5 . . ? H5B C5 C6 107.5 . . ? H5C C5 H5D 107.2 . . ? H5C C5 C6X 108.0 . . ? H5D C5 C6X 108.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C6X H6X1 109.5 . . ? C5 C6X H6X2 109.5 . . ? C5 C6X H6X3 109.5 . . ? H6X1 C6X H6X2 109.5 . . ? H6X1 C6X H6X3 109.5 . . ? H6X2 C6X H6X3 109.5 . . ? N1 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? N1 C7 C8 116.1(6) . . ? H7A C7 H7B 107.4 . . ? H7A C7 C8 108.3 . . ? H7B C7 C8 108.3 . . ? C7 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C7 C8 C9 111.4(7) . . ? H8A C8 H8B 108.0 . . ? H8A C8 C9 109.3 . . ? H8B C8 C9 109.3 . . ? C8 C9 H9A 108.1 . . ? C8 C9 H9B 108.1 . . ? C8 C9 H9C 108.4 . . ? C8 C9 H9D 108.4 . . ? C8 C9 C10 116.7(12) . . ? C8 C9 C10X 115.4(17) . . ? H9A C9 H9B 107.3 . . ? H9A C9 C10 108.1 . . ? H9B C9 C10 108.1 . . ? H9C C9 H9D 107.5 . . ? H9C C9 C10X 108.4 . . ? H9D C9 C10X 108.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10X H10D 109.5 . . ? C9 C10X H10E 109.5 . . ? C9 C10X H10F 109.5 . . ? H10D C10X H10E 109.5 . . ? H10D C10X H10F 109.5 . . ? H10E C10X H10F 109.5 . . ? N1 C11 H11A 108.6 . . ? N1 C11 H11B 108.6 . . ? N1 C11 C12 114.7(6) . . ? H11A C11 H11B 107.6 . . ? H11A C11 C12 108.6 . . ? H11B C11 C12 108.6 . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C11 C12 C13 111.4(8) . . ? H12A C12 H12B 108.0 . . ? H12A C12 C13 109.4 . . ? H12B C12 C13 109.4 . . ? C12 C13 H13A 108.0 . . ? C12 C13 H13B 108.0 . . ? C12 C13 H13C 109.7 . . ? C12 C13 H13D 109.7 . . ? C12 C13 C14 117.3(11) . . ? C12 C13 C14X 109.8(12) . . ? H13A C13 H13B 107.2 . . ? H13A C13 C14 108.0 . . ? H13B C13 C14 108.0 . . ? H13C C13 H13D 108.2 . . ? H13C C13 C14X 109.7 . . ? H13D C13 C14X 109.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14X H14D 109.5 . . ? C13 C14X H14E 109.5 . . ? C13 C14X H14F 109.5 . . ? H14D C14X H14E 109.5 . . ? H14D C14X H14F 109.5 . . ? H14E C14X H14F 109.5 . . ? N1 C15 H15A 108.5 . . ? N1 C15 H15B 108.5 . . ? N1 C15 C16 115.2(6) . . ? H15A C15 H15B 107.5 . . ? H15A C15 C16 108.5 . . ? H15B C15 C16 108.5 . . ? C15 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? C15 C16 C17 112.3(8) . . ? H16A C16 H16B 107.9 . . ? H16A C16 C17 109.1 . . ? H16B C16 C17 109.1 . . ? C16 C17 H17A 108.1 . . ? C16 C17 H17B 108.1 . . ? C16 C17 C18 116.6(9) . . ? H17A C17 H17B 107.3 . . ? H17A C17 C18 108.1 . . ? H17B C17 C18 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Ti2 O11 C2 156.9(11) . . ? C19 N2 C23 111.7(6) . . ? C19 N2 C27 106.5(5) . . ? C19 N2 C31 111.3(5) . . ? C23 N2 C27 110.8(5) . . ? C23 N2 C31 106.2(5) . . ? C27 N2 C31 110.5(6) . . ? N2 C19 H19A 108.5 . . ? N2 C19 H19B 108.5 . . ? N2 C19 C20 115.0(6) . . ? H19A C19 H19B 107.5 . . ? H19A C19 C20 108.5 . . ? H19B C19 C20 108.5 . . ? C19 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C19 C20 C21 111.1(7) . . ? H20A C20 H20B 108.0 . . ? H20A C20 C21 109.4 . . ? H20B C20 C21 109.4 . . ? C20 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C20 C21 C22 111.2(8) . . ? H21A C21 H21B 108.0 . . ? H21A C21 C22 109.4 . . ? H21B C21 C22 109.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 108.3 . . ? N2 C23 H23B 108.3 . . ? N2 C23 C24 116.0(6) . . ? H23A C23 H23B 107.4 . . ? H23A C23 C24 108.3 . . ? H23B C23 C24 108.3 . . ? C23 C24 H24A 109.8 . . ? C23 C24 H24B 109.8 . . ? C23 C24 C25 109.4(7) . . ? H24A C24 H24B 108.3 . . ? H24A C24 C25 109.8 . . ? H24B C24 C25 109.8 . . ? C24 C25 H25A 108.2 . . ? C24 C25 H25B 108.2 . . ? C24 C25 H25C 108.4 . . ? C24 C25 H25D 108.4 . . ? C24 C25 C26 116.5(12) . . ? C24 C25 C26X 115.3(13) . . ? H25A C25 H25B 107.3 . . ? H25A C25 C26 108.2 . . ? H25B C25 C26 108.2 . . ? H25C C25 H25D 107.5 . . ? H25C C25 C26X 108.4 . . ? H25D C25 C26X 108.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26X H26D 109.5 . . ? C25 C26X H26E 109.5 . . ? C25 C26X H26F 109.5 . . ? H26D C26X H26E 109.5 . . ? H26D C26X H26F 109.5 . . ? H26E C26X H26F 109.5 . . ? N2 C27 H27A 108.1 . . ? N2 C27 H27B 108.1 . . ? N2 C27 C28 116.7(6) . . ? H27A C27 H27B 107.3 . . ? H27A C27 C28 108.1 . . ? H27B C27 C28 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 C29 110.9(6) . . ? H28A C28 H28B 108.1 . . ? H28A C28 C29 109.5 . . ? H28B C28 C29 109.5 . . ? C28 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C28 C29 C30 113.0(7) . . ? H29A C29 H29B 107.8 . . ? H29A C29 C30 109.0 . . ? H29B C29 C30 109.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 H31A 107.8 . . ? N2 C31 H31B 107.8 . . ? N2 C31 C32 118.0(6) . . ? H31A C31 H31B 107.1 . . ? H31A C31 C32 107.8 . . ? H31B C31 C32 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 C33 110.7(7) . . ? H32A C32 H32B 108.1 . . ? H32A C32 C33 109.5 . . ? H32B C32 C33 109.5 . . ? C32 C33 H33A 108.6 . . ? C32 C33 H33B 108.6 . . ? C32 C33 C34 114.5(8) . . ? H33A C33 H33B 107.6 . . ? H33A C33 C34 108.6 . . ? H33B C33 C34 108.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Ti2 O14 Mo5 116.3(3) 2_556 . ? Mo4 O14 Mo5 116.3(3) 2_556 . ? C35 N3 C39 109.9(6) . . ? C35 N3 C43 106.5(5) . . ? C35 N3 C47 111.2(6) . . ? C39 N3 C43 111.3(6) . . ? C39 N3 C47 106.9(6) . . ? C43 N3 C47 111.1(6) . . ? N3 C35 H35A 108.5 . . ? N3 C35 H35B 108.5 . . ? N3 C35 C36 115.3(6) . . ? H35A C35 H35B 107.5 . . ? H35A C35 C36 108.5 . . ? H35B C35 C36 108.5 . . ? C35 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? C35 C36 C37 110.0(7) . . ? H36A C36 H36B 108.2 . . ? H36A C36 C37 109.7 . . ? H36B C36 C37 109.7 . . ? C36 C37 H37A 108.0 . . ? C36 C37 H37B 108.0 . . ? C36 C37 H37C 108.2 . . ? C36 C37 H37D 108.2 . . ? C36 C37 C38 117.4(12) . . ? C36 C37 C38X 116.6(13) . . ? H37A C37 H37B 107.2 . . ? H37A C37 C38 108.0 . . ? H37B C37 C38 108.0 . . ? H37C C37 H37D 107.3 . . ? H37C C37 C38X 108.2 . . ? H37D C37 C38X 108.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C38X H38D 109.5 . . ? C37 C38X H38E 109.5 . . ? C37 C38X H38F 109.5 . . ? H38D C38X H38E 109.5 . . ? H38D C38X H38F 109.5 . . ? H38E C38X H38F 109.5 . . ? N3 C39 H39A 108.0 . . ? N3 C39 H39B 108.0 . . ? N3 C39 C40 117.3(7) . . ? H39A C39 H39B 107.2 . . ? H39A C39 C40 108.0 . . ? H39B C39 C40 108.0 . . ? C39 C40 H40A 109.6 . . ? C39 C40 H40B 109.6 . . ? C39 C40 C41 110.2(9) . . ? H40A C40 H40B 108.1 . . ? H40A C40 C41 109.6 . . ? H40B C40 C41 109.6 . . ? C40 C41 H41A 108.4 . . ? C40 C41 H41B 108.4 . . ? C40 C41 H41C 107.5 . . ? C40 C41 H41D 107.5 . . ? C40 C41 C42 115.6(12) . . ? C40 C41 C42X 119.2(17) . . ? H41A C41 H41B 107.4 . . ? H41A C41 C42 108.4 . . ? H41B C41 C42 108.4 . . ? H41C C41 H41D 107.0 . . ? H41C C41 C42X 107.5 . . ? H41D C41 C42X 107.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C42X H42D 109.5 . . ? C41 C42X H42E 109.5 . . ? C41 C42X H42F 109.5 . . ? H42D C42X H42E 109.5 . . ? H42D C42X H42F 109.5 . . ? H42E C42X H42F 109.5 . . ? N3 C43 H43A 108.4 . . ? N3 C43 H43B 108.4 . . ? N3 C43 C44 115.6(6) . . ? H43A C43 H43B 107.4 . . ? H43A C43 C44 108.4 . . ? H43B C43 C44 108.4 . . ? C43 C44 H44A 109.4 . . ? C43 C44 H44B 109.4 . . ? C43 C44 C45 111.0(7) . . ? H44A C44 H44B 108.0 . . ? H44A C44 C45 109.4 . . ? H44B C44 C45 109.4 . . ? C44 C45 H45A 108.8 . . ? C44 C45 H45B 108.8 . . ? C44 C45 C46 113.7(10) . . ? H45A C45 H45B 107.7 . . ? H45A C45 C46 108.8 . . ? H45B C45 C46 108.8 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N3 C47 H47A 108.4 . . ? N3 C47 H47B 108.4 . . ? N3 C47 C48 115.5(6) . . ? H47A C47 H47B 107.5 . . ? H47A C47 C48 108.4 . . ? H47B C47 C48 108.4 . . ? C47 C48 H48A 109.9 . . ? C47 C48 H48B 109.9 . . ? C47 C48 C49 109.1(8) . . ? H48A C48 H48B 108.3 . . ? H48A C48 C49 109.9 . . ? H48B C48 C49 109.9 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? C48 C49 C50 110.6(10) . . ? H49A C49 H49B 108.1 . . ? H49A C49 C50 109.5 . . ? H49B C49 C50 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.417 _refine_diff_density_min -2.481 _refine_diff_density_rms 0.128 # Contents of RES file _computing_special_details ; TITL rje253 in C2/c CELL 0.71073 29.4619 18.6123 27.2737 90.000 113.343 90.000 ZERR 8.00 0.0007 0.0007 0.0009 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O TI MO UNIT 392 888 24 152 8 40 TEMP -113 SIZE 0.42 0.44 0.62 OMIT -3 50 L.S. 8 ACTA BOND $H FMAP 2 PLAN 10 EXYZ TI1 MO1 EADP TI1 MO1 EXYZ TI2 MO4 EADP TI2 MO4 CONN $TI $MO 6 SIMU C3 > C14X C23 > C26X C35 > C42X DELU C3 > C14X C23 > C26X C35 > C42X REM EXTI 0.000016 INSIGNIFICANT WGHT 0.024000 192.256104 FVAR 0.03070 0.65994 0.68155 0.55355 0.56910 0.59109 0.67588 PART 1 TI1 5 0.237798 0.363468 0.521531 10.50000 0.02260 0.02549 = 0.02214 -0.00714 0.00909 0.00034 PART 2 MO1 6 0.237798 0.363468 0.521531 10.50000 0.02260 0.02549 = 0.02214 -0.00714 0.00909 0.00034 PART 0 MO2 6 0.335276 0.267821 0.538190 11.00000 0.01737 0.03347 = 0.02582 -0.00689 0.00841 -0.00100 MO3 6 0.252335 0.209578 0.582194 11.00000 0.02629 0.03321 = 0.02080 -0.00009 0.01154 0.00201 PART 1 TI2 5 0.082155 0.250354 0.777240 10.50000 0.02443 0.05571 = 0.03912 0.00091 0.01340 0.00787 PART 2 MO4 6 0.082155 0.250354 0.777240 10.50000 0.02443 0.05571 = 0.03912 0.00091 0.01340 0.00787 PART 0 MO5 6 -0.005077 0.340407 0.687669 11.00000 0.04916 0.03121 = 0.04057 0.01224 0.02690 0.00633 MO6 6 -0.005598 0.163604 0.687259 11.00000 0.09406 0.03302 = 0.06285 -0.02043 0.05965 -0.02172 O1 4 0.257874 0.179546 0.642911 11.00000 0.04066 0.03689 = 0.02398 -0.00111 0.01647 0.00055 O2 4 0.184694 0.202553 0.538865 11.00000 0.02502 0.03477 = 0.02124 -0.00798 0.01076 -0.00208 O3 4 0.323996 0.232430 0.596859 11.00000 0.02137 0.03060 = 0.01831 -0.00467 0.00585 0.00209 O4 4 0.397190 0.281738 0.562163 11.00000 0.02332 0.04514 = 0.03146 -0.00887 0.01156 -0.00307 O5 4 0.309653 0.358177 0.545780 11.00000 0.02397 0.02828 = 0.02720 -0.00629 0.00918 -0.00323 O6 4 0.235638 0.375577 0.450390 11.00000 0.02842 0.02675 = 0.02414 -0.00268 0.00980 0.00290 O7 4 0.228417 0.449485 0.541132 11.00000 0.03558 0.02617 = 0.04353 -0.01103 0.01182 0.00221 O8 4 0.171448 0.327598 0.489988 11.00000 0.02045 0.03151 = 0.02863 -0.00368 0.00839 0.00190 O9 4 0.245558 0.310700 0.586601 11.00000 0.03177 0.02950 = 0.02947 -0.00895 0.01710 0.00353 O10 4 0.250000 0.250000 0.500000 10.50000 0.02093 0.02877 = 0.02301 -0.00219 0.01125 0.00046 O12 4 0.063470 0.324023 0.722204 11.00000 0.04354 0.03330 = 0.06483 -0.00217 0.03634 -0.00378 O15 4 0.000000 0.396884 0.750000 10.50000 0.06238 0.02092 = 0.09395 0.00000 0.05495 0.00000 O16 4 -0.008706 0.251121 0.648871 11.00000 0.05838 0.06422 = 0.03487 -0.00487 0.02605 -0.01201 O17 4 -0.071755 0.179287 0.677842 11.00000 0.07015 0.08948 = 0.06440 -0.04718 0.04013 -0.04156 O19 4 0.000000 0.107778 0.750000 10.50000 0.11432 0.02324 = 0.11324 0.00000 0.09253 0.00000 O20 4 0.062894 0.180134 0.720969 11.00000 0.06880 0.03379 = 0.07239 -0.00048 0.04891 0.00873 O21 4 0.000000 0.252006 0.750000 10.50000 0.04351 0.02157 = 0.03263 0.00000 0.02202 0.00000 PART 1 C1 1 0.205978 0.475203 0.578212 10.50000 0.04445 0.06407 = 0.07356 -0.02685 0.01914 0.00419 AFIX 33 H1A 2 0.207255 0.527798 0.579880 10.50000 -1.50000 H1B 2 0.224433 0.455412 0.613926 10.50000 -1.50000 H1C 2 0.171484 0.459319 0.565225 10.50000 -1.50000 AFIX 0 C2 1 0.197543 0.244616 0.839767 10.50000 0.04197 0.06859 = 0.11309 -0.02518 0.01153 0.00335 AFIX 33 H2A 2 0.220314 0.252532 0.822093 10.50000 -1.50000 H2B 2 0.202626 0.196294 0.855293 10.50000 -1.50000 H2C 2 0.203837 0.280351 0.868102 10.50000 -1.50000 AFIX 0 PART 0 SAME N1 C3 C4 C5 C6 SAME N1 C3 C4 C5 C6X SAME N1 C7 C8 C9 C10 SAME N1 C7 C8 C9 C10X SAME N1 C11 C12 C13 C14 SAME N1 C11 C12 C13 C14X N1 3 -0.066121 0.728209 0.438964 11.00000 0.04911 0.06334 = 0.04923 -0.00006 0.03773 0.00537 C3 1 -0.079241 0.803732 0.449814 11.00000 0.04493 0.06055 = 0.05452 -0.00720 0.03348 0.00108 AFIX 23 H3A 2 -0.115198 0.805805 0.441041 11.00000 -1.20000 H3B 2 -0.061871 0.813869 0.488441 11.00000 -1.20000 AFIX 0 C4 1 -0.066343 0.861660 0.418951 11.00000 0.05995 0.06485 = 0.09334 0.00239 0.04471 -0.00933 AFIX 23 H4A 2 -0.029953 0.866177 0.432198 11.00000 -1.20000 H4B 2 -0.079094 0.848236 0.380725 11.00000 -1.20000 AFIX 0 C5 1 -0.088033 0.932152 0.424763 11.00000 0.08716 0.06236 = 0.14895 0.00014 0.06009 -0.00981 PART 1 AFIX 23 H5A 2 -0.080830 0.967151 0.401463 21.00000 -1.20000 H5B 2 -0.124383 0.926191 0.410336 21.00000 -1.20000 AFIX 23 PART 2 H5C 2 -0.123529 0.931854 0.400729 -21.00000 -1.20000 H5D 2 -0.086025 0.935530 0.461793 -21.00000 -1.20000 AFIX 0 PART 1 C6 1 -0.073706 0.962746 0.474414 21.00000 0.20496 0.06743 = 0.14126 -0.00455 0.05030 0.03796 AFIX 33 H6A 2 -0.092163 1.007407 0.471717 21.00000 -1.50000 H6B 2 -0.038229 0.973297 0.488503 21.00000 -1.50000 H6C 2 -0.080493 0.929381 0.498478 21.00000 -1.50000 AFIX 0 PART 2 C6X 1 -0.066945 0.993935 0.414155 -21.00000 0.09896 AFIX 33 H6X1 2 -0.084445 1.036276 0.419113 -21.00000 -1.50000 H6X2 2 -0.069466 0.992530 0.377244 -21.00000 -1.50000 H6X3 2 -0.032064 0.996533 0.438634 -21.00000 -1.50000 AFIX 0 PART 0 C7 1 -0.011151 0.722122 0.451641 11.00000 0.05008 0.09214 = 0.05439 0.00357 0.03900 0.00914 AFIX 23 H7A 2 -0.004490 0.673082 0.442085 11.00000 -1.20000 H7B 2 -0.002998 0.756188 0.428452 11.00000 -1.20000 AFIX 0 C8 1 0.023142 0.736432 0.508654 11.00000 0.06133 0.11908 = 0.05540 -0.00243 0.03464 0.01411 AFIX 23 H8A 2 0.016388 0.784862 0.519196 11.00000 -1.20000 H8B 2 0.016856 0.700893 0.532241 11.00000 -1.20000 AFIX 0 C9 1 0.076120 0.731986 0.515894 11.00000 0.05854 0.12547 = 0.09832 -0.00646 0.02863 0.00879 PART 1 AFIX 23 H9A 2 0.082405 0.682773 0.506302 31.00000 -1.20000 H9B 2 0.081077 0.765344 0.490173 31.00000 -1.20000 AFIX 23 PART 2 H9C 2 0.096808 0.726982 0.554496 -31.00000 -1.20000 H9D 2 0.080578 0.687881 0.497999 -31.00000 -1.20000 AFIX 0 PART 1 C10 1 0.111774 0.747733 0.567077 31.00000 0.07248 0.21530 = 0.08807 -0.01936 0.01630 0.00766 AFIX 33 H10A 2 0.144908 0.741943 0.567276 31.00000 -1.50000 H10B 2 0.107776 0.714875 0.593162 31.00000 -1.50000 H10C 2 0.107494 0.797359 0.576477 31.00000 -1.50000 AFIX 0 PART 2 C10X 1 0.093490 0.790280 0.496309 -31.00000 0.07097 0.16119 = 0.10787 0.00101 0.02816 -0.02176 AFIX 33 H10D 2 0.128318 0.782559 0.502840 -31.00000 -1.50000 H10E 2 0.090315 0.834244 0.514470 -31.00000 -1.50000 H10F 2 0.074056 0.795040 0.457840 -31.00000 -1.50000 AFIX 0 PART 0 C11 1 -0.093513 0.707798 0.380635 11.00000 0.05330 0.06893 = 0.05209 -0.00368 0.03606 -0.00096 AFIX 23 H11A 2 -0.080593 0.737338 0.358834 11.00000 -1.20000 H11B 2 -0.086213 0.656904 0.376083 11.00000 -1.20000 AFIX 0 C12 1 -0.148957 0.717270 0.359360 11.00000 0.05246 0.09638 = 0.06199 -0.01789 0.03501 -0.01744 AFIX 23 H12A 2 -0.161247 0.698777 0.385876 11.00000 -1.20000 H12B 2 -0.157077 0.769063 0.354027 11.00000 -1.20000 AFIX 0 C13 1 -0.174246 0.678392 0.307616 11.00000 0.08156 0.14972 = 0.07015 -0.03294 0.01916 -0.01786 PART 1 AFIX 23 H13A 2 -0.161752 0.698144 0.281621 41.00000 -1.20000 H13B 2 -0.164122 0.627321 0.313384 41.00000 -1.20000 AFIX 23 PART 2 H13C 2 -0.200137 0.709479 0.282108 -41.00000 -1.20000 H13D 2 -0.149995 0.666729 0.292002 -41.00000 -1.20000 AFIX 0 PART 1 C14 1 -0.224659 0.680774 0.284850 41.00000 0.07192 0.10284 = 0.06553 -0.03386 0.02438 -0.00007 AFIX 33 H14A 2 -0.236653 0.654183 0.251075 41.00000 -1.50000 H14B 2 -0.235573 0.730883 0.278035 41.00000 -1.50000 H14C 2 -0.237950 0.658966 0.309091 41.00000 -1.50000 AFIX 0 PART 2 C14X 1 -0.196164 0.613503 0.316453 -41.00000 0.07959 0.15371 = 0.10174 -0.07941 0.05335 -0.04592 AFIX 33 H14D 2 -0.212269 0.587864 0.282545 -41.00000 -1.50000 H14E 2 -0.220757 0.625349 0.331043 -41.00000 -1.50000 H14F 2 -0.170444 0.582959 0.341810 -41.00000 -1.50000 AFIX 0 PART 0 C15 1 -0.080761 0.678376 0.474661 11.00000 0.07275 0.05722 = 0.05071 -0.00561 0.04847 0.00705 AFIX 23 H15A 2 -0.063747 0.694638 0.512104 11.00000 -1.20000 H15B 2 -0.116763 0.683191 0.464886 11.00000 -1.20000 AFIX 0 C16 1 -0.069059 0.600242 0.471770 11.00000 0.09900 0.06623 = 0.08459 0.01436 0.06931 0.01581 AFIX 23 H16A 2 -0.091226 0.580760 0.436641 11.00000 -1.20000 H16B 2 -0.034627 0.595682 0.474605 11.00000 -1.20000 AFIX 0 C17 1 -0.074970 0.556747 0.515197 11.00000 0.15824 0.06307 = 0.13300 0.02892 0.11506 0.03440 AFIX 23 H17A 2 -0.053271 0.577675 0.549989 11.00000 -1.20000 H17B 2 -0.109494 0.562027 0.511914 11.00000 -1.20000 AFIX 0 C18 1 -0.063976 0.480378 0.516228 11.00000 0.12819 0.12036 = 0.10610 0.04703 0.07479 0.04652 AFIX 33 H18A 2 -0.069299 0.457487 0.545875 11.00000 -1.50000 H18B 2 -0.029454 0.473932 0.521033 11.00000 -1.50000 H18C 2 -0.085774 0.458300 0.482470 11.00000 -1.50000 AFIX 0 O13 4 -0.011259 0.401844 0.639818 11.00000 0.09056 0.06732 = 0.08423 0.04400 0.05543 0.02410 O11 4 0.147116 0.251516 0.801094 11.00000 0.03499 0.15232 = 0.07419 0.00528 0.02311 0.01970 SAME N2 C23 C24 C25 C26X SAME N2 C23 C24 C25 C26 N2 3 -0.127627 -0.026751 0.671206 11.00000 0.05112 0.03182 = 0.02669 -0.00747 0.01087 -0.00963 C19 1 -0.130473 0.026338 0.712346 11.00000 0.06353 0.04228 = 0.03532 -0.01352 0.02182 -0.01435 AFIX 23 H19A 2 -0.111075 0.006946 0.748440 11.00000 -1.20000 H19B 2 -0.114666 0.071858 0.708777 11.00000 -1.20000 AFIX 0 C20 1 -0.182178 0.042810 0.708068 11.00000 0.07468 0.06375 = 0.05838 -0.02278 0.03462 -0.01119 AFIX 23 H20A 2 -0.199713 -0.002713 0.707637 11.00000 -1.20000 H20B 2 -0.200625 0.068348 0.674112 11.00000 -1.20000 AFIX 0 C21 1 -0.180975 0.089141 0.754824 11.00000 0.08887 0.06832 = 0.07576 -0.02720 0.05809 -0.02478 AFIX 23 H21A 2 -0.164996 0.061968 0.788544 11.00000 -1.20000 H21B 2 -0.161037 0.132790 0.757091 11.00000 -1.20000 AFIX 0 C22 1 -0.232083 0.110589 0.748284 11.00000 0.12643 0.11243 = 0.11045 -0.03417 0.08501 -0.00514 AFIX 33 H22A 2 -0.230234 0.140371 0.778651 11.00000 -1.50000 H22B 2 -0.251645 0.067436 0.746799 11.00000 -1.50000 H22C 2 -0.247793 0.137987 0.715126 11.00000 -1.50000 AFIX 0 C23 1 -0.157558 -0.001471 0.614606 11.00000 0.04630 0.03980 = 0.02960 -0.00917 0.01122 -0.00577 AFIX 23 H23A 2 -0.155017 -0.038293 0.589621 11.00000 -1.20000 H23B 2 -0.192713 0.001292 0.609475 11.00000 -1.20000 AFIX 0 C24 1 -0.142821 0.070254 0.599357 11.00000 0.06010 0.04658 = 0.04420 0.00313 0.00926 -0.01485 AFIX 23 H24A 2 -0.107774 0.068743 0.603955 11.00000 -1.20000 H24B 2 -0.146456 0.108403 0.622838 11.00000 -1.20000 AFIX 0 C25 1 -0.175480 0.086795 0.541692 11.00000 0.09776 0.09106 = 0.06287 0.02988 -0.00656 -0.02756 PART 1 AFIX 23 H25A 2 -0.210381 0.082165 0.537214 51.00000 -1.20000 H25B 2 -0.170097 0.137575 0.534603 51.00000 -1.20000 AFIX 23 PART 2 H25C 2 -0.180730 0.041826 0.520772 -51.00000 -1.20000 H25D 2 -0.208122 0.102840 0.539950 -51.00000 -1.20000 AFIX 0 PART 1 C26 1 -0.168450 0.043272 0.502163 51.00000 0.20891 0.10298 = 0.04016 0.01811 0.02639 -0.06077 AFIX 33 H26A 2 -0.191604 0.058298 0.466589 51.00000 -1.50000 H26B 2 -0.174451 -0.007198 0.507928 51.00000 -1.50000 H26C 2 -0.134471 0.048841 0.504838 51.00000 -1.50000 AFIX 0 PART 2 C26X 1 -0.156301 0.141619 0.516216 -51.00000 0.15765 0.08859 = 0.07657 0.03079 0.03343 -0.02494 AFIX 33 H26D 2 -0.179828 0.148782 0.479262 -51.00000 -1.50000 H26E 2 -0.124487 0.125746 0.516485 -51.00000 -1.50000 H26F 2 -0.151782 0.186934 0.535892 -51.00000 -1.50000 AFIX 0 PART 0 C27 1 -0.073329 -0.033501 0.681191 11.00000 0.03832 0.04338 = 0.02998 -0.00556 0.00504 -0.00601 AFIX 23 H27A 2 -0.059900 0.015456 0.682040 11.00000 -1.20000 H27B 2 -0.055780 -0.054773 0.717055 11.00000 -1.20000 AFIX 0 C28 1 -0.061178 -0.077549 0.641586 11.00000 0.04438 0.05279 = 0.04012 -0.01434 0.00530 -0.00315 AFIX 23 H28A 2 -0.073276 -0.052425 0.606749 11.00000 -1.20000 H28B 2 -0.078188 -0.124549 0.636356 11.00000 -1.20000 AFIX 0 C29 1 -0.005789 -0.089501 0.661074 11.00000 0.04419 0.05560 = 0.05648 -0.01382 0.00834 -0.00222 AFIX 23 H29A 2 0.011203 -0.042436 0.669762 11.00000 -1.20000 H29B 2 0.005537 -0.118326 0.694285 11.00000 -1.20000 AFIX 0 C30 1 0.008888 -0.127670 0.620335 11.00000 0.04808 0.12864 = 0.08318 -0.02944 0.01629 0.01310 AFIX 33 H30A 2 0.044791 -0.134679 0.635190 11.00000 -1.50000 H30B 2 -0.001011 -0.098494 0.587843 11.00000 -1.50000 H30C 2 -0.007645 -0.174464 0.611685 11.00000 -1.50000 AFIX 0 C31 1 -0.148713 -0.099473 0.676608 11.00000 0.05918 0.02933 = 0.03802 -0.01328 0.01522 -0.01930 AFIX 23 H31A 2 -0.184447 -0.093078 0.667829 11.00000 -1.20000 H31B 2 -0.145718 -0.131789 0.649212 11.00000 -1.20000 AFIX 0 C32 1 -0.126371 -0.137399 0.729783 11.00000 0.07068 0.03910 = 0.02848 -0.00495 0.01625 -0.01459 AFIX 23 H32A 2 -0.090860 -0.146509 0.738782 11.00000 -1.20000 H32B 2 -0.129094 -0.106328 0.757956 11.00000 -1.20000 AFIX 0 C33 1 -0.152333 -0.207454 0.728082 11.00000 0.09825 0.04606 = 0.06205 -0.00205 0.03092 -0.02447 AFIX 23 H33A 2 -0.188014 -0.197774 0.717464 11.00000 -1.20000 H33B 2 -0.148845 -0.238256 0.700185 11.00000 -1.20000 AFIX 0 C34 1 -0.133577 -0.248059 0.779825 11.00000 0.11410 0.04423 = 0.06499 0.00649 0.03372 -0.01093 AFIX 33 H34A 2 -0.152835 -0.292255 0.775661 11.00000 -1.50000 H34B 2 -0.136959 -0.218208 0.807786 11.00000 -1.50000 H34C 2 -0.098684 -0.260241 0.789832 11.00000 -1.50000 AFIX 0 O14 4 -0.071690 0.322710 0.677295 11.00000 0.03540 0.10571 = 0.05647 0.04184 0.02015 0.01853 O18 4 -0.010696 0.099489 0.641452 11.00000 0.12932 0.07560 = 0.10921 -0.05697 0.09609 -0.05007 SAME N3 C39 C40 C41 C42X SAME N3 C39 C40 C41 C42 SAME N3 C35 C36 C37 C38 SAME N3 C35 C36 C37 C38X N3 3 0.147753 0.496402 0.336725 11.00000 0.04453 0.03838 = 0.05379 0.01457 0.02211 0.01670 C35 1 0.127664 0.426121 0.348766 11.00000 0.04836 0.05055 = 0.05975 0.02339 0.02180 0.01464 AFIX 23 H35A 2 0.135547 0.387026 0.328803 11.00000 -1.20000 H35B 2 0.145161 0.415519 0.387305 11.00000 -1.20000 AFIX 0 C36 1 0.072659 0.425094 0.335038 11.00000 0.04786 0.07617 = 0.07331 0.03177 0.02702 0.01575 AFIX 23 H36A 2 0.054525 0.437306 0.296868 11.00000 -1.20000 H36B 2 0.064393 0.461497 0.356664 11.00000 -1.20000 AFIX 0 C37 1 0.056987 0.351149 0.346058 11.00000 0.04763 0.09608 = 0.11168 0.03843 0.02319 0.00283 PART 1 AFIX 23 H37A 2 0.067305 0.315578 0.325503 61.00000 -1.20000 H37B 2 0.075615 0.340343 0.384394 61.00000 -1.20000 AFIX 23 PART 2 H37C 2 0.079090 0.337004 0.382792 -61.00000 -1.20000 H37D 2 0.023129 0.354983 0.345098 -61.00000 -1.20000 AFIX 0 PART 1 C38 1 0.006194 0.340329 0.334077 61.00000 0.05043 0.15848 = 0.21817 0.10237 0.03004 -0.00134 AFIX 33 H38A 2 0.000964 0.290957 0.343197 61.00000 -1.50000 H38B 2 -0.012919 0.348497 0.295884 61.00000 -1.50000 H38C 2 -0.004668 0.374033 0.354844 61.00000 -1.50000 AFIX 0 PART 2 C38X 1 0.057294 0.295415 0.310999 -61.00000 0.07132 AFIX 33 H38D 2 0.047322 0.250246 0.322324 -61.00000 -1.50000 H38E 2 0.090660 0.290269 0.311727 -61.00000 -1.50000 H38F 2 0.034115 0.307083 0.274636 -61.00000 -1.50000 AFIX 0 PART 0 C39 1 0.141653 0.556036 0.371505 11.00000 0.06558 0.05011 = 0.07531 0.00206 0.03857 0.02114 AFIX 23 H39A 2 0.151272 0.601827 0.359808 11.00000 -1.20000 H39B 2 0.106105 0.559640 0.364561 11.00000 -1.20000 AFIX 0 C40 1 0.170280 0.549349 0.431111 11.00000 0.09361 0.08023 = 0.07197 0.00122 0.04385 0.02239 AFIX 23 H40A 2 0.205696 0.541309 0.438945 11.00000 -1.20000 H40B 2 0.157970 0.507548 0.444678 11.00000 -1.20000 AFIX 0 C41 1 0.164392 0.618168 0.459386 11.00000 0.13876 0.13638 = 0.08825 -0.03325 0.05862 0.03841 PART 1 AFIX 23 H41A 2 0.128671 0.628626 0.447484 71.00000 -1.20000 H41B 2 0.177537 0.608751 0.498274 71.00000 -1.20000 AFIX 23 PART 2 H41C 2 0.172733 0.659441 0.441606 -71.00000 -1.20000 H41D 2 0.128972 0.622775 0.452805 -71.00000 -1.20000 AFIX 0 PART 1 C42 1 0.187814 0.679440 0.450709 71.00000 0.19368 0.07923 = 0.08376 -0.01461 0.01544 0.04446 AFIX 33 H42A 2 0.181162 0.720476 0.469387 71.00000 -1.50000 H42B 2 0.175126 0.689661 0.412352 71.00000 -1.50000 H42C 2 0.223539 0.671049 0.464316 71.00000 -1.50000 AFIX 0 PART 2 C42X 1 0.192024 0.625640 0.515220 -71.00000 0.13304 0.17004 = 0.10397 -0.05482 0.03985 0.06131 AFIX 33 H42D 2 0.183986 0.671682 0.527281 -71.00000 -1.50000 H42E 2 0.227425 0.624094 0.522807 -71.00000 -1.50000 H42F 2 0.183722 0.586300 0.534083 -71.00000 -1.50000 AFIX 0 PART 0 C43 1 0.201668 0.483405 0.348214 11.00000 0.04632 0.04115 = 0.04730 0.01048 0.02227 0.01690 AFIX 23 H43A 2 0.218236 0.466088 0.385438 11.00000 -1.20000 H43B 2 0.203800 0.444512 0.324455 11.00000 -1.20000 AFIX 0 C44 1 0.229846 0.547648 0.341195 11.00000 0.05565 0.05288 = 0.06606 0.01607 0.02246 0.00584 AFIX 23 H44A 2 0.226924 0.587792 0.363581 11.00000 -1.20000 H44B 2 0.215270 0.563421 0.303449 11.00000 -1.20000 AFIX 0 C45 1 0.283875 0.529601 0.356804 11.00000 0.06475 0.07291 = 0.12325 -0.00506 0.05327 -0.00657 AFIX 23 H45A 2 0.298476 0.516049 0.395027 11.00000 -1.20000 H45B 2 0.286316 0.487381 0.335902 11.00000 -1.20000 AFIX 0 C46 1 0.313467 0.589908 0.347973 11.00000 0.07342 0.12233 = 0.13641 0.02650 0.03768 -0.02290 AFIX 33 H46A 2 0.347861 0.574516 0.358552 11.00000 -1.50000 H46B 2 0.312249 0.631462 0.369486 11.00000 -1.50000 H46C 2 0.299650 0.603197 0.310105 11.00000 -1.50000 AFIX 0 C47 1 0.119410 0.519170 0.279004 11.00000 0.05505 0.03737 = 0.06052 0.02121 0.01880 0.01411 AFIX 23 H47A 2 0.084606 0.528229 0.273479 11.00000 -1.20000 H47B 2 0.133376 0.565158 0.273115 11.00000 -1.20000 AFIX 0 C48 1 0.119944 0.466375 0.237690 11.00000 0.06662 0.05441 = 0.05252 0.01560 0.01507 0.01630 AFIX 23 H48A 2 0.109991 0.418305 0.245430 11.00000 -1.20000 H48B 2 0.153732 0.462705 0.238428 11.00000 -1.20000 AFIX 0 C49 1 0.084437 0.491391 0.183211 11.00000 0.12492 0.05713 = 0.05998 0.01289 0.00926 -0.00496 AFIX 23 H49A 2 0.092202 0.541620 0.177408 11.00000 -1.20000 H49B 2 0.050242 0.490110 0.181480 11.00000 -1.20000 AFIX 0 C50 1 0.088100 0.443328 0.139310 11.00000 0.18862 0.09134 = 0.05275 0.00517 0.02175 -0.00804 AFIX 33 H50A 2 0.064747 0.460181 0.104368 11.00000 -1.50000 H50B 2 0.080103 0.393695 0.144887 11.00000 -1.50000 H50C 2 0.121793 0.445366 0.140599 11.00000 -1.50000 HKLF 4 REM rje253 in C2/c REM R1 = 0.0682 for 11036 Fo > 4sig(Fo) and 0.0747 for all 12093 data REM 756 parameters refined using 261 restraints END WGHT 0.0239 192.2869 REM Highest difference peak 2.417, deepest hole -2.481, 1-sigma level 0.128 Q1 1 0.0253 0.1640 0.7112 11.00000 0.05 2.42 Q2 1 -0.0170 0.1987 0.6706 11.00000 0.05 1.36 Q3 1 0.0910 0.2867 0.7997 11.00000 0.05 1.03 Q4 1 0.2558 0.2206 0.8980 11.00000 0.05 0.93 Q5 1 0.3704 0.2617 0.5485 11.00000 0.05 0.79 Q6 1 0.2873 0.2187 0.5902 11.00000 0.05 0.76 Q7 1 -0.0391 0.3442 0.6808 11.00000 0.05 0.74 Q8 1 0.1819 0.6421 0.6105 11.00000 0.05 0.65 Q9 1 0.2402 0.2522 0.8569 11.00000 0.05 0.63 Q10 1 0.0155 0.4323 0.6671 11.00000 0.05 0.63 ; #===END data_rje479_salt_of_4 _database_code_depnum_ccdc_archive 'CCDC 832953' #TrackingRef '- TiMo5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C16 H36 N +,C4 H9 Mo5 O19 Ti 3-,0.5 C2 H3 N' _chemical_formula_sum 'C53 H118.5 Mo5 N3.5 O19 Ti' _chemical_formula_weight 1636.62 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' Ti Ti 0.2776 0.4457 '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 'P 21/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 24.9233(5) _cell_length_b 33.6182(8) _cell_length_c 16.8302(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.915(2) _cell_angle_gamma 90.00 _cell_volume 14099.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38987 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 29.53 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6760 _exptl_absorpt_coefficient_mu 1.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 134551 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 29.64 _reflns_number_total 34144 _reflns_number_gt 22904 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0114P)^2^+78.6078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 34144 _refine_ls_number_parameters 1535 _refine_ls_number_restraints 3238 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.309211(18) 0.386580(12) 0.44863(2) 0.02392(9) Uani 1 1 d . . . Mo2 Mo 0.221929(17) 0.420244(12) 0.31664(3) 0.02173(9) Uani 1 1 d . . . Mo3 Mo 0.29132(2) 0.379875(13) 0.17287(2) 0.02860(11) Uani 1 1 d . . . Mo4 Mo 0.379601(17) 0.346499(12) 0.30469(3) 0.02397(9) Uani 1 1 d . . . Mo5 Mo 0.251300(17) 0.324191(12) 0.32215(3) 0.02345(9) Uani 1 1 d . . . Ti1 Ti 0.34620(3) 0.43791(3) 0.29999(5) 0.02388(19) Uani 1 1 d . . . O1 O 0.38400(14) 0.48292(10) 0.2912(2) 0.0360(9) Uani 1 1 d . . . O2 O 0.31806(17) 0.38550(11) 0.5492(2) 0.0398(10) Uani 1 1 d . . . O3 O 0.16483(14) 0.44694(11) 0.3294(2) 0.0344(9) Uani 1 1 d . . . O4 O 0.2806(2) 0.37827(13) 0.0734(2) 0.0528(12) Uani 1 1 d . . . O5 O 0.43535(15) 0.31795(10) 0.2934(2) 0.0375(9) Uani 1 1 d . . . O6 O 0.21367(15) 0.28245(11) 0.3287(2) 0.0383(9) Uani 1 1 d . . . O7 O 0.34995(14) 0.42890(10) 0.4160(2) 0.0276(8) Uani 1 1 d . . . O8 O 0.27492(13) 0.45889(9) 0.31414(19) 0.0229(7) Uani 1 1 d . . . O9 O 0.32776(15) 0.42751(10) 0.1894(2) 0.0315(8) Uani 1 1 d . . . O10 O 0.40389(14) 0.39789(10) 0.2912(2) 0.0323(9) Uani 1 1 d . . . O11 O 0.37273(14) 0.35233(10) 0.4141(2) 0.0277(8) Uani 1 1 d . . . O12 O 0.24427(14) 0.41273(10) 0.43321(19) 0.0258(8) Uani 1 1 d . . . O13 O 0.22537(15) 0.41105(10) 0.2080(2) 0.0305(8) Uani 1 1 d . . . O14 O 0.35358(15) 0.34975(10) 0.1899(2) 0.0331(9) Uani 1 1 d . . . O15 O 0.27102(14) 0.33608(10) 0.42927(19) 0.0263(8) Uani 1 1 d . . . O16 O 0.19824(13) 0.36559(10) 0.3300(2) 0.0296(8) Uani 1 1 d . . . O17 O 0.24930(15) 0.33514(10) 0.2099(2) 0.0324(8) Uani 1 1 d . . . O18 O 0.32261(13) 0.30579(9) 0.30861(19) 0.0239(7) Uani 1 1 d . . . O19 O 0.30103(12) 0.38356(9) 0.31101(17) 0.0172(6) Uani 1 1 d . . . C1 C 0.4306(2) 0.50659(17) 0.2982(3) 0.0348(13) Uani 1 1 d . . . C2 C 0.4143(3) 0.54932(19) 0.3066(5) 0.061(2) Uani 1 1 d . . . H2A H 0.3942 0.5527 0.3557 0.091 Uiso 1 1 calc R . . H2B H 0.3916 0.5570 0.2610 0.091 Uiso 1 1 calc R . . H2C H 0.4464 0.5662 0.3085 0.091 Uiso 1 1 calc R . . C3 C 0.4619(3) 0.5011(2) 0.2224(4) 0.0575(19) Uani 1 1 d . . . H3A H 0.4720 0.4731 0.2169 0.086 Uiso 1 1 calc R . . H3B H 0.4944 0.5176 0.2246 0.086 Uiso 1 1 calc R . . H3C H 0.4396 0.5091 0.1767 0.086 Uiso 1 1 calc R . . C4 C 0.4621(3) 0.4921(2) 0.3704(4) 0.0571(19) Uani 1 1 d . . . H4A H 0.4723 0.4642 0.3628 0.086 Uiso 1 1 calc R . . H4B H 0.4399 0.4945 0.4177 0.086 Uiso 1 1 calc R . . H4C H 0.4946 0.5083 0.3774 0.086 Uiso 1 1 calc R . . Mo6 Mo 0.892670(18) 0.400886(14) 0.28297(3) 0.02932(11) Uani 1 1 d . . . Mo7 Mo 0.78678(2) 0.437746(12) 0.18718(3) 0.02968(11) Uani 1 1 d . . . Mo8 Mo 0.746917(17) 0.347246(13) 0.14283(2) 0.02361(9) Uani 1 1 d . . . Mo9 Mo 0.852283(16) 0.310189(12) 0.23777(2) 0.02008(9) Uani 1 1 d . . . Mo10 Mo 0.770987(16) 0.372065(12) 0.33008(2) 0.01909(9) Uani 1 1 d . . . Ti2 Ti 0.86520(4) 0.37592(3) 0.10415(5) 0.0271(2) Uani 1 1 d . . . O20 O 0.90402(16) 0.38150(11) 0.0165(2) 0.0395(10) Uani 1 1 d . . . O21 O 0.94300(16) 0.42291(13) 0.3359(2) 0.0480(11) Uani 1 1 d . . . O22 O 0.75877(18) 0.48330(10) 0.1713(2) 0.0451(11) Uani 1 1 d . . . O23 O 0.69285(14) 0.32562(11) 0.0980(2) 0.0332(9) Uani 1 1 d . . . O24 O 0.87740(14) 0.26445(10) 0.2595(2) 0.0293(8) Uani 1 1 d . . . O25 O 0.73557(14) 0.36929(10) 0.41530(19) 0.0255(8) Uani 1 1 d . . . O26 O 0.91549(14) 0.40117(10) 0.1799(2) 0.0331(9) Uani 1 1 d . . . O27 O 0.82635(16) 0.42792(10) 0.0989(2) 0.0345(9) Uani 1 1 d . . . O28 O 0.79821(14) 0.35146(10) 0.06514(19) 0.0274(8) Uani 1 1 d . . . O29 O 0.88750(13) 0.32483(9) 0.14541(19) 0.0257(8) Uani 1 1 d . . . O30 O 0.90593(13) 0.34614(10) 0.29438(19) 0.0254(7) Uani 1 1 d . . . O31 O 0.84726(15) 0.44856(10) 0.2511(2) 0.0317(9) Uani 1 1 d . . . O32 O 0.73029(14) 0.40179(10) 0.13871(19) 0.0296(8) Uani 1 1 d . . . O33 O 0.78875(13) 0.29902(9) 0.18093(18) 0.0204(7) Uani 1 1 d . . . O34 O 0.83713(14) 0.39548(10) 0.36270(19) 0.0261(8) Uani 1 1 d . . . O35 O 0.75057(14) 0.42158(9) 0.28627(19) 0.0249(8) Uani 1 1 d . . . O36 O 0.72378(13) 0.34765(10) 0.25366(19) 0.0248(7) Uani 1 1 d . . . O37 O 0.80967(13) 0.32178(9) 0.32953(18) 0.0219(7) Uani 1 1 d . . . O38 O 0.81987(13) 0.37415(9) 0.21160(18) 0.0202(7) Uani 1 1 d . . . C5 C 0.9370(2) 0.40561(16) -0.0332(3) 0.0297(12) Uani 1 1 d . . . C6 C 0.9927(3) 0.3883(2) -0.0313(4) 0.0532(18) Uani 1 1 d . . . H6A H 1.0075 0.3899 0.0229 0.080 Uiso 1 1 calc R . . H6B H 1.0156 0.4034 -0.0673 0.080 Uiso 1 1 calc R . . H6C H 0.9912 0.3604 -0.0483 0.080 Uiso 1 1 calc R . . C7 C 0.9143(3) 0.4031(2) -0.1164(4) 0.0526(17) Uani 1 1 d . . . H7A H 0.8781 0.4144 -0.1178 0.079 Uiso 1 1 calc R . . H7B H 0.9128 0.3752 -0.1332 0.079 Uiso 1 1 calc R . . H7C H 0.9373 0.4181 -0.1524 0.079 Uiso 1 1 calc R . . C8 C 0.9367(3) 0.44787(16) -0.0023(4) 0.0442(15) Uani 1 1 d . . . H8A H 0.9519 0.4484 0.0517 0.066 Uiso 1 1 calc R . . H8B H 0.8998 0.4578 -0.0018 0.066 Uiso 1 1 calc R . . H8C H 0.9583 0.4647 -0.0369 0.066 Uiso 1 1 calc R . . N1 N 0.28047(17) 0.52589(12) 0.0784(2) 0.0317(10) Uani 1 1 d DU . . C9 C 0.3296(2) 0.50055(18) 0.0652(3) 0.0389(13) Uani 1 1 d DU . . H9A H 0.3211 0.4729 0.0805 0.047 Uiso 1 1 calc R . . H9B H 0.3585 0.5100 0.1016 0.047 Uiso 1 1 calc R . . C10 C 0.3512(3) 0.5001(2) -0.0186(4) 0.0541(17) Uani 1 1 d DU A . H10A H 0.3226 0.4920 -0.0567 0.065 Uiso 1 1 calc R . . H10B H 0.3637 0.5271 -0.0334 0.065 Uiso 1 1 calc R . . C11 C 0.3975(3) 0.4709(3) -0.0211(5) 0.083(3) Uani 1 1 d DU . . H11A H 0.3952 0.4518 0.0234 0.099 Uiso 0.300(13) 1 calc PR A 1 H11B H 0.3966 0.4559 -0.0717 0.099 Uiso 0.300(13) 1 calc PR A 1 H11C H 0.4227 0.4776 0.0230 0.099 Uiso 0.700(13) 1 calc PR A 2 H11D H 0.3831 0.4441 -0.0100 0.099 Uiso 0.700(13) 1 calc PR A 2 C12X C 0.4487(6) 0.4949(7) -0.0141(15) 0.072(8) Uani 0.300(13) 1 d PDU A 1 H12A H 0.4796 0.4768 -0.0129 0.108 Uiso 0.300(13) 1 calc PR A 1 H12B H 0.4484 0.5105 0.0350 0.108 Uiso 0.300(13) 1 calc PR A 1 H12C H 0.4514 0.5128 -0.0598 0.108 Uiso 0.300(13) 1 calc PR A 1 C12Y C 0.4281(5) 0.4686(4) -0.0933(6) 0.088(5) Uani 0.700(13) 1 d PDU A 2 H12D H 0.4574 0.4494 -0.0861 0.132 Uiso 0.700(13) 1 calc PR A 2 H12E H 0.4430 0.4948 -0.1056 0.132 Uiso 0.700(13) 1 calc PR A 2 H12F H 0.4045 0.4599 -0.1372 0.132 Uiso 0.700(13) 1 calc PR A 2 C13 C 0.2900(2) 0.56883(16) 0.0540(3) 0.0418(14) Uani 1 1 d DU . . H13A H 0.2968 0.5696 -0.0038 0.050 Uiso 1 1 calc R . . H13B H 0.2568 0.5842 0.0635 0.050 Uiso 1 1 calc R . . C14 C 0.3363(3) 0.58914(19) 0.0972(4) 0.063(2) Uani 1 1 d DU . . H14A H 0.3686 0.5721 0.0945 0.076 Uiso 1 1 calc R . . H14B H 0.3272 0.5926 0.1538 0.076 Uiso 1 1 calc R . . C15 C 0.3482(3) 0.6294(2) 0.0610(5) 0.082(3) Uani 1 1 d DU . . H15A H 0.3165 0.6468 0.0662 0.099 Uiso 1 1 calc R . . H15B H 0.3553 0.6260 0.0037 0.099 Uiso 1 1 calc R . . C16 C 0.3962(4) 0.6490(3) 0.1010(7) 0.126(5) Uani 1 1 d DU . . H16A H 0.4033 0.6746 0.0752 0.189 Uiso 1 1 calc R . . H16B H 0.4277 0.6318 0.0963 0.189 Uiso 1 1 calc R . . H16C H 0.3887 0.6535 0.1572 0.189 Uiso 1 1 calc R . . C17 C 0.2687(2) 0.52236(16) 0.1667(3) 0.0347(12) Uani 1 1 d DU . . H17A H 0.2663 0.4938 0.1805 0.042 Uiso 1 1 calc R . . H17B H 0.2993 0.5337 0.1973 0.042 Uiso 1 1 calc R . . C18 C 0.2176(2) 0.54279(17) 0.1927(3) 0.0397(14) Uani 1 1 d DU . . H18A H 0.1861 0.5271 0.1747 0.048 Uiso 1 1 calc R . . H18B H 0.2152 0.5695 0.1680 0.048 Uiso 1 1 calc R . . C19 C 0.2173(3) 0.54686(18) 0.2830(3) 0.0520(17) Uani 1 1 d DU . . H19A H 0.2253 0.5206 0.3072 0.062 Uiso 1 1 calc R . . H19B H 0.2461 0.5655 0.2998 0.062 Uiso 1 1 calc R . . C20 C 0.1646(3) 0.5617(2) 0.3139(4) 0.068(2) Uani 1 1 d DU . . H20A H 0.1669 0.5640 0.3719 0.102 Uiso 1 1 calc R . . H20B H 0.1361 0.5429 0.2992 0.102 Uiso 1 1 calc R . . H20C H 0.1566 0.5878 0.2908 0.102 Uiso 1 1 calc R . . C21 C 0.2338(2) 0.51091(15) 0.0277(3) 0.0331(12) Uani 1 1 d DU . . H21A H 0.2018 0.5272 0.0398 0.040 Uiso 1 1 calc R . . H21B H 0.2423 0.5154 -0.0288 0.040 Uiso 1 1 calc R . . C22 C 0.2193(2) 0.46757(15) 0.0381(3) 0.0362(13) Uani 1 1 d DU . . H22A H 0.2105 0.4625 0.0943 0.043 Uiso 1 1 calc R . . H22B H 0.2504 0.4508 0.0244 0.043 Uiso 1 1 calc R . . C23 C 0.1718(2) 0.45659(18) -0.0146(4) 0.0467(15) Uani 1 1 d DU . . H23A H 0.1800 0.4632 -0.0704 0.056 Uiso 1 1 calc R . . H23B H 0.1403 0.4726 0.0011 0.056 Uiso 1 1 calc R . . C24 C 0.1579(3) 0.41284(19) -0.0091(5) 0.063(2) Uani 1 1 d DU . . H24A H 0.1268 0.4071 -0.0436 0.094 Uiso 1 1 calc R . . H24B H 0.1494 0.4062 0.0459 0.094 Uiso 1 1 calc R . . H24C H 0.1886 0.3969 -0.0261 0.094 Uiso 1 1 calc R . . N2 N 0.81763(16) 0.20688(11) 0.0498(2) 0.0259(9) Uani 1 1 d DU . . C25 C 0.8545(2) 0.24220(14) 0.0372(3) 0.0274(11) Uani 1 1 d DU . . H25A H 0.8363 0.2665 0.0561 0.033 Uiso 1 1 calc R . . H25B H 0.8874 0.2385 0.0702 0.033 Uiso 1 1 calc R . . C26 C 0.8708(2) 0.24851(18) -0.0482(3) 0.0430(15) Uani 1 1 d DU . . H26A H 0.8385 0.2549 -0.0809 0.052 Uiso 1 1 calc R . . H26B H 0.8864 0.2236 -0.0691 0.052 Uiso 1 1 calc R . . C27 C 0.9112(2) 0.28181(16) -0.0555(3) 0.0373(13) Uani 1 1 d DU . . H27A H 0.9172 0.2871 -0.1125 0.045 Uiso 1 1 calc R . . H27B H 0.8961 0.3063 -0.0318 0.045 Uiso 1 1 calc R . . C28 C 0.9639(3) 0.2730(3) -0.0161(5) 0.083(3) Uani 1 1 d DU . . H28A H 0.9881 0.2957 -0.0230 0.125 Uiso 1 1 calc R . . H28B H 0.9796 0.2493 -0.0400 0.125 Uiso 1 1 calc R . . H28C H 0.9585 0.2684 0.0407 0.125 Uiso 1 1 calc R . . C29 C 0.8432(2) 0.16822(14) 0.0229(3) 0.0290(11) Uani 1 1 d DU . . H29A H 0.8167 0.1465 0.0282 0.035 Uiso 1 1 calc R . . H29B H 0.8518 0.1706 -0.0342 0.035 Uiso 1 1 calc R . . C30 C 0.8938(2) 0.15658(16) 0.0680(3) 0.0358(13) Uani 1 1 d DU . . H30A H 0.8850 0.1505 0.1238 0.043 Uiso 1 1 calc R . . H30B H 0.9195 0.1791 0.0679 0.043 Uiso 1 1 calc R . . C31 C 0.9195(3) 0.12027(18) 0.0298(4) 0.0487(16) Uani 1 1 d DU . . H31A H 0.8918 0.0995 0.0212 0.058 Uiso 1 1 calc R . . H31B H 0.9337 0.1278 -0.0226 0.058 Uiso 1 1 calc R . . C32 C 0.9644(3) 0.1035(2) 0.0809(4) 0.069(2) Uani 1 1 d DU . . H32A H 0.9795 0.0801 0.0549 0.103 Uiso 1 1 calc R . . H32B H 0.9504 0.0959 0.1328 0.103 Uiso 1 1 calc R . . H32C H 0.9924 0.1237 0.0882 0.103 Uiso 1 1 calc R . . C33 C 0.8056(2) 0.20533(15) 0.1381(3) 0.0326(12) Uani 1 1 d DU . . H33A H 0.8400 0.2028 0.1679 0.039 Uiso 1 1 calc R . . H33B H 0.7891 0.2309 0.1535 0.039 Uiso 1 1 calc R . . C34 C 0.7689(3) 0.17181(19) 0.1634(3) 0.0498(16) Uani 1 1 d DU . . H34A H 0.7360 0.1723 0.1297 0.060 Uiso 1 1 calc R . . H34B H 0.7872 0.1461 0.1544 0.060 Uiso 1 1 calc R . . C35 C 0.7533(3) 0.1744(2) 0.2491(4) 0.071(2) Uani 1 1 d DU . . H35A H 0.7351 0.2002 0.2581 0.085 Uiso 1 1 calc R . . H35B H 0.7273 0.1530 0.2605 0.085 Uiso 1 1 calc R . . C36 C 0.7998(4) 0.1709(3) 0.3057(5) 0.091(3) Uani 1 1 d DU . . H36A H 0.7871 0.1731 0.3603 0.137 Uiso 1 1 calc R . . H36B H 0.8255 0.1923 0.2955 0.137 Uiso 1 1 calc R . . H36C H 0.8174 0.1451 0.2984 0.137 Uiso 1 1 calc R . . C37 C 0.76648(19) 0.21154(14) 0.0005(3) 0.0278(11) Uani 1 1 d DU . . H37A H 0.7429 0.1885 0.0108 0.033 Uiso 1 1 calc R . . H37B H 0.7758 0.2109 -0.0564 0.033 Uiso 1 1 calc R . . C38 C 0.7351(2) 0.24942(16) 0.0162(3) 0.0381(13) Uani 1 1 d DU . . H38A H 0.7289 0.2521 0.0740 0.046 Uiso 1 1 calc R . . H38B H 0.7562 0.2727 -0.0011 0.046 Uiso 1 1 calc R . . C39 C 0.6815(2) 0.24877(18) -0.0279(3) 0.0401(14) Uani 1 1 d DU . . H39A H 0.6605 0.2256 -0.0092 0.048 Uiso 1 1 calc R . . H39B H 0.6613 0.2731 -0.0141 0.048 Uiso 1 1 calc R . . C40 C 0.6854(3) 0.2465(2) -0.1158(4) 0.063(2) Uani 1 1 d DU . . H40A H 0.6493 0.2459 -0.1396 0.094 Uiso 1 1 calc R . . H40B H 0.7048 0.2223 -0.1304 0.094 Uiso 1 1 calc R . . H40C H 0.7047 0.2698 -0.1353 0.094 Uiso 1 1 calc R . . N3 N 0.34834(15) 0.26442(11) 0.5961(2) 0.0248(9) Uani 1 1 d DU . . C41 C 0.3292(2) 0.22504(14) 0.5611(3) 0.0295(11) Uani 1 1 d DU . . H41A H 0.3601 0.2066 0.5592 0.035 Uiso 1 1 calc R . . H41B H 0.3025 0.2133 0.5972 0.035 Uiso 1 1 calc R . . C42 C 0.3044(2) 0.22804(15) 0.4788(3) 0.0348(13) Uani 1 1 d DU . . H42A H 0.2702 0.2430 0.4818 0.042 Uiso 1 1 calc R . . H42B H 0.3288 0.2432 0.4442 0.042 Uiso 1 1 calc R . . C43 C 0.2937(4) 0.18851(18) 0.4422(4) 0.067(2) Uani 1 1 d DU . . H43A H 0.2668 0.1743 0.4741 0.080 Uiso 1 1 calc R . . H43B H 0.3272 0.1727 0.4435 0.080 Uiso 1 1 calc R . . C44 C 0.2734(3) 0.1916(2) 0.3572(4) 0.067(2) Uani 1 1 d DU . . H44A H 0.2668 0.1649 0.3359 0.100 Uiso 1 1 calc R . . H44B H 0.3003 0.2051 0.3250 0.100 Uiso 1 1 calc R . . H44C H 0.2399 0.2069 0.3556 0.100 Uiso 1 1 calc R . . C45 C 0.30221(19) 0.29347(14) 0.6002(3) 0.0260(10) Uani 1 1 d DU . . H45A H 0.2907 0.3001 0.5452 0.031 Uiso 1 1 calc R . . H45B H 0.3156 0.3183 0.6252 0.031 Uiso 1 1 calc R . . C46 C 0.2535(2) 0.27984(15) 0.6451(3) 0.0321(12) Uani 1 1 d DU . . H46A H 0.2370 0.2566 0.6181 0.038 Uiso 1 1 calc R . . H46B H 0.2642 0.2718 0.6997 0.038 Uiso 1 1 calc R . . C47 C 0.2135(2) 0.31359(17) 0.6483(4) 0.0506(17) Uani 1 1 d DU . . H47A H 0.2309 0.3368 0.6740 0.061 Uiso 1 1 calc R . . H47B H 0.2034 0.3213 0.5934 0.061 Uiso 1 1 calc R . . C48 C 0.1635(3) 0.3037(2) 0.6926(4) 0.0581(19) Uani 1 1 d DU . . H48A H 0.1393 0.3267 0.6918 0.087 Uiso 1 1 calc R . . H48B H 0.1729 0.2969 0.7477 0.087 Uiso 1 1 calc R . . H48C H 0.1455 0.2810 0.6671 0.087 Uiso 1 1 calc R . . C49 C 0.3723(2) 0.25607(15) 0.6779(3) 0.0292(11) Uani 1 1 d DU . . H49A H 0.3440 0.2449 0.7119 0.035 Uiso 1 1 calc R . . H49B H 0.4007 0.2356 0.6728 0.035 Uiso 1 1 calc R . . C50 C 0.3962(3) 0.29219(17) 0.7187(3) 0.0411(14) Uani 1 1 d DU . . H50A H 0.3677 0.3124 0.7262 0.049 Uiso 1 1 calc R . . H50B H 0.4239 0.3040 0.6846 0.049 Uiso 1 1 calc R . . C51 C 0.4211(2) 0.28146(17) 0.7992(3) 0.0406(14) Uani 1 1 d DU . . H51A H 0.3937 0.2689 0.8329 0.049 Uiso 1 1 calc R . . H51B H 0.4505 0.2621 0.7917 0.049 Uiso 1 1 calc R . . C52 C 0.4430(3) 0.3184(2) 0.8402(4) 0.064(2) Uani 1 1 d DU . . H52A H 0.4593 0.3110 0.8915 0.096 Uiso 1 1 calc R . . H52B H 0.4136 0.3373 0.8489 0.096 Uiso 1 1 calc R . . H52C H 0.4701 0.3308 0.8068 0.096 Uiso 1 1 calc R . . C53 C 0.3895(2) 0.28371(15) 0.5427(3) 0.0307(12) Uani 1 1 d DU . . H53A H 0.3721 0.2894 0.4906 0.037 Uiso 1 1 calc R . . H53B H 0.4003 0.3095 0.5664 0.037 Uiso 1 1 calc R . . C54 C 0.4397(2) 0.25944(17) 0.5286(3) 0.0384(13) Uani 1 1 d DU . . H54A H 0.4559 0.2516 0.5804 0.046 Uiso 1 1 calc R . . H54B H 0.4300 0.2349 0.4992 0.046 Uiso 1 1 calc R . . C55 C 0.4799(2) 0.28277(19) 0.4820(4) 0.0463(15) Uani 1 1 d DU . . H55A H 0.4884 0.3077 0.5110 0.056 Uiso 1 1 calc R . . H55B H 0.4635 0.2902 0.4301 0.056 Uiso 1 1 calc R . . C56 C 0.5311(2) 0.2604(2) 0.4679(4) 0.0537(18) Uani 1 1 d DU . . H56A H 0.5556 0.2771 0.4375 0.081 Uiso 1 1 calc R . . H56B H 0.5231 0.2361 0.4378 0.081 Uiso 1 1 calc R . . H56C H 0.5479 0.2534 0.5190 0.081 Uiso 1 1 calc R . . N4 N 0.06192(15) 0.32277(12) 0.2310(2) 0.0273(9) Uani 1 1 d DU . . C57 C 0.0835(2) 0.32370(18) 0.3160(3) 0.0385(13) Uani 1 1 d DU B . H57A H 0.0996 0.2975 0.3284 0.046 Uiso 1 1 calc R . . H57B H 0.1126 0.3437 0.3194 0.046 Uiso 1 1 calc R . . C58 C 0.0426(3) 0.3332(2) 0.3792(3) 0.063(2) Uani 1 1 d DU . . H58A H 0.0188 0.3101 0.3885 0.075 Uiso 0.392(14) 1 calc PR B 1 H58B H 0.0202 0.3563 0.3631 0.075 Uiso 0.392(14) 1 calc PR B 1 H58C H 0.0082 0.3201 0.3648 0.075 Uiso 0.608(14) 1 calc PR B 2 H58D H 0.0362 0.3623 0.3797 0.075 Uiso 0.608(14) 1 calc PR B 2 C59X C 0.0763(8) 0.3430(6) 0.4550(8) 0.063(5) Uani 0.392(14) 1 d PDU B 1 H59A H 0.1050 0.3622 0.4420 0.076 Uiso 0.392(14) 1 calc PR B 1 H59B H 0.0531 0.3552 0.4955 0.076 Uiso 0.392(14) 1 calc PR B 1 C60X C 0.1004(11) 0.3054(7) 0.4867(13) 0.099(9) Uani 0.392(14) 1 d PDU B 1 H60A H 0.0807 0.2969 0.5337 0.148 Uiso 0.392(14) 1 calc PR B 1 H60B H 0.1381 0.3101 0.5013 0.148 Uiso 0.392(14) 1 calc PR B 1 H60C H 0.0981 0.2847 0.4459 0.148 Uiso 0.392(14) 1 calc PR B 1 C59Y C 0.0598(5) 0.3199(3) 0.4633(5) 0.053(3) Uani 0.608(14) 1 d PDU B 2 H59C H 0.0295 0.3225 0.5002 0.063 Uiso 0.608(14) 1 calc PR B 2 H59D H 0.0716 0.2918 0.4627 0.063 Uiso 0.608(14) 1 calc PR B 2 C60Y C 0.1049(5) 0.3463(4) 0.4886(8) 0.074(5) Uani 0.608(14) 1 d PDU B 2 H60D H 0.1169 0.3390 0.5423 0.110 Uiso 0.608(14) 1 calc PR B 2 H60E H 0.0927 0.3740 0.4883 0.110 Uiso 0.608(14) 1 calc PR B 2 H60F H 0.1347 0.3432 0.4518 0.110 Uiso 0.608(14) 1 calc PR B 2 C61 C 0.0179(2) 0.29152(14) 0.2219(3) 0.0301(11) Uani 1 1 d DU . . H61A H -0.0135 0.3002 0.2526 0.036 Uiso 1 1 calc R . . H61B H 0.0067 0.2903 0.1653 0.036 Uiso 1 1 calc R . . C62 C 0.0335(2) 0.25008(16) 0.2489(4) 0.0457(15) Uani 1 1 d DU . . H62A H 0.0692 0.2434 0.2276 0.055 Uiso 1 1 calc R . . H62B H 0.0363 0.2496 0.3076 0.055 Uiso 1 1 calc R . . C63 C -0.0065(2) 0.21914(16) 0.2217(4) 0.0430(14) Uani 1 1 d DU . . H63A H -0.0427 0.2273 0.2389 0.052 Uiso 1 1 calc R . . H63B H -0.0071 0.2182 0.1629 0.052 Uiso 1 1 calc R . . C64 C 0.0052(3) 0.17813(18) 0.2531(4) 0.0572(18) Uani 1 1 d DU . . H64A H -0.0221 0.1595 0.2330 0.086 Uiso 1 1 calc R . . H64B H 0.0046 0.1785 0.3113 0.086 Uiso 1 1 calc R . . H64C H 0.0406 0.1696 0.2355 0.086 Uiso 1 1 calc R . . C65 C 0.1092(2) 0.31363(16) 0.1783(3) 0.0321(12) Uani 1 1 d DU . . H65A H 0.1371 0.3342 0.1875 0.039 Uiso 1 1 calc R . . H65B H 0.1247 0.2877 0.1948 0.039 Uiso 1 1 calc R . . C66 C 0.0963(2) 0.3119(2) 0.0903(3) 0.0451(15) Uani 1 1 d DU . . H66A H 0.0676 0.2921 0.0805 0.054 Uiso 1 1 calc R . . H66B H 0.0828 0.3382 0.0724 0.054 Uiso 1 1 calc R . . C67 C 0.1449(3) 0.3009(2) 0.0423(4) 0.0552(18) Uani 1 1 d DU . . H67A H 0.1739 0.3204 0.0529 0.066 Uiso 1 1 calc R . . H67B H 0.1580 0.2744 0.0596 0.066 Uiso 1 1 calc R . . C68 C 0.1325(3) 0.2999(3) -0.0458(4) 0.076(2) Uani 1 1 d DU . . H68A H 0.1650 0.2929 -0.0747 0.114 Uiso 1 1 calc R . . H68B H 0.1197 0.3261 -0.0632 0.114 Uiso 1 1 calc R . . H68C H 0.1046 0.2799 -0.0568 0.114 Uiso 1 1 calc R . . C69 C 0.0368(2) 0.36248(14) 0.2087(3) 0.0317(12) Uani 1 1 d DU . . H69A H 0.0210 0.3602 0.1545 0.038 Uiso 1 1 calc R . . H69B H 0.0071 0.3678 0.2454 0.038 Uiso 1 1 calc R . . C70 C 0.0742(2) 0.39770(16) 0.2102(4) 0.0417(14) Uani 1 1 d DU . . H70A H 0.0887 0.4013 0.2649 0.050 Uiso 1 1 calc R . . H70B H 0.1048 0.3923 0.1750 0.050 Uiso 1 1 calc R . . C71 C 0.0471(2) 0.43534(16) 0.1841(4) 0.0478(16) Uani 1 1 d DU . . H71A H 0.0178 0.4413 0.2214 0.057 Uiso 1 1 calc R . . H71B H 0.0304 0.4309 0.1310 0.057 Uiso 1 1 calc R . . C72 C 0.0831(3) 0.47101(18) 0.1797(4) 0.0528(17) Uani 1 1 d DU . . H72A H 0.0622 0.4942 0.1624 0.079 Uiso 1 1 calc R . . H72B H 0.1116 0.4659 0.1415 0.079 Uiso 1 1 calc R . . H72C H 0.0992 0.4762 0.2322 0.079 Uiso 1 1 calc R . . N5 N 0.83227(19) 0.53826(13) 0.3875(3) 0.0457(12) Uani 1 1 d DU C . C73 C 0.7954(3) 0.57170(19) 0.3625(4) 0.0566(16) Uani 1 1 d DU . . H73A H 0.7766 0.5795 0.4114 0.068 Uiso 0.408(15) 1 calc PR C 1 H73B H 0.8194 0.5942 0.3497 0.068 Uiso 0.408(15) 1 calc PR C 1 H73C H 0.8160 0.5966 0.3553 0.068 Uiso 0.592(15) 1 calc PR C 2 H73D H 0.7679 0.5763 0.4032 0.068 Uiso 0.592(15) 1 calc PR C 2 C74X C 0.7533(5) 0.5717(5) 0.2984(7) 0.045(4) Uani 0.408(15) 1 d PDU C 1 H74A H 0.7230 0.5883 0.3163 0.054 Uiso 0.408(15) 1 calc PR C 1 H74B H 0.7398 0.5442 0.2922 0.054 Uiso 0.408(15) 1 calc PR C 1 C75X C 0.7700(7) 0.5864(5) 0.2175(8) 0.053(4) Uani 0.408(15) 1 d PDU C 1 H75A H 0.7819 0.6145 0.2218 0.063 Uiso 0.408(15) 1 calc PR C 1 H75B H 0.8006 0.5704 0.1987 0.063 Uiso 0.408(15) 1 calc PR C 1 C76X C 0.7242(9) 0.5835(8) 0.1580(12) 0.057(6) Uani 0.408(15) 1 d PDU C 1 H76A H 0.7355 0.5944 0.1069 0.085 Uiso 0.408(15) 1 calc PR C 1 H76B H 0.6935 0.5988 0.1772 0.085 Uiso 0.408(15) 1 calc PR C 1 H76C H 0.7139 0.5556 0.1513 0.085 Uiso 0.408(15) 1 calc PR C 1 C74Y C 0.7686(5) 0.5585(4) 0.2822(7) 0.059(3) Uani 0.592(15) 1 d PDU C 2 H74C H 0.7964 0.5520 0.2429 0.071 Uiso 0.592(15) 1 calc PR C 2 H74D H 0.7462 0.5345 0.2904 0.071 Uiso 0.592(15) 1 calc PR C 2 C75Y C 0.7342(6) 0.5925(3) 0.2527(8) 0.073(4) Uani 0.592(15) 1 d PDU C 2 H75C H 0.7087 0.5999 0.2946 0.088 Uiso 0.592(15) 1 calc PR C 2 H75D H 0.7575 0.6158 0.2430 0.088 Uiso 0.592(15) 1 calc PR C 2 C76Y C 0.7031(8) 0.5830(7) 0.1775(10) 0.090(8) Uani 0.592(15) 1 d PDU C 2 H76D H 0.6830 0.6066 0.1602 0.134 Uiso 0.592(15) 1 calc PR C 2 H76E H 0.6782 0.5612 0.1875 0.134 Uiso 0.592(15) 1 calc PR C 2 H76F H 0.7281 0.5752 0.1359 0.134 Uiso 0.592(15) 1 calc PR C 2 C77 C 0.8721(3) 0.52867(19) 0.3219(4) 0.063(2) Uani 1 1 d DU . . H77A H 0.8955 0.5067 0.3407 0.075 Uiso 1 1 calc R C . H77B H 0.8516 0.5188 0.2750 0.075 Uiso 1 1 calc R . . C78 C 0.9075(3) 0.56251(19) 0.2956(4) 0.059(2) Uani 1 1 d DU C . H78A H 0.9231 0.5761 0.3428 0.071 Uiso 0.641(17) 1 calc PR D 1 H78B H 0.8856 0.5821 0.2654 0.071 Uiso 0.641(17) 1 calc PR D 1 H78C H 0.8887 0.5878 0.3065 0.071 Uiso 0.359(17) 1 calc PR D 2 H78D H 0.9407 0.5622 0.3287 0.071 Uiso 0.359(17) 1 calc PR D 2 C79X C 0.9532(4) 0.5468(4) 0.2426(6) 0.055(4) Uani 0.641(17) 1 d PDU C 1 H79A H 0.9741 0.5700 0.2242 0.066 Uiso 0.641(17) 1 calc PR D 1 H79B H 0.9775 0.5304 0.2762 0.066 Uiso 0.641(17) 1 calc PR D 1 C79Y C 0.9232(10) 0.5624(4) 0.2097(9) 0.049(5) Uani 0.359(17) 1 d PDU C 2 H79C H 0.8928 0.5734 0.1780 0.058 Uiso 0.359(17) 1 calc PR D 2 H79D H 0.9539 0.5808 0.2038 0.058 Uiso 0.359(17) 1 calc PR D 2 C80 C 0.9380(3) 0.5239(2) 0.1748(4) 0.067(2) Uani 1 1 d DU . . H80A H 0.9702 0.5157 0.1466 0.101 Uiso 0.641(17) 1 calc PR D 1 H80B H 0.9152 0.5400 0.1394 0.101 Uiso 0.641(17) 1 calc PR D 1 H80C H 0.9181 0.5004 0.1918 0.101 Uiso 0.641(17) 1 calc PR D 1 H80D H 0.9462 0.5276 0.1186 0.101 Uiso 0.359(17) 1 calc PR D 2 H80E H 0.9080 0.5053 0.1797 0.101 Uiso 0.359(17) 1 calc PR D 2 H80F H 0.9696 0.5133 0.2030 0.101 Uiso 0.359(17) 1 calc PR D 2 C81 C 0.8616(2) 0.55158(17) 0.4626(3) 0.0447(14) Uani 1 1 d DU . . H81A H 0.8852 0.5742 0.4490 0.054 Uiso 1 1 calc R C . H81B H 0.8348 0.5616 0.5004 0.054 Uiso 1 1 calc R . . C82 C 0.8954(2) 0.52032(18) 0.5045(4) 0.0519(16) Uani 1 1 d DU C . H82A H 0.9143 0.5042 0.4645 0.062 Uiso 1 1 calc R . . H82B H 0.8717 0.5023 0.5346 0.062 Uiso 1 1 calc R . . C83 C 0.9364(2) 0.53892(19) 0.5613(4) 0.0538(17) Uani 1 1 d DU . . H83A H 0.9615 0.5555 0.5305 0.065 Uiso 1 1 calc R C . H83B H 0.9176 0.5566 0.5988 0.065 Uiso 1 1 calc R . . C84 C 0.9681(3) 0.5085(2) 0.6079(5) 0.069(2) Uani 1 1 d DU C . H84A H 0.9938 0.5221 0.6431 0.104 Uiso 1 1 calc R . . H84B H 0.9874 0.4913 0.5712 0.104 Uiso 1 1 calc R . . H84C H 0.9436 0.4925 0.6396 0.104 Uiso 1 1 calc R . . C85 C 0.8008(3) 0.50023(17) 0.4025(4) 0.0479(17) Uani 1 1 d DU . . H85A H 0.7848 0.4911 0.3514 0.057 Uiso 1 1 calc R C . H85B H 0.8260 0.4794 0.4212 0.057 Uiso 1 1 calc R . . C86 C 0.7566(3) 0.50432(17) 0.4623(4) 0.0491(17) Uani 1 1 d DU C . H86A H 0.7290 0.5231 0.4419 0.059 Uiso 1 1 calc R . . H86B H 0.7716 0.5152 0.5126 0.059 Uiso 1 1 calc R . . C87 C 0.7308(3) 0.46407(18) 0.4780(4) 0.058(2) Uani 1 1 d DU . . H87A H 0.7200 0.4518 0.4267 0.070 Uiso 1 1 calc R C . H87B H 0.7575 0.4464 0.5041 0.070 Uiso 1 1 calc R . . C88 C 0.6829(3) 0.4677(2) 0.5293(5) 0.075(3) Uani 1 1 d DU C . H88A H 0.6685 0.4412 0.5401 0.113 Uiso 1 1 calc R . . H88B H 0.6555 0.4838 0.5020 0.113 Uiso 1 1 calc R . . H88C H 0.6933 0.4806 0.5795 0.113 Uiso 1 1 calc R . . N6 N 0.57350(15) 0.37488(13) 0.2627(3) 0.0338(10) Uani 1 1 d DU . . C89 C 0.5223(2) 0.38404(19) 0.2171(3) 0.0427(14) Uani 1 1 d DU . . H89A H 0.5040 0.4063 0.2440 0.051 Uiso 1 1 calc R . . H89B H 0.4985 0.3605 0.2200 0.051 Uiso 1 1 calc R . . C90 C 0.5288(2) 0.3950(2) 0.1305(4) 0.0600(18) Uani 1 1 d DU . . H90A H 0.5540 0.3762 0.1055 0.072 Uiso 1 1 calc R . . H90B H 0.5442 0.4220 0.1267 0.072 Uiso 1 1 calc R . . C91 C 0.4752(3) 0.3937(2) 0.0862(4) 0.0614(19) Uani 1 1 d DU . . H91A H 0.4479 0.4073 0.1186 0.074 Uiso 1 1 calc R . . H91B H 0.4784 0.4087 0.0359 0.074 Uiso 1 1 calc R . . C92 C 0.4560(3) 0.3528(2) 0.0677(4) 0.069(2) Uani 1 1 d DU . . H92A H 0.4211 0.3541 0.0402 0.104 Uiso 1 1 calc R . . H92B H 0.4524 0.3377 0.1171 0.104 Uiso 1 1 calc R . . H92C H 0.4819 0.3395 0.0334 0.104 Uiso 1 1 calc R . . C93 C 0.6147(2) 0.40868(16) 0.2542(4) 0.0376(13) Uani 1 1 d DU . . H93A H 0.6490 0.4002 0.2791 0.045 Uiso 1 1 calc R . . H93B H 0.6212 0.4131 0.1970 0.045 Uiso 1 1 calc R . . C94 C 0.5978(2) 0.44787(16) 0.2912(4) 0.0463(15) Uani 1 1 d DU . . H94A H 0.5621 0.4555 0.2697 0.056 Uiso 1 1 calc R . . H94B H 0.5947 0.4443 0.3494 0.056 Uiso 1 1 calc R . . C95 C 0.6370(2) 0.48071(17) 0.2751(5) 0.0551(18) Uani 1 1 d DU . . H95A H 0.6388 0.4853 0.2171 0.066 Uiso 1 1 calc R . . H95B H 0.6732 0.4726 0.2943 0.066 Uiso 1 1 calc R . . C96 C 0.6209(3) 0.51899(19) 0.3161(5) 0.066(2) Uani 1 1 d DU . . H96A H 0.6470 0.5399 0.3043 0.099 Uiso 1 1 calc R . . H96B H 0.6199 0.5146 0.3736 0.099 Uiso 1 1 calc R . . H96C H 0.5853 0.5272 0.2968 0.099 Uiso 1 1 calc R . . C97 C 0.5581(2) 0.36958(17) 0.3488(3) 0.0392(13) Uani 1 1 d DU . . H97A H 0.5392 0.3939 0.3661 0.047 Uiso 1 1 calc R . . H97B H 0.5324 0.3472 0.3518 0.047 Uiso 1 1 calc R . . C98 C 0.6035(2) 0.36167(18) 0.4066(3) 0.0432(14) Uani 1 1 d DU . . H98A H 0.6344 0.3789 0.3936 0.052 Uiso 1 1 calc R . . H98B H 0.6150 0.3336 0.4018 0.052 Uiso 1 1 calc R . . C99 C 0.5865(2) 0.36976(19) 0.4912(3) 0.0484(15) Uani 1 1 d DU . . H99A H 0.5785 0.3985 0.4967 0.058 Uiso 1 1 calc R . . H99B H 0.5530 0.3549 0.5015 0.058 Uiso 1 1 calc R . . C100 C 0.6279(3) 0.3584(2) 0.5529(4) 0.0573(18) Uani 1 1 d DU . . H10C H 0.6144 0.3646 0.6059 0.086 Uiso 1 1 calc R . . H10D H 0.6610 0.3733 0.5439 0.086 Uiso 1 1 calc R . . H10E H 0.6352 0.3298 0.5493 0.086 Uiso 1 1 calc R . . C101 C 0.6008(2) 0.33747(15) 0.2314(3) 0.0348(12) Uani 1 1 d DU . . H10F H 0.6105 0.3422 0.1754 0.042 Uiso 1 1 calc R . . H10G H 0.6346 0.3334 0.2620 0.042 Uiso 1 1 calc R . . C102 C 0.5681(2) 0.29933(15) 0.2352(4) 0.0398(14) Uani 1 1 d DU . . H10H H 0.5615 0.2924 0.2914 0.048 Uiso 1 1 calc R . . H10I H 0.5329 0.3033 0.2082 0.048 Uiso 1 1 calc R . . C103 C 0.5980(2) 0.26566(17) 0.1955(3) 0.0407(14) Uani 1 1 d DU . . H10J H 0.6012 0.2716 0.1381 0.049 Uiso 1 1 calc R . . H10K H 0.6347 0.2639 0.2186 0.049 Uiso 1 1 calc R . . C104 C 0.5703(3) 0.22611(18) 0.2050(4) 0.0585(19) Uani 1 1 d DU . . H10L H 0.5908 0.2054 0.1780 0.088 Uiso 1 1 calc R . . H10M H 0.5341 0.2276 0.1817 0.088 Uiso 1 1 calc R . . H10N H 0.5680 0.2197 0.2617 0.088 Uiso 1 1 calc R . . N7 N 0.4780(4) 0.3714(3) 0.6490(5) 0.105(3) Uani 1 1 d U . . C105 C 0.4645(3) 0.3899(2) 0.5966(5) 0.0569(18) Uani 1 1 d U . . C106 C 0.4486(3) 0.4137(2) 0.5283(5) 0.063(2) Uani 1 1 d U . . 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 0.0330(3) 0.0212(2) 0.0176(2) -0.00086(17) -0.00042(17) -0.00009(18) Mo2 0.0184(2) 0.0202(2) 0.0267(2) -0.00372(18) 0.00217(17) 0.00302(16) Mo3 0.0433(3) 0.0262(2) 0.0164(2) -0.00107(18) 0.00271(18) 0.0096(2) Mo4 0.0196(2) 0.0197(2) 0.0327(2) 0.00251(18) 0.00568(17) 0.00521(17) Mo5 0.0228(2) 0.01787(19) 0.0297(2) -0.00287(18) 0.00120(17) -0.00233(17) Ti1 0.0182(5) 0.0180(4) 0.0355(5) 0.0031(4) 0.0037(4) -0.0008(3) O1 0.022(2) 0.0255(19) 0.061(3) 0.0077(18) 0.0035(18) -0.0053(15) O2 0.065(3) 0.034(2) 0.0197(18) -0.0015(16) -0.0060(18) 0.001(2) O3 0.024(2) 0.033(2) 0.046(2) -0.0085(18) 0.0027(17) 0.0090(16) O4 0.089(4) 0.051(3) 0.0181(19) -0.0037(19) 0.004(2) 0.025(2) O5 0.031(2) 0.0270(19) 0.055(2) 0.0049(18) 0.0102(18) 0.0114(16) O6 0.030(2) 0.028(2) 0.057(3) -0.0004(19) -0.0004(18) -0.0076(16) O7 0.028(2) 0.0202(17) 0.035(2) -0.0037(15) -0.0075(15) -0.0029(14) O8 0.0225(18) 0.0175(16) 0.0287(18) -0.0017(14) 0.0030(14) 0.0039(14) O9 0.042(2) 0.0278(19) 0.0256(18) 0.0086(16) 0.0133(16) 0.0039(16) O10 0.0209(19) 0.0225(18) 0.054(2) 0.0054(17) 0.0092(17) 0.0018(15) O11 0.031(2) 0.0211(17) 0.0308(19) 0.0058(15) -0.0061(15) 0.0006(15) O12 0.033(2) 0.0232(17) 0.0215(17) -0.0029(14) 0.0065(15) 0.0016(15) O13 0.041(2) 0.0246(18) 0.0253(18) -0.0002(15) -0.0059(16) 0.0072(16) O14 0.042(2) 0.0278(19) 0.0296(19) 0.0002(16) 0.0149(16) 0.0104(17) O15 0.037(2) 0.0209(17) 0.0210(17) 0.0037(14) 0.0055(15) -0.0013(15) O16 0.0176(18) 0.0274(19) 0.044(2) -0.0026(17) 0.0057(15) -0.0025(14) O17 0.042(2) 0.0277(19) 0.0276(19) -0.0080(16) -0.0063(16) 0.0023(16) O18 0.0217(18) 0.0181(16) 0.0321(19) -0.0035(15) 0.0034(14) 0.0043(14) O19 0.0158(16) 0.0157(15) 0.0200(15) -0.0001(13) 0.0009(12) -0.0020(12) C1 0.026(3) 0.036(3) 0.042(3) 0.005(3) -0.003(2) -0.008(2) C2 0.070(5) 0.037(4) 0.075(5) 0.001(4) 0.004(4) -0.016(3) C3 0.032(4) 0.089(6) 0.052(4) 0.009(4) 0.003(3) -0.009(4) C4 0.043(4) 0.076(5) 0.052(4) 0.015(4) 0.000(3) -0.008(4) Mo6 0.0235(2) 0.0279(2) 0.0369(3) -0.0102(2) 0.01130(19) -0.00810(19) Mo7 0.0477(3) 0.0164(2) 0.0255(2) 0.00493(18) 0.0170(2) 0.01008(19) Mo8 0.0214(2) 0.0266(2) 0.0229(2) -0.00110(18) 0.00164(17) 0.00631(18) Mo9 0.0191(2) 0.01759(19) 0.0237(2) -0.00010(17) 0.00390(16) 0.00571(16) Mo10 0.0202(2) 0.01694(19) 0.0203(2) 0.00233(16) 0.00777(16) 0.00322(16) Ti2 0.0336(5) 0.0197(4) 0.0286(5) -0.0010(4) 0.0187(4) 0.0011(4) O20 0.054(3) 0.029(2) 0.036(2) -0.0012(17) 0.0323(19) -0.0019(18) O21 0.041(3) 0.050(3) 0.053(3) -0.018(2) 0.010(2) -0.021(2) O22 0.079(3) 0.0206(19) 0.036(2) 0.0107(17) 0.026(2) 0.0222(19) O23 0.026(2) 0.041(2) 0.033(2) -0.0072(17) -0.0063(15) 0.0069(17) O24 0.030(2) 0.0230(18) 0.035(2) 0.0014(16) 0.0026(16) 0.0101(15) O25 0.030(2) 0.0232(17) 0.0232(17) 0.0035(14) 0.0107(14) 0.0048(15) O26 0.028(2) 0.0298(19) 0.042(2) -0.0025(17) 0.0205(17) -0.0033(16) O27 0.053(3) 0.0245(19) 0.0267(19) 0.0097(16) 0.0194(17) 0.0073(17) O28 0.033(2) 0.0285(19) 0.0206(17) -0.0040(15) 0.0082(14) 0.0037(15) O29 0.0285(19) 0.0191(17) 0.0298(18) -0.0038(15) 0.0121(15) 0.0031(14) O30 0.0187(18) 0.0267(18) 0.0309(18) -0.0015(15) 0.0022(14) 0.0012(14) O31 0.041(2) 0.0183(17) 0.036(2) -0.0021(15) 0.0174(17) -0.0064(15) O32 0.033(2) 0.0302(19) 0.0255(18) 0.0045(16) 0.0044(15) 0.0137(16) O33 0.0200(17) 0.0171(15) 0.0243(17) -0.0016(14) 0.0019(13) 0.0000(13) O34 0.030(2) 0.0263(18) 0.0226(17) -0.0062(15) 0.0064(14) -0.0052(15) O35 0.034(2) 0.0176(16) 0.0237(17) 0.0033(14) 0.0135(15) 0.0094(14) O36 0.0191(18) 0.0269(18) 0.0284(18) -0.0026(15) 0.0062(14) 0.0030(14) O37 0.0257(18) 0.0200(16) 0.0201(16) 0.0053(14) 0.0043(13) 0.0027(14) O38 0.0226(17) 0.0168(15) 0.0214(16) 0.0040(13) 0.0080(13) 0.0020(13) C5 0.031(3) 0.033(3) 0.026(3) 0.008(2) 0.013(2) 0.001(2) C6 0.044(4) 0.058(4) 0.058(4) 0.013(3) 0.008(3) 0.017(3) C7 0.053(4) 0.067(5) 0.038(3) 0.008(3) 0.002(3) 0.000(4) C8 0.053(4) 0.030(3) 0.050(4) 0.006(3) 0.018(3) -0.005(3) N1 0.033(3) 0.033(2) 0.029(2) 0.010(2) -0.0042(18) 0.0027(19) C9 0.029(3) 0.045(3) 0.043(3) 0.009(3) -0.001(2) 0.005(2) C10 0.044(4) 0.062(4) 0.056(4) 0.010(3) 0.010(3) -0.001(3) C11 0.044(5) 0.118(7) 0.087(6) -0.016(5) 0.011(4) 0.019(4) C12X 0.054(8) 0.10(2) 0.062(16) 0.009(15) 0.005(12) 0.011(10) C12Y 0.073(9) 0.136(12) 0.056(7) 0.016(7) 0.014(6) 0.034(8) C13 0.049(4) 0.037(3) 0.038(3) 0.019(3) -0.010(3) -0.006(3) C14 0.075(5) 0.044(4) 0.070(5) 0.023(4) -0.032(4) -0.017(3) C15 0.071(6) 0.058(5) 0.116(7) 0.045(5) -0.044(5) -0.028(4) C16 0.121(9) 0.070(6) 0.184(11) 0.051(7) -0.079(8) -0.054(6) C17 0.046(3) 0.029(3) 0.029(3) 0.008(2) -0.004(2) 0.002(2) C18 0.043(4) 0.034(3) 0.042(3) 0.005(3) 0.009(3) -0.003(3) C19 0.081(5) 0.030(3) 0.046(3) 0.004(3) 0.015(3) 0.014(3) C20 0.093(6) 0.042(4) 0.070(5) -0.017(4) 0.033(4) -0.005(4) C21 0.034(3) 0.034(3) 0.031(3) 0.006(2) -0.004(2) 0.002(2) C22 0.037(3) 0.036(3) 0.036(3) 0.008(3) 0.000(2) -0.002(2) C23 0.042(4) 0.047(3) 0.050(4) 0.011(3) -0.007(3) -0.008(3) C24 0.061(5) 0.050(4) 0.077(5) 0.017(4) -0.021(4) -0.021(3) N2 0.029(2) 0.021(2) 0.028(2) -0.0076(17) 0.0019(17) 0.0026(17) C25 0.030(3) 0.025(2) 0.027(3) -0.005(2) -0.001(2) -0.002(2) C26 0.052(4) 0.049(4) 0.028(3) -0.002(3) 0.001(3) -0.018(3) C27 0.042(3) 0.033(3) 0.037(3) 0.000(3) 0.004(3) -0.006(2) C28 0.047(4) 0.108(7) 0.094(6) 0.038(5) -0.008(4) -0.024(5) C29 0.035(3) 0.024(2) 0.028(3) -0.008(2) 0.004(2) 0.006(2) C30 0.038(3) 0.032(3) 0.038(3) -0.006(3) -0.001(2) 0.009(2) C31 0.053(4) 0.047(4) 0.046(4) -0.005(3) 0.006(3) 0.023(3) C32 0.063(5) 0.068(5) 0.075(5) 0.003(4) 0.007(4) 0.038(4) C33 0.049(4) 0.025(3) 0.024(2) -0.005(2) 0.001(2) 0.008(2) C34 0.056(4) 0.047(4) 0.047(3) 0.003(3) 0.016(3) -0.003(3) C35 0.094(6) 0.068(5) 0.052(4) 0.000(4) 0.023(4) 0.001(5) C36 0.116(8) 0.087(7) 0.071(5) -0.014(5) -0.004(5) -0.004(6) C37 0.026(3) 0.026(3) 0.031(3) -0.007(2) 0.001(2) 0.004(2) C38 0.038(3) 0.030(3) 0.046(3) -0.013(3) -0.004(3) 0.008(2) C39 0.032(3) 0.037(3) 0.051(3) -0.003(3) -0.003(3) -0.001(2) C40 0.068(5) 0.073(5) 0.048(4) 0.004(4) -0.012(3) 0.016(4) N3 0.026(2) 0.026(2) 0.023(2) 0.0060(17) 0.0015(16) -0.0038(17) C41 0.036(3) 0.023(2) 0.030(3) 0.003(2) 0.005(2) 0.000(2) C42 0.043(3) 0.031(3) 0.031(3) 0.001(2) -0.001(2) -0.003(2) C43 0.108(7) 0.035(3) 0.056(4) -0.008(3) -0.030(4) 0.010(4) C44 0.110(7) 0.048(4) 0.042(4) -0.012(3) -0.023(4) 0.011(4) C45 0.027(3) 0.024(2) 0.027(3) 0.001(2) -0.003(2) -0.002(2) C46 0.034(3) 0.033(3) 0.030(3) 0.005(2) 0.003(2) -0.004(2) C47 0.042(4) 0.036(3) 0.074(5) 0.000(3) 0.016(3) 0.003(3) C48 0.046(4) 0.062(5) 0.067(5) 0.001(4) 0.016(3) 0.008(3) C49 0.030(3) 0.038(3) 0.020(2) 0.012(2) 0.000(2) -0.005(2) C50 0.056(4) 0.043(3) 0.024(3) 0.007(2) -0.009(3) -0.010(3) C51 0.049(4) 0.047(3) 0.026(3) 0.005(3) -0.005(2) -0.004(3) C52 0.087(6) 0.068(5) 0.038(4) -0.003(3) -0.022(4) -0.014(4) C53 0.033(3) 0.033(3) 0.027(3) 0.009(2) 0.002(2) -0.007(2) C54 0.034(3) 0.043(3) 0.039(3) 0.009(3) 0.008(2) -0.005(3) C55 0.040(3) 0.056(4) 0.043(3) 0.009(3) 0.013(3) -0.009(3) C56 0.037(4) 0.079(5) 0.046(4) 0.001(4) 0.008(3) -0.008(3) N4 0.016(2) 0.033(2) 0.033(2) -0.002(2) -0.0039(17) 0.0016(17) C57 0.036(3) 0.044(3) 0.035(3) -0.002(3) -0.011(2) -0.003(3) C58 0.068(5) 0.085(5) 0.034(3) -0.011(3) -0.005(3) 0.014(4) C59X 0.079(14) 0.069(12) 0.041(8) -0.012(9) -0.005(8) -0.014(11) C60X 0.12(2) 0.111(18) 0.060(13) 0.004(13) -0.035(12) 0.015(16) C59Y 0.081(9) 0.037(6) 0.040(5) -0.004(5) 0.000(5) -0.006(6) C60Y 0.071(10) 0.092(11) 0.057(8) -0.001(8) -0.017(6) -0.018(8) C61 0.019(3) 0.036(3) 0.035(3) 0.001(2) -0.003(2) -0.003(2) C62 0.031(3) 0.041(3) 0.065(4) 0.003(3) -0.007(3) -0.002(3) C63 0.032(3) 0.037(3) 0.060(4) -0.001(3) 0.004(3) -0.003(3) C64 0.053(4) 0.038(3) 0.081(5) 0.001(3) 0.011(4) -0.005(3) C65 0.021(3) 0.035(3) 0.040(3) 0.001(2) 0.004(2) -0.002(2) C66 0.038(4) 0.054(4) 0.044(3) -0.006(3) 0.009(3) 0.010(3) C67 0.041(4) 0.071(5) 0.054(4) 0.004(4) 0.021(3) 0.012(3) C68 0.084(6) 0.096(6) 0.050(4) 0.000(4) 0.033(4) 0.010(5) C69 0.022(3) 0.033(3) 0.040(3) -0.003(2) -0.003(2) 0.004(2) C70 0.033(3) 0.040(3) 0.053(4) 0.005(3) 0.001(3) -0.002(2) C71 0.040(4) 0.035(3) 0.069(4) 0.000(3) -0.014(3) -0.004(3) C72 0.049(4) 0.045(4) 0.065(4) 0.018(3) 0.000(3) -0.007(3) N5 0.058(3) 0.035(3) 0.045(3) -0.021(2) 0.031(2) -0.027(2) C73 0.064(4) 0.050(4) 0.056(4) -0.006(3) 0.019(3) -0.028(3) C74X 0.049(9) 0.031(9) 0.056(7) -0.024(7) 0.032(5) -0.009(6) C75X 0.060(10) 0.047(9) 0.052(7) -0.014(7) 0.011(6) -0.006(8) C76X 0.071(14) 0.024(9) 0.075(11) -0.011(9) -0.003(10) 0.011(10) C74Y 0.063(8) 0.054(8) 0.059(7) -0.025(6) 0.020(5) -0.025(6) C75Y 0.110(11) 0.050(7) 0.060(8) -0.007(6) -0.004(7) -0.031(7) C76Y 0.120(18) 0.075(12) 0.074(11) -0.006(10) -0.015(11) -0.034(12) C77 0.080(5) 0.053(4) 0.056(4) -0.035(3) 0.048(4) -0.035(3) C78 0.067(5) 0.053(4) 0.058(4) -0.024(3) 0.033(3) -0.033(3) C79X 0.037(6) 0.084(9) 0.045(6) 0.000(5) 0.012(5) -0.020(6) C79Y 0.063(13) 0.039(8) 0.044(8) 0.000(7) 0.018(9) -0.014(8) C80 0.082(6) 0.051(4) 0.070(5) -0.010(3) 0.048(4) -0.017(4) C81 0.052(4) 0.033(3) 0.049(3) -0.022(3) 0.025(3) -0.019(3) C82 0.051(4) 0.040(3) 0.066(4) -0.015(3) 0.027(3) -0.020(3) C83 0.045(4) 0.047(4) 0.069(4) -0.012(3) 0.027(3) -0.018(3) C84 0.059(5) 0.061(5) 0.087(6) -0.008(4) 0.018(4) -0.017(4) C85 0.063(4) 0.038(3) 0.044(3) -0.022(3) 0.030(3) -0.029(3) C86 0.060(4) 0.035(3) 0.053(4) -0.021(3) 0.032(3) -0.021(3) C87 0.076(5) 0.039(3) 0.061(4) -0.025(3) 0.039(4) -0.031(3) C88 0.090(6) 0.059(5) 0.078(5) -0.018(4) 0.045(5) -0.037(4) N6 0.010(2) 0.043(2) 0.049(3) 0.006(2) 0.0126(18) 0.0032(18) C89 0.024(3) 0.044(3) 0.060(3) 0.000(3) 0.003(3) 0.004(2) C90 0.034(4) 0.075(5) 0.070(4) 0.012(4) 0.000(3) -0.003(3) C91 0.057(5) 0.058(4) 0.069(5) 0.006(4) -0.015(4) 0.007(4) C92 0.063(5) 0.086(6) 0.058(5) -0.018(4) 0.006(4) -0.017(4) C93 0.022(3) 0.043(3) 0.048(3) 0.003(3) 0.007(2) -0.001(2) C94 0.029(3) 0.043(3) 0.067(4) 0.002(3) 0.012(3) 0.002(3) C95 0.032(4) 0.040(3) 0.094(5) 0.002(3) 0.008(3) 0.004(3) C96 0.036(4) 0.045(4) 0.117(7) -0.006(4) 0.007(4) -0.003(3) C97 0.031(3) 0.035(3) 0.053(3) 0.001(3) 0.019(2) 0.002(2) C98 0.041(4) 0.038(3) 0.051(3) 0.001(3) 0.009(3) 0.007(3) C99 0.047(4) 0.041(3) 0.058(4) -0.010(3) 0.022(3) -0.008(3) C100 0.081(5) 0.041(4) 0.050(4) 0.003(3) 0.015(3) 0.002(4) C101 0.017(3) 0.044(3) 0.044(3) -0.003(3) 0.011(2) 0.007(2) C102 0.026(3) 0.040(3) 0.053(4) 0.000(3) 0.006(3) 0.004(2) C103 0.033(3) 0.052(3) 0.038(3) -0.009(3) 0.001(3) 0.000(3) C104 0.066(5) 0.047(4) 0.063(5) -0.012(3) 0.005(4) 0.000(3) N7 0.118(7) 0.101(6) 0.094(6) 0.038(5) 0.000(5) -0.037(5) C105 0.052(4) 0.061(5) 0.058(4) -0.009(3) 0.002(3) -0.023(4) C106 0.051(4) 0.070(5) 0.067(5) -0.008(4) -0.022(4) 0.006(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 Mo1 O2 1.703(3) . ? Mo1 O7 1.837(3) . ? Mo1 O11 2.049(3) . ? Mo1 O12 1.857(3) . ? Mo1 O15 1.971(3) . ? Mo1 O19 2.324(3) . ? Mo2 O3 1.699(3) . ? Mo2 O8 1.854(3) . ? Mo2 O12 2.046(3) . ? Mo2 O13 1.858(3) . ? Mo2 O16 1.944(3) . ? Mo2 O19 2.329(3) . ? Mo3 O4 1.692(4) . ? Mo3 O9 1.860(4) . ? Mo3 O13 2.044(4) . ? Mo3 O14 1.871(4) . ? Mo3 O17 1.941(4) . ? Mo3 O19 2.337(3) . ? Mo4 O5 1.702(3) . ? Mo4 O10 1.846(3) . ? Mo4 O11 1.862(3) . ? Mo4 O14 2.030(4) . ? Mo4 O18 1.974(3) . ? Mo4 O19 2.325(3) . ? Mo5 O6 1.692(4) . ? Mo5 O15 1.903(3) . ? Mo5 O16 1.926(3) . ? Mo5 O17 1.925(3) . ? Mo5 O18 1.899(3) . ? Mo5 O19 2.358(3) . ? Ti1 O1 1.790(3) . ? Ti1 O7 1.976(4) . ? Ti1 O8 1.930(3) . ? Ti1 O9 1.942(4) . ? Ti1 O10 1.976(3) . ? Ti1 O19 2.156(3) . ? O1 C1 1.412(6) . ? C1 C2 1.500(8) . ? C1 C3 1.517(8) . ? C1 C4 1.516(8) . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? Mo6 O21 1.697(4) . ? Mo6 O26 1.835(3) . ? Mo6 O30 1.879(3) . ? Mo6 O31 2.029(4) . ? Mo6 O34 1.952(3) . ? Mo6 O38 2.339(3) . ? Mo7 O22 1.702(3) . ? Mo7 O27 1.826(3) . ? Mo7 O31 1.874(4) . ? Mo7 O32 2.018(4) . ? Mo7 O35 1.985(3) . ? Mo7 O38 2.326(3) . ? Mo8 O23 1.698(4) . ? Mo8 O28 1.849(3) . ? Mo8 O32 1.881(3) . ? Mo8 O33 2.026(3) . ? Mo8 O36 1.961(3) . ? Mo8 O38 2.323(3) . ? Mo9 O24 1.698(3) . ? Mo9 O29 1.864(3) . ? Mo9 O30 2.029(3) . ? Mo9 O33 1.875(3) . ? Mo9 O37 1.928(3) . ? Mo9 O38 2.337(3) . ? Mo10 O25 1.699(3) . ? Mo10 O34 1.900(3) . ? Mo10 O35 1.887(3) . ? Mo10 O36 1.914(3) . ? Mo10 O37 1.946(3) . ? Mo10 O38 2.354(3) . ? Ti2 O20 1.787(3) . ? Ti2 O26 1.966(4) . ? Ti2 O27 2.000(4) . ? Ti2 O28 1.965(4) . ? Ti2 O29 1.931(3) . ? Ti2 O38 2.148(3) . ? O20 C5 1.433(6) . ? C5 C6 1.505(8) . ? C5 C7 1.503(8) . ? C5 C8 1.513(7) . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? N1 C9 1.511(6) . ? N1 C13 1.520(6) . ? N1 C17 1.525(6) . ? N1 C21 1.518(6) . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.517(7) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.516(8) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 H11C 0.990 . ? C11 H11D 0.990 . ? C11 C12X 1.513(13) . ? C11 C12Y 1.447(9) . ? C12X H12A 0.980 . ? C12X H12B 0.980 . ? C12X H12C 0.980 . ? C12Y H12D 0.980 . ? C12Y H12E 0.980 . ? C12Y H12F 0.980 . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 C14 1.515(7) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.514(7) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.515(8) . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.516(7) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C18 C19 1.526(7) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.503(8) . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.512(6) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.513(7) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 C24 1.514(7) . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? N2 C25 1.519(6) . ? N2 C29 1.520(5) . ? N2 C33 1.521(6) . ? N2 C37 1.518(6) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C25 C26 1.514(6) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C26 C27 1.514(7) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C27 C28 1.490(8) . ? C28 H28A 0.980 . ? C28 H28B 0.980 . ? C28 H28C 0.980 . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C29 C30 1.512(6) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C30 C31 1.524(7) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C31 C32 1.509(8) . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C33 H33A 0.990 . ? C33 H33B 0.990 . ? C33 C34 1.517(7) . ? C34 H34A 0.990 . ? C34 H34B 0.990 . ? C34 C35 1.502(7) . ? C35 H35A 0.990 . ? C35 H35B 0.990 . ? C35 C36 1.494(9) . ? C36 H36A 0.980 . ? C36 H36B 0.980 . ? C36 H36C 0.980 . ? C37 H37A 0.990 . ? C37 H37B 0.990 . ? C37 C38 1.520(6) . ? C38 H38A 0.990 . ? C38 H38B 0.990 . ? C38 C39 1.519(7) . ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? C39 C40 1.485(7) . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? N3 C41 1.522(6) . ? N3 C45 1.511(6) . ? N3 C49 1.518(5) . ? N3 C53 1.520(5) . ? C41 H41A 0.990 . ? C41 H41B 0.990 . ? C41 C42 1.512(6) . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C42 C43 1.487(7) . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C43 C44 1.514(7) . ? C44 H44A 0.980 . ? C44 H44B 0.980 . ? C44 H44C 0.980 . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C45 C46 1.512(6) . ? C46 H46A 0.990 . ? C46 H46B 0.990 . ? C46 C47 1.512(7) . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C47 C48 1.499(7) . ? C48 H48A 0.980 . ? C48 H48B 0.980 . ? C48 H48C 0.980 . ? C49 H49A 0.990 . ? C49 H49B 0.990 . ? C49 C50 1.512(7) . ? C50 H50A 0.990 . ? C50 H50B 0.990 . ? C50 C51 1.524(6) . ? C51 H51A 0.990 . ? C51 H51B 0.990 . ? C51 C52 1.519(7) . ? C52 H52A 0.980 . ? C52 H52B 0.980 . ? C52 H52C 0.980 . ? C53 H53A 0.990 . ? C53 H53B 0.990 . ? C53 C54 1.514(7) . ? C54 H54A 0.990 . ? C54 H54B 0.990 . ? C54 C55 1.503(6) . ? C55 H55A 0.990 . ? C55 H55B 0.990 . ? C55 C56 1.504(7) . ? C56 H56A 0.980 . ? C56 H56B 0.980 . ? C56 H56C 0.980 . ? N4 C57 1.520(6) . ? N4 C61 1.525(6) . ? N4 C65 1.518(6) . ? N4 C69 1.519(6) . ? C57 H57A 0.990 . ? C57 H57B 0.990 . ? C57 C58 1.519(7) . ? C58 H58A 0.990 . ? C58 H58B 0.990 . ? C58 H58C 0.990 . ? C58 H58D 0.990 . ? C58 C59X 1.552(12) . ? C58 C59Y 1.539(10) . ? C59X H59A 0.990 . ? C59X H59B 0.990 . ? C59X C60X 1.494(13) . ? C60X H60A 0.980 . ? C60X H60B 0.980 . ? C60X H60C 0.980 . ? C59Y H59C 0.990 . ? C59Y H59D 0.990 . ? C59Y C60Y 1.488(11) . ? C60Y H60D 0.980 . ? C60Y H60E 0.980 . ? C60Y H60F 0.980 . ? C61 H61A 0.990 . ? C61 H61B 0.990 . ? C61 C62 1.514(7) . ? C62 H62A 0.990 . ? C62 H62B 0.990 . ? C62 C63 1.507(7) . ? C63 H63A 0.990 . ? C63 H63B 0.990 . ? C63 C64 1.504(7) . ? C64 H64A 0.980 . ? C64 H64B 0.980 . ? C64 H64C 0.980 . ? C65 H65A 0.990 . ? C65 H65B 0.990 . ? C65 C66 1.513(7) . ? C66 H66A 0.990 . ? C66 H66B 0.990 . ? C66 C67 1.513(7) . ? C67 H67A 0.990 . ? C67 H67B 0.990 . ? C67 C68 1.512(8) . ? C68 H68A 0.980 . ? C68 H68B 0.980 . ? C68 H68C 0.980 . ? C69 H69A 0.990 . ? C69 H69B 0.990 . ? C69 C70 1.506(7) . ? C70 H70A 0.990 . ? C70 H70B 0.990 . ? C70 C71 1.497(7) . ? C71 H71A 0.990 . ? C71 H71B 0.990 . ? C71 C72 1.501(7) . ? C72 H72A 0.980 . ? C72 H72B 0.980 . ? C72 H72C 0.980 . ? N5 C73 1.507(7) . ? N5 C77 1.530(6) . ? N5 C81 1.519(7) . ? N5 C85 1.524(6) . ? C73 H73A 0.990 . ? C73 H73B 0.990 . ? C73 H73C 0.990 . ? C73 H73D 0.990 . ? C73 C74X 1.493(11) . ? C73 C74Y 1.563(10) . ? C74X H74A 0.990 . ? C74X H74B 0.990 . ? C74X C75X 1.514(12) . ? C75X H75A 0.990 . ? C75X H75B 0.990 . ? C75X C76X 1.509(13) . ? C76X H76A 0.980 . ? C76X H76B 0.980 . ? C76X H76C 0.980 . ? C74Y H74C 0.990 . ? C74Y H74D 0.990 . ? C74Y C75Y 1.509(12) . ? C75Y H75C 0.990 . ? C75Y H75D 0.990 . ? C75Y C76Y 1.507(12) . ? C76Y H76D 0.980 . ? C76Y H76E 0.980 . ? C76Y H76F 0.980 . ? C77 H77A 0.990 . ? C77 H77B 0.990 . ? C77 C78 1.510(7) . ? C78 H78A 0.990 . ? C78 H78B 0.990 . ? C78 H78C 0.990 . ? C78 H78D 0.990 . ? C78 C79X 1.550(9) . ? C78 C79Y 1.503(11) . ? C79X H79A 0.990 . ? C79X H79B 0.990 . ? C79X C80 1.422(9) . ? C79Y H79C 0.990 . ? C79Y H79D 0.990 . ? C79Y C80 1.469(12) . ? C80 H80A 0.980 . ? C80 H80B 0.980 . ? C80 H80C 0.980 . ? C80 H80D 0.980 . ? C80 H80E 0.980 . ? C80 H80F 0.980 . ? C81 H81A 0.990 . ? C81 H81B 0.990 . ? C81 C82 1.513(8) . ? C82 H82A 0.990 . ? C82 H82B 0.990 . ? C82 C83 1.523(7) . ? C83 H83A 0.990 . ? C83 H83B 0.990 . ? C83 C84 1.503(8) . ? C84 H84A 0.980 . ? C84 H84B 0.980 . ? C84 H84C 0.980 . ? C85 H85A 0.990 . ? C85 H85B 0.990 . ? C85 C86 1.511(7) . ? C86 H86A 0.990 . ? C86 H86B 0.990 . ? C86 C87 1.522(7) . ? C87 H87A 0.990 . ? C87 H87B 0.990 . ? C87 C88 1.490(7) . ? C88 H88A 0.980 . ? C88 H88B 0.980 . ? C88 H88C 0.980 . ? N6 C89 1.510(6) . ? N6 C93 1.539(6) . ? N6 C97 1.516(6) . ? N6 C101 1.527(6) . ? C89 H89A 0.990 . ? C89 H89B 0.990 . ? C89 C90 1.515(7) . ? C90 H90A 0.990 . ? C90 H90B 0.990 . ? C90 C91 1.521(8) . ? C91 H91A 0.990 . ? C91 H91B 0.990 . ? C91 C92 1.489(8) . ? C92 H92A 0.980 . ? C92 H92B 0.980 . ? C92 H92C 0.980 . ? C93 H93A 0.990 . ? C93 H93B 0.990 . ? C93 C94 1.519(7) . ? C94 H94A 0.990 . ? C94 H94B 0.990 . ? C94 C95 1.502(7) . ? C95 H95A 0.990 . ? C95 H95B 0.990 . ? C95 C96 1.517(8) . ? C96 H96A 0.980 . ? C96 H96B 0.980 . ? C96 H96C 0.980 . ? C97 H97A 0.990 . ? C97 H97B 0.990 . ? C97 C98 1.504(7) . ? C98 H98A 0.990 . ? C98 H98B 0.990 . ? C98 C99 1.517(7) . ? C99 H99A 0.990 . ? C99 H99B 0.990 . ? C99 C100 1.501(8) . ? C100 H10C 0.980 . ? C100 H10D 0.980 . ? C100 H10E 0.980 . ? C101 H10F 0.990 . ? C101 H10G 0.990 . ? C101 C102 1.521(7) . ? C102 H10H 0.990 . ? C102 H10I 0.990 . ? C102 C103 1.517(7) . ? C103 H10J 0.990 . ? C103 H10K 0.990 . ? C103 C104 1.508(7) . ? C104 H10L 0.980 . ? C104 H10M 0.980 . ? C104 H10N 0.980 . ? N7 C105 1.126(10) . ? C105 C106 1.451(11) . ? 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 O2 Mo1 O7 104.51(17) . . ? O2 Mo1 O11 100.45(17) . . ? O2 Mo1 O12 104.34(17) . . ? O2 Mo1 O15 101.56(16) . . ? O2 Mo1 O19 175.57(15) . . ? O7 Mo1 O11 85.25(14) . . ? O7 Mo1 O12 94.37(15) . . ? O7 Mo1 O15 152.29(14) . . ? O7 Mo1 O19 77.04(13) . . ? O11 Mo1 O12 154.45(14) . . ? O11 Mo1 O15 80.93(14) . . ? O11 Mo1 O19 75.45(12) . . ? O12 Mo1 O15 88.12(14) . . ? O12 Mo1 O19 79.57(12) . . ? O15 Mo1 O19 76.30(12) . . ? O3 Mo2 O8 103.37(16) . . ? O3 Mo2 O12 99.19(16) . . ? O3 Mo2 O13 105.32(17) . . ? O3 Mo2 O16 103.18(16) . . ? O3 Mo2 O19 175.08(15) . . ? O8 Mo2 O12 85.71(14) . . ? O8 Mo2 O13 92.88(15) . . ? O8 Mo2 O16 152.00(14) . . ? O8 Mo2 O19 76.49(12) . . ? O12 Mo2 O13 155.08(14) . . ? O12 Mo2 O16 81.43(14) . . ? O12 Mo2 O19 75.88(12) . . ? O13 Mo2 O16 88.59(15) . . ? O13 Mo2 O19 79.59(13) . . ? O16 Mo2 O19 76.29(12) . . ? O4 Mo3 O9 104.14(19) . . ? O4 Mo3 O13 100.79(18) . . ? O4 Mo3 O14 104.61(18) . . ? O4 Mo3 O17 102.43(19) . . ? O4 Mo3 O19 176.63(17) . . ? O9 Mo3 O13 84.74(15) . . ? O9 Mo3 O14 92.37(16) . . ? O9 Mo3 O17 152.13(14) . . ? O9 Mo3 O19 76.30(12) . . ? O13 Mo3 O14 154.36(14) . . ? O13 Mo3 O17 82.19(15) . . ? O13 Mo3 O19 75.89(12) . . ? O14 Mo3 O17 88.95(16) . . ? O14 Mo3 O19 78.67(13) . . ? O17 Mo3 O19 76.69(12) . . ? O5 Mo4 O10 104.14(16) . . ? O5 Mo4 O11 104.94(17) . . ? O5 Mo4 O14 99.98(17) . . ? O5 Mo4 O18 101.65(16) . . ? O5 Mo4 O19 175.67(16) . . ? O10 Mo4 O11 93.33(16) . . ? O10 Mo4 O14 86.18(16) . . ? O10 Mo4 O18 152.93(14) . . ? O10 Mo4 O19 77.42(13) . . ? O11 Mo4 O14 154.39(14) . . ? O11 Mo4 O18 87.84(14) . . ? O11 Mo4 O19 78.90(13) . . ? O14 Mo4 O18 81.38(14) . . ? O14 Mo4 O19 76.00(12) . . ? O18 Mo4 O19 76.29(12) . . ? O6 Mo5 O15 104.32(17) . . ? O6 Mo5 O16 102.30(16) . . ? O6 Mo5 O17 102.52(17) . . ? O6 Mo5 O18 104.98(16) . . ? O6 Mo5 O19 177.93(15) . . ? O15 Mo5 O16 87.16(15) . . ? O15 Mo5 O17 153.10(14) . . ? O15 Mo5 O18 87.36(14) . . ? O15 Mo5 O19 76.67(12) . . ? O16 Mo5 O17 85.53(15) . . ? O16 Mo5 O18 152.70(14) . . ? O16 Mo5 O19 75.88(12) . . ? O17 Mo5 O18 87.37(15) . . ? O17 Mo5 O19 76.44(13) . . ? O18 Mo5 O19 76.82(12) . . ? O1 Ti1 O7 101.22(16) . . ? O1 Ti1 O8 100.83(15) . . ? O1 Ti1 O9 100.93(17) . . ? O1 Ti1 O10 100.65(16) . . ? O1 Ti1 O19 179.68(17) . . ? O7 Ti1 O8 87.89(14) . . ? O7 Ti1 O9 157.83(14) . . ? O7 Ti1 O10 86.92(15) . . ? O7 Ti1 O19 78.56(13) . . ? O8 Ti1 O9 88.85(15) . . ? O8 Ti1 O10 158.50(14) . . ? O8 Ti1 O19 79.41(13) . . ? O9 Ti1 O10 88.13(16) . . ? O9 Ti1 O19 79.28(13) . . ? O10 Ti1 O19 79.11(13) . . ? Ti1 O1 C1 154.6(4) . . ? Mo1 O7 Ti1 113.37(16) . . ? Mo2 O8 Ti1 113.84(16) . . ? Mo3 O9 Ti1 113.94(16) . . ? Mo4 O10 Ti1 112.80(17) . . ? Mo1 O11 Mo4 115.04(16) . . ? Mo1 O12 Mo2 114.56(15) . . ? Mo2 O13 Mo3 114.82(17) . . ? Mo3 O14 Mo4 115.26(16) . . ? Mo1 O15 Mo5 117.01(16) . . ? Mo2 O16 Mo5 117.71(17) . . ? Mo3 O17 Mo5 117.22(17) . . ? Mo4 O18 Mo5 116.97(16) . . ? Mo1 O19 Mo2 89.84(10) . . ? Mo1 O19 Mo3 178.94(16) . . ? Mo1 O19 Mo4 90.48(11) . . ? Mo1 O19 Mo5 89.75(10) . . ? Mo1 O19 Ti1 90.64(11) . . ? Mo2 O19 Mo3 89.68(11) . . ? Mo2 O19 Mo4 179.48(16) . . ? Mo2 O19 Mo5 89.92(10) . . ? Mo2 O19 Ti1 89.90(11) . . ? Mo3 O19 Mo4 90.00(10) . . ? Mo3 O19 Mo5 89.31(10) . . ? Mo3 O19 Ti1 90.30(11) . . ? Mo4 O19 Mo5 89.67(10) . . ? Mo4 O19 Ti1 90.51(11) . . ? Mo5 O19 Ti1 179.58(17) . . ? O1 C1 C2 108.8(5) . . ? O1 C1 C3 107.1(5) . . ? O1 C1 C4 107.5(5) . . ? C2 C1 C3 109.9(5) . . ? C2 C1 C4 111.7(6) . . ? C3 C1 C4 111.6(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O21 Mo6 O26 104.85(18) . . ? O21 Mo6 O30 104.26(19) . . ? O21 Mo6 O31 101.45(19) . . ? O21 Mo6 O34 101.91(17) . . ? O21 Mo6 O38 176.29(17) . . ? O26 Mo6 O30 92.59(15) . . ? O26 Mo6 O31 85.76(15) . . ? O26 Mo6 O34 152.22(16) . . ? O26 Mo6 O38 76.47(14) . . ? O30 Mo6 O31 153.77(14) . . ? O30 Mo6 O34 87.94(14) . . ? O30 Mo6 O38 79.05(13) . . ? O31 Mo6 O34 81.75(14) . . ? O31 Mo6 O38 75.11(13) . . ? O34 Mo6 O38 76.37(12) . . ? O22 Mo7 O27 105.12(16) . . ? O22 Mo7 O31 103.86(19) . . ? O22 Mo7 O32 101.17(19) . . ? O22 Mo7 O35 100.79(15) . . ? O22 Mo7 O38 176.42(16) . . ? O27 Mo7 O31 93.57(16) . . ? O27 Mo7 O32 86.86(16) . . ? O27 Mo7 O35 153.20(14) . . ? O27 Mo7 O38 77.46(13) . . ? O31 Mo7 O32 153.91(14) . . ? O31 Mo7 O35 86.73(14) . . ? O31 Mo7 O38 78.30(13) . . ? O32 Mo7 O35 81.49(14) . . ? O32 Mo7 O38 76.34(12) . . ? O35 Mo7 O38 76.38(11) . . ? O23 Mo8 O28 105.74(16) . . ? O23 Mo8 O32 103.19(17) . . ? O23 Mo8 O33 101.47(15) . . ? O23 Mo8 O36 100.51(16) . . ? O23 Mo8 O38 176.14(15) . . ? O28 Mo8 O32 93.07(15) . . ? O28 Mo8 O33 85.82(14) . . ? O28 Mo8 O36 152.79(15) . . ? O28 Mo8 O38 77.17(13) . . ? O32 Mo8 O33 154.65(14) . . ? O32 Mo8 O36 87.73(14) . . ? O32 Mo8 O38 78.99(13) . . ? O33 Mo8 O36 82.08(13) . . ? O33 Mo8 O38 76.07(12) . . ? O36 Mo8 O38 76.30(12) . . ? O24 Mo9 O29 104.00(15) . . ? O24 Mo9 O30 101.56(15) . . ? O24 Mo9 O33 103.53(15) . . ? O24 Mo9 O37 102.49(15) . . ? O24 Mo9 O38 177.82(15) . . ? O29 Mo9 O30 85.34(14) . . ? O29 Mo9 O33 91.86(14) . . ? O29 Mo9 O37 152.58(13) . . ? O29 Mo9 O38 76.46(12) . . ? O30 Mo9 O33 154.68(13) . . ? O30 Mo9 O37 82.57(13) . . ? O30 Mo9 O38 76.33(12) . . ? O33 Mo9 O37 88.72(13) . . ? O33 Mo9 O38 78.55(12) . . ? O37 Mo9 O38 76.81(12) . . ? O25 Mo10 O34 103.83(15) . . ? O25 Mo10 O35 103.76(14) . . ? O25 Mo10 O36 102.80(15) . . ? O25 Mo10 O37 102.73(14) . . ? O25 Mo10 O38 178.55(14) . . ? O34 Mo10 O35 88.55(15) . . ? O34 Mo10 O36 153.25(13) . . ? O34 Mo10 O37 86.20(14) . . ? O34 Mo10 O38 76.94(12) . . ? O35 Mo10 O36 87.52(15) . . ? O35 Mo10 O37 153.49(13) . . ? O35 Mo10 O38 77.45(12) . . ? O36 Mo10 O37 85.62(14) . . ? O36 Mo10 O38 76.38(12) . . ? O37 Mo10 O38 76.04(11) . . ? O20 Ti2 O26 98.16(17) . . ? O20 Ti2 O27 98.06(16) . . ? O20 Ti2 O28 103.67(17) . . ? O20 Ti2 O29 103.52(16) . . ? O20 Ti2 O38 175.39(15) . . ? O26 Ti2 O27 87.37(16) . . ? O26 Ti2 O28 157.97(14) . . ? O26 Ti2 O29 88.52(15) . . ? O26 Ti2 O38 78.74(13) . . ? O27 Ti2 O28 86.73(16) . . ? O27 Ti2 O29 158.40(14) . . ? O27 Ti2 O38 78.48(13) . . ? O28 Ti2 O29 89.21(15) . . ? O28 Ti2 O38 79.29(13) . . ? O29 Ti2 O38 79.92(13) . . ? Ti2 O20 C5 149.8(3) . . ? Mo6 O26 Ti2 114.00(17) . . ? Mo7 O27 Ti2 112.95(16) . . ? Mo8 O28 Ti2 112.91(16) . . ? Mo9 O29 Ti2 113.46(16) . . ? Mo6 O30 Mo9 114.95(16) . . ? Mo6 O31 Mo7 116.02(16) . . ? Mo7 O32 Mo8 114.65(17) . . ? Mo8 O33 Mo9 115.30(15) . . ? Mo6 O34 Mo10 117.49(16) . . ? Mo7 O35 Mo10 116.51(15) . . ? Mo8 O36 Mo10 117.07(16) . . ? Mo9 O37 Mo10 117.30(15) . . ? Mo6 O38 Mo7 90.43(11) . . ? Mo6 O38 Mo8 178.99(15) . . ? Mo6 O38 Mo9 89.64(11) . . ? Mo6 O38 Mo10 89.10(11) . . ? Mo6 O38 Ti2 90.43(12) . . ? Mo7 O38 Mo8 89.85(11) . . ? Mo7 O38 Mo9 179.15(15) . . ? Mo7 O38 Mo10 89.44(10) . . ? Mo7 O38 Ti2 90.89(11) . . ? Mo8 O38 Mo9 90.06(11) . . ? Mo8 O38 Mo10 89.94(11) . . ? Mo8 O38 Ti2 90.53(12) . . ? Mo9 O38 Mo10 89.71(10) . . ? Mo9 O38 Ti2 89.95(11) . . ? Mo10 O38 Ti2 179.42(18) . . ? O20 C5 C6 107.8(4) . . ? O20 C5 C7 107.6(5) . . ? O20 C5 C8 109.0(4) . . ? C6 C5 C7 109.3(5) . . ? C6 C5 C8 111.4(5) . . ? C7 C5 C8 111.6(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 N1 C13 111.4(4) . . ? C9 N1 C17 105.6(4) . . ? C9 N1 C21 110.3(4) . . ? C13 N1 C17 111.7(4) . . ? C13 N1 C21 106.6(4) . . ? C17 N1 C21 111.3(4) . . ? N1 C9 H9A 108.2 . . ? N1 C9 H9B 108.2 . . ? N1 C9 C10 116.2(4) . . ? H9A C9 H9B 107.4 . . ? H9A C9 C10 108.2 . . ? H9B C9 C10 108.2 . . ? C9 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? C9 C10 C11 108.3(5) . . ? H10A C10 H10B 108.4 . . ? H10A C10 C11 110.0 . . ? H10B C10 C11 110.0 . . ? C10 C11 H11A 110.3 . . ? C10 C11 H11B 110.3 . . ? C10 C11 H11C 107.8 . . ? C10 C11 H11D 107.8 . . ? C10 C11 C12X 107.2(11) . . ? C10 C11 C12Y 118.1(8) . . ? H11A C11 H11B 108.5 . . ? H11A C11 C12X 110.3 . . ? H11B C11 C12X 110.3 . . ? H11C C11 H11D 107.1 . . ? H11C C11 C12Y 107.8 . . ? H11D C11 C12Y 107.8 . . ? C11 C12X H12A 109.5 . . ? C11 C12X H12B 109.5 . . ? C11 C12X H12C 109.5 . . ? H12A C12X H12B 109.5 . . ? H12A C12X H12C 109.5 . . ? H12B C12X H12C 109.5 . . ? C11 C12Y H12D 109.5 . . ? C11 C12Y H12E 109.5 . . ? C11 C12Y H12F 109.5 . . ? H12D C12Y H12E 109.5 . . ? H12D C12Y H12F 109.5 . . ? H12E C12Y H12F 109.5 . . ? N1 C13 H13A 108.6 . . ? N1 C13 H13B 108.6 . . ? N1 C13 C14 114.8(4) . . ? H13A C13 H13B 107.5 . . ? H13A C13 C14 108.6 . . ? H13B C13 C14 108.6 . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C13 C14 C15 111.3(5) . . ? H14A C14 H14B 108.0 . . ? H14A C14 C15 109.4 . . ? H14B C14 C15 109.4 . . ? C14 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C14 C15 C16 111.8(6) . . ? H15A C15 H15B 107.9 . . ? H15A C15 C16 109.3 . . ? H15B C15 C16 109.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 H17A 108.5 . . ? N1 C17 H17B 108.5 . . ? N1 C17 C18 115.0(4) . . ? H17A C17 H17B 107.5 . . ? H17A C17 C18 108.5 . . ? H17B C17 C18 108.5 . . ? C17 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C17 C18 C19 110.3(5) . . ? H18A C18 H18B 108.1 . . ? H18A C18 C19 109.6 . . ? H18B C18 C19 109.6 . . ? C18 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C18 C19 C20 113.1(6) . . ? H19A C19 H19B 107.8 . . ? H19A C19 C20 109.0 . . ? H19B C19 C20 109.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 H21A 108.3 . . ? N1 C21 H21B 108.3 . . ? N1 C21 C22 115.9(4) . . ? H21A C21 H21B 107.4 . . ? H21A C21 C22 108.3 . . ? H21B C21 C22 108.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 C23 110.7(4) . . ? H22A C22 H22B 108.1 . . ? H22A C22 C23 109.5 . . ? H22B C22 C23 109.5 . . ? C22 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C22 C23 C24 112.3(5) . . ? H23A C23 H23B 107.9 . . ? H23A C23 C24 109.2 . . ? H23B C23 C24 109.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 N2 C29 111.6(4) . . ? C25 N2 C33 107.0(4) . . ? C25 N2 C37 110.3(4) . . ? C29 N2 C33 110.6(4) . . ? C29 N2 C37 106.2(3) . . ? C33 N2 C37 111.1(4) . . ? N2 C25 H25A 108.6 . . ? N2 C25 H25B 108.6 . . ? N2 C25 C26 114.5(4) . . ? H25A C25 H25B 107.6 . . ? H25A C25 C26 108.6 . . ? H25B C25 C26 108.6 . . ? C25 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C25 C26 C27 111.7(4) . . ? H26A C26 H26B 107.9 . . ? H26A C26 C27 109.3 . . ? H26B C26 C27 109.3 . . ? C26 C27 H27A 108.8 . . ? C26 C27 H27B 108.8 . . ? C26 C27 C28 113.6(5) . . ? H27A C27 H27B 107.7 . . ? H27A C27 C28 108.8 . . ? H27B C27 C28 108.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 H29A 108.5 . . ? N2 C29 H29B 108.5 . . ? N2 C29 C30 115.0(4) . . ? H29A C29 H29B 107.5 . . ? H29A C29 C30 108.5 . . ? H29B C29 C30 108.5 . . ? C29 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? C29 C30 C31 110.3(4) . . ? H30A C30 H30B 108.1 . . ? H30A C30 C31 109.6 . . ? H30B C30 C31 109.6 . . ? C30 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C30 C31 C32 111.8(5) . . ? H31A C31 H31B 107.9 . . ? H31A C31 C32 109.3 . . ? H31B C31 C32 109.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 108.4 . . ? N2 C33 H33B 108.4 . . ? N2 C33 C34 115.4(4) . . ? H33A C33 H33B 107.5 . . ? H33A C33 C34 108.4 . . ? H33B C33 C34 108.4 . . ? C33 C34 H34A 108.9 . . ? C33 C34 H34B 108.9 . . ? C33 C34 C35 113.2(5) . . ? H34A C34 H34B 107.8 . . ? H34A C34 C35 108.9 . . ? H34B C34 C35 108.9 . . ? C34 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? C34 C35 C36 113.4(7) . . ? H35A C35 H35B 107.7 . . ? H35A C35 C36 108.9 . . ? H35B C35 C36 108.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N2 C37 H37A 108.5 . . ? N2 C37 H37B 108.5 . . ? N2 C37 C38 114.9(4) . . ? H37A C37 H37B 107.5 . . ? H37A C37 C38 108.5 . . ? H37B C37 C38 108.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 C39 110.7(4) . . ? H38A C38 H38B 108.1 . . ? H38A C38 C39 109.5 . . ? H38B C38 C39 109.5 . . ? C38 C39 H39A 108.6 . . ? C38 C39 H39B 108.6 . . ? C38 C39 C40 114.6(5) . . ? H39A C39 H39B 107.6 . . ? H39A C39 C40 108.6 . . ? H39B C39 C40 108.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C41 N3 C45 110.3(4) . . ? C41 N3 C49 107.8(4) . . ? C41 N3 C53 110.6(4) . . ? C45 N3 C49 111.5(4) . . ? C45 N3 C53 105.8(3) . . ? C49 N3 C53 110.8(4) . . ? N3 C41 H41A 108.6 . . ? N3 C41 H41B 108.6 . . ? N3 C41 C42 114.7(4) . . ? H41A C41 H41B 107.6 . . ? H41A C41 C42 108.6 . . ? H41B C41 C42 108.6 . . ? C41 C42 H42A 109.0 . . ? C41 C42 H42B 109.0 . . ? C41 C42 C43 112.8(4) . . ? H42A C42 H42B 107.8 . . ? H42A C42 C43 109.0 . . ? H42B C42 C43 109.0 . . ? C42 C43 H43A 109.1 . . ? C42 C43 H43B 109.1 . . ? C42 C43 C44 112.6(5) . . ? H43A C43 H43B 107.8 . . ? H43A C43 C44 109.1 . . ? H43B C43 C44 109.1 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 H45A 108.2 . . ? N3 C45 H45B 108.2 . . ? N3 C45 C46 116.4(4) . . ? H45A C45 H45B 107.3 . . ? H45A C45 C46 108.2 . . ? H45B C45 C46 108.2 . . ? C45 C46 H46A 109.9 . . ? C45 C46 H46B 109.9 . . ? C45 C46 C47 109.0(4) . . ? H46A C46 H46B 108.3 . . ? H46A C46 C47 109.9 . . ? H46B C46 C47 109.9 . . ? C46 C47 H47A 108.8 . . ? C46 C47 H47B 108.8 . . ? C46 C47 C48 113.9(5) . . ? H47A C47 H47B 107.7 . . ? H47A C47 C48 108.8 . . ? H47B C47 C48 108.8 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N3 C49 H49A 108.7 . . ? N3 C49 H49B 108.7 . . ? N3 C49 C50 114.2(4) . . ? H49A C49 H49B 107.6 . . ? H49A C49 C50 108.7 . . ? H49B C49 C50 108.7 . . ? C49 C50 H50A 109.3 . . ? C49 C50 H50B 109.3 . . ? C49 C50 C51 111.4(4) . . ? H50A C50 H50B 108.0 . . ? H50A C50 C51 109.3 . . ? H50B C50 C51 109.3 . . ? C50 C51 H51A 109.6 . . ? C50 C51 H51B 109.6 . . ? C50 C51 C52 110.4(5) . . ? H51A C51 H51B 108.1 . . ? H51A C51 C52 109.6 . . ? H51B C51 C52 109.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N3 C53 H53A 108.4 . . ? N3 C53 H53B 108.4 . . ? N3 C53 C54 115.4(4) . . ? H53A C53 H53B 107.5 . . ? H53A C53 C54 108.4 . . ? H53B C53 C54 108.4 . . ? C53 C54 H54A 109.4 . . ? C53 C54 H54B 109.4 . . ? C53 C54 C55 111.0(5) . . ? H54A C54 H54B 108.0 . . ? H54A C54 C55 109.4 . . ? H54B C54 C55 109.4 . . ? C54 C55 H55A 108.9 . . ? C54 C55 H55B 108.9 . . ? C54 C55 C56 113.3(5) . . ? H55A C55 H55B 107.7 . . ? H55A C55 C56 108.9 . . ? H55B C55 C56 108.9 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C57 N4 C61 110.6(4) . . ? C57 N4 C65 106.7(4) . . ? C57 N4 C69 110.7(4) . . ? C61 N4 C65 111.5(4) . . ? C61 N4 C69 106.7(4) . . ? C65 N4 C69 110.7(4) . . ? N4 C57 H57A 108.4 . . ? N4 C57 H57B 108.4 . . ? N4 C57 C58 115.6(4) . . ? H57A C57 H57B 107.4 . . ? H57A C57 C58 108.4 . . ? H57B C57 C58 108.4 . . ? C57 C58 H58A 110.7 . . ? C57 C58 H58B 110.7 . . ? C57 C58 H58C 108.8 . . ? C57 C58 H58D 108.8 . . ? C57 C58 C59X 105.1(9) . . ? C57 C58 C59Y 113.7(7) . . ? H58A C58 H58B 108.8 . . ? H58A C58 C59X 110.7 . . ? H58B C58 C59X 110.7 . . ? H58C C58 H58D 107.7 . . ? H58C C58 C59Y 108.8 . . ? H58D C58 C59Y 108.8 . . ? C58 C59X H59A 109.9 . . ? C58 C59X H59B 109.9 . . ? C58 C59X C60X 108.8(13) . . ? H59A C59X H59B 108.3 . . ? H59A C59X C60X 109.9 . . ? H59B C59X C60X 109.9 . . ? C59X C60X H60A 109.5 . . ? C59X C60X H60B 109.5 . . ? C59X C60X H60C 109.5 . . ? H60A C60X H60B 109.5 . . ? H60A C60X H60C 109.5 . . ? H60B C60X H60C 109.5 . . ? C58 C59Y H59C 110.4 . . ? C58 C59Y H59D 110.4 . . ? C58 C59Y C60Y 106.7(9) . . ? H59C C59Y H59D 108.6 . . ? H59C C59Y C60Y 110.4 . . ? H59D C59Y C60Y 110.4 . . ? C59Y C60Y H60D 109.5 . . ? C59Y C60Y H60E 109.5 . . ? C59Y C60Y H60F 109.5 . . ? H60D C60Y H60E 109.5 . . ? H60D C60Y H60F 109.5 . . ? H60E C60Y H60F 109.5 . . ? N4 C61 H61A 108.5 . . ? N4 C61 H61B 108.5 . . ? N4 C61 C62 115.1(4) . . ? H61A C61 H61B 107.5 . . ? H61A C61 C62 108.5 . . ? H61B C61 C62 108.5 . . ? C61 C62 H62A 109.1 . . ? C61 C62 H62B 109.1 . . ? C61 C62 C63 112.3(5) . . ? H62A C62 H62B 107.9 . . ? H62A C62 C63 109.1 . . ? H62B C62 C63 109.1 . . ? C62 C63 H63A 108.8 . . ? C62 C63 H63B 108.8 . . ? C62 C63 C64 113.7(5) . . ? H63A C63 H63B 107.7 . . ? H63A C63 C64 108.8 . . ? H63B C63 C64 108.8 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N4 C65 H65A 108.5 . . ? N4 C65 H65B 108.5 . . ? N4 C65 C66 115.1(4) . . ? H65A C65 H65B 107.5 . . ? H65A C65 C66 108.5 . . ? H65B C65 C66 108.5 . . ? C65 C66 H66A 109.3 . . ? C65 C66 H66B 109.3 . . ? C65 C66 C67 111.8(5) . . ? H66A C66 H66B 107.9 . . ? H66A C66 C67 109.3 . . ? H66B C66 C67 109.3 . . ? C66 C67 H67A 109.2 . . ? C66 C67 H67B 109.2 . . ? C66 C67 C68 112.0(5) . . ? H67A C67 H67B 107.9 . . ? H67A C67 C68 109.2 . . ? H67B C67 C68 109.2 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68B 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N4 C69 H69A 108.3 . . ? N4 C69 H69B 108.3 . . ? N4 C69 C70 115.7(4) . . ? H69A C69 H69B 107.4 . . ? H69A C69 C70 108.3 . . ? H69B C69 C70 108.3 . . ? C69 C70 H70A 109.1 . . ? C69 C70 H70B 109.1 . . ? C69 C70 C71 112.5(5) . . ? H70A C70 H70B 107.8 . . ? H70A C70 C71 109.1 . . ? H70B C70 C71 109.1 . . ? C70 C71 H71A 108.5 . . ? C70 C71 H71B 108.5 . . ? C70 C71 C72 114.9(5) . . ? H71A C71 H71B 107.5 . . ? H71A C71 C72 108.5 . . ? H71B C71 C72 108.5 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72B 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C73 N5 C77 110.8(5) . . ? C73 N5 C81 107.2(4) . . ? C73 N5 C85 111.0(5) . . ? C77 N5 C81 110.7(5) . . ? C77 N5 C85 106.5(4) . . ? C81 N5 C85 110.6(4) . . ? N5 C73 H73A 105.2 . . ? N5 C73 H73B 105.2 . . ? N5 C73 H73C 110.5 . . ? N5 C73 H73D 110.5 . . ? N5 C73 C74X 128.3(8) . . ? N5 C73 C74Y 106.2(6) . . ? H73A C73 H73B 105.9 . . ? H73A C73 C74X 105.2 . . ? H73B C73 C74X 105.2 . . ? H73C C73 H73D 108.7 . . ? H73C C73 C74Y 110.5 . . ? H73D C73 C74Y 110.5 . . ? C73 C74X H74A 108.1 . . ? C73 C74X H74B 108.1 . . ? C73 C74X C75X 116.7(11) . . ? H74A C74X H74B 107.3 . . ? H74A C74X C75X 108.1 . . ? H74B C74X C75X 108.1 . . ? C74X C75X H75A 109.4 . . ? C74X C75X H75B 109.4 . . ? C74X C75X C76X 111.1(13) . . ? H75A C75X H75B 108.0 . . ? H75A C75X C76X 109.4 . . ? H75B C75X C76X 109.4 . . ? C75X C76X H76A 109.5 . . ? C75X C76X H76B 109.5 . . ? C75X C76X H76C 109.5 . . ? H76A C76X H76B 109.5 . . ? H76A C76X H76C 109.5 . . ? H76B C76X H76C 109.5 . . ? C73 C74Y H74C 110.2 . . ? C73 C74Y H74D 110.2 . . ? C73 C74Y C75Y 107.6(9) . . ? H74C C74Y H74D 108.5 . . ? H74C C74Y C75Y 110.2 . . ? H74D C74Y C75Y 110.2 . . ? C74Y C75Y H75C 108.9 . . ? C74Y C75Y H75D 108.9 . . ? C74Y C75Y C76Y 113.4(12) . . ? H75C C75Y H75D 107.7 . . ? H75C C75Y C76Y 108.9 . . ? H75D C75Y C76Y 108.9 . . ? C75Y C76Y H76D 109.5 . . ? C75Y C76Y H76E 109.5 . . ? C75Y C76Y H76F 109.5 . . ? H76D C76Y H76E 109.5 . . ? H76D C76Y H76F 109.5 . . ? H76E C76Y H76F 109.5 . . ? N5 C77 H77A 108.2 . . ? N5 C77 H77B 108.2 . . ? N5 C77 C78 116.2(5) . . ? H77A C77 H77B 107.4 . . ? H77A C77 C78 108.2 . . ? H77B C77 C78 108.2 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? C77 C78 H78C 108.2 . . ? C77 C78 H78D 108.2 . . ? C77 C78 C79X 110.5(6) . . ? C77 C78 C79Y 116.2(8) . . ? H78A C78 H78B 108.1 . . ? H78A C78 C79X 109.5 . . ? H78B C78 C79X 109.5 . . ? H78C C78 H78D 107.4 . . ? H78C C78 C79Y 108.2 . . ? H78D C78 C79Y 108.2 . . ? C78 C79X H79A 108.0 . . ? C78 C79X H79B 108.0 . . ? C78 C79X C80 117.2(7) . . ? H79A C79X H79B 107.3 . . ? H79A C79X C80 108.0 . . ? H79B C79X C80 108.0 . . ? C78 C79Y H79C 108.0 . . ? C78 C79Y H79D 108.0 . . ? C78 C79Y C80 117.3(10) . . ? H79C C79Y H79D 107.2 . . ? H79C C79Y C80 108.0 . . ? H79D C79Y C80 108.0 . . ? C79X C80 H80A 109.5 . . ? C79X C80 H80B 109.5 . . ? C79X C80 H80C 109.5 . . ? C79Y C80 H80D 109.5 . . ? C79Y C80 H80E 109.5 . . ? C79Y C80 H80F 109.5 . . ? H80A C80 H80B 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? H80D C80 H80E 109.5 . . ? H80D C80 H80F 109.5 . . ? H80E C80 H80F 109.5 . . ? N5 C81 H81A 108.3 . . ? N5 C81 H81B 108.3 . . ? N5 C81 C82 116.1(5) . . ? H81A C81 H81B 107.4 . . ? H81A C81 C82 108.3 . . ? H81B C81 C82 108.3 . . ? C81 C82 H82A 109.3 . . ? C81 C82 H82B 109.3 . . ? C81 C82 C83 111.7(5) . . ? H82A C82 H82B 107.9 . . ? H82A C82 C83 109.3 . . ? H82B C82 C83 109.3 . . ? C82 C83 H83A 109.0 . . ? C82 C83 H83B 109.0 . . ? C82 C83 C84 112.9(5) . . ? H83A C83 H83B 107.8 . . ? H83A C83 C84 109.0 . . ? H83B C83 C84 109.0 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84B 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N5 C85 H85A 108.6 . . ? N5 C85 H85B 108.6 . . ? N5 C85 C86 114.7(4) . . ? H85A C85 H85B 107.6 . . ? H85A C85 C86 108.6 . . ? H85B C85 C86 108.6 . . ? C85 C86 H86A 109.6 . . ? C85 C86 H86B 109.6 . . ? C85 C86 C87 110.4(4) . . ? H86A C86 H86B 108.1 . . ? H86A C86 C87 109.6 . . ? H86B C86 C87 109.6 . . ? C86 C87 H87A 109.3 . . ? C86 C87 H87B 109.3 . . ? C86 C87 C88 111.8(5) . . ? H87A C87 H87B 107.9 . . ? H87A C87 C88 109.3 . . ? H87B C87 C88 109.3 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88B 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C89 N6 C93 111.2(4) . . ? C89 N6 C97 106.5(4) . . ? C89 N6 C101 111.7(4) . . ? C93 N6 C97 110.8(4) . . ? C93 N6 C101 106.0(4) . . ? C97 N6 C101 110.7(4) . . ? N6 C89 H89A 108.3 . . ? N6 C89 H89B 108.3 . . ? N6 C89 C90 115.8(5) . . ? H89A C89 H89B 107.4 . . ? H89A C89 C90 108.3 . . ? H89B C89 C90 108.3 . . ? C89 C90 H90A 109.4 . . ? C89 C90 H90B 109.4 . . ? C89 C90 C91 111.0(5) . . ? H90A C90 H90B 108.0 . . ? H90A C90 C91 109.4 . . ? H90B C90 C91 109.4 . . ? C90 C91 H91A 108.8 . . ? C90 C91 H91B 108.8 . . ? C90 C91 C92 113.8(6) . . ? H91A C91 H91B 107.7 . . ? H91A C91 C92 108.8 . . ? H91B C91 C92 108.8 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92B 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? N6 C93 H93A 108.7 . . ? N6 C93 H93B 108.7 . . ? N6 C93 C94 114.4(4) . . ? H93A C93 H93B 107.6 . . ? H93A C93 C94 108.7 . . ? H93B C93 C94 108.7 . . ? C93 C94 H94A 109.2 . . ? C93 C94 H94B 109.2 . . ? C93 C94 C95 112.2(5) . . ? H94A C94 H94B 107.9 . . ? H94A C94 C95 109.2 . . ? H94B C94 C95 109.2 . . ? C94 C95 H95A 109.4 . . ? C94 C95 H95B 109.4 . . ? C94 C95 C96 111.3(5) . . ? H95A C95 H95B 108.0 . . ? H95A C95 C96 109.4 . . ? H95B C95 C96 109.4 . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96B 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? N6 C97 H97A 108.3 . . ? N6 C97 H97B 108.3 . . ? N6 C97 C98 116.1(4) . . ? H97A C97 H97B 107.4 . . ? H97A C97 C98 108.3 . . ? H97B C97 C98 108.3 . . ? C97 C98 H98A 109.4 . . ? C97 C98 H98B 109.4 . . ? C97 C98 C99 111.0(5) . . ? H98A C98 H98B 108.0 . . ? H98A C98 C99 109.4 . . ? H98B C98 C99 109.4 . . ? C98 C99 H99A 108.8 . . ? C98 C99 H99B 108.8 . . ? C98 C99 C100 113.9(5) . . ? H99A C99 H99B 107.7 . . ? H99A C99 C100 108.8 . . ? H99B C99 C100 108.8 . . ? C99 C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? C99 C100 H10E 109.5 . . ? H10C C100 H10D 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? N6 C101 H10F 108.3 . . ? N6 C101 H10G 108.3 . . ? N6 C101 C102 116.0(4) . . ? H10F C101 H10G 107.4 . . ? H10F C101 C102 108.3 . . ? H10G C101 C102 108.3 . . ? C101 C102 H10H 109.6 . . ? C101 C102 H10I 109.6 . . ? C101 C102 C103 110.1(4) . . ? H10H C102 H10I 108.2 . . ? H10H C102 C103 109.6 . . ? H10I C102 C103 109.6 . . ? C102 C103 H10J 109.1 . . ? C102 C103 H10K 109.1 . . ? C102 C103 C104 112.5(5) . . ? H10J C103 H10K 107.8 . . ? H10J C103 C104 109.1 . . ? H10K C103 C104 109.1 . . ? C103 C104 H10L 109.5 . . ? C103 C104 H10M 109.5 . . ? C103 C104 H10N 109.5 . . ? H10L C104 H10M 109.5 . . ? H10L C104 H10N 109.5 . . ? H10M C104 H10N 109.5 . . ? N7 C105 C106 178.3(9) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.378 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.125 # Contents of RES file _computing_special_details ; TITL rje479 in P2(1)/c CELL 0.71073 24.9233 33.6182 16.8302 90.0000 90.915 90.0000 ZERR 8 0.0005 0.0008 0.0003 0.0000 0.002 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Ti Mo UNIT 424 948 28 152 8 40 TEMP -123 REM colourless block SIZE 0.22 0.20 0.15 L.S. 8 BOND $H LIST 4 ACTA 52 FMAP 2 PLAN 10 CONN 6 $TI $MO rem OMIT -26 10 5 rem OMIT -25 12 5 SIMU N1 > C106 DELU N1 > C106 rem EXTI 0.000000 WGHT 0.011400 78.607803 FVAR 0.05501 0.30044 0.39247 0.40768 0.64140 MO1 6 0.309211 0.386580 0.448628 11.00000 0.03295 0.02120 = 0.01757 -0.00086 -0.00042 -0.00009 MO2 6 0.221929 0.420244 0.316645 11.00000 0.01837 0.02019 = 0.02668 -0.00372 0.00217 0.00302 MO3 6 0.291322 0.379875 0.172873 11.00000 0.04329 0.02619 = 0.01638 -0.00107 0.00271 0.00964 MO4 6 0.379601 0.346499 0.304691 11.00000 0.01964 0.01974 = 0.03268 0.00251 0.00568 0.00521 MO5 6 0.251300 0.324191 0.322152 11.00000 0.02280 0.01787 = 0.02971 -0.00287 0.00120 -0.00233 TI1 5 0.346198 0.437905 0.299991 11.00000 0.01822 0.01800 = 0.03551 0.00305 0.00370 -0.00080 O1 4 0.383996 0.482916 0.291184 11.00000 0.02167 0.02552 = 0.06092 0.00772 0.00349 -0.00534 O2 4 0.318059 0.385497 0.549175 11.00000 0.06528 0.03416 = 0.01967 -0.00152 -0.00604 0.00076 O3 4 0.164828 0.446940 0.329393 11.00000 0.02443 0.03255 = 0.04616 -0.00853 0.00274 0.00896 O4 4 0.280598 0.378273 0.073400 11.00000 0.08945 0.05091 = 0.01806 -0.00368 0.00350 0.02460 O5 4 0.435354 0.317948 0.293421 11.00000 0.03093 0.02702 = 0.05497 0.00492 0.01016 0.01135 O6 4 0.213674 0.282451 0.328704 11.00000 0.02990 0.02795 = 0.05712 -0.00039 -0.00042 -0.00759 O7 4 0.349947 0.428905 0.415956 11.00000 0.02767 0.02024 = 0.03476 -0.00370 -0.00747 -0.00289 O8 4 0.274923 0.458894 0.314144 11.00000 0.02254 0.01750 = 0.02869 -0.00169 0.00300 0.00391 O9 4 0.327764 0.427511 0.189388 11.00000 0.04163 0.02783 = 0.02559 0.00855 0.01327 0.00393 O10 4 0.403891 0.397891 0.291246 11.00000 0.02093 0.02251 = 0.05363 0.00536 0.00919 0.00177 O11 4 0.372727 0.352334 0.414101 11.00000 0.03093 0.02112 = 0.03080 0.00582 -0.00613 0.00058 O12 4 0.244266 0.412730 0.433215 11.00000 0.03281 0.02318 = 0.02153 -0.00292 0.00653 0.00157 O13 4 0.225374 0.411046 0.207973 11.00000 0.04133 0.02455 = 0.02533 -0.00018 -0.00586 0.00722 O14 4 0.353576 0.349751 0.189943 11.00000 0.04236 0.02781 = 0.02958 0.00018 0.01493 0.01040 O15 4 0.271021 0.336080 0.429266 11.00000 0.03719 0.02094 = 0.02097 0.00369 0.00554 -0.00130 O16 4 0.198242 0.365594 0.330001 11.00000 0.01756 0.02744 = 0.04402 -0.00264 0.00571 -0.00254 O17 4 0.249298 0.335137 0.209874 11.00000 0.04161 0.02770 = 0.02760 -0.00803 -0.00627 0.00234 O18 4 0.322613 0.305795 0.308615 11.00000 0.02170 0.01810 = 0.03208 -0.00353 0.00342 0.00426 O19 4 0.301027 0.383561 0.311013 11.00000 0.01579 0.01572 = 0.01997 -0.00009 0.00089 -0.00204 C1 1 0.430633 0.506586 0.298194 11.00000 0.02575 0.03607 = 0.04249 0.00478 -0.00286 -0.00848 C2 1 0.414283 0.549317 0.306575 11.00000 0.06981 0.03684 = 0.07510 0.00099 0.00360 -0.01592 AFIX 33 H2A 2 0.394202 0.552694 0.355709 11.00000 -1.50000 H2B 2 0.391592 0.557011 0.261031 11.00000 -1.50000 H2C 2 0.446374 0.566157 0.308458 11.00000 -1.50000 AFIX 0 C3 1 0.461919 0.501088 0.222387 11.00000 0.03162 0.08892 = 0.05201 0.00921 0.00323 -0.00921 AFIX 33 H3A 2 0.472031 0.473066 0.216862 11.00000 -1.50000 H3B 2 0.494356 0.517552 0.224644 11.00000 -1.50000 H3C 2 0.439577 0.509095 0.176687 11.00000 -1.50000 AFIX 0 C4 1 0.462145 0.492132 0.370412 11.00000 0.04329 0.07595 = 0.05216 0.01458 0.00012 -0.00776 AFIX 33 H4A 2 0.472287 0.464242 0.362813 11.00000 -1.50000 H4B 2 0.439941 0.494483 0.417716 11.00000 -1.50000 H4C 2 0.494571 0.508331 0.377376 11.00000 -1.50000 AFIX 0 MO6 6 0.892670 0.400886 0.282968 11.00000 0.02350 0.02787 = 0.03695 -0.01021 0.01130 -0.00810 MO7 6 0.786782 0.437746 0.187181 11.00000 0.04766 0.01639 = 0.02552 0.00493 0.01703 0.01008 MO8 6 0.746917 0.347246 0.142831 11.00000 0.02135 0.02664 = 0.02287 -0.00110 0.00164 0.00631 MO9 6 0.852283 0.310189 0.237770 11.00000 0.01911 0.01759 = 0.02367 -0.00010 0.00390 0.00571 MO10 6 0.770987 0.372065 0.330081 11.00000 0.02024 0.01694 = 0.02032 0.00233 0.00777 0.00322 TI2 5 0.865198 0.375920 0.104150 11.00000 0.03360 0.01972 = 0.02862 -0.00099 0.01875 0.00109 O20 4 0.904016 0.381500 0.016473 11.00000 0.05435 0.02902 = 0.03619 -0.00116 0.03229 -0.00187 O21 4 0.942999 0.422907 0.335871 11.00000 0.04083 0.05043 = 0.05294 -0.01800 0.00975 -0.02094 O22 4 0.758775 0.483297 0.171330 11.00000 0.07946 0.02062 = 0.03613 0.01070 0.02554 0.02222 O23 4 0.692848 0.325620 0.097984 11.00000 0.02575 0.04095 = 0.03257 -0.00720 -0.00633 0.00694 O24 4 0.877395 0.264450 0.259505 11.00000 0.02982 0.02295 = 0.03516 0.00138 0.00258 0.01006 O25 4 0.735567 0.369288 0.415302 11.00000 0.03035 0.02322 = 0.02318 0.00349 0.01067 0.00484 O26 4 0.915488 0.401174 0.179871 11.00000 0.02797 0.02977 = 0.04234 -0.00254 0.02047 -0.00331 O27 4 0.826349 0.427918 0.098939 11.00000 0.05297 0.02450 = 0.02670 0.00967 0.01945 0.00729 O28 4 0.798205 0.351461 0.065143 11.00000 0.03324 0.02851 = 0.02062 -0.00401 0.00817 0.00369 O29 4 0.887505 0.324825 0.145408 11.00000 0.02854 0.01908 = 0.02978 -0.00381 0.01215 0.00306 O30 4 0.905933 0.346137 0.294385 11.00000 0.01869 0.02673 = 0.03091 -0.00147 0.00217 0.00120 O31 4 0.847265 0.448561 0.251121 11.00000 0.04089 0.01834 = 0.03629 -0.00206 0.01739 -0.00637 O32 4 0.730287 0.401787 0.138706 11.00000 0.03317 0.03017 = 0.02554 0.00451 0.00442 0.01371 O33 4 0.788751 0.299020 0.180930 11.00000 0.01997 0.01708 = 0.02427 -0.00159 0.00194 0.00000 O34 4 0.837129 0.395482 0.362698 11.00000 0.02965 0.02633 = 0.02256 -0.00619 0.00637 -0.00516 O35 4 0.750568 0.421580 0.286271 11.00000 0.03375 0.01756 = 0.02374 0.00329 0.01351 0.00942 O36 4 0.723780 0.347647 0.253657 11.00000 0.01912 0.02688 = 0.02844 -0.00258 0.00623 0.00295 O37 4 0.809673 0.321778 0.329534 11.00000 0.02573 0.01998 = 0.02012 0.00533 0.00426 0.00267 O38 4 0.819866 0.374152 0.211604 11.00000 0.02256 0.01681 = 0.02139 0.00403 0.00795 0.00203 C5 1 0.936976 0.405612 -0.033206 11.00000 0.03062 0.03256 = 0.02621 0.00849 0.01287 0.00149 C6 1 0.992677 0.388315 -0.031336 11.00000 0.04358 0.05798 = 0.05842 0.01285 0.00847 0.01673 AFIX 33 H6A 2 1.007514 0.389852 0.022853 11.00000 -1.50000 H6B 2 1.015571 0.403384 -0.067337 11.00000 -1.50000 H6C 2 0.991215 0.360445 -0.048305 11.00000 -1.50000 AFIX 0 C7 1 0.914324 0.403131 -0.116382 11.00000 0.05285 0.06658 = 0.03846 0.00842 0.00213 0.00035 AFIX 33 H7A 2 0.878076 0.414431 -0.117789 11.00000 -1.50000 H7B 2 0.912834 0.375233 -0.133159 11.00000 -1.50000 H7C 2 0.937298 0.418111 -0.152418 11.00000 -1.50000 AFIX 0 C8 1 0.936715 0.447868 -0.002340 11.00000 0.05263 0.03016 = 0.05044 0.00590 0.01758 -0.00512 AFIX 33 H8A 2 0.951872 0.448430 0.051737 11.00000 -1.50000 H8B 2 0.899771 0.457833 -0.001816 11.00000 -1.50000 H8C 2 0.958334 0.464718 -0.036944 11.00000 -1.50000 AFIX 0 SAME N1 C9 C10 C11 C12Y SAME N1 C13 > C16 SAME N1 C17 > C20 SAME N1 C21 > C24 SAME N2 > C28 SAME N2 C29 > C32 SAME N2 C33 > C36 SAME N2 C37 > C40 SAME N3 > C44 SAME N3 C45 > C48 SAME N3 C49 > C52 SAME N3 C53 > C56 SAME N4 > C60X SAME N4 C57 C58 C59Y C60Y SAME N4 C61 > C64 SAME N4 C65 > C68 SAME N4 C69 > C72 SAME N5 > C76X SAME N5 C73 C74Y C75Y C76Y SAME N5 C77 C78 C79X C80 SAME N5 C77 C78 C79Y C80 SAME N5 C81 > C84 SAME N5 C85 > C88 SAME N6 > C92 SAME N6 C93 > C96 SAME N6 C97 > C100 SAME N6 C101 > C104 N1 3 0.280472 0.525889 0.078356 11.00000 0.03286 0.03274 = 0.02936 0.01040 -0.00420 0.00272 C9 1 0.329640 0.500555 0.065245 11.00000 0.02949 0.04462 = 0.04260 0.00904 -0.00126 0.00518 AFIX 23 H9A 2 0.321052 0.472859 0.080464 11.00000 -1.20000 H9B 2 0.358536 0.509966 0.101649 11.00000 -1.20000 AFIX 0 C10 1 0.351215 0.500137 -0.018551 11.00000 0.04406 0.06228 = 0.05635 0.00966 0.00971 -0.00075 AFIX 23 H10A 2 0.322619 0.491986 -0.056672 11.00000 -1.20000 H10B 2 0.363683 0.527057 -0.033354 11.00000 -1.20000 AFIX 0 C11 1 0.397502 0.470939 -0.021101 11.00000 0.04358 0.11761 = 0.08726 -0.01557 0.01052 0.01936 PART 1 AFIX 23 H11A 2 0.395192 0.451767 0.023362 21.00000 -1.20000 H11B 2 0.396565 0.455938 -0.071723 21.00000 -1.20000 AFIX 23 PART 2 H11C 2 0.422705 0.477638 0.022952 -21.00000 -1.20000 H11D 2 0.383059 0.444107 -0.010036 -21.00000 -1.20000 AFIX 0 PART 1 C12X 1 0.448733 0.494890 -0.014076 21.00000 0.05359 0.09969 = 0.06201 0.00904 0.00488 0.01149 AFIX 33 H12A 2 0.479605 0.476833 -0.012925 21.00000 -1.50000 H12B 2 0.448398 0.510550 0.035027 21.00000 -1.50000 H12C 2 0.451390 0.512805 -0.059779 21.00000 -1.50000 AFIX 0 PART 2 C12Y 1 0.428065 0.468561 -0.093334 -21.00000 0.07272 0.13627 = 0.05562 0.01624 0.01435 0.03403 AFIX 33 H12D 2 0.457358 0.449387 -0.086120 -21.00000 -1.50000 H12E 2 0.442984 0.494786 -0.105565 -21.00000 -1.50000 H12F 2 0.404550 0.459898 -0.137236 -21.00000 -1.50000 AFIX 0 PART 0 C13 1 0.290012 0.568826 0.054019 11.00000 0.04944 0.03708 = 0.03845 0.01873 -0.00991 -0.00592 AFIX 23 H13A 2 0.296827 0.569559 -0.003752 11.00000 -1.20000 H13B 2 0.256849 0.584211 0.063460 11.00000 -1.20000 AFIX 0 C14 1 0.336250 0.589138 0.097151 11.00000 0.07504 0.04415 = 0.07015 0.02291 -0.03195 -0.01687 AFIX 23 H14A 2 0.368596 0.572128 0.094473 11.00000 -1.20000 H14B 2 0.327233 0.592581 0.153811 11.00000 -1.20000 AFIX 0 C15 1 0.348231 0.629363 0.061022 11.00000 0.07108 0.05842 = 0.11611 0.04496 -0.04371 -0.02755 AFIX 23 H15A 2 0.316453 0.646786 0.066194 11.00000 -1.20000 H15B 2 0.355317 0.626038 0.003693 11.00000 -1.20000 AFIX 0 C16 1 0.396229 0.649039 0.100961 11.00000 0.12052 0.06992 = 0.18420 0.05099 -0.07892 -0.05385 AFIX 33 H16A 2 0.403329 0.674600 0.075184 11.00000 -1.50000 H16B 2 0.427706 0.631776 0.096290 11.00000 -1.50000 H16C 2 0.388705 0.653470 0.157246 11.00000 -1.50000 AFIX 0 C17 1 0.268661 0.522364 0.166723 11.00000 0.04644 0.02880 = 0.02879 0.00813 -0.00424 0.00179 AFIX 23 H17A 2 0.266286 0.493802 0.180549 11.00000 -1.20000 H17B 2 0.299257 0.533745 0.197297 11.00000 -1.20000 AFIX 0 C18 1 0.217618 0.542788 0.192734 11.00000 0.04292 0.03401 = 0.04239 0.00460 0.00879 -0.00281 AFIX 23 H18A 2 0.186097 0.527087 0.174721 11.00000 -1.20000 H18B 2 0.215168 0.569468 0.168045 11.00000 -1.20000 AFIX 0 C19 1 0.217261 0.546856 0.283050 11.00000 0.08059 0.02988 = 0.04595 0.00421 0.01473 0.01352 AFIX 23 H19A 2 0.225274 0.520626 0.307203 11.00000 -1.20000 H19B 2 0.246075 0.565461 0.299819 11.00000 -1.20000 AFIX 0 C20 1 0.164650 0.561682 0.313924 11.00000 0.09330 0.04237 = 0.07006 -0.01735 0.03278 -0.00540 AFIX 33 H20A 2 0.166937 0.563983 0.371926 11.00000 -1.50000 H20B 2 0.136085 0.542924 0.299187 11.00000 -1.50000 H20C 2 0.156629 0.587806 0.290787 11.00000 -1.50000 AFIX 0 C21 1 0.233763 0.510908 0.027680 11.00000 0.03447 0.03407 = 0.03068 0.00607 -0.00361 0.00208 AFIX 23 H21A 2 0.201791 0.527164 0.039751 11.00000 -1.20000 H21B 2 0.242320 0.515415 -0.028850 11.00000 -1.20000 AFIX 0 C22 1 0.219299 0.467571 0.038067 11.00000 0.03688 0.03585 = 0.03575 0.00834 0.00039 -0.00250 AFIX 23 H22A 2 0.210476 0.462488 0.094307 11.00000 -1.20000 H22B 2 0.250439 0.450764 0.024417 11.00000 -1.20000 AFIX 0 C23 1 0.171788 0.456591 -0.014572 11.00000 0.04248 0.04731 = 0.05002 0.01109 -0.00730 -0.00806 AFIX 23 H23A 2 0.180025 0.463241 -0.070368 11.00000 -1.20000 H23B 2 0.140307 0.472571 0.001068 11.00000 -1.20000 AFIX 0 C24 1 0.157900 0.412835 -0.009104 11.00000 0.06108 0.04956 = 0.07685 0.01692 -0.02073 -0.02057 AFIX 33 H24A 2 0.126787 0.407138 -0.043586 11.00000 -1.50000 H24B 2 0.149360 0.406156 0.045946 11.00000 -1.50000 H24C 2 0.188565 0.396895 -0.026132 11.00000 -1.50000 AFIX 0 N2 3 0.817632 0.206877 0.049804 11.00000 0.02941 0.02086 = 0.02752 -0.00757 0.00195 0.00255 C25 1 0.854515 0.242198 0.037165 11.00000 0.03028 0.02505 = 0.02668 -0.00488 -0.00149 -0.00175 AFIX 23 H25A 2 0.836329 0.266527 0.056059 11.00000 -1.20000 H25B 2 0.887353 0.238491 0.070208 11.00000 -1.20000 AFIX 0 C26 1 0.870751 0.248513 -0.048213 11.00000 0.05165 0.04898 = 0.02839 -0.00192 0.00128 -0.01773 AFIX 23 H26A 2 0.838507 0.254932 -0.080854 11.00000 -1.20000 H26B 2 0.886377 0.223608 -0.069055 11.00000 -1.20000 AFIX 0 C27 1 0.911245 0.281814 -0.055484 11.00000 0.04208 0.03286 = 0.03694 0.00005 0.00377 -0.00625 AFIX 23 H27A 2 0.917210 0.287141 -0.112517 11.00000 -1.20000 H27B 2 0.896135 0.306251 -0.031819 11.00000 -1.20000 AFIX 0 C28 1 0.963862 0.273048 -0.016066 11.00000 0.04721 0.10758 = 0.09409 0.03794 -0.00835 -0.02386 AFIX 33 H28A 2 0.988102 0.295694 -0.022990 11.00000 -1.50000 H28B 2 0.979594 0.249269 -0.040022 11.00000 -1.50000 H28C 2 0.958507 0.268414 0.040746 11.00000 -1.50000 AFIX 0 C29 1 0.843249 0.168221 0.022902 11.00000 0.03485 0.02428 = 0.02790 -0.00799 0.00435 0.00598 AFIX 23 H29A 2 0.816667 0.146540 0.028213 11.00000 -1.20000 H29B 2 0.851769 0.170593 -0.034156 11.00000 -1.20000 AFIX 0 C30 1 0.893799 0.156582 0.067977 11.00000 0.03791 0.03185 = 0.03753 -0.00569 -0.00121 0.00856 AFIX 23 H30A 2 0.885032 0.150509 0.123845 11.00000 -1.20000 H30B 2 0.919466 0.179056 0.067903 11.00000 -1.20000 AFIX 0 C31 1 0.919454 0.120272 0.029839 11.00000 0.05332 0.04709 = 0.04582 -0.00493 0.00623 0.02310 AFIX 23 H31A 2 0.891771 0.099533 0.021191 11.00000 -1.20000 H31B 2 0.933702 0.127798 -0.022636 11.00000 -1.20000 AFIX 0 C32 1 0.964370 0.103526 0.080890 11.00000 0.06253 0.06848 = 0.07532 0.00336 0.00750 0.03780 AFIX 33 H32A 2 0.979535 0.080094 0.054872 11.00000 -1.50000 H32B 2 0.950355 0.095895 0.132786 11.00000 -1.50000 H32C 2 0.992387 0.123713 0.088163 11.00000 -1.50000 AFIX 0 C33 1 0.805611 0.205326 0.138059 11.00000 0.04887 0.02514 = 0.02373 -0.00476 0.00101 0.00801 AFIX 23 H33A 2 0.839999 0.202848 0.167908 11.00000 -1.20000 H33B 2 0.789088 0.230905 0.153510 11.00000 -1.20000 AFIX 0 C34 1 0.768904 0.171815 0.163392 11.00000 0.05607 0.04709 = 0.04658 0.00307 0.01557 -0.00309 AFIX 23 H34A 2 0.736007 0.172284 0.129652 11.00000 -1.20000 H34B 2 0.787178 0.146097 0.154392 11.00000 -1.20000 AFIX 0 C35 1 0.753277 0.174417 0.249086 11.00000 0.09373 0.06753 = 0.05178 -0.00001 0.02312 0.00095 AFIX 23 H35A 2 0.735099 0.200174 0.258069 11.00000 -1.20000 H35B 2 0.727267 0.152982 0.260459 11.00000 -1.20000 AFIX 0 C36 1 0.799827 0.170931 0.305701 11.00000 0.11563 0.08716 = 0.07135 -0.01361 -0.00354 -0.00372 AFIX 33 H36A 2 0.787119 0.173069 0.360339 11.00000 -1.50000 H36B 2 0.825530 0.192315 0.295452 11.00000 -1.50000 H36C 2 0.817367 0.145124 0.298445 11.00000 -1.50000 AFIX 0 C37 1 0.766479 0.211545 0.000505 11.00000 0.02615 0.02641 = 0.03097 -0.00710 0.00090 0.00356 AFIX 23 H37A 2 0.742941 0.188456 0.010828 11.00000 -1.20000 H37B 2 0.775835 0.210866 -0.056426 11.00000 -1.20000 AFIX 0 C38 1 0.735064 0.249418 0.016239 11.00000 0.03831 0.02992 = 0.04582 -0.01256 -0.00399 0.00756 AFIX 23 H38A 2 0.728947 0.252052 0.073977 11.00000 -1.20000 H38B 2 0.756153 0.272713 -0.001146 11.00000 -1.20000 AFIX 0 C39 1 0.681456 0.248771 -0.027936 11.00000 0.03165 0.03746 = 0.05117 -0.00325 -0.00290 -0.00057 AFIX 23 H39A 2 0.660546 0.225647 -0.009248 11.00000 -1.20000 H39B 2 0.661275 0.273101 -0.014082 11.00000 -1.20000 AFIX 0 C40 1 0.685404 0.246485 -0.115790 11.00000 0.06764 0.07283 = 0.04783 0.00402 -0.01210 0.01643 AFIX 33 H40A 2 0.649277 0.245863 -0.139614 11.00000 -1.50000 H40B 2 0.704798 0.222272 -0.130389 11.00000 -1.50000 H40C 2 0.704741 0.269811 -0.135328 11.00000 -1.50000 AFIX 0 N3 3 0.348340 0.264423 0.596082 11.00000 0.02566 0.02612 = 0.02267 0.00600 0.00147 -0.00380 C41 1 0.329227 0.225044 0.561138 11.00000 0.03579 0.02338 = 0.02953 0.00348 0.00537 -0.00027 AFIX 23 H41A 2 0.360132 0.206588 0.559205 11.00000 -1.20000 H41B 2 0.302512 0.213315 0.597202 11.00000 -1.20000 AFIX 0 C42 1 0.304384 0.228038 0.478774 11.00000 0.04318 0.03072 = 0.03051 0.00075 -0.00111 -0.00337 AFIX 23 H42A 2 0.270240 0.242968 0.481821 11.00000 -1.20000 H42B 2 0.328795 0.243232 0.444244 11.00000 -1.20000 AFIX 0 C43 1 0.293683 0.188514 0.442195 11.00000 0.10764 0.03541 = 0.05578 -0.00771 -0.02950 0.01024 AFIX 23 H43A 2 0.266757 0.174256 0.474108 11.00000 -1.20000 H43B 2 0.327160 0.172661 0.443452 11.00000 -1.20000 AFIX 0 C44 1 0.273354 0.191633 0.357185 11.00000 0.10961 0.04763 = 0.04190 -0.01167 -0.02291 0.01141 AFIX 33 H44A 2 0.266781 0.164908 0.335908 11.00000 -1.50000 H44B 2 0.300258 0.205104 0.324965 11.00000 -1.50000 H44C 2 0.239861 0.206905 0.355648 11.00000 -1.50000 AFIX 0 C45 1 0.302213 0.293472 0.600203 11.00000 0.02735 0.02377 = 0.02677 0.00052 -0.00258 -0.00204 AFIX 23 H45A 2 0.290689 0.300094 0.545213 11.00000 -1.20000 H45B 2 0.315636 0.318293 0.625156 11.00000 -1.20000 AFIX 0 C46 1 0.253471 0.279844 0.645116 11.00000 0.03352 0.03267 = 0.03013 0.00467 0.00310 -0.00351 AFIX 23 H46A 2 0.237005 0.256598 0.618091 11.00000 -1.20000 H46B 2 0.264172 0.271790 0.699685 11.00000 -1.20000 AFIX 0 C47 1 0.213459 0.313586 0.648343 11.00000 0.04211 0.03606 = 0.07403 -0.00038 0.01555 0.00263 AFIX 23 H47A 2 0.230927 0.336819 0.674003 11.00000 -1.20000 H47B 2 0.203367 0.321341 0.593360 11.00000 -1.20000 AFIX 0 C48 1 0.163483 0.303682 0.692559 11.00000 0.04568 0.06214 = 0.06704 0.00080 0.01557 0.00794 AFIX 33 H48A 2 0.139326 0.326684 0.691777 11.00000 -1.50000 H48B 2 0.172895 0.296925 0.747683 11.00000 -1.50000 H48C 2 0.145546 0.280959 0.667133 11.00000 -1.50000 AFIX 0 C49 1 0.372324 0.256072 0.677893 11.00000 0.02991 0.03781 = 0.01996 0.01230 -0.00017 -0.00499 AFIX 23 H49A 2 0.344013 0.244882 0.711912 11.00000 -1.20000 H49B 2 0.400672 0.235645 0.672793 11.00000 -1.20000 AFIX 0 C50 1 0.396152 0.292188 0.718713 11.00000 0.05617 0.04289 = 0.02407 0.00706 -0.00878 -0.00974 AFIX 23 H50A 2 0.367728 0.312350 0.726224 11.00000 -1.20000 H50B 2 0.423944 0.303982 0.684561 11.00000 -1.20000 AFIX 0 C51 1 0.421104 0.281462 0.799166 11.00000 0.04872 0.04696 = 0.02589 0.00464 -0.00545 -0.00366 AFIX 23 H51A 2 0.393700 0.268870 0.832883 11.00000 -1.20000 H51B 2 0.450519 0.262097 0.791676 11.00000 -1.20000 AFIX 0 C52 1 0.442976 0.318438 0.840233 11.00000 0.08681 0.06763 = 0.03753 -0.00280 -0.02231 -0.01423 AFIX 33 H52A 2 0.459267 0.311031 0.891509 11.00000 -1.50000 H52B 2 0.413643 0.337285 0.848862 11.00000 -1.50000 H52C 2 0.470127 0.330849 0.806819 11.00000 -1.50000 AFIX 0 C53 1 0.389515 0.283711 0.542672 11.00000 0.03251 0.03268 = 0.02698 0.00899 0.00209 -0.00727 AFIX 23 H53A 2 0.372146 0.289387 0.490588 11.00000 -1.20000 H53B 2 0.400271 0.309507 0.566408 11.00000 -1.20000 AFIX 0 C54 1 0.439670 0.259445 0.528626 11.00000 0.03372 0.04295 = 0.03883 0.00906 0.00828 -0.00519 AFIX 23 H54A 2 0.455875 0.251586 0.580371 11.00000 -1.20000 H54B 2 0.430022 0.234892 0.499230 11.00000 -1.20000 AFIX 0 C55 1 0.479863 0.282773 0.481993 11.00000 0.04022 0.05559 = 0.04334 0.00924 0.01269 -0.00907 AFIX 23 H55A 2 0.488433 0.307661 0.510962 11.00000 -1.20000 H55B 2 0.463532 0.290178 0.430064 11.00000 -1.20000 AFIX 0 C56 1 0.531072 0.260372 0.467851 11.00000 0.03698 0.07885 = 0.04558 0.00121 0.00766 -0.00791 AFIX 33 H56A 2 0.555614 0.277098 0.437547 11.00000 -1.50000 H56B 2 0.523082 0.236058 0.437799 11.00000 -1.50000 H56C 2 0.547884 0.253366 0.518994 11.00000 -1.50000 AFIX 0 N4 3 0.061920 0.322774 0.231037 11.00000 0.01605 0.03315 = 0.03262 -0.00249 -0.00387 0.00164 C57 1 0.083477 0.323700 0.316028 11.00000 0.03589 0.04420 = 0.03493 -0.00239 -0.01118 -0.00308 AFIX 23 H57A 2 0.099582 0.297455 0.328381 11.00000 -1.20000 H57B 2 0.112555 0.343720 0.319407 11.00000 -1.20000 AFIX 0 C58 1 0.042574 0.333227 0.379196 11.00000 0.06809 0.08548 = 0.03403 -0.01100 -0.00528 0.01364 PART 1 AFIX 23 H58A 2 0.018847 0.310124 0.388450 31.00000 -1.20000 H58B 2 0.020229 0.356286 0.363055 31.00000 -1.20000 AFIX 23 PART 2 H58C 2 0.008208 0.320108 0.364815 -31.00000 -1.20000 H58D 2 0.036226 0.362295 0.379650 -31.00000 -1.20000 AFIX 0 PART 1 C59X 1 0.076267 0.343031 0.455022 31.00000 0.07889 0.06869 = 0.04099 -0.01240 -0.00517 -0.01429 AFIX 23 H59A 2 0.105007 0.362178 0.442049 31.00000 -1.20000 H59B 2 0.053092 0.355250 0.495546 31.00000 -1.20000 AFIX 0 C60X 1 0.100361 0.305435 0.486712 31.00000 0.12436 0.11112 = 0.05982 0.00428 -0.03478 0.01504 AFIX 33 H60A 2 0.080742 0.296893 0.533741 31.00000 -1.50000 H60B 2 0.138072 0.310066 0.501284 31.00000 -1.50000 H60C 2 0.098072 0.284686 0.445898 31.00000 -1.50000 AFIX 0 PART 2 C59Y 1 0.059802 0.319896 0.463255 -31.00000 0.08105 0.03726 = 0.04036 -0.00374 0.00026 -0.00584 AFIX 23 H59C 2 0.029500 0.322460 0.500232 -31.00000 -1.20000 H59D 2 0.071614 0.291782 0.462707 -31.00000 -1.20000 AFIX 0 C60Y 1 0.104886 0.346270 0.488577 -31.00000 0.07107 0.09165 = 0.05748 -0.00103 -0.01749 -0.01804 AFIX 33 H60D 2 0.116922 0.338951 0.542333 -31.00000 -1.50000 H60E 2 0.092734 0.373994 0.488291 -31.00000 -1.50000 H60F 2 0.134689 0.343232 0.451779 -31.00000 -1.50000 AFIX 0 PART 0 C61 1 0.017921 0.291518 0.221926 11.00000 0.01892 0.03590 = 0.03526 0.00126 -0.00309 -0.00342 AFIX 23 H61A 2 -0.013523 0.300245 0.252625 11.00000 -1.20000 H61B 2 0.006692 0.290291 0.165289 11.00000 -1.20000 AFIX 0 C62 1 0.033469 0.250082 0.248880 11.00000 0.03121 0.04077 = 0.06501 0.00328 -0.00691 -0.00209 AFIX 23 H62A 2 0.069166 0.243396 0.227636 11.00000 -1.20000 H62B 2 0.036298 0.249605 0.307613 11.00000 -1.20000 AFIX 0 C63 1 -0.006550 0.219145 0.221715 11.00000 0.03197 0.03734 = 0.05975 -0.00136 0.00403 -0.00311 AFIX 23 H63A 2 -0.042734 0.227266 0.238924 11.00000 -1.20000 H63B 2 -0.007061 0.218235 0.162913 11.00000 -1.20000 AFIX 0 C64 1 0.005153 0.178128 0.253132 11.00000 0.05328 0.03787 = 0.08071 0.00063 0.01062 -0.00482 AFIX 33 H64A 2 -0.022133 0.159544 0.232989 11.00000 -1.50000 H64B 2 0.004584 0.178520 0.311336 11.00000 -1.50000 H64C 2 0.040635 0.169588 0.235548 11.00000 -1.50000 AFIX 0 C65 1 0.109229 0.313633 0.178315 11.00000 0.02090 0.03529 = 0.04035 0.00149 0.00358 -0.00155 AFIX 23 H65A 2 0.137096 0.334185 0.187485 11.00000 -1.20000 H65B 2 0.124708 0.287739 0.194788 11.00000 -1.20000 AFIX 0 C66 1 0.096301 0.311931 0.090253 11.00000 0.03814 0.05367 = 0.04365 -0.00570 0.00875 0.00997 AFIX 23 H66A 2 0.067566 0.292107 0.080524 11.00000 -1.20000 H66B 2 0.082758 0.338188 0.072408 11.00000 -1.20000 AFIX 0 C67 1 0.144911 0.300863 0.042338 11.00000 0.04094 0.07145 = 0.05392 0.00433 0.02070 0.01217 AFIX 23 H67A 2 0.173872 0.320404 0.052908 11.00000 -1.20000 H67B 2 0.158039 0.274389 0.059556 11.00000 -1.20000 AFIX 0 C68 1 0.132463 0.299855 -0.045848 11.00000 0.08362 0.09589 = 0.04965 -0.00020 0.03336 0.01028 AFIX 33 H68A 2 0.164990 0.292884 -0.074696 11.00000 -1.50000 H68B 2 0.119746 0.326079 -0.063237 11.00000 -1.50000 H68C 2 0.104586 0.279947 -0.056776 11.00000 -1.50000 AFIX 0 C69 1 0.036821 0.362481 0.208667 11.00000 0.02187 0.03320 = 0.03988 -0.00300 -0.00309 0.00413 AFIX 23 H69A 2 0.021037 0.360153 0.154514 11.00000 -1.20000 H69B 2 0.007073 0.367847 0.245448 11.00000 -1.20000 AFIX 0 C70 1 0.074183 0.397701 0.210237 11.00000 0.03252 0.03958 = 0.05303 0.00546 0.00099 -0.00163 AFIX 23 H70A 2 0.088656 0.401253 0.264898 11.00000 -1.20000 H70B 2 0.104763 0.392305 0.174991 11.00000 -1.20000 AFIX 0 C71 1 0.047058 0.435341 0.184103 11.00000 0.03960 0.03476 = 0.06863 -0.00007 -0.01424 -0.00422 AFIX 23 H71A 2 0.017810 0.441286 0.221406 11.00000 -1.20000 H71B 2 0.030446 0.430896 0.131020 11.00000 -1.20000 AFIX 0 C72 1 0.083124 0.471007 0.179670 11.00000 0.04866 0.04458 = 0.06500 0.01763 -0.00044 -0.00717 AFIX 33 H72A 2 0.062156 0.494201 0.162438 11.00000 -1.50000 H72B 2 0.111594 0.465909 0.141486 11.00000 -1.50000 H72C 2 0.099168 0.476194 0.232193 11.00000 -1.50000 AFIX 0 N5 3 0.832266 0.538259 0.387452 11.00000 0.05833 0.03525 = 0.04460 -0.02097 0.03132 -0.02659 C73 1 0.795438 0.571697 0.362497 11.00000 0.06392 0.05032 = 0.05602 -0.00569 0.01926 -0.02796 PART 1 AFIX 23 H73A 2 0.776563 0.579550 0.411376 41.00000 -1.20000 H73B 2 0.819447 0.594177 0.349651 41.00000 -1.20000 AFIX 23 PART 2 H73C 2 0.816030 0.596581 0.355255 -41.00000 -1.20000 H73D 2 0.767871 0.576295 0.403193 -41.00000 -1.20000 AFIX 0 PART 1 C74X 1 0.753327 0.571680 0.298378 41.00000 0.04940 0.03134 = 0.05571 -0.02399 0.03204 -0.00929 AFIX 23 H74A 2 0.723013 0.588274 0.316281 41.00000 -1.20000 H74B 2 0.739760 0.544156 0.292231 41.00000 -1.20000 AFIX 0 C75X 1 0.770009 0.586449 0.217479 41.00000 0.05952 0.04690 = 0.05244 -0.01425 0.01127 -0.00626 AFIX 23 H75A 2 0.781896 0.614476 0.221787 41.00000 -1.20000 H75B 2 0.800649 0.570435 0.198744 41.00000 -1.20000 AFIX 0 C76X 1 0.724221 0.583540 0.157997 41.00000 0.07117 0.02358 = 0.07499 -0.01082 -0.00318 0.01095 AFIX 33 H76A 2 0.735535 0.594366 0.106862 41.00000 -1.50000 H76B 2 0.693512 0.598763 0.177232 41.00000 -1.50000 H76C 2 0.713882 0.555603 0.151274 41.00000 -1.50000 AFIX 0 PART 2 C74Y 1 0.768576 0.558453 0.282226 -41.00000 0.06291 0.05450 = 0.05949 -0.02515 0.02025 -0.02489 AFIX 23 H74C 2 0.796391 0.552008 0.242907 -41.00000 -1.20000 H74D 2 0.746217 0.534508 0.290438 -41.00000 -1.20000 AFIX 0 C75Y 1 0.734223 0.592511 0.252659 -41.00000 0.10973 0.05047 = 0.06006 -0.00662 -0.00413 -0.03129 AFIX 23 H75C 2 0.708661 0.599907 0.294592 -41.00000 -1.20000 H75D 2 0.757510 0.615813 0.242969 -41.00000 -1.20000 AFIX 0 C76Y 1 0.703146 0.583045 0.177480 -41.00000 0.11982 0.07464 = 0.07376 -0.00650 -0.01531 -0.03381 AFIX 33 H76D 2 0.682982 0.606609 0.160158 -41.00000 -1.50000 H76E 2 0.678153 0.561176 0.187514 -41.00000 -1.50000 H76F 2 0.728092 0.575195 0.135877 -41.00000 -1.50000 AFIX 0 PART 0 C77 1 0.872107 0.528673 0.321926 11.00000 0.08016 0.05311 = 0.05581 -0.03468 0.04833 -0.03484 AFIX 23 H77A 2 0.895497 0.506685 0.340691 11.00000 -1.20000 H77B 2 0.851633 0.518842 0.275015 11.00000 -1.20000 AFIX 0 C78 1 0.907460 0.562515 0.295562 11.00000 0.06652 0.05347 = 0.05788 -0.02370 0.03334 -0.03315 PART 1 AFIX 23 H78A 2 0.923081 0.576058 0.342764 51.00000 -1.20000 H78B 2 0.885639 0.582144 0.265402 51.00000 -1.20000 AFIX 23 PART 2 H78C 2 0.888662 0.587823 0.306506 -51.00000 -1.20000 H78D 2 0.940656 0.562193 0.328654 -51.00000 -1.20000 AFIX 0 PART 1 C79X 1 0.953172 0.546839 0.242600 51.00000 0.03733 0.08364 = 0.04518 -0.00050 0.01239 -0.02039 AFIX 23 H79A 2 0.974129 0.569992 0.224168 51.00000 -1.20000 H79B 2 0.977458 0.530421 0.276215 51.00000 -1.20000 AFIX 0 PART 2 C79Y 1 0.923153 0.562374 0.209728 -51.00000 0.06282 0.03945 = 0.04390 0.00036 0.01789 -0.01416 AFIX 23 H79C 2 0.892839 0.573407 0.178032 -51.00000 -1.20000 H79D 2 0.953864 0.580754 0.203783 -51.00000 -1.20000 AFIX 0 PART 0 C80 1 0.937975 0.523950 0.174834 11.00000 0.08186 0.05120 = 0.06982 -0.00999 0.04831 -0.01691 PART 1 AFIX 33 H80A 2 0.970181 0.515674 0.146558 51.00000 -1.50000 H80B 2 0.915159 0.540046 0.139431 51.00000 -1.50000 H80C 2 0.918112 0.500356 0.191817 51.00000 -1.50000 AFIX 33 PART 2 H80D 2 0.946231 0.527630 0.118575 -51.00000 -1.50000 H80E 2 0.908013 0.505274 0.179681 -51.00000 -1.50000 H80F 2 0.969571 0.513305 0.202962 -51.00000 -1.50000 AFIX 0 PART 0 C81 1 0.861641 0.551575 0.462635 11.00000 0.05204 0.03348 = 0.04950 -0.02164 0.02491 -0.01854 AFIX 23 H81A 2 0.885225 0.574184 0.449006 11.00000 -1.20000 H81B 2 0.834763 0.561569 0.500441 11.00000 -1.20000 AFIX 0 C82 1 0.895402 0.520315 0.504505 11.00000 0.05149 0.03952 = 0.06559 -0.01509 0.02710 -0.01984 AFIX 23 H82A 2 0.914306 0.504196 0.464457 11.00000 -1.20000 H82B 2 0.871699 0.502332 0.534572 11.00000 -1.20000 AFIX 0 C83 1 0.936415 0.538924 0.561287 11.00000 0.04549 0.04731 = 0.06930 -0.01212 0.02691 -0.01835 AFIX 23 H83A 2 0.961469 0.555516 0.530485 11.00000 -1.20000 H83B 2 0.917569 0.556578 0.598761 11.00000 -1.20000 AFIX 0 C84 1 0.968073 0.508544 0.607854 11.00000 0.05892 0.06115 = 0.08749 -0.00780 0.01777 -0.01678 AFIX 33 H84A 2 0.993843 0.522099 0.643127 11.00000 -1.50000 H84B 2 0.987403 0.491266 0.571159 11.00000 -1.50000 H84C 2 0.943611 0.492464 0.639631 11.00000 -1.50000 AFIX 0 C85 1 0.800763 0.500227 0.402460 11.00000 0.06258 0.03767 = 0.04434 -0.02170 0.02994 -0.02890 AFIX 23 H85A 2 0.784765 0.491060 0.351449 11.00000 -1.20000 H85B 2 0.826049 0.479409 0.421202 11.00000 -1.20000 AFIX 0 C86 1 0.756577 0.504316 0.462330 11.00000 0.05958 0.03543 = 0.05319 -0.02118 0.03249 -0.02064 AFIX 23 H86A 2 0.729039 0.523092 0.441905 11.00000 -1.20000 H86B 2 0.771553 0.515208 0.512635 11.00000 -1.20000 AFIX 0 C87 1 0.730846 0.464067 0.477959 11.00000 0.07637 0.03946 = 0.06065 -0.02502 0.03909 -0.03098 AFIX 23 H87A 2 0.720033 0.451778 0.426702 11.00000 -1.20000 H87B 2 0.757492 0.446358 0.504125 11.00000 -1.20000 AFIX 0 C88 1 0.682931 0.467727 0.529274 11.00000 0.08961 0.05921 = 0.07769 -0.01847 0.04466 -0.03730 AFIX 33 H88A 2 0.668482 0.441201 0.540140 11.00000 -1.50000 H88B 2 0.655497 0.483794 0.501969 11.00000 -1.50000 H88C 2 0.693298 0.480591 0.579465 11.00000 -1.50000 AFIX 0 N6 3 0.573505 0.374884 0.262657 11.00000 0.00988 0.04265 = 0.04912 0.00635 0.01262 0.00323 C89 1 0.522303 0.384041 0.217116 11.00000 0.02442 0.04403 = 0.05984 -0.00045 0.00286 0.00437 AFIX 23 H89A 2 0.503966 0.406290 0.244030 11.00000 -1.20000 H89B 2 0.498502 0.360527 0.220020 11.00000 -1.20000 AFIX 0 C90 1 0.528791 0.394966 0.130484 11.00000 0.03444 0.07543 = 0.07024 0.01245 0.00026 -0.00324 AFIX 23 H90A 2 0.553984 0.376151 0.105465 11.00000 -1.20000 H90B 2 0.544231 0.422018 0.126674 11.00000 -1.20000 AFIX 0 C91 1 0.475156 0.393741 0.086179 11.00000 0.05712 0.05780 = 0.06876 0.00589 -0.01484 0.00681 AFIX 23 H91A 2 0.447909 0.407327 0.118642 11.00000 -1.20000 H91B 2 0.478414 0.408733 0.035857 11.00000 -1.20000 AFIX 0 C92 1 0.456026 0.352753 0.067650 11.00000 0.06279 0.08602 = 0.05842 -0.01805 0.00558 -0.01659 AFIX 33 H92A 2 0.421107 0.354149 0.040189 11.00000 -1.50000 H92B 2 0.452447 0.337689 0.117134 11.00000 -1.50000 H92C 2 0.481938 0.339454 0.033437 11.00000 -1.50000 AFIX 0 C93 1 0.614674 0.408685 0.254171 11.00000 0.02212 0.04254 = 0.04843 0.00277 0.00728 -0.00083 AFIX 23 H93A 2 0.649025 0.400152 0.279120 11.00000 -1.20000 H93B 2 0.621157 0.413085 0.196960 11.00000 -1.20000 AFIX 0 C94 1 0.597826 0.447870 0.291214 11.00000 0.02948 0.04315 = 0.06654 0.00250 0.01227 0.00170 AFIX 23 H94A 2 0.562076 0.455510 0.269746 11.00000 -1.20000 H94B 2 0.594686 0.444336 0.349352 11.00000 -1.20000 AFIX 0 C95 1 0.637050 0.480706 0.275141 11.00000 0.03163 0.03978 = 0.09419 0.00201 0.00806 0.00420 AFIX 23 H95A 2 0.638808 0.485308 0.217141 11.00000 -1.20000 H95B 2 0.673208 0.472630 0.294260 11.00000 -1.20000 AFIX 0 C96 1 0.620901 0.518989 0.316099 11.00000 0.03608 0.04530 = 0.11655 -0.00597 0.00684 -0.00261 AFIX 33 H96A 2 0.647050 0.539860 0.304327 11.00000 -1.50000 H96B 2 0.619939 0.514644 0.373637 11.00000 -1.50000 H96C 2 0.585284 0.527189 0.296787 11.00000 -1.50000 AFIX 0 C97 1 0.558106 0.369584 0.348771 11.00000 0.03051 0.03520 = 0.05259 0.00140 0.01946 0.00231 AFIX 23 H97A 2 0.539154 0.393895 0.366057 11.00000 -1.20000 H97B 2 0.532363 0.347231 0.351834 11.00000 -1.20000 AFIX 0 C98 1 0.603489 0.361667 0.406617 11.00000 0.04101 0.03751 = 0.05132 0.00083 0.00912 0.00661 AFIX 23 H98A 2 0.634384 0.378852 0.393595 11.00000 -1.20000 H98B 2 0.615050 0.333607 0.401848 11.00000 -1.20000 AFIX 0 C99 1 0.586507 0.369757 0.491240 11.00000 0.04722 0.04065 = 0.05815 -0.01047 0.02193 -0.00805 AFIX 23 H99A 2 0.578465 0.398456 0.496708 11.00000 -1.20000 H99B 2 0.553040 0.354889 0.501514 11.00000 -1.20000 AFIX 0 C100 1 0.627889 0.358376 0.552929 11.00000 0.08133 0.04106 = 0.04995 0.00253 0.01510 0.00220 AFIX 33 H10C 2 0.614449 0.364626 0.605890 11.00000 -1.50000 H10D 2 0.661027 0.373275 0.543853 11.00000 -1.50000 H10E 2 0.635203 0.329796 0.549312 11.00000 -1.50000 AFIX 0 C101 1 0.600764 0.337471 0.231398 11.00000 0.01650 0.04369 = 0.04440 -0.00272 0.01100 0.00685 AFIX 23 H10F 2 0.610462 0.342162 0.175359 11.00000 -1.20000 H10G 2 0.634571 0.333417 0.262009 11.00000 -1.20000 AFIX 0 C102 1 0.568086 0.299333 0.235230 11.00000 0.02606 0.04037 = 0.05311 0.00048 0.00565 0.00374 AFIX 23 H10H 2 0.561482 0.292404 0.291403 11.00000 -1.20000 H10I 2 0.532934 0.303348 0.208194 11.00000 -1.20000 AFIX 0 C103 1 0.597971 0.265662 0.195461 11.00000 0.03266 0.05188 = 0.03768 -0.00891 0.00126 -0.00013 AFIX 23 H10J 2 0.601212 0.271622 0.138133 11.00000 -1.20000 H10K 2 0.634659 0.263923 0.218622 11.00000 -1.20000 AFIX 0 C104 1 0.570272 0.226115 0.205047 11.00000 0.06566 0.04674 = 0.06331 -0.01206 0.00507 0.00026 AFIX 33 H10L 2 0.590798 0.205410 0.178030 11.00000 -1.50000 H10M 2 0.534060 0.227569 0.181668 11.00000 -1.50000 H10N 2 0.567957 0.219664 0.261674 11.00000 -1.50000 AFIX 0 N7 3 0.477988 0.371436 0.649029 11.00000 0.11830 0.10123 = 0.09431 0.03756 0.00046 -0.03703 C105 1 0.464463 0.389895 0.596583 11.00000 0.05160 0.06081 = 0.05819 -0.00861 0.00243 -0.02255 C106 1 0.448640 0.413714 0.528258 11.00000 0.05098 0.06999 = 0.06658 -0.00778 -0.02215 0.00615 HKLF 4 REM rje479 in P2(1)/c REM R1 = 0.0586 for 22904 Fo > 4sig(Fo) and 0.0987 for all 34144 data REM 1535 parameters refined using 3238 restraints END WGHT 0.0065 80.1023 REM Highest difference peak 1.378, deepest hole -1.329, 1-sigma level 0.125 Q1 1 0.3223 0.3896 0.1778 11.00000 0.05 1.38 Q2 1 0.8092 0.4624 0.3724 11.00000 0.05 1.25 Q3 1 0.3220 0.2137 0.6800 11.00000 0.05 1.16 Q4 1 0.7313 0.2181 -0.2181 11.00000 0.05 1.00 Q5 1 0.1673 0.3573 0.1908 11.00000 0.05 0.91 Q6 1 0.3385 0.2920 0.4507 11.00000 0.05 0.90 Q7 1 0.6887 0.4044 0.1960 11.00000 0.05 0.89 Q8 1 0.6673 0.4114 0.2295 11.00000 0.05 0.88 Q9 1 -0.0249 0.3372 0.2017 11.00000 0.05 0.86 Q10 1 0.7944 0.1444 0.4074 11.00000 0.05 0.84 ; #===END data_rje270_salt_of_5 _database_code_depnum_ccdc_archive 'CCDC 832954' #TrackingRef '- TiMo5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C16 H36 N +,C7 H7 Mo5 O19 Ti 3-' _chemical_formula_sum 'C55 H115 Mo5 N3 O19 Ti' _chemical_formula_weight 1650.10 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' Ti Ti 0.2776 0.4457 '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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 23.8573(14) _cell_length_b 16.9901(10) _cell_length_c 17.3090(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7016.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 20087 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.25 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3400 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 50872 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.25 _reflns_number_total 8322 _reflns_number_gt 7184 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0000P)^2^+107.4965P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8322 _refine_ls_number_parameters 421 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1801 _refine_ls_goodness_of_fit_ref 1.334 _refine_ls_restrained_S_all 1.336 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.30531(4) 0.2500 0.77670(5) 0.0189(2) Uani 1 2 d S . . Mo2 Mo 0.19846(3) 0.15291(5) 0.69967(4) 0.0314(2) Uani 1 1 d . . . Mo3 Mo 0.32195(3) 0.15245(5) 0.61282(4) 0.0305(2) Uani 1 1 d . . . Ti1 Ti 0.22105(8) 0.2500 0.54636(10) 0.0166(4) Uani 1 2 d S . . O10 O 0.3375(4) 0.2500 0.8636(5) 0.032(2) Uani 1 2 d S . . O12 O 0.2490(2) 0.1721(3) 0.7876(3) 0.0273(13) Uani 1 1 d . . . O13 O 0.3463(2) 0.1729(3) 0.7172(3) 0.0274(13) Uani 1 1 d . . . O20 O 0.1541(3) 0.0835(5) 0.7354(4) 0.058(2) Uani 1 1 d . . . O22 O 0.1623(3) 0.2500 0.7328(4) 0.0291(19) Uani 1 2 d S . . O23 O 0.2615(3) 0.0911(3) 0.6599(4) 0.0324(14) Uani 1 1 d . . . O24 O 0.1748(2) 0.1706(3) 0.6006(3) 0.0247(12) Uani 1 1 d . . . O30 O 0.3682(3) 0.0838(5) 0.5823(4) 0.056(2) Uani 1 1 d . . . O33 O 0.3606(3) 0.2500 0.5869(4) 0.032(2) Uani 1 2 d S . . O34 O 0.2756(2) 0.1698(3) 0.5273(3) 0.0261(12) Uani 1 1 d . . . O40 O 0.2599(3) 0.2500 0.6550(4) 0.0128(13) Uani 1 2 d S . . O1 O 0.1804(3) 0.2500 0.4546(4) 0.0236(17) Uani 1 2 d S . . C1 C 0.1273(5) 0.2500 0.4274(6) 0.022(2) Uani 1 2 d S . . C2 C 0.0816(5) 0.2500 0.4757(7) 0.032(3) Uani 1 2 d S . . H2 H 0.0869 0.2500 0.5301 0.038 Uiso 1 2 calc SR . . C3 C 0.0278(5) 0.2500 0.4453(9) 0.038(3) Uani 1 2 d S . . H3 H -0.0033 0.2500 0.4797 0.046 Uiso 1 2 calc SR . . C4 C 0.0179(6) 0.2500 0.3665(9) 0.040(3) Uani 1 2 d S . . C5 C 0.0640(6) 0.2500 0.3194(8) 0.038(3) Uani 1 2 d S . . H5 H 0.0584 0.2500 0.2651 0.046 Uiso 1 2 calc SR . . C6 C 0.1184(5) 0.2500 0.3472(7) 0.027(3) Uani 1 2 d S . . H6 H 0.1493 0.2500 0.3126 0.033 Uiso 1 2 calc SR . . C7 C -0.0410(7) 0.2500 0.3342(11) 0.063(5) Uani 1 2 d S . . H7A H -0.0681 0.2500 0.3769 0.094 Uiso 0.50 2 calc SPR . . H7B H -0.0466 0.2029 0.3025 0.094 Uiso 0.25 1 calc PR . . H7C H -0.0466 0.2971 0.3025 0.094 Uiso 0.25 1 calc PR . . H7D H -0.0395 0.2500 0.2777 0.094 Uiso 0.50 2 calc SPR . . H7E H -0.0609 0.2971 0.3521 0.094 Uiso 0.25 1 calc PR . . H7F H -0.0609 0.2029 0.3521 0.094 Uiso 0.25 1 calc PR . . N1 N 0.3170(3) -0.0038(4) 0.9086(4) 0.0259(15) Uani 1 1 d . . . C111 C 0.2841(4) 0.0676(5) 0.9354(5) 0.0304(19) Uani 1 1 d . . . H11A H 0.2607 0.0862 0.8918 0.036 Uiso 1 1 calc R . . H11B H 0.3110 0.1101 0.9479 0.036 Uiso 1 1 calc R . . C112 C 0.2460(4) 0.0551(6) 1.0054(5) 0.036(2) Uani 1 1 d . . . H11C H 0.2157 0.0178 0.9920 0.044 Uiso 1 1 calc R . . H11D H 0.2679 0.0325 1.0486 0.044 Uiso 1 1 calc R . . C113 C 0.2211(6) 0.1334(7) 1.0295(8) 0.065(4) Uani 1 1 d . . . H11E H 0.2010 0.1568 0.9851 0.078 Uiso 1 1 calc R . . H11F H 0.2517 0.1697 1.0443 0.078 Uiso 1 1 calc R . . C114 C 0.1808(6) 0.1247(8) 1.0971(8) 0.079(4) Uani 1 1 d . . . H11G H 0.1659 0.1765 1.1112 0.118 Uiso 1 1 calc R . . H11H H 0.2007 0.1021 1.1414 0.118 Uiso 1 1 calc R . . H11I H 0.1499 0.0900 1.0822 0.118 Uiso 1 1 calc R . . C121 C 0.2784(4) -0.0705(5) 0.8842(5) 0.032(2) Uani 1 1 d . . . H12A H 0.3018 -0.1171 0.8723 0.038 Uiso 1 1 calc R . . H12B H 0.2542 -0.0843 0.9286 0.038 Uiso 1 1 calc R . . C122 C 0.2412(4) -0.0542(6) 0.8152(5) 0.036(2) Uani 1 1 d . . . H12C H 0.2637 -0.0335 0.7718 0.043 Uiso 1 1 calc R . . H12D H 0.2124 -0.0145 0.8288 0.043 Uiso 1 1 calc R . . C123 C 0.2129(5) -0.1322(7) 0.7919(7) 0.055(3) Uani 1 1 d . . . H12E H 0.2421 -0.1711 0.7779 0.066 Uiso 1 1 calc R . . H12F H 0.1917 -0.1533 0.8366 0.066 Uiso 1 1 calc R . . C124 C 0.1729(5) -0.1211(9) 0.7234(8) 0.074(4) Uani 1 1 d . . . H12G H 0.1559 -0.1718 0.7099 0.110 Uiso 1 1 calc R . . H12H H 0.1938 -0.1008 0.6789 0.110 Uiso 1 1 calc R . . H12I H 0.1434 -0.0836 0.7375 0.110 Uiso 1 1 calc R . . C131 C 0.3529(4) 0.0240(5) 0.8412(5) 0.0290(19) Uani 1 1 d . . . H13A H 0.3791 0.0648 0.8600 0.035 Uiso 1 1 calc R . . H13B H 0.3282 0.0488 0.8022 0.035 Uiso 1 1 calc R . . C132 C 0.3867(4) -0.0414(5) 0.8020(5) 0.034(2) Uani 1 1 d . . . H13C H 0.4129 -0.0651 0.8398 0.040 Uiso 1 1 calc R . . H13D H 0.3610 -0.0832 0.7837 0.040 Uiso 1 1 calc R . . C133 C 0.4198(5) -0.0087(6) 0.7338(6) 0.046(3) Uani 1 1 d . . . H13E H 0.4448 0.0338 0.7522 0.055 Uiso 1 1 calc R . . H13F H 0.3934 0.0144 0.6959 0.055 Uiso 1 1 calc R . . C134 C 0.4548(5) -0.0722(7) 0.6941(7) 0.053(3) Uani 1 1 d . . . H13G H 0.4760 -0.0486 0.6514 0.080 Uiso 1 1 calc R . . H13H H 0.4300 -0.1133 0.6739 0.080 Uiso 1 1 calc R . . H13I H 0.4809 -0.0953 0.7314 0.080 Uiso 1 1 calc R . . C141 C 0.3530(4) -0.0373(5) 0.9731(5) 0.031(2) Uani 1 1 d . . . H14A H 0.3277 -0.0602 1.0126 0.037 Uiso 1 1 calc R . . H14B H 0.3755 -0.0810 0.9515 0.037 Uiso 1 1 calc R . . C142 C 0.3925(4) 0.0194(6) 1.0132(6) 0.035(2) Uani 1 1 d . . . H14C H 0.3707 0.0601 1.0412 0.042 Uiso 1 1 calc R . . H14D H 0.4165 0.0460 0.9747 0.042 Uiso 1 1 calc R . . C143 C 0.4286(4) -0.0268(7) 1.0700(6) 0.044(3) Uani 1 1 d . . . H14E H 0.4039 -0.0577 1.1046 0.053 Uiso 1 1 calc R . . H14F H 0.4523 -0.0644 1.0409 0.053 Uiso 1 1 calc R . . C144 C 0.4653(5) 0.0246(8) 1.1176(7) 0.065(3) Uani 1 1 d . . . H14G H 0.4877 -0.0080 1.1527 0.097 Uiso 1 1 calc R . . H14H H 0.4421 0.0609 1.1478 0.097 Uiso 1 1 calc R . . H14I H 0.4903 0.0546 1.0837 0.097 Uiso 1 1 calc R . . N2 N 0.5274(4) 0.2500 0.6133(6) 0.053(3) Uani 1 2 d SDU . . C211 C 0.4863(5) 0.2500 0.5470(7) 0.043(3) Uani 1 2 d SDU . . H21A H 0.4620 0.2970 0.5519 0.051 Uiso 0.50 1 calc PR . . H21B H 0.4620 0.2030 0.5519 0.051 Uiso 0.50 1 calc PR . . C212 C 0.5124(6) 0.2500 0.4656(8) 0.062(5) Uani 1 2 d SDU . . H21C H 0.5469 0.2177 0.4655 0.075 Uiso 0.50 1 calc PR A . H21D H 0.5226 0.3044 0.4507 0.075 Uiso 0.50 1 calc PR . . C213 C 0.4691(9) 0.2154(14) 0.4054(11) 0.070(6) Uani 0.50 1 d PDU A -1 H21E H 0.4875 0.2154 0.3542 0.084 Uiso 0.50 1 calc PR A -1 H21F H 0.4623 0.1598 0.4195 0.084 Uiso 0.50 1 calc PR A -1 C214 C 0.4191(7) 0.2500 0.3972(11) 0.102(8) Uani 1 2 d SDU . . H21G H 0.3970 0.2212 0.3587 0.153 Uiso 0.50 1 calc PR A . H21H H 0.4244 0.3045 0.3800 0.153 Uiso 0.50 1 calc PR . . H21I H 0.3993 0.2496 0.4468 0.153 Uiso 1 2 calc SR . . C221 C 0.4917(5) 0.2500 0.6861(7) 0.062(5) Uani 1 2 d SDU . . H22A H 0.4567 0.2205 0.6760 0.074 Uiso 0.50 1 calc PR B . H22B H 0.4813 0.3049 0.6989 0.074 Uiso 0.50 1 calc PR . . C222 C 0.5226(8) 0.2121(12) 0.7575(10) 0.051(5) Uani 0.50 1 d PDU B -1 H22C H 0.5588 0.2390 0.7667 0.061 Uiso 0.50 1 calc PR B -1 H22D H 0.5301 0.1557 0.7478 0.061 Uiso 0.50 1 calc PR B -1 C223 C 0.4825(16) 0.2222(17) 0.8304(16) 0.050(7) Uani 0.50 1 d PDU B -1 H22E H 0.4463 0.1957 0.8197 0.060 Uiso 0.50 1 calc PR B -1 H22F H 0.4998 0.1960 0.8756 0.060 Uiso 0.50 1 calc PR B -1 C224 C 0.4724(14) 0.3003(19) 0.8482(17) 0.052(6) Uani 0.50 1 d PDU B -1 H22G H 0.4474 0.3034 0.8930 0.078 Uiso 0.50 1 calc PR B -1 H22H H 0.4548 0.3264 0.8039 0.078 Uiso 0.50 1 calc PR B -1 H22I H 0.5079 0.3265 0.8604 0.078 Uiso 0.50 1 calc PR B -1 C231 C 0.5656(6) 0.1784(9) 0.6108(10) 0.116(5) Uani 1 1 d DU . . H23A H 0.5905 0.1795 0.6565 0.140 Uiso 1 1 calc R B . H23B H 0.5895 0.1817 0.5642 0.140 Uiso 1 1 calc R . . C232 C 0.5339(10) 0.0994(10) 0.6096(15) 0.199(10) Uani 1 1 d DU B . H23C H 0.4958 0.1083 0.5888 0.238 Uiso 1 1 calc R . . H23D H 0.5299 0.0802 0.6633 0.238 Uiso 1 1 calc R . . C233 C 0.5640(11) 0.0330(12) 0.5594(12) 0.206(10) Uani 1 1 d DU . . H23E H 0.5352 -0.0026 0.5377 0.248 Uiso 1 1 calc R B . H23F H 0.5837 0.0582 0.5155 0.248 Uiso 1 1 calc R . . C234 C 0.6008(7) -0.0095(13) 0.6000(10) 0.115(7) Uani 1 1 d DU B . H23G H 0.6187 -0.0483 0.5661 0.172 Uiso 1 1 calc R . . H23H H 0.5813 -0.0367 0.6420 0.172 Uiso 1 1 calc R . . H23I H 0.6295 0.0254 0.6217 0.172 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0205(4) 0.0221(5) 0.0142(4) 0.000 -0.0059(3) 0.000 Mo2 0.0335(4) 0.0340(4) 0.0266(4) 0.0144(3) -0.0108(3) -0.0197(3) Mo3 0.0332(4) 0.0336(4) 0.0248(3) -0.0112(3) -0.0109(3) 0.0218(3) Ti1 0.0209(10) 0.0151(9) 0.0138(8) 0.000 -0.0064(7) 0.000 O10 0.030(5) 0.046(5) 0.020(4) 0.000 -0.006(3) 0.000 O12 0.028(3) 0.034(3) 0.020(3) 0.014(2) -0.007(2) -0.005(3) O13 0.024(3) 0.034(3) 0.023(3) 0.001(2) -0.006(2) 0.011(3) O20 0.054(5) 0.064(5) 0.055(5) 0.036(4) -0.016(4) -0.042(4) O22 0.016(4) 0.048(5) 0.023(4) 0.000 0.004(3) 0.000 O23 0.049(4) 0.011(3) 0.037(3) 0.004(2) -0.017(3) 0.006(3) O24 0.027(3) 0.022(3) 0.025(3) 0.000(2) -0.011(2) -0.005(2) O30 0.054(4) 0.071(5) 0.043(4) -0.024(4) -0.013(3) 0.053(4) O33 0.019(4) 0.058(6) 0.018(4) 0.000 -0.003(3) 0.000 O34 0.031(3) 0.027(3) 0.021(3) -0.008(2) -0.006(2) 0.005(2) O40 0.015(3) 0.014(3) 0.010(3) 0.000 -0.007(3) 0.000 O1 0.027(4) 0.024(4) 0.019(4) 0.000 -0.010(3) 0.000 C1 0.037(7) 0.006(5) 0.025(5) 0.000 -0.013(5) 0.000 C2 0.030(7) 0.035(7) 0.029(6) 0.000 -0.009(5) 0.000 C3 0.018(6) 0.042(8) 0.054(8) 0.000 -0.005(6) 0.000 C4 0.039(8) 0.031(7) 0.051(8) 0.000 -0.025(7) 0.000 C5 0.056(9) 0.022(6) 0.036(7) 0.000 -0.026(7) 0.000 C6 0.033(7) 0.018(6) 0.031(6) 0.000 -0.013(5) 0.000 C7 0.041(9) 0.066(12) 0.081(13) 0.000 -0.033(9) 0.000 N1 0.030(4) 0.016(3) 0.031(3) 0.016(3) -0.008(3) -0.005(3) C111 0.037(5) 0.019(4) 0.035(4) 0.008(4) -0.002(4) -0.003(4) C112 0.039(5) 0.035(5) 0.035(5) 0.011(4) 0.002(4) -0.002(4) C113 0.081(9) 0.051(7) 0.064(8) 0.004(6) 0.025(7) -0.003(7) C114 0.098(11) 0.059(8) 0.079(9) 0.005(7) 0.036(9) -0.001(8) C121 0.038(5) 0.021(4) 0.036(5) 0.015(4) -0.005(4) -0.012(4) C122 0.031(5) 0.041(5) 0.036(5) 0.010(4) -0.011(4) -0.006(4) C123 0.054(7) 0.052(7) 0.060(7) 0.001(6) -0.020(6) -0.022(6) C124 0.055(8) 0.085(10) 0.080(9) -0.017(8) -0.026(7) -0.020(7) C131 0.034(5) 0.027(4) 0.026(4) 0.009(3) -0.004(3) -0.009(4) C132 0.029(5) 0.033(5) 0.038(5) 0.014(4) -0.003(4) -0.004(4) C133 0.053(6) 0.045(6) 0.040(5) 0.011(5) 0.006(5) 0.011(5) C134 0.060(7) 0.050(7) 0.049(6) -0.002(5) 0.010(5) 0.013(6) C141 0.036(5) 0.032(5) 0.026(4) 0.017(4) -0.009(4) -0.001(4) C142 0.032(5) 0.032(5) 0.042(5) 0.000(4) -0.009(4) -0.005(4) C143 0.035(5) 0.061(7) 0.037(5) 0.007(5) -0.007(4) -0.007(5) C144 0.056(7) 0.086(10) 0.051(7) -0.003(7) -0.010(6) -0.008(7) N2 0.016(5) 0.098(8) 0.044(5) 0.000 0.004(4) 0.000 C211 0.028(6) 0.066(9) 0.035(5) 0.000 0.000(5) 0.000 C212 0.037(7) 0.106(14) 0.044(6) 0.000 0.010(6) 0.000 C213 0.084(12) 0.092(17) 0.035(8) -0.010(10) -0.003(9) 0.020(10) C214 0.051(9) 0.21(2) 0.045(10) 0.000 -0.006(8) 0.000 C221 0.018(6) 0.135(15) 0.033(6) 0.000 -0.002(5) 0.000 C222 0.036(10) 0.064(13) 0.052(8) 0.008(9) -0.010(7) -0.002(9) C223 0.061(14) 0.043(18) 0.045(9) 0.005(9) -0.013(9) 0.002(12) C224 0.059(19) 0.037(15) 0.060(18) -0.006(12) -0.030(12) -0.006(13) C231 0.060(8) 0.183(12) 0.107(11) 0.065(10) 0.044(7) 0.076(8) C232 0.26(2) 0.110(10) 0.23(2) 0.084(14) 0.131(18) 0.085(11) C233 0.27(2) 0.149(13) 0.20(2) 0.096(13) 0.098(16) 0.149(15) C234 0.080(11) 0.177(19) 0.087(12) -0.021(13) 0.004(9) 0.034(11) _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 O10 1.689(8) . ? Mo1 O12 1.895(6) . ? Mo1 O12 1.895(6) 7_565 ? Mo1 O13 1.932(6) . ? Mo1 O13 1.932(6) 7_565 ? Mo1 O40 2.368(6) . ? Mo2 O12 1.969(5) . ? Mo2 O20 1.701(6) . ? Mo2 O22 1.947(4) . ? Mo2 O23 1.960(6) . ? Mo2 O24 1.830(5) . ? Mo2 O40 2.338(5) . ? Mo3 O13 1.930(5) . ? Mo3 O23 1.956(7) . ? Mo3 O30 1.690(6) . ? Mo3 O33 1.949(4) . ? Mo3 O34 1.871(5) . ? Mo3 O40 2.339(5) . ? Ti1 O24 1.980(6) . ? Ti1 O24 1.980(6) 7_565 ? Ti1 O34 1.912(6) . ? Ti1 O34 1.912(6) 7_565 ? Ti1 O40 2.097(6) . ? Ti1 O1 1.861(7) . ? O22 Mo2 1.947(4) 7_565 ? O33 Mo3 1.949(4) 7_565 ? O40 Mo2 2.338(5) 7_565 ? O40 Mo3 2.339(5) 7_565 ? O1 C1 1.353(13) . ? C1 C2 1.372(17) . ? C1 C6 1.405(15) . ? C2 H2 0.950 . ? C2 C3 1.389(17) . ? C3 H3 0.950 . ? C3 C4 1.38(2) . ? C4 C5 1.37(2) . ? C4 C7 1.513(19) . ? C5 H5 0.950 . ? C5 C6 1.384(17) . ? C6 H6 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C7 H7D 0.980 . ? C7 H7E 0.980 . ? C7 H7F 0.980 . ? N1 C111 1.518(11) . ? N1 C121 1.520(10) . ? N1 C131 1.522(10) . ? N1 C141 1.519(9) . ? C111 H11A 0.990 . ? C111 H11B 0.990 . ? C111 C112 1.528(12) . ? C112 H11C 0.990 . ? C112 H11D 0.990 . ? C112 C113 1.515(15) . ? C113 H11E 0.990 . ? C113 H11F 0.990 . ? C113 C114 1.521(16) . ? C114 H11G 0.980 . ? C114 H11H 0.980 . ? C114 H11I 0.980 . ? C121 H12A 0.990 . ? C121 H12B 0.990 . ? C121 C122 1.513(11) . ? C122 H12C 0.990 . ? C122 H12D 0.990 . ? C122 C123 1.541(13) . ? C123 H12E 0.990 . ? C123 H12F 0.990 . ? C123 C124 1.534(15) . ? C124 H12G 0.980 . ? C124 H12H 0.980 . ? C124 H12I 0.980 . ? C131 H13A 0.990 . ? C131 H13B 0.990 . ? C131 C132 1.532(13) . ? C132 H13C 0.990 . ? C132 H13D 0.990 . ? C132 C133 1.523(13) . ? C133 H13E 0.990 . ? C133 H13F 0.990 . ? C133 C134 1.528(14) . ? C134 H13G 0.980 . ? C134 H13H 0.980 . ? C134 H13I 0.980 . ? C141 H14A 0.990 . ? C141 H14B 0.990 . ? C141 C142 1.516(12) . ? C142 H14C 0.990 . ? C142 H14D 0.990 . ? C142 C143 1.526(13) . ? C143 H14E 0.990 . ? C143 H14F 0.990 . ? C143 C144 1.486(15) . ? C144 H14G 0.980 . ? C144 H14H 0.980 . ? C144 H14I 0.980 . ? N2 C211 1.509(12) . ? N2 C221 1.521(13) . ? N2 C231 1.521(12) . ? N2 C231 1.521(12) 7_565 ? C211 H21A 0.990 . ? C211 H21B 0.990 . ? C211 C212 1.541(15) . ? C212 H21C 0.990 . ? C212 H21D 0.990 . ? C212 C213 1.58(2) . ? C213 H21E 0.990 . ? C213 H21F 0.990 . ? C213 C214 1.336(19) . ? C214 H21G 0.980 . ? C214 H21H 0.980 . ? C214 H21I 0.980 . ? C221 H22A 0.990 . ? C221 H22B 0.990 . ? C221 C222 1.576(16) . ? C222 H22C 0.990 . ? C222 H22D 0.990 . ? C222 C223 1.59(2) . ? C223 H22E 0.990 . ? C223 H22F 0.990 . ? C223 C224 1.384(19) . ? C224 H22G 0.980 . ? C224 H22H 0.980 . ? C224 H22I 0.980 . ? C231 H23A 0.990 . ? C231 H23B 0.990 . ? C231 C232 1.539(18) . ? C232 H23C 0.990 . ? C232 H23D 0.990 . ? C232 C233 1.60(2) . ? C233 H23E 0.990 . ? C233 H23F 0.990 . ? C233 C234 1.337(18) . ? C234 H23G 0.980 . ? C234 H23H 0.980 . ? C234 H23I 0.980 . ? 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 O10 Mo1 O12 103.5(3) . . ? O10 Mo1 O12 103.5(3) . 7_565 ? O10 Mo1 O13 104.2(3) . . ? O10 Mo1 O13 104.2(3) . 7_565 ? O10 Mo1 O40 179.8(3) . . ? O12 Mo1 O12 88.6(4) . 7_565 ? O12 Mo1 O13 86.5(3) . . ? O12 Mo1 O13 152.3(2) 7_565 . ? O12 Mo1 O13 86.5(3) 7_565 7_565 ? O12 Mo1 O13 152.3(2) . 7_565 ? O12 Mo1 O40 76.37(19) . . ? O12 Mo1 O40 76.37(19) 7_565 . ? O13 Mo1 O13 85.3(4) . 7_565 ? O13 Mo1 O40 76.0(2) . . ? O13 Mo1 O40 76.0(2) 7_565 . ? O12 Mo2 O20 102.4(3) . . ? O12 Mo2 O22 84.4(3) . . ? O12 Mo2 O23 83.7(2) . . ? O12 Mo2 O24 152.4(2) . . ? O12 Mo2 O40 75.8(2) . . ? O20 Mo2 O22 101.8(4) . . ? O20 Mo2 O23 103.6(4) . . ? O20 Mo2 O24 105.2(3) . . ? O20 Mo2 O40 178.0(3) . . ? O22 Mo2 O23 153.8(3) . . ? O22 Mo2 O24 90.0(3) . . ? O22 Mo2 O40 77.1(2) . . ? O23 Mo2 O24 89.8(2) . . ? O23 Mo2 O40 77.3(2) . . ? O24 Mo2 O40 76.6(2) . . ? O13 Mo3 O23 85.9(2) . . ? O13 Mo3 O30 102.7(3) . . ? O13 Mo3 O33 85.4(3) . . ? O13 Mo3 O34 152.9(2) . . ? O13 Mo3 O40 76.7(2) . . ? O23 Mo3 O30 104.0(4) . . ? O23 Mo3 O33 153.8(3) . . ? O23 Mo3 O34 88.7(2) . . ? O23 Mo3 O40 77.4(2) . . ? O30 Mo3 O33 101.9(4) . . ? O30 Mo3 O34 104.3(3) . . ? O30 Mo3 O40 178.5(3) . . ? O33 Mo3 O34 87.9(3) . . ? O33 Mo3 O40 76.7(2) . . ? O34 Mo3 O40 76.2(2) . . ? O24 Ti1 O24 85.9(3) . 7_565 ? O24 Ti1 O34 88.6(2) . . ? O24 Ti1 O34 161.2(2) 7_565 . ? O24 Ti1 O34 88.6(2) 7_565 7_565 ? O24 Ti1 O34 161.2(2) . 7_565 ? O24 Ti1 O40 79.7(2) . . ? O24 Ti1 O40 79.7(2) 7_565 . ? O24 Ti1 O1 96.6(2) . . ? O24 Ti1 O1 96.6(2) 7_565 . ? O34 Ti1 O34 90.9(4) . 7_565 ? O34 Ti1 O40 81.6(2) . . ? O34 Ti1 O40 81.6(2) 7_565 . ? O34 Ti1 O1 101.9(2) . . ? O34 Ti1 O1 101.9(2) 7_565 . ? O40 Ti1 O1 174.8(3) . . ? Mo1 O12 Mo2 118.2(3) . . ? Mo1 O13 Mo3 117.9(3) . . ? Mo2 O22 Mo2 115.8(4) . 7_565 ? Mo2 O23 Mo3 115.2(3) . . ? Mo2 O24 Ti1 112.6(3) . . ? Mo3 O33 Mo3 116.5(4) . 7_565 ? Mo3 O34 Ti1 112.2(3) . . ? Mo1 O40 Mo2 89.59(19) . . ? Mo1 O40 Mo2 89.59(19) . 7_565 ? Mo1 O40 Mo3 89.32(19) . . ? Mo1 O40 Mo3 89.32(19) . 7_565 ? Mo1 O40 Ti1 179.0(4) . . ? Mo2 O40 Mo2 89.8(2) . 7_565 ? Mo2 O40 Mo3 90.00(3) . . ? Mo2 O40 Mo3 90.00(3) 7_565 7_565 ? Mo2 O40 Mo3 178.9(3) . 7_565 ? Mo2 O40 Mo3 178.9(3) 7_565 . ? Mo2 O40 Ti1 91.1(2) . . ? Mo2 O40 Ti1 91.1(2) 7_565 . ? Mo3 O40 Mo3 90.2(2) . 7_565 ? Mo3 O40 Ti1 90.0(2) . . ? Mo3 O40 Ti1 90.0(2) 7_565 . ? Ti1 O1 C1 141.7(7) . . ? O1 C1 C2 122.2(10) . . ? O1 C1 C6 119.0(11) . . ? C2 C1 C6 118.8(11) . . ? C1 C2 H2 119.9 . . ? C1 C2 C3 120.3(12) . . ? H2 C2 C3 119.9 . . ? C2 C3 H3 119.0 . . ? C2 C3 C4 122.0(13) . . ? H3 C3 C4 119.0 . . ? C3 C4 C5 116.8(12) . . ? C3 C4 C7 121.4(15) . . ? C5 C4 C7 121.8(14) . . ? C4 C5 H5 118.4 . . ? C4 C5 C6 123.1(12) . . ? H5 C5 C6 118.4 . . ? C1 C6 C5 119.0(13) . . ? C1 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? C4 C7 H7D 109.5 . . ? C4 C7 H7E 109.5 . . ? C4 C7 H7F 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? H7D C7 H7E 109.5 . . ? H7D C7 H7F 109.5 . . ? H7E C7 H7F 109.5 . . ? C111 N1 C121 111.5(7) . . ? C111 N1 C131 106.1(6) . . ? C111 N1 C141 111.6(7) . . ? C121 N1 C131 111.0(7) . . ? C121 N1 C141 105.5(6) . . ? C131 N1 C141 111.3(6) . . ? N1 C111 H11A 108.3 . . ? N1 C111 H11B 108.3 . . ? N1 C111 C112 116.0(7) . . ? H11A C111 H11B 107.4 . . ? H11A C111 C112 108.3 . . ? H11B C111 C112 108.3 . . ? C111 C112 H11C 109.8 . . ? C111 C112 H11D 109.8 . . ? C111 C112 C113 109.3(8) . . ? H11C C112 H11D 108.3 . . ? H11C C112 C113 109.8 . . ? H11D C112 C113 109.8 . . ? C112 C113 H11E 109.2 . . ? C112 C113 H11F 109.2 . . ? C112 C113 C114 112.1(10) . . ? H11E C113 H11F 107.9 . . ? H11E C113 C114 109.2 . . ? H11F C113 C114 109.2 . . ? C113 C114 H11G 109.5 . . ? C113 C114 H11H 109.5 . . ? C113 C114 H11I 109.5 . . ? H11G C114 H11H 109.5 . . ? H11G C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? N1 C121 H12A 108.3 . . ? N1 C121 H12B 108.3 . . ? N1 C121 C122 116.0(7) . . ? H12A C121 H12B 107.4 . . ? H12A C121 C122 108.3 . . ? H12B C121 C122 108.3 . . ? C121 C122 H12C 110.1 . . ? C121 C122 H12D 110.1 . . ? C121 C122 C123 107.8(8) . . ? H12C C122 H12D 108.5 . . ? H12C C122 C123 110.1 . . ? H12D C122 C123 110.1 . . ? C122 C123 H12E 109.3 . . ? C122 C123 H12F 109.3 . . ? C122 C123 C124 111.6(10) . . ? H12E C123 H12F 108.0 . . ? H12E C123 C124 109.3 . . ? H12F C123 C124 109.3 . . ? C123 C124 H12G 109.5 . . ? C123 C124 H12H 109.5 . . ? C123 C124 H12I 109.5 . . ? H12G C124 H12H 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? N1 C131 H13A 108.7 . . ? N1 C131 H13B 108.7 . . ? N1 C131 C132 114.3(7) . . ? H13A C131 H13B 107.6 . . ? H13A C131 C132 108.7 . . ? H13B C131 C132 108.7 . . ? C131 C132 H13C 109.5 . . ? C131 C132 H13D 109.5 . . ? C131 C132 C133 110.6(7) . . ? H13C C132 H13D 108.1 . . ? H13C C132 C133 109.5 . . ? H13D C132 C133 109.5 . . ? C132 C133 H13E 109.2 . . ? C132 C133 H13F 109.2 . . ? C132 C133 C134 112.0(9) . . ? H13E C133 H13F 107.9 . . ? H13E C133 C134 109.2 . . ? H13F C133 C134 109.2 . . ? C133 C134 H13G 109.5 . . ? C133 C134 H13H 109.5 . . ? C133 C134 H13I 109.5 . . ? H13G C134 H13H 109.5 . . ? H13G C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? N1 C141 H14A 108.1 . . ? N1 C141 H14B 108.1 . . ? N1 C141 C142 116.7(7) . . ? H14A C141 H14B 107.3 . . ? H14A C141 C142 108.1 . . ? H14B C141 C142 108.1 . . ? C141 C142 H14C 110.0 . . ? C141 C142 H14D 110.0 . . ? C141 C142 C143 108.6(8) . . ? H14C C142 H14D 108.3 . . ? H14C C142 C143 110.0 . . ? H14D C142 C143 110.0 . . ? C142 C143 H14E 109.0 . . ? C142 C143 H14F 109.0 . . ? C142 C143 C144 112.8(10) . . ? H14E C143 H14F 107.8 . . ? H14E C143 C144 109.0 . . ? H14F C143 C144 109.0 . . ? C143 C144 H14G 109.5 . . ? C143 C144 H14H 109.5 . . ? C143 C144 H14I 109.5 . . ? H14G C144 H14H 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C211 N2 C221 105.4(9) . . ? C211 N2 C231 111.6(9) . . ? C211 N2 C231 111.6(9) . 7_565 ? C221 N2 C231 111.0(8) . . ? C221 N2 C231 111.0(8) . 7_565 ? C231 N2 C231 106.3(14) . 7_565 ? N2 C211 H21A 108.4 . . ? N2 C211 H21B 108.4 . . ? N2 C211 C212 115.6(10) . . ? H21A C211 H21B 107.4 . . ? H21A C211 C212 108.4 . . ? H21B C211 C212 108.4 . . ? C211 C212 H21C 109.7 . . ? C211 C212 H21D 109.7 . . ? C211 C212 C213 109.8(12) . . ? H21C C212 H21D 108.2 . . ? H21C C212 C213 109.7 . . ? H21D C212 C213 109.7 . . ? C212 C213 H21E 107.5 . . ? C212 C213 H21F 107.5 . . ? C212 C213 C214 119.4(16) . . ? H21E C213 H21F 107.0 . . ? H21E C213 C214 107.5 . . ? H21F C213 C214 107.5 . . ? C213 C214 H21G 109.5 . . ? C213 C214 H21H 109.5 . . ? C213 C214 H21I 109.5 . . ? H21G C214 H21H 109.5 . . ? H21G C214 H21I 109.5 . . ? H21H C214 H21I 109.5 . . ? N2 C221 H22A 109.0 . . ? N2 C221 H22B 109.0 . . ? N2 C221 C222 112.8(10) . . ? H22A C221 H22B 107.8 . . ? H22A C221 C222 109.0 . . ? H22B C221 C222 109.0 . . ? C221 C222 H22C 110.3 . . ? C221 C222 H22D 110.3 . . ? C221 C222 C223 107.2(16) . . ? H22C C222 H22D 108.5 . . ? H22C C222 C223 110.3 . . ? H22D C222 C223 110.3 . . ? C222 C223 H22E 109.1 . . ? C222 C223 H22F 109.1 . . ? C222 C223 C224 112.6(18) . . ? H22E C223 H22F 107.8 . . ? H22E C223 C224 109.1 . . ? H22F C223 C224 109.1 . . ? C223 C224 H22G 109.5 . . ? C223 C224 H22H 109.5 . . ? C223 C224 H22I 109.5 . . ? H22G C224 H22H 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? N2 C231 H23A 108.8 . . ? N2 C231 H23B 108.8 . . ? N2 C231 C232 113.8(11) . . ? H23A C231 H23B 107.7 . . ? H23A C231 C232 108.8 . . ? H23B C231 C232 108.8 . . ? C231 C232 H23C 108.8 . . ? C231 C232 H23D 108.8 . . ? C231 C232 C233 113.7(17) . . ? H23C C232 H23D 107.7 . . ? H23C C232 C233 108.8 . . ? H23D C232 C233 108.8 . . ? C232 C233 H23E 109.0 . . ? C232 C233 H23F 109.0 . . ? C232 C233 C234 113.0(19) . . ? H23E C233 H23F 107.8 . . ? H23E C233 C234 109.0 . . ? H23F C233 C234 109.0 . . ? C233 C234 H23G 109.5 . . ? C233 C234 H23H 109.5 . . ? C233 C234 H23I 109.5 . . ? H23G C234 H23H 109.5 . . ? H23G C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.591 _refine_diff_density_min -1.691 _refine_diff_density_rms 0.170 # Contents of RES file _computing_special_details ; TITL rje270 in Pnma CELL 0.71073 23.8573 16.9901 17.3090 90.000 90.000 90.000 ZERR 4.00 0.0014 0.0010 0.0010 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC C H N O TI MO UNIT 220 460 12 76 4 20 SIZE 0.5 0.32 0.2 TEMP -113 CONN $TI $MO 6 L.S. 8 ACTA 52 BOND $H FMAP 2 PLAN 10 DELU N2 > C234 SIMU N2 > C234 REM EXTI insignificant WGHT 0.000000 107.496498 FVAR 0.10074 MO1 6 0.305307 0.250000 0.776702 10.50000 0.02054 0.02213 = 0.01416 0.00000 -0.00586 0.00000 MO2 6 0.198463 0.152910 0.699666 11.00000 0.03348 0.03402 = 0.02657 0.01440 -0.01078 -0.01972 MO3 6 0.321949 0.152452 0.612817 11.00000 0.03317 0.03359 = 0.02478 -0.01119 -0.01086 0.02177 TI1 5 0.221051 0.250000 0.546363 10.50000 0.02093 0.01506 = 0.01381 0.00000 -0.00642 0.00000 O10 4 0.337490 0.250000 0.863591 10.50000 0.02966 0.04584 = 0.01952 0.00000 -0.00634 0.00000 O12 4 0.249005 0.172134 0.787618 11.00000 0.02800 0.03385 = 0.02000 0.01379 -0.00680 -0.00542 O13 4 0.346324 0.172921 0.717198 11.00000 0.02430 0.03443 = 0.02347 0.00103 -0.00581 0.01149 O20 4 0.154070 0.083498 0.735397 11.00000 0.05419 0.06386 = 0.05511 0.03647 -0.01558 -0.04227 O22 4 0.162328 0.250000 0.732755 10.50000 0.01603 0.04846 = 0.02283 0.00000 0.00398 0.00000 O23 4 0.261549 0.091104 0.659861 11.00000 0.04935 0.01091 = 0.03691 0.00444 -0.01656 0.00591 O24 4 0.174762 0.170626 0.600645 11.00000 0.02741 0.02167 = 0.02511 -0.00022 -0.01080 -0.00478 O30 4 0.368157 0.083759 0.582301 11.00000 0.05390 0.07086 = 0.04278 -0.02410 -0.01339 0.05330 O33 4 0.360644 0.250000 0.586945 10.50000 0.01883 0.05796 = 0.01825 0.00000 -0.00253 0.00000 O34 4 0.275574 0.169828 0.527303 11.00000 0.03057 0.02668 = 0.02098 -0.00773 -0.00611 0.00465 O40 4 0.259886 0.250000 0.655030 10.50000 0.01518 0.01357 = 0.00979 0.00000 -0.00736 0.00000 O1 4 0.180447 0.250000 0.454593 10.50000 0.02721 0.02446 = 0.01909 0.00000 -0.00994 0.00000 C1 1 0.127284 0.250000 0.427450 10.50000 0.03674 0.00610 = 0.02457 0.00000 -0.01286 0.00000 C2 1 0.081637 0.250000 0.475669 10.50000 0.03046 0.03534 = 0.02922 0.00000 -0.00882 0.00000 AFIX 43 H2 2 0.086912 0.250000 0.530070 10.50000 -1.20000 AFIX 0 C3 1 0.027751 0.250000 0.445295 10.50000 0.01844 0.04168 = 0.05417 0.00000 -0.00544 0.00000 AFIX 43 H3 2 -0.003299 0.250000 0.479658 10.50000 -1.20000 AFIX 0 C4 1 0.017912 0.250000 0.366508 10.50000 0.03861 0.03056 = 0.05133 0.00000 -0.02500 0.00000 C5 1 0.063988 0.250000 0.319430 10.50000 0.05589 0.02221 = 0.03627 0.00000 -0.02635 0.00000 AFIX 43 H5 2 0.058376 0.250000 0.265093 10.50000 -1.20000 AFIX 0 C6 1 0.118383 0.250000 0.347231 10.50000 0.03283 0.01800 = 0.03126 0.00000 -0.01322 0.00000 AFIX 43 H6 2 0.149253 0.250000 0.312561 10.50000 -1.20000 AFIX 0 C7 1 -0.041032 0.250000 0.334242 10.50000 0.04064 0.06649 = 0.08147 0.00000 -0.03347 0.00000 AFIX 123 H7A 2 -0.068052 0.250000 0.376887 10.25000 -1.50000 H7B 2 -0.046610 0.202904 0.302471 10.25000 -1.50000 H7C 2 -0.046610 0.297096 0.302471 10.25000 -1.50000 H7D 2 -0.039463 0.250000 0.277666 10.25000 -1.50000 H7E 2 -0.060905 0.297096 0.352082 10.25000 -1.50000 H7F 2 -0.060905 0.202904 0.352082 10.25000 -1.50000 AFIX 0 N1 3 0.317017 -0.003775 0.908609 11.00000 0.02986 0.01648 = 0.03147 0.01572 -0.00769 -0.00536 C111 1 0.284068 0.067597 0.935405 11.00000 0.03693 0.01944 = 0.03469 0.00842 -0.00231 -0.00287 AFIX 23 H11A 2 0.260684 0.086169 0.891814 11.00000 -1.20000 H11B 2 0.310973 0.110104 0.947865 11.00000 -1.20000 AFIX 0 C112 1 0.246042 0.055121 1.005350 11.00000 0.03860 0.03509 = 0.03539 0.01079 0.00211 -0.00245 AFIX 23 H11C 2 0.215674 0.017797 0.992042 11.00000 -1.20000 H11D 2 0.267947 0.032494 1.048554 11.00000 -1.20000 AFIX 0 C113 1 0.221116 0.133371 1.029543 11.00000 0.08142 0.05074 = 0.06376 0.00448 0.02481 -0.00313 AFIX 23 H11E 2 0.200973 0.156806 0.985143 11.00000 -1.20000 H11F 2 0.251739 0.169717 1.044276 11.00000 -1.20000 AFIX 0 C114 1 0.180824 0.124717 1.097079 11.00000 0.09792 0.05882 = 0.07915 0.00549 0.03585 -0.00142 AFIX 33 H11G 2 0.165948 0.176532 1.111165 11.00000 -1.50000 H11H 2 0.200701 0.102071 1.141361 11.00000 -1.50000 H11I 2 0.149854 0.089971 1.082237 11.00000 -1.50000 AFIX 0 C121 1 0.278419 -0.070472 0.884158 11.00000 0.03798 0.02145 = 0.03614 0.01507 -0.00504 -0.01240 AFIX 23 H12A 2 0.301761 -0.117113 0.872313 11.00000 -1.20000 H12B 2 0.254231 -0.084298 0.928607 11.00000 -1.20000 AFIX 0 C122 1 0.241151 -0.054180 0.815231 11.00000 0.03077 0.04063 = 0.03613 0.01015 -0.01093 -0.00635 AFIX 23 H12C 2 0.263739 -0.033510 0.771752 11.00000 -1.20000 H12D 2 0.212387 -0.014528 0.828822 11.00000 -1.20000 AFIX 0 C123 1 0.212890 -0.132211 0.791927 11.00000 0.05375 0.05164 = 0.05968 0.00136 -0.02010 -0.02241 AFIX 23 H12E 2 0.242078 -0.171095 0.777926 11.00000 -1.20000 H12F 2 0.191722 -0.153305 0.836552 11.00000 -1.20000 AFIX 0 C124 1 0.172877 -0.121104 0.723387 11.00000 0.05540 0.08508 = 0.08045 -0.01739 -0.02650 -0.01961 AFIX 33 H12G 2 0.155868 -0.171785 0.709929 11.00000 -1.50000 H12H 2 0.193812 -0.100822 0.678927 11.00000 -1.50000 H12I 2 0.143396 -0.083610 0.737529 11.00000 -1.50000 AFIX 0 C131 1 0.352866 0.023987 0.841201 11.00000 0.03425 0.02652 = 0.02619 0.00941 -0.00436 -0.00877 AFIX 23 H13A 2 0.379117 0.064834 0.860034 11.00000 -1.20000 H13B 2 0.328178 0.048784 0.802201 11.00000 -1.20000 AFIX 0 C132 1 0.386748 -0.041404 0.801991 11.00000 0.02946 0.03294 = 0.03845 0.01374 -0.00308 -0.00352 AFIX 23 H13C 2 0.412916 -0.065079 0.839811 11.00000 -1.20000 H13D 2 0.361034 -0.083184 0.783733 11.00000 -1.20000 AFIX 0 C133 1 0.419751 -0.008729 0.733822 11.00000 0.05279 0.04507 = 0.03985 0.01126 0.00585 0.01104 AFIX 23 H13E 2 0.444790 0.033798 0.752200 11.00000 -1.20000 H13F 2 0.393370 0.014350 0.695926 11.00000 -1.20000 AFIX 0 C134 1 0.454823 -0.072151 0.694059 11.00000 0.06008 0.04989 = 0.04932 -0.00207 0.01042 0.01331 AFIX 33 H13G 2 0.475985 -0.048584 0.651402 11.00000 -1.50000 H13H 2 0.430041 -0.113290 0.673854 11.00000 -1.50000 H13I 2 0.480936 -0.095255 0.731421 11.00000 -1.50000 AFIX 0 C141 1 0.352965 -0.037312 0.973116 11.00000 0.03566 0.03212 = 0.02596 0.01692 -0.00942 -0.00077 AFIX 23 H14A 2 0.327725 -0.060160 1.012589 11.00000 -1.20000 H14B 2 0.375544 -0.080978 0.951536 11.00000 -1.20000 AFIX 0 C142 1 0.392457 0.019407 1.013246 11.00000 0.03227 0.03216 = 0.04176 -0.00049 -0.00871 -0.00520 AFIX 23 H14C 2 0.370708 0.060075 1.041161 11.00000 -1.20000 H14D 2 0.416530 0.046001 0.974658 11.00000 -1.20000 AFIX 0 C143 1 0.428623 -0.026832 1.070015 11.00000 0.03546 0.06059 = 0.03701 0.00724 -0.00718 -0.00714 AFIX 23 H14E 2 0.403944 -0.057677 1.104623 11.00000 -1.20000 H14F 2 0.452257 -0.064411 1.040866 11.00000 -1.20000 AFIX 0 C144 1 0.465318 0.024561 1.117611 11.00000 0.05612 0.08650 = 0.05118 -0.00259 -0.01009 -0.00830 AFIX 33 H14G 2 0.487720 -0.007990 1.152701 11.00000 -1.50000 H14H 2 0.442130 0.060922 1.147782 11.00000 -1.50000 H14I 2 0.490308 0.054650 1.083744 11.00000 -1.50000 AFIX 0 SAME N2 C221 > C224 SAME N2 C231 > C234 N2 3 0.527400 0.250000 0.613269 10.50000 0.01577 0.09775 = 0.04404 0.00000 0.00388 0.00000 C211 1 0.486274 0.250000 0.547018 10.50000 0.02783 0.06561 = 0.03530 0.00000 0.00043 0.00000 AFIX 23 H21A 2 0.461981 0.296973 0.551944 10.50000 -1.20000 H21B 2 0.461981 0.203027 0.551944 10.50000 -1.20000 AFIX 0 C212 1 0.512356 0.250000 0.465560 10.50000 0.03729 0.10576 = 0.04371 0.00000 0.00959 0.00000 AFIX 23 H21C 2 0.546892 0.217696 0.465491 10.50000 -1.20000 H21D 2 0.522585 0.304406 0.450705 10.50000 -1.20000 AFIX 0 PART -1 C213 1 0.469092 0.215446 0.405443 10.50000 0.08405 0.09174 = 0.03466 -0.01015 -0.00346 0.01971 AFIX 23 H21E 2 0.487518 0.215428 0.354195 10.50000 -1.20000 H21F 2 0.462316 0.159765 0.419476 10.50000 -1.20000 AFIX 0 PART 0 C214 1 0.419126 0.250000 0.397184 10.50000 0.05138 0.20985 = 0.04509 0.00000 -0.00597 0.00000 AFIX 33 H21G 2 0.397039 0.221244 0.358685 10.50000 -1.50000 H21H 2 0.424372 0.304471 0.380020 10.50000 -1.50000 H21I 2 0.399326 0.249623 0.446789 10.50000 -1.50000 AFIX 0 C221 1 0.491728 0.250000 0.686117 10.50000 0.01774 0.13529 = 0.03314 0.00000 -0.00186 0.00000 AFIX 23 H22A 2 0.456716 0.220456 0.676041 10.50000 -1.20000 H22B 2 0.481335 0.304878 0.698943 10.50000 -1.20000 AFIX 0 PART -1 C222 1 0.522649 0.212130 0.757473 10.50000 0.03566 0.06359 = 0.05226 0.00759 -0.00985 -0.00242 AFIX 23 H22C 2 0.558840 0.239031 0.766735 10.50000 -1.20000 H22D 2 0.530113 0.155671 0.747759 10.50000 -1.20000 AFIX 0 C223 1 0.482473 0.222204 0.830381 10.50000 0.06108 0.04325 = 0.04466 0.00472 -0.01275 0.00160 AFIX 23 H22E 2 0.446338 0.195708 0.819692 10.50000 -1.20000 H22F 2 0.499764 0.196022 0.875580 10.50000 -1.20000 AFIX 0 C224 1 0.472416 0.300318 0.848223 10.50000 0.05914 0.03745 = 0.05971 -0.00645 -0.03041 -0.00619 AFIX 33 H22G 2 0.447351 0.303389 0.892978 10.50000 -1.50000 H22H 2 0.454836 0.326402 0.803919 10.50000 -1.50000 H22I 2 0.507937 0.326491 0.860411 10.50000 -1.50000 AFIX 0 PART 0 C231 1 0.565594 0.178357 0.610814 11.00000 0.05954 0.18332 = 0.10660 0.06505 0.04350 0.07609 AFIX 23 H23A 2 0.590532 0.179482 0.656516 11.00000 -1.20000 H23B 2 0.589522 0.181704 0.564200 11.00000 -1.20000 AFIX 0 C232 1 0.533936 0.099416 0.609641 11.00000 0.25632 0.10987 = 0.22994 0.08441 0.13123 0.08540 AFIX 23 H23C 2 0.495816 0.108311 0.588798 11.00000 -1.20000 H23D 2 0.529924 0.080192 0.663350 11.00000 -1.20000 AFIX 0 C233 1 0.564031 0.033008 0.559351 11.00000 0.27002 0.14899 = 0.20038 0.09563 0.09823 0.14933 AFIX 23 H23E 2 0.535174 -0.002615 0.537748 11.00000 -1.20000 H23F 2 0.583728 0.058239 0.515523 11.00000 -1.20000 AFIX 0 C234 1 0.600824 -0.009469 0.599995 11.00000 0.07979 0.17750 = 0.08710 -0.02093 0.00417 0.03396 AFIX 33 H23G 2 0.618677 -0.048263 0.566082 11.00000 -1.50000 H23H 2 0.581287 -0.036724 0.642004 11.00000 -1.50000 H23I 2 0.629487 0.025433 0.621700 11.00000 -1.50000 HKLF 4 REM rje270 in Pnma REM R1 = 0.0964 for 7184 Fo > 4sig(Fo) and 0.1081 for all 8322 data REM 421 parameters refined using 117 restraints END WGHT 0.0000 104.8252 REM Highest difference peak 1.591, deepest hole -1.691, 1-sigma level 0.170 Q1 1 0.6139 0.0678 0.5898 11.00000 0.05 1.59 Q2 1 0.5158 0.0885 0.5805 11.00000 0.05 1.32 Q3 1 0.2817 0.2112 0.7780 11.00000 0.05 1.23 Q4 1 0.5490 0.1223 0.6626 11.00000 0.05 1.19 Q5 1 0.2113 0.2007 0.7041 11.00000 0.05 1.15 Q6 1 0.3367 0.1061 0.6050 11.00000 0.05 1.06 Q7 1 0.3307 0.2107 0.7731 11.00000 0.05 1.02 Q8 1 0.2690 0.2500 0.7748 10.50000 0.05 1.00 Q9 1 0.5489 0.0259 0.5449 11.00000 0.05 0.99 Q10 1 0.3626 0.1444 0.6069 11.00000 0.05 0.99 ; #===END data_rje286_salt_of_6 _database_code_depnum_ccdc_archive 'CCDC 832955' #TrackingRef '- TiMo5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3 C16 H36 N +,C7 H5 Mo5 O20 Ti 3-' _chemical_formula_sum 'C55 H113 Mo5 N3 O20 Ti' _chemical_formula_weight 1664.08 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' Ti Ti 0.2776 0.4457 '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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 24.049(4) _cell_length_b 17.521(3) _cell_length_c 17.242(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7265(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 32479 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 61909 _diffrn_reflns_av_R_equivalents 0.1493 _diffrn_reflns_av_sigmaI/netI 0.1256 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 28.74 _reflns_number_total 9237 _reflns_number_gt 3755 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1193P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0047(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9237 _refine_ls_number_parameters 428 _refine_ls_number_restraints 520 _refine_ls_R_factor_all 0.2085 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2420 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.18677(3) 0.34432(4) 0.11854(4) 0.0589(3) Uani 1 1 d . . . Mo2 Mo 0.30876(3) 0.34414(4) 0.20684(4) 0.0556(3) Uani 1 1 d . . . Mo3 Mo 0.20280(4) 0.2500 0.28358(5) 0.0516(3) Uani 1 2 d S . . Ti1 Ti 0.28764(9) 0.2500 0.05360(11) 0.0526(6) Uani 1 2 d S . . O1 O 0.3413(6) 0.2500 -0.2704(7) 0.136(5) Uani 1 2 d S . . O2 O 0.3276(4) 0.2500 -0.0408(5) 0.071(2) Uani 1 2 d S . . O3 O 0.1492(3) 0.2500 0.0932(5) 0.066(2) Uani 1 2 d S . . O4 O 0.1413(3) 0.4100(4) 0.0871(4) 0.093(2) Uani 1 1 d . . . O5 O 0.3522(3) 0.4106(4) 0.2429(4) 0.086(2) Uani 1 1 d . . . O6 O 0.3452(3) 0.2500 0.2395(5) 0.062(2) Uani 1 2 d S . . O7 O 0.1702(4) 0.2500 0.3695(5) 0.075(3) Uani 1 2 d S . . O8 O 0.2588(2) 0.3248(3) 0.2950(3) 0.0626(16) Uani 1 1 d . . . O9 O 0.1625(2) 0.3242(3) 0.2239(3) 0.0623(16) Uani 1 1 d . . . O10 O 0.2331(3) 0.3274(3) 0.0337(3) 0.0649(16) Uani 1 1 d . . . O11 O 0.2465(2) 0.4031(3) 0.1662(3) 0.0653(16) Uani 1 1 d . . . O12 O 0.3325(2) 0.3271(3) 0.1076(3) 0.0611(15) Uani 1 1 d . . . O13 O 0.2488(3) 0.2500 0.1610(3) 0.0410(16) Uani 1 2 d S . . C1 C 0.3780(6) 0.2500 -0.0705(7) 0.063(3) Uani 1 2 d S . . C2 C 0.4250(7) 0.2500 -0.0221(10) 0.097(5) Uani 1 2 d S . . H2 H 0.4204 0.2500 0.0326 0.117 Uiso 1 2 calc SR . . C3 C 0.4785(7) 0.2500 -0.0537(11) 0.120(6) Uani 1 2 d S . . H3 H 0.5103 0.2500 -0.0211 0.144 Uiso 1 2 calc SR . . C4 C 0.4840(8) 0.2500 -0.1337(12) 0.120(7) Uani 1 2 d S . . H4 H 0.5201 0.2500 -0.1562 0.144 Uiso 1 2 calc SR . . C5 C 0.4400(10) 0.2500 -0.1789(10) 0.107(6) Uani 1 2 d S . . H5 H 0.4451 0.2500 -0.2335 0.128 Uiso 1 2 calc SR . . C6 C 0.3862(6) 0.2500 -0.1491(7) 0.067(4) Uani 1 2 d S . . C7 C 0.3391(8) 0.2500 -0.2014(8) 0.086(5) Uani 1 2 d S . . H7 H 0.3032 0.2500 -0.1785 0.103 Uiso 1 2 calc SR . . N1 N 0.1890(3) 0.5039(4) 0.4134(4) 0.0714(19) Uani 1 1 d DU . . C8 C 0.1522(4) 0.5359(5) 0.4767(5) 0.075(3) Uani 1 1 d DU . . H8A H 0.1765 0.5564 0.5181 0.090 Uiso 1 1 calc R . . H8B H 0.1311 0.5793 0.4549 0.090 Uiso 1 1 calc R . . C9 C 0.1117(4) 0.4818(6) 0.5131(6) 0.091(3) Uani 1 1 d DU . . H9A H 0.1324 0.4400 0.5386 0.109 Uiso 1 1 calc R . . H9B H 0.0882 0.4590 0.4720 0.109 Uiso 1 1 calc R . . C10 C 0.0751(5) 0.5200(7) 0.5717(7) 0.115(4) Uani 1 1 d DU . . H10A H 0.0990 0.5467 0.6097 0.138 Uiso 1 1 calc R . . H10B H 0.0526 0.5592 0.5448 0.138 Uiso 1 1 calc R . . C11 C 0.0373(5) 0.4689(9) 0.6142(8) 0.157(6) Uani 1 1 d DU . . H11A H 0.0147 0.4990 0.6504 0.235 Uiso 1 1 calc R . . H11B H 0.0591 0.4312 0.6432 0.235 Uiso 1 1 calc R . . H11C H 0.0129 0.4426 0.5774 0.235 Uiso 1 1 calc R . . C12 C 0.1547(4) 0.4775(5) 0.3441(5) 0.079(3) Uani 1 1 d DU . . H12A H 0.1803 0.4546 0.3055 0.094 Uiso 1 1 calc R . . H12B H 0.1291 0.4368 0.3617 0.094 Uiso 1 1 calc R . . C13 C 0.1215(5) 0.5376(6) 0.3048(6) 0.100(3) Uani 1 1 d DU . . H13A H 0.1468 0.5797 0.2899 0.121 Uiso 1 1 calc R . . H13B H 0.0944 0.5585 0.3425 0.121 Uiso 1 1 calc R . . C14 C 0.0905(6) 0.5128(7) 0.2346(7) 0.129(5) Uani 1 1 d DU . . H14A H 0.1174 0.4892 0.1984 0.155 Uiso 1 1 calc R . . H14B H 0.0639 0.4726 0.2503 0.155 Uiso 1 1 calc R . . C15 C 0.0595(7) 0.5718(8) 0.1920(8) 0.166(7) Uani 1 1 d DU . . H15A H 0.0409 0.5486 0.1473 0.249 Uiso 1 1 calc R . . H15B H 0.0853 0.6112 0.1740 0.249 Uiso 1 1 calc R . . H15C H 0.0317 0.5948 0.2263 0.249 Uiso 1 1 calc R . . C16 C 0.2210(4) 0.4349(5) 0.4422(6) 0.081(3) Uani 1 1 d DU . . H16A H 0.1938 0.3941 0.4540 0.097 Uiso 1 1 calc R . . H16B H 0.2446 0.4163 0.3992 0.097 Uiso 1 1 calc R . . C17 C 0.2572(5) 0.4451(6) 0.5119(6) 0.106(4) Uani 1 1 d DU . . H17A H 0.2355 0.4689 0.5543 0.127 Uiso 1 1 calc R . . H17B H 0.2886 0.4793 0.4990 0.127 Uiso 1 1 calc R . . C18 C 0.2793(7) 0.3686(8) 0.5383(10) 0.160(6) Uani 1 1 d DU . . H18A H 0.2479 0.3374 0.5574 0.192 Uiso 1 1 calc R . . H18B H 0.2956 0.3419 0.4931 0.192 Uiso 1 1 calc R . . C19 C 0.3210(10) 0.3735(15) 0.5989(14) 0.304(15) Uani 1 1 d DU . . H19A H 0.3339 0.3221 0.6123 0.456 Uiso 1 1 calc R . . H19B H 0.3048 0.3978 0.6449 0.456 Uiso 1 1 calc R . . H19C H 0.3525 0.4040 0.5805 0.456 Uiso 1 1 calc R . . C20 C 0.2284(4) 0.5673(5) 0.3892(5) 0.077(3) Uani 1 1 d DU . . H20A H 0.2058 0.6122 0.3745 0.093 Uiso 1 1 calc R . . H20B H 0.2507 0.5819 0.4352 0.093 Uiso 1 1 calc R . . C21 C 0.2676(5) 0.5512(7) 0.3245(6) 0.099(4) Uani 1 1 d DU . . H21A H 0.2466 0.5316 0.2793 0.119 Uiso 1 1 calc R . . H21B H 0.2944 0.5114 0.3408 0.119 Uiso 1 1 calc R . . C22 C 0.2988(6) 0.6220(8) 0.3015(8) 0.139(5) Uani 1 1 d DU . . H22A H 0.2714 0.6617 0.2868 0.167 Uiso 1 1 calc R . . H22B H 0.3193 0.6410 0.3474 0.167 Uiso 1 1 calc R . . C23 C 0.3387(7) 0.6123(10) 0.2367(9) 0.178(7) Uani 1 1 d DU . . H23A H 0.3566 0.6613 0.2255 0.268 Uiso 1 1 calc R . . H23B H 0.3188 0.5945 0.1905 0.268 Uiso 1 1 calc R . . H23C H 0.3670 0.5747 0.2513 0.268 Uiso 1 1 calc R . . N2 N 0.4818(4) 0.2500 0.3782(6) 0.103(4) Uani 1 2 d SDU . . C24 C 0.4441(5) 0.3189(7) 0.3815(8) 0.128(4) Uani 1 1 d DU A . H24A H 0.4193 0.3177 0.3357 0.154 Uiso 1 1 calc R . . H24B H 0.4205 0.3146 0.4282 0.154 Uiso 1 1 calc R . . C25 C 0.4726(8) 0.3941(9) 0.3833(13) 0.232(9) Uani 1 1 d DU . . H25A H 0.4937 0.4028 0.3348 0.278 Uiso 1 1 calc R A . H25B H 0.4986 0.3971 0.4277 0.278 Uiso 1 1 calc R . . C26 C 0.4277(10) 0.4507(12) 0.3915(15) 0.286(12) Uani 1 1 d DU A . H26A H 0.4224 0.4730 0.3393 0.343 Uiso 1 1 calc R . . H26B H 0.3936 0.4210 0.4028 0.343 Uiso 1 1 calc R . . C27 C 0.4272(11) 0.5121(15) 0.4428(14) 0.327(16) Uani 1 1 d DU . . H27A H 0.3962 0.5461 0.4301 0.490 Uiso 1 1 calc R A . H27B H 0.4623 0.5402 0.4386 0.490 Uiso 1 1 calc R . . H27C H 0.4228 0.4932 0.4960 0.490 Uiso 1 1 calc R . . C28 C 0.5230(6) 0.2500 0.4456(8) 0.116(5) Uani 0.50 1 d PDU A . H28A H 0.5471 0.2046 0.4395 0.140 Uiso 0.50 1 calc PR . . H28B H 0.5471 0.2954 0.4395 0.140 Uiso 0.50 1 calc PR . . C29 C 0.5020(7) 0.2500 0.5264(8) 0.156(7) Uani 1 2 d SDU . . H29A H 0.4789 0.2041 0.5359 0.188 Uiso 0.50 1 calc PR A . H29B H 0.4789 0.2959 0.5359 0.188 Uiso 0.50 1 calc PR . . C30 C 0.5523(9) 0.2500 0.5801(11) 0.209(11) Uani 0.50 1 d PDU A . H30A H 0.5750 0.2046 0.5674 0.251 Uiso 0.50 1 calc PR . . H30B H 0.5750 0.2954 0.5674 0.251 Uiso 0.50 1 calc PR . . C31 C 0.5430(15) 0.2500 0.6628(11) 0.32(2) Uani 1 2 d SDU . . H31A H 0.5789 0.2500 0.6898 0.486 Uiso 0.50 1 calc PR A . H31B H 0.5220 0.2043 0.6774 0.486 Uiso 0.50 1 calc PR . . H31C H 0.5220 0.2957 0.6774 0.486 Uiso 0.50 1 calc PR . . C32 C 0.5163(6) 0.264(3) 0.3044(8) 0.106(9) Uani 0.50 1 d PDU A -1 H32A H 0.5422 0.3068 0.3147 0.127 Uiso 0.50 1 calc PR A -1 H32B H 0.5392 0.2180 0.2946 0.127 Uiso 0.50 1 calc PR A -1 C33 C 0.4846(7) 0.2819(12) 0.2319(9) 0.103(8) Uani 0.50 1 d PDU A -1 H33A H 0.4696 0.3343 0.2349 0.123 Uiso 0.50 1 calc PR A -1 H33B H 0.4530 0.2461 0.2265 0.123 Uiso 0.50 1 calc PR A -1 C34 C 0.5218(11) 0.2750(13) 0.1636(13) 0.099(9) Uani 0.50 1 d PDU A -1 H34A H 0.5025 0.2977 0.1185 0.119 Uiso 0.50 1 calc PR A -1 H34B H 0.5554 0.3063 0.1736 0.119 Uiso 0.50 1 calc PR A -1 C35 C 0.5403(12) 0.1971(17) 0.1416(15) 0.112(8) Uani 0.50 1 d PDU A -1 H35A H 0.5677 0.2005 0.0996 0.168 Uiso 0.50 1 calc PR A -1 H35B H 0.5082 0.1673 0.1240 0.168 Uiso 0.50 1 calc PR A -1 H35C H 0.5573 0.1721 0.1866 0.168 Uiso 0.50 1 calc PR A -1 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 0.0677(5) 0.0577(5) 0.0513(5) 0.0098(4) 0.0039(4) 0.0169(4) Mo2 0.0640(5) 0.0503(5) 0.0525(4) -0.0101(3) 0.0063(4) -0.0122(4) Mo3 0.0609(7) 0.0569(7) 0.0370(5) 0.000 0.0092(5) 0.000 Ti1 0.0716(14) 0.0486(12) 0.0376(10) 0.000 0.0145(10) 0.000 O1 0.173(12) 0.163(13) 0.071(8) 0.000 0.016(8) 0.000 O2 0.080(6) 0.089(7) 0.042(5) 0.000 0.019(4) 0.000 O3 0.064(5) 0.081(6) 0.054(5) 0.000 -0.005(4) 0.000 O4 0.099(5) 0.098(6) 0.082(5) 0.013(4) -0.003(4) 0.038(4) O5 0.092(5) 0.074(5) 0.092(5) -0.022(4) 0.009(4) -0.025(4) O6 0.062(5) 0.071(6) 0.053(5) 0.000 -0.007(4) 0.000 O7 0.079(6) 0.101(7) 0.044(5) 0.000 0.026(4) 0.000 O8 0.077(4) 0.066(4) 0.045(3) -0.025(3) 0.007(3) -0.011(3) O9 0.066(4) 0.069(4) 0.052(3) 0.001(3) 0.011(3) 0.020(3) O10 0.089(4) 0.061(4) 0.045(3) 0.014(3) 0.001(3) 0.005(3) O11 0.089(4) 0.038(3) 0.069(4) -0.007(3) 0.016(3) 0.000(3) O12 0.072(4) 0.056(4) 0.056(3) 0.002(3) 0.019(3) -0.009(3) O13 0.051(4) 0.036(4) 0.036(4) 0.000 0.004(3) 0.000 C1 0.090(10) 0.046(7) 0.052(8) 0.000 0.017(7) 0.000 C2 0.113(14) 0.103(13) 0.076(11) 0.000 0.025(10) 0.000 C3 0.084(12) 0.171(19) 0.105(14) 0.000 0.021(11) 0.000 C4 0.092(14) 0.165(19) 0.102(15) 0.000 0.060(12) 0.000 C5 0.151(18) 0.106(13) 0.063(10) 0.000 0.046(12) 0.000 C6 0.101(11) 0.054(8) 0.047(7) 0.000 0.032(8) 0.000 C7 0.152(15) 0.063(9) 0.043(8) 0.000 0.025(9) 0.000 N1 0.088(5) 0.051(4) 0.075(5) -0.024(4) 0.003(3) -0.004(4) C8 0.089(6) 0.069(6) 0.067(5) -0.024(5) 0.002(4) 0.003(5) C9 0.093(7) 0.086(7) 0.093(7) -0.023(6) 0.008(5) -0.009(6) C10 0.095(8) 0.148(11) 0.102(9) -0.046(8) 0.018(6) -0.039(7) C11 0.099(10) 0.231(18) 0.139(12) 0.007(12) 0.023(8) -0.048(11) C12 0.105(7) 0.062(6) 0.069(6) -0.029(5) 0.000(5) -0.014(5) C13 0.122(9) 0.092(8) 0.088(7) -0.025(6) -0.015(6) 0.005(7) C14 0.182(13) 0.110(10) 0.096(9) -0.039(7) -0.039(8) 0.017(9) C15 0.230(18) 0.135(13) 0.133(12) -0.001(10) -0.078(11) 0.007(12) C16 0.093(7) 0.060(5) 0.089(6) -0.020(5) 0.012(5) 0.006(5) C17 0.121(9) 0.103(8) 0.093(8) -0.023(7) -0.006(6) 0.012(7) C18 0.172(14) 0.138(11) 0.169(14) 0.035(11) -0.064(11) -0.003(11) C19 0.31(3) 0.34(3) 0.26(3) 0.09(2) -0.16(2) -0.01(2) C20 0.089(6) 0.064(6) 0.078(6) -0.023(5) 0.004(5) -0.014(5) C21 0.110(8) 0.102(8) 0.085(7) -0.028(6) 0.021(6) -0.015(6) C22 0.142(12) 0.119(10) 0.156(12) -0.045(9) 0.065(9) -0.040(9) C23 0.189(16) 0.186(17) 0.160(15) -0.006(13) 0.087(12) -0.022(13) N2 0.045(6) 0.176(11) 0.086(6) 0.000 -0.005(5) 0.000 C24 0.076(8) 0.201(11) 0.107(9) 0.017(10) -0.005(7) 0.022(7) C25 0.26(2) 0.176(12) 0.263(19) 0.043(16) -0.053(18) -0.004(11) C26 0.32(3) 0.213(15) 0.33(3) -0.034(18) -0.18(2) 0.044(16) C27 0.35(3) 0.39(3) 0.24(3) -0.10(2) 0.10(3) 0.00(3) C28 0.076(10) 0.172(15) 0.101(8) 0.000 -0.025(8) 0.000 C29 0.125(14) 0.25(2) 0.094(8) 0.000 -0.019(9) 0.000 C30 0.19(2) 0.32(3) 0.114(12) 0.000 -0.061(14) 0.000 C31 0.33(4) 0.52(6) 0.123(13) 0.000 -0.07(2) 0.000 C32 0.058(9) 0.17(3) 0.094(8) -0.002(15) 0.000(6) -0.020(14) C33 0.074(12) 0.14(2) 0.096(9) 0.013(11) 0.014(8) 0.004(11) C34 0.069(14) 0.13(3) 0.097(10) 0.007(14) 0.011(10) -0.010(13) C35 0.09(2) 0.15(2) 0.094(19) 0.002(17) -0.012(15) 0.025(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 O3 1.933(4) . ? Mo1 O4 1.678(6) . ? Mo1 O9 1.941(5) . ? Mo1 O10 1.863(6) . ? Mo1 O11 1.950(6) . ? Mo1 O13 2.343(5) . ? Mo2 O5 1.684(6) . ? Mo2 O6 1.951(4) . ? Mo2 O8 1.966(5) . ? Mo2 O11 1.949(6) . ? Mo2 O12 1.828(5) . ? Mo2 O13 2.330(5) . ? Mo3 O7 1.676(7) . ? Mo3 O8 1.890(6) . ? Mo3 O8 1.890(6) 7_565 ? Mo3 O9 1.921(6) . ? Mo3 O9 1.921(6) 7_565 ? Mo3 O13 2.385(6) . ? Ti1 O2 1.890(8) . ? Ti1 O10 1.917(6) . ? Ti1 O10 1.917(6) 7_565 ? Ti1 O12 1.964(6) . ? Ti1 O12 1.964(6) 7_565 ? Ti1 O13 2.075(6) . ? O1 C7 1.192(15) . ? O2 C1 1.315(15) . ? O3 Mo1 1.933(4) 7_565 ? O6 Mo2 1.951(4) 7_565 ? O13 Mo1 2.343(5) 7_565 ? O13 Mo2 2.330(5) 7_565 ? C1 C2 1.406(19) . ? C1 C6 1.370(16) . ? C2 H2 0.950 . ? C2 C3 1.40(2) . ? C3 H3 0.950 . ? C3 C4 1.39(2) . ? C4 H4 0.950 . ? C4 C5 1.31(2) . ? C5 H5 0.950 . ? C5 C6 1.39(2) . ? C6 C7 1.45(2) . ? C7 H7 0.950 . ? N1 C8 1.512(9) . ? N1 C12 1.522(9) . ? N1 C16 1.517(9) . ? N1 C20 1.519(9) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C8 C9 1.496(10) . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.497(10) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.472(11) . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.486(10) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 C14 1.485(10) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.470(11) . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.494(10) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.512(11) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C18 C19 1.451(13) . ? C19 H19A 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.487(10) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.502(11) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.484(11) . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? N2 C24 1.510(10) . ? N2 C24 1.510(10) 7_565 ? N2 C28 1.527(12) . ? N2 C32 1.540(12) . ? N2 C32 1.540(12) 7_565 ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C24 C25 1.485(13) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C25 C26 1.471(13) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C26 C27 1.393(14) . ? C27 H27A 0.980 . ? C27 H27B 0.980 . ? C27 H27C 0.980 . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C28 C29 1.483(13) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C29 C30 1.523(13) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C30 C31 1.442(14) . ? C31 H31A 0.980 . ? C31 H31B 0.980 . ? C31 H31C 0.980 . ? C32 H32A 0.990 . ? C32 H32B 0.990 . ? C32 C33 1.497(13) . ? C33 H33A 0.990 . ? C33 H33B 0.990 . ? C33 C34 1.483(13) . ? C34 H34A 0.990 . ? C34 H34B 0.990 . ? C34 C35 1.485(14) . ? C35 H35A 0.980 . ? C35 H35B 0.980 . ? C35 H35C 0.980 . ? 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 O3 Mo1 O4 102.0(3) . . ? O3 Mo1 O9 85.2(3) . . ? O3 Mo1 O10 88.1(3) . . ? O3 Mo1 O11 153.0(3) . . ? O3 Mo1 O13 76.4(2) . . ? O4 Mo1 O9 103.3(3) . . ? O4 Mo1 O10 104.2(3) . . ? O4 Mo1 O11 104.8(3) . . ? O4 Mo1 O13 178.4(3) . . ? O9 Mo1 O10 152.4(2) . . ? O9 Mo1 O11 85.6(2) . . ? O9 Mo1 O13 76.8(2) . . ? O10 Mo1 O11 88.5(2) . . ? O10 Mo1 O13 75.7(2) . . ? O11 Mo1 O13 76.8(2) . . ? O5 Mo2 O6 101.5(3) . . ? O5 Mo2 O8 102.3(3) . . ? O5 Mo2 O11 104.1(3) . . ? O5 Mo2 O12 105.3(3) . . ? O5 Mo2 O13 178.1(3) . . ? O6 Mo2 O8 84.6(3) . . ? O6 Mo2 O11 153.8(3) . . ? O6 Mo2 O12 89.5(3) . . ? O6 Mo2 O13 77.2(2) . . ? O8 Mo2 O11 84.3(2) . . ? O8 Mo2 O12 152.4(2) . . ? O8 Mo2 O13 76.2(2) . . ? O11 Mo2 O12 89.4(3) . . ? O11 Mo2 O13 77.1(2) . . ? O12 Mo2 O13 76.2(2) . . ? O7 Mo3 O8 104.0(3) . . ? O7 Mo3 O8 104.0(3) . 7_565 ? O7 Mo3 O9 103.7(3) . . ? O7 Mo3 O9 103.7(3) . 7_565 ? O7 Mo3 O13 179.7(4) . . ? O8 Mo3 O8 87.8(4) . 7_565 ? O8 Mo3 O9 86.9(3) . . ? O8 Mo3 O9 152.3(2) 7_565 . ? O8 Mo3 O9 152.3(2) . 7_565 ? O8 Mo3 O9 86.9(3) 7_565 7_565 ? O8 Mo3 O13 76.21(18) . . ? O8 Mo3 O13 76.21(18) 7_565 . ? O9 Mo3 O9 85.2(4) . 7_565 ? O9 Mo3 O13 76.08(19) . . ? O9 Mo3 O13 76.08(19) 7_565 . ? O2 Ti1 O10 101.1(3) . . ? O2 Ti1 O10 101.1(3) . 7_565 ? O2 Ti1 O12 97.4(3) . . ? O2 Ti1 O12 97.4(3) . 7_565 ? O2 Ti1 O13 176.2(3) . . ? O10 Ti1 O10 90.1(4) . 7_565 ? O10 Ti1 O12 88.5(3) . . ? O10 Ti1 O12 161.3(2) 7_565 . ? O10 Ti1 O12 161.3(2) . 7_565 ? O10 Ti1 O12 88.5(3) 7_565 7_565 ? O10 Ti1 O13 81.5(2) . . ? O10 Ti1 O13 81.5(2) 7_565 . ? O12 Ti1 O12 86.9(4) . 7_565 ? O12 Ti1 O13 79.9(2) . . ? O12 Ti1 O13 79.9(2) 7_565 . ? Ti1 O2 C1 143.5(9) . . ? Mo1 O3 Mo1 117.5(4) . 7_565 ? Mo2 O6 Mo2 115.4(4) . 7_565 ? Mo2 O8 Mo3 118.3(2) . . ? Mo1 O9 Mo3 118.2(3) . . ? Mo1 O10 Ti1 112.4(3) . . ? Mo1 O11 Mo2 116.0(3) . . ? Mo2 O12 Ti1 112.6(3) . . ? Mo1 O13 Mo1 89.7(2) . 7_565 ? Mo1 O13 Mo2 90.05(3) . . ? Mo1 O13 Mo2 178.2(3) . 7_565 ? Mo1 O13 Mo2 90.04(3) 7_565 7_565 ? Mo1 O13 Mo2 178.2(3) 7_565 . ? Mo1 O13 Mo3 88.97(18) . . ? Mo1 O13 Mo3 88.97(18) 7_565 . ? Mo1 O13 Ti1 90.5(2) . . ? Mo1 O13 Ti1 90.5(2) 7_565 . ? Mo2 O13 Mo2 90.1(2) . 7_565 ? Mo2 O13 Mo3 89.22(18) . . ? Mo2 O13 Mo3 89.22(18) 7_565 . ? Mo2 O13 Ti1 91.3(2) . . ? Mo2 O13 Ti1 91.3(2) 7_565 . ? Mo3 O13 Ti1 179.2(3) . . ? O2 C1 C2 120.7(12) . . ? O2 C1 C6 121.2(14) . . ? C2 C1 C6 118.1(14) . . ? C1 C2 H2 119.7 . . ? C1 C2 C3 120.7(15) . . ? H2 C2 C3 119.7 . . ? C2 C3 H3 120.8 . . ? C2 C3 C4 118.4(18) . . ? H3 C3 C4 120.8 . . ? C3 C4 H4 119.6 . . ? C3 C4 C5 120.9(17) . . ? H4 C4 C5 119.6 . . ? C4 C5 H5 119.0 . . ? C4 C5 C6 122.0(16) . . ? H5 C5 C6 119.0 . . ? C1 C6 C5 119.9(16) . . ? C1 C6 C7 120.3(13) . . ? C5 C6 C7 119.9(14) . . ? O1 C7 C6 126.0(17) . . ? O1 C7 H7 117.0 . . ? C6 C7 H7 117.0 . . ? C8 N1 C12 111.3(7) . . ? C8 N1 C16 110.8(7) . . ? C8 N1 C20 107.0(6) . . ? C12 N1 C16 106.8(6) . . ? C12 N1 C20 110.2(7) . . ? C16 N1 C20 110.8(7) . . ? N1 C8 H8A 108.1 . . ? N1 C8 H8B 108.1 . . ? N1 C8 C9 116.7(7) . . ? H8A C8 H8B 107.3 . . ? H8A C8 C9 108.1 . . ? H8B C8 C9 108.1 . . ? C8 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C8 C9 C10 112.5(8) . . ? H9A C9 H9B 107.8 . . ? H9A C9 C10 109.1 . . ? H9B C9 C10 109.1 . . ? C9 C10 H10A 108.4 . . ? C9 C10 H10B 108.4 . . ? C9 C10 C11 115.3(11) . . ? H10A C10 H10B 107.5 . . ? H10A C10 C11 108.4 . . ? H10B C10 C11 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 108.4 . . ? N1 C12 H12B 108.4 . . ? N1 C12 C13 115.7(7) . . ? H12A C12 H12B 107.4 . . ? H12A C12 C13 108.4 . . ? H12B C12 C13 108.4 . . ? C12 C13 H13A 108.3 . . ? C12 C13 H13B 108.3 . . ? C12 C13 C14 115.7(9) . . ? H13A C13 H13B 107.4 . . ? H13A C13 C14 108.3 . . ? H13B C13 C14 108.3 . . ? C13 C14 H14A 108.0 . . ? C13 C14 H14B 108.0 . . ? C13 C14 C15 117.1(10) . . ? H14A C14 H14B 107.3 . . ? H14A C14 C15 108.0 . . ? H14B C14 C15 108.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 H16A 107.9 . . ? N1 C16 H16B 107.9 . . ? N1 C16 C17 117.7(8) . . ? H16A C16 H16B 107.2 . . ? H16A C16 C17 107.9 . . ? H16B C16 C17 107.9 . . ? C16 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? C16 C17 C18 110.0(9) . . ? H17A C17 H17B 108.2 . . ? H17A C17 C18 109.7 . . ? H17B C17 C18 109.7 . . ? C17 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? C17 C18 C19 114.1(14) . . ? H18A C18 H18B 107.6 . . ? H18A C18 C19 108.7 . . ? H18B C18 C19 108.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 107.9 . . ? N1 C20 H20B 107.9 . . ? N1 C20 C21 117.6(7) . . ? H20A C20 H20B 107.2 . . ? H20A C20 C21 107.9 . . ? H20B C20 C21 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 C22 110.9(9) . . ? H21A C21 H21B 108.0 . . ? H21A C21 C22 109.5 . . ? H21B C21 C22 109.5 . . ? C21 C22 H22A 108.5 . . ? C21 C22 H22B 108.5 . . ? C21 C22 C23 115.3(11) . . ? H22A C22 H22B 107.5 . . ? H22A C22 C23 108.5 . . ? H22B C22 C23 108.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 N2 C24 106.2(12) . 7_565 ? C24 N2 C28 111.2(8) . . ? C24 N2 C28 111.2(8) 7_565 . ? C24 N2 C32 103.1(18) . . ? C24 N2 C32 118.8(19) 7_565 . ? C24 N2 C32 118.8(19) . 7_565 ? C24 N2 C32 103.1(18) 7_565 7_565 ? C28 N2 C32 106.2(10) . . ? C28 N2 C32 106.2(10) . 7_565 ? N2 C24 H24A 108.3 . . ? N2 C24 H24B 108.3 . . ? N2 C24 C25 115.7(11) . . ? H24A C24 H24B 107.4 . . ? H24A C24 C25 108.3 . . ? H24B C24 C25 108.3 . . ? C24 C25 H25A 110.7 . . ? C24 C25 H25B 110.7 . . ? C24 C25 C26 105.2(15) . . ? H25A C25 H25B 108.8 . . ? H25A C25 C26 110.7 . . ? H25B C25 C26 110.7 . . ? C25 C26 H26A 105.8 . . ? C25 C26 H26B 105.8 . . ? C25 C26 C27 126(2) . . ? H26A C26 H26B 106.2 . . ? H26A C26 C27 105.8 . . ? H26B C26 C27 105.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 H28A 107.4 . . ? N2 C28 H28B 107.4 . . ? N2 C28 C29 119.5(12) . . ? H28A C28 H28B 107.0 . . ? H28A C28 C29 107.4 . . ? H28B C28 C29 107.4 . . ? C28 C29 H29A 110.2 . . ? C28 C29 H29B 110.2 . . ? C28 C29 C30 107.5(13) . . ? H29A C29 H29B 108.5 . . ? H29A C29 C30 110.2 . . ? H29B C29 C30 110.2 . . ? C29 C30 H30A 107.7 . . ? C29 C30 H30B 107.7 . . ? C29 C30 C31 118.6(19) . . ? H30A C30 H30B 107.1 . . ? H30A C30 C31 107.7 . . ? H30B C30 C31 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 H32A 108.1 . . ? N2 C32 H32B 108.1 . . ? N2 C32 C33 116.7(12) . . ? H32A C32 H32B 107.3 . . ? H32A C32 C33 108.1 . . ? H32B C32 C33 108.1 . . ? C32 C33 H33A 109.7 . . ? C32 C33 H33B 109.7 . . ? C32 C33 C34 109.8(15) . . ? H33A C33 H33B 108.2 . . ? H33A C33 C34 109.7 . . ? H33B C33 C34 109.7 . . ? C33 C34 H34A 108.0 . . ? C33 C34 H34B 108.0 . . ? C33 C34 C35 117.2(15) . . ? H34A C34 H34B 107.2 . . ? H34A C34 C35 108.0 . . ? H34B C34 C35 108.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.003 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.160 # Contents of RES file _computing_special_details ; TITL rje286 in Pnma CELL 0.71073 24.0494 17.5205 17.2421 90.000 90.000 90.000 ZERR 4.00 0.0037 0.0032 0.0029 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC C H N O TI MO UNIT 220 452 12 80 4 20 SIZE 0.3 0.2 0.2 TEMP -113 SHEL 5.8 0 L.S. 24 ACTA BOND $H FMAP 2 PLAN 10 SIMU N1 > C35 DELU N1 > C35 CONN $MO $TI 6 SADI C8 C9 C9 C10 C10 C11 SADI C12 C13 C13 C14 C14 C15 SADI C16 C17 C17 C18 C18 C19 SADI C20 C21 C21 C22 C22 C23 SADI C24 C25 C25 C26 C26 C27 SADI C28 C29 C29 C30 C30 C31 SADI C32 C33 C33 C34 C34 C35 WGHT 0.119300 EXTI 0.004713 FVAR 0.03978 MO1 6 0.186770 0.344319 0.118541 11.00000 0.06767 0.05765 = 0.05128 0.00981 0.00390 0.01685 MO2 6 0.308761 0.344139 0.206840 11.00000 0.06398 0.05026 = 0.05249 -0.01011 0.00631 -0.01220 MO3 6 0.202803 0.250000 0.283584 10.50000 0.06090 0.05692 = 0.03700 0.00000 0.00922 0.00000 TI1 5 0.287644 0.250000 0.053605 10.50000 0.07161 0.04862 = 0.03761 0.00000 0.01454 0.00000 O1 4 0.341321 0.250000 -0.270412 10.50000 0.17329 0.16306 = 0.07069 0.00000 0.01592 0.00000 O2 4 0.327601 0.250000 -0.040799 10.50000 0.08031 0.08945 = 0.04230 0.00000 0.01888 0.00000 O3 4 0.149220 0.250000 0.093223 10.50000 0.06411 0.08087 = 0.05384 0.00000 -0.00466 0.00000 O4 4 0.141272 0.409994 0.087137 11.00000 0.09881 0.09764 = 0.08187 0.01321 -0.00272 0.03771 O5 4 0.352236 0.410607 0.242853 11.00000 0.09156 0.07443 = 0.09158 -0.02196 0.00872 -0.02537 O6 4 0.345235 0.250000 0.239462 10.50000 0.06160 0.07087 = 0.05296 0.00000 -0.00700 0.00000 O7 4 0.170204 0.250000 0.369524 10.50000 0.07863 0.10112 = 0.04384 0.00000 0.02577 0.00000 O8 4 0.258839 0.324776 0.294971 11.00000 0.07662 0.06608 = 0.04513 -0.02534 0.00669 -0.01074 O9 4 0.162482 0.324244 0.223938 11.00000 0.06633 0.06876 = 0.05178 0.00108 0.01117 0.02003 O10 4 0.233140 0.327418 0.033675 11.00000 0.08883 0.06051 = 0.04540 0.01404 0.00122 0.00535 O11 4 0.246538 0.403080 0.166195 11.00000 0.08947 0.03765 = 0.06869 -0.00741 0.01578 0.00048 O12 4 0.332539 0.327094 0.107650 11.00000 0.07206 0.05566 = 0.05564 0.00199 0.01917 -0.00854 O13 4 0.248756 0.250000 0.161005 10.50000 0.05056 0.03650 = 0.03606 0.00000 0.00359 0.00000 C1 1 0.377957 0.250000 -0.070473 10.50000 0.09036 0.04555 = 0.05198 0.00000 0.01744 0.00000 C2 1 0.425050 0.250000 -0.022117 10.50000 0.11335 0.10281 = 0.07597 0.00000 0.02483 0.00000 AFIX 43 H2 2 0.420437 0.250000 0.032604 10.50000 -1.20000 AFIX 0 C3 1 0.478468 0.250000 -0.053665 10.50000 0.08400 0.17103 = 0.10453 0.00000 0.02120 0.00000 AFIX 43 H3 2 0.510315 0.250000 -0.021067 10.50000 -1.20000 AFIX 0 C4 1 0.483989 0.250000 -0.133720 10.50000 0.09194 0.16543 = 0.10162 0.00000 0.05965 0.00000 AFIX 43 H4 2 0.520056 0.250000 -0.156192 10.50000 -1.20000 AFIX 0 C5 1 0.440034 0.250000 -0.178862 10.50000 0.15119 0.10560 = 0.06281 0.00000 0.04587 0.00000 AFIX 43 H5 2 0.445108 0.250000 -0.233504 10.50000 -1.20000 AFIX 0 C6 1 0.386161 0.250000 -0.149105 10.50000 0.10071 0.05436 = 0.04735 0.00000 0.03231 0.00000 C7 1 0.339123 0.250000 -0.201352 10.50000 0.15187 0.06331 = 0.04299 0.00000 0.02494 0.00000 AFIX 43 H7 2 0.303167 0.250000 -0.178536 10.50000 -1.20000 AFIX 0 SAME N1 C12 > C15 SAME N1 C16 > C19 SAME N1 C20 > C23 SAME N2 C24 > C27 SAME N2 C28 > C31 SAME N2 C32 > C35 N1 3 0.188957 0.503916 0.413363 11.00000 0.08791 0.05133 = 0.07484 -0.02410 0.00313 -0.00423 C8 1 0.152222 0.535878 0.476714 11.00000 0.08926 0.06857 = 0.06705 -0.02441 0.00227 0.00333 AFIX 23 H8A 2 0.176494 0.556393 0.518140 11.00000 -1.20000 H8B 2 0.131060 0.579345 0.454928 11.00000 -1.20000 AFIX 0 C9 1 0.111713 0.481842 0.513101 11.00000 0.09270 0.08581 = 0.09300 -0.02255 0.00760 -0.00877 AFIX 23 H9A 2 0.132447 0.439990 0.538631 11.00000 -1.20000 H9B 2 0.088224 0.459028 0.472040 11.00000 -1.20000 AFIX 0 C10 1 0.075111 0.520008 0.571656 11.00000 0.09544 0.14804 = 0.10168 -0.04616 0.01780 -0.03917 AFIX 23 H10A 2 0.099029 0.546734 0.609686 11.00000 -1.20000 H10B 2 0.052555 0.559188 0.544788 11.00000 -1.20000 AFIX 0 C11 1 0.037291 0.468933 0.614225 11.00000 0.09920 0.23102 = 0.13941 0.00663 0.02307 -0.04763 AFIX 33 H11A 2 0.014720 0.498955 0.650401 11.00000 -1.50000 H11B 2 0.059087 0.431248 0.643207 11.00000 -1.50000 H11C 2 0.012888 0.442592 0.577407 11.00000 -1.50000 AFIX 0 C12 1 0.154742 0.477539 0.344089 11.00000 0.10491 0.06191 = 0.06900 -0.02924 0.00020 -0.01410 AFIX 23 H12A 2 0.180270 0.454627 0.305528 11.00000 -1.20000 H12B 2 0.129120 0.436838 0.361671 11.00000 -1.20000 AFIX 0 C13 1 0.121460 0.537645 0.304764 11.00000 0.12185 0.09165 = 0.08787 -0.02511 -0.01467 0.00507 AFIX 23 H13A 2 0.146777 0.579716 0.289857 11.00000 -1.20000 H13B 2 0.094447 0.558509 0.342549 11.00000 -1.20000 AFIX 0 C14 1 0.090489 0.512849 0.234618 11.00000 0.18190 0.11039 = 0.09554 -0.03910 -0.03933 0.01706 AFIX 23 H14A 2 0.117351 0.489172 0.198368 11.00000 -1.20000 H14B 2 0.063868 0.472625 0.250349 11.00000 -1.20000 AFIX 0 C15 1 0.059527 0.571782 0.192013 11.00000 0.22952 0.13456 = 0.13300 -0.00082 -0.07832 0.00670 AFIX 33 H15A 2 0.040857 0.548564 0.147339 11.00000 -1.50000 H15B 2 0.085347 0.611236 0.173952 11.00000 -1.50000 H15C 2 0.031731 0.594842 0.226341 11.00000 -1.50000 AFIX 0 C16 1 0.220962 0.434905 0.442240 11.00000 0.09347 0.06023 = 0.08946 -0.02036 0.01196 0.00626 AFIX 23 H16A 2 0.193751 0.394113 0.453994 11.00000 -1.20000 H16B 2 0.244588 0.416321 0.399180 11.00000 -1.20000 AFIX 0 C17 1 0.257193 0.445080 0.511870 11.00000 0.12135 0.10277 = 0.09345 -0.02316 -0.00569 0.01168 AFIX 23 H17A 2 0.235526 0.468926 0.554253 11.00000 -1.20000 H17B 2 0.288600 0.479327 0.498956 11.00000 -1.20000 AFIX 0 C18 1 0.279313 0.368596 0.538317 11.00000 0.17234 0.13762 = 0.16916 0.03504 -0.06429 -0.00293 AFIX 23 H18A 2 0.247859 0.337375 0.557437 11.00000 -1.20000 H18B 2 0.295606 0.341857 0.493129 11.00000 -1.20000 AFIX 0 C19 1 0.321016 0.373519 0.598912 11.00000 0.31201 0.33847 = 0.26183 0.09194 -0.16383 -0.01045 AFIX 33 H19A 2 0.333855 0.322105 0.612343 11.00000 -1.50000 H19B 2 0.304827 0.397811 0.644861 11.00000 -1.50000 H19C 2 0.352537 0.403965 0.580462 11.00000 -1.50000 AFIX 0 C20 1 0.228448 0.567272 0.389212 11.00000 0.08920 0.06443 = 0.07814 -0.02283 0.00405 -0.01410 AFIX 23 H20A 2 0.205813 0.612207 0.374545 11.00000 -1.20000 H20B 2 0.250682 0.581902 0.435190 11.00000 -1.20000 AFIX 0 C21 1 0.267629 0.551206 0.324526 11.00000 0.11008 0.10189 = 0.08546 -0.02846 0.02062 -0.01482 AFIX 23 H21A 2 0.246639 0.531597 0.279330 11.00000 -1.20000 H21B 2 0.294390 0.511365 0.340789 11.00000 -1.20000 AFIX 0 C22 1 0.298759 0.622003 0.301537 11.00000 0.14167 0.11929 = 0.15572 -0.04514 0.06453 -0.04017 AFIX 23 H22A 2 0.271420 0.661674 0.286782 11.00000 -1.20000 H22B 2 0.319329 0.641033 0.347359 11.00000 -1.20000 AFIX 0 C23 1 0.338686 0.612303 0.236691 11.00000 0.18946 0.18635 = 0.15963 -0.00613 0.08704 -0.02230 AFIX 33 H23A 2 0.356617 0.661301 0.225463 11.00000 -1.50000 H23B 2 0.318812 0.594470 0.190499 11.00000 -1.50000 H23C 2 0.367004 0.574731 0.251277 11.00000 -1.50000 AFIX 0 N2 3 0.481792 0.250000 0.378213 10.50000 0.04527 0.17609 = 0.08635 0.00000 -0.00482 0.00000 C24 1 0.444141 0.318913 0.381472 11.00000 0.07630 0.20065 = 0.10738 0.01715 -0.00461 0.02201 AFIX 23 H24A 2 0.419276 0.317660 0.335730 11.00000 -1.20000 H24B 2 0.420455 0.314636 0.428230 11.00000 -1.20000 AFIX 0 C25 1 0.472577 0.394140 0.383307 11.00000 0.25627 0.17563 = 0.26286 0.04281 -0.05314 -0.00423 AFIX 23 H25A 2 0.493657 0.402784 0.334778 11.00000 -1.20000 H25B 2 0.498579 0.397083 0.427720 11.00000 -1.20000 AFIX 0 C26 1 0.427743 0.450688 0.391508 11.00000 0.31904 0.21254 = 0.32547 -0.03351 -0.18038 0.04409 AFIX 23 H26A 2 0.422425 0.472955 0.339260 11.00000 -1.20000 H26B 2 0.393649 0.421043 0.402819 11.00000 -1.20000 AFIX 0 C27 1 0.427225 0.512094 0.442839 11.00000 0.35032 0.38599 = 0.24394 -0.09751 0.10294 0.00215 AFIX 33 H27A 2 0.396196 0.546098 0.430051 11.00000 -1.50000 H27B 2 0.462318 0.540219 0.438610 11.00000 -1.50000 H27C 2 0.422797 0.493160 0.495963 11.00000 -1.50000 AFIX 0 C28 1 0.523026 0.250000 0.445564 10.50000 0.07582 0.17212 = 0.10124 0.00000 -0.02493 0.00000 AFIX 23 H28A 2 0.547132 0.204590 0.439473 10.50000 -1.20000 H28B 2 0.547132 0.295410 0.439473 10.50000 -1.20000 AFIX 0 C29 1 0.501972 0.250000 0.526436 10.50000 0.12487 0.25047 = 0.09381 0.00000 -0.01886 0.00000 AFIX 23 H29A 2 0.478887 0.204142 0.535851 10.50000 -1.20000 H29B 2 0.478887 0.295858 0.535851 10.50000 -1.20000 AFIX 0 C30 1 0.552253 0.250000 0.580145 10.50000 0.19218 0.32214 = 0.11409 0.00000 -0.06138 0.00000 AFIX 23 H30A 2 0.574960 0.204557 0.567441 10.50000 -1.20000 H30B 2 0.574960 0.295443 0.567441 10.50000 -1.20000 AFIX 0 C31 1 0.543035 0.250000 0.662808 10.50000 0.32514 0.52454 = 0.12287 0.00000 -0.07277 0.00000 AFIX 33 H31A 2 0.578910 0.250000 0.689764 10.50000 -1.50000 H31B 2 0.521966 0.204330 0.677410 10.50000 -1.50000 H31C 2 0.521966 0.295670 0.677410 10.50000 -1.50000 AFIX 0 PART -1 C32 1 0.516319 0.264004 0.304374 10.50000 0.05771 0.16653 = 0.09447 -0.00176 0.00000 -0.01984 AFIX 23 H32A 2 0.542161 0.306805 0.314666 10.50000 -1.20000 H32B 2 0.539213 0.218039 0.294601 10.50000 -1.20000 AFIX 0 C33 1 0.484631 0.281852 0.231906 10.50000 0.07360 0.13848 = 0.09649 0.01329 0.01422 0.00372 AFIX 23 H33A 2 0.469551 0.334347 0.234898 10.50000 -1.20000 H33B 2 0.453018 0.246052 0.226509 10.50000 -1.20000 AFIX 0 C34 1 0.521812 0.275018 0.163609 10.50000 0.06884 0.13237 = 0.09690 0.00718 0.01104 -0.00952 AFIX 23 H34A 2 0.502491 0.297717 0.118459 10.50000 -1.20000 H34B 2 0.555351 0.306284 0.173560 10.50000 -1.20000 AFIX 0 C35 1 0.540310 0.197100 0.141593 10.50000 0.09284 0.14896 = 0.09418 0.00183 -0.01194 0.02477 AFIX 33 H35A 2 0.567665 0.200541 0.099610 10.50000 -1.50000 H35B 2 0.508221 0.167266 0.124041 10.50000 -1.50000 H35C 2 0.557252 0.172079 0.186601 10.50000 -1.50000 HKLF 4 REM rje286 in Pnma REM R1 = 0.0748 for 3755 Fo > 4sig(Fo) and 0.2085 for all 9237 data REM 428 parameters refined using 520 restraints END WGHT 0.1209 0.0000 REM Highest difference peak 1.003, deepest hole -0.881, 1-sigma level 0.160 Q1 1 0.5800 0.2368 0.5988 11.00000 0.05 1.00 Q2 1 0.3176 0.3294 0.5187 11.00000 0.05 0.84 Q3 1 0.1939 0.3752 0.0796 11.00000 0.05 0.83 Q4 1 0.3002 0.3501 0.2568 11.00000 0.05 0.75 Q5 1 0.3294 0.4111 0.2036 11.00000 0.05 0.74 Q6 1 0.3573 0.3757 0.2066 11.00000 0.05 0.73 Q7 1 0.3367 0.3496 0.2599 11.00000 0.05 0.69 Q8 1 0.4128 0.5109 0.3961 11.00000 0.05 0.69 Q9 1 0.3207 0.2500 -0.0004 10.50000 0.05 0.68 Q10 1 0.2990 0.3141 0.2402 11.00000 0.05 0.68 ; #===END data_rje260_salt_of_7 _database_code_depnum_ccdc_archive 'CCDC 832956' #TrackingRef '- TiMo5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '6 C16 H36 N +,Mo10 O37 Ti2 6-,2 C2 H3 N' _chemical_formula_sum 'C100 H222 Mo10 N8 O37 Ti2' _chemical_formula_weight 3184.06 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' Ti Ti 0.2776 0.4457 '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 tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 16.1864(17) _cell_length_b 16.1864(17) _cell_length_c 50.752(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13297(3) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 7931 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.43 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6552 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 114405 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -67 _diffrn_reflns_limit_l_max 67 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.67 _reflns_number_total 15970 _reflns_number_gt 14323 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0323P)^2^+26.3651P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000182(12) _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 -0.03(3) _refine_ls_number_reflns 15970 _refine_ls_number_parameters 724 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.49017(4) 0.49560(4) 0.464325(12) 0.01449(13) Uani 1 1 d . . . Mo2 Mo 0.33777(2) 0.48659(2) 0.424671(7) 0.01904(8) Uani 1 1 d . . . Mo3 Mo 0.49026(2) 0.35051(2) 0.421506(7) 0.01903(8) Uani 1 1 d . . . Mo4 Mo 0.62355(2) 0.50432(2) 0.417960(7) 0.01901(8) Uani 1 1 d . . . Mo5 Mo 0.47220(2) 0.64001(2) 0.421643(7) 0.01797(8) Uani 1 1 d . . . Mo6 Mo 0.47004(2) 0.49480(2) 0.375597(6) 0.02226(8) Uani 1 1 d . . . O1 O 0.49758(18) 0.49758(18) 0.5000 0.0246(9) Uani 1 2 d S . . O2 O 0.23405(19) 0.4706(2) 0.42652(6) 0.0275(7) Uani 1 1 d . . . O3 O 0.5016(2) 0.24639(18) 0.42041(7) 0.0314(7) Uani 1 1 d . . . O4 O 0.72729(19) 0.5184(2) 0.41449(6) 0.0294(7) Uani 1 1 d . . . O5 O 0.4582(2) 0.74395(19) 0.42159(7) 0.0293(7) Uani 1 1 d . . . O6 O 0.4620(2) 0.4963(2) 0.34242(6) 0.0362(8) Uani 1 1 d . . . O7 O 0.48097(15) 0.49561(16) 0.42149(5) 0.0148(5) Uani 1 1 d . . . O12 O 0.37227(17) 0.48049(18) 0.45960(5) 0.0211(6) Uani 1 1 d . . . O13 O 0.50525(18) 0.37764(17) 0.45664(5) 0.0199(6) Uani 1 1 d . . . O14 O 0.60573(16) 0.51073(18) 0.45395(5) 0.0190(6) Uani 1 1 d . . . O15 O 0.47356(18) 0.61359(17) 0.45725(5) 0.0184(6) Uani 1 1 d . . . O23 O 0.37695(18) 0.36564(18) 0.42270(6) 0.0206(6) Uani 1 1 d . . . O25 O 0.35028(18) 0.60060(19) 0.42330(6) 0.0227(6) Uani 1 1 d . . . O26 O 0.35772(18) 0.48041(19) 0.38700(6) 0.0251(7) Uani 1 1 d . . . O34 O 0.61005(18) 0.38986(18) 0.41700(6) 0.0227(7) Uani 1 1 d . . . O36 O 0.4870(2) 0.38085(19) 0.38383(6) 0.0258(7) Uani 1 1 d . . . O45 O 0.58466(19) 0.62569(19) 0.41751(6) 0.0245(7) Uani 1 1 d . . . O46 O 0.5859(2) 0.5108(2) 0.38167(5) 0.0274(7) Uani 1 1 d . . . O56 O 0.4567(2) 0.60968(19) 0.38467(6) 0.0240(7) Uani 1 1 d . . . N1 N 0.7659(2) 0.7957(2) 0.40762(7) 0.0194(7) Uani 1 1 d . . . C111 C 0.7389(3) 0.8443(3) 0.38340(8) 0.0229(9) Uani 1 1 d . . . H11A H 0.7836 0.8413 0.3701 0.027 Uiso 1 1 calc R . . H11B H 0.7327 0.9031 0.3885 0.027 Uiso 1 1 calc R . . C112 C 0.6587(3) 0.8159(3) 0.37055(9) 0.0298(10) Uani 1 1 d . . . H11C H 0.6633 0.7569 0.3656 0.036 Uiso 1 1 calc R . . H11D H 0.6126 0.8216 0.3832 0.036 Uiso 1 1 calc R . . C113 C 0.6410(3) 0.8675(3) 0.34613(9) 0.0286(10) Uani 1 1 d . . . H11E H 0.6367 0.9263 0.3513 0.034 Uiso 1 1 calc R . . H11F H 0.6881 0.8623 0.3338 0.034 Uiso 1 1 calc R . . C114 C 0.5623(3) 0.8424(4) 0.33200(11) 0.0421(14) Uani 1 1 d . . . H11G H 0.5656 0.7839 0.3271 0.063 Uiso 1 1 calc R . . H11H H 0.5557 0.8760 0.3161 0.063 Uiso 1 1 calc R . . H11I H 0.5149 0.8511 0.3437 0.063 Uiso 1 1 calc R . . C121 C 0.6974(3) 0.7949(3) 0.42821(8) 0.0220(9) Uani 1 1 d . . . H12A H 0.6467 0.7723 0.4200 0.026 Uiso 1 1 calc R . . H12B H 0.7137 0.7571 0.4426 0.026 Uiso 1 1 calc R . . C122 C 0.6776(3) 0.8784(3) 0.43988(10) 0.0332(11) Uani 1 1 d . . . H12C H 0.6683 0.9187 0.4255 0.040 Uiso 1 1 calc R . . H12D H 0.7252 0.8979 0.4505 0.040 Uiso 1 1 calc R . . C123 C 0.6016(3) 0.8746(4) 0.45718(11) 0.0386(13) Uani 1 1 d . . . H12E H 0.5530 0.8608 0.4462 0.046 Uiso 1 1 calc R . . H12F H 0.6086 0.8299 0.4703 0.046 Uiso 1 1 calc R . . C124 C 0.5856(5) 0.9549(5) 0.47138(15) 0.064(2) Uani 1 1 d . . . H12G H 0.6353 0.9714 0.4810 0.097 Uiso 1 1 calc R . . H12H H 0.5398 0.9476 0.4838 0.097 Uiso 1 1 calc R . . H12I H 0.5713 0.9978 0.4585 0.097 Uiso 1 1 calc R . . C131 C 0.8430(3) 0.8386(3) 0.41817(8) 0.0223(9) Uani 1 1 d . . . H13A H 0.8855 0.8387 0.4041 0.027 Uiso 1 1 calc R . . H13B H 0.8290 0.8968 0.4221 0.027 Uiso 1 1 calc R . . C132 C 0.8801(3) 0.8002(3) 0.44271(10) 0.0304(11) Uani 1 1 d . . . H13C H 0.8356 0.7874 0.4555 0.036 Uiso 1 1 calc R . . H13D H 0.9080 0.7478 0.4380 0.036 Uiso 1 1 calc R . . C133 C 0.9414(4) 0.8581(4) 0.45523(12) 0.0478(15) Uani 1 1 d . . . H13E H 0.9130 0.9099 0.4603 0.057 Uiso 1 1 calc R . . H13F H 0.9849 0.8721 0.4423 0.057 Uiso 1 1 calc R . . C134 C 0.9813(4) 0.8196(5) 0.47960(11) 0.0574(18) Uani 1 1 d . . . H13G H 0.9381 0.8029 0.4920 0.086 Uiso 1 1 calc R . . H13H H 1.0177 0.8601 0.4880 0.086 Uiso 1 1 calc R . . H13I H 1.0136 0.7711 0.4744 0.086 Uiso 1 1 calc R . . C141 C 0.7834(3) 0.7062(3) 0.40096(9) 0.0235(9) Uani 1 1 d . . . H14A H 0.7312 0.6802 0.3950 0.028 Uiso 1 1 calc R . . H14B H 0.8007 0.6775 0.4173 0.028 Uiso 1 1 calc R . . C142 C 0.8488(3) 0.6915(3) 0.38000(9) 0.0256(10) Uani 1 1 d . . . H14C H 0.9016 0.7172 0.3855 0.031 Uiso 1 1 calc R . . H14D H 0.8313 0.7172 0.3632 0.031 Uiso 1 1 calc R . . C143 C 0.8610(3) 0.5986(3) 0.37610(10) 0.0328(11) Uani 1 1 d . . . H14E H 0.8760 0.5735 0.3932 0.039 Uiso 1 1 calc R . . H14F H 0.8078 0.5740 0.3705 0.039 Uiso 1 1 calc R . . C144 C 0.9264(4) 0.5768(3) 0.35613(11) 0.0367(13) Uani 1 1 d . . . H14G H 0.9133 0.6031 0.3393 0.055 Uiso 1 1 calc R . . H14H H 0.9281 0.5167 0.3538 0.055 Uiso 1 1 calc R . . H14I H 0.9803 0.5963 0.3623 0.055 Uiso 1 1 calc R . . N2 N 0.2182(3) 0.1883(3) 0.40662(8) 0.0277(9) Uani 1 1 d . . . C211 C 0.2497(3) 0.1422(3) 0.38251(9) 0.0292(10) Uani 1 1 d . . . H21A H 0.2097 0.1501 0.3680 0.035 Uiso 1 1 calc R . . H21B H 0.2514 0.0825 0.3867 0.035 Uiso 1 1 calc R . . C212 C 0.3348(3) 0.1685(4) 0.37288(11) 0.0400(13) Uani 1 1 d . . . H21C H 0.3363 0.2294 0.3711 0.048 Uiso 1 1 calc R . . H21D H 0.3768 0.1523 0.3861 0.048 Uiso 1 1 calc R . . C213 C 0.3556(4) 0.1300(3) 0.34685(11) 0.0401(13) Uani 1 1 d . . . H21E H 0.3145 0.1479 0.3336 0.048 Uiso 1 1 calc R . . H21F H 0.3517 0.0691 0.3485 0.048 Uiso 1 1 calc R . . C214 C 0.4409(4) 0.1526(5) 0.33736(13) 0.0560(18) Uani 1 1 d . . . H21G H 0.4486 0.2125 0.3387 0.084 Uiso 1 1 calc R . . H21H H 0.4473 0.1356 0.3189 0.084 Uiso 1 1 calc R . . H21I H 0.4823 0.1245 0.3482 0.084 Uiso 1 1 calc R . . C221 C 0.2807(3) 0.1803(3) 0.42886(10) 0.0335(11) Uani 1 1 d . . . H22A H 0.3346 0.2013 0.4226 0.040 Uiso 1 1 calc R . . H22B H 0.2628 0.2160 0.4436 0.040 Uiso 1 1 calc R . . C222 C 0.2924(3) 0.0932(3) 0.43915(11) 0.0369(12) Uani 1 1 d . . . H22C H 0.2396 0.0734 0.4466 0.044 Uiso 1 1 calc R . . H22D H 0.3071 0.0565 0.4243 0.044 Uiso 1 1 calc R . . C223 C 0.3584(4) 0.0871(4) 0.45987(12) 0.0497(16) Uani 1 1 d . . . H22E H 0.3473 0.1278 0.4740 0.060 Uiso 1 1 calc R . . H22F H 0.4127 0.1005 0.4520 0.060 Uiso 1 1 calc R . . C224 C 0.3616(5) 0.0004(4) 0.47177(12) 0.0586(18) Uani 1 1 d . . . H22G H 0.3060 -0.0160 0.4774 0.088 Uiso 1 1 calc R . . H22H H 0.3987 0.0004 0.4870 0.088 Uiso 1 1 calc R . . H22I H 0.3821 -0.0387 0.4586 0.088 Uiso 1 1 calc R . . C231 C 0.1358(3) 0.1496(3) 0.41420(10) 0.0330(11) Uani 1 1 d . . . H23A H 0.1437 0.0895 0.4168 0.040 Uiso 1 1 calc R . . H23B H 0.0963 0.1572 0.3995 0.040 Uiso 1 1 calc R . . C232 C 0.0986(4) 0.1867(4) 0.43937(12) 0.0474(15) Uani 1 1 d . . . H23C H 0.1426 0.1910 0.4529 0.057 Uiso 1 1 calc R . . H23D H 0.0789 0.2433 0.4355 0.057 Uiso 1 1 calc R . . C233 C 0.0292(5) 0.1379(5) 0.45030(14) 0.071(2) Uani 1 1 d . . . H23E H 0.0477 0.0800 0.4526 0.085 Uiso 1 1 calc R . . H23F H -0.0166 0.1378 0.4374 0.085 Uiso 1 1 calc R . . C234 C -0.0029(5) 0.1689(6) 0.47613(16) 0.102(4) Uani 1 1 d . . . H23G H 0.0418 0.1690 0.4891 0.153 Uiso 1 1 calc R . . H23H H -0.0476 0.1329 0.4822 0.153 Uiso 1 1 calc R . . H23I H -0.0240 0.2253 0.4739 0.153 Uiso 1 1 calc R . . C241 C 0.2080(3) 0.2802(3) 0.40072(10) 0.0305(11) Uani 1 1 d . . . H24A H 0.1869 0.3077 0.4168 0.037 Uiso 1 1 calc R . . H24B H 0.2632 0.3036 0.3969 0.037 Uiso 1 1 calc R . . C242 C 0.1512(3) 0.3009(3) 0.37809(9) 0.0283(10) Uani 1 1 d . . . H24C H 0.0947 0.2807 0.3819 0.034 Uiso 1 1 calc R . . H24D H 0.1708 0.2735 0.3618 0.034 Uiso 1 1 calc R . . C243 C 0.1496(3) 0.3943(3) 0.37411(10) 0.0329(11) Uani 1 1 d . . . H24E H 0.2066 0.4140 0.3709 0.039 Uiso 1 1 calc R . . H24F H 0.1293 0.4210 0.3904 0.039 Uiso 1 1 calc R . . C244 C 0.0947(4) 0.4201(3) 0.35103(11) 0.0364(12) Uani 1 1 d . . . H24G H 0.1163 0.3963 0.3347 0.055 Uiso 1 1 calc R . . H24H H 0.0942 0.4805 0.3496 0.055 Uiso 1 1 calc R . . H24I H 0.0383 0.4002 0.3540 0.055 Uiso 1 1 calc R . . N3 N 0.2998(2) 0.7103(3) 0.49983(7) 0.0262(9) Uani 1 1 d . . . C311 C 0.3034(3) 0.7523(3) 0.47271(9) 0.0293(11) Uani 1 1 d . . . H31A H 0.3485 0.7936 0.4731 0.035 Uiso 1 1 calc R . . H31B H 0.3186 0.7099 0.4595 0.035 Uiso 1 1 calc R . . C312 C 0.2248(3) 0.7958(3) 0.46310(9) 0.0322(11) Uani 1 1 d . . . H31C H 0.2115 0.8426 0.4749 0.039 Uiso 1 1 calc R . . H31D H 0.1778 0.7566 0.4634 0.039 Uiso 1 1 calc R . . C313 C 0.2388(3) 0.8275(4) 0.43488(9) 0.0357(12) Uani 1 1 d . . . H31E H 0.2912 0.8591 0.4342 0.043 Uiso 1 1 calc R . . H31F H 0.2441 0.7798 0.4228 0.043 Uiso 1 1 calc R . . C314 C 0.1686(4) 0.8824(4) 0.42562(12) 0.0516(15) Uani 1 1 d . . . H31G H 0.1169 0.8508 0.4257 0.077 Uiso 1 1 calc R . . H31H H 0.1801 0.9019 0.4077 0.077 Uiso 1 1 calc R . . H31I H 0.1634 0.9298 0.4375 0.077 Uiso 1 1 calc R . . C321 C 0.3880(3) 0.7149(3) 0.51090(10) 0.0294(11) Uani 1 1 d . . . H32A H 0.3929 0.6742 0.5254 0.035 Uiso 1 1 calc R . . H32B H 0.4269 0.6980 0.4969 0.035 Uiso 1 1 calc R . . C322 C 0.4149(3) 0.7994(3) 0.52133(11) 0.0337(12) Uani 1 1 d . . . H32C H 0.3966 0.8432 0.5090 0.040 Uiso 1 1 calc R . . H32D H 0.3889 0.8097 0.5387 0.040 Uiso 1 1 calc R . . C323 C 0.5082(3) 0.8016(3) 0.52402(10) 0.0344(11) Uani 1 1 d . . . H32E H 0.5334 0.8018 0.5062 0.041 Uiso 1 1 calc R . . H32F H 0.5269 0.7511 0.5332 0.041 Uiso 1 1 calc R . . C324 C 0.5381(4) 0.8772(4) 0.53921(12) 0.0472(15) Uani 1 1 d . . . H32G H 0.5132 0.9271 0.5317 0.071 Uiso 1 1 calc R . . H32H H 0.5984 0.8810 0.5380 0.071 Uiso 1 1 calc R . . H32I H 0.5220 0.8721 0.5577 0.071 Uiso 1 1 calc R . . C331 C 0.2389(3) 0.7544(3) 0.51762(9) 0.0273(10) Uani 1 1 d . . . H33A H 0.1839 0.7533 0.5091 0.033 Uiso 1 1 calc R . . H33B H 0.2559 0.8130 0.5191 0.033 Uiso 1 1 calc R . . C332 C 0.2305(3) 0.7189(3) 0.54524(9) 0.0323(11) Uani 1 1 d . . . H33C H 0.2860 0.7105 0.5531 0.039 Uiso 1 1 calc R . . H33D H 0.2022 0.6647 0.5445 0.039 Uiso 1 1 calc R . . C333 C 0.1804(3) 0.7793(3) 0.56228(9) 0.0322(11) Uani 1 1 d . . . H33E H 0.1820 0.7603 0.5808 0.039 Uiso 1 1 calc R . . H33F H 0.2070 0.8344 0.5615 0.039 Uiso 1 1 calc R . . C334 C 0.0901(3) 0.7880(4) 0.55381(12) 0.0459(14) Uani 1 1 d . . . H33G H 0.0877 0.8087 0.5357 0.069 Uiso 1 1 calc R . . H33H H 0.0619 0.8270 0.5656 0.069 Uiso 1 1 calc R . . H33I H 0.0629 0.7340 0.5548 0.069 Uiso 1 1 calc R . . C341 C 0.2800(3) 0.6193(3) 0.49758(10) 0.0281(10) Uani 1 1 d . . . H34A H 0.2815 0.5950 0.5155 0.034 Uiso 1 1 calc R . . H34B H 0.3242 0.5926 0.4872 0.034 Uiso 1 1 calc R . . C342 C 0.1976(3) 0.5976(3) 0.48513(10) 0.0319(11) Uani 1 1 d . . . H34C H 0.1979 0.6130 0.4663 0.038 Uiso 1 1 calc R . . H34D H 0.1526 0.6286 0.4940 0.038 Uiso 1 1 calc R . . C343 C 0.1828(3) 0.5052(4) 0.48796(11) 0.0372(12) Uani 1 1 d . . . H34E H 0.2307 0.4751 0.4805 0.045 Uiso 1 1 calc R . . H34F H 0.1793 0.4913 0.5069 0.045 Uiso 1 1 calc R . . C344 C 0.1047(3) 0.4756(4) 0.47432(13) 0.0483(15) Uani 1 1 d . . . H34G H 0.0571 0.5061 0.4812 0.072 Uiso 1 1 calc R . . H34H H 0.0972 0.4164 0.4776 0.072 Uiso 1 1 calc R . . H34I H 0.1095 0.4851 0.4553 0.072 Uiso 1 1 calc R . . N4 N 0.7547(3) 0.7547(3) 0.5000 0.054(2) Uani 1 2 d S . . C41 C 0.7057(3) 0.7057(3) 0.5000 0.0352(18) Uani 1 2 d S . . C42 C 0.6408(3) 0.6408(3) 0.5000 0.048(2) Uani 1 2 d S . . N5 N 0.2228(4) 0.2228(4) 0.5000 0.087(4) Uani 1 2 d S . . C51 C 0.2719(4) 0.2719(4) 0.5000 0.043(2) Uani 1 2 d S . . C52 C 0.3349(4) 0.3349(4) 0.5000 0.066(3) Uani 1 2 d S . . 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 Ti1 0.0146(3) 0.0166(3) 0.0122(3) 0.0007(3) -0.0009(2) 0.0017(3) Mo2 0.01489(16) 0.02194(19) 0.02029(16) -0.00373(14) -0.00306(13) 0.00176(14) Mo3 0.02275(18) 0.01322(17) 0.02111(15) -0.00092(12) 0.00036(15) 0.00306(14) Mo4 0.01597(16) 0.02200(19) 0.01905(16) 0.00228(15) 0.00374(12) 0.00087(14) Mo5 0.02385(18) 0.01331(17) 0.01676(15) 0.00040(12) -0.00260(14) 0.00261(13) Mo6 0.0310(2) 0.02404(19) 0.01174(14) -0.00133(15) -0.00138(13) 0.00487(16) O1 0.0295(14) 0.0295(14) 0.0149(17) 0.0019(12) -0.0019(12) 0.001(2) O2 0.0186(15) 0.0333(18) 0.0307(18) -0.0060(15) -0.0035(13) 0.0006(14) O3 0.0364(18) 0.0167(15) 0.0410(19) -0.0017(13) 0.0007(18) 0.0038(15) O4 0.0225(16) 0.0351(19) 0.0307(17) 0.0058(15) 0.0074(13) 0.0027(14) O5 0.0393(19) 0.0191(16) 0.0294(18) 0.0011(13) -0.0077(16) 0.0056(14) O6 0.054(2) 0.042(2) 0.0129(13) -0.0004(15) -0.0036(14) 0.0056(18) O7 0.0158(13) 0.0155(13) 0.0132(11) 0.0002(10) -0.0027(10) 0.0022(11) O12 0.0161(14) 0.0260(17) 0.0212(14) -0.0007(12) 0.0021(11) 0.0004(12) O13 0.0226(15) 0.0164(14) 0.0208(13) 0.0043(11) -0.0007(12) 0.0016(12) O14 0.0146(13) 0.0252(16) 0.0173(13) 0.0018(12) -0.0025(10) -0.0001(12) O15 0.0205(15) 0.0164(14) 0.0183(13) -0.0024(11) -0.0004(11) 0.0034(11) O23 0.0222(15) 0.0194(15) 0.0202(15) -0.0023(12) -0.0009(12) -0.0045(12) O25 0.0210(15) 0.0239(16) 0.0232(15) -0.0040(13) -0.0058(13) 0.0069(12) O26 0.0237(16) 0.0279(18) 0.0236(14) -0.0062(13) -0.0078(12) 0.0014(13) O34 0.0191(15) 0.0202(16) 0.0289(17) 0.0047(13) 0.0066(13) 0.0082(12) O36 0.0301(18) 0.0240(16) 0.0232(14) -0.0068(12) 0.0005(13) 0.0038(13) O45 0.0247(16) 0.0188(16) 0.0299(17) 0.0018(13) 0.0020(13) 0.0001(12) O46 0.0340(18) 0.0348(19) 0.0136(13) -0.0017(13) 0.0032(12) -0.0026(15) O56 0.0323(18) 0.0242(16) 0.0156(14) 0.0007(12) -0.0033(13) 0.0048(13) N1 0.0228(19) 0.0172(18) 0.0183(17) 0.0009(14) 0.0055(14) -0.0011(14) C111 0.028(2) 0.022(2) 0.018(2) 0.0047(17) 0.0058(17) -0.0017(18) C112 0.028(3) 0.031(3) 0.030(3) 0.005(2) 0.001(2) -0.002(2) C113 0.028(2) 0.032(3) 0.026(2) 0.004(2) -0.0009(19) 0.001(2) C114 0.035(3) 0.060(4) 0.031(3) 0.007(3) -0.004(2) -0.008(3) C121 0.023(2) 0.023(2) 0.020(2) 0.0046(17) 0.0057(17) 0.0037(17) C122 0.037(3) 0.031(3) 0.032(3) 0.004(2) 0.014(2) 0.003(2) C123 0.036(3) 0.047(3) 0.034(3) 0.002(2) 0.014(2) 0.005(2) C124 0.069(5) 0.062(5) 0.062(5) -0.012(4) 0.033(4) 0.016(4) C131 0.026(2) 0.026(2) 0.015(2) -0.0010(17) 0.0027(17) -0.0017(18) C132 0.027(2) 0.038(3) 0.027(2) 0.005(2) 0.001(2) 0.000(2) C133 0.041(3) 0.060(4) 0.043(3) 0.005(3) -0.013(3) -0.008(3) C134 0.052(4) 0.088(5) 0.032(3) 0.006(3) -0.017(3) -0.006(3) C141 0.026(2) 0.017(2) 0.027(2) 0.0030(17) 0.0040(18) -0.0006(17) C142 0.028(2) 0.023(2) 0.026(2) 0.0003(18) 0.0031(19) 0.0022(18) C143 0.038(3) 0.024(2) 0.036(3) 0.003(2) 0.013(2) 0.001(2) C144 0.045(3) 0.029(3) 0.037(3) -0.003(2) 0.012(2) 0.003(2) N2 0.035(2) 0.026(2) 0.0223(19) -0.0050(16) -0.0105(17) 0.0004(17) C211 0.037(3) 0.025(2) 0.025(2) -0.0039(19) -0.010(2) -0.001(2) C212 0.036(3) 0.043(3) 0.041(3) 0.001(2) -0.005(2) -0.010(2) C213 0.046(3) 0.034(3) 0.040(3) 0.005(2) 0.002(3) -0.008(3) C214 0.049(4) 0.076(5) 0.043(4) 0.005(3) 0.003(3) -0.011(3) C221 0.039(3) 0.033(3) 0.028(3) -0.006(2) -0.016(2) 0.000(2) C222 0.039(3) 0.033(3) 0.038(3) -0.003(2) -0.012(2) -0.001(2) C223 0.058(4) 0.049(4) 0.043(3) -0.006(3) -0.024(3) 0.004(3) C224 0.074(5) 0.064(4) 0.038(3) -0.004(3) -0.022(3) 0.018(4) C231 0.034(3) 0.034(3) 0.031(2) -0.002(2) -0.009(2) 0.000(2) C232 0.045(3) 0.050(4) 0.047(4) -0.007(3) -0.001(3) 0.010(3) C233 0.075(5) 0.080(5) 0.059(4) -0.025(4) 0.009(4) -0.017(4) C234 0.068(6) 0.155(9) 0.082(6) -0.053(6) 0.030(5) -0.048(6) C241 0.038(3) 0.024(2) 0.029(2) 0.0000(19) -0.012(2) 0.000(2) C242 0.032(3) 0.024(2) 0.029(2) -0.0026(19) -0.008(2) 0.0010(19) C243 0.037(3) 0.026(2) 0.036(3) -0.004(2) -0.007(2) -0.005(2) C244 0.043(3) 0.028(3) 0.038(3) 0.005(2) -0.003(2) 0.001(2) N3 0.026(2) 0.032(2) 0.020(2) 0.0008(17) 0.0030(16) 0.0122(16) C311 0.030(3) 0.038(3) 0.020(2) -0.003(2) 0.0044(19) 0.009(2) C312 0.035(3) 0.040(3) 0.022(2) 0.005(2) 0.003(2) 0.005(2) C313 0.042(3) 0.046(3) 0.018(2) 0.000(2) 0.001(2) 0.001(2) C314 0.063(4) 0.046(4) 0.046(3) 0.009(3) -0.006(3) 0.002(3) C321 0.024(2) 0.028(2) 0.035(3) -0.006(2) -0.003(2) 0.0106(19) C322 0.038(3) 0.030(3) 0.033(3) -0.004(2) -0.001(2) 0.009(2) C323 0.042(3) 0.025(2) 0.036(3) 0.008(2) 0.004(2) -0.003(2) C324 0.053(4) 0.038(3) 0.050(4) 0.006(3) -0.006(3) -0.007(3) C331 0.032(3) 0.032(3) 0.018(2) 0.0012(18) 0.0004(18) 0.012(2) C332 0.036(3) 0.039(3) 0.021(2) 0.004(2) 0.002(2) 0.008(2) C333 0.035(3) 0.044(3) 0.018(2) -0.004(2) 0.000(2) 0.004(2) C334 0.032(3) 0.054(4) 0.052(4) -0.010(3) 0.005(3) 0.005(3) C341 0.025(2) 0.028(3) 0.031(2) -0.001(2) 0.001(2) 0.0101(19) C342 0.031(3) 0.039(3) 0.025(2) 0.001(2) 0.002(2) 0.012(2) C343 0.030(3) 0.045(3) 0.037(3) 0.003(3) 0.006(2) -0.002(2) C344 0.031(3) 0.059(4) 0.055(4) 0.001(3) 0.010(3) -0.006(3) N4 0.064(4) 0.064(4) 0.035(4) -0.001(3) 0.001(3) -0.036(4) C41 0.040(3) 0.040(3) 0.025(4) -0.003(2) 0.003(2) -0.007(4) C42 0.040(3) 0.040(3) 0.065(6) -0.012(3) 0.012(3) -0.012(4) N5 0.107(6) 0.107(6) 0.046(5) -0.016(4) 0.016(4) -0.062(7) C51 0.048(3) 0.048(3) 0.034(4) -0.001(3) 0.001(3) -0.011(4) C52 0.040(3) 0.040(3) 0.118(9) 0.027(4) -0.027(4) -0.017(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 Ti1 O1 1.8148(7) . ? Ti1 O7 2.179(3) . ? Ti1 O12 1.939(3) . ? Ti1 O13 1.964(3) . ? Ti1 O14 1.959(3) . ? Ti1 O15 1.962(3) . ? Mo2 O2 1.701(3) . ? Mo2 O7 2.328(3) . ? Mo2 O12 1.861(3) . ? Mo2 O23 2.060(3) . ? Mo2 O25 1.858(3) . ? Mo2 O26 1.941(3) . ? Mo3 O3 1.696(3) . ? Mo3 O7 2.353(3) . ? Mo3 O13 1.852(3) . ? Mo3 O23 1.851(3) . ? Mo3 O34 2.054(3) . ? Mo3 O36 1.975(3) . ? Mo4 O4 1.704(3) . ? Mo4 O7 2.319(3) . ? Mo4 O14 1.852(3) . ? Mo4 O34 1.866(3) . ? Mo4 O45 2.063(3) . ? Mo4 O46 1.943(3) . ? Mo5 O5 1.698(3) . ? Mo5 O7 2.342(3) . ? Mo5 O15 1.857(3) . ? Mo5 O25 2.076(3) . ? Mo5 O45 1.847(3) . ? Mo5 O56 1.956(3) . ? Mo6 O6 1.689(3) . ? Mo6 O7 2.336(3) . ? Mo6 O26 1.922(3) . ? Mo6 O36 1.911(3) . ? Mo6 O46 1.918(3) . ? Mo6 O56 1.928(3) . ? O1 Ti1 1.8148(7) 7_556 ? N1 C111 1.523(5) . ? N1 C121 1.523(5) . ? N1 C131 1.524(5) . ? N1 C141 1.516(5) . ? C111 H11A 0.990 . ? C111 H11B 0.990 . ? C111 C112 1.524(7) . ? C112 H11C 0.990 . ? C112 H11D 0.990 . ? C112 C113 1.522(6) . ? C113 H11E 0.990 . ? C113 H11F 0.990 . ? C113 C114 1.517(7) . ? C114 H11G 0.980 . ? C114 H11H 0.980 . ? C114 H11I 0.980 . ? C121 H12A 0.990 . ? C121 H12B 0.990 . ? C121 C122 1.511(6) . ? C122 H12C 0.990 . ? C122 H12D 0.990 . ? C122 C123 1.513(7) . ? C123 H12E 0.990 . ? C123 H12F 0.990 . ? C123 C124 1.509(8) . ? C124 H12G 0.980 . ? C124 H12H 0.980 . ? C124 H12I 0.980 . ? C131 H13A 0.990 . ? C131 H13B 0.990 . ? C131 C132 1.516(6) . ? C132 H13C 0.990 . ? C132 H13D 0.990 . ? C132 C133 1.506(7) . ? C133 H13E 0.990 . ? C133 H13F 0.990 . ? C133 C134 1.528(8) . ? C134 H13G 0.980 . ? C134 H13H 0.980 . ? C134 H13I 0.980 . ? C141 H14A 0.990 . ? C141 H14B 0.990 . ? C141 C142 1.520(6) . ? C142 H14C 0.990 . ? C142 H14D 0.990 . ? C142 C143 1.530(6) . ? C143 H14E 0.990 . ? C143 H14F 0.990 . ? C143 C144 1.508(7) . ? C144 H14G 0.980 . ? C144 H14H 0.980 . ? C144 H14I 0.980 . ? N2 C211 1.521(6) . ? N2 C221 1.521(6) . ? N2 C231 1.522(6) . ? N2 C241 1.525(6) . ? C211 H21A 0.990 . ? C211 H21B 0.990 . ? C211 C212 1.522(7) . ? C212 H21C 0.990 . ? C212 H21D 0.990 . ? C212 C213 1.499(8) . ? C213 H21E 0.990 . ? C213 H21F 0.990 . ? C213 C214 1.508(8) . ? C214 H21G 0.980 . ? C214 H21H 0.980 . ? C214 H21I 0.980 . ? C221 H22A 0.990 . ? C221 H22B 0.990 . ? C221 C222 1.515(7) . ? C222 H22C 0.990 . ? C222 H22D 0.990 . ? C222 C223 1.502(7) . ? C223 H22E 0.990 . ? C223 H22F 0.990 . ? C223 C224 1.528(9) . ? C224 H22G 0.980 . ? C224 H22H 0.980 . ? C224 H22I 0.980 . ? C231 H23A 0.990 . ? C231 H23B 0.990 . ? C231 C232 1.534(7) . ? C232 H23C 0.990 . ? C232 H23D 0.990 . ? C232 C233 1.481(9) . ? C233 H23E 0.990 . ? C233 H23F 0.990 . ? C233 C234 1.497(9) . ? C234 H23G 0.980 . ? C234 H23H 0.980 . ? C234 H23I 0.980 . ? C241 H24A 0.990 . ? C241 H24B 0.990 . ? C241 C242 1.510(6) . ? C242 H24C 0.990 . ? C242 H24D 0.990 . ? C242 C243 1.524(6) . ? C243 H24E 0.990 . ? C243 H24F 0.990 . ? C243 C244 1.530(7) . ? C244 H24G 0.980 . ? C244 H24H 0.980 . ? C244 H24I 0.980 . ? N3 C311 1.536(6) . ? N3 C321 1.536(6) . ? N3 C331 1.515(6) . ? N3 C341 1.512(6) . ? C311 H31A 0.990 . ? C311 H31B 0.990 . ? C311 C312 1.532(6) . ? C312 H31C 0.990 . ? C312 H31D 0.990 . ? C312 C313 1.538(6) . ? C313 H31E 0.990 . ? C313 H31F 0.990 . ? C313 C314 1.517(8) . ? C314 H31G 0.980 . ? C314 H31H 0.980 . ? C314 H31I 0.980 . ? C321 H32A 0.990 . ? C321 H32B 0.990 . ? C321 C322 1.529(7) . ? C322 H32C 0.990 . ? C322 H32D 0.990 . ? C322 C323 1.517(7) . ? C323 H32E 0.990 . ? C323 H32F 0.990 . ? C323 C324 1.525(8) . ? C324 H32G 0.980 . ? C324 H32H 0.980 . ? C324 H32I 0.980 . ? C331 H33A 0.990 . ? C331 H33B 0.990 . ? C331 C332 1.521(6) . ? C332 H33C 0.990 . ? C332 H33D 0.990 . ? C332 C333 1.538(6) . ? C333 H33E 0.990 . ? C333 H33F 0.990 . ? C333 C334 1.529(7) . ? C334 H33G 0.980 . ? C334 H33H 0.980 . ? C334 H33I 0.980 . ? C341 H34A 0.990 . ? C341 H34B 0.990 . ? C341 C342 1.517(7) . ? C342 H34C 0.990 . ? C342 H34D 0.990 . ? C342 C343 1.522(8) . ? C343 H34E 0.990 . ? C343 H34F 0.990 . ? C343 C344 1.519(8) . ? C344 H34G 0.980 . ? C344 H34H 0.980 . ? C344 H34I 0.980 . ? N4 C41 1.122(9) . ? C41 C42 1.486(10) . ? N5 C51 1.123(11) . ? C51 C52 1.444(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O7 178.98(11) . . ? O1 Ti1 O12 100.99(14) . . ? O1 Ti1 O13 101.95(12) . . ? O1 Ti1 O14 101.71(14) . . ? O1 Ti1 O15 100.05(12) . . ? O7 Ti1 O12 79.01(11) . . ? O7 Ti1 O13 79.07(11) . . ? O7 Ti1 O14 78.29(10) . . ? O7 Ti1 O15 78.93(11) . . ? O12 Ti1 O13 88.57(13) . . ? O12 Ti1 O14 157.30(12) . . ? O12 Ti1 O15 88.01(12) . . ? O13 Ti1 O14 87.10(13) . . ? O13 Ti1 O15 157.98(12) . . ? O14 Ti1 O15 87.70(12) . . ? O2 Mo2 O7 174.77(14) . . ? O2 Mo2 O12 103.62(14) . . ? O2 Mo2 O23 99.30(14) . . ? O2 Mo2 O25 105.13(15) . . ? O2 Mo2 O26 102.15(14) . . ? O7 Mo2 O12 76.75(11) . . ? O7 Mo2 O23 75.51(10) . . ? O7 Mo2 O25 80.02(11) . . ? O7 Mo2 O26 76.66(11) . . ? O12 Mo2 O23 84.46(12) . . ? O12 Mo2 O25 93.19(13) . . ? O12 Mo2 O26 152.29(12) . . ? O23 Mo2 O25 155.31(12) . . ? O23 Mo2 O26 81.49(12) . . ? O25 Mo2 O26 89.78(13) . . ? O3 Mo3 O7 176.79(14) . . ? O3 Mo3 O13 104.65(14) . . ? O3 Mo3 O23 103.90(15) . . ? O3 Mo3 O34 101.64(15) . . ? O3 Mo3 O36 102.61(15) . . ? O7 Mo3 O13 76.83(10) . . ? O7 Mo3 O23 78.74(11) . . ? O7 Mo3 O34 75.57(10) . . ? O7 Mo3 O36 75.51(11) . . ? O13 Mo3 O23 93.84(13) . . ? O13 Mo3 O34 84.83(13) . . ? O13 Mo3 O36 151.23(12) . . ? O23 Mo3 O34 153.89(12) . . ? O23 Mo3 O36 88.43(13) . . ? O34 Mo3 O36 80.80(13) . . ? O4 Mo4 O7 175.51(14) . . ? O4 Mo4 O14 104.35(14) . . ? O4 Mo4 O34 104.23(14) . . ? O4 Mo4 O45 99.90(14) . . ? O4 Mo4 O46 101.76(15) . . ? O7 Mo4 O14 76.84(10) . . ? O7 Mo4 O34 79.93(11) . . ? O7 Mo4 O45 75.82(11) . . ? O7 Mo4 O46 76.38(11) . . ? O14 Mo4 O34 93.62(13) . . ? O14 Mo4 O45 84.84(13) . . ? O14 Mo4 O46 152.01(13) . . ? O34 Mo4 O45 155.42(12) . . ? O34 Mo4 O46 89.57(14) . . ? O45 Mo4 O46 80.91(13) . . ? O5 Mo5 O7 175.81(13) . . ? O5 Mo5 O15 103.37(14) . . ? O5 Mo5 O25 100.25(14) . . ? O5 Mo5 O45 104.80(15) . . ? O5 Mo5 O56 103.32(14) . . ? O7 Mo5 O15 76.87(11) . . ? O7 Mo5 O25 75.59(10) . . ? O7 Mo5 O45 79.32(11) . . ? O7 Mo5 O56 75.75(11) . . ? O15 Mo5 O25 84.32(13) . . ? O15 Mo5 O45 94.01(13) . . ? O15 Mo5 O56 151.33(13) . . ? O25 Mo5 O45 154.57(12) . . ? O25 Mo5 O56 80.80(13) . . ? O45 Mo5 O56 89.18(14) . . ? O6 Mo6 O7 178.85(14) . . ? O6 Mo6 O26 103.21(16) . . ? O6 Mo6 O36 104.07(15) . . ? O6 Mo6 O46 103.53(16) . . ? O6 Mo6 O56 102.45(15) . . ? O7 Mo6 O26 76.83(10) . . ? O7 Mo6 O36 77.08(11) . . ? O7 Mo6 O46 76.41(10) . . ? O7 Mo6 O56 76.40(11) . . ? O26 Mo6 O36 87.32(14) . . ? O26 Mo6 O46 153.23(12) . . ? O26 Mo6 O56 86.52(13) . . ? O36 Mo6 O46 87.41(14) . . ? O36 Mo6 O56 153.47(12) . . ? O46 Mo6 O56 86.58(14) . . ? Ti1 O1 Ti1 173.2(3) . 7_556 ? Ti1 O7 Mo2 89.93(9) . . ? Ti1 O7 Mo3 89.72(10) . . ? Ti1 O7 Mo4 90.52(9) . . ? Ti1 O7 Mo5 90.04(9) . . ? Ti1 O7 Mo6 179.46(14) . . ? Mo2 O7 Mo3 90.05(9) . . ? Mo2 O7 Mo4 179.54(13) . . ? Mo2 O7 Mo5 90.11(9) . . ? Mo2 O7 Mo6 89.62(9) . . ? Mo3 O7 Mo4 89.84(9) . . ? Mo3 O7 Mo5 179.71(14) . . ? Mo3 O7 Mo6 89.98(9) . . ? Mo4 O7 Mo5 90.00(9) . . ? Mo4 O7 Mo6 89.93(9) . . ? Mo5 O7 Mo6 90.25(9) . . ? Ti1 O12 Mo2 113.98(14) . . ? Ti1 O13 Mo3 113.92(13) . . ? Ti1 O14 Mo4 114.01(13) . . ? Ti1 O15 Mo5 113.82(14) . . ? Mo2 O23 Mo3 115.61(14) . . ? Mo2 O25 Mo5 114.22(14) . . ? Mo2 O26 Mo6 116.59(14) . . ? Mo3 O34 Mo4 114.55(13) . . ? Mo3 O36 Mo6 117.10(14) . . ? Mo4 O45 Mo5 114.77(15) . . ? Mo4 O46 Mo6 116.83(15) . . ? Mo5 O56 Mo6 117.20(15) . . ? C111 N1 C121 110.5(3) . . ? C111 N1 C131 106.5(3) . . ? C111 N1 C141 111.6(3) . . ? C121 N1 C131 111.0(3) . . ? C121 N1 C141 106.2(3) . . ? C131 N1 C141 111.1(3) . . ? N1 C111 H11A 108.4 . . ? N1 C111 H11B 108.4 . . ? N1 C111 C112 115.7(4) . . ? H11A C111 H11B 107.4 . . ? H11A C111 C112 108.4 . . ? H11B C111 C112 108.4 . . ? C111 C112 H11C 109.6 . . ? C111 C112 H11D 109.6 . . ? C111 C112 C113 110.1(4) . . ? H11C C112 H11D 108.2 . . ? H11C C112 C113 109.6 . . ? H11D C112 C113 109.6 . . ? C112 C113 H11E 108.9 . . ? C112 C113 H11F 108.9 . . ? C112 C113 C114 113.3(4) . . ? H11E C113 H11F 107.7 . . ? H11E C113 C114 108.9 . . ? H11F C113 C114 108.9 . . ? C113 C114 H11G 109.5 . . ? C113 C114 H11H 109.5 . . ? C113 C114 H11I 109.5 . . ? H11G C114 H11H 109.5 . . ? H11G C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? N1 C121 H12A 108.6 . . ? N1 C121 H12B 108.6 . . ? N1 C121 C122 114.5(4) . . ? H12A C121 H12B 107.6 . . ? H12A C121 C122 108.6 . . ? H12B C121 C122 108.6 . . ? C121 C122 H12C 109.4 . . ? C121 C122 H12D 109.4 . . ? C121 C122 C123 111.3(4) . . ? H12C C122 H12D 108.0 . . ? H12C C122 C123 109.4 . . ? H12D C122 C123 109.4 . . ? C122 C123 H12E 109.1 . . ? C122 C123 H12F 109.1 . . ? C122 C123 C124 112.4(5) . . ? H12E C123 H12F 107.9 . . ? H12E C123 C124 109.1 . . ? H12F C123 C124 109.1 . . ? C123 C124 H12G 109.5 . . ? C123 C124 H12H 109.5 . . ? C123 C124 H12I 109.5 . . ? H12G C124 H12H 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? N1 C131 H13A 108.5 . . ? N1 C131 H13B 108.5 . . ? N1 C131 C132 115.3(4) . . ? H13A C131 H13B 107.5 . . ? H13A C131 C132 108.5 . . ? H13B C131 C132 108.5 . . ? C131 C132 H13C 109.5 . . ? C131 C132 H13D 109.5 . . ? C131 C132 C133 110.7(4) . . ? H13C C132 H13D 108.1 . . ? H13C C132 C133 109.5 . . ? H13D C132 C133 109.5 . . ? C132 C133 H13E 109.3 . . ? C132 C133 H13F 109.3 . . ? C132 C133 C134 111.5(5) . . ? H13E C133 H13F 108.0 . . ? H13E C133 C134 109.3 . . ? H13F C133 C134 109.3 . . ? C133 C134 H13G 109.5 . . ? C133 C134 H13H 109.5 . . ? C133 C134 H13I 109.5 . . ? H13G C134 H13H 109.5 . . ? H13G C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? N1 C141 H14A 108.3 . . ? N1 C141 H14B 108.3 . . ? N1 C141 C142 115.8(4) . . ? H14A C141 H14B 107.4 . . ? H14A C141 C142 108.3 . . ? H14B C141 C142 108.3 . . ? C141 C142 H14C 109.8 . . ? C141 C142 H14D 109.8 . . ? C141 C142 C143 109.5(4) . . ? H14C C142 H14D 108.2 . . ? H14C C142 C143 109.8 . . ? H14D C142 C143 109.8 . . ? C142 C143 H14E 108.7 . . ? C142 C143 H14F 108.7 . . ? C142 C143 C144 114.1(4) . . ? H14E C143 H14F 107.6 . . ? H14E C143 C144 108.7 . . ? H14F C143 C144 108.7 . . ? C143 C144 H14G 109.5 . . ? C143 C144 H14H 109.5 . . ? C143 C144 H14I 109.5 . . ? H14G C144 H14H 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C211 N2 C221 109.4(4) . . ? C211 N2 C231 107.2(4) . . ? C211 N2 C241 110.9(4) . . ? C221 N2 C231 111.1(4) . . ? C221 N2 C241 107.5(3) . . ? C231 N2 C241 110.9(4) . . ? N2 C211 H21A 108.5 . . ? N2 C211 H21B 108.5 . . ? N2 C211 C212 115.2(4) . . ? H21A C211 H21B 107.5 . . ? H21A C211 C212 108.5 . . ? H21B C211 C212 108.5 . . ? C211 C212 H21C 109.3 . . ? C211 C212 H21D 109.3 . . ? C211 C212 C213 111.7(4) . . ? H21C C212 H21D 107.9 . . ? H21C C212 C213 109.3 . . ? H21D C212 C213 109.3 . . ? C212 C213 H21E 109.1 . . ? C212 C213 H21F 109.1 . . ? C212 C213 C214 112.7(5) . . ? H21E C213 H21F 107.8 . . ? H21E C213 C214 109.1 . . ? H21F C213 C214 109.1 . . ? C213 C214 H21G 109.5 . . ? C213 C214 H21H 109.5 . . ? C213 C214 H21I 109.5 . . ? H21G C214 H21H 109.5 . . ? H21G C214 H21I 109.5 . . ? H21H C214 H21I 109.5 . . ? N2 C221 H22A 108.6 . . ? N2 C221 H22B 108.6 . . ? N2 C221 C222 114.8(4) . . ? H22A C221 H22B 107.6 . . ? H22A C221 C222 108.6 . . ? H22B C221 C222 108.6 . . ? C221 C222 H22C 109.0 . . ? C221 C222 H22D 109.0 . . ? C221 C222 C223 113.1(4) . . ? H22C C222 H22D 107.8 . . ? H22C C222 C223 109.0 . . ? H22D C222 C223 109.0 . . ? C222 C223 H22E 109.4 . . ? C222 C223 H22F 109.4 . . ? C222 C223 C224 111.2(5) . . ? H22E C223 H22F 108.0 . . ? H22E C223 C224 109.4 . . ? H22F C223 C224 109.4 . . ? C223 C224 H22G 109.5 . . ? C223 C224 H22H 109.5 . . ? C223 C224 H22I 109.5 . . ? H22G C224 H22H 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? N2 C231 H23A 109.0 . . ? N2 C231 H23B 109.0 . . ? N2 C231 C232 113.1(4) . . ? H23A C231 H23B 107.8 . . ? H23A C231 C232 109.0 . . ? H23B C231 C232 109.0 . . ? C231 C232 H23C 108.8 . . ? C231 C232 H23D 108.8 . . ? C231 C232 C233 113.6(5) . . ? H23C C232 H23D 107.7 . . ? H23C C232 C233 108.8 . . ? H23D C232 C233 108.8 . . ? C232 C233 H23E 108.7 . . ? C232 C233 H23F 108.7 . . ? C232 C233 C234 114.4(6) . . ? H23E C233 H23F 107.6 . . ? H23E C233 C234 108.7 . . ? H23F C233 C234 108.7 . . ? C233 C234 H23G 109.5 . . ? C233 C234 H23H 109.5 . . ? C233 C234 H23I 109.5 . . ? H23G C234 H23H 109.5 . . ? H23G C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? N2 C241 H24A 108.4 . . ? N2 C241 H24B 108.4 . . ? N2 C241 C242 115.6(4) . . ? H24A C241 H24B 107.4 . . ? H24A C241 C242 108.4 . . ? H24B C241 C242 108.4 . . ? C241 C242 H24C 109.8 . . ? C241 C242 H24D 109.8 . . ? C241 C242 C243 109.3(4) . . ? H24C C242 H24D 108.3 . . ? H24C C242 C243 109.8 . . ? H24D C242 C243 109.8 . . ? C242 C243 H24E 109.1 . . ? C242 C243 H24F 109.1 . . ? C242 C243 C244 112.5(4) . . ? H24E C243 H24F 107.8 . . ? H24E C243 C244 109.1 . . ? H24F C243 C244 109.1 . . ? C243 C244 H24G 109.5 . . ? C243 C244 H24H 109.5 . . ? C243 C244 H24I 109.5 . . ? H24G C244 H24H 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? C311 N3 C321 105.7(4) . . ? C311 N3 C331 110.5(3) . . ? C311 N3 C341 111.8(4) . . ? C321 N3 C331 111.3(4) . . ? C321 N3 C341 105.8(3) . . ? C331 N3 C341 111.5(4) . . ? N3 C311 H31A 108.0 . . ? N3 C311 H31B 108.0 . . ? N3 C311 C312 117.2(4) . . ? H31A C311 H31B 107.2 . . ? H31A C311 C312 108.0 . . ? H31B C311 C312 108.0 . . ? C311 C312 H31C 109.9 . . ? C311 C312 H31D 109.9 . . ? C311 C312 C313 109.1(4) . . ? H31C C312 H31D 108.3 . . ? H31C C312 C313 109.9 . . ? H31D C312 C313 109.9 . . ? C312 C313 H31E 109.2 . . ? C312 C313 H31F 109.2 . . ? C312 C313 C314 112.0(5) . . ? H31E C313 H31F 107.9 . . ? H31E C313 C314 109.2 . . ? H31F C313 C314 109.2 . . ? C313 C314 H31G 109.5 . . ? C313 C314 H31H 109.5 . . ? C313 C314 H31I 109.5 . . ? H31G C314 H31H 109.5 . . ? H31G C314 H31I 109.5 . . ? H31H C314 H31I 109.5 . . ? N3 C321 H32A 108.3 . . ? N3 C321 H32B 108.3 . . ? N3 C321 C322 115.7(4) . . ? H32A C321 H32B 107.4 . . ? H32A C321 C322 108.3 . . ? H32B C321 C322 108.3 . . ? C321 C322 H32C 109.7 . . ? C321 C322 H32D 109.7 . . ? C321 C322 C323 109.6(4) . . ? H32C C322 H32D 108.2 . . ? H32C C322 C323 109.7 . . ? H32D C322 C323 109.7 . . ? C322 C323 H32E 109.1 . . ? C322 C323 H32F 109.1 . . ? C322 C323 C324 112.4(5) . . ? H32E C323 H32F 107.9 . . ? H32E C323 C324 109.1 . . ? H32F C323 C324 109.1 . . ? C323 C324 H32G 109.5 . . ? C323 C324 H32H 109.5 . . ? C323 C324 H32I 109.5 . . ? H32G C324 H32H 109.5 . . ? H32G C324 H32I 109.5 . . ? H32H C324 H32I 109.5 . . ? N3 C331 H33A 108.4 . . ? N3 C331 H33B 108.4 . . ? N3 C331 C332 115.4(4) . . ? H33A C331 H33B 107.5 . . ? H33A C331 C332 108.4 . . ? H33B C331 C332 108.4 . . ? C331 C332 H33C 109.9 . . ? C331 C332 H33D 109.9 . . ? C331 C332 C333 108.9(4) . . ? H33C C332 H33D 108.3 . . ? H33C C332 C333 109.9 . . ? H33D C332 C333 109.9 . . ? C332 C333 H33E 108.8 . . ? C332 C333 H33F 108.8 . . ? C332 C333 C334 113.9(4) . . ? H33E C333 H33F 107.7 . . ? H33E C333 C334 108.8 . . ? H33F C333 C334 108.8 . . ? C333 C334 H33G 109.5 . . ? C333 C334 H33H 109.5 . . ? C333 C334 H33I 109.5 . . ? H33G C334 H33H 109.5 . . ? H33G C334 H33I 109.5 . . ? H33H C334 H33I 109.5 . . ? N3 C341 H34A 108.2 . . ? N3 C341 H34B 108.2 . . ? N3 C341 C342 116.3(4) . . ? H34A C341 H34B 107.4 . . ? H34A C341 C342 108.2 . . ? H34B C341 C342 108.2 . . ? C341 C342 H34C 109.9 . . ? C341 C342 H34D 109.9 . . ? C341 C342 C343 109.1(4) . . ? H34C C342 H34D 108.3 . . ? H34C C342 C343 109.9 . . ? H34D C342 C343 109.9 . . ? C342 C343 H34E 108.9 . . ? C342 C343 H34F 108.9 . . ? C342 C343 C344 113.4(5) . . ? H34E C343 H34F 107.7 . . ? H34E C343 C344 108.9 . . ? H34F C343 C344 108.9 . . ? C343 C344 H34G 109.5 . . ? C343 C344 H34H 109.5 . . ? C343 C344 H34I 109.5 . . ? H34G C344 H34H 109.5 . . ? H34G C344 H34I 109.5 . . ? H34H C344 H34I 109.5 . . ? N4 C41 C42 180.0(7) . . ? N5 C51 C52 180.0(8) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.892 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.117 # Contents of RES file _computing_special_details ; TITL rje260 in P4(1)2(1)2 CELL 0.71073 16.1864 16.1864 50.7519 90.000 90.000 90.000 ZERR 4.00 0.0017 0.0017 0.0074 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-Y, 0.5+X, 0.25+Z SYMM 0.5+Y, 0.5-X, 0.75+Z SYMM 0.5-X, 0.5+Y, 0.25-Z SYMM 0.5+X, 0.5-Y, 0.75-Z SYMM Y, X, -Z SYMM -Y, -X, 0.5-Z SFAC C H N O TI MO UNIT 400 888 32 148 8 40 SIZE 0.60 0.48 0.35 TEMP -113 L.S. 8 ACTA 52 BOND $H FMAP 2 PLAN 10 CONN $TI $MO 6 WGHT 0.032300 26.365095 EXTI 0.000182 FVAR 0.07558 TI1 5 0.490172 0.495603 0.464325 11.00000 0.01464 0.01659 = 0.01224 0.00067 -0.00085 0.00173 MO2 6 0.337771 0.486587 0.424671 11.00000 0.01489 0.02194 = 0.02029 -0.00373 -0.00306 0.00176 MO3 6 0.490257 0.350510 0.421506 11.00000 0.02275 0.01322 = 0.02111 -0.00092 0.00036 0.00306 MO4 6 0.623548 0.504321 0.417960 11.00000 0.01597 0.02200 = 0.01905 0.00228 0.00374 0.00087 MO5 6 0.472195 0.640006 0.421643 11.00000 0.02385 0.01331 = 0.01676 0.00040 -0.00260 0.00261 MO6 6 0.470042 0.494800 0.375597 11.00000 0.03101 0.02404 = 0.01174 -0.00133 -0.00138 0.00487 O1 4 0.497582 0.497582 0.500000 10.50000 0.02948 0.02948 = 0.01486 0.00186 -0.00186 0.00107 O2 4 0.234048 0.470565 0.426517 11.00000 0.01859 0.03331 = 0.03069 -0.00600 -0.00349 0.00056 O3 4 0.501649 0.246394 0.420411 11.00000 0.03643 0.01667 = 0.04100 -0.00169 0.00072 0.00377 O4 4 0.727291 0.518433 0.414492 11.00000 0.02249 0.03508 = 0.03068 0.00581 0.00739 0.00275 O5 4 0.458216 0.743952 0.421594 11.00000 0.03933 0.01914 = 0.02937 0.00111 -0.00768 0.00563 O6 4 0.461952 0.496305 0.342419 11.00000 0.05387 0.04200 = 0.01287 -0.00043 -0.00365 0.00558 O7 4 0.480974 0.495609 0.421486 11.00000 0.01584 0.01549 = 0.01317 0.00022 -0.00270 0.00222 O12 4 0.372268 0.480486 0.459600 11.00000 0.01607 0.02596 = 0.02122 -0.00074 0.00210 0.00040 O13 4 0.505250 0.377643 0.456638 11.00000 0.02262 0.01637 = 0.02077 0.00433 -0.00073 0.00162 O14 4 0.605728 0.510735 0.453948 11.00000 0.01455 0.02524 = 0.01728 0.00178 -0.00249 -0.00007 O15 4 0.473562 0.613594 0.457249 11.00000 0.02054 0.01638 = 0.01827 -0.00237 -0.00042 0.00344 O23 4 0.376945 0.365645 0.422700 11.00000 0.02225 0.01940 = 0.02022 -0.00234 -0.00086 -0.00449 O25 4 0.350276 0.600603 0.423304 11.00000 0.02098 0.02392 = 0.02320 -0.00398 -0.00575 0.00690 O26 4 0.357723 0.480413 0.387001 11.00000 0.02367 0.02791 = 0.02360 -0.00623 -0.00777 0.00140 O34 4 0.610049 0.389855 0.417003 11.00000 0.01914 0.02023 = 0.02887 0.00471 0.00662 0.00817 O36 4 0.487031 0.380849 0.383834 11.00000 0.03010 0.02405 = 0.02318 -0.00682 0.00053 0.00380 O45 4 0.584655 0.625694 0.417509 11.00000 0.02469 0.01883 = 0.02989 0.00185 0.00200 0.00014 O46 4 0.585914 0.510847 0.381667 11.00000 0.03396 0.03482 = 0.01356 -0.00173 0.00317 -0.00259 O56 4 0.456735 0.609675 0.384673 11.00000 0.03231 0.02418 = 0.01565 0.00071 -0.00330 0.00476 N1 3 0.765894 0.795749 0.407621 11.00000 0.02281 0.01721 = 0.01826 0.00086 0.00554 -0.00112 C111 1 0.738930 0.844329 0.383402 11.00000 0.02765 0.02246 = 0.01850 0.00471 0.00578 -0.00170 AFIX 23 H11A 2 0.783582 0.841262 0.370107 11.00000 -1.20000 H11B 2 0.732717 0.903058 0.388476 11.00000 -1.20000 AFIX 0 C112 1 0.658718 0.815878 0.370545 11.00000 0.02835 0.03101 = 0.03014 0.00517 0.00122 -0.00158 AFIX 23 H11C 2 0.663315 0.756908 0.365581 11.00000 -1.20000 H11D 2 0.612584 0.821557 0.383223 11.00000 -1.20000 AFIX 0 C113 1 0.641003 0.867484 0.346128 11.00000 0.02780 0.03155 = 0.02648 0.00358 -0.00087 0.00103 AFIX 23 H11E 2 0.636682 0.926277 0.351325 11.00000 -1.20000 H11F 2 0.688064 0.862297 0.333779 11.00000 -1.20000 AFIX 0 C114 1 0.562324 0.842400 0.331996 11.00000 0.03500 0.06004 = 0.03115 0.00737 -0.00401 -0.00759 AFIX 137 H11G 2 0.565564 0.783918 0.327107 11.00000 -1.50000 H11H 2 0.555681 0.876011 0.316076 11.00000 -1.50000 H11I 2 0.514897 0.851065 0.343676 11.00000 -1.50000 AFIX 0 C121 1 0.697417 0.794879 0.428206 11.00000 0.02330 0.02295 = 0.01972 0.00465 0.00567 0.00374 AFIX 23 H12A 2 0.646697 0.772261 0.420033 11.00000 -1.20000 H12B 2 0.713692 0.757079 0.442636 11.00000 -1.20000 AFIX 0 C122 1 0.677619 0.878432 0.439884 11.00000 0.03707 0.03063 = 0.03196 0.00421 0.01445 0.00334 AFIX 23 H12C 2 0.668334 0.918668 0.425494 11.00000 -1.20000 H12D 2 0.725216 0.897852 0.450453 11.00000 -1.20000 AFIX 0 C123 1 0.601606 0.874578 0.457177 11.00000 0.03556 0.04653 = 0.03360 0.00176 0.01445 0.00474 AFIX 23 H12E 2 0.553047 0.860789 0.446163 11.00000 -1.20000 H12F 2 0.608623 0.829901 0.470310 11.00000 -1.20000 AFIX 0 C124 1 0.585581 0.954877 0.471377 11.00000 0.06946 0.06207 = 0.06158 -0.01233 0.03326 0.01576 AFIX 137 H12G 2 0.635318 0.971430 0.481039 11.00000 -1.50000 H12H 2 0.539751 0.947594 0.483779 11.00000 -1.50000 H12I 2 0.571264 0.997768 0.458536 11.00000 -1.50000 AFIX 0 C131 1 0.842989 0.838554 0.418170 11.00000 0.02628 0.02555 = 0.01504 -0.00104 0.00270 -0.00174 AFIX 23 H13A 2 0.885465 0.838658 0.404135 11.00000 -1.20000 H13B 2 0.829040 0.896838 0.422067 11.00000 -1.20000 AFIX 0 C132 1 0.880109 0.800207 0.442707 11.00000 0.02667 0.03757 = 0.02686 0.00510 0.00102 -0.00028 AFIX 23 H13C 2 0.835604 0.787420 0.455451 11.00000 -1.20000 H13D 2 0.908023 0.747815 0.438011 11.00000 -1.20000 AFIX 0 C133 1 0.941426 0.858105 0.455232 11.00000 0.04065 0.06024 = 0.04259 0.00504 -0.01274 -0.00799 AFIX 23 H13E 2 0.913049 0.909899 0.460305 11.00000 -1.20000 H13F 2 0.984927 0.872133 0.442270 11.00000 -1.20000 AFIX 0 C134 1 0.981299 0.819581 0.479602 11.00000 0.05188 0.08842 = 0.03195 0.00586 -0.01732 -0.00578 AFIX 137 H13G 2 0.938137 0.802864 0.492050 11.00000 -1.50000 H13H 2 1.017741 0.860116 0.488008 11.00000 -1.50000 H13I 2 1.013590 0.771056 0.474378 11.00000 -1.50000 AFIX 0 C141 1 0.783352 0.706152 0.400962 11.00000 0.02647 0.01704 = 0.02702 0.00300 0.00402 -0.00064 AFIX 23 H14A 2 0.731196 0.680239 0.395002 11.00000 -1.20000 H14B 2 0.800723 0.677508 0.417282 11.00000 -1.20000 AFIX 0 C142 1 0.848807 0.691503 0.380002 11.00000 0.02777 0.02332 = 0.02582 0.00035 0.00307 0.00222 AFIX 23 H14C 2 0.901567 0.717182 0.385506 11.00000 -1.20000 H14D 2 0.831349 0.717203 0.363200 11.00000 -1.20000 AFIX 0 C143 1 0.860971 0.598594 0.376099 11.00000 0.03843 0.02360 = 0.03629 0.00307 0.01347 0.00069 AFIX 23 H14E 2 0.876027 0.573507 0.393229 11.00000 -1.20000 H14F 2 0.807850 0.573989 0.370451 11.00000 -1.20000 AFIX 0 C144 1 0.926418 0.576764 0.356126 11.00000 0.04469 0.02873 = 0.03675 -0.00348 0.01156 0.00325 AFIX 137 H14G 2 0.913326 0.603139 0.339253 11.00000 -1.50000 H14H 2 0.928142 0.516684 0.353803 11.00000 -1.50000 H14I 2 0.980313 0.596286 0.362342 11.00000 -1.50000 AFIX 0 N2 3 0.218175 0.188296 0.406618 11.00000 0.03461 0.02634 = 0.02226 -0.00503 -0.01047 0.00038 C211 1 0.249740 0.142249 0.382511 11.00000 0.03727 0.02488 = 0.02537 -0.00394 -0.00997 -0.00097 AFIX 23 H21A 2 0.209708 0.150061 0.367975 11.00000 -1.20000 H21B 2 0.251397 0.082504 0.386652 11.00000 -1.20000 AFIX 0 C212 1 0.334795 0.168548 0.372875 11.00000 0.03621 0.04310 = 0.04056 0.00089 -0.00498 -0.01035 AFIX 23 H21C 2 0.336345 0.229445 0.371129 11.00000 -1.20000 H21D 2 0.376835 0.152269 0.386058 11.00000 -1.20000 AFIX 0 C213 1 0.355586 0.129959 0.346849 11.00000 0.04622 0.03419 = 0.04004 0.00516 0.00248 -0.00770 AFIX 23 H21E 2 0.314507 0.147895 0.333577 11.00000 -1.20000 H21F 2 0.351714 0.069133 0.348479 11.00000 -1.20000 AFIX 0 C214 1 0.440909 0.152610 0.337357 11.00000 0.04896 0.07627 = 0.04267 0.00461 0.00300 -0.01113 AFIX 137 H21G 2 0.448552 0.212514 0.338737 11.00000 -1.50000 H21H 2 0.447328 0.135566 0.318941 11.00000 -1.50000 H21I 2 0.482299 0.124470 0.348222 11.00000 -1.50000 AFIX 0 C221 1 0.280650 0.180298 0.428861 11.00000 0.03932 0.03332 = 0.02790 -0.00595 -0.01591 -0.00020 AFIX 23 H22A 2 0.334628 0.201257 0.422579 11.00000 -1.20000 H22B 2 0.262798 0.216000 0.443641 11.00000 -1.20000 AFIX 0 C222 1 0.292447 0.093229 0.439153 11.00000 0.03918 0.03331 = 0.03835 -0.00339 -0.01216 -0.00092 AFIX 23 H22C 2 0.239559 0.073404 0.446637 11.00000 -1.20000 H22D 2 0.307051 0.056541 0.424257 11.00000 -1.20000 AFIX 0 C223 1 0.358448 0.087056 0.459872 11.00000 0.05789 0.04864 = 0.04267 -0.00559 -0.02406 0.00438 AFIX 23 H22E 2 0.347301 0.127815 0.473975 11.00000 -1.20000 H22F 2 0.412710 0.100461 0.451951 11.00000 -1.20000 AFIX 0 C224 1 0.361593 0.000414 0.471768 11.00000 0.07440 0.06378 = 0.03770 -0.00427 -0.02159 0.01804 AFIX 137 H22G 2 0.306024 -0.016049 0.477353 11.00000 -1.50000 H22H 2 0.398673 0.000380 0.487033 11.00000 -1.50000 H22I 2 0.382101 -0.038669 0.458550 11.00000 -1.50000 AFIX 0 C231 1 0.135821 0.149586 0.414201 11.00000 0.03404 0.03398 = 0.03101 -0.00156 -0.00854 -0.00019 AFIX 23 H23A 2 0.143727 0.089483 0.416790 11.00000 -1.20000 H23B 2 0.096283 0.157151 0.399515 11.00000 -1.20000 AFIX 0 C232 1 0.098649 0.186691 0.439369 11.00000 0.04489 0.05014 = 0.04731 -0.00691 -0.00097 0.00988 AFIX 23 H23C 2 0.142551 0.191047 0.452879 11.00000 -1.20000 H23D 2 0.078887 0.243276 0.435483 11.00000 -1.20000 AFIX 0 C233 1 0.029246 0.137887 0.450300 11.00000 0.07478 0.07977 = 0.05862 -0.02495 0.00870 -0.01675 AFIX 23 H23E 2 0.047668 0.080005 0.452579 11.00000 -1.20000 H23F 2 -0.016555 0.137848 0.437372 11.00000 -1.20000 AFIX 0 C234 1 -0.002915 0.168940 0.476129 11.00000 0.06830 0.15546 = 0.08225 -0.05307 0.03009 -0.04779 AFIX 137 H23G 2 0.041826 0.169015 0.489138 11.00000 -1.50000 H23H 2 -0.047611 0.132861 0.482232 11.00000 -1.50000 H23I 2 -0.024008 0.225268 0.473921 11.00000 -1.50000 AFIX 0 C241 1 0.208032 0.280151 0.400723 11.00000 0.03841 0.02436 = 0.02881 0.00001 -0.01196 -0.00020 AFIX 23 H24A 2 0.186930 0.307741 0.416778 11.00000 -1.20000 H24B 2 0.263222 0.303618 0.396893 11.00000 -1.20000 AFIX 0 C242 1 0.151151 0.300927 0.378087 11.00000 0.03193 0.02442 = 0.02869 -0.00260 -0.00754 0.00104 AFIX 23 H24C 2 0.094702 0.280713 0.381938 11.00000 -1.20000 H24D 2 0.170807 0.273519 0.361814 11.00000 -1.20000 AFIX 0 C243 1 0.149643 0.394261 0.374113 11.00000 0.03684 0.02634 = 0.03556 -0.00381 -0.00679 -0.00532 AFIX 23 H24E 2 0.206636 0.414036 0.370898 11.00000 -1.20000 H24F 2 0.129310 0.420959 0.390421 11.00000 -1.20000 AFIX 0 C244 1 0.094670 0.420144 0.351032 11.00000 0.04255 0.02832 = 0.03838 0.00524 -0.00301 0.00068 AFIX 137 H24G 2 0.116283 0.396316 0.334674 11.00000 -1.50000 H24H 2 0.094223 0.480525 0.349624 11.00000 -1.50000 H24I 2 0.038282 0.400173 0.354011 11.00000 -1.50000 AFIX 0 N3 3 0.299759 0.710338 0.499828 11.00000 0.02623 0.03229 = 0.01997 0.00080 0.00297 0.01224 C311 1 0.303353 0.752323 0.472707 11.00000 0.02998 0.03808 = 0.01971 -0.00288 0.00438 0.00918 AFIX 23 H31A 2 0.348509 0.793558 0.473080 11.00000 -1.20000 H31B 2 0.318566 0.709935 0.459509 11.00000 -1.20000 AFIX 0 C312 1 0.224848 0.795756 0.463103 11.00000 0.03531 0.03964 = 0.02161 0.00461 0.00304 0.00534 AFIX 23 H31C 2 0.211520 0.842590 0.474907 11.00000 -1.20000 H31D 2 0.177835 0.756642 0.463378 11.00000 -1.20000 AFIX 0 C313 1 0.238803 0.827505 0.434880 11.00000 0.04246 0.04636 = 0.01828 0.00001 0.00097 0.00086 AFIX 23 H31E 2 0.291162 0.859051 0.434226 11.00000 -1.20000 H31F 2 0.244087 0.779800 0.422790 11.00000 -1.20000 AFIX 0 C314 1 0.168578 0.882355 0.425621 11.00000 0.06325 0.04584 = 0.04573 0.00948 -0.00620 0.00223 AFIX 137 H31G 2 0.116913 0.850790 0.425681 11.00000 -1.50000 H31H 2 0.180100 0.901871 0.407715 11.00000 -1.50000 H31I 2 0.163354 0.929839 0.437485 11.00000 -1.50000 AFIX 0 C321 1 0.387963 0.714910 0.510903 11.00000 0.02450 0.02808 = 0.03548 -0.00634 -0.00267 0.01059 AFIX 23 H32A 2 0.392909 0.674236 0.525385 11.00000 -1.20000 H32B 2 0.426892 0.698018 0.496855 11.00000 -1.20000 AFIX 0 C322 1 0.414867 0.799389 0.521325 11.00000 0.03794 0.02979 = 0.03326 -0.00365 -0.00054 0.00887 AFIX 23 H32C 2 0.396551 0.843229 0.509041 11.00000 -1.20000 H32D 2 0.388938 0.809701 0.538683 11.00000 -1.20000 AFIX 0 C323 1 0.508202 0.801634 0.524021 11.00000 0.04200 0.02543 = 0.03577 0.00805 0.00380 -0.00302 AFIX 23 H32E 2 0.533371 0.801820 0.506243 11.00000 -1.20000 H32F 2 0.526928 0.751065 0.533226 11.00000 -1.20000 AFIX 0 C324 1 0.538118 0.877215 0.539209 11.00000 0.05290 0.03841 = 0.05021 0.00610 -0.00569 -0.00680 AFIX 137 H32G 2 0.513189 0.927095 0.531687 11.00000 -1.50000 H32H 2 0.598416 0.880988 0.537951 11.00000 -1.50000 H32I 2 0.521973 0.872135 0.557748 11.00000 -1.50000 AFIX 0 C331 1 0.238890 0.754386 0.517618 11.00000 0.03150 0.03238 = 0.01792 0.00120 0.00042 0.01234 AFIX 23 H33A 2 0.183887 0.753285 0.509094 11.00000 -1.20000 H33B 2 0.255857 0.812961 0.519112 11.00000 -1.20000 AFIX 0 C332 1 0.230547 0.718862 0.545238 11.00000 0.03619 0.03947 = 0.02123 0.00438 0.00217 0.00758 AFIX 23 H33C 2 0.285962 0.710492 0.553050 11.00000 -1.20000 H33D 2 0.202205 0.664714 0.544488 11.00000 -1.20000 AFIX 0 C333 1 0.180364 0.779339 0.562281 11.00000 0.03457 0.04441 = 0.01774 -0.00358 0.00036 0.00402 AFIX 23 H33E 2 0.182048 0.760330 0.580813 11.00000 -1.20000 H33F 2 0.206953 0.834372 0.561547 11.00000 -1.20000 AFIX 0 C334 1 0.090111 0.788033 0.553812 11.00000 0.03215 0.05391 = 0.05171 -0.00956 0.00511 0.00468 AFIX 137 H33G 2 0.087703 0.808674 0.535675 11.00000 -1.50000 H33H 2 0.061904 0.826958 0.565552 11.00000 -1.50000 H33I 2 0.062888 0.734040 0.554782 11.00000 -1.50000 AFIX 0 C341 1 0.279951 0.619305 0.497580 11.00000 0.02472 0.02821 = 0.03126 -0.00132 0.00091 0.01011 AFIX 23 H34A 2 0.281509 0.595008 0.515474 11.00000 -1.20000 H34B 2 0.324212 0.592592 0.487156 11.00000 -1.20000 AFIX 0 C342 1 0.197558 0.597596 0.485130 11.00000 0.03121 0.03915 = 0.02538 0.00067 0.00180 0.01240 AFIX 23 H34C 2 0.197888 0.613015 0.466254 11.00000 -1.20000 H34D 2 0.152648 0.628567 0.493950 11.00000 -1.20000 AFIX 0 C343 1 0.182794 0.505160 0.487957 11.00000 0.02954 0.04523 = 0.03681 0.00313 0.00604 -0.00225 AFIX 23 H34E 2 0.230715 0.475138 0.480524 11.00000 -1.20000 H34F 2 0.179267 0.491291 0.506922 11.00000 -1.20000 AFIX 0 C344 1 0.104704 0.475566 0.474318 11.00000 0.03132 0.05886 = 0.05474 0.00076 0.01050 -0.00561 AFIX 137 H34G 2 0.057074 0.506085 0.481201 11.00000 -1.50000 H34H 2 0.097170 0.416403 0.477642 11.00000 -1.50000 H34I 2 0.109474 0.485114 0.455311 11.00000 -1.50000 AFIX 0 N4 3 0.754714 0.754714 0.500000 10.50000 0.06393 0.06393 = 0.03482 -0.00118 0.00118 -0.03611 C41 1 0.705693 0.705693 0.500000 10.50000 0.04029 0.04029 = 0.02499 -0.00292 0.00292 -0.00707 C42 1 0.640774 0.640774 0.500000 10.50000 0.03992 0.03992 = 0.06527 -0.01180 0.01180 -0.01185 N5 3 0.222800 0.222800 0.500000 10.50000 0.10682 0.10682 = 0.04650 -0.01559 0.01559 -0.06222 C51 1 0.271867 0.271867 0.500000 10.50000 0.04783 0.04783 = 0.03428 -0.00147 0.00147 -0.01104 C52 1 0.334930 0.334930 0.500000 10.50000 0.04019 0.04019 = 0.11791 0.02673 -0.02673 -0.01704 HKLF 4 REM rje260 in P4(1)2(1)2 REM R1 = 0.0400 for 14323 Fo > 4sig(Fo) and 0.0484 for all 15970 data REM 724 parameters refined using 0 restraints END WGHT 0.0308 27.8009 REM Highest difference peak 0.892, deepest hole -1.333, 1-sigma level 0.117 Q1 1 0.5288 0.5141 0.3842 11.00000 0.05 0.89 Q2 1 0.5379 0.4986 0.3873 11.00000 0.05 0.87 Q3 1 0.6611 0.5167 0.4324 11.00000 0.05 0.84 Q4 1 0.5741 0.5149 0.4188 11.00000 0.05 0.76 Q5 1 0.4560 0.4399 0.3774 11.00000 0.05 0.73 Q6 1 0.2810 0.4975 0.4233 11.00000 0.05 0.73 Q7 1 0.3650 0.4877 0.4092 11.00000 0.05 0.72 Q8 1 0.5936 0.4522 0.4208 11.00000 0.05 0.72 Q9 1 0.4199 0.6455 0.4225 11.00000 0.05 0.72 Q10 1 0.4997 0.3947 0.4328 11.00000 0.05 0.70 ; #===END