# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. #=============================================================================== _journal_coden_Cambridge 0182 # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Marta E. G. Mosquera Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; _publ_contact_author_phone '0034 91 8854779' _publ_contact_author_fax '0034 91 8854683' _publ_contact_author_email martaeg.mosquera@uah.es _publ_contact_letter ; Alcal\'a 04/06/2008 Please receive the CIF for the paper submitted to be published in Chem. Commun. Thank you very much. Dr. Marta E. G. Mosquera. ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Mercury or Silver Atoms Bridging Trinuclear Titanium Imido-Nitrido Systems ; # The loop structure below should contain the names and addresses of all #authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Avelino Martin' ; Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; 'Noelia Martinez-Espada' ; Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; 'Miguel Mena' ; Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; 'Marta E. G. Mosquera' ; Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; ; A.Perez-Redondo ; ; Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; 'Carlos Yelamos' ; Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; _publ_requested_category FM _publ_contact_author_name 'Marta E. G. Mosquera' #========================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 699910' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H48 Ag Cl N4 Ti3, 2(C7 H8)' _chemical_formula_sum 'C44 H64 Ag Cl N4 Ti3' _chemical_formula_weight 936.01 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' Cl Cl 0.1484 0.1585 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.549(3) _cell_length_b 13.123(2) _cell_length_c 17.273(2) _cell_angle_alpha 75.127(9) _cell_angle_beta 74.609(11) _cell_angle_gamma 70.225(14) _cell_volume 2334.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 95 _cell_measurement_theta_max 20.413 _cell_measurement_theta_min 3.743 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.419 _exptl_crystal_size_mid 0.408 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_T_max 0.756 _exptl_special_details ; ? ; _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 49737 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10490 _reflns_number_gt 5858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1549P)^2^+9.4443P] 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 0.010(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10490 _refine_ls_number_parameters 569 _refine_ls_number_restraints 697 _refine_ls_R_factor_all 0.1660 _refine_ls_R_factor_gt 0.0967 _refine_ls_wR_factor_ref 0.3272 _refine_ls_wR_factor_gt 0.2612 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _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 Ag1 Ag 0.36891(9) 0.51128(6) 0.14063(6) 0.0805(4) Uani 1 1 d . A . Cl1 Cl 0.4596(3) 0.3352(2) 0.10531(15) 0.0689(7) Uani 1 1 d . . . Ti1 Ti 0.22985(12) 0.61670(12) 0.29948(8) 0.0415(4) Uani 1 1 d . A . Ti2 Ti 0.19888(11) 0.74703(11) 0.14296(8) 0.0394(4) Uani 1 1 d . . . Ti3 Ti 0.43252(11) 0.68935(10) 0.19287(8) 0.0358(3) Uani 1 1 d . A . N1 N 0.2561(6) 0.7528(6) 0.2377(4) 0.0422(14) Uani 1 1 d . A . N2 N 0.4108(6) 0.5547(5) 0.2653(4) 0.0407(14) Uani 1 1 d . A . H2 H 0.4642 0.5082 0.2982 0.049 Uiso 1 1 calc R . . N3 N 0.3771(5) 0.6968(5) 0.0929(4) 0.0403(13) Uani 1 1 d . A . H3 H 0.4125 0.7240 0.0414 0.048 Uiso 1 1 calc R . . N4 N 0.1570(5) 0.6147(6) 0.2096(4) 0.0446(15) Uani 1 1 d . A . H4 H 0.0839 0.5990 0.2153 0.053 Uiso 1 1 calc R . . C10 C 0.059(2) 0.631(2) 0.4103(11) 0.072(2) Uani 0.578(8) 1 d PDU A 1 C11 C 0.078(2) 0.528(2) 0.3911(10) 0.068(2) Uani 0.578(8) 1 d PDU A 1 C12 C 0.196(2) 0.4606(19) 0.4078(10) 0.069(2) Uani 0.578(8) 1 d PDU A 1 C13 C 0.249(2) 0.522(2) 0.4375(11) 0.069(2) Uani 0.578(8) 1 d PDU A 1 C14 C 0.170(2) 0.627(2) 0.4392(13) 0.070(2) Uani 0.578(8) 1 d PDU A 1 C16 C 0.3732(19) 0.459(2) 0.4620(11) 0.089(4) Uani 0.578(8) 1 d PU A 1 H16A H 0.3972 0.3851 0.4518 0.134 Uiso 0.578(8) 1 calc PR A 1 H16B H 0.3658 0.4563 0.5191 0.134 Uiso 0.578(8) 1 calc PR A 1 H16C H 0.4358 0.4942 0.4308 0.134 Uiso 0.578(8) 1 calc PR A 1 C17 C 0.197(2) 0.711(2) 0.4690(12) 0.087(3) Uani 0.578(8) 1 d PU A 1 H17A H 0.1288 0.7780 0.4650 0.130 Uiso 0.578(8) 1 calc PR A 1 H17B H 0.2731 0.7253 0.4364 0.130 Uiso 0.578(8) 1 calc PR A 1 H17C H 0.2056 0.6850 0.5250 0.130 Uiso 0.578(8) 1 calc PR A 1 C15 C 0.211(2) 0.3528(19) 0.3866(12) 0.087(3) Uani 0.578(8) 1 d PU A 1 H15A H 0.2896 0.3018 0.3972 0.131 Uiso 0.578(8) 1 calc PR A 1 H15B H 0.2092 0.3634 0.3297 0.131 Uiso 0.578(8) 1 calc PR A 1 H15C H 0.1436 0.3239 0.4191 0.131 Uiso 0.578(8) 1 calc PR A 1 C18 C -0.041(2) 0.750(2) 0.4099(12) 0.094(4) Uani 0.578(8) 1 d PU A 1 H18A H -0.0098 0.7964 0.4292 0.141 Uiso 0.578(8) 1 calc PR A 1 H18B H -0.1193 0.7438 0.4449 0.141 Uiso 0.578(8) 1 calc PR A 1 H18C H -0.0546 0.7830 0.3552 0.141 Uiso 0.578(8) 1 calc PR A 1 C19 C -0.036(2) 0.526(2) 0.3651(11) 0.083(3) Uani 0.578(8) 1 d PU A 1 H19A H -0.0962 0.5975 0.3623 0.124 Uiso 0.578(8) 1 calc PR A 1 H19B H -0.0736 0.4732 0.4042 0.124 Uiso 0.578(8) 1 calc PR A 1 H19C H -0.0121 0.5050 0.3123 0.124 Uiso 0.578(8) 1 calc PR A 1 C10' C 0.130(3) 0.488(3) 0.4005(16) 0.070(2) Uani 0.422(8) 1 d PU A 2 C11' C 0.041(3) 0.598(3) 0.3963(15) 0.069(2) Uani 0.422(8) 1 d PU A 2 C12' C 0.238(3) 0.493(3) 0.4269(17) 0.070(2) Uani 0.422(8) 1 d PU A 2 C13' C 0.208(3) 0.597(3) 0.4434(18) 0.069(2) Uani 0.422(8) 1 d PU A 2 C14' C 0.091(3) 0.663(3) 0.4239(14) 0.069(2) Uani 0.422(8) 1 d PU A 2 C15' C 0.3030 0.3616 0.4253 0.091(4) Uani 0.422(8) 1 d PU A 2 H15D H 0.2575 0.3370 0.3982 0.137 Uiso 0.422(8) 1 calc PR A 2 H15E H 0.3009 0.3211 0.4803 0.137 Uiso 0.422(8) 1 calc PR A 2 H15F H 0.3885 0.3495 0.3965 0.137 Uiso 0.422(8) 1 calc PR A 2 C16' C 0.290(3) 0.635(3) 0.4799(15) 0.087(4) Uani 0.422(8) 1 d PU A 2 H16D H 0.2468 0.7086 0.4905 0.130 Uiso 0.422(8) 1 calc PR A 2 H16E H 0.3676 0.6355 0.4419 0.130 Uiso 0.422(8) 1 calc PR A 2 H16F H 0.3069 0.5863 0.5300 0.130 Uiso 0.422(8) 1 calc PR A 2 C17' C 0.058(3) 0.774(3) 0.4445(16) 0.088(4) Uani 0.422(8) 1 d PU A 2 H17D H -0.0218 0.8172 0.4314 0.133 Uiso 0.422(8) 1 calc PR A 2 H17E H 0.1211 0.8091 0.4137 0.133 Uiso 0.422(8) 1 calc PR A 2 H17F H 0.0545 0.7661 0.5018 0.133 Uiso 0.422(8) 1 calc PR A 2 C18' C 0.042(3) 0.435(3) 0.3659(14) 0.075(3) Uani 0.422(8) 1 d PU A 2 H18D H 0.0865 0.3605 0.3599 0.113 Uiso 0.422(8) 1 calc PR A 2 H18E H 0.0249 0.4785 0.3139 0.113 Uiso 0.422(8) 1 calc PR A 2 H18F H -0.0360 0.4374 0.4041 0.113 Uiso 0.422(8) 1 calc PR A 2 C19' C -0.094(3) 0.672(3) 0.3798(15) 0.086(4) Uani 0.422(8) 1 d PU A 2 H19D H -0.1115 0.7434 0.3927 0.129 Uiso 0.422(8) 1 calc PR A 2 H19E H -0.1565 0.6376 0.4133 0.129 Uiso 0.422(8) 1 calc PR A 2 H19F H -0.0962 0.6801 0.3233 0.129 Uiso 0.422(8) 1 calc PR A 2 C20 C 0.0966(10) 0.9323(9) 0.0898(7) 0.0705(17) Uani 1 1 d U A . C21 C 0.0081(10) 0.8853(10) 0.1314(7) 0.0771(18) Uani 1 1 d U A . C22 C 0.0124(9) 0.7980(9) 0.0909(7) 0.0741(17) Uani 1 1 d U A . C23 C 0.1195(9) 0.8011(8) 0.0189(6) 0.0641(16) Uani 1 1 d U A . C24 C 0.1625(9) 0.8847(8) 0.0249(6) 0.0610(16) Uani 1 1 d U A . C25 C 0.2688(11) 0.9224(10) -0.0380(7) 0.085(3) Uani 1 1 d U . . H25A H 0.3011 0.8775 -0.0793 0.128 Uiso 1 1 calc R A . H25B H 0.3347 0.9155 -0.0112 0.128 Uiso 1 1 calc R . . H25C H 0.2369 0.9980 -0.0629 0.128 Uiso 1 1 calc R . . C26 C 0.1236(13) 1.0287(10) 0.1118(9) 0.094(3) Uani 1 1 d U . . H26A H 0.0672 1.0480 0.1612 0.141 Uiso 1 1 calc R A . H26B H 0.1116 1.0913 0.0682 0.141 Uiso 1 1 calc R . . H26C H 0.2085 1.0063 0.1195 0.141 Uiso 1 1 calc R . . C27 C -0.0909(14) 0.9162(13) 0.2080(8) 0.119(4) Uani 1 1 d U . . H27A H -0.1445 0.8690 0.2240 0.179 Uiso 1 1 calc R A . H27B H -0.1404 0.9915 0.1960 0.179 Uiso 1 1 calc R . . H27C H -0.0495 0.9072 0.2517 0.179 Uiso 1 1 calc R . . C28 C -0.0736(12) 0.7282(12) 0.1110(10) 0.108(3) Uani 1 1 d U . . H28A H -0.0482 0.6803 0.0720 0.162 Uiso 1 1 calc R A . H28B H -0.1578 0.7745 0.1091 0.162 Uiso 1 1 calc R . . H28C H -0.0705 0.6849 0.1648 0.162 Uiso 1 1 calc R . . C29 C 0.1715(14) 0.7305(11) -0.0468(8) 0.099(3) Uani 1 1 d U . . H29A H 0.1238 0.6796 -0.0372 0.149 Uiso 1 1 calc R A . H29B H 0.2577 0.6905 -0.0452 0.149 Uiso 1 1 calc R . . H29C H 0.1658 0.7769 -0.0994 0.149 Uiso 1 1 calc R . . C30 C 0.6536(7) 0.6518(7) 0.1358(5) 0.0454(13) Uani 1 1 d U . . C31 C 0.5969(7) 0.7657(6) 0.1086(5) 0.0434(13) Uani 1 1 d U A . C32 C 0.5419(7) 0.8183(7) 0.1781(5) 0.0447(13) Uani 1 1 d U . . C33 C 0.5704(8) 0.7346(7) 0.2488(5) 0.0480(13) Uani 1 1 d U A . C34 C 0.6399(7) 0.6334(7) 0.2214(5) 0.0476(13) Uani 1 1 d U A . C35 C 0.7195(9) 0.5663(8) 0.0819(6) 0.061(2) Uani 1 1 d U A . H35A H 0.7171 0.6005 0.0259 0.092 Uiso 1 1 calc R . . H35B H 0.6780 0.5098 0.0973 0.092 Uiso 1 1 calc R . . H35C H 0.8052 0.5342 0.0884 0.092 Uiso 1 1 calc R . . C36 C 0.5992(8) 0.8235(7) 0.0212(5) 0.0526(18) Uani 1 1 d U . . H36A H 0.6407 0.7708 -0.0142 0.079 Uiso 1 1 calc R A . H36B H 0.6436 0.8775 0.0092 0.079 Uiso 1 1 calc R . . H36C H 0.5148 0.8593 0.0129 0.079 Uiso 1 1 calc R . . C37 C 0.4739(10) 0.9380(7) 0.1771(6) 0.062(2) Uani 1 1 d U A . H37A H 0.4466 0.9515 0.2320 0.093 Uiso 1 1 calc R . . H37B H 0.4023 0.9581 0.1521 0.093 Uiso 1 1 calc R . . H37C H 0.5292 0.9813 0.1463 0.093 Uiso 1 1 calc R . . C38 C 0.5370(10) 0.7517(9) 0.3362(6) 0.066(2) Uani 1 1 d U . . H38A H 0.4912 0.8274 0.3383 0.099 Uiso 1 1 calc R A . H38B H 0.6124 0.7330 0.3568 0.099 Uiso 1 1 calc R . . H38C H 0.4861 0.7055 0.3689 0.099 Uiso 1 1 calc R . . C39 C 0.6940(9) 0.5250(8) 0.2765(7) 0.067(2) Uani 1 1 d U . . H39A H 0.7353 0.4683 0.2442 0.101 Uiso 1 1 calc R A . H39B H 0.6273 0.5046 0.3176 0.101 Uiso 1 1 calc R . . H39C H 0.7533 0.5339 0.3021 0.101 Uiso 1 1 calc R . . C1D C 0.5868(16) 0.1396(16) 0.2788(11) 0.122(3) Uani 1 1 d U . . H1D H 0.5606 0.1453 0.2310 0.147 Uiso 1 1 calc R . . C2D C 0.6047(16) 0.2282(17) 0.2979(11) 0.124(3) Uani 1 1 d U . . H2D H 0.5935 0.2949 0.2613 0.148 Uiso 1 1 calc R . . C3D C 0.6385(16) 0.2196(17) 0.3694(11) 0.128(3) Uani 1 1 d U . . H3D H 0.6476 0.2820 0.3802 0.154 Uiso 1 1 calc R . . C4D C 0.6588(16) 0.1304(17) 0.4232(12) 0.129(3) Uani 1 1 d U . . H4D H 0.6822 0.1299 0.4709 0.155 Uiso 1 1 calc R . . C5D C 0.6455(17) 0.0330(18) 0.4102(12) 0.134(3) Uani 1 1 d U . . C6D C 0.6101(16) 0.0404(17) 0.3351(11) 0.129(3) Uani 1 1 d U . . H6D H 0.6024 -0.0221 0.3234 0.155 Uiso 1 1 calc R . . C9D C 0.2080(18) 0.211(2) 0.2364(15) 0.178(5) Uani 1 1 d DU . . H9D H 0.2791 0.2321 0.2082 0.213 Uiso 1 1 calc R . . C12D C -0.020(2) 0.232(2) 0.2597(14) 0.172(5) Uani 1 1 d DU . . H12D H -0.0985 0.2698 0.2460 0.207 Uiso 1 1 calc R . . C11D C 0.0816(19) 0.260(2) 0.2205(16) 0.175(5) Uani 1 1 d DU . . C10D C 0.091(2) 0.338(2) 0.1575(16) 0.182(6) Uani 1 1 d U . . H10A H 0.1100 0.3086 0.1084 0.274 Uiso 1 1 calc R . . H10B H 0.1575 0.3661 0.1578 0.274 Uiso 1 1 calc R . . H10C H 0.0136 0.3957 0.1594 0.274 Uiso 1 1 calc R . . C7D C 0.6676(19) -0.0606(17) 0.4736(12) 0.161(6) Uani 1 1 d U . . H7D1 H 0.7158 -0.0510 0.5072 0.241 Uiso 1 1 calc R . . H7D2 H 0.7130 -0.1252 0.4500 0.241 Uiso 1 1 calc R . . H7D3 H 0.5888 -0.0690 0.5062 0.241 Uiso 1 1 calc R . . C13D C -0.003(2) 0.137(2) 0.3263(15) 0.181(5) Uani 1 1 d DU . . H13D H -0.0717 0.1120 0.3524 0.217 Uiso 1 1 calc R . . C15T C 0.201(2) 0.129(2) 0.2993(16) 0.185(6) Uani 1 1 d DU . . H15T H 0.2797 0.0911 0.3116 0.222 Uiso 1 1 calc R . . C14D C 0.107(2) 0.083(2) 0.3538(16) 0.186(6) Uani 1 1 d DU . . H14D H 0.1184 0.0264 0.3990 0.223 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 Ag1 0.1018(7) 0.0489(5) 0.1063(7) -0.0232(4) -0.0550(6) -0.0083(4) Cl1 0.0796(16) 0.0611(14) 0.0647(14) -0.0264(11) -0.0172(12) -0.0054(12) Ti1 0.0382(7) 0.0568(8) 0.0327(7) -0.0052(6) -0.0087(5) -0.0188(6) Ti2 0.0287(6) 0.0495(8) 0.0368(7) -0.0046(6) -0.0106(5) -0.0065(5) Ti3 0.0319(6) 0.0394(7) 0.0396(7) -0.0052(5) -0.0124(5) -0.0122(5) N1 0.037(3) 0.055(4) 0.033(3) -0.006(3) -0.003(2) -0.016(3) N2 0.040(3) 0.049(4) 0.038(3) -0.001(3) -0.017(3) -0.018(3) N3 0.034(3) 0.044(3) 0.040(3) 0.001(3) -0.008(2) -0.014(3) N4 0.030(3) 0.067(4) 0.041(3) -0.012(3) -0.005(2) -0.019(3) C10 0.076(4) 0.100(5) 0.040(3) -0.004(3) 0.001(3) -0.040(4) C11 0.074(4) 0.099(5) 0.038(3) -0.003(3) -0.004(3) -0.046(4) C12 0.077(4) 0.097(5) 0.039(3) -0.002(3) -0.004(3) -0.045(4) C13 0.077(4) 0.099(5) 0.037(3) -0.002(3) -0.008(3) -0.043(4) C14 0.080(5) 0.099(5) 0.039(3) -0.008(3) -0.004(3) -0.043(4) C16 0.083(7) 0.127(9) 0.042(7) 0.018(7) -0.020(6) -0.031(7) C17 0.107(7) 0.109(7) 0.055(6) -0.023(6) -0.009(6) -0.045(6) C15 0.105(7) 0.098(6) 0.057(6) -0.009(5) 0.001(6) -0.043(6) C18 0.087(6) 0.112(7) 0.057(6) 0.000(6) 0.006(5) -0.022(6) C19 0.079(6) 0.120(8) 0.056(6) 0.000(6) -0.009(5) -0.051(6) C10' 0.077(4) 0.098(5) 0.040(3) -0.004(3) -0.002(3) -0.046(4) C11' 0.074(4) 0.099(5) 0.039(3) -0.005(4) -0.003(3) -0.045(4) C12' 0.077(4) 0.098(5) 0.039(3) -0.002(3) -0.004(3) -0.043(4) C13' 0.077(4) 0.099(5) 0.038(3) -0.005(3) -0.005(3) -0.044(4) C14' 0.077(5) 0.098(5) 0.039(3) -0.008(3) -0.002(3) -0.043(4) C15' 0.093(7) 0.101(6) 0.057(6) 0.005(6) 0.007(6) -0.031(6) C16' 0.103(10) 0.126(11) 0.051(9) -0.014(9) -0.021(8) -0.056(9) C17' 0.105(8) 0.105(7) 0.057(7) -0.022(6) -0.001(7) -0.040(6) C18' 0.092(7) 0.097(7) 0.047(6) -0.009(5) -0.003(5) -0.050(6) C19' 0.075(7) 0.115(8) 0.053(7) 0.005(7) 0.001(6) -0.034(6) C20 0.065(3) 0.066(4) 0.073(4) -0.003(3) -0.036(3) 0.001(3) C21 0.056(3) 0.081(4) 0.077(4) 0.002(3) -0.034(3) 0.004(3) C22 0.051(3) 0.082(4) 0.091(4) 0.014(3) -0.047(3) -0.017(3) C23 0.060(3) 0.067(3) 0.071(3) -0.004(3) -0.046(3) -0.007(3) C24 0.059(3) 0.060(3) 0.065(3) 0.000(3) -0.039(3) -0.007(3) C25 0.070(5) 0.080(6) 0.087(6) 0.020(5) -0.031(4) -0.014(4) C26 0.105(7) 0.069(6) 0.104(7) -0.020(5) -0.041(6) 0.000(5) C27 0.091(7) 0.120(8) 0.086(6) 0.000(6) -0.012(5) 0.027(6) C28 0.076(6) 0.114(7) 0.138(8) 0.026(6) -0.057(6) -0.041(5) C29 0.118(7) 0.093(6) 0.092(6) -0.032(5) -0.066(5) 0.009(6) C30 0.036(3) 0.049(3) 0.057(3) -0.011(2) -0.014(2) -0.016(2) C31 0.039(3) 0.048(3) 0.052(3) -0.010(2) -0.013(2) -0.019(2) C32 0.045(3) 0.047(3) 0.052(3) -0.009(2) -0.015(2) -0.021(2) C33 0.047(3) 0.051(3) 0.056(3) -0.008(2) -0.019(2) -0.023(2) C34 0.040(3) 0.052(3) 0.061(3) -0.006(2) -0.023(2) -0.019(2) C35 0.052(4) 0.057(4) 0.076(5) -0.023(4) -0.011(4) -0.010(4) C36 0.054(4) 0.059(4) 0.052(4) -0.007(3) -0.012(3) -0.027(4) C37 0.080(5) 0.047(4) 0.059(5) -0.012(3) -0.009(4) -0.018(4) C38 0.079(5) 0.075(5) 0.053(4) -0.013(4) -0.017(4) -0.030(4) C39 0.054(4) 0.061(4) 0.090(6) 0.008(4) -0.042(4) -0.016(4) C1D 0.105(6) 0.135(7) 0.118(6) -0.021(5) -0.020(5) -0.026(6) C2D 0.106(6) 0.138(7) 0.120(6) -0.021(6) -0.024(5) -0.027(6) C3D 0.108(6) 0.145(7) 0.122(6) -0.021(6) -0.025(5) -0.026(6) C4D 0.104(6) 0.148(7) 0.121(6) -0.016(5) -0.022(5) -0.024(6) C5D 0.107(5) 0.143(7) 0.124(6) -0.007(5) -0.015(5) -0.019(6) C6D 0.108(6) 0.138(7) 0.122(6) -0.016(5) -0.013(5) -0.024(6) C9D 0.121(6) 0.232(13) 0.220(12) -0.167(10) 0.042(8) -0.068(8) C12D 0.120(6) 0.231(13) 0.217(12) -0.169(10) 0.038(8) -0.076(8) C11D 0.124(6) 0.232(13) 0.218(12) -0.167(10) 0.039(8) -0.074(8) C10D 0.146(9) 0.236(14) 0.213(14) -0.161(11) 0.034(9) -0.080(9) C7D 0.123(9) 0.154(9) 0.145(9) 0.014(8) -0.009(8) -0.008(8) C13D 0.126(6) 0.234(13) 0.224(12) -0.166(10) 0.039(8) -0.069(8) C15T 0.126(6) 0.234(13) 0.226(12) -0.163(10) 0.044(8) -0.062(8) C14D 0.129(7) 0.235(13) 0.227(12) -0.162(10) 0.041(8) -0.064(8) _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 Ag1 Cl1 2.358(2) . ? Ag1 N3 2.387(6) . ? Ag1 N4 2.507(6) . ? Ag1 N2 2.563(6) . ? Ag1 Ti2 3.0561(17) . ? Ag1 Ti3 3.0676(15) . ? Ag1 Ti1 3.1824(17) . ? Ti1 N1 1.907(7) . ? Ti1 N2 1.954(6) . ? Ti1 N4 1.962(6) . ? Ti1 C14' 2.40(2) . ? Ti1 C12' 2.38(3) . ? Ti1 C13' 2.39(3) . ? Ti1 C14 2.35(2) . ? Ti1 C10 2.351(18) . ? Ti1 C13 2.42(2) . ? Ti1 C10' 2.45(3) . ? Ti1 C11 2.427(18) . ? Ti1 C11' 2.42(3) . ? Ti2 N1 1.948(6) . ? Ti2 N4 1.955(7) . ? Ti2 N3 1.961(6) . ? Ti2 C21 2.352(10) . ? Ti2 C20 2.374(10) . ? Ti2 C22 2.375(8) . ? Ti2 C24 2.377(9) . ? Ti2 C23 2.400(8) . ? Ti2 Ti3 2.8487(18) . ? Ti3 N2 1.936(6) . ? Ti3 N1 1.947(6) . ? Ti3 N3 1.965(6) . ? Ti3 C32 2.361(7) . ? Ti3 C33 2.360(7) . ? Ti3 C34 2.402(7) . ? Ti3 C31 2.408(7) . ? Ti3 C30 2.408(8) . ? N2 H2 0.9100 . ? N3 H3 0.9100 . ? N4 H4 0.9100 . ? C10 C11 1.40(3) . ? C10 C14 1.48(4) . ? C10 C18 1.61(3) . ? C11 C12 1.40(3) . ? C11 C19 1.52(3) . ? C12 C13 1.42(3) . ? C12 C15 1.49(3) . ? C13 C14 1.37(4) . ? C13 C16 1.50(3) . ? C14 C17 1.48(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C10' C11' 1.46(5) . ? C10' C12' 1.47(5) . ? C10' C18' 1.69(4) . ? C11' C14' 1.41(4) . ? C11' C19' 1.59(4) . ? C12' C13' 1.37(5) . ? C12' C15' 1.64(4) . ? C12' C14' 2.30(5) . ? C13' C14' 1.41(4) . ? C13' C16' 1.54(4) . ? C14' C17' 1.48(4) . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C20 C21 1.323(16) . ? C20 C24 1.346(15) . ? C20 C26 1.555(17) . ? C21 C22 1.470(17) . ? C21 C27 1.544(17) . ? C22 C28 1.488(16) . ? C22 C23 1.507(15) . ? C23 C24 1.384(14) . ? C23 C29 1.518(15) . ? C24 C25 1.536(15) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C34 1.410(12) . ? C30 C31 1.423(11) . ? C30 C35 1.512(12) . ? C31 C32 1.430(11) . ? C31 C36 1.503(11) . ? C32 C33 1.444(11) . ? C32 C37 1.498(12) . ? C33 C34 1.425(12) . ? C33 C38 1.511(12) . ? C34 C39 1.530(12) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C1D C2D 1.38(2) . ? C1D C6D 1.40(2) . ? C1D H1D 0.9300 . ? C2D C3D 1.36(2) . ? C2D H2D 0.9300 . ? C3D C4D 1.29(2) . ? C3D H3D 0.9300 . ? C4D C5D 1.42(3) . ? C4D H4D 0.9300 . ? C5D C6D 1.43(3) . ? C5D C7D 1.42(2) . ? C6D H6D 0.9300 . ? C9D C15T 1.32(3) . ? C9D C11D 1.452(18) . ? C9D H9D 0.9300 . ? C12D C13D 1.459(18) . ? C12D C11D 1.31(3) . ? C12D H12D 0.9300 . ? C11D C10D 1.30(3) . ? C10D H10A 0.9600 . ? C10D H10B 0.9600 . ? C10D H10C 0.9600 . ? C7D H7D1 0.9600 . ? C7D H7D2 0.9600 . ? C7D H7D3 0.9600 . ? C13D C14D 1.37(3) . ? C13D H13D 0.9300 . ? C15T C14D 1.429(17) . ? C15T H15T 0.9300 . ? C14D H14D 0.9300 . ? 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 Cl1 Ag1 N3 140.98(17) . . ? Cl1 Ag1 N4 135.61(17) . . ? N3 Ag1 N4 79.0(2) . . ? Cl1 Ag1 N2 121.39(16) . . ? N3 Ag1 N2 78.2(2) . . ? N4 Ag1 N2 75.7(2) . . ? Cl1 Ag1 Ti2 160.20(8) . . ? N3 Ag1 Ti2 39.91(14) . . ? N4 Ag1 Ti2 39.62(16) . . ? N2 Ag1 Ti2 78.02(15) . . ? Cl1 Ag1 Ti3 141.99(8) . . ? N3 Ag1 Ti3 39.82(15) . . ? N4 Ag1 Ti3 78.56(15) . . ? N2 Ag1 Ti3 38.95(14) . . ? Ti2 Ag1 Ti3 55.44(4) . . ? Cl1 Ag1 Ti1 138.61(8) . . ? N3 Ag1 Ti1 78.48(15) . . ? N4 Ag1 Ti1 38.06(14) . . ? N2 Ag1 Ti1 37.87(14) . . ? Ti2 Ag1 Ti1 54.20(4) . . ? Ti3 Ag1 Ti1 54.14(4) . . ? N1 Ti1 N2 85.3(3) . . ? N1 Ti1 N4 86.2(3) . . ? N2 Ti1 N4 105.3(3) . . ? N1 Ti1 C14' 104.5(8) . . ? N2 Ti1 C14' 135.5(8) . . ? N4 Ti1 C14' 118.4(8) . . ? N1 Ti1 C12' 145.0(8) . . ? N2 Ti1 C12' 89.5(9) . . ? N4 Ti1 C12' 128.4(9) . . ? C14' Ti1 C12' 57.6(12) . . ? N1 Ti1 C13' 114.5(10) . . ? N2 Ti1 C13' 102.0(8) . . ? N4 Ti1 C13' 147.0(8) . . ? C14' Ti1 C13' 34.2(10) . . ? C12' Ti1 C13' 33.4(12) . . ? N1 Ti1 C14 109.4(7) . . ? N2 Ti1 C14 112.6(6) . . ? N4 Ti1 C14 139.8(7) . . ? C14' Ti1 C14 23.1(8) . . ? C12' Ti1 C14 42.2(10) . . ? C13' Ti1 C14 11.6(10) . . ? N1 Ti1 C10 115.8(6) . . ? N2 Ti1 C10 145.6(6) . . ? N4 Ti1 C10 103.1(7) . . ? C14' Ti1 C10 18.5(7) . . ? C12' Ti1 C10 57.3(10) . . ? C13' Ti1 C10 45.5(9) . . ? C14 Ti1 C10 36.7(8) . . ? N1 Ti1 C13 132.5(6) . . ? N2 Ti1 C13 88.7(6) . . ? N4 Ti1 C13 140.4(6) . . ? C14' Ti1 C13 52.5(9) . . ? C12' Ti1 C13 12.5(8) . . ? C13' Ti1 C13 22.9(9) . . ? C14 Ti1 C13 33.3(9) . . ? C10 Ti1 C13 56.9(8) . . ? N1 Ti1 C10' 159.8(9) . . ? N2 Ti1 C10' 113.5(9) . . ? N4 Ti1 C10' 95.4(8) . . ? C14' Ti1 C10' 57.1(10) . . ? C12' Ti1 C10' 35.5(11) . . ? C13' Ti1 C10' 56.3(11) . . ? C14 Ti1 C10' 57.7(10) . . ? C10 Ti1 C10' 44.2(10) . . ? C13 Ti1 C10' 45.6(9) . . ? N1 Ti1 C11 145.5(8) . . ? N2 Ti1 C11 129.0(7) . . ? N4 Ti1 C11 87.4(5) . . ? C14' Ti1 C11 50.6(9) . . ? C12' Ti1 C11 48.5(9) . . ? C13' Ti1 C11 60.8(10) . . ? C14 Ti1 C11 58.5(8) . . ? C10 Ti1 C11 34.1(8) . . ? C13 Ti1 C11 56.5(7) . . ? C10' Ti1 C11 15.9(8) . . ? N1 Ti1 C11' 125.0(10) . . ? N2 Ti1 C11' 147.1(9) . . ? N4 Ti1 C11' 90.6(7) . . ? C14' Ti1 C11' 34.1(9) . . ? C12' Ti1 C11' 58.6(11) . . ? C13' Ti1 C11' 56.6(10) . . ? C14 Ti1 C11' 49.8(9) . . ? C10 Ti1 C11' 15.6(7) . . ? C13 Ti1 C11' 62.1(9) . . ? C10' Ti1 C11' 35.0(11) . . ? C11 Ti1 C11' 21.3(8) . . ? N1 Ti2 N4 85.2(3) . . ? N1 Ti2 N3 86.3(3) . . ? N4 Ti2 N3 105.4(3) . . ? N1 Ti2 C21 109.5(4) . . ? N4 Ti2 C21 106.9(4) . . ? N3 Ti2 C21 144.9(3) . . ? N1 Ti2 C20 105.8(3) . . ? N4 Ti2 C20 139.5(3) . . ? N3 Ti2 C20 114.0(3) . . ? C21 Ti2 C20 32.5(4) . . ? N1 Ti2 C22 140.7(4) . . ? N4 Ti2 C22 89.3(3) . . ? N3 Ti2 C22 132.4(4) . . ? C21 Ti2 C22 36.2(4) . . ? C20 Ti2 C22 57.3(4) . . ? N1 Ti2 C24 128.9(3) . . ? N4 Ti2 C24 143.9(3) . . ? N3 Ti2 C24 90.2(3) . . ? C21 Ti2 C24 55.3(4) . . ? C20 Ti2 C24 32.9(4) . . ? C22 Ti2 C24 57.5(3) . . ? N1 Ti2 C23 161.9(3) . . ? N4 Ti2 C23 110.9(3) . . ? N3 Ti2 C23 96.8(3) . . ? C21 Ti2 C23 58.9(4) . . ? C20 Ti2 C23 56.7(4) . . ? C22 Ti2 C23 36.8(4) . . ? C24 Ti2 C23 33.7(3) . . ? N1 Ti2 Ti1 41.92(19) . . ? N4 Ti2 Ti1 43.53(18) . . ? N3 Ti2 Ti1 94.41(18) . . ? C21 Ti2 Ti1 118.5(3) . . ? C20 Ti2 Ti1 136.9(3) . . ? C22 Ti2 Ti1 124.1(3) . . ? C24 Ti2 Ti1 169.1(3) . . ? C23 Ti2 Ti1 154.3(3) . . ? N1 Ti2 Ti3 42.98(18) . . ? N4 Ti2 Ti3 93.66(18) . . ? N3 Ti2 Ti3 43.53(18) . . ? C21 Ti2 Ti3 144.9(3) . . ? C20 Ti2 Ti3 121.3(3) . . ? C22 Ti2 Ti3 175.6(3) . . ? C24 Ti2 Ti3 118.8(2) . . ? C23 Ti2 Ti3 138.8(3) . . ? Ti1 Ti2 Ti3 59.99(4) . . ? N1 Ti2 Ag1 91.0(2) . . ? N4 Ti2 Ag1 54.88(19) . . ? N3 Ti2 Ag1 51.34(18) . . ? C21 Ti2 Ag1 152.3(3) . . ? C20 Ti2 Ag1 157.7(3) . . ? C22 Ti2 Ag1 117.1(3) . . ? C24 Ti2 Ag1 124.8(3) . . ? C23 Ti2 Ag1 104.9(2) . . ? Ti1 Ti2 Ag1 65.17(5) . . ? Ti3 Ti2 Ag1 62.48(4) . . ? N2 Ti3 N1 84.8(3) . . ? N2 Ti3 N3 106.5(3) . . ? N1 Ti3 N3 86.2(3) . . ? N2 Ti3 C32 138.6(3) . . ? N1 Ti3 C32 108.9(3) . . ? N3 Ti3 C32 113.1(3) . . ? N2 Ti3 C33 103.0(3) . . ? N1 Ti3 C33 113.5(3) . . ? N3 Ti3 C33 145.9(3) . . ? C32 Ti3 C33 35.6(3) . . ? N2 Ti3 C34 87.0(3) . . ? N1 Ti3 C34 143.2(3) . . ? N3 Ti3 C34 130.5(3) . . ? C32 Ti3 C34 58.3(3) . . ? C33 Ti3 C34 34.8(3) . . ? N2 Ti3 C31 140.1(3) . . ? N1 Ti3 C31 133.9(3) . . ? N3 Ti3 C31 88.3(2) . . ? C32 Ti3 C31 34.9(3) . . ? C33 Ti3 C31 57.8(3) . . ? C34 Ti3 C31 56.9(3) . . ? N2 Ti3 C30 106.0(3) . . ? N1 Ti3 C30 167.0(3) . . ? N3 Ti3 C30 97.3(3) . . ? C32 Ti3 C30 58.2(3) . . ? C33 Ti3 C30 57.7(3) . . ? C34 Ti3 C30 34.1(3) . . ? C31 Ti3 C30 34.4(3) . . ? N2 Ti3 Ti1 43.24(18) . . ? N1 Ti3 Ti1 41.9(2) . . ? N3 Ti3 Ti1 94.27(18) . . ? C32 Ti3 Ti1 140.0(2) . . ? C33 Ti3 Ti1 119.2(2) . . ? C34 Ti3 Ti1 123.7(2) . . ? C31 Ti3 Ti1 174.65(19) . . ? C30 Ti3 Ti1 149.2(2) . . ? N2 Ti3 Ti2 94.11(18) . . ? N1 Ti3 Ti2 43.02(18) . . ? N3 Ti3 Ti2 43.44(18) . . ? C32 Ti3 Ti2 123.0(2) . . ? C33 Ti3 Ti2 149.8(2) . . ? C34 Ti3 Ti2 173.8(2) . . ? C31 Ti3 Ti2 120.05(19) . . ? C30 Ti3 Ti2 140.2(2) . . ? Ti1 Ti3 Ti2 59.92(5) . . ? N2 Ti3 Ag1 56.29(18) . . ? N1 Ti3 Ag1 90.6(2) . . ? N3 Ti3 Ag1 51.08(18) . . ? C32 Ti3 Ag1 154.9(2) . . ? C33 Ti3 Ag1 147.7(2) . . ? C34 Ti3 Ag1 114.0(2) . . ? C31 Ti3 Ag1 120.09(19) . . ? C30 Ti3 Ag1 101.29(19) . . ? Ti1 Ti3 Ag1 64.99(4) . . ? Ti2 Ti3 Ag1 62.07(4) . . ? Ti1 N1 Ti2 95.0(3) . . ? Ti1 N1 Ti3 95.2(3) . . ? Ti2 N1 Ti3 94.0(3) . . ? Ti3 N2 Ti1 94.0(3) . . ? Ti3 N2 Ag1 84.8(2) . . ? Ti1 N2 Ag1 88.5(2) . . ? Ti3 N2 H2 125.8 . . ? Ti1 N2 H2 125.8 . . ? Ag1 N2 H2 125.8 . . ? Ti2 N3 Ti3 93.0(3) . . ? Ti2 N3 Ag1 88.7(2) . . ? Ti3 N3 Ag1 89.1(2) . . ? Ti2 N3 H3 125.0 . . ? Ti3 N3 H3 125.0 . . ? Ag1 N3 H3 125.0 . . ? Ti2 N4 Ti1 93.1(3) . . ? Ti2 N4 Ag1 85.5(2) . . ? Ti1 N4 Ag1 90.0(2) . . ? Ti2 N4 H4 125.5 . . ? Ti1 N4 H4 125.5 . . ? Ag1 N4 H4 125.5 . . ? C11 C10 C14 108(2) . . ? C11 C10 C18 142(3) . . ? C14 C10 C18 110(2) . . ? C11 C10 Ti1 75.9(10) . . ? C14 C10 Ti1 71.7(11) . . ? C18 C10 Ti1 115.4(12) . . ? C12 C11 C10 107.3(19) . . ? C12 C11 C19 142(3) . . ? C10 C11 C19 110(3) . . ? C12 C11 Ti1 74.5(9) . . ? C10 C11 Ti1 70.0(10) . . ? C19 C11 Ti1 122.1(12) . . ? C11 C12 C13 108(2) . . ? C11 C12 C15 105(2) . . ? C13 C12 C15 147(3) . . ? C11 C12 Ti1 72.1(10) . . ? C13 C12 Ti1 71.5(11) . . ? C15 C12 Ti1 120.2(12) . . ? C14 C13 C12 110(2) . . ? C14 C13 C16 135(2) . . ? C12 C13 C16 114(3) . . ? C14 C13 Ti1 70.8(12) . . ? C12 C13 Ti1 74.6(10) . . ? C16 C13 Ti1 123.1(13) . . ? C13 C14 C10 106(2) . . ? C13 C14 C17 124(2) . . ? C10 C14 C17 131(2) . . ? C13 C14 Ti1 75.9(12) . . ? C10 C14 Ti1 71.6(11) . . ? C17 C14 Ti1 120.0(15) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11 C19 H19A 109.5 . . ? C11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C11' C10' C12' 106(3) . . ? C11' C10' C18' 94(3) . . ? C12' C10' C18' 159(3) . . ? C11' C10' Ti1 71.4(14) . . ? C12' C10' Ti1 69.6(15) . . ? C18' C10' Ti1 115.9(16) . . ? C10' C11' C14' 107(3) . . ? C10' C11' C19' 145(3) . . ? C14' C11' C19' 107(3) . . ? C10' C11' Ti1 73.6(15) . . ? C14' C11' Ti1 72.2(14) . . ? C19' C11' Ti1 121.5(17) . . ? C13' C12' C10' 107(3) . . ? C13' C12' C15' 163(3) . . ? C10' C12' C15' 89(2) . . ? C13' C12' C14' 34.7(18) . . ? C10' C12' C14' 72(2) . . ? C15' C12' C14' 161(2) . . ? C13' C12' Ti1 73.6(18) . . ? C10' C12' Ti1 74.9(16) . . ? C15' C12' Ti1 117.7(15) . . ? C14' C12' Ti1 61.7(10) . . ? C12' C13' C14' 112(3) . . ? C12' C13' C16' 124(3) . . ? C14' C13' C16' 124(4) . . ? C12' C13' Ti1 73.0(18) . . ? C14' C13' Ti1 73.3(15) . . ? C16' C13' Ti1 122(2) . . ? C13' C14' C11' 108(3) . . ? C13' C14' C17' 111(3) . . ? C11' C14' C17' 141(3) . . ? C13' C14' C12' 34(2) . . ? C11' C14' C12' 74(2) . . ? C17' C14' C12' 144(3) . . ? C13' C14' Ti1 72.4(16) . . ? C11' C14' Ti1 73.8(14) . . ? C17' C14' Ti1 122.0(18) . . ? C12' C14' Ti1 60.8(10) . . ? C12' C15' H15D 109.5 . . ? C12' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C12' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C13' C16' H16D 109.5 . . ? C13' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C13' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C14' C17' H17D 109.5 . . ? C14' C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C14' C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C10' C18' H18D 109.5 . . ? C10' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C10' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C11' C19' H19D 109.5 . . ? C11' C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C11' C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C21 C20 C24 110.7(11) . . ? C21 C20 C26 125.6(11) . . ? C24 C20 C26 123.7(11) . . ? C21 C20 Ti2 72.8(6) . . ? C24 C20 Ti2 73.7(6) . . ? C26 C20 Ti2 120.1(7) . . ? C20 C21 C22 109.2(10) . . ? C20 C21 C27 128.0(13) . . ? C22 C21 C27 122.8(12) . . ? C20 C21 Ti2 74.7(6) . . ? C22 C21 Ti2 72.8(5) . . ? C27 C21 Ti2 121.0(7) . . ? C21 C22 C28 129.1(12) . . ? C21 C22 C23 103.5(9) . . ? C28 C22 C23 127.3(12) . . ? C21 C22 Ti2 71.0(5) . . ? C28 C22 Ti2 123.8(7) . . ? C23 C22 Ti2 72.5(4) . . ? C24 C23 C22 104.4(9) . . ? C24 C23 C29 126.3(11) . . ? C22 C23 C29 129.3(10) . . ? C24 C23 Ti2 72.3(5) . . ? C22 C23 Ti2 70.7(5) . . ? C29 C23 Ti2 121.3(6) . . ? C20 C24 C23 112.3(10) . . ? C20 C24 C25 124.0(10) . . ? C23 C24 C25 123.6(10) . . ? C20 C24 Ti2 73.4(6) . . ? C23 C24 Ti2 74.1(5) . . ? C25 C24 Ti2 122.6(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C21 C27 H27A 109.5 . . ? C21 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C21 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C28 H28A 109.5 . . ? C22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 C29 H29A 109.5 . . ? C23 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C23 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C34 C30 C31 108.0(7) . . ? C34 C30 C35 126.1(8) . . ? C31 C30 C35 125.9(8) . . ? C34 C30 Ti3 72.7(4) . . ? C31 C30 Ti3 72.8(4) . . ? C35 C30 Ti3 121.2(5) . . ? C30 C31 C32 108.9(7) . . ? C30 C31 C36 126.1(7) . . ? C32 C31 C36 125.0(7) . . ? C30 C31 Ti3 72.8(4) . . ? C32 C31 Ti3 70.8(4) . . ? C36 C31 Ti3 124.7(5) . . ? C31 C32 C33 106.6(7) . . ? C31 C32 C37 126.5(7) . . ? C33 C32 C37 126.9(8) . . ? C31 C32 Ti3 74.4(4) . . ? C33 C32 Ti3 72.2(4) . . ? C37 C32 Ti3 121.2(6) . . ? C34 C33 C32 108.0(7) . . ? C34 C33 C38 125.8(8) . . ? C32 C33 C38 126.2(8) . . ? C34 C33 Ti3 74.2(4) . . ? C32 C33 Ti3 72.2(4) . . ? C38 C33 Ti3 121.1(6) . . ? C30 C34 C33 108.6(7) . . ? C30 C34 C39 126.5(8) . . ? C33 C34 C39 124.9(8) . . ? C30 C34 Ti3 73.2(4) . . ? C33 C34 Ti3 71.0(4) . . ? C39 C34 Ti3 123.5(5) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C2D C1D C6D 116.6(19) . . ? C2D C1D H1D 121.7 . . ? C6D C1D H1D 121.7 . . ? C1D C2D C3D 121(2) . . ? C1D C2D H2D 119.5 . . ? C3D C2D H2D 119.5 . . ? C4D C3D C2D 124(2) . . ? C4D C3D H3D 117.9 . . ? C2D C3D H3D 117.9 . . ? C3D C4D C5D 120(2) . . ? C3D C4D H4D 119.9 . . ? C5D C4D H4D 119.9 . . ? C6D C5D C7D 127(2) . . ? C6D C5D C4D 116.4(19) . . ? C7D C5D C4D 116(2) . . ? C5D C6D C1D 122(2) . . ? C5D C6D H6D 119.2 . . ? C1D C6D H6D 119.2 . . ? C15T C9D C11D 106(2) . . ? C15T C9D H9D 127.2 . . ? C11D C9D H9D 127.2 . . ? C13D C12D C11D 115(3) . . ? C13D C12D H12D 122.4 . . ? C11D C12D H12D 122.4 . . ? C10D C11D C9D 105(2) . . ? C10D C11D C12D 127(3) . . ? C9D C11D C12D 128(3) . . ? C11D C10D H10A 109.5 . . ? C11D C10D H10B 109.5 . . ? H10A C10D H10B 109.5 . . ? C11D C10D H10C 109.5 . . ? H10A C10D H10C 109.5 . . ? H10B C10D H10C 109.5 . . ? C5D C7D H7D1 109.5 . . ? C5D C7D H7D2 109.5 . . ? H7D1 C7D H7D2 109.5 . . ? C5D C7D H7D3 109.5 . . ? H7D1 C7D H7D3 109.5 . . ? H7D2 C7D H7D3 109.5 . . ? C14D C13D C12D 126(2) . . ? C14D C13D H13D 117.1 . . ? C12D C13D H13D 117.1 . . ? C9D C15T C14D 138(3) . . ? C9D C15T H15T 110.8 . . ? C14D C15T H15T 110.8 . . ? C13D C14D C15T 106(3) . . ? C13D C14D H14D 126.8 . . ? C15T C14D H14D 126.8 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.342 _refine_diff_density_min -2.445 _refine_diff_density_rms 0.155 #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-06-28 at 11:29:15 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : import dreduc sortav sortav_a struct data_5 _database_code_depnum_ccdc_archive 'CCDC 699911' _audit_creation_date 2008-06-28T11:29:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C60 H92 Hg2 N8 Ti6' _chemical_formula_sum 'C60 H92 Hg2 N8 Ti6' _chemical_formula_weight 1613.81 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' _space_group_IT_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.977(2) _cell_length_b 20.139(3) _cell_length_c 14.837(2) _cell_angle_alpha 90 _cell_angle_beta 104.01(2) _cell_angle_gamma 90 _cell_volume 3182.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 173 _cell_measurement_theta_min 3 _cell_measurement_theta_max 21 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.542 _exptl_crystal_size_mid 0.111 _exptl_crystal_size_min 0.109 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.051 0 1 0 0.028 -17 -1 1 0.254 18 -1 -1 0.264 1 -2 -18 0.026 -1 2 19 0.054 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.56 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 1.395 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.139 _diffrn_reflns_av_unetI/netI 0.1129 _diffrn_reflns_number 72220 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7307 _reflns_number_gt 4781 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR2002 (Giacovazzo,2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^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 none _refine_ls_number_reflns 7307 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.086 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.645 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.17 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.9275(6) 0.7287(3) 0.0539(5) 0.0259(16) Uani 1 1 d . . . C12 C 0.9024(6) 0.7266(3) 0.1437(4) 0.0253(16) Uani 1 1 d . . . C13 C 0.7909(6) 0.7626(3) 0.1406(4) 0.0264(16) Uani 1 1 d . . . C14 C 0.7462(6) 0.7867(3) 0.0489(4) 0.0224(15) Uani 1 1 d . . . C15 C 0.8295(5) 0.7661(3) -0.0049(4) 0.0198(14) Uani 1 1 d . . . C16 C 1.0358(6) 0.6941(3) 0.0252(5) 0.041(2) Uani 1 1 d . . . H16A H 1.0694 0.723 -0.0142 0.062 Uiso 1 1 calc R . . H16B H 1.0058 0.654 -0.0078 0.062 Uiso 1 1 calc R . . H16C H 1.1002 0.6834 0.0796 0.062 Uiso 1 1 calc R . . C17 C 0.9790(7) 0.6888(4) 0.2277(5) 0.047(2) Uani 1 1 d . . . H17A H 1.0605 0.6788 0.2182 0.071 Uiso 1 1 calc R . . H17B H 0.9366 0.6482 0.2352 0.071 Uiso 1 1 calc R . . H17C H 0.988 0.7155 0.2824 0.071 Uiso 1 1 calc R . . C18 C 0.7260(7) 0.7706(4) 0.2187(5) 0.042(2) Uani 1 1 d . . . H18A H 0.7874 0.7708 0.277 0.063 Uiso 1 1 calc R . . H18B H 0.6688 0.7344 0.2175 0.063 Uiso 1 1 calc R . . H18C H 0.6805 0.8118 0.2112 0.063 Uiso 1 1 calc R . . C19 C 0.6264(6) 0.8254(3) 0.0146(5) 0.0351(18) Uani 1 1 d . . . H19A H 0.6326 0.8519 -0.0378 0.053 Uiso 1 1 calc R . . H19B H 0.6131 0.8538 0.0633 0.053 Uiso 1 1 calc R . . H19C H 0.5571 0.7951 -0.0034 0.053 Uiso 1 1 calc R . . C20 C 0.8162(6) 0.7791(3) -0.1068(4) 0.0325(17) Uani 1 1 d . . . H20A H 0.898 0.7836 -0.1187 0.049 Uiso 1 1 calc R . . H20B H 0.7695 0.8193 -0.1244 0.049 Uiso 1 1 calc R . . H20C H 0.7728 0.7427 -0.1424 0.049 Uiso 1 1 calc R . . C21 C 1.0072(8) 0.9194(4) 0.4047(5) 0.0361(19) Uani 1 1 d . . . C22 C 0.9151(7) 0.9662(4) 0.3639(5) 0.0370(19) Uani 1 1 d . . . C23 C 0.9745(7) 1.0243(3) 0.3457(4) 0.0301(17) Uani 1 1 d . . . C24 C 1.1051(7) 1.0145(3) 0.3776(4) 0.0296(17) Uani 1 1 d . . . C25 C 1.1259(6) 0.9501(3) 0.4124(4) 0.0264(15) Uani 1 1 d . . . C26 C 0.9852(10) 0.8502(4) 0.4377(5) 0.069(3) Uani 1 1 d . . . H26A H 1.059 0.8237 0.4416 0.104 Uiso 1 1 calc R . . H26B H 0.9153 0.8303 0.3945 0.104 Uiso 1 1 calc R . . H26C H 0.9674 0.8529 0.4978 0.104 Uiso 1 1 calc R . . C27 C 0.7734(7) 0.9562(5) 0.3475(6) 0.068(3) Uani 1 1 d . . . H27A H 0.7306 0.9863 0.3001 0.102 Uiso 1 1 calc R . . H27B H 0.7483 0.9648 0.404 0.102 Uiso 1 1 calc R . . H27C H 0.7523 0.9113 0.3281 0.102 Uiso 1 1 calc R . . C28 C 0.9098(9) 1.0860(4) 0.3036(6) 0.066(3) Uani 1 1 d . . . H28A H 0.8306 1.0747 0.2627 0.1 Uiso 1 1 calc R . . H28B H 0.9611 1.1084 0.2692 0.1 Uiso 1 1 calc R . . H28C H 0.8962 1.1146 0.3519 0.1 Uiso 1 1 calc R . . C29 C 1.2070(8) 1.0655(4) 0.3749(6) 0.059(3) Uani 1 1 d . . . H29A H 1.2847 1.0431 0.3769 0.088 Uiso 1 1 calc R . . H29B H 1.2173 1.0947 0.4274 0.088 Uiso 1 1 calc R . . H29C H 1.1829 1.091 0.3186 0.088 Uiso 1 1 calc R . . C30 C 1.2507(8) 0.9183(5) 0.4587(6) 0.064(3) Uani 1 1 d . . . H30A H 1.2525 0.8735 0.4369 0.096 Uiso 1 1 calc R . . H30B H 1.2609 0.9181 0.5248 0.096 Uiso 1 1 calc R . . H30C H 1.3177 0.9432 0.4437 0.096 Uiso 1 1 calc R . . C31 C 1.3370(6) 0.9354(3) 0.0409(5) 0.0259(15) Uani 1 1 d . . . C32 C 1.3869(6) 0.9503(3) 0.1360(5) 0.0254(15) Uani 1 1 d . . . C33 C 1.3975(5) 0.8890(3) 0.1863(4) 0.0213(14) Uani 1 1 d . . . C34 C 1.3555(6) 0.8380(3) 0.1211(4) 0.0244(15) Uani 1 1 d . . . C35 C 1.3200(6) 0.8669(3) 0.0325(4) 0.0226(15) Uani 1 1 d . . . C36 C 1.3119(7) 0.9860(4) -0.0374(5) 0.045(2) Uani 1 1 d . . . H36A H 1.259 0.9665 -0.0921 0.068 Uiso 1 1 calc R . . H36B H 1.39 0.9993 -0.0502 0.068 Uiso 1 1 calc R . . H36C H 1.2709 1.0241 -0.0194 0.068 Uiso 1 1 calc R . . C37 C 1.4230(6) 1.0185(4) 0.1776(5) 0.041(2) Uani 1 1 d . . . H37A H 1.3963 1.0228 0.2343 0.062 Uiso 1 1 calc R . . H37B H 1.3831 1.052 0.1345 0.062 Uiso 1 1 calc R . . H37C H 1.5125 1.0237 0.1903 0.062 Uiso 1 1 calc R . . C38 C 1.4476(6) 0.8807(4) 0.2900(4) 0.0356(18) Uani 1 1 d . . . H38A H 1.4707 0.9233 0.318 0.053 Uiso 1 1 calc R . . H38B H 1.52 0.8523 0.3018 0.053 Uiso 1 1 calc R . . H38C H 1.384 0.8612 0.316 0.053 Uiso 1 1 calc R . . C39 C 1.3575(6) 0.7645(3) 0.1456(5) 0.0351(18) Uani 1 1 d . . . H39A H 1.4384 0.7531 0.184 0.053 Uiso 1 1 calc R . . H39B H 1.3413 0.7386 0.0897 0.053 Uiso 1 1 calc R . . H39C H 1.2941 0.7556 0.1786 0.053 Uiso 1 1 calc R . . C40 C 1.2730(6) 0.8287(4) -0.0585(5) 0.0402(19) Uani 1 1 d . . . H40A H 1.32 0.8421 -0.1023 0.06 Uiso 1 1 calc R . . H40B H 1.1856 0.8381 -0.0835 0.06 Uiso 1 1 calc R . . H40C H 1.284 0.7819 -0.0469 0.06 Uiso 1 1 calc R . . N1 N 1.1041(4) 0.8589(2) 0.2073(3) 0.0172(11) Uani 1 1 d . . . N12 N 0.8764(5) 0.9098(2) 0.1699(3) 0.0202(12) Uani 1 1 d . . . H12 H 0.8006 0.9239 0.162 0.024 Uiso 1 1 calc R . . N13 N 1.0325(5) 0.8791(3) 0.0255(3) 0.0224(12) Uani 1 1 d . . . N23 N 1.1226(5) 0.9868(2) 0.1747(3) 0.0209(12) Uani 1 1 d . . . Ti1 Ti 0.95002(10) 0.83854(5) 0.11365(7) 0.0175(2) Uani 1 1 d . . . Ti2 Ti 1.03329(10) 0.93783(6) 0.25029(7) 0.0171(2) Uani 1 1 d . . . Ti3 Ti 1.17554(10) 0.90697(5) 0.12092(7) 0.0178(2) Uani 1 1 d . . . Hg1 Hg 1.04746(2) 1.058503(12) 0.080349(16) 0.02155(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.019(4) 0.017(3) 0.039(4) -0.011(3) 0.002(3) -0.001(3) C12 0.029(4) 0.013(3) 0.027(4) 0.003(3) -0.005(3) -0.007(3) C13 0.030(4) 0.023(4) 0.024(4) -0.003(3) 0.003(3) -0.019(3) C14 0.015(3) 0.018(3) 0.031(4) -0.008(3) -0.002(3) -0.009(3) C15 0.013(3) 0.017(3) 0.022(3) -0.008(3) -0.008(3) -0.007(3) C16 0.030(4) 0.030(4) 0.060(5) -0.023(4) 0.005(4) 0.008(3) C17 0.049(5) 0.026(4) 0.054(5) 0.014(4) -0.012(4) -0.009(4) C18 0.047(5) 0.043(5) 0.039(5) -0.004(4) 0.017(4) -0.016(4) C19 0.022(4) 0.026(4) 0.056(5) -0.007(4) 0.007(3) -0.005(3) C20 0.031(4) 0.038(4) 0.027(4) -0.009(3) 0.003(3) -0.007(3) C21 0.065(6) 0.026(4) 0.020(4) -0.004(3) 0.017(4) -0.004(4) C22 0.032(4) 0.062(6) 0.021(4) -0.022(4) 0.015(3) -0.005(4) C23 0.044(5) 0.020(4) 0.026(4) -0.007(3) 0.008(3) 0.013(3) C24 0.039(4) 0.030(4) 0.021(4) -0.017(3) 0.010(3) -0.010(3) C25 0.034(4) 0.026(4) 0.017(3) -0.011(3) 0.001(3) 0.007(3) C26 0.145(10) 0.039(5) 0.033(5) -0.005(4) 0.039(6) -0.026(6) C27 0.042(5) 0.116(9) 0.055(6) -0.053(6) 0.032(4) -0.026(5) C28 0.110(8) 0.045(5) 0.039(5) -0.010(4) 0.006(5) 0.038(6) C29 0.074(6) 0.059(6) 0.048(5) -0.022(5) 0.022(5) -0.027(5) C30 0.066(6) 0.078(7) 0.037(5) -0.016(4) -0.009(4) 0.044(5) C31 0.018(3) 0.031(4) 0.032(4) 0.007(3) 0.012(3) 0.003(3) C32 0.014(3) 0.026(4) 0.040(4) 0.001(3) 0.012(3) -0.002(3) C33 0.014(3) 0.031(4) 0.019(3) 0.004(3) 0.005(3) -0.001(3) C34 0.016(3) 0.027(4) 0.031(4) -0.001(3) 0.005(3) 0.001(3) C35 0.019(3) 0.028(4) 0.025(4) 0.001(3) 0.014(3) 0.006(3) C36 0.042(5) 0.050(5) 0.047(5) 0.016(4) 0.017(4) -0.004(4) C37 0.026(4) 0.039(5) 0.059(5) -0.006(4) 0.013(4) -0.009(4) C38 0.025(4) 0.055(5) 0.024(4) 0.014(3) 0.002(3) -0.002(4) C39 0.031(4) 0.029(4) 0.048(5) 0.005(3) 0.014(4) 0.009(3) C40 0.036(4) 0.055(5) 0.030(4) -0.011(4) 0.011(3) 0.014(4) N1 0.016(3) 0.017(3) 0.018(3) 0.004(2) 0.003(2) 0.002(2) N12 0.020(3) 0.018(3) 0.022(3) -0.001(2) 0.005(2) 0.000(2) N13 0.022(3) 0.025(3) 0.018(3) -0.001(2) 0.001(2) 0.006(2) N23 0.019(3) 0.016(3) 0.027(3) 0.003(2) 0.003(2) 0.006(2) Ti1 0.0181(6) 0.0161(6) 0.0176(6) -0.0023(4) 0.0029(5) -0.0011(5) Ti2 0.0195(6) 0.0160(6) 0.0156(5) -0.0030(5) 0.0039(4) 0.0010(5) Ti3 0.0171(6) 0.0182(6) 0.0182(6) 0.0006(5) 0.0047(5) 0.0015(5) Hg1 0.02414(14) 0.02078(13) 0.01968(13) 0.00135(12) 0.00523(9) 0.00139(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C12 1.424(9) . ? C11 C15 1.425(8) . ? C11 C16 1.525(9) . ? C11 Ti1 2.373(6) . ? C12 C13 1.414(9) . ? C12 C17 1.527(9) . ? C12 Ti1 2.381(6) . ? C13 C14 1.415(9) . ? C13 C18 1.508(9) . ? C13 Ti1 2.426(6) . ? C14 C15 1.414(9) . ? C14 C19 1.507(8) . ? C14 Ti1 2.445(6) . ? C15 C20 1.507(8) . ? C15 Ti1 2.417(5) . ? C21 C22 1.406(10) . ? C21 C25 1.422(10) . ? C21 C26 1.516(10) . ? C21 Ti2 2.405(7) . ? C22 C23 1.398(10) . ? C22 C27 1.527(10) . ? C22 Ti2 2.432(7) . ? C23 C24 1.411(9) . ? C23 C28 1.491(10) . ? C23 Ti2 2.427(6) . ? C24 C25 1.395(9) . ? C24 C29 1.526(10) . ? C24 Ti2 2.420(6) . ? C25 C30 1.517(9) . ? C25 Ti2 2.387(6) . ? C31 C35 1.394(9) . ? C31 C32 1.416(9) . ? C31 C36 1.519(9) . ? C31 Ti3 2.429(6) . ? C32 C33 1.432(9) . ? C32 C37 1.519(9) . ? C32 Ti3 2.437(6) . ? C33 C34 1.410(9) . ? C33 C38 1.512(8) . ? C33 Ti3 2.421(6) . ? C34 C35 1.404(8) . ? C34 C39 1.523(9) . ? C34 Ti3 2.414(6) . ? C35 C40 1.532(9) . ? C35 Ti3 2.428(6) . ? N1 Ti3 1.918(5) . ? N1 Ti2 1.943(5) . ? N1 Ti1 1.955(5) . ? N12 Ti2 1.926(5) . ? N12 Ti1 1.933(5) . ? N13 Ti3 1.925(5) . ? N13 Ti1 1.941(5) . ? N13 Hg1 2.038(5) 3_775 ? N23 Ti2 1.930(5) . ? N23 Ti3 1.945(5) . ? N23 Hg1 2.041(5) . ? Ti1 Ti3 2.8124(16) . ? Ti1 Ti2 2.8367(15) . ? Ti2 Ti3 2.8214(16) . ? Ti3 Hg1 3.3530(12) . ? Ti3 Hg1 3.4429(13) 3_775 ? Hg1 N13 2.038(5) 3_775 ? Hg1 Hg1 3.3347(6) 3_775 ? Hg1 Ti3 3.4429(13) 3_775 ? 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 C12 C11 C15 107.5(6) . . ? C12 C11 C16 126.0(6) . . ? C15 C11 C16 126.5(6) . . ? C12 C11 Ti1 72.8(3) . . ? C15 C11 Ti1 74.4(3) . . ? C16 C11 Ti1 120.8(4) . . ? C13 C12 C11 108.4(5) . . ? C13 C12 C17 125.7(7) . . ? C11 C12 C17 125.8(6) . . ? C13 C12 Ti1 74.7(4) . . ? C11 C12 Ti1 72.3(3) . . ? C17 C12 Ti1 121.5(4) . . ? C12 C13 C14 107.7(6) . . ? C12 C13 C18 126.6(6) . . ? C14 C13 C18 125.6(7) . . ? C12 C13 Ti1 71.1(4) . . ? C14 C13 Ti1 73.9(4) . . ? C18 C13 Ti1 123.5(4) . . ? C15 C14 C13 108.7(6) . . ? C15 C14 C19 126.3(6) . . ? C13 C14 C19 125.0(6) . . ? C15 C14 Ti1 72.0(3) . . ? C13 C14 Ti1 72.4(3) . . ? C19 C14 Ti1 123.5(4) . . ? C14 C15 C11 107.7(6) . . ? C14 C15 C20 126.7(6) . . ? C11 C15 C20 125.6(6) . . ? C14 C15 Ti1 74.2(3) . . ? C11 C15 Ti1 71.0(3) . . ? C20 C15 Ti1 121.9(4) . . ? C22 C21 C25 107.1(6) . . ? C22 C21 C26 126.9(8) . . ? C25 C21 C26 126.0(7) . . ? C22 C21 Ti2 74.1(4) . . ? C25 C21 Ti2 72.0(4) . . ? C26 C21 Ti2 120.9(5) . . ? C23 C22 C21 108.8(6) . . ? C23 C22 C27 125.7(8) . . ? C21 C22 C27 125.4(8) . . ? C23 C22 Ti2 73.1(4) . . ? C21 C22 Ti2 72.1(4) . . ? C27 C22 Ti2 123.5(5) . . ? C22 C23 C24 107.6(6) . . ? C22 C23 C28 125.5(8) . . ? C24 C23 C28 126.8(7) . . ? C22 C23 Ti2 73.5(4) . . ? C24 C23 Ti2 72.8(4) . . ? C28 C23 Ti2 121.4(5) . . ? C25 C24 C23 108.4(6) . . ? C25 C24 C29 125.5(7) . . ? C23 C24 C29 126.1(7) . . ? C25 C24 Ti2 71.8(3) . . ? C23 C24 Ti2 73.4(4) . . ? C29 C24 Ti2 120.7(5) . . ? C24 C25 C21 108.0(6) . . ? C24 C25 C30 127.5(7) . . ? C21 C25 C30 124.3(7) . . ? C24 C25 Ti2 74.4(4) . . ? C21 C25 Ti2 73.4(4) . . ? C30 C25 Ti2 122.0(5) . . ? C35 C31 C32 108.0(6) . . ? C35 C31 C36 126.9(6) . . ? C32 C31 C36 125.1(7) . . ? C35 C31 Ti3 73.3(4) . . ? C32 C31 Ti3 73.4(4) . . ? C36 C31 Ti3 120.9(4) . . ? C31 C32 C33 107.5(6) . . ? C31 C32 C37 126.6(6) . . ? C33 C32 C37 125.9(6) . . ? C31 C32 Ti3 72.8(4) . . ? C33 C32 Ti3 72.2(3) . . ? C37 C32 Ti3 120.7(4) . . ? C34 C33 C32 107.3(5) . . ? C34 C33 C38 126.5(6) . . ? C32 C33 C38 126.2(6) . . ? C34 C33 Ti3 72.8(3) . . ? C32 C33 Ti3 73.5(3) . . ? C38 C33 Ti3 120.5(4) . . ? C35 C34 C33 108.1(6) . . ? C35 C34 C39 127.7(6) . . ? C33 C34 C39 124.1(6) . . ? C35 C34 Ti3 73.7(4) . . ? C33 C34 Ti3 73.3(4) . . ? C39 C34 Ti3 121.6(4) . . ? C31 C35 C34 109.0(6) . . ? C31 C35 C40 125.8(6) . . ? C34 C35 C40 125.1(6) . . ? C31 C35 Ti3 73.4(4) . . ? C34 C35 Ti3 72.6(4) . . ? C40 C35 Ti3 121.3(4) . . ? Ti3 N1 Ti2 93.9(2) . . ? Ti3 N1 Ti1 93.1(2) . . ? Ti2 N1 Ti1 93.4(2) . . ? Ti2 N12 Ti1 94.6(2) . . ? Ti3 N13 Ti1 93.3(2) . . ? Ti3 N13 Hg1 120.6(3) . 3_775 ? Ti1 N13 Hg1 126.5(3) . 3_775 ? Ti2 N23 Ti3 93.5(2) . . ? Ti2 N23 Hg1 125.6(3) . . ? Ti3 N23 Hg1 114.5(2) . . ? N12 Ti1 N13 106.9(2) . . ? N12 Ti1 N1 85.2(2) . . ? N13 Ti1 N1 85.7(2) . . ? N12 Ti1 C11 146.8(2) . . ? N13 Ti1 C11 99.4(2) . . ? N1 Ti1 C11 117.1(2) . . ? N12 Ti1 C12 119.2(2) . . ? N13 Ti1 C12 133.1(2) . . ? N1 Ti1 C12 104.9(2) . . ? C11 Ti1 C12 34.9(2) . . ? N12 Ti1 C15 123.4(2) . . ? N13 Ti1 C15 91.5(2) . . ? N1 Ti1 C15 150.5(2) . . ? C11 Ti1 C15 34.6(2) . . ? C12 Ti1 C15 57.2(2) . . ? N12 Ti1 C13 90.2(2) . . ? N13 Ti1 C13 148.0(2) . . ? N1 Ti1 C13 123.3(2) . . ? C11 Ti1 C13 57.3(2) . . ? C12 Ti1 C13 34.2(2) . . ? C15 Ti1 C13 56.7(2) . . ? N12 Ti1 C14 92.8(2) . . ? N13 Ti1 C14 116.5(2) . . ? N1 Ti1 C14 157.0(2) . . ? C11 Ti1 C14 56.8(2) . . ? C12 Ti1 C14 56.5(2) . . ? C15 Ti1 C14 33.8(2) . . ? C13 Ti1 C14 33.8(2) . . ? N12 Ti1 Ti3 94.35(15) . . ? N13 Ti1 Ti3 43.11(15) . . ? N1 Ti1 Ti3 42.92(14) . . ? C11 Ti1 Ti3 118.84(16) . . ? C12 Ti1 Ti3 133.47(17) . . ? C15 Ti1 Ti3 130.17(16) . . ? C13 Ti1 Ti3 164.70(16) . . ? C14 Ti1 Ti3 159.66(16) . . ? N12 Ti1 Ti2 42.60(15) . . ? N13 Ti1 Ti2 93.60(15) . . ? N1 Ti1 Ti2 43.15(14) . . ? C11 Ti1 Ti2 155.53(17) . . ? C12 Ti1 Ti2 125.52(16) . . ? C15 Ti1 Ti2 165.96(16) . . ? C13 Ti1 Ti2 116.54(16) . . ? C14 Ti1 Ti2 133.45(16) . . ? Ti3 Ti1 Ti2 59.93(4) . . ? N12 Ti2 N23 107.1(2) . . ? N12 Ti2 N1 85.7(2) . . ? N23 Ti2 N1 85.8(2) . . ? N12 Ti2 C25 138.8(2) . . ? N23 Ti2 C25 112.4(2) . . ? N1 Ti2 C25 108.0(2) . . ? N12 Ti2 C21 104.4(2) . . ? N23 Ti2 C21 145.8(2) . . ? N1 Ti2 C21 109.6(2) . . ? C25 Ti2 C21 34.5(2) . . ? N12 Ti2 C24 138.1(2) . . ? N23 Ti2 C24 90.7(2) . . ? N1 Ti2 C24 134.2(2) . . ? C25 Ti2 C24 33.7(2) . . ? C21 Ti2 C24 56.4(2) . . ? N12 Ti2 C23 104.3(2) . . ? N23 Ti2 C23 102.5(2) . . ? N1 Ti2 C23 164.1(2) . . ? C25 Ti2 C23 56.4(2) . . ? C21 Ti2 C23 56.3(2) . . ? C24 Ti2 C23 33.8(2) . . ? N12 Ti2 C22 87.2(2) . . ? N23 Ti2 C22 135.6(3) . . ? N1 Ti2 C22 138.0(2) . . ? C25 Ti2 C22 56.3(2) . . ? C21 Ti2 C22 33.8(3) . . ? C24 Ti2 C22 55.7(2) . . ? C23 Ti2 C22 33.4(2) . . ? N12 Ti2 Ti3 94.21(16) . . ? N23 Ti2 Ti3 43.48(15) . . ? N1 Ti2 Ti3 42.71(14) . . ? C25 Ti2 Ti3 122.51(17) . . ? C21 Ti2 Ti3 145.82(19) . . ? C24 Ti2 Ti3 122.85(17) . . ? C23 Ti2 Ti3 145.45(19) . . ? C22 Ti2 Ti3 178.55(18) . . ? N12 Ti2 Ti1 42.77(15) . . ? N23 Ti2 Ti1 93.78(16) . . ? N1 Ti2 Ti1 43.46(14) . . ? C25 Ti2 Ti1 141.08(16) . . ? C21 Ti2 Ti1 118.68(18) . . ? C24 Ti2 Ti1 174.65(17) . . ? C23 Ti2 Ti1 146.84(18) . . ? C22 Ti2 Ti1 121.82(18) . . ? Ti3 Ti2 Ti1 59.61(4) . . ? N1 Ti3 N13 87.2(2) . . ? N1 Ti3 N23 86.1(2) . . ? N13 Ti3 N23 105.7(2) . . ? N1 Ti3 C34 100.1(2) . . ? N13 Ti3 C34 110.8(2) . . ? N23 Ti3 C34 143.2(2) . . ? N1 Ti3 C33 101.0(2) . . ? N13 Ti3 C33 144.4(2) . . ? N23 Ti3 C33 109.3(2) . . ? C34 Ti3 C33 33.9(2) . . ? N1 Ti3 C35 128.3(2) . . ? N13 Ti3 C35 91.7(2) . . ? N23 Ti3 C35 142.7(2) . . ? C34 Ti3 C35 33.7(2) . . ? C33 Ti3 C35 56.0(2) . . ? N1 Ti3 C31 155.6(2) . . ? N13 Ti3 C31 105.7(2) . . ? N23 Ti3 C31 109.4(2) . . ? C34 Ti3 C31 56.1(2) . . ? C33 Ti3 C31 56.5(2) . . ? C35 Ti3 C31 33.4(2) . . ? N1 Ti3 C32 130.8(2) . . ? N13 Ti3 C32 139.5(2) . . ? N23 Ti3 C32 92.2(2) . . ? C34 Ti3 C32 56.3(2) . . ? C33 Ti3 C32 34.3(2) . . ? C35 Ti3 C32 55.7(2) . . ? C31 Ti3 C32 33.8(2) . . ? N1 Ti3 Ti1 43.94(14) . . ? N13 Ti3 Ti1 43.56(16) . . ? N23 Ti3 Ti1 94.19(15) . . ? C34 Ti3 Ti1 115.50(16) . . ? C33 Ti3 Ti1 137.15(16) . . ? C35 Ti3 Ti1 120.04(16) . . ? C31 Ti3 Ti1 146.79(17) . . ? C32 Ti3 Ti1 171.19(16) . . ? N1 Ti3 Ti2 43.41(15) . . ? N13 Ti3 Ti2 94.43(16) . . ? N23 Ti3 Ti2 43.05(15) . . ? C34 Ti3 Ti2 135.51(16) . . ? C33 Ti3 Ti2 115.40(15) . . ? C35 Ti3 Ti2 169.21(16) . . ? C31 Ti3 Ti2 150.48(17) . . ? C32 Ti3 Ti2 122.00(16) . . ? Ti1 Ti3 Ti2 60.46(4) . . ? N1 Ti3 Hg1 110.94(15) . . ? N13 Ti3 Hg1 84.36(15) . . ? N23 Ti3 Hg1 33.65(15) . . ? C34 Ti3 Hg1 146.23(16) . . ? C33 Ti3 Hg1 123.03(16) . . ? C35 Ti3 Hg1 120.39(15) . . ? C31 Ti3 Hg1 91.23(16) . . ? C32 Ti3 Hg1 92.25(15) . . ? Ti1 Ti3 Hg1 96.44(4) . . ? Ti2 Ti3 Hg1 69.18(3) . . ? N1 Ti3 Hg1 111.18(14) . 3_775 ? N13 Ti3 Hg1 30.62(15) . 3_775 ? N23 Ti3 Hg1 88.21(14) . 3_775 ? C34 Ti3 Hg1 121.81(15) . 3_775 ? C33 Ti3 Hg1 144.38(15) . 3_775 ? C35 Ti3 Hg1 91.08(15) . 3_775 ? C31 Ti3 Hg1 88.75(15) . 3_775 ? C32 Ti3 Hg1 117.93(16) . 3_775 ? Ti1 Ti3 Hg1 68.36(3) . 3_775 ? Ti2 Ti3 Hg1 98.70(4) . 3_775 ? Hg1 Ti3 Hg1 58.754(19) . 3_775 ? N13 Hg1 N23 173.0(2) 3_775 . ? N13 Hg1 Hg1 83.28(14) 3_775 3_775 ? N23 Hg1 Hg1 89.71(14) . 3_775 ? N13 Hg1 Ti3 141.60(14) 3_775 . ? N23 Hg1 Ti3 31.86(14) . . ? Hg1 Hg1 Ti3 61.97(2) 3_775 . ? N13 Hg1 Ti3 28.77(14) 3_775 3_775 ? N23 Hg1 Ti3 145.30(14) . 3_775 ? Hg1 Hg1 Ti3 59.28(2) 3_775 3_775 ? Ti3 Hg1 Ti3 121.246(19) . 3_775 ? #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 699912' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H94 Ag2 N8 Ti6, (C7 H8)' _chemical_formula_sum 'C67 H102 Ag2 N8 Ti6' _chemical_formula_weight 1522.71 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.923(3) _cell_length_b 15.546(3) _cell_length_c 16.496(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3827.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 92 _cell_measurement_theta_max 20.333 _cell_measurement_theta_min 3.153 _diffrn_ambient_temperature 200 _diffrn_radiation_probe x-ray _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.765 _exptl_special_details ; ? ; _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 83765 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.59 _reflns_number_total 4541 _reflns_number_gt 3401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication (Farrugia, 1999)' _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^)+(0.0738P)^2^+3.0160P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0086(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4541 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.023 0.000 0.000 413.3 -0.7 2 -0.027 0.500 0.500 413.2 -1.1 _platon_squeeze_details ;A molecule of toluene crystallize with every molecule of this compound but presented severe disorder and it was not possible to get a chemical sensible model for it, so Squeeze procedure was used to remove their contribution to the structure factors. ; 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 Ag1 Ag 0.02943(3) 0.91473(3) 0.53027(3) 0.04505(18) Uani 0.50 1 d P . . Ti1 Ti 0.22974(5) 0.91907(4) 0.5000 0.0306(2) Uani 1 2 d S . . Ti2 Ti 0.17757(4) 1.07155(3) 0.41572(3) 0.03069(17) Uani 1 1 d . . . N1 N 0.1043(2) 1.1114(2) 0.5000 0.0345(8) Uani 1 2 d S . . N2 N 0.2631(2) 1.0400(2) 0.5000 0.0302(7) Uani 1 2 d S . . N3 N 0.15503(18) 0.94527(16) 0.59389(14) 0.0338(5) Uani 1 1 d . . . H3 H 0.144(3) 0.909(3) 0.643(3) 0.072(13) Uiso 1 1 d . . . C1 C 0.3658(3) 0.8420(3) 0.5000 0.0488(12) Uani 1 2 d S . . C2 C 0.3192(3) 0.8144(2) 0.5687(2) 0.0494(9) Uani 1 1 d . . . C3 C 0.2412(3) 0.7685(2) 0.5433(2) 0.0562(10) Uani 1 1 d . . . C5 C 0.1256(2) 1.1322(2) 0.28781(17) 0.0398(7) Uani 1 1 d . . . C6 C 0.1578(3) 1.2017(2) 0.33626(19) 0.0436(8) Uani 1 1 d . . . C7 C 0.2519(2) 1.1886(2) 0.34658(19) 0.0461(8) Uani 1 1 d . . . C8 C 0.2768(2) 1.1120(2) 0.30434(18) 0.0424(7) Uani 1 1 d . . . C9 C 0.1989(2) 1.0772(2) 0.26863(17) 0.0405(7) Uani 1 1 d . . . C11 C 0.4544(4) 0.8911(5) 0.5000 0.079(2) Uani 1 2 d S . . H11A H 0.4727 0.9017 0.5549 0.119 Uiso 0.50 1 calc PR . . H11B H 0.4468 0.9449 0.4722 0.119 Uiso 0.50 1 calc PR . . H11C H 0.4993 0.8575 0.4729 0.119 Uiso 0.50 1 calc PR . . C12 C 0.3490(4) 0.8257(3) 0.6565(3) 0.0928(19) Uani 1 1 d . . . H12A H 0.3856 0.8762 0.6610 0.139 Uiso 1 1 calc R . . H12B H 0.3828 0.7762 0.6732 0.139 Uiso 1 1 calc R . . H12C H 0.2972 0.8317 0.6906 0.139 Uiso 1 1 calc R . . C13 C 0.1768(4) 0.7249(3) 0.5993(4) 0.106(2) Uani 1 1 d . . . H13A H 0.2009 0.6704 0.6157 0.159 Uiso 1 1 calc R . . H13B H 0.1208 0.7162 0.5719 0.159 Uiso 1 1 calc R . . H13C H 0.1674 0.7603 0.6463 0.159 Uiso 1 1 calc R . . C15 C 0.0311(3) 1.1229(3) 0.2589(3) 0.0591(10) Uani 1 1 d . . . H15A H 0.0230 1.0667 0.2359 0.089 Uiso 1 1 calc . . . H15B H 0.0189 1.1658 0.2186 0.089 Uiso 1 1 calc . . . H15C H -0.0091 1.1301 0.3038 0.089 Uiso 1 1 calc . . . C16 C 0.1039(3) 1.2767(2) 0.3684(3) 0.0663(12) Uani 1 1 d . . . H16A H 0.1304 1.3296 0.3504 0.100 Uiso 1 1 calc . . . H16B H 0.1037 1.2751 0.4266 0.100 Uiso 1 1 calc . . . H16C H 0.0435 1.2729 0.3487 0.100 Uiso 1 1 calc . . . C17 C 0.3167(3) 1.2502(3) 0.3884(3) 0.0726(13) Uani 1 1 d . . . H17A H 0.3401 1.2901 0.3495 0.109 Uiso 1 1 calc R . . H17B H 0.3652 1.2181 0.4119 0.109 Uiso 1 1 calc R . . H17C H 0.2857 1.2810 0.4303 0.109 Uiso 1 1 calc R . . C18 C 0.3719(3) 1.0779(3) 0.2978(3) 0.0679(12) Uani 1 1 d . . . H18A H 0.3706 1.0197 0.2786 0.102 Uiso 1 1 calc R . . H18B H 0.4000 1.0798 0.3501 0.102 Uiso 1 1 calc R . . H18C H 0.4053 1.1129 0.2605 0.102 Uiso 1 1 calc R . . C19 C 0.1952(3) 0.9989(3) 0.2134(2) 0.0568(10) Uani 1 1 d . . . H19A H 0.2476 0.9977 0.1796 0.085 Uiso 1 1 calc . . . H19B H 0.1427 1.0020 0.1800 0.085 Uiso 1 1 calc . . . H19C H 0.1931 0.9476 0.2457 0.085 Uiso 1 1 calc . . . 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 Ag1 0.0474(3) 0.0295(3) 0.0582(3) -0.00056(18) -0.0132(2) -0.00020(19) Ti1 0.0447(4) 0.0228(4) 0.0244(3) 0.000 0.000 0.0013(3) Ti2 0.0450(3) 0.0251(3) 0.0220(3) 0.0026(2) -0.0005(2) -0.0009(2) N1 0.0415(19) 0.0315(17) 0.0305(17) 0.000 0.000 0.0023(15) N2 0.0379(18) 0.0257(16) 0.0271(16) 0.000 0.000 -0.0016(14) N3 0.0458(14) 0.0303(12) 0.0252(12) 0.0029(10) 0.0003(10) -0.0020(11) C1 0.055(3) 0.032(2) 0.059(3) 0.000 0.000 0.014(2) C2 0.075(3) 0.0331(16) 0.0403(18) 0.0004(13) -0.0043(17) 0.0190(17) C3 0.074(2) 0.0274(16) 0.067(2) 0.0152(16) 0.022(2) 0.0133(16) C5 0.0522(18) 0.0403(17) 0.0267(14) 0.0132(13) -0.0033(13) -0.0028(14) C6 0.068(2) 0.0284(15) 0.0344(16) 0.0113(12) 0.0013(15) -0.0001(14) C7 0.066(2) 0.0403(18) 0.0323(15) 0.0101(14) -0.0037(15) -0.0147(16) C8 0.0516(19) 0.0480(18) 0.0275(14) 0.0097(13) 0.0040(14) -0.0020(15) C9 0.059(2) 0.0411(17) 0.0213(13) 0.0077(12) 0.0026(13) -0.0035(14) C11 0.045(3) 0.066(4) 0.127(6) 0.000 0.000 0.009(3) C12 0.147(5) 0.085(3) 0.046(2) -0.003(2) -0.027(3) 0.060(3) C13 0.113(4) 0.047(2) 0.158(6) 0.043(3) 0.067(4) 0.014(3) C15 0.058(2) 0.063(2) 0.055(2) 0.019(2) -0.0103(18) -0.0057(19) C16 0.103(3) 0.0389(19) 0.057(2) 0.0103(17) 0.007(2) 0.015(2) C17 0.091(3) 0.069(3) 0.057(2) 0.013(2) -0.018(2) -0.038(2) C18 0.056(2) 0.095(3) 0.054(2) 0.012(2) 0.0095(19) 0.001(2) C19 0.088(3) 0.054(2) 0.0286(15) -0.0038(15) 0.0064(17) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 Ag1 0.9985(11) 6_556 ? Ag1 N1 2.096(4) 5_576 ? Ag1 N3 2.200(3) . ? Ag1 Ag1 2.7929(11) 2_575 ? Ag1 Ag1 2.9660(10) 5_576 ? Ag1 Ti1 3.0315(11) . ? Ag1 Ti2 3.2222(9) 5_576 ? Ti1 N2 1.945(3) . ? Ti1 N3 1.951(3) . ? Ti1 N3 1.951(3) 6_556 ? Ti1 C1 2.358(5) . ? Ti1 C2 2.390(3) 6_556 ? Ti1 C2 2.390(3) . ? Ti1 C3 2.453(3) 6_556 ? Ti1 C3 2.453(3) . ? Ti1 Ti2 2.8562(9) 6_556 ? Ti1 Ti2 2.8562(9) . ? Ti1 Ag1 3.0315(11) 6_556 ? Ti2 N1 1.874(2) . ? Ti2 N2 1.950(2) . ? Ti2 N3 1.998(3) 6_556 ? Ti2 C7 2.417(3) . ? Ti2 C6 2.429(3) . ? Ti2 C5 2.438(3) . ? Ti2 C8 2.443(3) . ? Ti2 C9 2.449(3) . ? Ti2 Ti2 2.7804(11) 6_556 ? Ti2 Ag1 3.2222(9) 5_576 ? N1 Ti2 1.874(2) 6_556 ? N1 Ag1 2.096(4) 5_576 ? N1 Ag1 2.096(4) 2_575 ? N2 Ti2 1.950(2) 6_556 ? N3 Ti2 1.998(3) 6_556 ? N3 H3 1.00(5) . ? C1 C2 1.398(5) 6_556 ? C1 C2 1.398(5) . ? C1 C11 1.527(8) . ? C2 C3 1.428(6) . ? C2 C12 1.524(5) . ? C3 C3 1.428(8) 6_556 ? C3 C13 1.496(6) . ? C5 C9 1.424(5) . ? C5 C6 1.428(5) . ? C5 C15 1.495(5) . ? C6 C7 1.431(5) . ? C6 C16 1.511(5) . ? C7 C8 1.428(5) . ? C7 C17 1.526(5) . ? C8 C9 1.411(5) . ? C8 C18 1.519(5) . ? C9 C19 1.522(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? 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 Ag1 Ag1 N1 76.22(3) 6_556 5_576 ? Ag1 Ag1 N3 118.49(7) 6_556 . ? N1 Ag1 N3 165.07(8) 5_576 . ? Ag1 Ag1 Ag1 90.0 6_556 2_575 ? N1 Ag1 Ag1 83.37(10) 5_576 2_575 ? N3 Ag1 Ag1 93.62(7) . 2_575 ? Ag1 Ag1 Ag1 70.33(2) 6_556 5_576 ? N1 Ag1 Ag1 79.11(10) 5_576 5_576 ? N3 Ag1 Ag1 102.71(7) . 5_576 ? Ag1 Ag1 Ag1 19.67(2) 2_575 5_576 ? Ag1 Ag1 Ti1 80.521(10) 6_556 . ? N1 Ag1 Ti1 154.63(5) 5_576 . ? N3 Ag1 Ti1 39.97(7) . . ? Ag1 Ag1 Ti1 106.80(3) 2_575 . ? Ag1 Ag1 Ti1 102.52(3) 5_576 . ? Ag1 Ag1 Ti2 106.051(13) 6_556 5_576 ? N1 Ag1 Ti2 33.51(5) 5_576 5_576 ? N3 Ag1 Ti2 132.12(7) . 5_576 ? Ag1 Ag1 Ti2 68.63(2) 2_575 5_576 ? Ag1 Ag1 Ti2 75.52(2) 5_576 5_576 ? Ti1 Ag1 Ti2 171.68(2) . 5_576 ? N2 Ti1 N3 86.82(10) . . ? N2 Ti1 N3 86.82(10) . 6_556 ? N3 Ti1 N3 105.07(15) . 6_556 ? N2 Ti1 C1 105.71(17) . . ? N3 Ti1 C1 126.74(8) . . ? N3 Ti1 C1 126.74(8) 6_556 . ? N2 Ti1 C2 120.99(13) . 6_556 ? N3 Ti1 C2 146.89(11) . 6_556 ? N3 Ti1 C2 94.85(12) 6_556 6_556 ? C1 Ti1 C2 34.24(11) . 6_556 ? N2 Ti1 C2 120.99(13) . . ? N3 Ti1 C2 94.85(12) . . ? N3 Ti1 C2 146.89(11) 6_556 . ? C1 Ti1 C2 34.24(11) . . ? C2 Ti1 C2 56.65(17) 6_556 . ? N2 Ti1 C3 154.75(13) . 6_556 ? N3 Ti1 C3 118.04(13) . 6_556 ? N3 Ti1 C3 90.46(11) 6_556 6_556 ? C1 Ti1 C3 56.96(15) . 6_556 ? C2 Ti1 C3 34.26(13) 6_556 6_556 ? C2 Ti1 C3 56.61(12) . 6_556 ? N2 Ti1 C3 154.75(13) . . ? N3 Ti1 C3 90.46(11) . . ? N3 Ti1 C3 118.04(13) 6_556 . ? C1 Ti1 C3 56.96(15) . . ? C2 Ti1 C3 56.61(12) 6_556 . ? C2 Ti1 C3 34.26(13) . . ? C3 Ti1 C3 33.84(19) 6_556 . ? N2 Ti1 Ti2 42.91(7) . 6_556 ? N3 Ti1 Ti2 44.33(7) . 6_556 ? N3 Ti1 Ti2 93.29(8) 6_556 6_556 ? C1 Ti1 Ti2 131.04(10) . 6_556 ? C2 Ti1 Ti2 161.44(11) 6_556 6_556 ? C2 Ti1 Ti2 119.09(8) . 6_556 ? C3 Ti1 Ti2 162.29(11) 6_556 6_556 ? C3 Ti1 Ti2 132.01(9) . 6_556 ? N2 Ti1 Ti2 42.91(7) . . ? N3 Ti1 Ti2 93.29(8) . . ? N3 Ti1 Ti2 44.33(7) 6_556 . ? C1 Ti1 Ti2 131.04(10) . . ? C2 Ti1 Ti2 119.09(8) 6_556 . ? C2 Ti1 Ti2 161.44(11) . . ? C3 Ti1 Ti2 132.01(9) 6_556 . ? C3 Ti1 Ti2 162.29(11) . . ? Ti2 Ti1 Ti2 58.25(3) 6_556 . ? N2 Ti1 Ag1 105.90(10) . . ? N3 Ti1 Ag1 46.41(8) . . ? N3 Ti1 Ag1 64.65(8) 6_556 . ? C1 Ti1 Ag1 146.92(12) . . ? C2 Ti1 Ag1 127.84(10) 6_556 . ? C2 Ti1 Ag1 117.21(10) . . ? C3 Ti1 Ag1 95.49(10) 6_556 . ? C3 Ti1 Ag1 89.99(10) . . ? Ti2 Ti1 Ag1 70.70(2) 6_556 . ? Ti2 Ti1 Ag1 80.20(2) . . ? N2 Ti1 Ag1 105.90(10) . 6_556 ? N3 Ti1 Ag1 64.65(8) . 6_556 ? N3 Ti1 Ag1 46.41(8) 6_556 6_556 ? C1 Ti1 Ag1 146.92(12) . 6_556 ? C2 Ti1 Ag1 117.21(10) 6_556 6_556 ? C2 Ti1 Ag1 127.84(10) . 6_556 ? C3 Ti1 Ag1 89.99(10) 6_556 6_556 ? C3 Ti1 Ag1 95.49(10) . 6_556 ? Ti2 Ti1 Ag1 80.20(2) 6_556 6_556 ? Ti2 Ti1 Ag1 70.70(2) . 6_556 ? Ag1 Ti1 Ag1 18.96(2) . 6_556 ? N1 Ti2 N2 86.36(11) . . ? N1 Ti2 N3 106.58(13) . 6_556 ? N2 Ti2 N3 85.40(12) . 6_556 ? N1 Ti2 C7 111.67(14) . . ? N2 Ti2 C7 103.00(12) . . ? N3 Ti2 C7 141.20(11) 6_556 . ? N1 Ti2 C6 93.08(13) . . ? N2 Ti2 C6 132.35(13) . . ? N3 Ti2 C6 139.05(11) 6_556 . ? C7 Ti2 C6 34.33(12) . . ? N1 Ti2 C5 109.17(12) . . ? N2 Ti2 C5 157.31(12) . . ? N3 Ti2 C5 104.94(11) 6_556 . ? C7 Ti2 C5 56.40(11) . . ? C6 Ti2 C5 34.11(11) . . ? N1 Ti2 C8 145.76(14) . . ? N2 Ti2 C8 101.77(12) . . ? N3 Ti2 C8 107.20(11) 6_556 . ? C7 Ti2 C8 34.17(12) . . ? C6 Ti2 C8 56.86(12) . . ? C5 Ti2 C8 56.10(11) . . ? N1 Ti2 C9 143.03(12) . . ? N2 Ti2 C9 129.07(12) . . ? N3 Ti2 C9 88.78(10) 6_556 . ? C7 Ti2 C9 56.33(11) . . ? C6 Ti2 C9 56.72(11) . . ? C5 Ti2 C9 33.89(11) . . ? C8 Ti2 C9 33.54(11) . . ? N1 Ti2 Ti2 42.12(8) . 6_556 ? N2 Ti2 Ti2 44.53(7) . 6_556 ? N3 Ti2 Ti2 94.55(7) 6_556 6_556 ? C7 Ti2 Ti2 118.16(8) . 6_556 ? C6 Ti2 Ti2 122.65(8) . 6_556 ? C5 Ti2 Ti2 149.94(8) . 6_556 ? C8 Ti2 Ti2 138.78(8) . 6_556 ? C9 Ti2 Ti2 172.24(8) . 6_556 ? N1 Ti2 Ti1 94.15(9) . . ? N2 Ti2 Ti1 42.78(10) . . ? N3 Ti2 Ti1 43.04(7) 6_556 . ? C7 Ti2 Ti1 136.82(9) . . ? C6 Ti2 Ti1 170.83(9) . . ? C5 Ti2 Ti1 146.00(8) . . ? C8 Ti2 Ti1 114.50(8) . . ? C9 Ti2 Ti1 118.47(8) . . ? Ti2 Ti2 Ti1 60.874(14) 6_556 . ? N1 Ti2 Ag1 38.14(10) . 5_576 ? N2 Ti2 Ag1 116.56(8) . 5_576 ? N3 Ti2 Ag1 85.73(8) 6_556 5_576 ? C7 Ti2 Ag1 121.39(9) . 5_576 ? C6 Ti2 Ag1 88.70(9) . 5_576 ? C5 Ti2 Ag1 84.75(8) . 5_576 ? C8 Ti2 Ag1 140.56(8) . 5_576 ? C9 Ti2 Ag1 113.35(9) . 5_576 ? Ti2 Ti2 Ag1 73.949(13) 6_556 5_576 ? Ti1 Ti2 Ag1 100.47(2) . 5_576 ? Ti2 N1 Ti2 95.75(17) 6_556 . ? Ti2 N1 Ag1 131.92(15) 6_556 5_576 ? Ti2 N1 Ag1 108.35(10) . 5_576 ? Ti2 N1 Ag1 108.35(10) 6_556 2_575 ? Ti2 N1 Ag1 131.92(15) . 2_575 ? Ag1 N1 Ag1 27.55(6) 5_576 2_575 ? Ti1 N2 Ti2 94.32(12) . . ? Ti1 N2 Ti2 94.32(12) . 6_556 ? Ti2 N2 Ti2 90.94(15) . 6_556 ? Ti1 N3 Ti2 92.63(11) . 6_556 ? Ti1 N3 Ag1 93.62(10) . . ? Ti2 N3 Ag1 108.52(11) 6_556 . ? Ti1 N3 H3 128(3) . . ? Ti2 N3 H3 130(3) 6_556 . ? Ag1 N3 H3 97(3) . . ? C2 C1 C2 108.4(5) 6_556 . ? C2 C1 C11 125.8(2) 6_556 . ? C2 C1 C11 125.8(2) . . ? C2 C1 Ti1 74.2(2) 6_556 . ? C2 C1 Ti1 74.2(2) . . ? C11 C1 Ti1 119.4(4) . . ? C1 C2 C3 108.7(3) . . ? C1 C2 C12 126.1(4) . . ? C3 C2 C12 125.1(4) . . ? C1 C2 Ti1 71.6(2) . . ? C3 C2 Ti1 75.3(2) . . ? C12 C2 Ti1 122.4(3) . . ? C2 C3 C3 107.1(2) . 6_556 ? C2 C3 C13 124.6(4) . . ? C3 C3 C13 128.2(3) 6_556 . ? C2 C3 Ti1 70.47(18) . . ? C3 C3 Ti1 73.08(10) 6_556 . ? C13 C3 Ti1 124.5(3) . . ? C9 C5 C6 108.7(3) . . ? C9 C5 C15 126.6(3) . . ? C6 C5 C15 124.7(3) . . ? C9 C5 Ti2 73.48(16) . . ? C6 C5 Ti2 72.62(17) . . ? C15 C5 Ti2 122.6(2) . . ? C5 C6 C7 106.8(3) . . ? C5 C6 C16 127.0(4) . . ? C7 C6 C16 126.2(3) . . ? C5 C6 Ti2 73.26(17) . . ? C7 C6 Ti2 72.35(18) . . ? C16 C6 Ti2 121.2(2) . . ? C8 C7 C6 108.5(3) . . ? C8 C7 C17 125.4(4) . . ? C6 C7 C17 125.9(4) . . ? C8 C7 Ti2 73.90(18) . . ? C6 C7 Ti2 73.31(18) . . ? C17 C7 Ti2 123.3(2) . . ? C9 C8 C7 108.0(3) . . ? C9 C8 C18 127.3(3) . . ? C7 C8 C18 124.7(3) . . ? C9 C8 Ti2 73.47(17) . . ? C7 C8 Ti2 71.93(18) . . ? C18 C8 Ti2 122.0(2) . . ? C5 C9 C8 108.1(3) . . ? C5 C9 C19 125.8(3) . . ? C8 C9 C19 125.9(3) . . ? C5 C9 Ti2 72.63(16) . . ? C8 C9 Ti2 72.99(17) . . ? C19 C9 Ti2 124.0(2) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C15 H15A 109.5 . . ? C5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C6 C16 H16A 109.5 . . ? C6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C7 C17 H17A 109.5 . . ? C7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C8 C18 H18A 109.5 . . ? C8 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C8 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C9 C19 H19A 109.5 . . ? C9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.600 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.085