Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Jason Love' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email JASON.LOVE@NOTTINGHAM.AC.UK _publ_section_title ; Early-late, mixed-metal compounds supported by amidophosphine ligands ; _publ_requested_category FM loop_ _publ_author_name 'Jason Love' 'Alexander J. Blake' 'Paul A. Duckmanton' 'Peter B. Hitchcock' 'Q. Folashade Mokuolu' ; L.Shukla ; 'Claire Wilson' data_jan601 _database_code_depnum_ccdc_archive 'CCDC 216487' _audit_creation_date 2001-01-25T09:55:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (Ph2P(O)C6H4NHCH(tBu)2) _chemical_formula_moiety 'C27 H34 N O P' _chemical_formula_structural 'C27 H34 N O P' _chemical_formula_sum 'C27 H34 N O P' _chemical_formula_weight 419.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5913(5) _cell_length_b 11.8796(8) _cell_length_c 13.3003(9) _cell_angle_alpha 114.750(3) _cell_angle_beta 102.930(4) _cell_angle_gamma 92.017(4) _cell_volume 1188.69(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4587 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 23.534 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.134 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 7517 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_unetI/netI 0.057 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 23.56 _diffrn_reflns_theta_full 23.56 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 3507 _reflns_number_gt 2826 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.6081P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3507 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.214 _refine_diff_density_min -0.35 _refine_diff_density_rms 0.04 #----------------------------------------------------------------------------# # 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P P 0.24616(6) 0.73369(5) 0.03392(5) 0.02140(17) Uani 1 1 d . . . O O 0.18095(16) 0.68137(13) 0.10297(12) 0.0240(3) Uani 1 1 d . . . N N -0.1833(2) 0.39053(17) -0.29884(16) 0.0337(5) Uani 1 1 d . . . H1 H -0.189(3) 0.364(2) -0.247(2) 0.039(7) Uiso 1 1 d . . . C1 C 0.1412(2) 0.65461(18) -0.11648(17) 0.0217(5) Uani 1 1 d . . . C2 C 0.0227(2) 0.55374(19) -0.15215(18) 0.0229(5) Uani 1 1 d . . . H2 H 0.0018 0.5272 -0.0977 0.028 Uiso 1 1 calc R . . C3 C -0.0674(3) 0.48966(19) -0.26802(18) 0.0268(5) Uani 1 1 d . . . C4 C -0.0333(3) 0.5338(2) -0.3447(2) 0.0350(6) Uani 1 1 d . . . H4 H -0.0936 0.4946 -0.4229 0.042 Uiso 1 1 calc R . . C5 C 0.0869(3) 0.6335(2) -0.3080(2) 0.0351(6) Uani 1 1 d . . . H5 H 0.1087 0.6605 -0.362 0.042 Uiso 1 1 calc R . . C6 C 0.1760(3) 0.6949(2) -0.19509(19) 0.0289(5) Uani 1 1 d . . . H6 H 0.2589 0.7628 -0.1713 0.035 Uiso 1 1 calc R . . C7 C 0.2294(2) 0.89831(19) 0.08036(18) 0.0237(5) Uani 1 1 d . . . C8 C 0.1142(3) 0.9459(2) 0.1394(2) 0.0347(6) Uani 1 1 d . . . H8 H 0.0496 0.8928 0.1561 0.042 Uiso 1 1 calc R . . C9 C 0.0932(3) 1.0699(2) 0.1738(2) 0.0444(7) Uani 1 1 d . . . H9 H 0.0139 1.1016 0.2139 0.053 Uiso 1 1 calc R . . C10 C 0.1859(3) 1.1483(2) 0.1506(2) 0.0402(6) Uani 1 1 d . . . H10 H 0.1706 1.2336 0.1748 0.048 Uiso 1 1 calc R . . C11 C 0.3006(3) 1.1030(2) 0.0925(2) 0.0432(7) Uani 1 1 d . . . H11 H 0.3654 1.1567 0.0766 0.052 Uiso 1 1 calc R . . C12 C 0.3211(3) 0.9780(2) 0.0572(2) 0.0373(6) Uani 1 1 d . . . H12 H 0.3998 0.9466 0.0164 0.045 Uiso 1 1 calc R . . C13 C 0.4569(2) 0.72182(19) 0.04195(18) 0.0228(5) Uani 1 1 d . . . C14 C 0.5054(3) 0.6209(2) -0.0396(2) 0.0296(5) Uani 1 1 d . . . H14 H 0.4275 0.5623 -0.1062 0.036 Uiso 1 1 calc R . . C15 C 0.6665(3) 0.6055(2) -0.0242(2) 0.0334(6) Uani 1 1 d . . . H15 H 0.6987 0.5363 -0.0802 0.04 Uiso 1 1 calc R . . C16 C 0.7802(3) 0.6897(2) 0.0714(2) 0.0353(6) Uani 1 1 d . . . H16 H 0.8906 0.6785 0.0817 0.042 Uiso 1 1 calc R . . C17 C 0.7338(3) 0.7911(2) 0.1530(2) 0.0374(6) Uani 1 1 d . . . H17 H 0.8124 0.8496 0.2192 0.045 Uiso 1 1 calc R . . C18 C 0.5729(3) 0.8071(2) 0.13795(19) 0.0321(6) Uani 1 1 d . . . H18 H 0.5415 0.877 0.1938 0.039 Uiso 1 1 calc R . . C19 C -0.2854(3) 0.3127(2) -0.4144(2) 0.0398(6) Uani 1 1 d . . . H19 H -0.2594 0.3531 -0.4624 0.048 Uiso 1 1 calc R . . C20 C -0.2269(4) 0.1814(2) -0.4627(2) 0.0496(7) Uani 1 1 d . . . C21 C -0.2577(5) 0.1030(3) -0.4011(3) 0.0802(12) Uani 1 1 d . . . H21C H -0.3743 0.0814 -0.4154 0.12 Uiso 1 1 calc R . . H21B H -0.2094 0.1512 -0.3185 0.12 Uiso 1 1 calc R . . H21A H -0.2093 0.0261 -0.4299 0.12 Uiso 1 1 calc R . . C22 C -0.3027(4) 0.1042(3) -0.5921(3) 0.0770(11) Uani 1 1 d . . . H22C H -0.2526 0.0281 -0.6202 0.116 Uiso 1 1 calc R . . H22B H -0.2851 0.1541 -0.6325 0.116 Uiso 1 1 calc R . . H22A H -0.4189 0.0812 -0.606 0.116 Uiso 1 1 calc R . . C23 C -0.0447(4) 0.2038(3) -0.4485(3) 0.0672(9) Uani 1 1 d . . . H23C H -0.0046 0.123 -0.4778 0.101 Uiso 1 1 calc R . . H23B H 0.0107 0.2528 -0.3671 0.101 Uiso 1 1 calc R . . H23A H -0.0237 0.2497 -0.4916 0.101 Uiso 1 1 calc R . . C24 C -0.4663(3) 0.3284(2) -0.4142(2) 0.0473(7) Uani 1 1 d . . . C25 C -0.5816(4) 0.2649(3) -0.5356(3) 0.0742(10) Uani 1 1 d . . . H25C H -0.5856 0.1738 -0.566 0.111 Uiso 1 1 calc R . . H25B H -0.5427 0.2938 -0.5859 0.111 Uiso 1 1 calc R . . H25A H -0.69 0.2866 -0.5323 0.111 Uiso 1 1 calc R . . C26 C -0.5291(3) 0.2831(3) -0.3367(3) 0.0642(9) Uani 1 1 d . . . H26C H -0.4608 0.3276 -0.258 0.096 Uiso 1 1 calc R . . H26B H -0.5263 0.1929 -0.3642 0.096 Uiso 1 1 calc R . . H26A H -0.6403 0.2997 -0.3384 0.096 Uiso 1 1 calc R . . C27 C -0.4745(4) 0.4697(3) -0.3677(3) 0.0573(8) Uani 1 1 d . . . H27C H -0.5864 0.4841 -0.3689 0.086 Uiso 1 1 calc R . . H27B H -0.4359 0.5022 -0.4158 0.086 Uiso 1 1 calc R . . H27A H -0.4065 0.513 -0.2887 0.086 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 P 0.0195(3) 0.0201(3) 0.0233(3) 0.0080(2) 0.0063(2) 0.0022(2) O 0.0227(8) 0.0249(8) 0.0254(8) 0.0112(7) 0.0078(6) 0.0024(6) N 0.0484(13) 0.0257(11) 0.0206(11) 0.0102(9) -0.0002(9) -0.0118(9) C1 0.0212(11) 0.0206(11) 0.0231(12) 0.0087(9) 0.0069(9) 0.0048(9) C2 0.0252(11) 0.0214(11) 0.0224(12) 0.0092(9) 0.0073(9) 0.0054(9) C3 0.0339(13) 0.0200(11) 0.0253(12) 0.0091(10) 0.0076(10) 0.0019(10) C4 0.0496(15) 0.0285(13) 0.0193(12) 0.0071(10) 0.0029(11) -0.0046(11) C5 0.0478(15) 0.0337(14) 0.0256(13) 0.0141(11) 0.0120(12) -0.0011(12) C6 0.0310(12) 0.0247(12) 0.0299(13) 0.0115(11) 0.0077(10) -0.0023(10) C7 0.0231(11) 0.0223(11) 0.0231(12) 0.0087(10) 0.0040(9) 0.0020(9) C8 0.0327(13) 0.0291(13) 0.0448(15) 0.0155(12) 0.0158(12) 0.0063(11) C9 0.0410(15) 0.0333(14) 0.0598(18) 0.0154(13) 0.0233(14) 0.0166(12) C10 0.0485(16) 0.0211(13) 0.0453(16) 0.0119(12) 0.0062(13) 0.0088(12) C11 0.0525(17) 0.0294(14) 0.0569(17) 0.0237(13) 0.0218(14) 0.0047(12) C12 0.0416(14) 0.0284(13) 0.0471(16) 0.0159(12) 0.0225(12) 0.0061(11) C13 0.0218(11) 0.0223(11) 0.0258(12) 0.0115(10) 0.0071(10) 0.0013(9) C14 0.0277(12) 0.0225(12) 0.0362(14) 0.0098(11) 0.0098(10) 0.0033(10) C15 0.0311(13) 0.0236(12) 0.0458(15) 0.0113(11) 0.0179(12) 0.0076(11) C16 0.0227(12) 0.0393(14) 0.0489(16) 0.0224(13) 0.0122(12) 0.0075(11) C17 0.0231(12) 0.0437(15) 0.0335(14) 0.0083(12) 0.0032(11) -0.0013(11) C18 0.0263(12) 0.0345(13) 0.0286(13) 0.0063(11) 0.0093(11) 0.0033(11) C19 0.0556(16) 0.0312(14) 0.0224(13) 0.0100(11) -0.0020(12) -0.0158(12) C20 0.079(2) 0.0287(14) 0.0285(14) 0.0040(12) 0.0093(14) -0.0107(14) C21 0.151(4) 0.0300(16) 0.068(2) 0.0187(16) 0.048(2) 0.0122(19) C22 0.099(3) 0.060(2) 0.0387(18) -0.0064(16) 0.0168(18) -0.0216(19) C23 0.083(2) 0.0408(17) 0.066(2) 0.0148(16) 0.0140(18) 0.0093(17) C24 0.0502(17) 0.0457(16) 0.0379(16) 0.0236(13) -0.0113(13) -0.0137(13) C25 0.077(2) 0.060(2) 0.058(2) 0.0258(17) -0.0299(17) -0.0135(17) C26 0.0439(17) 0.082(2) 0.074(2) 0.052(2) -0.0021(15) -0.0134(16) C27 0.0612(19) 0.0568(19) 0.0513(18) 0.0268(16) 0.0047(15) 0.0029(15) #----------------------------------------------------------------------------# # 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 P O 1.4924(15) . ? P C13 1.803(2) . ? P C1 1.805(2) . ? P C7 1.810(2) . ? N C3 1.370(3) . ? N C19 1.462(3) . ? C1 C2 1.385(3) . ? C1 C6 1.400(3) . ? C2 C3 1.413(3) . ? C3 C4 1.404(3) . ? C4 C5 1.382(3) . ? C5 C6 1.379(3) . ? C7 C12 1.383(3) . ? C7 C8 1.390(3) . ? C8 C9 1.380(3) . ? C9 C10 1.376(3) . ? C10 C11 1.374(3) . ? C11 C12 1.388(3) . ? C13 C18 1.388(3) . ? C13 C14 1.392(3) . ? C14 C15 1.384(3) . ? C15 C16 1.372(3) . ? C16 C17 1.386(3) . ? C17 C18 1.383(3) . ? C19 C20 1.568(4) . ? C19 C24 1.572(4) . ? C20 C21 1.526(4) . ? C20 C23 1.535(4) . ? C20 C22 1.536(4) . ? C24 C26 1.529(4) . ? C24 C27 1.537(4) . ? C24 C25 1.539(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O P C13 113.39(9) . . ? O P C1 112.04(9) . . ? C13 P C1 106.10(9) . . ? O P C7 112.10(9) . . ? C13 P C7 105.90(10) . . ? C1 P C7 106.81(9) . . ? C3 N C19 126.2(2) . . ? C2 C1 C6 120.6(2) . . ? C2 C1 P 118.15(15) . . ? C6 C1 P 121.22(16) . . ? C1 C2 C3 121.2(2) . . ? N C3 C4 123.9(2) . . ? N C3 C2 118.91(19) . . ? C4 C3 C2 117.2(2) . . ? C5 C4 C3 120.9(2) . . ? C6 C5 C4 121.8(2) . . ? C5 C6 C1 118.3(2) . . ? C12 C7 C8 118.4(2) . . ? C12 C7 P 123.63(16) . . ? C8 C7 P 117.91(17) . . ? C9 C8 C7 120.2(2) . . ? C10 C9 C8 120.7(2) . . ? C11 C10 C9 119.8(2) . . ? C10 C11 C12 119.5(2) . . ? C7 C12 C11 121.3(2) . . ? C18 C13 C14 118.89(19) . . ? C18 C13 P 119.36(15) . . ? C14 C13 P 121.34(17) . . ? C15 C14 C13 120.3(2) . . ? C16 C15 C14 120.4(2) . . ? C15 C16 C17 119.9(2) . . ? C18 C17 C16 119.9(2) . . ? C17 C18 C13 120.5(2) . . ? N C19 C20 109.1(2) . . ? N C19 C24 108.51(19) . . ? C20 C19 C24 122.7(2) . . ? C21 C20 C23 108.6(3) . . ? C21 C20 C22 108.7(2) . . ? C23 C20 C22 105.7(2) . . ? C21 C20 C19 113.4(2) . . ? C23 C20 C19 107.7(2) . . ? C22 C20 C19 112.4(2) . . ? C26 C24 C27 107.1(2) . . ? C26 C24 C25 108.9(2) . . ? C27 C24 C25 107.1(2) . . ? C26 C24 C19 114.4(2) . . ? C27 C24 C19 106.4(2) . . ? C25 C24 C19 112.5(2) . . ? data_sep901 _database_code_depnum_ccdc_archive 'CCDC 216488' _audit_creation_date 2001-09-14T16:45:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ((Li(Ph2PC6H3NCHtBu2))4).3(pentane) _chemical_formula_moiety '(C108 H132 Li4 N4 P4).(3(C5 H12)' _chemical_formula_sum 'C123 H168 Li4 N4 P4' _chemical_formula_weight 1854.25 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 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 28.5865(16) _cell_length_b 12.2440(4) _cell_length_c 32.9959(19) _cell_angle_alpha 90 _cell_angle_beta 90.091(2) _cell_angle_gamma 90 _cell_volume 11549.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33953 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4024 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_T_min 0.9779 _exptl_absorpt_correction_T_max 0.9944 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 21796 _diffrn_reflns_av_R_equivalents 0.11 _diffrn_reflns_av_unetI/netI 0.1077 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 22 _diffrn_reflns_theta_full 22 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 7027 _reflns_number_gt 4542 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are two pentane solvate molecules; one in a general position and one disordered across an inversion centre. Both were refined with bond length constraints, isotropic C atoms and H atoms omitted. 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^)+(0.0862P)^2^+18.3579P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7027 _refine_ls_number_parameters 574 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1212 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.516 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.061 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 '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' P P 0.1023 0.0942 '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 Li1 Li 0.1372(3) -0.0595(7) 0.2740(2) 0.051(2) Uani 1 1 d . . . Li2 Li 0.0171(3) -0.0798(6) 0.1632(2) 0.047(2) Uani 1 1 d . . . P1 P 0.06491(4) 0.03932(9) 0.07411(4) 0.0382(4) Uani 1 1 d . A 1 P2 P 0.00399(4) -0.27121(9) 0.43041(4) 0.0396(4) Uani 1 1 d . B 1 N1 N 0.13482(12) -0.0701(3) 0.21543(11) 0.0389(9) Uani 1 1 d . A 1 N2 N 0.11212(12) -0.0674(3) 0.32835(11) 0.0380(9) Uani 1 1 d . A 1 C1 C 0.06368(14) 0.0472(3) 0.12979(13) 0.0328(11) Uani 1 1 d . A 1 C2 C 0.09614(15) -0.0192(3) 0.15011(13) 0.0360(11) Uani 1 1 d . A 1 H2 H 0.1156 -0.0657 0.1344 0.043 Uiso 1 1 calc R A 1 C3 C 0.10148(15) -0.0204(3) 0.19331(13) 0.0339(11) Uani 1 1 d . A 1 C4 C 0.06507(15) 0.0380(3) 0.21423(14) 0.0362(11) Uani 1 1 d . A 1 H4 H 0.0636 0.033 0.2429 0.043 Uiso 1 1 calc R A 1 C5 C 0.03217(15) 0.1008(3) 0.19439(14) 0.0369(11) Uani 1 1 d . A 1 H5 H 0.0097 0.14 0.2098 0.044 Uiso 1 1 calc R A 1 C6 C 0.03104(15) 0.1081(3) 0.15202(14) 0.0369(11) Uani 1 1 d . A 1 H6 H 0.0088 0.1532 0.1387 0.044 Uiso 1 1 calc R A 1 C7 C 0.11064(16) 0.1383(3) 0.06125(14) 0.0386(12) Uani 1 1 d . A 1 C8 C 0.14424(18) 0.1749(4) 0.08826(17) 0.0585(15) Uani 1 1 d . A 1 H8 H 0.1423 0.1543 0.116 0.07 Uiso 1 1 calc R A 1 C9 C 0.1810(2) 0.2422(5) 0.0753(2) 0.0752(18) Uani 1 1 d . A 1 H9 H 0.2036 0.2673 0.0943 0.09 Uiso 1 1 calc R A 1 C10 C 0.1845(2) 0.2719(5) 0.03521(19) 0.0665(16) Uani 1 1 d . A 1 H10 H 0.2101 0.3152 0.0263 0.08 Uiso 1 1 calc R A 1 C11 C 0.1508(2) 0.2384(4) 0.00814(16) 0.0567(14) Uani 1 1 d . A 1 H11 H 0.1522 0.2617 -0.0193 0.068 Uiso 1 1 calc R A 1 C12 C 0.11475(17) 0.1711(4) 0.02062(15) 0.0478(13) Uani 1 1 d . A 1 H12 H 0.0924 0.1465 0.0014 0.057 Uiso 1 1 calc R A 1 C13 C 0.01197(16) 0.1139(3) 0.05886(13) 0.0366(11) Uani 1 1 d . A 1 C14 C 0.00713(16) 0.2263(4) 0.06128(14) 0.0425(12) Uani 1 1 d . A 1 H14 H 0.0322 0.2689 0.0717 0.051 Uiso 1 1 calc R A 1 C15 C -0.03339(17) 0.2775(4) 0.04885(15) 0.0481(13) Uani 1 1 d . A 1 H15 H -0.0363 0.3545 0.051 0.058 Uiso 1 1 calc R A 1 C16 C -0.06970(17) 0.2165(4) 0.03327(14) 0.0487(13) Uani 1 1 d . A 1 H16 H -0.0977 0.2517 0.0247 0.058 Uiso 1 1 calc R A 1 C17 C -0.06562(17) 0.1055(4) 0.03004(14) 0.0471(13) Uani 1 1 d . A 1 H17 H -0.0906 0.0638 0.019 0.057 Uiso 1 1 calc R A 1 C18 C -0.02480(16) 0.0534(4) 0.04298(13) 0.0408(12) Uani 1 1 d . A 1 H18 H -0.0222 -0.0237 0.0409 0.049 Uiso 1 1 calc R A 1 C19 C 0.17164(15) -0.1321(4) 0.19355(14) 0.0438(12) Uani 1 1 d . A 1 H19 H 0.1611 -0.1339 0.1646 0.053 Uiso 1 1 calc R A 1 C20 C 0.21924(16) -0.0669(4) 0.19316(15) 0.0485(13) Uani 1 1 d . A 1 C21 C 0.2471(2) -0.0745(5) 0.23287(19) 0.0832(19) Uani 1 1 d . A 1 H21A H 0.2546 -0.1511 0.2385 0.125 Uiso 1 1 calc R A 1 H21B H 0.2284 -0.0446 0.2551 0.125 Uiso 1 1 calc R A 1 H21C H 0.2762 -0.0326 0.2303 0.125 Uiso 1 1 calc R A 1 C22 C 0.2511(2) -0.1054(6) 0.1588(2) 0.092(2) Uani 1 1 d . A 1 H22A H 0.2585 -0.1829 0.1625 0.138 Uiso 1 1 calc R A 1 H22B H 0.2802 -0.0628 0.1591 0.138 Uiso 1 1 calc R A 1 H22C H 0.2352 -0.095 0.1328 0.138 Uiso 1 1 calc R A 1 C23 C 0.20911(19) 0.0538(5) 0.18576(19) 0.0774(19) Uani 1 1 d . A 1 H23A H 0.1911 0.062 0.1607 0.116 Uiso 1 1 calc R A 1 H23B H 0.2387 0.0938 0.1833 0.116 Uiso 1 1 calc R A 1 H23C H 0.1911 0.0832 0.2085 0.116 Uiso 1 1 calc R A 1 C24 C 0.16894(16) -0.2534(4) 0.20845(15) 0.0478(13) Uani 1 1 d . A 1 C25 C 0.2062(2) -0.3261(5) 0.18878(18) 0.0738(17) Uani 1 1 d . A 1 H25A H 0.2373 -0.3002 0.1966 0.111 Uiso 1 1 calc R A 1 H25B H 0.2029 -0.3229 0.1592 0.111 Uiso 1 1 calc R A 1 H25C H 0.202 -0.4016 0.198 0.111 Uiso 1 1 calc R A 1 C26 C 0.17215(19) -0.2682(4) 0.25495(16) 0.0596(15) Uani 1 1 d . A 1 H26A H 0.1486 -0.2223 0.2681 0.089 Uiso 1 1 calc R A 1 H26B H 0.2034 -0.2469 0.2643 0.089 Uiso 1 1 calc R A 1 H26C H 0.1665 -0.345 0.2619 0.089 Uiso 1 1 calc R A 1 C27 C 0.12080(17) -0.2972(4) 0.19545(17) 0.0599(15) Uani 1 1 d . A 1 H27A H 0.0962 -0.2527 0.2079 0.09 Uiso 1 1 calc R A 1 H27B H 0.1175 -0.3732 0.2043 0.09 Uiso 1 1 calc R A 1 H27C H 0.118 -0.2935 0.1659 0.09 Uiso 1 1 calc R A 1 C28 C 0.01587(15) -0.2281(3) 0.37828(13) 0.0354(11) Uani 1 1 d . . 1 C29 C 0.05250(15) -0.1528(3) 0.37398(13) 0.0376(11) Uani 1 1 d . A 1 H29 H 0.0642 -0.1177 0.3976 0.045 Uiso 1 1 calc R A 1 C30 C 0.07346(16) -0.1261(3) 0.33527(14) 0.0364(11) Uani 1 1 d . A 1 C31 C 0.04756(15) -0.1707(3) 0.30140(13) 0.0376(11) Uani 1 1 d . . 1 H31 H 0.0568 -0.1505 0.2748 0.045 Uiso 1 1 calc R . 1 C32 C 0.01025(16) -0.2409(3) 0.30566(14) 0.0399(12) Uani 1 1 d . . 1 H32 H -0.0045 -0.2694 0.2821 0.048 Uiso 1 1 calc R . 1 C33 C -0.00636(15) -0.2712(3) 0.34384(14) 0.0390(12) Uani 1 1 d . . 1 H33 H -0.0321 -0.3199 0.3464 0.047 Uiso 1 1 calc R . 1 C34 C 0.04976(16) -0.3750(4) 0.43515(14) 0.0406(12) Uani 1 1 d . B 1 C35 C 0.07762(19) -0.4123(4) 0.40362(17) 0.0619(15) Uani 1 1 d . B 1 H35 H 0.0714 -0.3882 0.3768 0.074 Uiso 1 1 calc R B 1 C36 C 0.1141(2) -0.4837(5) 0.4105(2) 0.0754(18) Uani 1 1 d . B 1 H36 H 0.1327 -0.5079 0.3884 0.09 Uiso 1 1 calc R B 1 C37 C 0.12388(19) -0.5201(4) 0.4488(2) 0.0703(18) Uani 1 1 d . B 1 H37 H 0.1495 -0.5681 0.4534 0.084 Uiso 1 1 calc R B 1 C38 C 0.0965(2) -0.4866(4) 0.48054(19) 0.0641(16) Uani 1 1 d . B 1 H38 H 0.1024 -0.5134 0.5071 0.077 Uiso 1 1 calc R B 1 C39 C 0.06009(19) -0.4139(4) 0.47397(16) 0.0538(14) Uani 1 1 d . B 1 H39 H 0.0418 -0.3901 0.4963 0.065 Uiso 1 1 calc R B 1 C40 C -0.04958(16) -0.3522(4) 0.42330(13) 0.0413(12) Uani 1 1 d . B 1 C41 C -0.05039(18) -0.4625(4) 0.41317(16) 0.0536(14) Uani 1 1 d . B 1 H41 H -0.0218 -0.5015 0.4105 0.064 Uiso 1 1 calc R B 1 C42 C -0.0927(2) -0.5158(4) 0.40691(17) 0.0641(16) Uani 1 1 d . B 1 H42 H -0.093 -0.5911 0.3999 0.077 Uiso 1 1 calc R B 1 C43 C -0.1344(2) -0.4594(5) 0.41086(17) 0.0622(15) Uani 1 1 d . B 1 H43 H -0.1634 -0.4957 0.4066 0.075 Uiso 1 1 calc R B 1 C44 C -0.13369(18) -0.3517(5) 0.42088(16) 0.0581(15) Uani 1 1 d . B 1 H44 H -0.1623 -0.3128 0.4232 0.07 Uiso 1 1 calc R B 1 C45 C -0.09186(17) -0.2981(4) 0.42769(14) 0.0480(13) Uani 1 1 d . B 1 H45 H -0.0921 -0.2233 0.4355 0.058 Uiso 1 1 calc R B 1 C46 C 0.13620(15) -0.0152(4) 0.36266(14) 0.0410(12) Uani 1 1 d . A 1 H46 H 0.1137 -0.0191 0.3858 0.049 Uiso 1 1 calc R A 1 C47 C 0.18058(17) -0.0844(4) 0.37670(15) 0.0509(13) Uani 1 1 d . A 1 C48 C 0.22240(17) -0.0725(5) 0.34828(17) 0.0646(16) Uani 1 1 d . A 1 H48A H 0.2128 -0.0904 0.3205 0.097 Uiso 1 1 calc R A 1 H48B H 0.2474 -0.1223 0.3569 0.097 Uiso 1 1 calc R A 1 H48C H 0.2339 0.0029 0.3492 0.097 Uiso 1 1 calc R A 1 C49 C 0.1955(2) -0.0555(5) 0.41987(16) 0.0700(16) Uani 1 1 d . A 1 H49A H 0.1686 -0.0624 0.4381 0.105 Uiso 1 1 calc R A 1 H49B H 0.2071 0.0199 0.4205 0.105 Uiso 1 1 calc R A 1 H49C H 0.2204 -0.1052 0.4287 0.105 Uiso 1 1 calc R A 1 C50 C 0.16698(17) -0.2060(4) 0.37747(16) 0.0596(15) Uani 1 1 d . A 1 H50A H 0.1403 -0.2165 0.3957 0.089 Uiso 1 1 calc R A 1 H50B H 0.1936 -0.2494 0.3871 0.089 Uiso 1 1 calc R A 1 H50C H 0.1583 -0.2296 0.3501 0.089 Uiso 1 1 calc R A 1 C51 C 0.14122(16) 0.1081(4) 0.35275(14) 0.0446(12) Uani 1 1 d . A 1 C52 C 0.16076(17) 0.1307(4) 0.31006(14) 0.0502(13) Uani 1 1 d . A 1 H52A H 0.1928 0.1025 0.3082 0.075 Uiso 1 1 calc R A 1 H52B H 0.1609 0.2095 0.305 0.075 Uiso 1 1 calc R A 1 H52C H 0.1411 0.0944 0.2898 0.075 Uiso 1 1 calc R A 1 C53 C 0.09125(16) 0.1559(4) 0.35381(16) 0.0527(14) Uani 1 1 d . A 1 H53A H 0.0775 0.1436 0.3806 0.079 Uiso 1 1 calc R A 1 H53B H 0.072 0.12 0.3332 0.079 Uiso 1 1 calc R A 1 H53C H 0.0925 0.2345 0.3483 0.079 Uiso 1 1 calc R A 1 C54 C 0.16979(18) 0.1731(4) 0.38416(16) 0.0592(15) Uani 1 1 d . A 1 H54A H 0.1572 0.1596 0.4113 0.089 Uiso 1 1 calc R A 1 H54B H 0.1677 0.2513 0.378 0.089 Uiso 1 1 calc R A 1 H54C H 0.2026 0.1499 0.3832 0.089 Uiso 1 1 calc R A 1 C55 C 0.1366(4) 0.3221(10) 0.1953(4) 0.174(4) Uiso 1 1 d D C 2 C56 C 0.1148(6) 0.3750(14) 0.2262(5) 0.263(7) Uiso 1 1 d D C 2 C57 C 0.0851(5) 0.3842(12) 0.2566(5) 0.224(6) Uiso 1 1 d D C 2 C58 C 0.0713(6) 0.4665(15) 0.2869(5) 0.273(8) Uiso 1 1 d D C 2 C59 C 0.0341(4) 0.4305(9) 0.3121(4) 0.176(4) Uiso 1 1 d D C 2 C60 C 0.25 0.25 0.5 0.207(7) Uiso 1 2 d SD . 2 C62 C 0.2150(6) 0.0797(13) 0.5311(5) 0.247(7) Uiso 1 1 d D D 2 C61A C 0.2185(10) 0.168(2) 0.5065(10) 0.257(15) Uiso 0.5 1 d PD D 2 C61B C 0.2473(9) 0.1560(15) 0.5220(8) 0.189(10) Uiso 0.5 1 d PD D 2 M1 C 0.0649 0.0424 0.1723 0.01 Uiso 0 1 d P A 3 M2 C 0.0322 -0.1983 0.3397 0.01 Uiso 0 1 d P . 3 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 Li1 0.034(5) 0.078(6) 0.041(5) 0.002(4) 0.004(4) -0.002(4) Li2 0.043(5) 0.047(5) 0.052(5) 0.000(4) 0.012(4) 0.002(4) P1 0.0379(8) 0.0422(7) 0.0346(8) -0.0010(5) 0.0010(6) 0.0031(6) P2 0.0397(8) 0.0433(7) 0.0358(8) 0.0038(6) 0.0079(6) -0.0028(6) N1 0.028(2) 0.055(2) 0.033(2) 0.0026(18) 0.0031(18) 0.0082(19) N2 0.028(2) 0.053(2) 0.034(2) 0.0035(18) 0.0037(18) -0.0035(19) C1 0.027(3) 0.036(2) 0.035(3) 0.002(2) 0.002(2) 0.001(2) C2 0.031(3) 0.041(3) 0.036(3) -0.002(2) 0.004(2) 0.003(2) C3 0.028(3) 0.042(3) 0.031(3) -0.001(2) 0.006(2) -0.002(2) C4 0.032(3) 0.042(3) 0.035(3) -0.002(2) 0.005(2) -0.002(2) C5 0.030(3) 0.037(3) 0.043(3) -0.003(2) 0.007(2) 0.005(2) C6 0.031(3) 0.041(3) 0.039(3) 0.000(2) 0.001(2) 0.002(2) C7 0.039(3) 0.040(3) 0.037(3) 0.000(2) -0.001(2) 0.007(2) C8 0.053(4) 0.073(4) 0.050(3) 0.010(3) -0.002(3) -0.013(3) C9 0.060(4) 0.085(4) 0.080(5) 0.007(4) -0.011(3) -0.030(3) C10 0.055(4) 0.075(4) 0.069(5) 0.009(3) 0.013(3) -0.011(3) C11 0.067(4) 0.057(3) 0.046(3) 0.007(3) 0.014(3) 0.003(3) C12 0.050(3) 0.049(3) 0.044(3) -0.002(2) 0.005(3) -0.003(3) C13 0.037(3) 0.043(3) 0.030(3) -0.001(2) 0.005(2) 0.001(2) C14 0.038(3) 0.043(3) 0.046(3) 0.005(2) -0.006(2) 0.002(2) C15 0.047(3) 0.049(3) 0.048(3) 0.002(2) -0.002(3) 0.004(3) C16 0.043(3) 0.063(4) 0.040(3) 0.004(3) -0.002(2) 0.015(3) C17 0.035(3) 0.066(4) 0.040(3) -0.003(2) 0.000(2) -0.003(3) C18 0.045(3) 0.046(3) 0.031(3) -0.002(2) 0.005(2) 0.000(3) C19 0.036(3) 0.061(3) 0.035(3) 0.001(2) 0.001(2) 0.014(2) C20 0.032(3) 0.069(3) 0.044(3) 0.010(3) 0.005(2) 0.007(3) C21 0.055(4) 0.116(5) 0.079(5) 0.017(4) -0.013(3) -0.027(4) C22 0.078(5) 0.115(5) 0.083(5) 0.000(4) 0.041(4) 0.010(4) C23 0.052(4) 0.078(4) 0.103(5) 0.027(4) 0.012(3) -0.001(3) C24 0.040(3) 0.056(3) 0.047(3) -0.008(2) -0.005(2) 0.013(2) C25 0.066(4) 0.072(4) 0.084(5) -0.009(3) 0.005(3) 0.023(3) C26 0.060(4) 0.057(3) 0.062(4) 0.009(3) -0.005(3) 0.005(3) C27 0.050(3) 0.061(3) 0.069(4) -0.005(3) -0.004(3) 0.006(3) C28 0.035(3) 0.038(3) 0.033(3) 0.004(2) 0.004(2) 0.003(2) C29 0.036(3) 0.043(3) 0.034(3) 0.003(2) 0.003(2) 0.001(2) C30 0.032(3) 0.040(3) 0.038(3) 0.002(2) 0.002(2) 0.005(2) C31 0.036(3) 0.046(3) 0.030(3) 0.008(2) 0.005(2) 0.004(2) C32 0.043(3) 0.044(3) 0.033(3) -0.001(2) 0.003(2) -0.001(2) C33 0.029(3) 0.044(3) 0.044(3) 0.003(2) -0.001(2) -0.002(2) C34 0.036(3) 0.047(3) 0.039(3) 0.004(2) 0.000(2) -0.006(2) C35 0.059(4) 0.068(4) 0.059(4) 0.019(3) 0.014(3) 0.018(3) C36 0.065(4) 0.070(4) 0.091(5) 0.025(4) 0.030(4) 0.017(3) C37 0.037(3) 0.051(3) 0.122(6) 0.019(4) -0.016(4) 0.002(3) C38 0.067(4) 0.054(3) 0.071(4) 0.011(3) -0.020(4) -0.002(3) C39 0.067(4) 0.047(3) 0.048(4) 0.002(3) -0.008(3) -0.009(3) C40 0.039(3) 0.047(3) 0.038(3) 0.007(2) 0.007(2) -0.002(2) C41 0.048(3) 0.049(3) 0.064(4) 0.005(3) 0.002(3) -0.006(3) C42 0.064(4) 0.051(3) 0.077(4) 0.006(3) -0.009(3) -0.017(3) C43 0.046(4) 0.069(4) 0.071(4) 0.019(3) -0.004(3) -0.010(3) C44 0.039(3) 0.073(4) 0.062(4) 0.017(3) 0.001(3) 0.003(3) C45 0.045(3) 0.054(3) 0.044(3) 0.007(2) 0.009(3) 0.000(3) C46 0.035(3) 0.055(3) 0.033(3) 0.006(2) 0.006(2) -0.009(2) C47 0.040(3) 0.065(3) 0.049(3) 0.015(3) -0.004(3) -0.003(3) C48 0.037(3) 0.090(4) 0.067(4) 0.024(3) 0.007(3) 0.008(3) C49 0.067(4) 0.096(4) 0.047(4) 0.014(3) -0.012(3) -0.007(3) C50 0.045(3) 0.069(4) 0.065(4) 0.016(3) -0.002(3) 0.009(3) C51 0.037(3) 0.055(3) 0.042(3) 0.004(2) 0.006(2) -0.008(2) C52 0.042(3) 0.056(3) 0.052(3) 0.009(2) 0.005(3) -0.007(2) C53 0.039(3) 0.060(3) 0.060(4) 0.001(3) 0.001(3) -0.001(2) C54 0.047(3) 0.069(4) 0.061(4) -0.004(3) 0.000(3) -0.018(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N2 1.936(8) . ? Li1 N1 1.937(9) . ? Li2 M1 2.049(8) . ? Li2 C1 2.325(9) . ? P1 C7 1.833(5) . ? P1 C13 1.837(5) . ? P1 C1 1.840(4) . ? P2 C34 1.830(5) . ? P2 C28 1.832(4) . ? P2 C40 1.839(5) . ? N1 C3 1.345(5) . ? N1 C19 1.486(5) . ? N2 C30 1.338(5) . ? N2 C46 1.470(6) . ? C1 C6 1.403(6) . ? C1 C2 1.403(6) . ? C2 C3 1.433(6) . ? C3 C4 1.440(6) . ? C4 C5 1.379(6) . ? C5 C6 1.401(6) . ? C7 C8 1.384(7) . ? C7 C12 1.405(6) . ? C8 C9 1.403(7) . ? C9 C10 1.377(8) . ? C10 C11 1.377(7) . ? C11 C12 1.382(7) . ? C13 C14 1.386(6) . ? C13 C18 1.387(6) . ? C14 C15 1.379(6) . ? C15 C16 1.377(6) . ? C16 C17 1.369(6) . ? C17 C18 1.396(6) . ? C19 C24 1.567(7) . ? C19 C20 1.577(6) . ? C20 C23 1.526(7) . ? C20 C22 1.530(7) . ? C20 C21 1.535(7) . ? C24 C25 1.532(7) . ? C24 C27 1.537(7) . ? C24 C26 1.548(7) . ? C28 C29 1.402(6) . ? C28 C33 1.404(6) . ? C28 Li2 2.460(9) 2 ? C29 C30 1.449(6) . ? C30 C31 1.447(6) . ? C31 C32 1.377(6) . ? C31 Li2 2.456(9) 2 ? C32 C33 1.397(6) . ? C32 Li2 2.359(9) 2 ? C33 Li2 2.375(9) 2 ? C34 C35 1.389(7) . ? C34 C39 1.398(6) . ? C35 C36 1.379(7) . ? C36 C37 1.369(8) . ? C37 C38 1.370(8) . ? C38 C39 1.385(7) . ? C40 C45 1.386(6) . ? C40 C41 1.391(6) . ? C41 C42 1.391(7) . ? C42 C43 1.384(7) . ? C43 C44 1.360(7) . ? C44 C45 1.382(7) . ? C46 C51 1.552(6) . ? C46 C47 1.594(6) . ? C47 C48 1.527(7) . ? C47 C49 1.528(7) . ? C47 C50 1.539(7) . ? C51 C54 1.540(7) . ? C51 C52 1.541(6) . ? C51 C53 1.544(6) . ? C55 C56 1.360(12) . ? C56 C57 1.321(12) . ? C57 C58 1.473(13) . ? C58 C59 1.424(12) . ? C60 C61A 1.362(15) . ? C60 C61A 1.362(15) 7_556 ? C60 C61B 1.363(14) . ? C60 C61B 1.363(14) 7_556 ? C62 C61B 1.348(14) . ? C62 C61A 1.359(14) . ? C61A C61B 0.98(4) . ? M2 Li2 2.025(8) 2 ? 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 N2 Li1 N1 155.2(5) . . ? M1 Li2 C1 36.77(16) . . ? C7 P1 C13 101.3(2) . . ? C7 P1 C1 102.2(2) . . ? C13 P1 C1 103.33(19) . . ? C34 P2 C28 98.4(2) . . ? C34 P2 C40 103.4(2) . . ? C28 P2 C40 101.0(2) . . ? C3 N1 C19 118.0(4) . . ? C3 N1 Li1 122.4(4) . . ? C19 N1 Li1 119.6(4) . . ? C30 N2 C46 119.2(4) . . ? C30 N2 Li1 119.5(4) . . ? C46 N2 Li1 121.2(4) . . ? C6 C1 C2 119.9(4) . . ? C6 C1 P1 124.3(3) . . ? C2 C1 P1 115.7(3) . . ? C6 C1 Li2 74.1(3) . . ? C2 C1 Li2 76.4(3) . . ? P1 C1 Li2 116.7(3) . . ? C1 C2 C3 123.4(4) . . ? C1 C2 Li2 69.2(3) . . ? C3 C2 Li2 85.3(3) . . ? N1 C3 C2 128.2(4) . . ? N1 C3 C4 118.5(4) . . ? C2 C3 C4 113.3(4) . . ? C5 C4 C3 122.8(4) . . ? C4 C5 C6 121.6(4) . . ? C5 C6 C1 118.2(4) . . ? C5 C6 Li2 77.6(3) . . ? C1 C6 Li2 71.1(3) . . ? C8 C7 C12 117.6(4) . . ? C8 C7 P1 124.0(4) . . ? C12 C7 P1 118.1(4) . . ? C7 C8 C9 120.9(5) . . ? C10 C9 C8 120.2(5) . . ? C9 C10 C11 119.5(5) . . ? C10 C11 C12 120.4(5) . . ? C11 C12 C7 121.2(5) . . ? C14 C13 C18 118.4(4) . . ? C14 C13 P1 124.1(4) . . ? C18 C13 P1 117.5(3) . . ? C15 C14 C13 121.2(4) . . ? C16 C15 C14 119.8(4) . . ? C17 C16 C15 120.2(5) . . ? C16 C17 C18 120.1(5) . . ? C13 C18 C17 120.3(4) . . ? N1 C19 C24 107.3(4) . . ? N1 C19 C20 110.9(4) . . ? C24 C19 C20 121.7(4) . . ? C23 C20 C22 107.0(5) . . ? C23 C20 C21 107.0(5) . . ? C22 C20 C21 107.7(5) . . ? C23 C20 C19 109.1(4) . . ? C22 C20 C19 111.4(4) . . ? C21 C20 C19 114.2(4) . . ? C25 C24 C27 107.5(4) . . ? C25 C24 C26 108.2(4) . . ? C27 C24 C26 106.7(4) . . ? C25 C24 C19 112.5(4) . . ? C27 C24 C19 106.7(4) . . ? C26 C24 C19 114.8(4) . . ? C29 C28 C33 120.2(4) . . ? C29 C28 P2 115.1(3) . . ? C33 C28 P2 124.6(3) . . ? C29 C28 Li2 75.2(3) . 2 ? C33 C28 Li2 69.8(3) . 2 ? P2 C28 Li2 131.6(3) . 2 ? C28 C29 C30 123.2(4) . . ? N2 C30 C31 119.5(4) . . ? N2 C30 C29 127.9(4) . . ? C31 C30 C29 112.5(4) . . ? C32 C31 C30 123.5(4) . . ? C32 C31 Li2 69.5(3) . 2 ? C30 C31 Li2 81.1(3) . 2 ? C31 C32 C33 121.5(4) . . ? C31 C32 Li2 77.3(3) . 2 ? C33 C32 Li2 73.5(3) . 2 ? C32 C33 C28 118.4(4) . . ? C32 C33 Li2 72.2(3) . 2 ? C28 C33 Li2 76.5(3) . 2 ? C35 C34 C39 117.0(5) . . ? C35 C34 P2 125.1(4) . . ? C39 C34 P2 117.7(4) . . ? C36 C35 C34 121.3(5) . . ? C37 C36 C35 120.8(6) . . ? C36 C37 C38 119.4(5) . . ? C37 C38 C39 120.2(5) . . ? C38 C39 C34 121.3(5) . . ? C45 C40 C41 118.3(4) . . ? C45 C40 P2 117.1(4) . . ? C41 C40 P2 124.6(4) . . ? C42 C41 C40 120.4(5) . . ? C43 C42 C41 120.1(5) . . ? C44 C43 C42 119.6(5) . . ? C43 C44 C45 120.9(5) . . ? C44 C45 C40 120.7(5) . . ? N2 C46 C51 107.7(4) . . ? N2 C46 C47 111.4(4) . . ? C51 C46 C47 120.3(4) . . ? C48 C47 C49 109.4(4) . . ? C48 C47 C50 107.5(4) . . ? C49 C47 C50 106.2(4) . . ? C48 C47 C46 113.2(4) . . ? C49 C47 C46 111.6(4) . . ? C50 C47 C46 108.5(4) . . ? C54 C51 C52 109.3(4) . . ? C54 C51 C53 106.1(4) . . ? C52 C51 C53 106.8(4) . . ? C54 C51 C46 114.2(4) . . ? C52 C51 C46 113.6(4) . . ? C53 C51 C46 106.2(4) . . ? C57 C56 C55 154.9(19) . . ? C56 C57 C58 138.2(18) . . ? C59 C58 C57 112.7(16) . . ? C61A C60 C61A 180(3) . 7_556 ? C61A C60 C61B 42.1(17) . . ? C61A C60 C61B 137.9(17) 7_556 . ? C61A C60 C61B 137.9(17) . 7_556 ? C61A C60 C61B 42.1(17) 7_556 7_556 ? C61B C60 C61B 180.0(18) . 7_556 ? C61B C62 C61A 42.4(17) . . ? C61B C61A C62 68.2(14) . . ? C61B C61A C60 69.0(14) . . ? C62 C61A C60 137(2) . . ? C61A C61B C62 69.4(13) . . ? C61A C61B C60 68.9(13) . . ? C62 C61B C60 138(2) . . ? data_rhnpti _database_code_depnum_ccdc_archive 'CCDC 231686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H70 Cl7 N2 O P2 Rh Ti' _chemical_formula_weight 1260.05 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' P P 0.1023 0.0942 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7085(11) _cell_length_b 16.9770(15) _cell_length_c 17.5902(16) _cell_angle_alpha 108.187(2) _cell_angle_beta 108.333(2) _cell_angle_gamma 104.021(2) _cell_volume 2919.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7172 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.6 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Sadabs v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 24508 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.82 _reflns_number_total 13013 _reflns_number_gt 9576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution ; SIR92 - A program for crystal structure solution. Altomare, A.; Cascarano, G.;Giacovazzo, C.; Guagliardi, A. J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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^)+(0.0411P)^2^+4.0276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13010 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Rh1 Rh -0.08496(2) -0.367429(16) 0.360917(15) 0.02029(7) Uani 1 1 d . . . Ti1 Ti -0.09061(5) -0.17581(4) 0.83989(4) 0.02067(12) Uani 1 1 d . . . P1 P -0.08439(8) -0.26373(5) 0.48396(5) 0.01968(16) Uani 1 1 d . . . Cl1 Cl -0.15033(9) -0.11326(6) 0.94565(6) 0.03338(19) Uani 1 1 d . . . O1 O -0.3219(3) -0.35948(19) 0.24724(17) 0.0441(7) Uani 1 1 d . . . N1 N -0.2354(2) -0.26557(17) 0.73813(16) 0.0212(5) Uani 1 1 d . . . C1 C -0.4606(3) -0.2696(3) 0.6562(2) 0.0335(8) Uani 1 1 d . . . Cl2 Cl -0.02314(8) -0.06189(5) 0.80246(5) 0.02794(17) Uani 1 1 d . . . N2 N 0.0492(2) -0.21128(16) 0.88092(16) 0.0194(5) Uani 1 1 d . . . C2 C -0.5887(4) -0.2713(3) 0.6640(3) 0.0470(10) Uani 1 1 d . . . H2A H -0.6439 -0.2624 0.6151 0.071 Uiso 1 1 calc R . . H2B H -0.5696 -0.2233 0.7202 0.071 Uiso 1 1 calc R . . H2C H -0.6341 -0.3292 0.6617 0.071 Uiso 1 1 calc R . . Cl3 Cl 0.08551(8) -0.38462(5) 0.46205(5) 0.03115(18) Uani 1 1 d . . . C3 C -0.4965(3) -0.3364(3) 0.5625(2) 0.0394(9) Uani 1 1 d . . . H3A H -0.5524 -0.3211 0.5195 0.059 Uiso 1 1 calc R . . H3B H -0.5429 -0.3970 0.5542 0.059 Uiso 1 1 calc R . . H3C H -0.4173 -0.3338 0.5538 0.059 Uiso 1 1 calc R . . C4 C -0.3916(4) -0.1746(3) 0.6670(3) 0.0391(9) Uani 1 1 d . . . H4A H -0.4455 -0.1638 0.6192 0.059 Uiso 1 1 calc R . . H4B H -0.3075 -0.1690 0.6649 0.059 Uiso 1 1 calc R . . H4C H -0.3780 -0.1307 0.7240 0.059 Uiso 1 1 calc R . . C5 C -0.3706(3) -0.2837(2) 0.7343(2) 0.0270(7) Uani 1 1 d . . . H5A H -0.3561 -0.2314 0.7875 0.032 Uiso 1 1 calc R . . C6 C -0.5078(4) -0.3452(3) 0.8059(3) 0.0527(12) Uani 1 1 d . . . H6A H -0.5417 -0.3961 0.8185 0.079 Uiso 1 1 calc R . . H6B H -0.5805 -0.3346 0.7701 0.079 Uiso 1 1 calc R . . H6C H -0.4538 -0.2917 0.8615 0.079 Uiso 1 1 calc R . . P2 P 0.07305(8) -0.53290(5) 0.76004(5) 0.02041(17) Uani 1 1 d . . . C7 C -0.4252(3) -0.3662(3) 0.7548(2) 0.0339(8) Uani 1 1 d . . . C8 C -0.5078(4) -0.4567(3) 0.6746(3) 0.0427(10) Uani 1 1 d . . . H8A H -0.5363 -0.5026 0.6946 0.064 Uiso 1 1 calc R . . H8B H -0.4559 -0.4732 0.6427 0.064 Uiso 1 1 calc R . . H8C H -0.5840 -0.4521 0.6352 0.064 Uiso 1 1 calc R . . C9 C -0.3120(3) -0.3749(3) 0.8204(2) 0.0361(8) Uani 1 1 d . . . H9A H -0.3454 -0.4258 0.8331 0.054 Uiso 1 1 calc R . . H9B H -0.2676 -0.3199 0.8753 0.054 Uiso 1 1 calc R . . H9C H -0.2506 -0.3846 0.7949 0.054 Uiso 1 1 calc R . . C10 C 0.2776(3) -0.0512(2) 0.9375(2) 0.0301(7) Uani 1 1 d . . . H10A H 0.3650 -0.0197 0.9447 0.045 Uiso 1 1 calc R . . H10B H 0.2411 -0.0075 0.9592 0.045 Uiso 1 1 calc R . . H10C H 0.2219 -0.0901 0.8748 0.045 Uiso 1 1 calc R . . C11 C 0.3695(3) -0.0410(2) 1.0875(2) 0.0369(8) Uani 1 1 d . . . H11A H 0.4574 -0.0104 1.0949 0.055 Uiso 1 1 calc R . . H11B H 0.3737 -0.0734 1.1251 0.055 Uiso 1 1 calc R . . H11C H 0.3313 0.0032 1.1045 0.055 Uiso 1 1 calc R . . C12 C 0.1439(4) -0.1351(3) 1.1278(2) 0.0385(9) Uani 1 1 d . . . H12A H 0.1319 -0.1643 1.1663 0.058 Uiso 1 1 calc R . . H12B H 0.0806 -0.1067 1.1168 0.058 Uiso 1 1 calc R . . H12C H 0.2321 -0.0896 1.1563 0.058 Uiso 1 1 calc R . . C13 C 0.2849(3) -0.1079(2) 0.9901(2) 0.0261(7) Uani 1 1 d . . . C14 C 0.3587(3) -0.1675(2) 0.9622(2) 0.0308(7) Uani 1 1 d . . . H14A H 0.4451 -0.1296 0.9730 0.046 Uiso 1 1 calc R . . H14B H 0.3101 -0.2077 0.8992 0.046 Uiso 1 1 calc R . . H14C H 0.3676 -0.2030 0.9967 0.046 Uiso 1 1 calc R . . C16 C 0.1236(3) -0.2056(2) 1.0395(2) 0.0275(7) Uani 1 1 d . . . C18 C 0.2140(4) -0.2555(2) 1.0600(2) 0.0351(8) Uani 1 1 d . . . H18A H 0.1949 -0.2826 1.0985 0.053 Uiso 1 1 calc R . . H18B H 0.3045 -0.2133 1.0897 0.053 Uiso 1 1 calc R . . H18C H 0.2001 -0.3025 1.0048 0.053 Uiso 1 1 calc R . . C17 C -0.0162(3) -0.2718(2) 1.0007(2) 0.0299(7) Uani 1 1 d . . . H17A H -0.0254 -0.3001 1.0404 0.045 Uiso 1 1 calc R . . H17B H -0.0373 -0.3179 0.9428 0.045 Uiso 1 1 calc R . . H17C H -0.0756 -0.2399 0.9941 0.045 Uiso 1 1 calc R . . C21 C 0.0897(3) -0.4225(2) 0.76202(19) 0.0209(6) Uani 1 1 d . . . C19 C 0.0736(3) -0.27813(19) 0.82112(19) 0.0190(6) Uani 1 1 d . . . C22 C 0.1207(3) -0.4018(2) 0.69830(19) 0.0209(6) Uani 1 1 d . . . H22A H 0.1389 -0.4430 0.6576 0.025 Uiso 1 1 calc R . . C24 C 0.1012(3) -0.2601(2) 0.75512(19) 0.0201(6) Uani 1 1 d . . . H24A H 0.1040 -0.2050 0.7517 0.024 Uiso 1 1 calc R . . C20 C 0.0657(3) -0.36048(19) 0.82295(19) 0.0197(6) Uani 1 1 d . . . H20A H 0.0439 -0.3749 0.8659 0.024 Uiso 1 1 calc R . . C23 C 0.1246(3) -0.3210(2) 0.6949(2) 0.0221(6) Uani 1 1 d . . . H23A H 0.1436 -0.3073 0.6507 0.027 Uiso 1 1 calc R . . C26 C 0.2986(3) -0.4305(2) 0.9202(2) 0.0288(7) Uani 1 1 d . . . H26A H 0.3057 -0.3823 0.9031 0.035 Uiso 1 1 calc R . . C25 C 0.1963(3) -0.5112(2) 0.8663(2) 0.0251(7) Uani 1 1 d . . . C15 C 0.1430(3) -0.1576(2) 0.9771(2) 0.0228(6) Uani 1 1 d . . . H15A H 0.1135 -0.1072 0.9957 0.027 Uiso 1 1 calc R . . C27 C 0.3914(4) -0.4187(3) 0.9989(2) 0.0371(8) Uani 1 1 d . . . H27A H 0.4604 -0.3622 1.0360 0.045 Uiso 1 1 calc R . . C28 C 0.3842(4) -0.4884(3) 1.0237(2) 0.0406(9) Uani 1 1 d . . . H28A H 0.4481 -0.4797 1.0779 0.049 Uiso 1 1 calc R . . C29 C 0.2846(4) -0.5705(3) 0.9700(2) 0.0378(9) Uani 1 1 d . . . H29A H 0.2801 -0.6189 0.9867 0.045 Uiso 1 1 calc R . . C30 C 0.1911(4) -0.5824(2) 0.8915(2) 0.0318(8) Uani 1 1 d . . . H30A H 0.1227 -0.6392 0.8542 0.038 Uiso 1 1 calc R . . C31 C -0.0782(3) -0.5660(2) 0.7726(2) 0.0251(7) Uani 1 1 d . . . C35 C -0.1950(4) -0.5657(3) 0.8637(3) 0.0405(9) Uani 1 1 d . . . H35A H -0.1950 -0.5532 0.9202 0.049 Uiso 1 1 calc R . . C32 C -0.1949(4) -0.6032(3) 0.6995(3) 0.0409(9) Uani 1 1 d . . . H32A H -0.1963 -0.6171 0.6425 0.049 Uiso 1 1 calc R . . C34 C -0.3113(4) -0.6034(3) 0.7894(3) 0.0451(10) Uani 1 1 d . . . H34A H -0.3913 -0.6172 0.7948 0.054 Uiso 1 1 calc R . . C33 C -0.3112(4) -0.6205(3) 0.7086(3) 0.0499(11) Uani 1 1 d . . . H33A H -0.3912 -0.6446 0.6579 0.060 Uiso 1 1 calc R . . C36 C -0.0783(4) -0.5463(2) 0.8559(2) 0.0340(8) Uani 1 1 d . . . H36A H 0.0015 -0.5195 0.9072 0.041 Uiso 1 1 calc R . . C37 C -0.2128(3) -0.3141(2) 0.66527(19) 0.0207(6) Uani 1 1 d . . . C38 C -0.2299(3) -0.4044(2) 0.6407(2) 0.0247(7) Uani 1 1 d . . . H38A H -0.2571 -0.4348 0.6729 0.030 Uiso 1 1 calc R . . C39 C -0.2075(3) -0.4494(2) 0.5705(2) 0.0262(7) Uani 1 1 d . . . H39A H -0.2211 -0.5110 0.5539 0.031 Uiso 1 1 calc R . . C40 C -0.1657(3) -0.4063(2) 0.5238(2) 0.0242(7) Uani 1 1 d . . . H40A H -0.1526 -0.4386 0.4746 0.029 Uiso 1 1 calc R . . C41 C -0.1426(3) -0.31557(19) 0.54854(19) 0.0201(6) Uani 1 1 d . . . C42 C -0.1676(3) -0.2704(2) 0.61900(19) 0.0205(6) Uani 1 1 d . . . H42A H -0.1536 -0.2088 0.6357 0.025 Uiso 1 1 calc R . . C44 C 0.1105(3) -0.1216(2) 0.6437(2) 0.0308(8) Uani 1 1 d . . . H44A H 0.0452 -0.1239 0.6651 0.037 Uiso 1 1 calc R . . C45 C 0.2374(4) -0.0615(2) 0.6992(2) 0.0384(9) Uani 1 1 d . . . H45A H 0.2588 -0.0239 0.7586 0.046 Uiso 1 1 calc R . . C46 C 0.3317(4) -0.0566(2) 0.6684(3) 0.0401(9) Uani 1 1 d . . . H46A H 0.4188 -0.0168 0.7069 0.048 Uiso 1 1 calc R . . C48 C 0.1744(3) -0.1706(2) 0.5265(2) 0.0286(7) Uani 1 1 d . . . H48A H 0.1535 -0.2078 0.4671 0.034 Uiso 1 1 calc R . . C47 C 0.3003(3) -0.1093(2) 0.5816(3) 0.0355(8) Uani 1 1 d . . . H47A H 0.3649 -0.1036 0.5595 0.043 Uiso 1 1 calc R . . C43 C 0.0784(3) -0.1783(2) 0.5575(2) 0.0226(6) Uani 1 1 d . . . C52 C -0.3377(4) -0.1035(2) 0.4206(2) 0.0344(8) Uani 1 1 d . . . H52A H -0.3910 -0.0718 0.4047 0.041 Uiso 1 1 calc R . . C51 C -0.2097(4) -0.0733(2) 0.4333(2) 0.0328(8) Uani 1 1 d . . . H51A H -0.1745 -0.0203 0.4271 0.039 Uiso 1 1 calc R . . C49 C -0.1833(3) -0.1979(2) 0.46411(19) 0.0210(6) Uani 1 1 d . . . C50 C -0.1328(3) -0.1200(2) 0.4551(2) 0.0281(7) Uani 1 1 d . . . H50A H -0.0446 -0.0988 0.4641 0.034 Uiso 1 1 calc R . . C53 C -0.3877(4) -0.1792(2) 0.4309(3) 0.0367(8) Uani 1 1 d . . . H53A H -0.4749 -0.1988 0.4242 0.044 Uiso 1 1 calc R . . C54 C -0.3119(3) -0.2273(2) 0.4510(2) 0.0314(8) Uani 1 1 d . . . H54A H -0.3484 -0.2810 0.4559 0.038 Uiso 1 1 calc R . . C55 C -0.2292(4) -0.3610(2) 0.2893(2) 0.0296(7) Uani 1 1 d . . . C1S C -0.2706(5) -0.1810(4) 0.1930(4) 0.0744(15) Uani 1 1 d . . . H1SA H -0.2043 -0.1279 0.2470 0.089 Uiso 1 1 calc R . . H1SB H -0.2565 -0.2348 0.1977 0.089 Uiso 1 1 calc R . . Cl1S Cl -0.2510(2) -0.17270(12) 0.10269(13) 0.1091(6) Uani 1 1 d . . . Cl2S Cl -0.42465(12) -0.18811(9) 0.18673(9) 0.0718(4) Uani 1 1 d . . . C2S C 0.2008(4) -0.0304(4) 0.3475(3) 0.0625(13) Uani 1 1 d . . . H2SA H 0.1817 -0.0202 0.2932 0.075 Uiso 1 1 calc R . . H2SB H 0.2078 0.0234 0.3949 0.075 Uiso 1 1 calc R . . Cl3S Cl 0.34760(13) -0.04438(11) 0.37774(9) 0.0749(4) Uani 1 1 d . . . Cl4S Cl 0.07297(14) -0.12281(15) 0.32868(10) 0.1023(6) 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 Rh1 0.02516(13) 0.01936(12) 0.01683(12) 0.00632(9) 0.00898(10) 0.01076(10) Ti1 0.0226(3) 0.0211(3) 0.0195(3) 0.0068(2) 0.0099(2) 0.0110(2) P1 0.0235(4) 0.0180(4) 0.0182(4) 0.0071(3) 0.0087(3) 0.0095(3) Cl1 0.0375(5) 0.0369(5) 0.0296(4) 0.0089(4) 0.0190(4) 0.0205(4) O1 0.0436(16) 0.0583(18) 0.0310(14) 0.0139(13) 0.0135(13) 0.0294(14) N1 0.0191(13) 0.0225(13) 0.0217(13) 0.0092(11) 0.0090(10) 0.0071(11) C1 0.0215(17) 0.047(2) 0.037(2) 0.0226(17) 0.0120(15) 0.0145(16) Cl2 0.0349(4) 0.0213(4) 0.0270(4) 0.0092(3) 0.0125(3) 0.0116(3) N2 0.0237(13) 0.0178(12) 0.0171(12) 0.0057(10) 0.0099(10) 0.0086(11) C2 0.028(2) 0.068(3) 0.059(3) 0.036(2) 0.0209(19) 0.024(2) Cl3 0.0371(5) 0.0313(4) 0.0247(4) 0.0088(3) 0.0100(3) 0.0203(4) C3 0.0236(18) 0.055(2) 0.034(2) 0.0224(18) 0.0057(15) 0.0100(17) C4 0.034(2) 0.046(2) 0.049(2) 0.0273(19) 0.0195(18) 0.0237(18) C5 0.0196(16) 0.0363(18) 0.0271(17) 0.0141(15) 0.0115(13) 0.0106(14) C6 0.041(2) 0.087(3) 0.056(3) 0.047(3) 0.032(2) 0.028(2) P2 0.0267(4) 0.0178(4) 0.0178(4) 0.0066(3) 0.0107(3) 0.0094(3) C7 0.0267(18) 0.043(2) 0.0352(19) 0.0214(17) 0.0159(15) 0.0079(16) C8 0.0277(19) 0.046(2) 0.043(2) 0.0228(19) 0.0076(17) -0.0002(17) C9 0.034(2) 0.043(2) 0.037(2) 0.0254(18) 0.0171(16) 0.0105(17) C10 0.0260(18) 0.0242(17) 0.0342(19) 0.0075(14) 0.0139(15) 0.0049(14) C11 0.0285(19) 0.0337(19) 0.0297(19) 0.0028(15) 0.0054(15) 0.0049(16) C12 0.048(2) 0.042(2) 0.0234(18) 0.0091(16) 0.0175(17) 0.0172(18) C13 0.0233(16) 0.0248(16) 0.0234(16) 0.0061(13) 0.0071(13) 0.0074(13) C14 0.0247(17) 0.0311(18) 0.0310(18) 0.0083(15) 0.0098(14) 0.0103(15) C16 0.0311(18) 0.0310(18) 0.0233(16) 0.0109(14) 0.0134(14) 0.0143(15) C18 0.040(2) 0.041(2) 0.0303(19) 0.0185(16) 0.0140(16) 0.0212(17) C17 0.0346(19) 0.0335(19) 0.0269(17) 0.0135(15) 0.0180(15) 0.0136(15) C21 0.0221(16) 0.0192(15) 0.0199(15) 0.0071(12) 0.0085(12) 0.0077(12) C19 0.0167(14) 0.0185(14) 0.0180(14) 0.0052(12) 0.0061(11) 0.0058(12) C22 0.0229(16) 0.0203(15) 0.0171(14) 0.0039(12) 0.0094(12) 0.0081(13) C24 0.0180(15) 0.0194(15) 0.0212(15) 0.0092(12) 0.0062(12) 0.0063(12) C20 0.0227(15) 0.0204(15) 0.0175(14) 0.0082(12) 0.0106(12) 0.0071(12) C23 0.0233(16) 0.0257(16) 0.0183(15) 0.0109(13) 0.0100(12) 0.0073(13) C26 0.0269(17) 0.0310(18) 0.0298(18) 0.0113(15) 0.0137(14) 0.0129(15) C25 0.0285(17) 0.0271(17) 0.0208(16) 0.0086(13) 0.0125(13) 0.0116(14) C15 0.0243(16) 0.0197(15) 0.0207(15) 0.0054(12) 0.0083(13) 0.0082(13) C27 0.0298(19) 0.041(2) 0.0324(19) 0.0058(16) 0.0114(16) 0.0153(17) C28 0.036(2) 0.062(3) 0.0254(18) 0.0165(18) 0.0117(16) 0.026(2) C29 0.044(2) 0.055(2) 0.035(2) 0.0284(19) 0.0235(18) 0.029(2) C30 0.038(2) 0.0352(19) 0.0279(18) 0.0160(15) 0.0167(16) 0.0166(16) C31 0.0318(18) 0.0218(16) 0.0301(17) 0.0145(14) 0.0179(14) 0.0126(14) C35 0.047(2) 0.049(2) 0.050(2) 0.029(2) 0.035(2) 0.026(2) C32 0.032(2) 0.046(2) 0.034(2) 0.0100(17) 0.0142(16) 0.0060(17) C34 0.036(2) 0.041(2) 0.061(3) 0.018(2) 0.031(2) 0.0101(18) C33 0.029(2) 0.055(3) 0.048(2) 0.012(2) 0.0137(18) 0.0038(19) C36 0.040(2) 0.037(2) 0.0338(19) 0.0175(16) 0.0202(17) 0.0197(17) C37 0.0182(15) 0.0207(15) 0.0202(15) 0.0071(12) 0.0067(12) 0.0067(12) C38 0.0225(16) 0.0225(16) 0.0285(17) 0.0135(13) 0.0093(13) 0.0059(13) C39 0.0272(17) 0.0147(15) 0.0315(18) 0.0072(13) 0.0098(14) 0.0063(13) C40 0.0273(17) 0.0197(15) 0.0235(16) 0.0061(13) 0.0111(13) 0.0088(13) C41 0.0188(15) 0.0207(15) 0.0186(15) 0.0077(12) 0.0061(12) 0.0070(12) C42 0.0194(15) 0.0193(15) 0.0181(14) 0.0056(12) 0.0050(12) 0.0069(12) C44 0.038(2) 0.0248(17) 0.0246(17) 0.0120(14) 0.0116(15) 0.0049(15) C45 0.047(2) 0.0275(18) 0.0239(18) 0.0123(15) 0.0039(16) 0.0000(16) C46 0.0292(19) 0.034(2) 0.045(2) 0.0241(18) -0.0004(17) 0.0044(16) C48 0.0276(18) 0.0254(17) 0.0367(19) 0.0131(15) 0.0155(15) 0.0136(14) C47 0.0273(19) 0.0301(19) 0.054(2) 0.0227(18) 0.0164(17) 0.0133(15) C43 0.0253(16) 0.0199(15) 0.0228(16) 0.0107(13) 0.0075(13) 0.0103(13) C52 0.037(2) 0.037(2) 0.037(2) 0.0193(16) 0.0134(16) 0.0241(17) C51 0.039(2) 0.0288(18) 0.039(2) 0.0201(16) 0.0175(17) 0.0164(16) C49 0.0251(16) 0.0196(15) 0.0173(14) 0.0055(12) 0.0084(12) 0.0109(13) C50 0.0305(18) 0.0294(18) 0.0319(18) 0.0165(15) 0.0167(15) 0.0141(15) C53 0.0262(18) 0.038(2) 0.048(2) 0.0221(18) 0.0123(16) 0.0140(16) C54 0.0295(18) 0.0267(17) 0.0363(19) 0.0148(15) 0.0111(15) 0.0093(15) C55 0.038(2) 0.0260(17) 0.0248(17) 0.0067(14) 0.0162(16) 0.0143(15) C1S 0.061(3) 0.089(4) 0.078(4) 0.041(3) 0.026(3) 0.034(3) Cl1S 0.1546(18) 0.0875(11) 0.1199(14) 0.0549(11) 0.0941(14) 0.0387(12) Cl2S 0.0559(7) 0.0692(8) 0.0586(7) 0.0025(6) 0.0112(6) 0.0226(6) C2S 0.057(3) 0.092(4) 0.037(2) 0.019(2) 0.020(2) 0.036(3) Cl3S 0.0528(7) 0.1036(11) 0.0724(9) 0.0366(8) 0.0262(7) 0.0372(7) Cl4S 0.0550(8) 0.1871(19) 0.0596(8) 0.0592(11) 0.0283(7) 0.0225(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 Rh1 C55 1.813(4) . ? Rh1 P1 2.3218(8) . ? Rh1 P2 2.3374(8) 2_546 ? Rh1 Cl3 2.3678(8) . ? Ti1 N1 1.881(3) . ? Ti1 N2 1.889(3) . ? Ti1 Cl1 2.2410(9) . ? Ti1 Cl2 2.2760(10) . ? P1 C49 1.825(3) . ? P1 C43 1.830(3) . ? P1 C41 1.830(3) . ? O1 C55 1.116(4) . ? N1 C37 1.432(4) . ? N1 C5 1.513(4) . ? C1 C3 1.532(5) . ? C1 C4 1.538(5) . ? C1 C2 1.543(5) . ? C1 C5 1.573(5) . ? N2 C19 1.441(4) . ? N2 C15 1.510(4) . ? C5 C7 1.589(5) . ? C6 C7 1.544(5) . ? P2 C25 1.825(3) . ? P2 C21 1.826(3) . ? P2 C31 1.829(3) . ? P2 Rh1 2.3374(8) 2_546 ? C7 C9 1.534(5) . ? C7 C8 1.535(5) . ? C10 C13 1.527(5) . ? C11 C13 1.543(4) . ? C12 C16 1.539(5) . ? C13 C14 1.546(4) . ? C13 C15 1.578(4) . ? C16 C17 1.529(5) . ? C16 C18 1.534(5) . ? C16 C15 1.594(4) . ? C21 C22 1.397(4) . ? C21 C20 1.401(4) . ? C19 C20 1.390(4) . ? C19 C24 1.398(4) . ? C22 C23 1.382(4) . ? C24 C23 1.379(4) . ? C26 C25 1.375(5) . ? C26 C27 1.383(5) . ? C25 C30 1.406(5) . ? C27 C28 1.375(6) . ? C28 C29 1.376(6) . ? C29 C30 1.384(5) . ? C31 C32 1.375(5) . ? C31 C36 1.398(5) . ? C35 C34 1.381(6) . ? C35 C36 1.386(5) . ? C32 C33 1.392(5) . ? C34 C33 1.359(6) . ? C37 C42 1.396(4) . ? C37 C38 1.400(4) . ? C38 C39 1.374(5) . ? C39 C40 1.381(4) . ? C40 C41 1.393(4) . ? C41 C42 1.398(4) . ? C44 C43 1.387(4) . ? C44 C45 1.390(5) . ? C45 C46 1.371(6) . ? C46 C47 1.379(6) . ? C48 C47 1.387(5) . ? C48 C43 1.391(4) . ? C52 C53 1.369(5) . ? C52 C51 1.379(5) . ? C51 C50 1.382(5) . ? C49 C54 1.385(5) . ? C49 C50 1.389(4) . ? C53 C54 1.384(5) . ? C1S Cl1S 1.717(6) . ? C1S Cl2S 1.744(5) . ? C2S Cl3S 1.731(5) . ? C2S Cl4S 1.743(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C55 Rh1 P1 90.73(10) . . ? C55 Rh1 P2 91.42(10) . 2_546 ? P1 Rh1 P2 176.76(3) . 2_546 ? C55 Rh1 Cl3 172.37(11) . . ? P1 Rh1 Cl3 86.29(3) . . ? P2 Rh1 Cl3 91.88(3) 2_546 . ? N1 Ti1 N2 114.61(11) . . ? N1 Ti1 Cl1 110.96(8) . . ? N2 Ti1 Cl1 112.99(8) . . ? N1 Ti1 Cl2 105.73(8) . . ? N2 Ti1 Cl2 108.97(8) . . ? Cl1 Ti1 Cl2 102.58(4) . . ? C49 P1 C43 103.15(14) . . ? C49 P1 C41 103.99(14) . . ? C43 P1 C41 107.80(14) . . ? C49 P1 Rh1 116.99(10) . . ? C43 P1 Rh1 111.52(10) . . ? C41 P1 Rh1 112.53(10) . . ? C37 N1 C5 122.0(2) . . ? C37 N1 Ti1 117.78(19) . . ? C5 N1 Ti1 120.2(2) . . ? C3 C1 C4 108.7(3) . . ? C3 C1 C2 107.3(3) . . ? C4 C1 C2 105.9(3) . . ? C3 C1 C5 116.7(3) . . ? C4 C1 C5 107.5(3) . . ? C2 C1 C5 110.2(3) . . ? C19 N2 C15 121.9(2) . . ? C19 N2 Ti1 121.39(19) . . ? C15 N2 Ti1 116.22(18) . . ? N1 C5 C1 111.3(3) . . ? N1 C5 C7 114.8(3) . . ? C1 C5 C7 120.3(3) . . ? C25 P2 C21 105.05(14) . . ? C25 P2 C31 103.01(15) . . ? C21 P2 C31 101.73(14) . . ? C25 P2 Rh1 113.56(11) . 2_546 ? C21 P2 Rh1 115.11(10) . 2_546 ? C31 P2 Rh1 116.76(11) . 2_546 ? C9 C7 C8 109.8(3) . . ? C9 C7 C6 103.6(3) . . ? C8 C7 C6 107.8(3) . . ? C9 C7 C5 109.3(3) . . ? C8 C7 C5 116.2(3) . . ? C6 C7 C5 109.4(3) . . ? C10 C13 C11 105.7(3) . . ? C10 C13 C14 107.9(3) . . ? C11 C13 C14 107.7(3) . . ? C10 C13 C15 108.2(3) . . ? C11 C13 C15 110.1(3) . . ? C14 C13 C15 116.7(3) . . ? C17 C16 C18 107.7(3) . . ? C17 C16 C12 104.8(3) . . ? C18 C16 C12 107.9(3) . . ? C17 C16 C15 111.2(3) . . ? C18 C16 C15 115.4(3) . . ? C12 C16 C15 109.1(3) . . ? C22 C21 C20 119.8(3) . . ? C22 C21 P2 118.7(2) . . ? C20 C21 P2 121.4(2) . . ? C20 C19 C24 118.4(3) . . ? C20 C19 N2 123.9(3) . . ? C24 C19 N2 117.6(3) . . ? C23 C22 C21 119.5(3) . . ? C23 C24 C19 121.2(3) . . ? C19 C20 C21 120.6(3) . . ? C24 C23 C22 120.4(3) . . ? C25 C26 C27 120.7(3) . . ? C26 C25 C30 118.4(3) . . ? C26 C25 P2 123.3(3) . . ? C30 C25 P2 118.2(3) . . ? N2 C15 C13 112.6(2) . . ? N2 C15 C16 114.3(2) . . ? C13 C15 C16 119.2(3) . . ? C28 C27 C26 120.4(4) . . ? C27 C28 C29 120.1(3) . . ? C28 C29 C30 119.7(4) . . ? C29 C30 C25 120.6(3) . . ? C32 C31 C36 119.0(3) . . ? C32 C31 P2 119.3(3) . . ? C36 C31 P2 121.4(3) . . ? C34 C35 C36 120.2(4) . . ? C31 C32 C33 120.3(4) . . ? C33 C34 C35 119.8(4) . . ? C34 C33 C32 120.7(4) . . ? C35 C36 C31 120.0(4) . . ? C42 C37 C38 118.3(3) . . ? C42 C37 N1 120.0(3) . . ? C38 C37 N1 121.7(3) . . ? C39 C38 C37 120.5(3) . . ? C38 C39 C40 120.8(3) . . ? C39 C40 C41 120.3(3) . . ? C40 C41 C42 118.7(3) . . ? C40 C41 P1 117.1(2) . . ? C42 C41 P1 124.1(2) . . ? C37 C42 C41 121.3(3) . . ? C43 C44 C45 120.6(3) . . ? C46 C45 C44 120.0(3) . . ? C45 C46 C47 120.2(3) . . ? C47 C48 C43 120.6(3) . . ? C46 C47 C48 119.9(4) . . ? C44 C43 C48 118.5(3) . . ? C44 C43 P1 122.4(3) . . ? C48 C43 P1 119.0(2) . . ? C53 C52 C51 119.8(3) . . ? C52 C51 C50 120.1(3) . . ? C54 C49 C50 118.7(3) . . ? C54 C49 P1 121.2(2) . . ? C50 C49 P1 119.9(2) . . ? C51 C50 C49 120.5(3) . . ? C52 C53 C54 120.4(3) . . ? C53 C54 C49 120.4(3) . . ? O1 C55 Rh1 176.0(3) . . ? Cl1S C1S Cl2S 112.3(3) . . ? Cl3S C2S Cl4S 112.3(3) . . ? _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.791 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.084 data_may1501 _database_code_depnum_ccdc_archive 'CCDC 231687' _audit_creation_date 2001-05-11T11:29:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (PtCl2(P(C6H5)2(C6H4NHCHtBu2))2).2(CH2Cl2) _chemical_formula_moiety '(C54 H68 Cl2 N2 P2 Pt1).2(C1 H2 Cl2)' _chemical_formula_sum 'C56 H72 Cl6 N2 P2 Pt' _chemical_formula_weight 1242.89 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2195(6) _cell_length_b 14.8092(9) _cell_length_c 15.4020(11) _cell_angle_alpha 114.459(2) _cell_angle_beta 99.179(4) _cell_angle_gamma 95.075(4) _cell_volume 2871.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14284 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.952 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 19811 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_av_unetI/netI 0.1251 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.971 _reflns_number_total 9870 _reflns_number_gt 7288 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # 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^)+(0.0282P)^2^+11.2447P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 9870 _refine_ls_number_parameters 604 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.502 _refine_diff_density_min -1.367 _refine_diff_density_rms 0.16 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 Pt Pt 0.81155(2) 0.83393(2) 0.55650(3) 0.02221(11) Uani 1 1 d . A 1 Cl1 Cl 0.75500(14) 0.86080(16) 0.41711(16) 0.0308(5) Uani 1 1 d . A 1 Cl2 Cl 0.83174(16) 0.67414(15) 0.44912(17) 0.0362(5) Uani 1 1 d . A 1 P1 P 0.87619(14) 0.80574(16) 0.68453(17) 0.0251(5) Uani 1 1 d . A 1 P2 P 0.77963(14) 0.98990(16) 0.64393(17) 0.0231(5) Uani 1 1 d . A 1 N1 N 0.5309(5) 0.7950(5) 0.7420(6) 0.0358(19) Uani 1 1 d . A 1 H1 H 0.5232 0.8331 0.711 0.043 Uiso 1 1 calc R A 1 N2 N 0.4864(5) 1.1777(5) 0.7107(6) 0.0345(18) Uani 1 1 d . A 1 H2 H 0.4295 1.1825 0.6824 0.041 Uiso 1 1 calc R A 1 C1 C 0.9207(6) 0.6864(6) 0.6567(7) 0.034(2) Uani 1 1 d . A 1 C2 C 0.8529(7) 0.5995(7) 0.6256(8) 0.044(3) Uani 1 1 d . A 1 H2' H 0.7858 0.6029 0.6176 0.053 Uiso 1 1 calc R A 1 C3 C 0.8835(8) 0.5074(8) 0.6063(9) 0.059(3) Uani 1 1 d . A 1 H3 H 0.8373 0.448 0.5846 0.071 Uiso 1 1 calc R A 1 C4 C 0.9804(8) 0.5031(8) 0.6186(12) 0.091(5) Uani 1 1 d . A 1 H4 H 1.0019 0.4411 0.6079 0.109 Uiso 1 1 calc R A 1 C5 C 1.0461(8) 0.5888(8) 0.6466(11) 0.088(5) Uani 1 1 d . A 1 H5 H 1.1131 0.5852 0.6532 0.106 Uiso 1 1 calc R A 1 C6 C 1.0168(6) 0.6805(7) 0.6655(9) 0.058(3) Uani 1 1 d . A 1 H6 H 1.0633 0.7391 0.6845 0.07 Uiso 1 1 calc R A 1 C7 C 0.9842(5) 0.8997(6) 0.7562(6) 0.0255(19) Uani 1 1 d . A 1 C8 C 1.0137(6) 0.9406(6) 0.8568(7) 0.033(2) Uani 1 1 d . A 1 H8 H 0.9753 0.9214 0.8934 0.039 Uiso 1 1 calc R A 1 C9 C 1.0998(6) 1.0100(7) 0.9051(7) 0.038(2) Uani 1 1 d . A 1 H9 H 1.1201 1.0373 0.9741 0.045 Uiso 1 1 calc R A 1 C10 C 1.1548(6) 1.0382(7) 0.8517(8) 0.041(2) Uani 1 1 d . A 1 H10 H 1.2131 1.0856 0.8845 0.049 Uiso 1 1 calc R A 1 C11 C 1.1264(6) 0.9984(7) 0.7504(7) 0.037(2) Uani 1 1 d . A 1 H11 H 1.1643 1.0185 0.7139 0.044 Uiso 1 1 calc R A 1 C12 C 1.0416(5) 0.9289(6) 0.7042(7) 0.030(2) Uani 1 1 d . A 1 H12 H 1.0222 0.9005 0.635 0.035 Uiso 1 1 calc R A 1 C13 C 0.7924(5) 0.7987(6) 0.7604(6) 0.0262(19) Uani 1 1 d . A 1 C14 C 0.6962(5) 0.8017(5) 0.7290(6) 0.0226(18) Uani 1 1 d . A 1 H14 H 0.6783 0.8133 0.6729 0.027 Uiso 1 1 calc R A 1 C15 C 0.6244(6) 0.7881(6) 0.7776(6) 0.028(2) Uani 1 1 d . A 1 C16 C 0.6543(6) 0.7704(7) 0.8587(7) 0.036(2) Uani 1 1 d . A 1 H16 H 0.6081 0.7621 0.8942 0.043 Uiso 1 1 calc R A 1 C17 C 0.7488(6) 0.7645(7) 0.8886(7) 0.036(2) Uani 1 1 d . A 1 H17 H 0.7663 0.7502 0.9432 0.043 Uiso 1 1 calc R A 1 C18 C 0.8194(6) 0.7790(6) 0.8405(7) 0.031(2) Uani 1 1 d . A 1 H18 H 0.8848 0.7756 0.8621 0.037 Uiso 1 1 calc R A 1 C19 C 0.4438(6) 0.7430(7) 0.7524(7) 0.037(2) Uani 1 1 d . A 1 H19 H 0.4656 0.7244 0.8069 0.045 Uiso 1 1 calc R A 1 C20 C 0.4065(7) 0.6412(8) 0.6590(8) 0.054(3) Uani 1 1 d . A 1 C21 C 0.3643(14) 0.6494(11) 0.5659(12) 0.148(9) Uani 1 1 d . A 1 H21A H 0.4103 0.6953 0.5555 0.222 Uiso 1 1 calc R A 1 H21B H 0.3036 0.6756 0.5721 0.222 Uiso 1 1 calc R A 1 H21C H 0.3519 0.5828 0.5103 0.222 Uiso 1 1 calc R A 1 C22 C 0.4924(8) 0.5845(8) 0.6400(9) 0.060(3) Uani 1 1 d . A 1 H22A H 0.543 0.6245 0.6279 0.09 Uiso 1 1 calc R A 1 H22B H 0.4705 0.5193 0.5828 0.09 Uiso 1 1 calc R A 1 H22C H 0.5184 0.5738 0.6972 0.09 Uiso 1 1 calc R A 1 C23 C 0.3340(8) 0.5699(9) 0.6769(13) 0.101(6) Uani 1 1 d . A 1 H23A H 0.2756 0.5995 0.6889 0.152 Uiso 1 1 calc R A 1 H23B H 0.3636 0.5605 0.7338 0.152 Uiso 1 1 calc R A 1 H23C H 0.3167 0.5047 0.6192 0.152 Uiso 1 1 calc R A 1 C24 C 0.3757(6) 0.8216(9) 0.7902(8) 0.049(3) Uani 1 1 d . A 1 C25 C 0.3490(10) 0.8740(11) 0.7263(10) 0.091(5) Uani 1 1 d . A 1 H25A H 0.3136 0.8242 0.6614 0.137 Uiso 1 1 calc R A 1 H25B H 0.4079 0.9086 0.7204 0.137 Uiso 1 1 calc R A 1 H25C H 0.3082 0.9233 0.7558 0.137 Uiso 1 1 calc R A 1 C26 C 0.4296(8) 0.9046(8) 0.8887(10) 0.071(4) Uani 1 1 d . A 1 H26A H 0.4489 0.8751 0.9338 0.106 Uiso 1 1 calc R A 1 H26B H 0.3873 0.9533 0.9154 0.106 Uiso 1 1 calc R A 1 H26C H 0.4873 0.9388 0.8804 0.106 Uiso 1 1 calc R A 1 C27 C 0.2829(8) 0.7798(10) 0.8080(10) 0.076(4) Uani 1 1 d . A 1 H27A H 0.2448 0.7259 0.7465 0.115 Uiso 1 1 calc R A 1 H27B H 0.2452 0.8337 0.8331 0.115 Uiso 1 1 calc R A 1 H27C H 0.2988 0.7528 0.8558 0.115 Uiso 1 1 calc R A 1 C28 C 0.8320(6) 1.0778(6) 0.6026(6) 0.0251(19) Uani 1 1 d . A 1 C29 C 0.7805(6) 1.1450(6) 0.5798(7) 0.035(2) Uani 1 1 d . A 1 H29 H 0.7146 1.1446 0.5845 0.042 Uiso 1 1 calc R A 1 C30 C 0.8241(6) 1.2106(7) 0.5510(7) 0.040(2) Uani 1 1 d . A 1 H30 H 0.7876 1.2543 0.5346 0.049 Uiso 1 1 calc R A 1 C31 C 0.9206(7) 1.2148(7) 0.5452(7) 0.041(2) Uani 1 1 d . A 1 H31 H 0.9503 1.2609 0.5253 0.049 Uiso 1 1 calc R A 1 C32 C 0.9732(6) 1.1504(7) 0.5690(7) 0.036(2) Uani 1 1 d . A 1 H32 H 1.04 1.154 0.5677 0.043 Uiso 1 1 calc R A 1 C33 C 0.9286(6) 1.0812(7) 0.5946(7) 0.036(2) Uani 1 1 d . A 1 H33 H 0.9644 1.035 0.6069 0.043 Uiso 1 1 calc R A 1 C34 C 0.8199(6) 1.0577(6) 0.7772(6) 0.0273(19) Uani 1 1 d . A 1 C35 C 0.9068(6) 1.1257(6) 0.8211(7) 0.033(2) Uani 1 1 d . A 1 H35 H 0.948 1.1362 0.7821 0.039 Uiso 1 1 calc R A 1 C36 C 0.9327(7) 1.1778(7) 0.9219(7) 0.042(2) Uani 1 1 d . A 1 H36 H 0.9922 1.2236 0.9513 0.051 Uiso 1 1 calc R A 1 C37 C 0.8746(7) 1.1649(8) 0.9804(8) 0.046(3) Uani 1 1 d . A 1 H37 H 0.8932 1.2019 1.0494 0.055 Uiso 1 1 calc R A 1 C38 C 0.7892(7) 1.0977(7) 0.9379(7) 0.043(2) Uani 1 1 d . A 1 H38 H 0.7488 1.0877 0.9778 0.051 Uiso 1 1 calc R A 1 C39 C 0.7619(6) 1.0445(7) 0.8377(7) 0.036(2) Uani 1 1 d . A 1 H39 H 0.7027 0.9982 0.8093 0.043 Uiso 1 1 calc R A 1 C40 C 0.6500(5) 0.9916(6) 0.6272(6) 0.0235(19) Uani 1 1 d . A 1 C41 C 0.6191(5) 1.0822(6) 0.6802(6) 0.027(2) Uani 1 1 d . A 1 H41 H 0.6652 1.1395 0.7254 0.032 Uiso 1 1 calc R A 1 C42 C 0.5197(6) 1.0885(6) 0.6666(6) 0.0258(19) Uani 1 1 d . A 1 C43 C 0.4533(5) 1.0007(6) 0.6033(6) 0.0256(19) Uani 1 1 d . A 1 H43 H 0.3859 1.0022 0.5944 0.031 Uiso 1 1 calc R A 1 C44 C 0.4861(6) 0.9122(6) 0.5539(6) 0.028(2) Uani 1 1 d . A 1 H44 H 0.44 0.8537 0.5112 0.034 Uiso 1 1 calc R A 1 C45 C 0.5834(5) 0.9054(6) 0.5640(6) 0.0237(19) Uani 1 1 d . A 1 H45 H 0.604 0.8437 0.5289 0.028 Uiso 1 1 calc R A 1 C46 C 0.5371(6) 1.2649(6) 0.8003(7) 0.032(2) Uani 1 1 d . A 1 H46 H 0.605 1.2527 0.8127 0.038 Uiso 1 1 calc R A 1 C47 C 0.5443(7) 1.3592(7) 0.7764(8) 0.044(3) Uani 1 1 d . A 1 C48 C 0.5958(9) 1.4574(8) 0.8635(9) 0.075(4) Uani 1 1 d . A 1 H48A H 0.6592 1.448 0.891 0.112 Uiso 1 1 calc R A 1 H48B H 0.557 1.4765 0.9135 0.112 Uiso 1 1 calc R A 1 H48C H 0.6044 1.5107 0.842 0.112 Uiso 1 1 calc R A 1 C49 C 0.4457(9) 1.3757(9) 0.7336(11) 0.084(5) Uani 1 1 d . A 1 H49A H 0.412 1.3131 0.6775 0.126 Uiso 1 1 calc R A 1 H49B H 0.4553 1.4292 0.7125 0.126 Uiso 1 1 calc R A 1 H49C H 0.4068 1.3951 0.7835 0.126 Uiso 1 1 calc R A 1 C50 C 0.6052(9) 1.3368(9) 0.6976(9) 0.072(4) Uani 1 1 d . A 1 H50A H 0.6688 1.3258 0.7225 0.108 Uiso 1 1 calc R A 1 H50B H 0.6131 1.3941 0.6815 0.108 Uiso 1 1 calc R A 1 H50C H 0.5722 1.2763 0.6388 0.108 Uiso 1 1 calc R A 1 C51 C 0.4949(7) 1.2665(8) 0.8894(7) 0.045(3) Uani 1 1 d . A 1 C52 C 0.5651(9) 1.3358(10) 0.9864(9) 0.073(4) Uani 1 1 d . A 1 H52A H 0.6287 1.3153 0.9859 0.109 Uiso 1 1 calc R A 1 H52B H 0.5405 1.3308 1.0405 0.109 Uiso 1 1 calc R A 1 H52C H 0.5707 1.4055 0.9948 0.109 Uiso 1 1 calc R A 1 C53 C 0.3957(8) 1.2966(10) 0.8901(9) 0.078(4) Uani 1 1 d . A 1 H53A H 0.3997 1.365 0.8951 0.117 Uiso 1 1 calc R A 1 H53B H 0.373 1.2945 0.9462 0.117 Uiso 1 1 calc R A 1 H53C H 0.3503 1.2497 0.8296 0.117 Uiso 1 1 calc R A 1 C54 C 0.4859(11) 1.1610(9) 0.8826(10) 0.082(4) Uani 1 1 d . A 1 H54A H 0.5494 1.14 0.8828 0.124 Uiso 1 1 calc R A 1 H54B H 0.4404 1.1145 0.822 0.124 Uiso 1 1 calc R A 1 H54C H 0.4622 1.1601 0.9386 0.124 Uiso 1 1 calc R A 1 C55 C 0.8491(10) 0.6461(8) 0.2182(10) 0.080(4) Uani 1 1 d D B 2 H55A H 0.8095 0.679 0.266 0.096 Uiso 1 1 calc R B 2 H55B H 0.9135 0.6482 0.2553 0.096 Uiso 1 1 calc R B 2 Cl3 Cl 0.7949(3) 0.5215(3) 0.1468(4) 0.1180(15) Uani 1 1 d D B 2 Cl4 Cl 0.8626(3) 0.7134(3) 0.1509(3) 0.1024(13) Uani 1 1 d D B 2 C56 C 0.907(3) 0.4915(11) 0.929(2) 0.59(6) Uani 1 1 d D C 2 H56A H 0.8532 0.5069 0.9628 0.71 Uiso 1 1 calc R C 2 H56B H 0.9663 0.5001 0.977 0.71 Uiso 1 1 calc R C 2 Cl5 Cl 0.8812(4) 0.3717(4) 0.8398(6) 0.204(3) Uani 1 1 d D C 2 Cl6 Cl 0.9242(11) 0.5690(6) 0.8772(6) 0.333(7) Uani 1 1 d D C 2 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 Pt 0.01876(17) 0.02115(18) 0.0266(2) 0.00917(14) 0.00638(12) 0.00658(11) Cl1 0.0283(11) 0.0340(13) 0.0283(13) 0.0114(11) 0.0053(9) 0.0097(9) Cl2 0.0436(13) 0.0222(12) 0.0401(15) 0.0086(11) 0.0125(10) 0.0107(9) P1 0.0185(11) 0.0254(12) 0.0339(14) 0.0133(11) 0.0087(9) 0.0082(9) P2 0.0207(11) 0.0225(12) 0.0274(13) 0.0105(10) 0.0078(9) 0.0078(8) N1 0.030(4) 0.036(5) 0.055(6) 0.032(4) 0.009(4) 0.009(3) N2 0.030(4) 0.025(4) 0.041(5) 0.006(4) 0.007(3) 0.015(3) C1 0.036(5) 0.025(5) 0.041(6) 0.014(5) 0.006(4) 0.012(4) C2 0.034(5) 0.032(6) 0.064(8) 0.020(5) 0.004(5) 0.008(4) C3 0.052(7) 0.035(6) 0.079(9) 0.022(6) -0.007(6) 0.005(5) C4 0.058(8) 0.029(7) 0.167(16) 0.031(8) -0.001(8) 0.022(6) C5 0.034(6) 0.041(7) 0.160(15) 0.024(8) -0.008(7) 0.017(5) C6 0.025(6) 0.031(6) 0.112(11) 0.026(6) 0.006(5) 0.013(4) C7 0.026(5) 0.024(5) 0.030(5) 0.016(4) 0.003(4) 0.008(3) C8 0.028(5) 0.032(5) 0.042(6) 0.018(5) 0.009(4) 0.008(4) C9 0.038(5) 0.035(6) 0.029(6) 0.007(5) -0.002(4) 0.006(4) C10 0.023(5) 0.040(6) 0.057(8) 0.020(6) 0.003(5) 0.005(4) C11 0.029(5) 0.039(6) 0.050(7) 0.023(5) 0.014(4) 0.011(4) C12 0.022(4) 0.032(5) 0.026(5) 0.007(4) 0.002(4) 0.000(4) C13 0.023(5) 0.023(5) 0.034(6) 0.014(4) 0.009(4) 0.003(3) C14 0.021(4) 0.013(4) 0.029(5) 0.004(4) 0.008(4) 0.004(3) C15 0.025(5) 0.025(5) 0.033(6) 0.014(4) 0.007(4) 0.001(3) C16 0.030(5) 0.049(6) 0.028(6) 0.017(5) 0.009(4) -0.003(4) C17 0.038(5) 0.043(6) 0.035(6) 0.028(5) 0.002(4) 0.005(4) C18 0.027(5) 0.031(5) 0.041(6) 0.023(5) 0.004(4) 0.003(4) C19 0.022(5) 0.051(6) 0.051(7) 0.034(6) 0.005(4) 0.004(4) C20 0.045(6) 0.050(7) 0.061(8) 0.033(6) -0.022(5) -0.003(5) C21 0.210(19) 0.058(10) 0.110(15) 0.033(10) -0.105(13) -0.021(11) C22 0.062(7) 0.038(6) 0.065(9) 0.008(6) 0.018(6) -0.001(5) C23 0.037(7) 0.060(9) 0.218(19) 0.074(11) 0.024(9) 0.001(6) C24 0.024(5) 0.079(8) 0.068(8) 0.050(7) 0.017(5) 0.020(5) C25 0.115(11) 0.142(13) 0.096(11) 0.095(11) 0.076(9) 0.096(10) C26 0.052(7) 0.051(7) 0.098(11) 0.019(8) 0.024(7) 0.009(6) C27 0.054(8) 0.087(10) 0.076(10) 0.020(8) 0.034(7) 0.000(6) C28 0.028(5) 0.017(4) 0.022(5) 0.001(4) 0.004(4) 0.001(3) C29 0.028(5) 0.035(5) 0.049(7) 0.023(5) 0.014(4) 0.006(4) C30 0.042(6) 0.034(6) 0.052(7) 0.024(5) 0.010(5) 0.011(4) C31 0.051(6) 0.040(6) 0.037(6) 0.020(5) 0.015(5) -0.001(5) C32 0.031(5) 0.041(6) 0.039(6) 0.020(5) 0.011(4) 0.004(4) C33 0.020(5) 0.042(6) 0.052(7) 0.027(5) 0.006(4) 0.010(4) C34 0.028(5) 0.028(5) 0.032(5) 0.018(4) 0.006(4) 0.013(4) C35 0.035(5) 0.034(5) 0.028(6) 0.012(5) 0.006(4) 0.006(4) C36 0.040(6) 0.039(6) 0.031(6) 0.004(5) -0.006(4) 0.003(4) C37 0.055(7) 0.045(6) 0.031(6) 0.009(5) 0.007(5) 0.021(5) C38 0.058(7) 0.037(6) 0.025(6) 0.005(5) 0.006(5) 0.011(5) C39 0.037(5) 0.029(5) 0.042(6) 0.016(5) 0.008(4) 0.012(4) C40 0.024(4) 0.021(5) 0.036(5) 0.021(4) 0.008(4) 0.010(3) C41 0.020(4) 0.022(5) 0.033(5) 0.008(4) 0.005(4) 0.002(3) C42 0.026(5) 0.025(5) 0.027(5) 0.011(4) 0.009(4) 0.006(4) C43 0.015(4) 0.039(5) 0.030(5) 0.019(4) 0.009(4) 0.013(4) C44 0.032(5) 0.029(5) 0.026(5) 0.015(4) 0.005(4) 0.002(4) C45 0.018(4) 0.031(5) 0.031(5) 0.018(4) 0.011(3) 0.009(3) C46 0.031(5) 0.021(5) 0.033(6) 0.002(4) 0.006(4) 0.009(4) C47 0.050(6) 0.027(6) 0.040(7) 0.003(5) 0.007(5) 0.005(4) C48 0.100(10) 0.031(6) 0.071(10) 0.003(6) 0.021(7) -0.004(6) C49 0.077(9) 0.053(8) 0.137(14) 0.062(9) 0.000(8) 0.020(6) C50 0.099(10) 0.053(8) 0.065(9) 0.020(7) 0.039(8) 0.005(7) C51 0.053(6) 0.050(7) 0.038(6) 0.020(5) 0.025(5) 0.020(5) C52 0.081(9) 0.083(9) 0.045(8) 0.018(7) 0.008(6) 0.030(7) C53 0.057(8) 0.107(11) 0.071(10) 0.030(8) 0.038(7) 0.026(7) C54 0.138(13) 0.066(9) 0.067(10) 0.037(8) 0.057(9) 0.035(8) C55 0.087(9) 0.078(10) 0.061(9) 0.025(8) 0.007(7) -0.008(7) Cl3 0.129(4) 0.073(3) 0.128(4) 0.025(3) 0.029(3) -0.001(2) Cl4 0.070(2) 0.140(4) 0.130(4) 0.093(3) 0.025(2) 0.005(2) C56 0.37(5) 0.08(2) 1.20(16) 0.09(5) 0.39(8) -0.05(3) Cl5 0.152(5) 0.098(4) 0.297(9) 0.060(5) -0.049(5) 0.019(3) Cl6 0.69(2) 0.114(6) 0.152(7) 0.053(5) 0.003(10) 0.027(9) #----------------------------------------------------------------------------# # 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 Pt P1 2.254(2) . ? Pt P2 2.271(2) . ? Pt Cl2 2.334(2) . ? Pt Cl1 2.372(2) . ? P1 C13 1.822(8) . ? P1 C7 1.823(8) . ? P1 C1 1.834(8) . ? P2 C28 1.822(8) . ? P2 C40 1.824(7) . ? P2 C34 1.835(9) . ? N1 C15 1.384(10) . ? N1 C19 1.467(10) . ? N2 C42 1.379(10) . ? N2 C46 1.461(11) . ? C1 C6 1.365(12) . ? C1 C2 1.392(12) . ? C2 C3 1.395(13) . ? C3 C4 1.372(14) . ? C4 C5 1.371(15) . ? C5 C6 1.383(13) . ? C7 C8 1.383(12) . ? C7 C12 1.390(11) . ? C8 C9 1.401(12) . ? C9 C10 1.376(13) . ? C10 C11 1.393(13) . ? C11 C12 1.386(12) . ? C13 C14 1.386(11) . ? C13 C18 1.387(12) . ? C14 C15 1.406(10) . ? C15 C16 1.389(12) . ? C16 C17 1.372(12) . ? C17 C18 1.391(11) . ? C19 C20 1.563(14) . ? C19 C24 1.565(13) . ? C20 C21 1.521(17) . ? C20 C22 1.541(14) . ? C20 C23 1.546(15) . ? C24 C25 1.510(14) . ? C24 C27 1.520(13) . ? C24 C26 1.523(16) . ? C28 C33 1.398(11) . ? C28 C29 1.409(11) . ? C29 C30 1.366(12) . ? C30 C31 1.387(12) . ? C31 C32 1.390(12) . ? C32 C33 1.380(12) . ? C34 C35 1.396(12) . ? C34 C39 1.398(12) . ? C35 C36 1.384(12) . ? C36 C37 1.373(13) . ? C37 C38 1.374(13) . ? C38 C39 1.379(13) . ? C40 C45 1.392(11) . ? C40 C41 1.404(10) . ? C41 C42 1.411(11) . ? C42 C43 1.404(11) . ? C43 C44 1.382(11) . ? C44 C45 1.385(10) . ? C46 C51 1.577(12) . ? C46 C47 1.583(13) . ? C47 C48 1.528(14) . ? C47 C49 1.536(14) . ? C47 C50 1.545(14) . ? C51 C54 1.515(14) . ? C51 C53 1.517(14) . ? C51 C52 1.535(15) . ? C55 Cl4 1.727(11) . ? C55 Cl3 1.734(10) . ? C56 Cl6 1.664(18) . ? C56 Cl5 1.693(17) . ? 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 P1 Pt P2 97.16(8) . . ? P1 Pt Cl2 90.09(8) . . ? P2 Pt Cl2 172.57(8) . . ? P1 Pt Cl1 175.41(7) . . ? P2 Pt Cl1 85.51(8) . . ? Cl2 Pt Cl1 87.36(8) . . ? C13 P1 C7 111.7(4) . . ? C13 P1 C1 100.6(4) . . ? C7 P1 C1 103.0(4) . . ? C13 P1 Pt 114.6(3) . . ? C7 P1 Pt 109.3(3) . . ? C1 P1 Pt 117.0(3) . . ? C28 P2 C40 107.1(4) . . ? C28 P2 C34 102.7(4) . . ? C40 P2 C34 101.8(4) . . ? C28 P2 Pt 109.6(3) . . ? C40 P2 Pt 111.8(3) . . ? C34 P2 Pt 122.7(3) . . ? C15 N1 C19 124.3(7) . . ? C42 N2 C46 125.9(7) . . ? C6 C1 C2 119.7(8) . . ? C6 C1 P1 122.5(7) . . ? C2 C1 P1 117.9(6) . . ? C1 C2 C3 119.9(9) . . ? C4 C3 C2 119.8(10) . . ? C5 C4 C3 119.5(10) . . ? C4 C5 C6 121.2(10) . . ? C1 C6 C5 119.8(9) . . ? C8 C7 C12 118.6(8) . . ? C8 C7 P1 124.9(6) . . ? C12 C7 P1 116.5(7) . . ? C7 C8 C9 120.7(8) . . ? C10 C9 C8 119.4(9) . . ? C9 C10 C11 121.0(9) . . ? C12 C11 C10 118.5(8) . . ? C11 C12 C7 121.8(9) . . ? C14 C13 C18 119.7(7) . . ? C14 C13 P1 117.7(6) . . ? C18 C13 P1 122.1(6) . . ? C13 C14 C15 122.1(8) . . ? N1 C15 C16 125.7(7) . . ? N1 C15 C14 117.7(8) . . ? C16 C15 C14 116.6(7) . . ? C17 C16 C15 121.7(8) . . ? C16 C17 C18 121.2(8) . . ? C13 C18 C17 118.6(7) . . ? N1 C19 C20 109.3(8) . . ? N1 C19 C24 107.9(7) . . ? C20 C19 C24 121.2(8) . . ? C21 C20 C22 107.5(12) . . ? C21 C20 C23 109.8(11) . . ? C22 C20 C23 103.4(8) . . ? C21 C20 C19 116.0(9) . . ? C22 C20 C19 107.8(7) . . ? C23 C20 C19 111.5(10) . . ? C25 C24 C27 108.0(9) . . ? C25 C24 C26 105.5(11) . . ? C27 C24 C26 105.9(9) . . ? C25 C24 C19 114.4(8) . . ? C27 C24 C19 114.4(9) . . ? C26 C24 C19 107.9(8) . . ? C33 C28 C29 117.5(7) . . ? C33 C28 P2 119.2(6) . . ? C29 C28 P2 123.3(6) . . ? C30 C29 C28 120.8(8) . . ? C29 C30 C31 121.2(9) . . ? C30 C31 C32 118.9(8) . . ? C33 C32 C31 120.1(8) . . ? C32 C33 C28 121.4(8) . . ? C35 C34 C39 118.1(8) . . ? C35 C34 P2 121.6(6) . . ? C39 C34 P2 120.2(7) . . ? C36 C35 C34 119.6(8) . . ? C37 C36 C35 121.7(9) . . ? C36 C37 C38 119.1(10) . . ? C37 C38 C39 120.4(10) . . ? C38 C39 C34 121.1(9) . . ? C45 C40 C41 120.8(7) . . ? C45 C40 P2 121.0(6) . . ? C41 C40 P2 118.2(6) . . ? C40 C41 C42 120.3(8) . . ? N2 C42 C43 119.3(7) . . ? N2 C42 C41 122.4(8) . . ? C43 C42 C41 118.2(7) . . ? C44 C43 C42 120.0(7) . . ? C43 C44 C45 122.6(8) . . ? C44 C45 C40 118.0(7) . . ? N2 C46 C51 109.9(7) . . ? N2 C46 C47 107.3(7) . . ? C51 C46 C47 121.5(7) . . ? C48 C47 C49 108.8(9) . . ? C48 C47 C50 107.1(9) . . ? C49 C47 C50 107.2(10) . . ? C48 C47 C46 113.8(9) . . ? C49 C47 C46 113.2(8) . . ? C50 C47 C46 106.3(8) . . ? C54 C51 C53 107.9(10) . . ? C54 C51 C52 107.0(10) . . ? C53 C51 C52 109.8(9) . . ? C54 C51 C46 107.6(8) . . ? C53 C51 C46 113.6(9) . . ? C52 C51 C46 110.7(9) . . ? Cl4 C55 Cl3 113.2(8) . . ? Cl6 C56 Cl5 108.5(16) . . ? #===END data_sep2401 _database_code_depnum_ccdc_archive 'CCDC 231688' _audit_creation_date 2001-10-01T13:49:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[PtCl2{PPh2C6H4NCHtBu2}2TiCl2].4(CH2Cl2)' ; _chemical_formula_moiety ; '(C54 H66 Cl4 N2 P2 Pd1 Ti1).4(C1 H2 Cl2)' ; _chemical_formula_sum 'C58 H74 Cl12 N2 P2 Pd Ti' _chemical_formula_weight 1440.83 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9191(7) _cell_length_b 16.3451(5) _cell_length_c 16.8451(8) _cell_angle_alpha 83.180(3) _cell_angle_beta 67.379(2) _cell_angle_gamma 67.954(3) _cell_volume 3277.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13963 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.887 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 20373 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_unetI/netI 0.0673 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 11513 _reflns_number_gt 8750 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Bond length constraints (SADI) wre applied to the dichloromethane solvate molecules. 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^)+(0.1211P)^2^+14.6705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 11513 _refine_ls_number_parameters 686 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.101 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2263 _refine_ls_wR_factor_gt 0.2059 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.736 _refine_diff_density_min -1.703 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' 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 Pd Pd 0.55823(4) 0.72975(3) 0.57033(3) 0.03121(18) Uani 1 1 d . . . Ti Ti 0.48562(9) 0.75070(7) 1.04530(7) 0.0295(3) Uani 1 1 d . . . Cl1 Cl 0.46206(16) 0.64047(12) 1.13536(12) 0.0533(5) Uani 1 1 d . . . Cl2 Cl 0.48796(16) 0.84979(12) 1.12703(12) 0.0476(4) Uani 1 1 d . . . Cl3 Cl 0.70274(16) 0.62456(13) 0.46547(12) 0.0503(5) Uani 1 1 d . . . Cl4 Cl 0.44345(18) 0.75253(15) 0.49354(14) 0.0595(5) Uani 1 1 d . . . P1 P 0.41110(14) 0.82195(10) 0.67716(10) 0.0293(4) Uani 1 1 d . . . P2 P 0.69573(14) 0.71149(10) 0.62089(10) 0.0304(4) Uani 1 1 d . . . N1 N 0.3618(4) 0.8030(3) 1.0106(3) 0.0257(11) Uani 1 1 d . . . N2 N 0.6252(4) 0.7073(3) 0.9545(3) 0.0259(11) Uani 1 1 d . . . C1 C 0.4055(5) 0.7704(4) 0.7805(4) 0.0301(13) Uani 1 1 d . . . C2 C 0.3820(5) 0.8123(4) 0.8561(4) 0.0267(13) Uani 1 1 d . . . H2 H 0.3682 0.8738 0.8567 0.032 Uiso 1 1 calc R . . C3 C 0.3783(5) 0.7654(4) 0.9314(4) 0.0267(13) Uani 1 1 d . . . C4 C 0.4015(5) 0.6746(4) 0.9285(4) 0.0320(14) Uani 1 1 d . . . H4 H 0.4015 0.6416 0.9789 0.038 Uiso 1 1 calc R . . C5 C 0.4246(5) 0.6319(4) 0.8530(4) 0.0331(14) Uani 1 1 d . . . H5 H 0.4393 0.5703 0.8519 0.04 Uiso 1 1 calc R . . C6 C 0.4261(5) 0.6798(4) 0.7795(4) 0.0340(14) Uani 1 1 d . . . H6 H 0.4411 0.6511 0.7279 0.041 Uiso 1 1 calc R . . C7 C 0.4123(5) 0.9331(4) 0.6770(4) 0.0320(14) Uani 1 1 d . . . C8 C 0.3302(6) 0.9963(4) 0.7396(5) 0.0442(17) Uani 1 1 d . . . H8 H 0.2725 0.9817 0.7841 0.053 Uiso 1 1 calc R . . C9 C 0.3323(8) 1.0809(5) 0.7372(6) 0.056(2) Uani 1 1 d . . . H9 H 0.2784 1.1233 0.7815 0.067 Uiso 1 1 calc R . . C10 C 0.4139(8) 1.1032(5) 0.6696(6) 0.056(2) Uani 1 1 d . . . H10 H 0.4151 1.1612 0.6674 0.067 Uiso 1 1 calc R . . C11 C 0.4923(7) 1.0417(5) 0.6063(5) 0.0478(19) Uani 1 1 d . . . H11 H 0.5473 1.0575 0.56 0.057 Uiso 1 1 calc R . . C12 C 0.4923(6) 0.9571(4) 0.6093(5) 0.0386(15) Uani 1 1 d . . . H12 H 0.547 0.915 0.565 0.046 Uiso 1 1 calc R . . C13 C 0.2708(6) 0.8447(4) 0.6786(4) 0.0351(14) Uani 1 1 d . . . C14 C 0.2053(7) 0.7994(6) 0.7304(6) 0.053(2) Uani 1 1 d . . . H14 H 0.2312 0.7563 0.7679 0.064 Uiso 1 1 calc R . . C15 C 0.0996(8) 0.8173(7) 0.7277(7) 0.071(3) Uani 1 1 d . . . H15 H 0.0545 0.7853 0.7627 0.085 Uiso 1 1 calc R . . C16 C 0.0610(7) 0.8807(6) 0.6747(6) 0.060(2) Uani 1 1 d . . . H16 H -0.0115 0.8943 0.6746 0.072 Uiso 1 1 calc R . . C17 C 0.1282(7) 0.9243(6) 0.6220(6) 0.057(2) Uani 1 1 d . . . H17 H 0.1035 0.9662 0.5834 0.068 Uiso 1 1 calc R . . C18 C 0.2309(7) 0.9075(5) 0.6249(5) 0.0519(19) Uani 1 1 d . . . H18 H 0.2756 0.9395 0.5894 0.062 Uiso 1 1 calc R . . C19 C 0.2516(5) 0.8691(4) 1.0672(4) 0.0354(15) Uani 1 1 d . . . H19 H 0.2639 0.8686 1.122 0.043 Uiso 1 1 calc R . . C20 C 0.2321(5) 0.9686(4) 1.0395(4) 0.0359(15) Uani 1 1 d . . . C21 C 0.1761(7) 1.0277(5) 1.1220(5) 0.055(2) Uani 1 1 d . . . H21A H 0.163 1.0895 1.1062 0.082 Uiso 1 1 calc R . . H21B H 0.225 1.0099 1.155 0.082 Uiso 1 1 calc R . . H21C H 0.1048 1.021 1.1571 0.082 Uiso 1 1 calc R . . C22 C 0.1592(7) 1.0032(5) 0.9856(6) 0.055(2) Uani 1 1 d . . . H22A H 0.152 1.0645 0.9709 0.083 Uiso 1 1 calc R . . H22B H 0.0851 1.0006 1.0186 0.083 Uiso 1 1 calc R . . H22C H 0.1936 0.9669 0.9327 0.083 Uiso 1 1 calc R . . C23 C 0.3431(6) 0.9831(4) 0.9900(4) 0.0371(15) Uani 1 1 d . . . H23A H 0.3895 0.9643 1.025 0.056 Uiso 1 1 calc R . . H23B H 0.3279 1.0459 0.9777 0.056 Uiso 1 1 calc R . . H23C H 0.3824 0.9483 0.9358 0.056 Uiso 1 1 calc R . . C24 C 0.1546(6) 0.8323(4) 1.0957(5) 0.0412(17) Uani 1 1 d . . . C25 C 0.1219(6) 0.8162(5) 1.0219(5) 0.0487(18) Uani 1 1 d . . . H25A H 0.0603 0.7941 1.046 0.073 Uiso 1 1 calc R . . H25B H 0.1863 0.7726 0.9802 0.073 Uiso 1 1 calc R . . H25C H 0.0985 0.8718 0.9932 0.073 Uiso 1 1 calc R . . C26 C 0.0477(6) 0.8940(5) 1.1632(5) 0.055(2) Uani 1 1 d . . . H26A H 0.0637 0.9028 1.2126 0.082 Uiso 1 1 calc R . . H26B H -0.0098 0.8674 1.1821 0.082 Uiso 1 1 calc R . . H26C H 0.0209 0.9511 1.1377 0.082 Uiso 1 1 calc R . . C27 C 0.1892(6) 0.7437(5) 1.1387(5) 0.0487(19) Uani 1 1 d . . . H27A H 0.129 0.7202 1.157 0.073 Uiso 1 1 calc R . . H27B H 0.2037 0.7524 1.189 0.073 Uiso 1 1 calc R . . H27C H 0.2569 0.702 1.0977 0.073 Uiso 1 1 calc R . . C28 C 0.6634(5) 0.7621(4) 0.7237(4) 0.0271(13) Uani 1 1 d . . . C29 C 0.6584(5) 0.7139(4) 0.7980(4) 0.0262(12) Uani 1 1 d . . . H29 H 0.6728 0.6525 0.7955 0.031 Uiso 1 1 calc R . . C30 C 0.6329(5) 0.7533(4) 0.8758(4) 0.0255(12) Uani 1 1 d . . . C31 C 0.6084(5) 0.8448(4) 0.8787(4) 0.0291(13) Uani 1 1 d . . . H31 H 0.5892 0.8734 0.9315 0.035 Uiso 1 1 calc R . . C32 C 0.6120(5) 0.8938(4) 0.8047(4) 0.0306(14) Uani 1 1 d . . . H32 H 0.5939 0.9558 0.8076 0.037 Uiso 1 1 calc R . . C33 C 0.6413(5) 0.8534(4) 0.7283(4) 0.0300(13) Uani 1 1 d . . . H33 H 0.6469 0.887 0.6777 0.036 Uiso 1 1 calc R . . C34 C 0.7761(6) 0.5951(4) 0.6300(4) 0.0357(15) Uani 1 1 d . . . C35 C 0.7170(7) 0.5387(5) 0.6663(5) 0.0483(18) Uani 1 1 d . . . H35 H 0.638 0.5608 0.684 0.058 Uiso 1 1 calc R . . C36 C 0.7740(8) 0.4493(5) 0.6769(6) 0.058(2) Uani 1 1 d . . . H36 H 0.7336 0.4111 0.7024 0.07 Uiso 1 1 calc R . . C37 C 0.8873(8) 0.4175(5) 0.6505(5) 0.057(2) Uani 1 1 d . . . H37 H 0.9259 0.3569 0.6571 0.068 Uiso 1 1 calc R . . C38 C 0.9460(7) 0.4722(6) 0.6143(5) 0.060(2) Uani 1 1 d . . . H38 H 1.025 0.4489 0.5957 0.073 Uiso 1 1 calc R . . C39 C 0.8903(7) 0.5630(5) 0.6044(5) 0.0478(18) Uani 1 1 d . . . H39 H 0.9312 0.601 0.5805 0.057 Uiso 1 1 calc R . . C40 C 0.7913(6) 0.7624(4) 0.5456(4) 0.0375(15) Uani 1 1 d . . . C41 C 0.7818(6) 0.7932(5) 0.4678(5) 0.0438(17) Uani 1 1 d . . . H41 H 0.7253 0.7876 0.4529 0.053 Uiso 1 1 calc R . . C42 C 0.8544(8) 0.8323(5) 0.4113(5) 0.060(2) Uani 1 1 d . . . H42 H 0.8463 0.8545 0.3586 0.072 Uiso 1 1 calc R . . C43 C 0.9376(8) 0.8387(6) 0.4318(6) 0.064(3) Uani 1 1 d . . . H43 H 0.9879 0.8643 0.3925 0.077 Uiso 1 1 calc R . . C44 C 0.9495(7) 0.8081(6) 0.5095(6) 0.059(2) Uani 1 1 d . . . H44 H 1.0073 0.8127 0.5234 0.071 Uiso 1 1 calc R . . C45 C 0.8751(6) 0.7708(5) 0.5666(5) 0.0468(18) Uani 1 1 d . . . H45 H 0.8814 0.7508 0.6203 0.056 Uiso 1 1 calc R . . C46 C 0.7258(5) 0.6377(4) 0.9683(4) 0.0309(13) Uani 1 1 d . . . H46 H 0.6987 0.632 1.0322 0.037 Uiso 1 1 calc R . . C47 C 0.7550(5) 0.5411(4) 0.9345(4) 0.0327(14) Uani 1 1 d . . . C48 C 0.7882(7) 0.4734(4) 1.0018(5) 0.0483(19) Uani 1 1 d . . . H48A H 0.8576 0.4732 1.004 0.072 Uiso 1 1 calc R . . H48B H 0.7991 0.4142 0.9849 0.072 Uiso 1 1 calc R . . H48C H 0.7286 0.4901 1.0586 0.072 Uiso 1 1 calc R . . C49 C 0.8477(6) 0.5117(5) 0.8461(5) 0.0460(18) Uani 1 1 d . . . H49A H 0.8237 0.5483 0.8019 0.069 Uiso 1 1 calc R . . H49B H 0.8634 0.4497 0.8345 0.069 Uiso 1 1 calc R . . H49C H 0.9152 0.5182 0.8454 0.069 Uiso 1 1 calc R . . C50 C 0.6515(6) 0.5288(4) 0.9311(5) 0.0379(15) Uani 1 1 d . . . H50A H 0.6703 0.4668 0.9171 0.057 Uiso 1 1 calc R . . H50B H 0.6285 0.5663 0.887 0.057 Uiso 1 1 calc R . . H50C H 0.5903 0.5454 0.9872 0.057 Uiso 1 1 calc R . . C51 C 0.8223(6) 0.6729(4) 0.9497(5) 0.0403(16) Uani 1 1 d . . . C52 C 0.8794(6) 0.6956(5) 0.8549(5) 0.051(2) Uani 1 1 d . . . H52A H 0.9415 0.7129 0.8504 0.077 Uiso 1 1 calc R . . H52B H 0.825 0.7445 0.8374 0.077 Uiso 1 1 calc R . . H52C H 0.9076 0.6438 0.8173 0.077 Uiso 1 1 calc R . . C53 C 0.9143(7) 0.6066(5) 0.9794(6) 0.053(2) Uani 1 1 d . . . H53A H 0.8815 0.5951 1.0405 0.08 Uiso 1 1 calc R . . H53B H 0.9715 0.6315 0.9709 0.08 Uiso 1 1 calc R . . H53C H 0.9483 0.5512 0.9456 0.08 Uiso 1 1 calc R . . C54 C 0.7762(7) 0.7569(5) 1.0054(6) 0.052(2) Uani 1 1 d . . . H54A H 0.7212 0.8038 0.9866 0.077 Uiso 1 1 calc R . . H54B H 0.8374 0.776 0.9994 0.077 Uiso 1 1 calc R . . H54C H 0.7405 0.7445 1.0658 0.077 Uiso 1 1 calc R . . C55 C 0.8272(9) 0.6317(13) 1.2430(9) 0.222(14) Uani 1 1 d D A 1 H55A H 0.8683 0.5717 1.2159 0.266 Uiso 1 1 calc R A 1 H55B H 0.814 0.6268 1.3051 0.266 Uiso 1 1 calc R A 1 C56 C 1.2976(9) 0.8706(7) 0.3615(7) 0.082(3) Uani 1 1 d D B 1 H56A H 1.3743 0.8599 0.3193 0.099 Uiso 1 1 calc R B 1 H56B H 1.3031 0.8378 0.4139 0.099 Uiso 1 1 calc R B 1 C57 C 1.2342(18) 0.5960(13) 0.5714(15) 0.51(5) Uani 1 1 d D C 1 H57A H 1.2673 0.538 0.541 0.613 Uiso 1 1 calc R C 1 H57B H 1.2812 0.5963 0.6029 0.613 Uiso 1 1 calc R C 1 C58 C 0.455(2) 0.4458(14) 0.6673(14) 0.33(2) Uani 1 1 d D D 1 H58A H 0.5024 0.4122 0.6999 0.395 Uiso 1 1 calc R D 1 H58B H 0.4434 0.4039 0.637 0.395 Uiso 1 1 calc R D 1 Cl5 Cl 0.6966(4) 0.6800(3) 1.2279(3) 0.1363(15) Uani 1 1 d D A 1 Cl6 Cl 0.9072(3) 0.7015(2) 1.1940(3) 0.1078(11) Uani 1 1 d D A 1 Cl7 Cl 1.2267(3) 0.8319(4) 0.3182(3) 0.1354(16) Uani 1 1 d D B 1 Cl8 Cl 1.2285(3) 0.9843(2) 0.3877(3) 0.1176(12) Uani 1 1 d D B 1 Cl9 Cl 1.1011(4) 0.6096(3) 0.6442(4) 0.1538(19) Uani 1 1 d D C 1 Cl10 Cl 1.2335(5) 0.6787(4) 0.4968(7) 0.270(5) Uani 1 1 d D C 1 Cl11 Cl 0.5127(5) 0.5162(5) 0.5953(5) 0.224(4) Uani 1 1 d D D 1 Cl12 Cl 0.3169(11) 0.5256(6) 0.7404(6) 0.326(7) Uani 1 1 d D D 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 Pd 0.0369(3) 0.0317(3) 0.0263(3) 0.00054(19) -0.0115(2) -0.0137(2) Ti 0.0315(6) 0.0254(6) 0.0256(6) 0.0014(4) -0.0082(5) -0.0066(5) Cl1 0.0513(11) 0.0455(10) 0.0429(10) 0.0187(8) -0.0069(8) -0.0120(8) Cl2 0.0517(11) 0.0468(10) 0.0403(10) -0.0128(8) -0.0170(8) -0.0093(8) Cl3 0.0506(11) 0.0557(11) 0.0385(10) -0.0157(8) -0.0119(8) -0.0125(9) Cl4 0.0577(12) 0.0774(14) 0.0503(12) -0.0066(10) -0.0327(10) -0.0161(10) P1 0.0321(9) 0.0271(8) 0.0285(8) 0.0042(6) -0.0105(7) -0.0122(7) P2 0.0326(9) 0.0297(8) 0.0265(8) 0.0000(6) -0.0093(7) -0.0099(7) N1 0.029(3) 0.017(2) 0.027(3) 0.0017(19) -0.006(2) -0.0081(19) N2 0.031(3) 0.019(2) 0.027(3) 0.0023(19) -0.012(2) -0.007(2) C1 0.031(3) 0.027(3) 0.030(3) 0.004(2) -0.010(3) -0.011(3) C2 0.021(3) 0.020(3) 0.034(3) 0.001(2) -0.008(3) -0.004(2) C3 0.025(3) 0.022(3) 0.030(3) 0.000(2) -0.009(3) -0.005(2) C4 0.033(3) 0.026(3) 0.034(3) 0.008(3) -0.009(3) -0.014(3) C5 0.041(4) 0.019(3) 0.037(4) 0.001(2) -0.013(3) -0.011(3) C6 0.039(4) 0.028(3) 0.036(4) -0.002(3) -0.014(3) -0.013(3) C7 0.038(4) 0.028(3) 0.036(4) 0.008(3) -0.020(3) -0.014(3) C8 0.052(4) 0.033(4) 0.045(4) 0.007(3) -0.019(4) -0.013(3) C9 0.074(6) 0.035(4) 0.057(5) 0.003(3) -0.031(5) -0.011(4) C10 0.082(6) 0.037(4) 0.060(5) 0.020(4) -0.033(5) -0.031(4) C11 0.065(5) 0.041(4) 0.052(5) 0.022(3) -0.032(4) -0.031(4) C12 0.048(4) 0.038(4) 0.040(4) 0.013(3) -0.024(3) -0.022(3) C13 0.037(4) 0.037(3) 0.037(4) -0.002(3) -0.016(3) -0.016(3) C14 0.046(5) 0.062(5) 0.059(5) 0.014(4) -0.020(4) -0.030(4) C15 0.054(5) 0.085(7) 0.082(7) 0.011(5) -0.020(5) -0.040(5) C16 0.033(4) 0.072(6) 0.071(6) -0.017(5) -0.020(4) -0.009(4) C17 0.050(5) 0.065(5) 0.058(5) -0.002(4) -0.030(4) -0.013(4) C18 0.045(4) 0.055(5) 0.059(5) 0.010(4) -0.028(4) -0.017(4) C19 0.035(4) 0.025(3) 0.035(4) -0.001(3) -0.005(3) -0.005(3) C20 0.034(4) 0.021(3) 0.042(4) 0.000(3) -0.010(3) -0.003(3) C21 0.063(5) 0.033(4) 0.045(4) -0.008(3) 0.001(4) -0.011(3) C22 0.040(4) 0.043(4) 0.065(5) 0.012(4) -0.015(4) -0.006(3) C23 0.042(4) 0.019(3) 0.043(4) 0.001(3) -0.012(3) -0.008(3) C24 0.032(4) 0.032(3) 0.048(4) 0.003(3) -0.005(3) -0.010(3) C25 0.037(4) 0.048(4) 0.057(5) -0.001(3) -0.014(4) -0.014(3) C26 0.037(4) 0.049(4) 0.053(5) -0.003(4) 0.007(4) -0.012(3) C27 0.047(4) 0.038(4) 0.049(4) 0.007(3) -0.004(4) -0.020(3) C28 0.025(3) 0.026(3) 0.027(3) 0.000(2) -0.008(2) -0.007(2) C29 0.025(3) 0.023(3) 0.030(3) -0.002(2) -0.008(3) -0.008(2) C30 0.024(3) 0.019(3) 0.031(3) 0.004(2) -0.010(3) -0.006(2) C31 0.029(3) 0.027(3) 0.031(3) 0.002(2) -0.009(3) -0.012(2) C32 0.036(3) 0.020(3) 0.038(4) 0.006(2) -0.017(3) -0.011(2) C33 0.034(3) 0.026(3) 0.031(3) 0.006(2) -0.016(3) -0.010(3) C34 0.042(4) 0.030(3) 0.029(3) -0.005(3) -0.012(3) -0.005(3) C35 0.053(5) 0.034(4) 0.057(5) -0.001(3) -0.019(4) -0.015(3) C36 0.072(6) 0.026(4) 0.071(6) -0.001(4) -0.022(5) -0.014(4) C37 0.078(6) 0.027(4) 0.047(5) -0.007(3) -0.021(4) 0.002(4) C38 0.049(5) 0.060(5) 0.044(5) -0.012(4) -0.016(4) 0.013(4) C39 0.051(5) 0.040(4) 0.038(4) 0.001(3) -0.012(3) -0.005(3) C40 0.040(4) 0.033(3) 0.035(4) 0.001(3) -0.008(3) -0.014(3) C41 0.047(4) 0.047(4) 0.034(4) 0.001(3) -0.009(3) -0.018(3) C42 0.067(6) 0.054(5) 0.045(5) 0.012(4) -0.005(4) -0.025(4) C43 0.055(5) 0.056(5) 0.060(6) 0.003(4) 0.008(4) -0.028(4) C44 0.042(5) 0.060(5) 0.067(6) -0.002(4) -0.005(4) -0.024(4) C45 0.039(4) 0.048(4) 0.048(4) -0.003(3) -0.011(3) -0.013(3) C46 0.034(3) 0.026(3) 0.033(3) 0.005(2) -0.017(3) -0.007(3) C47 0.037(4) 0.021(3) 0.039(4) 0.005(3) -0.018(3) -0.005(3) C48 0.060(5) 0.026(3) 0.064(5) 0.017(3) -0.035(4) -0.014(3) C49 0.037(4) 0.037(4) 0.051(5) -0.007(3) -0.012(3) -0.001(3) C50 0.042(4) 0.020(3) 0.051(4) 0.002(3) -0.018(3) -0.010(3) C51 0.037(4) 0.033(3) 0.059(5) 0.008(3) -0.027(3) -0.013(3) C52 0.039(4) 0.046(4) 0.068(5) 0.020(4) -0.020(4) -0.020(3) C53 0.044(4) 0.037(4) 0.084(6) 0.011(4) -0.040(4) -0.008(3) C54 0.054(5) 0.033(4) 0.082(6) 0.004(4) -0.043(5) -0.013(3) C55 0.064(9) 0.41(3) 0.075(10) 0.116(15) 0.008(7) -0.022(14) C56 0.072(7) 0.129(9) 0.057(6) 0.005(6) -0.036(5) -0.036(6) C57 0.59(7) 0.15(2) 0.37(5) -0.12(3) 0.35(5) -0.19(3) C58 0.32(4) 0.38(4) 0.19(2) -0.18(3) 0.17(3) -0.23(3) Cl5 0.140(4) 0.163(4) 0.101(3) -0.010(2) -0.010(2) -0.081(3) Cl6 0.0764(19) 0.0791(19) 0.154(3) -0.0148(19) -0.043(2) -0.0069(15) Cl7 0.111(3) 0.221(5) 0.101(3) -0.031(3) -0.030(2) -0.087(3) Cl8 0.114(3) 0.098(2) 0.133(3) 0.037(2) -0.046(2) -0.039(2) Cl9 0.103(3) 0.168(4) 0.184(5) -0.057(4) -0.062(3) -0.014(3) Cl10 0.144(5) 0.132(4) 0.445(13) -0.050(6) 0.011(6) -0.061(4) Cl11 0.148(4) 0.242(6) 0.286(8) -0.156(6) -0.003(5) -0.105(4) Cl12 0.64(2) 0.317(11) 0.231(8) 0.076(8) -0.197(12) -0.378(14) #----------------------------------------------------------------------------# # 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 Pd P1 2.2795(17) . ? Pd P2 2.2895(18) . ? Pd Cl4 2.322(2) . ? Pd Cl3 2.3482(18) . ? Ti N2 1.885(5) . ? Ti N1 1.896(5) . ? Ti Cl1 2.251(2) . ? Ti Cl2 2.264(2) . ? P1 C7 1.822(6) . ? P1 C1 1.828(6) . ? P1 C13 1.837(7) . ? P2 C28 1.829(6) . ? P2 C40 1.832(7) . ? P2 C34 1.832(6) . ? N1 C3 1.436(8) . ? N1 C19 1.518(8) . ? N2 C30 1.431(7) . ? N2 C46 1.517(7) . ? C1 C2 1.384(9) . ? C1 C6 1.399(9) . ? C2 C3 1.396(8) . ? C3 C4 1.398(8) . ? C4 C5 1.393(9) . ? C5 C6 1.382(9) . ? C7 C8 1.390(10) . ? C7 C12 1.392(9) . ? C8 C9 1.390(11) . ? C9 C10 1.391(12) . ? C10 C11 1.369(12) . ? C11 C12 1.377(10) . ? C13 C14 1.372(10) . ? C13 C18 1.384(10) . ? C14 C15 1.407(12) . ? C15 C16 1.376(13) . ? C16 C17 1.371(13) . ? C17 C18 1.370(11) . ? C19 C24 1.568(9) . ? C19 C20 1.587(8) . ? C20 C22 1.526(11) . ? C20 C23 1.541(9) . ? C20 C21 1.547(10) . ? C24 C27 1.532(10) . ? C24 C26 1.539(10) . ? C24 C25 1.558(11) . ? C28 C29 1.390(8) . ? C28 C33 1.412(8) . ? C29 C30 1.390(8) . ? C30 C31 1.406(8) . ? C31 C32 1.394(9) . ? C32 C33 1.362(9) . ? C34 C39 1.373(10) . ? C34 C35 1.397(10) . ? C35 C36 1.405(10) . ? C36 C37 1.362(13) . ? C37 C38 1.368(13) . ? C38 C39 1.418(11) . ? C40 C41 1.383(10) . ? C40 C45 1.397(10) . ? C41 C42 1.391(11) . ? C42 C43 1.372(14) . ? C43 C44 1.393(13) . ? C44 C45 1.392(11) . ? C46 C51 1.564(9) . ? C46 C47 1.592(8) . ? C47 C49 1.529(10) . ? C47 C50 1.550(9) . ? C47 C48 1.563(9) . ? C51 C54 1.536(10) . ? C51 C53 1.546(9) . ? C51 C52 1.556(11) . ? C55 Cl5 1.795(11) . ? C55 Cl6 1.802(13) . ? C56 Cl7 1.742(9) . ? C56 Cl8 1.761(10) . ? C57 Cl9 1.730(15) . ? C57 Cl10 1.734(16) . ? C58 Cl11 1.748(15) . ? C58 Cl12 1.893(15) . ? 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 P1 Pd P2 98.62(6) . . ? P1 Pd Cl4 89.17(7) . . ? P2 Pd Cl4 168.81(7) . . ? P1 Pd Cl3 174.69(7) . . ? P2 Pd Cl3 83.11(6) . . ? Cl4 Pd Cl3 89.85(7) . . ? N2 Ti N1 114.9(2) . . ? N2 Ti Cl1 108.97(15) . . ? N1 Ti Cl1 109.95(16) . . ? N2 Ti Cl2 109.45(16) . . ? N1 Ti Cl2 109.13(15) . . ? Cl1 Ti Cl2 103.84(9) . . ? C7 P1 C1 111.3(3) . . ? C7 P1 C13 101.7(3) . . ? C1 P1 C13 102.8(3) . . ? C7 P1 Pd 114.3(2) . . ? C1 P1 Pd 108.6(2) . . ? C13 P1 Pd 117.4(2) . . ? C28 P2 C40 101.8(3) . . ? C28 P2 C34 103.8(3) . . ? C40 P2 C34 108.3(3) . . ? C28 P2 Pd 121.0(2) . . ? C40 P2 Pd 108.0(2) . . ? C34 P2 Pd 112.9(2) . . ? C3 N1 C19 123.8(5) . . ? C3 N1 Ti 113.1(4) . . ? C19 N1 Ti 122.6(4) . . ? C30 N2 C46 122.5(5) . . ? C30 N2 Ti 115.1(4) . . ? C46 N2 Ti 121.8(4) . . ? C2 C1 C6 119.6(6) . . ? C2 C1 P1 126.5(5) . . ? C6 C1 P1 113.9(5) . . ? C1 C2 C3 120.8(5) . . ? C2 C3 C4 118.7(6) . . ? C2 C3 N1 123.9(5) . . ? C4 C3 N1 117.2(5) . . ? C5 C4 C3 121.0(6) . . ? C6 C5 C4 119.4(5) . . ? C5 C6 C1 120.5(6) . . ? C8 C7 C12 119.1(6) . . ? C8 C7 P1 121.3(5) . . ? C12 C7 P1 119.4(5) . . ? C9 C8 C7 120.1(7) . . ? C8 C9 C10 119.7(8) . . ? C11 C10 C9 120.1(7) . . ? C10 C11 C12 120.6(7) . . ? C11 C12 C7 120.3(7) . . ? C14 C13 C18 119.2(7) . . ? C14 C13 P1 121.4(6) . . ? C18 C13 P1 119.4(5) . . ? C13 C14 C15 119.5(8) . . ? C16 C15 C14 120.4(8) . . ? C17 C16 C15 119.4(8) . . ? C18 C17 C16 120.3(8) . . ? C17 C18 C13 121.2(8) . . ? N1 C19 C24 112.0(5) . . ? N1 C19 C20 114.0(5) . . ? C24 C19 C20 120.9(5) . . ? C22 C20 C23 108.2(6) . . ? C22 C20 C21 108.2(6) . . ? C23 C20 C21 105.2(6) . . ? C22 C20 C19 114.8(6) . . ? C23 C20 C19 111.8(5) . . ? C21 C20 C19 108.2(6) . . ? C27 C24 C26 106.6(6) . . ? C27 C24 C25 107.1(6) . . ? C26 C24 C25 106.9(6) . . ? C27 C24 C19 108.8(6) . . ? C26 C24 C19 111.5(6) . . ? C25 C24 C19 115.4(6) . . ? C29 C28 C33 118.6(5) . . ? C29 C28 P2 122.3(4) . . ? C33 C28 P2 119.1(4) . . ? C28 C29 C30 121.7(5) . . ? C29 C30 C31 118.2(5) . . ? C29 C30 N2 124.1(5) . . ? C31 C30 N2 117.6(5) . . ? C32 C31 C30 120.5(6) . . ? C33 C32 C31 120.4(5) . . ? C32 C33 C28 120.5(6) . . ? C39 C34 C35 119.9(6) . . ? C39 C34 P2 122.5(5) . . ? C35 C34 P2 117.6(5) . . ? C34 C35 C36 120.1(8) . . ? C37 C36 C35 119.8(8) . . ? C36 C37 C38 120.5(7) . . ? C37 C38 C39 120.9(8) . . ? C34 C39 C38 118.9(8) . . ? C41 C40 C45 119.2(7) . . ? C41 C40 P2 120.9(6) . . ? C45 C40 P2 119.9(6) . . ? C40 C41 C42 120.5(8) . . ? C43 C42 C41 119.9(8) . . ? C42 C43 C44 120.9(8) . . ? C45 C44 C43 118.9(8) . . ? C44 C45 C40 120.6(8) . . ? N2 C46 C51 112.1(5) . . ? N2 C46 C47 114.3(5) . . ? C51 C46 C47 119.2(5) . . ? C49 C47 C50 106.6(6) . . ? C49 C47 C48 108.3(6) . . ? C50 C47 C48 104.3(5) . . ? C49 C47 C46 116.6(5) . . ? C50 C47 C46 111.9(5) . . ? C48 C47 C46 108.5(5) . . ? C54 C51 C53 105.1(6) . . ? C54 C51 C52 107.5(6) . . ? C53 C51 C52 107.7(6) . . ? C54 C51 C46 108.5(6) . . ? C53 C51 C46 110.5(5) . . ? C52 C51 C46 116.8(6) . . ? Cl5 C55 Cl6 108.1(8) . . ? Cl7 C56 Cl8 111.0(6) . . ? Cl9 C57 Cl10 111.7(13) . . ? Cl11 C58 Cl12 102.5(11) . . ? data_sep401 _database_code_depnum_ccdc_archive 'CCDC 231689' _audit_creation_date 2001-09-05T10:00:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[PtCl2{PPh2C6H3NCHiPr2}2TiCl2].4(C6D6)' _chemical_formula_moiety '(C54 H66 Cl4 N2 P2 Pt1 Ti1).4(C6 D6)' _chemical_formula_sum 'C78 H66 D24 Cl4 N2 P2 Pt Ti' _chemical_formula_weight 1526.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8106(6) _cell_length_b 15.2893(10) _cell_length_c 19.2600(13) _cell_angle_alpha 107.863(2) _cell_angle_beta 97.797(4) _cell_angle_gamma 103.977(4) _cell_volume 3658.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28261 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.39 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.762 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 19127 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_unetI/netI 0.0862 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 23.01 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _reflns_number_total 9883 _reflns_number_gt 8162 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Benzene solvate molecules were refined as rigid bodies. 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^)+(0.0605P)^2^+6.7635P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9883 _refine_ls_number_parameters 745 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.753 _refine_diff_density_min -1.344 _refine_diff_density_rms 0.124 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' 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 Pt Pt 0.70343(2) 0.85818(2) 0.510804(15) 0.02964(12) Uani 1 1 d . . . Ti Ti 0.74450(9) 1.06875(10) 0.93332(7) 0.0346(3) Uani 1 1 d . . . Cl1 Cl 0.64146(14) 0.89585(14) 0.40848(10) 0.0416(5) Uani 1 1 d . . . Cl2 Cl 0.64549(15) 0.69716(14) 0.43023(10) 0.0436(5) Uani 1 1 d . . . Cl3 Cl 0.87542(15) 1.14379(16) 1.03507(11) 0.0508(5) Uani 1 1 d . . . Cl4 Cl 0.60677(15) 1.06735(16) 0.98287(11) 0.0480(5) Uani 1 1 d . . . P1 P 0.75129(13) 1.01504(14) 0.58419(10) 0.0289(4) Uani 1 1 d . . . P2 P 0.75503(13) 0.79574(14) 0.59696(10) 0.0312(4) Uani 1 1 d . . . N1 N 0.7505(4) 1.1485(4) 0.8744(3) 0.0344(15) Uani 1 1 d . . . N2 N 0.7404(4) 0.9390(4) 0.8851(3) 0.0320(14) Uani 1 1 d . . . C1 C 0.6962(5) 1.0298(5) 0.6667(4) 0.0266(16) Uani 1 1 d . . . C2 C 0.7490(5) 1.0875(5) 0.7385(4) 0.0301(17) Uani 1 1 d . . . H2 H 0.8188 1.1235 0.7478 0.036 Uiso 1 1 calc R . . C3 C 0.6996(5) 1.0934(5) 0.7982(4) 0.0290(16) Uani 1 1 d . . . C4 C 0.5959(5) 1.0418(5) 0.7822(4) 0.0339(18) Uani 1 1 d . . . H4 H 0.5612 1.0458 0.8219 0.041 Uiso 1 1 calc R . . C5 C 0.5437(5) 0.9855(5) 0.7103(4) 0.0344(18) Uani 1 1 d . . . H5 H 0.4731 0.9511 0.7004 0.041 Uiso 1 1 calc R . . C6 C 0.5930(5) 0.9787(5) 0.6526(4) 0.0319(17) Uani 1 1 d . . . H6 H 0.5567 0.9392 0.6028 0.038 Uiso 1 1 calc R . . C7 C 0.8887(5) 1.0758(5) 0.6133(4) 0.0301(17) Uani 1 1 d . . . C8 C 0.9272(6) 1.1731(6) 0.6560(4) 0.041(2) Uani 1 1 d . . . H8 H 0.8815 1.2082 0.6726 0.05 Uiso 1 1 calc R . . C9 C 1.0322(6) 1.2201(6) 0.6750(4) 0.046(2) Uani 1 1 d . . . H9 H 1.0581 1.2865 0.7052 0.056 Uiso 1 1 calc R . . C10 C 1.0987(6) 1.1691(7) 0.6493(5) 0.047(2) Uani 1 1 d . . . H10 H 1.1703 1.2008 0.6618 0.056 Uiso 1 1 calc R . . C11 C 1.0616(6) 1.0734(7) 0.6062(5) 0.045(2) Uani 1 1 d . . . H11 H 1.1077 1.0393 0.5885 0.054 Uiso 1 1 calc R . . C12 C 0.9575(5) 1.0257(6) 0.5880(4) 0.0351(18) Uani 1 1 d . . . H12 H 0.9327 0.959 0.5583 0.042 Uiso 1 1 calc R . . C13 C 0.7098(5) 1.0967(5) 0.5436(4) 0.0329(17) Uani 1 1 d . . . C14 C 0.6292(5) 1.1318(6) 0.5613(4) 0.0365(18) Uani 1 1 d . . . H14 H 0.5921 1.1117 0.5946 0.044 Uiso 1 1 calc R . . C15 C 0.6021(6) 1.1964(6) 0.5305(5) 0.053(2) Uani 1 1 d . . . H15 H 0.5485 1.2221 0.5443 0.063 Uiso 1 1 calc R . . C16 C 0.6528(6) 1.2225(7) 0.4806(5) 0.055(2) Uani 1 1 d . . . H16 H 0.6331 1.2653 0.4588 0.066 Uiso 1 1 calc R . . C17 C 0.7318(7) 1.1878(6) 0.4616(5) 0.053(2) Uani 1 1 d . . . H17 H 0.7675 1.2071 0.4273 0.064 Uiso 1 1 calc R . . C18 C 0.7588(6) 1.1252(6) 0.4923(4) 0.0419(19) Uani 1 1 d . . . H18 H 0.8128 1.1004 0.4781 0.05 Uiso 1 1 calc R . . C19 C 0.7926(6) 1.2552(6) 0.9043(5) 0.056(2) Uani 1 1 d . . . H19 H 0.8025 1.264 0.9587 0.067 Uiso 1 1 calc R . . C20 C 0.7128(7) 1.3078(7) 0.9012(6) 0.069(3) Uani 1 1 d . . . C21 C 0.6714(9) 1.2944(9) 0.8123(7) 0.093(4) Uani 1 1 d . . . H21A H 0.7293 1.3205 0.7928 0.139 Uiso 1 1 calc R . . H21B H 0.6208 1.3291 0.8091 0.139 Uiso 1 1 calc R . . H21C H 0.6397 1.2258 0.7827 0.139 Uiso 1 1 calc R . . C22 C 0.7474(8) 1.4142(7) 0.9378(6) 0.076(3) Uani 1 1 d . . . H22A H 0.8126 1.4408 0.9261 0.114 Uiso 1 1 calc R . . H22B H 0.7568 1.4314 0.9922 0.114 Uiso 1 1 calc R . . H22C H 0.6959 1.4409 0.9194 0.114 Uiso 1 1 calc R . . C23 C 0.6144(8) 1.2634(8) 0.9156(7) 0.085(3) Uani 1 1 d . . . H23A H 0.5944 1.1934 0.8902 0.127 Uiso 1 1 calc R . . H23B H 0.5619 1.2887 0.8966 0.127 Uiso 1 1 calc R . . H23C H 0.6213 1.2784 0.9697 0.127 Uiso 1 1 calc R . . C24 C 0.9088(6) 1.3010(6) 0.9050(5) 0.048(2) Uani 1 1 d . . . C25 C 0.9636(7) 1.3720(7) 0.9855(6) 0.073(3) Uani 1 1 d . . . H25A H 0.9534 1.3385 1.0212 0.11 Uiso 1 1 calc R . . H25B H 0.935 1.4261 0.9979 0.11 Uiso 1 1 calc R . . H25C H 1.0371 1.3962 0.9883 0.11 Uiso 1 1 calc R . . C26 C 0.9243(8) 1.3516(8) 0.8494(7) 0.078(3) Uani 1 1 d . . . H26A H 0.8893 1.3063 0.7987 0.118 Uiso 1 1 calc R . . H26B H 0.9977 1.3754 0.8519 0.118 Uiso 1 1 calc R . . H26C H 0.8959 1.4059 0.8615 0.118 Uiso 1 1 calc R . . C27 C 0.9661(6) 1.2235(6) 0.8891(5) 0.050(2) Uani 1 1 d . . . H27A H 0.9589 1.1902 0.9251 0.074 Uiso 1 1 calc R . . H27B H 1.0388 1.2547 0.8941 0.074 Uiso 1 1 calc R . . H27C H 0.9365 1.1768 0.8382 0.074 Uiso 1 1 calc R . . C28 C 0.8079(5) 0.8694(5) 0.6966(4) 0.0283(16) Uani 1 1 d . . . C29 C 0.7500(5) 0.8725(5) 0.7505(4) 0.0286(16) Uani 1 1 d . . . H29 H 0.6794 0.8367 0.7363 0.034 Uiso 1 1 calc R . . C30 C 0.7959(5) 0.9285(5) 0.8261(4) 0.0283(16) Uani 1 1 d . . . C31 C 0.8974(5) 0.9832(5) 0.8448(4) 0.0312(17) Uani 1 1 d . . . H31 H 0.9287 1.0221 0.8957 0.037 Uiso 1 1 calc R . . C32 C 0.9548(5) 0.9825(5) 0.7907(4) 0.0337(18) Uani 1 1 d . . . H32 H 1.0245 1.0208 0.8045 0.04 Uiso 1 1 calc R . . C33 C 0.9104(5) 0.9262(5) 0.7174(4) 0.0313(17) Uani 1 1 d . . . H33 H 0.9495 0.9258 0.6804 0.038 Uiso 1 1 calc R . . C34 C 0.8590(5) 0.7451(5) 0.5764(4) 0.0363(18) Uani 1 1 d . . . C35 C 0.9009(6) 0.7029(6) 0.6231(4) 0.043(2) Uani 1 1 d . . . H35 H 0.8769 0.7025 0.667 0.052 Uiso 1 1 calc R . . C36 C 0.9771(6) 0.6618(7) 0.6053(5) 0.056(2) Uani 1 1 d . . . H36 H 1.0046 0.6319 0.6364 0.067 Uiso 1 1 calc R . . C37 C 1.0135(7) 0.6643(7) 0.5421(5) 0.061(3) Uani 1 1 d . . . H37 H 1.0655 0.6355 0.5297 0.073 Uiso 1 1 calc R . . C38 C 0.9751(6) 0.7076(7) 0.4980(5) 0.052(2) Uani 1 1 d . . . H38 H 1.0026 0.7115 0.4561 0.062 Uiso 1 1 calc R . . C39 C 0.8971(5) 0.7457(6) 0.5132(4) 0.0399(19) Uani 1 1 d . . . H39 H 0.8687 0.7729 0.4803 0.048 Uiso 1 1 calc R . . C40 C 0.6500(5) 0.6972(5) 0.5989(4) 0.0332(18) Uani 1 1 d . . . C41 C 0.5592(5) 0.7172(6) 0.6115(4) 0.0379(19) Uani 1 1 d . . . H41 H 0.5528 0.7793 0.6168 0.045 Uiso 1 1 calc R . . C42 C 0.4780(6) 0.6467(6) 0.6162(4) 0.042(2) Uani 1 1 d . . . H42 H 0.4166 0.6606 0.6255 0.05 Uiso 1 1 calc R . . C43 C 0.4873(6) 0.5573(6) 0.6074(4) 0.048(2) Uani 1 1 d . . . H43 H 0.4323 0.5096 0.6118 0.058 Uiso 1 1 calc R . . C44 C 0.5746(6) 0.5348(6) 0.5923(5) 0.049(2) Uani 1 1 d . . . H44 H 0.579 0.4716 0.5843 0.059 Uiso 1 1 calc R . . C45 C 0.6560(6) 0.6057(6) 0.5890(4) 0.042(2) Uani 1 1 d . . . H45 H 0.717 0.591 0.5797 0.051 Uiso 1 1 calc R . . C46 C 0.6962(5) 0.8605(6) 0.9140(4) 0.042(2) Uani 1 1 d . . . H46 H 0.6778 0.8966 0.9606 0.05 Uiso 1 1 calc R . . C47 C 0.7803(5) 0.8214(6) 0.9447(4) 0.0399(19) Uani 1 1 d . . . C48 C 0.8645(6) 0.9072(7) 1.0059(5) 0.056(2) Uani 1 1 d . . . H48A H 0.8929 0.9554 0.9844 0.084 Uiso 1 1 calc R . . H48B H 0.9193 0.884 1.0247 0.084 Uiso 1 1 calc R . . H48C H 0.8348 0.9362 1.0472 0.084 Uiso 1 1 calc R . . C49 C 0.7404(7) 0.7500(8) 0.9827(6) 0.068(3) Uani 1 1 d . . . H49A H 0.7963 0.7275 1.0004 0.102 Uiso 1 1 calc R . . H49B H 0.6851 0.695 0.9467 0.102 Uiso 1 1 calc R . . H49C H 0.7143 0.7819 1.0252 0.102 Uiso 1 1 calc R . . C50 C 0.8365(6) 0.7726(7) 0.8864(5) 0.058(2) Uani 1 1 d . . . H50A H 0.8637 0.8166 0.8611 0.087 Uiso 1 1 calc R . . H50B H 0.7882 0.7132 0.8494 0.087 Uiso 1 1 calc R . . H50C H 0.893 0.7575 0.9121 0.087 Uiso 1 1 calc R . . C51 C 0.5894(5) 0.7868(6) 0.8650(4) 0.0359(18) Uani 1 1 d . . . C52 C 0.5237(6) 0.7581(6) 0.9192(4) 0.045(2) Uani 1 1 d . . . H52A H 0.5209 0.8164 0.9574 0.068 Uiso 1 1 calc R . . H52B H 0.5549 0.7207 0.9435 0.068 Uiso 1 1 calc R . . H52C H 0.4541 0.7191 0.8906 0.068 Uiso 1 1 calc R . . C53 C 0.5924(6) 0.6955(6) 0.8076(4) 0.048(2) Uani 1 1 d . . . H53A H 0.6312 0.663 0.8321 0.072 Uiso 1 1 calc R . . H53B H 0.6255 0.7111 0.7692 0.072 Uiso 1 1 calc R . . H53C H 0.5223 0.6529 0.7842 0.072 Uiso 1 1 calc R . . C54 C 0.5279(5) 0.8359(6) 0.8246(4) 0.0383(19) Uani 1 1 d . . . H54A H 0.5247 0.8956 0.861 0.057 Uiso 1 1 calc R . . H54B H 0.4583 0.7925 0.8009 0.057 Uiso 1 1 calc R . . H54C H 0.5616 0.851 0.7863 0.057 Uiso 1 1 calc R . . C55 C 0.6850(6) 0.6948(6) 1.1658(5) 0.100(4) Uani 1 1 d G . . H55 H 0.7384 0.7505 1.1711 0.119 Uiso 1 1 calc R . . C56 C 0.6596(8) 0.6134(8) 1.1015(4) 0.106(5) Uani 1 1 d G . . H56 H 0.6958 0.6134 1.0629 0.127 Uiso 1 1 calc R . . C57 C 0.5814(8) 0.5319(5) 1.0936(5) 0.104(5) Uani 1 1 d G . . H57 H 0.5641 0.4762 1.0497 0.125 Uiso 1 1 calc R . . C58 C 0.5285(6) 0.5318(6) 1.1501(7) 0.105(5) Uani 1 1 d G . . H58 H 0.475 0.4761 1.1447 0.126 Uiso 1 1 calc R . . C59 C 0.5538(6) 0.6132(8) 1.2144(5) 0.093(4) Uani 1 1 d G . . H59 H 0.5176 0.6132 1.253 0.112 Uiso 1 1 calc R . . C60 C 0.6321(7) 0.6947(6) 1.2222(4) 0.082(4) Uani 1 1 d G . . H60 H 0.6494 0.7504 1.2662 0.099 Uiso 1 1 calc R . . C61 C 0.8948(8) 1.5619(5) 0.7779(4) 0.096(4) Uani 1 1 d G . . H61 H 0.9115 1.6177 0.8216 0.115 Uiso 1 1 calc R . . C62 C 0.7929(6) 1.5119(7) 0.7423(5) 0.104(4) Uani 1 1 d G . . H62 H 0.7398 1.5337 0.7617 0.125 Uiso 1 1 calc R . . C63 C 0.7685(6) 1.4302(6) 0.6784(5) 0.100(4) Uani 1 1 d G . . H63 H 0.6989 1.3961 0.6541 0.12 Uiso 1 1 calc R . . C64 C 0.8461(8) 1.3983(6) 0.6500(4) 0.100(4) Uani 1 1 d G . . H64 H 0.8295 1.3424 0.6064 0.12 Uiso 1 1 calc R . . C65 C 0.9481(7) 1.4482(7) 0.6856(5) 0.093(4) Uani 1 1 d G . . H65 H 1.0011 1.4265 0.6662 0.111 Uiso 1 1 calc R . . C66 C 0.9724(5) 1.5300(7) 0.7495(5) 0.089(4) Uani 1 1 d G . . H66 H 1.0421 1.5641 0.7738 0.107 Uiso 1 1 calc R . . C67 C 1.3365(5) 1.0118(5) 0.8423(3) 0.076(3) Uani 1 1 d G . . H67 H 1.3907 1.0412 0.8858 0.091 Uiso 1 1 calc R . . C68 C 1.3338(5) 1.0512(5) 0.7862(4) 0.081(3) Uani 1 1 d G . . H68 H 1.3862 1.1076 0.7914 0.097 Uiso 1 1 calc R . . C69 C 1.2544(5) 1.0082(6) 0.7225(4) 0.089(4) Uani 1 1 d G . . H69 H 1.2526 1.0351 0.6841 0.107 Uiso 1 1 calc R . . C70 C 1.1777(4) 0.9258(5) 0.7149(3) 0.070(3) Uani 1 1 d G . . H70 H 1.1235 0.8963 0.6713 0.085 Uiso 1 1 calc R . . C71 C 1.1804(5) 0.8863(4) 0.7710(4) 0.068(3) Uani 1 1 d G . . H71 H 1.128 0.83 0.7658 0.081 Uiso 1 1 calc R . . C72 C 1.2598(6) 0.9294(6) 0.8347(3) 0.078(3) Uani 1 1 d G . . H72 H 1.2616 0.9024 0.873 0.093 Uiso 1 1 calc R . . C73 C 1.2186(7) 0.5635(13) 0.6389(7) 0.159(8) Uani 1 1 d G . . H73 H 1.2055 0.5595 0.5881 0.191 Uiso 1 1 calc R . . C74 C 1.2269(6) 0.6487(9) 0.6958(10) 0.109(5) Uani 1 1 d G . . H74 H 1.2194 0.703 0.684 0.131 Uiso 1 1 calc R . . C75 C 1.2461(6) 0.6546(8) 0.7701(8) 0.126(6) Uani 1 1 d G . . H75 H 1.2517 0.7129 0.809 0.151 Uiso 1 1 calc R . . C76 C 1.2571(7) 0.5752(13) 0.7875(8) 0.166(9) Uani 1 1 d G . . H76 H 1.2702 0.5792 0.8382 0.199 Uiso 1 1 calc R . . C77 C 1.2489(7) 0.4900(9) 0.7305(13) 0.211(16) Uani 1 1 d G . . H77 H 1.2564 0.4357 0.7424 0.253 Uiso 1 1 calc R . . C78 C 1.2296(7) 0.4841(8) 0.6563(10) 0.193(14) Uani 1 1 d G . . H78 H 1.224 0.4258 0.6174 0.231 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 Pt 0.03276(18) 0.03102(19) 0.02831(18) 0.01589(14) 0.00597(11) 0.00871(12) Ti 0.0332(7) 0.0388(9) 0.0305(7) 0.0138(7) 0.0082(5) 0.0059(6) Cl1 0.0558(12) 0.0390(12) 0.0314(10) 0.0196(9) 0.0027(8) 0.0111(9) Cl2 0.0592(12) 0.0320(11) 0.0362(11) 0.0130(9) 0.0033(9) 0.0105(9) Cl3 0.0491(12) 0.0559(14) 0.0389(12) 0.0187(11) 0.0017(9) 0.0024(10) Cl4 0.0477(11) 0.0536(14) 0.0471(12) 0.0204(11) 0.0225(9) 0.0130(10) P1 0.0292(10) 0.0303(11) 0.0297(10) 0.0155(9) 0.0057(7) 0.0072(8) P2 0.0336(10) 0.0310(11) 0.0321(11) 0.0165(9) 0.0071(8) 0.0087(8) N1 0.032(3) 0.037(4) 0.034(4) 0.014(3) 0.008(3) 0.007(3) N2 0.030(3) 0.043(4) 0.032(3) 0.025(3) 0.008(2) 0.012(3) C1 0.023(4) 0.029(4) 0.032(4) 0.017(3) 0.005(3) 0.007(3) C2 0.029(4) 0.027(4) 0.035(4) 0.014(4) 0.007(3) 0.006(3) C3 0.030(4) 0.025(4) 0.034(4) 0.014(3) 0.002(3) 0.009(3) C4 0.037(4) 0.037(5) 0.033(4) 0.018(4) 0.011(3) 0.012(4) C5 0.033(4) 0.031(4) 0.044(5) 0.021(4) 0.012(3) 0.006(3) C6 0.029(4) 0.032(4) 0.033(4) 0.014(4) 0.002(3) 0.006(3) C7 0.028(4) 0.035(5) 0.036(4) 0.028(4) 0.005(3) 0.006(3) C8 0.046(5) 0.040(5) 0.039(5) 0.020(4) 0.007(3) 0.008(4) C9 0.043(5) 0.045(5) 0.042(5) 0.019(4) 0.001(4) -0.002(4) C10 0.026(4) 0.065(7) 0.052(5) 0.031(5) 0.005(4) 0.005(4) C11 0.037(5) 0.066(7) 0.048(5) 0.035(5) 0.014(4) 0.022(4) C12 0.037(4) 0.035(5) 0.039(4) 0.021(4) 0.006(3) 0.012(4) C13 0.029(4) 0.033(5) 0.039(4) 0.015(4) 0.002(3) 0.012(3) C14 0.031(4) 0.038(5) 0.039(4) 0.019(4) 0.001(3) 0.004(3) C15 0.036(5) 0.047(6) 0.072(6) 0.023(5) 0.001(4) 0.011(4) C16 0.049(5) 0.052(6) 0.067(6) 0.039(5) -0.009(4) 0.008(4) C17 0.061(6) 0.055(6) 0.060(6) 0.040(5) 0.015(4) 0.019(5) C18 0.048(5) 0.042(5) 0.046(5) 0.027(4) 0.013(4) 0.015(4) C19 0.044(5) 0.038(5) 0.063(6) -0.004(5) -0.002(4) 0.010(4) C20 0.065(6) 0.052(6) 0.110(9) 0.037(6) 0.043(6) 0.029(5) C21 0.111(9) 0.090(9) 0.095(9) 0.040(8) 0.010(7) 0.056(8) C22 0.077(7) 0.040(6) 0.100(8) 0.005(6) 0.014(6) 0.027(5) C23 0.077(7) 0.062(7) 0.123(10) 0.028(7) 0.032(7) 0.035(6) C24 0.052(5) 0.034(5) 0.049(5) 0.013(4) 0.007(4) 0.005(4) C25 0.056(6) 0.051(6) 0.079(7) -0.006(6) -0.003(5) 0.002(5) C26 0.099(8) 0.071(7) 0.114(9) 0.069(7) 0.057(7) 0.048(6) C27 0.037(4) 0.049(6) 0.061(6) 0.023(5) 0.007(4) 0.009(4) C28 0.032(4) 0.030(4) 0.029(4) 0.019(3) 0.002(3) 0.013(3) C29 0.025(4) 0.035(4) 0.030(4) 0.020(4) 0.003(3) 0.007(3) C30 0.032(4) 0.022(4) 0.033(4) 0.013(3) 0.004(3) 0.012(3) C31 0.025(4) 0.029(4) 0.039(4) 0.015(4) 0.002(3) 0.005(3) C32 0.022(4) 0.034(5) 0.044(5) 0.021(4) 0.004(3) 0.000(3) C33 0.033(4) 0.035(5) 0.034(4) 0.022(4) 0.010(3) 0.010(3) C34 0.037(4) 0.034(5) 0.040(5) 0.019(4) 0.005(3) 0.010(3) C35 0.056(5) 0.040(5) 0.045(5) 0.024(4) 0.012(4) 0.021(4) C36 0.055(5) 0.050(6) 0.070(6) 0.029(5) 0.011(5) 0.020(5) C37 0.051(5) 0.061(7) 0.076(7) 0.022(6) 0.021(5) 0.027(5) C38 0.049(5) 0.063(6) 0.056(6) 0.029(5) 0.027(4) 0.025(5) C39 0.036(4) 0.046(5) 0.046(5) 0.025(4) 0.013(3) 0.012(4) C40 0.044(4) 0.024(4) 0.023(4) 0.009(3) -0.001(3) -0.001(3) C41 0.035(4) 0.039(5) 0.037(4) 0.017(4) 0.000(3) 0.006(4) C42 0.036(4) 0.045(6) 0.042(5) 0.024(4) -0.001(3) 0.002(4) C43 0.047(5) 0.040(6) 0.048(5) 0.020(4) 0.000(4) -0.004(4) C44 0.060(6) 0.031(5) 0.053(5) 0.018(4) 0.007(4) 0.009(4) C45 0.046(5) 0.033(5) 0.051(5) 0.024(4) 0.007(4) 0.009(4) C46 0.036(4) 0.048(5) 0.043(5) 0.026(4) 0.006(3) 0.006(4) C47 0.042(4) 0.039(5) 0.044(5) 0.023(4) 0.005(3) 0.014(4) C48 0.050(5) 0.056(6) 0.060(6) 0.027(5) -0.009(4) 0.013(4) C49 0.055(6) 0.086(8) 0.081(7) 0.060(6) 0.005(5) 0.020(5) C50 0.057(5) 0.067(7) 0.068(6) 0.038(5) 0.014(4) 0.033(5) C51 0.034(4) 0.041(5) 0.036(4) 0.018(4) 0.010(3) 0.010(3) C52 0.043(5) 0.049(5) 0.051(5) 0.030(4) 0.015(4) 0.007(4) C53 0.067(6) 0.045(5) 0.038(5) 0.019(4) 0.009(4) 0.026(4) C54 0.023(4) 0.044(5) 0.047(5) 0.017(4) 0.004(3) 0.010(3) C55 0.114(10) 0.082(10) 0.099(10) 0.039(8) 0.036(8) 0.005(8) C56 0.196(15) 0.095(11) 0.062(8) 0.049(8) 0.050(8) 0.066(11) C57 0.170(14) 0.048(8) 0.070(9) 0.011(7) -0.021(8) 0.028(9) C58 0.092(9) 0.080(10) 0.151(14) 0.076(11) -0.004(9) 0.009(7) C59 0.091(9) 0.131(13) 0.086(9) 0.055(9) 0.022(7) 0.059(9) C60 0.086(8) 0.083(9) 0.053(7) -0.003(6) -0.017(6) 0.033(7) C61 0.109(10) 0.078(9) 0.087(9) 0.016(7) 0.014(8) 0.024(8) C62 0.112(11) 0.097(11) 0.116(11) 0.029(9) 0.036(8) 0.063(9) C63 0.088(9) 0.079(9) 0.117(11) 0.024(9) -0.010(7) 0.030(7) C64 0.120(11) 0.092(10) 0.083(9) 0.014(8) 0.009(8) 0.050(9) C65 0.137(12) 0.090(10) 0.098(10) 0.061(8) 0.053(9) 0.066(9) C66 0.075(8) 0.088(10) 0.125(11) 0.063(9) 0.019(7) 0.029(7) C67 0.063(7) 0.114(10) 0.054(6) 0.032(7) 0.012(5) 0.031(7) C68 0.047(6) 0.088(9) 0.136(11) 0.068(8) 0.033(6) 0.026(6) C69 0.058(7) 0.156(13) 0.113(10) 0.109(10) 0.042(6) 0.048(7) C70 0.059(6) 0.108(9) 0.060(6) 0.038(6) 0.021(5) 0.039(6) C71 0.065(6) 0.060(7) 0.088(8) 0.032(6) 0.027(6) 0.023(5) C72 0.092(8) 0.122(11) 0.054(7) 0.055(7) 0.031(6) 0.053(8) C73 0.039(7) 0.162(18) 0.210(19) -0.003(18) 0.017(8) 0.006(10) C74 0.043(7) 0.083(11) 0.202(17) 0.050(12) 0.028(9) 0.019(7) C75 0.056(8) 0.088(12) 0.194(18) 0.021(12) -0.019(9) 0.014(7) C76 0.073(10) 0.140(16) 0.27(3) 0.116(19) -0.041(11) 0.003(11) C77 0.045(8) 0.105(17) 0.48(5) 0.14(2) -0.018(17) 0.017(10) C78 0.064(10) 0.074(13) 0.37(4) -0.009(17) 0.024(15) 0.020(9) #----------------------------------------------------------------------------# # 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 Pt P1 2.2556(19) . ? Pt P2 2.2699(19) . ? Pt Cl1 2.3292(18) . ? Pt Cl2 2.340(2) . ? Ti N2 1.898(6) . ? Ti N1 1.899(6) . ? Ti Cl4 2.239(2) . ? Ti Cl3 2.255(2) . ? P1 C7 1.822(7) . ? P1 C13 1.822(7) . ? P1 C1 1.828(7) . ? P2 C34 1.822(7) . ? P2 C40 1.835(7) . ? P2 C28 1.838(7) . ? N1 C3 1.425(9) . ? N1 C19 1.486(10) . ? N2 C30 1.444(9) . ? N2 C46 1.507(9) . ? C1 C2 1.375(9) . ? C1 C6 1.395(9) . ? C2 C3 1.405(9) . ? C3 C4 1.397(9) . ? C4 C5 1.371(10) . ? C5 C6 1.371(10) . ? C7 C8 1.386(11) . ? C7 C12 1.406(10) . ? C8 C9 1.394(10) . ? C9 C10 1.389(12) . ? C10 C11 1.367(12) . ? C11 C12 1.386(10) . ? C13 C14 1.387(10) . ? C13 C18 1.388(10) . ? C14 C15 1.393(11) . ? C15 C16 1.363(12) . ? C16 C17 1.370(12) . ? C17 C18 1.365(11) . ? C19 C20 1.518(12) . ? C19 C24 1.585(11) . ? C20 C23 1.469(13) . ? C20 C22 1.484(13) . ? C20 C21 1.662(15) . ? C24 C26 1.511(12) . ? C24 C25 1.552(12) . ? C24 C27 1.555(12) . ? C28 C29 1.391(9) . ? C28 C33 1.399(9) . ? C29 C30 1.406(9) . ? C30 C31 1.381(9) . ? C31 C32 1.393(10) . ? C32 C33 1.369(10) . ? C34 C39 1.393(10) . ? C34 C35 1.398(11) . ? C35 C36 1.380(11) . ? C36 C37 1.385(12) . ? C37 C38 1.354(13) . ? C38 C39 1.367(11) . ? C40 C45 1.377(11) . ? C40 C41 1.395(10) . ? C41 C42 1.391(10) . ? C42 C43 1.364(12) . ? C43 C44 1.374(11) . ? C44 C45 1.385(11) . ? C46 C47 1.556(10) . ? C46 C51 1.582(10) . ? C47 C49 1.529(12) . ? C47 C48 1.551(11) . ? C47 C50 1.556(11) . ? C51 C53 1.505(11) . ? C51 C54 1.542(10) . ? C51 C52 1.565(10) . ? C55 C56 1.39 . ? C55 C60 1.39 . ? C56 C57 1.39 . ? C57 C58 1.39 . ? C58 C59 1.39 . ? C59 C60 1.39 . ? C61 C62 1.39 . ? C61 C66 1.39 . ? C62 C63 1.39 . ? C63 C64 1.39 . ? C64 C65 1.39 . ? C65 C66 1.39 . ? C67 C68 1.39 . ? C67 C72 1.39 . ? C68 C69 1.39 . ? C69 C70 1.39 . ? C70 C71 1.39 . ? C71 C72 1.39 . ? C73 C74 1.39 . ? C73 C78 1.39 . ? C74 C75 1.39 . ? C75 C76 1.39 . ? C76 C77 1.39 . ? C77 C78 1.39 . ? 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 P1 Pt P2 99.28(7) . . ? P1 Pt Cl1 90.27(7) . . ? P2 Pt Cl1 170.44(7) . . ? P1 Pt Cl2 176.43(7) . . ? P2 Pt Cl2 83.81(7) . . ? Cl1 Pt Cl2 86.64(7) . . ? N2 Ti N1 117.3(2) . . ? N2 Ti Cl4 107.91(18) . . ? N1 Ti Cl4 108.84(19) . . ? N2 Ti Cl3 111.30(18) . . ? N1 Ti Cl3 107.80(19) . . ? Cl4 Ti Cl3 102.68(9) . . ? C7 P1 C13 99.6(3) . . ? C7 P1 C1 109.6(3) . . ? C13 P1 C1 103.5(3) . . ? C7 P1 Pt 115.9(3) . . ? C13 P1 Pt 116.9(2) . . ? C1 P1 Pt 110.2(2) . . ? C34 P2 C40 106.3(4) . . ? C34 P2 C28 99.9(3) . . ? C40 P2 C28 103.3(3) . . ? C34 P2 Pt 112.2(2) . . ? C40 P2 Pt 111.0(2) . . ? C28 P2 Pt 122.5(2) . . ? C3 N1 C19 123.8(6) . . ? C3 N1 Ti 110.9(5) . . ? C19 N1 Ti 124.9(5) . . ? C30 N2 C46 125.1(6) . . ? C30 N2 Ti 112.5(4) . . ? C46 N2 Ti 121.9(5) . . ? C2 C1 C6 120.1(6) . . ? C2 C1 P1 124.6(5) . . ? C6 C1 P1 115.3(5) . . ? C1 C2 C3 120.1(6) . . ? C4 C3 C2 118.4(6) . . ? C4 C3 N1 118.4(6) . . ? C2 C3 N1 123.2(6) . . ? C5 C4 C3 121.1(6) . . ? C4 C5 C6 120.1(7) . . ? C5 C6 C1 120.2(7) . . ? C8 C7 C12 118.6(6) . . ? C8 C7 P1 121.2(6) . . ? C12 C7 P1 120.0(6) . . ? C7 C8 C9 120.9(8) . . ? C10 C9 C8 119.5(8) . . ? C11 C10 C9 120.3(7) . . ? C10 C11 C12 120.7(8) . . ? C11 C12 C7 120.0(7) . . ? C14 C13 C18 117.5(7) . . ? C14 C13 P1 122.5(6) . . ? C18 C13 P1 119.9(5) . . ? C13 C14 C15 120.5(7) . . ? C16 C15 C14 119.7(8) . . ? C15 C16 C17 120.8(8) . . ? C18 C17 C16 119.4(8) . . ? C17 C18 C13 122.0(8) . . ? N1 C19 C20 114.6(7) . . ? N1 C19 C24 117.7(6) . . ? C20 C19 C24 122.9(8) . . ? C23 C20 C22 112.3(8) . . ? C23 C20 C19 115.7(9) . . ? C22 C20 C19 117.6(8) . . ? C23 C20 C21 98.3(9) . . ? C22 C20 C21 101.7(9) . . ? C19 C20 C21 108.0(8) . . ? C26 C24 C25 110.0(8) . . ? C26 C24 C27 107.3(7) . . ? C25 C24 C27 104.9(7) . . ? C26 C24 C19 114.5(8) . . ? C25 C24 C19 108.3(7) . . ? C27 C24 C19 111.4(7) . . ? C29 C28 C33 119.6(6) . . ? C29 C28 P2 122.9(5) . . ? C33 C28 P2 117.4(5) . . ? C28 C29 C30 120.0(6) . . ? C31 C30 C29 118.8(6) . . ? C31 C30 N2 117.4(6) . . ? C29 C30 N2 123.6(6) . . ? C30 C31 C32 121.3(7) . . ? C33 C32 C31 119.7(6) . . ? C32 C33 C28 120.5(6) . . ? C39 C34 C35 118.5(7) . . ? C39 C34 P2 120.9(6) . . ? C35 C34 P2 120.6(6) . . ? C36 C35 C34 119.9(8) . . ? C35 C36 C37 120.0(9) . . ? C38 C37 C36 120.2(8) . . ? C37 C38 C39 120.7(8) . . ? C38 C39 C34 120.7(8) . . ? C45 C40 C41 118.6(7) . . ? C45 C40 P2 123.9(6) . . ? C41 C40 P2 117.4(6) . . ? C42 C41 C40 120.3(8) . . ? C43 C42 C41 119.5(8) . . ? C42 C43 C44 121.3(8) . . ? C43 C44 C45 119.0(8) . . ? C40 C45 C44 121.2(8) . . ? N2 C46 C47 111.7(6) . . ? N2 C46 C51 115.1(6) . . ? C47 C46 C51 119.0(7) . . ? C49 C47 C48 106.0(7) . . ? C49 C47 C50 107.1(7) . . ? C48 C47 C50 105.9(7) . . ? C49 C47 C46 113.1(6) . . ? C48 C47 C46 108.4(7) . . ? C50 C47 C46 115.7(6) . . ? C53 C51 C54 108.0(6) . . ? C53 C51 C52 107.8(7) . . ? C54 C51 C52 104.8(6) . . ? C53 C51 C46 116.6(6) . . ? C54 C51 C46 110.7(6) . . ? C52 C51 C46 108.2(6) . . ? C56 C55 C60 120 . . ? C55 C56 C57 120 . . ? C58 C57 C56 120 . . ? C57 C58 C59 120 . . ? C60 C59 C58 120 . . ? C59 C60 C55 120 . . ? C62 C61 C66 120 . . ? C63 C62 C61 120 . . ? C62 C63 C64 120 . . ? C65 C64 C63 120 . . ? C64 C65 C66 120 . . ? C65 C66 C61 120 . . ? C68 C67 C72 120 . . ? C69 C68 C67 120 . . ? C68 C69 C70 120 . . ? C69 C70 C71 120 . . ? C72 C71 C70 120 . . ? C71 C72 C67 120 . . ? C74 C73 C78 120 . . ? C75 C74 C73 120 . . ? C74 C75 C76 120 . . ? C75 C76 C77 120 . . ? C78 C77 C76 120 . . ? C77 C78 C73 120 . . ? data_sep801 _database_code_depnum_ccdc_archive 'CCDC 231690' _audit_creation_date 2001-09-13T17:21:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common {(OC)Pt{PPh2C6H4NSiMe3}3TiCl].2(C6D6) _chemical_formula_moiety ; '(C64 H69 Cl1 N3 O1 P3 Pt1 Si3 Ti1).2(C6 D6)' ; _chemical_formula_sum 'C76 H69 D12 Cl N3 O P3 Pt Si3 Ti' _chemical_formula_weight 1520.14 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.7651(3) _cell_length_b 23.4683(6) _cell_length_c 22.7171(5) _cell_angle_alpha 90 _cell_angle_beta 94.088(2) _cell_angle_gamma 90 _cell_volume 7319.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23564 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 0.784 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 32818 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_unetI/netI 0.0775 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 12819 _reflns_number_gt 9585 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The two deutero-benzene solvate molecules were poorly defined and were included as rigid bodies with a commmon Uiso for the C atoms. 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^)+(0.0417P)^2^+26.3744P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 12819 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.217 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.119 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 Pt Pt 0.781700(17) 0.323859(10) 0.819205(10) 0.02510(9) Uani 1 1 d . . . Ti Ti 1.18059(8) 0.24910(5) 0.67570(5) 0.0301(3) Uani 1 1 d . . . Cl Cl 1.31312(14) 0.21814(9) 0.63308(10) 0.0568(5) Uani 1 1 d . . . P1 P 0.92380(11) 0.36859(6) 0.85777(7) 0.0252(4) Uani 1 1 d . . . P2 P 0.81348(12) 0.22647(7) 0.82693(7) 0.0260(4) Uani 1 1 d . . . P3 P 0.76855(12) 0.34435(7) 0.71828(7) 0.0273(4) Uani 1 1 d . . . Si1 Si 1.31562(14) 0.35061(8) 0.73343(9) 0.0394(5) Uani 1 1 d . . . Si2 Si 1.18659(13) 0.12263(8) 0.73150(9) 0.0353(4) Uani 1 1 d . . . Si3 Si 1.07490(16) 0.26851(10) 0.54398(9) 0.0485(6) Uani 1 1 d . . . O O 0.6059(4) 0.3645(3) 0.8821(2) 0.0591(15) Uani 1 1 d . . . N1 N 1.2171(4) 0.3024(2) 0.7365(2) 0.0310(12) Uani 1 1 d . . . N2 N 1.1216(4) 0.1847(2) 0.7096(2) 0.0313(12) Uani 1 1 d . . . N3 N 1.0884(4) 0.2832(2) 0.6207(2) 0.0324(13) Uani 1 1 d . . . C1 C 1.0414(4) 0.3320(2) 0.8511(3) 0.0273(14) Uani 1 1 d . . . C2 C 1.0856(4) 0.3319(2) 0.7980(3) 0.0270(14) Uani 1 1 d . . . H2 H 1.0569 0.3528 0.7654 0.032 Uiso 1 1 calc R . . C3 C 1.1711(4) 0.3016(3) 0.7917(3) 0.0278(14) Uani 1 1 d . . . C4 C 1.2102(4) 0.2695(3) 0.8390(3) 0.0305(15) Uani 1 1 d . . . H4 H 1.2684 0.2483 0.8353 0.037 Uiso 1 1 calc R . . C5 C 1.1655(5) 0.2681(3) 0.8907(3) 0.0390(17) Uani 1 1 d . . . H5 H 1.1924 0.2455 0.9225 0.047 Uiso 1 1 calc R . . C6 C 1.0812(5) 0.2994(3) 0.8977(3) 0.0322(15) Uani 1 1 d . . . H6 H 1.0512 0.2985 0.9341 0.039 Uiso 1 1 calc R . . C7 C 0.9307(5) 0.3878(3) 0.9365(3) 0.0303(15) Uani 1 1 d . . . C8 C 1.0128(5) 0.4130(3) 0.9639(3) 0.0423(18) Uani 1 1 d . . . H8 H 1.0688 0.4183 0.9423 0.051 Uiso 1 1 calc R . . C9 C 1.0152(6) 0.4307(3) 1.0225(3) 0.052(2) Uani 1 1 d . . . H9 H 1.0722 0.4479 1.0407 0.063 Uiso 1 1 calc R . . C10 C 0.9352(7) 0.4233(3) 1.0534(3) 0.060(2) Uani 1 1 d . . . H10 H 0.9368 0.4351 1.0934 0.071 Uiso 1 1 calc R . . C11 C 0.8518(7) 0.3988(4) 1.0275(3) 0.060(2) Uani 1 1 d . . . H11 H 0.7959 0.3945 1.0493 0.072 Uiso 1 1 calc R . . C12 C 0.8502(6) 0.3805(3) 0.9690(3) 0.0466(19) Uani 1 1 d . . . H12 H 0.7934 0.3627 0.9513 0.056 Uiso 1 1 calc R . . C13 C 0.9424(5) 0.4408(3) 0.8291(3) 0.0273(14) Uani 1 1 d . . . C14 C 1.0305(5) 0.4638(3) 0.8155(3) 0.0364(16) Uani 1 1 d . . . H14 H 1.088 0.4414 0.8203 0.044 Uiso 1 1 calc R . . C15 C 1.0356(6) 0.5192(3) 0.7951(3) 0.0453(19) Uani 1 1 d . . . H15 H 1.0964 0.534 0.7848 0.054 Uiso 1 1 calc R . . C16 C 0.9540(6) 0.5530(3) 0.7894(3) 0.048(2) Uani 1 1 d . . . H16 H 0.9583 0.5911 0.7758 0.058 Uiso 1 1 calc R . . C17 C 0.8667(6) 0.5313(3) 0.8037(4) 0.051(2) Uani 1 1 d . . . H17 H 0.8099 0.5545 0.8003 0.061 Uiso 1 1 calc R . . C18 C 0.8607(5) 0.4756(3) 0.8229(3) 0.0408(17) Uani 1 1 d . . . H18 H 0.7994 0.4608 0.8321 0.049 Uiso 1 1 calc R . . C19 C 1.3494(6) 0.3609(4) 0.6568(4) 0.063(2) Uani 1 1 d . . . H19A H 1.2935 0.3762 0.6327 0.095 Uiso 1 1 calc R . . H19B H 1.3685 0.3242 0.6405 0.095 Uiso 1 1 calc R . . H19C H 1.404 0.3876 0.6566 0.095 Uiso 1 1 calc R . . C20 C 1.4225(5) 0.3221(4) 0.7782(4) 0.065(2) Uani 1 1 d . . . H20A H 1.4057 0.3167 0.819 0.098 Uiso 1 1 calc R . . H20B H 1.4768 0.3491 0.7774 0.098 Uiso 1 1 calc R . . H20C H 1.4417 0.2855 0.7619 0.098 Uiso 1 1 calc R . . C21 C 1.2796(7) 0.4207(3) 0.7637(5) 0.073(3) Uani 1 1 d . . . H21A H 1.262 0.4157 0.8044 0.109 Uiso 1 1 calc R . . H21B H 1.2237 0.4358 0.7395 0.109 Uiso 1 1 calc R . . H21C H 1.3343 0.4473 0.763 0.109 Uiso 1 1 calc R . . C22 C 0.8730(4) 0.1933(2) 0.7659(3) 0.0270(14) Uani 1 1 d . . . C23 C 0.9720(4) 0.2003(2) 0.7609(3) 0.0274(14) Uani 1 1 d . . . H23 H 1.01 0.2193 0.7914 0.033 Uiso 1 1 calc R . . C24 C 1.0167(4) 0.1798(2) 0.7119(3) 0.0269(14) Uani 1 1 d . . . C25 C 0.9606(5) 0.1530(3) 0.6669(3) 0.0336(15) Uani 1 1 d . . . H25 H 0.9903 0.1389 0.6333 0.04 Uiso 1 1 calc R . . C26 C 0.8619(5) 0.1470(3) 0.6709(3) 0.0356(16) Uani 1 1 d . . . H26 H 0.8232 0.1299 0.6394 0.043 Uiso 1 1 calc R . . C27 C 0.8187(5) 0.1656(3) 0.7206(3) 0.0304(15) Uani 1 1 d . . . H27 H 0.751 0.1595 0.7238 0.036 Uiso 1 1 calc R . . C28 C 0.7079(4) 0.1790(3) 0.8349(3) 0.0300(14) Uani 1 1 d . . . C29 C 0.7199(5) 0.1204(3) 0.8407(3) 0.0389(17) Uani 1 1 d . . . H29 H 0.7823 0.1038 0.8373 0.047 Uiso 1 1 calc R . . C30 C 0.6410(6) 0.0859(3) 0.8516(3) 0.0476(19) Uani 1 1 d . . . H30 H 0.6499 0.046 0.8564 0.057 Uiso 1 1 calc R . . C31 C 0.5505(6) 0.1093(3) 0.8555(3) 0.048(2) Uani 1 1 d . . . H31 H 0.4969 0.0854 0.8625 0.058 Uiso 1 1 calc R . . C32 C 0.5368(5) 0.1671(3) 0.8492(3) 0.0423(18) Uani 1 1 d . . . H32 H 0.4738 0.1831 0.8518 0.051 Uiso 1 1 calc R . . C33 C 0.6151(5) 0.2020(3) 0.8390(3) 0.0341(15) Uani 1 1 d . . . H33 H 0.6055 0.242 0.8348 0.041 Uiso 1 1 calc R . . C34 C 0.8873(4) 0.2030(3) 0.8933(3) 0.0297(14) Uani 1 1 d . . . C35 C 0.9516(5) 0.1571(3) 0.8948(3) 0.0412(17) Uani 1 1 d . . . H35 H 0.9616 0.1373 0.8593 0.049 Uiso 1 1 calc R . . C36 C 1.0010(6) 0.1397(3) 0.9466(3) 0.053(2) Uani 1 1 d . . . H36 H 1.0448 0.1085 0.9465 0.064 Uiso 1 1 calc R . . C37 C 0.9866(6) 0.1677(3) 0.9988(4) 0.053(2) Uani 1 1 d . . . H37 H 1.0208 0.1559 1.0345 0.064 Uiso 1 1 calc R . . C38 C 0.9221(6) 0.2133(3) 0.9988(3) 0.049(2) Uani 1 1 d . . . H38 H 0.9109 0.2324 1.0346 0.058 Uiso 1 1 calc R . . C39 C 0.8746(5) 0.2303(3) 0.9464(3) 0.0348(16) Uani 1 1 d . . . H39 H 0.8315 0.2619 0.9466 0.042 Uiso 1 1 calc R . . C40 C 1.3107(6) 0.1397(4) 0.7614(4) 0.066(3) Uani 1 1 d . . . H40A H 1.3077 0.1659 0.7948 0.098 Uiso 1 1 calc R . . H40B H 1.3467 0.1576 0.7307 0.098 Uiso 1 1 calc R . . H40C H 1.344 0.1046 0.7748 0.098 Uiso 1 1 calc R . . C41 C 1.1885(6) 0.0730(3) 0.6685(4) 0.057(2) Uani 1 1 d . . . H41A H 1.1216 0.0644 0.6536 0.086 Uiso 1 1 calc R . . H41B H 1.2215 0.0377 0.6815 0.086 Uiso 1 1 calc R . . H41C H 1.2235 0.0906 0.6371 0.086 Uiso 1 1 calc R . . C42 C 1.1235(6) 0.0882(4) 0.7916(4) 0.061(2) Uani 1 1 d . . . H42A H 1.0567 0.0785 0.7772 0.092 Uiso 1 1 calc R . . H42B H 1.1222 0.1144 0.825 0.092 Uiso 1 1 calc R . . H42C H 1.1584 0.0533 0.8041 0.092 Uiso 1 1 calc R . . C43 C 0.8804(4) 0.3601(3) 0.6828(3) 0.0267(14) Uani 1 1 d . . . C44 C 0.9398(4) 0.3174(3) 0.6642(2) 0.0267(14) Uani 1 1 d . . . H44 H 0.9199 0.2789 0.6678 0.032 Uiso 1 1 calc R . . C45 C 1.0290(5) 0.3290(3) 0.6399(3) 0.0329(15) Uani 1 1 d . . . C46 C 1.0587(5) 0.3865(3) 0.6362(3) 0.0355(16) Uani 1 1 d . . . H46 H 1.1185 0.3955 0.6198 0.043 Uiso 1 1 calc R . . C47 C 1.0015(5) 0.4290(3) 0.6561(3) 0.0358(16) Uani 1 1 d . . . H47 H 1.023 0.4674 0.654 0.043 Uiso 1 1 calc R . . C48 C 0.9129(5) 0.4177(3) 0.6793(3) 0.0345(16) Uani 1 1 d . . . H48 H 0.8743 0.448 0.6927 0.041 Uiso 1 1 calc R . . C49 C 0.6913(5) 0.4057(3) 0.6944(3) 0.0334(15) Uani 1 1 d . . . C50 C 0.6794(6) 0.4217(3) 0.6357(3) 0.055(2) Uani 1 1 d . . . H50 H 0.7139 0.4015 0.6075 0.066 Uiso 1 1 calc R . . C51 C 0.6189(6) 0.4660(3) 0.6169(4) 0.058(2) Uani 1 1 d . . . H51 H 0.6121 0.4759 0.5763 0.07 Uiso 1 1 calc R . . C52 C 0.5695(6) 0.4954(3) 0.6563(4) 0.058(2) Uani 1 1 d . . . H52 H 0.528 0.526 0.6435 0.07 Uiso 1 1 calc R . . C53 C 0.5798(6) 0.4806(3) 0.7155(4) 0.060(2) Uani 1 1 d . . . H53 H 0.5449 0.501 0.7433 0.072 Uiso 1 1 calc R . . C54 C 0.6412(6) 0.4360(3) 0.7343(4) 0.053(2) Uani 1 1 d . . . H54 H 0.6484 0.4264 0.775 0.064 Uiso 1 1 calc R . . C55 C 0.7079(4) 0.2900(3) 0.6697(3) 0.0295(15) Uani 1 1 d . . . C56 C 0.7279(5) 0.2791(3) 0.6124(3) 0.0405(17) Uani 1 1 d . . . H56 H 0.7788 0.2995 0.5958 0.049 Uiso 1 1 calc R . . C57 C 0.6761(6) 0.2392(3) 0.5782(3) 0.054(2) Uani 1 1 d . . . H57 H 0.6918 0.2324 0.5388 0.064 Uiso 1 1 calc R . . C58 C 0.6017(6) 0.2094(3) 0.6015(4) 0.055(2) Uani 1 1 d . . . H58 H 0.5665 0.1812 0.5787 0.066 Uiso 1 1 calc R . . C59 C 0.5793(5) 0.2207(3) 0.6577(4) 0.049(2) Uani 1 1 d . . . H59 H 0.5265 0.2011 0.6733 0.059 Uiso 1 1 calc R . . C60 C 0.6313(5) 0.2604(3) 0.6931(3) 0.0359(16) Uani 1 1 d . . . H60 H 0.6151 0.2671 0.7325 0.043 Uiso 1 1 calc R . . C61 C 0.9425(6) 0.2689(5) 0.5194(4) 0.074(3) Uani 1 1 d . . . H61A H 0.915 0.3066 0.5267 0.111 Uiso 1 1 calc R . . H61B H 0.9086 0.2401 0.5414 0.111 Uiso 1 1 calc R . . H61C H 0.9343 0.2603 0.4771 0.111 Uiso 1 1 calc R . . C62 C 1.1411(7) 0.3239(4) 0.5049(4) 0.075(3) Uani 1 1 d . . . H62A H 1.1138 0.3614 0.5129 0.113 Uiso 1 1 calc R . . H62B H 1.1344 0.3164 0.4623 0.113 Uiso 1 1 calc R . . H62C H 1.2102 0.3231 0.5187 0.113 Uiso 1 1 calc R . . C63 C 1.1248(8) 0.1967(4) 0.5293(4) 0.081(3) Uani 1 1 d . . . H63A H 1.0888 0.1678 0.5501 0.121 Uiso 1 1 calc R . . H63B H 1.1938 0.1953 0.5433 0.121 Uiso 1 1 calc R . . H63C H 1.1181 0.189 0.4868 0.121 Uiso 1 1 calc R . . C64 C 0.6726(5) 0.3485(3) 0.8579(3) 0.0366(16) Uani 1 1 d . . . C65 C 1.3804(11) 0.0356(10) 1.0079(8) 0.260(4) Uiso 1 1 d G A 1 H65 H 1.437 0.0422 1.0334 0.312 Uiso 1 1 calc R A 1 C66 C 1.3274(17) -0.0144(8) 1.0130(7) 0.260(4) Uiso 1 1 d G A 1 H66 H 1.3478 -0.0419 1.042 0.312 Uiso 1 1 calc R A 1 C67 C 1.2446(15) -0.0241(7) 0.9757(10) 0.260(4) Uiso 1 1 d G A 1 H67 H 1.2083 -0.0582 0.9792 0.312 Uiso 1 1 calc R A 1 C68 C 1.2147(10) 0.0162(10) 0.9333(8) 0.260(4) Uiso 1 1 d G A 1 H68 H 1.1581 0.0095 0.9078 0.312 Uiso 1 1 calc R A 1 C69 C 1.2678(16) 0.0661(8) 0.9282(7) 0.260(4) Uiso 1 1 d G A 1 H69 H 1.2474 0.0936 0.8992 0.312 Uiso 1 1 calc R A 1 C70 C 1.3506(15) 0.0758(7) 0.9655(10) 0.260(4) Uiso 1 1 d G A 1 H70 H 1.3868 0.11 0.9621 0.312 Uiso 1 1 calc R A 1 C71 C 1.2669(11) 0.4294(9) 0.9848(9) 0.260(4) Uiso 1 1 d G B 1 H71 H 1.201 0.4233 0.9708 0.312 Uiso 1 1 calc R B 1 C72 C 1.2897(15) 0.4704(8) 1.0278(9) 0.260(4) Uiso 1 1 d G B 1 H72 H 1.2393 0.4923 1.0431 0.312 Uiso 1 1 calc R B 1 C73 C 1.3861(19) 0.4792(7) 1.0482(6) 0.260(4) Uiso 1 1 d G B 1 H73 H 1.4016 0.5072 1.0776 0.312 Uiso 1 1 calc R B 1 C74 C 1.4597(11) 0.4471(9) 1.0257(9) 0.260(4) Uiso 1 1 d G B 1 H74 H 1.5256 0.4531 1.0397 0.312 Uiso 1 1 calc R B 1 C75 C 1.4370(15) 0.4061(8) 0.9827(9) 0.260(4) Uiso 1 1 d G B 1 H75 H 1.4873 0.3842 0.9673 0.312 Uiso 1 1 calc R B 1 C76 C 1.3406(19) 0.3973(7) 0.9622(6) 0.260(4) Uiso 1 1 d G B 1 H76 H 1.325 0.3693 0.9329 0.312 Uiso 1 1 calc R B 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 Pt 0.02549(13) 0.02262(13) 0.02756(14) -0.00067(11) 0.00444(9) 0.00068(11) Ti 0.0292(6) 0.0298(6) 0.0323(7) -0.0026(5) 0.0092(5) 0.0007(5) Cl 0.0469(11) 0.0569(12) 0.0703(14) -0.0081(10) 0.0300(10) 0.0031(9) P1 0.0293(9) 0.0212(8) 0.0252(9) -0.0017(7) 0.0033(7) -0.0015(7) P2 0.0269(8) 0.0221(8) 0.0293(9) -0.0009(7) 0.0039(7) -0.0008(7) P3 0.0282(9) 0.0240(8) 0.0296(9) 0.0005(7) 0.0010(7) 0.0035(7) Si1 0.0321(10) 0.0361(11) 0.0511(13) -0.0070(9) 0.0112(9) -0.0069(9) Si2 0.0295(10) 0.0301(10) 0.0464(12) -0.0016(9) 0.0029(9) 0.0029(8) Si3 0.0484(12) 0.0662(15) 0.0314(11) -0.0094(10) 0.0063(9) 0.0128(11) O 0.042(3) 0.087(4) 0.051(3) 0.000(3) 0.018(3) 0.018(3) N1 0.026(3) 0.030(3) 0.037(3) -0.003(2) 0.005(2) -0.001(2) N2 0.031(3) 0.028(3) 0.036(3) -0.006(2) 0.007(2) 0.000(2) N3 0.036(3) 0.034(3) 0.028(3) 0.001(2) 0.007(2) 0.005(3) C1 0.030(3) 0.023(3) 0.030(3) -0.003(3) -0.001(3) -0.001(3) C2 0.029(3) 0.024(3) 0.027(3) -0.001(3) -0.001(3) -0.005(3) C3 0.029(3) 0.025(3) 0.029(4) -0.004(3) 0.002(3) -0.003(3) C4 0.025(3) 0.030(3) 0.037(4) -0.002(3) 0.004(3) 0.005(3) C5 0.038(4) 0.038(4) 0.041(4) 0.007(3) 0.001(3) 0.002(3) C6 0.033(4) 0.030(3) 0.034(4) 0.001(3) 0.007(3) -0.001(3) C7 0.042(4) 0.021(3) 0.028(4) -0.005(3) 0.003(3) 0.002(3) C8 0.051(4) 0.042(4) 0.034(4) -0.008(3) 0.000(3) -0.008(4) C9 0.071(6) 0.049(5) 0.035(4) -0.009(4) -0.005(4) -0.006(4) C10 0.106(8) 0.045(5) 0.028(4) -0.010(4) 0.000(5) 0.003(5) C11 0.079(6) 0.065(6) 0.040(5) -0.007(4) 0.027(4) -0.004(5) C12 0.051(5) 0.054(5) 0.037(4) -0.009(4) 0.013(4) -0.007(4) C13 0.038(4) 0.023(3) 0.021(3) -0.004(3) 0.004(3) -0.001(3) C14 0.041(4) 0.028(4) 0.041(4) -0.003(3) 0.005(3) -0.007(3) C15 0.052(5) 0.040(4) 0.044(4) -0.001(3) 0.004(4) -0.018(4) C16 0.072(6) 0.027(4) 0.044(5) 0.005(3) -0.005(4) -0.010(4) C17 0.056(5) 0.027(4) 0.069(6) 0.008(4) 0.000(4) 0.010(4) C18 0.037(4) 0.029(4) 0.056(5) 0.007(3) 0.003(3) 0.003(3) C19 0.057(5) 0.075(6) 0.059(6) 0.013(5) 0.013(4) -0.021(5) C20 0.034(4) 0.082(6) 0.079(6) 0.000(5) -0.002(4) -0.013(4) C21 0.068(6) 0.043(5) 0.112(8) -0.025(5) 0.035(5) -0.019(4) C22 0.027(3) 0.021(3) 0.032(4) 0.005(3) -0.003(3) -0.001(3) C23 0.031(3) 0.019(3) 0.032(4) 0.000(3) -0.002(3) -0.001(3) C24 0.033(3) 0.017(3) 0.031(3) 0.002(3) 0.003(3) -0.001(3) C25 0.038(4) 0.033(4) 0.030(4) -0.005(3) 0.003(3) 0.009(3) C26 0.029(4) 0.037(4) 0.039(4) -0.011(3) -0.004(3) 0.003(3) C27 0.027(3) 0.027(4) 0.036(4) -0.004(3) -0.003(3) 0.000(3) C28 0.031(3) 0.031(3) 0.028(3) 0.000(3) 0.004(3) -0.005(3) C29 0.035(4) 0.028(4) 0.055(5) -0.004(3) 0.009(3) -0.004(3) C30 0.057(5) 0.032(4) 0.054(5) -0.001(4) 0.005(4) -0.017(4) C31 0.044(5) 0.053(5) 0.048(5) -0.002(4) 0.002(4) -0.030(4) C32 0.031(4) 0.056(5) 0.041(4) 0.003(4) 0.003(3) -0.011(4) C33 0.033(4) 0.036(4) 0.032(4) 0.000(3) -0.001(3) -0.001(3) C34 0.029(3) 0.026(3) 0.034(4) 0.003(3) 0.006(3) -0.003(3) C35 0.050(4) 0.034(4) 0.040(4) 0.003(3) 0.000(3) 0.008(3) C36 0.061(5) 0.049(5) 0.048(5) 0.010(4) -0.004(4) 0.020(4) C37 0.055(5) 0.061(5) 0.042(5) 0.021(4) -0.006(4) 0.008(4) C38 0.060(5) 0.058(5) 0.029(4) 0.004(4) 0.005(4) -0.004(4) C39 0.035(4) 0.033(4) 0.037(4) -0.002(3) 0.008(3) 0.000(3) C40 0.043(5) 0.047(5) 0.104(7) -0.014(5) -0.010(5) 0.005(4) C41 0.069(6) 0.035(4) 0.067(6) -0.013(4) 0.007(4) 0.012(4) C42 0.058(5) 0.060(5) 0.066(6) 0.027(5) 0.011(4) 0.017(4) C43 0.032(3) 0.026(3) 0.022(3) 0.000(3) 0.003(3) 0.003(3) C44 0.034(3) 0.027(3) 0.019(3) 0.003(3) 0.001(3) -0.002(3) C45 0.036(4) 0.037(4) 0.026(3) 0.002(3) 0.003(3) 0.010(3) C46 0.035(4) 0.038(4) 0.035(4) 0.012(3) 0.008(3) -0.001(3) C47 0.038(4) 0.026(3) 0.044(4) 0.000(3) 0.004(3) -0.002(3) C48 0.047(4) 0.029(4) 0.029(4) -0.003(3) 0.008(3) 0.004(3) C49 0.037(4) 0.027(3) 0.037(4) 0.005(3) -0.001(3) 0.011(3) C50 0.071(6) 0.051(5) 0.044(5) 0.004(4) 0.003(4) 0.025(4) C51 0.071(6) 0.056(5) 0.047(5) 0.011(4) -0.001(4) 0.026(5) C52 0.059(5) 0.047(5) 0.067(6) 0.023(4) -0.005(4) 0.025(4) C53 0.070(6) 0.044(5) 0.067(6) 0.003(4) 0.015(5) 0.034(4) C54 0.060(5) 0.051(5) 0.050(5) 0.009(4) 0.011(4) 0.019(4) C55 0.028(3) 0.025(3) 0.035(4) -0.001(3) -0.005(3) 0.004(3) C56 0.037(4) 0.047(4) 0.038(4) -0.005(3) 0.001(3) -0.004(3) C57 0.064(5) 0.056(5) 0.039(5) -0.016(4) -0.007(4) 0.002(4) C58 0.050(5) 0.049(5) 0.062(6) -0.013(4) -0.025(4) -0.006(4) C59 0.035(4) 0.044(5) 0.066(6) 0.005(4) -0.010(4) -0.004(4) C60 0.028(4) 0.038(4) 0.041(4) 0.000(3) -0.003(3) 0.002(3) C61 0.061(6) 0.111(8) 0.048(5) -0.025(5) -0.005(4) 0.006(6) C62 0.077(6) 0.110(8) 0.041(5) 0.010(5) 0.015(4) 0.008(6) C63 0.108(8) 0.086(7) 0.049(6) -0.030(5) 0.010(5) 0.029(6) C64 0.034(4) 0.041(4) 0.036(4) 0.001(3) 0.007(3) 0.000(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C64 1.884(7) . ? Pt P2 2.3313(16) . ? Pt P1 2.3348(16) . ? Pt P3 2.3370(17) . ? Ti N3 1.894(5) . ? Ti N2 1.904(5) . ? Ti N1 1.905(5) . ? Ti Cl 2.246(2) . ? P1 C13 1.840(6) . ? P1 C7 1.841(6) . ? P1 C1 1.849(6) . ? P2 C22 1.834(7) . ? P2 C34 1.841(6) . ? P2 C28 1.850(6) . ? P3 C43 1.825(6) . ? P3 C55 1.847(6) . ? P3 C49 1.848(6) . ? Si1 N1 1.771(5) . ? Si1 C19 1.849(8) . ? Si1 C20 1.853(8) . ? Si1 C21 1.862(8) . ? Si2 N2 1.762(5) . ? Si2 C40 1.837(8) . ? Si2 C41 1.846(7) . ? Si2 C42 1.854(8) . ? Si3 N3 1.774(5) . ? Si3 C62 1.850(9) . ? Si3 C63 1.860(9) . ? Si3 C61 1.868(8) . ? O C64 1.166(8) . ? N1 C3 1.445(8) . ? N2 C24 1.454(8) . ? N3 C45 1.437(8) . ? C1 C6 1.386(9) . ? C1 C2 1.388(8) . ? C2 C3 1.392(8) . ? C3 C4 1.388(9) . ? C4 C5 1.365(9) . ? C5 C6 1.393(9) . ? C7 C8 1.384(9) . ? C7 C12 1.385(9) . ? C8 C9 1.393(10) . ? C9 C10 1.359(12) . ? C10 C11 1.376(12) . ? C11 C12 1.396(10) . ? C13 C14 1.383(9) . ? C13 C18 1.388(9) . ? C14 C15 1.383(9) . ? C15 C16 1.375(11) . ? C16 C17 1.365(11) . ? C17 C18 1.383(9) . ? C22 C23 1.384(8) . ? C22 C27 1.389(8) . ? C23 C24 1.395(8) . ? C24 C25 1.388(9) . ? C25 C26 1.375(9) . ? C26 C27 1.384(9) . ? C28 C29 1.390(9) . ? C28 C33 1.397(9) . ? C29 C30 1.390(9) . ? C30 C31 1.369(11) . ? C31 C32 1.377(10) . ? C32 C33 1.386(9) . ? C34 C39 1.388(9) . ? C34 C35 1.394(9) . ? C35 C36 1.378(10) . ? C36 C37 1.381(11) . ? C37 C38 1.389(11) . ? C38 C39 1.377(9) . ? C43 C44 1.379(8) . ? C43 C48 1.427(9) . ? C44 C45 1.408(9) . ? C45 C46 1.413(9) . ? C46 C47 1.369(9) . ? C47 C48 1.388(9) . ? C49 C54 1.377(10) . ? C49 C50 1.382(10) . ? C50 C51 1.382(10) . ? C51 C52 1.351(11) . ? C52 C53 1.387(11) . ? C53 C54 1.394(10) . ? C55 C56 1.373(9) . ? C55 C60 1.399(9) . ? C56 C57 1.381(10) . ? C57 C58 1.377(11) . ? C58 C59 1.361(11) . ? C59 C60 1.394(10) . ? C65 C66 1.39 . ? C65 C70 1.39 . ? C66 C67 1.39 . ? C67 C68 1.39 . ? C68 C69 1.39 . ? C69 C70 1.39 . ? C71 C72 1.39 . ? C71 C76 1.39 . ? C72 C73 1.39 . ? C73 C74 1.39 . ? C74 C75 1.39 . ? C75 C76 1.39 . ? 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 C64 Pt P2 114.7(2) . . ? C64 Pt P1 111.1(2) . . ? P2 Pt P1 105.36(6) . . ? C64 Pt P3 112.7(2) . . ? P2 Pt P3 106.06(6) . . ? P1 Pt P3 106.25(6) . . ? N3 Ti N2 108.5(2) . . ? N3 Ti N1 109.3(2) . . ? N2 Ti N1 109.0(2) . . ? N3 Ti Cl 112.31(17) . . ? N2 Ti Cl 107.48(17) . . ? N1 Ti Cl 110.18(17) . . ? C13 P1 C7 96.9(3) . . ? C13 P1 C1 104.7(3) . . ? C7 P1 C1 102.0(3) . . ? C13 P1 Pt 114.5(2) . . ? C7 P1 Pt 117.3(2) . . ? C1 P1 Pt 118.41(19) . . ? C22 P2 C34 104.0(3) . . ? C22 P2 C28 102.4(3) . . ? C34 P2 C28 97.5(3) . . ? C22 P2 Pt 116.82(19) . . ? C34 P2 Pt 116.4(2) . . ? C28 P2 Pt 117.0(2) . . ? C43 P3 C55 103.7(3) . . ? C43 P3 C49 101.4(3) . . ? C55 P3 C49 97.9(3) . . ? C43 P3 Pt 117.8(2) . . ? C55 P3 Pt 116.4(2) . . ? C49 P3 Pt 116.8(2) . . ? N1 Si1 C19 111.4(3) . . ? N1 Si1 C20 109.2(3) . . ? C19 Si1 C20 108.7(4) . . ? N1 Si1 C21 108.9(3) . . ? C19 Si1 C21 108.9(4) . . ? C20 Si1 C21 109.7(5) . . ? N2 Si2 C40 111.4(3) . . ? N2 Si2 C41 109.8(3) . . ? C40 Si2 C41 111.1(4) . . ? N2 Si2 C42 108.3(3) . . ? C40 Si2 C42 107.1(4) . . ? C41 Si2 C42 109.1(4) . . ? N3 Si3 C62 108.4(4) . . ? N3 Si3 C63 109.8(3) . . ? C62 Si3 C63 110.5(5) . . ? N3 Si3 C61 108.9(3) . . ? C62 Si3 C61 110.9(5) . . ? C63 Si3 C61 108.4(5) . . ? C3 N1 Si1 115.3(4) . . ? C3 N1 Ti 120.7(4) . . ? Si1 N1 Ti 123.6(3) . . ? C24 N2 Si2 114.2(4) . . ? C24 N2 Ti 122.0(4) . . ? Si2 N2 Ti 123.2(3) . . ? C45 N3 Si3 114.9(4) . . ? C45 N3 Ti 119.1(4) . . ? Si3 N3 Ti 125.7(3) . . ? C6 C1 C2 119.3(6) . . ? C6 C1 P1 119.6(5) . . ? C2 C1 P1 120.8(5) . . ? C1 C2 C3 121.1(6) . . ? C4 C3 C2 118.8(6) . . ? C4 C3 N1 120.6(5) . . ? C2 C3 N1 120.5(5) . . ? C5 C4 C3 120.3(6) . . ? C4 C5 C6 121.1(6) . . ? C1 C6 C5 119.4(6) . . ? C8 C7 C12 118.2(6) . . ? C8 C7 P1 121.7(5) . . ? C12 C7 P1 120.0(5) . . ? C7 C8 C9 121.3(7) . . ? C10 C9 C8 119.3(8) . . ? C9 C10 C11 121.0(7) . . ? C10 C11 C12 119.4(8) . . ? C7 C12 C11 120.7(7) . . ? C14 C13 C18 117.7(6) . . ? C14 C13 P1 125.8(5) . . ? C18 C13 P1 116.5(5) . . ? C13 C14 C15 120.5(7) . . ? C16 C15 C14 120.9(7) . . ? C17 C16 C15 119.3(7) . . ? C16 C17 C18 120.0(7) . . ? C17 C18 C13 121.5(7) . . ? C23 C22 C27 118.4(6) . . ? C23 C22 P2 120.5(5) . . ? C27 C22 P2 120.8(5) . . ? C22 C23 C24 121.2(6) . . ? C25 C24 C23 119.3(6) . . ? C25 C24 N2 120.7(6) . . ? C23 C24 N2 119.9(5) . . ? C26 C25 C24 119.8(6) . . ? C25 C26 C27 120.4(6) . . ? C26 C27 C22 120.7(6) . . ? C29 C28 C33 118.7(6) . . ? C29 C28 P2 121.1(5) . . ? C33 C28 P2 120.1(5) . . ? C28 C29 C30 120.2(7) . . ? C31 C30 C29 120.3(7) . . ? C30 C31 C32 120.4(7) . . ? C31 C32 C33 119.8(7) . . ? C32 C33 C28 120.6(6) . . ? C39 C34 C35 117.0(6) . . ? C39 C34 P2 118.5(5) . . ? C35 C34 P2 124.4(5) . . ? C36 C35 C34 121.6(7) . . ? C35 C36 C37 119.9(7) . . ? C36 C37 C38 119.9(7) . . ? C39 C38 C37 119.1(7) . . ? C38 C39 C34 122.5(6) . . ? C44 C43 C48 118.4(6) . . ? C44 C43 P3 121.7(5) . . ? C48 C43 P3 119.7(5) . . ? C43 C44 C45 122.2(6) . . ? C44 C45 C46 118.2(6) . . ? C44 C45 N3 120.3(6) . . ? C46 C45 N3 121.5(6) . . ? C47 C46 C45 120.0(6) . . ? C46 C47 C48 121.9(6) . . ? C47 C48 C43 119.3(6) . . ? C54 C49 C50 117.7(6) . . ? C54 C49 P3 120.9(5) . . ? C50 C49 P3 121.4(5) . . ? C51 C50 C49 122.0(7) . . ? C52 C51 C50 120.0(8) . . ? C51 C52 C53 119.5(7) . . ? C52 C53 C54 120.2(8) . . ? C49 C54 C53 120.5(7) . . ? C56 C55 C60 118.3(6) . . ? C56 C55 P3 125.6(5) . . ? C60 C55 P3 115.9(5) . . ? C55 C56 C57 122.0(7) . . ? C58 C57 C56 119.7(8) . . ? C59 C58 C57 119.0(7) . . ? C58 C59 C60 122.1(7) . . ? C59 C60 C55 118.8(7) . . ? O C64 Pt 179.0(7) . . ? C66 C65 C70 120 . . ? C67 C66 C65 120 . . ? C68 C67 C66 120 . . ? C67 C68 C69 120 . . ? C70 C69 C68 120 . . ? C69 C70 C65 120 . . ? C72 C71 C76 120 . . ? C71 C72 C73 120 . . ? C72 C73 C74 120 . . ? C75 C74 C73 120 . . ? C74 C75 C76 120 . . ? C75 C76 C71 120 . . ? data_sep2301 _database_code_depnum_ccdc_archive 'CCDC 231691' _audit_creation_date 2001-09-28T09:17:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Me2Pt{PPh2C6H4NCHtBu2}2TiCl2].3.5(CH2Cl2)' ; _chemical_formula_moiety ; '(C56 H72 Cl2 N2 P2 Pt1 Ti1).3.5(C1 H2 Cl2)' ; _chemical_formula_sum 'C59.50 H79 Cl9 N2 P2 Pt Ti' _chemical_formula_weight 1446.23 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6890(13) _cell_length_b 16.2783(17) _cell_length_c 16.5855(15) _cell_angle_alpha 83.286(5) _cell_angle_beta 68.986(5) _cell_angle_gamma 69.327(5) _cell_volume 3227.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34973 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1466 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 0.662 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 15526 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_unetI/netI 0.0791 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 22.92 _diffrn_reflns_theta_full 22.92 _diffrn_measured_fraction_theta_full 0.947 _diffrn_measured_fraction_theta_max 0.947 _reflns_number_total 8411 _reflns_number_gt 7141 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; ******************************************************************************* The C55 and C56 methyl C ellipsoids are slightly small and flattened. It seems probable that this is due to a small (ca. 5%) incorporation of the dichloro analogue in the crystal. For this reason the Pt-Me bond distances are unreliable. *********************************************************************** There are poorly defined solvate molecules; 3 in general positions which were refined with distance constraints, and one apparently disordered across an inversion centre for which the C atom could not be located. 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^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8411 _refine_ls_number_parameters 659 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1633 _refine_ls_goodness_of_fit_ref 1.381 _refine_ls_restrained_S_all 1.422 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.755 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.127 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' 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 Pt Pt 0.54657(3) 0.73842(3) 0.57043(2) 0.04561(18) Uani 1 1 d . . . Ti Ti 0.48797(13) 0.74879(11) 1.04765(10) 0.0390(4) Uani 1 1 d . . . Cl1 Cl 0.4673(2) 0.63760(18) 1.13956(16) 0.0597(7) Uani 1 1 d . . . Cl2 Cl 0.4949(2) 0.84649(18) 1.13006(16) 0.0577(7) Uani 1 1 d . . . P1 P 0.4018(2) 0.82790(16) 0.67752(14) 0.0406(6) Uani 1 1 d . . . P2 P 0.6890(2) 0.72040(17) 0.61993(14) 0.0431(6) Uani 1 1 d . . . N1 N 0.3610(6) 0.8015(5) 1.0147(4) 0.0357(17) Uani 1 1 d . . . N2 N 0.6244(5) 0.7094(5) 0.9572(4) 0.0365(17) Uani 1 1 d . . . C1 C 0.3962(7) 0.7747(6) 0.7831(5) 0.037(2) Uani 1 1 d . . . C2 C 0.3767(7) 0.8154(6) 0.8582(6) 0.038(2) Uani 1 1 d . . . H2 H 0.3648 0.8765 0.8589 0.045 Uiso 1 1 calc R . . C3 C 0.3745(7) 0.7659(6) 0.9340(5) 0.034(2) Uani 1 1 d . . . C4 C 0.3968(7) 0.6755(6) 0.9305(6) 0.038(2) Uani 1 1 d . . . H4 H 0.3986 0.641 0.9806 0.046 Uiso 1 1 calc R . . C5 C 0.4165(7) 0.6356(6) 0.8535(6) 0.046(2) Uani 1 1 d . . . H5 H 0.4303 0.5743 0.8516 0.055 Uiso 1 1 calc R . . C6 C 0.4160(7) 0.6847(6) 0.7808(6) 0.045(2) Uani 1 1 d . . . H6 H 0.4292 0.6575 0.7285 0.054 Uiso 1 1 calc R . . C7 C 0.4019(8) 0.9393(6) 0.6821(6) 0.045(2) Uani 1 1 d . . . C8 C 0.3191(9) 1.0011(7) 0.7453(6) 0.051(3) Uani 1 1 d . . . H8 H 0.261 0.9843 0.7872 0.062 Uiso 1 1 calc R . . C9 C 0.3196(11) 1.0853(7) 0.7484(7) 0.069(3) Uani 1 1 d . . . H9 H 0.2663 1.1248 0.7939 0.083 Uiso 1 1 calc R . . C10 C 0.4019(11) 1.1106(8) 0.6819(8) 0.070(3) Uani 1 1 d . . . H10 H 0.4044 1.1682 0.6816 0.083 Uiso 1 1 calc R . . C11 C 0.4782(10) 1.0518(8) 0.6175(7) 0.061(3) Uani 1 1 d . . . H11 H 0.5308 1.0709 0.5716 0.073 Uiso 1 1 calc R . . C12 C 0.4818(9) 0.9661(7) 0.6166(6) 0.049(2) Uani 1 1 d . . . H12 H 0.5376 0.9263 0.5723 0.058 Uiso 1 1 calc R . . C13 C 0.2580(8) 0.8522(7) 0.6786(6) 0.047(2) Uani 1 1 d . . . C14 C 0.1886(9) 0.8127(9) 0.7330(7) 0.070(3) Uani 1 1 d . . . H14 H 0.2116 0.7728 0.7746 0.083 Uiso 1 1 calc R . . C15 C 0.0843(11) 0.8295(10) 0.7290(9) 0.086(4) Uani 1 1 d . . . H15 H 0.0371 0.8 0.7672 0.103 Uiso 1 1 calc R . . C16 C 0.0474(10) 0.8881(9) 0.6707(8) 0.073(3) Uani 1 1 d . . . H16 H -0.0251 0.901 0.669 0.088 Uiso 1 1 calc R . . C17 C 0.1195(10) 0.9271(8) 0.6153(8) 0.069(3) Uani 1 1 d . . . H17 H 0.0982 0.9657 0.5723 0.082 Uiso 1 1 calc R . . C18 C 0.2213(9) 0.9111(8) 0.6211(7) 0.064(3) Uani 1 1 d . . . H18 H 0.268 0.9417 0.5842 0.077 Uiso 1 1 calc R . . C19 C 0.2545(7) 0.8653(6) 1.0696(6) 0.049(2) Uani 1 1 d . . . H19 H 0.2703 0.8643 1.1242 0.059 Uiso 1 1 calc R . . C20 C 0.2334(7) 0.9648(6) 1.0440(6) 0.042(2) Uani 1 1 d . . . C21 C 0.1815(10) 1.0215(8) 1.1259(7) 0.068(3) Uani 1 1 d . . . H21A H 0.1106 1.0137 1.1609 0.102 Uiso 1 1 calc R . . H21B H 0.1687 1.0833 1.11 0.102 Uiso 1 1 calc R . . H21C H 0.2318 1.0037 1.1592 0.102 Uiso 1 1 calc R . . C22 C 0.1574(8) 0.9990(7) 0.9889(7) 0.060(3) Uani 1 1 d . . . H22A H 0.1898 0.9633 0.936 0.09 Uiso 1 1 calc R . . H22B H 0.1503 1.0603 0.9737 0.09 Uiso 1 1 calc R . . H22C H 0.0839 0.995 1.022 0.09 Uiso 1 1 calc R . . C23 C 0.3426(7) 0.9812(6) 0.9939(6) 0.046(2) Uani 1 1 d . . . H23A H 0.3799 0.9465 0.9402 0.068 Uiso 1 1 calc R . . H23B H 0.3907 0.964 1.0291 0.068 Uiso 1 1 calc R . . H23C H 0.3273 1.0438 0.9802 0.068 Uiso 1 1 calc R . . C24 C 0.1544(7) 0.8263(6) 1.1023(6) 0.047(2) Uani 1 1 d . . . C25 C 0.1199(8) 0.8106(8) 1.0255(7) 0.062(3) Uani 1 1 d . . . H25A H 0.0964 0.8664 0.9966 0.094 Uiso 1 1 calc R . . H25B H 0.0585 0.7872 1.0483 0.094 Uiso 1 1 calc R . . H25C H 0.1836 0.7686 0.984 0.094 Uiso 1 1 calc R . . C26 C 0.0511(9) 0.8868(8) 1.1683(7) 0.070(3) Uani 1 1 d . . . H26A H 0.0258 0.9439 1.1421 0.106 Uiso 1 1 calc R . . H26B H 0.0689 0.8946 1.2185 0.106 Uiso 1 1 calc R . . H26C H -0.0078 0.8606 1.1867 0.106 Uiso 1 1 calc R . . C27 C 0.1902(9) 0.7393(8) 1.1441(8) 0.069(3) Uani 1 1 d . . . H27A H 0.2566 0.6993 1.1026 0.104 Uiso 1 1 calc R . . H27B H 0.1303 0.7143 1.1623 0.104 Uiso 1 1 calc R . . H27C H 0.2072 0.7475 1.1946 0.104 Uiso 1 1 calc R . . C28 C 0.6626(7) 0.7675(6) 0.7247(5) 0.036(2) Uani 1 1 d . . . C29 C 0.6582(7) 0.7184(6) 0.7991(5) 0.037(2) Uani 1 1 d . . . H29 H 0.6739 0.6569 0.7961 0.045 Uiso 1 1 calc R . . C30 C 0.6316(6) 0.7566(5) 0.8769(5) 0.0323(19) Uani 1 1 d . . . C31 C 0.6066(7) 0.8470(5) 0.8816(5) 0.0343(19) Uani 1 1 d . . . H31 H 0.5859 0.8743 0.9356 0.041 Uiso 1 1 calc R . . C32 C 0.6121(7) 0.8977(6) 0.8068(6) 0.044(2) Uani 1 1 d . . . H32 H 0.5955 0.9593 0.8098 0.052 Uiso 1 1 calc R . . C33 C 0.6417(7) 0.8572(6) 0.7290(6) 0.042(2) Uani 1 1 d . . . H33 H 0.6478 0.891 0.6778 0.051 Uiso 1 1 calc R . . C34 C 0.7661(9) 0.6033(6) 0.6302(6) 0.053(3) Uani 1 1 d . . . C35 C 0.7052(10) 0.5471(8) 0.6651(7) 0.067(3) Uani 1 1 d . . . H35 H 0.6264 0.5703 0.6842 0.081 Uiso 1 1 calc R . . C36 C 0.7566(12) 0.4593(8) 0.6726(8) 0.078(4) Uani 1 1 d . . . H36 H 0.7134 0.4218 0.6951 0.094 Uiso 1 1 calc R . . C37 C 0.8705(13) 0.4249(9) 0.6476(8) 0.082(4) Uani 1 1 d . . . H37 H 0.9059 0.364 0.6543 0.098 Uiso 1 1 calc R . . C38 C 0.9338(10) 0.4791(8) 0.6127(7) 0.071(3) Uani 1 1 d . . . H38 H 1.0125 0.4552 0.5946 0.085 Uiso 1 1 calc R . . C39 C 0.8828(9) 0.5667(7) 0.6045(7) 0.059(3) Uani 1 1 d . . . H39 H 0.9266 0.6036 0.5811 0.071 Uiso 1 1 calc R . . C40 C 0.7929(7) 0.7687(6) 0.5471(5) 0.045(2) Uani 1 1 d . . . C41 C 0.7805(8) 0.8035(7) 0.4688(6) 0.057(3) Uani 1 1 d . . . H41 H 0.7197 0.8028 0.4544 0.068 Uiso 1 1 calc R . . C42 C 0.8592(9) 0.8396(8) 0.4112(7) 0.066(3) Uani 1 1 d . . . H42 H 0.8512 0.864 0.3581 0.079 Uiso 1 1 calc R . . C43 C 0.9449(9) 0.8392(8) 0.4321(7) 0.069(3) Uani 1 1 d . . . H43 H 0.9994 0.8611 0.392 0.083 Uiso 1 1 calc R . . C44 C 0.9567(9) 0.8077(8) 0.5102(7) 0.066(3) Uani 1 1 d . . . H44 H 1.0167 0.8104 0.5245 0.079 Uiso 1 1 calc R . . C45 C 0.8784(8) 0.7710(7) 0.5691(6) 0.057(3) Uani 1 1 d . . . H45 H 0.8858 0.7486 0.6229 0.069 Uiso 1 1 calc R . . C46 C 0.7248(7) 0.6399(6) 0.9700(6) 0.043(2) Uani 1 1 d . . . H46 H 0.6989 0.6324 1.0341 0.052 Uiso 1 1 calc R . . C47 C 0.7539(7) 0.5447(6) 0.9366(6) 0.042(2) Uani 1 1 d . . . C48 C 0.7884(8) 0.4759(7) 1.0028(7) 0.057(3) Uani 1 1 d . . . H48A H 0.7312 0.4911 1.06 0.086 Uiso 1 1 calc R . . H48B H 0.8592 0.4753 1.005 0.086 Uiso 1 1 calc R . . H48C H 0.7967 0.4176 0.9853 0.086 Uiso 1 1 calc R . . C49 C 0.8433(8) 0.5197(7) 0.8491(7) 0.061(3) Uani 1 1 d . . . H49A H 0.911 0.5272 0.8496 0.092 Uiso 1 1 calc R . . H49B H 0.818 0.5574 0.805 0.092 Uiso 1 1 calc R . . H49C H 0.8589 0.4582 0.8361 0.092 Uiso 1 1 calc R . . C50 C 0.6503(7) 0.5320(6) 0.9315(6) 0.046(2) Uani 1 1 d . . . H50A H 0.5899 0.5478 0.9872 0.069 Uiso 1 1 calc R . . H50B H 0.6675 0.4704 0.9177 0.069 Uiso 1 1 calc R . . H50C H 0.6273 0.5696 0.8863 0.069 Uiso 1 1 calc R . . C51 C 0.8235(8) 0.6771(6) 0.9547(7) 0.054(3) Uani 1 1 d . . . C52 C 0.8774(8) 0.7043(7) 0.8613(7) 0.062(3) Uani 1 1 d . . . H52A H 0.9076 0.6536 0.8224 0.093 Uiso 1 1 calc R . . H52B H 0.9375 0.725 0.8589 0.093 Uiso 1 1 calc R . . H52C H 0.8214 0.7515 0.8435 0.093 Uiso 1 1 calc R . . C53 C 0.9187(8) 0.6094(7) 0.9828(7) 0.062(3) Uani 1 1 d . . . H53A H 0.9496 0.5556 0.9481 0.093 Uiso 1 1 calc R . . H53B H 0.8892 0.5958 1.044 0.093 Uiso 1 1 calc R . . H53C H 0.9773 0.6344 0.9738 0.093 Uiso 1 1 calc R . . C54 C 0.7798(9) 0.7590(6) 1.0097(8) 0.061(3) Uani 1 1 d . . . H54A H 0.7446 0.7458 1.0702 0.091 Uiso 1 1 calc R . . H54B H 0.7251 0.8054 0.9898 0.091 Uiso 1 1 calc R . . H54C H 0.8415 0.7788 1.0048 0.091 Uiso 1 1 calc R . . C55 C 0.6750(8) 0.6455(7) 0.4689(5) 0.050(3) Uani 1 1 d . . . C56 C 0.4351(7) 0.7421(6) 0.5038(5) 0.034(2) Uani 1 1 d . . . C57 C 0.8262(11) 0.6102(10) 1.2456(11) 0.108(5) Uiso 1 1 d D A 1 H57A H 0.8148 0.5941 1.3069 0.13 Uiso 1 1 calc R A 1 H57B H 0.8752 0.5568 1.2098 0.13 Uiso 1 1 calc R A 1 C58 C 1.3129(14) 0.8492(8) 0.3491(13) 0.134(6) Uiso 1 1 d D B 1 H58A H 1.3602 0.8345 0.3856 0.16 Uiso 1 1 calc R B 1 H58B H 1.3626 0.8431 0.2881 0.16 Uiso 1 1 calc R B 1 C59 C 1.238(2) 0.594(3) 0.6542(12) 0.277(18) Uiso 1 1 d D C 1 H59A H 1.2995 0.539 0.6298 0.333 Uiso 1 1 calc R C 1 H59B H 1.2644 0.644 0.6318 0.333 Uiso 1 1 calc R C 1 Cl3 Cl 0.6973(3) 0.6475(3) 1.2296(2) 0.1180(15) Uani 1 1 d D A 1 Cl4 Cl 0.8911(4) 0.6888(3) 1.2189(4) 0.158(2) Uani 1 1 d D A 1 Cl5 Cl 1.2446(5) 0.7733(6) 0.3685(6) 0.270(6) Uani 1 1 d D B 1 Cl6 Cl 1.2278(6) 0.9580(6) 0.3686(5) 0.237(5) Uani 1 1 d D B 1 Cl7 Cl 1.1224(6) 0.6035(4) 0.6226(6) 0.212(4) Uani 1 1 d D C 1 Cl8 Cl 1.1950(7) 0.5924(5) 0.7692(6) 0.221(3) Uani 1 1 d D C 1 Cl9 Cl 1.4872(8) 0.4679(7) 0.6638(6) 0.126(3) Uani 0.5 1 d PD D 1 Cl10 Cl 1.5 0.5 0.5 0.48(2) Uani 1 2 d SD E 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 Pt 0.0550(3) 0.0521(3) 0.0335(2) 0.00552(17) -0.01291(19) -0.0263(2) Ti 0.0409(9) 0.0406(10) 0.0321(8) 0.0092(7) -0.0124(8) -0.0127(8) Cl1 0.0571(15) 0.0607(17) 0.0451(13) 0.0264(13) -0.0112(12) -0.0151(13) Cl2 0.0616(16) 0.0629(17) 0.0499(14) -0.0038(12) -0.0251(13) -0.0147(13) P1 0.0482(14) 0.0451(15) 0.0326(12) 0.0101(11) -0.0131(11) -0.0242(12) P2 0.0488(14) 0.0470(15) 0.0311(12) 0.0080(11) -0.0086(11) -0.0207(12) N1 0.038(4) 0.037(4) 0.037(4) 0.011(3) -0.015(3) -0.020(3) N2 0.036(4) 0.035(4) 0.041(4) 0.016(3) -0.017(3) -0.016(3) C1 0.039(5) 0.033(5) 0.037(5) 0.008(4) -0.008(4) -0.017(4) C2 0.037(5) 0.031(5) 0.047(5) 0.015(4) -0.016(4) -0.017(4) C3 0.032(5) 0.042(6) 0.034(5) 0.012(4) -0.013(4) -0.020(4) C4 0.040(5) 0.038(6) 0.040(5) 0.011(4) -0.014(4) -0.019(4) C5 0.048(5) 0.033(5) 0.053(6) 0.013(5) -0.012(5) -0.020(4) C6 0.046(5) 0.048(6) 0.040(5) 0.002(5) -0.008(5) -0.023(5) C7 0.054(6) 0.053(6) 0.037(5) 0.012(5) -0.025(5) -0.023(5) C8 0.063(6) 0.053(7) 0.041(5) 0.023(5) -0.023(5) -0.023(5) C9 0.108(9) 0.038(7) 0.062(7) 0.008(5) -0.035(7) -0.023(6) C10 0.097(9) 0.053(7) 0.079(8) 0.021(7) -0.044(8) -0.041(7) C11 0.075(8) 0.068(8) 0.057(7) 0.025(6) -0.034(6) -0.041(7) C12 0.068(6) 0.048(6) 0.042(5) 0.024(5) -0.026(5) -0.034(5) C13 0.059(6) 0.053(6) 0.044(5) 0.015(5) -0.026(5) -0.030(5) C14 0.050(6) 0.094(9) 0.075(8) 0.035(7) -0.032(6) -0.035(6) C15 0.071(8) 0.098(11) 0.094(10) 0.029(8) -0.027(8) -0.045(8) C16 0.060(7) 0.091(10) 0.071(8) -0.013(7) -0.019(7) -0.027(7) C17 0.078(8) 0.066(8) 0.066(7) 0.002(6) -0.036(7) -0.017(6) C18 0.056(7) 0.072(8) 0.077(8) 0.023(6) -0.035(6) -0.029(6) C19 0.039(5) 0.045(6) 0.045(5) 0.007(5) 0.002(5) -0.011(5) C20 0.040(5) 0.038(5) 0.045(5) 0.005(4) -0.010(4) -0.014(4) C21 0.079(8) 0.059(7) 0.059(7) -0.001(6) -0.005(6) -0.034(6) C22 0.039(5) 0.067(7) 0.068(7) 0.029(6) -0.021(5) -0.017(5) C23 0.054(6) 0.042(6) 0.049(5) 0.010(5) -0.024(5) -0.023(5) C24 0.041(5) 0.047(6) 0.043(5) 0.010(5) -0.005(5) -0.016(5) C25 0.045(6) 0.068(8) 0.081(8) 0.010(6) -0.027(6) -0.026(5) C26 0.052(6) 0.073(8) 0.067(7) 0.005(6) 0.011(6) -0.030(6) C27 0.059(7) 0.068(8) 0.077(8) 0.027(7) -0.013(6) -0.037(6) C28 0.030(4) 0.032(5) 0.041(5) -0.003(4) -0.008(4) -0.009(4) C29 0.038(5) 0.037(5) 0.039(5) 0.010(4) -0.011(4) -0.020(4) C30 0.032(4) 0.035(5) 0.032(5) 0.010(4) -0.013(4) -0.016(4) C31 0.038(5) 0.031(5) 0.034(5) 0.005(4) -0.014(4) -0.013(4) C32 0.052(6) 0.038(6) 0.049(6) 0.014(5) -0.020(5) -0.026(5) C33 0.047(5) 0.043(6) 0.037(5) 0.011(4) -0.013(4) -0.020(5) C34 0.080(8) 0.042(6) 0.032(5) 0.001(4) -0.010(5) -0.024(6) C35 0.070(7) 0.051(7) 0.067(7) 0.014(6) -0.010(6) -0.023(6) C36 0.095(10) 0.053(8) 0.078(8) 0.006(7) -0.014(8) -0.032(7) C37 0.108(11) 0.053(8) 0.057(7) 0.010(6) -0.014(8) -0.011(8) C38 0.067(7) 0.055(8) 0.058(7) 0.000(6) -0.007(6) 0.002(6) C39 0.053(7) 0.061(8) 0.053(6) 0.010(5) -0.014(5) -0.014(6) C40 0.044(5) 0.055(6) 0.033(5) 0.012(4) -0.006(4) -0.026(5) C41 0.052(6) 0.067(7) 0.041(5) 0.020(5) -0.008(5) -0.021(5) C42 0.061(7) 0.091(9) 0.044(6) 0.025(6) -0.012(6) -0.036(7) C43 0.051(7) 0.082(9) 0.050(6) 0.019(6) 0.012(6) -0.030(6) C44 0.051(6) 0.087(9) 0.063(7) 0.015(6) -0.020(6) -0.031(6) C45 0.059(6) 0.067(7) 0.050(6) 0.021(5) -0.022(6) -0.028(6) C46 0.040(5) 0.049(6) 0.036(5) 0.018(4) -0.013(4) -0.015(4) C47 0.039(5) 0.040(6) 0.043(5) 0.009(4) -0.009(4) -0.014(4) C48 0.047(6) 0.047(6) 0.077(7) 0.018(6) -0.027(6) -0.015(5) C49 0.054(6) 0.042(6) 0.070(7) -0.002(5) -0.010(6) -0.006(5) C50 0.051(6) 0.043(6) 0.054(6) 0.024(5) -0.029(5) -0.025(5) C51 0.043(5) 0.043(6) 0.083(7) 0.031(6) -0.034(6) -0.019(5) C52 0.048(6) 0.063(7) 0.077(7) 0.024(6) -0.019(6) -0.030(5) C53 0.056(6) 0.067(8) 0.083(8) 0.029(6) -0.046(6) -0.029(6) C54 0.068(7) 0.038(6) 0.095(8) 0.010(6) -0.050(7) -0.019(5) C55 0.053(6) 0.076(7) 0.006(4) -0.014(4) 0.012(4) -0.023(5) C56 0.042(5) 0.050(6) 0.026(4) -0.005(4) -0.023(4) -0.020(4) Cl3 0.105(3) 0.149(4) 0.078(2) 0.007(2) -0.031(2) -0.017(3) Cl4 0.128(4) 0.113(4) 0.233(6) -0.031(4) -0.091(4) 0.002(3) Cl5 0.091(3) 0.370(12) 0.356(11) -0.232(10) -0.015(5) -0.075(5) Cl6 0.155(5) 0.276(9) 0.210(7) 0.160(7) -0.046(5) -0.057(6) Cl7 0.176(6) 0.137(5) 0.368(11) 0.009(6) -0.172(7) -0.028(4) Cl8 0.219(8) 0.162(6) 0.299(11) -0.002(7) -0.106(8) -0.063(6) Cl9 0.131(7) 0.135(8) 0.130(7) -0.004(6) -0.034(6) -0.073(6) Cl10 0.270(17) 0.129(10) 0.84(5) -0.058(18) 0.10(2) -0.102(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C56 2.164(7) . ? Pt C55 2.193(9) . ? Pt P1 2.290(3) . ? Pt P2 2.291(2) . ? Ti N2 1.876(7) . ? Ti N1 1.891(7) . ? Ti Cl1 2.255(3) . ? Ti Cl2 2.262(3) . ? P1 C7 1.824(10) . ? P1 C1 1.849(8) . ? P1 C13 1.860(9) . ? P2 C28 1.844(9) . ? P2 C34 1.846(10) . ? P2 C40 1.853(8) . ? N1 C3 1.445(11) . ? N1 C19 1.494(12) . ? N2 C30 1.446(10) . ? N2 C46 1.507(11) . ? C1 C2 1.374(13) . ? C1 C6 1.394(13) . ? C2 C3 1.409(11) . ? C3 C4 1.398(12) . ? C4 C5 1.395(13) . ? C5 C6 1.367(12) . ? C7 C12 1.394(13) . ? C7 C8 1.409(14) . ? C8 C9 1.380(15) . ? C9 C10 1.409(16) . ? C10 C11 1.371(17) . ? C11 C12 1.380(15) . ? C13 C14 1.346(13) . ? C13 C18 1.369(13) . ? C14 C15 1.380(16) . ? C15 C16 1.377(17) . ? C16 C17 1.370(16) . ? C17 C18 1.362(15) . ? C19 C20 1.577(13) . ? C19 C24 1.604(12) . ? C20 C23 1.528(12) . ? C20 C21 1.529(14) . ? C20 C22 1.543(13) . ? C24 C27 1.500(14) . ? C24 C26 1.525(15) . ? C24 C25 1.582(14) . ? C28 C29 1.384(11) . ? C28 C33 1.392(12) . ? C29 C30 1.370(12) . ? C30 C31 1.393(12) . ? C31 C32 1.400(11) . ? C32 C33 1.378(13) . ? C34 C35 1.391(14) . ? C34 C39 1.411(14) . ? C35 C36 1.365(16) . ? C36 C37 1.376(18) . ? C37 C38 1.387(17) . ? C38 C39 1.364(15) . ? C40 C45 1.359(13) . ? C40 C41 1.397(12) . ? C41 C42 1.413(13) . ? C42 C43 1.334(16) . ? C43 C44 1.379(15) . ? C44 C45 1.422(14) . ? C46 C47 1.573(13) . ? C46 C51 1.597(12) . ? C47 C49 1.510(13) . ? C47 C50 1.536(12) . ? C47 C48 1.547(12) . ? C51 C54 1.516(15) . ? C51 C52 1.547(14) . ? C51 C53 1.559(12) . ? C57 Cl4 1.734(12) . ? C57 Cl3 1.759(12) . ? C58 Cl6 1.733(13) . ? C58 Cl5 1.735(13) . ? C59 Cl8 1.784(16) . ? C59 Cl7 1.786(16) . ? 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 C56 Pt C55 85.8(3) . . ? C56 Pt P1 90.5(2) . . ? C55 Pt P1 174.6(3) . . ? C56 Pt P2 169.8(2) . . ? C55 Pt P2 84.1(3) . . ? P1 Pt P2 99.73(8) . . ? N2 Ti N1 116.1(3) . . ? N2 Ti Cl1 109.4(2) . . ? N1 Ti Cl1 110.5(2) . . ? N2 Ti Cl2 109.0(2) . . ? N1 Ti Cl2 108.1(2) . . ? Cl1 Ti Cl2 102.85(11) . . ? C7 P1 C1 109.5(4) . . ? C7 P1 C13 100.0(4) . . ? C1 P1 C13 102.2(4) . . ? C7 P1 Pt 116.2(3) . . ? C1 P1 Pt 109.2(3) . . ? C13 P1 Pt 118.6(3) . . ? C28 P2 C34 102.8(4) . . ? C28 P2 C40 100.6(4) . . ? C34 P2 C40 106.2(5) . . ? C28 P2 Pt 121.1(3) . . ? C34 P2 Pt 111.9(3) . . ? C40 P2 Pt 112.6(3) . . ? C3 N1 C19 123.4(7) . . ? C3 N1 Ti 112.0(5) . . ? C19 N1 Ti 124.3(6) . . ? C30 N2 C46 121.5(7) . . ? C30 N2 Ti 116.1(5) . . ? C46 N2 Ti 122.1(5) . . ? C2 C1 C6 120.8(8) . . ? C2 C1 P1 126.1(6) . . ? C6 C1 P1 113.1(7) . . ? C1 C2 C3 119.6(8) . . ? C4 C3 C2 119.1(8) . . ? C4 C3 N1 116.9(7) . . ? C2 C3 N1 123.7(8) . . ? C5 C4 C3 120.2(8) . . ? C6 C5 C4 120.1(9) . . ? C5 C6 C1 120.2(9) . . ? C12 C7 C8 118.8(9) . . ? C12 C7 P1 118.5(8) . . ? C8 C7 P1 122.5(7) . . ? C9 C8 C7 122.2(9) . . ? C8 C9 C10 117.8(11) . . ? C11 C10 C9 119.7(10) . . ? C10 C11 C12 122.7(10) . . ? C11 C12 C7 118.6(10) . . ? C14 C13 C18 118.3(9) . . ? C14 C13 P1 122.5(7) . . ? C18 C13 P1 119.2(7) . . ? C13 C14 C15 120.7(10) . . ? C16 C15 C14 121.2(11) . . ? C17 C16 C15 117.3(11) . . ? C18 C17 C16 120.7(11) . . ? C17 C18 C13 121.7(10) . . ? N1 C19 C20 115.8(7) . . ? N1 C19 C24 112.7(8) . . ? C20 C19 C24 120.8(7) . . ? C23 C20 C21 105.7(8) . . ? C23 C20 C22 107.6(7) . . ? C21 C20 C22 108.5(9) . . ? C23 C20 C19 111.2(7) . . ? C21 C20 C19 109.4(7) . . ? C22 C20 C19 114.0(8) . . ? C27 C24 C26 108.1(8) . . ? C27 C24 C25 107.5(9) . . ? C26 C24 C25 107.7(8) . . ? C27 C24 C19 109.2(8) . . ? C26 C24 C19 112.0(8) . . ? C25 C24 C19 112.2(7) . . ? C29 C28 C33 119.1(8) . . ? C29 C28 P2 123.0(7) . . ? C33 C28 P2 117.9(6) . . ? C30 C29 C28 121.4(8) . . ? C29 C30 C31 119.3(7) . . ? C29 C30 N2 124.3(8) . . ? C31 C30 N2 116.4(7) . . ? C30 C31 C32 120.2(8) . . ? C33 C32 C31 119.2(8) . . ? C32 C33 C28 120.7(8) . . ? C35 C34 C39 117.7(10) . . ? C35 C34 P2 118.0(8) . . ? C39 C34 P2 124.4(8) . . ? C36 C35 C34 121.3(11) . . ? C35 C36 C37 120.3(12) . . ? C36 C37 C38 120.0(11) . . ? C39 C38 C37 120.0(11) . . ? C38 C39 C34 120.9(10) . . ? C45 C40 C41 120.6(8) . . ? C45 C40 P2 121.2(7) . . ? C41 C40 P2 118.2(7) . . ? C40 C41 C42 119.6(10) . . ? C43 C42 C41 119.4(9) . . ? C42 C43 C44 121.8(9) . . ? C43 C44 C45 119.6(10) . . ? C40 C45 C44 118.8(9) . . ? N2 C46 C47 116.7(7) . . ? N2 C46 C51 111.9(7) . . ? C47 C46 C51 118.8(8) . . ? C49 C47 C50 106.9(8) . . ? C49 C47 C48 108.4(8) . . ? C50 C47 C48 104.5(7) . . ? C49 C47 C46 115.8(7) . . ? C50 C47 C46 110.6(7) . . ? C48 C47 C46 110.1(8) . . ? C54 C51 C52 105.6(8) . . ? C54 C51 C53 107.1(9) . . ? C52 C51 C53 107.0(8) . . ? C54 C51 C46 109.2(8) . . ? C52 C51 C46 116.1(8) . . ? C53 C51 C46 111.2(7) . . ? Cl4 C57 Cl3 112.3(8) . . ? Cl6 C58 Cl5 115.5(10) . . ? Cl8 C59 Cl7 108.9(12) . . ?