# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Paul Kamer' 'Johanneke E. Ernsting' 'Martin Lutz' 'Angelica Marson' 'A. Spek' 'Van Leeuwen, Piet W.N.M. ' _publ_contact_author_name 'Prof Paul Kamer' _publ_contact_author_email PCJK@ST-ANDREWS.AC.UK _publ_section_title ; A Novel Hemilabile Calix[4],Quinoline-Based P,N-Ligand: Coordination Chemistry and Complex Characterisation ; # Attachment 'deposit.cif' data_s3382a _database_code_depnum_ccdc_archive 'CCDC 699253' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H60 N O4 P, C H2 Cl2' _chemical_formula_sum 'C55 H62 Cl2 N O4 P' _chemical_formula_weight 902.93 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' 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 0.0060 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2138(1) _cell_length_b 19.6378(1) _cell_length_c 22.6813(2) _cell_angle_alpha 65.8298(3) _cell_angle_beta 77.0409(3) _cell_angle_gamma 76.6873(3) _cell_volume 5169.01(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 147382 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102943 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 23594 _reflns_number_gt 19081 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, SortAV, SQUEEZE' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0491P)^2^+1.6491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23594 _refine_ls_number_parameters 1207 _refine_ls_number_restraints 204 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.097 _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 P1 P 0.77054(3) 0.13373(2) 0.252168(17) 0.01959(8) Uani 1 1 d . . . O11 O 0.85440(8) 0.14065(5) 0.29086(4) 0.0190(2) Uani 1 1 d . . . O12 O 0.82650(8) 0.15954(6) 0.17610(5) 0.0224(2) Uani 1 1 d . . . O13 O 0.78805(7) 0.04124(5) 0.27287(5) 0.0194(2) Uani 1 1 d . . . O14 O 0.68946(7) 0.07970(5) 0.39735(5) 0.0188(2) Uani 1 1 d . . . N1 N 0.48851(10) 0.18746(7) 0.47118(6) 0.0236(3) Uani 1 1 d . . . C11 C 0.96001(11) 0.12416(7) 0.30074(6) 0.0173(3) Uani 1 1 d . . . C12 C 0.98003(11) 0.09287(7) 0.36568(6) 0.0179(3) Uani 1 1 d . . . C13 C 1.08318(11) 0.07672(8) 0.37731(7) 0.0192(3) Uani 1 1 d . . . H13 H 1.0964 0.0545 0.4213 0.023 Uiso 1 1 calc R . . C14 C 1.16866(11) 0.09171(8) 0.32717(7) 0.0205(3) Uani 1 1 d . . . C15 C 1.14465(11) 0.12850(8) 0.26400(7) 0.0214(3) Uani 1 1 d . . . H15 H 1.2006 0.1420 0.2289 0.026 Uiso 1 1 calc R . . C16 C 1.04206(11) 0.14657(7) 0.24955(6) 0.0191(3) Uani 1 1 d . . . C17 C 1.02469(12) 0.18788(8) 0.17908(7) 0.0212(3) Uani 1 1 d . . . H17A H 0.9602 0.2259 0.1763 0.025 Uiso 1 1 calc R . . H17B H 1.0848 0.2147 0.1534 0.025 Uiso 1 1 calc R . . C18 C 0.91573(11) 0.11686(8) 0.15424(6) 0.0201(3) Uani 1 1 d . . . C19 C 1.01401(12) 0.13253(8) 0.15136(6) 0.0201(3) Uani 1 1 d . . . C110 C 1.10140(11) 0.09106(8) 0.12712(6) 0.0206(3) Uani 1 1 d . . . H110 H 1.1695 0.1007 0.1252 0.025 Uiso 1 1 calc R . . C111 C 1.09217(11) 0.03600(8) 0.10561(7) 0.0209(3) Uani 1 1 d . A . C112 C 0.99087(12) 0.02243(8) 0.10988(7) 0.0219(3) Uani 1 1 d . . . H112 H 0.9826 -0.0150 0.0957 0.026 Uiso 1 1 calc R . . C113 C 0.90199(11) 0.06214(8) 0.13421(7) 0.0219(3) Uani 1 1 d . . . C114 C 0.79213(12) 0.05100(9) 0.13511(7) 0.0257(3) Uani 1 1 d . . . H11A H 0.7956 0.0312 0.1008 0.031 Uiso 1 1 calc R . . H11B H 0.7481 0.1015 0.1219 0.031 Uiso 1 1 calc R . . C115 C 0.72404(11) 0.00158(8) 0.26004(7) 0.0197(3) Uani 1 1 d . . . C116 C 0.73449(11) -0.00015(8) 0.19778(7) 0.0222(3) Uani 1 1 d . . . C117 C 0.68118(12) -0.04963(9) 0.19028(7) 0.0251(3) Uani 1 1 d . . . H117 H 0.6897 -0.0519 0.1484 0.030 Uiso 1 1 calc R . . C118 C 0.61696(12) -0.09517(9) 0.24095(8) 0.0255(3) Uani 1 1 d . . . C119 C 0.60472(11) -0.08904(8) 0.30127(7) 0.0232(3) Uani 1 1 d . . . H119 H 0.5590 -0.1184 0.3365 0.028 Uiso 1 1 calc R . . C120 C 0.65618(11) -0.04199(8) 0.31234(7) 0.0195(3) Uani 1 1 d . . . C121 C 0.63039(11) -0.03902(8) 0.38010(7) 0.0197(3) Uani 1 1 d . . . H12A H 0.5885 0.0108 0.3771 0.024 Uiso 1 1 calc R . . H12B H 0.5863 -0.0782 0.4087 0.024 Uiso 1 1 calc R . . C122 C 0.75545(11) 0.01039(7) 0.41536(6) 0.0172(3) Uani 1 1 d . . . C123 C 0.72583(11) -0.05106(8) 0.41135(6) 0.0180(3) Uani 1 1 d . . . C124 C 0.78942(11) -0.12070(8) 0.43236(7) 0.0193(3) Uani 1 1 d . . . H124 H 0.7680 -0.1633 0.4316 0.023 Uiso 1 1 calc R . . C125 C 0.88435(11) -0.13026(8) 0.45470(6) 0.0183(3) Uani 1 1 d . . . C126 C 0.91608(11) -0.06555(8) 0.45103(6) 0.0177(3) Uani 1 1 d . . . H126 H 0.9831 -0.0696 0.4620 0.021 Uiso 1 1 calc R . . C127 C 0.85242(11) 0.00514(8) 0.43176(6) 0.0168(3) Uani 1 1 d . . . C128 C 0.89212(11) 0.07551(8) 0.42274(6) 0.0179(3) Uani 1 1 d . . . H12C H 0.9181 0.0680 0.4630 0.021 Uiso 1 1 calc R . . H12D H 0.8339 0.1187 0.4147 0.021 Uiso 1 1 calc R . . C129 C 1.28127(11) 0.06595(9) 0.34375(7) 0.0240(3) Uani 1 1 d . . . C130 C 1.29682(13) 0.10034(10) 0.39026(8) 0.0305(3) Uani 1 1 d . . . H13A H 1.3679 0.0817 0.4019 0.046 Uiso 1 1 calc R . . H13B H 1.2452 0.0858 0.4299 0.046 Uiso 1 1 calc R . . H13C H 1.2873 0.1555 0.3687 0.046 Uiso 1 1 calc R . . C131 C 1.36312(13) 0.08836(11) 0.28245(8) 0.0374(4) Uani 1 1 d . . . H13D H 1.4338 0.0701 0.2948 0.056 Uiso 1 1 calc R . . H13E H 1.3534 0.1435 0.2605 0.056 Uiso 1 1 calc R . . H13F H 1.3546 0.0659 0.2528 0.056 Uiso 1 1 calc R . . C132 C 1.29974(13) -0.02062(9) 0.37733(8) 0.0301(3) Uani 1 1 d . . . H13G H 1.2894 -0.0430 0.3480 0.045 Uiso 1 1 calc R . . H13H H 1.2499 -0.0362 0.4177 0.045 Uiso 1 1 calc R . . H13I H 1.3717 -0.0379 0.3876 0.045 Uiso 1 1 calc R . . C133 C 1.18907(12) -0.00854(8) 0.07840(7) 0.0237(3) Uani 1 1 d D . . C34A C 1.29091(18) 0.01808(14) 0.07635(13) 0.0382(6) Uani 0.73 1 d PDU A 1 H34A H 1.2876 0.0719 0.0487 0.057 Uiso 0.73 1 calc PR A 1 H34B H 1.3511 -0.0110 0.0584 0.057 Uiso 0.73 1 calc PR A 1 H34C H 1.2989 0.0103 0.1207 0.057 Uiso 0.73 1 calc PR A 1 C35A C 1.1942(2) -0.09132(13) 0.12100(13) 0.0446(6) Uani 0.73 1 d PDU A 1 H35A H 1.2558 -0.1202 0.1038 0.067 Uiso 0.73 1 calc PR A 1 H35B H 1.1303 -0.1087 0.1212 0.067 Uiso 0.73 1 calc PR A 1 H35C H 1.1999 -0.0988 0.1657 0.067 Uiso 0.73 1 calc PR A 1 C36A C 1.1795(2) 0.00556(17) 0.00830(12) 0.0462(7) Uani 0.73 1 d PDU A 1 H36A H 1.1764 0.0596 -0.0184 0.069 Uiso 0.73 1 calc PR A 1 H36B H 1.1153 -0.0111 0.0080 0.069 Uiso 0.73 1 calc PR A 1 H36C H 1.2407 -0.0228 -0.0097 0.069 Uiso 0.73 1 calc PR A 1 C34B C 1.1623(4) -0.0700(3) 0.0597(2) 0.0195(10) Uani 0.27 1 d PDU A 2 H34D H 1.1224 -0.1045 0.0977 0.029 Uiso 0.27 1 calc PR A 2 H34E H 1.2275 -0.0987 0.0457 0.029 Uiso 0.27 1 calc PR A 2 H34F H 1.1200 -0.0455 0.0239 0.029 Uiso 0.27 1 calc PR A 2 C35B C 1.2631(4) -0.0517(3) 0.1304(2) 0.0225(11) Uani 0.27 1 d PDU A 2 H35D H 1.2245 -0.0846 0.1702 0.034 Uiso 0.27 1 calc PR A 2 H35E H 1.2894 -0.0155 0.1404 0.034 Uiso 0.27 1 calc PR A 2 H35F H 1.3224 -0.0824 0.1136 0.034 Uiso 0.27 1 calc PR A 2 C36B C 1.2503(4) 0.0430(2) 0.0173(2) 0.0258(12) Uani 0.27 1 d PDU A 2 H36D H 1.3112 0.0127 0.0013 0.039 Uiso 0.27 1 calc PR A 2 H36E H 1.2743 0.0798 0.0279 0.039 Uiso 0.27 1 calc PR A 2 H36F H 1.2047 0.0698 -0.0165 0.039 Uiso 0.27 1 calc PR A 2 C137 C 0.55746(14) -0.14882(10) 0.23285(9) 0.0339(4) Uani 1 1 d . . . C138 C 0.43906(16) -0.11925(13) 0.24264(12) 0.0523(5) Uani 1 1 d . . . H13J H 0.3998 -0.1513 0.2356 0.078 Uiso 1 1 calc R . . H13K H 0.4247 -0.0672 0.2114 0.078 Uiso 1 1 calc R . . H13L H 0.4172 -0.1204 0.2872 0.078 Uiso 1 1 calc R . . C139 C 0.58172(18) -0.22886(11) 0.28383(10) 0.0458(5) Uani 1 1 d . . . H13M H 0.5591 -0.2281 0.3278 0.069 Uiso 1 1 calc R . . H13N H 0.6575 -0.2468 0.2780 0.069 Uiso 1 1 calc R . . H13O H 0.5440 -0.2629 0.2782 0.069 Uiso 1 1 calc R . . C140 C 0.58740(19) -0.15239(13) 0.16479(10) 0.0493(5) Uani 1 1 d . . . H14A H 0.5483 -0.1874 0.1619 0.074 Uiso 1 1 calc R . . H14B H 0.6630 -0.1700 0.1572 0.074 Uiso 1 1 calc R . . H14C H 0.5700 -0.1020 0.1317 0.074 Uiso 1 1 calc R . . C141 C 0.94676(11) -0.20950(8) 0.48480(7) 0.0215(3) Uani 1 1 d . . . C142 C 1.05804(12) -0.20693(9) 0.49224(8) 0.0316(4) Uani 1 1 d . . . H14D H 1.0957 -0.1793 0.4494 0.047 Uiso 1 1 calc R . . H14E H 1.0956 -0.2586 0.5101 0.047 Uiso 1 1 calc R . . H14F H 1.0540 -0.1813 0.5220 0.047 Uiso 1 1 calc R . . C143 C 0.95472(15) -0.25661(9) 0.44361(8) 0.0340(4) Uani 1 1 d . . . H14G H 0.8840 -0.2622 0.4414 0.051 Uiso 1 1 calc R . . H14H H 0.9953 -0.3066 0.4637 0.051 Uiso 1 1 calc R . . H14I H 0.9900 -0.2311 0.3994 0.051 Uiso 1 1 calc R . . C144 C 0.88675(12) -0.24769(8) 0.55312(7) 0.0265(3) Uani 1 1 d . . . H14J H 0.8858 -0.2196 0.5804 0.040 Uiso 1 1 calc R . . H14K H 0.9218 -0.2997 0.5732 0.040 Uiso 1 1 calc R . . H14L H 0.8145 -0.2481 0.5494 0.040 Uiso 1 1 calc R . . C145 C 0.61436(12) 0.08837(8) 0.45088(7) 0.0232(3) Uani 1 1 d . . . H14M H 0.6508 0.0903 0.4837 0.028 Uiso 1 1 calc R . . H14N H 0.5759 0.0446 0.4721 0.028 Uiso 1 1 calc R . . C146 C 0.53824(11) 0.16008(8) 0.42643(7) 0.0190(3) Uani 1 1 d . . . C147 C 0.52190(11) 0.19330(8) 0.36029(7) 0.0209(3) Uani 1 1 d . . . H147 H 0.5594 0.1710 0.3300 0.025 Uiso 1 1 calc R . . C148 C 0.45129(11) 0.25802(8) 0.34086(7) 0.0231(3) Uani 1 1 d . . . H148 H 0.4385 0.2810 0.2968 0.028 Uiso 1 1 calc R . . C149 C 0.39731(11) 0.29065(8) 0.38648(7) 0.0227(3) Uani 1 1 d . . . C150 C 0.32657(12) 0.35983(9) 0.36968(9) 0.0303(4) Uani 1 1 d . . . H150 H 0.3125 0.3859 0.3260 0.036 Uiso 1 1 calc R . . C151 C 0.27867(13) 0.38908(9) 0.41599(10) 0.0365(4) Uani 1 1 d . . . H151 H 0.2315 0.4354 0.4044 0.044 Uiso 1 1 calc R . . C152 C 0.29886(14) 0.35090(10) 0.48077(10) 0.0383(4) Uani 1 1 d . . . H152 H 0.2647 0.3717 0.5126 0.046 Uiso 1 1 calc R . . C153 C 0.36688(13) 0.28437(9) 0.49872(9) 0.0318(4) Uani 1 1 d . . . H153 H 0.3797 0.2593 0.5427 0.038 Uiso 1 1 calc R . . C154 C 0.41822(11) 0.25283(8) 0.45169(7) 0.0236(3) Uani 1 1 d . . . P2 P 0.65467(3) 0.35870(2) 0.248898(17) 0.01933(8) Uani 1 1 d . . . O21 O 0.62956(7) 0.45110(5) 0.22778(5) 0.0195(2) Uani 1 1 d . . . O22 O 0.66640(8) 0.33328(5) 0.32571(5) 0.0216(2) Uani 1 1 d . . . O23 O 0.77367(8) 0.34896(5) 0.21132(5) 0.0191(2) Uani 1 1 d . . . O24 O 0.65625(8) 0.40755(5) 0.10234(5) 0.0199(2) Uani 1 1 d . . . N2 N 0.59660(10) 0.30667(7) 0.01713(6) 0.0224(3) Uani 1 1 d . . . C21 C 0.52980(11) 0.49247(8) 0.23976(7) 0.0198(3) Uani 1 1 d . . . C22 C 0.47221(11) 0.53402(8) 0.18744(7) 0.0202(3) Uani 1 1 d . . . C23 C 0.38222(11) 0.58382(8) 0.19636(7) 0.0229(3) Uani 1 1 d . . . H23 H 0.3439 0.6122 0.1608 0.028 Uiso 1 1 calc R . . C24 C 0.34572(12) 0.59401(9) 0.25531(8) 0.0259(3) Uani 1 1 d . B . C25 C 0.40209(12) 0.54926(9) 0.30656(7) 0.0250(3) Uani 1 1 d . . . H25 H 0.3778 0.5540 0.3476 0.030 Uiso 1 1 calc R . . C26 C 0.49253(11) 0.49772(8) 0.30092(7) 0.0219(3) Uani 1 1 d . . . C27 C 0.53635(12) 0.44830(9) 0.36415(7) 0.0245(3) Uani 1 1 d . . . H27A H 0.5039 0.4717 0.3965 0.029 Uiso 1 1 calc R . . H27B H 0.5117 0.3989 0.3804 0.029 Uiso 1 1 calc R . . C28 C 0.71461(11) 0.37425(8) 0.34658(6) 0.0192(3) Uani 1 1 d . . . C29 C 0.65340(11) 0.43277(8) 0.36408(6) 0.0204(3) Uani 1 1 d . . . C210 C 0.70299(12) 0.47229(8) 0.38499(7) 0.0207(3) Uani 1 1 d . . . H210 H 0.6622 0.5122 0.3974 0.025 Uiso 1 1 calc R . . C211 C 0.81102(11) 0.45538(8) 0.38836(6) 0.0192(3) Uani 1 1 d . . . C212 C 0.86829(11) 0.39586(8) 0.37076(6) 0.0191(3) Uani 1 1 d . . . H212 H 0.9416 0.3831 0.3729 0.023 Uiso 1 1 calc R . . C213 C 0.82112(11) 0.35424(7) 0.35006(6) 0.0185(3) Uani 1 1 d . . . C214 C 0.88527(12) 0.29455(8) 0.32532(6) 0.0196(3) Uani 1 1 d . . . H21A H 0.8397 0.2599 0.3273 0.024 Uiso 1 1 calc R . . H21B H 0.9409 0.2646 0.3527 0.024 Uiso 1 1 calc R . . C215 C 0.87728(11) 0.36146(7) 0.20297(7) 0.0171(3) Uani 1 1 d . . . C216 C 0.93405(11) 0.33370(7) 0.25549(6) 0.0190(3) Uani 1 1 d . . . C217 C 1.03735(12) 0.34617(8) 0.24347(7) 0.0211(3) Uani 1 1 d . . . H217 H 1.0752 0.3279 0.2794 0.025 Uiso 1 1 calc R . . C218 C 1.08823(12) 0.38423(8) 0.18122(7) 0.0216(3) Uani 1 1 d . . . C219 C 1.03172(11) 0.40566(8) 0.12973(7) 0.0197(3) Uani 1 1 d . . . H219 H 1.0651 0.4296 0.0865 0.024 Uiso 1 1 calc R . . C220 C 0.92836(11) 0.39354(7) 0.13885(6) 0.0179(3) Uani 1 1 d . . . C221 C 0.87543(11) 0.41348(8) 0.07983(6) 0.0180(3) Uani 1 1 d . . . H22A H 0.9292 0.4222 0.0404 0.022 Uiso 1 1 calc R . . H22B H 0.8421 0.3705 0.0856 0.022 Uiso 1 1 calc R . . C222 C 0.68766(11) 0.47723(7) 0.08552(6) 0.0174(3) Uani 1 1 d . . . C223 C 0.79316(11) 0.48312(8) 0.07007(6) 0.0171(3) Uani 1 1 d . . . C224 C 0.82201(11) 0.55472(8) 0.04941(6) 0.0174(3) Uani 1 1 d . . . H224 H 0.8945 0.5595 0.0382 0.021 Uiso 1 1 calc R . . C225 C 0.74754(11) 0.61900(8) 0.04482(6) 0.0178(3) Uani 1 1 d . . . C226 C 0.64252(11) 0.60856(8) 0.06764(7) 0.0195(3) Uani 1 1 d . . . H226 H 0.5908 0.6509 0.0683 0.023 Uiso 1 1 calc R . . C227 C 0.61144(11) 0.53817(8) 0.08934(6) 0.0185(3) Uani 1 1 d . . . C228 C 0.50061(11) 0.52583(8) 0.12161(7) 0.0208(3) Uani 1 1 d . . . H22C H 0.4917 0.4746 0.1277 0.025 Uiso 1 1 calc R . . H22D H 0.4510 0.5627 0.0922 0.025 Uiso 1 1 calc R . . C229 C 0.24800(13) 0.65145(10) 0.26236(8) 0.0332(4) Uani 1 1 d D . . C30C C 0.15230(19) 0.62501(17) 0.25192(16) 0.0571(8) Uani 0.77 1 d PDU B 3 H30A H 0.1436 0.5747 0.2850 0.086 Uiso 0.77 1 calc PR B 3 H30B H 0.1653 0.6231 0.2083 0.086 Uiso 0.77 1 calc PR B 3 H30C H 0.0883 0.6607 0.2559 0.086 Uiso 0.77 1 calc PR B 3 C31C C 0.2593(2) 0.72808(14) 0.21146(15) 0.0560(8) Uani 0.77 1 d PDU B 3 H31A H 0.1961 0.7638 0.2170 0.084 Uiso 0.77 1 calc PR B 3 H31B H 0.2684 0.7262 0.1680 0.084 Uiso 0.77 1 calc PR B 3 H31C H 0.3208 0.7446 0.2159 0.084 Uiso 0.77 1 calc PR B 3 C32C C 0.2211(3) 0.6535(2) 0.33067(15) 0.0852(14) Uani 0.77 1 d PDU B 3 H32A H 0.2141 0.6025 0.3630 0.128 Uiso 0.77 1 calc PR B 3 H32B H 0.1546 0.6873 0.3338 0.128 Uiso 0.77 1 calc PR B 3 H32C H 0.2772 0.6719 0.3391 0.128 Uiso 0.77 1 calc PR B 3 C30D C 0.1918(6) 0.6903(4) 0.2014(3) 0.0399(18) Uani 0.23 1 d PDU B 4 H30D H 0.2440 0.7055 0.1621 0.060 Uiso 0.23 1 calc PR B 4 H30E H 0.1431 0.7351 0.2044 0.060 Uiso 0.23 1 calc PR B 4 H30F H 0.1525 0.6551 0.1990 0.060 Uiso 0.23 1 calc PR B 4 C31D C 0.2914(6) 0.7161(4) 0.2684(5) 0.052(2) Uani 0.23 1 d PDU B 4 H31D H 0.3394 0.7388 0.2286 0.078 Uiso 0.23 1 calc PR B 4 H31E H 0.3291 0.6949 0.3062 0.078 Uiso 0.23 1 calc PR B 4 H31F H 0.2326 0.7547 0.2741 0.078 Uiso 0.23 1 calc PR B 4 C32D C 0.1726(6) 0.6184(5) 0.3212(3) 0.064(3) Uani 0.23 1 d PDU B 4 H32D H 0.1112 0.6567 0.3236 0.096 Uiso 0.23 1 calc PR B 4 H32E H 0.2064 0.6010 0.3602 0.096 Uiso 0.23 1 calc PR B 4 H32F H 0.1502 0.5755 0.3187 0.096 Uiso 0.23 1 calc PR B 4 C233 C 0.86213(12) 0.50036(8) 0.41223(7) 0.0230(3) Uani 1 1 d . . . C234 C 0.83065(15) 0.58558(9) 0.37552(8) 0.0333(4) Uani 1 1 d . . . H23A H 0.8643 0.6137 0.3908 0.050 Uiso 1 1 calc R . . H23B H 0.7541 0.5990 0.3838 0.050 Uiso 1 1 calc R . . H23C H 0.8535 0.5984 0.3286 0.050 Uiso 1 1 calc R . . C235 C 0.82473(14) 0.47873(9) 0.48594(7) 0.0288(3) Uani 1 1 d . . . H23D H 0.8454 0.4243 0.5087 0.043 Uiso 1 1 calc R . . H23E H 0.7480 0.4916 0.4937 0.043 Uiso 1 1 calc R . . H23F H 0.8569 0.5065 0.5023 0.043 Uiso 1 1 calc R . . C236 C 0.98221(13) 0.48239(10) 0.40128(9) 0.0342(4) Uani 1 1 d . . . H23G H 1.0118 0.5146 0.4143 0.051 Uiso 1 1 calc R . . H23H H 1.0071 0.4918 0.3550 0.051 Uiso 1 1 calc R . . H23I H 1.0046 0.4292 0.4276 0.051 Uiso 1 1 calc R . . C237 C 1.19930(12) 0.40098(9) 0.17296(7) 0.0270(3) Uani 1 1 d . . . C238 C 1.19466(15) 0.45217(11) 0.21018(9) 0.0369(4) Uani 1 1 d . . . H23J H 1.2654 0.4624 0.2065 0.055 Uiso 1 1 calc R . . H23K H 1.1673 0.4268 0.2563 0.055 Uiso 1 1 calc R . . H23L H 1.1483 0.4999 0.1914 0.055 Uiso 1 1 calc R . . C239 C 1.27449(13) 0.32718(11) 0.20086(8) 0.0353(4) Uani 1 1 d . . . H23M H 1.2779 0.2950 0.1767 0.053 Uiso 1 1 calc R . . H23N H 1.2488 0.3008 0.2471 0.053 Uiso 1 1 calc R . . H23O H 1.3448 0.3387 0.1965 0.053 Uiso 1 1 calc R . . C240 C 1.24300(13) 0.44207(11) 0.10128(8) 0.0340(4) Uani 1 1 d . . . H24A H 1.3127 0.4535 0.0986 0.051 Uiso 1 1 calc R . . H24B H 1.1956 0.4892 0.0825 0.051 Uiso 1 1 calc R . . H24C H 1.2486 0.4098 0.0769 0.051 Uiso 1 1 calc R . . C241 C 0.77577(11) 0.69918(8) 0.01444(7) 0.0202(3) Uani 1 1 d . . . C242 C 0.72525(12) 0.74219(8) -0.04831(7) 0.0239(3) Uani 1 1 d . . . H24D H 0.7380 0.7947 -0.0672 0.036 Uiso 1 1 calc R . . H24E H 0.6494 0.7412 -0.0379 0.036 Uiso 1 1 calc R . . H24F H 0.7562 0.7180 -0.0798 0.036 Uiso 1 1 calc R . . C243 C 0.73312(14) 0.74060(9) 0.06159(8) 0.0297(3) Uani 1 1 d . . . H24G H 0.7677 0.7148 0.1007 0.045 Uiso 1 1 calc R . . H24H H 0.6571 0.7407 0.0741 0.045 Uiso 1 1 calc R . . H24I H 0.7473 0.7928 0.0401 0.045 Uiso 1 1 calc R . . C244 C 0.89446(12) 0.69902(9) -0.00355(8) 0.0263(3) Uani 1 1 d . . . H24J H 0.9281 0.6709 0.0358 0.039 Uiso 1 1 calc R . . H24K H 0.9088 0.7511 -0.0226 0.039 Uiso 1 1 calc R . . H24L H 0.9226 0.6749 -0.0353 0.039 Uiso 1 1 calc R . . C245 C 0.62928(14) 0.40110(8) 0.04754(7) 0.0266(3) Uani 1 1 d . . . H24M H 0.6894 0.4093 0.0117 0.032 Uiso 1 1 calc R . . H24N H 0.5687 0.4402 0.0317 0.032 Uiso 1 1 calc R . . C246 C 0.60155(11) 0.32366(8) 0.06680(7) 0.0211(3) Uani 1 1 d . . . C247 C 0.58187(12) 0.27505(8) 0.13308(7) 0.0232(3) Uani 1 1 d . . . H247 H 0.5873 0.2898 0.1671 0.028 Uiso 1 1 calc R . . C248 C 0.55478(12) 0.20637(8) 0.14700(7) 0.0248(3) Uani 1 1 d . . . H248 H 0.5406 0.1729 0.1911 0.030 Uiso 1 1 calc R . . C249 C 0.54797(11) 0.18539(8) 0.09574(7) 0.0225(3) Uani 1 1 d . . . C250 C 0.52148(12) 0.11497(9) 0.10593(9) 0.0288(3) Uani 1 1 d . . . H250 H 0.5060 0.0796 0.1491 0.035 Uiso 1 1 calc R . . C251 C 0.51819(13) 0.09784(9) 0.05372(9) 0.0332(4) Uani 1 1 d . . . H251 H 0.5003 0.0506 0.0610 0.040 Uiso 1 1 calc R . . C252 C 0.54098(13) 0.14935(10) -0.01037(9) 0.0328(4) Uani 1 1 d . . . H252 H 0.5382 0.1367 -0.0461 0.039 Uiso 1 1 calc R . . C253 C 0.56717(12) 0.21775(9) -0.02196(8) 0.0273(3) Uani 1 1 d . . . H253 H 0.5829 0.2520 -0.0656 0.033 Uiso 1 1 calc R . . C254 C 0.57085(11) 0.23749(8) 0.03082(7) 0.0222(3) Uani 1 1 d . . . Cl31 Cl 0.69637(3) 0.61605(2) 0.231841(19) 0.03343(9) Uani 1 1 d . . . Cl32 Cl 0.92097(4) 0.57694(3) 0.19143(3) 0.04767(12) Uani 1 1 d . . . C3 C 0.79690(13) 0.54758(9) 0.21375(8) 0.0282(3) Uani 1 1 d . . . H3A H 0.7988 0.4997 0.2525 0.034 Uiso 1 1 calc R . . H3B H 0.7808 0.5379 0.1775 0.034 Uiso 1 1 calc R . . Cl41 Cl 0.13862(4) 0.90480(3) 0.30344(3) 0.05570(14) Uani 1 1 d . . . Cl42 Cl -0.02831(4) 0.86682(3) 0.26401(3) 0.05473(14) Uani 1 1 d . . . C4 C 0.01151(15) 0.93386(11) 0.28245(9) 0.0410(4) Uani 1 1 d . . . H4A H -0.0383 0.9427 0.3193 0.049 Uiso 1 1 calc R . . H4B H 0.0095 0.9822 0.2442 0.049 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 P1 0.01942(18) 0.02091(18) 0.01586(16) -0.00710(14) -0.00264(13) 0.00208(14) O11 0.0201(5) 0.0178(5) 0.0171(5) -0.0068(4) -0.0014(4) -0.0005(4) O12 0.0235(5) 0.0223(5) 0.0163(5) -0.0063(4) -0.0021(4) 0.0032(4) O13 0.0182(5) 0.0215(5) 0.0194(5) -0.0083(4) -0.0034(4) -0.0029(4) O14 0.0178(5) 0.0168(5) 0.0178(5) -0.0058(4) -0.0006(4) 0.0019(4) N1 0.0226(6) 0.0229(6) 0.0220(6) -0.0085(5) 0.0005(5) -0.0008(5) C11 0.0200(7) 0.0140(6) 0.0180(6) -0.0065(5) -0.0021(5) -0.0029(5) C12 0.0227(7) 0.0139(6) 0.0173(6) -0.0068(5) 0.0003(5) -0.0049(5) C13 0.0230(7) 0.0170(6) 0.0176(6) -0.0068(5) -0.0015(5) -0.0042(5) C14 0.0214(7) 0.0190(7) 0.0219(7) -0.0092(6) 0.0007(5) -0.0056(5) C15 0.0233(7) 0.0203(7) 0.0197(7) -0.0084(6) 0.0053(5) -0.0086(6) C16 0.0267(7) 0.0136(6) 0.0166(6) -0.0062(5) 0.0001(5) -0.0049(5) C17 0.0279(7) 0.0167(7) 0.0161(6) -0.0042(5) 0.0010(5) -0.0057(6) C18 0.0227(7) 0.0210(7) 0.0127(6) -0.0050(5) -0.0017(5) 0.0010(5) C19 0.0272(7) 0.0165(6) 0.0128(6) -0.0022(5) -0.0012(5) -0.0045(6) C110 0.0220(7) 0.0208(7) 0.0158(6) -0.0046(5) 0.0004(5) -0.0049(6) C111 0.0227(7) 0.0211(7) 0.0161(6) -0.0060(5) -0.0008(5) -0.0019(6) C112 0.0255(7) 0.0237(7) 0.0179(7) -0.0097(6) -0.0023(5) -0.0038(6) C113 0.0219(7) 0.0275(8) 0.0156(6) -0.0080(6) -0.0027(5) -0.0027(6) C114 0.0216(7) 0.0376(9) 0.0202(7) -0.0138(6) -0.0024(6) -0.0041(6) C115 0.0163(6) 0.0219(7) 0.0232(7) -0.0107(6) -0.0059(5) 0.0002(5) C116 0.0176(7) 0.0261(7) 0.0230(7) -0.0113(6) -0.0046(5) 0.0015(6) C117 0.0230(7) 0.0313(8) 0.0262(7) -0.0180(6) -0.0056(6) 0.0014(6) C118 0.0234(7) 0.0255(8) 0.0337(8) -0.0180(7) -0.0066(6) -0.0001(6) C119 0.0200(7) 0.0207(7) 0.0298(8) -0.0108(6) -0.0052(6) -0.0008(6) C120 0.0160(6) 0.0199(7) 0.0229(7) -0.0092(6) -0.0057(5) 0.0019(5) C121 0.0171(6) 0.0209(7) 0.0206(7) -0.0073(6) -0.0029(5) -0.0029(5) C122 0.0188(6) 0.0157(6) 0.0133(6) -0.0036(5) -0.0010(5) -0.0007(5) C123 0.0172(6) 0.0204(7) 0.0150(6) -0.0056(5) -0.0008(5) -0.0039(5) C124 0.0207(7) 0.0164(6) 0.0201(7) -0.0063(5) -0.0019(5) -0.0038(5) C125 0.0182(7) 0.0172(6) 0.0158(6) -0.0047(5) -0.0005(5) -0.0006(5) C126 0.0162(6) 0.0199(7) 0.0156(6) -0.0054(5) -0.0022(5) -0.0025(5) C127 0.0192(6) 0.0180(6) 0.0124(6) -0.0056(5) 0.0010(5) -0.0047(5) C128 0.0202(7) 0.0185(7) 0.0158(6) -0.0073(5) -0.0018(5) -0.0040(5) C129 0.0194(7) 0.0281(8) 0.0241(7) -0.0108(6) 0.0007(6) -0.0051(6) C130 0.0230(8) 0.0375(9) 0.0376(9) -0.0190(7) -0.0012(6) -0.0109(7) C131 0.0218(8) 0.0499(11) 0.0299(9) -0.0086(8) 0.0033(7) -0.0046(7) C132 0.0277(8) 0.0295(8) 0.0334(8) -0.0121(7) -0.0087(7) -0.0002(6) C133 0.0230(7) 0.0252(7) 0.0233(7) -0.0116(6) -0.0005(6) -0.0028(6) C34A 0.0254(11) 0.0423(14) 0.0532(15) -0.0291(12) 0.0002(10) -0.0021(10) C35A 0.0383(14) 0.0336(13) 0.0572(16) -0.0216(12) 0.0060(12) -0.0009(11) C36A 0.0360(14) 0.0701(19) 0.0381(14) -0.0338(14) -0.0003(11) 0.0018(13) C34B 0.019(2) 0.021(2) 0.028(3) -0.022(2) 0.000(2) 0.0024(19) C35B 0.016(2) 0.025(3) 0.029(3) -0.018(2) -0.005(2) 0.011(2) C36B 0.026(3) 0.014(2) 0.028(3) -0.010(2) 0.018(2) -0.003(2) C137 0.0352(9) 0.0374(9) 0.0418(9) -0.0261(8) -0.0038(7) -0.0101(7) C138 0.0387(11) 0.0615(13) 0.0804(16) -0.0451(12) -0.0141(10) -0.0126(10) C139 0.0606(13) 0.0350(10) 0.0515(11) -0.0254(9) 0.0005(10) -0.0168(9) C140 0.0634(14) 0.0557(12) 0.0485(11) -0.0334(10) -0.0049(10) -0.0237(11) C141 0.0204(7) 0.0174(7) 0.0214(7) -0.0044(6) -0.0032(5) 0.0014(5) C142 0.0215(8) 0.0241(8) 0.0372(9) -0.0011(7) -0.0068(7) 0.0017(6) C143 0.0429(10) 0.0236(8) 0.0322(9) -0.0123(7) -0.0093(7) 0.0081(7) C144 0.0260(8) 0.0197(7) 0.0252(7) -0.0018(6) -0.0030(6) -0.0009(6) C145 0.0251(7) 0.0222(7) 0.0165(6) -0.0054(6) -0.0004(6) 0.0011(6) C146 0.0157(6) 0.0179(7) 0.0223(7) -0.0075(5) -0.0002(5) -0.0033(5) C147 0.0181(7) 0.0230(7) 0.0216(7) -0.0087(6) -0.0009(5) -0.0045(5) C148 0.0176(7) 0.0247(7) 0.0239(7) -0.0040(6) -0.0033(5) -0.0067(6) C149 0.0149(6) 0.0180(7) 0.0327(8) -0.0071(6) -0.0012(6) -0.0048(5) C150 0.0180(7) 0.0206(7) 0.0463(10) -0.0060(7) -0.0061(7) -0.0028(6) C151 0.0201(8) 0.0199(8) 0.0651(12) -0.0154(8) -0.0024(8) 0.0003(6) C152 0.0310(9) 0.0308(9) 0.0562(11) -0.0267(9) 0.0067(8) -0.0036(7) C153 0.0294(8) 0.0298(8) 0.0369(9) -0.0184(7) 0.0019(7) -0.0015(7) C154 0.0201(7) 0.0200(7) 0.0303(8) -0.0107(6) 0.0001(6) -0.0035(6) P2 0.02333(18) 0.01967(18) 0.01618(16) -0.00634(14) -0.00077(13) -0.00843(14) O21 0.0177(5) 0.0203(5) 0.0191(5) -0.0074(4) 0.0007(4) -0.0038(4) O22 0.0296(5) 0.0211(5) 0.0162(5) -0.0060(4) -0.0014(4) -0.0120(4) O23 0.0226(5) 0.0176(5) 0.0173(5) -0.0063(4) -0.0023(4) -0.0049(4) O24 0.0253(5) 0.0173(5) 0.0179(5) -0.0049(4) -0.0046(4) -0.0070(4) N2 0.0230(6) 0.0218(6) 0.0244(6) -0.0102(5) -0.0041(5) -0.0043(5) C21 0.0168(6) 0.0201(7) 0.0227(7) -0.0089(6) 0.0012(5) -0.0054(5) C22 0.0191(7) 0.0193(7) 0.0222(7) -0.0065(6) 0.0007(5) -0.0089(5) C23 0.0199(7) 0.0214(7) 0.0253(7) -0.0067(6) -0.0005(6) -0.0059(6) C24 0.0220(7) 0.0241(7) 0.0320(8) -0.0123(6) 0.0002(6) -0.0049(6) C25 0.0240(7) 0.0286(8) 0.0248(7) -0.0141(6) 0.0031(6) -0.0073(6) C26 0.0207(7) 0.0251(7) 0.0214(7) -0.0094(6) 0.0004(5) -0.0086(6) C27 0.0214(7) 0.0325(8) 0.0202(7) -0.0122(6) 0.0015(6) -0.0058(6) C28 0.0274(7) 0.0178(7) 0.0129(6) -0.0038(5) -0.0017(5) -0.0095(6) C29 0.0240(7) 0.0219(7) 0.0145(6) -0.0060(5) -0.0009(5) -0.0054(6) C210 0.0255(7) 0.0188(7) 0.0169(6) -0.0080(5) -0.0004(5) -0.0022(6) C211 0.0248(7) 0.0177(7) 0.0144(6) -0.0042(5) -0.0035(5) -0.0053(5) C212 0.0226(7) 0.0174(7) 0.0155(6) -0.0040(5) -0.0043(5) -0.0020(5) C213 0.0283(7) 0.0142(6) 0.0107(6) -0.0026(5) -0.0015(5) -0.0041(5) C214 0.0276(7) 0.0142(6) 0.0155(6) -0.0043(5) -0.0054(5) -0.0005(5) C215 0.0198(7) 0.0131(6) 0.0194(6) -0.0079(5) -0.0029(5) -0.0010(5) C216 0.0267(7) 0.0138(6) 0.0165(6) -0.0073(5) -0.0027(5) -0.0006(5) C217 0.0249(7) 0.0196(7) 0.0195(7) -0.0083(6) -0.0079(6) 0.0011(6) C218 0.0234(7) 0.0204(7) 0.0226(7) -0.0097(6) -0.0061(6) -0.0009(6) C219 0.0225(7) 0.0173(7) 0.0177(6) -0.0064(5) -0.0025(5) -0.0011(5) C220 0.0224(7) 0.0147(6) 0.0170(6) -0.0069(5) -0.0050(5) -0.0001(5) C221 0.0199(7) 0.0189(7) 0.0156(6) -0.0071(5) -0.0036(5) -0.0014(5) C222 0.0219(7) 0.0163(6) 0.0134(6) -0.0037(5) -0.0028(5) -0.0053(5) C223 0.0210(7) 0.0183(6) 0.0117(6) -0.0056(5) -0.0031(5) -0.0017(5) C224 0.0166(6) 0.0216(7) 0.0128(6) -0.0052(5) -0.0007(5) -0.0046(5) C225 0.0218(7) 0.0178(6) 0.0133(6) -0.0044(5) -0.0026(5) -0.0047(5) C226 0.0192(7) 0.0184(7) 0.0179(6) -0.0053(5) -0.0022(5) -0.0007(5) C227 0.0181(7) 0.0215(7) 0.0142(6) -0.0044(5) -0.0021(5) -0.0044(5) C228 0.0191(7) 0.0226(7) 0.0196(7) -0.0061(6) -0.0025(5) -0.0055(5) C229 0.0291(8) 0.0341(9) 0.0342(9) -0.0173(7) -0.0002(7) 0.0031(7) C30C 0.0262(12) 0.0601(18) 0.084(2) -0.0349(16) 0.0034(13) -0.0014(12) C31C 0.0463(16) 0.0319(13) 0.079(2) -0.0231(14) 0.0059(14) 0.0034(11) C32C 0.078(3) 0.112(3) 0.060(2) -0.059(2) -0.0196(19) 0.056(2) C30D 0.029(4) 0.048(5) 0.041(4) -0.023(4) -0.008(3) 0.010(3) C31D 0.046(5) 0.037(4) 0.094(7) -0.045(5) -0.030(5) 0.010(4) C32D 0.044(5) 0.048(6) 0.049(6) 0.003(4) 0.027(4) 0.016(4) C233 0.0296(8) 0.0198(7) 0.0231(7) -0.0098(6) -0.0076(6) -0.0036(6) C234 0.0495(10) 0.0200(8) 0.0354(9) -0.0089(7) -0.0154(8) -0.0086(7) C235 0.0378(9) 0.0278(8) 0.0255(8) -0.0141(6) -0.0084(7) -0.0023(7) C236 0.0308(9) 0.0393(9) 0.0450(10) -0.0259(8) -0.0045(7) -0.0110(7) C237 0.0248(8) 0.0353(9) 0.0227(7) -0.0105(6) -0.0057(6) -0.0066(6) C238 0.0361(9) 0.0477(11) 0.0368(9) -0.0205(8) -0.0071(7) -0.0150(8) C239 0.0250(8) 0.0459(10) 0.0318(9) -0.0118(8) -0.0088(7) -0.0006(7) C240 0.0273(8) 0.0465(10) 0.0281(8) -0.0090(7) -0.0051(7) -0.0139(7) C241 0.0223(7) 0.0167(7) 0.0190(7) -0.0038(5) -0.0012(5) -0.0054(5) C242 0.0247(7) 0.0195(7) 0.0223(7) -0.0018(6) -0.0033(6) -0.0051(6) C243 0.0398(9) 0.0218(7) 0.0280(8) -0.0107(6) 0.0011(7) -0.0092(7) C244 0.0245(8) 0.0210(7) 0.0285(8) -0.0015(6) -0.0050(6) -0.0082(6) C245 0.0395(9) 0.0226(7) 0.0209(7) -0.0071(6) -0.0082(6) -0.0096(7) C246 0.0210(7) 0.0207(7) 0.0222(7) -0.0076(6) -0.0046(5) -0.0036(5) C247 0.0254(7) 0.0247(7) 0.0206(7) -0.0078(6) -0.0048(6) -0.0058(6) C248 0.0237(7) 0.0238(7) 0.0238(7) -0.0041(6) -0.0050(6) -0.0060(6) C249 0.0148(6) 0.0215(7) 0.0310(8) -0.0094(6) -0.0062(6) -0.0005(5) C250 0.0231(8) 0.0211(7) 0.0425(9) -0.0112(7) -0.0075(7) -0.0031(6) C251 0.0273(8) 0.0233(8) 0.0553(11) -0.0204(8) -0.0094(7) -0.0020(6) C252 0.0271(8) 0.0341(9) 0.0480(10) -0.0287(8) -0.0080(7) 0.0024(7) C253 0.0238(8) 0.0303(8) 0.0320(8) -0.0178(7) -0.0036(6) -0.0009(6) C254 0.0170(7) 0.0227(7) 0.0292(8) -0.0133(6) -0.0042(6) -0.0001(5) Cl31 0.0376(2) 0.02652(19) 0.02937(19) -0.00663(16) -0.00186(16) -0.00265(16) Cl32 0.0332(2) 0.0555(3) 0.0555(3) -0.0230(2) -0.0015(2) -0.0101(2) C3 0.0359(9) 0.0248(8) 0.0237(7) -0.0086(6) -0.0030(6) -0.0071(7) Cl41 0.0496(3) 0.0657(3) 0.0531(3) -0.0200(3) -0.0190(2) -0.0051(3) Cl42 0.0539(3) 0.0561(3) 0.0440(3) 0.0004(2) -0.0158(2) -0.0174(2) C4 0.0414(10) 0.0414(10) 0.0268(8) -0.0076(8) -0.0027(7) 0.0067(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O11 1.6186(10) . ? P1 O12 1.6323(10) . ? P1 O13 1.6521(10) . ? O11 C11 1.4053(17) . ? O12 C18 1.4006(17) . ? O13 C115 1.4164(17) . ? O14 C122 1.3920(16) . ? O14 C145 1.4279(16) . ? N1 C146 1.3177(18) . ? N1 C154 1.3698(19) . ? C11 C16 1.3978(19) . ? C11 C12 1.4056(19) . ? C12 C13 1.386(2) . ? C12 C128 1.5125(18) . ? C13 C14 1.3995(19) . ? C13 H13 0.9500 . ? C14 C15 1.388(2) . ? C14 C129 1.536(2) . ? C15 C16 1.398(2) . ? C15 H15 0.9500 . ? C16 C17 1.5108(19) . ? C17 C19 1.506(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.384(2) . ? C18 C113 1.386(2) . ? C19 C110 1.396(2) . ? C110 C111 1.393(2) . ? C110 H110 0.9500 . ? C111 C112 1.399(2) . ? C111 C133 1.535(2) . ? C112 C113 1.390(2) . ? C112 H112 0.9500 . ? C113 C114 1.512(2) . ? C114 C116 1.519(2) . ? C114 H11A 0.9900 . ? C114 H11B 0.9900 . ? C115 C116 1.401(2) . ? C115 C120 1.410(2) . ? C116 C117 1.405(2) . ? C117 C118 1.382(2) . ? C117 H117 0.9500 . ? C118 C119 1.393(2) . ? C118 C137 1.538(2) . ? C119 C120 1.391(2) . ? C119 H119 0.9500 . ? C120 C121 1.5203(19) . ? C121 C123 1.5083(19) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 C127 1.3829(19) . ? C122 C123 1.3933(19) . ? C123 C124 1.3856(19) . ? C124 C125 1.402(2) . ? C124 H124 0.9500 . ? C125 C126 1.3930(19) . ? C125 C141 1.5360(19) . ? C126 C127 1.3986(19) . ? C126 H126 0.9500 . ? C127 C128 1.5102(18) . ? C128 H12C 0.9900 . ? C128 H12D 0.9900 . ? C129 C131 1.530(2) . ? C129 C130 1.535(2) . ? C129 C132 1.537(2) . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C131 H13F 0.9800 . ? C132 H13G 0.9800 . ? C132 H13H 0.9800 . ? C132 H13I 0.9800 . ? C133 C35A 1.508(3) . ? C133 C36B 1.525(4) . ? C133 C36A 1.528(3) . ? C133 C34A 1.537(3) . ? C133 C35B 1.544(4) . ? C133 C34B 1.565(4) . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C137 C140 1.532(3) . ? C137 C139 1.535(3) . ? C137 C138 1.538(3) . ? C138 H13J 0.9800 . ? C138 H13K 0.9800 . ? C138 H13L 0.9800 . ? C139 H13M 0.9800 . ? C139 H13N 0.9800 . ? C139 H13O 0.9800 . ? C140 H14A 0.9800 . ? C140 H14B 0.9800 . ? C140 H14C 0.9800 . ? C141 C142 1.532(2) . ? C141 C143 1.536(2) . ? C141 C144 1.537(2) . ? C142 H14D 0.9800 . ? C142 H14E 0.9800 . ? C142 H14F 0.9800 . ? C143 H14G 0.9800 . ? C143 H14H 0.9800 . ? C143 H14I 0.9800 . ? C144 H14J 0.9800 . ? C144 H14K 0.9800 . ? C144 H14L 0.9800 . ? C145 C146 1.5036(19) . ? C145 H14M 0.9900 . ? C145 H14N 0.9900 . ? C146 C147 1.415(2) . ? C147 C148 1.364(2) . ? C147 H147 0.9500 . ? C148 C149 1.411(2) . ? C148 H148 0.9500 . ? C149 C154 1.416(2) . ? C149 C150 1.420(2) . ? C150 C151 1.365(3) . ? C150 H150 0.9500 . ? C151 C152 1.405(3) . ? C151 H151 0.9500 . ? C152 C153 1.367(2) . ? C152 H152 0.9500 . ? C153 C154 1.416(2) . ? C153 H153 0.9500 . ? P2 O23 1.6216(10) . ? P2 O22 1.6377(10) . ? P2 O21 1.6475(10) . ? O21 C21 1.4136(17) . ? O22 C28 1.4000(16) . ? O23 C215 1.4039(17) . ? O24 C222 1.3976(16) . ? O24 C245 1.4270(17) . ? N2 C246 1.3176(19) . ? N2 C254 1.3704(19) . ? C21 C26 1.402(2) . ? C21 C22 1.407(2) . ? C22 C23 1.389(2) . ? C22 C228 1.5210(19) . ? C23 C24 1.395(2) . ? C23 H23 0.9500 . ? C24 C25 1.389(2) . ? C24 C229 1.533(2) . ? C25 C26 1.396(2) . ? C25 H25 0.9500 . ? C26 C27 1.519(2) . ? C27 C29 1.506(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C213 1.382(2) . ? C28 C29 1.391(2) . ? C29 C210 1.390(2) . ? C210 C211 1.401(2) . ? C210 H210 0.9500 . ? C211 C212 1.392(2) . ? C211 C233 1.5362(19) . ? C212 C213 1.399(2) . ? C212 H212 0.9500 . ? C213 C214 1.5085(19) . ? C214 C216 1.5127(19) . ? C214 H21A 0.9900 . ? C214 H21B 0.9900 . ? C215 C216 1.3999(19) . ? C215 C220 1.4045(19) . ? C216 C217 1.389(2) . ? C217 C218 1.395(2) . ? C217 H217 0.9500 . ? C218 C219 1.394(2) . ? C218 C237 1.532(2) . ? C219 C220 1.396(2) . ? C219 H219 0.9500 . ? C220 C221 1.5164(18) . ? C221 C223 1.5088(19) . ? C221 H22A 0.9900 . ? C221 H22B 0.9900 . ? C222 C223 1.3789(19) . ? C222 C227 1.394(2) . ? C223 C224 1.4033(19) . ? C224 C225 1.3924(19) . ? C224 H224 0.9500 . ? C225 C226 1.3992(19) . ? C225 C241 1.5361(19) . ? C226 C227 1.391(2) . ? C226 H226 0.9500 . ? C227 C228 1.5089(19) . ? C228 H22C 0.9900 . ? C228 H22D 0.9900 . ? C229 C32D 1.478(5) . ? C229 C31C 1.491(3) . ? C229 C32C 1.525(3) . ? C229 C30D 1.543(5) . ? C229 C30C 1.569(3) . ? C229 C31D 1.571(5) . ? C30C H30A 0.9800 . ? C30C H30B 0.9800 . ? C30C H30C 0.9800 . ? C31C H31A 0.9800 . ? C31C H31B 0.9800 . ? C31C H31C 0.9800 . ? C32C H32A 0.9800 . ? C32C H32B 0.9800 . ? C32C H32C 0.9800 . ? C30D H30D 0.9800 . ? C30D H30E 0.9800 . ? C30D H30F 0.9800 . ? C31D H31D 0.9800 . ? C31D H31E 0.9800 . ? C31D H31F 0.9800 . ? C32D H32D 0.9800 . ? C32D H32E 0.9800 . ? C32D H32F 0.9800 . ? C233 C236 1.530(2) . ? C233 C234 1.537(2) . ? C233 C235 1.538(2) . ? C234 H23A 0.9800 . ? C234 H23B 0.9800 . ? C234 H23C 0.9800 . ? C235 H23D 0.9800 . ? C235 H23E 0.9800 . ? C235 H23F 0.9800 . ? C236 H23G 0.9800 . ? C236 H23H 0.9800 . ? C236 H23I 0.9800 . ? C237 C240 1.532(2) . ? C237 C239 1.535(2) . ? C237 C238 1.540(2) . ? C238 H23J 0.9800 . ? C238 H23K 0.9800 . ? C238 H23L 0.9800 . ? C239 H23M 0.9800 . ? C239 H23N 0.9800 . ? C239 H23O 0.9800 . ? C240 H24A 0.9800 . ? C240 H24B 0.9800 . ? C240 H24C 0.9800 . ? C241 C244 1.529(2) . ? C241 C243 1.534(2) . ? C241 C242 1.538(2) . ? C242 H24D 0.9800 . ? C242 H24E 0.9800 . ? C242 H24F 0.9800 . ? C243 H24G 0.9800 . ? C243 H24H 0.9800 . ? C243 H24I 0.9800 . ? C244 H24J 0.9800 . ? C244 H24K 0.9800 . ? C244 H24L 0.9800 . ? C245 C246 1.509(2) . ? C245 H24M 0.9900 . ? C245 H24N 0.9900 . ? C246 C247 1.415(2) . ? C247 C248 1.367(2) . ? C247 H247 0.9500 . ? C248 C249 1.409(2) . ? C248 H248 0.9500 . ? C249 C250 1.419(2) . ? C249 C254 1.420(2) . ? C250 C251 1.368(2) . ? C250 H250 0.9500 . ? C251 C252 1.402(3) . ? C251 H251 0.9500 . ? C252 C253 1.370(2) . ? C252 H252 0.9500 . ? C253 C254 1.414(2) . ? C253 H253 0.9500 . ? Cl31 C3 1.7680(17) . ? Cl32 C3 1.7609(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? Cl41 C4 1.752(2) . ? Cl42 C4 1.747(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 O11 P1 O12 104.70(5) . . ? O11 P1 O13 100.75(5) . . ? O12 P1 O13 100.11(5) . . ? C11 O11 P1 146.02(9) . . ? C18 O12 P1 123.08(8) . . ? C115 O13 P1 125.45(9) . . ? C122 O14 C145 112.40(10) . . ? C146 N1 C154 117.47(13) . . ? C16 C11 O11 122.53(12) . . ? C16 C11 C12 119.70(13) . . ? O11 C11 C12 117.22(12) . . ? C13 C12 C11 118.85(12) . . ? C13 C12 C128 119.54(12) . . ? C11 C12 C128 121.60(12) . . ? C12 C13 C14 122.93(13) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C15 C14 C13 116.25(13) . . ? C15 C14 C129 123.88(13) . . ? C13 C14 C129 119.85(13) . . ? C14 C15 C16 123.06(13) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C11 C16 C15 118.64(13) . . ? C11 C16 C17 122.69(13) . . ? C15 C16 C17 118.65(12) . . ? C19 C17 C16 109.85(11) . . ? C19 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? C19 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C113 122.45(13) . . ? C19 C18 O12 118.91(13) . . ? C113 C18 O12 118.61(13) . . ? C18 C19 C110 117.73(13) . . ? C18 C19 C17 120.04(13) . . ? C110 C19 C17 122.03(13) . . ? C111 C110 C19 122.27(14) . . ? C111 C110 H110 118.9 . . ? C19 C110 H110 118.9 . . ? C110 C111 C112 117.47(13) . . ? C110 C111 C133 121.61(13) . . ? C112 C111 C133 120.92(13) . . ? C113 C112 C111 121.95(13) . . ? C113 C112 H112 119.0 . . ? C111 C112 H112 119.0 . . ? C18 C113 C112 118.13(13) . . ? C18 C113 C114 119.65(13) . . ? C112 C113 C114 122.09(13) . . ? C113 C114 C116 119.39(12) . . ? C113 C114 H11A 107.5 . . ? C116 C114 H11A 107.5 . . ? C113 C114 H11B 107.5 . . ? C116 C114 H11B 107.5 . . ? H11A C114 H11B 107.0 . . ? C116 C115 C120 120.10(13) . . ? C116 C115 O13 120.77(12) . . ? C120 C115 O13 118.87(12) . . ? C115 C116 C117 118.27(13) . . ? C115 C116 C114 126.24(13) . . ? C117 C116 C114 115.33(13) . . ? C118 C117 C116 123.15(14) . . ? C118 C117 H117 118.4 . . ? C116 C117 H117 118.4 . . ? C117 C118 C119 116.71(14) . . ? C117 C118 C137 123.37(14) . . ? C119 C118 C137 119.88(14) . . ? C120 C119 C118 123.13(14) . . ? C120 C119 H119 118.4 . . ? C118 C119 H119 118.4 . . ? C119 C120 C115 118.51(13) . . ? C119 C120 C121 116.61(13) . . ? C115 C120 C121 124.82(12) . . ? C123 C121 C120 113.92(11) . . ? C123 C121 H12A 108.8 . . ? C120 C121 H12A 108.8 . . ? C123 C121 H12B 108.8 . . ? C120 C121 H12B 108.8 . . ? H12A C121 H12B 107.7 . . ? C127 C122 O14 119.67(12) . . ? C127 C122 C123 121.15(12) . . ? O14 C122 C123 118.98(12) . . ? C124 C123 C122 118.61(13) . . ? C124 C123 C121 121.86(12) . . ? C122 C123 C121 119.39(12) . . ? C123 C124 C125 122.03(13) . . ? C123 C124 H124 119.0 . . ? C125 C124 H124 119.0 . . ? C126 C125 C124 117.06(12) . . ? C126 C125 C141 122.21(12) . . ? C124 C125 C141 120.66(12) . . ? C125 C126 C127 122.11(13) . . ? C125 C126 H126 118.9 . . ? C127 C126 H126 118.9 . . ? C122 C127 C126 118.40(12) . . ? C122 C127 C128 120.28(12) . . ? C126 C127 C128 121.07(12) . . ? C127 C128 C12 110.23(11) . . ? C127 C128 H12C 109.6 . . ? C12 C128 H12C 109.6 . . ? C127 C128 H12D 109.6 . . ? C12 C128 H12D 109.6 . . ? H12C C128 H12D 108.1 . . ? C131 C129 C130 108.91(13) . . ? C131 C129 C14 111.77(13) . . ? C130 C129 C14 110.44(12) . . ? C131 C129 C132 108.03(13) . . ? C130 C129 C132 109.01(13) . . ? C14 C129 C132 108.62(12) . . ? C129 C130 H13A 109.5 . . ? C129 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? C129 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? C129 C131 H13D 109.5 . . ? C129 C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? C129 C131 H13F 109.5 . . ? H13D C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? C129 C132 H13G 109.5 . . ? C129 C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? C129 C132 H13I 109.5 . . ? H13G C132 H13I 109.5 . . ? H13H C132 H13I 109.5 . . ? C35A C133 C36A 111.04(18) . . ? C35A C133 C111 108.97(14) . . ? C36B C133 C111 111.8(2) . . ? C36A C133 C111 108.52(14) . . ? C35A C133 C34A 109.41(17) . . ? C36A C133 C34A 107.46(17) . . ? C111 C133 C34A 111.44(14) . . ? C36B C133 C35B 108.6(3) . . ? C111 C133 C35B 110.1(2) . . ? C36B C133 C34B 106.7(3) . . ? C111 C133 C34B 113.7(2) . . ? C35B C133 C34B 105.6(3) . . ? C133 C34A H34A 109.5 . . ? C133 C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C133 C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C133 C35A H35A 109.5 . . ? C133 C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C133 C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C133 C36A H36A 109.5 . . ? C133 C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C133 C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C133 C34B H34D 109.5 . . ? C133 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C133 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C133 C35B H35D 109.5 . . ? C133 C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C133 C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C133 C36B H36D 109.5 . . ? C133 C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C133 C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C140 C137 C139 108.46(15) . . ? C140 C137 C138 108.21(17) . . ? C139 C137 C138 109.96(17) . . ? C140 C137 C118 112.20(15) . . ? C139 C137 C118 109.82(15) . . ? C138 C137 C118 108.17(14) . . ? C137 C138 H13J 109.5 . . ? C137 C138 H13K 109.5 . . ? H13J C138 H13K 109.5 . . ? C137 C138 H13L 109.5 . . ? H13J C138 H13L 109.5 . . ? H13K C138 H13L 109.5 . . ? C137 C139 H13M 109.5 . . ? C137 C139 H13N 109.5 . . ? H13M C139 H13N 109.5 . . ? C137 C139 H13O 109.5 . . ? H13M C139 H13O 109.5 . . ? H13N C139 H13O 109.5 . . ? C137 C140 H14A 109.5 . . ? C137 C140 H14B 109.5 . . ? H14A C140 H14B 109.5 . . ? C137 C140 H14C 109.5 . . ? H14A C140 H14C 109.5 . . ? H14B C140 H14C 109.5 . . ? C142 C141 C143 108.57(13) . . ? C142 C141 C125 112.36(12) . . ? C143 C141 C125 111.26(12) . . ? C142 C141 C144 108.43(12) . . ? C143 C141 C144 109.40(13) . . ? C125 C141 C144 106.75(11) . . ? C141 C142 H14D 109.5 . . ? C141 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? C141 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? C141 C143 H14G 109.5 . . ? C141 C143 H14H 109.5 . . ? H14G C143 H14H 109.5 . . ? C141 C143 H14I 109.5 . . ? H14G C143 H14I 109.5 . . ? H14H C143 H14I 109.5 . . ? C141 C144 H14J 109.5 . . ? C141 C144 H14K 109.5 . . ? H14J C144 H14K 109.5 . . ? C141 C144 H14L 109.5 . . ? H14J C144 H14L 109.5 . . ? H14K C144 H14L 109.5 . . ? O14 C145 C146 109.43(11) . . ? O14 C145 H14M 109.8 . . ? C146 C145 H14M 109.8 . . ? O14 C145 H14N 109.8 . . ? C146 C145 H14N 109.8 . . ? H14M C145 H14N 108.2 . . ? N1 C146 C147 124.00(13) . . ? N1 C146 C145 114.88(12) . . ? C147 C146 C145 121.11(12) . . ? C148 C147 C146 118.67(13) . . ? C148 C147 H147 120.7 . . ? C146 C147 H147 120.7 . . ? C147 C148 C149 119.72(14) . . ? C147 C148 H148 120.1 . . ? C149 C148 H148 120.1 . . ? C148 C149 C154 117.46(13) . . ? C148 C149 C150 123.35(15) . . ? C154 C149 C150 119.17(14) . . ? C151 C150 C149 120.33(16) . . ? C151 C150 H150 119.8 . . ? C149 C150 H150 119.8 . . ? C150 C151 C152 120.25(15) . . ? C150 C151 H151 119.9 . . ? C152 C151 H151 119.9 . . ? C153 C152 C151 121.09(16) . . ? C153 C152 H152 119.5 . . ? C151 C152 H152 119.5 . . ? C152 C153 C154 119.97(17) . . ? C152 C153 H153 120.0 . . ? C154 C153 H153 120.0 . . ? N1 C154 C149 122.67(13) . . ? N1 C154 C153 118.13(14) . . ? C149 C154 C153 119.19(14) . . ? O23 P2 O22 105.53(5) . . ? O23 P2 O21 100.57(5) . . ? O22 P2 O21 99.45(5) . . ? C21 O21 P2 124.89(8) . . ? C28 O22 P2 122.13(8) . . ? C215 O23 P2 146.41(9) . . ? C222 O24 C245 111.58(10) . . ? C246 N2 C254 117.65(13) . . ? C26 C21 C22 120.13(13) . . ? C26 C21 O21 120.96(13) . . ? C22 C21 O21 118.67(12) . . ? C23 C22 C21 118.83(13) . . ? C23 C22 C228 117.42(13) . . ? C21 C22 C228 123.71(13) . . ? C22 C23 C24 122.80(14) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 116.45(14) . . ? C25 C24 C229 122.47(14) . . ? C23 C24 C229 121.07(14) . . ? C24 C25 C26 123.49(14) . . ? C24 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C25 C26 C21 118.09(13) . . ? C25 C26 C27 115.50(13) . . ? C21 C26 C27 126.25(13) . . ? C29 C27 C26 119.37(12) . . ? C29 C27 H27A 107.5 . . ? C26 C27 H27A 107.5 . . ? C29 C27 H27B 107.5 . . ? C26 C27 H27B 107.5 . . ? H27A C27 H27B 107.0 . . ? C213 C28 C29 122.34(13) . . ? C213 C28 O22 118.76(12) . . ? C29 C28 O22 118.88(13) . . ? C210 C29 C28 117.77(13) . . ? C210 C29 C27 122.06(13) . . ? C28 C29 C27 120.04(13) . . ? C29 C210 C211 122.33(13) . . ? C29 C210 H210 118.8 . . ? C211 C210 H210 118.8 . . ? C212 C211 C210 117.44(13) . . ? C212 C211 C233 122.13(13) . . ? C210 C211 C233 120.41(12) . . ? C211 C212 C213 121.96(13) . . ? C211 C212 H212 119.0 . . ? C213 C212 H212 119.0 . . ? C28 C213 C212 118.13(13) . . ? C28 C213 C214 120.01(12) . . ? C212 C213 C214 121.55(13) . . ? C213 C214 C216 108.16(11) . . ? C213 C214 H21A 110.1 . . ? C216 C214 H21A 110.1 . . ? C213 C214 H21B 110.1 . . ? C216 C214 H21B 110.1 . . ? H21A C214 H21B 108.4 . . ? C216 C215 O23 121.75(12) . . ? C216 C215 C220 119.82(13) . . ? O23 C215 C220 117.83(12) . . ? C217 C216 C215 118.76(13) . . ? C217 C216 C214 118.70(12) . . ? C215 C216 C214 122.44(13) . . ? C216 C217 C218 123.17(13) . . ? C216 C217 H217 118.4 . . ? C218 C217 H217 118.4 . . ? C219 C218 C217 116.18(13) . . ? C219 C218 C237 124.05(13) . . ? C217 C218 C237 119.76(13) . . ? C218 C219 C220 122.99(13) . . ? C218 C219 H219 118.5 . . ? C220 C219 H219 118.5 . . ? C219 C220 C215 118.52(12) . . ? C219 C220 C221 119.48(12) . . ? C215 C220 C221 121.98(12) . . ? C223 C221 C220 111.80(11) . . ? C223 C221 H22A 109.3 . . ? C220 C221 H22A 109.3 . . ? C223 C221 H22B 109.3 . . ? C220 C221 H22B 109.3 . . ? H22A C221 H22B 107.9 . . ? C223 C222 C227 121.34(12) . . ? C223 C222 O24 119.69(12) . . ? C227 C222 O24 118.81(12) . . ? C222 C223 C224 118.36(12) . . ? C222 C223 C221 120.64(12) . . ? C224 C223 C221 120.85(12) . . ? C225 C224 C223 121.92(13) . . ? C225 C224 H224 119.0 . . ? C223 C224 H224 119.0 . . ? C224 C225 C226 117.19(12) . . ? C224 C225 C241 122.97(12) . . ? C226 C225 C241 119.82(12) . . ? C227 C226 C225 122.09(13) . . ? C227 C226 H226 119.0 . . ? C225 C226 H226 119.0 . . ? C226 C227 C222 118.22(13) . . ? C226 C227 C228 121.39(13) . . ? C222 C227 C228 120.17(12) . . ? C227 C228 C22 113.59(11) . . ? C227 C228 H22C 108.8 . . ? C22 C228 H22C 108.8 . . ? C227 C228 H22D 108.8 . . ? C22 C228 H22D 108.8 . . ? H22C C228 H22D 107.7 . . ? C31C C229 C32C 111.3(2) . . ? C32D C229 C24 112.1(4) . . ? C31C C229 C24 110.94(16) . . ? C32C C229 C24 112.77(17) . . ? C32D C229 C30D 110.3(4) . . ? C24 C229 C30D 114.1(3) . . ? C31C C229 C30C 108.3(2) . . ? C32C C229 C30C 106.0(2) . . ? C24 C229 C30C 107.29(15) . . ? C32D C229 C31D 109.9(4) . . ? C24 C229 C31D 104.7(3) . . ? C30D C229 C31D 105.2(4) . . ? C30C C229 C31D 147.3(3) . . ? C229 C30C H30A 109.5 . . ? C229 C30C H30B 109.5 . . ? H30A C30C H30B 109.5 . . ? C229 C30C H30C 109.5 . . ? H30A C30C H30C 109.5 . . ? H30B C30C H30C 109.5 . . ? C229 C31C H31A 109.5 . . ? C229 C31C H31B 109.5 . . ? H31A C31C H31B 109.5 . . ? C229 C31C H31C 109.5 . . ? H31A C31C H31C 109.5 . . ? H31B C31C H31C 109.5 . . ? C229 C32C H32A 109.5 . . ? C229 C32C H32B 109.5 . . ? H32A C32C H32B 109.5 . . ? C229 C32C H32C 109.5 . . ? H32A C32C H32C 109.5 . . ? H32B C32C H32C 109.5 . . ? C229 C30D H30D 109.5 . . ? C229 C30D H30E 109.5 . . ? H30D C30D H30E 109.5 . . ? C229 C30D H30F 109.5 . . ? H30D C30D H30F 109.5 . . ? H30E C30D H30F 109.5 . . ? C229 C31D H31D 109.5 . . ? C229 C31D H31E 109.5 . . ? H31D C31D H31E 109.5 . . ? C229 C31D H31F 109.5 . . ? H31D C31D H31F 109.5 . . ? H31E C31D H31F 109.5 . . ? C229 C32D H32D 109.5 . . ? C229 C32D H32E 109.5 . . ? H32D C32D H32E 109.5 . . ? C229 C32D H32F 109.5 . . ? H32D C32D H32F 109.5 . . ? H32E C32D H32F 109.5 . . ? C236 C233 C211 112.00(12) . . ? C236 C233 C234 107.88(14) . . ? C211 C233 C234 110.21(12) . . ? C236 C233 C235 108.34(13) . . ? C211 C233 C235 108.09(12) . . ? C234 C233 C235 110.31(13) . . ? C233 C234 H23A 109.5 . . ? C233 C234 H23B 109.5 . . ? H23A C234 H23B 109.5 . . ? C233 C234 H23C 109.5 . . ? H23A C234 H23C 109.5 . . ? H23B C234 H23C 109.5 . . ? C233 C235 H23D 109.5 . . ? C233 C235 H23E 109.5 . . ? H23D C235 H23E 109.5 . . ? C233 C235 H23F 109.5 . . ? H23D C235 H23F 109.5 . . ? H23E C235 H23F 109.5 . . ? C233 C236 H23G 109.5 . . ? C233 C236 H23H 109.5 . . ? H23G C236 H23H 109.5 . . ? C233 C236 H23I 109.5 . . ? H23G C236 H23I 109.5 . . ? H23H C236 H23I 109.5 . . ? C218 C237 C240 112.40(12) . . ? C218 C237 C239 110.19(13) . . ? C240 C237 C239 108.32(14) . . ? C218 C237 C238 108.15(13) . . ? C240 C237 C238 108.10(14) . . ? C239 C237 C238 109.64(13) . . ? C237 C238 H23J 109.5 . . ? C237 C238 H23K 109.5 . . ? H23J C238 H23K 109.5 . . ? C237 C238 H23L 109.5 . . ? H23J C238 H23L 109.5 . . ? H23K C238 H23L 109.5 . . ? C237 C239 H23M 109.5 . . ? C237 C239 H23N 109.5 . . ? H23M C239 H23N 109.5 . . ? C237 C239 H23O 109.5 . . ? H23M C239 H23O 109.5 . . ? H23N C239 H23O 109.5 . . ? C237 C240 H24A 109.5 . . ? C237 C240 H24B 109.5 . . ? H24A C240 H24B 109.5 . . ? C237 C240 H24C 109.5 . . ? H24A C240 H24C 109.5 . . ? H24B C240 H24C 109.5 . . ? C244 C241 C243 108.35(12) . . ? C244 C241 C225 112.29(12) . . ? C243 C241 C225 110.77(11) . . ? C244 C241 C242 108.39(12) . . ? C243 C241 C242 109.24(12) . . ? C225 C241 C242 107.74(11) . . ? C241 C242 H24D 109.5 . . ? C241 C242 H24E 109.5 . . ? H24D C242 H24E 109.5 . . ? C241 C242 H24F 109.5 . . ? H24D C242 H24F 109.5 . . ? H24E C242 H24F 109.5 . . ? C241 C243 H24G 109.5 . . ? C241 C243 H24H 109.5 . . ? H24G C243 H24H 109.5 . . ? C241 C243 H24I 109.5 . . ? H24G C243 H24I 109.5 . . ? H24H C243 H24I 109.5 . . ? C241 C244 H24J 109.5 . . ? C241 C244 H24K 109.5 . . ? H24J C244 H24K 109.5 . . ? C241 C244 H24L 109.5 . . ? H24J C244 H24L 109.5 . . ? H24K C244 H24L 109.5 . . ? O24 C245 C246 109.93(12) . . ? O24 C245 H24M 109.7 . . ? C246 C245 H24M 109.7 . . ? O24 C245 H24N 109.7 . . ? C246 C245 H24N 109.7 . . ? H24M C245 H24N 108.2 . . ? N2 C246 C247 124.10(13) . . ? N2 C246 C245 114.30(12) . . ? C247 C246 C245 121.60(13) . . ? C248 C247 C246 118.45(14) . . ? C248 C247 H247 120.8 . . ? C246 C247 H247 120.8 . . ? C247 C248 C249 119.83(14) . . ? C247 C248 H248 120.1 . . ? C249 C248 H248 120.1 . . ? C248 C249 C250 123.39(14) . . ? C248 C249 C254 117.56(13) . . ? C250 C249 C254 119.04(14) . . ? C251 C250 C249 120.21(16) . . ? C251 C250 H250 119.9 . . ? C249 C250 H250 119.9 . . ? C250 C251 C252 120.65(15) . . ? C250 C251 H251 119.7 . . ? C252 C251 H251 119.7 . . ? C253 C252 C251 120.66(15) . . ? C253 C252 H252 119.7 . . ? C251 C252 H252 119.7 . . ? C252 C253 C254 120.23(15) . . ? C252 C253 H253 119.9 . . ? C254 C253 H253 119.9 . . ? N2 C254 C253 118.39(14) . . ? N2 C254 C249 122.39(13) . . ? C253 C254 C249 119.22(14) . . ? Cl32 C3 Cl31 111.85(9) . . ? Cl32 C3 H3A 109.2 . . ? Cl31 C3 H3A 109.2 . . ? Cl32 C3 H3B 109.2 . . ? Cl31 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? Cl42 C4 Cl41 111.95(10) . . ? Cl42 C4 H4A 109.2 . . ? Cl41 C4 H4A 109.2 . . ? Cl42 C4 H4B 109.2 . . ? Cl41 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 P1 O11 C11 -47.09(16) . . . . ? O13 P1 O11 C11 56.47(16) . . . . ? O11 P1 O12 C18 68.46(12) . . . . ? O13 P1 O12 C18 -35.59(12) . . . . ? O11 P1 O13 C115 170.66(10) . . . . ? O12 P1 O13 C115 -82.11(11) . . . . ? P1 O11 C11 C16 55.6(2) . . . . ? P1 O11 C11 C12 -132.94(14) . . . . ? C16 C11 C12 C13 -7.52(19) . . . . ? O11 C11 C12 C13 -179.22(11) . . . . ? C16 C11 C12 C128 173.39(12) . . . . ? O11 C11 C12 C128 1.70(18) . . . . ? C11 C12 C13 C14 1.5(2) . . . . ? C128 C12 C13 C14 -179.44(12) . . . . ? C12 C13 C14 C15 3.9(2) . . . . ? C12 C13 C14 C129 -174.71(13) . . . . ? C13 C14 C15 C16 -3.4(2) . . . . ? C129 C14 C15 C16 175.16(13) . . . . ? O11 C11 C16 C15 179.23(12) . . . . ? C12 C11 C16 C15 7.99(19) . . . . ? O11 C11 C16 C17 -2.3(2) . . . . ? C12 C11 C16 C17 -173.52(12) . . . . ? C14 C15 C16 C11 -2.5(2) . . . . ? C14 C15 C16 C17 178.98(13) . . . . ? C11 C16 C17 C19 -80.12(16) . . . . ? C15 C16 C17 C19 98.36(15) . . . . ? P1 O12 C18 C19 -93.21(14) . . . . ? P1 O12 C18 C113 88.95(14) . . . . ? C113 C18 C19 C110 0.1(2) . . . . ? O12 C18 C19 C110 -177.68(12) . . . . ? C113 C18 C19 C17 -174.80(13) . . . . ? O12 C18 C19 C17 7.44(19) . . . . ? C16 C17 C19 C18 91.60(16) . . . . ? C16 C17 C19 C110 -83.06(16) . . . . ? C18 C19 C110 C111 0.7(2) . . . . ? C17 C19 C110 C111 175.44(13) . . . . ? C19 C110 C111 C112 -0.9(2) . . . . ? C19 C110 C111 C133 179.34(12) . . . . ? C110 C111 C112 C113 0.3(2) . . . . ? C133 C111 C112 C113 -179.86(13) . . . . ? C19 C18 C113 C112 -0.6(2) . . . . ? O12 C18 C113 C112 177.19(12) . . . . ? C19 C18 C113 C114 -176.54(13) . . . . ? O12 C18 C113 C114 1.22(19) . . . . ? C111 C112 C113 C18 0.3(2) . . . . ? C111 C112 C113 C114 176.22(13) . . . . ? C18 C113 C114 C116 -85.40(18) . . . . ? C112 C113 C114 C116 98.79(17) . . . . ? P1 O13 C115 C116 78.20(15) . . . . ? P1 O13 C115 C120 -107.55(13) . . . . ? C120 C115 C116 C117 -4.0(2) . . . . ? O13 C115 C116 C117 170.21(12) . . . . ? C120 C115 C116 C114 171.13(14) . . . . ? O13 C115 C116 C114 -14.7(2) . . . . ? C113 C114 C116 C115 48.7(2) . . . . ? C113 C114 C116 C117 -136.11(14) . . . . ? C115 C116 C117 C118 1.7(2) . . . . ? C114 C116 C117 C118 -173.93(14) . . . . ? C116 C117 C118 C119 1.3(2) . . . . ? C116 C117 C118 C137 179.32(14) . . . . ? C117 C118 C119 C120 -2.2(2) . . . . ? C137 C118 C119 C120 179.76(14) . . . . ? C118 C119 C120 C115 0.0(2) . . . . ? C118 C119 C120 C121 177.22(13) . . . . ? C116 C115 C120 C119 3.2(2) . . . . ? O13 C115 C120 C119 -171.10(12) . . . . ? C116 C115 C120 C121 -173.82(13) . . . . ? O13 C115 C120 C121 11.9(2) . . . . ? C119 C120 C121 C123 129.48(13) . . . . ? C115 C120 C121 C123 -53.46(18) . . . . ? C145 O14 C122 C127 -95.43(14) . . . . ? C145 O14 C122 C123 89.73(15) . . . . ? C127 C122 C123 C124 8.33(19) . . . . ? O14 C122 C123 C124 -176.90(12) . . . . ? C127 C122 C123 C121 -167.37(12) . . . . ? O14 C122 C123 C121 7.39(18) . . . . ? C120 C121 C123 C124 -69.89(17) . . . . ? C120 C121 C123 C122 105.66(14) . . . . ? C122 C123 C124 C125 -2.8(2) . . . . ? C121 C123 C124 C125 172.78(13) . . . . ? C123 C124 C125 C126 -4.1(2) . . . . ? C123 C124 C125 C141 173.09(12) . . . . ? C124 C125 C126 C127 5.82(19) . . . . ? C141 C125 C126 C127 -171.28(12) . . . . ? O14 C122 C127 C126 178.62(11) . . . . ? C123 C122 C127 C126 -6.65(19) . . . . ? O14 C122 C127 C128 -7.10(18) . . . . ? C123 C122 C127 C128 167.63(12) . . . . ? C125 C126 C127 C122 -0.62(19) . . . . ? C125 C126 C127 C128 -174.85(12) . . . . ? C122 C127 C128 C12 -107.57(14) . . . . ? C126 C127 C128 C12 66.55(16) . . . . ? C13 C12 C128 C127 -103.73(14) . . . . ? C11 C12 C128 C127 75.34(16) . . . . ? C15 C14 C129 C131 2.1(2) . . . . ? C13 C14 C129 C131 -179.42(14) . . . . ? C15 C14 C129 C130 123.49(15) . . . . ? C13 C14 C129 C130 -58.01(18) . . . . ? C15 C14 C129 C132 -117.02(15) . . . . ? C13 C14 C129 C132 61.48(17) . . . . ? C110 C111 C133 C35A 118.68(18) . . . . ? C112 C111 C133 C35A -61.1(2) . . . . ? C110 C111 C133 C36B -61.5(3) . . . . ? C112 C111 C133 C36B 118.7(3) . . . . ? C110 C111 C133 C36A -120.28(18) . . . . ? C112 C111 C133 C36A 59.9(2) . . . . ? C110 C111 C133 C34A -2.2(2) . . . . ? C112 C111 C133 C34A 178.05(16) . . . . ? C110 C111 C133 C35B 59.3(3) . . . . ? C112 C111 C133 C35B -120.5(2) . . . . ? C110 C111 C133 C34B 177.6(2) . . . . ? C112 C111 C133 C34B -2.2(3) . . . . ? C117 C118 C137 C140 6.5(2) . . . . ? C119 C118 C137 C140 -175.61(16) . . . . ? C117 C118 C137 C139 127.17(17) . . . . ? C119 C118 C137 C139 -54.9(2) . . . . ? C117 C118 C137 C138 -112.81(19) . . . . ? C119 C118 C137 C138 65.1(2) . . . . ? C126 C125 C141 C142 -15.49(19) . . . . ? C124 C125 C141 C142 167.51(13) . . . . ? C126 C125 C141 C143 -137.47(14) . . . . ? C124 C125 C141 C143 45.54(18) . . . . ? C126 C125 C141 C144 103.24(15) . . . . ? C124 C125 C141 C144 -73.76(16) . . . . ? C122 O14 C145 C146 -173.47(11) . . . . ? C154 N1 C146 C147 -1.2(2) . . . . ? C154 N1 C146 C145 179.91(13) . . . . ? O14 C145 C146 N1 -158.46(12) . . . . ? O14 C145 C146 C147 22.59(19) . . . . ? N1 C146 C147 C148 0.6(2) . . . . ? C145 C146 C147 C148 179.46(13) . . . . ? C146 C147 C148 C149 0.7(2) . . . . ? C147 C148 C149 C154 -1.3(2) . . . . ? C147 C148 C149 C150 176.75(14) . . . . ? C148 C149 C150 C151 -178.56(14) . . . . ? C154 C149 C150 C151 -0.6(2) . . . . ? C149 C150 C151 C152 -0.1(2) . . . . ? C150 C151 C152 C153 0.4(3) . . . . ? C151 C152 C153 C154 -0.1(3) . . . . ? C146 N1 C154 C149 0.5(2) . . . . ? C146 N1 C154 C153 -177.85(14) . . . . ? C148 C149 C154 N1 0.7(2) . . . . ? C150 C149 C154 N1 -177.39(14) . . . . ? C148 C149 C154 C153 179.03(14) . . . . ? C150 C149 C154 C153 0.9(2) . . . . ? C152 C153 C154 N1 177.78(15) . . . . ? C152 C153 C154 C149 -0.6(2) . . . . ? O23 P2 O21 C21 170.71(10) . . . . ? O22 P2 O21 C21 -81.40(11) . . . . ? O23 P2 O22 C28 65.84(11) . . . . ? O21 P2 O22 C28 -38.00(11) . . . . ? O22 P2 O23 C215 -45.04(17) . . . . ? O21 P2 O23 C215 57.98(16) . . . . ? P2 O21 C21 C26 81.24(15) . . . . ? P2 O21 C21 C22 -104.36(13) . . . . ? C26 C21 C22 C23 4.3(2) . . . . ? O21 C21 C22 C23 -170.12(12) . . . . ? C26 C21 C22 C228 -173.55(13) . . . . ? O21 C21 C22 C228 12.0(2) . . . . ? C21 C22 C23 C24 -0.6(2) . . . . ? C228 C22 C23 C24 177.40(13) . . . . ? C22 C23 C24 C25 -2.4(2) . . . . ? C22 C23 C24 C229 178.01(14) . . . . ? C23 C24 C25 C26 1.8(2) . . . . ? C229 C24 C25 C26 -178.62(14) . . . . ? C24 C25 C26 C21 1.8(2) . . . . ? C24 C25 C26 C27 -173.88(14) . . . . ? C22 C21 C26 C25 -4.9(2) . . . . ? O21 C21 C26 C25 169.46(12) . . . . ? C22 C21 C26 C27 170.29(13) . . . . ? O21 C21 C26 C27 -15.4(2) . . . . ? C25 C26 C27 C29 -138.62(14) . . . . ? C21 C26 C27 C29 46.1(2) . . . . ? P2 O22 C28 C213 -91.81(14) . . . . ? P2 O22 C28 C29 89.26(14) . . . . ? C213 C28 C29 C210 0.7(2) . . . . ? O22 C28 C29 C210 179.63(12) . . . . ? C213 C28 C29 C27 -175.39(13) . . . . ? O22 C28 C29 C27 3.51(19) . . . . ? C26 C27 C29 C210 99.35(16) . . . . ? C26 C27 C29 C28 -84.70(18) . . . . ? C28 C29 C210 C211 0.5(2) . . . . ? C27 C29 C210 C211 176.50(13) . . . . ? C29 C210 C211 C212 -1.0(2) . . . . ? C29 C210 C211 C233 -179.59(13) . . . . ? C210 C211 C212 C213 0.3(2) . . . . ? C233 C211 C212 C213 178.93(12) . . . . ? C29 C28 C213 C212 -1.3(2) . . . . ? O22 C28 C213 C212 179.77(11) . . . . ? C29 C28 C213 C214 -175.05(12) . . . . ? O22 C28 C213 C214 6.05(18) . . . . ? C211 C212 C213 C28 0.8(2) . . . . ? C211 C212 C213 C214 174.38(12) . . . . ? C28 C213 C214 C216 94.53(15) . . . . ? C212 C213 C214 C216 -78.96(16) . . . . ? P2 O23 C215 C216 56.9(2) . . . . ? P2 O23 C215 C220 -131.97(14) . . . . ? O23 C215 C216 C217 178.07(12) . . . . ? C220 C215 C216 C217 7.10(19) . . . . ? O23 C215 C216 C214 -5.49(19) . . . . ? C220 C215 C216 C214 -176.46(12) . . . . ? C213 C214 C216 C217 97.89(15) . . . . ? C213 C214 C216 C215 -78.55(16) . . . . ? C215 C216 C217 C218 -1.0(2) . . . . ? C214 C216 C217 C218 -177.53(13) . . . . ? C216 C217 C218 C219 -4.0(2) . . . . ? C216 C217 C218 C237 175.21(13) . . . . ? C217 C218 C219 C220 2.9(2) . . . . ? C237 C218 C219 C220 -176.25(13) . . . . ? C218 C219 C220 C215 3.0(2) . . . . ? C218 C219 C220 C221 -175.58(13) . . . . ? C216 C215 C220 C219 -8.08(19) . . . . ? O23 C215 C220 C219 -179.40(11) . . . . ? C216 C215 C220 C221 170.49(12) . . . . ? O23 C215 C220 C221 -0.83(18) . . . . ? C219 C220 C221 C223 -107.54(14) . . . . ? C215 C220 C221 C223 73.90(16) . . . . ? C245 O24 C222 C223 -96.09(15) . . . . ? C245 O24 C222 C227 88.45(15) . . . . ? C227 C222 C223 C224 -8.61(19) . . . . ? O24 C222 C223 C224 176.05(11) . . . . ? C227 C222 C223 C221 167.06(12) . . . . ? O24 C222 C223 C221 -8.29(18) . . . . ? C220 C221 C223 C222 -105.30(14) . . . . ? C220 C221 C223 C224 70.26(16) . . . . ? C222 C223 C224 C225 0.62(19) . . . . ? C221 C223 C224 C225 -175.04(12) . . . . ? C223 C224 C225 C226 5.98(19) . . . . ? C223 C224 C225 C241 -172.20(12) . . . . ? C224 C225 C226 C227 -5.0(2) . . . . ? C241 C225 C226 C227 173.26(12) . . . . ? C225 C226 C227 C222 -2.5(2) . . . . ? C225 C226 C227 C228 172.19(13) . . . . ? C223 C222 C227 C226 9.6(2) . . . . ? O24 C222 C227 C226 -175.06(12) . . . . ? C223 C222 C227 C228 -165.24(12) . . . . ? O24 C222 C227 C228 10.14(19) . . . . ? C226 C227 C228 C22 -66.43(17) . . . . ? C222 C227 C228 C22 108.20(15) . . . . ? C23 C22 C228 C227 126.50(14) . . . . ? C21 C22 C228 C227 -55.60(18) . . . . ? C25 C24 C229 C32D -48.8(5) . . . . ? C23 C24 C229 C32D 130.8(5) . . . . ? C25 C24 C229 C31C 125.6(2) . . . . ? C23 C24 C229 C31C -54.8(2) . . . . ? C25 C24 C229 C32C 0.1(3) . . . . ? C23 C24 C229 C32C 179.7(2) . . . . ? C25 C24 C229 C30D -175.1(3) . . . . ? C23 C24 C229 C30D 4.5(4) . . . . ? C25 C24 C229 C30C -116.29(19) . . . . ? C23 C24 C229 C30C 63.3(2) . . . . ? C25 C24 C229 C31D 70.4(4) . . . . ? C23 C24 C229 C31D -110.0(4) . . . . ? C212 C211 C233 C236 11.18(19) . . . . ? C210 C211 C233 C236 -170.28(13) . . . . ? C212 C211 C233 C234 131.28(15) . . . . ? C210 C211 C233 C234 -50.17(18) . . . . ? C212 C211 C233 C235 -108.10(15) . . . . ? C210 C211 C233 C235 70.45(16) . . . . ? C219 C218 C237 C240 -1.7(2) . . . . ? C217 C218 C237 C240 179.22(14) . . . . ? C219 C218 C237 C239 -122.60(15) . . . . ? C217 C218 C237 C239 58.31(18) . . . . ? C219 C218 C237 C238 117.57(16) . . . . ? C217 C218 C237 C238 -61.52(18) . . . . ? C224 C225 C241 C244 -5.56(19) . . . . ? C226 C225 C241 C244 176.30(13) . . . . ? C224 C225 C241 C243 -126.84(14) . . . . ? C226 C225 C241 C243 55.02(17) . . . . ? C224 C225 C241 C242 113.73(14) . . . . ? C226 C225 C241 C242 -64.41(16) . . . . ? C222 O24 C245 C246 176.93(12) . . . . ? C254 N2 C246 C247 -0.1(2) . . . . ? C254 N2 C246 C245 -179.41(13) . . . . ? O24 C245 C246 N2 -166.75(12) . . . . ? O24 C245 C246 C247 13.9(2) . . . . ? N2 C246 C247 C248 -0.8(2) . . . . ? C245 C246 C247 C248 178.51(14) . . . . ? C246 C247 C248 C249 0.5(2) . . . . ? C247 C248 C249 C250 179.33(14) . . . . ? C247 C248 C249 C254 0.5(2) . . . . ? C248 C249 C250 C251 -178.83(15) . . . . ? C254 C249 C250 C251 0.0(2) . . . . ? C249 C250 C251 C252 0.1(2) . . . . ? C250 C251 C252 C253 0.1(2) . . . . ? C251 C252 C253 C254 -0.4(2) . . . . ? C246 N2 C254 C253 -178.80(13) . . . . ? C246 N2 C254 C249 1.2(2) . . . . ? C252 C253 C254 N2 -179.51(14) . . . . ? C252 C253 C254 C249 0.5(2) . . . . ? C248 C249 C254 N2 -1.4(2) . . . . ? C250 C249 C254 N2 179.72(13) . . . . ? C248 C249 C254 C253 178.59(13) . . . . ? C250 C249 C254 C253 -0.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.423 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.046 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.004 0.244 0.884 169.3 43.9 2 0.004 0.756 0.116 169.4 44.3 3 0.500 0.500 0.500 259.9 79.9 _platon_squeeze_details ; ? ; #===END data_s3333a _database_code_depnum_ccdc_archive 'CCDC 699254' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H63 Cl N O4 P Pd, 2(C4 H10 O)' _chemical_formula_sum 'C63 H83 Cl N O6 P Pd' _chemical_formula_weight 1123.12 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' 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 0.0060 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.1478(2) _cell_length_b 12.93260(10) _cell_length_c 18.91510(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.6368(3) _cell_angle_gamma 90.00 _cell_volume 6375.38(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 192444 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99310 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14575 _reflns_number_gt 10908 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, SortAV' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0516P)^2^+2.8673P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14575 _refine_ls_number_parameters 706 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.171730(6) 1.065127(14) 0.508258(9) 0.02059(6) Uani 1 1 d . . . Cl1 Cl 0.13396(2) 1.07605(6) 0.61680(3) 0.03891(18) Uani 1 1 d . . . P1 P 0.21452(2) 1.05888(5) 0.41353(3) 0.01840(13) Uani 1 1 d . . . O1 O 0.17741(6) 1.03691(13) 0.34493(8) 0.0214(3) Uani 1 1 d . . . O2 O 0.24187(6) 1.16716(12) 0.39937(8) 0.0212(3) Uani 1 1 d . . . O3 O 0.26054(6) 0.97677(12) 0.40647(8) 0.0203(3) Uani 1 1 d . . . O4 O 0.17296(6) 0.86291(12) 0.42886(8) 0.0227(4) Uani 1 1 d . . . N1 N 0.09766(7) 1.00640(16) 0.45762(10) 0.0233(4) Uani 1 1 d . . . C1 C 0.17106(8) 1.03366(19) 0.27000(12) 0.0208(5) Uani 1 1 d . . . C2 C 0.14665(9) 0.94599(18) 0.23990(13) 0.0230(5) Uani 1 1 d . . . C3 C 0.13828(9) 0.94279(19) 0.16644(13) 0.0243(5) Uani 1 1 d . . . H3 H 0.1231 0.8824 0.1452 0.029 Uiso 1 1 calc R . . C4 C 0.15100(9) 1.0234(2) 0.12229(13) 0.0259(5) Uani 1 1 d . . . C5 C 0.17169(9) 1.11132(19) 0.15558(13) 0.0243(5) Uani 1 1 d . . . H5 H 0.1793 1.1690 0.1271 0.029 Uiso 1 1 calc R . . C6 C 0.18187(8) 1.11886(18) 0.22881(12) 0.0221(5) Uani 1 1 d . . . C7 C 0.20368(8) 1.21874(18) 0.26006(13) 0.0222(5) Uani 1 1 d . . . H7A H 0.1858 1.2372 0.3025 0.027 Uiso 1 1 calc R . . H7B H 0.1979 1.2752 0.2249 0.027 Uiso 1 1 calc R . . C8 C 0.27755(8) 1.17715(18) 0.34786(12) 0.0209(5) Uani 1 1 d . . . C9 C 0.26057(8) 1.20739(18) 0.28041(12) 0.0220(5) Uani 1 1 d . . . C10 C 0.29709(9) 1.22133(19) 0.23156(13) 0.0242(5) Uani 1 1 d . . . H10 H 0.2860 1.2415 0.1845 0.029 Uiso 1 1 calc R . . C11 C 0.34921(9) 1.20674(19) 0.24940(12) 0.0255(5) Uani 1 1 d D A . C12 C 0.36412(9) 1.17629(19) 0.31870(13) 0.0259(5) Uani 1 1 d . . . H12 H 0.3996 1.1661 0.3320 0.031 Uiso 1 1 calc R . . C13 C 0.32906(9) 1.16032(18) 0.36905(12) 0.0230(5) Uani 1 1 d . . . C14 C 0.34519(9) 1.13218(19) 0.44475(12) 0.0242(5) Uani 1 1 d . . . H14A H 0.3223 1.1692 0.4755 0.029 Uiso 1 1 calc R . . H14B H 0.3803 1.1592 0.4562 0.029 Uiso 1 1 calc R . . C15 C 0.30363(8) 0.94963(18) 0.45278(12) 0.0208(5) Uani 1 1 d . . . C16 C 0.34516(8) 1.01836(19) 0.46513(12) 0.0216(5) Uani 1 1 d . . . C17 C 0.38942(8) 0.9812(2) 0.50368(12) 0.0253(5) Uani 1 1 d . . . H17 H 0.4176 1.0271 0.5121 0.030 Uiso 1 1 calc R . . C18 C 0.39437(9) 0.8814(2) 0.53022(12) 0.0257(5) Uani 1 1 d . . . C19 C 0.35202(9) 0.8176(2) 0.51790(13) 0.0265(5) Uani 1 1 d . . . H19 H 0.3541 0.7491 0.5361 0.032 Uiso 1 1 calc R . . C20 C 0.30655(8) 0.84842(19) 0.48032(12) 0.0229(5) Uani 1 1 d . . . C21 C 0.26357(9) 0.76963(19) 0.47587(13) 0.0252(5) Uani 1 1 d . . . H21A H 0.2771 0.7039 0.4967 0.030 Uiso 1 1 calc R . . H21B H 0.2364 0.7941 0.5054 0.030 Uiso 1 1 calc R . . C22 C 0.19350(8) 0.79616(18) 0.38068(12) 0.0214(5) Uani 1 1 d . . . C23 C 0.23947(9) 0.74788(19) 0.40241(13) 0.0235(5) Uani 1 1 d . . . C24 C 0.26288(9) 0.68577(19) 0.35423(13) 0.0260(5) Uani 1 1 d . . . H24 H 0.2938 0.6509 0.3693 0.031 Uiso 1 1 calc R . . C25 C 0.24213(10) 0.67344(19) 0.28457(13) 0.0287(6) Uani 1 1 d . . . C26 C 0.19711(9) 0.72651(19) 0.26444(13) 0.0270(5) Uani 1 1 d . . . H26 H 0.1824 0.7195 0.2171 0.032 Uiso 1 1 calc R . . C27 C 0.17285(9) 0.78953(18) 0.31105(13) 0.0234(5) Uani 1 1 d . . . C28 C 0.12852(9) 0.85751(19) 0.28363(13) 0.0245(5) Uani 1 1 d . . . H28A H 0.1033 0.8156 0.2542 0.029 Uiso 1 1 calc R . . H28B H 0.1112 0.8854 0.3242 0.029 Uiso 1 1 calc R . . C29 C 0.14150(10) 1.0127(2) 0.04183(13) 0.0307(6) Uani 1 1 d . . . C30 C 0.08516(12) 0.9860(3) 0.02148(15) 0.0513(9) Uani 1 1 d . . . H30A H 0.0631 1.0397 0.0394 0.077 Uiso 1 1 calc R . . H30B H 0.0770 0.9192 0.0423 0.077 Uiso 1 1 calc R . . H30C H 0.0793 0.9821 -0.0303 0.077 Uiso 1 1 calc R . . C31 C 0.17632(12) 0.9263(2) 0.01654(15) 0.0399(7) Uani 1 1 d . . . H31A H 0.1701 0.9181 -0.0349 0.060 Uiso 1 1 calc R . . H31B H 0.1686 0.8613 0.0400 0.060 Uiso 1 1 calc R . . H31C H 0.2123 0.9448 0.0285 0.060 Uiso 1 1 calc R . . C32 C 0.15496(12) 1.1125(2) 0.00354(14) 0.0413(7) Uani 1 1 d . . . H32A H 0.1351 1.1701 0.0209 0.062 Uiso 1 1 calc R . . H32B H 0.1467 1.1042 -0.0476 0.062 Uiso 1 1 calc R . . H32C H 0.1917 1.1269 0.0129 0.062 Uiso 1 1 calc R . . C33 C 0.38906(9) 1.2263(2) 0.19591(14) 0.0371(7) Uani 1 1 d D . . C34A C 0.36672(18) 1.2594(5) 0.1249(2) 0.0566(19) Uani 0.617(5) 1 d PD A 1 H34A H 0.3944 1.2748 0.0946 0.085 Uiso 0.617(5) 1 calc PR A 1 H34B H 0.3458 1.3214 0.1297 0.085 Uiso 0.617(5) 1 calc PR A 1 H34C H 0.3452 1.2038 0.1035 0.085 Uiso 0.617(5) 1 calc PR A 1 C35A C 0.42475(19) 1.1346(4) 0.1935(3) 0.0561(18) Uani 0.617(5) 1 d PD A 1 H35A H 0.4056 1.0747 0.1738 0.084 Uiso 0.617(5) 1 calc PR A 1 H35B H 0.4393 1.1185 0.2416 0.084 Uiso 0.617(5) 1 calc PR A 1 H35C H 0.4525 1.1512 0.1636 0.084 Uiso 0.617(5) 1 calc PR A 1 C36A C 0.42321(18) 1.3203(4) 0.2279(3) 0.0591(18) Uani 0.617(5) 1 d PD A 1 H36A H 0.4495 1.3373 0.1956 0.089 Uiso 0.617(5) 1 calc PR A 1 H36B H 0.4398 1.3004 0.2742 0.089 Uiso 0.617(5) 1 calc PR A 1 H36C H 0.4013 1.3807 0.2335 0.089 Uiso 0.617(5) 1 calc PR A 1 C34B C 0.3842(3) 1.3362(4) 0.1658(4) 0.043(2) Uani 0.383(5) 1 d PD A 2 H34D H 0.4076 1.3446 0.1283 0.065 Uiso 0.383(5) 1 calc PR A 2 H34E H 0.3930 1.3863 0.2037 0.065 Uiso 0.383(5) 1 calc PR A 2 H34F H 0.3489 1.3480 0.1461 0.065 Uiso 0.383(5) 1 calc PR A 2 C35B C 0.3747(3) 1.1539(6) 0.1283(3) 0.045(2) Uani 0.383(5) 1 d PD A 2 H35D H 0.3402 1.1712 0.1076 0.068 Uiso 0.383(5) 1 calc PR A 2 H35E H 0.3756 1.0812 0.1430 0.068 Uiso 0.383(5) 1 calc PR A 2 H35F H 0.3995 1.1650 0.0929 0.068 Uiso 0.383(5) 1 calc PR A 2 C36B C 0.44307(18) 1.2012(7) 0.2206(4) 0.044(2) Uani 0.383(5) 1 d PD A 2 H36D H 0.4653 1.2152 0.1825 0.065 Uiso 0.383(5) 1 calc PR A 2 H36E H 0.4456 1.1280 0.2337 0.065 Uiso 0.383(5) 1 calc PR A 2 H36F H 0.4539 1.2439 0.2620 0.065 Uiso 0.383(5) 1 calc PR A 2 C37 C 0.44462(9) 0.8439(2) 0.56998(14) 0.0327(6) Uani 1 1 d . . . C38 C 0.48563(10) 0.8350(3) 0.51675(17) 0.0471(8) Uani 1 1 d . . . H38A H 0.4910 0.9029 0.4954 0.071 Uiso 1 1 calc R . . H38B H 0.4742 0.7856 0.4795 0.071 Uiso 1 1 calc R . . H38C H 0.5179 0.8110 0.5413 0.071 Uiso 1 1 calc R . . C39 C 0.46193(13) 0.9204(3) 0.62809(18) 0.0537(9) Uani 1 1 d . . . H39A H 0.4698 0.9869 0.6067 0.081 Uiso 1 1 calc R . . H39B H 0.4927 0.8937 0.6552 0.081 Uiso 1 1 calc R . . H39C H 0.4345 0.9297 0.6598 0.081 Uiso 1 1 calc R . . C40 C 0.43890(11) 0.7365(3) 0.60333(17) 0.0468(8) Uani 1 1 d . . . H40A H 0.4717 0.7157 0.6281 0.070 Uiso 1 1 calc R . . H40B H 0.4290 0.6862 0.5660 0.070 Uiso 1 1 calc R . . H40C H 0.4124 0.7391 0.6371 0.070 Uiso 1 1 calc R . . C41 C 0.26806(11) 0.6018(2) 0.23301(15) 0.0373(6) Uani 1 1 d . . . C42 C 0.25690(13) 0.4890(2) 0.25319(16) 0.0464(8) Uani 1 1 d . . . H42A H 0.2732 0.4420 0.2211 0.070 Uiso 1 1 calc R . . H42B H 0.2198 0.4773 0.2492 0.070 Uiso 1 1 calc R . . H42C H 0.2707 0.4760 0.3021 0.070 Uiso 1 1 calc R . . C43 C 0.24733(14) 0.6188(2) 0.15572(15) 0.0480(8) Uani 1 1 d . . . H43A H 0.2514 0.6916 0.1431 0.072 Uiso 1 1 calc R . . H43B H 0.2109 0.6003 0.1501 0.072 Uiso 1 1 calc R . . H43C H 0.2664 0.5754 0.1245 0.072 Uiso 1 1 calc R . . C44 C 0.32618(12) 0.6208(3) 0.23855(19) 0.0542(9) Uani 1 1 d . . . H44A H 0.3329 0.6934 0.2276 0.081 Uiso 1 1 calc R . . H44B H 0.3422 0.5762 0.2048 0.081 Uiso 1 1 calc R . . H44C H 0.3406 0.6051 0.2868 0.081 Uiso 1 1 calc R . . C45 C 0.12991(9) 0.8310(2) 0.46523(13) 0.0267(5) Uani 1 1 d . . . H45A H 0.1395 0.8283 0.5169 0.032 Uiso 1 1 calc R . . H45B H 0.1188 0.7610 0.4492 0.032 Uiso 1 1 calc R . . C46 C 0.08692(9) 0.9069(2) 0.44971(12) 0.0247(5) Uani 1 1 d . . . C47 C 0.03797(9) 0.8695(2) 0.42532(13) 0.0295(6) Uani 1 1 d . . . H47 H 0.0320 0.7972 0.4212 0.035 Uiso 1 1 calc R . . C48 C -0.00084(9) 0.9379(2) 0.40756(14) 0.0322(6) Uani 1 1 d . . . H48 H -0.0342 0.9137 0.3921 0.039 Uiso 1 1 calc R . . C49 C 0.00926(9) 1.0442(2) 0.41255(13) 0.0287(6) Uani 1 1 d . . . C50 C -0.02824(9) 1.1202(2) 0.39245(14) 0.0361(7) Uani 1 1 d . . . H50 H -0.0619 1.0993 0.3760 0.043 Uiso 1 1 calc R . . C51 C -0.01659(11) 1.2223(2) 0.39647(16) 0.0431(7) Uani 1 1 d . . . H51 H -0.0420 1.2724 0.3826 0.052 Uiso 1 1 calc R . . C52 C 0.03355(11) 1.2545(2) 0.42138(17) 0.0448(7) Uani 1 1 d . . . H52 H 0.0415 1.3262 0.4240 0.054 Uiso 1 1 calc R . . C53 C 0.07046(10) 1.1834(2) 0.44156(15) 0.0362(6) Uani 1 1 d . . . H53 H 0.1038 1.2060 0.4583 0.043 Uiso 1 1 calc R . . C54 C 0.05948(9) 1.0765(2) 0.43770(13) 0.0264(5) Uani 1 1 d . . . C55 C 0.23782(8) 1.12825(17) 0.55902(11) 0.0171(4) Uani 1 1 d . . . H55A H 0.2675 1.0861 0.5489 0.026 Uiso 1 1 calc R . . H55B H 0.2348 1.1296 0.6103 0.026 Uiso 1 1 calc R . . H55C H 0.2424 1.1989 0.5418 0.026 Uiso 1 1 calc R . . O5 O 0.02147(11) 0.6221(2) 0.3021(2) 0.1013(11) Uani 1 1 d U . . C56 C -0.04956(15) 0.7347(4) 0.2785(3) 0.0808(13) Uani 1 1 d U . . H56A H -0.0495 0.7661 0.3256 0.121 Uiso 1 1 calc R . . H56B H -0.0844 0.7362 0.2552 0.121 Uiso 1 1 calc R . . H56C H -0.0265 0.7736 0.2499 0.121 Uiso 1 1 calc R . . C57 C -0.03245(16) 0.6304(5) 0.2852(4) 0.120(2) Uani 1 1 d U . . H57A H -0.0505 0.5960 0.3229 0.145 Uiso 1 1 calc R . . H57B H -0.0417 0.5935 0.2402 0.145 Uiso 1 1 calc R . . C58 C 0.03863(18) 0.5275(4) 0.2964(2) 0.0755(12) Uani 1 1 d U . . H58A H 0.0256 0.4985 0.2499 0.091 Uiso 1 1 calc R . . H58B H 0.0255 0.4840 0.3340 0.091 Uiso 1 1 calc R . . C59 C 0.09601(17) 0.5240(4) 0.3026(2) 0.0740(12) Uani 1 1 d U . . H59A H 0.1091 0.5631 0.2635 0.111 Uiso 1 1 calc R . . H59B H 0.1075 0.4520 0.3006 0.111 Uiso 1 1 calc R . . H59C H 0.1091 0.5547 0.3479 0.111 Uiso 1 1 calc R . . O6 O 0.36170(7) 0.89128(16) 0.23826(10) 0.0383(5) Uani 1 1 d U . . C60 C 0.28681(12) 0.9292(3) 0.16464(18) 0.0511(8) Uani 1 1 d U . . H60A H 0.3044 0.9833 0.1397 0.077 Uiso 1 1 calc R . . H60B H 0.2502 0.9460 0.1642 0.077 Uiso 1 1 calc R . . H60C H 0.2909 0.8627 0.1409 0.077 Uiso 1 1 calc R . . C61 C 0.30946(10) 0.9224(2) 0.23935(16) 0.0376(7) Uani 1 1 d U . . H61A H 0.3074 0.9904 0.2630 0.045 Uiso 1 1 calc R . . H61B H 0.2903 0.8713 0.2660 0.045 Uiso 1 1 calc R . . C62 C 0.38597(11) 0.8827(3) 0.30746(15) 0.0431(7) Uani 1 1 d U . . H62A H 0.3678 0.8314 0.3351 0.052 Uiso 1 1 calc R . . H62B H 0.3854 0.9502 0.3321 0.052 Uiso 1 1 calc R . . C63 C 0.44054(12) 0.8486(3) 0.30151(18) 0.0600(10) Uani 1 1 d U . . H63A H 0.4407 0.7807 0.2786 0.090 Uiso 1 1 calc R . . H63B H 0.4584 0.8441 0.3490 0.090 Uiso 1 1 calc R . . H63C H 0.4580 0.8990 0.2731 0.090 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 Pd1 0.01544(9) 0.02460(11) 0.02137(10) -0.00339(8) -0.00070(6) -0.00009(7) Cl1 0.0195(3) 0.0713(5) 0.0262(3) -0.0142(3) 0.0038(2) -0.0045(3) P1 0.0160(3) 0.0193(3) 0.0196(3) -0.0010(2) -0.0007(2) -0.0003(2) O1 0.0201(8) 0.0239(9) 0.0197(8) 0.0001(7) -0.0017(6) -0.0021(6) O2 0.0203(8) 0.0215(9) 0.0216(8) -0.0003(7) -0.0006(6) -0.0018(6) O3 0.0173(7) 0.0208(8) 0.0222(8) 0.0018(7) -0.0017(6) 0.0022(6) O4 0.0203(8) 0.0214(9) 0.0269(9) -0.0025(7) 0.0044(6) -0.0015(6) N1 0.0185(9) 0.0274(12) 0.0236(10) -0.0026(9) -0.0007(8) 0.0005(8) C1 0.0182(11) 0.0229(12) 0.0205(12) -0.0014(10) -0.0032(9) 0.0028(9) C2 0.0209(11) 0.0216(13) 0.0258(12) 0.0009(10) -0.0032(9) 0.0017(9) C3 0.0247(12) 0.0220(13) 0.0251(12) -0.0033(10) -0.0053(9) -0.0016(10) C4 0.0245(12) 0.0268(13) 0.0254(13) 0.0005(11) -0.0041(10) 0.0026(10) C5 0.0243(12) 0.0222(13) 0.0259(13) 0.0047(11) -0.0017(9) 0.0027(10) C6 0.0185(11) 0.0208(13) 0.0257(12) -0.0001(10) -0.0052(9) 0.0014(9) C7 0.0234(11) 0.0160(12) 0.0262(12) 0.0038(10) -0.0047(9) 0.0000(9) C8 0.0223(11) 0.0190(12) 0.0211(12) -0.0011(10) 0.0004(9) -0.0025(9) C9 0.0232(11) 0.0156(12) 0.0262(12) 0.0001(10) -0.0038(9) -0.0016(9) C10 0.0263(12) 0.0224(13) 0.0231(12) 0.0053(10) -0.0028(9) -0.0024(10) C11 0.0249(12) 0.0254(13) 0.0258(13) 0.0040(11) -0.0009(10) -0.0043(10) C12 0.0177(11) 0.0258(13) 0.0330(13) 0.0058(11) -0.0046(10) -0.0017(9) C13 0.0232(11) 0.0207(12) 0.0244(12) 0.0032(10) -0.0023(9) -0.0032(9) C14 0.0193(11) 0.0280(14) 0.0246(12) 0.0007(10) -0.0032(9) -0.0029(10) C15 0.0167(10) 0.0275(13) 0.0181(11) 0.0021(10) -0.0001(8) 0.0046(9) C16 0.0209(11) 0.0265(13) 0.0172(11) 0.0040(10) 0.0006(9) 0.0005(10) C17 0.0168(11) 0.0341(14) 0.0246(13) 0.0011(11) 0.0001(9) -0.0020(10) C18 0.0204(11) 0.0344(15) 0.0218(12) 0.0048(11) -0.0006(9) 0.0043(10) C19 0.0236(12) 0.0306(14) 0.0253(13) 0.0077(11) 0.0026(10) 0.0038(10) C20 0.0207(11) 0.0268(13) 0.0215(12) 0.0023(10) 0.0028(9) 0.0024(10) C21 0.0244(12) 0.0242(13) 0.0268(13) 0.0060(11) 0.0005(10) -0.0005(10) C22 0.0226(11) 0.0151(11) 0.0269(12) 0.0008(10) 0.0048(9) -0.0029(9) C23 0.0247(11) 0.0192(12) 0.0267(13) 0.0043(10) 0.0027(9) -0.0026(9) C24 0.0250(12) 0.0181(12) 0.0354(14) 0.0062(11) 0.0048(10) 0.0027(10) C25 0.0361(14) 0.0204(13) 0.0302(14) -0.0020(11) 0.0073(11) -0.0038(11) C26 0.0329(13) 0.0231(13) 0.0245(13) -0.0014(10) -0.0011(10) -0.0057(10) C27 0.0252(12) 0.0178(12) 0.0271(13) 0.0020(10) 0.0009(9) -0.0044(9) C28 0.0242(12) 0.0239(13) 0.0244(12) -0.0022(10) -0.0034(9) -0.0048(10) C29 0.0365(14) 0.0303(15) 0.0238(13) -0.0010(11) -0.0060(10) -0.0008(11) C30 0.0446(17) 0.080(3) 0.0271(15) 0.0050(16) -0.0136(13) -0.0090(17) C31 0.0591(19) 0.0306(16) 0.0294(15) -0.0047(12) -0.0001(13) 0.0015(13) C32 0.0641(19) 0.0319(16) 0.0268(15) 0.0007(13) -0.0033(13) 0.0006(14) C33 0.0276(13) 0.0495(18) 0.0344(15) 0.0160(13) 0.0036(11) -0.0032(12) C34A 0.036(3) 0.098(6) 0.035(3) 0.029(3) 0.002(2) 0.000(3) C35A 0.043(3) 0.088(5) 0.039(3) 0.017(3) 0.015(2) 0.019(3) C36A 0.040(3) 0.083(5) 0.054(3) 0.025(3) 0.005(2) -0.025(3) C34B 0.040(4) 0.044(5) 0.047(5) 0.017(4) 0.016(4) -0.006(4) C35B 0.037(4) 0.064(6) 0.036(4) -0.015(4) 0.017(3) -0.010(4) C36B 0.029(4) 0.072(7) 0.030(4) 0.003(4) 0.003(3) -0.005(4) C37 0.0212(12) 0.0405(16) 0.0352(15) 0.0105(13) -0.0061(10) 0.0010(11) C38 0.0235(14) 0.059(2) 0.059(2) 0.0128(17) 0.0031(13) 0.0073(13) C39 0.0463(18) 0.062(2) 0.0483(19) 0.0006(17) -0.0231(15) 0.0128(16) C40 0.0288(14) 0.056(2) 0.0539(19) 0.0245(16) -0.0057(13) 0.0069(14) C41 0.0488(17) 0.0254(14) 0.0383(16) -0.0046(12) 0.0075(13) 0.0010(13) C42 0.073(2) 0.0265(16) 0.0398(17) -0.0043(13) 0.0055(15) 0.0087(15) C43 0.079(2) 0.0359(18) 0.0306(15) -0.0044(14) 0.0160(15) 0.0038(16) C44 0.054(2) 0.049(2) 0.062(2) -0.0162(17) 0.0208(16) 0.0070(16) C45 0.0236(12) 0.0293(14) 0.0276(13) 0.0032(11) 0.0051(10) -0.0008(10) C46 0.0210(11) 0.0316(14) 0.0218(12) -0.0011(10) 0.0041(9) -0.0010(10) C47 0.0247(12) 0.0305(15) 0.0336(14) -0.0063(12) 0.0046(10) -0.0063(11) C48 0.0197(12) 0.0436(17) 0.0331(14) -0.0109(13) 0.0010(10) -0.0037(11) C49 0.0214(12) 0.0396(16) 0.0248(13) -0.0074(11) 0.0005(10) 0.0027(10) C50 0.0199(12) 0.0519(19) 0.0352(15) -0.0078(14) -0.0063(10) 0.0065(12) C51 0.0318(14) 0.0471(19) 0.0482(18) -0.0066(15) -0.0108(12) 0.0160(13) C52 0.0394(16) 0.0331(16) 0.059(2) -0.0077(15) -0.0121(14) 0.0067(13) C53 0.0289(13) 0.0332(16) 0.0443(16) -0.0073(13) -0.0100(12) 0.0017(11) C54 0.0193(11) 0.0342(15) 0.0252(13) -0.0055(11) -0.0012(9) 0.0035(10) C55 0.0140(10) 0.0193(12) 0.0178(11) -0.0030(9) 0.0000(8) -0.0007(8) O5 0.0570(17) 0.0565(19) 0.188(4) 0.004(2) -0.006(2) -0.0190(15) C56 0.061(2) 0.081(3) 0.100(3) -0.029(3) 0.001(2) -0.008(2) C57 0.048(3) 0.106(4) 0.207(6) 0.030(4) 0.006(3) -0.033(3) C58 0.101(3) 0.080(3) 0.043(2) 0.006(2) -0.009(2) -0.029(3) C59 0.102(3) 0.074(3) 0.045(2) 0.002(2) 0.004(2) -0.003(2) O6 0.0314(10) 0.0479(12) 0.0357(11) -0.0034(9) 0.0036(8) 0.0078(9) C60 0.0389(17) 0.055(2) 0.058(2) 0.0021(17) -0.0071(14) 0.0094(15) C61 0.0308(14) 0.0311(16) 0.0517(18) -0.0001(13) 0.0085(12) 0.0034(11) C62 0.0494(17) 0.0469(19) 0.0328(15) -0.0069(14) 0.0016(13) 0.0109(15) C63 0.0474(19) 0.085(3) 0.0447(19) -0.0123(19) -0.0119(15) 0.0179(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C55 2.075(2) . ? Pd1 P1 2.1892(6) . ? Pd1 N1 2.2237(19) . ? Pd1 Cl1 2.3534(6) . ? P1 O1 1.5819(16) . ? P1 O2 1.6049(17) . ? P1 O3 1.6185(16) . ? O1 C1 1.414(3) . ? O2 C8 1.408(3) . ? O3 C15 1.414(3) . ? O4 C22 1.394(3) . ? O4 C45 1.427(3) . ? N1 C46 1.324(3) . ? N1 C54 1.379(3) . ? C1 C6 1.392(3) . ? C1 C2 1.399(3) . ? C2 C3 1.390(3) . ? C2 C28 1.511(3) . ? C3 C4 1.393(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 C29 1.528(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C7 1.513(3) . ? C7 C9 1.513(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.373(3) . ? C8 C13 1.391(3) . ? C9 C10 1.393(3) . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(3) . ? C11 C33 1.531(3) . ? C12 C13 1.390(3) . ? C12 H12 0.9500 . ? C13 C14 1.504(3) . ? C14 C16 1.522(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.408(3) . ? C15 C20 1.409(3) . ? C16 C17 1.402(3) . ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 C19 1.386(3) . ? C18 C37 1.538(3) . ? C19 C20 1.393(3) . ? C19 H19 0.9500 . ? C20 C21 1.514(3) . ? C21 C23 1.505(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.385(3) . ? C22 C23 1.387(3) . ? C23 C24 1.393(3) . ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 C26 1.389(4) . ? C25 C41 1.542(4) . ? C26 C27 1.391(3) . ? C26 H26 0.9500 . ? C27 C28 1.513(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.531(4) . ? C29 C32 1.535(4) . ? C29 C31 1.541(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34A 1.484(4) . ? C33 C36B 1.487(5) . ? C33 C35A 1.512(5) . ? C33 C34B 1.533(5) . ? C33 C36A 1.598(5) . ? C33 C35B 1.606(5) . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37 C39 1.519(4) . ? C37 C38 1.534(4) . ? C37 C40 1.538(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.533(4) . ? C41 C44 1.535(4) . ? C41 C42 1.541(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.503(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.410(3) . ? C47 C48 1.368(4) . ? C47 H47 0.9500 . ? C48 C49 1.401(4) . ? C48 H48 0.9500 . ? C49 C50 1.418(4) . ? C49 C54 1.423(3) . ? C50 C51 1.356(4) . ? C50 H50 0.9500 . ? C51 C52 1.419(4) . ? C51 H51 0.9500 . ? C52 C53 1.365(4) . ? C52 H52 0.9500 . ? C53 C54 1.412(4) . ? C53 H53 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? O5 C58 1.312(5) . ? O5 C57 1.424(5) . ? C56 C57 1.424(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.496(6) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? O6 C62 1.412(3) . ? O6 C61 1.426(3) . ? C60 C61 1.490(4) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.506(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? 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 Pd1 P1 86.08(6) . . ? C55 Pd1 N1 175.80(8) . . ? P1 Pd1 N1 96.88(5) . . ? C55 Pd1 Cl1 88.01(6) . . ? P1 Pd1 Cl1 173.99(2) . . ? N1 Pd1 Cl1 89.08(5) . . ? O1 P1 O2 105.77(9) . . ? O1 P1 O3 103.02(9) . . ? O2 P1 O3 102.38(8) . . ? O1 P1 Pd1 110.97(6) . . ? O2 P1 Pd1 111.63(6) . . ? O3 P1 Pd1 121.62(6) . . ? C1 O1 P1 147.35(14) . . ? C8 O2 P1 121.65(14) . . ? C15 O3 P1 132.23(14) . . ? C22 O4 C45 119.77(18) . . ? C46 N1 C54 117.8(2) . . ? C46 N1 Pd1 123.39(16) . . ? C54 N1 Pd1 118.64(16) . . ? C6 C1 C2 121.4(2) . . ? C6 C1 O1 121.7(2) . . ? C2 C1 O1 116.4(2) . . ? C3 C2 C1 117.4(2) . . ? C3 C2 C28 119.6(2) . . ? C1 C2 C28 123.0(2) . . ? C2 C3 C4 123.5(2) . . ? C2 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C5 C4 C3 116.4(2) . . ? C5 C4 C29 123.5(2) . . ? C3 C4 C29 120.1(2) . . ? C4 C5 C6 123.0(2) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C1 C6 C5 118.1(2) . . ? C1 C6 C7 123.0(2) . . ? C5 C6 C7 118.9(2) . . ? C6 C7 C9 110.38(19) . . ? C6 C7 H7A 109.6 . . ? C9 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? C9 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C13 123.0(2) . . ? C9 C8 O2 119.10(19) . . ? C13 C8 O2 117.8(2) . . ? C8 C9 C10 117.8(2) . . ? C8 C9 C7 120.1(2) . . ? C10 C9 C7 122.1(2) . . ? C11 C10 C9 122.2(2) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C12 117.4(2) . . ? C10 C11 C33 121.6(2) . . ? C12 C11 C33 121.0(2) . . ? C13 C12 C11 122.5(2) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C8 117.2(2) . . ? C12 C13 C14 122.6(2) . . ? C8 C13 C14 120.2(2) . . ? C13 C14 C16 118.0(2) . . ? C13 C14 H14A 107.8 . . ? C16 C14 H14A 107.8 . . ? C13 C14 H14B 107.8 . . ? C16 C14 H14B 107.8 . . ? H14A C14 H14B 107.1 . . ? C16 C15 C20 120.5(2) . . ? C16 C15 O3 120.7(2) . . ? C20 C15 O3 118.4(2) . . ? C17 C16 C15 117.6(2) . . ? C17 C16 C14 116.5(2) . . ? C15 C16 C14 125.8(2) . . ? C18 C17 C16 123.8(2) . . ? C18 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? C19 C18 C17 116.3(2) . . ? C19 C18 C37 122.3(2) . . ? C17 C18 C37 121.4(2) . . ? C18 C19 C20 123.5(2) . . ? C18 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C19 C20 C15 118.2(2) . . ? C19 C20 C21 115.8(2) . . ? C15 C20 C21 125.9(2) . . ? C23 C21 C20 115.5(2) . . ? C23 C21 H21A 108.4 . . ? C20 C21 H21A 108.4 . . ? C23 C21 H21B 108.4 . . ? C20 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C27 C22 C23 121.1(2) . . ? C27 C22 O4 121.2(2) . . ? C23 C22 O4 117.1(2) . . ? C22 C23 C24 118.8(2) . . ? C22 C23 C21 118.5(2) . . ? C24 C23 C21 122.6(2) . . ? C23 C24 C25 121.8(2) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C26 C25 C24 117.3(2) . . ? C26 C25 C41 122.0(2) . . ? C24 C25 C41 120.6(2) . . ? C25 C26 C27 122.4(2) . . ? C25 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? C22 C27 C26 118.4(2) . . ? C22 C27 C28 121.3(2) . . ? C26 C27 C28 120.0(2) . . ? C2 C28 C27 111.24(19) . . ? C2 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C2 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C4 C29 C30 110.3(2) . . ? C4 C29 C32 111.6(2) . . ? C30 C29 C32 108.9(2) . . ? C4 C29 C31 108.8(2) . . ? C30 C29 C31 109.8(2) . . ? C32 C29 C31 107.4(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34A C33 C35A 113.4(3) . . ? C34A C33 C11 114.0(2) . . ? C36B C33 C11 115.8(3) . . ? C35A C33 C11 110.2(3) . . ? C36B C33 C34B 111.6(4) . . ? C11 C33 C34B 111.0(3) . . ? C34A C33 C36A 106.9(3) . . ? C35A C33 C36A 106.3(3) . . ? C11 C33 C36A 105.4(2) . . ? C36B C33 C35B 106.2(4) . . ? C11 C33 C35B 107.6(3) . . ? C34B C33 C35B 103.8(4) . . ? C36A C33 C35B 146.4(4) . . ? C33 C34A H34A 109.5 . . ? C33 C34A H34B 109.5 . . ? C33 C34A H34C 109.5 . . ? C33 C35A H35A 109.5 . . ? C33 C35A H35B 109.5 . . ? C33 C35A H35C 109.5 . . ? C33 C36A H36A 109.5 . . ? C33 C36A H36B 109.5 . . ? C33 C36A H36C 109.5 . . ? C33 C34B H34D 109.5 . . ? C33 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C33 C35B H35D 109.5 . . ? C33 C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C33 C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C33 C36B H36D 109.5 . . ? C33 C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C33 C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C39 C37 C38 109.9(2) . . ? C39 C37 C18 110.0(2) . . ? C38 C37 C18 108.5(2) . . ? C39 C37 C40 108.9(2) . . ? C38 C37 C40 107.3(2) . . ? C18 C37 C40 112.2(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44 108.3(3) . . ? C43 C41 C42 108.2(2) . . ? C44 C41 C42 110.0(3) . . ? C43 C41 C25 112.1(2) . . ? C44 C41 C25 110.1(2) . . ? C42 C41 C25 108.1(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O4 C45 C46 108.86(19) . . ? O4 C45 H45A 109.9 . . ? C46 C45 H45A 109.9 . . ? O4 C45 H45B 109.9 . . ? C46 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? N1 C46 C47 123.3(2) . . ? N1 C46 C45 117.7(2) . . ? C47 C46 C45 119.0(2) . . ? C48 C47 C46 119.6(2) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C49 119.1(2) . . ? C47 C48 H48 120.5 . . ? C49 C48 H48 120.5 . . ? C48 C49 C50 122.6(2) . . ? C48 C49 C54 118.3(2) . . ? C50 C49 C54 119.0(2) . . ? C51 C50 C49 120.8(2) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C50 C51 C52 120.1(3) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C53 C52 C51 120.5(3) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C54 120.6(2) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? N1 C54 C53 119.3(2) . . ? N1 C54 C49 121.8(2) . . ? C53 C54 C49 118.9(2) . . ? Pd1 C55 H55A 109.5 . . ? Pd1 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Pd1 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C58 O5 C57 113.0(4) . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O5 C57 C56 112.9(4) . . ? O5 C57 H57A 109.0 . . ? C56 C57 H57A 109.0 . . ? O5 C57 H57B 109.0 . . ? C56 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? O5 C58 C59 111.7(4) . . ? O5 C58 H58A 109.3 . . ? C59 C58 H58A 109.3 . . ? O5 C58 H58B 109.3 . . ? C59 C58 H58B 109.3 . . ? H58A C58 H58B 108.0 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C62 O6 C61 111.6(2) . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O6 C61 C60 108.1(2) . . ? O6 C61 H61A 110.1 . . ? C60 C61 H61A 110.1 . . ? O6 C61 H61B 110.1 . . ? C60 C61 H61B 110.1 . . ? H61A C61 H61B 108.4 . . ? O6 C62 C63 108.1(2) . . ? O6 C62 H62A 110.1 . . ? C63 C62 H62A 110.1 . . ? O6 C62 H62B 110.1 . . ? C63 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C55 Pd1 P1 O1 -166.87(9) . . . . ? N1 Pd1 P1 O1 10.14(9) . . . . ? C55 Pd1 P1 O2 -49.15(9) . . . . ? N1 Pd1 P1 O2 127.86(8) . . . . ? C55 Pd1 P1 O3 71.84(10) . . . . ? N1 Pd1 P1 O3 -111.15(9) . . . . ? O2 P1 O1 C1 47.2(3) . . . . ? O3 P1 O1 C1 -59.9(3) . . . . ? Pd1 P1 O1 C1 168.5(3) . . . . ? O1 P1 O2 C8 -68.74(17) . . . . ? O3 P1 O2 C8 38.81(17) . . . . ? Pd1 P1 O2 C8 170.45(14) . . . . ? O1 P1 O3 C15 -173.75(19) . . . . ? O2 P1 O3 C15 76.6(2) . . . . ? Pd1 P1 O3 C15 -48.7(2) . . . . ? P1 Pd1 N1 C46 84.70(18) . . . . ? Cl1 Pd1 N1 C46 -94.51(18) . . . . ? P1 Pd1 N1 C54 -99.90(17) . . . . ? Cl1 Pd1 N1 C54 80.88(17) . . . . ? P1 O1 C1 C6 -55.0(4) . . . . ? P1 O1 C1 C2 133.8(3) . . . . ? C6 C1 C2 C3 6.4(3) . . . . ? O1 C1 C2 C3 177.68(19) . . . . ? C6 C1 C2 C28 -172.4(2) . . . . ? O1 C1 C2 C28 -1.1(3) . . . . ? C1 C2 C3 C4 -2.7(4) . . . . ? C28 C2 C3 C4 176.2(2) . . . . ? C2 C3 C4 C5 -1.9(4) . . . . ? C2 C3 C4 C29 178.7(2) . . . . ? C3 C4 C5 C6 3.0(4) . . . . ? C29 C4 C5 C6 -177.6(2) . . . . ? C2 C1 C6 C5 -5.4(3) . . . . ? O1 C1 C6 C5 -176.24(19) . . . . ? C2 C1 C6 C7 174.2(2) . . . . ? O1 C1 C6 C7 3.3(3) . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? C4 C5 C6 C7 -179.0(2) . . . . ? C1 C6 C7 C9 77.6(3) . . . . ? C5 C6 C7 C9 -102.9(2) . . . . ? P1 O2 C8 C9 92.6(2) . . . . ? P1 O2 C8 C13 -90.4(2) . . . . ? C13 C8 C9 C10 0.1(4) . . . . ? O2 C8 C9 C10 177.0(2) . . . . ? C13 C8 C9 C7 176.8(2) . . . . ? O2 C8 C9 C7 -6.4(3) . . . . ? C6 C7 C9 C8 -92.0(3) . . . . ? C6 C7 C9 C10 84.5(3) . . . . ? C8 C9 C10 C11 -0.7(4) . . . . ? C7 C9 C10 C11 -177.3(2) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C9 C10 C11 C33 -177.7(2) . . . . ? C10 C11 C12 C13 0.2(4) . . . . ? C33 C11 C12 C13 178.4(2) . . . . ? C11 C12 C13 C8 -0.7(4) . . . . ? C11 C12 C13 C14 -177.1(2) . . . . ? C9 C8 C13 C12 0.6(4) . . . . ? O2 C8 C13 C12 -176.4(2) . . . . ? C9 C8 C13 C14 177.1(2) . . . . ? O2 C8 C13 C14 0.2(3) . . . . ? C12 C13 C14 C16 -96.1(3) . . . . ? C8 C13 C14 C16 87.6(3) . . . . ? P1 O3 C15 C16 -71.4(3) . . . . ? P1 O3 C15 C20 115.2(2) . . . . ? C20 C15 C16 C17 1.8(3) . . . . ? O3 C15 C16 C17 -171.4(2) . . . . ? C20 C15 C16 C14 -173.7(2) . . . . ? O3 C15 C16 C14 13.1(3) . . . . ? C13 C14 C16 C17 131.6(2) . . . . ? C13 C14 C16 C15 -52.8(3) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C14 C16 C17 C18 175.7(2) . . . . ? C16 C17 C18 C19 -1.1(4) . . . . ? C16 C17 C18 C37 177.9(2) . . . . ? C17 C18 C19 C20 0.9(4) . . . . ? C37 C18 C19 C20 -178.1(2) . . . . ? C18 C19 C20 C15 0.6(4) . . . . ? C18 C19 C20 C21 -176.8(2) . . . . ? C16 C15 C20 C19 -2.0(3) . . . . ? O3 C15 C20 C19 171.4(2) . . . . ? C16 C15 C20 C21 175.1(2) . . . . ? O3 C15 C20 C21 -11.5(3) . . . . ? C19 C20 C21 C23 -128.6(2) . . . . ? C15 C20 C21 C23 54.3(3) . . . . ? C45 O4 C22 C27 83.9(3) . . . . ? C45 O4 C22 C23 -104.9(2) . . . . ? C27 C22 C23 C24 -4.8(3) . . . . ? O4 C22 C23 C24 -176.0(2) . . . . ? C27 C22 C23 C21 171.8(2) . . . . ? O4 C22 C23 C21 0.6(3) . . . . ? C20 C21 C23 C22 -99.4(3) . . . . ? C20 C21 C23 C24 77.0(3) . . . . ? C22 C23 C24 C25 1.9(4) . . . . ? C21 C23 C24 C25 -174.5(2) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? C23 C24 C25 C41 -178.3(2) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C41 C25 C26 C27 178.6(2) . . . . ? C23 C22 C27 C26 5.0(3) . . . . ? O4 C22 C27 C26 175.9(2) . . . . ? C23 C22 C27 C28 -168.3(2) . . . . ? O4 C22 C27 C28 2.5(3) . . . . ? C25 C26 C27 C22 -2.5(4) . . . . ? C25 C26 C27 C28 171.0(2) . . . . ? C3 C2 C28 C27 104.4(2) . . . . ? C1 C2 C28 C27 -76.9(3) . . . . ? C22 C27 C28 C2 102.3(3) . . . . ? C26 C27 C28 C2 -71.0(3) . . . . ? C5 C4 C29 C30 -124.1(3) . . . . ? C3 C4 C29 C30 55.2(3) . . . . ? C5 C4 C29 C32 -3.0(3) . . . . ? C3 C4 C29 C32 176.4(2) . . . . ? C5 C4 C29 C31 115.4(3) . . . . ? C3 C4 C29 C31 -65.3(3) . . . . ? C10 C11 C33 C34A -1.1(4) . . . . ? C12 C11 C33 C34A -179.3(3) . . . . ? C10 C11 C33 C36B -176.2(4) . . . . ? C12 C11 C33 C36B 5.6(5) . . . . ? C10 C11 C33 C35A -130.0(3) . . . . ? C12 C11 C33 C35A 51.8(4) . . . . ? C10 C11 C33 C34B 55.2(4) . . . . ? C12 C11 C33 C34B -123.0(4) . . . . ? C10 C11 C33 C36A 115.8(3) . . . . ? C12 C11 C33 C36A -62.4(3) . . . . ? C10 C11 C33 C35B -57.7(4) . . . . ? C12 C11 C33 C35B 124.1(4) . . . . ? C19 C18 C37 C39 -130.3(3) . . . . ? C17 C18 C37 C39 50.7(3) . . . . ? C19 C18 C37 C38 109.5(3) . . . . ? C17 C18 C37 C38 -69.5(3) . . . . ? C19 C18 C37 C40 -8.9(4) . . . . ? C17 C18 C37 C40 172.1(2) . . . . ? C26 C25 C41 C43 15.0(4) . . . . ? C24 C25 C41 C43 -166.2(2) . . . . ? C26 C25 C41 C44 135.7(3) . . . . ? C24 C25 C41 C44 -45.5(3) . . . . ? C26 C25 C41 C42 -104.2(3) . . . . ? C24 C25 C41 C42 74.6(3) . . . . ? C22 O4 C45 C46 -122.2(2) . . . . ? C54 N1 C46 C47 -3.2(3) . . . . ? Pd1 N1 C46 C47 172.27(18) . . . . ? C54 N1 C46 C45 174.6(2) . . . . ? Pd1 N1 C46 C45 -10.0(3) . . . . ? O4 C45 C46 N1 -49.4(3) . . . . ? O4 C45 C46 C47 128.5(2) . . . . ? N1 C46 C47 C48 1.0(4) . . . . ? C45 C46 C47 C48 -176.7(2) . . . . ? C46 C47 C48 C49 1.4(4) . . . . ? C47 C48 C49 C50 177.4(2) . . . . ? C47 C48 C49 C54 -1.5(4) . . . . ? C48 C49 C50 C51 -178.4(3) . . . . ? C54 C49 C50 C51 0.5(4) . . . . ? C49 C50 C51 C52 -0.3(5) . . . . ? C50 C51 C52 C53 -0.1(5) . . . . ? C51 C52 C53 C54 0.3(5) . . . . ? C46 N1 C54 C53 -176.4(2) . . . . ? Pd1 N1 C54 C53 8.0(3) . . . . ? C46 N1 C54 C49 3.0(3) . . . . ? Pd1 N1 C54 C49 -172.70(18) . . . . ? C52 C53 C54 N1 179.2(3) . . . . ? C52 C53 C54 C49 -0.1(4) . . . . ? C48 C49 C54 N1 -0.7(4) . . . . ? C50 C49 C54 N1 -179.6(2) . . . . ? C48 C49 C54 C53 178.7(2) . . . . ? C50 C49 C54 C53 -0.3(4) . . . . ? C58 O5 C57 C56 -169.0(5) . . . . ? C57 O5 C58 C59 170.6(4) . . . . ? C62 O6 C61 C60 -179.8(3) . . . . ? C61 O6 C62 C63 179.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.249 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.069 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 1.000 368.7 48.7 2 0.500 0.500 0.500 368.7 48.5 _platon_squeeze_details ; ? ; #===END data_s3346a _database_code_depnum_ccdc_archive 'CCDC 699255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H120 Cl2 N2 O8 P2 Pt, 5(C2 H3 N)' _chemical_formula_sum 'C118 H135 Cl2 N7 O8 P2 Pt' _chemical_formula_weight 2107.26 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' 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 0.0060 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.7427(6) _cell_length_b 20.2761(8) _cell_length_c 22.7693(10) _cell_angle_alpha 67.813(2) _cell_angle_beta 83.508(2) _cell_angle_gamma 75.3620(10) _cell_volume 6923.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2196 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61712 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.50 _reflns_number_total 22534 _reflns_number_gt 18863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction EvalCCD _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0304P)^2^+130.1771P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22534 _refine_ls_number_parameters 661 _refine_ls_number_restraints 1008 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2063 _refine_ls_wR_factor_gt 0.1987 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.099355(18) 0.181550(17) 0.320866(14) 0.01561(10) Uani 1 1 d . . . Cl1 Cl -0.01269(12) 0.14630(12) 0.29825(10) 0.0257(5) Uani 1 1 d . . . Cl2 Cl 0.05665(13) 0.14006(12) 0.42753(9) 0.0257(4) Uani 1 1 d . . . P1 P 0.13716(12) 0.20848(12) 0.21986(9) 0.0192(4) Uani 1 1 d . . . O11 O 0.1169(3) 0.1639(3) 0.1819(3) 0.0231(13) Uani 1 1 d . . . O12 O 0.0932(3) 0.2918(3) 0.1818(3) 0.0238(13) Uani 1 1 d . . . O13 O 0.2327(3) 0.2014(3) 0.2087(2) 0.0170(11) Uani 1 1 d . . . O14 O 0.2259(3) 0.0542(4) 0.2777(3) 0.0265(14) Uani 1 1 d . . . N1 N 0.2694(4) -0.1237(4) 0.3828(3) 0.0239(15) Uiso 1 1 d . . . C11 C 0.0499(6) 0.1436(5) 0.1648(4) 0.0278(19) Uiso 1 1 d . . . C12 C 0.0561(6) 0.0701(5) 0.1777(4) 0.032(2) Uiso 1 1 d . . . C13 C -0.0001(7) 0.0492(6) 0.1513(5) 0.043(3) Uiso 1 1 d . . . H11 H 0.0058 -0.0014 0.1598 0.052 Uiso 1 1 calc R . . C14 C -0.0629(6) 0.0981(6) 0.1139(5) 0.050(3) Uiso 1 1 d D A . C15 C -0.0736(7) 0.1732(6) 0.1067(5) 0.044(3) Uiso 1 1 d . . . H12 H -0.1199 0.2082 0.0843 0.053 Uiso 1 1 calc R . . C16 C -0.0184(6) 0.1966(5) 0.1315(5) 0.032(2) Uiso 1 1 d . . . C17 C -0.0376(6) 0.2762(5) 0.1243(5) 0.034(2) Uiso 1 1 d . . . H13 H -0.0921 0.3007 0.1043 0.041 Uiso 1 1 calc R . . H14 H -0.0419 0.2792 0.1670 0.041 Uiso 1 1 calc R . . C18 C 0.0909(5) 0.3214(5) 0.1147(4) 0.0254(18) Uiso 1 1 d . . . C19 C 0.0254(6) 0.3172(5) 0.0855(5) 0.034(2) Uiso 1 1 d . . . C110 C 0.0217(7) 0.3499(6) 0.0193(5) 0.041(2) Uiso 1 1 d . . . H15 H -0.0223 0.3469 -0.0018 0.049 Uiso 1 1 calc R . . C111 C 0.0809(6) 0.3867(5) -0.0162(4) 0.041(2) Uiso 1 1 d D . . C112 C 0.1468(6) 0.3896(5) 0.0158(4) 0.031(2) Uiso 1 1 d . . . H16 H 0.1879 0.4143 -0.0080 0.037 Uiso 1 1 calc R . . C113 C 0.1527(6) 0.3565(5) 0.0825(4) 0.029(2) Uiso 1 1 d . . . C114 C 0.2235(5) 0.3555(4) 0.1171(4) 0.0211(17) Uiso 1 1 d . . . H17 H 0.2049 0.3533 0.1605 0.025 Uiso 1 1 calc R . . H18 H 0.2425 0.4014 0.0951 0.025 Uiso 1 1 calc R . . C115 C 0.2969(5) 0.2190(4) 0.1633(4) 0.0150(15) Uiso 1 1 d . . . C116 C 0.2949(5) 0.2910(4) 0.1212(4) 0.0169(16) Uiso 1 1 d . . . C117 C 0.3637(5) 0.3041(4) 0.0818(4) 0.0205(17) Uiso 1 1 d . . . H19 H 0.3618 0.3523 0.0521 0.025 Uiso 1 1 calc R . . C118 C 0.4347(6) 0.2504(5) 0.0836(4) 0.0280(19) Uiso 1 1 d . . . C119 C 0.4354(5) 0.1799(5) 0.1291(4) 0.0222(17) Uiso 1 1 d . . . H110 H 0.4837 0.1422 0.1323 0.027 Uiso 1 1 calc R . . C120 C 0.3687(5) 0.1631(4) 0.1693(4) 0.0208(17) Uiso 1 1 d . . . C121 C 0.3772(5) 0.0873(4) 0.2196(4) 0.0195(16) Uiso 1 1 d . . . H111 H 0.3542 0.0909 0.2606 0.023 Uiso 1 1 calc R . . H112 H 0.4363 0.0621 0.2253 0.023 Uiso 1 1 calc R . . C122 C 0.2553(5) 0.0364(4) 0.2205(4) 0.0195(17) Uiso 1 1 d . . . C123 C 0.3311(5) 0.0434(4) 0.1996(4) 0.0208(17) Uiso 1 1 d . . . C124 C 0.3612(5) 0.0197(4) 0.1494(4) 0.0228(18) Uiso 1 1 d . . . H113 H 0.4141 0.0259 0.1314 0.027 Uiso 1 1 calc R . . C125 C 0.3162(6) -0.0124(5) 0.1249(5) 0.034(2) Uiso 1 1 d . . . C126 C 0.2358(6) -0.0167(5) 0.1501(4) 0.032(2) Uiso 1 1 d . . . H114 H 0.2023 -0.0356 0.1323 0.039 Uiso 1 1 calc R . . C127 C 0.2041(5) 0.0059(5) 0.2005(4) 0.0257(19) Uiso 1 1 d . . . C128 C 0.1171(6) 0.0098(5) 0.2229(5) 0.033(2) Uiso 1 1 d . . . H115 H 0.1113 0.0168 0.2640 0.039 Uiso 1 1 calc R . . H116 H 0.1035 -0.0375 0.2303 0.039 Uiso 1 1 calc R . . C129 C -0.1239(6) 0.0778(5) 0.0803(5) 0.075(4) Uiso 1 1 d D . . C13A C -0.1060(12) 0.1078(11) 0.0087(5) 0.012(8) Uiso 0.34(4) 1 d PD A 5 H17A H -0.1381 0.0896 -0.0129 0.019 Uiso 0.34(4) 1 calc PR A 5 H17B H -0.0470 0.0915 0.0004 0.019 Uiso 0.34(4) 1 calc PR A 5 H17C H -0.1215 0.1614 -0.0073 0.019 Uiso 0.34(4) 1 calc PR A 5 C13B C -0.1109(16) -0.0048(6) 0.1034(10) 0.048(10) Uiso 0.34(4) 1 d PD A 5 H18D H -0.1012 -0.0258 0.1491 0.072 Uiso 0.34(4) 1 calc PR A 5 H18E H -0.0630 -0.0246 0.0812 0.072 Uiso 0.34(4) 1 calc PR A 5 H18F H -0.1601 -0.0173 0.0948 0.072 Uiso 0.34(4) 1 calc PR A 5 C13C C -0.2119(6) 0.1123(16) 0.0941(12) 0.14(3) Uiso 0.34(4) 1 d PD A 5 H19G H -0.2369 0.0751 0.1266 0.215 Uiso 0.34(4) 1 calc PR A 5 H19H H -0.2438 0.1329 0.0552 0.215 Uiso 0.34(4) 1 calc PR A 5 H19I H -0.2117 0.1514 0.1095 0.215 Uiso 0.34(4) 1 calc PR A 5 C13D C -0.1323(19) 0.1294(13) 0.0115(7) 0.30(4) Uiso 0.66(4) 1 d PD A 6 H17J H -0.1257 0.1009 -0.0160 0.446 Uiso 0.66(4) 1 calc PR A 6 H17K H -0.0897 0.1577 0.0007 0.446 Uiso 0.66(4) 1 calc PR A 6 H17L H -0.1870 0.1628 0.0055 0.446 Uiso 0.66(4) 1 calc PR A 6 C13E C -0.0924(12) -0.0010(7) 0.0844(12) 0.069(7) Uiso 0.66(4) 1 d PD A 6 H18M H -0.0726 -0.0318 0.1273 0.103 Uiso 0.66(4) 1 calc PR A 6 H18N H -0.0470 -0.0037 0.0536 0.103 Uiso 0.66(4) 1 calc PR A 6 H18O H -0.1373 -0.0183 0.0750 0.103 Uiso 0.66(4) 1 calc PR A 6 C13F C -0.2079(7) 0.0857(17) 0.1143(13) 0.104(11) Uiso 0.66(4) 1 d PD A 6 H19P H -0.2009 0.0589 0.1600 0.156 Uiso 0.66(4) 1 calc PR A 6 H19Q H -0.2446 0.0658 0.0983 0.156 Uiso 0.66(4) 1 calc PR A 6 H19R H -0.2321 0.1376 0.1064 0.156 Uiso 0.66(4) 1 calc PR A 6 C133 C 0.0777(5) 0.4270(5) -0.0889(5) 0.055(3) Uiso 1 1 d D . . C134 C 0.0021(6) 0.4191(6) -0.1151(5) 0.061(3) Uiso 1 1 d D . . H120 H -0.0479 0.4386 -0.0946 0.092 Uiso 1 1 calc R . . H121 H 0.0059 0.3673 -0.1066 0.092 Uiso 1 1 calc R . . H122 H -0.0001 0.4464 -0.1610 0.092 Uiso 1 1 calc R . . C135 C 0.0725(7) 0.5080(4) -0.1042(5) 0.070(4) Uiso 1 1 d D . . H123 H 0.0712 0.5338 -0.1503 0.105 Uiso 1 1 calc R . . H124 H 0.1207 0.5135 -0.0873 0.105 Uiso 1 1 calc R . . H125 H 0.0221 0.5287 -0.0848 0.105 Uiso 1 1 calc R . . C136 C 0.1555(6) 0.3949(6) -0.1197(5) 0.075(4) Uiso 1 1 d D . . H126 H 0.1521 0.4188 -0.1659 0.113 Uiso 1 1 calc R . . H127 H 0.1604 0.3422 -0.1079 0.113 Uiso 1 1 calc R . . H128 H 0.2039 0.4028 -0.1052 0.113 Uiso 1 1 calc R . . C137 C 0.5117(6) 0.2653(5) 0.0440(4) 0.043(3) Uiso 1 1 d D . . C138 C 0.5022(9) 0.3449(5) 0.0013(6) 0.072(4) Uiso 1 1 d D . . H129 H 0.4546 0.3600 -0.0259 0.108 Uiso 1 1 calc R . . H130 H 0.5522 0.3511 -0.0250 0.108 Uiso 1 1 calc R . . H131 H 0.4936 0.3752 0.0274 0.108 Uiso 1 1 calc R . . C139 C 0.5828(9) 0.2452(8) 0.0888(6) 0.088(5) Uiso 1 1 d D . . H132 H 0.5650 0.2675 0.1209 0.131 Uiso 1 1 calc R . . H133 H 0.6300 0.2634 0.0644 0.131 Uiso 1 1 calc R . . H134 H 0.5990 0.1919 0.1096 0.131 Uiso 1 1 calc R . . C140 C 0.5325(10) 0.2163(7) 0.0052(7) 0.088(5) Uiso 1 1 d D . . H135 H 0.5434 0.1649 0.0338 0.131 Uiso 1 1 calc R . . H136 H 0.5816 0.2259 -0.0214 0.131 Uiso 1 1 calc R . . H137 H 0.4859 0.2264 -0.0218 0.131 Uiso 1 1 calc R . . C141 C 0.3562(6) -0.0399(5) 0.0714(5) 0.047(3) Uiso 1 1 d D . . C142 C 0.2997(8) -0.0736(8) 0.0494(8) 0.088(5) Uiso 1 1 d D . . H138 H 0.2519 -0.0355 0.0284 0.133 Uiso 1 1 calc R . . H139 H 0.2809 -0.1112 0.0861 0.133 Uiso 1 1 calc R . . H140 H 0.3299 -0.0958 0.0196 0.133 Uiso 1 1 calc R . . C143 C 0.4355(7) -0.0993(6) 0.0939(7) 0.073(4) Uiso 1 1 d D . . H141 H 0.4228 -0.1398 0.1312 0.109 Uiso 1 1 calc R . . H142 H 0.4759 -0.0786 0.1051 0.109 Uiso 1 1 calc R . . H143 H 0.4585 -0.1174 0.0599 0.109 Uiso 1 1 calc R . . C144 C 0.3824(9) 0.0220(6) 0.0156(6) 0.075(4) Uiso 1 1 d D . . H144 H 0.4092 0.0033 -0.0173 0.112 Uiso 1 1 calc R . . H145 H 0.4211 0.0415 0.0300 0.112 Uiso 1 1 calc R . . H146 H 0.3336 0.0610 -0.0019 0.112 Uiso 1 1 calc R . . C145 C 0.2650(5) 0.0057(4) 0.3379(4) 0.0205(17) Uiso 1 1 d . . . H147 H 0.2624 0.0340 0.3655 0.025 Uiso 1 1 calc R . . H148 H 0.3240 -0.0138 0.3298 0.025 Uiso 1 1 calc R . . C146 C 0.2240(5) -0.0576(4) 0.3721(4) 0.0203(17) Uiso 1 1 d . . . C147 C 0.1407(5) -0.0434(5) 0.3953(4) 0.0245(18) Uiso 1 1 d . . . H149 H 0.1097 0.0055 0.3861 0.029 Uiso 1 1 calc R . . C148 C 0.1064(6) -0.1005(5) 0.4306(4) 0.0283(19) Uiso 1 1 d . . . H150 H 0.0505 -0.0921 0.4449 0.034 Uiso 1 1 calc R . . C149 C 0.1551(5) -0.1730(5) 0.4458(4) 0.0263(19) Uiso 1 1 d . . . C150 C 0.1253(7) -0.2337(6) 0.4850(5) 0.043(3) Uiso 1 1 d . . . H151 H 0.0704 -0.2276 0.5017 0.052 Uiso 1 1 calc R . . C151 C 0.1765(7) -0.3032(7) 0.4996(6) 0.051(3) Uiso 1 1 d . . . H152 H 0.1577 -0.3446 0.5283 0.062 Uiso 1 1 calc R . . C152 C 0.2548(7) -0.3126(7) 0.4724(5) 0.047(3) Uiso 1 1 d . . . H153 H 0.2878 -0.3606 0.4806 0.057 Uiso 1 1 calc R . . C153 C 0.2856(6) -0.2538(6) 0.4338(5) 0.038(2) Uiso 1 1 d . . . H154 H 0.3399 -0.2613 0.4163 0.045 Uiso 1 1 calc R . . C154 C 0.2365(5) -0.1816(5) 0.4200(4) 0.0247(18) Uiso 1 1 d . . . P2 P 0.19826(12) 0.22028(11) 0.34620(9) 0.0152(4) Uani 1 1 d . . . O21 O 0.1853(3) 0.2470(3) 0.4049(2) 0.0157(11) Uani 1 1 d . . . O22 O 0.2799(3) 0.1558(3) 0.3618(2) 0.0187(11) Uani 1 1 d . . . O23 O 0.2215(3) 0.2877(3) 0.2899(3) 0.0197(12) Uani 1 1 d . . . O24 O 0.0552(3) 0.3504(3) 0.3208(3) 0.0208(12) Uani 1 1 d . . . N2 N -0.1374(5) 0.4484(4) 0.3071(4) 0.0298(17) Uiso 1 1 d . . . C21 C 0.1643(5) 0.2178(4) 0.4708(4) 0.0212(17) Uiso 1 1 d . . . C22 C 0.0958(5) 0.2607(5) 0.4913(4) 0.0228(18) Uiso 1 1 d . . . C23 C 0.0766(6) 0.2378(5) 0.5565(5) 0.034(2) Uiso 1 1 d . . . H21 H 0.0304 0.2663 0.5711 0.041 Uiso 1 1 calc R . . C24 C 0.1225(6) 0.1752(5) 0.6008(4) 0.041(2) Uiso 1 1 d D B . C25 C 0.1869(6) 0.1326(5) 0.5766(4) 0.030(2) Uiso 1 1 d . . . H22 H 0.2171 0.0876 0.6052 0.036 Uiso 1 1 calc R . . C26 C 0.2083(5) 0.1537(5) 0.5122(4) 0.0243(18) Uiso 1 1 d . . . C27 C 0.2760(5) 0.0987(4) 0.4940(4) 0.0208(17) Uiso 1 1 d . . . H23 H 0.2967 0.0572 0.5332 0.025 Uiso 1 1 calc R . . H24 H 0.2516 0.0793 0.4680 0.025 Uiso 1 1 calc R . . C28 C 0.3481(4) 0.1574(4) 0.3921(3) 0.0141(15) Uiso 1 1 d . . . C29 C 0.3482(5) 0.1281(4) 0.4575(4) 0.0178(16) Uiso 1 1 d . . . C210 C 0.4175(5) 0.1274(4) 0.4872(4) 0.0219(17) Uiso 1 1 d . . . H25 H 0.4193 0.1077 0.5322 0.026 Uiso 1 1 calc R . . C211 C 0.4846(5) 0.1548(4) 0.4523(4) 0.0208(17) Uiso 1 1 d . . . C212 C 0.4795(5) 0.1838(4) 0.3867(4) 0.0184(16) Uiso 1 1 d . . . H26 H 0.5236 0.2035 0.3621 0.022 Uiso 1 1 calc R . . C213 C 0.4118(5) 0.1850(4) 0.3555(4) 0.0176(16) Uiso 1 1 d . . . C214 C 0.4032(5) 0.2201(4) 0.2848(4) 0.0177(16) Uiso 1 1 d . . . H27 H 0.3683 0.1963 0.2706 0.021 Uiso 1 1 calc R . . H28 H 0.4583 0.2124 0.2642 0.021 Uiso 1 1 calc R . . C215 C 0.2807(5) 0.3314(4) 0.2671(4) 0.0162(16) Uiso 1 1 d . . . C216 C 0.3653(5) 0.3008(4) 0.2641(4) 0.0175(16) Uiso 1 1 d . . . C217 C 0.4184(5) 0.3483(4) 0.2396(4) 0.0205(17) Uiso 1 1 d . . . H29 H 0.4760 0.3281 0.2381 0.025 Uiso 1 1 calc R . . C218 C 0.3907(5) 0.4240(5) 0.2171(4) 0.0248(18) Uiso 1 1 d . . . C219 C 0.3058(5) 0.4508(5) 0.2169(4) 0.0243(18) Uiso 1 1 d . . . H210 H 0.2850 0.5023 0.1996 0.029 Uiso 1 1 calc R . . C220 C 0.2502(5) 0.4068(4) 0.2403(4) 0.0200(17) Uiso 1 1 d . . . C221 C 0.1588(5) 0.4416(5) 0.2372(4) 0.0252(18) Uiso 1 1 d . . . H211 H 0.1487 0.4913 0.2042 0.030 Uiso 1 1 calc R . . H212 H 0.1285 0.4121 0.2259 0.030 Uiso 1 1 calc R . . C222 C 0.0822(5) 0.3972(4) 0.3411(4) 0.0201(17) Uiso 1 1 d . . . C223 C 0.1283(5) 0.4459(5) 0.3009(4) 0.0249(18) Uiso 1 1 d . . . C224 C 0.1534(6) 0.4924(5) 0.3233(4) 0.028(2) Uiso 1 1 d . . . H213 H 0.1804 0.5285 0.2948 0.034 Uiso 1 1 calc R . . C225 C 0.1405(5) 0.4877(4) 0.3858(4) 0.029(2) Uiso 1 1 d D C . C226 C 0.0997(5) 0.4336(5) 0.4270(4) 0.0259(19) Uiso 1 1 d . . . H214 H 0.0907 0.4288 0.4703 0.031 Uiso 1 1 calc R . . C227 C 0.0725(5) 0.3873(4) 0.4058(4) 0.0206(17) Uiso 1 1 d . . . C228 C 0.0351(5) 0.3259(4) 0.4493(4) 0.0209(17) Uiso 1 1 d . . . H215 H 0.0068 0.3094 0.4233 0.025 Uiso 1 1 calc R . . H216 H -0.0073 0.3449 0.4765 0.025 Uiso 1 1 calc R . . C229 C 0.1009(5) 0.1490(5) 0.6723(5) 0.055(3) Uiso 1 1 d D . . C23A C 0.0574(10) 0.0872(7) 0.6906(7) 0.073(7) Uiso 0.68(2) 1 d PD B 1 H27A H 0.0935 0.0462 0.6808 0.110 Uiso 0.68(2) 1 calc PR B 1 H27B H 0.0064 0.1040 0.6666 0.110 Uiso 0.68(2) 1 calc PR B 1 H27C H 0.0440 0.0712 0.7361 0.110 Uiso 0.68(2) 1 calc PR B 1 C23B C 0.1818(7) 0.1218(9) 0.7096(6) 0.066(6) Uiso 0.68(2) 1 d PD B 1 H28D H 0.2139 0.1595 0.6938 0.098 Uiso 0.68(2) 1 calc PR B 1 H28E H 0.2141 0.0770 0.7038 0.098 Uiso 0.68(2) 1 calc PR B 1 H28F H 0.1686 0.1115 0.7548 0.098 Uiso 0.68(2) 1 calc PR B 1 C23C C 0.0484(10) 0.2129(7) 0.6894(7) 0.084(8) Uiso 0.68(2) 1 d PD B 1 H29G H 0.0333 0.1955 0.7347 0.126 Uiso 0.68(2) 1 calc PR B 1 H29H H -0.0017 0.2340 0.6642 0.126 Uiso 0.68(2) 1 calc PR B 1 H29I H 0.0801 0.2504 0.6804 0.126 Uiso 0.68(2) 1 calc PR B 1 C23D C 0.1171(18) 0.0653(6) 0.6991(9) 0.14(3) Uiso 0.32(2) 1 d PD B 2 H27J H 0.1202 0.0476 0.7455 0.206 Uiso 0.32(2) 1 calc PR B 2 H27K H 0.1695 0.0449 0.6816 0.206 Uiso 0.32(2) 1 calc PR B 2 H27L H 0.0721 0.0500 0.6875 0.206 Uiso 0.32(2) 1 calc PR B 2 C23E C 0.1515(14) 0.1744(17) 0.7070(8) 0.12(2) Uiso 0.32(2) 1 d PD B 2 H28M H 0.1277 0.1681 0.7496 0.173 Uiso 0.32(2) 1 calc PR B 2 H28N H 0.1511 0.2261 0.6836 0.173 Uiso 0.32(2) 1 calc PR B 2 H28O H 0.2084 0.1453 0.7104 0.173 Uiso 0.32(2) 1 calc PR B 2 C23F C 0.0084(7) 0.1796(12) 0.6814(7) 0.020(7) Uiso 0.32(2) 1 d PD B 2 H29P H -0.0059 0.1637 0.7268 0.030 Uiso 0.32(2) 1 calc PR B 2 H29Q H -0.0241 0.1615 0.6602 0.030 Uiso 0.32(2) 1 calc PR B 2 H29R H -0.0039 0.2332 0.6631 0.030 Uiso 0.32(2) 1 calc PR B 2 C233 C 0.5595(5) 0.1507(4) 0.4876(3) 0.0273(19) Uiso 1 1 d D . . C234 C 0.5327(6) 0.1810(5) 0.5405(4) 0.035(2) Uiso 1 1 d D . . H220 H 0.5070 0.2333 0.5220 0.052 Uiso 1 1 calc R . . H221 H 0.5810 0.1740 0.5647 0.052 Uiso 1 1 calc R . . H222 H 0.4928 0.1552 0.5688 0.052 Uiso 1 1 calc R . . C235 C 0.6030(6) 0.0703(4) 0.5161(5) 0.038(2) Uiso 1 1 d D . . H223 H 0.5642 0.0425 0.5437 0.058 Uiso 1 1 calc R . . H224 H 0.6498 0.0651 0.5409 0.058 Uiso 1 1 calc R . . H225 H 0.6230 0.0516 0.4819 0.058 Uiso 1 1 calc R . . C236 C 0.6203(6) 0.1923(5) 0.4433(4) 0.037(2) Uiso 1 1 d D . . H226 H 0.6364 0.1745 0.4083 0.055 Uiso 1 1 calc R . . H227 H 0.6695 0.1846 0.4669 0.055 Uiso 1 1 calc R . . H228 H 0.5942 0.2447 0.4263 0.055 Uiso 1 1 calc R . . C237 C 0.4532(5) 0.4726(4) 0.1931(3) 0.0272(19) Uiso 1 1 d D . . C238 C 0.5124(6) 0.4535(6) 0.2464(4) 0.043(3) Uiso 1 1 d D . . H229 H 0.5413 0.4019 0.2589 0.064 Uiso 1 1 calc R . . H230 H 0.4812 0.4621 0.2829 0.064 Uiso 1 1 calc R . . H231 H 0.5527 0.4842 0.2315 0.064 Uiso 1 1 calc R . . C239 C 0.5023(6) 0.4580(5) 0.1368(4) 0.038(2) Uiso 1 1 d D . . H232 H 0.5374 0.4932 0.1182 0.056 Uiso 1 1 calc R . . H233 H 0.4641 0.4634 0.1049 0.056 Uiso 1 1 calc R . . H234 H 0.5369 0.4082 0.1513 0.056 Uiso 1 1 calc R . . C240 C 0.4109(6) 0.5537(4) 0.1719(5) 0.042(2) Uiso 1 1 d D . . H235 H 0.4528 0.5829 0.1579 0.063 Uiso 1 1 calc R . . H236 H 0.3786 0.5638 0.2075 0.063 Uiso 1 1 calc R . . H237 H 0.3741 0.5666 0.1368 0.063 Uiso 1 1 calc R . . C241 C 0.1660(5) 0.5420(4) 0.4091(4) 0.038(2) Uiso 1 1 d D . . C24A C 0.0885(7) 0.5945(7) 0.4201(8) 0.057(6) Uiso 0.619(19) 1 d PD C 3 H238 H 0.0441 0.5683 0.4369 0.085 Uiso 0.619(19) 1 calc PR C 3 H239 H 0.0716 0.6346 0.3799 0.085 Uiso 0.619(19) 1 calc PR C 3 H240 H 0.0998 0.6143 0.4507 0.085 Uiso 0.619(19) 1 calc PR C 3 C24B C 0.2205(9) 0.5848(8) 0.3580(6) 0.071(7) Uiso 0.619(19) 1 d PD C 3 H241 H 0.2377 0.6188 0.3726 0.107 Uiso 0.619(19) 1 calc PR C 3 H242 H 0.1894 0.6124 0.3189 0.107 Uiso 0.619(19) 1 calc PR C 3 H243 H 0.2695 0.5507 0.3499 0.107 Uiso 0.619(19) 1 calc PR C 3 C24C C 0.2138(9) 0.4995(7) 0.4699(5) 0.052(5) Uiso 0.619(19) 1 d PD C 3 H244 H 0.2231 0.5336 0.4881 0.079 Uiso 0.619(19) 1 calc PR C 3 H245 H 0.2671 0.4712 0.4606 0.079 Uiso 0.619(19) 1 calc PR C 3 H246 H 0.1822 0.4661 0.5003 0.079 Uiso 0.619(19) 1 calc PR C 3 C24D C 0.1226(16) 0.6200(5) 0.3704(11) 0.084(14) Uiso 0.381(19) 1 d PD C 4 H247 H 0.0629 0.6263 0.3783 0.126 Uiso 0.381(19) 1 calc PR C 4 H248 H 0.1347 0.6295 0.3252 0.126 Uiso 0.381(19) 1 calc PR C 4 H249 H 0.1424 0.6543 0.3829 0.126 Uiso 0.381(19) 1 calc PR C 4 C24E C 0.1408(17) 0.5252(13) 0.4790(6) 0.075(12) Uiso 0.381(19) 1 d PD C 4 H250 H 0.1692 0.4752 0.5042 0.113 Uiso 0.381(19) 1 calc PR C 4 H251 H 0.0810 0.5297 0.4839 0.113 Uiso 0.381(19) 1 calc PR C 4 H252 H 0.1560 0.5599 0.4938 0.113 Uiso 0.381(19) 1 calc PR C 4 C24F C 0.2592(7) 0.5335(14) 0.4020(14) 0.091(15) Uiso 0.381(19) 1 d PD C 4 H253 H 0.2721 0.5731 0.3640 0.137 Uiso 0.381(19) 1 calc PR C 4 H254 H 0.2849 0.4862 0.3979 0.137 Uiso 0.381(19) 1 calc PR C 4 H255 H 0.2804 0.5356 0.4395 0.137 Uiso 0.381(19) 1 calc PR C 4 C245 C -0.0098(5) 0.3856(5) 0.2746(4) 0.0256(19) Uiso 1 1 d . . . H256 H -0.0021 0.3598 0.2444 0.031 Uiso 1 1 calc R . . H257 H -0.0053 0.4366 0.2502 0.031 Uiso 1 1 calc R . . C246 C -0.0948(6) 0.3861(5) 0.3046(4) 0.0277(19) Uiso 1 1 d . . . C247 C -0.1261(8) 0.3230(7) 0.3252(6) 0.056(3) Uiso 1 1 d . . . H258 H -0.0928 0.2784 0.3230 0.067 Uiso 1 1 calc R . . C248 C -0.2060(9) 0.3265(8) 0.3486(7) 0.069(4) Uiso 1 1 d . . . H259 H -0.2286 0.2845 0.3628 0.083 Uiso 1 1 calc R . . C249 C -0.2533(6) 0.3933(6) 0.3511(5) 0.036(2) Uiso 1 1 d . . . C250 C -0.3374(7) 0.4017(6) 0.3720(5) 0.044(3) Uiso 1 1 d . . . H260 H -0.3636 0.3621 0.3833 0.053 Uiso 1 1 calc R . . C251 C -0.3795(7) 0.4661(6) 0.3756(5) 0.041(2) Uiso 1 1 d . . . H261 H -0.4353 0.4713 0.3904 0.049 Uiso 1 1 calc R . . C252 C -0.3427(10) 0.5249(9) 0.3582(7) 0.077(4) Uiso 1 1 d . . . H262 H -0.3733 0.5702 0.3605 0.093 Uiso 1 1 calc R . . C253 C -0.2601(8) 0.5170(8) 0.3371(6) 0.062(3) Uiso 1 1 d . . . H263 H -0.2341 0.5566 0.3269 0.074 Uiso 1 1 calc R . . C254 C -0.2162(6) 0.4525(5) 0.3310(4) 0.029(2) Uiso 1 1 d . . . N31 N 0.7645(7) 0.0668(7) 0.3605(5) 0.071(3) Uiso 1 1 d D . . C31 C 0.8133(6) 0.0588(6) 0.3944(5) 0.042(2) Uiso 1 1 d D . . C32 C 0.8747(7) 0.0461(8) 0.4385(6) 0.063(3) Uiso 1 1 d D . . H32A H 0.8797 -0.0030 0.4710 0.094 Uiso 1 1 calc R . . H32B H 0.8587 0.0826 0.4588 0.094 Uiso 1 1 calc R . . H32C H 0.9279 0.0500 0.4162 0.094 Uiso 1 1 calc R . . N41 N 0.6317(6) 0.2535(6) 0.2583(5) 0.059(3) Uiso 1 1 d D . . C41 C 0.6976(6) 0.2331(6) 0.2445(5) 0.043(3) Uiso 1 1 d D . . C42 C 0.7811(7) 0.2089(9) 0.2260(8) 0.084(5) Uiso 1 1 d D . . H42A H 0.7878 0.2318 0.1800 0.126 Uiso 1 1 calc R . . H42B H 0.7943 0.1556 0.2383 0.126 Uiso 1 1 calc R . . H42C H 0.8184 0.2226 0.2473 0.126 Uiso 1 1 calc R . . N51 N 0.4482(8) 0.3834(8) 0.4290(7) 0.088(4) Uiso 1 1 d D . . C51 C 0.3946(6) 0.3636(6) 0.4213(6) 0.049(3) Uiso 1 1 d D . . C52 C 0.3272(6) 0.3374(6) 0.4123(5) 0.046(3) Uiso 1 1 d D . . H52A H 0.3181 0.3529 0.3668 0.069 Uiso 1 1 calc R . . H52B H 0.2772 0.3575 0.4325 0.069 Uiso 1 1 calc R . . H52C H 0.3398 0.2839 0.4314 0.069 Uiso 1 1 calc R . . N61 N 0.3990(11) 0.0668(7) 0.6648(8) 0.112(5) Uiso 1 1 d D . . C61 C 0.3996(8) 0.0066(6) 0.6877(6) 0.057(3) Uiso 1 1 d D . . C62 C 0.3957(9) -0.0682(6) 0.7203(6) 0.065(4) Uiso 1 1 d D . . H62A H 0.4471 -0.1000 0.7125 0.097 Uiso 1 1 calc R . . H62B H 0.3490 -0.0776 0.7048 0.097 Uiso 1 1 calc R . . H62C H 0.3883 -0.0781 0.7659 0.097 Uiso 1 1 calc R . . N71 N 0.5896(7) 0.0125(6) 0.1541(5) 0.065(3) Uiso 1 1 d D . . C71 C 0.6300(8) -0.0425(6) 0.1576(6) 0.057(3) Uiso 1 1 d D . . C72 C 0.6850(12) -0.1099(9) 0.1589(11) 0.128(8) Uiso 1 1 d D . . H72A H 0.6775 -0.1490 0.1991 0.192 Uiso 1 1 calc R . . H72B H 0.7422 -0.1045 0.1549 0.192 Uiso 1 1 calc R . . H72C H 0.6730 -0.1221 0.1236 0.192 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 Pt1 0.01084(15) 0.02031(16) 0.01229(15) -0.00169(11) 0.00012(10) -0.00445(11) Cl1 0.0143(9) 0.0394(12) 0.0233(10) -0.0065(9) -0.0001(8) -0.0139(8) Cl2 0.0287(11) 0.0330(11) 0.0168(10) -0.0070(8) 0.0068(8) -0.0160(9) P1 0.0122(10) 0.0315(12) 0.0136(10) -0.0048(9) -0.0004(8) -0.0094(8) O11 0.016(3) 0.044(4) 0.016(3) -0.011(3) 0.001(2) -0.019(3) O12 0.016(3) 0.031(3) 0.016(3) 0.000(2) -0.004(2) -0.004(2) O13 0.015(3) 0.021(3) 0.015(3) -0.004(2) -0.001(2) -0.009(2) O14 0.018(3) 0.053(4) 0.027(3) -0.030(3) 0.013(2) -0.021(3) P2 0.0138(9) 0.0173(10) 0.0125(9) -0.0040(8) 0.0008(7) -0.0031(8) O21 0.018(3) 0.018(3) 0.010(2) -0.004(2) 0.002(2) -0.006(2) O22 0.015(3) 0.024(3) 0.017(3) -0.007(2) -0.001(2) -0.005(2) O23 0.014(3) 0.020(3) 0.024(3) -0.004(2) -0.001(2) -0.008(2) O24 0.014(3) 0.021(3) 0.018(3) -0.002(2) 0.000(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.210(2) . ? Pt1 P2 2.215(2) . ? Pt1 Cl1 2.3387(19) . ? Pt1 Cl2 2.3420(19) . ? P1 O13 1.569(5) . ? P1 O11 1.577(6) . ? P1 O12 1.599(6) . ? O11 C11 1.426(10) . ? O12 C18 1.416(10) . ? O13 C115 1.421(9) . ? O14 C145 1.463(10) . ? O14 C122 1.480(9) . ? N1 C146 1.310(10) . ? N1 C154 1.367(11) . ? C11 C12 1.385(13) . ? C11 C16 1.412(13) . ? C12 C13 1.394(14) . ? C12 C128 1.501(13) . ? C13 C14 1.362(15) . ? C13 H11 0.9500 . ? C14 C15 1.435(14) . ? C14 C129 1.556(11) . ? C15 C16 1.394(14) . ? C15 H12 0.9500 . ? C16 C17 1.512(13) . ? C17 C19 1.503(13) . ? C17 H13 0.9900 . ? C17 H14 0.9900 . ? C18 C19 1.382(13) . ? C18 C113 1.387(12) . ? C19 C110 1.399(14) . ? C110 C111 1.389(14) . ? C110 H15 0.9500 . ? C111 C112 1.414(13) . ? C111 C133 1.544(12) . ? C112 C113 1.413(13) . ? C112 H16 0.9500 . ? C113 C114 1.487(12) . ? C114 C116 1.513(11) . ? C114 H17 0.9900 . ? C114 H18 0.9900 . ? C115 C116 1.406(10) . ? C115 C120 1.407(11) . ? C116 C117 1.395(11) . ? C117 C118 1.388(12) . ? C117 H19 0.9500 . ? C118 C119 1.410(12) . ? C118 C137 1.515(13) . ? C119 C120 1.388(11) . ? C119 H110 0.9500 . ? C120 C121 1.514(11) . ? C121 C123 1.526(11) . ? C121 H111 0.9900 . ? C121 H112 0.9900 . ? C122 C123 1.326(11) . ? C122 C127 1.375(12) . ? C123 C124 1.398(11) . ? C124 C125 1.386(13) . ? C124 H113 0.9500 . ? C125 C126 1.413(13) . ? C125 C141 1.544(14) . ? C126 C127 1.394(13) . ? C126 H114 0.9500 . ? C127 C128 1.481(12) . ? C128 H115 0.9900 . ? C128 H116 0.9900 . ? C129 C13C 1.516(7) . ? C129 C13B 1.517(7) . ? C129 C13D 1.519(7) . ? C129 C13E 1.521(7) . ? C129 C13F 1.528(7) . ? C129 C13A 1.535(7) . ? C13A H17A 0.9800 . ? C13A H17B 0.9800 . ? C13A H17C 0.9800 . ? C13B H18D 0.9800 . ? C13B H18E 0.9800 . ? C13B H18F 0.9800 . ? C13C H19G 0.9800 . ? C13C H19H 0.9800 . ? C13C H19I 0.9800 . ? C13D H17J 0.9800 . ? C13D H17K 0.9800 . ? C13D H17L 0.9800 . ? C13E H18M 0.9800 . ? C13E H18N 0.9800 . ? C13E H18O 0.9800 . ? C13F H19P 0.9800 . ? C13F H19Q 0.9800 . ? C13F H19R 0.9800 . ? C133 C136 1.524(7) . ? C133 C134 1.526(7) . ? C133 C135 1.527(7) . ? C134 H120 0.9800 . ? C134 H121 0.9800 . ? C134 H122 0.9800 . ? C135 H123 0.9800 . ? C135 H124 0.9800 . ? C135 H125 0.9800 . ? C136 H126 0.9800 . ? C136 H127 0.9800 . ? C136 H128 0.9800 . ? C137 C138 1.516(7) . ? C137 C140 1.520(7) . ? C137 C139 1.528(7) . ? C138 H129 0.9800 . ? C138 H130 0.9800 . ? C138 H131 0.9800 . ? C139 H132 0.9800 . ? C139 H133 0.9800 . ? C139 H134 0.9800 . ? C140 H135 0.9800 . ? C140 H136 0.9800 . ? C140 H137 0.9800 . ? C141 C142 1.518(7) . ? C141 C144 1.526(7) . ? C141 C143 1.535(7) . ? C142 H138 0.9800 . ? C142 H139 0.9800 . ? C142 H140 0.9800 . ? C143 H141 0.9800 . ? C143 H142 0.9800 . ? C143 H143 0.9800 . ? C144 H144 0.9800 . ? C144 H145 0.9800 . ? C144 H146 0.9800 . ? C145 C146 1.513(11) . ? C145 H147 0.9900 . ? C145 H148 0.9900 . ? C146 C147 1.433(12) . ? C147 C148 1.359(12) . ? C147 H149 0.9500 . ? C148 C149 1.420(12) . ? C148 H150 0.9500 . ? C149 C150 1.394(14) . ? C149 C154 1.416(12) . ? C150 C151 1.391(16) . ? C150 H151 0.9500 . ? C151 C152 1.385(16) . ? C151 H152 0.9500 . ? C152 C153 1.368(15) . ? C152 H153 0.9500 . ? C153 C154 1.422(13) . ? C153 H154 0.9500 . ? P2 O23 1.580(6) . ? P2 O21 1.596(5) . ? P2 O22 1.601(6) . ? O21 C21 1.429(9) . ? O22 C28 1.413(9) . ? O23 C215 1.421(9) . ? O24 C222 1.384(10) . ? O24 C245 1.448(10) . ? N2 C246 1.304(12) . ? N2 C254 1.365(12) . ? C21 C26 1.367(12) . ? C21 C22 1.405(11) . ? C22 C23 1.404(13) . ? C22 C228 1.510(11) . ? C23 C24 1.391(13) . ? C23 H21 0.9500 . ? C24 C25 1.402(13) . ? C24 C229 1.541(11) . ? C25 C26 1.397(12) . ? C25 H22 0.9500 . ? C26 C27 1.518(11) . ? C27 C29 1.507(11) . ? C27 H23 0.9900 . ? C27 H24 0.9900 . ? C28 C213 1.375(11) . ? C28 C29 1.380(11) . ? C29 C210 1.400(11) . ? C210 C211 1.408(11) . ? C210 H25 0.9500 . ? C211 C212 1.388(11) . ? C211 C233 1.534(11) . ? C212 C213 1.394(11) . ? C212 H26 0.9500 . ? C213 C214 1.503(11) . ? C214 C216 1.505(10) . ? C214 H27 0.9900 . ? C214 H28 0.9900 . ? C215 C220 1.394(11) . ? C215 C216 1.400(11) . ? C216 C217 1.394(11) . ? C217 C218 1.390(12) . ? C217 H29 0.9500 . ? C218 C219 1.387(12) . ? C218 C237 1.532(12) . ? C219 C220 1.377(12) . ? C219 H210 0.9500 . ? C220 C221 1.513(11) . ? C221 C223 1.510(12) . ? C221 H211 0.9900 . ? C221 H212 0.9900 . ? C222 C223 1.397(12) . ? C222 C227 1.405(11) . ? C223 C224 1.391(12) . ? C224 C225 1.384(12) . ? C224 H213 0.9500 . ? C225 C226 1.418(12) . ? C225 C241 1.552(10) . ? C226 C227 1.389(12) . ? C226 H214 0.9500 . ? C227 C228 1.498(11) . ? C228 H215 0.9900 . ? C228 H216 0.9900 . ? C229 C23A 1.509(7) . ? C229 C23E 1.510(7) . ? C229 C23C 1.527(7) . ? C229 C23D 1.532(7) . ? C229 C23F 1.539(7) . ? C229 C23B 1.544(7) . ? C23A H27A 0.9800 . ? C23A H27B 0.9800 . ? C23A H27C 0.9800 . ? C23B H28D 0.9800 . ? C23B H28E 0.9800 . ? C23B H28F 0.9800 . ? C23C H29G 0.9800 . ? C23C H29H 0.9800 . ? C23C H29I 0.9800 . ? C23D H27J 0.9800 . ? C23D H27K 0.9800 . ? C23D H27L 0.9800 . ? C23E H28M 0.9800 . ? C23E H28N 0.9800 . ? C23E H28O 0.9800 . ? C23F H29P 0.9800 . ? C23F H29Q 0.9800 . ? C23F H29R 0.9800 . ? C233 C235 1.523(7) . ? C233 C236 1.525(7) . ? C233 C234 1.526(7) . ? C234 H220 0.9800 . ? C234 H221 0.9800 . ? C234 H222 0.9800 . ? C235 H223 0.9800 . ? C235 H224 0.9800 . ? C235 H225 0.9800 . ? C236 H226 0.9800 . ? C236 H227 0.9800 . ? C236 H228 0.9800 . ? C237 C239 1.525(7) . ? C237 C238 1.526(7) . ? C237 C240 1.527(7) . ? C238 H229 0.9800 . ? C238 H230 0.9800 . ? C238 H231 0.9800 . ? C239 H232 0.9800 . ? C239 H233 0.9800 . ? C239 H234 0.9800 . ? C240 H235 0.9800 . ? C240 H236 0.9800 . ? C240 H237 0.9800 . ? C241 C24C 1.516(7) . ? C241 C24A 1.520(7) . ? C241 C24F 1.521(7) . ? C241 C24D 1.522(7) . ? C241 C24B 1.529(7) . ? C241 C24E 1.530(7) . ? C24A H238 0.9800 . ? C24A H239 0.9800 . ? C24A H240 0.9800 . ? C24B H241 0.9800 . ? C24B H242 0.9800 . ? C24B H243 0.9800 . ? C24C H244 0.9800 . ? C24C H245 0.9800 . ? C24C H246 0.9800 . ? C24D H247 0.9800 . ? C24D H248 0.9800 . ? C24D H249 0.9800 . ? C24E H250 0.9800 . ? C24E H251 0.9800 . ? C24E H252 0.9800 . ? C24F H253 0.9800 . ? C24F H254 0.9800 . ? C24F H255 0.9800 . ? C245 C246 1.507(12) . ? C245 H256 0.9900 . ? C245 H257 0.9900 . ? C246 C247 1.401(15) . ? C247 C248 1.377(18) . ? C247 H258 0.9500 . ? C248 C249 1.405(17) . ? C248 H259 0.9500 . ? C249 C254 1.390(13) . ? C249 C250 1.422(15) . ? C250 C251 1.346(15) . ? C250 H260 0.9500 . ? C251 C252 1.383(18) . ? C251 H261 0.9500 . ? C252 C253 1.40(2) . ? C252 H262 0.9500 . ? C253 C254 1.378(16) . ? C253 H263 0.9500 . ? N31 C31 1.126(9) . ? C31 C32 1.429(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N41 C41 1.130(9) . ? C41 C42 1.430(10) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N51 C51 1.125(9) . ? C51 C52 1.427(9) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N61 C61 1.130(9) . ? C61 C62 1.430(10) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N71 C71 1.127(9) . ? C71 C72 1.433(10) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? 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 Pt1 P2 95.25(7) . . ? P1 Pt1 Cl1 87.79(7) . . ? P2 Pt1 Cl1 175.34(8) . . ? P1 Pt1 Cl2 173.13(8) . . ? P2 Pt1 Cl2 89.92(7) . . ? Cl1 Pt1 Cl2 87.34(7) . . ? O13 P1 O11 103.1(3) . . ? O13 P1 O12 107.2(3) . . ? O11 P1 O12 105.1(3) . . ? O13 P1 Pt1 113.0(2) . . ? O11 P1 Pt1 119.6(2) . . ? O12 P1 Pt1 108.1(2) . . ? C11 O11 P1 142.0(6) . . ? C18 O12 P1 121.9(5) . . ? C115 O13 P1 145.7(5) . . ? C145 O14 C122 117.9(6) . . ? C146 N1 C154 118.1(7) . . ? C12 C11 C16 120.3(9) . . ? C12 C11 O11 118.0(8) . . ? C16 C11 O11 121.6(8) . . ? C11 C12 C13 119.6(9) . . ? C11 C12 C128 123.4(9) . . ? C13 C12 C128 116.9(9) . . ? C14 C13 C12 122.9(10) . . ? C14 C13 H11 118.5 . . ? C12 C13 H11 118.5 . . ? C13 C14 C15 116.5(9) . . ? C13 C14 C129 124.7(8) . . ? C15 C14 C129 118.8(8) . . ? C16 C15 C14 122.3(10) . . ? C16 C15 H12 118.9 . . ? C14 C15 H12 118.9 . . ? C15 C16 C11 117.8(9) . . ? C15 C16 C17 118.1(9) . . ? C11 C16 C17 124.0(9) . . ? C19 C17 C16 114.1(8) . . ? C19 C17 H13 108.7 . . ? C16 C17 H13 108.7 . . ? C19 C17 H14 108.7 . . ? C16 C17 H14 108.7 . . ? H13 C17 H14 107.6 . . ? C19 C18 C113 123.9(8) . . ? C19 C18 O12 118.5(8) . . ? C113 C18 O12 117.5(8) . . ? C18 C19 C110 117.9(9) . . ? C18 C19 C17 120.1(9) . . ? C110 C19 C17 122.0(9) . . ? C111 C110 C19 121.6(10) . . ? C111 C110 H15 119.2 . . ? C19 C110 H15 119.2 . . ? C110 C111 C112 118.5(8) . . ? C110 C111 C133 123.9(8) . . ? C112 C111 C133 117.6(7) . . ? C113 C112 C111 121.3(9) . . ? C113 C112 H16 119.4 . . ? C111 C112 H16 119.4 . . ? C18 C113 C112 116.8(8) . . ? C18 C113 C114 120.7(8) . . ? C112 C113 C114 122.4(8) . . ? C113 C114 C116 112.2(7) . . ? C113 C114 H17 109.2 . . ? C116 C114 H17 109.2 . . ? C113 C114 H18 109.2 . . ? C116 C114 H18 109.2 . . ? H17 C114 H18 107.9 . . ? C116 C115 C120 121.0(7) . . ? C116 C115 O13 122.0(6) . . ? C120 C115 O13 116.2(6) . . ? C117 C116 C115 118.0(7) . . ? C117 C116 C114 117.9(7) . . ? C115 C116 C114 124.0(7) . . ? C118 C117 C116 123.3(8) . . ? C118 C117 H19 118.3 . . ? C116 C117 H19 118.3 . . ? C117 C118 C119 116.4(8) . . ? C117 C118 C137 123.6(8) . . ? C119 C118 C137 119.8(8) . . ? C120 C119 C118 123.1(8) . . ? C120 C119 H110 118.5 . . ? C118 C119 H110 118.5 . . ? C119 C120 C115 118.0(7) . . ? C119 C120 C121 119.3(7) . . ? C115 C120 C121 122.7(7) . . ? C120 C121 C123 109.6(7) . . ? C120 C121 H111 109.7 . . ? C123 C121 H111 109.7 . . ? C120 C121 H112 109.7 . . ? C123 C121 H112 109.7 . . ? H111 C121 H112 108.2 . . ? C123 C122 C127 127.9(8) . . ? C123 C122 O14 116.5(7) . . ? C127 C122 O14 115.0(7) . . ? C122 C123 C124 116.0(8) . . ? C122 C123 C121 122.6(7) . . ? C124 C123 C121 120.4(7) . . ? C125 C124 C123 122.0(8) . . ? C125 C124 H113 119.0 . . ? C123 C124 H113 119.0 . . ? C124 C125 C126 117.5(9) . . ? C124 C125 C141 118.2(8) . . ? C126 C125 C141 124.4(9) . . ? C127 C126 C125 121.9(9) . . ? C127 C126 H114 119.1 . . ? C125 C126 H114 119.1 . . ? C122 C127 C126 114.6(8) . . ? C122 C127 C128 121.8(8) . . ? C126 C127 C128 122.7(8) . . ? C127 C128 C12 114.0(8) . . ? C127 C128 H115 108.7 . . ? C12 C128 H115 108.7 . . ? C127 C128 H116 108.7 . . ? C12 C128 H116 108.7 . . ? H115 C128 H116 107.6 . . ? C13C C129 C13B 110.5(7) . . ? C13C C129 C13D 90.0(14) . . ? C13B C129 C13D 125.4(12) . . ? C13C C129 C13E 125.6(12) . . ? C13B C129 C13E 18.8(12) . . ? C13D C129 C13E 110.5(7) . . ? C13C C129 C13F 21.0(14) . . ? C13B C129 C13F 92.2(13) . . ? C13D C129 C13F 109.5(6) . . ? C13E C129 C13F 109.3(6) . . ? C13C C129 C13A 109.5(7) . . ? C13B C129 C13A 109.4(6) . . ? C13D C129 C13A 20.9(13) . . ? C13E C129 C13A 92.3(12) . . ? C13F C129 C13A 127.4(12) . . ? C13C C129 C14 109.5(7) . . ? C13B C129 C14 109.7(6) . . ? C13D C129 C14 109.5(7) . . ? C13E C129 C14 109.7(6) . . ? C13F C129 C14 108.3(6) . . ? C13A C129 C14 108.1(6) . . ? C129 C13A H17A 109.5 . . ? C129 C13A H17B 109.5 . . ? H17A C13A H17B 109.5 . . ? C129 C13A H17C 109.5 . . ? H17A C13A H17C 109.5 . . ? H17B C13A H17C 109.5 . . ? C129 C13B H18D 109.5 . . ? C129 C13B H18E 109.5 . . ? H18D C13B H18E 109.5 . . ? C129 C13B H18F 109.5 . . ? H18D C13B H18F 109.5 . . ? H18E C13B H18F 109.5 . . ? C129 C13C H19G 109.5 . . ? C129 C13C H19H 109.5 . . ? H19G C13C H19H 109.5 . . ? C129 C13C H19I 109.5 . . ? H19G C13C H19I 109.5 . . ? H19H C13C H19I 109.5 . . ? C129 C13D H17J 109.5 . . ? C129 C13D H17K 109.5 . . ? H17J C13D H17K 109.5 . . ? C129 C13D H17L 109.4 . . ? H17J C13D H17L 109.5 . . ? H17K C13D H17L 109.5 . . ? C129 C13E H18M 109.5 . . ? C129 C13E H18N 109.5 . . ? H18M C13E H18N 109.5 . . ? C129 C13E H18O 109.5 . . ? H18M C13E H18O 109.5 . . ? H18N C13E H18O 109.5 . . ? C129 C13F H19P 109.5 . . ? C129 C13F H19Q 109.5 . . ? H19P C13F H19Q 109.5 . . ? C129 C13F H19R 109.5 . . ? H19P C13F H19R 109.5 . . ? H19Q C13F H19R 109.5 . . ? C136 C133 C134 109.3(6) . . ? C136 C133 C135 109.6(6) . . ? C134 C133 C135 109.0(6) . . ? C136 C133 C111 109.6(6) . . ? C134 C133 C111 110.3(6) . . ? C135 C133 C111 109.0(6) . . ? C133 C134 H120 109.5 . . ? C133 C134 H121 109.5 . . ? H120 C134 H121 109.5 . . ? C133 C134 H122 109.5 . . ? H120 C134 H122 109.5 . . ? H121 C134 H122 109.5 . . ? C133 C135 H123 109.5 . . ? C133 C135 H124 109.5 . . ? H123 C135 H124 109.5 . . ? C133 C135 H125 109.5 . . ? H123 C135 H125 109.5 . . ? H124 C135 H125 109.5 . . ? C133 C136 H126 109.5 . . ? C133 C136 H127 109.5 . . ? H126 C136 H127 109.5 . . ? C133 C136 H128 109.5 . . ? H126 C136 H128 109.5 . . ? H127 C136 H128 109.5 . . ? C118 C137 C138 112.7(9) . . ? C118 C137 C140 108.3(9) . . ? C138 C137 C140 110.7(8) . . ? C118 C137 C139 108.5(9) . . ? C138 C137 C139 107.9(8) . . ? C140 C137 C139 108.7(8) . . ? C137 C138 H129 109.5 . . ? C137 C138 H130 109.5 . . ? H129 C138 H130 109.5 . . ? C137 C138 H131 109.5 . . ? H129 C138 H131 109.5 . . ? H130 C138 H131 109.5 . . ? C137 C139 H132 109.5 . . ? C137 C139 H133 109.5 . . ? H132 C139 H133 109.5 . . ? C137 C139 H134 109.5 . . ? H132 C139 H134 109.5 . . ? H133 C139 H134 109.5 . . ? C137 C140 H135 109.5 . . ? C137 C140 H136 109.5 . . ? H135 C140 H136 109.5 . . ? C137 C140 H137 109.5 . . ? H135 C140 H137 109.5 . . ? H136 C140 H137 109.5 . . ? C142 C141 C144 110.4(8) . . ? C142 C141 C143 106.6(8) . . ? C144 C141 C143 105.8(8) . . ? C142 C141 C125 112.2(9) . . ? C144 C141 C125 110.6(9) . . ? C143 C141 C125 111.0(9) . . ? C141 C142 H138 109.5 . . ? C141 C142 H139 109.5 . . ? H138 C142 H139 109.5 . . ? C141 C142 H140 109.5 . . ? H138 C142 H140 109.5 . . ? H139 C142 H140 109.5 . . ? C141 C143 H141 109.5 . . ? C141 C143 H142 109.5 . . ? H141 C143 H142 109.5 . . ? C141 C143 H143 109.5 . . ? H141 C143 H143 109.5 . . ? H142 C143 H143 109.5 . . ? C141 C144 H144 109.5 . . ? C141 C144 H145 109.5 . . ? H144 C144 H145 109.5 . . ? C141 C144 H146 109.5 . . ? H144 C144 H146 109.5 . . ? H145 C144 H146 109.5 . . ? O14 C145 C146 112.2(6) . . ? O14 C145 H147 109.2 . . ? C146 C145 H147 109.2 . . ? O14 C145 H148 109.2 . . ? C146 C145 H148 109.2 . . ? H147 C145 H148 107.9 . . ? N1 C146 C147 123.0(8) . . ? N1 C146 C145 117.3(7) . . ? C147 C146 C145 119.5(7) . . ? C148 C147 C146 119.3(8) . . ? C148 C147 H149 120.3 . . ? C146 C147 H149 120.3 . . ? C147 C148 C149 119.2(8) . . ? C147 C148 H150 120.4 . . ? C149 C148 H150 120.4 . . ? C150 C149 C154 120.6(9) . . ? C150 C149 C148 122.0(9) . . ? C154 C149 C148 117.4(8) . . ? C151 C150 C149 119.4(10) . . ? C151 C150 H151 120.3 . . ? C149 C150 H151 120.3 . . ? C152 C151 C150 120.4(11) . . ? C152 C151 H152 119.8 . . ? C150 C151 H152 119.8 . . ? C153 C152 C151 121.2(11) . . ? C153 C152 H153 119.4 . . ? C151 C152 H153 119.4 . . ? C152 C153 C154 120.1(10) . . ? C152 C153 H154 120.0 . . ? C154 C153 H154 120.0 . . ? N1 C154 C149 122.8(8) . . ? N1 C154 C153 119.0(8) . . ? C149 C154 C153 118.2(8) . . ? O23 P2 O21 102.9(3) . . ? O23 P2 O22 106.9(3) . . ? O21 P2 O22 105.0(3) . . ? O23 P2 Pt1 112.3(2) . . ? O21 P2 Pt1 120.1(2) . . ? O22 P2 Pt1 108.8(2) . . ? C21 O21 P2 136.9(5) . . ? C28 O22 P2 122.4(5) . . ? C215 O23 P2 144.5(5) . . ? C222 O24 C245 114.9(6) . . ? C246 N2 C254 118.5(8) . . ? C26 C21 C22 121.4(8) . . ? C26 C21 O21 123.2(7) . . ? C22 C21 O21 115.4(7) . . ? C23 C22 C21 117.8(8) . . ? C23 C22 C228 115.8(8) . . ? C21 C22 C228 126.2(7) . . ? C24 C23 C22 122.7(9) . . ? C24 C23 H21 118.6 . . ? C22 C23 H21 118.6 . . ? C23 C24 C25 116.4(8) . . ? C23 C24 C229 123.0(8) . . ? C25 C24 C229 120.4(7) . . ? C26 C25 C24 122.5(9) . . ? C26 C25 H22 118.8 . . ? C24 C25 H22 118.8 . . ? C21 C26 C25 119.0(8) . . ? C21 C26 C27 125.6(8) . . ? C25 C26 C27 115.3(8) . . ? C29 C27 C26 115.1(7) . . ? C29 C27 H23 108.5 . . ? C26 C27 H23 108.5 . . ? C29 C27 H24 108.5 . . ? C26 C27 H24 108.5 . . ? H23 C27 H24 107.5 . . ? C213 C28 C29 123.6(7) . . ? C213 C28 O22 119.0(6) . . ? C29 C28 O22 117.3(6) . . ? C28 C29 C210 117.0(7) . . ? C28 C29 C27 120.1(7) . . ? C210 C29 C27 122.9(7) . . ? C29 C210 C211 122.0(8) . . ? C29 C210 H25 119.0 . . ? C211 C210 H25 119.0 . . ? C212 C211 C210 117.5(7) . . ? C212 C211 C233 123.1(7) . . ? C210 C211 C233 119.4(7) . . ? C211 C212 C213 122.1(7) . . ? C211 C212 H26 119.0 . . ? C213 C212 H26 119.0 . . ? C28 C213 C212 117.8(7) . . ? C28 C213 C214 119.3(7) . . ? C212 C213 C214 122.7(7) . . ? C213 C214 C216 111.8(6) . . ? C213 C214 H27 109.3 . . ? C216 C214 H27 109.3 . . ? C213 C214 H28 109.3 . . ? C216 C214 H28 109.3 . . ? H27 C214 H28 107.9 . . ? C220 C215 C216 120.6(7) . . ? C220 C215 O23 116.8(7) . . ? C216 C215 O23 122.2(7) . . ? C217 C216 C215 117.9(7) . . ? C217 C216 C214 117.4(7) . . ? C215 C216 C214 124.7(7) . . ? C218 C217 C216 122.9(8) . . ? C218 C217 H29 118.6 . . ? C216 C217 H29 118.6 . . ? C219 C218 C217 116.3(8) . . ? C219 C218 C237 123.9(7) . . ? C217 C218 C237 119.8(7) . . ? C220 C219 C218 123.5(8) . . ? C220 C219 H210 118.3 . . ? C218 C219 H210 118.3 . . ? C219 C220 C215 118.4(7) . . ? C219 C220 C221 119.3(7) . . ? C215 C220 C221 122.3(7) . . ? C223 C221 C220 109.2(7) . . ? C223 C221 H211 109.8 . . ? C220 C221 H211 109.8 . . ? C223 C221 H212 109.8 . . ? C220 C221 H212 109.8 . . ? H211 C221 H212 108.3 . . ? O24 C222 C223 121.2(7) . . ? O24 C222 C227 118.1(7) . . ? C223 C222 C227 120.1(8) . . ? C224 C223 C222 119.1(8) . . ? C224 C223 C221 120.6(8) . . ? C222 C223 C221 119.9(8) . . ? C225 C224 C223 122.2(8) . . ? C225 C224 H213 118.9 . . ? C223 C224 H213 118.9 . . ? C224 C225 C226 117.6(7) . . ? C224 C225 C241 121.3(7) . . ? C226 C225 C241 121.0(7) . . ? C227 C226 C225 121.5(8) . . ? C227 C226 H214 119.2 . . ? C225 C226 H214 119.2 . . ? C226 C227 C222 118.9(8) . . ? C226 C227 C228 122.7(7) . . ? C222 C227 C228 118.4(7) . . ? C227 C228 C22 114.8(7) . . ? C227 C228 H215 108.6 . . ? C22 C228 H215 108.6 . . ? C227 C228 H216 108.6 . . ? C22 C228 H216 108.6 . . ? H215 C228 H216 107.5 . . ? C23A C229 C23E 135.1(11) . . ? C23A C229 C23C 111.3(6) . . ? C23E C229 C23C 69.3(11) . . ? C23A C229 C23D 38.2(11) . . ? C23E C229 C23D 110.0(6) . . ? C23C C229 C23D 137.8(10) . . ? C23A C229 C23F 71.8(10) . . ? C23E C229 C23F 109.9(6) . . ? C23C C229 C23F 43.5(10) . . ? C23D C229 C23F 108.0(6) . . ? C23A C229 C24 110.4(6) . . ? C23E C229 C24 110.9(6) . . ? C23C C229 C24 110.0(6) . . ? C23D C229 C24 109.2(6) . . ? C23F C229 C24 108.9(6) . . ? C23A C229 C23B 109.1(6) . . ? C23E C229 C23B 39.9(12) . . ? C23C C229 C23B 107.3(6) . . ? C23D C229 C23B 74.0(12) . . ? C23F C229 C23B 139.1(9) . . ? C24 C229 C23B 108.6(6) . . ? C229 C23A H27A 109.5 . . ? C229 C23A H27B 109.5 . . ? H27A C23A H27B 109.5 . . ? C229 C23A H27C 109.5 . . ? H27A C23A H27C 109.5 . . ? H27B C23A H27C 109.5 . . ? C229 C23B H28D 109.5 . . ? C229 C23B H28E 109.5 . . ? H28D C23B H28E 109.5 . . ? C229 C23B H28F 109.5 . . ? H28D C23B H28F 109.5 . . ? H28E C23B H28F 109.5 . . ? C229 C23C H29G 109.5 . . ? C229 C23C H29H 109.5 . . ? H29G C23C H29H 109.5 . . ? C229 C23C H29I 109.5 . . ? H29G C23C H29I 109.5 . . ? H29H C23C H29I 109.5 . . ? C229 C23D H27J 109.5 . . ? C229 C23D H27K 109.5 . . ? H27J C23D H27K 109.5 . . ? C229 C23D H27L 109.5 . . ? H27J C23D H27L 109.5 . . ? H27K C23D H27L 109.5 . . ? C229 C23E H28M 109.5 . . ? C229 C23E H28N 109.5 . . ? H28M C23E H28N 109.5 . . ? C229 C23E H28O 109.5 . . ? H28M C23E H28O 109.5 . . ? H28N C23E H28O 109.5 . . ? C229 C23F H29P 109.5 . . ? C229 C23F H29Q 109.5 . . ? H29P C23F H29Q 109.5 . . ? C229 C23F H29R 109.5 . . ? H29P C23F H29R 109.5 . . ? H29Q C23F H29R 109.5 . . ? C235 C233 C236 108.4(6) . . ? C235 C233 C234 109.5(6) . . ? C236 C233 C234 108.9(6) . . ? C235 C233 C211 106.9(7) . . ? C236 C233 C211 112.1(7) . . ? C234 C233 C211 111.0(7) . . ? C233 C234 H220 109.5 . . ? C233 C234 H221 109.5 . . ? H220 C234 H221 109.5 . . ? C233 C234 H222 109.5 . . ? H220 C234 H222 109.5 . . ? H221 C234 H222 109.5 . . ? C233 C235 H223 109.5 . . ? C233 C235 H224 109.5 . . ? H223 C235 H224 109.5 . . ? C233 C235 H225 109.5 . . ? H223 C235 H225 109.5 . . ? H224 C235 H225 109.5 . . ? C233 C236 H226 109.5 . . ? C233 C236 H227 109.5 . . ? H226 C236 H227 109.5 . . ? C233 C236 H228 109.5 . . ? H226 C236 H228 109.5 . . ? H227 C236 H228 109.5 . . ? C239 C237 C238 109.0(6) . . ? C239 C237 C240 108.6(6) . . ? C238 C237 C240 109.2(7) . . ? C239 C237 C218 109.5(7) . . ? C238 C237 C218 108.7(7) . . ? C240 C237 C218 111.9(7) . . ? C237 C238 H229 109.5 . . ? C237 C238 H230 109.5 . . ? H229 C238 H230 109.5 . . ? C237 C238 H231 109.5 . . ? H229 C238 H231 109.5 . . ? H230 C238 H231 109.5 . . ? C237 C239 H232 109.5 . . ? C237 C239 H233 109.5 . . ? H232 C239 H233 109.5 . . ? C237 C239 H234 109.5 . . ? H232 C239 H234 109.5 . . ? H233 C239 H234 109.5 . . ? C237 C240 H235 109.5 . . ? C237 C240 H236 109.5 . . ? H235 C240 H236 109.5 . . ? C237 C240 H237 109.5 . . ? H235 C240 H237 109.5 . . ? H236 C240 H237 109.5 . . ? C24C C241 C24A 110.8(6) . . ? C24C C241 C24F 64.6(11) . . ? C24A C241 C24F 140.5(10) . . ? C24C C241 C24D 139.9(10) . . ? C24A C241 C24D 46.4(11) . . ? C24F C241 C24D 109.9(6) . . ? C24C C241 C24B 109.7(6) . . ? C24A C241 C24B 109.6(6) . . ? C24F C241 C24B 47.7(11) . . ? C24D C241 C24B 65.6(11) . . ? C24C C241 C24E 47.6(11) . . ? C24A C241 C24E 66.0(11) . . ? C24F C241 C24E 109.3(6) . . ? C24D C241 C24E 109.2(6) . . ? C24B C241 C24E 140.8(10) . . ? C24C C241 C225 109.3(6) . . ? C24A C241 C225 108.7(6) . . ? C24F C241 C225 109.6(6) . . ? C24D C241 C225 109.7(6) . . ? C24B C241 C225 108.8(6) . . ? C24E C241 C225 109.2(6) . . ? C241 C24A H238 109.5 . . ? C241 C24A H239 109.5 . . ? H238 C24A H239 109.5 . . ? C241 C24A H240 109.5 . . ? H238 C24A H240 109.5 . . ? H239 C24A H240 109.5 . . ? C241 C24B H241 109.5 . . ? C241 C24B H242 109.5 . . ? H241 C24B H242 109.5 . . ? C241 C24B H243 109.5 . . ? H241 C24B H243 109.5 . . ? H242 C24B H243 109.5 . . ? C241 C24C H244 109.5 . . ? C241 C24C H245 109.5 . . ? H244 C24C H245 109.5 . . ? C241 C24C H246 109.5 . . ? H244 C24C H246 109.5 . . ? H245 C24C H246 109.5 . . ? C241 C24D H247 109.5 . . ? C241 C24D H248 109.5 . . ? H247 C24D H248 109.5 . . ? C241 C24D H249 109.5 . . ? H247 C24D H249 109.5 . . ? H248 C24D H249 109.5 . . ? C241 C24E H250 109.5 . . ? C241 C24E H251 109.5 . . ? H250 C24E H251 109.5 . . ? C241 C24E H252 109.5 . . ? H250 C24E H252 109.5 . . ? H251 C24E H252 109.5 . . ? C241 C24F H253 109.5 . . ? C241 C24F H254 109.5 . . ? H253 C24F H254 109.5 . . ? C241 C24F H255 109.5 . . ? H253 C24F H255 109.5 . . ? H254 C24F H255 109.5 . . ? O24 C245 C246 112.7(7) . . ? O24 C245 H256 109.1 . . ? C246 C245 H256 109.1 . . ? O24 C245 H257 109.1 . . ? C246 C245 H257 109.1 . . ? H256 C245 H257 107.8 . . ? N2 C246 C247 123.2(9) . . ? N2 C246 C245 116.3(8) . . ? C247 C246 C245 120.4(9) . . ? C248 C247 C246 119.0(12) . . ? C248 C247 H258 120.5 . . ? C246 C247 H258 120.5 . . ? C247 C248 C249 118.9(13) . . ? C247 C248 H259 120.6 . . ? C249 C248 H259 120.6 . . ? C254 C249 C248 118.0(10) . . ? C254 C249 C250 120.2(9) . . ? C248 C249 C250 121.8(11) . . ? C251 C250 C249 119.7(10) . . ? C251 C250 H260 120.1 . . ? C249 C250 H260 120.1 . . ? C250 C251 C252 120.9(12) . . ? C250 C251 H261 119.5 . . ? C252 C251 H261 119.5 . . ? C251 C252 C253 119.6(14) . . ? C251 C252 H262 120.2 . . ? C253 C252 H262 120.2 . . ? C254 C253 C252 120.8(13) . . ? C254 C253 H263 119.6 . . ? C252 C253 H263 119.6 . . ? N2 C254 C253 118.9(9) . . ? N2 C254 C249 122.5(9) . . ? C253 C254 C249 118.6(10) . . ? N31 C31 C32 178.0(14) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N41 C41 C42 178.8(15) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N51 C51 C52 179.0(16) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N61 C61 C62 175.4(17) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N71 C71 C72 176.2(17) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 O13 31.4(2) . . . . ? Cl1 Pt1 P1 O13 -152.1(2) . . . . ? P2 Pt1 P1 O11 152.9(3) . . . . ? Cl1 Pt1 P1 O11 -30.6(3) . . . . ? P2 Pt1 P1 O12 -87.1(2) . . . . ? Cl1 Pt1 P1 O12 89.4(2) . . . . ? O13 P1 O11 C11 -177.7(9) . . . . ? O12 P1 O11 C11 -65.6(9) . . . . ? Pt1 P1 O11 C11 56.0(10) . . . . ? O13 P1 O12 C18 71.2(6) . . . . ? O11 P1 O12 C18 -38.0(6) . . . . ? Pt1 P1 O12 C18 -166.7(5) . . . . ? O11 P1 O13 C115 65.2(9) . . . . ? O12 P1 O13 C115 -45.4(9) . . . . ? Pt1 P1 O13 C115 -164.4(8) . . . . ? P1 O11 C11 C12 -127.2(9) . . . . ? P1 O11 C11 C16 57.3(13) . . . . ? C16 C11 C12 C13 7.6(14) . . . . ? O11 C11 C12 C13 -167.9(8) . . . . ? C16 C11 C12 C128 -168.0(9) . . . . ? O11 C11 C12 C128 16.5(13) . . . . ? C11 C12 C13 C14 -1.4(16) . . . . ? C128 C12 C13 C14 174.4(10) . . . . ? C12 C13 C14 C15 -5.1(16) . . . . ? C12 C13 C14 C129 176.4(9) . . . . ? C13 C14 C15 C16 5.9(16) . . . . ? C129 C14 C15 C16 -175.5(9) . . . . ? C14 C15 C16 C11 -0.2(15) . . . . ? C14 C15 C16 C17 -176.9(9) . . . . ? C12 C11 C16 C15 -6.7(14) . . . . ? O11 C11 C16 C15 168.7(8) . . . . ? C12 C11 C16 C17 169.9(9) . . . . ? O11 C11 C16 C17 -14.8(14) . . . . ? C15 C16 C17 C19 -117.5(10) . . . . ? C11 C16 C17 C19 66.0(12) . . . . ? P1 O12 C18 C19 89.8(9) . . . . ? P1 O12 C18 C113 -93.5(9) . . . . ? C113 C18 C19 C110 0.4(14) . . . . ? O12 C18 C19 C110 176.8(8) . . . . ? C113 C18 C19 C17 178.4(9) . . . . ? O12 C18 C19 C17 -5.1(13) . . . . ? C16 C17 C19 C18 -91.6(11) . . . . ? C16 C17 C19 C110 86.4(12) . . . . ? C18 C19 C110 C111 -1.0(15) . . . . ? C17 C19 C110 C111 -179.1(9) . . . . ? C19 C110 C111 C112 1.1(15) . . . . ? C19 C110 C111 C133 -176.9(8) . . . . ? C110 C111 C112 C113 -0.4(14) . . . . ? C133 C111 C112 C113 177.7(8) . . . . ? C19 C18 C113 C112 0.3(14) . . . . ? O12 C18 C113 C112 -176.3(8) . . . . ? C19 C18 C113 C114 -176.9(8) . . . . ? O12 C18 C113 C114 6.6(12) . . . . ? C111 C112 C113 C18 -0.2(13) . . . . ? C111 C112 C113 C114 176.9(8) . . . . ? C18 C113 C114 C116 90.3(10) . . . . ? C112 C113 C114 C116 -86.7(10) . . . . ? P1 O13 C115 C116 51.4(12) . . . . ? P1 O13 C115 C120 -138.3(8) . . . . ? C120 C115 C116 C117 5.2(11) . . . . ? O13 C115 C116 C117 174.9(7) . . . . ? C120 C115 C116 C114 -173.3(7) . . . . ? O13 C115 C116 C114 -3.5(12) . . . . ? C113 C114 C116 C117 104.6(9) . . . . ? C113 C114 C116 C115 -76.9(10) . . . . ? C115 C116 C117 C118 -2.3(12) . . . . ? C114 C116 C117 C118 176.3(8) . . . . ? C116 C117 C118 C119 -1.0(13) . . . . ? C116 C117 C118 C137 -175.8(8) . . . . ? C117 C118 C119 C120 1.6(13) . . . . ? C137 C118 C119 C120 176.6(8) . . . . ? C118 C119 C120 C115 1.2(13) . . . . ? C118 C119 C120 C121 -175.8(8) . . . . ? C116 C115 C120 C119 -4.6(12) . . . . ? O13 C115 C120 C119 -175.0(7) . . . . ? C116 C115 C120 C121 172.3(7) . . . . ? O13 C115 C120 C121 1.9(11) . . . . ? C119 C120 C121 C123 -104.8(9) . . . . ? C115 C120 C121 C123 78.3(9) . . . . ? C145 O14 C122 C123 -68.5(9) . . . . ? C145 O14 C122 C127 103.9(8) . . . . ? C127 C122 C123 C124 2.9(13) . . . . ? O14 C122 C123 C124 174.1(7) . . . . ? C127 C122 C123 C121 171.7(8) . . . . ? O14 C122 C123 C121 -17.1(11) . . . . ? C120 C121 C123 C122 -97.7(9) . . . . ? C120 C121 C123 C124 70.7(10) . . . . ? C122 C123 C124 C125 -3.0(12) . . . . ? C121 C123 C124 C125 -172.1(8) . . . . ? C123 C124 C125 C126 3.7(13) . . . . ? C123 C124 C125 C141 -177.3(8) . . . . ? C124 C125 C126 C127 -4.1(14) . . . . ? C141 C125 C126 C127 177.0(9) . . . . ? C123 C122 C127 C126 -3.2(13) . . . . ? O14 C122 C127 C126 -174.5(7) . . . . ? C123 C122 C127 C128 -172.5(9) . . . . ? O14 C122 C127 C128 16.1(12) . . . . ? C125 C126 C127 C122 3.7(13) . . . . ? C125 C126 C127 C128 172.9(9) . . . . ? C122 C127 C128 C12 98.1(10) . . . . ? C126 C127 C128 C12 -70.4(12) . . . . ? C11 C12 C128 C127 -68.5(12) . . . . ? C13 C12 C128 C127 115.8(10) . . . . ? C13 C14 C129 C13C 129.9(14) . . . . ? C15 C14 C129 C13C -48.6(14) . . . . ? C13 C14 C129 C13B 8.4(15) . . . . ? C15 C14 C129 C13B -170.1(13) . . . . ? C13 C14 C129 C13D -132.9(16) . . . . ? C15 C14 C129 C13D 48.6(16) . . . . ? C13 C14 C129 C13E -11.6(16) . . . . ? C15 C14 C129 C13E 170.0(14) . . . . ? C13 C14 C129 C13F 107.7(16) . . . . ? C15 C14 C129 C13F -70.8(15) . . . . ? C13 C14 C129 C13A -110.9(13) . . . . ? C15 C14 C129 C13A 70.7(13) . . . . ? C110 C111 C133 C136 -121.4(10) . . . . ? C112 C111 C133 C136 60.6(9) . . . . ? C110 C111 C133 C134 -1.0(11) . . . . ? C112 C111 C133 C134 -179.0(8) . . . . ? C110 C111 C133 C135 118.7(10) . . . . ? C112 C111 C133 C135 -59.3(9) . . . . ? C117 C118 C137 C138 -1.0(13) . . . . ? C119 C118 C137 C138 -175.6(9) . . . . ? C117 C118 C137 C140 -123.9(10) . . . . ? C119 C118 C137 C140 61.5(11) . . . . ? C117 C118 C137 C139 118.4(10) . . . . ? C119 C118 C137 C139 -56.2(11) . . . . ? C124 C125 C141 C142 -179.9(9) . . . . ? C126 C125 C141 C142 -1.0(13) . . . . ? C124 C125 C141 C144 -56.2(11) . . . . ? C126 C125 C141 C144 122.7(10) . . . . ? C124 C125 C141 C143 61.0(11) . . . . ? C126 C125 C141 C143 -120.1(10) . . . . ? C122 O14 C145 C146 -87.5(8) . . . . ? C154 N1 C146 C147 -2.6(12) . . . . ? C154 N1 C146 C145 172.4(7) . . . . ? O14 C145 C146 N1 118.9(8) . . . . ? O14 C145 C146 C147 -65.8(9) . . . . ? N1 C146 C147 C148 0.5(13) . . . . ? C145 C146 C147 C148 -174.5(8) . . . . ? C146 C147 C148 C149 2.6(13) . . . . ? C147 C148 C149 C150 175.9(9) . . . . ? C147 C148 C149 C154 -3.4(13) . . . . ? C154 C149 C150 C151 0.9(15) . . . . ? C148 C149 C150 C151 -178.5(10) . . . . ? C149 C150 C151 C152 -3.8(17) . . . . ? C150 C151 C152 C153 4.0(18) . . . . ? C151 C152 C153 C154 -1.2(17) . . . . ? C146 N1 C154 C149 1.7(12) . . . . ? C146 N1 C154 C153 -178.2(8) . . . . ? C150 C149 C154 N1 -178.1(9) . . . . ? C148 C149 C154 N1 1.3(13) . . . . ? C150 C149 C154 C153 1.8(13) . . . . ? C148 C149 C154 C153 -178.8(8) . . . . ? C152 C153 C154 N1 178.2(9) . . . . ? C152 C153 C154 C149 -1.6(14) . . . . ? P1 Pt1 P2 O23 33.2(2) . . . . ? Cl2 Pt1 P2 O23 -151.3(2) . . . . ? P1 Pt1 P2 O21 154.3(2) . . . . ? Cl2 Pt1 P2 O21 -30.2(2) . . . . ? P1 Pt1 P2 O22 -84.9(2) . . . . ? Cl2 Pt1 P2 O22 90.6(2) . . . . ? O23 P2 O21 C21 -179.6(7) . . . . ? O22 P2 O21 C21 -67.9(8) . . . . ? Pt1 P2 O21 C21 54.8(8) . . . . ? O23 P2 O22 C28 72.1(6) . . . . ? O21 P2 O22 C28 -36.7(6) . . . . ? Pt1 P2 O22 C28 -166.4(5) . . . . ? O21 P2 O23 C215 63.5(9) . . . . ? O22 P2 O23 C215 -46.8(9) . . . . ? Pt1 P2 O23 C215 -166.0(8) . . . . ? P2 O21 C21 C26 56.9(11) . . . . ? P2 O21 C21 C22 -124.6(7) . . . . ? C26 C21 C22 C23 3.7(13) . . . . ? O21 C21 C22 C23 -174.7(7) . . . . ? C26 C21 C22 C228 -170.2(8) . . . . ? O21 C21 C22 C228 11.3(12) . . . . ? C21 C22 C23 C24 0.0(14) . . . . ? C228 C22 C23 C24 174.6(9) . . . . ? C22 C23 C24 C25 -3.9(14) . . . . ? C22 C23 C24 C229 -178.9(8) . . . . ? C23 C24 C25 C26 4.4(14) . . . . ? C229 C24 C25 C26 179.5(8) . . . . ? C22 C21 C26 C25 -3.3(13) . . . . ? O21 C21 C26 C25 175.0(8) . . . . ? C22 C21 C26 C27 171.7(8) . . . . ? O21 C21 C26 C27 -10.0(13) . . . . ? C24 C25 C26 C21 -0.9(14) . . . . ? C24 C25 C26 C27 -176.4(8) . . . . ? C21 C26 C27 C29 58.9(11) . . . . ? C25 C26 C27 C29 -125.9(8) . . . . ? P2 O22 C28 C213 -93.5(8) . . . . ? P2 O22 C28 C29 89.0(8) . . . . ? C213 C28 C29 C210 0.2(12) . . . . ? O22 C28 C29 C210 177.6(7) . . . . ? C213 C28 C29 C27 -179.6(7) . . . . ? O22 C28 C29 C27 -2.3(11) . . . . ? C26 C27 C29 C28 -90.8(9) . . . . ? C26 C27 C29 C210 89.4(10) . . . . ? C28 C29 C210 C211 -0.2(12) . . . . ? C27 C29 C210 C211 179.6(7) . . . . ? C29 C210 C211 C212 0.7(12) . . . . ? C29 C210 C211 C233 -178.7(7) . . . . ? C210 C211 C212 C213 -1.2(12) . . . . ? C233 C211 C212 C213 178.1(7) . . . . ? C29 C28 C213 C212 -0.7(12) . . . . ? O22 C28 C213 C212 -178.0(7) . . . . ? C29 C28 C213 C214 -176.0(7) . . . . ? O22 C28 C213 C214 6.7(11) . . . . ? C211 C212 C213 C28 1.2(12) . . . . ? C211 C212 C213 C214 176.4(7) . . . . ? C28 C213 C214 C216 89.8(9) . . . . ? C212 C213 C214 C216 -85.3(9) . . . . ? P2 O23 C215 C220 -136.8(8) . . . . ? P2 O23 C215 C216 50.8(13) . . . . ? C220 C215 C216 C217 6.4(11) . . . . ? O23 C215 C216 C217 178.5(7) . . . . ? C220 C215 C216 C214 -172.7(7) . . . . ? O23 C215 C216 C214 -0.6(12) . . . . ? C213 C214 C216 C217 101.2(8) . . . . ? C213 C214 C216 C215 -79.7(10) . . . . ? C215 C216 C217 C218 -1.1(12) . . . . ? C214 C216 C217 C218 178.0(7) . . . . ? C216 C217 C218 C219 -3.7(12) . . . . ? C216 C217 C218 C237 177.8(7) . . . . ? C217 C218 C219 C220 3.5(13) . . . . ? C237 C218 C219 C220 -178.0(8) . . . . ? C218 C219 C220 C215 1.5(13) . . . . ? C218 C219 C220 C221 -179.4(8) . . . . ? C216 C215 C220 C219 -6.6(12) . . . . ? O23 C215 C220 C219 -179.1(7) . . . . ? C216 C215 C220 C221 174.4(7) . . . . ? O23 C215 C220 C221 1.9(11) . . . . ? C219 C220 C221 C223 -99.3(9) . . . . ? C215 C220 C221 C223 79.7(10) . . . . ? C245 O24 C222 C223 -70.7(10) . . . . ? C245 O24 C222 C227 118.2(8) . . . . ? O24 C222 C223 C224 179.4(7) . . . . ? C227 C222 C223 C224 -9.7(12) . . . . ? O24 C222 C223 C221 -7.8(12) . . . . ? C227 C222 C223 C221 163.0(8) . . . . ? C220 C221 C223 C224 68.1(10) . . . . ? C220 C221 C223 C222 -104.6(9) . . . . ? C222 C223 C224 C225 5.7(13) . . . . ? C221 C223 C224 C225 -167.1(8) . . . . ? C223 C224 C225 C226 -0.4(13) . . . . ? C223 C224 C225 C241 -177.7(7) . . . . ? C224 C225 C226 C227 -0.9(13) . . . . ? C241 C225 C226 C227 176.4(7) . . . . ? C225 C226 C227 C222 -3.2(13) . . . . ? C225 C226 C227 C228 175.1(8) . . . . ? O24 C222 C227 C226 179.7(7) . . . . ? C223 C222 C227 C226 8.5(12) . . . . ? O24 C222 C227 C228 1.3(11) . . . . ? C223 C222 C227 C228 -169.9(8) . . . . ? C226 C227 C228 C22 -73.6(10) . . . . ? C222 C227 C228 C22 104.7(9) . . . . ? C23 C22 C228 C227 126.6(8) . . . . ? C21 C22 C228 C227 -59.3(11) . . . . ? C23 C24 C229 C23A 101.2(11) . . . . ? C25 C24 C229 C23A -73.6(11) . . . . ? C23 C24 C229 C23E -96.9(15) . . . . ? C25 C24 C229 C23E 88.4(14) . . . . ? C23 C24 C229 C23C -22.1(12) . . . . ? C25 C24 C229 C23C 163.1(10) . . . . ? C23 C24 C229 C23D 141.8(15) . . . . ? C25 C24 C229 C23D -32.9(14) . . . . ? C23 C24 C229 C23F 24.1(14) . . . . ? C25 C24 C229 C23F -150.7(12) . . . . ? C23 C24 C229 C23B -139.2(10) . . . . ? C25 C24 C229 C23B 46.0(11) . . . . ? C212 C211 C233 C235 -109.9(8) . . . . ? C210 C211 C233 C235 69.4(9) . . . . ? C212 C211 C233 C236 8.8(10) . . . . ? C210 C211 C233 C236 -171.9(7) . . . . ? C212 C211 C233 C234 130.8(8) . . . . ? C210 C211 C233 C234 -49.9(9) . . . . ? C219 C218 C237 C239 -117.5(9) . . . . ? C217 C218 C237 C239 60.9(10) . . . . ? C219 C218 C237 C238 123.5(9) . . . . ? C217 C218 C237 C238 -58.1(10) . . . . ? C219 C218 C237 C240 2.9(11) . . . . ? C217 C218 C237 C240 -178.7(8) . . . . ? C224 C225 C241 C24C -131.7(9) . . . . ? C226 C225 C241 C24C 51.1(10) . . . . ? C224 C225 C241 C24A 107.3(10) . . . . ? C226 C225 C241 C24A -69.8(10) . . . . ? C224 C225 C241 C24F -62.6(14) . . . . ? C226 C225 C241 C24F 120.2(14) . . . . ? C224 C225 C241 C24D 58.1(14) . . . . ? C226 C225 C241 C24D -119.1(14) . . . . ? C224 C225 C241 C24B -11.9(10) . . . . ? C226 C225 C241 C24B 170.9(9) . . . . ? C224 C225 C241 C24E 177.7(13) . . . . ? C226 C225 C241 C24E 0.5(14) . . . . ? C222 O24 C245 C246 -93.7(8) . . . . ? C254 N2 C246 C247 0.1(14) . . . . ? C254 N2 C246 C245 176.7(8) . . . . ? O24 C245 C246 N2 105.2(9) . . . . ? O24 C245 C246 C247 -78.0(11) . . . . ? N2 C246 C247 C248 0.8(18) . . . . ? C245 C246 C247 C248 -175.8(11) . . . . ? C246 C247 C248 C249 -0.1(19) . . . . ? C247 C248 C249 C254 -1.4(18) . . . . ? C247 C248 C249 C250 177.0(11) . . . . ? C254 C249 C250 C251 -3.9(16) . . . . ? C248 C249 C250 C251 177.8(11) . . . . ? C249 C250 C251 C252 1.3(18) . . . . ? C250 C251 C252 C253 -1(2) . . . . ? C251 C252 C253 C254 3(2) . . . . ? C246 N2 C254 C253 176.4(10) . . . . ? C246 N2 C254 C249 -1.6(14) . . . . ? C252 C253 C254 N2 176.5(12) . . . . ? C252 C253 C254 C249 -5.3(18) . . . . ? C248 C249 C254 N2 2.3(15) . . . . ? C250 C249 C254 N2 -176.1(9) . . . . ? C248 C249 C254 C253 -175.8(11) . . . . ? C250 C249 C254 C253 5.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.873 _refine_diff_density_max 3.826 _refine_diff_density_min -1.520 _refine_diff_density_rms 0.168 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.158 0.500 0.774 1998.1 386.7 _platon_squeeze_details ; ; #===END