# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Prof. Bernhard Breit' _publ_contact_author_address ;Institut fur Organische Chemie und Biochemie Universitat Freiburg Albertstr. 21 D-79104 Freiburg Germany ; _publ_contact_author_email BERNHARD.BREIT@CHEMIE.UNI-FREIBURG.DE _publ_contact_author_phone 0049-(0)761-203-6050 _publ_contact_author_fax 0049-(0)761-203-8715 loop_ _publ_author_name _publ_author_address 'Bernhard Breit' ;Institut fur Organische Chemie und Biochemie Universitat Freiburg Albertstr. 21 D-79104 Freiburg Germany ; 'Andy Ch. Laungani' ;Institut fur Organische Chemie und Biochemie Universitat Freiburg Albertstr. 21 D-79104 Freiburg Germany ; _publ_section_title ;Supramolecular PhanePhos-analogous ligands through hydrogen-bonding for asymmetric hydrogenation ; # Attachment 'X-ray_structure_CCDC-661682.cif' data_al680_0m _database_code_depnum_ccdc_archive 'CCDC 661682' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C148 H196 Cl4 N8 O34 P4 Pt2' _chemical_formula_weight 3286.99 _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.0141(3) _cell_length_b 25.7458(4) _cell_length_c 17.7497(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.0210(10) _cell_angle_gamma 90.00 _cell_volume 7775.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 1.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.506 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'APEX2 (Bruker, 2005)' _diffrn_detector_area_resol_mean 'frames each covering 0.5\% in\w' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 174221 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 27.54 _reflns_number_total 35741 _reflns_number_gt 33331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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. The crystal is a near perfect pseudo-merohedral twin with the twin law 1 0 0 0 -1 0 0 0 -1. The ratio of twin components is 0.51:0.49. The unit cell contains 9 MeCO2Et molecules that in some cases display considerable thermal motion. This is quite well described by the thermal parameters of the atoms and so no disordered positions were modelled. In all cases MeCO2Et molecules were restrained to chemically realistic geometries using RESI and DFIX commands. ; _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^)+(0.0415P)^2^+0.2783P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(3) _refine_ls_number_reflns 35741 _refine_ls_number_parameters 1836 _refine_ls_number_restraints 648 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.032 _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 0.488061(19) 0.559521(7) 0.309963(11) 0.02175(6) Uani 1 1 d U . . P1 P 0.54987(12) 0.63372(8) 0.34473(9) 0.0214(4) Uani 1 1 d U . . P2 P 0.38244(12) 0.56669(9) 0.38531(10) 0.0207(4) Uani 1 1 d U . . Cl1 Cl 0.59832(12) 0.54755(8) 0.23101(9) 0.0299(5) Uani 1 1 d U . . Cl2 Cl 0.44050(14) 0.48162(9) 0.26184(11) 0.0356(5) Uani 1 1 d U . . C1 C 0.5445(5) 0.6807(3) 0.2677(4) 0.0244(14) Uani 1 1 d U . . C2 C 0.5153(7) 0.6657(3) 0.1969(4) 0.0307(15) Uani 1 1 d U . . H2 H 0.4993 0.6316 0.1889 0.037 Uiso 1 1 calc R . . C3 C 0.5103(7) 0.7014(3) 0.1392(4) 0.0357(16) Uani 1 1 d U . . H3 H 0.4913 0.6911 0.0924 0.043 Uiso 1 1 calc R . . C4 C 0.5328(5) 0.7515(4) 0.1495(4) 0.040(2) Uani 1 1 d U . . H4 H 0.5274 0.7756 0.1108 0.048 Uiso 1 1 calc R . . C5 C 0.5656(6) 0.7671(4) 0.2218(5) 0.044(2) Uani 1 1 d U . . H5 H 0.5842 0.8007 0.2285 0.053 Uiso 1 1 calc R . . C6 C 0.5689(5) 0.7328(4) 0.2791(4) 0.0336(18) Uani 1 1 d U . . H6 H 0.5872 0.7433 0.3261 0.040 Uiso 1 1 calc R . . C7 C 0.6527(5) 0.6195(3) 0.3666(4) 0.0249(16) Uani 1 1 d U . . C8 C 0.6741(5) 0.5769(3) 0.4074(5) 0.0345(18) Uani 1 1 d U . . H8 H 0.6345 0.5537 0.4205 0.041 Uiso 1 1 calc R . . C9 C 0.7467(5) 0.5656(4) 0.4302(4) 0.0340(18) Uani 1 1 d U . . H9 H 0.7569 0.5361 0.4588 0.041 Uiso 1 1 calc R . . C10 C 0.8070(6) 0.5995(4) 0.4099(5) 0.042(2) Uani 1 1 d U . . H10 H 0.8585 0.5919 0.4236 0.050 Uiso 1 1 calc R . . C11 C 0.7912(7) 0.6440(4) 0.3697(5) 0.048(2) Uani 1 1 d U . . H11 H 0.8316 0.6663 0.3558 0.058 Uiso 1 1 calc R . . C12 C 0.7117(5) 0.6552(4) 0.3497(5) 0.039(2) Uani 1 1 d U . . H12 H 0.6994 0.6862 0.3256 0.047 Uiso 1 1 calc R . . C13 C 0.5209(5) 0.6705(3) 0.4279(3) 0.0184(15) Uani 1 1 d U . . C14 C 0.4631(4) 0.7098(3) 0.4226(3) 0.0184(13) Uani 1 1 d U . . H14 H 0.4416 0.7182 0.3760 0.022 Uiso 1 1 calc R . . C15 C 0.4383(5) 0.7359(3) 0.4872(4) 0.0263(18) Uani 1 1 d U . . H15 H 0.3966 0.7591 0.4833 0.032 Uiso 1 1 calc R . . C16 C 0.4726(4) 0.7288(3) 0.5550(4) 0.0212(15) Uani 1 1 d U . . H16 H 0.4567 0.7481 0.5967 0.025 Uiso 1 1 calc R . . C17 C 0.5335(5) 0.6913(3) 0.5614(3) 0.0219(14) Uani 1 1 d U . . C18 C 0.5556(4) 0.6636(3) 0.4979(4) 0.0204(15) Uani 1 1 d U . . H18 H 0.5956 0.6392 0.5024 0.024 Uiso 1 1 calc R . . C19 C 0.5823(5) 0.6851(3) 0.6316(3) 0.0197(14) Uani 1 1 d U . . C20 C 0.5992(5) 0.7031(3) 0.7649(4) 0.0231(15) Uani 1 1 d U . . H20 H 0.6530 0.7128 0.7508 0.028 Uiso 1 1 calc R . . C21 C 0.5692(5) 0.7449(3) 0.8178(4) 0.0243(17) Uani 1 1 d U . . H21 H 0.5132 0.7380 0.8255 0.029 Uiso 1 1 calc R . . C22 C 0.5751(6) 0.7996(4) 0.7815(4) 0.043(2) Uani 1 1 d U . . H22A H 0.6290 0.8073 0.7704 0.064 Uiso 1 1 calc R . . H22B H 0.5549 0.8251 0.8159 0.064 Uiso 1 1 calc R . . H22C H 0.5449 0.8003 0.7358 0.064 Uiso 1 1 calc R . . C23 C 0.6081(6) 0.7444(4) 0.8967(4) 0.032(2) Uani 1 1 d U . . H23A H 0.5989 0.7115 0.9203 0.048 Uiso 1 1 calc R . . H23B H 0.5858 0.7716 0.9270 0.048 Uiso 1 1 calc R . . H23C H 0.6636 0.7500 0.8916 0.048 Uiso 1 1 calc R . . C24 C 0.6034(5) 0.6487(3) 0.7989(4) 0.0196(15) Uani 1 1 d U . . C25 C 0.6779(5) 0.5919(3) 0.8801(4) 0.0255(16) Uani 1 1 d U . . H25 H 0.6732 0.5623 0.8457 0.031 Uiso 1 1 calc R . . C26 C 0.7582(5) 0.5911(4) 0.9175(4) 0.0273(16) Uani 1 1 d U . . H26A H 0.7975 0.6013 0.8816 0.041 Uiso 1 1 calc R . . H26B H 0.7693 0.5567 0.9353 0.041 Uiso 1 1 calc R . . H26C H 0.7585 0.6149 0.9592 0.041 Uiso 1 1 calc R . . C27 C 0.6147(6) 0.5873(3) 0.9436(4) 0.0255(15) Uani 1 1 d U . . C28 C 0.5551(5) 0.5231(3) 1.0224(4) 0.0411(19) Uani 1 1 d U . . H28A H 0.5769 0.5351 1.0691 0.062 Uiso 1 1 calc R . . H28B H 0.5484 0.4861 1.0243 0.062 Uiso 1 1 calc R . . H28C H 0.5051 0.5394 1.0141 0.062 Uiso 1 1 calc R . . N1 N 0.5526(4) 0.7027(3) 0.6955(3) 0.0218(12) Uani 1 1 d U . . N2 N 0.6684(4) 0.6393(3) 0.8389(3) 0.0262(14) Uani 1 1 d U . . O1 O 0.6506(3) 0.6656(2) 0.6263(3) 0.0266(12) Uani 1 1 d U . . O2 O 0.5500(3) 0.6169(2) 0.7904(3) 0.0226(10) Uani 1 1 d U . . O3 O 0.5783(4) 0.6209(2) 0.9690(3) 0.0316(13) Uani 1 1 d U . . O4 O 0.6066(4) 0.5360(3) 0.9628(3) 0.0375(15) Uani 1 1 d U . . C29 C 0.3182(5) 0.6213(3) 0.3676(4) 0.0224(16) Uani 1 1 d U . . C30 C 0.3351(6) 0.6588(4) 0.3143(4) 0.0269(17) Uani 1 1 d U . . H30 H 0.3785 0.6547 0.2830 0.032 Uiso 1 1 calc R . . C31 C 0.2880(6) 0.7023(4) 0.3069(4) 0.034(2) Uani 1 1 d U . . H31 H 0.3013 0.7278 0.2721 0.040 Uiso 1 1 calc R . . C32 C 0.2207(6) 0.7084(4) 0.3513(4) 0.038(2) Uani 1 1 d U . . H32 H 0.1888 0.7373 0.3441 0.046 Uiso 1 1 calc R . . C33 C 0.2011(5) 0.6727(3) 0.4047(4) 0.0306(16) Uani 1 1 d U . . H33 H 0.1571 0.6774 0.4351 0.037 Uiso 1 1 calc R . . C34 C 0.2500(5) 0.6274(3) 0.4130(4) 0.0279(17) Uani 1 1 d U . . H34 H 0.2370 0.6021 0.4481 0.033 Uiso 1 1 calc R . . C35 C 0.3126(6) 0.5129(3) 0.3809(4) 0.0281(17) Uani 1 1 d U . . C36 C 0.2547(6) 0.5131(4) 0.3269(5) 0.035(2) Uani 1 1 d U . . H36 H 0.2493 0.5418 0.2956 0.041 Uiso 1 1 calc R . . C37 C 0.2060(7) 0.4729(4) 0.3183(6) 0.049(2) Uani 1 1 d U . . H37 H 0.1684 0.4731 0.2803 0.059 Uiso 1 1 calc R . . C38 C 0.2122(8) 0.4305(5) 0.3671(7) 0.063(4) Uani 1 1 d U . . H38 H 0.1755 0.4038 0.3646 0.076 Uiso 1 1 calc R . . C39 C 0.2726(7) 0.4281(5) 0.4190(6) 0.064(4) Uani 1 1 d U . . H39 H 0.2804 0.3988 0.4485 0.077 Uiso 1 1 calc R . . C40 C 0.3205(7) 0.4707(4) 0.4251(6) 0.052(3) Uani 1 1 d U . . H40 H 0.3601 0.4704 0.4613 0.062 Uiso 1 1 calc R . . C41 C 0.4132(5) 0.5682(3) 0.4836(4) 0.0225(15) Uani 1 1 d U . . C42 C 0.4795(5) 0.5373(3) 0.5036(4) 0.0250(15) Uani 1 1 d U . . H42 H 0.5059 0.5180 0.4673 0.030 Uiso 1 1 calc R . . C43 C 0.5037(6) 0.5366(3) 0.5774(3) 0.0257(14) Uani 1 1 d U . . H43 H 0.5462 0.5157 0.5901 0.031 Uiso 1 1 calc R . . C44 C 0.4693(5) 0.5643(4) 0.6321(3) 0.0288(16) Uani 1 1 d U . . H44 H 0.4868 0.5616 0.6816 0.035 Uiso 1 1 calc R . . C45 C 0.4058(5) 0.5977(3) 0.6133(3) 0.0180(14) Uani 1 1 d U . . C46 C 0.3782(4) 0.5980(3) 0.5387(4) 0.0209(15) Uani 1 1 d U . . H46 H 0.3354 0.6188 0.5263 0.025 Uiso 1 1 calc R . . C47 C 0.3586(5) 0.6289(3) 0.6692(4) 0.0182(14) Uani 1 1 d U . . C48 C 0.3491(5) 0.6625(3) 0.7964(4) 0.0162(14) Uani 1 1 d U . . H48 H 0.2947 0.6501 0.7973 0.019 Uiso 1 1 calc R . . C49 C 0.3868(5) 0.6505(3) 0.8735(4) 0.0229(16) Uani 1 1 d U . . H49 H 0.4425 0.6600 0.8708 0.027 Uiso 1 1 calc R . . C50 C 0.3817(7) 0.5923(4) 0.8882(5) 0.046(3) Uani 1 1 d U . . H50A H 0.3281 0.5828 0.8980 0.069 Uiso 1 1 calc R . . H50B H 0.4136 0.5835 0.9310 0.069 Uiso 1 1 calc R . . H50C H 0.4003 0.5737 0.8448 0.069 Uiso 1 1 calc R . . C51 C 0.3498(6) 0.6812(4) 0.9380(4) 0.035(2) Uani 1 1 d U . . H51A H 0.3579 0.7177 0.9297 0.052 Uiso 1 1 calc R . . H51B H 0.3737 0.6712 0.9847 0.052 Uiso 1 1 calc R . . H51C H 0.2944 0.6741 0.9399 0.052 Uiso 1 1 calc R . . C52 C 0.3481(5) 0.7208(3) 0.7757(4) 0.0212(14) Uani 1 1 d U . . C53 C 0.2780(4) 0.8037(3) 0.7944(4) 0.0226(13) Uani 1 1 d U . . H53 H 0.2809 0.8116 0.7405 0.027 Uiso 1 1 calc R . . C54 C 0.1995(6) 0.8216(4) 0.8236(5) 0.032(2) Uani 1 1 d U . . H54A H 0.1583 0.8036 0.7975 0.048 Uiso 1 1 calc R . . H54B H 0.1942 0.8583 0.8153 0.048 Uiso 1 1 calc R . . H54C H 0.1959 0.8144 0.8765 0.048 Uiso 1 1 calc R . . C55 C 0.3444(5) 0.8314(3) 0.8338(4) 0.0230(14) Uani 1 1 d U . . C56 C 0.4154(7) 0.9095(4) 0.8432(6) 0.048(3) Uani 1 1 d U . . H56A H 0.4062 0.9116 0.8965 0.073 Uiso 1 1 calc R . . H56B H 0.4154 0.9438 0.8220 0.073 Uiso 1 1 calc R . . H56C H 0.4654 0.8933 0.8343 0.073 Uiso 1 1 calc R . . N3 N 0.3901(4) 0.6351(2) 0.7379(3) 0.0169(12) Uani 1 1 d U . . H3A H 0.4359 0.6224 0.7471 0.020 Uiso 1 1 calc R . . N4 N 0.2844(4) 0.7473(3) 0.8039(3) 0.0185(12) Uani 1 1 d U . . O5 O 0.2938(3) 0.6464(2) 0.6527(3) 0.0231(11) Uani 1 1 d U . . O6 O 0.3983(3) 0.7420(2) 0.7373(3) 0.0202(11) Uani 1 1 d U . . O7 O 0.3828(4) 0.8141(3) 0.8881(3) 0.0405(16) Uani 1 1 d U . . O8 O 0.3525(4) 0.8781(3) 0.8076(4) 0.0357(15) Uani 1 1 d U . . Pt2 Pt 0.987403(19) 0.804063(6) 1.176591(11) 0.01975(6) Uani 1 1 d U . . P3 P 1.04998(12) 0.73029(8) 1.14100(9) 0.0201(4) Uani 1 1 d U . . P4 P 0.88252(13) 0.79661(9) 1.10068(9) 0.0193(4) Uani 1 1 d U . . Cl3 Cl 1.09741(12) 0.81652(7) 1.25624(9) 0.0268(4) Uani 1 1 d U . . Cl4 Cl 0.93811(13) 0.88216(8) 1.22510(10) 0.0294(4) Uani 1 1 d U . . C57 C 1.0482(4) 0.6828(3) 1.2181(3) 0.0241(14) Uani 1 1 d U . . C58 C 1.0180(6) 0.6959(3) 1.2869(3) 0.0248(15) Uani 1 1 d U . . H58 H 1.0012 0.7298 1.2952 0.030 Uiso 1 1 calc R . . C59 C 1.0116(8) 0.6593(3) 1.3455(4) 0.0368(17) Uani 1 1 d U . . H59 H 0.9913 0.6690 1.3920 0.044 Uiso 1 1 calc R . . C60 C 1.0360(5) 0.6090(3) 1.3328(5) 0.040(2) Uani 1 1 d U . . H60 H 1.0313 0.5845 1.3711 0.048 Uiso 1 1 calc R . . C61 C 1.0665(7) 0.5945(4) 1.2658(5) 0.042(2) Uani 1 1 d U . . H61 H 1.0832 0.5605 1.2583 0.051 Uiso 1 1 calc R . . C62 C 1.0729(5) 0.6316(3) 1.2066(4) 0.0299(16) Uani 1 1 d U . . H62 H 1.0935 0.6218 1.1602 0.036 Uiso 1 1 calc R . . C63 C 1.1525(5) 0.7443(3) 1.1161(4) 0.0228(15) Uani 1 1 d U . . C64 C 1.2130(5) 0.7104(4) 1.1335(4) 0.0298(16) Uani 1 1 d U . . H64 H 1.2029 0.6799 1.1598 0.036 Uiso 1 1 calc R . . C65 C 1.2876(6) 0.7226(3) 1.1116(5) 0.0344(18) Uani 1 1 d U . . H65 H 1.3283 0.6998 1.1230 0.041 Uiso 1 1 calc R . . C66 C 1.3047(6) 0.7684(4) 1.0726(4) 0.0368(18) Uani 1 1 d U . . H66 H 1.3562 0.7757 1.0584 0.044 Uiso 1 1 calc R . . C67 C 1.2456(5) 0.8026(4) 1.0554(4) 0.0353(16) Uani 1 1 d U . . H67 H 1.2566 0.8326 1.0283 0.042 Uiso 1 1 calc R . . C68 C 1.1654(5) 0.7918(3) 1.0795(4) 0.0266(17) Uani 1 1 d U . . H68 H 1.1247 0.8153 1.0711 0.032 Uiso 1 1 calc R . . C69 C 1.0181(7) 0.6920(3) 1.0584(3) 0.0227(15) Uani 1 1 d U . . C70 C 0.9598(4) 0.6536(3) 1.0637(4) 0.0239(15) Uani 1 1 d U . . H70 H 0.9353 0.6478 1.1098 0.029 Uiso 1 1 calc R . . C71 C 0.9384(5) 0.6250(3) 1.0040(4) 0.0200(15) Uani 1 1 d U . . H71 H 0.9006 0.5992 1.0091 0.024 Uiso 1 1 calc R . . C72 C 0.9737(5) 0.6345(3) 0.9329(3) 0.0192(15) Uani 1 1 d U . . H72 H 0.9562 0.6168 0.8905 0.023 Uiso 1 1 calc R . . C73 C 1.0345(4) 0.6701(3) 0.9267(3) 0.0154(12) Uani 1 1 d U . . C74 C 1.0567(5) 0.6997(3) 0.9890(3) 0.0203(15) Uani 1 1 d U . . H74 H 1.0965 0.7243 0.9848 0.024 Uiso 1 1 calc R . . C75 C 1.0812(5) 0.6763(3) 0.8553(4) 0.0214(15) Uani 1 1 d U . . C76 C 1.0997(5) 0.6557(3) 0.7241(4) 0.0193(14) Uani 1 1 d U . . H76 H 1.1532 0.6448 0.7371 0.023 Uiso 1 1 calc R . . C77 C 1.0658(5) 0.6150(3) 0.6677(4) 0.0234(16) Uani 1 1 d U . . H77 H 1.0110 0.6240 0.6570 0.028 Uiso 1 1 calc R . . C78 C 1.0675(5) 0.5616(4) 0.7048(4) 0.0352(16) Uani 1 1 d U . . H78A H 1.0526 0.5357 0.6686 0.053 Uiso 1 1 calc R . . H78B H 1.0313 0.5610 0.7462 0.053 Uiso 1 1 calc R . . H78C H 1.1195 0.5545 0.7228 0.053 Uiso 1 1 calc R . . C79 C 1.1099(6) 0.6125(3) 0.5940(4) 0.0293(18) Uani 1 1 d U . . H79A H 1.1633 0.6022 0.6033 0.044 Uiso 1 1 calc R . . H79B H 1.1093 0.6461 0.5704 0.044 Uiso 1 1 calc R . . H79C H 1.0853 0.5876 0.5613 0.044 Uiso 1 1 calc R . . C80 C 1.1047(5) 0.7103(3) 0.6905(4) 0.0237(16) Uani 1 1 d U . . C81 C 1.1784(5) 0.7706(3) 0.6093(4) 0.0226(15) Uani 1 1 d U . . H81 H 1.1724 0.8001 0.6438 0.027 Uiso 1 1 calc R . . C82 C 1.2598(6) 0.7722(3) 0.5745(4) 0.0292(17) Uani 1 1 d U . . H82A H 1.2987 0.7727 0.6137 0.044 Uiso 1 1 calc R . . H82B H 1.2649 0.8028 0.5441 0.044 Uiso 1 1 calc R . . H82C H 1.2674 0.7420 0.5436 0.044 Uiso 1 1 calc R . . C83 C 1.1149(6) 0.7735(3) 0.5482(4) 0.0261(15) Uani 1 1 d U . . C84 C 1.0539(5) 0.8295(3) 0.4635(4) 0.0351(17) Uani 1 1 d U . . H84A H 1.0706 0.8077 0.4226 0.053 Uiso 1 1 calc R . . H84B H 1.0540 0.8651 0.4474 0.053 Uiso 1 1 calc R . . H84C H 1.0018 0.8198 0.4787 0.053 Uiso 1 1 calc R . . N5 N 1.0542(3) 0.6561(2) 0.7923(3) 0.0191(11) Uani 1 1 d U . . H5A H 1.0079 0.6427 0.7920 0.023 Uiso 1 1 calc R . . N6 N 1.1687(4) 0.7223(2) 0.6509(3) 0.0202(13) Uani 1 1 d U . . H6A H 1.2066 0.7002 0.6500 0.024 Uiso 1 1 calc R . . O9 O 1.1470(3) 0.6967(2) 0.8586(3) 0.0269(12) Uani 1 1 d U . . O10 O 1.0506(3) 0.7431(2) 0.6973(3) 0.0280(12) Uani 1 1 d U . . O11 O 1.0810(4) 0.7378(2) 0.5193(3) 0.0315(13) Uani 1 1 d U . . O12 O 1.1080(4) 0.8232(2) 0.5273(3) 0.0324(14) Uani 1 1 d U . . C85 C 0.8172(5) 0.7410(3) 1.1154(4) 0.0205(15) Uani 1 1 d U . . C86 C 0.8341(5) 0.7041(4) 1.1702(4) 0.0273(18) Uani 1 1 d U . . H86 H 0.8773 0.7083 1.2016 0.033 Uiso 1 1 calc R . . C87 C 0.7860(7) 0.6606(4) 1.1777(4) 0.037(2) Uani 1 1 d U . . H87 H 0.7973 0.6355 1.2138 0.045 Uiso 1 1 calc R . . C88 C 0.7219(5) 0.6551(4) 1.1319(5) 0.0393(19) Uani 1 1 d U . . H88 H 0.6909 0.6255 1.1355 0.047 Uiso 1 1 calc R . . C89 C 0.7031(5) 0.6931(3) 1.0805(4) 0.0322(17) Uani 1 1 d U . . H89 H 0.6584 0.6894 1.0509 0.039 Uiso 1 1 calc R . . C90 C 0.7494(5) 0.7362(3) 1.0725(3) 0.0219(15) Uani 1 1 d U . . H90 H 0.7354 0.7621 1.0385 0.026 Uiso 1 1 calc R . . C91 C 0.8128(5) 0.8507(3) 1.1047(4) 0.0243(15) Uani 1 1 d U . . C92 C 0.7564(5) 0.8495(4) 1.1624(5) 0.0327(18) Uani 1 1 d U . . H92 H 0.7548 0.8218 1.1960 0.039 Uiso 1 1 calc R . . C93 C 0.7011(6) 0.8913(4) 1.1688(5) 0.0361(18) Uani 1 1 d U . . H93 H 0.6634 0.8905 1.2068 0.043 Uiso 1 1 calc R . . C94 C 0.7029(7) 0.9319(5) 1.1204(6) 0.051(3) Uani 1 1 d U . . H94 H 0.6683 0.9596 1.1265 0.061 Uiso 1 1 calc R . . C95 C 0.7578(7) 0.9320(4) 1.0602(5) 0.0428(19) Uani 1 1 d U . . H95 H 0.7566 0.9584 1.0244 0.051 Uiso 1 1 calc R . . C96 C 0.8156(6) 0.8911(4) 1.0545(5) 0.042(2) Uani 1 1 d U . . H96 H 0.8540 0.8922 1.0173 0.050 Uiso 1 1 calc R . . C97 C 0.9143(4) 0.7942(3) 1.0032(3) 0.0201(15) Uani 1 1 d U . . C98 C 0.9767(5) 0.8276(3) 0.9816(4) 0.0246(15) Uani 1 1 d U . . H98 H 0.9995 0.8494 1.0171 0.030 Uiso 1 1 calc R . . C99 C 1.0038(5) 0.8282(2) 0.9083(3) 0.0232(14) Uani 1 1 d U . . H99 H 1.0457 0.8495 0.8951 0.028 Uiso 1 1 calc R . . C100 C 0.9684(4) 0.7966(3) 0.8538(4) 0.0198(14) Uani 1 1 d U . . H100 H 0.9875 0.7964 0.8047 0.024 Uiso 1 1 calc R . . C101 C 0.9040(5) 0.7652(3) 0.8730(4) 0.0189(14) Uani 1 1 d U . . C102 C 0.8794(5) 0.7631(3) 0.9479(3) 0.0178(14) Uani 1 1 d U . . H102 H 0.8391 0.7406 0.9614 0.021 Uiso 1 1 calc R . . C103 C 0.8599(5) 0.7332(3) 0.8183(3) 0.0200(16) Uani 1 1 d U . . C104 C 0.8453(5) 0.6982(3) 0.6926(4) 0.0236(16) Uani 1 1 d U . . H104 H 0.7912 0.7113 0.6920 0.028 Uiso 1 1 calc R . . C105 C 0.8840(6) 0.7085(3) 0.6132(4) 0.0300(18) Uani 1 1 d U . . H105 H 0.9393 0.6980 0.6162 0.036 Uiso 1 1 calc R . . C106 C 0.8817(7) 0.7681(4) 0.5983(4) 0.039(2) Uani 1 1 d U . . H10A H 0.8950 0.7749 0.5467 0.058 Uiso 1 1 calc R . . H10B H 0.9187 0.7852 0.6307 0.058 Uiso 1 1 calc R . . H10C H 0.8298 0.7810 0.6084 0.058 Uiso 1 1 calc R . . C107 C 0.8474(6) 0.6793(4) 0.5514(4) 0.040(2) Uani 1 1 d U . . H10D H 0.8504 0.6428 0.5619 0.060 Uiso 1 1 calc R . . H10E H 0.8744 0.6867 0.5052 0.060 Uiso 1 1 calc R . . H10F H 0.7933 0.6894 0.5467 0.060 Uiso 1 1 calc R . . C108 C 0.8440(4) 0.6407(3) 0.7127(3) 0.0172(13) Uani 1 1 d U . . C109 C 0.7766(5) 0.5589(4) 0.6997(4) 0.0269(14) Uani 1 1 d U . . H109 H 0.7805 0.5514 0.7537 0.032 Uiso 1 1 calc R . . C110 C 0.6962(6) 0.5403(3) 0.6700(4) 0.0272(18) Uani 1 1 d U . . H11A H 0.6550 0.5589 0.6954 0.041 Uiso 1 1 calc R . . H11B H 0.6906 0.5038 0.6794 0.041 Uiso 1 1 calc R . . H11C H 0.6930 0.5468 0.6168 0.041 Uiso 1 1 calc R . . C111 C 0.8419(5) 0.5292(3) 0.6571(4) 0.0258(15) Uani 1 1 d U . . C112 C 0.9102(5) 0.4495(4) 0.6590(5) 0.0361(19) Uani 1 1 d U . . H11D H 0.8995 0.4446 0.6064 0.054 Uiso 1 1 calc R . . H11E H 0.9090 0.4165 0.6842 0.054 Uiso 1 1 calc R . . H11F H 0.9611 0.4649 0.6650 0.054 Uiso 1 1 calc R . . N7 N 0.8905(4) 0.7272(3) 0.7486(3) 0.0195(12) Uani 1 1 d U . . N8 N 0.7840(5) 0.6139(3) 0.6878(3) 0.0263(14) Uani 1 1 d U . . H8A H 0.7476 0.6299 0.6634 0.032 Uiso 1 1 calc R . . O13 O 0.7935(3) 0.7146(2) 0.8349(3) 0.0284(13) Uani 1 1 d U . . O14 O 0.8967(4) 0.6195(2) 0.7504(3) 0.0246(12) Uani 1 1 d U . . O15 O 0.8772(4) 0.5450(3) 0.6062(3) 0.0394(17) Uani 1 1 d U . . O16 O 0.8523(5) 0.4826(3) 0.6907(3) 0.0393(17) Uani 1 1 d U . . O200_1 O 0.4204(5) 0.4066(3) 0.5499(3) 0.0720(19) Uani 1 1 d DU . . O201_1 O 0.3933(3) 0.4360(2) 0.6641(3) 0.0524(14) Uani 1 1 d DU . . C200_1 C 0.5084(5) 0.3818(4) 0.6481(6) 0.064(3) Uani 1 1 d DU . . H20A_1 H 0.4963 0.3679 0.6969 0.096 Uiso 1 1 calc R . . H20B_1 H 0.5501 0.4068 0.6527 0.096 Uiso 1 1 calc R . . H20C_1 H 0.5247 0.3542 0.6153 0.096 Uiso 1 1 calc R . . C201_1 C 0.4367(4) 0.4078(3) 0.6161(3) 0.0482(19) Uani 1 1 d DU . . C202_1 C 0.3264(4) 0.4640(3) 0.6333(6) 0.064(3) Uani 1 1 d DU . . H20D_1 H 0.2895 0.4392 0.6123 0.077 Uiso 1 1 calc R . . H20E_1 H 0.3443 0.4862 0.5925 0.077 Uiso 1 1 calc R . . C203_1 C 0.2844(8) 0.4970(5) 0.6910(7) 0.090(5) Uani 1 1 d DU . . H20F_1 H 0.2509 0.4754 0.7212 0.135 Uiso 1 1 calc R . . H20G_1 H 0.2532 0.5227 0.6657 0.135 Uiso 1 1 calc R . . H20H_1 H 0.3223 0.5139 0.7227 0.135 Uiso 1 1 calc R . . O200_2 O 0.5963(5) 0.4103(3) 0.8947(4) 0.084(2) Uani 1 1 d DU . . O201_2 O 0.6399(4) 0.4341(3) 0.7817(3) 0.0687(18) Uani 1 1 d DU . . C200_2 C 0.5207(6) 0.4725(3) 0.8250(6) 0.062(3) Uani 1 1 d DU . . H20A_2 H 0.4851 0.4711 0.8669 0.093 Uiso 1 1 calc R . . H20B_2 H 0.4935 0.4628 0.7797 0.093 Uiso 1 1 calc R . . H20C_2 H 0.5408 0.5071 0.8199 0.093 Uiso 1 1 calc R . . C201_2 C 0.5878(5) 0.4354(4) 0.8384(4) 0.064(2) Uani 1 1 d DU . . C202_2 C 0.7075(5) 0.3992(4) 0.7872(6) 0.065(3) Uani 1 1 d DU . . H20D_2 H 0.7229 0.3951 0.8395 0.078 Uiso 1 1 calc R . . H20E_2 H 0.7517 0.4136 0.7597 0.078 Uiso 1 1 calc R . . C203_2 C 0.6852(9) 0.3474(5) 0.7546(8) 0.100(5) Uani 1 1 d DU . . H20F_2 H 0.6436 0.3324 0.7840 0.151 Uiso 1 1 calc R . . H20G_2 H 0.7299 0.3247 0.7553 0.151 Uiso 1 1 calc R . . H20H_2 H 0.6676 0.3520 0.7036 0.151 Uiso 1 1 calc R . . O200_3 O 0.1273(5) 0.9046(3) -0.0152(4) 0.056(2) Uani 1 1 d DU . . O201_3 O 0.1709(5) 0.9564(3) 0.0744(4) 0.080(3) Uani 1 1 d DU . . C200_3 C 0.2527(5) 0.9471(5) -0.0292(6) 0.058(3) Uani 1 1 d DU . . H20A_3 H 0.2589 0.9269 -0.0744 0.086 Uiso 1 1 calc R . . H20B_3 H 0.2941 0.9386 0.0055 0.086 Uiso 1 1 calc R . . H20C_3 H 0.2550 0.9833 -0.0414 0.086 Uiso 1 1 calc R . . C201_3 C 0.1748(5) 0.9349(3) 0.0061(4) 0.040(2) Uani 1 1 d DU . . C202_3 C 0.1020(5) 0.9455(4) 0.1202(5) 0.059(3) Uani 1 1 d DU . . H20D_3 H 0.1180 0.9433 0.1726 0.070 Uiso 1 1 calc R . . H20E_3 H 0.0809 0.9120 0.1058 0.070 Uiso 1 1 calc R . . C203_3 C 0.0383(8) 0.9854(5) 0.1134(9) 0.135(8) Uani 1 1 d DU . . H20F_3 H 0.0451 1.0115 0.1515 0.202 Uiso 1 1 calc R . . H20G_3 H -0.0120 0.9690 0.1197 0.202 Uiso 1 1 calc R . . H20H_3 H 0.0408 1.0013 0.0645 0.202 Uiso 1 1 calc R . . O200_4 O 0.1912(4) 0.5447(4) 0.1376(3) 0.071(3) Uani 1 1 d DU . . O201_4 O 0.2336(3) 0.5625(2) 0.0227(2) 0.0425(11) Uani 1 1 d DU . . C200_4 C 0.3296(4) 0.5650(4) 0.1187(4) 0.054(2) Uani 1 1 d DU . . H20A_4 H 0.3328 0.5719 0.1718 0.081 Uiso 1 1 calc R . . H20B_4 H 0.3505 0.5940 0.0912 0.081 Uiso 1 1 calc R . . H20C_4 H 0.3593 0.5343 0.1071 0.081 Uiso 1 1 calc R . . C201_4 C 0.2453(3) 0.5568(3) 0.0970(3) 0.0395(16) Uani 1 1 d DU . . C202_4 C 0.1535(3) 0.5573(5) -0.0046(3) 0.0446(19) Uani 1 1 d DU . . H20D_4 H 0.1210 0.5853 0.0143 0.054 Uiso 1 1 calc R . . H20E_4 H 0.1311 0.5245 0.0116 0.054 Uiso 1 1 calc R . . C203_4 C 0.1587(4) 0.5594(3) -0.0893(3) 0.0433(16) Uani 1 1 d DU . . H20F_4 H 0.1891 0.5892 -0.1041 0.065 Uiso 1 1 calc R . . H20G_4 H 0.1068 0.5621 -0.1102 0.065 Uiso 1 1 calc R . . H20H_4 H 0.1835 0.5284 -0.1077 0.065 Uiso 1 1 calc R . . O200_5 O 0.4002(5) 0.4527(2) 0.0545(5) 0.085(2) Uani 1 1 d DU . . O201_5 O 0.3410(4) 0.3799(2) 0.0864(4) 0.0651(17) Uani 1 1 d DU . . C200_5 C 0.4500(9) 0.3720(5) 0.0011(7) 0.100(5) Uani 1 1 d DU . . H20A_5 H 0.4859 0.3935 -0.0265 0.150 Uiso 1 1 calc R . . H20B_5 H 0.4186 0.3522 -0.0334 0.150 Uiso 1 1 calc R . . H20C_5 H 0.4790 0.3489 0.0332 0.150 Uiso 1 1 calc R . . C201_5 C 0.3969(6) 0.4060(2) 0.0489(6) 0.072(3) Uani 1 1 d DU . . C202_5 C 0.2909(5) 0.4089(3) 0.1384(5) 0.064(2) Uani 1 1 d DU . . H20D_5 H 0.2720 0.4401 0.1137 0.076 Uiso 1 1 calc R . . H20E_5 H 0.3215 0.4193 0.1820 0.076 Uiso 1 1 calc R . . C203_5 C 0.2212(6) 0.3762(4) 0.1638(6) 0.058(3) Uani 1 1 d DU . . H20F_5 H 0.2189 0.3449 0.1344 0.087 Uiso 1 1 calc R . . H20G_5 H 0.1735 0.3955 0.1570 0.087 Uiso 1 1 calc R . . H20H_5 H 0.2272 0.3674 0.2161 0.087 Uiso 1 1 calc R . . O200_6 O 0.6438(5) 0.4668(3) 0.5054(4) 0.065(2) Uani 1 1 d DU . . O201_6 O 0.6388(5) 0.3923(3) 0.4488(5) 0.086(3) Uani 1 1 d DU . . C200_6 C 0.7387(8) 0.4030(5) 0.5393(7) 0.098(6) Uani 1 1 d DU . . H20A_6 H 0.7708 0.4301 0.5599 0.148 Uiso 1 1 calc R . . H20B_6 H 0.7702 0.3811 0.5076 0.148 Uiso 1 1 calc R . . H20C_6 H 0.7169 0.3826 0.5796 0.148 Uiso 1 1 calc R . . C201_6 C 0.6737(5) 0.4263(3) 0.4941(5) 0.049(3) Uani 1 1 d DU . . C202_6 C 0.5711(5) 0.4122(3) 0.4081(6) 0.059(3) Uani 1 1 d DU . . H20D_6 H 0.5873 0.4374 0.3706 0.071 Uiso 1 1 calc R . . H20E_6 H 0.5343 0.4285 0.4424 0.071 Uiso 1 1 calc R . . C203_6 C 0.5347(8) 0.3655(4) 0.3712(7) 0.078(3) Uani 1 1 d DU . . H20F_6 H 0.5750 0.3453 0.3473 0.117 Uiso 1 1 calc R . . H20G_6 H 0.4973 0.3767 0.3342 0.117 Uiso 1 1 calc R . . H20H_6 H 0.5086 0.3448 0.4086 0.117 Uiso 1 1 calc R . . O200_7 O 0.6806(6) 0.8155(4) 0.3553(4) 0.081(3) Uani 1 1 d DU . . O201_7 O 0.7692(3) 0.8204(3) 0.4469(4) 0.080(2) Uani 1 1 d DU . . C200_7 C 0.6514(7) 0.7925(5) 0.4870(5) 0.079(4) Uani 1 1 d DU . . H20A_7 H 0.6590 0.8166 0.5276 0.119 Uiso 1 1 calc R . . H20B_7 H 0.6687 0.7586 0.5024 0.119 Uiso 1 1 calc R . . H20C_7 H 0.5967 0.7912 0.4739 0.119 Uiso 1 1 calc R . . C201_7 C 0.6982(4) 0.8097(4) 0.4198(4) 0.068(3) Uani 1 1 d DU . . C202_7 C 0.8228(7) 0.8320(5) 0.3847(6) 0.110(5) Uani 1 1 d DU . . H20D_7 H 0.8681 0.8512 0.4030 0.132 Uiso 1 1 calc R . . H20E_7 H 0.7964 0.8529 0.3469 0.132 Uiso 1 1 calc R . . C203_7 C 0.8485(9) 0.7811(5) 0.3512(7) 0.108(5) Uani 1 1 d DU . . H20F_7 H 0.8651 0.7582 0.3908 0.162 Uiso 1 1 calc R . . H20G_7 H 0.8913 0.7869 0.3171 0.162 Uiso 1 1 calc R . . H20H_7 H 0.8053 0.7657 0.3245 0.162 Uiso 1 1 calc R . . O200_8 O -0.0100(14) 0.4871(4) 0.3590(17) 0.394(19) Uani 1 1 d DU . . O201_8 O 0.0356(6) 0.4340(4) 0.4376(6) 0.128(4) Uani 1 1 d DU . . C200_8 C -0.0200(8) 0.3934(4) 0.3279(7) 0.088(4) Uani 1 1 d DU . . H20A_8 H -0.0627 0.3992 0.2936 0.132 Uiso 1 1 calc R . . H20B_8 H -0.0328 0.3652 0.3610 0.132 Uiso 1 1 calc R . . H20C_8 H 0.0266 0.3850 0.2999 0.132 Uiso 1 1 calc R . . C201_8 C -0.0059(10) 0.4416(4) 0.3732(6) 0.108(4) Uani 1 1 d DU . . C202_8 C 0.0615(8) 0.4796(4) 0.4799(7) 0.094(4) Uani 1 1 d DU . . H20D_8 H 0.0171 0.4990 0.4995 0.113 Uiso 1 1 calc R . . H20E_8 H 0.0933 0.5024 0.4488 0.113 Uiso 1 1 calc R . . C203_8 C 0.1102(7) 0.4556(7) 0.5437(8) 0.126(7) Uani 1 1 d DU . . H20F_8 H 0.0807 0.4281 0.5670 0.189 Uiso 1 1 calc R . . H20G_8 H 0.1222 0.4817 0.5805 0.189 Uiso 1 1 calc R . . H20H_8 H 0.1582 0.4418 0.5236 0.189 Uiso 1 1 calc R . . O200_9 O 0.8651(6) 0.5385(4) 0.1251(7) 0.153(5) Uani 1 1 d DU . . O201_9 O 0.8683(3) 0.4783(2) 0.2123(3) 0.0602(16) Uani 1 1 d DU . . C200_9 C 0.9824(6) 0.4868(5) 0.1362(7) 0.100(4) Uani 1 1 d DU . . H20A_9 H 0.9896 0.4883 0.0826 0.150 Uiso 1 1 calc R . . H20B_9 H 0.9897 0.4517 0.1532 0.150 Uiso 1 1 calc R . . H20C_9 H 1.0200 0.5090 0.1604 0.150 Uiso 1 1 calc R . . C201_9 C 0.9009(5) 0.5044(3) 0.1555(5) 0.077(3) Uani 1 1 d DU . . C202_9 C 0.7924(5) 0.4942(5) 0.2403(6) 0.080(4) Uani 1 1 d DU . . H20D_9 H 0.7534 0.4920 0.2005 0.096 Uiso 1 1 calc R . . H20E_9 H 0.7947 0.5298 0.2579 0.096 Uiso 1 1 calc R . . C203_9 C 0.7702(7) 0.4583(4) 0.3045(6) 0.075(3) Uani 1 1 d DU . . H20F_9 H 0.7624 0.4238 0.2855 0.113 Uiso 1 1 calc R . . H20G_9 H 0.7226 0.4704 0.3276 0.113 Uiso 1 1 calc R . . H20H_9 H 0.8117 0.4580 0.3413 0.113 Uiso 1 1 calc R . . H1N H 0.4988 0.7161 0.6984 0.090 Uiso 1 1 d R . . H2N H 0.7006 0.6655 0.8431 0.090 Uiso 1 1 d R . . H4N H 0.2436 0.7358 0.8295 0.090 Uiso 1 1 d R . . H7N H 0.9356 0.7318 0.7421 0.090 Uiso 1 1 d 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 0.01443(14) 0.02910(14) 0.02172(9) -0.00440(9) -0.00092(11) 0.0022(3) P1 0.0137(9) 0.0287(10) 0.0220(8) -0.0029(6) 0.0013(6) 0.0011(8) P2 0.0132(10) 0.0252(11) 0.0237(8) 0.0001(7) -0.0034(6) 0.0007(9) Cl1 0.0223(10) 0.0399(13) 0.0275(8) -0.0080(7) 0.0045(7) 0.0028(9) Cl2 0.0248(12) 0.0373(12) 0.0446(10) -0.0167(8) -0.0002(8) -0.0024(10) C1 0.0234(17) 0.0252(16) 0.0245(16) 0.0000(9) 0.0015(10) 0.0011(10) C2 0.017(4) 0.044(4) 0.031(3) -0.005(3) 0.000(4) 0.001(5) C3 0.018(4) 0.056(4) 0.033(3) 0.007(3) 0.013(4) 0.001(5) C4 0.026(6) 0.056(4) 0.038(4) 0.011(3) 0.010(3) 0.005(4) C5 0.027(6) 0.040(5) 0.067(5) 0.010(4) 0.008(4) 0.001(4) C6 0.021(4) 0.046(4) 0.034(4) 0.000(3) 0.010(3) -0.009(4) C7 0.012(3) 0.040(4) 0.023(4) -0.003(3) 0.004(3) 0.008(3) C8 0.014(4) 0.031(4) 0.059(5) -0.010(3) 0.010(3) 0.001(3) C9 0.024(4) 0.047(5) 0.031(3) -0.006(3) -0.008(3) 0.013(4) C10 0.016(4) 0.066(6) 0.043(4) -0.016(4) -0.004(3) 0.002(4) C11 0.046(2) 0.050(2) 0.049(2) -0.0008(10) -0.0005(10) -0.0006(10) C12 0.012(4) 0.065(6) 0.041(4) -0.001(4) -0.003(3) -0.006(4) C13 0.008(4) 0.025(3) 0.022(3) 0.001(2) 0.000(3) 0.000(3) C14 0.0176(16) 0.0190(16) 0.0187(15) 0.0002(9) -0.0012(9) -0.0001(10) C15 0.014(4) 0.038(5) 0.027(3) 0.012(3) 0.008(3) 0.007(3) C16 0.006(4) 0.029(4) 0.028(3) -0.003(3) 0.003(2) -0.006(3) C17 0.0207(17) 0.0224(17) 0.0225(16) -0.0002(9) -0.0005(9) 0.0000(10) C18 0.006(4) 0.030(4) 0.025(3) 0.003(2) 0.000(2) 0.000(3) C19 0.019(4) 0.019(4) 0.021(3) 0.007(2) 0.001(2) -0.005(3) C20 0.012(4) 0.034(4) 0.023(3) -0.003(3) -0.004(3) -0.003(3) C21 0.018(4) 0.030(4) 0.024(3) -0.002(3) -0.003(3) -0.004(3) C22 0.055(6) 0.030(4) 0.042(4) -0.008(3) -0.011(4) -0.004(5) C23 0.035(5) 0.031(4) 0.030(3) -0.013(3) -0.009(3) -0.003(4) C24 0.007(4) 0.030(4) 0.022(3) 0.000(3) -0.004(3) 0.004(3) C25 0.018(3) 0.033(4) 0.026(3) 0.006(3) -0.006(2) -0.001(3) C26 0.012(3) 0.039(4) 0.031(3) 0.010(3) -0.006(3) -0.001(3) C27 0.0246(18) 0.0273(17) 0.0247(17) 0.0003(9) -0.0015(10) -0.0006(10) C28 0.041(2) 0.041(2) 0.042(2) 0.0032(10) 0.0001(10) 0.0002(10) N1 0.0209(15) 0.0229(15) 0.0217(14) 0.0004(9) -0.0005(9) 0.0006(10) N2 0.009(3) 0.043(3) 0.026(3) 0.007(2) -0.007(2) -0.007(2) O1 0.016(3) 0.039(3) 0.025(2) -0.002(2) -0.0008(19) 0.010(2) O2 0.010(2) 0.027(3) 0.030(2) 0.001(2) -0.003(2) -0.002(2) O3 0.033(4) 0.041(3) 0.021(2) -0.003(2) 0.001(2) -0.006(3) O4 0.032(4) 0.044(3) 0.037(3) 0.015(2) -0.004(2) 0.003(3) C29 0.021(4) 0.024(4) 0.021(4) -0.004(3) -0.009(3) 0.004(3) C30 0.020(5) 0.033(4) 0.028(4) -0.008(3) -0.005(3) 0.000(3) C31 0.030(5) 0.039(5) 0.032(4) 0.012(3) -0.007(3) 0.000(4) C32 0.040(5) 0.037(4) 0.038(4) -0.006(3) -0.013(3) 0.018(4) C33 0.0291(18) 0.0315(18) 0.0312(18) -0.0016(10) -0.0010(10) 0.0016(10) C34 0.019(4) 0.034(4) 0.030(4) 0.003(3) -0.010(3) 0.003(3) C35 0.032(5) 0.021(3) 0.031(4) 0.000(3) -0.002(3) -0.002(3) C36 0.028(5) 0.027(4) 0.048(5) -0.005(3) -0.016(4) -0.001(3) C37 0.048(2) 0.049(2) 0.050(2) 0.0003(10) -0.0018(10) -0.0009(10) C38 0.041(7) 0.044(6) 0.105(9) 0.017(5) -0.027(6) -0.026(5) C39 0.064(7) 0.047(6) 0.082(7) 0.033(5) -0.031(6) -0.031(5) C40 0.046(6) 0.042(5) 0.068(6) 0.014(4) -0.036(5) -0.013(4) C41 0.021(4) 0.018(4) 0.029(3) 0.001(2) 0.000(2) 0.004(3) C42 0.014(3) 0.034(4) 0.027(3) -0.007(3) -0.005(3) 0.001(3) C43 0.0245(17) 0.0256(16) 0.0270(16) -0.0006(9) -0.0002(10) 0.0011(10) C44 0.027(4) 0.033(4) 0.027(3) -0.007(3) -0.008(2) 0.003(4) C45 0.012(4) 0.020(4) 0.022(3) 0.001(2) 0.002(2) -0.003(3) C46 0.005(4) 0.031(4) 0.027(3) 0.003(3) -0.003(2) 0.002(3) C47 0.011(4) 0.020(4) 0.023(3) 0.004(2) -0.006(2) -0.007(3) C48 0.012(4) 0.017(3) 0.020(3) 0.000(2) -0.001(3) 0.001(3) C49 0.016(4) 0.034(4) 0.019(3) 0.001(3) -0.003(3) 0.005(3) C50 0.060(8) 0.044(5) 0.033(4) 0.009(3) -0.009(4) 0.019(5) C51 0.044(6) 0.036(4) 0.024(3) 0.003(3) 0.012(3) 0.007(4) C52 0.0204(17) 0.0219(16) 0.0213(16) 0.0003(9) 0.0010(10) 0.0005(10) C53 0.014(3) 0.018(3) 0.036(3) -0.008(3) 0.003(2) 0.002(3) C54 0.019(4) 0.030(5) 0.048(4) -0.010(3) 0.006(3) 0.001(3) C55 0.019(4) 0.019(3) 0.030(3) -0.005(3) 0.011(3) 0.000(3) C56 0.048(7) 0.020(4) 0.077(6) -0.011(4) 0.016(5) -0.011(4) N3 0.0160(15) 0.0178(14) 0.0170(13) 0.0002(9) -0.0002(9) 0.0001(10) N4 0.007(2) 0.023(2) 0.025(3) -0.001(2) 0.005(2) -0.0030(18) O5 0.010(3) 0.027(3) 0.032(3) -0.001(2) -0.0007(19) 0.006(2) O6 0.006(3) 0.025(3) 0.030(2) 0.0077(19) 0.0024(18) -0.001(2) O7 0.038(4) 0.044(4) 0.039(3) 0.005(2) -0.013(2) -0.014(3) O8 0.019(4) 0.026(3) 0.062(4) 0.004(2) 0.001(3) -0.008(3) Pt2 0.01367(13) 0.02615(13) 0.01944(9) -0.00287(9) 0.00046(11) -0.0015(3) P3 0.0143(9) 0.0266(9) 0.0195(8) 0.0001(6) -0.0005(6) 0.0001(8) P4 0.0147(10) 0.0269(11) 0.0163(7) -0.0024(7) -0.0001(6) -0.0004(9) Cl3 0.0210(10) 0.0343(12) 0.0251(7) -0.0060(6) -0.0056(6) 0.0000(8) Cl4 0.0219(11) 0.0286(10) 0.0377(9) -0.0091(7) 0.0003(7) -0.0010(9) C57 0.014(3) 0.037(3) 0.021(3) 0.006(2) -0.004(2) -0.002(2) C58 0.016(4) 0.037(4) 0.021(3) 0.001(3) -0.007(3) 0.002(4) C59 0.026(4) 0.057(4) 0.027(3) 0.005(3) 0.009(4) -0.008(6) C60 0.036(6) 0.045(4) 0.039(4) 0.026(3) -0.005(3) -0.009(4) C61 0.045(7) 0.031(4) 0.051(4) 0.005(3) -0.019(4) 0.001(4) C62 0.021(4) 0.031(3) 0.037(4) 0.007(3) -0.011(3) -0.009(3) C63 0.021(3) 0.031(4) 0.016(3) -0.011(3) 0.004(3) 0.000(3) C64 0.024(4) 0.032(4) 0.033(4) -0.003(3) 0.002(3) -0.001(3) C65 0.0321(19) 0.0356(19) 0.0355(19) -0.0008(10) -0.0001(10) 0.0013(10) C66 0.018(4) 0.045(5) 0.047(4) -0.010(3) 0.010(3) -0.009(3) C67 0.031(4) 0.036(4) 0.039(4) -0.008(4) 0.004(3) 0.000(4) C68 0.014(3) 0.040(4) 0.026(3) -0.004(3) 0.002(3) 0.000(3) C69 0.020(4) 0.026(3) 0.022(3) -0.004(2) -0.005(3) 0.001(4) C70 0.012(3) 0.041(4) 0.018(3) 0.008(2) -0.003(2) -0.003(2) C71 0.014(4) 0.023(4) 0.023(3) -0.001(2) 0.004(3) -0.003(3) C72 0.020(4) 0.025(4) 0.013(2) 0.003(2) 0.000(2) -0.006(3) C73 0.009(3) 0.017(3) 0.020(3) 0.001(2) 0.003(2) 0.0051(19) C74 0.020(4) 0.016(3) 0.025(3) 0.002(2) 0.002(3) -0.002(3) C75 0.008(3) 0.027(4) 0.029(3) 0.000(3) 0.009(3) -0.002(3) C76 0.005(3) 0.028(3) 0.024(3) 0.001(2) 0.000(2) -0.001(3) C77 0.015(4) 0.030(4) 0.026(3) -0.005(3) -0.001(3) -0.001(3) C78 0.028(4) 0.039(4) 0.038(4) 0.004(3) 0.015(3) 0.000(4) C79 0.030(5) 0.026(4) 0.032(3) 0.000(3) 0.004(3) -0.009(3) C80 0.014(4) 0.030(4) 0.027(3) 0.001(3) 0.003(3) 0.005(3) C81 0.0219(17) 0.0226(17) 0.0232(17) -0.0002(9) 0.0006(10) 0.0005(10) C82 0.0286(19) 0.0296(19) 0.0294(18) 0.0011(10) 0.0017(10) -0.0006(10) C83 0.0253(17) 0.0276(17) 0.0254(17) 0.0015(9) 0.0024(10) 0.0010(10) C84 0.0357(19) 0.0343(19) 0.0352(19) 0.0031(10) -0.0009(10) 0.0009(10) N5 0.007(2) 0.026(3) 0.024(2) 0.004(2) 0.007(2) -0.0017(19) N6 0.0191(15) 0.0210(15) 0.0206(14) 0.0002(9) 0.0013(9) 0.0011(10) O9 0.011(3) 0.040(3) 0.030(2) -0.003(2) 0.0022(19) -0.004(2) O10 0.018(3) 0.036(3) 0.031(2) 0.001(2) 0.006(2) 0.004(2) O11 0.023(3) 0.037(3) 0.034(3) 0.003(2) -0.003(2) 0.003(2) O12 0.028(4) 0.030(3) 0.039(3) 0.014(2) -0.001(2) 0.004(3) C85 0.011(4) 0.028(4) 0.022(3) -0.002(3) 0.002(3) 0.002(3) C86 0.012(4) 0.042(5) 0.028(4) 0.004(3) 0.002(3) -0.005(3) C87 0.036(6) 0.035(5) 0.042(4) 0.003(3) 0.007(3) -0.003(4) C88 0.013(4) 0.044(5) 0.061(5) -0.006(3) 0.017(3) -0.002(3) C89 0.0304(19) 0.0332(18) 0.0329(18) -0.0008(10) 0.0019(10) -0.0012(10) C90 0.021(4) 0.027(4) 0.018(3) -0.009(2) -0.001(2) 0.001(3) C91 0.013(4) 0.031(4) 0.028(3) -0.005(3) -0.002(3) -0.003(3) C92 0.020(5) 0.037(5) 0.041(4) -0.009(3) 0.000(3) -0.003(3) C93 0.0356(19) 0.0363(19) 0.0364(19) -0.0006(7) 0.0008(7) 0.0005(7) C94 0.025(5) 0.053(6) 0.076(6) 0.010(5) 0.000(4) 0.006(4) C95 0.050(5) 0.029(4) 0.049(4) 0.007(3) 0.000(4) 0.006(3) C96 0.034(5) 0.039(5) 0.052(5) 0.007(3) 0.009(4) 0.008(4) C97 0.010(3) 0.028(4) 0.022(3) -0.002(2) 0.003(2) 0.007(3) C98 0.025(4) 0.019(3) 0.029(3) -0.007(2) -0.004(3) -0.006(3) C99 0.014(3) 0.018(2) 0.037(3) -0.003(2) 0.008(3) -0.006(2) C100 0.006(3) 0.023(4) 0.030(3) -0.004(2) 0.003(2) -0.005(3) C101 0.014(4) 0.016(3) 0.026(3) 0.001(2) -0.005(2) 0.001(3) C102 0.011(4) 0.015(3) 0.028(3) -0.003(2) 0.001(2) 0.002(3) C103 0.014(4) 0.023(4) 0.023(3) -0.003(2) -0.003(2) -0.001(3) C104 0.019(4) 0.037(4) 0.015(3) -0.001(3) 0.000(3) 0.000(3) C105 0.032(5) 0.034(4) 0.024(3) 0.005(3) 0.004(3) 0.006(4) C106 0.056(7) 0.043(4) 0.017(3) 0.008(3) 0.003(4) 0.014(5) C107 0.034(5) 0.065(6) 0.021(3) -0.002(3) 0.000(3) -0.003(5) C108 0.005(3) 0.034(3) 0.012(3) -0.002(2) -0.003(2) 0.009(2) C109 0.026(4) 0.034(4) 0.020(3) 0.002(3) -0.001(3) 0.001(4) C110 0.023(4) 0.024(4) 0.035(4) -0.002(3) -0.001(3) -0.006(3) C111 0.024(4) 0.030(4) 0.023(3) -0.002(3) -0.006(3) 0.002(3) C112 0.010(4) 0.032(4) 0.066(5) 0.007(4) 0.004(4) 0.004(3) N7 0.010(3) 0.029(3) 0.019(2) 0.003(2) 0.002(2) -0.001(2) N8 0.0255(17) 0.0265(17) 0.0269(16) -0.0003(9) -0.0012(9) 0.0007(10) O13 0.014(3) 0.050(3) 0.021(2) -0.002(2) 0.0024(19) -0.009(2) O14 0.016(3) 0.035(3) 0.023(2) -0.002(2) -0.0014(19) 0.004(3) O15 0.047(4) 0.042(4) 0.029(3) 0.005(2) 0.010(2) 0.016(3) O16 0.036(5) 0.025(3) 0.057(4) 0.004(2) -0.005(3) -0.001(3) O200_1 0.083(5) 0.065(4) 0.067(4) 0.017(3) -0.008(4) -0.005(4) O201_1 0.043(3) 0.047(3) 0.067(4) 0.003(3) 0.002(3) 0.001(2) C200_1 0.043(5) 0.059(6) 0.091(7) 0.004(5) -0.014(5) -0.010(4) C201_1 0.063(5) 0.035(4) 0.046(4) 0.006(3) 0.002(4) -0.007(3) C202_1 0.045(5) 0.053(5) 0.094(8) 0.018(5) -0.005(5) -0.009(4) C203_1 0.078(8) 0.046(6) 0.147(12) 0.027(6) 0.056(8) -0.006(5) O200_2 0.077(5) 0.086(5) 0.088(5) 0.032(4) 0.021(4) -0.003(4) O201_2 0.055(4) 0.087(4) 0.064(4) 0.027(4) 0.002(3) 0.016(3) C200_2 0.053(7) 0.038(5) 0.096(7) -0.014(4) -0.001(6) -0.018(5) C201_2 0.044(5) 0.085(7) 0.062(6) 0.020(5) 0.007(4) 0.000(4) C202_2 0.039(6) 0.089(7) 0.068(7) 0.031(6) 0.016(5) 0.007(5) C203_2 0.084(10) 0.113(9) 0.105(10) -0.029(8) -0.016(8) 0.046(8) O200_3 0.047(4) 0.061(4) 0.061(4) -0.014(3) 0.000(3) -0.028(3) O201_3 0.081(5) 0.073(5) 0.086(5) -0.049(4) 0.049(4) -0.046(4) C200_3 0.040(5) 0.062(6) 0.070(6) -0.031(5) 0.027(5) -0.021(4) C201_3 0.039(6) 0.038(6) 0.043(4) -0.006(4) 0.014(4) -0.001(4) C202_3 0.049(6) 0.059(5) 0.068(6) -0.016(5) 0.040(5) -0.025(4) C203_3 0.150(13) 0.052(7) 0.202(16) 0.069(9) 0.116(13) 0.037(8) O200_4 0.057(4) 0.108(8) 0.046(3) 0.018(4) 0.009(3) 0.013(5) O201_4 0.024(2) 0.054(3) 0.050(3) 0.002(3) -0.001(2) 0.006(3) C200_4 0.068(5) 0.060(5) 0.036(4) 0.001(4) -0.006(4) -0.008(5) C201_4 0.034(4) 0.044(4) 0.040(3) 0.010(4) 0.011(3) 0.023(4) C202_4 0.015(3) 0.057(5) 0.062(4) 0.008(5) -0.008(3) 0.010(4) C203_4 0.024(3) 0.055(4) 0.051(4) 0.009(4) -0.003(3) 0.011(4) O200_5 0.080(6) 0.061(4) 0.114(6) -0.017(4) -0.002(5) -0.032(4) O201_5 0.052(4) 0.074(4) 0.070(4) 0.020(3) 0.007(3) 0.005(3) C200_5 0.128(13) 0.089(8) 0.083(9) 0.032(6) 0.023(8) 0.010(8) C201_5 0.086(9) 0.040(4) 0.090(8) 0.033(5) -0.010(5) -0.017(5) C202_5 0.056(6) 0.044(5) 0.091(7) -0.012(4) -0.019(5) -0.002(4) C203_5 0.052(6) 0.050(6) 0.071(6) 0.006(5) -0.007(5) 0.006(4) O200_6 0.048(4) 0.082(5) 0.064(4) -0.030(4) -0.005(3) 0.027(4) O201_6 0.092(7) 0.061(4) 0.104(6) -0.026(4) -0.064(5) 0.034(4) C200_6 0.090(11) 0.098(10) 0.108(10) -0.067(9) -0.054(8) 0.050(8) C201_6 0.052(7) 0.036(6) 0.058(6) -0.014(4) 0.000(4) 0.006(5) C202_6 0.037(5) 0.047(5) 0.094(8) -0.005(5) -0.024(5) 0.018(4) C203_6 0.089(9) 0.066(7) 0.079(7) -0.011(5) -0.004(6) 0.014(6) O200_7 0.095(7) 0.090(7) 0.057(4) 0.005(4) -0.027(4) -0.031(6) O201_7 0.043(4) 0.130(7) 0.067(4) -0.015(4) -0.024(3) 0.014(4) C200_7 0.097(9) 0.070(8) 0.071(6) 0.032(6) 0.002(6) -0.011(6) C201_7 0.065(6) 0.055(6) 0.083(6) -0.004(6) -0.018(5) -0.030(6) C202_7 0.058(6) 0.207(14) 0.065(7) 0.023(8) 0.018(6) 0.054(8) C203_7 0.113(11) 0.124(11) 0.087(9) 0.052(7) 0.049(8) 0.027(9) O200_8 0.40(3) 0.098(6) 0.69(4) 0.061(13) -0.39(3) 0.012(14) O201_8 0.094(7) 0.117(7) 0.171(9) -0.008(6) -0.054(7) 0.005(6) C200_8 0.048(9) 0.092(8) 0.123(10) 0.031(6) -0.006(9) 0.017(8) C201_8 0.127(13) 0.097(7) 0.102(9) 0.012(6) -0.010(8) 0.038(9) C202_8 0.080(9) 0.111(10) 0.093(9) -0.002(7) 0.019(6) -0.012(8) C203_8 0.037(7) 0.24(2) 0.103(10) -0.030(11) 0.001(6) 0.047(10) O200_9 0.159(10) 0.095(7) 0.203(12) 0.093(7) 0.084(9) 0.025(6) O201_9 0.046(3) 0.066(4) 0.069(4) 0.009(3) 0.002(3) -0.006(3) C200_9 0.122(10) 0.078(8) 0.100(9) -0.030(6) 0.080(8) -0.015(7) C201_9 0.090(7) 0.049(5) 0.093(8) -0.001(5) 0.025(6) -0.024(5) C202_9 0.057(7) 0.117(10) 0.065(7) -0.002(6) 0.008(5) 0.048(7) C203_9 0.044(6) 0.087(8) 0.094(8) -0.031(6) 0.019(6) 0.001(5) _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 P2 2.248(2) . ? Pt1 P1 2.266(2) . ? Pt1 Cl2 2.325(2) . ? Pt1 Cl1 2.3622(19) . ? P1 C13 1.823(7) . ? P1 C1 1.828(7) . ? P1 C7 1.829(8) . ? P2 C29 1.809(9) . ? P2 C41 1.822(7) . ? P2 C35 1.826(9) . ? C1 C2 1.406(10) . ? C1 C6 1.417(12) . ? C2 C3 1.380(11) . ? C3 C4 1.358(13) . ? C4 C5 1.454(14) . ? C5 C6 1.349(12) . ? C7 C8 1.364(12) . ? C7 C12 1.394(13) . ? C8 C9 1.333(12) . ? C9 C10 1.393(13) . ? C10 C11 1.375(14) . ? C11 C12 1.428(14) . ? C13 C18 1.386(9) . ? C13 C14 1.413(10) . ? C14 C15 1.394(10) . ? C15 C16 1.350(10) . ? C16 C17 1.421(10) . ? C17 C18 1.386(10) . ? C17 C19 1.505(9) . ? C19 O1 1.270(10) . ? C19 N1 1.322(9) . ? C20 N1 1.466(9) . ? C20 C21 1.517(11) . ? C20 C24 1.527(11) . ? C21 C23 1.548(10) . ? C21 C22 1.552(12) . ? C24 O2 1.231(10) . ? C24 N2 1.336(10) . ? C25 N2 1.433(10) . ? C25 C26 1.518(11) . ? C25 C27 1.562(12) . ? C27 O3 1.156(10) . ? C27 O4 1.372(10) . ? C28 O4 1.412(10) . ? C29 C30 1.381(12) . ? C29 C34 1.422(12) . ? C30 C31 1.382(13) . ? C31 C32 1.399(14) . ? C32 C33 1.363(12) . ? C33 C34 1.439(11) . ? C35 C40 1.348(12) . ? C35 C36 1.376(11) . ? C36 C37 1.333(14) . ? C37 C38 1.397(15) . ? C38 C39 1.381(15) . ? C39 C40 1.370(14) . ? C41 C46 1.379(10) . ? C41 C42 1.425(10) . ? C42 C43 1.372(9) . ? C43 C44 1.339(10) . ? C44 C45 1.422(11) . ? C45 C46 1.404(9) . ? C45 C47 1.508(10) . ? C47 O5 1.226(9) . ? C47 N3 1.341(8) . ? C48 N3 1.437(9) . ? C48 C52 1.545(10) . ? C48 C49 1.543(9) . ? C49 C50 1.524(12) . ? C49 C51 1.527(10) . ? C52 O6 1.222(9) . ? C52 N4 1.373(10) . ? C53 N4 1.466(11) . ? C53 C54 1.506(11) . ? C53 C55 1.508(10) . ? C55 O7 1.247(10) . ? C55 O8 1.296(10) . ? C56 O8 1.482(12) . ? Pt2 P4 2.244(2) . ? Pt2 P3 2.267(2) . ? Pt2 Cl4 2.343(2) . ? Pt2 Cl3 2.3671(18) . ? P3 C63 1.836(9) . ? P3 C57 1.836(7) . ? P3 C69 1.848(7) . ? P4 C97 1.814(6) . ? P4 C85 1.831(9) . ? P4 C91 1.831(9) . ? C57 C58 1.367(10) . ? C57 C62 1.399(11) . ? C58 C59 1.407(10) . ? C59 C60 1.380(13) . ? C60 C61 1.351(14) . ? C61 C62 1.424(12) . ? C63 C64 1.384(12) . ? C63 C68 1.401(12) . ? C64 C65 1.365(13) . ? C65 C66 1.399(12) . ? C66 C67 1.371(13) . ? C67 C68 1.457(12) . ? C69 C70 1.404(12) . ? C69 C74 1.411(10) . ? C70 C71 1.339(10) . ? C71 C72 1.419(9) . ? C72 C73 1.386(10) . ? C73 C74 1.394(9) . ? C73 C75 1.504(9) . ? C75 O9 1.238(9) . ? C75 N5 1.315(9) . ? C76 N5 1.437(9) . ? C76 C80 1.531(11) . ? C76 C77 1.560(10) . ? C77 C79 1.511(11) . ? C77 C78 1.523(12) . ? C80 O10 1.253(10) . ? C80 N6 1.333(10) . ? C81 N6 1.456(10) . ? C81 C82 1.517(12) . ? C81 C83 1.532(11) . ? C83 O11 1.200(10) . ? C83 O12 1.338(9) . ? C84 O12 1.469(9) . ? C85 C86 1.389(11) . ? C85 C90 1.389(11) . ? C86 C87 1.392(13) . ? C87 C88 1.367(14) . ? C88 C89 1.374(12) . ? C89 C90 1.368(11) . ? C91 C96 1.371(12) . ? C91 C92 1.404(12) . ? C92 C93 1.434(13) . ? C93 C94 1.355(14) . ? C94 C95 1.419(15) . ? C95 C96 1.445(14) . ? C97 C102 1.399(9) . ? C97 C98 1.418(11) . ? C98 C99 1.380(9) . ? C99 C100 1.400(9) . ? C100 C101 1.403(10) . ? C101 C102 1.395(9) . ? C101 C103 1.478(10) . ? C103 O13 1.261(10) . ? C103 N7 1.351(9) . ? C104 N7 1.462(10) . ? C104 C108 1.524(11) . ? C104 C105 1.578(10) . ? C105 C107 1.468(12) . ? C105 C106 1.558(12) . ? C108 O14 1.244(9) . ? C108 N8 1.308(11) . ? C109 N8 1.438(13) . ? C109 C110 1.541(12) . ? C109 C111 1.548(11) . ? C111 O15 1.159(10) . ? C111 O16 1.351(10) . ? C112 O16 1.420(11) . ? O200_1 C201_1 1.207(4) . ? O201_1 C201_1 1.343(5) . ? O201_1 C202_1 1.455(5) . ? C200_1 C201_1 1.502(5) . ? C202_1 C203_1 1.510(5) . ? O200_2 C201_2 1.200(5) . ? O201_2 C201_2 1.341(5) . ? O201_2 C202_2 1.464(5) . ? C200_2 C201_2 1.506(5) . ? C202_2 C203_2 1.503(5) . ? O200_3 C201_3 1.185(4) . ? O201_3 C201_3 1.334(5) . ? O201_3 C202_3 1.455(5) . ? C200_3 C201_3 1.499(5) . ? C202_3 C203_3 1.498(5) . ? O200_4 C201_4 1.210(5) . ? O201_4 C201_4 1.341(4) . ? O201_4 C202_4 1.453(4) . ? C200_4 C201_4 1.500(5) . ? C202_4 C203_4 1.508(5) . ? O200_5 C201_5 1.209(5) . ? O201_5 C201_5 1.340(5) . ? O201_5 C202_5 1.461(5) . ? C200_5 C201_5 1.517(5) . ? C202_5 C203_5 1.524(5) . ? O200_6 C201_6 1.178(5) . ? O201_6 C201_6 1.328(5) . ? O201_6 C202_6 1.452(5) . ? C200_6 C201_6 1.492(5) . ? C202_6 C203_6 1.501(5) . ? O200_7 C201_7 1.193(5) . ? O201_7 C201_7 1.328(5) . ? O201_7 C202_7 1.464(5) . ? C200_7 C201_7 1.501(5) . ? C202_7 C203_7 1.504(5) . ? O200_8 C201_8 1.200(5) . ? O201_8 C201_8 1.357(5) . ? O201_8 C202_8 1.463(5) . ? C200_8 C201_8 1.499(5) . ? C202_8 C203_8 1.535(5) . ? O200_9 C201_9 1.197(5) . ? O201_9 C201_9 1.332(5) . ? O201_9 C202_9 1.444(5) . ? C200_9 C201_9 1.499(5) . ? C202_9 C203_9 1.515(5) . ? 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 P2 Pt1 P1 98.04(7) . . ? P2 Pt1 Cl2 90.64(8) . . ? P1 Pt1 Cl2 171.32(8) . . ? P2 Pt1 Cl1 177.21(8) . . ? P1 Pt1 Cl1 84.43(7) . . ? Cl2 Pt1 Cl1 86.89(7) . . ? C13 P1 C1 104.4(3) . . ? C13 P1 C7 101.0(4) . . ? C1 P1 C7 109.8(4) . . ? C13 P1 Pt1 122.2(3) . . ? C1 P1 Pt1 109.4(3) . . ? C7 P1 Pt1 109.4(3) . . ? C29 P2 C41 108.8(3) . . ? C29 P2 C35 100.9(4) . . ? C41 P2 C35 104.1(3) . . ? C29 P2 Pt1 116.3(3) . . ? C41 P2 Pt1 110.0(3) . . ? C35 P2 Pt1 115.6(3) . . ? C2 C1 C6 119.4(7) . . ? C2 C1 P1 120.3(6) . . ? C6 C1 P1 120.3(5) . . ? C3 C2 C1 120.1(8) . . ? C4 C3 C2 121.0(8) . . ? C3 C4 C5 119.3(8) . . ? C6 C5 C4 120.1(9) . . ? C5 C6 C1 120.0(8) . . ? C8 C7 C12 116.9(8) . . ? C8 C7 P1 122.0(7) . . ? C12 C7 P1 120.8(7) . . ? C9 C8 C7 125.7(9) . . ? C8 C9 C10 117.9(9) . . ? C11 C10 C9 120.8(9) . . ? C10 C11 C12 118.8(10) . . ? C7 C12 C11 119.8(10) . . ? C18 C13 C14 116.6(6) . . ? C18 C13 P1 122.9(6) . . ? C14 C13 P1 120.4(5) . . ? C15 C14 C13 120.1(6) . . ? C16 C15 C14 122.5(8) . . ? C15 C16 C17 118.5(7) . . ? C18 C17 C16 118.9(6) . . ? C18 C17 C19 117.9(7) . . ? C16 C17 C19 122.7(6) . . ? C17 C18 C13 123.1(7) . . ? O1 C19 N1 123.3(6) . . ? O1 C19 C17 119.1(6) . . ? N1 C19 C17 117.6(7) . . ? N1 C20 C21 110.1(6) . . ? N1 C20 C24 110.5(6) . . ? C21 C20 C24 115.0(6) . . ? C20 C21 C23 114.3(7) . . ? C20 C21 C22 111.5(6) . . ? C23 C21 C22 110.8(7) . . ? O2 C24 N2 123.7(7) . . ? O2 C24 C20 121.8(7) . . ? N2 C24 C20 114.4(7) . . ? N2 C25 C26 109.7(7) . . ? N2 C25 C27 110.8(7) . . ? C26 C25 C27 107.7(6) . . ? O3 C27 O4 124.8(8) . . ? O3 C27 C25 126.4(8) . . ? O4 C27 C25 108.8(7) . . ? C19 N1 C20 121.1(7) . . ? C24 N2 C25 121.3(7) . . ? C27 O4 C28 118.3(7) . . ? C30 C29 C34 118.8(8) . . ? C30 C29 P2 122.4(7) . . ? C34 C29 P2 118.7(6) . . ? C29 C30 C31 120.6(8) . . ? C30 C31 C32 120.8(8) . . ? C33 C32 C31 121.2(9) . . ? C32 C33 C34 118.3(8) . . ? C29 C34 C33 120.3(8) . . ? C40 C35 C36 118.7(8) . . ? C40 C35 P2 121.5(7) . . ? C36 C35 P2 119.6(6) . . ? C37 C36 C35 121.5(9) . . ? C36 C37 C38 119.3(10) . . ? C39 C38 C37 120.3(10) . . ? C40 C39 C38 117.4(10) . . ? C35 C40 C39 122.6(9) . . ? C46 C41 C42 118.4(6) . . ? C46 C41 P2 124.6(6) . . ? C42 C41 P2 117.0(5) . . ? C43 C42 C41 118.9(7) . . ? C44 C43 C42 123.6(8) . . ? C43 C44 C45 119.0(6) . . ? C46 C45 C44 118.6(6) . . ? C46 C45 C47 116.1(7) . . ? C44 C45 C47 125.0(6) . . ? C41 C46 C45 121.5(7) . . ? O5 C47 N3 122.1(7) . . ? O5 C47 C45 121.2(6) . . ? N3 C47 C45 116.6(7) . . ? N3 C48 C52 108.2(6) . . ? N3 C48 C49 109.9(6) . . ? C52 C48 C49 114.2(6) . . ? C50 C49 C51 111.0(7) . . ? C50 C49 C48 109.0(7) . . ? C51 C49 C48 112.9(6) . . ? O6 C52 N4 122.2(7) . . ? O6 C52 C48 123.9(7) . . ? N4 C52 C48 113.9(7) . . ? N4 C53 C54 109.3(7) . . ? N4 C53 C55 111.2(6) . . ? C54 C53 C55 111.1(6) . . ? O7 C55 O8 123.6(8) . . ? O7 C55 C53 125.5(7) . . ? O8 C55 C53 110.7(7) . . ? C47 N3 C48 121.4(7) . . ? C52 N4 C53 120.5(6) . . ? C55 O8 C56 115.4(7) . . ? P4 Pt2 P3 97.73(7) . . ? P4 Pt2 Cl4 90.53(8) . . ? P3 Pt2 Cl4 171.74(7) . . ? P4 Pt2 Cl3 177.11(7) . . ? P3 Pt2 Cl3 84.76(7) . . ? Cl4 Pt2 Cl3 86.98(7) . . ? C63 P3 C57 109.1(3) . . ? C63 P3 C69 101.1(4) . . ? C57 P3 C69 103.3(3) . . ? C63 P3 Pt2 110.4(3) . . ? C57 P3 Pt2 110.0(3) . . ? C69 P3 Pt2 122.0(3) . . ? C97 P4 C85 106.9(3) . . ? C97 P4 C91 104.9(3) . . ? C85 P4 C91 101.4(4) . . ? C97 P4 Pt2 109.7(2) . . ? C85 P4 Pt2 117.6(3) . . ? C91 P4 Pt2 115.2(3) . . ? C58 C57 C62 118.5(7) . . ? C58 C57 P3 120.5(6) . . ? C62 C57 P3 120.9(5) . . ? C57 C58 C59 121.6(8) . . ? C60 C59 C58 119.1(7) . . ? C61 C60 C59 121.2(7) . . ? C60 C61 C62 119.6(9) . . ? C57 C62 C61 120.1(8) . . ? C64 C63 C68 122.5(8) . . ? C64 C63 P3 121.9(6) . . ? C68 C63 P3 115.6(6) . . ? C65 C64 C63 118.9(8) . . ? C64 C65 C66 121.9(9) . . ? C67 C66 C65 119.9(9) . . ? C66 C67 C68 120.0(9) . . ? C63 C68 C67 116.7(8) . . ? C70 C69 C74 119.1(6) . . ? C70 C69 P3 122.1(6) . . ? C74 C69 P3 118.7(7) . . ? C71 C70 C69 121.7(7) . . ? C70 C71 C72 119.6(7) . . ? C73 C72 C71 120.0(6) . . ? C72 C73 C74 120.0(6) . . ? C72 C73 C75 122.1(6) . . ? C74 C73 C75 117.8(6) . . ? C73 C74 C69 119.3(7) . . ? O9 C75 N5 121.6(6) . . ? O9 C75 C73 118.8(6) . . ? N5 C75 C73 119.3(6) . . ? N5 C76 C80 110.6(6) . . ? N5 C76 C77 110.3(6) . . ? C80 C76 C77 112.8(6) . . ? C79 C77 C78 109.1(7) . . ? C79 C77 C76 113.6(7) . . ? C78 C77 C76 108.8(6) . . ? O10 C80 N6 119.7(7) . . ? O10 C80 C76 122.6(7) . . ? N6 C80 C76 117.7(7) . . ? N6 C81 C82 109.5(7) . . ? N6 C81 C83 108.7(7) . . ? C82 C81 C83 110.8(6) . . ? O11 C83 O12 124.9(7) . . ? O11 C83 C81 127.2(7) . . ? O12 C83 C81 107.7(7) . . ? C75 N5 C76 122.1(6) . . ? C80 N6 C81 124.0(7) . . ? C83 O12 C84 112.0(6) . . ? C86 C85 C90 119.6(8) . . ? C86 C85 P4 120.7(6) . . ? C90 C85 P4 119.7(6) . . ? C85 C86 C87 119.8(8) . . ? C88 C87 C86 119.6(9) . . ? C87 C88 C89 120.4(9) . . ? C90 C89 C88 120.8(8) . . ? C89 C90 C85 119.6(7) . . ? C96 C91 C92 121.0(8) . . ? C96 C91 P4 122.0(7) . . ? C92 C91 P4 117.0(6) . . ? C91 C92 C93 119.4(8) . . ? C94 C93 C92 120.9(10) . . ? C93 C94 C95 119.7(11) . . ? C94 C95 C96 120.0(9) . . ? C91 C96 C95 118.9(9) . . ? C102 C97 C98 118.3(6) . . ? C102 C97 P4 124.2(6) . . ? C98 C97 P4 117.5(5) . . ? C99 C98 C97 120.8(6) . . ? C98 C99 C100 120.0(7) . . ? C101 C100 C99 120.2(6) . . ? C102 C101 C100 119.2(6) . . ? C102 C101 C103 116.9(7) . . ? C100 C101 C103 123.9(6) . . ? C101 C102 C97 121.3(7) . . ? O13 C103 N7 121.0(7) . . ? O13 C103 C101 120.9(6) . . ? N7 C103 C101 118.0(7) . . ? N7 C104 C108 110.2(6) . . ? N7 C104 C105 107.6(7) . . ? C108 C104 C105 112.2(6) . . ? C107 C105 C106 111.5(7) . . ? C107 C105 C104 113.8(8) . . ? C106 C105 C104 107.8(7) . . ? O14 C108 N8 120.9(7) . . ? O14 C108 C104 122.8(7) . . ? N8 C108 C104 116.4(7) . . ? N8 C109 C110 109.5(7) . . ? N8 C109 C111 110.6(7) . . ? C110 C109 C111 108.5(7) . . ? O15 C111 O16 126.1(8) . . ? O15 C111 C109 125.4(8) . . ? O16 C111 C109 108.4(7) . . ? C103 N7 C104 118.6(6) . . ? C108 N8 C109 122.5(7) . . ? C111 O16 C112 116.7(7) . . ? C201_1 O201_1 C202_1 117.4(6) . . ? O200_1 C201_1 O201_1 120.3(7) . . ? O200_1 C201_1 C200_1 122.9(7) . . ? O201_1 C201_1 C200_1 116.6(6) . . ? O201_1 C202_1 C203_1 113.2(9) . . ? C201_2 O201_2 C202_2 119.0(7) . . ? O200_2 C201_2 O201_2 122.1(7) . . ? O200_2 C201_2 C200_2 124.4(8) . . ? O201_2 C201_2 C200_2 113.5(7) . . ? O201_2 C202_2 C203_2 108.7(9) . . ? C201_3 O201_3 C202_3 118.0(7) . . ? O200_3 C201_3 O201_3 121.9(7) . . ? O200_3 C201_3 C200_3 127.3(7) . . ? O201_3 C201_3 C200_3 109.8(6) . . ? O201_3 C202_3 C203_3 113.9(9) . . ? C201_4 O201_4 C202_4 117.1(5) . . ? O200_4 C201_4 O201_4 120.2(6) . . ? O200_4 C201_4 C200_4 127.6(6) . . ? O201_4 C201_4 C200_4 112.2(5) . . ? O201_4 C202_4 C203_4 105.9(5) . . ? C201_5 O201_5 C202_5 118.1(7) . . ? O200_5 C201_5 O201_5 119.4(8) . . ? O200_5 C201_5 C200_5 126.3(9) . . ? O201_5 C201_5 C200_5 114.3(7) . . ? O201_5 C202_5 C203_5 111.1(7) . . ? C201_6 O201_6 C202_6 115.0(7) . . ? O200_6 C201_6 O201_6 119.6(8) . . ? O200_6 C201_6 C200_6 125.7(8) . . ? O201_6 C201_6 C200_6 113.1(7) . . ? O201_6 C202_6 C203_6 105.2(8) . . ? C201_7 O201_7 C202_7 109.6(8) . . ? O200_7 C201_7 O201_7 123.4(8) . . ? O200_7 C201_7 C200_7 131.7(9) . . ? O201_7 C201_7 C200_7 104.8(7) . . ? O201_7 C202_7 C203_7 107.5(9) . . ? C201_8 O201_8 C202_8 118.1(9) . . ? O200_8 C201_8 O201_8 110.5(13) . . ? O200_8 C201_8 C200_8 133.3(15) . . ? O201_8 C201_8 C200_8 114.5(9) . . ? O201_8 C202_8 C203_8 102.5(10) . . ? C201_9 O201_9 C202_9 119.3(7) . . ? O200_9 C201_9 O201_9 120.0(8) . . ? O200_9 C201_9 C200_9 126.1(9) . . ? O201_9 C201_9 C200_9 113.9(8) . . ? O201_9 C202_9 C203_9 108.0(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4N O9 0.88 2.00 2.849(8) 162.3 1_455 N8 H8A O1 0.86 2.00 2.847(10) 168.3 . N2 H2N O13 0.87 2.03 2.880(9) 164.8 . N5 H5A O14 0.86 2.12 2.936(9) 159.1 . N7 H7N O10 0.79 2.13 2.903(9) 166.6 . N3 H3A O2 0.86 2.09 2.914(9) 159.2 . N1 H1N O6 0.98 1.96 2.910(9) 162.4 . N6 H6A O5 0.86 2.03 2.890(9) 177.0 1_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.123 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.097