# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2326 #TrackingRef 'web_deposit_cif_file_0_AndreiN.Vedernikov_1365084323.2326_LH_HCl.cif' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Organic salt ; _chemical_name_common 'Organic salt' _chemical_formula_moiety 'C18 H24 B N2, Cl, 0.41(O)' _chemical_formula_sum 'C18 H24 B Cl N2 O0.41' _chemical_formula_weight 321.18 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4357(8) _cell_length_b 13.7411(14) _cell_length_c 15.5693(15) _cell_angle_alpha 79.680(2) _cell_angle_beta 80.340(2) _cell_angle_gamma 89.731(2) _cell_volume 1749.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8573 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.7 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.219 _exptl_crystal_F_000 684.8 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_absorpt_coefficient_mu 0.219 _shelx_estimated_absorpt_T_min 0.912 _shelx_estimated_absorpt_T_max 0.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'three-circle diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 31045 _diffrn_reflns_sigmaI/netI 0.0203 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.197 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 6145 _reflns_number_gt 5548 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; The reflections were merged according to the crystal class for structure refinement and the calculation of statistics. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. These statistics refer to single and composite reflections containing twin component 1 only. ; _computing_data_collection 'Apex2 (Bruker, 2010)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2012)' _computing_structure_refinement SHELXL-2012 _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material Apex2 _refine_special_details ; Non-merohedral twinning by 180 deg. rotation around 010 real axis. Integrated and refined as two component twin with a 2nd component portion of 40.5(1)%. The structure contains two symmetrically independent molecules, one of which exhibit whole molecule disorder and therefore was both alternative orientations were refined using restraints on similar geometry and rigid body montions. The ratio bteween two alternative orientations was refined to about 3:2 ratio. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+1.3840P] 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 6145 _refine_ls_number_parameters 564 _refine_ls_number_restraints 295 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.38583(11) 0.87965(7) 0.45787(4) 0.0734(3) Uani 1 1 d . . . Cl2 Cl 0.63782(12) 0.43029(12) 0.34063(12) 0.0514(4) Uani 0.695(3) 1 d PD A 1 Cl2A Cl 0.6304(3) 0.3880(3) 0.3780(3) 0.0514(4) Uani 0.305(3) 1 d PD A 2 O1A O 0.3710(7) 0.4172(4) 0.5332(3) 0.061(2) Uani 0.384(6) 1 d P B 1 O2A O 0.4275(5) 0.3216(3) 0.5037(3) 0.0485(16) Uani 0.432(6) 1 d P C 2 B1 B 0.3391(3) 0.9483(2) 0.18817(15) 0.0314(5) Uani 1 1 d . . . C11 C 0.2806(2) 0.97250(16) 0.09207(13) 0.0298(5) Uani 1 1 d . . . H11 H 0.3785 0.9864 0.0452 0.036 Uiso 1 1 calc RD . . C12 C 0.1776(3) 1.06584(17) 0.08654(16) 0.0367(6) Uani 1 1 d . . . H12A H 0.2477 1.1236 0.0860 0.044 Uiso 1 1 calc RD . . H12B H 0.1371 1.0763 0.0296 0.044 Uiso 1 1 calc RD . . C13 C 0.0339(3) 1.06288(19) 0.16166(17) 0.0425(6) Uani 1 1 d . . . H13A H -0.0061 1.1308 0.1611 0.051 Uiso 1 1 calc RD . . H13B H -0.0536 1.0217 0.1502 0.051 Uiso 1 1 calc RD . . C14 C 0.0721(3) 1.0218(2) 0.25366(18) 0.0500(7) Uani 1 1 d . . . H14A H -0.0305 1.0077 0.2956 0.060 Uiso 1 1 calc RD . . H14B H 0.1315 1.0736 0.2730 0.060 Uiso 1 1 calc RD . . C15 C 0.1719(3) 0.9267(2) 0.25997(15) 0.0420(6) Uani 1 1 d . . . H15 H 0.2000 0.9108 0.3208 0.050 Uiso 1 1 calc RD . . C16 C 0.0822(3) 0.8356(2) 0.24293(18) 0.0479(7) Uani 1 1 d . . . H16A H 0.1466 0.7764 0.2574 0.057 Uiso 1 1 calc RD . . H16B H -0.0217 0.8260 0.2842 0.057 Uiso 1 1 calc RD . . C17 C 0.0486(3) 0.84136(19) 0.14880(17) 0.0426(6) Uani 1 1 d . . . H17A H -0.0449 0.8839 0.1413 0.051 Uiso 1 1 calc RD . . H17B H 0.0189 0.7743 0.1410 0.051 Uiso 1 1 calc RD . . C18 C 0.1900(3) 0.88202(18) 0.07621(16) 0.0363(5) Uani 1 1 d . . . H18A H 0.1493 0.9003 0.0196 0.044 Uiso 1 1 calc RD . . H18B H 0.2675 0.8285 0.0695 0.044 Uiso 1 1 calc RD . . C21 C 0.4530(3) 1.03739(17) 0.20518(15) 0.0331(5) Uani 1 1 d . . . C22 C 0.5417(3) 1.10820(18) 0.13992(16) 0.0361(6) Uani 1 1 d . . . H22 H 0.5347 1.1084 0.0796 0.043 Uiso 1 1 calc RD . . C23 C 0.6398(3) 1.1784(2) 0.16007(18) 0.0473(7) Uani 1 1 d . . . H23 H 0.6980 1.2264 0.1142 0.057 Uiso 1 1 calc RD . . C24 C 0.6525(3) 1.1782(2) 0.2479(2) 0.0587(9) Uani 1 1 d . . . H24 H 0.7180 1.2264 0.2631 0.070 Uiso 1 1 calc RD . . C25 C 0.5694(3) 1.1078(2) 0.3115(2) 0.0587(9) Uani 1 1 d . . . H25 H 0.5787 1.1051 0.3719 0.070 Uiso 1 1 calc RD . . N26 N 0.4737(3) 1.04169(17) 0.28904(14) 0.0446(6) Uani 1 1 d . . . H26 H 0.4203 0.9977 0.3322 0.053 Uiso 1 1 calc RD . . C31 C 0.4599(3) 0.85398(16) 0.19506(15) 0.0302(5) Uani 1 1 d . . . C32 C 0.5564(3) 0.82170(17) 0.12438(16) 0.0332(5) Uani 1 1 d . . . H32 H 0.5532 0.8553 0.0658 0.040 Uiso 1 1 calc RD . . C33 C 0.6566(3) 0.74248(18) 0.13674(17) 0.0380(6) Uani 1 1 d . . . H33 H 0.7204 0.7220 0.0871 0.046 Uiso 1 1 calc RD . . C34 C 0.6640(3) 0.69317(18) 0.22127(18) 0.0416(6) Uani 1 1 d . . . H34 H 0.7298 0.6373 0.2306 0.050 Uiso 1 1 calc RD . . C35 C 0.5747(3) 0.72644(19) 0.29098(18) 0.0427(6) Uani 1 1 d . . . H35 H 0.5816 0.6956 0.3499 0.051 Uiso 1 1 calc RD . . N36 N 0.4764(2) 0.80340(15) 0.27638(13) 0.0363(5) Uani 1 1 d . . . H36 H 0.4189 0.8221 0.3229 0.044 Uiso 1 1 calc RD . . B2 B 0.1691(5) 0.4369(3) 0.2519(3) 0.0290(6) Uani 0.587(3) 1 d PDU D 1 C41 C 0.3465(4) 0.4687(3) 0.1915(3) 0.0305(10) Uani 0.587(3) 1 d PDU D 1 H41 H 0.4237 0.4748 0.2326 0.037 Uiso 0.587(3) 1 calc PRD D 1 C42 C 0.3348(7) 0.5719(3) 0.1336(4) 0.0380(11) Uani 0.587(3) 1 d PDU D 1 H42A H 0.3175 0.6215 0.1730 0.046 Uiso 0.587(3) 1 calc PRD D 1 H42B H 0.4393 0.5886 0.0939 0.046 Uiso 0.587(3) 1 calc PRD D 1 C43 C 0.2010(10) 0.5817(11) 0.0765(8) 0.0403(8) Uani 0.587(3) 1 d PDU D 1 H43A H 0.1847 0.6529 0.0556 0.048 Uiso 0.587(3) 1 calc PRD D 1 H43B H 0.2373 0.5515 0.0237 0.048 Uiso 0.587(3) 1 calc PRD D 1 C44 C 0.0392(9) 0.5333(4) 0.1245(5) 0.0359(12) Uani 0.587(3) 1 d PDU D 1 H44A H -0.0285 0.5268 0.0796 0.043 Uiso 0.587(3) 1 calc PRD D 1 H44B H -0.0157 0.5782 0.1624 0.043 Uiso 0.587(3) 1 calc PRD D 1 C45 C 0.0484(6) 0.4310(4) 0.1823(4) 0.0338(11) Uani 0.587(3) 1 d PDU D 1 H45 H -0.0613 0.4109 0.2163 0.041 Uiso 0.587(3) 1 calc PRD D 1 C46 C 0.1106(6) 0.3485(3) 0.1298(3) 0.0365(10) Uani 0.587(3) 1 d PDU D 1 H46A H 0.0963 0.2843 0.1711 0.044 Uiso 0.587(3) 1 calc PRD D 1 H46B H 0.0420 0.3460 0.0844 0.044 Uiso 0.587(3) 1 calc PRD D 1 C47 C 0.2862(7) 0.3591(4) 0.0834(3) 0.0435(15) Uani 0.587(3) 1 d PDU D 1 H47A H 0.2939 0.4098 0.0289 0.052 Uiso 0.587(3) 1 calc PRD D 1 H47B H 0.3191 0.2955 0.0653 0.052 Uiso 0.587(3) 1 calc PRD D 1 C48 C 0.4048(6) 0.3880(4) 0.1396(3) 0.0446(11) Uani 0.587(3) 1 d PDU D 1 H48A H 0.4266 0.3284 0.1817 0.054 Uiso 0.587(3) 1 calc PRD D 1 H48B H 0.5075 0.4106 0.1002 0.054 Uiso 0.587(3) 1 calc PRD D 1 C51 C 0.1180(8) 0.5147(13) 0.3219(11) 0.0239(13) Uani 0.587(3) 1 d PDU D 1 C52 C 0.2213(5) 0.5630(3) 0.3625(2) 0.0321(9) Uani 0.587(3) 1 d PDU D 1 H52 H 0.3339 0.5542 0.3489 0.039 Uiso 0.587(3) 1 calc PRD D 1 C53 C 0.1635(8) 0.6234(7) 0.4221(5) 0.0379(19) Uani 0.587(3) 1 d PDU D 1 H53 H 0.2362 0.6561 0.4486 0.045 Uiso 0.587(3) 1 calc PRD D 1 C54 C -0.0007(7) 0.6362(5) 0.4432(4) 0.0389(14) Uani 0.587(3) 1 d PDU D 1 H54 H -0.0415 0.6785 0.4833 0.047 Uiso 0.587(3) 1 calc PRD D 1 C55 C -0.1019(5) 0.5873(3) 0.4054(2) 0.0337(9) Uani 0.587(3) 1 d PDU D 1 H55 H -0.2150 0.5937 0.4199 0.040 Uiso 0.587(3) 1 calc PRD D 1 N56 N -0.0403(5) 0.5295(3) 0.3471(3) 0.0275(9) Uani 0.587(3) 1 d PDU D 1 H56 H -0.1089 0.4990 0.3235 0.033 Uiso 0.587(3) 1 calc PRD D 1 C61 C 0.1722(6) 0.3335(4) 0.3258(3) 0.0258(10) Uani 0.587(3) 1 d PDU D 1 C62 C 0.0414(6) 0.2683(3) 0.3584(3) 0.0331(10) Uani 0.587(3) 1 d PDU D 1 H62 H -0.0547 0.2800 0.3344 0.040 Uiso 0.587(3) 1 calc PRD D 1 C63 C 0.0468(6) 0.1868(4) 0.4250(4) 0.0433(15) Uani 0.587(3) 1 d PDU D 1 H63 H -0.0447 0.1438 0.4462 0.052 Uiso 0.587(3) 1 calc PRD D 1 C64 C 0.1860(6) 0.1688(4) 0.4601(3) 0.0497(14) Uani 0.587(3) 1 d PDU D 1 H64 H 0.1926 0.1128 0.5049 0.060 Uiso 0.587(3) 1 calc PRD D 1 C65 C 0.3138(5) 0.2330(3) 0.4294(3) 0.0448(11) Uani 0.587(3) 1 d PDU D 1 H65 H 0.4098 0.2231 0.4538 0.054 Uiso 0.587(3) 1 calc PRD D 1 N66 N 0.3038(3) 0.3113(2) 0.36375(18) 0.0324(8) Uani 0.587(3) 1 d PDU D 1 H66 H 0.3893 0.3505 0.3445 0.039 Uiso 0.587(3) 1 calc PRD D 1 B2A B 0.1577(3) 0.4277(2) 0.25480(18) 0.0290(6) Uani 0.413(3) 1 d PRDU D 2 C41A C 0.3162(3) 0.4242(2) 0.18502(18) 0.0324(15) Uani 0.413(3) 1 d PRDU D 2 H41A H 0.4061 0.4051 0.2186 0.039 Uiso 0.413(3) 1 calc PRD D 2 C42A C 0.3550(10) 0.5317(4) 0.1306(5) 0.0380(11) Uani 0.413(3) 1 d PDU D 2 H42C H 0.3754 0.5759 0.1715 0.046 Uiso 0.413(3) 1 calc PRD D 2 H42D H 0.4548 0.5308 0.0870 0.046 Uiso 0.413(3) 1 calc PRD D 2 C43A C 0.2197(14) 0.5749(16) 0.0809(12) 0.0403(8) Uani 0.413(3) 1 d PDU D 2 H43C H 0.2405 0.6469 0.0606 0.048 Uiso 0.413(3) 1 calc PRD D 2 H43D H 0.2224 0.5444 0.0277 0.048 Uiso 0.413(3) 1 calc PRD D 2 C44A C 0.0512(13) 0.5583(6) 0.1371(7) 0.0359(12) Uani 0.413(3) 1 d PDU D 2 H44C H -0.0292 0.5717 0.0971 0.043 Uiso 0.413(3) 1 calc PRD D 2 H44D H 0.0362 0.6071 0.1773 0.043 Uiso 0.413(3) 1 calc PRD D 2 C45A C 0.0164(9) 0.4535(6) 0.1932(5) 0.0338(11) Uani 0.413(3) 1 d PDU D 2 H45A H -0.0890 0.4540 0.2336 0.041 Uiso 0.413(3) 1 calc PRD D 2 C46A C 0.0041(8) 0.3749(4) 0.1336(4) 0.0338(13) Uani 0.413(3) 1 d PDU D 2 H46C H -0.0371 0.3117 0.1721 0.041 Uiso 0.413(3) 1 calc PRD D 2 H46D H -0.0755 0.3969 0.0946 0.041 Uiso 0.413(3) 1 calc PRD D 2 C47A C 0.1632(8) 0.3557(4) 0.0756(4) 0.0323(14) Uani 0.413(3) 1 d PDU D 2 H47C H 0.1522 0.2929 0.0541 0.039 Uiso 0.413(3) 1 calc PRD D 2 H47D H 0.1843 0.4096 0.0232 0.039 Uiso 0.413(3) 1 calc PRD D 2 C48A C 0.3073(8) 0.3496(5) 0.1244(4) 0.0303(16) Uani 0.413(3) 1 d PDU D 2 H48C H 0.3068 0.2824 0.1603 0.036 Uiso 0.413(3) 1 calc PRD D 2 H48D H 0.4068 0.3575 0.0796 0.036 Uiso 0.413(3) 1 calc PRD D 2 C51A C 0.1509(13) 0.503(2) 0.3221(17) 0.0239(13) Uani 0.413(3) 1 d PDU D 2 C52A C 0.0180(8) 0.5503(6) 0.3595(5) 0.0302(16) Uani 0.413(3) 1 d PDU D 2 H52A H -0.0829 0.5418 0.3420 0.036 Uiso 0.413(3) 1 calc PRD D 2 C53A C 0.0277(9) 0.6098(6) 0.4215(5) 0.0301(17) Uani 0.413(3) 1 d PDU D 2 H53A H -0.0646 0.6428 0.4447 0.036 Uiso 0.413(3) 1 calc PRD D 2 C54A C 0.1734(9) 0.6211(10) 0.4495(7) 0.033(2) Uani 0.413(3) 1 d PDU D 2 H54A H 0.1831 0.6621 0.4915 0.039 Uiso 0.413(3) 1 calc PRD D 2 C55A C 0.3017(6) 0.5716(4) 0.4149(3) 0.0338(13) Uani 0.413(3) 1 d PDU D 2 H55A H 0.4018 0.5761 0.4343 0.041 Uiso 0.413(3) 1 calc PRD D 2 N56A N 0.2876(6) 0.5167(4) 0.3538(3) 0.0276(11) Uani 0.413(3) 1 d PDU D 2 H56A H 0.3743 0.4872 0.3323 0.033 Uiso 0.413(3) 1 calc PRD D 2 C61A C 0.1154(7) 0.3203(5) 0.3187(5) 0.0258(10) Uani 0.413(3) 1 d PDU D 2 C62A C 0.2318(6) 0.2588(4) 0.3512(3) 0.0279(12) Uani 0.413(3) 1 d PDU D 2 H62A H 0.3423 0.2751 0.3294 0.033 Uiso 0.413(3) 1 calc PRD D 2 C63A C 0.1904(8) 0.1746(4) 0.4146(4) 0.0375(16) Uani 0.413(3) 1 d PDU D 2 H63A H 0.2721 0.1343 0.4363 0.045 Uiso 0.413(3) 1 calc PRD D 2 C64A C 0.0296(8) 0.1490(5) 0.4466(6) 0.040(2) Uani 0.413(3) 1 d PDU D 2 H64A H -0.0007 0.0900 0.4883 0.048 Uiso 0.413(3) 1 calc PRD D 2 C65A C -0.0836(7) 0.2109(4) 0.4162(3) 0.0384(14) Uani 0.413(3) 1 d PDU D 2 H65A H -0.1946 0.1961 0.4380 0.046 Uiso 0.413(3) 1 calc PRD D 2 N66A N -0.0383(6) 0.2928(4) 0.3555(3) 0.0269(11) Uani 0.413(3) 1 d PDU D 2 H66A H -0.1147 0.3316 0.3383 0.032 Uiso 0.413(3) 1 calc PRD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0884(6) 0.1083(7) 0.0322(3) -0.0230(4) -0.0255(3) 0.0481(5) Cl2 0.0238(3) 0.0434(9) 0.0898(11) -0.0234(7) -0.0052(5) -0.0005(5) Cl2A 0.0238(3) 0.0434(9) 0.0898(11) -0.0234(7) -0.0052(5) -0.0005(5) O1A 0.085(4) 0.057(4) 0.040(3) -0.006(2) -0.012(3) 0.027(3) O2A 0.042(3) 0.066(3) 0.040(3) -0.012(2) -0.0115(18) 0.012(2) B1 0.0333(13) 0.0326(14) 0.0300(13) -0.0065(11) -0.0098(10) 0.0101(11) C11 0.0290(11) 0.0299(12) 0.0315(11) -0.0048(10) -0.0087(9) 0.0011(10) C12 0.0350(13) 0.0310(13) 0.0468(14) -0.0031(11) -0.0187(11) 0.0042(10) C13 0.0340(13) 0.0381(14) 0.0603(17) -0.0147(12) -0.0163(12) 0.0102(11) C14 0.0367(14) 0.070(2) 0.0505(16) -0.0285(15) -0.0103(12) 0.0181(13) C15 0.0360(13) 0.0614(17) 0.0280(11) -0.0040(12) -0.0082(10) 0.0151(12) C16 0.0343(14) 0.0487(16) 0.0506(16) 0.0104(13) 0.0003(12) 0.0055(12) C17 0.0355(14) 0.0337(14) 0.0581(17) -0.0053(12) -0.0100(12) -0.0017(11) C18 0.0333(13) 0.0363(13) 0.0415(13) -0.0081(11) -0.0113(11) -0.0015(10) C21 0.0305(12) 0.0422(14) 0.0336(12) -0.0176(11) -0.0144(10) 0.0186(10) C22 0.0293(12) 0.0438(14) 0.0428(14) -0.0208(12) -0.0143(11) 0.0120(11) C23 0.0266(12) 0.0547(17) 0.0701(18) -0.0311(15) -0.0145(12) 0.0097(12) C24 0.0290(13) 0.086(2) 0.082(2) -0.060(2) -0.0222(14) 0.0125(15) C25 0.0406(15) 0.097(3) 0.0611(18) -0.0560(19) -0.0291(14) 0.0298(16) N26 0.0424(12) 0.0628(15) 0.0390(12) -0.0258(11) -0.0195(10) 0.0243(11) C31 0.0279(11) 0.0292(12) 0.0331(12) -0.0014(10) -0.0085(9) 0.0004(9) C32 0.0310(12) 0.0320(13) 0.0370(13) -0.0060(10) -0.0072(10) 0.0026(10) C33 0.0291(12) 0.0355(13) 0.0521(15) -0.0122(12) -0.0096(10) 0.0025(10) C34 0.0290(12) 0.0327(13) 0.0646(17) -0.0068(12) -0.0145(12) 0.0073(10) C35 0.0361(13) 0.0384(14) 0.0521(15) 0.0072(12) -0.0199(11) 0.0017(12) N36 0.0312(11) 0.0390(11) 0.0361(11) 0.0014(9) -0.0069(8) 0.0059(9) B2 0.0331(13) 0.0242(14) 0.0279(12) -0.0054(10) 0.0004(10) 0.0042(11) C41 0.0249(19) 0.031(3) 0.028(2) 0.0028(19) 0.0093(15) -0.0065(19) C42 0.045(2) 0.031(3) 0.0341(15) -0.005(3) 0.0067(14) -0.006(3) C43 0.066(2) 0.025(2) 0.0274(16) -0.0030(11) -0.0036(16) 0.0036(19) C44 0.0507(19) 0.041(3) 0.023(2) -0.016(2) -0.0160(15) 0.007(2) C45 0.043(2) 0.041(3) 0.0196(17) -0.0154(15) 0.0001(17) -0.0077(19) C46 0.056(3) 0.028(2) 0.028(3) -0.0134(19) -0.006(2) -0.004(2) C47 0.063(4) 0.036(3) 0.032(3) -0.017(3) 0.002(3) 0.003(3) C48 0.040(3) 0.051(3) 0.039(2) -0.016(2) 0.013(2) 0.006(2) C51 0.027(3) 0.023(4) 0.0210(11) -0.002(2) -0.003(3) -0.001(3) C52 0.036(2) 0.036(3) 0.024(2) -0.0054(18) -0.0039(18) -0.0046(19) C53 0.063(4) 0.031(3) 0.023(4) -0.005(3) -0.014(2) -0.013(2) C54 0.065(3) 0.023(3) 0.028(3) -0.009(2) -0.002(2) 0.005(2) C55 0.041(2) 0.029(2) 0.028(2) -0.0045(16) 0.0034(17) 0.0096(18) N56 0.033(2) 0.027(2) 0.0232(19) -0.0073(15) -0.0035(18) 0.0021(18) C61 0.027(3) 0.0300(18) 0.0231(15) -0.0137(13) -0.002(2) 0.001(2) C62 0.030(3) 0.036(3) 0.033(2) -0.0075(19) -0.003(2) 0.003(2) C63 0.052(3) 0.028(4) 0.043(4) -0.001(3) 0.006(2) -0.005(3) C64 0.065(3) 0.047(3) 0.030(3) 0.005(3) -0.002(3) 0.018(2) C65 0.045(2) 0.059(3) 0.033(2) -0.013(2) -0.0071(19) 0.020(2) N66 0.0251(17) 0.040(2) 0.0314(18) -0.0093(15) -0.0013(14) 0.0083(15) B2A 0.0331(13) 0.0242(14) 0.0279(12) -0.0054(10) 0.0004(10) 0.0042(11) C41A 0.041(3) 0.016(3) 0.039(3) 0.001(3) -0.011(3) -0.003(3) C42A 0.045(2) 0.031(3) 0.0341(15) -0.005(3) 0.0067(14) -0.006(3) C43A 0.066(2) 0.025(2) 0.0274(16) -0.0030(11) -0.0036(16) 0.0036(19) C44A 0.0507(19) 0.041(3) 0.023(2) -0.016(2) -0.0160(15) 0.007(2) C45A 0.043(2) 0.041(3) 0.0196(17) -0.0154(15) 0.0001(17) -0.0077(19) C46A 0.036(3) 0.040(3) 0.029(3) -0.013(3) -0.011(3) 0.012(3) C47A 0.050(4) 0.031(3) 0.019(3) -0.011(2) -0.008(3) 0.011(3) C48A 0.034(4) 0.034(3) 0.023(4) -0.009(3) -0.001(3) 0.010(3) C51A 0.027(3) 0.023(4) 0.0210(11) -0.002(2) -0.003(3) -0.001(3) C52A 0.032(4) 0.033(4) 0.028(4) -0.004(3) -0.011(3) 0.008(3) C53A 0.046(4) 0.019(4) 0.023(4) -0.004(3) 0.000(3) 0.004(3) C54A 0.048(4) 0.026(4) 0.027(7) -0.012(4) -0.004(3) -0.004(3) C55A 0.036(3) 0.035(3) 0.031(3) -0.008(2) -0.005(2) -0.008(2) N56A 0.027(3) 0.031(3) 0.027(2) -0.010(2) -0.005(2) 0.003(2) C61A 0.027(3) 0.0300(18) 0.0231(15) -0.0137(13) -0.002(2) 0.001(2) C62A 0.034(3) 0.024(3) 0.026(3) -0.007(2) -0.003(2) 0.004(2) C63A 0.062(4) 0.030(3) 0.022(3) -0.010(3) -0.005(3) 0.016(3) C64A 0.069(5) 0.015(4) 0.034(5) -0.005(3) 0.003(3) -0.008(3) C65A 0.043(3) 0.037(3) 0.035(3) -0.019(3) 0.005(2) -0.012(3) N66A 0.025(3) 0.032(3) 0.026(2) -0.013(2) -0.003(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 B1 C11 1.631(3) . ? B1 C15 1.638(3) . ? B1 C21 1.644(4) . ? B1 C31 1.645(3) . ? C11 C18 1.541(3) . ? C11 C12 1.544(3) . ? C11 H11 1.0000 . ? C12 C13 1.532(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.529(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.548(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.551(4) . ? C15 H15 1.0000 . ? C16 C17 1.527(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.529(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C21 N26 1.358(3) . ? C21 C22 1.392(3) . ? C22 C23 1.385(3) . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 H23 0.9500 . ? C24 C25 1.356(4) . ? C24 H24 0.9500 . ? C25 N26 1.348(3) . ? C25 H25 0.9500 . ? N26 H26 0.8800 . ? C31 N36 1.360(3) . ? C31 C32 1.393(3) . ? C32 C33 1.381(3) . ? C32 H32 0.9500 . ? C33 C34 1.379(3) . ? C33 H33 0.9500 . ? C34 C35 1.362(4) . ? C34 H34 0.9500 . ? C35 N36 1.352(3) . ? C35 H35 0.9500 . ? N36 H36 0.8800 . ? B2 C45 1.619(5) . ? B2 C41 1.643(5) . ? B2 C61 1.664(6) . ? B2 C51 1.664(7) . ? C41 C48 1.519(5) . ? C41 C42 1.551(5) . ? C41 H41 1.0000 . ? C42 C43 1.542(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.534(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.536(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.553(5) . ? C45 H45 1.0000 . ? C46 C47 1.530(6) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.531(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C51 N56 1.353(6) . ? C51 C52 1.392(6) . ? C52 C53 1.382(6) . ? C52 H52 0.9500 . ? C53 C54 1.386(6) . ? C53 H53 0.9500 . ? C54 C55 1.357(6) . ? C54 H54 0.9500 . ? C55 N56 1.350(4) . ? C55 H55 0.9500 . ? N56 H56 0.8800 . ? C61 N66 1.351(5) . ? C61 C62 1.391(5) . ? C62 C63 1.390(6) . ? C62 H62 0.9500 . ? C63 C64 1.380(6) . ? C63 H63 0.9500 . ? C64 C65 1.362(6) . ? C64 H64 0.9500 . ? C65 N66 1.357(4) . ? C65 H65 0.9500 . ? N66 H66 0.8800 . ? B2A C41A 1.5814 . ? B2A C51A 1.589(8) . ? B2A C61A 1.629(7) . ? B2A C45A 1.650(6) . ? C41A C48A 1.522(6) . ? C41A C42A 1.572(6) . ? C41A H41A 1.0000 . ? C42A C43A 1.542(7) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? C43A C44A 1.533(8) . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? C44A C45A 1.546(7) . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C45A C46A 1.560(6) . ? C45A H45A 1.0000 . ? C46A C47A 1.537(6) . ? C46A H46C 0.9900 . ? C46A H46D 0.9900 . ? C47A C48A 1.533(7) . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C48A H48C 0.9900 . ? C48A H48D 0.9900 . ? C51A N56A 1.356(7) . ? C51A C52A 1.392(7) . ? C52A C53A 1.384(7) . ? C52A H52A 0.9500 . ? C53A C54A 1.389(6) . ? C53A H53A 0.9500 . ? C54A C55A 1.362(7) . ? C54A H54A 0.9500 . ? C55A N56A 1.336(5) . ? C55A H55A 0.9500 . ? N56A H56A 0.8800 . ? C61A N66A 1.353(6) . ? C61A C62A 1.393(6) . ? C62A C63A 1.383(6) . ? C62A H62A 0.9500 . ? C63A C64A 1.388(6) . ? C63A H63A 0.9500 . ? C64A C65A 1.363(7) . ? C64A H64A 0.9500 . ? C65A N66A 1.345(6) . ? C65A H65A 0.9500 . ? N66A H66A 0.8800 . ? 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 C11 B1 C15 104.51(17) . . ? C11 B1 C21 112.82(19) . . ? C15 B1 C21 113.70(19) . . ? C11 B1 C31 111.89(18) . . ? C15 B1 C31 112.37(19) . . ? C21 B1 C31 101.83(16) . . ? C18 C11 C12 112.19(17) . . ? C18 C11 B1 110.17(18) . . ? C12 C11 B1 109.87(18) . . ? C18 C11 H11 108.2 . . ? C12 C11 H11 108.2 . . ? B1 C11 H11 108.2 . . ? C13 C12 C11 115.3(2) . . ? C13 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? C13 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C12 114.05(19) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 C15 115.2(2) . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14B 108.5 . . ? C15 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 C16 113.62(19) . . ? C14 C15 B1 108.8(2) . . ? C16 C15 B1 109.19(19) . . ? C14 C15 H15 108.4 . . ? C16 C15 H15 108.4 . . ? B1 C15 H15 108.4 . . ? C17 C16 C15 115.8(2) . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 114.3(2) . . ? C16 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? C16 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 C11 115.49(19) . . ? C17 C18 H18A 108.4 . . ? C11 C18 H18A 108.4 . . ? C17 C18 H18B 108.4 . . ? C11 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? N26 C21 C22 114.6(2) . . ? N26 C21 B1 119.4(2) . . ? C22 C21 B1 125.91(19) . . ? C23 C22 C21 122.1(2) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 119.5(3) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 118.6(2) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? N26 C25 C24 119.9(2) . . ? N26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 N26 C21 125.3(3) . . ? C25 N26 H26 117.4 . . ? C21 N26 H26 117.4 . . ? N36 C31 C32 114.7(2) . . ? N36 C31 B1 119.07(19) . . ? C32 C31 B1 126.2(2) . . ? C33 C32 C31 122.1(2) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C34 C33 C32 119.9(2) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 118.5(2) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? N36 C35 C34 120.0(2) . . ? N36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 N36 C31 124.8(2) . . ? C35 N36 H36 117.6 . . ? C31 N36 H36 117.6 . . ? C45 B2 C41 105.8(3) . . ? C45 B2 C61 114.0(4) . . ? C41 B2 C61 112.8(3) . . ? C45 B2 C51 115.6(4) . . ? C41 B2 C51 110.3(6) . . ? C61 B2 C51 98.5(8) . . ? C48 C41 C42 114.5(3) . . ? C48 C41 B2 109.9(3) . . ? C42 C41 B2 108.5(3) . . ? C48 C41 H41 107.9 . . ? C42 C41 H41 107.9 . . ? B2 C41 H41 107.9 . . ? C43 C42 C41 115.6(5) . . ? C43 C42 H42A 108.4 . . ? C41 C42 H42A 108.4 . . ? C43 C42 H42B 108.4 . . ? C41 C42 H42B 108.4 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C42 114.4(6) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C43 C44 C45 115.6(5) . . ? C43 C44 H44A 108.4 . . ? C45 C44 H44A 108.4 . . ? C43 C44 H44B 108.4 . . ? C45 C44 H44B 108.4 . . ? H44A C44 H44B 107.4 . . ? C44 C45 C46 114.4(4) . . ? C44 C45 B2 109.8(4) . . ? C46 C45 B2 106.8(4) . . ? C44 C45 H45 108.6 . . ? C46 C45 H45 108.6 . . ? B2 C45 H45 108.6 . . ? C47 C46 C45 116.3(4) . . ? C47 C46 H46A 108.2 . . ? C45 C46 H46A 108.2 . . ? C47 C46 H46B 108.2 . . ? C45 C46 H46B 108.2 . . ? H46A C46 H46B 107.4 . . ? C46 C47 C48 114.7(4) . . ? C46 C47 H47A 108.6 . . ? C48 C47 H47A 108.6 . . ? C46 C47 H47B 108.6 . . ? C48 C47 H47B 108.6 . . ? H47A C47 H47B 107.6 . . ? C41 C48 C47 114.2(4) . . ? C41 C48 H48A 108.7 . . ? C47 C48 H48A 108.7 . . ? C41 C48 H48B 108.7 . . ? C47 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? N56 C51 C52 115.1(4) . . ? N56 C51 B2 118.0(5) . . ? C52 C51 B2 126.8(5) . . ? C53 C52 C51 121.4(5) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 119.9(5) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 118.8(5) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? N56 C55 C54 119.3(4) . . ? N56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C55 N56 C51 125.4(4) . . ? C55 N56 H56 117.3 . . ? C51 N56 H56 117.3 . . ? N66 C61 C62 114.9(4) . . ? N66 C61 B2 120.4(3) . . ? C62 C61 B2 124.5(4) . . ? C63 C62 C61 122.1(4) . . ? C63 C62 H62 118.9 . . ? C61 C62 H62 118.9 . . ? C64 C63 C62 119.5(5) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C65 C64 C63 118.7(4) . . ? C65 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? N66 C65 C64 119.8(4) . . ? N66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C61 N66 C65 124.9(3) . . ? C61 N66 H66 117.5 . . ? C65 N66 H66 117.5 . . ? C41A B2A C51A 119.1(7) . . ? C41A B2A C61A 111.2(3) . . ? C51A B2A C61A 103.9(13) . . ? C41A B2A C45A 103.9(3) . . ? C51A B2A C45A 109.7(7) . . ? C61A B2A C45A 108.9(4) . . ? C48A C41A C42A 111.5(4) . . ? C48A C41A B2A 113.9(3) . . ? C42A C41A B2A 108.0(3) . . ? C48A C41A H41A 107.7 . . ? C42A C41A H41A 107.7 . . ? B2A C41A H41A 107.7 . . ? C43A C42A C41A 113.8(7) . . ? C43A C42A H42C 108.8 . . ? C41A C42A H42C 108.8 . . ? C43A C42A H42D 108.8 . . ? C41A C42A H42D 108.8 . . ? H42C C42A H42D 107.7 . . ? C44A C43A C42A 113.7(8) . . ? C44A C43A H43C 108.8 . . ? C42A C43A H43C 108.8 . . ? C44A C43A H43D 108.8 . . ? C42A C43A H43D 108.8 . . ? H43C C43A H43D 107.7 . . ? C43A C44A C45A 115.1(8) . . ? C43A C44A H44C 108.5 . . ? C45A C44A H44C 108.5 . . ? C43A C44A H44D 108.5 . . ? C45A C44A H44D 108.5 . . ? H44C C44A H44D 107.5 . . ? C44A C45A C46A 111.4(5) . . ? C44A C45A B2A 108.7(6) . . ? C46A C45A B2A 112.0(5) . . ? C44A C45A H45A 108.2 . . ? C46A C45A H45A 108.2 . . ? B2A C45A H45A 108.2 . . ? C47A C46A C45A 114.7(5) . . ? C47A C46A H46C 108.6 . . ? C45A C46A H46C 108.6 . . ? C47A C46A H46D 108.6 . . ? C45A C46A H46D 108.6 . . ? H46C C46A H46D 107.6 . . ? C48A C47A C46A 113.2(5) . . ? C48A C47A H47C 108.9 . . ? C46A C47A H47C 108.9 . . ? C48A C47A H47D 108.9 . . ? C46A C47A H47D 108.9 . . ? H47C C47A H47D 107.7 . . ? C41A C48A C47A 116.9(4) . . ? C41A C48A H48C 108.1 . . ? C47A C48A H48C 108.1 . . ? C41A C48A H48D 108.1 . . ? C47A C48A H48D 108.1 . . ? H48C C48A H48D 107.3 . . ? N56A C51A C52A 114.3(6) . . ? N56A C51A B2A 117.0(6) . . ? C52A C51A B2A 128.4(6) . . ? C53A C52A C51A 122.3(6) . . ? C53A C52A H52A 118.9 . . ? C51A C52A H52A 118.9 . . ? C52A C53A C54A 119.5(6) . . ? C52A C53A H53A 120.2 . . ? C54A C53A H53A 120.2 . . ? C55A C54A C53A 118.0(6) . . ? C55A C54A H54A 121.0 . . ? C53A C54A H54A 121.0 . . ? N56A C55A C54A 120.4(5) . . ? N56A C55A H55A 119.8 . . ? C54A C55A H55A 119.8 . . ? C55A N56A C51A 125.4(5) . . ? C55A N56A H56A 117.3 . . ? C51A N56A H56A 117.3 . . ? N66A C61A C62A 115.0(5) . . ? N66A C61A B2A 120.8(5) . . ? C62A C61A B2A 123.2(5) . . ? C63A C62A C61A 121.6(5) . . ? C63A C62A H62A 119.2 . . ? C61A C62A H62A 119.2 . . ? C62A C63A C64A 120.0(5) . . ? C62A C63A H63A 120.0 . . ? C64A C63A H63A 120.0 . . ? C65A C64A C63A 118.1(6) . . ? C65A C64A H64A 121.0 . . ? C63A C64A H64A 121.0 . . ? N66A C65A C64A 120.0(5) . . ? N66A C65A H65A 120.0 . . ? C64A C65A H65A 120.0 . . ? C65A N66A C61A 125.2(5) . . ? C65A N66A H66A 117.4 . . ? C61A N66A H66A 117.4 . . ? 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 C15 B1 C11 C18 -62.0(2) . . . . ? C21 B1 C11 C18 174.02(17) . . . . ? C31 B1 C11 C18 59.9(2) . . . . ? C15 B1 C11 C12 62.1(2) . . . . ? C21 B1 C11 C12 -61.9(2) . . . . ? C31 B1 C11 C12 -176.03(18) . . . . ? C18 C11 C12 C13 68.7(2) . . . . ? B1 C11 C12 C13 -54.2(3) . . . . ? C11 C12 C13 C14 43.7(3) . . . . ? C12 C13 C14 C15 -45.0(3) . . . . ? C13 C14 C15 C16 -65.6(3) . . . . ? C13 C14 C15 B1 56.2(3) . . . . ? C11 B1 C15 C14 -62.8(2) . . . . ? C21 B1 C15 C14 60.7(2) . . . . ? C31 B1 C15 C14 175.70(19) . . . . ? C11 B1 C15 C16 61.7(2) . . . . ? C21 B1 C15 C16 -174.83(18) . . . . ? C31 B1 C15 C16 -59.8(2) . . . . ? C14 C15 C16 C17 67.0(3) . . . . ? B1 C15 C16 C17 -54.6(3) . . . . ? C15 C16 C17 C18 43.3(3) . . . . ? C16 C17 C18 C11 -42.8(3) . . . . ? C12 C11 C18 C17 -68.5(3) . . . . ? B1 C11 C18 C17 54.2(3) . . . . ? C11 B1 C21 N26 161.71(18) . . . . ? C15 B1 C21 N26 42.9(3) . . . . ? C31 B1 C21 N26 -78.2(2) . . . . ? C11 B1 C21 C22 -22.6(3) . . . . ? C15 B1 C21 C22 -141.3(2) . . . . ? C31 B1 C21 C22 97.5(2) . . . . ? N26 C21 C22 C23 -1.4(3) . . . . ? B1 C21 C22 C23 -177.4(2) . . . . ? C21 C22 C23 C24 0.7(4) . . . . ? C22 C23 C24 C25 0.9(4) . . . . ? C23 C24 C25 N26 -1.8(4) . . . . ? C24 C25 N26 C21 1.1(4) . . . . ? C22 C21 N26 C25 0.6(3) . . . . ? B1 C21 N26 C25 176.8(2) . . . . ? C11 B1 C31 N36 -158.1(2) . . . . ? C15 B1 C31 N36 -40.9(3) . . . . ? C21 B1 C31 N36 81.2(2) . . . . ? C11 B1 C31 C32 25.2(3) . . . . ? C15 B1 C31 C32 142.4(2) . . . . ? C21 B1 C31 C32 -95.6(2) . . . . ? N36 C31 C32 C33 2.0(3) . . . . ? B1 C31 C32 C33 178.8(2) . . . . ? C31 C32 C33 C34 -0.5(4) . . . . ? C32 C33 C34 C35 -2.0(4) . . . . ? C33 C34 C35 N36 2.9(4) . . . . ? C34 C35 N36 C31 -1.3(4) . . . . ? C32 C31 N36 C35 -1.1(3) . . . . ? B1 C31 N36 C35 -178.2(2) . . . . ? C45 B2 C41 C48 -64.1(4) . . . . ? C61 B2 C41 C48 61.1(4) . . . . ? C51 B2 C41 C48 170.2(7) . . . . ? C45 B2 C41 C42 61.8(4) . . . . ? C61 B2 C41 C42 -173.0(4) . . . . ? C51 B2 C41 C42 -63.9(7) . . . . ? C48 C41 C42 C43 69.4(8) . . . . ? B2 C41 C42 C43 -53.8(8) . . . . ? C41 C42 C43 C44 43.1(14) . . . . ? C42 C43 C44 C45 -42.7(14) . . . . ? C43 C44 C45 C46 -66.1(9) . . . . ? C43 C44 C45 B2 54.0(8) . . . . ? C41 B2 C45 C44 -62.2(5) . . . . ? C61 B2 C45 C44 173.3(4) . . . . ? C51 B2 C45 C44 60.2(9) . . . . ? C41 B2 C45 C46 62.3(5) . . . . ? C61 B2 C45 C46 -62.2(5) . . . . ? C51 B2 C45 C46 -175.3(9) . . . . ? C44 C45 C46 C47 66.7(6) . . . . ? B2 C45 C46 C47 -55.0(6) . . . . ? C45 C46 C47 C48 44.5(6) . . . . ? C42 C41 C48 C47 -68.3(5) . . . . ? B2 C41 C48 C47 54.1(5) . . . . ? C46 C47 C48 C41 -43.2(6) . . . . ? C45 B2 C51 N56 31.2(18) . . . . ? C41 B2 C51 N56 151.1(13) . . . . ? C61 B2 C51 N56 -90.7(15) . . . . ? C45 B2 C51 C52 -153.0(14) . . . . ? C41 B2 C51 C52 -33.0(19) . . . . ? C61 B2 C51 C52 85.2(17) . . . . ? N56 C51 C52 C53 -2(2) . . . . ? B2 C51 C52 C53 -177.6(12) . . . . ? C51 C52 C53 C54 0.6(15) . . . . ? C52 C53 C54 C55 1.1(12) . . . . ? C53 C54 C55 N56 -1.5(10) . . . . ? C54 C55 N56 C51 0.3(14) . . . . ? C52 C51 N56 C55 1(2) . . . . ? B2 C51 N56 C55 177.6(8) . . . . ? C45 B2 C61 N66 153.8(4) . . . . ? C41 B2 C61 N66 33.1(6) . . . . ? C51 B2 C61 N66 -83.2(5) . . . . ? C45 B2 C61 C62 -31.4(7) . . . . ? C41 B2 C61 C62 -152.0(5) . . . . ? C51 B2 C61 C62 91.6(6) . . . . ? N66 C61 C62 C63 0.0(8) . . . . ? B2 C61 C62 C63 -175.0(5) . . . . ? C61 C62 C63 C64 -0.4(10) . . . . ? C62 C63 C64 C65 1.2(9) . . . . ? C63 C64 C65 N66 -1.7(8) . . . . ? C62 C61 N66 C65 -0.6(7) . . . . ? B2 C61 N66 C65 174.7(4) . . . . ? C64 C65 N66 C61 1.5(7) . . . . ? C51A B2A C41A C48A -179.9(12) . . . . ? C61A B2A C41A C48A 59.4(4) . . . . ? C45A B2A C41A C48A -57.5(4) . . . . ? C51A B2A C41A C42A -55.5(12) . . . . ? C61A B2A C41A C42A -176.2(5) . . . . ? C45A B2A C41A C42A 66.9(4) . . . . ? C48A C41A C42A C43A 66.7(12) . . . . ? B2A C41A C42A C43A -59.2(11) . . . . ? C41A C42A C43A C44A 45(2) . . . . ? C42A C43A C44A C45A -44(2) . . . . ? C43A C44A C45A C46A -69.6(12) . . . . ? C43A C44A C45A B2A 54.3(11) . . . . ? C41A B2A C45A C44A -65.1(5) . . . . ? C51A B2A C45A C44A 63.3(13) . . . . ? C61A B2A C45A C44A 176.4(6) . . . . ? C41A B2A C45A C46A 58.4(6) . . . . ? C51A B2A C45A C46A -173.3(12) . . . . ? C61A B2A C45A C46A -60.1(7) . . . . ? C44A C45A C46A C47A 68.3(7) . . . . ? B2A C45A C46A C47A -53.6(8) . . . . ? C45A C46A C47A C48A 42.2(7) . . . . ? C42A C41A C48A C47A -70.2(7) . . . . ? B2A C41A C48A C47A 52.3(6) . . . . ? C46A C47A C48A C41A -41.2(8) . . . . ? C41A B2A C51A N56A -37(3) . . . . ? C61A B2A C51A N56A 87(2) . . . . ? C45A B2A C51A N56A -156.5(19) . . . . ? C41A B2A C51A C52A 149(2) . . . . ? C61A B2A C51A C52A -87(3) . . . . ? C45A B2A C51A C52A 30(3) . . . . ? N56A C51A C52A C53A 2(3) . . . . ? B2A C51A C52A C53A 176.3(18) . . . . ? C51A C52A C53A C54A -2(2) . . . . ? C52A C53A C54A C55A -0.6(17) . . . . ? C53A C54A C55A N56A 2.1(15) . . . . ? C54A C55A N56A C51A -1(2) . . . . ? C52A C51A N56A C55A -1(3) . . . . ? B2A C51A N56A C55A -175.4(12) . . . . ? C41A B2A C61A N66A -151.9(6) . . . . ? C51A B2A C61A N66A 78.9(7) . . . . ? C45A B2A C61A N66A -38.0(8) . . . . ? C41A B2A C61A C62A 39.4(8) . . . . ? C51A B2A C61A C62A -89.9(7) . . . . ? C45A B2A C61A C62A 153.2(7) . . . . ? N66A C61A C62A C63A 1.8(10) . . . . ? B2A C61A C62A C63A 171.1(5) . . . . ? C61A C62A C63A C64A 0.8(10) . . . . ? C62A C63A C64A C65A -2.5(12) . . . . ? C63A C64A C65A N66A 1.6(11) . . . . ? C64A C65A N66A C61A 1.2(10) . . . . ? C62A C61A N66A C65A -2.9(10) . . . . ? B2A C61A N66A C65A -172.5(5) . . . . ? 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 N26 H26 Cl1 0.88 2.29 3.111(3) 156 . N36 H36 Cl1 0.88 2.35 3.161(2) 154 . N56 H56 Cl2A 0.88 2.61 3.316(5) 138 1_455 N66 H66 Cl2A 0.88 2.27 3.012(4) 142 . N56A H56A Cl2A 0.88 2.68 3.422(6) 143 . N66A H66A Cl2A 0.88 2.31 3.073(6) 146 1_455 N56 H56 Cl2 0.88 2.29 3.068(4) 147 1_455 N66 H66 Cl2 0.88 2.36 3.200(3) 160 . N56A H56A Cl2 0.88 2.37 3.167(5) 151 . N66A H66A Cl2 0.88 2.48 3.331(6) 162 1_455 _refine_diff_density_max 0.597 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.040 _database_code_depnum_ccdc_archive 'CCDC 932583' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2334 #TrackingRef 'web_deposit_cif_file_1_AndreiN.Vedernikov_1365084323.2334_LPtMe3.cif' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Pt-complex ; _chemical_name_common Pt-complex _chemical_formula_moiety 'C21 H31 B N2 Pt' _chemical_formula_sum 'C21 H31 B N2 Pt' _chemical_formula_weight 517.38 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' B B 0.0013 0.0007 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7998(10) _cell_length_b 10.3648(8) _cell_length_c 14.9296(11) _cell_angle_alpha 90 _cell_angle_beta 111.4895(11) _cell_angle_gamma 90 _cell_volume 1987.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17909 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 32.1 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.730 _exptl_crystal_F_000 1016 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 7.067 _shelx_estimated_absorpt_T_min 0.226 _shelx_estimated_absorpt_T_max 0.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.128 _exptl_absorpt_correction_T_max 0.493 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'three-circle diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 31911 _diffrn_reflns_sigmaI/netI 0.0181 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.452 _diffrn_reflns_theta_max 29.993 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5790 _reflns_number_gt 5236 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; The reflections were merged according to the crystal class for structure refinement and the calculation of statistics. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex2 (Bruker, 2010)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material Apex2 _refine_special_details ; All H atoms were refined as riding on the attached atom with the exception of H11 atom that forms bond with Pt for which positional parameters were freely refined. The structure refinement at R1=5% shows ~5 e/A3 peak with unreasonable distance (near boron). Including this peak in the refinement lowers R1 below 3%. Difference map shows "shadow" of the main molecule with the peak being Pt atom. Thus the final refinement was conducted with the whole molecule disorder of the complex in 2 alternative orientations: main Pt1-C35 and "shadow" Pt1a-C35a. The ratio between the occupation factors of these complexes was refined as 0.9485(6):0.0515(6). Due to superposition of the complexes the geometry of the shadow complex was restrained to be similar to that of the main molecule using ShelXL SAME instruction; atomic displacement parameters were also restrained using SAME and DELU instruction. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+7.6500P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5790 _refine_ls_number_parameters 458 _refine_ls_number_restraints 820 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0550 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.953 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.310504(10) 0.483821(11) 0.161229(9) 0.02655(4) Uani 0.9485(6) 1 d PD A 1 C1 C 0.3809(4) 0.3071(3) 0.1768(3) 0.0462(10) Uani 0.9485(6) 1 d PDU A 1 H1A H 0.4317 0.3077 0.1451 0.069 Uiso 0.9485(6) 1 calc PRD A 1 H1B H 0.3282 0.2408 0.1474 0.069 Uiso 0.9485(6) 1 calc PRD A 1 H1C H 0.4165 0.2881 0.2454 0.069 Uiso 0.9485(6) 1 calc PRD A 1 C2 C 0.1984(4) 0.3990(4) 0.2053(4) 0.0511(11) Uani 0.9485(6) 1 d PDU A 1 H2A H 0.1513 0.3466 0.1527 0.077 Uiso 0.9485(6) 1 calc PRD A 1 H2B H 0.1586 0.4665 0.2224 0.077 Uiso 0.9485(6) 1 calc PRD A 1 H2C H 0.2327 0.3440 0.2614 0.077 Uiso 0.9485(6) 1 calc PRD A 1 C3 C 0.4020(4) 0.5196(4) 0.3035(3) 0.0418(9) Uani 0.9485(6) 1 d PDU A 1 H3A H 0.3708 0.4782 0.3455 0.063 Uiso 0.9485(6) 1 calc PRD A 1 H3B H 0.4065 0.6129 0.3150 0.063 Uiso 0.9485(6) 1 calc PRD A 1 H3C H 0.4720 0.4846 0.3173 0.063 Uiso 0.9485(6) 1 calc PRD A 1 B1 B 0.2542(3) 0.7035(3) 0.0173(3) 0.0235(6) Uani 0.9485(6) 1 d PDU A 1 C11 C 0.2242(3) 0.7208(3) 0.1136(2) 0.0264(6) Uani 0.9485(6) 1 d PDU A 1 H11 H 0.237(3) 0.650(4) 0.158(3) 0.032 Uiso 0.9485(6) 1 d PD A 1 C12 C 0.2852(3) 0.8350(3) 0.1745(3) 0.0319(7) Uani 0.9485(6) 1 d PDU A 1 H12A H 0.2653 0.8447 0.2315 0.038 Uiso 0.9485(6) 1 calc PRD A 1 H12B H 0.3605 0.8148 0.1979 0.038 Uiso 0.9485(6) 1 calc PRD A 1 C13 C 0.2667(3) 0.9641(3) 0.1202(3) 0.0408(9) Uani 0.9485(6) 1 d PDU A 1 H13A H 0.1981 0.9985 0.1156 0.049 Uiso 0.9485(6) 1 calc PRD A 1 H13B H 0.3205 1.0263 0.1583 0.049 Uiso 0.9485(6) 1 calc PRD A 1 C14 C 0.2693(3) 0.9556(3) 0.0191(3) 0.0421(9) Uani 0.9485(6) 1 d PDU A 1 H14A H 0.3430 0.9533 0.0246 0.051 Uiso 0.9485(6) 1 calc PRD A 1 H14B H 0.2379 1.0353 -0.0162 0.051 Uiso 0.9485(6) 1 calc PRD A 1 C15 C 0.2124(3) 0.8380(3) -0.0416(3) 0.0350(8) Uani 0.9485(6) 1 d PDU A 1 H15 H 0.2277 0.8359 -0.1020 0.042 Uiso 0.9485(6) 1 calc PRD A 1 C16 C 0.0929(3) 0.8494(4) -0.0694(3) 0.0493(11) Uani 0.9485(6) 1 d PDU A 1 H16A H 0.0703 0.9344 -0.1002 0.059 Uiso 0.9485(6) 1 calc PRD A 1 H16B H 0.0589 0.7824 -0.1181 0.059 Uiso 0.9485(6) 1 calc PRD A 1 C17 C 0.0534(3) 0.8356(5) 0.0135(4) 0.0503(12) Uani 0.9485(6) 1 d PDU A 1 H17A H -0.0226 0.8194 -0.0139 0.060 Uiso 0.9485(6) 1 calc PRD A 1 H17B H 0.0644 0.9185 0.0488 0.060 Uiso 0.9485(6) 1 calc PRD A 1 C18 C 0.1053(3) 0.7277(4) 0.0858(3) 0.0393(8) Uani 0.9485(6) 1 d PDU A 1 H18A H 0.0745 0.6439 0.0576 0.047 Uiso 0.9485(6) 1 calc PRD A 1 H18B H 0.0897 0.7414 0.1448 0.047 Uiso 0.9485(6) 1 calc PRD A 1 N2 N 0.4190(2) 0.5786(2) 0.11238(18) 0.0217(5) Uani 0.9485(6) 1 d PDU A 1 C21 C 0.3787(2) 0.6759(3) 0.0477(2) 0.0218(5) Uani 0.9485(6) 1 d PDU A 1 C22 C 0.4464(3) 0.7389(4) 0.0110(3) 0.0309(7) Uani 0.9485(6) 1 d PDU A 1 H22 H 0.4202 0.8053 -0.0356 0.037 Uiso 0.9485(6) 1 calc PRD A 1 C23 C 0.5511(3) 0.7056(4) 0.0419(3) 0.0366(8) Uani 0.9485(6) 1 d PDU A 1 H23 H 0.5967 0.7511 0.0184 0.044 Uiso 0.9485(6) 1 calc PRD A 1 C24 C 0.5885(3) 0.6065(4) 0.1064(3) 0.0372(8) Uani 0.9485(6) 1 d PDU A 1 H24 H 0.6594 0.5809 0.1270 0.045 Uiso 0.9485(6) 1 calc PRD A 1 C25 C 0.5203(3) 0.5452(4) 0.1404(2) 0.0310(7) Uani 0.9485(6) 1 d PDU A 1 H25 H 0.5456 0.4769 0.1854 0.037 Uiso 0.9485(6) 1 calc PRD A 1 N3 N 0.2167(2) 0.4616(3) 0.0115(2) 0.0272(5) Uani 0.9485(6) 1 d PDU A 1 C31 C 0.2025(2) 0.5721(3) -0.0415(2) 0.0263(6) Uani 0.9485(6) 1 d PDU A 1 C32 C 0.1514(3) 0.5619(4) -0.1417(3) 0.0371(8) Uani 0.9485(6) 1 d PDU A 1 H32 H 0.1412 0.6368 -0.1807 0.045 Uiso 0.9485(6) 1 calc PRD A 1 C33 C 0.1154(4) 0.4424(5) -0.1845(3) 0.0461(10) Uani 0.9485(6) 1 d PDU A 1 H33 H 0.0814 0.4362 -0.2524 0.055 Uiso 0.9485(6) 1 calc PRD A 1 C34 C 0.1294(4) 0.3345(4) -0.1284(3) 0.0440(10) Uani 0.9485(6) 1 d PDU A 1 H34 H 0.1045 0.2529 -0.1563 0.053 Uiso 0.9485(6) 1 calc PRD A 1 C35 C 0.1804(4) 0.3470(4) -0.0304(3) 0.0372(8) Uani 0.9485(6) 1 d PDU A 1 H35 H 0.1903 0.2725 0.0091 0.045 Uiso 0.9485(6) 1 calc PRD A 1 Pt1A Pt 0.2134(2) 0.7841(3) 0.0159(2) 0.0344(9) Uani 0.0515(6) 1 d PDU A 2 C1A C 0.202(3) 0.883(3) -0.1068(17) 0.043(5) Uani 0.0515(6) 1 d PDU A 2 H1A1 H 0.1294 0.9109 -0.1402 0.065 Uiso 0.0515(6) 1 calc PRD A 2 H1A2 H 0.2228 0.8269 -0.1492 0.065 Uiso 0.0515(6) 1 calc PRD A 2 H1A3 H 0.2472 0.9590 -0.0895 0.065 Uiso 0.0515(6) 1 calc PRD A 2 C2A C 0.0610(14) 0.841(3) -0.009(4) 0.046(6) Uani 0.0515(6) 1 d PDU A 2 H2A1 H 0.0616 0.9138 0.0334 0.069 Uiso 0.0515(6) 1 calc PRD A 2 H2A2 H 0.0223 0.7691 0.0039 0.069 Uiso 0.0515(6) 1 calc PRD A 2 H2A3 H 0.0273 0.8685 -0.0764 0.069 Uiso 0.0515(6) 1 calc PRD A 2 C3A C 0.268(3) 0.954(2) 0.090(3) 0.036(6) Uani 0.0515(6) 1 d PDU A 2 H3A1 H 0.3441 0.9574 0.1096 0.054 Uiso 0.0515(6) 1 calc PRD A 2 H3A2 H 0.2491 0.9574 0.1469 0.054 Uiso 0.0515(6) 1 calc PRD A 2 H3A3 H 0.2371 1.0275 0.0479 0.054 Uiso 0.0515(6) 1 calc PRD A 2 B1A B 0.2995(17) 0.5190(18) 0.1008(15) 0.028(3) Uani 0.0515(6) 1 d PDU A 2 C11A C 0.253(2) 0.612(2) 0.165(2) 0.031(3) Uani 0.0515(6) 1 d PDU A 2 H11A H 0.2313 0.6946 0.1285 0.037 Uiso 0.0515(6) 1 calc PRD A 2 C12A C 0.340(3) 0.648(4) 0.261(2) 0.037(5) Uani 0.0515(6) 1 d PDU A 2 H12C H 0.3624 0.7375 0.2564 0.045 Uiso 0.0515(6) 1 calc PRD A 2 H12D H 0.3102 0.6466 0.3123 0.045 Uiso 0.0515(6) 1 calc PRD A 2 C13A C 0.437(3) 0.562(4) 0.293(4) 0.042(5) Uani 0.0515(6) 1 d PDU A 2 H13C H 0.4868 0.5975 0.2664 0.050 Uiso 0.0515(6) 1 calc PRD A 2 H13D H 0.4698 0.5666 0.3643 0.050 Uiso 0.0515(6) 1 calc PRD A 2 C14A C 0.420(3) 0.420(3) 0.265(2) 0.041(5) Uani 0.0515(6) 1 d PDU A 2 H14C H 0.4018 0.3745 0.3152 0.049 Uiso 0.0515(6) 1 calc PRD A 2 H14D H 0.4864 0.3843 0.2661 0.049 Uiso 0.0515(6) 1 calc PRD A 2 C15A C 0.335(2) 0.388(2) 0.1662(19) 0.039(4) Uani 0.0515(6) 1 d PDU A 2 H15A H 0.3642 0.3256 0.1320 0.047 Uiso 0.0515(6) 1 calc PRD A 2 C16A C 0.237(3) 0.327(3) 0.177(3) 0.041(4) Uani 0.0515(6) 1 d PDU A 2 H16C H 0.1926 0.2918 0.1142 0.049 Uiso 0.0515(6) 1 calc PRD A 2 H16D H 0.2605 0.2536 0.2226 0.049 Uiso 0.0515(6) 1 calc PRD A 2 C17A C 0.170(4) 0.415(4) 0.213(5) 0.040(5) Uani 0.0515(6) 1 d PDU A 2 H17C H 0.2015 0.4186 0.2842 0.048 Uiso 0.0515(6) 1 calc PRD A 2 H17D H 0.1005 0.3746 0.1959 0.048 Uiso 0.0515(6) 1 calc PRD A 2 C18A C 0.155(2) 0.554(4) 0.174(3) 0.036(4) Uani 0.0515(6) 1 d PDU A 2 H18C H 0.1331 0.6084 0.2178 0.043 Uiso 0.0515(6) 1 calc PRD A 2 H18D H 0.0983 0.5544 0.1103 0.043 Uiso 0.0515(6) 1 calc PRD A 2 N2A N 0.3677(12) 0.718(2) 0.043(3) 0.026(2) Uani 0.0515(6) 1 d PDU A 2 C21A C 0.3913(16) 0.595(2) 0.078(3) 0.026(2) Uani 0.0515(6) 1 d PDU A 2 C22A C 0.496(2) 0.556(4) 0.104(4) 0.029(3) Uani 0.0515(6) 1 d PDU A 2 H22A H 0.5198 0.4820 0.1442 0.035 Uiso 0.0515(6) 1 calc PRD A 2 C23A C 0.564(2) 0.625(5) 0.073(5) 0.032(3) Uani 0.0515(6) 1 d PDU A 2 H23A H 0.6323 0.5940 0.0854 0.038 Uiso 0.0515(6) 1 calc PRD A 2 C24A C 0.530(3) 0.737(5) 0.023(5) 0.033(3) Uani 0.0515(6) 1 d PDU A 2 H24A H 0.5695 0.7782 -0.0100 0.040 Uiso 0.0515(6) 1 calc PRD A 2 C25A C 0.438(2) 0.790(3) 0.022(5) 0.030(3) Uani 0.0515(6) 1 d PDU A 2 H25A H 0.4237 0.8780 0.0055 0.036 Uiso 0.0515(6) 1 calc PRD A 2 N3A N 0.164(2) 0.6028(13) -0.0563(16) 0.032(3) Uani 0.0515(6) 1 d PDU A 2 C31A C 0.212(3) 0.4959(15) -0.0068(18) 0.032(3) Uani 0.0515(6) 1 d PDU A 2 C32A C 0.176(6) 0.3758(18) -0.051(3) 0.038(3) Uani 0.0515(6) 1 d PDU A 2 H32A H 0.1894 0.2993 -0.0129 0.046 Uiso 0.0515(6) 1 calc PRD A 2 C33A C 0.121(8) 0.370(3) -0.150(3) 0.040(3) Uani 0.0515(6) 1 d PDU A 2 H33A H 0.0978 0.2897 -0.1814 0.048 Uiso 0.0515(6) 1 calc PRD A 2 C34A C 0.102(7) 0.483(4) -0.202(2) 0.041(3) Uani 0.0515(6) 1 d PDU A 2 H34A H 0.0878 0.4835 -0.2692 0.049 Uiso 0.0515(6) 1 calc PRD A 2 C35A C 0.105(4) 0.595(3) -0.1513(19) 0.038(3) Uani 0.0515(6) 1 d PDU A 2 H35A H 0.0656 0.6677 -0.1834 0.045 Uiso 0.0515(6) 1 calc PRD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03734(7) 0.01794(6) 0.02677(6) 0.00108(4) 0.01458(5) -0.00193(5) C1 0.072(3) 0.0194(15) 0.047(2) 0.0093(15) 0.021(2) 0.0093(17) C2 0.073(3) 0.038(2) 0.052(2) -0.0007(19) 0.035(2) -0.015(2) C3 0.059(2) 0.0366(19) 0.0270(16) 0.0060(15) 0.0118(16) -0.0018(18) B1 0.0177(14) 0.0220(14) 0.0271(15) 0.0002(12) 0.0038(12) 0.0010(12) C11 0.0235(14) 0.0220(13) 0.0343(16) -0.0037(12) 0.0115(12) -0.0003(11) C12 0.0324(17) 0.0229(14) 0.0403(18) -0.0091(13) 0.0134(14) -0.0006(12) C13 0.0384(19) 0.0216(15) 0.054(2) -0.0061(15) 0.0069(17) 0.0037(14) C14 0.043(2) 0.0216(15) 0.051(2) 0.0088(15) 0.0043(17) 0.0027(14) C15 0.0328(18) 0.0277(15) 0.0358(17) 0.0089(14) 0.0023(14) 0.0060(13) C16 0.033(2) 0.039(2) 0.056(2) 0.0023(18) -0.0072(18) 0.0137(16) C17 0.0229(18) 0.045(2) 0.072(3) -0.010(2) 0.0041(18) 0.0082(15) C18 0.0241(16) 0.0375(18) 0.058(2) -0.0121(17) 0.0164(16) -0.0004(14) N2 0.0210(12) 0.0206(11) 0.0210(11) -0.0030(9) 0.0047(9) 0.0028(9) C21 0.0203(13) 0.0221(13) 0.0215(12) -0.0020(11) 0.0061(10) 0.0004(10) C22 0.0315(16) 0.0339(16) 0.0292(15) -0.0006(13) 0.0134(13) -0.0053(13) C23 0.0272(17) 0.050(2) 0.037(2) -0.0106(16) 0.0167(16) -0.0095(15) C24 0.0223(15) 0.048(2) 0.0384(19) -0.0156(16) 0.0083(13) 0.0025(14) C25 0.0263(15) 0.0321(15) 0.0276(15) -0.0061(13) 0.0015(12) 0.0084(13) N3 0.0236(12) 0.0256(12) 0.0347(14) -0.0087(11) 0.0134(11) -0.0053(10) C31 0.0167(13) 0.0307(15) 0.0306(15) -0.0056(12) 0.0077(11) -0.0002(11) C32 0.0239(15) 0.050(2) 0.0321(16) -0.0079(15) 0.0036(13) 0.0024(15) C33 0.0298(19) 0.063(2) 0.0395(19) -0.0235(19) 0.0055(16) -0.0038(19) C34 0.0306(19) 0.048(2) 0.055(2) -0.0281(18) 0.0167(18) -0.0140(19) C35 0.0329(17) 0.0311(16) 0.052(2) -0.0150(15) 0.0201(17) -0.0097(15) Pt1A 0.0245(13) 0.0363(15) 0.0378(15) 0.0134(10) 0.0058(10) 0.0008(10) C1A 0.038(11) 0.038(9) 0.042(8) 0.013(8) 0.001(9) 0.002(9) C2A 0.028(7) 0.040(11) 0.063(11) -0.003(10) 0.007(9) 0.007(8) C3A 0.035(10) 0.023(9) 0.048(10) 0.006(9) 0.011(11) 0.004(8) B1A 0.029(4) 0.027(4) 0.029(4) -0.004(4) 0.013(4) -0.003(4) C11A 0.035(6) 0.028(6) 0.033(6) -0.005(5) 0.016(5) -0.001(5) C12A 0.046(8) 0.032(8) 0.032(7) -0.003(7) 0.011(7) 0.002(7) C13A 0.052(8) 0.034(8) 0.036(8) 0.001(8) 0.011(8) 0.006(8) C14A 0.051(8) 0.031(7) 0.038(7) 0.002(7) 0.014(7) 0.005(7) C15A 0.046(7) 0.030(6) 0.043(6) 0.001(5) 0.016(6) 0.003(6) C16A 0.053(7) 0.028(7) 0.045(8) 0.000(7) 0.022(7) -0.002(7) C17A 0.052(8) 0.029(8) 0.044(9) -0.003(8) 0.025(7) -0.004(8) C18A 0.044(7) 0.030(8) 0.040(8) -0.004(8) 0.024(6) -0.003(7) N2A 0.025(4) 0.027(4) 0.026(4) -0.002(4) 0.007(4) -0.001(4) C21A 0.024(4) 0.027(4) 0.025(4) -0.005(4) 0.006(4) 0.001(4) C22A 0.024(4) 0.031(4) 0.027(4) -0.006(4) 0.005(4) 0.002(4) C23A 0.025(4) 0.039(4) 0.031(4) -0.008(4) 0.010(4) -0.001(4) C24A 0.027(4) 0.040(5) 0.032(5) -0.006(4) 0.012(4) -0.004(5) C25A 0.026(4) 0.035(5) 0.029(5) -0.004(5) 0.011(4) -0.005(4) N3A 0.022(4) 0.038(4) 0.033(4) -0.004(4) 0.009(4) -0.002(4) C31A 0.025(4) 0.035(4) 0.035(4) -0.009(4) 0.011(4) -0.004(4) C32A 0.029(4) 0.041(4) 0.044(4) -0.016(4) 0.013(4) -0.008(4) C33A 0.030(5) 0.046(5) 0.045(5) -0.020(4) 0.013(5) -0.009(5) C34A 0.028(5) 0.051(5) 0.041(5) -0.016(4) 0.009(5) -0.005(5) C35A 0.025(5) 0.048(4) 0.037(4) -0.009(4) 0.007(5) -0.002(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 C1 2.046(4) . ? Pt1 C3 2.068(4) . ? Pt1 C2 2.084(4) . ? Pt1 N2 2.130(3) . ? Pt1 N3 2.147(3) . ? Pt1 H11 1.99(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? B1 C21 1.634(5) . ? B1 C31 1.636(5) . ? B1 C15 1.637(5) . ? B1 C11 1.646(5) . ? C11 C18 1.540(5) . ? C11 C12 1.541(4) . ? C11 H11 0.96(4) . ? C12 C13 1.536(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.526(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.550(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.550(5) . ? C15 H15 1.0000 . ? C16 C17 1.531(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.537(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? N2 C25 1.350(4) . ? N2 C21 1.365(4) . ? C21 C22 1.405(4) . ? C22 C23 1.391(5) . ? C22 H22 0.9500 . ? C23 C24 1.372(6) . ? C23 H23 0.9500 . ? C24 C25 1.377(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N3 C35 1.350(4) . ? N3 C31 1.364(4) . ? C31 C32 1.404(5) . ? C32 C33 1.399(6) . ? C32 H32 0.9500 . ? C33 C34 1.369(7) . ? C33 H33 0.9500 . ? C34 C35 1.378(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? 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 C1 Pt1 C3 87.60(17) . . ? C1 Pt1 C2 87.88(19) . . ? C3 Pt1 C2 89.8(2) . . ? C1 Pt1 N2 95.03(15) . . ? C3 Pt1 N2 91.59(14) . . ? C2 Pt1 N2 176.83(16) . . ? C1 Pt1 N3 95.89(15) . . ? C3 Pt1 N3 175.73(13) . . ? C2 Pt1 N3 92.82(17) . . ? N2 Pt1 N3 85.65(10) . . ? C1 Pt1 H11 173.6(12) . . ? C3 Pt1 H11 89.3(12) . . ? C2 Pt1 H11 86.6(12) . . ? N2 Pt1 H11 90.6(12) . . ? N3 Pt1 H11 87.5(12) . . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Pt1 C2 H2A 109.5 . . ? Pt1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Pt1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Pt1 C3 H3A 109.5 . . ? Pt1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Pt1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C21 B1 C31 102.2(2) . . ? C21 B1 C15 115.3(3) . . ? C31 B1 C15 115.0(3) . . ? C21 B1 C11 110.6(3) . . ? C31 B1 C11 111.1(3) . . ? C15 B1 C11 103.0(3) . . ? C18 C11 C12 114.9(3) . . ? C18 C11 B1 110.7(3) . . ? C12 C11 B1 109.9(3) . . ? C18 C11 H11 97(2) . . ? C12 C11 H11 105(2) . . ? B1 C11 H11 118(2) . . ? C13 C12 C11 114.2(3) . . ? C13 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? C13 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C12 114.3(3) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 C15 115.7(3) . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14B 108.4 . . ? C15 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? C14 C15 C16 111.0(3) . . ? C14 C15 B1 110.6(3) . . ? C16 C15 B1 109.9(3) . . ? C14 C15 H15 108.4 . . ? C16 C15 H15 108.4 . . ? B1 C15 H15 108.4 . . ? C17 C16 C15 115.8(3) . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 115.0(3) . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C17 C18 C11 113.6(3) . . ? C17 C18 H18A 108.9 . . ? C11 C18 H18A 108.9 . . ? C17 C18 H18B 108.9 . . ? C11 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C25 N2 C21 121.0(3) . . ? C25 N2 Pt1 123.6(2) . . ? C21 N2 Pt1 115.3(2) . . ? N2 C21 C22 117.6(3) . . ? N2 C21 B1 116.1(3) . . ? C22 C21 B1 126.3(3) . . ? C23 C22 C21 120.9(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 119.7(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 118.2(3) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? N2 C25 C24 122.5(3) . . ? N2 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C35 N3 C31 121.3(3) . . ? C35 N3 Pt1 123.8(3) . . ? C31 N3 Pt1 114.7(2) . . ? N3 C31 C32 117.6(3) . . ? N3 C31 B1 116.5(3) . . ? C32 C31 B1 125.8(3) . . ? C33 C32 C31 120.6(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 119.8(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 118.5(4) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? N3 C35 C34 122.2(4) . . ? N3 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? 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 C21 B1 C11 C18 -172.0(3) . . . . ? C31 B1 C11 C18 -59.3(3) . . . . ? C15 B1 C11 C18 64.3(3) . . . . ? C21 B1 C11 C12 60.0(3) . . . . ? C31 B1 C11 C12 172.7(3) . . . . ? C15 B1 C11 C12 -63.7(3) . . . . ? C18 C11 C12 C13 -68.0(4) . . . . ? B1 C11 C12 C13 57.6(4) . . . . ? C11 C12 C13 C14 -44.7(5) . . . . ? C12 C13 C14 C15 42.6(5) . . . . ? C13 C14 C15 C16 68.9(4) . . . . ? C13 C14 C15 B1 -53.4(4) . . . . ? C21 B1 C15 C14 -59.3(4) . . . . ? C31 B1 C15 C14 -177.8(3) . . . . ? C11 B1 C15 C14 61.2(4) . . . . ? C21 B1 C15 C16 177.7(3) . . . . ? C31 B1 C15 C16 59.2(4) . . . . ? C11 B1 C15 C16 -61.7(4) . . . . ? C14 C15 C16 C17 -69.0(4) . . . . ? B1 C15 C16 C17 53.7(5) . . . . ? C15 C16 C17 C18 -42.2(5) . . . . ? C16 C17 C18 C11 43.1(5) . . . . ? C12 C11 C18 C17 68.8(4) . . . . ? B1 C11 C18 C17 -56.5(4) . . . . ? C25 N2 C21 C22 0.6(4) . . . . ? Pt1 N2 C21 C22 -178.1(2) . . . . ? C25 N2 C21 B1 178.1(3) . . . . ? Pt1 N2 C21 B1 -0.5(3) . . . . ? C31 B1 C21 N2 -67.0(3) . . . . ? C15 B1 C21 N2 167.6(3) . . . . ? C11 B1 C21 N2 51.4(4) . . . . ? C31 B1 C21 C22 110.4(3) . . . . ? C15 B1 C21 C22 -15.1(5) . . . . ? C11 B1 C21 C22 -131.3(3) . . . . ? N2 C21 C22 C23 -1.9(5) . . . . ? B1 C21 C22 C23 -179.2(3) . . . . ? C21 C22 C23 C24 2.5(6) . . . . ? C22 C23 C24 C25 -1.6(6) . . . . ? C21 N2 C25 C24 0.2(5) . . . . ? Pt1 N2 C25 C24 178.8(3) . . . . ? C23 C24 C25 N2 0.3(5) . . . . ? C35 N3 C31 C32 -1.8(5) . . . . ? Pt1 N3 C31 C32 173.3(2) . . . . ? C35 N3 C31 B1 -177.7(3) . . . . ? Pt1 N3 C31 B1 -2.6(3) . . . . ? C21 B1 C31 N3 69.0(3) . . . . ? C15 B1 C31 N3 -165.4(3) . . . . ? C11 B1 C31 N3 -49.0(4) . . . . ? C21 B1 C31 C32 -106.6(3) . . . . ? C15 B1 C31 C32 19.0(5) . . . . ? C11 B1 C31 C32 135.4(3) . . . . ? N3 C31 C32 C33 0.8(5) . . . . ? B1 C31 C32 C33 176.3(4) . . . . ? C31 C32 C33 C34 0.5(6) . . . . ? C32 C33 C34 C35 -0.9(7) . . . . ? C31 N3 C35 C34 1.4(6) . . . . ? Pt1 N3 C35 C34 -173.3(4) . . . . ? C33 C34 C35 N3 0.0(7) . . . . ? _refine_diff_density_max 3.469 _refine_diff_density_min -1.911 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 932584' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2364 #TrackingRef '19222_web_deposit_cif_file_2_AndreiN.Vedernikov_1365084323.2364_(MeO)2Bpy2_PtPh2(OH).cif' _audit_creation_method 'SHELXL-2012 & ZCIF' _chemical_name_systematic ; Pt-complex ; _chemical_name_common Pt-complex _chemical_formula_moiety 'C24 H25 B N2 O3 Pt, C4 H8 O' _chemical_formula_sum 'C28 H33 B N2 O4 Pt' _chemical_formula_weight 667.46 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' B B 0.0013 0.0007 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7630(7) _cell_length_b 12.1564(9) _cell_length_c 13.1947(10) _cell_angle_alpha 107.2164(10) _cell_angle_beta 103.3376(10) _cell_angle_gamma 97.3974(11) _cell_volume 1276.70(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7006 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 30.8 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.736 _exptl_crystal_F_000 660 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.015 _exptl_absorpt_coefficient_mu 5.533 _shelx_estimated_absorpt_T_min 0.444 _shelx_estimated_absorpt_T_max 0.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'three-circle diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 15028 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.444 _diffrn_reflns_theta_max 29.999 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 7376 _reflns_number_gt 6508 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex2 (Bruker, 2010)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'ShelXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'ShelXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material 'Apex2, SHELXL-2012' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.9050P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7376 _refine_ls_number_parameters 355 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.57237(2) 0.06502(2) 0.24727(2) 0.01677(4) Uani 1 1 d . . . . . O1 O 0.5836(3) -0.0171(2) 0.09665(18) 0.0248(5) Uani 1 1 d D . . . . H1 H 0.507(4) -0.068(4) 0.063(4) 0.09(2) Uiso 1 1 d D . . . . B1 B 0.6823(4) 0.2959(3) 0.4095(3) 0.0221(7) Uani 1 1 d . . . . . O2 O 0.6022(3) 0.17351(19) 0.40954(17) 0.0194(4) Uani 1 1 d . . . . . C2 C 0.4729(4) 0.1764(3) 0.4600(3) 0.0277(7) Uani 1 1 d . . . . . H2A H 0.4983 0.2490 0.5238 0.039(7) Uiso 1 1 calc R . . . . H2B H 0.4587 0.1081 0.4845 0.039(7) Uiso 1 1 calc R . . . . H2C H 0.3737 0.1740 0.4060 0.039(7) Uiso 1 1 calc R . . . . O3 O 0.7099(3) 0.3892(2) 0.51211(19) 0.0289(5) Uani 1 1 d . . . . . C3 C 0.8091(5) 0.3779(4) 0.6088(3) 0.0370(9) Uani 1 1 d . . . . . H3A H 0.8991 0.3438 0.5910 0.085(11) Uiso 1 1 calc R . . . . H3B H 0.7461 0.3263 0.6359 0.085(11) Uiso 1 1 calc R . . . . H3C H 0.8504 0.4558 0.6661 0.085(11) Uiso 1 1 calc R . . . . N1 N 0.4983(3) 0.2206(2) 0.2171(2) 0.0201(5) Uani 1 1 d . . . . . C11 C 0.5593(4) 0.3183(3) 0.3091(3) 0.0218(6) Uani 1 1 d . . . . . C12 C 0.5155(4) 0.4243(3) 0.3087(3) 0.0281(7) Uani 1 1 d . . . . . H12 H 0.5562 0.4924 0.3731 0.018(9) Uiso 1 1 calc R . . . . C13 C 0.4124(4) 0.4308(3) 0.2144(3) 0.0327(8) Uani 1 1 d . . . . . H13 H 0.3811 0.5027 0.2140 0.042(12) Uiso 1 1 calc R . . . . C14 C 0.3559(4) 0.3313(3) 0.1210(3) 0.0298(8) Uani 1 1 d . . . . . H14 H 0.2870 0.3341 0.0551 0.044(12) Uiso 1 1 calc R . . . . C15 C 0.4014(4) 0.2274(3) 0.1251(3) 0.0253(7) Uani 1 1 d . . . . . H15 H 0.3629 0.1589 0.0609 0.020(9) Uiso 1 1 calc R . . . . N2 N 0.8087(3) 0.1627(2) 0.2876(2) 0.0190(5) Uani 1 1 d . . . . . C21 C 0.8400(4) 0.2666(3) 0.3698(3) 0.0215(6) Uani 1 1 d . . . . . C22 C 0.9937(4) 0.3369(3) 0.4050(3) 0.0245(7) Uani 1 1 d . . . . . H22 H 1.0179 0.4107 0.4629 0.031(10) Uiso 1 1 calc R . . . . C23 C 1.1117(4) 0.3012(3) 0.3571(3) 0.0276(7) Uani 1 1 d . . . . . H23 H 1.2163 0.3495 0.3819 0.030(10) Uiso 1 1 calc R . . . . C24 C 1.0750(4) 0.1935(3) 0.2721(3) 0.0276(7) Uani 1 1 d . . . . . H24 H 1.1536 0.1671 0.2374 0.044(12) Uiso 1 1 calc R . . . . C25 C 0.9206(4) 0.1254(3) 0.2389(3) 0.0225(6) Uani 1 1 d . . . . . H25 H 0.8936 0.0515 0.1810 0.039(12) Uiso 1 1 calc R . . . . C31 C 0.3427(4) -0.0279(3) 0.2080(3) 0.0218(6) Uani 1 1 d . . . . . C32 C 0.2333(4) -0.0464(3) 0.1061(3) 0.0244(7) Uani 1 1 d . . . . . H32 H 0.2669 -0.0165 0.0541 0.034(11) Uiso 1 1 calc R . . . . C33 C 0.0760(4) -0.1078(3) 0.0791(3) 0.0289(7) Uani 1 1 d . . . . . H33 H 0.0041 -0.1196 0.0090 0.031(10) Uiso 1 1 calc R . . . . C34 C 0.0229(4) -0.1520(3) 0.1533(3) 0.0334(8) Uani 1 1 d . . . . . H34 H -0.0853 -0.1921 0.1355 0.033(11) Uiso 1 1 calc R . . . . C35 C 0.1305(4) -0.1367(3) 0.2537(3) 0.0324(8) Uani 1 1 d . . . . . H35 H 0.0962 -0.1672 0.3052 0.023(9) Uiso 1 1 calc R . . . . C36 C 0.2881(4) -0.0770(3) 0.2801(3) 0.0269(7) Uani 1 1 d . . . . . H36 H 0.3607 -0.0692 0.3488 0.026(10) Uiso 1 1 calc R . . . . C41 C 0.6555(4) -0.0654(3) 0.2943(3) 0.0206(6) Uani 1 1 d . . . . . C42 C 0.7613(4) -0.0386(3) 0.3993(3) 0.0245(7) Uani 1 1 d . . . . . H42 H 0.7931 0.0406 0.4483 0.028(10) Uiso 1 1 calc R . . . . C43 C 0.8208(4) -0.1270(3) 0.4331(3) 0.0283(7) Uani 1 1 d . . . . . H43 H 0.8920 -0.1075 0.5051 0.031(10) Uiso 1 1 calc R . . . . C44 C 0.7775(4) -0.2419(3) 0.3633(3) 0.0313(8) Uani 1 1 d . . . . . H44 H 0.8178 -0.3020 0.3866 0.046(12) Uiso 1 1 calc R . . . . C45 C 0.6741(5) -0.2692(3) 0.2585(3) 0.0330(8) Uani 1 1 d . . . . . H45 H 0.6445 -0.3483 0.2093 0.036(11) Uiso 1 1 calc R . . . . C46 C 0.6133(4) -0.1816(3) 0.2245(3) 0.0285(7) Uani 1 1 d . . . . . H46 H 0.5419 -0.2017 0.1525 0.039(11) Uiso 1 1 calc R . . . . O5 O 0.7920(4) 0.5261(3) 0.0390(3) 0.0528(8) Uani 1 1 d . . . . . C51 C 0.6911(6) 0.4124(4) -0.0027(4) 0.0522(12) Uani 1 1 d . . . . . H51A H 0.6940 0.3702 -0.0787 0.083(13) Uiso 1 1 calc R . . . . H51B H 0.5789 0.4183 -0.0045 0.083(13) Uiso 1 1 calc R . . . . C52 C 0.7547(5) 0.3484(4) 0.0747(4) 0.0515(12) Uani 1 1 d . . . . . H52A H 0.7046 0.3614 0.1361 0.095(15) Uiso 1 1 calc R . . . . H52B H 0.7360 0.2627 0.0349 0.095(15) Uiso 1 1 calc R . . . . C53 C 0.9292(6) 0.4033(4) 0.1159(4) 0.0476(11) Uani 1 1 d . . . . . H53A H 0.9872 0.3672 0.0629 0.085(14) Uiso 1 1 calc R . . . . H53B H 0.9784 0.3967 0.1888 0.085(14) Uiso 1 1 calc R . . . . C54 C 0.9282(5) 0.5301(4) 0.1248(4) 0.0424(10) Uani 1 1 d . . . . . H54A H 0.9189 0.5756 0.1981 0.073(12) Uiso 1 1 calc R . . . . H54B H 1.0281 0.5675 0.1145 0.073(12) 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 0.01600(6) 0.01927(6) 0.01743(6) 0.00846(4) 0.00558(4) 0.00508(4) O1 0.0273(12) 0.0289(13) 0.0172(11) 0.0059(10) 0.0071(10) 0.0057(11) B1 0.0229(17) 0.0203(17) 0.0251(17) 0.0086(14) 0.0071(14) 0.0085(14) O2 0.0196(10) 0.0232(11) 0.0190(10) 0.0087(9) 0.0084(8) 0.0077(9) C2 0.0252(17) 0.037(2) 0.0247(16) 0.0104(15) 0.0131(14) 0.0097(15) O3 0.0342(13) 0.0260(13) 0.0248(12) 0.0059(10) 0.0058(10) 0.0113(11) C3 0.039(2) 0.040(2) 0.0262(18) 0.0077(16) 0.0030(16) 0.0114(18) N1 0.0174(12) 0.0222(13) 0.0243(13) 0.0113(11) 0.0070(10) 0.0064(10) C11 0.0202(15) 0.0235(16) 0.0258(16) 0.0111(13) 0.0083(12) 0.0082(13) C12 0.0324(18) 0.0215(17) 0.0334(18) 0.0096(14) 0.0123(15) 0.0103(14) C13 0.0329(19) 0.0303(19) 0.046(2) 0.0212(17) 0.0151(17) 0.0161(16) C14 0.0261(17) 0.039(2) 0.0341(19) 0.0236(17) 0.0084(14) 0.0130(15) C15 0.0221(16) 0.0316(18) 0.0259(16) 0.0141(15) 0.0077(13) 0.0064(14) N2 0.0197(12) 0.0189(13) 0.0210(12) 0.0098(11) 0.0060(10) 0.0052(10) C21 0.0212(15) 0.0238(16) 0.0233(15) 0.0133(13) 0.0055(12) 0.0070(13) C22 0.0249(16) 0.0198(16) 0.0278(17) 0.0093(13) 0.0040(13) 0.0047(13) C23 0.0167(15) 0.0297(18) 0.0388(19) 0.0202(16) 0.0028(13) 0.0022(13) C24 0.0223(16) 0.037(2) 0.0316(18) 0.0180(16) 0.0113(14) 0.0114(14) C25 0.0236(15) 0.0264(17) 0.0245(16) 0.0131(14) 0.0100(13) 0.0122(13) C31 0.0183(14) 0.0198(15) 0.0298(16) 0.0085(13) 0.0105(13) 0.0054(12) C32 0.0247(16) 0.0224(16) 0.0273(16) 0.0099(14) 0.0071(13) 0.0056(13) C33 0.0219(16) 0.0269(18) 0.0304(18) 0.0048(15) 0.0007(14) 0.0033(14) C34 0.0236(17) 0.0262(18) 0.051(2) 0.0118(17) 0.0152(16) 0.0028(14) C35 0.0298(18) 0.032(2) 0.043(2) 0.0196(17) 0.0160(16) 0.0051(15) C36 0.0257(17) 0.0322(19) 0.0287(17) 0.0171(15) 0.0080(14) 0.0095(14) C41 0.0160(14) 0.0242(16) 0.0246(15) 0.0117(13) 0.0060(12) 0.0056(12) C42 0.0215(15) 0.0288(18) 0.0252(16) 0.0131(14) 0.0053(13) 0.0053(13) C43 0.0236(16) 0.038(2) 0.0301(18) 0.0191(16) 0.0078(14) 0.0101(15) C44 0.0284(18) 0.034(2) 0.046(2) 0.0273(18) 0.0149(16) 0.0143(15) C45 0.035(2) 0.0206(17) 0.044(2) 0.0115(16) 0.0102(17) 0.0088(15) C46 0.0286(17) 0.0257(18) 0.0298(18) 0.0111(15) 0.0030(14) 0.0065(14) O5 0.054(2) 0.0448(18) 0.055(2) 0.0263(16) -0.0046(16) 0.0092(15) C51 0.040(2) 0.049(3) 0.054(3) 0.015(2) -0.001(2) -0.005(2) C52 0.044(3) 0.039(2) 0.078(3) 0.026(2) 0.021(2) 0.009(2) C53 0.052(3) 0.038(2) 0.048(3) 0.016(2) 0.001(2) 0.013(2) C54 0.038(2) 0.039(2) 0.045(2) 0.0163(19) 0.0004(18) 0.0067(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 Pt1 O1 1.974(2) . ? Pt1 C41 2.026(3) . ? Pt1 C31 2.045(3) . ? Pt1 O2 2.091(2) . ? Pt1 N2 2.113(3) . ? Pt1 N1 2.191(3) . ? O1 H1 0.795(10) . ? B1 O3 1.430(4) . ? B1 O2 1.562(4) . ? B1 C11 1.619(5) . ? B1 C21 1.632(5) . ? O2 C2 1.440(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C3 1.423(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? N1 C15 1.343(4) . ? N1 C11 1.362(4) . ? C11 C12 1.392(4) . ? C12 C13 1.389(5) . ? C12 H12 0.9500 . ? C13 C14 1.381(5) . ? C13 H13 0.9500 . ? C14 C15 1.385(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? N2 C21 1.345(4) . ? N2 C25 1.346(4) . ? C21 C22 1.393(4) . ? C22 C23 1.383(5) . ? C22 H22 0.9500 . ? C23 C24 1.389(5) . ? C23 H23 0.9500 . ? C24 C25 1.390(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C31 C32 1.396(5) . ? C31 C36 1.401(4) . ? C32 C33 1.391(5) . ? C32 H32 0.9500 . ? C33 C34 1.386(5) . ? C33 H33 0.9500 . ? C34 C35 1.382(5) . ? C34 H34 0.9500 . ? C35 C36 1.388(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C46 1.384(5) . ? C41 C42 1.396(4) . ? C42 C43 1.396(5) . ? C42 H42 0.9500 . ? C43 C44 1.372(5) . ? C43 H43 0.9500 . ? C44 C45 1.384(5) . ? C44 H44 0.9500 . ? C45 C46 1.392(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? O5 C51 1.416(5) . ? O5 C54 1.427(5) . ? C51 C52 1.510(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.489(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.512(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 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 O1 Pt1 C41 88.48(11) . . ? O1 Pt1 C31 90.21(12) . . ? C41 Pt1 C31 89.45(12) . . ? O1 Pt1 O2 168.77(9) . . ? C41 Pt1 O2 93.74(11) . . ? C31 Pt1 O2 100.81(11) . . ? O1 Pt1 N2 89.92(10) . . ? C41 Pt1 N2 91.16(11) . . ? C31 Pt1 N2 179.38(11) . . ? O2 Pt1 N2 79.05(9) . . ? O1 Pt1 N1 97.45(10) . . ? C41 Pt1 N1 172.96(11) . . ? C31 Pt1 N1 94.29(11) . . ? O2 Pt1 N1 79.71(9) . . ? N2 Pt1 N1 85.09(10) . . ? Pt1 O1 H1 111(4) . . ? O3 B1 O2 113.6(3) . . ? O3 B1 C11 111.6(3) . . ? O2 B1 C11 104.4(3) . . ? O3 B1 C21 116.9(3) . . ? O2 B1 C21 101.8(2) . . ? C11 B1 C21 107.5(3) . . ? C2 O2 B1 114.4(2) . . ? C2 O2 Pt1 122.18(19) . . ? B1 O2 Pt1 102.15(17) . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 O3 B1 117.6(3) . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C15 N1 C11 120.3(3) . . ? C15 N1 Pt1 128.6(2) . . ? C11 N1 Pt1 111.1(2) . . ? N1 C11 C12 119.5(3) . . ? N1 C11 B1 113.6(3) . . ? C12 C11 B1 126.8(3) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 118.9(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N1 C15 C14 121.9(3) . . ? N1 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C21 N2 C25 122.1(3) . . ? C21 N2 Pt1 113.5(2) . . ? C25 N2 Pt1 124.4(2) . . ? N2 C21 C22 118.4(3) . . ? N2 C21 B1 112.9(3) . . ? C22 C21 B1 128.6(3) . . ? C23 C22 C21 121.0(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.1(3) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 118.5(3) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? N2 C25 C24 120.9(3) . . ? N2 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C32 C31 C36 116.9(3) . . ? C32 C31 Pt1 120.7(2) . . ? C36 C31 Pt1 122.3(2) . . ? C33 C32 C31 121.3(3) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C34 C33 C32 120.7(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C33 118.7(3) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 120.6(3) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 121.6(3) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? C46 C41 C42 118.2(3) . . ? C46 C41 Pt1 122.1(2) . . ? C42 C41 Pt1 119.7(2) . . ? C41 C42 C43 120.6(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C44 C43 C42 120.6(3) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 119.2(3) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C44 C45 C46 120.6(3) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C41 C46 C45 120.9(3) . . ? C41 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C51 O5 C54 109.5(3) . . ? O5 C51 C52 106.3(4) . . ? O5 C51 H51A 110.5 . . ? C52 C51 H51A 110.5 . . ? O5 C51 H51B 110.5 . . ? C52 C51 H51B 110.5 . . ? H51A C51 H51B 108.7 . . ? C53 C52 C51 102.5(4) . . ? C53 C52 H52A 111.3 . . ? C51 C52 H52A 111.3 . . ? C53 C52 H52B 111.3 . . ? C51 C52 H52B 111.3 . . ? H52A C52 H52B 109.2 . . ? C52 C53 C54 101.9(4) . . ? C52 C53 H53A 111.4 . . ? C54 C53 H53A 111.4 . . ? C52 C53 H53B 111.4 . . ? C54 C53 H53B 111.4 . . ? H53A C53 H53B 109.3 . . ? O5 C54 C53 105.8(3) . . ? O5 C54 H54A 110.6 . . ? C53 C54 H54A 110.6 . . ? O5 C54 H54B 110.6 . . ? C53 C54 H54B 110.6 . . ? H54A C54 H54B 108.7 . . ? 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 O3 B1 O2 C2 43.3(4) . . . . ? C11 B1 O2 C2 -78.4(3) . . . . ? C21 B1 O2 C2 169.8(2) . . . . ? O3 B1 O2 Pt1 177.4(2) . . . . ? C11 B1 O2 Pt1 55.7(2) . . . . ? C21 B1 O2 Pt1 -56.1(2) . . . . ? O2 B1 O3 C3 59.0(4) . . . . ? C11 B1 O3 C3 176.7(3) . . . . ? C21 B1 O3 C3 -59.1(4) . . . . ? C15 N1 C11 C12 2.5(5) . . . . ? Pt1 N1 C11 C12 -175.2(2) . . . . ? C15 N1 C11 B1 -176.4(3) . . . . ? Pt1 N1 C11 B1 5.9(3) . . . . ? O3 B1 C11 N1 -164.6(3) . . . . ? O2 B1 C11 N1 -41.5(3) . . . . ? C21 B1 C11 N1 66.1(3) . . . . ? O3 B1 C11 C12 16.6(5) . . . . ? O2 B1 C11 C12 139.7(3) . . . . ? C21 B1 C11 C12 -112.7(4) . . . . ? N1 C11 C12 C13 -1.1(5) . . . . ? B1 C11 C12 C13 177.7(3) . . . . ? C11 C12 C13 C14 -0.8(5) . . . . ? C12 C13 C14 C15 1.3(5) . . . . ? C11 N1 C15 C14 -2.1(5) . . . . ? Pt1 N1 C15 C14 175.1(2) . . . . ? C13 C14 C15 N1 0.1(5) . . . . ? C25 N2 C21 C22 -0.2(4) . . . . ? Pt1 N2 C21 C22 178.4(2) . . . . ? C25 N2 C21 B1 176.2(3) . . . . ? Pt1 N2 C21 B1 -5.3(3) . . . . ? O3 B1 C21 N2 165.7(3) . . . . ? O2 B1 C21 N2 41.4(3) . . . . ? C11 B1 C21 N2 -68.0(3) . . . . ? O3 B1 C21 C22 -18.4(5) . . . . ? O2 B1 C21 C22 -142.7(3) . . . . ? C11 B1 C21 C22 107.9(4) . . . . ? N2 C21 C22 C23 -0.1(5) . . . . ? B1 C21 C22 C23 -175.7(3) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C22 C23 C24 C25 -0.4(5) . . . . ? C21 N2 C25 C24 0.1(5) . . . . ? Pt1 N2 C25 C24 -178.3(2) . . . . ? C23 C24 C25 N2 0.2(5) . . . . ? C36 C31 C32 C33 1.9(5) . . . . ? Pt1 C31 C32 C33 -178.9(3) . . . . ? C31 C32 C33 C34 0.3(5) . . . . ? C32 C33 C34 C35 -1.6(5) . . . . ? C33 C34 C35 C36 0.7(6) . . . . ? C34 C35 C36 C31 1.6(6) . . . . ? C32 C31 C36 C35 -2.9(5) . . . . ? Pt1 C31 C36 C35 177.9(3) . . . . ? C46 C41 C42 C43 -0.9(5) . . . . ? Pt1 C41 C42 C43 -179.6(2) . . . . ? C41 C42 C43 C44 0.6(5) . . . . ? C42 C43 C44 C45 0.2(5) . . . . ? C43 C44 C45 C46 -0.8(6) . . . . ? C42 C41 C46 C45 0.4(5) . . . . ? Pt1 C41 C46 C45 179.0(3) . . . . ? C44 C45 C46 C41 0.5(6) . . . . ? C54 O5 C51 C52 9.7(5) . . . . ? O5 C51 C52 C53 -29.6(5) . . . . ? C51 C52 C53 C54 36.6(5) . . . . ? C51 O5 C54 C53 13.9(5) . . . . ? C52 C53 C54 O5 -31.8(5) . . . . ? _refine_diff_density_max 1.067 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.132 _database_code_depnum_ccdc_archive 'CCDC 932585' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2369 #TrackingRef '19223_web_deposit_cif_file_3_AndreiN.Vedernikov_1365084323.2369_Na_BO_MeOBpy2_Pt(OMe)2.cif' _audit_creation_method 'SHELXL-2012 & ZCIF' _chemical_name_systematic ; Pt-complex ; _chemical_name_common Pt-complex _chemical_formula_moiety '2(C44 H68 B2 N4 Na2 O8 Pt2), (C4 H8 O)' _chemical_formula_sum 'C23 H36 B N2 Na O4.25 Pt' _chemical_formula_weight 637.43 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' B B 0.0013 0.0007 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.5793(11) _cell_length_b 17.8585(11) _cell_length_c 17.6641(11) _cell_angle_alpha 90 _cell_angle_beta 116.3130(8) _cell_angle_gamma 90 _cell_volume 4970.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17591 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 30.1 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.703 _exptl_crystal_F_000 2528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_absorpt_coefficient_mu 5.695 _shelx_estimated_absorpt_T_min 0.411 _shelx_estimated_absorpt_T_max 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.412 _exptl_absorpt_correction_T_max 0.505 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'three-circle diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 60095 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.281 _diffrn_reflns_theta_max 29.999 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 14457 _reflns_number_gt 12135 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex2 (Bruker, 2010)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'ShelXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'ShelXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material 'Apex2, SHELXL-2012' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+11.9000P] 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 14457 _refine_ls_number_parameters 615 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.29279(9) 0.53575(8) 0.29122(9) 0.0245(3) Uani 1 1 d . . . . . Pt1 Pt 0.11715(2) 0.45602(2) 0.29237(2) 0.02033(3) Uani 1 1 d . . . . . O1A O 0.24454(15) 0.44466(14) 0.35017(16) 0.0264(5) Uani 1 1 d . . . . . C1A C 0.2761(2) 0.4114(3) 0.4301(3) 0.0360(9) Uani 1 1 d . . . . . H1A1 H 0.2574 0.4401 0.4660 0.054 Uiso 1 1 calc R U . . . H1A2 H 0.3383 0.4107 0.4557 0.054 Uiso 1 1 calc R U . . . H1A3 H 0.2549 0.3599 0.4245 0.054 Uiso 1 1 calc R U . . . O2A O 0.13538(16) 0.55990(13) 0.34261(17) 0.0274(5) Uani 1 1 d . . . . . C2A C 0.1112(3) 0.5667(2) 0.4092(3) 0.0328(8) Uani 1 1 d . . . . . H2A1 H 0.0508 0.5550 0.3877 0.049 Uiso 1 1 calc R U . . . H2A2 H 0.1217 0.6180 0.4310 0.049 Uiso 1 1 calc R U . . . H2A3 H 0.1446 0.5317 0.4546 0.049 Uiso 1 1 calc R U . . . N1A N 0.10370(17) 0.35123(16) 0.24512(17) 0.0212(6) Uani 1 1 d . . . . . C11A C 0.0341(2) 0.30715(18) 0.2282(2) 0.0191(6) Uani 1 1 d . . . . . C12A C 0.0346(2) 0.23457(19) 0.1984(2) 0.0238(7) Uani 1 1 d . . . . . H12A H -0.0131 0.2032 0.1859 0.029 Uiso 1 1 calc R U . . . C13A C 0.1021(2) 0.2070(2) 0.1865(2) 0.0293(8) Uani 1 1 d . . . . . H13A H 0.1010 0.1573 0.1668 0.035 Uiso 1 1 calc R U . . . C14A C 0.1710(3) 0.2531(2) 0.2037(3) 0.0347(9) Uani 1 1 d . . . . . H14A H 0.2180 0.2362 0.1953 0.042 Uiso 1 1 calc R U . . . C15A C 0.1696(2) 0.3242(2) 0.2333(3) 0.0312(8) Uani 1 1 d . . . . . H15A H 0.2172 0.3559 0.2460 0.037 Uiso 1 1 calc R U . . . N2A N -0.00878(18) 0.47600(16) 0.23223(18) 0.0228(6) Uani 1 1 d . . . . . C21A C -0.0688(2) 0.42293(18) 0.2211(2) 0.0214(6) Uani 1 1 d . . . . . C22A C -0.1533(2) 0.4469(2) 0.1875(2) 0.0282(8) Uani 1 1 d . . . . . H22A H -0.1961 0.4115 0.1814 0.034 Uiso 1 1 calc R U . . . C23A C -0.1769(3) 0.5202(2) 0.1630(3) 0.0341(9) Uani 1 1 d . . . . . H23A H -0.2346 0.5352 0.1412 0.041 Uiso 1 1 calc R U . . . C24A C -0.1151(3) 0.5709(2) 0.1706(3) 0.0361(9) Uani 1 1 d . . . . . H24A H -0.1296 0.6211 0.1518 0.043 Uiso 1 1 calc R U . . . C25A C -0.0324(2) 0.5477(2) 0.2059(3) 0.0310(8) Uani 1 1 d . . . . . H25A H 0.0104 0.5831 0.2122 0.037 Uiso 1 1 calc R U . . . B1A B -0.0470(2) 0.3346(2) 0.2439(2) 0.0183(7) Uani 1 1 d . . . . . O3A O -0.12342(14) 0.28950(13) 0.18597(15) 0.0215(5) Uani 1 1 d . . . . . C3A C -0.1507(2) 0.2961(2) 0.0973(2) 0.0292(8) Uani 1 1 d . . . . . H3A1 H -0.2046 0.2695 0.0669 0.044 Uiso 1 1 calc R U . . . H3A2 H -0.1077 0.2743 0.0827 0.044 Uiso 1 1 calc R U . . . H3A3 H -0.1584 0.3491 0.0813 0.044 Uiso 1 1 calc R U . . . C31A C -0.0325(2) 0.31368(17) 0.3412(2) 0.0182(6) Uani 1 1 d . . . . . C32A C -0.0227(2) 0.2281(2) 0.3576(2) 0.0282(7) Uani 1 1 d . . . . . H32A H -0.0779 0.2053 0.3467 0.034 Uiso 1 1 calc R U . . . H32B H -0.0013 0.2039 0.3204 0.034 Uiso 1 1 calc R U . . . C33A C 0.0404(3) 0.2187(2) 0.4495(3) 0.0383(9) Uani 1 1 d . . . . . H33A H 0.0669 0.1685 0.4603 0.046 Uiso 1 1 calc R U . . . H33B H 0.0132 0.2269 0.4874 0.046 Uiso 1 1 calc R U . . . C34A C 0.1051(2) 0.2803(3) 0.4603(3) 0.0396(10) Uani 1 1 d . . . . . H34A H 0.1420 0.2657 0.4336 0.048 Uiso 1 1 calc R U . . . H34B H 0.1410 0.2912 0.5208 0.048 Uiso 1 1 calc R U . . . C35A C 0.0492(2) 0.3484(2) 0.4149(2) 0.0274(7) Uani 1 1 d . . . . . H35A H 0.0795 0.3814 0.3913 0.033 Uiso 1 1 calc R U . . . C36A C 0.0183(3) 0.3941(2) 0.4690(2) 0.0358(9) Uani 1 1 d . . . . . H36A H 0.0180 0.3633 0.5155 0.043 Uiso 1 1 calc R U . . . H36B H 0.0549 0.4384 0.4935 0.043 Uiso 1 1 calc R U . . . C37A C -0.0706(3) 0.4176(2) 0.4087(3) 0.0369(9) Uani 1 1 d . . . . . H37A H -0.0702 0.4588 0.3714 0.044 Uiso 1 1 calc R U . . . H37B H -0.1036 0.4331 0.4392 0.044 Uiso 1 1 calc R U . . . C38A C -0.1058(2) 0.3443(2) 0.3585(2) 0.0290(8) Uani 1 1 d . . . . . H38A H -0.1568 0.3546 0.3048 0.035 Uiso 1 1 calc R U . . . H38B H -0.1210 0.3081 0.3920 0.035 Uiso 1 1 calc R U . . . Na2 Na 0.76639(9) 0.23432(8) 0.20471(9) 0.0268(3) Uani 1 1 d . . . . . Pt2 Pt 0.60221(2) 0.32020(2) 0.24970(2) 0.02595(4) Uani 1 1 d . . . . . O1B O 0.5899(2) 0.21173(16) 0.21396(19) 0.0433(8) Uani 1 1 d . . . . . C1B C 0.5381(3) 0.1992(2) 0.1285(3) 0.0416(10) Uani 1 1 d . . . . . H1B1 H 0.4796 0.2131 0.1150 0.062 Uiso 1 1 calc R U . . . H1B2 H 0.5402 0.1460 0.1156 0.062 Uiso 1 1 calc R U . . . H1B3 H 0.5581 0.2295 0.0946 0.062 Uiso 1 1 calc R U . . . O2B O 0.67717(16) 0.33139(17) 0.19103(17) 0.0342(6) Uani 1 1 d . . . . . C2B C 0.6393(2) 0.3722(3) 0.1151(3) 0.0360(9) Uani 1 1 d . . . . . H2B1 H 0.5841 0.3501 0.0785 0.054 Uiso 1 1 calc R U . . . H2B2 H 0.6760 0.3705 0.0866 0.054 Uiso 1 1 calc R U . . . H2B3 H 0.6315 0.4243 0.1275 0.054 Uiso 1 1 calc R U . . . N1B N 0.5264(2) 0.30098(16) 0.30555(19) 0.0262(6) Uani 1 1 d . . . . . C11B C 0.4678(2) 0.35189(19) 0.3043(2) 0.0225(7) Uani 1 1 d . . . . . C12B C 0.4127(3) 0.3294(2) 0.3386(2) 0.0292(8) Uani 1 1 d . . . . . H12B H 0.3714 0.3638 0.3383 0.035 Uiso 1 1 calc R U . . . C13B C 0.4170(3) 0.2588(2) 0.3726(3) 0.0399(10) Uani 1 1 d . . . . . H13B H 0.3788 0.2445 0.3947 0.048 Uiso 1 1 calc R U . . . C14B C 0.4782(3) 0.2097(2) 0.3735(3) 0.0449(11) Uani 1 1 d . . . . . H14B H 0.4834 0.1611 0.3972 0.054 Uiso 1 1 calc R U . . . C15B C 0.5309(3) 0.2322(2) 0.3400(3) 0.0382(9) Uani 1 1 d . . . . . H15B H 0.5728 0.1981 0.3408 0.046 Uiso 1 1 calc R U . . . N2B N 0.61805(18) 0.42822(18) 0.28518(19) 0.0253(6) Uani 1 1 d . . . . . C21B C 0.5536(2) 0.47113(19) 0.2849(2) 0.0218(7) Uani 1 1 d . . . . . C22B C 0.5695(2) 0.5479(2) 0.3019(2) 0.0288(8) Uani 1 1 d . . . . . H22B H 0.5253 0.5792 0.3007 0.035 Uiso 1 1 calc R U . . . C23B C 0.6476(3) 0.5792(3) 0.3205(3) 0.0417(10) Uani 1 1 d . . . . . H23B H 0.6570 0.6313 0.3313 0.050 Uiso 1 1 calc R U . . . C24B C 0.7119(3) 0.5332(3) 0.3229(3) 0.0491(12) Uani 1 1 d . . . . . H24B H 0.7669 0.5528 0.3375 0.059 Uiso 1 1 calc R U . . . C25B C 0.6950(2) 0.4591(3) 0.3040(3) 0.0401(10) Uani 1 1 d . . . . . H25B H 0.7387 0.4279 0.3040 0.048 Uiso 1 1 calc R U . . . B1B B 0.4601(2) 0.4366(2) 0.2658(2) 0.0188(7) Uani 1 1 d . . . . . O3B O 0.42348(14) 0.48629(13) 0.31105(14) 0.0209(5) Uani 1 1 d . . . . . C3B C 0.4698(2) 0.4917(2) 0.4001(2) 0.0256(7) Uani 1 1 d . . . . . H3B1 H 0.4808 0.4414 0.4247 0.038 Uiso 1 1 calc R U . . . H3B2 H 0.4369 0.5204 0.4226 0.038 Uiso 1 1 calc R U . . . H3B3 H 0.5239 0.5172 0.4144 0.038 Uiso 1 1 calc R U . . . C31B C 0.3914(2) 0.44108(19) 0.1644(2) 0.0200(6) Uani 1 1 d . . . . . C32B C 0.3000(2) 0.4268(3) 0.1525(2) 0.0367(9) Uani 1 1 d . . . . . H32C H 0.3011 0.3999 0.2020 0.044 Uiso 1 1 calc R U . . . H32D H 0.2696 0.4748 0.1462 0.044 Uiso 1 1 calc R U . . . C33B C 0.2559(3) 0.3795(3) 0.0732(3) 0.0484(12) Uani 1 1 d . . . . . H33C H 0.2342 0.4109 0.0217 0.058 Uiso 1 1 calc R U . . . H33D H 0.2085 0.3503 0.0742 0.058 Uiso 1 1 calc R U . . . C34B C 0.3278(3) 0.3282(3) 0.0782(3) 0.0531(13) Uani 1 1 d . . . . . H34C H 0.3142 0.3053 0.0226 0.064 Uiso 1 1 calc R U . . . H34D H 0.3390 0.2880 0.1203 0.064 Uiso 1 1 calc R U . . . C35B C 0.4044(2) 0.3817(2) 0.1054(2) 0.0323(8) Uani 1 1 d . . . . . H35B H 0.4583 0.3534 0.1379 0.039 Uiso 1 1 calc R U . . . C36B C 0.4097(3) 0.4247(3) 0.0338(3) 0.0445(11) Uani 1 1 d . . . . . H36C H 0.4480 0.3993 0.0145 0.053 Uiso 1 1 calc R U . . . H36D H 0.3530 0.4300 -0.0146 0.053 Uiso 1 1 calc R U . . . C37B C 0.4443(3) 0.4988(3) 0.0715(3) 0.0448(11) Uani 1 1 d . . . . . H37C H 0.4337 0.5369 0.0272 0.054 Uiso 1 1 calc R U . . . H37D H 0.5061 0.4960 0.1088 0.054 Uiso 1 1 calc R U . . . C38B C 0.3948(3) 0.5164(2) 0.1219(3) 0.0343(9) Uani 1 1 d . . . . . H38C H 0.3369 0.5342 0.0842 0.041 Uiso 1 1 calc R U . . . H38D H 0.4242 0.5553 0.1650 0.041 Uiso 1 1 calc R U . . . C1M C 0.7651(3) 0.1616(3) 0.3773(3) 0.0421(10) Uani 1 1 d . . . . . H1M1 H 0.7324 0.1326 0.3999 0.063 Uiso 1 1 calc R U . . . H1M2 H 0.7594 0.2151 0.3860 0.063 Uiso 1 1 calc R U . . . H1M3 H 0.8251 0.1472 0.4067 0.063 Uiso 1 1 calc R U . . . O1M O 0.73376(18) 0.14689(15) 0.28921(17) 0.0318(6) Uani 1 1 d . . . . . H1M H 0.6815 0.1562 0.2646 0.038 Uiso 1 1 calc R U . . . C2M C 0.3237(3) 0.6283(3) 0.4764(3) 0.0376(9) Uani 1 1 d . . . . . H2M1 H 0.3803 0.6491 0.4922 0.056 Uiso 1 1 calc R U . . . H2M2 H 0.3290 0.5765 0.4963 0.056 Uiso 1 1 calc R U . . . H2M3 H 0.2946 0.6582 0.5021 0.056 Uiso 1 1 calc R U . . . O2M O 0.27604(16) 0.62984(14) 0.38709(15) 0.0259(5) Uani 1 1 d . . . . . H2M H 0.2322 0.6035 0.3728 0.031 Uiso 1 1 calc R U . . . O1S O 0.9361(8) 0.4445(8) -0.0454(7) 0.120(4) Uani 0.5 1 d D U P A -1 C1S C 0.9836(10) 0.4467(8) 0.0365(8) 0.060(2) Uani 0.5 1 d D U P A -1 H1S1 H 0.9964 0.3950 0.0589 0.072 Uiso 0.5 1 calc R U P A -1 H1S2 H 0.9524 0.4723 0.0639 0.072 Uiso 0.5 1 calc R U P A -1 C2S C 1.0651(10) 0.4876(10) 0.0571(12) 0.067(2) Uani 0.5 1 d D U P A -1 H2S1 H 1.1102 0.4535 0.0585 0.080 Uiso 0.5 1 calc R U P A -1 H2S2 H 1.0855 0.5151 0.1112 0.080 Uiso 0.5 1 calc R U P A -1 C3S C 1.0343(13) 0.5401(11) -0.0182(13) 0.107(2) Uani 0.5 1 d D U P A -1 H3S1 H 1.0383 0.5933 -0.0007 0.128 Uiso 0.5 1 calc R U P A -1 H3S2 H 1.0657 0.5328 -0.0523 0.128 Uiso 0.5 1 calc R U P A -1 C4S C 0.9435(12) 0.5147(14) -0.0646(14) 0.094(2) Uani 0.5 1 d D U P A -1 H4S1 H 0.9069 0.5472 -0.0491 0.113 Uiso 0.5 1 calc R U P A -1 H4S2 H 0.9244 0.5192 -0.1262 0.113 Uiso 0.5 1 calc R U P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0237(7) 0.0229(7) 0.0301(7) 0.0020(6) 0.0147(6) 0.0026(5) Pt1 0.01968(6) 0.01879(6) 0.02255(6) 0.00119(5) 0.00938(5) -0.00366(5) O1A 0.0198(12) 0.0308(14) 0.0295(13) 0.0027(10) 0.0118(10) -0.0048(10) C1A 0.0264(19) 0.047(2) 0.035(2) 0.0107(18) 0.0137(16) 0.0053(17) O2A 0.0289(13) 0.0213(12) 0.0319(14) -0.0026(10) 0.0134(11) -0.0059(10) C2A 0.035(2) 0.0280(18) 0.039(2) -0.0040(16) 0.0199(18) -0.0004(16) N1A 0.0215(13) 0.0247(14) 0.0198(13) 0.0000(11) 0.0115(11) -0.0015(11) C11A 0.0212(15) 0.0188(15) 0.0181(14) 0.0006(11) 0.0093(12) -0.0016(12) C12A 0.0252(16) 0.0224(16) 0.0254(16) -0.0034(13) 0.0128(14) -0.0009(13) C13A 0.035(2) 0.0259(18) 0.0308(19) -0.0066(14) 0.0181(16) 0.0002(15) C14A 0.035(2) 0.039(2) 0.041(2) -0.0112(17) 0.0262(18) -0.0002(17) C15A 0.0269(18) 0.037(2) 0.039(2) -0.0064(17) 0.0223(17) -0.0079(15) N2A 0.0227(14) 0.0172(13) 0.0231(14) 0.0004(11) 0.0052(11) -0.0015(11) C21A 0.0215(16) 0.0189(15) 0.0209(15) 0.0014(12) 0.0068(13) 0.0026(12) C22A 0.0200(16) 0.0263(18) 0.0308(18) -0.0003(14) 0.0045(14) 0.0003(13) C23A 0.0276(19) 0.0280(19) 0.035(2) 0.0021(16) 0.0032(16) 0.0055(15) C24A 0.038(2) 0.0205(17) 0.036(2) 0.0040(15) 0.0047(17) 0.0065(15) C25A 0.0326(19) 0.0169(16) 0.036(2) 0.0046(14) 0.0085(16) -0.0023(14) B1A 0.0169(16) 0.0173(16) 0.0211(17) 0.0006(13) 0.0087(13) -0.0006(13) O3A 0.0188(11) 0.0232(12) 0.0216(11) -0.0017(9) 0.0083(9) -0.0045(9) C3A 0.0283(18) 0.0308(19) 0.0241(17) -0.0032(14) 0.0074(15) -0.0069(15) C31A 0.0171(14) 0.0156(14) 0.0227(15) 0.0000(12) 0.0096(12) 0.0006(11) C32A 0.038(2) 0.0206(16) 0.0325(19) 0.0042(14) 0.0210(16) 0.0016(15) C33A 0.039(2) 0.035(2) 0.038(2) 0.0149(18) 0.0144(18) 0.0094(18) C34A 0.0253(19) 0.050(3) 0.035(2) 0.0169(19) 0.0062(16) 0.0025(17) C35A 0.0265(18) 0.0324(19) 0.0205(16) 0.0027(14) 0.0079(14) -0.0087(14) C36A 0.048(2) 0.031(2) 0.0271(19) -0.0038(16) 0.0160(18) -0.0062(18) C37A 0.048(2) 0.032(2) 0.036(2) -0.0056(17) 0.0241(19) 0.0068(18) C38A 0.0236(17) 0.038(2) 0.0294(18) 0.0006(15) 0.0151(15) 0.0054(15) Na2 0.0266(7) 0.0248(7) 0.0316(8) -0.0012(6) 0.0151(6) -0.0008(6) Pt2 0.02648(7) 0.02621(7) 0.02465(7) 0.00015(5) 0.01088(5) 0.01161(5) O1B 0.062(2) 0.0306(15) 0.0354(16) -0.0005(12) 0.0198(15) 0.0177(14) C1B 0.046(2) 0.027(2) 0.053(3) -0.0093(18) 0.023(2) -0.0064(18) O2B 0.0217(13) 0.0508(18) 0.0312(14) -0.0015(12) 0.0125(11) 0.0135(12) C2B 0.0233(18) 0.049(2) 0.038(2) -0.0006(18) 0.0152(16) 0.0024(17) N1B 0.0365(17) 0.0210(14) 0.0209(14) 0.0020(11) 0.0125(13) 0.0077(12) C11B 0.0255(16) 0.0224(16) 0.0190(15) -0.0018(12) 0.0093(13) -0.0010(13) C12B 0.037(2) 0.0272(18) 0.0287(18) -0.0006(14) 0.0188(16) -0.0010(15) C13B 0.054(3) 0.036(2) 0.041(2) 0.0029(18) 0.031(2) -0.0079(19) C14B 0.073(3) 0.025(2) 0.044(2) 0.0055(18) 0.033(2) 0.000(2) C15B 0.058(3) 0.0231(18) 0.037(2) 0.0072(16) 0.024(2) 0.0113(18) N2B 0.0164(13) 0.0330(16) 0.0248(14) -0.0027(12) 0.0078(11) 0.0033(12) C21B 0.0184(15) 0.0259(17) 0.0200(15) -0.0023(12) 0.0074(12) 0.0021(12) C22B 0.0269(18) 0.0273(18) 0.0349(19) -0.0069(15) 0.0161(16) -0.0034(14) C23B 0.036(2) 0.036(2) 0.054(3) -0.016(2) 0.021(2) -0.0160(18) C24B 0.028(2) 0.059(3) 0.064(3) -0.020(2) 0.024(2) -0.017(2) C25B 0.0209(18) 0.054(3) 0.045(2) -0.012(2) 0.0146(17) 0.0001(17) B1B 0.0183(16) 0.0202(16) 0.0188(16) -0.0005(13) 0.0091(14) 0.0039(13) O3B 0.0188(11) 0.0268(12) 0.0169(11) -0.0007(9) 0.0077(9) 0.0059(9) C3B 0.0280(17) 0.0296(18) 0.0182(15) -0.0032(13) 0.0095(14) 0.0053(14) C31B 0.0161(14) 0.0251(16) 0.0202(15) -0.0001(12) 0.0092(12) 0.0032(12) C32B 0.0210(17) 0.062(3) 0.0261(19) -0.0002(18) 0.0093(15) -0.0043(17) C33B 0.027(2) 0.066(3) 0.043(3) -0.009(2) 0.0077(19) -0.015(2) C34B 0.047(3) 0.045(3) 0.052(3) -0.022(2) 0.009(2) -0.010(2) C35B 0.0284(19) 0.039(2) 0.0252(18) -0.0060(15) 0.0078(15) 0.0080(16) C36B 0.034(2) 0.073(3) 0.026(2) 0.001(2) 0.0134(17) 0.014(2) C37B 0.045(3) 0.058(3) 0.037(2) 0.020(2) 0.024(2) 0.010(2) C38B 0.032(2) 0.0302(19) 0.036(2) 0.0075(16) 0.0106(17) 0.0049(16) C1M 0.048(3) 0.049(3) 0.034(2) -0.0071(19) 0.022(2) -0.012(2) O1M 0.0375(15) 0.0299(14) 0.0311(14) -0.0026(11) 0.0180(12) -0.0008(11) C2M 0.031(2) 0.044(2) 0.033(2) 0.0003(18) 0.0095(17) 0.0036(18) O2M 0.0246(12) 0.0264(12) 0.0255(12) -0.0026(10) 0.0101(10) -0.0046(10) O1S 0.125(7) 0.133(7) 0.087(6) -0.015(6) 0.033(5) -0.041(6) C1S 0.075(5) 0.048(4) 0.057(4) 0.006(3) 0.028(4) -0.024(4) C2S 0.050(4) 0.067(4) 0.068(4) 0.021(3) 0.012(3) 0.010(3) C3S 0.093(5) 0.122(4) 0.116(4) -0.038(3) 0.056(4) -0.013(4) C4S 0.084(4) 0.141(4) 0.068(4) -0.022(3) 0.044(3) -0.029(3) _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 Na1 O1A 2.288(3) . ? Na1 O3B 2.338(3) . ? Na1 O1M 2.364(3) 2_655 ? Na1 O2M 2.494(3) . ? Na1 C3B 2.949(4) . ? Na1 Pt1 3.4085(14) . ? Na1 Na2 3.705(2) 2_655 ? Pt1 N2A 2.018(3) . ? Pt1 O1A 2.018(2) . ? Pt1 N1A 2.020(3) . ? Pt1 O2A 2.020(2) . ? O1A C1A 1.400(5) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? O2A C2A 1.421(5) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? N1A C15A 1.353(4) . ? N1A C11A 1.372(4) . ? C11A C12A 1.400(5) . ? C11A B1A 1.644(5) . ? C12A C13A 1.384(5) . ? C12A H12A 0.9500 . ? C13A C14A 1.384(5) . ? C13A H13A 0.9500 . ? C14A C15A 1.379(5) . ? C14A H14A 0.9500 . ? C15A H15A 0.9500 . ? N2A C25A 1.364(4) . ? N2A C21A 1.366(4) . ? C21A C22A 1.401(5) . ? C21A B1A 1.630(5) . ? C22A C23A 1.384(5) . ? C22A H22A 0.9500 . ? C23A C24A 1.373(6) . ? C23A H23A 0.9500 . ? C24A C25A 1.368(5) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? B1A O3A 1.511(4) . ? B1A C31A 1.665(5) . ? O3A C3A 1.426(4) . ? O3A Na2 2.324(3) 1_455 ? C3A Na2 3.066(4) 1_455 ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C31A C32A 1.550(5) . ? C31A C38A 1.551(5) . ? C31A C35A 1.576(5) . ? C32A C33A 1.516(6) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A C34A 1.532(6) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A C35A 1.546(5) . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C35A C36A 1.530(5) . ? C35A H35A 1.0000 . ? C36A C37A 1.509(6) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A C38A 1.548(6) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? Na2 O2B 2.278(3) . ? Na2 O3A 2.324(3) 1_655 ? Na2 O2M 2.365(3) 2_645 ? Na2 O1M 2.399(3) . ? Na2 C3A 3.066(4) 1_655 ? Na2 Pt2 3.6534(14) . ? Na2 Na1 3.705(2) 2_645 ? Pt2 N1B 2.009(3) . ? Pt2 N2B 2.009(3) . ? Pt2 O2B 2.015(3) . ? Pt2 O1B 2.019(3) . ? O1B C1B 1.393(5) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? O2B C2B 1.407(5) . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? N1B C15B 1.358(5) . ? N1B C11B 1.367(4) . ? C11B C12B 1.408(5) . ? C11B B1B 1.639(5) . ? C12B C13B 1.384(5) . ? C12B H12B 0.9500 . ? C13B C14B 1.383(7) . ? C13B H13B 0.9500 . ? C14B C15B 1.363(6) . ? C14B H14B 0.9500 . ? C15B H15B 0.9500 . ? N2B C25B 1.358(5) . ? N2B C21B 1.366(4) . ? C21B C22B 1.406(5) . ? C21B B1B 1.645(5) . ? C22B C23B 1.381(5) . ? C22B H22B 0.9500 . ? C23B C24B 1.383(6) . ? C23B H23B 0.9500 . ? C24B C25B 1.365(6) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? B1B O3B 1.515(4) . ? B1B C31B 1.660(5) . ? O3B C3B 1.418(4) . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C31B C32B 1.546(5) . ? C31B C38B 1.555(5) . ? C31B C35B 1.573(5) . ? C32B C33B 1.521(6) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33B C34B 1.531(7) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B C35B 1.543(6) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? C35B C36B 1.517(6) . ? C35B H35B 1.0000 . ? C36B C37B 1.485(7) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B C38B 1.528(6) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C1M O1M 1.427(5) . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? O1M Na1 2.364(3) 2_645 ? O1M H1M 0.8400 . ? C2M O2M 1.421(5) . ? C2M H2M1 0.9800 . ? C2M H2M2 0.9800 . ? C2M H2M3 0.9800 . ? O2M Na2 2.365(3) 2_655 ? O2M H2M 0.8400 . ? O1S C1S 1.311(16) . ? O1S C4S 1.322(17) . ? C1S C2S 1.502(9) . ? C2S C3S 1.518(10) . ? C3S C4S 1.504(9) . ? 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 O1A Na1 O3B 101.60(10) . . ? O1A Na1 O1M 148.91(11) . 2_655 ? O3B Na1 O1M 109.05(10) . 2_655 ? O1A Na1 O2M 89.47(10) . . ? O3B Na1 O2M 123.82(10) . . ? O1M Na1 O2M 77.94(9) 2_655 . ? O1A Na1 C3B 90.61(11) . . ? O3B Na1 C3B 28.20(8) . . ? O1M Na1 C3B 119.07(11) 2_655 . ? O2M Na1 C3B 98.34(10) . . ? O1A Na1 Pt1 34.97(6) . . ? O3B Na1 Pt1 132.36(8) . . ? O1M Na1 Pt1 114.60(8) 2_655 . ? O2M Na1 Pt1 84.12(7) . . ? C3B Na1 Pt1 125.57(9) . . ? O1A Na1 Na2 120.51(8) . 2_655 ? O3B Na1 Na2 128.63(8) . 2_655 ? O1M Na1 Na2 39.26(7) 2_655 2_655 ? O2M Na1 Na2 39.04(6) . 2_655 ? C3B Na1 Na2 117.83(9) . 2_655 ? Pt1 Na1 Na2 97.86(4) . 2_655 ? N2A Pt1 O1A 175.32(11) . . ? N2A Pt1 N1A 92.65(11) . . ? O1A Pt1 N1A 90.93(11) . . ? N2A Pt1 O2A 89.55(11) . . ? O1A Pt1 O2A 86.88(10) . . ? N1A Pt1 O2A 177.77(11) . . ? N2A Pt1 Na1 135.09(8) . . ? O1A Pt1 Na1 40.52(7) . . ? N1A Pt1 Na1 108.96(8) . . ? O2A Pt1 Na1 69.59(8) . . ? C1A O1A Pt1 114.1(2) . . ? C1A O1A Na1 134.4(2) . . ? Pt1 O1A Na1 104.51(11) . . ? O1A C1A H1A1 109.5 . . ? O1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? O1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C2A O2A Pt1 113.2(2) . . ? O2A C2A H2A1 109.5 . . ? O2A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? O2A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C15A N1A C11A 120.2(3) . . ? C15A N1A Pt1 116.3(2) . . ? C11A N1A Pt1 123.5(2) . . ? N1A C11A C12A 117.4(3) . . ? N1A C11A B1A 123.2(3) . . ? C12A C11A B1A 119.3(3) . . ? C13A C12A C11A 122.3(3) . . ? C13A C12A H12A 118.8 . . ? C11A C12A H12A 118.8 . . ? C14A C13A C12A 118.8(3) . . ? C14A C13A H13A 120.6 . . ? C12A C13A H13A 120.6 . . ? C15A C14A C13A 118.1(3) . . ? C15A C14A H14A 121.0 . . ? C13A C14A H14A 121.0 . . ? N1A C15A C14A 123.2(3) . . ? N1A C15A H15A 118.4 . . ? C14A C15A H15A 118.4 . . ? C25A N2A C21A 120.2(3) . . ? C25A N2A Pt1 116.3(2) . . ? C21A N2A Pt1 123.4(2) . . ? N2A C21A C22A 117.1(3) . . ? N2A C21A B1A 123.6(3) . . ? C22A C21A B1A 119.3(3) . . ? C23A C22A C21A 122.3(3) . . ? C23A C22A H22A 118.8 . . ? C21A C22A H22A 118.8 . . ? C24A C23A C22A 118.7(4) . . ? C24A C23A H23A 120.7 . . ? C22A C23A H23A 120.7 . . ? C25A C24A C23A 118.7(4) . . ? C25A C24A H24A 120.7 . . ? C23A C24A H24A 120.7 . . ? N2A C25A C24A 122.8(4) . . ? N2A C25A H25A 118.6 . . ? C24A C25A H25A 118.6 . . ? O3A B1A C21A 107.9(3) . . ? O3A B1A C11A 107.7(3) . . ? C21A B1A C11A 112.0(3) . . ? O3A B1A C31A 105.2(2) . . ? C21A B1A C31A 112.6(3) . . ? C11A B1A C31A 111.1(3) . . ? C3A O3A B1A 117.7(3) . . ? C3A O3A Na2 107.25(19) . 1_455 ? B1A O3A Na2 132.6(2) . 1_455 ? O3A C3A Na2 46.38(15) . 1_455 ? O3A C3A H3A1 109.5 . . ? Na2 C3A H3A1 63.5 1_455 . ? O3A C3A H3A2 109.5 . . ? Na2 C3A H3A2 130.7 1_455 . ? H3A1 C3A H3A2 109.5 . . ? O3A C3A H3A3 109.5 . . ? Na2 C3A H3A3 118.9 1_455 . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C32A C31A C38A 110.2(3) . . ? C32A C31A C35A 104.4(3) . . ? C38A C31A C35A 103.4(3) . . ? C32A C31A B1A 111.6(3) . . ? C38A C31A B1A 111.3(3) . . ? C35A C31A B1A 115.5(3) . . ? C33A C32A C31A 106.1(3) . . ? C33A C32A H32A 110.5 . . ? C31A C32A H32A 110.5 . . ? C33A C32A H32B 110.5 . . ? C31A C32A H32B 110.5 . . ? H32A C32A H32B 108.7 . . ? C32A C33A C34A 101.7(3) . . ? C32A C33A H33A 111.4 . . ? C34A C33A H33A 111.4 . . ? C32A C33A H33B 111.4 . . ? C34A C33A H33B 111.4 . . ? H33A C33A H33B 109.3 . . ? C33A C34A C35A 103.5(3) . . ? C33A C34A H34A 111.1 . . ? C35A C34A H34A 111.1 . . ? C33A C34A H34B 111.1 . . ? C35A C34A H34B 111.1 . . ? H34A C34A H34B 109.0 . . ? C36A C35A C34A 114.6(3) . . ? C36A C35A C31A 106.2(3) . . ? C34A C35A C31A 104.8(3) . . ? C36A C35A H35A 110.3 . . ? C34A C35A H35A 110.3 . . ? C31A C35A H35A 110.3 . . ? C37A C36A C35A 104.5(3) . . ? C37A C36A H36A 110.9 . . ? C35A C36A H36A 110.9 . . ? C37A C36A H36B 110.9 . . ? C35A C36A H36B 110.9 . . ? H36A C36A H36B 108.9 . . ? C36A C37A C38A 101.3(3) . . ? C36A C37A H37A 111.5 . . ? C38A C37A H37A 111.5 . . ? C36A C37A H37B 111.5 . . ? C38A C37A H37B 111.5 . . ? H37A C37A H37B 109.3 . . ? C37A C38A C31A 104.8(3) . . ? C37A C38A H38A 110.8 . . ? C31A C38A H38A 110.8 . . ? C37A C38A H38B 110.8 . . ? C31A C38A H38B 110.8 . . ? H38A C38A H38B 108.9 . . ? O2B Na2 O3A 103.91(11) . 1_655 ? O2B Na2 O2M 122.31(11) . 2_645 ? O3A Na2 O2M 105.45(10) 1_655 2_645 ? O2B Na2 O1M 102.59(11) . . ? O3A Na2 O1M 144.00(11) 1_655 . ? O2M Na2 O1M 79.83(10) 2_645 . ? O2B Na2 C3A 98.89(12) . 1_655 ? O3A Na2 C3A 26.37(9) 1_655 1_655 ? O2M Na2 C3A 87.23(10) 2_645 1_655 ? O1M Na2 C3A 158.45(12) . 1_655 ? O2B Na2 Pt2 29.57(8) . . ? O3A Na2 Pt2 129.91(8) 1_655 . ? O2M Na2 Pt2 116.15(8) 2_645 . ? O1M Na2 Pt2 73.02(7) . . ? C3A Na2 Pt2 128.45(9) 1_655 . ? O2B Na2 Na1 122.98(9) . 2_645 ? O3A Na2 Na1 131.88(8) 1_655 2_645 ? O2M Na2 Na1 41.62(7) 2_645 2_645 ? O1M Na2 Na1 38.59(7) . 2_645 ? C3A Na2 Na1 124.84(9) 1_655 2_645 ? Pt2 Na2 Na1 98.15(4) . 2_645 ? N1B Pt2 N2B 92.36(12) . . ? N1B Pt2 O2B 175.73(12) . . ? N2B Pt2 O2B 91.91(12) . . ? N1B Pt2 O1B 89.27(13) . . ? N2B Pt2 O1B 178.18(13) . . ? O2B Pt2 O1B 86.46(13) . . ? N1B Pt2 Na2 142.70(8) . . ? N2B Pt2 Na2 117.21(8) . . ? O2B Pt2 Na2 33.91(8) . . ? O1B Pt2 Na2 60.97(10) . . ? C1B O1B Pt2 114.9(2) . . ? O1B C1B H1B1 109.5 . . ? O1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? O1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C2B O2B Pt2 113.6(2) . . ? C2B O2B Na2 120.5(2) . . ? Pt2 O2B Na2 116.52(14) . . ? O2B C2B H2B1 109.5 . . ? O2B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? O2B C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C15B N1B C11B 120.2(3) . . ? C15B N1B Pt2 117.0(3) . . ? C11B N1B Pt2 122.6(2) . . ? N1B C11B C12B 117.4(3) . . ? N1B C11B B1B 122.9(3) . . ? C12B C11B B1B 119.7(3) . . ? C13B C12B C11B 122.1(4) . . ? C13B C12B H12B 119.0 . . ? C11B C12B H12B 119.0 . . ? C14B C13B C12B 118.4(4) . . ? C14B C13B H13B 120.8 . . ? C12B C13B H13B 120.8 . . ? C15B C14B C13B 118.8(4) . . ? C15B C14B H14B 120.6 . . ? C13B C14B H14B 120.6 . . ? N1B C15B C14B 123.0(4) . . ? N1B C15B H15B 118.5 . . ? C14B C15B H15B 118.5 . . ? C25B N2B C21B 120.5(3) . . ? C25B N2B Pt2 116.8(3) . . ? C21B N2B Pt2 122.5(2) . . ? N2B C21B C22B 117.5(3) . . ? N2B C21B B1B 122.9(3) . . ? C22B C21B B1B 119.7(3) . . ? C23B C22B C21B 121.9(4) . . ? C23B C22B H22B 119.1 . . ? C21B C22B H22B 119.1 . . ? C22B C23B C24B 118.7(4) . . ? C22B C23B H23B 120.6 . . ? C24B C23B H23B 120.6 . . ? C25B C24B C23B 118.8(4) . . ? C25B C24B H24B 120.6 . . ? C23B C24B H24B 120.6 . . ? N2B C25B C24B 122.7(4) . . ? N2B C25B H25B 118.7 . . ? C24B C25B H25B 118.7 . . ? O3B B1B C11B 107.4(3) . . ? O3B B1B C21B 107.0(3) . . ? C11B B1B C21B 111.7(3) . . ? O3B B1B C31B 105.3(2) . . ? C11B B1B C31B 112.3(3) . . ? C21B B1B C31B 112.7(3) . . ? C3B O3B B1B 117.1(2) . . ? C3B O3B Na1 100.60(19) . . ? B1B O3B Na1 139.55(19) . . ? O3B C3B Na1 51.20(15) . . ? O3B C3B H3B1 109.5 . . ? Na1 C3B H3B1 118.5 . . ? O3B C3B H3B2 109.5 . . ? Na1 C3B H3B2 58.8 . . ? H3B1 C3B H3B2 109.5 . . ? O3B C3B H3B3 109.5 . . ? Na1 C3B H3B3 131.8 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C32B C31B C38B 109.8(3) . . ? C32B C31B C35B 104.3(3) . . ? C38B C31B C35B 102.4(3) . . ? C32B C31B B1B 110.7(3) . . ? C38B C31B B1B 113.4(3) . . ? C35B C31B B1B 115.6(3) . . ? C33B C32B C31B 106.9(3) . . ? C33B C32B H32C 110.3 . . ? C31B C32B H32C 110.3 . . ? C33B C32B H32D 110.3 . . ? C31B C32B H32D 110.3 . . ? H32C C32B H32D 108.6 . . ? C32B C33B C34B 102.1(3) . . ? C32B C33B H33C 111.4 . . ? C34B C33B H33C 111.4 . . ? C32B C33B H33D 111.4 . . ? C34B C33B H33D 111.4 . . ? H33C C33B H33D 109.2 . . ? C33B C34B C35B 103.4(4) . . ? C33B C34B H34C 111.1 . . ? C35B C34B H34C 111.1 . . ? C33B C34B H34D 111.1 . . ? C35B C34B H34D 111.1 . . ? H34C C34B H34D 109.1 . . ? C36B C35B C34B 114.8(4) . . ? C36B C35B C31B 107.0(3) . . ? C34B C35B C31B 105.1(3) . . ? C36B C35B H35B 109.9 . . ? C34B C35B H35B 109.9 . . ? C31B C35B H35B 109.9 . . ? C37B C36B C35B 104.0(3) . . ? C37B C36B H36C 111.0 . . ? C35B C36B H36C 111.0 . . ? C37B C36B H36D 111.0 . . ? C35B C36B H36D 111.0 . . ? H36C C36B H36D 109.0 . . ? C36B C37B C38B 102.6(4) . . ? C36B C37B H37C 111.2 . . ? C38B C37B H37C 111.2 . . ? C36B C37B H37D 111.2 . . ? C38B C37B H37D 111.2 . . ? H37C C37B H37D 109.2 . . ? C37B C38B C31B 105.0(3) . . ? C37B C38B H38C 110.8 . . ? C31B C38B H38C 110.8 . . ? C37B C38B H38D 110.8 . . ? C31B C38B H38D 110.8 . . ? H38C C38B H38D 108.8 . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? C1M O1M Na1 133.5(3) . 2_645 ? C1M O1M Na2 118.4(2) . . ? Na1 O1M Na2 102.15(11) 2_645 . ? C1M O1M H1M 109.5 . . ? Na1 O1M H1M 88.6 2_645 . ? Na2 O1M H1M 93.3 . . ? O2M C2M H2M1 109.5 . . ? O2M C2M H2M2 109.5 . . ? H2M1 C2M H2M2 109.5 . . ? O2M C2M H2M3 109.5 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C2M O2M Na2 128.9(2) . 2_655 ? C2M O2M Na1 123.5(2) . . ? Na2 O2M Na1 99.34(10) 2_655 . ? C2M O2M H2M 109.5 . . ? Na2 O2M H2M 105.5 2_655 . ? Na1 O2M H2M 77.7 . . ? C1S O1S C4S 99.6(16) . . ? O1S C1S C2S 110.8(12) . . ? C1S C2S C3S 99.0(6) . . ? C4S C3S C2S 99.9(7) . . ? O1S C4S C3S 110.4(12) . . ? 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 C15A N1A C11A C12A -0.2(5) . . . . ? Pt1 N1A C11A C12A -177.8(2) . . . . ? C15A N1A C11A B1A 177.9(3) . . . . ? Pt1 N1A C11A B1A 0.4(4) . . . . ? N1A C11A C12A C13A 0.4(5) . . . . ? B1A C11A C12A C13A -177.8(3) . . . . ? C11A C12A C13A C14A -0.8(6) . . . . ? C12A C13A C14A C15A 1.0(6) . . . . ? C11A N1A C15A C14A 0.5(6) . . . . ? Pt1 N1A C15A C14A 178.2(3) . . . . ? C13A C14A C15A N1A -0.9(6) . . . . ? C25A N2A C21A C22A -4.3(5) . . . . ? Pt1 N2A C21A C22A 172.4(3) . . . . ? C25A N2A C21A B1A 175.1(3) . . . . ? Pt1 N2A C21A B1A -8.3(5) . . . . ? N2A C21A C22A C23A 2.6(6) . . . . ? B1A C21A C22A C23A -176.8(3) . . . . ? C21A C22A C23A C24A 1.1(6) . . . . ? C22A C23A C24A C25A -3.0(6) . . . . ? C21A N2A C25A C24A 2.5(6) . . . . ? Pt1 N2A C25A C24A -174.4(3) . . . . ? C23A C24A C25A N2A 1.3(7) . . . . ? N2A C21A B1A O3A -151.3(3) . . . . ? C22A C21A B1A O3A 28.0(4) . . . . ? N2A C21A B1A C11A -33.0(4) . . . . ? C22A C21A B1A C11A 146.4(3) . . . . ? N2A C21A B1A C31A 93.0(4) . . . . ? C22A C21A B1A C31A -87.6(4) . . . . ? N1A C11A B1A O3A 155.8(3) . . . . ? C12A C11A B1A O3A -26.1(4) . . . . ? N1A C11A B1A C21A 37.3(4) . . . . ? C12A C11A B1A C21A -144.6(3) . . . . ? N1A C11A B1A C31A -89.5(4) . . . . ? C12A C11A B1A C31A 88.6(4) . . . . ? C21A B1A O3A C3A 60.0(4) . . . . ? C11A B1A O3A C3A -61.1(4) . . . . ? C31A B1A O3A C3A -179.7(3) . . . . ? C21A B1A O3A Na2 -99.6(3) . . . 1_455 ? C11A B1A O3A Na2 139.3(2) . . . 1_455 ? C31A B1A O3A Na2 20.8(4) . . . 1_455 ? B1A O3A C3A Na2 -164.4(3) . . . 1_455 ? O3A B1A C31A C32A 55.8(3) . . . . ? C21A B1A C31A C32A 173.1(3) . . . . ? C11A B1A C31A C32A -60.4(3) . . . . ? O3A B1A C31A C38A -67.7(3) . . . . ? C21A B1A C31A C38A 49.6(4) . . . . ? C11A B1A C31A C38A 176.1(3) . . . . ? O3A B1A C31A C35A 174.8(3) . . . . ? C21A B1A C31A C35A -67.9(4) . . . . ? C11A B1A C31A C35A 58.6(4) . . . . ? C38A C31A C32A C33A -90.6(4) . . . . ? C35A C31A C32A C33A 19.8(4) . . . . ? B1A C31A C32A C33A 145.2(3) . . . . ? C31A C32A C33A C34A -39.6(4) . . . . ? C32A C33A C34A C35A 44.0(4) . . . . ? C33A C34A C35A C36A 84.3(4) . . . . ? C33A C34A C35A C31A -31.7(4) . . . . ? C32A C31A C35A C36A -114.2(3) . . . . ? C38A C31A C35A C36A 1.1(4) . . . . ? B1A C31A C35A C36A 123.0(3) . . . . ? C32A C31A C35A C34A 7.5(4) . . . . ? C38A C31A C35A C34A 122.8(3) . . . . ? B1A C31A C35A C34A -115.4(3) . . . . ? C34A C35A C36A C37A -142.9(3) . . . . ? C31A C35A C36A C37A -27.6(4) . . . . ? C35A C36A C37A C38A 42.8(4) . . . . ? C36A C37A C38A C31A -42.4(4) . . . . ? C32A C31A C38A C37A 136.2(3) . . . . ? C35A C31A C38A C37A 25.1(4) . . . . ? B1A C31A C38A C37A -99.5(3) . . . . ? C15B N1B C11B C12B -1.0(5) . . . . ? Pt2 N1B C11B C12B 174.1(3) . . . . ? C15B N1B C11B B1B 178.5(3) . . . . ? Pt2 N1B C11B B1B -6.4(4) . . . . ? N1B C11B C12B C13B 0.1(5) . . . . ? B1B C11B C12B C13B -179.4(4) . . . . ? C11B C12B C13B C14B 0.8(6) . . . . ? C12B C13B C14B C15B -0.9(7) . . . . ? C11B N1B C15B C14B 0.9(6) . . . . ? Pt2 N1B C15B C14B -174.4(4) . . . . ? C13B C14B C15B N1B 0.1(7) . . . . ? C25B N2B C21B C22B 2.0(5) . . . . ? Pt2 N2B C21B C22B -173.1(3) . . . . ? C25B N2B C21B B1B -177.8(3) . . . . ? Pt2 N2B C21B B1B 7.1(4) . . . . ? N2B C21B C22B C23B -1.5(6) . . . . ? B1B C21B C22B C23B 178.3(4) . . . . ? C21B C22B C23B C24B -0.6(7) . . . . ? C22B C23B C24B C25B 2.3(8) . . . . ? C21B N2B C25B C24B -0.3(7) . . . . ? Pt2 N2B C25B C24B 175.1(4) . . . . ? C23B C24B C25B N2B -1.9(8) . . . . ? N1B C11B B1B O3B -152.8(3) . . . . ? C12B C11B B1B O3B 26.7(4) . . . . ? N1B C11B B1B C21B -35.8(4) . . . . ? C12B C11B B1B C21B 143.7(3) . . . . ? N1B C11B B1B C31B 91.9(4) . . . . ? C12B C11B B1B C31B -88.6(4) . . . . ? N2B C21B B1B O3B 152.6(3) . . . . ? C22B C21B B1B O3B -27.2(4) . . . . ? N2B C21B B1B C11B 35.4(4) . . . . ? C22B C21B B1B C11B -144.4(3) . . . . ? N2B C21B B1B C31B -92.1(4) . . . . ? C22B C21B B1B C31B 88.1(4) . . . . ? C11B B1B O3B C3B 59.3(4) . . . . ? C21B B1B O3B C3B -60.7(4) . . . . ? C31B B1B O3B C3B 179.1(3) . . . . ? C11B B1B O3B Na1 -97.3(3) . . . . ? C21B B1B O3B Na1 142.6(2) . . . . ? C31B B1B O3B Na1 22.5(4) . . . . ? B1B O3B C3B Na1 -164.8(3) . . . . ? O3B B1B C31B C32B -49.7(4) . . . . ? C11B B1B C31B C32B 66.9(4) . . . . ? C21B B1B C31B C32B -166.0(3) . . . . ? O3B B1B C31B C38B 74.2(3) . . . . ? C11B B1B C31B C38B -169.2(3) . . . . ? C21B B1B C31B C38B -42.1(4) . . . . ? O3B B1B C31B C35B -167.9(3) . . . . ? C11B B1B C31B C35B -51.4(4) . . . . ? C21B B1B C31B C35B 75.7(4) . . . . ? C38B C31B C32B C33B 93.2(4) . . . . ? C35B C31B C32B C33B -15.9(4) . . . . ? B1B C31B C32B C33B -140.9(3) . . . . ? C31B C32B C33B C34B 36.6(5) . . . . ? C32B C33B C34B C35B -42.9(5) . . . . ? C33B C34B C35B C36B -83.9(5) . . . . ? C33B C34B C35B C31B 33.4(5) . . . . ? C32B C31B C35B C36B 111.7(3) . . . . ? C38B C31B C35B C36B -2.7(4) . . . . ? B1B C31B C35B C36B -126.5(3) . . . . ? C32B C31B C35B C34B -10.8(4) . . . . ? C38B C31B C35B C34B -125.2(3) . . . . ? B1B C31B C35B C34B 111.0(4) . . . . ? C34B C35B C36B C37B 144.5(4) . . . . ? C31B C35B C36B C37B 28.3(4) . . . . ? C35B C36B C37B C38B -42.7(4) . . . . ? C36B C37B C38B C31B 41.4(4) . . . . ? C32B C31B C38B C37B -133.4(3) . . . . ? C35B C31B C38B C37B -23.1(4) . . . . ? B1B C31B C38B C37B 102.1(4) . . . . ? 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 O1M H1M O1B 0.84 1.76 2.554(4) 157 . O2M H2M O2A 0.84 1.73 2.563(3) 173 . _refine_diff_density_max 3.259 _refine_diff_density_min -1.654 _refine_diff_density_rms 0.123 _diffrn_radiation_monochromator graphite _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _exptl_crystal_id 'Vedern-Shrin BBNPtMeOMe_MeOH_OxPdt' _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 0.0334971 _diffrn_orient_matrix_UB_12 0.0422037 _diffrn_orient_matrix_UB_13 0.0369331 _diffrn_orient_matrix_UB_21 0.0076854 _diffrn_orient_matrix_UB_22 0.0218001 _diffrn_orient_matrix_UB_23 -0.0483025 _diffrn_orient_matrix_UB_31 -0.0533480 _diffrn_orient_matrix_UB_32 0.0296487 _diffrn_orient_matrix_UB_33 -0.0170694 _diffrn_source_voltage 50.00 _diffrn_source_current 30.00 _diffrn_measurement_specimen_support 'MiTeGen loop' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart Apex II' _iucr_refine_instructions_details 'See _shelx_res_file' _database_code_depnum_ccdc_archive 'CCDC 932586'