# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guillaume Berthon-Gelloz' _publ_contact_author_email GUILLAUME.BERTHON@GMAIL.COM _publ_section_title ; IPr* An Easily Accessible Highly Hindered N-Heterocyclic Carbene ; loop_ _publ_author_name 'Guillaume Berthon-Gelloz' 'Istvan E. Marko' 'J Reek' 'Maxime A. Siegler' 'A Spek' 'Bernard Tinant' # Attachment '8-IPrs-AgCl.cif' data_gbg1343 _database_code_depnum_ccdc_archive 'CCDC 743047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H66 Ag Cl N2 O' _chemical_formula_weight 1130.60 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting ' monoclinic ' _symmetry_space_group_name_H-M ' P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.331(4) _cell_length_b 19.066(5) _cell_length_c 24.981(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.84(2) _cell_angle_gamma 90.00 _cell_volume 5852(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 25.3 _exptl_crystal_description prism _exptl_crystal_colour ' colourless ' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'RU200 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method '120 images, \D\F 2\%' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52872 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.37 _reflns_number_total 10644 _reflns_number_gt 9025 _reflns_threshold_expression >2sigma(I) _computing_data_collection mar _computing_cell_refinement mar _computing_data_reduction marhkl _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+9.5026P] 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 10644 _refine_ls_number_parameters 732 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.421722(16) 0.748842(10) 0.250008(8) 0.02200(8) Uani 1 1 d . . . Cl Cl 0.56408(7) 0.82409(5) 0.27633(4) 0.0491(2) Uani 1 1 d . . . C1 C 0.2942(2) 0.67824(13) 0.23436(9) 0.0162(5) Uani 1 1 d . . . N2 N 0.18560(16) 0.68788(10) 0.22532(8) 0.0163(4) Uani 1 1 d . . . C3 C 0.1308(2) 0.62391(13) 0.21873(10) 0.0186(5) Uani 1 1 d . . . H3 H 0.0545 0.6171 0.2122 0.0455(13) Uiso 1 1 calc R . . C4 C 0.2080(2) 0.57412(13) 0.22347(10) 0.0190(5) Uani 1 1 d . . . H4 H 0.1968 0.5249 0.2207 0.0455(13) Uiso 1 1 calc R . . N5 N 0.30691(16) 0.60794(10) 0.23306(8) 0.0151(4) Uani 1 1 d . . . C6 C 0.1332(2) 0.75564(12) 0.22495(10) 0.0164(5) Uani 1 1 d . . . C7 C 0.1027(2) 0.78258(13) 0.27346(10) 0.0184(5) Uani 1 1 d . . . C8 C 0.0565(2) 0.84915(13) 0.27270(10) 0.0199(5) Uani 1 1 d . . . H8 H 0.0380 0.8692 0.3055 0.0455(13) Uiso 1 1 calc R . . C9 C 0.0366(2) 0.88722(13) 0.22554(10) 0.0196(5) Uani 1 1 d . . . C10 C 0.0664(2) 0.85798(13) 0.17774(10) 0.0198(5) Uani 1 1 d . . . H10 H 0.0524 0.8835 0.1452 0.0455(13) Uiso 1 1 calc R . . C11 C 0.11584(19) 0.79252(13) 0.17635(10) 0.0176(5) Uani 1 1 d . . . C12 C 0.1184(2) 0.74098(13) 0.32573(11) 0.0225(6) Uani 1 1 d . . . H12 H 0.1712 0.7028 0.3192 0.0455(13) Uiso 1 1 calc R . . C13 C 0.0137(2) 0.70432(14) 0.33926(10) 0.0253(6) Uani 1 1 d . . . C14 C 0.0184(3) 0.63443(16) 0.35506(12) 0.0344(7) Uani 1 1 d . . . H14 H 0.0859 0.6102 0.3572 0.0455(13) Uiso 1 1 calc R . . C15 C -0.0759(3) 0.59959(17) 0.36783(14) 0.0446(9) Uani 1 1 d . . . H15 H -0.0716 0.5519 0.3788 0.0455(13) Uiso 1 1 calc R . . C16 C -0.1748(3) 0.63327(18) 0.36473(13) 0.0413(8) Uani 1 1 d . . . H16 H -0.2384 0.6091 0.3734 0.0455(13) Uiso 1 1 calc R . . C17 C -0.1807(3) 0.70275(18) 0.34891(12) 0.0371(7) Uani 1 1 d . . . H17 H -0.2487 0.7265 0.3466 0.0455(13) Uiso 1 1 calc R . . C18 C -0.0873(3) 0.73791(16) 0.33631(12) 0.0303(6) Uani 1 1 d . . . H18 H -0.0924 0.7856 0.3255 0.0455(13) Uiso 1 1 calc R . . C19 C 0.1729(2) 0.78581(14) 0.37121(10) 0.0234(6) Uani 1 1 d . . . C20 C 0.2787(3) 0.80940(17) 0.36654(12) 0.0347(7) Uani 1 1 d . . . H20 H 0.3131 0.7987 0.3349 0.0455(13) Uiso 1 1 calc R . . C21 C 0.3347(3) 0.84781(18) 0.40667(13) 0.0395(8) Uani 1 1 d . . . H21 H 0.4074 0.8623 0.4029 0.0455(13) Uiso 1 1 calc R . . C22 C 0.2849(3) 0.86535(17) 0.45258(12) 0.0360(7) Uani 1 1 d . . . H22 H 0.3229 0.8916 0.4805 0.0455(13) Uiso 1 1 calc R . . C23 C 0.1789(3) 0.84398(16) 0.45698(11) 0.0323(7) Uani 1 1 d . . . H23 H 0.1435 0.8568 0.4879 0.0455(13) Uiso 1 1 calc R . . C24 C 0.1233(2) 0.80419(15) 0.41707(11) 0.0273(6) Uani 1 1 d . . . H24 H 0.0509 0.7894 0.4211 0.0455(13) Uiso 1 1 calc R . . C25 C 0.1532(2) 0.76330(13) 0.12379(10) 0.0193(5) Uani 1 1 d . . . H25 H 0.1719 0.7129 0.1310 0.0455(13) Uiso 1 1 calc R . . C26 C 0.2577(2) 0.79822(13) 0.10775(10) 0.0208(5) Uani 1 1 d . . . C27 C 0.2891(2) 0.79031(16) 0.05551(12) 0.0308(6) Uani 1 1 d . . . H27 H 0.2431 0.7657 0.0295 0.0455(13) Uiso 1 1 calc R . . C28 C 0.3869(3) 0.81813(17) 0.04143(13) 0.0358(7) Uani 1 1 d . . . H28 H 0.4064 0.8135 0.0056 0.0455(13) Uiso 1 1 calc R . . C29 C 0.4562(3) 0.85253(16) 0.07930(13) 0.0331(7) Uani 1 1 d . . . H29 H 0.5235 0.8709 0.0698 0.0455(13) Uiso 1 1 calc R . . C30 C 0.4264(2) 0.85993(15) 0.13102(12) 0.0302(6) Uani 1 1 d . . . H30 H 0.4738 0.8831 0.1573 0.0455(13) Uiso 1 1 calc R . . C31 C 0.3272(2) 0.83361(14) 0.14488(11) 0.0241(6) Uani 1 1 d . . . H31 H 0.3069 0.8400 0.1804 0.0455(13) Uiso 1 1 calc R . . C32 C 0.0614(2) 0.76327(16) 0.07921(11) 0.0254(6) Uani 1 1 d . . . C33 C -0.0021(3) 0.7035(2) 0.07152(12) 0.0385(8) Uani 1 1 d . . . H33 H 0.0118 0.6644 0.0947 0.0455(13) Uiso 1 1 calc R . . C34 C -0.0858(3) 0.6997(3) 0.03057(13) 0.0522(10) Uani 1 1 d . . . H34 H -0.1282 0.6582 0.0258 0.0455(13) Uiso 1 1 calc R . . C35 C -0.1067(3) 0.7557(3) -0.00264(14) 0.0539(12) Uani 1 1 d . . . H35 H -0.1635 0.7531 -0.0307 0.0455(13) Uiso 1 1 calc R . . C36 C -0.0459(3) 0.8160(2) 0.00436(13) 0.0494(10) Uani 1 1 d . . . H36 H -0.0617 0.8550 -0.0186 0.0455(13) Uiso 1 1 calc R . . C37 C 0.0393(3) 0.82037(18) 0.04517(12) 0.0358(7) Uani 1 1 d . . . H37 H 0.0817 0.8619 0.0496 0.0455(13) Uiso 1 1 calc R . . C38 C -0.0150(3) 0.95881(15) 0.22645(12) 0.0278(6) Uani 1 1 d D . . C39 C 0.41178(19) 0.57396(12) 0.23878(10) 0.0159(5) Uani 1 1 d . . . C40 C 0.4619(2) 0.55794(13) 0.19207(10) 0.0174(5) Uani 1 1 d . . . C41 C 0.5606(2) 0.52305(13) 0.19778(10) 0.0206(5) Uani 1 1 d . . . H41 H 0.5949 0.5103 0.1665 0.0455(13) Uiso 1 1 calc R . . C42 C 0.6110(2) 0.50613(14) 0.24822(11) 0.0224(5) Uani 1 1 d . . . C43 C 0.5605(2) 0.52518(14) 0.29365(10) 0.0222(5) Uani 1 1 d . . . H43 H 0.5956 0.5152 0.3281 0.0455(13) Uiso 1 1 calc R . . C44 C 0.4597(2) 0.55846(13) 0.28992(10) 0.0189(5) Uani 1 1 d . . . C45 C 0.4066(2) 0.57776(13) 0.13725(10) 0.0194(5) Uani 1 1 d . . . H45 H 0.3655 0.6220 0.1431 0.0455(13) Uiso 1 1 calc R . . C46 C 0.3218(2) 0.52438(14) 0.11626(10) 0.0219(5) Uani 1 1 d . . . C47 C 0.3257(2) 0.45435(15) 0.13144(12) 0.0288(6) Uani 1 1 d . . . H47 H 0.3852 0.4377 0.1547 0.0455(13) Uiso 1 1 calc R . . C48 C 0.2436(3) 0.40830(18) 0.11298(14) 0.0400(8) Uani 1 1 d . . . H48 H 0.2466 0.3606 0.1241 0.0455(13) Uiso 1 1 calc R . . C49 C 0.1578(3) 0.4315(2) 0.07852(14) 0.0454(9) Uani 1 1 d . . . H49 H 0.1015 0.4000 0.0661 0.0455(13) Uiso 1 1 calc R . . C50 C 0.1539(3) 0.5010(2) 0.06208(13) 0.0403(8) Uani 1 1 d . . . H50 H 0.0956 0.5170 0.0379 0.0455(13) Uiso 1 1 calc R . . C51 C 0.2349(2) 0.54681(17) 0.08098(11) 0.0299(6) Uani 1 1 d . . . H51 H 0.2315 0.5944 0.0698 0.0455(13) Uiso 1 1 calc R . . C52 C 0.4877(2) 0.59608(14) 0.09633(10) 0.0209(5) Uani 1 1 d . . . C53 C 0.5171(2) 0.66552(15) 0.09020(12) 0.0299(6) Uani 1 1 d . . . H53 H 0.4879 0.7005 0.1120 0.0455(13) Uiso 1 1 calc R . . C54 C 0.5887(3) 0.68492(17) 0.05263(13) 0.0386(8) Uani 1 1 d . . . H54 H 0.6082 0.7327 0.0488 0.0455(13) Uiso 1 1 calc R . . C55 C 0.6315(2) 0.63379(17) 0.02080(12) 0.0323(7) Uani 1 1 d . . . H55 H 0.6794 0.6467 -0.0054 0.0455(13) Uiso 1 1 calc R . . C56 C 0.6046(2) 0.56479(16) 0.02717(11) 0.0295(6) Uani 1 1 d . . . H56 H 0.6354 0.5298 0.0060 0.0455(13) Uiso 1 1 calc R . . C57 C 0.5323(2) 0.54556(15) 0.06463(11) 0.0255(6) Uani 1 1 d . . . H57 H 0.5134 0.4976 0.0685 0.0455(13) Uiso 1 1 calc R . . C58 C 0.4013(2) 0.57405(15) 0.34036(10) 0.0235(6) Uani 1 1 d . . . H58 H 0.3513 0.6144 0.3315 0.0455(13) Uiso 1 1 calc R . . C59 C 0.3301(2) 0.51226(16) 0.35527(11) 0.0277(6) Uani 1 1 d . . . C60 C 0.2662(2) 0.5196(2) 0.39878(12) 0.0405(8) Uani 1 1 d . . . H60 H 0.2657 0.5629 0.4176 0.0455(13) Uiso 1 1 calc R . . C61 C 0.2032(3) 0.4635(3) 0.41467(13) 0.0521(11) Uani 1 1 d . . . H61 H 0.1594 0.4692 0.4439 0.0455(13) Uiso 1 1 calc R . . C62 C 0.2042(3) 0.4001(2) 0.38841(15) 0.0503(10) Uani 1 1 d . . . H62 H 0.1631 0.3617 0.4001 0.0455(13) Uiso 1 1 calc R . . C63 C 0.2649(3) 0.39285(19) 0.34527(15) 0.0430(8) Uani 1 1 d . . . H63 H 0.2645 0.3495 0.3265 0.0455(13) Uiso 1 1 calc R . . C64 C 0.3272(2) 0.44860(16) 0.32866(12) 0.0313(6) Uani 1 1 d . . . H64 H 0.3684 0.4427 0.2985 0.0455(13) Uiso 1 1 calc R . . C65 C 0.4812(2) 0.59747(15) 0.38680(10) 0.0240(6) Uani 1 1 d . . . C66 C 0.5265(2) 0.55088(16) 0.42527(11) 0.0280(6) Uani 1 1 d . . . H66 H 0.5051 0.5030 0.4236 0.0455(13) Uiso 1 1 calc R . . C67 C 0.6017(2) 0.57277(17) 0.46594(11) 0.0315(7) Uani 1 1 d . . . H67 H 0.6325 0.5399 0.4915 0.0455(13) Uiso 1 1 calc R . . C68 C 0.6322(2) 0.64270(18) 0.46942(12) 0.0341(7) Uani 1 1 d . . . H68 H 0.6837 0.6579 0.4975 0.0455(13) Uiso 1 1 calc R . . C69 C 0.5876(3) 0.69021(17) 0.43196(12) 0.0359(7) Uani 1 1 d . . . H69 H 0.6082 0.7382 0.4343 0.0455(13) Uiso 1 1 calc R . . C70 C 0.5124(3) 0.66760(16) 0.39068(11) 0.0302(6) Uani 1 1 d . . . H70 H 0.4821 0.7004 0.3650 0.0455(13) Uiso 1 1 calc R . . C71 C 0.7195(2) 0.46921(18) 0.25263(13) 0.0328(7) Uani 1 1 d D . . H38A H -0.086(2) 0.9604(19) 0.2096(13) 0.0455(13) Uiso 1 1 d D . . H38B H -0.012(3) 0.9775(19) 0.2627(11) 0.0455(13) Uiso 1 1 d D . . H38C H 0.034(3) 0.9945(16) 0.2142(14) 0.0455(13) Uiso 1 1 d D . . H71A H 0.749(3) 0.4628(19) 0.2900(10) 0.0455(13) Uiso 1 1 d D . . H71B H 0.712(3) 0.4223(14) 0.2368(14) 0.0455(13) Uiso 1 1 d D . . H71C H 0.774(3) 0.4984(17) 0.2368(14) 0.0455(13) Uiso 1 1 d D . . O100 O 0.87402(19) 0.60348(17) 0.18430(10) 0.0588(8) Uani 1 1 d D B . C101 C 0.8188(3) 0.58239(19) 0.13569(13) 0.0394(8) Uani 1 1 d . . . H10A H 0.8186 0.6208 0.1090 0.0455(13) Uiso 1 1 calc R . . H10B H 0.7424 0.5704 0.1412 0.0455(13) Uiso 1 1 calc R . . C102 C 0.8758(4) 0.5201(2) 0.11598(19) 0.0618(11) Uani 1 1 d . . . H10C H 0.8386 0.5043 0.0819 0.0455(13) Uiso 1 1 calc R . . H10D H 0.8752 0.4823 0.1425 0.0455(13) Uiso 1 1 calc R . . H10E H 0.9512 0.5325 0.1105 0.0455(13) Uiso 1 1 calc R . . C103 C 0.8200(5) 0.6479(4) 0.2133(2) 0.118(3) Uani 1 1 d D . . H10F H 0.7445 0.6308 0.2149 0.0455(13) Uiso 1 1 calc R A 1 H10G H 0.8549 0.6493 0.2505 0.0455(13) Uiso 1 1 calc R A 1 C04A C 0.8177(5) 0.7102(3) 0.1936(2) 0.0469(16) Uani 0.680(8) 1 d PD B 1 H04A H 0.7766 0.7411 0.2159 0.0455(13) Uiso 0.680(8) 1 calc PR B 1 H04B H 0.7825 0.7092 0.1569 0.0455(13) Uiso 0.680(8) 1 calc PR B 1 H04C H 0.8922 0.7279 0.1929 0.0455(13) Uiso 0.680(8) 1 calc PR B 1 C04B C 0.7221(6) 0.6852(4) 0.2137(3) 0.023(2) Uani 0.320(8) 1 d PD B 2 H04D H 0.7185 0.7078 0.2488 0.0455(13) Uiso 0.320(8) 1 calc PR B 2 H04E H 0.6607 0.6528 0.2072 0.0455(13) Uiso 0.320(8) 1 calc PR B 2 H04F H 0.7186 0.7210 0.1855 0.0455(13) Uiso 0.320(8) 1 calc PR B 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 Ag 0.02009(12) 0.01824(12) 0.02752(13) -0.00262(7) 0.00120(8) -0.00414(8) Cl 0.0460(5) 0.0399(5) 0.0590(5) -0.0011(4) -0.0101(4) -0.0253(4) C1 0.0180(12) 0.0151(12) 0.0157(12) 0.0001(9) 0.0030(9) 0.0004(10) N2 0.0162(10) 0.0149(10) 0.0179(10) -0.0015(8) 0.0019(8) 0.0012(8) C3 0.0163(12) 0.0198(13) 0.0198(12) -0.0024(10) 0.0030(10) -0.0019(10) C4 0.0186(13) 0.0174(12) 0.0212(13) -0.0001(10) 0.0038(10) -0.0019(10) N5 0.0156(10) 0.0148(10) 0.0149(10) 0.0001(8) 0.0017(8) -0.0004(8) C6 0.0126(11) 0.0158(12) 0.0210(13) -0.0014(9) 0.0020(9) 0.0005(9) C7 0.0176(12) 0.0191(13) 0.0188(12) -0.0014(10) 0.0028(10) -0.0012(10) C8 0.0175(12) 0.0207(13) 0.0221(13) -0.0048(10) 0.0047(10) 0.0017(10) C9 0.0151(12) 0.0171(12) 0.0265(13) -0.0024(10) 0.0018(10) 0.0003(10) C10 0.0190(13) 0.0194(13) 0.0208(13) 0.0021(10) -0.0001(10) 0.0001(10) C11 0.0133(12) 0.0204(13) 0.0191(12) -0.0028(10) 0.0023(9) -0.0008(10) C12 0.0286(15) 0.0202(13) 0.0194(13) -0.0016(10) 0.0060(11) 0.0041(11) C13 0.0378(16) 0.0233(14) 0.0160(13) -0.0041(10) 0.0091(11) -0.0046(12) C14 0.0474(19) 0.0264(15) 0.0311(16) -0.0024(12) 0.0124(14) -0.0007(13) C15 0.072(3) 0.0236(16) 0.0405(19) -0.0044(13) 0.0207(17) -0.0135(16) C16 0.052(2) 0.0386(18) 0.0360(18) -0.0137(14) 0.0209(15) -0.0194(16) C17 0.0384(18) 0.0436(18) 0.0310(16) -0.0107(14) 0.0133(13) -0.0072(14) C18 0.0330(16) 0.0297(15) 0.0293(15) -0.0018(12) 0.0096(12) -0.0041(12) C19 0.0281(15) 0.0228(14) 0.0191(13) 0.0025(10) 0.0009(11) 0.0035(11) C20 0.0314(16) 0.0445(18) 0.0289(16) -0.0075(13) 0.0062(12) -0.0007(14) C21 0.0298(17) 0.049(2) 0.0394(18) -0.0070(15) 0.0015(13) -0.0074(15) C22 0.048(2) 0.0349(17) 0.0244(15) -0.0032(12) -0.0037(13) -0.0033(14) C23 0.0454(19) 0.0318(16) 0.0205(14) -0.0031(12) 0.0064(12) -0.0008(14) C24 0.0332(16) 0.0280(15) 0.0211(14) -0.0006(11) 0.0052(11) -0.0001(12) C25 0.0208(13) 0.0203(13) 0.0172(12) -0.0005(10) 0.0030(10) 0.0014(10) C26 0.0211(13) 0.0193(12) 0.0225(13) 0.0011(10) 0.0044(10) 0.0022(10) C27 0.0299(16) 0.0373(17) 0.0259(15) -0.0055(12) 0.0064(12) -0.0027(13) C28 0.0368(17) 0.0413(18) 0.0317(16) 0.0002(13) 0.0157(13) -0.0002(14) C29 0.0297(16) 0.0273(15) 0.0444(18) 0.0011(13) 0.0152(13) -0.0046(12) C30 0.0268(15) 0.0237(14) 0.0408(17) -0.0060(12) 0.0070(12) -0.0049(12) C31 0.0247(14) 0.0220(14) 0.0260(14) 0.0002(11) 0.0051(11) -0.0002(11) C32 0.0204(14) 0.0397(16) 0.0167(13) -0.0048(11) 0.0050(10) 0.0032(12) C33 0.0298(16) 0.061(2) 0.0248(15) -0.0082(14) 0.0049(12) -0.0147(15) C34 0.0298(18) 0.100(3) 0.0260(17) -0.0126(19) 0.0004(13) -0.0195(19) C35 0.0226(16) 0.112(4) 0.0259(18) -0.015(2) -0.0022(13) 0.005(2) C36 0.046(2) 0.081(3) 0.0210(15) 0.0026(16) 0.0033(14) 0.034(2) C37 0.0363(17) 0.0480(19) 0.0229(15) 0.0013(13) 0.0024(12) 0.0144(15) C38 0.0279(15) 0.0222(14) 0.0332(16) -0.0019(12) 0.0022(12) 0.0074(12) C39 0.0152(12) 0.0136(11) 0.0189(12) 0.0001(9) 0.0011(9) 0.0006(9) C40 0.0194(13) 0.0147(12) 0.0183(12) -0.0007(9) 0.0023(10) -0.0011(10) C41 0.0198(13) 0.0209(13) 0.0217(13) -0.0011(10) 0.0053(10) 0.0018(10) C42 0.0213(13) 0.0214(13) 0.0250(14) 0.0044(10) 0.0038(10) 0.0021(11) C43 0.0218(13) 0.0243(13) 0.0203(13) 0.0052(10) 0.0005(10) 0.0014(11) C44 0.0206(13) 0.0182(12) 0.0178(12) 0.0019(10) 0.0014(10) 0.0005(10) C45 0.0190(13) 0.0207(13) 0.0186(12) 0.0011(10) 0.0022(10) 0.0038(10) C46 0.0206(13) 0.0295(14) 0.0165(12) -0.0033(10) 0.0066(10) 0.0006(11) C47 0.0289(15) 0.0254(14) 0.0324(15) -0.0039(12) 0.0041(12) -0.0015(12) C48 0.0414(19) 0.0357(17) 0.0442(19) -0.0091(14) 0.0107(15) -0.0141(15) C49 0.0341(18) 0.061(2) 0.0407(19) -0.0173(17) 0.0036(15) -0.0169(17) C50 0.0267(16) 0.065(2) 0.0287(16) -0.0047(15) -0.0019(12) -0.0055(15) C51 0.0253(15) 0.0427(17) 0.0215(14) 0.0010(12) 0.0013(11) 0.0008(13) C52 0.0214(13) 0.0262(14) 0.0149(12) 0.0019(10) 0.0010(10) 0.0012(11) C53 0.0363(17) 0.0245(15) 0.0305(15) 0.0037(11) 0.0131(13) 0.0031(12) C54 0.0435(19) 0.0321(17) 0.0421(18) 0.0101(14) 0.0155(15) -0.0027(14) C55 0.0267(15) 0.0470(18) 0.0241(14) 0.0042(13) 0.0085(11) -0.0038(13) C56 0.0251(15) 0.0415(17) 0.0224(14) -0.0052(12) 0.0051(11) -0.0004(12) C57 0.0255(14) 0.0282(14) 0.0231(13) -0.0052(11) 0.0039(11) -0.0019(12) C58 0.0227(14) 0.0301(14) 0.0178(13) 0.0026(11) 0.0020(10) 0.0077(11) C59 0.0177(13) 0.0458(18) 0.0190(13) 0.0097(12) -0.0009(10) 0.0029(12) C60 0.0263(16) 0.073(2) 0.0224(15) 0.0026(15) 0.0014(12) -0.0025(16) C61 0.0258(17) 0.105(3) 0.0259(17) 0.0240(19) 0.0046(13) -0.0067(19) C62 0.0257(17) 0.077(3) 0.047(2) 0.032(2) -0.0062(15) -0.0141(17) C63 0.0272(17) 0.045(2) 0.055(2) 0.0186(16) -0.0050(15) -0.0064(14) C64 0.0208(14) 0.0372(16) 0.0354(16) 0.0118(13) -0.0007(12) 0.0001(12) C65 0.0248(14) 0.0314(15) 0.0165(13) 0.0000(11) 0.0052(10) 0.0033(11) C66 0.0300(15) 0.0323(15) 0.0214(14) 0.0021(11) 0.0001(11) 0.0001(12) C67 0.0286(16) 0.0458(18) 0.0197(14) 0.0015(12) 0.0000(11) 0.0024(13) C68 0.0290(16) 0.0508(19) 0.0229(14) -0.0076(13) 0.0045(12) -0.0045(14) C69 0.0422(18) 0.0338(17) 0.0327(16) -0.0105(13) 0.0103(14) -0.0041(14) C70 0.0375(17) 0.0327(16) 0.0213(14) 0.0001(11) 0.0076(12) 0.0051(13) C71 0.0243(15) 0.0420(18) 0.0328(16) 0.0108(14) 0.0063(12) 0.0134(13) O100 0.0277(12) 0.109(2) 0.0386(14) -0.0189(14) -0.0040(10) 0.0014(14) C101 0.0301(17) 0.054(2) 0.0335(17) 0.0036(15) -0.0010(13) -0.0121(15) C102 0.060(3) 0.052(2) 0.073(3) -0.006(2) 0.003(2) -0.004(2) C103 0.060(3) 0.203(9) 0.086(4) -0.079(5) -0.014(3) 0.031(4) C04A 0.045(3) 0.061(4) 0.034(3) 0.003(3) 0.001(2) -0.026(3) C04B 0.022(5) 0.022(4) 0.027(5) -0.005(3) 0.004(3) 0.006(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 Ag C1 2.081(2) . ? Ag Cl 2.3189(9) . ? C1 N5 1.350(3) . ? C1 N2 1.352(3) . ? N2 C3 1.397(3) . ? N2 C6 1.444(3) . ? C3 C4 1.342(4) . ? C3 H3 0.9500 . ? C4 N5 1.383(3) . ? C4 H4 0.9500 . ? N5 C39 1.443(3) . ? C6 C7 1.397(4) . ? C6 C11 1.404(4) . ? C7 C8 1.391(4) . ? C7 C12 1.526(4) . ? C8 C9 1.388(4) . ? C8 H8 0.9500 . ? C9 C10 1.395(4) . ? C9 C38 1.507(4) . ? C10 C11 1.391(4) . ? C10 H10 0.9500 . ? C11 C25 1.533(3) . ? C12 C13 1.530(4) . ? C12 C19 1.531(4) . ? C12 H12 1.0000 . ? C13 C14 1.390(4) . ? C13 C18 1.398(4) . ? C14 C15 1.399(5) . ? C14 H14 0.9500 . ? C15 C16 1.374(5) . ? C15 H15 0.9500 . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C17 C18 1.392(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.389(4) . ? C19 C20 1.394(4) . ? C20 C21 1.379(4) . ? C20 H20 0.9500 . ? C21 C22 1.387(5) . ? C21 H21 0.9500 . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C23 C24 1.387(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C32 1.520(4) . ? C25 C26 1.534(4) . ? C25 H25 1.0000 . ? C26 C31 1.384(4) . ? C26 C27 1.400(4) . ? C27 C28 1.390(4) . ? C27 H27 0.9500 . ? C28 C29 1.385(5) . ? C28 H28 0.9500 . ? C29 C30 1.380(4) . ? C29 H29 0.9500 . ? C30 C31 1.392(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.387(4) . ? C32 C37 1.394(4) . ? C33 C34 1.393(5) . ? C33 H33 0.9500 . ? C34 C35 1.364(6) . ? C34 H34 0.9500 . ? C35 C36 1.376(6) . ? C35 H35 0.9500 . ? C36 C37 1.403(5) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.94(2) . ? C38 H38B 0.97(2) . ? C38 H38C 0.97(2) . ? C39 C44 1.393(3) . ? C39 C40 1.399(3) . ? C40 C41 1.384(4) . ? C40 C45 1.525(3) . ? C41 C42 1.395(4) . ? C41 H41 0.9500 . ? C42 C43 1.389(4) . ? C42 C71 1.507(4) . ? C43 C44 1.391(4) . ? C43 H43 0.9500 . ? C44 C58 1.532(4) . ? C45 C46 1.520(4) . ? C45 C52 1.530(3) . ? C45 H45 1.0000 . ? C46 C47 1.388(4) . ? C46 C51 1.395(4) . ? C47 C48 1.389(4) . ? C47 H47 0.9500 . ? C48 C49 1.380(5) . ? C48 H48 0.9500 . ? C49 C50 1.385(5) . ? C49 H49 0.9500 . ? C50 C51 1.381(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.385(4) . ? C52 C57 1.390(4) . ? C53 C54 1.392(4) . ? C53 H53 0.9500 . ? C54 C55 1.390(5) . ? C54 H54 0.9500 . ? C55 C56 1.369(4) . ? C55 H55 0.9500 . ? C56 C57 1.395(4) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C65 1.524(4) . ? C58 C59 1.534(4) . ? C58 H58 1.0000 . ? C59 C64 1.383(4) . ? C59 C60 1.402(4) . ? C60 C61 1.400(5) . ? C60 H60 0.9500 . ? C61 C62 1.375(6) . ? C61 H61 0.9500 . ? C62 C63 1.370(5) . ? C62 H62 0.9500 . ? C63 C64 1.395(4) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C66 1.390(4) . ? C65 C70 1.392(4) . ? C66 C67 1.381(4) . ? C66 H66 0.9500 . ? C67 C68 1.386(5) . ? C67 H67 0.9500 . ? C68 C69 1.383(5) . ? C68 H68 0.9500 . ? C69 C70 1.396(4) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 H71A 0.98(2) . ? C71 H71B 0.98(2) . ? C71 H71C 0.98(2) . ? O100 C103 1.330(6) . ? O100 C101 1.400(4) . ? C101 C102 1.485(5) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C103 C04A 1.286(8) . ? C103 C04B 1.401(8) . ? C103 H10F 0.9900 . ? C103 H10G 0.9900 . ? C04A H04A 0.9800 . ? C04A H04B 0.9800 . ? C04A H04C 0.9800 . ? C04B H04D 0.9800 . ? C04B H04E 0.9800 . ? C04B H04F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ag Cl 174.29(7) . . ? N5 C1 N2 104.2(2) . . ? N5 C1 Ag 124.02(18) . . ? N2 C1 Ag 131.71(18) . . ? C1 N2 C3 111.3(2) . . ? C1 N2 C6 124.0(2) . . ? C3 N2 C6 124.7(2) . . ? C4 C3 N2 105.9(2) . . ? C4 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C3 C4 N5 107.1(2) . . ? C3 C4 H4 126.4 . . ? N5 C4 H4 126.4 . . ? C1 N5 C4 111.4(2) . . ? C1 N5 C39 123.2(2) . . ? C4 N5 C39 125.3(2) . . ? C7 C6 C11 122.2(2) . . ? C7 C6 N2 118.5(2) . . ? C11 C6 N2 119.3(2) . . ? C8 C7 C6 117.6(2) . . ? C8 C7 C12 120.6(2) . . ? C6 C7 C12 121.8(2) . . ? C9 C8 C7 122.1(2) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C8 C9 C10 118.5(2) . . ? C8 C9 C38 120.4(2) . . ? C10 C9 C38 121.1(2) . . ? C11 C10 C9 121.9(2) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C6 117.6(2) . . ? C10 C11 C25 120.8(2) . . ? C6 C11 C25 121.6(2) . . ? C7 C12 C13 112.2(2) . . ? C7 C12 C19 111.2(2) . . ? C13 C12 C19 114.6(2) . . ? C7 C12 H12 106.0 . . ? C13 C12 H12 106.0 . . ? C19 C12 H12 106.0 . . ? C14 C13 C18 118.0(3) . . ? C14 C13 C12 119.1(3) . . ? C18 C13 C12 122.9(2) . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 121.2(3) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? C24 C19 C20 117.9(3) . . ? C24 C19 C12 123.8(3) . . ? C20 C19 C12 118.3(2) . . ? C21 C20 C19 121.7(3) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 118.9(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 121.2(3) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 120.4(3) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C32 C25 C11 111.6(2) . . ? C32 C25 C26 113.5(2) . . ? C11 C25 C26 112.7(2) . . ? C32 C25 H25 106.1 . . ? C11 C25 H25 106.1 . . ? C26 C25 H25 106.1 . . ? C31 C26 C27 118.2(3) . . ? C31 C26 C25 121.5(2) . . ? C27 C26 C25 120.1(2) . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 119.4(3) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.3(3) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C26 C31 C30 121.1(3) . . ? C26 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C37 118.6(3) . . ? C33 C32 C25 118.6(3) . . ? C37 C32 C25 122.8(3) . . ? C32 C33 C34 121.3(4) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 120.6(4) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C32 C37 C36 119.5(3) . . ? C32 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C9 C38 H38A 114(2) . . ? C9 C38 H38B 111(2) . . ? H38A C38 H38B 111(3) . . ? C9 C38 H38C 111(2) . . ? H38A C38 H38C 114(3) . . ? H38B C38 H38C 94(3) . . ? C44 C39 C40 122.4(2) . . ? C44 C39 N5 119.6(2) . . ? C40 C39 N5 118.1(2) . . ? C41 C40 C39 117.7(2) . . ? C41 C40 C45 122.3(2) . . ? C39 C40 C45 120.0(2) . . ? C40 C41 C42 121.7(2) . . ? C40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C43 C42 C41 118.7(2) . . ? C43 C42 C71 121.3(2) . . ? C41 C42 C71 120.0(2) . . ? C42 C43 C44 121.6(2) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C43 C44 C39 117.7(2) . . ? C43 C44 C58 120.8(2) . . ? C39 C44 C58 121.4(2) . . ? C46 C45 C40 112.7(2) . . ? C46 C45 C52 113.1(2) . . ? C40 C45 C52 112.9(2) . . ? C46 C45 H45 105.8 . . ? C40 C45 H45 105.8 . . ? C52 C45 H45 105.8 . . ? C47 C46 C51 118.4(3) . . ? C47 C46 C45 122.8(2) . . ? C51 C46 C45 118.8(2) . . ? C46 C47 C48 120.6(3) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C47 120.2(3) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C48 C49 C50 119.8(3) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 119.8(3) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C50 C51 C46 121.1(3) . . ? C50 C51 H51 119.4 . . ? C46 C51 H51 119.4 . . ? C53 C52 C57 118.7(2) . . ? C53 C52 C45 119.0(2) . . ? C57 C52 C45 122.4(2) . . ? C52 C53 C54 121.0(3) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C55 C54 C53 119.5(3) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C56 C55 C54 120.0(3) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.3(3) . . ? C55 C56 H56 119.8 . . ? C57 C56 H56 119.8 . . ? C52 C57 C56 120.4(3) . . ? C52 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C65 C58 C44 111.4(2) . . ? C65 C58 C59 112.8(2) . . ? C44 C58 C59 111.6(2) . . ? C65 C58 H58 106.9 . . ? C44 C58 H58 106.9 . . ? C59 C58 H58 106.9 . . ? C64 C59 C60 117.8(3) . . ? C64 C59 C58 123.3(2) . . ? C60 C59 C58 118.8(3) . . ? C61 C60 C59 120.3(4) . . ? C61 C60 H60 119.8 . . ? C59 C60 H60 119.8 . . ? C62 C61 C60 120.6(3) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C63 C62 C61 119.4(3) . . ? C63 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? C62 C63 C64 120.6(4) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C59 C64 C63 121.2(3) . . ? C59 C64 H64 119.4 . . ? C63 C64 H64 119.4 . . ? C66 C65 C70 118.3(3) . . ? C66 C65 C58 122.3(3) . . ? C70 C65 C58 119.4(2) . . ? C67 C66 C65 121.4(3) . . ? C67 C66 H66 119.3 . . ? C65 C66 H66 119.3 . . ? C66 C67 C68 119.9(3) . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C69 C68 C67 119.8(3) . . ? C69 C68 H68 120.1 . . ? C67 C68 H68 120.1 . . ? C68 C69 C70 120.0(3) . . ? C68 C69 H69 120.0 . . ? C70 C69 H69 120.0 . . ? C65 C70 C69 120.7(3) . . ? C65 C70 H70 119.7 . . ? C69 C70 H70 119.7 . . ? C42 C71 H71A 113(2) . . ? C42 C71 H71B 110(2) . . ? H71A C71 H71B 107(3) . . ? C42 C71 H71C 110(2) . . ? H71A C71 H71C 104(3) . . ? H71B C71 H71C 114(3) . . ? C103 O100 C101 115.2(3) . . ? O100 C101 C102 108.0(3) . . ? O100 C101 H10A 110.1 . . ? C102 C101 H10A 110.1 . . ? O100 C101 H10B 110.1 . . ? C102 C101 H10B 110.1 . . ? H10A C101 H10B 108.4 . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C04A C103 O100 112.0(7) . . ? C04A C103 C04B 62.8(5) . . ? O100 C103 C04B 143.0(6) . . ? C04A C103 H10F 109.2 . . ? O100 C103 H10F 109.2 . . ? C04B C103 H10F 49.7 . . ? C04A C103 H10G 109.2 . . ? O100 C103 H10G 109.2 . . ? C04B C103 H10G 106.7 . . ? H10F C103 H10G 107.9 . . ? C103 C04A H04A 109.5 . . ? C103 C04A H04B 109.5 . . ? H04A C04A H04B 109.5 . . ? C103 C04A H04C 109.5 . . ? H04A C04A H04C 109.5 . . ? H04B C04A H04C 109.5 . . ? C103 C04B H04D 109.5 . . ? C103 C04B H04E 109.5 . . ? H04D C04B H04E 109.5 . . ? C103 C04B H04F 109.5 . . ? H04D C04B H04F 109.5 . . ? H04E C04B H04F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl Ag C1 N5 -74.5(8) . . . . ? Cl Ag C1 N2 103.1(7) . . . . ? N5 C1 N2 C3 0.3(3) . . . . ? Ag C1 N2 C3 -177.59(18) . . . . ? N5 C1 N2 C6 177.8(2) . . . . ? Ag C1 N2 C6 -0.1(3) . . . . ? C1 N2 C3 C4 -0.5(3) . . . . ? C6 N2 C3 C4 -177.9(2) . . . . ? N2 C3 C4 N5 0.4(3) . . . . ? N2 C1 N5 C4 -0.1(3) . . . . ? Ag C1 N5 C4 178.04(16) . . . . ? N2 C1 N5 C39 177.4(2) . . . . ? Ag C1 N5 C39 -4.4(3) . . . . ? C3 C4 N5 C1 -0.2(3) . . . . ? C3 C4 N5 C39 -177.7(2) . . . . ? C1 N2 C6 C7 -88.0(3) . . . . ? C3 N2 C6 C7 89.1(3) . . . . ? C1 N2 C6 C11 91.3(3) . . . . ? C3 N2 C6 C11 -91.6(3) . . . . ? C11 C6 C7 C8 -1.9(4) . . . . ? N2 C6 C7 C8 177.4(2) . . . . ? C11 C6 C7 C12 177.9(2) . . . . ? N2 C6 C7 C12 -2.9(4) . . . . ? C6 C7 C8 C9 2.6(4) . . . . ? C12 C7 C8 C9 -177.1(2) . . . . ? C7 C8 C9 C10 -1.5(4) . . . . ? C7 C8 C9 C38 179.1(3) . . . . ? C8 C9 C10 C11 -0.5(4) . . . . ? C38 C9 C10 C11 178.8(2) . . . . ? C9 C10 C11 C6 1.2(4) . . . . ? C9 C10 C11 C25 -176.7(2) . . . . ? C7 C6 C11 C10 0.0(4) . . . . ? N2 C6 C11 C10 -179.2(2) . . . . ? C7 C6 C11 C25 178.0(2) . . . . ? N2 C6 C11 C25 -1.3(4) . . . . ? C8 C7 C12 C13 81.1(3) . . . . ? C6 C7 C12 C13 -98.7(3) . . . . ? C8 C7 C12 C19 -48.8(3) . . . . ? C6 C7 C12 C19 131.5(3) . . . . ? C7 C12 C13 C14 133.5(3) . . . . ? C19 C12 C13 C14 -98.5(3) . . . . ? C7 C12 C13 C18 -46.3(3) . . . . ? C19 C12 C13 C18 81.7(3) . . . . ? C18 C13 C14 C15 -0.4(4) . . . . ? C12 C13 C14 C15 179.8(3) . . . . ? C13 C14 C15 C16 0.4(5) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? C15 C16 C17 C18 0.0(5) . . . . ? C16 C17 C18 C13 0.0(5) . . . . ? C14 C13 C18 C17 0.2(4) . . . . ? C12 C13 C18 C17 180.0(3) . . . . ? C7 C12 C19 C24 116.1(3) . . . . ? C13 C12 C19 C24 -12.4(4) . . . . ? C7 C12 C19 C20 -64.2(3) . . . . ? C13 C12 C19 C20 167.3(3) . . . . ? C24 C19 C20 C21 2.2(5) . . . . ? C12 C19 C20 C21 -177.6(3) . . . . ? C19 C20 C21 C22 -1.6(5) . . . . ? C20 C21 C22 C23 -0.3(5) . . . . ? C21 C22 C23 C24 1.6(5) . . . . ? C22 C23 C24 C19 -1.0(5) . . . . ? C20 C19 C24 C23 -0.9(4) . . . . ? C12 C19 C24 C23 178.8(3) . . . . ? C10 C11 C25 C32 -53.8(3) . . . . ? C6 C11 C25 C32 128.3(3) . . . . ? C10 C11 C25 C26 75.3(3) . . . . ? C6 C11 C25 C26 -102.5(3) . . . . ? C32 C25 C26 C31 148.1(3) . . . . ? C11 C25 C26 C31 19.9(3) . . . . ? C32 C25 C26 C27 -36.7(3) . . . . ? C11 C25 C26 C27 -164.9(2) . . . . ? C31 C26 C27 C28 -0.8(4) . . . . ? C25 C26 C27 C28 -176.1(3) . . . . ? C26 C27 C28 C29 1.7(5) . . . . ? C27 C28 C29 C30 -1.0(5) . . . . ? C28 C29 C30 C31 -0.6(5) . . . . ? C27 C26 C31 C30 -0.8(4) . . . . ? C25 C26 C31 C30 174.4(2) . . . . ? C29 C30 C31 C26 1.5(4) . . . . ? C11 C25 C32 C33 -92.4(3) . . . . ? C26 C25 C32 C33 138.9(3) . . . . ? C11 C25 C32 C37 88.7(3) . . . . ? C26 C25 C32 C37 -40.1(3) . . . . ? C37 C32 C33 C34 0.5(4) . . . . ? C25 C32 C33 C34 -178.5(3) . . . . ? C32 C33 C34 C35 -0.3(5) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? C34 C35 C36 C37 0.9(5) . . . . ? C33 C32 C37 C36 0.1(4) . . . . ? C25 C32 C37 C36 179.0(3) . . . . ? C35 C36 C37 C32 -0.8(5) . . . . ? C1 N5 C39 C44 86.8(3) . . . . ? C4 N5 C39 C44 -96.0(3) . . . . ? C1 N5 C39 C40 -93.0(3) . . . . ? C4 N5 C39 C40 84.2(3) . . . . ? C44 C39 C40 C41 2.5(4) . . . . ? N5 C39 C40 C41 -177.7(2) . . . . ? C44 C39 C40 C45 -178.6(2) . . . . ? N5 C39 C40 C45 1.2(3) . . . . ? C39 C40 C41 C42 -2.0(4) . . . . ? C45 C40 C41 C42 179.1(2) . . . . ? C40 C41 C42 C43 -0.2(4) . . . . ? C40 C41 C42 C71 -178.9(3) . . . . ? C41 C42 C43 C44 2.1(4) . . . . ? C71 C42 C43 C44 -179.2(3) . . . . ? C42 C43 C44 C39 -1.7(4) . . . . ? C42 C43 C44 C58 175.3(2) . . . . ? C40 C39 C44 C43 -0.7(4) . . . . ? N5 C39 C44 C43 179.5(2) . . . . ? C40 C39 C44 C58 -177.7(2) . . . . ? N5 C39 C44 C58 2.5(4) . . . . ? C41 C40 C45 C46 95.9(3) . . . . ? C39 C40 C45 C46 -82.9(3) . . . . ? C41 C40 C45 C52 -33.7(3) . . . . ? C39 C40 C45 C52 147.5(2) . . . . ? C40 C45 C46 C47 -26.1(3) . . . . ? C52 C45 C46 C47 103.4(3) . . . . ? C40 C45 C46 C51 152.7(2) . . . . ? C52 C45 C46 C51 -77.8(3) . . . . ? C51 C46 C47 C48 -1.6(4) . . . . ? C45 C46 C47 C48 177.1(3) . . . . ? C46 C47 C48 C49 1.0(5) . . . . ? C47 C48 C49 C50 0.4(5) . . . . ? C48 C49 C50 C51 -1.1(5) . . . . ? C49 C50 C51 C46 0.5(5) . . . . ? C47 C46 C51 C50 0.9(4) . . . . ? C45 C46 C51 C50 -177.9(3) . . . . ? C46 C45 C52 C53 137.2(3) . . . . ? C40 C45 C52 C53 -93.3(3) . . . . ? C46 C45 C52 C57 -42.1(3) . . . . ? C40 C45 C52 C57 87.3(3) . . . . ? C57 C52 C53 C54 0.9(4) . . . . ? C45 C52 C53 C54 -178.5(3) . . . . ? C52 C53 C54 C55 -0.1(5) . . . . ? C53 C54 C55 C56 -1.1(5) . . . . ? C54 C55 C56 C57 1.6(5) . . . . ? C53 C52 C57 C56 -0.4(4) . . . . ? C45 C52 C57 C56 178.9(2) . . . . ? C55 C56 C57 C52 -0.8(4) . . . . ? C43 C44 C58 C65 39.1(3) . . . . ? C39 C44 C58 C65 -144.0(2) . . . . ? C43 C44 C58 C59 -87.9(3) . . . . ? C39 C44 C58 C59 89.0(3) . . . . ? C65 C58 C59 C64 -121.2(3) . . . . ? C44 C58 C59 C64 5.1(4) . . . . ? C65 C58 C59 C60 57.3(3) . . . . ? C44 C58 C59 C60 -176.4(2) . . . . ? C64 C59 C60 C61 0.8(4) . . . . ? C58 C59 C60 C61 -177.8(3) . . . . ? C59 C60 C61 C62 0.9(5) . . . . ? C60 C61 C62 C63 -2.0(5) . . . . ? C61 C62 C63 C64 1.4(5) . . . . ? C60 C59 C64 C63 -1.5(4) . . . . ? C58 C59 C64 C63 177.0(3) . . . . ? C62 C63 C64 C59 0.4(5) . . . . ? C44 C58 C65 C66 -94.4(3) . . . . ? C59 C58 C65 C66 32.0(4) . . . . ? C44 C58 C65 C70 84.3(3) . . . . ? C59 C58 C65 C70 -149.3(3) . . . . ? C70 C65 C66 C67 -1.1(4) . . . . ? C58 C65 C66 C67 177.6(3) . . . . ? C65 C66 C67 C68 1.0(4) . . . . ? C66 C67 C68 C69 -0.4(4) . . . . ? C67 C68 C69 C70 -0.2(4) . . . . ? C66 C65 C70 C69 0.5(4) . . . . ? C58 C65 C70 C69 -178.3(3) . . . . ? C68 C69 C70 C65 0.2(4) . . . . ? C103 O100 C101 C102 -165.1(5) . . . . ? C101 O100 C103 C04A -74.8(6) . . . . ? C101 O100 C103 C04B -1.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.544 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.075 # Attachment '10-IPrs-Rh-acac.cif' #============================================================================== data_11 _database_code_depnum_ccdc_archive 'CCDC 743051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H63 N2 O3 Rh, C2.5 H6, 2(C H2 CL2)' _chemical_formula_sum 'C79.50 H73 Cl4 N2 O3 Rh' _chemical_formula_weight 1349.11 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' Rh Rh -1.1178 0.9187 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1205(2) _cell_length_b 15.1256(3) _cell_length_c 19.1389(5) _cell_angle_alpha 86.866(1) _cell_angle_beta 87.613(1) _cell_angle_gamma 62.432(1) _cell_volume 3617.56(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41354 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 27.50 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1402 _exptl_absorpt_coefficient_mu 0.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2006/1)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100616 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16626 _reflns_number_gt 13803 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'PEAKREF (Schreurs, 2005)' _computing_data_reduction 'EVALCCD (Duisenberg et al., 2003)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+2.6552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16626 _refine_ls_number_parameters 853 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.681716(13) 0.137329(12) 0.208530(8) 0.02127(5) Uani 1 1 d . . . C1 C 0.71945(15) 0.24040(14) 0.23906(10) 0.0185(4) Uani 1 1 d . . . C2 C 0.79604(16) 0.34304(15) 0.24524(11) 0.0241(4) Uani 1 1 d . . . H2 H 0.8420 0.3723 0.2350 0.029 Uiso 1 1 calc R . . C3 C 0.71826(16) 0.37108(15) 0.29404(11) 0.0238(4) Uani 1 1 d . . . H3 H 0.6991 0.4233 0.3256 0.029 Uiso 1 1 calc R . . C4 C 0.58905(16) 0.30841(15) 0.33679(10) 0.0221(4) Uani 1 1 d . . . C5 C 0.48372(16) 0.38386(16) 0.33019(10) 0.0232(4) Uani 1 1 d . . . C6 C 0.40630(17) 0.37632(17) 0.37374(11) 0.0279(5) Uani 1 1 d . . . H6 H 0.3341 0.4261 0.3698 0.034 Uiso 1 1 calc R . . C7 C 0.43142(18) 0.29802(19) 0.42296(11) 0.0303(5) Uani 1 1 d . . . C8 C 0.53707(18) 0.22803(18) 0.43029(11) 0.0286(5) Uani 1 1 d . . . H8 H 0.5550 0.1758 0.4651 0.034 Uiso 1 1 calc R . . C9 C 0.61817(16) 0.23163(16) 0.38829(10) 0.0242(4) Uani 1 1 d . . . C10 C 0.73536(17) 0.15900(17) 0.40058(11) 0.0269(4) Uani 1 1 d . . . H10 H 0.7720 0.1494 0.3537 0.032 Uiso 1 1 calc R . . C11 C 0.45612(17) 0.47310(16) 0.27912(11) 0.0265(4) Uani 1 1 d . . . H11 H 0.5037 0.4474 0.2370 0.032 Uiso 1 1 calc R . . C12 C 0.3450(2) 0.2907(2) 0.46757(14) 0.0449(7) Uani 1 1 d . . . H12A H 0.3769 0.2322 0.4998 0.067 Uiso 1 1 calc R . . H12B H 0.2943 0.2840 0.4376 0.067 Uiso 1 1 calc R . . H12C H 0.3074 0.3511 0.4944 0.067 Uiso 1 1 calc R . . C13 C 0.87866(15) 0.20708(14) 0.16128(10) 0.0191(4) Uani 1 1 d . . . C14 C 0.98359(16) 0.15249(14) 0.18349(10) 0.0203(4) Uani 1 1 d . . . C15 C 1.06089(15) 0.09796(15) 0.13410(11) 0.0221(4) Uani 1 1 d . . . H15 H 1.1328 0.0597 0.1484 0.027 Uiso 1 1 calc R . . C16 C 1.03669(16) 0.09755(15) 0.06505(11) 0.0220(4) Uani 1 1 d . . . C17 C 0.93130(16) 0.15475(15) 0.04466(11) 0.0221(4) Uani 1 1 d . . . H17 H 0.9140 0.1558 -0.0029 0.026 Uiso 1 1 calc R . . C18 C 0.85062(15) 0.21040(14) 0.09173(10) 0.0193(4) Uani 1 1 d . . . C19 C 0.73542(15) 0.27466(15) 0.06959(10) 0.0222(4) Uani 1 1 d . . . H19 H 0.6902 0.2614 0.1060 0.027 Uiso 1 1 calc R . . C20 C 1.01596(16) 0.15350(15) 0.25852(11) 0.0229(4) Uani 1 1 d . . . H20 H 0.9498 0.1756 0.2884 0.028 Uiso 1 1 calc R . . C21 C 1.12274(17) 0.03741(17) 0.01317(12) 0.0305(5) Uani 1 1 d . . . H21A H 1.1624 0.0740 -0.0022 0.046 Uiso 1 1 calc R . . H21B H 1.0901 0.0260 -0.0273 0.046 Uiso 1 1 calc R . . H21C H 1.1718 -0.0269 0.0353 0.046 Uiso 1 1 calc R . . C22 C 0.6496(3) -0.1127(3) 0.1304(2) 0.0743(11) Uani 1 1 d . . . H22A H 0.6230 -0.0865 0.0834 0.111 Uiso 1 1 calc R . . H22B H 0.5898 -0.1058 0.1615 0.111 Uiso 1 1 calc R . . H22C H 0.7018 -0.1834 0.1284 0.111 Uiso 1 1 calc R . . C23 C 0.7025(2) -0.0546(2) 0.15827(15) 0.0421(6) Uani 1 1 d . . . C24 C 0.8129(2) -0.09946(18) 0.16205(14) 0.0395(6) Uani 1 1 d . . . H24 H 0.8504 -0.1679 0.1510 0.047 Uiso 1 1 calc R . . C25 C 0.87439(19) -0.05465(16) 0.18028(12) 0.0300(5) Uani 1 1 d . . . C26 C 0.9938(2) -0.11298(18) 0.17346(14) 0.0400(6) Uani 1 1 d . . . H26A H 1.0227 -0.0696 0.1528 0.060 Uiso 1 1 calc R . . H26B H 1.0125 -0.1693 0.1433 0.060 Uiso 1 1 calc R . . H26C H 1.0242 -0.1381 0.2198 0.060 Uiso 1 1 calc R . . C27 C 0.54172(18) 0.22340(17) 0.21363(12) 0.0292(5) Uani 1 1 d . . . C28 C 0.78864(19) 0.2029(2) 0.44588(11) 0.0336(5) Uani 1 1 d . . . C29 C 0.7362(2) 0.2984(2) 0.47063(13) 0.0408(6) Uani 1 1 d . . . H29 H 0.6623 0.3387 0.4620 0.049 Uiso 1 1 calc R . . C30 C 0.7916(3) 0.3355(3) 0.50815(15) 0.0548(8) Uani 1 1 d . . . H30 H 0.7554 0.4014 0.5244 0.066 Uiso 1 1 calc R . . C31 C 0.8980(3) 0.2776(3) 0.52180(15) 0.0609(10) Uani 1 1 d . . . H31 H 0.9354 0.3034 0.5472 0.073 Uiso 1 1 calc R . . C32 C 0.9501(3) 0.1821(3) 0.49845(15) 0.0577(9) Uani 1 1 d . . . H32 H 1.0235 0.1414 0.5084 0.069 Uiso 1 1 calc R . . C33 C 0.8965(2) 0.1451(2) 0.46085(14) 0.0443(6) Uani 1 1 d . . . H33 H 0.9336 0.0791 0.4447 0.053 Uiso 1 1 calc R . . C34 C 0.75312(17) 0.05581(18) 0.42775(12) 0.0309(5) Uani 1 1 d . . . C35 C 0.7786(2) -0.01872(19) 0.38096(14) 0.0381(6) Uani 1 1 d . . . H35 H 0.7861 -0.0053 0.3325 0.046 Uiso 1 1 calc R . . C36 C 0.7935(2) -0.1128(2) 0.40370(17) 0.0508(7) Uani 1 1 d . . . H36 H 0.8112 -0.1633 0.3709 0.061 Uiso 1 1 calc R . . C37 C 0.7827(2) -0.1332(2) 0.47328(19) 0.0555(8) Uani 1 1 d . . . H37 H 0.7920 -0.1974 0.4887 0.067 Uiso 1 1 calc R . . C38 C 0.7583(2) -0.0605(3) 0.52066(17) 0.0552(8) Uani 1 1 d . . . H38 H 0.7511 -0.0749 0.5690 0.066 Uiso 1 1 calc R . . C39 C 0.7440(2) 0.0341(2) 0.49874(14) 0.0426(6) Uani 1 1 d . . . H39 H 0.7281 0.0836 0.5320 0.051 Uiso 1 1 calc R . . C40 C 0.34151(18) 0.52108(16) 0.25350(12) 0.0293(5) Uani 1 1 d . . . C41 C 0.25662(19) 0.58993(18) 0.29254(14) 0.0359(5) Uani 1 1 d . . . H41 H 0.2701 0.6099 0.3357 0.043 Uiso 1 1 calc R . . C42 C 0.1527(2) 0.6298(2) 0.26941(16) 0.0449(6) Uani 1 1 d . . . H42 H 0.0954 0.6757 0.2972 0.054 Uiso 1 1 calc R . . C43 C 0.1323(2) 0.6032(2) 0.20633(17) 0.0509(8) Uani 1 1 d . . . H43 H 0.0610 0.6303 0.1905 0.061 Uiso 1 1 calc R . . C44 C 0.2153(2) 0.5373(2) 0.16644(15) 0.0466(7) Uani 1 1 d . . . H44 H 0.2014 0.5193 0.1227 0.056 Uiso 1 1 calc R . . C45 C 0.3194(2) 0.49672(18) 0.18947(13) 0.0367(5) Uani 1 1 d . . . H45 H 0.3763 0.4517 0.1610 0.044 Uiso 1 1 calc R . . C46 C 0.48208(17) 0.55017(16) 0.30949(12) 0.0282(5) Uani 1 1 d . . . C47 C 0.5061(2) 0.61234(19) 0.26449(14) 0.0376(5) Uani 1 1 d . . . H47 H 0.5046 0.6072 0.2153 0.045 Uiso 1 1 calc R . . C48 C 0.5321(2) 0.6818(2) 0.29033(17) 0.0499(7) Uani 1 1 d . . . H48 H 0.5490 0.7234 0.2588 0.060 Uiso 1 1 calc R . . C49 C 0.5336(2) 0.6910(2) 0.36125(17) 0.0527(8) Uani 1 1 d . . . H49 H 0.5514 0.7389 0.3788 0.063 Uiso 1 1 calc R . . C50 C 0.5092(2) 0.6306(2) 0.40643(16) 0.0477(7) Uani 1 1 d . . . H50 H 0.5102 0.6368 0.4555 0.057 Uiso 1 1 calc R . . C51 C 0.48314(19) 0.56067(19) 0.38111(13) 0.0361(5) Uani 1 1 d . . . H51 H 0.4659 0.5196 0.4129 0.043 Uiso 1 1 calc R . . C52 C 0.70151(17) 0.38590(16) 0.07102(11) 0.0261(4) Uani 1 1 d . . . C53 C 0.7724(2) 0.42483(18) 0.06986(15) 0.0428(6) Uani 1 1 d . . . H53 H 0.8470 0.3813 0.0675 0.051 Uiso 1 1 calc R . . C54 C 0.7362(2) 0.5272(2) 0.07210(18) 0.0544(8) Uani 1 1 d . . . H54 H 0.7863 0.5528 0.0722 0.065 Uiso 1 1 calc R . . C55 C 0.6289(2) 0.59154(19) 0.07416(15) 0.0484(7) Uani 1 1 d . . . H55 H 0.6044 0.6615 0.0753 0.058 Uiso 1 1 calc R . . C56 C 0.5573(2) 0.55360(19) 0.07459(14) 0.0454(7) Uani 1 1 d . . . H56 H 0.4828 0.5977 0.0757 0.054 Uiso 1 1 calc R . . C57 C 0.59266(18) 0.45221(18) 0.07344(13) 0.0359(5) Uani 1 1 d . . . H57 H 0.5422 0.4271 0.0743 0.043 Uiso 1 1 calc R . . C58 C 0.70811(16) 0.24776(15) 0.00037(11) 0.0251(4) Uani 1 1 d . . . C59 C 0.74181(18) 0.27249(18) -0.06386(12) 0.0317(5) Uani 1 1 d . . . H59 H 0.7822 0.3083 -0.0651 0.038 Uiso 1 1 calc R . . C60 C 0.7172(2) 0.2455(2) -0.12570(13) 0.0414(6) Uani 1 1 d . . . H60 H 0.7420 0.2614 -0.1691 0.050 Uiso 1 1 calc R . . C61 C 0.6567(2) 0.1955(2) -0.12454(14) 0.0458(7) Uani 1 1 d . . . H61 H 0.6403 0.1764 -0.1671 0.055 Uiso 1 1 calc R . . C62 C 0.6197(2) 0.17298(18) -0.06138(14) 0.0402(6) Uani 1 1 d . . . H62 H 0.5762 0.1402 -0.0606 0.048 Uiso 1 1 calc R . . C63 C 0.64626(17) 0.19851(16) 0.00081(13) 0.0307(5) Uani 1 1 d . . . H63 H 0.6218 0.1820 0.0441 0.037 Uiso 1 1 calc R . . C64 C 1.05887(16) 0.22839(16) 0.26689(12) 0.0258(4) Uani 1 1 d . . . C65 C 1.0644(2) 0.25628(19) 0.33407(13) 0.0406(6) Uani 1 1 d . . . H65 H 1.0392 0.2307 0.3729 0.049 Uiso 1 1 calc R . . C66 C 1.1061(3) 0.3206(2) 0.34473(16) 0.0538(8) Uani 1 1 d . . . H66 H 1.1098 0.3385 0.3910 0.065 Uiso 1 1 calc R . . C67 C 1.1425(2) 0.3594(2) 0.28974(18) 0.0532(8) Uani 1 1 d . . . H67 H 1.1716 0.4033 0.2977 0.064 Uiso 1 1 calc R . . C68 C 1.1363(2) 0.3337(2) 0.22295(17) 0.0485(7) Uani 1 1 d . . . H68 H 1.1605 0.3607 0.1843 0.058 Uiso 1 1 calc R . . C69 C 1.0948(2) 0.26834(19) 0.21168(14) 0.0374(5) Uani 1 1 d . . . H69 H 1.0912 0.2509 0.1653 0.045 Uiso 1 1 calc R . . C70 C 1.09465(18) 0.04880(16) 0.28580(11) 0.0262(4) Uani 1 1 d . . . C71 C 1.0554(2) -0.01453(19) 0.31323(12) 0.0359(5) Uani 1 1 d . . . H71 H 0.9804 0.0080 0.3161 0.043 Uiso 1 1 calc R . . C72 C 1.1252(3) -0.1112(2) 0.33660(14) 0.0495(7) Uani 1 1 d . . . H72 H 1.0975 -0.1542 0.3553 0.059 Uiso 1 1 calc R . . C73 C 1.2338(3) -0.1448(2) 0.33280(14) 0.0477(7) Uani 1 1 d . . . H73 H 1.2811 -0.2110 0.3484 0.057 Uiso 1 1 calc R . . C74 C 1.2734(2) -0.08219(19) 0.30634(14) 0.0443(6) Uani 1 1 d . . . H74 H 1.3484 -0.1049 0.3041 0.053 Uiso 1 1 calc R . . C75 C 1.20436(19) 0.01419(18) 0.28280(13) 0.0339(5) Uani 1 1 d . . . H75 H 1.2326 0.0569 0.2644 0.041 Uiso 1 1 calc R . . N1 N 0.79710(13) 0.26329(12) 0.21232(8) 0.0195(3) Uani 1 1 d . . . N2 N 0.67094(13) 0.30909(12) 0.28964(9) 0.0207(3) Uani 1 1 d . . . O1 O 0.63894(13) 0.03407(12) 0.17398(9) 0.0362(4) Uani 1 1 d . . . O2 O 0.83904(12) 0.03359(11) 0.20215(8) 0.0269(3) Uani 1 1 d . . . O3 O 0.45081(14) 0.27326(14) 0.21485(11) 0.0494(5) Uani 1 1 d . . . C1SA C 0.5215(3) 1.0365(2) 0.33634(18) 0.0603(8) Uani 0.687(3) 1 d PDU A 1 H1S1 H 0.5671 1.0580 0.3069 0.072 Uiso 0.687(3) 1 calc PR A 1 H1S2 H 0.5377 1.0390 0.3858 0.072 Uiso 0.687(3) 1 calc PR A 1 Cl1A Cl 0.38672(7) 1.12268(8) 0.32198(5) 0.0572(3) Uani 0.687(3) 1 d PDU A 1 Cl2A Cl 0.55631(16) 0.91407(11) 0.31874(14) 0.0942(7) Uani 0.687(3) 1 d PDU A 1 C1SB C 0.5215(3) 1.0365(2) 0.33634(18) 0.0603(8) Uani 0.165(3) 1 d PDU B 2 H1S3 H 0.5637 1.0267 0.2922 0.072 Uiso 0.165(3) 1 calc PR B 2 H1S4 H 0.5522 1.0616 0.3712 0.072 Uiso 0.165(3) 1 calc PR B 2 Cl1B Cl 0.38672(7) 1.12268(8) 0.32198(5) 0.0572(3) Uani 0.165(3) 1 d PDU B 2 Cl2B Cl 0.5256(7) 0.9253(5) 0.3668(6) 0.0942(7) Uani 0.165(3) 1 d PDU B 2 C1SC C 0.5215(3) 1.0365(2) 0.33634(18) 0.0603(8) Uani 0.1475(19) 1 d PDU C 3 H1S5 H 0.5975 1.0127 0.3224 0.072 Uiso 0.1475(19) 1 calc PR C 3 H1S6 H 0.4864 1.1100 0.3394 0.072 Uiso 0.1475(19) 1 calc PR C 3 Cl1C Cl 0.5086(7) 0.9774(7) 0.4168(4) 0.094(2) Uani 0.1475(19) 1 d PDU C 3 Cl2C Cl 0.4544(6) 0.9983(7) 0.2769(4) 0.094(2) Uani 0.1475(19) 1 d PDU C 3 C2S C 0.3835(2) 0.1526(2) 0.12464(16) 0.0489(7) Uani 1 1 d . . . H2S1 H 0.4606 0.1151 0.1350 0.059 Uiso 1 1 calc R . . H2S2 H 0.3450 0.1836 0.1682 0.059 Uiso 1 1 calc R . . Cl3S Cl 0.36377(9) 0.24742(9) 0.06051(5) 0.0803(3) Uani 1 1 d . . . Cl4S Cl 0.33864(8) 0.06927(8) 0.09815(7) 0.0875(3) Uani 1 1 d . . . C1P C 1.0834(15) 0.3051(6) -0.0070(8) 0.072(3) Uani 0.50 1 d PDU D -1 H1P1 H 1.1594 0.2879 -0.0098 0.108 Uiso 0.50 1 calc PR D -1 H1P2 H 1.0705 0.2597 -0.0352 0.108 Uiso 0.50 1 calc PR D -1 H1P3 H 1.0628 0.2989 0.0418 0.108 Uiso 0.50 1 calc PR D -1 C2P C 1.0177(5) 0.4115(4) -0.0345(3) 0.0519(13) Uani 0.50 1 d PDU D -1 H2P1 H 1.0480 0.4199 -0.0805 0.062 Uiso 0.50 1 calc PR D -1 H2P2 H 0.9440 0.4227 -0.0422 0.062 Uiso 0.50 1 calc PR D -1 C3P C 1.0127(7) 0.4900(5) 0.0127(4) 0.0398(16) Uani 0.50 1 d PDU D -1 H3P1 H 1.0864 0.4776 0.0219 0.048 Uiso 0.50 1 calc PR D -1 H3P2 H 0.9795 0.4837 0.0580 0.048 Uiso 0.50 1 calc PR D -1 C4P C 0.9500(5) 0.5959(4) -0.0173(4) 0.0568(15) Uani 0.50 1 d PDU D -1 H4P1 H 0.9848 0.6033 -0.0617 0.068 Uiso 0.50 1 calc PR D -1 H4P2 H 0.8770 0.6078 -0.0282 0.068 Uiso 0.50 1 calc PR D -1 C5P C 0.9423(14) 0.6739(7) 0.0323(7) 0.081(4) Uani 0.50 1 d PDU D -1 H5P1 H 0.9024 0.6710 0.0747 0.121 Uiso 0.50 1 calc PR D -1 H5P2 H 0.9054 0.7404 0.0093 0.121 Uiso 0.50 1 calc PR D -1 H5P3 H 1.0144 0.6609 0.0449 0.121 Uiso 0.50 1 calc PR D -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02217(9) 0.02058(8) 0.02198(9) -0.00172(6) -0.00061(6) -0.01052(6) C1 0.0174(9) 0.0200(9) 0.0168(9) 0.0005(7) -0.0020(7) -0.0075(8) C2 0.0213(10) 0.0214(10) 0.0311(11) -0.0028(8) 0.0007(8) -0.0110(8) C3 0.0218(10) 0.0221(10) 0.0276(11) -0.0070(8) 0.0013(8) -0.0097(8) C4 0.0219(10) 0.0272(10) 0.0189(10) -0.0052(8) 0.0022(8) -0.0126(9) C5 0.0221(10) 0.0271(11) 0.0198(10) -0.0057(8) 0.0000(8) -0.0103(9) C6 0.0186(10) 0.0371(12) 0.0249(11) -0.0048(9) 0.0000(8) -0.0098(9) C7 0.0258(11) 0.0462(14) 0.0230(11) -0.0019(10) 0.0010(9) -0.0201(10) C8 0.0284(11) 0.0409(13) 0.0208(10) 0.0045(9) -0.0029(8) -0.0201(10) C9 0.0229(10) 0.0319(11) 0.0189(10) -0.0029(8) -0.0015(8) -0.0134(9) C10 0.0240(11) 0.0351(12) 0.0201(10) 0.0034(9) -0.0027(8) -0.0128(9) C11 0.0233(10) 0.0275(11) 0.0249(11) -0.0049(9) 0.0029(8) -0.0084(9) C12 0.0287(13) 0.0692(19) 0.0378(14) 0.0079(13) 0.0028(11) -0.0246(13) C13 0.0167(9) 0.0164(9) 0.0229(10) -0.0015(7) 0.0033(7) -0.0067(7) C14 0.0199(9) 0.0186(9) 0.0219(10) 0.0020(8) -0.0026(8) -0.0087(8) C15 0.0146(9) 0.0192(9) 0.0272(11) 0.0018(8) -0.0035(8) -0.0033(8) C16 0.0187(10) 0.0188(9) 0.0250(10) -0.0013(8) 0.0008(8) -0.0057(8) C17 0.0189(10) 0.0212(10) 0.0214(10) -0.0001(8) -0.0019(8) -0.0053(8) C18 0.0163(9) 0.0172(9) 0.0224(10) 0.0015(7) -0.0009(7) -0.0062(8) C19 0.0165(9) 0.0225(10) 0.0204(10) 0.0042(8) -0.0005(7) -0.0035(8) C20 0.0205(10) 0.0248(10) 0.0217(10) 0.0004(8) -0.0009(8) -0.0091(8) C21 0.0196(10) 0.0315(12) 0.0304(12) -0.0063(9) 0.0000(9) -0.0026(9) C22 0.060(2) 0.0523(19) 0.124(3) -0.043(2) 0.004(2) -0.0336(17) C23 0.0457(15) 0.0357(14) 0.0519(16) -0.0144(12) 0.0049(12) -0.0238(12) C24 0.0424(14) 0.0241(12) 0.0513(15) -0.0118(11) 0.0069(12) -0.0141(11) C25 0.0356(12) 0.0223(11) 0.0260(11) 0.0008(9) 0.0008(9) -0.0086(9) C26 0.0340(13) 0.0265(12) 0.0475(15) -0.0050(11) -0.0026(11) -0.0034(10) C27 0.0288(12) 0.0280(11) 0.0360(12) -0.0077(9) -0.0032(9) -0.0167(10) C28 0.0332(12) 0.0532(15) 0.0214(11) 0.0054(10) -0.0028(9) -0.0265(12) C29 0.0414(14) 0.0581(17) 0.0313(13) -0.0032(12) -0.0040(11) -0.0296(13) C30 0.076(2) 0.071(2) 0.0376(15) -0.0056(14) -0.0062(14) -0.0503(19) C31 0.073(2) 0.112(3) 0.0360(15) 0.0118(17) -0.0172(15) -0.075(2) C32 0.0427(16) 0.102(3) 0.0414(16) 0.0061(17) -0.0106(13) -0.0450(18) C33 0.0319(13) 0.0677(19) 0.0360(14) 0.0050(13) -0.0055(11) -0.0257(13) C34 0.0209(10) 0.0395(13) 0.0303(12) 0.0098(10) -0.0079(9) -0.0129(10) C35 0.0361(13) 0.0407(14) 0.0382(14) 0.0072(11) -0.0116(11) -0.0185(11) C36 0.0448(16) 0.0459(16) 0.067(2) 0.0105(14) -0.0195(14) -0.0250(14) C37 0.0426(16) 0.0523(18) 0.079(2) 0.0299(17) -0.0209(15) -0.0302(14) C38 0.0411(16) 0.073(2) 0.0503(17) 0.0354(16) -0.0106(13) -0.0281(15) C39 0.0331(13) 0.0545(16) 0.0332(13) 0.0140(12) -0.0049(10) -0.0158(12) C40 0.0293(11) 0.0251(11) 0.0324(12) 0.0027(9) -0.0060(9) -0.0116(9) C41 0.0284(12) 0.0315(12) 0.0426(14) -0.0013(10) -0.0038(10) -0.0093(10) C42 0.0274(13) 0.0335(13) 0.0657(19) 0.0043(12) -0.0068(12) -0.0074(11) C43 0.0372(15) 0.0439(16) 0.074(2) 0.0224(15) -0.0290(14) -0.0212(13) C44 0.0547(17) 0.0427(15) 0.0505(16) 0.0119(13) -0.0275(14) -0.0286(14) C45 0.0443(14) 0.0327(13) 0.0351(13) 0.0016(10) -0.0095(11) -0.0192(11) C46 0.0187(10) 0.0244(11) 0.0353(12) -0.0036(9) -0.0029(9) -0.0042(8) C47 0.0348(13) 0.0357(13) 0.0400(14) 0.0028(11) -0.0084(10) -0.0141(11) C48 0.0493(17) 0.0392(15) 0.066(2) 0.0106(13) -0.0172(14) -0.0246(13) C49 0.0529(17) 0.0373(15) 0.071(2) -0.0070(14) -0.0196(15) -0.0219(13) C50 0.0503(16) 0.0464(16) 0.0472(16) -0.0168(13) -0.0067(13) -0.0209(13) C51 0.0337(13) 0.0372(13) 0.0370(13) -0.0115(10) 0.0026(10) -0.0153(11) C52 0.0218(10) 0.0241(10) 0.0194(10) 0.0001(8) -0.0001(8) 0.0002(8) C53 0.0273(12) 0.0238(12) 0.0638(18) 0.0058(11) 0.0135(12) -0.0024(10) C54 0.0465(16) 0.0282(13) 0.081(2) 0.0050(14) 0.0158(15) -0.0127(12) C55 0.0529(17) 0.0220(12) 0.0489(16) 0.0024(11) 0.0034(13) 0.0000(12) C56 0.0338(14) 0.0315(13) 0.0416(15) -0.0100(11) -0.0107(11) 0.0115(11) C57 0.0228(11) 0.0354(13) 0.0352(13) -0.0111(10) -0.0063(9) 0.0002(10) C58 0.0149(9) 0.0228(10) 0.0251(11) 0.0007(8) -0.0035(8) 0.0019(8) C59 0.0227(11) 0.0340(12) 0.0262(11) 0.0034(9) -0.0035(9) -0.0031(9) C60 0.0326(13) 0.0429(14) 0.0263(12) -0.0011(10) -0.0045(10) 0.0018(11) C61 0.0367(14) 0.0378(14) 0.0383(14) -0.0143(11) -0.0148(11) 0.0061(11) C62 0.0295(12) 0.0272(12) 0.0528(16) -0.0083(11) -0.0112(11) -0.0020(10) C63 0.0220(11) 0.0237(11) 0.0364(12) -0.0002(9) -0.0038(9) -0.0018(9) C64 0.0200(10) 0.0223(10) 0.0315(11) 0.0007(8) -0.0059(8) -0.0064(8) C65 0.0534(16) 0.0390(14) 0.0320(13) 0.0028(11) -0.0129(11) -0.0229(13) C66 0.072(2) 0.0475(17) 0.0491(17) -0.0042(13) -0.0264(15) -0.0311(16) C67 0.0572(18) 0.0392(15) 0.074(2) 0.0021(14) -0.0228(16) -0.0305(14) C68 0.0536(17) 0.0410(15) 0.0607(18) -0.0012(13) 0.0011(14) -0.0303(14) C69 0.0408(14) 0.0361(13) 0.0410(14) -0.0040(11) 0.0002(11) -0.0225(11) C70 0.0322(12) 0.0249(11) 0.0202(10) 0.0004(8) -0.0057(8) -0.0118(9) C71 0.0440(14) 0.0367(13) 0.0309(12) 0.0037(10) -0.0041(10) -0.0223(11) C72 0.083(2) 0.0366(14) 0.0358(14) 0.0100(11) -0.0107(14) -0.0341(15) C73 0.0646(19) 0.0280(13) 0.0384(15) 0.0066(11) -0.0233(13) -0.0101(13) C74 0.0402(14) 0.0340(14) 0.0437(15) 0.0014(11) -0.0166(12) -0.0035(11) C75 0.0310(12) 0.0302(12) 0.0353(13) 0.0029(10) -0.0087(10) -0.0095(10) N1 0.0174(8) 0.0185(8) 0.0205(8) -0.0012(6) 0.0007(6) -0.0066(7) N2 0.0184(8) 0.0225(8) 0.0206(8) -0.0032(7) 0.0015(6) -0.0089(7) O1 0.0324(9) 0.0302(9) 0.0511(10) -0.0121(8) 0.0008(8) -0.0177(7) O2 0.0254(8) 0.0209(7) 0.0316(8) -0.0003(6) -0.0015(6) -0.0084(6) O3 0.0262(10) 0.0448(11) 0.0746(14) -0.0247(10) -0.0051(9) -0.0115(8) C1SA 0.0593(18) 0.0622(19) 0.069(2) 0.0029(16) -0.0037(16) -0.0364(16) Cl1A 0.0502(5) 0.0723(6) 0.0593(6) 0.0018(4) -0.0028(4) -0.0371(5) Cl2A 0.0990(12) 0.0607(8) 0.141(2) 0.0001(10) -0.0314(13) -0.0501(8) C1SB 0.0593(18) 0.0622(19) 0.069(2) 0.0029(16) -0.0037(16) -0.0364(16) Cl1B 0.0502(5) 0.0723(6) 0.0593(6) 0.0018(4) -0.0028(4) -0.0371(5) Cl2B 0.0990(12) 0.0607(8) 0.141(2) 0.0001(10) -0.0314(13) -0.0501(8) C1SC 0.0593(18) 0.0622(19) 0.069(2) 0.0029(16) -0.0037(16) -0.0364(16) Cl1C 0.091(4) 0.127(5) 0.091(3) 0.029(3) -0.017(3) -0.074(4) Cl2C 0.091(4) 0.127(5) 0.091(3) 0.029(3) -0.017(3) -0.074(4) C2S 0.0473(16) 0.0543(17) 0.0543(17) -0.0095(14) -0.0053(13) -0.0303(14) Cl3S 0.0807(6) 0.1054(8) 0.0632(5) 0.0209(5) -0.0159(5) -0.0513(6) Cl4S 0.0675(6) 0.0881(7) 0.1311(9) -0.0459(7) 0.0048(6) -0.0526(6) C1P 0.067(7) 0.049(4) 0.098(9) -0.020(5) 0.007(6) -0.023(5) C2P 0.054(4) 0.067(3) 0.043(3) -0.004(3) -0.002(3) -0.035(3) C3P 0.029(4) 0.044(3) 0.042(6) 0.000(3) -0.001(3) -0.012(3) C4P 0.044(3) 0.052(3) 0.069(4) 0.016(3) -0.001(3) -0.019(3) C5P 0.074(10) 0.039(4) 0.124(11) -0.010(5) 0.029(7) -0.024(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 Rh1 C27 1.797(2) . ? Rh1 C1 1.9875(19) . ? Rh1 O2 2.0455(15) . ? Rh1 O1 2.0642(15) . ? C1 N1 1.367(2) . ? C1 N2 1.372(2) . ? C2 C3 1.336(3) . ? C2 N1 1.385(3) . ? C2 H2 0.9500 . ? C3 N2 1.388(3) . ? C3 H3 0.9500 . ? C4 C9 1.399(3) . ? C4 C5 1.400(3) . ? C4 N2 1.440(2) . ? C5 C6 1.390(3) . ? C5 C11 1.526(3) . ? C6 C7 1.390(3) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 C12 1.503(3) . ? C8 C9 1.392(3) . ? C8 H8 0.9500 . ? C9 C10 1.524(3) . ? C10 C34 1.526(3) . ? C10 C28 1.530(3) . ? C10 H10 1.0000 . ? C11 C46 1.523(3) . ? C11 C40 1.525(3) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.393(3) . ? C13 C18 1.396(3) . ? C13 N1 1.447(2) . ? C14 C15 1.390(3) . ? C14 C20 1.528(3) . ? C15 C16 1.380(3) . ? C15 H15 0.9500 . ? C16 C17 1.391(3) . ? C16 C21 1.505(3) . ? C17 C18 1.388(3) . ? C17 H17 0.9500 . ? C18 C19 1.523(3) . ? C19 C58 1.522(3) . ? C19 C52 1.523(3) . ? C19 H19 1.0000 . ? C20 C64 1.530(3) . ? C20 C70 1.531(3) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.519(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O1 1.266(3) . ? C23 C24 1.385(4) . ? C24 C25 1.390(3) . ? C24 H24 0.9500 . ? C25 O2 1.278(3) . ? C25 C26 1.502(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O3 1.149(3) . ? C28 C29 1.383(4) . ? C28 C33 1.394(4) . ? C29 C30 1.393(4) . ? C29 H29 0.9500 . ? C30 C31 1.372(5) . ? C30 H30 0.9500 . ? C31 C32 1.374(5) . ? C31 H31 0.9500 . ? C32 C33 1.372(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.382(4) . ? C34 C39 1.395(3) . ? C35 C36 1.387(4) . ? C35 H35 0.9500 . ? C36 C37 1.369(4) . ? C36 H36 0.9500 . ? C37 C38 1.371(5) . ? C37 H37 0.9500 . ? C38 C39 1.392(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.387(3) . ? C40 C41 1.391(3) . ? C41 C42 1.386(3) . ? C41 H41 0.9500 . ? C42 C43 1.376(4) . ? C42 H42 0.9500 . ? C43 C44 1.370(4) . ? C43 H43 0.9500 . ? C44 C45 1.386(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.387(3) . ? C46 C51 1.390(3) . ? C47 C48 1.383(4) . ? C47 H47 0.9500 . ? C48 C49 1.374(4) . ? C48 H48 0.9500 . ? C49 C50 1.372(4) . ? C49 H49 0.9500 . ? C50 C51 1.386(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.376(3) . ? C52 C57 1.394(3) . ? C53 C54 1.391(4) . ? C53 H53 0.9500 . ? C54 C55 1.370(4) . ? C54 H54 0.9500 . ? C55 C56 1.374(4) . ? C55 H55 0.9500 . ? C56 C57 1.377(4) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C63 1.385(3) . ? C58 C59 1.394(3) . ? C59 C60 1.381(3) . ? C59 H59 0.9500 . ? C60 C61 1.378(4) . ? C60 H60 0.9500 . ? C61 C62 1.384(4) . ? C61 H61 0.9500 . ? C62 C63 1.389(3) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C69 1.382(3) . ? C64 C65 1.391(3) . ? C65 C66 1.378(4) . ? C65 H65 0.9500 . ? C66 C67 1.372(5) . ? C66 H66 0.9500 . ? C67 C68 1.374(4) . ? C67 H67 0.9500 . ? C68 C69 1.392(4) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C71 1.383(3) . ? C70 C75 1.387(3) . ? C71 C72 1.393(4) . ? C71 H71 0.9500 . ? C72 C73 1.374(4) . ? C72 H72 0.9500 . ? C73 C74 1.371(4) . ? C73 H73 0.9500 . ? C74 C75 1.388(3) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C1SA Cl2A 1.731(4) . ? C1SA Cl1A 1.762(3) . ? C1SA H1S1 0.9900 . ? C1SA H1S2 0.9900 . ? C2S Cl4S 1.757(3) . ? C2S Cl3S 1.762(3) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C1P C2P 1.515(8) . ? C1P H1P1 0.9800 . ? C1P H1P2 0.9800 . ? C1P H1P3 0.9800 . ? C2P C3P 1.505(7) . ? C2P H2P1 0.9900 . ? C2P H2P2 0.9900 . ? C3P C4P 1.520(7) . ? C3P H3P1 0.9900 . ? C3P H3P2 0.9900 . ? C4P C5P 1.517(9) . ? C4P H4P1 0.9900 . ? C4P H4P2 0.9900 . ? C5P H5P1 0.9800 . ? C5P H5P2 0.9800 . ? C5P H5P3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Rh1 C1 91.09(9) . . ? C27 Rh1 O2 177.06(8) . . ? C1 Rh1 O2 91.79(7) . . ? C27 Rh1 O1 87.56(8) . . ? C1 Rh1 O1 177.85(7) . . ? O2 Rh1 O1 89.57(6) . . ? N1 C1 N2 102.98(16) . . ? N1 C1 Rh1 128.30(14) . . ? N2 C1 Rh1 128.66(14) . . ? C3 C2 N1 107.21(18) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? C2 C3 N2 106.64(18) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? C9 C4 C5 122.04(18) . . ? C9 C4 N2 118.32(18) . . ? C5 C4 N2 119.64(18) . . ? C6 C5 C4 117.51(19) . . ? C6 C5 C11 121.43(19) . . ? C4 C5 C11 121.01(18) . . ? C5 C6 C7 121.9(2) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 118.67(19) . . ? C8 C7 C12 120.9(2) . . ? C6 C7 C12 120.4(2) . . ? C7 C8 C9 122.0(2) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C8 C9 C4 117.63(19) . . ? C8 C9 C10 121.58(19) . . ? C4 C9 C10 120.68(18) . . ? C9 C10 C34 113.20(17) . . ? C9 C10 C28 111.89(19) . . ? C34 C10 C28 112.51(18) . . ? C9 C10 H10 106.2 . . ? C34 C10 H10 106.2 . . ? C28 C10 H10 106.2 . . ? C46 C11 C40 111.12(18) . . ? C46 C11 C5 111.12(18) . . ? C40 C11 C5 113.99(18) . . ? C46 C11 H11 106.7 . . ? C40 C11 H11 106.7 . . ? C5 C11 H11 106.7 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 122.21(18) . . ? C14 C13 N1 118.27(17) . . ? C18 C13 N1 119.52(17) . . ? C15 C14 C13 117.65(18) . . ? C15 C14 C20 119.83(17) . . ? C13 C14 C20 122.50(18) . . ? C16 C15 C14 122.21(18) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 118.35(18) . . ? C15 C16 C21 120.58(18) . . ? C17 C16 C21 121.07(19) . . ? C18 C17 C16 122.00(19) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C13 117.56(18) . . ? C17 C18 C19 122.33(18) . . ? C13 C18 C19 120.10(17) . . ? C58 C19 C52 111.32(16) . . ? C58 C19 C18 114.51(16) . . ? C52 C19 C18 112.56(17) . . ? C58 C19 H19 105.9 . . ? C52 C19 H19 105.9 . . ? C18 C19 H19 105.9 . . ? C14 C20 C64 112.55(17) . . ? C14 C20 C70 111.53(17) . . ? C64 C20 C70 111.54(17) . . ? C14 C20 H20 106.9 . . ? C64 C20 H20 106.9 . . ? C70 C20 H20 106.9 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C23 C24 125.8(2) . . ? O1 C23 C22 114.9(2) . . ? C24 C23 C22 119.2(2) . . ? C23 C24 C25 126.7(2) . . ? C23 C24 H24 116.7 . . ? C25 C24 H24 116.7 . . ? O2 C25 C24 126.1(2) . . ? O2 C25 C26 115.5(2) . . ? C24 C25 C26 118.4(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 Rh1 175.04(19) . . ? C29 C28 C33 118.4(2) . . ? C29 C28 C10 123.3(2) . . ? C33 C28 C10 118.3(2) . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.6(3) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 119.6(3) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C28 121.1(3) . . ? C32 C33 H33 119.5 . . ? C28 C33 H33 119.5 . . ? C35 C34 C39 118.6(2) . . ? C35 C34 C10 119.4(2) . . ? C39 C34 C10 122.0(2) . . ? C34 C35 C36 120.9(3) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C37 C36 C35 120.2(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 119.8(3) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C39 120.7(3) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 119.8(3) . . ? C38 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? C45 C40 C41 118.0(2) . . ? C45 C40 C11 120.1(2) . . ? C41 C40 C11 122.0(2) . . ? C42 C41 C40 120.9(2) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C43 C42 C41 120.1(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 119.7(2) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 120.5(3) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C40 120.8(3) . . ? C44 C45 H45 119.6 . . ? C40 C45 H45 119.6 . . ? C47 C46 C51 118.3(2) . . ? C47 C46 C11 119.3(2) . . ? C51 C46 C11 122.5(2) . . ? C48 C47 C46 120.8(3) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C49 C48 C47 120.5(3) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C50 C49 C48 119.5(3) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C49 C50 C51 120.6(3) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C50 C51 C46 120.5(3) . . ? C50 C51 H51 119.8 . . ? C46 C51 H51 119.8 . . ? C53 C52 C57 118.0(2) . . ? C53 C52 C19 123.63(19) . . ? C57 C52 C19 118.4(2) . . ? C52 C53 C54 120.8(2) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C55 C54 C53 120.6(3) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C54 C55 C56 119.2(2) . . ? C54 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? C55 C56 C57 120.5(2) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C56 C57 C52 120.9(2) . . ? C56 C57 H57 119.5 . . ? C52 C57 H57 119.5 . . ? C63 C58 C59 118.6(2) . . ? C63 C58 C19 119.18(19) . . ? C59 C58 C19 122.2(2) . . ? C60 C59 C58 120.7(2) . . ? C60 C59 H59 119.6 . . ? C58 C59 H59 119.6 . . ? C61 C60 C59 120.1(2) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C62 120.0(2) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C63 119.8(3) . . ? C61 C62 H62 120.1 . . ? C63 C62 H62 120.1 . . ? C58 C63 C62 120.7(2) . . ? C58 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C69 C64 C65 118.0(2) . . ? C69 C64 C20 123.8(2) . . ? C65 C64 C20 118.2(2) . . ? C66 C65 C64 120.6(3) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C67 C66 C65 121.2(3) . . ? C67 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? C66 C67 C68 119.0(3) . . ? C66 C67 H67 120.5 . . ? C68 C67 H67 120.5 . . ? C67 C68 C69 120.2(3) . . ? C67 C68 H68 119.9 . . ? C69 C68 H68 119.9 . . ? C64 C69 C68 121.1(2) . . ? C64 C69 H69 119.5 . . ? C68 C69 H69 119.5 . . ? C71 C70 C75 118.6(2) . . ? C71 C70 C20 119.0(2) . . ? C75 C70 C20 122.4(2) . . ? C70 C71 C72 120.3(3) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C73 C72 C71 120.5(3) . . ? C73 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? C74 C73 C72 119.6(2) . . ? C74 C73 H73 120.2 . . ? C72 C73 H73 120.2 . . ? C73 C74 C75 120.3(3) . . ? C73 C74 H74 119.9 . . ? C75 C74 H74 119.9 . . ? C70 C75 C74 120.8(2) . . ? C70 C75 H75 119.6 . . ? C74 C75 H75 119.6 . . ? C1 N1 C2 111.56(16) . . ? C1 N1 C13 125.81(16) . . ? C2 N1 C13 122.35(16) . . ? C1 N2 C3 111.61(16) . . ? C1 N2 C4 123.15(16) . . ? C3 N2 C4 124.91(17) . . ? C23 O1 Rh1 125.97(16) . . ? C25 O2 Rh1 125.64(15) . . ? Cl2A C1SA Cl1A 115.28(19) . . ? Cl2A C1SA H1S1 108.5 . . ? Cl1A C1SA H1S1 108.5 . . ? Cl2A C1SA H1S2 108.5 . . ? Cl1A C1SA H1S2 108.5 . . ? H1S1 C1SA H1S2 107.5 . . ? Cl4S C2S Cl3S 112.47(17) . . ? Cl4S C2S H2S1 109.1 . . ? Cl3S C2S H2S1 109.1 . . ? Cl4S C2S H2S2 109.1 . . ? Cl3S C2S H2S2 109.1 . . ? H2S1 C2S H2S2 107.8 . . ? C3P C2P C1P 114.6(6) . . ? C3P C2P H2P1 108.6 . . ? C1P C2P H2P1 108.6 . . ? C3P C2P H2P2 108.6 . . ? C1P C2P H2P2 108.6 . . ? H2P1 C2P H2P2 107.6 . . ? C2P C3P C4P 113.6(5) . . ? C2P C3P H3P1 108.8 . . ? C4P C3P H3P1 108.8 . . ? C2P C3P H3P2 108.8 . . ? C4P C3P H3P2 108.8 . . ? H3P1 C3P H3P2 107.7 . . ? C5P C4P C3P 112.8(7) . . ? C5P C4P H4P1 109.0 . . ? C3P C4P H4P1 109.0 . . ? C5P C4P H4P2 109.0 . . ? C3P C4P H4P2 109.0 . . ? H4P1 C4P H4P2 107.8 . . ? 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 C27 Rh1 C1 N1 -135.81(18) . . . . ? O2 Rh1 C1 N1 44.76(17) . . . . ? C27 Rh1 C1 N2 40.69(19) . . . . ? O2 Rh1 C1 N2 -138.74(17) . . . . ? N1 C2 C3 N2 -1.1(2) . . . . ? C9 C4 C5 C6 -4.5(3) . . . . ? N2 C4 C5 C6 175.73(18) . . . . ? C9 C4 C5 C11 173.03(19) . . . . ? N2 C4 C5 C11 -6.7(3) . . . . ? C4 C5 C6 C7 0.9(3) . . . . ? C11 C5 C6 C7 -176.6(2) . . . . ? C5 C6 C7 C8 2.5(3) . . . . ? C5 C6 C7 C12 -178.1(2) . . . . ? C6 C7 C8 C9 -2.4(3) . . . . ? C12 C7 C8 C9 178.2(2) . . . . ? C7 C8 C9 C4 -1.1(3) . . . . ? C7 C8 C9 C10 175.1(2) . . . . ? C5 C4 C9 C8 4.6(3) . . . . ? N2 C4 C9 C8 -175.64(18) . . . . ? C5 C4 C9 C10 -171.55(19) . . . . ? N2 C4 C9 C10 8.2(3) . . . . ? C8 C9 C10 C34 33.4(3) . . . . ? C4 C9 C10 C34 -150.6(2) . . . . ? C8 C9 C10 C28 -95.0(2) . . . . ? C4 C9 C10 C28 81.0(2) . . . . ? C6 C5 C11 C46 97.7(2) . . . . ? C4 C5 C11 C46 -79.8(2) . . . . ? C6 C5 C11 C40 -28.8(3) . . . . ? C4 C5 C11 C40 153.73(19) . . . . ? C18 C13 C14 C15 -1.8(3) . . . . ? N1 C13 C14 C15 179.28(17) . . . . ? C18 C13 C14 C20 176.23(18) . . . . ? N1 C13 C14 C20 -2.7(3) . . . . ? C13 C14 C15 C16 0.7(3) . . . . ? C20 C14 C15 C16 -177.44(18) . . . . ? C14 C15 C16 C17 0.7(3) . . . . ? C14 C15 C16 C21 -179.95(19) . . . . ? C15 C16 C17 C18 -0.9(3) . . . . ? C21 C16 C17 C18 179.69(19) . . . . ? C16 C17 C18 C13 -0.2(3) . . . . ? C16 C17 C18 C19 178.89(18) . . . . ? C14 C13 C18 C17 1.6(3) . . . . ? N1 C13 C18 C17 -179.54(17) . . . . ? C14 C13 C18 C19 -177.50(18) . . . . ? N1 C13 C18 C19 1.4(3) . . . . ? C17 C18 C19 C58 19.2(3) . . . . ? C13 C18 C19 C58 -161.74(18) . . . . ? C17 C18 C19 C52 -109.2(2) . . . . ? C13 C18 C19 C52 69.8(2) . . . . ? C15 C14 C20 C64 81.9(2) . . . . ? C13 C14 C20 C64 -96.1(2) . . . . ? C15 C14 C20 C70 -44.3(2) . . . . ? C13 C14 C20 C70 137.66(19) . . . . ? O1 C23 C24 C25 -3.4(5) . . . . ? C22 C23 C24 C25 174.0(3) . . . . ? C23 C24 C25 O2 6.0(4) . . . . ? C23 C24 C25 C26 -173.2(3) . . . . ? C9 C10 C28 C29 -1.7(3) . . . . ? C34 C10 C28 C29 -130.4(2) . . . . ? C9 C10 C28 C33 -179.3(2) . . . . ? C34 C10 C28 C33 52.0(3) . . . . ? C33 C28 C29 C30 1.4(4) . . . . ? C10 C28 C29 C30 -176.2(2) . . . . ? C28 C29 C30 C31 -0.9(4) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C30 C31 C32 C33 0.9(4) . . . . ? C31 C32 C33 C28 -0.4(4) . . . . ? C29 C28 C33 C32 -0.8(4) . . . . ? C10 C28 C33 C32 177.0(2) . . . . ? C9 C10 C34 C35 95.1(2) . . . . ? C28 C10 C34 C35 -136.8(2) . . . . ? C9 C10 C34 C39 -84.6(3) . . . . ? C28 C10 C34 C39 43.5(3) . . . . ? C39 C34 C35 C36 0.9(4) . . . . ? C10 C34 C35 C36 -178.9(2) . . . . ? C34 C35 C36 C37 0.2(4) . . . . ? C35 C36 C37 C38 -0.7(4) . . . . ? C36 C37 C38 C39 0.2(4) . . . . ? C37 C38 C39 C34 0.9(4) . . . . ? C35 C34 C39 C38 -1.4(4) . . . . ? C10 C34 C39 C38 178.3(2) . . . . ? C46 C11 C40 C45 135.8(2) . . . . ? C5 C11 C40 C45 -97.7(2) . . . . ? C46 C11 C40 C41 -44.0(3) . . . . ? C5 C11 C40 C41 82.5(3) . . . . ? C45 C40 C41 C42 2.6(4) . . . . ? C11 C40 C41 C42 -177.6(2) . . . . ? C40 C41 C42 C43 -1.4(4) . . . . ? C41 C42 C43 C44 -0.2(4) . . . . ? C42 C43 C44 C45 0.5(4) . . . . ? C43 C44 C45 C40 0.7(4) . . . . ? C41 C40 C45 C44 -2.2(4) . . . . ? C11 C40 C45 C44 178.0(2) . . . . ? C40 C11 C46 C47 -78.9(2) . . . . ? C5 C11 C46 C47 153.0(2) . . . . ? C40 C11 C46 C51 101.3(2) . . . . ? C5 C11 C46 C51 -26.7(3) . . . . ? C51 C46 C47 C48 1.1(4) . . . . ? C11 C46 C47 C48 -178.7(2) . . . . ? C46 C47 C48 C49 -0.6(4) . . . . ? C47 C48 C49 C50 0.1(4) . . . . ? C48 C49 C50 C51 0.0(4) . . . . ? C49 C50 C51 C46 0.5(4) . . . . ? C47 C46 C51 C50 -1.0(4) . . . . ? C11 C46 C51 C50 178.8(2) . . . . ? C58 C19 C52 C53 -110.4(2) . . . . ? C18 C19 C52 C53 19.7(3) . . . . ? C58 C19 C52 C57 69.4(2) . . . . ? C18 C19 C52 C57 -160.44(19) . . . . ? C57 C52 C53 C54 0.9(4) . . . . ? C19 C52 C53 C54 -179.3(3) . . . . ? C52 C53 C54 C55 -1.2(5) . . . . ? C53 C54 C55 C56 0.5(5) . . . . ? C54 C55 C56 C57 0.4(4) . . . . ? C55 C56 C57 C52 -0.7(4) . . . . ? C53 C52 C57 C56 0.0(4) . . . . ? C19 C52 C57 C56 -179.8(2) . . . . ? C52 C19 C58 C63 -124.7(2) . . . . ? C18 C19 C58 C63 106.2(2) . . . . ? C52 C19 C58 C59 54.2(3) . . . . ? C18 C19 C58 C59 -74.9(2) . . . . ? C63 C58 C59 C60 -2.2(3) . . . . ? C19 C58 C59 C60 178.9(2) . . . . ? C58 C59 C60 C61 1.4(3) . . . . ? C59 C60 C61 C62 0.6(4) . . . . ? C60 C61 C62 C63 -1.8(4) . . . . ? C59 C58 C63 C62 0.9(3) . . . . ? C19 C58 C63 C62 179.90(19) . . . . ? C61 C62 C63 C58 1.0(3) . . . . ? C14 C20 C64 C69 -18.3(3) . . . . ? C70 C20 C64 C69 107.9(2) . . . . ? C14 C20 C64 C65 163.2(2) . . . . ? C70 C20 C64 C65 -70.5(3) . . . . ? C69 C64 C65 C66 -1.0(4) . . . . ? C20 C64 C65 C66 177.6(2) . . . . ? C64 C65 C66 C67 0.4(5) . . . . ? C65 C66 C67 C68 0.4(5) . . . . ? C66 C67 C68 C69 -0.8(5) . . . . ? C65 C64 C69 C68 0.6(4) . . . . ? C20 C64 C69 C68 -177.8(2) . . . . ? C67 C68 C69 C64 0.2(4) . . . . ? C14 C20 C70 C71 -83.5(2) . . . . ? C64 C20 C70 C71 149.7(2) . . . . ? C14 C20 C70 C75 95.2(2) . . . . ? C64 C20 C70 C75 -31.6(3) . . . . ? C75 C70 C71 C72 -0.6(3) . . . . ? C20 C70 C71 C72 178.2(2) . . . . ? C70 C71 C72 C73 0.1(4) . . . . ? C71 C72 C73 C74 0.6(4) . . . . ? C72 C73 C74 C75 -0.7(4) . . . . ? C71 C70 C75 C74 0.5(3) . . . . ? C20 C70 C75 C74 -178.2(2) . . . . ? C73 C74 C75 C70 0.2(4) . . . . ? N2 C1 N1 C2 -0.1(2) . . . . ? Rh1 C1 N1 C2 177.12(14) . . . . ? N2 C1 N1 C13 173.88(17) . . . . ? Rh1 C1 N1 C13 -8.9(3) . . . . ? C3 C2 N1 C1 0.7(2) . . . . ? C3 C2 N1 C13 -173.45(18) . . . . ? C14 C13 N1 C1 -108.5(2) . . . . ? C18 C13 N1 C1 72.6(3) . . . . ? C14 C13 N1 C2 64.9(2) . . . . ? C18 C13 N1 C2 -114.1(2) . . . . ? N1 C1 N2 C3 -0.6(2) . . . . ? Rh1 C1 N2 C3 -177.79(14) . . . . ? N1 C1 N2 C4 -174.31(17) . . . . ? Rh1 C1 N2 C4 8.5(3) . . . . ? C2 C3 N2 C1 1.1(2) . . . . ? C2 C3 N2 C4 174.65(19) . . . . ? C9 C4 N2 C1 70.0(3) . . . . ? C5 C4 N2 C1 -110.2(2) . . . . ? C9 C4 N2 C3 -102.8(2) . . . . ? C5 C4 N2 C3 76.9(3) . . . . ? C24 C23 O1 Rh1 0.8(4) . . . . ? C22 C23 O1 Rh1 -176.8(2) . . . . ? C27 Rh1 O1 C23 -179.6(2) . . . . ? O2 Rh1 O1 C23 -0.2(2) . . . . ? C24 C25 O2 Rh1 -5.5(3) . . . . ? C26 C25 O2 Rh1 173.81(15) . . . . ? C1 Rh1 O2 C25 -175.87(17) . . . . ? O1 Rh1 O2 C25 2.47(17) . . . . ? C1P C2P C3P C4P 177.7(11) . . . . ? C2P C3P C4P C5P 177.8(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.924 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.065 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 359 52 ' ' _platon_squeeze_details ; ;