#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:13:23 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242483 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132509.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4132509 loop_ _publ_author_name 'Shing, Ka-Pan' 'Cao, Bei' 'Liu, Yungen' 'Lee, Hung Kay' 'Li, Ming-De' 'Phillips, David Lee' 'Chang, Xiao-Yong' 'Che, Chi-Ming' _publ_section_title ; Arylruthenium(III) Porphyrin-Catalyzed C-H Oxidation and Epoxidation at Room Temperature and [RuV(Por)(O)(Ph)] Intermediate by Spectroscopic Analysis and Density Functional Theory Calculations. ; _journal_issue 22 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7032 _journal_page_last 7042 _journal_paper_doi 10.1021/jacs.8b04470 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C54 H35 Cl8 N4 O Ru, C4 H10 O, C3 H7' _chemical_formula_sum 'C61 H52 Cl8 N4 O2 Ru' _chemical_formula_weight 1257.73 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _audit_creation_date 2014-06-20 _audit_creation_method ; Olex2 1.2 (compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846) ; _cell_angle_alpha 90 _cell_angle_beta 95.011(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.5729(12) _cell_length_b 21.6205(16) _cell_length_c 21.910(2) _cell_measurement_reflns_used 2707 _cell_measurement_temperature 100 _cell_measurement_theta_max 65.359 _cell_measurement_theta_min 29.465 _cell_volume 5933.1(9) _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.951 _diffrn_measured_fraction_theta_max 0.965 _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_unetI/netI 0.0487 _diffrn_reflns_Laue_measured_fraction_full 0.951 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 72964 _diffrn_reflns_point_group_measured_fraction_full 0.951 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 67.005 _diffrn_reflns_theta_min 2.877 _exptl_absorpt_coefficient_mu 5.814 _exptl_absorpt_correction_T_max 0.7529 _exptl_absorpt_correction_T_min 0.4553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1325 before and 0.0983 after correction. The Ratio of minimum to maximum transmission is 0.6047. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.408 _exptl_crystal_description prism _exptl_crystal_F_000 2568 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.556 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 707 _refine_ls_number_reflns 10195 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0641 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+29.9429P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1642 _refine_ls_wR_factor_ref 0.1784 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8606 _reflns_number_total 10195 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04470_si_002.cif _cod_data_source_block complex_1 _cod_original_cell_volume 5932.9(9) _cod_database_code 4132509 _shelxl_version_number 2013-4 _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. ; _shelx_estimated_absorpt_t_max 0.722 _shelx_estimated_absorpt_t_min 0.324 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Restrained distances C59-C60 = C61-C60 = C59_$1-C59 1.54 with sigma of 0.01 3. Rigid bond restraints C61, C60, C59 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints C61 \\sim C60 \\sim C59: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 5. Others Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C51A)= Sof(H51C)=Sof(H51D)=Sof(C53A)=Sof(H53C)=Sof(H53D)=1-FVAR(1) Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C51)= Sof(H51A)=Sof(H51B)=Sof(C53)=Sof(H53A)=Sof(H53B)=FVAR(1) 6.a Secondary CH2 refined with riding coordinates: C56(H56A,H56B), C57(H57A,H57B), C51(H51A,H51B), C53(H53A,H53B), C51A(H51C, H51D), C53A(H53C,H53D), C60(H60A,H60B), C59(H59A,H59B) 6.b Me refined with riding coordinates: C54(H54A,H54B,H54C), C54(H54D,H54E,H54F), C52(H52A,H52B,H52C), C52(H52D,H52E, H52F) 6.c Aromatic/amide H refined with riding coordinates: C2(H2), C46(H46), C8(H8), C12(H12), C13(H13), C17(H17), C31(H31), C3(H3), C18(H18), C36(H36), C25(H25), C23(H23), C41(H41), C50(H50), C35(H35), C49(H49), C7(H7), C48(H48), C37(H37), C24(H24), C42(H42), C43(H43), C47(H47), C30(H30), C29(H29) 6.d Idealised Me refined as rotating group: C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C61(H61A,H61B,H61C) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Ru1 Ru 0.99651(3) 0.08009(2) 0.76345(2) 0.02350(14) Uani 1 1 d . . . . . Cl5 Cl 0.74933(11) 0.28587(6) 0.70928(7) 0.0404(3) Uani 1 1 d . . . . . Cl7 Cl 0.90909(12) 0.06445(6) 0.52289(7) 0.0408(3) Uani 1 1 d . . . . . Cl1 Cl 1.23964(12) -0.13128(7) 0.82435(8) 0.0486(4) Uani 1 1 d . . . . . Cl2 Cl 1.39425(11) 0.05015(8) 0.68749(8) 0.0514(4) Uani 1 1 d . . . . . Cl8 Cl 0.76502(14) -0.12282(7) 0.65496(7) 0.0512(4) Uani 1 1 d . . . . . N3 N 0.9468(3) 0.14863(19) 0.8180(2) 0.0270(9) Uani 1 1 d . . . . . N2 N 1.1397(3) 0.07750(18) 0.8138(2) 0.0264(9) Uani 1 1 d . . . . . N4 N 0.8497(3) 0.07863(18) 0.7166(2) 0.0272(9) Uani 1 1 d . . . . . N1 N 1.0427(3) 0.00869(18) 0.71199(19) 0.0245(9) Uani 1 1 d . . . . . Cl6 Cl 0.58532(14) 0.10043(9) 0.83579(13) 0.0834(8) Uani 1 1 d . . . . . Cl4 Cl 1.20558(13) 0.28226(7) 0.83922(7) 0.0485(4) Uani 1 1 d . . . . . Cl3 Cl 1.12689(18) 0.12109(9) 1.01709(8) 0.0670(5) Uani 1 1 d . . . . . C1 C 0.9851(4) -0.0184(2) 0.6632(2) 0.0259(10) Uani 1 1 d . . . . . C4 C 1.1405(4) -0.0207(2) 0.7169(2) 0.0249(10) Uani 1 1 d . . . . . C11 C 1.0076(4) 0.1783(2) 0.8645(2) 0.0284(11) Uani 1 1 d . . . . . C45 C 1.0513(4) 0.1435(2) 0.7039(2) 0.0277(11) Uani 1 1 d . . . . . C2 C 1.0468(4) -0.0656(2) 0.6376(2) 0.0278(11) Uani 1 1 d . . . . . H2 H 1.0247 -0.0912 0.6036 0.033 Uiso 1 1 calc R . . . . C9 C 1.1741(4) 0.1166(2) 0.8613(2) 0.0272(11) Uani 1 1 d . . . . . C21 C 1.3254(4) -0.0429(2) 0.7568(2) 0.0299(11) Uani 1 1 d . . . . . C14 C 0.8478(4) 0.1758(2) 0.8137(3) 0.0297(11) Uani 1 1 d . . . . . C6 C 1.2241(4) 0.0386(2) 0.8058(2) 0.0277(11) Uani 1 1 d . . . . . C10 C 1.1138(4) 0.1642(2) 0.8839(2) 0.0288(11) Uani 1 1 d . . . . . C20 C 0.8813(4) -0.0015(2) 0.6407(2) 0.0273(11) Uani 1 1 d . . . . . C46 C 0.9825(5) 0.1777(3) 0.6645(3) 0.0563(19) Uani 1 1 d . . . . . H46 H 0.9078 0.1728 0.6662 0.068 Uiso 1 1 calc R . . . . C19 C 0.8185(4) 0.0424(2) 0.6663(2) 0.0286(11) Uani 1 1 d . . . . . C39 C 0.8360(4) -0.0328(2) 0.5835(2) 0.0300(11) Uani 1 1 d . . . . . C8 C 1.2815(4) 0.1013(3) 0.8837(3) 0.0331(12) Uani 1 1 d . . . . . H8 H 1.3233 0.1214 0.9160 0.040 Uiso 1 1 calc R . . . . C5 C 1.2249(4) -0.0069(2) 0.7612(2) 0.0282(11) Uani 1 1 d . . . . . C12 C 0.9449(4) 0.2252(2) 0.8906(3) 0.0349(12) Uani 1 1 d . . . . . H12 H 0.9678 0.2523 0.9232 0.042 Uiso 1 1 calc R . . . . C13 C 0.8469(4) 0.2233(3) 0.8600(3) 0.0367(13) Uani 1 1 d . . . . . H13 H 0.7878 0.2487 0.8675 0.044 Uiso 1 1 calc R . . . . C17 C 0.6761(4) 0.1009(3) 0.6820(3) 0.0368(13) Uani 1 1 d . . . . . H17 H 0.6073 0.1194 0.6791 0.044 Uiso 1 1 calc R . . . . C33 C 0.6601(4) 0.1959(2) 0.7730(3) 0.0332(12) Uani 1 1 d . . . . . C16 C 0.7632(4) 0.1153(2) 0.7269(3) 0.0314(12) Uani 1 1 d . . . . . C32 C 1.2137(4) 0.2611(2) 0.9162(3) 0.0349(12) Uani 1 1 d . . . . . C31 C 1.2630(5) 0.3006(3) 0.9593(3) 0.0449(15) Uani 1 1 d . . . . . H31 H 1.2933 0.3383 0.9470 0.054 Uiso 1 1 calc R . . . . C3 C 1.1427(4) -0.0673(2) 0.6708(2) 0.0289(11) Uani 1 1 d . . . . . H3 H 1.2004 -0.0942 0.6647 0.035 Uiso 1 1 calc R . . . . C38 C 0.6446(4) 0.2532(2) 0.7449(3) 0.0326(12) Uani 1 1 d . . . . . C26 C 1.4079(4) -0.0214(3) 0.7239(3) 0.0385(13) Uani 1 1 d . . . . . C18 C 0.7096(4) 0.0563(3) 0.6448(3) 0.0358(13) Uani 1 1 d . . . . . H18 H 0.6691 0.0378 0.6110 0.043 Uiso 1 1 calc R . . . . C36 C 0.4654(5) 0.2599(4) 0.7713(4) 0.0594(19) Uani 1 1 d . . . . . H36 H 0.3993 0.2813 0.7708 0.071 Uiso 1 1 calc R . . . . C28 C 1.1775(6) 0.1910(3) 0.9938(3) 0.0452(15) Uani 1 1 d . . . . . C25 C 1.5002(5) -0.0564(4) 0.7176(3) 0.0503(16) Uani 1 1 d . . . . . H25 H 1.5556 -0.0406 0.6951 0.060 Uiso 1 1 calc R . . . . C40 C 0.7830(5) -0.0893(3) 0.5845(3) 0.0400(14) Uani 1 1 d . . . . . C23 C 1.4303(5) -0.1368(3) 0.7768(3) 0.0450(15) Uani 1 1 d . . . . . H23 H 1.4372 -0.1768 0.7948 0.054 Uiso 1 1 calc R . . . . C44 C 0.8452(4) -0.0066(2) 0.5261(3) 0.0331(12) Uani 1 1 d . . . . . C41 C 0.7439(6) -0.1193(3) 0.5311(3) 0.0557(18) Uani 1 1 d . . . . . H41 H 0.7085 -0.1580 0.5329 0.067 Uiso 1 1 calc R . . . . C50 C 1.1593(5) 0.1534(3) 0.7007(3) 0.0495(16) Uani 1 1 d . . . . . H50 H 1.2088 0.1307 0.7272 0.059 Uiso 1 1 calc R . . . . C35 C 0.4765(5) 0.2031(4) 0.7990(4) 0.062(2) Uani 1 1 d . . . . . H35 H 0.4183 0.1850 0.8173 0.074 Uiso 1 1 calc R . . . . C49 C 1.1969(5) 0.1944(3) 0.6609(3) 0.0485(16) Uani 1 1 d . . . . . H49 H 1.2716 0.2007 0.6609 0.058 Uiso 1 1 calc R . . . . C15 C 0.7623(4) 0.1606(2) 0.7714(3) 0.0307(12) Uani 1 1 d . . . . . C34 C 0.5731(5) 0.1724(3) 0.8000(4) 0.0505(17) Uani 1 1 d . . . . . C27 C 1.1679(4) 0.2057(2) 0.9314(3) 0.0328(12) Uani 1 1 d . . . . . C7 C 1.3121(4) 0.0532(2) 0.8501(3) 0.0309(11) Uani 1 1 d . . . . . H7 H 1.3791 0.0327 0.8549 0.037 Uiso 1 1 calc R . . . . C22 C 1.3397(4) -0.1010(3) 0.7833(3) 0.0371(13) Uani 1 1 d . . . . . C48 C 1.1278(5) 0.2269(3) 0.6207(3) 0.0438(14) Uani 1 1 d . . . . . H48 H 1.1542 0.2546 0.5919 0.053 Uiso 1 1 calc R . . . . C37 C 0.5493(5) 0.2864(3) 0.7440(3) 0.0403(13) Uani 1 1 d . . . . . H37 H 0.5424 0.3259 0.7252 0.048 Uiso 1 1 calc R . . . . C24 C 1.5093(5) -0.1134(3) 0.7443(3) 0.0475(16) Uani 1 1 d . . . . . H24 H 1.5716 -0.1373 0.7402 0.057 Uiso 1 1 calc R . . . . C42 C 0.7574(6) -0.0920(3) 0.4756(3) 0.0566(18) Uani 1 1 d . . . . . H42 H 0.7324 -0.1127 0.4389 0.068 Uiso 1 1 calc R . . . . C43 C 0.8062(5) -0.0353(3) 0.4721(3) 0.0439(14) Uani 1 1 d . . . . . H43 H 0.8130 -0.0163 0.4335 0.053 Uiso 1 1 calc R . . . . C47 C 1.0191(6) 0.2185(4) 0.6230(4) 0.063(2) Uani 1 1 d . . . . . H47 H 0.9699 0.2409 0.5960 0.076 Uiso 1 1 calc R . . . . C30 C 1.2676(6) 0.2850(3) 1.0193(3) 0.0521(17) Uani 1 1 d . . . . . H30 H 1.2999 0.3126 1.0492 0.063 Uiso 1 1 calc R . . . . C29 C 1.2264(6) 0.2300(3) 1.0374(3) 0.0563(18) Uani 1 1 d . . . . . H29 H 1.2313 0.2189 1.0795 0.068 Uiso 1 1 calc R . . . . O1 O 0.9389(3) 0.00844(17) 0.83132(18) 0.0370(9) Uani 1 1 d . . . . . O2 O 0.9916(6) 0.3272(3) 1.0140(3) 0.0891(19) Uani 1 1 d . . . . . C56 C 0.9877(9) 0.3026(6) 1.0754(5) 0.096(3) Uani 1 1 d . . . . . H56A H 0.9514 0.3323 1.1010 0.115 Uiso 1 1 calc R . . . . H56B H 1.0610 0.2957 1.0945 0.115 Uiso 1 1 calc R . . . . C57 C 1.0411(9) 0.3861(5) 1.0134(6) 0.102(4) Uani 1 1 d . . . . . H57A H 1.1152 0.3831 1.0326 0.122 Uiso 1 1 calc R . . . . H57B H 1.0018 0.4157 1.0376 0.122 Uiso 1 1 calc R . . . . C55 C 0.9259(9) 0.2411(5) 1.0705(5) 0.099(3) Uani 1 1 d . . . . . H55A H 0.8565 0.2476 1.0475 0.148 Uiso 1 1 calc GR . . . . H55B H 0.9151 0.2260 1.1117 0.148 Uiso 1 1 calc GR . . . . H55C H 0.9669 0.2105 1.0493 0.148 Uiso 1 1 calc GR . . . . C58 C 1.0421(10) 0.4103(7) 0.9458(6) 0.129(5) Uani 1 1 d . . . . . H58A H 1.0911 0.3850 0.9239 0.194 Uiso 1 1 calc GR . . . . H58B H 1.0659 0.4535 0.9463 0.194 Uiso 1 1 calc GR . . . . H58C H 0.9700 0.4075 0.9250 0.194 Uiso 1 1 calc GR . . . . C54 C 0.7592(5) -0.0344(3) 0.8191(4) 0.0517(17) Uani 1 1 d . . . . . H54A H 0.7211 -0.0317 0.7782 0.078 Uiso 0.470(11) 1 calc R . P A 1 H54B H 0.7488 0.0040 0.8415 0.078 Uiso 0.470(11) 1 calc R . P A 1 H54C H 0.7313 -0.0693 0.8413 0.078 Uiso 0.470(11) 1 calc R . P A 1 H54D H 0.7616 -0.0286 0.7749 0.078 Uiso 0.530(11) 1 calc R . P A 2 H54E H 0.6864 -0.0270 0.8301 0.078 Uiso 0.530(11) 1 calc R . P A 2 H54F H 0.7804 -0.0769 0.8301 0.078 Uiso 0.530(11) 1 calc R . P A 2 C52 C 1.0622(5) -0.0283(3) 0.9175(3) 0.0490(16) Uani 1 1 d . . . . . H52A H 1.0924 -0.0443 0.8809 0.074 Uiso 0.470(11) 1 calc R . P A 1 H52B H 1.0392 -0.0629 0.9420 0.074 Uiso 0.470(11) 1 calc R . P A 1 H52C H 1.1164 -0.0041 0.9419 0.074 Uiso 0.470(11) 1 calc R . P A 1 H52D H 1.1311 -0.0089 0.9119 0.074 Uiso 0.530(11) 1 calc R . P A 2 H52E H 1.0739 -0.0670 0.9403 0.074 Uiso 0.530(11) 1 calc R . P A 2 H52F H 1.0190 -0.0002 0.9403 0.074 Uiso 0.530(11) 1 calc R . P A 2 C51 C 0.9650(12) 0.0134(6) 0.8980(6) 0.047(4) Uani 0.470(11) 1 d . . P A 1 H51A H 0.9029 0.0004 0.9197 0.056 Uiso 0.470(11) 1 calc R . P A 1 H51B H 0.9819 0.0569 0.9091 0.056 Uiso 0.470(11) 1 calc R . P A 1 C53 C 0.8773(11) -0.0440(6) 0.8131(6) 0.045(4) Uani 0.470(11) 1 d . . P A 1 H53A H 0.9026 -0.0798 0.8386 0.055 Uiso 0.470(11) 1 calc R . P A 1 H53B H 0.8880 -0.0539 0.7700 0.055 Uiso 0.470(11) 1 calc R . P A 1 C51A C 1.0032(9) -0.0420(5) 0.8544(5) 0.039(3) Uani 0.530(11) 1 d . . P A 2 H51C H 1.0562 -0.0518 0.8249 0.047 Uiso 0.530(11) 1 calc R . P A 2 H51D H 0.9573 -0.0789 0.8577 0.047 Uiso 0.530(11) 1 calc R . P A 2 C53A C 0.8351(9) 0.0106(5) 0.8533(6) 0.042(3) Uani 0.530(11) 1 d . . P A 2 H53C H 0.8061 0.0531 0.8483 0.050 Uiso 0.530(11) 1 calc R . P A 2 H53D H 0.8408 0.0005 0.8975 0.050 Uiso 0.530(11) 1 calc R . P A 2 C60 C 0.5512(15) -0.0565(6) 0.9414(6) 0.153(4) Uani 1 1 d D U . . . H60A H 0.5123 -0.0407 0.9033 0.183 Uiso 1 1 calc R . . . . H60B H 0.6235 -0.0380 0.9445 0.183 Uiso 1 1 calc R . . . . C59 C 0.4942(14) -0.0350(2) 0.9951(6) 0.153(5) Uani 1 1 d D U . . . H59A H 0.5238 -0.0568 1.0326 0.184 Uiso 1 1 calc R . . . . H59B H 0.4175 -0.0456 0.9881 0.184 Uiso 1 1 calc R . . . . C61 C 0.5621(17) -0.1255(7) 0.9359(9) 0.183(6) Uani 1 1 d D U . . . H61A H 0.5615 -0.1369 0.8926 0.274 Uiso 1 1 calc GR . . . . H61B H 0.5024 -0.1458 0.9538 0.274 Uiso 1 1 calc GR . . . . H61C H 0.6296 -0.1388 0.9578 0.274 Uiso 1 1 calc GR . . . . 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 Ru1 0.0207(2) 0.0164(2) 0.0330(2) -0.00014(15) -0.00040(15) -0.00141(13) Cl5 0.0410(7) 0.0346(7) 0.0455(8) 0.0039(6) 0.0029(6) -0.0053(6) Cl7 0.0500(8) 0.0282(7) 0.0438(8) 0.0083(6) 0.0021(6) 0.0001(6) Cl1 0.0469(8) 0.0324(7) 0.0663(10) 0.0149(7) 0.0032(7) 0.0064(6) Cl2 0.0325(7) 0.0558(9) 0.0671(10) 0.0209(8) 0.0115(7) 0.0036(6) Cl8 0.0658(10) 0.0336(8) 0.0522(9) 0.0075(7) -0.0065(7) -0.0212(7) N3 0.023(2) 0.020(2) 0.038(2) -0.0014(18) 0.0015(18) -0.0034(16) N2 0.025(2) 0.021(2) 0.033(2) -0.0017(18) 0.0023(18) -0.0032(16) N4 0.023(2) 0.018(2) 0.040(2) -0.0023(18) 0.0008(18) -0.0027(16) N1 0.022(2) 0.019(2) 0.032(2) 0.0017(17) -0.0024(17) -0.0017(16) Cl6 0.0376(9) 0.0616(11) 0.154(2) 0.0578(13) 0.0281(11) 0.0106(8) Cl4 0.0618(9) 0.0346(7) 0.0477(8) 0.0063(6) -0.0020(7) -0.0198(7) Cl3 0.1025(15) 0.0518(10) 0.0479(9) 0.0095(8) 0.0131(9) -0.0258(10) C1 0.027(2) 0.018(2) 0.033(3) 0.000(2) 0.001(2) -0.0007(19) C4 0.025(2) 0.018(2) 0.031(3) 0.002(2) 0.001(2) 0.0015(19) C11 0.031(3) 0.018(2) 0.037(3) 0.000(2) 0.006(2) -0.003(2) C45 0.026(2) 0.020(2) 0.037(3) -0.004(2) -0.002(2) -0.002(2) C2 0.032(3) 0.020(2) 0.031(3) -0.001(2) -0.001(2) 0.003(2) C9 0.027(2) 0.022(2) 0.032(3) 0.001(2) 0.003(2) -0.004(2) C21 0.030(3) 0.030(3) 0.029(3) -0.004(2) -0.003(2) 0.005(2) C14 0.028(3) 0.021(2) 0.040(3) -0.003(2) 0.004(2) -0.003(2) C6 0.023(2) 0.022(2) 0.038(3) 0.005(2) -0.001(2) 0.0005(19) C10 0.032(3) 0.021(2) 0.033(3) 0.001(2) 0.002(2) -0.006(2) C20 0.025(2) 0.020(2) 0.035(3) 0.003(2) -0.005(2) -0.003(2) C46 0.035(3) 0.064(4) 0.069(5) 0.026(4) -0.008(3) -0.017(3) C19 0.027(3) 0.020(2) 0.037(3) 0.000(2) -0.005(2) -0.002(2) C39 0.027(3) 0.025(3) 0.036(3) -0.001(2) -0.007(2) 0.003(2) C8 0.028(3) 0.031(3) 0.039(3) 0.002(2) -0.003(2) -0.008(2) C5 0.025(3) 0.024(3) 0.036(3) 0.004(2) 0.003(2) -0.001(2) C12 0.037(3) 0.023(3) 0.045(3) -0.008(2) 0.007(2) -0.003(2) C13 0.032(3) 0.027(3) 0.052(3) -0.008(3) 0.009(3) 0.001(2) C17 0.022(3) 0.028(3) 0.058(4) -0.003(3) -0.004(2) 0.002(2) C33 0.028(3) 0.024(3) 0.048(3) -0.005(2) 0.004(2) 0.003(2) C16 0.026(3) 0.020(2) 0.049(3) 0.000(2) 0.001(2) -0.003(2) C32 0.035(3) 0.026(3) 0.044(3) -0.002(2) -0.001(2) -0.003(2) C31 0.042(3) 0.035(3) 0.057(4) -0.006(3) -0.006(3) -0.010(3) C3 0.032(3) 0.021(2) 0.033(3) 0.002(2) 0.002(2) 0.004(2) C38 0.033(3) 0.025(3) 0.040(3) -0.007(2) 0.003(2) -0.002(2) C26 0.032(3) 0.044(3) 0.039(3) 0.002(3) -0.001(2) 0.007(2) C18 0.022(3) 0.031(3) 0.053(3) -0.005(3) -0.008(2) -0.002(2) C36 0.030(3) 0.066(5) 0.084(5) 0.004(4) 0.015(3) 0.021(3) C28 0.060(4) 0.038(3) 0.037(3) 0.001(3) 0.003(3) -0.011(3) C25 0.029(3) 0.073(5) 0.049(4) 0.000(4) 0.004(3) 0.010(3) C40 0.046(3) 0.025(3) 0.046(3) -0.002(3) -0.009(3) -0.006(2) C23 0.046(4) 0.038(3) 0.049(4) -0.003(3) -0.010(3) 0.018(3) C44 0.029(3) 0.028(3) 0.040(3) 0.004(2) -0.005(2) 0.001(2) C41 0.066(4) 0.044(4) 0.053(4) 0.001(3) -0.017(3) -0.020(3) C50 0.036(3) 0.046(4) 0.067(4) 0.026(3) 0.004(3) 0.005(3) C35 0.034(3) 0.062(5) 0.093(6) 0.030(4) 0.024(4) 0.016(3) C49 0.037(3) 0.047(4) 0.063(4) 0.013(3) 0.012(3) -0.001(3) C15 0.027(3) 0.017(2) 0.048(3) 0.000(2) 0.005(2) -0.002(2) C34 0.032(3) 0.042(4) 0.078(5) 0.022(3) 0.014(3) 0.006(3) C27 0.030(3) 0.026(3) 0.042(3) -0.004(2) -0.002(2) 0.001(2) C7 0.024(2) 0.027(3) 0.041(3) -0.001(2) -0.003(2) -0.001(2) C22 0.033(3) 0.036(3) 0.040(3) -0.001(3) -0.003(2) 0.004(2) C48 0.052(4) 0.041(3) 0.039(3) 0.002(3) 0.004(3) -0.011(3) C37 0.046(3) 0.027(3) 0.047(3) -0.001(3) 0.002(3) 0.006(3) C24 0.030(3) 0.059(4) 0.051(4) -0.002(3) -0.005(3) 0.021(3) C42 0.063(4) 0.053(4) 0.050(4) -0.011(3) -0.018(3) -0.005(3) C43 0.045(3) 0.044(4) 0.041(3) -0.001(3) -0.008(3) 0.000(3) C47 0.052(4) 0.059(4) 0.075(5) 0.033(4) -0.012(4) -0.013(3) C30 0.057(4) 0.040(4) 0.056(4) -0.011(3) -0.010(3) -0.007(3) C29 0.068(5) 0.058(4) 0.041(4) -0.001(3) -0.004(3) -0.003(4) O1 0.035(2) 0.030(2) 0.046(2) 0.0000(18) 0.0067(17) -0.0069(16) O2 0.096(5) 0.085(4) 0.084(4) -0.017(4) -0.008(4) 0.011(4) C56 0.095(7) 0.125(9) 0.067(6) -0.009(6) -0.002(5) 0.030(7) C57 0.084(7) 0.080(7) 0.137(10) -0.040(7) -0.011(7) 0.005(6) C55 0.105(8) 0.103(8) 0.093(7) 0.014(6) 0.031(6) 0.039(7) C58 0.082(8) 0.188(15) 0.120(10) 0.047(10) 0.015(7) 0.045(8) C54 0.041(3) 0.041(4) 0.073(5) 0.001(3) 0.004(3) -0.013(3) C52 0.051(4) 0.046(4) 0.049(4) 0.010(3) 0.001(3) -0.005(3) C51 0.055(8) 0.040(7) 0.046(8) -0.012(6) 0.006(6) -0.012(6) C53 0.049(8) 0.042(8) 0.045(8) 0.007(6) 0.002(6) -0.015(6) C51A 0.038(6) 0.033(6) 0.048(7) 0.009(5) 0.007(5) 0.004(5) C53A 0.035(6) 0.032(6) 0.058(7) -0.002(5) 0.003(5) 0.000(5) C60 0.203(12) 0.139(8) 0.122(8) 0.024(8) 0.044(8) 0.046(9) C59 0.204(12) 0.141(9) 0.119(8) 0.040(8) 0.042(8) 0.047(10) C61 0.243(16) 0.144(10) 0.157(12) -0.011(10) -0.006(12) 0.028(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_3 N3 Ru1 C45 91.37(19) . N3 Ru1 O1 88.89(15) . N2 Ru1 N3 90.22(16) . N2 Ru1 N4 176.39(17) . N2 Ru1 C45 91.92(18) . N2 Ru1 O1 86.80(15) . N4 Ru1 N3 89.79(16) . N4 Ru1 C45 91.69(18) . N4 Ru1 O1 89.59(15) . N1 Ru1 N3 177.07(16) . N1 Ru1 N2 89.90(16) . N1 Ru1 N4 89.92(16) . N1 Ru1 C45 91.55(18) . N1 Ru1 O1 88.19(15) . C45 Ru1 O1 178.70(17) . C11 N3 Ru1 126.5(3) . C14 N3 Ru1 126.5(3) . C14 N3 C11 107.0(4) . C9 N2 Ru1 126.8(3) . C6 N2 Ru1 127.2(3) . C6 N2 C9 106.0(4) . C19 N4 Ru1 126.5(3) . C19 N4 C16 106.4(4) . C16 N4 Ru1 127.0(4) . C1 N1 Ru1 127.1(3) . C1 N1 C4 105.7(4) . C4 N1 Ru1 127.2(3) . N1 C1 C2 110.2(4) . N1 C1 C20 125.1(5) . C20 C1 C2 124.7(5) . N1 C4 C5 124.7(5) . N1 C4 C3 110.0(4) . C5 C4 C3 125.3(5) . N3 C11 C10 125.1(5) . N3 C11 C12 109.6(5) . C10 C11 C12 125.3(5) . C46 C45 Ru1 121.8(4) . C46 C45 C50 116.8(5) . C50 C45 Ru1 121.3(4) . C3 C2 C1 107.3(5) . N2 C9 C10 125.1(5) . N2 C9 C8 109.9(4) . C10 C9 C8 125.0(5) . C26 C21 C5 122.1(5) . C22 C21 C5 121.6(5) . C22 C21 C26 116.3(5) . N3 C14 C13 108.6(5) . N3 C14 C15 125.9(5) . C15 C14 C13 125.5(5) . N2 C6 C5 125.1(5) . N2 C6 C7 109.5(4) . C5 C6 C7 125.3(5) . C11 C10 C27 116.5(5) . C9 C10 C11 126.0(5) . C9 C10 C27 117.5(5) . C1 C20 C39 116.9(5) . C19 C20 C1 125.6(5) . C19 C20 C39 117.5(4) . C47 C46 C45 121.9(6) . N4 C19 C20 125.4(4) . N4 C19 C18 109.8(5) . C20 C19 C18 124.7(5) . C40 C39 C20 122.2(5) . C40 C39 C44 116.5(5) . C44 C39 C20 121.3(5) . C7 C8 C9 107.3(5) . C4 C5 C21 115.8(5) . C6 C5 C4 125.9(5) . C6 C5 C21 118.2(5) . C13 C12 C11 106.9(5) . C12 C13 C14 107.9(5) . C18 C17 C16 107.9(5) . C38 C33 C15 122.1(5) . C34 C33 C38 115.5(5) . C34 C33 C15 122.3(5) . N4 C16 C17 109.1(5) . N4 C16 C15 125.2(5) . C15 C16 C17 125.6(5) . C31 C32 Cl4 119.0(5) . C31 C32 C27 122.8(6) . C27 C32 Cl4 118.1(4) . C30 C31 C32 119.3(6) . C2 C3 C4 106.9(5) . C33 C38 Cl5 118.5(4) . C33 C38 C37 123.5(5) . C37 C38 Cl5 117.9(4) . C21 C26 Cl2 119.0(4) . C21 C26 C25 122.1(6) . C25 C26 Cl2 118.9(5) . C17 C18 C19 106.7(5) . C35 C36 C37 120.6(6) . C27 C28 Cl3 118.9(5) . C29 C28 Cl3 118.8(5) . C29 C28 C27 122.2(6) . C24 C25 C26 118.9(6) . C39 C40 Cl8 118.6(4) . C41 C40 Cl8 119.3(5) . C41 C40 C39 122.2(6) . C24 C23 C22 118.9(6) . C39 C44 Cl7 118.0(4) . C43 C44 Cl7 119.4(5) . C43 C44 C39 122.6(5) . C42 C41 C40 118.7(6) . C49 C50 C45 122.1(6) . C36 C35 C34 119.5(6) . C50 C49 C48 120.7(6) . C14 C15 C33 118.4(5) . C16 C15 C14 125.6(5) . C16 C15 C33 116.0(5) . C33 C34 Cl6 118.6(5) . C35 C34 Cl6 118.6(5) . C35 C34 C33 122.8(6) . C32 C27 C10 121.7(5) . C32 C27 C28 115.5(5) . C28 C27 C10 122.8(5) . C8 C7 C6 107.3(5) . C21 C22 Cl1 119.0(4) . C21 C22 C23 122.5(6) . C23 C22 Cl1 118.5(5) . C49 C48 C47 118.7(6) . C36 C37 C38 118.0(6) . C25 C24 C23 121.4(6) . C43 C42 C41 121.5(6) . C42 C43 C44 118.5(6) . C46 C47 C48 119.8(6) . C31 C30 C29 120.8(6) . C30 C29 C28 119.2(6) . C51 O1 Ru1 122.3(6) . C53 O1 Ru1 123.6(6) . C53 O1 C51 114.1(8) . C51A O1 Ru1 122.8(5) . C51A O1 C53A 114.3(7) . C53A O1 Ru1 122.8(5) . C57 O2 C56 112.8(9) . O2 C56 C55 108.1(8) . O2 C57 C58 110.3(10) . O1 C51 C52 109.4(9) . O1 C53 C54 112.5(10) . O1 C51A C52 112.6(8) . O1 C53A C54 111.5(8) . C61 C60 C59 115.0(12) . C60 C59 C59 111.6(13) 3_657 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ru1 N3 2.036(4) . Ru1 N2 2.028(4) . Ru1 N4 2.033(4) . Ru1 N1 2.026(4) . Ru1 C45 2.053(5) . Ru1 O1 2.308(4) . Cl5 C38 1.738(6) . Cl7 C44 1.738(5) . Cl1 C22 1.737(6) . Cl2 C26 1.742(6) . Cl8 C40 1.738(6) . N3 C11 1.378(7) . N3 C14 1.373(7) . N2 C9 1.381(7) . N2 C6 1.378(6) . N4 C19 1.380(7) . N4 C16 1.380(7) . N1 C1 1.368(6) . N1 C4 1.381(6) . Cl6 C34 1.743(6) . Cl4 C32 1.741(6) . Cl3 C28 1.734(6) . C1 C2 1.426(7) . C1 C20 1.403(7) . C4 C5 1.406(7) . C4 C3 1.427(7) . C11 C10 1.399(7) . C11 C12 1.433(7) . C45 C46 1.380(8) . C45 C50 1.382(8) . C2 C3 1.353(7) . C9 C10 1.395(7) . C9 C8 1.434(7) . C21 C5 1.495(7) . C21 C26 1.393(8) . C21 C22 1.390(8) . C14 C13 1.444(8) . C14 C15 1.396(8) . C6 C5 1.386(8) . C6 C7 1.442(7) . C10 C27 1.492(7) . C20 C19 1.385(7) . C20 C39 1.491(7) . C46 C47 1.376(9) . C19 C18 1.440(7) . C39 C40 1.393(8) . C39 C44 1.394(8) . C8 C7 1.349(8) . C12 C13 1.351(8) . C17 C16 1.440(8) . C17 C18 1.354(8) . C33 C38 1.390(8) . C33 C15 1.498(7) . C33 C34 1.385(8) . C16 C15 1.383(8) . C32 C31 1.380(8) . C32 C27 1.382(8) . C31 C30 1.353(10) . C38 C37 1.394(8) . C26 C25 1.403(8) . C36 C35 1.373(10) . C36 C37 1.382(10) . C28 C27 1.397(8) . C28 C29 1.379(9) . C25 C24 1.365(10) . C40 C41 1.390(9) . C23 C22 1.395(8) . C23 C24 1.369(10) . C44 C43 1.387(8) . C41 C42 1.376(10) . C50 C49 1.357(9) . C35 C34 1.383(9) . C49 C48 1.375(9) . C48 C47 1.384(10) . C42 C43 1.375(10) . C30 C29 1.369(10) . O1 C51 1.473(14) . O1 C53 1.411(13) . O1 C51A 1.424(11) . O1 C53A 1.431(12) . O2 C56 1.450(12) . O2 C57 1.418(12) . C56 C55 1.539(16) . C57 C58 1.573(17) . C54 C53 1.517(15) . C54 C53A 1.515(13) . C52 C51 1.548(16) . C52 C51A 1.540(13) . C60 C59 1.505(9) . C60 C61 1.504(9) . C59 C59 1.532(10) 3_657 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_4 Ru1 N3 C11 C10 -2.8(7) . Ru1 N3 C11 C12 178.0(3) . Ru1 N3 C14 C13 -178.5(4) . Ru1 N3 C14 C15 0.8(8) . Ru1 N2 C9 C10 1.8(7) . Ru1 N2 C9 C8 -177.7(3) . Ru1 N2 C6 C5 -0.8(7) . Ru1 N2 C6 C7 178.2(3) . Ru1 N4 C19 C20 3.0(7) . Ru1 N4 C19 C18 -177.9(4) . Ru1 N4 C16 C17 178.0(4) . Ru1 N4 C16 C15 0.8(8) . Ru1 N1 C1 C2 177.7(3) . Ru1 N1 C1 C20 -1.1(7) . Ru1 N1 C4 C5 2.6(7) . Ru1 N1 C4 C3 -177.9(3) . Ru1 C45 C46 C47 -177.5(6) . Ru1 C45 C50 C49 178.9(6) . Ru1 O1 C51 C52 -97.7(8) . Ru1 O1 C53 C54 -98.7(9) . Ru1 O1 C51A C52 96.4(8) . Ru1 O1 C53A C54 99.9(8) . Cl5 C38 C37 C36 178.8(5) . Cl7 C44 C43 C42 179.0(5) . Cl2 C26 C25 C24 -177.7(5) . Cl8 C40 C41 C42 179.1(6) . N3 C11 C10 C9 -2.8(9) . N3 C11 C10 C27 174.8(5) . N3 C11 C12 C13 0.3(6) . N3 C14 C13 C12 1.1(6) . N3 C14 C15 C33 -179.1(5) . N3 C14 C15 C16 0.5(9) . N2 C9 C10 C11 3.4(8) . N2 C9 C10 C27 -174.2(5) . N2 C9 C8 C7 -0.1(6) . N2 C6 C5 C4 0.2(8) . N2 C6 C5 C21 176.9(5) . N2 C6 C7 C8 -1.3(6) . N4 C19 C18 C17 0.2(6) . N4 C16 C15 C14 -1.4(9) . N4 C16 C15 C33 178.3(5) . N1 C1 C2 C3 -0.2(6) . N1 C1 C20 C19 -4.1(8) . N1 C1 C20 C39 174.5(5) . N1 C4 C5 C21 -177.9(5) . N1 C4 C5 C6 -1.2(8) . N1 C4 C3 C2 0.7(6) . Cl4 C32 C31 C30 178.7(5) . Cl4 C32 C27 C10 0.7(7) . Cl4 C32 C27 C28 179.6(5) . Cl3 C28 C27 C10 1.3(8) . Cl3 C28 C27 C32 -177.6(5) . Cl3 C28 C29 C30 179.2(6) . C1 N1 C4 C5 179.7(5) . C1 N1 C4 C3 -0.8(5) . C1 C2 C3 C4 -0.3(6) . C1 C20 C19 N4 3.0(9) . C1 C20 C19 C18 -175.9(5) . C1 C20 C39 C40 86.8(7) . C1 C20 C39 C44 -93.0(6) . C4 N1 C1 C2 0.6(5) . C4 N1 C1 C20 -178.2(5) . C11 N3 C14 C13 -0.9(6) . C11 N3 C14 C15 178.4(5) . C11 C10 C27 C32 -83.3(7) . C11 C10 C27 C28 97.9(7) . C11 C12 C13 C14 -0.8(6) . C45 C46 C47 C48 -1.0(13) . C45 C50 C49 C48 -1.7(11) . C2 C1 C20 C19 177.2(5) . C2 C1 C20 C39 -4.2(8) . C9 N2 C6 C5 -177.8(5) . C9 N2 C6 C7 1.2(6) . C9 C10 C27 C32 94.6(6) . C9 C10 C27 C28 -84.3(7) . C9 C8 C7 C6 0.9(6) . C21 C26 C25 C24 0.3(10) . C14 N3 C11 C10 179.6(5) . C14 N3 C11 C12 0.4(6) . C6 N2 C9 C10 178.9(5) . C6 N2 C9 C8 -0.7(6) . C10 C11 C12 C13 -178.9(5) . C10 C9 C8 C7 -179.7(5) . C20 C1 C2 C3 178.6(5) . C20 C19 C18 C17 179.3(5) . C20 C39 C40 Cl8 2.5(8) . C20 C39 C40 C41 -177.9(6) . C20 C39 C44 Cl7 -1.1(7) . C20 C39 C44 C43 178.4(5) . C46 C45 C50 C49 -0.2(10) . C19 N4 C16 C17 0.4(6) . C19 N4 C16 C15 -176.7(5) . C19 C20 C39 C40 -94.6(6) . C19 C20 C39 C44 85.7(6) . C39 C20 C19 N4 -175.5(5) . C39 C20 C19 C18 5.6(8) . C39 C40 C41 C42 -0.5(11) . C39 C44 C43 C42 -0.5(9) . C8 C9 C10 C11 -177.2(5) . C8 C9 C10 C27 5.2(8) . C5 C4 C3 C2 -179.8(5) . C5 C21 C26 Cl2 0.8(7) . C5 C21 C26 C25 -177.2(6) . C5 C21 C22 Cl1 -1.9(7) . C5 C21 C22 C23 176.4(5) . C5 C6 C7 C8 177.7(5) . C12 C11 C10 C9 176.2(5) . C12 C11 C10 C27 -6.1(8) . C13 C14 C15 C33 0.0(8) . C13 C14 C15 C16 179.7(5) . C17 C16 C15 C14 -178.1(5) . C17 C16 C15 C33 1.6(8) . C33 C38 C37 C36 -1.6(9) . C16 N4 C19 C20 -179.4(5) . C16 N4 C19 C18 -0.4(6) . C16 C17 C18 C19 0.1(7) . C32 C31 C30 C29 1.5(11) . C31 C32 C27 C10 179.2(5) . C31 C32 C27 C28 -1.9(9) . C31 C30 C29 C28 -1.5(11) . C3 C4 C5 C21 2.7(7) . C3 C4 C5 C6 179.4(5) . C38 C33 C15 C14 82.5(7) . C38 C33 C15 C16 -97.2(6) . C38 C33 C34 Cl6 179.5(5) . C38 C33 C34 C35 0.5(11) . C26 C21 C5 C4 92.5(6) . C26 C21 C5 C6 -84.5(7) . C26 C21 C22 Cl1 -179.4(4) . C26 C21 C22 C23 -1.1(8) . C26 C25 C24 C23 0.0(10) . C18 C17 C16 N4 -0.3(7) . C18 C17 C16 C15 176.8(5) . C36 C35 C34 Cl6 179.7(7) . C36 C35 C34 C33 -1.2(13) . C40 C39 C44 Cl7 179.1(4) . C40 C39 C44 C43 -1.4(8) . C40 C41 C42 C43 -1.5(12) . C44 C39 C40 Cl8 -177.7(4) . C44 C39 C40 C41 1.9(9) . C41 C42 C43 C44 2.0(11) . C50 C45 C46 C47 1.5(11) . C50 C49 C48 C47 2.2(11) . C35 C36 C37 C38 0.8(11) . C49 C48 C47 C46 -0.8(12) . C15 C14 C13 C12 -178.2(5) . C15 C33 C38 Cl5 -2.5(8) . C15 C33 C38 C37 177.9(5) . C15 C33 C34 Cl6 2.6(9) . C15 C33 C34 C35 -176.5(7) . C34 C33 C38 Cl5 -179.4(5) . C34 C33 C38 C37 1.0(9) . C34 C33 C15 C14 -100.8(7) . C34 C33 C15 C16 79.5(8) . C27 C32 C31 C30 0.2(10) . C27 C28 C29 C30 -0.4(11) . C7 C6 C5 C4 -178.6(5) . C7 C6 C5 C21 -2.0(8) . C22 C21 C5 C4 -84.8(6) . C22 C21 C5 C6 98.2(6) . C22 C21 C26 Cl2 178.2(4) . C22 C21 C26 C25 0.2(9) . C22 C23 C24 C25 -0.8(10) . C37 C36 C35 C34 0.6(13) . C24 C23 C22 Cl1 179.7(5) . C24 C23 C22 C21 1.4(9) . C29 C28 C27 C10 -179.1(6) . C29 C28 C27 C32 2.0(10) . C56 O2 C57 C58 -179.7(8) . C57 O2 C56 C55 176.2(8) . C51 O1 C53 C54 82.1(12) . C51 O1 C51A C52 -19.0(8) . C51 O1 C53A C54 -139.2(10) . C51 C52 C51A O1 18.8(8) . C53 O1 C51 C52 81.6(11) . C53 O1 C51A C52 -142.2(10) . C53 O1 C53A C54 -16.9(9) . C53 C54 C53A O1 16.3(8) . C51A O1 C51 C52 18.5(8) . C51A O1 C53 C54 140.7(11) . C51A O1 C53A C54 -79.5(10) . C51A C52 C51 O1 -17.7(7) . C53A O1 C51 C52 140.8(10) . C53A O1 C53 C54 17.0(9) . C53A O1 C51A C52 -84.2(9) . C53A C54 C53 O1 -16.7(9) . C61 C60 C59 C59 168.6(18) 3_657