#------------------------------------------------------------------------------ #$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/08/4300882.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_4300882 loop_ _publ_author_name 'Jian Li' 'Peter I. Djurovich' 'Bert D. Alleyne' 'Muhammed Yousufuddin' 'Nam N. Ho' 'J. Christopher Thomas' 'Jonas C. Peters' 'Robert Bau' 'Mark E. Thompson' _publ_section_title ; Synthetic Control of Excited-State Properties in Cyclometalated Ir(III) Complexes Using Ancillary Ligands ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1713 _journal_page_last 1727 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C72 H78 Cl6 F6 Ir2 N8 O6 S2' _chemical_formula_weight 1926.64 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 81.376(4) _cell_angle_beta 89.894(4) _cell_angle_gamma 89.963(3) _cell_formula_units_Z 2 _cell_length_a 13.262(3) _cell_length_b 13.655(3) _cell_length_c 22.981(5) _cell_measurement_reflns_used 5576 _cell_measurement_temperature 143(2) _cell_measurement_theta_max 27.28 _cell_measurement_theta_min 2.42 _cell_volume 4114.6(16) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 143(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 22705 _diffrn_reflns_theta_full 25.68 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_min 0.90 _exptl_absorpt_coefficient_mu 3.542 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _refine_diff_density_max 2.363 _refine_diff_density_min -1.180 _refine_diff_density_rms 0.138 _refine_ls_extinction_coef 0.00000(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 936 _refine_ls_number_reflns 15335 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0473 _refine_ls_shift/su_max 7.050 _refine_ls_shift/su_mean 0.010 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+1.7724P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1170 _refine_ls_wR_factor_ref 0.1262 _reflns_number_gt 11755 _reflns_number_total 15335 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048599hrom20041007_011931.cif _[local]_cod_data_source_block irtbuncm _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 4114.6(15) _cod_database_code 4300882 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ir1 Ir 0.321177(17) 0.023109(17) 0.745064(10) 0.03019(9) Uani 1 1 d . . . Ir2 Ir 0.821220(17) 0.476915(17) 0.754942(10) 0.03035(9) Uani 1 1 d . . . Cl1 Cl 0.4254(6) 0.6203(5) 0.6780(3) 0.250(4) Uani 1 1 d . . . Cl2 Cl 0.2368(4) 0.5397(5) 0.6664(3) 0.226(3) Uani 1 1 d . . . Cl3 Cl 0.3984(5) 0.4125(4) 0.6962(2) 0.199(3) Uani 1 1 d . . . Cl4 Cl 0.7374(4) 0.9610(5) 0.8339(3) 0.221(3) Uani 1 1 d . . . Cl5 Cl 0.9251(6) 0.8799(5) 0.8217(3) 0.252(4) Uani 1 1 d . . . Cl6 Cl 0.8986(5) 1.0870(4) 0.8044(2) 0.197(3) Uani 1 1 d . . . S1 S 0.38811(16) 0.40823(18) 0.87114(10) 0.0608(6) Uani 1 1 d . . . S2 S 0.88820(16) 0.09159(18) 0.62891(10) 0.0609(6) Uani 1 1 d . . . F1 F 0.4120(5) 0.5103(5) 0.9560(3) 0.103(2) Uani 1 1 d . . . F2 F 0.4095(5) 0.3577(6) 0.9836(3) 0.123(3) Uani 1 1 d . . . F3 F 0.2718(4) 0.4318(6) 0.9594(3) 0.102(2) Uani 1 1 d . . . F4 F 0.9102(5) 0.1424(6) 0.5166(3) 0.118(2) Uani 1 1 d . . . F5 F 0.9121(5) -0.0103(5) 0.5438(3) 0.0988(19) Uani 1 1 d . . . F6 F 0.7721(4) 0.0690(6) 0.5403(2) 0.099(2) Uani 1 1 d . . . O1 O 0.3388(5) 0.4957(6) 0.8374(3) 0.087(2) Uani 1 1 d . . . O2 O 0.3358(5) 0.3204(5) 0.8652(3) 0.083(2) Uani 1 1 d . . . O3 O 0.4948(4) 0.4076(5) 0.8659(3) 0.0751(18) Uani 1 1 d . . . O4 O 0.9950(4) 0.0928(5) 0.6343(3) 0.0753(18) Uani 1 1 d . . . O5 O 0.8388(5) 0.0053(6) 0.6620(3) 0.087(2) Uani 1 1 d . . . O6 O 0.8358(5) 0.1796(5) 0.6347(3) 0.084(2) Uani 1 1 d . . . N1 N 0.2142(4) -0.0857(4) 0.7426(2) 0.0386(13) Uani 1 1 d . . . N2 N 0.4485(4) 0.1089(4) 0.7478(2) 0.0307(11) Uani 1 1 d . . . N3 N 0.2130(4) 0.0842(4) 0.8561(3) 0.0396(13) Uani 1 1 d . . . N4 N 0.2519(4) 0.1681(4) 0.6326(3) 0.0407(13) Uani 1 1 d . . . N5 N 0.9487(4) 0.3913(4) 0.7518(2) 0.0327(12) Uani 1 1 d . . . N6 N 0.7145(4) 0.5864(4) 0.7576(3) 0.0413(13) Uani 1 1 d . . . N7 N 0.7517(4) 0.3320(4) 0.8678(2) 0.0417(13) Uani 1 1 d . . . N8 N 0.7134(4) 0.4152(4) 0.6436(3) 0.0411(13) Uani 1 1 d . . . C1 C 0.1339(5) -0.0772(7) 0.7049(4) 0.059(2) Uani 1 1 d . . . H1 H 0.1223 -0.0157 0.6805 0.071 Uiso 1 1 calc R . . C2 C 0.0707(7) -0.1533(8) 0.7012(5) 0.081(3) Uani 1 1 d . . . H2 H 0.0155 -0.1460 0.6746 0.098 Uiso 1 1 calc R . . C3 C 0.0882(7) -0.2422(8) 0.7370(5) 0.084(3) Uani 1 1 d . . . H3 H 0.0441 -0.2964 0.7353 0.101 Uiso 1 1 calc R . . C4 C 0.1689(7) -0.2535(7) 0.7754(4) 0.070(3) Uani 1 1 d . . . H4 H 0.1811 -0.3152 0.7995 0.084 Uiso 1 1 calc R . . C5 C 0.2315(5) -0.1734(5) 0.7782(3) 0.0449(17) Uani 1 1 d . . . C6 C 0.3177(5) -0.1722(5) 0.8166(3) 0.0396(15) Uani 1 1 d . . . C7 C 0.3428(6) -0.2500(5) 0.8614(3) 0.0490(18) Uani 1 1 d . . . H7 H 0.3058 -0.3101 0.8654 0.059 Uiso 1 1 calc R . . C8 C 0.4213(6) -0.2398(6) 0.8999(3) 0.053(2) Uani 1 1 d . . . H8 H 0.4370 -0.2928 0.9302 0.064 Uiso 1 1 calc R . . C9 C 0.4772(6) -0.1527(6) 0.8945(3) 0.0513(19) Uani 1 1 d . . . C10 C 0.4534(5) -0.0762(5) 0.8486(3) 0.0421(16) Uani 1 1 d . . . H10 H 0.4924 -0.0172 0.8444 0.051 Uiso 1 1 calc R . . C11 C 0.3757(5) -0.0829(5) 0.8094(3) 0.0334(14) Uani 1 1 d . . . C12 C 0.5619(7) -0.1417(8) 0.9366(4) 0.084(3) Uani 1 1 d . . . H12A H 0.5403 -0.1672 0.9768 0.126 Uiso 1 1 calc R . . H12B H 0.5798 -0.0716 0.9341 0.126 Uiso 1 1 calc R . . H12C H 0.6207 -0.1791 0.9263 0.126 Uiso 1 1 calc R . . C13 C 0.2486(5) 0.0699(5) 0.8129(3) 0.0359(15) Uani 1 1 d . . . C14 C 0.1794(6) 0.0864(7) 0.9163(3) 0.054(2) Uani 1 1 d . . . C15 C 0.1187(8) 0.1796(8) 0.9172(4) 0.083(3) Uani 1 1 d . . . H15A H 0.1628 0.2374 0.9081 0.124 Uiso 1 1 calc R . . H15B H 0.0887 0.1788 0.9562 0.124 Uiso 1 1 calc R . . H15C H 0.0650 0.1831 0.8877 0.124 Uiso 1 1 calc R . . C16 C 0.2750(8) 0.0876(10) 0.9535(4) 0.095(4) Uani 1 1 d . . . H16A H 0.3093 0.0235 0.9560 0.142 Uiso 1 1 calc R . . H16B H 0.2569 0.0999 0.9931 0.142 Uiso 1 1 calc R . . H16C H 0.3201 0.1402 0.9351 0.142 Uiso 1 1 calc R . . C17 C 0.1176(9) -0.0064(9) 0.9337(5) 0.107(4) Uani 1 1 d . . . H17A H 0.0574 -0.0039 0.9089 0.161 Uiso 1 1 calc R . . H17B H 0.0972 -0.0109 0.9751 0.161 Uiso 1 1 calc R . . H17C H 0.1581 -0.0645 0.9286 0.161 Uiso 1 1 calc R . . C18 C 0.4607(5) 0.1803(5) 0.7825(3) 0.0448(17) Uani 1 1 d . . . H18 H 0.4054 0.1959 0.8057 0.054 Uiso 1 1 calc R . . C19 C 0.5498(6) 0.2310(5) 0.7852(4) 0.0518(19) Uani 1 1 d . . . H19 H 0.5558 0.2816 0.8093 0.062 Uiso 1 1 calc R . . C20 C 0.6304(6) 0.2062(6) 0.7519(4) 0.059(2) Uani 1 1 d . . . H20 H 0.6934 0.2385 0.7539 0.071 Uiso 1 1 calc R . . C21 C 0.6199(6) 0.1364(6) 0.7168(3) 0.054(2) Uani 1 1 d . . . H21 H 0.6754 0.1203 0.6938 0.065 Uiso 1 1 calc R . . C22 C 0.5274(5) 0.0874(5) 0.7139(3) 0.0373(15) Uani 1 1 d . . . C23 C 0.5052(5) 0.0132(5) 0.6759(3) 0.0379(15) Uani 1 1 d . . . C24 C 0.5728(6) -0.0120(7) 0.6341(3) 0.055(2) Uani 1 1 d . . . H24 H 0.6389 0.0151 0.6316 0.067 Uiso 1 1 calc R . . C25 C 0.5441(6) -0.0760(7) 0.5967(4) 0.066(2) Uani 1 1 d . . . H25 H 0.5900 -0.0915 0.5676 0.079 Uiso 1 1 calc R . . C26 C 0.4488(6) -0.1187(6) 0.6005(4) 0.058(2) Uani 1 1 d . . . C27 C 0.3833(5) -0.0956(5) 0.6443(3) 0.0453(17) Uani 1 1 d . . . H27 H 0.3183 -0.1253 0.6477 0.054 Uiso 1 1 calc R . . C28 C 0.4099(5) -0.0307(5) 0.6832(3) 0.0367(15) Uani 1 1 d . . . C29 C 0.4159(8) -0.1866(9) 0.5574(5) 0.093(3) Uani 1 1 d . . . H29A H 0.3968 -0.1467 0.5200 0.139 Uiso 1 1 calc R . . H29B H 0.3580 -0.2262 0.5737 0.139 Uiso 1 1 calc R . . H29C H 0.4717 -0.2307 0.5508 0.139 Uiso 1 1 calc R . . C30 C 0.2700(5) 0.1182(5) 0.6762(3) 0.0378(15) Uani 1 1 d . . . C31 C 0.2449(6) 0.2127(6) 0.5709(3) 0.055(2) Uani 1 1 d . . . C32 C 0.3481(7) 0.2555(9) 0.5534(4) 0.089(3) Uani 1 1 d . . . H32A H 0.3682 0.3010 0.5806 0.134 Uiso 1 1 calc R . . H32B H 0.3454 0.2916 0.5132 0.134 Uiso 1 1 calc R . . H32C H 0.3975 0.2017 0.5553 0.134 Uiso 1 1 calc R . . C33 C 0.1637(7) 0.2920(7) 0.5632(4) 0.073(3) Uani 1 1 d . . . H33A H 0.0997 0.2635 0.5789 0.109 Uiso 1 1 calc R . . H33B H 0.1560 0.3177 0.5213 0.109 Uiso 1 1 calc R . . H33C H 0.1832 0.3462 0.5844 0.109 Uiso 1 1 calc R . . C34 C 0.2184(8) 0.1303(8) 0.5363(4) 0.082(3) Uani 1 1 d . . . H34A H 0.2695 0.0779 0.5433 0.123 Uiso 1 1 calc R . . H34B H 0.2164 0.1566 0.4942 0.123 Uiso 1 1 calc R . . H34C H 0.1523 0.1029 0.5489 0.123 Uiso 1 1 calc R . . C35 C 0.9603(5) 0.3201(5) 0.7175(3) 0.0427(16) Uani 1 1 d . . . H35 H 0.9048 0.3042 0.6946 0.051 Uiso 1 1 calc R . . C36 C 1.0490(6) 0.2698(5) 0.7144(4) 0.053(2) Uani 1 1 d . . . H36 H 1.0549 0.2199 0.6899 0.064 Uiso 1 1 calc R . . C37 C 1.1302(6) 0.2931(6) 0.7479(4) 0.061(2) Uani 1 1 d . . . H37 H 1.1926 0.2595 0.7461 0.073 Uiso 1 1 calc R . . C38 C 1.1200(6) 0.3646(6) 0.7834(4) 0.054(2) Uani 1 1 d . . . H38 H 1.1756 0.3815 0.8059 0.065 Uiso 1 1 calc R . . C39 C 1.0272(5) 0.4126(5) 0.7862(3) 0.0392(15) Uani 1 1 d . . . C40 C 1.0053(5) 0.4871(5) 0.8238(3) 0.0393(15) Uani 1 1 d . . . C41 C 0.9110(5) 0.5304(4) 0.8176(3) 0.0336(14) Uani 1 1 d . . . C42 C 0.8830(5) 0.5965(6) 0.8557(3) 0.0459(17) Uani 1 1 d . . . H42 H 0.8185 0.6270 0.8518 0.055 Uiso 1 1 calc R . . C43 C 0.9490(6) 0.6185(7) 0.8994(4) 0.058(2) Uani 1 1 d . . . C44 C 1.0443(7) 0.5758(7) 0.9029(4) 0.067(2) Uani 1 1 d . . . H44 H 1.0905 0.5916 0.9316 0.080 Uiso 1 1 calc R . . C45 C 1.0727(6) 0.5114(7) 0.8658(4) 0.058(2) Uani 1 1 d . . . H45 H 1.1384 0.4833 0.8686 0.069 Uiso 1 1 calc R . . C46 C 0.9167(8) 0.6864(9) 0.9428(5) 0.092(3) Uani 1 1 d . . . H46A H 0.8996 0.6466 0.9806 0.137 Uiso 1 1 calc R . . H46B H 0.8576 0.7249 0.9273 0.137 Uiso 1 1 calc R . . H46C H 0.9720 0.7316 0.9483 0.137 Uiso 1 1 calc R . . C47 C 0.7708(5) 0.3823(5) 0.8236(3) 0.0357(15) Uani 1 1 d . . . C48 C 0.7446(6) 0.2872(6) 0.9298(3) 0.054(2) Uani 1 1 d . . . C49 C 0.7182(8) 0.3710(8) 0.9632(4) 0.084(3) Uani 1 1 d . . . H49A H 0.7683 0.4239 0.9546 0.126 Uiso 1 1 calc R . . H49B H 0.7180 0.3465 1.0056 0.126 Uiso 1 1 calc R . . H49C H 0.6513 0.3968 0.9512 0.126 Uiso 1 1 calc R . . C50 C 0.8478(7) 0.2455(9) 0.9464(5) 0.087(3) Uani 1 1 d . . . H50A H 0.8693 0.2028 0.9180 0.131 Uiso 1 1 calc R . . H50B H 0.8451 0.2067 0.9859 0.131 Uiso 1 1 calc R . . H50C H 0.8960 0.3000 0.9461 0.131 Uiso 1 1 calc R . . C51 C 0.6642(7) 0.2084(7) 0.9364(4) 0.077(3) Uani 1 1 d . . . H51A H 0.5998 0.2378 0.9219 0.115 Uiso 1 1 calc R . . H51B H 0.6573 0.1803 0.9781 0.115 Uiso 1 1 calc R . . H51C H 0.6830 0.1560 0.9137 0.115 Uiso 1 1 calc R . . C52 C 0.6342(5) 0.5768(7) 0.7946(4) 0.056(2) Uani 1 1 d . . . H52 H 0.6217 0.5149 0.8184 0.067 Uiso 1 1 calc R . . C53 C 0.5711(7) 0.6547(9) 0.7983(5) 0.083(3) Uani 1 1 d . . . H53 H 0.5157 0.6471 0.8249 0.100 Uiso 1 1 calc R . . C54 C 0.5877(7) 0.7434(8) 0.7637(5) 0.084(3) Uani 1 1 d . . . H54 H 0.5444 0.7981 0.7662 0.100 Uiso 1 1 calc R . . C55 C 0.6682(7) 0.7531(7) 0.7249(4) 0.067(2) Uani 1 1 d . . . H55 H 0.6793 0.8142 0.6999 0.081 Uiso 1 1 calc R . . C56 C 0.7327(5) 0.6739(5) 0.7224(3) 0.0437(16) Uani 1 1 d . . . C57 C 0.8187(5) 0.6728(5) 0.6835(3) 0.0388(15) Uani 1 1 d . . . C58 C 0.8420(6) 0.7503(5) 0.6381(3) 0.0491(18) Uani 1 1 d . . . H58 H 0.8029 0.8093 0.6332 0.059 Uiso 1 1 calc R . . C59 C 0.9213(6) 0.7409(5) 0.6009(3) 0.054(2) Uani 1 1 d . . . H59 H 0.9386 0.7947 0.5714 0.065 Uiso 1 1 calc R . . C60 C 0.9771(6) 0.6527(6) 0.6059(3) 0.0490(18) Uani 1 1 d . . . C61 C 0.9534(5) 0.5766(5) 0.6515(3) 0.0397(16) Uani 1 1 d . . . H61 H 0.9925 0.5177 0.6560 0.048 Uiso 1 1 calc R . . C62 C 0.8753(5) 0.5842(5) 0.6901(3) 0.0343(14) Uani 1 1 d . . . C63 C 1.0616(7) 0.6412(8) 0.5634(4) 0.081(3) Uani 1 1 d . . . H63A H 1.1208 0.6781 0.5736 0.121 Uiso 1 1 calc R . . H63B H 1.0401 0.6672 0.5233 0.121 Uiso 1 1 calc R . . H63C H 1.0789 0.5710 0.5657 0.121 Uiso 1 1 calc R . . C64 C 0.7477(5) 0.4304(5) 0.6869(3) 0.0359(15) Uani 1 1 d . . . C65 C 0.6794(6) 0.4138(6) 0.5830(3) 0.054(2) Uani 1 1 d . . . C66 C 0.6175(9) 0.5065(9) 0.5654(5) 0.103(4) Uani 1 1 d . . . H66A H 0.5561 0.5032 0.5893 0.155 Uiso 1 1 calc R . . H66B H 0.5993 0.5119 0.5237 0.155 Uiso 1 1 calc R . . H66C H 0.6571 0.5646 0.5716 0.155 Uiso 1 1 calc R . . C67 C 0.7742(7) 0.4125(10) 0.5463(4) 0.092(4) Uani 1 1 d . . . H67A H 0.8076 0.4771 0.5430 0.138 Uiso 1 1 calc R . . H67B H 0.7565 0.3985 0.5070 0.138 Uiso 1 1 calc R . . H67C H 0.8199 0.3609 0.5653 0.138 Uiso 1 1 calc R . . C68 C 0.6189(7) 0.3200(8) 0.5826(4) 0.079(3) Uani 1 1 d . . . H68A H 0.6622 0.2623 0.5944 0.118 Uiso 1 1 calc R . . H68B H 0.5928 0.3181 0.5429 0.118 Uiso 1 1 calc R . . H68C H 0.5624 0.3187 0.6103 0.118 Uiso 1 1 calc R . . C69 C 0.3483(9) 0.5244(9) 0.7028(5) 0.097(4) Uani 1 1 d . . . H69 H 0.3347 0.5259 0.7454 0.116 Uiso 1 1 calc R . . C70 C 0.8467(9) 0.9764(9) 0.7972(5) 0.097(4) Uani 1 1 d . . . H70 H 0.8328 0.9755 0.7545 0.117 Uiso 1 1 calc R . . C71 C 0.3680(7) 0.4257(7) 0.9463(4) 0.062(2) Uani 1 1 d . . . C72 C 0.8678(7) 0.0731(7) 0.5535(4) 0.062(2) Uani 1 1 d . . . 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 Ir1 0.03193(14) 0.02830(14) 0.03161(15) -0.00858(10) -0.00578(10) 0.00370(10) Ir2 0.03231(14) 0.02838(14) 0.03169(15) -0.00886(10) 0.00180(10) -0.00157(10) Cl1 0.330(8) 0.197(6) 0.212(6) 0.010(5) -0.065(5) -0.154(6) Cl2 0.168(5) 0.206(6) 0.275(7) 0.063(5) -0.074(5) -0.004(4) Cl3 0.306(6) 0.148(4) 0.129(4) 0.027(3) 0.074(4) 0.125(4) Cl4 0.166(4) 0.199(6) 0.267(7) 0.060(5) 0.071(5) 0.010(4) Cl5 0.325(8) 0.198(6) 0.219(7) 0.009(5) 0.061(6) 0.145(6) Cl6 0.298(6) 0.150(4) 0.130(4) 0.027(3) -0.077(4) -0.123(4) S1 0.0528(12) 0.0671(14) 0.0682(15) -0.0288(11) 0.0032(10) -0.0049(10) S2 0.0509(12) 0.0687(15) 0.0684(15) -0.0279(11) -0.0076(10) 0.0060(10) F1 0.120(5) 0.102(5) 0.099(5) -0.058(4) -0.011(4) -0.011(4) F2 0.141(6) 0.135(6) 0.081(5) 0.027(4) -0.029(4) 0.028(5) F3 0.073(4) 0.168(7) 0.073(4) -0.045(4) 0.016(3) 0.003(4) F4 0.137(6) 0.126(6) 0.076(4) 0.029(4) 0.018(4) -0.024(5) F5 0.117(5) 0.095(5) 0.096(5) -0.051(4) 0.008(4) 0.004(4) F6 0.070(4) 0.168(7) 0.069(4) -0.050(4) -0.015(3) -0.002(4) O1 0.096(5) 0.097(5) 0.067(4) -0.009(4) -0.014(4) 0.035(4) O2 0.079(4) 0.080(5) 0.099(5) -0.046(4) 0.007(4) -0.015(4) O3 0.047(3) 0.093(5) 0.090(5) -0.030(4) 0.005(3) -0.001(3) O4 0.047(3) 0.092(5) 0.092(5) -0.029(4) -0.011(3) 0.002(3) O5 0.096(5) 0.097(5) 0.067(4) -0.007(4) 0.005(4) -0.035(4) O6 0.073(4) 0.089(5) 0.102(6) -0.048(4) -0.016(4) 0.018(4) N1 0.034(3) 0.043(3) 0.042(3) -0.015(3) -0.003(2) -0.007(2) N2 0.038(3) 0.029(3) 0.025(3) -0.005(2) -0.004(2) 0.002(2) N3 0.043(3) 0.039(3) 0.038(3) -0.011(3) -0.002(3) 0.008(3) N4 0.040(3) 0.045(3) 0.037(3) -0.006(3) -0.010(3) 0.008(3) N5 0.039(3) 0.025(3) 0.034(3) -0.004(2) 0.004(2) 0.001(2) N6 0.033(3) 0.048(4) 0.046(4) -0.019(3) 0.001(2) 0.006(3) N7 0.047(3) 0.045(3) 0.033(3) -0.007(3) 0.004(3) -0.002(3) N8 0.040(3) 0.047(3) 0.039(3) -0.013(3) -0.003(3) -0.006(3) C1 0.037(4) 0.071(6) 0.072(6) -0.023(4) -0.011(4) 0.000(4) C2 0.062(6) 0.091(8) 0.096(8) -0.032(6) -0.019(5) -0.029(5) C3 0.071(6) 0.079(8) 0.108(9) -0.031(6) -0.003(6) -0.042(6) C4 0.077(6) 0.051(5) 0.083(7) -0.014(5) -0.007(5) -0.021(5) C5 0.045(4) 0.036(4) 0.057(5) -0.018(3) 0.004(3) -0.007(3) C6 0.044(4) 0.034(4) 0.044(4) -0.015(3) 0.004(3) 0.002(3) C7 0.066(5) 0.027(3) 0.054(5) -0.004(3) 0.012(4) 0.000(3) C8 0.061(5) 0.046(4) 0.048(5) 0.007(4) 0.003(4) 0.013(4) C9 0.055(5) 0.054(5) 0.040(4) 0.007(3) -0.011(3) 0.010(4) C10 0.039(4) 0.043(4) 0.042(4) 0.000(3) -0.010(3) 0.001(3) C11 0.040(3) 0.030(3) 0.032(4) -0.008(3) 0.002(3) 0.002(3) C12 0.077(6) 0.092(7) 0.071(7) 0.026(5) -0.037(5) 0.004(5) C13 0.036(3) 0.033(3) 0.038(4) -0.007(3) -0.010(3) 0.004(3) C14 0.054(5) 0.079(6) 0.031(4) -0.013(4) 0.006(3) 0.002(4) C15 0.095(7) 0.097(8) 0.064(6) -0.041(6) 0.012(5) 0.031(6) C16 0.093(8) 0.145(11) 0.048(6) -0.021(6) -0.016(5) 0.014(7) C17 0.141(10) 0.107(9) 0.071(7) -0.006(6) 0.039(7) -0.040(8) C18 0.050(4) 0.038(4) 0.047(4) -0.009(3) -0.004(3) 0.005(3) C19 0.059(5) 0.034(4) 0.065(5) -0.016(4) -0.013(4) -0.011(3) C20 0.060(5) 0.053(5) 0.063(6) -0.008(4) 0.001(4) -0.018(4) C21 0.055(5) 0.058(5) 0.051(5) -0.009(4) 0.005(4) -0.013(4) C22 0.035(3) 0.038(4) 0.037(4) 0.003(3) -0.001(3) -0.004(3) C23 0.042(4) 0.036(4) 0.036(4) -0.003(3) 0.000(3) 0.003(3) C24 0.046(4) 0.084(6) 0.038(4) -0.016(4) 0.004(3) 0.001(4) C25 0.065(5) 0.082(7) 0.057(6) -0.034(5) 0.009(4) 0.009(5) C26 0.067(5) 0.063(5) 0.052(5) -0.033(4) -0.001(4) 0.007(4) C27 0.045(4) 0.047(4) 0.047(4) -0.019(3) -0.011(3) 0.013(3) C28 0.045(4) 0.038(4) 0.028(3) -0.008(3) -0.008(3) 0.009(3) C29 0.113(8) 0.104(9) 0.076(7) -0.063(6) -0.011(6) 0.011(7) C30 0.031(3) 0.041(4) 0.042(4) -0.010(3) -0.008(3) 0.009(3) C31 0.056(5) 0.064(5) 0.040(4) 0.006(4) -0.010(3) 0.001(4) C32 0.071(6) 0.121(9) 0.066(7) 0.021(6) -0.008(5) -0.011(6) C33 0.082(6) 0.063(6) 0.069(6) 0.007(5) -0.021(5) 0.021(5) C34 0.102(8) 0.101(8) 0.045(5) -0.019(5) -0.022(5) 0.000(6) C35 0.051(4) 0.037(4) 0.042(4) -0.012(3) 0.003(3) -0.001(3) C36 0.066(5) 0.032(4) 0.066(5) -0.018(4) 0.008(4) 0.009(4) C37 0.058(5) 0.052(5) 0.072(6) -0.010(4) -0.005(4) 0.020(4) C38 0.050(4) 0.054(5) 0.060(5) -0.012(4) -0.006(4) 0.012(4) C39 0.040(4) 0.043(4) 0.033(4) 0.000(3) -0.005(3) 0.005(3) C40 0.042(4) 0.045(4) 0.032(4) -0.009(3) -0.005(3) -0.006(3) C41 0.038(3) 0.023(3) 0.041(4) -0.011(3) 0.002(3) -0.005(3) C42 0.048(4) 0.057(5) 0.036(4) -0.019(3) 0.007(3) -0.003(3) C43 0.064(5) 0.067(6) 0.051(5) -0.033(4) -0.002(4) -0.011(4) C44 0.069(6) 0.086(7) 0.052(5) -0.030(5) -0.019(4) -0.007(5) C45 0.045(4) 0.080(6) 0.051(5) -0.021(4) -0.011(4) 0.002(4) C46 0.108(8) 0.106(9) 0.075(7) -0.060(6) 0.006(6) -0.009(7) C47 0.032(3) 0.040(4) 0.037(4) -0.016(3) 0.007(3) -0.010(3) C48 0.058(5) 0.064(5) 0.036(4) 0.003(4) 0.006(3) 0.006(4) C49 0.112(8) 0.101(8) 0.040(5) -0.014(5) 0.023(5) -0.012(6) C50 0.078(7) 0.104(8) 0.071(7) 0.017(6) 0.001(5) 0.015(6) C51 0.095(7) 0.073(6) 0.055(6) 0.013(5) 0.016(5) -0.026(5) C52 0.040(4) 0.066(5) 0.063(5) -0.014(4) 0.011(4) 0.007(4) C53 0.068(6) 0.094(8) 0.094(8) -0.032(6) 0.017(5) 0.028(6) C54 0.068(6) 0.076(7) 0.114(9) -0.036(7) -0.001(6) 0.040(6) C55 0.071(6) 0.056(5) 0.077(7) -0.015(5) -0.002(5) 0.028(4) C56 0.050(4) 0.036(4) 0.048(4) -0.015(3) -0.003(3) 0.004(3) C57 0.042(4) 0.031(3) 0.045(4) -0.012(3) -0.009(3) 0.001(3) C58 0.064(5) 0.031(4) 0.051(5) 0.000(3) -0.016(4) 0.000(3) C59 0.066(5) 0.039(4) 0.052(5) 0.010(3) -0.012(4) -0.016(4) C60 0.059(5) 0.045(4) 0.039(4) 0.008(3) 0.003(3) -0.006(4) C61 0.041(4) 0.033(4) 0.045(4) -0.003(3) 0.003(3) -0.003(3) C62 0.040(4) 0.029(3) 0.035(4) -0.009(3) -0.005(3) 0.000(3) C63 0.081(6) 0.086(7) 0.065(6) 0.024(5) 0.031(5) -0.003(5) C64 0.029(3) 0.028(3) 0.053(5) -0.010(3) 0.005(3) -0.001(3) C65 0.056(5) 0.071(6) 0.035(4) -0.012(4) -0.009(3) 0.001(4) C66 0.123(10) 0.103(9) 0.081(8) -0.004(6) -0.038(7) 0.039(8) C67 0.078(7) 0.156(11) 0.044(5) -0.019(6) 0.013(5) -0.008(7) C68 0.078(6) 0.102(8) 0.064(6) -0.041(6) -0.019(5) -0.017(6) C69 0.129(10) 0.092(9) 0.070(7) -0.014(6) -0.016(6) 0.015(7) C70 0.131(10) 0.085(8) 0.073(8) -0.004(6) 0.002(7) -0.006(7) C71 0.070(6) 0.063(6) 0.051(5) -0.005(4) -0.011(4) -0.001(5) C72 0.060(5) 0.062(6) 0.064(6) -0.008(4) 0.006(4) 0.002(4) 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Ir1 C13 101.9(3) . . ? C30 Ir1 C11 174.5(3) . . ? C13 Ir1 C11 83.2(2) . . ? C30 Ir1 N1 97.4(2) . . ? C13 Ir1 N1 90.4(2) . . ? C11 Ir1 N1 80.2(2) . . ? C30 Ir1 N2 89.9(2) . . ? C13 Ir1 N2 96.9(2) . . ? C11 Ir1 N2 91.8(2) . . ? N1 Ir1 N2 168.5(2) . . ? C30 Ir1 C28 84.5(3) . . ? C13 Ir1 C28 172.7(2) . . ? C11 Ir1 C28 90.6(2) . . ? N1 Ir1 C28 92.3(2) . . ? N2 Ir1 C28 79.5(2) . . ? C47 Ir2 C64 102.0(3) . . ? C47 Ir2 C62 174.2(2) . . ? C64 Ir2 C62 83.2(3) . . ? C47 Ir2 N5 89.9(2) . . ? C64 Ir2 N5 97.1(2) . . ? C62 Ir2 N5 92.1(2) . . ? C47 Ir2 N6 97.6(2) . . ? C64 Ir2 N6 90.2(2) . . ? C62 Ir2 N6 79.6(2) . . ? N5 Ir2 N6 168.2(2) . . ? C47 Ir2 C41 84.1(2) . . ? C64 Ir2 C41 173.0(2) . . ? C62 Ir2 C41 90.9(2) . . ? N5 Ir2 C41 79.3(2) . . ? N6 Ir2 C41 92.4(2) . . ? O2 S1 O3 117.8(4) . . ? O2 S1 O1 111.3(5) . . ? O3 S1 O1 114.3(4) . . ? O2 S1 C71 105.0(4) . . ? O3 S1 C71 103.4(4) . . ? O1 S1 C71 103.1(4) . . ? O6 S2 O4 117.4(4) . . ? O6 S2 O5 111.3(5) . . ? O4 S2 O5 114.9(4) . . ? O6 S2 C72 105.0(4) . . ? O4 S2 C72 103.8(4) . . ? O5 S2 C72 102.3(4) . . ? C5 N1 C1 119.7(6) . . ? C5 N1 Ir1 116.0(4) . . ? C1 N1 Ir1 124.2(5) . . ? C18 N2 C22 118.6(6) . . ? C18 N2 Ir1 125.2(4) . . ? C22 N2 Ir1 116.1(4) . . ? C13 N3 C14 169.0(7) . . ? C30 N4 C31 165.1(7) . . ? C35 N5 C39 119.1(6) . . ? C35 N5 Ir2 125.1(5) . . ? C39 N5 Ir2 115.8(4) . . ? C52 N6 C56 120.4(6) . . ? C52 N6 Ir2 123.6(5) . . ? C56 N6 Ir2 115.8(4) . . ? C47 N7 C48 164.9(7) . . ? C64 N8 C65 168.7(7) . . ? C2 C1 N1 122.1(9) . . ? C1 C2 C3 118.3(9) . . ? C2 C3 C4 121.1(8) . . ? C3 C4 C5 118.8(9) . . ? N1 C5 C4 120.0(7) . . ? N1 C5 C6 114.3(6) . . ? C4 C5 C6 125.8(7) . . ? C7 C6 C11 119.6(7) . . ? C7 C6 C5 124.1(7) . . ? C11 C6 C5 116.3(6) . . ? C8 C7 C6 120.7(7) . . ? C7 C8 C9 120.6(7) . . ? C8 C9 C10 118.4(7) . . ? C8 C9 C12 120.5(7) . . ? C10 C9 C12 121.1(7) . . ? C11 C10 C9 122.9(7) . . ? C10 C11 C6 117.7(6) . . ? C10 C11 Ir1 128.9(5) . . ? C6 C11 Ir1 113.1(5) . . ? N3 C13 Ir1 170.0(6) . . ? N3 C14 C15 108.2(7) . . ? N3 C14 C17 106.2(7) . . ? C15 C14 C17 112.5(8) . . ? N3 C14 C16 106.3(6) . . ? C15 C14 C16 110.9(8) . . ? C17 C14 C16 112.4(9) . . ? N2 C18 C19 122.7(7) . . ? C18 C19 C20 118.0(7) . . ? C21 C20 C19 120.4(8) . . ? C20 C21 C22 120.3(8) . . ? N2 C22 C21 120.0(7) . . ? N2 C22 C23 114.4(6) . . ? C21 C22 C23 125.6(6) . . ? C24 C23 C28 121.1(7) . . ? C24 C23 C22 123.1(6) . . ? C28 C23 C22 115.8(6) . . ? C25 C24 C23 120.0(7) . . ? C24 C25 C26 121.1(7) . . ? C25 C26 C27 118.2(7) . . ? C25 C26 C29 120.8(8) . . ? C27 C26 C29 121.0(8) . . ? C28 C27 C26 122.4(7) . . ? C27 C28 C23 117.2(6) . . ? C27 C28 Ir1 128.5(5) . . ? C23 C28 Ir1 113.9(5) . . ? N4 C30 Ir1 170.4(6) . . ? N4 C31 C34 106.9(7) . . ? N4 C31 C33 110.2(7) . . ? C34 C31 C33 110.4(7) . . ? N4 C31 C32 106.6(6) . . ? C34 C31 C32 111.0(8) . . ? C33 C31 C32 111.6(8) . . ? N5 C35 C36 122.5(7) . . ? C35 C36 C37 118.7(7) . . ? C38 C37 C36 119.9(7) . . ? C37 C38 C39 119.6(8) . . ? N5 C39 C38 120.1(7) . . ? N5 C39 C40 114.8(6) . . ? C38 C39 C40 125.1(7) . . ? C41 C40 C45 120.7(7) . . ? C41 C40 C39 116.4(6) . . ? C45 C40 C39 122.9(7) . . ? C40 C41 C42 118.8(6) . . ? C40 C41 Ir2 113.6(4) . . ? C42 C41 Ir2 127.4(5) . . ? C41 C42 C43 120.8(7) . . ? C44 C43 C42 118.6(7) . . ? C44 C43 C46 120.6(8) . . ? C42 C43 C46 120.8(8) . . ? C45 C44 C43 121.2(7) . . ? C44 C45 C40 119.9(7) . . ? N7 C47 Ir2 171.0(6) . . ? N7 C48 C50 106.0(6) . . ? N7 C48 C51 109.3(7) . . ? C50 C48 C51 112.4(8) . . ? N7 C48 C49 105.7(7) . . ? C50 C48 C49 111.4(8) . . ? C51 C48 C49 111.7(7) . . ? N6 C52 C53 121.1(9) . . ? C54 C53 C52 119.9(9) . . ? C53 C54 C55 119.4(8) . . ? C54 C55 C56 120.1(9) . . ? N6 C56 C55 119.1(7) . . ? N6 C56 C57 114.7(6) . . ? C55 C56 C57 126.2(7) . . ? C58 C57 C62 120.1(7) . . ? C58 C57 C56 123.7(6) . . ? C62 C57 C56 116.1(6) . . ? C59 C58 C57 120.0(7) . . ? C58 C59 C60 120.7(7) . . ? C61 C60 C59 118.4(7) . . ? C61 C60 C63 121.0(7) . . ? C59 C60 C63 120.6(7) . . ? C62 C61 C60 122.3(7) . . ? C61 C62 C57 118.4(6) . . ? C61 C62 Ir2 128.0(5) . . ? C57 C62 Ir2 113.5(5) . . ? N8 C64 Ir2 170.0(6) . . ? N8 C65 C66 107.0(7) . . ? N8 C65 C67 106.0(7) . . ? C66 C65 C67 112.4(9) . . ? N8 C65 C68 107.5(6) . . ? C66 C65 C68 112.7(8) . . ? C67 C65 C68 110.9(8) . . ? Cl1 C69 Cl3 113.4(8) . . ? Cl1 C69 Cl2 109.2(7) . . ? Cl3 C69 Cl2 110.2(8) . . ? Cl4 C70 Cl6 110.5(8) . . ? Cl4 C70 Cl5 109.2(7) . . ? Cl6 C70 Cl5 112.1(8) . . ? F2 C71 F3 109.0(8) . . ? F2 C71 F1 104.8(8) . . ? F3 C71 F1 107.3(8) . . ? F2 C71 S1 113.0(7) . . ? F3 C71 S1 112.6(6) . . ? F1 C71 S1 109.7(6) . . ? F4 C72 F6 108.7(8) . . ? F4 C72 F5 105.0(7) . . ? F6 C72 F5 108.8(8) . . ? F4 C72 S2 111.5(7) . . ? F6 C72 S2 112.6(6) . . ? F5 C72 S2 109.9(6) . . ? 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 Ir1 C30 2.009(7) . ? Ir1 C13 2.013(7) . ? Ir1 C11 2.041(6) . ? Ir1 N1 2.062(5) . ? Ir1 N2 2.062(5) . ? Ir1 C28 2.062(6) . ? Ir2 C47 1.998(7) . ? Ir2 C64 2.027(7) . ? Ir2 C62 2.055(6) . ? Ir2 N5 2.062(5) . ? Ir2 N6 2.065(5) . ? Ir2 C41 2.085(6) . ? Cl1 C69 1.691(13) . ? Cl2 C69 1.696(12) . ? Cl3 C69 1.692(12) . ? Cl4 C70 1.674(12) . ? Cl5 C70 1.707(13) . ? Cl6 C70 1.691(13) . ? S1 O2 1.411(7) . ? S1 O3 1.420(6) . ? S1 O1 1.476(7) . ? S1 C71 1.797(9) . ? S2 O6 1.411(7) . ? S2 O4 1.422(6) . ? S2 O5 1.458(7) . ? S2 C72 1.810(10) . ? F1 C71 1.344(10) . ? F2 C71 1.289(10) . ? F3 C71 1.316(10) . ? F4 C72 1.299(10) . ? F5 C72 1.329(10) . ? F6 C72 1.308(10) . ? N1 C5 1.365(9) . ? N1 C1 1.368(9) . ? N2 C18 1.359(9) . ? N2 C22 1.361(8) . ? N3 C13 1.142(8) . ? N3 C14 1.459(9) . ? N4 C30 1.151(8) . ? N4 C31 1.460(9) . ? N5 C35 1.350(8) . ? N5 C39 1.366(8) . ? N6 C52 1.356(9) . ? N6 C56 1.360(9) . ? N7 C47 1.165(8) . ? N7 C48 1.468(9) . ? N8 C64 1.141(8) . ? N8 C65 1.468(9) . ? C1 C2 1.348(12) . ? C2 C3 1.380(15) . ? C3 C4 1.382(13) . ? C4 C5 1.384(10) . ? C5 C6 1.446(10) . ? C6 C7 1.404(10) . ? C6 C11 1.431(9) . ? C7 C8 1.387(11) . ? C8 C9 1.392(11) . ? C9 C10 1.404(9) . ? C9 C12 1.506(11) . ? C10 C11 1.382(9) . ? C14 C15 1.507(12) . ? C14 C17 1.512(13) . ? C14 C16 1.531(12) . ? C18 C19 1.376(10) . ? C19 C20 1.385(11) . ? C20 C21 1.345(11) . ? C21 C22 1.404(9) . ? C22 C23 1.463(10) . ? C23 C24 1.394(9) . ? C23 C28 1.399(9) . ? C24 C25 1.370(11) . ? C25 C26 1.389(11) . ? C26 C27 1.399(10) . ? C26 C29 1.519(11) . ? C27 C28 1.396(9) . ? C31 C34 1.513(13) . ? C31 C33 1.518(11) . ? C31 C32 1.519(11) . ? C35 C36 1.369(9) . ? C36 C37 1.388(12) . ? C37 C38 1.369(11) . ? C38 C39 1.400(9) . ? C39 C40 1.459(10) . ? C40 C41 1.381(9) . ? C40 C45 1.394(10) . ? C41 C42 1.398(9) . ? C42 C43 1.400(10) . ? C43 C44 1.389(11) . ? C43 C46 1.521(11) . ? C44 C45 1.366(11) . ? C48 C50 1.510(11) . ? C48 C51 1.506(11) . ? C48 C49 1.512(13) . ? C52 C53 1.365(12) . ? C53 C54 1.364(14) . ? C54 C55 1.384(12) . ? C55 C56 1.387(10) . ? C56 C57 1.448(9) . ? C57 C58 1.405(10) . ? C57 C62 1.413(9) . ? C58 C59 1.373(11) . ? C59 C60 1.404(11) . ? C60 C61 1.396(9) . ? C60 C63 1.508(11) . ? C61 C62 1.377(9) . ? C65 C66 1.512(13) . ? C65 C67 1.514(11) . ? C65 C68 1.514(12) . ?