# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yaofeng Chen' _publ_contact_author_email yaofchen@mail.sioc.ac.cn _publ_author_name 'Yaofeng Chen' data_cd201301 _database_code_depnum_ccdc_archive 'CCDC 851600' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H61 Cu I N6 Sc' _chemical_formula_weight 861.35 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 11.2772(9) _cell_length_b 36.002(3) _cell_length_c 14.1324(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.966(2) _cell_angle_gamma 90.00 _cell_volume 5543.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5590 _cell_measurement_theta_min 4.526 _cell_measurement_theta_max 43.979 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.311 _exptl_crystal_size_mid 0.248 _exptl_crystal_size_min 0.167 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30198 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10864 _reflns_number_gt 5683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10864 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # 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 0.020 0.000 0.500 861 288 ' ' 2 -0.079 0.500 0.000 861 288 ' ' _platon_squeeze_details ; ; 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 Sc1 Sc 0.67785(6) 0.161168(18) 0.06295(5) 0.04438(19) Uani 1 1 d . . . Cu1 Cu 0.63275(4) 0.214610(14) -0.09835(3) 0.06187(16) Uani 1 1 d . . . I1 I 0.71934(3) 0.247514(9) -0.21306(2) 0.08032(13) Uani 1 1 d . . . N1 N 0.6535(3) 0.10254(7) 0.0234(2) 0.0488(8) Uani 1 1 d . . . N2 N 0.8184(3) 0.15839(8) -0.0185(2) 0.0544(8) Uani 1 1 d . . . N3 N 0.8470(3) 0.19566(9) 0.1566(2) 0.0576(8) Uani 1 1 d . . . N4 N 0.6275(3) 0.15478(8) 0.2081(2) 0.0546(8) Uani 1 1 d . . . N5 N 0.5716(4) 0.16691(10) 0.4884(2) 0.0741(10) Uani 1 1 d . . . N6 N 0.5510(3) 0.19291(8) -0.01175(19) 0.0468(7) Uani 1 1 d . . . C1 C 0.5879(4) 0.05662(11) -0.1107(3) 0.0801(14) Uani 1 1 d . . . H1A H 0.6036 0.0377 -0.0612 0.120 Uiso 1 1 calc R . . H1B H 0.6180 0.0486 -0.1650 0.120 Uiso 1 1 calc R . . H1C H 0.5011 0.0610 -0.1327 0.120 Uiso 1 1 calc R . . C2 C 0.6523(4) 0.09209(10) -0.0688(3) 0.0573(10) Uani 1 1 d . . . C3 C 0.7101(4) 0.11192(11) -0.1275(3) 0.0619(11) Uani 1 1 d . . . H3 H 0.6852 0.1064 -0.1940 0.074 Uiso 1 1 calc R . . C4 C 0.8021(4) 0.13959(12) -0.1005(3) 0.0598(11) Uani 1 1 d . . . C5 C 0.8830(4) 0.14543(12) -0.1688(3) 0.0862(15) Uani 1 1 d . . . H5A H 0.8724 0.1703 -0.1942 0.129 Uiso 1 1 calc R . . H5B H 0.8609 0.1280 -0.2220 0.129 Uiso 1 1 calc R . . H5C H 0.9672 0.1417 -0.1339 0.129 Uiso 1 1 calc R . . C6 C 0.9269(4) 0.18287(13) 0.0114(3) 0.0841(14) Uani 1 1 d . . . H6A H 0.9425 0.1949 -0.0457 0.101 Uiso 1 1 calc R . . H6B H 0.9987 0.1684 0.0432 0.101 Uiso 1 1 calc R . . C7 C 0.9016(4) 0.21186(12) 0.0815(3) 0.0779(13) Uani 1 1 d . . . H7A H 0.9779 0.2242 0.1137 0.093 Uiso 1 1 calc R . . H7B H 0.8462 0.2304 0.0447 0.093 Uiso 1 1 calc R . . C11 C 0.6432(4) 0.07370(10) 0.0923(3) 0.0576(11) Uani 1 1 d . . . C12 C 0.7530(5) 0.05605(11) 0.1431(3) 0.0686(12) Uani 1 1 d . . . C13 C 0.7446(6) 0.02981(13) 0.2148(3) 0.0891(16) Uani 1 1 d . . . H13 H 0.8152 0.0176 0.2494 0.107 Uiso 1 1 calc R . . C14 C 0.6342(7) 0.02173(14) 0.2349(4) 0.1010(19) Uani 1 1 d . . . H14 H 0.6310 0.0045 0.2832 0.121 Uiso 1 1 calc R . . C15 C 0.5321(5) 0.03863(13) 0.1850(3) 0.0838(15) Uani 1 1 d . . . H15 H 0.4587 0.0332 0.2003 0.101 Uiso 1 1 calc R . . C16 C 0.5310(5) 0.06431(11) 0.1104(3) 0.0649(12) Uani 1 1 d . . . C17 C 0.4080(4) 0.08025(12) 0.0520(3) 0.0740(13) Uani 1 1 d . . . H17 H 0.4240 0.0964 0.0008 0.089 Uiso 1 1 calc R . . C18 C 0.3205(5) 0.04921(13) 0.0015(4) 0.1030(17) Uani 1 1 d . . . H18A H 0.2951 0.0349 0.0501 0.155 Uiso 1 1 calc R . . H18B H 0.3620 0.0334 -0.0342 0.155 Uiso 1 1 calc R . . H18C H 0.2497 0.0600 -0.0427 0.155 Uiso 1 1 calc R . . C19 C 0.3456(5) 0.10367(14) 0.1153(4) 0.1118(18) Uani 1 1 d . . . H19A H 0.3261 0.0883 0.1646 0.168 Uiso 1 1 calc R . . H19B H 0.2716 0.1143 0.0750 0.168 Uiso 1 1 calc R . . H19C H 0.4000 0.1232 0.1461 0.168 Uiso 1 1 calc R . . C20 C 0.8742(5) 0.06425(12) 0.1230(3) 0.0808(14) Uani 1 1 d . . . H20 H 0.8664 0.0882 0.0892 0.097 Uiso 1 1 calc R . . C21 C 0.9823(5) 0.06793(14) 0.2177(4) 0.1159(19) Uani 1 1 d . . . H21A H 0.9628 0.0868 0.2594 0.174 Uiso 1 1 calc R . . H21B H 1.0560 0.0747 0.1999 0.174 Uiso 1 1 calc R . . H21C H 0.9943 0.0446 0.2518 0.174 Uiso 1 1 calc R . . C22 C 0.9102(5) 0.03549(15) 0.0551(4) 0.121(2) Uani 1 1 d . . . H22A H 0.9210 0.0117 0.0867 0.182 Uiso 1 1 calc R . . H22B H 0.9856 0.0429 0.0409 0.182 Uiso 1 1 calc R . . H22C H 0.8466 0.0339 -0.0048 0.182 Uiso 1 1 calc R . . C31 C 0.8194(4) 0.22618(13) 0.2187(3) 0.0902(15) Uani 1 1 d . . . H31A H 0.7827 0.2160 0.2672 0.135 Uiso 1 1 calc R . . H31B H 0.7636 0.2435 0.1785 0.135 Uiso 1 1 calc R . . H31C H 0.8941 0.2388 0.2506 0.135 Uiso 1 1 calc R . . C32 C 0.9369(4) 0.17051(12) 0.2208(3) 0.0820(14) Uani 1 1 d . . . H32A H 0.9480 0.1488 0.1846 0.123 Uiso 1 1 calc R . . H32B H 0.9069 0.1633 0.2758 0.123 Uiso 1 1 calc R . . H32C H 1.0139 0.1831 0.2437 0.123 Uiso 1 1 calc R . . C33 C 0.6830(4) 0.13336(11) 0.2841(3) 0.0644(12) Uani 1 1 d . . . H33 H 0.7370 0.1153 0.2733 0.077 Uiso 1 1 calc R . . C34 C 0.6664(4) 0.13594(11) 0.3763(3) 0.0643(11) Uani 1 1 d . . . H34 H 0.7085 0.1199 0.4251 0.077 Uiso 1 1 calc R . . C35 C 0.5879(4) 0.16203(11) 0.3977(3) 0.0604(11) Uani 1 1 d . . . C36 C 0.5223(4) 0.18328(11) 0.3166(3) 0.0655(12) Uani 1 1 d . . . H36 H 0.4633 0.2002 0.3241 0.079 Uiso 1 1 calc R . . C37 C 0.5459(4) 0.17882(11) 0.2275(3) 0.0585(11) Uani 1 1 d . . . H37 H 0.5021 0.1935 0.1762 0.070 Uiso 1 1 calc R . . C38 C 0.6454(5) 0.14608(14) 0.5715(3) 0.1007(17) Uani 1 1 d . . . H38A H 0.6181 0.1207 0.5675 0.151 Uiso 1 1 calc R . . H38B H 0.6365 0.1569 0.6314 0.151 Uiso 1 1 calc R . . H38C H 0.7301 0.1469 0.5704 0.151 Uiso 1 1 calc R . . C39 C 0.4862(5) 0.19357(13) 0.5110(3) 0.0935(16) Uani 1 1 d . . . H39A H 0.4064 0.1899 0.4674 0.140 Uiso 1 1 calc R . . H39B H 0.5141 0.2183 0.5033 0.140 Uiso 1 1 calc R . . H39C H 0.4818 0.1901 0.5774 0.140 Uiso 1 1 calc R . . C40 C 0.4304(3) 0.20725(10) -0.0364(2) 0.0428(9) Uani 1 1 d . . . C41 C 0.3348(4) 0.18676(10) -0.1001(3) 0.0525(10) Uani 1 1 d . . . C42 C 0.2138(4) 0.19978(13) -0.1169(3) 0.0727(12) Uani 1 1 d . . . H42 H 0.1505 0.1862 -0.1574 0.087 Uiso 1 1 calc R . . C43 C 0.1861(4) 0.23208(14) -0.0752(4) 0.0797(14) Uani 1 1 d . . . H43 H 0.1050 0.2398 -0.0858 0.096 Uiso 1 1 calc R . . C44 C 0.2789(4) 0.25266(12) -0.0184(3) 0.0711(12) Uani 1 1 d . . . H44 H 0.2605 0.2751 0.0073 0.085 Uiso 1 1 calc R . . C45 C 0.4017(4) 0.24092(11) 0.0023(3) 0.0548(10) Uani 1 1 d . . . C46 C 0.5010(4) 0.26629(11) 0.0603(3) 0.0588(11) Uani 1 1 d . . . H46 H 0.5758 0.2515 0.0833 0.071 Uiso 1 1 calc R . . C47 C 0.5285(5) 0.29682(13) -0.0037(4) 0.1034(17) Uani 1 1 d . . . H47A H 0.5389 0.2864 -0.0635 0.155 Uiso 1 1 calc R . . H47B H 0.6024 0.3094 0.0300 0.155 Uiso 1 1 calc R . . H47C H 0.4616 0.3142 -0.0184 0.155 Uiso 1 1 calc R . . C48 C 0.4704(5) 0.28347(13) 0.1502(3) 0.0974(16) Uani 1 1 d . . . H48A H 0.5401 0.2970 0.1875 0.146 Uiso 1 1 calc R . . H48B H 0.4500 0.2641 0.1900 0.146 Uiso 1 1 calc R . . H48C H 0.4018 0.3000 0.1294 0.146 Uiso 1 1 calc R . . C49 C 0.3627(4) 0.15322(11) -0.1544(3) 0.0650(11) Uani 1 1 d . . . H49 H 0.4339 0.1407 -0.1118 0.078 Uiso 1 1 calc R . . C50 C 0.3981(5) 0.16520(13) -0.2481(3) 0.0872(15) Uani 1 1 d . . . H50A H 0.3280 0.1759 -0.2934 0.131 Uiso 1 1 calc R . . H50B H 0.4254 0.1439 -0.2776 0.131 Uiso 1 1 calc R . . H50C H 0.4629 0.1832 -0.2318 0.131 Uiso 1 1 calc R . . C51 C 0.2590(4) 0.12510(12) -0.1814(3) 0.0885(15) Uani 1 1 d . . . H51A H 0.2333 0.1185 -0.1239 0.133 Uiso 1 1 calc R . . H51B H 0.2871 0.1033 -0.2081 0.133 Uiso 1 1 calc R . . H51C H 0.1912 0.1357 -0.2292 0.133 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0453(4) 0.0436(4) 0.0437(4) -0.0003(3) 0.0106(3) -0.0019(3) Cu1 0.0543(3) 0.0745(4) 0.0593(3) 0.0115(3) 0.0191(3) 0.0004(3) I1 0.0680(2) 0.0992(3) 0.0787(2) 0.03176(18) 0.02774(16) 0.00361(17) N1 0.058(2) 0.0434(19) 0.0468(18) -0.0005(15) 0.0177(16) -0.0029(15) N2 0.046(2) 0.060(2) 0.060(2) 0.0022(17) 0.0191(17) -0.0042(17) N3 0.051(2) 0.055(2) 0.060(2) -0.0010(18) 0.0020(17) -0.0072(17) N4 0.071(2) 0.050(2) 0.0458(19) 0.0009(16) 0.0196(18) 0.0037(18) N5 0.106(3) 0.072(3) 0.051(2) -0.0013(18) 0.031(2) -0.003(2) N6 0.044(2) 0.0501(19) 0.0473(17) -0.0010(14) 0.0131(15) 0.0025(15) C1 0.105(4) 0.069(3) 0.067(3) -0.023(2) 0.024(3) -0.024(3) C2 0.065(3) 0.047(3) 0.058(3) -0.005(2) 0.013(2) 0.003(2) C3 0.079(3) 0.061(3) 0.046(2) -0.003(2) 0.018(2) 0.003(2) C4 0.065(3) 0.061(3) 0.061(3) 0.012(2) 0.029(2) 0.015(2) C5 0.082(4) 0.104(4) 0.086(3) 0.009(3) 0.046(3) 0.008(3) C6 0.071(3) 0.103(4) 0.080(3) 0.007(3) 0.024(3) -0.020(3) C7 0.063(3) 0.075(3) 0.083(3) 0.012(3) -0.004(3) -0.029(2) C11 0.079(3) 0.040(2) 0.055(2) -0.0067(19) 0.018(2) -0.005(2) C12 0.087(4) 0.050(3) 0.067(3) -0.003(2) 0.016(3) 0.005(3) C13 0.120(5) 0.056(3) 0.077(3) 0.012(3) 0.000(3) 0.013(3) C14 0.153(6) 0.068(4) 0.075(3) 0.026(3) 0.017(4) -0.011(4) C15 0.111(5) 0.066(3) 0.078(3) 0.009(3) 0.031(3) -0.019(3) C16 0.082(4) 0.050(3) 0.064(3) 0.000(2) 0.021(3) -0.012(2) C17 0.077(3) 0.066(3) 0.083(3) 0.002(3) 0.028(3) -0.018(3) C18 0.108(4) 0.092(4) 0.104(4) 0.002(3) 0.019(3) -0.037(3) C19 0.088(4) 0.114(4) 0.133(5) -0.019(4) 0.029(4) -0.008(3) C20 0.090(4) 0.058(3) 0.086(3) 0.002(3) 0.006(3) 0.005(3) C21 0.108(5) 0.096(4) 0.127(5) 0.000(3) -0.001(4) 0.027(3) C22 0.100(5) 0.125(5) 0.142(5) -0.034(4) 0.036(4) 0.015(4) C31 0.078(4) 0.082(4) 0.097(4) -0.021(3) -0.003(3) -0.002(3) C32 0.077(3) 0.077(3) 0.080(3) 0.010(3) -0.002(3) -0.006(3) C33 0.080(3) 0.057(3) 0.059(3) -0.006(2) 0.022(3) -0.002(2) C34 0.080(3) 0.059(3) 0.048(2) 0.006(2) 0.008(2) 0.000(2) C35 0.078(3) 0.057(3) 0.051(3) -0.002(2) 0.025(2) -0.009(2) C36 0.079(3) 0.060(3) 0.065(3) -0.004(2) 0.031(3) 0.004(2) C37 0.068(3) 0.052(3) 0.057(3) 0.000(2) 0.018(2) -0.005(2) C38 0.123(5) 0.129(5) 0.051(3) 0.003(3) 0.026(3) -0.005(4) C39 0.124(5) 0.095(4) 0.075(3) -0.013(3) 0.052(3) -0.003(3) C40 0.049(2) 0.048(2) 0.0330(18) 0.0100(17) 0.0128(18) 0.0003(19) C41 0.047(3) 0.057(3) 0.052(2) 0.012(2) 0.011(2) 0.001(2) C42 0.054(3) 0.080(4) 0.075(3) 0.013(3) 0.001(2) -0.013(3) C43 0.047(3) 0.086(4) 0.106(4) 0.002(3) 0.018(3) 0.010(3) C44 0.058(3) 0.074(3) 0.085(3) 0.003(3) 0.025(3) 0.022(3) C45 0.058(3) 0.065(3) 0.044(2) 0.010(2) 0.017(2) 0.003(2) C46 0.056(3) 0.060(3) 0.056(2) -0.006(2) 0.006(2) 0.008(2) C47 0.130(5) 0.091(4) 0.093(4) -0.006(3) 0.036(4) -0.033(3) C48 0.122(5) 0.108(4) 0.064(3) -0.016(3) 0.026(3) 0.007(3) C49 0.066(3) 0.056(3) 0.065(3) -0.001(2) 0.003(2) -0.012(2) C50 0.107(4) 0.097(4) 0.058(3) -0.011(2) 0.023(3) -0.014(3) C51 0.090(4) 0.077(3) 0.087(3) -0.007(3) 0.000(3) -0.020(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 Sc1 N6 1.920(3) . ? Sc1 N1 2.183(3) . ? Sc1 N2 2.188(3) . ? Sc1 N4 2.277(3) . ? Sc1 N3 2.372(3) . ? Sc1 Cu1 2.9255(8) . ? Cu1 N6 1.882(3) . ? Cu1 I1 2.4089(5) . ? N1 C2 1.353(4) . ? N1 C11 1.449(4) . ? N2 C4 1.313(5) . ? N2 C6 1.478(5) . ? N3 C7 1.477(5) . ? N3 C32 1.482(5) . ? N3 C31 1.489(5) . ? N4 C33 1.339(5) . ? N4 C37 1.342(4) . ? N5 C35 1.352(4) . ? N5 C39 1.452(5) . ? N5 C38 1.460(5) . ? N6 C40 1.411(4) . ? C1 C2 1.513(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.379(5) . ? C3 C4 1.418(5) . ? C3 H3 0.9300 . ? C4 C5 1.505(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.516(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C11 C16 1.395(5) . ? C11 C12 1.412(6) . ? C12 C13 1.405(6) . ? C12 C20 1.497(6) . ? C13 C14 1.378(7) . ? C13 H13 0.9300 . ? C14 C15 1.331(7) . ? C14 H14 0.9300 . ? C15 C16 1.400(5) . ? C15 H15 0.9300 . ? C16 C17 1.531(6) . ? C17 C19 1.527(6) . ? C17 C18 1.539(6) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C22 1.536(6) . ? C20 C21 1.565(6) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.367(5) . ? C33 H33 0.9300 . ? C34 C35 1.376(5) . ? C34 H34 0.9300 . ? C35 C36 1.417(5) . ? C36 C37 1.362(5) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C45 1.402(5) . ? C40 C41 1.420(5) . ? C41 C42 1.404(5) . ? C41 C49 1.507(5) . ? C42 C43 1.375(6) . ? C42 H42 0.9300 . ? C43 C44 1.362(6) . ? C43 H43 0.9300 . ? C44 C45 1.404(5) . ? C44 H44 0.9300 . ? C45 C46 1.512(5) . ? C46 C47 1.506(5) . ? C46 C48 1.530(5) . ? C46 H46 0.9800 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C51 1.519(5) . ? C49 C50 1.541(5) . ? C49 H49 0.9800 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? 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 N6 Sc1 N1 114.08(12) . . ? N6 Sc1 N2 106.03(11) . . ? N1 Sc1 N2 83.19(11) . . ? N6 Sc1 N4 103.39(12) . . ? N1 Sc1 N4 95.09(11) . . ? N2 Sc1 N4 148.46(12) . . ? N6 Sc1 N3 111.89(12) . . ? N1 Sc1 N3 132.77(11) . . ? N2 Sc1 N3 74.36(12) . . ? N4 Sc1 N3 84.37(11) . . ? N6 Sc1 Cu1 39.23(8) . . ? N1 Sc1 Cu1 116.83(8) . . ? N2 Sc1 Cu1 67.91(8) . . ? N4 Sc1 Cu1 137.29(9) . . ? N3 Sc1 Cu1 92.49(8) . . ? N6 Cu1 I1 173.58(9) . . ? N6 Cu1 Sc1 40.18(9) . . ? I1 Cu1 Sc1 145.97(3) . . ? C2 N1 C11 117.8(3) . . ? C2 N1 Sc1 119.0(2) . . ? C11 N1 Sc1 123.2(2) . . ? C4 N2 C6 118.5(3) . . ? C4 N2 Sc1 122.2(3) . . ? C6 N2 Sc1 118.7(3) . . ? C7 N3 C32 109.6(3) . . ? C7 N3 C31 108.8(3) . . ? C32 N3 C31 107.7(3) . . ? C7 N3 Sc1 103.3(2) . . ? C32 N3 Sc1 110.2(2) . . ? C31 N3 Sc1 117.1(2) . . ? C33 N4 C37 114.3(3) . . ? C33 N4 Sc1 127.4(3) . . ? C37 N4 Sc1 117.5(3) . . ? C35 N5 C39 123.7(4) . . ? C35 N5 C38 120.5(4) . . ? C39 N5 C38 115.7(3) . . ? C40 N6 Cu1 106.9(2) . . ? C40 N6 Sc1 152.5(2) . . ? Cu1 N6 Sc1 100.59(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.2(4) . . ? N1 C2 C1 119.7(3) . . ? C3 C2 C1 117.1(3) . . ? C2 C3 C4 128.9(4) . . ? C2 C3 H3 115.6 . . ? C4 C3 H3 115.6 . . ? N2 C4 C3 121.8(3) . . ? N2 C4 C5 121.6(4) . . ? C3 C4 C5 116.6(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 108.4(3) . . ? N2 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? N2 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N3 C7 C6 112.4(3) . . ? N3 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C16 C11 C12 121.0(4) . . ? C16 C11 N1 122.1(4) . . ? C12 C11 N1 116.9(4) . . ? C13 C12 C11 117.1(5) . . ? C13 C12 C20 120.3(5) . . ? C11 C12 C20 122.6(4) . . ? C14 C13 C12 121.5(5) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 119.9(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 122.6(5) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C11 C16 C15 117.8(4) . . ? C11 C16 C17 123.3(4) . . ? C15 C16 C17 119.0(4) . . ? C19 C17 C16 112.4(4) . . ? C19 C17 C18 109.6(4) . . ? C16 C17 C18 111.2(4) . . ? C19 C17 H17 107.8 . . ? C16 C17 H17 107.8 . . ? C18 C17 H17 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C12 C20 C22 112.8(4) . . ? C12 C20 C21 113.7(4) . . ? C22 C20 C21 108.6(4) . . ? C12 C20 H20 107.1 . . ? C22 C20 H20 107.1 . . ? C21 C20 H20 107.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C33 C34 125.1(4) . . ? N4 C33 H33 117.5 . . ? C34 C33 H33 117.5 . . ? C33 C34 C35 120.6(4) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? N5 C35 C34 123.3(4) . . ? N5 C35 C36 121.8(4) . . ? C34 C35 C36 114.9(4) . . ? C37 C36 C35 119.9(4) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? N4 C37 C36 124.9(4) . . ? N4 C37 H37 117.5 . . ? C36 C37 H37 117.5 . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 N6 121.7(3) . . ? C45 C40 C41 118.8(4) . . ? N6 C40 C41 119.5(3) . . ? C42 C41 C40 118.7(4) . . ? C42 C41 C49 120.2(4) . . ? C40 C41 C49 121.0(4) . . ? C43 C42 C41 121.9(4) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C44 C43 C42 119.2(4) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 121.7(4) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C40 C45 C44 119.6(4) . . ? C40 C45 C46 121.3(4) . . ? C44 C45 C46 118.9(4) . . ? C47 C46 C45 110.7(3) . . ? C47 C46 C48 109.2(4) . . ? C45 C46 C48 113.5(4) . . ? C47 C46 H46 107.7 . . ? C45 C46 H46 107.7 . . ? C48 C46 H46 107.7 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C41 C49 C51 114.5(4) . . ? C41 C49 C50 110.4(3) . . ? C51 C49 C50 108.9(3) . . ? C41 C49 H49 107.6 . . ? C51 C49 H49 107.6 . . ? C50 C49 H49 107.6 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 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 N1 Sc1 Cu1 N6 95.93(15) . . . . ? N2 Sc1 Cu1 N6 165.52(16) . . . . ? N4 Sc1 Cu1 N6 -38.08(18) . . . . ? N3 Sc1 Cu1 N6 -122.47(15) . . . . ? N6 Sc1 Cu1 I1 176.91(14) . . . . ? N1 Sc1 Cu1 I1 -87.16(10) . . . . ? N2 Sc1 Cu1 I1 -17.57(11) . . . . ? N4 Sc1 Cu1 I1 138.83(12) . . . . ? N3 Sc1 Cu1 I1 54.44(9) . . . . ? N6 Sc1 N1 C2 61.4(3) . . . . ? N2 Sc1 N1 C2 -43.1(3) . . . . ? N4 Sc1 N1 C2 168.5(3) . . . . ? N3 Sc1 N1 C2 -104.4(3) . . . . ? Cu1 Sc1 N1 C2 17.9(3) . . . . ? N6 Sc1 N1 C11 -121.1(3) . . . . ? N2 Sc1 N1 C11 134.3(3) . . . . ? N4 Sc1 N1 C11 -14.0(3) . . . . ? N3 Sc1 N1 C11 73.0(3) . . . . ? Cu1 Sc1 N1 C11 -164.7(3) . . . . ? N6 Sc1 N2 C4 -72.9(3) . . . . ? N1 Sc1 N2 C4 40.3(3) . . . . ? N4 Sc1 N2 C4 128.9(3) . . . . ? N3 Sc1 N2 C4 178.3(3) . . . . ? Cu1 Sc1 N2 C4 -82.3(3) . . . . ? N6 Sc1 N2 C6 97.8(3) . . . . ? N1 Sc1 N2 C6 -149.1(3) . . . . ? N4 Sc1 N2 C6 -60.4(4) . . . . ? N3 Sc1 N2 C6 -11.0(3) . . . . ? Cu1 Sc1 N2 C6 88.3(3) . . . . ? N6 Sc1 N3 C7 -68.9(3) . . . . ? N1 Sc1 N3 C7 97.2(3) . . . . ? N2 Sc1 N3 C7 32.5(2) . . . . ? N4 Sc1 N3 C7 -171.0(3) . . . . ? Cu1 Sc1 N3 C7 -33.8(2) . . . . ? N6 Sc1 N3 C32 174.1(2) . . . . ? N1 Sc1 N3 C32 -19.8(3) . . . . ? N2 Sc1 N3 C32 -84.5(3) . . . . ? N4 Sc1 N3 C32 71.9(3) . . . . ? Cu1 Sc1 N3 C32 -150.8(2) . . . . ? N6 Sc1 N3 C31 50.6(3) . . . . ? N1 Sc1 N3 C31 -143.3(3) . . . . ? N2 Sc1 N3 C31 152.0(3) . . . . ? N4 Sc1 N3 C31 -51.6(3) . . . . ? Cu1 Sc1 N3 C31 85.7(3) . . . . ? N6 Sc1 N4 C33 175.6(3) . . . . ? N1 Sc1 N4 C33 59.3(3) . . . . ? N2 Sc1 N4 C33 -25.9(4) . . . . ? N3 Sc1 N4 C33 -73.2(3) . . . . ? Cu1 Sc1 N4 C33 -160.8(3) . . . . ? N6 Sc1 N4 C37 -15.4(3) . . . . ? N1 Sc1 N4 C37 -131.7(3) . . . . ? N2 Sc1 N4 C37 143.1(3) . . . . ? N3 Sc1 N4 C37 95.8(3) . . . . ? Cu1 Sc1 N4 C37 8.2(3) . . . . ? I1 Cu1 N6 C40 17.1(9) . . . . ? Sc1 Cu1 N6 C40 -178.5(3) . . . . ? I1 Cu1 N6 Sc1 -164.4(7) . . . . ? N1 Sc1 N6 C40 73.4(5) . . . . ? N2 Sc1 N6 C40 163.0(5) . . . . ? N4 Sc1 N6 C40 -28.5(5) . . . . ? N3 Sc1 N6 C40 -117.8(5) . . . . ? Cu1 Sc1 N6 C40 176.9(6) . . . . ? N1 Sc1 N6 Cu1 -103.56(13) . . . . ? N2 Sc1 N6 Cu1 -13.95(15) . . . . ? N4 Sc1 N6 Cu1 154.53(11) . . . . ? N3 Sc1 N6 Cu1 65.28(14) . . . . ? C11 N1 C2 C3 -151.9(4) . . . . ? Sc1 N1 C2 C3 25.7(5) . . . . ? C11 N1 C2 C1 26.7(5) . . . . ? Sc1 N1 C2 C1 -155.7(3) . . . . ? N1 C2 C3 C4 17.1(7) . . . . ? C1 C2 C3 C4 -161.5(4) . . . . ? C6 N2 C4 C3 171.4(4) . . . . ? Sc1 N2 C4 C3 -17.9(5) . . . . ? C6 N2 C4 C5 -6.5(6) . . . . ? Sc1 N2 C4 C5 164.2(3) . . . . ? C2 C3 C4 N2 -21.9(7) . . . . ? C2 C3 C4 C5 156.1(4) . . . . ? C4 N2 C6 C7 158.1(4) . . . . ? Sc1 N2 C6 C7 -12.9(4) . . . . ? C32 N3 C7 C6 65.4(4) . . . . ? C31 N3 C7 C6 -177.1(3) . . . . ? Sc1 N3 C7 C6 -52.1(4) . . . . ? N2 C6 C7 N3 45.2(5) . . . . ? C2 N1 C11 C16 -96.0(4) . . . . ? Sc1 N1 C11 C16 86.5(4) . . . . ? C2 N1 C11 C12 85.9(4) . . . . ? Sc1 N1 C11 C12 -91.6(4) . . . . ? C16 C11 C12 C13 -2.3(6) . . . . ? N1 C11 C12 C13 175.9(3) . . . . ? C16 C11 C12 C20 177.5(4) . . . . ? N1 C11 C12 C20 -4.3(6) . . . . ? C11 C12 C13 C14 -0.2(7) . . . . ? C20 C12 C13 C14 179.9(4) . . . . ? C12 C13 C14 C15 0.8(8) . . . . ? C13 C14 C15 C16 1.1(8) . . . . ? C12 C11 C16 C15 4.1(6) . . . . ? N1 C11 C16 C15 -174.0(3) . . . . ? C12 C11 C16 C17 -175.0(4) . . . . ? N1 C11 C16 C17 6.9(6) . . . . ? C14 C15 C16 C11 -3.5(7) . . . . ? C14 C15 C16 C17 175.6(4) . . . . ? C11 C16 C17 C19 -116.2(4) . . . . ? C15 C16 C17 C19 64.7(5) . . . . ? C11 C16 C17 C18 120.5(4) . . . . ? C15 C16 C17 C18 -58.6(5) . . . . ? C13 C12 C20 C22 81.3(5) . . . . ? C11 C12 C20 C22 -98.5(5) . . . . ? C13 C12 C20 C21 -42.9(6) . . . . ? C11 C12 C20 C21 137.3(4) . . . . ? C37 N4 C33 C34 -3.4(6) . . . . ? Sc1 N4 C33 C34 165.9(3) . . . . ? N4 C33 C34 C35 -0.1(7) . . . . ? C39 N5 C35 C34 -178.0(4) . . . . ? C38 N5 C35 C34 4.8(6) . . . . ? C39 N5 C35 C36 0.6(6) . . . . ? C38 N5 C35 C36 -176.6(4) . . . . ? C33 C34 C35 N5 -177.2(4) . . . . ? C33 C34 C35 C36 4.1(6) . . . . ? N5 C35 C36 C37 176.7(4) . . . . ? C34 C35 C36 C37 -4.6(6) . . . . ? C33 N4 C37 C36 2.9(6) . . . . ? Sc1 N4 C37 C36 -167.6(3) . . . . ? C35 C36 C37 N4 1.1(6) . . . . ? Cu1 N6 C40 C45 -86.0(3) . . . . ? Sc1 N6 C40 C45 97.1(6) . . . . ? Cu1 N6 C40 C41 95.5(3) . . . . ? Sc1 N6 C40 C41 -81.3(6) . . . . ? C45 C40 C41 C42 -4.1(5) . . . . ? N6 C40 C41 C42 174.4(3) . . . . ? C45 C40 C41 C49 171.7(3) . . . . ? N6 C40 C41 C49 -9.8(5) . . . . ? C40 C41 C42 C43 1.5(6) . . . . ? C49 C41 C42 C43 -174.3(4) . . . . ? C41 C42 C43 C44 2.0(7) . . . . ? C42 C43 C44 C45 -2.9(7) . . . . ? N6 C40 C45 C44 -175.2(3) . . . . ? C41 C40 C45 C44 3.3(5) . . . . ? N6 C40 C45 C46 9.2(5) . . . . ? C41 C40 C45 C46 -172.4(3) . . . . ? C43 C44 C45 C40 0.2(6) . . . . ? C43 C44 C45 C46 176.0(4) . . . . ? C40 C45 C46 C47 97.8(4) . . . . ? C44 C45 C46 C47 -77.9(5) . . . . ? C40 C45 C46 C48 -138.9(4) . . . . ? C44 C45 C46 C48 45.4(5) . . . . ? C42 C41 C49 C51 -30.2(5) . . . . ? C40 C41 C49 C51 154.1(3) . . . . ? C42 C41 C49 C50 93.0(4) . . . . ? C40 C41 C49 C50 -82.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.633 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.068 #===END data_dm1132 _database_code_depnum_ccdc_archive 'CCDC 851601' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H70 Cl N5 Rh Sc' _chemical_formula_weight 852.37 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' Sc Sc 0.2519 0.3716 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.2520(12) _cell_length_b 22.398(2) _cell_length_c 15.4942(14) _cell_angle_alpha 90.00 _cell_angle_beta 110.3550(10) _cell_angle_gamma 90.00 _cell_volume 4311.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5582 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9104 _exptl_absorpt_correction_T_max 0.9688 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28282 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8452 _reflns_number_gt 5731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8452 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 -0.46934(2) -0.477948(16) -0.72246(2) 0.01477(10) Uani 1 1 d . . . Sc1 Sc -0.73809(6) -0.66640(4) -0.79963(5) 0.01198(18) Uani 1 1 d . . . Cl1 Cl -0.70345(8) -0.75011(5) -0.69115(7) 0.0222(2) Uani 1 1 d . . . N1 N -0.9108(2) -0.65862(15) -0.8128(2) 0.0127(7) Uani 1 1 d . . . N2 N -0.8007(3) -0.63630(16) -0.9442(2) 0.0162(8) Uani 1 1 d . . . N3 N -0.6377(2) -0.71825(16) -0.8751(2) 0.0154(7) Uani 1 1 d . . . N4 N -0.3479(3) -0.77816(19) -0.8079(3) 0.0302(10) Uani 1 1 d . . . N5 N -0.6468(3) -0.60159(16) -0.7357(2) 0.0162(8) Uani 1 1 d . . . C11 C -0.9461(3) -0.69122(19) -0.7473(3) 0.0140(9) Uani 1 1 d . . . C12 C -0.9419(3) -0.6640(2) -0.6638(3) 0.0162(9) Uani 1 1 d . . . C13 C -0.9696(3) -0.6979(2) -0.6008(3) 0.0211(10) Uani 1 1 d . . . H13 H -0.9661 -0.6803 -0.5441 0.025 Uiso 1 1 calc R . . C14 C -1.0023(3) -0.7568(2) -0.6181(3) 0.0217(10) Uani 1 1 d . . . H14 H -1.0206 -0.7793 -0.5736 0.026 Uiso 1 1 calc R . . C15 C -1.0078(3) -0.7822(2) -0.7002(3) 0.0192(10) Uani 1 1 d . . . H15 H -1.0317 -0.8224 -0.7126 0.023 Uiso 1 1 calc R . . C16 C -0.9796(3) -0.7510(2) -0.7655(3) 0.0155(9) Uani 1 1 d . . . C20 C -0.9068(3) -0.5994(2) -0.6416(3) 0.0203(10) Uani 1 1 d . . . H20 H -0.9052 -0.5803 -0.6995 0.024 Uiso 1 1 calc R . . C21 C -0.9836(4) -0.5636(2) -0.6083(3) 0.0347(12) Uani 1 1 d . . . H21A H -1.0561 -0.5652 -0.6547 0.052 Uiso 1 1 calc R . . H21B H -0.9594 -0.5220 -0.5984 0.052 Uiso 1 1 calc R . . H21C H -0.9848 -0.5806 -0.5504 0.052 Uiso 1 1 calc R . . C22 C -0.7920(4) -0.5976(2) -0.5709(3) 0.0295(11) Uani 1 1 d . . . H22C H -0.7440 -0.6208 -0.5939 0.044 Uiso 1 1 calc R . . H22B H -0.7918 -0.6146 -0.5126 0.044 Uiso 1 1 calc R . . H22A H -0.7671 -0.5561 -0.5611 0.044 Uiso 1 1 calc R . . C17 C -0.9858(3) -0.7819(2) -0.8551(3) 0.0186(9) Uani 1 1 d . . . H17 H -0.9453 -0.7568 -0.8854 0.022 Uiso 1 1 calc R . . C19 C -0.9342(4) -0.8432(2) -0.8385(3) 0.0312(12) Uani 1 1 d . . . H19B H -0.8594 -0.8397 -0.7966 0.047 Uiso 1 1 calc R . . H19A H -0.9356 -0.8602 -0.8972 0.047 Uiso 1 1 calc R . . H19C H -0.9741 -0.8692 -0.8109 0.047 Uiso 1 1 calc R . . C18 C -1.1029(4) -0.7856(3) -0.9206(3) 0.0361(13) Uani 1 1 d . . . H18A H -1.1345 -0.7455 -0.9308 0.054 Uiso 1 1 calc R . . H18C H -1.1440 -0.8111 -0.8933 0.054 Uiso 1 1 calc R . . H18B H -1.1052 -0.8026 -0.9795 0.054 Uiso 1 1 calc R . . C1 C -1.0923(3) -0.6126(2) -0.8624(3) 0.0262(11) Uani 1 1 d . . . H1B H -1.0966 -0.6354 -0.8098 0.039 Uiso 1 1 calc R . . H1A H -1.1489 -0.6260 -0.9188 0.039 Uiso 1 1 calc R . . H1C H -1.1018 -0.5700 -0.8529 0.039 Uiso 1 1 calc R . . C2 C -0.9830(3) -0.62252(19) -0.8713(3) 0.0152(9) Uani 1 1 d . . . C3 C -0.9661(3) -0.5928(2) -0.9442(3) 0.0189(9) Uani 1 1 d . . . H3 H -1.0169 -0.5624 -0.9726 0.023 Uiso 1 1 calc R . . C4 C -0.8843(3) -0.60145(19) -0.9815(3) 0.0158(9) Uani 1 1 d . . . C5 C -0.8993(3) -0.5683(2) -1.0700(3) 0.0225(10) Uani 1 1 d . . . H17A H -0.9101 -0.5971 -1.1201 0.034 Uiso 1 1 calc R . . H5B H -0.8352 -0.5442 -1.0628 0.034 Uiso 1 1 calc R . . H5C H -0.9623 -0.5422 -1.0844 0.034 Uiso 1 1 calc R . . C6 C -0.7332(3) -0.6487(2) -1.0004(3) 0.0252(11) Uani 1 1 d . . . H6A H -0.7223 -0.6115 -1.0305 0.030 Uiso 1 1 calc R . . H6B H -0.7701 -0.6779 -1.0492 0.030 Uiso 1 1 calc R . . C7 C -0.6258(3) -0.6734(2) -0.9407(3) 0.0240(10) Uani 1 1 d . . . H7B H -0.5896 -0.6919 -0.9802 0.029 Uiso 1 1 calc R . . H7A H -0.5797 -0.6403 -0.9061 0.029 Uiso 1 1 calc R . . C8 C -0.5288(3) -0.7385(2) -0.8129(3) 0.0200(10) Uani 1 1 d . . . H8A H -0.5380 -0.7616 -0.7617 0.024 Uiso 1 1 calc R . . H8B H -0.4856 -0.7027 -0.7858 0.024 Uiso 1 1 calc R . . C9 C -0.4654(3) -0.7762(2) -0.8572(3) 0.0227(10) Uani 1 1 d . . . H9B H -0.4935 -0.8175 -0.8633 0.027 Uiso 1 1 calc R . . H9A H -0.4787 -0.7608 -0.9201 0.027 Uiso 1 1 calc R . . C10 C -0.7025(3) -0.7699(2) -0.9227(3) 0.0225(10) Uani 1 1 d . . . H10C H -0.6627 -0.7923 -0.9548 0.034 Uiso 1 1 calc R . . H10B H -0.7707 -0.7558 -0.9673 0.034 Uiso 1 1 calc R . . H10A H -0.7171 -0.7959 -0.8774 0.034 Uiso 1 1 calc R . . C23 C -0.2972(4) -0.7213(3) -0.8166(4) 0.0474(15) Uani 1 1 d . . . H23A H -0.2195 -0.7237 -0.7829 0.071 Uiso 1 1 calc R . . H23B H -0.3280 -0.6890 -0.7910 0.071 Uiso 1 1 calc R . . H23C H -0.3101 -0.7133 -0.8818 0.071 Uiso 1 1 calc R . . C24 C -0.3198(4) -0.7958(3) -0.7116(3) 0.0388(13) Uani 1 1 d . . . H24A H -0.2413 -0.7962 -0.6819 0.058 Uiso 1 1 calc R . . H24B H -0.3483 -0.8358 -0.7084 0.058 Uiso 1 1 calc R . . H24C H -0.3509 -0.7673 -0.6799 0.058 Uiso 1 1 calc R . . C25 C -0.5925(3) -0.55652(19) -0.6896(3) 0.0145(9) Uani 1 1 d . . . C26 C -0.6406(3) -0.49637(19) -0.6934(3) 0.0160(9) Uani 1 1 d . . . C27 C -0.5818(3) -0.4497(2) -0.6416(3) 0.0170(9) Uani 1 1 d . . . H27A H -0.6141 -0.4088 -0.6521 0.020 Uiso 1 1 calc R . . C28 C -0.4713(3) -0.4557(2) -0.5858(3) 0.0185(9) Uani 1 1 d . . . H28A H -0.4297 -0.4207 -0.5511 0.022 Uiso 1 1 calc R . . C29 C -0.4233(3) -0.5126(2) -0.5773(3) 0.0179(9) Uani 1 1 d . . . H29A H -0.3453 -0.5169 -0.5396 0.021 Uiso 1 1 calc R . . C30 C -0.4764(3) -0.56032(19) -0.6318(3) 0.0161(9) Uani 1 1 d . . . C31 C -0.7586(3) -0.4884(2) -0.7503(3) 0.0208(10) Uani 1 1 d . . . H31A H -0.7936 -0.5283 -0.7529 0.025 Uiso 1 1 calc R . . C32 C -0.7756(4) -0.4705(2) -0.8489(3) 0.0330(12) Uani 1 1 d . . . H32A H -0.7390 -0.4991 -0.8758 0.049 Uiso 1 1 calc R . . H32B H -0.7460 -0.4305 -0.8496 0.049 Uiso 1 1 calc R . . H32C H -0.8528 -0.4703 -0.8849 0.049 Uiso 1 1 calc R . . C33 C -0.8163(4) -0.4450(2) -0.7070(3) 0.0323(12) Uani 1 1 d . . . H33A H -0.8053 -0.4575 -0.6438 0.048 Uiso 1 1 calc R . . H33B H -0.8935 -0.4450 -0.7431 0.048 Uiso 1 1 calc R . . H33C H -0.7872 -0.4047 -0.7065 0.048 Uiso 1 1 calc R . . C34 C -0.4208(3) -0.6196(2) -0.6280(3) 0.0219(10) Uani 1 1 d . . . H34A H -0.4507 -0.6377 -0.6908 0.026 Uiso 1 1 calc R . . C35 C -0.4469(4) -0.6623(2) -0.5612(3) 0.0283(11) Uani 1 1 d . . . H35A H -0.5252 -0.6655 -0.5780 0.042 Uiso 1 1 calc R . . H35B H -0.4155 -0.6469 -0.4983 0.042 Uiso 1 1 calc R . . H35C H -0.4168 -0.7018 -0.5647 0.042 Uiso 1 1 calc R . . C36 C -0.2995(4) -0.6145(2) -0.6041(3) 0.0351(12) Uani 1 1 d . . . H36A H -0.2841 -0.5874 -0.6476 0.053 Uiso 1 1 calc R . . H36B H -0.2695 -0.6540 -0.6077 0.053 Uiso 1 1 calc R . . H36C H -0.2669 -0.5987 -0.5415 0.053 Uiso 1 1 calc R . . C37 C -0.5228(4) -0.4981(2) -0.8658(3) 0.0238(10) Uani 1 1 d . . . H37A H -0.5862 -0.5256 -0.8868 0.029 Uiso 1 1 calc R . . C38 C -0.4245(3) -0.5271(2) -0.8220(3) 0.0230(10) Uani 1 1 d . . . H38A H -0.4304 -0.5714 -0.8174 0.028 Uiso 1 1 calc R . . C39 C -0.3194(4) -0.5059(3) -0.8303(4) 0.0414(14) Uani 1 1 d . . . H39A H -0.2724 -0.5409 -0.8266 0.050 Uiso 1 1 calc R . . H39B H -0.3347 -0.4873 -0.8915 0.050 Uiso 1 1 calc R . . C40 C -0.2605(4) -0.4620(2) -0.7573(4) 0.0372(13) Uani 1 1 d . . . H40A H -0.2224 -0.4332 -0.7836 0.045 Uiso 1 1 calc R . . H40B H -0.2057 -0.4836 -0.7067 0.045 Uiso 1 1 calc R . . C41 C -0.3330(3) -0.4278(2) -0.7180(3) 0.0255(11) Uani 1 1 d . . . H41A H -0.2942 -0.4094 -0.6566 0.031 Uiso 1 1 calc R . . C42 C -0.4246(4) -0.3968(2) -0.7699(3) 0.0268(11) Uani 1 1 d . . . H42A H -0.4391 -0.3606 -0.7384 0.032 Uiso 1 1 calc R . . C43 C -0.4634(4) -0.3913(2) -0.8742(3) 0.0336(12) Uani 1 1 d . . . H43A H -0.5019 -0.3529 -0.8924 0.040 Uiso 1 1 calc R . . H43B H -0.4001 -0.3906 -0.8942 0.040 Uiso 1 1 calc R . . C44 C -0.5368(5) -0.4412(2) -0.9232(3) 0.0416(14) Uani 1 1 d . . . H44A H -0.5230 -0.4506 -0.9806 0.050 Uiso 1 1 calc R . . H44B H -0.6123 -0.4276 -0.9407 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01517(16) 0.01703(18) 0.01435(16) -0.00276(15) 0.00796(12) -0.00299(16) Sc1 0.0095(3) 0.0145(4) 0.0135(4) 0.0009(3) 0.0060(3) 0.0004(3) Cl1 0.0187(5) 0.0229(6) 0.0282(6) 0.0099(5) 0.0123(4) 0.0041(5) N1 0.0092(15) 0.019(2) 0.0120(17) 0.0016(14) 0.0057(13) -0.0018(15) N2 0.0150(17) 0.021(2) 0.0172(18) 0.0028(15) 0.0113(14) 0.0026(16) N3 0.0140(16) 0.0140(19) 0.0192(18) 0.0021(15) 0.0070(14) 0.0011(15) N4 0.0191(19) 0.034(3) 0.040(2) -0.001(2) 0.0148(17) 0.0037(19) N5 0.0158(17) 0.019(2) 0.0145(17) -0.0028(15) 0.0061(14) -0.0029(16) C11 0.0085(18) 0.022(2) 0.012(2) 0.0043(17) 0.0040(15) 0.0014(18) C12 0.0102(19) 0.022(2) 0.017(2) -0.0002(18) 0.0052(16) -0.0007(18) C13 0.019(2) 0.033(3) 0.012(2) -0.0017(19) 0.0079(17) -0.004(2) C14 0.019(2) 0.031(3) 0.017(2) 0.007(2) 0.0079(18) -0.006(2) C15 0.014(2) 0.020(3) 0.025(2) 0.0023(19) 0.0088(18) -0.0039(19) C16 0.0072(18) 0.022(2) 0.016(2) -0.0002(18) 0.0020(15) 0.0012(18) C20 0.025(2) 0.021(3) 0.018(2) -0.0021(18) 0.0108(18) -0.002(2) C21 0.042(3) 0.030(3) 0.039(3) 0.000(2) 0.023(2) 0.009(3) C22 0.036(3) 0.026(3) 0.023(2) -0.005(2) 0.006(2) -0.007(2) C17 0.021(2) 0.022(3) 0.016(2) -0.0029(18) 0.0106(17) -0.004(2) C19 0.044(3) 0.027(3) 0.031(3) -0.003(2) 0.024(2) -0.005(2) C18 0.026(2) 0.058(4) 0.024(3) -0.016(2) 0.008(2) -0.007(3) C1 0.017(2) 0.038(3) 0.025(2) 0.011(2) 0.0085(19) 0.015(2) C2 0.0122(19) 0.019(2) 0.015(2) -0.0028(17) 0.0055(16) -0.0019(18) C3 0.015(2) 0.021(3) 0.019(2) 0.0030(18) 0.0042(17) 0.0085(19) C4 0.017(2) 0.018(2) 0.013(2) 0.0020(17) 0.0057(17) -0.0013(18) C5 0.022(2) 0.030(3) 0.018(2) 0.007(2) 0.0106(18) 0.004(2) C6 0.029(2) 0.029(3) 0.026(2) 0.011(2) 0.020(2) 0.009(2) C7 0.022(2) 0.025(3) 0.034(3) 0.006(2) 0.021(2) 0.001(2) C8 0.016(2) 0.020(3) 0.024(2) -0.0003(19) 0.0087(18) 0.0031(19) C9 0.021(2) 0.022(3) 0.026(2) -0.003(2) 0.0087(18) 0.004(2) C10 0.024(2) 0.020(3) 0.025(2) -0.0075(19) 0.0101(19) -0.001(2) C23 0.029(3) 0.050(4) 0.071(4) 0.006(3) 0.026(3) -0.007(3) C24 0.023(2) 0.042(4) 0.046(3) 0.005(3) 0.006(2) 0.009(2) C25 0.015(2) 0.020(2) 0.012(2) 0.0048(18) 0.0100(16) -0.0009(18) C26 0.017(2) 0.020(2) 0.015(2) 0.0015(17) 0.0098(17) -0.0026(18) C27 0.021(2) 0.018(2) 0.016(2) 0.0019(18) 0.0113(18) 0.0021(19) C28 0.024(2) 0.018(2) 0.017(2) -0.0066(18) 0.0120(18) -0.0033(19) C29 0.018(2) 0.023(3) 0.014(2) -0.0028(18) 0.0068(17) -0.0014(19) C30 0.0126(19) 0.021(2) 0.016(2) -0.0012(18) 0.0067(16) -0.0005(18) C31 0.018(2) 0.015(3) 0.031(2) 0.0004(19) 0.0111(19) 0.0000(19) C32 0.023(2) 0.047(4) 0.025(2) 0.007(2) 0.003(2) 0.002(2) C33 0.021(2) 0.035(3) 0.040(3) -0.001(2) 0.009(2) 0.010(2) C34 0.021(2) 0.021(3) 0.019(2) -0.0051(19) 0.0012(18) 0.001(2) C35 0.034(3) 0.022(3) 0.025(2) 0.006(2) 0.006(2) 0.006(2) C36 0.022(2) 0.038(3) 0.042(3) -0.003(3) 0.006(2) 0.009(2) C37 0.034(3) 0.023(3) 0.017(2) -0.0056(19) 0.012(2) -0.005(2) C38 0.027(2) 0.026(3) 0.023(2) -0.010(2) 0.0173(19) -0.005(2) C39 0.037(3) 0.050(4) 0.050(3) -0.020(3) 0.031(3) -0.013(3) C40 0.027(3) 0.042(4) 0.047(3) -0.008(3) 0.018(2) -0.007(2) C41 0.019(2) 0.034(3) 0.030(3) -0.008(2) 0.016(2) -0.016(2) C42 0.035(3) 0.021(3) 0.032(3) 0.000(2) 0.023(2) -0.009(2) C43 0.050(3) 0.026(3) 0.034(3) 0.002(2) 0.026(2) -0.006(3) C44 0.067(4) 0.038(3) 0.026(3) 0.004(2) 0.024(3) 0.005(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 Rh1 C41 2.108(4) . ? Rh1 C42 2.121(4) . ? Rh1 C37 2.132(4) . ? Rh1 C38 2.140(4) . ? Rh1 C28 2.184(4) . ? Rh1 C29 2.254(4) . ? Rh1 C30 2.340(4) . ? Rh1 C27 2.344(4) . ? Rh1 C26 2.497(4) . ? Rh1 C25 2.568(4) . ? Sc1 N5 1.928(4) . ? Sc1 N2 2.206(3) . ? Sc1 N1 2.233(3) . ? Sc1 N3 2.360(3) . ? Sc1 Cl1 2.4525(13) . ? N1 C2 1.337(5) . ? N1 C11 1.453(5) . ? N2 C4 1.313(5) . ? N2 C6 1.475(5) . ? N3 C7 1.476(5) . ? N3 C10 1.476(5) . ? N3 C8 1.500(5) . ? N4 C24 1.461(6) . ? N4 C23 1.468(6) . ? N4 C9 1.477(5) . ? N5 C25 1.300(5) . ? C11 C16 1.407(6) . ? C11 C12 1.413(5) . ? C12 C13 1.384(6) . ? C12 C20 1.523(6) . ? C13 C14 1.385(6) . ? C13 H13 0.9500 . ? C14 C15 1.373(6) . ? C14 H14 0.9500 . ? C15 C16 1.386(6) . ? C15 H15 0.9500 . ? C16 C17 1.527(6) . ? C20 C21 1.520(6) . ? C20 C22 1.535(6) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C22 H22A 0.9800 . ? C17 C19 1.515(6) . ? C17 C18 1.533(6) . ? C17 H17 1.0000 . ? C19 H19B 0.9800 . ? C19 H19A 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18C 0.9800 . ? C18 H18B 0.9800 . ? C1 C2 1.517(5) . ? C1 H1B 0.9800 . ? C1 H1A 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.395(6) . ? C3 C4 1.409(5) . ? C3 H3 0.9500 . ? C4 C5 1.510(5) . ? C5 H17A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.508(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 C9 1.514(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.483(6) . ? C25 C30 1.489(5) . ? C26 C27 1.381(6) . ? C26 C31 1.514(6) . ? C27 C28 1.425(6) . ? C27 H27A 1.0000 . ? C28 C29 1.410(6) . ? C28 H28A 1.0000 . ? C29 C30 1.391(6) . ? C29 H29A 1.0000 . ? C30 C34 1.509(6) . ? C31 C32 1.519(6) . ? C31 C33 1.529(6) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.523(6) . ? C34 C35 1.536(6) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.402(6) . ? C37 C44 1.527(7) . ? C37 H37A 1.0000 . ? C38 C39 1.518(6) . ? C38 H38A 1.0000 . ? C39 C40 1.498(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.512(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.386(6) . ? C41 H41A 1.0000 . ? C42 C43 1.520(6) . ? C42 H42A 1.0000 . ? C43 C44 1.503(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Rh1 C42 38.26(18) . . ? C41 Rh1 C37 96.72(17) . . ? C42 Rh1 C37 81.49(18) . . ? C41 Rh1 C38 81.25(17) . . ? C42 Rh1 C38 90.56(18) . . ? C37 Rh1 C38 38.31(17) . . ? C41 Rh1 C28 98.38(17) . . ? C42 Rh1 C28 103.85(17) . . ? C37 Rh1 C28 161.22(17) . . ? C38 Rh1 C28 156.31(17) . . ? C41 Rh1 C29 102.70(16) . . ? C42 Rh1 C29 129.04(17) . . ? C37 Rh1 C29 147.49(17) . . ? C38 Rh1 C29 119.68(17) . . ? C28 Rh1 C29 37.03(15) . . ? C41 Rh1 C30 127.82(16) . . ? C42 Rh1 C30 163.31(16) . . ? C37 Rh1 C30 112.97(16) . . ? C38 Rh1 C30 96.07(16) . . ? C28 Rh1 C30 65.29(15) . . ? C29 Rh1 C30 35.20(14) . . ? C41 Rh1 C27 122.44(16) . . ? C42 Rh1 C27 105.14(17) . . ? C37 Rh1 C27 124.87(16) . . ? C38 Rh1 C27 155.74(16) . . ? C28 Rh1 C27 36.47(15) . . ? C29 Rh1 C27 63.95(15) . . ? C30 Rh1 C27 74.10(14) . . ? C41 Rh1 C26 154.77(16) . . ? C42 Rh1 C26 125.84(16) . . ? C37 Rh1 C26 99.17(16) . . ? C38 Rh1 C26 122.85(15) . . ? C28 Rh1 C26 62.94(14) . . ? C29 Rh1 C26 73.18(14) . . ? C30 Rh1 C26 62.17(13) . . ? C27 Rh1 C26 32.96(14) . . ? C41 Rh1 C25 162.75(16) . . ? C42 Rh1 C25 158.34(16) . . ? C37 Rh1 C25 93.31(15) . . ? C38 Rh1 C25 98.35(16) . . ? C28 Rh1 C25 75.04(14) . . ? C29 Rh1 C25 62.36(14) . . ? C30 Rh1 C25 34.94(13) . . ? C27 Rh1 C25 60.82(14) . . ? C26 Rh1 C25 34.01(13) . . ? N5 Sc1 N2 103.80(14) . . ? N5 Sc1 N1 115.38(13) . . ? N2 Sc1 N1 82.63(11) . . ? N5 Sc1 N3 105.29(13) . . ? N2 Sc1 N3 74.03(12) . . ? N1 Sc1 N3 136.86(12) . . ? N5 Sc1 Cl1 106.81(11) . . ? N2 Sc1 Cl1 147.57(10) . . ? N1 Sc1 Cl1 93.66(9) . . ? N3 Sc1 Cl1 87.71(9) . . ? C2 N1 C11 116.7(3) . . ? C2 N1 Sc1 125.3(2) . . ? C11 N1 Sc1 117.7(2) . . ? C4 N2 C6 116.3(3) . . ? C4 N2 Sc1 126.2(3) . . ? C6 N2 Sc1 116.8(3) . . ? C7 N3 C10 111.9(3) . . ? C7 N3 C8 109.8(3) . . ? C10 N3 C8 110.3(3) . . ? C7 N3 Sc1 102.7(2) . . ? C10 N3 Sc1 107.6(2) . . ? C8 N3 Sc1 114.3(2) . . ? C24 N4 C23 111.5(4) . . ? C24 N4 C9 112.6(4) . . ? C23 N4 C9 111.1(4) . . ? C25 N5 Sc1 174.5(3) . . ? C16 C11 C12 120.2(4) . . ? C16 C11 N1 119.5(3) . . ? C12 C11 N1 120.2(4) . . ? C13 C12 C11 118.3(4) . . ? C13 C12 C20 119.9(4) . . ? C11 C12 C20 121.9(4) . . ? C12 C13 C14 121.9(4) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 119.1(4) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 121.8(4) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C11 118.7(4) . . ? C15 C16 C17 119.4(4) . . ? C11 C16 C17 121.8(4) . . ? C21 C20 C12 112.9(4) . . ? C21 C20 C22 111.0(4) . . ? C12 C20 C22 109.6(4) . . ? C21 C20 H20 107.7 . . ? C12 C20 H20 107.7 . . ? C22 C20 H20 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22C 109.5 . . ? C20 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C20 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C19 C17 C16 112.2(3) . . ? C19 C17 C18 110.8(4) . . ? C16 C17 C18 110.4(3) . . ? C19 C17 H17 107.7 . . ? C16 C17 H17 107.7 . . ? C18 C17 H17 107.7 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? C17 C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? N1 C2 C3 124.0(3) . . ? N1 C2 C1 120.5(3) . . ? C3 C2 C1 115.5(4) . . ? C2 C3 C4 129.0(4) . . ? C2 C3 H3 115.5 . . ? C4 C3 H3 115.5 . . ? N2 C4 C3 123.6(4) . . ? N2 C4 C5 121.1(3) . . ? C3 C4 C5 115.3(4) . . ? C4 C5 H17A 109.5 . . ? C4 C5 H5B 109.5 . . ? H17A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H17A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 110.1(3) . . ? N2 C6 H6A 109.6 . . ? C7 C6 H6A 109.6 . . ? N2 C6 H6B 109.6 . . ? C7 C6 H6B 109.6 . . ? H6A C6 H6B 108.2 . . ? N3 C7 C6 111.5(3) . . ? N3 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? N3 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? H7B C7 H7A 108.0 . . ? N3 C8 C9 116.0(3) . . ? N3 C8 H8A 108.3 . . ? C9 C8 H8A 108.3 . . ? N3 C8 H8B 108.3 . . ? C9 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? N4 C9 C8 115.7(4) . . ? N4 C9 H9B 108.4 . . ? C8 C9 H9B 108.4 . . ? N4 C9 H9A 108.4 . . ? C8 C9 H9A 108.4 . . ? H9B C9 H9A 107.4 . . ? N3 C10 H10C 109.5 . . ? N3 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? N3 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 122.4(4) . . ? N5 C25 C30 123.0(4) . . ? C26 C25 C30 114.6(4) . . ? N5 C25 Rh1 133.7(3) . . ? C26 C25 Rh1 70.3(2) . . ? C30 C25 Rh1 64.1(2) . . ? C27 C26 C25 121.1(4) . . ? C27 C26 C31 120.6(4) . . ? C25 C26 C31 118.2(4) . . ? C27 C26 Rh1 67.4(2) . . ? C25 C26 Rh1 75.7(2) . . ? C31 C26 Rh1 134.0(3) . . ? C26 C27 C28 122.3(4) . . ? C26 C27 Rh1 79.6(2) . . ? C28 C27 Rh1 65.6(2) . . ? C26 C27 H27A 118.4 . . ? C28 C27 H27A 118.4 . . ? Rh1 C27 H27A 118.4 . . ? C29 C28 C27 118.4(4) . . ? C29 C28 Rh1 74.2(2) . . ? C27 C28 Rh1 77.9(2) . . ? C29 C28 H28A 120.7 . . ? C27 C28 H28A 120.7 . . ? Rh1 C28 H28A 120.7 . . ? C30 C29 C28 121.4(4) . . ? C30 C29 Rh1 75.8(2) . . ? C28 C29 Rh1 68.8(2) . . ? C30 C29 H29A 118.8 . . ? C28 C29 H29A 118.8 . . ? Rh1 C29 H29A 118.8 . . ? C29 C30 C25 121.3(4) . . ? C29 C30 C34 121.0(4) . . ? C25 C30 C34 117.5(4) . . ? C29 C30 Rh1 69.0(2) . . ? C25 C30 Rh1 80.9(2) . . ? C34 C30 Rh1 126.6(3) . . ? C26 C31 C32 112.2(3) . . ? C26 C31 C33 113.1(4) . . ? C32 C31 C33 110.6(4) . . ? C26 C31 H31A 106.8 . . ? C32 C31 H31A 106.8 . . ? C33 C31 H31A 106.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 C36 113.8(4) . . ? C30 C34 C35 110.7(4) . . ? C36 C34 C35 110.4(4) . . ? C30 C34 H34A 107.2 . . ? C36 C34 H34A 107.2 . . ? C35 C34 H34A 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C44 124.9(4) . . ? C38 C37 Rh1 71.2(2) . . ? C44 C37 Rh1 111.0(3) . . ? C38 C37 H37A 114.0 . . ? C44 C37 H37A 114.0 . . ? Rh1 C37 H37A 114.0 . . ? C37 C38 C39 122.6(5) . . ? C37 C38 Rh1 70.5(2) . . ? C39 C38 Rh1 113.2(3) . . ? C37 C38 H38A 114.3 . . ? C39 C38 H38A 114.3 . . ? Rh1 C38 H38A 114.3 . . ? C40 C39 C38 113.2(4) . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? C38 C39 H39B 108.9 . . ? H39A C39 H39B 107.8 . . ? C39 C40 C41 113.6(4) . . ? C39 C40 H40A 108.9 . . ? C41 C40 H40A 108.9 . . ? C39 C40 H40B 108.9 . . ? C41 C40 H40B 108.9 . . ? H40A C40 H40B 107.7 . . ? C42 C41 C40 124.8(4) . . ? C42 C41 Rh1 71.4(2) . . ? C40 C41 Rh1 112.0(3) . . ? C42 C41 H41A 113.7 . . ? C40 C41 H41A 113.7 . . ? Rh1 C41 H41A 113.7 . . ? C41 C42 C43 124.1(4) . . ? C41 C42 Rh1 70.4(3) . . ? C43 C42 Rh1 113.9(3) . . ? C41 C42 H42A 113.7 . . ? C43 C42 H42A 113.7 . . ? Rh1 C42 H42A 113.7 . . ? C44 C43 C42 113.4(4) . . ? C44 C43 H43A 108.9 . . ? C42 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? C42 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C43 C44 C37 113.6(4) . . ? C43 C44 H44A 108.9 . . ? C37 C44 H44A 108.9 . . ? C43 C44 H44B 108.9 . . ? C37 C44 H44B 108.9 . . ? H44A C44 H44B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Sc1 N1 C2 75.7(3) . . . . ? N2 Sc1 N1 C2 -26.1(3) . . . . ? N3 Sc1 N1 C2 -83.2(4) . . . . ? Cl1 Sc1 N1 C2 -173.7(3) . . . . ? N5 Sc1 N1 C11 -98.4(3) . . . . ? N2 Sc1 N1 C11 159.8(3) . . . . ? N3 Sc1 N1 C11 102.7(3) . . . . ? Cl1 Sc1 N1 C11 12.1(3) . . . . ? N5 Sc1 N2 C4 -84.2(4) . . . . ? N1 Sc1 N2 C4 30.2(3) . . . . ? N3 Sc1 N2 C4 173.6(4) . . . . ? Cl1 Sc1 N2 C4 115.4(3) . . . . ? N5 Sc1 N2 C6 85.8(3) . . . . ? N1 Sc1 N2 C6 -159.8(3) . . . . ? N3 Sc1 N2 C6 -16.4(3) . . . . ? Cl1 Sc1 N2 C6 -74.6(4) . . . . ? N5 Sc1 N3 C7 -63.8(3) . . . . ? N2 Sc1 N3 C7 36.5(2) . . . . ? N1 Sc1 N3 C7 96.5(3) . . . . ? Cl1 Sc1 N3 C7 -170.6(2) . . . . ? N5 Sc1 N3 C10 178.0(3) . . . . ? N2 Sc1 N3 C10 -81.7(3) . . . . ? N1 Sc1 N3 C10 -21.8(3) . . . . ? Cl1 Sc1 N3 C10 71.2(2) . . . . ? N5 Sc1 N3 C8 55.1(3) . . . . ? N2 Sc1 N3 C8 155.4(3) . . . . ? N1 Sc1 N3 C8 -144.6(3) . . . . ? Cl1 Sc1 N3 C8 -51.7(3) . . . . ? N2 Sc1 N5 C25 105(3) . . . . ? N1 Sc1 N5 C25 17(3) . . . . ? N3 Sc1 N5 C25 -178(100) . . . . ? Cl1 Sc1 N5 C25 -86(3) . . . . ? C2 N1 C11 C16 98.6(4) . . . . ? Sc1 N1 C11 C16 -86.8(4) . . . . ? C2 N1 C11 C12 -84.4(4) . . . . ? Sc1 N1 C11 C12 90.3(4) . . . . ? C16 C11 C12 C13 1.1(6) . . . . ? N1 C11 C12 C13 -175.9(3) . . . . ? C16 C11 C12 C20 -179.6(4) . . . . ? N1 C11 C12 C20 3.4(6) . . . . ? C11 C12 C13 C14 -0.9(6) . . . . ? C20 C12 C13 C14 179.8(4) . . . . ? C12 C13 C14 C15 -0.3(6) . . . . ? C13 C14 C15 C16 1.3(6) . . . . ? C14 C15 C16 C11 -1.1(6) . . . . ? C14 C15 C16 C17 179.1(4) . . . . ? C12 C11 C16 C15 -0.2(6) . . . . ? N1 C11 C16 C15 176.8(3) . . . . ? C12 C11 C16 C17 179.6(3) . . . . ? N1 C11 C16 C17 -3.3(5) . . . . ? C13 C12 C20 C21 -49.6(5) . . . . ? C11 C12 C20 C21 131.2(4) . . . . ? C13 C12 C20 C22 74.7(5) . . . . ? C11 C12 C20 C22 -104.6(4) . . . . ? C15 C16 C17 C19 -47.3(5) . . . . ? C11 C16 C17 C19 132.9(4) . . . . ? C15 C16 C17 C18 76.9(5) . . . . ? C11 C16 C17 C18 -102.9(5) . . . . ? C11 N1 C2 C3 -173.3(4) . . . . ? Sc1 N1 C2 C3 12.5(6) . . . . ? C11 N1 C2 C1 5.4(6) . . . . ? Sc1 N1 C2 C1 -168.8(3) . . . . ? N1 C2 C3 C4 12.4(7) . . . . ? C1 C2 C3 C4 -166.3(4) . . . . ? C6 N2 C4 C3 169.5(4) . . . . ? Sc1 N2 C4 C3 -20.5(6) . . . . ? C6 N2 C4 C5 -9.6(6) . . . . ? Sc1 N2 C4 C5 160.4(3) . . . . ? C2 C3 C4 N2 -8.4(7) . . . . ? C2 C3 C4 C5 170.7(4) . . . . ? C4 N2 C6 C7 163.6(4) . . . . ? Sc1 N2 C6 C7 -7.4(5) . . . . ? C10 N3 C7 C6 61.0(5) . . . . ? C8 N3 C7 C6 -176.1(4) . . . . ? Sc1 N3 C7 C6 -54.1(4) . . . . ? N2 C6 C7 N3 43.3(5) . . . . ? C7 N3 C8 C9 -70.0(5) . . . . ? C10 N3 C8 C9 53.8(5) . . . . ? Sc1 N3 C8 C9 175.3(3) . . . . ? C24 N4 C9 C8 53.6(6) . . . . ? C23 N4 C9 C8 -72.4(5) . . . . ? N3 C8 C9 N4 159.2(4) . . . . ? Sc1 N5 C25 C26 -48(3) . . . . ? Sc1 N5 C25 C30 134(3) . . . . ? Sc1 N5 C25 Rh1 -142(3) . . . . ? C41 Rh1 C25 N5 -110.6(6) . . . . ? C42 Rh1 C25 N5 90.1(6) . . . . ? C37 Rh1 C25 N5 14.9(4) . . . . ? C38 Rh1 C25 N5 -23.3(4) . . . . ? C28 Rh1 C25 N5 180.0(4) . . . . ? C29 Rh1 C25 N5 -142.5(4) . . . . ? C30 Rh1 C25 N5 -111.9(5) . . . . ? C27 Rh1 C25 N5 143.5(4) . . . . ? C26 Rh1 C25 N5 116.4(5) . . . . ? C41 Rh1 C25 C26 132.9(5) . . . . ? C42 Rh1 C25 C26 -26.4(5) . . . . ? C37 Rh1 C25 C26 -101.5(2) . . . . ? C38 Rh1 C25 C26 -139.7(2) . . . . ? C28 Rh1 C25 C26 63.5(2) . . . . ? C29 Rh1 C25 C26 101.1(2) . . . . ? C30 Rh1 C25 C26 131.6(3) . . . . ? C27 Rh1 C25 C26 27.1(2) . . . . ? C41 Rh1 C25 C30 1.3(6) . . . . ? C42 Rh1 C25 C30 -158.0(4) . . . . ? C37 Rh1 C25 C30 126.8(3) . . . . ? C38 Rh1 C25 C30 88.7(3) . . . . ? C28 Rh1 C25 C30 -68.1(2) . . . . ? C29 Rh1 C25 C30 -30.6(2) . . . . ? C27 Rh1 C25 C30 -104.6(3) . . . . ? C26 Rh1 C25 C30 -131.6(3) . . . . ? N5 C25 C26 C27 178.1(4) . . . . ? C30 C25 C26 C27 -4.2(5) . . . . ? Rh1 C25 C26 C27 -51.9(3) . . . . ? N5 C25 C26 C31 2.6(5) . . . . ? C30 C25 C26 C31 -179.7(3) . . . . ? Rh1 C25 C26 C31 132.6(3) . . . . ? N5 C25 C26 Rh1 -130.0(3) . . . . ? C30 C25 C26 Rh1 47.7(3) . . . . ? C41 Rh1 C26 C27 -16.3(5) . . . . ? C42 Rh1 C26 C27 -58.6(3) . . . . ? C37 Rh1 C26 C27 -144.6(3) . . . . ? C38 Rh1 C26 C27 -177.3(3) . . . . ? C28 Rh1 C26 C27 29.3(3) . . . . ? C29 Rh1 C26 C27 67.8(3) . . . . ? C30 Rh1 C26 C27 104.2(3) . . . . ? C25 Rh1 C26 C27 133.1(4) . . . . ? C41 Rh1 C26 C25 -149.4(4) . . . . ? C42 Rh1 C26 C25 168.3(2) . . . . ? C37 Rh1 C26 C25 82.3(2) . . . . ? C38 Rh1 C26 C25 49.6(3) . . . . ? C28 Rh1 C26 C25 -103.8(3) . . . . ? C29 Rh1 C26 C25 -65.3(2) . . . . ? C30 Rh1 C26 C25 -28.9(2) . . . . ? C27 Rh1 C26 C25 -133.1(4) . . . . ? C41 Rh1 C26 C31 95.1(5) . . . . ? C42 Rh1 C26 C31 52.8(5) . . . . ? C37 Rh1 C26 C31 -33.3(4) . . . . ? C38 Rh1 C26 C31 -65.9(5) . . . . ? C28 Rh1 C26 C31 140.7(5) . . . . ? C29 Rh1 C26 C31 179.2(4) . . . . ? C30 Rh1 C26 C31 -144.5(5) . . . . ? C27 Rh1 C26 C31 111.4(5) . . . . ? C25 Rh1 C26 C31 -115.5(5) . . . . ? C25 C26 C27 C28 3.4(6) . . . . ? C31 C26 C27 C28 178.8(4) . . . . ? Rh1 C26 C27 C28 -52.2(3) . . . . ? C25 C26 C27 Rh1 55.7(3) . . . . ? C31 C26 C27 Rh1 -128.9(3) . . . . ? C41 Rh1 C27 C26 171.9(3) . . . . ? C42 Rh1 C27 C26 134.2(3) . . . . ? C37 Rh1 C27 C26 44.1(3) . . . . ? C38 Rh1 C27 C26 5.5(5) . . . . ? C28 Rh1 C27 C26 -132.8(4) . . . . ? C29 Rh1 C27 C26 -99.3(3) . . . . ? C30 Rh1 C27 C26 -63.1(2) . . . . ? C25 Rh1 C27 C26 -27.9(2) . . . . ? C41 Rh1 C27 C28 -55.3(3) . . . . ? C42 Rh1 C27 C28 -92.9(3) . . . . ? C37 Rh1 C27 C28 177.0(3) . . . . ? C38 Rh1 C27 C28 138.4(4) . . . . ? C29 Rh1 C27 C28 33.5(3) . . . . ? C30 Rh1 C27 C28 69.8(3) . . . . ? C26 Rh1 C27 C28 132.8(4) . . . . ? C25 Rh1 C27 C28 105.0(3) . . . . ? C26 C27 C28 C29 -5.7(6) . . . . ? Rh1 C27 C28 C29 -64.3(3) . . . . ? C26 C27 C28 Rh1 58.6(4) . . . . ? C41 Rh1 C28 C29 -100.0(3) . . . . ? C42 Rh1 C28 C29 -138.6(3) . . . . ? C37 Rh1 C28 C29 116.8(5) . . . . ? C38 Rh1 C28 C29 -12.7(5) . . . . ? C30 Rh1 C28 C29 27.9(2) . . . . ? C27 Rh1 C28 C29 124.5(4) . . . . ? C26 Rh1 C28 C29 97.9(3) . . . . ? C25 Rh1 C28 C29 63.7(2) . . . . ? C41 Rh1 C28 C27 135.5(3) . . . . ? C42 Rh1 C28 C27 96.8(3) . . . . ? C37 Rh1 C28 C27 -7.7(7) . . . . ? C38 Rh1 C28 C27 -137.2(4) . . . . ? C29 Rh1 C28 C27 -124.5(4) . . . . ? C30 Rh1 C28 C27 -96.6(3) . . . . ? C26 Rh1 C28 C27 -26.6(2) . . . . ? C25 Rh1 C28 C27 -60.8(3) . . . . ? C27 C28 C29 C30 9.4(6) . . . . ? Rh1 C28 C29 C30 -56.9(4) . . . . ? C27 C28 C29 Rh1 66.3(3) . . . . ? C41 Rh1 C29 C30 -140.4(2) . . . . ? C42 Rh1 C29 C30 -171.8(2) . . . . ? C37 Rh1 C29 C30 -15.2(4) . . . . ? C38 Rh1 C29 C30 -53.4(3) . . . . ? C28 Rh1 C29 C30 132.5(4) . . . . ? C27 Rh1 C29 C30 99.4(3) . . . . ? C26 Rh1 C29 C30 65.3(2) . . . . ? C25 Rh1 C29 C30 30.3(2) . . . . ? C41 Rh1 C29 C28 87.1(3) . . . . ? C42 Rh1 C29 C28 55.7(3) . . . . ? C37 Rh1 C29 C28 -147.7(3) . . . . ? C38 Rh1 C29 C28 174.2(2) . . . . ? C30 Rh1 C29 C28 -132.5(4) . . . . ? C27 Rh1 C29 C28 -33.0(2) . . . . ? C26 Rh1 C29 C28 -67.1(2) . . . . ? C25 Rh1 C29 C28 -102.1(3) . . . . ? C28 C29 C30 C25 -10.8(6) . . . . ? Rh1 C29 C30 C25 -64.5(3) . . . . ? C28 C29 C30 C34 174.6(4) . . . . ? Rh1 C29 C30 C34 120.9(4) . . . . ? C28 C29 C30 Rh1 53.7(3) . . . . ? N5 C25 C30 C29 -174.5(4) . . . . ? C26 C25 C30 C29 7.9(5) . . . . ? Rh1 C25 C30 C29 58.6(3) . . . . ? N5 C25 C30 C34 0.3(6) . . . . ? C26 C25 C30 C34 -177.4(3) . . . . ? Rh1 C25 C30 C34 -126.7(4) . . . . ? N5 C25 C30 Rh1 126.9(3) . . . . ? C26 C25 C30 Rh1 -50.7(3) . . . . ? C41 Rh1 C30 C29 51.9(3) . . . . ? C42 Rh1 C30 C29 22.6(6) . . . . ? C37 Rh1 C30 C29 171.2(2) . . . . ? C38 Rh1 C30 C29 135.5(2) . . . . ? C28 Rh1 C30 C29 -29.3(2) . . . . ? C27 Rh1 C30 C29 -67.1(2) . . . . ? C26 Rh1 C30 C29 -100.4(3) . . . . ? C25 Rh1 C30 C29 -128.6(3) . . . . ? C41 Rh1 C30 C25 -179.5(2) . . . . ? C42 Rh1 C30 C25 151.2(5) . . . . ? C37 Rh1 C30 C25 -60.2(3) . . . . ? C38 Rh1 C30 C25 -95.9(2) . . . . ? C28 Rh1 C30 C25 99.3(3) . . . . ? C29 Rh1 C30 C25 128.6(3) . . . . ? C27 Rh1 C30 C25 61.5(2) . . . . ? C26 Rh1 C30 C25 28.2(2) . . . . ? C41 Rh1 C30 C34 -61.8(4) . . . . ? C42 Rh1 C30 C34 -91.1(6) . . . . ? C37 Rh1 C30 C34 57.5(4) . . . . ? C38 Rh1 C30 C34 21.8(4) . . . . ? C28 Rh1 C30 C34 -143.0(4) . . . . ? C29 Rh1 C30 C34 -113.7(4) . . . . ? C27 Rh1 C30 C34 179.2(4) . . . . ? C26 Rh1 C30 C34 145.9(4) . . . . ? C25 Rh1 C30 C34 117.7(4) . . . . ? C27 C26 C31 C32 93.6(5) . . . . ? C25 C26 C31 C32 -90.9(5) . . . . ? Rh1 C26 C31 C32 6.4(6) . . . . ? C27 C26 C31 C33 -32.4(5) . . . . ? C25 C26 C31 C33 143.1(4) . . . . ? Rh1 C26 C31 C33 -119.5(4) . . . . ? C29 C30 C34 C36 -29.8(6) . . . . ? C25 C30 C34 C36 155.4(4) . . . . ? Rh1 C30 C34 C36 55.9(5) . . . . ? C29 C30 C34 C35 95.2(5) . . . . ? C25 C30 C34 C35 -79.5(4) . . . . ? Rh1 C30 C34 C35 -179.1(3) . . . . ? C41 Rh1 C37 C38 66.7(3) . . . . ? C42 Rh1 C37 C38 101.9(3) . . . . ? C28 Rh1 C37 C38 -150.0(5) . . . . ? C29 Rh1 C37 C38 -60.0(4) . . . . ? C30 Rh1 C37 C38 -69.4(3) . . . . ? C27 Rh1 C37 C38 -155.6(3) . . . . ? C26 Rh1 C37 C38 -133.0(3) . . . . ? C25 Rh1 C37 C38 -99.3(3) . . . . ? C41 Rh1 C37 C44 -54.5(4) . . . . ? C42 Rh1 C37 C44 -19.3(3) . . . . ? C38 Rh1 C37 C44 -121.1(5) . . . . ? C28 Rh1 C37 C44 88.9(6) . . . . ? C29 Rh1 C37 C44 178.9(3) . . . . ? C30 Rh1 C37 C44 169.4(3) . . . . ? C27 Rh1 C37 C44 83.3(4) . . . . ? C26 Rh1 C37 C44 105.9(3) . . . . ? C25 Rh1 C37 C44 139.6(3) . . . . ? C44 C37 C38 C39 -2.6(7) . . . . ? Rh1 C37 C38 C39 -105.6(4) . . . . ? C44 C37 C38 Rh1 103.0(4) . . . . ? C41 Rh1 C38 C37 -112.7(3) . . . . ? C42 Rh1 C38 C37 -75.4(3) . . . . ? C28 Rh1 C38 C37 156.4(4) . . . . ? C29 Rh1 C38 C37 147.6(3) . . . . ? C30 Rh1 C38 C37 119.9(3) . . . . ? C27 Rh1 C38 C37 55.7(5) . . . . ? C26 Rh1 C38 C37 59.2(3) . . . . ? C25 Rh1 C38 C37 84.7(3) . . . . ? C41 Rh1 C38 C39 5.4(4) . . . . ? C42 Rh1 C38 C39 42.7(4) . . . . ? C37 Rh1 C38 C39 118.1(5) . . . . ? C28 Rh1 C38 C39 -85.5(6) . . . . ? C29 Rh1 C38 C39 -94.3(4) . . . . ? C30 Rh1 C38 C39 -122.0(4) . . . . ? C27 Rh1 C38 C39 173.8(4) . . . . ? C26 Rh1 C38 C39 177.3(3) . . . . ? C25 Rh1 C38 C39 -157.2(4) . . . . ? C37 C38 C39 C40 90.1(6) . . . . ? Rh1 C38 C39 C40 9.1(6) . . . . ? C38 C39 C40 C41 -25.1(7) . . . . ? C39 C40 C41 C42 -52.6(7) . . . . ? C39 C40 C41 Rh1 29.5(6) . . . . ? C37 Rh1 C41 C42 67.0(3) . . . . ? C38 Rh1 C41 C42 102.2(3) . . . . ? C28 Rh1 C41 C42 -101.8(3) . . . . ? C29 Rh1 C41 C42 -139.2(3) . . . . ? C30 Rh1 C41 C42 -166.9(2) . . . . ? C27 Rh1 C41 C42 -72.2(3) . . . . ? C26 Rh1 C41 C42 -61.8(5) . . . . ? C25 Rh1 C41 C42 -167.8(4) . . . . ? C42 Rh1 C41 C40 -120.9(5) . . . . ? C37 Rh1 C41 C40 -53.9(4) . . . . ? C38 Rh1 C41 C40 -18.7(4) . . . . ? C28 Rh1 C41 C40 137.3(3) . . . . ? C29 Rh1 C41 C40 99.9(4) . . . . ? C30 Rh1 C41 C40 72.2(4) . . . . ? C27 Rh1 C41 C40 166.9(3) . . . . ? C26 Rh1 C41 C40 177.3(3) . . . . ? C25 Rh1 C41 C40 71.3(6) . . . . ? C40 C41 C42 C43 -1.9(7) . . . . ? Rh1 C41 C42 C43 -106.2(4) . . . . ? C40 C41 C42 Rh1 104.3(5) . . . . ? C37 Rh1 C42 C41 -112.4(3) . . . . ? C38 Rh1 C42 C41 -75.0(3) . . . . ? C28 Rh1 C42 C41 86.0(3) . . . . ? C29 Rh1 C42 C41 55.2(3) . . . . ? C30 Rh1 C42 C41 38.6(7) . . . . ? C27 Rh1 C42 C41 123.7(3) . . . . ? C26 Rh1 C42 C41 152.4(2) . . . . ? C25 Rh1 C42 C41 170.2(3) . . . . ? C41 Rh1 C42 C43 119.6(5) . . . . ? C37 Rh1 C42 C43 7.2(3) . . . . ? C38 Rh1 C42 C43 44.5(4) . . . . ? C28 Rh1 C42 C43 -154.5(3) . . . . ? C29 Rh1 C42 C43 174.7(3) . . . . ? C30 Rh1 C42 C43 158.1(4) . . . . ? C27 Rh1 C42 C43 -116.8(3) . . . . ? C26 Rh1 C42 C43 -88.0(4) . . . . ? C25 Rh1 C42 C43 -70.2(6) . . . . ? C41 C42 C43 C44 88.5(6) . . . . ? Rh1 C42 C43 C44 6.7(5) . . . . ? C42 C43 C44 C37 -23.3(6) . . . . ? C38 C37 C44 C43 -52.4(6) . . . . ? Rh1 C37 C44 C43 28.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.616 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.128 #===END data_mo_dm11164_0m _database_code_depnum_ccdc_archive 'CCDC 851602' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H70 Cl Ir N5 Sc' _chemical_formula_weight 941.66 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 23.527(3) _cell_length_b 12.3238(13) _cell_length_c 15.6154(16) _cell_angle_alpha 90.00 _cell_angle_beta 105.940(2) _cell_angle_gamma 90.00 _cell_volume 4353.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 8394 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 29.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 3.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3907 _exptl_absorpt_correction_T_max 0.6369 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15211 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8417 _reflns_number_gt 7851 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Atoms C24 and C24' are disorder terminal atoms of ligand, of which occupancy were set as 0.5. The distance between C24 and N4 was fixed at 1.48 angstrom for refinement. Atoms (N4, C24, C24') and (C4, C5, C6 and C7) atomic displacement parameters were restrained to be the same with su of 0.01 (SIMU instruction). ; _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(5) _chemical_absolute_configuration ad _refine_ls_number_reflns 8417 _refine_ls_number_parameters 492 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.005 _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 Ir1 Ir 1.003214(11) 0.558719(11) 0.752409(12) 0.02137(5) Uani 1 1 d . . . Sc1 Sc 0.89309(4) 0.15027(7) 0.62125(6) 0.02283(18) Uani 1 1 d . . . Cl1 Cl 0.91392(6) -0.00681(11) 0.71953(10) 0.0425(3) Uani 1 1 d . . . N1 N 0.79949(17) 0.1630(3) 0.6240(2) 0.0214(8) Uani 1 1 d . . . N2 N 0.8567(2) 0.1941(4) 0.4811(3) 0.0441(12) Uani 1 1 d . . . N3 N 0.9598(3) 0.0814(5) 0.5492(4) 0.0603(16) Uani 1 1 d . A . N4 N 1.1077(3) 0.0963(4) 0.5642(4) 0.0562(15) Uani 1 1 d DU . . N5 N 0.93649(19) 0.2755(4) 0.6801(3) 0.0225(9) Uani 1 1 d . . . C1 C 0.7014(3) 0.2482(5) 0.5905(4) 0.0316(13) Uani 1 1 d . . . H1A H 0.6797 0.1803 0.5906 0.047 Uiso 1 1 calc R . . H1B H 0.6776 0.2974 0.5455 0.047 Uiso 1 1 calc R . . H1C H 0.7096 0.2823 0.6494 0.047 Uiso 1 1 calc R . . C2 C 0.7589(2) 0.2243(4) 0.5691(3) 0.0242(10) Uani 1 1 d . . . C3 C 0.7647(3) 0.2688(4) 0.4892(3) 0.0310(12) Uani 1 1 d . . . H3 H 0.7348 0.3187 0.4603 0.037 Uiso 1 1 calc R . . C4 C 0.8088(3) 0.2494(6) 0.4468(4) 0.0403(17) Uani 1 1 d U . . C5 C 0.7968(3) 0.3002(6) 0.3539(3) 0.0543(18) Uani 1 1 d U . . H5A H 0.8268 0.3556 0.3543 0.081 Uiso 1 1 calc R . . H5B H 0.7576 0.3336 0.3375 0.081 Uiso 1 1 calc R . . H5C H 0.7986 0.2437 0.3104 0.081 Uiso 1 1 calc R . . C6 C 0.8971(4) 0.1802(8) 0.4245(5) 0.079(2) Uani 1 1 d U . . H6A H 0.8970 0.2465 0.3887 0.095 Uiso 1 1 calc R . . H6B H 0.8840 0.1185 0.3832 0.095 Uiso 1 1 calc R . . C7 C 0.9609(4) 0.1583(7) 0.4860(6) 0.081(2) Uani 1 1 d U . . H7A H 0.9865 0.1330 0.4493 0.097 Uiso 1 1 calc R . . H7B H 0.9777 0.2266 0.5158 0.097 Uiso 1 1 calc R . . C8 C 1.0172(3) 0.0478(5) 0.6098(5) 0.0473(15) Uani 1 1 d . . . H8A H 1.0093 -0.0128 0.6466 0.057 Uiso 1 1 calc R A . H8B H 1.0322 0.1091 0.6508 0.057 Uiso 1 1 calc R . . C9 C 1.0672(3) 0.0122(6) 0.5716(5) 0.0547(18) Uani 1 1 d . A . H9A H 1.0897 -0.0463 0.6097 0.066 Uiso 1 1 calc R . . H9B H 1.0497 -0.0190 0.5117 0.066 Uiso 1 1 calc R . . C10 C 0.9310(4) -0.0225(7) 0.4990(7) 0.082(3) Uani 1 1 d . . . H10A H 0.8893 -0.0083 0.4690 0.123 Uiso 1 1 calc R A . H10B H 0.9339 -0.0820 0.5416 0.123 Uiso 1 1 calc R . . H10C H 0.9516 -0.0427 0.4546 0.123 Uiso 1 1 calc R . . C11 C 0.78190(19) 0.1088(4) 0.6944(3) 0.0206(9) Uani 1 1 d . . . C12 C 0.79211(19) 0.1553(4) 0.7794(3) 0.0217(9) Uani 1 1 d . . . C13 C 0.7749(2) 0.0979(4) 0.8450(3) 0.0248(9) Uani 1 1 d . . . H13 H 0.7821 0.1286 0.9028 0.030 Uiso 1 1 calc R . . C14 C 0.7479(2) -0.0023(4) 0.8283(3) 0.0258(10) Uani 1 1 d . . . H14 H 0.7363 -0.0400 0.8739 0.031 Uiso 1 1 calc R . . C15 C 0.7379(2) -0.0469(4) 0.7443(3) 0.0275(10) Uani 1 1 d . . . H15 H 0.7185 -0.1151 0.7323 0.033 Uiso 1 1 calc R . . C16 C 0.7556(2) 0.0057(4) 0.6766(3) 0.0238(9) Uani 1 1 d . . . C17 C 0.7456(3) -0.0499(4) 0.5874(3) 0.0328(12) Uani 1 1 d . . . H17 H 0.7640 -0.0036 0.5496 0.039 Uiso 1 1 calc R . . C18 C 0.6806(3) -0.0623(5) 0.5388(4) 0.0530(18) Uani 1 1 d . . . H18A H 0.6602 -0.0984 0.5778 0.080 Uiso 1 1 calc R . . H18B H 0.6765 -0.1060 0.4850 0.080 Uiso 1 1 calc R . . H18C H 0.6632 0.0095 0.5222 0.080 Uiso 1 1 calc R . . C19 C 0.7769(3) -0.1611(4) 0.5983(4) 0.0378(13) Uani 1 1 d . . . H19A H 0.8191 -0.1513 0.6272 0.057 Uiso 1 1 calc R . . H19B H 0.7716 -0.1943 0.5397 0.057 Uiso 1 1 calc R . . H19C H 0.7597 -0.2084 0.6351 0.057 Uiso 1 1 calc R . . C20 C 0.8211(2) 0.2665(4) 0.8017(3) 0.0272(10) Uani 1 1 d . . . H20 H 0.8303 0.2955 0.7473 0.033 Uiso 1 1 calc R . . C21 C 0.7796(3) 0.3478(4) 0.8300(4) 0.0412(13) Uani 1 1 d . . . H21A H 0.7691 0.3198 0.8824 0.062 Uiso 1 1 calc R . . H21B H 0.7436 0.3574 0.7810 0.062 Uiso 1 1 calc R . . H21C H 0.7997 0.4178 0.8445 0.062 Uiso 1 1 calc R . . C22 C 0.8789(2) 0.2562(5) 0.8755(3) 0.0386(13) Uani 1 1 d . . . H22A H 0.8703 0.2356 0.9312 0.058 Uiso 1 1 calc R . . H22B H 0.8997 0.3258 0.8834 0.058 Uiso 1 1 calc R . . H22C H 0.9037 0.2004 0.8591 0.058 Uiso 1 1 calc R . . C23 C 1.1446(4) 0.0641(6) 0.5074(6) 0.069(2) Uani 1 1 d . A . H23A H 1.1684 0.0009 0.5334 0.104 Uiso 1 1 calc R . . H23B H 1.1708 0.1243 0.5026 0.104 Uiso 1 1 calc R . . H23C H 1.1194 0.0455 0.4481 0.104 Uiso 1 1 calc R . . C24 C 1.1434(13) 0.1423(16) 0.6474(14) 0.079(6) Uani 0.50 1 d PDU A 1 H24A H 1.1454 0.2213 0.6414 0.119 Uiso 0.50 1 calc PR A 1 H24B H 1.1834 0.1119 0.6613 0.119 Uiso 0.50 1 calc PR A 1 H24C H 1.1256 0.1248 0.6955 0.119 Uiso 0.50 1 calc PR A 1 C24' C 1.1474(13) 0.1013(19) 0.6571(14) 0.081(6) Uani 0.50 1 d PDU A 2 H24F H 1.1637 0.0290 0.6752 0.121 Uiso 0.50 1 calc PR A 2 H24D H 1.1248 0.1259 0.6976 0.121 Uiso 0.50 1 calc PR A 2 H24E H 1.1798 0.1521 0.6593 0.121 Uiso 0.50 1 calc PR A 2 C25 C 0.9501(2) 0.3626(4) 0.7265(3) 0.0216(9) Uani 1 1 d . . . C26 C 1.0074(2) 0.3783(4) 0.7956(3) 0.0242(9) Uani 1 1 d . . . C27 C 1.0110(2) 0.4476(4) 0.8690(3) 0.0306(11) Uani 1 1 d . . . H27A H 1.0478 0.4485 0.9197 0.037 Uiso 1 1 calc R . . C28 C 0.9662(3) 0.5217(5) 0.8673(4) 0.0324(12) Uani 1 1 d . . . H28A H 0.9702 0.5752 0.9168 0.039 Uiso 1 1 calc R . . C29 C 0.9188(3) 0.5318(5) 0.7859(4) 0.0309(11) Uani 1 1 d . . . H29A H 0.8903 0.5935 0.7797 0.037 Uiso 1 1 calc R . . C30 C 0.9139(2) 0.4617(3) 0.7132(3) 0.0218(9) Uani 1 1 d . . . C31 C 0.8633(2) 0.4683(4) 0.6293(3) 0.0286(11) Uani 1 1 d . . . H31 H 0.8421 0.3972 0.6235 0.034 Uiso 1 1 calc R . . C32 C 0.8177(3) 0.5562(5) 0.6322(5) 0.0491(16) Uani 1 1 d . . . H32A H 0.8015 0.5426 0.6826 0.074 Uiso 1 1 calc R . . H32B H 0.7857 0.5546 0.5767 0.074 Uiso 1 1 calc R . . H32C H 0.8368 0.6276 0.6391 0.074 Uiso 1 1 calc R . . C33 C 0.8853(3) 0.4800(5) 0.5470(3) 0.0383(13) Uani 1 1 d . . . H33A H 0.9024 0.5523 0.5463 0.057 Uiso 1 1 calc R . . H33B H 0.8521 0.4704 0.4936 0.057 Uiso 1 1 calc R . . H33C H 0.9154 0.4248 0.5480 0.057 Uiso 1 1 calc R . . C34 C 1.0545(2) 0.2911(5) 0.8001(4) 0.0270(12) Uani 1 1 d . . . H34 H 1.0493 0.2639 0.7382 0.032 Uiso 1 1 calc R . . C35 C 1.0419(3) 0.1946(4) 0.8561(4) 0.0444(14) Uani 1 1 d . . . H35A H 1.0450 0.2193 0.9169 0.067 Uiso 1 1 calc R . . H35B H 1.0708 0.1369 0.8577 0.067 Uiso 1 1 calc R . . H35C H 1.0020 0.1669 0.8290 0.067 Uiso 1 1 calc R . . C36 C 1.1183(2) 0.3285(5) 0.8354(4) 0.0458(14) Uani 1 1 d . . . H36A H 1.1278 0.3788 0.7927 0.069 Uiso 1 1 calc R . . H36B H 1.1446 0.2655 0.8435 0.069 Uiso 1 1 calc R . . H36C H 1.1235 0.3653 0.8927 0.069 Uiso 1 1 calc R . . C37 C 1.0049(5) 0.7310(5) 0.7659(7) 0.056(2) Uani 1 1 d . . . H37A H 0.9760 0.7584 0.7973 0.068 Uiso 1 1 calc R . . C38 C 0.9773(3) 0.7004(4) 0.6753(5) 0.0481(16) Uani 1 1 d . . . H38A H 0.9336 0.7128 0.6553 0.058 Uiso 1 1 calc R . . C39 C 1.0091(3) 0.7191(6) 0.6040(4) 0.0589(18) Uani 1 1 d . . . H39A H 1.0371 0.7804 0.6216 0.071 Uiso 1 1 calc R . . H39B H 0.9800 0.7381 0.5470 0.071 Uiso 1 1 calc R . . C40 C 1.0436(3) 0.6143(7) 0.5914(4) 0.063(2) Uani 1 1 d . . . H40A H 1.0182 0.5699 0.5430 0.076 Uiso 1 1 calc R . . H40B H 1.0792 0.6354 0.5733 0.076 Uiso 1 1 calc R . . C41 C 1.0613(4) 0.5496(5) 0.6714(6) 0.052(2) Uani 1 1 d . . . H41A H 1.0740 0.4742 0.6618 0.062 Uiso 1 1 calc R . . C42 C 1.0917(2) 0.5957(6) 0.7587(5) 0.0468(15) Uani 1 1 d . . . H42A H 1.1208 0.5448 0.7974 0.056 Uiso 1 1 calc R . . C43 C 1.1103(3) 0.7100(5) 0.7703(4) 0.0508(16) Uani 1 1 d . . . H43A H 1.1146 0.7391 0.7133 0.061 Uiso 1 1 calc R . . H43B H 1.1492 0.7154 0.8153 0.061 Uiso 1 1 calc R . . C44 C 1.0640(3) 0.7777(5) 0.8008(5) 0.0599(19) Uani 1 1 d . . . H44A H 1.0744 0.7793 0.8667 0.072 Uiso 1 1 calc R . . H44B H 1.0641 0.8533 0.7793 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01978(7) 0.02294(7) 0.02218(7) -0.00334(12) 0.00707(5) -0.00142(12) Sc1 0.0254(4) 0.0225(4) 0.0240(4) -0.0039(3) 0.0125(3) -0.0054(3) Cl1 0.0360(7) 0.0339(7) 0.0612(9) 0.0141(6) 0.0195(6) 0.0023(6) N1 0.028(2) 0.0228(18) 0.0155(17) 0.0003(14) 0.0105(15) -0.0049(15) N2 0.039(3) 0.076(4) 0.023(2) -0.003(2) 0.018(2) -0.008(3) N3 0.075(4) 0.079(4) 0.039(3) -0.008(3) 0.036(3) 0.030(3) N4 0.055(3) 0.034(3) 0.091(4) -0.016(3) 0.040(3) -0.008(2) N5 0.019(2) 0.025(2) 0.022(2) -0.0031(17) 0.0028(17) -0.0024(17) C1 0.026(3) 0.031(3) 0.035(3) 0.005(2) 0.004(2) 0.003(2) C2 0.031(3) 0.023(2) 0.018(2) -0.0002(19) 0.005(2) -0.0063(19) C3 0.044(3) 0.027(3) 0.019(3) 0.003(2) 0.003(2) -0.008(2) C4 0.049(4) 0.052(4) 0.019(3) -0.003(2) 0.007(3) -0.032(3) C5 0.077(5) 0.069(4) 0.018(3) 0.001(2) 0.014(3) -0.033(3) C6 0.079(5) 0.124(6) 0.049(4) 0.011(4) 0.045(4) 0.019(5) C7 0.079(4) 0.095(4) 0.082(4) -0.004(3) 0.048(3) 0.009(3) C8 0.038(3) 0.046(3) 0.064(4) -0.023(3) 0.023(3) -0.009(3) C9 0.040(3) 0.059(4) 0.077(5) -0.025(4) 0.034(3) -0.011(3) C10 0.044(4) 0.101(6) 0.096(7) -0.051(5) 0.011(4) 0.004(4) C11 0.021(2) 0.022(2) 0.021(2) 0.0041(17) 0.0086(17) 0.0021(17) C12 0.017(2) 0.030(2) 0.019(2) 0.0010(17) 0.0068(17) 0.0002(18) C13 0.024(2) 0.031(2) 0.021(2) -0.0017(18) 0.0090(18) -0.0011(19) C14 0.029(2) 0.031(3) 0.022(2) 0.0084(18) 0.0147(19) 0.000(2) C15 0.038(3) 0.023(2) 0.026(2) 0.0036(18) 0.016(2) -0.0066(19) C16 0.031(2) 0.023(2) 0.018(2) 0.0007(17) 0.0092(18) -0.0003(19) C17 0.054(3) 0.023(2) 0.024(2) -0.0003(18) 0.015(2) -0.006(2) C18 0.067(5) 0.050(4) 0.031(3) -0.007(3) -0.006(3) 0.004(3) C19 0.061(4) 0.025(3) 0.033(3) -0.005(2) 0.022(3) -0.005(2) C20 0.032(3) 0.032(3) 0.018(2) -0.0016(18) 0.0076(19) -0.007(2) C21 0.053(4) 0.030(3) 0.039(3) -0.012(2) 0.011(3) -0.003(2) C22 0.033(3) 0.056(3) 0.027(2) -0.006(2) 0.007(2) -0.020(3) C23 0.067(5) 0.067(5) 0.086(6) 0.007(4) 0.042(5) 0.004(4) C24 0.071(9) 0.050(11) 0.126(11) -0.042(9) 0.040(8) -0.035(10) C24' 0.068(9) 0.063(12) 0.119(11) -0.046(10) 0.039(9) -0.012(11) C25 0.021(2) 0.022(2) 0.024(2) 0.0027(18) 0.0087(18) -0.0039(18) C26 0.026(2) 0.023(2) 0.024(2) 0.0005(18) 0.0076(19) 0.0017(19) C27 0.030(3) 0.036(3) 0.023(2) 0.0031(19) 0.002(2) -0.006(2) C28 0.041(3) 0.032(3) 0.031(3) -0.003(2) 0.020(3) 0.004(3) C29 0.027(3) 0.034(3) 0.038(3) -0.002(2) 0.019(2) 0.000(2) C30 0.016(2) 0.025(2) 0.026(2) -0.0018(17) 0.0078(18) -0.0009(17) C31 0.018(2) 0.026(2) 0.037(3) 0.0013(19) 0.001(2) -0.0006(18) C32 0.027(3) 0.053(4) 0.062(4) 0.003(3) 0.002(3) 0.014(3) C33 0.043(3) 0.039(3) 0.026(3) 0.010(2) -0.001(2) -0.006(2) C34 0.018(3) 0.029(3) 0.027(3) 0.003(2) -0.004(2) 0.008(2) C35 0.041(3) 0.031(3) 0.057(4) 0.016(2) 0.005(3) 0.002(2) C36 0.025(3) 0.041(3) 0.064(4) 0.000(3) 0.000(3) 0.002(2) C37 0.047(3) 0.042(3) 0.085(7) -0.013(4) 0.027(4) -0.003(5) C38 0.032(3) 0.032(3) 0.070(4) 0.015(3) -0.002(3) 0.001(2) C39 0.054(4) 0.068(4) 0.045(4) 0.016(3) -0.003(3) -0.011(3) C40 0.063(5) 0.085(5) 0.047(4) -0.012(4) 0.024(3) -0.032(4) C41 0.052(5) 0.042(4) 0.078(6) -0.016(3) 0.046(5) -0.011(3) C42 0.019(3) 0.056(4) 0.061(4) 0.015(3) 0.004(3) 0.003(3) C43 0.039(3) 0.060(4) 0.048(3) 0.008(3) 0.003(3) -0.012(3) C44 0.086(5) 0.050(4) 0.054(4) -0.020(3) 0.036(4) -0.029(4) _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 Ir1 C41 2.105(7) . ? Ir1 C42 2.107(6) . ? Ir1 C38 2.113(5) . ? Ir1 C37 2.133(6) . ? Ir1 C29 2.213(5) . ? Ir1 C28 2.245(6) . ? Ir1 C27 2.245(5) . ? Ir1 C26 2.317(4) . ? Ir1 C30 2.347(4) . ? Sc1 N5 1.937(4) . ? Sc1 N2 2.188(5) . ? Sc1 N1 2.220(4) . ? Sc1 N3 2.328(5) . ? Sc1 Cl1 2.4352(15) . ? N1 C2 1.329(6) . ? N1 C11 1.441(5) . ? N2 C4 1.299(9) . ? N2 C6 1.475(8) . ? N3 C7 1.373(10) . ? N3 C8 1.480(9) . ? N3 C10 1.558(10) . ? N4 C9 1.434(9) . ? N4 C24 1.455(16) . ? N4 C23 1.456(10) . ? N4 C24' 1.496(16) . ? N5 C25 1.286(6) . ? C1 C2 1.508(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.404(7) . ? C3 C4 1.396(9) . ? C3 H3 0.9500 . ? C4 C5 1.534(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.567(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.522(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.404(6) . ? C11 C16 1.407(6) . ? C12 C13 1.393(6) . ? C12 C20 1.528(6) . ? C13 C14 1.381(7) . ? C13 H13 0.9500 . ? C14 C15 1.381(7) . ? C14 H14 0.9500 . ? C15 C16 1.398(6) . ? C15 H15 0.9500 . ? C16 C17 1.512(6) . ? C17 C18 1.516(9) . ? C17 C19 1.542(7) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.527(7) . ? C20 C21 1.545(7) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24' H24F 0.9800 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C25 C30 1.471(6) . ? C25 C26 1.489(6) . ? C26 C27 1.413(7) . ? C26 C34 1.531(7) . ? C27 C28 1.390(8) . ? C27 H27A 1.0000 . ? C28 C29 1.448(8) . ? C28 H28A 1.0000 . ? C29 C30 1.407(7) . ? C29 H29A 1.0000 . ? C30 C31 1.511(6) . ? C31 C33 1.517(8) . ? C31 C32 1.535(7) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.521(7) . ? C34 C35 1.551(8) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.435(12) . ? C37 C44 1.464(12) . ? C37 H37A 1.0000 . ? C38 C39 1.521(10) . ? C38 H38A 1.0000 . ? C39 C40 1.566(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.444(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.468(11) . ? C41 H41A 1.0000 . ? C42 C43 1.472(9) . ? C42 H42A 1.0000 . ? C43 C44 1.549(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Ir1 C42 40.8(3) . . ? C41 Ir1 C38 80.5(3) . . ? C42 Ir1 C38 88.5(2) . . ? C41 Ir1 C37 96.6(3) . . ? C42 Ir1 C37 77.8(4) . . ? C38 Ir1 C37 39.5(3) . . ? C41 Ir1 C29 155.1(2) . . ? C42 Ir1 C29 163.9(2) . . ? C38 Ir1 C29 96.9(2) . . ? C37 Ir1 C29 96.9(3) . . ? C41 Ir1 C28 158.0(3) . . ? C42 Ir1 C28 127.0(2) . . ? C38 Ir1 C28 120.5(3) . . ? C37 Ir1 C28 97.1(3) . . ? C29 Ir1 C28 37.9(2) . . ? C41 Ir1 C27 122.2(3) . . ? C42 Ir1 C27 103.6(2) . . ? C38 Ir1 C27 155.8(2) . . ? C37 Ir1 C27 122.2(3) . . ? C29 Ir1 C27 66.2(2) . . ? C28 Ir1 C27 36.1(2) . . ? C41 Ir1 C26 98.1(2) . . ? C42 Ir1 C26 103.4(2) . . ? C38 Ir1 C26 160.2(2) . . ? C37 Ir1 C26 158.2(3) . . ? C29 Ir1 C26 75.92(19) . . ? C28 Ir1 C26 64.37(19) . . ? C27 Ir1 C26 36.03(17) . . ? C41 Ir1 C30 119.9(3) . . ? C42 Ir1 C30 157.6(2) . . ? C38 Ir1 C30 100.1(2) . . ? C37 Ir1 C30 121.6(3) . . ? C29 Ir1 C30 35.77(19) . . ? C28 Ir1 C30 65.76(19) . . ? C27 Ir1 C30 76.64(17) . . ? C26 Ir1 C30 63.30(16) . . ? N5 Sc1 N2 106.78(19) . . ? N5 Sc1 N1 109.31(17) . . ? N2 Sc1 N1 83.31(16) . . ? N5 Sc1 N3 100.5(2) . . ? N2 Sc1 N3 74.8(2) . . ? N1 Sc1 N3 147.07(19) . . ? N5 Sc1 Cl1 110.22(13) . . ? N2 Sc1 Cl1 141.48(15) . . ? N1 Sc1 Cl1 94.20(10) . . ? N3 Sc1 Cl1 88.23(16) . . ? C2 N1 C11 116.7(4) . . ? C2 N1 Sc1 124.7(3) . . ? C11 N1 Sc1 118.4(3) . . ? C4 N2 C6 116.3(5) . . ? C4 N2 Sc1 126.8(4) . . ? C6 N2 Sc1 115.5(4) . . ? C7 N3 C8 117.4(7) . . ? C7 N3 C10 107.3(7) . . ? C8 N3 C10 106.7(5) . . ? C7 N3 Sc1 104.1(4) . . ? C8 N3 Sc1 114.3(4) . . ? C10 N3 Sc1 106.6(5) . . ? C9 N4 C24 116.3(13) . . ? C9 N4 C23 111.8(5) . . ? C24 N4 C23 110.7(15) . . ? C9 N4 C24' 101.7(13) . . ? C24 N4 C24' 20.6(12) . . ? C23 N4 C24' 106.4(14) . . ? C25 N5 Sc1 161.8(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.5(5) . . ? N1 C2 C1 119.9(4) . . ? C3 C2 C1 115.7(5) . . ? C4 C3 C2 128.4(5) . . ? C4 C3 H3 115.8 . . ? C2 C3 H3 115.8 . . ? N2 C4 C3 124.6(5) . . ? N2 C4 C5 121.1(6) . . ? C3 C4 C5 114.3(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 108.6(6) . . ? N2 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? N2 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N3 C7 C6 110.9(7) . . ? N3 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? N3 C8 C9 119.8(6) . . ? N3 C8 H8A 107.4 . . ? C9 C8 H8A 107.4 . . ? N3 C8 H8B 107.4 . . ? C9 C8 H8B 107.4 . . ? H8A C8 H8B 106.9 . . ? N4 C9 C8 115.1(6) . . ? N4 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? N4 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 120.5(4) . . ? C12 C11 N1 121.4(4) . . ? C16 C11 N1 118.1(4) . . ? C13 C12 C11 118.6(4) . . ? C13 C12 C20 119.3(4) . . ? C11 C12 C20 122.1(4) . . ? C14 C13 C12 121.8(4) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 119.0(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C16 121.7(4) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C11 118.4(4) . . ? C15 C16 C17 118.9(4) . . ? C11 C16 C17 122.7(4) . . ? C16 C17 C18 112.8(5) . . ? C16 C17 C19 110.6(4) . . ? C18 C17 C19 110.5(4) . . ? C16 C17 H17 107.6 . . ? C18 C17 H17 107.6 . . ? C19 C17 H17 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C12 C20 C22 110.2(4) . . ? C12 C20 C21 111.7(4) . . ? C22 C20 C21 109.9(4) . . ? C12 C20 H20 108.3 . . ? C22 C20 H20 108.3 . . ? C21 C20 H20 108.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? N4 C24' H24F 109.5 . . ? N4 C24' H24D 109.5 . . ? H24F C24' H24D 109.5 . . ? N4 C24' H24E 109.5 . . ? H24F C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? N5 C25 C30 124.6(4) . . ? N5 C25 C26 123.6(4) . . ? C30 C25 C26 111.6(4) . . ? C27 C26 C25 120.5(4) . . ? C27 C26 C34 120.3(4) . . ? C25 C26 C34 116.2(4) . . ? C27 C26 Ir1 69.2(3) . . ? C25 C26 Ir1 87.5(3) . . ? C34 C26 Ir1 131.2(4) . . ? C28 C27 C26 120.3(5) . . ? C28 C27 Ir1 72.0(3) . . ? C26 C27 Ir1 74.8(3) . . ? C28 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? Ir1 C27 H27A 119.7 . . ? C27 C28 C29 118.1(5) . . ? C27 C28 Ir1 72.0(3) . . ? C29 C28 Ir1 69.9(3) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? Ir1 C28 H28A 120.5 . . ? C30 C29 C28 121.9(5) . . ? C30 C29 Ir1 77.3(3) . . ? C28 C29 Ir1 72.2(3) . . ? C30 C29 H29A 119.0 . . ? C28 C29 H29A 119.0 . . ? Ir1 C29 H29A 119.0 . . ? C29 C30 C25 118.7(4) . . ? C29 C30 C31 122.5(4) . . ? C25 C30 C31 117.0(4) . . ? C29 C30 Ir1 66.9(3) . . ? C25 C30 Ir1 86.8(3) . . ? C31 C30 Ir1 129.4(3) . . ? C30 C31 C33 111.7(4) . . ? C30 C31 C32 113.8(4) . . ? C33 C31 C32 111.2(5) . . ? C30 C31 H31 106.6 . . ? C33 C31 H31 106.6 . . ? C32 C31 H31 106.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 C26 115.7(5) . . ? C36 C34 C35 110.5(4) . . ? C26 C34 C35 108.5(5) . . ? C36 C34 H34 107.3 . . ? C26 C34 H34 107.3 . . ? C35 C34 H34 107.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C44 126.7(9) . . ? C38 C37 Ir1 69.5(3) . . ? C44 C37 Ir1 114.7(6) . . ? C38 C37 H37A 112.8 . . ? C44 C37 H37A 112.8 . . ? Ir1 C37 H37A 112.8 . . ? C37 C38 C39 120.1(6) . . ? C37 C38 Ir1 71.0(4) . . ? C39 C38 Ir1 114.8(4) . . ? C37 C38 H38A 114.6 . . ? C39 C38 H38A 114.6 . . ? Ir1 C38 H38A 114.6 . . ? C38 C39 C40 110.0(5) . . ? C38 C39 H39A 109.7 . . ? C40 C39 H39A 109.7 . . ? C38 C39 H39B 109.7 . . ? C40 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C41 C40 C39 112.6(6) . . ? C41 C40 H40A 109.1 . . ? C39 C40 H40A 109.1 . . ? C41 C40 H40B 109.1 . . ? C39 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C40 C41 C42 122.7(6) . . ? C40 C41 Ir1 114.1(6) . . ? C42 C41 Ir1 69.7(4) . . ? C40 C41 H41A 114.2 . . ? C42 C41 H41A 114.2 . . ? Ir1 C41 H41A 114.2 . . ? C41 C42 C43 122.5(6) . . ? C41 C42 Ir1 69.5(4) . . ? C43 C42 Ir1 118.0(5) . . ? C41 C42 H42A 113.3 . . ? C43 C42 H42A 113.3 . . ? Ir1 C42 H42A 113.3 . . ? C42 C43 C44 110.0(5) . . ? C42 C43 H43A 109.7 . . ? C44 C43 H43A 109.7 . . ? C42 C43 H43B 109.7 . . ? C44 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C37 C44 C43 110.5(6) . . ? C37 C44 H44A 109.6 . . ? C43 C44 H44A 109.6 . . ? C37 C44 H44B 109.6 . . ? C43 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.314 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.096