# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Wen-Zhen Wang' _publ_contact_author_email wzwang@xsyu.edu.cn _publ_section_title ; Fine tuning of pentachromium (II) metal string complexes through elaborate design of ligands ; _publ_author_name 'Wen-Zhen Wang' # Attachment 'ic12029-squeeze-new.cif' data_ic12029_squezze _database_code_depnum_ccdc_archive 'CCDC 829384' #TrackingRef 'ic12029-squeeze-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H40 Cl2 Cr5 N24' _chemical_formula_weight 1380.02 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 10.5897(6) _cell_length_b 10.5897(6) _cell_length_c 26.8588(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3012.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2618 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 26.60 _exptl_crystal_description 'square pyramidal' _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7698 _exptl_absorpt_correction_T_max 0.8454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1771 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1771 _reflns_number_gt 1543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _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. The SQUEEZE function in the PLATON package was then applied to remove the solvents electron density, thereby improving the final cycle of refinement, converging at values of R1 (wR2) from 7.96% (18.72%) to 7.08% (16,64%), respectively. ; _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^)+(0.0714P)^2^+16.4920P] 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 1771 _refine_ls_number_parameters 100 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.0000 0.0000 0.17771(10) 0.0247(6) Uani 0.510(2) 4 d SP . 1 Cr1' Cr 0.0000 0.0000 0.15971(11) 0.0247(6) Uani 0.490(2) 4 d SP . 2 Cr2 Cr 0.0000 0.0000 0.08362(4) 0.0242(3) Uani 1 4 d SU . . Cr3 Cr 0.0000 0.0000 0.01018(6) 0.0205(5) Uani 0.50 4 d SPU . . Cl1 Cl 0.0000 0.0000 0.26380(9) 0.0530(6) Uani 1 4 d S . . N1 N 0.1023(7) -0.1705(9) 0.1593(3) 0.0243(13) Uani 0.510(2) 1 d P . 1 N2 N -0.0070(5) -0.1914(5) 0.08644(17) 0.0226(7) Uani 0.510(2) 1 d P . 1 N1' N 0.0600(7) -0.1907(9) 0.1674(4) 0.0243(13) Uani 0.490(2) 1 d P . 2 N2' N -0.1211(5) -0.1462(5) 0.07731(18) 0.0226(7) Uani 0.490(2) 1 d P . 2 N3 N -0.0650(3) -0.1803(3) 0.0000 0.0242(8) Uani 1 2 d S . . N4 N -0.1482(5) -0.4271(4) 0.0000 0.0418(11) Uani 1 2 d S . . C1 C 0.1010(10) -0.2539(11) 0.1992(4) 0.0392(13) Uiso 0.510(2) 1 d P . 1 H1A H 0.0631 -0.2253 0.2292 0.047 Uiso 0.510(2) 1 calc PR . 1 C2 C 0.1496(9) -0.3739(10) 0.1991(4) 0.0468(15) Uiso 0.510(2) 1 d P . 1 H2A H 0.1406 -0.4316 0.2259 0.056 Uiso 0.510(2) 1 calc PR . 1 C3 C 0.2201(8) -0.4046(8) 0.1508(3) 0.0408(13) Uiso 0.510(2) 1 d P . 1 H3A H 0.2693 -0.4794 0.1489 0.049 Uiso 0.510(2) 1 calc PR . 1 C4 C 0.2137(7) -0.3284(7) 0.1115(3) 0.0384(11) Uiso 0.510(2) 1 d P . 1 H4A H 0.2469 -0.3558 0.0805 0.046 Uiso 0.510(2) 1 calc PR . 1 C5 C 0.1584(6) -0.2077(6) 0.1151(2) 0.0268(9) Uiso 0.510(2) 1 d P . 1 C6 C -0.0561(6) -0.2537(6) 0.0459(2) 0.0243(10) Uiso 0.510(2) 1 d P . 1 C7 C -0.1013(8) -0.3767(7) 0.0438(2) 0.0313(11) Uiso 0.510(2) 1 d P . 1 H7A H -0.1000 -0.4273 0.0730 0.038 Uiso 0.510(2) 1 calc PR . 1 C1' C 0.1251(10) -0.2419(11) 0.2045(4) 0.0392(13) Uiso 0.490(2) 1 d P . 2 H1'A H 0.1311 -0.1974 0.2351 0.047 Uiso 0.490(2) 1 calc PR . 2 C2' C 0.1837(10) -0.3560(10) 0.2003(4) 0.0468(15) Uiso 0.490(2) 1 d P . 2 H2'A H 0.2332 -0.3872 0.2271 0.056 Uiso 0.490(2) 1 calc PR . 2 C3' C 0.1720(9) -0.4241(9) 0.1587(3) 0.0408(13) Uiso 0.490(2) 1 d P . 2 H3'A H 0.2048 -0.5075 0.1569 0.049 Uiso 0.490(2) 1 calc PR . 2 C4' C 0.1122(8) -0.3717(8) 0.1194(3) 0.0384(11) Uiso 0.490(2) 1 d P . 2 H4'A H 0.1098 -0.4149 0.0884 0.046 Uiso 0.490(2) 1 calc PR . 2 C5' C 0.0535(6) -0.2533(6) 0.1243(2) 0.0268(9) Uiso 0.490(2) 1 d P . 2 C6' C -0.1188(7) -0.2268(6) 0.0373(2) 0.0243(10) Uiso 0.490(2) 1 d P . 2 C7' C -0.1585(8) -0.3536(7) 0.0379(3) 0.0313(11) Uiso 0.490(2) 1 d P . 2 H7'A H -0.1946 -0.3864 0.0675 0.038 Uiso 0.490(2) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0300(5) 0.0300(5) 0.0140(16) 0.000 0.000 0.000 Cr1' 0.0300(5) 0.0300(5) 0.0140(16) 0.000 0.000 0.000 Cr2 0.0229(4) 0.0229(4) 0.0269(5) 0.000 0.000 0.000 Cr3 0.0185(5) 0.0185(5) 0.0245(10) 0.000 0.000 0.000 Cl1 0.0496(8) 0.0496(8) 0.0596(13) 0.000 0.000 0.000 N1 0.021(4) 0.027(3) 0.025(3) 0.003(2) -0.004(3) -0.006(3) N2 0.0244(18) 0.0239(18) 0.0194(17) 0.0008(14) 0.0019(14) 0.0000(15) N1' 0.021(4) 0.027(3) 0.025(3) 0.003(2) -0.004(3) -0.006(3) N2' 0.0244(18) 0.0239(18) 0.0194(17) 0.0008(14) 0.0019(14) 0.0000(15) N3 0.0186(18) 0.0188(18) 0.035(2) 0.000 0.000 0.0034(14) N4 0.053(3) 0.027(2) 0.046(3) 0.000 0.000 -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.163(10) 4 ? Cr1 N1 2.163(10) 2 ? Cr1 N1 2.163(10) . ? Cr1 N1 2.163(10) 3 ? Cr1 Cl1 2.312(3) . ? Cr1 Cr2 2.527(3) . ? Cr1' Cr2 2.044(3) . ? Cr1' N1' 2.128(10) 2 ? Cr1' N1' 2.128(10) 4 ? Cr1' N1' 2.128(10) . ? Cr1' N1' 2.128(10) 3 ? Cr2 Cr3 1.972(2) . ? Cr2 N2' 2.018(5) 2 ? Cr2 N2' 2.018(5) 4 ? Cr2 N2' 2.018(5) . ? Cr2 N2' 2.018(5) 3 ? Cr2 N2 2.029(5) 2 ? Cr2 N2 2.029(5) 4 ? Cr2 N2 2.029(5) . ? Cr2 N2 2.029(5) 3 ? Cr2 Cr3 2.5193(19) 9 ? Cr3 Cr3 0.547(3) 9 ? Cr3 N3 2.048(4) 3 ? Cr3 N3 2.048(4) . ? Cr3 N3 2.048(4) 9 ? Cr3 N3 2.048(4) 11 ? Cr3 Cr2 2.5193(19) 9 ? N1 C5 1.385(11) . ? N1 C1 1.390(14) . ? N2 C6 1.376(8) . ? N2 C5 1.920(8) . ? N1' C1' 1.326(15) . ? N1' C5' 1.337(12) . ? N2' C6' 1.372(8) . ? N3 C6' 1.254(7) . ? N3 C6' 1.254(7) 10 ? N3 C6 1.460(6) 10 ? N3 C6 1.460(6) . ? N3 Cr3 2.048(4) 9 ? N4 C7' 1.285(8) . ? N4 C7' 1.285(8) 10 ? N4 C7 1.383(7) 10 ? N4 C7 1.383(7) . ? C1 C2 1.371(16) . ? C2 C3 1.531(14) . ? C3 C4 1.330(11) . ? C4 C5 1.409(10) . ? C6 C7 1.389(10) . ? C1' C2' 1.363(17) . ? C2' C3' 1.334(14) . ? C3' C4' 1.351(11) . ? C4' C5' 1.406(10) . ? C6' C7' 1.407(10) . ? C6' C6' 2.005(12) 10 ? C7' C7' 2.033(14) 10 ? 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 N1 Cr1 N1 87.00(11) 4 2 ? N1 Cr1 N1 87.00(11) 4 . ? N1 Cr1 N1 153.5(5) 2 . ? N1 Cr1 N1 153.5(5) 4 3 ? N1 Cr1 N1 87.00(11) 2 3 ? N1 Cr1 N1 87.00(11) . 3 ? N1 Cr1 Cl1 103.2(3) 4 . ? N1 Cr1 Cl1 103.2(3) 2 . ? N1 Cr1 Cl1 103.2(3) . . ? N1 Cr1 Cl1 103.2(3) 3 . ? N1 Cr1 Cr2 76.8(3) 4 . ? N1 Cr1 Cr2 76.8(3) 2 . ? N1 Cr1 Cr2 76.8(3) . . ? N1 Cr1 Cr2 76.8(3) 3 . ? Cl1 Cr1 Cr2 180.0 . . ? Cr2 Cr1' N1' 95.6(3) . 2 ? Cr2 Cr1' N1' 95.6(3) . 4 ? N1' Cr1' N1' 89.46(5) 2 4 ? Cr2 Cr1' N1' 95.6(3) . . ? N1' Cr1' N1' 168.8(5) 2 . ? N1' Cr1' N1' 89.45(5) 4 . ? Cr2 Cr1' N1' 95.6(3) . 3 ? N1' Cr1' N1' 89.46(5) 2 3 ? N1' Cr1' N1' 168.8(5) 4 3 ? N1' Cr1' N1' 89.45(5) . 3 ? Cr3 Cr2 N2' 85.19(14) . 2 ? Cr3 Cr2 N2' 85.19(14) . 4 ? N2' Cr2 N2' 89.60(2) 2 4 ? Cr3 Cr2 N2' 85.18(14) . . ? N2' Cr2 N2' 170.4(3) 2 . ? N2' Cr2 N2' 89.60(2) 4 . ? Cr3 Cr2 N2' 85.19(14) . 3 ? N2' Cr2 N2' 89.60(2) 2 3 ? N2' Cr2 N2' 170.4(3) 4 3 ? N2' Cr2 N2' 89.60(2) . 3 ? Cr3 Cr2 N2 92.14(13) . 2 ? N2' Cr2 N2 38.1(2) 2 2 ? N2' Cr2 N2 52.9(2) 4 2 ? N2' Cr2 N2 142.4(2) . 2 ? N2' Cr2 N2 127.6(2) 3 2 ? Cr3 Cr2 N2 92.14(13) . 4 ? N2' Cr2 N2 127.6(2) 2 4 ? N2' Cr2 N2 38.1(2) 4 4 ? N2' Cr2 N2 52.9(2) . 4 ? N2' Cr2 N2 142.4(2) 3 4 ? N2 Cr2 N2 89.919(10) 2 4 ? Cr3 Cr2 N2 92.14(13) . . ? N2' Cr2 N2 142.4(2) 2 . ? N2' Cr2 N2 127.6(2) 4 . ? N2' Cr2 N2 38.1(2) . . ? N2' Cr2 N2 52.9(2) 3 . ? N2 Cr2 N2 175.7(3) 2 . ? N2 Cr2 N2 89.920(10) 4 . ? Cr3 Cr2 N2 92.14(13) . 3 ? N2' Cr2 N2 52.9(2) 2 3 ? N2' Cr2 N2 142.4(2) 4 3 ? N2' Cr2 N2 127.6(2) . 3 ? N2' Cr2 N2 38.1(2) 3 3 ? N2 Cr2 N2 89.920(10) 2 3 ? N2 Cr2 N2 175.7(3) 4 3 ? N2 Cr2 N2 89.920(10) . 3 ? Cr3 Cr2 Cr1' 180.0 . . ? N2' Cr2 Cr1' 94.81(14) 2 . ? N2' Cr2 Cr1' 94.81(14) 4 . ? N2' Cr2 Cr1' 94.82(14) . . ? N2' Cr2 Cr1' 94.81(14) 3 . ? N2 Cr2 Cr1' 87.86(13) 2 . ? N2 Cr2 Cr1' 87.86(13) 4 . ? N2 Cr2 Cr1' 87.86(13) . . ? N2 Cr2 Cr1' 87.86(13) 3 . ? Cr3 Cr2 Cr3 0.0 . 9 ? N2' Cr2 Cr3 85.19(14) 2 9 ? N2' Cr2 Cr3 85.19(14) 4 9 ? N2' Cr2 Cr3 85.18(14) . 9 ? N2' Cr2 Cr3 85.19(14) 3 9 ? N2 Cr2 Cr3 92.14(13) 2 9 ? N2 Cr2 Cr3 92.14(13) 4 9 ? N2 Cr2 Cr3 92.14(13) . 9 ? N2 Cr2 Cr3 92.14(13) 3 9 ? Cr1' Cr2 Cr3 180.0 . 9 ? Cr3 Cr2 Cr1 180.0 . . ? N2' Cr2 Cr1 94.81(14) 2 . ? N2' Cr2 Cr1 94.81(14) 4 . ? N2' Cr2 Cr1 94.82(14) . . ? N2' Cr2 Cr1 94.81(14) 3 . ? N2 Cr2 Cr1 87.86(13) 2 . ? N2 Cr2 Cr1 87.86(13) 4 . ? N2 Cr2 Cr1 87.86(13) . . ? N2 Cr2 Cr1 87.86(13) 3 . ? Cr1' Cr2 Cr1 0.0 . . ? Cr3 Cr2 Cr1 180.0 9 . ? Cr3 Cr3 Cr2 180.0 9 . ? Cr3 Cr3 N3 82.33(5) 9 3 ? Cr2 Cr3 N3 97.67(5) . 3 ? Cr3 Cr3 N3 82.33(5) 9 . ? Cr2 Cr3 N3 97.67(5) . . ? N3 Cr3 N3 88.978(13) 3 . ? Cr3 Cr3 N3 82.33(5) 9 9 ? Cr2 Cr3 N3 97.67(5) . 9 ? N3 Cr3 N3 88.979(13) 3 9 ? N3 Cr3 N3 164.65(10) . 9 ? Cr3 Cr3 N3 82.32(5) 9 11 ? Cr2 Cr3 N3 97.67(5) . 11 ? N3 Cr3 N3 164.65(10) 3 11 ? N3 Cr3 N3 88.979(13) . 11 ? N3 Cr3 N3 88.977(13) 9 11 ? Cr3 Cr3 Cr2 0.0 9 9 ? Cr2 Cr3 Cr2 180.0 . 9 ? N3 Cr3 Cr2 82.33(5) 3 9 ? N3 Cr3 Cr2 82.33(5) . 9 ? N3 Cr3 Cr2 82.33(5) 9 9 ? N3 Cr3 Cr2 82.33(5) 11 9 ? C5 N1 C1 119.1(9) . . ? C5 N1 Cr1 130.4(6) . . ? C1 N1 Cr1 110.4(7) . . ? C6 N2 C5 128.2(5) . . ? C6 N2 Cr2 117.6(4) . . ? C5 N2 Cr2 94.1(3) . . ? C1' N1' C5' 118.3(9) . . ? C1' N1' Cr1' 128.1(8) . . ? C5' N1' Cr1' 111.7(6) . . ? C6' N2' Cr2 122.1(4) . . ? C6' N3 C6' 106.1(7) . 10 ? C6' N3 C6 119.6(5) . 10 ? C6' N3 C6 31.3(3) 10 10 ? C6' N3 C6 31.3(3) . . ? C6' N3 C6 119.6(5) 10 . ? C6 N3 C6 115.1(5) 10 . ? C6' N3 Cr3 128.7(3) . 9 ? C6' N3 Cr3 114.4(3) 10 9 ? C6 N3 Cr3 111.2(3) 10 9 ? C6 N3 Cr3 126.0(3) . 9 ? C6' N3 Cr3 114.4(3) . . ? C6' N3 Cr3 128.7(3) 10 . ? C6 N3 Cr3 126.0(3) 10 . ? C6 N3 Cr3 111.2(3) . . ? Cr3 N3 Cr3 15.35(10) 9 . ? C7' N4 C7' 104.6(8) . 10 ? C7' N4 C7 118.0(5) . 10 ? C7' N4 C7 28.9(4) 10 10 ? C7' N4 C7 28.9(4) . . ? C7' N4 C7 118.0(5) 10 . ? C7 N4 C7 116.4(7) 10 . ? C2 C1 N1 125.6(10) . . ? C1 C2 C3 112.5(9) . . ? C4 C3 C2 121.2(8) . . ? C3 C4 C5 121.2(7) . . ? N1 C5 C4 119.6(7) . . ? N1 C5 N2 85.8(5) . . ? C4 C5 N2 115.7(5) . . ? N2 C6 C7 127.8(6) . . ? N2 C6 N3 115.9(5) . . ? C7 C6 N3 116.3(5) . . ? N4 C7 C6 121.4(6) . . ? N1' C1' C2' 122.5(11) . . ? C3' C2' C1' 120.4(11) . . ? C2' C3' C4' 118.4(9) . . ? C3' C4' C5' 120.0(7) . . ? N1' C5' C4' 120.0(7) . . ? N3 C6' N2' 112.9(6) . . ? N3 C6' C7' 121.3(6) . . ? N2' C6' C7' 125.5(6) . . ? N3 C6' C6' 36.9(3) . 10 ? N2' C6' C6' 141.5(4) . 10 ? C7' C6' C6' 90.6(4) . 10 ? N4 C7' C6' 123.0(6) . . ? N4 C7' C7' 37.7(4) . 10 ? C6' C7' C7' 89.4(4) . 10 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.560 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.082 # Attachment 'ic11438-squeeze-new.cif' data_ic11438_squeeze _database_code_depnum_ccdc_archive 'CCDC 829385' #TrackingRef 'ic11438-squeeze-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H36 Cl2 Cr5 N28' _chemical_formula_weight 1383.99 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' Cr Cr 0.3209 0.6236 '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 10.4539(2) _cell_length_b 12.7977(3) _cell_length_c 25.2298(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.3254(13) _cell_angle_gamma 90.00 _cell_volume 3309.66(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32994 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5830 _reflns_number_gt 3962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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. The SQUEEZE function in the PLATON package was then applied to remove the solvents' electron density, thereby improving the final cycle of refinement, converging at values of R1 (wR2) from 7.47% (20.07%) to 6.70% (18.74%), respectively. ; _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^)+(0.1301P)^2^+5.7316P] 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 5830 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1874 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.012 _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 Cr1 Cr 0.42410(7) 0.88221(6) 0.32640(3) 0.0444(3) Uani 1 1 d . . . Cr2 Cr 0.4579(5) 0.9328(4) 0.40600(13) 0.0351(6) Uani 0.5007(16) 1 d P A 1 Cr2' Cr 0.4665(5) 0.9525(4) 0.42229(13) 0.0351(6) Uani 0.4993(16) 1 d P A 2 Cr3 Cr 0.5000 1.0000 0.5000 0.0392(4) Uani 1.001(3) 2 d SP . . Cl1 Cl 0.38335(13) 0.81675(11) 0.23178(4) 0.0567(4) Uani 1 1 d . A . N3 N 0.6835(3) 0.9368(3) 0.51255(13) 0.0344(8) Uani 1 1 d . A . N8 N 0.5742(3) 1.1364(3) 0.47553(13) 0.0357(8) Uani 1 1 d . A . C7 C 0.9316(5) 0.8542(4) 0.5289(2) 0.0530(13) Uani 1 1 d . . . H7A H 1.0137 0.8197 0.5363 0.064 Uiso 0.5007(16) 1 calc PR A 1 H7B H 1.0202 0.8327 0.5340 0.064 Uiso 0.4993(16) 1 calc PR A 2 C20 C 0.6830(6) 1.3147(4) 0.4441(2) 0.0635(15) Uani 1 1 d . . . H20A H 0.7168 1.3779 0.4327 0.076 Uiso 0.5007(16) 1 calc PR A 1 H20B H 0.7173 1.3781 0.4332 0.076 Uiso 0.4993(16) 1 calc PR A 2 N1 N 0.5232(7) 0.7539(6) 0.3597(3) 0.0287(16) Uiso 0.5007(16) 1 d P A 1 N2 N 0.6146(6) 0.8515(5) 0.4335(2) 0.0274(14) Uiso 0.5007(16) 1 d P A 1 N4 N 0.3152(6) 1.0532(5) 0.3967(3) 0.0331(15) Uiso 0.5007(16) 1 d P . 1 N5 N 0.3277(9) 1.0332(7) 0.3068(4) 0.032(2) Uiso 0.5007(16) 1 d P A 1 N11 N 0.6033(7) 0.9631(7) 0.3202(3) 0.0313(17) Uiso 0.5007(16) 1 d P A 1 N16 N 0.5872(6) 1.0612(5) 0.3954(3) 0.0330(15) Uiso 0.5007(16) 1 d P A 1 N17 N 0.3403(6) 0.8430(5) 0.4346(3) 0.0348(16) Uiso 0.5007(16) 1 d P . 1 N18 N 0.2524(12) 0.8287(10) 0.3436(5) 0.038(4) Uiso 0.5007(16) 1 d P A 1 N19 N 0.6305(8) 0.5664(6) 0.4082(3) 0.0426(18) Uiso 0.5007(16) 1 d P A 1 N20 N 0.2199(10) 1.2308(7) 0.2812(4) 0.048(2) Uiso 0.5007(16) 1 d P A 1 N25 N 0.8470(10) 1.0440(9) 0.3186(4) 0.051(3) Uiso 0.5007(16) 1 d P A 1 N26 N 0.0056(13) 0.7678(11) 0.3677(5) 0.056(4) Uiso 0.5007(16) 1 d P A 1 C1 C 0.5274(15) 0.6561(12) 0.3340(6) 0.065(5) Uiso 0.5007(16) 1 d P A 1 H1 H 0.4904 0.6525 0.2966 0.078 Uiso 0.5007(16) 1 calc PR A 1 C2 C 0.5792(14) 0.5674(11) 0.3580(6) 0.068(4) Uiso 0.5007(16) 1 d P A 1 H2 H 0.5774 0.5052 0.3373 0.081 Uiso 0.5007(16) 1 calc PR A 1 C3 C 0.6558(9) 0.6608(7) 0.4316(4) 0.047(2) Uiso 0.5007(16) 1 d P A 1 H3 H 0.7136 0.6639 0.4657 0.056 Uiso 0.5007(16) 1 calc PR A 1 C4 C 0.6014(8) 0.7559(6) 0.4086(3) 0.0351(19) Uiso 0.5007(16) 1 d P A 1 C5 C 0.7162(8) 0.8719(7) 0.4762(4) 0.026(2) Uiso 0.5007(16) 1 d P A 1 C6 C 0.8404(10) 0.8303(9) 0.4822(4) 0.037(3) Uiso 0.5007(16) 1 d P A 1 H6 H 0.8631 0.7864 0.4551 0.044 Uiso 0.5007(16) 1 calc PR A 1 C8 C 0.9005(9) 0.9307(8) 0.5652(4) 0.046(2) Uiso 0.5007(16) 1 d P A 1 H8A H 0.9633 0.9506 0.5961 0.055 Uiso 0.5007(16) 1 calc PR A 1 C9 C 0.7777(8) 0.9758(7) 0.5551(3) 0.0324(18) Uiso 0.5007(16) 1 d P . 1 C10 C 0.2899(8) 1.0937(6) 0.3449(3) 0.0323(18) Uiso 0.5007(16) 1 d P A 1 C11 C 0.2376(9) 1.1940(7) 0.3312(4) 0.045(2) Uiso 0.5007(16) 1 d P A 1 H11 H 0.2144 1.2364 0.3587 0.054 Uiso 0.5007(16) 1 calc PR A 1 C12 C 0.2605(10) 1.1730(9) 0.2455(5) 0.040(3) Uiso 0.5007(16) 1 d P A 1 H12 H 0.2535 1.2000 0.2100 0.048 Uiso 0.5007(16) 1 calc PR A 1 C13 C 0.3129(9) 1.0752(7) 0.2562(3) 0.030(2) Uiso 0.5007(16) 1 d P A 1 H13 H 0.3392 1.0363 0.2281 0.036 Uiso 0.5007(16) 1 calc PR A 1 C18 C 0.6122(9) 1.1521(6) 0.4255(3) 0.0299(18) Uiso 0.5007(16) 1 d P A 1 C19 C 0.6675(11) 1.2428(8) 0.4107(4) 0.045(2) Uiso 0.5007(16) 1 d P A 1 H19 H 0.6925 1.2496 0.3767 0.054 Uiso 0.5007(16) 1 calc PR A 1 C21 C 0.6572(12) 1.3151(10) 0.4964(5) 0.059(3) Uiso 0.5007(16) 1 d P A 1 H21 H 0.6809 1.3714 0.5209 0.070 Uiso 0.5007(16) 1 calc PR A 1 C22 C 0.5950(9) 1.2277(7) 0.5090(3) 0.037(2) Uiso 0.5007(16) 1 d P . 1 C39 C 0.6747(13) 0.9282(11) 0.2838(6) 0.041(4) Uiso 0.5007(16) 1 d P A 1 H39 H 0.6413 0.8742 0.2591 0.049 Uiso 0.5007(16) 1 calc PR A 1 C40 C 0.7895(14) 0.9692(11) 0.2829(6) 0.051(4) Uiso 0.5007(16) 1 d P A 1 H40 H 0.8350 0.9457 0.2561 0.061 Uiso 0.5007(16) 1 calc PR A 1 C41 C 0.7832(9) 1.0730(7) 0.3540(4) 0.043(2) Uiso 0.5007(16) 1 d P A 1 H41 H 0.8222 1.1227 0.3802 0.051 Uiso 0.5007(16) 1 calc PR A 1 C42 C 0.6576(8) 1.0355(6) 0.3565(3) 0.0335(18) Uiso 0.5007(16) 1 d P A 1 C47 C 0.2333(9) 0.8195(7) 0.3948(4) 0.041(2) Uiso 0.5007(16) 1 d P A 1 C48 C 0.1087(9) 0.7936(8) 0.4046(4) 0.044(2) Uiso 0.5007(16) 1 d P A 1 H48 H 0.0981 0.7949 0.4411 0.053 Uiso 0.5007(16) 1 calc PR A 1 C49 C 0.0230(10) 0.7970(8) 0.3135(4) 0.049(2) Uiso 0.5007(16) 1 d P A 1 H49 H -0.0516 0.7987 0.2850 0.059 Uiso 0.5007(16) 1 calc PR A 1 C50 C 0.1401(9) 0.8216(8) 0.3020(4) 0.040(2) Uiso 0.5007(16) 1 d P A 1 H50 H 0.1472 0.8342 0.2656 0.048 Uiso 0.5007(16) 1 calc PR A 1 N6 N 0.3650(10) 1.0283(8) 0.3059(4) 0.043(3) Uiso 0.4993(16) 1 d P A 2 N7 N 0.4715(7) 1.0818(5) 0.3896(3) 0.0363(16) Uiso 0.4993(16) 1 d P A 2 N9 N 0.4483(7) 0.7881(5) 0.4428(3) 0.0382(16) Uiso 0.4993(16) 1 d P . 2 N10 N 0.4768(9) 0.7259(7) 0.3604(3) 0.046(2) Uiso 0.4993(16) 1 d P A 2 N12 N 0.6526(7) 0.9186(6) 0.4201(3) 0.0365(16) Uiso 0.4993(16) 1 d P A 2 N13 N 0.2676(6) 0.9504(5) 0.4124(3) 0.0312(15) Uiso 0.4993(16) 1 d P . 2 N14 N 0.2330(12) 0.8417(10) 0.3390(5) 0.037(4) Uiso 0.4993(16) 1 d P A 2 N15 N 0.6168(8) 0.9200(7) 0.3273(3) 0.040(2) Uiso 0.4993(16) 1 d P A 2 N21 N 0.2695(11) 1.2289(8) 0.2777(4) 0.058(3) Uiso 0.4993(16) 1 d P A 2 N22 N 0.5563(16) 0.5301(12) 0.4055(6) 0.115(4) Uiso 0.4993(16) 1 d P A 2 N23 N 0.8598(10) 1.0145(9) 0.3279(4) 0.051(3) Uiso 0.4993(16) 1 d P A 2 N24 N -0.0036(14) 0.7879(11) 0.3590(6) 0.060(5) Uiso 0.4993(16) 1 d P A 2 C14 C 0.2803(12) 1.0420(10) 0.2575(5) 0.054(3) Uiso 0.4993(16) 1 d P A 2 H14 H 0.2512 0.9836 0.2351 0.065 Uiso 0.4993(16) 1 calc PR A 2 C15 C 0.2384(14) 1.1397(12) 0.2418(6) 0.067(4) Uiso 0.4993(16) 1 d P A 2 H15 H 0.1875 1.1500 0.2067 0.080 Uiso 0.4993(16) 1 calc PR A 2 C16 C 0.3483(10) 1.2063(8) 0.3237(4) 0.053(2) Uiso 0.4993(16) 1 d P A 2 H16 H 0.3737 1.2624 0.3482 0.063 Uiso 0.4993(16) 1 calc PR A 2 C17 C 0.3985(9) 1.1069(7) 0.3400(4) 0.040(2) Uiso 0.4993(16) 1 d P A 2 C23 C 0.4813(10) 0.7055(8) 0.4139(4) 0.052(2) Uiso 0.4993(16) 1 d P A 2 C24 C 0.5311(14) 0.6102(11) 0.4369(6) 0.086(4) Uiso 0.4993(16) 1 d P A 2 H24 H 0.5473 0.6019 0.4750 0.103 Uiso 0.4993(16) 1 calc PR A 2 C25 C 0.5267(14) 0.5579(10) 0.3541(5) 0.060(3) Uiso 0.4993(16) 1 d P A 2 H25 H 0.5348 0.5046 0.3288 0.072 Uiso 0.4993(16) 1 calc PR A 2 C26 C 0.4867(12) 0.6513(9) 0.3328(5) 0.040(3) Uiso 0.4993(16) 1 d P A 2 H26 H 0.4656 0.6584 0.2946 0.048 Uiso 0.4993(16) 1 calc PR A 2 C27 C 0.6556(14) 0.9482(11) 0.2800(6) 0.043(4) Uiso 0.4993(16) 1 d P A 2 H27 H 0.5994 0.9345 0.2463 0.052 Uiso 0.4993(16) 1 calc PR A 2 C28 C 0.7781(14) 0.9973(12) 0.2808(6) 0.054(4) Uiso 0.4993(16) 1 d P A 2 H28 H 0.8019 1.0179 0.2479 0.064 Uiso 0.4993(16) 1 calc PR A 2 C29 C 0.8200(10) 0.9893(8) 0.3733(4) 0.051(2) Uiso 0.4993(16) 1 d P A 2 H29 H 0.8755 1.0061 0.4068 0.061 Uiso 0.4993(16) 1 calc PR A 2 C30 C 0.7010(8) 0.9394(7) 0.3747(3) 0.039(2) Uiso 0.4993(16) 1 d P A 2 C31 C 0.7364(10) 0.9040(8) 0.4706(4) 0.035(3) Uiso 0.4993(16) 1 d P A 2 C32 C 0.8584(11) 0.8600(9) 0.4776(5) 0.043(3) Uiso 0.4993(16) 1 d P A 2 H32 H 0.8913 0.8343 0.4476 0.052 Uiso 0.4993(16) 1 calc PR A 2 C33 C 0.8789(9) 0.8788(8) 0.5727(4) 0.038(2) Uiso 0.4993(16) 1 d P A 2 H33 H 0.9286 0.8716 0.6083 0.046 Uiso 0.4993(16) 1 calc PR A 2 C34 C 0.7514(8) 0.9144(7) 0.5640(3) 0.0358(19) Uiso 0.4993(16) 1 d P . 2 C35 C 0.1847(9) 0.8826(7) 0.3806(4) 0.042(2) Uiso 0.4993(16) 1 d P A 2 C36 C 0.0645(10) 0.8462(9) 0.3889(4) 0.054(3) Uiso 0.4993(16) 1 d P A 2 H36 H 0.0351 0.8692 0.4202 0.065 Uiso 0.4993(16) 1 calc PR A 2 C37 C 0.0478(13) 0.7310(11) 0.3204(5) 0.075(3) Uiso 0.4993(16) 1 d P A 2 H37 H 0.0042 0.6714 0.3030 0.090 Uiso 0.4993(16) 1 calc PR A 2 C38 C 0.1613(10) 0.7646(9) 0.3092(4) 0.054(3) Uiso 0.4993(16) 1 d P A 2 H38 H 0.1927 0.7342 0.2799 0.065 Uiso 0.4993(16) 1 calc PR A 2 C43 C 0.5469(10) 1.1511(6) 0.4228(3) 0.0324(19) Uiso 0.4993(16) 1 d P A 2 C44 C 0.6075(10) 1.2416(7) 0.4042(4) 0.033(2) Uiso 0.4993(16) 1 d P A 2 H44 H 0.5990 1.2545 0.3666 0.040 Uiso 0.4993(16) 1 calc PR A 2 C45 C 0.7008(10) 1.2869(8) 0.4967(4) 0.040(2) Uiso 0.4993(16) 1 d P A 2 H45 H 0.7497 1.3312 0.5234 0.049 Uiso 0.4993(16) 1 calc PR A 2 C46 C 0.6476(9) 1.1923(7) 0.5129(3) 0.034(2) Uiso 0.4993(16) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0443(5) 0.0542(5) 0.0356(4) -0.0066(3) 0.0104(3) 0.0023(3) Cr2 0.0364(7) 0.0422(16) 0.0264(18) -0.0011(11) 0.0055(14) 0.0057(9) Cr2' 0.0364(7) 0.0422(16) 0.0264(18) -0.0011(11) 0.0055(14) 0.0057(9) Cr3 0.0345(6) 0.0390(6) 0.0452(6) -0.0011(4) 0.0108(4) 0.0067(4) Cl1 0.0691(8) 0.0721(8) 0.0301(6) -0.0122(6) 0.0127(5) -0.0043(7) N3 0.0359(19) 0.044(2) 0.0237(17) -0.0016(15) 0.0064(14) 0.0074(16) N8 0.042(2) 0.041(2) 0.0256(18) -0.0006(15) 0.0103(15) 0.0054(16) C7 0.038(3) 0.068(3) 0.052(3) -0.004(3) 0.008(2) 0.015(2) C20 0.092(4) 0.051(3) 0.050(3) 0.016(3) 0.021(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N6 2.005(10) . ? Cr1 N1 2.033(7) . ? Cr1 N18 2.046(12) . ? Cr1 N15 2.067(8) . ? Cr1 Cr2 2.073(3) . ? Cr1 N14 2.147(13) . ? Cr1 N11 2.173(7) . ? Cr1 N5 2.190(9) . ? Cr1 N10 2.204(9) . ? Cr1 Cl1 2.4865(13) . ? Cr1 Cr2' 2.537(3) . ? Cr2 N17 1.924(9) . ? Cr2 N2 1.949(8) . ? Cr2 N4 2.126(8) . ? Cr2 N16 2.178(8) . ? Cr2 Cr3 2.480(2) . ? Cr2' N7 1.854(9) . ? Cr2' N12 2.005(8) . ? Cr2' Cr3 2.016(3) . ? Cr2' N13 2.046(8) . ? Cr2' N9 2.185(9) . ? Cr3 Cr2' 2.016(3) 3_676 ? Cr3 N3 2.048(3) . ? Cr3 N3 2.048(3) 3_676 ? Cr3 N8 2.054(4) . ? Cr3 N8 2.054(4) 3_676 ? Cr3 Cr2 2.480(2) 3_676 ? N3 C5 1.330(9) . ? N3 C31 1.354(10) . ? N3 C34 1.382(9) . ? N3 C9 1.399(9) . ? N8 C46 1.306(9) . ? N8 C43 1.319(9) . ? N8 C18 1.409(9) . ? N8 C22 1.433(10) . ? C7 C33 1.365(10) . ? C7 C32 1.369(12) . ? C7 C6 1.395(11) . ? C7 C8 1.422(11) . ? C20 C19 1.237(11) . ? C20 C45 1.351(11) . ? C20 C21 1.396(13) . ? C20 C44 1.482(11) . ? N1 C4 1.339(10) . ? N1 C1 1.414(17) . ? N2 C4 1.370(10) . ? N2 C5 1.381(10) . ? N4 C10 1.384(10) . ? N4 C9 1.739(10) 3_676 ? N5 C10 1.351(12) . ? N5 C13 1.367(13) . ? N11 C42 1.347(11) . ? N11 C39 1.368(15) . ? N16 C42 1.377(10) . ? N16 C18 1.387(10) . ? N17 C47 1.383(11) . ? N17 C22 1.710(11) 3_676 ? N18 C47 1.349(15) . ? N18 C50 1.416(15) . ? N19 C2 1.275(15) . ? N19 C3 1.348(12) . ? N20 C12 1.300(15) . ? N20 C11 1.326(13) . ? N25 C41 1.271(13) . ? N25 C40 1.370(18) . ? N26 C48 1.320(16) . ? N26 C49 1.464(17) . ? C1 C2 1.35(2) . ? C3 C4 1.419(12) . ? C5 C6 1.384(13) . ? C8 C9 1.385(12) . ? C9 N4 1.739(10) 3_676 ? C10 C11 1.411(12) . ? C12 C13 1.371(15) . ? C18 C19 1.381(13) . ? C21 C22 1.363(14) . ? C22 N17 1.710(11) 3_676 ? C39 C40 1.314(19) . ? C41 C42 1.411(12) . ? C47 C48 1.412(13) . ? C49 C50 1.349(13) . ? N6 C17 1.325(13) . ? N6 C14 1.371(15) . ? N7 C43 1.359(11) . ? N7 C17 1.370(11) . ? N9 C23 1.365(12) . ? N9 C46 1.662(11) 3_676 ? N10 C26 1.197(14) . ? N10 C23 1.367(13) . ? N12 C30 1.366(11) . ? N12 C31 1.409(12) . ? N13 C35 1.369(11) . ? N13 C34 1.852(11) 3_676 ? N14 C35 1.355(15) . ? N14 C38 1.371(16) . ? N15 C30 1.361(11) . ? N15 C27 1.383(16) . ? N21 C16 1.316(14) . ? N21 C15 1.455(18) . ? N22 C25 1.321(19) . ? N22 C24 1.352(19) . ? N23 C29 1.332(14) . ? N23 C28 1.339(18) . ? N24 C36 1.191(16) . ? N24 C37 1.406(19) . ? C14 C15 1.358(19) . ? C16 C17 1.407(13) . ? C23 C24 1.406(16) . ? C25 C26 1.343(17) . ? C27 C28 1.42(2) . ? C29 C30 1.405(13) . ? C31 C32 1.374(15) . ? C33 C34 1.385(12) . ? C34 N13 1.852(11) 3_676 ? C35 C36 1.394(13) . ? C37 C38 1.343(16) . ? C43 C44 1.442(12) . ? C45 C46 1.425(13) . ? C46 N9 1.661(11) 3_676 ? 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 Cr1 N1 165.0(4) . . ? N6 Cr1 N18 97.4(5) . . ? N1 Cr1 N18 92.3(4) . . ? N6 Cr1 N15 92.0(4) . . ? N1 Cr1 N15 76.6(3) . . ? N18 Cr1 N15 165.8(4) . . ? N6 Cr1 Cr2 86.8(3) . . ? N1 Cr1 Cr2 82.9(2) . . ? N18 Cr1 Cr2 83.6(4) . . ? N15 Cr1 Cr2 86.3(3) . . ? N6 Cr1 N14 90.9(5) . . ? N1 Cr1 N14 99.0(4) . . ? N18 Cr1 N14 6.8(6) . . ? N15 Cr1 N14 171.0(4) . . ? Cr2 Cr1 N14 85.3(4) . . ? N6 Cr1 N11 76.3(4) . . ? N1 Cr1 N11 92.1(3) . . ? N18 Cr1 N11 168.4(4) . . ? N15 Cr1 N11 15.7(2) . . ? Cr2 Cr1 N11 86.3(2) . . ? N14 Cr1 N11 165.1(4) . . ? N6 Cr1 N5 9.7(4) . . ? N1 Cr1 N5 168.6(3) . . ? N18 Cr1 N5 87.6(4) . . ? N15 Cr1 N5 101.6(4) . . ? Cr2 Cr1 N5 85.8(3) . . ? N14 Cr1 N5 81.2(4) . . ? N11 Cr1 N5 85.9(3) . . ? N6 Cr1 N10 171.1(4) . . ? N1 Cr1 N10 15.8(3) . . ? N18 Cr1 N10 77.1(4) . . ? N15 Cr1 N10 92.2(4) . . ? Cr2 Cr1 N10 85.7(3) . . ? N14 Cr1 N10 83.8(4) . . ? N11 Cr1 N10 107.9(3) . . ? N5 Cr1 N10 163.2(3) . . ? N6 Cr1 Cl1 94.6(3) . . ? N1 Cr1 Cl1 95.83(19) . . ? N18 Cr1 Cl1 95.7(3) . . ? N15 Cr1 Cl1 94.2(2) . . ? Cr2 Cr1 Cl1 178.49(15) . . ? N14 Cr1 Cl1 94.1(3) . . ? N11 Cr1 Cl1 94.55(19) . . ? N5 Cr1 Cl1 95.5(2) . . ? N10 Cr1 Cl1 92.9(2) . . ? N6 Cr1 Cr2' 84.4(3) . . ? N1 Cr1 Cr2' 85.0(2) . . ? N18 Cr1 Cr2' 85.0(4) . . ? N15 Cr1 Cr2' 85.3(2) . . ? Cr2 Cr1 Cr2' 2.6(3) . . ? N14 Cr1 Cr2' 86.4(3) . . ? N11 Cr1 Cr2' 84.7(2) . . ? N5 Cr1 Cr2' 83.6(3) . . ? N10 Cr1 Cr2' 88.2(2) . . ? Cl1 Cr1 Cr2' 178.88(13) . . ? N17 Cr2 N2 95.8(4) . . ? N17 Cr2 Cr1 100.2(3) . . ? N2 Cr2 Cr1 98.6(2) . . ? N17 Cr2 N4 89.3(3) . . ? N2 Cr2 N4 161.5(3) . . ? Cr1 Cr2 N4 97.9(3) . . ? N17 Cr2 N16 162.7(3) . . ? N2 Cr2 N16 87.0(3) . . ? Cr1 Cr2 N16 96.2(3) . . ? N4 Cr2 N16 83.0(3) . . ? N17 Cr2 Cr3 81.7(2) . . ? N2 Cr2 Cr3 82.3(2) . . ? Cr1 Cr2 Cr3 177.8(3) . . ? N4 Cr2 Cr3 80.9(2) . . ? N16 Cr2 Cr3 81.8(2) . . ? N7 Cr2' N12 93.9(4) . . ? N7 Cr2' Cr3 98.6(3) . . ? N12 Cr2' Cr3 96.2(3) . . ? N7 Cr2' N13 94.3(3) . . ? N12 Cr2' N13 164.3(3) . . ? Cr3 Cr2' N13 95.8(3) . . ? N7 Cr2' N9 167.5(3) . . ? N12 Cr2' N9 85.9(3) . . ? Cr3 Cr2' N9 93.8(3) . . ? N13 Cr2' N9 83.2(3) . . ? N7 Cr2' Cr1 84.7(3) . . ? N12 Cr2' Cr1 83.5(2) . . ? Cr3 Cr2' Cr1 176.7(3) . . ? N13 Cr2' Cr1 84.0(2) . . ? N9 Cr2' Cr1 82.9(2) . . ? Cr2' Cr3 Cr2' 179.998(1) 3_676 . ? Cr2' Cr3 N3 89.45(17) 3_676 . ? Cr2' Cr3 N3 90.55(17) . . ? Cr2' Cr3 N3 90.56(17) 3_676 3_676 ? Cr2' Cr3 N3 89.44(17) . 3_676 ? N3 Cr3 N3 179.999(2) . 3_676 ? Cr2' Cr3 N8 91.87(18) 3_676 . ? Cr2' Cr3 N8 88.12(18) . . ? N3 Cr3 N8 89.12(14) . . ? N3 Cr3 N8 90.88(14) 3_676 . ? Cr2' Cr3 N8 88.13(18) 3_676 3_676 ? Cr2' Cr3 N8 91.87(18) . 3_676 ? N3 Cr3 N8 90.88(14) . 3_676 ? N3 Cr3 N8 89.12(14) 3_676 3_676 ? N8 Cr3 N8 180.00(17) . 3_676 ? Cr2' Cr3 Cr2 177.2(3) 3_676 . ? Cr2' Cr3 Cr2 2.8(3) . . ? N3 Cr3 Cr2 89.75(14) . . ? N3 Cr3 Cr2 90.25(14) 3_676 . ? N8 Cr3 Cr2 90.79(15) . . ? N8 Cr3 Cr2 89.20(15) 3_676 . ? Cr2' Cr3 Cr2 2.8(3) 3_676 3_676 ? Cr2' Cr3 Cr2 177.2(3) . 3_676 ? N3 Cr3 Cr2 90.25(14) . 3_676 ? N3 Cr3 Cr2 89.75(14) 3_676 3_676 ? N8 Cr3 Cr2 89.21(15) . 3_676 ? N8 Cr3 Cr2 90.80(15) 3_676 3_676 ? Cr2 Cr3 Cr2 180.000(1) . 3_676 ? C5 N3 C31 21.3(5) . . ? C5 N3 C34 111.4(6) . . ? C31 N3 C34 117.2(6) . . ? C5 N3 C9 120.9(6) . . ? C31 N3 C9 112.1(6) . . ? C34 N3 C9 36.7(4) . . ? C5 N3 Cr3 120.0(4) . . ? C31 N3 Cr3 121.0(5) . . ? C34 N3 Cr3 121.3(4) . . ? C9 N3 Cr3 118.3(4) . . ? C46 N8 C43 129.1(6) . . ? C46 N8 C18 109.8(6) . . ? C43 N8 C18 28.3(4) . . ? C46 N8 C22 29.3(4) . . ? C43 N8 C22 117.1(6) . . ? C18 N8 C22 111.9(5) . . ? C46 N8 Cr3 116.9(4) . . ? C43 N8 Cr3 113.9(4) . . ? C18 N8 Cr3 125.5(4) . . ? C22 N8 Cr3 122.6(4) . . ? C33 C7 C32 120.8(7) . . ? C33 C7 C6 114.5(7) . . ? C32 C7 C6 18.7(6) . . ? C33 C7 C8 30.6(4) . . ? C32 C7 C8 114.5(7) . . ? C6 C7 C8 119.3(7) . . ? C19 C20 C45 116.6(8) . . ? C19 C20 C21 128.5(8) . . ? C45 C20 C21 24.3(6) . . ? C19 C20 C44 24.1(5) . . ? C45 C20 C44 116.9(6) . . ? C21 C20 C44 117.9(7) . . ? C4 N1 C1 111.7(9) . . ? C4 N1 Cr1 122.3(6) . . ? C1 N1 Cr1 125.8(8) . . ? C4 N2 C5 121.3(7) . . ? C4 N2 Cr2 108.1(5) . . ? C5 N2 Cr2 129.9(5) . . ? C10 N4 C9 135.4(6) . 3_676 ? C10 N4 Cr2 112.0(5) . . ? C9 N4 Cr2 104.2(4) 3_676 . ? C10 N5 C13 116.3(8) . . ? C10 N5 Cr1 122.1(6) . . ? C13 N5 Cr1 121.4(7) . . ? C42 N11 C39 117.9(8) . . ? C42 N11 Cr1 122.2(6) . . ? C39 N11 Cr1 119.0(7) . . ? C42 N16 C18 121.5(7) . . ? C42 N16 Cr2 109.8(5) . . ? C18 N16 Cr2 128.3(6) . . ? C47 N17 C22 128.4(7) . 3_676 ? C47 N17 Cr2 110.0(6) . . ? C22 N17 Cr2 116.8(5) 3_676 . ? C47 N18 C50 116.5(10) . . ? C47 N18 Cr1 122.2(9) . . ? C50 N18 Cr1 119.9(8) . . ? C2 N19 C3 115.8(10) . . ? C12 N20 C11 117.0(9) . . ? C41 N25 C40 116.3(11) . . ? C48 N26 C49 111.2(11) . . ? C2 C1 N1 125.9(13) . . ? N19 C2 C1 120.5(14) . . ? N19 C3 C4 124.1(8) . . ? N1 C4 N2 115.4(7) . . ? N1 C4 C3 118.9(7) . . ? N2 C4 C3 125.5(7) . . ? N3 C5 N2 113.1(7) . . ? N3 C5 C6 121.8(8) . . ? N2 C5 C6 125.1(8) . . ? C5 C6 C7 118.6(9) . . ? C9 C8 C7 119.3(8) . . ? C8 C9 N3 118.7(7) . . ? C8 C9 N4 114.0(7) . 3_676 ? N3 C9 N4 93.1(5) . 3_676 ? N5 C10 N4 115.4(7) . . ? N5 C10 C11 120.1(8) . . ? N4 C10 C11 124.3(7) . . ? N20 C11 C10 122.1(9) . . ? N20 C12 C13 123.8(10) . . ? N5 C13 C12 120.7(9) . . ? C19 C18 N16 126.9(8) . . ? C19 C18 N8 124.7(7) . . ? N16 C18 N8 108.4(6) . . ? C20 C19 C18 116.5(9) . . ? C22 C21 C20 114.0(10) . . ? C21 C22 N8 123.8(8) . . ? C21 C22 N17 120.0(8) . 3_676 ? N8 C22 N17 92.7(6) . 3_676 ? C40 C39 N11 120.1(13) . . ? C39 C40 N25 123.5(14) . . ? N25 C41 C42 123.6(9) . . ? N11 C42 N16 115.8(7) . . ? N11 C42 C41 118.4(8) . . ? N16 C42 C41 125.6(8) . . ? N18 C47 N17 115.2(9) . . ? N18 C47 C48 120.2(9) . . ? N17 C47 C48 124.5(8) . . ? N26 C48 C47 126.1(10) . . ? C50 C49 N26 123.0(10) . . ? C49 C50 N18 120.8(10) . . ? C17 N6 C14 121.5(10) . . ? C17 N6 Cr1 120.7(7) . . ? C14 N6 Cr1 117.5(8) . . ? C43 N7 C17 124.2(7) . . ? C43 N7 Cr2' 111.8(5) . . ? C17 N7 Cr2' 123.8(6) . . ? C23 N9 C46 136.5(7) . 3_676 ? C23 N9 Cr2' 125.2(6) . . ? C46 N9 Cr2' 96.1(5) 3_676 . ? C26 N10 C23 115.6(10) . . ? C26 N10 Cr1 122.8(8) . . ? C23 N10 Cr1 120.9(7) . . ? C30 N12 C31 121.2(8) . . ? C30 N12 Cr2' 120.1(6) . . ? C31 N12 Cr2' 116.0(6) . . ? C35 N13 C34 133.2(6) . 3_676 ? C35 N13 Cr2' 126.2(6) . . ? C34 N13 Cr2' 96.8(4) 3_676 . ? C35 N14 C38 117.1(11) . . ? C35 N14 Cr1 121.3(8) . . ? C38 N14 Cr1 121.1(9) . . ? C30 N15 C27 117.5(9) . . ? C30 N15 Cr1 120.9(6) . . ? C27 N15 Cr1 120.1(8) . . ? C16 N21 C15 113.6(10) . . ? C25 N22 C24 109.5(14) . . ? C29 N23 C28 118.2(11) . . ? C36 N24 C37 120.0(13) . . ? C15 C14 N6 119.5(13) . . ? C14 C15 N21 121.5(13) . . ? N21 C16 C17 126.1(10) . . ? N6 C17 N7 116.4(8) . . ? N6 C17 C16 117.5(9) . . ? N7 C17 C16 126.0(8) . . ? N9 C23 N10 114.6(9) . . ? N9 C23 C24 124.3(10) . . ? N10 C23 C24 120.7(10) . . ? N22 C24 C23 121.1(14) . . ? N22 C25 C26 128.9(13) . . ? N10 C26 C25 122.2(11) . . ? N15 C27 C28 121.2(13) . . ? N23 C28 C27 120.0(13) . . ? N23 C29 C30 123.9(10) . . ? N15 C30 N12 114.7(8) . . ? N15 C30 C29 119.0(8) . . ? N12 C30 C29 125.8(8) . . ? N3 C31 C32 122.5(9) . . ? N3 C31 N12 112.9(7) . . ? C32 C31 N12 124.6(9) . . ? C7 C32 C31 118.5(10) . . ? C7 C33 C34 118.6(8) . . ? N3 C34 C33 121.1(7) . . ? N3 C34 N13 92.4(5) . 3_676 ? C33 C34 N13 114.7(7) . 3_676 ? N14 C35 N13 114.2(9) . . ? N14 C35 C36 118.0(9) . . ? N13 C35 C36 127.6(9) . . ? N24 C36 C35 124.0(12) . . ? C38 C37 N24 116.9(13) . . ? C37 C38 N14 121.7(12) . . ? N8 C43 N7 120.9(7) . . ? N8 C43 C44 114.8(7) . . ? N7 C43 C44 124.3(8) . . ? C43 C44 C20 119.7(7) . . ? C20 C45 C46 121.3(8) . . ? N8 C46 C45 117.8(7) . . ? N8 C46 N9 102.8(6) . 3_676 ? C45 C46 N9 112.7(8) . 3_676 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.611 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.214 # Attachment 'ic13942.cif' data_ic13942 _database_code_depnum_ccdc_archive 'CCDC 829386' #TrackingRef 'ic13942.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H56 Cl4 Cr5 N26 S2' _chemical_formula_weight 1751.35 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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)/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 14.8488(2) _cell_length_b 31.4891(4) _cell_length_c 15.9630(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.5875(6) _cell_angle_gamma 90.00 _cell_volume 7428.44(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9654 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46127 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16938 _reflns_number_gt 9632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0868P)^2^+0.1571P] 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 16938 _refine_ls_number_parameters 992 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.003 _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 Cr1 Cr 0.57136(4) 0.182529(18) 0.30076(4) 0.03073(16) Uani 1 1 d . . . Cr2 Cr 0.6241(5) 0.1596(2) 0.4185(4) 0.0253(8) Uani 0.515(10) 1 d P A 1 Cr3 Cr 0.6908(8) 0.1294(4) 0.5605(7) 0.0250(10) Uani 0.515(10) 1 d P A 1 Cr4 Cr 0.7409(5) 0.1065(2) 0.6674(4) 0.0249(7) Uani 0.515(10) 1 d P A 1 Cr2' Cr 0.6335(7) 0.1556(3) 0.4383(5) 0.0253(8) Uani 0.485(10) 1 d P A 2 Cr3' Cr 0.6828(12) 0.1333(5) 0.5452(9) 0.0250(10) Uani 0.485(10) 1 d P A 2 Cr4' Cr 0.7502(7) 0.1022(3) 0.6879(5) 0.0249(7) Uani 0.485(10) 1 d P A 2 Cr5 Cr 0.79999(4) 0.075085(18) 0.80511(4) 0.03187(16) Uani 1 1 d . . . S1 S 0.48722(8) 0.26591(3) 0.04605(7) 0.0461(3) Uani 1 1 d . A . S2 S 0.89008(8) -0.00366(4) 1.06730(7) 0.0538(3) Uani 1 1 d . A . N1 N 0.49759(18) 0.22541(8) 0.36816(17) 0.0235(6) Uani 1 1 d . A . N2 N 0.52519(18) 0.18240(9) 0.48442(17) 0.0235(6) Uani 1 1 d . . . N3 N 0.56463(18) 0.13881(8) 0.59789(17) 0.0224(6) Uani 1 1 d . . . N4 N 0.61675(18) 0.09359(8) 0.70481(17) 0.0233(6) Uani 1 1 d . . . N5 N 0.67282(19) 0.04549(9) 0.80569(18) 0.0280(7) Uani 1 1 d . A . N6 N 0.4002(2) 0.15051(10) 0.66268(19) 0.0345(8) Uani 1 1 d . A . N7 N 0.64867(19) 0.13415(9) 0.24993(17) 0.0256(7) Uani 1 1 d . A . N8 N 0.73505(18) 0.13156(9) 0.37676(17) 0.0246(7) Uani 1 1 d . . . N9 N 0.81072(18) 0.12482(8) 0.50969(17) 0.0222(6) Uani 1 1 d . . . N10 N 0.87218(18) 0.11702(8) 0.64704(17) 0.0234(6) Uani 1 1 d . . . N11 N 0.92495(19) 0.10338(9) 0.78552(18) 0.0277(7) Uani 1 1 d . A . N12 N 0.9762(2) 0.11621(10) 0.44672(19) 0.0315(7) Uani 1 1 d . A . N13 N 0.68036(19) 0.22548(9) 0.31017(17) 0.0260(7) Uani 1 1 d . A . N14 N 0.70003(18) 0.21144(8) 0.45249(17) 0.0225(6) Uani 1 1 d . . . N15 N 0.72011(18) 0.19132(8) 0.59192(17) 0.0221(6) Uani 1 1 d . . . N16 N 0.73787(19) 0.16370(8) 0.72602(17) 0.0236(6) Uani 1 1 d . . . N17 N 0.74738(19) 0.13144(9) 0.85634(18) 0.0261(7) Uani 1 1 d . A . N18 N 0.7560(2) 0.27326(9) 0.64673(19) 0.0301(7) Uani 1 1 d . A . N19 N 0.46750(19) 0.13792(9) 0.30387(18) 0.0268(7) Uani 1 1 d . A . N20 N 0.55920(18) 0.10299(9) 0.40659(17) 0.0237(6) Uani 1 1 d . . . N21 N 0.65475(18) 0.07169(8) 0.51110(17) 0.0221(6) Uani 1 1 d . . . N22 N 0.75224(18) 0.04667(8) 0.62142(17) 0.0239(6) Uani 1 1 d . . . N23 N 0.84459(19) 0.02363(9) 0.73693(18) 0.0269(7) Uani 1 1 d . A . N24 N 0.6224(2) -0.00839(9) 0.4450(2) 0.0379(8) Uani 1 1 d . A . N25 N 0.5189(2) 0.20679(11) 0.1748(2) 0.0382(8) Uani 1 1 d . A . N26 N 0.8469(2) 0.04893(10) 0.9300(2) 0.0393(8) Uani 1 1 d . A . C1 C 0.4656(2) 0.26175(11) 0.3313(2) 0.0301(8) Uani 1 1 d . . . H1 H 0.4722 0.2658 0.2733 0.036 Uiso 1 1 calc R A . C2 C 0.4245(3) 0.29281(12) 0.3729(2) 0.0347(9) Uani 1 1 d . A . H2 H 0.4016 0.3175 0.3441 0.042 Uiso 1 1 calc R . . C3 C 0.4166(3) 0.28776(11) 0.4580(2) 0.0341(9) Uani 1 1 d . . . H3 H 0.3898 0.3094 0.4887 0.041 Uiso 1 1 calc R A . C4 C 0.4479(2) 0.25121(11) 0.4978(2) 0.0317(9) Uani 1 1 d . A . H4 H 0.4432 0.2474 0.5562 0.038 Uiso 1 1 calc R . . C5 C 0.4872(2) 0.21928(11) 0.4509(2) 0.0262(8) Uani 1 1 d . A . C6 C 0.5009(2) 0.16455(10) 0.5574(2) 0.0244(8) Uani 1 1 d . A . C7 C 0.4171(2) 0.16851(12) 0.5909(2) 0.0324(9) Uani 1 1 d . . . H7 H 0.3708 0.1848 0.5608 0.039 Uiso 1 1 calc R A . C8 C 0.4649(2) 0.12656(11) 0.7029(2) 0.0311(9) Uani 1 1 d . . . H8 H 0.4549 0.1147 0.7559 0.037 Uiso 1 1 calc R A . C9 C 0.5469(2) 0.11834(10) 0.6698(2) 0.0238(8) Uani 1 1 d . A . C10 C 0.6005(2) 0.05922(11) 0.7543(2) 0.0252(8) Uani 1 1 d . A . C11 C 0.5181(2) 0.03689(11) 0.7497(2) 0.0314(9) Uani 1 1 d . . . H11 H 0.4683 0.0460 0.7121 0.038 Uiso 1 1 calc R A . C12 C 0.5097(3) 0.00204(12) 0.7998(2) 0.0383(10) Uani 1 1 d . A . H12 H 0.4537 -0.0127 0.7981 0.046 Uiso 1 1 calc R . . C13 C 0.5838(3) -0.01173(12) 0.8531(3) 0.0408(10) Uani 1 1 d . . . H13 H 0.5793 -0.0358 0.8883 0.049 Uiso 1 1 calc R A . C14 C 0.6629(3) 0.01020(11) 0.8536(2) 0.0351(9) Uani 1 1 d . A . H14 H 0.7138 0.0004 0.8891 0.042 Uiso 1 1 calc R . . C15 C 0.6205(3) 0.11741(12) 0.1729(2) 0.0318(9) Uani 1 1 d . . . H15 H 0.5712 0.1305 0.1403 0.038 Uiso 1 1 calc R A . C16 C 0.6602(3) 0.08252(12) 0.1405(2) 0.0368(9) Uani 1 1 d . A . H16 H 0.6398 0.0719 0.0862 0.044 Uiso 1 1 calc R . . C17 C 0.7317(3) 0.06294(12) 0.1896(2) 0.0355(9) Uani 1 1 d . . . H17 H 0.7605 0.0387 0.1689 0.043 Uiso 1 1 calc R A . C18 C 0.7600(2) 0.07897(11) 0.2677(2) 0.0301(8) Uani 1 1 d . A . H18 H 0.8081 0.0656 0.3015 0.036 Uiso 1 1 calc R . . C19 C 0.7180(2) 0.11504(11) 0.2978(2) 0.0247(8) Uani 1 1 d . A . C20 C 0.8159(2) 0.12548(10) 0.4251(2) 0.0243(8) Uani 1 1 d . A . C21 C 0.9008(2) 0.12269(11) 0.3951(2) 0.0311(9) Uani 1 1 d . . . H21 H 0.9053 0.1255 0.3364 0.037 Uiso 1 1 calc R A . C22 C 0.9692(2) 0.11356(11) 0.5283(2) 0.0311(9) Uani 1 1 d . . . H22 H 1.0220 0.1074 0.5647 0.037 Uiso 1 1 calc R A . C23 C 0.8871(2) 0.11947(10) 0.5639(2) 0.0234(8) Uani 1 1 d . A . C24 C 0.9411(2) 0.12126(10) 0.7110(2) 0.0261(8) Uani 1 1 d . A . C25 C 1.0218(2) 0.14430(12) 0.7055(2) 0.0323(9) Uani 1 1 d . . . H25 H 1.0305 0.1595 0.6555 0.039 Uiso 1 1 calc R A . C26 C 1.0876(3) 0.14484(12) 0.7716(2) 0.0374(10) Uani 1 1 d . A . H26 H 1.1425 0.1598 0.7675 0.045 Uiso 1 1 calc R . . C27 C 1.0730(3) 0.12304(13) 0.8453(3) 0.0412(10) Uani 1 1 d . . . H27 H 1.1191 0.1216 0.8910 0.049 Uiso 1 1 calc R A . C28 C 0.9919(3) 0.10405(12) 0.8504(2) 0.0338(9) Uani 1 1 d . A . H28 H 0.9811 0.0905 0.9016 0.041 Uiso 1 1 calc R . . C29 C 0.7061(2) 0.24512(12) 0.2404(2) 0.0321(9) Uani 1 1 d . . . H29 H 0.6748 0.2382 0.1874 0.039 Uiso 1 1 calc R A . C30 C 0.7747(3) 0.27438(12) 0.2424(2) 0.0379(10) Uani 1 1 d . A . H30 H 0.7890 0.2882 0.1924 0.045 Uiso 1 1 calc R . . C31 C 0.8225(3) 0.28329(13) 0.3192(3) 0.0396(10) Uani 1 1 d . . . H31 H 0.8706 0.3033 0.3224 0.048 Uiso 1 1 calc R A . C32 C 0.8001(3) 0.26307(12) 0.3910(2) 0.0333(9) Uani 1 1 d . A . H32 H 0.8339 0.2686 0.4435 0.040 Uiso 1 1 calc R . . C33 C 0.7270(2) 0.23425(11) 0.3865(2) 0.0271(8) Uani 1 1 d . A . C34 C 0.7207(2) 0.22340(10) 0.5342(2) 0.0234(8) Uani 1 1 d . A . C35 C 0.7356(2) 0.26496(11) 0.5652(2) 0.0292(8) Uani 1 1 d . . . H35 H 0.7308 0.2880 0.5265 0.035 Uiso 1 1 calc R A . C36 C 0.7597(2) 0.24113(11) 0.7011(2) 0.0290(8) Uani 1 1 d . . . H36 H 0.7771 0.2466 0.7589 0.035 Uiso 1 1 calc R A . C37 C 0.7384(2) 0.19915(10) 0.6755(2) 0.0236(8) Uani 1 1 d . A . C38 C 0.7201(2) 0.16578(10) 0.8087(2) 0.0239(8) Uani 1 1 d . A . C39 C 0.6716(3) 0.19868(12) 0.8438(2) 0.0316(9) Uani 1 1 d . . . H39 H 0.6489 0.2216 0.8094 0.038 Uiso 1 1 calc R A . C40 C 0.6570(3) 0.19792(13) 0.9272(2) 0.0392(10) Uani 1 1 d . A . H40 H 0.6252 0.2204 0.9512 0.047 Uiso 1 1 calc R . . C41 C 0.6897(3) 0.16339(12) 0.9764(2) 0.0365(9) Uani 1 1 d . . . H41 H 0.6826 0.1624 1.0349 0.044 Uiso 1 1 calc R A . C42 C 0.7317(3) 0.13137(12) 0.9389(2) 0.0313(9) Uani 1 1 d . A . H42 H 0.7514 0.1075 0.9721 0.038 Uiso 1 1 calc R . . C43 C 0.3886(2) 0.14221(12) 0.2548(2) 0.0335(9) Uani 1 1 d . . . H43 H 0.3806 0.1667 0.2201 0.040 Uiso 1 1 calc R A . C44 C 0.3198(3) 0.11347(13) 0.2521(3) 0.0427(10) Uani 1 1 d . A . H44 H 0.2663 0.1173 0.2151 0.051 Uiso 1 1 calc R . . C45 C 0.3302(3) 0.07839(14) 0.3052(3) 0.0457(11) Uani 1 1 d . . . H45 H 0.2833 0.0579 0.3056 0.055 Uiso 1 1 calc R A . C46 C 0.4095(3) 0.07379(13) 0.3572(2) 0.0392(10) Uani 1 1 d . A . H46 H 0.4168 0.0502 0.3942 0.047 Uiso 1 1 calc R . . C47 C 0.4785(2) 0.10331(11) 0.3557(2) 0.0266(8) Uani 1 1 d . A . C48 C 0.5946(2) 0.06608(11) 0.4422(2) 0.0251(8) Uani 1 1 d . A . C49 C 0.5819(3) 0.02521(12) 0.4099(2) 0.0370(10) Uani 1 1 d . . . H49 H 0.5420 0.0214 0.3602 0.044 Uiso 1 1 calc R A . C50 C 0.6796(2) -0.00257(11) 0.5137(2) 0.0310(9) Uani 1 1 d . . . H50 H 0.7094 -0.0266 0.5395 0.037 Uiso 1 1 calc R A . C51 C 0.6975(2) 0.03742(10) 0.5493(2) 0.0237(8) Uani 1 1 d . A . C52 C 0.8195(2) 0.01944(10) 0.6531(2) 0.0279(8) Uani 1 1 d . A . C53 C 0.8656(3) -0.00873(12) 0.6057(2) 0.0359(9) Uani 1 1 d . . . H53 H 0.8518 -0.0098 0.5463 0.043 Uiso 1 1 calc R A . C54 C 0.9310(3) -0.03505(13) 0.6438(3) 0.0468(11) Uani 1 1 d . A . H54 H 0.9610 -0.0549 0.6114 0.056 Uiso 1 1 calc R . . C55 C 0.9528(3) -0.03229(13) 0.7295(3) 0.0501(12) Uani 1 1 d . . . H55 H 0.9964 -0.0508 0.7575 0.060 Uiso 1 1 calc R A . C56 C 0.9103(3) -0.00239(12) 0.7735(3) 0.0382(10) Uani 1 1 d . A . H56 H 0.9274 0.0004 0.8322 0.046 Uiso 1 1 calc R . . C57 C 0.5055(2) 0.23070(12) 0.1217(2) 0.0330(9) Uani 1 1 d . . . C58 C 0.8656(3) 0.02719(13) 0.9862(3) 0.0356(9) Uani 1 1 d . . . C59 C 0.1687(4) 0.15350(17) 0.4092(4) 0.0805(18) Uani 1 1 d . . . H59A H 0.1598 0.1386 0.3544 0.097 Uiso 1 1 calc R . . H59B H 0.1089 0.1636 0.4235 0.097 Uiso 1 1 calc R . . Cl1 Cl 0.23961(10) 0.19664(4) 0.40063(9) 0.0744(4) Uani 1 1 d . . . Cl2 Cl 0.21382(10) 0.11783(4) 0.48718(10) 0.0783(4) Uani 1 1 d . . . C60 C 0.2313(4) 0.0647(2) 0.6706(3) 0.0845(19) Uani 1 1 d . . . H60A H 0.2790 0.0565 0.6344 0.101 Uiso 1 1 calc R . . H60B H 0.2154 0.0947 0.6586 0.101 Uiso 1 1 calc R . . Cl3 Cl 0.27165(10) 0.05996(6) 0.77109(10) 0.0897(5) Uani 1 1 d . . . Cl4 Cl 0.13185(11) 0.03168(5) 0.64459(11) 0.0956(5) Uani 1 1 d . . . C61 C 0.3727(4) 0.14180(17) 1.0224(3) 0.0680(15) Uani 1 1 d D . . H61 H 0.3674 0.1678 1.0515 0.082 Uiso 1 1 calc R . . C62 C 0.3027(4) 0.1140(2) 1.0164(3) 0.0662(15) Uani 1 1 d D . . H62 H 0.2472 0.1209 1.0382 0.079 Uiso 1 1 calc R . . C63 C 0.3135(5) 0.0764(2) 0.9788(4) 0.091(2) Uani 1 1 d D . . H63 H 0.2667 0.0558 0.9753 0.109 Uiso 1 1 calc R . . C64 C 0.3962(6) 0.0683(2) 0.9446(4) 0.101(2) Uani 1 1 d D . . H64 H 0.4045 0.0421 0.9168 0.122 Uiso 1 1 calc R . . C65 C 0.4646(4) 0.0976(2) 0.9512(3) 0.0704(16) Uani 1 1 d D . . H65 H 0.5207 0.0918 0.9295 0.084 Uiso 1 1 calc R . . C66 C 0.4514(4) 0.1329(2) 0.9869(3) 0.0746(17) Uani 1 1 d D . . H66 H 0.4976 0.1538 0.9892 0.090 Uiso 1 1 calc R . . C67 C 0.8920(3) 0.1555(2) 0.1635(3) 0.0687(17) Uani 1 1 d . . . H67 H 0.8288 0.1562 0.1686 0.082 Uiso 1 1 calc R . . C68 C 0.9280(5) 0.12274(19) 0.1208(3) 0.0736(17) Uani 1 1 d . . . H68 H 0.8898 0.1005 0.0982 0.088 Uiso 1 1 calc R . . C69 C 1.0174(5) 0.1219(2) 0.1105(4) 0.0832(18) Uani 1 1 d . . . H69 H 1.0416 0.0994 0.0798 0.100 Uiso 1 1 calc R . . C70 C 1.0721(4) 0.1530(2) 0.1439(5) 0.088(2) Uani 1 1 d . . . H70 H 1.1348 0.1521 0.1365 0.105 Uiso 1 1 calc R . . C71 C 1.0397(5) 0.1854(2) 0.1879(4) 0.090(2) Uani 1 1 d . . . H71 H 1.0795 0.2069 0.2112 0.108 Uiso 1 1 calc R . . C72 C 0.9471(5) 0.18723(19) 0.1990(3) 0.0798(18) Uani 1 1 d . . . H72 H 0.9231 0.2096 0.2300 0.096 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 Cr1 0.0260(3) 0.0270(3) 0.0396(4) -0.0020(3) 0.0052(3) -0.0014(3) Cr2 0.0219(14) 0.0223(13) 0.032(3) -0.0024(15) 0.0043(16) 0.0005(9) Cr3 0.0215(19) 0.0210(19) 0.033(3) -0.0039(18) 0.0062(19) -0.0003(13) Cr4 0.0237(13) 0.0210(12) 0.030(2) -0.0022(14) 0.0034(15) 0.0003(9) Cr2' 0.0219(14) 0.0223(13) 0.032(3) -0.0024(15) 0.0043(16) 0.0005(9) Cr3' 0.0215(19) 0.0210(19) 0.033(3) -0.0039(18) 0.0062(19) -0.0003(13) Cr4' 0.0237(13) 0.0210(12) 0.030(2) -0.0022(14) 0.0034(15) 0.0003(9) Cr5 0.0273(3) 0.0276(3) 0.0405(4) -0.0048(3) 0.0026(3) -0.0009(3) S1 0.0551(7) 0.0423(6) 0.0392(6) 0.0036(5) -0.0040(5) 0.0013(5) S2 0.0469(7) 0.0671(8) 0.0477(7) 0.0205(6) 0.0064(5) 0.0106(6) N1 0.0215(15) 0.0230(15) 0.0253(17) 0.0038(12) -0.0015(12) 0.0021(12) N2 0.0232(15) 0.0249(15) 0.0221(16) 0.0028(12) 0.0001(12) 0.0061(13) N3 0.0223(15) 0.0217(14) 0.0226(16) -0.0006(12) -0.0015(12) 0.0022(12) N4 0.0236(16) 0.0236(15) 0.0224(16) 0.0039(12) 0.0000(12) 0.0035(13) N5 0.0296(17) 0.0238(15) 0.0301(17) 0.0037(13) -0.0003(13) -0.0010(13) N6 0.0322(18) 0.0386(18) 0.0337(19) 0.0078(15) 0.0087(14) 0.0097(15) N7 0.0302(17) 0.0252(16) 0.0217(16) 0.0007(13) 0.0028(13) -0.0006(13) N8 0.0205(15) 0.0247(15) 0.0283(17) 0.0021(13) 0.0006(13) 0.0019(13) N9 0.0219(15) 0.0187(14) 0.0263(16) 0.0016(12) 0.0032(12) 0.0009(12) N10 0.0231(15) 0.0218(15) 0.0247(16) 0.0010(12) -0.0006(12) 0.0020(12) N11 0.0268(17) 0.0249(16) 0.0298(18) 0.0024(13) -0.0052(13) 0.0011(13) N12 0.0269(17) 0.0376(18) 0.0302(19) -0.0027(14) 0.0029(14) 0.0032(14) N13 0.0265(16) 0.0271(16) 0.0243(17) 0.0055(13) 0.0024(13) 0.0000(13) N14 0.0216(15) 0.0232(15) 0.0220(16) 0.0045(12) -0.0009(12) -0.0023(12) N15 0.0201(15) 0.0221(15) 0.0236(16) 0.0022(12) -0.0008(12) 0.0023(12) N16 0.0254(16) 0.0237(15) 0.0212(16) 0.0008(12) -0.0009(12) 0.0008(13) N17 0.0247(16) 0.0270(16) 0.0258(17) 0.0017(13) -0.0025(13) -0.0004(13) N18 0.0324(18) 0.0265(16) 0.0308(19) 0.0009(14) -0.0002(14) -0.0008(14) N19 0.0247(16) 0.0306(16) 0.0239(16) 0.0029(13) -0.0036(13) 0.0017(13) N20 0.0229(16) 0.0245(15) 0.0230(16) 0.0029(12) -0.0009(12) -0.0011(13) N21 0.0224(15) 0.0224(15) 0.0215(16) 0.0022(12) 0.0025(12) 0.0017(12) N22 0.0251(16) 0.0236(15) 0.0221(16) 0.0018(12) -0.0025(12) 0.0020(13) N23 0.0278(16) 0.0223(15) 0.0294(18) 0.0050(13) -0.0028(13) 0.0034(13) N24 0.046(2) 0.0246(17) 0.040(2) -0.0039(15) -0.0108(16) -0.0020(15) N25 0.0343(19) 0.039(2) 0.041(2) 0.0034(17) 0.0003(16) -0.0036(16) N26 0.035(2) 0.0362(19) 0.045(2) 0.0017(17) -0.0048(16) 0.0020(16) C1 0.027(2) 0.031(2) 0.032(2) 0.0072(17) 0.0002(16) -0.0003(17) C2 0.032(2) 0.026(2) 0.044(3) 0.0052(18) -0.0029(18) 0.0034(17) C3 0.034(2) 0.026(2) 0.041(2) -0.0004(17) 0.0010(18) 0.0076(17) C4 0.026(2) 0.033(2) 0.036(2) -0.0022(17) 0.0028(16) 0.0031(17) C5 0.0171(17) 0.0264(19) 0.034(2) 0.0021(16) -0.0028(15) 0.0010(15) C6 0.0239(19) 0.0227(18) 0.026(2) -0.0004(15) -0.0003(15) 0.0018(15) C7 0.029(2) 0.035(2) 0.034(2) 0.0056(17) 0.0064(17) 0.0103(17) C8 0.035(2) 0.029(2) 0.031(2) 0.0052(16) 0.0102(17) 0.0044(17) C9 0.0275(19) 0.0216(17) 0.0216(19) -0.0004(15) -0.0007(15) 0.0010(15) C10 0.0269(19) 0.0255(18) 0.0235(19) 0.0004(15) 0.0034(15) 0.0009(16) C11 0.028(2) 0.029(2) 0.036(2) 0.0012(17) -0.0031(16) -0.0044(17) C12 0.035(2) 0.034(2) 0.045(3) 0.0031(19) 0.0002(19) -0.0079(18) C13 0.045(3) 0.030(2) 0.046(3) 0.0131(19) 0.001(2) -0.0029(19) C14 0.040(2) 0.028(2) 0.036(2) 0.0069(17) -0.0035(18) 0.0010(18) C15 0.037(2) 0.037(2) 0.021(2) 0.0059(17) 0.0007(16) -0.0068(18) C16 0.045(2) 0.038(2) 0.029(2) -0.0021(18) 0.0078(18) -0.007(2) C17 0.040(2) 0.029(2) 0.039(2) -0.0033(18) 0.0135(19) -0.0004(18) C18 0.029(2) 0.030(2) 0.031(2) -0.0003(16) 0.0036(16) 0.0010(17) C19 0.0251(19) 0.0268(18) 0.0228(19) 0.0039(15) 0.0046(15) -0.0037(16) C20 0.0257(19) 0.0205(17) 0.027(2) 0.0005(15) 0.0037(15) 0.0023(15) C21 0.027(2) 0.037(2) 0.030(2) 0.0011(17) 0.0062(16) 0.0046(17) C22 0.0219(19) 0.033(2) 0.037(2) -0.0028(17) -0.0034(16) 0.0049(16) C23 0.0221(18) 0.0196(17) 0.028(2) 0.0017(15) -0.0009(15) 0.0033(15) C24 0.0255(19) 0.0207(18) 0.031(2) -0.0015(15) -0.0032(16) 0.0049(15) C25 0.031(2) 0.030(2) 0.036(2) 0.0035(17) 0.0025(17) 0.0018(17) C26 0.033(2) 0.032(2) 0.045(3) 0.0034(19) -0.0072(19) -0.0067(18) C27 0.035(2) 0.045(2) 0.039(2) 0.005(2) -0.0143(19) -0.003(2) C28 0.033(2) 0.036(2) 0.030(2) 0.0036(17) -0.0077(17) -0.0005(18) C29 0.032(2) 0.038(2) 0.026(2) 0.0046(17) 0.0034(16) 0.0024(18) C30 0.039(2) 0.043(2) 0.032(2) 0.0078(19) 0.0070(18) -0.007(2) C31 0.033(2) 0.040(2) 0.046(3) 0.007(2) 0.0067(19) -0.0128(19) C32 0.032(2) 0.038(2) 0.030(2) 0.0023(17) -0.0005(17) -0.0069(18) C33 0.027(2) 0.0229(18) 0.032(2) 0.0002(16) 0.0039(16) 0.0023(16) C34 0.0190(17) 0.0243(18) 0.027(2) 0.0042(15) 0.0005(14) -0.0002(15) C35 0.032(2) 0.0239(19) 0.031(2) 0.0028(16) 0.0003(16) -0.0026(16) C36 0.030(2) 0.0280(19) 0.028(2) -0.0025(16) -0.0014(16) -0.0009(17) C37 0.0202(18) 0.0233(18) 0.027(2) -0.0006(15) -0.0008(15) 0.0046(15) C38 0.0259(19) 0.0229(18) 0.0221(19) -0.0025(15) -0.0024(15) -0.0057(15) C39 0.039(2) 0.029(2) 0.027(2) 0.0034(16) 0.0049(17) 0.0018(17) C40 0.045(3) 0.036(2) 0.038(2) -0.0087(19) 0.0114(19) 0.002(2) C41 0.045(2) 0.041(2) 0.024(2) 0.0001(18) 0.0045(18) -0.004(2) C42 0.034(2) 0.035(2) 0.025(2) 0.0047(17) 0.0014(16) -0.0018(18) C43 0.028(2) 0.040(2) 0.032(2) 0.0097(17) -0.0054(17) 0.0008(18) C44 0.026(2) 0.055(3) 0.044(3) 0.014(2) -0.0124(18) -0.006(2) C45 0.035(2) 0.050(3) 0.051(3) 0.010(2) -0.005(2) -0.014(2) C46 0.034(2) 0.039(2) 0.042(2) 0.0145(19) -0.0062(18) -0.0053(19) C47 0.026(2) 0.0287(19) 0.025(2) 0.0010(16) 0.0004(15) 0.0006(16) C48 0.0250(19) 0.0250(19) 0.025(2) 0.0015(15) 0.0012(15) 0.0003(15) C49 0.041(2) 0.028(2) 0.038(2) -0.0005(18) -0.0164(18) -0.0017(18) C50 0.031(2) 0.0259(19) 0.035(2) 0.0026(16) -0.0027(17) 0.0019(16) C51 0.0213(18) 0.0212(18) 0.029(2) 0.0024(15) 0.0042(15) 0.0015(15) C52 0.0259(19) 0.0200(18) 0.037(2) 0.0037(16) 0.0005(16) 0.0018(16) C53 0.040(2) 0.032(2) 0.034(2) -0.0033(17) -0.0045(18) 0.0087(18) C54 0.047(3) 0.040(2) 0.051(3) -0.011(2) -0.007(2) 0.020(2) C55 0.051(3) 0.042(2) 0.053(3) -0.001(2) -0.014(2) 0.024(2) C56 0.040(2) 0.035(2) 0.037(2) 0.0024(18) -0.0101(19) 0.0090(19) C57 0.027(2) 0.038(2) 0.033(2) -0.0111(19) 0.0012(17) -0.0026(18) C58 0.026(2) 0.042(2) 0.039(2) -0.008(2) 0.0052(18) -0.0040(19) C59 0.059(3) 0.083(4) 0.096(4) 0.042(3) -0.013(3) -0.026(3) Cl1 0.0769(10) 0.0531(7) 0.0930(11) 0.0249(7) 0.0077(8) -0.0088(7) Cl2 0.0662(9) 0.0645(8) 0.1005(11) 0.0320(8) -0.0109(8) -0.0115(7) C60 0.080(4) 0.107(5) 0.071(4) 0.028(3) 0.028(3) 0.023(4) Cl3 0.0725(10) 0.1145(13) 0.0822(11) 0.0214(9) 0.0073(8) 0.0057(9) Cl4 0.0799(11) 0.0849(11) 0.1164(14) 0.0128(10) -0.0189(9) 0.0027(9) C61 0.081(4) 0.064(3) 0.055(3) -0.012(3) -0.019(3) 0.022(3) C62 0.059(4) 0.103(5) 0.035(3) 0.006(3) -0.001(2) 0.029(4) C63 0.096(5) 0.094(5) 0.074(4) 0.040(4) -0.034(4) -0.046(4) C64 0.151(7) 0.089(5) 0.058(4) -0.021(3) -0.020(4) 0.033(5) C65 0.057(4) 0.113(5) 0.040(3) -0.010(3) 0.003(3) 0.011(4) C66 0.061(4) 0.105(5) 0.053(4) 0.018(3) -0.019(3) -0.013(4) C67 0.042(3) 0.100(5) 0.061(4) 0.046(3) -0.006(3) -0.019(3) C68 0.092(5) 0.076(4) 0.049(3) 0.019(3) -0.011(3) -0.022(4) C69 0.101(5) 0.066(4) 0.083(4) 0.032(3) 0.011(4) 0.017(4) C70 0.051(4) 0.084(5) 0.127(6) 0.050(4) 0.004(4) 0.012(4) C71 0.081(5) 0.087(5) 0.095(5) 0.019(4) -0.017(4) -0.036(4) C72 0.112(5) 0.074(4) 0.056(4) 0.022(3) 0.016(3) 0.016(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 Cr1 N19 2.090(3) . ? Cr1 Cr2 2.093(6) . ? Cr1 N1 2.100(3) . ? Cr1 N13 2.103(3) . ? Cr1 N7 2.116(3) . ? Cr1 N25 2.220(3) . ? Cr1 Cr2' 2.449(7) . ? Cr2 N2 2.021(8) . ? Cr2 N20 2.027(8) . ? Cr2 N14 2.027(8) . ? Cr2 N8 2.037(8) . ? Cr2 Cr3 2.566(12) . ? Cr3 Cr4 1.933(13) . ? Cr3 N9 2.032(13) . ? Cr3 N21 2.033(13) . ? Cr3 N3 2.043(13) . ? Cr3 N15 2.049(13) . ? Cr4 N16 2.031(8) . ? Cr4 N10 2.034(7) . ? Cr4 N4 2.034(7) . ? Cr4 N22 2.036(7) . ? Cr4 Cr5 2.492(6) . ? Cr2' Cr3' 1.924(13) . ? Cr2' N2 2.019(12) . ? Cr2' N14 2.019(12) . ? Cr2' N8 2.024(12) . ? Cr2' N20 2.027(12) . ? Cr3' N3 2.026(19) . ? Cr3' N15 2.030(19) . ? Cr3' N21 2.046(19) . ? Cr3' N9 2.051(19) . ? Cr3' Cr4' 2.588(13) . ? Cr4' N10 2.038(11) . ? Cr4' N16 2.042(11) . ? Cr4' N4 2.043(11) . ? Cr4' N22 2.049(11) . ? Cr4' Cr5 2.124(6) . ? Cr5 N23 2.095(3) . ? Cr5 N5 2.107(3) . ? Cr5 N11 2.109(3) . ? Cr5 N17 2.134(3) . ? Cr5 N26 2.206(3) . ? S1 C57 1.643(4) . ? S2 C58 1.631(5) . ? N1 C1 1.352(4) . ? N1 C5 1.358(4) . ? N2 C6 1.373(4) . ? N2 C5 1.377(4) . ? N3 C6 1.361(4) . ? N3 C9 1.364(4) . ? N4 C9 1.372(4) . ? N4 C10 1.374(4) . ? N5 C10 1.357(4) . ? N5 C14 1.365(4) . ? N6 C7 1.324(4) . ? N6 C8 1.336(4) . ? N7 C19 1.361(4) . ? N7 C15 1.365(4) . ? N8 C19 1.364(4) . ? N8 C20 1.376(4) . ? N9 C20 1.360(4) . ? N9 C23 1.368(4) . ? N10 C23 1.369(4) . ? N10 C24 1.380(4) . ? N11 C24 1.359(4) . ? N11 C28 1.364(4) . ? N12 C22 1.319(4) . ? N12 C21 1.339(5) . ? N13 C29 1.361(4) . ? N13 C33 1.369(4) . ? N14 C34 1.364(4) . ? N14 C33 1.367(4) . ? N15 C37 1.359(4) . ? N15 C34 1.368(4) . ? N16 C38 1.373(4) . ? N16 C37 1.377(4) . ? N17 C42 1.360(4) . ? N17 C38 1.360(4) . ? N18 C36 1.331(4) . ? N18 C35 1.334(4) . ? N19 C43 1.352(4) . ? N19 C47 1.368(4) . ? N20 C48 1.375(4) . ? N20 C47 1.381(4) . ? N21 C48 1.359(4) . ? N21 C51 1.365(4) . ? N22 C51 1.374(4) . ? N22 C52 1.375(4) . ? N23 C52 1.360(4) . ? N23 C56 1.361(4) . ? N24 C49 1.316(5) . ? N24 C50 1.332(5) . ? N25 C57 1.137(5) . ? N26 C58 1.142(5) . ? C1 C2 1.359(5) . ? C2 C3 1.384(5) . ? C3 C4 1.373(5) . ? C4 C5 1.413(5) . ? C6 C7 1.406(5) . ? C8 C9 1.398(5) . ? C10 C11 1.408(5) . ? C11 C12 1.370(5) . ? C12 C13 1.393(5) . ? C13 C14 1.362(5) . ? C15 C16 1.372(5) . ? C16 C17 1.399(5) . ? C17 C18 1.373(5) . ? C18 C19 1.403(5) . ? C20 C21 1.394(5) . ? C22 C23 1.407(5) . ? C24 C25 1.411(5) . ? C25 C26 1.366(5) . ? C26 C27 1.398(5) . ? C27 C28 1.355(5) . ? C29 C30 1.371(5) . ? C30 C31 1.384(5) . ? C31 C32 1.380(5) . ? C32 C33 1.411(5) . ? C34 C35 1.408(5) . ? C36 C37 1.410(5) . ? C38 C39 1.409(5) . ? C39 C40 1.370(5) . ? C40 C41 1.400(5) . ? C41 C42 1.356(5) . ? C43 C44 1.362(5) . ? C44 C45 1.391(5) . ? C45 C46 1.381(5) . ? C46 C47 1.385(5) . ? C48 C49 1.392(5) . ? C50 C51 1.397(5) . ? C52 C53 1.389(5) . ? C53 C54 1.374(5) . ? C54 C55 1.378(6) . ? C55 C56 1.365(5) . ? C59 Cl1 1.732(5) . ? C59 Cl2 1.760(5) . ? C60 Cl3 1.663(6) . ? C60 Cl4 1.821(6) . ? C61 C62 1.356(7) . ? C61 C66 1.376(7) . ? C62 C63 1.343(8) . ? C63 C64 1.415(8) . ? C64 C65 1.369(8) . ? C65 C66 1.272(7) . ? C67 C68 1.372(8) . ? C67 C72 1.379(8) . ? C68 C69 1.355(8) . ? C69 C70 1.348(8) . ? C70 C71 1.355(9) . ? C71 C72 1.406(8) . ? 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 N19 Cr1 Cr2 87.7(2) . . ? N19 Cr1 N1 89.83(11) . . ? Cr2 Cr1 N1 86.0(2) . . ? N19 Cr1 N13 174.18(11) . . ? Cr2 Cr1 N13 86.5(2) . . ? N1 Cr1 N13 89.20(11) . . ? N19 Cr1 N7 87.38(11) . . ? Cr2 Cr1 N7 85.8(2) . . ? N1 Cr1 N7 171.41(11) . . ? N13 Cr1 N7 92.75(11) . . ? N19 Cr1 N25 93.33(11) . . ? Cr2 Cr1 N25 178.5(2) . . ? N1 Cr1 N25 95.05(12) . . ? N13 Cr1 N25 92.48(11) . . ? N7 Cr1 N25 93.22(12) . . ? N19 Cr1 Cr2' 87.7(3) . . ? Cr2 Cr1 Cr2' 0.2(6) . . ? N1 Cr1 Cr2' 86.2(3) . . ? N13 Cr1 Cr2' 86.5(3) . . ? N7 Cr1 Cr2' 85.6(3) . . ? N25 Cr1 Cr2' 178.4(3) . . ? N2 Cr2 N20 89.9(3) . . ? N2 Cr2 N14 89.3(3) . . ? N20 Cr2 N14 168.6(4) . . ? N2 Cr2 N8 167.5(4) . . ? N20 Cr2 N8 88.9(3) . . ? N14 Cr2 N8 89.5(3) . . ? N2 Cr2 Cr1 96.7(3) . . ? N20 Cr2 Cr1 94.9(3) . . ? N14 Cr2 Cr1 96.5(3) . . ? N8 Cr2 Cr1 95.7(3) . . ? N2 Cr2 Cr3 84.8(4) . . ? N20 Cr2 Cr3 84.0(4) . . ? N14 Cr2 Cr3 84.5(4) . . ? N8 Cr2 Cr3 82.7(4) . . ? Cr1 Cr2 Cr3 178.2(5) . . ? Cr4 Cr3 N9 92.8(5) . . ? Cr4 Cr3 N21 94.2(5) . . ? N9 Cr3 N21 89.4(5) . . ? Cr4 Cr3 N3 94.7(5) . . ? N9 Cr3 N3 172.4(5) . . ? N21 Cr3 N3 91.6(5) . . ? Cr4 Cr3 N15 94.8(5) . . ? N9 Cr3 N15 89.6(5) . . ? N21 Cr3 N15 170.9(5) . . ? N3 Cr3 N15 88.3(5) . . ? Cr4 Cr3 Cr2 179.8(8) . . ? N9 Cr3 Cr2 87.2(4) . . ? N21 Cr3 Cr2 85.6(4) . . ? N3 Cr3 Cr2 85.3(4) . . ? N15 Cr3 Cr2 85.3(4) . . ? Cr3 Cr4 N16 93.0(5) . . ? Cr3 Cr4 N10 95.2(5) . . ? N16 Cr4 N10 89.7(3) . . ? Cr3 Cr4 N4 93.0(5) . . ? N16 Cr4 N4 88.9(3) . . ? N10 Cr4 N4 171.7(4) . . ? Cr3 Cr4 N22 93.8(5) . . ? N16 Cr4 N22 173.2(4) . . ? N10 Cr4 N22 88.8(3) . . ? N4 Cr4 N22 91.7(3) . . ? Cr3 Cr4 Cr5 177.6(5) . . ? N16 Cr4 Cr5 88.1(2) . . ? N10 Cr4 Cr5 86.8(2) . . ? N4 Cr4 Cr5 85.0(2) . . ? N22 Cr4 Cr5 85.1(2) . . ? Cr3' Cr2' N2 94.4(7) . . ? Cr3' Cr2' N14 94.5(7) . . ? N2 Cr2' N14 89.6(5) . . ? Cr3' Cr2' N8 93.3(7) . . ? N2 Cr2' N8 172.3(4) . . ? N14 Cr2' N8 90.1(5) . . ? Cr3' Cr2' N20 94.2(7) . . ? N2 Cr2' N20 89.9(5) . . ? N14 Cr2' N20 171.2(4) . . ? N8 Cr2' N20 89.2(5) . . ? Cr3' Cr2' Cr1 178.8(8) . . ? N2 Cr2' Cr1 86.4(3) . . ? N14 Cr2' Cr1 86.4(3) . . ? N8 Cr2' Cr1 85.9(3) . . ? N20 Cr2' Cr1 84.9(3) . . ? Cr2' Cr3' N3 93.8(7) . . ? Cr2' Cr3' N15 93.7(7) . . ? N3 Cr3' N15 89.2(8) . . ? Cr2' Cr3' N21 93.4(8) . . ? N3 Cr3' N21 91.7(8) . . ? N15 Cr3' N21 172.8(7) . . ? Cr2' Cr3' N9 94.9(8) . . ? N3 Cr3' N9 171.3(7) . . ? N15 Cr3' N9 89.5(7) . . ? N21 Cr3' N9 88.5(7) . . ? Cr2' Cr3' Cr4' 179.1(11) . . ? N3 Cr3' Cr4' 86.7(6) . . ? N15 Cr3' Cr4' 87.1(6) . . ? N21 Cr3' Cr4' 85.9(5) . . ? N9 Cr3' Cr4' 84.6(5) . . ? N10 Cr4' N16 89.3(4) . . ? N10 Cr4' N4 167.5(3) . . ? N16 Cr4' N4 88.3(4) . . ? N10 Cr4' N22 88.3(4) . . ? N16 Cr4' N22 166.0(3) . . ? N4 Cr4' N22 91.0(4) . . ? N10 Cr4' Cr5 97.4(4) . . ? N16 Cr4' Cr5 98.8(4) . . ? N4 Cr4' Cr5 95.1(4) . . ? N22 Cr4' Cr5 95.2(4) . . ? N10 Cr4' Cr3' 84.9(5) . . ? N16 Cr4' Cr3' 82.3(5) . . ? N4 Cr4' Cr3' 82.6(5) . . ? N22 Cr4' Cr3' 83.7(5) . . ? Cr5 Cr4' Cr3' 177.4(6) . . ? N23 Cr5 N5 89.37(11) . . ? N23 Cr5 N11 85.55(11) . . ? N5 Cr5 N11 171.70(11) . . ? N23 Cr5 Cr4' 87.4(3) . . ? N5 Cr5 Cr4' 86.9(3) . . ? N11 Cr5 Cr4' 86.3(3) . . ? N23 Cr5 N17 171.28(11) . . ? N5 Cr5 N17 90.26(11) . . ? N11 Cr5 N17 93.77(11) . . ? Cr4' Cr5 N17 83.9(3) . . ? N23 Cr5 N26 95.33(11) . . ? N5 Cr5 N26 92.01(11) . . ? N11 Cr5 N26 94.98(12) . . ? Cr4' Cr5 N26 177.1(3) . . ? N17 Cr5 N26 93.39(11) . . ? N23 Cr5 Cr4 87.19(18) . . ? N5 Cr5 Cr4 86.62(18) . . ? N11 Cr5 Cr4 86.58(18) . . ? Cr4' Cr5 Cr4 0.4(5) . . ? N17 Cr5 Cr4 84.09(18) . . ? N26 Cr5 Cr4 177.13(19) . . ? C1 N1 C5 118.3(3) . . ? C1 N1 Cr1 120.0(2) . . ? C5 N1 Cr1 121.4(2) . . ? C6 N2 C5 122.9(3) . . ? C6 N2 Cr2' 115.0(3) . . ? C5 N2 Cr2' 121.5(3) . . ? C6 N2 Cr2 124.1(3) . . ? C5 N2 Cr2 112.8(3) . . ? Cr2' N2 Cr2 10.1(3) . . ? C6 N3 C9 119.9(3) . . ? C6 N3 Cr3' 116.4(4) . . ? C9 N3 Cr3' 123.7(4) . . ? C6 N3 Cr3 124.2(3) . . ? C9 N3 Cr3 115.8(3) . . ? Cr3' N3 Cr3 8.1(5) . . ? C9 N4 C10 120.9(3) . . ? C9 N4 Cr4 115.9(3) . . ? C10 N4 Cr4 122.8(3) . . ? C9 N4 Cr4' 125.0(3) . . ? C10 N4 Cr4' 114.0(3) . . ? Cr4 N4 Cr4' 10.4(3) . . ? C10 N5 C14 118.4(3) . . ? C10 N5 Cr5 120.9(2) . . ? C14 N5 Cr5 120.6(2) . . ? C7 N6 C8 118.0(3) . . ? C19 N7 C15 118.9(3) . . ? C19 N7 Cr1 120.8(2) . . ? C15 N7 Cr1 119.5(2) . . ? C19 N8 C20 122.6(3) . . ? C19 N8 Cr2' 120.7(3) . . ? C20 N8 Cr2' 115.5(3) . . ? C19 N8 Cr2 112.6(3) . . ? C20 N8 Cr2 124.5(3) . . ? Cr2' N8 Cr2 10.0(3) . . ? C20 N9 C23 120.4(3) . . ? C20 N9 Cr3 122.1(3) . . ? C23 N9 Cr3 117.4(3) . . ? C20 N9 Cr3' 114.6(4) . . ? C23 N9 Cr3' 125.0(4) . . ? Cr3 N9 Cr3' 8.1(5) . . ? C23 N10 C24 122.2(3) . . ? C23 N10 Cr4 114.3(3) . . ? C24 N10 Cr4 123.5(3) . . ? C23 N10 Cr4' 123.7(3) . . ? C24 N10 Cr4' 113.8(3) . . ? Cr4 N10 Cr4' 10.4(3) . . ? C24 N11 C28 118.7(3) . . ? C24 N11 Cr5 122.5(2) . . ? C28 N11 Cr5 118.7(2) . . ? C22 N12 C21 118.4(3) . . ? C29 N13 C33 118.6(3) . . ? C29 N13 Cr1 120.6(2) . . ? C33 N13 Cr1 120.8(2) . . ? C34 N14 C33 122.5(3) . . ? C34 N14 Cr2' 114.2(3) . . ? C33 N14 Cr2' 123.2(3) . . ? C34 N14 Cr2 123.1(3) . . ? C33 N14 Cr2 114.4(3) . . ? Cr2' N14 Cr2 10.1(3) . . ? C37 N15 C34 120.9(3) . . ? C37 N15 Cr3' 123.0(4) . . ? C34 N15 Cr3' 115.9(4) . . ? C37 N15 Cr3 115.5(3) . . ? C34 N15 Cr3 123.6(3) . . ? Cr3' N15 Cr3 8.1(5) . . ? C38 N16 C37 122.4(3) . . ? C38 N16 Cr4 120.0(3) . . ? C37 N16 Cr4 116.5(3) . . ? C38 N16 Cr4' 111.3(3) . . ? C37 N16 Cr4' 126.0(3) . . ? Cr4 N16 Cr4' 10.4(3) . . ? C42 N17 C38 118.2(3) . . ? C42 N17 Cr5 118.3(2) . . ? C38 N17 Cr5 123.1(2) . . ? C36 N18 C35 118.6(3) . . ? C43 N19 C47 118.4(3) . . ? C43 N19 Cr1 121.3(2) . . ? C47 N19 Cr1 120.3(2) . . ? C48 N20 C47 121.6(3) . . ? C48 N20 Cr2' 114.2(3) . . ? C47 N20 Cr2' 124.1(3) . . ? C48 N20 Cr2 123.0(3) . . ? C47 N20 Cr2 115.2(3) . . ? Cr2' N20 Cr2 10.1(3) . . ? C48 N21 C51 120.0(3) . . ? C48 N21 Cr3 123.9(3) . . ? C51 N21 Cr3 116.1(3) . . ? C48 N21 Cr3' 116.1(4) . . ? C51 N21 Cr3' 123.8(4) . . ? Cr3 N21 Cr3' 8.1(5) . . ? C51 N22 C52 121.7(3) . . ? C51 N22 Cr4 115.8(3) . . ? C52 N22 Cr4 121.9(3) . . ? C51 N22 Cr4' 125.3(3) . . ? C52 N22 Cr4' 112.9(3) . . ? Cr4 N22 Cr4' 10.3(3) . . ? C52 N23 C56 118.7(3) . . ? C52 N23 Cr5 121.1(2) . . ? C56 N23 Cr5 119.5(2) . . ? C49 N24 C50 117.9(3) . . ? C57 N25 Cr1 157.5(3) . . ? C58 N26 Cr5 165.0(3) . . ? N1 C1 C2 123.5(3) . . ? C1 C2 C3 118.8(3) . . ? C4 C3 C2 119.5(4) . . ? C3 C4 C5 119.4(4) . . ? N1 C5 N2 114.6(3) . . ? N1 C5 C4 120.4(3) . . ? N2 C5 C4 124.7(3) . . ? N3 C6 N2 114.8(3) . . ? N3 C6 C7 118.2(3) . . ? N2 C6 C7 127.0(3) . . ? N6 C7 C6 122.7(3) . . ? N6 C8 C9 122.3(3) . . ? N3 C9 N4 114.3(3) . . ? N3 C9 C8 118.5(3) . . ? N4 C9 C8 127.0(3) . . ? N5 C10 N4 115.2(3) . . ? N5 C10 C11 120.3(3) . . ? N4 C10 C11 124.3(3) . . ? C12 C11 C10 119.9(3) . . ? C11 C12 C13 119.7(4) . . ? C14 C13 C12 118.3(4) . . ? C13 C14 N5 123.4(4) . . ? N7 C15 C16 122.9(4) . . ? C15 C16 C17 118.2(4) . . ? C18 C17 C16 119.7(4) . . ? C17 C18 C19 120.1(3) . . ? N7 C19 N8 114.4(3) . . ? N7 C19 C18 120.2(3) . . ? N8 C19 C18 125.2(3) . . ? N9 C20 N8 115.3(3) . . ? N9 C20 C21 118.8(3) . . ? N8 C20 C21 125.8(3) . . ? N12 C21 C20 121.8(3) . . ? N12 C22 C23 123.0(3) . . ? N9 C23 N10 114.7(3) . . ? N9 C23 C22 117.3(3) . . ? N10 C23 C22 127.8(3) . . ? N11 C24 N10 115.2(3) . . ? N11 C24 C25 119.4(3) . . ? N10 C24 C25 125.3(3) . . ? C26 C25 C24 120.4(4) . . ? C25 C26 C27 119.1(4) . . ? C28 C27 C26 118.6(4) . . ? C27 C28 N11 123.3(4) . . ? N13 C29 C30 123.6(3) . . ? C29 C30 C31 118.2(3) . . ? C32 C31 C30 119.9(4) . . ? C31 C32 C33 120.1(3) . . ? N14 C33 N13 114.8(3) . . ? N14 C33 C32 125.5(3) . . ? N13 C33 C32 119.7(3) . . ? N14 C34 N15 115.1(3) . . ? N14 C34 C35 127.3(3) . . ? N15 C34 C35 117.4(3) . . ? N18 C35 C34 122.5(3) . . ? N18 C36 C37 122.0(3) . . ? N15 C37 N16 114.6(3) . . ? N15 C37 C36 118.2(3) . . ? N16 C37 C36 127.2(3) . . ? N17 C38 N16 115.2(3) . . ? N17 C38 C39 119.8(3) . . ? N16 C38 C39 124.8(3) . . ? C40 C39 C38 120.7(3) . . ? C39 C40 C41 118.6(4) . . ? C42 C41 C40 118.6(4) . . ? C41 C42 N17 123.8(3) . . ? N19 C43 C44 123.8(3) . . ? C43 C44 C45 118.1(4) . . ? C46 C45 C44 119.1(4) . . ? C45 C46 C47 120.5(4) . . ? N19 C47 N20 114.0(3) . . ? N19 C47 C46 120.0(3) . . ? N20 C47 C46 125.9(3) . . ? N21 C48 N20 114.8(3) . . ? N21 C48 C49 118.3(3) . . ? N20 C48 C49 126.6(3) . . ? N24 C49 C48 123.1(3) . . ? N24 C50 C51 122.7(3) . . ? N21 C51 N22 114.7(3) . . ? N21 C51 C50 117.9(3) . . ? N22 C51 C50 127.3(3) . . ? N23 C52 N22 114.9(3) . . ? N23 C52 C53 119.7(3) . . ? N22 C52 C53 125.2(3) . . ? C54 C53 C52 120.6(4) . . ? C53 C54 C55 119.3(4) . . ? C56 C55 C54 118.6(4) . . ? N23 C56 C55 122.8(4) . . ? N25 C57 S1 179.0(4) . . ? N26 C58 S2 178.7(4) . . ? Cl1 C59 Cl2 111.4(3) . . ? Cl3 C60 Cl4 112.1(3) . . ? C62 C61 C66 121.0(5) . . ? C63 C62 C61 118.4(5) . . ? C62 C63 C64 118.5(6) . . ? C65 C64 C63 120.9(6) . . ? C66 C65 C64 118.6(6) . . ? C65 C66 C61 122.4(6) . . ? C68 C67 C72 120.3(5) . . ? C69 C68 C67 120.6(6) . . ? C70 C69 C68 119.8(6) . . ? C69 C70 C71 121.6(6) . . ? C70 C71 C72 119.8(6) . . ? C67 C72 C71 117.9(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.995 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.102