Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Four quadruple metal-metal bonds lined up: Linear nonachromium(II) metal string complexes ; _publ_contact_author_name 'Shie-Ming Peng' _publ_contact_author_email SMPENG@NTU.EDU.TW loop_ _publ_author_name 'Shie-Ming Peng' R.H.Ismayilov 'Gene-Hsiang Lee' 'Rui-Ren Wang' ; Wen-Zhen Wang ; 'Chen-Yu Yeh' data_ic11235 _database_code_depnum_ccdc_archive 'CCDC 623204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C124 H114 Cl2 Cr9 N40 O' _chemical_formula_weight 2719.45 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 44.392(3) _cell_length_b 14.3963(10) _cell_length_c 18.6471(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.391(4) _cell_angle_gamma 90.00 _cell_volume 11864.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5584 _exptl_absorpt_coefficient_mu 0.907 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.998 _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 46502 _diffrn_reflns_av_R_equivalents 0.1001 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10382 _reflns_number_gt 4710 _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 ; We examined the structure and concluded that the C2/c option is better than the Cc option for the following reasons: (1)The intensities statistics shows this structure is super centrics. (mean \/cxE2-1\/cxis 1.148 where 0.968 is expected for centrosym and 0.736 for non-centrosym.) (2)We solved structure by C2/c and Cc options and checked with check CIF/PLATON report. The reports of C2/c option only give several alerts in level C, but the reports of Cc option give alerts in level A & B (detection the centre of symmetry and many others). We also checked the bond distances and angles, C2/c option is more meaningful than the Cc option. The coordinates and anisotropic thermal ellipsoids of solvent molecules for benzene and hexane (C49-C54 and C55-C60) were refined. Solvent molecules of ether (O1, C61, C61' and C62) were included in the calculatins but were not refined, and the occupancies of solvent atoms O1, C61 and C61' were set to 0.5. 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^)+(0.1090P)^2^+51.0938P] 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 10382 _refine_ls_number_parameters 771 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1884 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2618 _refine_ls_wR_factor_gt 0.1929 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.20230(3) 0.62995(8) 0.29514(6) 0.0468(4) Uani 1 1 d . . . Cr3 Cr 0.10001(3) 0.63382(8) 0.26977(6) 0.0469(4) Uani 1 1 d . . . Cr2 Cr 0.15486(8) 0.6297(2) 0.28289(17) 0.0391(10) Uiso 0.50 1 d P . 1 Cr4 Cr 0.05423(7) 0.6359(2) 0.25905(16) 0.0379(10) Uiso 0.50 1 d P . 1 Cr2' Cr 0.14630(8) 0.6321(2) 0.28129(17) 0.0406(11) Uiso 0.50 1 d P . 2 Cr4' Cr 0.04563(8) 0.6360(2) 0.25783(17) 0.0392(10) Uiso 0.50 1 d P . 2 Cr5 Cr 0.0000 0.63614(12) 0.2500 0.0477(5) Uani 1 2 d S . . Cl1 Cl 0.25978(4) 0.63368(13) 0.30767(10) 0.0504(5) Uani 1 1 d . . . N1 N 0.19795(13) 0.4862(4) 0.3138(3) 0.0435(15) Uani 1 1 d . . . N2 N 0.14861(12) 0.5100(4) 0.3372(3) 0.0407(15) Uani 1 1 d . . . N3 N 0.09931(12) 0.5427(4) 0.3547(3) 0.0397(14) Uani 1 1 d . . . N4 N 0.04999(12) 0.5902(4) 0.3612(3) 0.0421(15) Uani 1 1 d . . . N5 N 0.00012(12) 0.6380(4) 0.3592(3) 0.0372(14) Uani 1 1 d . . . N6 N -0.04947(12) 0.6841(4) 0.3436(3) 0.0429(15) Uani 1 1 d . . . N7 N -0.09971(12) 0.7224(4) 0.3167(3) 0.0375(14) Uani 1 1 d . . . N8 N -0.14974(13) 0.7490(4) 0.2763(3) 0.0420(15) Uani 1 1 d . . . N9 N -0.19798(12) 0.7734(4) 0.2237(3) 0.0420(15) Uani 1 1 d . . . N10 N 0.00278(17) 0.6393(5) 0.5074(4) 0.072(2) Uani 1 1 d . . . N11 N 0.19856(13) 0.6589(4) 0.4042(3) 0.0434(15) Uani 1 1 d . . . N12 N 0.14972(12) 0.7056(4) 0.3738(3) 0.0425(15) Uani 1 1 d . . . N13 N 0.09996(12) 0.7460(4) 0.3375(3) 0.0404(14) Uani 1 1 d . . . N14 N 0.05012(13) 0.7688(4) 0.2939(3) 0.0439(15) Uani 1 1 d . . . N15 N 0.0000 0.7772(6) 0.2500 0.040(2) Uani 1 2 d S . . N16 N 0.0000 0.9682(8) 0.2500 0.089(4) Uani 1 2 d S . . N17 N 0.19943(13) 0.6005(4) 0.1837(3) 0.0416(14) Uani 1 1 d . . . N18 N 0.14962(12) 0.5552(4) 0.1899(3) 0.0400(14) Uani 1 1 d . . . N19 N 0.09954(13) 0.5212(4) 0.2020(3) 0.0397(14) Uani 1 1 d . . . N20 N 0.04956(12) 0.5028(4) 0.2233(3) 0.0395(14) Uani 1 1 d . . . N21 N 0.0000 0.4949(6) 0.2500 0.039(2) Uani 1 2 d S . . N22 N 0.0000 0.3032(8) 0.2500 0.084(3) Uani 1 2 d S . . C1 C 0.22104(17) 0.4291(6) 0.2995(4) 0.050(2) Uani 1 1 d . . . H1A H 0.2399 0.4562 0.2914 0.060 Uiso 1 1 calc R . . C2 C 0.21832(18) 0.3345(6) 0.2963(4) 0.059(2) Uani 1 1 d . . . H2A H 0.2350 0.2970 0.2862 0.070 Uiso 1 1 calc R . . C3 C 0.19078(19) 0.2941(6) 0.3081(4) 0.061(2) Uani 1 1 d . . . H3A H 0.1884 0.2285 0.3062 0.073 Uiso 1 1 calc R . . C4 C 0.16704(18) 0.3500(5) 0.3225(4) 0.052(2) Uani 1 1 d . . . H4A H 0.1479 0.3236 0.3296 0.063 Uiso 1 1 calc R . . C5 C 0.17122(16) 0.4466(5) 0.3267(4) 0.0424(18) Uani 1 1 d . . . C6 C 0.12393(15) 0.4883(5) 0.3729(4) 0.0409(18) Uani 1 1 d . . . C7 C 0.12273(16) 0.4209(5) 0.4262(4) 0.0468(19) Uani 1 1 d . . . H7A H 0.1399 0.3830 0.4396 0.056 Uiso 1 1 calc R . . C8 C 0.09674(17) 0.4099(6) 0.4592(4) 0.055(2) Uani 1 1 d . . . H8A H 0.0956 0.3629 0.4946 0.066 Uiso 1 1 calc R . . C9 C 0.07214(16) 0.4665(6) 0.4413(4) 0.052(2) Uani 1 1 d . . . H9A H 0.0543 0.4597 0.4651 0.062 Uiso 1 1 calc R . . C10 C 0.07356(15) 0.5330(5) 0.3887(4) 0.0416(18) Uani 1 1 d . . . C11 C 0.02592(16) 0.6115(5) 0.3994(4) 0.0442(18) Uani 1 1 d . . . C12 C 0.02667(16) 0.6153(6) 0.4742(4) 0.051(2) Uani 1 1 d . . . H12A H 0.0450 0.6000 0.5024 0.061 Uiso 1 1 calc R . . C13 C -0.02295(16) 0.6669(5) 0.4653(4) 0.0466(19) Uani 1 1 d . . . H13A H -0.0400 0.6876 0.4882 0.056 Uiso 1 1 calc R . . C14 C -0.02455(15) 0.6653(5) 0.3919(4) 0.0421(18) Uani 1 1 d . . . C15 C -0.07415(16) 0.7358(5) 0.3622(3) 0.0390(17) Uani 1 1 d . . . C16 C -0.07382(17) 0.8006(5) 0.4175(4) 0.051(2) Uani 1 1 d . . . H16A H -0.0556 0.8132 0.4468 0.061 Uiso 1 1 calc R . . C17 C -0.10025(18) 0.8466(6) 0.4294(4) 0.057(2) Uani 1 1 d . . . H17A H -0.1005 0.8886 0.4687 0.069 Uiso 1 1 calc R . . C18 C -0.12684(17) 0.8312(5) 0.3835(4) 0.049(2) Uani 1 1 d . . . H18A H -0.1451 0.8621 0.3915 0.059 Uiso 1 1 calc R . . C19 C -0.12569(16) 0.7704(5) 0.3267(4) 0.0434(18) Uani 1 1 d . . . C20 C -0.17192(16) 0.8134(5) 0.2556(4) 0.0433(18) Uani 1 1 d . . . C21 C -0.16903(17) 0.9102(5) 0.2597(4) 0.050(2) Uani 1 1 d . . . H21A H -0.1512 0.9369 0.2832 0.060 Uiso 1 1 calc R . . C22 C -0.19141(18) 0.9656(6) 0.2305(4) 0.053(2) Uani 1 1 d . . . H22A H -0.1893 1.0313 0.2325 0.064 Uiso 1 1 calc R . . C23 C -0.21792(16) 0.9253(6) 0.1970(4) 0.049(2) Uani 1 1 d . . . H23A H -0.2341 0.9629 0.1769 0.059 Uiso 1 1 calc R . . C24 C -0.21980(16) 0.8317(6) 0.1941(4) 0.0456(19) Uani 1 1 d . . . H24A H -0.2375 0.8050 0.1698 0.055 Uiso 1 1 calc R . . C25 C 0.22253(16) 0.6429(5) 0.4540(4) 0.0474(19) Uani 1 1 d . . . H25A H 0.2404 0.6175 0.4378 0.057 Uiso 1 1 calc R . . C26 C 0.22222(18) 0.6614(6) 0.5264(4) 0.058(2) Uani 1 1 d . . . H26A H 0.2396 0.6509 0.5590 0.069 Uiso 1 1 calc R . . C27 C 0.19610(18) 0.6955(6) 0.5498(4) 0.054(2) Uani 1 1 d . . . H27A H 0.1951 0.7089 0.5994 0.064 Uiso 1 1 calc R . . C28 C 0.17123(16) 0.7104(5) 0.5010(4) 0.048(2) Uani 1 1 d . . . H28A H 0.1529 0.7323 0.5174 0.058 Uiso 1 1 calc R . . C29 C 0.17276(16) 0.6938(5) 0.4280(4) 0.0418(18) Uani 1 1 d . . . C30 C 0.12591(17) 0.7653(5) 0.3816(4) 0.0460(19) Uani 1 1 d . . . C31 C 0.12660(17) 0.8436(6) 0.4254(4) 0.057(2) Uani 1 1 d . . . H31A H 0.1448 0.8606 0.4533 0.068 Uiso 1 1 calc R . . C32 C 0.10102(19) 0.8958(6) 0.4281(4) 0.065(2) Uani 1 1 d . . . H32A H 0.1015 0.9484 0.4590 0.078 Uiso 1 1 calc R . . C33 C 0.07440(17) 0.8738(6) 0.3870(4) 0.056(2) Uani 1 1 d . . . H33A H 0.0565 0.9087 0.3912 0.067 Uiso 1 1 calc R . . C34 C 0.07448(16) 0.7998(5) 0.3396(4) 0.0439(19) Uani 1 1 d . . . C35 C 0.02555(16) 0.8260(6) 0.2728(4) 0.0446(19) Uani 1 1 d . . . C36 C 0.02547(17) 0.9198(6) 0.2706(4) 0.059(2) Uani 1 1 d . . . H36A H 0.0437 0.9526 0.2838 0.071 Uiso 1 1 calc R . . C37 C 0.22330(16) 0.6152(5) 0.1450(4) 0.050(2) Uani 1 1 d . . . H37A H 0.2412 0.6410 0.1692 0.060 Uiso 1 1 calc R . . C38 C 0.22334(17) 0.5952(5) 0.0730(4) 0.051(2) Uani 1 1 d . . . H38A H 0.2411 0.6035 0.0489 0.062 Uiso 1 1 calc R . . C39 C 0.19693(17) 0.5627(6) 0.0366(4) 0.055(2) Uani 1 1 d . . . H39A H 0.1959 0.5504 -0.0136 0.066 Uiso 1 1 calc R . . C40 C 0.17199(16) 0.5482(5) 0.0743(4) 0.049(2) Uani 1 1 d . . . H40A H 0.1536 0.5268 0.0495 0.058 Uiso 1 1 calc R . . C41 C 0.17338(15) 0.5644(5) 0.1483(4) 0.0427(18) Uani 1 1 d . . . C42 C 0.12545(16) 0.4973(5) 0.1708(4) 0.0419(18) Uani 1 1 d . . . C43 C 0.12565(16) 0.4182(5) 0.1280(4) 0.0469(19) Uani 1 1 d . . . H43A H 0.1438 0.3981 0.1096 0.056 Uiso 1 1 calc R . . C44 C 0.09926(16) 0.3698(5) 0.1128(4) 0.051(2) Uani 1 1 d . . . H44A H 0.0990 0.3173 0.0819 0.061 Uiso 1 1 calc R . . C45 C 0.07314(17) 0.3957(5) 0.1414(4) 0.049(2) Uani 1 1 d . . . H45A H 0.0548 0.3628 0.1290 0.058 Uiso 1 1 calc R . . C46 C 0.07374(15) 0.4702(5) 0.1883(4) 0.0393(18) Uani 1 1 d . . . C47 C 0.02534(15) 0.4467(6) 0.2351(3) 0.0413(18) Uani 1 1 d . . . C48 C 0.02527(16) 0.3512(5) 0.2377(4) 0.052(2) Uani 1 1 d . . . H48A H 0.0433 0.3182 0.2307 0.062 Uiso 1 1 calc R . . C49 C 0.1927(3) 0.1819(9) 0.4982(8) 0.112(4) Uani 1 1 d . . . H49A H 0.1921 0.2475 0.4923 0.135 Uiso 1 1 calc R . . C50 C 0.2075(2) 0.1444(9) 0.5571(6) 0.087(3) Uani 1 1 d . . . H50A H 0.2167 0.1838 0.5937 0.104 Uiso 1 1 calc R . . C51 C 0.2096(2) 0.0519(9) 0.5651(6) 0.084(3) Uani 1 1 d . . . H51A H 0.2200 0.0266 0.6074 0.101 Uiso 1 1 calc R . . C52 C 0.1971(3) -0.0051(8) 0.5139(8) 0.097(3) Uani 1 1 d . . . H52A H 0.1988 -0.0706 0.5189 0.116 Uiso 1 1 calc R . . C53 C 0.1814(3) 0.0344(12) 0.4532(7) 0.128(5) Uani 1 1 d . . . H53A H 0.1725 -0.0043 0.4156 0.153 Uiso 1 1 calc R . . C54 C 0.1788(3) 0.1272(12) 0.4478(7) 0.131(6) Uani 1 1 d . . . H54A H 0.1670 0.1539 0.4079 0.157 Uiso 1 1 calc R . . C55 C 0.1415(3) 0.1216(10) 0.1355(9) 0.154(7) Uani 1 1 d . . . H55A H 0.1398 0.0955 0.0867 0.230 Uiso 1 1 d R . . H55B H 0.1582 0.0913 0.1647 0.230 Uiso 1 1 d R . . H55C H 0.1455 0.1885 0.1331 0.230 Uiso 1 1 d R . . C56 C 0.1145(4) 0.1070(11) 0.1671(10) 0.171(7) Uani 1 1 d . . . H56A H 0.1103 0.0395 0.1687 0.206 Uiso 1 1 calc R . . H56B H 0.0976 0.1368 0.1372 0.206 Uiso 1 1 calc R . . C57 C 0.1160(4) 0.1448(10) 0.2400(9) 0.148(6) Uani 1 1 d . . . H57A H 0.1335 0.1162 0.2687 0.177 Uiso 1 1 calc R . . H57B H 0.1200 0.2123 0.2375 0.177 Uiso 1 1 calc R . . C58 C 0.0894(4) 0.1310(11) 0.2777(10) 0.160(6) Uani 1 1 d . . . H58A H 0.0716 0.1478 0.2444 0.192 Uiso 1 1 calc R . . H58B H 0.0879 0.0638 0.2880 0.192 Uiso 1 1 calc R . . C59 C 0.0872(4) 0.1795(13) 0.3431(9) 0.175(7) Uani 1 1 d . . . H59A H 0.0907 0.2463 0.3343 0.209 Uiso 1 1 calc R . . H59B H 0.1037 0.1579 0.3785 0.209 Uiso 1 1 calc R . . C60 C 0.0570(4) 0.1700(12) 0.3776(8) 0.167(6) Uani 1 1 d . . . H60A H 0.0581 0.2073 0.4217 0.250 Uiso 1 1 d R . . H60B H 0.0537 0.1047 0.3895 0.250 Uiso 1 1 d R . . H60C H 0.0403 0.1920 0.3440 0.250 Uiso 1 1 d R . . O1 O 0.0000 1.0000 0.5000 0.200 Uiso 1 2 d S . . C61 C 0.0097 0.9081 0.5084 0.200 Uiso 0.50 1 d P A 1 H61A H 0.0200 0.8929 0.4669 0.240 Uiso 0.50 1 d P B 1 H61B H -0.0081 0.8701 0.5061 0.240 Uiso 0.50 1 d P C 1 C61' C 0.0186 0.9757 0.5627 0.200 Uiso 0.50 1 d P A 2 H61C H 0.0077 0.9910 0.6032 0.240 Uiso 0.50 1 d P D 2 H61D H 0.0360 1.0153 0.5650 0.240 Uiso 0.50 1 d P E 2 C62 C 0.0299 0.8771 0.5733 0.200 Uiso 1 1 d . . . H62A H 0.0341 0.8119 0.5694 0.300 Uiso 0.50 1 d P F 1 H62B H 0.0485 0.9113 0.5761 0.300 Uiso 0.50 1 d P G 1 H62C H 0.0199 0.8881 0.6160 0.300 Uiso 0.50 1 d P H 1 H62D H 0.0421 0.8724 0.6184 0.300 Uiso 0.50 1 d P I 2 H62E H 0.0129 0.8357 0.5736 0.300 Uiso 0.50 1 d P J 2 H62F H 0.0417 0.8604 0.5348 0.300 Uiso 0.50 1 d P K 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 0.0529(8) 0.0460(8) 0.0411(7) 0.0020(6) 0.0019(6) -0.0005(6) Cr3 0.0627(8) 0.0431(8) 0.0348(7) 0.0002(6) 0.0037(6) -0.0010(6) Cr5 0.0638(12) 0.0444(11) 0.0336(9) 0.000 -0.0012(8) 0.000 Cl1 0.0423(11) 0.0531(13) 0.0554(12) 0.0015(9) 0.0024(9) 0.0005(9) N1 0.034(4) 0.049(4) 0.047(4) 0.006(3) -0.001(3) 0.005(3) N2 0.033(3) 0.049(4) 0.038(3) 0.007(3) -0.004(3) -0.008(3) N3 0.034(3) 0.047(4) 0.038(3) -0.001(3) -0.002(3) -0.002(3) N4 0.034(3) 0.059(4) 0.033(3) 0.005(3) 0.004(3) -0.002(3) N5 0.029(3) 0.047(4) 0.034(3) 0.000(3) -0.001(3) 0.001(3) N6 0.034(3) 0.056(4) 0.039(3) -0.003(3) 0.004(3) -0.003(3) N7 0.032(3) 0.043(4) 0.037(3) -0.004(3) 0.003(3) 0.000(3) N8 0.038(4) 0.043(4) 0.044(3) -0.008(3) 0.001(3) 0.005(3) N9 0.028(3) 0.051(4) 0.047(3) 0.002(3) 0.002(3) 0.003(3) N10 0.065(5) 0.094(6) 0.057(4) 0.001(4) 0.001(4) 0.002(4) N11 0.035(3) 0.053(4) 0.041(3) 0.005(3) -0.004(3) -0.004(3) N12 0.034(3) 0.049(4) 0.043(3) -0.008(3) 0.001(3) -0.002(3) N13 0.033(3) 0.045(4) 0.043(3) 0.000(3) 0.005(3) -0.001(3) N14 0.035(3) 0.047(4) 0.049(4) -0.006(3) -0.001(3) 0.003(3) N15 0.032(5) 0.054(6) 0.034(5) 0.000 -0.001(4) 0.000 N16 0.087(9) 0.067(8) 0.111(9) 0.000 -0.003(7) 0.000 N17 0.038(4) 0.040(4) 0.047(3) 0.000(3) 0.007(3) 0.004(3) N18 0.033(3) 0.048(4) 0.038(3) -0.005(3) 0.001(3) 0.001(3) N19 0.045(4) 0.039(4) 0.035(3) 0.003(3) 0.002(3) 0.002(3) N20 0.032(3) 0.044(4) 0.042(3) 0.000(3) -0.001(3) -0.002(3) N21 0.034(5) 0.047(5) 0.035(4) 0.000 -0.003(4) 0.000 N22 0.083(9) 0.084(9) 0.087(8) 0.000 0.008(7) 0.000 C1 0.037(5) 0.059(6) 0.054(5) 0.008(4) -0.005(4) -0.003(4) C2 0.045(5) 0.057(6) 0.075(6) 0.005(5) 0.016(4) 0.003(4) C3 0.060(6) 0.040(5) 0.085(6) 0.001(4) 0.015(5) 0.001(4) C4 0.049(5) 0.050(6) 0.057(5) 0.003(4) 0.005(4) 0.004(4) C5 0.034(4) 0.053(5) 0.039(4) 0.008(4) -0.007(3) -0.002(4) C6 0.035(4) 0.050(5) 0.035(4) 0.003(4) -0.005(3) -0.003(4) C7 0.037(4) 0.056(5) 0.047(4) 0.009(4) 0.000(4) -0.001(4) C8 0.051(5) 0.065(6) 0.049(5) 0.024(4) 0.004(4) 0.009(4) C9 0.034(4) 0.072(6) 0.049(5) 0.020(4) 0.003(3) 0.001(4) C10 0.031(4) 0.057(5) 0.035(4) 0.003(4) -0.005(3) -0.002(4) C11 0.040(4) 0.054(5) 0.039(4) -0.001(4) 0.004(4) -0.011(4) C12 0.028(4) 0.076(6) 0.050(5) 0.005(4) 0.007(4) 0.012(4) C13 0.038(4) 0.058(5) 0.045(5) -0.001(4) 0.006(4) 0.003(4) C14 0.035(4) 0.052(5) 0.040(4) 0.003(4) 0.006(3) -0.004(4) C15 0.041(4) 0.043(5) 0.034(4) -0.004(3) 0.003(3) 0.001(4) C16 0.047(5) 0.057(5) 0.048(5) -0.010(4) -0.003(4) 0.002(4) C17 0.053(5) 0.062(6) 0.058(5) -0.019(4) 0.006(4) 0.010(4) C18 0.043(5) 0.047(5) 0.057(5) -0.006(4) 0.001(4) 0.010(4) C19 0.034(4) 0.048(5) 0.048(4) -0.003(4) 0.001(4) -0.001(4) C20 0.038(4) 0.047(5) 0.046(4) -0.002(4) 0.009(3) 0.002(4) C21 0.044(5) 0.048(5) 0.056(5) -0.001(4) 0.000(4) 0.003(4) C22 0.052(5) 0.046(5) 0.062(5) 0.004(4) 0.010(4) 0.008(4) C23 0.033(4) 0.051(6) 0.063(5) 0.010(4) 0.002(4) 0.008(4) C24 0.033(4) 0.053(6) 0.051(5) 0.003(4) 0.006(3) -0.006(4) C25 0.039(4) 0.050(5) 0.051(5) 0.008(4) -0.005(4) -0.001(4) C26 0.051(5) 0.074(6) 0.047(5) 0.005(4) -0.004(4) -0.005(5) C27 0.054(5) 0.071(6) 0.033(4) -0.003(4) -0.006(4) -0.007(4) C28 0.042(5) 0.059(5) 0.044(5) 0.000(4) 0.003(4) -0.008(4) C29 0.038(4) 0.045(5) 0.041(4) 0.003(4) -0.003(4) -0.012(4) C30 0.043(5) 0.051(5) 0.043(4) -0.003(4) -0.001(4) -0.008(4) C31 0.037(5) 0.074(6) 0.056(5) -0.022(5) -0.010(4) -0.005(4) C32 0.057(6) 0.065(6) 0.072(6) -0.030(5) -0.003(5) 0.002(5) C33 0.037(4) 0.071(6) 0.057(5) -0.013(5) -0.005(4) 0.011(4) C34 0.037(4) 0.053(5) 0.040(4) -0.010(4) -0.002(3) -0.008(4) C35 0.040(4) 0.044(5) 0.050(5) -0.001(4) 0.007(4) 0.004(4) C36 0.037(5) 0.048(6) 0.088(6) 0.001(5) -0.016(4) 0.007(4) C37 0.031(4) 0.059(5) 0.058(5) 0.002(4) 0.001(4) -0.004(4) C38 0.046(5) 0.061(5) 0.050(5) 0.004(4) 0.017(4) 0.008(4) C39 0.052(5) 0.069(6) 0.045(5) -0.003(4) 0.006(4) 0.002(4) C40 0.033(4) 0.059(5) 0.055(5) -0.001(4) 0.006(4) 0.002(4) C41 0.036(4) 0.045(5) 0.047(5) 0.004(4) 0.005(4) 0.002(4) C42 0.038(4) 0.057(5) 0.031(4) 0.005(4) 0.002(3) 0.003(4) C43 0.038(4) 0.052(5) 0.051(5) -0.012(4) 0.004(3) 0.001(4) C44 0.045(5) 0.052(5) 0.056(5) -0.012(4) 0.005(4) 0.003(4) C45 0.042(5) 0.058(5) 0.044(4) -0.010(4) 0.002(4) -0.008(4) C46 0.033(4) 0.047(5) 0.038(4) 0.007(4) -0.001(3) 0.002(4) C47 0.028(4) 0.057(6) 0.038(4) -0.001(4) -0.003(3) 0.001(4) C48 0.039(4) 0.040(5) 0.080(6) -0.010(4) 0.026(4) -0.010(4) C49 0.103(9) 0.086(9) 0.143(12) 0.010(9) -0.011(8) -0.019(8) C50 0.091(8) 0.094(10) 0.074(7) -0.004(6) 0.005(6) 0.000(7) C51 0.069(7) 0.101(9) 0.081(7) 0.028(7) -0.002(5) -0.002(7) C52 0.088(8) 0.078(8) 0.124(10) -0.013(8) 0.014(7) -0.023(7) C53 0.169(14) 0.147(14) 0.068(8) -0.021(9) 0.019(8) -0.083(11) C54 0.150(12) 0.133(13) 0.099(10) 0.060(9) -0.040(8) -0.075(11) C55 0.132(12) 0.152(14) 0.184(15) 0.096(12) 0.051(11) 0.049(11) C56 0.22(2) 0.123(13) 0.177(18) 0.043(13) 0.025(15) 0.050(14) C57 0.176(16) 0.127(13) 0.152(14) -0.033(10) 0.077(12) -0.042(11) C58 0.173(17) 0.139(15) 0.172(17) 0.004(12) 0.044(13) -0.023(12) C59 0.22(2) 0.173(17) 0.133(14) -0.021(13) 0.029(13) -0.030(15) C60 0.165(16) 0.206(18) 0.133(13) -0.008(12) 0.036(12) -0.020(13) _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 Cr2 2.097(4) . ? Cr1 N11 2.097(6) . ? Cr1 N9 2.100(6) 2 ? Cr1 N1 2.111(6) . ? Cr1 N17 2.113(6) . ? Cr1 Cr2' 2.475(4) . ? Cr1 Cl1 2.541(2) . ? Cr3 Cr4 2.024(3) . ? Cr3 Cr2' 2.046(4) . ? Cr3 N13 2.050(6) . ? Cr3 N19 2.055(6) . ? Cr3 N7 2.055(5) 2 ? Cr3 N3 2.059(6) . ? Cr3 Cr4' 2.404(4) . ? Cr3 Cr2 2.425(4) . ? Cr2 N2 2.031(6) . ? Cr2 N18 2.033(6) . ? Cr2 N8 2.043(6) 2 ? Cr2 N12 2.047(6) . ? Cr4 N6 2.027(6) 2 ? Cr4 N20 2.034(7) . ? Cr4 N14 2.034(7) . ? Cr4 N4 2.041(6) . ? Cr4 Cr5 2.397(3) . ? Cr2' N8 2.010(6) 2 ? Cr2' N12 2.017(6) . ? Cr2' N2 2.041(7) . ? Cr2' N18 2.048(6) . ? Cr4' Cr5 2.017(3) . ? Cr4' N4 2.030(6) . ? Cr4' N14 2.030(7) . ? Cr4' N6 2.036(6) 2 ? Cr4' N20 2.036(7) . ? Cr5 Cr4' 2.017(3) 2 ? Cr5 N15 2.031(9) . ? Cr5 N21 2.034(8) . ? Cr5 N5 2.036(5) 2 ? Cr5 N5 2.036(5) . ? Cr5 Cr4 2.397(3) 2 ? N1 C5 1.358(8) . ? N1 C1 1.359(9) . ? N2 C6 1.371(8) . ? N2 C5 1.384(9) . ? N3 C6 1.362(8) . ? N3 C10 1.365(8) . ? N4 C11 1.373(8) . ? N4 C10 1.390(9) . ? N5 C14 1.360(8) . ? N5 C11 1.363(8) . ? N6 C14 1.386(8) . ? N6 C15 1.395(8) . ? N6 Cr4 2.027(6) 2 ? N6 Cr4' 2.036(6) 2 ? N7 C15 1.365(8) . ? N7 C19 1.372(8) . ? N7 Cr3 2.055(5) 2 ? N8 C20 1.381(9) . ? N8 C19 1.389(9) . ? N8 Cr2' 2.010(6) 2 ? N8 Cr2 2.043(6) 2 ? N9 C24 1.360(9) . ? N9 C20 1.377(9) . ? N9 Cr1 2.100(6) 2 ? N10 C12 1.323(9) . ? N10 C13 1.382(9) . ? N11 C29 1.363(9) . ? N11 C25 1.365(8) . ? N12 C29 1.380(8) . ? N12 C30 1.380(9) . ? N13 C34 1.375(9) . ? N13 C30 1.379(9) . ? N14 C34 1.386(8) . ? N14 C35 1.394(9) . ? N15 C35 1.368(8) . ? N15 C35 1.368(8) 2 ? N16 C36 1.352(9) . ? N16 C36 1.352(9) 2 ? N17 C37 1.354(8) . ? N17 C41 1.378(8) . ? N18 C41 1.373(8) . ? N18 C42 1.379(9) . ? N19 C46 1.364(8) . ? N19 C42 1.380(8) . ? N20 C47 1.379(9) . ? N20 C46 1.389(8) . ? N21 C47 1.372(8) . ? N21 C47 1.372(8) 2 ? N22 C48 1.356(8) . ? N22 C48 1.356(8) 2 ? C1 C2 1.368(11) . ? C2 C3 1.390(10) . ? C3 C4 1.373(10) . ? C4 C5 1.404(10) . ? C6 C7 1.394(9) . ? C7 C8 1.366(9) . ? C8 C9 1.379(10) . ? C9 C10 1.376(10) . ? C11 C12 1.394(9) . ? C13 C14 1.366(9) . ? C15 C16 1.390(9) . ? C16 C17 1.383(10) . ? C17 C18 1.409(10) . ? C18 C19 1.379(10) . ? C20 C21 1.401(10) . ? C21 C22 1.349(10) . ? C22 C23 1.405(10) . ? C23 C24 1.350(10) . ? C25 C26 1.376(10) . ? C26 C27 1.368(10) . ? C27 C28 1.380(10) . ? C28 C29 1.389(9) . ? C30 C31 1.390(10) . ? C31 C32 1.367(10) . ? C32 C33 1.383(10) . ? C33 C34 1.385(10) . ? C35 C36 1.351(11) . ? C37 C38 1.373(10) . ? C38 C39 1.380(10) . ? C39 C40 1.382(10) . ? C40 C41 1.396(9) . ? C42 C43 1.392(10) . ? C43 C44 1.370(10) . ? C44 C45 1.373(10) . ? C45 C46 1.382(10) . ? C47 C48 1.375(10) . ? C49 C54 1.334(16) . ? C49 C50 1.341(15) . ? C50 C51 1.341(14) . ? C51 C52 1.339(14) . ? C52 C53 1.394(16) . ? C53 C54 1.344(18) . ? C55 C56 1.403(18) . ? C56 C57 1.460(19) . ? C57 C58 1.443(18) . ? C58 C59 1.416(18) . ? C59 C60 1.545(19) . ? O1 C61 1.3962 . ? O1 C61 1.3962 5_576 ? O1 C61' 1.4103 5_576 ? O1 C61' 1.4103 . ? C61 C62 1.5035 . ? C61' C62 1.5121 . ? 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 Cr2 Cr1 N11 86.31(18) . . ? Cr2 Cr1 N9 84.74(18) . 2 ? N11 Cr1 N9 87.3(2) . 2 ? Cr2 Cr1 N1 84.83(18) . . ? N11 Cr1 N1 91.0(2) . . ? N9 Cr1 N1 169.5(2) 2 . ? Cr2 Cr1 N17 85.72(18) . . ? N11 Cr1 N17 172.0(2) . . ? N9 Cr1 N17 92.1(2) 2 . ? N1 Cr1 N17 88.1(2) . . ? Cr2 Cr1 Cr2' 0.85(16) . . ? N11 Cr1 Cr2' 85.89(18) . . ? N9 Cr1 Cr2' 83.98(18) 2 . ? N1 Cr1 Cr2' 85.57(18) . . ? N17 Cr1 Cr2' 86.14(17) . . ? Cr2 Cr1 Cl1 178.52(11) . . ? N11 Cr1 Cl1 94.42(16) . . ? N9 Cr1 Cl1 94.00(16) 2 . ? N1 Cr1 Cl1 96.45(17) . . ? N17 Cr1 Cl1 93.55(16) . . ? Cr2' Cr1 Cl1 177.95(11) . . ? Cr4 Cr3 Cr2' 179.61(14) . . ? Cr4 Cr3 N13 89.42(18) . . ? Cr2' Cr3 N13 90.23(19) . . ? Cr4 Cr3 N19 89.94(19) . . ? Cr2' Cr3 N19 90.41(19) . . ? N13 Cr3 N19 179.3(2) . . ? Cr4 Cr3 N7 88.90(18) . 2 ? Cr2' Cr3 N7 91.28(18) . 2 ? N13 Cr3 N7 89.6(2) . 2 ? N19 Cr3 N7 90.5(2) . 2 ? Cr4 Cr3 N3 89.87(18) . . ? Cr2' Cr3 N3 89.95(18) . . ? N13 Cr3 N3 91.6(2) . . ? N19 Cr3 N3 88.3(2) . . ? N7 Cr3 N3 178.3(2) 2 . ? Cr4 Cr3 Cr4' 0.37(16) . . ? Cr2' Cr3 Cr4' 179.29(13) . . ? N13 Cr3 Cr4' 89.29(18) . . ? N19 Cr3 Cr4' 90.06(18) . . ? N7 Cr3 Cr4' 89.25(17) 2 . ? N3 Cr3 Cr4' 89.53(18) . . ? Cr4 Cr3 Cr2 179.45(14) . . ? Cr2' Cr3 Cr2 0.74(16) . . ? N13 Cr3 Cr2 90.93(18) . . ? N19 Cr3 Cr2 89.71(18) . . ? N7 Cr3 Cr2 91.53(17) 2 . ? N3 Cr3 Cr2 89.69(18) . . ? Cr4' Cr3 Cr2 179.19(13) . . ? N2 Cr2 N18 88.1(3) . . ? N2 Cr2 N8 165.8(3) . 2 ? N18 Cr2 N8 89.1(3) . 2 ? N2 Cr2 N12 90.5(3) . . ? N18 Cr2 N12 167.1(3) . . ? N8 Cr2 N12 89.0(3) 2 . ? N2 Cr2 Cr1 97.5(2) . . ? N18 Cr2 Cr1 97.3(2) . . ? N8 Cr2 Cr1 96.7(2) 2 . ? N12 Cr2 Cr1 95.6(2) . . ? N2 Cr2 Cr3 83.6(2) . . ? N18 Cr2 Cr3 83.87(19) . . ? N8 Cr2 Cr3 82.3(2) 2 . ? N12 Cr2 Cr3 83.19(19) . . ? Cr1 Cr2 Cr3 178.45(18) . . ? Cr3 Cr4 N6 96.5(2) . 2 ? Cr3 Cr4 N20 95.1(2) . . ? N6 Cr4 N20 90.8(3) 2 . ? Cr3 Cr4 N14 95.8(2) . . ? N6 Cr4 N14 88.6(3) 2 . ? N20 Cr4 N14 169.0(3) . . ? Cr3 Cr4 N4 94.7(2) . . ? N6 Cr4 N4 168.7(3) 2 . ? N20 Cr4 N4 89.2(3) . . ? N14 Cr4 N4 89.2(3) . . ? Cr3 Cr4 Cr5 178.20(17) . . ? N6 Cr4 Cr5 85.31(19) 2 . ? N20 Cr4 Cr5 84.69(19) . . ? N14 Cr4 Cr5 84.3(2) . . ? N4 Cr4 Cr5 83.46(19) . . ? N8 Cr2' N12 90.8(3) 2 . ? N8 Cr2' N2 172.4(3) 2 . ? N12 Cr2' N2 91.1(3) . . ? N8 Cr2' Cr3 93.4(2) 2 . ? N12 Cr2' Cr3 94.5(2) . . ? N2 Cr2' Cr3 93.8(2) . . ? N8 Cr2' N18 89.6(3) 2 . ? N12 Cr2' N18 171.5(3) . . ? N2 Cr2' N18 87.4(3) . . ? Cr3 Cr2' N18 94.0(2) . . ? N8 Cr2' Cr1 86.6(2) 2 . ? N12 Cr2' Cr1 85.6(2) . . ? N2 Cr2' Cr1 86.2(2) . . ? Cr3 Cr2' Cr1 180.0(2) . . ? N18 Cr2' Cr1 86.0(2) . . ? Cr5 Cr4' N4 94.3(2) . . ? Cr5 Cr4' N14 95.1(2) . . ? N4 Cr4' N14 89.6(3) . . ? Cr5 Cr4' N6 95.9(2) . 2 ? N4 Cr4' N6 169.7(3) . 2 ? N14 Cr4' N6 88.5(3) . 2 ? Cr5 Cr4' N20 95.4(2) . . ? N4 Cr4' N20 89.5(3) . . ? N14 Cr4' N20 169.5(3) . . ? N6 Cr4' N20 90.5(3) 2 . ? Cr5 Cr4' Cr3 178.66(18) . . ? N4 Cr4' Cr3 84.4(2) . . ? N14 Cr4' Cr3 85.1(2) . . ? N6 Cr4' Cr3 85.38(19) 2 . ? N20 Cr4' Cr3 84.37(19) . . ? Cr4' Cr5 Cr4' 179.9(2) 2 . ? Cr4' Cr5 N15 90.07(10) 2 . ? Cr4' Cr5 N15 90.07(10) . . ? Cr4' Cr5 N21 89.93(10) 2 . ? Cr4' Cr5 N21 89.93(10) . . ? N15 Cr5 N21 180.000(2) . . ? Cr4' Cr5 N5 91.12(17) 2 2 ? Cr4' Cr5 N5 88.89(17) . 2 ? N15 Cr5 N5 89.23(16) . 2 ? N21 Cr5 N5 90.77(16) . 2 ? Cr4' Cr5 N5 88.89(17) 2 . ? Cr4' Cr5 N5 91.12(17) . . ? N15 Cr5 N5 89.23(16) . . ? N21 Cr5 N5 90.77(16) . . ? N5 Cr5 N5 178.5(3) 2 . ? Cr4' Cr5 Cr4 0.11(17) 2 2 ? Cr4' Cr5 Cr4 179.82(15) . 2 ? N15 Cr5 Cr4 90.08(9) . 2 ? N21 Cr5 Cr4 89.92(9) . 2 ? N5 Cr5 Cr4 91.23(16) 2 2 ? N5 Cr5 Cr4 88.77(16) . 2 ? Cr4' Cr5 Cr4 179.82(15) 2 . ? Cr4' Cr5 Cr4 0.11(17) . . ? N15 Cr5 Cr4 90.08(9) . . ? N21 Cr5 Cr4 89.92(9) . . ? N5 Cr5 Cr4 88.77(16) 2 . ? N5 Cr5 Cr4 91.23(16) . . ? Cr4 Cr5 Cr4 179.84(18) 2 . ? C5 N1 C1 118.0(7) . . ? C5 N1 Cr1 122.4(5) . . ? C1 N1 Cr1 118.5(5) . . ? C6 N2 C5 122.7(6) . . ? C6 N2 Cr2 126.1(5) . . ? C5 N2 Cr2 110.8(4) . . ? C6 N2 Cr2' 116.1(5) . . ? C5 N2 Cr2' 119.9(5) . . ? Cr2 N2 Cr2' 10.71(13) . . ? C6 N3 C10 120.9(6) . . ? C6 N3 Cr3 119.2(5) . . ? C10 N3 Cr3 119.7(5) . . ? C11 N4 C10 122.5(6) . . ? C11 N4 Cr4' 114.2(5) . . ? C10 N4 Cr4' 122.9(5) . . ? C11 N4 Cr4 123.8(5) . . ? C10 N4 Cr4 113.7(4) . . ? Cr4' N4 Cr4 10.72(13) . . ? C14 N5 C11 120.3(6) . . ? C14 N5 Cr5 121.7(4) . . ? C11 N5 Cr5 118.0(4) . . ? C14 N6 C15 122.7(6) . . ? C14 N6 Cr4 123.5(5) . 2 ? C15 N6 Cr4 113.7(4) . 2 ? C14 N6 Cr4' 113.9(5) . 2 ? C15 N6 Cr4' 123.3(4) . 2 ? Cr4 N6 Cr4' 10.74(13) 2 2 ? C15 N7 C19 120.3(6) . . ? C15 N7 Cr3 121.2(4) . 2 ? C19 N7 Cr3 118.4(4) . 2 ? C20 N8 C19 121.5(6) . . ? C20 N8 Cr2' 120.0(5) . 2 ? C19 N8 Cr2' 117.1(5) . 2 ? C20 N8 Cr2 111.9(5) . 2 ? C19 N8 Cr2 126.3(5) . 2 ? Cr2' N8 Cr2 10.73(13) 2 2 ? C24 N9 C20 117.0(6) . . ? C24 N9 Cr1 119.3(5) . 2 ? C20 N9 Cr1 122.9(5) . 2 ? C12 N10 C13 117.8(7) . . ? C29 N11 C25 117.7(6) . . ? C29 N11 Cr1 122.4(4) . . ? C25 N11 Cr1 119.9(5) . . ? C29 N12 C30 121.4(6) . . ? C29 N12 Cr2' 123.6(5) . . ? C30 N12 Cr2' 114.8(5) . . ? C29 N12 Cr2 114.1(5) . . ? C30 N12 Cr2 124.5(5) . . ? Cr2' N12 Cr2 10.70(13) . . ? C34 N13 C30 120.8(6) . . ? C34 N13 Cr3 120.7(5) . . ? C30 N13 Cr3 118.5(5) . . ? C34 N14 C35 121.8(6) . . ? C34 N14 Cr4' 123.6(5) . . ? C35 N14 Cr4' 114.4(5) . . ? C34 N14 Cr4 114.3(5) . . ? C35 N14 Cr4 123.9(5) . . ? Cr4' N14 Cr4 10.74(13) . . ? C35 N15 C35 118.1(9) . 2 ? C35 N15 Cr5 120.9(5) . . ? C35 N15 Cr5 120.9(5) 2 . ? C36 N16 C36 118.0(11) . 2 ? C37 N17 C41 117.8(6) . . ? C37 N17 Cr1 121.0(5) . . ? C41 N17 Cr1 121.1(5) . . ? C41 N18 C42 122.2(6) . . ? C41 N18 Cr2 113.5(5) . . ? C42 N18 Cr2 124.3(5) . . ? C41 N18 Cr2' 122.5(5) . . ? C42 N18 Cr2' 115.3(4) . . ? Cr2 N18 Cr2' 10.68(13) . . ? C46 N19 C42 120.3(6) . . ? C46 N19 Cr3 120.0(5) . . ? C42 N19 Cr3 119.7(5) . . ? C47 N20 C46 121.7(6) . . ? C47 N20 Cr4 123.8(5) . . ? C46 N20 Cr4 114.4(5) . . ? C47 N20 Cr4' 114.2(5) . . ? C46 N20 Cr4' 124.1(5) . . ? Cr4 N20 Cr4' 10.73(13) . . ? C47 N21 C47 119.2(9) . 2 ? C47 N21 Cr5 120.4(4) . . ? C47 N21 Cr5 120.4(4) 2 . ? C48 N22 C48 118.7(11) . 2 ? N1 C1 C2 123.0(7) . . ? C1 C2 C3 119.0(8) . . ? C4 C3 C2 119.2(8) . . ? C3 C4 C5 119.5(8) . . ? N1 C5 N2 113.9(7) . . ? N1 C5 C4 121.2(7) . . ? N2 C5 C4 124.6(7) . . ? N3 C6 N2 114.0(6) . . ? N3 C6 C7 119.6(6) . . ? N2 C6 C7 126.3(7) . . ? C8 C7 C6 119.5(7) . . ? C7 C8 C9 120.4(7) . . ? C10 C9 C8 119.7(7) . . ? N3 C10 C9 119.9(6) . . ? N3 C10 N4 113.7(6) . . ? C9 C10 N4 126.2(6) . . ? N5 C11 N4 115.7(6) . . ? N5 C11 C12 118.6(6) . . ? N4 C11 C12 125.5(6) . . ? N10 C12 C11 122.3(7) . . ? C14 C13 N10 121.8(7) . . ? N5 C14 C13 119.1(6) . . ? N5 C14 N6 113.1(6) . . ? C13 C14 N6 127.7(6) . . ? N7 C15 C16 120.4(6) . . ? N7 C15 N6 113.4(6) . . ? C16 C15 N6 126.1(6) . . ? C17 C16 C15 119.4(7) . . ? C16 C17 C18 120.1(7) . . ? C19 C18 C17 118.5(7) . . ? N7 C19 C18 121.1(6) . . ? N7 C19 N8 113.5(6) . . ? C18 C19 N8 125.4(7) . . ? N9 C20 N8 112.9(6) . . ? N9 C20 C21 120.6(7) . . ? N8 C20 C21 126.4(7) . . ? C22 C21 C20 120.4(7) . . ? C21 C22 C23 119.3(8) . . ? C24 C23 C22 118.5(7) . . ? C23 C24 N9 124.1(7) . . ? N11 C25 C26 123.8(7) . . ? C27 C26 C25 118.0(7) . . ? C26 C27 C28 119.7(7) . . ? C27 C28 C29 120.6(7) . . ? N11 C29 N12 113.2(6) . . ? N11 C29 C28 120.2(6) . . ? N12 C29 C28 126.6(7) . . ? N13 C30 N12 114.6(6) . . ? N13 C30 C31 119.0(7) . . ? N12 C30 C31 126.3(7) . . ? C32 C31 C30 119.7(7) . . ? C31 C32 C33 121.5(8) . . ? C32 C33 C34 118.5(7) . . ? N13 C34 C33 120.2(6) . . ? N13 C34 N14 113.4(6) . . ? C33 C34 N14 126.3(7) . . ? C36 C35 N15 120.3(7) . . ? C36 C35 N14 126.8(7) . . ? N15 C35 N14 112.8(7) . . ? C35 C36 N16 121.5(8) . . ? N17 C37 C38 124.2(7) . . ? C37 C38 C39 118.2(7) . . ? C38 C39 C40 119.0(7) . . ? C39 C40 C41 121.0(7) . . ? N18 C41 N17 114.8(6) . . ? N18 C41 C40 125.3(6) . . ? N17 C41 C40 119.6(6) . . ? N18 C42 N19 113.5(6) . . ? N18 C42 C43 126.6(6) . . ? N19 C42 C43 119.8(7) . . ? C44 C43 C42 118.9(7) . . ? C43 C44 C45 121.2(7) . . ? C44 C45 C46 119.4(7) . . ? N19 C46 C45 120.1(6) . . ? N19 C46 N20 113.7(6) . . ? C45 C46 N20 126.1(6) . . ? N21 C47 C48 119.6(7) . . ? N21 C47 N20 113.7(7) . . ? C48 C47 N20 126.5(7) . . ? N22 C48 C47 121.3(8) . . ? C54 C49 C50 119.9(12) . . ? C49 C50 C51 120.9(11) . . ? C52 C51 C50 120.6(11) . . ? C51 C52 C53 118.2(12) . . ? C54 C53 C52 119.9(12) . . ? C49 C54 C53 120.3(13) . . ? C55 C56 C57 111.6(18) . . ? C58 C57 C56 115.7(17) . . ? C59 C58 C57 118.6(16) . . ? C58 C59 C60 116.7(15) . . ? C61 O1 C61 180.0 . 5_576 ? C61 O1 C61' 118.6 . 5_576 ? C61 O1 C61' 61.4 5_576 5_576 ? C61 O1 C61' 61.4 . . ? C61 O1 C61' 118.6 5_576 . ? C61' O1 C61' 180.0 5_576 . ? O1 C61 C62 121.7 . . ? O1 C61' C62 120.2 . . ? C61 C62 C61' 56.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.977 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.182 # Attachment 'G_n9mpchem communrevised #Cr9 chem comm suibmit2nd revised Cr92nd revised B614597C comp 2.cif' data_ic11787 _database_code_depnum_ccdc_archive 'CCDC 623205' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C111 H93 Cl3 Cr9 N42 S2' _chemical_formula_weight 2653.74 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' 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 C2/c 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' '-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 43.5722(13) _cell_length_b 14.4390(5) _cell_length_c 19.2834(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.1689(17) _cell_angle_gamma 90.00 _cell_volume 12008.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5408 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.979 _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 31810 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10533 _reflns_number_gt 4321 _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 ; We examined the structure and concluded that the C2/c option is better than the Cc option for the following reasons: (1)The intensities statistics shows this structure is super centrics. (mean \/cxE2-1\/cxis 1.086 where 0.968 is expected for centrosym and 0.736 for non-centrosym.) (2)We solved structure by C2/c and Cc options and checked with check CIF/PLATON report. The reports of C2/c option only give several alerts in level C, but the reports of Cc option give alerts in level A & B (detection the centre of symmetry and many others). We also checked the bond distances and angles, C2/c option is more meaningful than the Cc option. Solvent molecules (C1S-C12S, C50, Cl1-Cl3) were included in the calculatins but were not refined, and the occupancies of solvent atoms were set to 0.5. 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^)+(0.1122P)^2^+102.9418P] 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 10533 _refine_ls_number_parameters 681 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2330 _refine_ls_R_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.3432 _refine_ls_wR_factor_gt 0.2902 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.29343(4) 0.11791(12) 0.19792(9) 0.0557(5) Uani 1 1 d . . . Cr3 Cr 0.39783(4) 0.11973(11) 0.22574(8) 0.0483(5) Uani 1 1 d . . . Cr2 Cr 0.34104(10) 0.1172(3) 0.2089(2) 0.0469(13) Uiso 0.50 1 d P . 1 Cr4 Cr 0.44378(10) 0.1218(3) 0.2364(2) 0.0416(13) Uiso 0.50 1 d P . 1 Cr2' Cr 0.35132(11) 0.1179(3) 0.2143(2) 0.0480(13) Uiso 0.50 1 d P . 2 Cr4' Cr 0.45435(10) 0.1210(3) 0.2420(2) 0.0434(13) Uiso 0.50 1 d P . 2 Cr5 Cr 0.5000 0.12154(15) 0.2500 0.0471(6) Uani 1 2 d S . . S1 S 0.17806(9) 0.1378(4) 0.1505(3) 0.160(3) Uani 1 1 d . . . N1 N 0.2964(2) -0.0248(6) 0.1773(5) 0.058(2) Uani 1 1 d . . . N2 N 0.34672(18) -0.0028(6) 0.1582(4) 0.051(2) Uani 1 1 d . . . N3 N 0.39717(18) 0.0296(5) 0.1444(4) 0.044(2) Uani 1 1 d . . . N4 N 0.44772(18) 0.0750(6) 0.1400(4) 0.046(2) Uani 1 1 d . . . N5 N 0.49824(17) 0.1225(5) 0.1439(4) 0.0425(19) Uani 1 1 d . . . N6 N 0.54888(19) 0.1677(6) 0.1608(4) 0.051(2) Uani 1 1 d . . . N7 N 0.60063(18) 0.2091(5) 0.1913(4) 0.046(2) Uani 1 1 d . . . N8 N 0.65211(19) 0.2349(6) 0.2316(4) 0.053(2) Uani 1 1 d . . . N9 N 0.7024(2) 0.2608(6) 0.2822(5) 0.055(2) Uani 1 1 d . . . N10 N 0.4935(2) 0.1270(7) -0.0009(5) 0.068(3) Uani 1 1 d . . . N11 N 0.29512(19) 0.1445(6) 0.0939(5) 0.059(2) Uani 1 1 d . . . N12 N 0.34573(19) 0.1926(6) 0.1231(4) 0.051(2) Uani 1 1 d . . . N13 N 0.39694(19) 0.2300(5) 0.1582(4) 0.045(2) Uani 1 1 d . . . N14 N 0.44837(18) 0.2531(6) 0.2045(5) 0.050(2) Uani 1 1 d . . . N15 N 0.5000 0.2625(7) 0.2500 0.047(3) Uani 1 2 d S . . N16 N 0.5000 0.4531(9) 0.2500 0.082(5) Uani 1 2 d S . . N17 N 0.2983(2) 0.0899(6) 0.3055(4) 0.056(2) Uani 1 1 d . . . N18 N 0.34793(19) 0.0432(6) 0.3007(4) 0.055(2) Uani 1 1 d . . . N19 N 0.39912(18) 0.0090(5) 0.2926(4) 0.044(2) Uani 1 1 d . . . N20 N 0.44995(18) -0.0106(5) 0.2740(4) 0.046(2) Uani 1 1 d . . . N21 N 0.5000 -0.0184(7) 0.2500 0.040(3) Uani 1 2 d S . . N22 N 0.5000 -0.2092(10) 0.2500 0.074(4) Uani 1 2 d S . . N23 N 0.2410(2) 0.1220(6) 0.1859(5) 0.054(2) Uani 1 1 d . . . C1 C 0.2726(3) -0.0803(10) 0.1830(7) 0.083(4) Uani 1 1 d . . . H1A H 0.2535 -0.0519 0.1893 0.100 Uiso 1 1 calc R . . C2 C 0.2732(3) -0.1713(11) 0.1808(8) 0.106(5) Uani 1 1 d . . . H2A H 0.2552 -0.2069 0.1849 0.128 Uiso 1 1 calc R . . C3 C 0.3012(3) -0.2141(10) 0.1722(8) 0.099(5) Uani 1 1 d . . . H3A H 0.3029 -0.2797 0.1721 0.119 Uiso 1 1 calc R . . C4 C 0.3257(3) -0.1613(8) 0.1640(6) 0.069(3) Uani 1 1 d . . . H4A H 0.3447 -0.1896 0.1575 0.083 Uiso 1 1 calc R . . C5 C 0.3234(2) -0.0658(8) 0.1650(5) 0.057(3) Uani 1 1 d . . . C6 C 0.3717(2) -0.0246(8) 0.1244(5) 0.052(3) Uani 1 1 d . . . C7 C 0.3721(2) -0.0909(8) 0.0711(5) 0.058(3) Uani 1 1 d . . . H7A H 0.3540 -0.1260 0.0556 0.070 Uiso 1 1 calc R . . C8 C 0.3985(2) -0.1049(7) 0.0416(6) 0.058(3) Uani 1 1 d . . . H8A H 0.3993 -0.1529 0.0083 0.069 Uiso 1 1 calc R . . C9 C 0.4242(3) -0.0479(8) 0.0609(6) 0.070(3) Uani 1 1 d . . . H9A H 0.4423 -0.0551 0.0391 0.084 Uiso 1 1 calc R . . C10 C 0.4232(2) 0.0195(7) 0.1124(5) 0.050(3) Uani 1 1 d . . . C11 C 0.4715(2) 0.0975(7) 0.1023(6) 0.051(3) Uani 1 1 d . . . C12 C 0.4697(2) 0.1037(8) 0.0295(5) 0.060(3) Uani 1 1 d . . . H12A H 0.4505 0.0904 0.0012 0.073 Uiso 1 1 calc R . . C13 C 0.5205(3) 0.1498(8) 0.0420(6) 0.061(3) Uani 1 1 d . . . H13A H 0.5380 0.1675 0.0208 0.073 Uiso 1 1 calc R . . C14 C 0.5234(2) 0.1481(7) 0.1139(6) 0.048(3) Uani 1 1 d . . . C15 C 0.5738(2) 0.2209(7) 0.1445(6) 0.052(3) Uani 1 1 d . . . C16 C 0.5724(2) 0.2846(8) 0.0910(6) 0.059(3) Uani 1 1 d . . . H16A H 0.5535 0.2969 0.0612 0.071 Uiso 1 1 calc R . . C17 C 0.6000(3) 0.3305(8) 0.0825(6) 0.071(3) Uani 1 1 d . . . H17A H 0.5999 0.3734 0.0451 0.085 Uiso 1 1 calc R . . C18 C 0.6270(3) 0.3158(8) 0.1257(6) 0.062(3) Uani 1 1 d . . . H18A H 0.6457 0.3448 0.1171 0.075 Uiso 1 1 calc R . . C19 C 0.6268(2) 0.2574(7) 0.1826(6) 0.050(3) Uani 1 1 d . . . C20 C 0.6751(3) 0.2991(9) 0.2511(6) 0.058(3) Uani 1 1 d . . . C21 C 0.6716(3) 0.3950(8) 0.2473(6) 0.064(3) Uani 1 1 d . . . H21A H 0.6526 0.4212 0.2258 0.077 Uiso 1 1 calc R . . C22 C 0.6955(3) 0.4512(9) 0.2746(7) 0.076(4) Uani 1 1 d . . . H22A H 0.6931 0.5166 0.2731 0.092 Uiso 1 1 calc R . . C23 C 0.7229(3) 0.4131(9) 0.3040(7) 0.078(4) Uani 1 1 d . . . H23A H 0.7400 0.4512 0.3218 0.094 Uiso 1 1 calc R . . C24 C 0.7253(3) 0.3183(9) 0.3071(6) 0.066(3) Uani 1 1 d . . . H24A H 0.7444 0.2922 0.3283 0.079 Uiso 1 1 calc R . . C25 C 0.2699(3) 0.1287(8) 0.0452(6) 0.059(3) Uani 1 1 d . . . H25A H 0.2515 0.1066 0.0606 0.071 Uiso 1 1 calc R . . C26 C 0.2698(3) 0.1428(8) -0.0243(7) 0.073(4) Uani 1 1 d . . . H26A H 0.2517 0.1303 -0.0566 0.087 Uiso 1 1 calc R . . C27 C 0.2964(3) 0.1760(9) -0.0481(6) 0.071(4) Uani 1 1 d . . . H27A H 0.2968 0.1856 -0.0968 0.086 Uiso 1 1 calc R . . C28 C 0.3219(3) 0.1944(8) -0.0009(6) 0.067(3) Uani 1 1 d . . . H28A H 0.3402 0.2176 -0.0164 0.080 Uiso 1 1 calc R . . C29 C 0.3212(3) 0.1793(8) 0.0706(6) 0.061(3) Uani 1 1 d . . . C30 C 0.3704(2) 0.2522(8) 0.1152(6) 0.053(3) Uani 1 1 d . . . C31 C 0.3687(3) 0.3260(8) 0.0723(6) 0.061(3) Uani 1 1 d . . . H31A H 0.3497 0.3430 0.0449 0.073 Uiso 1 1 calc R . . C32 C 0.3952(3) 0.3763(9) 0.0692(7) 0.081(4) Uani 1 1 d . . . H32A H 0.3947 0.4263 0.0371 0.097 Uiso 1 1 calc R . . C33 C 0.4226(3) 0.3554(8) 0.1121(6) 0.069(3) Uani 1 1 d . . . H33A H 0.4408 0.3909 0.1098 0.082 Uiso 1 1 calc R . . C34 C 0.4230(2) 0.2824(8) 0.1580(6) 0.058(3) Uani 1 1 d . . . C35 C 0.4736(2) 0.3103(8) 0.2252(6) 0.060(3) Uani 1 1 d . . . C36 C 0.4745(2) 0.4051(8) 0.2290(7) 0.074(4) Uani 1 1 d . . . H36A H 0.4557 0.4382 0.2159 0.089 Uiso 1 1 calc R . . C37 C 0.2750(2) 0.1116(7) 0.3418(6) 0.055(3) Uani 1 1 d . . . H37A H 0.2564 0.1362 0.3166 0.067 Uiso 1 1 calc R . . C38 C 0.2764(3) 0.1009(9) 0.4109(7) 0.074(4) Uani 1 1 d . . . H38A H 0.2591 0.1163 0.4336 0.089 Uiso 1 1 calc R . . C39 C 0.3038(3) 0.0664(9) 0.4496(6) 0.073(3) Uani 1 1 d . . . H39A H 0.3056 0.0583 0.4989 0.087 Uiso 1 1 calc R . . C40 C 0.3279(2) 0.0448(8) 0.4138(6) 0.061(3) Uani 1 1 d . . . H40A H 0.3467 0.0215 0.4386 0.073 Uiso 1 1 calc R . . C41 C 0.3252(2) 0.0566(7) 0.3423(6) 0.053(3) Uani 1 1 d . . . C42 C 0.3733(2) -0.0144(7) 0.3219(5) 0.051(3) Uani 1 1 d . . . C43 C 0.3732(2) -0.0910(8) 0.3650(5) 0.057(3) Uani 1 1 d . . . H43A H 0.3546 -0.1107 0.3811 0.068 Uiso 1 1 calc R . . C44 C 0.4004(2) -0.1376(7) 0.3838(5) 0.056(3) Uani 1 1 d . . . H44A H 0.4012 -0.1865 0.4170 0.067 Uiso 1 1 calc R . . C45 C 0.4271(2) -0.1150(7) 0.3552(5) 0.057(3) Uani 1 1 d . . . H45A H 0.4459 -0.1483 0.3681 0.068 Uiso 1 1 calc R . . C46 C 0.4256(2) -0.0427(7) 0.3074(5) 0.047(3) Uani 1 1 d . . . C47 C 0.4745(2) -0.0674(8) 0.2625(5) 0.051(3) Uani 1 1 d . . . C48 C 0.4746(3) -0.1624(8) 0.2603(6) 0.064(3) Uani 1 1 d . . . H48A H 0.4563 -0.1954 0.2662 0.077 Uiso 1 1 calc R . . C49 C 0.2174(3) 0.1310(10) 0.1741(8) 0.085(4) Uani 1 1 d . . . C50 C 0.6795 0.5571 0.5108 0.200 Uiso 0.50 1 d P A 1 H50A H 0.6721 0.5147 0.5460 0.240 Uiso 0.50 1 calc PR A 1 Cl1 Cl 0.6521 0.6143 0.4540 0.200 Uiso 0.50 1 d P A 1 Cl2 Cl 0.7049 0.6421 0.5410 0.200 Uiso 0.50 1 d P A 1 Cl3 Cl 0.6995 0.5095 0.4502 0.200 Uiso 0.50 1 d P A 1 C1S C 0.6013 0.6202 0.2774 0.200 Uiso 0.50 1 d P B 2 H1SA H 0.5802 0.6363 0.2562 0.300 Uiso 0.50 1 calc PR B 2 H1SB H 0.6053 0.5550 0.2679 0.300 Uiso 0.50 1 calc PR B 2 H1SC H 0.6161 0.6593 0.2574 0.300 Uiso 0.50 1 calc PR B 2 C2S C 0.6046 0.6355 0.3550 0.200 Uiso 0.50 1 d P B 2 H2SA H 0.5901 0.5959 0.3769 0.240 Uiso 0.50 1 calc PR B 2 H2SB H 0.6010 0.7012 0.3663 0.240 Uiso 0.50 1 calc PR B 2 C3S C 0.6377 0.6077 0.3780 0.200 Uiso 0.50 1 d P B 2 H3SA H 0.6507 0.6455 0.3506 0.240 Uiso 0.50 1 calc PR B 2 H3SB H 0.6398 0.5426 0.3634 0.240 Uiso 0.50 1 calc PR B 2 C4S C 0.6521 0.6143 0.4540 0.200 Uiso 0.50 1 d P B 2 H4SA H 0.6402 0.5724 0.4810 0.240 Uiso 0.50 1 calc PR B 2 H4SB H 0.6485 0.6781 0.4698 0.240 Uiso 0.50 1 calc PR B 2 C5S C 0.6870 0.5924 0.4760 0.200 Uiso 0.50 1 d P B 2 H5SA H 0.6978 0.6063 0.4354 0.240 Uiso 0.50 1 calc PR B 2 H5SB H 0.6889 0.5248 0.4844 0.240 Uiso 0.50 1 calc PR B 2 C6S C 0.7049 0.6421 0.5410 0.200 Uiso 0.50 1 d P B 2 H6SA H 0.7265 0.6211 0.5482 0.300 Uiso 0.50 1 calc PR B 2 H6SB H 0.6953 0.6273 0.5826 0.300 Uiso 0.50 1 calc PR B 2 H6SC H 0.7043 0.7092 0.5333 0.300 Uiso 0.50 1 calc PR B 2 C7S C 0.4092 0.4497 -0.1970 0.200 Uiso 0.50 1 d P C 1 H7SA H 0.3868 0.4497 -0.2137 0.300 Uiso 0.50 1 calc PR C 1 H7SB H 0.4196 0.4067 -0.2253 0.300 Uiso 0.50 1 calc PR C 1 H7SC H 0.4174 0.5122 -0.2011 0.300 Uiso 0.50 1 calc PR C 1 C8S C 0.4146 0.4198 -0.1220 0.200 Uiso 0.50 1 d P C 1 H8SA H 0.4049 0.3581 -0.1199 0.240 Uiso 0.50 1 calc PR C 1 H8SB H 0.4028 0.4628 -0.0958 0.240 Uiso 0.50 1 calc PR C 1 C9S C 0.4466 0.4128 -0.0815 0.200 Uiso 0.50 1 d P C 1 H9SA H 0.4520 0.4770 -0.0663 0.240 Uiso 0.50 1 calc PR C 1 H9SB H 0.4438 0.3786 -0.0383 0.240 Uiso 0.50 1 calc PR C 1 C10S C 0.4757 0.3742 -0.1026 0.200 Uiso 0.50 1 d P C 1 H10A H 0.4789 0.4017 -0.1480 0.240 Uiso 0.50 1 calc PR C 1 H10B H 0.4733 0.3065 -0.1093 0.240 Uiso 0.50 1 calc PR C 1 C11S C 0.5035 0.3929 -0.0496 0.200 Uiso 0.50 1 d P C 1 H11A H 0.5045 0.3509 -0.0088 0.240 Uiso 0.50 1 calc PR C 1 H11B H 0.5041 0.4580 -0.0334 0.240 Uiso 0.50 1 calc PR C 1 C12S C 0.5286 0.3726 -0.0931 0.200 Uiso 0.50 1 d P C 1 H12B H 0.5489 0.3821 -0.0647 0.300 Uiso 0.50 1 calc PR C 1 H12C H 0.5265 0.4143 -0.1336 0.300 Uiso 0.50 1 calc PR C 1 H12D H 0.5268 0.3083 -0.1093 0.300 Uiso 0.50 1 calc PR C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0508(11) 0.0582(12) 0.0581(11) 0.0023(9) 0.0073(8) -0.0009(9) Cr3 0.0582(11) 0.0414(10) 0.0457(10) 0.0016(8) 0.0094(8) 0.0017(8) Cr5 0.0583(15) 0.0387(14) 0.0448(13) 0.000 0.0092(11) 0.000 S1 0.053(2) 0.227(6) 0.196(5) 0.111(5) 0.007(3) 0.000(3) N1 0.050(6) 0.057(6) 0.069(6) -0.010(5) 0.013(5) -0.013(5) N2 0.042(5) 0.053(6) 0.056(5) -0.004(4) 0.005(4) 0.004(4) N3 0.043(5) 0.050(5) 0.037(4) -0.002(4) 0.004(4) 0.000(4) N4 0.042(5) 0.052(5) 0.043(5) 0.005(4) 0.007(4) 0.004(4) N5 0.042(5) 0.043(5) 0.044(5) 0.005(4) 0.012(4) 0.001(4) N6 0.046(5) 0.059(6) 0.052(5) 0.004(5) 0.016(4) 0.002(4) N7 0.040(5) 0.053(5) 0.047(5) 0.008(4) 0.012(4) 0.002(4) N8 0.044(5) 0.054(6) 0.064(6) 0.015(5) 0.018(5) -0.002(5) N9 0.042(6) 0.058(6) 0.068(6) -0.002(5) 0.015(5) -0.011(5) N10 0.071(7) 0.084(7) 0.051(5) 0.003(5) 0.016(5) -0.003(6) N11 0.038(5) 0.072(6) 0.064(6) 0.006(5) 0.002(5) 0.004(5) N12 0.044(5) 0.052(6) 0.056(5) 0.015(4) 0.006(4) 0.008(4) N13 0.044(5) 0.043(5) 0.049(5) 0.008(4) 0.013(4) 0.002(4) N14 0.040(5) 0.042(5) 0.070(6) 0.006(4) 0.014(4) 0.002(4) N15 0.051(8) 0.033(7) 0.061(8) 0.000 0.020(6) 0.000 N16 0.059(10) 0.039(8) 0.149(14) 0.000 0.018(9) 0.000 N17 0.047(5) 0.061(6) 0.064(6) -0.001(5) 0.021(5) -0.005(5) N18 0.042(5) 0.058(6) 0.065(6) 0.014(5) 0.010(5) -0.003(5) N19 0.047(5) 0.045(5) 0.043(5) -0.001(4) 0.007(4) 0.001(4) N20 0.044(5) 0.044(5) 0.054(5) -0.002(4) 0.014(4) -0.001(4) N21 0.046(7) 0.032(6) 0.041(7) 0.000 0.000(5) 0.000 N22 0.070(10) 0.061(9) 0.095(11) 0.000 0.023(8) 0.000 N23 0.030(5) 0.060(6) 0.068(6) 0.011(5) -0.006(5) 0.000(5) C1 0.071(9) 0.065(9) 0.117(11) -0.028(8) 0.026(8) -0.028(8) C2 0.086(11) 0.093(12) 0.151(15) -0.014(11) 0.055(10) -0.024(9) C3 0.094(11) 0.071(10) 0.145(14) -0.015(9) 0.061(10) -0.017(9) C4 0.069(8) 0.053(8) 0.092(9) 0.000(7) 0.032(7) -0.004(7) C5 0.050(7) 0.068(9) 0.054(7) 0.001(6) 0.009(5) -0.018(6) C6 0.050(7) 0.065(8) 0.041(6) 0.009(6) 0.004(5) 0.001(6) C7 0.057(7) 0.065(8) 0.054(7) -0.017(6) 0.014(6) -0.010(6) C8 0.058(7) 0.053(7) 0.064(7) -0.017(6) 0.012(6) -0.002(6) C9 0.069(8) 0.076(9) 0.068(8) -0.018(7) 0.025(6) -0.002(7) C10 0.053(7) 0.052(7) 0.042(6) 0.008(5) -0.002(5) 0.000(6) C11 0.037(6) 0.057(7) 0.058(7) -0.005(6) 0.003(5) 0.003(5) C12 0.041(6) 0.101(9) 0.041(6) -0.011(6) 0.010(5) -0.018(6) C13 0.057(7) 0.080(8) 0.050(7) 0.000(6) 0.021(6) -0.003(6) C14 0.037(6) 0.053(7) 0.056(7) -0.001(5) 0.011(5) -0.002(5) C15 0.048(7) 0.054(7) 0.059(7) 0.004(6) 0.024(6) -0.002(5) C16 0.049(7) 0.064(8) 0.064(7) 0.013(6) 0.009(6) -0.002(6) C17 0.076(9) 0.066(8) 0.072(8) 0.017(7) 0.018(7) -0.005(7) C18 0.046(7) 0.063(8) 0.080(8) 0.009(7) 0.013(6) -0.004(6) C19 0.039(6) 0.056(7) 0.056(7) 0.000(6) 0.014(5) 0.002(5) C20 0.046(7) 0.070(9) 0.063(7) -0.005(6) 0.025(6) -0.007(6) C21 0.062(8) 0.060(8) 0.073(8) -0.005(7) 0.014(6) -0.005(7) C22 0.077(9) 0.057(8) 0.099(10) -0.012(7) 0.025(8) -0.012(8) C23 0.085(10) 0.058(9) 0.093(10) -0.009(7) 0.014(8) -0.033(8) C24 0.046(7) 0.080(10) 0.073(8) -0.017(7) 0.015(6) -0.022(6) C25 0.058(7) 0.070(8) 0.048(7) 0.007(6) 0.000(6) 0.008(6) C26 0.054(8) 0.072(9) 0.087(10) -0.007(7) -0.007(7) 0.004(7) C27 0.071(9) 0.093(10) 0.049(7) -0.003(7) 0.002(7) 0.019(7) C28 0.058(8) 0.083(9) 0.061(8) 0.004(7) 0.014(6) 0.009(7) C29 0.058(8) 0.064(8) 0.060(8) 0.007(6) 0.002(6) 0.018(6) C30 0.046(7) 0.052(7) 0.063(7) 0.009(6) 0.015(6) 0.010(6) C31 0.049(7) 0.061(8) 0.074(8) 0.023(7) 0.012(6) 0.005(6) C32 0.077(9) 0.070(9) 0.092(10) 0.040(8) 0.004(8) 0.004(8) C33 0.056(8) 0.056(8) 0.095(9) 0.029(7) 0.014(7) 0.004(6) C34 0.045(7) 0.057(7) 0.073(8) 0.011(6) 0.017(6) 0.007(6) C35 0.048(7) 0.052(7) 0.084(9) 0.005(6) 0.028(6) 0.012(6) C36 0.046(7) 0.042(7) 0.132(12) 0.006(7) 0.006(7) 0.003(6) C37 0.049(7) 0.053(7) 0.065(8) -0.008(6) 0.009(6) -0.001(5) C38 0.056(8) 0.080(9) 0.094(10) -0.015(8) 0.039(7) -0.002(7) C39 0.073(9) 0.084(9) 0.063(8) -0.006(7) 0.018(7) -0.011(7) C40 0.048(7) 0.073(8) 0.065(8) -0.002(6) 0.016(6) -0.007(6) C41 0.046(7) 0.060(7) 0.055(7) -0.004(6) 0.016(6) 0.000(6) C42 0.051(7) 0.050(7) 0.053(7) -0.003(6) 0.014(5) -0.004(6) C43 0.045(7) 0.065(8) 0.061(7) 0.016(6) 0.012(5) -0.004(6) C44 0.051(7) 0.057(7) 0.062(7) 0.026(6) 0.017(6) -0.001(6) C45 0.055(7) 0.061(8) 0.056(7) 0.010(6) 0.009(5) 0.008(6) C46 0.048(7) 0.045(6) 0.049(6) 0.006(5) 0.005(5) 0.000(5) C47 0.042(6) 0.057(8) 0.052(7) -0.003(6) 0.002(5) -0.008(6) C48 0.058(8) 0.043(7) 0.096(9) 0.003(6) 0.025(7) 0.002(6) C49 0.073(10) 0.083(10) 0.100(11) 0.037(8) 0.008(9) 0.002(9) _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 N11 2.055(9) . ? Cr1 Cr2 2.055(5) . ? Cr1 N17 2.094(9) . ? Cr1 N9 2.101(9) 2_655 ? Cr1 N1 2.106(9) . ? Cr1 N23 2.265(9) . ? Cr1 Cr2' 2.497(5) . ? Cr3 Cr4 1.984(4) . ? Cr3 Cr2' 2.007(5) . ? Cr3 N3 2.034(8) . ? Cr3 N7 2.050(8) 2_655 ? Cr3 N19 2.050(8) . ? Cr3 N13 2.054(8) . ? Cr3 Cr4' 2.438(5) . ? Cr3 Cr2 2.450(5) . ? Cr2 N12 2.014(9) . ? Cr2 N2 2.021(9) . ? Cr2 N8 2.050(9) 2_655 ? Cr2 N18 2.054(9) . ? Cr4 N4 2.009(8) . ? Cr4 N14 2.012(9) . ? Cr4 N20 2.049(9) . ? Cr4 N6 2.071(9) 2_655 ? Cr4 Cr5 2.426(4) . ? Cr2' N8 2.003(9) 2_655 ? Cr2' N18 2.009(9) . ? Cr2' N2 2.046(9) . ? Cr2' N12 2.047(9) . ? Cr4' Cr5 1.973(4) . ? Cr4' N20 2.016(9) . ? Cr4' N6 2.016(9) 2_655 ? Cr4' N14 2.043(9) . ? Cr4' N4 2.057(9) . ? Cr5 Cr4' 1.973(4) 2_655 ? Cr5 N21 2.021(10) . ? Cr5 N15 2.035(11) . ? Cr5 N5 2.037(7) 2_655 ? Cr5 N5 2.037(7) . ? Cr5 Cr4 2.426(4) 2_655 ? S1 C49 1.713(15) . ? N1 C1 1.327(13) . ? N1 C5 1.369(13) . ? N2 C6 1.383(12) . ? N2 C5 1.384(12) . ? N3 C6 1.368(12) . ? N3 C10 1.375(12) . ? N4 C10 1.380(12) . ? N4 C11 1.386(12) . ? N5 C14 1.360(11) . ? N5 C11 1.365(12) . ? N6 C14 1.358(12) . ? N6 C15 1.399(12) . ? N6 Cr4' 2.016(9) 2_655 ? N6 Cr4 2.071(9) 2_655 ? N7 C19 1.366(12) . ? N7 C15 1.383(12) . ? N7 Cr3 2.050(8) 2_655 ? N8 C20 1.378(13) . ? N8 C19 1.385(12) . ? N8 Cr2' 2.003(9) 2_655 ? N8 Cr2 2.050(9) 2_655 ? N9 C24 1.334(12) . ? N9 C20 1.370(13) . ? N9 Cr1 2.101(9) 2_655 ? N10 C12 1.306(12) . ? N10 C13 1.377(13) . ? N11 C25 1.360(12) . ? N11 C29 1.375(13) . ? N12 C29 1.377(13) . ? N12 C30 1.400(12) . ? N13 C30 1.364(12) . ? N13 C34 1.365(12) . ? N14 C34 1.387(13) . ? N14 C35 1.387(13) . ? N15 C35 1.369(11) 2_655 ? N15 C35 1.369(11) . ? N16 C36 1.324(12) 2_655 ? N16 C36 1.324(12) . ? N17 C37 1.350(12) . ? N17 C41 1.371(12) . ? N18 C41 1.372(12) . ? N18 C42 1.396(12) . ? N19 C42 1.371(12) . ? N19 C46 1.371(12) . ? N20 C47 1.390(12) . ? N20 C46 1.395(12) . ? N21 C47 1.367(11) 2_655 ? N21 C47 1.367(11) . ? N22 C48 1.336(12) 2_655 ? N22 C48 1.336(12) . ? N23 C49 1.028(14) . ? C1 C2 1.316(18) . ? C2 C3 1.400(18) . ? C3 C4 1.337(15) . ? C4 C5 1.382(15) . ? C6 C7 1.405(14) . ? C7 C8 1.369(13) . ? C8 C9 1.398(14) . ? C9 C10 1.395(14) . ? C11 C12 1.398(14) . ? C13 C14 1.374(14) . ? C15 C16 1.377(14) . ? C16 C17 1.407(14) . ? C17 C18 1.358(14) . ? C18 C19 1.385(14) . ? C20 C21 1.395(15) . ? C21 C22 1.367(15) . ? C22 C23 1.364(16) . ? C23 C24 1.373(16) . ? C25 C26 1.355(15) . ? C26 C27 1.393(15) . ? C27 C28 1.358(15) . ? C28 C29 1.401(14) . ? C30 C31 1.345(14) . ? C31 C32 1.371(15) . ? C32 C33 1.386(15) . ? C33 C34 1.375(14) . ? C35 C36 1.371(15) . ? C37 C38 1.334(15) . ? C38 C39 1.408(16) . ? C39 C40 1.374(14) . ? C40 C41 1.377(14) . ? C42 C43 1.383(14) . ? C43 C44 1.368(13) . ? C44 C45 1.395(13) . ? C45 C46 1.388(13) . ? C47 C48 1.373(15) . ? C50 Cl3 1.6993 . ? C50 Cl2 1.7004 . ? C50 Cl1 1.7150 . ? C1S C2S 1.4990 . ? C2S C3S 1.5031 . ? C3S C4S 1.5115 . ? C4S C5S 1.5528 . ? C5S C6S 1.5565 . ? C7S C8S 1.4955 . ? C8S C9S 1.4997 . ? C9S C10S 1.4932 . ? C10S C11S 1.4951 . ? C11S C12S 1.4987 . ? 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 N11 Cr1 Cr2 85.7(3) . . ? N11 Cr1 N17 172.3(3) . . ? Cr2 Cr1 N17 86.5(3) . . ? N11 Cr1 N9 88.9(4) . 2_655 ? Cr2 Cr1 N9 85.8(3) . 2_655 ? N17 Cr1 N9 90.9(3) . 2_655 ? N11 Cr1 N1 89.3(4) . . ? Cr2 Cr1 N1 85.8(3) . . ? N17 Cr1 N1 89.8(3) . . ? N9 Cr1 N1 171.5(3) 2_655 . ? N11 Cr1 N23 94.1(3) . . ? Cr2 Cr1 N23 178.8(3) . . ? N17 Cr1 N23 93.7(3) . . ? N9 Cr1 N23 93.0(3) 2_655 . ? N1 Cr1 N23 95.4(3) . . ? N11 Cr1 Cr2' 87.0(3) . . ? Cr2 Cr1 Cr2' 1.39(19) . . ? N17 Cr1 Cr2' 85.3(3) . . ? N9 Cr1 Cr2' 85.3(3) 2_655 . ? N1 Cr1 Cr2' 86.4(3) . . ? N23 Cr1 Cr2' 178.0(3) . . ? Cr4 Cr3 Cr2' 179.6(2) . . ? Cr4 Cr3 N3 89.6(3) . . ? Cr2' Cr3 N3 90.2(3) . . ? Cr4 Cr3 N7 89.3(3) . 2_655 ? Cr2' Cr3 N7 90.8(3) . 2_655 ? N3 Cr3 N7 178.7(3) . 2_655 ? Cr4 Cr3 N19 90.5(3) . . ? Cr2' Cr3 N19 89.8(3) . . ? N3 Cr3 N19 89.0(3) . . ? N7 Cr3 N19 90.3(3) 2_655 . ? Cr4 Cr3 N13 89.0(3) . . ? Cr2' Cr3 N13 90.7(3) . . ? N3 Cr3 N13 90.5(3) . . ? N7 Cr3 N13 90.2(3) 2_655 . ? N19 Cr3 N13 179.3(3) . . ? Cr4 Cr3 Cr4' 1.48(18) . . ? Cr2' Cr3 Cr4' 178.90(17) . . ? N3 Cr3 Cr4' 90.4(2) . . ? N7 Cr3 Cr4' 88.5(2) 2_655 . ? N19 Cr3 Cr4' 89.3(2) . . ? N13 Cr3 Cr4' 90.2(3) . . ? Cr4 Cr3 Cr2 178.34(16) . . ? Cr2' Cr3 Cr2 1.30(19) . . ? N3 Cr3 Cr2 89.1(3) . . ? N7 Cr3 Cr2 91.9(2) 2_655 . ? N19 Cr3 Cr2 90.5(2) . . ? N13 Cr3 Cr2 90.0(3) . . ? Cr4' Cr3 Cr2 179.51(17) . . ? N12 Cr2 N2 91.9(4) . . ? N12 Cr2 N8 89.3(4) . 2_655 ? N2 Cr2 N8 164.5(4) . 2_655 ? N12 Cr2 N18 165.9(4) . . ? N2 Cr2 N18 87.6(4) . . ? N8 Cr2 N18 87.5(4) 2_655 . ? N12 Cr2 Cr1 97.6(3) . . ? N2 Cr2 Cr1 98.4(3) . . ? N8 Cr2 Cr1 96.8(3) 2_655 . ? N18 Cr2 Cr1 96.5(3) . . ? N12 Cr2 Cr3 83.3(3) . . ? N2 Cr2 Cr3 83.5(3) . . ? N8 Cr2 Cr3 81.3(3) 2_655 . ? N18 Cr2 Cr3 82.7(3) . . ? Cr1 Cr2 Cr3 177.9(2) . . ? Cr3 Cr4 N4 96.7(3) . . ? Cr3 Cr4 N14 97.2(3) . . ? N4 Cr4 N14 90.5(4) . . ? Cr3 Cr4 N20 95.9(3) . . ? N4 Cr4 N20 89.3(4) . . ? N14 Cr4 N20 166.9(4) . . ? Cr3 Cr4 N6 96.9(3) . 2_655 ? N4 Cr4 N6 166.3(4) . 2_655 ? N14 Cr4 N6 89.1(4) . 2_655 ? N20 Cr4 N6 88.0(4) . 2_655 ? Cr3 Cr4 Cr5 179.0(2) . . ? N4 Cr4 Cr5 83.2(3) . . ? N14 Cr4 Cr5 83.8(3) . . ? N20 Cr4 Cr5 83.1(3) . . ? N6 Cr4 Cr5 83.2(3) 2_655 . ? N8 Cr2' Cr3 94.6(3) 2_655 . ? N8 Cr2' N18 90.0(4) 2_655 . ? Cr3 Cr2' N18 96.2(3) . . ? N8 Cr2' N2 170.1(4) 2_655 . ? Cr3 Cr2' N2 95.2(3) . . ? N18 Cr2' N2 88.1(4) . . ? N8 Cr2' N12 89.7(4) 2_655 . ? Cr3 Cr2' N12 94.7(3) . . ? N18 Cr2' N12 169.1(4) . . ? N2 Cr2' N12 90.3(4) . . ? N8 Cr2' Cr1 85.3(3) 2_655 . ? Cr3 Cr2' Cr1 178.8(2) . . ? N18 Cr2' Cr1 85.0(3) . . ? N2 Cr2' Cr1 84.9(3) . . ? N12 Cr2' Cr1 84.1(3) . . ? Cr5 Cr4' N20 96.8(3) . . ? Cr5 Cr4' N6 97.4(3) . 2_655 ? N20 Cr4' N6 90.5(4) . 2_655 ? Cr5 Cr4' N14 95.8(3) . . ? N20 Cr4' N14 167.3(4) . . ? N6 Cr4' N14 89.7(4) 2_655 . ? Cr5 Cr4' N4 94.5(3) . . ? N20 Cr4' N4 88.9(4) . . ? N6 Cr4' N4 168.0(4) 2_655 . ? N14 Cr4' N4 88.2(4) . . ? Cr5 Cr4' Cr3 177.1(2) . . ? N20 Cr4' Cr3 83.9(3) . . ? N6 Cr4' Cr3 85.4(3) 2_655 . ? N14 Cr4' Cr3 83.5(3) . . ? N4 Cr4' Cr3 82.7(3) . . ? Cr4' Cr5 Cr4' 179.6(3) 2_655 . ? Cr4' Cr5 N21 89.78(13) 2_655 . ? Cr4' Cr5 N21 89.78(13) . . ? Cr4' Cr5 N15 90.22(13) 2_655 . ? Cr4' Cr5 N15 90.22(13) . . ? N21 Cr5 N15 180.000(1) . . ? Cr4' Cr5 N5 91.6(2) 2_655 2_655 ? Cr4' Cr5 N5 88.4(2) . 2_655 ? N21 Cr5 N5 90.4(2) . 2_655 ? N15 Cr5 N5 89.6(2) . 2_655 ? Cr4' Cr5 N5 88.4(2) 2_655 . ? Cr4' Cr5 N5 91.6(2) . . ? N21 Cr5 N5 90.4(2) . . ? N15 Cr5 N5 89.6(2) . . ? N5 Cr5 N5 179.2(4) 2_655 . ? Cr4' Cr5 Cr4 1.73(18) 2_655 2_655 ? Cr4' Cr5 Cr4 178.30(18) . 2_655 ? N21 Cr5 Cr4 90.10(11) . 2_655 ? N15 Cr5 Cr4 89.90(11) . 2_655 ? N5 Cr5 Cr4 89.9(2) 2_655 2_655 ? N5 Cr5 Cr4 90.1(2) . 2_655 ? Cr4' Cr5 Cr4 178.30(18) 2_655 . ? Cr4' Cr5 Cr4 1.73(18) . . ? N21 Cr5 Cr4 90.10(11) . . ? N15 Cr5 Cr4 89.90(11) . . ? N5 Cr5 Cr4 90.1(2) 2_655 . ? N5 Cr5 Cr4 89.9(2) . . ? Cr4 Cr5 Cr4 179.8(2) 2_655 . ? C1 N1 C5 117.1(10) . . ? C1 N1 Cr1 120.4(8) . . ? C5 N1 Cr1 122.2(7) . . ? C6 N2 C5 122.2(9) . . ? C6 N2 Cr2 125.5(7) . . ? C5 N2 Cr2 112.1(7) . . ? C6 N2 Cr2' 114.7(7) . . ? C5 N2 Cr2' 121.9(7) . . ? Cr2 N2 Cr2' 12.55(17) . . ? C6 N3 C10 120.0(8) . . ? C6 N3 Cr3 120.4(7) . . ? C10 N3 Cr3 119.5(7) . . ? C10 N4 C11 121.9(8) . . ? C10 N4 Cr4 112.9(6) . . ? C11 N4 Cr4 125.1(7) . . ? C10 N4 Cr4' 123.5(7) . . ? C11 N4 Cr4' 114.3(6) . . ? Cr4 N4 Cr4' 12.86(16) . . ? C14 N5 C11 119.6(8) . . ? C14 N5 Cr5 120.7(7) . . ? C11 N5 Cr5 119.7(6) . . ? C14 N6 C15 123.5(9) . . ? C14 N6 Cr4' 113.0(7) . 2_655 ? C15 N6 Cr4' 123.4(7) . 2_655 ? C14 N6 Cr4 124.8(7) . 2_655 ? C15 N6 Cr4 111.7(7) . 2_655 ? Cr4' N6 Cr4 12.77(16) 2_655 2_655 ? C19 N7 C15 120.1(8) . . ? C19 N7 Cr3 118.8(7) . 2_655 ? C15 N7 Cr3 121.1(6) . 2_655 ? C20 N8 C19 120.5(9) . . ? C20 N8 Cr2' 122.0(8) . 2_655 ? C19 N8 Cr2' 116.2(7) . 2_655 ? C20 N8 Cr2 111.2(7) . 2_655 ? C19 N8 Cr2 127.9(7) . 2_655 ? Cr2' N8 Cr2 12.54(17) 2_655 2_655 ? C24 N9 C20 117.6(10) . . ? C24 N9 Cr1 120.3(8) . 2_655 ? C20 N9 Cr1 121.6(7) . 2_655 ? C12 N10 C13 117.1(9) . . ? C25 N11 C29 117.5(10) . . ? C25 N11 Cr1 120.4(7) . . ? C29 N11 Cr1 122.2(7) . . ? C29 N12 C30 122.1(9) . . ? C29 N12 Cr2 111.7(7) . . ? C30 N12 Cr2 126.2(7) . . ? C29 N12 Cr2' 122.9(7) . . ? C30 N12 Cr2' 114.7(7) . . ? Cr2 N12 Cr2' 12.55(17) . . ? C30 N13 C34 120.2(9) . . ? C30 N13 Cr3 120.4(7) . . ? C34 N13 Cr3 119.4(7) . . ? C34 N14 C35 122.1(9) . . ? C34 N14 Cr4 112.4(7) . . ? C35 N14 Cr4 125.6(7) . . ? C34 N14 Cr4' 124.3(7) . . ? C35 N14 Cr4' 113.4(7) . . ? Cr4 N14 Cr4' 12.93(16) . . ? C35 N15 C35 119.5(13) 2_655 . ? C35 N15 Cr5 120.3(6) 2_655 . ? C35 N15 Cr5 120.3(6) . . ? C36 N16 C36 116.9(14) 2_655 . ? C37 N17 C41 117.7(9) . . ? C37 N17 Cr1 119.5(8) . . ? C41 N17 Cr1 122.6(7) . . ? C41 N18 C42 121.3(9) . . ? C41 N18 Cr2' 123.6(7) . . ? C42 N18 Cr2' 114.5(7) . . ? C41 N18 Cr2 113.7(7) . . ? C42 N18 Cr2 125.1(7) . . ? Cr2' N18 Cr2 12.52(17) . . ? C42 N19 C46 119.9(9) . . ? C42 N19 Cr3 120.0(7) . . ? C46 N19 Cr3 120.1(6) . . ? C47 N20 C46 122.0(8) . . ? C47 N20 Cr4' 113.5(6) . . ? C46 N20 Cr4' 124.5(7) . . ? C47 N20 Cr4 124.0(7) . . ? C46 N20 Cr4 113.8(6) . . ? Cr4' N20 Cr4 12.90(16) . . ? C47 N21 C47 117.7(12) 2_655 . ? C47 N21 Cr5 121.1(6) 2_655 . ? C47 N21 Cr5 121.1(6) . . ? C48 N22 C48 119.2(14) 2_655 . ? C49 N23 Cr1 171.0(11) . . ? C2 C1 N1 125.4(13) . . ? C1 C2 C3 117.9(13) . . ? C4 C3 C2 119.1(14) . . ? C3 C4 C5 120.4(12) . . ? N1 C5 C4 120.0(10) . . ? N1 C5 N2 113.2(10) . . ? C4 C5 N2 126.7(11) . . ? N3 C6 N2 113.4(9) . . ? N3 C6 C7 120.3(9) . . ? N2 C6 C7 126.2(10) . . ? C8 C7 C6 120.1(10) . . ? C7 C8 C9 119.5(10) . . ? C10 C9 C8 119.6(10) . . ? N3 C10 N4 114.0(9) . . ? N3 C10 C9 120.4(10) . . ? N4 C10 C9 125.4(10) . . ? N5 C11 N4 113.2(9) . . ? N5 C11 C12 119.6(9) . . ? N4 C11 C12 127.0(9) . . ? N10 C12 C11 122.1(10) . . ? C14 C13 N10 123.4(10) . . ? N6 C14 N5 114.0(9) . . ? N6 C14 C13 128.1(9) . . ? N5 C14 C13 117.9(9) . . ? C16 C15 N7 120.9(9) . . ? C16 C15 N6 125.5(10) . . ? N7 C15 N6 113.5(9) . . ? C15 C16 C17 117.1(10) . . ? C18 C17 C16 122.4(11) . . ? C17 C18 C19 118.6(10) . . ? N7 C19 C18 120.5(10) . . ? N7 C19 N8 113.3(9) . . ? C18 C19 N8 126.0(9) . . ? N9 C20 N8 113.6(10) . . ? N9 C20 C21 120.5(10) . . ? N8 C20 C21 125.6(11) . . ? C22 C21 C20 119.7(12) . . ? C23 C22 C21 119.7(12) . . ? C22 C23 C24 118.5(12) . . ? N9 C24 C23 123.9(12) . . ? C26 C25 N11 123.1(11) . . ? C25 C26 C27 119.5(11) . . ? C28 C27 C26 119.1(11) . . ? C27 C28 C29 120.0(11) . . ? N11 C29 N12 113.8(10) . . ? N11 C29 C28 120.8(10) . . ? N12 C29 C28 125.4(11) . . ? C31 C30 N13 121.7(10) . . ? C31 C30 N12 125.5(10) . . ? N13 C30 N12 112.8(9) . . ? C30 C31 C32 118.4(11) . . ? C31 C32 C33 121.2(11) . . ? C34 C33 C32 118.7(11) . . ? N13 C34 C33 119.6(10) . . ? N13 C34 N14 114.6(9) . . ? C33 C34 N14 125.8(10) . . ? N15 C35 C36 117.9(11) . . ? N15 C35 N14 113.2(9) . . ? C36 C35 N14 128.7(10) . . ? N16 C36 C35 123.7(11) . . ? C38 C37 N17 124.1(11) . . ? C37 C38 C39 119.1(11) . . ? C40 C39 C38 117.8(11) . . ? C39 C40 C41 120.8(11) . . ? N17 C41 N18 112.5(9) . . ? N17 C41 C40 120.5(9) . . ? N18 C41 C40 126.9(10) . . ? N19 C42 C43 121.1(10) . . ? N19 C42 N18 113.2(9) . . ? C43 C42 N18 125.6(9) . . ? C44 C43 C42 118.5(10) . . ? C43 C44 C45 121.3(10) . . ? C46 C45 C44 118.5(10) . . ? N19 C46 C45 120.3(9) . . ? N19 C46 N20 113.4(9) . . ? C45 C46 N20 126.2(9) . . ? N21 C47 C48 120.3(10) . . ? N21 C47 N20 112.7(9) . . ? C48 C47 N20 126.9(10) . . ? N22 C48 C47 121.1(11) . . ? N23 C49 S1 175.3(16) . . ? Cl3 C50 Cl2 98.9 . . ? Cl3 C50 Cl1 97.7 . . ? Cl2 C50 Cl1 103.4 . . ? C1S C2S C3S 102.0 . . ? C2S C3S C4S 121.2 . . ? C3S C4S C5S 120.4 . . ? C4S C5S C6S 119.1 . . ? C7S C8S C9S 122.2 . . ? C10S C9S C8S 130.0 . . ? C9S C10S C11S 112.5 . . ? C10S C11S C12S 99.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.035 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.218