# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Igor Fedushkin' _publ_contact_author_email IGORFED@IOMC.RAS.RU _publ_section_title ; Acenaphthene-1,2-diimine Chromium Complexes ; loop_ _publ_author_name 'Igor Fedushkin' 'Georgy K Fukin' 'Valentine M Makarov' 'Vladimir G. Sokolov' # Attachment 'B909814C_compound_2.cif' data_crbianm _database_code_depnum_ccdc_archive 'CCDC 732682' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H74 Cl3 Cr Mg N2 O4.25' _chemical_formula_weight 989.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mg Mg 0.0486 0.0363 '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 21.2323(9) _cell_length_b 26.7013(11) _cell_length_c 18.5352(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.0390(10) _cell_angle_gamma 90.00 _cell_volume 10449.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description rhombus _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4216 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8642 _exptl_absorpt_correction_T_max 0.9384 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74190 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.00 _reflns_number_total 16254 _reflns_number_gt 11644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.1287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16254 _refine_ls_number_parameters 1171 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1A Cr 0.380604(18) 0.129800(14) 0.26727(2) 0.02172(10) Uani 1 1 d . . . Cr1B Cr 0.114009(18) -0.179161(14) 0.20212(2) 0.02246(10) Uani 1 1 d . . . Cl1A Cl 0.28126(3) 0.14315(2) 0.31775(3) 0.02810(16) Uani 1 1 d . . . Cl1B Cl 0.16117(3) -0.19463(2) 0.33138(3) 0.03087(17) Uani 1 1 d . . . Mg1A Mg 0.24473(4) 0.11992(3) 0.18966(5) 0.0265(2) Uani 1 1 d . . . Mg1B Mg 0.24780(4) -0.15082(3) 0.27763(4) 0.0251(2) Uani 1 1 d . . . N1A N 0.42709(9) 0.18116(7) 0.33269(10) 0.0216(5) Uani 1 1 d . . . O1B O 0.31744(9) -0.11481(7) 0.22532(10) 0.0334(5) Uani 1 1 d . . . N1B N 0.02315(10) -0.15469(7) 0.18882(11) 0.0241(5) Uani 1 1 d . . . C1B C -0.00195(12) -0.10488(9) 0.19089(14) 0.0270(7) Uani 1 1 d . . . C1A C 0.40397(11) 0.21765(9) 0.38054(13) 0.0226(6) Uani 1 1 d . . . O1A O 0.22561(9) 0.09237(7) 0.08421(10) 0.0350(5) Uani 1 1 d . . . Cl2A Cl 0.32828(3) 0.17843(2) 0.15780(3) 0.02844(16) Uani 1 1 d . . . Cl2B Cl 0.15956(3) -0.09585(2) 0.22155(4) 0.03244(17) Uani 1 1 d . . . O2A O 0.17620(9) 0.17424(7) 0.16772(9) 0.0322(5) Uani 1 1 d . . . N2A N 0.47104(9) 0.10756(7) 0.25788(10) 0.0223(5) Uani 1 1 d . . . N2B N 0.07099(9) -0.24211(7) 0.16106(11) 0.0230(5) Uani 1 1 d . . . O2B O 0.31635(9) -0.20043(7) 0.32086(10) 0.0359(5) Uani 1 1 d . . . C2A C 0.39193(11) 0.26715(9) 0.35551(13) 0.0239(6) Uani 1 1 d . . . C2B C -0.02886(13) -0.08823(10) 0.25277(14) 0.0308(7) Uani 1 1 d . . . Cl3A Cl 0.33240(3) 0.05605(2) 0.21008(4) 0.03007(16) Uani 1 1 d . . . Cl3B Cl 0.21726(3) -0.20391(3) 0.16982(4) 0.03489(18) Uani 1 1 d . . . O3B O 0.27027(9) -0.10608(7) 0.36874(9) 0.0369(5) Uani 1 1 d . . . O3A O 0.17637(8) 0.07307(7) 0.22579(10) 0.0368(5) Uani 1 1 d . . . C3A C 0.37664(12) 0.30230(9) 0.40613(14) 0.0268(7) Uani 1 1 d . . . H3AA H 0.3695 0.3361 0.3913 0.032 Uiso 1 1 calc R . . C3B C -0.05580(15) -0.04082(10) 0.24982(17) 0.0410(8) Uani 1 1 d . . . H3BA H -0.0743 -0.0288 0.2909 0.049 Uiso 1 1 calc R . . C4A C 0.37164(12) 0.28953(10) 0.47703(14) 0.0284(7) Uani 1 1 d . . . H4AA H 0.3617 0.3144 0.5107 0.034 Uiso 1 1 calc R . . C4B C -0.05662(16) -0.01082(11) 0.18995(17) 0.0481(9) Uani 1 1 d . . . H4BA H -0.0766 0.0210 0.1892 0.058 Uiso 1 1 calc R . . C5A C 0.38100(12) 0.24059(10) 0.49949(14) 0.0284(7) Uani 1 1 d . . . H5AA H 0.3763 0.2320 0.5484 0.034 Uiso 1 1 calc R . . C5B C -0.02807(15) -0.02722(10) 0.13043(16) 0.0423(9) Uani 1 1 d . . . H5BA H -0.0275 -0.0059 0.0895 0.051 Uiso 1 1 calc R . . C6A C 0.39718(11) 0.20361(9) 0.45206(13) 0.0244(6) Uani 1 1 d . . . C6B C 0.00007(13) -0.07476(10) 0.12956(15) 0.0329(7) Uani 1 1 d . . . C7A C 0.39635(13) 0.28144(9) 0.27716(14) 0.0286(7) Uani 1 1 d . . . H7AA H 0.4058 0.2503 0.2503 0.034 Uiso 1 1 calc R . . C7B C -0.02581(14) -0.12003(10) 0.32055(14) 0.0366(8) Uani 1 1 d . . . H7BA H -0.0175 -0.1554 0.3063 0.044 Uiso 1 1 calc R . . C8A C 0.33338(14) 0.30226(11) 0.24205(16) 0.0408(8) Uani 1 1 d . . . H8AA H 0.2997 0.2778 0.2468 0.061 Uiso 1 1 calc R . . H8AB H 0.3366 0.3089 0.1906 0.061 Uiso 1 1 calc R . . H8AC H 0.3235 0.3335 0.2663 0.061 Uiso 1 1 calc R . . C8B C 0.02948(15) -0.10333(12) 0.37376(16) 0.0459(9) Uani 1 1 d . . . H8BA H 0.0686 -0.1045 0.3501 0.069 Uiso 1 1 calc R . . H8BB H 0.0334 -0.1257 0.4159 0.069 Uiso 1 1 calc R . . H8BC H 0.0221 -0.0690 0.3896 0.069 Uiso 1 1 calc R . . C9A C 0.45074(15) 0.31873(12) 0.27012(17) 0.0462(9) Uani 1 1 d . . . H9AA H 0.4906 0.3044 0.2924 0.069 Uiso 1 1 calc R . . H9AB H 0.4421 0.3501 0.2947 0.069 Uiso 1 1 calc R . . H9AC H 0.4542 0.3254 0.2187 0.069 Uiso 1 1 calc R . . C9B C -0.08756(16) -0.11958(12) 0.35600(17) 0.0475(9) Uani 1 1 d . . . H9BA H -0.1223 -0.1314 0.3211 0.071 Uiso 1 1 calc R . . H9BB H -0.0966 -0.0854 0.3712 0.071 Uiso 1 1 calc R . . H9BC H -0.0835 -0.1417 0.3985 0.071 Uiso 1 1 calc R . . C10A C 0.40808(12) 0.15015(10) 0.47786(14) 0.0290(7) Uani 1 1 d . . . H10A H 0.4116 0.1289 0.4340 0.035 Uiso 1 1 calc R . . C10B C 0.02954(14) -0.09305(11) 0.06356(15) 0.0368(8) Uani 1 1 d . . . H10B H 0.0514 -0.1254 0.0767 0.044 Uiso 1 1 calc R . . C11A C 0.35263(14) 0.13030(11) 0.51523(16) 0.0388(8) Uani 1 1 d . . . H11A H 0.3615 0.0958 0.5314 0.058 Uiso 1 1 calc R . . H11B H 0.3141 0.1309 0.4811 0.058 Uiso 1 1 calc R . . H11C H 0.3466 0.1514 0.5573 0.058 Uiso 1 1 calc R . . C11B C 0.07928(15) -0.05634(12) 0.04136(17) 0.0479(9) Uani 1 1 d . . . H11D H 0.1112 -0.0505 0.0826 0.072 Uiso 1 1 calc R . . H11E H 0.0588 -0.0246 0.0264 0.072 Uiso 1 1 calc R . . H11F H 0.0997 -0.0704 0.0009 0.072 Uiso 1 1 calc R . . C12B C -0.02022(15) -0.10313(12) 0.00082(16) 0.0456(9) Uani 1 1 d . . . H12A H -0.0516 -0.1267 0.0161 0.068 Uiso 1 1 calc R . . H12B H -0.0001 -0.1175 -0.0397 0.068 Uiso 1 1 calc R . . H12C H -0.0412 -0.0717 -0.0147 0.068 Uiso 1 1 calc R . . C12A C 0.47041(14) 0.14503(12) 0.52720(18) 0.0474(9) Uani 1 1 d . . . H12D H 0.4760 0.1102 0.5431 0.071 Uiso 1 1 calc R . . H12E H 0.4693 0.1668 0.5696 0.071 Uiso 1 1 calc R . . H12F H 0.5058 0.1549 0.5004 0.071 Uiso 1 1 calc R . . C13B C -0.01804(12) -0.19084(9) 0.16581(13) 0.0230(6) Uani 1 1 d . . . C13A C 0.48986(11) 0.17778(9) 0.33360(13) 0.0220(6) Uani 1 1 d . . . C14A C 0.54247(11) 0.20532(9) 0.37169(13) 0.0224(6) Uani 1 1 d . . . C14B C -0.08690(12) -0.19287(10) 0.14704(13) 0.0257(7) Uani 1 1 d . . . C15A C 0.59801(12) 0.18100(9) 0.35344(13) 0.0229(6) Uani 1 1 d . . . C15B C -0.09956(11) -0.24219(10) 0.11945(13) 0.0262(7) Uani 1 1 d . . . C16B C -0.04325(12) -0.27095(9) 0.12004(13) 0.0244(6) Uani 1 1 d . . . C16A C 0.58362(12) 0.13940(9) 0.30591(13) 0.0240(6) Uani 1 1 d . . . C17A C 0.51373(11) 0.13832(9) 0.29405(13) 0.0217(6) Uani 1 1 d . . . C17B C 0.00803(11) -0.23782(9) 0.15072(12) 0.0217(6) Uani 1 1 d . . . C18A C 0.55005(12) 0.24623(9) 0.41776(13) 0.0262(7) Uani 1 1 d . . . H18A H 0.5143 0.2639 0.4312 0.031 Uiso 1 1 calc R . . C18B C -0.13803(12) -0.16133(10) 0.14979(14) 0.0302(7) Uani 1 1 d . . . H18B H -0.1318 -0.1278 0.1663 0.036 Uiso 1 1 calc R . . C19B C -0.19935(13) -0.17917(11) 0.12799(15) 0.0349(8) Uani 1 1 d . . . H19A H -0.2343 -0.1575 0.1315 0.042 Uiso 1 1 calc R . . C19A C 0.61178(13) 0.26106(10) 0.44434(14) 0.0309(7) Uani 1 1 d . . . H19B H 0.6165 0.2889 0.4764 0.037 Uiso 1 1 calc R . . C20A C 0.66568(12) 0.23740(10) 0.42647(14) 0.0296(7) Uani 1 1 d . . . H20A H 0.7064 0.2489 0.4457 0.036 Uiso 1 1 calc R . . C20B C -0.21081(13) -0.22756(11) 0.10134(15) 0.0365(8) Uani 1 1 d . . . H20B H -0.2529 -0.2383 0.0869 0.044 Uiso 1 1 calc R . . C21A C 0.65958(12) 0.19542(10) 0.37873(14) 0.0284(7) Uani 1 1 d . . . C21B C -0.15956(12) -0.26052(10) 0.09596(13) 0.0292(7) Uani 1 1 d . . . C22B C -0.16320(13) -0.30989(11) 0.06967(14) 0.0339(7) Uani 1 1 d . . . H22A H -0.2032 -0.3239 0.0527 0.041 Uiso 1 1 calc R . . C22A C 0.70899(12) 0.16666(10) 0.35505(15) 0.0317(7) Uani 1 1 d . . . H22B H 0.7518 0.1752 0.3703 0.038 Uiso 1 1 calc R . . C23B C -0.10912(13) -0.33807(10) 0.06843(14) 0.0305(7) Uani 1 1 d . . . H23A H -0.1127 -0.3712 0.0499 0.037 Uiso 1 1 calc R . . C23A C 0.69570(13) 0.12656(10) 0.31030(15) 0.0325(7) Uani 1 1 d . . . H23B H 0.7300 0.1077 0.2953 0.039 Uiso 1 1 calc R . . C24B C -0.04792(13) -0.31937(10) 0.09385(14) 0.0297(7) Uani 1 1 d . . . H24A H -0.0113 -0.3397 0.0928 0.036 Uiso 1 1 calc R . . C24A C 0.63277(12) 0.11173(10) 0.28507(14) 0.0281(7) Uani 1 1 d . . . H24B H 0.6252 0.0833 0.2545 0.034 Uiso 1 1 calc R . . C25B C 0.09594(11) -0.28581(9) 0.12998(13) 0.0221(6) Uani 1 1 d . . . C25A C 0.49502(11) 0.06301(9) 0.22700(13) 0.0229(6) Uani 1 1 d . . . C26B C 0.11146(11) -0.32816(9) 0.17345(14) 0.0241(6) Uani 1 1 d . . . C26A C 0.52079(13) 0.02478(9) 0.27428(14) 0.0289(7) Uani 1 1 d . . . C27B C 0.12988(12) -0.37105(9) 0.13932(14) 0.0260(7) Uani 1 1 d . . . H27A H 0.1394 -0.4004 0.1674 0.031 Uiso 1 1 calc R . . C27A C 0.54628(14) -0.01728(10) 0.24307(16) 0.0388(8) Uani 1 1 d . . . H27B H 0.5638 -0.0435 0.2736 0.047 Uiso 1 1 calc R . . C28B C 0.13470(12) -0.37238(9) 0.06611(14) 0.0282(7) Uani 1 1 d . . . H28A H 0.1467 -0.4025 0.0440 0.034 Uiso 1 1 calc R . . C28A C 0.54662(14) -0.02165(10) 0.16907(15) 0.0369(8) Uani 1 1 d . . . H28B H 0.5650 -0.0502 0.1491 0.044 Uiso 1 1 calc R . . C29B C 0.12202(12) -0.32956(10) 0.02424(15) 0.0295(7) Uani 1 1 d . . . H29A H 0.1276 -0.3301 -0.0259 0.035 Uiso 1 1 calc R . . C29A C 0.52044(13) 0.01517(9) 0.12444(15) 0.0317(7) Uani 1 1 d . . . H29B H 0.5205 0.0115 0.0735 0.038 Uiso 1 1 calc R . . C30A C 0.49361(12) 0.05803(9) 0.15177(13) 0.0247(6) Uani 1 1 d . . . C30B C 0.10130(12) -0.28615(9) 0.05550(13) 0.0255(6) Uani 1 1 d . . . C31B C 0.10607(12) -0.32646(10) 0.25455(14) 0.0277(7) Uani 1 1 d . . . H31A H 0.1067 -0.2906 0.2700 0.033 Uiso 1 1 calc R . . C31A C 0.51601(14) 0.02706(10) 0.35498(15) 0.0348(7) Uani 1 1 d . . . H31B H 0.5113 0.0631 0.3682 0.042 Uiso 1 1 calc R . . C32B C 0.16142(14) -0.35312(11) 0.29758(14) 0.0378(8) Uani 1 1 d . . . H32A H 0.2013 -0.3383 0.2860 0.057 Uiso 1 1 calc R . . H32B H 0.1606 -0.3887 0.2848 0.057 Uiso 1 1 calc R . . H32C H 0.1579 -0.3495 0.3496 0.057 Uiso 1 1 calc R . . C32A C 0.45713(16) -0.00030(14) 0.37368(17) 0.0539(10) Uani 1 1 d . . . H32D H 0.4197 0.0138 0.3454 0.081 Uiso 1 1 calc R . . H32E H 0.4530 0.0036 0.4255 0.081 Uiso 1 1 calc R . . H32F H 0.4607 -0.0360 0.3622 0.081 Uiso 1 1 calc R . . C33B C 0.04351(14) -0.34944(12) 0.27182(16) 0.0413(8) Uani 1 1 d . . . H33A H 0.0082 -0.3322 0.2439 0.062 Uiso 1 1 calc R . . H33B H 0.0395 -0.3458 0.3238 0.062 Uiso 1 1 calc R . . H33C H 0.0426 -0.3850 0.2589 0.062 Uiso 1 1 calc R . . C33A C 0.57500(16) 0.00706(13) 0.39974(17) 0.0520(10) Uani 1 1 d . . . H33D H 0.6122 0.0257 0.3876 0.078 Uiso 1 1 calc R . . H33E H 0.5803 -0.0285 0.3889 0.078 Uiso 1 1 calc R . . H33F H 0.5704 0.0111 0.4515 0.078 Uiso 1 1 calc R . . C34A C 0.46301(13) 0.09833(9) 0.10113(13) 0.0279(7) Uani 1 1 d . . . H34A H 0.4232 0.1090 0.1212 0.034 Uiso 1 1 calc R . . C34B C 0.08394(14) -0.24055(10) 0.00833(14) 0.0334(7) Uani 1 1 d . . . H34B H 0.0642 -0.2157 0.0394 0.040 Uiso 1 1 calc R . . C35A C 0.44422(15) 0.07929(11) 0.02434(15) 0.0391(8) Uani 1 1 d . . . H35A H 0.4168 0.0499 0.0261 0.059 Uiso 1 1 calc R . . H35B H 0.4824 0.0701 0.0019 0.059 Uiso 1 1 calc R . . H35C H 0.4214 0.1057 -0.0044 0.059 Uiso 1 1 calc R . . C35B C 0.14205(15) -0.21537(11) -0.01790(15) 0.0402(8) Uani 1 1 d . . . H35D H 0.1726 -0.2074 0.0239 0.060 Uiso 1 1 calc R . . H35E H 0.1291 -0.1845 -0.0439 0.060 Uiso 1 1 calc R . . H35F H 0.1617 -0.2381 -0.0505 0.060 Uiso 1 1 calc R . . C36B C 0.03472(14) -0.25274(12) -0.05534(16) 0.0425(8) Uani 1 1 d . . . H36A H -0.0021 -0.2686 -0.0372 0.064 Uiso 1 1 calc R . . H36B H 0.0532 -0.2756 -0.0887 0.064 Uiso 1 1 calc R . . H36C H 0.0215 -0.2218 -0.0810 0.064 Uiso 1 1 calc R . . C36A C 0.50492(15) 0.14490(11) 0.09876(17) 0.0432(8) Uani 1 1 d . . . H36D H 0.5166 0.1571 0.1482 0.065 Uiso 1 1 calc R . . H36E H 0.4816 0.1711 0.0701 0.065 Uiso 1 1 calc R . . H36F H 0.5433 0.1363 0.0764 0.065 Uiso 1 1 calc R . . C37A C 0.18796(15) 0.04859(12) 0.06497(17) 0.0486(9) Uani 1 1 d . . . H37A H 0.1439 0.0531 0.0769 0.058 Uiso 1 1 calc R . . H37B H 0.2063 0.0186 0.0905 0.058 Uiso 1 1 calc R . . C37B C 0.3723(2) -0.14275(17) 0.2021(3) 0.0858(15) Uani 1 1 d . . . H37C H 0.4037 -0.1491 0.2444 0.103 Uiso 1 1 calc R . . H37D H 0.3580 -0.1754 0.1810 0.103 Uiso 1 1 calc R . . C38A C 0.19002(16) 0.04400(13) -0.01570(17) 0.0510(10) Uani 1 1 d . . . H38A H 0.1807 0.0093 -0.0326 0.061 Uiso 1 1 calc R . . H38B H 0.1597 0.0673 -0.0426 0.061 Uiso 1 1 calc R . . C38B C 0.4014(2) -0.11285(16) 0.1477(2) 0.0780(14) Uani 1 1 d . . . H38C H 0.4475 -0.1092 0.1612 0.094 Uiso 1 1 calc R . . H38D H 0.3942 -0.1286 0.0992 0.094 Uiso 1 1 calc R . . C39A C 0.25653(17) 0.05801(13) -0.02408(19) 0.0550(10) Uani 1 1 d . . . H39A H 0.2609 0.0694 -0.0741 0.066 Uiso 1 1 calc R . . H39B H 0.2856 0.0295 -0.0122 0.066 Uiso 1 1 calc R . . C39B C 0.36931(17) -0.06411(13) 0.1484(2) 0.0798(12) Uani 1 1 d . . . H39C H 0.3630 -0.0499 0.0988 0.096 Uiso 1 1 calc R . . H39D H 0.3949 -0.0403 0.1802 0.096 Uiso 1 1 calc R . . C40A C 0.26968(16) 0.10012(12) 0.02957(17) 0.0484(9) Uani 1 1 d . . . H40A H 0.3141 0.0988 0.0520 0.058 Uiso 1 1 calc R . . H40B H 0.2622 0.1330 0.0055 0.058 Uiso 1 1 calc R . . C40B C 0.3077(2) -0.07301(16) 0.1762(3) 0.0839(14) Uani 1 1 d . . . H40C H 0.2941 -0.0430 0.2019 0.101 Uiso 1 1 calc R . . H40D H 0.2749 -0.0811 0.1359 0.101 Uiso 1 1 calc R . . C41A C 0.15783(15) 0.20786(11) 0.22434(16) 0.0433(9) Uani 1 1 d . . . H41A H 0.1957 0.2226 0.2522 0.052 Uiso 1 1 calc R . . H41B H 0.1329 0.1897 0.2583 0.052 Uiso 1 1 calc R . . C41B C 0.3698(2) -0.19117(16) 0.3736(2) 0.0779(14) Uani 1 1 d . . . H41C H 0.3576 -0.1911 0.4237 0.093 Uiso 1 1 calc R . . H41D H 0.3912 -0.1593 0.3642 0.093 Uiso 1 1 calc R . . C42A C 0.11884(17) 0.24732(14) 0.18473(17) 0.0574(10) Uani 1 1 d . . . H42A H 0.1211 0.2792 0.2120 0.069 Uiso 1 1 calc R . . H42B H 0.0740 0.2368 0.1751 0.069 Uiso 1 1 calc R . . C42B C 0.41179(18) -0.23789(16) 0.3589(3) 0.0901(14) Uani 1 1 d U . . H42C H 0.4366 -0.2317 0.3175 0.108 Uiso 1 1 calc R . . H42D H 0.4412 -0.2463 0.4022 0.108 Uiso 1 1 calc R . . C43B C 0.36348(17) -0.27939(13) 0.3415(2) 0.0584(11) Uani 1 1 d . . . H43A H 0.3723 -0.2982 0.2977 0.070 Uiso 1 1 calc R . . H43B H 0.3629 -0.3030 0.3826 0.070 Uiso 1 1 calc R . . C43A C 0.15014(17) 0.25205(12) 0.11422(17) 0.0504(9) Uani 1 1 d . . . H43C H 0.1205 0.2664 0.0749 0.061 Uiso 1 1 calc R . . H43D H 0.1886 0.2732 0.1212 0.061 Uiso 1 1 calc R . . C44A C 0.16629(15) 0.19955(11) 0.09800(15) 0.0400(8) Uani 1 1 d . . . H44A H 0.1313 0.1836 0.0667 0.048 Uiso 1 1 calc R . . H44B H 0.2052 0.1982 0.0729 0.048 Uiso 1 1 calc R . . C44B C 0.30539(19) -0.25254(14) 0.3293(3) 0.0916(16) Uani 1 1 d U . . H44C H 0.2805 -0.2656 0.2852 0.110 Uiso 1 1 calc R . . H44D H 0.2804 -0.2578 0.3709 0.110 Uiso 1 1 calc R . . C45A C 0.19356(14) 0.03403(11) 0.27941(16) 0.0387(8) Uani 1 1 d . . . H45A H 0.2303 0.0446 0.3134 0.046 Uiso 1 1 calc R . . H45B H 0.2045 0.0026 0.2554 0.046 Uiso 1 1 calc R . . C45B C 0.3057(3) -0.05706(16) 0.3706(2) 0.0863(15) Uani 1 1 d . . . H45C H 0.2898 -0.0351 0.3296 0.104 Uiso 1 1 calc R . . H45D H 0.3518 -0.0623 0.3700 0.104 Uiso 1 1 calc R . . C46A C 0.13479(16) 0.02672(13) 0.3198(2) 0.0577(10) Uani 1 1 d . . . H46A H 0.1222 -0.0090 0.3199 0.069 Uiso 1 1 calc R . . H46B H 0.1427 0.0386 0.3705 0.069 Uiso 1 1 calc R . . C46B C 0.2902(2) -0.03548(15) 0.4435(2) 0.0768(13) Uani 1 1 d . . . H46C H 0.3239 -0.0123 0.4639 0.092 Uiso 1 1 calc R . . H46D H 0.2493 -0.0174 0.4380 0.092 Uiso 1 1 calc R . . C47A C 0.08538(19) 0.0574(2) 0.2782(3) 0.0979(16) Uani 1 1 d U . . H47A H 0.0476 0.0364 0.2642 0.118 Uiso 1 1 calc R . . H47B H 0.0726 0.0851 0.3090 0.118 Uiso 1 1 calc R . . C47B C 0.2871(2) -0.07746(16) 0.4875(2) 0.0930(14) Uani 1 1 d U . . H47C H 0.2673 -0.0696 0.5322 0.112 Uiso 1 1 calc R . . H47D H 0.3295 -0.0924 0.5006 0.112 Uiso 1 1 calc R . . C48A C 0.10792(14) 0.07679(15) 0.2163(2) 0.0650(12) Uani 1 1 d . . . H48A H 0.0949 0.1122 0.2096 0.078 Uiso 1 1 calc R . . H48B H 0.0906 0.0576 0.1730 0.078 Uiso 1 1 calc R . . C48B C 0.2451(3) -0.11131(19) 0.4364(2) 0.0997(16) Uani 1 1 d U . . H48C H 0.2476 -0.1465 0.4533 0.120 Uiso 1 1 calc R . . H48D H 0.2004 -0.1002 0.4328 0.120 Uiso 1 1 calc R . . O1SA O 0.34009(14) -0.37449(11) 0.46921(16) 0.0802(9) Uani 1 1 d . . . C1SA C 0.3418(2) -0.42022(17) 0.4281(2) 0.0844(14) Uani 1 1 d . . . H1SA H 0.3599 -0.4477 0.4597 0.101 Uiso 1 1 calc R . . H1SB H 0.3686 -0.4158 0.3879 0.101 Uiso 1 1 calc R . . C2SA C 0.27594(19) -0.43241(15) 0.3989(2) 0.0707(13) Uani 1 1 d . . . H2SA H 0.2693 -0.4690 0.3933 0.085 Uiso 1 1 calc R . . H2SB H 0.2637 -0.4156 0.3519 0.085 Uiso 1 1 calc R . . C3SA C 0.24014(18) -0.41054(15) 0.4605(2) 0.0732(13) Uani 1 1 d . . . H3SA H 0.1950 -0.4041 0.4443 0.088 Uiso 1 1 calc R . . H3SB H 0.2436 -0.4324 0.5039 0.088 Uiso 1 1 calc R . . C4SA C 0.27664(16) -0.36371(14) 0.4732(2) 0.0640(12) Uani 1 1 d . . . H4SA H 0.2619 -0.3385 0.4361 0.077 Uiso 1 1 calc R . . H4SB H 0.2707 -0.3500 0.5216 0.077 Uiso 1 1 calc R . . O1SB O -0.2067(2) -0.00163(13) 0.3443(3) 0.1533(19) Uani 1 1 d . . . C1SB C -0.2361(3) -0.0385(2) 0.3836(4) 0.145(2) Uani 1 1 d . . . H1SC H -0.2045 -0.0562 0.4176 0.174 Uiso 1 1 calc R . . H1SG H -0.2684 -0.0233 0.4117 0.174 Uiso 1 1 calc R . . C2SB C -0.2644(2) -0.0715(2) 0.3314(3) 0.111(2) Uani 1 1 d . . . H2SC H -0.3108 -0.0719 0.3336 0.134 Uiso 1 1 calc R . . H2SD H -0.2481 -0.1058 0.3417 0.134 Uiso 1 1 calc R . . C3SB C -0.25055(11) -0.05606(4) 0.2569(2) 0.0918(16) Uani 1 1 d D . . H3SC H -0.2890 -0.0567 0.2218 0.110 Uiso 1 1 calc R . . H3SD H -0.2172 -0.0771 0.2387 0.110 Uiso 1 1 calc R . . C4SB C -0.22745(18) -0.00254(6) 0.2733(3) 0.146(2) Uani 1 1 d DU . . H4SC H -0.1928 0.0062 0.2438 0.175 Uiso 1 1 calc R . . H4SD H -0.2625 0.0217 0.2624 0.175 Uiso 1 1 calc R . . C1SC C 0.00102(7) -0.46853(6) 0.04446(10) 0.0609(11) Uani 1 1 d D . . H1SD H 0.0000 -0.4755 0.0968 0.073 Uiso 0.50 1 calc PR A 1 H1SE H 0.0039 -0.4324 0.0335 0.073 Uiso 0.50 1 calc PR A 1 H1SF H -0.0112 -0.4849 0.0889 0.073 Uiso 0.50 1 calc PR A 2 H1SH H 0.0137 -0.4342 0.0603 0.073 Uiso 0.50 1 calc PR A 2 O1SC O -0.04150(12) -0.49719(11) -0.00434(16) 0.101(2) Uani 0.50 1 d PDU . 1 C2SC C -0.0583(3) -0.45937(4) 0.00717(10) 0.055(2) Uani 0.50 1 d PD . 2 H2SE H -0.0581 -0.4290 -0.0235 0.067 Uiso 0.50 1 calc PR . 2 H2SF H -0.0915 -0.4560 0.0407 0.067 Uiso 0.50 1 calc PR . 2 C3SC C -0.0671(4) -0.50701(6) -0.03864(15) 0.095(3) Uani 0.50 1 d PDU . 2 H3SE H -0.0875 -0.4987 -0.0877 0.115 Uiso 0.50 1 calc PR . 2 H3SF H -0.0948 -0.5308 -0.0158 0.115 Uiso 0.50 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 Cr1A 0.02127(19) 0.02094(19) 0.02292(19) -0.00390(16) 0.00227(16) -0.00025(16) Cr1B 0.0220(2) 0.0199(2) 0.0250(2) -0.00206(16) 0.00065(17) -0.00139(16) Cl1A 0.0228(3) 0.0348(3) 0.0271(3) -0.0039(3) 0.0046(3) 0.0004(3) Cl1B 0.0354(3) 0.0334(3) 0.0235(3) 0.0030(3) 0.0017(3) -0.0085(3) Mg1A 0.0235(4) 0.0269(4) 0.0289(4) -0.0013(4) 0.0013(4) -0.0025(4) Mg1B 0.0260(4) 0.0252(4) 0.0236(4) -0.0014(3) 0.0005(4) -0.0034(4) N1A 0.0241(10) 0.0191(10) 0.0217(10) -0.0024(8) 0.0030(9) -0.0008(8) O1B 0.0368(10) 0.0276(9) 0.0353(10) 0.0030(8) 0.0021(9) -0.0065(8) N1B 0.0278(11) 0.0206(10) 0.0240(10) 0.0007(9) 0.0023(9) -0.0009(9) C1B 0.0280(13) 0.0201(12) 0.0317(14) -0.0003(11) -0.0028(11) -0.0002(11) C1A 0.0183(12) 0.0233(12) 0.0262(13) -0.0059(10) 0.0028(10) 0.0015(10) O1A 0.0313(10) 0.0391(10) 0.0343(10) -0.0054(8) 0.0023(8) -0.0063(8) Cl2A 0.0292(3) 0.0286(3) 0.0270(3) 0.0031(3) 0.0005(3) -0.0049(3) Cl2B 0.0306(3) 0.0215(3) 0.0431(4) 0.0016(3) -0.0065(3) -0.0033(3) O2A 0.0334(10) 0.0337(10) 0.0286(9) -0.0005(8) -0.0008(8) 0.0067(8) N2A 0.0258(10) 0.0191(10) 0.0223(10) 0.0009(8) 0.0040(9) 0.0006(9) N2B 0.0226(10) 0.0220(10) 0.0250(10) -0.0017(9) 0.0046(9) -0.0007(9) O2B 0.0330(10) 0.0253(9) 0.0466(11) 0.0038(8) -0.0095(9) -0.0024(8) C2A 0.0209(12) 0.0230(12) 0.0281(13) -0.0008(11) 0.0039(11) -0.0009(10) C2B 0.0359(14) 0.0247(13) 0.0311(14) -0.0036(11) -0.0003(12) 0.0034(12) Cl3A 0.0272(3) 0.0223(3) 0.0403(4) -0.0064(3) 0.0015(3) -0.0028(3) Cl3B 0.0240(3) 0.0465(4) 0.0340(3) -0.0162(3) 0.0026(3) -0.0026(3) O3B 0.0387(10) 0.0455(11) 0.0271(9) -0.0106(8) 0.0058(8) -0.0139(9) O3A 0.0269(9) 0.0390(11) 0.0453(11) 0.0057(9) 0.0072(9) -0.0048(8) C3A 0.0257(13) 0.0209(12) 0.0337(14) -0.0056(11) 0.0028(11) 0.0003(11) C3B 0.0532(18) 0.0280(14) 0.0418(16) -0.0070(13) 0.0046(14) 0.0063(13) C4A 0.0271(13) 0.0289(13) 0.0292(13) -0.0128(11) 0.0037(11) 0.0032(11) C4B 0.073(2) 0.0212(14) 0.0498(18) -0.0013(13) 0.0032(17) 0.0178(14) C5A 0.0269(13) 0.0377(15) 0.0213(12) -0.0038(11) 0.0062(11) 0.0000(12) C5B 0.0581(19) 0.0254(14) 0.0425(17) 0.0077(13) 0.0005(15) 0.0031(14) C6A 0.0204(12) 0.0261(13) 0.0260(13) -0.0040(11) -0.0005(11) 0.0001(10) C6B 0.0376(15) 0.0302(14) 0.0308(14) 0.0036(12) 0.0026(12) 0.0007(12) C7A 0.0400(15) 0.0185(12) 0.0279(13) -0.0015(11) 0.0061(12) 0.0013(11) C7B 0.0538(17) 0.0291(14) 0.0272(14) -0.0011(12) 0.0058(13) 0.0093(13) C8A 0.0478(17) 0.0412(16) 0.0317(15) 0.0111(13) -0.0036(14) 0.0103(14) C8B 0.0553(18) 0.0504(18) 0.0329(15) 0.0000(14) 0.0089(14) 0.0203(15) C9A 0.0539(19) 0.0474(18) 0.0394(16) 0.0034(14) 0.0154(15) -0.0094(15) C9B 0.061(2) 0.0425(17) 0.0416(17) -0.0048(14) 0.0180(15) -0.0021(15) C10A 0.0338(14) 0.0263(13) 0.0264(13) 0.0015(11) 0.0003(12) 0.0030(11) C10B 0.0394(15) 0.0390(15) 0.0324(14) 0.0098(12) 0.0060(13) 0.0046(13) C11A 0.0438(16) 0.0327(15) 0.0401(16) 0.0101(13) 0.0058(14) -0.0007(13) C11B 0.0397(16) 0.0571(19) 0.0457(17) 0.0172(15) -0.0006(15) -0.0070(15) C12B 0.0534(18) 0.0499(18) 0.0347(16) -0.0006(14) 0.0101(14) -0.0057(16) C12A 0.0409(17) 0.0439(17) 0.0556(19) 0.0184(15) -0.0030(15) 0.0063(14) C13B 0.0239(12) 0.0241(12) 0.0215(12) 0.0005(10) 0.0044(10) 0.0004(10) C13A 0.0249(13) 0.0217(12) 0.0194(12) 0.0000(10) 0.0032(10) -0.0001(10) C14A 0.0232(12) 0.0241(12) 0.0197(12) 0.0013(10) 0.0021(10) 0.0008(10) C14B 0.0269(13) 0.0304(13) 0.0193(12) 0.0032(10) 0.0007(11) -0.0002(11) C15A 0.0272(13) 0.0215(12) 0.0198(12) 0.0033(10) 0.0020(10) 0.0015(10) C15B 0.0217(12) 0.0349(14) 0.0226(12) 0.0035(11) 0.0046(11) -0.0015(11) C16B 0.0281(13) 0.0248(13) 0.0206(12) 0.0012(10) 0.0047(11) -0.0067(11) C16A 0.0246(12) 0.0223(12) 0.0248(12) 0.0023(10) 0.0020(11) -0.0020(10) C17A 0.0210(12) 0.0227(12) 0.0221(12) 0.0000(10) 0.0048(10) 0.0020(10) C17B 0.0225(12) 0.0254(12) 0.0177(11) 0.0034(10) 0.0051(10) -0.0028(10) C18A 0.0266(13) 0.0249(13) 0.0269(13) -0.0002(11) 0.0017(11) 0.0007(11) C18B 0.0309(14) 0.0321(14) 0.0272(13) 0.0034(11) 0.0010(12) 0.0046(12) C19B 0.0227(13) 0.0492(17) 0.0324(14) 0.0030(13) 0.0011(12) 0.0064(12) C19A 0.0358(14) 0.0278(13) 0.0282(13) -0.0032(11) -0.0011(12) -0.0049(12) C20A 0.0291(14) 0.0302(14) 0.0283(13) 0.0020(11) -0.0032(11) -0.0098(12) C20B 0.0224(13) 0.0538(18) 0.0328(15) 0.0078(13) 0.0012(12) -0.0023(13) C21A 0.0250(13) 0.0327(14) 0.0273(13) 0.0092(11) 0.0027(11) -0.0026(11) C21B 0.0268(13) 0.0392(15) 0.0211(13) 0.0051(11) 0.0005(11) -0.0061(12) C22B 0.0299(14) 0.0464(16) 0.0247(13) -0.0036(12) 0.0000(12) -0.0147(13) C22A 0.0190(13) 0.0385(15) 0.0377(15) 0.0050(12) 0.0030(12) 0.0004(12) C23B 0.0339(14) 0.0325(14) 0.0253(13) -0.0038(11) 0.0042(12) -0.0098(12) C23A 0.0242(13) 0.0381(15) 0.0363(15) 0.0035(12) 0.0089(12) 0.0053(12) C24B 0.0294(14) 0.0317(14) 0.0281(14) -0.0031(11) 0.0039(12) -0.0043(12) C24A 0.0322(14) 0.0256(13) 0.0275(13) -0.0001(11) 0.0074(11) 0.0015(11) C25B 0.0173(11) 0.0196(12) 0.0292(13) -0.0028(10) 0.0020(10) -0.0053(10) C25A 0.0236(12) 0.0179(12) 0.0283(13) -0.0049(10) 0.0077(11) -0.0017(10) C26B 0.0193(12) 0.0225(12) 0.0305(13) -0.0014(11) 0.0030(11) -0.0066(10) C26A 0.0345(14) 0.0205(13) 0.0313(14) 0.0020(11) 0.0021(12) -0.0005(11) C27B 0.0240(13) 0.0221(12) 0.0319(14) -0.0003(11) 0.0025(11) -0.0009(11) C27A 0.0448(16) 0.0223(14) 0.0502(17) 0.0080(13) 0.0092(14) 0.0074(13) C28B 0.0304(14) 0.0218(13) 0.0327(14) -0.0092(11) 0.0052(12) -0.0028(11) C28A 0.0488(16) 0.0218(13) 0.0423(16) -0.0081(12) 0.0152(14) 0.0063(12) C29B 0.0291(13) 0.0283(14) 0.0311(14) -0.0014(11) 0.0034(12) -0.0033(11) C29A 0.0416(15) 0.0220(13) 0.0324(14) -0.0053(11) 0.0081(12) 0.0000(12) C30A 0.0243(12) 0.0233(12) 0.0275(13) -0.0013(10) 0.0070(11) -0.0023(11) C30B 0.0248(13) 0.0255(13) 0.0265(13) -0.0024(11) 0.0043(11) -0.0017(11) C31B 0.0319(14) 0.0237(13) 0.0276(13) -0.0009(11) 0.0036(11) -0.0003(11) C31A 0.0474(16) 0.0256(14) 0.0318(14) 0.0059(12) 0.0063(13) 0.0000(13) C32B 0.0435(16) 0.0445(17) 0.0239(14) -0.0031(12) -0.0036(13) 0.0055(14) C32A 0.0500(19) 0.076(2) 0.0361(17) 0.0093(16) 0.0069(15) -0.0048(18) C33B 0.0390(16) 0.0555(18) 0.0314(15) 0.0054(14) 0.0130(13) -0.0006(15) C33A 0.0501(19) 0.062(2) 0.0424(18) 0.0137(16) -0.0022(16) -0.0014(16) C34A 0.0329(14) 0.0253(13) 0.0257(13) -0.0010(11) 0.0032(11) -0.0030(11) C34B 0.0463(16) 0.0265(14) 0.0275(14) -0.0030(11) 0.0043(13) 0.0038(13) C35A 0.0490(17) 0.0378(16) 0.0298(14) -0.0036(12) 0.0004(13) 0.0035(14) C35B 0.0586(18) 0.0345(15) 0.0271(14) 0.0050(12) 0.0034(14) -0.0110(14) C36B 0.0410(16) 0.0451(17) 0.0405(16) 0.0089(14) -0.0002(14) 0.0052(14) C36A 0.0459(17) 0.0384(16) 0.0431(17) 0.0073(14) -0.0052(14) -0.0087(14) C37A 0.0416(17) 0.0544(19) 0.0493(18) -0.0177(15) 0.0029(15) -0.0211(15) C37B 0.068(2) 0.075(3) 0.120(3) 0.023(3) 0.037(2) 0.012(2) C38A 0.0529(19) 0.0511(19) 0.0470(18) -0.0103(15) -0.0051(16) -0.0019(16) C38B 0.074(3) 0.072(3) 0.092(3) 0.003(2) 0.030(2) 0.002(2) C39A 0.061(2) 0.055(2) 0.0502(19) -0.0198(16) 0.0130(17) -0.0119(17) C39B 0.094(2) 0.0369(19) 0.125(3) 0.0178(18) 0.087(2) 0.0065(17) C40A 0.0564(19) 0.0477(18) 0.0438(17) -0.0083(14) 0.0180(15) -0.0136(16) C40B 0.083(3) 0.063(3) 0.111(3) 0.016(2) 0.038(3) 0.004(2) C41A 0.0479(17) 0.0453(17) 0.0370(16) -0.0069(13) 0.0055(14) 0.0155(14) C41B 0.086(3) 0.066(2) 0.074(3) 0.001(2) -0.026(2) 0.004(2) C42A 0.071(2) 0.067(2) 0.0358(17) 0.0053(15) 0.0139(16) 0.0321(18) C42B 0.048(2) 0.083(3) 0.135(3) 0.051(2) -0.011(2) 0.004(2) C43B 0.060(2) 0.054(2) 0.058(2) -0.0042(17) -0.0080(18) 0.0196(17) C43A 0.067(2) 0.0469(18) 0.0379(17) 0.0072(14) 0.0072(16) 0.0140(16) C44A 0.0409(16) 0.0507(18) 0.0270(14) 0.0033(13) -0.0036(13) 0.0082(14) C44B 0.060(2) 0.0350(19) 0.173(4) 0.013(2) -0.022(3) -0.0006(18) C45A 0.0373(15) 0.0312(15) 0.0488(17) 0.0045(13) 0.0109(14) 0.0003(13) C45B 0.120(4) 0.066(3) 0.070(3) -0.005(2) 0.000(3) -0.028(3) C46A 0.059(2) 0.054(2) 0.066(2) 0.0135(17) 0.0282(17) 0.0051(17) C46B 0.095(3) 0.067(2) 0.061(2) -0.0309(19) -0.026(2) 0.014(2) C47A 0.042(2) 0.157(4) 0.096(3) 0.056(3) 0.017(2) 0.011(2) C47B 0.136(3) 0.092(3) 0.053(2) -0.0284(19) 0.014(2) -0.063(2) C48A 0.0267(16) 0.076(2) 0.093(3) 0.029(2) 0.0077(18) -0.0081(16) C48B 0.134(3) 0.105(3) 0.063(2) -0.021(2) 0.027(2) -0.051(3) O1SA 0.0747(18) 0.0749(18) 0.091(2) -0.0136(15) 0.0087(16) -0.0015(15) C1SA 0.069(3) 0.101(3) 0.085(3) -0.043(2) 0.017(2) 0.006(2) C2SA 0.081(3) 0.061(2) 0.069(2) -0.002(2) 0.002(2) 0.005(2) C3SA 0.050(2) 0.070(2) 0.099(3) 0.038(2) 0.006(2) -0.0007(19) C4SA 0.047(2) 0.054(2) 0.090(3) -0.007(2) -0.002(2) 0.0089(17) O1SB 0.148(3) 0.0572(19) 0.242(5) -0.043(2) -0.041(3) -0.018(2) C1SB 0.098(4) 0.153(5) 0.187(5) -0.097(4) 0.029(4) -0.010(4) C2SB 0.075(3) 0.156(5) 0.106(4) -0.044(3) 0.029(3) -0.020(3) C3SB 0.107(3) 0.062(3) 0.113(4) -0.012(2) 0.039(3) -0.014(2) C4SB 0.158(5) 0.139(4) 0.140(4) 0.034(4) 0.017(4) 0.057(4) C1SC 0.078(2) 0.051(2) 0.056(2) 0.0039(17) 0.0125(19) -0.0085(19) O1SC 0.146(5) 0.088(4) 0.064(3) 0.023(3) -0.011(4) -0.001(4) C2SC 0.069(4) 0.026(3) 0.075(5) 0.004(3) 0.024(4) 0.020(3) C3SC 0.078(5) 0.052(4) 0.149(6) 0.008(4) -0.023(4) -0.018(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 Cr1A N1A 2.0183(19) . ? Cr1A N2A 2.035(2) . ? Cr1A Cl3A 2.4126(7) . ? Cr1A Cl1A 2.4223(7) . ? Cr1A Cl2A 2.5617(7) . ? Cr1A Mg1A 3.0964(9) . ? Cr1B N2B 2.023(2) . ? Cr1B N1B 2.027(2) . ? Cr1B Cl3B 2.4243(8) . ? Cr1B Cl2B 2.4373(7) . ? Cr1B Cl1B 2.5316(7) . ? Cr1B Mg1B 3.1249(9) . ? Cl1A Mg1A 2.4972(10) . ? Cl1B Mg1B 2.4758(11) . ? Mg1A O2A 2.0645(19) . ? Mg1A O3A 2.080(2) . ? Mg1A O1A 2.088(2) . ? Mg1A Cl2A 2.4812(11) . ? Mg1A Cl3A 2.5236(10) . ? Mg1B O2B 2.0664(19) . ? Mg1B O3B 2.0825(19) . ? Mg1B O1B 2.086(2) . ? Mg1B Cl3B 2.4800(10) . ? Mg1B Cl2B 2.5169(10) . ? N1A C13A 1.334(3) . ? N1A C1A 1.438(3) . ? O1B C40B 1.442(5) . ? O1B C37B 1.485(5) . ? N1B C13B 1.342(3) . ? N1B C1B 1.435(3) . ? C1B C6B 1.397(4) . ? C1B C2B 1.406(4) . ? C1A C6A 1.400(3) . ? C1A C2A 1.415(3) . ? O1A C37A 1.440(4) . ? O1A C40A 1.464(4) . ? O2A C44A 1.454(3) . ? O2A C41A 1.465(3) . ? N2A C17A 1.348(3) . ? N2A C25A 1.437(3) . ? N2B C17B 1.335(3) . ? N2B C25B 1.428(3) . ? O2B C44B 1.422(4) . ? O2B C41B 1.439(4) . ? C2A C3A 1.389(4) . ? C2A C7A 1.514(4) . ? C2B C3B 1.388(4) . ? C2B C7B 1.512(4) . ? O3B C48B 1.422(5) . ? O3B C45B 1.508(5) . ? O3A C48A 1.449(4) . ? O3A C45A 1.460(3) . ? C3A C4A 1.373(4) . ? C3B C4B 1.367(4) . ? C4A C5A 1.379(4) . ? C4B C5B 1.385(4) . ? C5A C6A 1.389(4) . ? C5B C6B 1.404(4) . ? C6A C10A 1.515(4) . ? C6B C10B 1.513(4) . ? C7A C8A 1.529(4) . ? C7A C9A 1.541(4) . ? C7B C8B 1.519(4) . ? C7B C9B 1.527(4) . ? C10A C11A 1.523(4) . ? C10A C12A 1.534(4) . ? C10B C12B 1.511(4) . ? C10B C11B 1.529(4) . ? C13B C17B 1.411(3) . ? C13B C14B 1.468(3) . ? C13A C17A 1.408(3) . ? C13A C14A 1.456(3) . ? C14A C18A 1.385(3) . ? C14A C15A 1.418(4) . ? C14B C18B 1.379(4) . ? C14B C15B 1.428(4) . ? C15A C21A 1.396(4) . ? C15A C16A 1.431(3) . ? C15B C21B 1.391(3) . ? C15B C16B 1.420(4) . ? C16B C24B 1.381(4) . ? C16B C17B 1.470(3) . ? C16A C24A 1.367(4) . ? C16A C17A 1.478(3) . ? C18A C19A 1.408(4) . ? C18B C19B 1.405(4) . ? C19B C20B 1.395(4) . ? C19A C20A 1.378(4) . ? C20A C21A 1.426(4) . ? C20B C21B 1.411(4) . ? C21A C22A 1.407(4) . ? C21B C22B 1.405(4) . ? C22B C23B 1.375(4) . ? C22A C23A 1.366(4) . ? C23B C24B 1.425(4) . ? C23A C24A 1.424(4) . ? C25B C30B 1.397(3) . ? C25B C26B 1.407(3) . ? C25A C30A 1.398(3) . ? C25A C26A 1.417(3) . ? C26B C27B 1.384(4) . ? C26B C31B 1.520(4) . ? C26A C27A 1.398(4) . ? C26A C31A 1.511(4) . ? C27B C28B 1.372(4) . ? C27A C28A 1.377(4) . ? C28B C29B 1.392(4) . ? C28A C29A 1.365(4) . ? C29B C30B 1.388(4) . ? C29A C30A 1.397(4) . ? C30A C34A 1.527(3) . ? C30B C34B 1.521(4) . ? C31B C32B 1.525(4) . ? C31B C33B 1.527(4) . ? C31A C32A 1.519(4) . ? C31A C33A 1.524(4) . ? C34A C35A 1.524(4) . ? C34A C36A 1.532(4) . ? C34B C36B 1.527(4) . ? C34B C35B 1.529(4) . ? C37A C38A 1.505(5) . ? C37B C38B 1.470(6) . ? C38A C39A 1.485(5) . ? C38B C39B 1.469(5) . ? C39A C40A 1.507(4) . ? C39B C40B 1.474(6) . ? C41A C42A 1.485(4) . ? C41B C42B 1.574(6) . ? C42A C43A 1.532(5) . ? C42B C43B 1.521(5) . ? C43B C44B 1.424(5) . ? C43A C44A 1.481(4) . ? C45A C46A 1.533(5) . ? C45B C46B 1.535(6) . ? C46A C47A 1.481(5) . ? C46B C47B 1.391(6) . ? C47A C48A 1.389(6) . ? C47B C48B 1.527(6) . ? O1SA C4SA 1.387(5) . ? O1SA C1SA 1.442(5) . ? C1SA C2SA 1.482(6) . ? C2SA C3SA 1.551(6) . ? C3SA C4SA 1.477(5) . ? O1SB C4SB 1.343(7) . ? O1SB C1SB 1.412(8) . ? C1SB C2SB 1.396(8) . ? C2SB C3SB 1.499(7) . ? C3SB C4SB 1.5310(10) . ? C1SC C2SC 1.394(6) . ? C1SC O1SC 1.4308(10) . ? C1SC O1SC 1.505(4) 3_545 ? C1SC C3SC 1.562(8) 3_545 ? O1SC C1SC 1.505(4) 3_545 ? O1SC O1SC 1.759(5) 3_545 ? C2SC C3SC 1.5299(10) . ? C3SC C1SC 1.563(8) 3_545 ? 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 N1A Cr1A N2A 80.99(8) . . ? N1A Cr1A Cl3A 167.58(6) . . ? N2A Cr1A Cl3A 94.86(6) . . ? N1A Cr1A Cl1A 93.36(6) . . ? N2A Cr1A Cl1A 160.73(6) . . ? Cl3A Cr1A Cl1A 86.76(2) . . ? N1A Cr1A Cl2A 105.99(6) . . ? N2A Cr1A Cl2A 114.50(6) . . ? Cl3A Cr1A Cl2A 86.40(2) . . ? Cl1A Cr1A Cl2A 84.76(2) . . ? N1A Cr1A Mg1A 135.22(6) . . ? N2A Cr1A Mg1A 140.97(6) . . ? Cl3A Cr1A Mg1A 52.77(2) . . ? Cl1A Cr1A Mg1A 52.08(2) . . ? Cl2A Cr1A Mg1A 50.95(2) . . ? N2B Cr1B N1B 80.55(8) . . ? N2B Cr1B Cl3B 93.72(6) . . ? N1B Cr1B Cl3B 158.68(6) . . ? N2B Cr1B Cl2B 166.02(6) . . ? N1B Cr1B Cl2B 94.68(6) . . ? Cl3B Cr1B Cl2B 85.99(3) . . ? N2B Cr1B Cl1B 109.78(6) . . ? N1B Cr1B Cl1B 116.38(6) . . ? Cl3B Cr1B Cl1B 84.91(2) . . ? Cl2B Cr1B Cl1B 84.13(2) . . ? N2B Cr1B Mg1B 136.30(6) . . ? N1B Cr1B Mg1B 141.72(6) . . ? Cl3B Cr1B Mg1B 51.21(2) . . ? Cl2B Cr1B Mg1B 52.04(2) . . ? Cl1B Cr1B Mg1B 50.59(2) . . ? Cr1A Cl1A Mg1A 78.00(3) . . ? Mg1B Cl1B Cr1B 77.22(3) . . ? O2A Mg1A O3A 89.13(8) . . ? O2A Mg1A O1A 89.97(8) . . ? O3A Mg1A O1A 90.92(8) . . ? O2A Mg1A Cl2A 91.00(6) . . ? O3A Mg1A Cl2A 174.92(7) . . ? O1A Mg1A Cl2A 94.16(6) . . ? O2A Mg1A Cl1A 98.90(6) . . ? O3A Mg1A Cl1A 90.04(6) . . ? O1A Mg1A Cl1A 171.09(7) . . ? Cl2A Mg1A Cl1A 84.92(3) . . ? O2A Mg1A Cl3A 176.23(7) . . ? O3A Mg1A Cl3A 94.24(6) . . ? O1A Mg1A Cl3A 88.29(6) . . ? Cl2A Mg1A Cl3A 85.80(3) . . ? Cl1A Mg1A Cl3A 82.81(3) . . ? O2A Mg1A Cr1A 129.38(6) . . ? O3A Mg1A Cr1A 123.32(6) . . ? O1A Mg1A Cr1A 123.02(6) . . ? Cl2A Mg1A Cr1A 53.31(2) . . ? Cl1A Mg1A Cr1A 49.92(2) . . ? Cl3A Mg1A Cr1A 49.57(2) . . ? O2B Mg1B O3B 87.79(8) . . ? O2B Mg1B O1B 88.34(8) . . ? O3B Mg1B O1B 89.97(8) . . ? O2B Mg1B Cl1B 93.66(6) . . ? O3B Mg1B Cl1B 93.51(6) . . ? O1B Mg1B Cl1B 176.05(6) . . ? O2B Mg1B Cl3B 93.43(6) . . ? O3B Mg1B Cl3B 178.09(7) . . ? O1B Mg1B Cl3B 91.54(6) . . ? Cl1B Mg1B Cl3B 84.94(3) . . ? O2B Mg1B Cl2B 175.79(7) . . ? O3B Mg1B Cl2B 95.59(6) . . ? O1B Mg1B Cl2B 94.16(6) . . ? Cl1B Mg1B Cl2B 83.66(3) . . ? Cl3B Mg1B Cl2B 83.13(3) . . ? O2B Mg1B Cr1B 126.04(6) . . ? O3B Mg1B Cr1B 128.46(6) . . ? O1B Mg1B Cr1B 123.97(6) . . ? Cl1B Mg1B Cr1B 52.19(2) . . ? Cl3B Mg1B Cr1B 49.64(2) . . ? Cl2B Mg1B Cr1B 49.77(2) . . ? C13A N1A C1A 116.32(19) . . ? C13A N1A Cr1A 112.73(15) . . ? C1A N1A Cr1A 130.82(16) . . ? C40B O1B C37B 105.7(3) . . ? C40B O1B Mg1B 126.1(2) . . ? C37B O1B Mg1B 121.3(2) . . ? C13B N1B C1B 116.4(2) . . ? C13B N1B Cr1B 112.76(16) . . ? C1B N1B Cr1B 130.31(16) . . ? C6B C1B C2B 122.1(2) . . ? C6B C1B N1B 117.9(2) . . ? C2B C1B N1B 119.9(2) . . ? C6A C1A C2A 121.8(2) . . ? C6A C1A N1A 118.6(2) . . ? C2A C1A N1A 119.5(2) . . ? C37A O1A C40A 108.8(2) . . ? C37A O1A Mg1A 124.49(17) . . ? C40A O1A Mg1A 121.49(16) . . ? Mg1A Cl2A Cr1A 75.74(3) . . ? Cr1B Cl2B Mg1B 78.19(3) . . ? C44A O2A C41A 109.1(2) . . ? C44A O2A Mg1A 122.33(17) . . ? C41A O2A Mg1A 121.65(15) . . ? C17A N2A C25A 117.1(2) . . ? C17A N2A Cr1A 111.76(16) . . ? C25A N2A Cr1A 130.77(15) . . ? C17B N2B C25B 114.88(19) . . ? C17B N2B Cr1B 112.85(16) . . ? C25B N2B Cr1B 131.21(15) . . ? C44B O2B C41B 102.7(3) . . ? C44B O2B Mg1B 123.6(2) . . ? C41B O2B Mg1B 128.8(2) . . ? C3A C2A C1A 117.2(2) . . ? C3A C2A C7A 121.3(2) . . ? C1A C2A C7A 121.5(2) . . ? C3B C2B C1B 117.2(2) . . ? C3B C2B C7B 121.8(3) . . ? C1B C2B C7B 121.0(2) . . ? Cr1A Cl3A Mg1A 77.66(3) . . ? Cr1B Cl3B Mg1B 79.15(3) . . ? C48B O3B C45B 107.3(3) . . ? C48B O3B Mg1B 125.7(2) . . ? C45B O3B Mg1B 126.0(2) . . ? C48A O3A C45A 107.9(2) . . ? C48A O3A Mg1A 130.16(19) . . ? C45A O3A Mg1A 121.05(16) . . ? C4A C3A C2A 121.7(2) . . ? C4B C3B C2B 122.4(3) . . ? C3A C4A C5A 120.1(2) . . ? C3B C4B C5B 119.5(3) . . ? C4A C5A C6A 121.3(2) . . ? C4B C5B C6B 121.2(3) . . ? C5A C6A C1A 117.8(2) . . ? C5A C6A C10A 120.6(2) . . ? C1A C6A C10A 121.6(2) . . ? C1B C6B C5B 117.5(3) . . ? C1B C6B C10B 121.5(2) . . ? C5B C6B C10B 120.9(2) . . ? C2A C7A C8A 111.1(2) . . ? C2A C7A C9A 111.5(2) . . ? C8A C7A C9A 111.0(2) . . ? C2B C7B C8B 109.7(2) . . ? C2B C7B C9B 112.9(2) . . ? C8B C7B C9B 111.0(2) . . ? C6A C10A C11A 111.8(2) . . ? C6A C10A C12A 111.5(2) . . ? C11A C10A C12A 111.0(2) . . ? C12B C10B C6B 111.4(2) . . ? C12B C10B C11B 110.7(2) . . ? C6B C10B C11B 111.5(2) . . ? N1B C13B C17B 116.5(2) . . ? N1B C13B C14B 134.6(2) . . ? C17B C13B C14B 108.8(2) . . ? N1A C13A C17A 117.2(2) . . ? N1A C13A C14A 133.3(2) . . ? C17A C13A C14A 109.3(2) . . ? C18A C14A C15A 117.5(2) . . ? C18A C14A C13A 136.9(2) . . ? C15A C14A C13A 105.5(2) . . ? C18B C14B C15B 117.2(2) . . ? C18B C14B C13B 137.5(2) . . ? C15B C14B C13B 105.3(2) . . ? C21A C15A C14A 124.5(2) . . ? C21A C15A C16A 123.5(2) . . ? C14A C15A C16A 111.9(2) . . ? C21B C15B C16B 123.7(2) . . ? C21B C15B C14B 124.6(2) . . ? C16B C15B C14B 111.7(2) . . ? C24B C16B C15B 118.3(2) . . ? C24B C16B C17B 136.2(2) . . ? C15B C16B C17B 105.4(2) . . ? C24A C16A C15A 118.3(2) . . ? C24A C16A C17A 137.1(2) . . ? C15A C16A C17A 104.6(2) . . ? N2A C17A C13A 117.1(2) . . ? N2A C17A C16A 134.3(2) . . ? C13A C17A C16A 108.6(2) . . ? N2B C17B C13B 117.1(2) . . ? N2B C17B C16B 133.9(2) . . ? C13B C17B C16B 108.8(2) . . ? C14A C18A C19A 118.8(2) . . ? C14B C18B C19B 119.4(3) . . ? C20B C19B C18B 122.5(3) . . ? C20A C19A C18A 123.6(2) . . ? C19A C20A C21A 119.1(2) . . ? C19B C20B C21B 119.7(2) . . ? C15A C21A C22A 116.6(2) . . ? C15A C21A C20A 116.5(2) . . ? C22A C21A C20A 126.9(2) . . ? C15B C21B C22B 117.0(2) . . ? C15B C21B C20B 116.5(2) . . ? C22B C21B C20B 126.5(2) . . ? C23B C22B C21B 120.3(2) . . ? C23A C22A C21A 120.3(2) . . ? C22B C23B C24B 122.5(3) . . ? C22A C23A C24A 123.0(3) . . ? C16B C24B C23B 118.3(2) . . ? C16A C24A C23A 118.3(2) . . ? C30B C25B C26B 121.5(2) . . ? C30B C25B N2B 118.4(2) . . ? C26B C25B N2B 120.0(2) . . ? C30A C25A C26A 121.0(2) . . ? C30A C25A N2A 120.3(2) . . ? C26A C25A N2A 118.7(2) . . ? C27B C26B C25B 117.6(2) . . ? C27B C26B C31B 122.1(2) . . ? C25B C26B C31B 120.3(2) . . ? C27A C26A C25A 117.6(2) . . ? C27A C26A C31A 120.7(2) . . ? C25A C26A C31A 121.4(2) . . ? C28B C27B C26B 121.8(2) . . ? C28A C27A C26A 121.5(3) . . ? C27B C28B C29B 120.0(2) . . ? C29A C28A C27A 119.9(3) . . ? C30B C29B C28B 120.3(2) . . ? C28A C29A C30A 121.7(3) . . ? C29A C30A C25A 118.2(2) . . ? C29A C30A C34A 121.2(2) . . ? C25A C30A C34A 120.6(2) . . ? C29B C30B C25B 118.7(2) . . ? C29B C30B C34B 119.8(2) . . ? C25B C30B C34B 121.5(2) . . ? C26B C31B C32B 111.7(2) . . ? C26B C31B C33B 110.7(2) . . ? C32B C31B C33B 110.0(2) . . ? C26A C31A C32A 110.4(2) . . ? C26A C31A C33A 112.8(2) . . ? C32A C31A C33A 110.9(2) . . ? C35A C34A C30A 113.0(2) . . ? C35A C34A C36A 109.8(2) . . ? C30A C34A C36A 112.2(2) . . ? C30B C34B C36B 112.2(2) . . ? C30B C34B C35B 112.3(2) . . ? C36B C34B C35B 111.0(2) . . ? O1A C37A C38A 103.8(3) . . ? C38B C37B O1B 108.9(3) . . ? C39A C38A C37A 102.2(3) . . ? C39B C38B C37B 104.3(4) . . ? C38A C39A C40A 103.4(3) . . ? C38B C39B C40B 106.8(3) . . ? O1A C40A C39A 105.3(3) . . ? O1B C40B C39B 105.8(3) . . ? O2A C41A C42A 104.9(2) . . ? O2B C41B C42B 99.6(3) . . ? C41A C42A C43A 102.2(3) . . ? C43B C42B C41B 103.4(3) . . ? C44B C43B C42B 102.7(3) . . ? C44A C43A C42A 103.0(3) . . ? O2A C44A C43A 105.9(2) . . ? O2B C44B C43B 111.2(3) . . ? O3A C45A C46A 105.4(2) . . ? O3B C45B C46B 101.2(3) . . ? C47A C46A C45A 104.1(3) . . ? C47B C46B C45B 103.9(3) . . ? C48A C47A C46A 110.5(3) . . ? C46B C47B C48B 100.1(3) . . ? C47A C48A O3A 107.6(3) . . ? O3B C48B C47B 103.8(4) . . ? C4SA O1SA C1SA 106.4(3) . . ? O1SA C1SA C2SA 107.6(3) . . ? C1SA C2SA C3SA 99.5(3) . . ? C4SA C3SA C2SA 98.4(3) . . ? O1SA C4SA C3SA 108.2(3) . . ? C4SB O1SB C1SB 112.1(4) . . ? C2SB C1SB O1SB 105.2(6) . . ? C1SB C2SB C3SB 110.8(5) . . ? C2SB C3SB C4SB 99.4(4) . . ? O1SB C4SB C3SB 106.1(3) . . ? C2SC C1SC O1SC 45.80(14) . . ? C2SC C1SC O1SC 113.3(2) . 3_545 ? O1SC C1SC O1SC 73.57(19) . 3_545 ? C2SC C1SC C3SC 144.2(2) . 3_545 ? O1SC C1SC C3SC 104.15(19) . 3_545 ? O1SC C1SC C3SC 31.51(13) 3_545 3_545 ? C1SC O1SC C1SC 106.42(19) . 3_545 ? C1SC O1SC O1SC 55.14(12) . 3_545 ? C1SC O1SC O1SC 51.28(15) 3_545 3_545 ? C1SC C2SC C3SC 100.4(4) . . ? C2SC C3SC C1SC 109.1(5) . 3_545 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.642 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.092 _publ_section_references ; Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2000) SMART. Bruker Molecular Analysis Research Tool, v. 5.625 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; # Attachment 'B909814C_compound_3.cif' data_crbian2m _database_code_depnum_ccdc_archive 'CCDC 732683' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H112 Cl2 Cr2 N4 O4' _chemical_formula_weight 1464.72 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9610(4) _cell_length_b 12.6123(5) _cell_length_c 15.0320(6) _cell_angle_alpha 82.2590(10) _cell_angle_beta 78.5530(10) _cell_angle_gamma 65.1620(10) _cell_volume 2013.61(13) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 0.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8268 _exptl_absorpt_correction_T_max 0.9550 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17855 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8249 _reflns_number_gt 6458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.1134P)^2^+0.7239P] 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 8249 _refine_ls_number_parameters 461 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1798 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.095 _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 0.41352(3) 0.05085(3) 0.10271(2) 0.02888(10) Uani 1 1 d U . . Cl1 Cl 0.49212(5) -0.12911(5) 0.02974(4) 0.03604(14) Uani 1 1 d U . . N1 N 0.38059(17) 0.18625(16) 0.17578(14) 0.0314(4) Uani 1 1 d U . . N2 N 0.35879(17) -0.01607(17) 0.22548(14) 0.0330(4) Uani 1 1 d . . . C1 C 0.3176(2) 0.1762(2) 0.25810(17) 0.0332(5) Uani 1 1 d U . . C2 C 0.3048(2) 0.0691(2) 0.28494(16) 0.0337(5) Uani 1 1 d . . . C3 C 0.2357(2) 0.0761(2) 0.37819(17) 0.0396(6) Uani 1 1 d . . . C4 C 0.2101(2) 0.1892(2) 0.40415(18) 0.0427(6) Uani 1 1 d . . . C5 C 0.2586(2) 0.2536(2) 0.33440(18) 0.0399(6) Uani 1 1 d . . . C6 C 0.2430(2) 0.3649(2) 0.3504(2) 0.0485(7) Uani 1 1 d . . . H6A H 0.2754 0.4098 0.3055 0.058 Uiso 1 1 calc R . . C7 C 0.1773(3) 0.4098(3) 0.4359(2) 0.0604(9) Uani 1 1 d . . . H7A H 0.1661 0.4861 0.4475 0.073 Uiso 1 1 calc R . . C8 C 0.1294(3) 0.3484(3) 0.5021(2) 0.0642(10) Uani 1 1 d . . . H8A H 0.0852 0.3828 0.5580 0.077 Uiso 1 1 calc R . . C9 C 0.1451(2) 0.2324(3) 0.4883(2) 0.0533(8) Uani 1 1 d . . . C10 C 0.1029(3) 0.1564(3) 0.5495(2) 0.0632(10) Uani 1 1 d . . . H10A H 0.0582 0.1812 0.6080 0.076 Uiso 1 1 calc R . . C11 C 0.1260(3) 0.0471(3) 0.5250(2) 0.0608(9) Uani 1 1 d . . . H11A H 0.0955 -0.0014 0.5673 0.073 Uiso 1 1 calc R . . C12 C 0.1937(2) 0.0031(3) 0.43906(19) 0.0482(7) Uani 1 1 d . . . H12A H 0.2092 -0.0733 0.4242 0.058 Uiso 1 1 calc R . . C13 C 0.4197(2) 0.2807(2) 0.15643(18) 0.0357(5) Uani 1 1 d . . . C14 C 0.5269(2) 0.2703(2) 0.18822(19) 0.0418(6) Uani 1 1 d . . . C15 C 0.5603(3) 0.3658(3) 0.1731(2) 0.0501(7) Uani 1 1 d . . . H15A H 0.6322 0.3604 0.1945 0.060 Uiso 1 1 calc R . . C16 C 0.4917(3) 0.4662(3) 0.1282(3) 0.0660(9) Uani 1 1 d . . . H16A H 0.5137 0.5314 0.1205 0.079 Uiso 1 1 calc R . . C17 C 0.3895(3) 0.4732(3) 0.0936(3) 0.0723(10) Uani 1 1 d . . . H17A H 0.3437 0.5429 0.0608 0.087 Uiso 1 1 calc R . . C18 C 0.3527(2) 0.3815(2) 0.1057(2) 0.0488(7) Uani 1 1 d . . . C19 C 0.6073(3) 0.1580(3) 0.2348(3) 0.0624(9) Uani 1 1 d . . . H19A H 0.5760 0.0974 0.2297 0.075 Uiso 1 1 calc R . . C20 C 0.7435(3) 0.1137(3) 0.1895(3) 0.0717(10) Uani 1 1 d . . . H20A H 0.7923 0.0403 0.2211 0.108 Uiso 1 1 calc R . . H20B H 0.7763 0.1722 0.1925 0.108 Uiso 1 1 calc R . . H20C H 0.7493 0.0999 0.1258 0.108 Uiso 1 1 calc R . . C21 C 0.5975(4) 0.1716(5) 0.3352(3) 0.1015(15) Uani 1 1 d U . . H21A H 0.5098 0.1994 0.3637 0.152 Uiso 1 1 calc R . . H21B H 0.6309 0.2284 0.3423 0.152 Uiso 1 1 calc R . . H21C H 0.6456 0.0959 0.3643 0.152 Uiso 1 1 calc R . . C22 C 0.2381(3) 0.3930(2) 0.0685(2) 0.0555(8) Uani 1 1 d . . . H22A H 0.2373 0.3134 0.0737 0.067 Uiso 1 1 calc R . . C23 C 0.1190(3) 0.4722(3) 0.1251(3) 0.0696(10) Uani 1 1 d . . . H23A H 0.1185 0.4437 0.1891 0.104 Uiso 1 1 calc R . . H23B H 0.0468 0.4720 0.1038 0.104 Uiso 1 1 calc R . . H23C H 0.1149 0.5521 0.1189 0.104 Uiso 1 1 calc R . . C24 C 0.2426(3) 0.4344(3) -0.0312(3) 0.0673(9) Uani 1 1 d . . . H24A H 0.3204 0.3821 -0.0662 0.101 Uiso 1 1 calc R . . H24B H 0.2389 0.5141 -0.0383 0.101 Uiso 1 1 calc R . . H24C H 0.1713 0.4337 -0.0537 0.101 Uiso 1 1 calc R . . C25 C 0.3798(2) -0.1339(2) 0.25958(17) 0.0384(6) Uani 1 1 d . . . C26 C 0.4725(3) -0.1930(2) 0.31468(18) 0.0425(6) Uani 1 1 d . . . C27 C 0.4866(3) -0.3049(3) 0.3515(2) 0.0566(8) Uani 1 1 d . . . H27A H 0.5471 -0.3453 0.3904 0.068 Uiso 1 1 calc R . . C28 C 0.4151(4) -0.3576(3) 0.3327(3) 0.0697(10) Uani 1 1 d . . . H28A H 0.4252 -0.4330 0.3596 0.084 Uiso 1 1 calc R . . C29 C 0.3290(3) -0.3020(3) 0.2754(3) 0.0667(9) Uani 1 1 d . . . H29A H 0.2815 -0.3403 0.2617 0.080 Uiso 1 1 calc R . . C30 C 0.3099(3) -0.1891(2) 0.2366(2) 0.0466(7) Uani 1 1 d . . . C31 C 0.5589(3) -0.1413(3) 0.3326(2) 0.0547(8) Uani 1 1 d . . . H31A H 0.5321 -0.0605 0.3029 0.066 Uiso 1 1 calc R . . C32 C 0.5529(3) -0.1314(4) 0.4325(3) 0.0860(13) Uani 1 1 d . . . H32A H 0.4665 -0.0859 0.4595 0.129 Uiso 1 1 calc R . . H32B H 0.6056 -0.0921 0.4400 0.129 Uiso 1 1 calc R . . H32C H 0.5829 -0.2098 0.4629 0.129 Uiso 1 1 calc R . . C33 C 0.6935(3) -0.2124(4) 0.2892(2) 0.0696(10) Uani 1 1 d . . . H33A H 0.6963 -0.2178 0.2243 0.104 Uiso 1 1 calc R . . H33B H 0.7235 -0.2912 0.3190 0.104 Uiso 1 1 calc R . . H33C H 0.7466 -0.1735 0.2967 0.104 Uiso 1 1 calc R . . C34 C 0.2119(2) -0.1276(3) 0.1746(2) 0.0502(7) Uani 1 1 d . . . H34A H 0.2242 -0.0564 0.1453 0.060 Uiso 1 1 calc R . . C35 C 0.0811(3) -0.0868(4) 0.2290(3) 0.0769(11) Uani 1 1 d . . . H35A H 0.0739 -0.0378 0.2770 0.115 Uiso 1 1 calc R . . H35B H 0.0649 -0.1550 0.2566 0.115 Uiso 1 1 calc R . . H35C H 0.0201 -0.0414 0.1886 0.115 Uiso 1 1 calc R . . C36 C 0.2255(3) -0.2042(3) 0.0982(3) 0.0605(8) Uani 1 1 d . . . H36A H 0.1609 -0.1608 0.0601 0.091 Uiso 1 1 calc R . . H36B H 0.2162 -0.2759 0.1249 0.091 Uiso 1 1 calc R . . H36C H 0.3080 -0.2245 0.0609 0.091 Uiso 1 1 calc R . . O1S O 0.22550(15) 0.12341(15) 0.05342(12) 0.0391(4) Uani 1 1 d . . . C1S C 0.2148(3) 0.1305(3) -0.0413(2) 0.0585(8) Uani 1 1 d . . . H1SA H 0.2616 0.0527 -0.0670 0.070 Uiso 1 1 calc R . . H1SB H 0.2481 0.1860 -0.0764 0.070 Uiso 1 1 calc R . . C2S C 0.0792(3) 0.1723(4) -0.0446(3) 0.0792(12) Uani 1 1 d . . . H2SA H 0.0567 0.2242 -0.0996 0.095 Uiso 1 1 calc R . . H2SB H 0.0564 0.1054 -0.0449 0.095 Uiso 1 1 calc R . . C3S C 0.0151(3) 0.2372(4) 0.0389(3) 0.0844(13) Uani 1 1 d . . . H3SA H -0.0656 0.2308 0.0612 0.101 Uiso 1 1 calc R . . H3SB H -0.0005 0.3210 0.0271 0.101 Uiso 1 1 calc R . . C4S C 0.1019(2) 0.1808(2) 0.1061(2) 0.0467(7) Uani 1 1 d . . . H4SA H 0.1008 0.2402 0.1435 0.056 Uiso 1 1 calc R . . H4SB H 0.0777 0.1228 0.1468 0.056 Uiso 1 1 calc R . . O2S O -0.14310(19) 0.31971(12) 0.25266(12) 0.0701(7) Uani 1 1 d D A . C5S C -0.0970(3) 0.2442(2) 0.32895(13) 0.0847(13) Uani 1 1 d D A . H5SA H -0.0059 0.2200 0.3236 0.102 Uiso 1 1 calc R . . H5SB H -0.1141 0.1733 0.3329 0.102 Uiso 1 1 calc R . . C6S C -0.1647(2) 0.31398(15) 0.41180(17) 0.1025(17) Uani 1 1 d D . . H6SA H -0.1121 0.2907 0.4571 0.123 Uiso 1 1 d . . . H6SB H -0.2387 0.2982 0.4364 0.123 Uiso 1 1 d . . . C7S C -0.1550(3) 0.4265(2) 0.37053(18) 0.081(2) Uani 0.592(8) 1 d PD A 1 H7SA H -0.2116 0.4935 0.4076 0.097 Uiso 0.592(8) 1 calc PR A 1 H7SB H -0.0685 0.4204 0.3635 0.097 Uiso 0.592(8) 1 calc PR A 1 C7S' C -0.2569(4) 0.4287(3) 0.3765(2) 0.085(3) Uani 0.408(8) 1 d PDU A 2 H7SC H -0.2673 0.4947 0.4109 0.102 Uiso 0.408(8) 1 calc PR A 2 H7SD H -0.3393 0.4265 0.3790 0.102 Uiso 0.408(8) 1 calc PR A 2 C8S C -0.1950(3) 0.43744(15) 0.27945(17) 0.0831(12) Uani 1 1 d D . . H8SA H -0.2750 0.4786 0.2641 0.100 Uiso 1 1 d . . . H8SB H -0.1404 0.4751 0.2469 0.100 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.02822(17) 0.02679(18) 0.0323(2) -0.00794(14) -0.00630(14) -0.00927(14) Cl1 0.0403(3) 0.0289(3) 0.0390(3) -0.0072(2) -0.0052(2) -0.0130(2) N1 0.0268(8) 0.0298(9) 0.0380(10) -0.0072(8) -0.0100(8) -0.0082(7) N2 0.0296(9) 0.0290(9) 0.0356(10) -0.0076(8) -0.0068(8) -0.0050(7) C1 0.0235(10) 0.0317(11) 0.0407(12) -0.0125(9) -0.0124(9) -0.0014(9) C2 0.0259(10) 0.0371(12) 0.0335(12) -0.0081(10) -0.0072(9) -0.0053(9) C3 0.0262(11) 0.0478(14) 0.0357(13) -0.0080(11) -0.0086(9) -0.0028(10) C4 0.0245(10) 0.0521(15) 0.0426(14) -0.0176(12) -0.0122(10) 0.0005(10) C5 0.0267(11) 0.0411(13) 0.0459(14) -0.0185(11) -0.0138(10) 0.0003(10) C6 0.0338(12) 0.0460(14) 0.0615(17) -0.0247(13) -0.0173(12) -0.0015(11) C7 0.0418(14) 0.0591(17) 0.072(2) -0.0408(16) -0.0201(14) 0.0031(13) C8 0.0391(14) 0.079(2) 0.0564(18) -0.0426(17) -0.0149(13) 0.0077(15) C9 0.0288(12) 0.074(2) 0.0412(15) -0.0242(14) -0.0099(11) 0.0022(13) C10 0.0349(14) 0.093(3) 0.0393(15) -0.0188(16) -0.0070(12) 0.0007(15) C11 0.0378(14) 0.085(2) 0.0399(16) -0.0033(15) -0.0029(12) -0.0079(15) C12 0.0353(13) 0.0589(17) 0.0393(14) -0.0032(12) -0.0065(11) -0.0078(12) C13 0.0309(10) 0.0301(11) 0.0485(14) -0.0141(10) -0.0104(10) -0.0094(9) C14 0.0340(11) 0.0431(13) 0.0514(15) -0.0102(11) -0.0137(11) -0.0134(10) C15 0.0422(13) 0.0524(15) 0.0653(18) -0.0176(13) -0.0164(13) -0.0208(12) C16 0.0674(17) 0.0427(15) 0.109(3) -0.0102(16) -0.0401(18) -0.0293(14) C17 0.0736(18) 0.0337(14) 0.127(3) 0.0041(16) -0.057(2) -0.0231(13) C18 0.0461(13) 0.0288(12) 0.080(2) -0.0052(12) -0.0310(13) -0.0133(10) C19 0.0446(14) 0.0663(19) 0.087(2) 0.0170(16) -0.0389(15) -0.0270(14) C20 0.0468(16) 0.0512(17) 0.119(3) -0.0206(18) -0.0332(18) -0.0084(14) C21 0.0572(19) 0.146(3) 0.086(3) 0.024(2) -0.0304(18) -0.026(2) C22 0.0498(14) 0.0311(13) 0.095(2) 0.0040(13) -0.0416(15) -0.0147(11) C23 0.0488(16) 0.0459(17) 0.115(3) -0.0047(18) -0.0411(18) -0.0078(14) C24 0.0712(18) 0.0445(16) 0.103(3) 0.0138(16) -0.0563(18) -0.0268(14) C25 0.0380(12) 0.0349(12) 0.0359(13) -0.0066(10) -0.0006(10) -0.0097(10) C26 0.0498(14) 0.0359(13) 0.0360(13) -0.0067(10) -0.0097(11) -0.0091(11) C27 0.0726(19) 0.0443(16) 0.0423(16) 0.0049(12) -0.0180(14) -0.0118(14) C28 0.091(2) 0.0491(18) 0.067(2) 0.0184(15) -0.0201(19) -0.0294(17) C29 0.077(2) 0.0535(18) 0.078(2) 0.0093(16) -0.0162(18) -0.0360(16) C30 0.0480(14) 0.0416(14) 0.0525(16) 0.0023(12) -0.0082(12) -0.0215(11) C31 0.0618(16) 0.0391(14) 0.0608(18) -0.0029(13) -0.0380(14) -0.0058(13) C32 0.0482(17) 0.109(3) 0.081(2) -0.057(2) -0.0253(16) 0.0098(18) C33 0.072(2) 0.097(3) 0.0469(18) -0.0145(17) -0.0074(16) -0.0395(19) C34 0.0397(13) 0.0452(14) 0.072(2) 0.0015(13) -0.0126(13) -0.0231(11) C35 0.0483(17) 0.079(2) 0.103(3) 0.001(2) -0.0044(19) -0.0310(17) C36 0.0610(16) 0.0491(16) 0.089(2) 0.0028(15) -0.0306(16) -0.0333(13) O1S 0.0295(8) 0.0394(9) 0.0475(10) -0.0076(7) -0.0135(7) -0.0083(7) C1S 0.0536(15) 0.072(2) 0.0532(17) -0.0067(15) -0.0287(14) -0.0186(15) C2S 0.0557(18) 0.083(2) 0.100(3) -0.020(2) -0.0471(19) -0.0095(18) C3S 0.0460(17) 0.106(3) 0.092(3) -0.006(2) -0.0293(18) -0.0139(19) C4S 0.0283(11) 0.0395(13) 0.0681(18) -0.0018(13) -0.0091(12) -0.0094(10) O2S 0.0554(12) 0.0642(14) 0.0878(17) -0.0300(12) -0.0225(12) -0.0090(11) C5S 0.062(2) 0.0515(19) 0.137(4) -0.011(2) -0.052(2) -0.0020(16) C6S 0.075(2) 0.127(4) 0.084(3) -0.002(3) -0.043(2) -0.008(3) C7S 0.073(4) 0.059(3) 0.103(5) -0.048(3) -0.048(3) 0.008(3) C7S' 0.088(5) 0.074(4) 0.089(5) -0.030(3) -0.032(4) -0.014(3) C8S 0.106(3) 0.0541(19) 0.108(3) 0.0012(19) -0.060(2) -0.0336(19) _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 2.0116(19) . ? Cr1 N2 2.028(2) . ? Cr1 O1S 2.2790(16) . ? Cr1 Cl1 2.3890(6) . ? Cr1 Cl1 2.3931(7) 2_655 ? Cl1 Cr1 2.3930(7) 2_655 ? N1 C1 1.335(3) . ? N1 C13 1.429(3) . ? N2 C2 1.348(3) . ? N2 C25 1.437(3) . ? C1 C2 1.418(4) . ? C1 C5 1.473(3) . ? C2 C3 1.472(3) . ? C3 C12 1.385(4) . ? C3 C4 1.420(4) . ? C4 C9 1.393(4) . ? C4 C5 1.422(4) . ? C5 C6 1.384(4) . ? C6 C7 1.418(4) . ? C7 C8 1.362(5) . ? C8 C9 1.433(5) . ? C9 C10 1.416(5) . ? C10 C11 1.374(5) . ? C11 C12 1.426(4) . ? C13 C18 1.402(4) . ? C13 C14 1.405(3) . ? C14 C15 1.398(4) . ? C14 C19 1.510(4) . ? C15 C16 1.360(4) . ? C16 C17 1.385(4) . ? C17 C18 1.380(4) . ? C18 C22 1.526(4) . ? C19 C21 1.517(6) . ? C19 C20 1.525(5) . ? C22 C23 1.517(5) . ? C22 C24 1.518(5) . ? C25 C30 1.405(4) . ? C25 C26 1.406(4) . ? C26 C27 1.398(4) . ? C26 C31 1.512(4) . ? C27 C28 1.370(5) . ? C28 C29 1.370(5) . ? C29 C30 1.405(4) . ? C30 C34 1.522(4) . ? C31 C32 1.509(5) . ? C31 C33 1.532(5) . ? C34 C35 1.521(4) . ? C34 C36 1.541(5) . ? O1S C1S 1.442(4) . ? O1S C4S 1.458(3) . ? C1S C2S 1.489(4) . ? C2S C3S 1.484(6) . ? C3S C4S 1.485(5) . ? O2S C8S 1.4282(10) . ? O2S C5S 1.4287(10) . ? C5S C6S 1.5089(10) . ? C6S C7S' 1.5093(10) . ? C6S C7S 1.5110(10) . ? C7S C8S 1.5085(10) . ? C7S' C8S 1.5114(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 N2 82.59(8) . . ? N1 Cr1 O1S 97.49(7) . . ? N2 Cr1 O1S 96.68(7) . . ? N1 Cr1 Cl1 167.88(6) . . ? N2 Cr1 Cl1 94.57(6) . . ? O1S Cr1 Cl1 94.54(5) . . ? N1 Cr1 Cl1 92.50(6) . 2_655 ? N2 Cr1 Cl1 169.68(6) . 2_655 ? O1S Cr1 Cl1 92.94(5) . 2_655 ? Cl1 Cr1 Cl1 88.36(2) . 2_655 ? Cr1 Cl1 Cr1 91.64(2) . 2_655 ? C1 N1 C13 118.28(19) . . ? C1 N1 Cr1 110.12(16) . . ? C13 N1 Cr1 131.44(16) . . ? C2 N2 C25 118.0(2) . . ? C2 N2 Cr1 109.48(16) . . ? C25 N2 Cr1 132.07(15) . . ? N1 C1 C2 118.1(2) . . ? N1 C1 C5 133.5(2) . . ? C2 C1 C5 108.3(2) . . ? N2 C2 C1 117.3(2) . . ? N2 C2 C3 133.7(2) . . ? C1 C2 C3 108.9(2) . . ? C12 C3 C4 119.0(3) . . ? C12 C3 C2 135.9(3) . . ? C4 C3 C2 105.1(2) . . ? C9 C4 C3 124.1(3) . . ? C9 C4 C5 123.6(3) . . ? C3 C4 C5 112.3(2) . . ? C6 C5 C4 119.0(2) . . ? C6 C5 C1 135.7(3) . . ? C4 C5 C1 105.3(2) . . ? C5 C6 C7 117.9(3) . . ? C8 C7 C6 123.0(3) . . ? C7 C8 C9 120.6(3) . . ? C4 C9 C10 116.1(3) . . ? C4 C9 C8 115.9(3) . . ? C10 C9 C8 128.1(3) . . ? C11 C10 C9 120.5(3) . . ? C10 C11 C12 123.1(3) . . ? C3 C12 C11 117.3(3) . . ? C18 C13 C14 120.6(2) . . ? C18 C13 N1 120.4(2) . . ? C14 C13 N1 119.0(2) . . ? C15 C14 C13 118.4(2) . . ? C15 C14 C19 120.2(2) . . ? C13 C14 C19 121.4(3) . . ? C16 C15 C14 121.2(3) . . ? C15 C16 C17 119.7(3) . . ? C18 C17 C16 121.7(3) . . ? C17 C18 C13 118.2(3) . . ? C17 C18 C22 120.4(3) . . ? C13 C18 C22 121.4(2) . . ? C14 C19 C21 111.5(3) . . ? C14 C19 C20 111.9(3) . . ? C21 C19 C20 110.1(3) . . ? C23 C22 C24 111.1(3) . . ? C23 C22 C18 110.9(3) . . ? C24 C22 C18 112.2(3) . . ? C30 C25 C26 120.9(2) . . ? C30 C25 N2 120.2(2) . . ? C26 C25 N2 118.9(2) . . ? C27 C26 C25 118.1(3) . . ? C27 C26 C31 119.6(3) . . ? C25 C26 C31 122.3(2) . . ? C28 C27 C26 121.4(3) . . ? C29 C28 C27 120.3(3) . . ? C28 C29 C30 121.0(3) . . ? C25 C30 C29 118.2(3) . . ? C25 C30 C34 121.5(2) . . ? C29 C30 C34 120.3(3) . . ? C32 C31 C26 112.9(3) . . ? C32 C31 C33 110.1(2) . . ? C26 C31 C33 110.7(3) . . ? C35 C34 C30 111.0(3) . . ? C35 C34 C36 110.6(3) . . ? C30 C34 C36 112.5(2) . . ? C1S O1S C4S 109.4(2) . . ? C1S O1S Cr1 122.41(16) . . ? C4S O1S Cr1 127.82(16) . . ? O1S C1S C2S 106.1(3) . . ? C3S C2S C1S 105.1(3) . . ? C2S C3S C4S 105.0(3) . . ? O1S C4S C3S 106.2(3) . . ? C8S O2S C5S 107.73(19) . . ? O2S C5S C6S 106.16(19) . . ? C5S C6S C7S' 105.2(2) . . ? C5S C6S C7S 95.9(2) . . ? C7S' C6S C7S 46.5(3) . . ? C8S C7S C6S 101.8(2) . . ? C6S C7S' C8S 101.8(2) . . ? O2S C8S C7S 103.9(2) . . ? O2S C8S C7S' 103.3(3) . . ? C7S C8S C7S' 46.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cr1 Cl1 Cr1 -94.2(3) . . . 2_655 ? N2 Cr1 Cl1 Cr1 -170.09(6) . . . 2_655 ? O1S Cr1 Cl1 Cr1 92.82(5) . . . 2_655 ? Cl1 Cr1 Cl1 Cr1 0.0 2_655 . . 2_655 ? N2 Cr1 N1 C1 -12.94(15) . . . . ? O1S Cr1 N1 C1 82.87(15) . . . . ? Cl1 Cr1 N1 C1 -90.0(3) . . . . ? Cl1 Cr1 N1 C1 176.16(14) 2_655 . . . ? N2 Cr1 N1 C13 162.2(2) . . . . ? O1S Cr1 N1 C13 -102.01(19) . . . . ? Cl1 Cr1 N1 C13 85.1(4) . . . . ? Cl1 Cr1 N1 C13 -8.72(19) 2_655 . . . ? N1 Cr1 N2 C2 13.27(15) . . . . ? O1S Cr1 N2 C2 -83.45(16) . . . . ? Cl1 Cr1 N2 C2 -178.57(15) . . . . ? Cl1 Cr1 N2 C2 75.3(4) 2_655 . . . ? N1 Cr1 N2 C25 -158.8(2) . . . . ? O1S Cr1 N2 C25 104.5(2) . . . . ? Cl1 Cr1 N2 C25 9.4(2) . . . . ? Cl1 Cr1 N2 C25 -96.8(4) 2_655 . . . ? C13 N1 C1 C2 -165.24(19) . . . . ? Cr1 N1 C1 C2 10.6(2) . . . . ? C13 N1 C1 C5 11.5(4) . . . . ? Cr1 N1 C1 C5 -172.6(2) . . . . ? C25 N2 C2 C1 161.8(2) . . . . ? Cr1 N2 C2 C1 -11.6(2) . . . . ? C25 N2 C2 C3 -15.2(4) . . . . ? Cr1 N2 C2 C3 171.5(2) . . . . ? N1 C1 C2 N2 0.8(3) . . . . ? C5 C1 C2 N2 -176.75(19) . . . . ? N1 C1 C2 C3 178.45(19) . . . . ? C5 C1 C2 C3 0.9(3) . . . . ? N2 C2 C3 C12 -4.1(5) . . . . ? C1 C2 C3 C12 178.7(3) . . . . ? N2 C2 C3 C4 176.8(2) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C12 C3 C4 C9 0.4(4) . . . . ? C2 C3 C4 C9 179.7(2) . . . . ? C12 C3 C4 C5 -179.6(2) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C9 C4 C5 C6 1.2(4) . . . . ? C3 C4 C5 C6 -178.8(2) . . . . ? C9 C4 C5 C1 -179.1(2) . . . . ? C3 C4 C5 C1 0.9(3) . . . . ? N1 C1 C5 C6 1.5(5) . . . . ? C2 C1 C5 C6 178.5(3) . . . . ? N1 C1 C5 C4 -178.1(2) . . . . ? C2 C1 C5 C4 -1.1(2) . . . . ? C4 C5 C6 C7 -0.9(4) . . . . ? C1 C5 C6 C7 179.5(3) . . . . ? C5 C6 C7 C8 0.0(4) . . . . ? C6 C7 C8 C9 0.8(4) . . . . ? C3 C4 C9 C10 -0.4(4) . . . . ? C5 C4 C9 C10 179.7(2) . . . . ? C3 C4 C9 C8 179.5(2) . . . . ? C5 C4 C9 C8 -0.4(4) . . . . ? C7 C8 C9 C4 -0.5(4) . . . . ? C7 C8 C9 C10 179.4(3) . . . . ? C4 C9 C10 C11 -0.2(4) . . . . ? C8 C9 C10 C11 179.9(3) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C4 C3 C12 C11 0.2(4) . . . . ? C2 C3 C12 C11 -178.8(3) . . . . ? C10 C11 C12 C3 -0.8(4) . . . . ? C1 N1 C13 C18 -100.9(3) . . . . ? Cr1 N1 C13 C18 84.3(3) . . . . ? C1 N1 C13 C14 79.7(3) . . . . ? Cr1 N1 C13 C14 -95.1(3) . . . . ? C18 C13 C14 C15 4.0(4) . . . . ? N1 C13 C14 C15 -176.6(2) . . . . ? C18 C13 C14 C19 -173.9(3) . . . . ? N1 C13 C14 C19 5.5(4) . . . . ? C13 C14 C15 C16 -0.4(4) . . . . ? C19 C14 C15 C16 177.5(3) . . . . ? C14 C15 C16 C17 -2.5(5) . . . . ? C15 C16 C17 C18 1.9(6) . . . . ? C16 C17 C18 C13 1.7(6) . . . . ? C16 C17 C18 C22 178.7(4) . . . . ? C14 C13 C18 C17 -4.6(5) . . . . ? N1 C13 C18 C17 176.0(3) . . . . ? C14 C13 C18 C22 178.4(3) . . . . ? N1 C13 C18 C22 -1.0(4) . . . . ? C15 C14 C19 C21 71.5(4) . . . . ? C13 C14 C19 C21 -110.6(3) . . . . ? C15 C14 C19 C20 -52.4(4) . . . . ? C13 C14 C19 C20 125.5(3) . . . . ? C17 C18 C22 C23 -73.5(4) . . . . ? C13 C18 C22 C23 103.4(3) . . . . ? C17 C18 C22 C24 51.4(4) . . . . ? C13 C18 C22 C24 -131.6(3) . . . . ? C2 N2 C25 C30 110.1(3) . . . . ? Cr1 N2 C25 C30 -78.3(3) . . . . ? C2 N2 C25 C26 -71.0(3) . . . . ? Cr1 N2 C25 C26 100.5(3) . . . . ? C30 C25 C26 C27 -4.8(4) . . . . ? N2 C25 C26 C27 176.3(2) . . . . ? C30 C25 C26 C31 173.3(3) . . . . ? N2 C25 C26 C31 -5.6(4) . . . . ? C25 C26 C27 C28 1.9(4) . . . . ? C31 C26 C27 C28 -176.2(3) . . . . ? C26 C27 C28 C29 1.3(5) . . . . ? C27 C28 C29 C30 -1.6(6) . . . . ? C26 C25 C30 C29 4.5(4) . . . . ? N2 C25 C30 C29 -176.6(3) . . . . ? C26 C25 C30 C34 -178.1(3) . . . . ? N2 C25 C30 C34 0.8(4) . . . . ? C28 C29 C30 C25 -1.3(5) . . . . ? C28 C29 C30 C34 -178.7(3) . . . . ? C27 C26 C31 C32 -59.2(4) . . . . ? C25 C26 C31 C32 122.7(3) . . . . ? C27 C26 C31 C33 64.8(4) . . . . ? C25 C26 C31 C33 -113.3(3) . . . . ? C25 C30 C34 C35 -104.2(3) . . . . ? C29 C30 C34 C35 73.2(4) . . . . ? C25 C30 C34 C36 131.4(3) . . . . ? C29 C30 C34 C36 -51.3(4) . . . . ? N1 Cr1 O1S C1S 128.0(2) . . . . ? N2 Cr1 O1S C1S -148.6(2) . . . . ? Cl1 Cr1 O1S C1S -53.4(2) . . . . ? Cl1 Cr1 O1S C1S 35.1(2) 2_655 . . . ? N1 Cr1 O1S C4S -44.2(2) . . . . ? N2 Cr1 O1S C4S 39.2(2) . . . . ? Cl1 Cr1 O1S C4S 134.31(19) . . . . ? Cl1 Cr1 O1S C4S -137.10(19) 2_655 . . . ? C4S O1S C1S C2S -11.3(3) . . . . ? Cr1 O1S C1S C2S 175.2(2) . . . . ? O1S C1S C2S C3S 25.0(4) . . . . ? C1S C2S C3S C4S -29.1(5) . . . . ? C1S O1S C4S C3S -7.0(3) . . . . ? Cr1 O1S C4S C3S 166.1(2) . . . . ? C2S C3S C4S O1S 22.4(4) . . . . ? C8S O2S C5S C6S 21.3(4) . . . . ? O2S C5S C6S C7S' 4.0(4) . . . . ? O2S C5S C6S C7S -42.5(3) . . . . ? C5S C6S C7S C8S 47.2(3) . . . . ? C7S' C6S C7S C8S -58.1(2) . . . . ? C5S C6S C7S' C8S -25.7(5) . . . . ? C7S C6S C7S' C8S 58.0(2) . . . . ? C5S O2S C8S C7S 10.0(3) . . . . ? C5S O2S C8S C7S' -38.0(4) . . . . ? C6S C7S C8S O2S -37.2(3) . . . . ? C6S C7S C8S C7S' 58.0(2) . . . . ? C6S C7S' C8S O2S 38.6(4) . . . . ? C6S C7S' C8S C7S -58.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.964 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.078 _publ_section_references ; Bruker (2003) SAINTPlus Data Reduction and Correction Program v. 6.45a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005) SMART. Bruker Molecular Analysis Research Tool, v. 5.632 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; # Attachment 'B909814C_compound_4.cif' data_crbian1m _database_code_depnum_ccdc_archive 'CCDC 732684' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H144 Cr N4 Na O8' _chemical_formula_weight 1653.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 13.4096(6) _cell_length_b 21.0138(9) _cell_length_c 32.2379(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.8320(10) _cell_angle_gamma 90.00 _cell_volume 9083.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 980 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description rhombus _exptl_crystal_colour black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3580 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9142 _exptl_absorpt_correction_T_max 0.9720 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37971 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8869 _reflns_number_gt 6206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.1026P)^2^+5.1786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens refall _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8869 _refine_ls_number_parameters 778 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1617 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _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 0.21473(2) 0.2500 0.01584(10) Uani 1 2 d S . . N1 N 0.01062(12) 0.19458(7) 0.31127(5) 0.0183(4) Uani 1 1 d . . . N2 N -0.14258(12) 0.23560(7) 0.26562(5) 0.0173(4) Uani 1 1 d . . . C1 C -0.07922(14) 0.20378(9) 0.33111(6) 0.0189(4) Uani 1 1 d . . . C2 C -0.15781(14) 0.22755(9) 0.30728(6) 0.0182(4) Uani 1 1 d . . . C3 C -0.24353(15) 0.23925(9) 0.33443(6) 0.0200(5) Uani 1 1 d . . . C4 C -0.21156(14) 0.21762(9) 0.37434(6) 0.0188(4) Uani 1 1 d . . . C5 C -0.11244(15) 0.19514(9) 0.37400(6) 0.0208(5) Uani 1 1 d . . . C6 C -0.07170(15) 0.17302(10) 0.41105(6) 0.0250(5) Uani 1 1 d D . . H6 H -0.0058(6) 0.1586(8) 0.4149(6) 0.022(5) Uiso 1 1 d D . . C7 C -0.13120(17) 0.17506(10) 0.44740(6) 0.0288(5) Uani 1 1 d D . . H7 H -0.1013(12) 0.1608(9) 0.4720(3) 0.037(6) Uiso 1 1 d D . . C8 C -0.22727(17) 0.19745(10) 0.44718(6) 0.0267(5) Uani 1 1 d . . . H8 H -0.2655(19) 0.1950(12) 0.4720(8) 0.041(7) Uiso 1 1 d . . . C9 C -0.27163(15) 0.21992(9) 0.40974(6) 0.0213(5) Uani 1 1 d . . . C10 C -0.36888(16) 0.24545(10) 0.40418(6) 0.0250(5) Uani 1 1 d . . . H10 H -0.4152(17) 0.2460(10) 0.4272(7) 0.030(6) Uiso 1 1 d . . . C11 C -0.40010(16) 0.26717(10) 0.36617(6) 0.0248(5) Uani 1 1 d . . . H11 H -0.4678(18) 0.2833(11) 0.3619(7) 0.032(6) Uiso 1 1 d . . . C12 C -0.33806(15) 0.26458(10) 0.33051(6) 0.0240(5) Uani 1 1 d . . . H12 H -0.3563(17) 0.2817(11) 0.3046(7) 0.030(6) Uiso 1 1 d . . . C13 C 0.08472(14) 0.16795(10) 0.33827(6) 0.0205(4) Uani 1 1 d . . . C14 C 0.09362(15) 0.10112(10) 0.34125(6) 0.0244(5) Uani 1 1 d . . . C15 C 0.15394(16) 0.07595(10) 0.37282(7) 0.0285(5) Uani 1 1 d . . . H15 H 0.1579(17) 0.0292(11) 0.3775(7) 0.033(6) Uiso 1 1 d . . . C16 C 0.20636(17) 0.11525(11) 0.39978(6) 0.0306(5) Uani 1 1 d D . . H16 H 0.2450(11) 0.0964(8) 0.4210(4) 0.042(7) Uiso 1 1 d D . . C17 C 0.20402(16) 0.18029(11) 0.39424(6) 0.0274(5) Uani 1 1 d . . . H17 H 0.2417(17) 0.2063(11) 0.4115(7) 0.029(6) Uiso 1 1 d . . . C18 C 0.14429(15) 0.20807(10) 0.36345(6) 0.0215(5) Uani 1 1 d . . . C19 C 0.03760(18) 0.05823(10) 0.31065(8) 0.0334(6) Uani 1 1 d . . . H19 H 0.028(2) 0.0848(14) 0.2843(9) 0.060(8) Uiso 1 1 d . . . C20 C 0.09584(19) -0.00128(12) 0.29953(8) 0.0416(7) Uani 1 1 d D . . H20A H 0.058(2) -0.0275(13) 0.2791(8) 0.051(8) Uiso 1 1 d . . . H20B H 0.102(3) -0.0260(7) 0.3240(4) 0.097(12) Uiso 1 1 d D . . H20C H 0.1591(7) 0.0107(11) 0.2902(7) 0.054(8) Uiso 1 1 d D . . C21 C -0.0661(2) 0.04153(15) 0.32349(12) 0.0729(10) Uani 1 1 d . . . H21A H -0.0971 0.0140 0.3025 0.109 Uiso 1 1 calc R . . H21B H -0.1055 0.0805 0.3263 0.109 Uiso 1 1 calc R . . H21C H -0.0635 0.0192 0.3502 0.109 Uiso 1 1 calc R . . C22 C 0.14266(16) 0.28018(10) 0.35778(6) 0.0243(5) Uani 1 1 d D . . H22 H 0.1390(17) 0.2867(10) 0.3291(2) 0.029(6) Uiso 1 1 d D . . C23 C 0.24140(18) 0.31102(11) 0.36943(7) 0.0301(5) Uani 1 1 d . . . H23A H 0.2384(19) 0.3526(12) 0.3632(8) 0.041(7) Uiso 1 1 d . . . H23B H 0.2472(19) 0.3101(11) 0.3977(8) 0.039(7) Uiso 1 1 d . . . H23C H 0.3013(17) 0.2897(10) 0.3570(7) 0.028(6) Uiso 1 1 d . . . C24 C 0.05872(17) 0.31281(10) 0.38141(7) 0.0284(5) Uani 1 1 d . . . H24A H 0.0639(16) 0.3590(10) 0.3794(6) 0.025(6) Uiso 1 1 d . . . H24B H -0.0081(18) 0.3030(10) 0.3727(7) 0.029(6) Uiso 1 1 d . . . H24C H 0.0650(17) 0.3042(11) 0.4099(7) 0.032(6) Uiso 1 1 d . . . C25 C -0.22697(14) 0.26210(9) 0.24445(6) 0.0189(4) Uani 1 1 d . . . C26 C -0.30526(15) 0.22216(9) 0.23053(5) 0.0206(5) Uani 1 1 d . . . C27 C -0.39345(16) 0.25040(10) 0.21673(6) 0.0245(5) Uani 1 1 d . . . H27 H -0.4499(17) 0.2256(11) 0.2088(7) 0.027(6) Uiso 1 1 d . . . C28 C -0.40446(15) 0.31579(10) 0.21567(6) 0.0253(5) Uani 1 1 d . . . H28 H -0.4664(17) 0.3344(11) 0.2082(7) 0.030(6) Uiso 1 1 d . . . C29 C -0.32520(16) 0.35470(9) 0.22671(6) 0.0236(5) Uani 1 1 d D . . H29 H -0.3321(15) 0.3987(3) 0.2242(6) 0.017(5) Uiso 1 1 d D . . C30 C -0.23492(15) 0.32898(9) 0.24071(6) 0.0202(5) Uani 1 1 d . . . C31 C -0.29492(15) 0.14982(10) 0.23179(6) 0.0231(5) Uani 1 1 d . . . H31 H -0.2283(17) 0.1423(10) 0.2298(6) 0.023(5) Uiso 1 1 d . . . C32 C -0.33362(19) 0.12101(10) 0.27203(7) 0.0321(6) Uani 1 1 d . . . H32A H -0.2979(19) 0.1343(11) 0.2966(8) 0.041(7) Uiso 1 1 d . . . H32B H -0.3265(17) 0.0750(11) 0.2727(7) 0.032(6) Uiso 1 1 d . . . H32C H -0.407(2) 0.1314(11) 0.2744(7) 0.037(7) Uiso 1 1 d . . . C33 C -0.34730(17) 0.11778(10) 0.19510(7) 0.0294(5) Uani 1 1 d D . . H33A H -0.3322(16) 0.0730(10) 0.1925(6) 0.025(6) Uiso 1 1 d . . . H33B H -0.4161(18) 0.1223(10) 0.1958(7) 0.026(6) Uiso 1 1 d . . . H33C H -0.3315(16) 0.1336(9) 0.1688(3) 0.038(7) Uiso 1 1 d D . . C34 C -0.14746(15) 0.37183(9) 0.25204(6) 0.0223(5) Uani 1 1 d . . . H34 H -0.0900(16) 0.3447(10) 0.2514(6) 0.022(5) Uiso 1 1 d . . . C35 C -0.15229(18) 0.39390(11) 0.29725(7) 0.0341(6) Uani 1 1 d D . . H35A H -0.0967(18) 0.4206(11) 0.3045(7) 0.034(6) Uiso 1 1 d . . . H35B H -0.2067(8) 0.4203(7) 0.3028(7) 0.041(7) Uiso 1 1 d D . . H35C H -0.1523(19) 0.3627(5) 0.3179(4) 0.036(6) Uiso 1 1 d D . . C36 C -0.13818(18) 0.42871(11) 0.22309(7) 0.0321(6) Uani 1 1 d . . . H36A H -0.0809(16) 0.4521(9) 0.2310(6) 0.017(5) Uiso 1 1 d . . . H36B H -0.196(2) 0.4625(14) 0.2254(9) 0.061(8) Uiso 1 1 d . . . H36C H -0.1347(19) 0.4189(12) 0.1927(8) 0.042(7) Uiso 1 1 d . . . Na1 Na 0.5000 0.0000 0.5000 0.0223(3) Uani 1 2 d S . . O1S O 0.56584(11) 0.00978(7) 0.43082(4) 0.0277(4) Uani 1 1 d . . . O2S O 0.36370(11) -0.06698(7) 0.47489(4) 0.0293(4) Uani 1 1 d . . . O3S O 0.40597(11) 0.09135(7) 0.48527(4) 0.0290(4) Uani 1 1 d . . . O4S O 0.10208(17) 0.02625(11) 0.52688(7) 0.0718(7) Uani 1 1 d . . . C1S C 0.50642(17) 0.01682(11) 0.39342(7) 0.0289(5) Uani 1 1 d . . . H1SA H 0.4958(17) -0.0270(11) 0.3804(7) 0.028(6) Uiso 1 1 d . . . H1SB H 0.4390(16) 0.0315(10) 0.4005(6) 0.022(5) Uiso 1 1 d . . . C2S C 0.56589(18) 0.05953(12) 0.36523(7) 0.0345(6) Uani 1 1 d . . . H2SA H 0.5572(16) 0.1022(10) 0.3709(6) 0.018(5) Uiso 1 1 d . . . H2SB H 0.557(2) 0.0474(15) 0.3359(9) 0.069(9) Uiso 1 1 d . . . C3S C 0.67304(18) 0.04332(12) 0.37736(7) 0.0327(6) Uani 1 1 d . . . H3SA H 0.6959(19) 0.0048(12) 0.3655(8) 0.040(7) Uiso 1 1 d . . . H3SB H 0.7215(17) 0.0774(10) 0.3697(6) 0.026(6) Uiso 1 1 d . . . C4S C 0.66441(17) 0.03411(11) 0.42373(7) 0.0290(5) Uani 1 1 d . . . H4SA H 0.7074(19) 0.0043(12) 0.4329(7) 0.038(7) Uiso 1 1 d . . . H4SB H 0.6682(17) 0.0745(11) 0.4375(7) 0.028(6) Uiso 1 1 d . . . C5S C 0.38721(18) -0.11623(11) 0.44528(7) 0.0317(6) Uani 1 1 d . . . H5SA H 0.4563(17) -0.1097(10) 0.4354(6) 0.025(6) Uiso 1 1 d . . . H5SB H 0.386(2) -0.1569(13) 0.4595(8) 0.049(8) Uiso 1 1 d . . . C6S C 0.30656(19) -0.11258(11) 0.41203(7) 0.0345(6) Uani 1 1 d D . . H6SA H 0.3029(19) -0.1505(5) 0.3969(5) 0.044(7) Uiso 1 1 d D . . H6SB H 0.3239(19) -0.0807(12) 0.3924(8) 0.041(7) Uiso 1 1 d . . . C7S C 0.21642(17) -0.09416(11) 0.43752(7) 0.0319(6) Uani 1 1 d D . . H7SA H 0.1917(17) -0.1292(11) 0.4492(7) 0.026(6) Uiso 1 1 d . . . H7SB H 0.1621(8) -0.0773(9) 0.4227(5) 0.051(8) Uiso 1 1 d D . . C8S C 0.26103(18) -0.04823(11) 0.46878(7) 0.0352(6) Uani 1 1 d . . . H8SA H 0.2554(19) -0.0051(12) 0.4592(8) 0.039(7) Uiso 1 1 d . . . H8SB H 0.2213(19) -0.0500(12) 0.4950(8) 0.043(7) Uiso 1 1 d . . . C9S C 0.44884(17) 0.14563(10) 0.46464(7) 0.0298(5) Uani 1 1 d . . . H9SA H 0.4236(17) 0.1440(10) 0.4348(7) 0.025(6) Uiso 1 1 d . . . H9SB H 0.5241(16) 0.1415(9) 0.4675(6) 0.021(5) Uiso 1 1 d . . . C10S C 0.41129(19) 0.20371(10) 0.48763(7) 0.0327(6) Uani 1 1 d . . . H10A H 0.4054(19) 0.2380(12) 0.4703(8) 0.041(7) Uiso 1 1 d . . . H10B H 0.4588(17) 0.2156(10) 0.5104(7) 0.026(6) Uiso 1 1 d . . . C11S C 0.31224(17) 0.18095(10) 0.50484(6) 0.0279(5) Uani 1 1 d . . . H11A H 0.2968(19) 0.2030(12) 0.5289(8) 0.038(7) Uiso 1 1 d . . . H11B H 0.2678(19) 0.1834(11) 0.4822(7) 0.037(7) Uiso 1 1 d . . . C12S C 0.33380(16) 0.11227(10) 0.51505(6) 0.0254(5) Uani 1 1 d . . . H12A H 0.2736(19) 0.0825(12) 0.5131(7) 0.038(7) Uiso 1 1 d . . . H12B H 0.3674(18) 0.1098(11) 0.5425(7) 0.033(6) Uiso 1 1 d . . . C13S C 0.0560(3) 0.08306(15) 0.51496(11) 0.0663(10) Uani 1 1 d . . . H13A H -0.0138 0.0757 0.5057 0.080 Uiso 1 1 calc R . . H13B H 0.0928 0.1042 0.4924 0.080 Uiso 1 1 calc R . . C14S C 0.0603(3) 0.12249(17) 0.55516(11) 0.0697(10) Uani 1 1 d . . . H14A H 0.1205 0.1498 0.5561 0.084 Uiso 1 1 calc R . . H14B H 0.0004 0.1497 0.5576 0.084 Uiso 1 1 calc R . . C15S C 0.0642(3) 0.07270(16) 0.58928(12) 0.0740(11) Uani 1 1 d . . . H15A H 0.0059 0.0763 0.6076 0.089 Uiso 1 1 calc R . . H15B H 0.1261 0.0766 0.6062 0.089 Uiso 1 1 calc R . . C16S C 0.0621(3) 0.00965(17) 0.56494(12) 0.0747(11) Uani 1 1 d . . . H16A H 0.1033 -0.0232 0.5790 0.090 Uiso 1 1 calc R . . H16B H -0.0069 -0.0065 0.5616 0.090 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 0.0148(2) 0.0175(2) 0.01526(19) 0.000 0.00242(16) 0.000 N1 0.0151(8) 0.0221(8) 0.0178(7) -0.0001(6) 0.0031(6) 0.0025(6) N2 0.0155(8) 0.0197(7) 0.0167(7) -0.0001(6) 0.0017(6) -0.0002(6) C1 0.0205(10) 0.0197(9) 0.0167(9) -0.0010(7) 0.0052(7) 0.0014(8) C2 0.0171(9) 0.0200(9) 0.0176(9) -0.0012(7) 0.0016(7) 0.0003(7) C3 0.0216(10) 0.0191(9) 0.0196(9) -0.0035(8) 0.0044(8) -0.0027(8) C4 0.0216(9) 0.0174(9) 0.0175(9) -0.0016(7) 0.0036(7) 0.0000(8) C5 0.0241(10) 0.0195(9) 0.0190(9) -0.0008(8) 0.0037(8) -0.0011(8) C6 0.0241(10) 0.0309(11) 0.0203(9) 0.0059(8) 0.0055(8) 0.0050(9) C7 0.0335(12) 0.0347(11) 0.0184(9) 0.0072(9) 0.0047(9) 0.0029(10) C8 0.0318(11) 0.0302(11) 0.0184(9) 0.0001(8) 0.0095(8) -0.0011(9) C9 0.0239(10) 0.0205(9) 0.0199(9) -0.0011(8) 0.0087(8) -0.0035(8) C10 0.0257(11) 0.0252(10) 0.0243(10) -0.0026(8) 0.0106(8) -0.0016(9) C11 0.0193(10) 0.0276(10) 0.0277(10) -0.0018(9) 0.0045(8) 0.0018(8) C12 0.0212(10) 0.0273(10) 0.0236(10) 0.0012(8) 0.0041(8) 0.0009(8) C13 0.0169(9) 0.0287(10) 0.0160(9) 0.0026(8) 0.0051(7) 0.0027(8) C14 0.0203(10) 0.0271(10) 0.0261(10) 0.0034(8) 0.0044(8) 0.0026(8) C15 0.0248(11) 0.0279(11) 0.0331(11) 0.0070(9) 0.0053(9) 0.0078(9) C16 0.0307(11) 0.0396(12) 0.0214(10) 0.0089(9) 0.0004(9) 0.0107(10) C17 0.0251(11) 0.0397(12) 0.0174(9) -0.0007(9) -0.0009(8) 0.0035(9) C18 0.0199(10) 0.0290(10) 0.0158(9) -0.0002(8) 0.0049(7) 0.0060(8) C19 0.0303(12) 0.0224(10) 0.0474(13) -0.0001(10) -0.0057(10) 0.0052(9) C20 0.0398(14) 0.0377(13) 0.0475(14) -0.0080(12) 0.0065(12) 0.0022(11) C21 0.0382(16) 0.0591(17) 0.122(3) -0.0492(17) 0.0234(16) -0.0103(14) C22 0.0269(10) 0.0309(11) 0.0152(9) -0.0009(8) 0.0022(8) 0.0007(9) C23 0.0331(12) 0.0353(12) 0.0221(10) -0.0026(9) 0.0032(9) -0.0012(10) C24 0.0328(12) 0.0261(10) 0.0264(11) -0.0051(9) 0.0027(9) 0.0038(9) C25 0.0161(9) 0.0248(9) 0.0161(9) -0.0005(8) 0.0053(7) 0.0006(8) C26 0.0210(10) 0.0284(10) 0.0126(8) -0.0005(8) 0.0049(7) -0.0002(8) C27 0.0200(10) 0.0321(11) 0.0214(10) -0.0006(8) 0.0019(8) -0.0026(9) C28 0.0165(10) 0.0375(11) 0.0218(10) 0.0044(9) 0.0014(8) 0.0057(9) C29 0.0247(10) 0.0243(10) 0.0220(10) 0.0017(8) 0.0025(8) 0.0075(8) C30 0.0201(10) 0.0246(10) 0.0158(9) 0.0004(8) 0.0017(7) 0.0000(8) C31 0.0179(10) 0.0252(10) 0.0262(10) -0.0016(8) 0.0037(8) -0.0022(8) C32 0.0451(14) 0.0243(11) 0.0270(11) 0.0016(9) 0.0052(10) -0.0069(10) C33 0.0311(12) 0.0278(11) 0.0293(11) -0.0066(9) 0.0019(9) -0.0040(9) C34 0.0201(10) 0.0202(9) 0.0267(10) -0.0013(8) -0.0007(8) 0.0022(8) C35 0.0372(13) 0.0356(12) 0.0293(11) -0.0055(10) -0.0017(10) -0.0072(10) C36 0.0353(12) 0.0283(11) 0.0324(11) 0.0049(9) -0.0053(10) -0.0109(10) Na1 0.0250(6) 0.0220(5) 0.0200(5) 0.0011(4) 0.0041(4) 0.0015(5) O1S 0.0276(8) 0.0340(8) 0.0216(7) 0.0054(6) 0.0044(6) -0.0005(6) O2S 0.0281(8) 0.0324(8) 0.0274(7) -0.0082(6) 0.0027(6) 0.0015(6) O3S 0.0320(8) 0.0226(7) 0.0328(8) 0.0015(6) 0.0109(6) 0.0047(6) O4S 0.0612(14) 0.0821(15) 0.0724(14) 0.0152(12) 0.0092(12) 0.0115(12) C1S 0.0286(11) 0.0322(11) 0.0258(10) -0.0015(9) 0.0000(9) 0.0004(9) C2S 0.0382(13) 0.0423(13) 0.0231(10) 0.0071(10) 0.0032(10) 0.0023(11) C3S 0.0317(12) 0.0411(13) 0.0256(11) 0.0027(10) 0.0079(9) 0.0003(10) C4S 0.0283(11) 0.0307(11) 0.0278(11) 0.0048(9) 0.0001(9) -0.0009(9) C5S 0.0343(12) 0.0261(11) 0.0350(12) -0.0080(9) 0.0096(10) -0.0002(9) C6S 0.0442(13) 0.0325(12) 0.0271(11) -0.0061(10) 0.0064(10) -0.0130(10) C7S 0.0293(12) 0.0335(12) 0.0328(11) -0.0008(10) 0.0017(10) -0.0041(10) C8S 0.0281(12) 0.0365(12) 0.0409(13) -0.0103(11) 0.0000(10) 0.0073(10) C9S 0.0311(12) 0.0288(11) 0.0296(11) 0.0061(9) 0.0062(9) 0.0047(9) C10S 0.0414(13) 0.0253(11) 0.0313(11) 0.0052(9) 0.0015(10) 0.0058(10) C11S 0.0356(12) 0.0257(11) 0.0224(10) 0.0020(8) 0.0045(9) 0.0091(9) C12S 0.0278(11) 0.0260(10) 0.0225(10) 0.0015(8) 0.0034(9) 0.0056(9) C13S 0.0531(18) 0.0631(19) 0.083(2) 0.0172(17) 0.0071(17) 0.0065(16) C14S 0.061(2) 0.069(2) 0.079(2) -0.0013(18) 0.0012(18) 0.0006(17) C15S 0.076(2) 0.064(2) 0.082(2) 0.0015(19) -0.0036(19) -0.0037(18) C16S 0.061(2) 0.073(2) 0.091(2) 0.0244(19) 0.0203(18) 0.0047(17) _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 2.0230(15) . ? Cr1 N1 2.0230(15) 2 ? Cr1 N2 2.0319(16) 2 ? Cr1 N2 2.0320(16) . ? N1 C1 1.386(2) . ? N1 C13 1.426(2) . ? N2 C2 1.372(2) . ? N2 C25 1.426(2) . ? C1 C2 1.388(3) . ? C1 C5 1.470(3) . ? C2 C3 1.475(3) . ? C3 C12 1.379(3) . ? C3 C4 1.425(3) . ? C4 C9 1.407(3) . ? C4 C5 1.411(3) . ? C5 C6 1.386(3) . ? C6 C7 1.428(3) . ? C7 C8 1.371(3) . ? C8 C9 1.418(3) . ? C9 C10 1.419(3) . ? C10 C11 1.368(3) . ? C11 C12 1.430(3) . ? C13 C18 1.410(3) . ? C13 C14 1.413(3) . ? C14 C15 1.395(3) . ? C14 C19 1.526(3) . ? C15 C16 1.383(3) . ? C16 C17 1.379(3) . ? C17 C18 1.394(3) . ? C18 C22 1.526(3) . ? C19 C21 1.498(4) . ? C19 C20 1.520(3) . ? C22 C23 1.516(3) . ? C22 C24 1.531(3) . ? C25 C26 1.412(3) . ? C25 C30 1.414(3) . ? C26 C27 1.390(3) . ? C26 C31 1.527(3) . ? C27 C28 1.382(3) . ? C28 C29 1.383(3) . ? C29 C30 1.395(3) . ? C30 C34 1.519(3) . ? C31 C33 1.524(3) . ? C31 C32 1.529(3) . ? C34 C36 1.523(3) . ? C34 C35 1.532(3) . ? Na1 O3S 2.3416(14) . ? Na1 O3S 2.3416(14) 5_656 ? Na1 O1S 2.4193(14) . ? Na1 O1S 2.4194(14) 5_656 ? Na1 O2S 2.4359(15) 5_656 ? Na1 O2S 2.4360(15) . ? O1S C4S 1.439(3) . ? O1S C1S 1.443(3) . ? O2S C8S 1.443(3) . ? O2S C5S 1.446(3) . ? O3S C12S 1.442(3) . ? O3S C9S 1.444(3) . ? O4S C16S 1.390(4) . ? O4S C13S 1.396(4) . ? C1S C2S 1.513(3) . ? C2S C3S 1.522(3) . ? C3S C4S 1.513(3) . ? C5S C6S 1.514(3) . ? C6S C7S 1.522(3) . ? C7S C8S 1.513(3) . ? C9S C10S 1.518(3) . ? C10S C11S 1.524(3) . ? C11S C12S 1.507(3) . ? C13S C14S 1.539(5) . ? C14S C15S 1.518(5) . ? C15S C16S 1.540(5) . ? 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 155.83(9) . 2 ? N1 Cr1 N2 103.53(6) . 2 ? N1 Cr1 N2 81.75(6) 2 2 ? N1 Cr1 N2 81.74(6) . . ? N1 Cr1 N2 103.53(6) 2 . ? N2 Cr1 N2 155.08(9) 2 . ? C1 N1 C13 112.07(15) . . ? C1 N1 Cr1 111.84(12) . . ? C13 N1 Cr1 135.79(12) . . ? C2 N2 C25 112.84(15) . . ? C2 N2 Cr1 111.72(12) . . ? C25 N2 Cr1 135.12(12) . . ? N1 C1 C2 116.94(16) . . ? N1 C1 C5 133.97(17) . . ? C2 C1 C5 109.08(17) . . ? N2 C2 C1 117.61(17) . . ? N2 C2 C3 133.51(17) . . ? C1 C2 C3 108.88(16) . . ? C12 C3 C4 118.04(18) . . ? C12 C3 C2 137.14(18) . . ? C4 C3 C2 104.81(16) . . ? C9 C4 C5 124.62(17) . . ? C9 C4 C3 123.59(18) . . ? C5 C4 C3 111.78(17) . . ? C6 C5 C4 117.72(18) . . ? C6 C5 C1 136.94(19) . . ? C4 C5 C1 105.32(16) . . ? C5 C6 C7 118.63(19) . . ? C8 C7 C6 122.81(19) . . ? C7 C8 C9 120.07(18) . . ? C4 C9 C8 116.15(18) . . ? C4 C9 C10 116.50(17) . . ? C8 C9 C10 127.34(18) . . ? C11 C10 C9 120.54(19) . . ? C10 C11 C12 122.24(19) . . ? C3 C12 C11 119.07(18) . . ? C18 C13 C14 120.56(18) . . ? C18 C13 N1 120.05(17) . . ? C14 C13 N1 119.29(17) . . ? C15 C14 C13 118.31(19) . . ? C15 C14 C19 121.50(19) . . ? C13 C14 C19 120.19(18) . . ? C16 C15 C14 121.1(2) . . ? C17 C16 C15 120.01(19) . . ? C16 C17 C18 121.3(2) . . ? C17 C18 C13 118.31(19) . . ? C17 C18 C22 120.53(18) . . ? C13 C18 C22 121.16(17) . . ? C21 C19 C20 110.8(2) . . ? C21 C19 C14 114.2(2) . . ? C20 C19 C14 112.86(19) . . ? C23 C22 C18 112.57(17) . . ? C23 C22 C24 109.33(17) . . ? C18 C22 C24 113.24(17) . . ? C26 C25 C30 120.58(17) . . ? C26 C25 N2 120.06(17) . . ? C30 C25 N2 119.15(17) . . ? C27 C26 C25 118.22(18) . . ? C27 C26 C31 120.65(18) . . ? C25 C26 C31 121.10(17) . . ? C28 C27 C26 121.48(19) . . ? C27 C28 C29 119.98(19) . . ? C28 C29 C30 120.94(18) . . ? C29 C30 C25 118.46(18) . . ? C29 C30 C34 120.76(17) . . ? C25 C30 C34 120.77(17) . . ? C33 C31 C26 112.25(17) . . ? C33 C31 C32 108.99(17) . . ? C26 C31 C32 112.65(17) . . ? C30 C34 C36 112.81(17) . . ? C30 C34 C35 111.41(17) . . ? C36 C34 C35 110.52(17) . . ? O3S Na1 O3S 180.00(6) . 5_656 ? O3S Na1 O1S 86.91(5) . . ? O3S Na1 O1S 93.10(5) 5_656 . ? O3S Na1 O1S 93.09(5) . 5_656 ? O3S Na1 O1S 86.90(5) 5_656 5_656 ? O1S Na1 O1S 180.0 . 5_656 ? O3S Na1 O2S 89.59(5) . 5_656 ? O3S Na1 O2S 90.41(5) 5_656 5_656 ? O1S Na1 O2S 88.58(5) . 5_656 ? O1S Na1 O2S 91.43(5) 5_656 5_656 ? O3S Na1 O2S 90.41(5) . . ? O3S Na1 O2S 89.59(5) 5_656 . ? O1S Na1 O2S 91.42(5) . . ? O1S Na1 O2S 88.57(5) 5_656 . ? O2S Na1 O2S 180.0 5_656 . ? C4S O1S C1S 109.16(15) . . ? C4S O1S Na1 121.68(12) . . ? C1S O1S Na1 125.06(12) . . ? C8S O2S C5S 108.79(16) . . ? C8S O2S Na1 126.69(13) . . ? C5S O2S Na1 117.59(12) . . ? C12S O3S C9S 109.96(15) . . ? C12S O3S Na1 118.66(11) . . ? C9S O3S Na1 121.62(12) . . ? C16S O4S C13S 106.4(3) . . ? O1S C1S C2S 105.86(18) . . ? C1S C2S C3S 102.52(18) . . ? C4S C3S C2S 101.36(18) . . ? O1S C4S C3S 106.62(17) . . ? O2S C5S C6S 105.71(18) . . ? C5S C6S C7S 101.28(18) . . ? C8S C7S C6S 102.27(18) . . ? O2S C8S C7S 106.50(18) . . ? O3S C9S C10S 105.86(17) . . ? C9S C10S C11S 102.85(18) . . ? C12S C11S C10S 102.39(18) . . ? O3S C12S C11S 105.96(16) . . ? O4S C13S C14S 102.6(3) . . ? C15S C14S C13S 103.9(3) . . ? C14S C15S C16S 102.9(3) . . ? O4S C16S C15S 103.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cr1 N1 C1 -103.86(12) 2 . . . ? N2 Cr1 N1 C1 156.03(12) 2 . . . ? N2 Cr1 N1 C1 0.86(12) . . . . ? N1 Cr1 N1 C13 69.18(18) 2 . . . ? N2 Cr1 N1 C13 -30.93(19) 2 . . . ? N2 Cr1 N1 C13 173.89(19) . . . . ? N1 Cr1 N2 C2 1.46(13) . . . . ? N1 Cr1 N2 C2 157.43(12) 2 . . . ? N2 Cr1 N2 C2 -102.93(12) 2 . . . ? N1 Cr1 N2 C25 174.22(18) . . . . ? N1 Cr1 N2 C25 -29.81(18) 2 . . . ? N2 Cr1 N2 C25 69.83(17) 2 . . . ? C13 N1 C1 C2 -177.89(17) . . . . ? Cr1 N1 C1 C2 -3.1(2) . . . . ? C13 N1 C1 C5 3.7(3) . . . . ? Cr1 N1 C1 C5 178.50(18) . . . . ? C25 N2 C2 C1 -178.13(16) . . . . ? Cr1 N2 C2 C1 -3.7(2) . . . . ? C25 N2 C2 C3 1.6(3) . . . . ? Cr1 N2 C2 C3 176.01(18) . . . . ? N1 C1 C2 N2 4.6(3) . . . . ? C5 C1 C2 N2 -176.60(16) . . . . ? N1 C1 C2 C3 -175.12(16) . . . . ? C5 C1 C2 C3 3.6(2) . . . . ? N2 C2 C3 C12 -3.7(4) . . . . ? C1 C2 C3 C12 176.0(2) . . . . ? N2 C2 C3 C4 177.1(2) . . . . ? C1 C2 C3 C4 -3.2(2) . . . . ? C12 C3 C4 C9 0.9(3) . . . . ? C2 C3 C4 C9 -179.76(18) . . . . ? C12 C3 C4 C5 -177.85(18) . . . . ? C2 C3 C4 C5 1.5(2) . . . . ? C9 C4 C5 C6 0.8(3) . . . . ? C3 C4 C5 C6 179.57(18) . . . . ? C9 C4 C5 C1 -178.12(18) . . . . ? C3 C4 C5 C1 0.6(2) . . . . ? N1 C1 C5 C6 -2.8(4) . . . . ? C2 C1 C5 C6 178.7(2) . . . . ? N1 C1 C5 C4 175.8(2) . . . . ? C2 C1 C5 C4 -2.7(2) . . . . ? C4 C5 C6 C7 -0.9(3) . . . . ? C1 C5 C6 C7 177.6(2) . . . . ? C5 C6 C7 C8 0.6(3) . . . . ? C6 C7 C8 C9 0.0(3) . . . . ? C5 C4 C9 C8 -0.3(3) . . . . ? C3 C4 C9 C8 -178.86(18) . . . . ? C5 C4 C9 C10 178.62(18) . . . . ? C3 C4 C9 C10 0.0(3) . . . . ? C7 C8 C9 C4 -0.1(3) . . . . ? C7 C8 C9 C10 -178.9(2) . . . . ? C4 C9 C10 C11 -0.9(3) . . . . ? C8 C9 C10 C11 177.8(2) . . . . ? C9 C10 C11 C12 0.9(3) . . . . ? C4 C3 C12 C11 -0.9(3) . . . . ? C2 C3 C12 C11 180.0(2) . . . . ? C10 C11 C12 C3 0.1(3) . . . . ? C1 N1 C13 C18 -86.5(2) . . . . ? Cr1 N1 C13 C18 100.4(2) . . . . ? C1 N1 C13 C14 89.8(2) . . . . ? Cr1 N1 C13 C14 -83.3(2) . . . . ? C18 C13 C14 C15 7.3(3) . . . . ? N1 C13 C14 C15 -169.02(18) . . . . ? C18 C13 C14 C19 -173.13(19) . . . . ? N1 C13 C14 C19 10.6(3) . . . . ? C13 C14 C15 C16 -2.0(3) . . . . ? C19 C14 C15 C16 178.4(2) . . . . ? C14 C15 C16 C17 -3.7(3) . . . . ? C15 C16 C17 C18 4.3(3) . . . . ? C16 C17 C18 C13 0.9(3) . . . . ? C16 C17 C18 C22 180.00(19) . . . . ? C14 C13 C18 C17 -6.7(3) . . . . ? N1 C13 C18 C17 169.53(18) . . . . ? C14 C13 C18 C22 174.19(18) . . . . ? N1 C13 C18 C22 -9.6(3) . . . . ? C15 C14 C19 C21 91.9(3) . . . . ? C13 C14 C19 C21 -87.7(3) . . . . ? C15 C14 C19 C20 -35.8(3) . . . . ? C13 C14 C19 C20 144.7(2) . . . . ? C17 C18 C22 C23 30.9(3) . . . . ? C13 C18 C22 C23 -150.04(18) . . . . ? C17 C18 C22 C24 -93.8(2) . . . . ? C13 C18 C22 C24 85.3(2) . . . . ? C2 N2 C25 C26 -84.4(2) . . . . ? Cr1 N2 C25 C26 102.9(2) . . . . ? C2 N2 C25 C30 90.3(2) . . . . ? Cr1 N2 C25 C30 -82.4(2) . . . . ? C30 C25 C26 C27 -5.9(3) . . . . ? N2 C25 C26 C27 168.82(17) . . . . ? C30 C25 C26 C31 175.99(17) . . . . ? N2 C25 C26 C31 -9.3(3) . . . . ? C25 C26 C27 C28 1.4(3) . . . . ? C31 C26 C27 C28 179.50(18) . . . . ? C26 C27 C28 C29 3.0(3) . . . . ? C27 C28 C29 C30 -2.8(3) . . . . ? C28 C29 C30 C25 -1.7(3) . . . . ? C28 C29 C30 C34 178.85(18) . . . . ? C26 C25 C30 C29 6.1(3) . . . . ? N2 C25 C30 C29 -168.70(17) . . . . ? C26 C25 C30 C34 -174.48(17) . . . . ? N2 C25 C30 C34 10.8(3) . . . . ? C27 C26 C31 C33 37.3(3) . . . . ? C25 C26 C31 C33 -144.59(18) . . . . ? C27 C26 C31 C32 -86.1(2) . . . . ? C25 C26 C31 C32 91.9(2) . . . . ? C29 C30 C34 C36 -38.2(3) . . . . ? C25 C30 C34 C36 142.35(19) . . . . ? C29 C30 C34 C35 86.8(2) . . . . ? C25 C30 C34 C35 -92.7(2) . . . . ? O3S Na1 O1S C4S 103.48(14) . . . . ? O3S Na1 O1S C4S -76.52(14) 5_656 . . . ? O1S Na1 O1S C4S -117(11) 5_656 . . . ? O2S Na1 O1S C4S 13.81(14) 5_656 . . . ? O2S Na1 O1S C4S -166.19(14) . . . . ? O3S Na1 O1S C1S -51.24(15) . . . . ? O3S Na1 O1S C1S 128.76(15) 5_656 . . . ? O1S Na1 O1S C1S 89(11) 5_656 . . . ? O2S Na1 O1S C1S -140.91(15) 5_656 . . . ? O2S Na1 O1S C1S 39.09(15) . . . . ? O3S Na1 O2S C8S -17.26(16) . . . . ? O3S Na1 O2S C8S 162.74(16) 5_656 . . . ? O1S Na1 O2S C8S -104.17(16) . . . . ? O1S Na1 O2S C8S 75.83(16) 5_656 . . . ? O2S Na1 O2S C8S 154(14) 5_656 . . . ? O3S Na1 O2S C5S 130.16(14) . . . . ? O3S Na1 O2S C5S -49.84(14) 5_656 . . . ? O1S Na1 O2S C5S 43.25(14) . . . . ? O1S Na1 O2S C5S -136.75(14) 5_656 . . . ? O2S Na1 O2S C5S -59(14) 5_656 . . . ? O3S Na1 O3S C12S -21(8) 5_656 . . . ? O1S Na1 O3S C12S 173.96(14) . . . . ? O1S Na1 O3S C12S -6.04(14) 5_656 . . . ? O2S Na1 O3S C12S -97.44(14) 5_656 . . . ? O2S Na1 O3S C12S 82.56(14) . . . . ? O3S Na1 O3S C9S 122(8) 5_656 . . . ? O1S Na1 O3S C9S -43.54(14) . . . . ? O1S Na1 O3S C9S 136.46(14) 5_656 . . . ? O2S Na1 O3S C9S 45.06(14) 5_656 . . . ? O2S Na1 O3S C9S -134.95(14) . . . . ? C4S O1S C1S C2S -11.7(2) . . . . ? Na1 O1S C1S C2S 145.62(14) . . . . ? O1S C1S C2S C3S 31.1(2) . . . . ? C1S C2S C3S C4S -37.4(2) . . . . ? C1S O1S C4S C3S -12.7(2) . . . . ? Na1 O1S C4S C3S -170.98(13) . . . . ? C2S C3S C4S O1S 31.4(2) . . . . ? C8S O2S C5S C6S 17.7(2) . . . . ? Na1 O2S C5S C6S -135.21(14) . . . . ? O2S C5S C6S C7S -34.9(2) . . . . ? C5S C6S C7S C8S 38.2(2) . . . . ? C5S O2S C8S C7S 7.3(2) . . . . ? Na1 O2S C8S C7S 157.05(13) . . . . ? C6S C7S C8S O2S -28.9(2) . . . . ? C12S O3S C9S C10S 8.4(2) . . . . ? Na1 O3S C9S C10S -136.94(14) . . . . ? O3S C9S C10S C11S -27.6(2) . . . . ? C9S C10S C11S C12S 35.5(2) . . . . ? C9S O3S C12S C11S 14.6(2) . . . . ? Na1 O3S C12S C11S 161.14(13) . . . . ? C10S C11S C12S O3S -31.3(2) . . . . ? C16S O4S C13S C14S 45.2(3) . . . . ? O4S C13S C14S C15S -26.1(3) . . . . ? C13S C14S C15S C16S 0.2(4) . . . . ? C13S O4S C16S C15S -45.4(3) . . . . ? C14S C15S C16S O4S 25.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.038 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.080 _publ_section_references ; Bruker (2003) SAINTPlus Data Reduction and Correction Program v. 6.45a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005) SMART. Bruker Molecular Analysis Research Tool, v. 5.632 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ;