# 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 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Christopher Kozak' _publ_contact_author_email CKOZAK@MUN.CA _publ_section_title ; Structure and magnetic behavior of mono- and bimetallic chromium(III) complexes of amine-bis(phenolate) ligands ; loop_ _publ_author_name 'Christopher Kozak' 'Julie L. Collins' 'Loiuse N. Dawe' 'Rebecca K. Dean' 'Andreas Decken' 'Stephanie L. Granville' ; K.M.Hattenhauer ; # Attachment 'CIFs.txt' data_cmpd_1 _database_code_depnum_ccdc_archive 'CCDC 733954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C29 H42 O3 N1)2 Li4 [C6 H6]0.75' _chemical_formula_sum 'C62.50 H88.50 Li4 N2 O6' _chemical_formula_weight 991.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.599(4) _cell_length_b 14.427(7) _cell_length_c 20.499(9) _cell_angle_alpha 106.425(13) _cell_angle_beta 93.594(7) _cell_angle_gamma 91.928(8) _cell_volume 2997(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13434 _cell_measurement_theta_min 2.3632 _cell_measurement_theta_max 30.9848 _exptl_crystal_description Chunk _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1075 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9911 _exptl_absorpt_correction_T_min 0.9812 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 24396 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 26.50 _reflns_number_total 12170 _reflns_number_gt 10331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1562P)^2^+2.0616P] 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 12170 _refine_ls_number_parameters 731 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.2800 _refine_ls_wR_factor_gt 0.2678 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.002 _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 O1 O 0.02467(18) 1.00396(13) 0.22945(9) 0.0400(4) Uani 1 1 d . . . O2 O 0.2389(3) 1.19115(15) 0.29981(12) 0.0655(7) Uani 1 1 d . . . O3 O 0.24899(16) 0.93252(12) 0.28080(9) 0.0339(4) Uani 1 1 d . . . O4 O 0.24103(16) 0.71350(13) 0.32873(9) 0.0361(4) Uani 1 1 d . . . O5 O 0.04593(19) 0.51950(13) 0.23902(11) 0.0451(5) Uani 1 1 d . . . O6 O 0.09525(16) 0.75661(12) 0.21584(8) 0.0321(4) Uani 1 1 d . . . N1 N 0.1181(2) 1.09076(16) 0.37543(12) 0.0399(5) Uani 1 1 d . . . N2 N -0.04310(19) 0.68805(15) 0.31751(11) 0.0337(5) Uani 1 1 d . . . C1 C -0.0651(2) 1.06703(18) 0.24533(14) 0.0375(6) Uani 1 1 d . . . C2 C -0.1372(3) 1.09715(19) 0.19493(16) 0.0426(6) Uani 1 1 d . . . C3 C -0.1128(3) 1.0577(2) 0.11930(16) 0.0490(7) Uani 1 1 d . . . C4 C 0.0252(3) 1.0822(3) 0.10841(18) 0.0610(9) Uani 1 1 d . . . H1 H 0.0308 1.1448 0.0985 0.073 Uiso 1 1 calc R . . H2 H 0.0538 1.0318 0.0700 0.073 Uiso 1 1 calc R . . H3 H 0.0791 1.0856 0.1498 0.073 Uiso 1 1 calc R . . C5 C -0.1395(3) 0.9472(2) 0.09526(15) 0.0506(7) Uani 1 1 d . . . H4 H -0.1041 0.9187 0.1300 0.061 Uiso 1 1 calc R . . H5 H -0.1003 0.9202 0.0524 0.061 Uiso 1 1 calc R . . H6 H -0.2311 0.9325 0.0881 0.061 Uiso 1 1 calc R . . C6 C -0.1990(4) 1.0999(3) 0.0735(2) 0.0663(9) Uani 1 1 d . . . H7 H -0.1553 1.1027 0.0333 0.080 Uiso 1 1 calc R . . H8 H -0.2200 1.1652 0.0989 0.080 Uiso 1 1 calc R . . H9 H -0.2770 1.0587 0.0590 0.080 Uiso 1 1 calc R . . C7 C -0.2327(3) 1.1601(2) 0.21626(18) 0.0498(7) Uani 1 1 d . . . H10 H -0.2813 1.1800 0.1826 0.060 Uiso 1 1 calc R . . C8 C -0.2616(3) 1.1957(2) 0.28361(19) 0.0526(8) Uani 1 1 d . . . C9 C -0.3744(4) 1.2568(3) 0.3035(2) 0.0714(11) Uani 1 1 d . . . H11 H -0.4500 1.2145 0.3005 0.086 Uiso 1 1 calc R . . H12 H -0.3878 1.2969 0.2725 0.086 Uiso 1 1 calc R . . H13 H -0.3581 1.2986 0.3504 0.086 Uiso 1 1 calc R . . C10 C -0.1864(3) 1.1687(2) 0.33255(17) 0.0472(7) Uani 1 1 d . . . H14 H -0.2009 1.1944 0.3793 0.057 Uiso 1 1 calc R . . C11 C -0.0907(3) 1.10491(19) 0.31469(15) 0.0411(6) Uani 1 1 d . . . C12 C -0.0212(3) 1.0692(2) 0.36801(14) 0.0419(6) Uani 1 1 d . . . H15 H -0.0560 1.0986 0.4125 0.050 Uiso 1 1 calc R . . H16 H -0.0376 0.9983 0.3567 0.050 Uiso 1 1 calc R . . C13 C 0.1531(3) 1.1940(2) 0.40546(16) 0.0488(7) Uani 1 1 d . . . H17 H 0.0759 1.2362 0.3995 0.059 Uiso 1 1 d . . . H18 H 0.1557 1.2112 0.4525 0.059 Uiso 1 1 d . . . C14 C 0.2696(5) 1.2308(4) 0.3758(3) 0.0511(12) Uani 0.60 1 d P . . C15 C 0.2641(8) 1.3410(3) 0.3873(3) 0.116(2) Uani 1 1 d . . . C16A C 0.2744(17) 1.3549(9) 0.3077(8) 0.101(4) Uani 0.40 1 d P . . C17 C 0.2411(7) 1.2613(4) 0.2642(3) 0.116(2) Uani 1 1 d . . . C18 C 0.1866(3) 1.0302(2) 0.41148(14) 0.0429(6) Uani 1 1 d . . . H19 H 0.1440 0.9648 0.3990 0.052 Uiso 1 1 calc R . . H20 H 0.1840 1.0588 0.4613 0.052 Uiso 1 1 calc R . . C19 C 0.3230(2) 1.02193(19) 0.39378(13) 0.0378(6) Uani 1 1 d . . . C20 C 0.4223(3) 1.0638(2) 0.44243(14) 0.0435(6) Uani 1 1 d . . . H21 H 0.4037 1.0957 0.4878 0.052 Uiso 1 1 calc R . . C21 C 0.5479(3) 1.0598(2) 0.42595(15) 0.0437(6) Uani 1 1 d . . . C22 C 0.6556(3) 1.1082(3) 0.47767(16) 0.0540(8) Uani 1 1 d . . . H22 H 0.6690 1.1756 0.4774 0.065 Uiso 1 1 calc R . . H23 H 0.7330 1.0739 0.4659 0.065 Uiso 1 1 calc R . . H24 H 0.6345 1.1064 0.5232 0.065 Uiso 1 1 calc R . . C23 C 0.5705(3) 1.0105(2) 0.35933(15) 0.0412(6) Uani 1 1 d . . . H25 H 0.6558 1.0064 0.3475 0.049 Uiso 1 1 calc R . . C24 C 0.4752(2) 0.96664(17) 0.30865(13) 0.0348(5) Uani 1 1 d . . . C25 C 0.5078(2) 0.91594(18) 0.23568(14) 0.0369(5) Uani 1 1 d . . . C26 C 0.6517(3) 0.9130(2) 0.23035(17) 0.0474(7) Uani 1 1 d . . . H26 H 0.6858 0.8680 0.2540 0.057 Uiso 1 1 calc R . . H27 H 0.6913 0.9779 0.2514 0.057 Uiso 1 1 calc R . . H28 H 0.6697 0.8914 0.1822 0.057 Uiso 1 1 calc R . . C27 C 0.4545(3) 0.81025(19) 0.21177(15) 0.0411(6) Uani 1 1 d . . . H32 H 0.4971 0.7747 0.1719 0.049 Uiso 1 1 calc R . . H33 H 0.3634 0.8087 0.1996 0.049 Uiso 1 1 calc R . . H34 H 0.4691 0.7801 0.2486 0.049 Uiso 1 1 calc R . . C28 C 0.4545(3) 0.9706(2) 0.18718(15) 0.0442(6) Uani 1 1 d . . . H29 H 0.5030 1.0324 0.1955 0.053 Uiso 1 1 calc R . . H30 H 0.3656 0.9828 0.1950 0.053 Uiso 1 1 calc R . . H31 H 0.4609 0.9318 0.1399 0.053 Uiso 1 1 calc R . . C29 C 0.3482(2) 0.97271(17) 0.32652(13) 0.0342(5) Uani 1 1 d . . . C30 C 0.2287(2) 0.68031(17) 0.38218(12) 0.0316(5) Uani 1 1 d . . . C31 C 0.3265(2) 0.63293(17) 0.40818(12) 0.0323(5) Uani 1 1 d . . . C32 C 0.4568(2) 0.6236(2) 0.37783(14) 0.0391(6) Uani 1 1 d . . . C33 C 0.5196(3) 0.7251(2) 0.38775(19) 0.0535(8) Uani 1 1 d . . . H35 H 0.4957 0.7477 0.3481 0.064 Uiso 1 1 calc R . . H36 H 0.6118 0.7220 0.3925 0.064 Uiso 1 1 calc R . . H37 H 0.4912 0.7701 0.4290 0.064 Uiso 1 1 calc R . . C34 C 0.5487(3) 0.5695(3) 0.41282(19) 0.0567(8) Uani 1 1 d . . . H38 H 0.5962 0.6157 0.4517 0.068 Uiso 1 1 calc R . . H39 H 0.6076 0.5360 0.3802 0.068 Uiso 1 1 calc R . . H40 H 0.5008 0.5220 0.4289 0.068 Uiso 1 1 calc R . . C35 C 0.4432(3) 0.5685(3) 0.30171(16) 0.0565(8) Uani 1 1 d . . . H41 H 0.5109 0.5911 0.2786 0.068 Uiso 1 1 calc R . . H42 H 0.3608 0.5800 0.2818 0.068 Uiso 1 1 calc R . . H43 H 0.4492 0.4991 0.2961 0.068 Uiso 1 1 calc R . . C36 C 0.3022(2) 0.59747(18) 0.46277(13) 0.0352(5) Uani 1 1 d . . . H44 H 0.3676 0.5659 0.4804 0.042 Uiso 1 1 calc R . . C37 C 0.1880(3) 0.60545(18) 0.49318(12) 0.0362(5) Uani 1 1 d . . . C38 C 0.1641(3) 0.5638(2) 0.55106(14) 0.0459(6) Uani 1 1 d . . . H45 H 0.2132 0.5063 0.5468 0.055 Uiso 1 1 calc R . . H46 H 0.0738 0.5457 0.5495 0.055 Uiso 1 1 calc R . . H47 H 0.1898 0.6121 0.5945 0.055 Uiso 1 1 calc R . . C39 C 0.0942(2) 0.65294(18) 0.46759(12) 0.0347(5) Uani 1 1 d . . . H48 H 0.0154 0.6601 0.4877 0.042 Uiso 1 1 calc R . . C40 C 0.1123(2) 0.69034(18) 0.41337(12) 0.0333(5) Uani 1 1 d . . . C41 C 0.0085(2) 0.74134(19) 0.38734(13) 0.0365(5) Uani 1 1 d . . . H49 H -0.0607 0.7498 0.4185 0.044 Uiso 1 1 calc R . . H50 H 0.0414 0.8065 0.3875 0.044 Uiso 1 1 calc R . . C42 C -0.1095(3) 0.5963(2) 0.31423(14) 0.0413(6) Uani 1 1 d . . . H51 H -0.1354 0.6028 0.3631 0.049 Uiso 1 1 d . . . H52 H -0.1818 0.5866 0.2911 0.049 Uiso 1 1 d . . . C43A C -0.0964(7) 0.5147(5) 0.2424(4) 0.0454(16) Uani 0.40 1 d P . . C44 C -0.1139(4) 0.4153(3) 0.2617(3) 0.0803(13) Uani 1 1 d . . . C45A C -0.0490(15) 0.3583(8) 0.1903(6) 0.085(4) Uani 0.40 1 d P . . C46A C 0.0752(15) 0.4214(8) 0.1963(12) 0.140(8) Uani 0.40 1 d P . . C47 C -0.1207(2) 0.74887(19) 0.28545(13) 0.0371(6) Uani 1 1 d . . . H53 H -0.0847 0.8164 0.3007 0.045 Uiso 1 1 calc R . . H54 H -0.2078 0.7487 0.3003 0.045 Uiso 1 1 calc R . . C48 C -0.1253(2) 0.71243(17) 0.20870(13) 0.0347(5) Uani 1 1 d . . . C49 C -0.2371(3) 0.6730(2) 0.17041(15) 0.0424(6) Uani 1 1 d . . . H55 H -0.3117 0.6698 0.1932 0.051 Uiso 1 1 calc R . . C50 C -0.2428(3) 0.6384(2) 0.10048(16) 0.0471(7) Uani 1 1 d . . . C51 C -0.3654(3) 0.5970(3) 0.05888(19) 0.0666(10) Uani 1 1 d . . . H56 H -0.3736 0.5272 0.0530 0.080 Uiso 1 1 calc R . . H57 H -0.3650 0.6087 0.0141 0.080 Uiso 1 1 calc R . . H58 H -0.4369 0.6282 0.0827 0.080 Uiso 1 1 calc R . . C52 C -0.1300(3) 0.6433(2) 0.06909(14) 0.0441(6) Uani 1 1 d . . . H59 H -0.1325 0.6192 0.0208 0.053 Uiso 1 1 calc R . . C53 C -0.0138(3) 0.68154(18) 0.10449(13) 0.0367(5) Uani 1 1 d . . . C54 C 0.1072(3) 0.6827(2) 0.06738(13) 0.0408(6) Uani 1 1 d . . . C55 C 0.0815(3) 0.6409(3) -0.01031(15) 0.0572(8) Uani 1 1 d . . . H60 H 0.0284 0.5809 -0.0204 0.069 Uiso 1 1 calc R . . H61 H 0.1619 0.6273 -0.0313 0.069 Uiso 1 1 calc R . . H62 H 0.0377 0.6879 -0.0287 0.069 Uiso 1 1 calc R . . C56 C 0.1629(3) 0.7870(2) 0.08009(15) 0.0458(6) Uani 1 1 d . . . H63 H 0.0958 0.8283 0.0719 0.055 Uiso 1 1 calc R . . H64 H 0.2295 0.7873 0.0491 0.055 Uiso 1 1 calc R . . H65 H 0.1988 0.8115 0.1274 0.055 Uiso 1 1 calc R . . C57 C 0.2060(3) 0.6212(2) 0.09043(15) 0.0452(6) Uani 1 1 d . . . H66 H 0.1793 0.5526 0.0719 0.054 Uiso 1 1 calc R . . H67 H 0.2141 0.6385 0.1404 0.054 Uiso 1 1 calc R . . H68 H 0.2879 0.6333 0.0738 0.054 Uiso 1 1 calc R . . C58 C -0.0121(2) 0.71764(16) 0.17657(12) 0.0317(5) Uani 1 1 d . . . C59 C 0.3656(8) 0.3776(5) 0.1299(3) 0.0935(19) Uani 0.75 1 d P . . H69 H 0.3229 0.4310 0.1558 0.112 Uiso 0.75 1 calc PR . . C60 C 0.4922(9) 0.3829(7) 0.1287(4) 0.107(3) Uani 0.75 1 d P . . H70 H 0.5397 0.4398 0.1547 0.128 Uiso 0.75 1 calc PR . . C61 C 0.5530(7) 0.3064(8) 0.0900(5) 0.110(3) Uani 0.75 1 d P . . H71 H 0.6423 0.3115 0.0887 0.131 Uiso 0.75 1 calc PR . . C62 C 0.4904(11) 0.2268(8) 0.0550(5) 0.137(4) Uani 0.75 1 d P . . H72 H 0.5325 0.1757 0.0261 0.164 Uiso 0.75 1 calc PR . . C63 C 0.3611(11) 0.2180(7) 0.0607(5) 0.138(3) Uani 0.75 1 d P . . H73 H 0.3160 0.1574 0.0411 0.166 Uiso 0.75 1 calc PR . . C64 C 0.3000(7) 0.2954(7) 0.0940(4) 0.102(2) Uani 0.75 1 d P . . H74 H 0.2101 0.2923 0.0921 0.123 Uiso 0.75 1 calc PR . . C14A C 0.1494(7) 1.2469(5) 0.3546(4) 0.0498(18) Uani 0.40 1 d P . . C16 C 0.1976(8) 1.3514(5) 0.3354(7) 0.092(3) Uani 0.60 1 d P . . C43 C -0.0273(4) 0.5134(3) 0.2988(2) 0.0373(9) Uani 0.60 1 d P . . C45 C -0.1227(9) 0.4094(6) 0.1955(4) 0.080(2) Uani 0.60 1 d P . . C46 C 0.0004(7) 0.4555(5) 0.1807(3) 0.0583(15) Uani 0.60 1 d P . . Li1 Li 0.1774(4) 1.0566(3) 0.2797(2) 0.0398(9) Uani 1 1 d . . . Li2 Li 0.0946(5) 0.8917(3) 0.2263(3) 0.0451(10) Uani 1 1 d . . . Li3 Li 0.2346(4) 0.8035(3) 0.2843(2) 0.0406(10) Uani 1 1 d . . . Li4 Li 0.1097(4) 0.6541(3) 0.2622(2) 0.0355(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0449(10) 0.0334(9) 0.0412(10) 0.0092(8) 0.0032(8) 0.0071(8) O2 0.108(2) 0.0329(11) 0.0565(13) 0.0137(10) 0.0167(13) -0.0064(11) O3 0.0323(9) 0.0294(8) 0.0385(9) 0.0079(7) 0.0009(7) -0.0013(7) O4 0.0335(9) 0.0424(10) 0.0378(9) 0.0200(8) 0.0043(7) 0.0017(7) O5 0.0492(11) 0.0297(9) 0.0576(12) 0.0124(9) 0.0126(9) 0.0030(8) O6 0.0351(9) 0.0288(8) 0.0325(8) 0.0100(7) -0.0002(7) -0.0026(7) N1 0.0390(12) 0.0347(11) 0.0421(12) 0.0041(9) 0.0064(9) 0.0008(9) N2 0.0322(10) 0.0329(10) 0.0401(11) 0.0163(9) 0.0039(8) 0.0052(8) C1 0.0373(13) 0.0276(12) 0.0476(15) 0.0109(11) 0.0029(11) 0.0011(10) C2 0.0413(14) 0.0316(13) 0.0567(16) 0.0167(12) 0.0004(12) -0.0030(10) C3 0.0518(17) 0.0464(16) 0.0532(17) 0.0236(14) -0.0029(13) -0.0032(13) C4 0.060(2) 0.072(2) 0.0566(19) 0.0289(17) 0.0052(15) -0.0086(17) C5 0.0605(18) 0.0490(17) 0.0417(15) 0.0135(13) -0.0011(13) -0.0015(14) C6 0.075(2) 0.065(2) 0.068(2) 0.0356(18) -0.0087(18) 0.0049(18) C7 0.0434(15) 0.0330(14) 0.073(2) 0.0173(14) -0.0059(14) 0.0001(11) C8 0.0415(15) 0.0312(14) 0.082(2) 0.0114(14) 0.0023(15) 0.0018(11) C9 0.056(2) 0.0470(18) 0.102(3) 0.0059(19) 0.0018(19) 0.0150(16) C10 0.0411(14) 0.0335(14) 0.0612(18) 0.0037(13) 0.0073(13) -0.0018(11) C11 0.0381(13) 0.0320(13) 0.0508(15) 0.0082(11) 0.0047(11) -0.0022(10) C12 0.0384(14) 0.0423(14) 0.0424(14) 0.0068(12) 0.0091(11) -0.0003(11) C13 0.0472(16) 0.0401(15) 0.0485(16) -0.0048(12) 0.0055(13) 0.0035(12) C14 0.049(3) 0.039(2) 0.060(3) 0.007(2) 0.001(2) -0.002(2) C15 0.202(7) 0.037(2) 0.099(4) 0.013(2) -0.020(4) -0.036(3) C16A 0.117(12) 0.064(7) 0.125(12) 0.039(7) -0.016(9) -0.021(7) C17 0.166(6) 0.061(3) 0.130(5) 0.046(3) -0.008(4) -0.012(3) C18 0.0446(15) 0.0485(16) 0.0358(13) 0.0119(12) 0.0066(11) 0.0006(12) C19 0.0376(13) 0.0374(13) 0.0380(13) 0.0111(11) 0.0015(10) -0.0027(10) C20 0.0453(15) 0.0458(15) 0.0362(13) 0.0081(12) 0.0009(11) -0.0054(12) C21 0.0410(14) 0.0448(15) 0.0448(15) 0.0140(12) -0.0013(11) -0.0061(11) C22 0.0457(16) 0.064(2) 0.0476(16) 0.0119(15) -0.0050(13) -0.0123(14) C23 0.0360(13) 0.0379(14) 0.0497(15) 0.0135(12) 0.0022(11) -0.0039(11) C24 0.0342(12) 0.0275(11) 0.0431(13) 0.0112(10) 0.0020(10) -0.0021(9) C25 0.0359(13) 0.0308(12) 0.0428(14) 0.0085(11) 0.0062(10) -0.0022(10) C26 0.0385(14) 0.0407(15) 0.0592(17) 0.0063(13) 0.0130(13) -0.0002(11) C27 0.0431(14) 0.0324(13) 0.0460(15) 0.0078(11) 0.0075(11) 0.0002(11) C28 0.0501(16) 0.0375(14) 0.0469(15) 0.0142(12) 0.0094(12) 0.0018(12) C29 0.0366(13) 0.0267(11) 0.0391(13) 0.0099(10) -0.0001(10) -0.0021(9) C30 0.0340(12) 0.0298(12) 0.0323(12) 0.0115(10) 0.0017(9) -0.0010(9) C31 0.0311(12) 0.0300(12) 0.0343(12) 0.0081(10) -0.0025(9) -0.0020(9) C32 0.0314(12) 0.0426(14) 0.0452(14) 0.0154(12) 0.0027(10) 0.0021(10) C33 0.0384(15) 0.0535(18) 0.071(2) 0.0216(16) 0.0108(14) -0.0082(13) C34 0.0351(14) 0.074(2) 0.069(2) 0.0335(18) 0.0048(14) 0.0111(14) C35 0.0466(17) 0.070(2) 0.0516(18) 0.0118(16) 0.0124(14) 0.0147(15) C36 0.0362(13) 0.0333(12) 0.0372(13) 0.0125(10) -0.0008(10) 0.0004(10) C37 0.0436(14) 0.0343(13) 0.0318(12) 0.0118(10) 0.0002(10) 0.0003(10) C38 0.0500(16) 0.0536(17) 0.0396(14) 0.0230(13) 0.0021(12) -0.0027(13) C39 0.0381(13) 0.0339(12) 0.0325(12) 0.0095(10) 0.0054(10) 0.0009(10) C40 0.0354(12) 0.0318(12) 0.0335(12) 0.0102(10) 0.0041(10) 0.0032(9) C41 0.0404(13) 0.0350(13) 0.0354(12) 0.0104(10) 0.0079(10) 0.0088(10) C42 0.0354(13) 0.0454(15) 0.0470(15) 0.0203(12) 0.0037(11) -0.0041(11) C43A 0.043(4) 0.031(3) 0.062(4) 0.016(3) 0.002(3) -0.004(3) C44 0.094(3) 0.0379(17) 0.113(4) 0.025(2) 0.033(3) -0.0120(18) C45A 0.135(11) 0.043(5) 0.070(6) 0.000(5) 0.034(7) -0.014(6) C46A 0.093(10) 0.035(5) 0.27(2) -0.008(8) 0.089(12) 0.004(6) C47 0.0349(12) 0.0388(13) 0.0409(13) 0.0152(11) 0.0053(10) 0.0109(10) C48 0.0381(13) 0.0280(12) 0.0388(13) 0.0100(10) 0.0033(10) 0.0063(10) C49 0.0364(13) 0.0371(14) 0.0512(16) 0.0083(12) 0.0030(11) 0.0051(11) C50 0.0393(14) 0.0412(15) 0.0532(17) 0.0027(13) -0.0032(12) 0.0033(12) C51 0.0453(17) 0.075(2) 0.063(2) -0.0036(18) -0.0087(15) -0.0062(16) C52 0.0467(15) 0.0384(14) 0.0396(14) 0.0000(11) -0.0024(12) 0.0022(12) C53 0.0441(14) 0.0268(11) 0.0378(13) 0.0070(10) 0.0019(11) 0.0016(10) C54 0.0480(15) 0.0399(14) 0.0319(13) 0.0060(11) 0.0032(11) 0.0000(11) C55 0.0593(19) 0.070(2) 0.0347(15) 0.0034(14) 0.0040(13) -0.0014(16) C56 0.0525(16) 0.0432(15) 0.0425(15) 0.0138(12) 0.0061(12) -0.0032(12) C57 0.0471(15) 0.0380(14) 0.0469(15) 0.0049(12) 0.0094(12) 0.0029(12) C58 0.0366(12) 0.0220(11) 0.0370(12) 0.0101(9) -0.0006(10) 0.0014(9) C59 0.121(6) 0.092(5) 0.066(4) 0.016(3) 0.019(4) 0.014(4) C60 0.123(6) 0.123(6) 0.071(4) 0.035(4) -0.036(4) -0.036(5) C61 0.057(4) 0.161(8) 0.114(6) 0.049(6) -0.016(4) 0.006(4) C62 0.128(8) 0.153(9) 0.112(6) 0.011(6) -0.023(6) 0.072(7) C63 0.135(8) 0.121(7) 0.118(7) -0.019(6) -0.033(6) -0.019(6) C64 0.082(4) 0.140(7) 0.081(4) 0.025(5) 0.007(3) 0.002(4) C14A 0.045(4) 0.024(3) 0.073(5) 0.003(3) 0.005(3) 0.002(3) C16 0.071(5) 0.038(3) 0.155(9) 0.007(4) 0.025(5) -0.004(3) C43 0.049(2) 0.031(2) 0.034(2) 0.0127(17) 0.0024(18) -0.0032(17) C45 0.098(6) 0.063(4) 0.067(4) 0.004(4) -0.002(4) -0.042(4) C46 0.072(4) 0.054(3) 0.034(2) -0.010(2) 0.018(2) -0.024(3) Li1 0.045(2) 0.032(2) 0.043(2) 0.0112(18) 0.0057(19) 0.0003(18) Li2 0.049(3) 0.035(2) 0.052(3) 0.012(2) 0.001(2) 0.0030(19) Li3 0.045(2) 0.036(2) 0.045(2) 0.0194(19) -0.0015(19) -0.0042(18) Li4 0.037(2) 0.031(2) 0.041(2) 0.0125(17) 0.0069(17) 0.0044(16) _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 O1 C1 1.330(3) . ? O1 Li2 1.790(5) . ? O1 Li1 1.877(5) . ? O2 C17 1.406(5) . ? O2 C14 1.511(6) . ? O2 C14A 1.575(8) . ? O2 Li1 1.948(5) . ? O3 C29 1.360(3) . ? O3 Li3 1.884(5) . ? O3 Li2 1.899(5) . ? O3 Li1 1.973(5) . ? O4 C30 1.326(3) . ? O4 Li3 1.786(5) . ? O4 Li4 1.885(5) . ? O5 C46 1.338(5) . ? O5 C46A 1.493(11) . ? O5 C43 1.512(5) . ? O5 C43A 1.515(7) . ? O5 Li4 1.950(5) . ? O6 C58 1.358(3) . ? O6 Li2 1.900(5) . ? O6 Li3 1.935(5) . ? O6 Li4 1.976(4) . ? N1 C13 1.467(4) . ? N1 C18 1.476(4) . ? N1 C12 1.488(3) . ? N1 Li1 2.029(5) . ? N2 C42 1.461(3) . ? N2 C47 1.478(3) . ? N2 C41 1.480(3) . ? N2 Li4 2.030(5) . ? C1 C11 1.419(4) . ? C1 C2 1.420(4) . ? C1 Li1 2.643(5) . ? C2 C7 1.391(4) . ? C2 C3 1.535(4) . ? C3 C6 1.529(4) . ? C3 C4 1.539(5) . ? C3 C5 1.539(4) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.388(5) . ? C7 H10 0.9500 . ? C8 C10 1.392(5) . ? C8 C9 1.516(4) . ? C9 H11 0.9800 . ? C9 H12 0.9800 . ? C9 H13 0.9800 . ? C10 C11 1.388(4) . ? C10 H14 0.9500 . ? C11 C12 1.499(4) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 C14A 1.455(9) . ? C13 C14 1.551(6) . ? C13 H17 1.0570 . ? C13 H18 0.9243 . ? C13 H17 1.0570 . ? C14 C14A 1.369(9) . ? C14 C15 1.544(7) . ? C15 C16 1.287(12) . ? C15 C16A 1.708(17) . ? C15 C14A 1.744(9) . ? C16A C16 1.028(17) . ? C16A C17 1.411(14) . ? C17 C16 1.755(12) . ? C18 C19 1.513(4) . ? C18 H19 0.9900 . ? C18 H20 0.9900 . ? C19 C20 1.397(4) . ? C19 C29 1.408(4) . ? C20 C21 1.393(4) . ? C20 H21 0.9500 . ? C21 C23 1.390(4) . ? C21 C22 1.513(4) . ? C22 H22 0.9800 . ? C22 H23 0.9800 . ? C22 H24 0.9800 . ? C23 C24 1.398(4) . ? C23 H25 0.9500 . ? C24 C29 1.416(4) . ? C24 C25 1.535(4) . ? C25 C28 1.527(4) . ? C25 C26 1.537(4) . ? C25 C27 1.539(4) . ? C26 H26 0.9800 . ? C26 H27 0.9800 . ? C26 H28 0.9800 . ? C27 H32 0.9800 . ? C27 H33 0.9800 . ? C27 H34 0.9800 . ? C28 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C29 Li1 2.500(5) . ? C29 Li3 2.576(5) . ? C30 C31 1.418(3) . ? C30 C40 1.418(3) . ? C30 Li4 2.615(5) . ? C31 C36 1.390(3) . ? C31 C32 1.545(3) . ? C32 C35 1.533(4) . ? C32 C34 1.534(4) . ? C32 C33 1.541(4) . ? C33 H35 0.9800 . ? C33 H36 0.9800 . ? C33 H37 0.9800 . ? C34 H38 0.9800 . ? C34 H39 0.9800 . ? C34 H40 0.9800 . ? C35 H41 0.9800 . ? C35 H42 0.9800 . ? C35 H43 0.9800 . ? C36 C37 1.389(4) . ? C36 H44 0.9500 . ? C37 C39 1.385(4) . ? C37 C38 1.505(3) . ? C38 H45 0.9800 . ? C38 H46 0.9800 . ? C38 H47 0.9800 . ? C39 C40 1.386(3) . ? C39 H48 0.9500 . ? C40 C41 1.497(3) . ? C41 H49 0.9900 . ? C41 H50 0.9900 . ? C42 C43 1.476(5) . ? C42 C43A 1.622(8) . ? C42 H51 1.0347 . ? C42 H52 0.8610 . ? C43A C43 1.334(9) . ? C43A C45 1.555(10) . ? C43A C44 1.599(8) . ? C43A C46 1.730(10) . ? C43A H52 1.5759 . ? C44 C45 1.332(9) . ? C44 C43 1.624(6) . ? C44 C45A 1.666(12) . ? C45A C45 1.083(15) . ? C45A C46 1.549(12) . ? C45A C46A 1.553(18) . ? C46A C46 1.029(19) . ? C47 C48 1.508(4) . ? C47 H53 0.9900 . ? C47 H54 0.9900 . ? C48 C49 1.389(4) . ? C48 C58 1.414(4) . ? C49 C50 1.375(4) . ? C49 H55 0.9500 . ? C50 C52 1.402(4) . ? C50 C51 1.514(4) . ? C51 H56 0.9800 . ? C51 H57 0.9800 . ? C51 H58 0.9800 . ? C52 C53 1.401(4) . ? C52 H59 0.9500 . ? C53 C58 1.420(4) . ? C53 C54 1.534(4) . ? C54 C57 1.531(4) . ? C54 C55 1.538(4) . ? C54 C56 1.542(4) . ? C55 H60 0.9800 . ? C55 H61 0.9800 . ? C55 H62 0.9800 . ? C56 H63 0.9800 . ? C56 H64 0.9800 . ? C56 H65 0.9800 . ? C57 H66 0.9800 . ? C57 H67 0.9800 . ? C57 H68 0.9800 . ? C58 Li4 2.509(5) . ? C58 Li2 2.616(5) . ? C59 C60 1.344(11) . ? C59 C64 1.348(11) . ? C59 H69 0.9500 . ? C60 C61 1.371(12) . ? C60 H70 0.9500 . ? C61 C62 1.302(13) . ? C61 H71 0.9500 . ? C62 C63 1.387(14) . ? C62 H72 0.9500 . ? C63 C64 1.344(12) . ? C63 H73 0.9500 . ? C64 H74 0.9500 . ? C14A C16 1.731(12) . ? C14A Li1 2.777(8) . ? C14A H17 1.2814 . ? C14A H17 1.2814 . ? C43 Li4 2.755(6) . ? C45 C46 1.530(9) . ? Li1 Li2 2.428(7) . ? Li2 Li3 2.449(6) . ? Li3 Li4 2.406(6) . ? 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 C1 O1 Li2 153.3(2) . . ? C1 O1 Li1 109.8(2) . . ? Li2 O1 Li1 82.9(2) . . ? C17 O2 C14 114.4(4) . . ? C17 O2 C14A 95.1(4) . . ? C14 O2 C14A 52.6(4) . . ? C17 O2 Li1 135.9(3) . . ? C14 O2 Li1 108.6(3) . . ? C14A O2 Li1 103.5(3) . . ? C29 O3 Li3 104.0(2) . . ? C29 O3 Li2 170.6(2) . . ? Li3 O3 Li2 80.7(2) . . ? C29 O3 Li1 95.45(19) . . ? Li3 O3 Li1 152.6(2) . . ? Li2 O3 Li1 77.6(2) . . ? C30 O4 Li3 154.4(2) . . ? C30 O4 Li4 107.78(19) . . ? Li3 O4 Li4 81.8(2) . . ? C46 O5 C46A 42.2(9) . . ? C46 O5 C43 112.2(3) . . ? C46A O5 C43 111.3(7) . . ? C46 O5 C43A 74.4(4) . . ? C46A O5 C43A 104.7(6) . . ? C43 O5 C43A 52.3(3) . . ? C46 O5 Li4 133.3(3) . . ? C46A O5 Li4 140.4(5) . . ? C43 O5 Li4 104.8(2) . . ? C43A O5 Li4 110.0(3) . . ? C58 O6 Li2 105.6(2) . . ? C58 O6 Li3 169.6(2) . . ? Li2 O6 Li3 79.4(2) . . ? C58 O6 Li4 95.80(18) . . ? Li2 O6 Li4 146.4(2) . . ? Li3 O6 Li4 75.89(19) . . ? C13 N1 C18 111.9(2) . . ? C13 N1 C12 112.9(2) . . ? C18 N1 C12 112.7(2) . . ? C13 N1 Li1 105.6(2) . . ? C18 N1 Li1 106.6(2) . . ? C12 N1 Li1 106.6(2) . . ? C42 N2 C47 112.2(2) . . ? C42 N2 C41 112.9(2) . . ? C47 N2 C41 112.20(19) . . ? C42 N2 Li4 106.3(2) . . ? C47 N2 Li4 107.06(19) . . ? C41 N2 Li4 105.6(2) . . ? O1 C1 C11 119.1(2) . . ? O1 C1 C2 122.1(2) . . ? C11 C1 C2 118.8(2) . . ? O1 C1 Li1 41.93(15) . . ? C11 C1 Li1 91.41(19) . . ? C2 C1 Li1 136.6(2) . . ? C7 C2 C1 117.8(3) . . ? C7 C2 C3 121.7(3) . . ? C1 C2 C3 120.5(2) . . ? C6 C3 C2 112.3(3) . . ? C6 C3 C4 107.9(3) . . ? C2 C3 C4 110.1(3) . . ? C6 C3 C5 106.7(3) . . ? C2 C3 C5 110.1(2) . . ? C4 C3 C5 109.6(3) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C8 C7 C2 124.2(3) . . ? C8 C7 H10 117.9 . . ? C2 C7 H10 117.9 . . ? C7 C8 C10 117.1(3) . . ? C7 C8 C9 122.1(3) . . ? C10 C8 C9 120.7(3) . . ? C8 C9 H11 109.5 . . ? C8 C9 H12 109.5 . . ? H11 C9 H12 109.5 . . ? C8 C9 H13 109.5 . . ? H11 C9 H13 109.5 . . ? H12 C9 H13 109.5 . . ? C11 C10 C8 121.6(3) . . ? C11 C10 H14 119.2 . . ? C8 C10 H14 119.2 . . ? C10 C11 C1 120.4(3) . . ? C10 C11 C12 120.0(3) . . ? C1 C11 C12 119.4(2) . . ? N1 C12 C11 114.7(2) . . ? N1 C12 H15 108.6 . . ? C11 C12 H15 108.6 . . ? N1 C12 H16 108.6 . . ? C11 C12 H16 108.6 . . ? H15 C12 H16 107.6 . . ? C14A C13 N1 112.2(4) . . ? C14A C13 C14 54.0(4) . . ? N1 C13 C14 114.3(3) . . ? C14A C13 H17 58.8 . . ? N1 C13 H17 110.4 . . ? C14 C13 H17 108.6 . . ? C14A C13 H18 134.9 . . ? N1 C13 H18 111.4 . . ? C14 C13 H18 115.1 . . ? H17 C13 H18 95.3 . . ? C14A C13 H17 58.8 . . ? N1 C13 H17 110.4 . . ? C14 C13 H17 108.6 . . ? H17 C13 H17 0.0 . . ? H18 C13 H17 95.3 . . ? C14A C14 O2 66.1(4) . . ? C14A C14 C15 73.3(5) . . ? O2 C14 C15 102.4(4) . . ? C14A C14 C13 59.4(4) . . ? O2 C14 C13 102.7(3) . . ? C15 C14 C13 109.1(4) . . ? C16 C15 C14 105.8(5) . . ? C16 C15 C16A 36.9(6) . . ? C14 C15 C16A 104.0(6) . . ? C16 C15 C14A 67.7(6) . . ? C14 C15 C14A 48.7(3) . . ? C16A C15 C14A 90.1(6) . . ? C16 C16A C17 90.6(11) . . ? C16 C16A C15 48.7(10) . . ? C17 C16A C15 103.2(8) . . ? O2 C17 C16A 112.2(7) . . ? O2 C17 C16 91.9(5) . . ? C16A C17 C16 35.9(7) . . ? N1 C18 C19 111.4(2) . . ? N1 C18 H19 109.3 . . ? C19 C18 H19 109.3 . . ? N1 C18 H20 109.3 . . ? C19 C18 H20 109.3 . . ? H19 C18 H20 108.0 . . ? C20 C19 C29 120.3(2) . . ? C20 C19 C18 121.1(2) . . ? C29 C19 C18 118.6(2) . . ? C21 C20 C19 121.5(3) . . ? C21 C20 H21 119.2 . . ? C19 C20 H21 119.2 . . ? C23 C21 C20 117.1(3) . . ? C23 C21 C22 121.0(3) . . ? C20 C21 C22 121.8(3) . . ? C21 C22 H22 109.5 . . ? C21 C22 H23 109.5 . . ? H22 C22 H23 109.5 . . ? C21 C22 H24 109.5 . . ? H22 C22 H24 109.5 . . ? H23 C22 H24 109.5 . . ? C21 C23 C24 123.9(3) . . ? C21 C23 H25 118.1 . . ? C24 C23 H25 118.1 . . ? C23 C24 C29 117.9(2) . . ? C23 C24 C25 120.7(2) . . ? C29 C24 C25 121.4(2) . . ? C28 C25 C24 109.7(2) . . ? C28 C25 C26 107.9(2) . . ? C24 C25 C26 111.5(2) . . ? C28 C25 C27 109.5(2) . . ? C24 C25 C27 111.6(2) . . ? C26 C25 C27 106.6(2) . . ? C25 C26 H26 109.5 . . ? C25 C26 H27 109.5 . . ? H26 C26 H27 109.5 . . ? C25 C26 H28 109.5 . . ? H26 C26 H28 109.5 . . ? H27 C26 H28 109.5 . . ? C25 C27 H32 109.5 . . ? C25 C27 H33 109.5 . . ? H32 C27 H33 109.5 . . ? C25 C27 H34 109.5 . . ? H32 C27 H34 109.5 . . ? H33 C27 H34 109.5 . . ? C25 C28 H29 109.5 . . ? C25 C28 H30 109.5 . . ? H29 C28 H30 109.5 . . ? C25 C28 H31 109.5 . . ? H29 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? O3 C29 C19 118.5(2) . . ? O3 C29 C24 122.2(2) . . ? C19 C29 C24 119.3(2) . . ? O3 C29 Li1 51.78(15) . . ? C19 C29 Li1 91.05(19) . . ? C24 C29 Li1 126.6(2) . . ? O3 C29 Li3 45.23(14) . . ? C19 C29 Li3 112.4(2) . . ? C24 C29 Li3 109.40(19) . . ? Li1 C29 Li3 95.16(17) . . ? O4 C30 C31 122.4(2) . . ? O4 C30 C40 118.8(2) . . ? C31 C30 C40 118.8(2) . . ? O4 C30 Li4 43.35(14) . . ? C31 C30 Li4 134.35(19) . . ? C40 C30 Li4 90.80(18) . . ? C36 C31 C30 117.9(2) . . ? C36 C31 C32 121.3(2) . . ? C30 C31 C32 120.8(2) . . ? C35 C32 C34 107.2(2) . . ? C35 C32 C33 109.6(3) . . ? C34 C32 C33 106.6(2) . . ? C35 C32 C31 110.9(2) . . ? C34 C32 C31 112.6(2) . . ? C33 C32 C31 109.8(2) . . ? C32 C33 H35 109.5 . . ? C32 C33 H36 109.5 . . ? H35 C33 H36 109.5 . . ? C32 C33 H37 109.5 . . ? H35 C33 H37 109.5 . . ? H36 C33 H37 109.5 . . ? C32 C34 H38 109.5 . . ? C32 C34 H39 109.5 . . ? H38 C34 H39 109.5 . . ? C32 C34 H40 109.5 . . ? H38 C34 H40 109.5 . . ? H39 C34 H40 109.5 . . ? C32 C35 H41 109.5 . . ? C32 C35 H42 109.5 . . ? H41 C35 H42 109.5 . . ? C32 C35 H43 109.5 . . ? H41 C35 H43 109.5 . . ? H42 C35 H43 109.5 . . ? C37 C36 C31 124.0(2) . . ? C37 C36 H44 118.0 . . ? C31 C36 H44 118.0 . . ? C39 C37 C36 117.3(2) . . ? C39 C37 C38 120.3(2) . . ? C36 C37 C38 122.4(2) . . ? C37 C38 H45 109.5 . . ? C37 C38 H46 109.5 . . ? H45 C38 H46 109.5 . . ? C37 C38 H47 109.5 . . ? H45 C38 H47 109.5 . . ? H46 C38 H47 109.5 . . ? C37 C39 C40 121.7(2) . . ? C37 C39 H48 119.2 . . ? C40 C39 H48 119.2 . . ? C39 C40 C30 120.4(2) . . ? C39 C40 C41 120.0(2) . . ? C30 C40 C41 119.7(2) . . ? N2 C41 C40 112.5(2) . . ? N2 C41 H49 109.1 . . ? C40 C41 H49 109.1 . . ? N2 C41 H50 109.1 . . ? C40 C41 H50 109.1 . . ? H49 C41 H50 107.8 . . ? N2 C42 C43 113.2(3) . . ? N2 C42 C43A 112.3(3) . . ? C43 C42 C43A 50.7(3) . . ? N2 C42 H51 105.8 . . ? C43 C42 H51 105.0 . . ? C43A C42 H51 140.6 . . ? N2 C42 H52 114.2 . . ? C43 C42 H52 115.1 . . ? C43A C42 H52 71.4 . . ? H51 C42 H52 102.0 . . ? C43 C43A O5 63.8(4) . . ? C43 C43A C45 109.6(6) . . ? O5 C43A C45 97.4(5) . . ? C43 C43A C44 66.6(4) . . ? O5 C43A C44 99.7(4) . . ? C45 C43A C44 49.9(4) . . ? C43 C43A C42 59.0(4) . . ? O5 C43A C42 100.2(4) . . ? C45 C43A C42 150.3(6) . . ? C44 C43A C42 103.2(5) . . ? C43 C43A C46 100.4(5) . . ? O5 C43A C46 48.1(3) . . ? C45 C43A C46 55.2(4) . . ? C44 C43A C46 87.5(4) . . ? C42 C43A C46 148.2(5) . . ? C43 C43A H52 86.4 . . ? O5 C43A H52 129.2 . . ? C45 C43A H52 132.2 . . ? C44 C43A H52 104.7 . . ? C42 C43A H52 31.2 . . ? C46 C43A H52 167.7 . . ? C45 C44 C43A 63.3(5) . . ? C45 C44 C43 105.8(4) . . ? C43A C44 C43 48.9(3) . . ? C45 C44 C45A 40.4(6) . . ? C43A C44 C45A 89.3(5) . . ? C43 C44 C45A 108.1(5) . . ? C45 C45A C46 68.4(8) . . ? C45 C45A C46A 104.0(10) . . ? C46 C45A C46A 38.7(7) . . ? C45 C45A C44 53.0(7) . . ? C46 C45A C44 91.5(6) . . ? C46A C45A C44 101.4(9) . . ? C46 C46A O5 60.8(6) . . ? C46 C46A C45A 70.5(11) . . ? O5 C46A C45A 104.8(9) . . ? N2 C47 C48 111.3(2) . . ? N2 C47 H53 109.4 . . ? C48 C47 H53 109.4 . . ? N2 C47 H54 109.4 . . ? C48 C47 H54 109.4 . . ? H53 C47 H54 108.0 . . ? C49 C48 C58 120.6(2) . . ? C49 C48 C47 121.1(2) . . ? C58 C48 C47 118.3(2) . . ? C50 C49 C48 121.9(3) . . ? C50 C49 H55 119.0 . . ? C48 C49 H55 119.0 . . ? C49 C50 C52 117.1(3) . . ? C49 C50 C51 121.7(3) . . ? C52 C50 C51 121.2(3) . . ? C50 C51 H56 109.5 . . ? C50 C51 H57 109.5 . . ? H56 C51 H57 109.5 . . ? C50 C51 H58 109.5 . . ? H56 C51 H58 109.5 . . ? H57 C51 H58 109.5 . . ? C53 C52 C50 124.1(3) . . ? C53 C52 H59 118.0 . . ? C50 C52 H59 118.0 . . ? C52 C53 C58 117.1(2) . . ? C52 C53 C54 121.7(2) . . ? C58 C53 C54 121.2(2) . . ? C57 C54 C53 110.6(2) . . ? C57 C54 C55 107.2(2) . . ? C53 C54 C55 111.7(2) . . ? C57 C54 C56 109.8(2) . . ? C53 C54 C56 111.0(2) . . ? C55 C54 C56 106.5(2) . . ? C54 C55 H60 109.5 . . ? C54 C55 H61 109.5 . . ? H60 C55 H61 109.5 . . ? C54 C55 H62 109.5 . . ? H60 C55 H62 109.5 . . ? H61 C55 H62 109.5 . . ? C54 C56 H63 109.5 . . ? C54 C56 H64 109.5 . . ? H63 C56 H64 109.5 . . ? C54 C56 H65 109.5 . . ? H63 C56 H65 109.5 . . ? H64 C56 H65 109.5 . . ? C54 C57 H66 109.5 . . ? C54 C57 H67 109.5 . . ? H66 C57 H67 109.5 . . ? C54 C57 H68 109.5 . . ? H66 C57 H68 109.5 . . ? H67 C57 H68 109.5 . . ? O6 C58 C48 118.8(2) . . ? O6 C58 C53 122.0(2) . . ? C48 C58 C53 119.2(2) . . ? O6 C58 Li4 51.60(14) . . ? C48 C58 Li4 91.16(18) . . ? C53 C58 Li4 126.52(19) . . ? O6 C58 Li2 44.41(14) . . ? C48 C58 Li2 108.70(19) . . ? C53 C58 Li2 113.95(19) . . ? Li4 C58 Li2 92.77(17) . . ? C60 C59 C64 119.2(7) . . ? C60 C59 H69 120.4 . . ? C64 C59 H69 120.4 . . ? C59 C60 C61 120.1(7) . . ? C59 C60 H70 120.0 . . ? C61 C60 H70 120.0 . . ? C62 C61 C60 121.2(8) . . ? C62 C61 H71 119.4 . . ? C60 C61 H71 119.4 . . ? C61 C62 C63 118.8(8) . . ? C61 C62 H72 120.6 . . ? C63 C62 H72 120.6 . . ? C64 C63 C62 119.8(9) . . ? C64 C63 H73 120.1 . . ? C62 C63 H73 120.1 . . ? C63 C64 C59 120.3(8) . . ? C63 C64 H74 119.9 . . ? C59 C64 H74 119.9 . . ? C14 C14A C13 66.5(5) . . ? C14 C14A O2 61.3(4) . . ? C13 C14A O2 104.1(4) . . ? C14 C14A C16 93.1(6) . . ? C13 C14A C16 146.1(7) . . ? O2 C14A C16 87.3(5) . . ? C14 C14A C15 58.0(4) . . ? C13 C14A C15 103.6(5) . . ? O2 C14A C15 91.5(5) . . ? C16 C14A C15 43.5(4) . . ? C14 C14A Li1 77.6(4) . . ? C13 C14A Li1 76.0(3) . . ? O2 C14A Li1 43.0(2) . . ? C16 C14A Li1 127.8(5) . . ? C15 C14A Li1 129.5(4) . . ? C14 C14A H17 107.5 . . ? C13 C14A H17 44.9 . . ? O2 C14A H17 143.1 . . ? C16 C14A H17 129.5 . . ? C15 C14A H17 112.6 . . ? Li1 C14A H17 101.9 . . ? C14 C14A H17 107.5 . . ? C13 C14A H17 44.9 . . ? O2 C14A H17 143.1 . . ? C16 C14A H17 129.5 . . ? C15 C14A H17 112.6 . . ? Li1 C14A H17 101.9 . . ? H17 C14A H17 0.0 . . ? C16A C16 C15 94.4(12) . . ? C16A C16 C14A 122.6(10) . . ? C15 C16 C14A 68.8(6) . . ? C16A C16 C17 53.5(9) . . ? C15 C16 C17 106.4(6) . . ? C14A C16 C17 78.3(4) . . ? C43A C43 C42 70.3(4) . . ? C43A C43 O5 64.0(4) . . ? C42 C43 O5 107.3(3) . . ? C43A C43 C44 64.6(4) . . ? C42 C43 C44 108.9(3) . . ? O5 C43 C44 98.7(3) . . ? C43A C43 Li4 80.2(4) . . ? C42 C43 Li4 76.8(2) . . ? O5 C43 Li4 43.18(16) . . ? C44 C43 Li4 138.2(3) . . ? C45A C45 C44 86.6(9) . . ? C45A C45 C46 70.4(8) . . ? C44 C45 C46 107.0(5) . . ? C45A C45 C43A 119.8(10) . . ? C44 C45 C43A 66.7(5) . . ? C46 C45 C43A 68.2(4) . . ? C46A C46 O5 77.0(10) . . ? C46A C46 C45 108.5(10) . . ? O5 C46 C45 106.9(4) . . ? C46A C46 C45A 70.8(10) . . ? O5 C46 C45A 113.2(6) . . ? C45 C46 C45A 41.2(6) . . ? C46A C46 C43A 117.1(12) . . ? O5 C46 C43A 57.5(3) . . ? C45 C46 C43A 56.6(4) . . ? C45A C46 C43A 88.7(6) . . ? O1 Li1 O2 125.0(3) . . ? O1 Li1 O3 96.8(2) . . ? O2 Li1 O3 136.9(3) . . ? O1 Li1 N1 99.8(2) . . ? O2 Li1 N1 87.3(2) . . ? O3 Li1 N1 96.7(2) . . ? O1 Li1 Li2 47.02(16) . . ? O2 Li1 Li2 165.9(3) . . ? O3 Li1 Li2 49.84(16) . . ? N1 Li1 Li2 104.9(2) . . ? O1 Li1 C29 129.0(2) . . ? O2 Li1 C29 105.9(2) . . ? O3 Li1 C29 32.78(10) . . ? N1 Li1 C29 84.96(18) . . ? Li2 Li1 C29 82.47(18) . . ? O1 Li1 C1 28.26(10) . . ? O2 Li1 C1 101.7(2) . . ? O3 Li1 C1 121.4(2) . . ? N1 Li1 C1 82.98(18) . . ? Li2 Li1 C1 73.48(18) . . ? C29 Li1 C1 149.2(2) . . ? O1 Li1 C14A 110.0(3) . . ? O2 Li1 C14A 33.48(19) . . ? O3 Li1 C14A 145.3(3) . . ? N1 Li1 C14A 58.1(2) . . ? Li2 Li1 C14A 151.9(3) . . ? C29 Li1 C14A 115.1(2) . . ? C1 Li1 C14A 81.8(2) . . ? O1 Li2 O3 102.5(2) . . ? O1 Li2 O6 155.8(3) . . ? O3 Li2 O6 99.5(2) . . ? O1 Li2 Li1 50.11(18) . . ? O3 Li2 Li1 52.54(17) . . ? O6 Li2 Li1 151.4(3) . . ? O1 Li2 Li3 146.8(3) . . ? O3 Li2 Li3 49.39(16) . . ? O6 Li2 Li3 50.96(16) . . ? Li1 Li2 Li3 100.4(2) . . ? O1 Li2 C58 127.1(3) . . ? O3 Li2 C58 129.5(2) . . ? O6 Li2 C58 30.02(10) . . ? Li1 Li2 C58 174.5(3) . . ? Li3 Li2 C58 80.67(18) . . ? O4 Li3 O3 152.5(3) . . ? O4 Li3 O6 103.6(2) . . ? O3 Li3 O6 98.8(2) . . ? O4 Li3 Li4 50.87(16) . . ? O3 Li3 Li4 149.2(3) . . ? O6 Li3 Li4 52.82(16) . . ? O4 Li3 Li2 144.9(3) . . ? O3 Li3 Li2 49.94(16) . . ? O6 Li3 Li2 49.68(16) . . ? Li4 Li3 Li2 99.7(2) . . ? O4 Li3 C29 125.0(2) . . ? O3 Li3 C29 30.82(11) . . ? O6 Li3 C29 129.6(2) . . ? Li4 Li3 C29 170.3(2) . . ? Li2 Li3 C29 80.52(18) . . ? O4 Li4 O5 126.4(2) . . ? O4 Li4 O6 98.5(2) . . ? O5 Li4 O6 133.7(3) . . ? O4 Li4 N2 100.3(2) . . ? O5 Li4 N2 87.12(18) . . ? O6 Li4 N2 96.42(19) . . ? O4 Li4 Li3 47.29(15) . . ? O5 Li4 Li3 166.7(3) . . ? O6 Li4 Li3 51.28(15) . . ? N2 Li4 Li3 105.2(2) . . ? O4 Li4 C58 130.6(2) . . ? O5 Li4 C58 102.9(2) . . ? O6 Li4 C58 32.59(10) . . ? N2 Li4 C58 84.53(17) . . ? Li3 Li4 C58 83.73(17) . . ? O4 Li4 C30 28.86(10) . . ? O5 Li4 C30 102.70(18) . . ? O6 Li4 C30 123.6(2) . . ? N2 Li4 C30 83.17(17) . . ? Li3 Li4 C30 74.28(17) . . ? C58 Li4 C30 150.91(19) . . ? O4 Li4 C43 112.0(2) . . ? O5 Li4 C43 32.06(12) . . ? O6 Li4 C43 143.3(2) . . ? N2 Li4 C43 59.37(15) . . ? Li3 Li4 C43 154.5(2) . . ? C58 Li4 C43 112.50(19) . . ? C30 Li4 C43 83.26(16) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.991 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.066 #===END data_cmpd_2 _database_code_depnum_ccdc_archive 'CCDC 733955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C35 H53 O3 N1) Li2]2' _chemical_formula_sum 'C70 H106 Li4 N2 O6' _chemical_formula_weight 1099.38 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 16.331(4) _cell_length_b 14.455(4) _cell_length_c 28.696(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.989(5) _cell_angle_gamma 90.00 _cell_volume 6765(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12452 _cell_measurement_theta_min 2.7955 _cell_measurement_theta_max 30.6400 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9970 _exptl_absorpt_correction_T_min 0.9928 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 44372 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6994 _reflns_number_gt 6423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0563P)^2^+10.8979P] 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 6994 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.1952 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _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 O1 O 0.37966(10) 0.81557(12) 0.17357(6) 0.0324(4) Uani 1 1 d . . . O2 O 0.50692(13) 0.76959(13) 0.08674(6) 0.0462(5) Uani 1 1 d . . . O3 O 0.54735(9) 0.76855(11) 0.20776(6) 0.0287(4) Uani 1 1 d . . . N1 N 0.52095(11) 0.92553(14) 0.14018(7) 0.0297(5) Uani 1 1 d . . . C1 C 0.33791(14) 0.86306(17) 0.14040(8) 0.0289(5) Uani 1 1 d . . . C2 C 0.26118(14) 0.83246(18) 0.12047(9) 0.0323(5) Uani 1 1 d . . . C3 C 0.22124(15) 0.74389(19) 0.13756(10) 0.0372(6) Uani 1 1 d . . . C4 C 0.27782(17) 0.66063(19) 0.12918(10) 0.0413(6) Uani 1 1 d . . . H1 H 0.2845 0.6535 0.0956 0.050 Uiso 1 1 calc R . . H2 H 0.2534 0.6043 0.1415 0.050 Uiso 1 1 calc R . . H3 H 0.3315 0.6713 0.1451 0.050 Uiso 1 1 calc R . . C5 C 0.20367(16) 0.7527(2) 0.18954(10) 0.0422(7) Uani 1 1 d . . . H4 H 0.2529 0.7750 0.2070 0.051 Uiso 1 1 calc R . . H5 H 0.1882 0.6921 0.2016 0.051 Uiso 1 1 calc R . . H6 H 0.1587 0.7966 0.1931 0.051 Uiso 1 1 calc R . . C6 C 0.13918(18) 0.7230(2) 0.11133(12) 0.0521(8) Uani 1 1 d . . . H7 H 0.1129 0.6703 0.1260 0.063 Uiso 1 1 calc R . . H8 H 0.1487 0.7079 0.0788 0.063 Uiso 1 1 calc R . . H9 H 0.1034 0.7773 0.1124 0.063 Uiso 1 1 calc R . . C7 C 0.22323(15) 0.88573(18) 0.08466(9) 0.0352(6) Uani 1 1 d . . . H10 H 0.1721 0.8649 0.0712 0.042 Uiso 1 1 calc R . . C8 C 0.25583(15) 0.96742(18) 0.06757(9) 0.0338(5) Uani 1 1 d . . . C9 C 0.21527(18) 1.0202(2) 0.02602(10) 0.0425(7) Uani 1 1 d . . . C10 C 0.1267(2) 0.9902(2) 0.01553(13) 0.0661(10) Uani 1 1 d . . . H11 H 0.1253 0.9247 0.0067 0.079 Uiso 1 1 calc R . . H12 H 0.1025 1.0274 -0.0102 0.079 Uiso 1 1 calc R . . H13 H 0.0952 0.9992 0.0433 0.079 Uiso 1 1 calc R . . C11 C 0.2150(2) 1.1244(2) 0.03590(11) 0.0523(8) Uani 1 1 d . . . H14 H 0.1916 1.1358 0.0661 0.063 Uiso 1 1 calc R . . H15 H 0.1818 1.1561 0.0113 0.063 Uiso 1 1 calc R . . H16 H 0.2713 1.1480 0.0365 0.063 Uiso 1 1 calc R . . C12 C 0.2651(3) 1.0023(3) -0.01680(11) 0.0712(11) Uani 1 1 d . . . H17 H 0.2377 1.0315 -0.0442 0.085 Uiso 1 1 calc R . . H18 H 0.2693 0.9355 -0.0220 0.085 Uiso 1 1 calc R . . H19 H 0.3202 1.0286 -0.0115 0.085 Uiso 1 1 calc R . . C13 C 0.33042(15) 0.99615(18) 0.08815(9) 0.0329(5) Uani 1 1 d . . . H20 H 0.3546 1.0513 0.0772 0.039 Uiso 1 1 calc R . . C14 C 0.37093(14) 0.94735(17) 0.12415(8) 0.0299(5) Uani 1 1 d . . . C15 C 0.44845(14) 0.98445(17) 0.14758(9) 0.0314(5) Uani 1 1 d . . . H21 H 0.4587 1.0473 0.1355 0.038 Uiso 1 1 calc R . . H22 H 0.4411 0.9898 0.1815 0.038 Uiso 1 1 calc R . . C16 C 0.54674(16) 0.92901(19) 0.09161(9) 0.0386(6) Uani 1 1 d . . . H23 H 0.4982 0.9523 0.0734 0.046 Uiso 1 1 d . . . H24 H 0.5892 0.9743 0.0878 0.046 Uiso 1 1 d . . . C17 C 0.5689(3) 0.8401(3) 0.07169(15) 0.0378(10) Uani 0.60 1 d P . . H25 H 0.6260 0.8293 0.0814 0.046 Uiso 0.60 1 d P . . C18 C 0.5486(3) 0.8334(3) 0.01663(11) 0.0645(10) Uani 1 1 d . . . H26 H 0.6016 0.8037 0.0111 0.076 Uiso 1 1 d . . . H27 H 0.5196 0.8720 -0.0076 0.076 Uiso 0.60 1 d P . . H27A H 0.5701 0.8933 0.0099 0.076 Uiso 0.40 1 d P . . C19 C 0.4974(4) 0.7397(6) 0.00643(19) 0.0653(17) Uani 0.60 1 d P . . H28 H 0.5360 0.6960 -0.0089 0.075 Uiso 0.60 1 d P . . H29 H 0.4540 0.7511 -0.0179 0.076 Uiso 1 1 d . . . C20 C 0.4703(3) 0.7175(4) 0.05043(13) 0.0998(18) Uani 1 1 d . . . H30 H 0.5018 0.6634 0.0549 0.114 Uiso 1 1 d . . . H31 H 0.4109 0.7136 0.0578 0.114 Uiso 1 1 d . . . C21 C 0.58893(14) 0.94430(17) 0.17519(9) 0.0328(5) Uani 1 1 d . . . H32 H 0.5663 0.9530 0.2062 0.039 Uiso 1 1 calc R . . H33 H 0.6170 1.0022 0.1669 0.039 Uiso 1 1 calc R . . C22 C 0.65003(14) 0.86628(17) 0.17768(8) 0.0293(5) Uani 1 1 d . . . C23 C 0.72992(14) 0.88025(18) 0.16427(8) 0.0314(5) Uani 1 1 d . . . H34 H 0.7459 0.9403 0.1548 0.038 Uiso 1 1 calc R . . C24 C 0.78687(14) 0.80893(18) 0.16432(8) 0.0306(5) Uani 1 1 d . . . C25 C 0.87550(14) 0.82246(18) 0.15038(9) 0.0322(5) Uani 1 1 d . . . C26 C 0.89369(16) 0.92244(19) 0.13656(10) 0.0403(6) Uani 1 1 d . . . H35 H 0.8889 0.9629 0.1637 0.048 Uiso 1 1 calc R . . H36 H 0.8543 0.9420 0.1115 0.048 Uiso 1 1 calc R . . H37 H 0.9494 0.9264 0.1256 0.048 Uiso 1 1 calc R . . C27 C 0.89171(16) 0.7607(2) 0.10846(10) 0.0429(7) Uani 1 1 d . . . H38 H 0.8575 0.7811 0.0813 0.052 Uiso 1 1 calc R . . H39 H 0.8783 0.6964 0.1158 0.052 Uiso 1 1 calc R . . H40 H 0.9497 0.7649 0.1014 0.052 Uiso 1 1 calc R . . C28 C 0.93419(16) 0.7964(3) 0.19173(11) 0.0521(8) Uani 1 1 d . . . H41 H 0.9908 0.8081 0.1836 0.063 Uiso 1 1 calc R . . H42 H 0.9276 0.7307 0.1991 0.063 Uiso 1 1 calc R . . H43 H 0.9216 0.8338 0.2190 0.063 Uiso 1 1 calc R . . C29 C 0.75936(14) 0.72198(17) 0.17745(8) 0.0302(5) Uani 1 1 d . . . H44 H 0.7969 0.6719 0.1767 0.036 Uiso 1 1 calc R . . C30 C 0.68009(14) 0.70305(17) 0.19173(8) 0.0288(5) Uani 1 1 d . . . C31 C 0.65470(15) 0.60347(17) 0.20403(9) 0.0327(6) Uani 1 1 d . . . C32 C 0.72683(18) 0.5359(2) 0.20334(12) 0.0492(8) Uani 1 1 d . . . H45 H 0.7468 0.5329 0.1718 0.059 Uiso 1 1 calc R . . H46 H 0.7088 0.4743 0.2127 0.059 Uiso 1 1 calc R . . H47 H 0.7711 0.5572 0.2251 0.059 Uiso 1 1 calc R . . C33 C 0.62172(17) 0.59769(19) 0.25316(9) 0.0386(6) Uani 1 1 d . . . H48 H 0.6626 0.6229 0.2760 0.046 Uiso 1 1 calc R . . H49 H 0.6107 0.5329 0.2608 0.046 Uiso 1 1 calc R . . H50 H 0.5709 0.6336 0.2541 0.046 Uiso 1 1 calc R . . C34 C 0.58820(19) 0.5696(2) 0.16831(10) 0.0463(7) Uani 1 1 d . . . H51 H 0.5678 0.5092 0.1781 0.056 Uiso 1 1 calc R . . H52 H 0.6114 0.5637 0.1376 0.056 Uiso 1 1 calc R . . H53 H 0.5429 0.6141 0.1664 0.056 Uiso 1 1 calc R . . C35 C 0.62454(13) 0.77817(17) 0.19287(8) 0.0277(5) Uani 1 1 d . . . C17A C 0.4997(4) 0.8558(5) 0.0594(2) 0.0353(14) Uani 0.40 1 d P . . H25A H 0.4411 0.8757 0.0574 0.043 Uiso 0.40 1 d P . . C19A C 0.4694(6) 0.8033(8) 0.0115(3) 0.064(3) Uani 0.40 1 d P . . H28A H 0.4262 0.8364 0.0143 0.076 Uiso 0.40 1 d P . . Li1 Li 0.4841(3) 0.7937(3) 0.15050(14) 0.0338(9) Uani 1 1 d . . . Li2 Li 0.4345(3) 0.7816(3) 0.22645(15) 0.0399(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0243(8) 0.0393(10) 0.0334(9) 0.0045(8) 0.0001(7) 0.0003(7) O2 0.0690(14) 0.0389(11) 0.0314(10) -0.0038(8) 0.0092(9) -0.0043(10) O3 0.0231(8) 0.0350(9) 0.0285(8) 0.0015(7) 0.0056(6) 0.0003(7) N1 0.0230(9) 0.0321(11) 0.0344(11) 0.0005(9) 0.0052(8) 0.0013(8) C1 0.0247(11) 0.0343(13) 0.0282(12) -0.0017(10) 0.0048(9) 0.0038(10) C2 0.0269(12) 0.0365(13) 0.0338(13) 0.0006(11) 0.0029(10) 0.0015(10) C3 0.0284(12) 0.0387(14) 0.0444(15) 0.0028(12) -0.0009(11) -0.0033(11) C4 0.0446(15) 0.0353(14) 0.0435(15) 0.0027(12) -0.0025(12) -0.0024(12) C5 0.0323(13) 0.0459(16) 0.0490(17) 0.0084(13) 0.0084(12) -0.0009(12) C6 0.0374(15) 0.0512(18) 0.066(2) 0.0137(15) -0.0098(14) -0.0110(13) C7 0.0298(12) 0.0391(14) 0.0361(13) -0.0021(11) -0.0046(10) -0.0019(11) C8 0.0335(13) 0.0361(13) 0.0315(13) -0.0011(11) -0.0014(10) 0.0008(11) C9 0.0468(16) 0.0429(16) 0.0368(14) 0.0043(12) -0.0066(12) 0.0003(13) C10 0.062(2) 0.060(2) 0.073(2) 0.0221(18) -0.0340(18) -0.0064(17) C11 0.0569(19) 0.0455(17) 0.0525(18) 0.0108(14) -0.0145(15) 0.0017(14) C12 0.090(3) 0.086(3) 0.0369(17) 0.0015(17) -0.0042(17) 0.017(2) C13 0.0322(12) 0.0315(13) 0.0351(13) -0.0006(10) 0.0029(10) 0.0009(10) C14 0.0250(11) 0.0333(13) 0.0317(12) -0.0036(10) 0.0038(9) 0.0038(10) C15 0.0256(11) 0.0311(13) 0.0375(13) -0.0022(10) 0.0020(10) 0.0022(10) C16 0.0334(13) 0.0464(16) 0.0366(14) 0.0064(12) 0.0076(11) -0.0039(12) C17 0.033(2) 0.047(3) 0.034(2) 0.002(2) 0.0060(18) 0.0023(19) C18 0.094(3) 0.065(2) 0.0367(16) 0.0069(15) 0.0250(17) 0.020(2) C19 0.053(3) 0.109(6) 0.033(3) 0.004(3) -0.005(2) -0.010(4) C20 0.092(3) 0.167(5) 0.042(2) -0.027(3) 0.011(2) -0.058(3) C21 0.0249(11) 0.0331(13) 0.0404(14) -0.0013(11) 0.0028(10) -0.0025(10) C22 0.0244(11) 0.0320(13) 0.0314(12) -0.0006(10) 0.0026(9) -0.0003(9) C23 0.0260(11) 0.0331(13) 0.0352(13) 0.0005(10) 0.0022(10) -0.0039(10) C24 0.0245(11) 0.0391(14) 0.0283(12) -0.0013(10) 0.0020(9) -0.0020(10) C25 0.0233(11) 0.0405(14) 0.0334(13) -0.0010(11) 0.0059(10) -0.0014(10) C26 0.0295(13) 0.0451(16) 0.0472(16) -0.0049(12) 0.0092(11) -0.0071(11) C27 0.0323(13) 0.0491(16) 0.0487(16) -0.0084(13) 0.0141(12) -0.0047(12) C28 0.0266(13) 0.079(2) 0.0510(18) 0.0086(16) 0.0011(12) -0.0008(14) C29 0.0266(11) 0.0349(13) 0.0292(12) -0.0029(10) 0.0036(9) 0.0040(10) C30 0.0272(11) 0.0337(13) 0.0259(11) -0.0021(10) 0.0044(9) -0.0009(10) C31 0.0306(12) 0.0330(13) 0.0354(13) 0.0012(10) 0.0093(10) 0.0011(10) C32 0.0458(16) 0.0357(15) 0.068(2) 0.0068(14) 0.0236(15) 0.0059(13) C33 0.0403(14) 0.0386(14) 0.0376(14) 0.0050(12) 0.0101(11) -0.0010(12) C34 0.0573(18) 0.0395(16) 0.0423(16) -0.0059(13) 0.0047(13) -0.0095(13) C35 0.0226(11) 0.0360(13) 0.0249(11) -0.0027(10) 0.0045(9) -0.0014(9) C17A 0.037(3) 0.040(4) 0.029(3) 0.003(3) 0.003(3) 0.003(3) C19A 0.049(5) 0.093(7) 0.048(5) -0.025(5) -0.010(4) 0.012(5) Li1 0.032(2) 0.039(2) 0.031(2) -0.0002(18) 0.0037(17) -0.0018(18) Li2 0.028(2) 0.059(3) 0.034(2) 0.005(2) 0.0051(18) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.332(3) . ? O1 Li2 1.791(5) . ? O1 Li1 1.889(5) . ? O2 C20 1.395(4) . ? O2 C17A 1.474(7) . ? O2 C17 1.515(5) . ? O2 Li1 1.918(5) . ? O3 C35 1.359(3) . ? O3 Li2 1.905(5) 2_655 ? O3 Li1 1.929(4) . ? O3 Li2 1.955(4) . ? N1 C16 1.478(3) . ? N1 C15 1.483(3) . ? N1 C21 1.483(3) . ? N1 Li1 2.025(5) . ? C1 C2 1.421(3) . ? C1 C14 1.421(3) . ? C1 Li1 2.593(5) . ? C2 C7 1.402(4) . ? C2 C3 1.529(4) . ? C3 C6 1.533(4) . ? C3 C5 1.539(4) . ? C3 C4 1.544(4) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.395(4) . ? C7 H10 0.9500 . ? C8 C13 1.389(3) . ? C8 C9 1.536(4) . ? C9 C10 1.525(4) . ? C9 C12 1.531(5) . ? C9 C11 1.533(4) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.390(3) . ? C13 H20 0.9500 . ? C14 C15 1.501(3) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.459(5) . ? C16 C17A 1.579(7) . ? C16 H23 0.9854 . ? C16 H24 0.9639 . ? C17 C17A 1.188(8) . ? C17 C18 1.600(5) . ? C17 H25 0.9723 . ? C18 C19A 1.364(10) . ? C18 C17A 1.534(7) . ? C18 C19 1.610(8) . ? C18 H26 0.9867 . ? C18 H27 0.9926 . ? C18 H27A 0.9578 . ? C19 C19A 1.039(11) . ? C19 C20 1.397(7) . ? C19 H28 1.0106 . ? C19 H29 0.9822 . ? C19 H29 0.9822 . ? C20 C19A 1.669(12) . ? C20 H30 0.9409 . ? C20 H31 1.0062 . ? C21 C22 1.505(3) . ? C21 H32 0.9900 . ? C21 H33 0.9900 . ? C22 C23 1.394(3) . ? C22 C35 1.416(3) . ? C23 C24 1.388(3) . ? C23 H34 0.9500 . ? C24 C29 1.393(4) . ? C24 C25 1.534(3) . ? C25 C26 1.532(4) . ? C25 C27 1.532(4) . ? C25 C28 1.533(4) . ? C26 H35 0.9800 . ? C26 H36 0.9800 . ? C26 H37 0.9800 . ? C27 H38 0.9800 . ? C27 H39 0.9800 . ? C27 H40 0.9800 . ? C28 H41 0.9800 . ? C28 H42 0.9800 . ? C28 H43 0.9800 . ? C29 C30 1.405(3) . ? C29 H44 0.9500 . ? C30 C35 1.416(3) . ? C30 C31 1.544(3) . ? C31 C32 1.532(4) . ? C31 C34 1.534(4) . ? C31 C33 1.537(3) . ? C32 H45 0.9800 . ? C32 H46 0.9800 . ? C32 H47 0.9800 . ? C33 H48 0.9800 . ? C33 H49 0.9800 . ? C33 H50 0.9800 . ? C34 H51 0.9800 . ? C34 H52 0.9800 . ? C34 H53 0.9800 . ? C35 Li1 2.548(5) . ? C35 Li2 2.555(5) 2_655 ? C17A C19A 1.624(11) . ? C17A Li1 2.788(7) . ? C17A H23 1.4525 . ? C17A H25A 0.9980 . ? C19A H27 1.4161 . ? C19A H29 1.1497 . ? C19A H29 1.1497 . ? C19A H28A 0.8592 . ? Li1 Li2 2.371(6) . ? Li2 O3 1.905(5) 2_655 ? Li2 Li2 2.469(9) 2_655 ? Li2 C35 2.555(5) 2_655 ? 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 C1 O1 Li2 164.2(2) . . ? C1 O1 Li1 105.90(19) . . ? Li2 O1 Li1 80.20(19) . . ? C20 O2 C17A 92.2(4) . . ? C20 O2 C17 114.6(3) . . ? C17A O2 C17 46.8(3) . . ? C20 O2 Li1 135.6(3) . . ? C17A O2 Li1 109.9(3) . . ? C17 O2 Li1 108.4(2) . . ? C35 O3 Li2 101.70(18) . 2_655 ? C35 O3 Li1 100.18(18) . . ? Li2 O3 Li1 151.0(2) 2_655 . ? C35 O3 Li2 168.4(2) . . ? Li2 O3 Li2 79.5(2) 2_655 . ? Li1 O3 Li2 75.26(19) . . ? C16 N1 C15 112.62(19) . . ? C16 N1 C21 113.12(18) . . ? C15 N1 C21 111.90(19) . . ? C16 N1 Li1 105.75(19) . . ? C15 N1 Li1 105.93(18) . . ? C21 N1 Li1 106.88(19) . . ? O1 C1 C2 122.3(2) . . ? O1 C1 C14 119.2(2) . . ? C2 C1 C14 118.5(2) . . ? O1 C1 Li1 44.49(13) . . ? C2 C1 Li1 135.4(2) . . ? C14 C1 Li1 90.31(17) . . ? C7 C2 C1 118.1(2) . . ? C7 C2 C3 121.0(2) . . ? C1 C2 C3 120.9(2) . . ? C2 C3 C6 112.6(2) . . ? C2 C3 C5 110.2(2) . . ? C6 C3 C5 106.9(2) . . ? C2 C3 C4 109.5(2) . . ? C6 C3 C4 106.5(2) . . ? C5 C3 C4 111.0(2) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C8 C7 C2 124.1(2) . . ? C8 C7 H10 118.0 . . ? C2 C7 H10 118.0 . . ? C13 C8 C7 116.5(2) . . ? C13 C8 C9 121.0(2) . . ? C7 C8 C9 122.4(2) . . ? C10 C9 C12 109.4(3) . . ? C10 C9 C11 107.7(3) . . ? C12 C9 C11 108.7(3) . . ? C10 C9 C8 112.2(2) . . ? C12 C9 C8 108.3(2) . . ? C11 C9 C8 110.5(2) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 122.5(2) . . ? C8 C13 H20 118.8 . . ? C14 C13 H20 118.8 . . ? C13 C14 C1 120.3(2) . . ? C13 C14 C15 120.6(2) . . ? C1 C14 C15 119.0(2) . . ? N1 C15 C14 113.1(2) . . ? N1 C15 H21 109.0 . . ? C14 C15 H21 109.0 . . ? N1 C15 H22 109.0 . . ? C14 C15 H22 109.0 . . ? H21 C15 H22 107.8 . . ? C17 C16 N1 115.4(3) . . ? C17 C16 C17A 45.8(3) . . ? N1 C16 C17A 112.0(3) . . ? C17 C16 H23 107.6 . . ? N1 C16 H23 104.5 . . ? C17A C16 H23 64.2 . . ? C17 C16 H24 111.0 . . ? N1 C16 H24 111.9 . . ? C17A C16 H24 136.0 . . ? H23 C16 H24 105.7 . . ? C17A C17 C16 72.4(4) . . ? C17A C17 O2 64.7(4) . . ? C16 C17 O2 107.3(3) . . ? C17A C17 C18 64.8(4) . . ? C16 C17 C18 113.4(3) . . ? O2 C17 C18 97.7(3) . . ? C17A C17 H25 178.2 . . ? C16 C17 H25 106.4 . . ? O2 C17 H25 117.1 . . ? C18 C17 H25 114.8 . . ? C19A C18 C17A 67.9(5) . . ? C19A C18 C17 105.8(5) . . ? C17A C18 C17 44.5(3) . . ? C19A C18 C19 39.8(5) . . ? C17A C18 C19 92.0(4) . . ? C17 C18 C19 108.0(3) . . ? C19A C18 H26 132.7 . . ? C17A C18 H26 136.0 . . ? C17 C18 H26 92.8 . . ? C19 C18 H26 93.3 . . ? C19A C18 H27 71.9 . . ? C17A C18 H27 101.1 . . ? C17 C18 H27 136.4 . . ? C19 C18 H27 97.0 . . ? H26 C18 H27 121.4 . . ? C19A C18 H27A 128.4 . . ? C17A C18 H27A 100.5 . . ? C17 C18 H27A 94.8 . . ? C19 C18 H27A 156.4 . . ? H26 C18 H27A 91.5 . . ? H27 C18 H27A 61.1 . . ? C19A C19 C20 85.2(8) . . ? C19A C19 C18 57.3(7) . . ? C20 C19 C18 102.4(5) . . ? C19A C19 H28 154.6 . . ? C20 C19 H28 118.9 . . ? C18 C19 H28 105.9 . . ? C19A C19 H29 69.3 . . ? C20 C19 H29 115.5 . . ? C18 C19 H29 109.7 . . ? H28 C19 H29 103.9 . . ? C19A C19 H29 69.3 . . ? C20 C19 H29 115.5 . . ? C18 C19 H29 109.7 . . ? H28 C19 H29 103.9 . . ? H29 C19 H29 0.0 . . ? O2 C20 C19 114.1(4) . . ? O2 C20 C19A 95.0(4) . . ? C19 C20 C19A 38.3(4) . . ? O2 C20 H30 97.8 . . ? C19 C20 H30 96.8 . . ? C19A C20 H30 134.0 . . ? O2 C20 H31 104.7 . . ? C19 C20 H31 123.9 . . ? C19A C20 H31 102.0 . . ? H30 C20 H31 116.8 . . ? N1 C21 C22 111.5(2) . . ? N1 C21 H32 109.3 . . ? C22 C21 H32 109.3 . . ? N1 C21 H33 109.3 . . ? C22 C21 H33 109.3 . . ? H32 C21 H33 108.0 . . ? C23 C22 C35 120.6(2) . . ? C23 C22 C21 120.4(2) . . ? C35 C22 C21 118.9(2) . . ? C24 C23 C22 121.9(2) . . ? C24 C23 H34 119.0 . . ? C22 C23 H34 119.0 . . ? C23 C24 C29 116.4(2) . . ? C23 C24 C25 123.1(2) . . ? C29 C24 C25 120.5(2) . . ? C26 C25 C27 107.6(2) . . ? C26 C25 C28 108.1(2) . . ? C27 C25 C28 109.7(2) . . ? C26 C25 C24 112.7(2) . . ? C27 C25 C24 109.5(2) . . ? C28 C25 C24 109.1(2) . . ? C25 C26 H35 109.5 . . ? C25 C26 H36 109.5 . . ? H35 C26 H36 109.5 . . ? C25 C26 H37 109.5 . . ? H35 C26 H37 109.5 . . ? H36 C26 H37 109.5 . . ? C25 C27 H38 109.5 . . ? C25 C27 H39 109.5 . . ? H38 C27 H39 109.5 . . ? C25 C27 H40 109.5 . . ? H38 C27 H40 109.5 . . ? H39 C27 H40 109.5 . . ? C25 C28 H41 109.5 . . ? C25 C28 H42 109.5 . . ? H41 C28 H42 109.5 . . ? C25 C28 H43 109.5 . . ? H41 C28 H43 109.5 . . ? H42 C28 H43 109.5 . . ? C24 C29 C30 124.7(2) . . ? C24 C29 H44 117.6 . . ? C30 C29 H44 117.6 . . ? C29 C30 C35 117.3(2) . . ? C29 C30 C31 120.7(2) . . ? C35 C30 C31 122.0(2) . . ? C32 C31 C34 107.8(2) . . ? C32 C31 C33 106.5(2) . . ? C34 C31 C33 109.0(2) . . ? C32 C31 C30 112.1(2) . . ? C34 C31 C30 109.5(2) . . ? C33 C31 C30 111.8(2) . . ? C31 C32 H45 109.5 . . ? C31 C32 H46 109.5 . . ? H45 C32 H46 109.5 . . ? C31 C32 H47 109.5 . . ? H45 C32 H47 109.5 . . ? H46 C32 H47 109.5 . . ? C31 C33 H48 109.5 . . ? C31 C33 H49 109.5 . . ? H48 C33 H49 109.5 . . ? C31 C33 H50 109.5 . . ? H48 C33 H50 109.5 . . ? H49 C33 H50 109.5 . . ? C31 C34 H51 109.5 . . ? C31 C34 H52 109.5 . . ? H51 C34 H52 109.5 . . ? C31 C34 H53 109.5 . . ? H51 C34 H53 109.5 . . ? H52 C34 H53 109.5 . . ? O3 C35 C22 118.8(2) . . ? O3 C35 C30 122.3(2) . . ? C22 C35 C30 118.9(2) . . ? O3 C35 Li1 48.15(14) . . ? C22 C35 Li1 92.62(18) . . ? C30 C35 Li1 128.15(19) . . ? O3 C35 Li2 46.90(14) . 2_655 ? C22 C35 Li2 113.13(19) . 2_655 ? C30 C35 Li2 107.95(19) . 2_655 ? Li1 C35 Li2 93.32(15) . 2_655 ? C17 C17A O2 68.4(4) . . ? C17 C17A C18 70.7(4) . . ? O2 C17A C18 102.5(4) . . ? C17 C17A C16 61.8(4) . . ? O2 C17A C16 103.4(4) . . ? C18 C17A C16 110.6(4) . . ? C17 C17A C19A 113.9(6) . . ? O2 C17A C19A 93.9(6) . . ? C18 C17A C19A 51.1(4) . . ? C16 C17A C19A 157.8(6) . . ? C17 C17A Li1 78.0(4) . . ? O2 C17A Li1 40.3(2) . . ? C18 C17A Li1 139.4(4) . . ? C16 C17A Li1 74.5(3) . . ? C19A C17A Li1 127.2(5) . . ? C17 C17A H23 97.4 . . ? O2 C17A H23 131.8 . . ? C18 C17A H23 116.2 . . ? C16 C17A H23 37.6 . . ? C19A C17A H23 132.4 . . ? Li1 C17A H23 92.6 . . ? C17 C17A H25A 165.1 . . ? O2 C17A H25A 109.0 . . ? C18 C17A H25A 123.5 . . ? C16 C17A H25A 106.0 . . ? C19A C17A H25A 80.7 . . ? Li1 C17A H25A 90.8 . . ? H23 C17A H25A 73.1 . . ? C19 C19A C18 82.9(7) . . ? C19 C19A C17A 114.5(8) . . ? C18 C19A C17A 61.0(4) . . ? C19 C19A C20 56.5(7) . . ? C18 C19A C20 100.9(6) . . ? C17A C19A C20 77.8(5) . . ? C19 C19A H27 107.4 . . ? C18 C19A H27 41.8 . . ? C17A C19A H27 81.0 . . ? C20 C19A H27 142.7 . . ? C19 C19A H29 53.0 . . ? C18 C19A H29 117.3 . . ? C17A C19A H29 166.5 . . ? C20 C19A H29 89.8 . . ? H27 C19A H29 106.6 . . ? C19 C19A H29 53.0 . . ? C18 C19A H29 117.3 . . ? C17A C19A H29 166.5 . . ? C20 C19A H29 89.8 . . ? H27 C19A H29 106.6 . . ? H29 C19A H29 0.0 . . ? C19 C19A H28A 150.8 . . ? C18 C19A H28A 126.2 . . ? C17A C19A H28A 82.9 . . ? C20 C19A H28A 109.2 . . ? H27 C19A H28A 98.1 . . ? H29 C19A H28A 106.4 . . ? H29 C19A H28A 106.4 . . ? O1 Li1 O2 126.0(2) . . ? O1 Li1 O3 100.7(2) . . ? O2 Li1 O3 131.1(2) . . ? O1 Li1 N1 100.0(2) . . ? O2 Li1 N1 87.57(19) . . ? O3 Li1 N1 98.7(2) . . ? O1 Li1 Li2 48.08(15) . . ? O2 Li1 Li2 163.0(3) . . ? O3 Li1 Li2 52.87(15) . . ? N1 Li1 Li2 108.8(2) . . ? O1 Li1 C35 130.9(2) . . ? O2 Li1 C35 102.99(19) . . ? O3 Li1 C35 31.66(9) . . ? N1 Li1 C35 83.46(16) . . ? Li2 Li1 C35 84.09(17) . . ? O1 Li1 C1 29.61(10) . . ? O2 Li1 C1 100.77(19) . . ? O3 Li1 C1 128.1(2) . . ? N1 Li1 C1 84.16(17) . . ? Li2 Li1 C1 76.96(17) . . ? C35 Li1 C1 152.6(2) . . ? O1 Li1 C17A 113.7(2) . . ? O2 Li1 C17A 29.81(16) . . ? O3 Li1 C17A 142.1(2) . . ? N1 Li1 C17A 61.16(18) . . ? Li2 Li1 C17A 159.7(3) . . ? C35 Li1 C17A 110.6(2) . . ? C1 Li1 C17A 84.19(19) . . ? O1 Li2 O3 155.8(3) . 2_655 ? O1 Li2 O3 103.4(2) . . ? O3 Li2 O3 99.4(2) 2_655 . ? O1 Li2 Li1 51.72(16) . . ? O3 Li2 Li1 151.1(2) 2_655 . ? O3 Li2 Li1 51.88(15) . . ? O1 Li2 Li2 147.6(3) . 2_655 ? O3 Li2 Li2 51.12(17) 2_655 2_655 ? O3 Li2 Li2 49.34(15) . 2_655 ? Li1 Li2 Li2 100.1(3) . 2_655 ? O1 Li2 C35 125.3(2) . 2_655 ? O3 Li2 C35 31.40(9) 2_655 2_655 ? O3 Li2 C35 130.8(2) . 2_655 ? Li1 Li2 C35 176.2(3) . 2_655 ? Li2 Li2 C35 82.0(2) 2_655 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.293 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.048 #===END data_cmpd_3 _database_code_depnum_ccdc_archive 'CCDC 733956' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C29 H42 O3 N1) (C4 H8 O) Cr Cl (C7 H8)0.6' _chemical_formula_sum 'C37.20 H54.80 Cl Cr N O4 ' _chemical_formula_weight 667.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 16.182(4) _cell_length_b 16.300(3) _cell_length_c 16.266(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.046(4) _cell_angle_gamma 90.00 _cell_volume 3786.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 118(2) _cell_measurement_reflns_used 12630 _cell_measurement_theta_min 2.4391 _cell_measurement_theta_max 30.6011 _exptl_crystal_description Irregular _exptl_crystal_colour Pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.9637 _exptl_absorpt_correction_T_max 0.9879 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 118(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 25913 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7833 _reflns_number_gt 6351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1311P)^2^+7.0630P] 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 7833 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.1049 _refine_ls_wR_factor_ref 0.2911 _refine_ls_wR_factor_gt 0.2758 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 0.41554(6) 0.75122(4) 0.51370(5) 0.0337(3) Uani 1 1 d . . . Cl1 Cl 0.41221(10) 0.80652(8) 0.37988(8) 0.0449(4) Uani 1 1 d . . . O1 O 0.5317(2) 0.6969(3) 0.5452(2) 0.0471(9) Uani 1 1 d . . . O2 O 0.4996(7) 0.8403(7) 0.5959(8) 0.031(2) Uani 0.50 1 d P . . O3 O 0.2975(3) 0.8006(2) 0.4792(2) 0.0462(9) Uani 1 1 d . . . O4 O 0.3504(2) 0.64618(19) 0.4454(2) 0.0370(8) Uani 1 1 d . . . O2A O 0.4626(8) 0.8581(8) 0.5850(9) 0.041(3) Uani 0.50 1 d P . . N1 N 0.4215(3) 0.7153(2) 0.6409(2) 0.0295(8) Uani 1 1 d . . . C1 C 0.6026(3) 0.6772(3) 0.6283(3) 0.0365(10) Uani 1 1 d . . . C2 C 0.6966(3) 0.6791(3) 0.6443(3) 0.0394(11) Uani 1 1 d . . . C3 C 0.7210(4) 0.7046(5) 0.5672(4) 0.0584(17) Uani 1 1 d . . . C4 C 0.6913(5) 0.7939(5) 0.5396(6) 0.083(2) Uani 1 1 d . . . H1 H 0.6961 0.8242 0.5937 0.099 Uiso 1 1 calc R . . H2 H 0.6265 0.7955 0.4896 0.099 Uiso 1 1 calc R . . H3 H 0.7324 0.8192 0.5178 0.099 Uiso 1 1 calc R . . C5 C 0.6702(5) 0.6488(6) 0.4816(4) 0.079(2) Uani 1 1 d . . . H4 H 0.6103 0.6310 0.4769 0.094 Uiso 1 1 calc R . . H5 H 0.7091 0.6006 0.4882 0.094 Uiso 1 1 calc R . . H6 H 0.6590 0.6790 0.4253 0.094 Uiso 1 1 calc R . . C6 C 0.8267(5) 0.6972(6) 0.5989(5) 0.087(3) Uani 1 1 d . . . H7 H 0.8362 0.6835 0.5452 0.105 Uiso 1 1 calc R . . H8 H 0.8536 0.6539 0.6459 0.105 Uiso 1 1 calc R . . H9 H 0.8576 0.7495 0.6256 0.105 Uiso 1 1 calc R . . C7 C 0.7659(4) 0.6570(3) 0.7326(3) 0.0380(11) Uani 1 1 d . . . H10 H 0.8290 0.6572 0.7438 0.046 Uiso 1 1 calc R . . C8 C 0.7484(4) 0.6347(3) 0.8053(3) 0.0377(11) Uani 1 1 d . . . C9 C 0.8272(4) 0.6099(4) 0.8989(4) 0.0564(16) Uani 1 1 d . . . H11 H 0.8847 0.6385 0.9098 0.068 Uiso 1 1 calc R . . H12 H 0.8370 0.5505 0.8998 0.068 Uiso 1 1 calc R . . H13 H 0.8109 0.6245 0.9480 0.068 Uiso 1 1 calc R . . C10 C 0.6560(3) 0.6339(3) 0.7879(3) 0.0344(10) Uani 1 1 d . . . H14 H 0.6419 0.6201 0.8367 0.041 Uiso 1 1 calc R . . C11 C 0.5836(3) 0.6530(3) 0.7004(3) 0.0317(10) Uani 1 1 d . . . C12 C 0.4836(3) 0.6415(3) 0.6802(3) 0.0334(10) Uani 1 1 d . . . H15 H 0.4564 0.5956 0.6356 0.040 Uiso 1 1 calc R . . H16 H 0.4832 0.6253 0.7386 0.040 Uiso 1 1 calc R . . C13 C 0.4570(3) 0.7859(3) 0.7080(3) 0.0348(10) Uani 1 1 d . . . C14 C 0.5303(6) 0.8361(5) 0.6964(5) 0.0280(18) Uani 0.50 1 d P . . C15 C 0.5386(11) 0.9247(13) 0.7330(15) 0.039(4) Uani 0.50 1 d P . . C16 C 0.5553(17) 0.9721(10) 0.6621(12) 0.079(6) Uani 0.50 1 d P . . C17 C 0.5106(8) 0.9241(4) 0.5759(6) 0.095(3) Uani 1 1 d . . . C18 C 0.3266(3) 0.6880(3) 0.6254(3) 0.0338(10) Uani 1 1 d . . . H17 H 0.3326 0.6663 0.6848 0.041 Uiso 1 1 calc R . . H18 H 0.3052 0.6424 0.5799 0.041 Uiso 1 1 calc R . . C19 C 0.2523(3) 0.7541(3) 0.5905(3) 0.0354(10) Uani 1 1 d . . . C20 C 0.1920(3) 0.7582(3) 0.6295(3) 0.0408(11) Uani 1 1 d . . . H19 H 0.2023 0.7236 0.6804 0.049 Uiso 1 1 calc R . . C21 C 0.1170(4) 0.8124(4) 0.5949(4) 0.0454(12) Uani 1 1 d . . . C22 C 0.0481(4) 0.8138(5) 0.6329(4) 0.0626(18) Uani 1 1 d . . . H20 H 0.0796 0.7966 0.6983 0.075 Uiso 1 1 calc R . . H21 H -0.0036 0.7761 0.5968 0.075 Uiso 1 1 calc R . . H22 H 0.0235 0.8695 0.6282 0.075 Uiso 1 1 calc R . . C23 C 0.1058(4) 0.8642(3) 0.5222(4) 0.0423(12) Uani 1 1 d . . . H23 H 0.0560 0.9028 0.4998 0.051 Uiso 1 1 calc R . . C24 C 0.1644(4) 0.8620(3) 0.4804(3) 0.0377(11) Uani 1 1 d . . . C25 C 0.1464(4) 0.9167(3) 0.3973(3) 0.0420(12) Uani 1 1 d . . . C26 C 0.0610(4) 0.9738(4) 0.3703(4) 0.0530(14) Uani 1 1 d . . . H24 H 0.0545 0.9865 0.4259 0.064 Uiso 1 1 calc R . . H25 H 0.0042 0.9463 0.3242 0.064 Uiso 1 1 calc R . . H26 H 0.0703 1.0248 0.3438 0.064 Uiso 1 1 calc R . . C27 C 0.1256(5) 0.8623(4) 0.3126(4) 0.0646(18) Uani 1 1 d . . . H27 H 0.0834 0.8915 0.2554 0.078 Uiso 1 1 calc R . . H28 H 0.0959 0.8113 0.3170 0.078 Uiso 1 1 calc R . . H29 H 0.1842 0.8496 0.3115 0.078 Uiso 1 1 calc R . . C28 C 0.2311(4) 0.9712(3) 0.4186(4) 0.0541(15) Uani 1 1 d . . . H30 H 0.2340 0.9825 0.3609 0.065 Uiso 1 1 calc R . . H31 H 0.2885 0.9431 0.4627 0.065 Uiso 1 1 calc R . . H32 H 0.2251 1.0230 0.4460 0.065 Uiso 1 1 calc R . . C29 C 0.2395(4) 0.8053(3) 0.5160(3) 0.0371(11) Uani 1 1 d . . . C30 C 0.2504(4) 0.6464(3) 0.3773(4) 0.0510(14) Uani 1 1 d . . . H33 H 0.2352 0.6925 0.3330 0.061 Uiso 1 1 calc R . . H34 H 0.2111 0.6508 0.4090 0.061 Uiso 1 1 calc R . . C31 C 0.2354(5) 0.5649(4) 0.3280(5) 0.0695(19) Uani 1 1 d . . . H35 H 0.2294 0.5198 0.3656 0.083 Uiso 1 1 calc R . . H36 H 0.1791 0.5660 0.2663 0.083 Uiso 1 1 calc R . . C32 C 0.3217(5) 0.5565(4) 0.3190(5) 0.071(2) Uani 1 1 d . . . H37 H 0.3180 0.5898 0.2665 0.085 Uiso 1 1 calc R . . H38 H 0.3330 0.4985 0.3093 0.085 Uiso 1 1 calc R . . C33 C 0.3980(4) 0.5883(4) 0.4115(5) 0.0591(16) Uani 1 1 d . . . H39 H 0.4268 0.5427 0.4562 0.071 Uiso 1 1 calc R . . H40 H 0.4474 0.6167 0.4028 0.071 Uiso 1 1 calc R . . C34 C 0.1985(9) 0.5050(10) 0.6439(11) 0.091(4) Uani 0.60 1 d P . . H41 H 0.1860 0.5582 0.6639 0.109 Uiso 0.60 1 calc PR . . H42 H 0.1963 0.5110 0.5829 0.109 Uiso 0.60 1 calc PR . . H43 H 0.2606 0.4856 0.6894 0.109 Uiso 0.60 1 calc PR . . C35 C 0.1290(8) 0.4469(9) 0.6370(8) 0.069(3) Uani 0.60 1 d P . . C36 C 0.1379(9) 0.3689(10) 0.6495(9) 0.085(4) Uani 0.60 1 d P . . H44 H 0.1979 0.3447 0.6706 0.102 Uiso 0.60 1 calc PR . . C37 C 0.0626(9) 0.3193(7) 0.6330(9) 0.073(3) Uani 0.60 1 d P . . H45 H 0.0750 0.2627 0.6475 0.087 Uiso 0.60 1 calc PR . . C38 C -0.0169(9) 0.3415(8) 0.6020(10) 0.099(6) Uani 0.60 1 d P . . H46 H -0.0657 0.3019 0.5808 0.118 Uiso 0.60 1 calc PR . . C39 C -0.0391(8) 0.4240(11) 0.5966(8) 0.087(5) Uani 0.60 1 d P . . H47 H -0.0997 0.4427 0.5833 0.104 Uiso 0.60 1 calc PR . . C40 C 0.0380(9) 0.4809(7) 0.6128(7) 0.067(3) Uani 0.60 1 d P . . H48 H 0.0280 0.5385 0.6075 0.080 Uiso 0.60 1 calc PR . . C14A C 0.4374(9) 0.8679(6) 0.6606(7) 0.047(3) Uani 0.50 1 d P . . C15A C 0.4998(13) 0.9376(14) 0.7174(13) 0.050(5) Uani 0.50 1 d P . . C16A C 0.4953(18) 0.9828(13) 0.6416(14) 0.094(9) Uani 0.50 1 d P . . 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 0.0487(5) 0.0305(4) 0.0264(4) -0.0020(3) 0.0214(4) -0.0046(3) Cl1 0.0691(9) 0.0441(7) 0.0299(6) 0.0015(5) 0.0303(6) -0.0002(6) O1 0.0391(19) 0.077(3) 0.0253(17) 0.0044(17) 0.0152(15) 0.0004(18) O2 0.048(6) 0.026(5) 0.020(4) 0.001(3) 0.018(5) -0.005(4) O3 0.074(3) 0.0396(19) 0.0386(19) 0.0124(15) 0.0380(19) 0.0193(18) O4 0.0413(18) 0.0313(17) 0.0357(17) -0.0033(14) 0.0159(15) 0.0039(14) O2A 0.062(8) 0.040(6) 0.031(5) -0.004(4) 0.029(6) -0.008(5) N1 0.037(2) 0.0272(18) 0.0274(18) -0.0007(15) 0.0173(16) -0.0039(16) C1 0.038(3) 0.041(3) 0.030(2) 0.001(2) 0.016(2) -0.004(2) C2 0.040(3) 0.046(3) 0.036(2) -0.004(2) 0.021(2) -0.008(2) C3 0.040(3) 0.096(5) 0.045(3) 0.013(3) 0.025(3) -0.008(3) C4 0.081(5) 0.099(6) 0.078(5) 0.039(5) 0.045(4) -0.011(4) C5 0.059(4) 0.154(8) 0.035(3) -0.004(4) 0.032(3) -0.004(4) C6 0.055(4) 0.166(9) 0.052(4) 0.025(5) 0.034(3) -0.020(5) C7 0.041(3) 0.039(3) 0.037(2) -0.005(2) 0.020(2) -0.008(2) C8 0.045(3) 0.036(2) 0.034(2) -0.001(2) 0.020(2) 0.001(2) C9 0.048(3) 0.086(5) 0.035(3) 0.009(3) 0.020(2) 0.015(3) C10 0.046(3) 0.029(2) 0.034(2) 0.0009(19) 0.023(2) 0.003(2) C11 0.037(2) 0.029(2) 0.032(2) -0.0013(18) 0.0181(19) -0.0046(19) C12 0.042(3) 0.031(2) 0.033(2) 0.0025(19) 0.022(2) -0.001(2) C13 0.046(3) 0.034(2) 0.029(2) -0.0001(19) 0.022(2) -0.002(2) C14 0.042(5) 0.029(4) 0.017(4) -0.011(3) 0.017(4) -0.014(4) C15 0.050(10) 0.030(7) 0.032(9) 0.001(6) 0.014(8) -0.010(8) C16 0.16(2) 0.046(9) 0.047(9) -0.002(7) 0.067(13) -0.032(11) C17 0.193(9) 0.048(4) 0.092(5) -0.035(4) 0.106(6) -0.062(5) C18 0.041(3) 0.034(2) 0.031(2) 0.0022(19) 0.020(2) -0.003(2) C19 0.042(3) 0.033(2) 0.031(2) -0.0032(19) 0.017(2) -0.003(2) C20 0.036(2) 0.053(3) 0.033(2) 0.011(2) 0.016(2) 0.004(2) C21 0.035(3) 0.060(3) 0.038(3) 0.011(2) 0.015(2) 0.002(2) C22 0.039(3) 0.092(5) 0.063(4) 0.035(4) 0.028(3) 0.024(3) C23 0.038(3) 0.046(3) 0.041(3) 0.009(2) 0.016(2) 0.005(2) C24 0.047(3) 0.032(2) 0.031(2) -0.0004(19) 0.015(2) -0.001(2) C25 0.058(3) 0.034(2) 0.036(3) 0.004(2) 0.023(2) 0.006(2) C26 0.060(3) 0.056(3) 0.040(3) 0.011(3) 0.022(3) 0.013(3) C27 0.104(5) 0.053(3) 0.033(3) 0.009(3) 0.030(3) 0.028(4) C28 0.076(4) 0.040(3) 0.060(4) 0.015(3) 0.044(3) 0.013(3) C29 0.050(3) 0.036(2) 0.031(2) 0.002(2) 0.023(2) 0.004(2) C30 0.048(3) 0.043(3) 0.051(3) -0.003(3) 0.015(3) -0.002(3) C31 0.074(4) 0.052(4) 0.064(4) -0.013(3) 0.017(3) -0.018(3) C32 0.099(5) 0.051(4) 0.075(5) -0.031(3) 0.051(4) -0.019(4) C33 0.061(4) 0.044(3) 0.076(4) -0.017(3) 0.035(3) 0.007(3) C34 0.069(8) 0.103(11) 0.115(11) -0.018(9) 0.056(8) -0.023(8) C35 0.056(6) 0.087(9) 0.059(7) -0.029(6) 0.024(5) -0.030(6) C36 0.052(7) 0.118(12) 0.071(8) 0.031(8) 0.017(6) 0.039(8) C37 0.066(8) 0.054(6) 0.086(9) 0.026(6) 0.027(7) 0.001(6) C38 0.067(8) 0.051(7) 0.108(11) 0.039(7) -0.016(7) -0.029(6) C39 0.052(6) 0.149(14) 0.053(7) -0.034(8) 0.020(5) -0.011(8) C40 0.101(9) 0.050(6) 0.047(6) -0.014(5) 0.032(6) -0.011(6) C14A 0.080(8) 0.031(5) 0.036(5) -0.002(4) 0.033(5) -0.006(5) C15A 0.076(13) 0.040(9) 0.015(6) -0.006(6) 0.006(9) -0.018(10) C16A 0.16(2) 0.071(11) 0.050(10) -0.004(8) 0.050(13) 0.055(14) _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 O3 1.899(4) . ? Cr1 O1 1.916(4) . ? Cr1 O2 2.009(13) . ? Cr1 O2A 2.032(14) . ? Cr1 O4 2.043(3) . ? Cr1 N1 2.109(4) . ? Cr1 Cl1 2.3329(14) . ? O1 C1 1.337(6) . ? O2 O2A 0.613(11) . ? O2 C17 1.434(14) . ? O2 C14 1.469(14) . ? O2 C14A 1.822(15) . ? O3 C29 1.332(6) . ? O4 C30 1.471(6) . ? O4 C33 1.478(6) . ? O2A C17 1.375(15) . ? O2A C14A 1.475(16) . ? O2A C14 1.656(15) . ? N1 C13 1.502(6) . ? N1 C18 1.502(6) . ? N1 C12 1.504(6) . ? C1 C11 1.401(6) . ? C1 C2 1.419(7) . ? C2 C7 1.390(7) . ? C2 C3 1.539(7) . ? C3 C4 1.532(11) . ? C3 C5 1.538(10) . ? C3 C6 1.543(8) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.388(7) . ? C7 H10 0.9500 . ? C8 C10 1.386(7) . ? C8 C9 1.511(7) . ? C9 H11 0.9800 . ? C9 H12 0.9800 . ? C9 H13 0.9800 . ? C10 C11 1.388(6) . ? C10 H14 0.9500 . ? C11 C12 1.504(6) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 C14A 1.500(11) . ? C13 C14 1.524(9) . ? C14 C14A 1.429(15) . ? C14 C15 1.54(2) . ? C14 C15A 1.80(2) . ? C15 C15A 0.59(2) . ? C15 C16 1.51(3) . ? C15 C16A 1.62(3) . ? C15 C14A 1.76(2) . ? C16 C16A 0.88(3) . ? C16 C17 1.466(18) . ? C16 C15A 1.64(3) . ? C17 C16A 1.538(18) . ? C18 C19 1.511(7) . ? C18 H17 0.9900 . ? C18 H18 0.9900 . ? C19 C20 1.395(7) . ? C19 C29 1.405(7) . ? C20 C21 1.388(7) . ? C20 H19 0.9500 . ? C21 C23 1.393(7) . ? C21 C22 1.508(7) . ? C22 H20 0.9800 . ? C22 H21 0.9800 . ? C22 H22 0.9800 . ? C23 C24 1.403(7) . ? C23 H23 0.9500 . ? C24 C29 1.415(7) . ? C24 C25 1.529(7) . ? C25 C28 1.530(8) . ? C25 C27 1.536(7) . ? C25 C26 1.549(7) . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C28 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? C30 C31 1.511(8) . ? C30 H33 0.9900 . ? C30 H34 0.9900 . ? C31 C32 1.477(10) . ? C31 H35 0.9900 . ? C31 H36 0.9900 . ? C32 C33 1.520(9) . ? C32 H37 0.9900 . ? C32 H38 0.9900 . ? C33 H39 0.9900 . ? C33 H40 0.9900 . ? C34 C35 1.433(16) . ? C34 H41 0.9800 . ? C34 H42 0.9800 . ? C34 H43 0.9800 . ? C35 C36 1.285(18) . ? C35 C40 1.444(17) . ? C36 C37 1.379(18) . ? C36 H44 0.9500 . ? C37 C38 1.197(17) . ? C37 H45 0.9500 . ? C38 C39 1.38(2) . ? C38 H46 0.9500 . ? C39 C40 1.476(17) . ? C39 H47 0.9500 . ? C40 H48 0.9500 . ? C14A C15A 1.51(2) . ? C15A C16A 1.41(3) . ? 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 O3 Cr1 O1 177.29(17) . . ? O3 Cr1 O2 99.4(3) . . ? O1 Cr1 O2 83.3(3) . . ? O3 Cr1 O2A 82.0(3) . . ? O1 Cr1 O2A 100.7(3) . . ? O2 Cr1 O2A 17.4(3) . . ? O3 Cr1 O4 90.24(15) . . ? O1 Cr1 O4 87.06(15) . . ? O2 Cr1 O4 169.2(3) . . ? O2A Cr1 O4 171.0(3) . . ? O3 Cr1 N1 89.03(14) . . ? O1 Cr1 N1 91.32(14) . . ? O2 Cr1 N1 81.0(4) . . ? O2A Cr1 N1 81.1(4) . . ? O4 Cr1 N1 94.32(14) . . ? O3 Cr1 Cl1 88.95(11) . . ? O1 Cr1 Cl1 91.00(11) . . ? O2 Cr1 Cl1 93.1(3) . . ? O2A Cr1 Cl1 92.3(4) . . ? O4 Cr1 Cl1 92.09(10) . . ? N1 Cr1 Cl1 173.29(11) . . ? C1 O1 Cr1 130.4(3) . . ? O2A O2 C17 72(2) . . ? O2A O2 C14 97(2) . . ? C17 O2 C14 106.5(9) . . ? O2A O2 C14A 47(2) . . ? C17 O2 C14A 93.3(7) . . ? C14 O2 C14A 50.1(6) . . ? O2A O2 Cr1 83(2) . . ? C17 O2 Cr1 130.9(8) . . ? C14 O2 Cr1 118.4(8) . . ? C14A O2 Cr1 100.2(6) . . ? C29 O3 Cr1 135.7(3) . . ? C30 O4 C33 107.7(4) . . ? C30 O4 Cr1 120.7(3) . . ? C33 O4 Cr1 120.8(3) . . ? O2 O2A C17 83(2) . . ? O2 O2A C14A 115(3) . . ? C17 O2A C14A 113.4(10) . . ? O2 O2A C14 62(2) . . ? C17 O2A C14 99.8(9) . . ? C14A O2A C14 53.9(7) . . ? O2 O2A Cr1 79(2) . . ? C17 O2A Cr1 133.4(8) . . ? C14A O2A Cr1 113.1(9) . . ? C14 O2A Cr1 108.4(7) . . ? C13 N1 C18 111.1(3) . . ? C13 N1 C12 110.7(3) . . ? C18 N1 C12 105.1(3) . . ? C13 N1 Cr1 109.0(3) . . ? C18 N1 Cr1 110.3(3) . . ? C12 N1 Cr1 110.6(3) . . ? O1 C1 C11 119.5(4) . . ? O1 C1 C2 121.1(4) . . ? C11 C1 C2 119.4(4) . . ? C7 C2 C1 117.3(4) . . ? C7 C2 C3 121.4(5) . . ? C1 C2 C3 121.3(4) . . ? C4 C3 C5 109.7(6) . . ? C4 C3 C2 109.4(5) . . ? C5 C3 C2 110.2(5) . . ? C4 C3 C6 108.5(6) . . ? C5 C3 C6 107.0(6) . . ? C2 C3 C6 112.0(5) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C8 C7 C2 124.0(5) . . ? C8 C7 H10 118.0 . . ? C2 C7 H10 118.0 . . ? C10 C8 C7 117.5(5) . . ? C10 C8 C9 121.4(4) . . ? C7 C8 C9 121.1(5) . . ? C8 C9 H11 109.5 . . ? C8 C9 H12 109.5 . . ? H11 C9 H12 109.5 . . ? C8 C9 H13 109.5 . . ? H11 C9 H13 109.5 . . ? H12 C9 H13 109.5 . . ? C8 C10 C11 121.1(4) . . ? C8 C10 H14 119.5 . . ? C11 C10 H14 119.5 . . ? C10 C11 C1 120.7(4) . . ? C10 C11 C12 119.9(4) . . ? C1 C11 C12 119.2(4) . . ? N1 C12 C11 115.4(4) . . ? N1 C12 H15 108.4 . . ? C11 C12 H15 108.4 . . ? N1 C12 H16 108.4 . . ? C11 C12 H16 108.4 . . ? H15 C12 H16 107.5 . . ? C14A C13 N1 113.1(5) . . ? C14A C13 C14 56.4(6) . . ? N1 C13 C14 112.0(4) . . ? C14A C14 O2 77.9(7) . . ? C14A C14 C13 60.9(6) . . ? O2 C14 C13 106.7(7) . . ? C14A C14 C15 72.7(8) . . ? O2 C14 C15 108.0(11) . . ? C13 C14 C15 112.7(10) . . ? C14A C14 O2A 56.5(6) . . ? O2 C14 O2A 21.6(5) . . ? C13 C14 O2A 95.7(7) . . ? C15 C14 O2A 96.5(10) . . ? C14A C14 C15A 54.3(8) . . ? O2 C14 C15A 100.9(9) . . ? C13 C14 C15A 99.8(9) . . ? C15 C14 C15A 18.4(8) . . ? O2A C14 C15A 84.8(8) . . ? C15A C15 C16 91(4) . . ? C15A C15 C14 107(4) . . ? C16 C15 C14 101.4(15) . . ? C15A C15 C16A 59(4) . . ? C16 C15 C16A 32.5(11) . . ? C14 C15 C16A 105.7(15) . . ? C15A C15 C14A 56(4) . . ? C16 C15 C14A 101.7(14) . . ? C14 C15 C14A 50.7(8) . . ? C16A C15 C14A 80.2(13) . . ? C16A C16 C17 77(2) . . ? C16A C16 C15 80(2) . . ? C17 C16 C15 105.7(13) . . ? C16A C16 C15A 59(2) . . ? C17 C16 C15A 101.0(13) . . ? C15 C16 C15A 21.2(8) . . ? O2A C17 O2 25.1(5) . . ? O2A C17 C16 111.4(9) . . ? O2 C17 C16 110.5(9) . . ? O2A C17 C16A 97.4(12) . . ? O2 C17 C16A 110.9(11) . . ? C16 C17 C16A 34.1(10) . . ? N1 C18 C19 114.9(4) . . ? N1 C18 H17 108.5 . . ? C19 C18 H17 108.5 . . ? N1 C18 H18 108.5 . . ? C19 C18 H18 108.5 . . ? H17 C18 H18 107.5 . . ? C20 C19 C29 120.8(4) . . ? C20 C19 C18 117.8(4) . . ? C29 C19 C18 121.2(4) . . ? C21 C20 C19 120.8(5) . . ? C21 C20 H19 119.6 . . ? C19 C20 H19 119.6 . . ? C20 C21 C23 118.0(5) . . ? C20 C21 C22 121.1(5) . . ? C23 C21 C22 120.8(5) . . ? C21 C22 H20 109.5 . . ? C21 C22 H21 109.5 . . ? H20 C22 H21 109.5 . . ? C21 C22 H22 109.5 . . ? H20 C22 H22 109.5 . . ? H21 C22 H22 109.5 . . ? C21 C23 C24 123.2(5) . . ? C21 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C23 C24 C29 117.7(4) . . ? C23 C24 C25 121.5(4) . . ? C29 C24 C25 120.8(4) . . ? C24 C25 C28 111.2(4) . . ? C24 C25 C27 109.0(4) . . ? C28 C25 C27 109.5(5) . . ? C24 C25 C26 112.0(4) . . ? C28 C25 C26 107.5(4) . . ? C27 C25 C26 107.6(5) . . ? C25 C26 H24 109.5 . . ? C25 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C25 C26 H26 109.5 . . ? H24 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C25 C27 H27 109.5 . . ? C25 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C25 C27 H29 109.5 . . ? H27 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C25 C28 H30 109.5 . . ? C25 C28 H31 109.5 . . ? H30 C28 H31 109.5 . . ? C25 C28 H32 109.5 . . ? H30 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? O3 C29 C19 120.2(4) . . ? O3 C29 C24 120.4(4) . . ? C19 C29 C24 119.4(4) . . ? O4 C30 C31 104.0(5) . . ? O4 C30 H33 111.0 . . ? C31 C30 H33 111.0 . . ? O4 C30 H34 111.0 . . ? C31 C30 H34 111.0 . . ? H33 C30 H34 109.0 . . ? C32 C31 C30 102.2(5) . . ? C32 C31 H35 111.3 . . ? C30 C31 H35 111.3 . . ? C32 C31 H36 111.3 . . ? C30 C31 H36 111.3 . . ? H35 C31 H36 109.2 . . ? C31 C32 C33 103.7(5) . . ? C31 C32 H37 111.0 . . ? C33 C32 H37 111.0 . . ? C31 C32 H38 111.0 . . ? C33 C32 H38 111.0 . . ? H37 C32 H38 109.0 . . ? O4 C33 C32 105.3(5) . . ? O4 C33 H39 110.7 . . ? C32 C33 H39 110.7 . . ? O4 C33 H40 110.7 . . ? C32 C33 H40 110.7 . . ? H39 C33 H40 108.8 . . ? C35 C34 H41 109.5 . . ? C35 C34 H42 109.5 . . ? H41 C34 H42 109.5 . . ? C35 C34 H43 109.5 . . ? H41 C34 H43 109.5 . . ? H42 C34 H43 109.5 . . ? C36 C35 C34 128.1(14) . . ? C36 C35 C40 116.5(11) . . ? C34 C35 C40 115.5(13) . . ? C35 C36 C37 121.8(11) . . ? C35 C36 H44 119.1 . . ? C37 C36 H44 119.1 . . ? C38 C37 C36 125.6(12) . . ? C38 C37 H45 117.2 . . ? C36 C37 H45 117.2 . . ? C37 C38 C39 121.1(11) . . ? C37 C38 H46 119.5 . . ? C39 C38 H46 119.5 . . ? C38 C39 C40 115.3(12) . . ? C38 C39 H47 122.4 . . ? C40 C39 H47 122.4 . . ? C35 C40 C39 118.5(11) . . ? C35 C40 H48 120.8 . . ? C39 C40 H48 120.8 . . ? C14 C14A O2A 69.5(8) . . ? C14 C14A C13 62.7(6) . . ? O2A C14A C13 104.9(8) . . ? C14 C14A C15A 75.6(10) . . ? O2A C14A C15A 102.9(13) . . ? C13 C14A C15A 115.9(11) . . ? C14 C14A C15 56.6(8) . . ? O2A C14A C15 94.6(11) . . ? C13 C14A C15 102.7(9) . . ? C15A C14A C15 19.0(10) . . ? C14 C14A O2 52.0(6) . . ? O2A C14A O2 17.7(6) . . ? C13 C14A O2 92.1(7) . . ? C15A C14A O2 98.4(12) . . ? C15 C14A O2 85.6(10) . . ? C15 C15A C16A 100(5) . . ? C15 C15A C14A 105(5) . . ? C16A C15A C14A 96.5(15) . . ? C15 C15A C16 67(4) . . ? C16A C15A C16 32.5(11) . . ? C14A C15A C16 107.6(15) . . ? C15 C15A C14 55(4) . . ? C16A C15A C14 102.6(15) . . ? C14A C15A C14 50.1(9) . . ? C16 C15A C14 86.6(13) . . ? C16 C16A C15A 88(2) . . ? C16 C16A C17 68.5(18) . . ? C15A C16A C17 108.9(15) . . ? C16 C16A C15 67.2(18) . . ? C15A C16A C15 21.2(11) . . ? C17 C16A C15 97.6(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.004 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.096 #===END data_cmpd_4 _database_code_depnum_ccdc_archive 'CCDC 733957' _publ_section_abstract ; Please see full paper. ; # start Validation Reply Form _vrf_PLAT390_RD116-1 ; PROBLEM: Deviating Methyl C17A X-C-H Bond Angle ...... 131.00 Deg. RESPONSE: C17A is part of a disordered THF group. Its occupancy was refined and determined to be 0.35. C17 is the corresponding, 0.65 occupancy counter-part. ; _vrf_PLAT770_RD116-1 ; PROBLEM: Suspect C-H Bond in CIF: C17A -- H23 .. 1.42 Ang. RESPONSE: C17A is part of a disordered THF group. Its occupancy was refined and determined to be 0.35. C17 is the corresponding, 0.65 occupancy counter-part. ; _vrf_PLAT773_RD116-1 ; PROBLEM: Suspect C-C Bond in CIF: C43 -- C43 .. 1.73 Ang. RESPONSE: C43 is part of a disordered, partial-occupancy toluene molecule. It has been modelled such that C43 does not in fact form a bond with itself, but rather is in one orientation half the time, and the other orientation, the other half. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H61 Cl Cr N O4 (C7 H8)0.5' _chemical_formula_sum 'C42.50 H65 Cl Cr N O4' _chemical_formula_weight 741.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.816(2) _cell_length_b 20.060(4) _cell_length_c 16.455(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.055(4) _cell_angle_gamma 90.00 _cell_volume 4219.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17503 _cell_measurement_theta_min 2.1975 _cell_measurement_theta_max 30.8114 _exptl_crystal_description Prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.373 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_correction_T_min 0.9147 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 37202 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8726 _reflns_number_gt 7959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0889P)^2^+7.2254P] 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 8726 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1964 _refine_ls_wR_factor_gt 0.1906 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 0.44902(4) 0.31544(2) 0.59093(3) 0.01901(15) Uani 1 1 d . . . Cl1 Cl 0.43671(6) 0.34161(4) 0.72847(5) 0.0301(2) Uani 1 1 d . . . O1 O 0.33503(17) 0.25479(11) 0.59792(12) 0.0244(5) Uani 1 1 d . . . O2 O 0.5557(2) 0.24285(12) 0.61587(13) 0.0323(5) Uani 1 1 d . . . O3 O 0.55896(16) 0.38022(10) 0.57906(13) 0.0232(5) Uani 1 1 d . . . O4 O 0.34565(16) 0.38990(10) 0.55697(13) 0.0241(5) Uani 1 1 d . . . N1 N 0.46582(19) 0.27946(12) 0.47116(15) 0.0198(5) Uani 1 1 d . . . C1 C 0.2821(2) 0.21385(14) 0.54607(18) 0.0204(6) Uani 1 1 d . . . C2 C 0.2132(2) 0.16584(15) 0.57612(19) 0.0228(6) Uani 1 1 d . . . C3 C 0.1978(3) 0.16133(17) 0.6681(2) 0.0302(7) Uani 1 1 d . . . C4 C 0.1531(3) 0.22650(19) 0.6988(2) 0.0402(9) Uani 1 1 d . . . H1 H 0.1095 0.2476 0.6547 0.048 Uiso 1 1 calc R . . H2 H 0.2106 0.2565 0.7166 0.048 Uiso 1 1 calc R . . H3 H 0.1106 0.2172 0.7446 0.048 Uiso 1 1 calc R . . C5 C 0.1229(4) 0.1043(2) 0.6859(2) 0.0478(11) Uani 1 1 d . . . H4 H 0.1287 0.0688 0.6455 0.057 Uiso 1 1 calc R . . H5 H 0.0510 0.1211 0.6831 0.057 Uiso 1 1 calc R . . H6 H 0.1414 0.0865 0.7406 0.057 Uiso 1 1 calc R . . C6 C 0.3020(3) 0.14695(19) 0.7163(2) 0.0406(9) Uani 1 1 d . . . H7 H 0.3014 0.1669 0.7706 0.049 Uiso 1 1 calc R . . H8 H 0.3594 0.1661 0.6876 0.049 Uiso 1 1 calc R . . H9 H 0.3118 0.0987 0.7215 0.049 Uiso 1 1 calc R . . C7 C 0.1613(2) 0.12364(15) 0.52009(18) 0.0236(6) Uani 1 1 d . . . H10 H 0.1143 0.0919 0.5399 0.028 Uiso 1 1 calc R . . C8 C 0.1736(2) 0.12474(15) 0.43625(18) 0.0215(6) Uani 1 1 d . . . C9 C 0.1140(2) 0.07410(16) 0.37992(19) 0.0254(7) Uani 1 1 d . . . C10 C 0.1343(3) 0.08536(19) 0.2903(2) 0.0348(8) Uani 1 1 d . . . H11 H 0.2046 0.1038 0.2867 0.042 Uiso 1 1 calc R . . H12 H 0.0824 0.1167 0.2659 0.042 Uiso 1 1 calc R . . H13 H 0.1288 0.0428 0.2611 0.042 Uiso 1 1 calc R . . C11 C -0.0037(3) 0.0807(2) 0.3891(2) 0.0408(9) Uani 1 1 d . . . H14 H -0.0422 0.0687 0.3376 0.049 Uiso 1 1 calc R . . H15 H -0.0200 0.1268 0.4033 0.049 Uiso 1 1 calc R . . H16 H -0.0240 0.0507 0.4323 0.049 Uiso 1 1 calc R . . C12 C 0.1488(3) 0.00316(18) 0.4034(3) 0.0428(9) Uani 1 1 d . . . H17 H 0.0907 -0.0278 0.3908 0.051 Uiso 1 1 calc R . . H18 H 0.1695 0.0014 0.4618 0.051 Uiso 1 1 calc R . . H19 H 0.2083 -0.0095 0.3725 0.051 Uiso 1 1 calc R . . C13 C 0.2404(2) 0.17266(15) 0.40840(18) 0.0205(6) Uani 1 1 d . . . H20 H 0.2502 0.1753 0.3518 0.025 Uiso 1 1 calc R . . C14 C 0.2937(2) 0.21721(14) 0.46192(17) 0.0189(6) Uani 1 1 d . . . C15 C 0.3605(2) 0.26988(15) 0.42648(17) 0.0206(6) Uani 1 1 d . . . H21 H 0.3222 0.3128 0.4260 0.025 Uiso 1 1 calc R . . H22 H 0.3709 0.2580 0.3692 0.025 Uiso 1 1 calc R . . C16 C 0.5238(2) 0.21417(15) 0.47588(19) 0.0236(6) Uani 1 1 d . . . H23 H 0.4812 0.1808 0.4774 0.029 Uiso 1 1 d . . . H24 H 0.5626 0.2073 0.4279 0.029 Uiso 1 1 d . . . C17 C 0.6086(4) 0.2136(3) 0.5466(3) 0.0276(11) Uani 0.65 1 d P . . C18 C 0.6346(3) 0.14165(19) 0.5776(2) 0.0413(9) Uani 1 1 d . . . C19 C 0.6579(8) 0.1531(4) 0.6690(5) 0.066(2) Uani 0.65 1 d P . . C20 C 0.5902(5) 0.2098(3) 0.6891(3) 0.0746(18) Uani 1 1 d . . . C21 C 0.5232(2) 0.32967(16) 0.42355(18) 0.0234(6) Uani 1 1 d . . . H25 H 0.5268 0.3133 0.3671 0.028 Uiso 1 1 calc R . . H26 H 0.4833 0.3720 0.4211 0.028 Uiso 1 1 calc R . . C22 C 0.6319(2) 0.34314(15) 0.45934(18) 0.0214(6) Uani 1 1 d . . . C23 C 0.7191(2) 0.32628(16) 0.41704(19) 0.0243(6) Uani 1 1 d . . . H27 H 0.7093 0.3063 0.3647 0.029 Uiso 1 1 calc R . . C24 C 0.8199(2) 0.33843(16) 0.4506(2) 0.0246(6) Uani 1 1 d . . . C25 C 0.9193(3) 0.31799(19) 0.4100(2) 0.0342(8) Uani 1 1 d . . . C26 C 0.8939(3) 0.2819(3) 0.3291(3) 0.0562(13) Uani 1 1 d . . . H28 H 0.8268 0.2980 0.3043 0.067 Uiso 1 1 calc R . . H29 H 0.8895 0.2338 0.3390 0.067 Uiso 1 1 calc R . . H30 H 0.9492 0.2908 0.2923 0.067 Uiso 1 1 calc R . . C27 C 0.9848(3) 0.2715(2) 0.4677(3) 0.0503(11) Uani 1 1 d . . . H31 H 0.9383 0.2458 0.5006 0.060 Uiso 1 1 calc R . . H32 H 1.0328 0.2981 0.5036 0.060 Uiso 1 1 calc R . . H33 H 1.0252 0.2409 0.4357 0.060 Uiso 1 1 calc R . . C28 C 0.9837(3) 0.3807(2) 0.3938(3) 0.0507(11) Uani 1 1 d . . . H34 H 0.9716 0.4145 0.4351 0.061 Uiso 1 1 calc R . . H35 H 0.9624 0.3983 0.3396 0.061 Uiso 1 1 calc R . . H36 H 1.0582 0.3692 0.3965 0.061 Uiso 1 1 calc R . . C29 C 0.8292(2) 0.37094(15) 0.52581(19) 0.0241(6) Uani 1 1 d . . . H37 H 0.8975 0.3817 0.5481 0.029 Uiso 1 1 calc R . . C30 C 0.7447(2) 0.38865(15) 0.57030(18) 0.0223(6) Uani 1 1 d . . . C31 C 0.7624(2) 0.42424(17) 0.6527(2) 0.0280(7) Uani 1 1 d . . . C32 C 0.8764(3) 0.4459(2) 0.6696(2) 0.0366(8) Uani 1 1 d . . . H38 H 0.9070 0.4555 0.6180 0.044 Uiso 1 1 calc R . . H39 H 0.9160 0.4100 0.6980 0.044 Uiso 1 1 calc R . . H40 H 0.8793 0.4860 0.7037 0.044 Uiso 1 1 calc R . . C33 C 0.6944(3) 0.48782(18) 0.6536(2) 0.0359(8) Uani 1 1 d . . . H41 H 0.7337 0.5257 0.6338 0.043 Uiso 1 1 calc R . . H42 H 0.6760 0.4968 0.7094 0.043 Uiso 1 1 calc R . . H43 H 0.6304 0.4813 0.6183 0.043 Uiso 1 1 calc R . . C34 C 0.7334(3) 0.3776(2) 0.7213(2) 0.0428(9) Uani 1 1 d . . . H44 H 0.7456 0.3313 0.7057 0.051 Uiso 1 1 calc R . . H45 H 0.6594 0.3836 0.7310 0.051 Uiso 1 1 calc R . . H46 H 0.7766 0.3882 0.7712 0.051 Uiso 1 1 calc R . . C35 C 0.6436(2) 0.37066(14) 0.53765(18) 0.0208(6) Uani 1 1 d . . . C36 C 0.3737(3) 0.45989(15) 0.5771(2) 0.0304(7) Uani 1 1 d . . . H47 H 0.3942 0.4839 0.5282 0.036 Uiso 1 1 calc R . . H48 H 0.4325 0.4617 0.6194 0.036 Uiso 1 1 calc R . . C37 C 0.2770(3) 0.49032(17) 0.6081(2) 0.0347(8) Uani 1 1 d . . . H49 H 0.2711 0.5381 0.5933 0.042 Uiso 1 1 calc R . . H50 H 0.2770 0.4859 0.6681 0.042 Uiso 1 1 calc R . . C38 C 0.1890(3) 0.45024(18) 0.5657(2) 0.0346(8) Uani 1 1 d . . . H51 H 0.1244 0.4530 0.5952 0.041 Uiso 1 1 calc R . . H52 H 0.1737 0.4653 0.5088 0.041 Uiso 1 1 calc R . . C39 C 0.2338(2) 0.38072(17) 0.5689(2) 0.0329(8) Uani 1 1 d . . . H53 H 0.2241 0.3596 0.6222 0.039 Uiso 1 1 calc R . . H54 H 0.1999 0.3526 0.5251 0.039 Uiso 1 1 calc R . . C40 C 0.5531(5) 0.4735(3) 0.8823(4) 0.0745(16) Uani 1 1 d . . . C41 C 0.4529(6) 0.4514(4) 0.9191(5) 0.0376(16) Uani 0.50 1 d P . . C42 C 0.4230(3) 0.46655(18) 0.9863(3) 0.0475(11) Uani 1 1 d . . . C43 C 0.4779(7) 0.5095(4) 1.0472(5) 0.0411(18) Uani 0.50 1 d P . . C44 C 0.3917(7) 0.4824(5) 1.0529(8) 0.063(3) Uani 0.50 1 d P . . C17A C 0.5289(7) 0.1833(4) 0.5579(6) 0.0235(18) Uani 0.35 1 d P . . C19A C 0.5829(14) 0.1360(6) 0.6572(9) 0.054(3) Uani 0.35 1 d P . . 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 0.0209(3) 0.0192(3) 0.0170(3) -0.00181(18) 0.00165(18) -0.00181(18) Cl1 0.0348(4) 0.0365(4) 0.0197(4) -0.0073(3) 0.0057(3) -0.0070(3) O1 0.0328(12) 0.0244(11) 0.0163(10) -0.0038(8) 0.0040(8) -0.0103(9) O2 0.0476(15) 0.0307(12) 0.0180(11) -0.0003(9) -0.0021(10) 0.0134(11) O3 0.0206(11) 0.0231(11) 0.0264(11) -0.0060(9) 0.0049(8) -0.0047(8) O4 0.0187(10) 0.0223(11) 0.0316(12) -0.0011(9) 0.0033(9) -0.0022(8) N1 0.0188(12) 0.0200(12) 0.0206(12) -0.0001(10) 0.0004(9) 0.0004(9) C1 0.0223(14) 0.0197(14) 0.0194(14) -0.0033(11) 0.0036(11) -0.0017(11) C2 0.0251(15) 0.0223(15) 0.0214(15) -0.0021(12) 0.0048(12) -0.0026(12) C3 0.044(2) 0.0277(17) 0.0202(15) -0.0035(13) 0.0093(14) -0.0136(15) C4 0.049(2) 0.040(2) 0.0346(19) -0.0067(16) 0.0211(17) -0.0061(17) C5 0.070(3) 0.051(2) 0.0247(18) -0.0070(17) 0.0202(18) -0.033(2) C6 0.063(3) 0.036(2) 0.0218(17) 0.0036(15) -0.0013(16) -0.0114(18) C7 0.0263(15) 0.0227(15) 0.0222(15) 0.0011(12) 0.0038(12) -0.0039(12) C8 0.0203(14) 0.0226(14) 0.0213(14) -0.0007(12) -0.0003(11) -0.0018(11) C9 0.0263(16) 0.0261(16) 0.0237(15) -0.0041(12) 0.0003(12) -0.0062(12) C10 0.0368(19) 0.042(2) 0.0256(17) -0.0081(15) 0.0007(14) -0.0159(16) C11 0.0283(18) 0.054(2) 0.041(2) -0.0184(18) 0.0063(15) -0.0155(16) C12 0.053(2) 0.0266(18) 0.047(2) -0.0074(16) -0.0075(18) -0.0075(16) C13 0.0183(14) 0.0243(14) 0.0189(14) 0.0000(12) 0.0004(11) 0.0003(11) C14 0.0197(14) 0.0193(14) 0.0178(13) 0.0007(11) 0.0024(11) 0.0002(11) C15 0.0195(14) 0.0258(15) 0.0163(13) 0.0010(11) 0.0004(11) -0.0027(11) C16 0.0259(15) 0.0191(14) 0.0260(15) -0.0032(12) 0.0040(12) -0.0004(12) C17 0.030(3) 0.029(3) 0.024(2) -0.003(2) 0.0015(19) 0.008(2) C18 0.051(2) 0.0313(19) 0.040(2) -0.0007(16) -0.0104(17) 0.0185(17) C19 0.092(7) 0.051(5) 0.049(4) -0.006(3) -0.030(4) 0.025(5) C20 0.121(5) 0.064(3) 0.035(2) 0.002(2) -0.017(3) 0.053(3) C21 0.0232(15) 0.0283(15) 0.0190(14) 0.0018(12) 0.0033(12) -0.0040(12) C22 0.0208(15) 0.0204(14) 0.0232(15) 0.0001(12) 0.0031(11) -0.0020(11) C23 0.0224(15) 0.0263(15) 0.0247(15) -0.0043(13) 0.0044(12) -0.0042(12) C24 0.0215(15) 0.0248(15) 0.0281(16) -0.0028(13) 0.0058(12) -0.0010(12) C25 0.0220(16) 0.041(2) 0.040(2) -0.0143(16) 0.0083(14) -0.0042(14) C26 0.033(2) 0.081(3) 0.056(3) -0.037(2) 0.0186(19) -0.005(2) C27 0.032(2) 0.056(3) 0.064(3) -0.014(2) 0.0067(18) 0.0142(18) C28 0.037(2) 0.063(3) 0.055(3) -0.014(2) 0.0245(19) -0.0151(19) C29 0.0204(15) 0.0249(15) 0.0268(16) -0.0020(13) 0.0001(12) -0.0009(12) C30 0.0223(15) 0.0208(14) 0.0233(15) 0.0013(12) -0.0009(11) -0.0001(11) C31 0.0241(16) 0.0356(18) 0.0239(15) -0.0065(14) -0.0001(12) -0.0044(13) C32 0.0274(18) 0.049(2) 0.0321(18) -0.0131(16) -0.0037(14) -0.0061(15) C33 0.0310(18) 0.0369(19) 0.040(2) -0.0183(16) 0.0015(15) -0.0024(15) C34 0.041(2) 0.060(3) 0.0269(18) 0.0073(18) -0.0008(15) -0.0030(18) C35 0.0209(14) 0.0181(14) 0.0238(15) -0.0007(11) 0.0040(11) -0.0011(11) C36 0.0279(17) 0.0186(15) 0.045(2) -0.0001(14) 0.0075(14) -0.0004(12) C37 0.0347(19) 0.0246(16) 0.046(2) 0.0037(15) 0.0114(16) 0.0046(14) C38 0.0267(17) 0.0363(19) 0.042(2) 0.0089(16) 0.0089(14) 0.0053(14) C39 0.0150(15) 0.0326(18) 0.052(2) -0.0012(16) 0.0068(14) -0.0015(13) C40 0.082(4) 0.049(3) 0.089(4) 0.014(3) -0.013(3) 0.007(3) C41 0.044(4) 0.030(4) 0.038(4) 0.005(3) -0.003(3) 0.006(3) C42 0.039(2) 0.0210(18) 0.079(3) 0.008(2) -0.020(2) -0.0038(16) C43 0.060(5) 0.023(3) 0.038(4) 0.001(3) -0.012(4) 0.006(3) C44 0.041(5) 0.045(5) 0.105(9) 0.040(6) 0.015(5) 0.010(4) C17A 0.028(5) 0.015(4) 0.027(5) -0.005(3) -0.001(4) 0.002(3) C19A 0.084(11) 0.028(6) 0.052(8) 0.007(6) 0.009(8) 0.006(7) _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 O1 1.911(2) . ? Cr1 O3 1.937(2) . ? Cr1 O2 2.020(2) . ? Cr1 O4 2.048(2) . ? Cr1 N1 2.124(3) . ? Cr1 Cl1 2.3394(9) . ? O1 C1 1.334(3) . ? O2 C20 1.418(5) . ? O2 C17 1.488(5) . ? O2 C17A 1.552(9) . ? O3 C35 1.335(3) . ? O4 C39 1.473(4) . ? O4 C36 1.481(4) . ? N1 C21 1.500(4) . ? N1 C15 1.503(4) . ? N1 C16 1.505(4) . ? C1 C14 1.405(4) . ? C1 C2 1.419(4) . ? C2 C7 1.387(4) . ? C2 C3 1.542(4) . ? C3 C4 1.527(5) . ? C3 C6 1.531(5) . ? C3 C5 1.535(5) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.400(4) . ? C7 H10 0.9500 . ? C8 C13 1.387(4) . ? C8 C9 1.541(4) . ? C9 C11 1.532(5) . ? C9 C10 1.532(5) . ? C9 C12 1.532(5) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.398(4) . ? C13 H20 0.9500 . ? C14 C15 1.503(4) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17A 1.481(10) . ? C16 C17 1.535(6) . ? C16 H23 0.8647 . ? C16 H24 0.9717 . ? C17 C17A 1.214(11) . ? C17 C18 1.558(6) . ? C18 C19A 1.514(15) . ? C18 C19 1.531(8) . ? C18 C17A 1.606(9) . ? C19 C19A 1.025(17) . ? C19 C20 1.481(9) . ? C20 C19A 1.571(14) . ? C21 C22 1.498(4) . ? C21 H25 0.9900 . ? C21 H26 0.9900 . ? C22 C23 1.398(4) . ? C22 C35 1.400(4) . ? C23 C24 1.390(4) . ? C23 H27 0.9500 . ? C24 C29 1.396(4) . ? C24 C25 1.536(4) . ? C25 C26 1.530(5) . ? C25 C27 1.537(6) . ? C25 C28 1.537(5) . ? C26 H28 0.9800 . ? C26 H29 0.9800 . ? C26 H30 0.9800 . ? C27 H31 0.9800 . ? C27 H32 0.9800 . ? C27 H33 0.9800 . ? C28 H34 0.9800 . ? C28 H35 0.9800 . ? C28 H36 0.9800 . ? C29 C30 1.395(4) . ? C29 H37 0.9500 . ? C30 C35 1.414(4) . ? C30 C31 1.535(4) . ? C31 C34 1.532(5) . ? C31 C32 1.532(5) . ? C31 C33 1.545(5) . ? C32 H38 0.9800 . ? C32 H39 0.9800 . ? C32 H40 0.9800 . ? C33 H41 0.9800 . ? C33 H42 0.9800 . ? C33 H43 0.9800 . ? C34 H44 0.9800 . ? C34 H45 0.9800 . ? C34 H46 0.9800 . ? C36 C37 1.502(5) . ? C36 H47 0.9900 . ? C36 H48 0.9900 . ? C37 C38 1.514(5) . ? C37 H49 0.9900 . ? C37 H50 0.9900 . ? C38 C39 1.507(5) . ? C38 H51 0.9900 . ? C38 H52 0.9900 . ? C39 H53 0.9900 . ? C39 H54 0.9900 . ? C40 C43 1.298(10) 3_667 ? C40 C44 1.520(14) 3_667 ? C40 C41 1.523(10) . ? C41 C42 1.233(9) . ? C41 C43 1.281(11) 3_667 ? C42 C44 1.236(13) . ? C42 C43 1.464(9) . ? C42 C43 1.499(10) 3_667 ? C43 C44 1.240(13) . ? C43 C41 1.281(11) 3_667 ? C43 C40 1.298(10) 3_667 ? C43 C42 1.498(10) 3_667 ? C43 C43 1.732(17) 3_667 ? C44 C40 1.520(14) 3_667 ? C17A C19A 1.974(17) . ? C17A H23 1.4194 . ? 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 O1 Cr1 O3 176.39(10) . . ? O1 Cr1 O2 92.19(11) . . ? O3 Cr1 O2 90.99(10) . . ? O1 Cr1 O4 89.90(9) . . ? O3 Cr1 O4 86.81(9) . . ? O2 Cr1 O4 175.51(9) . . ? O1 Cr1 N1 88.14(9) . . ? O3 Cr1 N1 90.70(9) . . ? O2 Cr1 N1 80.33(9) . . ? O4 Cr1 N1 95.78(9) . . ? O1 Cr1 Cl1 88.88(7) . . ? O3 Cr1 Cl1 92.65(7) . . ? O2 Cr1 Cl1 93.22(7) . . ? O4 Cr1 Cl1 90.79(7) . . ? N1 Cr1 Cl1 172.78(7) . . ? C1 O1 Cr1 135.19(18) . . ? C20 O2 C17 109.6(3) . . ? C20 O2 C17A 101.8(4) . . ? C17 O2 C17A 47.0(4) . . ? C20 O2 Cr1 132.5(3) . . ? C17 O2 Cr1 117.9(2) . . ? C17A O2 Cr1 108.2(3) . . ? C35 O3 Cr1 125.33(18) . . ? C39 O4 C36 108.1(2) . . ? C39 O4 Cr1 119.33(19) . . ? C36 O4 Cr1 119.24(18) . . ? C21 N1 C15 106.7(2) . . ? C21 N1 C16 110.7(2) . . ? C15 N1 C16 109.7(2) . . ? C21 N1 Cr1 110.00(18) . . ? C15 N1 Cr1 110.53(17) . . ? C16 N1 Cr1 109.26(18) . . ? O1 C1 C14 121.1(3) . . ? O1 C1 C2 119.7(3) . . ? C14 C1 C2 119.2(3) . . ? C7 C2 C1 117.6(3) . . ? C7 C2 C3 121.8(3) . . ? C1 C2 C3 120.5(3) . . ? C4 C3 C6 108.9(3) . . ? C4 C3 C5 108.7(3) . . ? C6 C3 C5 107.1(3) . . ? C4 C3 C2 110.6(3) . . ? C6 C3 C2 110.6(3) . . ? C5 C3 C2 110.9(3) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 124.3(3) . . ? C2 C7 H10 117.8 . . ? C8 C7 H10 117.8 . . ? C13 C8 C7 116.8(3) . . ? C13 C8 C9 123.3(3) . . ? C7 C8 C9 119.8(3) . . ? C11 C9 C10 108.5(3) . . ? C11 C9 C12 109.0(3) . . ? C10 C9 C12 108.2(3) . . ? C11 C9 C8 109.5(3) . . ? C10 C9 C8 111.8(3) . . ? C12 C9 C8 109.8(3) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 121.4(3) . . ? C8 C13 H20 119.3 . . ? C14 C13 H20 119.3 . . ? C13 C14 C1 120.6(3) . . ? C13 C14 C15 118.1(3) . . ? C1 C14 C15 121.3(3) . . ? C14 C15 N1 114.6(2) . . ? C14 C15 H21 108.6 . . ? N1 C15 H21 108.6 . . ? C14 C15 H22 108.6 . . ? N1 C15 H22 108.6 . . ? H21 C15 H22 107.6 . . ? C17A C16 N1 113.6(4) . . ? C17A C16 C17 47.4(4) . . ? N1 C16 C17 111.5(3) . . ? C17A C16 H23 68.8 . . ? N1 C16 H23 111.3 . . ? C17 C16 H23 112.8 . . ? C17A C16 H24 133.5 . . ? N1 C16 H24 111.2 . . ? C17 C16 H24 103.8 . . ? H23 C16 H24 105.9 . . ? C17A C17 O2 69.2(5) . . ? C17A C17 C16 64.0(5) . . ? O2 C17 C16 103.9(3) . . ? C17A C17 C18 69.5(5) . . ? O2 C17 C18 102.3(3) . . ? C16 C17 C18 112.3(4) . . ? C19A C18 C19 39.4(7) . . ? C19A C18 C17 104.9(6) . . ? C19 C18 C17 101.8(4) . . ? C19A C18 C17A 78.4(7) . . ? C19 C18 C17A 102.9(5) . . ? C17 C18 C17A 45.1(4) . . ? C19A C19 C20 75.2(10) . . ? C19A C19 C18 69.4(9) . . ? C20 C19 C18 104.9(5) . . ? O2 C20 C19 108.8(5) . . ? O2 C20 C19A 98.6(6) . . ? C19 C20 C19A 39.1(6) . . ? C22 C21 N1 113.1(2) . . ? C22 C21 H25 109.0 . . ? N1 C21 H25 109.0 . . ? C22 C21 H26 109.0 . . ? N1 C21 H26 109.0 . . ? H25 C21 H26 107.8 . . ? C23 C22 C35 121.1(3) . . ? C23 C22 C21 120.9(3) . . ? C35 C22 C21 118.0(3) . . ? C24 C23 C22 120.8(3) . . ? C24 C23 H27 119.6 . . ? C22 C23 H27 119.6 . . ? C23 C24 C29 116.9(3) . . ? C23 C24 C25 123.8(3) . . ? C29 C24 C25 119.3(3) . . ? C26 C25 C24 111.9(3) . . ? C26 C25 C27 108.9(3) . . ? C24 C25 C27 109.1(3) . . ? C26 C25 C28 108.7(3) . . ? C24 C25 C28 109.2(3) . . ? C27 C25 C28 109.1(3) . . ? C25 C26 H28 109.5 . . ? C25 C26 H29 109.5 . . ? H28 C26 H29 109.5 . . ? C25 C26 H30 109.5 . . ? H28 C26 H30 109.5 . . ? H29 C26 H30 109.5 . . ? C25 C27 H31 109.5 . . ? C25 C27 H32 109.5 . . ? H31 C27 H32 109.5 . . ? C25 C27 H33 109.5 . . ? H31 C27 H33 109.5 . . ? H32 C27 H33 109.5 . . ? C25 C28 H34 109.5 . . ? C25 C28 H35 109.5 . . ? H34 C28 H35 109.5 . . ? C25 C28 H36 109.5 . . ? H34 C28 H36 109.5 . . ? H35 C28 H36 109.5 . . ? C30 C29 C24 124.3(3) . . ? C30 C29 H37 117.9 . . ? C24 C29 H37 117.9 . . ? C29 C30 C35 117.4(3) . . ? C29 C30 C31 120.7(3) . . ? C35 C30 C31 121.9(3) . . ? C34 C31 C32 108.5(3) . . ? C34 C31 C30 109.8(3) . . ? C32 C31 C30 111.8(3) . . ? C34 C31 C33 109.3(3) . . ? C32 C31 C33 107.2(3) . . ? C30 C31 C33 110.1(3) . . ? C31 C32 H38 109.5 . . ? C31 C32 H39 109.5 . . ? H38 C32 H39 109.5 . . ? C31 C32 H40 109.5 . . ? H38 C32 H40 109.5 . . ? H39 C32 H40 109.5 . . ? C31 C33 H41 109.5 . . ? C31 C33 H42 109.5 . . ? H41 C33 H42 109.5 . . ? C31 C33 H43 109.5 . . ? H41 C33 H43 109.5 . . ? H42 C33 H43 109.5 . . ? C31 C34 H44 109.5 . . ? C31 C34 H45 109.5 . . ? H44 C34 H45 109.5 . . ? C31 C34 H46 109.5 . . ? H44 C34 H46 109.5 . . ? H45 C34 H46 109.5 . . ? O3 C35 C22 119.2(3) . . ? O3 C35 C30 121.7(3) . . ? C22 C35 C30 119.1(3) . . ? O4 C36 C37 105.6(3) . . ? O4 C36 H47 110.6 . . ? C37 C36 H47 110.6 . . ? O4 C36 H48 110.6 . . ? C37 C36 H48 110.6 . . ? H47 C36 H48 108.8 . . ? C36 C37 C38 103.5(3) . . ? C36 C37 H49 111.1 . . ? C38 C37 H49 111.1 . . ? C36 C37 H50 111.1 . . ? C38 C37 H50 111.1 . . ? H49 C37 H50 109.0 . . ? C39 C38 C37 101.9(3) . . ? C39 C38 H51 111.4 . . ? C37 C38 H51 111.4 . . ? C39 C38 H52 111.4 . . ? C37 C38 H52 111.4 . . ? H51 C38 H52 109.3 . . ? O4 C39 C38 104.6(3) . . ? O4 C39 H53 110.8 . . ? C38 C39 H53 110.8 . . ? O4 C39 H54 110.8 . . ? C38 C39 H54 110.8 . . ? H53 C39 H54 108.9 . . ? C43 C40 C44 51.5(6) 3_667 3_667 ? C43 C40 C41 53.3(5) 3_667 . ? C44 C40 C41 104.7(7) 3_667 . ? C42 C41 C43 73.1(6) . 3_667 ? C42 C41 C40 127.4(7) . . ? C43 C41 C40 54.3(5) 3_667 . ? C41 C42 C44 178.8(7) . . ? C41 C42 C43 126.4(6) . . ? C44 C42 C43 53.9(6) . . ? C41 C42 C43 54.9(5) . 3_667 ? C44 C42 C43 125.4(7) . 3_667 ? C43 C42 C43 71.6(6) . 3_667 ? C44 C43 C41 145.9(11) . 3_667 ? C44 C43 C40 73.5(9) . 3_667 ? C41 C43 C40 72.4(6) 3_667 3_667 ? C44 C43 C42 53.6(7) . . ? C41 C43 C42 160.4(9) 3_667 . ? C40 C43 C42 127.2(8) 3_667 . ? C44 C43 C42 161.9(9) . 3_667 ? C41 C43 C42 52.0(5) 3_667 3_667 ? C40 C43 C42 124.4(7) 3_667 3_667 ? C42 C43 C42 108.4(6) . 3_667 ? C44 C43 C43 108.7(10) . 3_667 ? C41 C43 C43 105.2(9) 3_667 3_667 ? C40 C43 C43 177.3(9) 3_667 3_667 ? C42 C43 C43 55.2(5) . 3_667 ? C42 C43 C43 53.3(5) 3_667 3_667 ? C42 C44 C43 72.5(7) . . ? C42 C44 C40 127.4(8) . 3_667 ? C43 C44 C40 55.0(6) . 3_667 ? C17 C17A C16 68.6(5) . . ? C17 C17A O2 63.7(5) . . ? C16 C17A O2 103.5(5) . . ? C17 C17A C18 65.4(5) . . ? C16 C17A C18 112.6(6) . . ? O2 C17A C18 97.4(5) . . ? C17 C17A C19A 96.7(8) . . ? C16 C17A C19A 161.0(8) . . ? O2 C17A C19A 79.1(6) . . ? C18 C17A C19A 48.7(5) . . ? C17 C17A H23 100.8 . . ? C16 C17A H23 34.6 . . ? O2 C17A H23 131.5 . . ? C18 C17A H23 118.1 . . ? C19A C17A H23 149.1 . . ? C19 C19A C18 71.2(10) . . ? C19 C19A C20 65.7(9) . . ? C18 C19A C20 101.5(8) . . ? C19 C19A C17A 105.4(11) . . ? C18 C19A C17A 52.8(5) . . ? C20 C19A C17A 80.3(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.725 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.082 #===END data_cmpd_5 _database_code_depnum_ccdc_archive 'CCDC 733958' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C48 H54 Cl2 Cr2 N4 O5, C7 H8' _chemical_formula_sum 'C55 H62 Cl2 Cr2 N4 O5' _exptl_crystal_recrystallization_method 'CHLOROFORM, TOLUENE' _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Green _diffrn_ambient_temperature 198(1) _chemical_formula_weight 1033.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_space_group_name_Hall '-P 2yac' _symmetry_int_tables_number 13 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 14.222(3) _cell_length_b 13.867(3) _cell_length_c 14.612(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.533(3) _cell_angle_gamma 90.00 _cell_volume 2732.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used 5572 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.24 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8119 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18165 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6028 _reflns_number_gt 3105 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.1469P)^2^] 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 6028 _refine_ls_number_parameters 335 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2609 _refine_ls_wR_factor_gt 0.2174 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.045 _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 0.33955(6) 0.52448(6) 0.17950(5) 0.0414(3) Uani 1 1 d . . . Cl1 Cl 0.21637(10) 0.53941(10) 0.02826(8) 0.0532(4) Uani 1 1 d . . . O1 O 0.3645(2) 0.3939(2) 0.1540(2) 0.0435(8) Uani 1 1 d . . . O2 O 0.3155(3) 0.6597(2) 0.2152(2) 0.0508(9) Uani 1 1 d . . . O3 O 0.2500 0.4799(3) 0.2500 0.0416(11) Uani 1 2 d S . . N1 N 0.4658(3) 0.5134(3) 0.3018(3) 0.0418(10) Uani 1 1 d . . . N2 N 0.4476(3) 0.5728(3) 0.1223(3) 0.0467(11) Uani 1 1 d . . . C1 C 0.3928(4) 0.7250(4) 0.2441(3) 0.0505(13) Uani 1 1 d . . . C2 C 0.3839(5) 0.8146(4) 0.2003(4) 0.0621(16) Uani 1 1 d . . . C3 C 0.4669(5) 0.8751(4) 0.2284(4) 0.0683(17) Uani 1 1 d . . . H3 H 0.4628 0.9369 0.1994 0.082 Uiso 1 1 calc R . . C4 C 0.5546(5) 0.8479(5) 0.2971(4) 0.0686(18) Uani 1 1 d . . . C5 C 0.5606(5) 0.7584(4) 0.3390(4) 0.0616(16) Uani 1 1 d . . . H5 H 0.6205 0.7391 0.3864 0.074 Uiso 1 1 calc R . . C6 C 0.4800(4) 0.6958(4) 0.3130(3) 0.0528(14) Uani 1 1 d . . . C7 C 0.2882(5) 0.8441(5) 0.1259(5) 0.077(2) Uani 1 1 d . . . H7A H 0.2647 0.7918 0.0791 0.115 Uiso 1 1 calc R . . H7B H 0.2992 0.9022 0.0925 0.115 Uiso 1 1 calc R . . H7C H 0.2384 0.8575 0.1577 0.115 Uiso 1 1 calc R . . C8 C 0.6424(6) 0.9161(6) 0.3233(6) 0.096(2) Uani 1 1 d . . . H8A H 0.6540 0.9406 0.3889 0.144 Uiso 1 1 calc R . . H8B H 0.6286 0.9701 0.2778 0.144 Uiso 1 1 calc R . . H8C H 0.7015 0.8815 0.3203 0.144 Uiso 1 1 calc R . . C9 C 0.3841(3) 0.3213(4) 0.2174(3) 0.0401(11) Uani 1 1 d . . . C10 C 0.3523(4) 0.2286(4) 0.1832(4) 0.0488(13) Uani 1 1 d . . . C11 C 0.3741(5) 0.1524(4) 0.2463(4) 0.0605(15) Uani 1 1 d . . . H11 H 0.3522 0.0899 0.2223 0.073 Uiso 1 1 calc R . . C12 C 0.4269(5) 0.1627(4) 0.3442(4) 0.0600(16) Uani 1 1 d . . . C13 C 0.4547(4) 0.2537(4) 0.3767(3) 0.0493(13) Uani 1 1 d . . . H13 H 0.4902 0.2627 0.4432 0.059 Uiso 1 1 calc R . . C14 C 0.4335(4) 0.3340(4) 0.3166(3) 0.0414(12) Uani 1 1 d . . . C15 C 0.2927(5) 0.2146(4) 0.0792(4) 0.0613(16) Uani 1 1 d . . . H15A H 0.3363 0.2192 0.0393 0.092 Uiso 1 1 calc R . . H15B H 0.2415 0.2646 0.0596 0.092 Uiso 1 1 calc R . . H15C H 0.2612 0.1509 0.0706 0.092 Uiso 1 1 calc R . . C16 C 0.4499(6) 0.0772(5) 0.4110(5) 0.093(3) Uani 1 1 d . . . H16A H 0.5189 0.0576 0.4230 0.140 Uiso 1 1 calc R . . H16B H 0.4057 0.0237 0.3814 0.140 Uiso 1 1 calc R . . H16C H 0.4400 0.0947 0.4723 0.140 Uiso 1 1 calc R . . C17 C 0.4585(4) 0.4297(4) 0.3652(3) 0.0448(12) Uani 1 1 d . . . H17A H 0.5227 0.4236 0.4175 0.054 Uiso 1 1 calc R . . H17B H 0.4075 0.4454 0.3959 0.054 Uiso 1 1 calc R . . C18 C 0.4821(4) 0.6016(4) 0.3640(3) 0.0500(13) Uani 1 1 d . . . H18A H 0.5471 0.5955 0.4151 0.060 Uiso 1 1 calc R . . H18B H 0.4305 0.6034 0.3963 0.060 Uiso 1 1 calc R . . C19 C 0.5518(4) 0.4949(4) 0.2663(3) 0.0514(14) Uani 1 1 d . . . H19A H 0.5566 0.4248 0.2555 0.062 Uiso 1 1 calc R . . H19B H 0.6138 0.5152 0.3163 0.062 Uiso 1 1 calc R . . C20 C 0.5422(4) 0.5476(4) 0.1745(3) 0.0499(14) Uani 1 1 d . . . C21 C 0.6215(4) 0.5626(5) 0.1421(4) 0.0610(16) Uani 1 1 d . . . H21 H 0.6861 0.5426 0.1798 0.073 Uiso 1 1 calc R . . C22 C 0.6058(5) 0.6079(5) 0.0525(4) 0.0628(17) Uani 1 1 d . . . H22 H 0.6591 0.6181 0.0275 0.075 Uiso 1 1 calc R . . C23 C 0.5108(5) 0.6372(4) 0.0018(4) 0.0618(16) Uani 1 1 d . . . H23 H 0.4986 0.6701 -0.0579 0.074 Uiso 1 1 calc R . . C24 C 0.4333(4) 0.6191(4) 0.0374(3) 0.0540(14) Uani 1 1 d . . . H24 H 0.3683 0.6397 0.0013 0.065 Uiso 1 1 calc R . . C25 C 0.3421(7) 0.8364(8) 0.8420(7) 0.064(3) Uani 0.50 1 d PD . . C26 C 0.2536(8) 0.8077(8) 0.8550(8) 0.076(4) Uani 0.50 1 d PD . . C27 C 0.1966(5) 0.7344(6) 0.7993(5) 0.086(2) Uani 1 1 d D . . C28 C 0.2177(7) 0.7029(11) 0.7177(7) 0.094(5) Uani 0.50 1 d PD . . C29 C 0.3664(8) 0.7986(8) 0.7644(7) 0.069(3) Uani 0.50 1 d PD . . C30 C 0.4096(12) 0.9103(10) 0.9094(9) 0.089(5) Uani 0.50 1 d P . . H30A H 0.3754 0.9725 0.9024 0.134 Uiso 0.50 1 calc PR . . H30B H 0.4707 0.9176 0.8926 0.134 Uiso 0.50 1 calc PR . . H30C H 0.4260 0.8880 0.9763 0.134 Uiso 0.50 1 calc PR . . 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 0.0554(6) 0.0450(5) 0.0151(4) 0.0037(3) -0.0012(3) -0.0048(4) Cl1 0.0622(9) 0.0647(9) 0.0200(6) 0.0070(5) -0.0047(5) -0.0037(7) O1 0.058(2) 0.049(2) 0.0181(15) 0.0021(14) 0.0036(14) -0.0030(16) O2 0.070(2) 0.040(2) 0.0308(18) 0.0032(15) -0.0002(16) -0.0051(17) O3 0.053(3) 0.047(3) 0.016(2) 0.000 -0.0007(19) 0.000 N1 0.053(3) 0.046(2) 0.0202(19) 0.0080(17) 0.0023(17) -0.0057(19) N2 0.067(3) 0.047(3) 0.0177(18) 0.0026(17) 0.0022(18) -0.012(2) C1 0.071(4) 0.044(3) 0.030(3) -0.002(2) 0.005(2) -0.012(3) C2 0.092(5) 0.048(3) 0.042(3) -0.002(3) 0.014(3) -0.005(3) C3 0.103(5) 0.047(3) 0.057(4) 0.002(3) 0.029(4) -0.012(3) C4 0.093(5) 0.066(4) 0.045(3) -0.006(3) 0.018(3) -0.022(4) C5 0.077(4) 0.069(4) 0.034(3) -0.007(3) 0.010(3) -0.023(3) C6 0.074(4) 0.055(3) 0.023(2) -0.006(2) 0.007(2) -0.015(3) C7 0.110(6) 0.051(4) 0.055(4) 0.016(3) 0.007(4) 0.004(4) C8 0.105(6) 0.087(6) 0.093(6) -0.006(4) 0.027(5) -0.040(5) C9 0.046(3) 0.046(3) 0.027(2) 0.006(2) 0.009(2) 0.002(2) C10 0.058(3) 0.053(3) 0.038(3) 0.003(2) 0.018(2) 0.002(3) C11 0.089(4) 0.047(3) 0.052(4) 0.005(3) 0.033(3) 0.006(3) C12 0.087(4) 0.052(4) 0.045(3) 0.018(3) 0.028(3) 0.019(3) C13 0.064(4) 0.056(4) 0.028(3) 0.012(2) 0.016(2) 0.016(3) C14 0.044(3) 0.056(3) 0.023(2) 0.007(2) 0.009(2) 0.007(2) C15 0.090(4) 0.054(4) 0.038(3) -0.008(3) 0.017(3) -0.014(3) C16 0.159(8) 0.058(4) 0.065(4) 0.024(4) 0.040(5) 0.030(5) C17 0.050(3) 0.056(3) 0.019(2) 0.008(2) -0.001(2) -0.006(2) C18 0.059(3) 0.060(3) 0.019(2) -0.003(2) -0.004(2) -0.011(3) C19 0.053(3) 0.072(4) 0.022(2) 0.008(2) 0.002(2) -0.011(3) C20 0.063(4) 0.058(3) 0.020(2) 0.003(2) 0.001(2) -0.020(3) C21 0.059(4) 0.088(4) 0.030(3) 0.004(3) 0.005(2) -0.022(3) C22 0.078(4) 0.078(4) 0.027(3) -0.003(3) 0.010(3) -0.029(3) C23 0.091(5) 0.060(4) 0.028(3) 0.004(3) 0.011(3) -0.024(3) C24 0.078(4) 0.056(3) 0.020(2) 0.005(2) 0.004(2) -0.011(3) C25 0.064(8) 0.061(8) 0.061(8) 0.024(6) 0.014(6) 0.007(6) C26 0.107(11) 0.078(9) 0.051(8) 0.003(7) 0.036(7) -0.009(8) C27 0.087(5) 0.106(6) 0.069(5) -0.019(5) 0.032(4) -0.034(5) C28 0.110(14) 0.106(12) 0.051(9) -0.006(8) 0.003(7) -0.014(10) C29 0.065(8) 0.069(9) 0.069(9) 0.019(7) 0.016(7) 0.022(7) C30 0.133(12) 0.079(10) 0.044(7) 0.006(7) 0.011(7) -0.059(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.905(3) . ? Cr1 O3 1.9745(16) . ? Cr1 O2 2.004(4) . ? Cr1 N2 2.080(4) . ? Cr1 N1 2.098(4) . ? Cr1 Cl1 2.3526(14) . ? O1 C9 1.337(5) . ? O2 C1 1.383(6) . ? O3 Cr1 1.9745(16) 2 ? N1 C19 1.494(6) . ? N1 C18 1.498(6) . ? N1 C17 1.510(6) . ? N2 C24 1.354(6) . ? N2 C20 1.364(7) . ? C1 C2 1.384(8) . ? C1 C6 1.387(7) . ? C2 C3 1.399(8) . ? C2 C7 1.504(8) . ? C3 C4 1.381(9) . ? C3 H3 0.9500 . ? C4 C5 1.375(8) . ? C4 C8 1.514(9) . ? C5 C6 1.391(7) . ? C5 H5 0.9500 . ? C6 C18 1.500(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.402(7) . ? C9 C14 1.407(6) . ? C10 C11 1.370(7) . ? C10 C15 1.500(7) . ? C11 C12 1.396(8) . ? C11 H11 0.9500 . ? C12 C13 1.362(8) . ? C12 C16 1.504(8) . ? C13 C14 1.390(7) . ? C13 H13 0.9500 . ? C14 C17 1.494(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.495(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.369(8) . ? C21 C22 1.406(7) . ? C21 H21 0.9500 . ? C22 C23 1.380(8) . ? C22 H22 0.9500 . ? C23 C24 1.383(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C29 1.3900(10) . ? C25 C26 1.3900(11) . ? C25 C30 1.529(15) . ? C26 C27 1.3901(10) . ? C27 C29 1.3896(10) 2_556 ? C27 C28 1.3900(11) . ? C27 C28 1.3902(11) 2_556 ? C28 C27 1.3902(11) 2_556 ? C29 C27 1.3896(10) 2_556 ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 O1 Cr1 O3 89.77(16) . . ? O1 Cr1 O2 176.38(13) . . ? O3 Cr1 O2 88.00(17) . . ? O1 Cr1 N2 91.14(16) . . ? O3 Cr1 N2 172.72(11) . . ? O2 Cr1 N2 90.71(16) . . ? O1 Cr1 N1 86.27(15) . . ? O3 Cr1 N1 93.00(11) . . ? O2 Cr1 N1 91.00(15) . . ? N2 Cr1 N1 79.85(15) . . ? O1 Cr1 Cl1 91.67(10) . . ? O3 Cr1 Cl1 96.11(5) . . ? O2 Cr1 Cl1 91.40(10) . . ? N2 Cr1 Cl1 91.08(12) . . ? N1 Cr1 Cl1 170.65(12) . . ? C9 O1 Cr1 126.2(3) . . ? C1 O2 Cr1 120.5(3) . . ? Cr1 O3 Cr1 143.5(3) 2 . ? C19 N1 C18 111.5(4) . . ? C19 N1 C17 107.7(4) . . ? C18 N1 C17 106.4(4) . . ? C19 N1 Cr1 106.9(3) . . ? C18 N1 Cr1 112.5(3) . . ? C17 N1 Cr1 111.8(3) . . ? C24 N2 C20 117.9(4) . . ? C24 N2 Cr1 127.3(4) . . ? C20 N2 Cr1 114.6(3) . . ? O2 C1 C2 120.0(5) . . ? O2 C1 C6 118.1(5) . . ? C2 C1 C6 121.7(5) . . ? C1 C2 C3 117.3(6) . . ? C1 C2 C7 120.4(6) . . ? C3 C2 C7 122.3(6) . . ? C4 C3 C2 122.1(6) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 118.9(6) . . ? C5 C4 C8 121.4(7) . . ? C3 C4 C8 119.7(6) . . ? C4 C5 C6 120.9(6) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 119.1(5) . . ? C1 C6 C18 119.1(5) . . ? C5 C6 C18 121.6(5) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 C10 118.1(4) . . ? O1 C9 C14 123.1(4) . . ? C10 C9 C14 118.7(4) . . ? C11 C10 C9 119.3(5) . . ? C11 C10 C15 121.1(5) . . ? C9 C10 C15 119.6(5) . . ? C10 C11 C12 122.9(6) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 117.0(5) . . ? C13 C12 C16 121.6(6) . . ? C11 C12 C16 121.3(6) . . ? C12 C13 C14 122.7(5) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C13 C14 C9 119.2(5) . . ? C13 C14 C17 116.1(4) . . ? C9 C14 C17 124.5(4) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 N1 116.3(4) . . ? C14 C17 H17A 108.2 . . ? N1 C17 H17A 108.2 . . ? C14 C17 H17B 108.2 . . ? N1 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? N1 C18 C6 115.7(4) . . ? N1 C18 H18A 108.4 . . ? C6 C18 H18A 108.4 . . ? N1 C18 H18B 108.4 . . ? C6 C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? N1 C19 C20 112.1(4) . . ? N1 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N1 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N2 C20 C21 122.8(5) . . ? N2 C20 C19 114.8(4) . . ? C21 C20 C19 122.2(5) . . ? C20 C21 C22 119.1(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C23 C22 C21 118.0(5) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? N2 C24 C23 121.6(5) . . ? N2 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C29 C25 C26 118.3(10) . . ? C29 C25 C30 120.7(9) . . ? C26 C25 C30 121.0(9) . . ? C25 C26 C27 121.0(9) . . ? C25 C26 C29 116.9(8) . 2_556 ? C28 C27 C26 119.2(9) . . ? C29 C27 C28 119.8(9) 2_556 2_556 ? C27 C28 C27 119.7(9) . 2_556 ? C27 C28 C29 116.1(10) 2_556 2_556 ? C27 C29 C25 120.9(10) 2_556 . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.097 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.108 #===END data_cmpd_6 _database_code_depnum_ccdc_archive 'CCDC 733959' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '{[(C36 H50 O2 N2) Cr Cl][(C36 H51 O2 N2) Cr Cl](O H)}(C7 H8)2' _chemical_formula_sum 'C86 H118 Cl2 Cr2 N4 O5' _chemical_formula_weight 1462.80 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8636(18) _cell_length_b 16.1865(16) _cell_length_c 18.334(2) _cell_angle_alpha 71.836(7) _cell_angle_beta 78.206(9) _cell_angle_gamma 67.999(7) _cell_volume 4126.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 118(2) _cell_measurement_reflns_used 18023 _cell_measurement_theta_min 2.2726 _cell_measurement_theta_max 30.8311 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9622 _exptl_absorpt_correction_T_min 0.9230 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 118(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 71780 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.50 _reflns_number_total 17081 _reflns_number_gt 16418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1090P)^2^+4.7729P] 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 17081 _refine_ls_number_parameters 893 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1905 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _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 0.16614(3) 0.79883(3) 0.17480(2) 0.02110(11) Uani 1 1 d . . . Cr2 Cr 0.37710(2) 0.64609(3) 0.27789(2) 0.02043(11) Uani 1 1 d . . . Cl1 Cl 0.05992(4) 0.78743(5) 0.28395(3) 0.02826(15) Uani 1 1 d . . . Cl2 Cl 0.48440(4) 0.67027(4) 0.17272(3) 0.02758(14) Uani 1 1 d . . . O1 O 0.15016(12) 0.92038(12) 0.17582(10) 0.0265(4) Uani 1 1 d . . . O2 O 0.19439(11) 0.66579(12) 0.17340(9) 0.0229(3) Uani 1 1 d . . . O3 O 0.34023(12) 0.56946(12) 0.22783(10) 0.0239(3) Uani 1 1 d . . . H117 H 0.2838 0.6101 0.2089 0.029 Uiso 1 1 d . . . O4 O 0.40499(12) 0.71987(12) 0.32499(10) 0.0254(4) Uani 1 1 d . . . O5 O 0.27453(11) 0.75266(11) 0.23188(9) 0.0223(3) Uani 1 1 d . . . H118 H 0.2771 0.8032 0.2399 0.027 Uiso 1 1 d . . . N1 N 0.24262(14) 0.82326(14) 0.06620(11) 0.0224(4) Uani 1 1 d . . . N2 N 0.06327(14) 0.83989(15) 0.10235(12) 0.0250(4) Uani 1 1 d . . . N3 N 0.29364(14) 0.61247(14) 0.38066(11) 0.0216(4) Uani 1 1 d . . . N4 N 0.47243(14) 0.52677(15) 0.33828(12) 0.0246(4) Uani 1 1 d . . . C1 C 0.20208(17) 0.97416(17) 0.14619(14) 0.0255(5) Uani 1 1 d . . . C2 C 0.18186(18) 1.05329(18) 0.17293(15) 0.0284(5) Uani 1 1 d . . . C3 C 0.11242(19) 1.0688(2) 0.24348(16) 0.0339(6) Uani 1 1 d . . . C4 C 0.01651(19) 1.0828(2) 0.22579(17) 0.0357(6) Uani 1 1 d . . . H1 H -0.0150 1.1486 0.2040 0.043 Uiso 1 1 calc R . . H2 H -0.0185 1.0603 0.2735 0.043 Uiso 1 1 calc R . . H3 H 0.0220 1.0484 0.1886 0.043 Uiso 1 1 calc R . . C5 C 0.1396(2) 0.9847(2) 0.31331(16) 0.0413(7) Uani 1 1 d . . . H4 H 0.1110 0.9403 0.3139 0.050 Uiso 1 1 calc R . . H5 H 0.1189 1.0049 0.3610 0.050 Uiso 1 1 calc R . . H6 H 0.2062 0.9555 0.3094 0.050 Uiso 1 1 calc R . . C6 C 0.1064(2) 1.1537(2) 0.2671(2) 0.0473(8) Uani 1 1 d . . . H7 H 0.1505 1.1356 0.3044 0.057 Uiso 1 1 calc R . . H8 H 0.0445 1.1802 0.2907 0.057 Uiso 1 1 calc R . . H9 H 0.1201 1.1996 0.2214 0.057 Uiso 1 1 calc R . . C7 C 0.2274(2) 1.1155(2) 0.13369(17) 0.0347(6) Uani 1 1 d . . . H10 H 0.2135 1.1691 0.1509 0.042 Uiso 1 1 calc R . . C8 C 0.2926(2) 1.1036(2) 0.07042(18) 0.0361(6) Uani 1 1 d . . . C9 C 0.3399(3) 1.1749(2) 0.0260(2) 0.0527(9) Uani 1 1 d . . . C10 C 0.4368(3) 1.1378(3) 0.0426(6) 0.155(4) Uani 1 1 d . . . H11 H 0.4418 1.1553 0.0877 0.187 Uiso 1 1 calc R . . H12 H 0.4739 1.1632 -0.0021 0.187 Uiso 1 1 calc R . . H13 H 0.4588 1.0704 0.0531 0.187 Uiso 1 1 calc R . . C11 C 0.2951(3) 1.2655(3) 0.0482(3) 0.0781(15) Uani 1 1 d . . . H14 H 0.2470 1.3064 0.0147 0.094 Uiso 1 1 calc R . . H15 H 0.3410 1.2948 0.0424 0.094 Uiso 1 1 calc R . . H16 H 0.2685 1.2540 0.1020 0.094 Uiso 1 1 calc R . . C12 C 0.3279(7) 1.2012(5) -0.0597(3) 0.151(4) Uani 1 1 d . . . H17 H 0.3789 1.1596 -0.0853 0.182 Uiso 1 1 calc R . . H18 H 0.3269 1.2648 -0.0831 0.182 Uiso 1 1 calc R . . H19 H 0.2703 1.1959 -0.0658 0.182 Uiso 1 1 calc R . . C13 C 0.31618(19) 1.02159(19) 0.04951(17) 0.0320(6) Uani 1 1 d . . . H20 H 0.3624 1.0098 0.0084 0.038 Uiso 1 1 calc R . . C14 C 0.27361(17) 0.95625(18) 0.08748(15) 0.0259(5) Uani 1 1 d . . . C15 C 0.31155(17) 0.86502(17) 0.06636(14) 0.0252(5) Uani 1 1 d . . . H21 H 0.3454 0.8740 0.0144 0.030 Uiso 1 1 calc R . . H22 H 0.3560 0.8207 0.1032 0.030 Uiso 1 1 calc R . . C16 C 0.17718(17) 0.88807(17) 0.00880(14) 0.0260(5) Uani 1 1 d . . . H23 H 0.2040 0.8801 -0.0433 0.031 Uiso 1 1 calc R . . H24 H 0.1672 0.9523 0.0084 0.031 Uiso 1 1 calc R . . C17 C 0.08726(17) 0.87200(17) 0.02685(14) 0.0247(5) Uani 1 1 d . . . C18 C 0.03116(19) 0.89124(18) -0.02951(15) 0.0299(5) Uani 1 1 d . . . H25 H 0.0497 0.9139 -0.0824 0.036 Uiso 1 1 calc R . . C19 C -0.05218(19) 0.87705(19) -0.00775(16) 0.0325(6) Uani 1 1 d . . . H26 H -0.0912 0.8887 -0.0454 0.039 Uiso 1 1 calc R . . C20 C -0.07757(18) 0.8457(2) 0.06958(16) 0.0334(6) Uani 1 1 d . . . H27 H -0.1351 0.8369 0.0860 0.040 Uiso 1 1 calc R . . C21 C -0.01831(17) 0.8273(2) 0.12293(15) 0.0303(5) Uani 1 1 d . . . H28 H -0.0359 0.8049 0.1761 0.036 Uiso 1 1 calc R . . C22 C 0.29352(17) 0.73447(17) 0.04354(14) 0.0250(5) Uani 1 1 d . . . H29 H 0.3379 0.6937 0.0815 0.030 Uiso 1 1 calc R . . H30 H 0.3286 0.7479 -0.0074 0.030 Uiso 1 1 calc R . . C23 C 0.23281(17) 0.68412(17) 0.03917(14) 0.0245(5) Uani 1 1 d . . . C24 C 0.22678(18) 0.67088(17) -0.03064(14) 0.0272(5) Uani 1 1 d . . . H31 H 0.2590 0.6967 -0.0763 0.033 Uiso 1 1 calc R . . C25 C 0.17433(18) 0.62047(18) -0.03473(15) 0.0282(5) Uani 1 1 d . . . C26 C 0.1654(2) 0.6040(2) -0.11042(16) 0.0343(6) Uani 1 1 d . . . C27 C 0.2000(2) 0.6674(2) -0.18079(17) 0.0435(7) Uani 1 1 d . . . H32 H 0.1496 0.7246 -0.1977 0.052 Uiso 1 1 calc R . . H33 H 0.2241 0.6365 -0.2226 0.052 Uiso 1 1 calc R . . H34 H 0.2486 0.6819 -0.1673 0.052 Uiso 1 1 calc R . . C28 C 0.0641(2) 0.6245(3) -0.11770(19) 0.0466(8) Uani 1 1 d . . . H35 H 0.0485 0.5681 -0.0941 0.056 Uiso 1 1 calc R . . H36 H 0.0535 0.6462 -0.1723 0.056 Uiso 1 1 calc R . . H37 H 0.0258 0.6721 -0.0913 0.056 Uiso 1 1 calc R . . C29 C 0.2185(3) 0.5032(2) -0.1099(2) 0.0599(10) Uani 1 1 d . . . H38 H 0.2816 0.4970 -0.1322 0.072 Uiso 1 1 calc R . . H39 H 0.1895 0.4833 -0.1405 0.072 Uiso 1 1 calc R . . H40 H 0.2186 0.4647 -0.0567 0.072 Uiso 1 1 calc R . . C30 C 0.12986(18) 0.58325(18) 0.03432(15) 0.0288(5) Uani 1 1 d . . . H41 H 0.0951 0.5474 0.0323 0.035 Uiso 1 1 calc R . . C31 C 0.13231(17) 0.59454(18) 0.10678(15) 0.0270(5) Uani 1 1 d . . . C32 C 0.07810(19) 0.5465(2) 0.17543(15) 0.0305(6) Uani 1 1 d . . . C33 C -0.0227(2) 0.5806(2) 0.15950(18) 0.0385(6) Uani 1 1 d . . . H42 H -0.0569 0.6350 0.1792 0.046 Uiso 1 1 calc R . . H43 H -0.0490 0.5316 0.1853 0.046 Uiso 1 1 calc R . . H44 H -0.0263 0.5969 0.1038 0.046 Uiso 1 1 calc R . . C34 C 0.1192(2) 0.4415(2) 0.18489(19) 0.0435(7) Uani 1 1 d . . . H45 H 0.0884 0.4238 0.1540 0.052 Uiso 1 1 calc R . . H46 H 0.1107 0.4091 0.2393 0.052 Uiso 1 1 calc R . . H47 H 0.1846 0.4247 0.1674 0.052 Uiso 1 1 calc R . . C35 C 0.0779(2) 0.5635(3) 0.25328(17) 0.0434(8) Uani 1 1 d . . . H48 H 0.1298 0.5159 0.2797 0.052 Uiso 1 1 calc R . . H49 H 0.0208 0.5609 0.2852 0.052 Uiso 1 1 calc R . . H50 H 0.0829 0.6244 0.2447 0.052 Uiso 1 1 calc R . . C36 C 0.18511(16) 0.64702(17) 0.10758(14) 0.0225(5) Uani 1 1 d . . . C37 C 0.33866(17) 0.48283(17) 0.27067(14) 0.0244(5) Uani 1 1 d . . . C38 C 0.38553(18) 0.40312(19) 0.24396(15) 0.0283(5) Uani 1 1 d . . . C39 C 0.44000(19) 0.40173(19) 0.16377(16) 0.0307(6) Uani 1 1 d . . . C40 C 0.5221(3) 0.4338(3) 0.1561(2) 0.0589(10) Uani 1 1 d . . . H51 H 0.5037 0.5008 0.1348 0.071 Uiso 1 1 calc R . . H52 H 0.5718 0.4036 0.1215 0.071 Uiso 1 1 calc R . . H53 H 0.5432 0.4173 0.2070 0.071 Uiso 1 1 calc R . . C41 C 0.3803(3) 0.4618(3) 0.1001(2) 0.0617(11) Uani 1 1 d . . . H54 H 0.3521 0.4252 0.0860 0.074 Uiso 1 1 calc R . . H55 H 0.4174 0.4865 0.0551 0.074 Uiso 1 1 calc R . . H56 H 0.3324 0.5129 0.1178 0.074 Uiso 1 1 calc R . . C42 C 0.4808(3) 0.3043(3) 0.1513(2) 0.0617(11) Uani 1 1 d . . . H57 H 0.5419 0.2743 0.1690 0.074 Uiso 1 1 calc R . . H58 H 0.4849 0.3084 0.0962 0.074 Uiso 1 1 calc R . . H59 H 0.4415 0.2681 0.1805 0.074 Uiso 1 1 calc R . . C43 C 0.3795(2) 0.32052(19) 0.29474(16) 0.0316(6) Uani 1 1 d . . . H60 H 0.4104 0.2656 0.2783 0.038 Uiso 1 1 calc R . . C44 C 0.3312(2) 0.31274(18) 0.36827(15) 0.0304(5) Uani 1 1 d . . . C45 C 0.3292(2) 0.2176(2) 0.41814(17) 0.0385(7) Uani 1 1 d . . . C46 C 0.2829(3) 0.1805(2) 0.3757(2) 0.0484(8) Uani 1 1 d . . . H61 H 0.2170 0.2002 0.3909 0.058 Uiso 1 1 calc R . . H62 H 0.3080 0.1130 0.3892 0.058 Uiso 1 1 calc R . . H63 H 0.2943 0.2047 0.3199 0.058 Uiso 1 1 calc R . . C47 C 0.4282(3) 0.1518(2) 0.4291(2) 0.0511(8) Uani 1 1 d . . . H64 H 0.4510 0.1204 0.3875 0.061 Uiso 1 1 calc R . . H65 H 0.4294 0.1059 0.4789 0.061 Uiso 1 1 calc R . . H66 H 0.4671 0.1872 0.4278 0.061 Uiso 1 1 calc R . . C48 C 0.2771(3) 0.2221(2) 0.49732(19) 0.0495(8) Uani 1 1 d . . . H67 H 0.3194 0.2130 0.5335 0.059 Uiso 1 1 calc R . . H68 H 0.2491 0.1736 0.5159 0.059 Uiso 1 1 calc R . . H69 H 0.2292 0.2826 0.4934 0.059 Uiso 1 1 calc R . . C49 C 0.28485(18) 0.39341(18) 0.39132(15) 0.0279(5) Uani 1 1 d . . . H70 H 0.2504 0.3911 0.4404 0.034 Uiso 1 1 calc R . . C50 C 0.28849(17) 0.47785(17) 0.34301(14) 0.0250(5) Uani 1 1 d . . . C51 C 0.23478(17) 0.56529(17) 0.36784(14) 0.0249(5) Uani 1 1 d . . . H71 H 0.1939 0.6084 0.3279 0.030 Uiso 1 1 calc R . . H72 H 0.1959 0.5504 0.4162 0.030 Uiso 1 1 calc R . . C52 C 0.35374(17) 0.55019(17) 0.44250(14) 0.0247(5) Uani 1 1 d . . . H73 H 0.3213 0.5109 0.4808 0.030 Uiso 1 1 calc R . . H74 H 0.3668 0.5878 0.4694 0.030 Uiso 1 1 calc R . . C53 C 0.44158(17) 0.49025(18) 0.41109(14) 0.0252(5) Uani 1 1 d . . . C54 C 0.49126(19) 0.40535(19) 0.45503(16) 0.0307(6) Uani 1 1 d . . . H75 H 0.4678 0.3808 0.5058 0.037 Uiso 1 1 calc R . . C55 C 0.5757(2) 0.3566(2) 0.42388(17) 0.0365(6) Uani 1 1 d . . . H76 H 0.6101 0.2973 0.4524 0.044 Uiso 1 1 calc R . . C56 C 0.6093(2) 0.3955(2) 0.35069(18) 0.0382(7) Uani 1 1 d . . . H77 H 0.6682 0.3646 0.3291 0.046 Uiso 1 1 calc R . . C57 C 0.55567(18) 0.48047(19) 0.30935(16) 0.0311(6) Uani 1 1 d . . . H78 H 0.5786 0.5068 0.2589 0.037 Uiso 1 1 calc R . . C58 C 0.23159(16) 0.69555(17) 0.40643(14) 0.0238(5) Uani 1 1 d . . . H79 H 0.1953 0.6751 0.4549 0.029 Uiso 1 1 calc R . . H80 H 0.1884 0.7339 0.3671 0.029 Uiso 1 1 calc R . . C59 C 0.27743(16) 0.75533(16) 0.42013(13) 0.0223(5) Uani 1 1 d . . . C60 C 0.23380(17) 0.80324(17) 0.47643(14) 0.0246(5) Uani 1 1 d . . . H81 H 0.1805 0.7929 0.5063 0.030 Uiso 1 1 calc R . . C61 C 0.26551(18) 0.86515(17) 0.49014(14) 0.0266(5) Uani 1 1 d . . . C62 C 0.2176(2) 0.9141(2) 0.55461(16) 0.0351(6) Uani 1 1 d . . . C63 C 0.1253(4) 0.9811(4) 0.5331(3) 0.123(3) Uani 1 1 d . . . H82 H 0.1308 1.0413 0.5044 0.148 Uiso 1 1 calc R . . H83 H 0.0835 0.9872 0.5801 0.148 Uiso 1 1 calc R . . H84 H 0.1014 0.9584 0.5009 0.148 Uiso 1 1 calc R . . C64 C 0.2065(3) 0.8430(3) 0.63001(19) 0.0559(10) Uani 1 1 d . . . H85 H 0.1479 0.8336 0.6342 0.067 Uiso 1 1 calc R . . H86 H 0.2078 0.8653 0.6736 0.067 Uiso 1 1 calc R . . H87 H 0.2565 0.7845 0.6307 0.067 Uiso 1 1 calc R . . C65 C 0.2752(4) 0.9620(3) 0.5712(2) 0.0754(15) Uani 1 1 d . . . H88 H 0.3150 0.9192 0.6112 0.090 Uiso 1 1 calc R . . H89 H 0.2350 1.0162 0.5891 0.090 Uiso 1 1 calc R . . H90 H 0.3126 0.9813 0.5240 0.090 Uiso 1 1 calc R . . C66 C 0.34212(18) 0.88080(18) 0.44269(15) 0.0276(5) Uani 1 1 d . . . H91 H 0.3639 0.9246 0.4501 0.033 Uiso 1 1 calc R . . C67 C 0.38831(17) 0.83565(17) 0.38521(14) 0.0248(5) Uani 1 1 d . . . C68 C 0.46925(19) 0.85921(19) 0.33200(16) 0.0297(5) Uani 1 1 d . . . C69 C 0.4880(2) 0.9367(2) 0.34958(19) 0.0427(7) Uani 1 1 d . . . H92 H 0.4523 0.9964 0.3183 0.051 Uiso 1 1 calc R . . H93 H 0.5532 0.9287 0.3373 0.051 Uiso 1 1 calc R . . H94 H 0.4706 0.9347 0.4044 0.051 Uiso 1 1 calc R . . C70 C 0.55670(19) 0.7738(2) 0.34248(18) 0.0367(6) Uani 1 1 d . . . H95 H 0.5887 0.7731 0.3832 0.044 Uiso 1 1 calc R . . H96 H 0.5967 0.7763 0.2940 0.044 Uiso 1 1 calc R . . H97 H 0.5403 0.7178 0.3569 0.044 Uiso 1 1 calc R . . C71 C 0.4478(2) 0.8916(2) 0.24710(16) 0.0364(6) Uani 1 1 d . . . H98 H 0.4691 0.8383 0.2253 0.044 Uiso 1 1 calc R . . H99 H 0.4790 0.9356 0.2174 0.044 Uiso 1 1 calc R . . H100 H 0.3817 0.9215 0.2448 0.044 Uiso 1 1 calc R . . C72 C 0.35706(16) 0.76881(16) 0.37531(14) 0.0231(5) Uani 1 1 d . . . C73 C 0.8082(3) 0.8060(3) 0.2758(3) 0.0670(11) Uani 1 1 d . . . H101 H 0.8492 0.7740 0.2380 0.080 Uiso 1 1 calc R . . H102 H 0.7564 0.7833 0.2942 0.080 Uiso 1 1 calc R . . H103 H 0.8416 0.7944 0.3195 0.080 Uiso 1 1 calc R . . C74 C 0.7738(2) 0.9076(3) 0.23883(19) 0.0515(9) Uani 1 1 d . . . C75 C 0.8209(2) 0.9639(3) 0.24026(19) 0.0493(8) Uani 1 1 d . . . H104 H 0.8779 0.9360 0.2615 0.059 Uiso 1 1 calc R . . C76 C 0.7889(3) 1.0590(3) 0.2122(2) 0.0552(9) Uani 1 1 d . . . H105 H 0.8241 1.0944 0.2139 0.066 Uiso 1 1 calc R . . C77 C 0.7077(3) 1.1013(3) 0.1822(2) 0.0659(12) Uani 1 1 d . . . H106 H 0.6843 1.1667 0.1655 0.079 Uiso 1 1 calc R . . C78 C 0.6597(3) 1.0510(4) 0.1761(2) 0.0723(14) Uani 1 1 d . . . H107 H 0.6034 1.0812 0.1538 0.087 Uiso 1 1 calc R . . C79 C 0.6928(3) 0.9518(4) 0.2030(2) 0.0752(14) Uani 1 1 d . . . H108 H 0.6599 0.9166 0.1964 0.090 Uiso 1 1 calc R . . C80 C 0.9943(5) 0.2937(7) 0.4462(6) 0.162(4) Uani 1 1 d . . . H109 H 1.0499 0.2839 0.4103 0.194 Uiso 1 1 calc R . . H110 H 0.9664 0.2475 0.4503 0.194 Uiso 1 1 calc R . . H111 H 1.0098 0.2877 0.4971 0.194 Uiso 1 1 calc R . . C81 C 0.9273(4) 0.3896(6) 0.4167(4) 0.104(2) Uani 1 1 d . . . C82 C 0.9287(5) 0.4610(7) 0.4370(4) 0.116(3) Uani 1 1 d . . . H112 H 0.9738 0.4529 0.4681 0.139 Uiso 1 1 calc R . . C83 C 0.8663(7) 0.5449(7) 0.4135(5) 0.121(3) Uani 1 1 d . . . H113 H 0.8692 0.5950 0.4282 0.145 Uiso 1 1 calc R . . C84 C 0.7978(6) 0.5618(6) 0.3688(5) 0.124(3) Uani 1 1 d . . . H114 H 0.7543 0.6215 0.3528 0.149 Uiso 1 1 calc R . . C85 C 0.7967(7) 0.4852(8) 0.3487(4) 0.136(4) Uani 1 1 d . . . H115 H 0.7509 0.4912 0.3194 0.164 Uiso 1 1 calc R . . C86 C 0.8644(6) 0.4001(6) 0.3728(4) 0.110(3) Uani 1 1 d . . . H116 H 0.8658 0.3485 0.3577 0.132 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 0.0187(2) 0.0262(2) 0.01693(19) -0.00382(15) -0.00191(14) -0.00718(16) Cr2 0.0185(2) 0.0240(2) 0.0185(2) -0.00568(15) -0.00218(14) -0.00644(15) Cl1 0.0200(3) 0.0410(3) 0.0200(3) -0.0052(2) -0.0006(2) -0.0088(2) Cl2 0.0223(3) 0.0338(3) 0.0248(3) -0.0076(2) 0.0023(2) -0.0098(2) O1 0.0264(9) 0.0266(9) 0.0231(8) -0.0056(7) 0.0007(7) -0.0074(7) O2 0.0234(8) 0.0275(9) 0.0188(8) -0.0043(7) -0.0039(6) -0.0100(7) O3 0.0247(8) 0.0254(8) 0.0214(8) -0.0042(7) -0.0052(7) -0.0084(7) O4 0.0212(8) 0.0322(9) 0.0258(9) -0.0126(7) 0.0001(7) -0.0095(7) O5 0.0214(8) 0.0233(8) 0.0223(8) -0.0063(6) -0.0031(6) -0.0070(7) N1 0.0253(10) 0.0241(10) 0.0167(9) -0.0042(8) -0.0006(8) -0.0087(8) N2 0.0231(10) 0.0283(11) 0.0204(10) -0.0058(8) -0.0041(8) -0.0047(8) N3 0.0220(10) 0.0248(10) 0.0181(9) -0.0049(8) -0.0032(7) -0.0078(8) N4 0.0232(10) 0.0273(10) 0.0236(10) -0.0076(8) -0.0067(8) -0.0058(8) C1 0.0247(12) 0.0279(12) 0.0219(11) -0.0033(9) -0.0077(9) -0.0064(10) C2 0.0262(12) 0.0318(13) 0.0276(13) -0.0092(10) -0.0118(10) -0.0040(10) C3 0.0304(14) 0.0416(15) 0.0302(14) -0.0169(12) -0.0075(11) -0.0041(12) C4 0.0261(13) 0.0441(16) 0.0341(14) -0.0178(12) -0.0033(11) -0.0021(12) C5 0.0417(16) 0.0494(18) 0.0245(13) -0.0117(12) -0.0088(12) -0.0015(14) C6 0.0471(18) 0.0538(19) 0.0470(18) -0.0312(16) -0.0065(14) -0.0078(15) C7 0.0336(14) 0.0370(15) 0.0403(15) -0.0148(12) -0.0106(12) -0.0118(12) C8 0.0341(15) 0.0355(15) 0.0457(16) -0.0125(13) -0.0054(12) -0.0168(12) C9 0.051(2) 0.0453(18) 0.075(2) -0.0250(17) 0.0090(18) -0.0312(16) C10 0.040(2) 0.046(3) 0.367(13) -0.027(5) -0.014(4) -0.024(2) C11 0.064(3) 0.0351(19) 0.127(4) -0.009(2) 0.000(3) -0.0214(18) C12 0.300(11) 0.169(7) 0.068(3) -0.034(4) 0.050(5) -0.203(8) C13 0.0289(13) 0.0343(14) 0.0368(14) -0.0108(11) -0.0028(11) -0.0139(11) C14 0.0239(12) 0.0287(12) 0.0260(12) -0.0068(10) -0.0047(9) -0.0087(10) C15 0.0240(12) 0.0283(12) 0.0236(11) -0.0065(10) 0.0014(9) -0.0113(10) C16 0.0292(13) 0.0265(12) 0.0194(11) -0.0026(9) -0.0047(9) -0.0077(10) C17 0.0260(12) 0.0241(12) 0.0209(11) -0.0047(9) -0.0038(9) -0.0052(10) C18 0.0335(14) 0.0305(13) 0.0222(12) -0.0047(10) -0.0083(10) -0.0057(11) C19 0.0305(14) 0.0342(14) 0.0310(13) -0.0099(11) -0.0124(11) -0.0027(11) C20 0.0235(13) 0.0432(15) 0.0326(14) -0.0092(12) -0.0079(11) -0.0081(11) C21 0.0225(12) 0.0411(15) 0.0257(12) -0.0077(11) -0.0032(10) -0.0092(11) C22 0.0233(12) 0.0269(12) 0.0238(12) -0.0081(10) 0.0032(9) -0.0089(10) C23 0.0228(11) 0.0234(11) 0.0247(12) -0.0061(9) -0.0017(9) -0.0054(9) C24 0.0301(13) 0.0270(12) 0.0222(12) -0.0071(10) -0.0012(10) -0.0071(10) C25 0.0319(13) 0.0273(12) 0.0246(12) -0.0086(10) -0.0054(10) -0.0060(10) C26 0.0465(16) 0.0333(14) 0.0266(13) -0.0114(11) -0.0059(11) -0.0132(12) C27 0.0513(19) 0.059(2) 0.0255(14) -0.0121(13) -0.0023(13) -0.0245(16) C28 0.057(2) 0.060(2) 0.0336(15) -0.0081(14) -0.0125(14) -0.0311(17) C29 0.086(3) 0.0413(18) 0.050(2) -0.0251(16) -0.0189(19) -0.0010(18) C30 0.0294(13) 0.0304(13) 0.0284(13) -0.0068(10) -0.0062(10) -0.0110(11) C31 0.0253(12) 0.0299(13) 0.0268(12) -0.0062(10) -0.0042(10) -0.0103(10) C32 0.0310(13) 0.0386(14) 0.0274(13) -0.0058(11) -0.0021(10) -0.0205(12) C33 0.0317(15) 0.0516(18) 0.0387(15) -0.0119(13) -0.0021(12) -0.0217(13) C34 0.0476(18) 0.0390(16) 0.0430(17) -0.0015(13) -0.0002(14) -0.0230(14) C35 0.0521(18) 0.068(2) 0.0259(14) -0.0079(14) 0.0010(12) -0.0443(17) C36 0.0216(11) 0.0255(11) 0.0206(11) -0.0065(9) -0.0034(9) -0.0069(9) C37 0.0244(12) 0.0258(12) 0.0245(12) -0.0046(9) -0.0064(9) -0.0096(10) C38 0.0294(13) 0.0319(13) 0.0258(12) -0.0099(10) -0.0049(10) -0.0095(11) C39 0.0312(13) 0.0323(13) 0.0287(13) -0.0128(11) -0.0004(10) -0.0081(11) C40 0.052(2) 0.083(3) 0.057(2) -0.040(2) 0.0144(17) -0.032(2) C41 0.053(2) 0.079(3) 0.0359(17) -0.0238(18) -0.0057(15) 0.0047(19) C42 0.073(3) 0.047(2) 0.050(2) -0.0203(17) 0.0104(19) -0.0060(18) C43 0.0362(14) 0.0283(13) 0.0336(14) -0.0117(11) -0.0062(11) -0.0102(11) C44 0.0389(14) 0.0291(13) 0.0279(13) -0.0058(10) -0.0087(11) -0.0149(11) C45 0.0578(19) 0.0274(13) 0.0350(15) -0.0052(11) -0.0106(13) -0.0188(13) C46 0.072(2) 0.0429(17) 0.0439(18) -0.0102(14) -0.0087(16) -0.0334(17) C47 0.070(2) 0.0312(16) 0.0487(19) -0.0018(14) -0.0207(17) -0.0124(16) C48 0.084(3) 0.0355(16) 0.0369(16) -0.0032(13) -0.0074(16) -0.0333(17) C49 0.0323(13) 0.0308(13) 0.0244(12) -0.0068(10) -0.0045(10) -0.0141(11) C50 0.0247(12) 0.0281(12) 0.0251(12) -0.0077(10) -0.0045(9) -0.0102(10) C51 0.0243(12) 0.0288(12) 0.0247(12) -0.0080(10) -0.0017(9) -0.0118(10) C52 0.0263(12) 0.0271(12) 0.0192(11) -0.0047(9) -0.0054(9) -0.0064(10) C53 0.0243(12) 0.0311(13) 0.0240(12) -0.0096(10) -0.0058(9) -0.0097(10) C54 0.0337(14) 0.0314(13) 0.0257(12) -0.0060(10) -0.0084(11) -0.0076(11) C55 0.0345(15) 0.0330(14) 0.0364(15) -0.0093(12) -0.0148(12) 0.0010(12) C56 0.0280(14) 0.0402(16) 0.0371(15) -0.0129(12) -0.0078(11) 0.0033(12) C57 0.0255(13) 0.0348(14) 0.0298(13) -0.0097(11) -0.0034(10) -0.0051(11) C58 0.0201(11) 0.0280(12) 0.0222(11) -0.0086(9) 0.0000(9) -0.0064(9) C59 0.0222(11) 0.0226(11) 0.0203(11) -0.0040(9) -0.0061(9) -0.0048(9) C60 0.0246(12) 0.0265(12) 0.0195(11) -0.0041(9) -0.0031(9) -0.0059(10) C61 0.0332(13) 0.0240(12) 0.0200(11) -0.0060(9) -0.0047(10) -0.0052(10) C62 0.0445(16) 0.0332(14) 0.0258(13) -0.0146(11) 0.0021(11) -0.0083(12) C63 0.104(4) 0.135(5) 0.079(3) -0.080(4) -0.046(3) 0.080(4) C64 0.086(3) 0.058(2) 0.0351(17) -0.0252(16) 0.0268(17) -0.042(2) C65 0.129(4) 0.093(3) 0.045(2) -0.048(2) 0.039(2) -0.083(3) C66 0.0337(13) 0.0262(12) 0.0242(12) -0.0061(10) -0.0047(10) -0.0107(10) C67 0.0261(12) 0.0265(12) 0.0215(11) -0.0048(9) -0.0047(9) -0.0084(10) C68 0.0319(13) 0.0328(13) 0.0296(13) -0.0091(11) -0.0007(10) -0.0169(11) C69 0.0520(19) 0.0475(17) 0.0420(16) -0.0186(14) 0.0090(14) -0.0327(15) C70 0.0265(13) 0.0433(16) 0.0437(16) -0.0114(13) -0.0025(12) -0.0160(12) C71 0.0398(16) 0.0422(16) 0.0271(13) -0.0058(12) 0.0020(11) -0.0189(13) C72 0.0233(11) 0.0240(11) 0.0200(11) -0.0049(9) -0.0055(9) -0.0047(9) C73 0.052(2) 0.079(3) 0.073(3) -0.030(2) 0.025(2) -0.034(2) C74 0.0345(16) 0.080(3) 0.0357(16) -0.0217(17) 0.0115(13) -0.0161(17) C75 0.0435(18) 0.063(2) 0.0360(16) -0.0200(15) -0.0057(13) -0.0054(16) C76 0.055(2) 0.067(2) 0.0338(16) -0.0204(16) 0.0030(15) -0.0080(18) C77 0.044(2) 0.086(3) 0.044(2) -0.0078(19) 0.0114(16) -0.011(2) C78 0.0384(19) 0.108(4) 0.0389(19) 0.009(2) -0.0046(15) -0.012(2) C79 0.044(2) 0.139(5) 0.047(2) -0.016(3) 0.0093(17) -0.049(3) C80 0.079(5) 0.218(11) 0.188(9) -0.089(8) 0.043(5) -0.050(6) C81 0.073(4) 0.149(6) 0.096(4) -0.056(4) 0.042(3) -0.050(4) C82 0.103(5) 0.194(8) 0.113(5) -0.100(6) 0.056(4) -0.104(6) C83 0.141(7) 0.164(8) 0.105(5) -0.086(6) 0.073(5) -0.104(6) C84 0.129(6) 0.122(6) 0.104(5) 0.002(4) 0.037(5) -0.074(5) C85 0.172(8) 0.205(10) 0.068(4) 0.015(5) -0.010(4) -0.143(8) C86 0.162(7) 0.158(7) 0.068(4) -0.055(4) 0.031(4) -0.118(6) _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 O1 1.8930(18) . ? Cr1 O5 1.9737(17) . ? Cr1 O2 2.0360(18) . ? Cr1 N2 2.096(2) . ? Cr1 N1 2.115(2) . ? Cr1 Cl1 2.3457(7) . ? Cr2 O4 1.8875(17) . ? Cr2 O5 1.9713(17) . ? Cr2 O3 2.0484(17) . ? Cr2 N4 2.099(2) . ? Cr2 N3 2.117(2) . ? Cr2 Cl2 2.3356(7) . ? O1 C1 1.338(3) . ? O2 C36 1.380(3) . ? O3 C37 1.384(3) . ? O3 H117 0.9470 . ? O4 C72 1.332(3) . ? O5 H118 0.8910 . ? N1 C15 1.486(3) . ? N1 C16 1.493(3) . ? N1 C22 1.502(3) . ? N2 C21 1.345(3) . ? N2 C17 1.347(3) . ? N3 C58 1.488(3) . ? N3 C52 1.490(3) . ? N3 C51 1.499(3) . ? N4 C57 1.344(3) . ? N4 C53 1.352(3) . ? C1 C14 1.407(4) . ? C1 C2 1.415(4) . ? C2 C7 1.391(4) . ? C2 C3 1.537(4) . ? C3 C6 1.530(4) . ? C3 C4 1.539(4) . ? C3 C5 1.542(4) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.397(4) . ? C7 H10 0.9500 . ? C8 C13 1.391(4) . ? C8 C9 1.541(4) . ? C9 C10 1.484(6) . ? C9 C11 1.515(5) . ? C9 C12 1.527(7) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.394(4) . ? C13 H20 0.9500 . ? C14 C15 1.513(4) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.498(4) . ? C16 H23 0.9900 . ? C16 H24 0.9900 . ? C17 C18 1.387(4) . ? C18 C19 1.384(4) . ? C18 H25 0.9500 . ? C19 C20 1.379(4) . ? C19 H26 0.9500 . ? C20 C21 1.383(4) . ? C20 H27 0.9500 . ? C21 H28 0.9500 . ? C22 C23 1.503(3) . ? C22 H29 0.9900 . ? C22 H30 0.9900 . ? C23 C24 1.389(3) . ? C23 C36 1.410(3) . ? C24 C25 1.392(4) . ? C24 H31 0.9500 . ? C25 C30 1.393(4) . ? C25 C26 1.535(3) . ? C26 C27 1.526(4) . ? C26 C29 1.528(4) . ? C26 C28 1.539(4) . ? C27 H32 0.9800 . ? C27 H33 0.9800 . ? C27 H34 0.9800 . ? C28 H35 0.9800 . ? C28 H36 0.9800 . ? C28 H37 0.9800 . ? C29 H38 0.9800 . ? C29 H39 0.9800 . ? C29 H40 0.9800 . ? C30 C31 1.406(4) . ? C30 H41 0.9500 . ? C31 C36 1.403(3) . ? C31 C32 1.542(4) . ? C32 C35 1.534(4) . ? C32 C33 1.542(4) . ? C32 C34 1.542(4) . ? C33 H42 0.9800 . ? C33 H43 0.9800 . ? C33 H44 0.9800 . ? C34 H45 0.9800 . ? C34 H46 0.9800 . ? C34 H47 0.9800 . ? C35 H48 0.9800 . ? C35 H49 0.9800 . ? C35 H50 0.9800 . ? C37 C50 1.396(4) . ? C37 C38 1.408(4) . ? C38 C43 1.395(4) . ? C38 C39 1.548(4) . ? C39 C41 1.503(4) . ? C39 C42 1.535(4) . ? C39 C40 1.540(5) . ? C40 H51 0.9800 . ? C40 H52 0.9800 . ? C40 H53 0.9800 . ? C41 H54 0.9800 . ? C41 H55 0.9800 . ? C41 H56 0.9800 . ? C42 H57 0.9800 . ? C42 H58 0.9800 . ? C42 H59 0.9800 . ? C43 C44 1.402(4) . ? C43 H60 0.9500 . ? C44 C49 1.386(4) . ? C44 C45 1.534(4) . ? C45 C48 1.525(5) . ? C45 C46 1.536(4) . ? C45 C47 1.544(5) . ? C46 H61 0.9800 . ? C46 H62 0.9800 . ? C46 H63 0.9800 . ? C47 H64 0.9800 . ? C47 H65 0.9800 . ? C47 H66 0.9800 . ? C48 H67 0.9800 . ? C48 H68 0.9800 . ? C48 H69 0.9800 . ? C49 C50 1.393(4) . ? C49 H70 0.9500 . ? C50 C51 1.509(3) . ? C51 H71 0.9900 . ? C51 H72 0.9900 . ? C52 C53 1.491(3) . ? C52 H73 0.9900 . ? C52 H74 0.9900 . ? C53 C54 1.384(4) . ? C54 C55 1.386(4) . ? C54 H75 0.9500 . ? C55 C56 1.383(4) . ? C55 H76 0.9500 . ? C56 C57 1.388(4) . ? C56 H77 0.9500 . ? C57 H78 0.9500 . ? C58 C59 1.510(3) . ? C58 H79 0.9900 . ? C58 H80 0.9900 . ? C59 C60 1.397(3) . ? C59 C72 1.410(3) . ? C60 C61 1.381(4) . ? C60 H81 0.9500 . ? C61 C66 1.400(4) . ? C61 C62 1.539(3) . ? C62 C63 1.501(5) . ? C62 C65 1.522(5) . ? C62 C64 1.526(4) . ? C63 H82 0.9800 . ? C63 H83 0.9800 . ? C63 H84 0.9800 . ? C64 H85 0.9800 . ? C64 H86 0.9800 . ? C64 H87 0.9800 . ? C65 H88 0.9800 . ? C65 H89 0.9800 . ? C65 H90 0.9800 . ? C66 C67 1.395(4) . ? C66 H91 0.9500 . ? C67 C72 1.418(3) . ? C67 C68 1.539(4) . ? C68 C69 1.529(4) . ? C68 C70 1.542(4) . ? C68 C71 1.545(4) . ? C69 H92 0.9800 . ? C69 H93 0.9800 . ? C69 H94 0.9800 . ? C70 H95 0.9800 . ? C70 H96 0.9800 . ? C70 H97 0.9800 . ? C71 H98 0.9800 . ? C71 H99 0.9800 . ? C71 H100 0.9800 . ? C73 C74 1.498(6) . ? C73 H101 0.9800 . ? C73 H102 0.9800 . ? C73 H103 0.9800 . ? C74 C75 1.387(5) . ? C74 C79 1.399(6) . ? C75 C76 1.385(5) . ? C75 H104 0.9500 . ? C76 C77 1.350(6) . ? C76 H105 0.9500 . ? C77 C78 1.346(7) . ? C77 H106 0.9500 . ? C78 C79 1.441(7) . ? C78 H107 0.9500 . ? C79 H108 0.9500 . ? C80 C81 1.520(11) . ? C80 H109 0.9800 . ? C80 H110 0.9800 . ? C80 H111 0.9800 . ? C81 C82 1.329(9) . ? C81 C86 1.337(10) . ? C82 C83 1.346(12) . ? C82 H112 0.9500 . ? C83 C84 1.389(11) . ? C83 H113 0.9500 . ? C84 C85 1.406(12) . ? C84 H114 0.9500 . ? C85 C86 1.397(12) . ? C85 H115 0.9500 . ? C86 H116 0.9500 . ? 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 O1 Cr1 O5 89.36(7) . . ? O1 Cr1 O2 175.37(7) . . ? O5 Cr1 O2 86.71(7) . . ? O1 Cr1 N2 94.59(8) . . ? O5 Cr1 N2 172.13(8) . . ? O2 Cr1 N2 89.03(8) . . ? O1 Cr1 N1 87.44(8) . . ? O5 Cr1 N1 93.09(8) . . ? O2 Cr1 N1 90.33(7) . . ? N2 Cr1 N1 80.31(8) . . ? O1 Cr1 Cl1 90.08(6) . . ? O5 Cr1 Cl1 96.14(5) . . ? O2 Cr1 Cl1 92.76(5) . . ? N2 Cr1 Cl1 90.66(6) . . ? N1 Cr1 Cl1 170.41(6) . . ? O4 Cr2 O5 90.67(7) . . ? O4 Cr2 O3 177.21(7) . . ? O5 Cr2 O3 87.11(7) . . ? O4 Cr2 N4 90.95(8) . . ? O5 Cr2 N4 172.00(8) . . ? O3 Cr2 N4 91.02(7) . . ? O4 Cr2 N3 87.12(8) . . ? O5 Cr2 N3 91.92(7) . . ? O3 Cr2 N3 91.26(7) . . ? N4 Cr2 N3 80.34(8) . . ? O4 Cr2 Cl2 91.36(6) . . ? O5 Cr2 Cl2 94.97(5) . . ? O3 Cr2 Cl2 90.52(5) . . ? N4 Cr2 Cl2 92.82(6) . . ? N3 Cr2 Cl2 172.97(6) . . ? C1 O1 Cr1 132.81(16) . . ? C36 O2 Cr1 119.64(14) . . ? C37 O3 Cr2 118.66(14) . . ? C37 O3 H117 114.2 . . ? Cr2 O3 H117 103.4 . . ? C72 O4 Cr2 132.65(16) . . ? Cr2 O5 Cr1 147.70(9) . . ? Cr2 O5 H118 108.5 . . ? Cr1 O5 H118 103.8 . . ? C15 N1 C16 108.91(19) . . ? C15 N1 C22 107.07(19) . . ? C16 N1 C22 110.42(19) . . ? C15 N1 Cr1 112.32(14) . . ? C16 N1 Cr1 107.59(15) . . ? C22 N1 Cr1 110.53(14) . . ? C21 N2 C17 118.2(2) . . ? C21 N2 Cr1 126.22(17) . . ? C17 N2 Cr1 115.07(17) . . ? C58 N3 C52 108.82(18) . . ? C58 N3 C51 107.26(18) . . ? C52 N3 C51 110.05(19) . . ? C58 N3 Cr2 112.35(15) . . ? C52 N3 Cr2 108.57(15) . . ? C51 N3 Cr2 109.78(14) . . ? C57 N4 C53 118.5(2) . . ? C57 N4 Cr2 126.35(18) . . ? C53 N4 Cr2 114.85(16) . . ? O1 C1 C14 122.0(2) . . ? O1 C1 C2 118.7(2) . . ? C14 C1 C2 119.3(2) . . ? C7 C2 C1 117.8(2) . . ? C7 C2 C3 121.5(2) . . ? C1 C2 C3 120.7(2) . . ? C6 C3 C2 112.5(3) . . ? C6 C3 C4 107.6(2) . . ? C2 C3 C4 110.1(2) . . ? C6 C3 C5 107.5(2) . . ? C2 C3 C5 110.2(2) . . ? C4 C3 C5 108.8(3) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 123.8(3) . . ? C2 C7 H10 118.1 . . ? C8 C7 H10 118.1 . . ? C13 C8 C7 116.9(3) . . ? C13 C8 C9 120.0(3) . . ? C7 C8 C9 123.0(3) . . ? C10 C9 C11 108.1(4) . . ? C10 C9 C12 113.7(6) . . ? C11 C9 C12 103.8(5) . . ? C10 C9 C8 109.5(4) . . ? C11 C9 C8 112.4(3) . . ? C12 C9 C8 109.4(3) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 121.6(3) . . ? C8 C13 H20 119.2 . . ? C14 C13 H20 119.2 . . ? C13 C14 C1 120.1(2) . . ? C13 C14 C15 117.3(2) . . ? C1 C14 C15 122.5(2) . . ? N1 C15 C14 115.4(2) . . ? N1 C15 H21 108.4 . . ? C14 C15 H21 108.4 . . ? N1 C15 H22 108.4 . . ? C14 C15 H22 108.4 . . ? H21 C15 H22 107.5 . . ? N1 C16 C17 111.8(2) . . ? N1 C16 H23 109.3 . . ? C17 C16 H23 109.3 . . ? N1 C16 H24 109.3 . . ? C17 C16 H24 109.3 . . ? H23 C16 H24 107.9 . . ? N2 C17 C18 122.1(2) . . ? N2 C17 C16 115.1(2) . . ? C18 C17 C16 122.7(2) . . ? C19 C18 C17 119.1(2) . . ? C19 C18 H25 120.4 . . ? C17 C18 H25 120.4 . . ? C20 C19 C18 118.8(2) . . ? C20 C19 H26 120.6 . . ? C18 C19 H26 120.6 . . ? C19 C20 C21 119.2(3) . . ? C19 C20 H27 120.4 . . ? C21 C20 H27 120.4 . . ? N2 C21 C20 122.4(2) . . ? N2 C21 H28 118.8 . . ? C20 C21 H28 118.8 . . ? N1 C22 C23 113.7(2) . . ? N1 C22 H29 108.8 . . ? C23 C22 H29 108.8 . . ? N1 C22 H30 108.8 . . ? C23 C22 H30 108.8 . . ? H29 C22 H30 107.7 . . ? C24 C23 C36 120.4(2) . . ? C24 C23 C22 120.5(2) . . ? C36 C23 C22 119.0(2) . . ? C23 C24 C25 121.0(2) . . ? C23 C24 H31 119.5 . . ? C25 C24 H31 119.5 . . ? C24 C25 C30 116.8(2) . . ? C24 C25 C26 123.0(2) . . ? C30 C25 C26 120.2(2) . . ? C27 C26 C29 110.0(3) . . ? C27 C26 C25 111.9(2) . . ? C29 C26 C25 109.2(2) . . ? C27 C26 C28 107.0(3) . . ? C29 C26 C28 109.0(3) . . ? C25 C26 C28 109.7(2) . . ? C26 C27 H32 109.5 . . ? C26 C27 H33 109.5 . . ? H32 C27 H33 109.5 . . ? C26 C27 H34 109.5 . . ? H32 C27 H34 109.5 . . ? H33 C27 H34 109.5 . . ? C26 C28 H35 109.5 . . ? C26 C28 H36 109.5 . . ? H35 C28 H36 109.5 . . ? C26 C28 H37 109.5 . . ? H35 C28 H37 109.5 . . ? H36 C28 H37 109.5 . . ? C26 C29 H38 109.5 . . ? C26 C29 H39 109.5 . . ? H38 C29 H39 109.5 . . ? C26 C29 H40 109.5 . . ? H38 C29 H40 109.5 . . ? H39 C29 H40 109.5 . . ? C25 C30 C31 125.2(2) . . ? C25 C30 H41 117.4 . . ? C31 C30 H41 117.4 . . ? C36 C31 C30 115.7(2) . . ? C36 C31 C32 128.2(2) . . ? C30 C31 C32 116.1(2) . . ? C35 C32 C31 115.3(2) . . ? C35 C32 C33 106.5(2) . . ? C31 C32 C33 109.5(2) . . ? C35 C32 C34 107.3(3) . . ? C31 C32 C34 108.8(2) . . ? C33 C32 C34 109.4(2) . . ? C32 C33 H42 109.5 . . ? C32 C33 H43 109.5 . . ? H42 C33 H43 109.5 . . ? C32 C33 H44 109.5 . . ? H42 C33 H44 109.5 . . ? H43 C33 H44 109.5 . . ? C32 C34 H45 109.5 . . ? C32 C34 H46 109.5 . . ? H45 C34 H46 109.5 . . ? C32 C34 H47 109.5 . . ? H45 C34 H47 109.5 . . ? H46 C34 H47 109.5 . . ? C32 C35 H48 109.5 . . ? C32 C35 H49 109.5 . . ? H48 C35 H49 109.5 . . ? C32 C35 H50 109.5 . . ? H48 C35 H50 109.5 . . ? H49 C35 H50 109.5 . . ? O2 C36 C31 123.5(2) . . ? O2 C36 C23 115.7(2) . . ? C31 C36 C23 120.8(2) . . ? O3 C37 C50 116.4(2) . . ? O3 C37 C38 122.5(2) . . ? C50 C37 C38 121.1(2) . . ? C43 C38 C37 115.7(2) . . ? C43 C38 C39 119.2(2) . . ? C37 C38 C39 125.1(2) . . ? C41 C39 C42 107.4(3) . . ? C41 C39 C40 109.9(3) . . ? C42 C39 C40 105.6(3) . . ? C41 C39 C38 111.1(2) . . ? C42 C39 C38 112.4(3) . . ? C40 C39 C38 110.2(2) . . ? C39 C40 H51 109.5 . . ? C39 C40 H52 109.5 . . ? H51 C40 H52 109.5 . . ? C39 C40 H53 109.5 . . ? H51 C40 H53 109.5 . . ? H52 C40 H53 109.5 . . ? C39 C41 H54 109.5 . . ? C39 C41 H55 109.5 . . ? H54 C41 H55 109.5 . . ? C39 C41 H56 109.5 . . ? H54 C41 H56 109.5 . . ? H55 C41 H56 109.5 . . ? C39 C42 H57 109.5 . . ? C39 C42 H58 109.5 . . ? H57 C42 H58 109.5 . . ? C39 C42 H59 109.5 . . ? H57 C42 H59 109.5 . . ? H58 C42 H59 109.5 . . ? C38 C43 C44 124.7(3) . . ? C38 C43 H60 117.6 . . ? C44 C43 H60 117.6 . . ? C49 C44 C43 117.3(2) . . ? C49 C44 C45 123.1(3) . . ? C43 C44 C45 119.5(2) . . ? C48 C45 C44 112.0(2) . . ? C48 C45 C46 109.3(3) . . ? C44 C45 C46 108.2(2) . . ? C48 C45 C47 108.7(3) . . ? C44 C45 C47 109.1(3) . . ? C46 C45 C47 109.4(3) . . ? C45 C46 H61 109.5 . . ? C45 C46 H62 109.5 . . ? H61 C46 H62 109.5 . . ? C45 C46 H63 109.5 . . ? H61 C46 H63 109.5 . . ? H62 C46 H63 109.5 . . ? C45 C47 H64 109.5 . . ? C45 C47 H65 109.5 . . ? H64 C47 H65 109.5 . . ? C45 C47 H66 109.5 . . ? H64 C47 H66 109.5 . . ? H65 C47 H66 109.5 . . ? C45 C48 H67 109.5 . . ? C45 C48 H68 109.5 . . ? H67 C48 H68 109.5 . . ? C45 C48 H69 109.5 . . ? H67 C48 H69 109.5 . . ? H68 C48 H69 109.5 . . ? C44 C49 C50 120.4(2) . . ? C44 C49 H70 119.8 . . ? C50 C49 H70 119.8 . . ? C49 C50 C37 120.7(2) . . ? C49 C50 C51 119.7(2) . . ? C37 C50 C51 119.6(2) . . ? N3 C51 C50 113.5(2) . . ? N3 C51 H71 108.9 . . ? C50 C51 H71 108.9 . . ? N3 C51 H72 108.9 . . ? C50 C51 H72 108.9 . . ? H71 C51 H72 107.7 . . ? N3 C52 C53 111.9(2) . . ? N3 C52 H73 109.2 . . ? C53 C52 H73 109.2 . . ? N3 C52 H74 109.2 . . ? C53 C52 H74 109.2 . . ? H73 C52 H74 107.9 . . ? N4 C53 C54 122.1(2) . . ? N4 C53 C52 115.5(2) . . ? C54 C53 C52 122.3(2) . . ? C53 C54 C55 119.1(3) . . ? C53 C54 H75 120.5 . . ? C55 C54 H75 120.5 . . ? C56 C55 C54 119.0(3) . . ? C56 C55 H76 120.5 . . ? C54 C55 H76 120.5 . . ? C55 C56 C57 119.0(3) . . ? C55 C56 H77 120.5 . . ? C57 C56 H77 120.5 . . ? N4 C57 C56 122.2(3) . . ? N4 C57 H78 118.9 . . ? C56 C57 H78 118.9 . . ? N3 C58 C59 115.88(19) . . ? N3 C58 H79 108.3 . . ? C59 C58 H79 108.3 . . ? N3 C58 H80 108.3 . . ? C59 C58 H80 108.3 . . ? H79 C58 H80 107.4 . . ? C60 C59 C72 120.1(2) . . ? C60 C59 C58 117.0(2) . . ? C72 C59 C58 122.8(2) . . ? C61 C60 C59 122.2(2) . . ? C61 C60 H81 118.9 . . ? C59 C60 H81 118.9 . . ? C60 C61 C66 116.8(2) . . ? C60 C61 C62 120.8(2) . . ? C66 C61 C62 122.4(2) . . ? C63 C62 C65 111.3(4) . . ? C63 C62 C64 109.5(4) . . ? C65 C62 C64 105.1(3) . . ? C63 C62 C61 109.5(3) . . ? C65 C62 C61 111.7(3) . . ? C64 C62 C61 109.7(2) . . ? C62 C63 H82 109.5 . . ? C62 C63 H83 109.5 . . ? H82 C63 H83 109.5 . . ? C62 C63 H84 109.5 . . ? H82 C63 H84 109.5 . . ? H83 C63 H84 109.5 . . ? C62 C64 H85 109.5 . . ? C62 C64 H86 109.5 . . ? H85 C64 H86 109.5 . . ? C62 C64 H87 109.5 . . ? H85 C64 H87 109.5 . . ? H86 C64 H87 109.5 . . ? C62 C65 H88 109.5 . . ? C62 C65 H89 109.5 . . ? H88 C65 H89 109.5 . . ? C62 C65 H90 109.5 . . ? H88 C65 H90 109.5 . . ? H89 C65 H90 109.5 . . ? C67 C66 C61 123.7(2) . . ? C67 C66 H91 118.2 . . ? C61 C66 H91 118.2 . . ? C66 C67 C72 118.2(2) . . ? C66 C67 C68 121.4(2) . . ? C72 C67 C68 120.4(2) . . ? C69 C68 C67 111.8(2) . . ? C69 C68 C70 107.8(2) . . ? C67 C68 C70 110.1(2) . . ? C69 C68 C71 107.7(2) . . ? C67 C68 C71 109.7(2) . . ? C70 C68 C71 109.6(2) . . ? C68 C69 H92 109.5 . . ? C68 C69 H93 109.5 . . ? H92 C69 H93 109.5 . . ? C68 C69 H94 109.5 . . ? H92 C69 H94 109.5 . . ? H93 C69 H94 109.5 . . ? C68 C70 H95 109.5 . . ? C68 C70 H96 109.5 . . ? H95 C70 H96 109.5 . . ? C68 C70 H97 109.5 . . ? H95 C70 H97 109.5 . . ? H96 C70 H97 109.5 . . ? C68 C71 H98 109.5 . . ? C68 C71 H99 109.5 . . ? H98 C71 H99 109.5 . . ? C68 C71 H100 109.5 . . ? H98 C71 H100 109.5 . . ? H99 C71 H100 109.5 . . ? O4 C72 C59 122.4(2) . . ? O4 C72 C67 118.7(2) . . ? C59 C72 C67 118.8(2) . . ? C74 C73 H101 109.5 . . ? C74 C73 H102 109.5 . . ? H101 C73 H102 109.5 . . ? C74 C73 H103 109.5 . . ? H101 C73 H103 109.5 . . ? H102 C73 H103 109.5 . . ? C75 C74 C79 116.1(4) . . ? C75 C74 C73 120.7(3) . . ? C79 C74 C73 123.2(4) . . ? C76 C75 C74 123.2(4) . . ? C76 C75 H104 118.4 . . ? C74 C75 H104 118.4 . . ? C77 C76 C75 120.2(4) . . ? C77 C76 H105 119.9 . . ? C75 C76 H105 119.9 . . ? C78 C77 C76 120.1(5) . . ? C78 C77 H106 120.0 . . ? C76 C77 H106 120.0 . . ? C77 C78 C79 120.8(4) . . ? C77 C78 H107 119.6 . . ? C79 C78 H107 119.6 . . ? C74 C79 C78 119.5(4) . . ? C74 C79 H108 120.2 . . ? C78 C79 H108 120.2 . . ? C81 C80 H109 109.5 . . ? C81 C80 H110 109.5 . . ? H109 C80 H110 109.5 . . ? C81 C80 H111 109.5 . . ? H109 C80 H111 109.5 . . ? H110 C80 H111 109.5 . . ? C82 C81 C86 120.7(8) . . ? C82 C81 C80 120.5(8) . . ? C86 C81 C80 118.8(8) . . ? C81 C82 C83 120.0(8) . . ? C81 C82 H112 120.0 . . ? C83 C82 H112 120.0 . . ? C82 C83 C84 123.3(7) . . ? C82 C83 H113 118.4 . . ? C84 C83 H113 118.4 . . ? C83 C84 C85 115.9(8) . . ? C83 C84 H114 122.0 . . ? C85 C84 H114 122.0 . . ? C86 C85 C84 118.7(8) . . ? C86 C85 H115 120.7 . . ? C84 C85 H115 120.7 . . ? C81 C86 C85 121.4(7) . . ? C81 C86 H116 119.3 . . ? C85 C86 H116 119.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.077 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.082 #===END