# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Syntheses, structures and reactions of a series of beta-diketiminatoyttrium compounds ; _publ_requested_category FM loop_ _publ_author_name 'M. Lappert' 'Yanxiang Cheng.' 'Peter B. Hitchcock' 'Xuehong Wei.' # Attachment 'mfl_apr2008.cif' data_(3a)-apr1103 _database_code_depnum_ccdc_archive 'CCDC 684941' _audit_creation_date 2003-04-09T14:02:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C62 H98 Cl6 Li2 N4 O4 Y2, C4 H10 O' _chemical_formula_sum 'C66 H108 Cl6 Li2 N4 O5 Y2' _chemical_formula_weight 1441.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5518(3) _cell_length_b 26.9951(7) _cell_length_c 25.3522(7) _cell_angle_alpha 90 _cell_angle_beta 95.190(1) _cell_angle_gamma 90 _cell_volume 7873.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 528569 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5983 _exptl_absorpt_correction_T_max 0.846 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.531811E-1 _diffrn_orient_matrix_ub_12 0.148859E-1 _diffrn_orient_matrix_ub_13 -0.24682E-1 _diffrn_orient_matrix_ub_21 0.560441E-1 _diffrn_orient_matrix_ub_22 0.90986E-2 _diffrn_orient_matrix_ub_23 0.30862E-1 _diffrn_orient_matrix_ub_31 0.03983 _diffrn_orient_matrix_ub_32 -0.326782E-1 _diffrn_orient_matrix_ub_33 -0.26505E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_unetI/netI 0.0799 _diffrn_reflns_number 46077 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.939 _diffrn_measured_fraction_theta_max 0.939 _reflns_number_total 13084 _reflns_number_gt 9362 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The diffraction was weak , becoming essentially non-existent above 23 degrees theta. 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^)+(0.0320P)^2^+61.1621P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 13084 _refine_ls_number_parameters 770 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1918 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.08 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.1 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Y Y -2.7962 3.5667 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y1 Y 0.41876(6) 0.06220(3) 0.29837(3) 0.0282(2) Uani 1 1 d . . . Y2 Y 0.56932(6) -0.04127(3) 0.20305(3) 0.0272(2) Uani 1 1 d . . . Li1 Li 0.8079(13) 0.0049(6) 0.1351(7) 0.050(4) Uani 1 1 d . C . Li2 Li 0.1730(12) 0.0222(6) 0.3652(6) 0.043(4) Uani 1 1 d . D . Cl1 Cl 0.62592(15) 0.01938(8) 0.28521(8) 0.0332(5) Uani 1 1 d . . . Cl2 Cl 0.20529(16) 0.09018(8) 0.30791(9) 0.0379(5) Uani 1 1 d . . . Cl3 Cl 0.36592(17) -0.00964(8) 0.36390(9) 0.0411(6) Uani 1 1 d . . . Cl4 Cl 0.36147(15) 0.00128(7) 0.21583(8) 0.0323(5) Uani 1 1 d . . . Cl5 Cl 0.78209(17) -0.06697(8) 0.18788(10) 0.0435(6) Uani 1 1 d . . . Cl6 Cl 0.61208(18) 0.03210(8) 0.13754(9) 0.0408(6) Uani 1 1 d . . . O1 O 0.9289(5) 0.0444(3) 0.1709(3) 0.0536(18) Uani 1 1 d . . . O2 O 0.8160(6) -0.0093(4) 0.0596(3) 0.079(3) Uani 1 1 d . . . O3 O 0.1560(5) 0.0427(2) 0.4375(3) 0.0499(16) Uani 1 1 d . . . O4 O 0.0550(5) -0.0199(2) 0.3286(3) 0.0518(17) Uani 1 1 d . . . O5 O 0.9708(9) -0.2330(3) 0.4512(4) 0.091(3) Uani 1 1 d . . . N1 N 0.4401(5) 0.1283(2) 0.2419(3) 0.0295(16) Uani 1 1 d . . . N2 N 0.5293(5) 0.1147(2) 0.3550(3) 0.0339(17) Uani 1 1 d . . . N3 N 0.5499(5) -0.1066(2) 0.2617(3) 0.0326(16) Uani 1 1 d . . . N4 N 0.4644(5) -0.0973(2) 0.1497(3) 0.0303(16) Uani 1 1 d . . . C1 C 0.5476(7) 0.1475(3) 0.2401(3) 0.034(2) Uani 1 1 d . . . C2 C 0.6335(7) 0.1467(3) 0.2835(4) 0.034(2) Uani 1 1 d . . . H2 H 0.7099 0.1545 0.2751 0.041 Uiso 1 1 calc R . . C3 C 0.6234(6) 0.1363(3) 0.3365(4) 0.033(2) Uani 1 1 d . . . C4 C 0.5832(8) 0.1709(3) 0.1894(4) 0.047(2) Uani 1 1 d . . . H4A H 0.5934 0.145 0.1632 0.07 Uiso 1 1 calc R . . H4B H 0.6565 0.1889 0.1971 0.07 Uiso 1 1 calc R . . H4C H 0.5226 0.194 0.1753 0.07 Uiso 1 1 calc R . . C5 C 0.7250(7) 0.1513(3) 0.3746(4) 0.045(2) Uani 1 1 d . . . H5A H 0.7038 0.1803 0.3948 0.067 Uiso 1 1 calc R . . H5B H 0.7915 0.1594 0.3548 0.067 Uiso 1 1 calc R . . H5C H 0.7458 0.1239 0.399 0.067 Uiso 1 1 calc R . . C6 C 0.3557(7) 0.1405(3) 0.1980(4) 0.037(2) Uani 1 1 d . . . C7 C 0.2742(7) 0.1784(3) 0.2038(4) 0.037(2) Uani 1 1 d . . . C8 C 0.1964(8) 0.1878(4) 0.1604(5) 0.052(3) Uani 1 1 d . . . H8 H 0.141 0.2135 0.163 0.062 Uiso 1 1 calc R . . C9 C 0.1948(8) 0.1623(4) 0.1147(5) 0.058(3) Uani 1 1 d . . . H9 H 0.1401 0.1705 0.0857 0.07 Uiso 1 1 calc R . . C10 C 0.2728(8) 0.1243(4) 0.1101(4) 0.051(3) Uani 1 1 d . . . H10 H 0.2714 0.1057 0.0782 0.061 Uiso 1 1 calc R . . C11 C 0.3529(7) 0.1135(3) 0.1521(4) 0.038(2) Uani 1 1 d . . . H11 H 0.4066 0.0872 0.1492 0.045 Uiso 1 1 calc R . . C12 C 0.2763(7) 0.2080(3) 0.2541(4) 0.045(2) Uani 1 1 d . . . H12 H 0.3107 0.1862 0.2833 0.054 Uiso 1 1 calc R . . C13 C 0.1550(7) 0.2233(4) 0.2685(5) 0.057(3) Uani 1 1 d . . . H13A H 0.1624 0.2421 0.3017 0.085 Uiso 1 1 calc R . . H13B H 0.108 0.1936 0.2729 0.085 Uiso 1 1 calc R . . H13C H 0.1172 0.2439 0.2402 0.085 Uiso 1 1 calc R . . C14 C 0.3550(9) 0.2527(4) 0.2524(5) 0.068(3) Uani 1 1 d . . . H14A H 0.355 0.2711 0.2857 0.101 Uiso 1 1 calc R . . H14B H 0.3268 0.2741 0.2228 0.101 Uiso 1 1 calc R . . H14C H 0.4342 0.2417 0.2476 0.101 Uiso 1 1 calc R . . C15 C 0.5227(7) 0.1149(3) 0.4110(4) 0.039(2) Uani 1 1 d . . . C16 C 0.4875(8) 0.1580(4) 0.4366(4) 0.048(2) Uani 1 1 d . . . C17 C 0.4832(9) 0.1547(5) 0.4918(5) 0.067(3) Uani 1 1 d . . . H17 H 0.4608 0.1832 0.5103 0.081 Uiso 1 1 calc R . . C18 C 0.5096(10) 0.1124(6) 0.5204(5) 0.071(4) Uani 1 1 d . . . H18 H 0.5058 0.1118 0.5577 0.085 Uiso 1 1 calc R . . C19 C 0.5412(9) 0.0718(5) 0.4941(5) 0.061(3) Uani 1 1 d . . . H19 H 0.5594 0.0421 0.5133 0.073 Uiso 1 1 calc R . . C20 C 0.5476(8) 0.0726(4) 0.4397(4) 0.052(3) Uani 1 1 d . . . H20 H 0.5695 0.0434 0.4222 0.063 Uiso 1 1 calc R . . C21 C 0.4544(8) 0.2054(4) 0.4063(4) 0.054(3) Uani 1 1 d . . . H21 H 0.4807 0.2021 0.3699 0.065 Uiso 1 1 calc R . . C22 C 0.3232(9) 0.2122(4) 0.4006(5) 0.072(3) Uani 1 1 d . . . H22A H 0.3035 0.2428 0.3809 0.107 Uiso 1 1 calc R . . H22B H 0.2948 0.2143 0.4358 0.107 Uiso 1 1 calc R . . H22C H 0.2866 0.1839 0.3814 0.107 Uiso 1 1 calc R . . C23 C 0.5116(11) 0.2516(4) 0.4318(7) 0.099(5) Uani 1 1 d . . . H23A H 0.4875 0.2808 0.4106 0.148 Uiso 1 1 calc R . . H23B H 0.5963 0.2482 0.4335 0.148 Uiso 1 1 calc R . . H23C H 0.4877 0.2555 0.4677 0.148 Uiso 1 1 calc R . . C24 C 0.4457(7) -0.1270(3) 0.2647(3) 0.0308(19) Uani 1 1 d . . . C25 C 0.3610(7) -0.1287(3) 0.2214(4) 0.032(2) Uani 1 1 d . . . H25 H 0.2852 -0.1375 0.2298 0.038 Uiso 1 1 calc R . . C26 C 0.3714(7) -0.1193(3) 0.1676(4) 0.034(2) Uani 1 1 d . . . C27 C 0.4132(7) -0.1505(3) 0.3158(4) 0.042(2) Uani 1 1 d . . . H27A H 0.4741 -0.1738 0.3289 0.064 Uiso 1 1 calc R . . H27B H 0.3393 -0.1682 0.309 0.064 Uiso 1 1 calc R . . H27C H 0.4051 -0.1246 0.3423 0.064 Uiso 1 1 calc R . . C28 C 0.2695(7) -0.1349(4) 0.1294(4) 0.043(2) Uani 1 1 d . . . H28A H 0.249 -0.1078 0.1045 0.065 Uiso 1 1 calc R . . H28B H 0.2027 -0.1426 0.1491 0.065 Uiso 1 1 calc R . . H28C H 0.2908 -0.1642 0.1097 0.065 Uiso 1 1 calc R . . C29 C 0.6354(6) -0.1148(3) 0.3067(4) 0.035(2) Uani 1 1 d . . . C30 C 0.7230(7) -0.1501(3) 0.3014(4) 0.042(2) Uani 1 1 d . . . C31 C 0.8036(8) -0.1565(4) 0.3447(5) 0.055(3) Uani 1 1 d . . . H31 H 0.8644 -0.1798 0.3422 0.066 Uiso 1 1 calc R . . C32 C 0.7993(9) -0.1304(4) 0.3911(5) 0.063(3) Uani 1 1 d . . . H32 H 0.8544 -0.1366 0.4204 0.075 Uiso 1 1 calc R . . C33 C 0.7140(9) -0.0953(4) 0.3943(4) 0.052(3) Uani 1 1 d . . . H33 H 0.711 -0.0764 0.4257 0.063 Uiso 1 1 calc R . . C34 C 0.6334(7) -0.0879(4) 0.3521(3) 0.040(2) Uani 1 1 d . . . H34 H 0.575 -0.0634 0.3544 0.048 Uiso 1 1 calc R . . C35 C 0.7278(7) -0.1811(3) 0.2525(4) 0.049(3) Uani 1 1 d . . . H35 H 0.6914 -0.1612 0.2221 0.059 Uiso 1 1 calc R . . C36 C 0.8499(8) -0.1955(4) 0.2388(5) 0.063(3) Uani 1 1 d . . . H36A H 0.844 -0.2153 0.2063 0.094 Uiso 1 1 calc R . . H36B H 0.8886 -0.215 0.2679 0.094 Uiso 1 1 calc R . . H36C H 0.8951 -0.1655 0.2336 0.094 Uiso 1 1 calc R . . C37 C 0.6545(9) -0.2284(4) 0.2558(5) 0.065(3) Uani 1 1 d . . . H37A H 0.6587 -0.2481 0.2235 0.097 Uiso 1 1 calc R . . H37B H 0.5734 -0.2194 0.2595 0.097 Uiso 1 1 calc R . . H37C H 0.6846 -0.248 0.2866 0.097 Uiso 1 1 calc R . . C38 C 0.4768(6) -0.1014(3) 0.0950(3) 0.0303(19) Uani 1 1 d . . . C39 C 0.5234(7) -0.1446(3) 0.0734(4) 0.035(2) Uani 1 1 d . B . C40 C 0.5325(7) -0.1460(4) 0.0187(4) 0.044(2) Uani 1 1 d . . . H40 H 0.5627 -0.175 0.0037 0.053 Uiso 1 1 calc R . . C41 C 0.4992(7) -0.1068(3) -0.0142(4) 0.041(2) Uani 1 1 d . . . H41 H 0.5059 -0.109 -0.0512 0.05 Uiso 1 1 calc R . . C42 C 0.4565(7) -0.0647(3) 0.0072(4) 0.041(2) Uani 1 1 d . . . H42 H 0.4339 -0.0373 -0.0148 0.049 Uiso 1 1 calc R . . C43 C 0.4466(7) -0.0624(3) 0.0604(3) 0.036(2) Uani 1 1 d . . . H43 H 0.4177 -0.0327 0.0746 0.043 Uiso 1 1 calc R . . C44 C 0.5645(8) -0.1876(3) 0.1081(4) 0.048(2) Uani 1 1 d . . . H44 H 0.5527 -0.1789 0.1455 0.058 Uiso 1 1 calc R A 1 C45 C 0.6944(9) -0.1969(4) 0.1047(5) 0.067(3) Uani 1 1 d . B . H45A H 0.7197 -0.2247 0.1278 0.1 Uiso 1 1 calc R . . H45B H 0.7385 -0.1672 0.116 0.1 Uiso 1 1 calc R . . H45C H 0.7083 -0.2049 0.0681 0.1 Uiso 1 1 calc R . . C46 C 0.4978(9) -0.2355(4) 0.0939(5) 0.062(3) Uani 1 1 d . B 1 H46A H 0.5274 -0.262 0.1178 0.093 Uiso 1 1 calc R B 1 H46B H 0.5084 -0.2447 0.0573 0.093 Uiso 1 1 calc R B 1 H46C H 0.415 -0.2303 0.0976 0.093 Uiso 1 1 calc R B 1 C47 C 1.0507(8) 0.0385(4) 0.1721(5) 0.063(3) Uani 1 1 d . C 1 H47A H 1.0838 0.0317 0.2088 0.076 Uiso 1 1 calc R C 1 H47B H 1.0864 0.0693 0.1599 0.076 Uiso 1 1 calc R C 1 C48 C 1.0762(9) -0.0035(5) 0.1369(5) 0.084(4) Uani 1 1 d . C 1 H48A H 1.1605 -0.008 0.1377 0.126 Uiso 1 1 calc R C 1 H48B H 1.0441 0.0037 0.1006 0.126 Uiso 1 1 calc R C 1 H48C H 1.0408 -0.0338 0.1493 0.126 Uiso 1 1 calc R C 1 C49 C 0.8965(10) 0.0805(5) 0.2094(6) 0.082(4) Uani 1 1 d . C 1 H49A H 0.8151 0.0743 0.2168 0.099 Uiso 1 1 calc R C 1 H49B H 0.9464 0.0757 0.2428 0.099 Uiso 1 1 calc R C 1 C50 C 0.9065(12) 0.1299(5) 0.1928(8) 0.133(7) Uani 1 1 d . C 1 H50A H 0.883 0.1522 0.2205 0.2 Uiso 1 1 calc R C 1 H50B H 0.8561 0.1353 0.1601 0.2 Uiso 1 1 calc R C 1 H50C H 0.9873 0.1367 0.1864 0.2 Uiso 1 1 calc R C 1 C51 C 0.7817(13) -0.0592(7) 0.0439(6) 0.120(7) Uani 1 1 d . C 1 H51A H 0.7372 -0.0735 0.0718 0.144 Uiso 1 1 calc R C 1 H51B H 0.7286 -0.0572 0.0111 0.144 Uiso 1 1 calc R C 1 C52 C 0.8743(12) -0.0926(6) 0.0348(7) 0.113(6) Uani 1 1 d . C 1 H52A H 0.8418 -0.1251 0.0245 0.169 Uiso 1 1 calc R C 1 H52B H 0.9266 -0.0959 0.0672 0.169 Uiso 1 1 calc R C 1 H52C H 0.9177 -0.0797 0.0063 0.169 Uiso 1 1 calc R C 1 C53 C 0.8386(11) 0.0232(8) 0.0182(5) 0.104(6) Uani 1 1 d . C 1 H53A H 0.7758 0.0207 -0.0109 0.125 Uiso 1 1 calc R C 1 H53B H 0.9129 0.0142 0.0041 0.125 Uiso 1 1 calc R C 1 C54 C 0.8453(12) 0.0744(7) 0.0386(7) 0.114(6) Uani 1 1 d . C 1 H54A H 0.8609 0.0971 0.0099 0.17 Uiso 1 1 calc R C 1 H54B H 0.908 0.0768 0.0672 0.17 Uiso 1 1 calc R C 1 H54C H 0.7713 0.0833 0.0522 0.17 Uiso 1 1 calc R C 1 C55 C 0.1802(11) 0.0942(4) 0.4509(5) 0.071(3) Uani 1 1 d . D 1 H55A H 0.2205 0.096 0.487 0.085 Uiso 1 1 calc R D 1 H55B H 0.2331 0.108 0.426 0.085 Uiso 1 1 calc R D 1 C56 C 0.0772(12) 0.1237(5) 0.4488(9) 0.144(8) Uani 1 1 d . D 1 H56A H 0.098 0.158 0.4581 0.216 Uiso 1 1 calc R D 1 H56B H 0.0253 0.1107 0.4741 0.216 Uiso 1 1 calc R D 1 H56C H 0.0378 0.1226 0.413 0.216 Uiso 1 1 calc R D 1 C57 C 0.1817(10) 0.0110(4) 0.4804(5) 0.070(3) Uani 1 1 d . D 1 H57A H 0.1376 0.0214 0.5102 0.084 Uiso 1 1 calc R D 1 H57B H 0.2656 0.013 0.4922 0.084 Uiso 1 1 calc R D 1 C58 C 0.1503(10) -0.0419(4) 0.4651(5) 0.070(3) Uani 1 1 d . D 1 H58A H 0.1689 -0.0637 0.4956 0.104 Uiso 1 1 calc R D 1 H58B H 0.1947 -0.0523 0.4359 0.104 Uiso 1 1 calc R D 1 H58C H 0.0669 -0.044 0.454 0.104 Uiso 1 1 calc R D 1 C59 C -0.0673(8) -0.0162(4) 0.3290(5) 0.069(3) Uani 1 1 d . D 1 H59A H -0.0983 -0.0473 0.343 0.083 Uiso 1 1 calc R D 1 H59B H -0.1033 -0.0113 0.2924 0.083 Uiso 1 1 calc R D 1 C60 C -0.0973(9) 0.0262(4) 0.3627(5) 0.071(3) Uani 1 1 d . D 1 H60A H -0.182 0.0283 0.363 0.106 Uiso 1 1 calc R D 1 H60B H -0.0679 0.057 0.3484 0.106 Uiso 1 1 calc R D 1 H60C H -0.0619 0.0212 0.3989 0.106 Uiso 1 1 calc R D 1 C61 C 0.0895(10) -0.0580(6) 0.2907(6) 0.089(4) Uani 1 1 d . D 1 H61A H 0.0302 -0.06 0.26 0.107 Uiso 1 1 calc R D 1 H61B H 0.1647 -0.0488 0.2775 0.107 Uiso 1 1 calc R D 1 C62 C 0.0996(12) -0.1045(6) 0.3167(7) 0.120(6) Uani 1 1 d . D 1 H62A H 0.1223 -0.1298 0.2919 0.179 Uiso 1 1 calc R D 1 H62B H 0.0248 -0.1135 0.3294 0.179 Uiso 1 1 calc R D 1 H62C H 0.1589 -0.1024 0.3469 0.179 Uiso 1 1 calc R D 1 C63 C 1.0727(14) -0.2321(7) 0.4248(7) 0.116(6) Uani 1 1 d . E 1 H63A H 1.0542 -0.2203 0.3881 0.139 Uiso 1 1 calc R E 1 H63B H 1.1046 -0.2661 0.4233 0.139 Uiso 1 1 calc R E 1 C64 C 1.1586(17) -0.1999(8) 0.4519(9) 0.169(9) Uani 1 1 d . E 1 H64A H 1.2287 -0.1996 0.4328 0.253 Uiso 1 1 calc R E 1 H64B H 1.1781 -0.2121 0.4881 0.253 Uiso 1 1 calc R E 1 H64C H 1.1272 -0.1663 0.4532 0.253 Uiso 1 1 calc R E 1 C65 C 0.8818(13) -0.2655(5) 0.4285(5) 0.085(4) Uani 1 1 d . E 1 H65A H 0.9117 -0.2999 0.4289 0.102 Uiso 1 1 calc R E 1 H65B H 0.8601 -0.256 0.3912 0.102 Uiso 1 1 calc R E 1 C66 C 0.7784(15) -0.2631(6) 0.4585(7) 0.121(6) Uani 1 1 d . E 1 H66A H 0.7186 -0.2856 0.4425 0.181 Uiso 1 1 calc R E 1 H66B H 0.7482 -0.2292 0.4577 0.181 Uiso 1 1 calc R E 1 H66C H 0.7998 -0.273 0.4953 0.181 Uiso 1 1 calc R E 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0183(4) 0.0278(4) 0.0381(5) -0.0005(4) 0.0008(3) -0.0023(3) Y2 0.0188(4) 0.0262(4) 0.0359(5) -0.0011(4) -0.0002(3) -0.0015(3) Li1 0.035(8) 0.060(11) 0.051(11) 0.002(8) -0.013(7) -0.009(7) Li2 0.030(8) 0.041(9) 0.058(11) 0.005(8) -0.004(7) -0.010(6) Cl1 0.0203(9) 0.0369(12) 0.0413(13) -0.0061(10) -0.0031(8) 0.0005(8) Cl2 0.0212(10) 0.0402(13) 0.0526(15) 0.0050(10) 0.0055(9) 0.0023(8) Cl3 0.0274(10) 0.0425(13) 0.0535(15) 0.0121(11) 0.0043(10) -0.0022(9) Cl4 0.0193(9) 0.0328(11) 0.0436(13) -0.0084(9) -0.0040(8) -0.0008(8) Cl5 0.0227(10) 0.0412(13) 0.0672(17) 0.0011(11) 0.0079(10) 0.0021(9) Cl6 0.0346(11) 0.0413(13) 0.0465(14) 0.0107(10) 0.0031(10) -0.0028(9) O1 0.028(3) 0.064(5) 0.068(5) -0.015(4) -0.002(3) -0.011(3) O2 0.052(4) 0.135(8) 0.052(5) -0.023(5) 0.006(4) -0.034(5) O3 0.050(4) 0.057(4) 0.041(4) -0.002(3) -0.004(3) -0.004(3) O4 0.029(3) 0.057(4) 0.068(5) -0.014(4) 0.002(3) -0.015(3) O5 0.117(8) 0.076(6) 0.080(7) 0.005(5) 0.015(6) 0.026(6) N1 0.027(4) 0.027(4) 0.033(4) 0.003(3) -0.004(3) 0.001(3) N2 0.023(3) 0.035(4) 0.043(5) -0.008(3) -0.003(3) -0.007(3) N3 0.023(3) 0.035(4) 0.039(4) 0.000(3) 0.000(3) 0.004(3) N4 0.025(3) 0.025(4) 0.040(5) -0.001(3) 0.000(3) -0.001(3) C1 0.041(5) 0.023(5) 0.041(6) 0.002(4) 0.017(4) 0.003(4) C2 0.019(4) 0.036(5) 0.046(6) -0.003(4) 0.001(4) -0.006(3) C3 0.020(4) 0.022(4) 0.056(6) -0.006(4) -0.001(4) 0.000(3) C4 0.042(5) 0.043(6) 0.056(7) 0.011(5) 0.015(5) -0.009(4) C5 0.030(5) 0.049(6) 0.054(7) -0.006(5) -0.005(4) -0.006(4) C6 0.022(4) 0.038(5) 0.050(6) 0.006(4) 0.004(4) -0.009(4) C7 0.020(4) 0.034(5) 0.057(6) 0.013(4) 0.006(4) 0.002(3) C8 0.033(5) 0.047(6) 0.076(8) 0.016(6) 0.004(5) 0.009(4) C9 0.032(5) 0.074(8) 0.067(8) 0.019(6) -0.009(5) 0.002(5) C10 0.047(6) 0.058(7) 0.045(6) -0.001(5) -0.006(5) -0.005(5) C11 0.030(5) 0.030(5) 0.053(6) 0.009(4) 0.003(4) 0.001(4) C12 0.028(5) 0.037(5) 0.070(7) 0.000(5) 0.007(5) 0.001(4) C13 0.032(5) 0.046(6) 0.094(9) 0.007(6) 0.018(5) 0.007(4) C14 0.050(6) 0.045(6) 0.109(10) -0.003(6) 0.015(6) -0.004(5) C15 0.025(4) 0.041(6) 0.051(6) -0.002(5) 0.002(4) -0.009(4) C16 0.035(5) 0.052(6) 0.057(7) -0.014(5) 0.006(5) -0.010(4) C17 0.045(6) 0.099(10) 0.059(8) -0.043(7) 0.013(6) -0.010(6) C18 0.061(7) 0.107(11) 0.044(8) 0.010(8) -0.003(6) -0.024(7) C19 0.045(6) 0.073(8) 0.062(8) 0.020(7) -0.010(5) -0.020(6) C20 0.041(5) 0.055(7) 0.059(8) -0.003(5) -0.009(5) -0.009(5) C21 0.050(6) 0.049(6) 0.065(7) -0.020(5) 0.020(5) -0.003(5) C22 0.056(7) 0.065(8) 0.095(10) -0.015(7) 0.012(6) 0.002(6) C23 0.074(9) 0.058(8) 0.165(15) -0.022(9) 0.014(9) -0.010(7) C24 0.028(4) 0.029(5) 0.036(5) 0.003(4) 0.003(4) 0.000(3) C25 0.022(4) 0.021(4) 0.051(6) -0.002(4) -0.001(4) 0.000(3) C26 0.026(4) 0.027(5) 0.049(6) -0.001(4) -0.002(4) 0.002(3) C27 0.038(5) 0.051(6) 0.040(6) 0.003(4) 0.009(4) -0.007(4) C28 0.024(4) 0.059(6) 0.045(6) -0.009(5) -0.003(4) -0.010(4) C29 0.021(4) 0.028(5) 0.055(6) 0.016(4) 0.002(4) 0.002(3) C30 0.031(5) 0.037(5) 0.056(7) 0.009(5) -0.006(4) -0.006(4) C31 0.025(5) 0.067(7) 0.070(8) 0.017(6) -0.013(5) 0.006(5) C32 0.044(6) 0.083(8) 0.056(8) 0.028(6) -0.024(5) -0.008(6) C33 0.055(6) 0.066(7) 0.033(6) 0.010(5) -0.009(5) -0.003(5) C34 0.038(5) 0.060(6) 0.020(5) 0.010(4) -0.006(4) -0.009(4) C35 0.028(5) 0.043(6) 0.074(8) 0.009(5) -0.003(5) 0.004(4) C36 0.029(5) 0.061(7) 0.099(9) 0.006(6) 0.006(5) 0.020(5) C37 0.052(6) 0.039(6) 0.103(10) -0.002(6) 0.008(6) -0.003(5) C38 0.019(4) 0.034(5) 0.037(5) -0.005(4) -0.002(3) -0.007(3) C39 0.028(4) 0.033(5) 0.043(6) -0.011(4) -0.005(4) -0.002(4) C40 0.038(5) 0.047(6) 0.047(6) -0.019(5) 0.001(4) -0.004(4) C41 0.041(5) 0.047(6) 0.036(6) 0.000(5) 0.003(4) -0.006(4) C42 0.040(5) 0.038(5) 0.044(6) 0.007(5) -0.007(4) -0.013(4) C43 0.032(5) 0.042(5) 0.032(6) 0.000(4) -0.004(4) -0.009(4) C44 0.050(6) 0.044(6) 0.049(6) -0.011(5) 0.000(5) 0.009(5) C45 0.051(6) 0.068(8) 0.080(9) -0.002(6) 0.001(6) 0.021(6) C46 0.067(7) 0.042(6) 0.075(8) 0.010(6) 0.002(6) -0.003(5) C47 0.035(5) 0.073(8) 0.079(9) -0.012(6) -0.011(5) -0.004(5) C48 0.033(6) 0.120(11) 0.098(10) -0.043(9) -0.006(6) 0.010(6) C49 0.053(7) 0.083(10) 0.112(11) -0.034(8) 0.014(7) -0.024(6) C50 0.083(10) 0.087(11) 0.24(2) -0.058(13) 0.075(12) -0.025(8) C51 0.092(11) 0.188(17) 0.085(11) -0.089(11) 0.033(8) -0.061(11) C52 0.070(9) 0.136(14) 0.136(14) -0.038(11) 0.029(9) -0.030(9) C53 0.053(8) 0.208(19) 0.052(9) 0.026(11) 0.010(6) 0.035(10) C54 0.074(10) 0.161(17) 0.108(14) 0.050(13) 0.021(9) 0.019(11) C55 0.088(9) 0.054(7) 0.068(8) -0.008(6) -0.006(7) -0.014(6) C56 0.071(10) 0.052(9) 0.31(3) -0.028(12) 0.027(13) -0.010(7) C57 0.069(8) 0.083(9) 0.055(8) 0.007(7) -0.001(6) 0.009(7) C58 0.069(7) 0.071(8) 0.069(8) 0.015(7) 0.006(6) -0.011(6) C59 0.025(5) 0.073(8) 0.106(10) -0.026(7) -0.012(5) -0.008(5) C60 0.039(6) 0.083(9) 0.088(9) -0.021(7) -0.007(6) 0.010(6) C61 0.053(7) 0.105(12) 0.111(12) -0.010(10) 0.016(7) -0.026(7) C62 0.072(10) 0.111(13) 0.181(18) -0.015(13) 0.041(10) -0.016(9) C63 0.094(12) 0.138(15) 0.121(14) 0.044(12) 0.042(11) 0.049(11) C64 0.119(16) 0.18(2) 0.21(2) 0.066(18) -0.002(16) -0.023(15) C65 0.122(12) 0.061(8) 0.070(9) -0.007(7) -0.001(9) 0.027(8) C66 0.129(14) 0.132(15) 0.106(13) -0.011(11) 0.030(11) 0.014(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y1 N1 2.315(6) . ? Y1 N2 2.317(6) . ? Y1 Cl2 2.611(2) . ? Y1 Cl3 2.660(2) . ? Y1 Cl4 2.696(2) . ? Y1 Cl1 2.705(2) . ? Y2 N4 2.300(6) . ? Y2 N3 2.330(7) . ? Y2 Cl5 2.616(2) . ? Y2 Cl6 2.660(2) . ? Y2 Cl1 2.684(2) . ? Y2 Cl4 2.707(2) . ? Li1 O1 1.921(16) . ? Li1 O2 1.961(19) . ? Li1 Cl6 2.385(16) . ? Li1 Cl5 2.391(17) . ? Li2 O3 1.941(18) . ? Li2 O4 1.944(15) . ? Li2 Cl2 2.391(15) . ? Li2 Cl3 2.391(15) . ? O1 C47 1.414(11) . ? O1 C49 1.452(13) . ? O2 C53 1.411(16) . ? O2 C51 1.449(16) . ? O3 C57 1.395(12) . ? O3 C55 1.451(12) . ? O4 C59 1.417(10) . ? O4 C61 1.488(15) . ? O5 C63 1.405(16) . ? O5 C65 1.433(15) . ? N1 C1 1.350(10) . ? N1 C6 1.448(10) . ? N2 C3 1.353(10) . ? N2 C15 1.429(11) . ? N3 C24 1.332(10) . ? N3 C29 1.457(10) . ? N4 C26 1.342(10) . ? N4 C38 1.413(10) . ? C1 C2 1.414(11) . ? C1 C4 1.522(11) . ? C2 C3 1.388(12) . ? C3 C5 1.506(11) . ? C6 C11 1.372(12) . ? C6 C7 1.408(11) . ? C7 C8 1.378(13) . ? C7 C12 1.503(13) . ? C8 C9 1.347(14) . ? C9 C10 1.378(14) . ? C10 C11 1.377(12) . ? C12 C14 1.513(12) . ? C12 C13 1.537(11) . ? C15 C20 1.372(13) . ? C15 C16 1.409(13) . ? C16 C17 1.409(15) . ? C16 C21 1.524(14) . ? C17 C18 1.369(16) . ? C18 C19 1.350(16) . ? C19 C20 1.389(15) . ? C21 C22 1.521(13) . ? C21 C23 1.528(14) . ? C24 C25 1.403(11) . ? C24 C27 1.519(11) . ? C25 C26 1.402(12) . ? C26 C28 1.516(11) . ? C29 C34 1.363(12) . ? C29 C30 1.405(12) . ? C30 C31 1.383(13) . ? C30 C35 1.502(13) . ? C31 C32 1.376(15) . ? C32 C33 1.374(14) . ? C33 C34 1.370(12) . ? C35 C36 1.532(12) . ? C35 C37 1.540(13) . ? C38 C43 1.395(11) . ? C38 C39 1.415(11) . ? C39 C40 1.401(12) . ? C39 C44 1.505(12) . ? C40 C41 1.380(13) . ? C41 C42 1.372(12) . ? C42 C43 1.365(12) . ? C44 C46 1.531(13) . ? C44 C45 1.532(13) . ? C47 C48 1.488(14) . ? C49 C50 1.406(18) . ? C51 C52 1.434(19) . ? C53 C54 1.47(2) . ? C55 C56 1.429(16) . ? C57 C58 1.516(15) . ? C59 C60 1.486(14) . ? C61 C62 1.419(18) . ? C63 C64 1.44(2) . ? C65 C66 1.474(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N2 80.1(2) . . ? N1 Y1 Cl2 89.34(16) . . ? N2 Y1 Cl2 103.77(17) . . ? N1 Y1 Cl3 172.51(16) . . ? N2 Y1 Cl3 101.77(19) . . ? Cl2 Y1 Cl3 83.17(7) . . ? N1 Y1 Cl4 91.30(17) . . ? N2 Y1 Cl4 159.49(17) . . ? Cl2 Y1 Cl4 94.64(7) . . ? Cl3 Y1 Cl4 89.19(7) . . ? N1 Y1 Cl1 96.22(16) . . ? N2 Y1 Cl1 83.88(17) . . ? Cl2 Y1 Cl1 171.26(7) . . ? Cl3 Y1 Cl1 91.20(7) . . ? Cl4 Y1 Cl1 78.55(6) . . ? N4 Y2 N3 78.5(2) . . ? N4 Y2 Cl5 101.05(16) . . ? N3 Y2 Cl5 92.23(16) . . ? N4 Y2 Cl6 103.92(18) . . ? N3 Y2 Cl6 174.83(16) . . ? Cl5 Y2 Cl6 82.86(7) . . ? N4 Y2 Cl1 159.40(17) . . ? N3 Y2 Cl1 89.83(17) . . ? Cl5 Y2 Cl1 96.30(7) . . ? Cl6 Y2 Cl1 89.10(7) . . ? N4 Y2 Cl4 85.61(16) . . ? N3 Y2 Cl4 96.15(16) . . ? Cl5 Y2 Cl4 170.21(7) . . ? Cl6 Y2 Cl4 88.60(7) . . ? Cl1 Y2 Cl4 78.73(6) . . ? O1 Li1 O2 118.2(9) . . ? O1 Li1 Cl6 117.9(8) . . ? O2 Li1 Cl6 102.4(6) . . ? O1 Li1 Cl5 107.9(7) . . ? O2 Li1 Cl5 114.0(8) . . ? Cl6 Li1 Cl5 93.9(6) . . ? O3 Li2 O4 119.4(8) . . ? O3 Li2 Cl2 112.9(7) . . ? O4 Li2 Cl2 107.4(7) . . ? O3 Li2 Cl3 106.8(7) . . ? O4 Li2 Cl3 113.5(7) . . ? Cl2 Li2 Cl3 94.1(5) . . ? Y2 Cl1 Y1 101.55(6) . . ? Li2 Cl2 Y1 92.0(4) . . ? Li2 Cl3 Y1 90.8(4) . . ? Y1 Cl4 Y2 101.17(6) . . ? Li1 Cl5 Y2 91.9(4) . . ? Li1 Cl6 Y2 91.0(4) . . ? C47 O1 C49 112.2(8) . . ? C47 O1 Li1 128.9(8) . . ? C49 O1 Li1 118.0(8) . . ? C53 O2 C51 116.1(12) . . ? C53 O2 Li1 129.2(11) . . ? C51 O2 Li1 114.4(9) . . ? C57 O3 C55 112.5(8) . . ? C57 O3 Li2 121.9(8) . . ? C55 O3 Li2 117.4(8) . . ? C59 O4 C61 112.3(8) . . ? C59 O4 Li2 127.7(8) . . ? C61 O4 Li2 119.7(7) . . ? C63 O5 C65 114.9(12) . . ? C1 N1 C6 116.4(7) . . ? C1 N1 Y1 117.7(5) . . ? C6 N1 Y1 123.2(5) . . ? C3 N2 C15 117.3(7) . . ? C3 N2 Y1 117.6(6) . . ? C15 N2 Y1 122.8(5) . . ? C24 N3 C29 116.4(7) . . ? C24 N3 Y2 119.2(5) . . ? C29 N3 Y2 121.2(5) . . ? C26 N4 C38 116.9(7) . . ? C26 N4 Y2 119.2(6) . . ? C38 N4 Y2 122.3(5) . . ? N1 C1 C2 123.5(8) . . ? N1 C1 C4 120.5(8) . . ? C2 C1 C4 116.0(7) . . ? C3 C2 C1 129.9(7) . . ? N2 C3 C2 124.3(7) . . ? N2 C3 C5 119.8(8) . . ? C2 C3 C5 115.9(7) . . ? C11 C6 C7 120.6(8) . . ? C11 C6 N1 119.6(8) . . ? C7 C6 N1 119.7(8) . . ? C8 C7 C6 116.4(9) . . ? C8 C7 C12 122.6(8) . . ? C6 C7 C12 120.9(8) . . ? C9 C8 C7 123.4(9) . . ? C8 C9 C10 119.6(10) . . ? C11 C10 C9 119.4(10) . . ? C6 C11 C10 120.5(8) . . ? C7 C12 C14 111.3(8) . . ? C7 C12 C13 113.6(8) . . ? C14 C12 C13 110.9(8) . . ? C20 C15 C16 119.8(10) . . ? C20 C15 N2 119.8(9) . . ? C16 C15 N2 120.3(8) . . ? C15 C16 C17 116.3(10) . . ? C15 C16 C21 122.0(9) . . ? C17 C16 C21 121.7(10) . . ? C18 C17 C16 123.5(11) . . ? C19 C18 C17 118.2(11) . . ? C18 C19 C20 121.2(11) . . ? C15 C20 C19 120.9(10) . . ? C22 C21 C16 110.6(8) . . ? C22 C21 C23 109.3(9) . . ? C16 C21 C23 113.2(10) . . ? N3 C24 C25 122.6(8) . . ? N3 C24 C27 121.0(7) . . ? C25 C24 C27 116.4(7) . . ? C26 C25 C24 129.8(7) . . ? N4 C26 C25 123.4(7) . . ? N4 C26 C28 120.3(8) . . ? C25 C26 C28 116.3(7) . . ? C34 C29 C30 120.7(8) . . ? C34 C29 N3 121.2(7) . . ? C30 C29 N3 118.1(8) . . ? C31 C30 C29 116.6(9) . . ? C31 C30 C35 120.9(9) . . ? C29 C30 C35 122.5(8) . . ? C32 C31 C30 122.7(10) . . ? C33 C32 C31 119.1(9) . . ? C34 C33 C32 119.7(10) . . ? C29 C34 C33 121.3(9) . . ? C30 C35 C36 115.6(8) . . ? C30 C35 C37 110.8(8) . . ? C36 C35 C37 108.9(8) . . ? C43 C38 N4 121.0(7) . . ? C43 C38 C39 117.6(8) . . ? N4 C38 C39 121.4(8) . . ? C40 C39 C38 118.0(8) . . ? C40 C39 C44 120.6(8) . . ? C38 C39 C44 121.4(8) . . ? C41 C40 C39 122.5(9) . . ? C42 C41 C40 119.1(9) . . ? C43 C42 C41 119.7(9) . . ? C42 C43 C38 123.1(9) . . ? C39 C44 C46 112.8(8) . . ? C39 C44 C45 110.7(8) . . ? C46 C44 C45 108.8(8) . . ? O1 C47 C48 108.8(8) . . ? C50 C49 O1 113.8(12) . . ? C52 C51 O2 116.1(12) . . ? O2 C53 C54 109.3(12) . . ? C56 C55 O3 112.5(10) . . ? O3 C57 C58 110.6(9) . . ? O4 C59 C60 110.1(8) . . ? C62 C61 O4 109.1(13) . . ? O5 C63 C64 110.7(17) . . ? O5 C65 C66 110.6(12) . . ? #===END data_(3b)-mar2603 _database_code_depnum_ccdc_archive 'CCDC 684942' _audit_creation_date 2003-04-01T10:48:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C66 H106 Cl6 Li2 N4 O4 Y2, C4 H10 O' _chemical_formula_sum 'C70 H116 Cl6 Li2 N4 O5 Y2' _chemical_formula_weight 1498.07 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _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 30.2936(3) _cell_length_b 13.7202(2) _cell_length_c 22.7889(2) _cell_angle_alpha 90 _cell_angle_beta 122.693(1) _cell_angle_gamma 90 _cell_volume 7971.28(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25463 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4907 _exptl_absorpt_correction_T_max 0.5621 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_number 41119 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 6999 _reflns_number_gt 6035 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0271P)^2^+15.1179P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00042(6) _refine_ls_number_reflns 6999 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.071 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.445 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.054 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Y Y 0.189481(8) 0.771074(17) 0.020514(11) 0.01867(8) Uani 1 1 d . . . Cl1 Cl 0.28895(2) 0.82912(4) 0.06164(3) 0.02576(15) Uani 1 1 d . . . Cl2 Cl 0.23301(2) 0.65886(4) 0.13162(3) 0.02770(15) Uani 1 1 d . . . Cl3 Cl 0.19918(2) 0.90586(4) 0.10800(3) 0.02615(14) Uani 1 1 d . . . O1 O 0.24316(8) 0.82416(14) 0.27326(10) 0.0377(5) Uani 1 1 d . . . O2 O 0.33717(7) 0.81966(15) 0.24637(10) 0.0395(5) Uani 1 1 d . . . O3 O 0 1.2660(5) -0.25 0.1263(19) Uani 1 2 d S . . N1 N 0.13096(7) 0.87841(14) -0.06739(10) 0.0211(4) Uani 1 1 d . . . N2 N 0.11135(7) 0.67655(14) -0.03584(10) 0.0215(4) Uani 1 1 d . . . C1 C 0.09358(9) 0.85118(18) -0.13152(12) 0.0234(5) Uani 1 1 d . . . C2 C 0.07061(9) 0.75846(18) -0.14794(12) 0.0264(6) Uani 1 1 d . . . H2 H 0.0468 0.7469 -0.1964 0.032 Uiso 1 1 calc R . . C3 C 0.07687(9) 0.68001(18) -0.10489(12) 0.0240(5) Uani 1 1 d . . . C4 C 0.07305(10) 0.9231(2) -0.19094(13) 0.0334(6) Uani 1 1 d . . . H4A H 0.0544 0.9758 -0.1842 0.05 Uiso 1 1 calc R . . H4B H 0.049 0.8898 -0.2351 0.05 Uiso 1 1 calc R . . H4C H 0.1025 0.9504 -0.1921 0.05 Uiso 1 1 calc R . . C5 C 0.04013(11) 0.5947(2) -0.14188(14) 0.0365(7) Uani 1 1 d . . . H5A H 0.0586 0.5438 -0.1506 0.055 Uiso 1 1 calc R . . H5B H 0.0097 0.6168 -0.1863 0.055 Uiso 1 1 calc R . . H5C H 0.0284 0.5683 -0.1126 0.055 Uiso 1 1 calc R . . C6 C 0.14701(9) 0.97936(18) -0.05746(12) 0.0225(5) Uani 1 1 d . . . C7 C 0.12204(10) 1.05483(18) -0.04437(13) 0.0270(6) Uani 1 1 d . . . C8 C 0.14404(11) 1.1477(2) -0.03456(16) 0.0401(7) Uani 1 1 d . . . H8 H 0.1278 1.2006 -0.0264 0.048 Uiso 1 1 calc R . . C9 C 0.18831(12) 1.1665(2) -0.03608(17) 0.0450(8) Uani 1 1 d . . . H9 H 0.2019 1.2308 -0.0287 0.054 Uiso 1 1 calc R . . C10 C 0.21243(11) 1.0915(2) -0.04832(15) 0.0386(7) Uani 1 1 d . . . H10 H 0.243 1.1032 -0.0492 0.046 Uiso 1 1 calc R . . C11 C 0.19149(9) 0.9992(2) -0.05934(13) 0.0288(6) Uani 1 1 d . . . H11 H 0.2078 0.9474 -0.0685 0.035 Uiso 1 1 calc R . . C12 C 0.07298(10) 1.04849(19) -0.03940(14) 0.0313(6) Uani 1 1 d . . . C13 C 0.02938(12) 1.1131(2) -0.09682(18) 0.0508(8) Uani 1 1 d . . . H13A H 0.043 1.179 -0.0935 0.076 Uiso 1 1 calc R . . H13B H -0.0003 1.1159 -0.0908 0.076 Uiso 1 1 calc R . . H13C H 0.0177 1.0855 -0.1427 0.076 Uiso 1 1 calc R . . C14 C 0.08793(12) 1.0877(2) 0.03236(17) 0.0455(8) Uani 1 1 d . . . H14A H 0.1026 1.1534 0.039 0.068 Uiso 1 1 calc R . . H14B H 0.1141 1.0446 0.069 0.068 Uiso 1 1 calc R . . H14C H 0.0566 1.0901 0.0348 0.068 Uiso 1 1 calc R . . C15 C 0.05043(11) 0.9467(2) -0.04623(18) 0.0429(7) Uani 1 1 d . . . H15A H 0.0403 0.9189 -0.0915 0.064 Uiso 1 1 calc R . . H15B H 0.0196 0.9508 -0.0429 0.064 Uiso 1 1 calc R . . H15C H 0.077 0.9051 -0.0087 0.064 Uiso 1 1 calc R . . C16 C 0.11359(9) 0.58580(18) -0.00155(12) 0.0234(5) Uani 1 1 d . . . C17 C 0.09215(9) 0.57274(18) 0.03958(12) 0.0248(5) Uani 1 1 d . . . C18 C 0.09959(10) 0.4815(2) 0.07063(14) 0.0341(6) Uani 1 1 d . . . H18 H 0.0861 0.4708 0.0992 0.041 Uiso 1 1 calc R . . C19 C 0.12563(11) 0.4059(2) 0.06188(16) 0.0403(7) Uani 1 1 d . . . H19 H 0.1295 0.3449 0.0839 0.048 Uiso 1 1 calc R . . C20 C 0.14589(11) 0.41942(19) 0.02104(16) 0.0373(7) Uani 1 1 d . . . H20 H 0.1636 0.3678 0.0142 0.045 Uiso 1 1 calc R . . C21 C 0.14012(10) 0.50922(19) -0.00987(14) 0.0303(6) Uani 1 1 d . . . H21 H 0.1546 0.5191 -0.0375 0.036 Uiso 1 1 calc R . . C22 C 0.06257(9) 0.65311(19) 0.05275(13) 0.0279(6) Uani 1 1 d . . . C23 C 0.10057(11) 0.7343(2) 0.09665(16) 0.0398(7) Uani 1 1 d . . . H23A H 0.1295 0.7072 0.1405 0.06 Uiso 1 1 calc R . . H23B H 0.0821 0.7836 0.1066 0.06 Uiso 1 1 calc R . . H23C H 0.1146 0.7644 0.071 0.06 Uiso 1 1 calc R . . C24 C 0.01702(10) 0.6952(2) -0.01604(14) 0.0331(6) Uani 1 1 d . . . H24A H -0.0073 0.6428 -0.044 0.05 Uiso 1 1 calc R . . H24B H 0.0308 0.7253 -0.042 0.05 Uiso 1 1 calc R . . H24C H -0.0015 0.7445 -0.006 0.05 Uiso 1 1 calc R . . C25 C 0.03811(12) 0.6127(2) 0.09198(16) 0.0441(7) Uani 1 1 d . . . H25A H 0.0134 0.5604 0.0645 0.066 Uiso 1 1 calc R . . H25B H 0.0195 0.665 0.0992 0.066 Uiso 1 1 calc R . . H25C H 0.0659 0.5868 0.1373 0.066 Uiso 1 1 calc R . . C26 C 0.24250(15) 0.7548(2) 0.3190(2) 0.0572(9) Uani 1 1 d . . . H26A H 0.2058 0.7366 0.3017 0.069 Uiso 1 1 calc R . . H26B H 0.2581 0.7839 0.3659 0.069 Uiso 1 1 calc R . . C27 C 0.27181(16) 0.6685(3) 0.3235(2) 0.0661(10) Uani 1 1 d . . . H27A H 0.2712 0.6215 0.3555 0.099 Uiso 1 1 calc R . . H27B H 0.3082 0.6866 0.341 0.099 Uiso 1 1 calc R . . H27C H 0.2559 0.6391 0.2772 0.099 Uiso 1 1 calc R . . C28 C 0.22897(13) 0.9203(2) 0.28270(17) 0.0478(8) Uani 1 1 d . . . H28A H 0.2397 0.9682 0.2602 0.057 Uiso 1 1 calc R . . H28B H 0.2486 0.9353 0.3332 0.057 Uiso 1 1 calc R . . C29 C 0.17197(15) 0.9318(3) 0.2533(2) 0.0641(10) Uani 1 1 d . . . H29A H 0.1649 0.9984 0.2617 0.096 Uiso 1 1 calc R . . H29B H 0.1611 0.8855 0.2759 0.096 Uiso 1 1 calc R . . H29C H 0.1523 0.9191 0.2031 0.096 Uiso 1 1 calc R . . C30 C 0.36277(11) 0.7280(2) 0.25256(16) 0.0481(8) Uani 1 1 d . . . H30A H 0.3701 0.7243 0.2152 0.058 Uiso 1 1 calc R . . H30B H 0.3384 0.6744 0.2449 0.058 Uiso 1 1 calc R . . C31 C 0.41284(13) 0.7127(3) 0.32109(16) 0.0567(9) Uani 1 1 d . . . H31A H 0.4277 0.6493 0.3211 0.085 Uiso 1 1 calc R . . H31B H 0.406 0.7143 0.3584 0.085 Uiso 1 1 calc R . . H31C H 0.4377 0.7645 0.3287 0.085 Uiso 1 1 calc R . . C32 C 0.36609(13) 0.8999(3) 0.24331(17) 0.0548(9) Uani 1 1 d . . . H32A H 0.3727 0.889 0.2057 0.066 Uiso 1 1 calc R . . H32B H 0.4004 0.9057 0.288 0.066 Uiso 1 1 calc R . . C33 C 0.33532(15) 0.9903(3) 0.2295(2) 0.0813(13) Uani 1 1 d . . . H33A H 0.3549 1.0458 0.2277 0.122 Uiso 1 1 calc R . . H33B H 0.329 1.0006 0.267 0.122 Uiso 1 1 calc R . . H33C H 0.3017 0.9844 0.1849 0.122 Uiso 1 1 calc R . . C34 C 0.0454(3) 1.3167(5) -0.2271(4) 0.144(3) Uani 1 1 d . . . H34A H 0.0562 1.3492 -0.1825 0.173 Uiso 1 1 calc R . . H34B H 0.0388 1.3679 -0.2615 0.173 Uiso 1 1 calc R . . C35 C 0.0867(3) 1.2564(7) -0.2171(4) 0.188(4) Uani 1 1 d . . . H35A H 0.1182 1.296 -0.2009 0.283 Uiso 1 1 calc R . . H35B H 0.0766 1.2249 -0.2613 0.283 Uiso 1 1 calc R . . H35C H 0.0941 1.2065 -0.1822 0.283 Uiso 1 1 calc R . . Li1 Li 0.26040(17) 0.8060(3) 0.2033(2) 0.0325(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 Y 0.01581(12) 0.02001(13) 0.01849(12) -0.00205(10) 0.00814(9) 0.00023(9) Cl1 0.0200(3) 0.0316(4) 0.0267(3) -0.0110(3) 0.0133(3) -0.0057(2) Cl2 0.0292(3) 0.0228(3) 0.0239(3) 0.0016(2) 0.0096(3) 0.0009(3) Cl3 0.0287(3) 0.0234(3) 0.0240(3) -0.0040(2) 0.0127(3) 0.0029(2) O1 0.0521(12) 0.0312(11) 0.0381(11) 0.0047(9) 0.0298(10) 0.0034(9) O2 0.0310(10) 0.0480(13) 0.0356(11) -0.0062(9) 0.0154(9) -0.0042(9) O3 0.105(4) 0.171(6) 0.119(4) 0 0.072(4) 0 N1 0.0203(10) 0.0201(11) 0.0239(10) 0.0007(8) 0.0126(9) 0.0033(8) N2 0.0197(10) 0.0211(11) 0.0230(10) -0.0014(8) 0.0111(9) -0.0023(8) C1 0.0197(12) 0.0285(14) 0.0228(12) 0.0018(11) 0.0120(11) 0.0043(11) C2 0.0232(13) 0.0320(15) 0.0190(12) -0.0025(11) 0.0082(11) -0.0011(11) C3 0.0206(12) 0.0260(14) 0.0243(13) -0.0051(11) 0.0114(11) -0.0015(10) C4 0.0328(15) 0.0339(16) 0.0275(14) 0.0048(12) 0.0124(12) 0.0045(12) C5 0.0336(15) 0.0388(17) 0.0288(14) -0.0070(12) 0.0115(12) -0.0118(13) C6 0.0212(12) 0.0222(13) 0.0206(12) 0.0039(10) 0.0089(10) 0.0020(10) C7 0.0252(13) 0.0248(14) 0.0326(14) 0.0004(11) 0.0167(12) 0.0009(11) C8 0.0426(17) 0.0232(15) 0.0612(19) -0.0045(14) 0.0325(16) -0.0007(13) C9 0.0445(18) 0.0284(16) 0.070(2) -0.0035(15) 0.0358(17) -0.0103(13) C10 0.0297(15) 0.0406(17) 0.0520(18) 0.0045(14) 0.0263(14) -0.0034(13) C11 0.0235(13) 0.0337(16) 0.0320(14) 0.0043(12) 0.0167(12) 0.0053(11) C12 0.0265(14) 0.0258(15) 0.0459(16) -0.0016(12) 0.0225(13) 0.0033(11) C13 0.0370(17) 0.050(2) 0.069(2) 0.0096(17) 0.0307(17) 0.0171(15) C14 0.0441(18) 0.0454(19) 0.061(2) -0.0115(16) 0.0376(17) -0.0012(14) C15 0.0349(16) 0.0383(17) 0.074(2) -0.0068(16) 0.0411(16) -0.0027(13) C16 0.0183(12) 0.0217(13) 0.0234(12) -0.0028(10) 0.0068(10) -0.0058(10) C17 0.0176(12) 0.0246(14) 0.0262(13) -0.0003(11) 0.0077(11) -0.0023(10) C18 0.0321(14) 0.0322(16) 0.0403(15) 0.0058(13) 0.0211(13) -0.0022(12) C19 0.0382(16) 0.0245(15) 0.0564(19) 0.0081(14) 0.0244(15) -0.0008(13) C20 0.0325(15) 0.0209(15) 0.0592(19) -0.0044(13) 0.0252(15) -0.0006(11) C21 0.0279(14) 0.0247(14) 0.0402(15) -0.0043(12) 0.0198(12) -0.0033(11) C22 0.0241(13) 0.0288(14) 0.0306(14) 0.0014(11) 0.0147(12) 0.0002(11) C23 0.0330(15) 0.0405(17) 0.0453(17) -0.0129(14) 0.0207(14) -0.0018(13) C24 0.0269(14) 0.0324(15) 0.0419(16) 0.0034(13) 0.0199(13) 0.0032(12) C25 0.0452(18) 0.050(2) 0.0498(18) 0.0093(15) 0.0342(16) 0.0085(15) C26 0.074(2) 0.049(2) 0.070(2) 0.0202(18) 0.053(2) 0.0120(18) C27 0.082(3) 0.045(2) 0.072(3) 0.0149(19) 0.042(2) 0.0087(19) C28 0.070(2) 0.0364(18) 0.0469(18) -0.0085(14) 0.0379(18) -0.0007(16) C29 0.073(3) 0.053(2) 0.069(2) 0.0016(19) 0.040(2) 0.0206(19) C30 0.0314(16) 0.058(2) 0.0449(17) -0.0060(16) 0.0141(14) 0.0056(15) C31 0.0472(19) 0.077(3) 0.0370(17) 0.0031(17) 0.0174(15) 0.0058(18) C32 0.0413(18) 0.064(2) 0.0453(19) -0.0112(17) 0.0142(16) -0.0178(17) C33 0.050(2) 0.052(2) 0.089(3) -0.002(2) 0.003(2) -0.0135(19) C34 0.180(7) 0.125(5) 0.213(8) 0.001(5) 0.162(7) -0.014(5) C35 0.119(6) 0.274(11) 0.183(8) 0.102(7) 0.089(6) 0.028(6) Li1 0.030(2) 0.034(3) 0.029(2) -0.0002(19) 0.013(2) 0.0027(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N1 2.3427(19) . ? Y N2 2.3768(19) . ? Y Cl3 2.6169(6) . ? Y Cl2 2.6294(6) . ? Y Cl1 2.6727(6) 7_565 ? Y Cl1 2.7462(6) . ? Cl1 Y 2.6727(6) 7_565 ? Cl2 Li1 2.443(5) . ? Cl3 Li1 2.384(4) . ? O1 C26 1.420(3) . ? O1 C28 1.439(3) . ? O1 Li1 1.943(5) . ? O2 C32 1.431(4) . ? O2 C30 1.443(4) . ? O2 Li1 1.985(5) . ? O3 C34 1.368(7) . ? O3 C34 1.368(7) 2_554 ? N1 C1 1.330(3) . ? N1 C6 1.445(3) . ? N2 C3 1.339(3) . ? N2 C16 1.452(3) . ? C1 C2 1.400(3) . ? C1 C4 1.512(3) . ? C2 C3 1.399(3) . ? C3 C5 1.519(3) . ? C6 C11 1.398(3) . ? C6 C7 1.406(3) . ? C7 C8 1.399(4) . ? C7 C12 1.553(3) . ? C8 C9 1.384(4) . ? C9 C10 1.374(4) . ? C10 C11 1.379(4) . ? C12 C15 1.525(4) . ? C12 C14 1.539(4) . ? C12 C13 1.541(4) . ? C16 C21 1.397(3) . ? C16 C17 1.411(3) . ? C17 C18 1.395(4) . ? C17 C22 1.549(3) . ? C18 C19 1.382(4) . ? C19 C20 1.376(4) . ? C20 C21 1.383(4) . ? C22 C23 1.524(4) . ? C22 C24 1.536(4) . ? C22 C25 1.540(4) . ? C26 C27 1.449(5) . ? C28 C29 1.485(5) . ? C30 C31 1.492(4) . ? C32 C33 1.480(5) . ? C34 C35 1.412(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y N2 78.94(7) . . ? N1 Y Cl3 85.92(5) . . ? N2 Y Cl3 117.81(5) . . ? N1 Y Cl2 161.05(5) . . ? N2 Y Cl2 92.06(5) . . ? Cl3 Y Cl2 83.61(2) . . ? N1 Y Cl1 94.75(5) . 7_565 ? N2 Y Cl1 83.67(5) . 7_565 ? Cl3 Y Cl1 158.09(2) . 7_565 ? Cl2 Y Cl1 100.85(2) . 7_565 ? N1 Y Cl1 107.07(5) . . ? N2 Y Cl1 158.67(5) . . ? Cl3 Y Cl1 83.341(19) . . ? Cl2 Y Cl1 87.37(2) . . ? Cl1 Y Cl1 75.52(2) 7_565 . ? Y Cl1 Y 104.48(2) 7_565 . ? Li1 Cl2 Y 88.44(10) . . ? Li1 Cl3 Y 90.01(11) . . ? C26 O1 C28 112.4(2) . . ? C26 O1 Li1 129.3(2) . . ? C28 O1 Li1 118.3(2) . . ? C32 O2 C30 111.3(2) . . ? C32 O2 Li1 129.3(2) . . ? C30 O2 Li1 113.0(2) . . ? C34 O3 C34 118.9(8) . 2_554 ? C1 N1 C6 117.14(19) . . ? C1 N1 Y 124.39(16) . . ? C6 N1 Y 115.69(14) . . ? C3 N2 C16 116.28(19) . . ? C3 N2 Y 122.17(15) . . ? C16 N2 Y 115.70(14) . . ? N1 C1 C2 123.6(2) . . ? N1 C1 C4 119.7(2) . . ? C2 C1 C4 116.7(2) . . ? C3 C2 C1 130.7(2) . . ? N2 C3 C2 125.1(2) . . ? N2 C3 C5 119.8(2) . . ? C2 C3 C5 115.0(2) . . ? C11 C6 C7 120.1(2) . . ? C11 C6 N1 115.5(2) . . ? C7 C6 N1 124.4(2) . . ? C8 C7 C6 116.1(2) . . ? C8 C7 C12 115.6(2) . . ? C6 C7 C12 128.3(2) . . ? C9 C8 C7 123.3(3) . . ? C10 C9 C8 119.7(3) . . ? C9 C10 C11 118.8(2) . . ? C10 C11 C6 122.0(2) . . ? C15 C12 C14 106.7(2) . . ? C15 C12 C13 108.0(2) . . ? C14 C12 C13 109.1(2) . . ? C15 C12 C7 115.9(2) . . ? C14 C12 C7 108.3(2) . . ? C13 C12 C7 108.7(2) . . ? C21 C16 C17 120.0(2) . . ? C21 C16 N2 115.8(2) . . ? C17 C16 N2 124.2(2) . . ? C18 C17 C16 116.4(2) . . ? C18 C17 C22 119.5(2) . . ? C16 C17 C22 124.1(2) . . ? C19 C18 C17 123.3(2) . . ? C20 C19 C18 119.6(3) . . ? C19 C20 C21 119.0(3) . . ? C20 C21 C16 121.6(2) . . ? C23 C22 C24 109.8(2) . . ? C23 C22 C25 108.2(2) . . ? C24 C22 C25 106.2(2) . . ? C23 C22 C17 109.7(2) . . ? C24 C22 C17 111.4(2) . . ? C25 C22 C17 111.5(2) . . ? O1 C26 C27 110.4(3) . . ? O1 C28 C29 113.5(3) . . ? O2 C30 C31 114.5(3) . . ? O2 C32 C33 108.8(3) . . ? O3 C34 C35 112.6(7) . . ? O1 Li1 O2 110.2(2) . . ? O1 Li1 Cl3 104.62(19) . . ? O2 Li1 Cl3 121.5(2) . . ? O1 Li1 Cl2 120.7(2) . . ? O2 Li1 Cl2 107.01(19) . . ? Cl3 Li1 Cl2 92.83(15) . . ? # Attachment 'Revised_4a_5a_5c_8.cif' data_(4a)-jul2803 _database_code_depnum_ccdc_archive 'CCDC 684943' _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C74 H114 Cl6 Li2 N4 O4 Y2, C4 H10 O' _chemical_formula_sum 'C78 H124 Cl6 Li2 N4 O5 Y2' _chemical_formula_weight 1602.21 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 12.3176(2) _cell_length_b 15.3330(2) _cell_length_c 25.3952(5) _cell_angle_alpha 95.054(1) _cell_angle_beta 99.880(1) _cell_angle_gamma 113.161(1) _cell_volume 4279.75(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 69376 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.713 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.584 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4868 _exptl_absorpt_correction_T_max 0.5577 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.53485E-2 _diffrn_orient_matrix_ub_12 0.290017E-1 _diffrn_orient_matrix_ub_13 -0.337464E-1 _diffrn_orient_matrix_ub_21 -0.896483E-1 _diffrn_orient_matrix_ub_22 -0.360578E-1 _diffrn_orient_matrix_ub_23 -0.136798E-1 _diffrn_orient_matrix_ub_31 -0.121739E-1 _diffrn_orient_matrix_ub_32 0.551689E-1 _diffrn_orient_matrix_ub_33 0.17895E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_number 28952 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 24.73 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 14282 _reflns_number_gt 10976 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; All the thf ligands are poorly defined, and were included with 1,2 SADI restraints. For the O2 thf ligand alternative discrete orientations could be discerned and were included with isotropic C atoms and a common isotropic displacement parameter. 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^)+(0.0465P)^2^+9.8924P] 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_number_reflns 14282 _refine_ls_number_parameters 868 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.075 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' 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 Y1 Y 0.90613(4) 0.75428(3) 0.198656(18) 0.03449(14) Uani 1 1 d . . . Y2 Y 1.21083(4) 1.00801(3) 0.278950(18) 0.03589(14) Uani 1 1 d . . . Li1 Li 0.8678(9) 1.0032(7) 0.2326(5) 0.061(3) Uani 1 1 d . . . Li2 Li 1.2576(11) 0.8179(9) 0.1666(5) 0.080(4) Uani 1 1 d . . . Cl1 Cl 1.05438(13) 0.93057(9) 0.17848(5) 0.0472(3) Uani 1 1 d . . . Cl2 Cl 1.05992(13) 0.83574(10) 0.29506(5) 0.0492(3) Uani 1 1 d . . . Cl3 Cl 1.06550(13) 0.70004(11) 0.16777(7) 0.0607(4) Uani 1 1 d . . . Cl4 Cl 0.75850(12) 0.83592(10) 0.20962(6) 0.0490(3) Uani 1 1 d . A . Cl5 Cl 1.05290(13) 1.07526(11) 0.29548(6) 0.0555(4) Uani 1 1 d . A . Cl6 Cl 1.35460(13) 0.94747(11) 0.23811(6) 0.0546(4) Uani 1 1 d . . . O5 O 1.1852(6) 0.6053(4) 0.5166(2) 0.0959(17) Uani 1 1 d . . . N1 N 0.7662(4) 0.6515(3) 0.12100(15) 0.0395(10) Uani 1 1 d . . . N2 N 0.7938(4) 0.6286(3) 0.24083(16) 0.0367(9) Uani 1 1 d . . . N3 N 1.3249(4) 1.0314(3) 0.36786(16) 0.0371(10) Uani 1 1 d . . . N4 N 1.3501(4) 1.1662(3) 0.28214(16) 0.0387(10) Uani 1 1 d . . . C1 C 0.6516(5) 0.5973(4) 0.1224(2) 0.0459(13) Uani 1 1 d . . . C2 C 0.6118(5) 0.5689(4) 0.1690(2) 0.0456(13) Uani 1 1 d . . . H2 H 0.5262 0.5409 0.1644 0.055 Uiso 1 1 calc R . . C3 C 0.6761(5) 0.5744(4) 0.2215(2) 0.0409(12) Uani 1 1 d . . . C4 C 0.5526(6) 0.5580(5) 0.0706(2) 0.0638(17) Uani 1 1 d . . . H4C H 0.4984 0.5908 0.0708 0.096 Uiso 1 1 calc R . . H4B H 0.5061 0.4887 0.0685 0.096 Uiso 1 1 calc R . . H4A H 0.5893 0.5693 0.0392 0.096 Uiso 1 1 calc R . . C5 C 0.6000(5) 0.5094(4) 0.2549(3) 0.0565(15) Uani 1 1 d . . . H5C H 0.652 0.4928 0.2821 0.085 Uiso 1 1 calc R . . H5B H 0.5389 0.4504 0.2311 0.085 Uiso 1 1 calc R . . H5A H 0.5595 0.5426 0.2731 0.085 Uiso 1 1 calc R . . C6 C 0.7965(5) 0.6497(4) 0.0683(2) 0.0461(13) Uani 1 1 d . . . C7 C 0.8060(6) 0.7244(4) 0.0392(2) 0.0581(16) Uani 1 1 d . . . C8 C 0.8302(8) 0.7168(5) -0.0123(2) 0.080(2) Uani 1 1 d . . . H8 H 0.8361 0.7666 -0.0329 0.097 Uiso 1 1 calc R . . C9 C 0.8458(8) 0.6376(6) -0.0336(3) 0.086(2) Uani 1 1 d . . . H9 H 0.8608 0.6329 -0.0689 0.103 Uiso 1 1 calc R . . C10 C 0.8399(7) 0.5660(5) -0.0043(3) 0.072(2) Uani 1 1 d . . . H10 H 0.8523 0.5127 -0.0193 0.086 Uiso 1 1 calc R . . C11 C 0.8160(6) 0.5701(4) 0.0470(2) 0.0525(14) Uani 1 1 d . . . C12 C 0.7894(7) 0.8126(5) 0.0606(2) 0.072(2) Uani 1 1 d . . . H12 H 0.8019 0.8179 0.1009 0.086 Uiso 1 1 calc R . . C13 C 0.6600(9) 0.7999(7) 0.0386(4) 0.109(3) Uani 1 1 d . . . H13C H 0.6499 0.8569 0.0531 0.164 Uiso 1 1 calc R . . H13B H 0.6033 0.7429 0.0496 0.164 Uiso 1 1 calc R . . H13A H 0.6435 0.7916 -0.0011 0.164 Uiso 1 1 calc R . . C14 C 0.8784(8) 0.9062(5) 0.0489(3) 0.086(2) Uani 1 1 d . . . H14C H 0.9613 0.9129 0.0622 0.128 Uiso 1 1 calc R . . H14B H 0.8679 0.9603 0.0672 0.128 Uiso 1 1 calc R . . H14A H 0.8636 0.9057 0.0097 0.128 Uiso 1 1 calc R . . C15 C 0.8120(6) 0.4890(4) 0.0782(2) 0.0584(16) Uani 1 1 d . . . H15 H 0.8117 0.5103 0.1165 0.07 Uiso 1 1 calc R . . C16 C 0.9236(7) 0.4674(5) 0.0795(3) 0.074(2) Uani 1 1 d . . . H16C H 0.9181 0.4156 0.1004 0.111 Uiso 1 1 calc R . . H16B H 0.9969 0.5254 0.0966 0.111 Uiso 1 1 calc R . . H16A H 0.9273 0.4473 0.0424 0.111 Uiso 1 1 calc R . . C17 C 0.6978(7) 0.3970(5) 0.0558(3) 0.089(2) Uani 1 1 d . . . H17C H 0.6988 0.3471 0.0773 0.133 Uiso 1 1 calc R . . H17B H 0.6946 0.3749 0.0179 0.133 Uiso 1 1 calc R . . H17A H 0.6264 0.4096 0.0578 0.133 Uiso 1 1 calc R . . C18 C 0.8487(5) 0.6147(4) 0.2929(2) 0.0429(12) Uani 1 1 d . . . C19 C 0.8413(5) 0.6612(4) 0.3421(2) 0.0489(14) Uani 1 1 d . . . C20 C 0.8994(7) 0.6461(5) 0.3901(2) 0.0705(19) Uani 1 1 d . . . H20 H 0.8955 0.6764 0.4236 0.085 Uiso 1 1 calc R . . C21 C 0.9621(8) 0.5894(6) 0.3912(3) 0.086(2) Uani 1 1 d . . . H21 H 1.0019 0.5817 0.4249 0.103 Uiso 1 1 calc R . . C22 C 0.9666(7) 0.5438(5) 0.3431(3) 0.074(2) Uani 1 1 d . . . H22 H 1.0081 0.503 0.344 0.089 Uiso 1 1 calc R . . C23 C 0.9119(5) 0.5558(4) 0.2931(2) 0.0493(14) Uani 1 1 d . . . C24 C 0.7722(6) 0.7238(5) 0.3450(2) 0.0594(16) Uani 1 1 d . . . H24 H 0.7365 0.7272 0.3072 0.071 Uiso 1 1 calc R . . C25 C 0.8511(7) 0.8252(5) 0.3749(3) 0.077(2) Uani 1 1 d . . . H25C H 0.802 0.8623 0.3752 0.116 Uiso 1 1 calc R . . H25B H 0.9168 0.8559 0.3566 0.116 Uiso 1 1 calc R . . H25A H 0.8855 0.8231 0.4123 0.116 Uiso 1 1 calc R . . C26 C 0.6677(8) 0.6790(6) 0.3742(4) 0.100(3) Uani 1 1 d . . . H26C H 0.6229 0.7194 0.3752 0.15 Uiso 1 1 calc R . . H26B H 0.7014 0.6751 0.4114 0.15 Uiso 1 1 calc R . . H26A H 0.6129 0.6143 0.3546 0.15 Uiso 1 1 calc R . . C27 C 0.9181(5) 0.5044(4) 0.2405(2) 0.0509(14) Uani 1 1 d . . . H27 H 0.912 0.5445 0.2121 0.061 Uiso 1 1 calc R . . C28 C 1.0375(6) 0.4941(6) 0.2434(3) 0.076(2) Uani 1 1 d . . . H28C H 1.1054 0.5577 0.2548 0.115 Uiso 1 1 calc R . . H28B H 1.0387 0.4654 0.2076 0.115 Uiso 1 1 calc R . . H28A H 1.0448 0.4526 0.2698 0.115 Uiso 1 1 calc R . . C29 C 0.8113(6) 0.4070(5) 0.2221(3) 0.0718(19) Uani 1 1 d . . . H29C H 0.8169 0.3759 0.1879 0.108 Uiso 1 1 calc R . . H29B H 0.7357 0.4155 0.2168 0.108 Uiso 1 1 calc R . . H29A H 0.8124 0.3665 0.2498 0.108 Uiso 1 1 calc R . . C30 C 1.4425(5) 1.0883(4) 0.3814(2) 0.0409(12) Uani 1 1 d . . . C31 C 1.5059(5) 1.1530(4) 0.3501(2) 0.0441(13) Uani 1 1 d . . . H31 H 1.5911 1.1721 0.3588 0.053 Uiso 1 1 calc R . . C32 C 1.4658(5) 1.1943(4) 0.3084(2) 0.0425(12) Uani 1 1 d . . . C33 C 1.5220(5) 1.0895(5) 0.4347(2) 0.0565(15) Uani 1 1 d . . . H33C H 1.4715 1.0476 0.4561 0.085 Uiso 1 1 calc R . . H33B H 1.5634 1.1554 0.455 0.085 Uiso 1 1 calc R . . H33A H 1.5823 1.0662 0.4272 0.085 Uiso 1 1 calc R . . C34 C 1.5658(5) 1.2773(4) 0.2936(3) 0.0618(17) Uani 1 1 d . . . H34C H 1.5904 1.2537 0.2626 0.093 Uiso 1 1 calc R . . H34B H 1.6354 1.3061 0.3246 0.093 Uiso 1 1 calc R . . H34A H 1.5364 1.3259 0.284 0.093 Uiso 1 1 calc R . . C35 C 1.2724(5) 0.9775(4) 0.40832(19) 0.0403(12) Uani 1 1 d . . . C36 C 1.2174(5) 1.0171(4) 0.4415(2) 0.0458(13) Uani 1 1 d . . . C37 C 1.1683(5) 0.9653(5) 0.4802(2) 0.0587(16) Uani 1 1 d . . . H37 H 1.132 0.9911 0.5038 0.07 Uiso 1 1 calc R . . C38 C 1.1710(6) 0.8778(5) 0.4854(3) 0.0653(18) Uani 1 1 d . . . H38 H 1.1364 0.8439 0.5122 0.078 Uiso 1 1 calc R . . C39 C 1.2233(6) 0.8390(5) 0.4521(2) 0.0609(17) Uani 1 1 d . . . H39 H 1.2234 0.7779 0.4557 0.073 Uiso 1 1 calc R . . C40 C 1.2762(5) 0.8879(4) 0.4131(2) 0.0503(14) Uani 1 1 d . . . C41 C 1.2138(5) 1.1139(4) 0.4367(2) 0.0479(14) Uani 1 1 d . . . H41 H 1.2215 1.1261 0.3992 0.058 Uiso 1 1 calc R . . C42 C 1.0947(6) 1.1165(5) 0.4448(3) 0.0694(18) Uani 1 1 d . . . H42C H 1.0267 1.0651 0.4186 0.104 Uiso 1 1 calc R . . H42B H 1.0952 1.179 0.4391 0.104 Uiso 1 1 calc R . . H42A H 1.086 1.1069 0.4817 0.104 Uiso 1 1 calc R . . C43 C 1.3197(6) 1.1955(5) 0.4765(3) 0.0712(19) Uani 1 1 d . . . H43C H 1.315 1.2569 0.4721 0.107 Uiso 1 1 calc R . . H43B H 1.3963 1.1976 0.4692 0.107 Uiso 1 1 calc R . . H43A H 1.316 1.1845 0.5137 0.107 Uiso 1 1 calc R . . C44 C 1.3385(7) 0.8431(5) 0.3789(2) 0.0654(18) Uani 1 1 d . . . H44 H 1.3636 0.883 0.3504 0.078 Uiso 1 1 calc R . . C45 C 1.4520(7) 0.8411(6) 0.4142(3) 0.089(2) Uani 1 1 d . . . H45C H 1.4904 0.8126 0.3914 0.134 Uiso 1 1 calc R . . H45B H 1.4287 0.8024 0.4424 0.134 Uiso 1 1 calc R . . H45A H 1.5092 0.9069 0.4311 0.134 Uiso 1 1 calc R . . C46 C 1.2553(8) 0.7393(6) 0.3509(3) 0.100(3) Uani 1 1 d . . . H46C H 1.299 0.7141 0.3294 0.15 Uiso 1 1 calc R . . H46B H 1.1833 0.7383 0.327 0.15 Uiso 1 1 calc R . . H46A H 1.2307 0.6991 0.3784 0.15 Uiso 1 1 calc R . . C47 C 1.3202(5) 1.2328(4) 0.2520(2) 0.0440(13) Uani 1 1 d . . . C48 C 1.2913(5) 1.3016(4) 0.2790(2) 0.0500(14) Uani 1 1 d . . . C49 C 1.2599(6) 1.3642(4) 0.2499(3) 0.0619(17) Uani 1 1 d . . . H49 H 1.2389 1.4103 0.2679 0.074 Uiso 1 1 calc R . . C50 C 1.2587(6) 1.3605(4) 0.1957(3) 0.0684(19) Uani 1 1 d . . . H50 H 1.2376 1.404 0.1765 0.082 Uiso 1 1 calc R . . C51 C 1.2881(6) 1.2940(4) 0.1695(3) 0.0625(17) Uani 1 1 d . . . H51 H 1.2865 1.2918 0.1319 0.075 Uiso 1 1 calc R . . C52 C 1.3207(5) 1.2288(4) 0.1964(2) 0.0519(14) Uani 1 1 d . . . C53 C 1.2962(6) 1.3119(4) 0.3395(2) 0.0577(16) Uani 1 1 d . . . H53 H 1.2942 1.2508 0.3512 0.069 Uiso 1 1 calc R . . C54 C 1.1900(7) 1.3274(5) 0.3547(3) 0.078(2) Uani 1 1 d . . . H54C H 1.1986 1.3332 0.3941 0.117 Uiso 1 1 calc R . . H54B H 1.114 1.2725 0.3366 0.117 Uiso 1 1 calc R . . H54A H 1.189 1.3865 0.3433 0.117 Uiso 1 1 calc R . . C55 C 1.4152(7) 1.3939(6) 0.3709(3) 0.086(2) Uani 1 1 d . . . H55C H 1.4172 1.3991 0.4099 0.129 Uiso 1 1 calc R . . H55B H 1.4213 1.4545 0.3592 0.129 Uiso 1 1 calc R . . H55A H 1.4835 1.3806 0.3639 0.129 Uiso 1 1 calc R . . C56 C 1.3552(6) 1.1587(5) 0.1647(2) 0.0645(17) Uani 1 1 d . . . H56 H 1.3691 1.1141 0.1888 0.077 Uiso 1 1 calc R . . C57 C 1.2573(7) 1.0995(5) 0.1145(2) 0.0703(19) Uani 1 1 d . . . H57C H 1.2822 1.0542 0.0959 0.106 Uiso 1 1 calc R . . H57B H 1.2451 1.1424 0.09 0.106 Uiso 1 1 calc R . . H57A H 1.1814 1.0636 0.1253 0.106 Uiso 1 1 calc R . . C58 C 1.4734(8) 1.2142(7) 0.1461(4) 0.113(3) Uani 1 1 d . . . H58C H 1.5388 1.2512 0.1779 0.169 Uiso 1 1 calc R . . H58B H 1.4607 1.2581 0.1225 0.169 Uiso 1 1 calc R . . H58A H 1.4954 1.1683 0.1262 0.169 Uiso 1 1 calc R . . O1 O 0.8672(5) 1.0702(4) 0.1716(2) 0.0939(17) Uani 1 1 d D A . C59 C 0.9696(7) 1.1473(5) 0.1622(3) 0.085(2) Uani 1 1 d D . . H59A H 0.9948 1.1271 0.13 0.102 Uiso 1 1 calc R A . H59B H 1.0387 1.1691 0.194 0.102 Uiso 1 1 calc R . . C60 C 0.9302(9) 1.2236(7) 0.1533(6) 0.160(5) Uani 1 1 d D A . H60A H 0.9602 1.2545 0.123 0.192 Uiso 1 1 calc R . . H60B H 0.9603 1.2732 0.1864 0.192 Uiso 1 1 calc R . . C61 C 0.7926(10) 1.1741(7) 0.1397(7) 0.176(6) Uani 1 1 d D . . H61A H 0.7596 1.2007 0.1668 0.211 Uiso 1 1 calc R A . H61B H 0.7594 1.1833 0.1033 0.211 Uiso 1 1 calc R . . C62 C 0.7612(7) 1.0715(6) 0.1409(4) 0.099(3) Uani 1 1 d D A . H62A H 0.6922 1.0437 0.1585 0.119 Uiso 1 1 calc R . . H62B H 0.7397 1.0347 0.1038 0.119 Uiso 1 1 calc R . . O3 O 1.2643(6) 0.8487(5) 0.0951(2) 0.1053(19) Uani 1 1 d D . . C67 C 1.1569(10) 0.8125(9) 0.0539(4) 0.129(4) Uani 1 1 d D . . H67A H 1.1184 0.7413 0.0493 0.155 Uiso 1 1 calc R . . H67B H 1.0994 0.8372 0.0647 0.155 Uiso 1 1 calc R . . C68 C 1.1814(17) 0.8401(19) 0.0041(7) 0.287(13) Uani 1 1 d D . . H68A H 1.1497 0.8877 -0.0062 0.344 Uiso 1 1 calc R . . H68B H 1.1487 0.784 -0.0256 0.344 Uiso 1 1 calc R . . C69 C 1.3204(19) 0.8847(17) 0.0198(7) 0.263(11) Uani 1 1 d D . . H69A H 1.3491 0.8437 -0.001 0.316 Uiso 1 1 calc R . . H69B H 1.3508 0.9485 0.0085 0.316 Uiso 1 1 calc R . . C70 C 1.3750(11) 0.8971(9) 0.0779(6) 0.143(4) Uani 1 1 d D . . H70A H 1.4303 0.8647 0.0843 0.171 Uiso 1 1 calc R . . H70B H 1.4179 0.9657 0.0952 0.171 Uiso 1 1 calc R . . O4 O 1.3674(6) 0.7540(5) 0.1726(3) 0.114(2) Uani 1 1 d D . . C71 C 1.4190(13) 0.7405(7) 0.2251(6) 0.173(6) Uani 1 1 d D . . H71A H 1.3908 0.7668 0.2544 0.207 Uiso 1 1 calc R . . H71B H 1.5087 0.771 0.2331 0.207 Uiso 1 1 calc R . . C72 C 1.3716(12) 0.6342(7) 0.2182(6) 0.159(5) Uani 1 1 d D . . H72A H 1.313 0.6083 0.2412 0.19 Uiso 1 1 calc R . . H72B H 1.4381 0.6135 0.2274 0.19 Uiso 1 1 calc R . . C73 C 1.3064(10) 0.5999(8) 0.1549(6) 0.143(4) Uani 1 1 d D . . H73A H 1.322 0.546 0.1389 0.172 Uiso 1 1 calc R . . H73B H 1.2178 0.5798 0.1493 0.172 Uiso 1 1 calc R . . C74 C 1.3629(14) 0.6863(8) 0.1317(5) 0.177(7) Uani 1 1 d D . . H74A H 1.4447 0.696 0.1269 0.213 Uiso 1 1 calc R . . H74B H 1.312 0.6854 0.0968 0.213 Uiso 1 1 calc R . . C75 C 1.1569(8) 0.6464(6) 0.5612(3) 0.087(2) Uani 1 1 d . . . H75B H 1.2135 0.7153 0.5719 0.104 Uiso 1 1 calc R . . H75A H 1.1677 0.6138 0.5924 0.104 Uiso 1 1 calc R . . C76 C 1.0323(8) 0.6379(6) 0.5485(4) 0.099(3) Uani 1 1 d . . . H76C H 1.0152 0.6662 0.5804 0.148 Uiso 1 1 calc R . . H76B H 0.9761 0.5698 0.538 0.148 Uiso 1 1 calc R . . H76A H 1.0222 0.672 0.5184 0.148 Uiso 1 1 calc R . . C77 C 1.2955(9) 0.6006(7) 0.5265(5) 0.122(4) Uani 1 1 d . . . H77B H 1.2973 0.5604 0.5548 0.147 Uiso 1 1 calc R . . H77A H 1.3595 0.6662 0.5411 0.147 Uiso 1 1 calc R . . C78 C 1.3235(12) 0.5615(9) 0.4794(6) 0.174(6) Uani 1 1 d . . . H78C H 1.4024 0.5589 0.4897 0.261 Uiso 1 1 calc R . . H78B H 1.3262 0.6027 0.4518 0.261 Uiso 1 1 calc R . . H78A H 1.2608 0.4965 0.4646 0.261 Uiso 1 1 calc R . . O2 O 0.7634(6) 1.0462(5) 0.2696(3) 0.114(2) Uani 0.516(9) 1 d PD A 1 C63 C 0.6466(13) 1.0030(13) 0.2664(7) 0.104(2) Uiso 0.516(9) 1 d PD A 1 H63A H 0.6061 0.9463 0.237 0.125 Uiso 0.516(9) 1 calc PR A 1 H63B H 0.6064 1.0474 0.2618 0.125 Uiso 0.516(9) 1 calc PR A 1 C64 C 0.6522(16) 0.9748(12) 0.3220(6) 0.104(2) Uiso 0.516(9) 1 d PD A 1 H64A H 0.6717 0.9182 0.3238 0.125 Uiso 0.516(9) 1 calc PR A 1 H64B H 0.5768 0.9632 0.3347 0.125 Uiso 0.516(9) 1 calc PR A 1 C66 C 0.8194(18) 1.1325(11) 0.3131(7) 0.104(2) Uiso 0.516(9) 1 d PD A 1 H66A H 0.7902 1.1829 0.3061 0.125 Uiso 0.516(9) 1 calc PR A 1 H66B H 0.9091 1.1602 0.3226 0.125 Uiso 0.516(9) 1 calc PR A 1 C65 C 0.7605(17) 1.0708(13) 0.3531(7) 0.104(2) Uiso 0.516(9) 1 d PD A 1 H65A H 0.7308 1.1071 0.3767 0.125 Uiso 0.516(9) 1 calc PR A 1 H65B H 0.8215 1.0556 0.3765 0.125 Uiso 0.516(9) 1 calc PR A 1 O2A O 0.7634(6) 1.0462(5) 0.2696(3) 0.114(2) Uani 0.484(9) 1 d P A 2 C63A C 0.6860(17) 0.9842(14) 0.3023(7) 0.104(2) Uiso 0.484(9) 1 d PD A 2 H63C H 0.6784 0.9173 0.2948 0.125 Uiso 0.484(9) 1 calc PR A 2 H63D H 0.604 0.9834 0.2947 0.125 Uiso 0.484(9) 1 calc PR A 2 C64A C 0.7538(19) 1.0317(12) 0.3617(7) 0.104(2) Uiso 0.484(9) 1 d PD A 2 H64C H 0.8097 1.004 0.3775 0.125 Uiso 0.484(9) 1 calc PR A 2 H64D H 0.6992 1.0329 0.3859 0.125 Uiso 0.484(9) 1 calc PR A 2 C65A C 0.8204(18) 1.1317(13) 0.3439(7) 0.104(2) Uiso 0.484(9) 1 d PD A 2 H65C H 0.8111 1.1818 0.3678 0.125 Uiso 0.484(9) 1 calc PR A 2 H65D H 0.908 1.1469 0.3505 0.125 Uiso 0.484(9) 1 calc PR A 2 C66A C 0.777(2) 1.1391(11) 0.2848(7) 0.104(2) Uiso 0.484(9) 1 d PD A 2 H66C H 0.7003 1.147 0.2777 0.125 Uiso 0.484(9) 1 calc PR A 2 H66D H 0.8398 1.1879 0.2704 0.125 Uiso 0.484(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0403(3) 0.0331(3) 0.0311(3) 0.00032(19) 0.0036(2) 0.0193(2) Y2 0.0393(3) 0.0363(3) 0.0311(3) 0.0012(2) 0.0018(2) 0.0181(2) Li1 0.050(6) 0.049(6) 0.081(7) 0.003(5) 0.002(5) 0.025(5) Li2 0.061(7) 0.087(9) 0.087(8) -0.019(7) 0.019(6) 0.033(7) Cl1 0.0562(8) 0.0416(7) 0.0333(7) 0.0074(5) -0.0006(6) 0.0137(6) Cl2 0.0539(8) 0.0439(8) 0.0364(7) 0.0090(6) -0.0039(6) 0.0116(7) Cl3 0.0501(9) 0.0508(9) 0.0831(11) -0.0077(8) 0.0171(8) 0.0260(7) Cl4 0.0511(8) 0.0472(8) 0.0570(8) 0.0038(6) 0.0122(6) 0.0300(7) Cl5 0.0500(8) 0.0538(9) 0.0618(9) -0.0113(7) 0.0014(7) 0.0298(7) Cl6 0.0534(8) 0.0606(9) 0.0551(8) -0.0032(7) 0.0111(7) 0.0323(8) O5 0.100(4) 0.086(4) 0.085(4) -0.008(3) -0.011(3) 0.040(3) N1 0.045(3) 0.047(3) 0.029(2) -0.0027(18) 0.0016(18) 0.027(2) N2 0.045(3) 0.036(2) 0.034(2) 0.0033(18) 0.0089(19) 0.023(2) N3 0.038(2) 0.042(2) 0.033(2) 0.0030(18) 0.0051(18) 0.020(2) N4 0.042(2) 0.038(2) 0.037(2) 0.0005(18) 0.0035(19) 0.022(2) C1 0.046(3) 0.050(3) 0.041(3) -0.004(2) -0.001(2) 0.026(3) C2 0.037(3) 0.045(3) 0.053(3) 0.000(3) 0.002(2) 0.020(3) C3 0.045(3) 0.034(3) 0.049(3) 0.003(2) 0.009(2) 0.024(3) C4 0.057(4) 0.074(4) 0.048(3) -0.012(3) -0.010(3) 0.027(3) C5 0.053(4) 0.049(4) 0.069(4) 0.016(3) 0.019(3) 0.020(3) C6 0.055(3) 0.052(3) 0.029(3) -0.003(2) 0.001(2) 0.027(3) C7 0.087(5) 0.059(4) 0.034(3) 0.002(3) 0.005(3) 0.041(4) C8 0.143(7) 0.081(5) 0.036(3) 0.014(3) 0.021(4) 0.065(5) C9 0.148(8) 0.088(5) 0.040(4) 0.006(4) 0.032(4) 0.065(5) C10 0.112(6) 0.071(5) 0.049(4) 0.001(3) 0.026(4) 0.054(4) C11 0.069(4) 0.049(3) 0.043(3) -0.002(3) 0.012(3) 0.030(3) C12 0.121(6) 0.077(5) 0.035(3) 0.011(3) 0.011(4) 0.062(5) C13 0.134(8) 0.102(7) 0.129(8) 0.024(6) 0.047(7) 0.079(6) C14 0.139(7) 0.061(5) 0.052(4) 0.006(3) -0.010(4) 0.051(5) C15 0.081(4) 0.056(4) 0.048(3) 0.000(3) 0.019(3) 0.038(4) C16 0.095(5) 0.066(4) 0.076(5) 0.002(4) 0.018(4) 0.052(4) C17 0.095(6) 0.060(5) 0.106(6) 0.007(4) 0.024(5) 0.027(4) C18 0.050(3) 0.041(3) 0.040(3) 0.011(2) 0.008(2) 0.021(3) C19 0.061(4) 0.048(3) 0.039(3) 0.009(2) 0.014(3) 0.023(3) C20 0.104(6) 0.085(5) 0.037(3) 0.014(3) 0.015(3) 0.053(5) C21 0.127(7) 0.109(6) 0.044(4) 0.024(4) 0.006(4) 0.075(6) C22 0.100(6) 0.084(5) 0.064(4) 0.029(4) 0.012(4) 0.062(5) C23 0.057(4) 0.047(3) 0.048(3) 0.013(3) 0.008(3) 0.027(3) C24 0.077(4) 0.068(4) 0.042(3) 0.003(3) 0.017(3) 0.039(4) C25 0.103(6) 0.059(4) 0.071(5) -0.011(3) 0.028(4) 0.036(4) C26 0.101(6) 0.088(6) 0.119(7) -0.006(5) 0.055(6) 0.040(5) C27 0.059(4) 0.049(3) 0.057(4) 0.013(3) 0.016(3) 0.033(3) C28 0.071(5) 0.093(5) 0.084(5) 0.011(4) 0.015(4) 0.056(4) C29 0.077(5) 0.053(4) 0.091(5) 0.002(4) 0.032(4) 0.030(4) C30 0.042(3) 0.048(3) 0.035(3) -0.001(2) 0.005(2) 0.024(3) C31 0.032(3) 0.050(3) 0.049(3) 0.003(3) 0.005(2) 0.019(3) C32 0.043(3) 0.037(3) 0.046(3) 0.002(2) 0.006(2) 0.018(3) C33 0.045(3) 0.077(4) 0.043(3) 0.002(3) -0.001(3) 0.027(3) C34 0.051(4) 0.053(4) 0.074(4) 0.015(3) 0.001(3) 0.018(3) C35 0.039(3) 0.046(3) 0.030(3) 0.003(2) -0.001(2) 0.015(3) C36 0.038(3) 0.059(4) 0.035(3) 0.005(2) 0.003(2) 0.018(3) C37 0.050(4) 0.083(5) 0.042(3) 0.015(3) 0.016(3) 0.024(3) C38 0.062(4) 0.076(5) 0.052(4) 0.025(3) 0.011(3) 0.020(4) C39 0.071(4) 0.059(4) 0.045(3) 0.013(3) -0.004(3) 0.025(3) C40 0.059(4) 0.053(3) 0.033(3) 0.003(3) -0.005(3) 0.025(3) C41 0.051(3) 0.061(4) 0.037(3) 0.002(3) 0.014(2) 0.028(3) C42 0.062(4) 0.086(5) 0.078(5) 0.017(4) 0.029(4) 0.043(4) C43 0.068(4) 0.063(4) 0.070(4) -0.012(3) 0.003(3) 0.024(4) C44 0.099(5) 0.073(4) 0.044(3) 0.016(3) 0.010(3) 0.057(4) C45 0.101(6) 0.116(7) 0.073(5) 0.004(4) 0.014(4) 0.073(6) C46 0.140(8) 0.088(6) 0.077(5) -0.019(4) -0.022(5) 0.076(6) C47 0.038(3) 0.038(3) 0.051(3) 0.006(2) 0.001(2) 0.014(2) C48 0.049(3) 0.038(3) 0.061(4) 0.006(3) 0.004(3) 0.020(3) C49 0.059(4) 0.043(3) 0.085(5) 0.009(3) 0.005(3) 0.027(3) C50 0.078(5) 0.042(4) 0.080(5) 0.013(3) -0.005(4) 0.028(3) C51 0.067(4) 0.055(4) 0.053(4) 0.015(3) -0.004(3) 0.019(3) C52 0.053(3) 0.046(3) 0.050(3) 0.008(3) -0.001(3) 0.018(3) C53 0.070(4) 0.044(3) 0.064(4) 0.004(3) 0.017(3) 0.029(3) C54 0.079(5) 0.058(4) 0.105(6) -0.003(4) 0.033(4) 0.036(4) C55 0.079(5) 0.100(6) 0.069(5) -0.006(4) 0.004(4) 0.037(5) C56 0.085(5) 0.067(4) 0.044(3) 0.005(3) 0.004(3) 0.038(4) C57 0.094(5) 0.057(4) 0.048(4) 0.000(3) 0.015(3) 0.021(4) C58 0.083(6) 0.137(8) 0.103(7) -0.027(6) 0.022(5) 0.039(6) O1 0.075(3) 0.072(3) 0.127(5) 0.041(3) -0.005(3) 0.029(3) C59 0.089(6) 0.070(5) 0.100(6) 0.027(4) 0.020(5) 0.036(5) C60 0.097(8) 0.087(7) 0.288(17) 0.070(9) 0.012(9) 0.035(6) C61 0.124(10) 0.098(8) 0.298(18) 0.054(10) -0.004(10) 0.053(8) C62 0.089(6) 0.097(6) 0.114(7) 0.018(5) -0.002(5) 0.051(5) O3 0.090(4) 0.129(5) 0.092(4) -0.015(4) 0.036(4) 0.041(4) C67 0.119(9) 0.174(11) 0.103(8) 0.041(8) 0.042(7) 0.058(8) C68 0.165(17) 0.42(4) 0.172(18) 0.033(19) 0.015(14) 0.03(2) C69 0.33(3) 0.35(3) 0.173(18) 0.086(19) 0.13(2) 0.16(3) C70 0.163(11) 0.141(10) 0.181(13) 0.064(9) 0.095(10) 0.092(9) O4 0.123(5) 0.108(5) 0.146(6) 0.003(5) 0.060(5) 0.075(4) C71 0.210(15) 0.069(7) 0.230(17) -0.019(9) 0.078(13) 0.047(8) C72 0.146(11) 0.095(8) 0.236(16) -0.011(9) 0.026(11) 0.067(8) C73 0.098(8) 0.089(7) 0.235(15) 0.030(9) 0.032(9) 0.034(6) C74 0.319(19) 0.148(11) 0.185(12) 0.083(10) 0.176(14) 0.163(13) C75 0.091(6) 0.083(5) 0.060(5) 0.003(4) -0.002(4) 0.020(5) C76 0.095(6) 0.085(6) 0.097(6) 0.006(5) 0.007(5) 0.025(5) C77 0.087(7) 0.086(7) 0.170(11) -0.018(6) 0.002(7) 0.031(6) C78 0.151(11) 0.161(12) 0.196(13) -0.061(10) -0.003(10) 0.086(10) O2 0.095(4) 0.116(5) 0.142(5) -0.017(4) 0.027(4) 0.065(4) O2A 0.095(4) 0.116(5) 0.142(5) -0.017(4) 0.027(4) 0.065(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y1 N1 2.344(4) . ? Y1 N2 2.356(4) . ? Y1 Cl4 2.6180(14) . ? Y1 Cl3 2.6189(15) . ? Y1 Cl2 2.6740(13) . ? Y1 Cl1 2.7543(14) . ? Y2 N4 2.340(4) . ? Y2 N3 2.361(4) . ? Y2 Cl5 2.6088(14) . ? Y2 Cl6 2.6129(14) . ? Y2 Cl2 2.6811(14) . ? Y2 Cl1 2.7590(13) . ? Li1 O1 1.933(12) . ? Li1 O2 1.985(12) . ? Li1 Cl5 2.329(10) . ? Li1 Cl4 2.342(10) . ? Li2 O3 1.923(15) . ? Li2 O4 1.951(14) . ? Li2 Cl6 2.330(12) . ? Li2 Cl3 2.353(13) . ? O5 C77 1.370(10) . ? O5 C75 1.410(9) . ? N1 C1 1.336(7) . ? N1 C6 1.450(6) . ? N2 C3 1.330(6) . ? N2 C18 1.452(6) . ? N3 C30 1.326(6) . ? N3 C35 1.454(6) . ? N4 C32 1.343(6) . ? N4 C47 1.449(6) . ? C1 C2 1.397(8) . ? C1 C4 1.521(7) . ? C2 C3 1.406(7) . ? C3 C5 1.509(7) . ? C6 C7 1.394(8) . ? C6 C11 1.413(7) . ? C7 C8 1.396(8) . ? C7 C12 1.515(8) . ? C8 C9 1.380(9) . ? C9 C10 1.365(9) . ? C10 C11 1.385(8) . ? C11 C15 1.522(8) . ? C12 C14 1.515(10) . ? C12 C13 1.523(11) . ? C15 C17 1.522(9) . ? C15 C16 1.531(9) . ? C18 C23 1.406(7) . ? C18 C19 1.418(7) . ? C19 C20 1.390(8) . ? C19 C24 1.517(8) . ? C20 C21 1.371(10) . ? C21 C22 1.374(9) . ? C22 C23 1.395(8) . ? C23 C27 1.520(8) . ? C24 C25 1.513(9) . ? C24 C26 1.550(9) . ? C27 C29 1.516(8) . ? C27 C28 1.530(8) . ? C30 C31 1.403(7) . ? C30 C33 1.523(7) . ? C31 C32 1.396(7) . ? C32 C34 1.512(8) . ? C35 C36 1.402(7) . ? C35 C40 1.407(8) . ? C36 C37 1.390(8) . ? C36 C41 1.516(8) . ? C37 C38 1.372(9) . ? C38 C39 1.373(9) . ? C39 C40 1.391(8) . ? C40 C44 1.534(8) . ? C41 C43 1.526(8) . ? C41 C42 1.531(8) . ? C44 C46 1.535(10) . ? C44 C45 1.539(9) . ? C47 C48 1.400(8) . ? C47 C52 1.408(8) . ? C48 C49 1.392(8) . ? C48 C53 1.520(8) . ? C49 C50 1.368(9) . ? C50 C51 1.367(9) . ? C51 C52 1.403(8) . ? C52 C56 1.519(8) . ? C53 C54 1.524(9) . ? C53 C55 1.530(9) . ? C56 C57 1.521(9) . ? C56 C58 1.548(10) . ? O1 C62 1.410(8) . ? O1 C59 1.423(8) . ? C59 C60 1.452(9) . ? C60 C61 1.519(11) . ? C61 C62 1.470(10) . ? O3 C67 1.413(10) . ? O3 C70 1.438(9) . ? C67 C68 1.411(13) . ? C68 C69 1.534(13) . ? C69 C70 1.474(12) . ? O4 C74 1.380(10) . ? O4 C71 1.443(12) . ? C71 C72 1.482(11) . ? C72 C73 1.607(12) . ? C73 C74 1.463(11) . ? C75 C76 1.463(11) . ? C77 C78 1.446(14) . ? O2 C63 1.311(13) . ? O2 C66 1.488(13) . ? C63 C64 1.511(14) . ? C64 C65 1.568(14) . ? C66 C65 1.529(14) . ? C63A C64A 1.549(14) . ? C64A C65A 1.577(14) . ? C65A C66A 1.533(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N2 81.58(15) . . ? N1 Y1 Cl4 89.49(10) . . ? N2 Y1 Cl4 89.66(10) . . ? N1 Y1 Cl3 87.12(11) . . ? N2 Y1 Cl3 104.28(10) . . ? Cl4 Y1 Cl3 164.98(5) . . ? N1 Y1 Cl2 167.49(11) . . ? N2 Y1 Cl2 87.82(10) . . ? Cl4 Y1 Cl2 97.11(5) . . ? Cl3 Y1 Cl2 89.09(5) . . ? N1 Y1 Cl1 113.45(11) . . ? N2 Y1 Cl1 163.72(10) . . ? Cl4 Y1 Cl1 84.44(5) . . ? Cl3 Y1 Cl1 83.50(5) . . ? Cl2 Y1 Cl1 77.91(4) . . ? N4 Y2 N3 82.60(14) . . ? N4 Y2 Cl5 88.44(10) . . ? N3 Y2 Cl5 101.96(10) . . ? N4 Y2 Cl6 88.62(11) . . ? N3 Y2 Cl6 91.32(10) . . ? Cl5 Y2 Cl6 165.90(5) . . ? N4 Y2 Cl2 169.51(10) . . ? N3 Y2 Cl2 88.01(11) . . ? Cl5 Y2 Cl2 88.96(5) . . ? Cl6 Y2 Cl2 96.28(5) . . ? N4 Y2 Cl1 112.02(10) . . ? N3 Y2 Cl1 164.89(11) . . ? Cl5 Y2 Cl1 82.90(5) . . ? Cl6 Y2 Cl1 85.43(5) . . ? Cl2 Y2 Cl1 77.71(4) . . ? O1 Li1 O2 98.7(5) . . ? O1 Li1 Cl5 111.6(5) . . ? O2 Li1 Cl5 101.7(5) . . ? O1 Li1 Cl4 114.0(5) . . ? O2 Li1 Cl4 103.9(5) . . ? Cl5 Li1 Cl4 122.6(4) . . ? O3 Li2 O4 99.1(6) . . ? O3 Li2 Cl6 115.9(7) . . ? O4 Li2 Cl6 102.4(6) . . ? O3 Li2 Cl3 111.1(6) . . ? O4 Li2 Cl3 106.4(6) . . ? Cl6 Li2 Cl3 118.9(5) . . ? Y1 Cl1 Y2 100.12(4) . . ? Y1 Cl2 Y2 104.25(4) . . ? Li2 Cl3 Y1 119.1(3) . . ? Li1 Cl4 Y1 109.9(3) . . ? Li1 Cl5 Y2 114.5(3) . . ? Li2 Cl6 Y2 115.0(3) . . ? C77 O5 C75 115.6(7) . . ? C1 N1 C6 116.7(4) . . ? C1 N1 Y1 121.3(3) . . ? C6 N1 Y1 121.8(3) . . ? C3 N2 C18 117.1(4) . . ? C3 N2 Y1 122.3(3) . . ? C18 N2 Y1 120.2(3) . . ? C30 N3 C35 117.3(4) . . ? C30 N3 Y2 120.9(3) . . ? C35 N3 Y2 121.6(3) . . ? C32 N4 C47 117.8(4) . . ? C32 N4 Y2 119.2(3) . . ? C47 N4 Y2 122.7(3) . . ? N1 C1 C2 125.1(5) . . ? N1 C1 C4 120.7(5) . . ? C2 C1 C4 114.2(5) . . ? C1 C2 C3 131.4(5) . . ? N2 C3 C2 124.7(5) . . ? N2 C3 C5 121.5(5) . . ? C2 C3 C5 113.7(5) . . ? C7 C6 C11 120.7(5) . . ? C7 C6 N1 121.0(5) . . ? C11 C6 N1 118.3(5) . . ? C6 C7 C8 118.4(5) . . ? C6 C7 C12 123.1(5) . . ? C8 C7 C12 118.5(6) . . ? C9 C8 C7 120.6(6) . . ? C10 C9 C8 120.7(6) . . ? C9 C10 C11 121.0(6) . . ? C10 C11 C6 118.6(6) . . ? C10 C11 C15 118.8(5) . . ? C6 C11 C15 122.7(5) . . ? C7 C12 C14 114.2(6) . . ? C7 C12 C13 110.2(6) . . ? C14 C12 C13 110.0(6) . . ? C11 C15 C17 112.4(6) . . ? C11 C15 C16 112.1(5) . . ? C17 C15 C16 109.5(5) . . ? C23 C18 C19 121.0(5) . . ? C23 C18 N2 118.1(5) . . ? C19 C18 N2 120.9(5) . . ? C20 C19 C18 117.1(5) . . ? C20 C19 C24 119.0(5) . . ? C18 C19 C24 123.8(5) . . ? C21 C20 C19 122.9(6) . . ? C20 C21 C22 119.1(6) . . ? C21 C22 C23 121.7(6) . . ? C22 C23 C18 118.2(5) . . ? C22 C23 C27 120.7(5) . . ? C18 C23 C27 121.1(5) . . ? C25 C24 C19 113.0(6) . . ? C25 C24 C26 107.8(5) . . ? C19 C24 C26 110.2(6) . . ? C29 C27 C23 111.2(5) . . ? C29 C27 C28 110.5(5) . . ? C23 C27 C28 113.3(5) . . ? N3 C30 C31 125.2(5) . . ? N3 C30 C33 121.5(5) . . ? C31 C30 C33 113.3(5) . . ? C32 C31 C30 131.3(5) . . ? N4 C32 C31 125.5(5) . . ? N4 C32 C34 120.2(5) . . ? C31 C32 C34 114.2(5) . . ? C36 C35 C40 121.7(5) . . ? C36 C35 N3 117.9(5) . . ? C40 C35 N3 120.4(5) . . ? C37 C36 C35 117.4(5) . . ? C37 C36 C41 120.6(5) . . ? C35 C36 C41 121.9(5) . . ? C38 C37 C36 121.6(6) . . ? C37 C38 C39 120.4(6) . . ? C38 C39 C40 120.9(6) . . ? C39 C40 C35 117.9(6) . . ? C39 C40 C44 118.5(5) . . ? C35 C40 C44 123.6(5) . . ? C36 C41 C43 111.7(5) . . ? C36 C41 C42 112.8(5) . . ? C43 C41 C42 109.4(5) . . ? C40 C44 C46 112.6(6) . . ? C40 C44 C45 111.0(5) . . ? C46 C44 C45 107.3(6) . . ? C48 C47 C52 120.4(5) . . ? C48 C47 N4 119.1(5) . . ? C52 C47 N4 120.6(5) . . ? C49 C48 C47 119.2(6) . . ? C49 C48 C53 118.7(5) . . ? C47 C48 C53 122.0(5) . . ? C50 C49 C48 121.1(6) . . ? C51 C50 C49 119.7(6) . . ? C50 C51 C52 122.1(6) . . ? C51 C52 C47 117.5(6) . . ? C51 C52 C56 118.9(6) . . ? C47 C52 C56 123.6(5) . . ? C48 C53 C54 113.7(6) . . ? C48 C53 C55 110.6(5) . . ? C54 C53 C55 109.5(5) . . ? C52 C56 C57 112.2(6) . . ? C52 C56 C58 110.2(6) . . ? C57 C56 C58 107.9(6) . . ? C62 O1 C59 108.8(6) . . ? C62 O1 Li1 123.1(6) . . ? C59 O1 Li1 125.2(5) . . ? O1 C59 C60 105.3(7) . . ? C59 C60 C61 105.1(8) . . ? C62 C61 C60 106.0(8) . . ? O1 C62 C61 104.2(7) . . ? C67 O3 C70 115.8(8) . . ? C67 O3 Li2 119.8(7) . . ? C70 O3 Li2 124.0(8) . . ? C68 C67 O3 111.1(11) . . ? C67 C68 C69 99.3(13) . . ? C70 C69 C68 115.8(13) . . ? O3 C70 C69 97.2(11) . . ? C74 O4 C71 111.3(9) . . ? C74 O4 Li2 123.3(9) . . ? C71 O4 Li2 120.1(8) . . ? O4 C71 C72 101.7(10) . . ? C71 C72 C73 103.3(10) . . ? C74 C73 C72 102.9(10) . . ? O4 C74 C73 98.6(8) . . ? O5 C75 C76 111.6(7) . . ? O5 C77 C78 114.0(10) . . ? C63 O2 C66 110.1(12) . . ? C63 O2 Li1 129.4(10) . . ? C66 O2 Li1 119.9(9) . . ? O2 C63 C64 98.0(12) . . ? C63 C64 C65 96.6(13) . . ? O2 C66 C65 89.9(11) . . ? C66 C65 C64 110.6(14) . . ? C63A C64A C65A 91.4(13) . . ? C66A C65A C64A 116.4(14) . . ? #===END data_(4b)-feb704 _database_code_depnum_ccdc_archive 'CCDC 684944' _audit_creation_date 2004-02-10T08:02:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C74 H122 Cl6 Li2 N4 O4 Y2, 0.5(C4 H10 O)' _chemical_formula_sum 'C76 H127 Cl6 Li2 N4 O4.50 Y2' _chemical_formula_weight 1573.22 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9001(2) _cell_length_b 26.5237(5) _cell_length_c 25.2112(4) _cell_angle_alpha 90 _cell_angle_beta 94.508(1) _cell_angle_gamma 90 _cell_volume 8599.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 60631 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3332 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.736 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.657506E-1 _diffrn_orient_matrix_ub_12 -0.148268E-1 _diffrn_orient_matrix_ub_13 -0.16966E-1 _diffrn_orient_matrix_ub_21 0.35901E-2 _diffrn_orient_matrix_ub_22 0.233718E-1 _diffrn_orient_matrix_ub_23 -0.309258E-1 _diffrn_orient_matrix_ub_31 0.413581E-1 _diffrn_orient_matrix_ub_32 -0.256003E-1 _diffrn_orient_matrix_ub_33 -0.184076E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_unetI/netI 0.0659 _diffrn_reflns_number 55318 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 15060 _reflns_number_gt 10586 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The ether ligands and the disordered ether solvate molecule were very poorly defined, and were included with isotropic displacement parameters for the C atoms of the ether ligands and C and O atoms of the ether solvate and with SADI bond length constraints. H atoms for the disordered solvate molecule were omitted. 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^)+(0.0768P)^2^+27.9014P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 15060 _refine_ls_number_parameters 765 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.415 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y1 Y 0.60101(4) 0.104687(19) 0.24068(2) 0.02632(14) Uani 1 1 d . . . Y2 Y 0.45379(4) 0.188819(19) 0.35324(2) 0.02641(14) Uani 1 1 d . . . Li1 Li 0.7910(7) 0.1578(4) 0.3759(4) 0.041(2) Uani 1 1 d . . . Li2 Li 0.2705(10) 0.0797(5) 0.2607(5) 0.066(3) Uani 1 1 d . . . Cl1 Cl 0.51739(11) 0.19567(5) 0.25497(5) 0.0335(3) Uani 1 1 d . . . Cl2 Cl 0.53193(11) 0.09335(5) 0.34001(5) 0.0359(3) Uani 1 1 d . . . Cl3 Cl 0.78398(11) 0.11880(6) 0.29245(6) 0.0379(3) Uani 1 1 d . . . Cl4 Cl 0.41378(11) 0.07382(6) 0.20680(6) 0.0464(4) Uani 1 1 d . . . Cl5 Cl 0.64580(11) 0.20940(6) 0.38848(6) 0.0389(3) Uani 1 1 d . . . Cl6 Cl 0.27445(10) 0.14649(6) 0.32440(6) 0.0392(3) Uani 1 1 d . . . O1 O 0.9160(3) 0.20046(19) 0.3836(2) 0.0599(13) Uani 1 1 d D . . O2 O 0.8040(4) 0.1099(2) 0.43666(18) 0.0657(14) Uani 1 1 d D . . O3 O 0.1466(4) 0.0945(3) 0.2143(2) 0.094(2) Uani 1 1 d D . . O4 O 0.2473(6) 0.0153(3) 0.2913(3) 0.106(2) Uani 1 1 d D . . N1 N 0.6668(3) 0.13934(16) 0.16358(17) 0.0295(10) Uani 1 1 d . . . N2 N 0.6631(3) 0.02976(15) 0.20611(17) 0.0287(10) Uani 1 1 d . . . N3 N 0.3771(3) 0.26919(16) 0.34033(17) 0.0297(10) Uani 1 1 d . . . N4 N 0.4041(3) 0.20251(17) 0.43940(17) 0.0319(10) Uani 1 1 d . . . C1 C 0.7513(4) 0.1193(2) 0.1448(2) 0.0312(12) Uani 1 1 d . . . C2 C 0.7940(4) 0.0726(2) 0.1593(2) 0.0325(13) Uani 1 1 d . . . H2 H 0.8643 0.0687 0.1513 0.039 Uiso 1 1 calc R . . C3 C 0.7531(4) 0.0307(2) 0.1832(2) 0.0318(13) Uani 1 1 d . . . C4 C 0.8092(5) 0.1472(2) 0.1039(2) 0.0408(14) Uani 1 1 d . . . H4A H 0.761 0.1695 0.083 0.061 Uiso 1 1 calc R . . H4B H 0.8393 0.1229 0.0802 0.061 Uiso 1 1 calc R . . H4C H 0.8649 0.1674 0.122 0.061 Uiso 1 1 calc R . . C5 C 0.8190(5) -0.0167(2) 0.1813(3) 0.0458(16) Uani 1 1 d . . . H5A H 0.8776 -0.0146 0.2084 0.069 Uiso 1 1 calc R . . H5B H 0.8453 -0.0198 0.1461 0.069 Uiso 1 1 calc R . . H5C H 0.7764 -0.0462 0.1883 0.069 Uiso 1 1 calc R . . C6 C 0.6263(4) 0.1861(2) 0.1399(2) 0.0329(13) Uani 1 1 d . . . C7 C 0.6705(5) 0.2329(2) 0.1553(2) 0.0389(14) Uani 1 1 d . . . C8 C 0.6232(5) 0.2762(2) 0.1327(3) 0.0488(16) Uani 1 1 d . . . H8 H 0.6508 0.3083 0.1429 0.059 Uiso 1 1 calc R . . C9 C 0.5388(6) 0.2740(3) 0.0967(3) 0.0527(18) Uani 1 1 d . . . H9 H 0.509 0.3041 0.082 0.063 Uiso 1 1 calc R . . C10 C 0.4968(5) 0.2279(3) 0.0815(3) 0.0504(17) Uani 1 1 d . . . H10 H 0.4382 0.2266 0.0563 0.06 Uiso 1 1 calc R . . C11 C 0.5392(5) 0.1829(2) 0.1027(2) 0.0385(14) Uani 1 1 d . . . C12 C 0.7673(5) 0.2389(2) 0.1932(2) 0.0430(15) Uani 1 1 d . . . H12 H 0.7936 0.2046 0.2037 0.052 Uiso 1 1 calc R . . C13 C 0.7459(6) 0.2676(3) 0.2434(3) 0.0567(18) Uani 1 1 d . . . H13A H 0.8103 0.2704 0.2666 0.085 Uiso 1 1 calc R . . H13B H 0.6934 0.2496 0.2621 0.085 Uiso 1 1 calc R . . H13C H 0.7202 0.3014 0.2338 0.085 Uiso 1 1 calc R . . C14 C 0.8541(6) 0.2671(3) 0.1660(3) 0.0575(18) Uani 1 1 d . . . H14A H 0.9157 0.2703 0.1911 0.086 Uiso 1 1 calc R . . H14B H 0.8293 0.3007 0.1549 0.086 Uiso 1 1 calc R . . H14C H 0.8722 0.248 0.1347 0.086 Uiso 1 1 calc R . . C15 C 0.4965(5) 0.1326(3) 0.0833(2) 0.0468(16) Uani 1 1 d . . . H15 H 0.5087 0.1082 0.1134 0.056 Uiso 1 1 calc R . . C16 C 0.3793(5) 0.1328(3) 0.0674(3) 0.065(2) Uani 1 1 d . . . H16A H 0.3571 0.099 0.0557 0.097 Uiso 1 1 calc R . . H16B H 0.3642 0.1568 0.0383 0.097 Uiso 1 1 calc R . . H16C H 0.3418 0.1428 0.0981 0.097 Uiso 1 1 calc R . . C17 C 0.5542(6) 0.1124(3) 0.0371(3) 0.063(2) Uani 1 1 d . . . H17A H 0.5251 0.0796 0.0258 0.095 Uiso 1 1 calc R . . H17B H 0.6281 0.1085 0.0485 0.095 Uiso 1 1 calc R . . H17C H 0.5463 0.1361 0.0073 0.095 Uiso 1 1 calc R . . C18 C 0.6180(4) -0.0201(2) 0.2121(2) 0.0350(13) Uani 1 1 d . . . C19 C 0.6317(5) -0.0471(2) 0.2599(2) 0.0389(14) Uani 1 1 d . . . C20 C 0.5941(6) -0.0964(2) 0.2607(3) 0.0534(18) Uani 1 1 d . . . H20 H 0.6028 -0.1151 0.2928 0.064 Uiso 1 1 calc R . . C21 C 0.5453(6) -0.1184(3) 0.2168(3) 0.065(2) Uani 1 1 d . . . H21 H 0.5234 -0.1525 0.218 0.078 Uiso 1 1 calc R . . C22 C 0.5280(6) -0.0909(3) 0.1706(3) 0.0581(19) Uani 1 1 d . . . H22 H 0.4916 -0.1061 0.1404 0.07 Uiso 1 1 calc R . . C23 C 0.5626(5) -0.0415(2) 0.1671(3) 0.0425(15) Uani 1 1 d . . . C24 C 0.6877(5) -0.0257(2) 0.3096(2) 0.0459(16) Uani 1 1 d . . . H24 H 0.6988 0.0113 0.3042 0.055 Uiso 1 1 calc R . . C25 C 0.7946(6) -0.0510(4) 0.3222(3) 0.077(2) Uani 1 1 d . . . H25A H 0.8291 -0.0361 0.3545 0.115 Uiso 1 1 calc R . . H25B H 0.8377 -0.0459 0.2923 0.115 Uiso 1 1 calc R . . H25C H 0.7848 -0.0872 0.3277 0.115 Uiso 1 1 calc R . . C26 C 0.6228(7) -0.0328(3) 0.3574(3) 0.067(2) Uani 1 1 d . . . H26A H 0.6602 -0.0185 0.3893 0.1 Uiso 1 1 calc R . . H26B H 0.611 -0.0688 0.3629 0.1 Uiso 1 1 calc R . . H26C H 0.5559 -0.0156 0.3506 0.1 Uiso 1 1 calc R . . C27 C 0.5436(6) -0.0138(3) 0.1152(3) 0.0534(18) Uani 1 1 d . . . H27 H 0.5613 0.0225 0.122 0.064 Uiso 1 1 calc R . . C28 C 0.4303(6) -0.0160(3) 0.0929(3) 0.073(2) Uani 1 1 d . . . H28A H 0.4222 0.0026 0.0592 0.109 Uiso 1 1 calc R . . H28B H 0.386 -0.0008 0.1184 0.109 Uiso 1 1 calc R . . H28C H 0.4099 -0.0513 0.0867 0.109 Uiso 1 1 calc R . . C29 C 0.6131(7) -0.0330(3) 0.0736(3) 0.075(2) Uani 1 1 d . . . H29A H 0.5988 -0.0139 0.0405 0.112 Uiso 1 1 calc R . . H29B H 0.5991 -0.0688 0.0669 0.112 Uiso 1 1 calc R . . H29C H 0.6861 -0.0286 0.0865 0.112 Uiso 1 1 calc R . . C30 C 0.2997(4) 0.2854(2) 0.3681(2) 0.0374(14) Uani 1 1 d . . . C31 C 0.2686(5) 0.2622(2) 0.4143(2) 0.0395(14) Uani 1 1 d . . . H31 H 0.2012 0.2716 0.4233 0.047 Uiso 1 1 calc R . . C32 C 0.3187(4) 0.2280(2) 0.4490(2) 0.0371(14) Uani 1 1 d . . . C33 C 0.2383(5) 0.3328(2) 0.3516(3) 0.0495(17) Uani 1 1 d . . . H33A H 0.2713 0.3497 0.3227 0.074 Uiso 1 1 calc R . . H33B H 0.2372 0.3556 0.3821 0.074 Uiso 1 1 calc R . . H33C H 0.1669 0.3235 0.3393 0.074 Uiso 1 1 calc R . . C34 C 0.2683(5) 0.2222(3) 0.5015(2) 0.0526(17) Uani 1 1 d . . . H34A H 0.3159 0.2041 0.5271 0.079 Uiso 1 1 calc R . . H34B H 0.2034 0.2031 0.4955 0.079 Uiso 1 1 calc R . . H34C H 0.2534 0.2556 0.5157 0.079 Uiso 1 1 calc R . . C35 C 0.4102(4) 0.3017(2) 0.2985(2) 0.0324(13) Uani 1 1 d . . . C36 C 0.4959(5) 0.3336(2) 0.3101(2) 0.0394(14) Uani 1 1 d . . . C37 C 0.5296(5) 0.3638(2) 0.2696(3) 0.0486(16) Uani 1 1 d . . . H37 H 0.5867 0.386 0.2771 0.058 Uiso 1 1 calc R . . C38 C 0.4812(5) 0.3619(3) 0.2187(3) 0.0507(17) Uani 1 1 d . . . H38 H 0.5057 0.3823 0.1913 0.061 Uiso 1 1 calc R . . C39 C 0.3980(5) 0.3305(2) 0.2078(2) 0.0443(15) Uani 1 1 d . . . H39 H 0.365 0.3298 0.1727 0.053 Uiso 1 1 calc R . . C40 C 0.3602(4) 0.2996(2) 0.2465(2) 0.0364(13) Uani 1 1 d . . . C41 C 0.5487(5) 0.3380(3) 0.3658(3) 0.0514(17) Uani 1 1 d . . . H41 H 0.5332 0.3062 0.3849 0.062 Uiso 1 1 calc R . . C42 C 0.6677(5) 0.3424(3) 0.3669(3) 0.0605(19) Uani 1 1 d . . . H42A H 0.697 0.3446 0.4039 0.091 Uiso 1 1 calc R . . H42B H 0.6861 0.3727 0.3475 0.091 Uiso 1 1 calc R . . H42C H 0.6957 0.3126 0.3501 0.091 Uiso 1 1 calc R . . C43 C 0.5038(7) 0.3814(3) 0.3968(3) 0.074(2) Uani 1 1 d . . . H43A H 0.5389 0.3828 0.4327 0.112 Uiso 1 1 calc R . . H43B H 0.4292 0.376 0.3991 0.112 Uiso 1 1 calc R . . H43C H 0.5148 0.4133 0.3784 0.112 Uiso 1 1 calc R . . C44 C 0.2652(5) 0.2668(2) 0.2313(3) 0.0454(15) Uani 1 1 d . . . H44 H 0.25 0.246 0.2629 0.054 Uiso 1 1 calc R . . C45 C 0.1694(5) 0.2999(3) 0.2154(3) 0.062(2) Uani 1 1 d . . . H45A H 0.1567 0.3228 0.2447 0.092 Uiso 1 1 calc R . . H45B H 0.1084 0.2783 0.2076 0.092 Uiso 1 1 calc R . . H45C H 0.1822 0.3196 0.1837 0.092 Uiso 1 1 calc R . . C46 C 0.2832(6) 0.2315(3) 0.1855(3) 0.064(2) Uani 1 1 d . . . H46A H 0.2209 0.211 0.1771 0.097 Uiso 1 1 calc R . . H46B H 0.3424 0.2094 0.1956 0.097 Uiso 1 1 calc R . . H46C H 0.2981 0.2513 0.1542 0.097 Uiso 1 1 calc R . . C47 C 0.4589(5) 0.1786(2) 0.4851(2) 0.0376(14) Uani 1 1 d . . . C48 C 0.5298(5) 0.2079(3) 0.5177(2) 0.0410(15) Uani 1 1 d . . . C49 C 0.5751(6) 0.1857(3) 0.5641(3) 0.060(2) Uani 1 1 d . . . H49 H 0.621 0.2052 0.5872 0.072 Uiso 1 1 calc R . . C50 C 0.5560(6) 0.1373(3) 0.5773(3) 0.066(2) Uani 1 1 d . . . H50 H 0.5861 0.1237 0.6098 0.079 Uiso 1 1 calc R . . C51 C 0.4927(6) 0.1078(3) 0.5434(3) 0.062(2) Uani 1 1 d . . . H51 H 0.4827 0.0733 0.5517 0.075 Uiso 1 1 calc R . . C52 C 0.4429(5) 0.1281(3) 0.4969(2) 0.0483(16) Uani 1 1 d . . . C53 C 0.5558(5) 0.2622(2) 0.5044(2) 0.0453(15) Uani 1 1 d . . . H53 H 0.535 0.2675 0.4658 0.054 Uiso 1 1 calc R . . C54 C 0.6730(5) 0.2731(3) 0.5134(3) 0.0600(19) Uani 1 1 d . . . H54A H 0.6863 0.3083 0.5042 0.09 Uiso 1 1 calc R . . H54B H 0.7112 0.2508 0.4908 0.09 Uiso 1 1 calc R . . H54C H 0.6962 0.2673 0.5508 0.09 Uiso 1 1 calc R . . C55 C 0.4947(7) 0.2999(3) 0.5358(3) 0.074(2) Uani 1 1 d . . . H55A H 0.5132 0.3343 0.526 0.111 Uiso 1 1 calc R . . H55B H 0.5119 0.2949 0.574 0.111 Uiso 1 1 calc R . . H55C H 0.42 0.2947 0.5275 0.111 Uiso 1 1 calc R . . C56 C 0.3716(8) 0.0942(3) 0.4621(3) 0.077(3) Uani 1 1 d . . . H56 H 0.3571 0.1114 0.427 0.093 Uiso 1 1 calc R . . C57 C 0.2695(9) 0.0867(4) 0.4859(6) 0.130(5) Uani 1 1 d . . . H57A H 0.2245 0.0652 0.4624 0.195 Uiso 1 1 calc R . . H57B H 0.2359 0.1195 0.4899 0.195 Uiso 1 1 calc R . . H57C H 0.2816 0.0706 0.5208 0.195 Uiso 1 1 calc R . . C58 C 0.4160(10) 0.0431(3) 0.4518(4) 0.109(4) Uani 1 1 d . . . H58A H 0.3657 0.0237 0.429 0.163 Uiso 1 1 calc R . . H58B H 0.4307 0.0253 0.4857 0.163 Uiso 1 1 calc R . . H58C H 0.4804 0.0469 0.4341 0.163 Uiso 1 1 calc R . . C59 C 0.9079(11) 0.2545(4) 0.3754(5) 0.127(4) Uiso 1 1 d D . . H59A H 0.953 0.2642 0.3471 0.152 Uiso 1 1 calc R . . H59B H 0.8354 0.2627 0.3626 0.152 Uiso 1 1 calc R . . C60 C 0.9359(9) 0.2843(4) 0.4214(4) 0.110(4) Uiso 1 1 d D . . H60A H 0.9279 0.3201 0.4124 0.165 Uiso 1 1 calc R . . H60B H 1.0084 0.2775 0.4339 0.165 Uiso 1 1 calc R . . H60C H 0.8906 0.2757 0.4495 0.165 Uiso 1 1 calc R . . C61 C 1.0173(9) 0.1856(5) 0.3731(5) 0.126(4) Uiso 1 1 d D . . H61A H 1.0697 0.2089 0.3903 0.151 Uiso 1 1 calc R . . H61B H 1.0249 0.1853 0.3343 0.151 Uiso 1 1 calc R . . C62 C 1.0308(15) 0.1335(6) 0.3959(7) 0.206(8) Uiso 1 1 d D . . H62A H 1.1001 0.1208 0.3895 0.308 Uiso 1 1 calc R . . H62B H 0.9778 0.1111 0.3787 0.308 Uiso 1 1 calc R . . H62C H 1.0232 0.1345 0.4342 0.308 Uiso 1 1 calc R . . C63 C 0.7964(11) 0.0572(4) 0.4282(6) 0.140(5) Uiso 1 1 d D . . H63A H 0.7982 0.0496 0.3899 0.168 Uiso 1 1 calc R . . H63B H 0.7298 0.0446 0.4401 0.168 Uiso 1 1 calc R . . C64 C 0.8854(13) 0.0321(7) 0.4591(7) 0.196(7) Uiso 1 1 d D . . H64A H 0.8818 -0.0043 0.4529 0.294 Uiso 1 1 calc R . . H64B H 0.8819 0.039 0.4971 0.294 Uiso 1 1 calc R . . H64C H 0.9509 0.0452 0.4474 0.294 Uiso 1 1 calc R . . C65 C 0.7553(8) 0.1191(4) 0.4851(4) 0.092(3) Uiso 1 1 d D . . H65A H 0.7309 0.087 0.4999 0.111 Uiso 1 1 calc R . . H65B H 0.6949 0.1418 0.4783 0.111 Uiso 1 1 calc R . . C66 C 0.8355(11) 0.1430(6) 0.5231(6) 0.165(6) Uiso 1 1 d D . . H66A H 0.8052 0.1501 0.5567 0.248 Uiso 1 1 calc R . . H66B H 0.8594 0.1745 0.5078 0.248 Uiso 1 1 calc R . . H66C H 0.8946 0.12 0.5296 0.248 Uiso 1 1 calc R . . C67 C 0.0515(9) 0.1093(4) 0.2361(5) 0.115(4) Uiso 1 1 d D . . H67A H 0.0544 0.0991 0.274 0.138 Uiso 1 1 calc R . . H67B H -0.0073 0.0911 0.217 0.138 Uiso 1 1 calc R . . C68 C 0.0312(12) 0.1662(5) 0.2319(6) 0.154(5) Uiso 1 1 d D . . H68A H -0.0341 0.1742 0.2475 0.231 Uiso 1 1 calc R . . H68B H 0.0261 0.1763 0.1944 0.231 Uiso 1 1 calc R . . H68C H 0.0885 0.1844 0.2512 0.231 Uiso 1 1 calc R . . C69 C 0.1402(12) 0.1024(6) 0.1567(5) 0.145(5) Uiso 1 1 d D . . H69A H 0.0816 0.1252 0.1457 0.174 Uiso 1 1 calc R . . H69B H 0.2053 0.1178 0.1459 0.174 Uiso 1 1 calc R . . C70 C 0.1242(19) 0.0536(8) 0.1320(9) 0.273(12) Uiso 1 1 d D . . H70A H 0.1201 0.0573 0.0932 0.41 Uiso 1 1 calc R . . H70B H 0.0592 0.0389 0.1427 0.41 Uiso 1 1 calc R . . H70C H 0.1824 0.0313 0.1434 0.41 Uiso 1 1 calc R . . C71 C 0.3240(14) -0.0216(7) 0.3031(7) 0.204(8) Uiso 1 1 d D . . H71A H 0.3097 -0.0425 0.3343 0.244 Uiso 1 1 calc R . . H71B H 0.3949 -0.0072 0.3081 0.244 Uiso 1 1 calc R . . C72 C 0.3053(13) -0.0493(6) 0.2520(6) 0.175(6) Uiso 1 1 d D . . H72A H 0.3528 -0.0781 0.2517 0.263 Uiso 1 1 calc R . . H72B H 0.3175 -0.0266 0.2224 0.263 Uiso 1 1 calc R . . H72C H 0.2333 -0.0613 0.2482 0.263 Uiso 1 1 calc R . . C73 C 0.1414(16) 0.0053(13) 0.3094(13) 0.342(16) Uiso 1 1 d D . . H73A H 0.1024 0.0371 0.3126 0.41 Uiso 1 1 calc R . . H73B H 0.1012 -0.0173 0.2842 0.41 Uiso 1 1 calc R . . C74 C 0.162(3) -0.0195(14) 0.3624(14) 0.40(2) Uiso 1 1 d D . . H74A H 0.0958 -0.0291 0.3762 0.605 Uiso 1 1 calc R . . H74B H 0.1988 0.0041 0.3872 0.605 Uiso 1 1 calc R . . H74C H 0.2048 -0.0496 0.3587 0.605 Uiso 1 1 calc R . . O1A O 0.5079(10) 0.5117(6) 0.5101(7) 0.117(5) Uiso 0.5 1 d PD . . C1A C 0.6005(12) 0.5071(10) 0.4870(10) 0.270(12) Uiso 1 1 d D . . C2A C 0.6770(17) 0.5422(8) 0.5069(8) 0.215(8) Uiso 1 1 d 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 Y1 0.0250(3) 0.0258(3) 0.0284(3) -0.0019(2) 0.0034(2) 0.0014(2) Y2 0.0248(3) 0.0277(3) 0.0271(3) -0.0009(2) 0.0041(2) -0.0006(2) Li1 0.031(5) 0.050(6) 0.041(5) -0.007(5) -0.001(4) -0.001(5) Li2 0.048(7) 0.078(9) 0.074(8) -0.015(7) 0.018(6) -0.009(6) Cl1 0.0407(8) 0.0302(7) 0.0308(7) 0.0049(6) 0.0108(6) 0.0092(6) Cl2 0.0429(8) 0.0291(7) 0.0370(7) 0.0069(6) 0.0113(6) 0.0048(6) Cl3 0.0282(7) 0.0471(8) 0.0380(7) -0.0053(7) 0.0006(6) -0.0012(6) Cl4 0.0300(8) 0.0579(10) 0.0508(9) -0.0178(8) 0.0015(7) -0.0050(7) Cl5 0.0276(7) 0.0462(8) 0.0429(8) -0.0106(7) 0.0024(6) -0.0023(6) Cl6 0.0273(7) 0.0444(8) 0.0459(8) -0.0049(7) 0.0022(6) -0.0054(6) O1 0.031(2) 0.064(3) 0.084(4) -0.011(3) 0.002(2) -0.005(2) O2 0.080(4) 0.066(3) 0.050(3) 0.002(3) -0.007(3) 0.016(3) O3 0.044(3) 0.153(6) 0.084(4) -0.026(4) -0.002(3) -0.003(3) O4 0.100(5) 0.079(4) 0.140(6) 0.007(4) 0.018(4) -0.041(4) N1 0.030(3) 0.029(2) 0.030(2) 0.001(2) 0.0025(19) 0.003(2) N2 0.031(3) 0.021(2) 0.034(2) -0.0026(19) 0.004(2) -0.0028(19) N3 0.028(2) 0.028(2) 0.034(2) -0.003(2) 0.003(2) 0.0028(19) N4 0.026(2) 0.040(3) 0.030(2) -0.005(2) 0.0053(19) -0.004(2) C1 0.034(3) 0.030(3) 0.029(3) -0.006(2) 0.003(2) -0.001(2) C2 0.024(3) 0.034(3) 0.040(3) -0.003(3) 0.008(2) 0.001(2) C3 0.029(3) 0.029(3) 0.037(3) -0.008(3) 0.005(2) 0.000(2) C4 0.042(4) 0.040(3) 0.043(3) 0.003(3) 0.018(3) 0.003(3) C5 0.045(4) 0.030(3) 0.065(4) 0.003(3) 0.016(3) 0.010(3) C6 0.034(3) 0.038(3) 0.028(3) 0.002(3) 0.008(2) 0.005(3) C7 0.046(4) 0.036(3) 0.036(3) 0.004(3) 0.011(3) 0.002(3) C8 0.062(4) 0.037(3) 0.049(4) 0.006(3) 0.015(3) 0.004(3) C9 0.063(5) 0.043(4) 0.052(4) 0.013(3) 0.004(4) 0.018(3) C10 0.049(4) 0.061(5) 0.040(4) 0.009(3) -0.005(3) 0.016(3) C11 0.043(4) 0.042(3) 0.031(3) 0.004(3) 0.005(3) 0.006(3) C12 0.049(4) 0.033(3) 0.047(4) 0.001(3) 0.001(3) -0.007(3) C13 0.060(5) 0.061(4) 0.049(4) -0.006(4) 0.002(3) -0.016(4) C14 0.056(4) 0.047(4) 0.071(5) -0.008(4) 0.015(4) -0.013(3) C15 0.045(4) 0.052(4) 0.042(3) -0.002(3) -0.009(3) 0.004(3) C16 0.048(4) 0.070(5) 0.073(5) -0.005(4) -0.011(4) -0.003(4) C17 0.060(5) 0.073(5) 0.055(4) -0.020(4) -0.005(4) 0.008(4) C18 0.033(3) 0.025(3) 0.048(3) -0.005(3) 0.008(3) 0.002(2) C19 0.038(3) 0.032(3) 0.048(4) 0.002(3) 0.009(3) 0.001(3) C20 0.066(5) 0.035(4) 0.060(4) 0.006(3) 0.011(4) -0.006(3) C21 0.072(5) 0.029(3) 0.097(6) -0.001(4) 0.020(5) -0.011(3) C22 0.055(5) 0.040(4) 0.079(5) -0.013(4) 0.004(4) -0.015(3) C23 0.039(4) 0.036(3) 0.052(4) -0.008(3) 0.002(3) -0.003(3) C24 0.055(4) 0.041(4) 0.042(3) 0.010(3) 0.011(3) 0.007(3) C25 0.066(5) 0.093(6) 0.069(5) -0.006(5) -0.006(4) 0.021(5) C26 0.086(6) 0.062(5) 0.054(4) 0.010(4) 0.018(4) 0.001(4) C27 0.063(5) 0.043(4) 0.051(4) -0.015(3) -0.011(3) -0.006(3) C28 0.078(6) 0.070(5) 0.067(5) -0.019(4) -0.015(4) 0.004(4) C29 0.081(6) 0.093(6) 0.050(4) -0.011(4) 0.003(4) -0.002(5) C30 0.032(3) 0.036(3) 0.043(3) -0.005(3) 0.001(3) 0.003(3) C31 0.028(3) 0.050(4) 0.042(3) -0.005(3) 0.010(3) 0.004(3) C32 0.031(3) 0.048(4) 0.033(3) -0.008(3) 0.007(3) -0.009(3) C33 0.048(4) 0.049(4) 0.053(4) -0.003(3) 0.011(3) 0.020(3) C34 0.046(4) 0.074(5) 0.040(4) -0.003(3) 0.016(3) 0.000(4) C35 0.035(3) 0.026(3) 0.037(3) 0.001(2) 0.008(3) 0.003(2) C36 0.044(4) 0.030(3) 0.044(3) -0.001(3) 0.005(3) 0.002(3) C37 0.047(4) 0.033(3) 0.065(4) 0.004(3) 0.005(3) -0.011(3) C38 0.055(4) 0.048(4) 0.050(4) 0.017(3) 0.009(3) -0.002(3) C39 0.047(4) 0.045(4) 0.041(3) 0.012(3) 0.006(3) 0.002(3) C40 0.032(3) 0.034(3) 0.044(3) 0.005(3) 0.004(3) 0.007(3) C41 0.059(4) 0.043(4) 0.052(4) -0.001(3) 0.003(3) -0.013(3) C42 0.057(5) 0.049(4) 0.073(5) 0.012(4) -0.009(4) -0.010(3) C43 0.072(6) 0.083(6) 0.067(5) -0.031(5) 0.002(4) -0.016(5) C44 0.040(4) 0.050(4) 0.045(4) 0.009(3) -0.006(3) -0.002(3) C45 0.044(4) 0.082(5) 0.058(4) -0.004(4) -0.004(3) 0.009(4) C46 0.053(4) 0.059(5) 0.077(5) -0.017(4) -0.021(4) 0.008(4) C47 0.037(3) 0.051(4) 0.026(3) 0.000(3) 0.006(2) -0.001(3) C48 0.036(3) 0.061(4) 0.027(3) -0.003(3) 0.008(3) -0.002(3) C49 0.053(4) 0.097(6) 0.030(3) 0.002(4) -0.003(3) -0.012(4) C50 0.069(5) 0.091(6) 0.037(4) 0.025(4) -0.005(4) -0.009(5) C51 0.077(5) 0.069(5) 0.041(4) 0.015(4) 0.006(4) -0.004(4) C52 0.062(4) 0.056(4) 0.027(3) 0.007(3) 0.001(3) -0.006(3) C53 0.045(4) 0.052(4) 0.038(3) -0.011(3) 0.005(3) -0.008(3) C54 0.048(4) 0.078(5) 0.054(4) -0.011(4) 0.000(3) -0.018(4) C55 0.074(6) 0.074(5) 0.078(5) -0.030(5) 0.030(4) -0.009(4) C56 0.123(8) 0.058(5) 0.049(4) 0.023(4) -0.008(5) -0.034(5) C57 0.089(8) 0.087(8) 0.205(14) -0.012(8) -0.041(9) -0.021(6) C58 0.184(12) 0.067(6) 0.080(6) -0.002(5) 0.040(7) -0.035(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y1 N2 2.337(4) . ? Y1 N1 2.367(4) . ? Y1 Cl4 2.6286(15) . ? Y1 Cl3 2.6326(15) . ? Y1 Cl1 2.6793(14) . ? Y1 Cl2 2.7397(14) . ? Y2 N4 2.341(4) . ? Y2 N3 2.362(4) . ? Y2 Cl5 2.6223(15) . ? Y2 Cl6 2.6224(14) . ? Y2 Cl1 2.6766(13) . ? Y2 Cl2 2.7554(14) . ? Li1 O1 1.968(11) . ? Li1 O2 1.988(11) . ? Li1 Cl3 2.339(10) . ? Li1 Cl5 2.361(10) . ? Li2 O4 1.908(16) . ? Li2 O3 1.946(15) . ? Li2 Cl4 2.385(12) . ? Li2 Cl6 2.388(13) . ? O1 C61 1.410(10) . ? O1 C59 1.452(10) . ? O2 C63 1.416(11) . ? O2 C65 1.437(9) . ? O3 C67 1.438(10) . ? O3 C69 1.463(11) . ? O4 C71 1.407(13) . ? O4 C73 1.497(15) . ? N1 C1 1.333(7) . ? N1 C6 1.456(7) . ? N2 C3 1.337(7) . ? N2 C18 1.457(7) . ? N3 C30 1.335(7) . ? N3 C35 1.451(7) . ? N4 C32 1.331(7) . ? N4 C47 1.449(7) . ? C1 C2 1.394(8) . ? C1 C4 1.514(8) . ? C2 C3 1.388(8) . ? C3 C5 1.520(8) . ? C6 C7 1.407(8) . ? C6 C11 1.408(8) . ? C7 C8 1.402(9) . ? C7 C12 1.519(9) . ? C8 C9 1.364(9) . ? C9 C10 1.379(10) . ? C10 C11 1.400(9) . ? C11 C15 1.511(9) . ? C12 C13 1.522(9) . ? C12 C14 1.550(9) . ? C15 C17 1.527(9) . ? C15 C16 1.533(9) . ? C18 C19 1.402(8) . ? C18 C23 1.411(8) . ? C19 C20 1.394(9) . ? C19 C24 1.509(9) . ? C20 C21 1.361(10) . ? C21 C22 1.377(11) . ? C22 C23 1.391(9) . ? C23 C27 1.504(9) . ? C24 C26 1.532(9) . ? C24 C25 1.545(10) . ? C27 C29 1.520(10) . ? C27 C28 1.525(10) . ? C30 C31 1.402(8) . ? C30 C33 1.526(8) . ? C31 C32 1.385(8) . ? C32 C34 1.529(8) . ? C35 C36 1.405(8) . ? C35 C40 1.416(8) . ? C36 C37 1.393(9) . ? C36 C41 1.516(9) . ? C37 C38 1.385(9) . ? C38 C39 1.369(9) . ? C39 C40 1.393(8) . ? C40 C44 1.528(8) . ? C41 C43 1.531(10) . ? C41 C42 1.537(10) . ? C44 C46 1.519(9) . ? C44 C45 1.544(9) . ? C47 C52 1.392(9) . ? C47 C48 1.414(8) . ? C48 C49 1.396(9) . ? C48 C53 1.522(9) . ? C49 C50 1.353(11) . ? C50 C51 1.378(11) . ? C51 C52 1.401(9) . ? C52 C56 1.514(10) . ? C53 C55 1.532(9) . ? C53 C54 1.538(9) . ? C56 C57 1.502(14) . ? C56 C58 1.502(13) . ? C59 C60 1.424(11) . ? C61 C62 1.501(13) . ? C63 C64 1.492(13) . ? C65 C66 1.494(12) . ? C67 C68 1.534(12) . ? C69 C70 1.444(14) . ? C71 C72 1.486(13) . ? C73 C74 1.494(16) . ? O1A C1A 1.375(15) . ? O1A C1A 1.492(15) 3_666 ? C1A C2A 1.419(15) . ? 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 N2 Y1 N1 82.45(15) . . ? N2 Y1 Cl4 86.96(11) . . ? N1 Y1 Cl4 103.51(11) . . ? N2 Y1 Cl3 89.18(11) . . ? N1 Y1 Cl3 89.23(11) . . ? Cl4 Y1 Cl3 166.06(5) . . ? N2 Y1 Cl1 165.84(11) . . ? N1 Y1 Cl1 86.26(11) . . ? Cl4 Y1 Cl1 87.41(5) . . ? Cl3 Y1 Cl1 99.21(5) . . ? N2 Y1 Cl2 113.16(11) . . ? N1 Y1 Cl2 163.05(11) . . ? Cl4 Y1 Cl2 84.62(5) . . ? Cl3 Y1 Cl2 84.59(5) . . ? Cl1 Y1 Cl2 79.20(4) . . ? N4 Y2 N3 81.12(16) . . ? N4 Y2 Cl5 88.49(11) . . ? N3 Y2 Cl5 103.49(11) . . ? N4 Y2 Cl6 91.37(11) . . ? N3 Y2 Cl6 89.84(11) . . ? Cl5 Y2 Cl6 166.48(5) . . ? N4 Y2 Cl1 167.06(12) . . ? N3 Y2 Cl1 88.09(11) . . ? Cl5 Y2 Cl1 87.10(5) . . ? Cl6 Y2 Cl1 95.76(5) . . ? N4 Y2 Cl2 112.61(12) . . ? N3 Y2 Cl2 165.02(11) . . ? Cl5 Y2 Cl2 83.54(5) . . ? Cl6 Y2 Cl2 84.04(5) . . ? Cl1 Y2 Cl2 78.97(4) . . ? O1 Li1 O2 105.8(5) . . ? O1 Li1 Cl3 108.5(5) . . ? O2 Li1 Cl3 113.9(5) . . ? O1 Li1 Cl5 107.8(5) . . ? O2 Li1 Cl5 106.6(4) . . ? Cl3 Li1 Cl5 113.7(4) . . ? O4 Li2 O3 106.1(7) . . ? O4 Li2 Cl4 109.0(6) . . ? O3 Li2 Cl4 107.9(6) . . ? O4 Li2 Cl6 112.9(6) . . ? O3 Li2 Cl6 103.2(6) . . ? Cl4 Li2 Cl6 117.1(5) . . ? Y2 Cl1 Y1 102.66(4) . . ? Y1 Cl2 Y2 99.10(4) . . ? Li1 Cl3 Y1 118.6(2) . . ? Li2 Cl4 Y1 121.9(3) . . ? Li1 Cl5 Y2 124.9(2) . . ? Li2 Cl6 Y2 118.4(3) . . ? C61 O1 C59 107.9(8) . . ? C61 O1 Li1 125.8(7) . . ? C59 O1 Li1 120.3(7) . . ? C63 O2 C65 105.4(8) . . ? C63 O2 Li1 120.9(7) . . ? C65 O2 Li1 122.1(6) . . ? C67 O3 C69 110.9(9) . . ? C67 O3 Li2 120.7(7) . . ? C69 O3 Li2 127.3(8) . . ? C71 O4 C73 117.1(17) . . ? C71 O4 Li2 125.4(11) . . ? C73 O4 Li2 117.2(15) . . ? C1 N1 C6 118.1(4) . . ? C1 N1 Y1 119.6(3) . . ? C6 N1 Y1 121.9(3) . . ? C3 N2 C18 115.4(4) . . ? C3 N2 Y1 118.7(3) . . ? C18 N2 Y1 125.6(3) . . ? C30 N3 C35 117.7(4) . . ? C30 N3 Y2 122.7(4) . . ? C35 N3 Y2 119.4(3) . . ? C32 N4 C47 115.9(5) . . ? C32 N4 Y2 122.6(4) . . ? C47 N4 Y2 121.2(3) . . ? N1 C1 C2 125.3(5) . . ? N1 C1 C4 120.6(5) . . ? C2 C1 C4 114.1(5) . . ? C3 C2 C1 132.1(5) . . ? N2 C3 C2 125.1(5) . . ? N2 C3 C5 120.3(5) . . ? C2 C3 C5 114.6(5) . . ? C7 C6 C11 121.5(5) . . ? C7 C6 N1 120.9(5) . . ? C11 C6 N1 117.6(5) . . ? C8 C7 C6 117.2(6) . . ? C8 C7 C12 118.6(6) . . ? C6 C7 C12 124.2(5) . . ? C9 C8 C7 122.3(6) . . ? C8 C9 C10 120.0(6) . . ? C9 C10 C11 121.1(6) . . ? C10 C11 C6 118.0(6) . . ? C10 C11 C15 120.5(6) . . ? C6 C11 C15 121.3(5) . . ? C7 C12 C13 112.4(5) . . ? C7 C12 C14 111.1(5) . . ? C13 C12 C14 108.1(5) . . ? C11 C15 C17 111.7(6) . . ? C11 C15 C16 114.0(6) . . ? C17 C15 C16 109.4(6) . . ? C19 C18 C23 120.5(5) . . ? C19 C18 N2 121.9(5) . . ? C23 C18 N2 117.6(5) . . ? C20 C19 C18 118.1(6) . . ? C20 C19 C24 119.1(6) . . ? C18 C19 C24 122.8(5) . . ? C21 C20 C19 122.0(7) . . ? C20 C21 C22 119.7(6) . . ? C21 C22 C23 121.4(7) . . ? C22 C23 C18 118.2(6) . . ? C22 C23 C27 119.0(6) . . ? C18 C23 C27 122.7(5) . . ? C19 C24 C26 110.6(6) . . ? C19 C24 C25 111.6(6) . . ? C26 C24 C25 108.6(6) . . ? C23 C27 C29 111.9(6) . . ? C23 C27 C28 112.8(6) . . ? C29 C27 C28 109.4(6) . . ? N3 C30 C31 124.7(5) . . ? N3 C30 C33 121.0(5) . . ? C31 C30 C33 114.3(5) . . ? C32 C31 C30 131.4(5) . . ? N4 C32 C31 124.8(5) . . ? N4 C32 C34 121.4(6) . . ? C31 C32 C34 113.8(5) . . ? C36 C35 C40 120.6(5) . . ? C36 C35 N3 118.6(5) . . ? C40 C35 N3 120.7(5) . . ? C37 C36 C35 118.8(6) . . ? C37 C36 C41 119.4(6) . . ? C35 C36 C41 121.8(5) . . ? C38 C37 C36 120.9(6) . . ? C39 C38 C37 119.9(6) . . ? C38 C39 C40 122.0(6) . . ? C39 C40 C35 117.9(5) . . ? C39 C40 C44 118.5(5) . . ? C35 C40 C44 123.5(5) . . ? C36 C41 C43 111.8(6) . . ? C36 C41 C42 113.5(6) . . ? C43 C41 C42 110.5(6) . . ? C46 C44 C40 111.9(5) . . ? C46 C44 C45 108.7(5) . . ? C40 C44 C45 110.6(5) . . ? C52 C47 C48 120.3(6) . . ? C52 C47 N4 121.2(5) . . ? C48 C47 N4 118.4(5) . . ? C49 C48 C47 117.7(6) . . ? C49 C48 C53 120.0(6) . . ? C47 C48 C53 122.3(5) . . ? C50 C49 C48 122.3(7) . . ? C49 C50 C51 119.8(7) . . ? C50 C51 C52 120.7(7) . . ? C47 C52 C51 118.9(6) . . ? C47 C52 C56 122.8(6) . . ? C51 C52 C56 118.3(6) . . ? C48 C53 C55 111.9(6) . . ? C48 C53 C54 112.1(6) . . ? C55 C53 C54 109.9(6) . . ? C57 C56 C58 107.9(7) . . ? C57 C56 C52 111.1(8) . . ? C58 C56 C52 114.5(8) . . ? C60 C59 O1 114.9(10) . . ? O1 C61 C62 105.5(11) . . ? O2 C63 C64 108.7(12) . . ? O2 C65 C66 106.8(9) . . ? O3 C67 C68 112.8(10) . . ? C70 C69 O3 107.1(14) . . ? O4 C71 C72 95.5(12) . . ? C74 C73 O4 104(2) . . ? C1A O1A C1A 147.2(13) . 3_666 ? O1A C1A C2A 113(2) . . ? C2A C1A O1A 146(2) . 3_666 ? #===END data_(5a)-jun603 _database_code_depnum_ccdc_archive 'CCDC 684945' _audit_creation_date 2003-06-04T15:20:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H57 Cl2 N2 O2 Y' _chemical_formula_sum 'C37 H57 Cl2 N2 O2 Y' _chemical_formula_weight 721.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4162(1) _cell_length_b 24.0744(3) _cell_length_c 20.4590(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7593.07(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 54481 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5341 _exptl_absorpt_correction_T_max 0.5812 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.363697E-1 _diffrn_orient_matrix_ub_12 0.179784E-1 _diffrn_orient_matrix_ub_13 0.308149E-1 _diffrn_orient_matrix_ub_21 0.518441E-1 _diffrn_orient_matrix_ub_22 0.303E-3 _diffrn_orient_matrix_ub_23 0.249635E-1 _diffrn_orient_matrix_ub_31 0.140407E-1 _diffrn_orient_matrix_ub_32 0.454507E-1 _diffrn_orient_matrix_ub_33 -0.123555E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_unetI/netI 0.0357 _diffrn_reflns_number 75616 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 6673 _reflns_number_gt 5210 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _refine_special_details ; The disordered O2 THF ligand is included as two alterative orientations with 1,2 distance restraints (SADI) and isotropic displacement parameters. 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^)+(0.0137P)^2^+20.9549P] 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_number_reflns 6673 _refine_ls_number_parameters 395 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.583 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.16073(3) 0.412411(15) 0.13010(2) 0.03693(12) Uani 1 1 d . . . Cl1 Cl 0.07028(8) 0.40941(5) 0.02588(8) 0.0710(4) Uani 1 1 d . A . Cl2 Cl 0.20575(10) 0.43821(5) 0.24682(6) 0.0618(4) Uani 1 1 d . A . O1 O 0.12131(19) 0.50991(11) 0.12564(16) 0.0497(8) Uani 1 1 d . A . N1 N 0.2101(2) 0.31899(12) 0.13753(14) 0.0286(7) Uani 1 1 d . A . N2 N 0.2972(2) 0.42093(12) 0.07874(15) 0.0315(7) Uani 1 1 d . A . C1 C 0.2927(3) 0.30247(15) 0.13535(19) 0.0364(9) Uani 1 1 d . . . C2 C 0.3624(3) 0.33560(17) 0.1163(2) 0.0419(11) Uani 1 1 d . A . H2 H 0.4177 0.3197 0.1247 0.05 Uiso 1 1 calc R . . C3 C 0.3656(2) 0.38795(16) 0.08704(19) 0.0331(9) Uani 1 1 d . . . C4 C 0.3187(3) 0.24312(17) 0.1531(2) 0.0503(12) Uani 1 1 d . A . H4C H 0.2675 0.219 0.1512 0.075 Uiso 1 1 calc R . . H4B H 0.3429 0.2425 0.1974 0.075 Uiso 1 1 calc R . . H4A H 0.3624 0.2298 0.122 0.075 Uiso 1 1 calc R . . C5 C 0.4552(3) 0.40481(18) 0.0641(2) 0.0494(12) Uani 1 1 d . A . H5C H 0.4897 0.4171 0.1017 0.074 Uiso 1 1 calc R . . H5B H 0.4502 0.4352 0.0325 0.074 Uiso 1 1 calc R . . H5A H 0.4836 0.373 0.0433 0.074 Uiso 1 1 calc R . . C6 C 0.1449(3) 0.27756(14) 0.15236(18) 0.0296(9) Uani 1 1 d . . . C7 C 0.0986(3) 0.25416(16) 0.0996(2) 0.0462(11) Uani 1 1 d . A . C8 C 0.0336(4) 0.21644(19) 0.1141(3) 0.0649(15) Uani 1 1 d . . . H8 H 0.0013 0.2005 0.0793 0.078 Uiso 1 1 calc R A . C9 C 0.0143(3) 0.2014(2) 0.1771(3) 0.0658(15) Uani 1 1 d . A . H9 H -0.0309 0.1756 0.1856 0.079 Uiso 1 1 calc R . . C10 C 0.0607(3) 0.22391(18) 0.2281(2) 0.0504(12) Uani 1 1 d . . . H10 H 0.047 0.2134 0.2716 0.06 Uiso 1 1 calc R A . C11 C 0.1277(3) 0.26200(16) 0.21711(19) 0.0343(9) Uani 1 1 d . A . C12 C 0.1217(4) 0.26830(18) 0.0294(2) 0.0619(15) Uani 1 1 d . . . H12 H 0.1451 0.3071 0.0294 0.074 Uiso 1 1 calc R A . C13 C 0.0440(5) 0.2677(2) -0.0169(3) 0.100(3) Uani 1 1 d . A . H13C H 0.0176 0.2307 -0.0167 0.149 Uiso 1 1 calc R . . H13B H 0.0633 0.2768 -0.0612 0.149 Uiso 1 1 calc R . . H13A H 0.0013 0.2952 -0.0024 0.149 Uiso 1 1 calc R . . C14 C 0.1950(5) 0.2301(2) 0.0041(2) 0.093(2) Uani 1 1 d . A . H14C H 0.2466 0.2348 0.0315 0.139 Uiso 1 1 calc R . . H14B H 0.209 0.2399 -0.0412 0.139 Uiso 1 1 calc R . . H14A H 0.1758 0.1913 0.006 0.139 Uiso 1 1 calc R . . C15 C 0.1791(3) 0.28326(17) 0.27473(19) 0.0425(11) Uani 1 1 d . . . H15 H 0.2245 0.3094 0.2581 0.051 Uiso 1 1 calc R A . C16 C 0.2250(4) 0.2347(2) 0.3103(2) 0.0666(15) Uani 1 1 d . A . H16C H 0.1815 0.2084 0.3265 0.1 Uiso 1 1 calc R . . H16B H 0.2586 0.2493 0.3472 0.1 Uiso 1 1 calc R . . H16A H 0.264 0.2157 0.2798 0.1 Uiso 1 1 calc R . . C17 C 0.1227(4) 0.3144(2) 0.3241(2) 0.0671(16) Uani 1 1 d . A . H17C H 0.095 0.3461 0.3026 0.101 Uiso 1 1 calc R . . H17B H 0.159 0.3277 0.3602 0.101 Uiso 1 1 calc R . . H17A H 0.078 0.2893 0.3412 0.101 Uiso 1 1 calc R . . C18 C 0.3089(2) 0.47094(16) 0.04061(19) 0.0328(9) Uani 1 1 d . . . C19 C 0.2883(3) 0.46958(17) -0.0265(2) 0.0390(10) Uani 1 1 d . A . C20 C 0.2963(3) 0.51861(19) -0.0619(2) 0.0498(12) Uani 1 1 d . . . H20 H 0.2828 0.5186 -0.1072 0.06 Uiso 1 1 calc R A . C21 C 0.3233(3) 0.5672(2) -0.0327(2) 0.0533(13) Uani 1 1 d . A . H21 H 0.3271 0.6004 -0.0576 0.064 Uiso 1 1 calc R . . C22 C 0.3446(3) 0.56767(18) 0.0327(2) 0.0468(11) Uani 1 1 d . . . H22 H 0.3635 0.6013 0.0524 0.056 Uiso 1 1 calc R A . C23 C 0.3391(3) 0.51978(16) 0.0702(2) 0.0368(9) Uani 1 1 d . A . C24 C 0.2610(3) 0.41616(19) -0.0607(2) 0.0499(11) Uani 1 1 d . . . H24 H 0.2341 0.3913 -0.0271 0.06 Uiso 1 1 calc R A . C25 C 0.1933(4) 0.4261(2) -0.1145(3) 0.0813(19) Uani 1 1 d . A . H25C H 0.1416 0.4433 -0.0955 0.122 Uiso 1 1 calc R . . H25B H 0.1775 0.3905 -0.1346 0.122 Uiso 1 1 calc R . . H25A H 0.2177 0.4508 -0.1479 0.122 Uiso 1 1 calc R . . C26 C 0.3389(4) 0.3856(3) -0.0895(3) 0.0863(19) Uani 1 1 d . A . H26C H 0.3675 0.4094 -0.1218 0.129 Uiso 1 1 calc R . . H26B H 0.3193 0.3514 -0.1107 0.129 Uiso 1 1 calc R . . H26A H 0.3799 0.3765 -0.0545 0.129 Uiso 1 1 calc R . . C27 C 0.3698(3) 0.52205(18) 0.1404(2) 0.0507(12) Uani 1 1 d . . . H27 H 0.3622 0.4843 0.16 0.061 Uiso 1 1 calc R A . C28 C 0.4674(4) 0.5371(2) 0.1432(3) 0.0843(19) Uani 1 1 d . A . H28C H 0.5009 0.5093 0.1191 0.126 Uiso 1 1 calc R . . H28B H 0.4866 0.5378 0.1889 0.126 Uiso 1 1 calc R . . H28A H 0.4764 0.5738 0.1235 0.126 Uiso 1 1 calc R . . C29 C 0.3201(4) 0.5639(2) 0.1824(3) 0.0791(18) Uani 1 1 d . A . H29C H 0.3271 0.6012 0.164 0.119 Uiso 1 1 calc R . . H29B H 0.343 0.5632 0.2271 0.119 Uiso 1 1 calc R . . H29A H 0.2584 0.554 0.183 0.119 Uiso 1 1 calc R . . C30 C 0.0808(5) 0.5419(2) 0.1770(3) 0.092(2) Uani 1 1 d . . . H30B H 0.1145 0.5388 0.218 0.111 Uiso 1 1 calc R A . H30A H 0.0211 0.5284 0.1851 0.111 Uiso 1 1 calc R . . C31 C 0.0791(5) 0.6019(2) 0.1535(3) 0.098(2) Uani 1 1 d . A . H31B H 0.019 0.6164 0.1533 0.118 Uiso 1 1 calc R . . H31A H 0.1149 0.6257 0.1823 0.118 Uiso 1 1 calc R . . C32 C 0.1153(4) 0.60131(17) 0.0856(3) 0.0589(14) Uani 1 1 d . . . H32B H 0.1764 0.6141 0.0853 0.071 Uiso 1 1 calc R A . H32A H 0.0808 0.6253 0.0562 0.071 Uiso 1 1 calc R . . C33 C 0.1090(3) 0.54105(17) 0.0655(3) 0.0548(13) Uani 1 1 d . A . H33B H 0.0516 0.533 0.0461 0.066 Uiso 1 1 calc R . . H33A H 0.1546 0.5317 0.0333 0.066 Uiso 1 1 calc R . . O2 O 0.0304(3) 0.3844(2) 0.1885(2) 0.0401(14) Uiso 0.604(6) 1 d PD A 1 C34 C -0.0391(5) 0.3515(3) 0.1586(4) 0.049(2) Uiso 0.604(6) 1 d PD A 1 H34A H -0.0548 0.3197 0.1869 0.058 Uiso 0.604(6) 1 calc PR A 1 H34B H -0.0208 0.3372 0.1154 0.058 Uiso 0.604(6) 1 calc PR A 1 C35 C -0.1152(6) 0.3909(4) 0.1514(5) 0.067(3) Uiso 0.604(6) 1 d PD A 1 H35A H -0.1686 0.3743 0.1699 0.081 Uiso 0.604(6) 1 calc PR A 1 H35B H -0.1254 0.4 0.1049 0.081 Uiso 0.604(6) 1 calc PR A 1 C36 C -0.0889(6) 0.4424(4) 0.1895(5) 0.074(3) Uiso 0.604(6) 1 d PD A 1 H36A H -0.0696 0.4724 0.1598 0.089 Uiso 0.604(6) 1 calc PR A 1 H36B H -0.1373 0.4562 0.2169 0.089 Uiso 0.604(6) 1 calc PR A 1 C37 C -0.0159(5) 0.4218(3) 0.2305(3) 0.0438(19) Uiso 0.604(6) 1 d PD A 1 H37A H 0.0218 0.4529 0.2446 0.053 Uiso 0.604(6) 1 calc PR A 1 H37B H -0.0379 0.4023 0.2697 0.053 Uiso 0.604(6) 1 calc PR A 1 O2A O 0.0086(5) 0.4043(3) 0.1580(4) 0.041(2) Uiso 0.396(6) 1 d PD A 2 C34A C -0.0232(9) 0.3818(7) 0.2197(6) 0.079(5) Uiso 0.396(6) 1 d PD A 2 H34C H -0.0399 0.4121 0.2499 0.094 Uiso 0.396(6) 1 calc PR A 2 H34D H 0.0218 0.3586 0.241 0.094 Uiso 0.396(6) 1 calc PR A 2 C35A C -0.1003(9) 0.3475(6) 0.2019(7) 0.075(5) Uiso 0.396(6) 1 d PD A 2 H35C H -0.0847 0.3076 0.2007 0.09 Uiso 0.396(6) 1 calc PR A 2 H35D H -0.1473 0.3528 0.2343 0.09 Uiso 0.396(6) 1 calc PR A 2 C36A C -0.1288(10) 0.3667(7) 0.1361(7) 0.076(5) Uiso 0.396(6) 1 d PD A 2 H36C H -0.191 0.3767 0.1361 0.091 Uiso 0.396(6) 1 calc PR A 2 H36D H -0.1186 0.3377 0.1026 0.091 Uiso 0.396(6) 1 calc PR A 2 C37A C -0.0733(10) 0.4165(7) 0.1239(9) 0.108(6) Uiso 0.396(6) 1 d PD A 2 H37C H -0.0633 0.4218 0.0765 0.129 Uiso 0.396(6) 1 calc PR A 2 H37D H -0.1008 0.4504 0.1419 0.129 Uiso 0.396(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0351(2) 0.02079(18) 0.0549(3) -0.00616(18) 0.0140(2) -0.00195(18) Cl1 0.0547(7) 0.0382(6) 0.1201(12) -0.0111(7) -0.0381(8) 0.0081(6) Cl2 0.0989(10) 0.0385(6) 0.0481(7) -0.0060(6) 0.0208(7) -0.0110(7) O1 0.0530(18) 0.0210(14) 0.075(2) -0.0026(15) 0.0185(17) 0.0038(13) N1 0.0407(19) 0.0210(15) 0.0240(16) -0.0004(13) 0.0058(15) -0.0014(14) N2 0.0313(18) 0.0269(17) 0.0363(18) 0.0003(14) 0.0033(15) -0.0025(14) C1 0.046(3) 0.026(2) 0.037(2) 0.0007(17) 0.010(2) 0.0046(18) C2 0.035(2) 0.035(2) 0.056(3) 0.009(2) 0.007(2) 0.0083(18) C3 0.031(2) 0.033(2) 0.036(2) 0.0010(18) 0.0058(18) -0.0004(18) C4 0.055(3) 0.032(2) 0.063(3) 0.011(2) 0.023(2) 0.010(2) C5 0.035(2) 0.044(3) 0.069(3) 0.007(2) 0.011(2) 0.001(2) C6 0.039(2) 0.0195(18) 0.030(2) -0.0002(15) -0.0003(17) -0.0013(16) C7 0.072(3) 0.024(2) 0.042(3) -0.0043(19) -0.013(2) -0.004(2) C8 0.082(4) 0.039(3) 0.074(4) 0.000(3) -0.029(3) -0.025(3) C9 0.059(3) 0.043(3) 0.096(4) 0.008(3) 0.003(3) -0.019(3) C10 0.057(3) 0.039(2) 0.056(3) 0.014(2) 0.013(2) -0.002(2) C11 0.039(2) 0.028(2) 0.036(2) 0.0042(17) 0.0034(18) 0.0036(18) C12 0.126(5) 0.026(2) 0.034(3) -0.0064(19) -0.016(3) -0.010(3) C13 0.186(7) 0.057(4) 0.056(4) -0.007(3) -0.061(4) -0.014(4) C14 0.186(7) 0.055(3) 0.037(3) -0.009(3) 0.015(4) 0.019(4) C15 0.062(3) 0.039(2) 0.027(2) 0.0050(18) -0.004(2) 0.001(2) C16 0.090(4) 0.064(4) 0.046(3) 0.013(3) -0.010(3) 0.022(3) C17 0.120(5) 0.046(3) 0.035(3) 0.002(2) 0.012(3) 0.012(3) C18 0.030(2) 0.029(2) 0.039(2) 0.0016(17) 0.0063(18) 0.0002(17) C19 0.038(2) 0.038(2) 0.041(2) 0.0010(19) 0.004(2) 0.008(2) C20 0.058(3) 0.052(3) 0.039(3) 0.007(2) 0.004(2) 0.011(2) C21 0.060(3) 0.044(3) 0.055(3) 0.017(2) 0.012(2) -0.001(2) C22 0.053(3) 0.037(2) 0.051(3) 0.006(2) 0.004(2) -0.011(2) C23 0.035(2) 0.033(2) 0.042(2) 0.0058(18) 0.007(2) -0.0073(19) C24 0.058(3) 0.048(3) 0.043(3) -0.011(2) -0.006(2) 0.012(2) C25 0.104(5) 0.075(4) 0.065(4) -0.017(3) -0.034(3) 0.011(3) C26 0.079(4) 0.081(4) 0.099(5) -0.046(4) 0.005(4) 0.008(3) C27 0.071(3) 0.038(2) 0.044(3) 0.003(2) -0.003(2) -0.022(2) C28 0.087(4) 0.076(4) 0.090(5) 0.006(3) -0.038(4) -0.023(3) C29 0.113(5) 0.072(4) 0.052(3) -0.012(3) 0.005(3) -0.025(4) C30 0.121(5) 0.035(3) 0.121(5) 0.011(3) 0.078(5) 0.025(3) C31 0.143(6) 0.031(3) 0.120(6) 0.000(3) 0.057(5) 0.020(3) C32 0.073(3) 0.026(2) 0.078(4) 0.003(2) -0.009(3) -0.001(2) C33 0.059(3) 0.031(2) 0.075(4) 0.001(2) -0.014(3) 0.006(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N2 2.361(3) . ? Y N1 2.379(3) . ? Y O2A 2.422(7) . ? Y O1 2.426(3) . ? Y O2 2.433(5) . ? Y Cl1 2.5487(14) . ? Y Cl2 2.5631(13) . ? O1 C30 1.445(6) . ? O1 C33 1.453(5) . ? N1 C1 1.334(5) . ? N1 C6 1.449(5) . ? N2 C3 1.330(5) . ? N2 C18 1.446(5) . ? C1 C2 1.395(6) . ? C1 C4 1.528(5) . ? C2 C3 1.396(5) . ? C3 C5 1.514(5) . ? C6 C11 1.402(5) . ? C6 C7 1.411(5) . ? C7 C8 1.385(6) . ? C7 C12 1.519(6) . ? C8 C9 1.372(7) . ? C9 C10 1.375(7) . ? C10 C11 1.399(6) . ? C11 C15 1.510(6) . ? C12 C13 1.527(7) . ? C12 C14 1.546(8) . ? C15 C17 1.529(6) . ? C15 C16 1.548(6) . ? C18 C23 1.402(5) . ? C18 C19 1.409(6) . ? C19 C20 1.391(6) . ? C19 C24 1.524(6) . ? C20 C21 1.378(6) . ? C21 C22 1.377(6) . ? C22 C23 1.388(5) . ? C23 C27 1.512(6) . ? C24 C26 1.526(7) . ? C24 C25 1.536(6) . ? C27 C29 1.530(7) . ? C27 C28 1.548(7) . ? C30 C31 1.523(7) . ? C31 C32 1.496(8) . ? C32 C33 1.511(6) . ? O2 C37 1.435(7) . ? O2 C34 1.467(8) . ? C34 C35 1.514(9) . ? C35 C36 1.520(11) . ? C36 C37 1.488(9) . ? O2A C34A 1.459(12) . ? O2A C37A 1.472(13) . ? C34A C35A 1.491(13) . ? C35A C36A 1.490(13) . ? C36A C37A 1.493(14) . ? 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 N2 Y N1 79.94(10) . . ? N2 Y O2A 167.2(2) . . ? N1 Y O2A 102.6(2) . . ? N2 Y O1 97.03(10) . . ? N1 Y O1 175.55(11) . . ? O2A Y O1 81.06(19) . . ? N2 Y O2 168.15(14) . . ? N1 Y O2 88.33(14) . . ? O1 Y O2 94.58(14) . . ? N2 Y Cl1 96.76(8) . . ? N1 Y Cl1 101.64(8) . . ? O2A Y Cl1 70.44(18) . . ? O1 Y Cl1 81.89(8) . . ? O2 Y Cl1 87.21(12) . . ? N2 Y Cl2 98.76(8) . . ? N1 Y Cl2 94.75(8) . . ? O2A Y Cl2 93.56(18) . . ? O1 Y Cl2 82.44(8) . . ? O2 Y Cl2 80.39(12) . . ? Cl1 Y Cl2 159.14(5) . . ? C30 O1 C33 106.5(4) . . ? C30 O1 Y 126.6(3) . . ? C33 O1 Y 124.3(2) . . ? C1 N1 C6 117.7(3) . . ? C1 N1 Y 125.8(2) . . ? C6 N1 Y 116.2(2) . . ? C3 N2 C18 117.8(3) . . ? C3 N2 Y 126.7(2) . . ? C18 N2 Y 115.1(2) . . ? N1 C1 C2 125.1(3) . . ? N1 C1 C4 121.4(3) . . ? C2 C1 C4 113.5(4) . . ? C1 C2 C3 131.5(4) . . ? N2 C3 C2 124.5(4) . . ? N2 C3 C5 121.6(3) . . ? C2 C3 C5 114.0(4) . . ? C11 C6 C7 121.4(4) . . ? C11 C6 N1 120.9(3) . . ? C7 C6 N1 117.7(3) . . ? C8 C7 C6 117.6(4) . . ? C8 C7 C12 121.3(4) . . ? C6 C7 C12 121.1(4) . . ? C9 C8 C7 122.0(5) . . ? C8 C9 C10 119.8(4) . . ? C9 C10 C11 121.4(4) . . ? C10 C11 C6 117.8(4) . . ? C10 C11 C15 119.0(4) . . ? C6 C11 C15 123.3(4) . . ? C7 C12 C13 113.6(5) . . ? C7 C12 C14 110.7(4) . . ? C13 C12 C14 111.1(4) . . ? C11 C15 C17 112.6(4) . . ? C11 C15 C16 110.6(4) . . ? C17 C15 C16 108.6(4) . . ? C23 C18 C19 121.0(4) . . ? C23 C18 N2 120.4(3) . . ? C19 C18 N2 118.6(3) . . ? C20 C19 C18 117.9(4) . . ? C20 C19 C24 120.1(4) . . ? C18 C19 C24 122.0(4) . . ? C21 C20 C19 121.3(4) . . ? C22 C21 C20 120.1(4) . . ? C21 C22 C23 121.0(4) . . ? C22 C23 C18 118.5(4) . . ? C22 C23 C27 118.4(4) . . ? C18 C23 C27 123.0(3) . . ? C19 C24 C26 111.5(4) . . ? C19 C24 C25 112.7(4) . . ? C26 C24 C25 109.4(4) . . ? C23 C27 C29 113.6(4) . . ? C23 C27 C28 110.4(4) . . ? C29 C27 C28 108.1(4) . . ? O1 C30 C31 106.4(4) . . ? C32 C31 C30 106.1(4) . . ? C31 C32 C33 103.8(4) . . ? O1 C33 C32 104.9(4) . . ? C37 O2 C34 103.0(5) . . ? C37 O2 Y 122.1(4) . . ? C34 O2 Y 123.2(4) . . ? O2 C34 C35 105.6(6) . . ? C34 C35 C36 104.8(7) . . ? C37 C36 C35 102.6(7) . . ? O2 C37 C36 104.4(6) . . ? C34A O2A C37A 101.3(10) . . ? C34A O2A Y 124.0(8) . . ? C37A O2A Y 134.6(8) . . ? O2A C34A C35A 105.2(10) . . ? C36A C35A C34A 106.5(12) . . ? C35A C36A C37A 103.3(13) . . ? O2A C37A C36A 104.6(11) . . ? #===END data_(5b)-apr2003 _database_code_depnum_ccdc_archive 'CCDC 684946' _audit_creation_date 2003-04-15T13:52:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C33 H49 Cl2 N2 O2 Y, C4 H10 O' _chemical_formula_sum 'C37 H59 Cl2 N2 O3 Y' _chemical_formula_weight 739.67 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.2932(2) _cell_length_b 13.5936(1) _cell_length_c 20.4397(3) _cell_angle_alpha 90 _cell_angle_beta 94.757(1) _cell_angle_gamma 90 _cell_volume 3957.67(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33710 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6194 _exptl_absorpt_correction_T_max 0.7116 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.284652E-1 _diffrn_orient_matrix_ub_12 0.54184E-1 _diffrn_orient_matrix_ub_13 0.248359E-1 _diffrn_orient_matrix_ub_21 0.504511E-1 _diffrn_orient_matrix_ub_22 -0.80332E-2 _diffrn_orient_matrix_ub_23 0.365256E-1 _diffrn_orient_matrix_ub_31 0.396634E-1 _diffrn_orient_matrix_ub_32 0.491043E-1 _diffrn_orient_matrix_ub_33 -0.214297E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_unetI/netI 0.0483 _diffrn_reflns_number 52115 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 9026 _reflns_number_gt 6967 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0327P)^2^+5.0363P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 9026 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.883 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.133961(17) 0.258435(17) 0.053848(12) 0.02197(7) Uani 1 1 d . . . Cl1 Cl 0.14814(5) 0.42218(5) -0.00812(4) 0.03635(17) Uani 1 1 d . . . Cl2 Cl 0.08748(5) 0.09762(5) 0.11081(3) 0.03366(16) Uani 1 1 d . . . O1 O -0.00355(14) 0.22207(14) -0.01765(9) 0.0336(5) Uani 1 1 d . . . O2 O 0.02759(13) 0.34796(13) 0.11481(9) 0.0284(4) Uani 1 1 d . . . O3 O -0.2932(3) 0.2422(3) 0.1268(2) 0.1172(14) Uani 1 1 d . . . N1 N 0.26298(15) 0.27171(15) 0.13298(11) 0.0246(5) Uani 1 1 d . . . N2 N 0.25150(16) 0.18154(16) -0.00106(11) 0.0268(5) Uani 1 1 d . . . C1 C 0.33400(19) 0.2087(2) 0.14117(14) 0.0281(6) Uani 1 1 d . . . C2 C 0.3592(2) 0.1430(2) 0.09248(14) 0.0320(6) Uani 1 1 d . . . H2 H 0.4092 0.0997 0.1062 0.038 Uiso 1 1 calc R . . C3 C 0.3231(2) 0.1305(2) 0.02732(14) 0.0321(6) Uani 1 1 d . . . C4 C 0.3939(2) 0.2046(2) 0.20563(15) 0.0388(7) Uani 1 1 d . . . H4A H 0.4178 0.2705 0.217 0.058 Uiso 1 1 calc R . . H4B H 0.4468 0.1597 0.2015 0.058 Uiso 1 1 calc R . . H4C H 0.356 0.1808 0.2402 0.058 Uiso 1 1 calc R . . C5 C 0.3708(2) 0.0527(3) -0.01126(17) 0.0493(9) Uani 1 1 d . . . H5A H 0.3269 -0.0015 -0.0218 0.074 Uiso 1 1 calc R . . H5B H 0.4262 0.0278 0.0151 0.074 Uiso 1 1 calc R . . H5C H 0.39 0.0815 -0.052 0.074 Uiso 1 1 calc R . . C6 C 0.24468(18) 0.33145(19) 0.18869(13) 0.0251(6) Uani 1 1 d . . . C7 C 0.28218(19) 0.42636(19) 0.20191(13) 0.0271(6) Uani 1 1 d . . . C8 C 0.2543(2) 0.4726(2) 0.25837(14) 0.0330(6) Uani 1 1 d . . . H8 H 0.279 0.5361 0.2688 0.04 Uiso 1 1 calc R . . C9 C 0.1936(2) 0.4321(2) 0.29956(14) 0.0351(7) Uani 1 1 d . . . H9 H 0.1774 0.4669 0.3373 0.042 Uiso 1 1 calc R . . C10 C 0.1565(2) 0.3398(2) 0.28526(14) 0.0348(7) Uani 1 1 d . . . H10 H 0.1138 0.3106 0.3128 0.042 Uiso 1 1 calc R . . C11 C 0.18228(19) 0.2907(2) 0.23044(13) 0.0292(6) Uani 1 1 d . . . H11 H 0.1569 0.2273 0.2208 0.035 Uiso 1 1 calc R . . C12 C 0.3516(2) 0.4840(2) 0.16248(14) 0.0320(6) Uani 1 1 d . . . C13 C 0.3045(2) 0.5803(2) 0.13814(17) 0.0451(8) Uani 1 1 d . . . H13A H 0.3477 0.6177 0.1129 0.068 Uiso 1 1 calc R . . H13B H 0.2883 0.6194 0.1759 0.068 Uiso 1 1 calc R . . H13C H 0.2473 0.5652 0.1101 0.068 Uiso 1 1 calc R . . C14 C 0.3841(2) 0.4323(2) 0.10185(16) 0.0417(8) Uani 1 1 d . . . H14A H 0.4276 0.4751 0.0805 0.062 Uiso 1 1 calc R . . H14B H 0.3296 0.4179 0.071 0.062 Uiso 1 1 calc R . . H14C H 0.4159 0.3707 0.1151 0.062 Uiso 1 1 calc R . . C15 C 0.4393(2) 0.5074(3) 0.20872(17) 0.0509(9) Uani 1 1 d . . . H15A H 0.4845 0.5441 0.1846 0.076 Uiso 1 1 calc R . . H15B H 0.4681 0.4459 0.2253 0.076 Uiso 1 1 calc R . . H15C H 0.4213 0.5471 0.2456 0.076 Uiso 1 1 calc R . . C16 C 0.22292(19) 0.1621(2) -0.06903(13) 0.0289(6) Uani 1 1 d . . . C17 C 0.2578(2) 0.2106(2) -0.12298(14) 0.0338(7) Uani 1 1 d . . . C18 C 0.2169(2) 0.1846(3) -0.18533(15) 0.0455(8) Uani 1 1 d . . . H18 H 0.2387 0.2165 -0.2225 0.055 Uiso 1 1 calc R . . C19 C 0.1470(2) 0.1156(3) -0.19561(17) 0.0538(9) Uani 1 1 d . . . H19 H 0.1218 0.1007 -0.2389 0.065 Uiso 1 1 calc R . . C20 C 0.1137(2) 0.0680(3) -0.14258(17) 0.0484(9) Uani 1 1 d . . . H20 H 0.0656 0.0199 -0.1488 0.058 Uiso 1 1 calc R . . C21 C 0.1516(2) 0.0917(2) -0.08046(15) 0.0371(7) Uani 1 1 d . . . H21 H 0.1285 0.0592 -0.0439 0.045 Uiso 1 1 calc R . . C22 C 0.3379(2) 0.2877(2) -0.12239(15) 0.0366(7) Uani 1 1 d . . . C23 C 0.2987(3) 0.3825(3) -0.15461(18) 0.0510(9) Uani 1 1 d . . . H23A H 0.2691 0.3676 -0.1985 0.077 Uiso 1 1 calc R . . H23B H 0.3499 0.4296 -0.1583 0.077 Uiso 1 1 calc R . . H23C H 0.252 0.4111 -0.1277 0.077 Uiso 1 1 calc R . . C24 C 0.4157(2) 0.2455(3) -0.1620(2) 0.0564(10) Uani 1 1 d . . . H24A H 0.4403 0.1849 -0.141 0.085 Uiso 1 1 calc R . . H24B H 0.4664 0.2937 -0.1632 0.085 Uiso 1 1 calc R . . H24C H 0.3897 0.231 -0.2068 0.085 Uiso 1 1 calc R . . C25 C 0.3834(2) 0.3162(3) -0.05477(16) 0.0438(8) Uani 1 1 d . . . H25A H 0.4097 0.2574 -0.0324 0.066 Uiso 1 1 calc R . . H25B H 0.3361 0.3456 -0.0287 0.066 Uiso 1 1 calc R . . H25C H 0.4337 0.3639 -0.0598 0.066 Uiso 1 1 calc R . . C26 C -0.0289(3) 0.2748(3) -0.07888(18) 0.0598(11) Uani 1 1 d . . . H26A H 0.0256 0.2793 -0.1056 0.072 Uiso 1 1 calc R . . H26B H -0.0508 0.3421 -0.0698 0.072 Uiso 1 1 calc R . . C27 C -0.1068(3) 0.2154(3) -0.11419(19) 0.0613(10) Uani 1 1 d . . . H27A H -0.151 0.2584 -0.1408 0.074 Uiso 1 1 calc R . . H27B H -0.0813 0.1654 -0.1431 0.074 Uiso 1 1 calc R . . C28 C -0.1539(2) 0.1678(3) -0.05916(18) 0.0546(9) Uani 1 1 d . . . H28A H -0.1968 0.2141 -0.0392 0.066 Uiso 1 1 calc R . . H28B H -0.1892 0.1083 -0.0743 0.066 Uiso 1 1 calc R . . C29 C -0.0711(2) 0.1421(2) -0.01215(16) 0.0413(8) Uani 1 1 d . . . H29A H -0.09 0.1375 0.0333 0.05 Uiso 1 1 calc R . . H29B H -0.0436 0.0784 -0.0241 0.05 Uiso 1 1 calc R . . C30 C -0.0565(2) 0.3095(3) 0.14078(19) 0.0500(9) Uani 1 1 d . . . H30A H -0.04 0.2684 0.1801 0.06 Uiso 1 1 calc R . . H30B H -0.0927 0.2688 0.1074 0.06 Uiso 1 1 calc R . . C31 C -0.1127(2) 0.3973(3) 0.15838(18) 0.0495(9) Uani 1 1 d . . . H31A H -0.1556 0.4191 0.1206 0.059 Uiso 1 1 calc R . . H31B H -0.1499 0.3828 0.196 0.059 Uiso 1 1 calc R . . C32 C -0.0391(2) 0.4731(3) 0.17614(18) 0.0478(8) Uani 1 1 d . . . H32A H -0.0123 0.4647 0.222 0.057 Uiso 1 1 calc R . . H32B H -0.0651 0.5404 0.1706 0.057 Uiso 1 1 calc R . . C33 C 0.0335(2) 0.4538(2) 0.12845(16) 0.0366(7) Uani 1 1 d . . . H33A H 0.0198 0.4923 0.0877 0.044 Uiso 1 1 calc R . . H33B H 0.097 0.4716 0.148 0.044 Uiso 1 1 calc R . . C34 C -0.2713(3) 0.1451(3) 0.1423(2) 0.0777(13) Uani 1 1 d . . . H34A H -0.2157 0.1441 0.1746 0.093 Uiso 1 1 calc R . . H34B H -0.2537 0.1114 0.1022 0.093 Uiso 1 1 calc R . . C35 C -0.3478(3) 0.0884(4) 0.1697(2) 0.0854(14) Uani 1 1 d . . . H35A H -0.3265 0.0209 0.1791 0.128 Uiso 1 1 calc R . . H35B H -0.4028 0.0871 0.1377 0.128 Uiso 1 1 calc R . . H35C H -0.3646 0.1197 0.2103 0.128 Uiso 1 1 calc R . . C36 C -0.3598(4) 0.2622(5) 0.0783(4) 0.119(2) Uani 1 1 d . . . H36A H -0.4219 0.2475 0.0942 0.143 Uiso 1 1 calc R . . H36B H -0.3512 0.2173 0.0412 0.143 Uiso 1 1 calc R . . C37 C -0.3614(4) 0.3624(5) 0.0539(3) 0.120(2) Uani 1 1 d . . . H37A H -0.4108 0.369 0.0179 0.18 Uiso 1 1 calc R . . H37B H -0.3004 0.3782 0.0378 0.18 Uiso 1 1 calc R . . H37C H -0.3739 0.4077 0.0894 0.18 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 Y 0.02203(12) 0.01956(13) 0.02429(13) 0.00230(10) 0.00174(9) -0.00024(10) Cl1 0.0372(4) 0.0296(4) 0.0431(4) 0.0140(3) 0.0085(3) 0.0015(3) Cl2 0.0397(4) 0.0253(3) 0.0349(4) 0.0083(3) -0.0035(3) -0.0088(3) O1 0.0356(11) 0.0298(10) 0.0333(11) 0.0044(8) -0.0095(9) -0.0048(9) O2 0.0274(10) 0.0250(10) 0.0334(10) 0.0012(8) 0.0066(8) 0.0015(8) O3 0.083(3) 0.090(3) 0.175(4) 0.033(3) -0.009(3) -0.005(2) N1 0.0251(11) 0.0204(11) 0.0277(11) -0.0015(9) -0.0014(9) -0.0019(9) N2 0.0280(12) 0.0248(11) 0.0281(12) -0.0023(9) 0.0046(10) -0.0008(9) C1 0.0276(14) 0.0239(14) 0.0326(15) 0.0038(11) 0.0005(12) -0.0006(11) C2 0.0310(15) 0.0273(14) 0.0373(16) 0.0017(12) 0.0007(12) 0.0096(12) C3 0.0307(15) 0.0267(14) 0.0399(16) -0.0016(12) 0.0095(13) 0.0017(12) C4 0.0375(17) 0.0404(17) 0.0367(17) -0.0012(14) -0.0068(14) 0.0084(14) C5 0.047(2) 0.050(2) 0.051(2) -0.0151(16) 0.0018(16) 0.0202(16) C6 0.0244(13) 0.0236(13) 0.0259(14) 0.0010(10) -0.0052(11) 0.0018(11) C7 0.0255(14) 0.0250(14) 0.0299(14) -0.0010(11) -0.0040(11) -0.0014(11) C8 0.0336(16) 0.0273(15) 0.0367(16) -0.0066(12) -0.0060(13) -0.0009(12) C9 0.0379(17) 0.0372(16) 0.0299(15) -0.0076(13) 0.0004(13) 0.0064(13) C10 0.0339(16) 0.0399(17) 0.0310(15) 0.0034(13) 0.0043(13) 0.0033(13) C11 0.0297(15) 0.0260(14) 0.0314(15) 0.0016(11) -0.0005(12) -0.0005(11) C12 0.0299(15) 0.0276(14) 0.0378(16) -0.0032(12) -0.0006(13) -0.0094(12) C13 0.058(2) 0.0292(16) 0.0484(19) 0.0042(14) 0.0044(16) -0.0064(15) C14 0.0446(18) 0.0346(17) 0.0475(19) -0.0002(14) 0.0142(15) -0.0111(14) C15 0.0382(19) 0.059(2) 0.054(2) -0.0027(17) -0.0045(16) -0.0188(17) C16 0.0265(14) 0.0311(15) 0.0295(14) -0.0054(11) 0.0053(12) 0.0009(11) C17 0.0302(15) 0.0393(16) 0.0324(15) -0.0040(13) 0.0069(12) -0.0046(13) C18 0.0440(19) 0.063(2) 0.0308(16) -0.0033(15) 0.0095(15) -0.0095(17) C19 0.049(2) 0.074(3) 0.0372(19) -0.0154(17) -0.0008(16) -0.0173(19) C20 0.0412(19) 0.055(2) 0.049(2) -0.0123(17) 0.0069(16) -0.0190(16) C21 0.0352(16) 0.0386(17) 0.0389(17) -0.0055(13) 0.0113(14) -0.0091(13) C22 0.0321(16) 0.0423(17) 0.0370(16) -0.0028(13) 0.0127(13) -0.0068(13) C23 0.053(2) 0.048(2) 0.053(2) 0.0047(17) 0.0125(17) -0.0079(17) C24 0.0438(19) 0.062(2) 0.068(2) -0.0143(19) 0.0308(18) -0.0149(18) C25 0.0356(18) 0.050(2) 0.0462(19) -0.0038(15) 0.0049(15) -0.0176(15) C26 0.068(3) 0.053(2) 0.053(2) 0.0258(18) -0.0278(19) -0.0110(19) C27 0.057(2) 0.074(3) 0.048(2) 0.0078(19) -0.0220(18) -0.001(2) C28 0.039(2) 0.064(2) 0.058(2) -0.0030(19) -0.0137(17) -0.0026(17) C29 0.0344(17) 0.0442(18) 0.0437(18) -0.0004(15) -0.0067(14) -0.0124(14) C30 0.0401(19) 0.0445(19) 0.070(2) -0.0030(17) 0.0301(18) -0.0054(15) C31 0.0408(19) 0.052(2) 0.059(2) 0.0061(17) 0.0227(17) 0.0082(16) C32 0.048(2) 0.0434(19) 0.053(2) -0.0089(16) 0.0080(17) 0.0139(16) C33 0.0338(16) 0.0251(15) 0.0510(19) -0.0055(13) 0.0037(14) 0.0025(12) C34 0.078(3) 0.070(3) 0.086(3) -0.016(3) 0.014(3) -0.013(3) C35 0.078(3) 0.091(4) 0.089(4) -0.011(3) 0.018(3) -0.010(3) C36 0.077(4) 0.134(6) 0.142(6) 0.035(5) -0.023(4) -0.026(4) C37 0.084(4) 0.112(5) 0.161(6) 0.040(4) -0.016(4) -0.007(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N2 2.343(2) . ? Y N1 2.357(2) . ? Y O2 2.3790(18) . ? Y O1 2.4015(19) . ? Y Cl1 2.5773(7) . ? Y Cl2 2.5892(7) . ? O1 C26 1.461(4) . ? O1 C29 1.464(3) . ? O2 C30 1.451(3) . ? O2 C33 1.467(3) . ? O3 C36 1.345(7) . ? O3 C34 1.388(6) . ? N1 C1 1.328(3) . ? N1 C6 1.440(3) . ? N2 C3 1.330(4) . ? N2 C16 1.440(3) . ? C1 C2 1.407(4) . ? C1 C4 1.512(4) . ? C2 C3 1.398(4) . ? C3 C5 1.514(4) . ? C6 C11 1.399(4) . ? C6 C7 1.415(4) . ? C7 C8 1.401(4) . ? C7 C12 1.543(4) . ? C8 C9 1.374(4) . ? C9 C10 1.384(4) . ? C10 C11 1.380(4) . ? C12 C14 1.530(4) . ? C12 C13 1.536(4) . ? C12 C15 1.540(4) . ? C16 C21 1.404(4) . ? C16 C17 1.411(4) . ? C17 C18 1.403(4) . ? C17 C22 1.551(4) . ? C18 C19 1.374(5) . ? C19 C20 1.380(5) . ? C20 C21 1.377(4) . ? C22 C25 1.528(4) . ? C22 C23 1.532(5) . ? C22 C24 1.539(4) . ? C26 C27 1.509(5) . ? C27 C28 1.504(5) . ? C28 C29 1.502(4) . ? C30 C31 1.499(4) . ? C31 C32 1.495(5) . ? C32 C33 1.505(4) . ? C34 C35 1.484(6) . ? C36 C37 1.450(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Y N1 79.14(8) . . ? N2 Y O2 173.78(7) . . ? N1 Y O2 95.68(7) . . ? N2 Y O1 101.53(7) . . ? N1 Y O1 171.02(7) . . ? O2 Y O1 84.12(7) . . ? N2 Y Cl1 93.51(6) . . ? N1 Y Cl1 100.50(5) . . ? O2 Y Cl1 83.99(5) . . ? O1 Y Cl1 88.42(5) . . ? N2 Y Cl2 93.42(6) . . ? N1 Y Cl2 88.36(5) . . ? O2 Y Cl2 89.85(5) . . ? O1 Y Cl2 82.67(5) . . ? Cl1 Y Cl2 169.65(2) . . ? C26 O1 C29 108.1(2) . . ? C26 O1 Y 123.55(18) . . ? C29 O1 Y 128.14(16) . . ? C30 O2 C33 108.7(2) . . ? C30 O2 Y 126.28(17) . . ? C33 O2 Y 124.88(16) . . ? C36 O3 C34 119.6(5) . . ? C1 N1 C6 116.8(2) . . ? C1 N1 Y 125.70(18) . . ? C6 N1 Y 113.75(15) . . ? C3 N2 C16 118.2(2) . . ? C3 N2 Y 125.50(18) . . ? C16 N2 Y 112.76(16) . . ? N1 C1 C2 124.0(3) . . ? N1 C1 C4 120.4(2) . . ? C2 C1 C4 115.7(2) . . ? C3 C2 C1 130.9(3) . . ? N2 C3 C2 124.2(3) . . ? N2 C3 C5 120.0(3) . . ? C2 C3 C5 115.8(3) . . ? C11 C6 C7 119.7(2) . . ? C11 C6 N1 115.2(2) . . ? C7 C6 N1 125.1(2) . . ? C8 C7 C6 116.0(2) . . ? C8 C7 C12 116.2(2) . . ? C6 C7 C12 127.8(2) . . ? C9 C8 C7 124.2(3) . . ? C8 C9 C10 119.0(3) . . ? C11 C10 C9 119.1(3) . . ? C10 C11 C6 122.1(3) . . ? C14 C12 C13 106.5(3) . . ? C14 C12 C15 107.8(3) . . ? C13 C12 C15 109.6(3) . . ? C14 C12 C7 116.2(2) . . ? C13 C12 C7 108.5(2) . . ? C15 C12 C7 108.1(2) . . ? C21 C16 C17 119.2(3) . . ? C21 C16 N2 115.5(2) . . ? C17 C16 N2 125.3(2) . . ? C18 C17 C16 116.4(3) . . ? C18 C17 C22 115.4(3) . . ? C16 C17 C22 128.2(3) . . ? C19 C18 C17 123.6(3) . . ? C18 C19 C20 119.6(3) . . ? C21 C20 C19 118.7(3) . . ? C20 C21 C16 122.5(3) . . ? C25 C22 C23 106.8(3) . . ? C25 C22 C24 107.3(3) . . ? C23 C22 C24 110.0(3) . . ? C25 C22 C17 115.9(2) . . ? C23 C22 C17 108.8(3) . . ? C24 C22 C17 108.0(3) . . ? O1 C26 C27 105.6(3) . . ? C28 C27 C26 103.3(3) . . ? C29 C28 C27 101.6(3) . . ? O1 C29 C28 105.5(3) . . ? O2 C30 C31 106.1(3) . . ? C32 C31 C30 103.2(3) . . ? C31 C32 C33 103.4(3) . . ? O2 C33 C32 105.2(2) . . ? O3 C34 C35 114.9(4) . . ? O3 C36 C37 115.7(5) . . ? #===END data_(5c)-oct803 _database_code_depnum_ccdc_archive 'CCDC 684947' _audit_creation_date 2003-10-08T09:52:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H57 Cl2 N2 O2 Y' _chemical_formula_sum 'C41 H57 Cl2 N2 O2 Y' _chemical_formula_weight 769.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _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 34.5375(4) _cell_length_b 11.3522(1) _cell_length_c 23.4944(3) _cell_angle_alpha 90 _cell_angle_beta 117.072(1) _cell_angle_gamma 90 _cell_volume 8202.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 96424 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6694 _exptl_absorpt_correction_T_max 0.7728 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.9121E-2 _diffrn_orient_matrix_ub_12 -0.133016E-1 _diffrn_orient_matrix_ub_13 0.464479E-1 _diffrn_orient_matrix_ub_21 0.309175E-1 _diffrn_orient_matrix_ub_22 -0.80554E-2 _diffrn_orient_matrix_ub_23 0.80885E-2 _diffrn_orient_matrix_ub_31 0.42717E-2 _diffrn_orient_matrix_ub_32 0.867052E-1 _diffrn_orient_matrix_ub_33 0.78772E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_unetI/netI 0.04 _diffrn_reflns_number 50120 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 9338 _reflns_number_gt 7593 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There is disorder in the two THF groups. Disordered atomswere left isotropic and for the O2 THF group 1,2 distance restraints (SADI) weree applied. 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^)+(0.0320P)^2^+13.9206P] 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_number_reflns 9338 _refine_ls_number_parameters 429 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.559 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.154983(7) 0.238319(18) 0.179287(10) 0.02222(7) Uani 1 1 d . . . Cl1 Cl 0.164429(19) 0.01460(5) 0.19786(3) 0.03112(14) Uani 1 1 d . C . Cl2 Cl 0.16803(2) 0.46300(5) 0.18618(3) 0.03429(14) Uani 1 1 d . C . O1 O 0.22559(5) 0.22650(14) 0.18776(9) 0.0325(4) Uani 1 1 d . B . N1 N 0.11702(6) 0.21577(16) 0.06646(8) 0.0228(4) Uani 1 1 d . C . N2 N 0.08268(6) 0.26015(15) 0.16472(8) 0.0220(4) Uani 1 1 d . C . C1 C 0.07462(7) 0.22522(19) 0.02994(11) 0.0242(5) Uani 1 1 d . . . H1 H 0.0652 0.2145 -0.0145 0.029 Uiso 1 1 calc R C . C2 C 0.04164(7) 0.24877(19) 0.04745(10) 0.0235(4) Uani 1 1 d . C . C3 C 0.04686(7) 0.26379(18) 0.10982(10) 0.0232(5) Uani 1 1 d . . . H3 H 0.0209 0.2788 0.113 0.028 Uiso 1 1 calc R C . C4 C -0.00363(8) 0.2591(2) -0.00496(11) 0.0255(5) Uani 1 1 d . . . C5 C -0.02266(8) 0.1696(2) -0.05021(11) 0.0324(5) Uani 1 1 d . C . H5 H -0.0065 0.1005 -0.0478 0.039 Uiso 1 1 calc R . . C6 C -0.06492(9) 0.1807(3) -0.09865(12) 0.0416(7) Uani 1 1 d . . . H6 H -0.0774 0.1192 -0.129 0.05 Uiso 1 1 calc R C . C7 C -0.08885(9) 0.2808(3) -0.10289(13) 0.0441(7) Uani 1 1 d . C . H7 H -0.1177 0.2883 -0.1363 0.053 Uiso 1 1 calc R . . C8 C -0.07095(9) 0.3691(3) -0.05874(13) 0.0425(7) Uani 1 1 d . . . H8 H -0.0874 0.4378 -0.0615 0.051 Uiso 1 1 calc R C . C9 C -0.02889(8) 0.3583(2) -0.01002(12) 0.0327(5) Uani 1 1 d . C . H9 H -0.017 0.4197 0.0206 0.039 Uiso 1 1 calc R . . C10 C 0.14163(7) 0.1963(2) 0.03105(10) 0.0247(5) Uani 1 1 d . . . C11 C 0.14910(8) 0.0803(2) 0.01633(11) 0.0314(5) Uani 1 1 d . C . C12 C 0.17379(10) 0.0665(3) -0.01649(14) 0.0453(7) Uani 1 1 d . . . H12 H 0.1791 -0.0108 -0.0268 0.054 Uiso 1 1 calc R C . C13 C 0.19060(11) 0.1608(3) -0.03429(15) 0.0529(8) Uani 1 1 d . C . H13 H 0.2079 0.1485 -0.0557 0.063 Uiso 1 1 calc R . . C14 C 0.18224(10) 0.2737(3) -0.02099(14) 0.0451(7) Uani 1 1 d . . . H14 H 0.1934 0.3388 -0.0343 0.054 Uiso 1 1 calc R C . C15 C 0.15781(8) 0.2942(2) 0.01149(12) 0.0318(5) Uani 1 1 d . C . C16 C 0.12944(8) -0.0278(2) 0.03112(12) 0.0336(6) Uani 1 1 d . . . H16 H 0.1202 -0.0054 0.0643 0.04 Uiso 1 1 calc R C . C17 C 0.08894(11) -0.0672(3) -0.02874(14) 0.0531(8) Uani 1 1 d . C . H17C H 0.0676 -0.0031 -0.0434 0.08 Uiso 1 1 calc R . . H17B H 0.0763 -0.1365 -0.0186 0.08 Uiso 1 1 calc R . . H17A H 0.097 -0.087 -0.0625 0.08 Uiso 1 1 calc R . . C18 C 0.16168(10) -0.1300(2) 0.05761(16) 0.0501(8) Uani 1 1 d . C . H18C H 0.1714 -0.1533 0.026 0.075 Uiso 1 1 calc R . . H18B H 0.1475 -0.197 0.0667 0.075 Uiso 1 1 calc R . . H18A H 0.1868 -0.105 0.0971 0.075 Uiso 1 1 calc R . . C19 C 0.14631(9) 0.4191(2) 0.02042(13) 0.0384(6) Uani 1 1 d . . . H19 H 0.1346 0.4176 0.0522 0.046 Uiso 1 1 calc R C . C20 C 0.18581(12) 0.5008(3) 0.04607(17) 0.0622(9) Uani 1 1 d . C . H20C H 0.2076 0.472 0.0877 0.093 Uiso 1 1 calc R . . H20B H 0.1768 0.5806 0.0509 0.093 Uiso 1 1 calc R . . H20A H 0.1983 0.5023 0.0161 0.093 Uiso 1 1 calc R . . C21 C 0.11046(12) 0.4664(3) -0.04298(15) 0.0663(10) Uani 1 1 d . C . H21C H 0.1208 0.4656 -0.0755 0.099 Uiso 1 1 calc R . . H21B H 0.1031 0.5473 -0.0369 0.099 Uiso 1 1 calc R . . H21A H 0.0846 0.4165 -0.057 0.099 Uiso 1 1 calc R . . C22 C 0.07475(7) 0.27363(19) 0.22001(10) 0.0230(5) Uani 1 1 d . . . C23 C 0.07215(7) 0.1724(2) 0.25239(11) 0.0252(5) Uani 1 1 d . C . C24 C 0.06560(8) 0.1860(2) 0.30616(11) 0.0331(6) Uani 1 1 d . . . H24 H 0.0643 0.1181 0.3288 0.04 Uiso 1 1 calc R C . C25 C 0.06096(9) 0.2959(2) 0.32731(12) 0.0378(6) Uani 1 1 d . C . H25 H 0.0567 0.3034 0.3644 0.045 Uiso 1 1 calc R . . C26 C 0.06252(9) 0.3948(2) 0.29431(12) 0.0342(6) Uani 1 1 d . . . H26 H 0.0588 0.4702 0.3087 0.041 Uiso 1 1 calc R C . C27 C 0.06939(8) 0.3869(2) 0.24028(11) 0.0275(5) Uani 1 1 d . C . C28 C 0.07244(8) 0.0490(2) 0.22705(12) 0.0307(5) Uani 1 1 d . . . H28 H 0.0876 0.0535 0.1996 0.037 Uiso 1 1 calc R C . C29 C 0.02551(9) 0.0101(3) 0.18457(15) 0.0460(7) Uani 1 1 d . C . H29C H 0.0094 0.0094 0.2097 0.069 Uiso 1 1 calc R . . H29B H 0.0255 -0.0691 0.168 0.069 Uiso 1 1 calc R . . H29A H 0.0117 0.0652 0.1488 0.069 Uiso 1 1 calc R . . C30 C 0.09625(11) -0.0413(3) 0.27914(15) 0.0540(8) Uani 1 1 d . C . H30C H 0.1266 -0.0169 0.3043 0.081 Uiso 1 1 calc R . . H30B H 0.0953 -0.1182 0.2596 0.081 Uiso 1 1 calc R . . H30A H 0.0822 -0.0471 0.3071 0.081 Uiso 1 1 calc R . . C31 C 0.06843(8) 0.4993(2) 0.20402(12) 0.0310(5) Uani 1 1 d . . . H31 H 0.0805 0.4807 0.1736 0.037 Uiso 1 1 calc R C . C32 C 0.09604(10) 0.5969(2) 0.24875(14) 0.0432(7) Uani 1 1 d . C . H32C H 0.085 0.6156 0.2794 0.065 Uiso 1 1 calc R . . H32B H 0.0945 0.6674 0.2237 0.065 Uiso 1 1 calc R . . H32A H 0.1263 0.5705 0.2718 0.065 Uiso 1 1 calc R . . C33 C 0.02162(9) 0.5425(2) 0.16511(13) 0.0407(6) Uani 1 1 d . C . H33C H 0.0045 0.4816 0.1344 0.061 Uiso 1 1 calc R . . H33B H 0.0216 0.6145 0.1421 0.061 Uiso 1 1 calc R . . H33A H 0.0089 0.559 0.1939 0.061 Uiso 1 1 calc R . . C34 C 0.24316(8) 0.1261(2) 0.16825(14) 0.0363(6) Uani 1 1 d . . . H34B H 0.2201 0.0859 0.1308 0.044 Uiso 1 1 calc R A 1 H34A H 0.2568 0.0687 0.2036 0.044 Uiso 1 1 calc R A 1 C35 C 0.27619(10) 0.1792(3) 0.15170(16) 0.0472(7) Uani 0.507(19) 1 d P B 1 H35A H 0.2625 0.2209 0.1102 0.057 Uiso 0.507(19) 1 calc PR B 1 H35B H 0.2969 0.1195 0.151 0.057 Uiso 0.507(19) 1 calc PR B 1 C36 C 0.2984(2) 0.2660(7) 0.2086(5) 0.041(2) Uiso 0.507(19) 1 d P B 1 H36A H 0.3205 0.2252 0.2469 0.049 Uiso 0.507(19) 1 calc PR B 1 H36B H 0.3124 0.3319 0.1974 0.049 Uiso 0.507(19) 1 calc PR B 1 C37 C 0.26155(9) 0.3089(3) 0.21972(15) 0.0450(7) Uani 0.507(19) 1 d P B 1 H37A H 0.2703 0.3116 0.2661 0.054 Uiso 0.507(19) 1 calc PR B 1 H37B H 0.2528 0.3891 0.2019 0.054 Uiso 0.507(19) 1 calc PR B 1 O2 O 0.19101(16) 0.2513(4) 0.29286(19) 0.0274(12) Uiso 0.566(10) 1 d PD C 1 C38 C 0.2218(2) 0.1678(5) 0.3379(2) 0.0348(13) Uiso 0.566(10) 1 d PD C 1 H38A H 0.2521 0.1895 0.3484 0.042 Uiso 0.566(10) 1 calc PR C 1 H38B H 0.216 0.0869 0.3203 0.042 Uiso 0.566(10) 1 calc PR C 1 C39 C 0.2140(3) 0.1774(8) 0.3977(4) 0.070(2) Uiso 0.566(10) 1 d PD C 1 H39A H 0.1962 0.1101 0.3993 0.084 Uiso 0.566(10) 1 calc PR C 1 H39B H 0.242 0.1765 0.4371 0.084 Uiso 0.566(10) 1 calc PR C 1 C40 C 0.1919(3) 0.2846(6) 0.3930(3) 0.060(2) Uiso 0.566(10) 1 d PD C 1 H40A H 0.211 0.339 0.4272 0.072 Uiso 0.566(10) 1 calc PR C 1 H40B H 0.1656 0.2697 0.3986 0.072 Uiso 0.566(10) 1 calc PR C 1 C41 C 0.1797(2) 0.3372(5) 0.3317(2) 0.0369(14) Uiso 0.566(10) 1 d PD C 1 H41A H 0.1956 0.4121 0.3366 0.044 Uiso 0.566(10) 1 calc PR C 1 H41B H 0.1481 0.3541 0.3101 0.044 Uiso 0.566(10) 1 calc PR C 1 C35A C 0.27619(10) 0.1792(3) 0.15170(16) 0.0472(7) Uani 0.493(19) 1 d P B 2 H35C H 0.3016 0.126 0.1651 0.057 Uiso 0.493(19) 1 calc PR B 2 H35D H 0.2636 0.1913 0.1049 0.057 Uiso 0.493(19) 1 calc PR B 2 C36A C 0.2899(2) 0.2938(7) 0.1854(5) 0.038(2) Uiso 0.493(19) 1 d P B 2 H36C H 0.2848 0.3587 0.1547 0.045 Uiso 0.493(19) 1 calc PR B 2 H36D H 0.3212 0.2923 0.2166 0.045 Uiso 0.493(19) 1 calc PR B 2 C37A C 0.26155(9) 0.3089(3) 0.21972(15) 0.0450(7) Uani 0.493(19) 1 d P B 2 H37C H 0.2782 0.2895 0.2657 0.054 Uiso 0.493(19) 1 calc PR B 2 H37D H 0.2507 0.3907 0.2155 0.054 Uiso 0.493(19) 1 calc PR B 2 O2A O 0.1828(2) 0.2420(4) 0.2941(2) 0.0248(15) Uiso 0.434(10) 1 d PD C 2 C38A C 0.2067(3) 0.1499(7) 0.3385(3) 0.047(2) Uiso 0.434(10) 1 d PD C 2 H38C H 0.2295 0.1177 0.3284 0.056 Uiso 0.434(10) 1 calc PR C 2 H38D H 0.187 0.085 0.3365 0.056 Uiso 0.434(10) 1 calc PR C 2 C39A C 0.2272(3) 0.2053(7) 0.4046(3) 0.042(2) Uiso 0.434(10) 1 d PD C 2 H39C H 0.219 0.1609 0.4337 0.05 Uiso 0.434(10) 1 calc PR C 2 H39D H 0.2593 0.2054 0.4227 0.05 Uiso 0.434(10) 1 calc PR C 2 C40A C 0.2101(3) 0.3301(8) 0.3962(3) 0.058(3) Uiso 0.434(10) 1 d PD C 2 H40C H 0.1871 0.3367 0.4103 0.069 Uiso 0.434(10) 1 calc PR C 2 H40D H 0.2338 0.3858 0.4215 0.069 Uiso 0.434(10) 1 calc PR C 2 C41A C 0.1928(3) 0.3544(6) 0.3293(3) 0.0403(19) Uiso 0.434(10) 1 d PD C 2 H41C H 0.2142 0.3995 0.321 0.048 Uiso 0.434(10) 1 calc PR C 2 H41D H 0.166 0.4023 0.3149 0.048 Uiso 0.434(10) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.01957(11) 0.02462(11) 0.02042(11) 0.00023(9) 0.00731(8) 0.00042(9) Cl1 0.0306(3) 0.0256(3) 0.0352(3) 0.0021(2) 0.0133(3) 0.0010(2) Cl2 0.0321(3) 0.0256(3) 0.0403(3) 0.0008(2) 0.0122(3) 0.0004(2) O1 0.0225(9) 0.0308(9) 0.0442(10) -0.0085(7) 0.0152(8) -0.0020(7) N1 0.0213(10) 0.0280(10) 0.0200(9) -0.0005(7) 0.0101(8) -0.0006(7) N2 0.0231(9) 0.0242(9) 0.0200(9) -0.0006(7) 0.0109(8) 0.0005(7) C1 0.0267(12) 0.0265(11) 0.0182(10) -0.0003(9) 0.0092(9) -0.0017(9) C2 0.0223(11) 0.0251(11) 0.0212(11) -0.0001(9) 0.0083(9) -0.0013(9) C3 0.0221(11) 0.0228(11) 0.0269(12) -0.0013(9) 0.0130(9) -0.0004(9) C4 0.0244(11) 0.0314(12) 0.0212(11) 0.0009(9) 0.0110(9) 0.0000(9) C5 0.0294(14) 0.0398(14) 0.0281(13) -0.0059(11) 0.0132(11) -0.0016(11) C6 0.0303(15) 0.0632(19) 0.0274(13) -0.0113(13) 0.0098(11) -0.0112(13) C7 0.0225(13) 0.078(2) 0.0268(13) 0.0073(13) 0.0067(11) 0.0041(13) C8 0.0350(15) 0.0548(17) 0.0374(15) 0.0107(13) 0.0160(13) 0.0149(13) C9 0.0320(14) 0.0346(13) 0.0298(13) 0.0008(10) 0.0125(11) 0.0029(10) C10 0.0202(11) 0.0360(12) 0.0184(11) 0.0012(9) 0.0092(9) -0.0003(9) C11 0.0318(14) 0.0380(14) 0.0283(13) -0.0027(10) 0.0170(11) -0.0007(10) C12 0.0566(19) 0.0438(16) 0.0527(18) -0.0054(13) 0.0400(16) 0.0021(14) C13 0.059(2) 0.062(2) 0.062(2) 0.0024(16) 0.0493(18) 0.0038(16) C14 0.0491(18) 0.0502(17) 0.0509(17) 0.0052(14) 0.0357(15) -0.0051(13) C15 0.0283(13) 0.0399(14) 0.0282(13) 0.0043(10) 0.0136(11) -0.0011(10) C16 0.0402(15) 0.0330(13) 0.0336(14) -0.0078(10) 0.0222(12) -0.0051(11) C17 0.059(2) 0.0587(19) 0.0424(17) -0.0160(14) 0.0232(15) -0.0211(16) C18 0.059(2) 0.0351(15) 0.068(2) -0.0017(14) 0.0381(17) -0.0006(13) C19 0.0510(17) 0.0327(14) 0.0383(15) 0.0091(11) 0.0261(13) 0.0029(12) C20 0.082(3) 0.0460(18) 0.073(2) -0.0040(16) 0.047(2) -0.0196(17) C21 0.082(3) 0.065(2) 0.0496(19) 0.0235(17) 0.0283(19) 0.0276(19) C22 0.0210(11) 0.0290(11) 0.0190(11) -0.0032(9) 0.0092(9) -0.0012(9) C23 0.0252(12) 0.0268(11) 0.0241(12) -0.0003(9) 0.0115(10) -0.0020(9) C24 0.0398(15) 0.0361(13) 0.0260(13) 0.0029(10) 0.0173(11) -0.0025(11) C25 0.0486(17) 0.0446(15) 0.0281(13) -0.0050(11) 0.0243(13) -0.0040(12) C26 0.0417(15) 0.0347(13) 0.0323(14) -0.0087(11) 0.0220(12) -0.0022(11) C27 0.0264(12) 0.0301(12) 0.0267(12) -0.0022(9) 0.0127(10) -0.0022(9) C28 0.0362(14) 0.0271(12) 0.0361(13) -0.0015(10) 0.0227(12) -0.0024(10) C29 0.0444(17) 0.0466(16) 0.0556(18) -0.0202(14) 0.0303(15) -0.0131(13) C30 0.073(2) 0.0350(15) 0.059(2) 0.0123(14) 0.0354(18) 0.0122(15) C31 0.0352(14) 0.0278(12) 0.0350(13) 0.0002(10) 0.0204(12) 0.0017(10) C32 0.0491(17) 0.0307(13) 0.0488(17) -0.0033(12) 0.0216(14) -0.0051(12) C33 0.0404(16) 0.0374(14) 0.0464(16) 0.0055(12) 0.0216(13) 0.0049(12) C34 0.0284(13) 0.0332(13) 0.0483(16) -0.0059(11) 0.0183(12) 0.0023(10) C35 0.0451(17) 0.0408(15) 0.070(2) -0.0063(14) 0.0389(16) -0.0014(13) C37 0.0289(15) 0.0452(16) 0.0616(19) -0.0211(14) 0.0211(14) -0.0138(12) C35A 0.0451(17) 0.0408(15) 0.070(2) -0.0063(14) 0.0389(16) -0.0014(13) C37A 0.0289(15) 0.0452(16) 0.0616(19) -0.0211(14) 0.0211(14) -0.0138(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y O1 2.3586(16) . ? Y N2 2.3741(18) . ? Y N1 2.3765(18) . ? Y O2 2.381(4) . ? Y O2A 2.416(5) . ? Y Cl1 2.5724(6) . ? Y Cl2 2.5823(6) . ? O1 C34 1.460(3) . ? O1 C37 1.460(3) . ? N1 C1 1.322(3) . ? N1 C10 1.452(3) . ? N2 C3 1.320(3) . ? N2 C22 1.452(3) . ? C1 C2 1.402(3) . ? C2 C3 1.403(3) . ? C2 C4 1.491(3) . ? C4 C9 1.396(3) . ? C4 C5 1.399(3) . ? C5 C6 1.389(4) . ? C6 C7 1.381(4) . ? C7 C8 1.371(4) . ? C8 C9 1.386(4) . ? C10 C15 1.411(3) . ? C10 C11 1.415(3) . ? C11 C12 1.395(3) . ? C11 C16 1.517(3) . ? C12 C13 1.371(4) . ? C13 C14 1.381(4) . ? C14 C15 1.391(4) . ? C15 C19 1.513(4) . ? C16 C18 1.530(4) . ? C16 C17 1.531(4) . ? C19 C20 1.529(4) . ? C19 C21 1.537(4) . ? C22 C23 1.404(3) . ? C22 C27 1.412(3) . ? C23 C24 1.389(3) . ? C23 C28 1.523(3) . ? C24 C25 1.379(4) . ? C25 C26 1.380(4) . ? C26 C27 1.396(3) . ? C27 C31 1.526(3) . ? C28 C30 1.520(4) . ? C28 C29 1.532(4) . ? C31 C32 1.527(3) . ? C31 C33 1.531(4) . ? C34 C35 1.490(4) . ? C35 C36 1.553(7) . ? C36 C37 1.491(7) . ? O2 C38 1.458(6) . ? O2 C41 1.503(6) . ? C38 C39 1.550(8) . ? C39 C40 1.414(8) . ? C40 C41 1.435(7) . ? O2A C38A 1.444(8) . ? O2A C41A 1.474(7) . ? C38A C39A 1.518(9) . ? C39A C40A 1.513(9) . ? C40A C41A 1.432(9) . ? 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 Y N2 175.88(6) . . ? O1 Y N1 96.45(6) . . ? N2 Y N1 80.81(6) . . ? O1 Y O2 85.18(13) . . ? N2 Y O2 97.70(13) . . ? N1 Y O2 176.80(13) . . ? O1 Y O2A 92.06(16) . . ? N2 Y O2A 90.98(16) . . ? N1 Y O2A 169.75(16) . . ? O2 Y O2A 7.49(17) . . ? O1 Y Cl1 83.29(4) . . ? N2 Y Cl1 99.87(4) . . ? N1 Y Cl1 92.63(5) . . ? O2 Y Cl1 84.83(10) . . ? O2A Y Cl1 82.68(12) . . ? O1 Y Cl2 84.65(4) . . ? N2 Y Cl2 92.75(4) . . ? N1 Y Cl2 99.69(5) . . ? O2 Y Cl2 83.18(10) . . ? O2A Y Cl2 86.75(12) . . ? Cl1 Y Cl2 163.63(2) . . ? C34 O1 C37 106.48(18) . . ? C34 O1 Y 125.42(14) . . ? C37 O1 Y 127.72(14) . . ? C1 N1 C10 113.88(18) . . ? C1 N1 Y 126.94(15) . . ? C10 N1 Y 119.08(13) . . ? C3 N2 C22 113.34(18) . . ? C3 N2 Y 126.90(14) . . ? C22 N2 Y 119.75(13) . . ? N1 C1 C2 129.3(2) . . ? C1 C2 C3 126.5(2) . . ? C1 C2 C4 117.35(19) . . ? C3 C2 C4 116.2(2) . . ? N2 C3 C2 129.4(2) . . ? C9 C4 C5 117.5(2) . . ? C9 C4 C2 120.9(2) . . ? C5 C4 C2 121.6(2) . . ? C6 C5 C4 120.8(2) . . ? C7 C6 C5 120.3(3) . . ? C8 C7 C6 119.9(2) . . ? C7 C8 C9 120.1(3) . . ? C8 C9 C4 121.4(2) . . ? C15 C10 C11 120.7(2) . . ? C15 C10 N1 119.2(2) . . ? C11 C10 N1 120.1(2) . . ? C12 C11 C10 117.7(2) . . ? C12 C11 C16 119.1(2) . . ? C10 C11 C16 123.1(2) . . ? C13 C12 C11 122.1(3) . . ? C12 C13 C14 119.7(3) . . ? C13 C14 C15 121.4(3) . . ? C14 C15 C10 118.4(2) . . ? C14 C15 C19 119.7(2) . . ? C10 C15 C19 121.7(2) . . ? C11 C16 C18 112.8(2) . . ? C11 C16 C17 110.0(2) . . ? C18 C16 C17 110.1(2) . . ? C15 C19 C20 112.3(2) . . ? C15 C19 C21 109.9(2) . . ? C20 C19 C21 110.5(3) . . ? C23 C22 C27 120.8(2) . . ? C23 C22 N2 118.89(19) . . ? C27 C22 N2 120.30(19) . . ? C24 C23 C22 118.6(2) . . ? C24 C23 C28 119.4(2) . . ? C22 C23 C28 121.8(2) . . ? C25 C24 C23 121.5(2) . . ? C24 C25 C26 119.5(2) . . ? C25 C26 C27 121.6(2) . . ? C26 C27 C22 117.9(2) . . ? C26 C27 C31 118.9(2) . . ? C22 C27 C31 123.1(2) . . ? C30 C28 C23 113.8(2) . . ? C30 C28 C29 110.8(2) . . ? C23 C28 C29 109.0(2) . . ? C27 C31 C32 112.0(2) . . ? C27 C31 C33 110.5(2) . . ? C32 C31 C33 109.7(2) . . ? O1 C34 C35 104.1(2) . . ? C34 C35 C36 99.7(3) . . ? C37 C36 C35 103.4(4) . . ? O1 C37 C36 107.1(3) . . ? C38 O2 C41 106.6(4) . . ? C38 O2 Y 127.6(3) . . ? C41 O2 Y 124.9(3) . . ? O2 C38 C39 104.0(4) . . ? C40 C39 C38 107.4(6) . . ? C39 C40 C41 109.8(5) . . ? C40 C41 O2 107.5(4) . . ? C38A O2A C41A 108.1(5) . . ? C38A O2A Y 127.0(4) . . ? C41A O2A Y 121.0(4) . . ? O2A C38A C39A 106.6(5) . . ? C40A C39A C38A 106.4(6) . . ? C41A C40A C39A 105.4(6) . . ? C40A C41A O2A 108.9(6) . . ? #===END data_(6)-apr904 _database_code_depnum_ccdc_archive 'CCDC 684948' _audit_creation_date 2004-04-07T07:44:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C42 H58 Cl1 N4 Si4 Y' _chemical_formula_sum 'C42 H58 Cl1 N4 Si4 Y' _chemical_formula_weight 855.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 11.8676(2) _cell_length_b 12.4721(2) _cell_length_c 15.7658(3) _cell_angle_alpha 84.567(1) _cell_angle_beta 86.136(1) _cell_angle_gamma 89.915(1) _cell_volume 2317.77(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30094 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6003 _exptl_absorpt_correction_T_max 0.6772 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.785483E-1 _diffrn_orient_matrix_ub_12 0.169369E-1 _diffrn_orient_matrix_ub_13 -0.245639E-1 _diffrn_orient_matrix_ub_21 -0.232657E-1 _diffrn_orient_matrix_ub_22 0.754939E-1 _diffrn_orient_matrix_ub_23 -0.176216E-1 _diffrn_orient_matrix_ub_31 0.205352E-1 _diffrn_orient_matrix_ub_32 0.223781E-1 _diffrn_orient_matrix_ub_33 0.562518E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_number 38237 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.965 _reflns_number_total 8497 _reflns_number_gt 7731 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0194P)^2^+2.1498P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 8497 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.081 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.207 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.428 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.670775(18) 0.674463(18) 0.266171(14) 0.01840(7) Uani 1 1 d . . . Cl Cl 0.50553(5) 0.54569(5) 0.31126(4) 0.03181(15) Uani 1 1 d . . . Si1 Si 0.39698(6) 0.80018(6) 0.19235(5) 0.02595(16) Uani 1 1 d . . . Si2 Si 0.72182(6) 0.58462(6) 0.04728(4) 0.02388(15) Uani 1 1 d . . . Si3 Si 0.68385(6) 0.82387(6) 0.45952(4) 0.02655(16) Uani 1 1 d . . . Si4 Si 0.77640(6) 0.42632(5) 0.39631(4) 0.02457(16) Uani 1 1 d . . . N1 N 0.54310(16) 0.79860(16) 0.20348(12) 0.0212(4) Uani 1 1 d . . . N2 N 0.73417(16) 0.67633(15) 0.12400(12) 0.0203(4) Uani 1 1 d . . . N3 N 0.74123(16) 0.77894(16) 0.36387(12) 0.0217(4) Uani 1 1 d . . . N4 N 0.79505(16) 0.54955(16) 0.33209(12) 0.0210(4) Uani 1 1 d . . . C1 C 0.6163(2) 0.87885(19) 0.18114(14) 0.0205(5) Uani 1 1 d . . . C2 C 0.7298(2) 0.86428(19) 0.14951(15) 0.0218(5) Uani 1 1 d . . . H2 H 0.7812 0.9206 0.1565 0.026 Uiso 1 1 calc R . . C3 C 0.77525(19) 0.77594(19) 0.10883(15) 0.0205(5) Uani 1 1 d . . . C4 C 0.5829(2) 0.99328(19) 0.19027(16) 0.0236(5) Uani 1 1 d . . . C5 C 0.6153(2) 1.0759(2) 0.12756(18) 0.0317(6) Uani 1 1 d . . . H5 H 0.6607 1.0602 0.0784 0.038 Uiso 1 1 calc R . . C6 C 0.5815(3) 1.1813(2) 0.1367(2) 0.0423(7) Uani 1 1 d . . . H6 H 0.6025 1.2369 0.0931 0.051 Uiso 1 1 calc R . . C7 C 0.5180(3) 1.2052(2) 0.2083(2) 0.0426(8) Uani 1 1 d . . . H7 H 0.4954 1.2773 0.2145 0.051 Uiso 1 1 calc R . . C8 C 0.4868(3) 1.1246(2) 0.2714(2) 0.0411(7) Uani 1 1 d . . . H8 H 0.443 1.1414 0.3211 0.049 Uiso 1 1 calc R . . C9 C 0.5191(2) 1.0190(2) 0.26275(17) 0.0307(6) Uani 1 1 d . . . H9 H 0.4975 0.9639 0.3066 0.037 Uiso 1 1 calc R . . C10 C 0.8743(2) 0.8027(2) 0.04580(16) 0.0241(5) Uani 1 1 d . . . C11 C 0.8660(2) 0.8834(2) -0.02078(18) 0.0345(6) Uani 1 1 d . . . H11 H 0.7973 0.9219 -0.0261 0.041 Uiso 1 1 calc R . . C12 C 0.9568(3) 0.9082(2) -0.07960(19) 0.0429(7) Uani 1 1 d . . . H12 H 0.9495 0.9619 -0.1259 0.052 Uiso 1 1 calc R . . C13 C 1.0575(3) 0.8547(2) -0.07051(19) 0.0417(7) Uani 1 1 d . . . H13 H 1.1201 0.8723 -0.1101 0.05 Uiso 1 1 calc R . . C14 C 1.0677(2) 0.7761(3) -0.00444(19) 0.0397(7) Uani 1 1 d . . . H14 H 1.1378 0.7402 0.002 0.048 Uiso 1 1 calc R . . C15 C 0.9760(2) 0.7486(2) 0.05321(18) 0.0327(6) Uani 1 1 d . . . H15 H 0.983 0.6927 0.0978 0.039 Uiso 1 1 calc R . . C16 C 0.3484(3) 0.9224(2) 0.1269(2) 0.0444(8) Uani 1 1 d . . . H16A H 0.392 0.9301 0.0716 0.067 Uiso 1 1 calc R . . H16B H 0.3596 0.9864 0.157 0.067 Uiso 1 1 calc R . . H16C H 0.268 0.9147 0.1178 0.067 Uiso 1 1 calc R . . C17 C 0.3652(2) 0.6831(2) 0.13262(19) 0.0370(7) Uani 1 1 d . . . H17A H 0.4093 0.6893 0.0775 0.055 Uiso 1 1 calc R . . H17B H 0.2845 0.6821 0.1231 0.055 Uiso 1 1 calc R . . H17C H 0.3852 0.6162 0.1659 0.055 Uiso 1 1 calc R . . C18 C 0.3146(2) 0.7866(3) 0.29766(19) 0.0387(7) Uani 1 1 d . . . H18A H 0.3308 0.8482 0.3292 0.058 Uiso 1 1 calc R . . H18B H 0.3358 0.7198 0.3304 0.058 Uiso 1 1 calc R . . H18C H 0.2337 0.7847 0.2887 0.058 Uiso 1 1 calc R . . C19 C 0.6294(3) 0.4750(2) 0.1000(2) 0.0491(8) Uani 1 1 d . . . H19A H 0.5585 0.5056 0.1223 0.074 Uiso 1 1 calc R . . H19B H 0.6676 0.437 0.1472 0.074 Uiso 1 1 calc R . . H19C H 0.6131 0.4243 0.0585 0.074 Uiso 1 1 calc R . . C20 C 0.6530(3) 0.6570(3) -0.04368(19) 0.0417(7) Uani 1 1 d . . . H20A H 0.7031 0.7146 -0.0708 0.063 Uiso 1 1 calc R . . H20B H 0.5817 0.6883 -0.0228 0.063 Uiso 1 1 calc R . . H20C H 0.6377 0.6065 -0.0855 0.063 Uiso 1 1 calc R . . C21 C 0.8542(2) 0.5229(2) 0.00642(19) 0.0397(7) Uani 1 1 d . . . H21A H 0.9047 0.5793 -0.022 0.059 Uiso 1 1 calc R . . H21B H 0.8367 0.4718 -0.0345 0.059 Uiso 1 1 calc R . . H21C H 0.8913 0.4848 0.0541 0.059 Uiso 1 1 calc R . . C22 C 0.8478(2) 0.79105(19) 0.33087(15) 0.0209(5) Uani 1 1 d . . . C23 C 0.9079(2) 0.71061(19) 0.28985(15) 0.0216(5) Uani 1 1 d . . . H23 H 0.966 0.7354 0.2482 0.026 Uiso 1 1 calc R . . C24 C 0.89227(19) 0.59686(19) 0.30318(14) 0.0199(5) Uani 1 1 d . . . C25 C 0.9105(2) 0.8950(2) 0.33378(16) 0.0247(5) Uani 1 1 d . . . C26 C 0.8604(2) 0.9928(2) 0.30817(16) 0.0289(6) Uani 1 1 d . . . H26 H 0.7851 0.9938 0.2911 0.035 Uiso 1 1 calc R . . C27 C 0.9193(3) 1.0885(2) 0.30737(19) 0.0368(7) Uani 1 1 d . . . H27 H 0.8847 1.1546 0.2889 0.044 Uiso 1 1 calc R . . C28 C 1.0279(3) 1.0885(2) 0.3331(2) 0.0437(8) Uani 1 1 d . . . H28 H 1.0682 1.1544 0.3323 0.052 Uiso 1 1 calc R . . C29 C 1.0779(3) 0.9923(2) 0.3603(2) 0.0480(8) Uani 1 1 d . . . H29 H 1.1522 0.9923 0.3792 0.058 Uiso 1 1 calc R . . C30 C 1.0202(2) 0.8959(2) 0.3601(2) 0.0368(7) Uani 1 1 d . . . H30 H 1.0556 0.83 0.3779 0.044 Uiso 1 1 calc R . . C31 C 0.9932(2) 0.53003(19) 0.28021(15) 0.0224(5) Uani 1 1 d . . . C32 C 1.0994(2) 0.5518(2) 0.30684(17) 0.0283(6) Uani 1 1 d . . . H32 H 1.1099 0.6126 0.3375 0.034 Uiso 1 1 calc R . . C33 C 1.1904(2) 0.4854(2) 0.28900(19) 0.0375(7) Uani 1 1 d . . . H33 H 1.2625 0.5002 0.3082 0.045 Uiso 1 1 calc R . . C34 C 1.1757(2) 0.3983(2) 0.24338(18) 0.0402(7) Uani 1 1 d . . . H34 H 1.2377 0.3524 0.2317 0.048 Uiso 1 1 calc R . . C35 C 1.0714(3) 0.3770(2) 0.21439(18) 0.0365(7) Uani 1 1 d . . . H35 H 1.0621 0.3177 0.1818 0.044 Uiso 1 1 calc R . . C36 C 0.9806(2) 0.4424(2) 0.23320(16) 0.0285(6) Uani 1 1 d . . . H36 H 0.9088 0.4274 0.2137 0.034 Uiso 1 1 calc R . . C37 C 0.6753(3) 0.9725(2) 0.46815(19) 0.0402(7) Uani 1 1 d . . . H37A H 0.7515 1.0038 0.4605 0.06 Uiso 1 1 calc R . . H37B H 0.6413 0.9856 0.5246 0.06 Uiso 1 1 calc R . . H37C H 0.6289 1.0058 0.4239 0.06 Uiso 1 1 calc R . . C38 C 0.7718(3) 0.7655(3) 0.54525(19) 0.0449(8) Uani 1 1 d . . . H38A H 0.8483 0.7959 0.5361 0.067 Uiso 1 1 calc R . . H38B H 0.7754 0.6871 0.544 0.067 Uiso 1 1 calc R . . H38C H 0.7383 0.7826 0.6008 0.067 Uiso 1 1 calc R . . C39 C 0.5382(2) 0.7681(3) 0.4733(2) 0.0432(7) Uani 1 1 d . . . H39A H 0.4939 0.8003 0.4273 0.065 Uiso 1 1 calc R . . H39B H 0.503 0.7847 0.5285 0.065 Uiso 1 1 calc R . . H39C H 0.5409 0.6898 0.4713 0.065 Uiso 1 1 calc R . . C40 C 0.6821(2) 0.4581(2) 0.48902(18) 0.0375(7) Uani 1 1 d . . . H40A H 0.7183 0.5122 0.5195 0.056 Uiso 1 1 calc R . . H40B H 0.6676 0.3926 0.5276 0.056 Uiso 1 1 calc R . . H40C H 0.6105 0.4865 0.469 0.056 Uiso 1 1 calc R . . C41 C 0.9089(2) 0.3702(2) 0.44025(19) 0.0383(7) Uani 1 1 d . . . H41A H 0.9614 0.3518 0.3932 0.057 Uiso 1 1 calc R . . H41B H 0.8909 0.3054 0.4789 0.057 Uiso 1 1 calc R . . H41C H 0.9439 0.4241 0.4717 0.057 Uiso 1 1 calc R . . C42 C 0.7083(2) 0.3244(2) 0.33746(19) 0.0368(7) Uani 1 1 d . . . H42A H 0.7586 0.3081 0.2885 0.055 Uiso 1 1 calc R . . H42B H 0.6369 0.3529 0.3172 0.055 Uiso 1 1 calc R . . H42C H 0.6936 0.2585 0.3756 0.055 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 Y 0.01535(12) 0.01915(12) 0.02049(12) -0.00114(9) -0.00069(8) 0.00025(8) Cl 0.0204(3) 0.0325(3) 0.0407(4) 0.0046(3) 0.0003(3) -0.0057(3) Si1 0.0176(3) 0.0293(4) 0.0308(4) -0.0009(3) -0.0038(3) 0.0028(3) Si2 0.0237(3) 0.0235(4) 0.0250(4) -0.0063(3) 0.0000(3) 0.0007(3) Si3 0.0252(4) 0.0303(4) 0.0248(4) -0.0073(3) -0.0003(3) 0.0007(3) Si4 0.0238(4) 0.0220(4) 0.0270(4) 0.0029(3) -0.0021(3) -0.0016(3) N1 0.0182(10) 0.0213(10) 0.0235(10) 0.0008(8) -0.0016(8) 0.0011(8) N2 0.0185(10) 0.0205(10) 0.0216(10) -0.0013(8) 0.0004(8) 0.0011(8) N3 0.0198(10) 0.0234(11) 0.0224(10) -0.0041(8) -0.0017(8) 0.0019(8) N4 0.0187(10) 0.0204(10) 0.0236(10) 0.0001(8) -0.0023(8) -0.0008(8) C1 0.0219(12) 0.0208(12) 0.0188(12) -0.0005(10) -0.0040(9) 0.0016(10) C2 0.0196(12) 0.0208(12) 0.0253(12) -0.0037(10) -0.0004(10) -0.0020(10) C3 0.0188(12) 0.0221(12) 0.0206(12) -0.0001(10) -0.0033(9) -0.0009(10) C4 0.0232(13) 0.0196(12) 0.0288(13) -0.0024(10) -0.0069(10) 0.0034(10) C5 0.0359(15) 0.0250(14) 0.0340(15) -0.0016(11) -0.0026(12) 0.0017(11) C6 0.0536(19) 0.0253(15) 0.0474(18) 0.0041(13) -0.0101(15) 0.0029(13) C7 0.0511(19) 0.0232(15) 0.057(2) -0.0102(14) -0.0189(16) 0.0099(13) C8 0.0443(17) 0.0389(17) 0.0433(17) -0.0189(14) -0.0067(14) 0.0129(14) C9 0.0309(14) 0.0302(14) 0.0314(14) -0.0048(12) -0.0031(11) 0.0047(11) C10 0.0225(13) 0.0235(13) 0.0258(13) -0.0026(10) 0.0020(10) -0.0022(10) C11 0.0339(15) 0.0316(15) 0.0355(15) 0.0039(12) 0.0062(12) 0.0031(12) C12 0.0499(19) 0.0376(17) 0.0369(16) 0.0084(13) 0.0122(14) -0.0043(14) C13 0.0351(16) 0.0452(18) 0.0423(17) -0.0054(14) 0.0172(13) -0.0117(14) C14 0.0226(14) 0.0489(18) 0.0469(18) -0.0074(15) 0.0063(12) 0.0027(13) C15 0.0254(14) 0.0356(15) 0.0358(15) 0.0009(12) 0.0011(11) 0.0006(12) C16 0.0372(17) 0.0411(17) 0.056(2) 0.0049(15) -0.0227(15) 0.0051(14) C17 0.0300(15) 0.0414(17) 0.0408(16) -0.0062(13) -0.0086(12) -0.0020(12) C18 0.0217(14) 0.0466(18) 0.0471(17) -0.0069(14) 0.0049(12) 0.0015(12) C19 0.063(2) 0.0348(17) 0.0504(19) -0.0168(15) 0.0095(16) -0.0209(15) C20 0.0368(16) 0.056(2) 0.0350(16) -0.0132(14) -0.0102(13) 0.0098(14) C21 0.0392(16) 0.0431(17) 0.0385(16) -0.0148(14) -0.0017(13) 0.0159(14) C22 0.0216(12) 0.0209(12) 0.0205(12) -0.0002(10) -0.0054(10) -0.0005(10) C23 0.0181(12) 0.0230(13) 0.0230(12) -0.0013(10) 0.0023(9) 0.0000(10) C24 0.0172(12) 0.0243(12) 0.0186(12) -0.0023(10) -0.0034(9) 0.0026(10) C25 0.0219(13) 0.0253(13) 0.0276(13) -0.0065(11) -0.0008(10) -0.0011(10) C26 0.0278(14) 0.0281(14) 0.0313(14) -0.0046(11) -0.0045(11) 0.0011(11) C27 0.0447(17) 0.0240(14) 0.0428(17) -0.0055(12) -0.0077(13) -0.0003(12) C28 0.0434(18) 0.0290(16) 0.060(2) -0.0111(14) -0.0065(15) -0.0115(13) C29 0.0319(16) 0.0389(18) 0.077(2) -0.0124(16) -0.0204(16) -0.0068(14) C30 0.0298(15) 0.0277(14) 0.0548(18) -0.0071(13) -0.0124(13) 0.0015(12) C31 0.0200(12) 0.0237(13) 0.0224(12) 0.0020(10) 0.0012(10) 0.0013(10) C32 0.0206(13) 0.0306(14) 0.0328(14) 0.0000(11) 0.0000(11) -0.0010(11) C33 0.0212(14) 0.0483(18) 0.0407(16) 0.0053(14) 0.0025(12) 0.0042(12) C34 0.0344(16) 0.0462(18) 0.0369(16) 0.0028(14) 0.0108(13) 0.0185(14) C35 0.0473(18) 0.0317(15) 0.0298(15) -0.0060(12) 0.0062(13) 0.0108(13) C36 0.0293(14) 0.0305(14) 0.0251(13) -0.0016(11) 0.0005(11) 0.0019(11) C37 0.0443(17) 0.0385(17) 0.0390(16) -0.0139(13) 0.0031(13) 0.0048(14) C38 0.056(2) 0.0473(19) 0.0335(16) -0.0084(14) -0.0119(14) 0.0049(15) C39 0.0326(16) 0.0536(19) 0.0437(17) -0.0141(15) 0.0084(13) -0.0052(14) C40 0.0387(16) 0.0386(16) 0.0329(15) 0.0033(13) 0.0049(12) -0.0069(13) C41 0.0355(16) 0.0422(17) 0.0351(15) 0.0104(13) -0.0062(12) 0.0042(13) C42 0.0388(16) 0.0249(14) 0.0477(17) -0.0048(13) -0.0071(13) -0.0035(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N3 2.3079(19) . ? Y N2 2.3137(19) . ? Y N1 2.3611(19) . ? Y N4 2.3612(19) . ? Y Cl 2.5566(6) . ? Si1 N1 1.755(2) . ? Si1 C18 1.863(3) . ? Si1 C17 1.863(3) . ? Si1 C16 1.871(3) . ? Si2 N2 1.755(2) . ? Si2 C19 1.852(3) . ? Si2 C21 1.852(3) . ? Si2 C20 1.858(3) . ? Si3 N3 1.753(2) . ? Si3 C39 1.855(3) . ? Si3 C38 1.857(3) . ? Si3 C37 1.874(3) . ? Si4 N4 1.764(2) . ? Si4 C40 1.853(3) . ? Si4 C42 1.859(3) . ? Si4 C41 1.869(3) . ? N1 C1 1.332(3) . ? N2 C3 1.330(3) . ? N3 C22 1.338(3) . ? N4 C24 1.329(3) . ? C1 C2 1.422(3) . ? C1 C4 1.498(3) . ? C2 C3 1.415(3) . ? C3 C10 1.504(3) . ? C4 C9 1.390(4) . ? C4 C5 1.395(4) . ? C5 C6 1.391(4) . ? C6 C7 1.372(4) . ? C7 C8 1.378(4) . ? C8 C9 1.388(4) . ? C10 C15 1.389(4) . ? C10 C11 1.392(4) . ? C11 C12 1.389(4) . ? C12 C13 1.378(4) . ? C13 C14 1.373(4) . ? C14 C15 1.392(4) . ? C22 C23 1.412(3) . ? C22 C25 1.502(3) . ? C23 C24 1.425(3) . ? C24 C31 1.502(3) . ? C25 C26 1.393(4) . ? C25 C30 1.394(4) . ? C26 C27 1.383(4) . ? C27 C28 1.376(4) . ? C28 C29 1.383(4) . ? C29 C30 1.385(4) . ? C31 C32 1.390(3) . ? C31 C36 1.391(4) . ? C32 C33 1.389(4) . ? C33 C34 1.377(4) . ? C34 C35 1.383(4) . ? C35 C36 1.384(4) . ? 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 N3 Y N2 125.66(7) . . ? N3 Y N1 99.31(7) . . ? N2 Y N1 79.87(7) . . ? N3 Y N4 80.31(7) . . ? N2 Y N4 101.56(7) . . ? N1 Y N4 178.48(7) . . ? N3 Y Cl 120.04(5) . . ? N2 Y Cl 114.29(5) . . ? N1 Y Cl 89.11(5) . . ? N4 Y Cl 89.81(5) . . ? N1 Si1 C18 112.02(12) . . ? N1 Si1 C17 106.55(11) . . ? C18 Si1 C17 109.17(14) . . ? N1 Si1 C16 113.47(12) . . ? C18 Si1 C16 109.25(15) . . ? C17 Si1 C16 106.11(14) . . ? N2 Si2 C19 105.50(12) . . ? N2 Si2 C21 116.76(12) . . ? C19 Si2 C21 107.82(15) . . ? N2 Si2 C20 107.03(12) . . ? C19 Si2 C20 110.66(16) . . ? C21 Si2 C20 109.00(14) . . ? N3 Si3 C39 104.96(12) . . ? N3 Si3 C38 106.65(12) . . ? C39 Si3 C38 111.28(15) . . ? N3 Si3 C37 118.48(12) . . ? C39 Si3 C37 108.08(14) . . ? C38 Si3 C37 107.39(14) . . ? N4 Si4 C40 105.02(12) . . ? N4 Si4 C42 110.84(12) . . ? C40 Si4 C42 109.94(14) . . ? N4 Si4 C41 114.25(12) . . ? C40 Si4 C41 106.62(14) . . ? C42 Si4 C41 109.92(14) . . ? C1 N1 Si1 127.23(17) . . ? C1 N1 Y 97.55(14) . . ? Si1 N1 Y 135.08(11) . . ? C3 N2 Si2 125.59(16) . . ? C3 N2 Y 100.93(14) . . ? Si2 N2 Y 133.10(10) . . ? C22 N3 Si3 127.08(16) . . ? C22 N3 Y 99.60(14) . . ? Si3 N3 Y 133.12(11) . . ? C24 N4 Si4 127.20(17) . . ? C24 N4 Y 98.58(14) . . ? Si4 N4 Y 134.16(10) . . ? N1 C1 C2 124.2(2) . . ? N1 C1 C4 120.6(2) . . ? C2 C1 C4 115.2(2) . . ? C3 C2 C1 127.7(2) . . ? N2 C3 C2 123.3(2) . . ? N2 C3 C10 121.7(2) . . ? C2 C3 C10 115.0(2) . . ? C9 C4 C5 118.7(2) . . ? C9 C4 C1 120.0(2) . . ? C5 C4 C1 121.3(2) . . ? C6 C5 C4 120.3(3) . . ? C7 C6 C5 120.3(3) . . ? C6 C7 C8 120.0(3) . . ? C7 C8 C9 120.3(3) . . ? C8 C9 C4 120.4(3) . . ? C15 C10 C11 118.6(2) . . ? C15 C10 C3 120.9(2) . . ? C11 C10 C3 120.5(2) . . ? C12 C11 C10 120.9(3) . . ? C13 C12 C11 119.6(3) . . ? C14 C13 C12 120.3(3) . . ? C13 C14 C15 120.3(3) . . ? C10 C15 C14 120.2(3) . . ? N3 C22 C23 123.6(2) . . ? N3 C22 C25 120.8(2) . . ? C23 C22 C25 115.5(2) . . ? C22 C23 C24 128.0(2) . . ? N4 C24 C23 123.8(2) . . ? N4 C24 C31 120.2(2) . . ? C23 C24 C31 115.9(2) . . ? C26 C25 C30 118.6(2) . . ? C26 C25 C22 120.3(2) . . ? C30 C25 C22 121.1(2) . . ? C27 C26 C25 120.6(2) . . ? C28 C27 C26 120.3(3) . . ? C27 C28 C29 119.7(3) . . ? C28 C29 C30 120.3(3) . . ? C29 C30 C25 120.3(3) . . ? C32 C31 C36 118.7(2) . . ? C32 C31 C24 121.5(2) . . ? C36 C31 C24 119.8(2) . . ? C33 C32 C31 120.6(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C35 120.5(3) . . ? C34 C35 C36 119.6(3) . . ? C35 C36 C31 120.8(3) . . ? #===END data_(7)-may2703 _database_code_depnum_ccdc_archive 'CCDC 684949' _audit_creation_date 2003-05-22T16:16:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (Y(OtBu)(C6H4iPrNC(Me)CHC(Me)MC6H4iPr)2) _chemical_formula_moiety 'C50 H67 N4 O1 Y' _chemical_formula_sum 'C50 H67 N4 O1 Y' _chemical_formula_weight 828.99 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5959(1) _cell_length_b 17.9182(2) _cell_length_c 21.0703(2) _cell_angle_alpha 90 _cell_angle_beta 98.21 _cell_angle_gamma 90 _cell_volume 4706.78(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34782 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.17 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7141 _exptl_absorpt_correction_T_max 0.8374 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.689059E-1 _diffrn_orient_matrix_ub_12 0.108268E-1 _diffrn_orient_matrix_ub_13 -0.166025E-1 _diffrn_orient_matrix_ub_21 0.358801E-1 _diffrn_orient_matrix_ub_22 -0.40989E-1 _diffrn_orient_matrix_ub_23 0.27285E-1 _diffrn_orient_matrix_ub_31 -0.199658E-1 _diffrn_orient_matrix_ub_32 -0.362953E-1 _diffrn_orient_matrix_ub_33 -0.35766E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_unetI/netI 0.0452 _diffrn_reflns_number 60670 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 10723 _reflns_number_gt 8417 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The methyls of the tBu group have an alternative low occupancy orientation which was refined with isotropic C atoms. 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^)+(0.0233P)^2^+4.1158P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 10723 _refine_ls_number_parameters 522 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.349 _refine_diff_density_min -0.39 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.981203(16) 0.337703(11) 0.239548(9) 0.02014(6) Uani 1 1 d . . . O O 1.02001(13) 0.44278(8) 0.21775(8) 0.0345(4) Uani 1 1 d . A . N1 N 0.81476(14) 0.33205(10) 0.16883(8) 0.0264(4) Uani 1 1 d . . . N2 N 0.85729(14) 0.31197(9) 0.30993(8) 0.0217(4) Uani 1 1 d . . . N3 N 1.04495(14) 0.22409(10) 0.20301(8) 0.0260(4) Uani 1 1 d . . . N4 N 1.13534(14) 0.31481(10) 0.31642(8) 0.0227(4) Uani 1 1 d . . . C1 C 0.74312(18) 0.27958(12) 0.17538(10) 0.0284(5) Uani 1 1 d . . . C2 C 0.73464(18) 0.24272(12) 0.23340(10) 0.0290(5) Uani 1 1 d . . . H2 H 0.6925 0.1985 0.2295 0.035 Uiso 1 1 calc R . . C3 C 0.77935(17) 0.26169(11) 0.29625(10) 0.0247(5) Uani 1 1 d . . . C4 C 0.6623(2) 0.25606(14) 0.11842(12) 0.0404(6) Uani 1 1 d . . . H4A H 0.6053 0.2935 0.1108 0.061 Uiso 1 1 calc R . . H4B H 0.6313 0.2077 0.1274 0.061 Uiso 1 1 calc R . . H4C H 0.6983 0.2518 0.0803 0.061 Uiso 1 1 calc R . . C5 C 0.73012(19) 0.22411(13) 0.34944(11) 0.0334(5) Uani 1 1 d . . . H5A H 0.7843 0.1931 0.3751 0.05 Uiso 1 1 calc R . . H5B H 0.67 0.1927 0.3308 0.05 Uiso 1 1 calc R . . H5C H 0.7043 0.2622 0.3769 0.05 Uiso 1 1 calc R . . C6 C 0.80435(19) 0.37458(13) 0.11013(10) 0.0313(5) Uani 1 1 d . . . C7 C 0.7261(2) 0.42974(14) 0.09549(12) 0.0374(6) Uani 1 1 d . . . C8 C 0.7277(2) 0.47047(16) 0.03897(13) 0.0514(7) Uani 1 1 d . . . H8 H 0.6754 0.5083 0.0282 0.062 Uiso 1 1 calc R . . C9 C 0.8023(3) 0.45777(17) -0.00161(13) 0.0565(8) Uani 1 1 d . . . H9 H 0.8006 0.4862 -0.0398 0.068 Uiso 1 1 calc R . . C10 C 0.8789(3) 0.40389(17) 0.01344(13) 0.0520(7) Uani 1 1 d . . . H10 H 0.9311 0.395 -0.0141 0.062 Uiso 1 1 calc R . . C11 C 0.8799(2) 0.36242(14) 0.06897(11) 0.0391(6) Uani 1 1 d . . . H11 H 0.933 0.325 0.0792 0.047 Uiso 1 1 calc R . . C12 C 0.6441(2) 0.44910(15) 0.13938(14) 0.0448(7) Uani 1 1 d . . . H12 H 0.646 0.4088 0.1724 0.054 Uiso 1 1 calc R . . C13 C 0.6745(3) 0.52211(18) 0.17409(18) 0.0691(10) Uani 1 1 d . . . H13A H 0.6214 0.5341 0.2023 0.104 Uiso 1 1 calc R . . H13B H 0.6762 0.5622 0.1426 0.104 Uiso 1 1 calc R . . H13C H 0.7454 0.5171 0.1997 0.104 Uiso 1 1 calc R . . C14 C 0.5295(2) 0.4535(2) 0.10337(18) 0.0758(11) Uani 1 1 d . . . H14A H 0.4798 0.4658 0.1336 0.114 Uiso 1 1 calc R . . H14B H 0.5096 0.4052 0.0832 0.114 Uiso 1 1 calc R . . H14C H 0.5258 0.4922 0.0703 0.114 Uiso 1 1 calc R . . C15 C 0.88736(16) 0.33478(13) 0.37518(9) 0.0248(4) Uani 1 1 d . . . C16 C 0.86482(17) 0.40782(13) 0.39335(11) 0.0295(5) Uani 1 1 d . . . C17 C 0.9008(2) 0.42943(16) 0.45629(12) 0.0419(6) Uani 1 1 d . . . H17 H 0.8876 0.4789 0.4692 0.05 Uiso 1 1 calc R . . C18 C 0.9548(2) 0.38133(19) 0.50006(12) 0.0509(8) Uani 1 1 d . . . H18 H 0.9776 0.3975 0.5428 0.061 Uiso 1 1 calc R . . C19 C 0.9761(2) 0.30953(18) 0.48212(12) 0.0472(7) Uani 1 1 d . . . H19 H 1.0129 0.2759 0.5125 0.057 Uiso 1 1 calc R . . C20 C 0.94359(18) 0.28643(15) 0.41936(11) 0.0338(5) Uani 1 1 d . . . H20 H 0.9599 0.2374 0.4066 0.041 Uiso 1 1 calc R . . C21 C 0.79874(19) 0.45979(13) 0.34660(13) 0.0361(6) Uani 1 1 d . . . H21 H 0.8188 0.4501 0.3031 0.043 Uiso 1 1 calc R . . C22 C 0.6802(2) 0.44142(18) 0.3438(2) 0.0694(10) Uani 1 1 d . . . H22A H 0.6377 0.475 0.3134 0.104 Uiso 1 1 calc R . . H22B H 0.659 0.4478 0.3864 0.104 Uiso 1 1 calc R . . H22C H 0.6675 0.3896 0.3297 0.104 Uiso 1 1 calc R . . C23 C 0.8177(3) 0.54258(15) 0.36120(16) 0.0588(8) Uani 1 1 d . . . H23A H 0.7725 0.5725 0.329 0.088 Uiso 1 1 calc R . . H23B H 0.8933 0.5546 0.3601 0.088 Uiso 1 1 calc R . . H23C H 0.7995 0.5538 0.4039 0.088 Uiso 1 1 calc R . . C24 C 1.06715(17) 0.17034(12) 0.24675(11) 0.0260(5) Uani 1 1 d . . . C25 C 1.10047(18) 0.18293(12) 0.31238(11) 0.0280(5) Uani 1 1 d . . . H25 H 1.0919 0.1419 0.3397 0.034 Uiso 1 1 calc R . . C26 C 1.14464(16) 0.24765(12) 0.34323(10) 0.0247(5) Uani 1 1 d . . . C27 C 1.0634(2) 0.08932(13) 0.22649(12) 0.0384(6) Uani 1 1 d . . . H27A H 0.9903 0.0765 0.2071 0.058 Uiso 1 1 calc R . . H27B H 1.0847 0.0577 0.2641 0.058 Uiso 1 1 calc R . . H27C H 1.1128 0.0813 0.1952 0.058 Uiso 1 1 calc R . . C28 C 1.20627(19) 0.23690(14) 0.40996(11) 0.0356(6) Uani 1 1 d . . . H28A H 1.2835 0.2383 0.4078 0.053 Uiso 1 1 calc R . . H28B H 1.1874 0.1885 0.427 0.053 Uiso 1 1 calc R . . H28C H 1.1877 0.2769 0.4381 0.053 Uiso 1 1 calc R . . C29 C 1.02378(19) 0.20306(12) 0.13667(11) 0.0302(5) Uani 1 1 d . . . C30 C 1.0970(2) 0.22059(13) 0.09473(11) 0.0350(6) Uani 1 1 d . . . C31 C 1.0695(3) 0.20074(16) 0.03044(13) 0.0506(7) Uani 1 1 d . . . H31 H 1.1183 0.2116 0.0012 0.061 Uiso 1 1 calc R . . C32 C 0.9742(3) 0.16605(17) 0.00788(13) 0.0585(8) Uani 1 1 d . . . H32 H 0.9583 0.153 -0.0362 0.07 Uiso 1 1 calc R . . C33 C 0.9022(3) 0.15027(15) 0.04906(13) 0.0504(7) Uani 1 1 d . . . H33 H 0.8361 0.1265 0.0336 0.06 Uiso 1 1 calc R . . C34 C 0.9264(2) 0.16914(13) 0.11328(12) 0.0384(6) Uani 1 1 d . . . H34 H 0.876 0.1589 0.1417 0.046 Uiso 1 1 calc R . . C35 C 1.2034(2) 0.25801(14) 0.11816(12) 0.0380(6) Uani 1 1 d . . . H35 H 1.1964 0.2834 0.1596 0.046 Uiso 1 1 calc R . . C36 C 1.2339(4) 0.3169(2) 0.07228(19) 0.1060(17) Uani 1 1 d . . . H36A H 1.3028 0.3392 0.0899 0.159 Uiso 1 1 calc R . . H36B H 1.1786 0.3557 0.0665 0.159 Uiso 1 1 calc R . . H36C H 1.2398 0.2938 0.0308 0.159 Uiso 1 1 calc R . . C37 C 1.2913(3) 0.2001(2) 0.1317(3) 0.1024(16) Uani 1 1 d . . . H37A H 1.3596 0.2249 0.1468 0.154 Uiso 1 1 calc R . . H37B H 1.2975 0.1723 0.0923 0.154 Uiso 1 1 calc R . . H37C H 1.2737 0.1655 0.1647 0.154 Uiso 1 1 calc R . . C38 C 1.20461(17) 0.37281(12) 0.34572(10) 0.0232(4) Uani 1 1 d . . . C39 C 1.31072(17) 0.37887(11) 0.33319(10) 0.0243(4) Uani 1 1 d . . . C40 C 1.37334(18) 0.43664(12) 0.36263(10) 0.0278(5) Uani 1 1 d . . . H40 H 1.4457 0.4409 0.3552 0.033 Uiso 1 1 calc R . . C41 C 1.33382(19) 0.48794(13) 0.40228(11) 0.0317(5) Uani 1 1 d . . . H41 H 1.3785 0.5266 0.422 0.038 Uiso 1 1 calc R . . C42 C 1.2285(2) 0.48221(13) 0.41280(11) 0.0352(6) Uani 1 1 d . . . H42 H 1.1998 0.5176 0.4393 0.042 Uiso 1 1 calc R . . C43 C 1.16472(19) 0.42501(13) 0.38479(11) 0.0308(5) Uani 1 1 d . . . H43 H 1.0924 0.4214 0.3924 0.037 Uiso 1 1 calc R . . C44 C 1.35792(18) 0.32555(13) 0.28832(12) 0.0343(5) Uani 1 1 d . . . H44 H 1.2991 0.2922 0.268 0.041 Uiso 1 1 calc R . . C45 C 1.4026(2) 0.36778(16) 0.23517(13) 0.0479(7) Uani 1 1 d . . . H45A H 1.4322 0.3322 0.207 0.072 Uiso 1 1 calc R . . H45B H 1.4594 0.4018 0.2541 0.072 Uiso 1 1 calc R . . H45C H 1.345 0.3965 0.2102 0.072 Uiso 1 1 calc R . . C46 C 1.4460(2) 0.27662(16) 0.32433(16) 0.0558(8) Uani 1 1 d . . . H46A H 1.4742 0.2431 0.294 0.084 Uiso 1 1 calc R . . H46B H 1.4162 0.247 0.3567 0.084 Uiso 1 1 calc R . . H46C H 1.504 0.3083 0.3453 0.084 Uiso 1 1 calc R . . C47 C 1.0524(2) 0.51533(13) 0.20326(12) 0.0365(6) Uani 1 1 d . . . C48 C 0.9936(3) 0.54030(19) 0.13840(18) 0.0401(9) Uani 0.808(6) 1 d P A 1 H48A H 0.916 0.5368 0.1386 0.06 Uiso 0.808(6) 1 calc PR A 1 H48B H 1.0141 0.5081 0.1046 0.06 Uiso 0.808(6) 1 calc PR A 1 H48C H 1.0128 0.5921 0.1303 0.06 Uiso 0.808(6) 1 calc PR A 1 C49 C 1.0156(4) 0.56733(19) 0.25555(17) 0.0550(12) Uani 0.808(6) 1 d P A 1 H49A H 0.9375 0.5644 0.2535 0.082 Uiso 0.808(6) 1 calc PR A 1 H49B H 1.0364 0.6189 0.2479 0.082 Uiso 0.808(6) 1 calc PR A 1 H49C H 1.0499 0.5513 0.2981 0.082 Uiso 0.808(6) 1 calc PR A 1 C50 C 1.1699(3) 0.5192(2) 0.2059(2) 0.0638(14) Uani 0.808(6) 1 d P A 1 H50A H 1.2045 0.5026 0.2481 0.096 Uiso 0.808(6) 1 calc PR A 1 H50B H 1.1912 0.5707 0.1985 0.096 Uiso 0.808(6) 1 calc PR A 1 H50C H 1.1922 0.4868 0.1727 0.096 Uiso 0.808(6) 1 calc PR A 1 C48A C 0.9708(15) 0.5547(11) 0.1666(10) 0.058(5) Uiso 0.192(6) 1 d P A 2 H48D H 0.9351 0.5224 0.1325 0.087 Uiso 0.192(6) 1 calc PR A 2 H48E H 1.0011 0.5983 0.1474 0.087 Uiso 0.192(6) 1 calc PR A 2 H48F H 0.9186 0.5714 0.1939 0.087 Uiso 0.192(6) 1 calc PR A 2 C49A C 1.1155(13) 0.5561(8) 0.2582(7) 0.049(4) Uiso 0.192(6) 1 d P A 2 H49D H 1.1708 0.5229 0.2802 0.074 Uiso 0.192(6) 1 calc PR A 2 H49E H 1.0674 0.5721 0.2883 0.074 Uiso 0.192(6) 1 calc PR A 2 H49F H 1.1497 0.5999 0.242 0.074 Uiso 0.192(6) 1 calc PR A 2 C50A C 1.1461(16) 0.4930(11) 0.1571(11) 0.072(6) Uiso 0.192(6) 1 d P A 2 H50D H 1.2067 0.4686 0.1835 0.108 Uiso 0.192(6) 1 calc PR A 2 H50E H 1.1712 0.5385 0.1381 0.108 Uiso 0.192(6) 1 calc PR A 2 H50F H 1.1152 0.459 0.123 0.108 Uiso 0.192(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.02114(10) 0.01897(10) 0.01987(9) -0.00022(8) 0.00142(7) -0.00098(9) O 0.0384(10) 0.0236(8) 0.0390(9) 0.0080(7) -0.0024(8) -0.0073(7) N1 0.0290(10) 0.0256(10) 0.0232(9) 0.0021(8) -0.0017(7) -0.0022(8) N2 0.0213(9) 0.0234(9) 0.0194(8) -0.0005(7) -0.0007(7) 0.0003(7) N3 0.0276(10) 0.0242(9) 0.0264(9) -0.0041(7) 0.0041(8) -0.0021(8) N4 0.0191(9) 0.0236(9) 0.0251(9) -0.0010(7) 0.0018(7) -0.0007(7) C1 0.0292(12) 0.0250(11) 0.0283(12) -0.0021(9) -0.0054(9) -0.0008(9) C2 0.0288(12) 0.0234(11) 0.0327(12) 0.0015(9) -0.0026(10) -0.0060(9) C3 0.0249(11) 0.0205(11) 0.0283(11) 0.0024(9) 0.0024(9) 0.0025(9) C4 0.0432(15) 0.0393(14) 0.0333(13) -0.0003(11) -0.0125(11) -0.0123(12) C5 0.0331(13) 0.0308(13) 0.0369(13) 0.0065(10) 0.0068(11) -0.0053(10) C6 0.0385(14) 0.0301(12) 0.0225(11) 0.0035(9) -0.0047(10) -0.0071(10) C7 0.0374(14) 0.0375(14) 0.0341(13) 0.0098(11) -0.0062(11) -0.0033(11) C8 0.0567(19) 0.0494(17) 0.0440(16) 0.0205(13) -0.0064(14) 0.0008(14) C9 0.076(2) 0.0592(19) 0.0325(14) 0.0190(13) 0.0013(15) -0.0084(17) C10 0.070(2) 0.0562(18) 0.0317(14) 0.0069(13) 0.0119(14) -0.0038(16) C11 0.0483(16) 0.0400(14) 0.0283(12) 0.0022(10) 0.0035(11) 0.0000(12) C12 0.0373(15) 0.0450(16) 0.0510(16) 0.0180(13) 0.0025(12) 0.0062(12) C13 0.073(2) 0.052(2) 0.087(3) -0.0012(18) 0.031(2) 0.0040(17) C14 0.0375(18) 0.098(3) 0.089(3) 0.036(2) -0.0018(17) 0.0056(18) C15 0.0170(10) 0.0373(12) 0.0203(10) 0.0002(9) 0.0031(8) -0.0018(9) C16 0.0214(12) 0.0378(13) 0.0305(12) -0.0085(10) 0.0077(9) -0.0046(10) C17 0.0378(15) 0.0572(17) 0.0331(13) -0.0161(12) 0.0135(12) -0.0102(12) C18 0.0474(17) 0.081(2) 0.0236(13) -0.0125(14) 0.0038(12) -0.0159(16) C19 0.0343(15) 0.079(2) 0.0259(13) 0.0133(13) -0.0030(11) -0.0025(14) C20 0.0273(13) 0.0467(15) 0.0273(12) 0.0054(10) 0.0038(10) 0.0025(11) C21 0.0319(14) 0.0270(12) 0.0493(15) -0.0068(11) 0.0057(11) 0.0010(10) C22 0.0294(16) 0.056(2) 0.121(3) 0.017(2) 0.0034(17) 0.0070(14) C23 0.071(2) 0.0330(15) 0.072(2) -0.0112(14) 0.0098(17) -0.0034(14) C24 0.0215(11) 0.0227(11) 0.0348(12) -0.0013(9) 0.0079(9) -0.0022(9) C25 0.0269(12) 0.0258(11) 0.0317(12) 0.0042(9) 0.0057(10) -0.0007(9) C26 0.0168(10) 0.0291(12) 0.0283(11) 0.0037(9) 0.0037(9) 0.0000(9) C27 0.0461(16) 0.0233(12) 0.0455(15) -0.0020(10) 0.0056(12) -0.0016(11) C28 0.0319(13) 0.0391(14) 0.0327(13) 0.0090(10) -0.0064(10) -0.0010(11) C29 0.0393(14) 0.0216(11) 0.0294(12) -0.0067(9) 0.0034(10) -0.0009(10) C30 0.0468(15) 0.0293(12) 0.0294(12) -0.0056(10) 0.0071(11) -0.0001(11) C31 0.074(2) 0.0477(17) 0.0325(14) -0.0089(12) 0.0161(14) -0.0102(15) C32 0.091(2) 0.0522(18) 0.0303(14) -0.0123(13) 0.0007(15) -0.0153(17) C33 0.0616(19) 0.0436(17) 0.0410(15) -0.0108(12) -0.0097(14) -0.0123(14) C34 0.0449(15) 0.0317(13) 0.0373(13) -0.0055(11) 0.0015(11) -0.0041(11) C35 0.0439(15) 0.0384(14) 0.0345(13) -0.0074(11) 0.0148(11) -0.0065(11) C36 0.133(4) 0.109(3) 0.069(2) 0.022(2) -0.008(2) -0.080(3) C37 0.046(2) 0.064(2) 0.195(5) -0.037(3) 0.007(3) 0.0020(18) C38 0.0239(11) 0.0226(11) 0.0222(10) 0.0028(8) 0.0001(9) -0.0005(9) C39 0.0220(11) 0.0230(11) 0.0269(11) 0.0018(9) -0.0001(9) 0.0022(9) C40 0.0245(12) 0.0297(12) 0.0283(11) 0.0013(9) 0.0009(9) -0.0019(9) C41 0.0391(14) 0.0270(12) 0.0277(12) -0.0016(9) 0.0004(10) -0.0088(10) C42 0.0429(15) 0.0322(13) 0.0327(13) -0.0060(10) 0.0135(11) -0.0016(11) C43 0.0281(13) 0.0336(13) 0.0317(12) -0.0036(10) 0.0076(10) -0.0021(10) C44 0.0238(12) 0.0330(13) 0.0469(14) -0.0119(11) 0.0079(10) -0.0033(10) C45 0.0505(17) 0.0513(17) 0.0455(16) -0.0095(13) 0.0193(13) 0.0034(13) C46 0.0509(18) 0.0419(16) 0.078(2) 0.0016(15) 0.0198(16) 0.0184(14) C47 0.0406(15) 0.0267(12) 0.0405(14) 0.0106(10) -0.0003(11) -0.0088(11) C48 0.046(2) 0.0341(18) 0.038(2) 0.0116(15) 0.0014(16) -0.0065(15) C49 0.085(3) 0.0313(18) 0.046(2) -0.0005(15) 0.0023(19) -0.0004(18) C50 0.040(2) 0.061(3) 0.088(3) 0.034(2) -0.001(2) -0.0105(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y O 2.0147(15) . ? Y N2 2.3471(17) . ? Y N3 2.3576(17) . ? Y N4 2.3798(17) . ? Y N1 2.3946(18) . ? O C47 1.409(3) . ? N1 C1 1.324(3) . ? N1 C6 1.443(3) . ? N2 C3 1.333(3) . ? N2 C15 1.432(3) . ? N3 C24 1.335(3) . ? N3 C29 1.436(3) . ? N4 C26 1.327(3) . ? N4 C38 1.438(3) . ? C1 C2 1.407(3) . ? C1 C4 1.518(3) . ? C2 C3 1.405(3) . ? C3 C5 1.514(3) . ? C6 C11 1.393(3) . ? C6 C7 1.399(3) . ? C7 C8 1.399(3) . ? C7 C12 1.521(4) . ? C8 C9 1.376(4) . ? C9 C10 1.370(4) . ? C10 C11 1.385(3) . ? C12 C13 1.521(4) . ? C12 C14 1.534(4) . ? C15 C20 1.389(3) . ? C15 C16 1.404(3) . ? C16 C17 1.394(3) . ? C16 C21 1.515(3) . ? C17 C18 1.370(4) . ? C18 C19 1.378(4) . ? C19 C20 1.390(3) . ? C21 C22 1.522(4) . ? C21 C23 1.527(3) . ? C24 C25 1.405(3) . ? C24 C27 1.512(3) . ? C25 C26 1.405(3) . ? C26 C28 1.518(3) . ? C29 C34 1.395(3) . ? C29 C30 1.401(3) . ? C30 C31 1.395(3) . ? C30 C35 1.517(3) . ? C31 C32 1.375(4) . ? C32 C33 1.371(4) . ? C33 C34 1.386(3) . ? C35 C37 1.515(4) . ? C35 C36 1.517(4) . ? C38 C43 1.387(3) . ? C38 C39 1.403(3) . ? C39 C40 1.392(3) . ? C39 C44 1.523(3) . ? C40 C41 1.382(3) . ? C41 C42 1.380(3) . ? C42 C43 1.381(3) . ? C44 C45 1.524(4) . ? C44 C46 1.528(4) . ? C47 C48A 1.387(19) . ? C47 C50 1.475(4) . ? C47 C49A 1.498(15) . ? C47 C48 1.526(4) . ? C47 C49 1.563(4) . ? C47 C50A 1.681(19) . ? 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 O Y N2 122.18(6) . . ? O Y N3 128.87(7) . . ? N2 Y N3 108.96(6) . . ? O Y N4 96.62(6) . . ? N2 Y N4 95.03(6) . . ? N3 Y N4 77.91(6) . . ? O Y N1 96.72(6) . . ? N2 Y N1 77.45(6) . . ? N3 Y N1 93.96(6) . . ? N4 Y N1 166.65(6) . . ? C47 O Y 177.25(16) . . ? C1 N1 C6 118.99(18) . . ? C1 N1 Y 120.95(14) . . ? C6 N1 Y 118.39(13) . . ? C3 N2 C15 119.08(17) . . ? C3 N2 Y 122.12(13) . . ? C15 N2 Y 116.21(12) . . ? C24 N3 C29 118.31(18) . . ? C24 N3 Y 116.44(13) . . ? C29 N3 Y 121.34(14) . . ? C26 N4 C38 117.46(17) . . ? C26 N4 Y 117.37(13) . . ? C38 N4 Y 123.61(13) . . ? N1 C1 C2 124.1(2) . . ? N1 C1 C4 120.3(2) . . ? C2 C1 C4 115.5(2) . . ? C3 C2 C1 129.5(2) . . ? N2 C3 C2 123.44(19) . . ? N2 C3 C5 120.48(19) . . ? C2 C3 C5 116.02(19) . . ? C11 C6 C7 119.7(2) . . ? C11 C6 N1 117.7(2) . . ? C7 C6 N1 122.5(2) . . ? C6 C7 C8 117.5(2) . . ? C6 C7 C12 123.0(2) . . ? C8 C7 C12 119.5(2) . . ? C9 C8 C7 122.4(3) . . ? C10 C9 C8 119.6(3) . . ? C9 C10 C11 119.6(3) . . ? C10 C11 C6 121.2(3) . . ? C13 C12 C7 110.0(2) . . ? C13 C12 C14 110.4(3) . . ? C7 C12 C14 112.6(3) . . ? C20 C15 C16 120.1(2) . . ? C20 C15 N2 120.3(2) . . ? C16 C15 N2 119.45(19) . . ? C17 C16 C15 117.9(2) . . ? C17 C16 C21 121.5(2) . . ? C15 C16 C21 120.6(2) . . ? C18 C17 C16 121.9(3) . . ? C17 C18 C19 120.0(2) . . ? C18 C19 C20 119.8(3) . . ? C15 C20 C19 120.3(2) . . ? C16 C21 C22 109.7(2) . . ? C16 C21 C23 114.2(2) . . ? C22 C21 C23 110.0(2) . . ? N3 C24 C25 124.57(19) . . ? N3 C24 C27 120.2(2) . . ? C25 C24 C27 115.1(2) . . ? C26 C25 C24 129.1(2) . . ? N4 C26 C25 123.1(2) . . ? N4 C26 C28 120.77(19) . . ? C25 C26 C28 116.11(19) . . ? C34 C29 C30 120.0(2) . . ? C34 C29 N3 119.4(2) . . ? C30 C29 N3 120.5(2) . . ? C31 C30 C29 117.4(2) . . ? C31 C30 C35 120.9(2) . . ? C29 C30 C35 121.6(2) . . ? C32 C31 C30 122.3(3) . . ? C33 C32 C31 119.9(3) . . ? C32 C33 C34 119.6(3) . . ? C33 C34 C29 120.7(2) . . ? C30 C35 C37 110.3(2) . . ? C30 C35 C36 113.1(2) . . ? C37 C35 C36 110.6(3) . . ? C43 C38 C39 119.7(2) . . ? C43 C38 N4 119.55(19) . . ? C39 C38 N4 120.73(18) . . ? C40 C39 C38 117.91(19) . . ? C40 C39 C44 119.8(2) . . ? C38 C39 C44 122.33(19) . . ? C41 C40 C39 122.3(2) . . ? C42 C41 C40 119.0(2) . . ? C43 C42 C41 120.0(2) . . ? C42 C43 C38 121.1(2) . . ? C45 C44 C39 111.2(2) . . ? C45 C44 C46 109.4(2) . . ? C39 C44 C46 111.8(2) . . ? C48A C47 O 112.1(8) . . ? O C47 C50 110.8(2) . . ? C48A C47 C49A 116.8(10) . . ? O C47 C49A 114.9(6) . . ? O C47 C48 110.3(2) . . ? C50 C47 C48 112.1(3) . . ? O C47 C49 105.9(2) . . ? C50 C47 C49 110.0(3) . . ? C48 C47 C49 107.6(3) . . ? C48A C47 C50A 108.9(11) . . ? O C47 C50A 98.9(7) . . ? C49A C47 C50A 102.9(10) . . ? #===END data_(8)-jul1303 _database_code_depnum_ccdc_archive 'CCDC 684950' _audit_creation_date 2003-07-11T15:43:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C38 H94 Cl6 Li2 O6 Si4 Y2' _chemical_formula_sum 'C38 H94 Cl6 Li2 O6 Si4 Y2' _chemical_formula_weight 1163.89 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.8150(3) _cell_length_b 20.0248(3) _cell_length_c 10.6476(2) _cell_angle_alpha 90 _cell_angle_beta 99.532(1) _cell_angle_gamma 90 _cell_volume 3115.18(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18182 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5051 _exptl_absorpt_correction_T_max 0.6448 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.697149E-1 _diffrn_orient_matrix_ub_12 0.339942E-1 _diffrn_orient_matrix_ub_13 0.101047E-1 _diffrn_orient_matrix_ub_21 0.12912E-1 _diffrn_orient_matrix_ub_22 -0.53466E-2 _diffrn_orient_matrix_ub_23 -0.649475E-1 _diffrn_orient_matrix_ub_31 -0.635799E-1 _diffrn_orient_matrix_ub_32 0.361886E-1 _diffrn_orient_matrix_ub_33 -0.190875E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_unetI/netI 0.042 _diffrn_reflns_number 32120 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 5466 _reflns_number_gt 4454 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0557P)^2^+11.0376P] 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_number_reflns 5466 _refine_ls_number_parameters 227 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.011 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' 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 Y Y 0.35594(3) 0.51109(2) 0.43892(4) 0.02545(15) Uani 1 1 d . . . Li Li 0.2446(7) 0.3829(5) 0.2338(9) 0.049(2) Uani 1 1 d . A . Cl1 Cl 0.50725(8) 0.58514(6) 0.48845(11) 0.0322(3) Uani 1 1 d . . . Cl2 Cl 0.35166(9) 0.47093(7) 0.20412(11) 0.0378(3) Uani 1 1 d . . . Cl3 Cl 0.24232(9) 0.41126(7) 0.44916(12) 0.0398(3) Uani 1 1 d . . . Si1 Si 0.27538(11) 0.66190(7) 0.25889(15) 0.0393(4) Uani 1 1 d . . . Si2 Si 0.14299(10) 0.60104(8) 0.42929(17) 0.0432(4) Uani 1 1 d . . . O1 O 0.3619(3) 0.51577(18) 0.6597(3) 0.0367(8) Uani 1 1 d . . . O2 O 0.3036(3) 0.3000(2) 0.1972(5) 0.0714(14) Uani 1 1 d D . . O3 O 0.1281(4) 0.3835(3) 0.1205(5) 0.0853(17) Uani 1 1 d D . . C1 C 0.2617(3) 0.6095(2) 0.3986(5) 0.0328(11) Uani 1 1 d . . . H1 H 0.2892 0.639 0.4707 0.039 Uiso 1 1 calc R . . C2 C 0.2618(5) 0.7535(3) 0.2878(8) 0.070(2) Uani 1 1 d . . . H2C H 0.2007 0.7619 0.3083 0.104 Uiso 1 1 calc R . . H2B H 0.2693 0.7785 0.2111 0.104 Uiso 1 1 calc R . . H2A H 0.3083 0.7678 0.3591 0.104 Uiso 1 1 calc R . . C3 C 0.1901(5) 0.6399(4) 0.1131(6) 0.070(2) Uani 1 1 d . . . H3C H 0.1981 0.5931 0.0906 0.106 Uiso 1 1 calc R . . H3B H 0.2 0.6687 0.0421 0.106 Uiso 1 1 calc R . . H3A H 0.1279 0.6466 0.1308 0.106 Uiso 1 1 calc R . . C4 C 0.3892(4) 0.6558(3) 0.2055(6) 0.0495(15) Uani 1 1 d . . . H4C H 0.4374 0.67 0.2749 0.074 Uiso 1 1 calc R . . H4B H 0.3897 0.6848 0.1315 0.074 Uiso 1 1 calc R . . H4A H 0.4001 0.6095 0.1823 0.074 Uiso 1 1 calc R . . C5 C 0.0742(5) 0.5427(4) 0.3134(7) 0.069(2) Uani 1 1 d . . . H5C H 0.072 0.5598 0.2266 0.103 Uiso 1 1 calc R . . H5B H 0.0118 0.5395 0.3324 0.103 Uiso 1 1 calc R . . H5A H 0.1027 0.4984 0.3204 0.103 Uiso 1 1 calc R . . C6 C 0.1406(4) 0.5667(4) 0.5932(7) 0.0606(18) Uani 1 1 d . . . H6C H 0.1699 0.5227 0.6012 0.091 Uiso 1 1 calc R . . H6B H 0.077 0.5626 0.6066 0.091 Uiso 1 1 calc R . . H6A H 0.1736 0.597 0.657 0.091 Uiso 1 1 calc R . . C7 C 0.0753(5) 0.6809(4) 0.4224(9) 0.076(2) Uani 1 1 d . . . H7C H 0.1057 0.712 0.4868 0.113 Uiso 1 1 calc R . . H7B H 0.0135 0.6712 0.4392 0.113 Uiso 1 1 calc R . . H7A H 0.0714 0.7009 0.3377 0.113 Uiso 1 1 calc R . . C8 C 0.3848(4) 0.5750(3) 0.7394(5) 0.0492(15) Uani 1 1 d . . . H8B H 0.3438 0.6127 0.7086 0.059 Uiso 1 1 calc R . . H8A H 0.4489 0.5888 0.739 0.059 Uiso 1 1 calc R . . C9 C 0.3718(5) 0.5543(4) 0.8699(6) 0.0634(19) Uani 1 1 d . . . H9B H 0.3075 0.5605 0.8821 0.076 Uiso 1 1 calc R . . H9A H 0.4126 0.5796 0.9361 0.076 Uiso 1 1 calc R . . C10 C 0.3972(5) 0.4812(4) 0.8723(6) 0.0642(19) Uani 1 1 d . . . H10B H 0.4644 0.4751 0.8861 0.077 Uiso 1 1 calc R . . H10A H 0.3717 0.4569 0.9395 0.077 Uiso 1 1 calc R . . C11 C 0.3542(5) 0.4585(3) 0.7426(5) 0.0490(15) Uani 1 1 d . . . H11B H 0.3871 0.4193 0.7155 0.059 Uiso 1 1 calc R . . H11A H 0.2893 0.4463 0.741 0.059 Uiso 1 1 calc R . . C12 C 0.4013(5) 0.2911(5) 0.2210(8) 0.084(2) Uiso 1 1 d D . . H12B H 0.4296 0.3265 0.2796 0.101 Uiso 1 1 calc R . . H12A H 0.4161 0.2474 0.2629 0.101 Uiso 1 1 calc R . . C13 C 0.4389(7) 0.2937(5) 0.1052(9) 0.100(3) Uiso 1 1 d D . . H13C H 0.4126 0.2577 0.0483 0.15 Uiso 1 1 calc R . . H13B H 0.5055 0.2883 0.1248 0.15 Uiso 1 1 calc R . . H13A H 0.4242 0.3369 0.0635 0.15 Uiso 1 1 calc R . . C14 C 0.2608(7) 0.2452(5) 0.1320(10) 0.105(3) Uiso 1 1 d D . . H14B H 0.3053 0.219 0.0925 0.126 Uiso 1 1 calc R . . H14A H 0.2109 0.2601 0.0642 0.126 Uiso 1 1 calc R . . C15 C 0.2244(12) 0.2053(8) 0.2257(15) 0.198(7) Uiso 1 1 d D . . H15C H 0.2748 0.19 0.2909 0.297 Uiso 1 1 calc R . . H15B H 0.1919 0.1666 0.1839 0.297 Uiso 1 1 calc R . . H15A H 0.182 0.2324 0.2658 0.297 Uiso 1 1 calc R . . C16 C 0.0373(8) 0.3650(7) 0.1487(11) 0.139(4) Uiso 1 1 d D A . H16B H -0.0002 0.4059 0.1491 0.167 Uiso 1 1 calc R . . H16A H 0.0064 0.3356 0.08 0.167 Uiso 1 1 calc R . . C17 C 0.0406(9) 0.3340(6) 0.2593(12) 0.134(4) Uiso 1 1 d D . . H17C H 0.0737 0.2917 0.2576 0.2 Uiso 1 1 calc R A . H17B H -0.0217 0.325 0.2744 0.2 Uiso 1 1 calc R . . H17A H 0.0724 0.3623 0.3278 0.2 Uiso 1 1 calc R . . C18 C 0.118(2) 0.3798(14) -0.0149(16) 0.222(19) Uiso 0.52(2) 1 d PD A 1 H18A H 0.1506 0.3406 -0.0418 0.266 Uiso 0.52(2) 1 calc PR A 1 H18B H 0.0524 0.3768 -0.0536 0.266 Uiso 0.52(2) 1 calc PR A 1 C19 C 0.1540(10) 0.4356(8) -0.0473(14) 0.153(5) Uiso 0.52(2) 1 d PD A 1 H19A H 0.1448 0.4391 -0.1403 0.23 Uiso 0.52(2) 1 calc PR A 1 H19B H 0.2197 0.4358 -0.0136 0.23 Uiso 0.52(2) 1 calc PR A 1 H19C H 0.1247 0.4735 -0.0122 0.23 Uiso 0.52(2) 1 calc PR A 1 C18A C 0.0931(15) 0.4334(12) 0.024(2) 0.152(13) Uiso 0.48(2) 1 d PD A 2 H18C H 0.0332 0.4195 -0.0245 0.183 Uiso 0.48(2) 1 calc PR A 2 H18D H 0.0862 0.4774 0.064 0.183 Uiso 0.48(2) 1 calc PR A 2 C19A C 0.1540(10) 0.4356(8) -0.0473(14) 0.153(5) Uiso 0.48(2) 1 d PD A 2 H19D H 0.1386 0.4707 -0.1113 0.23 Uiso 0.48(2) 1 calc PR A 2 H19E H 0.1567 0.3924 -0.09 0.23 Uiso 0.48(2) 1 calc PR A 2 H19F H 0.2137 0.4453 0.0044 0.23 Uiso 0.48(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0284(3) 0.0267(3) 0.0199(2) -0.00007(18) 0.00014(17) 0.00007(19) Li 0.048(6) 0.050(6) 0.045(5) -0.013(5) -0.001(4) 0.000(5) Cl1 0.0314(6) 0.0269(6) 0.0361(6) 0.0003(5) -0.0015(5) 0.0000(5) Cl2 0.0480(8) 0.0420(7) 0.0223(6) -0.0047(5) 0.0029(5) -0.0026(6) Cl3 0.0435(7) 0.0367(7) 0.0385(7) 0.0026(6) 0.0043(6) -0.0095(6) Si1 0.0442(9) 0.0308(8) 0.0398(8) 0.0094(6) -0.0019(7) -0.0033(6) Si2 0.0314(8) 0.0381(9) 0.0593(10) 0.0064(7) 0.0056(7) 0.0026(6) O1 0.052(2) 0.039(2) 0.0193(17) -0.0016(15) 0.0046(15) -0.0014(17) O2 0.077(3) 0.041(3) 0.095(4) -0.028(3) 0.013(3) -0.007(2) O3 0.068(3) 0.101(4) 0.078(4) -0.021(3) -0.016(3) -0.010(3) C1 0.034(3) 0.029(3) 0.034(3) 0.001(2) 0.001(2) -0.001(2) C2 0.072(5) 0.041(4) 0.098(6) 0.016(4) 0.022(4) 0.002(3) C3 0.067(5) 0.085(5) 0.052(4) 0.026(4) -0.012(3) -0.014(4) C4 0.062(4) 0.044(3) 0.043(3) 0.008(3) 0.009(3) -0.006(3) C5 0.043(4) 0.069(5) 0.087(5) 0.008(4) -0.007(4) -0.016(3) C6 0.047(4) 0.070(5) 0.070(4) 0.011(4) 0.025(3) 0.000(3) C7 0.050(4) 0.062(5) 0.118(7) 0.016(5) 0.023(4) 0.017(3) C8 0.059(4) 0.052(4) 0.037(3) -0.017(3) 0.008(3) -0.004(3) C9 0.077(5) 0.085(5) 0.030(3) -0.015(3) 0.014(3) 0.003(4) C10 0.082(5) 0.084(5) 0.027(3) 0.008(3) 0.008(3) 0.000(4) C11 0.067(4) 0.054(4) 0.027(3) 0.010(3) 0.011(3) -0.003(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y O1 2.340(3) . ? Y C1 2.412(5) . ? Y Cl2 2.6169(12) . ? Y Cl3 2.6272(13) . ? Y Cl1 2.6665(13) . ? Y Cl1 2.8107(12) 3_666 ? Li O3 1.936(11) . ? Li O2 1.944(11) . ? Li Cl3 2.368(10) . ? Li Cl2 2.427(11) . ? Cl1 Y 2.8107(12) 3_666 ? Si1 C1 1.859(5) . ? Si1 C4 1.870(6) . ? Si1 C2 1.876(7) . ? Si1 C3 1.884(7) . ? Si2 C1 1.849(5) . ? Si2 C5 1.873(7) . ? Si2 C6 1.881(7) . ? Si2 C7 1.882(7) . ? O1 C11 1.463(7) . ? O1 C8 1.465(6) . ? O2 C14 1.394(9) . ? O2 C12 1.439(8) . ? O3 C18 1.426(15) . ? O3 C18A 1.463(15) . ? O3 C16 1.473(10) . ? C8 C9 1.492(8) . ? C9 C10 1.510(10) . ? C10 C11 1.494(8) . ? C12 C13 1.435(10) . ? C14 C15 1.450(13) . ? C16 C17 1.325(11) . ? C18 C19 1.311(16) . ? 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 Y C1 94.03(15) . . ? O1 Y Cl2 164.39(9) . . ? C1 Y Cl2 99.17(12) . . ? O1 Y Cl3 84.63(9) . . ? C1 Y Cl3 105.86(12) . . ? Cl2 Y Cl3 83.77(4) . . ? O1 Y Cl1 83.61(9) . . ? C1 Y Cl1 91.34(12) . . ? Cl2 Y Cl1 104.27(4) . . ? Cl3 Y Cl1 159.77(4) . . ? O1 Y Cl1 81.13(9) . 3_666 ? C1 Y Cl1 168.17(12) . 3_666 ? Cl2 Y Cl1 87.39(4) . 3_666 ? Cl3 Y Cl1 84.53(4) . 3_666 ? Cl1 Y Cl1 77.44(4) . 3_666 ? O3 Li O2 105.3(5) . . ? O3 Li Cl3 116.6(5) . . ? O2 Li Cl3 118.5(5) . . ? O3 Li Cl2 116.7(5) . . ? O2 Li Cl2 105.6(5) . . ? Cl3 Li Cl2 93.8(3) . . ? Y Cl1 Y 102.56(4) . 3_666 ? Li Cl2 Y 90.7(2) . . ? Li Cl3 Y 91.7(3) . . ? C1 Si1 C4 115.4(2) . . ? C1 Si1 C2 113.0(3) . . ? C4 Si1 C2 103.9(3) . . ? C1 Si1 C3 112.4(3) . . ? C4 Si1 C3 104.5(3) . . ? C2 Si1 C3 106.7(4) . . ? C1 Si2 C5 111.8(3) . . ? C1 Si2 C6 111.2(3) . . ? C5 Si2 C6 107.0(3) . . ? C1 Si2 C7 115.6(3) . . ? C5 Si2 C7 106.0(4) . . ? C6 Si2 C7 104.7(4) . . ? C11 O1 C8 108.6(4) . . ? C11 O1 Y 125.5(3) . . ? C8 O1 Y 125.5(3) . . ? C14 O2 C12 110.5(6) . . ? C14 O2 Li 126.1(6) . . ? C12 O2 Li 122.9(5) . . ? C18 O3 C16 104.2(11) . . ? C18A O3 C16 94.9(9) . . ? C18 O3 Li 124.4(13) . . ? C18A O3 Li 128.1(12) . . ? C16 O3 Li 128.4(7) . . ? Si2 C1 Si1 115.2(3) . . ? Si2 C1 Y 115.6(2) . . ? Si1 C1 Y 117.8(2) . . ? O1 C8 C9 105.1(5) . . ? C8 C9 C10 102.5(5) . . ? C11 C10 C9 102.2(5) . . ? O1 C11 C10 104.8(5) . . ? C13 C12 O2 111.5(7) . . ? O2 C14 C15 106.3(10) . . ? C17 C16 O3 113.5(11) . . ? C19 C18 O3 104.0(16) . . ? #===END #===END data_(9)-nov1403 _database_code_depnum_ccdc_archive 'CCDC 684951' _audit_creation_date 2003-11-17T16:47:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C98 H134 Cl4 K2 N6 O2 Y2, 4(C4 H10 O)' _chemical_formula_sum 'C114 H174 Cl4 K2 N6 O6 Y2' _chemical_formula_weight 2122.41 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 12.9490(1) _cell_length_b 14.4721(2) _cell_length_c 17.0897(2) _cell_angle_alpha 70.257(1) _cell_angle_beta 73.489(1) _cell_angle_gamma 81.903(1) _cell_volume 2886.47(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31166 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7121 _exptl_absorpt_correction_T_max 0.7649 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.18076E-1 _diffrn_orient_matrix_ub_12 -0.723572E-1 _diffrn_orient_matrix_ub_13 0.159619E-1 _diffrn_orient_matrix_ub_21 -0.652745E-1 _diffrn_orient_matrix_ub_22 -0.101019E-1 _diffrn_orient_matrix_ub_23 -0.158043E-1 _diffrn_orient_matrix_ub_31 0.437773E-1 _diffrn_orient_matrix_ub_32 0.8084E-2 _diffrn_orient_matrix_ub_33 -0.602234E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_unetI/netI 0.0428 _diffrn_reflns_number 46919 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.72 _diffrn_reflns_theta_full 25.72 _diffrn_measured_fraction_theta_full 0.961 _diffrn_measured_fraction_theta_max 0.961 _reflns_number_total 10598 _reflns_number_gt 8871 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H on N3 was refined; other H atoms were riding. 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^)+(0.0315P)^2^+4.1679P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10598 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.095 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.532 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y Y 0.45795(2) 0.336622(19) 0.222925(16) 0.02068(8) Uani 1 1 d . . . K K 0.55146(5) 0.58994(5) 0.04644(4) 0.03372(16) Uani 1 1 d . . . Cl1 Cl 0.60294(6) 0.34979(5) 0.07807(4) 0.03178(17) Uani 1 1 d . . . Cl2 Cl 0.33817(5) 0.45659(5) 0.12824(4) 0.02857(16) Uani 1 1 d . . . O1 O 0.58203(16) 0.20605(15) 0.28131(13) 0.0338(5) Uani 1 1 d . . . O2 O 0.0566(4) -0.1498(3) 0.2553(2) 0.1098(14) Uani 1 1 d . . . O3 O -0.0163(4) 0.8031(5) 0.0207(4) 0.170(2) Uani 1 1 d . . . N1 N 0.32620(17) 0.29425(16) 0.35882(14) 0.0223(5) Uani 1 1 d . . . N2 N 0.35924(18) 0.20451(16) 0.21905(14) 0.0222(5) Uani 1 1 d . . . N3 N 0.4969(2) 0.47351(17) 0.24217(16) 0.0264(5) Uani 1 1 d . . . H1X H 0.432(3) 0.490(2) 0.2531(19) 0.028(9) Uiso 1 1 d . . . C1 C 0.2813(2) 0.2087(2) 0.40164(17) 0.0228(6) Uani 1 1 d . . . H1 H 0.2464 0.1996 0.4605 0.027 Uiso 1 1 calc R . . C2 C 0.2777(2) 0.12961(19) 0.37281(17) 0.0225(6) Uani 1 1 d . . . C3 C 0.3061(2) 0.13580(19) 0.28537(17) 0.0229(6) Uani 1 1 d . . . H3 H 0.2842 0.0838 0.2726 0.028 Uiso 1 1 calc R . . C4 C 0.2274(2) 0.0387(2) 0.43594(17) 0.0251(6) Uani 1 1 d . . . C5 C 0.1407(2) 0.0410(2) 0.50635(19) 0.0327(7) Uani 1 1 d . . . H5 H 0.1126 0.1025 0.5141 0.039 Uiso 1 1 calc R . . C6 C 0.0951(3) -0.0443(2) 0.5649(2) 0.0408(8) Uani 1 1 d . . . H6 H 0.0372 -0.0409 0.6127 0.049 Uiso 1 1 calc R . . C7 C 0.1331(3) -0.1344(2) 0.5544(2) 0.0454(9) Uani 1 1 d . . . H7 H 0.1015 -0.1929 0.5947 0.055 Uiso 1 1 calc R . . C8 C 0.2167(3) -0.1387(2) 0.4852(2) 0.0468(9) Uani 1 1 d . . . H8 H 0.2424 -0.2004 0.477 0.056 Uiso 1 1 calc R . . C9 C 0.2642(3) -0.0533(2) 0.42722(19) 0.0359(7) Uani 1 1 d . . . H9 H 0.3232 -0.0578 0.3804 0.043 Uiso 1 1 calc R . . C10 C 0.2925(2) 0.3641(2) 0.40686(17) 0.0233(6) Uani 1 1 d . . . C11 C 0.1962(2) 0.4210(2) 0.40085(18) 0.0279(6) Uani 1 1 d . . . C12 C 0.1618(3) 0.4836(2) 0.4508(2) 0.0361(7) Uani 1 1 d . . . H12 H 0.0971 0.5231 0.4475 0.043 Uiso 1 1 calc R . . C13 C 0.2200(3) 0.4893(2) 0.5051(2) 0.0402(8) Uani 1 1 d . . . H13 H 0.1942 0.531 0.54 0.048 Uiso 1 1 calc R . . C14 C 0.3152(3) 0.4348(2) 0.5089(2) 0.0358(7) Uani 1 1 d . . . H14 H 0.3551 0.4401 0.546 0.043 Uiso 1 1 calc R . . C15 C 0.3550(2) 0.3717(2) 0.45937(18) 0.0277(6) Uani 1 1 d . . . C16 C 0.1293(2) 0.4139(2) 0.3432(2) 0.0350(7) Uani 1 1 d . . . H16 H 0.1777 0.3859 0.2988 0.042 Uiso 1 1 calc R . . C17 C 0.0823(3) 0.5128(3) 0.2963(2) 0.0511(9) Uani 1 1 d . . . H17A H 0.0407 0.5032 0.2601 0.077 Uiso 1 1 calc R . . H17B H 0.1409 0.5564 0.2603 0.077 Uiso 1 1 calc R . . H17C H 0.0349 0.5424 0.3384 0.077 Uiso 1 1 calc R . . C18 C 0.0381(3) 0.3441(3) 0.3941(3) 0.0493(9) Uani 1 1 d . . . H18A H -0.0035 0.3405 0.3555 0.074 Uiso 1 1 calc R . . H18B H -0.0093 0.3685 0.4397 0.074 Uiso 1 1 calc R . . H18C H 0.0685 0.2785 0.4198 0.074 Uiso 1 1 calc R . . C19 C 0.4594(2) 0.3118(2) 0.46478(19) 0.0319(7) Uani 1 1 d . . . H19 H 0.4867 0.2922 0.4114 0.038 Uiso 1 1 calc R . . C20 C 0.5458(3) 0.3702(3) 0.4690(2) 0.0440(8) Uani 1 1 d . . . H20A H 0.612 0.3286 0.4724 0.066 Uiso 1 1 calc R . . H20B H 0.5204 0.3919 0.5201 0.066 Uiso 1 1 calc R . . H20C H 0.5605 0.4277 0.4174 0.066 Uiso 1 1 calc R . . C21 C 0.4406(3) 0.2176(3) 0.5417(2) 0.0460(9) Uani 1 1 d . . . H21A H 0.5092 0.1796 0.544 0.069 Uiso 1 1 calc R . . H21B H 0.3896 0.1782 0.5353 0.069 Uiso 1 1 calc R . . H21C H 0.4109 0.2346 0.5948 0.069 Uiso 1 1 calc R . . C22 C 0.3530(2) 0.2011(2) 0.13680(17) 0.0239(6) Uani 1 1 d . . . C23 C 0.4397(2) 0.1575(2) 0.08778(18) 0.0286(6) Uani 1 1 d . . . C24 C 0.4330(3) 0.1594(2) 0.00697(19) 0.0366(7) Uani 1 1 d . . . H24 H 0.4907 0.1305 -0.0272 0.044 Uiso 1 1 calc R . . C25 C 0.3449(3) 0.2021(3) -0.0242(2) 0.0416(8) Uani 1 1 d . . . H25 H 0.3432 0.2043 -0.08 0.05 Uiso 1 1 calc R . . C26 C 0.2589(3) 0.2418(2) 0.02573(19) 0.0360(7) Uani 1 1 d . . . H26 H 0.1975 0.2695 0.0044 0.043 Uiso 1 1 calc R . . C27 C 0.2606(2) 0.2419(2) 0.10735(18) 0.0271(6) Uani 1 1 d . . . C28 C 0.5339(2) 0.1030(2) 0.1233(2) 0.0339(7) Uani 1 1 d . . . H28 H 0.5445 0.1352 0.1636 0.041 Uiso 1 1 calc R . . C29 C 0.5077(3) -0.0043(2) 0.1753(2) 0.0483(9) Uani 1 1 d . . . H29A H 0.5691 -0.0383 0.198 0.072 Uiso 1 1 calc R . . H29B H 0.4935 -0.0371 0.138 0.072 Uiso 1 1 calc R . . H29C H 0.4438 -0.006 0.2231 0.072 Uiso 1 1 calc R . . C30 C 0.6404(3) 0.1064(3) 0.0540(2) 0.0489(9) Uani 1 1 d . . . H30A H 0.6976 0.0701 0.0811 0.073 Uiso 1 1 calc R . . H30B H 0.6594 0.1749 0.0239 0.073 Uiso 1 1 calc R . . H30C H 0.6321 0.0762 0.0129 0.073 Uiso 1 1 calc R . . C31 C 0.1614(2) 0.2807(2) 0.16243(19) 0.0310(7) Uani 1 1 d . . . H31 H 0.1847 0.2967 0.2072 0.037 Uiso 1 1 calc R . . C32 C 0.1071(3) 0.3739(3) 0.1122(2) 0.0425(8) Uani 1 1 d . . . H32A H 0.0443 0.3948 0.1515 0.064 Uiso 1 1 calc R . . H32B H 0.0836 0.3603 0.0676 0.064 Uiso 1 1 calc R . . H32C H 0.1584 0.4263 0.0853 0.064 Uiso 1 1 calc R . . C33 C 0.0779(3) 0.2016(3) 0.2088(2) 0.0461(9) Uani 1 1 d . . . H33A H 0.0148 0.2277 0.2441 0.069 Uiso 1 1 calc R . . H33B H 0.1098 0.1438 0.2455 0.069 Uiso 1 1 calc R . . H33C H 0.0556 0.1829 0.1662 0.069 Uiso 1 1 calc R . . C34 C 0.5506(2) 0.5479(2) 0.24675(17) 0.0245(6) Uani 1 1 d . . . C35 C 0.4940(2) 0.6342(2) 0.26371(17) 0.0291(7) Uani 1 1 d . . . C36 C 0.5519(3) 0.7071(2) 0.2654(2) 0.0372(8) Uani 1 1 d . . . H36 H 0.5139 0.7641 0.2769 0.045 Uiso 1 1 calc R . . C37 C 0.6625(3) 0.6994(3) 0.2509(2) 0.0450(9) Uani 1 1 d . . . H37 H 0.7003 0.7508 0.2515 0.054 Uiso 1 1 calc R . . C38 C 0.7174(3) 0.6161(3) 0.2355(2) 0.0414(8) Uani 1 1 d . . . H38 H 0.7936 0.6103 0.2263 0.05 Uiso 1 1 calc R . . C39 C 0.6642(2) 0.5400(2) 0.23321(18) 0.0301(7) Uani 1 1 d . . . C40 C 0.3717(2) 0.6484(2) 0.27796(19) 0.0328(7) Uani 1 1 d . . . H40 H 0.3411 0.5823 0.3094 0.039 Uiso 1 1 calc R . . C41 C 0.3395(3) 0.6871(3) 0.1927(2) 0.0412(8) Uani 1 1 d . . . H41A H 0.3725 0.6439 0.1578 0.062 Uiso 1 1 calc R . . H41B H 0.3644 0.7537 0.1617 0.062 Uiso 1 1 calc R . . H41C H 0.2608 0.6884 0.204 0.062 Uiso 1 1 calc R . . C42 C 0.3193(3) 0.7154(3) 0.3324(2) 0.0513(9) Uani 1 1 d . . . H42A H 0.3395 0.6906 0.3872 0.077 Uiso 1 1 calc R . . H42B H 0.2407 0.7164 0.3434 0.077 Uiso 1 1 calc R . . H42C H 0.344 0.7821 0.3017 0.077 Uiso 1 1 calc R . . C43 C 0.7300(2) 0.4500(2) 0.2173(2) 0.0375(8) Uani 1 1 d . . . H43 H 0.6786 0.3995 0.2268 0.045 Uiso 1 1 calc R . . C44 C 0.8016(3) 0.4056(3) 0.2802(2) 0.0518(10) Uani 1 1 d . . . H44A H 0.8427 0.3476 0.2681 0.078 Uiso 1 1 calc R . . H44B H 0.7563 0.3865 0.3393 0.078 Uiso 1 1 calc R . . H44C H 0.8516 0.4544 0.2733 0.078 Uiso 1 1 calc R . . C45 C 0.7997(3) 0.4721(3) 0.1253(2) 0.0522(10) Uani 1 1 d . . . H45A H 0.8408 0.4121 0.1177 0.078 Uiso 1 1 calc R . . H45B H 0.8497 0.5228 0.1139 0.078 Uiso 1 1 calc R . . H45C H 0.7535 0.4956 0.0853 0.078 Uiso 1 1 calc R . . C46 C 0.5499(3) 0.1155(3) 0.3496(2) 0.0522(10) Uani 1 1 d . . . H46A H 0.5116 0.1298 0.4036 0.063 Uiso 1 1 calc R . . H46B H 0.5007 0.0816 0.3345 0.063 Uiso 1 1 calc R . . C47 C 0.6449(4) 0.0547(4) 0.3607(4) 0.100(2) Uani 1 1 d . . . H47A H 0.6317 -0.0151 0.3728 0.12 Uiso 1 1 calc R . . H47B H 0.669 0.0609 0.4086 0.12 Uiso 1 1 calc R . . C48 C 0.7292(4) 0.0925(3) 0.2750(3) 0.0734(13) Uani 1 1 d . . . H48A H 0.8032 0.0811 0.2831 0.088 Uiso 1 1 calc R . . H48B H 0.7244 0.0612 0.233 0.088 Uiso 1 1 calc R . . C49 C 0.6986(3) 0.1970(3) 0.2481(3) 0.0657(13) Uani 1 1 d . . . H49A H 0.7188 0.2244 0.1846 0.079 Uiso 1 1 calc R . . H49B H 0.7354 0.233 0.2716 0.079 Uiso 1 1 calc R . . C50 C 0.1108(5) -0.0706(4) 0.2347(4) 0.1036(19) Uani 1 1 d . . . H50A H 0.1485 -0.0802 0.28 0.124 Uiso 1 1 calc R . . H50B H 0.0579 -0.0144 0.2365 0.124 Uiso 1 1 calc R . . C51 C 0.1877(5) -0.0436(4) 0.1545(4) 0.0990(18) Uani 1 1 d . . . H51A H 0.2224 0.0155 0.1481 0.148 Uiso 1 1 calc R . . H51B H 0.1518 -0.03 0.1082 0.148 Uiso 1 1 calc R . . H51C H 0.2423 -0.0974 0.1516 0.148 Uiso 1 1 calc R . . C52 C -0.0137(6) -0.1841(7) 0.3327(4) 0.155(3) Uani 1 1 d . . . H52A H 0.0305 -0.2178 0.3739 0.186 Uiso 1 1 calc R . . H52B H -0.0493 -0.1256 0.3487 0.186 Uiso 1 1 calc R . . C53 C -0.0914(7) -0.2435(6) 0.3491(5) 0.161(4) Uani 1 1 d . . . H53A H -0.1305 -0.2595 0.4098 0.241 Uiso 1 1 calc R . . H53B H -0.0599 -0.304 0.3362 0.241 Uiso 1 1 calc R . . H53C H -0.1414 -0.2109 0.3132 0.241 Uiso 1 1 calc R . . C54 C 0.0867(7) 0.7484(7) 0.0099(8) 0.199(5) Uani 1 1 d . . . H54A H 0.1104 0.7487 -0.0506 0.239 Uiso 1 1 calc R . . H54B H 0.1394 0.7853 0.0182 0.239 Uiso 1 1 calc R . . C55 C 0.0936(7) 0.6597(6) 0.0574(5) 0.145(3) Uani 1 1 d . . . H55A H 0.1671 0.6322 0.041 0.218 Uiso 1 1 calc R . . H55B H 0.0426 0.6211 0.0502 0.218 Uiso 1 1 calc R . . H55C H 0.0763 0.6576 0.1177 0.218 Uiso 1 1 calc R . . C56 C -0.0438(8) 0.8299(8) 0.0859(7) 0.171(4) Uani 1 1 d . . . H56A H 0.0214 0.8508 0.0935 0.205 Uiso 1 1 calc R . . H56B H -0.0693 0.772 0.1361 0.205 Uiso 1 1 calc R . . C57 C -0.1283(5) 0.9105(5) 0.0880(5) 0.132(3) Uani 1 1 d . . . H57A H -0.1433 0.9236 0.143 0.199 Uiso 1 1 calc R . . H57B H -0.1943 0.891 0.0818 0.199 Uiso 1 1 calc R . . H57C H -0.103 0.97 0.0408 0.199 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 Y 0.02231(14) 0.01981(14) 0.01870(14) -0.00458(10) -0.00438(10) -0.00260(10) K 0.0395(4) 0.0330(4) 0.0270(3) -0.0058(3) -0.0076(3) -0.0074(3) Cl1 0.0307(4) 0.0337(4) 0.0241(4) -0.0067(3) 0.0002(3) -0.0006(3) Cl2 0.0292(4) 0.0274(4) 0.0277(4) -0.0035(3) -0.0114(3) -0.0013(3) O1 0.0323(11) 0.0297(11) 0.0362(12) -0.0066(9) -0.0107(9) 0.0029(9) O2 0.148(4) 0.119(3) 0.063(2) -0.039(2) 0.017(2) -0.073(3) O3 0.118(4) 0.246(7) 0.183(6) -0.116(5) -0.071(4) 0.064(4) N1 0.0239(12) 0.0237(12) 0.0198(11) -0.0084(10) -0.0030(9) -0.0042(9) N2 0.0273(12) 0.0216(12) 0.0177(11) -0.0073(10) -0.0047(10) -0.0012(9) N3 0.0211(13) 0.0255(13) 0.0337(14) -0.0125(11) -0.0048(11) -0.0013(10) C1 0.0245(14) 0.0260(15) 0.0167(13) -0.0057(11) -0.0043(11) -0.0023(11) C2 0.0254(14) 0.0218(14) 0.0186(14) -0.0050(11) -0.0036(11) -0.0036(11) C3 0.0284(15) 0.0186(14) 0.0237(14) -0.0084(11) -0.0074(12) -0.0012(11) C4 0.0291(15) 0.0239(15) 0.0222(14) -0.0050(12) -0.0074(12) -0.0047(12) C5 0.0340(17) 0.0286(16) 0.0306(16) -0.0071(13) -0.0009(13) -0.0063(13) C6 0.0416(19) 0.040(2) 0.0321(17) -0.0044(15) 0.0006(15) -0.0116(15) C7 0.061(2) 0.0288(18) 0.0392(19) 0.0023(15) -0.0098(18) -0.0192(16) C8 0.070(2) 0.0247(17) 0.039(2) -0.0060(15) -0.0067(18) -0.0067(16) C9 0.050(2) 0.0261(17) 0.0262(16) -0.0080(13) -0.0022(14) -0.0004(14) C10 0.0279(15) 0.0229(14) 0.0178(13) -0.0072(11) 0.0003(11) -0.0074(11) C11 0.0269(15) 0.0301(16) 0.0259(15) -0.0107(13) -0.0009(12) -0.0067(12) C12 0.0315(16) 0.0363(18) 0.0402(18) -0.0191(15) -0.0005(14) -0.0005(13) C13 0.0432(19) 0.043(2) 0.0393(19) -0.0274(16) 0.0020(15) -0.0062(15) C14 0.0441(19) 0.0411(19) 0.0297(17) -0.0198(15) -0.0071(14) -0.0090(15) C15 0.0322(16) 0.0277(16) 0.0229(15) -0.0084(12) -0.0031(12) -0.0072(12) C16 0.0259(15) 0.0409(19) 0.0402(18) -0.0170(15) -0.0075(14) 0.0009(13) C17 0.049(2) 0.048(2) 0.054(2) -0.0036(18) -0.0212(18) -0.0090(17) C18 0.041(2) 0.042(2) 0.069(3) -0.0097(18) -0.0251(19) -0.0084(16) C19 0.0380(17) 0.0375(18) 0.0254(15) -0.0134(13) -0.0125(13) -0.0005(14) C20 0.0418(19) 0.051(2) 0.0418(19) -0.0095(16) -0.0182(16) -0.0067(16) C21 0.058(2) 0.040(2) 0.042(2) -0.0084(16) -0.0226(18) -0.0018(17) C22 0.0336(16) 0.0211(14) 0.0182(14) -0.0063(11) -0.0048(12) -0.0093(12) C23 0.0365(16) 0.0262(15) 0.0246(15) -0.0106(12) -0.0040(13) -0.0073(13) C24 0.0450(19) 0.0428(19) 0.0252(16) -0.0178(14) -0.0013(14) -0.0100(15) C25 0.056(2) 0.052(2) 0.0234(16) -0.0154(15) -0.0088(16) -0.0160(17) C26 0.0390(18) 0.0436(19) 0.0291(17) -0.0083(14) -0.0143(14) -0.0102(15) C27 0.0317(16) 0.0277(16) 0.0227(14) -0.0069(12) -0.0056(12) -0.0096(12) C28 0.0397(18) 0.0316(17) 0.0303(16) -0.0144(14) -0.0057(14) 0.0039(14) C29 0.060(2) 0.0357(19) 0.046(2) -0.0141(16) -0.0116(18) 0.0058(17) C30 0.042(2) 0.054(2) 0.048(2) -0.0234(18) -0.0028(17) 0.0077(17) C31 0.0272(15) 0.0385(18) 0.0289(16) -0.0107(13) -0.0081(13) -0.0045(13) C32 0.0334(18) 0.046(2) 0.047(2) -0.0103(16) -0.0162(16) 0.0009(15) C33 0.0348(18) 0.051(2) 0.044(2) -0.0116(17) 0.0014(16) -0.0099(16) C34 0.0301(15) 0.0271(15) 0.0164(13) -0.0048(11) -0.0064(12) -0.0061(12) C35 0.0409(17) 0.0265(16) 0.0185(14) -0.0048(12) -0.0067(13) -0.0044(13) C36 0.055(2) 0.0298(17) 0.0314(17) -0.0127(14) -0.0121(15) -0.0079(15) C37 0.060(2) 0.040(2) 0.044(2) -0.0142(16) -0.0167(18) -0.0214(17) C38 0.0383(18) 0.050(2) 0.0407(19) -0.0117(16) -0.0138(15) -0.0147(16) C39 0.0330(16) 0.0330(17) 0.0251(15) -0.0051(13) -0.0102(13) -0.0081(13) C40 0.0410(18) 0.0251(16) 0.0303(16) -0.0110(13) -0.0037(14) -0.0001(13) C41 0.0407(19) 0.043(2) 0.0424(19) -0.0158(16) -0.0131(16) 0.0025(15) C42 0.062(2) 0.049(2) 0.043(2) -0.0259(18) -0.0095(18) 0.0132(18) C43 0.0245(16) 0.0440(19) 0.0458(19) -0.0137(16) -0.0111(14) -0.0034(14) C44 0.040(2) 0.060(2) 0.051(2) -0.0099(19) -0.0195(17) 0.0093(17) C45 0.042(2) 0.069(3) 0.048(2) -0.025(2) -0.0098(17) 0.0047(18) C46 0.053(2) 0.037(2) 0.045(2) 0.0079(17) -0.0091(18) 0.0069(16) C47 0.069(3) 0.060(3) 0.123(5) 0.034(3) -0.031(3) 0.000(2) C48 0.057(3) 0.065(3) 0.102(4) -0.031(3) -0.032(3) 0.023(2) C49 0.0306(19) 0.058(3) 0.078(3) 0.010(2) -0.0109(19) 0.0081(17) C50 0.115(5) 0.085(4) 0.107(5) -0.046(4) 0.002(4) -0.021(4) C51 0.113(4) 0.079(4) 0.088(4) -0.025(3) 0.011(3) -0.029(3) C52 0.146(6) 0.221(9) 0.094(5) -0.081(6) 0.052(5) -0.087(7) C53 0.184(8) 0.188(8) 0.097(5) -0.038(5) 0.029(5) -0.119(7) C54 0.098(6) 0.139(8) 0.328(15) -0.059(9) -0.028(8) 0.010(6) C55 0.177(8) 0.102(5) 0.112(5) -0.009(4) -0.020(5) 0.038(5) C56 0.162(8) 0.232(11) 0.173(9) -0.117(8) -0.092(7) 0.056(7) C57 0.096(5) 0.094(5) 0.184(8) -0.027(5) -0.028(5) 0.014(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y N3 2.259(2) . ? Y N1 2.400(2) . ? Y O1 2.4351(19) . ? Y N2 2.473(2) . ? Y Cl2 2.6093(7) . ? Y Cl1 2.6134(7) . ? K N3 3.116(3) . ? K Cl1 3.1557(10) 2_665 ? K Cl2 3.1733(10) 2_665 ? K C34 3.265(3) . ? K Cl2 3.2850(9) . ? K C25 3.328(3) 2_665 ? K Cl1 3.3315(10) . ? K C26 3.378(3) 2_665 ? K C24 3.449(3) 2_665 ? K C27 3.530(3) 2_665 ? Cl1 K 3.1557(10) 2_665 ? Cl2 K 3.1733(10) 2_665 ? O1 C46 1.448(4) . ? O1 C49 1.458(4) . ? O2 C50 1.321(6) . ? O2 C52 1.350(6) . ? O3 C56 1.243(8) . ? O3 C54 1.450(9) . ? N1 C1 1.325(3) . ? N1 C10 1.456(3) . ? N2 C3 1.317(3) . ? N2 C22 1.448(3) . ? N3 C34 1.395(4) . ? C1 C2 1.401(4) . ? C2 C3 1.408(4) . ? C2 C4 1.484(4) . ? C4 C9 1.392(4) . ? C4 C5 1.399(4) . ? C5 C6 1.381(4) . ? C6 C7 1.378(5) . ? C7 C8 1.370(5) . ? C8 C9 1.388(4) . ? C10 C11 1.404(4) . ? C10 C15 1.406(4) . ? C11 C12 1.394(4) . ? C11 C16 1.519(4) . ? C12 C13 1.380(5) . ? C13 C14 1.372(5) . ? C14 C15 1.400(4) . ? C15 C19 1.508(4) . ? C16 C17 1.523(5) . ? C16 C18 1.527(4) . ? C19 C20 1.525(4) . ? C19 C21 1.532(4) . ? C22 C27 1.406(4) . ? C22 C23 1.408(4) . ? C23 C24 1.399(4) . ? C23 C28 1.517(4) . ? C24 C25 1.376(5) . ? C24 K 3.449(3) 2_665 ? C25 C26 1.382(5) . ? C25 K 3.328(3) 2_665 ? C26 C27 1.402(4) . ? C26 K 3.378(3) 2_665 ? C27 C31 1.523(4) . ? C27 K 3.530(3) 2_665 ? C28 C30 1.536(4) . ? C28 C29 1.537(4) . ? C31 C32 1.532(4) . ? C31 C33 1.535(4) . ? C34 C39 1.417(4) . ? C34 C35 1.431(4) . ? C35 C36 1.389(4) . ? C35 C40 1.527(4) . ? C36 C37 1.378(5) . ? C37 C38 1.376(5) . ? C38 C39 1.396(4) . ? C39 C43 1.513(4) . ? C40 C42 1.527(4) . ? C40 C41 1.530(4) . ? C43 C45 1.524(5) . ? C43 C44 1.537(5) . ? C46 C47 1.428(5) . ? C47 C48 1.534(7) . ? C48 C49 1.455(6) . ? C50 C51 1.412(7) . ? C52 C53 1.323(9) . ? C54 C55 1.272(10) . ? C56 C57 1.485(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Y N1 91.81(8) . . ? N3 Y O1 106.26(8) . . ? N1 Y O1 90.61(7) . . ? N3 Y N2 162.65(8) . . ? N1 Y N2 75.65(7) . . ? O1 Y N2 86.14(7) . . ? N3 Y Cl2 84.66(7) . . ? N1 Y Cl2 99.21(6) . . ? O1 Y Cl2 165.17(5) . . ? N2 Y Cl2 85.57(5) . . ? N3 Y Cl1 97.47(7) . . ? N1 Y Cl1 169.90(6) . . ? O1 Y Cl1 82.99(5) . . ? N2 Y Cl1 96.05(5) . . ? Cl2 Y Cl1 85.68(2) . . ? N3 K Cl1 128.07(5) . 2_665 ? N3 K Cl2 137.03(5) . 2_665 ? Cl1 K Cl2 68.26(2) 2_665 2_665 ? N3 K C34 25.11(6) . . ? Cl1 K C34 141.95(6) 2_665 . ? Cl2 K C34 147.22(6) 2_665 . ? N3 K Cl2 61.76(5) . . ? Cl1 K Cl2 68.83(2) 2_665 . ? Cl2 K Cl2 103.36(2) 2_665 . ? C34 K Cl2 84.53(5) . . ? N3 K C25 106.45(7) . 2_665 ? Cl1 K C25 105.49(6) 2_665 2_665 ? Cl2 K C25 105.03(6) 2_665 2_665 ? C34 K C25 81.55(7) . 2_665 ? Cl2 K C25 146.15(7) . 2_665 ? N3 K Cl1 69.29(5) . . ? Cl1 K Cl1 103.79(2) 2_665 . ? Cl2 K Cl1 68.04(2) 2_665 . ? C34 K Cl1 87.76(5) . . ? Cl2 K Cl1 64.92(2) . . ? C25 K Cl1 144.39(7) 2_665 . ? N3 K C26 116.84(7) . 2_665 ? Cl1 K C26 108.84(6) 2_665 2_665 ? Cl2 K C26 84.38(6) 2_665 2_665 ? C34 K C26 92.52(7) . 2_665 ? Cl2 K C26 169.79(6) . 2_665 ? C25 K C26 23.77(8) 2_665 2_665 ? Cl1 K C26 124.84(6) . 2_665 ? N3 K C24 116.07(7) . 2_665 ? Cl1 K C24 83.52(6) 2_665 2_665 ? Cl2 K C24 104.34(5) 2_665 2_665 ? C34 K C24 93.97(7) . 2_665 ? Cl2 K C24 129.41(6) . 2_665 ? C25 K C24 23.34(8) 2_665 2_665 ? Cl1 K C24 165.66(6) . 2_665 ? C26 K C24 40.91(8) 2_665 2_665 ? N3 K C27 139.32(7) . 2_665 ? Cl1 K C27 90.20(5) 2_665 2_665 ? Cl2 K C27 63.75(5) 2_665 2_665 ? C34 K C27 115.64(7) . 2_665 ? Cl2 K C27 158.73(5) . 2_665 ? C25 K C27 41.28(7) 2_665 2_665 ? Cl1 K C27 119.62(5) . 2_665 ? C26 K C27 23.27(7) 2_665 2_665 ? C24 K C27 47.18(7) 2_665 2_665 ? Y Cl1 K 98.80(3) . 2_665 ? Y Cl1 K 82.67(2) . . ? K Cl1 K 76.21(2) 2_665 . ? Y Cl2 K 98.45(3) . 2_665 ? Y Cl2 K 83.66(2) . . ? K Cl2 K 76.64(2) 2_665 . ? C46 O1 C49 107.1(2) . . ? C46 O1 Y 124.83(18) . . ? C49 O1 Y 127.53(19) . . ? C50 O2 C52 121.9(5) . . ? C56 O3 C54 114.8(8) . . ? C1 N1 C10 112.0(2) . . ? C1 N1 Y 127.53(18) . . ? C10 N1 Y 120.31(16) . . ? C3 N2 C22 113.8(2) . . ? C3 N2 Y 127.02(17) . . ? C22 N2 Y 119.11(16) . . ? C34 N3 Y 163.8(2) . . ? C34 N3 K 83.42(15) . . ? Y N3 K 93.64(8) . . ? N1 C1 C2 129.5(2) . . ? C1 C2 C3 123.5(2) . . ? C1 C2 C4 118.6(2) . . ? C3 C2 C4 117.4(2) . . ? N2 C3 C2 128.3(3) . . ? C9 C4 C5 116.8(3) . . ? C9 C4 C2 121.2(3) . . ? C5 C4 C2 122.0(3) . . ? C6 C5 C4 121.4(3) . . ? C7 C6 C5 120.5(3) . . ? C8 C7 C6 119.4(3) . . ? C7 C8 C9 120.3(3) . . ? C8 C9 C4 121.7(3) . . ? C11 C10 C15 121.6(3) . . ? C11 C10 N1 118.6(2) . . ? C15 C10 N1 119.8(2) . . ? C12 C11 C10 118.0(3) . . ? C12 C11 C16 120.3(3) . . ? C10 C11 C16 121.6(3) . . ? C13 C12 C11 121.2(3) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 121.5(3) . . ? C14 C15 C10 117.6(3) . . ? C14 C15 C19 120.8(3) . . ? C10 C15 C19 121.6(3) . . ? C11 C16 C17 113.5(3) . . ? C11 C16 C18 111.0(3) . . ? C17 C16 C18 109.1(3) . . ? C15 C19 C20 112.3(3) . . ? C15 C19 C21 110.6(3) . . ? C20 C19 C21 110.6(3) . . ? C27 C22 C23 121.4(2) . . ? C27 C22 N2 119.2(2) . . ? C23 C22 N2 119.4(2) . . ? C24 C23 C22 117.9(3) . . ? C24 C23 C28 120.3(3) . . ? C22 C23 C28 121.7(3) . . ? C25 C24 C23 121.6(3) . . ? C25 C24 K 73.40(19) . 2_665 ? C23 C24 K 84.56(18) . 2_665 ? C24 C25 C26 119.9(3) . . ? C24 C25 K 83.26(19) . 2_665 ? C26 C25 K 80.16(19) . 2_665 ? C25 C26 C27 121.2(3) . . ? C25 C26 K 76.08(19) . 2_665 ? C27 C26 K 84.47(17) . 2_665 ? C26 C27 C22 118.0(3) . . ? C26 C27 C31 119.4(3) . . ? C22 C27 C31 122.5(2) . . ? C26 C27 K 72.26(17) . 2_665 ? C22 C27 K 81.28(16) . 2_665 ? C31 C27 K 118.87(18) . 2_665 ? C23 C28 C30 113.6(3) . . ? C23 C28 C29 110.5(3) . . ? C30 C28 C29 109.8(3) . . ? C27 C31 C32 113.9(3) . . ? C27 C31 C33 110.6(3) . . ? C32 C31 C33 108.8(3) . . ? N3 C34 C39 120.2(3) . . ? N3 C34 C35 121.7(3) . . ? C39 C34 C35 118.1(3) . . ? N3 C34 K 71.47(14) . . ? C39 C34 K 95.98(17) . . ? C35 C34 K 102.00(17) . . ? C36 C35 C34 119.2(3) . . ? C36 C35 C40 119.7(3) . . ? C34 C35 C40 121.1(3) . . ? C37 C36 C35 122.2(3) . . ? C38 C37 C36 118.9(3) . . ? C37 C38 C39 121.8(3) . . ? C38 C39 C34 119.7(3) . . ? C38 C39 C43 118.7(3) . . ? C34 C39 C43 121.6(3) . . ? C42 C40 C35 113.8(3) . . ? C42 C40 C41 109.3(3) . . ? C35 C40 C41 111.5(2) . . ? C39 C43 C45 112.0(3) . . ? C39 C43 C44 111.8(3) . . ? C45 C43 C44 109.4(3) . . ? C47 C46 O1 108.1(3) . . ? C46 C47 C48 104.8(3) . . ? C49 C48 C47 101.9(4) . . ? C48 C49 O1 106.7(3) . . ? O2 C50 C51 118.2(5) . . ? C53 C52 O2 124.4(7) . . ? C55 C54 O3 119.2(9) . . ? O3 C56 C57 117.6(8) . . ? #===END