Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'M. Lappert' 'P. B. Hitchcock' 'Xue-Hong Wei.' _publ_contact_author_name 'M. Lappert' _publ_contact_author_address ; School of Chemistry & Molecular Science University of Sussex BRIGHTON BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and structures of some bimetallic (Li/Ca, Li/Zn, Li/Li) diamides derived from 1,2-bis(neopentylamino)benzene and of Li2[{N(SiMe2NPri2)}2C6H4-1,2](thf)3 ; _publ_requested_category FM data_(1)-jul2603 _database_code_depnum_ccdc_archive 'CCDC 284204' _audit_creation_date 2003-07-25T15:07:07-00:00 _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 'C32 H58 Ca1 I1 Li1 N2 O4' _chemical_formula_sum 'C32 H58 Ca1 I1 Li1 N2 O4' _chemical_formula_weight 708.72 _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 11.5585(1) _cell_length_b 10.8561(1) _cell_length_c 28.5205(3) _cell_angle_alpha 90 _cell_angle_beta 90.538(1) _cell_angle_gamma 90 _cell_volume 3578.60(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 55553 _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 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.073 _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 0.6018 _exptl_absorpt_correction_T_max 0.6848 #----------------------------------------------------------------------------# # 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 0.517448E-1 _diffrn_orient_matrix_ub_12 -0.25278E-1 _diffrn_orient_matrix_ub_13 0.26599E-1 _diffrn_orient_matrix_ub_21 -0.618012E-1 _diffrn_orient_matrix_ub_22 -0.560599E-1 _diffrn_orient_matrix_ub_23 0.118802E-1 _diffrn_orient_matrix_ub_31 0.314456E-1 _diffrn_orient_matrix_ub_32 -0.685807E-1 _diffrn_orient_matrix_ub_33 -0.195152E-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 0.0523 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_number 39655 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 6267 _reflns_number_gt 5636 _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^)+(0.0000P)^2^+25.2462P] 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 6267 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.219 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.897 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.101 #----------------------------------------------------------------------------# # 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 Ca Ca 0.29765(9) 0.50906(10) 0.12455(4) 0.0259(3) Uani 1 1 d . . . Li Li 0.1487(9) 0.7164(9) 0.1369(4) 0.034(2) Uani 1 1 d . . . I I 0.02526(3) 0.48532(4) 0.130978(16) 0.03850(15) Uani 1 1 d . . . O1 O 0.5031(3) 0.5102(4) 0.11900(15) 0.0359(10) Uani 1 1 d . . . O2 O 0.3181(4) 0.3272(4) 0.07410(15) 0.0348(10) Uani 1 1 d . . . O3 O 0.3151(4) 0.3472(4) 0.18316(17) 0.0453(12) Uani 1 1 d . . . O4 O 0.0423(4) 0.8503(4) 0.13867(16) 0.0379(10) Uani 1 1 d . . . N1 N 0.2790(4) 0.7116(4) 0.08685(16) 0.0256(10) Uani 1 1 d . . . N2 N 0.2864(4) 0.6751(4) 0.17965(16) 0.0248(10) Uani 1 1 d . . . C1 C 0.3586(5) 0.7824(5) 0.1122(2) 0.0254(12) Uani 1 1 d . . . C2 C 0.3636(5) 0.7614(5) 0.1625(2) 0.0261(12) Uani 1 1 d . . . C3 C 0.4465(5) 0.8283(6) 0.1888(2) 0.0341(14) Uani 1 1 d . . . H3 H 0.4517 0.8152 0.2217 0.041 Uiso 1 1 calc R . . C4 C 0.5216(5) 0.9138(6) 0.1678(2) 0.0381(15) Uani 1 1 d . . . H4 H 0.5777 0.9557 0.1865 0.046 Uiso 1 1 calc R . . C5 C 0.5141(5) 0.9365(6) 0.1213(2) 0.0388(15) Uani 1 1 d . . . H5 H 0.5633 0.9959 0.1073 0.047 Uiso 1 1 calc R . . C6 C 0.4331(5) 0.8715(5) 0.0937(2) 0.0328(13) Uani 1 1 d . . . H6 H 0.4287 0.8887 0.061 0.039 Uiso 1 1 calc R . . C7 C 0.2776(5) 0.7466(6) 0.0371(2) 0.0325(13) Uani 1 1 d . . . H7A H 0.3549 0.7282 0.0242 0.039 Uiso 1 1 calc R . . H7B H 0.2667 0.8369 0.0353 0.039 Uiso 1 1 calc R . . C8 C 0.1869(5) 0.6863(6) 0.0053(2) 0.0331(14) Uani 1 1 d . . . C9 C 0.0640(5) 0.7284(7) 0.0178(2) 0.0450(17) Uani 1 1 d . . . H9A H 0.0079 0.688 -0.0031 0.068 Uiso 1 1 calc R . . H9B H 0.0581 0.8179 0.0141 0.068 Uiso 1 1 calc R . . H9C H 0.0478 0.7061 0.0504 0.068 Uiso 1 1 calc R . . C10 C 0.1938(6) 0.5458(6) 0.0076(2) 0.0425(16) Uani 1 1 d . . . H10A H 0.1348 0.51 -0.0132 0.064 Uiso 1 1 calc R . . H10B H 0.1804 0.5185 0.0398 0.064 Uiso 1 1 calc R . . H10C H 0.2706 0.5187 -0.0024 0.064 Uiso 1 1 calc R . . C11 C 0.2136(6) 0.7277(7) -0.0450(2) 0.0438(16) Uani 1 1 d . . . H11A H 0.1574 0.6906 -0.0668 0.066 Uiso 1 1 calc R . . H11B H 0.2918 0.7013 -0.0534 0.066 Uiso 1 1 calc R . . H11C H 0.2084 0.8177 -0.047 0.066 Uiso 1 1 calc R . . C12 C 0.2902(5) 0.6507(6) 0.2299(2) 0.0311(13) Uani 1 1 d . . . H12A H 0.3696 0.6683 0.2413 0.037 Uiso 1 1 calc R . . H12B H 0.2764 0.5615 0.2346 0.037 Uiso 1 1 calc R . . C13 C 0.2047(5) 0.7220(6) 0.2616(2) 0.0333(14) Uani 1 1 d . . . C14 C 0.0810(6) 0.6792(7) 0.2528(3) 0.0488(18) Uani 1 1 d . . . H14A H 0.0593 0.6959 0.2201 0.073 Uiso 1 1 calc R . . H14B H 0.0287 0.7236 0.2736 0.073 Uiso 1 1 calc R . . H14C H 0.0755 0.5906 0.2588 0.073 Uiso 1 1 calc R . . C15 C 0.2084(6) 0.8610(6) 0.2532(2) 0.0410(15) Uani 1 1 d . . . H15A H 0.2872 0.8913 0.2588 0.062 Uiso 1 1 calc R . . H15B H 0.1551 0.9021 0.2747 0.062 Uiso 1 1 calc R . . H15C H 0.1853 0.8786 0.2208 0.062 Uiso 1 1 calc R . . C16 C 0.2380(6) 0.6949(7) 0.3128(2) 0.0470(17) Uani 1 1 d . . . H16A H 0.3175 0.7225 0.3188 0.071 Uiso 1 1 calc R . . H16B H 0.2324 0.6062 0.3186 0.071 Uiso 1 1 calc R . . H16C H 0.1852 0.7389 0.3337 0.071 Uiso 1 1 calc R . . C17 C 0.5745(6) 0.5198(8) 0.1608(3) 0.0520(19) Uani 1 1 d . . . H17A H 0.591 0.437 0.1739 0.062 Uiso 1 1 calc R . . H17B H 0.5351 0.5694 0.185 0.062 Uiso 1 1 calc R . . C18 C 0.6813(7) 0.5796(13) 0.1465(4) 0.102(4) Uani 1 1 d . . . H18A H 0.6994 0.6485 0.1681 0.122 Uiso 1 1 calc R . . H18B H 0.746 0.5199 0.1481 0.122 Uiso 1 1 calc R . . C19 C 0.6698(7) 0.6245(9) 0.1006(3) 0.064(2) Uani 1 1 d . . . H19A H 0.738 0.6012 0.0818 0.077 Uiso 1 1 calc R . . H19B H 0.6633 0.7155 0.1008 0.077 Uiso 1 1 calc R . . C20 C 0.5619(6) 0.5678(6) 0.0803(2) 0.0403(15) Uani 1 1 d . . . H20A H 0.5123 0.6317 0.0657 0.048 Uiso 1 1 calc R . . H20B H 0.5816 0.5058 0.0562 0.048 Uiso 1 1 calc R . . C21 C 0.4130(6) 0.2887(7) 0.0454(3) 0.0456(17) Uani 1 1 d . . . H21A H 0.4822 0.2723 0.0651 0.055 Uiso 1 1 calc R . . H21B H 0.4324 0.354 0.0225 0.055 Uiso 1 1 calc R . . C22 C 0.3771(8) 0.1742(7) 0.0202(3) 0.061(2) Uani 1 1 d . . . H22A H 0.4148 0.1009 0.0342 0.073 Uiso 1 1 calc R . . H22B H 0.3974 0.1788 -0.0134 0.073 Uiso 1 1 calc R . . C23 C 0.2487(8) 0.1691(9) 0.0262(3) 0.075(3) Uani 1 1 d . . . H23A H 0.2084 0.2109 -0.0001 0.091 Uiso 1 1 calc R . . H23B H 0.2215 0.0827 0.0279 0.091 Uiso 1 1 calc R . . C24 C 0.2282(7) 0.2339(8) 0.0707(3) 0.060(2) Uani 1 1 d . . . H24A H 0.1506 0.2725 0.0705 0.072 Uiso 1 1 calc R . . H24B H 0.2335 0.176 0.0974 0.072 Uiso 1 1 calc R . . C25 C 0.3990(6) 0.2501(7) 0.1834(3) 0.0465(17) Uani 1 1 d . . . H25A H 0.4713 0.2775 0.1991 0.056 Uiso 1 1 calc R . . H25B H 0.4172 0.2248 0.151 0.056 Uiso 1 1 calc R . . C26 C 0.3455(7) 0.1446(8) 0.2099(4) 0.073(3) Uani 1 1 d . . . H26A H 0.336 0.0715 0.1895 0.088 Uiso 1 1 calc R . . H26B H 0.3936 0.1219 0.2375 0.088 Uiso 1 1 calc R . . C27 C 0.2301(9) 0.1944(9) 0.2248(5) 0.113(5) Uani 1 1 d . . . H27A H 0.1673 0.1564 0.2058 0.136 Uiso 1 1 calc R . . H27B H 0.2165 0.1752 0.2582 0.136 Uiso 1 1 calc R . . C28 C 0.2312(9) 0.3152(8) 0.2183(4) 0.088(4) Uani 1 1 d . . . H28A H 0.251 0.357 0.2482 0.106 Uiso 1 1 calc R . . H28B H 0.1535 0.3434 0.2081 0.106 Uiso 1 1 calc R . . C29 C 0.0777(7) 0.9685(7) 0.1227(3) 0.060(2) Uani 1 1 d . . . H29A H 0.1021 1.0197 0.1497 0.072 Uiso 1 1 calc R . . H29B H 0.1445 0.9597 0.1015 0.072 Uiso 1 1 calc R . . C30 C -0.0141(7) 1.0262(7) 0.0987(3) 0.059(2) Uani 1 1 d . . . H30A H 0.006 1.0402 0.0655 0.07 Uiso 1 1 calc R . . H30B H -0.0322 1.1066 0.1133 0.07 Uiso 1 1 calc R . . C31 C -0.1186(7) 0.9379(8) 0.1024(3) 0.061(2) Uani 1 1 d . . . H31A H -0.1902 0.9832 0.1102 0.073 Uiso 1 1 calc R . . H31B H -0.131 0.8918 0.0728 0.073 Uiso 1 1 calc R . . C32 C -0.0818(6) 0.8519(7) 0.1423(3) 0.0512(19) Uani 1 1 d . . . H32A H -0.1063 0.8845 0.1731 0.061 Uiso 1 1 calc R . . H32B H -0.1146 0.7684 0.1379 0.061 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 Ca 0.0225(5) 0.0211(6) 0.0342(6) 0.0019(5) 0.0011(5) 0.0001(4) Li 0.027(5) 0.033(5) 0.042(6) 0.002(5) 0.004(4) 0.005(4) I 0.0242(2) 0.0381(2) 0.0533(3) -0.0049(2) 0.00351(16) -0.00695(17) O1 0.028(2) 0.037(2) 0.042(2) 0.0038(19) -0.0025(18) 0.0008(18) O2 0.034(2) 0.029(2) 0.042(2) -0.0041(19) 0.0011(19) -0.0027(18) O3 0.054(3) 0.030(2) 0.052(3) 0.016(2) 0.021(2) 0.010(2) O4 0.027(2) 0.030(2) 0.057(3) 0.007(2) -0.001(2) 0.0057(18) N1 0.023(2) 0.026(2) 0.027(2) 0.005(2) -0.0018(19) 0.0002(19) N2 0.022(2) 0.027(2) 0.026(2) 0.0034(19) 0.0006(19) -0.0022(19) C1 0.019(3) 0.020(3) 0.037(3) 0.001(2) 0.001(2) 0.003(2) C2 0.023(3) 0.022(3) 0.033(3) -0.001(2) -0.001(2) 0.001(2) C3 0.028(3) 0.036(3) 0.039(3) -0.005(3) -0.003(3) -0.004(3) C4 0.027(3) 0.032(3) 0.055(4) -0.007(3) -0.002(3) -0.005(3) C5 0.030(3) 0.029(3) 0.057(4) 0.006(3) 0.005(3) -0.011(3) C6 0.029(3) 0.030(3) 0.039(3) 0.008(3) 0.005(3) -0.002(3) C7 0.032(3) 0.035(3) 0.030(3) 0.007(3) 0.002(3) 0.005(3) C8 0.032(3) 0.038(3) 0.029(3) 0.003(3) -0.005(2) 0.007(3) C9 0.033(3) 0.058(5) 0.044(4) 0.004(3) -0.009(3) 0.007(3) C10 0.051(4) 0.042(4) 0.035(4) -0.001(3) -0.003(3) 0.004(3) C11 0.050(4) 0.051(4) 0.031(3) 0.009(3) -0.006(3) 0.005(3) C12 0.031(3) 0.032(3) 0.030(3) 0.005(3) -0.001(2) 0.000(3) C13 0.033(3) 0.036(3) 0.031(3) 0.002(3) 0.003(3) -0.002(3) C14 0.034(4) 0.063(5) 0.050(4) -0.004(4) 0.009(3) -0.006(3) C15 0.046(4) 0.037(4) 0.040(4) -0.002(3) 0.006(3) 0.005(3) C16 0.050(4) 0.055(4) 0.036(4) 0.002(3) 0.006(3) -0.001(3) C17 0.036(4) 0.060(5) 0.060(5) 0.018(4) -0.014(3) -0.004(3) C18 0.038(5) 0.183(13) 0.085(7) 0.053(8) -0.010(5) -0.044(6) C19 0.054(5) 0.073(6) 0.063(5) 0.008(4) 0.002(4) -0.031(4) C20 0.035(3) 0.044(4) 0.042(4) -0.001(3) 0.009(3) -0.004(3) C21 0.045(4) 0.046(4) 0.046(4) -0.002(3) 0.012(3) 0.002(3) C22 0.078(6) 0.040(4) 0.066(5) -0.009(4) 0.024(4) 0.002(4) C23 0.075(6) 0.068(6) 0.083(6) -0.040(5) 0.019(5) -0.027(5) C24 0.052(5) 0.057(5) 0.071(5) -0.022(4) 0.011(4) -0.016(4) C25 0.038(4) 0.053(4) 0.049(4) 0.019(3) 0.004(3) 0.011(3) C26 0.059(5) 0.044(5) 0.117(8) 0.037(5) 0.025(5) 0.013(4) C27 0.082(7) 0.061(6) 0.199(13) 0.067(7) 0.089(8) 0.033(5) C28 0.100(8) 0.057(5) 0.109(8) 0.043(5) 0.071(7) 0.035(5) C29 0.045(4) 0.040(4) 0.095(6) 0.009(4) -0.001(4) -0.008(3) C30 0.061(5) 0.047(4) 0.069(5) 0.015(4) 0.023(4) 0.006(4) C31 0.039(4) 0.077(6) 0.065(5) -0.015(4) -0.014(4) 0.018(4) C32 0.031(4) 0.041(4) 0.081(6) 0.005(4) 0.010(4) 0.005(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 Ca O1 2.381(4) . ? Ca N2 2.396(5) . ? Ca O3 2.433(4) . ? Ca O2 2.455(4) . ? Ca N1 2.456(5) . ? Ca I 3.1660(11) . ? Li O4 1.905(11) . ? Li N2 2.046(11) . ? Li N1 2.085(11) . ? Li I 2.891(10) . ? O1 C20 1.445(8) . ? O1 C17 1.448(8) . ? O2 C21 1.438(8) . ? O2 C24 1.454(8) . ? O3 C25 1.432(8) . ? O3 C28 1.443(9) . ? O4 C29 1.423(8) . ? O4 C32 1.439(8) . ? N1 C1 1.396(7) . ? N1 C7 1.468(7) . ? N2 C2 1.386(7) . ? N2 C12 1.458(7) . ? C1 C6 1.401(8) . ? C1 C2 1.454(8) . ? C2 C3 1.411(8) . ? C3 C4 1.408(9) . ? C4 C5 1.352(10) . ? C5 C6 1.408(9) . ? C7 C8 1.529(8) . ? C8 C10 1.529(9) . ? C8 C11 1.537(8) . ? C8 C9 1.538(9) . ? C12 C13 1.552(8) . ? C13 C14 1.522(9) . ? C13 C15 1.528(9) . ? C13 C16 1.534(9) . ? C17 C18 1.457(10) . ? C18 C19 1.401(12) . ? C19 C20 1.503(10) . ? C21 C22 1.491(10) . ? C22 C23 1.497(12) . ? C23 C24 1.472(11) . ? C25 C26 1.508(10) . ? C26 C27 1.504(12) . ? C27 C28 1.325(12) . ? C29 C30 1.404(11) . ? C30 C31 1.546(11) . ? C31 C32 1.530(11) . ? 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 Ca N2 95.74(15) . . ? O1 Ca O3 88.45(15) . . ? N2 Ca O3 95.60(16) . . ? O1 Ca O2 82.16(15) . . ? N2 Ca O2 174.49(15) . . ? O3 Ca O2 79.28(16) . . ? O1 Ca N1 92.86(15) . . ? N2 Ca N1 66.95(15) . . ? O3 Ca N1 162.55(17) . . ? O2 Ca N1 118.15(15) . . ? O1 Ca C2 76.83(15) . . ? O1 Ca I 175.60(11) . . ? N2 Ca I 87.89(11) . . ? O3 Ca I 88.71(12) . . ? O2 Ca I 94.00(10) . . ? N1 Ca I 90.85(11) . . ? C2 Ca I 107.39(11) . . ? C1 Ca I 108.35(10) . . ? O4 Li N2 130.6(6) . . ? O4 Li N1 120.5(5) . . ? N2 Li N1 80.8(4) . . ? O4 Li I 110.2(4) . . ? N2 Li I 103.0(4) . . ? N1 Li I 107.3(4) . . ? C2 Li I 129.9(4) . . ? C1 Li I 132.6(4) . . ? Li I Ca 56.08(19) . . ? C20 O1 C17 109.2(5) . . ? C20 O1 Ca 122.0(4) . . ? C17 O1 Ca 120.5(4) . . ? C21 O2 C24 107.9(5) . . ? C21 O2 Ca 130.3(4) . . ? C24 O2 Ca 121.8(4) . . ? C25 O3 C28 106.2(5) . . ? C25 O3 Ca 126.0(4) . . ? C28 O3 Ca 126.8(4) . . ? C29 O4 C32 107.6(5) . . ? C29 O4 Li 119.5(5) . . ? C32 O4 Li 130.9(5) . . ? C1 N1 C7 111.0(5) . . ? C1 N1 Li 96.2(4) . . ? C7 N1 Li 130.8(5) . . ? C1 N1 Ca 102.2(3) . . ? C7 N1 Ca 130.9(4) . . ? Li N1 Ca 77.5(3) . . ? C2 N2 C12 117.1(5) . . ? C2 N2 Li 98.2(4) . . ? C12 N2 Li 129.9(5) . . ? C2 N2 Ca 103.8(3) . . ? C12 N2 Ca 120.4(4) . . ? Li N2 Ca 79.7(3) . . ? N1 C1 C6 126.1(5) . . ? N1 C1 C2 116.4(5) . . ? C6 C1 C2 117.5(5) . . ? N2 C2 C3 126.6(5) . . ? N2 C2 C1 115.8(5) . . ? C3 C2 C1 117.6(5) . . ? C4 C3 C2 122.2(6) . . ? C5 C4 C3 120.2(6) . . ? C4 C5 C6 119.6(6) . . ? C1 C6 C5 122.8(6) . . ? N1 C7 C8 117.7(5) . . ? C10 C8 C7 111.5(5) . . ? C10 C8 C11 108.8(5) . . ? C7 C8 C11 106.7(5) . . ? C10 C8 C9 109.5(6) . . ? C7 C8 C9 111.3(5) . . ? C11 C8 C9 108.9(5) . . ? N2 C12 C13 117.9(5) . . ? C14 C13 C15 107.6(6) . . ? C14 C13 C16 109.0(5) . . ? C15 C13 C16 109.3(5) . . ? C14 C13 C12 110.7(5) . . ? C15 C13 C12 112.5(5) . . ? C16 C13 C12 107.7(5) . . ? O1 C17 C18 106.2(6) . . ? C19 C18 C17 110.1(7) . . ? C18 C19 C20 106.8(7) . . ? O1 C20 C19 106.1(5) . . ? O2 C21 C22 107.8(6) . . ? C21 C22 C23 104.4(6) . . ? C24 C23 C22 104.3(7) . . ? O2 C24 C23 105.7(6) . . ? O3 C25 C26 106.3(5) . . ? C27 C26 C25 103.7(6) . . ? C28 C27 C26 107.8(8) . . ? C27 C28 O3 110.0(7) . . ? C30 C29 O4 109.9(6) . . ? C29 C30 C31 106.1(6) . . ? C32 C31 C30 102.5(6) . . ? O4 C32 C31 103.0(6) . . ? #===END data_(2)-nov1203 _database_code_depnum_ccdc_archive 'CCDC 284205' _audit_creation_date 2003-11-14T14:14:30-00:00 _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 'C48 H78 Cl1 N6 Zn3, C16 H32 Li1 O4' _chemical_formula_sum 'C64 H110 Cl1 Li1 N6 O4 Zn3' _chemical_formula_weight 1266.08 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pa-3 _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_Int_Tables_number 205 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' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-y, -z, -x' 'y-1/2, z, -x-1/2' '-y-1/2, z-1/2, x' 'y, -z-1/2, x-1/2' '-z, -x, -y' 'z, -x-1/2, y-1/2' 'z-1/2, x, -y-1/2' '-z-1/2, x-1/2, y' _cell_length_a 24.2097(3) _cell_length_b 24.2097(3) _cell_length_c 24.2097(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14189.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 56140 _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 colouirless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5424 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.089 _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 0.7806 _exptl_absorpt_correction_T_max 0.8566 #----------------------------------------------------------------------------# # 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 0.338424E-1 _diffrn_orient_matrix_ub_12 -0.4846E-3 _diffrn_orient_matrix_ub_13 0.236774E-1 _diffrn_orient_matrix_ub_21 -0.236799E-1 _diffrn_orient_matrix_ub_22 -0.929E-4 _diffrn_orient_matrix_ub_23 0.33844E-1 _diffrn_orient_matrix_ub_31 -0.3438E-3 _diffrn_orient_matrix_ub_32 -0.413028E-1 _diffrn_orient_matrix_ub_33 -0.3539E-3 _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 0.0715 _diffrn_reflns_av_unetI/netI 0.0251 _diffrn_reflns_number 69186 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 4175 _reflns_number_gt 3287 _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 thf groups. All the thf C atoms were left isotropic and O-C and C-C SADI constraints were 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^)+(0.0910P)^2^+30.6215P] 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 4175 _refine_ls_number_parameters 231 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1798 _refine_ls_wR_factor_gt 0.1631 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.967 _refine_diff_density_min -0.54 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # 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' Zn Zn 0.2839 1.4301 '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' Cl Cl 0.1484 0.1585 '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 Zn Zn 0.81889(2) 0.42022(2) 0.13520(2) 0.0391(2) Uani 1 1 d . . . Cl Cl 0.82267(4) 0.32267(4) 0.17733(4) 0.0408(4) Uani 1 3 d S . . Li Li 0.7259(6) 0.2259(6) 0.2741(6) 0.094(6) Uani 1 3 d S A . O2 O 0.6973(2) 0.2142(2) 0.2021(2) 0.1006(16) Uani 1 1 d D . . O3 O 0.6792(3) 0.1792(3) 0.3208(3) 0.120(3) Uani 1 3 d SD . . N1 N 0.82261(14) 0.38543(15) 0.05775(15) 0.0395(8) Uani 1 1 d . . . N2 N 0.74029(15) 0.42793(15) 0.12595(16) 0.0428(9) Uani 1 1 d . . . C1 C 0.76558(19) 0.36790(18) 0.0506(2) 0.0453(11) Uani 1 1 d . . . C2 C 0.72434(19) 0.39049(18) 0.0863(2) 0.0459(11) Uani 1 1 d . . . C3 C 0.6698(2) 0.3706(2) 0.0780(2) 0.0590(14) Uani 1 1 d . . . H3 H 0.6406 0.3848 0.1001 0.071 Uiso 1 1 calc R . . C4 C 0.6582(3) 0.3312(3) 0.0388(3) 0.0738(18) Uani 1 1 d . . . H4 H 0.6213 0.3186 0.0351 0.089 Uiso 1 1 calc R . . C5 C 0.6978(3) 0.3097(3) 0.0051(3) 0.0746(18) Uani 1 1 d . . . H5 H 0.6889 0.2828 -0.0221 0.09 Uiso 1 1 calc R . . C6 C 0.7521(2) 0.3284(2) 0.0119(2) 0.0586(13) Uani 1 1 d . . . H6 H 0.7804 0.3134 -0.0108 0.07 Uiso 1 1 calc R . . C7 C 0.8478(2) 0.41317(19) 0.0088(2) 0.0477(11) Uani 1 1 d . . . H7A H 0.8461 0.3867 -0.0223 0.057 Uiso 1 1 calc R . . H7B H 0.8874 0.419 0.0172 0.057 Uiso 1 1 calc R . . C8 C 0.8245(2) 0.4690(2) -0.0125(2) 0.0523(12) Uani 1 1 d . . . C9 C 0.7670(3) 0.4637(3) -0.0363(3) 0.090(2) Uani 1 1 d . . . H9A H 0.7667 0.4349 -0.0648 0.135 Uiso 1 1 calc R . . H9B H 0.7559 0.499 -0.0527 0.135 Uiso 1 1 calc R . . H9C H 0.741 0.4538 -0.0069 0.135 Uiso 1 1 calc R . . C10 C 0.8638(3) 0.4870(3) -0.0591(3) 0.084(2) Uani 1 1 d . . . H10A H 0.9014 0.4905 -0.0445 0.127 Uiso 1 1 calc R . . H10B H 0.8516 0.5227 -0.0739 0.127 Uiso 1 1 calc R . . H10C H 0.8633 0.4593 -0.0887 0.127 Uiso 1 1 calc R . . C11 C 0.8252(3) 0.5134(2) 0.0319(2) 0.0689(16) Uani 1 1 d . . . H11A H 0.8625 0.5166 0.0472 0.103 Uiso 1 1 calc R . . H11B H 0.7993 0.5035 0.0614 0.103 Uiso 1 1 calc R . . H11C H 0.8142 0.5489 0.0157 0.103 Uiso 1 1 calc R . . C12 C 0.70107(19) 0.44620(19) 0.1677(2) 0.0508(12) Uani 1 1 d . . . H12A H 0.7207 0.4486 0.2034 0.061 Uiso 1 1 calc R . . H12B H 0.6722 0.4175 0.1715 0.061 Uiso 1 1 calc R . . C13 C 0.6720(2) 0.5024(2) 0.1569(3) 0.0618(14) Uani 1 1 d . . . C14 C 0.6417(3) 0.5028(3) 0.1020(3) 0.087(2) Uani 1 1 d . . . H14A H 0.6141 0.4732 0.1015 0.13 Uiso 1 1 calc R . . H14B H 0.6682 0.4971 0.0719 0.13 Uiso 1 1 calc R . . H14C H 0.6233 0.5385 0.0971 0.13 Uiso 1 1 calc R . . C15 C 0.7143(3) 0.5486(2) 0.1572(3) 0.0784(19) Uani 1 1 d . . . H15A H 0.7338 0.5489 0.1927 0.118 Uiso 1 1 calc R . . H15B H 0.6956 0.5841 0.1519 0.118 Uiso 1 1 calc R . . H15C H 0.7409 0.5428 0.1273 0.118 Uiso 1 1 calc R . . C16 C 0.6308(3) 0.5117(3) 0.2035(3) 0.093(2) Uani 1 1 d . . . H16A H 0.6035 0.4818 0.2036 0.139 Uiso 1 1 calc R . . H16B H 0.612 0.5471 0.1981 0.139 Uiso 1 1 calc R . . H16C H 0.6504 0.5121 0.239 0.139 Uiso 1 1 calc R . . C21 C 0.6991(8) 0.1437(9) 0.3640(9) 0.197(9) Uiso 0.67 1 d PD A . H21A H 0.7174 0.166 0.393 0.236 Uiso 0.67 1 calc PR . . H21B H 0.7264 0.1173 0.3489 0.236 Uiso 0.67 1 calc PR . . C22 C 0.6522(5) 0.1132(6) 0.3881(7) 0.120(4) Uiso 0.67 1 d PD . . H22A H 0.6423 0.0806 0.3654 0.144 Uiso 0.67 1 calc PR A . H22B H 0.6602 0.1011 0.4263 0.144 Uiso 0.67 1 calc PR . . C17 C 0.7113(16) 0.1639(14) 0.1743(17) 0.33(2) Uiso 0.540(12) 1 d PD A 1 H17A H 0.7119 0.1328 0.2008 0.395 Uiso 0.540(12) 1 calc PR A 1 H17B H 0.7484 0.167 0.1573 0.395 Uiso 0.540(12) 1 calc PR A 1 C18 C 0.6683(9) 0.1539(7) 0.1303(9) 0.128(7) Uiso 0.540(12) 1 d PD A 1 H18A H 0.6817 0.1286 0.1011 0.154 Uiso 0.540(12) 1 calc PR A 1 H18B H 0.6333 0.1396 0.146 0.154 Uiso 0.540(12) 1 calc PR A 1 C19 C 0.6629(9) 0.2112(6) 0.1106(7) 0.120(6) Uiso 0.540(12) 1 d PD A 1 H19A H 0.6243 0.219 0.0995 0.144 Uiso 0.540(12) 1 calc PR A 1 H19B H 0.6874 0.2177 0.0784 0.144 Uiso 0.540(12) 1 calc PR A 1 C20 C 0.6796(8) 0.2473(7) 0.1583(7) 0.126(7) Uiso 0.540(12) 1 d PD A 1 H20A H 0.7098 0.2724 0.1468 0.151 Uiso 0.540(12) 1 calc PR A 1 H20B H 0.6478 0.2702 0.1702 0.151 Uiso 0.540(12) 1 calc PR A 1 C17A C 0.6536(10) 0.1721(9) 0.1915(9) 0.144(9) Uiso 0.460(12) 1 d PD A 2 H17C H 0.6232 0.1745 0.2187 0.173 Uiso 0.460(12) 1 calc PR A 2 H17D H 0.6688 0.1341 0.1914 0.173 Uiso 0.460(12) 1 calc PR A 2 C18A C 0.6353(7) 0.1899(9) 0.1346(7) 0.104(6) Uiso 0.460(12) 1 d PD A 2 H18C H 0.6071 0.1651 0.1183 0.125 Uiso 0.460(12) 1 calc PR A 2 H18D H 0.6227 0.2288 0.1332 0.125 Uiso 0.460(12) 1 calc PR A 2 C19A C 0.6914(5) 0.1817(6) 0.1108(5) 0.066(4) Uiso 0.460(12) 1 d PD A 2 H19C H 0.7024 0.1423 0.1114 0.08 Uiso 0.460(12) 1 calc PR A 2 H19D H 0.6937 0.1959 0.0725 0.08 Uiso 0.460(12) 1 calc PR A 2 C20A C 0.7248(7) 0.2150(7) 0.1491(6) 0.095(5) Uiso 0.460(12) 1 d PD A 2 H20C H 0.7624 0.1991 0.1525 0.114 Uiso 0.460(12) 1 calc PR A 2 H20D H 0.7281 0.2533 0.1354 0.114 Uiso 0.460(12) 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 Zn 0.0343(3) 0.0364(3) 0.0465(3) -0.0034(2) -0.0031(2) -0.0002(2) Cl 0.0408(4) 0.0408(4) 0.0408(4) -0.0009(4) -0.0009(4) 0.0009(4) Li 0.094(6) 0.094(6) 0.094(6) -0.019(8) -0.019(8) 0.019(8) O2 0.112(4) 0.112(4) 0.077(3) -0.024(3) -0.018(3) 0.036(3) O3 0.120(3) 0.120(3) 0.120(3) -0.002(4) -0.002(4) 0.002(4) N1 0.042(2) 0.0364(19) 0.041(2) 0.0033(16) -0.0062(16) -0.0013(16) N2 0.0337(19) 0.038(2) 0.057(2) 0.0038(17) -0.0007(17) 0.0004(15) C1 0.049(3) 0.038(2) 0.049(3) 0.009(2) -0.016(2) -0.001(2) C2 0.042(2) 0.038(2) 0.057(3) 0.014(2) -0.012(2) -0.004(2) C3 0.045(3) 0.061(3) 0.071(4) 0.013(3) -0.012(3) -0.008(2) C4 0.062(4) 0.073(4) 0.086(4) 0.012(3) -0.032(3) -0.030(3) C5 0.077(4) 0.074(4) 0.073(4) -0.008(3) -0.027(4) -0.021(3) C6 0.070(3) 0.050(3) 0.056(3) 0.001(2) -0.020(3) -0.001(3) C7 0.054(3) 0.044(3) 0.045(3) 0.004(2) 0.000(2) 0.006(2) C8 0.059(3) 0.047(3) 0.051(3) 0.013(2) -0.009(2) -0.001(2) C9 0.094(5) 0.068(4) 0.107(5) 0.038(4) -0.046(4) -0.004(3) C10 0.111(5) 0.066(4) 0.077(4) 0.029(3) 0.023(4) -0.001(4) C11 0.100(5) 0.040(3) 0.067(4) 0.009(3) -0.008(3) 0.009(3) C12 0.040(2) 0.042(3) 0.071(3) 0.007(2) 0.002(2) 0.000(2) C13 0.044(3) 0.052(3) 0.090(4) 0.007(3) 0.007(3) 0.012(2) C14 0.073(4) 0.066(4) 0.121(6) 0.022(4) -0.023(4) 0.020(3) C15 0.064(4) 0.041(3) 0.130(6) 0.006(3) 0.008(4) 0.011(3) C16 0.067(4) 0.081(5) 0.131(6) 0.000(4) 0.030(4) 0.023(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 Zn N2 1.925(4) . ? Zn N1 1.981(4) 7_556 ? Zn N1 2.057(4) . ? Zn Cl 2.5742(15) . ? Li O2 1.897(8) . ? Li O3 1.96(3) . ? O2 C20 1.395(14) . ? O2 C17 1.433(17) . ? O2 C20A 1.445(13) . ? O2 C17A 1.492(15) . ? O3 C21 1.437(14) . ? O3 C21 1.437(14) 10_645 ? O3 C21 1.437(14) 7_556 ? N1 C1 1.455(6) . ? N1 C7 1.493(6) . ? N1 Zn 1.981(4) 10_645 ? N2 C2 1.375(6) . ? N2 C12 1.455(6) . ? C1 C6 1.377(7) . ? C1 C2 1.431(7) . ? C2 C3 1.421(7) . ? C3 C4 1.373(8) . ? C4 C5 1.363(10) . ? C5 C6 1.400(8) . ? C7 C8 1.551(6) . ? C8 C9 1.513(8) . ? C8 C11 1.522(8) . ? C8 C10 1.540(8) . ? C12 C13 1.553(7) . ? C13 C15 1.518(8) . ? C13 C14 1.518(9) . ? C13 C16 1.523(9) . ? C21 C22 1.473(14) . ? C22 C22 1.36(2) 10_645 ? C17 C18 1.508(17) . ? C18 C19 1.474(15) . ? C19 C20 1.505(14) . ? C17A C18A 1.510(16) . ? C18A C19A 1.489(14) . ? C19A C20A 1.471(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 Zn N1 146.91(16) . 7_556 ? N2 Zn N1 88.69(15) . . ? N1 Zn N1 123.00(19) 7_556 . ? N2 Zn Cl 99.80(11) . . ? N1 Zn Cl 90.79(11) 7_556 . ? N1 Zn Cl 89.08(10) . . ? Zn Cl Zn 71.53(5) 7_556 . ? O2 Li O2 114.7(6) . 7_556 ? O2 Li O3 103.5(8) . . ? C20 O2 C17 101.8(19) . . ? C20A O2 C17A 100.6(12) . . ? C20 O2 Li 136.4(9) . . ? C17 O2 Li 118.2(14) . . ? C20A O2 Li 130.1(10) . . ? C17A O2 Li 121.2(12) . . ? C21 O3 C21 90.5(12) . 7_556 ? C21 O3 Li 124.9(8) . . ? C1 N1 C7 115.1(4) . . ? C1 N1 Zn 106.5(3) . 10_645 ? C7 N1 Zn 111.7(3) . 10_645 ? C1 N1 Zn 100.8(3) . . ? C7 N1 Zn 123.9(3) . . ? Zn N1 Zn 96.33(15) 10_645 . ? C2 N2 C12 120.1(4) . . ? C2 N2 Zn 107.1(3) . . ? C12 N2 Zn 126.4(3) . . ? C6 C1 C2 120.8(5) . . ? C6 C1 N1 120.6(5) . . ? C2 C1 N1 118.6(4) . . ? N2 C2 C3 125.7(5) . . ? N2 C2 C1 118.6(4) . . ? C3 C2 C1 115.7(5) . . ? C4 C3 C2 121.5(6) . . ? C5 C4 C3 122.4(5) . . ? C4 C5 C6 117.8(6) . . ? C1 C6 C5 121.8(6) . . ? N1 C7 C8 120.4(4) . . ? C9 C8 C11 109.8(5) . . ? C9 C8 C10 108.2(5) . . ? C11 C8 C10 108.1(5) . . ? C9 C8 C7 112.8(4) . . ? C11 C8 C7 112.2(4) . . ? C10 C8 C7 105.4(4) . . ? N2 C12 C13 116.5(4) . . ? C15 C13 C14 108.9(6) . . ? C15 C13 C16 109.2(6) . . ? C14 C13 C16 109.4(5) . . ? C15 C13 C12 109.8(4) . . ? C14 C13 C12 111.8(5) . . ? C16 C13 C12 107.6(5) . . ? O3 C21 C22 109.2(15) . . ? C22 C22 C21 101.3(11) 10_645 . ? O2 C17 C18 107.7(18) . . ? C19 C18 C17 98(2) . . ? C18 C19 C20 105.9(15) . . ? O2 C20 C19 109.4(13) . . ? O2 C17A C18A 99.7(13) . . ? C19A C18A C17A 92.7(15) . . ? C20A C19A C18A 100.6(12) . . ? O2 C20A C19A 107.4(11) . . ? #===END data_(3)-oct1703 _database_code_depnum_ccdc_archive 'CCDC 284206' _audit_creation_date 2003-12-19T16:40:52-00:00 _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_name_systematic ; ? ; _chemical_formula_moiety 'C48 H84 Li1 N4 O4 Zn1' _chemical_formula_sum 'C48 H84 Li1 N4 O4 Zn1' _chemical_formula_weight 853.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnn _symmetry_space_group_name_Hall '-P 2ab 2bc' _symmetry_Int_Tables_number 48 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y, z-1/2' _cell_length_a 11.2835(2) _cell_length_b 14.1788(3) _cell_length_c 15.7345(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2517.31(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14232 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 930 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.53 _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 0.8495 _exptl_absorpt_correction_T_max 0.9803 #----------------------------------------------------------------------------# # 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 -0.98217E-2 _diffrn_orient_matrix_ub_12 0.247974E-1 _diffrn_orient_matrix_ub_13 -0.590784E-1 _diffrn_orient_matrix_ub_21 -0.756798E-1 _diffrn_orient_matrix_ub_22 -0.361242E-1 _diffrn_orient_matrix_ub_23 -0.58424E-2 _diffrn_orient_matrix_ub_31 -0.450609E-1 _diffrn_orient_matrix_ub_32 0.552657E-1 _diffrn_orient_matrix_ub_33 0.226893E-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 0.0604 _diffrn_reflns_av_unetI/netI 0.027 _diffrn_reflns_number 22071 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 25.09 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 2228 _reflns_number_gt 1924 _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^)+(0.0853P)^2^+4.3597P] 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 2228 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 0.822 _refine_ls_restrained_S_all 0.822 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.285 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # 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' Zn Zn 0.2839 1.4301 '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 Zn Zn 0.25 0.75 0.75 0.0266(2) Uani 1 4 d S . . Li Li 0.25 0.75 0.25 0.039(2) Uani 1 4 d S . . O O 0.15505(18) 0.82809(14) 0.32292(13) 0.0479(5) Uani 1 1 d . . . N N 0.18644(19) 0.64544(14) 0.67848(13) 0.0321(5) Uani 1 1 d . . . C1 C 0.2171(2) 0.55982(17) 0.71001(17) 0.0310(5) Uani 1 1 d . . . C2 C 0.1911(3) 0.47174(19) 0.6729(2) 0.0426(7) Uani 1 1 d . . . H2 H 0.1512 0.4703 0.6197 0.051 Uiso 1 1 calc R . . C3 C 0.2216(3) 0.3874(2) 0.7112(2) 0.0516(8) Uani 1 1 d . . . H3 H 0.2034 0.3294 0.684 0.062 Uiso 1 1 calc R . . C4 C 0.1340(3) 0.6532(2) 0.59450(17) 0.0432(7) Uani 1 1 d . . . H4A H 0.1454 0.5924 0.5647 0.052 Uiso 1 1 calc R . . H4B H 0.1784 0.7018 0.5623 0.052 Uiso 1 1 calc R . . C5 C 0.0016(3) 0.6785(2) 0.5912(2) 0.0496(8) Uani 1 1 d . . . C6 C -0.0168(4) 0.7783(2) 0.6248(2) 0.0665(10) Uani 1 1 d . . . H6A H 0.0291 0.8228 0.5902 0.1 Uiso 1 1 calc R . . H6B H 0.0099 0.7817 0.684 0.1 Uiso 1 1 calc R . . H6C H -0.1011 0.7946 0.6217 0.1 Uiso 1 1 calc R . . C7 C -0.0345(4) 0.6749(3) 0.4972(3) 0.0831(13) Uani 1 1 d . . . H7A H 0.0121 0.721 0.465 0.125 Uiso 1 1 calc R . . H7B H -0.119 0.6899 0.4918 0.125 Uiso 1 1 calc R . . H7C H -0.0198 0.6115 0.4747 0.125 Uiso 1 1 calc R . . C8 C -0.0698(3) 0.6078(3) 0.6436(3) 0.0696(11) Uani 1 1 d . . . H8A H -0.0566 0.5441 0.6216 0.104 Uiso 1 1 calc R . . H8B H -0.1543 0.6233 0.6399 0.104 Uiso 1 1 calc R . . H8C H -0.0443 0.6108 0.7031 0.104 Uiso 1 1 calc R . . C9 C 0.0370(3) 0.8623(2) 0.3070(2) 0.0562(8) Uani 1 1 d . . . H9A H -0.0216 0.811 0.314 0.067 Uiso 1 1 calc R . . H9B H 0.0307 0.8874 0.2484 0.067 Uiso 1 1 calc R . . C10 C 0.0153(4) 0.9389(3) 0.3707(3) 0.0783(12) Uani 1 1 d . . . H10A H -0.0227 0.9941 0.3433 0.094 Uiso 1 1 calc R . . H10B H -0.0366 0.9162 0.4171 0.094 Uiso 1 1 calc R . . C11 C 0.1315(4) 0.9636(4) 0.4032(4) 0.113(2) Uani 1 1 d . . . H11A H 0.1608 1.0217 0.3752 0.136 Uiso 1 1 calc R . . H11B H 0.1276 0.975 0.4652 0.136 Uiso 1 1 calc R . . C12 C 0.2098(4) 0.8857(3) 0.3852(3) 0.0844(14) Uani 1 1 d . . . H12A H 0.2868 0.9094 0.3638 0.101 Uiso 1 1 calc R . . H12B H 0.2244 0.8488 0.4376 0.101 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 Zn 0.0344(3) 0.0178(3) 0.0276(3) 0 0 0 Li 0.038(5) 0.034(5) 0.045(5) 0 0 0 O 0.0430(11) 0.0495(12) 0.0510(12) -0.0143(9) -0.0099(9) 0.0137(9) N 0.0394(12) 0.0270(11) 0.0299(10) -0.0009(9) 0.0002(9) -0.0016(9) C1 0.0283(12) 0.0249(12) 0.0398(13) -0.0018(11) 0.0056(10) -0.0021(9) C2 0.0399(15) 0.0297(14) 0.0581(18) -0.0073(13) -0.0032(13) -0.0044(12) C3 0.0413(17) 0.0247(14) 0.089(2) -0.0086(15) -0.0013(15) -0.0036(11) C4 0.0569(18) 0.0376(15) 0.0351(14) -0.0029(12) -0.0058(13) -0.0101(13) C5 0.0567(19) 0.0401(16) 0.0521(17) -0.0050(14) -0.0188(15) -0.0025(14) C6 0.084(3) 0.0474(19) 0.068(2) -0.0076(17) -0.025(2) 0.0201(18) C7 0.103(3) 0.071(2) 0.075(3) -0.014(2) -0.049(2) 0.009(2) C8 0.0432(19) 0.060(2) 0.105(3) -0.003(2) -0.0065(19) -0.0048(16) C9 0.0484(18) 0.059(2) 0.061(2) -0.0089(16) -0.0098(15) 0.0146(15) C10 0.068(2) 0.064(2) 0.103(3) -0.027(2) -0.007(2) 0.0238(19) C11 0.068(3) 0.089(3) 0.183(5) -0.082(4) -0.015(3) 0.018(2) C12 0.063(2) 0.094(3) 0.096(3) -0.052(3) -0.025(2) 0.014(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 Zn N 1.995(2) . ? Zn N 1.995(2) 3_566 ? Zn N 1.995(2) 2_565 ? Zn N 1.995(2) 4_556 ? Li O 1.9210(19) 3_565 ? Li O 1.9210(19) . ? Li O 1.9210(19) 4 ? Li O 1.9210(19) 2_565 ? O C12 1.418(4) . ? O C9 1.440(4) . ? N C1 1.356(3) . ? N C4 1.452(3) . ? C1 C2 1.409(4) . ? C1 C1 1.461(5) 4_556 ? C2 C3 1.382(4) . ? C3 C3 1.380(7) 4_556 ? C4 C5 1.538(4) . ? C5 C8 1.527(5) . ? C5 C6 1.526(4) . ? C5 C7 1.535(5) . ? C9 C10 1.498(5) . ? C10 C11 1.451(6) . ? C11 C12 1.442(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Zn N 137.85(12) . 3_566 ? N Zn N 111.31(12) . 2_565 ? N Zn N 83.98(12) 3_566 2_565 ? N Zn N 83.98(12) . 4_556 ? N Zn N 111.31(12) 3_566 4_556 ? N Zn N 137.85(12) 2_565 4_556 ? O Li O 112.20(12) 3_565 . ? O Li O 106.65(12) 3_565 4 ? O Li O 109.61(13) . 4 ? O Li O 109.61(13) 3_565 2_565 ? O Li O 106.65(12) . 2_565 ? O Li O 112.20(12) 4 2_565 ? C12 O C9 109.2(2) . . ? C12 O Li 120.1(2) . . ? C9 O Li 127.33(18) . . ? C1 N C4 120.3(2) . . ? C1 N Zn 111.54(16) . . ? C4 N Zn 127.10(17) . . ? N C1 C2 126.1(2) . . ? N C1 C1 116.40(14) . 4_556 ? C2 C1 C1 117.54(16) . 4_556 ? C3 C2 C1 122.3(3) . . ? C3 C3 C2 120.07(18) 4_556 . ? N C4 C5 116.4(2) . . ? C8 C5 C6 110.5(3) . . ? C8 C5 C7 111.1(3) . . ? C6 C5 C7 109.2(3) . . ? C8 C5 C4 110.0(3) . . ? C6 C5 C4 109.6(3) . . ? C7 C5 C4 106.4(3) . . ? O C9 C10 106.2(3) . . ? C11 C10 C9 105.3(3) . . ? C12 C11 C10 107.4(3) . . ? O C12 C11 108.1(3) . . ? #===END data_(5)-oct1303 _database_code_depnum_ccdc_archive 'CCDC 284207' _audit_creation_date 2003-10-15T10:05:10-00:00 _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 ; '[(LH)Zn(L)Zn(L)Li(OEt2)]' ; _chemical_formula_moiety 'C52 H89 Li1 N6 O1 Zn2' _chemical_formula_sum 'C52 H89 Li1 N6 O1 Zn2' _chemical_formula_weight 951.97 _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 11.9582(3) _cell_length_b 14.8108(5) _cell_length_c 16.8878(5) _cell_angle_alpha 85.507(2) _cell_angle_beta 77.579(2) _cell_angle_gamma 68.404(1) _cell_volume 2715.95(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19802 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.922 _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 0.755 _exptl_absorpt_correction_T_max 0.955 #----------------------------------------------------------------------------# # 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 0.511444E-1 _diffrn_orient_matrix_ub_12 0.15307E-1 _diffrn_orient_matrix_ub_13 0.328106E-1 _diffrn_orient_matrix_ub_21 0.205612E-1 _diffrn_orient_matrix_ub_22 -0.66514E-1 _diffrn_orient_matrix_ub_23 0.24216E-1 _diffrn_orient_matrix_ub_31 0.734212E-1 _diffrn_orient_matrix_ub_32 -0.24792E-1 _diffrn_orient_matrix_ub_33 -0.448717E-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 0.1154 _diffrn_reflns_av_unetI/netI 0.0962 _diffrn_reflns_number 20961 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 23.01 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 7472 _reflns_number_gt 5622 _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 hydrogen atom on N6 was located on a difference map and refined isotropic; other hydrogens were in riding mode. 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^)+(0.0654P)^2^+4.1353P] 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 7472 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.792 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.079 #----------------------------------------------------------------------------# # 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' Zn Zn 0.2839 1.4301 '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 Zn1 Zn 0.44137(5) 0.29664(4) 0.23168(3) 0.02998(19) Uani 1 1 d . . . Zn2 Zn 0.65345(5) 0.12677(4) 0.25570(3) 0.02948(19) Uani 1 1 d . . . Li Li 0.3088(9) 0.4836(7) 0.2927(6) 0.050(2) Uani 1 1 d . . . O1 O 0.2322(4) 0.6103(3) 0.3365(3) 0.0581(11) Uani 1 1 d . . . N1 N 0.4902(4) 0.2087(3) 0.3308(2) 0.0293(9) Uani 1 1 d . . . N2 N 0.5259(3) 0.1519(3) 0.1848(2) 0.0264(9) Uani 1 1 d . . . N3 N 0.4600(4) 0.4219(3) 0.1967(3) 0.0335(10) Uani 1 1 d . . . N4 N 0.2610(4) 0.3785(3) 0.2459(2) 0.0333(10) Uani 1 1 d . . . N5 N 0.8269(3) 0.1012(3) 0.2414(2) 0.0326(10) Uani 1 1 d . . . N6 N 0.7119(4) -0.0244(3) 0.2929(3) 0.0324(10) Uani 1 1 d . . . H6N H 0.656(5) -0.040(4) 0.326(3) 0.037(15) Uiso 1 1 d . . . C1 C 0.4234(4) 0.1477(3) 0.3223(3) 0.0274(11) Uani 1 1 d . . . C2 C 0.4417(4) 0.1182(3) 0.2404(3) 0.0268(11) Uani 1 1 d . . . C3 C 0.3797(4) 0.0613(4) 0.2241(3) 0.0323(12) Uani 1 1 d . . . H3 H 0.3918 0.04 0.1702 0.039 Uiso 1 1 calc R . . C4 C 0.2997(4) 0.0349(4) 0.2860(3) 0.0386(13) Uani 1 1 d . . . H4 H 0.2572 -0.0035 0.2738 0.046 Uiso 1 1 calc R . . C5 C 0.2818(5) 0.0638(4) 0.3642(3) 0.0370(13) Uani 1 1 d . . . H5 H 0.2266 0.0458 0.4059 0.044 Uiso 1 1 calc R . . C6 C 0.3443(4) 0.1196(4) 0.3828(3) 0.0347(12) Uani 1 1 d . . . H6 H 0.3327 0.1385 0.4373 0.042 Uiso 1 1 calc R . . C7 C 0.4606(5) 0.2590(4) 0.4088(3) 0.0330(12) Uani 1 1 d . . . H7A H 0.3757 0.2651 0.4349 0.04 Uiso 1 1 calc R . . H7B H 0.4596 0.3257 0.3963 0.04 Uiso 1 1 calc R . . C8 C 0.5404(5) 0.2174(4) 0.4717(3) 0.0380(13) Uani 1 1 d . . . C9 C 0.6714(5) 0.2145(5) 0.4396(3) 0.0475(15) Uani 1 1 d . . . H9A H 0.7207 0.187 0.4811 0.071 Uiso 1 1 calc R . . H9B H 0.6698 0.2806 0.4265 0.071 Uiso 1 1 calc R . . H9C H 0.7076 0.1742 0.3907 0.071 Uiso 1 1 calc R . . C10 C 0.5432(6) 0.1164(4) 0.4989(4) 0.0537(16) Uani 1 1 d . . . H10A H 0.5957 0.092 0.539 0.081 Uiso 1 1 calc R . . H10B H 0.576 0.0727 0.4519 0.081 Uiso 1 1 calc R . . H10C H 0.4598 0.1194 0.5232 0.081 Uiso 1 1 calc R . . C11 C 0.4829(5) 0.2866(5) 0.5451(3) 0.0483(15) Uani 1 1 d . . . H11A H 0.5314 0.2624 0.5875 0.072 Uiso 1 1 calc R . . H11B H 0.3986 0.2897 0.5663 0.072 Uiso 1 1 calc R . . H11C H 0.4823 0.3516 0.5283 0.072 Uiso 1 1 calc R . . C12 C 0.5602(4) 0.1178(4) 0.1002(3) 0.0303(11) Uani 1 1 d . . . H12A H 0.5473 0.0554 0.1003 0.036 Uiso 1 1 calc R . . H12B H 0.6494 0.1035 0.0817 0.036 Uiso 1 1 calc R . . C13 C 0.4952(5) 0.1833(4) 0.0363(3) 0.0326(12) Uani 1 1 d . . . C14 C 0.3563(5) 0.2134(5) 0.0601(3) 0.0464(14) Uani 1 1 d . . . H14A H 0.3185 0.2555 0.018 0.07 Uiso 1 1 calc R . . H14B H 0.3268 0.2486 0.1117 0.07 Uiso 1 1 calc R . . H14C H 0.3342 0.1554 0.0659 0.07 Uiso 1 1 calc R . . C15 C 0.5302(6) 0.2741(4) 0.0224(3) 0.0500(15) Uani 1 1 d . . . H15A H 0.4879 0.3157 -0.0183 0.075 Uiso 1 1 calc R . . H15B H 0.6192 0.2545 0.0031 0.075 Uiso 1 1 calc R . . H15C H 0.5059 0.31 0.0734 0.075 Uiso 1 1 calc R . . C16 C 0.5413(5) 0.1268(4) -0.0433(3) 0.0463(14) Uani 1 1 d . . . H16A H 0.5014 0.1671 -0.0855 0.069 Uiso 1 1 calc R . . H16B H 0.5217 0.0676 -0.036 0.069 Uiso 1 1 calc R . . H16C H 0.6304 0.1093 -0.0597 0.069 Uiso 1 1 calc R . . C17 C 0.3610(5) 0.4733(4) 0.1573(3) 0.0369(13) Uani 1 1 d . . . C18 C 0.2530(4) 0.4475(4) 0.1837(3) 0.0320(12) Uani 1 1 d . . . C19 C 0.1542(5) 0.4930(4) 0.1451(3) 0.0411(13) Uani 1 1 d . . . H19 H 0.0835 0.4757 0.1601 0.049 Uiso 1 1 calc R . . C20 C 0.1563(6) 0.5629(5) 0.0852(4) 0.0524(16) Uani 1 1 d . . . H20 H 0.0876 0.5928 0.0601 0.063 Uiso 1 1 calc R . . C21 C 0.2571(6) 0.5881(4) 0.0629(3) 0.0517(16) Uani 1 1 d . . . H21 H 0.2576 0.6367 0.0228 0.062 Uiso 1 1 calc R . . C22 C 0.3592(5) 0.5442(4) 0.0977(3) 0.0433(14) Uani 1 1 d . . . H22 H 0.4287 0.5627 0.0808 0.052 Uiso 1 1 calc R . . C23 C 0.5790(5) 0.4304(4) 0.1633(3) 0.0395(13) Uani 1 1 d . . . H23A H 0.5764 0.4595 0.1087 0.047 Uiso 1 1 calc R . . H23B H 0.6418 0.364 0.1564 0.047 Uiso 1 1 calc R . . C24 C 0.6225(5) 0.4901(4) 0.2123(3) 0.0429(14) Uani 1 1 d . . . C25 C 0.5314(6) 0.5943(4) 0.2226(4) 0.0587(17) Uani 1 1 d . . . H25A H 0.5223 0.6235 0.1692 0.088 Uiso 1 1 calc R . . H25B H 0.5617 0.6318 0.2523 0.088 Uiso 1 1 calc R . . H25C H 0.4517 0.5947 0.2531 0.088 Uiso 1 1 calc R . . C26 C 0.7474(6) 0.4899(5) 0.1653(4) 0.0601(18) Uani 1 1 d . . . H26A H 0.7387 0.5193 0.1119 0.09 Uiso 1 1 calc R . . H26B H 0.8061 0.423 0.1586 0.09 Uiso 1 1 calc R . . H26C H 0.7772 0.5274 0.1953 0.09 Uiso 1 1 calc R . . C27 C 0.6358(5) 0.4450(5) 0.2949(3) 0.0525(16) Uani 1 1 d . . . H27A H 0.6948 0.3781 0.2884 0.079 Uiso 1 1 calc R . . H27B H 0.556 0.4448 0.3249 0.079 Uiso 1 1 calc R . . H27C H 0.6651 0.4828 0.325 0.079 Uiso 1 1 calc R . . C28 C 0.1630(4) 0.3391(4) 0.2686(3) 0.0363(12) Uani 1 1 d . . . H28A H 0.2013 0.2688 0.2792 0.044 Uiso 1 1 calc R . . H28B H 0.1242 0.3455 0.2213 0.044 Uiso 1 1 calc R . . C29 C 0.0588(5) 0.3849(4) 0.3437(3) 0.0401(13) Uani 1 1 d . . . C30 C -0.0151(5) 0.4936(4) 0.3317(4) 0.0539(16) Uani 1 1 d . . . H30A H -0.0493 0.5015 0.2828 0.081 Uiso 1 1 calc R . . H30B H 0.0393 0.5306 0.326 0.081 Uiso 1 1 calc R . . H30C H -0.082 0.5175 0.3789 0.081 Uiso 1 1 calc R . . C31 C -0.0269(5) 0.3268(5) 0.3525(4) 0.0555(17) Uani 1 1 d . . . H31A H -0.0614 0.3351 0.3036 0.083 Uiso 1 1 calc R . . H31B H -0.0935 0.3505 0.3998 0.083 Uiso 1 1 calc R . . H31C H 0.0199 0.2578 0.3598 0.083 Uiso 1 1 calc R . . C32 C 0.1114(5) 0.3728(5) 0.4195(3) 0.0492(15) Uani 1 1 d . . . H32A H 0.1583 0.304 0.4271 0.074 Uiso 1 1 calc R . . H32B H 0.0443 0.3966 0.4665 0.074 Uiso 1 1 calc R . . H32C H 0.1655 0.41 0.4139 0.074 Uiso 1 1 calc R . . C33 C 0.8753(4) 0.0342(4) 0.2983(3) 0.0336(12) Uani 1 1 d . . . C34 C 0.8136(4) -0.0312(4) 0.3295(3) 0.0296(11) Uani 1 1 d . . . C35 C 0.8432(5) -0.0908(4) 0.3948(3) 0.0411(13) Uani 1 1 d . . . H35 H 0.7971 -0.1306 0.4163 0.049 Uiso 1 1 calc R . . C36 C 0.9407(5) -0.0932(4) 0.4298(3) 0.0479(15) Uani 1 1 d . . . H36 H 0.961 -0.134 0.4749 0.057 Uiso 1 1 calc R . . C37 C 1.0063(5) -0.0347(5) 0.3970(4) 0.0503(16) Uani 1 1 d . . . H37 H 1.0741 -0.037 0.4189 0.06 Uiso 1 1 calc R . . C38 C 0.9754(5) 0.0268(4) 0.3329(3) 0.0444(14) Uani 1 1 d . . . H38 H 1.0232 0.0654 0.3116 0.053 Uiso 1 1 calc R . . C39 C 0.8884(5) 0.1675(4) 0.2068(3) 0.0380(13) Uani 1 1 d . . . H39A H 0.9377 0.1734 0.245 0.046 Uiso 1 1 calc R . . H39B H 0.8252 0.2324 0.2022 0.046 Uiso 1 1 calc R . . C40 C 0.9734(5) 0.1384(4) 0.1228(3) 0.0420(14) Uani 1 1 d . . . C41 C 0.9002(5) 0.1312(5) 0.0615(4) 0.0560(17) Uani 1 1 d . . . H41A H 0.8336 0.1936 0.0584 0.084 Uiso 1 1 calc R . . H41B H 0.8655 0.0806 0.0787 0.084 Uiso 1 1 calc R . . H41C H 0.9544 0.1146 0.0081 0.084 Uiso 1 1 calc R . . C42 C 1.0263(7) 0.2184(6) 0.0967(5) 0.081(2) Uani 1 1 d . . . H42A H 0.9591 0.2807 0.0943 0.122 Uiso 1 1 calc R . . H42B H 1.0802 0.2029 0.0431 0.122 Uiso 1 1 calc R . . H42C H 1.0736 0.2229 0.1361 0.122 Uiso 1 1 calc R . . C43 C 1.0774(5) 0.0411(5) 0.1265(4) 0.0629(19) Uani 1 1 d . . . H43A H 1.1253 0.0453 0.1655 0.094 Uiso 1 1 calc R . . H43B H 1.1307 0.0251 0.0727 0.094 Uiso 1 1 calc R . . H43C H 1.0429 -0.0096 0.1436 0.094 Uiso 1 1 calc R . . C44 C 0.7466(5) -0.0790(4) 0.2148(3) 0.0452(14) Uani 1 1 d . . . H44A H 0.6873 -0.0415 0.1807 0.054 Uiso 1 1 calc R . . H44B H 0.828 -0.0782 0.1868 0.054 Uiso 1 1 calc R . . C45 C 0.7533(6) -0.1816(4) 0.2158(4) 0.0553(17) Uani 1 1 d . . . C46 C 0.6144(13) -0.1727(9) 0.2524(7) 0.167(7) Uani 1 1 d . . . H46A H 0.5596 -0.126 0.2203 0.251 Uiso 1 1 calc R . . H46B H 0.5913 -0.1505 0.3087 0.251 Uiso 1 1 calc R . . H46C H 0.6072 -0.2363 0.2504 0.251 Uiso 1 1 calc R . . C47 C 0.833(2) -0.2481(8) 0.2610(11) 0.319(16) Uani 1 1 d . . . H47A H 0.8152 -0.2229 0.3161 0.478 Uiso 1 1 calc R . . H47B H 0.9178 -0.2579 0.2352 0.478 Uiso 1 1 calc R . . H47C H 0.8201 -0.3102 0.2636 0.478 Uiso 1 1 calc R . . C48 C 0.7754(6) -0.2159(5) 0.1310(4) 0.0617(18) Uani 1 1 d . . . H48A H 0.7175 -0.1677 0.1017 0.093 Uiso 1 1 calc R . . H48B H 0.7635 -0.278 0.132 0.093 Uiso 1 1 calc R . . H48C H 0.8596 -0.2243 0.1035 0.093 Uiso 1 1 calc R . . C49 C 0.1552(7) 0.6864(6) 0.2919(5) 0.079(2) Uani 1 1 d . . . H49A H 0.0738 0.7167 0.3276 0.095 Uiso 1 1 calc R . . H49B H 0.1428 0.657 0.2454 0.095 Uiso 1 1 calc R . . C50 C 0.2056(8) 0.7637(6) 0.2610(6) 0.102(3) Uani 1 1 d . . . H50A H 0.1482 0.8128 0.232 0.152 Uiso 1 1 calc R . . H50B H 0.2848 0.7349 0.2239 0.152 Uiso 1 1 calc R . . H50C H 0.2168 0.7942 0.3066 0.152 Uiso 1 1 calc R . . C51 C 0.2316(7) 0.6398(5) 0.4137(4) 0.068(2) Uani 1 1 d . . . H51A H 0.146 0.6671 0.4445 0.082 Uiso 1 1 calc R . . H51B H 0.2674 0.691 0.4082 0.082 Uiso 1 1 calc R . . C52 C 0.3041(6) 0.5553(5) 0.4585(4) 0.0630(18) Uani 1 1 d . . . H52A H 0.3032 0.5765 0.5122 0.094 Uiso 1 1 calc R . . H52B H 0.389 0.5289 0.4282 0.094 Uiso 1 1 calc R . . H52C H 0.2679 0.505 0.4644 0.094 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 Zn1 0.0282(3) 0.0297(4) 0.0321(3) 0.0001(2) -0.0049(3) -0.0112(3) Zn2 0.0211(3) 0.0358(4) 0.0325(3) -0.0025(3) -0.0043(2) -0.0114(3) Li 0.042(5) 0.051(6) 0.060(6) -0.009(5) -0.003(5) -0.020(5) O1 0.057(3) 0.051(3) 0.063(3) -0.019(2) -0.004(2) -0.015(2) N1 0.032(2) 0.032(2) 0.025(2) -0.0006(18) -0.0089(18) -0.0109(18) N2 0.023(2) 0.026(2) 0.028(2) -0.0038(17) -0.0005(17) -0.0086(17) N3 0.029(2) 0.036(3) 0.039(2) -0.001(2) -0.007(2) -0.0153(19) N4 0.026(2) 0.038(3) 0.034(2) -0.001(2) -0.0013(19) -0.0119(19) N5 0.019(2) 0.039(3) 0.037(2) -0.004(2) 0.0008(18) -0.0100(18) N6 0.026(2) 0.032(3) 0.037(2) -0.0055(19) 0.000(2) -0.011(2) C1 0.018(2) 0.031(3) 0.034(3) -0.001(2) -0.008(2) -0.008(2) C2 0.018(2) 0.028(3) 0.030(3) 0.001(2) -0.005(2) -0.004(2) C3 0.025(3) 0.035(3) 0.039(3) -0.006(2) -0.005(2) -0.012(2) C4 0.028(3) 0.037(3) 0.058(4) 0.001(3) -0.011(3) -0.020(2) C5 0.029(3) 0.044(3) 0.038(3) 0.007(3) -0.006(2) -0.016(2) C6 0.028(3) 0.049(3) 0.028(3) 0.007(2) -0.007(2) -0.014(2) C7 0.035(3) 0.032(3) 0.032(3) -0.002(2) -0.004(2) -0.013(2) C8 0.039(3) 0.039(3) 0.033(3) -0.004(2) -0.006(2) -0.011(2) C9 0.035(3) 0.063(4) 0.043(3) -0.019(3) -0.007(3) -0.013(3) C10 0.073(4) 0.049(4) 0.043(3) 0.008(3) -0.028(3) -0.019(3) C11 0.051(4) 0.062(4) 0.031(3) -0.007(3) -0.009(3) -0.018(3) C12 0.030(3) 0.034(3) 0.029(3) -0.007(2) -0.005(2) -0.013(2) C13 0.035(3) 0.038(3) 0.026(3) 0.001(2) -0.008(2) -0.014(2) C14 0.039(3) 0.061(4) 0.037(3) 0.002(3) -0.014(3) -0.013(3) C15 0.072(4) 0.045(4) 0.038(3) 0.003(3) -0.013(3) -0.026(3) C16 0.053(4) 0.054(4) 0.034(3) -0.007(3) -0.005(3) -0.023(3) C17 0.043(3) 0.031(3) 0.035(3) -0.007(2) -0.005(3) -0.012(2) C18 0.029(3) 0.031(3) 0.031(3) -0.005(2) -0.004(2) -0.006(2) C19 0.033(3) 0.043(3) 0.042(3) 0.003(3) -0.008(3) -0.009(3) C20 0.046(4) 0.058(4) 0.044(3) 0.011(3) -0.017(3) -0.005(3) C21 0.056(4) 0.050(4) 0.040(3) 0.011(3) -0.009(3) -0.011(3) C22 0.048(3) 0.040(3) 0.039(3) 0.006(3) -0.005(3) -0.017(3) C23 0.040(3) 0.036(3) 0.042(3) -0.004(2) -0.003(3) -0.016(3) C24 0.038(3) 0.045(4) 0.049(3) -0.003(3) -0.005(3) -0.022(3) C25 0.074(5) 0.043(4) 0.069(4) -0.006(3) -0.013(4) -0.031(3) C26 0.055(4) 0.076(5) 0.061(4) -0.004(3) 0.000(3) -0.043(4) C27 0.045(3) 0.068(4) 0.047(4) -0.005(3) -0.007(3) -0.023(3) C28 0.024(3) 0.043(3) 0.040(3) -0.003(2) -0.002(2) -0.013(2) C29 0.028(3) 0.047(3) 0.040(3) 0.002(3) -0.002(2) -0.010(2) C30 0.042(3) 0.051(4) 0.053(4) -0.007(3) 0.001(3) -0.003(3) C31 0.034(3) 0.073(5) 0.060(4) -0.010(3) 0.004(3) -0.025(3) C32 0.035(3) 0.061(4) 0.047(3) -0.008(3) 0.000(3) -0.014(3) C33 0.023(3) 0.040(3) 0.036(3) -0.012(2) -0.001(2) -0.009(2) C34 0.020(2) 0.036(3) 0.028(3) -0.004(2) -0.003(2) -0.004(2) C35 0.038(3) 0.038(3) 0.038(3) -0.006(3) -0.001(3) -0.007(2) C36 0.035(3) 0.057(4) 0.038(3) -0.006(3) -0.011(3) 0.003(3) C37 0.029(3) 0.071(4) 0.047(4) -0.016(3) -0.007(3) -0.011(3) C38 0.027(3) 0.060(4) 0.045(3) -0.010(3) -0.002(3) -0.015(3) C39 0.028(3) 0.040(3) 0.046(3) -0.007(3) -0.001(2) -0.015(2) C40 0.028(3) 0.056(4) 0.044(3) -0.008(3) 0.000(2) -0.020(3) C41 0.044(4) 0.074(5) 0.046(4) 0.001(3) -0.009(3) -0.018(3) C42 0.069(5) 0.100(6) 0.078(5) -0.005(4) 0.028(4) -0.057(5) C43 0.035(3) 0.086(5) 0.047(4) -0.012(3) 0.000(3) 0.000(3) C44 0.048(3) 0.053(4) 0.037(3) -0.010(3) -0.003(3) -0.022(3) C45 0.082(5) 0.035(3) 0.052(4) -0.003(3) -0.029(3) -0.014(3) C46 0.233(15) 0.187(13) 0.129(9) -0.080(9) 0.074(10) -0.174(12) C47 0.55(3) 0.052(7) 0.35(2) -0.070(10) -0.39(3) 0.076(12) C48 0.071(5) 0.058(4) 0.061(4) -0.020(3) -0.011(4) -0.026(4) C49 0.079(5) 0.061(5) 0.084(5) -0.012(4) -0.023(4) -0.003(4) C50 0.095(6) 0.059(5) 0.118(7) 0.007(5) -0.004(6) -0.001(5) C51 0.067(5) 0.069(5) 0.064(4) -0.033(4) -0.001(4) -0.018(4) C52 0.057(4) 0.066(5) 0.064(4) -0.023(4) 0.002(3) -0.023(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 Zn1 N3 1.979(4) . ? Zn1 N4 2.019(4) . ? Zn1 N1 2.087(4) . ? Zn1 N2 2.138(4) . ? Zn2 N5 1.929(4) . ? Zn2 N2 2.049(4) . ? Zn2 N1 2.079(4) . ? Zn2 N6 2.171(4) . ? Li O1 1.889(10) . ? Li N4 2.102(11) . ? Li N3 2.118(10) . ? O1 C51 1.404(7) . ? O1 C49 1.445(8) . ? N1 C1 1.442(6) . ? N1 C7 1.475(6) . ? N2 C2 1.426(6) . ? N2 C12 1.474(6) . ? N3 C17 1.421(7) . ? N3 C23 1.461(6) . ? N4 C18 1.400(7) . ? N4 C28 1.461(6) . ? N5 C33 1.382(7) . ? N5 C39 1.451(7) . ? N6 C34 1.447(6) . ? N6 C44 1.499(7) . ? C1 C6 1.385(7) . ? C1 C2 1.430(7) . ? C2 C3 1.386(7) . ? C3 C4 1.393(7) . ? C4 C5 1.368(7) . ? C5 C6 1.391(7) . ? C7 C8 1.523(7) . ? C8 C10 1.521(8) . ? C8 C9 1.530(8) . ? C8 C11 1.540(7) . ? C12 C13 1.533(7) . ? C13 C14 1.521(7) . ? C13 C16 1.527(7) . ? C13 C15 1.536(8) . ? C17 C22 1.394(8) . ? C17 C18 1.450(7) . ? C18 C19 1.397(7) . ? C19 C20 1.392(8) . ? C20 C21 1.360(9) . ? C21 C22 1.387(8) . ? C23 C24 1.541(7) . ? C24 C27 1.513(8) . ? C24 C25 1.524(8) . ? C24 C26 1.533(8) . ? C28 C29 1.566(7) . ? C29 C32 1.515(8) . ? C29 C31 1.540(8) . ? C29 C30 1.547(8) . ? C33 C38 1.408(7) . ? C33 C34 1.428(7) . ? C34 C35 1.382(7) . ? C35 C36 1.404(8) . ? C36 C37 1.383(9) . ? C37 C38 1.381(8) . ? C39 C40 1.545(7) . ? C40 C41 1.525(8) . ? C40 C43 1.525(8) . ? C40 C42 1.533(9) . ? C44 C45 1.492(8) . ? C45 C47 1.399(11) . ? C45 C48 1.494(8) . ? C45 C46 1.603(13) . ? C49 C50 1.492(12) . ? C51 C52 1.491(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 Zn1 N4 82.56(17) . . ? N3 Zn1 N1 130.34(17) . . ? N4 Zn1 N1 114.60(16) . . ? N3 Zn1 N2 134.24(16) . . ? N4 Zn1 N2 125.57(16) . . ? N1 Zn1 N2 74.72(15) . . ? N5 Zn2 N2 138.15(16) . . ? N5 Zn2 N1 138.60(16) . . ? N2 Zn2 N1 76.81(15) . . ? N5 Zn2 N6 81.65(17) . . ? N2 Zn2 N6 109.12(16) . . ? N1 Zn2 N6 110.76(16) . . ? O1 Li N4 139.0(6) . . ? O1 Li N3 132.3(6) . . ? N4 Li N3 77.4(4) . . ? C51 O1 C49 113.2(5) . . ? C51 O1 Li 127.0(5) . . ? C49 O1 Li 119.5(5) . . ? C1 N1 C7 118.0(4) . . ? C1 N1 Zn2 96.0(3) . . ? C7 N1 Zn2 133.8(3) . . ? C1 N1 Zn1 94.8(3) . . ? C7 N1 Zn1 116.2(3) . . ? Zn2 N1 Zn1 88.90(15) . . ? C2 N2 C12 117.8(4) . . ? C2 N2 Zn2 97.7(3) . . ? C12 N2 Zn2 122.1(3) . . ? C2 N2 Zn1 93.1(3) . . ? C12 N2 Zn1 129.6(3) . . ? Zn2 N2 Zn1 88.32(15) . . ? C17 N3 C23 117.9(4) . . ? C17 N3 Zn1 106.2(3) . . ? C23 N3 Zn1 122.9(3) . . ? C17 N3 Li 75.6(4) . . ? C23 N3 Li 137.6(4) . . ? Zn1 N3 Li 85.5(3) . . ? C18 N4 C28 118.4(4) . . ? C18 N4 Zn1 105.2(3) . . ? C28 N4 Zn1 123.8(3) . . ? C18 N4 Li 77.1(4) . . ? C28 N4 Li 136.0(4) . . ? Zn1 N4 Li 85.0(3) . . ? C33 N5 C39 118.9(4) . . ? C33 N5 Zn2 109.7(3) . . ? C39 N5 Zn2 125.9(3) . . ? C34 N6 C44 115.2(4) . . ? C34 N6 Zn2 100.6(3) . . ? C44 N6 Zn2 103.7(3) . . ? C6 C1 C2 119.7(4) . . ? C6 C1 N1 127.3(4) . . ? C2 C1 N1 113.0(4) . . ? C3 C2 N2 128.0(4) . . ? C3 C2 C1 118.5(4) . . ? N2 C2 C1 113.5(4) . . ? C2 C3 C4 120.6(5) . . ? C5 C4 C3 120.8(5) . . ? C4 C5 C6 120.0(5) . . ? C1 C6 C5 120.5(5) . . ? N1 C7 C8 120.3(4) . . ? C10 C8 C7 111.9(4) . . ? C10 C8 C9 109.7(5) . . ? C7 C8 C9 111.2(4) . . ? C10 C8 C11 109.0(5) . . ? C7 C8 C11 106.6(4) . . ? C9 C8 C11 108.3(5) . . ? N2 C12 C13 119.1(4) . . ? C14 C13 C16 109.4(4) . . ? C14 C13 C12 112.2(4) . . ? C16 C13 C12 107.7(4) . . ? C14 C13 C15 109.8(5) . . ? C16 C13 C15 107.6(4) . . ? C12 C13 C15 110.1(4) . . ? C22 C17 N3 126.4(5) . . ? C22 C17 C18 118.8(5) . . ? N3 C17 C18 114.8(4) . . ? C22 C17 Li 131.5(5) . . ? N3 C17 Li 66.4(4) . . ? C18 C17 Li 71.6(4) . . ? C19 C18 N4 127.5(5) . . ? C19 C18 C17 117.4(5) . . ? N4 C18 C17 115.0(4) . . ? C19 C18 Li 134.1(4) . . ? N4 C18 Li 65.6(4) . . ? C17 C18 Li 70.7(4) . . ? C20 C19 C18 122.0(5) . . ? C21 C20 C19 119.6(5) . . ? C20 C21 C22 121.2(5) . . ? C21 C22 C17 120.9(6) . . ? N3 C23 C24 117.3(4) . . ? C27 C24 C25 109.4(5) . . ? C27 C24 C26 109.5(5) . . ? C25 C24 C26 109.3(5) . . ? C27 C24 C23 110.2(5) . . ? C25 C24 C23 110.5(5) . . ? C26 C24 C23 107.9(5) . . ? N4 C28 C29 117.8(4) . . ? C32 C29 C31 109.6(5) . . ? C32 C29 C30 109.3(5) . . ? C31 C29 C30 109.3(5) . . ? C32 C29 C28 110.6(4) . . ? C31 C29 C28 105.1(4) . . ? C30 C29 C28 112.8(4) . . ? N5 C33 C38 127.0(5) . . ? N5 C33 C34 117.2(4) . . ? C38 C33 C34 115.7(5) . . ? C35 C34 C33 121.6(5) . . ? C35 C34 N6 122.5(5) . . ? C33 C34 N6 115.6(4) . . ? C34 C35 C36 120.7(6) . . ? C37 C36 C35 118.3(6) . . ? C38 C37 C36 121.4(5) . . ? C37 C38 C33 122.1(6) . . ? N5 C39 C40 115.4(4) . . ? C41 C40 C43 109.0(5) . . ? C41 C40 C42 109.6(6) . . ? C43 C40 C42 109.9(5) . . ? C41 C40 C39 110.1(4) . . ? C43 C40 C39 111.2(5) . . ? C42 C40 C39 107.0(5) . . ? C45 C44 N6 120.0(5) . . ? C47 C45 C44 117.1(8) . . ? C47 C45 C48 112.1(8) . . ? C44 C45 C48 109.7(5) . . ? C47 C45 C46 110.1(13) . . ? C44 C45 C46 103.1(6) . . ? C48 C45 C46 103.5(6) . . ? O1 C49 C50 114.2(7) . . ? O1 C51 C52 110.0(5) . . ? #===END data_(6)-oct703 _database_code_depnum_ccdc_archive 'CCDC 284208' _audit_creation_date 2003-10-07T10:34:52-00:00 _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_name_systematic ; ? ; _chemical_formula_moiety 'C34 H68 Li2 N4 O3 Si2' _chemical_formula_sum 'C34 H68 Li2 N4 O3 Si2' _chemical_formula_weight 650.98 _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 14.1330(2) _cell_length_b 15.8542(2) _cell_length_c 18.1662(3) _cell_angle_alpha 90 _cell_angle_beta 96.491(1) _cell_angle_gamma 90 _cell_volume 4044.36(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31078 _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 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 -0.105392E-1 _diffrn_orient_matrix_ub_12 -0.33741E-1 _diffrn_orient_matrix_ub_13 0.44863E-1 _diffrn_orient_matrix_ub_21 0.181161E-1 _diffrn_orient_matrix_ub_22 -0.525653E-1 _diffrn_orient_matrix_ub_23 -0.254169E-1 _diffrn_orient_matrix_ub_31 0.680589E-1 _diffrn_orient_matrix_ub_32 0.8767E-2 _diffrn_orient_matrix_ub_33 0.202665E-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 0.0745 _diffrn_reflns_av_unetI/netI 0.0373 _diffrn_reflns_number 39381 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 6991 _reflns_number_gt 6120 _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^)+(0.0905P)^2^+2.4877P] 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 6991 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.064 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.57 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 Li1 Li 0.8888(2) 0.7547(2) 0.1150(2) 0.0482(9) Uani 1 1 d . . . Li2 Li 0.7382(2) 0.7393(2) 0.17091(17) 0.0367(7) Uani 1 1 d . . . Si1 Si 0.80331(4) 0.94139(3) 0.11221(3) 0.03596(17) Uani 1 1 d . . . Si2 Si 0.83072(4) 0.56533(3) 0.07501(3) 0.03130(17) Uani 1 1 d . . . O1 O 0.60346(10) 0.72593(10) 0.18407(7) 0.0407(3) Uani 1 1 d . . . O2 O 0.80501(12) 0.72526(10) 0.27258(8) 0.0504(4) Uani 1 1 d . . . O3 O 1.02316(11) 0.76932(13) 0.13018(11) 0.0628(5) Uani 1 1 d . . . N1 N 0.78437(11) 0.83585(10) 0.10387(9) 0.0315(4) Uani 1 1 d . . . N2 N 0.79460(10) 0.66562(9) 0.08908(8) 0.0289(3) Uani 1 1 d . . . N3 N 0.70259(13) 0.99757(10) 0.13058(10) 0.0411(4) Uani 1 1 d . . . N4 N 0.74395(13) 0.48981(10) 0.08745(10) 0.0385(4) Uani 1 1 d . . . C1 C 0.72183(12) 0.79872(11) 0.04736(9) 0.0274(4) Uani 1 1 d . . . C2 C 0.72659(12) 0.70812(11) 0.04011(9) 0.0263(4) Uani 1 1 d . . . C3 C 0.66234(13) 0.66899(12) -0.01369(10) 0.0313(4) Uani 1 1 d . . . H3 H 0.664 0.6094 -0.0185 0.038 Uiso 1 1 calc R . . C4 C 0.59607(14) 0.71458(13) -0.06036(10) 0.0351(4) Uani 1 1 d . . . H4 H 0.5536 0.6861 -0.0963 0.042 Uiso 1 1 calc R . . C5 C 0.59230(14) 0.80143(13) -0.05418(10) 0.0352(4) Uani 1 1 d . . . H5 H 0.5476 0.8329 -0.0862 0.042 Uiso 1 1 calc R . . C6 C 0.65437(13) 0.84261(12) -0.00085(10) 0.0318(4) Uani 1 1 d . . . H6 H 0.6509 0.9023 0.003 0.038 Uiso 1 1 calc R . . C7 C 0.84954(17) 0.98719(15) 0.02764(14) 0.0503(6) Uani 1 1 d . . . H7A H 0.8596 1.048 0.0346 0.075 Uiso 1 1 calc R . . H7B H 0.8031 0.9774 -0.0158 0.075 Uiso 1 1 calc R . . H7C H 0.91 0.9601 0.0201 0.075 Uiso 1 1 calc R . . C8 C 0.90327(19) 0.95487(17) 0.18880(15) 0.0605(7) Uani 1 1 d . . . H8A H 0.9171 1.015 0.1961 0.091 Uiso 1 1 calc R . . H8B H 0.9602 0.9259 0.1755 0.091 Uiso 1 1 calc R . . H8C H 0.8846 0.9307 0.2347 0.091 Uiso 1 1 calc R . . C9 C 0.6377(2) 0.95706(15) 0.17765(15) 0.0583(7) Uani 1 1 d . . . H9 H 0.6525 0.8954 0.1775 0.07 Uiso 1 1 calc R . . C10 C 0.5330(2) 0.96574(18) 0.1463(2) 0.0776(10) Uani 1 1 d . . . H10A H 0.525 0.9479 0.0943 0.116 Uiso 1 1 calc R . . H10B H 0.5132 1.0247 0.1497 0.116 Uiso 1 1 calc R . . H10C H 0.4937 0.9301 0.1748 0.116 Uiso 1 1 calc R . . C11 C 0.6524(3) 0.9849(3) 0.25815(18) 0.0977(13) Uani 1 1 d . . . H11A H 0.7198 0.9791 0.2771 0.147 Uiso 1 1 calc R . . H11B H 0.6139 0.9496 0.2875 0.147 Uiso 1 1 calc R . . H11C H 0.6331 1.044 0.2618 0.147 Uiso 1 1 calc R . . C12 C 0.6861(2) 1.08904(14) 0.12001(15) 0.0568(6) Uani 1 1 d . . . H12 H 0.6317 1.1035 0.1485 0.068 Uiso 1 1 calc R . . C13 C 0.6546(3) 1.1125(2) 0.04040(19) 0.0794(9) Uani 1 1 d . . . H13A H 0.6003 1.0773 0.0213 0.119 Uiso 1 1 calc R . . H13B H 0.7073 1.1035 0.0106 0.119 Uiso 1 1 calc R . . H13C H 0.6357 1.172 0.0378 0.119 Uiso 1 1 calc R . . C14 C 0.7703(3) 1.14248(18) 0.1533(2) 0.0933(11) Uani 1 1 d . . . H14A H 0.7884 1.1255 0.2049 0.14 Uiso 1 1 calc R . . H14B H 0.7521 1.2022 0.1517 0.14 Uiso 1 1 calc R . . H14C H 0.8244 1.1341 0.1248 0.14 Uiso 1 1 calc R . . C15 C 0.87061(18) 0.55206(15) -0.01959(13) 0.0483(6) Uani 1 1 d . . . H15A H 0.8908 0.4936 -0.0259 0.072 Uiso 1 1 calc R . . H15B H 0.9241 0.5901 -0.0248 0.072 Uiso 1 1 calc R . . H15C H 0.8178 0.5655 -0.0574 0.072 Uiso 1 1 calc R . . C16 C 0.94099(17) 0.54884(16) 0.14176(14) 0.0528(6) Uani 1 1 d . . . H16A H 0.9651 0.4915 0.1361 0.079 Uiso 1 1 calc R . . H16B H 0.9256 0.5567 0.1926 0.079 Uiso 1 1 calc R . . H16C H 0.9897 0.5898 0.1314 0.079 Uiso 1 1 calc R . . C17 C 0.67428(17) 0.50788(14) 0.13942(14) 0.0478(5) Uani 1 1 d . . . H17 H 0.6809 0.5692 0.1519 0.057 Uiso 1 1 calc R . . C18 C 0.5714(2) 0.49488(18) 0.1055(2) 0.0713(8) Uani 1 1 d . . . H18A H 0.5604 0.5258 0.0586 0.107 Uiso 1 1 calc R . . H18B H 0.5281 0.5158 0.1398 0.107 Uiso 1 1 calc R . . H18C H 0.5599 0.4346 0.0963 0.107 Uiso 1 1 calc R . . C19 C 0.6926(3) 0.45990(19) 0.21261(16) 0.0736(8) Uani 1 1 d . . . H19A H 0.7588 0.4682 0.2337 0.11 Uiso 1 1 calc R . . H19B H 0.6807 0.3996 0.2037 0.11 Uiso 1 1 calc R . . H19C H 0.6498 0.4811 0.2473 0.11 Uiso 1 1 calc R . . C20 C 0.74323(19) 0.40168(14) 0.06117(15) 0.0540(6) Uani 1 1 d . . . H20 H 0.6982 0.3703 0.0899 0.065 Uiso 1 1 calc R . . C21 C 0.7043(3) 0.39336(19) -0.02035(18) 0.0799(9) Uani 1 1 d . . . H21A H 0.6423 0.4215 -0.029 0.12 Uiso 1 1 calc R . . H21B H 0.697 0.3335 -0.0333 0.12 Uiso 1 1 calc R . . H21C H 0.7487 0.4197 -0.0511 0.12 Uiso 1 1 calc R . . C22 C 0.8393(2) 0.35802(16) 0.07677(17) 0.0665(8) Uani 1 1 d . . . H22A H 0.8623 0.3634 0.1295 0.1 Uiso 1 1 calc R . . H22B H 0.885 0.3844 0.0471 0.1 Uiso 1 1 calc R . . H22C H 0.8324 0.2982 0.0637 0.1 Uiso 1 1 calc R . . C23 C 0.52290(14) 0.72951(15) 0.12788(11) 0.0424(5) Uani 1 1 d . . . H23A H 0.5192 0.6775 0.0976 0.051 Uiso 1 1 calc R . . H23B H 0.5285 0.7785 0.0949 0.051 Uiso 1 1 calc R . . C24 C 0.43546(16) 0.73804(18) 0.16809(13) 0.0539(6) Uani 1 1 d . . . H24A H 0.3946 0.6874 0.1603 0.065 Uiso 1 1 calc R . . H24B H 0.3978 0.7882 0.1504 0.065 Uiso 1 1 calc R . . C25 C 0.47308(17) 0.74736(17) 0.24891(12) 0.0507(6) Uani 1 1 d . . . H25A H 0.4786 0.8075 0.2634 0.061 Uiso 1 1 calc R . . H25B H 0.4315 0.7181 0.2811 0.061 Uiso 1 1 calc R . . C26 C 0.56863(17) 0.70648(18) 0.25291(12) 0.0519(6) Uani 1 1 d . . . H26A H 0.6117 0.7293 0.2949 0.062 Uiso 1 1 calc R . . H26B H 0.5632 0.6447 0.2592 0.062 Uiso 1 1 calc R . . C27 C 0.8190(2) 0.64314(17) 0.30431(15) 0.0647(7) Uani 1 1 d . . . H27A H 0.8284 0.6008 0.2658 0.078 Uiso 1 1 calc R . . H27B H 0.7637 0.6262 0.3299 0.078 Uiso 1 1 calc R . . C28 C 0.9061(2) 0.6518(2) 0.35775(16) 0.0714(8) Uani 1 1 d . . . H28A H 0.9644 0.6486 0.3324 0.086 Uiso 1 1 calc R . . H28B H 0.9088 0.6077 0.3965 0.086 Uiso 1 1 calc R . . C29 C 0.8944(2) 0.7377(2) 0.38978(16) 0.0740(8) Uani 1 1 d . . . H29A H 0.9567 0.7664 0.3997 0.089 Uiso 1 1 calc R . . H29B H 0.8649 0.7339 0.4366 0.089 Uiso 1 1 calc R . . C30 C 0.8303(2) 0.78439(18) 0.33168(14) 0.0630(7) Uani 1 1 d . . . H30A H 0.7726 0.8047 0.3524 0.076 Uiso 1 1 calc R . . H30B H 0.8639 0.8335 0.3133 0.076 Uiso 1 1 calc R . . C31 C 1.0852(2) 0.7561(3) 0.19817(19) 0.0850(11) Uani 1 1 d . . . H31A H 1.07 0.7966 0.2366 0.102 Uiso 1 1 calc R . . H31B H 1.0777 0.6981 0.2169 0.102 Uiso 1 1 calc R . . C32 C 1.1790(2) 0.7689(3) 0.1806(2) 0.1064(16) Uani 1 1 d . . . H32A H 1.2086 0.7144 0.1695 0.128 Uiso 1 1 calc R . . H32B H 1.2185 0.7958 0.2226 0.128 Uiso 1 1 calc R . . C33 C 1.1715(2) 0.8245(3) 0.1149(2) 0.0951(13) Uani 1 1 d . . . H33A H 1.1798 0.8843 0.1298 0.114 Uiso 1 1 calc R . . H33B H 1.2203 0.8097 0.082 0.114 Uiso 1 1 calc R . . C34 C 1.0756(2) 0.8099(3) 0.07731(16) 0.0810(10) Uani 1 1 d . . . H34A H 1.0451 0.8641 0.0611 0.097 Uiso 1 1 calc R . . H34B H 1.0782 0.7736 0.0333 0.097 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 Li1 0.0287(17) 0.0406(19) 0.073(2) -0.0009(17) -0.0035(16) -0.0032(14) Li2 0.0363(17) 0.0420(18) 0.0316(16) -0.0008(13) 0.0036(13) -0.0006(14) Si1 0.0392(3) 0.0290(3) 0.0400(3) -0.0038(2) 0.0060(2) -0.0076(2) Si2 0.0318(3) 0.0296(3) 0.0327(3) 0.00220(19) 0.0046(2) 0.0057(2) O1 0.0341(7) 0.0608(9) 0.0278(7) 0.0018(6) 0.0066(6) -0.0007(7) O2 0.0632(10) 0.0491(9) 0.0355(8) -0.0050(7) -0.0087(7) 0.0054(8) O3 0.0289(8) 0.0779(12) 0.0790(12) 0.0125(10) -0.0054(8) -0.0089(8) N1 0.0309(8) 0.0294(8) 0.0338(8) -0.0029(6) 0.0018(6) -0.0027(6) N2 0.0256(7) 0.0291(8) 0.0315(8) 0.0013(6) 0.0013(6) 0.0022(6) N3 0.0539(11) 0.0249(8) 0.0473(10) -0.0046(7) 0.0182(8) -0.0037(7) N4 0.0453(10) 0.0263(8) 0.0447(9) -0.0012(7) 0.0083(7) 0.0001(7) C1 0.0267(9) 0.0289(9) 0.0272(8) -0.0018(7) 0.0063(7) -0.0016(7) C2 0.0253(8) 0.0288(9) 0.0255(8) 0.0019(7) 0.0063(7) 0.0013(7) C3 0.0367(10) 0.0291(9) 0.0280(9) -0.0018(7) 0.0037(7) -0.0003(8) C4 0.0397(11) 0.0379(10) 0.0264(9) -0.0023(7) -0.0022(8) -0.0017(8) C5 0.0384(11) 0.0385(11) 0.0278(9) 0.0030(8) -0.0005(8) 0.0083(8) C6 0.0382(10) 0.0261(9) 0.0316(9) 0.0013(7) 0.0054(8) 0.0037(8) C7 0.0509(13) 0.0429(12) 0.0604(14) 0.0050(10) 0.0211(11) -0.0039(10) C8 0.0597(16) 0.0519(14) 0.0661(16) -0.0085(12) -0.0088(12) -0.0201(12) C9 0.0762(17) 0.0356(12) 0.0708(16) 0.0040(11) 0.0415(14) 0.0082(11) C10 0.0623(17) 0.0518(16) 0.128(3) -0.0054(16) 0.0500(18) 0.0004(13) C11 0.142(3) 0.097(3) 0.0646(19) 0.0132(18) 0.054(2) 0.037(2) C12 0.0728(17) 0.0273(11) 0.0752(17) -0.0031(11) 0.0300(13) 0.0020(11) C13 0.091(2) 0.0633(18) 0.090(2) 0.0289(16) 0.0380(18) 0.0303(16) C14 0.119(3) 0.0325(14) 0.131(3) -0.0229(16) 0.026(2) -0.0214(16) C15 0.0570(14) 0.0452(12) 0.0458(12) 0.0041(9) 0.0196(10) 0.0154(10) C16 0.0430(12) 0.0565(14) 0.0565(14) 0.0010(11) -0.0045(10) 0.0141(11) C17 0.0530(13) 0.0326(11) 0.0613(14) -0.0005(10) 0.0221(11) -0.0060(9) C18 0.0515(15) 0.0540(15) 0.112(2) -0.0001(15) 0.0243(15) -0.0111(12) C19 0.102(2) 0.0597(17) 0.0649(17) 0.0093(13) 0.0339(16) -0.0170(16) C20 0.0700(16) 0.0273(10) 0.0656(15) -0.0050(10) 0.0119(12) -0.0008(11) C21 0.101(2) 0.0548(17) 0.080(2) -0.0286(15) -0.0069(18) -0.0035(16) C22 0.087(2) 0.0328(12) 0.0816(19) 0.0054(12) 0.0198(16) 0.0181(13) C23 0.0350(11) 0.0578(13) 0.0340(10) -0.0020(9) 0.0017(8) -0.0006(9) C24 0.0347(11) 0.0790(17) 0.0485(13) -0.0011(12) 0.0072(10) -0.0060(11) C25 0.0456(13) 0.0670(16) 0.0421(12) 0.0013(11) 0.0170(10) 0.0006(11) C26 0.0485(13) 0.0743(17) 0.0354(11) 0.0098(11) 0.0151(10) 0.0055(12) C27 0.086(2) 0.0498(14) 0.0556(15) 0.0006(12) -0.0029(13) 0.0017(14) C28 0.0784(19) 0.077(2) 0.0565(15) 0.0152(14) -0.0008(14) 0.0219(16) C29 0.0772(19) 0.090(2) 0.0495(15) -0.0131(14) -0.0155(13) 0.0072(17) C30 0.0788(19) 0.0573(16) 0.0488(14) -0.0132(11) -0.0100(13) 0.0056(13) C31 0.0472(16) 0.129(3) 0.0760(19) 0.033(2) -0.0075(14) -0.0118(17) C32 0.0489(17) 0.175(4) 0.090(2) 0.059(3) -0.0165(16) -0.037(2) C33 0.0508(17) 0.140(3) 0.092(2) 0.051(2) -0.0047(16) -0.0278(19) C34 0.0487(15) 0.139(3) 0.0554(16) 0.0123(18) 0.0060(12) 0.0011(17) #----------------------------------------------------------------------------# # 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 Li1 O3 1.902(4) . ? Li1 N1 1.951(4) . ? Li1 N2 1.961(4) . ? Li2 O1 1.958(4) . ? Li2 O2 1.989(4) . ? Li2 N1 2.105(4) . ? Li2 N2 2.116(4) . ? Si1 N1 1.6985(16) . ? Si1 N3 1.7430(19) . ? Si1 C8 1.880(2) . ? Si1 C7 1.882(2) . ? Si2 N2 1.6981(16) . ? Si2 N4 1.7467(18) . ? Si2 C15 1.880(2) . ? Si2 C16 1.882(2) . ? O1 C26 1.428(2) . ? O1 C23 1.442(2) . ? O2 C27 1.428(3) . ? O2 C30 1.440(3) . ? O3 C34 1.430(4) . ? O3 C31 1.447(3) . ? N1 C1 1.406(2) . ? N2 C2 1.406(2) . ? N3 C9 1.470(3) . ? N3 C12 1.478(3) . ? N4 C17 1.467(3) . ? N4 C20 1.476(3) . ? C1 C6 1.404(3) . ? C1 C2 1.445(3) . ? C2 C3 1.401(3) . ? C3 C4 1.392(3) . ? C4 C5 1.383(3) . ? C5 C6 1.394(3) . ? C9 C11 1.519(4) . ? C9 C10 1.530(4) . ? C12 C13 1.511(4) . ? C12 C14 1.529(4) . ? C17 C18 1.527(4) . ? C17 C19 1.528(4) . ? C20 C22 1.522(4) . ? C20 C21 1.526(4) . ? C23 C24 1.511(3) . ? C24 C25 1.511(3) . ? C25 C26 1.492(3) . ? C27 C28 1.486(4) . ? C28 C29 1.498(4) . ? C29 C30 1.505(4) . ? C31 C32 1.413(4) . ? C32 C33 1.479(4) . ? C33 C34 1.465(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 O3 Li1 N1 131.7(2) . . ? O3 Li1 N2 139.7(2) . . ? N1 Li1 N2 87.99(16) . . ? O1 Li2 O2 103.92(16) . . ? O1 Li2 N1 121.23(18) . . ? O2 Li2 N1 118.21(17) . . ? O1 Li2 N2 118.36(17) . . ? O2 Li2 N2 114.45(17) . . ? N1 Li2 N2 80.16(12) . . ? N1 Si1 N3 113.37(8) . . ? N1 Si1 C8 106.01(10) . . ? N3 Si1 C8 111.22(11) . . ? N1 Si1 C7 111.90(10) . . ? N3 Si1 C7 109.00(10) . . ? C8 Si1 C7 105.02(12) . . ? N2 Si2 N4 113.26(8) . . ? N2 Si2 C15 111.64(9) . . ? N4 Si2 C15 109.21(10) . . ? N2 Si2 C16 105.91(10) . . ? N4 Si2 C16 111.33(11) . . ? C15 Si2 C16 105.15(11) . . ? C26 O1 C23 107.79(15) . . ? C26 O1 Li2 124.51(16) . . ? C23 O1 Li2 127.63(15) . . ? C27 O2 C30 106.34(18) . . ? C27 O2 Li2 120.38(17) . . ? C30 O2 Li2 132.18(18) . . ? C34 O3 C31 109.2(2) . . ? C34 O3 Li1 122.8(2) . . ? C31 O3 Li1 127.2(2) . . ? C1 N1 Si1 123.88(13) . . ? C1 N1 Li1 101.85(16) . . ? Si1 N1 Li1 122.05(14) . . ? C1 N1 Li2 84.69(13) . . ? Si1 N1 Li2 136.12(13) . . ? Li1 N1 Li2 74.96(16) . . ? C2 N2 Si2 123.31(12) . . ? C2 N2 Li1 101.77(16) . . ? Si2 N2 Li1 120.19(14) . . ? C2 N2 Li2 83.99(13) . . ? Si2 N2 Li2 140.01(13) . . ? Li1 N2 Li2 74.52(16) . . ? C9 N3 C12 113.85(18) . . ? C9 N3 Si1 117.69(15) . . ? C12 N3 Si1 126.66(15) . . ? C17 N4 C20 114.35(18) . . ? C17 N4 Si2 118.78(14) . . ? C20 N4 Si2 125.88(15) . . ? C6 C1 N1 125.05(16) . . ? C6 C1 C2 118.12(16) . . ? N1 C1 C2 116.81(15) . . ? C3 C2 N2 124.89(16) . . ? C3 C2 C1 118.07(16) . . ? N2 C2 C1 117.03(15) . . ? C4 C3 C2 122.21(17) . . ? C5 C4 C3 119.80(17) . . ? C4 C5 C6 119.72(17) . . ? C5 C6 C1 122.08(17) . . ? N3 C9 C11 114.0(3) . . ? N3 C9 C10 112.6(2) . . ? C11 C9 C10 110.7(3) . . ? N3 C12 C13 113.0(2) . . ? N3 C12 C14 112.8(2) . . ? C13 C12 C14 112.0(3) . . ? N4 C17 C18 113.0(2) . . ? N4 C17 C19 113.8(2) . . ? C18 C17 C19 110.1(2) . . ? N4 C20 C22 113.4(2) . . ? N4 C20 C21 112.6(2) . . ? C22 C20 C21 110.9(2) . . ? O1 C23 C24 106.55(16) . . ? C23 C24 C25 105.14(18) . . ? C26 C25 C24 102.82(18) . . ? O1 C26 C25 105.26(18) . . ? O2 C27 C28 104.2(2) . . ? C27 C28 C29 102.6(2) . . ? C28 C29 C30 105.0(2) . . ? O2 C30 C29 106.4(2) . . ? C32 C31 O3 106.3(3) . . ? C31 C32 C33 106.5(3) . . ? C34 C33 C32 105.1(3) . . ? O3 C34 C33 106.3(2) . . ? #===END