Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Smith, J David' 'Eaborn, C.' 'El-Hamruni, Salima M.' 'Hill, Michael S.' 'Hitchcock, Peter B.' _publ_contact_author_name 'Dr J David Smith' _publ_contact_author_address ; School of Chemistry, Physics & Environmental Science University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'J.D.SMITH@SUSSEX.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Syntheses and structures of lithium cyanocuprates containing the C(SiMe3)3, C(SiMe3)2(SiMe2NMe2) and C(SiMe3)(SiMe2OMe)2 groups ; data_sep298-JDS1D _database_code_CSD 188683 _audit_creation_date 2002-03-05T09:38:15-00:00 _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 _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [{(Me3Si)3CCuCNLi(thf)2}2] _chemical_formula_sum 'C38 H86 Cu2 Li2 N2 O4 Si6' _chemical_formula_weight 944.59 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.452(8) _cell_length_b 17.080(11) _cell_length_c 18.748(13) _cell_angle_alpha 82.91(5) _cell_angle_beta 73.53(5) _cell_angle_gamma 84.41(5) _cell_volume 4090(5) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.15 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method 'omega-2theta scans' _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.148 _diffrn_reflns_number 9978 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 21.98 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 9978 _reflns_number_gt 5492 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Two independent molecules; one on an inversion centre and the other in a general position. 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^)+(0.0804P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 9978 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1543 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.195 _refine_ls_wR_factor_gt 0.1578 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.574 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 Li1 Li 0.0754(12) 0.3195(10) 0.3066(9) 0.041(4) Uani 1 1 d . . . Li2 Li -0.1076(12) 0.3282(10) 0.4204(9) 0.038(4) Uani 1 1 d . . . Li3 Li -0.0982(11) -0.0103(10) 0.0471(8) 0.034(4) Uani 1 1 d . . . Cu1 Cu 0.15552(8) 0.09527(7) 0.39097(6) 0.0303(3) Uani 1 1 d . . . Cu2 Cu -0.15708(9) 0.55902(7) 0.30285(6) 0.0334(3) Uani 1 1 d . . . Cu3 Cu 0.18465(9) -0.22198(7) 0.02735(7) 0.0354(4) Uani 1 1 d . . . Si1 Si 0.3700(2) 0.05637(17) 0.30265(15) 0.0359(7) Uani 1 1 d . . . Si2 Si 0.2911(2) -0.01975(17) 0.46602(14) 0.0314(7) Uani 1 1 d . . . Si3 Si 0.20367(19) -0.06801(16) 0.34271(14) 0.0299(7) Uani 1 1 d . . . Si4 Si -0.2527(2) 0.72693(18) 0.33196(16) 0.0446(8) Uani 1 1 d . . . Si5 Si -0.3786(2) 0.58753(19) 0.32009(16) 0.0436(8) Uani 1 1 d . . . Si6 Si -0.21989(19) 0.66033(16) 0.17930(14) 0.0301(7) Uani 1 1 d . . . Si7 Si 0.4050(2) -0.26205(19) -0.04861(15) 0.0461(8) Uani 1 1 d . . . Si8 Si 0.3135(2) -0.31065(18) 0.12109(15) 0.0393(8) Uani 1 1 d . . . Si9 Si 0.2465(3) -0.3908(2) 0.0026(2) 0.0609(10) Uani 1 1 d . . . O1 O 0.2105(5) 0.3386(4) 0.3086(4) 0.048(2) Uani 1 1 d . . . O2 O 0.0696(6) 0.2915(5) 0.2134(4) 0.059(2) Uani 1 1 d . . . O3 O -0.2350(5) 0.3125(4) 0.4014(4) 0.0437(18) Uani 1 1 d . . . O4 O -0.1302(5) 0.3574(5) 0.5168(4) 0.061(2) Uani 1 1 d . . . O5 O -0.2193(4) -0.0312(4) 0.0233(3) 0.0386(18) Uani 1 1 d . . . O6 O -0.1357(5) 0.0052(5) 0.1501(3) 0.054(2) Uani 1 1 d . . . N1 N 0.0057(6) 0.2380(5) 0.3972(4) 0.037(2) Uani 1 1 d . . . N2 N -0.0276(7) 0.4123(6) 0.3349(5) 0.050(3) Uani 1 1 d . . . N3 N 0.0252(6) -0.0866(5) 0.0235(4) 0.039(2) Uani 1 1 d . . . C1 C 0.2631(6) 0.0098(5) 0.3744(5) 0.028(2) Uani 1 1 d . . . C2 C 0.4497(8) 0.1178(7) 0.3404(6) 0.054(3) Uani 1 1 d . . . H2C H 0.5049 0.1406 0.2989 0.081 Uiso 1 1 calc R . . H2B H 0.4806 0.0843 0.3758 0.081 Uiso 1 1 calc R . . H2A H 0.4047 0.1605 0.3658 0.081 Uiso 1 1 calc R . . C3 C 0.3233(8) 0.1301(6) 0.2328(5) 0.045(3) Uani 1 1 d . . . H3C H 0.3832 0.1531 0.1959 0.067 Uiso 1 1 calc R . . H3B H 0.2782 0.1722 0.2591 0.067 Uiso 1 1 calc R . . H3A H 0.2843 0.1032 0.2073 0.067 Uiso 1 1 calc R . . C4 C 0.4677(7) -0.0148(7) 0.2448(6) 0.058(3) Uani 1 1 d . . . H4C H 0.5217 0.0148 0.2081 0.087 Uiso 1 1 calc R . . H4B H 0.4324 -0.0445 0.2187 0.087 Uiso 1 1 calc R . . H4A H 0.4995 -0.0517 0.2777 0.087 Uiso 1 1 calc R . . C5 C 0.1927(7) -0.0837(6) 0.5322(5) 0.043(3) Uani 1 1 d . . . H5C H 0.2118 -0.0972 0.5792 0.064 Uiso 1 1 calc R . . H5B H 0.1907 -0.1323 0.51 0.064 Uiso 1 1 calc R . . H5A H 0.1241 -0.0552 0.5422 0.064 Uiso 1 1 calc R . . C6 C 0.4200(7) -0.0757(7) 0.4575(6) 0.053(3) Uani 1 1 d . . . H6C H 0.4302 -0.0896 0.5074 0.079 Uiso 1 1 calc R . . H6B H 0.4753 -0.0427 0.4269 0.079 Uiso 1 1 calc R . . H6A H 0.4219 -0.1241 0.4338 0.079 Uiso 1 1 calc R . . C7 C 0.2916(8) 0.0660(7) 0.5186(6) 0.053(3) Uani 1 1 d . . . H7C H 0.3067 0.0469 0.5662 0.079 Uiso 1 1 calc R . . H7B H 0.2234 0.0951 0.5284 0.079 Uiso 1 1 calc R . . H7A H 0.345 0.1012 0.4889 0.079 Uiso 1 1 calc R . . C8 C 0.2763(8) -0.1669(6) 0.3452(5) 0.043(3) Uani 1 1 d . . . H8C H 0.241 -0.2053 0.3279 0.065 Uiso 1 1 calc R . . H8B H 0.2787 -0.1844 0.3965 0.065 Uiso 1 1 calc R . . H8A H 0.3472 -0.163 0.3126 0.065 Uiso 1 1 calc R . . C9 C 0.0649(7) -0.0819(7) 0.3962(6) 0.052(3) Uani 1 1 d . . . H9C H 0.0388 -0.1238 0.3765 0.078 Uiso 1 1 calc R . . H9B H 0.023 -0.0324 0.391 0.078 Uiso 1 1 calc R . . H9A H 0.0605 -0.0968 0.4492 0.078 Uiso 1 1 calc R . . C10 C 0.1951(8) -0.0447(6) 0.2430(5) 0.043(3) Uani 1 1 d . . . H10C H 0.1632 -0.0877 0.2293 0.064 Uiso 1 1 calc R . . H10B H 0.265 -0.039 0.2092 0.064 Uiso 1 1 calc R . . H10A H 0.1526 0.0048 0.2389 0.064 Uiso 1 1 calc R . . C11 C 0.0588(7) 0.1813(7) 0.3973(5) 0.034(3) Uani 1 1 d . . . C12 C -0.2583(6) 0.6405(5) 0.2826(5) 0.025(2) Uani 1 1 d . . . C13 C -0.3072(13) 0.7081(8) 0.4358(6) 0.102(6) Uani 1 1 d . . . H13C H -0.3025 0.7553 0.4593 0.153 Uiso 1 1 calc R . . H13B H -0.2675 0.6633 0.455 0.153 Uiso 1 1 calc R . . H13A H -0.3802 0.6959 0.4475 0.153 Uiso 1 1 calc R . . C14 C -0.1190(10) 0.7579(7) 0.3210(8) 0.078(4) Uani 1 1 d . . . H14C H -0.1236 0.8037 0.3488 0.117 Uiso 1 1 calc R . . H14B H -0.0852 0.772 0.2679 0.117 Uiso 1 1 calc R . . H14A H -0.0782 0.7141 0.3405 0.117 Uiso 1 1 calc R . . C15 C -0.3271(9) 0.8194(6) 0.3027(6) 0.061(3) Uani 1 1 d . . . H15C H -0.3208 0.8625 0.3308 0.091 Uiso 1 1 calc R . . H15B H -0.4005 0.8091 0.313 0.091 Uiso 1 1 calc R . . H15A H -0.2985 0.8344 0.249 0.091 Uiso 1 1 calc R . . C16 C -0.3858(9) 0.5269(8) 0.4131(6) 0.088(5) Uani 1 1 d . . . H16C H -0.4511 0.5004 0.43 0.132 Uiso 1 1 calc R . . H16B H -0.3831 0.5618 0.4501 0.132 Uiso 1 1 calc R . . H16A H -0.3271 0.4872 0.4072 0.132 Uiso 1 1 calc R . . C17 C -0.3932(8) 0.5110(7) 0.2614(7) 0.064(4) Uani 1 1 d . . . H17C H -0.4586 0.4858 0.2849 0.096 Uiso 1 1 calc R . . H17B H -0.3349 0.4711 0.2569 0.096 Uiso 1 1 calc R . . H17A H -0.3939 0.5361 0.2116 0.096 Uiso 1 1 calc R . . C18 C -0.5010(8) 0.6531(8) 0.3350(7) 0.080(4) Uani 1 1 d . . . H18C H -0.561 0.6208 0.3548 0.12 Uiso 1 1 calc R . . H18B H -0.5047 0.6821 0.2872 0.12 Uiso 1 1 calc R . . H18A H -0.5014 0.6906 0.3706 0.12 Uiso 1 1 calc R . . C19 C -0.1650(7) 0.5695(7) 0.1318(6) 0.051(3) Uani 1 1 d . . . H19C H -0.1458 0.5829 0.0775 0.077 Uiso 1 1 calc R . . H19B H -0.2171 0.53 0.1457 0.077 Uiso 1 1 calc R . . H19A H -0.1032 0.548 0.1472 0.077 Uiso 1 1 calc R . . C20 C -0.3299(8) 0.7019(7) 0.1406(5) 0.050(3) Uani 1 1 d . . . H20C H -0.3048 0.7111 0.086 0.075 Uiso 1 1 calc R . . H20B H -0.3581 0.752 0.1612 0.075 Uiso 1 1 calc R . . H20A H -0.3845 0.6644 0.1542 0.075 Uiso 1 1 calc R . . C21 C -0.1160(8) 0.7324(6) 0.1418(6) 0.048(3) Uani 1 1 d . . . H21C H -0.0998 0.74 0.0871 0.073 Uiso 1 1 calc R . . H21B H -0.0534 0.7117 0.1565 0.073 Uiso 1 1 calc R . . H21A H -0.1407 0.7831 0.1621 0.073 Uiso 1 1 calc R . . C22 C -0.0721(8) 0.4693(7) 0.3227(6) 0.040(3) Uani 1 1 d . . . C23 C 0.2510(8) 0.3252(8) 0.3708(7) 0.066(4) Uani 1 1 d . . . H23B H 0.2575 0.2678 0.3864 0.079 Uiso 1 1 calc R . . H23A H 0.2048 0.3517 0.4133 0.079 Uiso 1 1 calc R . . C24 C 0.3562(10) 0.3590(9) 0.3466(9) 0.101(6) Uani 1 1 d . . . H24B H 0.3582 0.4012 0.3779 0.121 Uiso 1 1 calc R . . H24A H 0.411 0.3172 0.3514 0.121 Uiso 1 1 calc R . . C25 C 0.3713(11) 0.3894(13) 0.2728(8) 0.135(8) Uani 1 1 d . . . H25B H 0.4338 0.3624 0.2413 0.163 Uiso 1 1 calc R . . H25A H 0.3828 0.4465 0.2677 0.163 Uiso 1 1 calc R . . C26 C 0.2819(9) 0.3785(9) 0.2480(7) 0.077(4) Uani 1 1 d . . . H26B H 0.2502 0.4303 0.2327 0.092 Uiso 1 1 calc R . . H26A H 0.3024 0.3469 0.2047 0.092 Uiso 1 1 calc R . . C27 C 0.0656(15) 0.3481(10) 0.1516(9) 0.127(7) Uani 1 1 d . . . H27B H 0.1067 0.3934 0.1506 0.152 Uiso 1 1 calc R . . H27A H -0.0071 0.3679 0.1549 0.152 Uiso 1 1 calc R . . C28 C 0.1099(14) 0.3063(17) 0.0842(8) 0.154(11) Uani 1 1 d . . . H28B H 0.0763 0.3266 0.0443 0.185 Uiso 1 1 calc R . . H28A H 0.1857 0.3116 0.0649 0.185 Uiso 1 1 calc R . . C29 C 0.087(2) 0.2263(15) 0.1108(12) 0.208(15) Uani 1 1 d . . . H29B H 0.148 0.1904 0.0896 0.25 Uiso 1 1 calc R . . H29A H 0.0276 0.2125 0.0948 0.25 Uiso 1 1 calc R . . C30 C 0.0625(13) 0.2170(10) 0.1926(8) 0.102(5) Uani 1 1 d . . . H30B H -0.0085 0.199 0.2148 0.122 Uiso 1 1 calc R . . H30A H 0.1124 0.1778 0.2095 0.122 Uiso 1 1 calc R . . C31 C -0.2411(9) 0.2984(8) 0.3290(6) 0.065(4) Uani 1 1 d . . . H31B H -0.1878 0.257 0.3079 0.079 Uiso 1 1 calc R . . H31A H -0.2305 0.3473 0.2942 0.079 Uiso 1 1 calc R . . C32 C -0.3475(9) 0.2719(10) 0.3410(8) 0.095(5) Uani 1 1 d . . . H32B H -0.3805 0.301 0.3038 0.114 Uiso 1 1 calc R . . H32A H -0.3441 0.2146 0.3356 0.114 Uiso 1 1 calc R . . C33 C -0.4048(10) 0.2870(11) 0.4129(8) 0.110(6) Uani 1 1 d . . . H33B H -0.4476 0.2421 0.4374 0.132 Uiso 1 1 calc R . . H33A H -0.4516 0.3351 0.411 0.132 Uiso 1 1 calc R . . C34 C -0.3319(7) 0.2980(7) 0.4550(6) 0.049(3) Uani 1 1 d . . . H34B H -0.3565 0.3434 0.4851 0.059 Uiso 1 1 calc R . . H34A H -0.3247 0.2501 0.4892 0.059 Uiso 1 1 calc R . . C35 C -0.0657(10) 0.3331(8) 0.5638(7) 0.068(4) Uani 1 1 d . . . H35B H 0.0021 0.3107 0.5346 0.082 Uiso 1 1 calc R . . H35A H -0.0984 0.292 0.6033 0.082 Uiso 1 1 calc R . . C36 C -0.0515(14) 0.4010(9) 0.5967(10) 0.119(7) Uani 1 1 d . . . H36B H 0.012 0.4267 0.5666 0.143 Uiso 1 1 calc R . . H36A H -0.0455 0.386 0.6481 0.143 Uiso 1 1 calc R . . C37 C -0.1427(15) 0.4532(11) 0.5976(10) 0.141(8) Uani 1 1 d . . . H37B H -0.1238 0.5087 0.5836 0.17 Uiso 1 1 calc R . . H37A H -0.1927 0.4493 0.6479 0.17 Uiso 1 1 calc R . . C38 C -0.1881(11) 0.4272(9) 0.5425(8) 0.095(5) Uani 1 1 d . . . H38B H -0.2619 0.4164 0.566 0.114 Uiso 1 1 calc R . . H38A H -0.1845 0.4688 0.5003 0.114 Uiso 1 1 calc R . . C39 C 0.2966(7) -0.3035(6) 0.0253(5) 0.036(3) Uani 1 1 d . . . C40 C 0.4148(8) -0.1539(7) -0.0480(6) 0.057(3) Uani 1 1 d . . . H40C H 0.4741 -0.136 -0.0888 0.085 Uiso 1 1 calc R . . H40B H 0.4245 -0.1439 -0.0001 0.085 Uiso 1 1 calc R . . H40A H 0.3509 -0.1251 -0.0547 0.085 Uiso 1 1 calc R . . C41 C 0.5349(8) -0.3117(8) -0.0477(6) 0.071(4) Uani 1 1 d . . . H41C H 0.5889 -0.2866 -0.0885 0.107 Uiso 1 1 calc R . . H41B H 0.5356 -0.3678 -0.0543 0.107 Uiso 1 1 calc R . . H41A H 0.5484 -0.3066 0.0002 0.107 Uiso 1 1 calc R . . C42 C 0.3941(11) -0.2711(8) -0.1466(6) 0.084(5) Uani 1 1 d . . . H42C H 0.4537 -0.2482 -0.1839 0.126 Uiso 1 1 calc R . . H42B H 0.3297 -0.2428 -0.1529 0.126 Uiso 1 1 calc R . . H42A H 0.3932 -0.3271 -0.1533 0.126 Uiso 1 1 calc R . . C43 C 0.1897(8) -0.3040(9) 0.1980(6) 0.079(4) Uani 1 1 d . . . H43C H 0.2058 -0.3083 0.2462 0.118 Uiso 1 1 calc R . . H43B H 0.147 -0.3471 0.1975 0.118 Uiso 1 1 calc R . . H43A H 0.1517 -0.2532 0.1906 0.118 Uiso 1 1 calc R . . C44 C 0.3850(7) -0.2276(6) 0.1359(5) 0.045(3) Uani 1 1 d . . . H44C H 0.3915 -0.2346 0.1871 0.068 Uiso 1 1 calc R . . H44B H 0.3465 -0.1771 0.1278 0.068 Uiso 1 1 calc R . . H44A H 0.4544 -0.2278 0.1005 0.068 Uiso 1 1 calc R . . C45 C 0.3871(8) -0.4046(7) 0.1463(6) 0.060(3) Uani 1 1 d . . . H45C H 0.3934 -0.4048 0.1971 0.09 Uiso 1 1 calc R . . H45B H 0.4565 -0.4077 0.1111 0.09 Uiso 1 1 calc R . . H45A H 0.3497 -0.4502 0.1437 0.09 Uiso 1 1 calc R . . C46 C 0.3480(10) -0.4700(7) -0.0311(8) 0.084(5) Uani 1 1 d . . . H46C H 0.3155 -0.5144 -0.042 0.126 Uiso 1 1 calc R . . H46B H 0.3833 -0.4883 0.0076 0.126 Uiso 1 1 calc R . . H46A H 0.3986 -0.4492 -0.0766 0.126 Uiso 1 1 calc R . . C47 C 0.1545(10) -0.4424(8) 0.0837(9) 0.107(6) Uani 1 1 d . . . H47C H 0.1309 -0.4882 0.0678 0.16 Uiso 1 1 calc R . . H47B H 0.0947 -0.4061 0.1034 0.16 Uiso 1 1 calc R . . H47A H 0.1895 -0.4603 0.1227 0.16 Uiso 1 1 calc R . . C48 C 0.1681(12) -0.3676(9) -0.0648(10) 0.131(8) Uani 1 1 d . . . H48C H 0.144 -0.4166 -0.0744 0.197 Uiso 1 1 calc R . . H48B H 0.2107 -0.3421 -0.1117 0.197 Uiso 1 1 calc R . . H48A H 0.1081 -0.3319 -0.044 0.197 Uiso 1 1 calc R . . C49 C 0.0836(7) -0.1401(6) 0.0255(5) 0.032(2) Uani 1 1 d . . . C50 C -0.2880(8) -0.0876(7) 0.0685(7) 0.062(4) Uani 1 1 d . . . H50B H -0.314 -0.0733 0.1205 0.074 Uiso 1 1 calc R . . H50A H -0.2519 -0.141 0.0692 0.074 Uiso 1 1 calc R . . C51 C -0.3743(11) -0.0864(10) 0.0348(8) 0.119(7) Uani 1 1 d . . . H51B H -0.3901 -0.1411 0.032 0.143 Uiso 1 1 calc R . . H51A H -0.4372 -0.0593 0.0658 0.143 Uiso 1 1 calc R . . C52 C -0.3458(8) -0.0465(8) -0.0368(6) 0.068(4) Uani 1 1 d . . . H52B H -0.3984 -0.0031 -0.0421 0.082 Uiso 1 1 calc R . . H52A H -0.3411 -0.0833 -0.0747 0.082 Uiso 1 1 calc R . . C53 C -0.2422(7) -0.0138(7) -0.0480(5) 0.045(3) Uani 1 1 d . . . H53B H -0.1883 -0.0395 -0.0875 0.055 Uiso 1 1 calc R . . H53A H -0.2457 0.0439 -0.0624 0.055 Uiso 1 1 calc R . . C54 C -0.0747(10) -0.0193(9) 0.1995(7) 0.081(5) Uani 1 1 d . . . H54B H -0.0041 -0.0002 0.1783 0.097 Uiso 1 1 calc R . . H54A H -0.0687 -0.0777 0.2077 0.097 Uiso 1 1 calc R . . C55 C -0.1255(10) 0.0140(10) 0.2701(7) 0.095(5) Uani 1 1 d . . . H55B H -0.1463 -0.0287 0.3111 0.115 Uiso 1 1 calc R . . H55A H -0.0779 0.0471 0.2831 0.115 Uiso 1 1 calc R . . C56 C -0.2158(14) 0.0615(12) 0.2588(8) 0.140(8) Uani 1 1 d . . . H56B H -0.2797 0.0405 0.2938 0.168 Uiso 1 1 calc R . . H56A H -0.2122 0.1168 0.2682 0.168 Uiso 1 1 calc R . . C57 C -0.2177(10) 0.0587(9) 0.1848(7) 0.092(5) Uani 1 1 d . . . H57B H -0.209 0.1121 0.1573 0.11 Uiso 1 1 calc R . . H57A H -0.2853 0.041 0.184 0.11 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 0.034(10) 0.037(11) 0.046(11) 0.010(8) -0.008(8) -0.001(8) Li2 0.035(9) 0.040(11) 0.045(10) -0.018(8) -0.015(8) 0.003(8) Li3 0.035(9) 0.043(11) 0.026(9) -0.025(8) -0.002(7) 0.004(8) Cu1 0.0271(7) 0.0292(8) 0.0305(7) -0.0020(5) -0.0018(5) -0.0020(5) Cu2 0.0353(7) 0.0288(8) 0.0377(8) -0.0007(6) -0.0141(6) -0.0015(6) Cu3 0.0327(7) 0.0330(8) 0.0421(8) -0.0082(6) -0.0125(6) 0.0026(6) Si1 0.0247(15) 0.0374(19) 0.0380(17) 0.0008(14) 0.0025(13) -0.0042(13) Si2 0.0337(16) 0.0346(18) 0.0271(15) -0.0068(13) -0.0080(12) -0.0039(13) Si3 0.0322(16) 0.0322(18) 0.0254(15) -0.0012(12) -0.0072(12) -0.0077(13) Si4 0.069(2) 0.037(2) 0.0327(17) -0.0106(14) -0.0213(16) 0.0053(16) Si5 0.0326(17) 0.051(2) 0.0377(18) 0.0100(15) 0.0018(14) -0.0084(14) Si6 0.0299(15) 0.0330(18) 0.0274(15) -0.0002(12) -0.0053(12) -0.0132(13) Si7 0.0486(19) 0.056(2) 0.0295(17) -0.0095(15) -0.0070(14) 0.0107(16) Si8 0.0364(17) 0.046(2) 0.0339(17) -0.0017(14) -0.0071(13) -0.0063(14) Si9 0.063(2) 0.037(2) 0.104(3) -0.025(2) -0.054(2) 0.0074(17) O1 0.033(4) 0.073(6) 0.038(4) 0.013(4) -0.012(4) -0.013(4) O2 0.089(6) 0.053(6) 0.044(5) -0.007(4) -0.026(4) -0.019(5) O3 0.030(4) 0.061(5) 0.038(4) -0.007(4) -0.004(3) -0.008(3) O4 0.048(5) 0.085(7) 0.058(5) -0.034(5) -0.024(4) 0.018(4) O5 0.028(4) 0.064(5) 0.028(4) 0.007(3) -0.014(3) -0.016(3) O6 0.043(4) 0.090(6) 0.030(4) -0.010(4) -0.017(3) 0.019(4) N1 0.027(5) 0.042(6) 0.036(5) 0.004(4) 0.001(4) -0.008(4) N2 0.045(6) 0.040(6) 0.069(7) 0.003(5) -0.026(5) -0.002(5) N3 0.035(5) 0.028(6) 0.051(6) -0.002(4) -0.011(4) 0.000(4) C1 0.018(5) 0.033(6) 0.030(6) 0.000(5) -0.003(4) -0.007(4) C2 0.036(6) 0.061(8) 0.068(8) 0.002(6) -0.019(6) -0.015(6) C3 0.046(6) 0.045(7) 0.033(6) 0.007(5) 0.006(5) -0.009(5) C4 0.031(6) 0.068(9) 0.060(8) 0.001(6) 0.006(6) 0.002(6) C5 0.045(6) 0.056(8) 0.030(6) -0.013(5) -0.010(5) -0.004(5) C6 0.044(7) 0.064(9) 0.053(7) 0.002(6) -0.021(6) 0.001(6) C7 0.056(7) 0.075(9) 0.041(7) -0.029(6) -0.027(6) 0.004(6) C8 0.060(7) 0.040(7) 0.034(6) -0.012(5) -0.019(5) 0.003(5) C9 0.043(7) 0.067(9) 0.055(7) -0.005(6) -0.022(6) -0.029(6) C10 0.051(7) 0.054(8) 0.023(6) -0.005(5) -0.008(5) -0.002(5) C11 0.023(6) 0.058(8) 0.020(6) 0.002(5) -0.003(4) -0.014(5) C12 0.029(5) 0.019(6) 0.023(5) 0.001(4) -0.003(4) 0.001(4) C13 0.196(17) 0.088(12) 0.029(7) -0.021(7) -0.044(9) 0.017(11) C14 0.113(11) 0.037(8) 0.114(11) -0.007(7) -0.078(9) -0.012(7) C15 0.077(9) 0.045(8) 0.060(8) -0.008(6) -0.022(7) 0.014(6) C16 0.071(9) 0.110(12) 0.055(8) 0.055(8) 0.006(7) -0.020(8) C17 0.046(7) 0.065(9) 0.081(9) 0.014(7) -0.017(6) -0.031(6) C18 0.031(7) 0.112(12) 0.076(9) 0.009(8) 0.010(6) 0.001(7) C19 0.033(6) 0.070(9) 0.044(7) -0.007(6) 0.002(5) -0.013(6) C20 0.059(7) 0.064(8) 0.036(6) 0.008(6) -0.029(6) -0.016(6) C21 0.051(7) 0.050(8) 0.043(7) 0.001(6) -0.008(5) -0.026(6) C22 0.041(7) 0.039(8) 0.045(7) -0.009(6) -0.013(5) -0.014(6) C23 0.051(8) 0.089(10) 0.070(9) 0.012(7) -0.035(7) -0.029(7) C24 0.072(10) 0.132(15) 0.113(13) 0.056(11) -0.061(10) -0.054(9) C25 0.058(10) 0.28(3) 0.073(11) 0.010(14) -0.003(9) -0.089(13) C26 0.069(9) 0.105(12) 0.052(8) 0.012(8) -0.009(7) -0.035(8) C27 0.192(19) 0.120(16) 0.089(13) 0.053(12) -0.075(13) -0.074(14) C28 0.091(13) 0.33(4) 0.023(9) -0.008(15) 0.001(8) 0.001(17) C29 0.36(4) 0.19(3) 0.092(18) -0.042(16) -0.12(2) 0.11(3) C30 0.140(14) 0.101(15) 0.078(12) -0.007(10) -0.057(10) 0.003(11) C31 0.069(9) 0.098(11) 0.033(7) -0.029(7) -0.007(6) -0.017(7) C32 0.052(8) 0.155(16) 0.097(12) -0.063(11) -0.016(8) -0.047(9) C33 0.048(9) 0.22(2) 0.068(10) 0.007(11) -0.024(8) -0.055(10) C34 0.042(7) 0.058(8) 0.043(7) -0.001(6) -0.009(6) -0.005(6) C35 0.079(9) 0.085(11) 0.053(8) -0.022(7) -0.035(7) 0.000(8) C36 0.186(19) 0.069(12) 0.149(16) -0.019(11) -0.118(15) -0.014(12) C37 0.21(2) 0.135(17) 0.114(14) -0.062(13) -0.105(15) 0.069(16) C38 0.092(11) 0.127(14) 0.076(10) -0.068(10) -0.037(9) 0.050(10) C39 0.033(6) 0.034(7) 0.042(6) -0.013(5) -0.011(5) 0.002(5) C40 0.046(7) 0.063(9) 0.048(7) 0.013(6) 0.002(6) -0.006(6) C41 0.043(7) 0.108(12) 0.051(8) -0.006(7) 0.002(6) 0.011(7) C42 0.123(12) 0.089(11) 0.040(8) -0.011(7) -0.028(8) 0.018(9) C43 0.042(7) 0.133(14) 0.050(8) 0.000(8) 0.004(6) -0.017(8) C44 0.039(6) 0.063(8) 0.037(6) -0.007(5) -0.015(5) -0.003(5) C45 0.053(7) 0.066(9) 0.067(8) 0.017(7) -0.035(6) -0.008(6) C46 0.094(10) 0.059(10) 0.128(12) -0.048(9) -0.073(9) 0.031(8) C47 0.085(11) 0.051(10) 0.202(18) -0.034(11) -0.062(12) 0.000(8) C48 0.164(15) 0.073(11) 0.23(2) -0.082(12) -0.168(16) 0.050(11) C49 0.038(6) 0.020(6) 0.038(6) -0.008(5) -0.005(5) -0.006(5) C50 0.056(8) 0.058(9) 0.065(8) 0.037(7) -0.016(6) -0.034(6) C51 0.085(10) 0.169(17) 0.121(13) 0.097(12) -0.069(10) -0.103(11) C52 0.054(8) 0.125(12) 0.032(7) 0.002(7) -0.017(6) -0.032(8) C53 0.042(7) 0.067(8) 0.028(6) -0.004(5) -0.005(5) -0.021(6) C54 0.074(9) 0.121(13) 0.058(9) -0.031(8) -0.037(7) 0.031(8) C55 0.083(10) 0.155(16) 0.053(9) -0.025(9) -0.032(8) 0.031(10) C56 0.163(17) 0.20(2) 0.068(11) -0.075(12) -0.066(11) 0.101(15) C57 0.075(10) 0.145(15) 0.055(9) -0.030(9) -0.030(7) 0.059(10) #----------------------------------------------------------------------------# # 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 O1 1.888(17) . ? Li1 O2 1.891(19) . ? Li1 N2 2.020(19) . ? Li1 N1 2.115(17) . ? Li2 O4 1.867(17) . ? Li2 O3 1.896(16) . ? Li2 N1 2.054(18) . ? Li2 N2 2.13(2) . ? Li3 O5 1.883(16) . ? Li3 O6 1.897(15) . ? Li3 N3 1.988(17) . ? Li3 N3 2.119(19) 2 ? Cu1 C11 1.857(11) . ? Cu1 C1 1.941(9) . ? Cu2 C22 1.885(12) . ? Cu2 C12 1.931(8) . ? Cu3 C49 1.858(10) . ? Cu3 C39 1.944(9) . ? Si1 C1 1.836(9) . ? Si1 C2 1.892(10) . ? Si1 C4 1.894(10) . ? Si1 C3 1.899(9) . ? Si2 C1 1.861(9) . ? Si2 C7 1.866(10) . ? Si2 C5 1.871(10) . ? Si2 C6 1.872(10) . ? Si3 C1 1.852(10) . ? Si3 C8 1.870(10) . ? Si3 C9 1.874(10) . ? Si3 C10 1.897(9) . ? Si4 C12 1.855(9) . ? Si4 C14 1.872(12) . ? Si4 C13 1.875(11) . ? Si4 C15 1.894(10) . ? Si5 C12 1.847(9) . ? Si5 C17 1.867(12) . ? Si5 C18 1.871(11) . ? Si5 C16 1.897(10) . ? Si6 C12 1.855(9) . ? Si6 C19 1.868(11) . ? Si6 C20 1.871(9) . ? Si6 C21 1.878(10) . ? Si7 C39 1.833(10) . ? Si7 C40 1.866(12) . ? Si7 C41 1.870(10) . ? Si7 C42 1.911(11) . ? Si8 C39 1.862(10) . ? Si8 C43 1.873(11) . ? Si8 C44 1.878(11) . ? Si8 C45 1.883(10) . ? Si9 C39 1.836(10) . ? Si9 C48 1.848(12) . ? Si9 C47 1.854(16) . ? Si9 C46 1.859(11) . ? O1 C23 1.407(11) . ? O1 C26 1.412(12) . ? O2 C30 1.396(16) . ? O2 C27 1.424(15) . ? O3 C34 1.424(11) . ? O3 C31 1.435(11) . ? O4 C35 1.405(12) . ? O4 C38 1.417(13) . ? O5 C50 1.425(11) . ? O5 C53 1.444(10) . ? O6 C54 1.404(12) . ? O6 C57 1.422(12) . ? N1 C11 1.146(11) . ? N2 C22 1.125(12) . ? N3 C49 1.149(11) . ? N3 Li3 2.119(19) 2 ? C23 C24 1.508(15) . ? C24 C25 1.382(17) . ? C25 C26 1.443(16) . ? C27 C28 1.47(2) . ? C28 C29 1.43(3) . ? C29 C30 1.47(2) . ? C31 C32 1.491(15) . ? C32 C33 1.391(17) . ? C33 C34 1.460(15) . ? C35 C36 1.431(17) . ? C36 C37 1.443(19) . ? C37 C38 1.469(18) . ? C50 C51 1.467(14) . ? C51 C52 1.395(15) . ? C52 C53 1.502(13) . ? C54 C55 1.464(16) . ? C55 C56 1.445(17) . ? C56 C57 1.401(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 O2 113.5(9) . . ? O1 Li1 N2 112.5(10) . . ? O2 Li1 N2 108.7(8) . . ? O1 Li1 N1 111.2(8) . . ? O2 Li1 N1 112.7(9) . . ? N2 Li1 N1 97.1(8) . . ? O4 Li2 O3 110.8(8) . . ? O4 Li2 N1 112.3(8) . . ? O3 Li2 N1 115.7(9) . . ? O4 Li2 N2 113.5(9) . . ? O3 Li2 N2 108.2(8) . . ? N1 Li2 N2 95.5(7) . . ? O5 Li3 O6 107.7(8) . . ? O5 Li3 N3 118.9(8) . . ? O6 Li3 N3 109.9(8) . . ? O5 Li3 N3 111.1(8) . 2 ? O6 Li3 N3 113.3(8) . 2 ? N3 Li3 N3 95.7(7) . 2 ? C11 Cu1 C1 174.3(4) . . ? C22 Cu2 C12 171.9(4) . . ? C49 Cu3 C39 176.5(4) . . ? C1 Si1 C2 114.3(5) . . ? C1 Si1 C4 114.9(5) . . ? C2 Si1 C4 105.2(5) . . ? C1 Si1 C3 112.9(4) . . ? C2 Si1 C3 102.8(5) . . ? C4 Si1 C3 105.6(5) . . ? C1 Si2 C7 113.2(5) . . ? C1 Si2 C5 113.5(4) . . ? C7 Si2 C5 104.1(5) . . ? C1 Si2 C6 113.3(4) . . ? C7 Si2 C6 105.9(5) . . ? C5 Si2 C6 106.0(5) . . ? C1 Si3 C8 113.6(4) . . ? C1 Si3 C9 114.0(4) . . ? C8 Si3 C9 107.4(5) . . ? C1 Si3 C10 113.1(5) . . ? C8 Si3 C10 105.5(4) . . ? C9 Si3 C10 102.4(4) . . ? C12 Si4 C14 115.2(5) . . ? C12 Si4 C13 112.5(5) . . ? C14 Si4 C13 103.4(7) . . ? C12 Si4 C15 113.8(5) . . ? C14 Si4 C15 105.1(5) . . ? C13 Si4 C15 105.7(6) . . ? C12 Si5 C17 114.4(4) . . ? C12 Si5 C18 114.4(5) . . ? C17 Si5 C18 105.9(6) . . ? C12 Si5 C16 113.3(5) . . ? C17 Si5 C16 101.7(6) . . ? C18 Si5 C16 105.9(6) . . ? C12 Si6 C19 112.5(4) . . ? C12 Si6 C20 113.4(4) . . ? C19 Si6 C20 106.5(5) . . ? C12 Si6 C21 114.0(4) . . ? C19 Si6 C21 104.4(5) . . ? C20 Si6 C21 105.3(5) . . ? C39 Si7 C40 114.0(5) . . ? C39 Si7 C41 114.0(5) . . ? C40 Si7 C41 107.0(6) . . ? C39 Si7 C42 112.7(5) . . ? C40 Si7 C42 103.7(6) . . ? C41 Si7 C42 104.4(5) . . ? C39 Si8 C43 114.9(5) . . ? C39 Si8 C44 113.3(5) . . ? C43 Si8 C44 102.2(5) . . ? C39 Si8 C45 113.4(5) . . ? C43 Si8 C45 106.0(6) . . ? C44 Si8 C45 105.9(5) . . ? C39 Si9 C48 113.7(6) . . ? C39 Si9 C47 113.6(6) . . ? C48 Si9 C47 102.1(8) . . ? C39 Si9 C46 114.2(5) . . ? C48 Si9 C46 108.8(6) . . ? C47 Si9 C46 103.1(6) . . ? C23 O1 C26 109.7(8) . . ? C23 O1 Li1 126.7(8) . . ? C26 O1 Li1 123.2(8) . . ? C30 O2 C27 107.6(11) . . ? C30 O2 Li1 129.2(9) . . ? C27 O2 Li1 123.1(11) . . ? C34 O3 C31 109.3(7) . . ? C34 O3 Li2 127.4(8) . . ? C31 O3 Li2 122.4(8) . . ? C35 O4 C38 107.0(9) . . ? C35 O4 Li2 125.0(8) . . ? C38 O4 Li2 124.2(9) . . ? C50 O5 C53 108.9(7) . . ? C50 O5 Li3 121.3(8) . . ? C53 O5 Li3 127.5(7) . . ? C54 O6 C57 108.5(8) . . ? C54 O6 Li3 125.6(8) . . ? C57 O6 Li3 124.4(8) . . ? C11 N1 Li2 166.9(9) . . ? C11 N1 Li1 109.6(8) . . ? Li2 N1 Li1 83.2(7) . . ? C22 N2 Li1 154.2(10) . . ? C22 N2 Li2 117.5(9) . . ? Li1 N2 Li2 83.6(7) . . ? C49 N3 Li3 163.5(9) . . ? C49 N3 Li3 111.2(8) . 2 ? Li3 N3 Li3 84.3(7) . 2 ? Si1 C1 Si3 114.9(5) . . ? Si1 C1 Si2 114.2(4) . . ? Si3 C1 Si2 113.2(5) . . ? Si1 C1 Cu1 102.7(4) . . ? Si3 C1 Cu1 104.2(4) . . ? Si2 C1 Cu1 106.1(4) . . ? N1 C11 Cu1 174.2(9) . . ? Si5 C12 Si6 113.5(5) . . ? Si5 C12 Si4 114.7(5) . . ? Si6 C12 Si4 113.9(5) . . ? Si5 C12 Cu2 100.4(4) . . ? Si6 C12 Cu2 104.1(4) . . ? Si4 C12 Cu2 108.5(4) . . ? N2 C22 Cu2 174.7(10) . . ? O1 C23 C24 106.5(9) . . ? C25 C24 C23 106.4(11) . . ? C24 C25 C26 110.1(12) . . ? O1 C26 C25 107.2(10) . . ? O2 C27 C28 106.0(16) . . ? C29 C28 C27 102.9(15) . . ? C28 C29 C30 109(2) . . ? O2 C30 C29 105.9(15) . . ? O3 C31 C32 105.5(9) . . ? C33 C32 C31 107.5(10) . . ? C32 C33 C34 108.0(11) . . ? O3 C34 C33 106.5(9) . . ? O4 C35 C36 107.8(11) . . ? C35 C36 C37 105.3(13) . . ? C36 C37 C38 105.8(13) . . ? O4 C38 C37 107.5(11) . . ? Si7 C39 Si9 114.6(5) . . ? Si7 C39 Si8 114.5(5) . . ? Si9 C39 Si8 115.2(5) . . ? Si7 C39 Cu3 102.9(5) . . ? Si9 C39 Cu3 103.9(4) . . ? Si8 C39 Cu3 103.6(4) . . ? N3 C49 Cu3 176.3(9) . . ? O5 C50 C51 106.3(8) . . ? C52 C51 C50 108.8(10) . . ? C51 C52 C53 107.9(9) . . ? O5 C53 C52 105.2(8) . . ? O6 C54 C55 107.8(10) . . ? C56 C55 C54 106.2(11) . . ? C57 C56 C55 108.2(11) . . ? C56 C57 O6 108.9(10) . . ? #===END data_nov1098-JDS1E _database_code_CSD 188684 _audit_creation_date 2002-03-04T15:52:15-00:00 _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 _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common ; [{(Me2NSiMe2)(Me3Si)2CCuCNLi(thf)2}2] ; _chemical_formula_moiety 'C40 H92 Cu2 Li2 N4 O4 Si6' _chemical_formula_sum 'C40 H92 Cu2 Li2 N4 O4 Si6' _chemical_formula_weight 1002.68 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.344(6) _cell_length_b 13.797(12) _cell_length_c 16.934(12) _cell_angle_alpha 103.59(7) _cell_angle_beta 94.01(5) _cell_angle_gamma 106.63(6) _cell_volume 2872(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scans' _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0802 _diffrn_reflns_number 7019 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 22.02 _diffrn_reflns_theta_full 22.02 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 7019 _reflns_number_gt 4889 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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^)+(0.1235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding' _refine_ls_extinction_method none _refine_ls_number_reflns 7019 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1908 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.005 _refine_diff_density_min -0.72 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 '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' Si Si 0.0817 0.0704 '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 Cu1 Cu 0.35607(6) 0.26986(7) 0.00038(5) 0.0340(3) Uani 1 1 d . . . Cu2 Cu 0.67322(6) 0.18204(6) 0.44280(5) 0.0333(3) Uani 1 1 d . . . Si1 Si 0.21582(16) 0.38805(16) -0.06292(13) 0.0404(5) Uani 1 1 d . . . Si2 Si 0.30151(15) 0.22825(16) -0.17831(12) 0.0377(5) Uani 1 1 d . . . Si3 Si 0.13659(15) 0.15346(16) -0.06635(12) 0.0399(5) Uani 1 1 d . . . Si4 Si 0.81654(14) 0.10364(14) 0.54221(11) 0.0288(5) Uani 1 1 d . . . Si5 Si 0.65837(16) 0.21220(16) 0.62268(12) 0.0376(5) Uani 1 1 d . . . Si6 Si 0.85303(16) 0.33867(15) 0.55778(12) 0.0391(5) Uani 1 1 d . . . O1 O 0.3264(4) 0.1834(5) 0.2524(3) 0.0589(15) Uani 1 1 d . . . O2 O 0.3684(4) -0.0022(4) 0.1320(3) 0.0560(15) Uani 1 1 d . . . O3 O 0.7610(4) 0.2850(4) 0.2032(4) 0.0566(15) Uani 1 1 d . . . O4 O 0.6341(4) 0.4272(4) 0.2929(3) 0.0591(15) Uani 1 1 d . . . N1 N 0.5055(5) 0.2472(5) 0.1307(4) 0.0479(17) Uani 1 1 d . . . N2 N 0.5569(5) 0.1710(5) 0.2817(4) 0.0525(17) Uani 1 1 d . . . N3 N 0.2046(5) 0.4364(5) 0.0382(4) 0.0480(16) Uani 1 1 d . . . N4 N 0.9197(4) 0.1171(5) 0.4849(3) 0.0374(14) Uani 1 1 d . . . C1 C 0.2453(5) 0.2635(5) -0.0831(4) 0.0322(16) Uani 1 1 d . . . C2 C 0.0865(6) 0.3752(7) -0.1244(5) 0.060(2) Uani 1 1 d . . . H2A H 0.0736 0.4432 -0.1121 0.09 Uiso 1 1 calc R . . H2B H 0.0287 0.3233 -0.1099 0.09 Uiso 1 1 calc R . . H2C H 0.0903 0.3523 -0.1832 0.09 Uiso 1 1 calc R . . C3 C 0.3185(7) 0.4943(6) -0.0906(6) 0.065(3) Uani 1 1 d . . . H3A H 0.2988 0.5588 -0.0787 0.098 Uiso 1 1 calc R . . H3B H 0.3234 0.4726 -0.1492 0.098 Uiso 1 1 calc R . . H3C H 0.3871 0.507 -0.0583 0.098 Uiso 1 1 calc R . . C4 C 0.1278(8) 0.4896(8) 0.0641(6) 0.089(3) Uani 1 1 d . . . H4A H 0.0673 0.4664 0.0203 0.134 Uiso 1 1 calc R . . H4B H 0.1608 0.5656 0.0754 0.134 Uiso 1 1 calc R . . H4C H 0.1035 0.4725 0.1139 0.134 Uiso 1 1 calc R . . C5 C 0.2931(7) 0.4689(8) 0.1020(6) 0.086(3) Uani 1 1 d . . . H5A H 0.3442 0.4326 0.0842 0.129 Uiso 1 1 calc R . . H5B H 0.2687 0.4513 0.1517 0.129 Uiso 1 1 calc R . . H5C H 0.3268 0.5449 0.1139 0.129 Uiso 1 1 calc R . . C6 C 0.2254(7) 0.2372(7) -0.2723(4) 0.059(2) Uani 1 1 d . . . H6A H 0.2597 0.2175 -0.3202 0.089 Uiso 1 1 calc R . . H6B H 0.2238 0.3093 -0.265 0.089 Uiso 1 1 calc R . . H6C H 0.153 0.1894 -0.2808 0.089 Uiso 1 1 calc R . . C7 C 0.4416(6) 0.3109(7) -0.1717(5) 0.061(2) Uani 1 1 d . . . H7A H 0.4676 0.2891 -0.2236 0.091 Uiso 1 1 calc R . . H7B H 0.4855 0.3021 -0.1268 0.091 Uiso 1 1 calc R . . H7C H 0.4451 0.3848 -0.1614 0.091 Uiso 1 1 calc R . . C8 C 0.3096(7) 0.0915(6) -0.2049(5) 0.057(2) Uani 1 1 d . . . H8A H 0.34 0.0785 -0.2559 0.086 Uiso 1 1 calc R . . H8B H 0.2386 0.0413 -0.2123 0.086 Uiso 1 1 calc R . . H8C H 0.3545 0.0829 -0.1604 0.086 Uiso 1 1 calc R . . C9 C 0.1864(7) 0.0520(6) -0.0332(5) 0.058(2) Uani 1 1 d . . . H9A H 0.1265 -0.0038 -0.0254 0.088 Uiso 1 1 calc R . . H9B H 0.235 0.0852 0.0186 0.088 Uiso 1 1 calc R . . H9C H 0.2236 0.022 -0.0755 0.088 Uiso 1 1 calc R . . C10 C 0.0624(6) 0.1968(7) 0.0172(5) 0.059(2) Uani 1 1 d . . . H10A H 0.0067 0.1359 0.0231 0.089 Uiso 1 1 calc R . . H10B H 0.0305 0.2476 0.0035 0.089 Uiso 1 1 calc R . . H10C H 0.111 0.2297 0.069 0.089 Uiso 1 1 calc R . . C11 C 0.0340(6) 0.0773(6) -0.1586(5) 0.061(2) Uani 1 1 d . . . H11A H -0.0195 0.0214 -0.1443 0.092 Uiso 1 1 calc R . . H11B H 0.0677 0.0463 -0.2032 0.092 Uiso 1 1 calc R . . H11C H 0.0002 0.1244 -0.1766 0.092 Uiso 1 1 calc R . . C12 C 0.4525(5) 0.2592(6) 0.0809(4) 0.0404(19) Uani 1 1 d . . . C13 C 0.7543(5) 0.2098(5) 0.5486(4) 0.0278(15) Uani 1 1 d . . . C14 C 0.7207(5) -0.0299(5) 0.4922(4) 0.0405(18) Uani 1 1 d . . . H14A H 0.7569 -0.0829 0.49 0.061 Uiso 1 1 calc R . . H14B H 0.6929 -0.0327 0.4363 0.061 Uiso 1 1 calc R . . H14C H 0.6622 -0.044 0.5241 0.061 Uiso 1 1 calc R . . C15 C 0.8728(6) 0.0997(6) 0.6462(4) 0.0382(18) Uani 1 1 d . . . H15A H 0.9048 0.0431 0.6396 0.057 Uiso 1 1 calc R . . H15B H 0.8162 0.0871 0.6799 0.057 Uiso 1 1 calc R . . H15C H 0.9268 0.167 0.6732 0.057 Uiso 1 1 calc R . . C16 C 0.8994(6) 0.0836(6) 0.3966(5) 0.054(2) Uani 1 1 d . . . H16A H 0.8235 0.0657 0.3782 0.081 Uiso 1 1 calc R . . H16B H 0.9223 0.0218 0.3771 0.081 Uiso 1 1 calc R . . H16C H 0.9386 0.1404 0.3744 0.081 Uiso 1 1 calc R . . C17 C 1.0307(5) 0.1450(6) 0.5161(5) 0.048(2) Uani 1 1 d . . . H17A H 1.041 0.1681 0.5763 0.072 Uiso 1 1 calc R . . H17B H 1.0712 0.2021 0.4948 0.072 Uiso 1 1 calc R . . H17C H 1.0551 0.0839 0.4985 0.072 Uiso 1 1 calc R . . C18 C 0.7246(7) 0.2871(6) 0.7309(4) 0.055(2) Uani 1 1 d . . . H18A H 0.6709 0.2863 0.7676 0.083 Uiso 1 1 calc R . . H18B H 0.7625 0.3598 0.7322 0.083 Uiso 1 1 calc R . . H18C H 0.7746 0.254 0.7491 0.083 Uiso 1 1 calc R . . C19 C 0.5782(6) 0.0804(6) 0.6310(5) 0.048(2) Uani 1 1 d . . . H19A H 0.5298 0.0891 0.6711 0.071 Uiso 1 1 calc R . . H19B H 0.6255 0.0443 0.6489 0.071 Uiso 1 1 calc R . . H19C H 0.5374 0.0386 0.5773 0.071 Uiso 1 1 calc R . . C20 C 0.5565(6) 0.2722(7) 0.5943(5) 0.060(2) Uani 1 1 d . . . H20A H 0.5077 0.2718 0.635 0.09 Uiso 1 1 calc R . . H20B H 0.5171 0.2316 0.54 0.09 Uiso 1 1 calc R . . H20C H 0.5915 0.3447 0.5933 0.09 Uiso 1 1 calc R . . C21 C 0.9073(6) 0.3463(6) 0.4601(5) 0.054(2) Uani 1 1 d . . . H21A H 0.9591 0.4156 0.4677 0.081 Uiso 1 1 calc R . . H21B H 0.8496 0.3352 0.4165 0.081 Uiso 1 1 calc R . . H21C H 0.9417 0.292 0.4446 0.081 Uiso 1 1 calc R . . C22 C 0.7982(7) 0.4506(6) 0.5822(5) 0.061(2) Uani 1 1 d . . . H22A H 0.8542 0.5162 0.5861 0.091 Uiso 1 1 calc R . . H22B H 0.771 0.4541 0.6348 0.091 Uiso 1 1 calc R . . H22C H 0.7408 0.4402 0.5387 0.091 Uiso 1 1 calc R . . C23 C 0.9703(6) 0.3784(6) 0.6395(5) 0.065(3) Uani 1 1 d . . . H23A H 1.0177 0.4473 0.6393 0.097 Uiso 1 1 calc R . . H23B H 1.0081 0.3265 0.6287 0.097 Uiso 1 1 calc R . . H23C H 0.9464 0.3824 0.6933 0.097 Uiso 1 1 calc R . . C24 C 0.6004(5) 0.1706(6) 0.3427(4) 0.0382(18) Uani 1 1 d . . . C25 C 0.3137(9) 0.1828(9) 0.3350(6) 0.090(3) Uani 1 1 d . . . H25A H 0.3824 0.2178 0.3714 0.108 Uiso 1 1 calc R . . H25B H 0.2866 0.1098 0.3393 0.108 Uiso 1 1 calc R . . C26 C 0.2397(13) 0.2383(14) 0.3587(8) 0.148(6) Uani 1 1 d . . . H26A H 0.1829 0.1957 0.3824 0.177 Uiso 1 1 calc R . . H26B H 0.276 0.3054 0.4004 0.177 Uiso 1 1 calc R . . C27 C 0.1975(12) 0.2570(15) 0.2887(9) 0.163(7) Uani 1 1 d . . . H27A H 0.2101 0.3333 0.2974 0.196 Uiso 1 1 calc R . . H27B H 0.1202 0.2214 0.2772 0.196 Uiso 1 1 calc R . . C28 C 0.2458(7) 0.2185(9) 0.2203(6) 0.084(3) Uani 1 1 d . . . H28A H 0.1929 0.1599 0.1789 0.101 Uiso 1 1 calc R . . H28B H 0.2766 0.275 0.194 0.101 Uiso 1 1 calc R . . C29 C 0.2703(8) -0.0716(7) 0.1404(6) 0.074(3) Uani 1 1 d . . . H29A H 0.2137 -0.039 0.1363 0.089 Uiso 1 1 calc R . . H29B H 0.2752 -0.0862 0.1948 0.089 Uiso 1 1 calc R . . C30 C 0.2450(8) -0.1703(7) 0.0748(6) 0.081(3) Uani 1 1 d . . . H30A H 0.2101 -0.2315 0.0949 0.097 Uiso 1 1 calc R . . H30B H 0.1985 -0.1692 0.027 0.097 Uiso 1 1 calc R . . C31 C 0.3465(10) -0.1729(10) 0.0538(9) 0.120(5) Uani 1 1 d . . . H31A H 0.3407 -0.209 -0.005 0.144 Uiso 1 1 calc R . . H31B H 0.3778 -0.2098 0.0873 0.144 Uiso 1 1 calc R . . C32 C 0.4116(9) -0.0611(11) 0.0717(9) 0.129(5) Uani 1 1 d . . . H32A H 0.4858 -0.0524 0.0922 0.154 Uiso 1 1 calc R . . H32B H 0.4105 -0.0367 0.0212 0.154 Uiso 1 1 calc R . . C33 C 0.7898(8) 0.1915(7) 0.1986(8) 0.092(4) Uani 1 1 d . . . H33A H 0.7671 0.162 0.2448 0.11 Uiso 1 1 calc R . . H33B H 0.7549 0.1381 0.1465 0.11 Uiso 1 1 calc R . . C34 C 0.9026(7) 0.2186(7) 0.2029(6) 0.069(3) Uani 1 1 d . . . H34A H 0.9334 0.1999 0.2499 0.082 Uiso 1 1 calc R . . H34B H 0.9216 0.1806 0.1518 0.082 Uiso 1 1 calc R . . C35 C 0.9414(7) 0.3292(8) 0.2132(8) 0.093(4) Uani 1 1 d . . . H35A H 0.9962 0.3458 0.1777 0.111 Uiso 1 1 calc R . . H35B H 0.973 0.3658 0.271 0.111 Uiso 1 1 calc R . . C36 C 0.8504(7) 0.3626(7) 0.1901(7) 0.074(3) Uani 1 1 d . . . H36A H 0.8565 0.4331 0.2251 0.089 Uiso 1 1 calc R . . H36B H 0.8451 0.3643 0.1318 0.089 Uiso 1 1 calc R . . C37 C 0.5410(9) 0.4514(9) 0.3108(7) 0.097(4) Uani 1 1 d . . . H37A H 0.4784 0.3877 0.2938 0.116 Uiso 1 1 calc R . . H37B H 0.5299 0.5038 0.2829 0.116 Uiso 1 1 calc R . . C38 C 0.5609(16) 0.4953(12) 0.4019(10) 0.159(8) Uani 1 1 d . . . H38A H 0.5512 0.4391 0.4305 0.19 Uiso 1 1 calc R . . H38B H 0.5142 0.5378 0.4205 0.19 Uiso 1 1 calc R . . C39 C 0.6739(17) 0.5620(10) 0.4152(8) 0.155(8) Uani 1 1 d . . . H39A H 0.6814 0.6291 0.401 0.187 Uiso 1 1 calc R . . H39B H 0.7078 0.5765 0.4724 0.187 Uiso 1 1 calc R . . C40 C 0.7176(9) 0.4916(9) 0.3561(7) 0.096(4) Uani 1 1 d . . . H40A H 0.7754 0.5338 0.333 0.115 Uiso 1 1 calc R . . H40B H 0.7462 0.4479 0.3844 0.115 Uiso 1 1 calc R . . Li1 Li 0.4302(9) 0.1367(11) 0.1945(8) 0.049(3) Uani 1 1 d . . . Li2 Li 0.6253(9) 0.2919(10) 0.2238(8) 0.044(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0267(5) 0.0441(5) 0.0334(5) 0.0197(4) -0.0028(4) 0.0085(4) Cu2 0.0303(5) 0.0408(5) 0.0322(5) 0.0193(4) -0.0027(4) 0.0101(4) Si1 0.0383(12) 0.0368(12) 0.0525(13) 0.0231(10) 0.0067(10) 0.0124(10) Si2 0.0370(12) 0.0484(13) 0.0332(12) 0.0203(10) 0.0050(9) 0.0144(10) Si3 0.0305(11) 0.0406(12) 0.0431(12) 0.0194(10) -0.0003(9) -0.0026(9) Si4 0.0255(10) 0.0355(11) 0.0281(10) 0.0144(9) 0.0000(8) 0.0098(8) Si5 0.0369(12) 0.0454(12) 0.0374(12) 0.0163(10) 0.0108(9) 0.0180(10) Si6 0.0411(12) 0.0322(11) 0.0404(12) 0.0113(9) 0.0016(10) 0.0056(9) O1 0.052(4) 0.084(4) 0.054(4) 0.030(3) 0.016(3) 0.031(3) O2 0.041(3) 0.065(4) 0.057(4) 0.017(3) 0.009(3) 0.008(3) O3 0.038(3) 0.038(3) 0.097(4) 0.022(3) 0.002(3) 0.015(3) O4 0.055(4) 0.061(4) 0.070(4) 0.022(3) 0.007(3) 0.027(3) N1 0.029(3) 0.071(5) 0.047(4) 0.035(4) -0.007(3) 0.008(3) N2 0.048(4) 0.064(5) 0.049(4) 0.029(4) -0.004(3) 0.013(3) N3 0.044(4) 0.041(4) 0.058(4) 0.006(3) 0.002(3) 0.020(3) N4 0.034(3) 0.059(4) 0.027(3) 0.018(3) 0.006(3) 0.020(3) C1 0.026(4) 0.034(4) 0.038(4) 0.021(3) -0.002(3) 0.002(3) C2 0.062(6) 0.064(6) 0.067(6) 0.027(5) 0.000(5) 0.035(5) C3 0.076(6) 0.041(5) 0.089(7) 0.042(5) 0.020(5) 0.013(5) C4 0.090(8) 0.096(8) 0.085(8) 0.003(6) 0.015(6) 0.052(7) C5 0.076(7) 0.099(8) 0.071(7) -0.017(6) -0.023(6) 0.048(6) C6 0.075(6) 0.085(6) 0.032(5) 0.029(4) 0.011(4) 0.034(5) C7 0.040(5) 0.086(7) 0.059(6) 0.030(5) 0.018(4) 0.012(5) C8 0.067(6) 0.061(6) 0.054(5) 0.014(4) 0.013(4) 0.035(5) C9 0.060(5) 0.042(5) 0.066(6) 0.028(4) -0.004(4) -0.004(4) C10 0.043(5) 0.064(6) 0.069(6) 0.032(5) 0.011(4) 0.002(4) C11 0.040(5) 0.060(6) 0.070(6) 0.023(5) -0.002(4) -0.007(4) C12 0.025(4) 0.052(5) 0.043(5) 0.029(4) -0.003(4) -0.002(3) C13 0.027(4) 0.032(4) 0.027(4) 0.010(3) 0.005(3) 0.012(3) C14 0.041(4) 0.041(4) 0.044(4) 0.017(4) 0.006(4) 0.016(4) C15 0.041(4) 0.049(5) 0.037(4) 0.020(4) 0.008(3) 0.024(4) C16 0.054(5) 0.065(6) 0.056(5) 0.025(4) 0.020(4) 0.030(4) C17 0.028(4) 0.067(5) 0.054(5) 0.016(4) 0.009(4) 0.021(4) C18 0.070(6) 0.066(6) 0.033(4) 0.010(4) 0.021(4) 0.024(5) C19 0.032(4) 0.059(5) 0.050(5) 0.023(4) 0.006(4) 0.006(4) C20 0.055(5) 0.072(6) 0.078(6) 0.036(5) 0.025(5) 0.040(5) C21 0.055(5) 0.037(4) 0.065(6) 0.022(4) 0.013(4) -0.002(4) C22 0.072(6) 0.034(5) 0.075(6) 0.021(4) 0.017(5) 0.008(4) C23 0.060(6) 0.049(5) 0.068(6) 0.019(4) -0.009(5) -0.008(4) C24 0.035(4) 0.046(5) 0.037(5) 0.024(4) 0.000(4) 0.009(3) C25 0.104(9) 0.120(9) 0.083(8) 0.057(7) 0.049(7) 0.061(8) C26 0.159(14) 0.232(19) 0.096(11) 0.049(11) 0.063(10) 0.112(14) C27 0.138(13) 0.28(2) 0.128(13) 0.033(13) 0.017(10) 0.169(15) C28 0.057(6) 0.131(9) 0.082(7) 0.041(7) 0.012(5) 0.047(6) C29 0.074(7) 0.062(6) 0.092(8) 0.033(6) 0.027(6) 0.016(5) C30 0.078(7) 0.063(7) 0.089(8) 0.014(6) 0.006(6) 0.009(5) C31 0.096(10) 0.091(10) 0.157(13) -0.008(8) 0.029(9) 0.038(8) C32 0.071(8) 0.130(12) 0.163(13) -0.006(10) 0.063(9) 0.025(8) C33 0.070(7) 0.054(6) 0.168(11) 0.040(7) 0.043(7) 0.030(5) C34 0.067(6) 0.072(7) 0.085(7) 0.035(5) 0.017(5) 0.036(5) C35 0.043(6) 0.082(8) 0.144(10) 0.014(7) 0.023(6) 0.019(5) C36 0.062(6) 0.046(5) 0.111(8) 0.039(5) 0.002(6) 0.001(5) C37 0.097(9) 0.110(9) 0.115(10) 0.040(8) 0.036(7) 0.068(8) C38 0.30(2) 0.116(13) 0.150(15) 0.069(11) 0.160(16) 0.138(15) C39 0.33(3) 0.071(9) 0.077(9) 0.019(8) 0.037(13) 0.084(13) C40 0.114(10) 0.080(8) 0.083(8) 0.003(6) -0.017(7) 0.035(7) Li1 0.035(7) 0.071(9) 0.048(8) 0.033(7) 0.004(6) 0.013(6) Li2 0.024(6) 0.054(8) 0.051(8) 0.018(6) -0.010(5) 0.006(6) #----------------------------------------------------------------------------# # 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 Cu1 C12 1.870(7) . ? Cu1 C1 1.941(6) . ? Cu2 C24 1.843(7) . ? Cu2 C13 1.922(6) . ? Si1 N3 1.719(7) . ? Si1 C1 1.832(7) . ? Si1 C3 1.873(8) . ? Si1 C2 1.892(8) . ? Si2 C1 1.846(7) . ? Si2 C7 1.870(8) . ? Si2 C8 1.871(8) . ? Si2 C6 1.875(7) . ? Si3 C10 1.865(8) . ? Si3 C1 1.868(7) . ? Si3 C11 1.878(8) . ? Si3 C9 1.889(8) . ? Si4 N4 1.731(6) . ? Si4 C13 1.866(6) . ? Si4 C14 1.875(7) . ? Si4 C15 1.885(7) . ? Si5 C13 1.857(6) . ? Si5 C19 1.871(8) . ? Si5 C20 1.871(7) . ? Si5 C18 1.889(8) . ? Si6 C13 1.849(7) . ? Si6 C21 1.865(8) . ? Si6 C22 1.865(8) . ? Si6 C23 1.875(8) . ? O1 C25 1.423(10) . ? O1 C28 1.425(10) . ? O1 Li1 1.923(14) . ? O2 C32 1.413(11) . ? O2 C29 1.422(10) . ? O2 Li1 1.869(15) . ? O3 C36 1.427(9) . ? O3 C33 1.436(10) . ? O3 Li2 1.892(13) . ? O4 C37 1.411(11) . ? O4 C40 1.413(11) . ? O4 Li2 1.923(14) . ? N1 C12 1.135(8) . ? N1 Li2 2.012(12) . ? N1 Li1 2.133(14) . ? N2 C24 1.151(8) . ? N2 Li1 2.032(13) . ? N2 Li2 2.144(14) . ? N3 C5 1.433(10) . ? N3 C4 1.458(10) . ? N4 C16 1.439(9) . ? N4 C17 1.445(8) . ? C25 C26 1.437(15) . ? C26 C27 1.387(17) . ? C27 C28 1.431(15) . ? C29 C30 1.475(12) . ? C30 C31 1.432(14) . ? C31 C32 1.484(16) . ? C33 C34 1.435(12) . ? C34 C35 1.427(13) . ? C35 C36 1.477(12) . ? C37 C38 1.493(17) . ? C38 C39 1.49(2) . ? C39 C40 1.494(16) . ? Li1 Li2 2.782(17) . ? 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 C12 Cu1 C1 172.8(3) . . ? C24 Cu2 C13 173.9(3) . . ? N3 Si1 C1 113.3(3) . . ? N3 Si1 C3 106.5(4) . . ? C1 Si1 C3 112.9(4) . . ? N3 Si1 C2 105.9(4) . . ? C1 Si1 C2 111.9(3) . . ? C3 Si1 C2 105.7(4) . . ? C1 Si2 C7 112.7(3) . . ? C1 Si2 C8 114.2(3) . . ? C7 Si2 C8 103.2(4) . . ? C1 Si2 C6 114.0(3) . . ? C7 Si2 C6 107.1(4) . . ? C8 Si2 C6 104.7(4) . . ? C10 Si3 C1 113.3(3) . . ? C10 Si3 C11 105.8(4) . . ? C1 Si3 C11 115.1(3) . . ? C10 Si3 C9 104.0(4) . . ? C1 Si3 C9 112.8(3) . . ? C11 Si3 C9 104.9(4) . . ? C10 Si3 Cu1 103.8(3) . . ? N4 Si4 C13 112.7(3) . . ? N4 Si4 C14 105.6(3) . . ? C13 Si4 C14 112.4(3) . . ? N4 Si4 C15 106.2(3) . . ? C13 Si4 C15 112.6(3) . . ? C14 Si4 C15 106.8(3) . . ? C13 Si5 C19 115.1(3) . . ? C13 Si5 C20 112.3(3) . . ? C19 Si5 C20 103.7(4) . . ? C13 Si5 C18 112.5(3) . . ? C19 Si5 C18 105.0(4) . . ? C20 Si5 C18 107.6(4) . . ? C13 Si6 C21 112.2(3) . . ? C13 Si6 C22 113.5(3) . . ? C21 Si6 C22 104.4(4) . . ? C13 Si6 C23 115.8(3) . . ? C21 Si6 C23 106.1(4) . . ? C22 Si6 C23 103.7(4) . . ? C25 O1 C28 107.9(7) . . ? C25 O1 Li1 125.0(6) . . ? C28 O1 Li1 127.1(6) . . ? C32 O2 C29 106.5(7) . . ? C32 O2 Li1 127.5(7) . . ? C29 O2 Li1 125.8(6) . . ? C36 O3 C33 107.6(6) . . ? C36 O3 Li2 130.5(6) . . ? C33 O3 Li2 121.9(6) . . ? C37 O4 C40 108.5(8) . . ? C37 O4 Li2 120.1(7) . . ? C40 O4 Li2 126.2(6) . . ? C12 N1 Li2 155.4(7) . . ? C12 N1 Li1 116.0(6) . . ? Li2 N1 Li1 84.3(5) . . ? C24 N2 Li1 155.8(7) . . ? C24 N2 Li2 119.1(6) . . ? Li1 N2 Li2 83.5(5) . . ? C5 N3 C4 110.0(7) . . ? C5 N3 Si1 121.5(6) . . ? C4 N3 Si1 123.5(6) . . ? C16 N4 C17 112.2(6) . . ? C16 N4 Si4 120.8(5) . . ? C17 N4 Si4 126.3(5) . . ? Si1 C1 Si2 115.9(3) . . ? Si1 C1 Si3 113.2(4) . . ? Si2 C1 Si3 114.1(4) . . ? Si1 C1 Cu1 110.4(3) . . ? Si2 C1 Cu1 101.9(3) . . ? Si3 C1 Cu1 99.3(3) . . ? N1 C12 Cu1 175.3(6) . . ? Si6 C13 Si5 114.4(3) . . ? Si6 C13 Si4 112.1(3) . . ? Si5 C13 Si4 114.6(3) . . ? Si6 C13 Cu2 102.2(3) . . ? Si5 C13 Cu2 105.3(3) . . ? Si4 C13 Cu2 106.8(3) . . ? N2 C24 Cu2 175.2(7) . . ? O1 C25 C26 107.3(9) . . ? C27 C26 C25 107.5(11) . . ? C26 C27 C28 109.7(10) . . ? O1 C28 C27 106.3(8) . . ? O2 C29 C30 108.9(8) . . ? C31 C30 C29 103.3(9) . . ? C30 C31 C32 105.0(9) . . ? O2 C32 C31 107.7(9) . . ? C34 C33 O3 108.1(8) . . ? C35 C34 C33 106.7(8) . . ? C34 C35 C36 107.1(8) . . ? O3 C36 C35 104.2(7) . . ? O4 C37 C38 103.5(10) . . ? C37 C38 C39 101.4(11) . . ? C40 C39 C38 100.1(11) . . ? O4 C40 C39 107.5(11) . . ? O2 Li1 O1 109.2(6) . . ? O2 Li1 N2 118.9(7) . . ? O1 Li1 N2 105.1(7) . . ? O2 Li1 N1 116.7(7) . . ? O1 Li1 N1 110.1(7) . . ? N2 Li1 N1 95.7(6) . . ? O2 Li1 Li2 138.0(7) . . ? O1 Li1 Li2 112.8(7) . . ? N2 Li1 Li2 50.0(4) . . ? N1 Li1 Li2 46.0(4) . . ? O3 Li2 O4 111.0(6) . . ? O3 Li2 N1 120.5(7) . . ? O4 Li2 N1 109.7(6) . . ? O3 Li2 N2 108.1(6) . . ? O4 Li2 N2 110.4(7) . . ? N1 Li2 N2 96.0(5) . . ? O3 Li2 Li1 131.5(7) . . ? O4 Li2 Li1 116.6(6) . . ? N1 Li2 Li1 49.7(4) . . ? N2 Li2 Li1 46.5(4) . . ? #===END data_apr999-JDS3 _database_code_CSD 188685 _audit_creation_date 1999-04-13T10:16:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H70 Cu2 Li2 N2 O6 Si6' _chemical_formula_structural 'C30 H70 CU2 LI2 N2 O6 SI6' _chemical_formula_sum 'C30 H70 Cu2 Li2 N2 O6 Si6' _chemical_formula_weight 864.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.916(9) _cell_length_b 9.4377(19) _cell_length_c 17.892(4) _cell_angle_alpha 90 _cell_angle_beta 109.06(2) _cell_angle_gamma 90 _cell_volume 4775(2) _cell_formula_units_Z 4 _cell_measurement_temperature 239(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.5 _cell_measurement_theta_max 7.1 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_factor_muR 0.175 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 1 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.7384 _exptl_absorpt_correction_T_max 0.8135 _exptl_absorpt_correction_T_ave 0.7946 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 239(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.3881E-2 _diffrn_orient_matrix_ub_12 0.29627E-1 _diffrn_orient_matrix_ub_13 -0.51191E-1 _diffrn_orient_matrix_ub_21 -0.34183E-1 _diffrn_orient_matrix_ub_22 -0.20483E-1 _diffrn_orient_matrix_ub_23 -0.28053E-1 _diffrn_orient_matrix_ub_31 -0.8197E-2 _diffrn_orient_matrix_ub_32 0.99648E-1 _diffrn_orient_matrix_ub_33 0.9446E-2 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -2 _diffrn_standards_decay_corr_max 1 _diffrn_standards_decay_corr_min 0.964 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 3 -2 7 3 -1 _diffrn_reflns_number 4275 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4199 _reflns_number_gt 2999 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 (Enraf Nonius, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin,Pearce & Prout, 1993)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # 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 _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 4199 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.573 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.076 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 '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' Si Si 0.0817 0.0704 '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 Cu Cu 0.414398(17) 0.38539(6) 0.16321(3) 0.04101(19) Uani 1 1 d . . . Li Li 0.4322(2) 0.2889(8) 0.3763(4) 0.0463(17) Uani 1 1 d . . . Si1 Si 0.38080(4) 0.56561(13) 0.27135(7) 0.0426(3) Uani 1 1 d . . . Si2 Si 0.34162(4) 0.26736(14) 0.23082(7) 0.0454(3) Uani 1 1 d . . . Si3 Si 0.31633(5) 0.49606(15) 0.09872(8) 0.0537(4) Uani 1 1 d . . . O1 O 0.40421(10) 0.4773(3) 0.35709(16) 0.0454(7) Uani 1 1 d . . . O2 O 0.38987(10) 0.1825(3) 0.28964(17) 0.0472(7) Uani 1 1 d . . . O3 O 0.42837(12) 0.1833(4) 0.46775(18) 0.0682(10) Uani 1 1 d . . . N N 0.50077(13) 0.3139(4) 0.1192(2) 0.0511(10) Uani 1 1 d . . . C1 C 0.35889(13) 0.4322(4) 0.1932(2) 0.0357(9) Uani 1 1 d . . . C2 C 0.43013(19) 0.6798(5) 0.2607(3) 0.0663(14) Uani 1 1 d . . . H2A H 0.4397 0.7475 0.3039 0.1 Uiso 1 1 calc R . . H2B H 0.4192 0.7303 0.2108 0.1 Uiso 1 1 calc R . . H2C H 0.4569 0.6205 0.262 0.1 Uiso 1 1 calc R . . C3 C 0.33477(19) 0.6871(6) 0.2863(3) 0.0752(17) Uani 1 1 d . . . H3A H 0.3496 0.7534 0.3285 0.113 Uiso 1 1 calc R . . H3B H 0.3113 0.6318 0.3001 0.113 Uiso 1 1 calc R . . H3C H 0.3196 0.739 0.2378 0.113 Uiso 1 1 calc R . . C4 C 0.4240(2) 0.5520(6) 0.4307(3) 0.0733(16) Uani 1 1 d . . . H4A H 0.4357 0.4843 0.4735 0.11 Uiso 1 1 calc R . . H4B H 0.3998 0.6106 0.4403 0.11 Uiso 1 1 calc R . . H4C H 0.4499 0.6115 0.428 0.11 Uiso 1 1 calc R . . C5 C 0.3099(2) 0.1342(6) 0.1543(4) 0.0819(19) Uani 1 1 d . . . H5A H 0.3023 0.0516 0.1801 0.123 Uiso 1 1 calc R . . H5B H 0.33 0.1064 0.1239 0.123 Uiso 1 1 calc R . . H5C H 0.2809 0.1758 0.1193 0.123 Uiso 1 1 calc R . . C6 C 0.30520(18) 0.2936(7) 0.2972(3) 0.0787(18) Uani 1 1 d . . . H6A H 0.2974 0.2022 0.3144 0.118 Uiso 1 1 calc R . . H6B H 0.2763 0.3433 0.2686 0.118 Uiso 1 1 calc R . . H6C H 0.323 0.3489 0.3429 0.118 Uiso 1 1 calc R . . C7 C 0.4143(2) 0.0773(6) 0.2618(3) 0.0755(17) Uani 1 1 d . . . H7A H 0.4408 0.0425 0.3054 0.113 Uiso 1 1 calc R . . H7B H 0.4259 0.1179 0.2218 0.113 Uiso 1 1 calc R . . H7C H 0.393 -0.0004 0.239 0.113 Uiso 1 1 calc R . . C8 C 0.25354(17) 0.5026(7) 0.0979(3) 0.0793(18) Uani 1 1 d . . . H8A H 0.2334 0.5368 0.0469 0.119 Uiso 1 1 calc R . . H8B H 0.2513 0.5661 0.1391 0.119 Uiso 1 1 calc R . . H8C H 0.2435 0.4084 0.1071 0.119 Uiso 1 1 calc R . . C9 C 0.31560(19) 0.3838(8) 0.0119(3) 0.086(2) Uani 1 1 d . . . H9A H 0.2928 0.4219 -0.0357 0.128 Uiso 1 1 calc R . . H9B H 0.3069 0.2876 0.0202 0.128 Uiso 1 1 calc R . . H9C H 0.3468 0.384 0.0063 0.128 Uiso 1 1 calc R . . C10 C 0.3321(2) 0.6780(7) 0.0718(4) 0.108(3) Uani 1 1 d . . . H10A H 0.309 0.7076 0.0222 0.161 Uiso 1 1 calc R . . H10B H 0.3633 0.6756 0.0662 0.161 Uiso 1 1 calc R . . H10C H 0.3321 0.7446 0.1131 0.161 Uiso 1 1 calc R . . C11 C 0.46761(16) 0.3419(5) 0.1344(2) 0.0454(11) Uani 1 1 d . . . C12 C 0.3979(2) 0.0663(7) 0.4645(3) 0.086(2) Uani 1 1 d . . . H12A H 0.401 -0.0033 0.4258 0.103 Uiso 1 1 calc R . . H12B H 0.365 0.0981 0.4486 0.103 Uiso 1 1 calc R . . C13 C 0.4117(3) 0.0029(8) 0.5430(4) 0.109(3) Uani 1 1 d . . . H13A H 0.4128 -0.1005 0.5393 0.13 Uiso 1 1 calc R . . H13B H 0.3889 0.0282 0.5698 0.13 Uiso 1 1 calc R . . C14 C 0.4585(3) 0.0591(8) 0.5866(4) 0.099(2) Uani 1 1 d . . . H14A H 0.4611 0.0796 0.6415 0.119 Uiso 1 1 calc R . . H14B H 0.4832 -0.0089 0.5863 0.119 Uiso 1 1 calc R . . C15 C 0.4630(2) 0.1895(8) 0.5450(3) 0.0851(19) Uani 1 1 d . . . H15A H 0.4574 0.2725 0.5737 0.102 Uiso 1 1 calc R . . H15B H 0.4948 0.1967 0.541 0.102 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 Cu 0.0358(3) 0.0473(3) 0.0412(3) -0.0012(2) 0.0143(2) 0.0018(2) Li 0.036(4) 0.056(5) 0.045(4) 0.010(4) 0.010(3) -0.001(3) Si1 0.0431(7) 0.0344(7) 0.0498(7) -0.0050(5) 0.0144(6) 0.0029(5) Si2 0.0383(7) 0.0440(7) 0.0491(7) 0.0000(6) 0.0078(5) -0.0088(5) Si3 0.0417(7) 0.0625(9) 0.0500(8) 0.0098(7) 0.0054(6) 0.0072(6) O1 0.0469(17) 0.0502(19) 0.0367(16) -0.0105(14) 0.0104(13) -0.0027(14) O2 0.0500(18) 0.0391(17) 0.0460(17) 0.0003(14) 0.0066(14) -0.0018(14) O3 0.067(2) 0.083(3) 0.048(2) 0.0196(18) 0.0089(17) -0.025(2) N 0.045(2) 0.059(3) 0.052(2) -0.002(2) 0.0190(18) 0.0037(19) C1 0.033(2) 0.035(2) 0.039(2) -0.0007(18) 0.0109(17) -0.0014(17) C2 0.073(4) 0.047(3) 0.078(4) -0.005(3) 0.022(3) -0.015(3) C3 0.079(4) 0.062(4) 0.084(4) -0.014(3) 0.025(3) 0.024(3) C4 0.087(4) 0.077(4) 0.050(3) -0.030(3) 0.015(3) -0.006(3) C5 0.076(4) 0.056(4) 0.084(4) -0.010(3) -0.014(3) -0.021(3) C6 0.054(3) 0.100(5) 0.093(4) 0.024(4) 0.040(3) -0.010(3) C7 0.087(4) 0.054(3) 0.070(4) -0.009(3) 0.005(3) 0.020(3) C8 0.050(3) 0.097(5) 0.082(4) -0.006(4) 0.009(3) 0.021(3) C9 0.058(3) 0.147(6) 0.045(3) -0.010(4) 0.007(2) 0.007(4) C10 0.111(5) 0.086(5) 0.101(5) 0.051(4) 0.001(4) -0.003(4) C11 0.041(2) 0.053(3) 0.040(2) 0.001(2) 0.012(2) 0.005(2) C12 0.096(5) 0.092(5) 0.065(4) 0.016(3) 0.021(3) -0.036(4) C13 0.114(6) 0.092(5) 0.124(6) 0.058(5) 0.044(5) 0.002(4) C14 0.119(6) 0.098(5) 0.068(4) 0.024(4) 0.014(4) 0.003(5) C15 0.081(4) 0.120(5) 0.046(3) 0.022(3) 0.008(3) -0.022(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 Cu C11 1.872(5) . ? Cu C1 1.955(4) . ? Li O2 1.932(8) . ? Li O1 1.948(8) . ? Li O3 1.950(8) . ? Li N 1.995(8) 2_655 ? Si1 O1 1.684(3) . ? Si1 C1 1.836(4) . ? Si1 C3 1.877(5) . ? Si1 C2 1.887(5) . ? Si2 O2 1.685(3) . ? Si2 C1 1.835(4) . ? Si2 C5 1.872(5) . ? Si2 C6 1.872(5) . ? Si3 C1 1.854(4) . ? Si3 C8 1.874(5) . ? Si3 C9 1.874(6) . ? Si3 C10 1.885(7) . ? O1 C4 1.440(5) . ? O2 C7 1.417(6) . ? O3 C12 1.420(6) . ? O3 C15 1.432(6) . ? N C11 1.142(5) . ? N Li 1.995(8) 2_655 ? C12 C13 1.458(8) . ? C13 C14 1.463(9) . ? C14 C15 1.467(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Cu C1 179.60(19) . . ? O2 Li O1 101.6(3) . . ? O2 Li O3 101.9(4) . . ? O1 Li O3 118.4(4) . . ? O2 Li N 118.7(4) . 2_655 ? O1 Li N 105.5(4) . 2_655 ? O3 Li N 111.1(4) . 2_655 ? O1 Si1 C1 107.05(17) . . ? O1 Si1 C3 106.2(2) . . ? C1 Si1 C3 115.5(2) . . ? O1 Si1 C2 105.6(2) . . ? C1 Si1 C2 114.3(2) . . ? C3 Si1 C2 107.4(3) . . ? O2 Si2 C1 110.23(17) . . ? O2 Si2 C5 105.3(2) . . ? C1 Si2 C5 115.9(2) . . ? O2 Si2 C6 102.9(2) . . ? C1 Si2 C6 114.4(2) . . ? C5 Si2 C6 106.9(3) . . ? C1 Si3 C8 114.0(2) . . ? C1 Si3 C9 113.0(2) . . ? C8 Si3 C9 105.7(3) . . ? C1 Si3 C10 112.0(2) . . ? C8 Si3 C10 107.5(3) . . ? C9 Si3 C10 103.8(3) . . ? C4 O1 Si1 121.0(3) . . ? C4 O1 Li 105.1(4) . . ? Si1 O1 Li 129.8(3) . . ? C7 O2 Si2 123.3(3) . . ? C7 O2 Li 111.6(4) . . ? Si2 O2 Li 117.2(3) . . ? C12 O3 C15 108.9(4) . . ? C12 O3 Li 125.1(4) . . ? C15 O3 Li 124.5(4) . . ? C11 N Li 163.3(4) . 2_655 ? Si2 C1 Si1 112.0(2) . . ? Si2 C1 Si3 114.7(2) . . ? Si1 C1 Si3 116.1(2) . . ? Si2 C1 Cu 106.0(2) . . ? Si1 C1 Cu 103.89(19) . . ? Si3 C1 Cu 102.42(19) . . ? N C11 Cu 177.9(4) . . ? O3 C12 C13 107.7(5) . . ? C12 C13 C14 106.5(5) . . ? C15 C14 C13 105.3(5) . . ? O3 C15 C14 107.4(5) . . ? #===END