# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1175 data_global _publ_contact_author ; R\"udiger Mews Institut f\"ur Anorganische und Physikalische Chemie Universit\"at Bremen Postfach 330 440 D-28334 Bremen ; _publ_contact_author_fax '049 421 218 4267' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Syntheses and structures of some homoleptic acetonitrile lanthanoid(III) complexes. ; loop_ _publ_author_name _publ_author_address ; 'Prof. Dr. Deacon, Glen B.' Department of Chemistry Monash University Clayton Victoria 3158 Australia ; 'Dipl. Chem. G\"ortler, Bernd' Institut f\"ur Anorganische und Physikalische Chemie Universit\"at Bremen Postfach 330 440 28334 Bremen Germany ; 'Dr. Junk, Peter C.' Department of Chemistry James Cook University Townsville Queensland 4811 Australia ; 'Dr. Lork, Enno' Institut f\"ur Anorganische und Physikalische Chemie Universit\"at Bremen Postfach 330 440 D-28334 Bremen ; 'Prof. Dr. Mews, R\"udiger' Institut f\"ur Anorganische und Physikalische Chemie Universit\"at Bremen Postfach 330 440 D-28334 Bremen ; 'Dr. Petersen, Jan' Institut f\"ur Anorganische und Physikalische Chemie Universit\"at Bremen Postfach 330 440 28334 Bremen Germany ; 'Prof. Dr. Zemva, Boris' Department of Inorganic Chemistry and Technology Jozef Stefan Institute Jamova 39 1000 Ljubljana Slovenia ; data_pet33 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 As3 F18 La N10' _chemical_formula_weight 1116.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6740(10) _cell_length_b 20.534(2) _cell_length_c 16.3120(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.590(10) _cell_angle_gamma 90.00 _cell_volume 4126.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 63 _cell_measurement_theta_min 14.840 _cell_measurement_theta_max 17.467 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 3.532 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.1432 _exptl_absorpt_correction_T_max 0.3324 _exptl_absorpt_process_details 'Walker & Stuart, 1983' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 10468 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5126 _reflns_number_gt 2967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Two of the three AsF6 anions (As2 with F7 to F18; As3 with F19 to F30) were built out of two slightly displaced octahedra. These two octahedra were fixed to an ideal geometry. 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5126 _refine_ls_number_parameters 588 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.002 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.78627(4) 0.146049(17) 0.15208(2) 0.03850(17) Uani 1 1 d . . . N1 N 0.8001(6) 0.1427(3) 0.3165(4) 0.049(3) Uani 1 1 d . . . C1 C 0.8112(9) 0.1391(3) 0.3850(5) 0.052(4) Uani 1 1 d . . . C10 C 0.8267(10) 0.1357(4) 0.4782(5) 0.082(5) Uani 1 1 d . . . H10A H 0.9045 0.1357 0.5050 0.135(7) Uiso 1 1 calc R . . H10B H 0.7938 0.0956 0.4932 0.135(7) Uiso 1 1 calc R . . H10C H 0.7922 0.1734 0.4978 0.135(7) Uiso 1 1 calc R . . N2 N 0.8192(5) 0.2672(3) 0.2055(4) 0.049(3) Uani 1 1 d . . . C2 C 0.8221(6) 0.3206(3) 0.2192(4) 0.048(3) Uani 1 1 d . . . C20 C 0.8267(8) 0.3900(3) 0.2404(5) 0.067(4) Uani 1 1 d . . . H20A H 0.7564 0.4103 0.2156 0.135(7) Uiso 1 1 calc R . . H20B H 0.8834 0.4111 0.2181 0.135(7) Uiso 1 1 calc R . . H20C H 0.8433 0.3952 0.3019 0.135(7) Uiso 1 1 calc R . . N3 N 0.9969(5) 0.1509(3) 0.2097(5) 0.057(3) Uani 1 1 d . . . C3 C 1.0875(7) 0.1475(4) 0.2208(6) 0.058(4) Uani 1 1 d . . . C30 C 1.2094(7) 0.1424(4) 0.2330(6) 0.084(5) Uani 1 1 d . . . H30A H 1.2359 0.1040 0.2674 0.135(7) Uiso 1 1 calc R . . H30B H 1.2439 0.1815 0.2616 0.135(7) Uiso 1 1 calc R . . H30C H 1.2272 0.1383 0.1779 0.135(7) Uiso 1 1 calc R . . N4 N 0.6268(5) 0.0595(3) 0.1309(4) 0.054(3) Uani 1 1 d . . . C4 C 0.5477(8) 0.0330(3) 0.1193(6) 0.062(4) Uani 1 1 d . . . C40 C 0.4430(7) 0.0000(4) 0.1070(6) 0.097(5) Uani 1 1 d . . . H40A H 0.4374 -0.0210 0.1598 0.135(7) Uiso 1 1 calc R . . H40B H 0.4369 -0.0331 0.0628 0.135(7) Uiso 1 1 calc R . . H40C H 0.3843 0.0318 0.0902 0.135(7) Uiso 1 1 calc R . . N5 N 0.6457(5) 0.1768(3) 0.0126(4) 0.057(3) Uani 1 1 d . . . C5 C 0.5887(6) 0.2016(3) -0.0414(5) 0.048(3) Uani 1 1 d . . . C50 C 0.5183(6) 0.2349(3) -0.1121(5) 0.069(4) Uani 1 1 d . . . H50A H 0.5272 0.2821 -0.1044 0.135(7) Uiso 1 1 calc R . . H50B H 0.4426 0.2231 -0.1150 0.135(7) Uiso 1 1 calc R . . H50C H 0.5376 0.2221 -0.1646 0.135(7) Uiso 1 1 calc R . . N6 N 0.8326(8) 0.0746(3) 0.0310(4) 0.052(4) Uani 1 1 d . . . C6 C 0.8594(10) 0.0543(4) -0.0225(6) 0.054(5) Uani 1 1 d . . . C60 C 0.8959(9) 0.0261(4) -0.0938(5) 0.082(5) Uani 1 1 d . . . H60A H 0.8410 0.0340 -0.1461 0.135(7) Uiso 1 1 calc R . . H60B H 0.9067 -0.0209 -0.0852 0.135(7) Uiso 1 1 calc R . . H60C H 0.9645 0.0465 -0.0977 0.135(7) Uiso 1 1 calc R . . N7 N 0.6145(6) 0.1979(3) 0.1827(6) 0.056(4) Uani 1 1 d . . . C7 C 0.5393(8) 0.2220(4) 0.1983(9) 0.064(5) Uani 1 1 d . . . C70 C 0.4446(9) 0.2556(5) 0.2186(9) 0.105(7) Uani 1 1 d . . . H70A H 0.4591 0.2635 0.2795 0.135(7) Uiso 1 1 calc R . . H70B H 0.3799 0.2282 0.2012 0.135(7) Uiso 1 1 calc R . . H70C H 0.4324 0.2972 0.1885 0.135(7) Uiso 1 1 calc R . . N8 N 0.8765(7) 0.2172(3) 0.0533(4) 0.058(3) Uani 1 1 d . . . C8 C 0.9156(9) 0.2524(4) 0.0187(6) 0.056(4) Uani 1 1 d . . . C80 C 0.9685(9) 0.2995(4) -0.0248(6) 0.087(5) Uani 1 1 d . . . H80A H 0.9134 0.3236 -0.0658 0.135(7) Uiso 1 1 calc R . . H80B H 1.0168 0.2767 -0.0541 0.135(7) Uiso 1 1 calc R . . H80C H 1.0109 0.3300 0.0163 0.135(7) Uiso 1 1 calc R . . N9 N 0.8682(5) 0.0344(2) 0.2201(4) 0.054(3) Uani 1 1 d . . . C9 C 0.9185(7) -0.0039(3) 0.2588(5) 0.055(4) Uani 1 1 d . . . C90 C 0.9853(8) -0.0546(4) 0.3099(6) 0.078(5) Uani 1 1 d . . . H90A H 0.9543 -0.0975 0.2924 0.135(7) Uiso 1 1 calc R . . H90B H 0.9867 -0.0476 0.3696 0.135(7) Uiso 1 1 calc R . . H90C H 1.0594 -0.0524 0.3018 0.135(7) Uiso 1 1 calc R . . N10 N 0.4629(9) 0.1027(5) 0.2915(7) 0.123(6) Uani 1 1 d . . . C100 C 0.5032(9) 0.0693(5) 0.3399(8) 0.096(6) Uani 1 1 d . . . C101 C 0.5420(14) 0.0291(5) 0.4059(9) 0.285(17) Uani 1 1 d . . . H10D H 0.5672 0.0550 0.4572 0.135(7) Uiso 1 1 calc R . . H10E H 0.6027 0.0037 0.3949 0.135(7) Uiso 1 1 calc R . . H10F H 0.4843 -0.0004 0.4133 0.135(7) Uiso 1 1 calc R . . As1 As 0.17871(8) 0.08956(4) 0.48521(6) 0.0658(4) Uani 1 1 d . . . F1 F 0.3069(5) 0.1012(2) 0.5432(3) 0.095(3) Uani 1 1 d . . . F2 F 0.1309(5) 0.1419(2) 0.5506(3) 0.091(3) Uani 1 1 d . . . F3 F 0.0516(5) 0.0815(3) 0.4265(4) 0.128(3) Uani 1 1 d . . . F4 F 0.1957(6) 0.1548(3) 0.4243(3) 0.110(3) Uani 1 1 d . . . F5 F 0.1670(6) 0.0269(2) 0.5493(4) 0.122(4) Uani 1 1 d . . . F6 F 0.2229(7) 0.0376(3) 0.4237(4) 0.150(5) Uani 1 1 d . . . As2 As 0.21979(8) 0.14948(4) 0.96233(5) 0.0738(5) Uani 1 1 d D . . As3 As 0.67910(7) 0.12903(4) 0.71146(6) 0.0765(5) Uani 1 1 d D . . F7 F 0.3406(5) 0.1381(6) 0.9512(6) 0.214(14) Uani 0.50 1 d PD . . F8 F 0.2626(10) 0.2070(3) 1.0280(6) 0.35(3) Uani 0.50 1 d PD . . F9 F 0.2412(9) 0.0979(4) 1.0384(4) 0.161(10) Uani 0.50 1 d PD . . F10 F 0.1985(8) 0.2009(4) 0.8863(4) 0.149(8) Uani 0.50 1 d PDU . . F11 F 0.1768(9) 0.0918(3) 0.8966(6) 0.148(10) Uani 0.50 1 d PD . . F12 F 0.0989(5) 0.1607(5) 0.9736(6) 0.25(2) Uani 0.50 1 d PD . . F13 F 0.1340(11) 0.1994(6) 0.9879(6) 0.41(4) Uani 0.50 1 d PD . . F14 F 0.3093(9) 0.1683(7) 1.0476(5) 0.200(12) Uani 0.50 1 d PD . . F15 F 0.1319(8) 0.1298(7) 0.8770(5) 0.213(13) Uani 0.50 1 d PD . . F16 F 0.3062(11) 0.0993(6) 0.9374(5) 0.260(19) Uani 0.50 1 d PD . . F17 F 0.2652(12) 0.2070(6) 0.9121(6) 0.27(2) Uani 0.50 1 d PD . . F18 F 0.1758(13) 0.0912(7) 1.0125(7) 0.64(3) Uani 0.50 1 d PD . . F19 F 0.6744(6) 0.0533(3) 0.7186(6) 0.171(11) Uani 0.50 1 d PD . . F20 F 0.6847(6) 0.2046(3) 0.7052(7) 0.226(18) Uani 0.50 1 d PD . . F21 F 0.6784(10) 0.1228(5) 0.6162(4) 0.259(12) Uani 0.50 1 d PDU . . F22 F 0.5528(5) 0.1322(4) 0.6891(7) 0.254(13) Uani 0.50 1 d PD . . F23 F 0.8060(5) 0.1258(4) 0.7346(7) 0.225(15) Uani 0.50 1 d PD . . F24 F 0.6804(9) 0.1348(5) 0.8073(4) 0.206(13) Uani 0.50 1 d PD . . F25 F 0.7738(7) 0.1554(3) 0.7969(4) 0.204(13) Uani 0.50 1 d PD . . F26 F 0.7219(7) 0.0512(3) 0.7330(5) 0.089(6) Uani 0.50 1 d PD . . F27 F 0.7702(7) 0.1384(5) 0.6506(6) 0.278(17) Uani 0.50 1 d PD . . F28 F 0.5852(7) 0.1027(3) 0.6258(5) 0.162(10) Uani 0.50 1 d PD . . F29 F 0.6365(8) 0.2069(3) 0.6898(6) 0.30(2) Uani 0.50 1 d PD . . F30 F 0.5884(8) 0.1197(6) 0.7722(7) 0.341(18) Uani 0.50 1 d PDU . . 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 La1 0.0365(2) 0.04077(19) 0.0368(2) 0.0020(2) 0.0058(2) 0.0023(2) N1 0.045(5) 0.060(4) 0.045(3) 0.006(3) 0.020(5) 0.012(4) C1 0.063(8) 0.044(4) 0.053(5) 0.004(4) 0.019(7) 0.014(5) C10 0.121(11) 0.089(6) 0.046(5) 0.017(5) 0.039(9) 0.030(7) N2 0.055(4) 0.050(3) 0.046(4) 0.000(3) 0.019(5) -0.007(4) C2 0.048(5) 0.053(4) 0.043(4) -0.001(4) 0.009(5) 0.000(4) C20 0.092(8) 0.047(4) 0.063(5) 0.003(4) 0.023(8) -0.006(5) N3 0.042(4) 0.071(4) 0.058(5) 0.004(4) 0.012(5) 0.000(4) C3 0.046(5) 0.071(5) 0.056(7) -0.007(5) 0.008(7) -0.010(5) C30 0.038(5) 0.156(9) 0.065(7) -0.022(7) 0.025(8) -0.008(6) N4 0.052(4) 0.043(3) 0.067(5) -0.001(3) 0.016(6) -0.003(3) C4 0.071(6) 0.047(4) 0.059(6) 0.005(4) 0.000(7) -0.005(5) C40 0.076(7) 0.098(6) 0.101(8) 0.027(7) -0.011(9) -0.047(6) N5 0.057(5) 0.070(4) 0.041(3) 0.013(3) 0.002(5) 0.016(4) C5 0.037(5) 0.055(4) 0.053(5) 0.002(4) 0.012(6) 0.001(4) C50 0.054(6) 0.076(5) 0.065(6) 0.022(4) -0.010(6) 0.003(4) N6 0.066(6) 0.053(4) 0.042(4) -0.007(3) 0.023(7) 0.013(5) C6 0.061(8) 0.046(5) 0.054(5) 0.001(4) 0.014(9) 0.018(5) C60 0.089(9) 0.096(7) 0.064(6) 0.002(6) 0.021(9) 0.018(7) N7 0.043(5) 0.076(5) 0.060(5) -0.006(5) 0.032(7) -0.005(4) C7 0.059(6) 0.049(5) 0.088(9) -0.014(6) 0.028(11) 0.008(5) C70 0.082(8) 0.094(8) 0.162(13) 0.015(9) 0.074(14) 0.018(7) N8 0.078(6) 0.052(4) 0.048(4) 0.010(3) 0.023(6) -0.007(4) C8 0.070(8) 0.057(5) 0.051(5) 0.013(4) 0.035(8) 0.014(6) C80 0.107(10) 0.085(6) 0.089(7) 0.025(6) 0.064(11) 0.015(7) N9 0.057(5) 0.048(3) 0.054(4) 0.006(3) 0.008(5) 0.010(3) C9 0.064(6) 0.044(4) 0.053(5) 0.003(4) 0.008(6) 0.002(4) C90 0.081(8) 0.076(5) 0.079(6) 0.019(5) 0.023(9) 0.021(6) N10 0.100(8) 0.115(8) 0.168(12) 0.006(8) 0.061(12) -0.008(7) C100 0.085(9) 0.081(7) 0.116(10) -0.028(7) 0.013(10) 0.030(6) C101 0.37(3) 0.073(7) 0.29(2) -0.011(11) -0.17(2) 0.032(12) As1 0.0727(7) 0.0647(5) 0.0565(5) -0.0025(5) 0.0082(7) 0.0060(5) F1 0.080(4) 0.109(4) 0.091(4) 0.016(3) 0.010(5) -0.004(4) F2 0.122(6) 0.081(3) 0.078(3) -0.013(3) 0.039(6) 0.016(4) F3 0.087(4) 0.164(5) 0.117(5) -0.054(5) -0.007(6) 0.011(4) F4 0.140(6) 0.122(4) 0.073(3) 0.031(3) 0.031(6) 0.032(5) F5 0.142(7) 0.067(3) 0.162(6) 0.027(4) 0.047(8) -0.006(4) F6 0.179(9) 0.129(5) 0.133(6) -0.061(5) 0.017(9) 0.030(6) As2 0.1007(9) 0.0552(5) 0.0746(6) -0.0073(5) 0.0389(9) -0.0131(6) As3 0.0651(7) 0.0750(6) 0.0994(8) 0.0047(6) 0.0397(10) 0.0025(5) F7 0.048(8) 0.38(3) 0.22(3) 0.00(2) 0.031(17) -0.033(15) F8 0.76(9) 0.118(14) 0.157(19) -0.057(12) 0.06(3) -0.18(3) F9 0.24(2) 0.129(11) 0.150(13) 0.088(11) 0.12(2) 0.102(14) F10 0.161(14) 0.180(14) 0.125(10) 0.091(10) 0.070(13) 0.009(12) F11 0.171(18) 0.129(12) 0.171(18) -0.082(12) 0.095(19) -0.059(14) F12 0.132(14) 0.133(15) 0.55(6) 0.05(2) 0.22(4) 0.065(13) F13 0.71(8) 0.27(3) 0.26(3) -0.05(3) 0.13(6) 0.36(4) F14 0.20(2) 0.32(3) 0.073(9) -0.058(16) 0.019(16) -0.04(2) F15 0.087(11) 0.29(3) 0.22(2) -0.124(19) -0.047(16) 0.012(15) F16 0.45(4) 0.216(19) 0.084(11) 0.001(11) 0.01(2) 0.24(2) F17 0.34(4) 0.21(2) 0.23(2) 0.048(18) -0.01(3) -0.19(2) F18 1.10(7) 0.39(3) 0.34(4) 0.10(4) -0.02(7) -0.580 F19 0.125(13) 0.196(17) 0.200(19) 0.031(15) 0.055(18) -0.118(12) F20 0.115(11) 0.052(8) 0.51(5) 0.083(16) 0.06(2) 0.016(8) F21 0.33(2) 0.291(18) 0.179(14) 0.129(14) 0.118(17) 0.060(17) F22 0.070(9) 0.47(3) 0.178(19) 0.02(2) -0.061(13) -0.009(15) F23 0.181(18) 0.126(12) 0.35(3) 0.067(18) 0.02(3) 0.057(13) F24 0.24(2) 0.173(14) 0.147(15) -0.094(12) -0.064(18) 0.099(15) F25 0.26(3) 0.241(18) 0.075(9) -0.067(10) -0.030(14) -0.116(18) F26 0.119(11) 0.065(6) 0.070(7) 0.014(6) -0.007(9) 0.018(7) F27 0.26(3) 0.44(3) 0.151(16) -0.13(2) 0.08(2) -0.25(3) F28 0.157(14) 0.120(9) 0.146(13) 0.035(9) -0.094(13) -0.073(9) F29 0.41(3) 0.118(14) 0.30(3) 0.019(16) -0.10(3) 0.156(18) F30 0.35(3) 0.34(2) 0.36(2) -0.044(18) 0.130(19) 0.000(18) _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 La1 N7 2.575(9) . y La1 N3 2.616(6) . y La1 N5 2.616(4) . y La1 N8 2.629(9) . y La1 N6 2.635(8) . y La1 N2 2.636(5) . y La1 N1 2.648(7) . y La1 N9 2.650(5) . y La1 N4 2.653(7) . y N1 C1 1.095(11) . y C1 C10 1.488(12) . ? N2 C2 1.119(7) . y C2 C20 1.465(9) . ? N3 C3 1.122(11) . y C3 C30 1.514(13) . ? N4 C4 1.117(11) . y C4 C40 1.462(12) . ? N5 C5 1.121(6) . y C5 C50 1.453(7) . ? N6 C6 1.091(14) . y C6 C60 1.468(15) . ? N7 C7 1.154(15) . y C7 C70 1.488(17) . ? N8 C8 1.102(12) . y C8 C80 1.455(14) . ? N9 C9 1.110(7) . y C9 C90 1.472(8) . ? N10 C100 1.079(11) . ? C100 C101 1.353(13) . ? As1 F6 1.649(8) . ? As1 F3 1.677(5) . ? As1 F5 1.685(6) . ? As1 F1 1.694(5) . ? As1 F4 1.711(6) . ? As1 F2 1.723(6) . ? As2 F7 1.602(6) . ? As2 F10 1.602(6) . ? As2 F12 1.602(6) . ? As2 F8 1.602(6) . ? As2 F11 1.604(6) . ? As2 F9 1.605(6) . ? As2 F15 1.616(7) . ? As2 F17 1.619(7) . ? As2 F13 1.620(7) . ? As2 F18 1.622(7) . ? As2 F14 1.622(7) . ? As2 F16 1.624(7) . ? As3 F22 1.557(6) . ? As3 F21 1.557(6) . ? As3 F20 1.559(6) . ? As3 F19 1.562(6) . ? As3 F24 1.564(6) . ? As3 F23 1.565(6) . ? As3 F30 1.696(5) . ? As3 F28 1.697(5) . ? As3 F29 1.697(5) . ? As3 F26 1.698(5) . ? As3 F25 1.700(5) . ? As3 F27 1.701(5) . ? F7 F16 0.910(15) . ? F7 F17 1.743(15) . ? F8 F14 0.998(15) . ? F8 F13 1.615(13) . ? F9 F18 0.849(14) . ? F9 F14 1.673(11) . ? F10 F17 0.860(12) . ? F10 F15 1.675(10) . ? F11 F15 0.974(13) . ? F11 F16 1.626(12) . ? F12 F13 0.914(15) . ? F12 F18 1.761(17) . ? F19 F26 0.594(11) . ? F20 F29 0.605(11) . ? F21 F27 1.209(11) . ? F21 F28 1.295(11) . ? F22 F28 1.342(10) . ? F22 F30 1.349(11) . ? F23 F25 1.328(11) . ? F23 F27 1.363(11) . ? F24 F30 1.212(10) . ? F24 F25 1.305(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 N7 La1 N3 138.8(2) . . y N7 La1 N5 68.6(3) . . y N3 La1 N5 137.1(3) . . y N7 La1 N8 113.5(3) . . y N3 La1 N8 69.2(2) . . y N5 La1 N8 68.8(2) . . y N7 La1 N6 136.3(3) . . y N3 La1 N6 84.4(3) . . y N5 La1 N6 73.1(2) . . y N8 La1 N6 69.2(2) . . y N7 La1 N2 67.7(2) . . y N3 La1 N2 77.1(2) . . y N5 La1 N2 94.71(16) . . y N8 La1 N2 67.7(2) . . y N6 La1 N2 136.7(3) . . y N7 La1 N1 70.9(3) . . y N3 La1 N1 79.5(3) . . y N5 La1 N1 139.2(2) . . y N8 La1 N1 134.52(19) . . y N6 La1 N1 140.48(18) . . y N2 La1 N1 73.88(19) . . y N7 La1 N9 122.9(3) . . y N3 La1 N9 67.41(19) . . y N5 La1 N9 133.84(16) . . y N8 La1 N9 123.6(2) . . y N6 La1 N9 72.4(2) . . y N2 La1 N9 131.45(15) . . y N1 La1 N9 68.1(2) . . y N7 La1 N4 69.5(2) . . y N3 La1 N4 138.95(18) . . y N5 La1 N4 72.92(19) . . y N8 La1 N4 136.13(19) . . y N6 La1 N4 80.0(3) . . y N2 La1 N4 137.0(2) . . y N1 La1 N4 88.9(2) . . y N9 La1 N4 71.71(17) . . y C1 N1 La1 175.8(8) . . y N1 C1 C10 178.9(9) . . y C2 N2 La1 170.7(5) . . y N2 C2 C20 177.9(9) . . y C3 N3 La1 167.2(8) . . y N3 C3 C30 178.3(12) . . y C4 N4 La1 167.0(5) . . y N4 C4 C40 177.5(12) . . y C5 N5 La1 166.9(5) . . y N5 C5 C50 177.9(9) . . y C6 N6 La1 168.1(9) . . y N6 C6 C60 179.2(9) . . y C7 N7 La1 178.1(9) . . y N7 C7 C70 177.7(10) . . y C8 N8 La1 172.0(7) . . y N8 C8 C80 178.5(9) . . y C9 N9 La1 165.0(5) . . y N9 C9 C90 179.9(12) . . y N10 C100 C101 171.8(18) . . ? F6 As1 F3 90.4(3) . . ? F6 As1 F5 88.6(4) . . ? F3 As1 F5 93.7(3) . . ? F6 As1 F1 90.8(3) . . ? F3 As1 F1 177.5(3) . . ? F5 As1 F1 88.5(3) . . ? F6 As1 F4 92.6(4) . . ? F3 As1 F4 88.9(3) . . ? F5 As1 F4 177.1(3) . . ? F1 As1 F4 88.8(3) . . ? F6 As1 F2 178.3(4) . . ? F3 As1 F2 89.1(3) . . ? F5 As1 F2 89.8(3) . . ? F1 As1 F2 89.8(3) . . ? F4 As1 F2 89.0(3) . . ? F7 As2 F10 90.0(2) . . ? F7 As2 F12 179.8(3) . . ? F10 As2 F12 90.14(19) . . ? F7 As2 F8 90.1(2) . . ? F10 As2 F8 90.05(19) . . ? F12 As2 F8 90.0(2) . . ? F7 As2 F11 90.0(2) . . ? F10 As2 F11 90.0(2) . . ? F12 As2 F11 89.9(2) . . ? F8 As2 F11 179.9(3) . . ? F7 As2 F9 89.93(19) . . ? F10 As2 F9 179.9(3) . . ? F12 As2 F9 89.9(2) . . ? F8 As2 F9 90.0(2) . . ? F11 As2 F9 89.91(19) . . ? F7 As2 F15 110.4(5) . . ? F10 As2 F15 62.7(4) . . ? F12 As2 F15 69.6(6) . . ? F8 As2 F15 144.8(5) . . ? F11 As2 F15 35.2(5) . . ? F9 As2 F15 117.2(4) . . ? F7 As2 F17 65.5(6) . . ? F10 As2 F17 31.0(5) . . ? F12 As2 F17 114.6(6) . . ? F8 As2 F17 72.3(5) . . ? F11 As2 F17 107.8(5) . . ? F9 As2 F17 149.0(5) . . ? F15 As2 F17 90.1(2) . . ? F7 As2 F13 147.2(6) . . ? F10 As2 F13 77.4(6) . . ? F12 As2 F13 33.0(6) . . ? F8 As2 F13 60.2(5) . . ? F11 As2 F13 119.8(5) . . ? F9 As2 F13 102.7(6) . . ? F15 As2 F13 90.7(4) . . ? F17 As2 F13 90.5(4) . . ? F7 As2 F18 113.6(7) . . ? F10 As2 F18 149.5(5) . . ? F12 As2 F18 66.2(7) . . ? F8 As2 F18 108.0(5) . . ? F11 As2 F18 71.9(5) . . ? F9 As2 F18 30.5(5) . . ? F15 As2 F18 90.0(2) . . ? F17 As2 F18 179.1(8) . . ? F13 As2 F18 90.3(4) . . ? F7 As2 F14 68.7(6) . . ? F10 As2 F14 117.6(4) . . ? F12 As2 F14 111.3(6) . . ? F8 As2 F14 36.1(5) . . ? F11 As2 F14 143.9(5) . . ? F9 As2 F14 62.4(4) . . ? F15 As2 F14 179.0(8) . . ? F17 As2 F14 90.0(2) . . ? F13 As2 F14 90.3(4) . . ? F18 As2 F14 89.9(2) . . ? F7 As2 F16 32.8(6) . . ? F10 As2 F16 103.0(5) . . ? F12 As2 F16 147.1(6) . . ? F8 As2 F16 119.6(5) . . ? F11 As2 F16 60.5(5) . . ? F9 As2 F16 76.9(5) . . ? F15 As2 F16 89.7(4) . . ? F17 As2 F16 89.7(4) . . ? F13 As2 F16 179.6(3) . . ? F18 As2 F16 89.4(4) . . ? F14 As2 F16 89.4(4) . . ? F22 As3 F21 90.3(2) . . ? F22 As3 F20 90.2(2) . . ? F21 As3 F20 90.3(2) . . ? F22 As3 F19 90.2(2) . . ? F21 As3 F19 90.1(2) . . ? F20 As3 F19 179.4(3) . . ? F22 As3 F24 90.0(2) . . ? F21 As3 F24 179.5(3) . . ? F20 As3 F24 90.0(2) . . ? F19 As3 F24 89.6(2) . . ? F22 As3 F23 179.6(3) . . ? F21 As3 F23 90.1(2) . . ? F20 As3 F23 89.8(2) . . ? F19 As3 F23 89.7(2) . . ? F24 As3 F23 89.6(2) . . ? F22 As3 F30 48.8(4) . . ? F21 As3 F30 136.8(4) . . ? F20 As3 F30 101.4(6) . . ? F19 As3 F30 78.6(6) . . ? F24 As3 F30 43.4(4) . . ? F23 As3 F30 130.8(4) . . ? F22 As3 F28 48.5(4) . . ? F21 As3 F28 46.7(4) . . ? F20 As3 F28 107.3(4) . . ? F19 As3 F28 73.3(4) . . ? F24 As3 F28 133.5(4) . . ? F23 As3 F28 131.9(4) . . ? F30 As3 F28 90.31(19) . . ? F22 As3 F29 69.7(4) . . ? F21 As3 F29 86.7(6) . . ? F20 As3 F29 20.9(4) . . ? F19 As3 F29 159.6(4) . . ? F24 As3 F29 93.7(6) . . ? F23 As3 F29 110.4(4) . . ? F30 As3 F29 90.08(19) . . ? F28 As3 F29 90.09(18) . . ? F22 As3 F26 110.4(4) . . ? F21 As3 F26 93.2(5) . . ? F20 As3 F26 159.0(4) . . ? F19 As3 F26 20.5(4) . . ? F24 As3 F26 86.3(5) . . ? F23 As3 F26 69.5(4) . . ? F30 As3 F26 90.03(19) . . ? F28 As3 F26 89.96(17) . . ? F29 As3 F26 179.9(3) . . ? F22 As3 F25 131.9(4) . . ? F21 As3 F25 133.0(4) . . ? F20 As3 F25 72.7(4) . . ? F19 As3 F25 106.7(4) . . ? F24 As3 F25 46.9(4) . . ? F23 As3 F25 47.8(4) . . ? F30 As3 F25 90.09(19) . . ? F28 As3 F25 179.6(2) . . ? F29 As3 F25 89.97(18) . . ? F26 As3 F25 89.99(18) . . ? F22 As3 F27 131.3(4) . . ? F21 As3 F27 43.3(4) . . ? F20 As3 F27 78.5(6) . . ? F19 As3 F27 101.5(6) . . ? F24 As3 F27 136.5(4) . . ? F23 As3 F27 49.1(4) . . ? F30 As3 F27 179.9(3) . . ? F28 As3 F27 89.76(18) . . ? F29 As3 F27 89.90(19) . . ? F26 As3 F27 89.99(19) . . ? F25 As3 F27 89.84(19) . . ? F16 F7 As2 75.0(8) . . ? F16 F7 F17 115.5(9) . . ? As2 F7 F17 57.7(4) . . ? F14 F8 As2 73.1(6) . . ? F14 F8 F13 121.3(10) . . ? As2 F8 F13 60.5(4) . . ? F18 F9 As2 75.8(8) . . ? F18 F9 F14 127.5(15) . . ? As2 F9 F14 59.3(4) . . ? F17 F10 As2 75.6(8) . . ? F17 F10 F15 126.0(12) . . ? As2 F10 F15 59.1(4) . . ? F15 F11 As2 73.1(7) . . ? F15 F11 F16 120.9(9) . . ? As2 F11 F16 60.4(4) . . ? F13 F12 As2 74.6(8) . . ? F13 F12 F18 114.8(10) . . ? As2 F12 F18 57.4(4) . . ? F12 F13 F8 124.9(10) . . ? F12 F13 As2 72.5(7) . . ? F8 F13 As2 59.4(5) . . ? F8 F14 As2 70.9(7) . . ? F8 F14 F9 113.9(11) . . ? As2 F14 F9 58.3(4) . . ? F11 F15 As2 71.7(6) . . ? F11 F15 F10 115.1(9) . . ? As2 F15 F10 58.2(4) . . ? F7 F16 As2 72.3(7) . . ? F7 F16 F11 124.2(10) . . ? As2 F16 F11 59.1(4) . . ? F10 F17 As2 73.4(7) . . ? F10 F17 F7 116.8(12) . . ? As2 F17 F7 56.8(5) . . ? F9 F18 As2 73.7(7) . . ? F9 F18 F12 116.1(14) . . ? As2 F18 F12 56.3(5) . . ? F26 F19 As3 92.8(9) . . ? F29 F20 As3 92.6(10) . . ? F27 F21 F28 146.4(8) . . ? F27 F21 As3 74.7(5) . . ? F28 F21 As3 72.4(4) . . ? F28 F22 F30 126.7(8) . . ? F28 F22 As3 71.2(4) . . ? F30 F22 As3 71.0(4) . . ? F25 F23 F27 126.4(8) . . ? F25 F23 As3 71.5(4) . . ? F27 F23 As3 70.7(4) . . ? F30 F24 F25 145.4(8) . . ? F30 F24 As3 74.1(5) . . ? F25 F24 As3 72.0(4) . . ? F24 F25 F23 113.7(6) . . ? F24 F25 As3 61.1(4) . . ? F23 F25 As3 60.8(4) . . ? F19 F26 As3 66.8(8) . . ? F21 F27 F23 118.3(8) . . ? F21 F27 As3 62.0(4) . . ? F23 F27 As3 60.2(4) . . ? F21 F28 F22 113.7(7) . . ? F21 F28 As3 61.0(4) . . ? F22 F28 As3 60.3(3) . . ? F20 F29 As3 66.6(8) . . ? F24 F30 F22 118.9(8) . . ? F24 F30 As3 62.5(4) . . ? F22 F30 As3 60.2(4) . . ? _diffrn_measured_fraction_theta_max 0.540 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.540 _refine_diff_density_max 0.440 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.068 #=END data_pet29 _audit_creation_method SHELXL-93 _chemical_name_systematic ; (SAPRS-9)-Nonakis(acetonitril)samarium(III)-hexafluoroarsenat(V)- acetonitril(1/3) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H36 As3 F18 N12 Sm' _chemical_formula_weight 1209.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' .0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.098(2) _cell_length_b 16.5100(10) _cell_length_c 23.949(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.950(10) _cell_angle_gamma 90.00 _cell_volume 4642.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 14.022 _cell_measurement_theta_max 15.036 _exptl_crystal_description plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2348 _exptl_absorpt_coefficient_mu 3.491 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.1666 _exptl_absorpt_correction_T_max 0.7216 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 13029 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.1286 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10544 _reflns_number_observed 4141 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. The AsF6-anion containing As(3) is disordered. It was refined as two octahedrons with one common F-As-F axis. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+( 0.0193P)^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 refU _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00017(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_ls_number_reflns 10544 _refine_ls_number_parameters 573 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_obs 0.0419 _refine_ls_wR_factor_all 0.0949 _refine_ls_wR_factor_obs 0.0786 _refine_ls_goodness_of_fit_all 0.745 _refine_ls_goodness_of_fit_obs 1.028 _refine_ls_restrained_S_all 0.745 _refine_ls_restrained_S_obs 1.028 _refine_ls_shift/esd_max 0.077 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sm1 Sm 0.31014(3) 0.18071(2) 0.18833(2) 0.03369(9) Uani 1 d . . N1 N 0.4125(4) 0.2773(3) 0.1349(2) 0.0491(14) Uani 1 d . . C1 C 0.4463(6) 0.3056(4) 0.0999(3) 0.049(2) Uani 1 d . . C10 C 0.4849(7) 0.3445(4) 0.0527(3) 0.076(3) Uani 1 d . . H10A H 0.5667(12) 0.3350(29) 0.0578(14) 0.147(7) Uiso 1 calc R . H10B H 0.4703(44) 0.4028(7) 0.0530(15) 0.147(7) Uiso 1 calc R . H10C H 0.4434(36) 0.3214(25) 0.0159(3) 0.147(7) Uiso 1 calc R . N2 N 0.2343(5) 0.1549(3) 0.0818(2) 0.0505(14) Uani 1 d . . C2 C 0.2388(5) 0.1312(3) 0.0383(3) 0.046(2) Uani 1 d . . C20 C 0.2406(7) 0.0995(4) -0.0174(3) 0.076(3) Uani 1 d . . H20A H 0.2100(49) 0.1402(15) -0.0470(4) 0.147(7) Uiso 1 calc R . H20B H 0.1938(43) 0.0504(22) -0.0249(11) 0.147(7) Uiso 1 calc R . H20C H 0.3191(9) 0.0864(34) -0.0184(9) 0.147(7) Uiso 1 calc R . N3 N 0.4651(4) 0.1050(3) 0.1543(2) 0.0451(13) Uani 1 d . . C3 C 0.5388(5) 0.0887(4) 0.1355(3) 0.043(2) Uani 1 d . . C30 C 0.6373(6) 0.0731(4) 0.1122(3) 0.070(2) Uani 1 d . . H30A H 0.6128(9) 0.0683(35) 0.0703(4) 0.147(7) Uiso 1 calc R . H30B H 0.6740(29) 0.0226(19) 0.1284(19) 0.147(7) Uiso 1 calc R . H30C H 0.6915(23) 0.1180(17) 0.1223(21) 0.147(7) Uiso 1 calc R . N4 N 0.2809(5) 0.2804(3) 0.2632(2) 0.0478(14) Uani 1 d . . C4 C 0.2339(6) 0.3163(4) 0.2902(3) 0.046(2) Uani 1 d . . C40 C 0.1647(6) 0.3632(4) 0.3214(3) 0.072(3) Uani 1 d . . H40A H 0.2053(22) 0.4130(17) 0.3365(21) 0.147(7) Uiso 1 calc R . H40B H 0.1510(42) 0.3308(14) 0.3534(15) 0.147(7) Uiso 1 calc R . H40C H 0.0917(21) 0.3772(30) 0.2952(7) 0.147(7) Uiso 1 calc R . N5 N 0.1166(4) 0.1560(3) 0.2059(2) 0.0468(13) Uani 1 d . . C5 C 0.0415(6) 0.1357(4) 0.2248(3) 0.046(2) Uani 1 d . . C50 C -0.0490(7) 0.1061(4) 0.2480(3) 0.077(2) Uani 1 d . . H50A H -0.1194(13) 0.1351(24) 0.2304(18) 0.147(7) Uiso 1 calc R . H50B H -0.0301(23) 0.1147(31) 0.2897(5) 0.147(7) Uiso 1 calc R . H50C H -0.0597(32) 0.0480(8) 0.2398(21) 0.147(7) Uiso 1 calc R . N6 N 0.3388(5) 0.1065(3) 0.2835(2) 0.0525(15) Uani 1 d . . C6 C 0.3450(6) 0.0905(3) 0.3295(3) 0.043(2) Uani 1 d . . C60 C 0.3515(6) 0.0709(5) 0.3894(3) 0.073(2) Uani 1 d . . H60A H 0.3911(45) 0.0191(19) 0.3991(8) 0.147(7) Uiso 1 calc R . H60B H 0.2743(7) 0.0668(35) 0.3954(6) 0.147(7) Uiso 1 calc R . H60C H 0.3933(44) 0.1136(19) 0.4142(3) 0.147(7) Uiso 1 calc R . N7 N 0.1854(4) 0.2998(3) 0.1449(2) 0.0452(13) Uani 1 d . . C7 C 0.1417(5) 0.3601(4) 0.1309(2) 0.0416(15) Uani 1 d . . C70 C 0.0864(6) 0.4370(4) 0.1117(3) 0.069(2) Uani 1 d . . H70A H 0.0782(47) 0.4430(17) 0.0702(6) 0.147(7) Uiso 1 calc R . H70B H 0.1328(26) 0.4816(4) 0.1320(19) 0.147(7) Uiso 1 calc R . H70C H 0.0110(21) 0.4383(15) 0.1200(23) 0.147(7) Uiso 1 calc R . N8 N 0.2496(5) 0.0341(3) 0.1669(2) 0.0469(13) Uani 1 d . . C8 C 0.2020(6) -0.0232(4) 0.1505(3) 0.049(2) Uani 1 d . . C80 C 0.1407(6) -0.0959(4) 0.1264(3) 0.068(2) Uani 1 d . . H80A H 0.0709(26) -0.0806(4) 0.0981(19) 0.147(7) Uiso 1 calc R . H80B H 0.1210(44) -0.1275(18) 0.1573(5) 0.147(7) Uiso 1 calc R . H80C H 0.1889(20) -0.1285(18) 0.1076(22) 0.147(7) Uiso 1 calc R . N9 N 0.5052(5) 0.2081(3) 0.2528(2) 0.053(2) Uani 1 d . . C9 C 0.5924(6) 0.2029(4) 0.2833(3) 0.047(2) Uani 1 d . . C90 C 0.7063(5) 0.1953(4) 0.3234(3) 0.062(2) Uani 1 d . . H90A H 0.7330(22) 0.1393(9) 0.3232(19) 0.147(7) Uiso 1 calc R . H90B H 0.7012(11) 0.2099(34) 0.3623(5) 0.147(7) Uiso 1 calc R . H90C H 0.7600(13) 0.2316(26) 0.3111(14) 0.147(7) Uiso 1 calc R . As1 As 0.55288(8) 0.15836(5) -0.06531(4) 0.0574(2) Uani 1 d . . F1 F 0.5949(5) 0.1495(3) -0.1272(2) 0.116(2) Uani 1 d . . F2 F 0.5063(7) 0.2493(4) -0.0853(3) 0.189(4) Uani 1 d . . F3 F 0.5048(6) 0.1680(3) -0.0045(2) 0.134(2) Uani 1 d . . F4 F 0.4288(6) 0.1192(5) -0.1015(3) 0.175(3) Uani 1 d . . F5 F 0.6726(6) 0.1982(5) -0.0324(3) 0.227(4) Uani 1 d . . F6 F 0.5991(7) 0.0674(3) -0.0454(2) 0.188(4) Uani 1 d . . As2 As 0.07328(7) 0.32861(5) -0.06627(3) 0.0492(2) Uani 1 d . . F7 F 0.0355(4) 0.3297(3) -0.0037(2) 0.112(2) Uani 1 d . . F8 F 0.1135(5) 0.3232(3) -0.1289(2) 0.119(2) Uani 1 d . . F9 F 0.1093(5) 0.4259(3) -0.0582(2) 0.117(2) Uani 1 d . . F10 F -0.0614(4) 0.3553(3) -0.1008(2) 0.116(2) Uani 1 d . . F11 F 0.2078(4) 0.3041(3) -0.0314(2) 0.106(2) Uani 1 d . . F12 F 0.0360(5) 0.2306(3) -0.0723(3) 0.137(2) Uani 1 d . . As3 As 0.81124(9) 0.34518(4) 0.19023(5) 0.0582(2) Uani 1 d . . F13 F 0.8717(5) 0.4340(3) 0.2131(3) 0.145(2) Uani 1 d . . F14 F 0.7506(6) 0.2552(3) 0.1707(3) 0.145(2) Uani 1 d . . F15 F 0.9030(13) 0.2982(10) 0.2428(7) 0.109(5) Uani 0.50 d P . F16 F 0.7151(16) 0.3854(10) 0.1357(6) 0.140(5) Uani 0.50 d P . F17 F 0.7229(12) 0.3598(9) 0.2367(7) 0.099(4) Uani 0.50 d P . F18 F 0.8896(14) 0.3260(12) 0.1450(7) 0.151(6) Uani 0.50 d P . F19 F 0.8033(16) 0.3800(13) 0.1228(6) 0.167(7) Uani 0.50 d P . F20 F 0.8319(23) 0.3154(13) 0.2578(6) 0.186(9) Uani 0.50 d P . F21 F 0.9425(10) 0.3104(9) 0.1889(9) 0.133(5) Uani 0.50 d P . F22 F 0.6839(13) 0.3862(10) 0.1880(11) 0.153(7) Uani 0.50 d P . N100 N 0.0885(7) -0.0421(5) -0.0990(4) 0.118(3) Uani 1 d . . C101 C 0.0806(8) -0.1042(5) -0.0792(4) 0.088(3) Uani 1 d . . C102 C 0.0748(7) -0.1868(5) -0.0582(3) 0.098(3) Uani 1 d . . H10D H 0.0610(48) -0.1852(5) -0.0195(11) 0.147(7) Uiso 1 calc R . H10E H 0.1469(19) -0.2147(12) -0.0568(23) 0.147(7) Uiso 1 calc R . H10F H 0.0125(32) -0.2160(12) -0.0841(14) 0.147(7) Uiso 1 calc R . N110 N 0.6381(8) 0.4807(6) -0.0858(5) 0.167(5) Uani 1 d . . C111 C 0.6947(9) 0.4476(6) -0.0473(6) 0.111(4) Uani 1 d . . C112 C 0.7742(8) 0.3992(5) -0.0055(4) 0.104(3) Uani 1 d . . H11A H 0.7754(39) 0.4182(24) 0.0333(4) 0.147(7) Uiso 1 calc R . H11B H 0.8506(12) 0.4042(28) -0.0124(16) 0.147(7) Uiso 1 calc R . H11C H 0.7505(29) 0.3423(8) -0.0094(18) 0.147(7) Uiso 1 calc R . N120 N 0.7155(5) 0.0022(4) 0.2568(3) 0.070(2) Uani 1 d . . C121 C 0.6291(7) -0.0259(4) 0.2580(3) 0.056(2) Uani 1 d . . C122 C 0.5204(6) -0.0628(4) 0.2586(3) 0.063(2) Uani 1 d . . H12A H 0.4640(14) -0.0203(4) 0.2589(25) 0.147(7) Uiso 1 calc R . H12B H 0.5290(13) -0.0965(28) 0.2930(13) 0.147(7) Uiso 1 calc R . H12C H 0.4948(25) -0.0965(28) 0.2242(13) 0.147(7) Uiso 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 Sm1 0.0349(2) 0.03243(15) 0.0336(2) -0.0013(2) 0.00790(13) 0.0014(2) N1 0.045(3) 0.046(3) 0.057(4) 0.009(3) 0.014(3) 0.002(3) C1 0.061(5) 0.035(4) 0.052(4) -0.003(3) 0.015(4) 0.006(4) C10 0.109(7) 0.075(6) 0.054(5) 0.002(4) 0.039(5) -0.020(5) N2 0.065(4) 0.046(3) 0.039(3) 0.002(2) 0.008(3) -0.002(3) C2 0.047(4) 0.039(4) 0.051(4) -0.003(3) 0.011(4) -0.006(3) C20 0.099(7) 0.084(6) 0.051(5) -0.026(4) 0.030(5) -0.020(5) N3 0.043(3) 0.040(3) 0.053(3) -0.009(2) 0.013(3) 0.003(3) C3 0.032(4) 0.047(4) 0.048(4) 0.001(3) 0.006(3) 0.004(3) C30 0.066(6) 0.070(5) 0.081(6) -0.003(4) 0.035(5) 0.018(5) N4 0.060(4) 0.042(3) 0.042(3) -0.006(2) 0.012(3) 0.002(3) C4 0.064(5) 0.031(3) 0.042(3) -0.001(3) 0.012(3) -0.012(4) C40 0.108(7) 0.065(5) 0.060(5) -0.010(4) 0.051(5) 0.004(5) N5 0.035(3) 0.048(3) 0.059(3) -0.007(2) 0.015(3) 0.000(2) C5 0.037(4) 0.043(4) 0.055(4) -0.006(3) 0.003(3) -0.002(3) C50 0.086(6) 0.071(5) 0.091(6) -0.001(4) 0.056(5) -0.014(5) N6 0.056(4) 0.048(3) 0.050(3) 0.010(3) 0.004(3) -0.008(3) C6 0.048(4) 0.039(3) 0.041(4) 0.004(3) 0.008(3) 0.002(3) C60 0.088(6) 0.097(6) 0.041(4) 0.020(4) 0.029(4) 0.010(5) N7 0.051(3) 0.047(3) 0.038(3) 0.002(2) 0.012(3) 0.016(3) C7 0.035(4) 0.056(4) 0.034(3) -0.006(3) 0.009(3) -0.002(3) C70 0.077(6) 0.046(4) 0.074(5) 0.012(4) 0.000(5) 0.020(4) N8 0.053(4) 0.039(3) 0.054(3) -0.003(3) 0.024(3) -0.010(3) C8 0.052(4) 0.040(3) 0.056(4) -0.001(3) 0.015(4) 0.006(3) C80 0.064(6) 0.039(4) 0.092(6) -0.002(4) 0.006(5) -0.013(4) N9 0.042(3) 0.069(4) 0.043(3) -0.007(3) 0.001(3) -0.013(3) C9 0.054(4) 0.040(4) 0.050(4) -0.006(3) 0.018(4) -0.008(3) C90 0.037(4) 0.072(5) 0.076(6) -0.009(4) 0.012(4) 0.006(4) As1 0.0593(6) 0.0549(5) 0.0566(5) -0.0003(4) 0.0111(5) -0.0022(4) F1 0.128(5) 0.135(5) 0.101(4) 0.009(3) 0.059(4) 0.006(4) F2 0.323(11) 0.112(5) 0.132(5) 0.024(4) 0.055(6) 0.103(6) F3 0.201(7) 0.129(5) 0.084(4) 0.012(3) 0.056(4) 0.031(5) F4 0.125(6) 0.269(8) 0.131(5) -0.036(6) 0.029(4) -0.094(6) F5 0.132(6) 0.297(10) 0.223(8) -0.093(7) -0.015(6) -0.112(7) F6 0.341(11) 0.109(5) 0.107(4) 0.028(4) 0.038(6) 0.089(6) As2 0.0477(5) 0.0511(5) 0.0482(5) -0.0019(4) 0.0107(4) -0.0009(4) F7 0.100(4) 0.160(5) 0.080(3) -0.003(3) 0.029(3) 0.000(4) F8 0.121(4) 0.172(5) 0.070(3) -0.010(4) 0.034(3) -0.015(4) F9 0.124(5) 0.051(3) 0.179(5) -0.006(3) 0.041(4) -0.002(3) F10 0.075(4) 0.167(5) 0.095(4) 0.008(4) 0.000(3) 0.009(4) F11 0.068(3) 0.125(4) 0.117(4) 0.036(3) 0.004(3) 0.028(3) F12 0.138(5) 0.075(4) 0.202(6) -0.031(4) 0.049(5) -0.038(4) As3 0.0617(5) 0.0560(4) 0.0608(4) 0.0007(5) 0.0224(4) 0.0048(6) F13 0.151(6) 0.081(4) 0.205(7) -0.022(4) 0.044(5) -0.031(4) F14 0.155(6) 0.095(4) 0.183(6) -0.058(4) 0.035(5) -0.032(4) F15 0.092(10) 0.112(9) 0.119(14) 0.007(9) 0.016(8) 0.040(8) F16 0.130(14) 0.187(14) 0.088(10) 0.045(10) -0.003(9) 0.053(12) F17 0.079(10) 0.112(10) 0.119(12) -0.004(8) 0.051(9) 0.023(7) F18 0.109(13) 0.229(19) 0.118(13) -0.010(13) 0.036(10) 0.035(13) F19 0.131(14) 0.284(21) 0.095(10) 0.055(11) 0.040(11) 0.058(15) F20 0.284(31) 0.209(21) 0.077(9) 0.028(11) 0.068(16) -0.018(21) F21 0.055(7) 0.143(11) 0.197(16) 0.014(13) 0.021(10) 0.048(8) F22 0.092(11) 0.118(12) 0.265(22) -0.083(15) 0.078(16) -0.005(9) N100 0.068(5) 0.083(6) 0.177(9) -0.021(6) -0.019(6) -0.002(5) C101 0.085(7) 0.061(5) 0.094(7) -0.008(5) -0.024(5) 0.005(5) C102 0.084(7) 0.095(7) 0.101(7) 0.022(6) -0.004(6) 0.005(6) N110 0.100(8) 0.117(8) 0.259(14) -0.027(8) -0.007(8) 0.019(7) C111 0.062(7) 0.086(8) 0.185(14) -0.018(8) 0.030(8) -0.006(6) C112 0.103(9) 0.106(8) 0.099(8) -0.010(6) 0.020(7) 0.014(7) N120 0.061(4) 0.060(4) 0.090(5) 0.003(4) 0.020(4) -0.007(4) C121 0.060(5) 0.040(4) 0.066(5) 0.001(3) 0.012(4) 0.013(4) C122 0.063(6) 0.050(4) 0.079(6) 0.014(4) 0.022(5) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N5 2.510(5) . y Sm1 N4 2.521(5) . y Sm1 N9 2.530(5) . y Sm1 N2 2.530(5) . y Sm1 N6 2.537(5) . y Sm1 N7 2.543(5) . y Sm1 N1 2.545(5) . y Sm1 N3 2.545(5) . y Sm1 N8 2.546(5) . y N1 C1 1.120(7) . y C1 C10 1.470(9) . ? N2 C2 1.127(7) . y C2 C20 1.439(8) . ? N3 C3 1.123(7) . y C3 C30 1.456(9) . ? N4 C4 1.126(7) . y C4 C40 1.470(9) . ? N5 C5 1.158(8) . y C5 C50 1.428(9) . ? N6 C6 1.117(7) . y C6 C60 1.456(8) . ? N7 C7 1.140(7) . y C7 C70 1.458(8) . ? N8 C8 1.127(7) . y C8 C80 1.455(8) . ? N9 C9 1.132(7) . y C9 C90 1.483(8) . ? As1 F5 1.613(6) . ? As1 F2 1.634(5) . ? As1 F6 1.634(5) . ? As1 F4 1.672(6) . ? As1 F1 1.685(5) . ? As1 F3 1.701(5) . ? As2 F9 1.663(4) . ? As2 F7 1.668(5) . ? As2 F12 1.677(5) . ? As2 F8 1.688(5) . ? As2 F11 1.690(4) . ? As2 F10 1.698(5) . ? As3 F18 1.633(14) . ? As3 F20 1.653(14) . ? As3 F15 1.656(13) . ? As3 F16 1.664(12) . ? As3 F13 1.671(5) . ? As3 F22 1.672(14) . ? As3 F14 1.672(5) . ? As3 F19 1.696(14) . ? As3 F21 1.697(11) . ? As3 F17 1.736(13) . ? N100 C101 1.143(11) . ? C101 C102 1.462(10) . ? N110 C111 1.146(13) . ? C111 C112 1.449(12) . ? N120 C121 1.151(8) . ? C121 C122 1.452(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Sm1 N4 71.9(2) . . y N5 Sm1 N9 134.2(2) . . y N4 Sm1 N9 73.7(2) . . y N5 Sm1 N2 90.9(2) . . y N4 Sm1 N2 138.4(2) . . y N9 Sm1 N2 134.7(2) . . y N5 Sm1 N6 72.6(2) . . y N4 Sm1 N6 71.8(2) . . y N9 Sm1 N6 68.4(2) . . y N2 Sm1 N6 139.7(2) . . y N5 Sm1 N7 73.1(2) . . y N4 Sm1 N7 67.34(15) . . y N9 Sm1 N7 119.1(2) . . y N2 Sm1 N7 71.5(2) . . y N6 Sm1 N7 132.8(2) . . y N5 Sm1 N1 140.6(2) . . y N4 Sm1 N1 96.7(2) . . y N9 Sm1 N1 72.5(2) . . y N2 Sm1 N1 72.6(2) . . y N6 Sm1 N1 140.9(2) . . y N7 Sm1 N1 67.9(2) . . y N5 Sm1 N3 139.7(2) . . y N4 Sm1 N3 142.1(2) . . y N9 Sm1 N3 68.4(2) . . y N2 Sm1 N3 73.2(2) . . y N6 Sm1 N3 95.7(2) . . y N7 Sm1 N3 131.2(2) . . y N1 Sm1 N3 70.2(2) . . y N5 Sm1 N8 69.2(2) . . y N4 Sm1 N8 132.9(2) . . y N9 Sm1 N8 118.3(2) . . y N2 Sm1 N8 67.7(2) . . y N6 Sm1 N8 72.1(2) . . y N7 Sm1 N8 122.6(2) . . y N1 Sm1 N8 130.2(2) . . y N3 Sm1 N8 70.5(2) . . y C1 N1 Sm1 161.4(5) . . y N1 C1 C10 177.1(8) . . y C2 N2 Sm1 154.8(6) . . y N2 C2 C20 177.9(7) . . y C3 N3 Sm1 164.2(5) . . y N3 C3 C30 176.1(7) . . y C4 N4 Sm1 158.2(5) . . y N4 C4 C40 175.4(7) . . y C5 N5 Sm1 164.6(5) . . y N5 C5 C50 176.7(7) . . y C6 N6 Sm1 164.2(5) . . y N6 C6 C60 178.8(7) . . y C7 N7 Sm1 169.7(5) . . y N7 C7 C70 178.8(7) . . y C8 N8 Sm1 165.0(5) . . y N8 C8 C80 177.1(7) . . y C9 N9 Sm1 165.2(5) . . y N9 C9 C90 179.4(7) . . y F5 As1 F2 88.5(4) . . ? F5 As1 F6 91.6(4) . . ? F2 As1 F6 179.8(4) . . ? F5 As1 F4 177.9(4) . . ? F2 As1 F4 90.0(4) . . ? F6 As1 F4 89.8(4) . . ? F5 As1 F1 92.2(4) . . ? F2 As1 F1 88.7(3) . . ? F6 As1 F1 91.3(3) . . ? F4 As1 F1 86.2(3) . . ? F5 As1 F3 89.7(4) . . ? F2 As1 F3 90.0(3) . . ? F6 As1 F3 90.0(3) . . ? F4 As1 F3 91.8(3) . . ? F1 As1 F3 177.6(3) . . ? F9 As2 F7 90.3(3) . . ? F9 As2 F12 178.1(3) . . ? F7 As2 F12 87.8(3) . . ? F9 As2 F8 91.8(3) . . ? F7 As2 F8 177.5(3) . . ? F12 As2 F8 90.1(3) . . ? F9 As2 F11 88.8(3) . . ? F7 As2 F11 89.9(2) . . ? F12 As2 F11 91.1(3) . . ? F8 As2 F11 88.7(2) . . ? F9 As2 F10 90.0(3) . . ? F7 As2 F10 89.8(3) . . ? F12 As2 F10 90.1(3) . . ? F8 As2 F10 91.6(2) . . ? F11 As2 F10 178.8(3) . . ? F18 As3 F15 91.3(7) . . ? F18 As3 F16 87.9(8) . . ? F16 As3 F15 175.6(8) . . ? F18 As3 F13 96.2(7) . . ? F15 As3 F13 90.1(6) . . ? F16 As3 F13 94.3(6) . . ? F18 As3 F14 85.9(7) . . ? F15 As3 F14 88.0(6) . . ? F16 As3 F14 87.6(6) . . ? F13 As3 F14 177.2(3) . . ? F18 As3 F17 176.2(8) . . ? F15 As3 F17 88.9(6) . . ? F16 As3 F17 91.5(7) . . ? F13 As3 F17 87.5(5) . . ? F14 As3 F17 90.4(5) . . ? N100 C101 C102 174.6(12) . . ? N110 C111 C112 170.6(15) . . ? N120 C121 C122 178.7(8) . . ? _refine_diff_density_max .783 _refine_diff_density_min -.700 _refine_diff_density_rms .102 #=END data_bg3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 Al3 Cl12 N10 Pr' _chemical_formula_weight 1057.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' 'Pr' 'Pr' -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.0970(10) _cell_length_b 13.2510(10) _cell_length_c 14.2070(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.49 _cell_angle_gamma 90.00 _cell_volume 2338.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 4.917 _cell_measurement_theta_max 12.541 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.811 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4097 _exptl_absorpt_correction_T_max 0.4646 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 12319 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10520 _reflns_number_gt 9542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material SHELXL-97 _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^)+(0.0286P)^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 refU _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00203(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.262(8) _refine_ls_number_reflns 10520 _refine_ls_number_parameters 428 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.282179(12) 0.384167(15) 0.109025(11) 0.02077(5) Uani 1 1 d . . . N1 N 0.4903(2) 0.3723(3) 0.1711(2) 0.0363(8) Uani 1 1 d . . . C10 C 0.5789(3) 0.3748(4) 0.2138(2) 0.0291(7) Uani 1 1 d . . . C11 C 0.6935(2) 0.3799(5) 0.2705(3) 0.0380(8) Uani 1 1 d . . . H11A H 0.7232 0.4441 0.2568 0.097(4) Uiso 1 1 calc R . . H11B H 0.7315 0.3239 0.2512 0.097(4) Uiso 1 1 calc R . . H11C H 0.7027 0.3752 0.3416 0.097(4) Uiso 1 1 calc R . . N2 N 0.3215(3) 0.2950(3) -0.0375(2) 0.0336(7) Uani 1 1 d . . . C20 C 0.3258(3) 0.2572(3) -0.1080(3) 0.0315(8) Uani 1 1 d . . . C21 C 0.3309(4) 0.2080(4) -0.1981(3) 0.0462(11) Uani 1 1 d . . . H21A H 0.2695 0.1622 -0.2230 0.097(4) Uiso 1 1 calc R . . H21B H 0.3980 0.1696 -0.1834 0.097(4) Uiso 1 1 calc R . . H21C H 0.3285 0.2592 -0.2485 0.097(4) Uiso 1 1 calc R . . N3 N 0.3312(3) 0.2020(3) 0.1748(3) 0.0350(8) Uani 1 1 d . . . C30 C 0.3505(3) 0.1295(3) 0.2192(3) 0.0305(8) Uani 1 1 d . . . C31 C 0.3765(4) 0.0376(3) 0.2765(4) 0.0436(10) Uani 1 1 d . . . H31A H 0.4039 0.0542 0.3473 0.097(4) Uiso 1 1 calc R . . H31B H 0.4316 0.0003 0.2575 0.097(4) Uiso 1 1 calc R . . H31C H 0.3117 -0.0041 0.2634 0.097(4) Uiso 1 1 calc R . . N4 N 0.2898(3) 0.5635(3) 0.1858(3) 0.0348(8) Uani 1 1 d . . . C40 C 0.3049(4) 0.6299(3) 0.2385(3) 0.0365(9) Uani 1 1 d . . . C41 C 0.3232(5) 0.7158(4) 0.3070(4) 0.0570(14) Uani 1 1 d . . . H41A H 0.3566 0.6920 0.3752 0.097(4) Uiso 1 1 calc R . . H41B H 0.2543 0.7483 0.3013 0.097(4) Uiso 1 1 calc R . . H41C H 0.3710 0.7646 0.2903 0.097(4) Uiso 1 1 calc R . . N5 N 0.1365(3) 0.4737(3) -0.0329(2) 0.0366(7) Uani 1 1 d . . . C50 C 0.0794(3) 0.5041(3) -0.1046(3) 0.0367(9) Uani 1 1 d . . . C51 C 0.0061(4) 0.5449(4) -0.1968(4) 0.0582(14) Uani 1 1 d . . . H51A H -0.0412 0.4910 -0.2336 0.097(4) Uiso 1 1 calc R . . H51B H 0.0477 0.5724 -0.2373 0.097(4) Uiso 1 1 calc R . . H51C H -0.0376 0.5986 -0.1814 0.097(4) Uiso 1 1 calc R . . N6 N 0.1266(2) 0.3952(3) 0.1854(2) 0.0341(7) Uani 1 1 d . . . C60 C 0.0687(3) 0.3929(4) 0.2294(2) 0.0315(7) Uani 1 1 d . . . C61 C -0.0067(3) 0.3882(6) 0.2864(3) 0.0491(10) Uani 1 1 d . . . H61A H -0.0734 0.3554 0.2465 0.097(4) Uiso 1 1 calc R . . H61B H -0.0227 0.4567 0.3035 0.097(4) Uiso 1 1 calc R . . H61C H 0.0256 0.3493 0.3473 0.097(4) Uiso 1 1 calc R . . N7 N 0.3685(3) 0.5095(3) 0.0164(3) 0.0373(7) Uani 1 1 d . . . C70 C 0.4055(3) 0.5596(3) -0.0284(3) 0.0346(8) Uani 1 1 d . . . C71 C 0.4531(4) 0.6231(4) -0.0863(4) 0.0558(13) Uani 1 1 d . . . H71A H 0.4639 0.6912 -0.0579 0.097(4) Uiso 1 1 calc R . . H71B H 0.4051 0.6263 -0.1550 0.097(4) Uiso 1 1 calc R . . H71C H 0.5227 0.5948 -0.0851 0.097(4) Uiso 1 1 calc R . . N8 N 0.1297(3) 0.2599(2) 0.0222(3) 0.0351(7) Uani 1 1 d . . . C80 C 0.0677(3) 0.2075(3) -0.0276(3) 0.0375(9) Uani 1 1 d . . . C81 C -0.0126(4) 0.1408(4) -0.0936(4) 0.0636(15) Uani 1 1 d . . . H81A H -0.0767 0.1382 -0.0721 0.097(4) Uiso 1 1 calc R . . H81B H 0.0175 0.0728 -0.0911 0.097(4) Uiso 1 1 calc R . . H81C H -0.0325 0.1666 -0.1616 0.097(4) Uiso 1 1 calc R . . N9 N 0.3594(2) 0.3793(4) 0.30116(19) 0.0326(6) Uani 1 1 d . . . C90 C 0.3993(3) 0.3726(4) 0.3841(2) 0.0298(8) Uani 1 1 d . . . C91 C 0.4499(4) 0.3653(4) 0.4909(3) 0.0475(13) Uani 1 1 d . . . H91A H 0.4080 0.3195 0.5187 0.097(4) Uiso 1 1 calc R . . H91B H 0.4524 0.4323 0.5208 0.097(4) Uiso 1 1 calc R . . H91C H 0.5232 0.3392 0.5054 0.097(4) Uiso 1 1 calc R . . Al1 Al 0.26262(10) 0.58438(10) -0.41130(9) 0.0358(3) Uani 1 1 d . . . Cl1 Cl 0.39470(11) 0.68453(10) -0.39643(11) 0.0460(3) Uani 1 1 d . . . Cl2 Cl 0.20586(11) 0.53288(12) -0.56007(9) 0.0635(4) Uani 1 1 d . . . Cl3 Cl 0.13966(10) 0.65778(12) -0.36986(12) 0.0595(3) Uani 1 1 d . . . Cl4 Cl 0.32236(13) 0.45915(10) -0.31484(11) 0.0693(4) Uani 1 1 d . . . Al2 Al 0.25442(10) 0.86782(10) 0.01444(9) 0.0372(3) Uani 1 1 d . . . Cl5 Cl 0.15767(8) 0.88264(19) 0.10851(9) 0.0633(3) Uani 1 1 d . . . Cl6 Cl 0.19600(12) 0.74690(9) -0.08623(10) 0.0547(3) Uani 1 1 d . . . Cl8 Cl 0.24892(16) 1.00504(10) -0.06434(13) 0.0719(4) Uani 1 1 d . . . Cl7 Cl 0.41670(10) 0.83841(13) 0.10115(11) 0.0685(4) Uani 1 1 d . . . Al3 Al 0.24055(10) 0.07090(9) 0.50012(9) 0.0316(2) Uani 1 1 d . . . Cl9 Cl 0.40285(11) 0.09001(12) 0.59524(11) 0.0522(4) Uani 1 1 d . . . Cl10 Cl 0.13325(9) 0.07663(9) 0.58521(9) 0.0419(2) Uani 1 1 d . . . Cl11 Cl 0.20266(10) 0.18597(9) 0.39018(9) 0.0512(3) Uani 1 1 d . . . Cl12 Cl 0.22879(10) -0.07350(8) 0.43086(9) 0.0485(3) Uani 1 1 d . . . N100 N 0.0534(6) 0.2894(6) 0.7428(4) 0.106(2) Uani 1 1 d . . . C100 C 0.0467(5) 0.3125(5) 0.6650(4) 0.0651(15) Uani 1 1 d . . . C101 C 0.0395(4) 0.3397(4) 0.5655(4) 0.0591(13) Uani 1 1 d . . . H10A H -0.0106 0.2941 0.5187 0.097(4) Uiso 1 1 calc R . . H10B H 0.1108 0.3342 0.5572 0.097(4) Uiso 1 1 calc R . . H10C H 0.0136 0.4092 0.5524 0.097(4) 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 Pr1 0.02014(7) 0.02245(7) 0.01921(7) -0.00074(11) 0.00552(5) -0.00036(11) N1 0.0283(14) 0.045(2) 0.0353(14) -0.0010(18) 0.0095(11) -0.0017(17) C10 0.0292(15) 0.0271(19) 0.0327(15) 0.0014(18) 0.0122(12) 0.0025(19) C11 0.0261(15) 0.0410(19) 0.0423(18) 0.003(3) 0.0042(13) -0.004(3) N2 0.0341(17) 0.0402(18) 0.0279(16) -0.0045(14) 0.0117(14) -0.0032(14) C20 0.0319(19) 0.0317(19) 0.0306(19) -0.0049(15) 0.0096(15) -0.0039(15) C21 0.063(3) 0.046(3) 0.034(2) -0.0101(18) 0.023(2) -0.008(2) N3 0.0369(19) 0.0297(17) 0.0353(18) 0.0009(14) 0.0071(15) 0.0020(15) C30 0.031(2) 0.029(2) 0.0296(19) -0.0067(15) 0.0076(16) -0.0001(16) C31 0.048(3) 0.029(2) 0.052(3) 0.0089(19) 0.013(2) 0.0022(19) N4 0.042(2) 0.0279(17) 0.0328(17) -0.0047(14) 0.0095(15) -0.0021(15) C40 0.045(2) 0.030(2) 0.030(2) -0.0002(16) 0.0056(18) 0.0028(18) C41 0.092(4) 0.034(2) 0.040(3) -0.0148(19) 0.014(3) -0.002(3) N5 0.0312(17) 0.0378(18) 0.0365(18) 0.0057(15) 0.0045(15) -0.0027(14) C50 0.032(2) 0.036(2) 0.035(2) 0.0095(16) 0.0018(17) -0.0059(17) C51 0.051(3) 0.064(3) 0.045(3) 0.023(2) -0.006(2) -0.005(2) N6 0.0301(13) 0.042(2) 0.0325(13) -0.0028(17) 0.0137(11) -0.0031(17) C60 0.0268(14) 0.037(2) 0.0283(14) -0.004(2) 0.0058(12) 0.000(2) C61 0.0364(18) 0.074(3) 0.045(2) -0.014(4) 0.0233(16) -0.013(4) N7 0.0380(18) 0.0339(17) 0.0440(19) 0.0059(15) 0.0188(16) 0.0006(14) C70 0.034(2) 0.032(2) 0.039(2) 0.0020(16) 0.0133(17) -0.0032(16) C71 0.064(3) 0.061(3) 0.052(3) 0.006(2) 0.032(3) -0.016(3) N8 0.0284(16) 0.0328(17) 0.0416(18) -0.0035(15) 0.0077(14) -0.0063(14) C80 0.034(2) 0.033(2) 0.046(2) 0.0001(17) 0.0129(18) -0.0063(17) C81 0.049(3) 0.057(3) 0.074(4) -0.018(3) 0.004(3) -0.023(2) N9 0.0355(13) 0.0355(15) 0.0251(12) 0.000(2) 0.0069(10) 0.006(2) C90 0.0294(15) 0.032(2) 0.0284(15) -0.0003(17) 0.0092(12) 0.0017(18) C91 0.054(2) 0.056(4) 0.0253(17) 0.0027(18) 0.0031(16) 0.009(2) Al1 0.0352(6) 0.0379(7) 0.0342(6) -0.0051(5) 0.0109(5) -0.0058(5) Cl1 0.0347(7) 0.0451(7) 0.0586(8) -0.0011(6) 0.0152(6) -0.0071(5) Cl2 0.0603(8) 0.0851(10) 0.0418(6) -0.0254(7) 0.0115(6) -0.0142(7) Cl3 0.0455(7) 0.0704(9) 0.0722(9) -0.0197(7) 0.0322(6) -0.0075(6) Cl4 0.0779(9) 0.0507(7) 0.0699(8) 0.0190(6) 0.0101(7) -0.0071(7) Al2 0.0364(5) 0.0383(9) 0.0356(5) -0.0030(5) 0.0093(4) 0.0006(5) Cl5 0.0391(5) 0.0951(9) 0.0614(6) -0.0080(12) 0.0241(5) 0.0014(11) Cl6 0.0749(9) 0.0327(6) 0.0471(6) -0.0050(5) 0.0059(6) -0.0067(6) Cl8 0.1101(13) 0.0311(6) 0.0764(10) 0.0023(6) 0.0325(10) -0.0052(7) Cl7 0.0322(6) 0.1038(11) 0.0652(8) -0.0182(7) 0.0092(5) 0.0103(6) Al3 0.0325(6) 0.0312(6) 0.0307(5) 0.0003(4) 0.0094(5) -0.0005(5) Cl9 0.0318(6) 0.0637(9) 0.0543(8) -0.0029(7) 0.0042(6) -0.0051(6) Cl10 0.0376(5) 0.0481(6) 0.0442(6) 0.0036(5) 0.0191(5) 0.0050(5) Cl11 0.0626(7) 0.0425(6) 0.0475(6) 0.0146(5) 0.0161(6) 0.0035(5) Cl12 0.0619(7) 0.0356(5) 0.0517(6) -0.0093(5) 0.0234(5) -0.0047(5) N100 0.154(6) 0.116(5) 0.058(3) 0.012(3) 0.048(4) 0.039(5) C100 0.072(4) 0.073(4) 0.052(3) 0.002(3) 0.022(3) 0.019(3) C101 0.062(3) 0.060(3) 0.056(3) 0.007(2) 0.020(3) 0.010(3) _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 Pr1 N8 2.581(3) . y Pr1 N2 2.583(3) . y Pr1 N5 2.584(3) . y Pr1 N1 2.590(3) . y Pr1 N7 2.591(3) . y Pr1 N9 2.594(3) . y Pr1 N3 2.595(4) . y Pr1 N6 2.599(3) . y Pr1 N4 2.603(3) . y N1 C10 1.126(4) . y C10 C11 1.463(4) . ? N2 C20 1.138(5) . y C20 C21 1.456(5) . ? N3 C30 1.133(5) . y C30 C31 1.444(6) . ? N4 C40 1.132(5) . y C40 C41 1.467(6) . ? N5 C50 1.129(5) . y C50 C51 1.460(5) . ? N6 C60 1.125(4) . y C60 C61 1.463(5) . ? N7 C70 1.129(5) . y C70 C71 1.449(6) . ? N8 C80 1.130(5) . y C80 C81 1.464(6) . ? N9 C90 1.131(4) . y C90 C91 1.454(5) . ? Al1 Cl3 2.1183(18) . ? Al1 Cl2 2.1188(16) . ? Al1 Cl4 2.1363(19) . ? Al1 Cl1 2.1368(18) . ? Al2 Cl6 2.1223(18) . ? Al2 Cl5 2.1224(16) . ? Al2 Cl8 2.1244(19) . ? Al2 Cl7 2.1273(17) . ? Al3 Cl11 2.1258(16) . ? Al3 Cl10 2.1259(16) . ? Al3 Cl12 2.1348(16) . ? Al3 Cl9 2.1416(18) . ? N100 C100 1.123(7) . ? C100 C101 1.433(7) . ? 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 N8 Pr1 N2 69.18(10) . . y N8 Pr1 N5 69.62(11) . . y N2 Pr1 N5 82.40(11) . . y N8 Pr1 N1 134.07(12) . . y N2 Pr1 N1 77.86(10) . . y N5 Pr1 N1 136.97(11) . . y N8 Pr1 N7 124.22(11) . . y N2 Pr1 N7 69.72(11) . . y N5 Pr1 N7 69.06(11) . . y N1 Pr1 N7 68.30(11) . . y N8 Pr1 N9 118.13(12) . . y N2 Pr1 N9 136.54(12) . . y N5 Pr1 N9 141.05(12) . . y N1 Pr1 N9 67.86(9) . . y N7 Pr1 N9 117.60(12) . . y N8 Pr1 N3 69.14(11) . . y N2 Pr1 N3 76.99(11) . . y N5 Pr1 N3 138.19(11) . . y N1 Pr1 N3 73.00(13) . . y N7 Pr1 N3 132.96(11) . . y N9 Pr1 N3 68.19(13) . . y N8 Pr1 N6 69.23(11) . . y N2 Pr1 N6 138.19(11) . . y N5 Pr1 N6 79.46(11) . . y N1 Pr1 N6 137.81(9) . . y N7 Pr1 N6 134.60(12) . . y N9 Pr1 N6 69.96(9) . . y N3 Pr1 N6 92.24(13) . . y N8 Pr1 N4 134.74(11) . . y N2 Pr1 N4 139.82(11) . . y N5 Pr1 N4 80.12(11) . . y N1 Pr1 N4 90.92(12) . . y N7 Pr1 N4 70.28(11) . . y N9 Pr1 N4 68.38(13) . . y N3 Pr1 N4 136.57(10) . . y N6 Pr1 N4 72.82(13) . . y C10 N1 Pr1 167.1(3) . . y N1 C10 C11 178.7(5) . . y C20 N2 Pr1 171.7(3) . . y N2 C20 C21 179.5(5) . . y C30 N3 Pr1 167.3(3) . . y N3 C30 C31 179.3(5) . . y C40 N4 Pr1 164.3(3) . . y N4 C40 C41 179.3(5) . . y C50 N5 Pr1 168.9(4) . . y N5 C50 C51 179.2(5) . . y C60 N6 Pr1 170.3(3) . . y N6 C60 C61 179.2(6) . . y C70 N7 Pr1 175.6(3) . . y N7 C70 C71 179.5(5) . . y C80 N8 Pr1 170.0(3) . . y N8 C80 C81 178.9(5) . . y C90 N9 Pr1 174.6(3) . . y N9 C90 C91 179.1(5) . . y Cl3 Al1 Cl2 111.59(8) . . ? Cl3 Al1 Cl4 109.54(8) . . ? Cl2 Al1 Cl4 109.33(8) . . ? Cl3 Al1 Cl1 110.51(8) . . ? Cl2 Al1 Cl1 108.40(8) . . ? Cl4 Al1 Cl1 107.38(8) . . ? Cl6 Al2 Cl5 109.54(9) . . ? Cl6 Al2 Cl8 110.27(7) . . ? Cl5 Al2 Cl8 108.98(10) . . ? Cl6 Al2 Cl7 109.42(8) . . ? Cl5 Al2 Cl7 109.79(7) . . ? Cl8 Al2 Cl7 108.82(9) . . ? Cl11 Al3 Cl10 110.47(7) . . ? Cl11 Al3 Cl12 109.78(7) . . ? Cl10 Al3 Cl12 109.27(7) . . ? Cl11 Al3 Cl9 109.42(8) . . ? Cl10 Al3 Cl9 109.87(7) . . ? Cl12 Al3 Cl9 108.00(8) . . ? N100 C100 C101 178.5(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.127 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.071 #=END data_YB1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H24 Al3 Cl12 N8 Yb1' _chemical_formula_weight 1007.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 25.281(4) _cell_length_b 15.536(2) _cell_length_c 10.370(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4073.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 15.773 _cell_measurement_theta_max 29.968 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 3.170 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.438 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Walker & Stuart, 1983' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 6094 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4848 _reflns_number_observed 3704 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0338P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4848 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_obs 0.0340 _refine_ls_wR_factor_all 0.0788 _refine_ls_wR_factor_obs 0.0754 _refine_ls_goodness_of_fit_all 0.931 _refine_ls_goodness_of_fit_obs 1.026 _refine_ls_restrained_S_all 0.931 _refine_ls_restrained_S_obs 1.026 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Yb1 Yb 0.162258(8) 0.2500 0.19842(2) 0.02452(7) Uani 1 d S . N1 N 0.0741(2) 0.2500 0.1071(4) 0.0324(10) Uani 1 d S . C1 C 0.0328(2) 0.2500 0.0635(5) 0.0316(12) Uani 1 d S . C2 C -0.0195(2) 0.2500 0.0083(6) 0.0426(14) Uani 1 d S . H2A H -0.0316(8) 0.30946(5) -0.0029(42) 0.067(5) Uiso 0.50 calc PR . H2B H -0.0438(4) 0.2195(26) 0.0660(22) 0.067(5) Uiso 0.50 calc PR . H2C H -0.0187(4) 0.2211(26) -0.0756(21) 0.067(5) Uiso 0.50 calc PR . N2 N 0.2542(2) 0.2500 0.1505(5) 0.0388(11) Uani 1 d S . C3 C 0.2986(2) 0.2500 0.1377(6) 0.0386(14) Uani 1 d S . C4 C 0.3565(2) 0.2500 0.1202(7) 0.056(2) Uani 1 d S . H4A H 0.3683(3) 0.1920(8) 0.0970(53) 0.067(5) Uiso 0.50 calc PR . H4B H 0.3736(2) 0.2678(35) 0.2007(18) 0.067(5) Uiso 0.50 calc PR . H4C H 0.3660(3) 0.2903(27) 0.0512(38) 0.067(5) Uiso 0.50 calc PR . N3 N 0.1000(2) 0.2500 0.3689(5) 0.0368(11) Uani 1 d S . C5 C 0.0645(2) 0.2500 0.4353(5) 0.0357(13) Uani 1 d S . C6 C 0.0194(2) 0.2500 0.5214(6) 0.055(2) Uani 1 d S . H6A H 0.0289(6) 0.2790(25) 0.6021(18) 0.067(5) Uiso 0.50 calc PR . H6B H 0.0089(11) 0.19053(4) 0.5399(33) 0.067(5) Uiso 0.50 calc PR . H6C H -0.0101(6) 0.2805(24) 0.4806(19) 0.067(5) Uiso 0.50 calc PR . N4 N 0.20190(12) 0.1558(2) 0.3559(3) 0.0375(8) Uani 1 d . . C7 C 0.21866(14) 0.1062(3) 0.4260(4) 0.0323(8) Uani 1 d . . C8 C 0.2400(2) 0.0424(2) 0.5144(4) 0.0370(9) Uani 1 d . . H8A H 0.2580(10) 0.0715(2) 0.5857(16) 0.067(5) Uiso 1 calc R . H8B H 0.2652(9) 0.0056(12) 0.4685(8) 0.067(5) Uiso 1 calc R . H8C H 0.2111(2) 0.0070(13) 0.5484(22) 0.067(5) Uiso 1 calc R . N5 N 0.13969(14) 0.1047(2) 0.1459(3) 0.0394(8) Uani 1 d . . C9 C 0.1180(2) 0.0424(3) 0.1340(4) 0.0373(9) Uani 1 d . . C10 C 0.0886(2) -0.0378(3) 0.1202(5) 0.0512(12) Uani 1 d . . H10A H 0.0851(10) -0.0655(10) 0.2047(7) 0.067(5) Uiso 1 calc R . H10B H 0.1076(6) -0.0763(8) 0.0614(23) 0.067(5) Uiso 1 calc R . H10C H 0.0534(5) -0.0256(3) 0.0853(27) 0.067(5) Uiso 1 calc R . N6 N 0.1707(2) 0.2500 -0.0310(5) 0.0398(12) Uani 1 d S . C11 C 0.1696(2) 0.2500 -0.1406(6) 0.0387(13) Uani 1 d S . C12 C 0.1683(2) 0.2500 -0.2819(6) 0.054(2) Uani 1 d S . H12A H 0.1385(11) 0.2850(23) -0.3119(6) 0.067(5) Uiso 0.50 calc PR . H12B H 0.1642(17) 0.1909(3) -0.3132(6) 0.067(5) Uiso 0.50 calc PR . H12C H 0.2015(8) 0.2741(26) -0.3152(6) 0.067(5) Uiso 0.50 calc PR . Al1 Al 0.33215(6) 0.2500 0.7391(2) 0.0280(3) Uani 1 d S . Cl1 Cl 0.41313(5) 0.2500 0.79272(15) 0.0426(3) Uani 1 d S . Cl2 Cl 0.29481(4) 0.13806(7) 0.81509(11) 0.0484(3) Uani 1 d . . Cl3 Cl 0.32511(6) 0.2500 0.53441(14) 0.0432(3) Uani 1 d S . Al2 Al 0.41994(5) 0.00331(8) 0.20866(12) 0.0363(3) Uani 1 d . . Cl4 Cl 0.34590(5) 0.04385(13) 0.28786(14) 0.0738(4) Uani 1 d . . Cl5 Cl 0.47696(5) 0.10102(8) 0.2382(2) 0.0661(4) Uani 1 d . . Cl6 Cl 0.44445(6) -0.10898(9) 0.30956(15) 0.0713(4) Uani 1 d . . Cl7 Cl 0.40925(5) -0.02275(10) 0.01090(12) 0.0690(4) Uani 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 Yb1 0.02395(10) 0.02430(11) 0.02530(11) 0.000 0.00101(10) 0.000 N1 0.032(2) 0.031(3) 0.034(3) 0.000 0.003(2) 0.000 C1 0.040(3) 0.021(3) 0.033(3) 0.000 0.001(2) 0.000 C2 0.032(3) 0.047(4) 0.049(4) 0.000 -0.010(3) 0.000 N2 0.035(2) 0.051(3) 0.031(2) 0.000 0.001(2) 0.000 C3 0.032(3) 0.053(4) 0.030(3) 0.000 0.001(2) 0.000 C4 0.027(3) 0.085(6) 0.054(4) 0.000 0.006(3) 0.000 N3 0.033(2) 0.045(3) 0.032(3) 0.000 0.003(2) 0.000 C5 0.038(3) 0.042(3) 0.027(3) 0.000 -0.002(2) 0.000 C6 0.042(3) 0.081(5) 0.044(4) 0.000 0.015(3) 0.000 N4 0.033(2) 0.042(2) 0.037(2) 0.005(2) -0.0047(15) -0.0027(15) C7 0.033(2) 0.034(2) 0.030(2) -0.004(2) -0.003(2) -0.002(2) C8 0.046(2) 0.030(2) 0.035(2) 0.006(2) -0.005(2) 0.004(2) N5 0.049(2) 0.030(2) 0.039(2) 0.000(2) -0.007(2) -0.001(2) C9 0.046(2) 0.026(2) 0.039(2) -0.002(2) -0.008(2) 0.008(2) C10 0.056(3) 0.029(2) 0.069(3) -0.003(2) 0.000(3) -0.005(2) N6 0.033(2) 0.048(3) 0.038(3) 0.000 -0.002(2) 0.000 C11 0.028(3) 0.052(4) 0.037(3) 0.000 0.001(2) 0.000 C12 0.040(3) 0.090(6) 0.031(3) 0.000 0.005(3) 0.000 Al1 0.0295(7) 0.0245(8) 0.0299(8) 0.000 -0.0022(7) 0.000 Cl1 0.0303(6) 0.0572(9) 0.0403(7) 0.000 -0.0039(6) 0.000 Cl2 0.0570(6) 0.0396(6) 0.0486(6) 0.0098(5) 0.0003(5) -0.0144(5) Cl3 0.0569(9) 0.0420(8) 0.0309(7) 0.000 -0.0085(6) 0.000 Al2 0.0388(6) 0.0344(7) 0.0356(6) -0.0030(6) 0.0001(6) -0.0018(5) Cl4 0.0497(7) 0.1122(13) 0.0595(8) -0.0140(8) 0.0137(6) 0.0137(7) Cl5 0.0675(8) 0.0460(7) 0.0847(10) -0.0107(7) -0.0044(7) -0.0204(6) Cl6 0.0805(9) 0.0501(8) 0.0833(10) 0.0246(8) -0.0101(8) -0.0042(6) Cl7 0.0651(8) 0.0989(12) 0.0429(6) -0.0221(7) -0.0062(6) 0.0087(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N3 2.367(5) . ? Yb1 N2 2.378(5) . ? Yb1 N6 2.388(5) . ? Yb1 N5 2.391(4) . ? Yb1 N5 2.391(4) 7_565 ? Yb1 N4 2.411(3) 7_565 ? Yb1 N4 2.411(3) . ? Yb1 N1 2.422(4) . ? N1 C1 1.138(7) . ? C1 C2 1.441(7) . ? N2 C3 1.128(7) . ? C3 C4 1.475(8) . ? N3 C5 1.131(7) . ? C5 C6 1.449(8) . ? N4 C7 1.141(5) . ? C7 C8 1.454(5) . ? N5 C9 1.119(5) . ? C9 C10 1.458(6) . ? N6 C11 1.137(8) . ? C11 C12 1.467(9) . ? Al1 Cl1 2.121(2) . ? Al1 Cl3 2.130(2) . ? Al1 Cl2 2.1300(14) . ? Al1 Cl2 2.1300(14) 7_565 ? Al2 Cl7 2.108(2) . ? Al2 Cl5 2.116(2) . ? Al2 Cl6 2.127(2) . ? Al2 Cl4 2.139(2) . ? 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 Yb1 N2 143.7(2) . . ? N3 Yb1 N6 143.5(2) . . ? N2 Yb1 N6 72.8(2) . . ? N3 Yb1 N5 90.65(9) . . ? N2 Yb1 N5 100.71(9) . . ? N6 Yb1 N5 78.14(9) . . ? N3 Yb1 N5 90.65(9) . 7_565 ? N2 Yb1 N5 100.71(9) . 7_565 ? N6 Yb1 N5 78.14(9) . 7_565 ? N5 Yb1 N5 141.5(2) . 7_565 ? N3 Yb1 N4 76.72(12) . 7_565 ? N2 Yb1 N4 74.63(11) . 7_565 ? N6 Yb1 N4 129.61(10) . 7_565 ? N5 Yb1 N4 145.73(12) . 7_565 ? N5 Yb1 N4 71.37(12) 7_565 7_565 ? N3 Yb1 N4 76.72(12) . . ? N2 Yb1 N4 74.63(11) . . ? N6 Yb1 N4 129.61(10) . . ? N5 Yb1 N4 71.37(12) . . ? N5 Yb1 N4 145.73(12) 7_565 . ? N4 Yb1 N4 74.7(2) 7_565 . ? N3 Yb1 N1 71.4(2) . . ? N2 Yb1 N1 144.9(2) . . ? N6 Yb1 N1 72.10(15) . . ? N5 Yb1 N1 72.02(8) . . ? N5 Yb1 N1 72.02(8) 7_565 . ? N4 Yb1 N1 130.35(10) 7_565 . ? N4 Yb1 N1 130.35(10) . . ? C1 N1 Yb1 179.6(4) . . ? N1 C1 C2 179.9(5) . . ? C3 N2 Yb1 174.7(5) . . ? N2 C3 C4 179.7(7) . . ? C5 N3 Yb1 169.1(4) . . ? N3 C5 C6 179.4(6) . . ? C7 N4 Yb1 174.8(3) . . ? N4 C7 C8 179.5(4) . . ? C9 N5 Yb1 163.4(3) . . ? N5 C9 C10 178.6(5) . . ? C11 N6 Yb1 173.4(5) . . ? N6 C11 C12 179.8(3) . . ? Cl1 Al1 Cl3 110.00(9) . . ? Cl1 Al1 Cl2 109.31(6) . . ? Cl3 Al1 Cl2 109.37(6) . . ? Cl1 Al1 Cl2 109.31(6) . 7_565 ? Cl3 Al1 Cl2 109.37(6) . 7_565 ? Cl2 Al1 Cl2 109.47(10) . 7_565 ? Cl7 Al2 Cl5 111.48(8) . . ? Cl7 Al2 Cl6 111.01(8) . . ? Cl5 Al2 Cl6 108.59(8) . . ? Cl7 Al2 Cl4 108.54(8) . . ? Cl5 Al2 Cl4 109.22(8) . . ? Cl6 Al2 Cl4 107.92(9) . . ? _refine_diff_density_max 1.415 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.125