# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; Department of Chemistry Monash University Clayton, Vic. 3168 AUSTRALIA ; _publ_contact_author_email 'glen.deacon@monash.edu and peter.junk@monash.edu' _publ_contact_author_fax '+61 3 9905 4597' _publ_contact_author_phone '+61 3 9905 4570 and +61 3 9905 4568' _publ_contact_author_name 'Prof. Glen B. Deacon and Prof. Peter C. Junk' _publ_section_title ; The effect of the lanthanoid element on (Ar)-C-F-Ln coordination and C-F activation ; loop_ _publ_author_name 'G. B. Deacon' 'C. M. Forsyth' 'P. C. Junk' 'R. P. Kelly' 'A. Urbatsch' 'J. Wang' data_[La(p-HC6F4NC2H4NEt2)3].PhMe.CIF _database_code_depnum_ccdc_archive 'CCDC 859374' _chemical_name_systematic ; tris(N,N-diethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine-F,N,N'/F,N) -lanthanum(iii) toluene solvate ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point '138\%C (dec.)' _chemical_formula_moiety 'C36 H45 F12 La N6,1/2(C7 H8),1/2(C7 H8)' _chemical_formula_sum 'C43 H53 F12 La N6' _chemical_formula_weight 1020.82 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.168(2) _cell_length_b 11.251(2) _cell_length_c 20.709(4) _cell_angle_alpha 102.76(3) _cell_angle_beta 99.50(3) _cell_angle_gamma 92.84(3) _cell_volume 2269.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 41028 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 30.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28470 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7794 _reflns_number_gt 7091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Toluene solvate molecules were refined each with two half occupancies on two sites by symmetry. C34 displays disorders and has been solved with two half occupancies on two sites. 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. The highest difference electron density peak is 3.68 e\%A^-3^ and is located 1.31 \%A from C20 in a chemically non-sensical position. The spurious residual peaks presumably result from unaccounted for twinning. The ethyl group C33, C34 was modelled as disordered with C34 occupying two positions ca 2.0 \%A apart with refined occupancies of 0.62:0.38 The lattice toluene molecules were modelled as disordered over a symmetry site and were refined as isotropic atoms with their geometry restrained to typical values (eg. C-C 1.39 \%A; C-C-C 120\%; Ar-C(Me) 1.50 \%A) and occupancies fixed at 0.5. ; _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^)+(0.0416P)^2^+21.3371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7794 _refine_ls_number_parameters 572 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.221 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.58687(4) 0.83541(4) 0.73273(2) 0.01402(13) Uani 1 1 d . . . F1 F 0.4209(4) 1.0223(4) 0.7260(2) 0.0220(9) Uani 1 1 d . . . N1 N 0.5289(7) 0.9595(6) 0.8372(3) 0.0228(14) Uani 1 1 d . . . C1 C 0.5644(9) 0.9118(8) 0.8978(4) 0.0305(19) Uani 1 1 d . . . H1A H 0.4853 0.9077 0.9197 0.037 Uiso 1 1 calc R . . H1B H 0.6361 0.9674 0.9302 0.037 Uiso 1 1 calc R . . F2 F 0.2856(5) 1.2215(4) 0.7238(2) 0.0332(11) Uani 1 1 d . . . N2 N 0.5245(6) 0.7025(6) 0.8209(3) 0.0213(13) Uani 1 1 d . . . C2 C 0.6113(8) 0.7871(7) 0.8793(4) 0.0260(17) Uani 1 1 d . . . H2A H 0.7026 0.7954 0.8691 0.031 Uiso 1 1 calc R . . H2B H 0.6173 0.7500 0.9187 0.031 Uiso 1 1 calc R . . F3 F 0.3606(9) 1.3209(6) 0.9597(3) 0.076(2) Uani 1 1 d . . . N3 N 0.8158(6) 0.7741(6) 0.7604(3) 0.0212(13) Uani 1 1 d . . . C3 C 0.4633(8) 1.0623(7) 0.8436(4) 0.0275(18) Uani 1 1 d . . . F4 F 0.4986(8) 1.1322(5) 0.9638(3) 0.068(2) Uani 1 1 d . . . N4 N 0.7868(6) 1.0116(6) 0.7430(3) 0.0223(14) Uani 1 1 d . . . C4 C 0.4054(8) 1.0972(7) 0.7851(4) 0.0239(17) Uani 1 1 d . . . F5 F 0.6467(4) 0.6162(4) 0.6661(2) 0.0209(9) Uani 1 1 d . . . N5 N 0.4897(6) 0.8133(6) 0.6171(3) 0.0188(13) Uani 1 1 d . A . C5 C 0.3355(8) 1.1979(7) 0.7826(4) 0.0279(18) Uani 1 1 d . . . F6 F 0.6997(5) 0.3895(4) 0.6112(2) 0.0364(12) Uani 1 1 d . . . N6 N 0.6940(7) 0.7042(7) 0.4822(3) 0.0350(18) Uani 1 1 d . . . C6 C 0.3167(10) 1.2759(8) 0.8412(5) 0.040(2) Uani 1 1 d . . . H6 H 0.2680 1.3458 0.8409 0.048 Uiso 1 1 calc R . . F7 F 1.1230(5) 0.4594(5) 0.7533(3) 0.0492(14) Uani 1 1 d . . . C7 C 0.3724(11) 1.2465(9) 0.8994(5) 0.045(3) Uani 1 1 d . . . F8 F 1.0706(5) 0.6805(4) 0.8089(3) 0.0428(13) Uani 1 1 d . . . C8 C 0.4438(11) 1.1465(9) 0.9028(4) 0.043(2) Uani 1 1 d . . . F9 F 0.3166(4) 0.7627(4) 0.6915(2) 0.0225(9) Uani 1 1 d . . . C9 C 0.3820(8) 0.6957(7) 0.8303(4) 0.0244(17) Uani 1 1 d . . . H9A H 0.3270 0.6428 0.7890 0.029 Uiso 1 1 calc R . . H9B H 0.3508 0.7786 0.8352 0.029 Uiso 1 1 calc R . . F10 F 0.0508(4) 0.7485(5) 0.6535(2) 0.0318(11) Uani 1 1 d . A . C10 C 0.3571(8) 0.6466(8) 0.8907(4) 0.0313(19) Uani 1 1 d . . . H10A H 0.3831 0.5627 0.8853 0.047 Uiso 1 1 calc R . . H10B H 0.2619 0.6470 0.8935 0.047 Uiso 1 1 calc R . . H10C H 0.4104 0.6985 0.9319 0.047 Uiso 1 1 calc R . . F11 F 0.1094(5) 0.8475(5) 0.4499(2) 0.0351(11) Uani 1 1 d . A . C11 C 0.5753(9) 0.5797(7) 0.8106(4) 0.0309(19) Uani 1 1 d . . . H11A H 0.5779 0.5504 0.8524 0.037 Uiso 1 1 calc R . . H11B H 0.6682 0.5870 0.8024 0.037 Uiso 1 1 calc R . . F12 F 0.3686(5) 0.8680(4) 0.4867(2) 0.0285(10) Uani 1 1 d . . . C12 C 0.4928(11) 0.4857(9) 0.7530(6) 0.055(3) Uani 1 1 d . . . H12A H 0.4064 0.4651 0.7647 0.082 Uiso 1 1 calc R . . H12B H 0.5404 0.4118 0.7440 0.082 Uiso 1 1 calc R . . H12C H 0.4779 0.5189 0.7127 0.082 Uiso 1 1 calc R . . C13 C 0.9154(8) 0.8720(7) 0.8013(4) 0.0247(17) Uani 1 1 d . . . H13A H 0.9956 0.8731 0.7800 0.030 Uiso 1 1 calc R . . H13B H 0.9431 0.8560 0.8465 0.030 Uiso 1 1 calc R . . C14 C 0.8593(8) 0.9940(7) 0.8083(4) 0.0244(17) Uani 1 1 d . . . H14A H 0.7971 1.0012 0.8408 0.029 Uiso 1 1 calc R . . H14B H 0.9332 1.0595 0.8265 0.029 Uiso 1 1 calc R . . C15 C 0.8577(7) 0.6634(6) 0.7366(4) 0.0169(15) Uani 1 1 d . . . C16 C 0.7676(7) 0.5767(7) 0.6879(4) 0.0190(15) Uani 1 1 d . . . C17 C 0.7953(8) 0.4608(7) 0.6595(4) 0.0247(17) Uani 1 1 d . . . C18 C 0.9149(9) 0.4176(7) 0.6797(4) 0.0314(19) Uani 1 1 d . . . H18 H 0.9350 0.3374 0.6603 0.038 Uiso 1 1 calc R . . C19 C 1.0047(8) 0.4971(8) 0.7297(5) 0.033(2) Uani 1 1 d . . . C20 C 0.9764(8) 0.6132(7) 0.7584(4) 0.0248(17) Uani 1 1 d . . . C21 C 0.8726(8) 0.9915(7) 0.6900(4) 0.0256(17) Uani 1 1 d . . . H21A H 0.8199 1.0045 0.6479 0.031 Uiso 1 1 calc R . . H21B H 0.8934 0.9050 0.6813 0.031 Uiso 1 1 calc R . . C22 C 1.0047(9) 1.0731(8) 0.7065(5) 0.038(2) Uani 1 1 d . . . H22A H 0.9858 1.1589 0.7115 0.056 Uiso 1 1 calc R . . H22B H 1.0553 1.0501 0.6699 0.056 Uiso 1 1 calc R . . H22C H 1.0575 1.0624 0.7486 0.056 Uiso 1 1 calc R . . C23 C 0.7369(8) 1.1348(7) 0.7525(5) 0.032(2) Uani 1 1 d . . . H23A H 0.8139 1.1975 0.7699 0.038 Uiso 1 1 calc R . . H23B H 0.6782 1.1435 0.7866 0.038 Uiso 1 1 calc R . . C24 C 0.6597(10) 1.1577(8) 0.6880(5) 0.041(2) Uani 1 1 d . . . H24A H 0.7225 1.1745 0.6593 0.061 Uiso 1 1 calc R . . H24B H 0.6077 1.2281 0.6987 0.061 Uiso 1 1 calc R . . H24C H 0.5990 1.0852 0.6643 0.061 Uiso 1 1 calc R . . C25 C 0.5914(7) 0.8129(7) 0.5745(4) 0.0213(16) Uani 1 1 d . . . H25A H 0.6810 0.8256 0.6035 0.026 Uiso 1 1 calc R A . H25B H 0.5815 0.8829 0.5528 0.026 Uiso 1 1 calc R . . C26 C 0.5854(8) 0.6976(8) 0.5204(4) 0.0261(17) Uani 1 1 d . . . H26A H 0.5930 0.6265 0.5412 0.031 Uiso 1 1 calc R . . H26B H 0.4980 0.6860 0.4895 0.031 Uiso 1 1 calc R . . C27 C 0.3566(7) 0.8110(6) 0.5907(3) 0.0165(14) Uani 1 1 d . . . C28 C 0.2636(7) 0.7857(6) 0.6301(3) 0.0179(15) Uani 1 1 d . . . C29 C 0.1291(8) 0.7788(7) 0.6111(4) 0.0222(16) Uani 1 1 d . . . C30 C 0.0688(8) 0.7968(7) 0.5498(4) 0.0250(17) Uani 1 1 d . . . H30 H -0.0256 0.7904 0.5358 0.030 Uiso 1 1 calc R . . C31 C 0.1579(8) 0.8250(7) 0.5101(4) 0.0227(16) Uani 1 1 d . . . C32 C 0.2932(8) 0.8330(7) 0.5291(4) 0.0212(16) Uani 1 1 d . . . C33 C 0.7210(12) 0.5821(11) 0.4479(5) 0.057(3) Uani 0.359(17) 1 d P A 1 H33A H 0.7365 0.5351 0.4832 0.068 Uiso 0.359(17) 1 calc PR A 1 H33B H 0.6356 0.5452 0.4181 0.068 Uiso 0.359(17) 1 calc PR A 1 C34 C 0.822(2) 0.553(2) 0.4085(13) 0.035(7) Uani 0.359(17) 1 d P A 1 H34A H 0.8056 0.5896 0.3693 0.053 Uiso 0.359(17) 1 calc PR A 1 H34B H 0.8206 0.4644 0.3933 0.053 Uiso 0.359(17) 1 calc PR A 1 H34C H 0.9098 0.5864 0.4357 0.053 Uiso 0.359(17) 1 calc PR A 1 C33A C 0.7210(12) 0.5821(11) 0.4479(5) 0.057(3) Uani 0.64 1 d P A 2 H33C H 0.7703 0.5879 0.4111 0.068 Uiso 0.641(17) 1 calc PR A 2 H33D H 0.6357 0.5310 0.4280 0.068 Uiso 0.641(17) 1 calc PR A 2 C34A C 0.8021(16) 0.5258(13) 0.4977(8) 0.044(4) Uani 0.641(17) 1 d P A 2 H34D H 0.8483 0.4598 0.4740 0.066 Uiso 0.641(17) 1 calc PR A 2 H34E H 0.7433 0.4924 0.5236 0.066 Uiso 0.641(17) 1 calc PR A 2 H34F H 0.8683 0.5880 0.5282 0.066 Uiso 0.641(17) 1 calc PR A 2 C35 C 0.6550(9) 0.7794(10) 0.4327(5) 0.045(3) Uani 1 1 d . . . H35A H 0.5828 0.8297 0.4465 0.054 Uiso 1 1 calc R . . H35B H 0.6199 0.7248 0.3880 0.054 Uiso 1 1 calc R . . C36 C 0.7711(12) 0.8606(9) 0.4280(6) 0.059(3) Uani 1 1 d . . . H36A H 0.8063 0.9142 0.4723 0.088 Uiso 1 1 calc R . . H36B H 0.7424 0.9105 0.3958 0.088 Uiso 1 1 calc R . . H36C H 0.8412 0.8107 0.4126 0.088 Uiso 1 1 calc R . . C37 C -0.113(4) 0.474(4) 0.9119(17) 0.149(14) Uiso 0.50 1 d PDU B -1 H37A H -0.1993 0.4364 0.9167 0.224 Uiso 0.50 1 calc PR B -1 H37B H -0.0716 0.4148 0.8810 0.224 Uiso 0.50 1 calc PR B -1 H37C H -0.1282 0.5466 0.8940 0.224 Uiso 0.50 1 calc PR B -1 C38 C -0.021(3) 0.510(2) 0.9806(15) 0.137(13) Uiso 0.50 1 d PDU B -1 C39 C 0.116(3) 0.521(3) 0.9845(16) 0.110(12) Uiso 0.50 1 d PD B -1 H39 H 0.1511 0.5048 0.9439 0.132 Uiso 0.50 1 calc PR B -1 C40 C 0.205(3) 0.554(3) 1.0451(17) 0.130(14) Uiso 0.50 1 d PD B -1 H40 H 0.2987 0.5587 1.0465 0.156 Uiso 0.50 1 calc PR B -1 C41 C 0.152(3) 0.580(3) 1.1039(16) 0.136(16) Uiso 0.50 1 d PD B -1 H41 H 0.2101 0.6078 1.1462 0.163 Uiso 0.50 1 calc PR B -1 C42 C 0.015(3) 0.564(3) 1.1010(15) 0.130(15) Uiso 0.50 1 d PD B -1 H42 H -0.0200 0.5764 1.1414 0.157 Uiso 0.50 1 calc PR B -1 C43 C -0.070(3) 0.532(3) 1.0395(15) 0.091(10) Uiso 0.50 1 d PD B -1 H43 H -0.1642 0.5243 1.0381 0.110 Uiso 0.50 1 calc PR B -1 C44 C -0.074(4) 1.191(3) 1.0103(18) 0.134(11) Uiso 0.50 1 d PDU C -1 H44A H -0.0021 1.2556 1.0334 0.201 Uiso 0.50 1 calc PR C -1 H44B H -0.1441 1.1924 1.0374 0.201 Uiso 0.50 1 calc PR C -1 H44C H -0.1113 1.2060 0.9663 0.201 Uiso 0.50 1 calc PR C -1 C45 C -0.018(3) 1.069(2) 1.0007(12) 0.111(10) Uiso 0.50 1 d PDU C -1 C46 C 0.099(3) 1.068(3) 0.9726(15) 0.108(13) Uiso 0.50 1 d PD C -1 H46 H 0.1375 1.1378 0.9612 0.130 Uiso 0.50 1 calc PR C -1 C47 C 0.152(3) 0.957(3) 0.9633(17) 0.130(14) Uiso 0.50 1 d PD C -1 H47 H 0.2300 0.9451 0.9434 0.156 Uiso 0.50 1 calc PR C -1 C48 C 0.093(3) 0.868(3) 0.9827(17) 0.116(13) Uiso 0.50 1 d PD C -1 H48 H 0.1360 0.7941 0.9777 0.139 Uiso 0.50 1 calc PR C -1 C49 C -0.024(3) 0.865(2) 1.0093(16) 0.096(10) Uiso 0.50 1 d PD C -1 H49 H -0.0603 0.7941 1.0205 0.115 Uiso 0.50 1 calc PR C -1 C50 C -0.083(2) 0.975(2) 1.0181(13) 0.067(7) Uiso 0.50 1 d PD C -1 H50 H -0.1644 0.9842 1.0351 0.080 Uiso 0.50 1 calc PR C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0133(2) 0.0159(2) 0.0136(2) 0.00610(14) 0.00165(14) -0.00023(14) F1 0.027(2) 0.021(2) 0.018(2) 0.0024(17) 0.0059(17) 0.0041(17) N1 0.028(4) 0.021(3) 0.020(3) 0.007(3) 0.004(3) -0.002(3) C1 0.037(5) 0.036(5) 0.017(4) 0.006(3) 0.003(3) -0.002(4) F2 0.036(3) 0.027(3) 0.040(3) 0.016(2) 0.005(2) 0.011(2) N2 0.022(3) 0.023(3) 0.023(3) 0.011(3) 0.007(3) 0.001(3) C2 0.023(4) 0.036(5) 0.021(4) 0.016(3) 0.001(3) -0.003(3) F3 0.147(7) 0.052(4) 0.038(3) 0.007(3) 0.035(4) 0.050(4) N3 0.021(3) 0.021(3) 0.021(3) 0.006(3) 0.003(3) -0.002(3) C3 0.033(5) 0.022(4) 0.027(4) 0.002(3) 0.011(3) -0.005(3) F4 0.134(7) 0.045(4) 0.025(3) 0.006(3) 0.011(3) 0.030(4) N4 0.019(3) 0.021(3) 0.028(3) 0.010(3) 0.004(3) 0.002(3) C4 0.029(4) 0.023(4) 0.020(4) 0.002(3) 0.010(3) -0.004(3) F5 0.015(2) 0.025(2) 0.022(2) 0.0077(17) -0.0017(16) -0.0006(17) N5 0.018(3) 0.024(3) 0.016(3) 0.009(2) 0.002(2) -0.001(2) C5 0.028(5) 0.021(4) 0.037(5) 0.004(3) 0.016(4) 0.001(3) F6 0.040(3) 0.025(3) 0.038(3) 0.003(2) -0.004(2) 0.002(2) N6 0.029(4) 0.062(5) 0.024(4) 0.019(3) 0.015(3) 0.019(3) C6 0.049(6) 0.033(5) 0.044(5) 0.010(4) 0.021(5) 0.017(4) F7 0.025(3) 0.044(3) 0.080(4) 0.019(3) 0.003(3) 0.018(2) C7 0.067(7) 0.034(5) 0.036(5) -0.005(4) 0.026(5) 0.016(5) F8 0.023(3) 0.033(3) 0.062(4) 0.007(2) -0.017(2) 0.005(2) C8 0.069(7) 0.043(6) 0.019(4) 0.004(4) 0.015(4) 0.010(5) F9 0.019(2) 0.034(3) 0.018(2) 0.0135(18) 0.0038(17) 0.0007(18) C9 0.022(4) 0.029(4) 0.022(4) 0.009(3) 0.000(3) -0.006(3) F10 0.019(2) 0.048(3) 0.035(3) 0.018(2) 0.0119(19) 0.004(2) C10 0.024(4) 0.046(5) 0.030(4) 0.019(4) 0.009(3) -0.001(4) F11 0.034(3) 0.051(3) 0.024(2) 0.019(2) 0.000(2) 0.014(2) C11 0.034(5) 0.022(4) 0.048(5) 0.020(4) 0.021(4) 0.008(3) F12 0.030(3) 0.042(3) 0.021(2) 0.019(2) 0.0085(19) 0.008(2) C12 0.068(8) 0.029(5) 0.070(7) -0.001(5) 0.044(6) -0.008(5) C13 0.025(4) 0.023(4) 0.025(4) 0.009(3) -0.003(3) -0.003(3) C14 0.020(4) 0.026(4) 0.025(4) 0.006(3) 0.000(3) -0.004(3) C15 0.011(4) 0.003(3) 0.034(4) 0.004(3) 0.000(3) 0.002(2) C16 0.009(4) 0.026(4) 0.027(4) 0.017(3) 0.002(3) 0.004(3) C17 0.026(4) 0.021(4) 0.025(4) 0.004(3) 0.002(3) -0.007(3) C18 0.033(5) 0.021(4) 0.045(5) 0.016(4) 0.008(4) 0.005(3) C19 0.021(5) 0.032(5) 0.049(5) 0.019(4) -0.001(4) 0.009(3) C20 0.021(4) 0.016(4) 0.038(5) 0.009(3) 0.004(3) -0.001(3) C21 0.020(4) 0.027(4) 0.033(4) 0.012(3) 0.009(3) -0.002(3) C22 0.028(5) 0.039(5) 0.049(6) 0.012(4) 0.017(4) -0.010(4) C23 0.027(5) 0.020(4) 0.054(6) 0.010(4) 0.019(4) 0.002(3) C24 0.044(6) 0.034(5) 0.056(6) 0.025(4) 0.022(5) 0.008(4) C25 0.016(4) 0.027(4) 0.026(4) 0.014(3) 0.006(3) 0.003(3) C26 0.019(4) 0.038(5) 0.022(4) 0.008(3) 0.002(3) 0.006(3) C27 0.019(4) 0.015(3) 0.017(3) 0.004(3) 0.005(3) 0.003(3) C28 0.017(4) 0.021(4) 0.016(4) 0.009(3) -0.001(3) 0.001(3) C29 0.023(4) 0.021(4) 0.026(4) 0.009(3) 0.008(3) 0.001(3) C30 0.015(4) 0.033(4) 0.028(4) 0.008(3) 0.002(3) 0.008(3) C31 0.020(4) 0.028(4) 0.020(4) 0.008(3) -0.003(3) 0.009(3) C32 0.028(4) 0.022(4) 0.018(4) 0.007(3) 0.012(3) 0.005(3) C33 0.068(8) 0.080(8) 0.036(6) 0.021(5) 0.028(5) 0.044(6) C34 0.024(14) 0.044(15) 0.047(15) 0.016(12) 0.024(11) 0.005(10) C35 0.032(5) 0.081(8) 0.033(5) 0.027(5) 0.013(4) 0.019(5) C36 0.081(9) 0.032(5) 0.057(7) 0.024(5) -0.021(6) -0.005(5) C34A 0.055(10) 0.022(7) 0.059(10) 0.009(7) 0.017(8) 0.011(6) C33A 0.068(8) 0.080(8) 0.036(6) 0.021(5) 0.028(5) 0.044(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 N5 2.388(6) . ? La1 N3 2.473(6) . ? La1 N1 2.479(6) . ? La1 F5 2.699(4) . ? La1 N4 2.717(6) . ? La1 N2 2.731(6) . ? La1 F9 2.765(4) . ? La1 F1 2.773(4) . ? F1 C4 1.362(8) . ? N1 C3 1.356(11) . ? N1 C1 1.470(10) . ? C1 C2 1.494(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? F2 C5 1.327(10) . ? N2 C11 1.483(10) . ? N2 C2 1.484(10) . ? N2 C9 1.495(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? F3 C7 1.368(10) . ? N3 C15 1.352(9) . ? N3 C13 1.467(9) . ? C3 C4 1.401(11) . ? C3 C8 1.423(11) . ? F4 C8 1.341(11) . ? N4 C23 1.483(10) . ? N4 C14 1.487(10) . ? N4 C21 1.497(10) . ? C4 C5 1.373(12) . ? F5 C16 1.368(8) . ? N5 C27 1.369(9) . ? N5 C25 1.466(9) . ? C5 C6 1.380(12) . ? F6 C17 1.355(9) . ? N6 C33 1.463(13) . ? N6 C26 1.468(10) . ? N6 C35 1.485(11) . ? C6 C7 1.361(14) . ? C6 H6 0.9500 . ? F7 C19 1.347(9) . ? C7 C8 1.377(14) . ? F8 C20 1.354(9) . ? F9 C28 1.381(8) . ? C9 C10 1.526(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C29 1.363(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? F11 C31 1.345(8) . ? C11 C12 1.507(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C32 1.362(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.499(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.407(10) . ? C15 C20 1.407(10) . ? C16 C17 1.370(11) . ? C17 C18 1.367(12) . ? C18 C19 1.380(12) . ? C18 H18 0.9500 . ? C19 C20 1.376(12) . ? C21 C22 1.534(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.514(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.505(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.404(10) . ? C27 C32 1.412(10) . ? C28 C29 1.353(11) . ? C29 C30 1.378(11) . ? C30 C31 1.390(11) . ? C30 H30 0.9500 . ? C31 C32 1.359(11) . ? C33 C34 1.42(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.487(15) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.527(18) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C43 1.37(4) . ? C38 C39 1.387(19) . ? C39 C40 1.382(18) . ? C39 H39 0.9500 . ? C40 C41 1.389(18) . ? C40 H40 0.9500 . ? C41 C42 1.383(19) . ? C41 H41 0.9500 . ? C42 C43 1.382(18) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.497(18) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.372(17) . ? C45 C46 1.405(18) . ? C46 C47 1.375(18) . ? C46 H46 0.9500 . ? C47 C48 1.320(18) . ? C47 H47 0.9500 . ? C48 C49 1.392(18) . ? C48 H48 0.9500 . ? C49 C50 1.394(18) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 La1 N3 118.6(2) . . ? N5 La1 N1 131.3(2) . . ? N3 La1 N1 108.0(2) . . ? N5 La1 F5 73.41(17) . . ? N3 La1 F5 61.28(17) . . ? N1 La1 F5 147.64(17) . . ? N5 La1 N4 98.8(2) . . ? N3 La1 N4 65.03(19) . . ? N1 La1 N4 88.0(2) . . ? F5 La1 N4 110.74(16) . . ? N5 La1 N2 128.9(2) . . ? N3 La1 N2 85.09(19) . . ? N1 La1 N2 65.66(19) . . ? F5 La1 N2 82.51(16) . . ? N4 La1 N2 132.05(19) . . ? N5 La1 F9 61.18(16) . . ? N3 La1 F9 147.40(17) . . ? N1 La1 F9 87.08(18) . . ? F5 La1 F9 90.33(13) . . ? N4 La1 F9 146.22(16) . . ? N2 La1 F9 74.92(16) . . ? N5 La1 F1 72.66(17) . . ? N3 La1 F1 148.25(17) . . ? N1 La1 F1 60.03(17) . . ? F5 La1 F1 144.55(12) . . ? N4 La1 F1 84.44(16) . . ? N2 La1 F1 111.58(16) . . ? F9 La1 F1 64.31(13) . . ? C4 F1 La1 117.6(4) . . ? C3 N1 C1 117.2(6) . . ? C3 N1 La1 127.2(5) . . ? C1 N1 La1 115.6(5) . . ? N1 C1 C2 110.0(6) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C11 N2 C2 109.6(6) . . ? C11 N2 C9 110.9(6) . . ? C2 N2 C9 111.2(6) . . ? C11 N2 La1 114.1(4) . . ? C2 N2 La1 92.8(4) . . ? C9 N2 La1 116.7(4) . . ? N2 C2 C1 114.6(7) . . ? N2 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C15 N3 C13 118.4(6) . . ? C15 N3 La1 125.9(5) . . ? C13 N3 La1 115.5(5) . . ? N1 C3 C4 118.6(7) . . ? N1 C3 C8 129.6(8) . . ? C4 C3 C8 111.7(8) . . ? C23 N4 C14 110.0(6) . . ? C23 N4 C21 111.5(6) . . ? C14 N4 C21 111.6(6) . . ? C23 N4 La1 111.4(5) . . ? C14 N4 La1 93.9(4) . . ? C21 N4 La1 117.1(4) . . ? F1 C4 C5 118.3(7) . . ? F1 C4 C3 115.6(7) . . ? C5 C4 C3 126.1(7) . . ? C16 F5 La1 117.9(4) . . ? C27 N5 C25 120.7(6) . . ? C27 N5 La1 126.9(4) . . ? C25 N5 La1 112.1(4) . . ? F2 C5 C4 120.5(7) . . ? F2 C5 C6 119.2(8) . . ? C4 C5 C6 120.3(8) . . ? C33 N6 C26 111.2(8) . . ? C33 N6 C35 110.4(7) . . ? C26 N6 C35 108.5(7) . . ? C7 C6 C5 115.7(8) . . ? C7 C6 H6 122.1 . . ? C5 C6 H6 122.1 . . ? C6 C7 F3 119.2(8) . . ? C6 C7 C8 124.6(8) . . ? F3 C7 C8 116.1(9) . . ? F4 C8 C7 118.1(8) . . ? F4 C8 C3 120.3(9) . . ? C7 C8 C3 121.5(8) . . ? C28 F9 La1 113.7(4) . . ? N2 C9 C10 115.0(6) . . ? N2 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? N2 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 114.0(8) . . ? N2 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N2 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 110.8(6) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N4 C14 C13 112.3(6) . . ? N4 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? N3 C15 C16 118.2(6) . . ? N3 C15 C20 129.5(7) . . ? C16 C15 C20 111.9(6) . . ? F5 C16 C17 119.2(7) . . ? F5 C16 C15 115.8(6) . . ? C17 C16 C15 124.9(7) . . ? F6 C17 C18 120.8(7) . . ? F6 C17 C16 117.9(7) . . ? C18 C17 C16 121.2(7) . . ? C17 C18 C19 116.2(8) . . ? C17 C18 H18 121.9 . . ? C19 C18 H18 121.9 . . ? F7 C19 C20 118.1(8) . . ? F7 C19 C18 119.4(8) . . ? C20 C19 C18 122.4(8) . . ? F8 C20 C19 116.7(7) . . ? F8 C20 C15 120.2(7) . . ? C19 C20 C15 123.0(7) . . ? N4 C21 C22 115.8(7) . . ? N4 C21 H21A 108.3 . . ? C22 C21 H21A 108.3 . . ? N4 C21 H21B 108.3 . . ? C22 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 112.7(7) . . ? N4 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N4 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 114.8(6) . . ? N5 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? N5 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.5 . . ? N6 C26 C25 110.7(7) . . ? N6 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? N5 C27 C28 117.5(6) . . ? N5 C27 C32 130.6(6) . . ? C28 C27 C32 111.8(6) . . ? C29 C28 F9 119.2(6) . . ? C29 C28 C27 124.8(7) . . ? F9 C28 C27 116.0(6) . . ? C28 C29 F10 118.3(7) . . ? C28 C29 C30 122.6(7) . . ? F10 C29 C30 119.1(7) . . ? C29 C30 C31 114.3(7) . . ? C29 C30 H30 122.9 . . ? C31 C30 H30 122.9 . . ? F11 C31 C32 117.4(7) . . ? F11 C31 C30 119.1(7) . . ? C32 C31 C30 123.5(7) . . ? C31 C32 F12 117.2(7) . . ? C31 C32 C27 123.0(7) . . ? F12 C32 C27 119.7(7) . . ? C34 C33 N6 126.6(14) . . ? C34 C33 H33A 105.7 . . ? N6 C33 H33A 105.7 . . ? C34 C33 H33B 105.7 . . ? N6 C33 H33B 105.7 . . ? H33A C33 H33B 106.1 . . ? N6 C35 C36 111.0(8) . . ? N6 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? N6 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C43 C38 C39 118(2) . . ? C43 C38 C37 122(3) . . ? C39 C38 C37 120(3) . . ? C40 C39 C38 123(2) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C39 C40 C41 118(2) . . ? C39 C40 H40 121.0 . . ? C41 C40 H40 121.0 . . ? C42 C41 C40 120(2) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 120(2) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C38 C43 C42 121(3) . . ? C38 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C50 C45 C46 128(2) . . ? C50 C45 C44 119(2) . . ? C46 C45 C44 113(2) . . ? C47 C46 C45 114(2) . . ? C47 C46 H46 123.2 . . ? C45 C46 H46 123.2 . . ? C48 C47 C46 118(2) . . ? C48 C47 H47 121.0 . . ? C46 C47 H47 121.0 . . ? C47 C48 C49 130(2) . . ? C47 C48 H48 115.1 . . ? C49 C48 H48 115.1 . . ? C48 C49 C50 114(2) . . ? C48 C49 H49 123.0 . . ? C50 C49 H49 123.0 . . ? C45 C50 C49 116.1(19) . . ? C45 C50 H50 122.0 . . ? C49 C50 H50 122.0 . . ? H34D C34A H34E 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 3.679 _refine_diff_density_min -3.042 _refine_diff_density_rms 0.145 # Attachment '2 [LaF(p-HC6F4NC2H4NMe2)2]3.1.5PhMe.CIF' data_[LaF(p-HC6F4NC2H4NMe2)2]3.3/2PhMe.CIF _database_code_depnum_ccdc_archive 'CCDC 859380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexa(N,N-dimethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine-F,N,N') -tris-fluoro-trislanthanum(iii) toluene solvate ; _chemical_name_common ? _chemical_melting_point '235\%C (dec.)' _chemical_formula_moiety 'C60 H66 F27 La3 N12,1.5(C7 H8)' _chemical_formula_sum 'C70.50 H78 F27 La3 N12' _chemical_formula_weight 2023.18 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 22.6999(3) _cell_length_b 22.6999(3) _cell_length_c 53.1241(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 23706.6(7) _cell_formula_units_Z 12 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 259544 _cell_measurement_theta_min 1.790 _cell_measurement_theta_max 30.095 _exptl_crystal_description rhombus _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11988 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5487 _exptl_absorpt_correction_T_max 0.8900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 178478 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 63 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9264 _reflns_number_gt 6352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; A toluene solvate molecule in asymmetric unit was refined with equal occupancies on two sites. 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. Lattice toluene solvent was modelled as disordered over two positions with each component refined with isotropic thermal parameters and the geometry restrained to typical values (eg. C-C 1.39 \%A; C-C-C 120 \%; Ar-C(Me) 1.50 \%A). The occupancies were fixed at 0.60:0.40 after a trial refinement and the thermal parameters of atoms of each component were constrained to be similar. ; _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^)+(0.0368P)^2^+848.8799P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9264 _refine_ls_number_parameters 679 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.86920(2) 0.96343(2) 0.108181(8) 0.02489(13) Uani 1 1 d . . . F1 F 0.9039(2) 0.9491(2) 0.06235(8) 0.0301(10) Uani 1 1 d . . . N1 N 0.7802(3) 0.8690(3) 0.08186(13) 0.0292(15) Uani 1 1 d . . . C1 C 0.7164(4) 0.8211(4) 0.09446(16) 0.036(2) Uani 1 1 d . . . H1A H 0.7094 0.7745 0.0932 0.043 Uiso 1 1 calc R . . H1B H 0.6779 0.8216 0.0859 0.043 Uiso 1 1 calc R . . La2 La 0.70402(2) 0.23979(2) 0.003372(9) 0.03228(15) Uani 1 1 d . . . F2 F 0.9474(2) 0.9174(2) 0.02081(9) 0.0358(11) Uani 1 1 d . . . N2 N 0.7802(3) 0.8537(3) 0.13509(13) 0.0311(15) Uani 1 1 d . . . C2 C 0.7172(4) 0.8393(5) 0.12189(16) 0.035(2) Uani 1 1 d . . . H2A H 0.7117 0.8798 0.1231 0.043 Uiso 1 1 calc R . . H2B H 0.6779 0.8013 0.1305 0.043 Uiso 1 1 calc R . . F3 F 0.7292(3) 0.7312(3) 0.00695(10) 0.0509(14) Uani 1 1 d . . . N3 N 0.8176(3) 1.0182(4) 0.13373(13) 0.0319(16) Uani 1 1 d . . . C3 C 0.7936(4) 0.8522(4) 0.05916(14) 0.0252(16) Uani 1 1 d . . . F4 F 0.6851(2) 0.7562(3) 0.04884(10) 0.0474(13) Uani 1 1 d . . . N4 N 0.8275(3) 1.0360(3) 0.08044(13) 0.0306(15) Uani 1 1 d . . . C4 C 0.7515(4) 0.7973(4) 0.04322(16) 0.0338(19) Uani 1 1 d . . . F5 F 0.9165(2) 1.0026(3) 0.15426(9) 0.0371(11) Uani 1 1 d . . . N5 N 0.6504(4) 0.1332(4) 0.02900(14) 0.0395(18) Uani 1 1 d . . . C5 C 0.7747(4) 0.7848(4) 0.02083(17) 0.0345(19) Uani 1 1 d . . . F6 F 0.9763(3) 1.0589(3) 0.19753(10) 0.0540(15) Uani 1 1 d . . . N6 N 0.6300(4) 0.1251(4) -0.02413(15) 0.0409(18) Uani 1 1 d . . . C6 C 0.8398(5) 0.8226(4) 0.01264(16) 0.035(2) Uani 1 1 d . . . H6 H 0.8553 0.8114 -0.0022 0.042 Uiso 1 1 calc R . . F7 F 0.8143(4) 1.1272(3) 0.21114(11) 0.0708(19) Uani 1 1 d . . . N7 N 0.7980(4) 0.2461(4) -0.02261(14) 0.0363(17) Uani 1 1 d . . . C7 C 0.8821(4) 0.8780(4) 0.02712(14) 0.0273(17) Uani 1 1 d . . . F8 F 0.7619(3) 1.0836(3) 0.16681(11) 0.0578(16) Uani 1 1 d . . . N8 N 0.8145(4) 0.2606(4) 0.03049(14) 0.0379(17) Uani 1 1 d . . . C8 C 0.8588(4) 0.8924(4) 0.04864(15) 0.0287(17) Uani 1 1 d . . . F9 F 0.9367(2) 0.9123(2) 0.10815(9) 0.0328(10) Uani 1 1 d . . . C9 C 0.7915(5) 0.7951(5) 0.13371(18) 0.042(2) Uani 1 1 d . . . H9A H 0.8333 0.8059 0.1428 0.062 Uiso 1 1 calc R . . H9B H 0.7959 0.7854 0.1161 0.062 Uiso 1 1 calc R . . H9C H 0.7529 0.7552 0.1414 0.062 Uiso 1 1 calc R . . F10 F 0.6657(3) 0.2479(3) 0.04975(10) 0.0430(12) Uani 1 1 d . . . C10 C 0.7741(5) 0.8661(5) 0.16194(17) 0.046(2) Uani 1 1 d . . . H10A H 0.7343 0.8264 0.1691 0.068 Uiso 1 1 calc R . . H10B H 0.7687 0.9062 0.1636 0.068 Uiso 1 1 calc R . . H10C H 0.8152 0.8741 0.1709 0.068 Uiso 1 1 calc R . . F11 F 0.6060(3) 0.2499(3) 0.09251(11) 0.0559(15) Uani 1 1 d . . . C11 C 0.7693(4) 1.0338(5) 0.12081(17) 0.038(2) Uani 1 1 d . . . H11A H 0.7858 1.0832 0.1221 0.045 Uiso 1 1 calc R . . H11B H 0.7244 1.0090 0.1292 0.045 Uiso 1 1 calc R . . F12 F 0.5281(5) 0.0175(4) 0.10429(15) 0.099(3) Uani 1 1 d . . . C12 C 0.7620(4) 1.0136(5) 0.09338(16) 0.036(2) Uani 1 1 d . . . H12A H 0.7340 0.9635 0.0922 0.043 Uiso 1 1 calc R . . H12B H 0.7373 1.0332 0.0845 0.043 Uiso 1 1 calc R . . F13 F 0.5819(4) 0.0114(3) 0.06137(13) 0.075(2) Uani 1 1 d . . . C13 C 0.8385(4) 1.0425(4) 0.15735(15) 0.0324(19) Uani 1 1 d . . . F14 F 0.7183(2) 0.2891(3) -0.04294(10) 0.0419(12) Uani 1 1 d . . . C14 C 0.8913(4) 1.0367(4) 0.16816(16) 0.0341(19) Uani 1 1 d . . . F15 F 0.7453(3) 0.3571(3) -0.08620(11) 0.0525(14) Uani 1 1 d . . . C15 C 0.9219(5) 1.0632(5) 0.19095(18) 0.044(2) Uani 1 1 d . . . F16 F 0.9315(3) 0.3241(4) -0.09921(11) 0.0661(18) Uani 1 1 d . . . C16 C 0.8978(6) 1.0958(5) 0.20589(18) 0.051(3) Uani 1 1 d . . . H16 H 0.9177 1.1151 0.2217 0.061 Uiso 1 1 calc R . . F17 F 0.9102(3) 0.2616(3) -0.05584(11) 0.0572(16) Uani 1 1 d . . . C17 C 0.8429(6) 1.0986(5) 0.1966(2) 0.054(3) Uani 1 1 d . . . F18 F 0.7543(2) 0.3583(2) 0.00361(10) 0.0407(12) Uani 1 1 d . . . C18 C 0.8146(5) 1.0754(5) 0.17361(17) 0.043(2) Uani 1 1 d . . . C19 C 0.8726(4) 1.1105(4) 0.08258(18) 0.038(2) Uani 1 1 d . . . H19A H 0.8512 1.1336 0.0743 0.057 Uiso 1 1 calc R . . H19B H 0.9163 1.1238 0.0745 0.057 Uiso 1 1 calc R . . H19C H 0.8801 1.1234 0.1004 0.057 Uiso 1 1 calc R . . C20 C 0.8134(5) 1.0178(5) 0.05395(16) 0.038(2) Uani 1 1 d . . . H20A H 0.7829 0.9686 0.0524 0.056 Uiso 1 1 calc R . . H20B H 0.8561 1.0309 0.0451 0.056 Uiso 1 1 calc R . . H20C H 0.7917 1.0417 0.0465 0.056 Uiso 1 1 calc R . . C21 C 0.6328(5) 0.0694(5) 0.01626(19) 0.045(2) Uani 1 1 d . . . H21A H 0.5832 0.0376 0.0176 0.055 Uiso 1 1 calc R . . H21B H 0.6566 0.0480 0.0244 0.055 Uiso 1 1 calc R . . C22 C 0.6532(5) 0.0830(5) -0.01124(18) 0.041(2) Uani 1 1 d . . . H22A H 0.7034 0.1059 -0.0124 0.049 Uiso 1 1 calc R . . H22B H 0.6344 0.0389 -0.0201 0.049 Uiso 1 1 calc R . . C23 C 0.6236(5) 0.1291(5) 0.05203(17) 0.039(2) Uani 1 1 d . . . C24 C 0.6302(5) 0.1887(5) 0.06322(18) 0.041(2) Uani 1 1 d . . . C25 C 0.6009(5) 0.1909(5) 0.08563(18) 0.044(2) Uani 1 1 d . . . C26 C 0.5654(6) 0.1338(6) 0.1001(2) 0.062(3) Uani 1 1 d . . . H26 H 0.5448 0.1346 0.1156 0.074 Uiso 1 1 calc R . . C27 C 0.5613(7) 0.0752(6) 0.0909(2) 0.070(3) Uani 1 1 d . . . C28 C 0.5887(6) 0.0720(5) 0.0682(2) 0.052(3) Uani 1 1 d . . . C29 C 0.5563(5) 0.0956(5) -0.0222(2) 0.050(2) Uani 1 1 d . . . H29A H 0.5336 0.0484 -0.0281 0.075 Uiso 1 1 calc R . . H29B H 0.5420 0.1219 -0.0326 0.075 Uiso 1 1 calc R . . H29C H 0.5438 0.0968 -0.0046 0.075 Uiso 1 1 calc R . . C30 C 0.6486(5) 0.1301(5) -0.05106(19) 0.049(2) Uani 1 1 d . . . H30A H 0.6221 0.0854 -0.0590 0.074 Uiso 1 1 calc R . . H30B H 0.6972 0.1456 -0.0526 0.074 Uiso 1 1 calc R . . H30C H 0.6388 0.1627 -0.0594 0.074 Uiso 1 1 calc R . . C31 C 0.8478(5) 0.2313(5) -0.01057(17) 0.042(2) Uani 1 1 d . . . H31A H 0.8940 0.2716 -0.0117 0.050 Uiso 1 1 calc R . . H31B H 0.8482 0.1930 -0.0194 0.050 Uiso 1 1 calc R . . C32 C 0.8283(5) 0.2126(5) 0.01700(17) 0.041(2) Uani 1 1 d . . . H32A H 0.7873 0.1669 0.0178 0.049 Uiso 1 1 calc R . . H32B H 0.8656 0.2102 0.0257 0.049 Uiso 1 1 calc R . . C33 C 0.8142(4) 0.2742(5) -0.04604(17) 0.037(2) Uani 1 1 d . . . C34 C 0.7730(4) 0.2985(5) -0.05666(17) 0.037(2) Uani 1 1 d . . . C35 C 0.7858(5) 0.3326(5) -0.07900(18) 0.041(2) Uani 1 1 d . . . C36 C 0.8400(5) 0.3437(5) -0.09392(19) 0.048(2) Uani 1 1 d . . . H36 H 0.8501 0.3679 -0.1094 0.057 Uiso 1 1 calc R . . C37 C 0.8784(5) 0.3169(6) -0.0847(2) 0.052(3) Uani 1 1 d . . . C38 C 0.8676(5) 0.2849(5) -0.06233(18) 0.041(2) Uani 1 1 d . . . C39 C 0.8016(5) 0.2399(5) 0.05711(18) 0.047(2) Uani 1 1 d . . . H39A H 0.8437 0.2466 0.0649 0.070 Uiso 1 1 calc R . . H39B H 0.7666 0.1918 0.0582 0.070 Uiso 1 1 calc R . . H39C H 0.7860 0.2675 0.0659 0.070 Uiso 1 1 calc R . . C40 C 0.8724(5) 0.3305(5) 0.0288(2) 0.048(2) Uani 1 1 d . . . H40A H 0.9132 0.3320 0.0356 0.071 Uiso 1 1 calc R . . H40B H 0.8623 0.3611 0.0386 0.071 Uiso 1 1 calc R . . H40C H 0.8802 0.3450 0.0112 0.071 Uiso 1 1 calc R . . C41 C 0.611(2) 0.605(2) 0.1215(8) 0.140(12) Uiso 0.40 1 d PDU A 1 H41A H 0.6425 0.6017 0.1329 0.210 Uiso 0.40 1 calc PR A 1 H41B H 0.6337 0.6267 0.1057 0.210 Uiso 0.40 1 calc PR A 1 H41C H 0.5721 0.5599 0.1180 0.210 Uiso 0.40 1 calc PR A 1 C42 C 0.5859(14) 0.6464(14) 0.1331(5) 0.138(10) Uiso 0.40 1 d PDU A 1 C43 C 0.598(2) 0.661(2) 0.1579(5) 0.129(10) Uiso 0.40 1 d PDU A 1 H43 H 0.6206 0.6432 0.1676 0.155 Uiso 0.40 1 calc PR A 1 C44 C 0.576(2) 0.702(2) 0.1690(6) 0.121(10) Uiso 0.40 1 d PDU A 1 H44 H 0.5879 0.7170 0.1860 0.145 Uiso 0.40 1 calc PR A 1 C45 C 0.538(2) 0.722(2) 0.1551(7) 0.137(10) Uiso 0.40 1 d PDU A 1 H45 H 0.5150 0.7418 0.1632 0.164 Uiso 0.40 1 calc PR A 1 C46 C 0.532(2) 0.712(2) 0.1295(7) 0.138(11) Uiso 0.40 1 d PDU A 1 H46 H 0.5181 0.7365 0.1190 0.165 Uiso 0.40 1 calc PR A 1 C47 C 0.548(2) 0.665(2) 0.1192(5) 0.138(11) Uiso 0.40 1 d PDU A 1 H47 H 0.5323 0.6467 0.1029 0.166 Uiso 0.40 1 calc PR A 1 C51 C 0.4615(10) 0.7045(12) 0.1170(4) 0.099(7) Uiso 0.60 1 d PDU B 2 H51A H 0.4209 0.6953 0.1265 0.148 Uiso 0.60 1 calc PR B 2 H51B H 0.4490 0.6701 0.1038 0.148 Uiso 0.60 1 calc PR B 2 H51C H 0.4815 0.7497 0.1093 0.148 Uiso 0.60 1 calc PR B 2 C52 C 0.5084(8) 0.7023(8) 0.1330(3) 0.111(6) Uiso 0.60 1 d PDU B 2 C53 C 0.5326(13) 0.7463(11) 0.1529(4) 0.123(7) Uiso 0.60 1 d PDU B 2 H53 H 0.5223 0.7818 0.1545 0.148 Uiso 0.60 1 calc PR B 2 C54 C 0.5721(13) 0.7382(12) 0.1705(4) 0.112(7) Uiso 0.60 1 d PDU B 2 H54 H 0.5855 0.7649 0.1854 0.134 Uiso 0.60 1 calc PR B 2 C55 C 0.5923(14) 0.6912(13) 0.1665(4) 0.095(6) Uiso 0.60 1 d PDU B 2 H55 H 0.6190 0.6849 0.1788 0.114 Uiso 0.60 1 calc PR B 2 C56 C 0.5744(11) 0.6532(11) 0.1449(4) 0.083(5) Uiso 0.60 1 d PDU B 2 H56 H 0.5876 0.6199 0.1424 0.099 Uiso 0.60 1 calc PR B 2 C57 C 0.5371(11) 0.6636(11) 0.1268(3) 0.079(5) Uiso 0.60 1 d PDU B 2 H57 H 0.5314 0.6445 0.1104 0.095 Uiso 0.60 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0210(2) 0.0255(2) 0.0280(3) -0.00322(18) 0.00030(18) 0.01157(19) F1 0.024(2) 0.028(2) 0.029(2) -0.0042(19) 0.0012(19) 0.0060(19) N1 0.020(3) 0.029(4) 0.034(4) -0.003(3) -0.001(3) 0.009(3) C1 0.022(4) 0.032(5) 0.044(5) -0.005(4) -0.005(4) 0.007(4) La2 0.0300(3) 0.0288(3) 0.0401(3) 0.0024(2) 0.0035(2) 0.0162(2) F2 0.030(3) 0.038(3) 0.038(3) 0.002(2) 0.006(2) 0.016(2) N2 0.028(4) 0.030(4) 0.031(4) 0.002(3) 0.003(3) 0.011(3) C2 0.027(4) 0.036(5) 0.039(5) 0.004(4) 0.009(4) 0.013(4) F3 0.043(3) 0.045(3) 0.052(3) -0.021(3) -0.007(3) 0.013(3) N3 0.031(4) 0.035(4) 0.036(4) -0.001(3) 0.002(3) 0.021(3) C3 0.023(4) 0.029(4) 0.024(4) -0.001(3) -0.005(3) 0.013(3) F4 0.027(3) 0.048(3) 0.049(3) -0.013(3) 0.000(2) 0.006(2) N4 0.032(4) 0.028(4) 0.036(4) 0.000(3) -0.002(3) 0.018(3) C4 0.022(4) 0.036(5) 0.040(5) -0.005(4) -0.003(4) 0.013(4) F5 0.039(3) 0.046(3) 0.034(3) -0.010(2) -0.006(2) 0.027(2) N5 0.044(4) 0.031(4) 0.045(4) 0.001(3) 0.007(4) 0.020(4) C5 0.033(5) 0.028(4) 0.040(5) -0.012(4) -0.011(4) 0.012(4) F6 0.056(4) 0.063(4) 0.039(3) -0.005(3) -0.013(3) 0.026(3) N6 0.038(4) 0.037(4) 0.049(5) 0.000(4) 0.004(4) 0.021(4) C6 0.043(5) 0.034(5) 0.032(5) -0.007(4) -0.005(4) 0.021(4) F7 0.115(6) 0.069(4) 0.049(4) -0.017(3) 0.012(4) 0.062(4) N7 0.033(4) 0.041(4) 0.037(4) 0.003(3) 0.001(3) 0.020(3) C7 0.028(4) 0.030(4) 0.025(4) 0.006(3) 0.009(3) 0.016(4) F8 0.071(4) 0.069(4) 0.056(4) -0.007(3) 0.014(3) 0.052(4) N8 0.042(4) 0.035(4) 0.041(4) 0.002(3) 0.001(3) 0.023(4) C8 0.028(4) 0.026(4) 0.032(4) -0.002(3) -0.002(3) 0.013(4) F9 0.028(2) 0.034(3) 0.040(3) 0.004(2) 0.006(2) 0.018(2) C9 0.042(5) 0.038(5) 0.046(5) 0.001(4) 0.007(4) 0.021(4) F10 0.051(3) 0.038(3) 0.042(3) 0.002(2) 0.004(2) 0.023(3) C10 0.046(6) 0.048(6) 0.035(5) 0.004(4) 0.009(4) 0.017(5) F11 0.058(4) 0.060(4) 0.052(3) -0.009(3) 0.001(3) 0.031(3) C11 0.031(5) 0.041(5) 0.047(5) -0.004(4) 0.001(4) 0.022(4) F12 0.135(7) 0.069(5) 0.080(5) 0.033(4) 0.053(5) 0.042(5) C12 0.032(5) 0.043(5) 0.040(5) -0.001(4) 0.000(4) 0.025(4) F13 0.114(6) 0.045(4) 0.068(4) 0.018(3) 0.024(4) 0.040(4) C13 0.036(5) 0.029(4) 0.031(4) -0.005(3) 0.007(4) 0.015(4) F14 0.034(3) 0.050(3) 0.046(3) 0.007(2) 0.005(2) 0.025(3) C14 0.040(5) 0.033(5) 0.030(4) -0.003(4) 0.004(4) 0.018(4) F15 0.050(3) 0.063(4) 0.055(3) 0.019(3) 0.006(3) 0.036(3) C15 0.051(6) 0.037(5) 0.037(5) 0.001(4) -0.001(4) 0.017(5) F16 0.072(4) 0.098(5) 0.055(4) 0.024(4) 0.026(3) 0.062(4) C16 0.076(8) 0.036(5) 0.035(5) -0.010(4) 0.004(5) 0.024(5) F17 0.059(4) 0.081(4) 0.057(4) 0.013(3) 0.015(3) 0.054(4) C17 0.074(8) 0.044(6) 0.049(6) -0.008(5) 0.012(5) 0.034(6) F18 0.038(3) 0.032(3) 0.053(3) 0.001(2) 0.002(2) 0.018(2) C18 0.060(6) 0.043(5) 0.035(5) -0.003(4) 0.005(4) 0.031(5) C19 0.037(5) 0.030(5) 0.049(5) -0.003(4) 0.000(4) 0.018(4) C20 0.038(5) 0.038(5) 0.040(5) 0.001(4) 0.001(4) 0.022(4) C21 0.046(6) 0.038(5) 0.055(6) 0.009(4) 0.008(5) 0.022(5) C22 0.039(5) 0.036(5) 0.050(6) -0.003(4) 0.005(4) 0.020(4) C23 0.040(5) 0.035(5) 0.041(5) 0.009(4) 0.004(4) 0.017(4) C24 0.036(5) 0.044(5) 0.043(5) 0.006(4) -0.002(4) 0.020(4) C25 0.044(5) 0.049(6) 0.042(5) -0.013(4) -0.002(4) 0.025(5) C26 0.068(8) 0.074(8) 0.040(6) 0.013(6) 0.016(5) 0.032(7) C27 0.082(9) 0.053(7) 0.064(8) 0.026(6) 0.026(7) 0.027(7) C28 0.063(7) 0.040(6) 0.049(6) 0.011(5) 0.010(5) 0.024(5) C29 0.038(5) 0.047(6) 0.061(7) -0.001(5) 0.003(5) 0.019(5) C30 0.057(6) 0.039(5) 0.053(6) -0.006(5) -0.006(5) 0.025(5) C31 0.044(5) 0.042(5) 0.046(5) 0.002(4) 0.001(4) 0.027(5) C32 0.041(5) 0.043(5) 0.049(6) 0.007(4) 0.002(4) 0.030(5) C33 0.030(5) 0.037(5) 0.045(5) -0.005(4) -0.003(4) 0.018(4) C34 0.034(5) 0.037(5) 0.041(5) -0.004(4) -0.001(4) 0.019(4) C35 0.038(5) 0.046(5) 0.044(5) 0.000(4) -0.001(4) 0.024(5) C36 0.045(6) 0.055(6) 0.046(6) 0.009(5) 0.003(5) 0.027(5) C37 0.041(6) 0.059(7) 0.061(7) 0.003(5) 0.014(5) 0.030(5) C38 0.037(5) 0.048(6) 0.048(6) 0.004(4) 0.004(4) 0.028(5) C39 0.050(6) 0.058(6) 0.041(5) 0.005(5) -0.003(4) 0.033(5) C40 0.039(5) 0.034(5) 0.065(7) -0.003(5) -0.005(5) 0.015(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 La1 F9 2.339(4) . ? La1 F9 2.345(4) 3_675 ? La1 N3 2.492(7) . ? La1 N1 2.510(6) . ? La1 F1 2.628(4) . ? La1 F5 2.642(5) . ? La1 N2 2.701(7) . ? La1 N4 2.710(6) . ? F1 C8 1.384(9) . ? N1 C3 1.344(10) . ? N1 C1 1.468(10) . ? C1 C2 1.512(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? La2 F18 2.339(5) . ? La2 F18 2.340(5) 3_665 ? La2 N7 2.485(7) . ? La2 N5 2.499(7) . ? La2 F10 2.650(5) . ? La2 F14 2.655(5) . ? La2 N6 2.714(8) . ? La2 N8 2.721(7) . ? F2 C7 1.337(9) . ? N2 C10 1.474(11) . ? N2 C9 1.476(11) . ? N2 C2 1.476(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? F3 C5 1.354(9) . ? N3 C13 1.357(11) . ? N3 C11 1.479(11) . ? C3 C8 1.408(11) . ? C3 C4 1.412(11) . ? F4 C4 1.352(9) . ? N4 C20 1.457(11) . ? N4 C12 1.479(10) . ? N4 C19 1.479(10) . ? C4 C5 1.386(12) . ? F5 C14 1.383(9) . ? N5 C23 1.348(11) . ? N5 C21 1.462(12) . ? C5 C6 1.356(12) . ? F6 C15 1.333(11) . ? N6 C29 1.463(12) . ? N6 C22 1.469(12) . ? N6 C30 1.479(12) . ? C6 C7 1.374(12) . ? C6 H6 0.9500 . ? F7 C17 1.364(11) . ? N7 C33 1.362(11) . ? N7 C31 1.477(11) . ? C7 C8 1.366(11) . ? F8 C18 1.349(11) . ? N8 C32 1.462(11) . ? N8 C39 1.473(12) . ? N8 C40 1.473(11) . ? F9 La1 2.345(4) 2_765 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? F10 C24 1.371(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? F11 C25 1.337(11) . ? C11 C12 1.512(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C27 1.341(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? F13 C28 1.354(12) . ? C13 C14 1.393(12) . ? C13 C18 1.415(12) . ? F14 C34 1.363(10) . ? C14 C15 1.376(12) . ? F15 C35 1.346(10) . ? C15 C16 1.371(14) . ? F16 C37 1.371(11) . ? C16 C17 1.372(16) . ? C16 H16 0.9500 . ? F17 C38 1.357(10) . ? C17 C18 1.356(14) . ? F18 La2 2.340(5) 2_655 ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.517(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.417(13) . ? C23 C28 1.422(13) . ? C24 C25 1.376(13) . ? C25 C26 1.370(15) . ? C26 C27 1.375(17) . ? C26 H26 0.9500 . ? C27 C28 1.376(16) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.528(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.409(12) . ? C33 C34 1.417(12) . ? C34 C35 1.366(13) . ? C35 C36 1.376(13) . ? C36 C37 1.377(14) . ? C36 H36 0.9500 . ? C37 C38 1.350(14) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.442(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C47 1.353(9) . ? C42 C43 1.355(8) . ? C43 C44 1.390(8) . ? C43 H43 0.9500 . ? C44 C45 1.369(9) . ? C44 H44 0.9500 . ? C45 C46 1.377(9) . ? C45 H45 0.9500 . ? C46 C47 1.386(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C51 C52 1.383(10) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.368(9) . ? C52 C57 1.370(8) . ? C53 C54 1.368(9) . ? C53 H53 0.9500 . ? C54 C55 1.372(9) . ? C54 H54 0.9500 . ? C55 C56 1.368(9) . ? C55 H55 0.9500 . ? C56 C57 1.380(9) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F9 La1 F9 82.3(2) . 3_675 ? F9 La1 N3 146.6(2) . . ? F9 La1 N3 91.8(2) 3_675 . ? F9 La1 N1 91.30(19) . . ? F9 La1 N1 145.63(19) 3_675 . ? N3 La1 N1 110.6(2) . . ? F9 La1 F1 68.10(15) . . ? F9 La1 F1 83.77(14) 3_675 . ? N3 La1 F1 144.14(19) . . ? N1 La1 F1 62.69(17) . . ? F9 La1 F5 84.91(15) . . ? F9 La1 F5 68.07(16) 3_675 . ? N3 La1 F5 62.64(19) . . ? N1 La1 F5 145.23(19) . . ? F1 La1 F5 143.47(14) . . ? F9 La1 N2 85.19(18) . . ? F9 La1 N2 145.66(18) 3_675 . ? N3 La1 N2 81.4(2) . . ? N1 La1 N2 66.2(2) . . ? F1 La1 N2 120.54(17) . . ? F5 La1 N2 79.08(18) . . ? F9 La1 N4 144.67(18) . . ? F9 La1 N4 85.18(18) 3_675 . ? N3 La1 N4 66.3(2) . . ? N1 La1 N4 80.8(2) . . ? F1 La1 N4 77.81(18) . . ? F5 La1 N4 120.37(18) . . ? N2 La1 N4 121.4(2) . . ? C8 F1 La1 118.3(4) . . ? C3 N1 C1 118.7(7) . . ? C3 N1 La1 122.8(5) . . ? C1 N1 La1 116.9(5) . . ? N1 C1 C2 111.4(7) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? F18 La2 F18 82.2(2) . 3_665 ? F18 La2 N7 91.5(2) . . ? F18 La2 N7 146.0(2) 3_665 . ? F18 La2 N5 146.3(2) . . ? F18 La2 N5 92.0(2) 3_665 . ? N7 La2 N5 110.3(2) . . ? F18 La2 F10 84.48(17) . . ? F18 La2 F10 68.24(17) 3_665 . ? N7 La2 F10 144.6(2) . . ? N5 La2 F10 62.8(2) . . ? F18 La2 F14 68.49(17) . . ? F18 La2 F14 84.15(17) 3_665 . ? N7 La2 F14 62.66(19) . . ? N5 La2 F14 144.2(2) . . ? F10 La2 F14 143.84(16) . . ? F18 La2 N6 145.0(2) . . ? F18 La2 N6 84.6(2) 3_665 . ? N7 La2 N6 81.8(2) . . ? N5 La2 N6 66.2(2) . . ? F10 La2 N6 120.0(2) . . ? F14 La2 N6 78.0(2) . . ? F18 La2 N8 85.4(2) . . ? F18 La2 N8 145.4(2) 3_665 . ? N7 La2 N8 66.0(2) . . ? N5 La2 N8 80.8(2) . . ? F10 La2 N8 78.57(19) . . ? F14 La2 N8 120.67(19) . . ? N6 La2 N8 121.7(2) . . ? C10 N2 C9 107.2(7) . . ? C10 N2 C2 109.1(7) . . ? C9 N2 C2 111.3(7) . . ? C10 N2 La1 115.7(5) . . ? C9 N2 La1 114.7(5) . . ? C2 N2 La1 98.5(5) . . ? N2 C2 C1 113.3(7) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C13 N3 C11 118.7(7) . . ? C13 N3 La1 123.5(5) . . ? C11 N3 La1 117.2(5) . . ? N1 C3 C8 119.1(7) . . ? N1 C3 C4 129.7(7) . . ? C8 C3 C4 111.2(7) . . ? C20 N4 C12 108.1(7) . . ? C20 N4 C19 109.0(7) . . ? C12 N4 C19 111.1(7) . . ? C20 N4 La1 116.6(5) . . ? C12 N4 La1 97.8(5) . . ? C19 N4 La1 113.6(5) . . ? F4 C4 C5 117.1(7) . . ? F4 C4 C3 120.4(7) . . ? C5 C4 C3 122.4(8) . . ? C14 F5 La1 118.1(4) . . ? C23 N5 C21 117.5(7) . . ? C23 N5 La2 123.1(6) . . ? C21 N5 La2 117.8(6) . . ? F3 C5 C6 119.6(8) . . ? F3 C5 C4 116.9(8) . . ? C6 C5 C4 123.4(8) . . ? C29 N6 C22 111.7(8) . . ? C29 N6 C30 108.6(8) . . ? C22 N6 C30 108.7(7) . . ? C29 N6 La2 114.8(6) . . ? C22 N6 La2 97.0(5) . . ? C30 N6 La2 115.5(6) . . ? C5 C6 C7 116.1(8) . . ? C5 C6 H6 121.9 . . ? C7 C6 H6 121.9 . . ? C33 N7 C31 116.5(7) . . ? C33 N7 La2 123.8(6) . . ? C31 N7 La2 118.6(5) . . ? F2 C7 C8 118.9(7) . . ? F2 C7 C6 120.4(7) . . ? C8 C7 C6 120.7(8) . . ? C32 N8 C39 108.4(7) . . ? C32 N8 C40 111.4(7) . . ? C39 N8 C40 109.2(8) . . ? C32 N8 La2 97.7(5) . . ? C39 N8 La2 115.8(6) . . ? C40 N8 La2 113.8(5) . . ? C7 C8 F1 117.9(7) . . ? C7 C8 C3 125.7(7) . . ? F1 C8 C3 116.2(7) . . ? La1 F9 La1 157.7(2) . 2_765 ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C24 F10 La2 118.1(5) . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 110.9(7) . . ? N3 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N4 C12 C11 113.8(7) . . ? N4 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? N4 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? N3 C13 C14 118.9(7) . . ? N3 C13 C18 129.2(8) . . ? C14 C13 C18 111.9(8) . . ? C34 F14 La2 118.1(5) . . ? C15 C14 F5 117.0(8) . . ? C15 C14 C13 126.3(8) . . ? F5 C14 C13 116.7(7) . . ? F6 C15 C16 121.5(9) . . ? F6 C15 C14 118.9(9) . . ? C16 C15 C14 119.6(10) . . ? C15 C16 C17 115.7(9) . . ? C15 C16 H16 122.1 . . ? C17 C16 H16 122.1 . . ? C18 C17 F7 116.7(10) . . ? C18 C17 C16 124.8(9) . . ? F7 C17 C16 118.5(9) . . ? La2 F18 La2 157.8(2) . 2_655 ? F8 C18 C17 117.9(8) . . ? F8 C18 C13 120.6(8) . . ? C17 C18 C13 121.5(9) . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C22 109.8(7) . . ? N5 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? N5 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? N6 C22 C21 114.2(7) . . ? N6 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? N6 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N5 C23 C24 119.1(8) . . ? N5 C23 C28 129.7(9) . . ? C24 C23 C28 111.2(8) . . ? F10 C24 C25 118.4(9) . . ? F10 C24 C23 116.5(8) . . ? C25 C24 C23 125.1(9) . . ? F11 C25 C26 120.6(9) . . ? F11 C25 C24 118.1(9) . . ? C26 C25 C24 121.3(10) . . ? C25 C26 C27 116.0(10) . . ? C25 C26 H26 122.0 . . ? C27 C26 H26 122.0 . . ? F12 C27 C26 119.3(11) . . ? F12 C27 C28 117.4(11) . . ? C26 C27 C28 123.3(10) . . ? F13 C28 C27 117.7(9) . . ? F13 C28 C23 119.5(9) . . ? C27 C28 C23 122.8(10) . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N6 C30 H30A 109.5 . . ? N6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N7 C31 C32 109.2(7) . . ? N7 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? N7 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? N8 C32 C31 113.9(7) . . ? N8 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? N8 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? N7 C33 C38 130.4(8) . . ? N7 C33 C34 118.1(8) . . ? C38 C33 C34 111.5(8) . . ? F14 C34 C35 118.2(8) . . ? F14 C34 C33 116.9(8) . . ? C35 C34 C33 124.8(8) . . ? F15 C35 C34 119.0(8) . . ? F15 C35 C36 119.6(8) . . ? C34 C35 C36 121.4(9) . . ? C35 C36 C37 114.8(9) . . ? C35 C36 H36 122.6 . . ? C37 C36 H36 122.6 . . ? C38 C37 F16 118.1(9) . . ? C38 C37 C36 124.5(9) . . ? F16 C37 C36 117.4(9) . . ? C37 C38 F17 117.4(8) . . ? C37 C38 C33 122.8(9) . . ? F17 C38 C33 119.8(8) . . ? N8 C39 H39A 109.5 . . ? N8 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N8 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N8 C40 H40A 109.5 . . ? N8 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N8 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C47 C42 C43 122.2(7) . . ? C47 C42 C41 119.0(8) . . ? C43 C42 C41 118.6(8) . . ? C42 C43 C44 118.9(7) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.5 . . ? C45 C44 C43 118.9(7) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C44 C45 C46 120.3(8) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.8 . . ? C45 C46 C47 118.2(9) . . ? C45 C46 H46 120.9 . . ? C47 C46 H46 120.9 . . ? C42 C47 C46 118.4(9) . . ? C42 C47 H47 120.8 . . ? C46 C47 H47 120.8 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C57 120.5(8) . . ? C53 C52 C51 119.1(8) . . ? C57 C52 C51 119.7(8) . . ? C52 C53 C54 118.8(8) . . ? C52 C53 H53 120.6 . . ? C54 C53 H53 120.6 . . ? C53 C54 C55 119.6(7) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C56 C55 C54 120.8(7) . . ? C56 C55 H55 119.6 . . ? C54 C55 H55 119.6 . . ? C55 C56 C57 119.4(8) . . ? C55 C56 H56 120.3 . . ? C57 C56 H56 120.3 . . ? C52 C57 C56 118.1(8) . . ? C52 C57 H57 121.0 . . ? C56 C57 H57 121.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.327 _refine_diff_density_min -1.473 _refine_diff_density_rms 0.159 # Attachment '3 [Ce(p-HC6F4NC2H4NEt2)3].0.5PhMe.CIF' data_[Ce(p-HC6F4NC2H4NEt2)3].PhMe.CIF _database_code_depnum_ccdc_archive 'CCDC 859381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(N,N-diethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine-F,N,N'/F,N) -cerium(iii) toluene solvate ; _chemical_name_common ? _chemical_melting_point '190-194 \%C' _chemical_formula_moiety 'C36 H45 Ce F12 N6, 1/2(C7 H8)' _chemical_formula_sum 'C39.50 H49 Ce F12 N6' _chemical_formula_weight 975.97 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.233(2) _cell_length_b 11.421(2) _cell_length_c 18.757(4) _cell_angle_alpha 81.03(3) _cell_angle_beta 78.85(3) _cell_angle_gamma 85.71(3) _cell_volume 2122.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 31041 _cell_measurement_theta_min 1.118 _cell_measurement_theta_max 30.530 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8182 _exptl_absorpt_correction_T_max 0.9231 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23644 _diffrn_reflns_av_R_equivalents 0.2295 _diffrn_reflns_av_sigmaI/netI 0.2869 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7417 _reflns_number_gt 3387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; A toluene solvate molecule was refined with two half occupancies on two sites by symmetry. 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. The collected data was from a relatively single fragment of a larger twinned crystal. The poorly diffracting specimen gave observable (I>2\sI) data only to a resolution 1.02 \%A. presumably leading to the high R(int) value. The lattice toluene molecule was modelled as disordered over a symmetry site and was refined at fixed occupancy of 0.5 with the geometry restrained to typical values (C-C 1.39 \%A; C-C-C 120 \%; Ar-C(Me) 1.50 \%A). The anisotropic thermal parameters were also restrained to approximate isotrpic behaviour. ; _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^)+(0.0584P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7417 _refine_ls_number_parameters 566 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.2151 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.1922 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.57046(6) 0.78492(6) 0.74509(4) 0.0294(2) Uani 1 1 d . . . F1 F 0.4694(5) 0.5833(5) 0.8226(3) 0.0358(17) Uani 1 1 d . . . N1 N 0.3620(7) 0.7225(8) 0.7197(5) 0.029(2) Uani 1 1 d . . . C1 C 0.3046(9) 0.6183(8) 0.7499(6) 0.022(3) Uani 1 1 d . . . F2 F 0.3880(6) 0.3655(5) 0.8834(4) 0.0520(19) Uani 1 1 d . . . N2 N 0.3805(8) 0.9632(7) 0.7301(5) 0.035(2) Uani 1 1 d . . . C2 C 0.3630(10) 0.5386(9) 0.8006(6) 0.026(3) Uani 1 1 d . . . F3 F 0.0540(6) 0.4108(6) 0.7374(5) 0.071(2) Uani 1 1 d . . . N3 N 0.6921(8) 0.8754(7) 0.6258(5) 0.033(2) Uani 1 1 d . . . C3 C 0.3227(12) 0.4284(9) 0.8316(7) 0.041(3) Uani 1 1 d . . . F4 F 0.1376(6) 0.6208(5) 0.6740(4) 0.051(2) Uani 1 1 d . . . N4 N 0.6994(7) 0.6280(7) 0.6600(5) 0.026(2) Uani 1 1 d . . . C4 C 0.2175(11) 0.3819(10) 0.8135(7) 0.044(4) Uani 1 1 d . . . H4 H 0.1881 0.3052 0.8350 0.053 Uiso 1 1 calc R . . F5 F 0.7338(6) 0.9710(5) 0.7396(4) 0.0382(16) Uani 1 1 d . . . N5 N 0.5853(8) 0.7967(7) 0.8679(5) 0.034(2) Uani 1 1 d . . . C5 C 0.1565(11) 0.4517(11) 0.7628(8) 0.050(4) Uani 1 1 d . . . F6 F 0.8689(6) 1.1680(5) 0.7270(5) 0.058(2) Uani 1 1 d . . . N6 N 0.2813(9) 0.7178(8) 1.0167(6) 0.048(3) Uani 1 1 d . . . C6 C 0.2012(10) 0.5634(10) 0.7279(7) 0.038(3) Uani 1 1 d . . . F7 F 0.9378(7) 1.1974(7) 0.4696(4) 0.076(3) Uani 1 1 d . . . C7 C 0.2888(10) 0.8082(9) 0.6763(7) 0.037(3) Uani 1 1 d . . . H7A H 0.1948 0.8148 0.7015 0.045 Uiso 1 1 calc R . . H7B H 0.2903 0.7823 0.6281 0.045 Uiso 1 1 calc R . . F8 F 0.8012(7) 1.0087(6) 0.4801(4) 0.067(2) Uani 1 1 d . . . C8 C 0.3498(11) 0.9261(10) 0.6649(6) 0.041(3) Uani 1 1 d . . . H8A H 0.4331 0.9239 0.6281 0.049 Uiso 1 1 calc R . . H8B H 0.2880 0.9870 0.6441 0.049 Uiso 1 1 calc R . . F9 F 0.8116(5) 0.7287(5) 0.7907(3) 0.0345(16) Uani 1 1 d . . . C9 C 0.2588(9) 0.9609(10) 0.7900(7) 0.041(3) Uani 1 1 d . . . H9A H 0.2831 0.9865 0.8336 0.049 Uiso 1 1 calc R . . H9B H 0.2304 0.8782 0.8041 0.049 Uiso 1 1 calc R . . F10 F 1.0483(5) 0.7252(6) 0.8332(4) 0.0490(19) Uani 1 1 d . . . C10 C 0.1409(10) 1.0398(11) 0.7688(8) 0.061(4) Uani 1 1 d . . . H10A H 0.1657 1.1228 0.7581 0.091 Uiso 1 1 calc R . . H10B H 0.0646 1.0311 0.8096 0.091 Uiso 1 1 calc R . . H10C H 0.1166 1.0162 0.7252 0.091 Uiso 1 1 calc R . . F11 F 0.8361(6) 0.8740(6) 1.0491(4) 0.0527(19) Uani 1 1 d . . . C11 C 0.4375(11) 1.0819(9) 0.7131(8) 0.054(4) Uani 1 1 d . . . H11A H 0.3732 1.1401 0.6923 0.065 Uiso 1 1 calc R . . H11B H 0.5200 1.0795 0.6756 0.065 Uiso 1 1 calc R . . F12 F 0.6045(6) 0.8841(6) 1.0079(4) 0.0483(18) Uani 1 1 d . . . C12 C 0.4699(12) 1.1227(11) 0.7825(9) 0.078(5) Uani 1 1 d . . . H12A H 0.3868 1.1429 0.8148 0.117 Uiso 1 1 calc R . . H12B H 0.5243 1.1926 0.7680 0.117 Uiso 1 1 calc R . . H12C H 0.5193 1.0585 0.8085 0.117 Uiso 1 1 calc R . . C13 C 0.7618(11) 0.9754(10) 0.6114(7) 0.036(3) Uani 1 1 d . . . C14 C 0.7850(10) 1.0260(9) 0.6700(8) 0.033(3) Uani 1 1 d . . . C15 C 0.8526(11) 1.1257(11) 0.6661(8) 0.041(3) Uani 1 1 d . . . C16 C 0.9099(11) 1.1857(11) 0.5990(8) 0.046(4) Uani 1 1 d . . . H16 H 0.9605 1.2534 0.5956 0.055 Uiso 1 1 calc R . . C17 C 0.8911(11) 1.1436(11) 0.5379(9) 0.054(4) Uani 1 1 d . . . C18 C 0.8209(11) 1.0417(11) 0.5439(7) 0.044(3) Uani 1 1 d . . . C19 C 0.6958(10) 0.8074(10) 0.5646(6) 0.037(3) Uani 1 1 d . . . H19A H 0.7881 0.8022 0.5366 0.045 Uiso 1 1 calc R . . H19B H 0.6382 0.8489 0.5309 0.045 Uiso 1 1 calc R . . C20 C 0.6479(10) 0.6837(9) 0.5937(6) 0.035(3) Uani 1 1 d . . . H20A H 0.5493 0.6876 0.6053 0.042 Uiso 1 1 calc R . . H20B H 0.6758 0.6329 0.5547 0.042 Uiso 1 1 calc R . . C21 C 0.6512(10) 0.5062(9) 0.6768(7) 0.039(3) Uani 1 1 d . . . H21A H 0.6834 0.4643 0.6339 0.047 Uiso 1 1 calc R . . H21B H 0.5525 0.5101 0.6857 0.047 Uiso 1 1 calc R . . C22 C 0.6997(11) 0.4345(9) 0.7454(7) 0.056(4) Uani 1 1 d . . . H22A H 0.7880 0.3970 0.7302 0.083 Uiso 1 1 calc R . . H22B H 0.6366 0.3732 0.7685 0.083 Uiso 1 1 calc R . . H22C H 0.7052 0.4882 0.7806 0.083 Uiso 1 1 calc R . . C23 C 0.8505(9) 0.6255(9) 0.6434(6) 0.030(3) Uani 1 1 d . . . H23A H 0.8786 0.7083 0.6300 0.036 Uiso 1 1 calc R . . H23B H 0.8831 0.5921 0.6891 0.036 Uiso 1 1 calc R . . C24 C 0.9184(10) 0.5568(10) 0.5839(6) 0.042(3) Uani 1 1 d . . . H24A H 0.8993 0.4727 0.5984 0.063 Uiso 1 1 calc R . . H24B H 1.0149 0.5657 0.5759 0.063 Uiso 1 1 calc R . . H24C H 0.8855 0.5869 0.5384 0.063 Uiso 1 1 calc R . . C25 C 0.6975(10) 0.8024(9) 0.8976(7) 0.032(3) Uani 1 1 d . . . C26 C 0.8180(11) 0.7672(9) 0.8553(7) 0.036(3) Uani 1 1 d . . . C27 C 0.9398(11) 0.7654(10) 0.8768(7) 0.036(3) Uani 1 1 d . . . C28 C 0.9497(10) 0.7997(10) 0.9424(6) 0.037(3) Uani 1 1 d . . . H28 H 1.0333 0.7986 0.9575 0.044 Uiso 1 1 calc R . . C29 C 0.8325(12) 0.8362(10) 0.9857(7) 0.041(3) Uani 1 1 d . . . C30 C 0.7107(11) 0.8385(9) 0.9623(7) 0.034(3) Uani 1 1 d . . . C31 C 0.4511(10) 0.8070(9) 0.9143(6) 0.034(3) Uani 1 1 d . . . H31A H 0.3835 0.8132 0.8824 0.040 Uiso 1 1 calc R . . H31B H 0.4440 0.8817 0.9357 0.040 Uiso 1 1 calc R . . C32 C 0.4179(11) 0.7057(10) 0.9759(6) 0.038(3) Uani 1 1 d . . . H32A H 0.4293 0.6301 0.9553 0.046 Uiso 1 1 calc R . . H32B H 0.4811 0.7024 1.0101 0.046 Uiso 1 1 calc R . . C33 C 0.2309(13) 0.6063(12) 1.0560(8) 0.067(4) Uani 1 1 d . . . H33A H 0.1522 0.6221 1.0938 0.081 Uiso 1 1 calc R . . H33B H 0.3001 0.5629 1.0815 0.081 Uiso 1 1 calc R . . C34 C 0.1926(13) 0.5307(11) 1.0061(8) 0.074(5) Uani 1 1 d . . . H34A H 0.1405 0.5791 0.9727 0.112 Uiso 1 1 calc R . . H34B H 0.1389 0.4663 1.0353 0.112 Uiso 1 1 calc R . . H34C H 0.2732 0.4971 0.9776 0.112 Uiso 1 1 calc R . . C35 C 0.2860(12) 0.8008(12) 1.0726(8) 0.066(4) Uani 1 1 d . . . H35A H 0.3160 0.7551 1.1163 0.079 Uiso 1 1 calc R . . H35B H 0.3509 0.8625 1.0508 0.079 Uiso 1 1 calc R . . C36 C 0.1565(14) 0.8563(12) 1.0942(9) 0.085(5) Uani 1 1 d . . . H36A H 0.1244 0.8972 1.0505 0.128 Uiso 1 1 calc R . . H36B H 0.1627 0.9139 1.1269 0.128 Uiso 1 1 calc R . . H36C H 0.0943 0.7957 1.1199 0.128 Uiso 1 1 calc R . . C37 C 0.445(3) 0.682(2) 0.4471(18) 0.09(2) Uani 0.50 1 d PDU A -1 H37A H 0.3566 0.6837 0.4334 0.140 Uiso 0.50 1 calc PR A -1 H37B H 0.5122 0.7010 0.4029 0.140 Uiso 0.50 1 calc PR A -1 H37C H 0.4442 0.7398 0.4804 0.140 Uiso 0.50 1 calc PR A -1 C38 C 0.475(2) 0.5631(17) 0.4838(13) 0.050(7) Uani 0.50 1 d PDU A -1 C39 C 0.391(3) 0.511(2) 0.5449(16) 0.058(17) Uani 0.50 1 d PDU A -1 H39 H 0.3109 0.5518 0.5646 0.069 Uiso 0.50 1 calc PR A -1 C40 C 0.426(2) 0.398(2) 0.5774(13) 0.062(8) Uani 0.50 1 d PDU A -1 H40 H 0.3678 0.3613 0.6193 0.074 Uiso 0.50 1 calc PR A -1 C41 C 0.541(3) 0.339(2) 0.5501(16) 0.076(18) Uani 0.50 1 d PDU A -1 H41 H 0.5653 0.2632 0.5737 0.091 Uiso 0.50 1 calc PR A -1 C42 C 0.622(2) 0.392(2) 0.4878(14) 0.063(9) Uani 0.50 1 d PD A -1 H42 H 0.7000 0.3494 0.4668 0.076 Uiso 0.50 1 calc PR A -1 C43 C 0.593(3) 0.507(2) 0.4549(16) 0.051(16) Uani 0.50 1 d PDU A -1 H43 H 0.6525 0.5447 0.4140 0.061 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0245(4) 0.0351(4) 0.0292(5) -0.0054(3) -0.0055(3) -0.0017(3) F1 0.038(4) 0.034(3) 0.042(5) -0.004(3) -0.023(4) -0.006(3) N1 0.021(5) 0.050(6) 0.016(6) 0.002(5) -0.008(4) 0.001(5) C1 0.004(5) 0.026(6) 0.030(7) 0.011(6) -0.003(5) 0.004(5) F2 0.055(4) 0.043(4) 0.057(5) 0.003(4) -0.018(4) 0.000(3) N2 0.028(5) 0.034(6) 0.040(7) -0.004(5) 0.001(5) -0.010(4) C2 0.026(6) 0.022(6) 0.032(8) -0.006(6) -0.007(6) 0.003(5) F3 0.045(4) 0.057(5) 0.121(8) -0.009(5) -0.037(5) -0.018(4) N3 0.034(5) 0.025(5) 0.045(7) -0.011(5) -0.010(5) -0.012(4) C3 0.055(8) 0.019(7) 0.049(9) 0.001(6) -0.018(8) -0.002(6) F4 0.043(4) 0.053(4) 0.067(5) -0.004(4) -0.035(4) -0.008(3) N4 0.022(5) 0.031(5) 0.027(6) 0.001(4) -0.009(5) -0.009(4) C4 0.035(7) 0.029(7) 0.073(11) -0.016(7) -0.021(8) 0.011(6) F5 0.049(4) 0.035(4) 0.030(4) -0.010(3) -0.001(4) -0.005(3) N5 0.015(5) 0.053(6) 0.035(7) -0.014(5) 0.001(5) -0.003(4) C5 0.019(7) 0.045(8) 0.089(12) -0.017(8) -0.007(8) -0.009(6) F6 0.058(5) 0.042(4) 0.081(6) -0.020(4) -0.018(5) 0.001(3) N6 0.043(7) 0.048(7) 0.048(8) -0.004(6) 0.011(6) -0.020(5) C6 0.019(6) 0.045(8) 0.053(9) -0.013(7) -0.009(6) -0.004(6) F7 0.061(5) 0.082(6) 0.065(6) 0.026(5) 0.014(5) -0.019(4) C7 0.031(7) 0.039(7) 0.043(9) -0.004(6) -0.014(7) 0.001(6) F8 0.079(5) 0.077(5) 0.039(5) 0.016(4) -0.010(5) -0.021(4) C8 0.034(7) 0.055(8) 0.037(9) -0.015(7) -0.014(7) 0.017(6) F9 0.042(4) 0.049(4) 0.016(4) -0.014(3) -0.005(3) -0.004(3) C9 0.024(6) 0.051(8) 0.050(9) -0.018(7) -0.004(7) 0.010(6) F10 0.021(3) 0.075(5) 0.052(5) -0.028(4) 0.004(4) 0.000(3) C10 0.028(7) 0.070(9) 0.081(12) -0.020(8) -0.002(8) 0.017(7) F11 0.044(4) 0.083(5) 0.036(5) -0.024(4) -0.007(4) -0.010(4) C11 0.043(8) 0.032(7) 0.090(12) 0.008(8) -0.027(8) -0.014(6) F12 0.030(4) 0.079(5) 0.039(5) -0.027(4) 0.002(4) -0.005(3) C12 0.057(9) 0.060(10) 0.129(16) -0.053(10) -0.013(10) -0.010(7) C13 0.044(7) 0.039(8) 0.027(8) -0.004(7) -0.014(7) -0.001(6) C14 0.011(6) 0.020(7) 0.062(11) 0.002(7) 0.003(6) 0.001(5) C15 0.031(7) 0.049(8) 0.043(10) -0.024(8) 0.004(7) 0.007(6) C16 0.034(8) 0.044(8) 0.055(11) -0.002(8) 0.000(8) -0.003(6) C17 0.022(7) 0.041(9) 0.080(13) 0.022(9) 0.008(8) 0.003(6) C18 0.033(7) 0.062(9) 0.033(9) 0.006(8) -0.013(7) 0.012(7) C19 0.030(7) 0.058(8) 0.025(8) -0.018(7) 0.000(6) 0.001(6) C20 0.030(7) 0.049(8) 0.030(8) -0.010(6) -0.010(6) -0.006(6) C21 0.020(6) 0.035(7) 0.062(10) -0.016(7) -0.002(6) 0.003(5) C22 0.052(8) 0.026(7) 0.090(12) -0.012(7) -0.007(8) -0.012(6) C23 0.024(6) 0.036(7) 0.039(8) -0.020(6) -0.016(6) 0.002(5) C24 0.031(7) 0.062(8) 0.038(9) -0.025(7) -0.005(6) -0.005(6) C25 0.020(6) 0.048(7) 0.035(8) -0.024(6) -0.006(6) 0.001(5) C26 0.034(7) 0.030(7) 0.046(9) -0.012(6) -0.009(7) 0.000(5) C27 0.027(7) 0.054(8) 0.030(8) -0.010(6) -0.007(7) -0.001(6) C28 0.016(6) 0.067(8) 0.027(8) -0.016(7) 0.006(6) -0.001(6) C29 0.044(8) 0.054(8) 0.036(9) -0.022(7) -0.021(7) -0.010(6) C30 0.029(7) 0.046(7) 0.028(8) -0.014(6) 0.002(6) -0.013(6) C31 0.033(7) 0.043(7) 0.028(8) -0.005(6) -0.016(6) -0.001(6) C32 0.044(8) 0.050(8) 0.021(8) -0.002(6) -0.008(6) -0.008(6) C33 0.057(9) 0.065(10) 0.071(12) 0.001(9) 0.005(9) -0.016(8) C34 0.074(10) 0.056(9) 0.095(14) -0.011(9) -0.010(10) -0.020(8) C35 0.050(9) 0.091(11) 0.048(11) -0.013(9) 0.008(8) 0.009(8) C36 0.090(12) 0.084(11) 0.089(14) -0.040(10) -0.016(11) 0.011(9) C37 0.10(2) 0.09(2) 0.10(2) -0.021(10) -0.028(10) -0.006(9) C38 0.059(11) 0.053(10) 0.048(11) -0.024(9) -0.019(9) -0.009(8) C39 0.060(18) 0.063(19) 0.057(19) -0.018(9) -0.020(10) -0.002(9) C40 0.066(11) 0.068(11) 0.053(11) -0.015(9) -0.007(9) -0.010(9) C41 0.079(19) 0.078(19) 0.08(2) -0.015(9) -0.030(10) -0.010(9) C42 0.057(19) 0.10(3) 0.03(2) -0.024(18) 0.005(17) -0.035(18) C43 0.054(17) 0.053(17) 0.051(18) -0.018(9) -0.012(9) -0.005(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 N5 2.363(9) . ? Ce1 N1 2.452(8) . ? Ce1 N3 2.453(9) . ? Ce1 F1 2.686(5) . ? Ce1 N4 2.687(8) . ? Ce1 N2 2.728(8) . ? Ce1 F9 2.764(5) . ? Ce1 F5 2.779(6) . ? F1 C2 1.392(10) . ? N1 C1 1.359(11) . ? N1 C7 1.436(11) . ? C1 C2 1.399(12) . ? C1 C6 1.425(13) . ? F2 C3 1.366(12) . ? N2 C8 1.450(13) . ? N2 C11 1.481(12) . ? N2 C9 1.506(13) . ? C2 C3 1.359(13) . ? F3 C5 1.372(12) . ? N3 C13 1.356(13) . ? N3 C19 1.475(13) . ? C3 C4 1.356(13) . ? F4 C6 1.364(12) . ? N4 C21 1.478(12) . ? N4 C20 1.479(12) . ? N4 C23 1.516(11) . ? C4 C5 1.360(15) . ? F5 C14 1.379(13) . ? N5 C25 1.379(11) . ? N5 C31 1.485(13) . ? C5 C6 1.406(15) . ? F6 C15 1.349(13) . ? N6 C33 1.446(14) . ? N6 C32 1.466(13) . ? N6 C35 1.528(15) . ? F7 C17 1.344(15) . ? C7 C8 1.494(13) . ? F8 C18 1.364(13) . ? F9 C26 1.367(12) . ? C9 C10 1.528(13) . ? F10 C27 1.342(12) . ? F11 C29 1.335(12) . ? C11 C12 1.550(17) . ? F12 C30 1.371(12) . ? C13 C14 1.386(15) . ? C13 C18 1.421(16) . ? C14 C15 1.361(15) . ? C15 C16 1.380(16) . ? C16 C17 1.362(17) . ? C17 C18 1.391(16) . ? C19 C20 1.514(13) . ? C21 C22 1.558(15) . ? C23 C24 1.495(14) . ? C25 C30 1.375(14) . ? C25 C26 1.399(15) . ? C26 C27 1.380(13) . ? C27 C28 1.371(15) . ? C28 C29 1.388(15) . ? C29 C30 1.396(14) . ? C31 C32 1.510(14) . ? C33 C34 1.490(17) . ? C35 C36 1.438(16) . ? C37 C38 1.461(17) . ? C38 C39 1.374(17) . ? C38 C43 1.381(17) . ? C39 C40 1.389(17) . ? C40 C41 1.367(18) . ? C41 C42 1.378(18) . ? C42 C43 1.395(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 N5 Ce1 N1 118.6(3) . . ? N5 Ce1 N3 133.5(3) . . ? N1 Ce1 N3 105.2(3) . . ? N5 Ce1 F1 75.1(2) . . ? N1 Ce1 F1 62.1(2) . . ? N3 Ce1 F1 144.7(2) . . ? N5 Ce1 N4 127.4(3) . . ? N1 Ce1 N4 87.5(3) . . ? N3 Ce1 N4 65.7(3) . . ? F1 Ce1 N4 80.3(2) . . ? N5 Ce1 N2 97.3(3) . . ? N1 Ce1 N2 65.4(3) . . ? N3 Ce1 N2 86.8(3) . . ? F1 Ce1 N2 112.8(2) . . ? N4 Ce1 N2 135.2(3) . . ? N5 Ce1 F9 60.8(2) . . ? N1 Ce1 F9 150.0(2) . . ? N3 Ce1 F9 88.9(2) . . ? F1 Ce1 F9 91.06(16) . . ? N4 Ce1 F9 74.2(2) . . ? N2 Ce1 F9 143.1(2) . . ? N5 Ce1 F5 73.6(2) . . ? N1 Ce1 F5 147.1(2) . . ? N3 Ce1 F5 60.8(2) . . ? F1 Ce1 F5 146.38(17) . . ? N4 Ce1 F5 109.5(2) . . ? N2 Ce1 F5 83.4(2) . . ? F9 Ce1 F5 62.83(16) . . ? C2 F1 Ce1 117.7(5) . . ? C1 N1 C7 118.0(8) . . ? C1 N1 Ce1 124.7(6) . . ? C7 N1 Ce1 116.9(6) . . ? N1 C1 C2 120.2(8) . . ? N1 C1 C6 128.5(9) . . ? C2 C1 C6 110.2(9) . . ? C8 N2 C11 111.1(9) . . ? C8 N2 C9 110.7(8) . . ? C11 N2 C9 111.1(9) . . ? C8 N2 Ce1 93.1(6) . . ? C11 N2 Ce1 112.4(6) . . ? C9 N2 Ce1 117.1(6) . . ? C3 C2 F1 118.9(9) . . ? C3 C2 C1 127.0(10) . . ? F1 C2 C1 114.0(8) . . ? C13 N3 C19 117.4(10) . . ? C13 N3 Ce1 127.3(8) . . ? C19 N3 Ce1 115.1(6) . . ? C4 C3 C2 121.3(10) . . ? C4 C3 F2 119.9(10) . . ? C2 C3 F2 118.8(10) . . ? C21 N4 C20 105.9(8) . . ? C21 N4 C23 110.6(7) . . ? C20 N4 C23 109.2(8) . . ? C21 N4 Ce1 116.3(6) . . ? C20 N4 Ce1 94.6(6) . . ? C23 N4 Ce1 118.1(6) . . ? C3 C4 C5 116.0(11) . . ? C14 F5 Ce1 115.2(6) . . ? C25 N5 C31 119.8(9) . . ? C25 N5 Ce1 128.8(7) . . ? C31 N5 Ce1 111.3(6) . . ? C4 C5 F3 120.8(11) . . ? C4 C5 C6 123.2(10) . . ? F3 C5 C6 115.8(11) . . ? C33 N6 C32 112.9(10) . . ? C33 N6 C35 108.4(11) . . ? C32 N6 C35 106.2(9) . . ? F4 C6 C5 117.5(9) . . ? F4 C6 C1 120.6(9) . . ? C5 C6 C1 121.8(10) . . ? N1 C7 C8 109.7(8) . . ? N2 C8 C7 115.6(10) . . ? C26 F9 Ce1 113.7(6) . . ? N2 C9 C10 114.3(9) . . ? N2 C11 C12 111.5(11) . . ? N3 C13 C14 118.5(11) . . ? N3 C13 C18 131.1(12) . . ? C14 C13 C18 110.4(11) . . ? C15 C14 F5 116.2(12) . . ? C15 C14 C13 126.6(12) . . ? F5 C14 C13 117.2(9) . . ? F6 C15 C14 121.8(13) . . ? F6 C15 C16 117.6(12) . . ? C14 C15 C16 120.6(13) . . ? C17 C16 C15 117.2(12) . . ? F7 C17 C16 122.5(13) . . ? F7 C17 C18 116.9(15) . . ? C16 C17 C18 120.6(13) . . ? F8 C18 C17 116.9(13) . . ? F8 C18 C13 118.4(11) . . ? C17 C18 C13 124.5(13) . . ? N3 C19 C20 110.3(9) . . ? N4 C20 C19 113.6(8) . . ? N4 C21 C22 112.1(8) . . ? C24 C23 N4 116.7(8) . . ? C30 C25 N5 130.3(10) . . ? C30 C25 C26 114.1(10) . . ? N5 C25 C26 115.6(10) . . ? F9 C26 C27 119.3(11) . . ? F9 C26 C25 117.1(9) . . ? C27 C26 C25 123.6(12) . . ? F10 C27 C28 120.4(9) . . ? F10 C27 C26 118.5(11) . . ? C28 C27 C26 121.0(12) . . ? C27 C28 C29 117.2(10) . . ? F11 C29 C28 120.0(10) . . ? F11 C29 C30 119.3(11) . . ? C28 C29 C30 120.7(11) . . ? F12 C30 C25 122.0(9) . . ? F12 C30 C29 114.6(10) . . ? C25 C30 C29 123.4(11) . . ? N5 C31 C32 115.1(9) . . ? N6 C32 C31 112.3(9) . . ? N6 C33 C34 111.9(12) . . ? C36 C35 N6 110.5(11) . . ? C39 C38 C43 121.7(18) . . ? C39 C38 C37 121(2) . . ? C43 C38 C37 117(2) . . ? C38 C39 C40 119(2) . . ? C41 C40 C39 121(2) . . ? C40 C41 C42 119(2) . . ? C41 C42 C43 121(2) . . ? C38 C43 C42 117.9(19) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.094 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.169 # Attachment 'abs[Ce(p-HC6F4NC2H4NMe2)2F]3.CIF' data_[CeF(p-HC6F4NC2H4NMe2)2]3.1.5PhMe.CIF _database_code_depnum_ccdc_archive 'CCDC 859382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexa(N,N-dimethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine-F,N,N') -tris-fluoro-triscerium(iii) toluene solvate ; _chemical_name_common ; hexa(N,N-dimethyl-N'-(2,3,5,6- tetrafluorophenyl)ethylenediamine-F,N,N') -tris-fluoro-triscerium(iii) toluene solvate ; _chemical_melting_point '248 C (dec.)' _chemical_formula_moiety 'C60 H66 Ce3 F27 N12,1.5(C7 H8)' _chemical_formula_sum 'C70.50 H78 Ce3 F27 N12' _chemical_formula_weight 2026.81 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall -R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 22.712(3) _cell_length_b 22.712(3) _cell_length_c 53.514(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 23907(7) _cell_formula_units_Z 12 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 51415 _cell_measurement_theta_min 1.285 _cell_measurement_theta_max 27.856 _exptl_crystal_description rhombus _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12024 _exptl_absorpt_coefficient_mu 1.796 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6623 _exptl_absorpt_correction_T_max 0.8846 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42852 _diffrn_reflns_av_R_equivalents 0.1634 _diffrn_reflns_av_sigmaI/netI 0.1293 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 63 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9362 _reflns_number_gt 4638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. The lattice toluene molecule was modelled as disordered over two positions and refined with occupancies fixed at 0.5:0.5 and the geometry restrained to typical values (eg C-C 1.39 \%A; C-C-C 120 \%; Ar-C(Me) 1.50 \%A). The carbons atoms were refined with a single isotropic thermal parameter for each molecule. ; _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^)+(0.2000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9362 _refine_ls_number_parameters 666 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1573 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1894 _refine_ls_wR_factor_gt 0.1438 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.29753(3) 0.53688(3) 0.058556(10) 0.02306(19) Uani 1 1 d . . . F4 F 0.0910(3) 0.3528(3) 0.11701(11) 0.0498(17) Uani 1 1 d . . . N1 N 0.2035(4) 0.4481(4) 0.08400(13) 0.028(2) Uani 1 1 d . . . C1 C 0.1864(5) 0.4613(5) 0.10664(17) 0.025(2) Uani 1 1 d . . . C53 C 0.0177(17) 0.7419(18) -0.0326(6) 0.167(8) Uiso 0.50 1 d PD A 2 H53 H 0.0284 0.7130 -0.0420 0.200 Uiso 0.50 1 calc PR A 2 Ce2 Ce 0.57399(3) 0.37074(3) 0.163623(10) 0.0281(2) Uani 1 1 d . . . F3 F 0.0658(3) 0.3957(3) 0.15871(11) 0.0545(18) Uani 1 1 d . . . N2 N 0.1895(4) 0.4492(4) 0.03184(14) 0.032(2) Uani 1 1 d . . . C2 C 0.1319(5) 0.4193(5) 0.12273(18) 0.026(2) Uani 1 1 d . . . F2 F 0.2509(3) 0.6141(3) 0.14568(9) 0.0370(15) Uani 1 1 d . . . N3 N 0.3521(4) 0.4862(4) 0.03347(14) 0.030(2) Uani 1 1 d . . . C3 C 0.1187(5) 0.4419(6) 0.14473(18) 0.034(3) Uani 1 1 d . . . F1 F 0.2827(3) 0.5715(3) 0.10427(9) 0.0305(14) Uani 1 1 d . . . N4 N 0.3698(4) 0.4954(4) 0.08623(13) 0.026(2) Uani 1 1 d . . . C4 C 0.1570(5) 0.5075(5) 0.15363(17) 0.029(3) Uani 1 1 d . . . H4 H 0.1459 0.5226 0.1685 0.035 Uiso 1 1 calc R . . F5 F 0.3385(3) 0.5866(3) 0.01320(9) 0.0374(15) Uani 1 1 d . . . N5 N 0.5811(4) 0.4645(4) 0.18943(15) 0.033(2) Uani 1 1 d . . . C5 C 0.2116(5) 0.5486(5) 0.13945(17) 0.028(3) Uani 1 1 d . . . F6 F 0.3925(3) 0.6437(3) -0.03063(10) 0.0541(19) Uani 1 1 d . . . N6 N 0.5945(4) 0.4801(4) 0.13645(16) 0.035(2) Uani 1 1 d . . . C6 C 0.2259(5) 0.5266(5) 0.11768(17) 0.025(2) Uani 1 1 d . . . F7 F 0.4591(4) 0.4811(4) -0.04396(12) 0.072(2) Uani 1 1 d . . . N7 N 0.4687(4) 0.3179(4) 0.13857(15) 0.035(2) Uani 1 1 d . . . C7 C 0.1559(5) 0.3844(5) 0.07157(16) 0.030(3) Uani 1 1 d . . . H7A H 0.1094 0.3777 0.0725 0.036 Uiso 1 1 calc R . . H7B H 0.1559 0.3459 0.0802 0.036 Uiso 1 1 calc R . . F8 F 0.4161(3) 0.4291(4) -0.00011(11) 0.0582(19) Uani 1 1 d . . . N8 N 0.4613(4) 0.2982(4) 0.19113(16) 0.037(2) Uani 1 1 d . . . C8 C 0.1748(5) 0.3853(5) 0.04502(17) 0.033(3) Uani 1 1 d . . . H8A H 0.1372 0.3460 0.0363 0.039 Uiso 1 1 calc R . . H8B H 0.2155 0.3800 0.0441 0.039 Uiso 1 1 calc R . . F9 F 0.2460(3) 0.6033(3) 0.05863(9) 0.0305(14) Uani 1 1 d . . . C9 C 0.2017(5) 0.4425(6) 0.00505(17) 0.045(3) Uani 1 1 d . . . H9A H 0.2395 0.4336 0.0034 0.067 Uiso 1 1 calc R . . H9B H 0.2130 0.4848 -0.0037 0.067 Uiso 1 1 calc R . . H9C H 0.1606 0.4048 -0.0023 0.067 Uiso 1 1 calc R . . F10 F 0.5791(3) 0.2710(3) 0.16338(10) 0.0394(15) Uani 1 1 d . . . C10 C 0.1306(5) 0.4610(5) 0.03306(19) 0.040(3) Uani 1 1 d . . . H10A H 0.1408 0.5016 0.0233 0.061 Uiso 1 1 calc R . . H10B H 0.1221 0.4677 0.0505 0.061 Uiso 1 1 calc R . . H10C H 0.0901 0.4215 0.0262 0.061 Uiso 1 1 calc R . . F11 F 0.6239(3) 0.3849(3) 0.20946(10) 0.0385(15) Uani 1 1 d . . . C11 C 0.3755(5) 0.5074(5) 0.00979(19) 0.034(3) Uani 1 1 d . . . F12 F 0.6906(3) 0.4119(3) 0.25291(11) 0.0523(18) Uani 1 1 d . . . C12 C 0.3709(5) 0.5602(5) -0.00068(17) 0.030(3) Uani 1 1 d . . . F13 F 0.6552(4) 0.5963(4) 0.26563(11) 0.063(2) Uani 1 1 d . . . C13 C 0.3976(6) 0.5892(6) -0.0237(2) 0.041(3) Uani 1 1 d . . . F14 F 0.5946(4) 0.5759(3) 0.22196(11) 0.0583(19) Uani 1 1 d . . . C14 C 0.4282(6) 0.5648(7) -0.03886(19) 0.050(4) Uani 1 1 d . . . H14 H 0.4460 0.5840 -0.0548 0.061 Uiso 1 1 calc R . . F15 F 0.5823(3) 0.3324(3) 0.11745(10) 0.0397(15) Uani 1 1 d . . . C15 C 0.4318(6) 0.5110(7) -0.0297(2) 0.050(4) Uani 1 1 d . . . F16 F 0.5836(4) 0.2726(3) 0.07456(11) 0.058(2) Uani 1 1 d . . . C16 C 0.4076(5) 0.4828(6) -0.00623(19) 0.039(3) Uani 1 1 d . . . F17 F 0.3518(4) 0.1972(5) 0.06334(14) 0.100(3) Uani 1 1 d . . . C17 C 0.3676(5) 0.4378(5) 0.04603(18) 0.032(3) Uani 1 1 d . . . H17A H 0.4169 0.4544 0.0447 0.039 Uiso 1 1 calc R . . H17B H 0.3430 0.3932 0.0376 0.039 Uiso 1 1 calc R . . F18 F 0.3466(4) 0.2507(4) 0.10612(13) 0.079(2) Uani 1 1 d . . . C18 C 0.3472(5) 0.4295(5) 0.07343(17) 0.032(3) Uani 1 1 d . . . H18A H 0.2972 0.4014 0.0747 0.038 Uiso 1 1 calc R . . H18B H 0.3671 0.4050 0.0821 0.038 Uiso 1 1 calc R . . C19 C 0.4436(5) 0.5396(5) 0.08391(18) 0.038(3) Uani 1 1 d . . . H19A H 0.4573 0.5837 0.0917 0.057 Uiso 1 1 calc R . . H19B H 0.4562 0.5464 0.0662 0.057 Uiso 1 1 calc R . . H19C H 0.4667 0.5184 0.0923 0.057 Uiso 1 1 calc R . . C20 C 0.3513(6) 0.4809(5) 0.11265(18) 0.041(3) Uani 1 1 d . . . H20A H 0.3772 0.4618 0.1203 0.062 Uiso 1 1 calc R . . H20B H 0.3025 0.4482 0.1141 0.062 Uiso 1 1 calc R . . H20C H 0.3617 0.5231 0.1213 0.062 Uiso 1 1 calc R . . C21 C 0.6093(5) 0.4804(5) 0.21245(19) 0.032(3) Uani 1 1 d . . . C22 C 0.6324(5) 0.4393(5) 0.22293(18) 0.034(3) Uani 1 1 d . . . C23 C 0.6660(6) 0.4528(5) 0.24545(19) 0.037(3) Uani 1 1 d . . . C24 C 0.6745(6) 0.5057(5) 0.2604(2) 0.044(3) Uani 1 1 d . . . H24 H 0.6966 0.5148 0.2762 0.053 Uiso 1 1 calc R . . C25 C 0.6494(6) 0.5438(6) 0.2512(2) 0.048(3) Uani 1 1 d . . . C26 C 0.6190(6) 0.5339(5) 0.2292(2) 0.039(3) Uani 1 1 d . . . C27 C 0.5662(5) 0.5135(6) 0.17703(18) 0.041(3) Uani 1 1 d . . . H27A H 0.6067 0.5596 0.1780 0.049 Uiso 1 1 calc R . . H27B H 0.5284 0.5145 0.1859 0.049 Uiso 1 1 calc R . . C28 C 0.5468(5) 0.4946(5) 0.14954(18) 0.038(3) Uani 1 1 d . . . H28A H 0.5007 0.4542 0.1487 0.046 Uiso 1 1 calc R . . H28B H 0.5454 0.5326 0.1410 0.046 Uiso 1 1 calc R . . C29 C 0.5747(6) 0.4670(6) 0.10964(18) 0.048(3) Uani 1 1 d . . . H29A H 0.5261 0.4336 0.1083 0.072 Uiso 1 1 calc R . . H29B H 0.6011 0.4491 0.1014 0.072 Uiso 1 1 calc R . . H29C H 0.5840 0.5095 0.1016 0.072 Uiso 1 1 calc R . . C30 C 0.6632(6) 0.5385(6) 0.1380(2) 0.050(3) Uani 1 1 d . . . H30A H 0.6642 0.5781 0.1302 0.075 Uiso 1 1 calc R . . H30B H 0.6948 0.5282 0.1292 0.075 Uiso 1 1 calc R . . H30C H 0.6767 0.5486 0.1555 0.075 Uiso 1 1 calc R . . C31 C 0.4646(5) 0.2921(5) 0.11517(19) 0.035(3) Uani 1 1 d . . . C32 C 0.5229(6) 0.2975(5) 0.10391(19) 0.038(3) Uani 1 1 d . . . C33 C 0.5256(7) 0.2691(6) 0.0818(2) 0.041(3) Uani 1 1 d . . . C34 C 0.4674(7) 0.2340(6) 0.0677(2) 0.059(4) Uani 1 1 d . . . H34 H 0.4678 0.2132 0.0523 0.071 Uiso 1 1 calc R . . C35 C 0.4090(7) 0.2298(7) 0.0766(2) 0.064(4) Uani 1 1 d . . . C36 C 0.4063(6) 0.2576(6) 0.0996(2) 0.049(3) Uani 1 1 d . . . C37 C 0.4045(5) 0.3006(5) 0.15120(19) 0.041(3) Uani 1 1 d . . . H37A H 0.3723 0.2511 0.1499 0.049 Uiso 1 1 calc R . . H37B H 0.3835 0.3249 0.1432 0.049 Uiso 1 1 calc R . . C38 C 0.4189(5) 0.3206(5) 0.1777(2) 0.039(3) Uani 1 1 d . . . H38A H 0.3749 0.3021 0.1866 0.047 Uiso 1 1 calc R . . H38B H 0.4417 0.3707 0.1787 0.047 Uiso 1 1 calc R . . C39 C 0.4297(6) 0.2235(6) 0.1892(2) 0.055(4) Uani 1 1 d . . . H39A H 0.4596 0.2091 0.1969 0.082 Uiso 1 1 calc R . . H39B H 0.4228 0.2102 0.1715 0.082 Uiso 1 1 calc R . . H39C H 0.3858 0.2017 0.1978 0.082 Uiso 1 1 calc R . . C40 C 0.4669(5) 0.3170(6) 0.21779(19) 0.047(3) Uani 1 1 d . . . H40A H 0.4213 0.2983 0.2250 0.071 Uiso 1 1 calc R . . H40B H 0.4913 0.3667 0.2194 0.071 Uiso 1 1 calc R . . H40C H 0.4918 0.2986 0.2267 0.071 Uiso 1 1 calc R . . C41 C 0.0626(11) 0.7365(13) -0.0265(4) 0.086(4) Uiso 0.50 1 d PD B 1 H41A H 0.1085 0.7760 -0.0254 0.129 Uiso 0.50 1 calc PR B 1 H41B H 0.0561 0.7155 -0.0430 0.129 Uiso 0.50 1 calc PR B 1 H41C H 0.0566 0.7034 -0.0136 0.129 Uiso 0.50 1 calc PR B 1 C42 C 0.0107(9) 0.7592(9) -0.0227(3) 0.086(4) Uiso 0.50 1 d PD B 1 C43 C -0.0010(13) 0.7917(14) -0.0423(4) 0.086(4) Uiso 0.50 1 d PD B 1 H43 H 0.0247 0.8028 -0.0573 0.103 Uiso 0.50 1 calc PR B 1 C44 C -0.0509(12) 0.8070(13) -0.0390(4) 0.086(4) Uiso 0.50 1 d PD B 1 H44 H -0.0693 0.8180 -0.0531 0.103 Uiso 0.50 1 calc PR B 1 C45 C -0.0747(12) 0.8066(13) -0.0158(4) 0.086(4) Uiso 0.50 1 d PD B 1 H45 H -0.0933 0.8348 -0.0119 0.103 Uiso 0.50 1 calc PR B 1 C46 C -0.0717(13) 0.7654(15) 0.0019(4) 0.086(4) Uiso 0.50 1 d PD B 1 H46 H -0.1028 0.7497 0.0155 0.103 Uiso 0.50 1 calc PR B 1 C47 C -0.0232(15) 0.7468(17) -0.0002(4) 0.086(4) Uiso 0.50 1 d PD B 1 H47 H -0.0132 0.7261 0.0133 0.103 Uiso 0.50 1 calc PR B 1 C52 C 0.0115(18) 0.7927(19) -0.0438(5) 0.167(8) Uiso 0.50 1 d PD A 2 H52 H 0.0308 0.8112 -0.0597 0.200 Uiso 0.50 1 calc PR A 2 C50 C -0.0383(17) 0.8680(15) -0.0419(6) 0.167(8) Uiso 0.50 1 d PD A 2 H50A H -0.0650 0.8793 -0.0305 0.250 Uiso 0.25 1 calc PR A 2 H50B H -0.0633 0.8501 -0.0575 0.250 Uiso 0.25 1 calc PR A 2 H50C H 0.0053 0.9090 -0.0454 0.250 Uiso 0.25 1 calc PR A 2 H50D H -0.0170 0.8796 -0.0584 0.250 Uiso 0.25 1 calc PR A 2 H50E H -0.0187 0.9088 -0.0314 0.250 Uiso 0.25 1 calc PR A 2 H50F H -0.0873 0.8499 -0.0436 0.250 Uiso 0.25 1 calc PR A 2 C56 C -0.0558(19) 0.790(2) -0.0064(6) 0.167(8) Uiso 0.50 1 d PD A 2 H56 H -0.0827 0.8054 0.0020 0.200 Uiso 0.50 1 calc PR A 2 C54 C 0.0077(18) 0.7347(18) -0.0075(6) 0.167(8) Uiso 0.50 1 d PD A 2 H54 H 0.0360 0.7248 0.0026 0.200 Uiso 0.50 1 calc PR A 2 C55 C -0.043(2) 0.742(2) 0.0032(6) 0.167(8) Uiso 0.50 1 d PD A 2 H55 H -0.0681 0.7140 0.0169 0.200 Uiso 0.50 1 calc PR A 2 C51 C -0.0256(11) 0.8151(12) -0.0299(4) 0.167(8) Uiso 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0253(4) 0.0216(4) 0.0224(3) -0.0004(3) 0.0029(3) 0.0117(3) F4 0.050(4) 0.034(4) 0.052(4) 0.009(3) 0.018(3) 0.010(3) N1 0.034(5) 0.027(5) 0.021(5) -0.007(4) -0.002(4) 0.013(4) C1 0.026(6) 0.027(6) 0.019(6) 0.007(5) -0.001(5) 0.012(5) Ce2 0.0257(4) 0.0274(4) 0.0335(4) -0.0040(3) -0.0027(3) 0.0150(3) F3 0.059(5) 0.045(4) 0.050(4) 0.013(3) 0.025(4) 0.019(4) N2 0.032(5) 0.037(6) 0.030(5) -0.008(4) -0.002(4) 0.018(5) C2 0.028(6) 0.013(6) 0.036(6) -0.002(5) 0.005(5) 0.008(5) F2 0.043(4) 0.033(4) 0.028(3) -0.003(3) 0.001(3) 0.014(3) N3 0.030(5) 0.038(6) 0.024(5) -0.001(4) 0.003(4) 0.018(5) C3 0.032(7) 0.051(8) 0.019(6) 0.013(6) 0.015(5) 0.021(6) F1 0.030(3) 0.027(3) 0.023(3) -0.005(3) -0.001(3) 0.005(3) N4 0.026(5) 0.027(5) 0.025(5) -0.006(4) -0.001(4) 0.014(4) C4 0.033(7) 0.038(7) 0.023(6) 0.004(5) 0.008(5) 0.023(6) F5 0.063(4) 0.036(4) 0.023(3) 0.006(3) 0.013(3) 0.032(3) N5 0.038(6) 0.035(6) 0.031(5) -0.007(4) 0.003(4) 0.022(5) C5 0.050(7) 0.031(7) 0.017(5) -0.010(5) 0.000(5) 0.031(6) F6 0.066(5) 0.060(5) 0.030(4) 0.010(3) 0.005(3) 0.026(4) N6 0.032(6) 0.028(5) 0.046(6) -0.002(5) -0.003(5) 0.016(5) C6 0.019(6) 0.019(6) 0.024(6) 0.014(5) 0.005(5) 0.000(5) F7 0.070(5) 0.113(7) 0.047(4) -0.009(4) 0.020(4) 0.057(5) N7 0.034(6) 0.040(6) 0.032(5) -0.009(4) -0.004(4) 0.019(5) C7 0.032(6) 0.026(6) 0.030(6) -0.010(5) -0.002(5) 0.013(5) F8 0.064(5) 0.073(5) 0.055(4) -0.020(4) 0.007(4) 0.047(4) N8 0.037(6) 0.033(6) 0.044(6) -0.012(5) 0.002(5) 0.020(5) C8 0.041(7) 0.019(6) 0.037(7) -0.012(5) -0.006(5) 0.014(5) F9 0.032(3) 0.031(3) 0.034(3) -0.003(3) -0.006(3) 0.021(3) C9 0.036(7) 0.054(8) 0.033(7) -0.010(6) 0.000(5) 0.014(6) F10 0.039(4) 0.026(3) 0.056(4) -0.003(3) 0.003(3) 0.018(3) C10 0.035(7) 0.045(8) 0.042(7) 0.001(6) -0.002(6) 0.021(6) F11 0.048(4) 0.031(4) 0.043(4) -0.005(3) -0.007(3) 0.025(3) C11 0.034(7) 0.038(7) 0.031(6) -0.001(5) 0.005(5) 0.018(6) F12 0.059(5) 0.050(4) 0.050(4) -0.004(3) -0.019(3) 0.030(4) C12 0.039(7) 0.028(6) 0.020(6) -0.002(5) 0.011(5) 0.015(6) F13 0.091(6) 0.074(5) 0.047(4) -0.029(4) -0.027(4) 0.059(5) C13 0.042(8) 0.039(8) 0.041(7) 0.003(6) -0.006(6) 0.018(6) F14 0.085(5) 0.057(5) 0.058(4) -0.013(4) -0.012(4) 0.054(4) C14 0.052(9) 0.088(11) 0.018(6) -0.008(7) -0.003(6) 0.040(8) F15 0.028(4) 0.051(4) 0.038(4) -0.007(3) -0.002(3) 0.018(3) C15 0.031(7) 0.088(11) 0.035(7) -0.025(7) 0.001(6) 0.032(8) F16 0.079(5) 0.068(5) 0.038(4) 0.001(4) 0.021(4) 0.047(5) C16 0.038(7) 0.046(8) 0.031(7) -0.005(6) 0.005(5) 0.020(6) F17 0.062(6) 0.141(8) 0.078(6) -0.060(6) -0.038(5) 0.035(6) C17 0.040(7) 0.023(6) 0.046(7) -0.006(5) 0.002(5) 0.024(6) F18 0.044(5) 0.115(7) 0.077(5) -0.029(5) -0.022(4) 0.040(5) C18 0.035(7) 0.027(6) 0.031(6) 0.008(5) 0.010(5) 0.014(5) C19 0.033(7) 0.039(7) 0.041(7) -0.005(6) -0.005(5) 0.018(6) C20 0.054(8) 0.041(7) 0.041(7) 0.011(6) 0.009(6) 0.033(6) C21 0.027(6) 0.031(7) 0.033(7) 0.011(5) 0.013(5) 0.012(5) C22 0.044(7) 0.042(7) 0.023(6) -0.004(5) -0.001(5) 0.027(6) C23 0.058(8) 0.033(7) 0.032(7) 0.010(5) 0.016(6) 0.031(7) C24 0.062(9) 0.032(7) 0.041(7) -0.001(6) -0.014(6) 0.026(7) C25 0.060(9) 0.030(7) 0.054(8) -0.014(6) -0.009(7) 0.023(7) C26 0.056(8) 0.028(7) 0.043(7) -0.003(6) 0.000(6) 0.028(6) C27 0.039(7) 0.051(8) 0.042(7) -0.004(6) 0.011(6) 0.030(7) C28 0.046(8) 0.024(6) 0.043(7) 0.003(5) -0.003(6) 0.015(6) C29 0.055(8) 0.066(9) 0.023(6) -0.002(6) -0.006(6) 0.031(7) C30 0.049(8) 0.045(8) 0.059(8) 0.007(7) 0.002(7) 0.025(7) C31 0.025(7) 0.037(7) 0.037(7) 0.004(5) 0.004(5) 0.010(6) C32 0.045(8) 0.034(7) 0.035(7) 0.000(6) -0.009(6) 0.020(6) C33 0.074(10) 0.035(7) 0.026(6) -0.001(5) 0.005(7) 0.036(7) C34 0.088(11) 0.059(9) 0.029(7) -0.015(6) -0.020(8) 0.036(9) C35 0.064(11) 0.082(11) 0.047(9) -0.013(8) -0.008(8) 0.038(9) C36 0.023(7) 0.057(9) 0.059(9) 0.003(7) -0.009(6) 0.013(6) C37 0.044(8) 0.040(7) 0.044(7) -0.007(6) 0.007(6) 0.024(6) C38 0.020(6) 0.030(7) 0.062(8) -0.002(6) 0.001(6) 0.008(5) C39 0.063(9) 0.040(8) 0.061(9) 0.007(7) 0.014(7) 0.026(7) C40 0.039(7) 0.049(8) 0.049(8) 0.003(6) 0.017(6) 0.019(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 Ce1 F9 2.325(5) . ? Ce1 F9 2.332(5) 2_665 ? Ce1 N3 2.467(8) . ? Ce1 N1 2.484(8) . ? Ce1 F1 2.642(5) . ? Ce1 F5 2.642(5) . ? Ce1 N2 2.673(8) . ? Ce1 N4 2.706(8) . ? F4 C2 1.355(10) . ? N1 C1 1.352(11) . ? N1 C7 1.463(11) . ? C1 C2 1.416(12) . ? C1 C6 1.421(13) . ? C53 C54 1.361(9) . ? C53 C52 1.368(9) . ? C53 H53 0.9500 . ? Ce2 F10 2.325(5) . ? Ce2 F10 2.328(5) 3_665 ? Ce2 N7 2.466(8) . ? Ce2 N5 2.474(8) . ? Ce2 F11 2.653(5) . ? Ce2 F15 2.658(5) . ? Ce2 N8 2.686(9) . ? Ce2 N6 2.710(8) . ? F3 C3 1.358(11) . ? N2 C9 1.482(11) . ? N2 C10 1.493(12) . ? N2 C8 1.495(11) . ? C2 C3 1.376(13) . ? F2 C5 1.340(11) . ? N3 C11 1.365(11) . ? N3 C17 1.474(11) . ? C3 C4 1.381(14) . ? F1 C6 1.379(10) . ? N4 C20 1.464(11) . ? N4 C19 1.468(11) . ? N4 C18 1.484(11) . ? C4 C5 1.352(13) . ? C4 H4 0.9500 . ? F5 C12 1.376(10) . ? N5 C21 1.351(12) . ? N5 C27 1.474(12) . ? C5 C6 1.369(12) . ? F6 C13 1.351(12) . ? N6 C28 1.460(12) . ? N6 C30 1.461(12) . ? N6 C29 1.488(12) . ? F7 C15 1.362(12) . ? N7 C31 1.366(12) . ? N7 C37 1.472(12) . ? C7 C8 1.481(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? F8 C16 1.365(12) . ? N8 C40 1.477(12) . ? N8 C39 1.479(13) . ? N8 C38 1.481(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 Ce1 2.332(5) 3_565 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? F10 Ce2 2.328(5) 2_655 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? F11 C22 1.358(11) . ? C11 C12 1.374(13) . ? C11 C16 1.409(14) . ? F12 C23 1.361(11) . ? C12 C13 1.387(13) . ? F13 C25 1.369(12) . ? C13 C14 1.353(15) . ? F14 C26 1.376(11) . ? C14 C15 1.357(16) . ? C14 H14 0.9500 . ? F15 C32 1.380(11) . ? C15 C16 1.391(15) . ? F16 C33 1.337(12) . ? F17 C35 1.332(14) . ? C17 C18 1.521(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? F18 C36 1.330(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.395(13) . ? C21 C26 1.437(14) . ? C22 C23 1.377(14) . ? C23 C24 1.376(14) . ? C24 C25 1.344(14) . ? C24 H24 0.9500 . ? C25 C26 1.328(14) . ? C27 C28 1.534(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.404(14) . ? C31 C36 1.420(14) . ? C32 C33 1.365(14) . ? C33 C34 1.377(15) . ? C34 C35 1.366(17) . ? C34 H34 0.9500 . ? C35 C36 1.402(16) . ? C37 C38 1.475(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.516(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C47 1.377(9) . ? C42 C43 1.384(9) . ? C43 C44 1.351(9) . ? C43 H43 0.9500 . ? C44 C45 1.356(9) . ? C44 H44 0.9500 . ? C45 C46 1.356(9) . ? C45 H45 0.9500 . ? C46 C47 1.369(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C52 C51 1.398(10) . ? C52 H52 0.9500 . ? C50 C51 1.511(8) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C50 H50D 0.9800 . ? C50 H50E 0.9800 . ? C50 H50F 0.9800 . ? C56 C55 1.375(9) . ? C56 C51 1.408(10) . ? C56 H56 0.9500 . ? C54 C55 1.357(9) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F9 Ce1 F9 82.6(3) . 2_665 ? F9 Ce1 N3 146.7(2) . . ? F9 Ce1 N3 91.7(2) 2_665 . ? F9 Ce1 N1 91.1(2) . . ? F9 Ce1 N1 146.2(2) 2_665 . ? N3 Ce1 N1 110.4(3) . . ? F9 Ce1 F1 68.00(17) . . ? F9 Ce1 F1 83.87(16) 2_665 . ? N3 Ce1 F1 144.2(2) . . ? N1 Ce1 F1 63.1(2) . . ? F9 Ce1 F5 84.73(17) . . ? F9 Ce1 F5 66.96(17) 2_665 . ? N3 Ce1 F5 63.1(2) . . ? N1 Ce1 F5 145.7(2) . . ? F1 Ce1 F5 142.52(16) . . ? F9 Ce1 N2 84.9(2) . . ? F9 Ce1 N2 145.4(2) 2_665 . ? N3 Ce1 N2 81.3(3) . . ? N1 Ce1 N2 65.9(2) . . ? F1 Ce1 N2 120.7(2) . . ? F5 Ce1 N2 79.8(2) . . ? F9 Ce1 N4 144.5(2) . . ? F9 Ce1 N4 85.2(2) 2_665 . ? N3 Ce1 N4 66.5(2) . . ? N1 Ce1 N4 80.9(2) . . ? F1 Ce1 N4 77.68(19) . . ? F5 Ce1 N4 120.4(2) . . ? N2 Ce1 N4 121.6(2) . . ? C1 N1 C7 118.4(8) . . ? C1 N1 Ce1 122.5(6) . . ? C7 N1 Ce1 117.6(5) . . ? N1 C1 C2 130.3(9) . . ? N1 C1 C6 120.2(9) . . ? C2 C1 C6 109.5(8) . . ? C54 C53 C52 116.9(10) . . ? C54 C53 H53 121.5 . . ? C52 C53 H53 121.5 . . ? F10 Ce2 F10 82.6(3) . 3_665 ? F10 Ce2 N7 91.8(2) . . ? F10 Ce2 N7 146.4(2) 3_665 . ? F10 Ce2 N5 145.9(2) . . ? F10 Ce2 N5 91.0(2) 3_665 . ? N7 Ce2 N5 110.7(3) . . ? F10 Ce2 F11 84.10(18) . . ? F10 Ce2 F11 68.22(19) 3_665 . ? N7 Ce2 F11 144.4(2) . . ? N5 Ce2 F11 62.6(2) . . ? F10 Ce2 F15 68.25(18) . . ? F10 Ce2 F15 84.38(18) 3_665 . ? N7 Ce2 F15 63.0(2) . . ? N5 Ce2 F15 144.7(2) . . ? F11 Ce2 F15 143.46(17) . . ? F10 Ce2 N8 84.4(2) . . ? F10 Ce2 N8 144.4(2) 3_665 . ? N7 Ce2 N8 66.7(3) . . ? N5 Ce2 N8 81.6(3) . . ? F11 Ce2 N8 77.6(2) . . ? F15 Ce2 N8 120.7(2) . . ? F10 Ce2 N6 145.1(2) . . ? F10 Ce2 N6 85.4(2) 3_665 . ? N7 Ce2 N6 80.5(3) . . ? N5 Ce2 N6 66.6(3) . . ? F11 Ce2 N6 121.2(2) . . ? F15 Ce2 N6 78.1(2) . . ? N8 Ce2 N6 122.0(3) . . ? C9 N2 C10 106.9(8) . . ? C9 N2 C8 108.6(8) . . ? C10 N2 C8 111.7(8) . . ? C9 N2 Ce1 116.4(6) . . ? C10 N2 Ce1 114.5(6) . . ? C8 N2 Ce1 98.5(5) . . ? F4 C2 C3 117.0(9) . . ? F4 C2 C1 119.7(9) . . ? C3 C2 C1 123.3(9) . . ? C11 N3 C17 119.3(8) . . ? C11 N3 Ce1 122.6(7) . . ? C17 N3 Ce1 117.6(6) . . ? F3 C3 C2 117.2(10) . . ? F3 C3 C4 118.7(9) . . ? C2 C3 C4 124.1(9) . . ? C6 F1 Ce1 118.2(5) . . ? C20 N4 C19 109.7(8) . . ? C20 N4 C18 107.7(7) . . ? C19 N4 C18 110.6(7) . . ? C20 N4 Ce1 116.7(6) . . ? C19 N4 Ce1 113.5(6) . . ? C18 N4 Ce1 97.7(5) . . ? C5 C4 C3 114.6(9) . . ? C5 C4 H4 122.7 . . ? C3 C4 H4 122.7 . . ? C12 F5 Ce1 117.4(5) . . ? C21 N5 C27 117.7(8) . . ? C21 N5 Ce2 123.9(7) . . ? C27 N5 Ce2 117.3(6) . . ? F2 C5 C4 119.9(9) . . ? F2 C5 C6 118.0(9) . . ? C4 C5 C6 121.9(10) . . ? C28 N6 C30 110.1(8) . . ? C28 N6 C29 108.9(8) . . ? C30 N6 C29 108.3(8) . . ? C28 N6 Ce2 98.3(6) . . ? C30 N6 Ce2 114.7(6) . . ? C29 N6 Ce2 115.9(6) . . ? C5 C6 F1 118.5(9) . . ? C5 C6 C1 126.3(9) . . ? F1 C6 C1 115.1(8) . . ? C31 N7 C37 117.4(8) . . ? C31 N7 Ce2 123.4(7) . . ? C37 N7 Ce2 118.1(6) . . ? N1 C7 C8 110.9(8) . . ? N1 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? C40 N8 C39 108.8(8) . . ? C40 N8 C38 110.2(8) . . ? C39 N8 C38 109.4(8) . . ? C40 N8 Ce2 115.8(6) . . ? C39 N8 Ce2 115.6(6) . . ? C38 N8 Ce2 96.2(6) . . ? C7 C8 N2 112.8(8) . . ? C7 C8 H8A 109.0 . . ? N2 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? N2 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? Ce1 F9 Ce1 157.4(3) . 3_565 ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Ce2 F10 Ce2 157.4(3) . 2_655 ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C22 F11 Ce2 117.3(5) . . ? N3 C11 C12 120.0(9) . . ? N3 C11 C16 127.7(10) . . ? C12 C11 C16 112.3(9) . . ? C11 C12 F5 116.8(8) . . ? C11 C12 C13 124.8(10) . . ? F5 C12 C13 118.4(9) . . ? F6 C13 C14 120.5(11) . . ? F6 C13 C12 117.4(10) . . ? C14 C13 C12 122.0(11) . . ? C13 C14 C15 115.2(11) . . ? C13 C14 H14 122.4 . . ? C15 C14 H14 122.4 . . ? C32 F15 Ce2 117.8(6) . . ? C14 C15 F7 119.6(11) . . ? C14 C15 C16 123.7(11) . . ? F7 C15 C16 116.8(12) . . ? F8 C16 C15 115.3(10) . . ? F8 C16 C11 122.7(10) . . ? C15 C16 C11 121.9(11) . . ? N3 C17 C18 111.2(7) . . ? N3 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? N3 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N4 C18 C17 112.9(8) . . ? N4 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? N4 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C22 118.3(10) . . ? N5 C21 C26 130.3(10) . . ? C22 C21 C26 111.4(10) . . ? F11 C22 C23 118.5(9) . . ? F11 C22 C21 117.7(9) . . ? C23 C22 C21 123.8(10) . . ? F12 C23 C24 120.0(10) . . ? F12 C23 C22 118.5(9) . . ? C24 C23 C22 121.6(10) . . ? C25 C24 C23 115.4(11) . . ? C25 C24 H24 122.3 . . ? C23 C24 H24 122.3 . . ? C26 C25 C24 124.7(11) . . ? C26 C25 F13 117.5(10) . . ? C24 C25 F13 117.8(11) . . ? C25 C26 F14 119.3(10) . . ? C25 C26 C21 122.9(10) . . ? F14 C26 C21 117.8(10) . . ? N5 C27 C28 111.3(8) . . ? N5 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? N5 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? N6 C28 C27 112.4(8) . . ? N6 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? N6 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N6 C30 H30A 109.5 . . ? N6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N7 C31 C32 119.7(10) . . ? N7 C31 C36 128.2(10) . . ? C32 C31 C36 112.1(10) . . ? C33 C32 F15 117.7(10) . . ? C33 C32 C31 126.5(11) . . ? F15 C32 C31 115.8(9) . . ? F16 C33 C32 119.9(11) . . ? F16 C33 C34 120.6(11) . . ? C32 C33 C34 119.4(12) . . ? C35 C34 C33 117.9(12) . . ? C35 C34 H34 121.0 . . ? C33 C34 H34 121.0 . . ? F17 C35 C34 119.8(12) . . ? F17 C35 C36 117.9(12) . . ? C34 C35 C36 122.2(12) . . ? F18 C36 C35 116.6(11) . . ? F18 C36 C31 121.7(11) . . ? C35 C36 C31 121.7(11) . . ? N7 C37 C38 108.8(9) . . ? N7 C37 H37A 109.9 . . ? C38 C37 H37A 109.9 . . ? N7 C37 H37B 109.9 . . ? C38 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? C37 C38 N8 116.3(9) . . ? C37 C38 H38A 108.2 . . ? N8 C38 H38A 108.2 . . ? C37 C38 H38B 108.2 . . ? N8 C38 H38B 108.2 . . ? H38A C38 H38B 107.4 . . ? N8 C39 H39A 109.5 . . ? N8 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N8 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N8 C40 H40A 109.5 . . ? N8 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N8 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C47 C42 C43 122.1(9) . . ? C47 C42 C41 119.8(9) . . ? C43 C42 C41 118.0(8) . . ? C44 C43 C42 116.8(9) . . ? C44 C43 H43 121.6 . . ? C42 C43 H43 121.6 . . ? C43 C44 C45 119.9(9) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 119.2(10) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 118.7(8) . . ? C45 C46 H46 120.6 . . ? C47 C46 H46 120.6 . . ? C46 C47 C42 117.7(10) . . ? C46 C47 H47 121.2 . . ? C42 C47 H47 121.2 . . ? C53 C52 C51 114.0(10) . . ? C53 C52 H52 123.0 . . ? C51 C52 H52 123.0 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C51 C50 H50D 109.5 . . ? H50A C50 H50D 141.1 . . ? H50B C50 H50D 56.3 . . ? H50C C50 H50D 56.3 . . ? C51 C50 H50E 109.5 . . ? H50A C50 H50E 56.3 . . ? H50B C50 H50E 141.1 . . ? H50C C50 H50E 56.3 . . ? H50D C50 H50E 109.5 . . ? C51 C50 H50F 109.5 . . ? H50A C50 H50F 56.3 . . ? H50B C50 H50F 56.3 . . ? H50C C50 H50F 141.1 . . ? H50D C50 H50F 109.5 . . ? H50E C50 H50F 109.5 . . ? C55 C56 C51 113.4(10) . . ? C55 C56 H56 123.3 . . ? C51 C56 H56 123.3 . . ? C55 C54 C53 120.1(12) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 118.1(10) . . ? C54 C55 H55 121.0 . . ? C56 C55 H55 121.0 . . ? C52 C51 C56 126.3(9) . . ? C52 C51 C50 116.9(8) . . ? C56 C51 C50 116.7(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.109 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.186 # Attachment '5 [Nd(p-HC6F4NC2H4NMe2)3].CIF' data_[Nd(p-HC6F4NC2H4NMe2)3].CIF _database_code_depnum_ccdc_archive 'CCDC 859383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(N,N-dimethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine -F,N,N'/N,N)-neodymium(iii) ; _chemical_name_common ? _chemical_melting_point '174-178 \%C' _chemical_formula_moiety 'C30 H33 F12 N6 Nd' _chemical_formula_sum 'C30 H33 F12 N6 Nd' _chemical_formula_weight 849.86 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7596(3) _cell_length_b 9.7779(3) _cell_length_c 17.8383(6) _cell_angle_alpha 89.367(2) _cell_angle_beta 75.192(2) _cell_angle_gamma 81.488(2) _cell_volume 1626.98(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 34618 _cell_measurement_theta_min 1.560 _cell_measurement_theta_max 30.115 _exptl_crystal_description Rhombus _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6764 _exptl_absorpt_correction_T_max 0.8762 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28652 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7464 _reflns_number_gt 7111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7464 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.175123(9) 0.261606(9) 0.265147(5) 0.01577(4) Uani 1 1 d . . . F1 F -0.00384(12) 0.36344(13) 0.18749(7) 0.0286(3) Uani 1 1 d . . . N1 N 0.24548(17) 0.20513(17) 0.12778(9) 0.0226(3) Uani 1 1 d . . . C1 C 0.1549(2) 0.2343(2) 0.08130(11) 0.0232(4) Uani 1 1 d . . . F2 F -0.19633(15) 0.44794(17) 0.10842(9) 0.0458(4) Uani 1 1 d . . . N2 N 0.46043(17) 0.19013(17) 0.21316(10) 0.0232(3) Uani 1 1 d . . . C2 C 0.0240(2) 0.3209(2) 0.11135(11) 0.0257(4) Uani 1 1 d . . . F3 F 0.0951(2) 0.1841(2) -0.10946(9) 0.0662(5) Uani 1 1 d . . . N3 N 0.18428(16) 0.09913(16) 0.37230(9) 0.0183(3) Uani 1 1 d . . . C3 C -0.0768(2) 0.3635(2) 0.07160(14) 0.0334(5) Uani 1 1 d . . . F4 F 0.28093(16) 0.09284(16) -0.03209(8) 0.0436(3) Uani 1 1 d . . . N4 N 0.04292(17) 0.03784(17) 0.25556(9) 0.0208(3) Uani 1 1 d . . . C4 C -0.0565(3) 0.3211(3) -0.00450(15) 0.0443(6) Uani 1 1 d . . . H4 H -0.1242 0.3510 -0.0335 0.053 Uiso 1 1 calc R . . F5 F 0.28978(12) 0.33221(11) 0.37354(7) 0.0239(2) Uani 1 1 d . . . N5 N 0.17906(17) 0.50686(16) 0.27218(9) 0.0205(3) Uani 1 1 d . . . C5 C 0.0678(3) 0.2329(3) -0.03553(14) 0.0422(6) Uani 1 1 d . . . F6 F 0.42428(14) 0.40028(13) 0.47691(8) 0.0318(3) Uani 1 1 d . . . N6 N -0.07536(17) 0.39789(17) 0.36334(10) 0.0224(3) Uani 1 1 d . . . C6 C 0.1687(2) 0.1882(2) 0.00455(12) 0.0318(5) Uani 1 1 d . . . F7 F 0.36040(13) -0.02351(14) 0.59891(7) 0.0320(3) Uani 1 1 d . . . C7 C 0.3939(2) 0.1424(2) 0.09121(12) 0.0308(4) Uani 1 1 d . . . H7A H 0.4175 0.1597 0.0349 0.037 Uiso 1 1 calc R . . H7B H 0.4051 0.0412 0.0982 0.037 Uiso 1 1 calc R . . F8 F 0.24452(13) -0.10091(13) 0.49347(7) 0.0302(3) Uani 1 1 d . . . C8 C 0.4948(2) 0.2062(2) 0.12890(13) 0.0310(4) Uani 1 1 d . . . H8A H 0.5945 0.1618 0.1058 0.037 Uiso 1 1 calc R . . H8B H 0.4887 0.3060 0.1175 0.037 Uiso 1 1 calc R . . F9 F 0.26759(15) 0.51888(14) 0.11407(7) 0.0333(3) Uani 1 1 d . . . C9 C 0.4993(2) 0.0459(2) 0.23246(15) 0.0343(5) Uani 1 1 d . . . H9A H 0.4422 -0.0126 0.2128 0.051 Uiso 1 1 calc R . . H9B H 0.4803 0.0385 0.2889 0.051 Uiso 1 1 calc R . . H9C H 0.6014 0.0155 0.2086 0.051 Uiso 1 1 calc R . . F10 F 0.4980(2) 0.62851(18) 0.04148(8) 0.0561(5) Uani 1 1 d . . . C10 C 0.5518(2) 0.2731(3) 0.24375(16) 0.0370(5) Uani 1 1 d . . . H10A H 0.6523 0.2465 0.2154 0.055 Uiso 1 1 calc R . . H10B H 0.5408 0.2557 0.2990 0.055 Uiso 1 1 calc R . . H10C H 0.5222 0.3717 0.2369 0.055 Uiso 1 1 calc R . . F11 F 0.57629(16) 0.74095(16) 0.28076(9) 0.0441(3) Uani 1 1 d . . . C11 C 0.30836(19) 0.24090(19) 0.43039(11) 0.0199(3) Uani 1 1 d . . . F12 F 0.35063(15) 0.62996(14) 0.35535(7) 0.0344(3) Uani 1 1 d . . . C12 C 0.3767(2) 0.2773(2) 0.48321(12) 0.0231(4) Uani 1 1 d . . . C13 C 0.3954(2) 0.1913(2) 0.54286(11) 0.0251(4) Uani 1 1 d . . . H13 H 0.4407 0.2157 0.5810 0.030 Uiso 1 1 calc R . . C14 C 0.3440(2) 0.0681(2) 0.54320(11) 0.0242(4) Uani 1 1 d . . . C15 C 0.2782(2) 0.0290(2) 0.48862(11) 0.0219(4) Uani 1 1 d . . . C16 C 0.25216(18) 0.11657(19) 0.42835(10) 0.0184(3) Uani 1 1 d . . . C17 C 0.1123(2) -0.0237(2) 0.37869(12) 0.0225(4) Uani 1 1 d . . . H17A H 0.0709 -0.0411 0.4340 0.027 Uiso 1 1 calc R . . H17B H 0.1829 -0.1055 0.3559 0.027 Uiso 1 1 calc R . . C18 C -0.0053(2) -0.0023(2) 0.33677(12) 0.0229(4) Uani 1 1 d . . . H18A H -0.0467 -0.0891 0.3379 0.028 Uiso 1 1 calc R . . H18B H -0.0823 0.0703 0.3650 0.028 Uiso 1 1 calc R . . C19 C 0.1439(2) -0.0762(2) 0.20918(13) 0.0278(4) Uani 1 1 d . . . H19A H 0.0966 -0.1584 0.2115 0.042 Uiso 1 1 calc R . . H19B H 0.2280 -0.0973 0.2301 0.042 Uiso 1 1 calc R . . H19C H 0.1741 -0.0486 0.1552 0.042 Uiso 1 1 calc R . . C20 C -0.0838(2) 0.0622(2) 0.22391(13) 0.0289(4) Uani 1 1 d . . . H20A H -0.1318 -0.0201 0.2309 0.043 Uiso 1 1 calc R . . H20B H -0.0538 0.0810 0.1685 0.043 Uiso 1 1 calc R . . H20C H -0.1502 0.1417 0.2513 0.043 Uiso 1 1 calc R . . C21 C 0.2959(2) 0.56825(18) 0.23817(11) 0.0203(4) Uani 1 1 d . . . C22 C 0.3441(2) 0.5718(2) 0.15710(12) 0.0251(4) Uani 1 1 d . . . C23 C 0.4625(3) 0.6288(2) 0.11954(12) 0.0337(5) Uani 1 1 d . . . C24 C 0.5433(3) 0.6879(2) 0.15914(14) 0.0359(5) Uani 1 1 d . . . H24 H 0.6255 0.7268 0.1330 0.043 Uiso 1 1 calc R . . C25 C 0.4987(2) 0.6875(2) 0.23851(14) 0.0302(4) Uani 1 1 d . . . C26 C 0.3806(2) 0.6310(2) 0.27720(11) 0.0243(4) Uani 1 1 d . . . C27 C 0.0849(2) 0.5780(2) 0.34262(12) 0.0258(4) Uani 1 1 d . . . H27A H 0.0859 0.6790 0.3391 0.031 Uiso 1 1 calc R . . H27B H 0.1187 0.5455 0.3885 0.031 Uiso 1 1 calc R . . C28 C -0.0649(2) 0.5469(2) 0.35064(13) 0.0277(4) Uani 1 1 d . . . H28A H -0.1314 0.6024 0.3948 0.033 Uiso 1 1 calc R . . H28B H -0.0950 0.5749 0.3031 0.033 Uiso 1 1 calc R . . C29 C -0.0719(2) 0.3651(2) 0.44404(12) 0.0267(4) Uani 1 1 d . . . H29A H -0.1533 0.4210 0.4800 0.040 Uiso 1 1 calc R . . H29B H 0.0178 0.3860 0.4531 0.040 Uiso 1 1 calc R . . H29C H -0.0780 0.2668 0.4524 0.040 Uiso 1 1 calc R . . C30 C -0.2168(2) 0.3749(2) 0.35459(14) 0.0311(5) Uani 1 1 d . . . H30A H -0.2925 0.4357 0.3914 0.047 Uiso 1 1 calc R . . H30B H -0.2288 0.2782 0.3650 0.047 Uiso 1 1 calc R . . H30C H -0.2229 0.3957 0.3016 0.047 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 Nd1 0.01586(5) 0.01623(5) 0.01552(5) -0.00265(3) -0.00640(3) 0.00099(3) F1 0.0255(6) 0.0358(7) 0.0236(6) -0.0072(5) -0.0117(5) 0.0087(5) N1 0.0222(8) 0.0260(8) 0.0183(7) -0.0036(6) -0.0062(6) 0.0025(6) C1 0.0272(10) 0.0248(9) 0.0195(9) -0.0011(7) -0.0090(7) -0.0047(7) F2 0.0345(7) 0.0535(9) 0.0519(9) -0.0003(7) -0.0253(7) 0.0101(6) N2 0.0169(7) 0.0241(8) 0.0277(8) -0.0024(7) -0.0072(6) 0.0026(6) C2 0.0305(10) 0.0284(10) 0.0211(9) -0.0012(8) -0.0129(8) -0.0022(8) F3 0.0740(12) 0.1008(15) 0.0311(8) -0.0181(9) -0.0288(8) -0.0079(11) N3 0.0192(7) 0.0180(7) 0.0194(7) -0.0003(6) -0.0082(6) -0.0027(6) C3 0.0322(11) 0.0365(12) 0.0363(12) 0.0016(9) -0.0197(9) -0.0011(9) F4 0.0465(8) 0.0517(9) 0.0298(7) -0.0191(6) -0.0078(6) -0.0007(7) N4 0.0186(7) 0.0218(8) 0.0241(8) -0.0039(6) -0.0108(6) -0.0001(6) C4 0.0483(15) 0.0577(16) 0.0382(13) 0.0052(12) -0.0308(12) -0.0092(12) F5 0.0302(6) 0.0205(5) 0.0262(6) 0.0028(4) -0.0154(5) -0.0061(4) N5 0.0231(8) 0.0188(7) 0.0185(7) -0.0015(6) -0.0044(6) -0.0006(6) C5 0.0531(15) 0.0577(16) 0.0237(11) -0.0044(10) -0.0205(10) -0.0136(12) F6 0.0341(7) 0.0288(6) 0.0387(7) -0.0064(5) -0.0183(6) -0.0083(5) N6 0.0200(8) 0.0224(8) 0.0233(8) -0.0051(6) -0.0031(6) -0.0020(6) C6 0.0363(11) 0.0371(12) 0.0236(10) -0.0050(9) -0.0101(9) -0.0064(9) F7 0.0276(6) 0.0476(8) 0.0216(6) 0.0104(5) -0.0106(5) -0.0018(5) C7 0.0277(10) 0.0382(12) 0.0216(10) -0.0072(8) -0.0042(8) 0.0074(9) F8 0.0323(6) 0.0298(6) 0.0332(6) 0.0109(5) -0.0141(5) -0.0098(5) C8 0.0229(10) 0.0317(11) 0.0350(11) -0.0008(9) -0.0038(8) 0.0000(8) F9 0.0481(8) 0.0342(7) 0.0216(6) 0.0009(5) -0.0140(5) -0.0095(6) C9 0.0278(11) 0.0310(11) 0.0430(13) 0.0036(9) -0.0107(9) 0.0018(9) F10 0.0845(12) 0.0560(10) 0.0227(7) -0.0021(6) 0.0080(7) -0.0323(9) C10 0.0247(10) 0.0364(12) 0.0522(14) -0.0112(10) -0.0167(10) 0.0006(9) F11 0.0443(8) 0.0438(8) 0.0542(9) 0.0023(7) -0.0227(7) -0.0207(7) C11 0.0191(8) 0.0219(9) 0.0192(8) 0.0001(7) -0.0075(7) -0.0002(7) F12 0.0479(8) 0.0383(7) 0.0238(6) 0.0044(5) -0.0167(6) -0.0159(6) C12 0.0188(9) 0.0256(9) 0.0251(9) -0.0067(7) -0.0071(7) -0.0004(7) C13 0.0188(9) 0.0381(11) 0.0188(9) -0.0064(8) -0.0089(7) 0.0029(8) C14 0.0173(8) 0.0375(11) 0.0156(8) 0.0028(8) -0.0044(7) 0.0033(8) C15 0.0181(8) 0.0262(9) 0.0207(9) 0.0029(7) -0.0040(7) -0.0029(7) C16 0.0152(8) 0.0216(9) 0.0178(8) -0.0019(7) -0.0045(6) 0.0002(6) C17 0.0242(9) 0.0210(9) 0.0252(9) 0.0017(7) -0.0100(7) -0.0061(7) C18 0.0200(9) 0.0234(9) 0.0270(10) -0.0017(7) -0.0082(7) -0.0045(7) C19 0.0282(10) 0.0241(10) 0.0308(11) -0.0073(8) -0.0097(8) 0.0012(8) C20 0.0260(10) 0.0295(10) 0.0361(11) -0.0046(9) -0.0181(9) -0.0012(8) C21 0.0240(9) 0.0149(8) 0.0211(9) 0.0009(7) -0.0070(7) 0.0022(7) C22 0.0331(10) 0.0190(9) 0.0232(9) -0.0007(7) -0.0087(8) -0.0010(8) C23 0.0445(13) 0.0271(10) 0.0228(10) -0.0004(8) 0.0032(9) -0.0053(9) C24 0.0338(11) 0.0290(11) 0.0399(13) -0.0013(9) 0.0028(10) -0.0100(9) C25 0.0313(11) 0.0224(10) 0.0397(12) 0.0004(8) -0.0129(9) -0.0058(8) C26 0.0307(10) 0.0201(9) 0.0231(9) 0.0007(7) -0.0100(8) -0.0014(7) C27 0.0303(10) 0.0184(9) 0.0247(10) -0.0053(7) -0.0003(8) -0.0029(7) C28 0.0258(10) 0.0199(9) 0.0312(10) -0.0043(8) 0.0007(8) 0.0028(7) C29 0.0261(10) 0.0288(10) 0.0227(9) -0.0042(8) -0.0006(8) -0.0055(8) C30 0.0205(9) 0.0346(11) 0.0365(12) -0.0098(9) -0.0051(8) -0.0014(8) _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 Nd1 N5 2.4092(16) . ? Nd1 N1 2.4163(16) . ? Nd1 N3 2.4827(15) . ? Nd1 F1 2.5793(11) . ? Nd1 F5 2.6138(11) . ? Nd1 N2 2.6870(16) . ? Nd1 N4 2.7273(16) . ? Nd1 N6 2.7782(16) . ? F1 C2 1.372(2) . ? N1 C1 1.358(2) . ? N1 C7 1.471(3) . ? C1 C2 1.406(3) . ? C1 C6 1.413(3) . ? F2 C3 1.345(3) . ? N2 C9 1.466(3) . ? N2 C8 1.466(3) . ? N2 C10 1.491(3) . ? C2 C3 1.369(3) . ? F3 C5 1.354(3) . ? N3 C16 1.358(2) . ? N3 C17 1.468(2) . ? C3 C4 1.380(3) . ? F4 C6 1.357(3) . ? N4 C18 1.472(3) . ? N4 C20 1.474(2) . ? N4 C19 1.475(2) . ? C4 C5 1.371(4) . ? F5 C11 1.373(2) . ? N5 C21 1.368(2) . ? N5 C27 1.465(2) . ? C5 C6 1.378(3) . ? F6 C12 1.345(2) . ? N6 C30 1.477(3) . ? N6 C29 1.479(3) . ? N6 C28 1.487(3) . ? F7 C14 1.354(2) . ? C7 C8 1.529(3) . ? F8 C15 1.355(2) . ? F9 C22 1.353(2) . ? F10 C23 1.346(3) . ? F11 C25 1.354(3) . ? C11 C12 1.364(3) . ? C11 C16 1.410(3) . ? F12 C26 1.350(2) . ? C12 C13 1.381(3) . ? C13 C14 1.371(3) . ? C14 C15 1.381(3) . ? C15 C16 1.417(3) . ? C17 C18 1.511(3) . ? C21 C22 1.403(3) . ? C21 C26 1.413(3) . ? C22 C23 1.372(3) . ? C23 C24 1.372(3) . ? C24 C25 1.371(3) . ? C25 C26 1.373(3) . ? C27 C28 1.508(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Nd1 N1 104.24(6) . . ? N5 Nd1 N3 125.51(5) . . ? N1 Nd1 N3 126.91(5) . . ? N5 Nd1 F1 76.72(5) . . ? N1 Nd1 F1 64.11(5) . . ? N3 Nd1 F1 138.58(5) . . ? N5 Nd1 F5 67.11(5) . . ? N1 Nd1 F5 138.97(5) . . ? N3 Nd1 F5 62.30(4) . . ? F1 Nd1 F5 140.58(4) . . ? N5 Nd1 N2 95.73(5) . . ? N1 Nd1 N2 68.41(5) . . ? N3 Nd1 N2 87.74(5) . . ? F1 Nd1 N2 127.88(5) . . ? F5 Nd1 N2 72.62(4) . . ? N5 Nd1 N4 152.70(5) . . ? N1 Nd1 N4 77.17(5) . . ? N3 Nd1 N4 67.14(5) . . ? F1 Nd1 N4 79.75(4) . . ? F5 Nd1 N4 129.29(4) . . ? N2 Nd1 N4 109.66(5) . . ? N5 Nd1 N6 68.55(5) . . ? N1 Nd1 N6 133.02(5) . . ? N3 Nd1 N6 86.27(5) . . ? F1 Nd1 N6 69.17(4) . . ? F5 Nd1 N6 83.06(4) . . ? N2 Nd1 N6 154.93(5) . . ? N4 Nd1 N6 90.30(5) . . ? C2 F1 Nd1 117.64(11) . . ? C1 N1 C7 117.73(16) . . ? C1 N1 Nd1 122.71(13) . . ? C7 N1 Nd1 119.50(12) . . ? N1 C1 C2 118.30(17) . . ? N1 C1 C6 129.94(19) . . ? C2 C1 C6 111.75(18) . . ? C9 N2 C8 110.88(17) . . ? C9 N2 C10 106.82(17) . . ? C8 N2 C10 107.04(17) . . ? C9 N2 Nd1 108.81(12) . . ? C8 N2 Nd1 106.33(11) . . ? C10 N2 Nd1 116.95(12) . . ? C3 C2 F1 118.28(19) . . ? C3 C2 C1 125.58(19) . . ? F1 C2 C1 116.13(16) . . ? C16 N3 C17 115.72(15) . . ? C16 N3 Nd1 123.86(12) . . ? C17 N3 Nd1 120.41(11) . . ? F2 C3 C2 118.4(2) . . ? F2 C3 C4 120.7(2) . . ? C2 C3 C4 120.9(2) . . ? C18 N4 C20 107.65(15) . . ? C18 N4 C19 110.30(16) . . ? C20 N4 C19 107.50(15) . . ? C18 N4 Nd1 103.75(10) . . ? C20 N4 Nd1 116.30(12) . . ? C19 N4 Nd1 111.20(11) . . ? C5 C4 C3 115.5(2) . . ? C11 F5 Nd1 119.86(10) . . ? C21 N5 C27 114.92(15) . . ? C21 N5 Nd1 123.76(12) . . ? C27 N5 Nd1 114.88(11) . . ? F3 C5 C4 119.5(2) . . ? F3 C5 C6 116.7(2) . . ? C4 C5 C6 123.8(2) . . ? C30 N6 C29 107.23(16) . . ? C30 N6 C28 107.49(16) . . ? C29 N6 C28 109.31(16) . . ? C30 N6 Nd1 120.51(12) . . ? C29 N6 Nd1 107.95(11) . . ? C28 N6 Nd1 104.01(11) . . ? F4 C6 C5 116.8(2) . . ? F4 C6 C1 120.84(19) . . ? C5 C6 C1 122.3(2) . . ? N1 C7 C8 108.80(17) . . ? N2 C8 C7 112.50(17) . . ? C12 C11 F5 118.42(17) . . ? C12 C11 C16 126.12(18) . . ? F5 C11 C16 115.45(15) . . ? F6 C12 C11 118.67(18) . . ? F6 C12 C13 120.27(17) . . ? C11 C12 C13 121.05(19) . . ? C14 C13 C12 115.28(18) . . ? F7 C14 C13 119.06(18) . . ? F7 C14 C15 117.03(19) . . ? C13 C14 C15 123.90(18) . . ? F8 C15 C14 116.42(17) . . ? F8 C15 C16 121.03(17) . . ? C14 C15 C16 122.49(18) . . ? N3 C16 C11 118.04(16) . . ? N3 C16 C15 130.88(17) . . ? C11 C16 C15 111.08(16) . . ? N3 C17 C18 110.12(15) . . ? N4 C18 C17 113.92(15) . . ? N5 C21 C22 120.58(18) . . ? N5 C21 C26 126.17(17) . . ? C22 C21 C26 113.25(18) . . ? F9 C22 C23 118.55(18) . . ? F9 C22 C21 118.10(18) . . ? C23 C22 C21 123.34(19) . . ? F10 C23 C24 119.5(2) . . ? F10 C23 C22 118.5(2) . . ? C24 C23 C22 122.0(2) . . ? C25 C24 C23 116.3(2) . . ? F11 C25 C24 119.0(2) . . ? F11 C25 C26 118.3(2) . . ? C24 C25 C26 122.6(2) . . ? F12 C26 C25 117.62(18) . . ? F12 C26 C21 119.79(17) . . ? C25 C26 C21 122.49(19) . . ? N5 C27 C28 108.37(16) . . ? N6 C28 C27 112.37(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.251 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.068 # Attachment '6 [Nd(p-HC6F4NC2H4NEt2)3].CIF' data_[Nd(p-HC6F4NC2H4NEt2)3].CIF _database_code_depnum_ccdc_archive 'CCDC 859384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(N,N-diethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine -F,N,N'/F,N)-neodymium(iii) ; _chemical_name_common ? _chemical_melting_point 132-140C _chemical_formula_moiety 'C36 H45 F12 N6 Nd' _chemical_formula_sum 'C36 H45 F12 N6 Nd' _chemical_formula_weight 934.02 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 21.120(4) _cell_length_b 10.559(2) _cell_length_c 17.562(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.42(3) _cell_angle_gamma 90.00 _cell_volume 3809.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 10519 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 30.51 _exptl_crystal_description plates _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.457 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8445 _exptl_absorpt_correction_T_max 0.9576 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42892 _diffrn_reflns_av_R_equivalents 0.1969 _diffrn_reflns_av_sigmaI/netI 0.1134 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6723 _reflns_number_gt 4317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Each ethyl group of C23/c24, C33/c34 and C35/c36 displayed disorders and refined with 60%/40% occupancies on two sites respectively. 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. The ethyl groups C33 C34 and C35 C36 were modelled with the terminal carbon atom disordered over two positions. The occupancies were fixed at 0.8:0.2 after trail refinement. The bond C-C distances and the anisotropic thermal parameters of each of the disorder components were restrained for the final refinememnt. ; _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^)+(0.0826P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6723 _refine_ls_number_parameters 522 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.229007(19) 0.63283(4) 0.10031(2) 0.01930(16) Uani 1 1 d . . . F1 F 0.14698(18) 0.7339(4) -0.0217(3) 0.0254(11) Uani 1 1 d . . . N1 N 0.1339(3) 0.7323(6) 0.1250(4) 0.0251(16) Uani 1 1 d . . . C1 C 0.1244(3) 0.7188(7) 0.2056(5) 0.0250(19) Uani 1 1 d . . . H1A H 0.0817 0.6788 0.2036 0.030 Uiso 1 1 calc R . . H1B H 0.1243 0.8037 0.2295 0.030 Uiso 1 1 calc R . . F2 F 0.0516(2) 0.7968(5) -0.1452(3) 0.0399(13) Uani 1 1 d . . . N2 N 0.1884(3) 0.5181(6) 0.2186(3) 0.0194(15) Uani 1 1 d . . . C2 C 0.1772(3) 0.6399(6) 0.2551(4) 0.0221(18) Uani 1 1 d . . . H2A H 0.2181 0.6892 0.2664 0.027 Uiso 1 1 calc R . . H2B H 0.1657 0.6223 0.3056 0.027 Uiso 1 1 calc R . . F3 F -0.0841(2) 0.8962(5) 0.0251(3) 0.0507(15) Uani 1 1 d . . . N3 N 0.3290(3) 0.6747(6) 0.1956(4) 0.0207(15) Uani 1 1 d . . . C3 C 0.0833(3) 0.7762(7) 0.0687(5) 0.0234(19) Uani 1 1 d . . . F4 F 0.0091(2) 0.8428(4) 0.1469(3) 0.0416(13) Uani 1 1 d . . . N4 N 0.2726(3) 0.8665(6) 0.0886(4) 0.0242(15) Uani 1 1 d . . . C4 C 0.0882(3) 0.7741(7) -0.0100(5) 0.0232(19) Uani 1 1 d . . . F5 F 0.30964(19) 0.4430(4) 0.1383(3) 0.0279(11) Uani 1 1 d . . . N5 N 0.2457(3) 0.5336(6) -0.0150(3) 0.0193(14) Uani 1 1 d . A . C5 C 0.0395(4) 0.8060(8) -0.0728(5) 0.031(2) Uani 1 1 d . . . F6 F 0.3916(2) 0.2488(5) 0.1842(3) 0.0434(13) Uani 1 1 d . . . N6 N 0.4040(3) 0.3826(6) -0.0340(4) 0.0294(17) Uani 1 1 d . . . C6 C -0.0204(4) 0.8473(7) -0.0640(6) 0.036(2) Uani 1 1 d . . . H6 H -0.0547 0.8694 -0.1072 0.044 Uiso 1 1 calc R . . F7 F 0.5289(2) 0.5173(5) 0.3631(3) 0.0550(16) Uani 1 1 d . . . C7 C -0.0265(4) 0.8539(8) 0.0110(6) 0.036(2) Uani 1 1 d . . . F8 F 0.4485(2) 0.7068(5) 0.3240(3) 0.0520(15) Uani 1 1 d . . . C8 C 0.0221(4) 0.8247(8) 0.0761(5) 0.030(2) Uani 1 1 d . . . F9 F 0.13185(19) 0.4865(4) 0.0179(3) 0.0292(11) Uani 1 1 d . . . C9 C 0.2363(4) 0.4431(7) 0.2775(5) 0.0255(19) Uani 1 1 d . . . H9A H 0.2216 0.4418 0.3271 0.031 Uiso 1 1 calc R . . H9B H 0.2788 0.4876 0.2880 0.031 Uiso 1 1 calc R . . F10 F 0.0230(2) 0.4399(4) -0.0901(3) 0.0387(13) Uani 1 1 d . A . C10 C 0.2468(4) 0.3080(8) 0.2547(6) 0.042(2) Uani 1 1 d . . . H10A H 0.2088 0.2568 0.2580 0.063 Uiso 1 1 calc R . . H10B H 0.2857 0.2736 0.2904 0.063 Uiso 1 1 calc R . . H10C H 0.2527 0.3061 0.2010 0.063 Uiso 1 1 calc R . . F11 F 0.1419(2) 0.4488(4) -0.2864(3) 0.0392(12) Uani 1 1 d . A . C11 C 0.1264(3) 0.4452(7) 0.1902(5) 0.0224(18) Uani 1 1 d . . . H11A H 0.1365 0.3677 0.1635 0.027 Uiso 1 1 calc R . . H11B H 0.0964 0.4973 0.1508 0.027 Uiso 1 1 calc R . . F12 F 0.2486(2) 0.5062(4) -0.1827(3) 0.0375(12) Uani 1 1 d . . . C12 C 0.0910(4) 0.4061(8) 0.2534(5) 0.035(2) Uani 1 1 d . . . H12A H 0.1191 0.3503 0.2913 0.052 Uiso 1 1 calc R . . H12B H 0.0508 0.3613 0.2290 0.052 Uiso 1 1 calc R . . H12C H 0.0805 0.4819 0.2803 0.052 Uiso 1 1 calc R . . C13 C 0.3438(4) 0.8059(7) 0.2189(5) 0.030(2) Uani 1 1 d . . . H13A H 0.3866 0.8295 0.2090 0.037 Uiso 1 1 calc R . . H13B H 0.3464 0.8153 0.2756 0.037 Uiso 1 1 calc R . . C14 C 0.2934(4) 0.8902(7) 0.1748(5) 0.028(2) Uani 1 1 d U . . H14A H 0.3094 0.9784 0.1829 0.034 Uiso 1 1 calc R . . H14B H 0.2546 0.8834 0.1971 0.034 Uiso 1 1 calc R . . C15 C 0.3751(4) 0.5853(7) 0.2256(5) 0.0242(19) Uani 1 1 d . . . C16 C 0.3659(4) 0.4632(8) 0.1957(5) 0.0265(19) Uani 1 1 d . . . C17 C 0.4070(4) 0.3641(8) 0.2180(5) 0.0295(19) Uani 1 1 d . . . C18 C 0.4631(4) 0.3769(8) 0.2745(5) 0.035(2) Uani 1 1 d . . . H18 H 0.4923 0.3085 0.2908 0.042 Uiso 1 1 calc R . . C19 C 0.4744(4) 0.4965(9) 0.3061(5) 0.037(2) Uani 1 1 d . . . C20 C 0.4327(4) 0.5960(8) 0.2842(5) 0.035(2) Uani 1 1 d . . . C21 C 0.3296(4) 0.8700(7) 0.0529(5) 0.0287(19) Uani 1 1 d . . . H21A H 0.3600 0.8015 0.0761 0.034 Uiso 1 1 calc R . . H21B H 0.3526 0.9516 0.0663 0.034 Uiso 1 1 calc R . . C22 C 0.3124(4) 0.8550(8) -0.0348(5) 0.037(2) Uani 1 1 d . . . H22A H 0.2830 0.7828 -0.0492 0.055 Uiso 1 1 calc R . . H22B H 0.3522 0.8404 -0.0532 0.055 Uiso 1 1 calc R . . H22C H 0.2910 0.9322 -0.0589 0.055 Uiso 1 1 calc R . . C23 C 0.2218(4) 0.9627(7) 0.0498(5) 0.028(2) Uani 1 1 d DU . . H23A H 0.1846 0.9576 0.0752 0.034 Uiso 1 1 calc R . . H23B H 0.2055 0.9381 -0.0057 0.034 Uiso 1 1 calc R . . C24 C 0.2441(4) 1.0991(7) 0.0524(6) 0.043(3) Uani 1 1 d D . . H24A H 0.2573 1.1273 0.1069 0.064 Uiso 1 1 calc R . . H24B H 0.2084 1.1524 0.0241 0.064 Uiso 1 1 calc R . . H24C H 0.2811 1.1061 0.0278 0.064 Uiso 1 1 calc R . . C25 C 0.3137(3) 0.5227(6) -0.0230(5) 0.0229(18) Uani 1 1 d . . . H25A H 0.3429 0.5630 0.0229 0.028 Uiso 1 1 calc R A . H25B H 0.3182 0.5699 -0.0702 0.028 Uiso 1 1 calc R . . C26 C 0.3355(3) 0.3881(7) -0.0294(5) 0.0245(19) Uani 1 1 d . A . H26A H 0.3299 0.3395 0.0168 0.029 Uiso 1 1 calc R . . H26B H 0.3080 0.3484 -0.0767 0.029 Uiso 1 1 calc R . . C27 C 0.1965(3) 0.4980(6) -0.0752(5) 0.0212(18) Uani 1 1 d . . . C28 C 0.1347(4) 0.4745(7) -0.0599(5) 0.0227(18) Uani 1 1 d . A . C29 C 0.0789(4) 0.4519(7) -0.1144(5) 0.029(2) Uani 1 1 d . . . C30 C 0.0786(4) 0.4399(7) -0.1921(5) 0.033(2) Uani 1 1 d . A . H30 H 0.0401 0.4210 -0.2306 0.040 Uiso 1 1 calc R . . C31 C 0.1376(4) 0.4569(7) -0.2106(5) 0.028(2) Uani 1 1 d . . . C32 C 0.1935(4) 0.4830(7) -0.1557(5) 0.0258(19) Uani 1 1 d . A . C33 C 0.4115(4) 0.4099(9) -0.1130(6) 0.045(2) Uani 0.80 1 d PDU A 1 H33A H 0.3855 0.4859 -0.1333 0.053 Uiso 0.80 1 calc PR A 1 H33B H 0.3944 0.3379 -0.1477 0.053 Uiso 0.80 1 calc PR A 1 C34 C 0.4822(5) 0.4326(13) -0.1145(8) 0.059(4) Uani 0.80 1 d PDU A 1 H34A H 0.4850 0.4551 -0.1678 0.089 Uiso 0.80 1 calc PR A 1 H34B H 0.5074 0.3555 -0.0981 0.089 Uiso 0.80 1 calc PR A 1 H34C H 0.4997 0.5020 -0.0788 0.089 Uiso 0.80 1 calc PR A 1 C35 C 0.4341(4) 0.2611(9) -0.0043(6) 0.046(2) Uani 0.80 1 d PU A 1 H35A H 0.4808 0.2664 -0.0049 0.055 Uiso 0.80 1 calc PR A 1 H35B H 0.4319 0.2545 0.0513 0.055 Uiso 0.80 1 calc PR A 1 C36 C 0.4101(6) 0.1460(10) -0.0411(8) 0.052(4) Uani 0.80 1 d P A 1 H36A H 0.4123 0.1485 -0.0962 0.078 Uiso 0.80 1 calc PR A 1 H36B H 0.3648 0.1342 -0.0378 0.078 Uiso 0.80 1 calc PR A 1 H36C H 0.4365 0.0754 -0.0148 0.078 Uiso 0.80 1 calc PR A 1 C33A C 0.4115(4) 0.4099(9) -0.1130(6) 0.045(2) Uani 0.20 1 d P A 2 H33C H 0.3675 0.4222 -0.1470 0.053 Uiso 0.20 1 calc PR A 2 H33D H 0.4303 0.3339 -0.1323 0.053 Uiso 0.20 1 calc PR A 2 C34A C 0.452(2) 0.521(4) -0.124(3) 0.066(16) Uani 0.20 1 d PDU A 2 H34D H 0.4370 0.5960 -0.1003 0.100 Uiso 0.20 1 calc PR A 2 H34E H 0.4479 0.5355 -0.1798 0.100 Uiso 0.20 1 calc PR A 2 H34F H 0.4976 0.5041 -0.0983 0.100 Uiso 0.20 1 calc PR A 2 C35A C 0.4341(4) 0.2611(9) -0.0043(6) 0.046(2) Uani 0.20 1 d PU A 2 H35C H 0.4333 0.2535 0.0517 0.055 Uiso 0.20 1 calc PR A 2 H35D H 0.4072 0.1916 -0.0327 0.055 Uiso 0.20 1 calc PR A 2 C36A C 0.5007(18) 0.244(4) -0.012(3) 0.033(10) Uani 0.20 1 d PU A 2 H36D H 0.5155 0.1586 0.0059 0.049 Uiso 0.20 1 calc PR A 2 H36E H 0.5288 0.3067 0.0209 0.049 Uiso 0.20 1 calc PR A 2 H36F H 0.5026 0.2550 -0.0664 0.049 Uiso 0.20 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0171(2) 0.0220(2) 0.0182(2) -0.0008(2) 0.00283(16) 0.00036(19) F1 0.020(2) 0.028(2) 0.027(3) 0.001(2) 0.004(2) 0.0008(19) N1 0.025(4) 0.020(4) 0.030(4) 0.003(3) 0.006(3) -0.001(3) C1 0.022(4) 0.026(4) 0.027(5) -0.009(4) 0.006(4) -0.005(4) F2 0.042(3) 0.049(3) 0.025(3) 0.014(3) -0.002(2) 0.002(2) N2 0.018(3) 0.026(4) 0.015(4) 0.002(3) 0.004(3) 0.008(3) C2 0.020(4) 0.024(4) 0.023(5) -0.003(4) 0.005(3) -0.005(3) F3 0.019(2) 0.059(3) 0.075(4) 0.015(3) 0.011(3) 0.016(2) N3 0.016(3) 0.021(3) 0.026(4) -0.002(3) 0.007(3) -0.005(3) C3 0.020(4) 0.020(4) 0.031(5) 0.005(4) 0.007(4) 0.004(3) F4 0.032(3) 0.052(3) 0.043(3) 0.005(3) 0.014(2) 0.011(2) N4 0.013(3) 0.029(4) 0.030(4) 0.000(3) 0.003(3) -0.001(3) C4 0.021(4) 0.018(4) 0.029(5) 0.005(4) 0.003(4) 0.001(3) F5 0.028(2) 0.030(3) 0.024(3) -0.002(2) 0.001(2) 0.006(2) N5 0.016(3) 0.030(4) 0.011(4) 0.003(3) 0.002(3) 0.000(3) C5 0.027(5) 0.032(5) 0.033(6) 0.004(4) 0.005(4) 0.000(4) F6 0.054(3) 0.040(3) 0.038(3) 0.008(3) 0.016(3) 0.015(3) N6 0.030(4) 0.031(4) 0.031(4) 0.008(3) 0.014(3) 0.010(3) C6 0.030(5) 0.029(5) 0.041(6) 0.015(4) -0.010(4) 0.003(4) F7 0.027(3) 0.069(4) 0.055(4) 0.023(3) -0.018(3) 0.001(3) C7 0.019(4) 0.043(6) 0.051(7) 0.008(5) 0.015(4) 0.004(4) F8 0.040(3) 0.055(4) 0.048(4) 0.001(3) -0.017(3) -0.009(3) C8 0.027(5) 0.033(5) 0.032(6) 0.007(4) 0.008(4) 0.004(4) F9 0.027(2) 0.035(3) 0.028(3) -0.003(2) 0.009(2) -0.004(2) C9 0.026(4) 0.032(5) 0.019(5) 0.010(4) 0.004(4) -0.001(4) F10 0.024(3) 0.050(3) 0.039(3) -0.001(2) 0.002(2) -0.010(2) C10 0.035(5) 0.043(6) 0.048(7) 0.016(5) 0.010(5) 0.004(4) F11 0.046(3) 0.050(3) 0.019(3) -0.005(2) 0.001(2) 0.000(2) C11 0.018(4) 0.023(4) 0.026(5) -0.009(4) 0.003(4) -0.005(3) F12 0.036(3) 0.053(3) 0.023(3) 0.006(2) 0.006(2) 0.001(2) C12 0.038(5) 0.029(5) 0.038(6) 0.003(4) 0.011(4) -0.003(4) C13 0.033(5) 0.025(5) 0.030(5) 0.001(4) 0.001(4) -0.008(4) C14 0.039(4) 0.015(4) 0.039(5) -0.017(4) 0.027(4) -0.016(3) C15 0.023(4) 0.028(4) 0.022(5) 0.005(4) 0.007(4) -0.004(4) C16 0.022(4) 0.037(5) 0.020(5) 0.008(4) 0.003(4) 0.014(4) C17 0.034(5) 0.035(5) 0.023(5) 0.002(4) 0.013(4) 0.002(4) C18 0.028(5) 0.042(6) 0.039(6) 0.018(5) 0.015(4) 0.013(4) C19 0.021(5) 0.052(6) 0.034(6) 0.021(5) 0.000(4) 0.000(4) C20 0.035(5) 0.038(5) 0.033(6) 0.004(4) 0.007(4) -0.012(4) C21 0.025(4) 0.024(4) 0.036(5) 0.007(4) 0.005(4) -0.001(4) C22 0.042(5) 0.036(5) 0.033(6) -0.004(4) 0.011(4) -0.007(4) C23 0.026(4) 0.023(4) 0.035(5) 0.009(4) 0.006(4) 0.002(3) C24 0.028(5) 0.021(5) 0.067(8) 0.001(5) -0.012(5) 0.004(4) C25 0.028(4) 0.019(4) 0.020(5) 0.004(4) 0.000(4) 0.006(4) C26 0.020(4) 0.030(5) 0.022(5) -0.002(4) 0.004(3) -0.003(4) C27 0.018(4) 0.015(4) 0.029(5) -0.004(4) 0.001(4) -0.002(3) C28 0.024(4) 0.027(5) 0.016(5) 0.004(4) 0.003(4) 0.005(4) C29 0.029(5) 0.025(5) 0.031(6) -0.001(4) 0.006(4) -0.002(4) C30 0.034(5) 0.028(5) 0.032(6) -0.008(4) -0.003(4) 0.000(4) C31 0.039(5) 0.019(4) 0.023(5) -0.005(4) -0.001(4) 0.005(4) C32 0.031(5) 0.024(5) 0.026(5) -0.006(4) 0.013(4) -0.004(4) C33 0.049(5) 0.038(5) 0.056(6) 0.009(4) 0.031(5) 0.015(4) C34 0.067(7) 0.055(7) 0.066(8) -0.016(6) 0.037(6) -0.025(6) C35 0.044(5) 0.048(5) 0.049(5) 0.003(4) 0.019(4) 0.015(4) C36 0.072(9) 0.034(7) 0.062(9) 0.004(7) 0.042(8) 0.006(6) C33A 0.049(5) 0.038(5) 0.056(6) 0.009(4) 0.031(5) 0.015(4) C34A 0.064(18) 0.069(18) 0.065(19) 0.006(10) 0.012(10) 0.004(10) C35A 0.044(5) 0.048(5) 0.049(5) 0.003(4) 0.019(4) 0.015(4) C36A 0.029(13) 0.035(13) 0.032(13) -0.001(9) 0.003(9) 0.007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N5 2.378(6) . ? Nd1 N1 2.395(6) . ? Nd1 N3 2.412(6) . ? Nd1 F5 2.615(4) . ? Nd1 F1 2.647(4) . ? Nd1 N4 2.658(6) . ? Nd1 F9 2.705(4) . ? Nd1 N2 2.709(6) . ? F1 C4 1.372(8) . ? N1 C3 1.357(9) . ? N1 C1 1.480(10) . ? C1 C2 1.497(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? F2 C5 1.357(10) . ? N2 C2 1.481(9) . ? N2 C9 1.495(9) . ? N2 C11 1.501(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? F3 C7 1.371(9) . ? N3 C15 1.371(9) . ? N3 C13 1.458(9) . ? C3 C4 1.411(11) . ? C3 C8 1.424(10) . ? F4 C8 1.348(10) . ? N4 C21 1.481(9) . ? N4 C14 1.496(10) . ? N4 C23 1.520(9) . ? C4 C5 1.363(11) . ? F5 C16 1.385(8) . ? N5 C27 1.351(9) . ? N5 C25 1.481(9) . ? C5 C6 1.381(11) . ? F6 C17 1.360(9) . ? N6 C33 1.460(11) . ? N6 C26 1.469(9) . ? N6 C35 1.472(10) . ? C6 C7 1.354(12) . ? C6 H6 0.9500 . ? F7 C19 1.357(9) . ? C7 C8 1.382(12) . ? F8 C20 1.364(10) . ? F9 C28 1.387(8) . ? C9 C10 1.512(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C29 1.351(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? F11 C31 1.357(9) . ? C11 C12 1.532(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C32 1.376(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.464(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.388(11) . ? C15 C20 1.404(11) . ? C16 C17 1.358(10) . ? C17 C18 1.365(11) . ? C18 C19 1.378(12) . ? C18 H18 0.9500 . ? C19 C20 1.367(11) . ? C21 C22 1.506(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.513(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.506(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.409(10) . ? C27 C28 1.415(10) . ? C28 C29 1.356(10) . ? C29 C30 1.368(11) . ? C30 C31 1.370(11) . ? C30 H30 0.9500 . ? C31 C32 1.369(11) . ? C33 C34 1.518(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.415(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Nd1 N1 130.1(2) . . ? N5 Nd1 N3 113.1(2) . . ? N1 Nd1 N3 115.5(2) . . ? N5 Nd1 F5 70.31(17) . . ? N1 Nd1 F5 144.51(18) . . ? N3 Nd1 F5 63.24(17) . . ? N5 Nd1 F1 71.75(16) . . ? N1 Nd1 F1 63.31(18) . . ? N3 Nd1 F1 142.28(16) . . ? F5 Nd1 F1 141.33(13) . . ? N5 Nd1 N4 102.8(2) . . ? N1 Nd1 N4 85.83(19) . . ? N3 Nd1 N4 67.69(19) . . ? F5 Nd1 N4 120.96(15) . . ? F1 Nd1 N4 74.73(16) . . ? N5 Nd1 F9 62.36(16) . . ? N1 Nd1 F9 77.48(17) . . ? N3 Nd1 F9 155.46(17) . . ? F5 Nd1 F9 93.85(13) . . ? F1 Nd1 F9 61.59(13) . . ? N4 Nd1 F9 136.23(16) . . ? N5 Nd1 N2 126.26(19) . . ? N1 Nd1 N2 68.23(19) . . ? N3 Nd1 N2 86.08(19) . . ? F5 Nd1 N2 76.40(15) . . ? F1 Nd1 N2 122.46(15) . . ? N4 Nd1 N2 130.63(19) . . ? F9 Nd1 N2 79.60(16) . . ? C4 F1 Nd1 116.6(4) . . ? C3 N1 C1 118.1(6) . . ? C3 N1 Nd1 124.7(5) . . ? C1 N1 Nd1 115.8(4) . . ? N1 C1 C2 111.2(6) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C2 N2 C9 108.1(6) . . ? C2 N2 C11 111.9(5) . . ? C9 N2 C11 110.9(6) . . ? C2 N2 Nd1 93.2(4) . . ? C9 N2 Nd1 118.9(4) . . ? C11 N2 Nd1 112.4(4) . . ? N2 C2 C1 113.9(6) . . ? N2 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N2 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C15 N3 C13 117.4(6) . . ? C15 N3 Nd1 124.7(5) . . ? C13 N3 Nd1 117.7(5) . . ? N1 C3 C4 119.0(7) . . ? N1 C3 C8 129.4(8) . . ? C4 C3 C8 111.6(7) . . ? C21 N4 C14 110.3(6) . . ? C21 N4 C23 110.7(6) . . ? C14 N4 C23 110.6(6) . . ? C21 N4 Nd1 112.7(4) . . ? C14 N4 Nd1 95.9(4) . . ? C23 N4 Nd1 115.7(4) . . ? C5 C4 F1 119.6(7) . . ? C5 C4 C3 125.2(7) . . ? F1 C4 C3 115.2(6) . . ? C16 F5 Nd1 117.7(4) . . ? C27 N5 C25 119.3(6) . . ? C27 N5 Nd1 123.4(5) . . ? C25 N5 Nd1 117.0(4) . . ? F2 C5 C4 118.1(7) . . ? F2 C5 C6 120.3(8) . . ? C4 C5 C6 121.7(8) . . ? C33 N6 C26 111.7(6) . . ? C33 N6 C35 112.1(6) . . ? C26 N6 C35 111.4(6) . . ? C7 C6 C5 115.0(8) . . ? C7 C6 H6 122.5 . . ? C5 C6 H6 122.5 . . ? C6 C7 F3 118.8(8) . . ? C6 C7 C8 124.9(8) . . ? F3 C7 C8 116.3(8) . . ? F4 C8 C7 117.4(7) . . ? F4 C8 C3 121.2(7) . . ? C7 C8 C3 121.4(8) . . ? C28 F9 Nd1 112.2(4) . . ? N2 C9 C10 115.7(7) . . ? N2 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? N2 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 115.6(6) . . ? N2 C11 H11A 108.4 . . ? C12 C11 H11A 108.4 . . ? N2 C11 H11B 108.4 . . ? C12 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 110.3(6) . . ? N3 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N3 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 C14 N4 116.1(6) . . ? C13 C14 H14A 108.3 . . ? N4 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? N4 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? N3 C15 C16 118.0(7) . . ? N3 C15 C20 130.0(7) . . ? C16 C15 C20 111.9(7) . . ? C17 C16 C15 125.7(8) . . ? C17 C16 F5 118.2(7) . . ? C15 C16 F5 116.1(6) . . ? C16 C17 C18 121.4(8) . . ? C16 C17 F6 119.6(7) . . ? C18 C17 F6 119.0(7) . . ? C17 C18 C19 115.1(8) . . ? C17 C18 H18 122.5 . . ? C19 C18 H18 122.5 . . ? F7 C19 C20 117.6(8) . . ? F7 C19 C18 118.9(8) . . ? C20 C19 C18 123.5(8) . . ? C19 C20 F8 116.7(8) . . ? C19 C20 C15 122.4(8) . . ? F8 C20 C15 120.8(8) . . ? N4 C21 C22 113.8(6) . . ? N4 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N4 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 116.1(6) . . ? N4 C23 H23A 108.3 . . ? C24 C23 H23A 108.3 . . ? N4 C23 H23B 108.3 . . ? C24 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 113.6(6) . . ? N5 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? N5 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N6 C26 C25 111.3(6) . . ? N6 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? N6 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? N5 C27 C32 131.6(7) . . ? N5 C27 C28 118.4(7) . . ? C32 C27 C28 110.0(6) . . ? C29 C28 F9 118.8(7) . . ? C29 C28 C27 125.9(7) . . ? F9 C28 C27 115.1(6) . . ? F10 C29 C28 118.2(7) . . ? F10 C29 C30 120.3(7) . . ? C28 C29 C30 121.4(8) . . ? C31 C30 C29 115.5(8) . . ? C31 C30 H30 122.2 . . ? C29 C30 H30 122.2 . . ? F11 C31 C32 117.4(7) . . ? F11 C31 C30 119.8(7) . . ? C32 C31 C30 122.8(8) . . ? C31 C32 F12 116.9(7) . . ? C31 C32 C27 124.1(7) . . ? F12 C32 C27 118.7(7) . . ? N6 C33 C34 111.8(9) . . ? N6 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? N6 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C36 C35 N6 120.5(9) . . ? C36 C35 H35A 107.2 . . ? N6 C35 H35A 107.2 . . ? C36 C35 H35B 107.2 . . ? N6 C35 H35B 107.2 . . ? H35A C35 H35B 106.8 . . ? H34D C34A H34E 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? H36D C36A H36E 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.622 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.170 # Attachment 'abs[Nd(p-HC6F4NC2H4NEt2)2F]2.hexane.CIF' data_[Nd(p-HC6F4NC2H4NEt2)2F]2.C6H14.CIF _database_code_depnum_ccdc_archive 'CCDC 859385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(N,N-dimethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine -F,N,N')-bis-fluoro-neodymium(iii) hexane solvate ; _chemical_name_common ; tetrakis(N,N-dimethyl-N'-(2,3,5,6- tetrafluorophenyl)ethylenediamine -F,N,N')-bis-fluoro-neodymium(iii) hexane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C48 H56 F18 N8 Nd2, C6 H14' _chemical_formula_sum 'C54 H70 F18 N8 Nd2' _chemical_formula_weight 1461.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.5793(5) _cell_length_b 22.1566(6) _cell_length_c 28.3427(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11667.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 106787 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 30.52 _exptl_crystal_description rhombus _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 1.856 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6059 _exptl_absorpt_correction_T_max 0.8361 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86431 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13405 _reflns_number_gt 10761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. After refinement of the primary molecule, attempts to model the residual electron density in the lattice voids as disordered hexane solvent gave unsatisfactory refinements. Subsequently, the electron density in voids was accounted for using PLATON/SQUEEZE (see below). ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.254 0.482 -0.003 185 62 2 0.255 0.018 0.497 185 62 3 0.245 0.518 0.497 185 62 4 0.245 0.982 0.997 185 62 5 0.755 0.482 0.503 185 62 6 0.755 0.018 1.003 185 62 7 0.745 0.518 0.003 185 62 8 0.745 0.982 0.503 185 62 _platon_squeeze_details ; Spek, A.L. (1990), Acta Cryst. A46, C-34 ; _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^)+(0.2000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13405 _refine_ls_number_parameters 693 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.538574(8) 0.316629(6) 0.156358(5) 0.01828(4) Uani 1 1 d . . . F1 F 0.50176(8) 0.30072(7) 0.24607(5) 0.0268(3) Uani 1 1 d . . . N1 N 0.61357(11) 0.36293(10) 0.21643(7) 0.0240(5) Uani 1 1 d . . . C1 C 0.59940(14) 0.36397(12) 0.26352(9) 0.0243(6) Uani 1 1 d . . . Nd2 Nd 0.429001(8) 0.171283(6) 0.153046(5) 0.01905(4) Uani 1 1 d . . . F2 F 0.45946(10) 0.29523(8) 0.33641(6) 0.0386(4) Uani 1 1 d . . . N2 N 0.68223(12) 0.30124(10) 0.14171(7) 0.0240(5) Uani 1 1 d . . . C2 C 0.63600(15) 0.39338(13) 0.30040(10) 0.0291(6) Uani 1 1 d . . . F3 F 0.65453(10) 0.41854(9) 0.37916(6) 0.0488(5) Uani 1 1 d . . . N3 N 0.53654(12) 0.37870(10) 0.08628(8) 0.0255(5) Uani 1 1 d . . . C3 C 0.61541(16) 0.38818(14) 0.34668(10) 0.0337(7) Uani 1 1 d . . . F4 F 0.69302(10) 0.43003(8) 0.29103(6) 0.0451(5) Uani 1 1 d . . . N4 N 0.45354(12) 0.41279(10) 0.16589(8) 0.0235(5) Uani 1 1 d . . . C4 C 0.55677(16) 0.35577(14) 0.36129(10) 0.0323(7) Uani 1 1 d . . . H4 H 0.5434 0.3529 0.3936 0.039 Uiso 1 1 calc R . . F5 F 0.55055(8) 0.26182(7) 0.07409(5) 0.0281(4) Uani 1 1 d . . . N5 N 0.43414(12) 0.11457(10) 0.07974(8) 0.0270(5) Uani 1 1 d . . . C5 C 0.51843(16) 0.32751(13) 0.32576(10) 0.0284(6) Uani 1 1 d . . . F6 F 0.57192(10) 0.20874(8) -0.01012(6) 0.0436(5) Uani 1 1 d . . . N6 N 0.51888(12) 0.07738(10) 0.15751(8) 0.0251(5) Uani 1 1 d . . . C6 C 0.53976(15) 0.33140(12) 0.28008(10) 0.0252(6) Uani 1 1 d . . . F7 F 0.55961(11) 0.39878(10) -0.08324(6) 0.0563(6) Uani 1 1 d . . . N8 N 0.28462(12) 0.18396(10) 0.14038(8) 0.0244(5) Uani 1 1 d . . . C7 C 0.68521(15) 0.38380(13) 0.20231(9) 0.0298(6) Uani 1 1 d . . . H7A H 0.7220 0.3661 0.2235 0.036 Uiso 1 1 calc R . . H7B H 0.6878 0.4283 0.2051 0.036 Uiso 1 1 calc R . . F8 F 0.54108(11) 0.45124(9) -0.00268(6) 0.0518(5) Uani 1 1 d . . . N7 N 0.35635(12) 0.11573(10) 0.20950(8) 0.0252(5) Uani 1 1 d . . . C8 C 0.70038(15) 0.36518(13) 0.15169(9) 0.0284(6) Uani 1 1 d . . . H8A H 0.6723 0.3914 0.1302 0.034 Uiso 1 1 calc R . . H8B H 0.7521 0.3718 0.1449 0.034 Uiso 1 1 calc R . . F9 F 0.54261(8) 0.21380(7) 0.16126(5) 0.0227(3) Uani 1 1 d . . . C9 C 0.71250(15) 0.25814(13) 0.17744(10) 0.0307(6) Uani 1 1 d . . . F10 F 0.42445(8) 0.27413(7) 0.16220(5) 0.0225(3) Uani 1 1 d . . . C10 C 0.79424(16) 0.25737(15) 0.18080(11) 0.0412(8) Uani 1 1 d . . . H10A H 0.8145 0.2418 0.1513 0.062 Uiso 1 1 calc R . . H10B H 0.8090 0.2314 0.2070 0.062 Uiso 1 1 calc R . . H10C H 0.8119 0.2985 0.1862 0.062 Uiso 1 1 calc R . . F11 F 0.41252(8) 0.23165(7) 0.07453(5) 0.0281(4) Uani 1 1 d . . . C11 C 0.70892(16) 0.28895(14) 0.09273(10) 0.0346(7) Uani 1 1 d . . . F12 F 0.38771(10) 0.29146(8) -0.00602(6) 0.0421(4) Uani 1 1 d . . . C12 C 0.70450(18) 0.22225(15) 0.07866(11) 0.0482(9) Uani 1 1 d . . . H12A H 0.7392 0.1989 0.0972 0.072 Uiso 1 1 calc R . . H12B H 0.7156 0.2181 0.0450 0.072 Uiso 1 1 calc R . . H12C H 0.6558 0.2071 0.0847 0.072 Uiso 1 1 calc R . . F13 F 0.41032(11) 0.10975(9) -0.09045(6) 0.0535(5) Uani 1 1 d . . . C13 C 0.54425(14) 0.35874(13) 0.04125(9) 0.0271(6) Uani 1 1 d . . . F14 F 0.43586(12) 0.05004(9) -0.01291(6) 0.0525(5) Uani 1 1 d . . . C14 C 0.55307(15) 0.29673(13) 0.03401(9) 0.0271(6) Uani 1 1 d . . . F15 F 0.46281(8) 0.18006(7) 0.24373(5) 0.0289(4) Uani 1 1 d . . . C15 C 0.56359(16) 0.26872(15) -0.00883(10) 0.0351(7) Uani 1 1 d . . . F16 F 0.50627(10) 0.17601(8) 0.33403(6) 0.0410(5) Uani 1 1 d . . . C16 C 0.56482(16) 0.30177(16) -0.04995(11) 0.0400(8) Uani 1 1 d . . . H16 H 0.5710 0.2835 -0.0800 0.048 Uiso 1 1 calc R . . F17 F 0.32125(10) 0.03693(9) 0.36667(7) 0.0553(5) Uani 1 1 d . . . C17 C 0.55660(16) 0.36244(17) -0.04451(10) 0.0392(8) Uani 1 1 d . . . F18 F 0.28019(9) 0.03761(8) 0.27852(6) 0.0436(5) Uani 1 1 d . . . C18 C 0.54641(16) 0.39085(14) -0.00170(10) 0.0337(7) Uani 1 1 d . . . C19 C 0.51987(15) 0.44275(12) 0.09285(9) 0.0284(6) Uani 1 1 d . . . H19A H 0.4772 0.4536 0.0737 0.034 Uiso 1 1 calc R . . H19B H 0.5609 0.4676 0.0820 0.034 Uiso 1 1 calc R . . C20 C 0.50515(15) 0.45556(12) 0.14400(9) 0.0269(6) Uani 1 1 d . . . H20A H 0.5511 0.4539 0.1616 0.032 Uiso 1 1 calc R . . H20B H 0.4858 0.4970 0.1470 0.032 Uiso 1 1 calc R . . C21 C 0.44076(15) 0.43302(13) 0.21533(10) 0.0292(6) Uani 1 1 d . . . H21A H 0.4267 0.4761 0.2149 0.035 Uiso 1 1 calc R . . H21B H 0.4864 0.4297 0.2332 0.035 Uiso 1 1 calc R . . C22 C 0.38274(16) 0.39715(14) 0.24111(10) 0.0368(7) Uani 1 1 d . . . H22A H 0.3353 0.4087 0.2290 0.055 Uiso 1 1 calc R . . H22B H 0.3852 0.4058 0.2750 0.055 Uiso 1 1 calc R . . H22C H 0.3905 0.3539 0.2359 0.055 Uiso 1 1 calc R . . C23 C 0.38527(14) 0.40896(13) 0.13859(10) 0.0286(6) Uani 1 1 d . . . H23A H 0.3542 0.3779 0.1533 0.034 Uiso 1 1 calc R . . H23B H 0.3967 0.3953 0.1062 0.034 Uiso 1 1 calc R . . C24 C 0.34274(17) 0.46787(14) 0.13544(11) 0.0392(7) Uani 1 1 d . . . H24A H 0.3289 0.4809 0.1672 0.059 Uiso 1 1 calc R . . H24B H 0.2994 0.4615 0.1164 0.059 Uiso 1 1 calc R . . H24C H 0.3727 0.4990 0.1207 0.059 Uiso 1 1 calc R . . C25 C 0.42453(14) 0.13818(13) 0.03601(9) 0.0273(6) Uani 1 1 d . . . C26 C 0.41165(14) 0.20081(13) 0.03228(9) 0.0275(6) Uani 1 1 d . . . C27 C 0.39896(16) 0.23143(14) -0.00822(10) 0.0334(7) Uani 1 1 d . . . C28 C 0.39927(16) 0.20225(16) -0.05122(10) 0.0384(8) Uani 1 1 d . . . H28 H 0.3915 0.2231 -0.0801 0.046 Uiso 1 1 calc R . . C29 C 0.41140(17) 0.14193(16) -0.04962(10) 0.0384(8) Uani 1 1 d . . . C30 C 0.42473(16) 0.11022(14) -0.00843(10) 0.0340(7) Uani 1 1 d . . . C31 C 0.45528(16) 0.05101(12) 0.08280(10) 0.0317(7) Uani 1 1 d . . . H31A H 0.4986 0.0441 0.0632 0.038 Uiso 1 1 calc R . . H31B H 0.4160 0.0253 0.0704 0.038 Uiso 1 1 calc R . . C32 C 0.47117(15) 0.03371(12) 0.13350(10) 0.0290(6) Uani 1 1 d . . . H32A H 0.4253 0.0309 0.1511 0.035 Uiso 1 1 calc R . . H32B H 0.4941 -0.0066 0.1340 0.035 Uiso 1 1 calc R . . C33 C 0.58683(15) 0.08803(13) 0.13077(11) 0.0320(7) Uani 1 1 d . . . H33A H 0.6148 0.1197 0.1473 0.038 Uiso 1 1 calc R . . H33B H 0.5742 0.1040 0.0992 0.038 Uiso 1 1 calc R . . C34 C 0.63517(17) 0.03290(14) 0.12426(13) 0.0471(9) Uani 1 1 d . . . H34A H 0.6486 0.0168 0.1552 0.071 Uiso 1 1 calc R . . H34B H 0.6787 0.0446 0.1070 0.071 Uiso 1 1 calc R . . H34C H 0.6092 0.0019 0.1064 0.071 Uiso 1 1 calc R . . C35 C 0.53406(15) 0.05403(12) 0.20557(10) 0.0293(6) Uani 1 1 d . . . H35A H 0.5520 0.0121 0.2029 0.035 Uiso 1 1 calc R . . H35B H 0.4884 0.0528 0.2236 0.035 Uiso 1 1 calc R . . C36 C 0.58872(17) 0.09107(13) 0.23327(11) 0.0375(7) Uani 1 1 d . . . H36A H 0.6373 0.0823 0.2216 0.056 Uiso 1 1 calc R . . H36B H 0.5856 0.0806 0.2668 0.056 Uiso 1 1 calc R . . H36C H 0.5784 0.1341 0.2292 0.056 Uiso 1 1 calc R . . C37 C 0.37003(14) 0.11002(12) 0.25622(9) 0.0245(6) Uani 1 1 d . . . C38 C 0.42745(14) 0.14318(12) 0.27510(9) 0.0257(6) Uani 1 1 d . . . C39 C 0.44944(15) 0.14224(14) 0.32112(10) 0.0304(7) Uani 1 1 d . . . C40 C 0.41306(17) 0.10723(15) 0.35404(10) 0.0376(8) Uani 1 1 d . . . H40 H 0.4264 0.1064 0.3864 0.045 Uiso 1 1 calc R . . C41 C 0.35704(17) 0.07417(15) 0.33690(11) 0.0367(7) Uani 1 1 d . . . C42 C 0.33517(15) 0.07424(13) 0.29044(10) 0.0315(7) Uani 1 1 d . . . C43 C 0.28621(15) 0.09301(12) 0.19270(10) 0.0298(6) Uani 1 1 d . . . H43A H 0.2479 0.1051 0.2150 0.036 Uiso 1 1 calc R . . H43B H 0.2873 0.0484 0.1912 0.036 Uiso 1 1 calc R . . C44 C 0.27011(15) 0.11834(12) 0.14427(9) 0.0283(6) Uani 1 1 d . . . H44A H 0.2997 0.0967 0.1206 0.034 Uiso 1 1 calc R . . H44B H 0.2189 0.1108 0.1367 0.034 Uiso 1 1 calc R . . C45 C 0.25122(15) 0.21892(13) 0.17938(10) 0.0294(6) Uani 1 1 d . . . H45A H 0.2655 0.2617 0.1759 0.035 Uiso 1 1 calc R . . H45B H 0.2715 0.2043 0.2096 0.035 Uiso 1 1 calc R . . C46 C 0.16994(16) 0.21610(14) 0.18269(11) 0.0381(7) Uani 1 1 d . . . H46A H 0.1487 0.2356 0.1549 0.057 Uiso 1 1 calc R . . H46B H 0.1540 0.2371 0.2113 0.057 Uiso 1 1 calc R . . H46C H 0.1545 0.1738 0.1840 0.057 Uiso 1 1 calc R . . C47 C 0.25662(15) 0.20415(14) 0.09420(10) 0.0335(7) Uani 1 1 d . . . H47A H 0.2060 0.1908 0.0914 0.040 Uiso 1 1 calc R . . H47B H 0.2843 0.1836 0.0691 0.040 Uiso 1 1 calc R . . C48 C 0.25947(18) 0.27160(14) 0.08521(11) 0.0448(8) Uani 1 1 d . . . H48A H 0.2205 0.2915 0.1026 0.067 Uiso 1 1 calc R . . H48B H 0.2538 0.2794 0.0514 0.067 Uiso 1 1 calc R . . H48C H 0.3059 0.2875 0.0959 0.067 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 Nd1 0.01757(8) 0.01763(8) 0.01965(8) -0.00076(5) 0.00054(5) -0.00142(5) F1 0.0254(9) 0.0314(9) 0.0235(8) -0.0043(6) -0.0002(6) -0.0070(7) N1 0.0222(12) 0.0249(12) 0.0250(12) -0.0033(9) 0.0005(9) -0.0023(10) C1 0.0228(14) 0.0222(14) 0.0279(14) -0.0041(11) -0.0030(11) 0.0035(11) Nd2 0.01833(8) 0.01793(8) 0.02091(8) 0.00017(5) -0.00142(5) -0.00178(5) F2 0.0368(10) 0.0487(11) 0.0301(9) -0.0030(8) 0.0088(7) -0.0059(9) N2 0.0188(12) 0.0299(13) 0.0235(12) -0.0034(9) 0.0022(9) 0.0014(10) C2 0.0239(15) 0.0302(16) 0.0331(16) -0.0065(12) -0.0044(12) -0.0016(12) F3 0.0430(11) 0.0675(13) 0.0359(10) -0.0218(9) -0.0130(8) -0.0004(10) N3 0.0250(12) 0.0251(12) 0.0264(12) 0.0027(10) -0.0003(9) 0.0017(10) C3 0.0312(17) 0.0409(18) 0.0290(16) -0.0158(13) -0.0108(12) 0.0082(14) F4 0.0399(11) 0.0501(12) 0.0454(11) -0.0166(9) -0.0019(8) -0.0179(9) N4 0.0208(12) 0.0224(12) 0.0274(12) -0.0015(9) 0.0021(9) -0.0003(9) C4 0.0342(17) 0.0399(18) 0.0229(15) -0.0030(13) 0.0014(12) 0.0094(14) F5 0.0317(9) 0.0288(9) 0.0237(8) -0.0016(7) 0.0017(7) 0.0003(7) N5 0.0295(13) 0.0261(13) 0.0254(12) -0.0029(10) -0.0002(10) -0.0032(10) C5 0.0269(15) 0.0310(16) 0.0275(15) -0.0021(12) 0.0013(12) 0.0030(12) F6 0.0451(11) 0.0476(12) 0.0381(10) -0.0153(9) 0.0077(8) -0.0047(9) N6 0.0201(12) 0.0207(12) 0.0347(13) -0.0008(10) -0.0026(9) -0.0015(9) C6 0.0237(14) 0.0267(15) 0.0252(14) -0.0080(11) -0.0051(11) 0.0024(12) F7 0.0553(13) 0.0880(16) 0.0257(10) 0.0188(10) -0.0056(9) -0.0224(11) N8 0.0221(12) 0.0276(13) 0.0234(11) 0.0010(9) -0.0028(9) -0.0018(10) C7 0.0250(15) 0.0307(16) 0.0336(16) -0.0057(12) 0.0007(12) -0.0103(12) F8 0.0612(14) 0.0534(13) 0.0407(11) 0.0183(9) 0.0021(9) 0.0017(10) N7 0.0213(12) 0.0235(12) 0.0306(13) 0.0028(10) -0.0013(9) -0.0028(10) C8 0.0223(14) 0.0308(16) 0.0320(16) 0.0015(12) 0.0027(11) -0.0064(12) F9 0.0189(8) 0.0206(8) 0.0285(8) 0.0005(6) -0.0002(6) 0.0001(6) C9 0.0216(15) 0.0382(17) 0.0323(16) 0.0066(13) -0.0011(12) 0.0062(13) F10 0.0200(8) 0.0207(8) 0.0268(8) -0.0005(6) -0.0001(6) -0.0019(6) C10 0.0305(17) 0.055(2) 0.0381(18) 0.0078(15) 0.0010(14) 0.0149(15) F11 0.0303(9) 0.0303(9) 0.0237(8) 0.0001(7) -0.0010(7) 0.0009(7) C11 0.0312(17) 0.0456(19) 0.0270(16) -0.0068(13) 0.0105(12) 0.0000(14) F12 0.0441(11) 0.0479(12) 0.0344(10) 0.0136(8) -0.0019(8) 0.0066(9) C12 0.0366(19) 0.065(2) 0.043(2) -0.0183(17) 0.0009(15) 0.0136(17) F13 0.0629(14) 0.0733(14) 0.0244(10) -0.0123(9) 0.0043(9) -0.0252(11) C13 0.0194(14) 0.0394(17) 0.0225(14) 0.0043(12) -0.0011(11) -0.0030(12) F14 0.0770(15) 0.0460(12) 0.0346(11) -0.0141(9) 0.0050(9) -0.0100(11) C14 0.0224(14) 0.0369(17) 0.0221(14) 0.0040(12) 0.0012(11) -0.0030(12) F15 0.0291(9) 0.0309(9) 0.0266(8) 0.0056(7) -0.0017(7) -0.0079(7) C15 0.0249(16) 0.053(2) 0.0274(16) -0.0054(14) 0.0043(12) -0.0068(14) F16 0.0403(11) 0.0509(12) 0.0317(9) 0.0019(8) -0.0096(8) -0.0048(9) C16 0.0279(17) 0.066(2) 0.0261(16) -0.0032(15) 0.0018(12) -0.0127(16) F17 0.0398(11) 0.0773(15) 0.0488(12) 0.0347(11) 0.0083(9) -0.0024(10) C17 0.0257(16) 0.070(3) 0.0222(15) 0.0113(15) -0.0023(12) -0.0157(16) F18 0.0337(10) 0.0427(11) 0.0544(12) 0.0202(9) 0.0013(8) -0.0094(9) C18 0.0292(16) 0.0404(19) 0.0316(16) 0.0100(14) -0.0020(12) -0.0057(14) C19 0.0273(15) 0.0260(15) 0.0318(16) 0.0077(12) 0.0024(12) -0.0015(12) C20 0.0261(15) 0.0171(14) 0.0376(16) 0.0014(11) 0.0013(12) -0.0003(11) C21 0.0318(16) 0.0262(15) 0.0297(15) -0.0022(12) -0.0010(12) 0.0050(12) C22 0.0315(17) 0.0415(19) 0.0374(18) 0.0015(14) 0.0087(13) 0.0051(14) C23 0.0204(14) 0.0317(16) 0.0337(15) 0.0020(12) -0.0032(12) 0.0015(12) C24 0.0299(17) 0.0391(18) 0.0485(19) 0.0056(15) -0.0003(14) 0.0059(14) C25 0.0223(14) 0.0349(16) 0.0248(14) -0.0044(12) 0.0004(11) -0.0082(12) C26 0.0220(14) 0.0383(17) 0.0223(14) -0.0016(12) -0.0014(11) -0.0008(12) C27 0.0244(15) 0.047(2) 0.0288(16) 0.0056(13) -0.0007(12) -0.0024(14) C28 0.0299(17) 0.065(2) 0.0205(15) 0.0065(14) 0.0001(12) -0.0106(16) C29 0.0322(17) 0.058(2) 0.0247(16) -0.0079(14) 0.0034(12) -0.0163(16) C30 0.0336(17) 0.0376(18) 0.0307(16) -0.0092(13) 0.0031(13) -0.0116(14) C31 0.0375(17) 0.0245(15) 0.0330(16) -0.0082(12) -0.0001(13) -0.0030(13) C32 0.0297(16) 0.0201(14) 0.0372(16) -0.0033(12) -0.0029(13) -0.0018(12) C33 0.0267(16) 0.0318(16) 0.0376(17) -0.0040(13) 0.0013(13) 0.0005(13) C34 0.0337(19) 0.041(2) 0.066(2) -0.0089(17) 0.0058(16) 0.0071(15) C35 0.0316(16) 0.0214(14) 0.0350(16) 0.0032(12) -0.0046(12) 0.0049(12) C36 0.0358(18) 0.0327(17) 0.0440(19) -0.0017(14) -0.0109(14) 0.0052(14) C37 0.0218(14) 0.0233(14) 0.0284(15) 0.0042(11) 0.0025(11) 0.0054(11) C38 0.0260(15) 0.0250(15) 0.0260(14) 0.0055(11) 0.0055(11) 0.0028(12) C39 0.0258(15) 0.0375(17) 0.0280(15) 0.0031(13) -0.0009(12) 0.0051(13) C40 0.0373(18) 0.049(2) 0.0263(16) 0.0114(14) 0.0039(13) 0.0112(15) C41 0.0283(16) 0.0442(19) 0.0376(18) 0.0192(14) 0.0094(13) 0.0076(14) C42 0.0232(15) 0.0296(16) 0.0418(18) 0.0095(13) 0.0055(12) 0.0020(12) C43 0.0233(15) 0.0253(15) 0.0409(17) 0.0023(12) 0.0013(12) -0.0048(12) C44 0.0226(15) 0.0285(16) 0.0338(16) -0.0053(12) -0.0029(12) -0.0051(12) C45 0.0266(15) 0.0312(16) 0.0304(16) -0.0002(12) -0.0021(12) 0.0031(13) C46 0.0286(17) 0.0466(19) 0.0389(18) 0.0014(15) 0.0027(13) 0.0071(15) C47 0.0225(15) 0.0490(19) 0.0292(16) 0.0028(14) -0.0041(12) 0.0009(14) C48 0.0369(19) 0.051(2) 0.047(2) 0.0215(16) 0.0005(15) 0.0110(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 F9 2.2838(15) . ? Nd1 F10 2.3260(14) . ? Nd1 N3 2.416(2) . ? Nd1 N1 2.428(2) . ? Nd1 F5 2.6384(15) . ? Nd1 F1 2.6565(14) . ? Nd1 N4 2.666(2) . ? Nd1 N2 2.723(2) . ? Nd1 Nd2 3.8110(2) . ? F1 C6 1.375(3) . ? N1 C1 1.360(3) . ? N1 C7 1.465(3) . ? C1 C6 1.403(4) . ? C1 C2 1.407(4) . ? Nd2 F10 2.2950(15) . ? Nd2 F9 2.3232(15) . ? Nd2 N7 2.428(2) . ? Nd2 N5 2.430(2) . ? Nd2 F11 2.6144(15) . ? Nd2 F15 2.6531(15) . ? Nd2 N6 2.671(2) . ? Nd2 N8 2.721(2) . ? F2 C5 1.343(3) . ? N2 C8 1.483(3) . ? N2 C11 1.499(3) . ? N2 C9 1.501(3) . ? C2 F4 1.361(3) . ? C2 C3 1.371(4) . ? F3 C3 1.352(3) . ? N3 C13 1.358(3) . ? N3 C19 1.464(3) . ? C3 C4 1.369(4) . ? N4 C20 1.484(3) . ? N4 C23 1.488(3) . ? N4 C21 1.490(3) . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? F5 C14 1.375(3) . ? N5 C25 1.357(3) . ? N5 C31 1.465(3) . ? C5 C6 1.357(4) . ? F6 C15 1.338(4) . ? N6 C32 1.478(3) . ? N6 C35 1.484(3) . ? N6 C33 1.491(3) . ? F7 C17 1.363(3) . ? N8 C47 1.478(3) . ? N8 C44 1.483(3) . ? N8 C45 1.486(3) . ? C7 C8 1.519(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? F8 C18 1.342(4) . ? N7 C37 1.354(3) . ? N7 C43 1.476(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.522(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? F11 C26 1.379(3) . ? C11 C12 1.533(4) . ? F12 C27 1.348(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? F13 C29 1.359(3) . ? C13 C14 1.399(4) . ? C13 C18 1.411(4) . ? F14 C30 1.355(4) . ? C14 C15 1.378(4) . ? F15 C38 1.375(3) . ? C15 C16 1.377(4) . ? F16 C39 1.345(3) . ? C16 C17 1.362(5) . ? C16 H16 0.9500 . ? F17 C41 1.354(3) . ? C17 C18 1.380(4) . ? F18 C42 1.348(3) . ? C19 C20 1.503(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.526(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.528(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.404(4) . ? C25 C26 1.412(4) . ? C26 C27 1.354(4) . ? C27 C28 1.380(4) . ? C28 C29 1.356(5) . ? C28 H28 0.9500 . ? C29 C30 1.385(4) . ? C31 C32 1.516(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.527(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.524(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.401(4) . ? C37 C42 1.410(4) . ? C38 C39 1.367(4) . ? C39 C40 1.389(4) . ? C40 C41 1.362(5) . ? C40 H40 0.9500 . ? C41 C42 1.378(4) . ? C43 C44 1.513(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.514(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.517(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F9 Nd1 F10 67.78(5) . . ? F9 Nd1 N3 128.20(6) . . ? F10 Nd1 N3 105.94(6) . . ? F9 Nd1 N1 111.10(6) . . ? F10 Nd1 N1 130.12(6) . . ? N3 Nd1 N1 110.18(7) . . ? F9 Nd1 F5 65.91(5) . . ? F10 Nd1 F5 87.33(5) . . ? N3 Nd1 F5 62.40(6) . . ? N1 Nd1 F5 140.00(6) . . ? F9 Nd1 F1 79.51(5) . . ? F10 Nd1 F1 69.11(5) . . ? N3 Nd1 F1 149.13(6) . . ? N1 Nd1 F1 62.13(6) . . ? F5 Nd1 F1 143.76(5) . . ? F9 Nd1 N4 144.15(6) . . ? F10 Nd1 N4 77.06(6) . . ? N3 Nd1 N4 67.62(7) . . ? N1 Nd1 N4 86.06(7) . . ? F5 Nd1 N4 120.48(6) . . ? F1 Nd1 N4 81.75(6) . . ? F9 Nd1 N2 81.50(6) . . ? F10 Nd1 N2 148.63(6) . . ? N3 Nd1 N2 87.78(7) . . ? N1 Nd1 N2 66.24(7) . . ? F5 Nd1 N2 74.04(6) . . ? F1 Nd1 N2 112.44(6) . . ? N4 Nd1 N2 134.14(7) . . ? F9 Nd1 Nd2 34.52(4) . . ? F10 Nd1 Nd2 34.18(4) . . ? N3 Nd1 Nd2 116.90(5) . . ? N1 Nd1 Nd2 132.92(5) . . ? F5 Nd1 Nd2 68.55(3) . . ? F1 Nd1 Nd2 76.94(3) . . ? N4 Nd1 Nd2 111.18(5) . . ? N2 Nd1 Nd2 114.46(5) . . ? C6 F1 Nd1 118.25(15) . . ? C1 N1 C7 116.0(2) . . ? C1 N1 Nd1 125.74(17) . . ? C7 N1 Nd1 117.60(16) . . ? N1 C1 C6 118.2(2) . . ? N1 C1 C2 130.0(3) . . ? C6 C1 C2 111.8(2) . . ? F10 Nd2 F9 67.64(5) . . ? F10 Nd2 N7 114.09(6) . . ? F9 Nd2 N7 130.13(6) . . ? F10 Nd2 N5 127.70(6) . . ? F9 Nd2 N5 105.05(6) . . ? N7 Nd2 N5 108.85(7) . . ? F10 Nd2 F11 65.41(5) . . ? F9 Nd2 F11 89.10(5) . . ? N7 Nd2 F11 139.03(6) . . ? N5 Nd2 F11 62.70(6) . . ? F10 Nd2 F15 80.01(5) . . ? F9 Nd2 F15 70.00(5) . . ? N7 Nd2 F15 61.99(6) . . ? N5 Nd2 F15 148.97(6) . . ? F11 Nd2 F15 144.58(5) . . ? F10 Nd2 N6 142.29(6) . . ? F9 Nd2 N6 75.11(6) . . ? N7 Nd2 N6 85.50(7) . . ? N5 Nd2 N6 67.24(7) . . ? F11 Nd2 N6 120.80(6) . . ? F15 Nd2 N6 82.14(6) . . ? F10 Nd2 N8 82.88(6) . . ? F9 Nd2 N8 150.13(6) . . ? N7 Nd2 N8 65.87(7) . . ? N5 Nd2 N8 88.82(7) . . ? F11 Nd2 N8 73.71(6) . . ? F15 Nd2 N8 110.71(6) . . ? N6 Nd2 N8 134.67(7) . . ? F10 Nd2 Nd1 34.70(4) . . ? F9 Nd2 Nd1 33.85(4) . . ? N7 Nd2 Nd1 135.15(5) . . ? N5 Nd2 Nd1 115.92(5) . . ? F11 Nd2 Nd1 69.59(3) . . ? F15 Nd2 Nd1 77.74(3) . . ? N6 Nd2 Nd1 108.85(5) . . ? N8 Nd2 Nd1 116.28(5) . . ? C8 N2 C11 106.0(2) . . ? C8 N2 C9 113.2(2) . . ? C11 N2 C9 112.7(2) . . ? C8 N2 Nd1 94.25(15) . . ? C11 N2 Nd1 119.22(16) . . ? C9 N2 Nd1 110.12(15) . . ? F4 C2 C3 117.0(2) . . ? F4 C2 C1 120.5(2) . . ? C3 C2 C1 122.5(3) . . ? C13 N3 C19 117.2(2) . . ? C13 N3 Nd1 125.83(18) . . ? C19 N3 Nd1 116.77(16) . . ? F3 C3 C4 118.9(3) . . ? F3 C3 C2 117.4(3) . . ? C4 C3 C2 123.7(3) . . ? C20 N4 C23 111.7(2) . . ? C20 N4 C21 107.7(2) . . ? C23 N4 C21 111.7(2) . . ? C20 N4 Nd1 94.88(15) . . ? C23 N4 Nd1 114.00(16) . . ? C21 N4 Nd1 115.47(16) . . ? C3 C4 C5 115.3(3) . . ? C3 C4 H4 122.4 . . ? C5 C4 H4 122.4 . . ? C14 F5 Nd1 118.30(15) . . ? C25 N5 C31 117.4(2) . . ? C25 N5 Nd2 125.19(18) . . ? C31 N5 Nd2 117.20(16) . . ? F2 C5 C6 119.1(3) . . ? F2 C5 C4 119.8(3) . . ? C6 C5 C4 121.0(3) . . ? C32 N6 C35 107.9(2) . . ? C32 N6 C33 112.2(2) . . ? C35 N6 C33 111.2(2) . . ? C32 N6 Nd2 96.50(15) . . ? C35 N6 Nd2 115.71(16) . . ? C33 N6 Nd2 112.46(16) . . ? C5 C6 F1 119.2(2) . . ? C5 C6 C1 125.6(3) . . ? F1 C6 C1 115.2(2) . . ? C47 N8 C44 107.4(2) . . ? C47 N8 C45 110.7(2) . . ? C44 N8 C45 112.3(2) . . ? C47 N8 Nd2 119.68(17) . . ? C44 N8 Nd2 93.91(15) . . ? C45 N8 Nd2 111.56(15) . . ? N1 C7 C8 109.9(2) . . ? N1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C37 N7 C43 116.7(2) . . ? C37 N7 Nd2 125.97(17) . . ? C43 N7 Nd2 116.80(16) . . ? N2 C8 C7 113.4(2) . . ? N2 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? N2 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? Nd1 F9 Nd2 111.63(6) . . ? N2 C9 C10 115.0(2) . . ? Nd2 F10 Nd1 111.12(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C26 F11 Nd2 119.15(15) . . ? N2 C11 C12 113.5(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 118.0(2) . . ? N3 C13 C18 130.5(3) . . ? C14 C13 C18 111.4(3) . . ? F5 C14 C15 118.7(3) . . ? F5 C14 C13 115.3(2) . . ? C15 C14 C13 126.0(3) . . ? C38 F15 Nd2 118.02(15) . . ? F6 C15 C16 120.2(3) . . ? F6 C15 C14 119.2(3) . . ? C16 C15 C14 120.6(3) . . ? C17 C16 C15 115.3(3) . . ? C17 C16 H16 122.4 . . ? C15 C16 H16 122.4 . . ? C16 C17 F7 119.2(3) . . ? C16 C17 C18 124.4(3) . . ? F7 C17 C18 116.4(3) . . ? F8 C18 C17 116.5(3) . . ? F8 C18 C13 121.2(3) . . ? C17 C18 C13 122.2(3) . . ? N3 C19 C20 110.1(2) . . ? N3 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? N3 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? N4 C20 C19 113.6(2) . . ? N4 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? N4 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? N4 C21 C22 114.0(2) . . ? N4 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N4 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 115.0(2) . . ? N4 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? N4 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C30 130.5(3) . . ? N5 C25 C26 118.0(2) . . ? C30 C25 C26 111.5(3) . . ? C27 C26 F11 119.3(3) . . ? C27 C26 C25 125.8(3) . . ? F11 C26 C25 114.8(2) . . ? F12 C27 C26 118.8(3) . . ? F12 C27 C28 120.3(3) . . ? C26 C27 C28 120.9(3) . . ? C29 C28 C27 115.7(3) . . ? C29 C28 H28 122.2 . . ? C27 C28 H28 122.2 . . ? C28 C29 F13 119.1(3) . . ? C28 C29 C30 123.9(3) . . ? F13 C29 C30 117.0(3) . . ? F14 C30 C29 116.6(3) . . ? F14 C30 C25 121.2(3) . . ? C29 C30 C25 122.1(3) . . ? N5 C31 C32 110.6(2) . . ? N5 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C31 112.8(2) . . ? N6 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? N6 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? N6 C33 C34 115.6(2) . . ? N6 C33 H33A 108.4 . . ? C34 C33 H33A 108.4 . . ? N6 C33 H33B 108.4 . . ? C34 C33 H33B 108.4 . . ? H33A C33 H33B 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N6 C35 C36 114.3(2) . . ? N6 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? N6 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N7 C37 C38 117.9(2) . . ? N7 C37 C42 129.7(3) . . ? C38 C37 C42 112.4(2) . . ? C39 C38 F15 118.9(3) . . ? C39 C38 C37 125.7(3) . . ? F15 C38 C37 115.4(2) . . ? F16 C39 C38 119.1(3) . . ? F16 C39 C40 120.7(3) . . ? C38 C39 C40 120.3(3) . . ? C41 C40 C39 115.6(3) . . ? C41 C40 H40 122.2 . . ? C39 C40 H40 122.2 . . ? F17 C41 C40 118.7(3) . . ? F17 C41 C42 116.8(3) . . ? C40 C41 C42 124.4(3) . . ? F18 C42 C41 117.5(3) . . ? F18 C42 C37 121.0(3) . . ? C41 C42 C37 121.5(3) . . ? N7 C43 C44 109.9(2) . . ? N7 C43 H43A 109.7 . . ? C44 C43 H43A 109.7 . . ? N7 C43 H43B 109.7 . . ? C44 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? N8 C44 C43 113.3(2) . . ? N8 C44 H44A 108.9 . . ? C43 C44 H44A 108.9 . . ? N8 C44 H44B 108.9 . . ? C43 C44 H44B 108.9 . . ? H44A C44 H44B 107.7 . . ? N8 C45 C46 116.2(2) . . ? N8 C45 H45A 108.2 . . ? C46 C45 H45A 108.2 . . ? N8 C45 H45B 108.2 . . ? C46 C45 H45B 108.2 . . ? H45A C45 H45B 107.4 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N8 C47 C48 115.8(2) . . ? N8 C47 H47A 108.3 . . ? C48 C47 H47A 108.3 . . ? N8 C47 H47B 108.3 . . ? C48 C47 H47B 108.3 . . ? H47A C47 H47B 107.4 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.816 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.090 data_[Nd(p-HC6F4NC2H4NEt2)2F]2.CIF _database_code_depnum_ccdc_archive 'CCDC 859386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(N,N-diethyl-N'-(2,3,5,6-tetrafluorophenyl)ethylenediamine -F,N,N')-bis-fluoro-neodymium(iii) ; _chemical_name_common ; tetrakis(N,N-diethyl-N'-(2,3,5,6- tetrafluorophenyl)ethylenediamine -F,N,N')-bis-fluoro-neodymium(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 F18 N8 Nd2' _chemical_formula_sum 'C48 H60 F18 N8 Nd2' _chemical_formula_weight 1379.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.115(2) _cell_length_b 12.644(3) _cell_length_c 20.204(4) _cell_angle_alpha 72.95(3) _cell_angle_beta 76.68(3) _cell_angle_gamma 68.60(3) _cell_volume 2728.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 36078 _cell_measurement_theta_min 1.064 _cell_measurement_theta_max 30.514 _exptl_crystal_description rhombus _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 1.985 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4369 _exptl_absorpt_correction_T_max 0.8574 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23861 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9087 _reflns_number_gt 8120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9087 _refine_ls_number_parameters 693 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.88834(2) 0.59995(2) 0.203445(13) 0.02285(11) Uani 1 1 d . . . F9 F 0.8844(3) 0.7246(3) 0.26766(17) 0.0331(7) Uani 1 1 d . . . N1 N 1.0270(4) 0.4073(4) 0.2474(2) 0.0261(9) Uani 1 1 d . . . C1 C 1.1439(5) 0.3674(5) 0.2047(3) 0.0370(13) Uani 1 1 d . . . H1A H 1.1521 0.2942 0.1927 0.044 Uiso 1 1 calc R . . H1B H 1.2092 0.3512 0.2318 0.044 Uiso 1 1 calc R . . Nd2 Nd 0.68690(2) 0.82956(2) 0.306317(14) 0.02659(11) Uani 1 1 d . . . F10 F 0.6962(3) 0.6847(3) 0.25621(17) 0.0311(7) Uani 1 1 d . . . N2 N 1.1216(4) 0.5794(4) 0.1513(2) 0.0305(10) Uani 1 1 d . . . C2 C 1.1541(5) 0.4600(5) 0.1386(3) 0.0342(13) Uani 1 1 d . . . H2A H 1.2373 0.4379 0.1145 0.041 Uiso 1 1 calc R . . H2B H 1.1010 0.4625 0.1071 0.041 Uiso 1 1 calc R . . F1 F 0.8243(3) 0.4821(3) 0.3268(2) 0.0569(11) Uani 1 1 d . . . N3 N 0.8639(5) 0.6591(5) 0.0807(3) 0.0389(12) Uani 1 1 d . . . C3 C 1.0043(5) 0.3347(4) 0.3092(3) 0.0242(10) Uani 1 1 d . . . F2 F 0.7494(4) 0.3561(4) 0.4488(3) 0.092(2) Uani 1 1 d . . . N4 N 0.7516(5) 0.4983(5) 0.1754(3) 0.0489(14) Uani 1 1 d . . . C4 C 0.8947(5) 0.3712(5) 0.3516(3) 0.0369(13) Uani 1 1 d . . . F3 F 1.1072(4) 0.0484(4) 0.4284(2) 0.0695(14) Uani 1 1 d . . . N5 N 0.6002(4) 0.8118(4) 0.4278(3) 0.0380(11) Uani 1 1 d . . . C5 C 0.8579(6) 0.3078(6) 0.4138(3) 0.0494(17) Uani 1 1 d . . . F4 F 1.1819(4) 0.1674(4) 0.3078(3) 0.0862(18) Uani 1 1 d . . . N6 N 0.4537(4) 0.8569(4) 0.3262(3) 0.0420(12) Uani 1 1 d . . . C6 C 0.9266(6) 0.1971(5) 0.4414(3) 0.0380(14) Uani 1 1 d . . . H6 H 0.8999 0.1507 0.4840 0.046 Uiso 1 1 calc R . . F5 F 0.8867(3) 0.8155(3) 0.13530(19) 0.0412(8) Uani 1 1 d . . . N7 N 0.6275(4) 1.0360(4) 0.2487(2) 0.0298(10) Uani 1 1 d . . . C7 C 1.0341(6) 0.1582(5) 0.4043(3) 0.0400(14) Uani 1 1 d . . . F6 F 0.8684(5) 1.0346(4) 0.0655(4) 0.098(2) Uani 1 1 d . . . N8 N 0.8072(5) 0.9435(4) 0.3373(3) 0.0364(11) Uani 1 1 d . . . C8 C 1.0754(5) 0.2206(5) 0.3407(3) 0.0358(13) Uani 1 1 d . . . F7 F 0.8221(6) 0.9483(7) -0.1374(3) 0.125(3) Uani 1 1 d . . . C9 C 1.1391(5) 0.6609(5) 0.0824(3) 0.0393(14) Uani 1 1 d . . . H9A H 1.1046 0.7416 0.0893 0.047 Uiso 1 1 calc R . . H9B H 1.0921 0.6542 0.0506 0.047 Uiso 1 1 calc R . . F8 F 0.8378(5) 0.7357(5) -0.0698(2) 0.0894(18) Uani 1 1 d . . . C10 C 1.2689(6) 0.6441(7) 0.0451(4) 0.0534(18) Uani 1 1 d . . . H10A H 1.3158 0.6561 0.0742 0.080 Uiso 1 1 calc R . . H10B H 1.2683 0.7008 0.0000 0.080 Uiso 1 1 calc R . . H10C H 1.3048 0.5648 0.0374 0.080 Uiso 1 1 calc R . . F11 F 0.7905(4) 0.6382(4) 0.39865(19) 0.0634(13) Uani 1 1 d . . . C11 C 1.1931(6) 0.5758(6) 0.2023(3) 0.0433(15) Uani 1 1 d . . . H11A H 1.2790 0.5405 0.1859 0.052 Uiso 1 1 calc R . . H11B H 1.1725 0.5249 0.2475 0.052 Uiso 1 1 calc R . . F12 F 0.9096(5) 0.4643(5) 0.4940(2) 0.093(2) Uani 1 1 d . . . C12 C 1.1738(7) 0.6941(8) 0.2135(4) 0.061(2) Uani 1 1 d . . . H12A H 1.2112 0.7389 0.1721 0.091 Uiso 1 1 calc R . . H12B H 1.2098 0.6848 0.2544 0.091 Uiso 1 1 calc R . . H12C H 1.0877 0.7356 0.2212 0.091 Uiso 1 1 calc R . . F13 F 0.6518(5) 0.6437(5) 0.6714(2) 0.0860(17) Uani 1 1 d . . . C13 C 0.8389(7) 0.5738(7) 0.0536(4) 0.060(2) Uani 1 1 d . . . H13A H 0.9051 0.5457 0.0174 0.072 Uiso 1 1 calc R . . H13B H 0.7640 0.6116 0.0323 0.072 Uiso 1 1 calc R . . F14 F 0.5327(5) 0.8140(5) 0.5770(2) 0.0893(19) Uani 1 1 d . . . C14 C 0.8264(7) 0.4689(6) 0.1162(5) 0.058(2) Uani 1 1 d . . . H14A H 0.7966 0.4189 0.0999 0.070 Uiso 1 1 calc R . . H14B H 0.9070 0.4216 0.1291 0.070 Uiso 1 1 calc R . . F15 F 0.6483(3) 0.8912(3) 0.17331(18) 0.0392(8) Uani 1 1 d . . . C15 C 0.8569(5) 0.7656(6) 0.0387(3) 0.0443(16) Uani 1 1 d . . . F16 F 0.5812(4) 0.9538(4) 0.0472(2) 0.0574(11) Uani 1 1 d . . . C16 C 0.8689(6) 0.8498(6) 0.0662(3) 0.0476(17) Uani 1 1 d . . . F17 F 0.4561(4) 1.3478(3) 0.0579(2) 0.0550(10) Uani 1 1 d . . . C17 C 0.8599(7) 0.9621(7) 0.0307(5) 0.076(3) Uani 1 1 d . . . F18 F 0.5155(4) 1.2884(3) 0.1837(2) 0.0494(9) Uani 1 1 d . . . C18 C 0.8420(7) 0.9980(8) -0.0395(5) 0.084(3) Uani 1 1 d . . . H18 H 0.8350 1.0755 -0.0656 0.101 Uiso 1 1 calc R . . C19 C 0.8350(8) 0.9160(10) -0.0685(4) 0.081(3) Uani 1 1 d . . . C20 C 0.8431(7) 0.8062(8) -0.0330(4) 0.064(2) Uani 1 1 d . . . C21 C 0.7349(8) 0.3911(7) 0.2264(4) 0.061(2) Uani 1 1 d . . . H21A H 0.8120 0.3421 0.2437 0.073 Uiso 1 1 calc R . . H21B H 0.7134 0.3458 0.2016 0.073 Uiso 1 1 calc R . . C22 C 0.6391(10) 0.4144(9) 0.2889(5) 0.087(3) Uani 1 1 d . . . H22A H 0.6545 0.4662 0.3109 0.130 Uiso 1 1 calc R . . H22B H 0.6410 0.3404 0.3228 0.130 Uiso 1 1 calc R . . H22C H 0.5602 0.4515 0.2732 0.130 Uiso 1 1 calc R . . C23 C 0.6335(7) 0.5852(7) 0.1589(4) 0.060(2) Uani 1 1 d . . . H23A H 0.6481 0.6567 0.1276 0.072 Uiso 1 1 calc R . . H23B H 0.5865 0.6061 0.2029 0.072 Uiso 1 1 calc R . . C24 C 0.5572(9) 0.5502(8) 0.1253(6) 0.079(3) Uani 1 1 d . . . H24A H 0.5996 0.5344 0.0799 0.119 Uiso 1 1 calc R . . H24B H 0.4815 0.6137 0.1185 0.119 Uiso 1 1 calc R . . H24C H 0.5408 0.4798 0.1556 0.119 Uiso 1 1 calc R . . C25 C 0.4734(6) 0.8776(6) 0.4436(3) 0.0487(16) Uani 1 1 d . . . H25A H 0.4657 0.9381 0.4678 0.058 Uiso 1 1 calc R . . H25B H 0.4304 0.8244 0.4749 0.058 Uiso 1 1 calc R . . C26 C 0.4184(6) 0.9350(6) 0.3762(4) 0.0456(16) Uani 1 1 d . . . H26A H 0.3301 0.9610 0.3879 0.055 Uiso 1 1 calc R . . H26B H 0.4426 1.0053 0.3526 0.055 Uiso 1 1 calc R . . C27 C 0.6534(5) 0.7322(5) 0.4826(3) 0.0374(13) Uani 1 1 d . . . C28 C 0.7543(6) 0.6396(6) 0.4679(3) 0.0481(17) Uani 1 1 d . . . C29 C 0.8177(6) 0.5516(6) 0.5165(4) 0.0521(18) Uani 1 1 d . . . C30 C 0.7868(7) 0.5486(6) 0.5864(4) 0.0561(19) Uani 1 1 d . . . H30 H 0.8297 0.4884 0.6209 0.067 Uiso 1 1 calc R . . C31 C 0.6872(7) 0.6409(7) 0.6030(4) 0.058(2) Uani 1 1 d . . . C32 C 0.6247(6) 0.7280(6) 0.5537(4) 0.0516(18) Uani 1 1 d . . . C33 C 0.4337(6) 0.7427(6) 0.3585(4) 0.0524(17) Uani 1 1 d . . . H33A H 0.4783 0.7038 0.3991 0.063 Uiso 1 1 calc R . . H33B H 0.4677 0.6930 0.3241 0.063 Uiso 1 1 calc R . . C34 C 0.3040(7) 0.7496(8) 0.3826(5) 0.070(2) Uani 1 1 d . . . H34A H 0.2724 0.7890 0.4214 0.106 Uiso 1 1 calc R . . H34B H 0.2980 0.6706 0.3982 0.106 Uiso 1 1 calc R . . H34C H 0.2575 0.7937 0.3438 0.106 Uiso 1 1 calc R . . C35 C 0.3849(6) 0.9204(6) 0.2666(4) 0.0494(16) Uani 1 1 d . . . H35A H 0.4054 0.9929 0.2437 0.059 Uiso 1 1 calc R . . H35B H 0.2985 0.9435 0.2849 0.059 Uiso 1 1 calc R . . C36 C 0.4069(7) 0.8505(7) 0.2107(4) 0.0570(18) Uani 1 1 d . . . H36A H 0.4930 0.8110 0.2004 0.085 Uiso 1 1 calc R . . H36B H 0.3767 0.9040 0.1679 0.085 Uiso 1 1 calc R . . H36C H 0.3651 0.7924 0.2285 0.085 Uiso 1 1 calc R . . C37 C 0.6448(5) 1.1164(5) 0.2826(3) 0.0359(13) Uani 1 1 d . . . H37A H 0.5666 1.1737 0.2949 0.043 Uiso 1 1 calc R . . H37B H 0.6968 1.1597 0.2500 0.043 Uiso 1 1 calc R . . C38 C 0.7018(6) 1.0477(5) 0.3479(3) 0.0409(14) Uani 1 1 d . . . H38A H 0.7274 1.0997 0.3651 0.049 Uiso 1 1 calc R . . H38B H 0.6411 1.0217 0.3845 0.049 Uiso 1 1 calc R . . C39 C 0.5884(5) 1.0835(5) 0.1855(3) 0.0291(12) Uani 1 1 d . . . C40 C 0.5991(5) 1.0071(5) 0.1445(3) 0.0374(13) Uani 1 1 d . . . C41 C 0.5639(6) 1.0390(6) 0.0794(3) 0.0429(15) Uani 1 1 d . . . C42 C 0.5147(6) 1.1547(6) 0.0476(3) 0.0463(16) Uani 1 1 d . . . H42 H 0.4904 1.1789 0.0026 0.056 Uiso 1 1 calc R . . C43 C 0.5034(5) 1.2325(5) 0.0858(3) 0.0402(14) Uani 1 1 d . . . C44 C 0.5378(5) 1.2009(5) 0.1511(3) 0.0346(13) Uani 1 1 d . . . C45 C 0.8957(6) 0.9715(6) 0.2770(4) 0.0441(15) Uani 1 1 d . . . H45A H 0.8547 1.0064 0.2349 0.053 Uiso 1 1 calc R . . H45B H 0.9578 0.8973 0.2700 0.053 Uiso 1 1 calc R . . C46 C 0.9588(7) 1.0538(7) 0.2813(5) 0.065(2) Uani 1 1 d . . . H46A H 0.8989 1.1262 0.2912 0.097 Uiso 1 1 calc R . . H46B H 1.0088 1.0718 0.2367 0.097 Uiso 1 1 calc R . . H46C H 1.0091 1.0162 0.3187 0.097 Uiso 1 1 calc R . . C47 C 0.8590(7) 0.8913(6) 0.4039(4) 0.0499(17) Uani 1 1 d . . . H47A H 0.7973 0.8699 0.4417 0.060 Uiso 1 1 calc R . . H47B H 0.8820 0.9502 0.4159 0.060 Uiso 1 1 calc R . . C48 C 0.9689(7) 0.7827(7) 0.3999(5) 0.064(2) Uani 1 1 d . . . H48A H 0.9508 0.7300 0.3799 0.096 Uiso 1 1 calc R . . H48B H 0.9898 0.7426 0.4470 0.096 Uiso 1 1 calc R . . H48C H 1.0364 0.8061 0.3703 0.096 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 Nd1 0.01941(18) 0.01711(16) 0.03018(18) -0.00418(12) -0.00835(12) -0.00173(12) F9 0.0195(16) 0.0392(18) 0.0452(18) -0.0204(15) -0.0062(13) -0.0053(14) N1 0.023(2) 0.019(2) 0.026(2) -0.0035(17) -0.0036(17) 0.0022(17) C1 0.030(3) 0.029(3) 0.035(3) -0.005(2) 0.001(2) 0.004(2) Nd2 0.01998(18) 0.02228(17) 0.03341(19) -0.00704(13) -0.00916(12) 0.00171(12) F10 0.0157(15) 0.0223(15) 0.0537(19) -0.0088(14) -0.0050(13) -0.0041(12) N2 0.022(2) 0.031(2) 0.034(2) -0.006(2) -0.0058(19) -0.0032(19) C2 0.032(3) 0.028(3) 0.034(3) -0.008(2) 0.002(2) -0.002(2) F1 0.040(2) 0.0320(19) 0.055(2) 0.0090(17) 0.0105(17) 0.0123(16) N3 0.036(3) 0.044(3) 0.033(3) -0.008(2) -0.009(2) -0.005(2) C3 0.021(3) 0.020(2) 0.030(3) -0.010(2) -0.008(2) 0.001(2) F2 0.061(3) 0.063(3) 0.074(3) 0.019(2) 0.034(2) 0.016(2) N4 0.047(4) 0.043(3) 0.061(4) -0.003(3) -0.021(3) -0.018(3) C4 0.031(3) 0.023(3) 0.039(3) -0.002(2) -0.003(2) 0.006(2) F3 0.044(2) 0.044(2) 0.071(3) 0.023(2) -0.004(2) 0.0121(18) N5 0.028(3) 0.033(3) 0.038(3) -0.007(2) -0.005(2) 0.007(2) C5 0.038(4) 0.041(4) 0.044(4) -0.001(3) 0.009(3) 0.000(3) F4 0.049(3) 0.051(3) 0.082(3) 0.022(2) 0.021(2) 0.025(2) N6 0.022(3) 0.033(3) 0.063(3) -0.010(2) -0.009(2) 0.001(2) C6 0.044(4) 0.031(3) 0.027(3) 0.001(2) -0.002(2) -0.007(3) F5 0.038(2) 0.0273(17) 0.056(2) -0.0020(15) -0.0167(16) -0.0078(15) N7 0.031(3) 0.024(2) 0.034(2) -0.0061(19) -0.0098(19) -0.0050(19) C7 0.036(3) 0.026(3) 0.042(3) 0.005(2) -0.015(3) 0.003(3) F6 0.070(4) 0.039(2) 0.173(6) 0.020(3) -0.035(4) -0.026(2) N8 0.030(3) 0.032(3) 0.047(3) -0.011(2) -0.015(2) -0.003(2) C8 0.023(3) 0.029(3) 0.043(3) -0.003(2) -0.007(2) 0.004(2) F7 0.090(4) 0.157(6) 0.052(3) 0.046(3) -0.021(3) -0.001(4) C9 0.028(3) 0.038(3) 0.042(3) 0.001(3) -0.004(2) -0.008(3) F8 0.099(4) 0.107(4) 0.041(2) -0.018(3) -0.028(3) 0.003(3) C10 0.028(3) 0.057(4) 0.057(4) 0.002(3) 0.000(3) -0.008(3) F11 0.050(2) 0.066(3) 0.035(2) -0.0129(18) -0.0111(17) 0.031(2) C11 0.028(3) 0.055(4) 0.050(4) -0.012(3) -0.010(3) -0.014(3) F12 0.091(4) 0.080(3) 0.056(3) -0.022(2) -0.036(3) 0.054(3) C12 0.050(5) 0.085(6) 0.068(5) -0.033(4) -0.005(4) -0.036(4) F13 0.087(4) 0.095(4) 0.033(2) -0.011(2) -0.005(2) 0.015(3) C13 0.055(5) 0.079(5) 0.055(4) -0.039(4) -0.013(4) -0.010(4) F14 0.090(4) 0.078(3) 0.047(2) -0.023(2) -0.008(2) 0.040(3) C14 0.052(5) 0.034(3) 0.095(6) -0.015(4) -0.041(4) -0.003(3) F15 0.044(2) 0.0234(16) 0.049(2) -0.0100(14) -0.0256(16) 0.0039(14) C15 0.022(3) 0.058(4) 0.037(3) -0.005(3) -0.007(2) 0.003(3) F16 0.067(3) 0.049(2) 0.057(2) -0.0205(19) -0.037(2) 0.005(2) C16 0.030(3) 0.040(3) 0.048(4) 0.016(3) -0.005(3) -0.004(3) F17 0.050(2) 0.034(2) 0.058(2) 0.0089(17) -0.0150(19) 0.0031(17) C17 0.046(5) 0.045(4) 0.116(8) 0.021(5) -0.024(5) -0.013(4) F18 0.059(2) 0.0253(17) 0.060(2) -0.0063(16) -0.0201(19) -0.0038(16) C18 0.045(5) 0.061(5) 0.087(7) 0.051(5) -0.009(4) -0.001(4) C19 0.057(6) 0.089(7) 0.047(5) 0.016(5) -0.007(4) 0.009(5) C20 0.042(4) 0.085(6) 0.040(4) -0.003(4) -0.012(3) 0.005(4) C21 0.075(6) 0.043(4) 0.071(5) 0.000(4) -0.023(4) -0.028(4) C22 0.092(7) 0.092(7) 0.086(7) 0.002(5) -0.015(5) -0.057(6) C23 0.052(5) 0.058(5) 0.070(5) 0.001(4) -0.029(4) -0.019(4) C24 0.068(6) 0.070(6) 0.113(7) -0.018(5) -0.044(5) -0.020(5) C25 0.034(4) 0.042(4) 0.046(4) -0.008(3) 0.004(3) 0.008(3) C26 0.019(3) 0.042(4) 0.058(4) -0.012(3) -0.001(3) 0.009(3) C27 0.028(3) 0.034(3) 0.037(3) -0.006(2) -0.004(2) 0.004(2) C28 0.040(4) 0.048(4) 0.039(3) -0.006(3) -0.015(3) 0.010(3) C29 0.040(4) 0.046(4) 0.045(4) -0.007(3) -0.010(3) 0.014(3) C30 0.055(5) 0.050(4) 0.041(4) 0.000(3) -0.015(3) 0.005(3) C31 0.057(5) 0.062(5) 0.037(4) -0.009(3) -0.007(3) 0.002(4) C32 0.043(4) 0.045(4) 0.043(4) -0.015(3) 0.003(3) 0.012(3) C33 0.035(4) 0.049(4) 0.063(4) -0.001(3) -0.006(3) -0.012(3) C34 0.053(5) 0.077(6) 0.072(5) -0.003(4) 0.005(4) -0.030(4) C35 0.023(3) 0.052(4) 0.067(4) -0.009(3) -0.013(3) -0.003(3) C36 0.040(4) 0.061(5) 0.072(5) -0.012(4) -0.016(3) -0.015(3) C37 0.032(3) 0.029(3) 0.042(3) -0.012(2) -0.010(3) 0.000(2) C38 0.043(4) 0.031(3) 0.051(4) -0.017(3) -0.019(3) -0.002(3) C39 0.019(3) 0.028(3) 0.037(3) -0.008(2) -0.007(2) -0.002(2) C40 0.032(3) 0.029(3) 0.046(3) -0.007(3) -0.019(3) 0.002(2) C41 0.036(4) 0.040(3) 0.049(4) -0.014(3) -0.018(3) 0.002(3) C42 0.044(4) 0.043(4) 0.040(3) -0.004(3) -0.020(3) 0.004(3) C43 0.025(3) 0.035(3) 0.045(3) 0.002(3) -0.010(3) 0.004(2) C44 0.033(3) 0.022(3) 0.045(3) -0.007(2) -0.010(3) -0.003(2) C45 0.033(3) 0.045(4) 0.060(4) -0.020(3) -0.010(3) -0.010(3) C46 0.048(5) 0.068(5) 0.093(6) -0.033(5) -0.012(4) -0.023(4) C47 0.053(4) 0.047(4) 0.055(4) -0.014(3) -0.031(3) -0.007(3) C48 0.051(5) 0.059(5) 0.084(6) -0.023(4) -0.050(4) 0.011(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 Nd1 F9 2.299(3) . ? Nd1 F10 2.326(3) . ? Nd1 N3 2.426(5) . ? Nd1 N1 2.444(4) . ? Nd1 F1 2.609(4) . ? Nd1 F5 2.665(3) . ? Nd1 N4 2.669(5) . ? Nd1 N2 2.724(5) . ? F9 Nd2 2.350(3) . ? N1 C3 1.353(7) . ? N1 C1 1.475(7) . ? C1 C2 1.511(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? Nd2 F10 2.296(3) . ? Nd2 N5 2.417(5) . ? Nd2 N7 2.433(4) . ? Nd2 N8 2.660(5) . ? Nd2 N6 2.666(5) . ? Nd2 F11 2.669(4) . ? Nd2 F15 2.671(3) . ? N2 C11 1.473(7) . ? N2 C9 1.492(7) . ? N2 C2 1.498(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? F1 C4 1.363(7) . ? N3 C15 1.349(9) . ? N3 C13 1.488(9) . ? C3 C4 1.403(8) . ? C3 C8 1.427(7) . ? F2 C5 1.357(8) . ? N4 C14 1.382(10) . ? N4 C23 1.491(10) . ? N4 C21 1.492(9) . ? C4 C5 1.355(8) . ? F3 C7 1.361(7) . ? N5 C27 1.362(8) . ? N5 C25 1.467(8) . ? C5 C6 1.367(9) . ? F4 C8 1.339(7) . ? N6 C33 1.483(8) . ? N6 C35 1.483(8) . ? N6 C26 1.502(9) . ? C6 C7 1.341(9) . ? C6 H6 0.9500 . ? F5 C16 1.379(8) . ? N7 C39 1.356(7) . ? N7 C37 1.475(7) . ? C7 C8 1.386(8) . ? F6 C17 1.351(12) . ? N8 C45 1.476(8) . ? N8 C47 1.485(8) . ? N8 C38 1.491(8) . ? F7 C19 1.361(10) . ? C9 C10 1.546(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F8 C20 1.343(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? F11 C28 1.369(8) . ? C11 C12 1.503(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C29 1.352(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? F13 C31 1.357(8) . ? C13 C14 1.567(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? F14 C32 1.350(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? F15 C40 1.365(7) . ? C15 C16 1.399(11) . ? C15 C20 1.414(10) . ? F16 C41 1.345(7) . ? C16 C17 1.367(10) . ? F17 C43 1.352(7) . ? C17 C18 1.398(14) . ? F18 C44 1.363(7) . ? C18 C19 1.367(15) . ? C18 H18 0.9500 . ? C19 C20 1.343(14) . ? C21 C22 1.524(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.509(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.520(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.389(9) . ? C27 C28 1.395(9) . ? C28 C29 1.370(9) . ? C29 C30 1.367(10) . ? C30 C31 1.395(11) . ? C30 H30 0.9500 . ? C31 C32 1.368(10) . ? C33 C34 1.513(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.549(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.510(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.401(8) . ? C39 C44 1.411(8) . ? C40 C41 1.377(8) . ? C41 C42 1.378(9) . ? C42 C43 1.371(9) . ? C42 H42 0.9500 . ? C43 C44 1.378(9) . ? C45 C46 1.529(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.531(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F9 Nd1 F10 67.78(11) . . ? F9 Nd1 N3 124.13(15) . . ? F10 Nd1 N3 102.21(15) . . ? F9 Nd1 N1 108.48(13) . . ? F10 Nd1 N1 126.65(13) . . ? N3 Nd1 N1 118.79(16) . . ? F9 Nd1 F1 82.08(13) . . ? F10 Nd1 F1 64.44(11) . . ? N3 Nd1 F1 145.42(17) . . ? N1 Nd1 F1 62.41(13) . . ? F9 Nd1 F5 62.14(11) . . ? F10 Nd1 F5 86.94(11) . . ? N3 Nd1 F5 62.54(15) . . ? N1 Nd1 F5 140.84(13) . . ? F1 Nd1 F5 141.11(12) . . ? F9 Nd1 N4 142.19(17) . . ? F10 Nd1 N4 74.74(16) . . ? N3 Nd1 N4 68.13(18) . . ? N1 Nd1 N4 89.65(16) . . ? F1 Nd1 N4 77.44(17) . . ? F5 Nd1 N4 121.68(14) . . ? F9 Nd1 N2 90.13(13) . . ? F10 Nd1 N2 156.46(12) . . ? N3 Nd1 N2 83.06(16) . . ? N1 Nd1 N2 66.74(14) . . ? F1 Nd1 N2 122.47(13) . . ? F5 Nd1 N2 75.06(13) . . ? N4 Nd1 N2 127.68(17) . . ? Nd1 F9 Nd2 111.32(12) . . ? C3 N1 C1 117.3(4) . . ? C3 N1 Nd1 124.3(3) . . ? C1 N1 Nd1 118.4(3) . . ? N1 C1 C2 109.9(4) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? F10 Nd2 F9 67.40(11) . . ? F10 Nd2 N5 116.12(15) . . ? F9 Nd2 N5 124.06(14) . . ? F10 Nd2 N7 123.78(13) . . ? F9 Nd2 N7 113.79(14) . . ? N5 Nd2 N7 107.81(16) . . ? F10 Nd2 N8 146.76(14) . . ? F9 Nd2 N8 79.43(13) . . ? N5 Nd2 N8 83.94(18) . . ? N7 Nd2 N8 67.40(15) . . ? F10 Nd2 N6 81.61(14) . . ? F9 Nd2 N6 148.91(14) . . ? N5 Nd2 N6 67.14(18) . . ? N7 Nd2 N6 85.00(16) . . ? N8 Nd2 N6 131.62(16) . . ? F10 Nd2 F11 78.53(13) . . ? F9 Nd2 F11 64.85(12) . . ? N5 Nd2 F11 62.06(14) . . ? N7 Nd2 F11 156.42(15) . . ? N8 Nd2 F11 89.73(16) . . ? N6 Nd2 F11 107.76(16) . . ? F10 Nd2 F15 62.47(11) . . ? F9 Nd2 F15 87.05(11) . . ? N5 Nd2 F15 147.07(15) . . ? N7 Nd2 F15 61.53(13) . . ? N8 Nd2 F15 115.28(14) . . ? N6 Nd2 F15 80.52(15) . . ? F11 Nd2 F15 138.77(11) . . ? Nd2 F10 Nd1 112.31(12) . . ? C11 N2 C9 113.4(5) . . ? C11 N2 C2 109.8(5) . . ? C9 N2 C2 107.9(4) . . ? C11 N2 Nd1 114.1(4) . . ? C9 N2 Nd1 114.3(3) . . ? C2 N2 Nd1 95.7(3) . . ? N2 C2 C1 113.5(5) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C4 F1 Nd1 119.8(3) . . ? C15 N3 C13 118.4(6) . . ? C15 N3 Nd1 125.7(4) . . ? C13 N3 Nd1 115.4(4) . . ? N1 C3 C4 118.7(5) . . ? N1 C3 C8 130.2(5) . . ? C4 C3 C8 111.1(5) . . ? C14 N4 C23 112.0(6) . . ? C14 N4 C21 109.8(6) . . ? C23 N4 C21 110.4(6) . . ? C14 N4 Nd1 94.8(4) . . ? C23 N4 Nd1 110.8(4) . . ? C21 N4 Nd1 118.2(4) . . ? C5 C4 F1 119.6(5) . . ? C5 C4 C3 125.7(5) . . ? F1 C4 C3 114.6(5) . . ? C27 N5 C25 116.3(5) . . ? C27 N5 Nd2 125.2(4) . . ? C25 N5 Nd2 117.7(4) . . ? C4 C5 F2 118.5(6) . . ? C4 C5 C6 121.7(6) . . ? F2 C5 C6 119.8(5) . . ? C33 N6 C35 110.5(5) . . ? C33 N6 C26 113.5(5) . . ? C35 N6 C26 107.7(5) . . ? C33 N6 Nd2 110.0(4) . . ? C35 N6 Nd2 118.6(4) . . ? C26 N6 Nd2 95.8(3) . . ? C7 C6 C5 115.5(5) . . ? C7 C6 H6 122.2 . . ? C5 C6 H6 122.2 . . ? C16 F5 Nd1 117.1(4) . . ? C39 N7 C37 116.5(4) . . ? C39 N7 Nd2 126.1(3) . . ? C37 N7 Nd2 117.3(3) . . ? C6 C7 F3 118.8(5) . . ? C6 C7 C8 124.5(5) . . ? F3 C7 C8 116.6(6) . . ? C45 N8 C47 112.7(5) . . ? C45 N8 C38 112.7(5) . . ? C47 N8 C38 107.3(5) . . ? C45 N8 Nd2 110.3(3) . . ? C47 N8 Nd2 116.7(4) . . ? C38 N8 Nd2 96.1(3) . . ? F4 C8 C7 117.6(5) . . ? F4 C8 C3 120.9(5) . . ? C7 C8 C3 121.4(5) . . ? N2 C9 C10 117.2(5) . . ? N2 C9 H9A 108.0 . . ? C10 C9 H9A 108.0 . . ? N2 C9 H9B 108.0 . . ? C10 C9 H9B 108.0 . . ? H9A C9 H9B 107.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C28 F11 Nd2 116.8(3) . . ? N2 C11 C12 113.3(6) . . ? N2 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N2 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 108.4(5) . . ? N3 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? N3 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? N4 C14 C13 115.8(6) . . ? N4 C14 H14A 108.3 . . ? C13 C14 H14A 108.3 . . ? N4 C14 H14B 108.3 . . ? C13 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C40 F15 Nd2 118.0(3) . . ? N3 C15 C16 118.6(6) . . ? N3 C15 C20 128.8(7) . . ? C16 C15 C20 112.5(7) . . ? C17 C16 F5 118.8(8) . . ? C17 C16 C15 125.1(8) . . ? F5 C16 C15 116.0(5) . . ? F6 C17 C16 118.1(9) . . ? F6 C17 C18 122.5(8) . . ? C16 C17 C18 119.4(10) . . ? C19 C18 C17 116.6(7) . . ? C19 C18 H18 121.7 . . ? C17 C18 H18 121.7 . . ? C20 C19 F7 119.2(11) . . ? C20 C19 C18 123.4(8) . . ? F7 C19 C18 117.3(10) . . ? F8 C20 C19 115.8(8) . . ? F8 C20 C15 121.4(8) . . ? C19 C20 C15 122.8(9) . . ? N4 C21 C22 114.4(7) . . ? N4 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? N4 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 117.7(7) . . ? N4 C23 H23A 107.9 . . ? C24 C23 H23A 107.9 . . ? N4 C23 H23B 107.9 . . ? C24 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 109.8(5) . . ? N5 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? N5 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? N6 C26 C25 113.9(5) . . ? N6 C26 H26A 108.8 . . ? C25 C26 H26A 108.8 . . ? N6 C26 H26B 108.8 . . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? N5 C27 C32 130.1(6) . . ? N5 C27 C28 117.9(5) . . ? C32 C27 C28 112.0(6) . . ? F11 C28 C29 118.7(6) . . ? F11 C28 C27 115.9(5) . . ? C29 C28 C27 125.4(6) . . ? F12 C29 C30 120.3(6) . . ? F12 C29 C28 118.2(6) . . ? C30 C29 C28 121.5(6) . . ? C29 C30 C31 114.7(6) . . ? C29 C30 H30 122.6 . . ? C31 C30 H30 122.6 . . ? F13 C31 C32 119.1(7) . . ? F13 C31 C30 117.8(6) . . ? C32 C31 C30 123.1(6) . . ? F14 C32 C31 116.8(6) . . ? F14 C32 C27 119.9(6) . . ? C31 C32 C27 123.3(6) . . ? N6 C33 C34 114.7(6) . . ? N6 C33 H33A 108.6 . . ? C34 C33 H33A 108.6 . . ? N6 C33 H33B 108.6 . . ? C34 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N6 C35 C36 114.8(6) . . ? N6 C35 H35A 108.6 . . ? C36 C35 H35A 108.6 . . ? N6 C35 H35B 108.6 . . ? C36 C35 H35B 108.6 . . ? H35A C35 H35B 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N7 C37 C38 109.6(5) . . ? N7 C37 H37A 109.8 . . ? C38 C37 H37A 109.8 . . ? N7 C37 H37B 109.8 . . ? C38 C37 H37B 109.8 . . ? H37A C37 H37B 108.2 . . ? N8 C38 C37 113.7(5) . . ? N8 C38 H38A 108.8 . . ? C37 C38 H38A 108.8 . . ? N8 C38 H38B 108.8 . . ? C37 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? N7 C39 C40 117.6(5) . . ? N7 C39 C44 131.0(5) . . ? C40 C39 C44 111.3(5) . . ? F15 C40 C41 118.6(5) . . ? F15 C40 C39 115.5(5) . . ? C41 C40 C39 125.9(6) . . ? F16 C41 C40 117.9(5) . . ? F16 C41 C42 121.1(6) . . ? C40 C41 C42 121.0(6) . . ? C43 C42 C41 115.0(6) . . ? C43 C42 H42 122.5 . . ? C41 C42 H42 122.5 . . ? F17 C43 C42 118.4(5) . . ? F17 C43 C44 117.4(6) . . ? C42 C43 C44 124.2(5) . . ? F18 C44 C43 117.0(5) . . ? F18 C44 C39 120.3(5) . . ? C43 C44 C39 122.6(5) . . ? N8 C45 C46 117.2(6) . . ? N8 C45 H45A 108.0 . . ? C46 C45 H45A 108.0 . . ? N8 C45 H45B 108.0 . . ? C46 C45 H45B 108.0 . . ? H45A C45 H45B 107.2 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N8 C47 C48 112.6(6) . . ? N8 C47 H47A 109.1 . . ? C48 C47 H47A 109.1 . . ? N8 C47 H47B 109.1 . . ? C48 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.312 _refine_diff_density_min -1.322 _refine_diff_density_rms 0.141