# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Samiran Mitra' _publ_contact_author_email 'SMITRA 2002@YAHOO.COM' _publ_section_title ; Syntheses, Characterization, Magnetism and Photoluminescence of a Homodinuclear Ln(III) - Schiff Base Family ; loop_ _publ_author_name 'Samiran Mitra' 'Luca Carrella' 'Joy Chakraborty' 'Loic Charbonniere' 'Guillaume Chastanet' ; M.E.Fallah ; 'Dominique Luneau' 'Guillaume Pilet' 'Aurkie Ray' 'Eva Rentschler' 'Raymond Ziessel' # Attachment 'New_Complex1-Nd.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 612533' _audit_creation_date 04-02-12 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #******************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 12.911(5) _cell_angle_alpha 90 _cell_length_b 11.938(5) _cell_angle_beta 110.732(5) _cell_length_c 13.960(5) _cell_angle_gamma 90 _cell_volume 2012.3(14) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Nd ' -0.1943 3.0179 22.6845 2.6625 19.6847 0.2106 12.7740 15.8850 2.8514 137.9030 1.9849 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C36 H36 N8 Nd2 O10 ' _chemical_formula_moiety ' C36 H36 N8 Nd2 O10 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1029.20 _cell_measurement_reflns_used 4025 _cell_measurement_theta_min 1 _cell_measurement_theta_max 33 _cell_measurement_temperature 293(1) _exptl_crystal_description ' rhombic ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_meas 1.703 # Non-dispersive F(000): _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.615 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method \w/2\q # Sheldrick geometric approximatio 0.40 0.48 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.48 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 293(1) _diffrn_reflns_number 9886 _reflns_number_total 6550 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 6550 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7706 _diffrn_reflns_theta_min 1.848 _diffrn_reflns_theta_max 33.205 _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 26.904 _diffrn_measured_fraction_theta_full 0.959 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -19 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -1.01 _refine_diff_density_max 1.00 _refine_ls_number_reflns 4052 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 #_refine_ls_R_factor_ref 0.0385 _refine_ls_wR_factor_ref 0.0455 _refine_ls_goodness_of_fit_ref 1.1014 #_reflns_number_all 6536 _refine_ls_R_factor_all 0.0732 _refine_ls_wR_factor_all 0.0685 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4052 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_gt 0.0455 _refine_ls_shift/su_max 0.005467 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.01 0.279 0.627 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999) SIR97: a new tool for crystal structure determination and refinement.J. App. Cryst. 32, 115-119 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group _atom_site_attached_hydrogens Nd1 Nd 0.019423(18) 0.159898(18) 0.025719(16) 0.0327 1.0000 Uani . . . . . . N1 N 0.0866(3) 0.3143(4) 0.2067(3) 0.0419 1.0000 Uani . . . . . . O2 O 0.0260(4) 0.3455(3) 0.1184(3) 0.0625 1.0000 Uani . . . . . . O3 O 0.1167(4) 0.2143(3) 0.2151(3) 0.0629 1.0000 Uani . . . . . . O4 O 0.1154(4) 0.3780(4) 0.2793(3) 0.0643 1.0000 Uani . . . . . . O5 O 0.1932(3) 0.1566(3) 0.0276(3) 0.0507 1.0000 Uani . . . . . . C6 C 0.2518(5) 0.1707(5) -0.0310(5) 0.0532 1.0000 Uani . . . . . . C7 C 0.3587(6) 0.1214(6) -0.0027(6) 0.0691 1.0000 Uani . . . . . . C8 C 0.4205(8) 0.1341(9) -0.0658(9) 0.0988 1.0000 Uani . . . . . . C9 C 0.3811(11) 0.1948(11) -0.1563(11) 0.1335 1.0000 Uani . . . . . . C10 C 0.2808(9) 0.2428(9) -0.1818(8) 0.1077 1.0000 Uani . . . . . . C11 C 0.2119(7) 0.2330(6) -0.1231(6) 0.0658 1.0000 Uani . . . . . . C12 C 0.1080(6) 0.2911(5) -0.1593(5) 0.0625 1.0000 Uani . . . . . . N13 N 0.0303(4) 0.2861(4) -0.1223(4) 0.0514 1.0000 Uani . . . . . . C14 C -0.0697(7) 0.3534(5) -0.1774(5) 0.0647 1.0000 Uani . . . . . . C15 C -0.1362(6) 0.3751(5) -0.1116(5) 0.0628 1.0000 Uani . . . . . . N16 N -0.1642(4) 0.2672(4) -0.0732(3) 0.0480 1.0000 Uani . . . . . . C17 C -0.2333(5) 0.2792(6) -0.0098(5) 0.0615 1.0000 Uani . . . . . . C18 C -0.2533(4) 0.1664(6) 0.0271(4) 0.0562 1.0000 Uani . . . . . . N19 N -0.1460(3) 0.1154(4) 0.0885(3) 0.0444 1.0000 Uani . . . . . . C20 C -0.1432(5) 0.0528(5) 0.1632(4) 0.0497 1.0000 Uani . . . . . . C21 C -0.0453(4) -0.0038(4) 0.2304(4) 0.0463 1.0000 Uani . . . . . . C22 C -0.0423(6) -0.0321(6) 0.3303(5) 0.0627 1.0000 Uani . . . . . . C23 C 0.0499(7) -0.0802(7) 0.4010(5) 0.0769 1.0000 Uani . . . . . . C24 C 0.1402(6) -0.1029(6) 0.3732(4) 0.0642 1.0000 Uani . . . . . . C25 C 0.1378(5) -0.0792(4) 0.2751(4) 0.0470 1.0000 Uani . . . . . . C26 C 0.0446(4) -0.0339(4) 0.2020(3) 0.0351 1.0000 Uani . . . . . . O27 O 0.0421(3) -0.0196(3) 0.1052(2) 0.0356 1.0000 Uani . . . . . . H262 H -0.1103 -0.0190 0.3487 0.0787 1.0000 Uiso . . . . . . H263 H 0.0526 -0.0979 0.4725 0.0925 1.0000 Uiso . . . . . . H264 H 0.2091 -0.1362 0.4252 0.0747 1.0000 Uiso . . . . . . H265 H 0.2050 -0.0954 0.2563 0.0544 1.0000 Uiso . . . . . . H181 H -0.3008 0.1736 0.0702 0.0634 1.0000 Uiso . . . . . . H182 H -0.2924 0.1166 -0.0331 0.0634 1.0000 Uiso . . . . . . H171 H -0.3055 0.3148 -0.0513 0.0683 1.0000 Uiso . . . . . . H172 H -0.1942 0.3284 0.0505 0.0683 1.0000 Uiso . . . . . . H151 H -0.2061 0.4157 -0.1519 0.0670 1.0000 Uiso . . . . . . H152 H -0.0923 0.4232 -0.0518 0.0670 1.0000 Uiso . . . . . . H141 H -0.0459 0.4265 -0.1990 0.0710 1.0000 Uiso . . . . . . H142 H -0.1161 0.3116 -0.2405 0.0710 1.0000 Uiso . . . . . . H112 H 0.3902 0.0772 0.0645 0.0929 1.0000 Uiso . . . . . . H113 H 0.4967 0.0995 -0.0457 0.1314 1.0000 Uiso . . . . . . H114 H 0.4245 0.2020 -0.2041 0.1823 1.0000 Uiso . . . . . . H115 H 0.2517 0.2905 -0.2463 0.1423 1.0000 Uiso . . . . . . 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 0.03495(11) 0.02588(10) 0.03260(10) -0.00050(9) 0.00626(7) 0.00224(10) N1 0.0400(19) 0.043(2) 0.0375(19) -0.0054(15) 0.0066(15) -0.0065(17) O2 0.078(3) 0.044(2) 0.0418(18) -0.0084(16) -0.0089(17) 0.012(2) O3 0.081(3) 0.042(2) 0.047(2) -0.0002(16) -0.0019(19) 0.009(2) O4 0.082(3) 0.053(2) 0.045(2) -0.0197(18) 0.0068(19) -0.004(2) O5 0.0412(17) 0.057(2) 0.055(2) 0.0057(17) 0.0191(15) 0.0015(18) C6 0.053(3) 0.043(3) 0.070(3) -0.013(2) 0.029(3) -0.014(2) C7 0.057(4) 0.058(4) 0.102(5) -0.012(4) 0.040(4) -0.008(3) C8 0.075(6) 0.102(7) 0.143(9) -0.001(6) 0.067(6) -0.001(5) C9 0.142(10) 0.141(10) 0.178(12) 0.038(9) 0.132(10) 0.011(8) C10 0.125(8) 0.123(8) 0.112(7) 0.026(6) 0.088(7) -0.006(7) C11 0.088(5) 0.052(3) 0.074(4) 0.004(3) 0.050(4) -0.014(3) C12 0.082(5) 0.047(3) 0.059(3) 0.011(3) 0.025(3) -0.009(3) N13 0.064(3) 0.032(2) 0.051(2) 0.0064(17) 0.012(2) 0.000(2) C14 0.086(5) 0.034(3) 0.058(3) 0.016(2) 0.006(3) 0.006(3) C15 0.069(4) 0.030(2) 0.067(4) 0.004(2) -0.004(3) 0.013(3) N16 0.043(2) 0.038(2) 0.049(2) -0.0026(17) 0.0002(17) 0.0069(18) C17 0.044(3) 0.066(4) 0.060(3) -0.014(3) 0.000(2) 0.023(3) C18 0.034(2) 0.078(4) 0.048(3) 0.000(3) 0.0027(18) 0.011(3) N19 0.038(2) 0.048(2) 0.042(2) -0.0059(17) 0.0072(15) 0.0065(18) C20 0.051(3) 0.056(3) 0.046(3) -0.009(2) 0.022(2) -0.006(2) C21 0.055(3) 0.049(3) 0.038(2) -0.0062(18) 0.0191(19) -0.005(2) C22 0.085(4) 0.066(4) 0.049(3) 0.009(3) 0.040(3) 0.011(3) C23 0.115(6) 0.079(5) 0.041(3) 0.014(3) 0.034(4) 0.012(4) C24 0.089(5) 0.057(3) 0.039(3) 0.012(2) 0.013(3) 0.012(3) C25 0.056(3) 0.035(2) 0.044(2) 0.0050(18) 0.010(2) 0.006(2) C26 0.045(2) 0.0271(18) 0.0290(16) -0.0013(13) 0.0077(15) -0.0053(17) O27 0.0426(16) 0.0314(13) 0.0294(13) -0.0017(12) 0.0083(11) 0.0037(13) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nd1 . O27 . 2.383(3) yes Nd1 . N19 . 2.634(5) yes Nd1 . N16 . 2.617(4) yes Nd1 . N13 . 2.601(5) yes Nd1 . O5 . 2.235(4) yes Nd1 . O3 . 2.577(4) yes Nd1 . O2 . 2.553(4) yes Nd1 . N1 . 2.996(4) yes Nd1 . O27 2_555 2.398(3) yes N1 . O4 . 1.216(5) yes N1 . O3 . 1.248(6) yes N1 . O2 . 1.260(5) yes O5 . C6 . 1.306(7) yes C6 . C11 . 1.415(9) yes C6 . C7 . 1.421(9) yes C7 . H112 . 1.026 no C7 . C8 . 1.391(11) yes C8 . H113 . 1.011 no C8 . C9 . 1.387(16) yes C9 . H114 . 1.015 no C9 . C10 . 1.344(16) yes C10 . H115 . 1.019 no C10 . C11 . 1.411(10) yes C11 . C12 . 1.434(10) yes C12 . N13 . 1.282(8) yes N13 . C14 . 1.483(8) yes C14 . H142 . 1.005 no C14 . H141 . 1.006 no C14 . C15 . 1.486(11) yes C15 . H152 . 1.007 no C15 . H151 . 1.003 no C15 . N16 . 1.487(8) yes N16 . C17 . 1.469(8) yes C17 . H172 . 1.004 no C17 . H171 . 1.002 no C17 . C18 . 1.496(10) yes C18 . H182 . 1.006 no C18 . H181 . 1.004 no C18 . N19 . 1.478(6) yes N19 . C20 . 1.273(7) yes C20 . C21 . 1.447(8) yes C21 . C26 . 1.399(7) yes C21 . C22 . 1.423(7) yes C22 . H262 . 1.010 no C22 . C23 . 1.375(10) yes C23 . H263 . 1.009 no C23 . C24 . 1.379(11) yes C24 . H264 . 1.010 no C24 . C25 . 1.387(8) yes C25 . H265 . 1.010 no C25 . C26 . 1.383(6) yes C26 . O27 . 1.352(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O27 . Nd1 . N19 . 69.15(13) yes O27 . Nd1 . N16 . 128.69(13) yes N19 . Nd1 . N16 . 65.47(15) yes O27 . Nd1 . N13 . 149.16(13) yes N19 . Nd1 . N13 . 131.25(15) yes N16 . Nd1 . N13 . 65.83(16) yes O27 . Nd1 . O5 . 91.23(13) yes N19 . Nd1 . O5 . 157.16(14) yes N16 . Nd1 . O5 . 137.11(15) yes N13 . Nd1 . O5 . 71.53(15) yes O27 . Nd1 . O3 . 79.27(12) yes N19 . Nd1 . O3 . 82.36(15) yes N16 . Nd1 . O3 . 116.05(14) yes N13 . Nd1 . O3 . 121.71(15) yes O5 . Nd1 . O3 . 82.54(16) yes O27 . Nd1 . O2 . 124.61(12) yes N19 . Nd1 . O2 . 83.79(16) yes N16 . Nd1 . O2 . 72.77(13) yes N13 . Nd1 . O2 . 84.16(15) yes O5 . Nd1 . O2 . 98.98(16) yes O27 . Nd1 . N1 . 102.07(11) yes N19 . Nd1 . N1 . 82.54(13) yes N16 . Nd1 . N1 . 94.67(13) yes N13 . Nd1 . N1 . 103.45(14) yes O5 . Nd1 . N1 . 90.64(14) yes O27 . Nd1 . O27 2_555 71.32(11) yes N19 . Nd1 . O27 2_555 91.37(12) yes N16 . Nd1 . O27 2_555 86.91(12) yes N13 . Nd1 . O27 2_555 84.01(13) yes O5 . Nd1 . O27 2_555 93.27(13) yes O3 . Nd1 . O2 . 49.02(12) yes O3 . Nd1 . N1 . 24.41(12) yes O2 . Nd1 . N1 . 24.61(11) yes O3 . Nd1 . O27 2_555 150.21(11) yes O2 . Nd1 . O27 2_555 159.32(11) yes N1 . Nd1 . O27 2_555 172.38(11) yes O4 . N1 . O3 . 121.8(5) yes O4 . N1 . O2 . 122.1(5) yes O3 . N1 . O2 . 116.2(4) yes O4 . N1 . Nd1 . 178.6(4) yes O3 . N1 . Nd1 . 58.6(2) yes O2 . N1 . Nd1 . 57.6(2) yes N1 . O2 . Nd1 . 97.8(3) yes N1 . O3 . Nd1 . 97.0(3) yes C6 . O5 . Nd1 . 142.3(4) yes C11 . C6 . C7 . 118.4(6) yes C11 . C6 . O5 . 122.1(6) yes C7 . C6 . O5 . 119.5(6) yes H112 . C7 . C8 . 120.241 no H112 . C7 . C6 . 119.952 no C8 . C7 . C6 . 119.8(8) yes H113 . C8 . C9 . 118.192 no H113 . C8 . C7 . 120.052 no C9 . C8 . C7 . 121.8(9) yes H114 . C9 . C10 . 119.548 no H114 . C9 . C8 . 122.275 no C10 . C9 . C8 . 118.2(8) yes H115 . C10 . C11 . 116.668 no H115 . C10 . C9 . 119.467 no C11 . C10 . C9 . 123.9(9) yes C12 . C11 . C6 . 124.7(6) yes C12 . C11 . C10 . 117.3(7) yes C6 . C11 . C10 . 118.0(8) yes N13 . C12 . C11 . 127.1(6) yes C14 . N13 . C12 . 115.3(5) yes C14 . N13 . Nd1 . 116.3(4) yes C12 . N13 . Nd1 . 128.1(4) yes H142 . C14 . H141 . 108.545 no H142 . C14 . C15 . 109.493 no H141 . C14 . C15 . 109.902 no H142 . C14 . N13 . 108.877 no H141 . C14 . N13 . 108.802 no C15 . C14 . N13 . 111.2(5) yes H152 . C15 . H151 . 108.653 no H152 . C15 . N16 . 109.477 no H151 . C15 . N16 . 109.661 no H152 . C15 . C14 . 109.384 no H151 . C15 . C14 . 109.801 no N16 . C15 . C14 . 109.8(5) yes C17 . N16 . Nd1 . 111.1(3) yes C17 . N16 . C15 . 114.2(5) yes Nd1 . N16 . C15 . 108.9(3) yes H172 . C17 . H171 . 108.960 no H172 . C17 . C18 . 109.590 no H171 . C17 . C18 . 110.021 no H172 . C17 . N16 . 109.250 no H171 . C17 . N16 . 109.383 no C18 . C17 . N16 . 109.6(5) yes H182 . C18 . H181 . 108.630 no H182 . C18 . N19 . 109.381 no H181 . C18 . N19 . 109.491 no H182 . C18 . C17 . 109.882 no H181 . C18 . C17 . 110.207 no N19 . C18 . C17 . 109.2(5) yes C20 . N19 . C18 . 117.7(5) yes C20 . N19 . Nd1 . 126.9(4) yes C18 . N19 . Nd1 . 115.3(4) yes C21 . C20 . N19 . 124.7(5) yes C26 . C21 . C22 . 118.6(5) yes C26 . C21 . C20 . 124.0(4) yes C22 . C21 . C20 . 117.4(5) yes H262 . C22 . C23 . 119.513 no H262 . C22 . C21 . 119.219 no C23 . C22 . C21 . 121.2(6) yes H263 . C23 . C24 . 120.099 no H263 . C23 . C22 . 120.965 no C24 . C23 . C22 . 118.9(5) yes H264 . C24 . C25 . 119.694 no H264 . C24 . C23 . 119.507 no C25 . C24 . C23 . 120.8(6) yes H265 . C25 . C26 . 119.084 no H265 . C25 . C24 . 119.756 no C26 . C25 . C24 . 121.2(6) yes O27 . C26 . C25 . 119.6(4) yes O27 . C26 . C21 . 121.5(4) yes C25 . C26 . C21 . 118.9(4) yes Nd1 . O27 . Nd1 2_555 108.68(11) yes Nd1 . O27 . C26 . 122.4(2) yes Nd1 2_555 O27 . C26 . 123.9(3) yes # Attachment 'New_Complex2-Pr.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 672292' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _refine_special_details ; 'the residual electron density is localised around the metallic atoms Several absorption corrections have been tried but none gave a perfect result Then it has been choose to keep the one (multi-scan) given the best result.' ; _cell_length_a 12.8085(4) _cell_length_b 11.9086(6) _cell_length_c 13.8970(5) _cell_angle_alpha 90 _cell_angle_beta 110.368(2) _cell_angle_gamma 90 _cell_volume 1987.19(14) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Pr -0.2180 2.8214 22.0440 2.7739 19.6697 0.2221 12.3856 16.7669 2.8243 143.6440 2.0583 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C54 N9 O6 Pr3 # Dc = 2.16 Fooo = 1016.00 Mu = 36.93 M = 645.47 # Found Formula = C36 H38 N8 O10 Pr2 # Dc = 1.65 FOOO = 1016.00 Mu = 24.85 M = 492.32 _chemical_formula_sum 'C36 H38 N8 O10 Pr2' _chemical_formula_moiety 'C36 H38 N8 O10 Pr2' _chemical_compound_source ? _chemical_formula_weight 1024.56 # Structure does not match formula _cell_measurement_reflns_used 29377 _cell_measurement_theta_min 1 _cell_measurement_theta_max 38 _cell_measurement_temperature 120(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 2.485 # Sheldrick geometric approximatio 0.65 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.87 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120(2) _diffrn_reflns_number 30639 _reflns_number_total 10558 _diffrn_reflns_av_R_equivalents 0.100 # Number of reflections with Friedels Law is 10558 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10601 _diffrn_reflns_theta_min 1.864 _diffrn_reflns_theta_max 37.725 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 36.971 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -22 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.37 _refine_diff_density_max 3.47 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5396 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 _oxford_refine_ls_R_factor_ref 0.0528 _refine_ls_wR_factor_ref 0.0600 _refine_ls_goodness_of_fit_ref 1.0657 _refine_ls_shift/su_max 0.000862 # The values computed from all data _oxford_reflns_number_all 10538 _refine_ls_R_factor_all 0.0988 _refine_ls_wR_factor_all 0.1223 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6217 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_gt 0.0649 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.867 0.992 0.673 0.301 0.160 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pr1 Pr 0.51964(2) 0.16125(2) 0.527051(18) 0.0176 1.0000 Uani . . . . . . . O27 O 0.5414(3) -0.0198(3) 0.6069(2) 0.0205 1.0000 Uani . . . . . . . C26 C 0.5434(4) -0.0349(4) 0.7036(3) 0.0182 1.0000 Uani . . . . . . . C25 C 0.6371(4) -0.0828(4) 0.7771(4) 0.0238 1.0000 Uani . . . . . . . C24 C 0.6389(5) -0.1054(5) 0.8757(4) 0.0302 1.0000 Uani . . . . . . . C23 C 0.5468(6) -0.0823(6) 0.9031(4) 0.0370 1.0000 Uani . . . . . . . C22 C 0.4545(5) -0.0331(5) 0.8324(4) 0.0312 1.0000 Uani . . . . . . . C21 C 0.4524(4) -0.0043(5) 0.7331(4) 0.0249 1.0000 Uani . . . . . . . C20 C 0.3533(4) 0.0528(5) 0.6651(4) 0.0254 1.0000 Uani . . . . . . . N19 N 0.3510(3) 0.1165(4) 0.5901(3) 0.0224 1.0000 Uani . . . . . . . C18 C 0.2435(4) 0.1676(5) 0.5289(4) 0.0282 1.0000 Uani . . . . . . . C17 C 0.2622(4) 0.2821(5) 0.4907(4) 0.0305 1.0000 Uani . . . . . . . N16 N 0.3330(4) 0.2683(4) 0.4276(3) 0.0240 1.0000 Uani . . . . . . . C15 C 0.3606(5) 0.3773(4) 0.3899(4) 0.0289 1.0000 Uani . . . . . . . C14 C 0.4284(5) 0.3548(5) 0.3218(5) 0.0308 1.0000 Uani . . . . . . . N13 N 0.5297(4) 0.2875(4) 0.3766(3) 0.0260 1.0000 Uani . . . . . . . C12 C 0.6054(5) 0.2891(5) 0.3368(5) 0.0334 1.0000 Uani . . . . . . . C11 C 0.7118(5) 0.2303(5) 0.3721(5) 0.0318 1.0000 Uani . . . . . . . C10 C 0.7760(7) 0.2353(8) 0.3087(7) 0.0567 1.0000 Uani . . . . . . . C9 C 0.8784(7) 0.1856(9) 0.3346(8) 0.0617 1.0000 Uani . . . . . . . C8 C 0.9207(6) 0.1279(7) 0.4276(7) 0.0446 1.0000 Uani . . . . . . . C7 C 0.8603(5) 0.1214(5) 0.4927(5) 0.0318 1.0000 Uani . . . . . . . C6 C 0.7528(4) 0.1706(4) 0.4658(4) 0.0244 1.0000 Uani . . . . . . . O5 O 0.6953(3) 0.1606(3) 0.5272(3) 0.0250 1.0000 Uani . . . . . . . N1 N 0.5889(4) 0.3171(4) 0.7096(3) 0.0219 1.0000 Uani . . . . . . . O3 O 0.5229(3) 0.3481(3) 0.6218(3) 0.0298 1.0000 Uani . . . . . . . O2 O 0.6216(3) 0.2158(3) 0.7175(3) 0.0291 1.0000 Uani . . . . . . . O4 O 0.6192(4) 0.3821(4) 0.7825(3) 0.0305 1.0000 Uani . . . . . . . H251 H 0.6991 -0.0998 0.7596 0.0269 1.0000 Uiso R . . . . . . H241 H 0.7023 -0.1364 0.9239 0.0351 1.0000 Uiso R . . . . . . H231 H 0.5474 -0.0995 0.9684 0.0449 1.0000 Uiso R . . . . . . H221 H 0.3924 -0.0184 0.8503 0.0389 1.0000 Uiso R . . . . . . H201 H 0.2872 0.0429 0.6773 0.0309 1.0000 Uiso R . . . . . . H181 H 0.1957 0.1749 0.5696 0.0321 1.0000 Uiso R . . . . . . H182 H 0.2073 0.1198 0.4707 0.0319 1.0000 Uiso R . . . . . . H171 H 0.2983 0.3303 0.5481 0.0339 1.0000 Uiso R . . . . . . H172 H 0.1916 0.3148 0.4499 0.0339 1.0000 Uiso R . . . . . . H151 H 0.4027 0.4241 0.4474 0.0308 1.0000 Uiso R . . . . . . H152 H 0.2923 0.4151 0.3505 0.0307 1.0000 Uiso R . . . . . . H141 H 0.4509 0.4262 0.3012 0.0349 1.0000 Uiso R . . . . . . H142 H 0.3828 0.3144 0.2605 0.0347 1.0000 Uiso R . . . . . . H121 H 0.5914 0.3331 0.2781 0.0392 1.0000 Uiso R . . . . . . H101 H 0.7478 0.2735 0.2467 0.0729 1.0000 Uiso R . . . . . . H91 H 0.9188 0.1900 0.2912 0.0811 1.0000 Uiso R . . . . . . H81 H 0.9903 0.0936 0.4461 0.0572 1.0000 Uiso R . . . . . . H71 H 0.8903 0.0841 0.5553 0.0391 1.0000 Uiso R . . . . . . H27 H 0.2950 0.2275 0.3731 0.0330 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01820(9) 0.01439(9) 0.01725(9) -0.00054(10) 0.00231(6) 0.00065(11) O27 0.0246(14) 0.0150(13) 0.0185(13) -0.0010(11) 0.0031(11) 0.0012(12) C26 0.0264(19) 0.0112(17) 0.0152(15) 0.0005(12) 0.0052(14) -0.0016(14) C25 0.029(2) 0.0171(19) 0.0220(19) 0.0019(16) 0.0043(17) 0.0005(17) C24 0.042(3) 0.022(2) 0.022(2) 0.0061(18) 0.006(2) 0.007(2) C23 0.053(4) 0.035(3) 0.023(2) 0.006(2) 0.015(2) 0.006(3) C22 0.041(3) 0.030(3) 0.028(2) 0.0039(19) 0.019(2) 0.006(2) C21 0.029(2) 0.024(2) 0.0203(17) -0.0012(16) 0.0072(16) -0.0013(18) C20 0.025(2) 0.027(2) 0.025(2) -0.0043(18) 0.0097(17) 0.0015(18) N19 0.0205(16) 0.0234(19) 0.0210(16) -0.0004(14) 0.0043(13) 0.0040(15) C18 0.0193(17) 0.038(3) 0.023(2) 0.001(2) 0.0025(15) 0.003(2) C17 0.025(2) 0.034(3) 0.026(2) -0.001(2) 0.0007(18) 0.012(2) N16 0.0251(18) 0.0183(18) 0.0220(17) -0.0003(14) -0.0002(14) 0.0027(14) C15 0.032(2) 0.0153(19) 0.031(2) 0.0030(17) -0.0006(19) 0.0032(18) C14 0.037(3) 0.021(3) 0.030(2) 0.0049(19) 0.005(2) 0.000(2) N13 0.029(2) 0.0204(19) 0.0251(19) 0.0040(15) 0.0048(16) 0.0000(16) C12 0.039(3) 0.026(3) 0.034(3) 0.008(2) 0.011(2) -0.004(2) C11 0.036(3) 0.029(3) 0.035(3) 0.003(2) 0.018(2) -0.007(2) C10 0.060(5) 0.065(6) 0.058(5) 0.029(4) 0.036(4) 0.007(4) C9 0.052(4) 0.084(7) 0.067(5) 0.018(5) 0.044(4) 0.002(4) C8 0.034(3) 0.047(4) 0.061(4) 0.000(3) 0.028(3) 0.000(3) C7 0.026(2) 0.026(2) 0.044(3) -0.002(2) 0.013(2) -0.002(2) C6 0.0229(18) 0.018(2) 0.032(2) -0.0035(18) 0.0096(17) -0.0041(17) O5 0.0230(14) 0.0261(16) 0.0251(15) 0.0005(15) 0.0073(12) 0.0004(15) N1 0.0216(16) 0.0204(19) 0.0203(16) -0.0012(13) 0.0029(13) -0.0027(13) O3 0.0365(19) 0.0200(18) 0.0196(14) -0.0036(14) -0.0072(13) 0.0036(16) O2 0.0362(19) 0.0192(16) 0.0222(16) -0.0010(13) -0.0021(14) 0.0043(15) O4 0.038(2) 0.0250(19) 0.0211(16) -0.0057(14) 0.0012(15) 0.0006(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1504(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pr1 . O27 2_656 2.429(3) yes Pr1 . O27 . 2.396(4) yes Pr1 . N19 . 2.653(4) yes Pr1 . N16 . 2.636(4) yes Pr1 . N13 . 2.615(4) yes Pr1 . O5 . 2.249(3) yes Pr1 . O3 . 2.578(4) yes Pr1 . O2 . 2.594(4) yes O27 . C26 . 1.349(5) yes C26 . C25 . 1.398(7) yes C26 . C21 . 1.411(7) yes C25 . C24 . 1.389(7) yes C25 . H251 . 0.930 no C24 . C23 . 1.387(9) yes C24 . H241 . 0.931 no C23 . C22 . 1.377(9) yes C23 . H231 . 0.927 no C22 . C21 . 1.413(7) yes C22 . H221 . 0.928 no C21 . C20 . 1.460(7) yes C20 . N19 . 1.281(7) yes C20 . H201 . 0.926 no N19 . C18 . 1.475(6) yes C18 . C17 . 1.512(9) yes C18 . H181 . 0.972 no C18 . H182 . 0.964 no C17 . N16 . 1.474(7) yes C17 . H171 . 0.961 no C17 . H172 . 0.966 no N16 . C15 . 1.488(7) yes N16 . H27 . 0.890 no C15 . C14 . 1.515(9) yes C15 . H151 . 0.970 no C15 . H152 . 0.966 no C14 . N13 . 1.489(7) yes C14 . H141 . 0.973 no C14 . H142 . 0.975 no N13 . C12 . 1.273(8) yes C12 . C11 . 1.457(9) yes C12 . H121 . 0.933 no C11 . C10 . 1.399(9) yes C11 . C6 . 1.414(8) yes C10 . C9 . 1.368(12) yes C10 . H101 . 0.929 no C9 . C8 . 1.396(12) yes C9 . H91 . 0.923 no C8 . C7 . 1.383(9) yes C8 . H81 . 0.931 no C7 . C6 . 1.421(8) yes C7 . H71 . 0.932 no C6 . O5 . 1.313(6) yes N1 . O3 . 1.274(5) yes N1 . O2 . 1.269(6) yes N1 . O4 . 1.226(6) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O27 2_656 Pr1 . O27 . 71.64(12) yes O27 2_656 Pr1 . N19 . 91.81(13) yes O27 . Pr1 . N19 . 69.09(13) yes O27 2_656 Pr1 . N16 . 86.70(12) yes O27 . Pr1 . N16 . 128.01(13) yes N19 . Pr1 . N16 . 64.92(14) yes O27 2_656 Pr1 . N13 . 83.03(13) yes O27 . Pr1 . N13 . 149.03(14) yes N19 . Pr1 . N13 . 130.70(14) yes N16 . Pr1 . N13 . 65.85(15) yes O27 2_656 Pr1 . O5 . 93.06(13) yes O27 . Pr1 . O5 . 92.35(13) yes N19 . Pr1 . O5 . 158.17(13) yes N16 . Pr1 . O5 . 136.61(14) yes N13 . Pr1 . O5 . 71.06(14) yes O27 2_656 Pr1 . O3 . 158.99(11) yes O27 . Pr1 . O3 . 124.17(12) yes N19 . Pr1 . O3 . 82.83(14) yes N16 . Pr1 . O3 . 72.61(12) yes N13 . Pr1 . O3 . 85.15(14) yes O27 2_656 Pr1 . O2 . 150.33(12) yes O27 . Pr1 . O2 . 79.43(12) yes N19 . Pr1 . O2 . 83.80(14) yes N16 . Pr1 . O2 . 117.17(13) yes N13 . Pr1 . O2 . 121.65(14) yes O5 . Pr1 . O3 . 99.44(14) yes O5 . Pr1 . O2 . 81.45(14) yes O3 . Pr1 . O2 . 49.46(12) yes Pr1 2_656 O27 . Pr1 . 108.36(12) yes Pr1 2_656 O27 . C26 . 124.1(3) yes Pr1 . O27 . C26 . 122.7(3) yes O27 . C26 . C25 . 119.7(4) yes O27 . C26 . C21 . 121.6(4) yes C25 . C26 . C21 . 118.7(4) yes C26 . C25 . C24 . 120.9(5) yes C26 . C25 . H251 . 119.5 no C24 . C25 . H251 . 119.5 no C25 . C24 . C23 . 120.6(5) yes C25 . C24 . H241 . 119.8 no C23 . C24 . H241 . 119.6 no C24 . C23 . C22 . 119.3(5) yes C24 . C23 . H231 . 120.4 no C22 . C23 . H231 . 120.3 no C23 . C22 . C21 . 121.3(6) yes C23 . C22 . H221 . 119.5 no C21 . C22 . H221 . 119.2 no C22 . C21 . C26 . 118.9(5) yes C22 . C21 . C20 . 117.5(5) yes C26 . C21 . C20 . 123.5(4) yes C21 . C20 . N19 . 124.8(5) yes C21 . C20 . H201 . 117.8 no N19 . C20 . H201 . 117.4 no Pr1 . N19 . C20 . 126.7(3) yes Pr1 . N19 . C18 . 115.5(3) yes C20 . N19 . C18 . 117.8(4) yes N19 . C18 . C17 . 110.1(4) yes N19 . C18 . H181 . 110.6 no C17 . C18 . H181 . 109.4 no N19 . C18 . H182 . 108.7 no C17 . C18 . H182 . 109.1 no H181 . C18 . H182 . 109.0 no C18 . C17 . N16 . 108.2(4) yes C18 . C17 . H171 . 109.7 no N16 . C17 . H171 . 110.0 no C18 . C17 . H172 . 109.8 no N16 . C17 . H172 . 109.9 no H171 . C17 . H172 . 109.1 no Pr1 . N16 . C17 . 112.1(3) yes Pr1 . N16 . C15 . 108.9(3) yes C17 . N16 . C15 . 112.5(4) yes Pr1 . N16 . H27 . 108.1 no C17 . N16 . H27 . 107.4 no C15 . N16 . H27 . 107.6 no N16 . C15 . C14 . 108.9(4) yes N16 . C15 . H151 . 110.0 no C14 . C15 . H151 . 110.0 no N16 . C15 . H152 . 109.1 no C14 . C15 . H152 . 109.3 no H151 . C15 . H152 . 109.5 no C15 . C14 . N13 . 111.3(4) yes C15 . C14 . H141 . 108.7 no N13 . C14 . H141 . 109.1 no C15 . C14 . H142 . 109.5 no N13 . C14 . H142 . 109.4 no H141 . C14 . H142 . 108.8 no C14 . N13 . Pr1 . 116.2(4) yes C14 . N13 . C12 . 115.5(5) yes Pr1 . N13 . C12 . 127.8(4) yes N13 . C12 . C11 . 127.7(5) yes N13 . C12 . H121 . 116.3 no C11 . C12 . H121 . 116.0 no C12 . C11 . C10 . 116.9(6) yes C12 . C11 . C6 . 123.7(5) yes C10 . C11 . C6 . 119.3(6) yes C11 . C10 . C9 . 122.4(7) yes C11 . C10 . H101 . 118.7 no C9 . C10 . H101 . 118.9 no C10 . C9 . C8 . 119.0(7) yes C10 . C9 . H91 . 120.6 no C8 . C9 . H91 . 120.4 no C9 . C8 . C7 . 120.5(7) yes C9 . C8 . H81 . 119.8 no C7 . C8 . H81 . 119.7 no C8 . C7 . C6 . 121.1(6) yes C8 . C7 . H71 . 119.6 no C6 . C7 . H71 . 119.3 no C7 . C6 . C11 . 117.7(5) yes C7 . C6 . O5 . 120.2(5) yes C11 . C6 . O5 . 122.2(5) yes C6 . O5 . Pr1 . 141.8(3) yes O3 . N1 . O2 . 116.6(4) yes O3 . N1 . O4 . 121.5(4) yes O2 . N1 . O4 . 121.9(4) yes Pr1 . O3 . N1 . 97.3(3) yes Pr1 . O2 . N1 . 96.6(3) yes # Attachment 'New_Complex3-Sm.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 672291' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 12.8175(6) _cell_length_b 11.8739(4) _cell_length_c 13.7328(7) _cell_angle_alpha 90 _cell_angle_beta 110.205(2) _cell_angle_gamma 90 _cell_volume 1961.43(15) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Sm -0.1638 3.4418 24.0042 2.4727 19.4258 0.1965 13.4396 14.3996 2.8960 128.0070 2.2096 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C36 H36 N6 O4 Sm2 # Dc = 1.55 Fooo = 1028.00 Mu = 30.06 M = 458.76 # Found Formula = C36 H38 N8 O10 Sm2 # Dc = 1.77 FOOO = 1028.00 Mu = 30.30 M = 521.77 _chemical_formula_sum 'C36 H38 N8 O10 Sm2' _chemical_formula_moiety 'C36 H38 N8 O10 Sm2' _chemical_compound_source ? _chemical_formula_weight 1043.55 _cell_measurement_reflns_used 20642 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 120(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.11 _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 3.030 # Sheldrick geometric approximatio 0.76 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120(2) _diffrn_reflns_number 14195 _reflns_number_total 4589 _diffrn_reflns_av_R_equivalents 0.104 # Number of reflections with Friedels Law is 4589 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4630 _diffrn_reflns_theta_min 1.875 _diffrn_reflns_theta_max 27.772 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.938 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.09 _refine_diff_density_max 1.54 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2522 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 _oxford_refine_ls_R_factor_ref 0.0433 _refine_ls_wR_factor_ref 0.0419 _refine_ls_goodness_of_fit_ref 1.1345 _refine_ls_shift/su_max 0.000491 # The values computed from all data _oxford_reflns_number_all 4570 _refine_ls_R_factor_all 0.0983 _refine_ls_wR_factor_all 0.0789 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2522 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_gt 0.0419 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.309 0.148 0.195 0.752E-01 0.608E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Sm1 Sm 0.51638(3) 0.15909(4) 0.52628(3) 0.0210 1.0000 Uani . . . . . . . O27 O 0.5418(5) -0.0201(5) 0.6050(5) 0.0259 1.0000 Uani . . . . . . . C26 C 0.5476(7) -0.0351(7) 0.7035(6) 0.0235 1.0000 Uani . . . . . . . C25 C 0.6419(7) -0.0805(7) 0.7778(6) 0.0229 1.0000 Uani . . . . . . . C24 C 0.6454(8) -0.1046(7) 0.8769(7) 0.0304 1.0000 Uani . . . . . . . C23 C 0.5554(8) -0.0850(8) 0.9071(7) 0.0348 1.0000 Uani . . . . . . . C22 C 0.4617(8) -0.0371(7) 0.8362(7) 0.0327 1.0000 Uani . . . . . . . C21 C 0.4559(7) -0.0092(7) 0.7352(7) 0.0259 1.0000 Uani . . . . . . . C20 C 0.3569(7) 0.0492(7) 0.6680(6) 0.0263 1.0000 Uani . . . . . . . N19 N 0.3536(5) 0.1135(6) 0.5923(5) 0.0255 1.0000 Uani . . . . . . . C18 C 0.2449(6) 0.1643(9) 0.5324(6) 0.0275 1.0000 Uani . . . . . . . C17 C 0.2636(7) 0.2771(7) 0.4935(7) 0.0325 1.0000 Uani . . . . . . . N16 N 0.3343(6) 0.2670(6) 0.4296(5) 0.0288 1.0000 Uani . . . . . . . C15 C 0.3595(7) 0.3753(7) 0.3892(7) 0.0327 1.0000 Uani . . . . . . . C14 C 0.4301(7) 0.3526(8) 0.3237(6) 0.0293 1.0000 Uani . . . . . . . N13 N 0.5296(6) 0.2837(6) 0.3789(5) 0.0283 1.0000 Uani . . . . . . . C12 C 0.6077(7) 0.2868(7) 0.3407(7) 0.0317 1.0000 Uani . . . . . . . C11 C 0.7136(7) 0.2316(7) 0.3780(7) 0.0287 1.0000 Uani . . . . . . . C10 C 0.7819(9) 0.2407(11) 0.3170(9) 0.0544 1.0000 Uani . . . . . . . C9 C 0.8849(9) 0.1905(10) 0.3464(9) 0.0588 1.0000 Uani . . . . . . . C8 C 0.9228(8) 0.1298(8) 0.4377(9) 0.0466 1.0000 Uani . . . . . . . C7 C 0.8590(7) 0.1196(7) 0.4994(8) 0.0337 1.0000 Uani . . . . . . . C6 C 0.7520(6) 0.1668(8) 0.4712(6) 0.0275 1.0000 Uani . . . . . . . O5 O 0.6910(4) 0.1548(6) 0.5305(4) 0.0297 1.0000 Uani . . . . . . . N1 N 0.5862(6) 0.3140(7) 0.7083(6) 0.0315 1.0000 Uani . . . . . . . O3 O 0.5253(5) 0.3454(6) 0.6164(4) 0.0333 1.0000 Uani . . . . . . . O2 O 0.6134(5) 0.2102(4) 0.7164(4) 0.0293 1.0000 Uani . . . . . . . O4 O 0.6163(5) 0.3790(5) 0.7810(5) 0.0307 1.0000 Uani . . . . . . . H251 H 0.7039 -0.0951 0.7595 0.0270 1.0000 Uiso R . . . . . . H241 H 0.7106 -0.1348 0.9250 0.0349 1.0000 Uiso R . . . . . . H231 H 0.5573 -0.1034 0.9738 0.0410 1.0000 Uiso R . . . . . . H221 H 0.4006 -0.0230 0.8565 0.0398 1.0000 Uiso R . . . . . . H201 H 0.2911 0.0394 0.6815 0.0329 1.0000 Uiso R . . . . . . H181 H 0.1997 0.1721 0.5755 0.0330 1.0000 Uiso R . . . . . . H182 H 0.2074 0.1160 0.4738 0.0329 1.0000 Uiso R . . . . . . H171 H 0.3006 0.3255 0.5521 0.0371 1.0000 Uiso R . . . . . . H172 H 0.1930 0.3101 0.4535 0.0371 1.0000 Uiso R . . . . . . H151 H 0.3993 0.4237 0.4472 0.0349 1.0000 Uiso R . . . . . . H152 H 0.2914 0.4123 0.3480 0.0350 1.0000 Uiso R . . . . . . H141 H 0.4541 0.4242 0.3040 0.0341 1.0000 Uiso R . . . . . . H142 H 0.3860 0.3126 0.2617 0.0338 1.0000 Uiso R . . . . . . H121 H 0.5939 0.3302 0.2813 0.0360 1.0000 Uiso R . . . . . . H101 H 0.7564 0.2810 0.2551 0.0690 1.0000 Uiso R . . . . . . H91 H 0.9289 0.1972 0.3051 0.0771 1.0000 Uiso R . . . . . . H81 H 0.9925 0.0956 0.4581 0.0579 1.0000 Uiso R . . . . . . H71 H 0.8867 0.0806 0.5619 0.0410 1.0000 Uiso R . . . . . . H14 H 0.2964 0.2259 0.3745 0.0381 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02191(17) 0.01780(17) 0.02077(18) -0.0008(2) 0.00413(12) 0.0010(2) O27 0.032(3) 0.020(3) 0.023(3) -0.001(3) 0.007(3) 0.002(3) C26 0.030(4) 0.018(4) 0.019(4) -0.003(4) 0.004(3) 0.006(4) C25 0.026(4) 0.022(4) 0.020(4) 0.004(3) 0.006(3) 0.004(3) C24 0.037(5) 0.027(5) 0.025(4) 0.002(4) 0.007(4) -0.001(4) C23 0.053(6) 0.031(5) 0.018(4) 0.003(4) 0.009(4) 0.004(4) C22 0.040(5) 0.026(4) 0.037(5) -0.002(4) 0.019(4) 0.003(4) C21 0.029(5) 0.016(4) 0.032(5) -0.004(3) 0.010(4) 0.000(3) C20 0.033(5) 0.023(4) 0.026(4) -0.004(3) 0.014(4) -0.003(4) N19 0.018(3) 0.032(4) 0.024(3) -0.002(3) 0.005(3) 0.003(3) C18 0.019(4) 0.034(4) 0.029(4) 0.001(5) 0.008(3) -0.003(4) C17 0.025(4) 0.029(5) 0.038(5) 0.000(4) 0.004(4) 0.013(4) N16 0.027(4) 0.024(4) 0.026(4) -0.005(3) -0.003(3) 0.001(3) C15 0.026(4) 0.024(4) 0.038(5) 0.002(4) -0.002(4) 0.008(3) C14 0.032(4) 0.026(5) 0.026(4) -0.003(4) 0.005(3) -0.001(4) N13 0.033(4) 0.017(4) 0.028(4) 0.002(3) 0.002(3) 0.001(3) C12 0.040(5) 0.027(5) 0.024(4) 0.006(4) 0.005(4) 0.002(4) C11 0.031(5) 0.024(4) 0.031(5) -0.002(4) 0.011(4) -0.005(4) C10 0.056(7) 0.058(7) 0.059(7) 0.009(6) 0.031(6) 0.005(6) C9 0.050(7) 0.074(9) 0.068(8) 0.012(7) 0.042(6) 0.000(6) C8 0.038(6) 0.037(6) 0.071(8) 0.001(5) 0.027(5) 0.000(4) C7 0.032(5) 0.023(4) 0.047(5) -0.008(4) 0.014(4) -0.008(4) C6 0.026(4) 0.021(4) 0.036(4) -0.005(4) 0.012(3) -0.006(4) O5 0.026(3) 0.032(3) 0.034(3) 0.003(3) 0.014(2) 0.002(3) N1 0.017(3) 0.041(6) 0.037(4) -0.002(4) 0.011(3) -0.002(3) O3 0.040(3) 0.026(3) 0.022(3) -0.005(3) -0.005(2) 0.003(4) O2 0.043(4) 0.010(3) 0.024(3) 0.000(2) -0.001(3) 0.004(2) O4 0.036(4) 0.029(3) 0.024(3) -0.006(3) 0.007(3) -0.004(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.06529(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sm1 . O27 2_656 2.366(6) yes Sm1 . O27 . 2.358(6) yes Sm1 . N19 . 2.603(7) yes Sm1 . N16 . 2.591(7) yes Sm1 . N13 . 2.560(7) yes Sm1 . O5 . 2.220(5) yes Sm1 . O3 . 2.518(7) yes Sm1 . O2 . 2.548(5) yes O27 . C26 . 1.341(9) yes C26 . C25 . 1.393(11) yes C26 . C21 . 1.421(11) yes C25 . C24 . 1.376(11) yes C25 . H251 . 0.929 no C24 . C23 . 1.375(13) yes C24 . H241 . 0.938 no C23 . C22 . 1.380(12) yes C23 . H231 . 0.933 no C22 . C21 . 1.403(12) yes C22 . H221 . 0.933 no C21 . C20 . 1.460(12) yes C20 . N19 . 1.278(10) yes C20 . H201 . 0.931 no N19 . C18 . 1.480(10) yes C18 . C17 . 1.492(13) yes C18 . H181 . 0.965 no C18 . H182 . 0.970 no C17 . N16 . 1.469(11) yes C17 . H171 . 0.969 no C17 . H172 . 0.965 no N16 . C15 . 1.480(11) yes N16 . H14 . 0.890 no C15 . C14 . 1.505(12) yes C15 . H151 . 0.972 no C15 . H152 . 0.966 no C14 . N13 . 1.484(11) yes C14 . H141 . 0.974 no C14 . H142 . 0.968 no N13 . C12 . 1.281(11) yes C12 . C11 . 1.433(12) yes C12 . H121 . 0.929 no C11 . C10 . 1.408(13) yes C11 . C6 . 1.427(12) yes C10 . C9 . 1.376(15) yes C10 . H101 . 0.932 no C9 . C8 . 1.381(15) yes C9 . H91 . 0.931 no C8 . C7 . 1.372(13) yes C8 . H81 . 0.932 no C7 . C6 . 1.406(12) yes C7 . H71 . 0.931 no C6 . O5 . 1.317(9) yes N1 . O3 . 1.288(9) yes N1 . O2 . 1.276(9) yes N1 . O4 . 1.214(9) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O27 2_656 Sm1 . O27 . 71.2(2) yes O27 2_656 Sm1 . N19 . 92.3(2) yes O27 . Sm1 . N19 . 69.7(2) yes O27 2_656 Sm1 . N16 . 87.9(2) yes O27 . Sm1 . N16 . 129.7(2) yes N19 . Sm1 . N16 . 66.0(2) yes O27 2_656 Sm1 . N13 . 83.7(2) yes O27 . Sm1 . N13 . 148.0(2) yes N19 . Sm1 . N13 . 132.5(2) yes N16 . Sm1 . N13 . 66.6(2) yes O27 2_656 Sm1 . O5 . 93.1(2) yes O27 . Sm1 . O5 . 89.4(2) yes N19 . Sm1 . O5 . 155.3(2) yes N16 . Sm1 . O5 . 138.3(2) yes N13 . Sm1 . O5 . 72.1(2) yes O27 2_656 Sm1 . O3 . 159.4(2) yes O27 . Sm1 . O3 . 126.31(18) yes N19 . Sm1 . O3 . 85.3(2) yes N16 . Sm1 . O3 . 72.4(2) yes N13 . Sm1 . O3 . 82.9(2) yes O27 2_656 Sm1 . O2 . 149.39(19) yes O27 . Sm1 . O2 . 78.69(19) yes N19 . Sm1 . O2 . 81.9(2) yes N16 . Sm1 . O2 . 116.2(2) yes N13 . Sm1 . O2 . 122.0(2) yes O5 . Sm1 . O3 . 97.6(2) yes O5 . Sm1 . O2 . 81.3(2) yes O3 . Sm1 . O2 . 50.49(18) yes Sm1 2_656 O27 . Sm1 . 108.8(2) yes Sm1 2_656 O27 . C26 . 124.7(5) yes Sm1 . O27 . C26 . 122.2(5) yes O27 . C26 . C25 . 121.4(8) yes O27 . C26 . C21 . 121.2(7) yes C25 . C26 . C21 . 117.3(8) yes C26 . C25 . C24 . 121.9(8) yes C26 . C25 . H251 . 118.8 no C24 . C25 . H251 . 119.3 no C25 . C24 . C23 . 121.3(8) yes C25 . C24 . H241 . 119.5 no C23 . C24 . H241 . 119.2 no C24 . C23 . C22 . 118.2(8) yes C24 . C23 . H231 . 121.1 no C22 . C23 . H231 . 120.7 no C23 . C22 . C21 . 122.1(9) yes C23 . C22 . H221 . 118.7 no C21 . C22 . H221 . 119.3 no C26 . C21 . C22 . 119.0(8) yes C26 . C21 . C20 . 122.6(8) yes C22 . C21 . C20 . 118.3(8) yes C21 . C20 . N19 . 125.1(8) yes C21 . C20 . H201 . 117.6 no N19 . C20 . H201 . 117.3 no Sm1 . N19 . C20 . 127.0(5) yes Sm1 . N19 . C18 . 115.8(5) yes C20 . N19 . C18 . 117.1(7) yes N19 . C18 . C17 . 109.2(6) yes N19 . C18 . H181 . 110.3 no C17 . C18 . H181 . 109.7 no N19 . C18 . H182 . 108.8 no C17 . C18 . H182 . 109.3 no H181 . C18 . H182 . 109.6 no C18 . C17 . N16 . 110.4(7) yes C18 . C17 . H171 . 109.2 no N16 . C17 . H171 . 108.6 no C18 . C17 . H172 . 109.5 no N16 . C17 . H172 . 110.1 no H171 . C17 . H172 . 109.0 no Sm1 . N16 . C17 . 111.5(5) yes Sm1 . N16 . C15 . 110.3(5) yes C17 . N16 . C15 . 114.3(7) yes Sm1 . N16 . H14 . 107.2 no C17 . N16 . H14 . 106.6 no C15 . N16 . H14 . 106.5 no N16 . C15 . C14 . 108.8(7) yes N16 . C15 . H151 . 109.0 no C14 . C15 . H151 . 110.0 no N16 . C15 . H152 . 110.1 no C14 . C15 . H152 . 109.9 no H151 . C15 . H152 . 108.9 no C15 . C14 . N13 . 112.4(7) yes C15 . C14 . H141 . 108.8 no N13 . C14 . H141 . 109.0 no C15 . C14 . H142 . 108.9 no N13 . C14 . H142 . 108.5 no H141 . C14 . H142 . 109.3 no C14 . N13 . Sm1 . 116.3(5) yes C14 . N13 . C12 . 115.5(7) yes Sm1 . N13 . C12 . 127.9(6) yes N13 . C12 . C11 . 128.2(8) yes N13 . C12 . H121 . 115.8 no C11 . C12 . H121 . 116.0 no C12 . C11 . C10 . 117.3(9) yes C12 . C11 . C6 . 123.9(8) yes C10 . C11 . C6 . 118.8(8) yes C11 . C10 . C9 . 121.5(11) yes C11 . C10 . H101 . 119.2 no C9 . C10 . H101 . 119.2 no C10 . C9 . C8 . 119.5(10) yes C10 . C9 . H91 . 120.4 no C8 . C9 . H91 . 120.1 no C9 . C8 . C7 . 120.6(10) yes C9 . C8 . H81 . 120.0 no C7 . C8 . H81 . 119.4 no C8 . C7 . C6 . 121.8(9) yes C8 . C7 . H71 . 119.6 no C6 . C7 . H71 . 118.6 no C11 . C6 . C7 . 117.6(8) yes C11 . C6 . O5 . 121.2(7) yes C7 . C6 . O5 . 121.1(8) yes C6 . O5 . Sm1 . 142.2(5) yes O3 . N1 . O2 . 114.8(7) yes O3 . N1 . O4 . 122.3(8) yes O2 . N1 . O4 . 122.8(7) yes Sm1 . O3 . N1 . 97.9(5) yes Sm1 . O2 . N1 . 96.8(5) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C25 . H251 . O4 3_646 175 0.93 2.57 3.495(13) yes C18 . H182 . O4 4_454 141 0.97 2.50 3.312(13) yes C15 . H151 . O3 . 122 0.97 2.51 3.131(13) yes N16 . H14 . O4 4_454 146 0.89 2.55 3.322(13) yes # Attachment 'New_Complex4-Tb.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 664111' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _refine_special_details ; 'the residual electron density is localised around the metallic atoms. Several absorption corrections have been tried but none gave a perfect result. Then it has been choose to keep the one (multi-scan) given the best result. The program SQUEEZE has been used in order to identify if there was any solvent in voids in the structure. It appears that the solvent atoms (if there is any) are too disordered to be refined.' ; _cell_length_a 11.1489(11) _cell_length_b 13.4793(9) _cell_length_c 13.6232(12) _cell_angle_alpha 90 _cell_angle_beta 94.018(4) _cell_angle_gamma 90 _cell_volume 2042.3(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C36 H38 Cl2 N6 O4 Tb2 # Dc = 1.64 Fooo = 984.00 Mu = 36.08 M = 503.75 # Found Formula = C36 H38 Cl2 N6 O4 Tb2 # Dc = 1.64 FOOO = 984.00 Mu = 36.08 M = 503.75 _chemical_formula_sum 'C36 H38 Cl2 N6 O4 Tb2' _chemical_formula_moiety 'C36 H38 Cl2 N6 O4 Tb2' _chemical_compound_source ? _chemical_formula_weight 1007.47 _cell_measurement_reflns_used 3342 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 290(1) _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.27 _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 3.608 # Sheldrick geometric approximatio 0.40 0.48 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.48 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 290(1) _diffrn_reflns_number 6842 _reflns_number_total 4343 _diffrn_reflns_av_R_equivalents 0.035 # Number of reflections with Friedels Law is 4343 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4903 _diffrn_reflns_theta_min 1.831 _diffrn_reflns_theta_max 27.999 _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 25.199 _diffrn_measured_fraction_theta_full 0.961 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.79 _refine_diff_density_max 2.24 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 2885 _refine_ls_number_restraints 0 _refine_ls_number_parameters 226 _oxford_refine_ls_R_factor_ref 0.0572 _refine_ls_wR_factor_ref 0.0657 _refine_ls_goodness_of_fit_ref 1.0885 _refine_ls_shift/su_max 0.001702 # The values computed from all data _oxford_reflns_number_all 4313 _refine_ls_R_factor_all 0.0864 _refine_ls_wR_factor_all 0.0866 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3112 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_gt 0.0684 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.30 0.995 0.869 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Tb1 Tb 1.01879(3) -0.13725(3) -0.01353(2) 0.0401 1.0000 Uani . . . . . . . Cl1 Cl 1.1347(2) -0.2695(2) -0.11722(18) 0.0698 1.0000 Uani . . . . . . . O27 O 1.0402(5) 0.0153(4) -0.0924(4) 0.0438 1.0000 Uani . . . . . . . C26 C 1.1271(8) 0.0323(6) -0.1563(6) 0.0475 1.0000 Uani . . . . . . . C25 C 1.0920(8) 0.0655(6) -0.2506(6) 0.0492 1.0000 Uani . . . . . . . C24 C 1.1799(11) 0.0909(8) -0.3139(7) 0.0673 1.0000 Uani . . . . . . . C23 C 1.3004(11) 0.0816(9) -0.2859(8) 0.0795 1.0000 Uani . . . . . . . C22 C 1.3359(9) 0.0460(7) -0.1941(8) 0.0634 1.0000 Uani . . . . . . . C21 C 1.2504(8) 0.0164(6) -0.1283(6) 0.0478 1.0000 Uani . . . . . . . C20 C 1.2937(8) -0.0255(6) -0.0343(7) 0.0517 1.0000 Uani . . . . . . . N19 N 1.2339(6) -0.0752(5) 0.0229(5) 0.0497 1.0000 Uani . . . . . . . C18 C 1.2934(9) -0.1127(8) 0.1161(7) 0.0615 1.0000 Uani . . . . . . . C17 C 1.2561(9) -0.2149(8) 0.1319(7) 0.0648 1.0000 Uani . . . . . . . N16 N 1.1247(6) -0.2212(5) 0.1340(5) 0.0472 1.0000 Uani . . . . . . . C15 C 1.0740(10) -0.3207(7) 0.1422(7) 0.0606 1.0000 Uani . . . . . . . C14 C 0.9428(10) -0.3150(7) 0.1522(7) 0.0614 1.0000 Uani . . . . . . . N13 N 0.8845(7) -0.2562(5) 0.0687(5) 0.0513 1.0000 Uani . . . . . . . C12 C 0.7709(9) -0.2675(6) 0.0524(6) 0.0531 1.0000 Uani . . . . . . . C11 C 0.6935(8) -0.2248(6) -0.0274(7) 0.0522 1.0000 Uani . . . . . . . C10 C 0.5702(9) -0.2443(8) -0.0268(9) 0.0693 1.0000 Uani . . . . . . . C9 C 0.4893(9) -0.2129(9) -0.1040(11) 0.0811 1.0000 Uani . . . . . . . C8 C 0.5351(9) -0.1632(9) -0.1815(9) 0.0718 1.0000 Uani . . . . . . . C7 C 0.6536(9) -0.1413(8) -0.1838(8) 0.0622 1.0000 Uani . . . . . . . C6 C 0.7379(8) -0.1686(7) -0.1064(7) 0.0533 1.0000 Uani . . . . . . . O5 O 0.8520(6) -0.1470(5) -0.1078(4) 0.0538 1.0000 Uani . . . . . . . H251 H 1.0109 0.0712 -0.2706 0.0589 1.0000 Uiso R . . . . . . H241 H 1.1568 0.1145 -0.3764 0.0821 1.0000 Uiso R . . . . . . H231 H 1.3577 0.0993 -0.3290 0.0970 1.0000 Uiso R . . . . . . H221 H 1.4175 0.0412 -0.1748 0.0771 1.0000 Uiso R . . . . . . H201 H 1.3742 -0.0145 -0.0149 0.0622 1.0000 Uiso R . . . . . . H181 H 1.3797 -0.1098 0.1130 0.0730 1.0000 Uiso R . . . . . . H182 H 1.2705 -0.0718 0.1706 0.0729 1.0000 Uiso R . . . . . . H171 H 1.2930 -0.2391 0.1936 0.0771 1.0000 Uiso R . . . . . . H172 H 1.2817 -0.2561 0.0790 0.0771 1.0000 Uiso R . . . . . . H151 H 1.1123 -0.3528 0.1994 0.0720 1.0000 Uiso R . . . . . . H152 H 1.0891 -0.3588 0.0841 0.0719 1.0000 Uiso R . . . . . . H141 H 0.9089 -0.3812 0.1509 0.0740 1.0000 Uiso R . . . . . . H142 H 0.9279 -0.2834 0.2142 0.0740 1.0000 Uiso R . . . . . . H121 H 0.7330 -0.3075 0.0963 0.0639 1.0000 Uiso R . . . . . . H101 H 0.5415 -0.2783 0.0259 0.0841 1.0000 Uiso R . . . . . . H91 H 0.4073 -0.2258 -0.1028 0.0971 1.0000 Uiso R . . . . . . H81 H 0.4827 -0.1436 -0.2341 0.0850 1.0000 Uiso R . . . . . . H71 H 0.6799 -0.1072 -0.2379 0.0740 1.0000 Uiso R . . . . . . H21 H 1.1053 -0.1876 0.1866 0.0700 1.0000 Uiso 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 Tb1 0.0431(2) 0.0384(2) 0.0387(2) 0.00218(15) 0.00232(13) -0.00092(17) Cl1 0.0739(16) 0.0771(16) 0.0582(13) -0.0112(11) 0.0041(11) 0.0083(13) O27 0.042(3) 0.048(3) 0.041(3) 0.006(2) 0.005(2) 0.004(2) C26 0.066(5) 0.035(3) 0.043(4) 0.001(3) 0.016(4) -0.009(4) C25 0.062(5) 0.044(4) 0.043(4) 0.005(3) 0.009(3) 0.008(4) C24 0.094(8) 0.057(5) 0.054(5) 0.014(4) 0.026(5) 0.004(6) C23 0.089(8) 0.084(8) 0.072(6) 0.024(6) 0.046(6) -0.002(7) C22 0.056(5) 0.052(5) 0.085(7) 0.011(4) 0.025(5) -0.011(4) C21 0.049(5) 0.048(4) 0.046(4) -0.006(3) 0.003(3) -0.007(4) C20 0.043(4) 0.041(4) 0.072(6) -0.003(4) 0.007(4) -0.005(4) N19 0.044(3) 0.051(4) 0.053(4) -0.001(3) -0.004(3) -0.001(3) C18 0.052(5) 0.082(7) 0.049(5) 0.015(4) -0.015(4) -0.001(5) C17 0.069(6) 0.073(6) 0.052(5) 0.014(4) -0.003(4) 0.012(5) N16 0.055(4) 0.043(3) 0.043(3) 0.004(3) -0.005(3) 0.012(3) C15 0.085(7) 0.045(4) 0.051(5) 0.012(4) -0.003(4) 0.011(5) C14 0.090(7) 0.046(5) 0.048(5) 0.017(4) 0.002(4) -0.004(5) N13 0.063(5) 0.050(4) 0.042(3) 0.002(3) 0.012(3) -0.009(3) C12 0.064(5) 0.044(4) 0.053(4) -0.004(3) 0.017(4) -0.003(4) C11 0.048(5) 0.035(4) 0.074(5) -0.005(4) 0.010(4) 0.001(4) C10 0.052(6) 0.062(6) 0.096(8) -0.014(5) 0.022(5) -0.007(5) C9 0.037(5) 0.073(7) 0.133(11) -0.023(7) 0.004(6) -0.006(5) C8 0.046(5) 0.076(7) 0.091(8) -0.015(6) -0.012(5) 0.016(5) C7 0.052(5) 0.067(6) 0.067(6) -0.013(4) -0.004(4) 0.002(4) C6 0.048(5) 0.046(4) 0.065(5) -0.010(4) 0.002(4) -0.002(4) O5 0.048(3) 0.065(4) 0.049(3) 0.003(3) 0.000(2) -0.010(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2098(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Tb1 . O27 2_755 2.313(5) yes Tb1 . Cl1 . 2.665(3) yes Tb1 . O27 . 2.340(5) yes Tb1 . N19 . 2.555(7) yes Tb1 . N16 . 2.526(6) yes Tb1 . N13 . 2.511(7) yes Tb1 . O5 . 2.189(6) yes O27 . C26 . 1.367(9) yes C26 . C25 . 1.390(11) yes C26 . C21 . 1.417(13) yes C25 . C24 . 1.392(12) yes C25 . H251 . 0.930 no C24 . C23 . 1.377(16) yes C24 . H241 . 0.928 no C23 . C22 . 1.371(15) yes C23 . H231 . 0.929 no C22 . C21 . 1.411(12) yes C22 . H221 . 0.931 no C21 . C20 . 1.452(13) yes C20 . N19 . 1.254(11) yes C20 . H201 . 0.930 no N19 . C18 . 1.481(11) yes C18 . C17 . 1.460(15) yes C18 . H181 . 0.967 no C18 . H182 . 0.973 no C17 . N16 . 1.470(12) yes C17 . H171 . 0.965 no C17 . H172 . 0.969 no N16 . C15 . 1.462(12) yes N16 . H21 . 0.887 no C15 . C14 . 1.481(15) yes C15 . H151 . 0.965 no C15 . H152 . 0.967 no C14 . N13 . 1.497(11) yes C14 . H141 . 0.969 no C14 . H142 . 0.970 no N13 . C12 . 1.279(12) yes C12 . C11 . 1.459(14) yes C12 . H121 . 0.928 no C11 . C10 . 1.401(13) yes C11 . C6 . 1.431(13) yes C10 . C9 . 1.403(17) yes C10 . H101 . 0.927 no C9 . C8 . 1.378(18) yes C9 . H91 . 0.932 no C8 . C7 . 1.356(15) yes C8 . H81 . 0.931 no C7 . C6 . 1.411(14) yes C7 . H71 . 0.933 no C6 . O5 . 1.306(11) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O27 2_755 Tb1 . Cl1 . 167.40(16) yes O27 2_755 Tb1 . O27 . 72.8(2) yes Cl1 . Tb1 . O27 . 106.01(14) yes O27 2_755 Tb1 . N19 . 87.1(2) yes Cl1 . Tb1 . N19 . 80.71(17) yes O27 . Tb1 . N19 . 71.2(2) yes O27 2_755 Tb1 . N16 . 87.7(2) yes Cl1 . Tb1 . N16 . 84.56(16) yes O27 . Tb1 . N16 . 134.6(2) yes N19 . Tb1 . N16 . 67.2(2) yes O27 2_755 Tb1 . N13 . 88.4(2) yes Cl1 . Tb1 . N13 . 97.79(18) yes O27 . Tb1 . N13 . 148.1(2) yes N19 . Tb1 . N13 . 134.7(2) yes N16 . Tb1 . N13 . 67.6(2) yes O27 2_755 Tb1 . O5 . 98.1(2) yes Cl1 . Tb1 . O5 . 94.16(18) yes O27 . Tb1 . O5 . 83.9(2) yes N19 . Tb1 . O5 . 151.7(2) yes N16 . Tb1 . O5 . 140.4(2) yes N13 . Tb1 . O5 . 73.4(2) yes Tb1 . O27 . Tb1 2_755 107.2(2) yes Tb1 . O27 . C26 . 122.7(5) yes Tb1 2_755 O27 . C26 . 121.5(5) yes O27 . C26 . C25 . 118.5(8) yes O27 . C26 . C21 . 121.4(7) yes C25 . C26 . C21 . 120.1(7) yes C26 . C25 . C24 . 119.2(9) yes C26 . C25 . H251 . 120.1 no C24 . C25 . H251 . 120.7 no C25 . C24 . C23 . 121.4(9) yes C25 . C24 . H241 . 119.4 no C23 . C24 . H241 . 119.2 no C24 . C23 . C22 . 120.0(8) yes C24 . C23 . H231 . 120.1 no C22 . C23 . H231 . 119.9 no C23 . C22 . C21 . 120.8(9) yes C23 . C22 . H221 . 119.7 no C21 . C22 . H221 . 119.4 no C26 . C21 . C22 . 118.2(8) yes C26 . C21 . C20 . 123.6(7) yes C22 . C21 . C20 . 118.2(8) yes C21 . C20 . N19 . 126.7(8) yes C21 . C20 . H201 . 116.2 no N19 . C20 . H201 . 117.1 no Tb1 . N19 . C20 . 126.0(6) yes Tb1 . N19 . C18 . 114.4(5) yes C20 . N19 . C18 . 119.3(8) yes N19 . C18 . C17 . 109.5(8) yes N19 . C18 . H181 . 109.6 no C17 . C18 . H181 . 109.8 no N19 . C18 . H182 . 109.6 no C17 . C18 . H182 . 109.3 no H181 . C18 . H182 . 109.0 no C18 . C17 . N16 . 110.6(8) yes C18 . C17 . H171 . 109.8 no N16 . C17 . H171 . 109.2 no C18 . C17 . H172 . 109.2 no N16 . C17 . H172 . 109.1 no H171 . C17 . H172 . 109.0 no C17 . N16 . Tb1 . 111.7(5) yes C17 . N16 . C15 . 116.4(7) yes Tb1 . N16 . C15 . 108.1(5) yes C17 . N16 . H21 . 106.6 no Tb1 . N16 . H21 . 106.7 no C15 . N16 . H21 . 106.9 no N16 . C15 . C14 . 110.4(8) yes N16 . C15 . H151 . 108.8 no C14 . C15 . H151 . 109.4 no N16 . C15 . H152 . 109.6 no C14 . C15 . H152 . 109.4 no H151 . C15 . H152 . 109.2 no C15 . C14 . N13 . 109.6(7) yes C15 . C14 . H141 . 109.7 no N13 . C14 . H141 . 109.0 no C15 . C14 . H142 . 109.5 no N13 . C14 . H142 . 109.7 no H141 . C14 . H142 . 109.3 no C14 . N13 . Tb1 . 115.9(6) yes C14 . N13 . C12 . 116.2(7) yes Tb1 . N13 . C12 . 127.8(6) yes N13 . C12 . C11 . 127.5(8) yes N13 . C12 . H121 . 116.5 no C11 . C12 . H121 . 115.9 no C12 . C11 . C10 . 116.8(9) yes C12 . C11 . C6 . 123.5(8) yes C10 . C11 . C6 . 119.7(9) yes C11 . C10 . C9 . 121.2(11) yes C11 . C10 . H101 . 119.4 no C9 . C10 . H101 . 119.4 no C10 . C9 . C8 . 117.9(9) yes C10 . C9 . H91 . 120.7 no C8 . C9 . H91 . 121.4 no C9 . C8 . C7 . 122.5(11) yes C9 . C8 . H81 . 118.8 no C7 . C8 . H81 . 118.7 no C8 . C7 . C6 . 121.6(11) yes C8 . C7 . H71 . 119.1 no C6 . C7 . H71 . 119.3 no C11 . C6 . C7 . 116.9(9) yes C11 . C6 . O5 . 121.1(8) yes C7 . C6 . O5 . 121.9(9) yes C6 . O5 . Tb1 . 142.4(6) yes