# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'Cif-global.cif' # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in Dalton Transactions ; _publ_contact_author ; Jean-Pierre Costes ; _publ_contact_author_address ; Laboratoire de Chimie de Coordination 205 Route de Narbonne 31077 Toulouse Cedex 04 ; _publ_contact_author_email Jean-Pierre.Costes@lcc-toulouse.fr #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ;Structural and Magnetic Studies of original tetranuclear CoII-LnIII complexes (LnIII = Gd, Tb, Y) ; loop_ _publ_author_name _publ_author_address J.-P.Costes ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; 'Laure Vendier' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; 'Wolfgang Wernsdorfer' ; Institut N\'eel CNRS & Universit\'e J. Fourier BP 166 38042 GRENOBLE Cedex, France ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Gottingen, Germany. MULTI SCAN - c.f. r.h. blessing, acta cryst. (1995), a51, 33-38 WINGX - 1.63 Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-Ray Diffraction Data. Farrugia, L. J. Appl. Crystallogr., 1999, 32, 837. ORTEP3 for Windows, Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565.; ; _publ_contact_author_name 'Jean-Pierre Costes' # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # =====END data_complex(2) _database_code_depnum_ccdc_archive 'CCDC 793512' #TrackingRef 'Cif-global.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H30 Co2 N4 O26 Tb2, 4(C3 H6 O)' _chemical_formula_sum 'C44 H54 Co2 N4 O30 Tb2' _chemical_formula_weight 1554.63 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4478(10) _cell_length_b 20.0927(19) _cell_length_c 13.3732(13) _cell_angle_alpha 90 _cell_angle_beta 92.491(11) _cell_angle_gamma 90 _cell_volume 2804.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.275 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.167 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.322 _exptl_absorpt_correction_T_max 0.619 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 4 _diffrn_standards_decay_% 0.1 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_number 26129 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _reflns_number_total 4985 _reflns_number_gt 4092 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4985 _refine_ls_number_parameters 379 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.06 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.667 _refine_diff_density_min -1.096 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3766(4) 0.9726(2) 0.9239(3) 0.0391(10) Uani 1 1 d . . . H1 H 0.4598 0.9904 0.9161 0.047 Uiso 1 1 calc R . . C2 C 0.3337(3) 0.92440(19) 0.8518(3) 0.0308(8) Uani 1 1 d . . . C3 C 0.2133(3) 0.89305(17) 0.8522(3) 0.0232(7) Uani 1 1 d . . . C4 C -0.1874(4) 1.15699(18) 1.2207(3) 0.0306(8) Uani 1 1 d . . . C5 C -0.2733(4) 1.1717(2) 1.2927(3) 0.0467(11) Uani 1 1 d . . . H5 H -0.2524 1.2042 1.3423 0.056 Uiso 1 1 calc R . . C6 C -0.3906(4) 1.1391(3) 1.2928(4) 0.0566(14) Uani 1 1 d . . . H6 H -0.4499 1.1496 1.3423 0.068 Uiso 1 1 calc R . . C7 C 0.4205(4) 0.9076(2) 0.7775(3) 0.0462(11) Uani 1 1 d . . . H7 H 0.5011 0.9295 0.7769 0.055 Uiso 1 1 calc R . . C8 C -0.0448(4) 1.2426(2) 1.2787(3) 0.0426(10) Uani 1 1 d . . . H8A H -0.0436 1.2266 1.348 0.064 Uiso 1 1 calc R . . H8B H -0.1119 1.2763 1.2689 0.064 Uiso 1 1 calc R . . H8C H 0.0385 1.2622 1.2651 0.064 Uiso 1 1 calc R . . C9 C 0.2392(3) 1.13019(17) 1.3091(3) 0.0276(8) Uani 1 1 d . . . H9 H 0.2702 1.1541 1.3665 0.033 Uiso 1 1 calc R . . C10 C 0.2607(3) 1.05968(16) 1.3096(2) 0.0220(7) Uani 1 1 d . . . C11 C 0.2180(3) 1.01800(15) 1.2296(2) 0.0196(7) Uani 1 1 d . . . C12 C 0.2566(3) 0.95049(16) 1.2351(3) 0.0232(7) Uani 1 1 d . . . C13 C 0.3302(3) 0.92577(18) 1.3141(3) 0.0300(8) Uani 1 1 d . . . H13 H 0.3554 0.8803 1.315 0.036 Uiso 1 1 calc R . . C14 C 0.3681(4) 0.96801(19) 1.3935(3) 0.0341(9) Uani 1 1 d . . . H14 H 0.417 0.9508 1.4492 0.041 Uiso 1 1 calc R . . C15 C 0.3350(4) 1.03347(18) 1.3911(3) 0.0288(8) Uani 1 1 d . . . H15 H 0.3621 1.0618 1.4448 0.035 Uiso 1 1 calc R . . C16 C 0.2706(4) 0.84865(17) 1.1404(3) 0.0381(10) Uani 1 1 d . . . H16A H 0.2501 0.8196 1.1964 0.057 Uiso 1 1 calc R . . H16B H 0.3638 0.8539 1.1386 0.057 Uiso 1 1 calc R . . H16C H 0.2377 0.8288 1.0775 0.057 Uiso 1 1 calc R . . C100 C 0.7119(6) 0.9269(3) 0.3096(5) 0.0771(17) Uani 1 1 d . . . H10A H 0.694 0.9035 0.2463 0.116 Uiso 1 1 calc R . . H10B H 0.6464 0.961 0.3186 0.116 Uiso 1 1 calc R . . H10C H 0.711 0.8951 0.3651 0.116 Uiso 1 1 calc R . . C101 C 0.8399(5) 0.9589(2) 0.3079(3) 0.0494(11) Uani 1 1 d . . . C102 C 0.8755(7) 1.0071(3) 0.3887(5) 0.0781(18) Uani 1 1 d . . . H10D H 0.9609 1.0251 0.3778 0.117 Uiso 1 1 calc R . . H10E H 0.8761 0.9844 0.4536 0.117 Uiso 1 1 calc R . . H10F H 0.813 1.0434 0.3881 0.117 Uiso 1 1 calc R . . C103 C 0.8758(8) 0.7691(4) 0.4127(8) 0.118(3) Uani 1 1 d . . . H10J H 0.9072 0.7256 0.4363 0.177 Uiso 1 1 calc R . . H10K H 0.8706 0.7695 0.3393 0.177 Uiso 1 1 calc R . . H10L H 0.7907 0.7773 0.4381 0.177 Uiso 1 1 calc R . . C104 C 0.9628(5) 0.8204(3) 0.4485(4) 0.0573(13) Uani 1 1 d . . . C105 C 1.0858(7) 0.8274(4) 0.4061(8) 0.132(4) Uani 1 1 d . . . H10G H 1.1147 0.8736 0.4129 0.198 Uiso 1 1 calc R . . H10H H 1.0792 0.8153 0.3351 0.198 Uiso 1 1 calc R . . H10I H 1.1475 0.7979 0.4413 0.198 Uiso 1 1 calc R . . N1 N 0.0123(3) 1.27474(14) 1.0306(2) 0.0307(7) Uani 1 1 d . . . N2 N 0.3232(3) 1.15463(16) 0.9822(3) 0.0396(9) Uani 1 1 d . . . O1 O 0.1465(2) 1.03812(10) 1.15213(17) 0.0200(5) Uani 1 1 d . . . O2 O 0.2123(2) 0.91286(11) 1.15339(19) 0.0284(5) Uani 1 1 d . . . O3 O -0.0525(2) 0.94097(11) 1.03924(17) 0.0204(5) Uani 1 1 d D . . H103 H -0.064(4) 0.9375(18) 1.0990(10) 0.024 Uiso 1 1 d D . . O4 O -0.0706(2) 1.18727(12) 1.2110(2) 0.0324(6) Uani 1 1 d . . . O5 O 0.1247(2) 0.90613(10) 0.91641(17) 0.0214(5) Uani 1 1 d . . . O6 O 0.3181(2) 0.99360(14) 0.9948(2) 0.0364(6) Uani 1 1 d . . . O7 O 0.1086(3) 1.26198(12) 1.0892(2) 0.0349(6) Uani 1 1 d . . . O8 O -0.0422(3) 1.22490(11) 0.9888(2) 0.0333(6) Uani 1 1 d . . . O9 O -0.0255(3) 1.33109(12) 1.0164(2) 0.0429(7) Uani 1 1 d . . . O10 O 0.3174(3) 1.13964(14) 1.0732(2) 0.0422(7) Uani 1 1 d . . . O11 O 0.2185(3) 1.17181(13) 0.9383(2) 0.0384(7) Uani 1 1 d . . . O12 O 0.4231(3) 1.1524(2) 0.9388(3) 0.0679(11) Uani 1 1 d . . . O13 O 0.1849(3) 1.16291(12) 1.2423(2) 0.0321(6) Uani 1 1 d . . . O14 O 0.9133(4) 0.9451(2) 0.2450(3) 0.0796(12) Uani 1 1 d . . . O15 O 0.9309(6) 0.8574(2) 0.5140(4) 0.1040(16) Uani 1 1 d . . . Co1 Co 0.13234(4) 0.97464(2) 1.03169(3) 0.01907(10) Uani 1 1 d . . . Tb1 Tb 0.084222(15) 1.140217(7) 1.083192(12) 0.02016(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0200(19) 0.057(3) 0.040(2) -0.0129(19) 0.0041(19) -0.0073(17) C2 0.0214(17) 0.043(2) 0.028(2) -0.0070(16) 0.0027(16) -0.0031(15) C3 0.0189(16) 0.0301(17) 0.0203(17) -0.0027(14) -0.0022(15) 0.0049(13) C4 0.029(2) 0.0347(19) 0.027(2) -0.0072(15) -0.0025(17) 0.0012(15) C5 0.040(3) 0.061(3) 0.039(3) -0.029(2) 0.007(2) -0.001(2) C6 0.036(2) 0.090(4) 0.046(3) -0.027(3) 0.021(2) -0.003(2) C7 0.026(2) 0.071(3) 0.043(3) -0.018(2) 0.011(2) -0.0091(19) C8 0.047(2) 0.035(2) 0.045(2) -0.0254(19) -0.006(2) -0.0019(18) C9 0.0255(18) 0.0313(19) 0.0256(19) -0.0054(15) -0.0035(16) -0.0003(14) C10 0.0187(16) 0.0287(17) 0.0183(17) -0.0015(13) -0.0008(14) -0.0006(13) C11 0.0141(15) 0.0214(16) 0.0235(18) 0.0013(13) 0.0017(14) -0.0024(12) C12 0.0223(17) 0.0212(16) 0.0256(18) 0.0002(13) -0.0042(15) -0.0021(13) C13 0.0298(19) 0.0253(18) 0.034(2) 0.0027(15) -0.0083(17) 0.0036(15) C14 0.035(2) 0.039(2) 0.027(2) 0.0050(16) -0.0123(18) 0.0039(16) C15 0.0282(19) 0.036(2) 0.0214(18) -0.0041(15) -0.0031(16) -0.0005(15) C16 0.042(2) 0.0218(18) 0.050(3) -0.0083(16) -0.013(2) 0.0121(16) C100 0.070(4) 0.078(4) 0.083(4) 0.018(3) 0.001(3) -0.016(3) C101 0.060(3) 0.059(3) 0.029(2) 0.006(2) 0.009(2) 0.005(2) C102 0.103(5) 0.073(4) 0.058(4) -0.005(3) 0.001(4) -0.012(3) C103 0.084(5) 0.074(5) 0.193(10) -0.027(5) -0.018(6) -0.013(4) C104 0.053(3) 0.056(3) 0.063(3) 0.014(3) 0.008(3) 0.005(2) C105 0.081(5) 0.126(7) 0.195(10) 0.061(7) 0.067(6) 0.025(5) N1 0.0349(18) 0.0251(16) 0.0319(18) 0.0042(12) -0.0010(16) 0.0013(13) N2 0.034(2) 0.0329(18) 0.052(2) 0.0135(15) 0.0052(18) -0.0058(14) O1 0.0219(12) 0.0168(10) 0.0205(12) 0.0009(9) -0.0069(10) 0.0016(9) O2 0.0314(13) 0.0197(12) 0.0329(14) -0.0035(10) -0.0126(12) 0.0080(10) O3 0.0211(12) 0.0226(11) 0.0174(11) 0.0003(9) 0.0005(10) 0.0000(9) O4 0.0299(14) 0.0299(13) 0.0370(15) -0.0159(11) -0.0032(12) -0.0036(11) O5 0.0172(11) 0.0214(11) 0.0255(13) -0.0049(9) 0.0004(10) -0.0010(8) O6 0.0186(12) 0.0483(16) 0.0425(16) -0.0210(13) 0.0041(12) -0.0067(11) O7 0.0343(15) 0.0226(13) 0.0467(17) 0.0025(11) -0.0121(14) -0.0041(10) O8 0.0346(15) 0.0221(12) 0.0421(16) 0.0018(11) -0.0123(13) -0.0009(10) O9 0.062(2) 0.0187(13) 0.0478(18) 0.0083(12) -0.0047(16) 0.0120(12) O10 0.0273(14) 0.0526(17) 0.0465(18) 0.0199(14) 0.0000(13) -0.0035(12) O11 0.0331(16) 0.0409(15) 0.0408(17) 0.0119(12) -0.0020(14) -0.0067(12) O12 0.0330(18) 0.090(3) 0.083(3) 0.035(2) 0.0279(19) -0.0003(16) O13 0.0379(15) 0.0251(12) 0.0319(15) -0.0044(11) -0.0133(13) 0.0033(11) O14 0.086(3) 0.114(3) 0.041(2) -0.004(2) 0.021(2) -0.001(2) O15 0.113(4) 0.103(4) 0.096(4) -0.017(3) 0.010(3) 0.006(3) Co1 0.0159(2) 0.0191(2) 0.0219(2) -0.00306(17) -0.00307(19) 0.00060(16) Tb1 0.01915(9) 0.01574(9) 0.02508(10) 0.00017(6) -0.00486(7) -0.00103(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O6 1.226(5) . ? C1 C2 1.424(5) . ? C1 H1 0.95 . ? C2 C3 1.407(5) . ? C2 C7 1.415(5) . ? C3 O5 1.316(4) . ? C3 C4 1.418(5) 3_577 ? C4 O4 1.374(5) . ? C4 C5 1.376(5) . ? C4 C3 1.418(5) 3_577 ? C5 C6 1.389(6) . ? C5 H5 0.95 . ? C6 C7 1.356(6) 3_577 ? C6 H6 0.95 . ? C7 C6 1.356(6) 3_577 ? C7 H7 0.95 . ? C8 O4 1.451(4) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 O13 1.228(4) . ? C9 C10 1.434(5) . ? C9 H9 0.95 . ? C10 C15 1.412(5) . ? C10 C11 1.415(5) . ? C11 O1 1.315(4) . ? C11 C12 1.416(4) . ? C12 C13 1.372(5) . ? C12 O2 1.392(4) . ? C13 C14 1.403(6) . ? C13 H13 0.95 . ? C14 C15 1.360(5) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C16 O2 1.441(4) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C100 C101 1.485(7) . ? C100 H10A 0.98 . ? C100 H10B 0.98 . ? C100 H10C 0.98 . ? C101 O14 1.196(6) . ? C101 C102 1.485(7) . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? C102 H10F 0.98 . ? C103 C104 1.443(9) . ? C103 H10J 0.98 . ? C103 H10K 0.98 . ? C103 H10L 0.98 . ? C104 O15 1.206(7) . ? C104 C105 1.434(8) . ? C105 H10G 0.98 . ? C105 H10H 0.98 . ? C105 H10I 0.98 . ? N1 O9 1.211(4) . ? N1 O8 1.270(4) . ? N1 O7 1.275(4) . ? N1 Tb1 2.884(3) . ? N2 O12 1.217(5) . ? N2 O10 1.258(5) . ? N2 O11 1.266(5) . ? N2 Tb1 2.904(3) . ? O1 Co1 2.055(2) . ? O1 Tb1 2.330(2) . ? O2 Co1 2.184(2) . ? O3 Co1 2.053(2) . ? O3 Co1 2.098(2) 3_577 ? O3 Tb1 2.325(2) 3_577 ? O3 H103 0.818(10) . ? O4 Tb1 2.583(2) . ? O5 Co1 2.066(2) . ? O5 Tb1 2.373(2) 3_577 ? O6 Co1 2.059(2) . ? O7 Tb1 2.461(2) . ? O8 Tb1 2.468(3) . ? O10 Tb1 2.446(3) . ? O11 Tb1 2.522(3) . ? O13 Tb1 2.377(3) . ? Co1 O3 2.098(2) 3_577 ? Co1 Tb1 3.4388(5) . ? Tb1 O3 2.325(2) 3_577 ? Tb1 O5 2.373(2) 3_577 ? 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 O6 C1 C2 127.3(3) . . ? O6 C1 H1 116.4 . . ? C2 C1 H1 116.4 . . ? C3 C2 C7 119.8(3) . . ? C3 C2 C1 123.8(3) . . ? C7 C2 C1 116.4(3) . . ? O5 C3 C2 124.6(3) . . ? O5 C3 C4 118.1(3) . 3_577 ? C2 C3 C4 117.3(3) . 3_577 ? O4 C4 C5 125.4(3) . . ? O4 C4 C3 113.1(3) . 3_577 ? C5 C4 C3 121.5(4) . 3_577 ? C4 C5 C6 120.1(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 120.2(4) 3_577 . ? C7 C6 H6 119.9 3_577 . ? C5 C6 H6 119.9 . . ? C6 C7 C2 121.1(4) 3_577 . ? C6 C7 H7 119.4 3_577 . ? C2 C7 H7 119.4 . . ? O4 C8 H8A 109.5 . . ? O4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O13 C9 C10 126.9(3) . . ? O13 C9 H9 116.6 . . ? C10 C9 H9 116.6 . . ? C15 C10 C11 120.5(3) . . ? C15 C10 C9 116.9(3) . . ? C11 C10 C9 122.5(3) . . ? O1 C11 C10 124.3(3) . . ? O1 C11 C12 119.1(3) . . ? C10 C11 C12 116.6(3) . . ? C13 C12 O2 124.3(3) . . ? C13 C12 C11 122.4(3) . . ? O2 C12 C11 113.3(3) . . ? C12 C13 C14 119.6(3) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 120.6(3) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O14 C101 C102 121.0(5) . . ? O14 C101 C100 121.0(5) . . ? C102 C101 C100 118.0(5) . . ? C101 C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C101 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? C104 C103 H10J 109.5 . . ? C104 C103 H10K 109.5 . . ? H10J C103 H10K 109.5 . . ? C104 C103 H10L 109.5 . . ? H10J C103 H10L 109.5 . . ? H10K C103 H10L 109.5 . . ? O15 C104 C105 120.6(7) . . ? O15 C104 C103 119.4(6) . . ? C105 C104 C103 120.0(7) . . ? C104 C105 H10G 109.5 . . ? C104 C105 H10H 109.5 . . ? H10G C105 H10H 109.5 . . ? C104 C105 H10I 109.5 . . ? H10G C105 H10I 109.5 . . ? H10H C105 H10I 109.5 . . ? O9 N1 O8 122.1(3) . . ? O9 N1 O7 121.8(3) . . ? O8 N1 O7 116.1(3) . . ? O9 N1 Tb1 173.6(3) . . ? O8 N1 Tb1 58.36(16) . . ? O7 N1 Tb1 58.07(16) . . ? O12 N2 O10 122.0(4) . . ? O12 N2 O11 122.1(4) . . ? O10 N2 O11 115.9(3) . . ? O12 N2 Tb1 172.1(3) . . ? O10 N2 Tb1 56.47(18) . . ? O11 N2 Tb1 60.02(18) . . ? C11 O1 Co1 116.49(19) . . ? C11 O1 Tb1 136.22(19) . . ? Co1 O1 Tb1 103.12(9) . . ? C12 O2 C16 116.9(3) . . ? C12 O2 Co1 112.33(19) . . ? C16 O2 Co1 124.7(2) . . ? Co1 O3 Co1 93.89(9) . 3_577 ? Co1 O3 Tb1 107.60(9) . 3_577 ? Co1 O3 Tb1 101.94(10) 3_577 3_577 ? Co1 O3 H103 105(3) . . ? Co1 O3 H103 116(3) 3_577 . ? Tb1 O3 H103 127(3) 3_577 . ? C4 O4 C8 114.9(3) . . ? C4 O4 Tb1 119.0(2) . . ? C8 O4 Tb1 126.1(2) . . ? C3 O5 Co1 127.9(2) . . ? C3 O5 Tb1 126.6(2) . 3_577 ? Co1 O5 Tb1 105.41(9) . 3_577 ? C1 O6 Co1 128.9(3) . . ? N1 O7 Tb1 95.85(19) . . ? N1 O8 Tb1 95.7(2) . . ? N2 O10 Tb1 98.1(2) . . ? N2 O11 Tb1 94.2(2) . . ? C9 O13 Tb1 136.1(2) . . ? O3 Co1 O1 101.65(9) . . ? O3 Co1 O6 166.28(9) . . ? O1 Co1 O6 92.07(10) . . ? O3 Co1 O5 79.11(9) . . ? O1 Co1 O5 176.16(9) . . ? O6 Co1 O5 87.20(9) . . ? O3 Co1 O3 86.11(9) . 3_577 ? O1 Co1 O3 82.32(9) . 3_577 ? O6 Co1 O3 95.91(11) . 3_577 ? O5 Co1 O3 101.50(9) . 3_577 ? O3 Co1 O2 96.09(10) . . ? O1 Co1 O2 75.91(9) . . ? O6 Co1 O2 87.11(11) . . ? O5 Co1 O2 100.29(9) . . ? O3 Co1 O2 158.12(9) 3_577 . ? O3 Co1 Tb1 99.38(6) . . ? O1 Co1 Tb1 41.29(6) . . ? O6 Co1 Tb1 90.94(7) . . ? O5 Co1 Tb1 142.46(7) . . ? O3 Co1 Tb1 41.41(6) 3_577 . ? O2 Co1 Tb1 117.08(6) . . ? O3 Tb1 O1 71.93(8) 3_577 . ? O3 Tb1 O5 67.86(8) 3_577 3_577 ? O1 Tb1 O5 83.96(8) . 3_577 ? O3 Tb1 O13 144.02(8) 3_577 . ? O1 Tb1 O13 73.11(8) . . ? O5 Tb1 O13 116.40(9) 3_577 . ? O3 Tb1 O10 94.02(9) 3_577 . ? O1 Tb1 O10 75.86(8) . . ? O5 Tb1 O10 156.44(8) 3_577 . ? O13 Tb1 O10 69.31(10) . . ? O3 Tb1 O7 137.07(8) 3_577 . ? O1 Tb1 O7 146.67(8) . . ? O5 Tb1 O7 118.95(8) 3_577 . ? O13 Tb1 O7 74.85(9) . . ? O10 Tb1 O7 84.53(9) . . ? O3 Tb1 O8 93.82(9) 3_577 . ? O1 Tb1 O8 160.66(8) . . ? O5 Tb1 O8 78.45(8) 3_577 . ? O13 Tb1 O8 122.15(8) . . ? O10 Tb1 O8 119.18(9) . . ? O7 Tb1 O8 51.95(9) . . ? O3 Tb1 O11 72.70(9) 3_577 . ? O1 Tb1 O11 111.74(8) . . ? O5 Tb1 O11 130.00(9) 3_577 . ? O13 Tb1 O11 113.58(10) . . ? O10 Tb1 O11 50.98(10) . . ? O7 Tb1 O11 73.43(9) . . ? O8 Tb1 O11 74.74(9) . . ? O3 Tb1 O4 130.44(8) 3_577 . ? O1 Tb1 O4 103.44(8) . . ? O5 Tb1 O4 62.60(7) 3_577 . ? O13 Tb1 O4 66.60(9) . . ? O10 Tb1 O4 133.78(10) . . ? O7 Tb1 O4 71.41(9) . . ? O8 Tb1 O4 75.50(9) . . ? O11 Tb1 O4 143.27(9) . . ? O3 Tb1 N1 117.26(9) 3_577 . ? O1 Tb1 N1 170.69(9) . . ? O5 Tb1 N1 97.95(9) 3_577 . ? O13 Tb1 N1 98.00(9) . . ? O10 Tb1 N1 103.93(9) . . ? O7 Tb1 N1 26.08(9) . . ? O8 Tb1 N1 25.98(9) . . ? O11 Tb1 N1 74.01(9) . . ? O4 Tb1 N1 69.78(9) . . ? O3 Tb1 N2 80.89(9) 3_577 . ? O1 Tb1 N2 92.34(9) . . ? O5 Tb1 N2 148.15(9) 3_577 . ? O13 Tb1 N2 92.36(11) . . ? O10 Tb1 N2 25.38(10) . . ? O7 Tb1 N2 80.00(9) . . ? O8 Tb1 N2 98.34(10) . . ? O11 Tb1 N2 25.77(10) . . ? O4 Tb1 N2 147.88(9) . . ? N1 Tb1 N2 90.76(9) . . ? O3 Tb1 Co1 36.65(6) 3_577 . ? O1 Tb1 Co1 35.59(6) . . ? O5 Tb1 Co1 76.31(5) 3_577 . ? O13 Tb1 Co1 107.58(6) . . ? O10 Tb1 Co1 80.20(7) . . ? O7 Tb1 Co1 162.29(7) . . ? O8 Tb1 Co1 130.11(6) . . ? O11 Tb1 Co1 89.92(6) . . ? O4 Tb1 Co1 126.00(6) . . ? N1 Tb1 Co1 153.71(7) . . ? N2 Tb1 Co1 82.37(7) . . ? #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_complex(1) _database_code_depnum_ccdc_archive 'CCDC 793513' #TrackingRef 'Cif-global.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H30 Co2 Gd2 N4 O26, C3 H6 O' _chemical_formula_sum 'C35 H36 Co2 Gd2 N4 O27' _chemical_formula_weight 1377.04 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9145(6) _cell_length_b 11.0981(7) _cell_length_c 12.7917(7) _cell_angle_alpha 72.514(3) _cell_angle_beta 66.084(2) _cell_angle_gamma 62.621(3) _cell_volume 1245.29(12) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 32.74 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.472 _exptl_absorpt_correction_T_max 0.766 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _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 Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_unetI/netI 0.0121 _diffrn_reflns_number 30578 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 4548 _reflns_number_gt 4285 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR2004 (Giacovazzo et al, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0751P)^2^+5.2178P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4548 _refine_ls_number_parameters 263 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.741 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.198 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6945(6) 0.7370(6) 0.3805(6) 0.0358(12) Uani 1 1 d . . . C2 C 0.6543(7) 0.7907(7) 0.4812(6) 0.0419(14) Uani 1 1 d . . . C3 C 0.6860(8) 0.8964(7) 0.4797(7) 0.0520(17) Uani 1 1 d . . . H3 H 0.6592 0.9289 0.5497 0.062 Uiso 1 1 calc R . . C4 C 0.7569(9) 0.9566(8) 0.3766(8) 0.059(2) Uani 1 1 d . . . H4 H 0.7798 1.0297 0.3762 0.071 Uiso 1 1 calc R . . C5 C 0.7940(8) 0.9125(7) 0.2764(7) 0.0537(18) Uani 1 1 d . . . H5 H 0.8402 0.9567 0.2058 0.064 Uiso 1 1 calc R . . C6 C 0.7646(7) 0.8004(7) 0.2751(6) 0.0455(15) Uani 1 1 d . . . C7 C 0.8054(9) 0.7616(9) 0.1651(8) 0.0610(19) Uani 1 1 d . . . H7 H 0.8484 0.814 0.0994 0.073 Uiso 1 1 calc R . . C8 C 0.5425(8) 0.7601(8) 0.6862(7) 0.0525(17) Uani 1 1 d . . . H8A H 0.6324 0.736 0.7018 0.079 Uiso 1 1 calc R . . H8B H 0.4855 0.7103 0.7466 0.079 Uiso 1 1 calc R . . H8C H 0.4857 0.8589 0.6853 0.079 Uiso 1 1 calc R . . C9 C 0.5224(9) 0.6104(8) 0.0913(6) 0.0512(17) Uani 1 1 d . . . C10 C 0.4362(7) 0.5922(7) 0.2069(6) 0.0423(14) Uani 1 1 d . . . C11 C 0.2862(8) 0.6357(8) 0.2313(8) 0.0565(18) Uani 1 1 d . . . C12 C 0.2269(10) 0.7078(11) 0.1352(10) 0.080(3) Uani 1 1 d . . . H12 H 0.1254 0.7392 0.1492 0.095 Uiso 1 1 calc R . . C13 C 0.3121(14) 0.7298(12) 0.0295(9) 0.090(3) Uani 1 1 d . . . H13 H 0.2702 0.7819 -0.0303 0.108 Uiso 1 1 calc R . . C14 C 0.4623(13) 0.6780(12) 0.0042(8) 0.079(3) Uani 1 1 d . . . H14 H 0.5227 0.6894 -0.0731 0.095 Uiso 1 1 calc R . . C15 C 0.8151(11) 0.3874(10) 0.6601(8) 0.070(2) Uani 1 1 d . . . H15 H 0.9133 0.3568 0.6568 0.084 Uiso 1 1 calc R . . O15 O 0.3317(11) 0.8591(9) 0.3900(9) 0.047(2) Uani 0.5 1 d P . . C20 C 0.2603(15) 0.9236(11) 0.3272(11) 0.039(3) Uani 0.5 1 d P . . C22 C 0.1053(18) 0.9444(16) 0.3630(17) 0.063(4) Uani 0.5 1 d P . . H22A H 0.0801 0.8892 0.4381 0.094 Uiso 0.5 1 calc PR . . H22B H 0.0895 0.9163 0.3055 0.094 Uiso 0.5 1 calc PR . . H22C H 0.0439 1.0415 0.3693 0.094 Uiso 0.5 1 calc PR . . N1 N 0.9036(6) 0.2334(6) 0.1435(5) 0.0468(13) Uani 1 1 d . . . N2 N 1.0183(7) 0.3544(10) 0.3184(7) 0.074(2) Uani 1 1 d . . . O1 O 0.6659(5) 0.6319(4) 0.3864(4) 0.0401(10) Uani 1 1 d . . . O2 O 0.5767(5) 0.7244(5) 0.5788(4) 0.0517(12) Uani 1 1 d . . . O3 O 0.6261(4) 0.3916(4) 0.4525(3) 0.0281(7) Uani 1 1 d D . . HO3 H 0.661(7) 0.303(2) 0.488(5) 0.034 Uiso 1 1 d D . . O13 O 0.7908(7) 0.6694(7) 0.1474(5) 0.067 Uani 1 1 d . . . O4 O 0.6757(7) 0.5493(6) 0.0786(4) 0.064 Uani 1 1 d . . . O5 O 0.5023(5) 0.5337(5) 0.2871(4) 0.041 Uani 1 1 d . . . O6 O 0.7864(5) 0.4412(6) 0.5747(5) 0.063 Uani 1 1 d . . . O7 O 0.7813(5) 0.2545(5) 0.2214(4) 0.045 Uani 1 1 d . . . O8 O 0.9537(6) 0.3255(6) 0.1174(5) 0.057 Uani 1 1 d . . . O9 O 0.9688(6) 0.1310(6) 0.0961(5) 0.064 Uani 1 1 d . . . O10 O 0.9343(6) 0.2915(7) 0.3535(5) 0.071 Uani 1 1 d . . . O11 O 0.9804(6) 0.4718(7) 0.2634(5) 0.065 Uani 1 1 d . . . O12 O 1.1367(9) 0.3001(13) 0.3357(10) 0.141 Uani 1 1 d . . . Co1 Co 0.58590(8) 0.53663(8) 0.54678(7) 0.032 Uani 1 1 d . . . Gd1 Gd 0.75077(3) 0.47013(3) 0.26513(2) 0.035 Uani 1 1 d . . . C16 C 0.7701(11) 0.5697(11) -0.0345(7) 0.07 Uani 1 1 d . . . H16A H 0.7645 0.5239 -0.0861 0.106 Uiso 1 1 calc R . . H16B H 0.8702 0.5313 -0.0328 0.106 Uiso 1 1 calc R . . H16C H 0.741 0.6681 -0.0628 0.106 Uiso 1 1 calc R . . C21 C 0.324(2) 0.9917(15) 0.2085(14) 0.064(5) Uani 0.5 1 d P . . H21A H 0.4129 0.9965 0.2048 0.096 Uiso 0.5 1 calc PR . . H21B H 0.2531 1.0845 0.1941 0.096 Uiso 0.5 1 calc PR . . H21C H 0.3463 0.9381 0.1499 0.096 Uiso 0.5 1 calc PR . . 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 C1 0.025(3) 0.037(3) 0.045(3) -0.005(2) -0.006(2) -0.016(2) C2 0.032(3) 0.042(3) 0.048(4) -0.003(3) -0.012(3) -0.014(3) C3 0.052(4) 0.047(4) 0.061(4) -0.009(3) -0.020(4) -0.020(3) C4 0.067(5) 0.045(4) 0.079(6) -0.002(4) -0.030(4) -0.030(4) C5 0.049(4) 0.047(4) 0.062(5) 0.012(3) -0.016(3) -0.029(3) C6 0.038(3) 0.048(4) 0.048(4) 0.002(3) -0.013(3) -0.020(3) C7 0.062(5) 0.067(5) 0.062(5) -0.005(4) -0.020(4) -0.034(4) C8 0.051(4) 0.065(4) 0.054(4) -0.016(3) -0.018(3) -0.026(4) C9 0.062(4) 0.067(4) 0.034(3) -0.001(3) -0.019(3) -0.033(4) C10 0.046(4) 0.046(3) 0.036(3) -0.005(3) -0.023(3) -0.011(3) C11 0.042(4) 0.060(4) 0.067(5) -0.012(4) -0.026(4) -0.010(3) C12 0.053(5) 0.087(6) 0.105(8) -0.014(6) -0.044(5) -0.016(5) C13 0.113(9) 0.109(8) 0.065(6) 0.021(6) -0.060(7) -0.051(7) C14 0.108(8) 0.108(7) 0.048(5) 0.011(5) -0.044(5) -0.061(7) C15 0.070(6) 0.070(5) 0.068(6) -0.017(4) -0.032(5) -0.013(4) O15 0.058(6) 0.031(4) 0.058(6) 0.007(4) -0.035(5) -0.016(4) C20 0.060(8) 0.020(5) 0.043(7) -0.001(5) -0.020(6) -0.017(5) C22 0.060(9) 0.042(7) 0.090(13) -0.001(8) -0.041(9) -0.012(7) N1 0.038(3) 0.056(3) 0.043(3) -0.008(3) -0.003(2) -0.024(3) N2 0.034(3) 0.113(6) 0.070(5) -0.027(5) -0.016(3) -0.017(4) O1 0.032(2) 0.044(2) 0.044(2) -0.0064(19) -0.0007(18) -0.0236(19) O2 0.048(3) 0.065(3) 0.047(3) -0.017(2) -0.006(2) -0.028(2) O3 0.0252(18) 0.0319(19) 0.0261(18) -0.0002(15) -0.0076(15) -0.0129(15) O13 0.084 0.088 0.043 0.005 -0.009 -0.062 O4 0.077 0.081 0.035 -0.006 -0.004 -0.045 O5 0.031 0.06 0.026 -0.005 -0.012 -0.012 O6 0.038 0.08 0.079 -0.031 -0.025 -0.012 O7 0.036 0.054 0.041 -0.007 -0.002 -0.022 O8 0.05 0.068 0.051 -0.021 0.01 -0.036 O9 0.056 0.057 0.069 -0.026 0.001 -0.022 O10 0.03 0.092 0.06 -0.003 -0.008 -0.008 O11 0.042 0.096 0.068 -0.025 -0.011 -0.033 O12 0.056 0.189 0.179 -0.022 -0.069 -0.023 Co1 0.025 0.043 0.031 -0.009 -0.007 -0.015 Gd1 0.028 0.048 0.026 -0.004 -0.001 -0.019 C16 0.083 0.094 0.04 -0.002 -0.006 -0.054 C21 0.103(14) 0.040(7) 0.044(8) 0.011(6) -0.033(9) -0.025(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.314(7) . ? C1 C2 1.404(9) . ? C1 C6 1.409(9) . ? C2 C3 1.360(10) . ? C2 O2 1.408(8) . ? C3 C4 1.379(12) . ? C3 H3 0.95 . ? C4 C5 1.350(12) . ? C4 H4 0.95 . ? C5 C6 1.426(10) . ? C5 H5 0.95 . ? C6 C7 1.429(11) . ? C7 O13 1.201(10) . ? C7 H7 0.95 . ? C8 O2 1.400(8) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C14 1.368(11) . ? C9 C10 1.408(10) . ? C9 O4 1.445(10) . ? C10 O5 1.327(7) . ? C10 C11 1.401(10) . ? C11 C15 1.421(13) 2_666 ? C11 C12 1.466(12) . ? C12 C13 1.320(15) . ? C12 H12 0.95 . ? C13 C14 1.392(16) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 O6 1.167(10) . ? C15 C11 1.421(13) 2_666 ? C15 H15 0.95 . ? O15 C20 1.189(15) . ? C20 C22 1.48(2) . ? C20 C21 1.51(2) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? N1 O9 1.219(8) . ? N1 O7 1.266(7) . ? N1 O8 1.272(8) . ? N1 Gd1 2.903(6) . ? N2 O12 1.232(10) . ? N2 O11 1.245(11) . ? N2 O10 1.264(11) . ? N2 Gd1 2.877(7) . ? O1 Co1 2.045(4) . ? O1 Gd1 2.339(4) . ? O2 Co1 2.192(5) . ? O3 Co1 2.069(4) 2_666 ? O3 Co1 2.080(4) . ? O3 Gd1 2.356(4) . ? O3 HO3 0.916(10) . ? O13 Gd1 2.388(6) . ? O4 C16 1.419(9) . ? O4 Gd1 2.608(6) . ? O5 Co1 2.022(4) 2_666 ? O5 Gd1 2.381(4) . ? O6 Co1 2.077(5) . ? O7 Gd1 2.463(5) . ? O8 Gd1 2.492(5) . ? O10 Gd1 2.461(5) . ? O11 Gd1 2.506(5) . ? Co1 O5 2.022(4) 2_666 ? Co1 O3 2.069(4) 2_666 ? Co1 Gd1 3.4471(8) . ? Co1 Gd1 3.5034(8) 2_666 ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 120.1(6) . . ? O1 C1 C6 122.3(6) . . ? C2 C1 C6 117.6(6) . . ? C3 C2 C1 122.1(6) . . ? C3 C2 O2 126.2(7) . . ? C1 C2 O2 111.7(5) . . ? C2 C3 C4 120.1(7) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.5(7) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.8(7) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 118.8(7) . . ? C1 C6 C7 123.9(7) . . ? C5 C6 C7 117.2(7) . . ? O13 C7 C6 126.5(8) . . ? O13 C7 H7 116.7 . . ? C6 C7 H7 116.7 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 121.8(8) . . ? C14 C9 O4 126.1(8) . . ? C10 C9 O4 112.1(6) . . ? O5 C10 C11 123.6(7) . . ? O5 C10 C9 117.9(6) . . ? C11 C10 C9 118.6(6) . . ? C10 C11 C15 126.5(7) . 2_666 ? C10 C11 C12 117.5(8) . . ? C15 C11 C12 116.0(8) 2_666 . ? C13 C12 C11 121.1(9) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 121.1(9) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C9 C14 C13 119.7(9) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? O6 C15 C11 124.7(9) . 2_666 ? O6 C15 H15 117.6 . . ? C11 C15 H15 117.6 2_666 . ? O15 C20 C22 121.6(13) . . ? O15 C20 C21 120.8(14) . . ? C22 C20 C21 117.6(13) . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O9 N1 O7 121.9(6) . . ? O9 N1 O8 122.1(6) . . ? O7 N1 O8 116.0(6) . . ? O9 N1 Gd1 177.6(5) . . ? O7 N1 Gd1 57.4(3) . . ? O8 N1 Gd1 58.7(3) . . ? O12 N2 O11 120.5(10) . . ? O12 N2 O10 120.9(10) . . ? O11 N2 O10 118.6(6) . . ? O12 N2 Gd1 176.0(8) . . ? O11 N2 Gd1 60.3(4) . . ? O10 N2 Gd1 58.3(4) . . ? C1 O1 Co1 117.8(4) . . ? C1 O1 Gd1 135.1(4) . . ? Co1 O1 Gd1 103.50(17) . . ? C8 O2 C2 117.0(5) . . ? C8 O2 Co1 126.9(5) . . ? C2 O2 Co1 113.2(4) . . ? Co1 O3 Co1 95.41(15) 2_666 . ? Co1 O3 Gd1 104.54(15) 2_666 . ? Co1 O3 Gd1 101.82(15) . . ? Co1 O3 HO3 115(4) 2_666 . ? Co1 O3 HO3 113(4) . . ? Gd1 O3 HO3 123(4) . . ? C7 O13 Gd1 133.9(6) . . ? C16 O4 C9 115.8(6) . . ? C16 O4 Gd1 124.1(5) . . ? C9 O4 Gd1 118.0(4) . . ? C10 O5 Co1 126.2(4) . 2_666 ? C10 O5 Gd1 128.4(4) . . ? Co1 O5 Gd1 105.14(17) 2_666 . ? C15 O6 Co1 130.0(7) . . ? N1 O7 Gd1 97.0(4) . . ? N1 O8 Gd1 95.4(4) . . ? N2 O10 Gd1 95.7(5) . . ? N2 O11 Gd1 94.1(5) . . ? O5 Co1 O1 172.35(18) 2_666 . ? O5 Co1 O3 81.57(16) 2_666 2_666 ? O1 Co1 O3 97.63(16) . 2_666 ? O5 Co1 O6 88.0(2) 2_666 . ? O1 Co1 O6 93.1(2) . . ? O3 Co1 O6 169.1(2) 2_666 . ? O5 Co1 O3 104.71(17) 2_666 . ? O1 Co1 O3 82.74(16) . . ? O3 Co1 O3 84.59(15) 2_666 . ? O6 Co1 O3 95.25(18) . . ? O5 Co1 O2 97.24(19) 2_666 . ? O1 Co1 O2 75.30(18) . . ? O3 Co1 O2 98.08(17) 2_666 . ? O6 Co1 O2 86.1(2) . . ? O3 Co1 O2 158.03(17) . . ? O5 Co1 Gd1 146.33(14) 2_666 . ? O1 Co1 Gd1 41.28(12) . . ? O3 Co1 Gd1 96.58(11) 2_666 . ? O6 Co1 Gd1 90.44(17) . . ? O3 Co1 Gd1 41.98(10) . . ? O2 Co1 Gd1 116.20(14) . . ? O5 Co1 Gd1 41.01(12) 2_666 2_666 ? O1 Co1 Gd1 137.97(13) . 2_666 ? O3 Co1 Gd1 40.61(10) 2_666 2_666 ? O6 Co1 Gd1 128.80(19) . 2_666 ? O3 Co1 Gd1 94.71(10) . 2_666 ? O2 Co1 Gd1 101.49(13) . 2_666 ? Gd1 Co1 Gd1 127.61(2) . 2_666 ? O1 Gd1 O3 71.01(14) . . ? O1 Gd1 O5 86.44(15) . . ? O3 Gd1 O5 68.69(14) . . ? O1 Gd1 O13 72.20(18) . . ? O3 Gd1 O13 142.27(18) . . ? O5 Gd1 O13 101.04(19) . . ? O1 Gd1 O10 96.4(2) . . ? O3 Gd1 O10 72.45(16) . . ? O5 Gd1 O10 137.67(18) . . ? O13 Gd1 O10 120.1(2) . . ? O1 Gd1 O7 153.95(15) . . ? O3 Gd1 O7 82.95(14) . . ? O5 Gd1 O7 83.41(16) . . ? O13 Gd1 O7 133.33(18) . . ? O10 Gd1 O7 75.8(2) . . ? O1 Gd1 O8 149.43(15) . . ? O3 Gd1 O8 126.53(16) . . ? O5 Gd1 O8 122.12(16) . . ? O13 Gd1 O8 90.2(2) . . ? O10 Gd1 O8 70.5(2) . . ? O7 Gd1 O8 51.49(15) . . ? O1 Gd1 O11 76.98(17) . . ? O3 Gd1 O11 110.11(18) . . ? O5 Gd1 O11 162.52(19) . . ? O13 Gd1 O11 68.8(2) . . ? O10 Gd1 O11 51.5(2) . . ? O7 Gd1 O11 113.98(19) . . ? O8 Gd1 O11 73.33(18) . . ? O1 Gd1 O4 118.55(18) . . ? O3 Gd1 O4 128.38(16) . . ? O5 Gd1 O4 62.09(16) . . ? O13 Gd1 O4 65.15(19) . . ? O10 Gd1 O4 142.9(2) . . ? O7 Gd1 O4 77.17(17) . . ? O8 Gd1 O4 72.8(2) . . ? O11 Gd1 O4 121.5(2) . . ? O1 Gd1 N2 87.0(2) . . ? O3 Gd1 N2 91.96(19) . . ? O5 Gd1 N2 160.6(2) . . ? O13 Gd1 N2 94.2(3) . . ? O10 Gd1 N2 25.9(2) . . ? O7 Gd1 N2 94.8(2) . . ? O8 Gd1 N2 69.1(2) . . ? O11 Gd1 N2 25.6(2) . . ? O4 Gd1 N2 136.4(2) . . ? O1 Gd1 N1 166.86(17) . . ? O3 Gd1 N1 104.73(15) . . ? O5 Gd1 N1 103.80(16) . . ? O13 Gd1 N1 113.00(19) . . ? O10 Gd1 N1 70.5(2) . . ? O7 Gd1 N1 25.66(15) . . ? O8 Gd1 N1 25.85(16) . . ? O11 Gd1 N1 93.42(18) . . ? O4 Gd1 N1 74.06(18) . . ? N2 Gd1 N1 80.7(2) . . ? O1 Gd1 Co1 35.23(11) . . ? O3 Gd1 Co1 36.20(9) . . ? O5 Gd1 Co1 78.98(10) . . ? O13 Gd1 Co1 107.42(15) . . ? O10 Gd1 Co1 79.61(14) . . ? O7 Gd1 Co1 118.92(11) . . ? O8 Gd1 Co1 150.01(14) . . ? O11 Gd1 Co1 90.32(14) . . ? O4 Gd1 Co1 136.44(14) . . ? N2 Gd1 Co1 85.18(15) . . ? N1 Gd1 Co1 137.89(12) . . ? O4 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # ===== END data_complex(3) _database_code_depnum_ccdc_archive 'CCDC 793514' #TrackingRef 'Cif-global.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H30 Co2 N4 O26 Y2, C3 H6 O' _chemical_formula_sum 'C35 H36 Co2 N4 O27 Y2' _chemical_formula_weight 1240.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9150(9) _cell_length_b 11.0980(10) _cell_length_c 12.7920(7) _cell_angle_alpha 72.514(3) _cell_angle_beta 66.084(5) _cell_angle_gamma 62.621(2) _cell_volume 1245.36(17) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4896 _cell_measurement_theta_min 2.9125 _cell_measurement_theta_max 32.2242 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET) (compiled May 29 2008,13:12:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.721 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_orient_matrix_ub_11 0.0343301886 _diffrn_orient_matrix_ub_12 0.0042946889 _diffrn_orient_matrix_ub_13 -0.0609509657 _diffrn_orient_matrix_ub_21 0.0305002885 _diffrn_orient_matrix_ub_22 -0.0724224727 _diffrn_orient_matrix_ub_23 0.005075372 _diffrn_orient_matrix_ub_31 -0.0627195794 _diffrn_orient_matrix_ub_32 0.001546571 _diffrn_orient_matrix_ub_33 -0.0064877176 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_unetI/netI 0.0457 _diffrn_reflns_number 8991 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 4545 _reflns_number_gt 3251 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4545 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1634 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.13 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.125 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6964(6) 0.7330(6) 0.3790(5) 0.0389(13) Uani 1 1 d . . . C2 C 0.6589(6) 0.7874(6) 0.4762(5) 0.0438(14) Uani 1 1 d . . . C3 C 0.6906(7) 0.8946(7) 0.4740(6) 0.0550(16) Uani 1 1 d . . . H3 H 0.6646 0.9277 0.5435 0.066 Uiso 1 1 calc R . . C4 C 0.7597(8) 0.9532(7) 0.3707(7) 0.0615(19) Uani 1 1 d . . . H4 H 0.7824 1.0267 0.3693 0.074 Uiso 1 1 calc R . . C5 C 0.7966(7) 0.9089(7) 0.2702(7) 0.0595(18) Uani 1 1 d . . . H5 H 0.8437 0.9514 0.199 0.071 Uiso 1 1 calc R . . C6 C 0.7638(6) 0.7972(6) 0.2728(5) 0.0453(14) Uani 1 1 d . . . C7 C 0.8019(9) 0.7567(8) 0.1664(8) 0.069(2) Uani 1 1 d . . . H7 H 0.8457 0.8083 0.1004 0.083 Uiso 1 1 calc R . . C8 C 0.5453(8) 0.7582(8) 0.6821(6) 0.0605(18) Uani 1 1 d . . . H8A H 0.6335 0.7312 0.7014 0.091 Uiso 1 1 calc R . . H8B H 0.4827 0.7135 0.7422 0.091 Uiso 1 1 calc R . . H8C H 0.493 0.8579 0.6774 0.091 Uiso 1 1 calc R . . C9 C 0.5249(7) 0.6082(7) 0.0908(5) 0.0512(16) Uani 1 1 d . . . C10 C 0.4385(6) 0.5950(6) 0.2071(5) 0.0439(14) Uani 1 1 d . . . C11 C 0.2871(7) 0.6392(8) 0.2325(7) 0.0627(19) Uani 1 1 d . . . C12 C 0.2290(9) 0.7109(10) 0.1350(9) 0.086(3) Uani 1 1 d . . . H12 H 0.1272 0.7466 0.1484 0.103 Uiso 1 1 calc R . . C13 C 0.3178(12) 0.7257(11) 0.0288(8) 0.095(3) Uani 1 1 d . . . H13 H 0.2765 0.7738 -0.0318 0.114 Uiso 1 1 calc R . . C14 C 0.4665(10) 0.6754(10) 0.0016(7) 0.078(2) Uani 1 1 d . . . H14 H 0.5269 0.6865 -0.0758 0.094 Uiso 1 1 calc R . . C15 C 0.8134(10) 0.3827(9) 0.6585(7) 0.075(2) Uani 1 1 d . . . H15 H 0.9118 0.3497 0.6554 0.09 Uiso 1 1 calc R . . O15 O 0.3314(11) 0.8608(10) 0.3960(9) 0.066(3) Uani 0.5 1 d P . . C20 C 0.2580(16) 0.9273(14) 0.3311(14) 0.061(4) Uani 0.5 1 d P . . C22 C 0.098(2) 0.952(2) 0.373(2) 0.126(10) Uani 0.5 1 d P . . H22A H 0.0689 0.9178 0.4556 0.189 Uiso 0.5 1 calc PR . . H22B H 0.0815 0.9049 0.3301 0.189 Uiso 0.5 1 calc PR . . H22C H 0.0408 1.051 0.3607 0.189 Uiso 0.5 1 calc PR . . N1 N 0.8966(5) 0.2396(6) 0.1466(5) 0.0506(13) Uani 1 1 d . . . N2 N 1.0153(7) 0.3615(9) 0.3158(7) 0.078(2) Uani 1 1 d . . . O1 O 0.6674(4) 0.6283(4) 0.3854(3) 0.0416(9) Uani 1 1 d . . . O2 O 0.5827(5) 0.7189(5) 0.5772(4) 0.0583(12) Uani 1 1 d . . . O3 O 0.6261(4) 0.3919(4) 0.4510(3) 0.0289(7) Uani 1 1 d . . . H3A H 0.6716 0.2928 0.4808 0.035 Uiso 1 1 calc R . . O13 O 0.7870(6) 0.6670(6) 0.1473(4) 0.0764(16) Uani 1 1 d . . . O4 O 0.6768(6) 0.5468(5) 0.0788(4) 0.0673(14) Uani 1 1 d . . . O5 O 0.5038(4) 0.5364(4) 0.2875(3) 0.0398(9) Uani 1 1 d . . . O6 O 0.7878(5) 0.4363(6) 0.5738(5) 0.0697(14) Uani 1 1 d . . . O7 O 0.7737(4) 0.2629(4) 0.2239(4) 0.0486(10) Uani 1 1 d . . . O8 O 0.9481(5) 0.3305(5) 0.1197(4) 0.0608(12) Uani 1 1 d . . . O9 O 0.9604(5) 0.1389(5) 0.0992(5) 0.0674(13) Uani 1 1 d . . . O10 O 0.9302(5) 0.2994(6) 0.3513(4) 0.0824(18) Uani 1 1 d . . . O11 O 0.9752(5) 0.4759(7) 0.2619(5) 0.0731(15) Uani 1 1 d . . . O12 O 1.1312(7) 0.3114(11) 0.3330(8) 0.155(4) Uani 1 1 d . . . Co1 Co 0.58720(7) 0.53405(8) 0.54644(6) 0.0345(2) Uani 1 1 d . . . Y1 Y 0.74875(5) 0.47141(6) 0.26609(4) 0.0379(2) Uani 1 1 d . . . C16 C 0.7688(10) 0.5707(10) -0.0354(6) 0.078(2) Uani 1 1 d . . . H16A H 0.7529 0.5362 -0.089 0.116 Uiso 1 1 calc R . . H16B H 0.8706 0.5229 -0.0375 0.116 Uiso 1 1 calc R . . H16C H 0.7459 0.6692 -0.0582 0.116 Uiso 1 1 calc R . . C21 C 0.322(2) 0.9957(13) 0.2113(12) 0.075(5) Uani 0.5 1 d P . . H21A H 0.4055 1.0089 0.2097 0.113 Uiso 0.5 1 calc PR . . H21B H 0.2479 1.0848 0.1936 0.113 Uiso 0.5 1 calc PR . . H21C H 0.3535 0.9372 0.1536 0.113 Uiso 0.5 1 calc PR . . 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 C1 0.024(3) 0.046(3) 0.050(4) -0.009(3) -0.010(2) -0.017(2) C2 0.031(3) 0.047(3) 0.050(4) -0.002(3) -0.012(3) -0.016(3) C3 0.057(4) 0.054(4) 0.061(4) -0.008(3) -0.021(3) -0.026(3) C4 0.069(5) 0.050(4) 0.080(6) -0.006(4) -0.029(4) -0.032(4) C5 0.051(4) 0.050(4) 0.074(5) 0.009(3) -0.024(4) -0.024(3) C6 0.040(3) 0.052(4) 0.046(4) 0.002(3) -0.011(3) -0.027(3) C7 0.073(5) 0.072(5) 0.083(6) -0.011(4) -0.034(4) -0.036(4) C8 0.057(4) 0.083(5) 0.054(4) -0.015(4) -0.025(3) -0.029(4) C9 0.054(4) 0.072(4) 0.032(3) 0.004(3) -0.019(3) -0.031(4) C10 0.041(3) 0.050(4) 0.039(3) -0.006(3) -0.015(3) -0.014(3) C11 0.045(4) 0.072(5) 0.065(5) -0.017(4) -0.018(3) -0.012(3) C12 0.054(5) 0.102(7) 0.100(7) -0.017(5) -0.047(5) -0.009(5) C13 0.117(8) 0.117(8) 0.069(6) 0.026(5) -0.063(6) -0.055(7) C14 0.098(7) 0.116(7) 0.041(4) 0.009(4) -0.032(4) -0.062(6) C15 0.078(6) 0.074(5) 0.065(5) -0.018(4) -0.031(5) -0.010(4) O15 0.075(7) 0.051(6) 0.080(7) 0.003(5) -0.043(6) -0.022(5) C20 0.067(9) 0.051(8) 0.075(10) -0.014(7) -0.014(8) -0.036(7) C22 0.097(16) 0.089(15) 0.22(3) -0.050(16) -0.107(19) 0.013(12) N1 0.040(3) 0.056(3) 0.052(3) -0.008(3) -0.003(3) -0.026(3) N2 0.035(4) 0.120(7) 0.071(5) -0.023(5) -0.018(3) -0.017(4) O1 0.037(2) 0.048(2) 0.042(2) -0.0079(18) -0.0022(17) -0.0256(19) O2 0.055(3) 0.076(3) 0.053(3) -0.024(2) -0.004(2) -0.035(2) O3 0.0257(17) 0.0349(19) 0.0271(18) -0.0011(14) -0.0075(14) -0.0152(15) O13 0.102(4) 0.099(4) 0.047(3) 0.004(3) -0.011(3) -0.074(4) O4 0.082(4) 0.085(4) 0.038(3) -0.015(2) 0.000(2) -0.048(3) O5 0.032(2) 0.064(3) 0.0222(19) -0.0045(17) -0.0119(16) -0.0154(19) O6 0.046(3) 0.094(4) 0.076(4) -0.030(3) -0.032(3) -0.011(3) O7 0.036(2) 0.060(3) 0.044(2) -0.006(2) -0.0035(19) -0.022(2) O8 0.054(3) 0.073(3) 0.051(3) -0.021(2) 0.013(2) -0.039(3) O9 0.056(3) 0.063(3) 0.075(4) -0.030(3) -0.002(3) -0.020(3) O10 0.034(3) 0.115(5) 0.055(3) 0.001(3) -0.007(2) -0.009(3) O11 0.042(3) 0.113(5) 0.077(4) -0.032(3) -0.010(3) -0.036(3) O12 0.051(4) 0.244(11) 0.170(8) -0.045(7) -0.061(5) -0.025(5) Co1 0.0262(4) 0.0512(5) 0.0324(4) -0.0103(3) -0.0071(3) -0.0190(3) Y1 0.0295(3) 0.0548(4) 0.0268(3) -0.0042(2) -0.0012(2) -0.0217(3) C16 0.095(6) 0.110(7) 0.040(4) -0.001(4) -0.008(4) -0.067(6) C21 0.147(16) 0.028(6) 0.050(8) 0.005(6) -0.055(10) -0.020(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.310(7) . ? C1 C2 1.375(9) . ? C1 C6 1.409(8) . ? C2 C3 1.373(9) . ? C2 O2 1.435(7) . ? C3 C4 1.365(10) . ? C3 H3 0.95 . ? C4 C5 1.355(10) . ? C4 H4 0.95 . ? C5 C6 1.428(9) . ? C5 H5 0.95 . ? C6 C7 1.401(10) . ? C7 O13 1.184(9) . ? C7 H7 0.95 . ? C8 O2 1.380(8) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C14 1.380(9) . ? C9 C10 1.408(8) . ? C9 O4 1.433(8) . ? C10 O5 1.325(7) . ? C10 C11 1.411(9) . ? C11 C15 1.417(11) 2_666 ? C11 C12 1.473(11) . ? C12 C13 1.326(13) . ? C12 H12 0.95 . ? C13 C14 1.376(13) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 O6 1.145(9) . ? C15 C11 1.417(11) 2_666 ? C15 H15 0.95 . ? O15 C20 1.226(17) . ? C20 C22 1.51(2) . ? C20 C21 1.53(2) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? N1 O9 1.205(7) . ? N1 O7 1.266(6) . ? N1 O8 1.268(6) . ? N1 Y1 2.847(6) . ? N2 O12 1.210(8) . ? N2 O11 1.219(9) . ? N2 O10 1.266(9) . ? N2 Y1 2.851(6) . ? O1 Co1 2.047(4) . ? O1 Y1 2.286(4) . ? O2 Co1 2.177(5) . ? O3 Co1 2.068(3) . ? O3 Co1 2.072(3) 2_666 ? O3 Y1 2.331(3) . ? O3 H3A 1 . ? O13 Y1 2.352(5) . ? O4 C16 1.426(8) . ? O4 Y1 2.603(5) . ? O5 Co1 2.029(4) 2_666 ? O5 Y1 2.344(4) . ? O6 Co1 2.074(5) . ? O7 Y1 2.403(4) . ? O8 Y1 2.452(4) . ? O10 Y1 2.404(5) . ? O11 Y1 2.474(5) . ? Co1 O5 2.029(4) 2_666 ? Co1 O3 2.072(3) 2_666 ? Co1 Y1 3.4201(9) . ? Co1 Y1 3.4911(9) 2_666 ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 121.2(5) . . ? O1 C1 C6 122.0(5) . . ? C2 C1 C6 116.8(5) . . ? C3 C2 C1 123.1(6) . . ? C3 C2 O2 125.6(6) . . ? C1 C2 O2 111.3(5) . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 121.5(6) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 119.1(7) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C1 123.0(6) . . ? C7 C6 C5 116.9(6) . . ? C1 C6 C5 120.0(6) . . ? O13 C7 C6 128.9(8) . . ? O13 C7 H7 115.5 . . ? C6 C7 H7 115.5 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 122.7(7) . . ? C14 C9 O4 125.5(6) . . ? C10 C9 O4 111.8(5) . . ? O5 C10 C9 118.4(5) . . ? O5 C10 C11 122.8(6) . . ? C9 C10 C11 118.7(6) . . ? C10 C11 C15 126.4(7) . 2_666 ? C10 C11 C12 116.5(7) . . ? C15 C11 C12 117.0(7) 2_666 . ? C13 C12 C11 120.5(7) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 123.5(8) . . ? C12 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C9 117.7(8) . . ? C13 C14 H14 121.2 . . ? C9 C14 H14 121.2 . . ? O6 C15 C11 126.5(9) . 2_666 ? O6 C15 H15 116.7 . . ? C11 C15 H15 116.7 2_666 . ? O15 C20 C22 119.9(16) . . ? O15 C20 C21 121.0(14) . . ? C22 C20 C21 118.9(16) . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O9 N1 O7 122.5(5) . . ? O9 N1 O8 121.4(5) . . ? O7 N1 O8 116.0(5) . . ? O9 N1 Y1 177.9(5) . . ? O7 N1 Y1 56.9(3) . . ? O8 N1 Y1 59.2(3) . . ? O12 N2 O11 120.7(9) . . ? O12 N2 O10 122.7(9) . . ? O11 N2 O10 116.6(6) . . ? O12 N2 Y1 177.1(7) . . ? O11 N2 Y1 59.8(3) . . ? O10 N2 Y1 56.8(3) . . ? C1 O1 Co1 117.6(4) . . ? C1 O1 Y1 134.8(3) . . ? Co1 O1 Y1 104.12(16) . . ? C8 O2 C2 117.5(5) . . ? C8 O2 Co1 127.7(5) . . ? C2 O2 Co1 113.2(4) . . ? Co1 O3 Co1 94.90(14) . 2_666 ? Co1 O3 Y1 101.89(14) . . ? Co1 O3 Y1 104.77(14) 2_666 . ? Co1 O3 H3A 117.3 . . ? Co1 O3 H3A 117.3 2_666 . ? Y1 O3 H3A 117.3 . . ? C7 O13 Y1 131.8(5) . . ? C16 O4 C9 114.2(6) . . ? C16 O4 Y1 125.5(5) . . ? C9 O4 Y1 117.6(3) . . ? C10 O5 Co1 125.7(4) . 2_666 ? C10 O5 Y1 128.3(3) . . ? Co1 O5 Y1 105.72(14) 2_666 . ? C15 O6 Co1 128.6(6) . . ? N1 O7 Y1 96.8(3) . . ? N1 O8 Y1 94.4(3) . . ? N2 O10 Y1 97.0(5) . . ? N2 O11 Y1 95.0(4) . . ? O5 Co1 O1 172.93(16) 2_666 . ? O5 Co1 O3 104.87(15) 2_666 . ? O1 Co1 O3 81.72(14) . . ? O5 Co1 O3 80.43(14) 2_666 2_666 ? O1 Co1 O3 97.83(14) . 2_666 ? O3 Co1 O3 85.10(14) . 2_666 ? O5 Co1 O6 88.7(2) 2_666 . ? O1 Co1 O6 93.3(2) . . ? O3 Co1 O6 95.03(17) . . ? O3 Co1 O6 168.8(2) 2_666 . ? O5 Co1 O2 98.09(17) 2_666 . ? O1 Co1 O2 75.32(16) . . ? O3 Co1 O2 157.03(16) . . ? O3 Co1 O2 98.37(16) 2_666 . ? O6 Co1 O2 85.9(2) . . ? O5 Co1 Y1 146.44(12) 2_666 . ? O1 Co1 Y1 40.40(11) . . ? O3 Co1 Y1 41.82(9) . . ? O3 Co1 Y1 97.01(10) 2_666 . ? O6 Co1 Y1 90.44(15) . . ? O2 Co1 Y1 115.30(12) . . ? O5 Co1 Y1 40.27(10) 2_666 2_666 ? O1 Co1 Y1 137.86(11) . 2_666 ? O3 Co1 Y1 94.99(9) . 2_666 ? O3 Co1 Y1 40.21(9) 2_666 2_666 ? O6 Co1 Y1 128.79(17) . 2_666 ? O2 Co1 Y1 102.31(12) . 2_666 ? Y1 Co1 Y1 127.63(2) . 2_666 ? O1 Y1 O3 71.33(13) . . ? O1 Y1 O5 86.46(13) . . ? O3 Y1 O5 69.00(12) . . ? O1 Y1 O13 73.32(17) . . ? O3 Y1 O13 143.45(17) . . ? O5 Y1 O13 99.98(17) . . ? O1 Y1 O7 153.43(14) . . ? O3 Y1 O7 82.13(13) . . ? O5 Y1 O7 82.85(14) . . ? O13 Y1 O7 132.49(17) . . ? O1 Y1 O10 95.47(18) . . ? O3 Y1 O10 72.91(15) . . ? O5 Y1 O10 138.99(17) . . ? O13 Y1 O10 119.9(2) . . ? O7 Y1 O10 77.4(2) . . ? O1 Y1 O8 149.06(14) . . ? O3 Y1 O8 126.46(14) . . ? O5 Y1 O8 122.35(15) . . ? O13 Y1 O8 89.34(18) . . ? O7 Y1 O8 52.55(14) . . ? O10 Y1 O8 70.80(18) . . ? O1 Y1 O11 76.57(16) . . ? O3 Y1 O11 110.96(17) . . ? O5 Y1 O11 161.66(18) . . ? O13 Y1 O11 68.8(2) . . ? O7 Y1 O11 115.47(17) . . ? O10 Y1 O11 51.3(2) . . ? O8 Y1 O11 73.27(17) . . ? O1 Y1 O4 119.93(15) . . ? O3 Y1 O4 128.49(13) . . ? O5 Y1 O4 62.50(14) . . ? O13 Y1 O4 64.47(17) . . ? O7 Y1 O4 75.91(15) . . ? O10 Y1 O4 142.08(18) . . ? O8 Y1 O4 71.63(17) . . ? O11 Y1 O4 120.54(18) . . ? O1 Y1 N1 166.70(15) . . ? O3 Y1 N1 104.17(14) . . ? O5 Y1 N1 103.83(14) . . ? O13 Y1 N1 112.36(17) . . ? O7 Y1 N1 26.21(13) . . ? O10 Y1 N1 71.23(19) . . ? O8 Y1 N1 26.38(13) . . ? O11 Y1 N1 94.01(17) . . ? O4 Y1 N1 72.89(16) . . ? O1 Y1 N2 86.15(19) . . ? O3 Y1 N2 92.87(19) . . ? O5 Y1 N2 161.80(19) . . ? O13 Y1 N2 93.8(2) . . ? O7 Y1 N2 96.6(2) . . ? O10 Y1 N2 26.2(2) . . ? O8 Y1 N2 69.29(19) . . ? O11 Y1 N2 25.2(2) . . ? O4 Y1 N2 135.14(19) . . ? N1 Y1 N2 81.5(2) . . ? O1 Y1 Co1 35.47(10) . . ? O3 Y1 Co1 36.28(9) . . ? O5 Y1 Co1 79.15(9) . . ? O13 Y1 Co1 108.76(14) . . ? O7 Y1 Co1 118.21(10) . . ? O10 Y1 Co1 79.19(13) . . ? O8 Y1 Co1 149.83(12) . . ? O11 Y1 Co1 90.62(13) . . ? O4 Y1 Co1 137.70(11) . . ? N1 Y1 Co1 137.39(11) . . ? N2 Y1 Co1 85.19(14) . . ? O4 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF