# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2010 data_General _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _audit_creation_date 2006-12-28 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Wing-Tak Wong' _publ_contact_author_email wtwong@hkucc.hku.hk _publ_contact_author_fax '(852) 2547 2933' _publ_contact_author_phone '(852) 2859 2157' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ? # 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Ga-Lai Law.' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; 'Ka-Leung Wong.' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; 'Kwok-Kin Lau.' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; 'Hoi-Lam Tam.' . ; Department of Physics Hong Kong Baptist University 224 Waterloo Road Kowloon Tong Hong Kong SAR, P. R. CHINA ; ; Kwok-Wai Cheah ; . ; Department of Physics Hong Kong Baptist University 224 Waterloo Road Kowloon Tong Hong Kong SAR, P. R. CHINA ; 'Wing-Tak Wong.' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_section_references ; Bruker AXS Inc. (1998) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT, version 6.02, Madison, Wisconsin, USA. Flack, H.D. (1983). Acta Cryst. A39, 876-881. Johnson, C. K. (1976). ORTEP-II. Report ORNL-5138. Oak Ridge National Laboratory, Tennesse, USA. Larson, A. C. (1970), Crystallographic Computing, eq. 22, 291-294. ed F. R. Ahmed, Munksgaard, Copenhagen. Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. Sheldrick, G.M. (1997) SADABS, SHELXS97, G\"ottingen University, G\"ottingen, Germany. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; All non-H atoms were refined anisotropically. The C-bound H atoms were placed at their geometrically calculated positions with C-H = 0.95 \%A and in the riding model with U~iso~(H) = 1.2 U~eq~(C). Data merged with Friedels pairs not averaged. ; #============================================================================== data_Eu-wt0964w _database_code_depnum_ccdc_archive 'CCDC 600403' # Kin-Eu-cinnamate _audit_creation_date 2006-12-12 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Eu O6 ' _chemical_formula_moiety 'C27 H21 Eu O6 ' _chemical_formula_weight 593.42 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 22.649(4) _cell_length_b 22.649(4) _cell_length_c 7.744(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3440.3(10) _cell_formula_units_Z 6 _cell_measurement_reflns_used 6841 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 303(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764.00 _exptl_absorpt_coefficient_mu 2.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.801 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ' Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6841 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9841 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9841 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1605 _reflns_number_gt 1309 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0240 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1317 _refine_ls_number_parameters 112 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.005]' _refine_ls_shift/su_max 0.0310 _refine_diff_density_max 1.48 _refine_diff_density_min -0.84 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 4.6(38) _refine_ls_abs_structure_details 'Flack (1983). 682 Friedel Pairs' _refine_ls_abs_structure_Flack -0.05(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Eu Eu -0.158 3.668 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Eu(1) Eu 0.0000 0.0000 0.3330(1) 0.01771(6) Uani 1.00 3 d S . . O(1) O 0.08047(13) 0.0598(1) 0.5990(4) 0.0248(7) Uani 1.00 1 d . . . O(2) O 0.0774(2) 0.1186(2) 0.3785(4) 0.0372(8) Uani 1.00 1 d . . . C(1) C 0.1000(2) 0.1171(2) 0.5242(5) 0.0250(10) Uani 1.00 1 d . . . C(2) C 0.1505(2) 0.1805(2) 0.6087(5) 0.0280(10) Uani 1.00 1 d . . . C(3) C 0.1654(2) 0.2409(2) 0.5491(5) 0.0318(12) Uani 1.00 1 d . . . C(4) C 0.2125(2) 0.3083(2) 0.6237(5) 0.0316(11) Uani 1.00 1 d . . . C(5) C 0.2077(3) 0.3643(2) 0.5702(6) 0.0409(13) Uani 1.00 1 d . . . C(6) C 0.2500(3) 0.4285(2) 0.6415(7) 0.048(2) Uani 1.00 1 d . . . C(7) C 0.2971(3) 0.4381(2) 0.7633(6) 0.051(2) Uani 1.00 1 d . . . C(8) C 0.3032(3) 0.3827(3) 0.8169(7) 0.047(1) Uani 1.00 1 d . . . C(9) C 0.2611(2) 0.3184(2) 0.7491(6) 0.0379(12) Uani 1.00 1 d . . . H(1) H 0.1732 0.1780 0.7093 0.034 Uiso 1.00 1 c R . . H(2) H 0.1430 0.2410 0.4454 0.038 Uiso 1.00 1 c R . . H(3) H 0.1754 0.3588 0.4843 0.049 Uiso 1.00 1 c R . . H(4) H 0.2457 0.4662 0.6042 0.057 Uiso 1.00 1 c R . . H(5) H 0.3256 0.4821 0.8112 0.061 Uiso 1.00 1 c R . . H(6) H 0.3365 0.3891 0.9007 0.056 Uiso 1.00 1 c R . . H(7) H 0.2653 0.2808 0.7880 0.046 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Eu(1) 0.01918(10) 0.01918(10) 0.0148(1) 0.00958(5) 0.0000 0.0000 O(1) 0.0222(13) 0.0221(13) 0.027(2) 0.0090(12) 0.0036(12) 0.0001(12) O(2) 0.046(2) 0.024(2) 0.029(2) 0.008(1) -0.011(1) -0.0012(13) C(1) 0.022(2) 0.025(2) 0.026(2) 0.010(2) 0.005(2) 0.002(2) C(2) 0.027(2) 0.026(2) 0.024(2) 0.008(2) -0.003(2) -0.001(2) C(3) 0.031(2) 0.029(2) 0.029(3) 0.010(2) -0.003(2) -0.001(2) C(4) 0.034(2) 0.024(2) 0.029(2) 0.008(2) 0.002(2) -0.002(2) C(5) 0.041(3) 0.033(2) 0.049(3) 0.018(2) 0.001(2) 0.004(2) C(6) 0.057(3) 0.026(2) 0.059(4) 0.020(2) 0.017(3) 0.002(2) C(7) 0.051(3) 0.028(3) 0.051(4) 0.003(2) 0.009(3) -0.011(2) C(8) 0.043(3) 0.039(3) 0.042(3) 0.009(2) -0.004(2) -0.005(2) C(9) 0.039(3) 0.028(2) 0.038(3) 0.011(2) -0.003(2) 0.001(2) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Eu(1) O(1) 2.633(3) ? . . Eu(1) O(1) 2.633(3) ? . 2_555 Eu(1) O(1) 2.633(3) ? . 3_555 Eu(1) O(1) 2.443(3) ? . 4_554 Eu(1) O(1) 2.443(3) ? . 5_554 Eu(1) O(1) 2.443(3) ? . 6_554 Eu(1) O(2) 2.389(3) ? . . Eu(1) O(2) 2.389(4) ? . 2_555 Eu(1) O(2) 2.389(4) ? . 3_555 O(1) Eu(1) 2.443(3) ? . 4_555 O(1) C(1) 1.281(5) ? . . O(2) C(1) 1.246(5) ? . . C(1) C(2) 1.469(5) ? . . C(2) C(3) 1.317(7) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.474(5) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.390(8) ? . . C(4) C(9) 1.399(7) ? . . C(5) C(6) 1.394(6) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.359(8) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.393(9) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.386(6) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Eu(1) O(1) 65.26(9) ? 2_555 . . O(1) Eu(1) O(1) 65.26(8) ? 3_555 . . O(1) Eu(1) O(1) 124.75(9) ? 4_554 . . O(1) Eu(1) O(1) 102.92(9) ? 5_554 . . O(1) Eu(1) O(1) 161.3(1) ? 6_554 . . O(2) Eu(1) O(1) 51.4(1) ? . . . O(2) Eu(1) O(1) 116.1(1) ? 2_555 . . O(2) Eu(1) O(1) 80.7(1) ? 3_555 . . Eu(1) O(1) C(1) 88.1(2) ? . . . Eu(1) O(1) Eu(1) 99.34(8) ? . . 4_555 O(1) Eu(1) O(1) 65.3(1) ? 3_555 . 2_555 O(1) Eu(1) O(1) 102.9(1) ? 4_554 . 2_555 O(1) Eu(1) O(1) 161.26(8) ? 5_554 . 2_555 O(1) Eu(1) O(1) 124.75(8) ? 6_554 . 2_555 O(2) Eu(1) O(1) 80.7(1) ? . . 2_555 O(2) Eu(1) O(1) 51.38(9) ? 2_555 . 2_555 O(2) Eu(1) O(1) 116.1(1) ? 3_555 . 2_555 Eu(1) O(1) C(1) 88.1(2) ? . 2_555 2_555 Eu(1) O(1) Eu(1) 99.3(1) ? . 2_555 4_555 O(1) Eu(1) O(1) 161.26(9) ? 4_554 . 3_555 O(1) Eu(1) O(1) 124.8(1) ? 5_554 . 3_555 O(1) Eu(1) O(1) 102.92(9) ? 6_554 . 3_555 O(2) Eu(1) O(1) 116.1(1) ? . . 3_555 O(2) Eu(1) O(1) 80.7(1) ? 2_555 . 3_555 O(2) Eu(1) O(1) 51.4(1) ? 3_555 . 3_555 Eu(1) O(1) C(1) 88.1(2) ? . 3_555 3_555 Eu(1) O(1) Eu(1) 99.3(1) ? . 3_555 4_555 O(1) Eu(1) O(1) 71.1(1) ? 5_554 . 4_554 O(1) Eu(1) O(1) 71.1(1) ? 6_554 . 4_554 O(2) Eu(1) O(1) 73.9(1) ? . . 4_554 O(2) Eu(1) O(1) 80.6(1) ? 2_555 . 4_554 Eu(1) O(1) C(1) 132.9(3) ? . 4_554 4_554 O(1) Eu(1) O(1) 71.06(9) ? 6_554 . 5_554 O(2) Eu(1) O(1) 80.6(1) ? . . 5_554 O(2) Eu(1) O(1) 140.3(1) ? 2_555 . 5_554 O(2) Eu(1) O(1) 73.9(1) ? 3_555 . 5_554 Eu(1) O(1) C(1) 132.9(2) ? . 5_554 5_554 O(2) Eu(1) O(1) 140.3(1) ? . . 6_554 O(2) Eu(1) O(1) 73.9(1) ? 2_555 . 6_554 O(2) Eu(1) O(1) 80.6(1) ? 3_555 . 6_554 Eu(1) O(1) C(1) 132.9(3) ? . 6_554 6_554 O(2) Eu(1) O(2) 117.9(1) ? 2_555 . . O(2) Eu(1) O(2) 117.9(1) ? 3_555 . . Eu(1) O(2) C(1) 100.5(3) ? . . . O(2) Eu(1) O(2) 117.9(1) ? 3_555 . 2_555 Eu(1) O(2) C(1) 100.5(3) ? . 2_555 2_555 Eu(1) O(2) C(1) 100.5(4) ? . 3_555 3_555 O(1) Eu(1) O(1) 71.1(1) ? . 4_555 2_555 O(1) Eu(1) O(1) 71.06(9) ? . 4_555 3_555 C(1) O(1) Eu(1) 132.9(3) ? . . 4_555 O(1) Eu(1) O(2) 73.9(1) ? . 4_555 4_555 O(1) Eu(1) O(2) 80.6(1) ? . 4_555 5_555 O(1) C(1) O(2) 120.0(3) ? . . . O(1) C(1) C(2) 119.6(4) ? . . . O(2) C(1) C(2) 120.4(4) ? . . . C(1) C(2) C(3) 121.9(4) ? . . . C(1) C(2) H(1) 119.0450 ? . . . H(1) C(2) C(3) 119.0444 ? . . . C(2) C(3) H(2) 116.0532 ? . . . C(2) C(3) C(4) 127.9(4) ? . . . H(2) C(3) C(4) 116.0529 ? . . . C(3) C(4) C(5) 118.8(4) ? . . . C(3) C(4) C(9) 123.0(5) ? . . . C(9) C(4) C(5) 118.2(4) ? . . . C(4) C(5) C(6) 120.6(5) ? . . . C(4) C(5) H(3) 119.7000 ? . . . C(4) C(9) H(7) 119.7861 ? . . . C(4) C(9) C(8) 120.4(5) ? . . . H(3) C(5) C(6) 119.6991 ? . . . C(5) C(6) C(7) 121.1(6) ? . . . C(5) C(6) H(4) 119.4617 ? . . . C(6) C(7) C(8) 119.2(4) ? . . . H(4) C(6) C(7) 119.4621 ? . . . C(6) C(7) H(5) 120.4245 ? . . . C(7) C(8) C(9) 120.6(5) ? . . . H(5) C(7) C(8) 120.4241 ? . . . C(7) C(8) H(6) 119.7088 ? . . . C(8) C(9) H(7) 119.7866 ? . . . H(6) C(8) C(9) 119.7081 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Eu(1) Eu(1) 3.872(2) ? . 4_555 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC611367 rev Tb-wt0997w.cif' # CCDC611367 rev ised Tb -wt0997w data_Tb-wt0997w _database_code_depnum_ccdc_archive 'CCDC 611367' # -Tb-cinnamate _audit_creation_date 2006-12-11 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 O6 Tb ' _chemical_formula_moiety 'C27 H21 O6 Tb ' _chemical_formula_weight 600.38 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 22.647(4) _cell_length_b 22.647(4) _cell_length_c 7.703(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3421.5(10) _cell_formula_units_Z 6 _cell_measurement_reflns_used 7000 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 303(1) #------------------------------------------------------------------------------ _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776.00 _exptl_absorpt_coefficient_mu 3.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7000 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9947 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9947 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1703 _reflns_number_gt 1374 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0380 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1381 _refine_ls_number_parameters 111 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.155]' _refine_ls_shift/su_max 0.0030 _refine_diff_density_max 1.56 _refine_diff_density_min -1.82 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 775 Friedel Pairs' _refine_ls_abs_structure_Flack -0.02(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Tb Tb -0.172 4.154 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Tb(1) Tb 0.0000 0.0000 0.1673(2) 0.01761(8) Uani 1.00 3 d S . . O(1) O 0.0800(3) 0.0586(3) 0.4354(7) 0.0264(13) Uani 1.00 1 d . . . O(2) O 0.0764(3) 0.1170(3) 0.2144(7) 0.037(2) Uani 1.00 1 d . . . C(1) C 0.0993(4) 0.1160(4) 0.3604(9) 0.026(2) Uani 1.00 1 d . . . C(2) C 0.1505(4) 0.1800(4) 0.4446(10) 0.029(2) Uani 1.00 1 d . . . C(3) C 0.1648(4) 0.2402(4) 0.3833(10) 0.030(2) Uani 1.00 1 d . . . C(4) C 0.2119(4) 0.3077(4) 0.4585(10) 0.031(2) Uani 1.00 1 d . . . C(5) C 0.2068(5) 0.3636(4) 0.4056(12) 0.041(2) Uani 1.00 1 d . . . C(6) C 0.2487(5) 0.4278(5) 0.476(1) 0.048(3) Uani 1.00 1 d . . . C(7) C 0.2967(5) 0.4375(5) 0.5977(12) 0.048(3) Uani 1.00 1 d . . . C(8) C 0.3032(5) 0.3824(5) 0.6510(12) 0.046(3) Uani 1.00 1 d . . . C(9) C 0.2611(4) 0.3178(4) 0.5820(11) 0.036(2) Uani 1.00 1 d . . . H(1) H 0.1736 0.1778 0.5453 0.032 Uiso 1.00 1 c R . . H(2) H 0.1424 0.2400 0.2790 0.034 Uiso 1.00 1 c R . . H(3) H 0.1741 0.3578 0.3201 0.049 Uiso 1.00 1 c R . . H(4) H 0.2441 0.4653 0.4391 0.057 Uiso 1.00 1 c R . . H(5) H 0.3252 0.4815 0.6454 0.050 Uiso 1.00 1 c R . . H(6) H 0.3367 0.3889 0.7350 0.049 Uiso 1.00 1 c R . . H(7) H 0.2658 0.2804 0.6192 0.040 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tb(1) 0.0182(1) 0.0182(1) 0.0164(2) 0.00911(7) 0.0000 0.0000 O(1) 0.022(2) 0.023(3) 0.031(3) 0.009(2) 0.002(2) 0.001(2) O(2) 0.046(3) 0.026(3) 0.027(3) 0.009(3) -0.007(2) 0.000(2) C(1) 0.026(4) 0.024(4) 0.026(4) 0.012(3) 0.007(3) -0.000(3) C(2) 0.027(4) 0.027(4) 0.027(4) 0.009(3) -0.003(3) -0.000(3) C(3) 0.029(4) 0.027(4) 0.029(4) 0.010(3) -0.003(3) -0.002(3) C(4) 0.034(4) 0.023(4) 0.029(4) 0.009(3) 0.000(3) -0.000(3) C(5) 0.045(5) 0.033(4) 0.045(5) 0.020(4) -0.001(4) 0.001(4) C(6) 0.058(6) 0.026(4) 0.060(6) 0.021(4) 0.016(5) 0.003(4) C(7) 0.050(6) 0.027(5) 0.048(6) 0.004(5) 0.008(5) -0.010(4) C(8) 0.041(5) 0.038(5) 0.043(5) 0.008(4) -0.005(4) -0.006(4) C(9) 0.038(5) 0.027(4) 0.035(4) 0.011(4) -0.002(4) 0.002(3) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Tb(1) O(1) 2.628(5) ? . . Tb(1) O(1) 2.628(6) ? . 2_555 Tb(1) O(1) 2.628(6) ? . 3_555 Tb(1) O(1) 2.414(6) ? . 4_554 Tb(1) O(1) 2.414(6) ? . 5_554 Tb(1) O(1) 2.414(5) ? . 6_554 Tb(1) O(2) 2.359(5) ? . . Tb(1) O(2) 2.359(7) ? . 2_555 Tb(1) O(2) 2.359(8) ? . 3_555 O(1) Tb(1) 2.414(5) ? . 4_555 O(1) C(1) 1.28(1) ? . . O(2) C(1) 1.24(1) ? . . C(1) C(2) 1.479(9) ? . . C(2) C(3) 1.32(1) ? . . C(2) H(1) 0.9501 ? . . C(3) C(4) 1.48(1) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.39(2) ? . . C(4) C(9) 1.39(1) ? . . C(5) C(6) 1.39(1) ? . . C(5) H(3) 0.9499 ? . . C(6) C(7) 1.37(2) ? . . C(6) H(4) 0.9499 ? . . C(7) C(8) 1.39(2) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.39(1) ? . . C(8) H(6) 0.9501 ? . . C(9) H(7) 0.9501 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Tb(1) O(1) 64.7(2) ? 2_555 . . O(1) Tb(1) O(1) 64.7(2) ? 3_555 . . O(1) Tb(1) O(1) 125.5(2) ? 4_554 . . O(1) Tb(1) O(1) 102.8(2) ? 5_554 . . O(1) Tb(1) O(1) 160.4(2) ? 6_554 . . O(2) Tb(1) O(1) 51.6(2) ? . . . O(2) Tb(1) O(1) 115.6(2) ? 2_555 . . O(2) Tb(1) O(1) 80.0(2) ? 3_555 . . Tb(1) O(1) C(1) 87.6(4) ? . . . Tb(1) O(1) Tb(1) 99.5(2) ? . . 4_555 O(1) Tb(1) O(1) 64.7(2) ? 3_555 . 2_555 O(1) Tb(1) O(1) 102.8(2) ? 4_554 . 2_555 O(1) Tb(1) O(1) 160.4(2) ? 5_554 . 2_555 O(1) Tb(1) O(1) 125.5(2) ? 6_554 . 2_555 O(2) Tb(1) O(1) 80.0(2) ? . . 2_555 O(2) Tb(1) O(1) 51.6(2) ? 2_555 . 2_555 O(2) Tb(1) O(1) 115.6(2) ? 3_555 . 2_555 Tb(1) O(1) C(1) 87.6(5) ? . 2_555 2_555 Tb(1) O(1) Tb(1) 99.5(2) ? . 2_555 4_555 O(1) Tb(1) O(1) 160.4(2) ? 4_554 . 3_555 O(1) Tb(1) O(1) 125.5(2) ? 5_554 . 3_555 O(1) Tb(1) O(1) 102.8(2) ? 6_554 . 3_555 O(2) Tb(1) O(1) 115.6(2) ? . . 3_555 O(2) Tb(1) O(1) 80.0(2) ? 2_555 . 3_555 O(2) Tb(1) O(1) 51.6(2) ? 3_555 . 3_555 Tb(1) O(1) C(1) 87.6(4) ? . 3_555 3_555 Tb(1) O(1) Tb(1) 99.5(2) ? . 3_555 4_555 O(1) Tb(1) O(1) 71.3(2) ? 5_554 . 4_554 O(1) Tb(1) O(1) 71.3(2) ? 6_554 . 4_554 O(2) Tb(1) O(1) 74.5(2) ? . . 4_554 O(2) Tb(1) O(1) 80.4(2) ? 2_555 . 4_554 O(2) Tb(1) O(1) 140.9(2) ? 3_555 . 4_554 Tb(1) O(1) C(1) 132.2(5) ? . 4_554 4_554 O(1) Tb(1) O(1) 71.3(2) ? 6_554 . 5_554 O(2) Tb(1) O(1) 80.4(2) ? . . 5_554 O(2) Tb(1) O(1) 140.9(2) ? 2_555 . 5_554 O(2) Tb(1) O(1) 74.5(2) ? 3_555 . 5_554 Tb(1) O(1) C(1) 132.2(4) ? . 5_554 5_554 O(2) Tb(1) O(1) 140.9(2) ? . . 6_554 O(2) Tb(1) O(1) 74.5(2) ? 2_555 . 6_554 O(2) Tb(1) O(1) 80.4(2) ? 3_555 . 6_554 Tb(1) O(1) C(1) 132.2(6) ? . 6_554 6_554 O(2) Tb(1) O(2) 117.7(3) ? 2_555 . . O(2) Tb(1) O(2) 117.7(2) ? 3_555 . . Tb(1) O(2) C(1) 101.3(5) ? . . . O(2) Tb(1) O(2) 117.7(2) ? 3_555 . 2_555 Tb(1) O(2) C(1) 101.3(5) ? . 2_555 2_555 Tb(1) O(2) C(1) 101.3(7) ? . 3_555 3_555 O(1) Tb(1) O(1) 71.3(2) ? . 4_555 2_555 O(1) Tb(1) O(1) 71.3(2) ? . 4_555 3_555 C(1) O(1) Tb(1) 132.2(6) ? . . 4_555 O(1) Tb(1) O(2) 74.5(2) ? . 4_555 4_555 O(1) Tb(1) O(2) 80.4(2) ? . 4_555 5_555 O(1) C(1) O(2) 119.5(6) ? . . . O(1) C(1) C(2) 119.9(7) ? . . . O(2) C(1) C(2) 120.5(7) ? . . . C(1) C(2) C(3) 121.5(8) ? . . . C(1) C(2) H(1) 119.2305 ? . . . H(1) C(2) C(3) 119.2207 ? . . . C(2) C(3) H(2) 116.3208 ? . . . C(2) C(3) C(4) 127.4(8) ? . . . H(2) C(3) C(4) 116.3251 ? . . . C(3) C(4) C(5) 118.9(8) ? . . . C(3) C(4) C(9) 122.7(9) ? . . . C(9) C(4) C(5) 118.4(7) ? . . . C(4) C(5) C(6) 120(1) ? . . . C(4) C(5) H(3) 119.5432 ? . . . C(4) C(9) H(7) 119.8664 ? . . . C(4) C(9) C(8) 120(1) ? . . . H(3) C(5) C(6) 119.5508 ? . . . C(5) C(6) C(7) 120(1) ? . . . C(5) C(6) H(4) 119.6879 ? . . . C(6) C(7) C(8) 119.4(8) ? . . . H(4) C(6) C(7) 119.6888 ? . . . C(6) C(7) H(5) 120.2885 ? . . . C(7) C(8) C(9) 120.4(9) ? . . . H(5) C(7) C(8) 120.2944 ? . . . C(7) C(8) H(6) 119.8182 ? . . . C(8) C(9) H(7) 119.8653 ? . . . H(6) C(8) C(9) 119.8250 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Tb(1) Tb(1) 3.852(3) ? . 4_555 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC611368 rev Gd-wt0999w.cif' # CCDC611368 revised Gd -wt0999w data_Gd-wt0999w _database_code_depnum_ccdc_archive 'CCDC 611368' # Kin-K296-Gd-cinnamate _audit_creation_date 2006-12-07 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Gd O6 ' _chemical_formula_moiety 'C27 H21 Gd O6 ' _chemical_formula_weight 598.71 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 22.654(6) _cell_length_b 22.654(6) _cell_length_c 7.722(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3432.0(16) _cell_formula_units_Z 6 _cell_measurement_reflns_used 6917 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1770.00 _exptl_absorpt_coefficient_mu 2.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.707 _exptl_absorpt_correction_T_max 0.863 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ' Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6917 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9915 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9915 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1701 _reflns_number_gt 1472 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0220 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1478 _refine_ls_number_parameters 112 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.015]' _refine_ls_shift/su_max 0.0210 _refine_diff_density_max 0.70 _refine_diff_density_min -0.74 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 2.3(34) _refine_ls_abs_structure_details 'Flack (1983). 773 Friedel Pairs' _refine_ls_abs_structure_Flack 0.00(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Gd Gd -0.165 3.904 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Gd(1) Gd 0.0000 0.0000 0.33577(12) 0.01705(5) Uani 1.00 3 d S . . O(1) O -0.02107(12) 0.05908(12) 0.6021(3) 0.0254(6) Uani 1.00 1 d . . . O(2) O 0.0410(2) 0.1180(1) 0.3814(3) 0.0368(7) Uani 1.00 1 d . . . C(1) C 0.0167(2) 0.1165(2) 0.5279(4) 0.0249(8) Uani 1.00 1 d . . . C(2) C 0.0297(2) 0.1802(2) 0.6123(4) 0.0277(9) Uani 1.00 1 d . . . C(3) C 0.0755(2) 0.2406(2) 0.5515(4) 0.0307(9) Uani 1.00 1 d . . . C(4) C 0.0959(2) 0.3081(2) 0.6262(4) 0.0312(9) Uani 1.00 1 d . . . C(5) C 0.1567(2) 0.3639(2) 0.5734(5) 0.0399(11) Uani 1.00 1 d . . . C(6) C 0.1791(2) 0.4281(2) 0.6438(6) 0.0466(11) Uani 1.00 1 d . . . C(7) C 0.1410(3) 0.4377(2) 0.7662(5) 0.0494(13) Uani 1.00 1 d . . . C(8) C 0.0794(2) 0.3826(2) 0.8197(6) 0.0459(12) Uani 1.00 1 d . . . C(9) C 0.0568(2) 0.3179(2) 0.7505(5) 0.0373(10) Uani 1.00 1 d . . . H(1) H 0.0046 0.1779 0.7131 0.033 Uiso 1.00 1 c R . . H(2) H 0.0979 0.2406 0.4475 0.037 Uiso 1.00 1 c R . . H(3) H 0.1834 0.3582 0.4876 0.048 Uiso 1.00 1 c R . . H(4) H 0.2212 0.4656 0.6068 0.056 Uiso 1.00 1 c R . . H(5) H 0.1565 0.4817 0.8143 0.059 Uiso 1.00 1 c R . . H(6) H 0.0525 0.3891 0.9038 0.055 Uiso 1.00 1 c R . . H(7) H 0.0147 0.2804 0.7879 0.045 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Gd(1) 0.01798(9) 0.01798(9) 0.01520(11) 0.00899(4) 0.0000 0.0000 O(1) 0.0259(11) 0.0213(11) 0.0287(11) 0.0117(9) -0.0020(10) -0.0002(10) O(2) 0.052(2) 0.0261(13) 0.0291(13) 0.0174(13) 0.0092(12) 0.0001(10) C(1) 0.024(2) 0.025(2) 0.027(2) 0.012(1) -0.0028(12) 0.0016(13) C(2) 0.036(2) 0.027(2) 0.024(2) 0.019(2) 0.0034(13) -0.0013(13) C(3) 0.036(2) 0.027(2) 0.029(2) 0.016(2) 0.001(2) -0.003(1) C(4) 0.038(2) 0.021(2) 0.032(2) 0.013(2) -0.001(1) 0.0006(13) C(5) 0.037(2) 0.033(2) 0.046(2) 0.014(2) 0.004(2) 0.004(2) C(6) 0.042(2) 0.025(2) 0.058(3) 0.006(2) -0.014(2) 0.002(2) C(7) 0.070(3) 0.027(2) 0.049(3) 0.023(2) -0.021(2) -0.009(2) C(8) 0.064(3) 0.037(2) 0.042(2) 0.029(2) -0.001(2) -0.007(2) C(9) 0.045(2) 0.029(2) 0.038(2) 0.018(2) 0.004(2) 0.001(2) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Gd(1) Gd(1) 3.861(1) ? . 4_555 Gd(1) O(1) 2.624(3) ? . . Gd(1) O(1) 2.624(2) ? . 2_555 Gd(1) O(1) 2.624(3) ? . 3_555 Gd(1) O(2) 2.377(3) ? . . Gd(1) O(2) 2.377(3) ? . 2_555 Gd(1) O(2) 2.377(4) ? . 3_555 O(1) Gd(1) 2.432(3) ? . 4_555 O(1) C(1) 1.280(4) ? . . O(2) C(1) 1.251(4) ? . . C(1) C(2) 1.473(6) ? . . C(2) C(3) 1.322(4) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.475(5) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.386(5) ? . . C(4) C(9) 1.397(6) ? . . C(5) C(6) 1.389(6) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.369(7) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.391(5) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.396(6) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Gd(1) Gd(1) O(1) 42.10(7) ? . 4_555 . O(1) Gd(1) Gd(1) 38.41(7) ? . . 4_555 Gd(1) Gd(1) O(1) 42.10(5) ? . 4_555 2_555 O(1) Gd(1) Gd(1) 38.41(5) ? 2_555 . 4_555 Gd(1) Gd(1) O(1) 42.10(6) ? . 4_555 3_555 O(1) Gd(1) Gd(1) 38.41(6) ? 3_555 . 4_555 O(2) Gd(1) Gd(1) 81.48(6) ? . . 4_555 O(2) Gd(1) Gd(1) 81.48(6) ? 2_555 . 4_555 O(2) Gd(1) Gd(1) 81.48(6) ? 3_555 . 4_555 Gd(1) Gd(1) O(2) 98.52(6) ? . 4_555 4_555 Gd(1) Gd(1) O(2) 98.52(6) ? . 4_555 6_555 Gd(1) O(1) Gd(1) 99.5(1) ? . . 4_555 O(1) Gd(1) O(1) 65.10(8) ? 2_555 . . O(1) Gd(1) O(1) 65.1(1) ? 3_555 . . O(2) Gd(1) O(1) 51.60(8) ? . . . O(2) Gd(1) O(1) 80.42(9) ? 2_555 . . O(2) Gd(1) O(1) 116.06(9) ? 3_555 . . Gd(1) O(1) C(1) 88.2(2) ? . . . Gd(1) O(1) Gd(1) 99.50(7) ? . 2_555 4_555 O(1) Gd(1) O(1) 65.10(7) ? 3_555 . 2_555 O(2) Gd(1) O(1) 116.06(9) ? . . 2_555 O(2) Gd(1) O(1) 51.60(9) ? 2_555 . 2_555 O(2) Gd(1) O(1) 80.42(9) ? 3_555 . 2_555 Gd(1) O(1) C(1) 88.2(2) ? . 2_555 2_555 Gd(1) O(1) Gd(1) 99.5(1) ? . 3_555 4_555 O(2) Gd(1) O(1) 80.4(1) ? . . 3_555 O(2) Gd(1) O(1) 116.06(9) ? 2_555 . 3_555 O(2) Gd(1) O(1) 51.60(9) ? 3_555 . 3_555 Gd(1) O(1) C(1) 88.2(2) ? . 3_555 3_555 O(2) Gd(1) O(2) 117.8(1) ? 2_555 . . O(2) Gd(1) O(2) 117.8(1) ? 2_555 . . Gd(1) O(2) C(1) 100.6(2) ? . . . O(2) Gd(1) O(2) 117.8(1) ? 3_555 . 2_555 Gd(1) O(2) C(1) 100.6(2) ? . 2_555 2_555 Gd(1) O(2) C(1) 100.6(3) ? . 3_555 3_555 O(1) Gd(1) O(1) 70.98(9) ? . 4_555 2_555 O(1) Gd(1) O(1) 71.0(1) ? . 4_555 3_555 C(1) O(1) Gd(1) 132.5(2) ? . . 4_555 O(1) Gd(1) O(2) 74.13(9) ? . 4_555 4_555 O(1) Gd(1) O(2) 80.39(9) ? . 4_555 6_555 O(1) C(1) O(2) 119.6(3) ? . . . O(1) C(1) C(2) 120.2(3) ? . . . O(2) C(1) C(2) 120.2(3) ? . . . C(1) C(2) C(3) 121.8(3) ? . . . C(1) C(2) H(1) 119.0918 ? . . . H(1) C(2) C(3) 119.0921 ? . . . C(2) C(3) H(2) 116.1625 ? . . . C(2) C(3) C(4) 127.7(3) ? . . . H(2) C(3) C(4) 116.1637 ? . . . C(3) C(4) C(5) 119.0(4) ? . . . C(3) C(4) C(9) 122.5(3) ? . . . C(9) C(4) C(5) 118.5(3) ? . . . C(4) C(5) C(6) 121.1(4) ? . . . C(4) C(5) H(3) 119.4403 ? . . . C(4) C(9) H(7) 119.9564 ? . . . C(4) C(9) C(8) 120.1(3) ? . . . H(3) C(5) C(6) 119.4399 ? . . . C(5) C(6) C(7) 120.4(3) ? . . . C(5) C(6) H(4) 119.7761 ? . . . C(6) C(7) C(8) 119.5(4) ? . . . H(4) C(6) C(7) 119.7768 ? . . . C(6) C(7) H(5) 120.2688 ? . . . C(7) C(8) C(9) 120.4(5) ? . . . H(5) C(7) C(8) 120.2679 ? . . . C(7) C(8) H(6) 119.8061 ? . . . C(8) C(9) H(7) 119.9576 ? . . . H(6) C(8) C(9) 119.8061 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Gd(1) Gd(1) 3.861(1) ? . 4_555 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC611369 rev Er-wt1235w.cif' # CCDC611369 revised Er -wt1235w data_Er-wt1235w _database_code_depnum_ccdc_archive 'CCDC 611369' # Kin-K369#2 17-5-2006 _audit_creation_date 2006-05-18 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Er O6 ' _chemical_formula_moiety 'C27 H21 Er O6 ' _chemical_formula_weight 608.72 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.548(1) _cell_length_b 7.886(1) _cell_length_c 13.048(1) _cell_angle_alpha 90 _cell_angle_beta 94.15(1) _cell_angle_gamma 90 _cell_volume 1185.1(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6989 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598.00 _exptl_absorpt_coefficient_mu 3.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_T_max 0.651 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6989 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9746 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9746 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0\s(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0\s(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2834 _reflns_number_gt 2681 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0270 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2686 _refine_ls_number_parameters 330 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.05]' _refine_ls_shift/su_max 0.0340 _refine_diff_density_max 1.01 _refine_diff_density_min -0.62 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 30.9(28) _refine_ls_abs_structure_details 'Flack (1983). 2834 Friedel Pairs' _refine_ls_abs_structure_Flack -0.04(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Er Er -0.259 4.958 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Er(1) Er 0.03962(2) 0.5369(2) 0.475890(10) 0.02234(5) Uani 1.00 1 d . . . O(1) O 0.1768(4) 0.3648(6) 0.4166(4) 0.0366(12) Uani 1.00 1 d . . . O(2) O -0.0938(4) 0.6098(6) 0.5845(3) 0.0346(11) Uani 1.00 1 d . . . O(3) O 0.0406(4) 0.3103(6) 0.5872(3) 0.0315(11) Uani 1.00 1 d . . . O(4) O 0.0841(4) 0.6754(6) 0.3233(3) 0.0350(12) Uani 1.00 1 d . . . O(5) O 0.1693(4) 0.6773(6) 0.5782(4) 0.0351(12) Uani 1.00 1 d . . . O(6) O -0.1030(4) 0.4245(6) 0.3704(4) 0.0377(12) Uani 1.00 1 d . . . C(1) C 0.1807(5) 0.2039(8) 0.4105(5) 0.029(2) Uani 1.00 1 d . . . C(2) C 0.2952(10) 0.127(2) 0.3951(9) 0.033(2) Uani 1.00 1 d . . . C(3) C 0.3126(10) -0.037(2) 0.3921(9) 0.038(2) Uani 1.00 1 d . . . C(4) C 0.4205(6) -0.1282(9) 0.3798(5) 0.034(2) Uani 1.00 1 d . . . C(5) C 0.5279(6) -0.0498(10) 0.3840(5) 0.041(2) Uani 1.00 1 d . . . C(6) C 0.6269(6) -0.1387(11) 0.3681(6) 0.046(2) Uani 1.00 1 d . . . C(7) C 0.6229(7) -0.3094(11) 0.3480(7) 0.052(2) Uani 1.00 1 d . . . C(8) C 0.5152(8) -0.3946(12) 0.3442(8) 0.062(3) Uani 1.00 1 d . . . C(9) C 0.4163(7) -0.3045(9) 0.3601(7) 0.046(2) Uani 1.00 1 d . . . C(10) C -0.0026(5) 0.2791(8) 0.6746(5) 0.029(1) Uani 1.00 1 d . . . C(11) C 0.0534(7) 0.3546(9) 0.7697(5) 0.038(2) Uani 1.00 1 d . . . C(12) C 0.0263(6) 0.3038(9) 0.8604(5) 0.034(2) Uani 1.00 1 d . . . C(13) C 0.0842(6) 0.3493(9) 0.9605(5) 0.033(2) Uani 1.00 1 d . . . C(14) C 0.1881(7) 0.4402(11) 0.9696(5) 0.047(2) Uani 1.00 1 d . . . C(15) C 0.2411(7) 0.4745(11) 1.0659(6) 0.053(2) Uani 1.00 1 d . . . C(16) C 0.1935(7) 0.4199(11) 1.1534(6) 0.050(2) Uani 1.00 1 d . . . C(17) C 0.0902(7) 0.3283(13) 1.1444(6) 0.056(2) Uani 1.00 1 d . . . C(18) C 0.0374(7) 0.2938(11) 1.0502(5) 0.044(2) Uani 1.00 1 d . . . C(19) C 0.1684(5) 0.7985(8) 0.6417(5) 0.030(2) Uani 1.00 1 d . . . C(20) C 0.2478(5) 0.7853(8) 0.7362(5) 0.033(2) Uani 1.00 1 d . . . C(21) C 0.2377(6) 0.8852(9) 0.8164(5) 0.036(2) Uani 1.00 1 d . . . C(22) C 0.3107(6) 0.8806(9) 0.9144(5) 0.036(2) Uani 1.00 1 d . . . C(23) C 0.4177(6) 0.7971(11) 0.9237(6) 0.045(2) Uani 1.00 1 d . . . C(24) C 0.4818(9) 0.791(2) 1.0158(9) 0.057(3) Uani 1.00 1 d . . . C(25) C 0.4410(8) 0.8722(12) 1.1023(6) 0.056(2) Uani 1.00 1 d . . . C(26) C 0.3355(8) 0.9541(12) 1.0936(6) 0.059(3) Uani 1.00 1 d . . . C(27) C 0.2701(7) 0.9580(11) 1.0004(6) 0.049(2) Uani 1.00 1 d . . . H(1) H 0.3592 0.2006 0.3871 0.040 Uiso 1.00 1 c R . . H(2) H 0.2461 -0.1062 0.3988 0.045 Uiso 1.00 1 c R . . H(3) H 0.5332 0.0683 0.3983 0.049 Uiso 1.00 1 c R . . H(4) H 0.6994 -0.0813 0.3710 0.055 Uiso 1.00 1 c R . . H(5) H 0.6920 -0.3698 0.3367 0.062 Uiso 1.00 1 c R . . H(6) H 0.5111 -0.5129 0.3307 0.075 Uiso 1.00 1 c R . . H(7) H 0.3438 -0.3617 0.3579 0.055 Uiso 1.00 1 c R . . H(8) H 0.1099 0.4413 0.7647 0.046 Uiso 1.00 1 c R . . H(9) H -0.0381 0.2291 0.8616 0.041 Uiso 1.00 1 c R . . H(10) H 0.2224 0.4785 0.9097 0.056 Uiso 1.00 1 c R . . H(11) H 0.3117 0.5369 1.0715 0.064 Uiso 1.00 1 c R . . H(12) H 0.2304 0.4443 1.2192 0.060 Uiso 1.00 1 c R . . H(13) H 0.0564 0.2897 1.2044 0.067 Uiso 1.00 1 c R . . H(14) H -0.0328 0.2305 1.0454 0.053 Uiso 1.00 1 c R . . H(15) H 0.3077 0.7025 0.7390 0.040 Uiso 1.00 1 c R . . H(16) H 0.1779 0.9680 0.8105 0.043 Uiso 1.00 1 c R . . H(17) H 0.4461 0.7438 0.8652 0.054 Uiso 1.00 1 c R . . H(18) H 0.5538 0.7328 1.0214 0.069 Uiso 1.00 1 c R . . H(19) H 0.4860 0.8703 1.1662 0.067 Uiso 1.00 1 c R . . H(20) H 0.3074 1.0082 1.1520 0.071 Uiso 1.00 1 c R . . H(21) H 0.1970 1.0140 0.9952 0.058 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er(1) 0.02784(11) 0.01738(10) 0.02149(10) -0.0006(3) -0.00026(7) -0.0003(2) O(1) 0.042(3) 0.028(2) 0.041(3) 0.002(2) 0.010(2) 0.001(2) O(2) 0.037(2) 0.036(2) 0.031(2) 0.003(2) 0.004(2) 0.008(2) O(3) 0.044(2) 0.023(2) 0.027(2) 0.002(2) 0.003(2) 0.001(2) O(4) 0.045(2) 0.033(2) 0.028(2) 0.005(2) 0.006(2) 0.004(2) O(5) 0.037(2) 0.032(2) 0.035(2) 0.000(2) -0.004(2) -0.002(2) O(6) 0.042(2) 0.031(2) 0.038(2) -0.003(2) -0.008(2) -0.001(2) C(1) 0.034(3) 0.031(3) 0.023(3) -0.001(3) 0.006(2) 0.002(2) C(2) 0.032(4) 0.026(4) 0.042(5) 0.002(3) 0.011(3) 0.005(3) C(3) 0.028(4) 0.038(5) 0.046(5) -0.002(4) -0.001(4) 0.004(4) C(4) 0.040(3) 0.028(3) 0.035(3) 0.006(3) -0.001(3) -0.003(3) C(5) 0.041(4) 0.033(4) 0.048(4) 0.003(3) -0.003(3) -0.008(3) C(6) 0.035(4) 0.049(4) 0.054(4) 0.004(3) -0.002(3) -0.002(4) C(7) 0.043(4) 0.048(5) 0.064(5) 0.025(4) 0.003(4) -0.005(4) C(8) 0.065(5) 0.036(4) 0.087(7) 0.008(4) 0.010(5) -0.010(5) C(9) 0.044(4) 0.031(4) 0.064(5) -0.007(3) 0.007(3) -0.004(4) C(10) 0.039(3) 0.021(3) 0.028(3) 0.003(3) 0.004(2) -0.000(2) C(11) 0.054(4) 0.031(3) 0.030(3) -0.009(3) 0.000(3) -0.006(3) C(12) 0.042(3) 0.030(3) 0.031(3) -0.005(3) -0.000(3) -0.007(3) C(13) 0.043(3) 0.032(3) 0.024(3) 0.001(3) -0.000(2) -0.004(3) C(14) 0.059(4) 0.050(5) 0.031(3) -0.010(4) 0.003(3) -0.001(3) C(15) 0.056(4) 0.060(5) 0.042(4) -0.014(4) -0.010(3) -0.004(4) C(16) 0.055(4) 0.057(5) 0.035(4) 0.004(4) -0.007(3) -0.007(4) C(17) 0.061(5) 0.080(6) 0.028(3) 0.000(5) 0.009(3) 0.000(4) C(18) 0.049(4) 0.048(4) 0.036(4) -0.004(4) 0.004(3) 0.001(3) C(19) 0.032(3) 0.027(3) 0.030(3) -0.005(3) -0.005(2) 0.005(3) C(20) 0.035(3) 0.025(3) 0.039(3) -0.002(3) -0.007(3) 0.002(3) C(21) 0.034(3) 0.038(4) 0.033(3) 0.001(3) -0.007(3) 0.003(3) C(22) 0.044(4) 0.033(3) 0.030(3) -0.005(3) -0.007(3) 0.002(3) C(23) 0.045(4) 0.052(5) 0.037(4) 0.003(4) -0.006(3) -0.004(3) C(24) 0.041(6) 0.069(6) 0.059(8) -0.005(6) -0.017(5) 0.014(6) C(25) 0.070(5) 0.060(5) 0.035(4) -0.007(5) -0.016(4) 0.005(4) C(26) 0.084(6) 0.060(5) 0.034(4) 0.001(5) -0.003(4) -0.012(4) C(27) 0.059(5) 0.043(4) 0.043(4) 0.002(4) -0.004(3) -0.007(3) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Er(1) O(1) 2.265(5) ? . . Er(1) O(2) 2.242(5) ? . . Er(1) O(3) 2.302(4) ? . . Er(1) O(3) 2.465(4) ? . 2_556 Er(1) O(4) 2.360(5) ? . . Er(1) O(5) 2.228(4) ? . . Er(1) O(6) 2.250(5) ? . . O(1) C(1) 1.272(8) ? . . O(2) C(1) 1.254(8) ? . 2_556 O(3) Er(1) 2.465(4) ? . 2_546 O(3) C(10) 1.300(7) ? . . O(4) C(10) 1.249(8) ? . 2_556 O(5) C(19) 1.265(8) ? . . O(6) C(19) 1.252(8) ? . 2_546 C(1) O(2) 1.254(8) ? . 2_546 C(1) C(2) 1.48(1) ? . . C(2) C(3) 1.32(2) ? . . C(2) H(1) 0.95 ? . . C(3) C(4) 1.45(1) ? . . C(3) H(2) 0.95 ? . . C(4) C(5) 1.38(1) ? . . C(4) C(9) 1.41(1) ? . . C(5) C(6) 1.37(1) ? . . C(5) H(3) 0.95 ? . . C(6) C(7) 1.37(1) ? . . C(6) H(4) 0.95 ? . . C(7) C(8) 1.41(1) ? . . C(7) H(5) 0.95 ? . . C(8) C(9) 1.37(1) ? . . C(8) H(6) 0.95 ? . . C(9) H(7) 0.95 ? . . C(10) O(4) 1.249(8) ? . 2_546 C(10) C(11) 1.482(9) ? . . C(11) C(12) 1.309(9) ? . . C(11) H(8) 0.95 ? . . C(12) C(13) 1.467(9) ? . . C(12) H(9) 0.95 ? . . C(13) C(14) 1.39(1) ? . . C(13) C(18) 1.40(1) ? . . C(14) C(15) 1.38(1) ? . . C(14) H(10) 0.95 ? . . C(15) C(16) 1.37(1) ? . . C(15) H(11) 0.95 ? . . C(16) C(17) 1.39(1) ? . . C(16) H(12) 0.95 ? . . C(17) C(18) 1.36(1) ? . . C(17) H(13) 0.95 ? . . C(18) H(14) 0.95 ? . . C(19) O(6) 1.252(8) ? . 2_556 C(19) C(20) 1.486(8) ? . . C(20) C(21) 1.322(9) ? . . C(20) H(15) 0.95 ? . . C(21) C(22) 1.481(9) ? . . C(21) H(16) 0.95 ? . . C(22) C(23) 1.40(1) ? . . C(22) C(27) 1.39(1) ? . . C(23) C(24) 1.37(1) ? . . C(23) H(17) 0.95 ? . . C(24) C(25) 1.41(2) ? . . C(24) H(18) 0.95 ? . . C(25) C(26) 1.38(1) ? . . C(25) H(19) 0.95 ? . . C(26) C(27) 1.39(1) ? . . C(26) H(20) 0.95 ? . . C(27) H(21) 0.95 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Er(1) O(1) 154.1(2) ? . . . O(3) Er(1) O(1) 77.2(2) ? . . . O(3) Er(1) O(1) 131.7(2) ? 2_556 . . O(4) Er(1) O(1) 77.8(2) ? . . . O(5) Er(1) O(1) 92.6(2) ? . . . O(6) Er(1) O(1) 93.1(2) ? . . . Er(1) O(1) C(1) 130.3(4) ? . . . O(3) Er(1) O(2) 76.8(2) ? . . . O(3) Er(1) O(2) 74.2(2) ? 2_556 . . O(4) Er(1) O(2) 128.0(2) ? . . . O(5) Er(1) O(2) 87.5(2) ? . . . O(6) Er(1) O(2) 89.0(2) ? . . . Er(1) O(2) C(1) 140.7(4) ? . . 2_556 O(3) Er(1) O(3) 151.0(2) ? 2_556 . . O(4) Er(1) O(3) 154.2(2) ? . . . O(5) Er(1) O(3) 92.0(2) ? . . . O(6) Er(1) O(3) 92.9(2) ? . . . Er(1) O(3) C(10) 135.7(4) ? . . . Er(1) O(3) Er(1) 118.9(2) ? . . 2_546 O(4) Er(1) O(3) 54.0(2) ? . . 2_556 O(5) Er(1) O(3) 89.2(2) ? . . 2_556 O(6) Er(1) O(3) 84.2(2) ? . . 2_556 Er(1) O(3) C(10) 88.2(3) ? . 2_556 2_556 Er(1) O(3) Er(1) 118.9(2) ? . 2_556 2_556 O(5) Er(1) O(4) 95.6(2) ? . . . O(6) Er(1) O(4) 82.0(2) ? . . . Er(1) O(4) C(10) 94.2(4) ? . . 2_556 O(6) Er(1) O(5) 173.2(2) ? . . . Er(1) O(5) C(19) 136.9(4) ? . . . Er(1) O(6) C(19) 142.9(4) ? . . 2_546 O(1) C(1) O(2) 123.7(6) ? . . 2_546 O(1) C(1) C(2) 116.8(7) ? . . . O(2) C(1) O(1) 123.7(6) ? . 2_556 2_556 O(2) C(1) C(2) 119.4(7) ? . 2_556 2_556 O(3) Er(1) O(2) 74.2(2) ? . 2_546 2_546 C(10) O(3) Er(1) 88.2(3) ? . . 2_546 O(3) Er(1) O(4) 54.0(2) ? . 2_546 2_546 O(3) Er(1) O(5) 89.2(2) ? . 2_546 2_546 O(3) Er(1) O(6) 84.2(2) ? . 2_546 2_546 O(3) Er(1) O(3) 151.0(2) ? . 2_546 2_546 O(3) C(10) C(11) 119.1(6) ? . . . O(3) C(10) O(4) 118.7(5) ? . . 2_546 O(4) C(10) O(3) 118.7(5) ? . 2_556 2_556 O(4) C(10) C(11) 121.9(6) ? . 2_556 2_556 O(5) C(19) O(6) 123.5(5) ? . . 2_556 O(5) C(19) C(20) 117.2(6) ? . . . O(6) C(19) O(5) 123.5(5) ? . 2_546 2_546 O(6) C(19) C(20) 119.4(6) ? . 2_546 2_546 C(2) C(1) O(2) 119.4(7) ? . . 2_546 C(1) O(2) Er(1) 140.7(4) ? . 2_546 2_546 C(1) C(2) C(3) 123(1) ? . . . C(1) C(2) H(1) 118.4 ? . . . H(1) C(2) C(3) 118.4 ? . . . C(2) C(3) H(2) 115.7 ? . . . C(2) C(3) C(4) 128(1) ? . . . H(2) C(3) C(4) 115.7 ? . . . C(3) C(4) C(5) 123.2(8) ? . . . C(3) C(4) C(9) 119.1(7) ? . . . C(4) C(5) H(3) 119.3 ? . . . C(9) C(4) C(5) 117.7(7) ? . . . C(4) C(5) C(6) 121.4(7) ? . . . C(4) C(9) H(7) 119.4 ? . . . C(4) C(9) C(8) 121.2(7) ? . . . H(3) C(5) C(6) 119.3 ? . . . C(5) C(6) C(7) 120.9(7) ? . . . C(5) C(6) H(4) 119.5 ? . . . C(6) C(7) C(8) 119.5(8) ? . . . H(4) C(6) C(7) 119.5 ? . . . C(6) C(7) H(5) 120.4 ? . . . C(7) C(8) C(9) 119.2(8) ? . . . C(7) C(8) H(6) 120.4 ? . . . H(5) C(7) C(8) 120.3 ? . . . C(8) C(9) H(7) 119.4 ? . . . H(6) C(8) C(9) 120.4 ? . . . C(11) C(10) O(4) 121.9(6) ? . . 2_546 C(10) O(4) Er(1) 94.2(4) ? . 2_546 2_546 C(10) C(11) H(8) 119.5 ? . . . C(10) C(11) C(12) 121.0(6) ? . . . H(8) C(11) C(12) 119.4 ? . . . C(11) C(12) H(9) 116.3 ? . . . C(11) C(12) C(13) 127.3(6) ? . . . H(9) C(12) C(13) 116.3 ? . . . C(12) C(13) C(14) 122.3(6) ? . . . C(12) C(13) C(18) 119.4(6) ? . . . C(13) C(14) H(10) 120.0 ? . . . C(18) C(13) C(14) 118.2(6) ? . . . C(13) C(14) C(15) 119.9(7) ? . . . C(13) C(18) H(14) 119.3 ? . . . C(13) C(18) C(17) 121.3(7) ? . . . H(10) C(14) C(15) 120.0 ? . . . C(14) C(15) C(16) 121.1(8) ? . . . C(14) C(15) H(11) 119.4 ? . . . C(15) C(16) C(17) 119.0(7) ? . . . H(11) C(15) C(16) 119.4 ? . . . C(15) C(16) H(12) 120.4 ? . . . C(16) C(17) C(18) 120.4(7) ? . . . C(16) C(17) H(13) 119.4 ? . . . H(12) C(16) C(17) 120.5 ? . . . C(17) C(18) H(14) 119.3 ? . . . H(13) C(17) C(18) 119.4 ? . . . C(19) O(6) Er(1) 142.9(4) ? . 2_556 2_556 C(20) C(19) O(6) 119.4(6) ? . . 2_556 C(19) C(20) C(21) 122.0(6) ? . . . C(19) C(20) H(15) 119.0 ? . . . H(15) C(20) C(21) 119.0 ? . . . C(20) C(21) H(16) 116.9 ? . . . C(20) C(21) C(22) 126.3(6) ? . . . H(16) C(21) C(22) 116.9 ? . . . C(21) C(22) C(23) 122.1(6) ? . . . C(21) C(22) C(27) 118.8(6) ? . . . C(22) C(23) H(17) 119.6 ? . . . C(27) C(22) C(23) 119.1(6) ? . . . C(22) C(23) C(24) 120.7(8) ? . . . C(22) C(27) H(21) 119.8 ? . . . C(22) C(27) C(26) 120.3(8) ? . . . H(17) C(23) C(24) 119.6 ? . . . C(23) C(24) C(25) 119(1) ? . . . C(23) C(24) H(18) 120.0 ? . . . C(24) C(25) C(26) 119.5(8) ? . . . H(18) C(24) C(25) 120.0 ? . . . C(24) C(25) H(19) 120.2 ? . . . C(25) C(26) C(27) 120.4(8) ? . . . C(25) C(26) H(20) 119.8 ? . . . H(19) C(25) C(26) 120.2 ? . . . C(26) C(27) H(21) 119.8 ? . . . H(20) C(26) C(27) 119.8 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Er(1) O(2) 3.525(5) ? . 2_546 Er(1) C(1) 3.237(6) ? . . Er(1) C(1) 3.309(6) ? . 2_556 Er(1) C(10) 3.358(6) ? . . Er(1) C(10) 2.750(6) ? . 2_556 Er(1) C(19) 3.268(6) ? . . Er(1) C(19) 3.335(6) ? . 2_546 O(1) O(2) 2.227(7) ? . 2_546 O(1) O(3) 2.850(7) ? . . O(1) O(4) 2.905(7) ? . . O(1) O(5) 3.249(7) ? . . O(1) O(6) 3.278(7) ? . . O(1) C(2) 2.35(1) ? . . O(1) C(3) 3.56(1) ? . . O(1) C(6) 3.480(9) ? . 2_656 O(1) C(16) 3.480(9) ? . 1_554 O(1) H(1) 2.52 ? . . O(1) H(4) 3.06 ? . 2_656 O(1) H(7) 3.03 ? . 1_565 O(1) H(12) 2.76 ? . 1_554 O(1) H(13) 3.06 ? . 1_554 O(2) Er(1) 3.525(5) ? . 2_556 O(2) O(1) 2.227(7) ? . 2_556 O(2) O(3) 2.825(6) ? . . O(2) O(3) 2.846(6) ? . 2_556 O(2) O(5) 3.091(6) ? . . O(2) O(6) 3.148(7) ? . . O(2) O(6) 3.387(7) ? . 2_556 O(2) C(2) 2.36(1) ? . 2_556 O(2) C(3) 2.82(1) ? . 2_556 O(2) C(10) 3.019(8) ? . . O(2) C(11) 3.490(8) ? . . O(2) C(19) 3.407(7) ? . . O(2) H(1) 3.20 ? . 2_556 O(2) H(2) 2.47 ? . 2_556 O(2) H(8) 3.47 ? . . O(3) O(2) 2.846(6) ? . 2_546 O(3) O(4) 2.194(6) ? . 2_546 O(3) O(5) 3.259(6) ? . . O(3) O(5) 3.298(6) ? . 2_546 O(3) O(6) 3.300(6) ? . . O(3) O(6) 3.166(7) ? . 2_546 O(3) C(1) 3.029(8) ? . . O(3) C(11) 2.400(8) ? . . O(3) C(12) 3.581(7) ? . . O(3) H(2) 3.39 ? . 2_556 O(3) H(4) 3.13 ? . 2_656 O(3) H(5) 3.48 ? . 2_656 O(3) H(8) 2.61 ? . . O(4) O(3) 2.194(6) ? . 2_556 O(4) O(5) 3.399(6) ? . . O(4) O(6) 3.025(7) ? . . O(4) C(3) 3.54(1) ? . 1_565 O(4) C(11) 2.391(8) ? . 2_556 O(4) C(12) 2.821(8) ? . 2_556 O(4) C(16) 3.312(9) ? . 1_554 O(4) H(2) 2.68 ? . 1_565 O(4) H(7) 3.01 ? . 1_565 O(4) H(8) 3.22 ? . 2_556 O(4) H(9) 2.47 ? . 2_556 O(4) H(12) 2.89 ? . 1_554 O(4) H(13) 3.42 ? . 1_554 O(5) O(3) 3.298(6) ? . 2_556 O(5) O(6) 2.217(7) ? . 2_556 O(5) C(6) 3.464(9) ? . 2_656 O(5) C(20) 2.351(8) ? . . O(5) C(21) 3.551(8) ? . . O(5) H(2) 3.083 ? . 1_565 O(5) H(3) 3.53 ? . 2_656 O(5) H(4) 2.60 ? . 2_656 O(5) H(8) 3.18 ? . . O(5) H(15) 2.55 ? . . O(6) O(2) 3.387(7) ? . 2_546 O(6) O(3) 3.166(7) ? . 2_556 O(6) O(5) 2.217(7) ? . 2_546 O(6) C(10) 3.122(8) ? . 2_556 O(6) C(20) 2.366(8) ? . 2_546 O(6) C(21) 2.812(8) ? . 2_546 O(6) H(2) 3.55 ? . 2_556 O(6) H(5) 2.88 ? . 1_465 O(6) H(13) 3.13 ? . 1_554 O(6) H(15) 3.19 ? . 2_546 O(6) H(16) 2.48 ? . 2_546 C(1) Er(1) 3.309(6) ? . 2_546 C(1) C(3) 2.46(1) ? . . C(1) H(1) 2.11 ? . . C(1) H(2) 2.57 ? . . C(1) H(4) 3.51 ? . 2_656 C(1) H(5) 3.56 ? . 2_656 C(1) H(12) 3.22 ? . 1_554 C(1) H(13) 3.03 ? . 1_554 C(2) O(2) 2.36(1) ? . 2_546 C(2) C(4) 2.50(1) ? . . C(2) C(5) 3.04(1) ? . . C(2) C(7) 3.45(1) ? . 2_656 C(2) H(2) 1.93 ? . . C(2) H(3) 2.78 ? . . C(2) H(5) 3.49 ? . 2_656 C(2) H(12) 3.44 ? . 1_554 C(2) H(20) 3.32 ? . 1_544 C(3) O(2) 2.82(1) ? . 2_546 C(3) O(4) 3.54(1) ? . 1_545 C(3) C(5) 2.50(1) ? . . C(3) C(9) 2.47(1) ? . . C(3) H(1) 1.95 ? . . C(3) H(3) 2.67 ? . . C(3) H(7) 2.63 ? . . C(3) H(20) 3.15 ? . 1_544 C(4) C(6) 2.40(1) ? . . C(4) C(7) 2.80(1) ? . . C(4) C(8) 2.43(1) ? . . C(4) H(1) 2.69 ? . . C(4) H(2) 2.05 ? . . C(4) H(3) 2.03 ? . . C(4) H(4) 3.25 ? . . C(4) H(6) 3.29 ? . . C(4) H(7) 2.05 ? . . C(4) H(19) 2.94 ? . 1_544 C(4) H(20) 3.34 ? . 1_544 C(5) C(7) 2.39(1) ? . . C(5) C(8) 2.77(1) ? . . C(5) C(9) 2.40(1) ? . . C(5) H(1) 2.78 ? . . C(5) H(2) 3.30 ? . . C(5) H(4) 2.02 ? . . C(5) H(5) 3.24 ? . . C(5) H(7) 3.25 ? . . C(5) H(15) 3.25 ? . 2_646 C(5) H(19) 2.92 ? . 1_544 C(6) O(1) 3.480(9) ? . 2_646 C(6) O(5) 3.464(9) ? . 2_646 C(6) C(8) 2.40(1) ? . . C(6) C(9) 2.76(1) ? . . C(6) H(1) 3.436 ? . 2_646 C(6) H(3) 2.01 ? . . C(6) H(5) 2.02 ? . . C(6) H(6) 3.26 ? . . C(6) H(15) 3.15 ? . 2_646 C(6) H(19) 3.00 ? . 1_544 C(7) C(2) 3.45(1) ? . 2_646 C(7) C(9) 2.40(1) ? . . C(7) H(1) 3.45 ? . 2_646 C(7) H(3) 3.24 ? . . C(7) H(4) 2.02 ? . . C(7) H(6) 2.06 ? . . C(7) H(7) 3.26 ? . . C(7) H(19) 3.10 ? . 1_544 C(8) H(3) 3.46 ? . 2_646 C(8) H(4) 3.26 ? . . C(8) H(5) 2.06 ? . . C(8) H(7) 2.02 ? . . C(8) H(19) 3.12 ? . 1_544 C(9) H(2) 2.59 ? . . C(9) H(3) 3.26 ? . . C(9) H(3) 3.32 ? . 2_646 C(9) H(5) 3.26 ? . . C(9) H(6) 2.03 ? . . C(9) H(12) 3.37 ? . 1_544 C(9) H(19) 3.04 ? . 1_544 C(10) Er(1) 2.750(6) ? . 2_546 C(10) O(6) 3.122(8) ? . 2_546 C(10) C(12) 2.431(8) ? . . C(10) H(2) 3.04 ? . 2_556 C(10) H(8) 2.12 ? . . C(10) H(9) 2.53 ? . . C(11) O(4) 2.391(8) ? . 2_546 C(11) C(13) 2.490(9) ? . . C(11) C(14) 3.01(1) ? . . C(11) H(4) 3.54 ? . 2_656 C(11) H(9) 1.93 ? . . C(11) H(10) 2.75 ? . . C(11) H(16) 3.40 ? . 1_545 C(12) O(4) 2.821(8) ? . 2_546 C(12) C(14) 2.51(1) ? . . C(12) C(18) 2.472(9) ? . . C(12) H(8) 1.96 ? . . C(12) H(10) 2.69 ? . . C(12) H(14) 2.62 ? . . C(12) H(16) 3.27 ? . 1_545 C(12) H(21) 3.42 ? . 1_545 C(13) C(15) 2.41(1) ? . . C(13) C(16) 2.789(9) ? . . C(13) C(17) 2.401(9) ? . . C(13) H(8) 2.69 ? . . C(13) H(9) 2.07 ? . . C(13) H(10) 2.04 ? . . C(13) H(11) 3.26 ? . . C(13) H(13) 3.26 ? . . C(13) H(14) 2.04 ? . . C(13) H(21) 2.97 ? . 1_545 C(14) C(16) 2.40(1) ? . . C(14) C(17) 2.76(1) ? . . C(14) C(18) 2.39(1) ? . . C(14) H(8) 2.76 ? . . C(14) H(9) 3.32 ? . . C(14) H(11) 2.03 ? . . C(14) H(12) 3.26 ? . . C(14) H(14) 3.25 ? . . C(14) H(21) 3.38 ? . 1_545 C(15) C(17) 2.38(1) ? . . C(15) C(18) 2.75(1) ? . . C(15) H(10) 2.03 ? . . C(15) H(12) 2.03 ? . . C(15) H(13) 3.24 ? . . C(16) O(1) 3.480(9) ? . 1_556 C(16) O(4) 3.312(9) ? . 1_556 C(16) C(18) 2.39(1) ? . . C(16) H(7) 3.53 ? . 1_566 C(16) H(10) 3.25 ? . . C(16) H(11) 2.02 ? . . C(16) H(13) 2.04 ? . . C(16) H(14) 3.24 ? . . C(16) H(20) 3.50 ? . 1_545 C(17) H(11) 3.24 ? . . C(17) H(12) 2.04 ? . . C(17) H(14) 2.00 ? . . C(17) H(20) 3.55 ? . 1_545 C(17) H(21) 3.44 ? . 1_545 C(18) H(9) 2.60 ? . . C(18) H(10) 3.26 ? . . C(18) H(12) 3.24 ? . . C(18) H(13) 2.01 ? . . C(18) H(21) 3.00 ? . 1_545 C(19) Er(1) 3.335(6) ? . 2_556 C(19) C(21) 2.458(9) ? . . C(19) H(2) 3.44 ? . 1_565 C(19) H(4) 3.37 ? . 2_656 C(19) H(5) 3.08 ? . 2_666 C(19) H(8) 3.34 ? . . C(19) H(15) 2.12 ? . . C(19) H(16) 2.57 ? . . C(20) O(6) 2.366(8) ? . 2_556 C(20) C(22) 2.501(9) ? . . C(20) C(23) 3.024(9) ? . . C(20) H(4) 3.29 ? . 2_656 C(20) H(5) 2.98 ? . 2_666 C(20) H(6) 3.38 ? . 2_666 C(20) H(8) 3.18 ? . . C(20) H(10) 3.34 ? . . C(20) H(16) 1.95 ? . . C(20) H(17) 2.76 ? . . C(21) O(6) 2.812(8) ? . 2_556 C(21) C(23) 2.52(1) ? . . C(21) C(27) 2.47(1) ? . . C(21) H(5) 2.94 ? . 2_666 C(21) H(10) 3.44 ? . . C(21) H(15) 1.97 ? . . C(21) H(17) 2.69 ? . . C(21) H(21) 2.62 ? . . C(22) C(24) 2.40(1) ? . . C(22) C(25) 2.78(1) ? . . C(22) C(26) 2.41(1) ? . . C(22) H(10) 3.33 ? . . C(22) H(11) 3.40 ? . . C(22) H(15) 2.68 ? . . C(22) H(16) 2.09 ? . . C(22) H(17) 2.04 ? . . C(22) H(18) 3.26 ? . . C(22) H(20) 3.26 ? . . C(22) H(21) 2.04 ? . . C(23) C(25) 2.40(1) ? . . C(23) C(26) 2.77(1) ? . . C(23) C(27) 2.40(1) ? . . C(23) H(10) 3.37 ? . . C(23) H(11) 3.13 ? . . C(23) H(15) 2.74 ? . . C(23) H(16) 3.33 ? . . C(23) H(18) 2.02 ? . . C(23) H(19) 3.26 ? . . C(23) H(21) 3.26 ? . . C(24) C(26) 2.40(2) ? . . C(24) C(27) 2.77(1) ? . . C(24) H(11) 2.94 ? . . C(24) H(17) 2.01 ? . . C(24) H(19) 2.06 ? . . C(24) H(20) 3.26 ? . . C(25) C(27) 2.40(1) ? . . C(25) H(11) 3.05 ? . . C(25) H(17) 3.26 ? . . C(25) H(18) 2.05 ? . . C(25) H(20) 2.02 ? . . C(25) H(21) 3.25 ? . . C(26) H(11) 3.31 ? . . C(26) H(18) 3.26 ? . . C(26) H(19) 2.03 ? . . C(26) H(21) 2.03 ? . . C(27) H(11) 3.47 ? . . C(27) H(16) 2.63 ? . . C(27) H(17) 3.26 ? . . C(27) H(19) 3.25 ? . . C(27) H(20) 2.03 ? . . H(1) O(2) 3.20 ? . 2_546 H(1) C(6) 3.43 ? . 2_656 H(1) C(7) 3.45 ? . 2_656 H(2) O(2) 2.47 ? . 2_546 H(2) O(3) 3.39 ? . 2_546 H(2) O(4) 2.68 ? . 1_545 H(2) O(5) 3.08 ? . 1_545 H(2) O(6) 3.55 ? . 2_546 H(2) C(10) 3.04 ? . 2_546 H(2) C(19) 3.44 ? . 1_545 H(3) O(5) 3.53 ? . 2_646 H(3) C(8) 3.46 ? . 2_656 H(3) C(9) 3.32 ? . 2_656 H(4) O(1) 3.06 ? . 2_646 H(4) O(3) 3.13 ? . 2_646 H(4) O(5) 2.60 ? . 2_646 H(4) C(1) 3.51 ? . 2_646 H(4) C(11) 3.54 ? . 2_646 H(4) C(19) 3.37 ? . 2_646 H(4) C(20) 3.29 ? . 2_646 H(5) O(3) 3.48 ? . 2_646 H(5) O(6) 2.88 ? . 1_645 H(5) C(1) 3.56 ? . 2_646 H(5) C(2) 3.49 ? . 2_646 H(5) C(19) 3.08 ? . 2_636 H(5) C(20) 2.98 ? . 2_636 H(5) C(21) 2.94 ? . 2_636 H(6) C(20) 3.38 ? . 2_636 H(7) O(1) 3.03 ? . 1_545 H(7) O(4) 3.01 ? . 1_545 H(7) C(16) 3.53 ? . 1_544 H(8) O(4) 3.22 ? . 2_546 H(9) O(4) 2.47 ? . 2_546 H(12) O(1) 2.76 ? . 1_556 H(12) O(4) 2.89 ? . 1_556 H(12) C(1) 3.22 ? . 1_556 H(12) C(2) 3.44 ? . 1_556 H(12) C(9) 3.37 ? . 1_566 H(13) O(1) 3.06 ? . 1_556 H(13) O(4) 3.42 ? . 1_556 H(13) O(6) 3.13 ? . 1_556 H(13) C(1) 3.03 ? . 1_556 H(15) O(6) 3.19 ? . 2_556 H(15) C(5) 3.25 ? . 2_656 H(15) C(6) 3.15 ? . 2_656 H(16) O(6) 2.48 ? . 2_556 H(16) C(11) 3.40 ? . 1_565 H(16) C(12) 3.27 ? . 1_565 H(19) C(4) 2.94 ? . 1_566 H(19) C(5) 2.92 ? . 1_566 H(19) C(6) 3.00 ? . 1_566 H(19) C(7) 3.10 ? . 1_566 H(19) C(8) 3.12 ? . 1_566 H(19) C(9) 3.04 ? . 1_566 H(20) C(2) 3.32 ? . 1_566 H(20) C(3) 3.15 ? . 1_566 H(20) C(4) 3.34 ? . 1_566 H(20) C(16) 3.50 ? . 1_565 H(20) C(17) 3.55 ? . 1_565 H(21) C(12) 3.42 ? . 1_565 H(21) C(13) 2.97 ? . 1_565 H(21) C(14) 3.38 ? . 1_565 H(21) C(17) 3.44 ? . 1_565 H(21) C(18) 3.00 ? . 1_565 Er(1) Er(1) 4.107(2) ? . 2_546 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_Ho-wt1266w _database_code_depnum_ccdc_archive 'CCDC 631228' #-Kin-K368 - Ho cinnamate #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Ho O6 ' _chemical_formula_moiety 'C27 H21 Ho O6 ' _chemical_formula_weight 606.39 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.544(1) _cell_length_b 7.9169(9) _cell_length_c 13.071(2) _cell_angle_alpha 90 _cell_angle_beta 94.136(2) _cell_angle_gamma 90 _cell_volume 1191.5(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7328 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596.00 _exptl_absorpt_coefficient_mu 3.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.509 _exptl_absorpt_correction_T_max 0.646 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7328 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9748 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9748 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0\s(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0\s(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2853 _reflns_number_gt 2708 _reflns_threshold_expression I>2.0\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0260 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2710 _refine_ls_number_parameters 330 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.0115]' _refine_ls_shift/su_max 0.0280 _refine_diff_density_max 0.73 _refine_diff_density_min -0.52 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 25.2(28) _refine_ls_abs_structure_details 'Flack (1983). 2853 Friedel-pairs' _refine_ls_abs_structure_Flack -0.027(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ho Ho -0.218 4.678 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ho(1) Ho 0.46010(2) 0.4926(2) 0.524000(10) 0.02617(5) Uani 1.00 1 d . . . O(1) O 0.5956(3) 0.4208(6) 0.4168(3) 0.0423(11) Uani 1.00 1 d . . . O(2) O 0.3223(4) 0.6652(6) 0.5828(3) 0.0393(11) Uani 1.00 1 d . . . O(3) O 0.5403(3) 0.2198(5) 0.5884(3) 0.0354(10) Uani 1.00 1 d . . . O(4) O 0.4162(4) 0.3532(6) 0.6766(3) 0.0408(11) Uani 1.00 1 d . . . O(5) O 0.3292(4) 0.3506(6) 0.4211(3) 0.0419(11) Uani 1.00 1 d . . . O(6) O 0.6031(4) 0.6049(6) 0.6293(3) 0.0449(12) Uani 1.00 1 d . . . C(1) C 0.3171(5) 0.8249(8) 0.5898(4) 0.034(1) Uani 1.00 1 d . . . C(2) C 0.2037(8) 0.899(1) 0.6046(8) 0.041(2) Uani 1.00 1 d . . . C(3) C 0.1887(9) 1.065(1) 0.6084(7) 0.042(2) Uani 1.00 1 d . . . C(4) C 0.0805(5) 1.1588(8) 0.6209(5) 0.040(2) Uani 1.00 1 d . . . C(5) C -0.0287(6) 1.0783(9) 0.6166(5) 0.048(2) Uani 1.00 1 d . . . C(6) C -0.1279(6) 1.1689(10) 0.6328(6) 0.053(2) Uani 1.00 1 d . . . C(7) C -0.1224(7) 1.3390(11) 0.6531(6) 0.062(2) Uani 1.00 1 d . . . C(8) C -0.0161(7) 1.4197(11) 0.6561(7) 0.067(2) Uani 1.00 1 d . . . C(9) C 0.0843(7) 1.3316(10) 0.6397(6) 0.058(2) Uani 1.00 1 d . . . C(10) C 0.4966(5) 0.2512(7) 0.6752(4) 0.0320(13) Uani 1.00 1 d . . . C(11) C 0.5534(6) 0.1734(8) 0.7693(4) 0.041(2) Uani 1.00 1 d . . . C(12) C 0.5273(5) 0.2251(8) 0.8608(4) 0.040(2) Uani 1.00 1 d . . . C(13) C 0.5845(5) 0.1802(8) 0.9603(4) 0.038(2) Uani 1.00 1 d . . . C(14) C 0.5374(6) 0.2351(10) 1.0499(5) 0.048(2) Uani 1.00 1 d . . . C(15) C 0.5908(7) 0.1974(11) 1.1447(5) 0.060(2) Uani 1.00 1 d . . . C(16) C 0.6931(7) 0.1078(10) 1.1533(5) 0.057(2) Uani 1.00 1 d . . . C(17) C 0.7417(7) 0.0518(10) 1.0661(5) 0.060(2) Uani 1.00 1 d . . . C(18) C 0.6877(6) 0.0881(10) 0.9701(5) 0.051(2) Uani 1.00 1 d . . . C(19) C 0.3318(5) 0.2315(8) 0.3579(4) 0.033(1) Uani 1.00 1 d . . . C(20) C 0.2517(5) 0.2436(8) 0.2632(4) 0.039(2) Uani 1.00 1 d . . . C(21) C 0.2618(5) 0.1445(8) 0.1834(4) 0.039(2) Uani 1.00 1 d . . . C(22) C 0.1903(5) 0.1486(9) 0.0852(4) 0.041(2) Uani 1.00 1 d . . . C(23) C 0.0818(6) 0.2292(10) 0.0762(5) 0.048(2) Uani 1.00 1 d . . . C(24) C 0.0172(9) 0.233(2) -0.0180(7) 0.062(3) Uani 1.00 1 d . . . C(25) C 0.0596(7) 0.1548(12) -0.1024(6) 0.067(2) Uani 1.00 1 d . . . C(26) C 0.1636(8) 0.0756(12) -0.0936(6) 0.069(3) Uani 1.00 1 d . . . C(27) C 0.2294(7) 0.0707(10) -0.0001(5) 0.055(2) Uani 1.00 1 d . . . H(1) H 0.1391 0.8272 0.6117 0.050 Uiso 1.00 1 c R . . H(2) H 0.2563 1.1313 0.6024 0.050 Uiso 1.00 1 c R . . H(3) H -0.0340 0.9607 0.6023 0.058 Uiso 1.00 1 c R . . H(4) H -0.2008 1.1129 0.6299 0.064 Uiso 1.00 1 c R . . H(5) H -0.1909 1.4004 0.6650 0.074 Uiso 1.00 1 c R . . H(6) H -0.0119 1.5375 0.6697 0.080 Uiso 1.00 1 c R . . H(7) H 0.1565 1.3896 0.6412 0.069 Uiso 1.00 1 c R . . H(8) H 0.6088 0.0858 0.7636 0.049 Uiso 1.00 1 c R . . H(9) H 0.4636 0.3009 0.8621 0.048 Uiso 1.00 1 c R . . H(10) H 0.4677 0.2993 1.0455 0.058 Uiso 1.00 1 c R . . H(11) H 0.5566 0.2337 1.2049 0.073 Uiso 1.00 1 c R . . H(12) H 0.7302 0.0846 1.2190 0.068 Uiso 1.00 1 c R . . H(13) H 0.8119 -0.0114 1.0716 0.072 Uiso 1.00 1 c R . . H(14) H 0.7216 0.0495 0.9102 0.061 Uiso 1.00 1 c R . . H(15) H 0.1914 0.3255 0.2605 0.047 Uiso 1.00 1 c R . . H(16) H 0.3215 0.0617 0.1897 0.047 Uiso 1.00 1 c R . . H(17) H 0.0522 0.2810 0.1345 0.058 Uiso 1.00 1 c R . . H(18) H -0.0555 0.2900 -0.0243 0.075 Uiso 1.00 1 c R . . H(19) H 0.0154 0.1566 -0.1666 0.080 Uiso 1.00 1 c R . . H(20) H 0.1922 0.0227 -0.1520 0.082 Uiso 1.00 1 c R . . H(21) H 0.3018 0.0132 0.0050 0.066 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ho(1) 0.03170(11) 0.02160(10) 0.02480(10) -0.0009(2) -0.00070(6) -0.0006(2) O(1) 0.038(2) 0.050(2) 0.039(2) 0.010(2) 0.006(2) 0.009(2) O(2) 0.043(2) 0.033(2) 0.044(2) 0.004(2) 0.010(2) 0.005(2) O(3) 0.047(2) 0.029(2) 0.031(2) -0.002(2) 0.002(2) 0.000(2) O(4) 0.047(2) 0.040(2) 0.036(2) 0.006(2) 0.004(2) 0.005(2) O(5) 0.044(2) 0.038(2) 0.043(2) -0.005(2) -0.007(2) -0.004(2) O(6) 0.048(2) 0.039(2) 0.045(2) -0.007(2) -0.012(2) 0.002(2) C(1) 0.040(3) 0.037(3) 0.027(3) 0.004(3) 0.006(2) 0.003(2) C(2) 0.036(4) 0.033(5) 0.056(6) -0.004(4) 0.012(4) -0.006(4) C(3) 0.037(4) 0.046(5) 0.043(5) -0.005(4) 0.005(3) -0.004(4) C(4) 0.042(3) 0.038(3) 0.041(3) 0.006(3) 0.002(3) -0.004(3) C(5) 0.047(4) 0.043(4) 0.053(4) 0.004(3) 0.002(3) -0.009(3) C(6) 0.043(4) 0.054(4) 0.062(4) 0.005(3) -0.002(3) -0.004(4) C(7) 0.053(4) 0.064(5) 0.068(5) 0.020(4) 0.001(4) -0.006(4) C(8) 0.077(5) 0.040(4) 0.082(6) 0.014(4) 0.001(4) -0.006(4) C(9) 0.057(4) 0.043(4) 0.074(5) 0.001(3) 0.008(4) -0.008(4) C(10) 0.049(3) 0.021(2) 0.025(2) -0.004(2) 0.000(2) 0.005(2) C(11) 0.058(4) 0.034(3) 0.030(3) 0.002(3) -0.001(3) 0.002(3) C(12) 0.050(3) 0.036(3) 0.034(3) 0.004(3) 0.001(2) 0.005(3) C(13) 0.049(3) 0.036(3) 0.029(3) -0.001(3) 0.002(2) 0.003(2) C(14) 0.056(4) 0.054(4) 0.035(3) 0.006(4) 0.005(3) -0.001(3) C(15) 0.073(5) 0.081(6) 0.029(3) -0.001(5) 0.009(3) -0.001(4) C(16) 0.067(4) 0.066(5) 0.036(3) -0.003(4) -0.009(3) 0.009(3) C(17) 0.063(4) 0.065(5) 0.052(4) 0.016(4) -0.005(3) 0.006(4) C(18) 0.061(4) 0.054(4) 0.038(3) 0.007(4) 0.005(3) 0.001(3) C(19) 0.034(3) 0.033(3) 0.034(3) -0.004(2) -0.001(2) -0.001(2) C(20) 0.041(3) 0.035(3) 0.039(3) 0.003(3) -0.011(2) -0.001(3) C(21) 0.040(3) 0.039(3) 0.039(3) -0.000(3) -0.003(2) 0.004(3) C(22) 0.047(3) 0.041(3) 0.035(3) -0.004(3) -0.007(3) 0.002(3) C(23) 0.050(3) 0.055(4) 0.038(3) 0.003(3) -0.007(3) -0.003(3) C(24) 0.056(6) 0.071(5) 0.056(7) 0.002(5) -0.019(4) 0.006(5) C(25) 0.080(5) 0.076(6) 0.041(4) -0.017(5) -0.018(4) 0.004(4) C(26) 0.092(6) 0.074(6) 0.038(4) 0.005(5) -0.002(4) -0.007(4) C(27) 0.063(4) 0.055(4) 0.044(4) 0.009(4) -0.001(3) -0.008(3) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ho(1) O(1) 2.247(4) ? . . Ho(1) O(2) 2.273(4) ? . . Ho(1) O(3) 2.474(4) ? . . Ho(1) O(3) 2.322(4) ? . 2_656 Ho(1) O(4) 2.366(4) ? . . Ho(1) O(5) 2.251(4) ? . . Ho(1) O(6) 2.254(4) ? . . O(1) C(1) 1.270(7) ? . 2_646 O(2) C(1) 1.269(7) ? . . O(3) Ho(1) 2.322(4) ? . 2_646 O(3) C(10) 1.298(6) ? . . O(4) C(10) 1.232(7) ? . . O(5) C(19) 1.255(7) ? . . O(6) C(19) 1.257(7) ? . 2_656 C(1) O(1) 1.270(7) ? . 2_656 C(1) C(2) 1.46(1) ? . . C(2) C(3) 1.32(2) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.47(1) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.410(9) ? . . C(4) C(9) 1.39(1) ? . . C(5) C(6) 1.38(1) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.37(1) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.38(1) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.38(1) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . C(10) C(11) 1.485(8) ? . . C(11) C(12) 1.320(8) ? . . C(11) H(8) 0.9500 ? . . C(12) C(13) 1.459(8) ? . . C(12) H(9) 0.9500 ? . . C(13) C(14) 1.397(9) ? . . C(13) C(18) 1.395(9) ? . . C(14) C(15) 1.376(9) ? . . C(14) H(10) 0.9500 ? . . C(15) C(16) 1.38(1) ? . . C(15) H(11) 0.9500 ? . . C(16) C(17) 1.38(1) ? . . C(16) H(12) 0.9500 ? . . C(17) C(18) 1.39(1) ? . . C(17) H(13) 0.9500 ? . . C(18) H(14) 0.9500 ? . . C(19) O(6) 1.257(7) ? . 2_646 C(19) C(20) 1.494(7) ? . . C(20) C(21) 1.317(9) ? . . C(20) H(15) 0.9500 ? . . C(21) C(22) 1.475(8) ? . . C(21) H(16) 0.9500 ? . . C(22) C(23) 1.404(9) ? . . C(22) C(27) 1.38(1) ? . . C(23) C(24) 1.39(1) ? . . C(23) H(17) 0.9500 ? . . C(24) C(25) 1.39(1) ? . . C(24) H(18) 0.9500 ? . . C(25) C(26) 1.35(1) ? . . C(25) H(19) 0.9500 ? . . C(26) C(27) 1.39(1) ? . . C(26) H(20) 0.9500 ? . . C(27) C(22) 1.38(1) ? . . C(27) C(26) 1.39(1) ? . . C(27) H(21) 0.9500 ? . . H(5) C(7) 0.9500 ? . . H(7) C(9) 0.9500 ? . . H(16) C(21) 0.9500 ? . . H(19) C(25) 0.9500 ? . . H(21) C(27) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Ho(1) O(1) 154.0(2) ? . . . O(3) Ho(1) O(1) 74.4(1) ? . . . O(3) Ho(1) O(1) 76.8(1) ? 2_656 . . O(4) Ho(1) O(1) 127.5(2) ? . . . O(5) Ho(1) O(1) 88.2(2) ? . . . O(6) Ho(1) O(1) 88.2(2) ? . . . Ho(1) O(1) C(1) 141.7(4) ? . . 2_646 O(3) Ho(1) O(2) 131.6(1) ? . . . O(3) Ho(1) O(2) 77.2(1) ? 2_656 . . O(4) Ho(1) O(2) 78.3(2) ? . . . O(5) Ho(1) O(2) 92.7(2) ? . . . O(6) Ho(1) O(2) 93.2(2) ? . . . Ho(1) O(2) C(1) 131.4(4) ? . . . O(3) Ho(1) O(3) 151.1(1) ? 2_656 . . O(4) Ho(1) O(3) 53.4(1) ? . . . O(5) Ho(1) O(3) 89.2(1) ? . . . O(6) Ho(1) O(3) 84.1(1) ? . . . Ho(1) O(3) C(10) 88.3(3) ? . . . Ho(1) O(3) Ho(1) 118.5(1) ? . . 2_646 O(4) Ho(1) O(3) 154.7(1) ? . . 2_656 O(5) Ho(1) O(3) 92.2(1) ? . . 2_656 O(6) Ho(1) O(3) 92.8(2) ? . . 2_656 Ho(1) O(3) C(10) 135.9(4) ? . 2_656 2_656 Ho(1) O(3) Ho(1) 118.5(1) ? . 2_656 2_656 O(5) Ho(1) O(4) 95.5(2) ? . . . O(6) Ho(1) O(4) 82.0(1) ? . . . Ho(1) O(4) C(10) 94.9(3) ? . . . O(6) Ho(1) O(5) 173.0(2) ? . . . Ho(1) O(5) C(19) 136.2(4) ? . . . Ho(1) O(6) C(19) 143.2(4) ? . . 2_656 O(1) C(1) O(2) 123.3(5) ? . 2_646 2_646 O(1) C(1) C(2) 119.4(6) ? . 2_646 2_646 O(2) C(1) O(1) 123.3(5) ? . . 2_656 O(2) C(1) C(2) 117.4(6) ? . . . C(10) O(3) Ho(1) 135.9(4) ? . . 2_646 O(3) Ho(1) O(2) 77.2(1) ? . 2_646 2_646 O(3) Ho(1) O(6) 92.8(2) ? . 2_646 2_646 O(3) Ho(1) O(1) 76.8(1) ? . 2_646 2_646 O(3) Ho(1) O(5) 92.2(1) ? . 2_646 2_646 O(3) C(10) O(4) 118.6(5) ? . . . O(3) C(10) C(11) 117.9(5) ? . . . O(4) C(10) C(11) 123.2(5) ? . . . O(5) C(19) O(6) 123.7(5) ? . . 2_646 O(5) C(19) C(20) 117.0(5) ? . . . O(6) C(19) O(5) 123.7(5) ? . 2_656 2_656 O(6) C(19) C(20) 119.3(5) ? . 2_656 2_656 C(2) C(1) O(1) 119.4(6) ? . . 2_656 C(1) O(1) Ho(1) 141.7(4) ? . 2_656 2_656 C(1) C(2) C(3) 121.8(9) ? . . . C(1) C(2) H(1) 119.1163 ? . . . H(1) C(2) C(3) 119.1165 ? . . . C(2) C(3) H(2) 115.8628 ? . . . C(2) C(3) C(4) 128.3(9) ? . . . H(2) C(3) C(4) 115.8631 ? . . . C(3) C(4) C(5) 122.0(7) ? . . . C(3) C(4) C(9) 120.0(7) ? . . . C(4) C(5) H(3) 119.7405 ? . . . C(9) C(4) C(5) 118.0(6) ? . . . C(4) C(5) C(6) 120.5(7) ? . . . C(4) C(9) H(7) 119.7553 ? . . . C(4) C(9) C(8) 120.5(7) ? . . . H(3) C(5) C(6) 119.7409 ? . . . C(5) C(6) C(7) 120.8(7) ? . . . C(5) C(6) H(4) 119.5808 ? . . . C(6) C(7) C(8) 119.1(7) ? . . . H(4) C(6) C(7) 119.5807 ? . . . C(6) C(7) H(5) 120.4289 ? . . . C(7) C(8) C(9) 121.0(8) ? . . . C(7) C(8) H(6) 119.4914 ? . . . H(5) C(7) C(8) 120.4283 ? . . . C(8) C(9) H(7) 119.7557 ? . . . H(6) C(8) C(9) 119.4915 ? . . . C(10) C(11) C(12) 120.4(6) ? . . . C(10) C(11) H(8) 119.8122 ? . . . H(8) C(11) C(12) 119.8119 ? . . . C(11) C(12) H(9) 116.0810 ? . . . C(11) C(12) C(13) 127.8(6) ? . . . H(9) C(12) C(13) 116.0811 ? . . . C(12) C(13) C(18) 122.6(5) ? . . . C(12) C(13) C(14) 119.6(6) ? . . . C(18) C(13) C(14) 117.8(5) ? . . . C(13) C(14) H(10) 119.6117 ? . . . C(13) C(14) C(15) 120.8(7) ? . . . C(13) C(18) H(14) 119.4735 ? . . . C(13) C(18) C(17) 121.1(6) ? . . . H(10) C(14) C(15) 119.6115 ? . . . C(14) C(15) C(16) 120.8(7) ? . . . C(14) C(15) H(11) 119.6242 ? . . . C(15) C(16) C(17) 119.8(6) ? . . . H(11) C(15) C(16) 119.6241 ? . . . C(15) C(16) H(12) 120.1002 ? . . . C(16) C(17) C(18) 119.8(7) ? . . . C(16) C(17) H(13) 120.1169 ? . . . H(12) C(16) C(17) 120.1004 ? . . . C(17) C(18) H(14) 119.4733 ? . . . H(13) C(17) C(18) 120.1165 ? . . . C(19) O(6) Ho(1) 143.2(4) ? . 2_646 2_646 C(20) C(19) O(6) 119.3(5) ? . . 2_646 C(19) C(20) C(21) 122.2(5) ? . . . C(19) C(20) H(15) 118.8815 ? . . . H(15) C(20) C(21) 118.8809 ? . . . C(20) C(21) H(16) 116.5625 ? . . . C(20) C(21) C(22) 126.9(6) ? . . . H(16) C(21) C(22) 116.5622 ? . . . C(21) C(22) C(23) 121.5(6) ? . . . C(21) C(22) C(27) 119.9(6) ? . . . C(22) C(23) H(17) 119.9109 ? . . . C(27) C(22) C(23) 118.5(6) ? . . . C(22) C(23) C(24) 120.2(7) ? . . . C(22) C(27) H(21) 119.7076 ? . . . C(22) C(27) C(26) 120.6(7) ? . . . H(17) C(23) C(24) 119.9108 ? . . . C(23) C(24) C(25) 119.7(9) ? . . . C(23) C(24) H(18) 120.1376 ? . . . C(24) C(25) C(26) 120.2(7) ? . . . H(18) C(24) C(25) 120.1374 ? . . . C(24) C(25) H(19) 119.9222 ? . . . C(25) C(26) C(27) 120.8(7) ? . . . C(25) C(26) H(20) 119.5961 ? . . . H(19) C(25) C(26) 119.9221 ? . . . C(26) C(27) H(21) 119.7073 ? . . . H(20) C(26) C(27) 119.5961 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ho(1) O(1) 3.546(5) ? . 2_656 Ho(1) C(1) 3.254(6) ? . . Ho(1) C(1) 3.339(6) ? . 2_646 Ho(1) C(10) 2.760(5) ? . . Ho(1) C(10) 3.377(5) ? . 2_656 Ho(1) C(19) 3.273(6) ? . . Ho(1) C(19) 3.346(5) ? . 2_656 O(1) Ho(1) 3.546(5) ? . 2_646 O(1) O(2) 2.234(6) ? . 2_646 O(1) O(3) 2.860(6) ? . . O(1) O(3) 2.837(6) ? . 2_656 O(1) O(5) 3.129(6) ? . . O(1) O(6) 3.133(6) ? . . O(1) O(6) 3.417(6) ? . 2_646 O(1) C(2) 2.36(1) ? . 2_646 O(1) C(3) 2.78(1) ? . 2_646 O(1) C(10) 3.039(7) ? . 2_656 O(1) C(11) 3.502(7) ? . 2_656 O(1) C(19) 3.431(7) ? . . O(1) H(1) 3.1990 ? . 2_646 O(1) H(2) 2.4138 ? . 2_646 O(1) H(8) 3.4682 ? . 2_656 O(1) H(11) 3.1436 ? . 1_554 O(2) O(1) 2.234(6) ? . 2_656 O(2) O(3) 2.868(6) ? . 2_656 O(2) O(4) 2.930(6) ? . . O(2) O(5) 3.272(6) ? . . O(2) O(6) 3.290(6) ? . . O(2) C(2) 2.33(1) ? . . O(2) C(3) 3.54(1) ? . . O(2) C(6) 3.474(8) ? . 2_546 O(2) C(16) 3.496(8) ? . 2_657 O(2) H(1) 2.5242 ? . . O(2) H(4) 3.0507 ? . 2_546 O(2) H(7) 3.0360 ? . 1_545 O(2) H(11) 3.0631 ? . 2_657 O(2) H(12) 2.7766 ? . 2_657 O(3) O(1) 2.837(6) ? . 2_646 O(3) O(2) 2.868(6) ? . 2_646 O(3) O(4) 2.176(6) ? . . O(3) O(5) 3.321(5) ? . . O(3) O(5) 3.295(6) ? . 2_646 O(3) O(6) 3.171(6) ? . . O(3) O(6) 3.314(5) ? . 2_646 O(3) C(1) 3.063(7) ? . 2_646 O(3) C(11) 2.386(7) ? . . O(3) C(12) 3.574(7) ? . . O(3) H(2) 3.3697 ? . 1_545 O(3) H(4) 3.1160 ? . 1_645 O(3) H(5) 3.4970 ? . 1_645 O(3) H(8) 2.5945 ? . . O(4) O(5) 3.418(6) ? . . O(4) O(6) 3.033(6) ? . . O(4) C(3) 3.55(1) ? . 1_545 O(4) C(11) 2.393(7) ? . . O(4) C(12) 2.832(7) ? . . O(4) C(15) 3.593(9) ? . 2_657 O(4) C(16) 3.317(9) ? . 2_657 O(4) H(2) 2.6791 ? . 1_545 O(4) H(7) 3.0146 ? . 1_545 O(4) H(8) 3.2180 ? . . O(4) H(9) 2.4807 ? . . O(4) H(11) 3.3905 ? . 2_657 O(4) H(12) 2.8997 ? . 2_657 O(5) O(3) 3.295(6) ? . 2_656 O(5) O(6) 2.214(6) ? . 2_646 O(5) C(6) 3.466(8) ? . 2_546 O(5) C(20) 2.347(7) ? . . O(5) C(21) 3.545(7) ? . . O(5) H(2) 3.1024 ? . 1_545 O(5) H(3) 3.5091 ? . 2_546 O(5) H(4) 2.6096 ? . 2_546 O(5) H(8) 3.1704 ? . 2_656 O(5) H(15) 2.5483 ? . . O(6) O(1) 3.417(6) ? . 2_656 O(6) O(3) 3.314(5) ? . 2_656 O(6) O(5) 2.214(6) ? . 2_656 O(6) C(10) 3.134(7) ? . . O(6) C(20) 2.377(7) ? . 2_656 O(6) C(21) 2.824(7) ? . 2_656 O(6) H(2) 3.5430 ? . 2_646 O(6) H(5) 2.8869 ? . 1_645 O(6) H(11) 3.1164 ? . 2_657 O(6) H(15) 3.2031 ? . 2_656 O(6) H(16) 2.4851 ? . 2_656 C(1) Ho(1) 3.339(6) ? . 2_656 C(1) O(3) 3.063(7) ? . 2_656 C(1) C(3) 2.43(1) ? . . C(1) H(1) 2.0944 ? . . C(1) H(2) 2.5339 ? . . C(1) H(4) 3.5081 ? . 2_546 C(1) H(5) 3.5875 ? . 2_546 C(1) H(11) 3.0464 ? . 2_657 C(1) H(12) 3.2183 ? . 2_657 C(2) O(1) 2.36(1) ? . 2_656 C(2) C(4) 2.52(1) ? . . C(2) C(5) 3.05(1) ? . . C(2) C(7) 3.46(1) ? . 2_546 C(2) H(2) 1.9343 ? . . C(2) H(3) 2.7856 ? . . C(2) H(5) 3.5162 ? . 2_546 C(2) H(12) 3.4430 ? . 2_657 C(2) H(20) 3.3400 ? . 1_566 C(3) O(1) 2.78(1) ? . 2_656 C(3) O(4) 3.55(1) ? . 1_565 C(3) C(5) 2.52(1) ? . . C(3) C(9) 2.48(1) ? . . C(3) H(1) 1.9667 ? . . C(3) H(3) 2.6957 ? . . C(3) H(7) 2.6388 ? . . C(3) H(20) 3.1471 ? . 1_566 C(4) C(6) 2.423(9) ? . . C(4) C(7) 2.80(1) ? . . C(4) C(8) 2.41(1) ? . . C(4) H(1) 2.7159 ? . . C(4) H(2) 2.0730 ? . . C(4) H(3) 2.0538 ? . . C(4) H(4) 3.2781 ? . . C(4) H(6) 3.2608 ? . . C(4) H(7) 2.0360 ? . . C(4) H(19) 2.9295 ? . 1_566 C(4) H(20) 3.3300 ? . 1_566 C(5) C(7) 2.39(1) ? . . C(5) C(8) 2.75(1) ? . . C(5) C(9) 2.40(1) ? . . C(5) H(1) 2.7795 ? . . C(5) H(2) 3.3351 ? . . C(5) H(4) 2.0259 ? . . C(5) H(5) 3.2529 ? . . C(5) H(7) 3.2629 ? . . C(5) H(15) 3.2490 ? . 2_556 C(5) H(19) 2.9101 ? . 1_566 C(6) O(2) 3.474(8) ? . 2_556 C(6) O(5) 3.466(9) ? . 2_556 C(6) C(8) 2.38(1) ? . . C(6) C(9) 2.76(1) ? . . C(6) H(1) 3.4262 ? . 2_556 C(6) H(3) 2.0274 ? . . C(6) H(5) 2.0268 ? . . C(6) H(6) 3.2319 ? . . C(6) H(15) 3.1663 ? . 2_556 C(6) H(19) 2.9991 ? . 1_566 C(7) C(2) 3.46(1) ? . 2_556 C(7) C(9) 2.41(1) ? . . C(7) H(1) 3.4539 ? . 2_556 C(7) H(3) 3.2475 ? . . C(7) H(4) 2.0186 ? . . C(7) H(6) 2.0260 ? . . C(7) H(7) 3.2595 ? . . C(7) H(19) 3.1031 ? . 1_566 C(8) H(3) 3.4834 ? . 2_556 C(8) H(4) 3.2338 ? . . C(8) H(5) 2.0352 ? . . C(8) H(7) 2.0298 ? . . C(8) H(19) 3.1176 ? . 1_566 C(9) H(2) 2.6141 ? . . C(9) H(3) 3.2600 ? . . C(9) H(3) 3.3352 ? . 2_556 C(9) H(5) 3.2639 ? . . C(9) H(6) 2.0272 ? . . C(9) H(12) 3.3823 ? . 2_667 C(9) H(19) 3.0423 ? . 1_566 C(10) Ho(1) 3.377(5) ? . 2_646 C(10) O(1) 3.039(7) ? . 2_646 C(10) C(12) 2.435(7) ? . . C(10) H(2) 3.0203 ? . 1_545 C(10) H(8) 2.1236 ? . . C(10) H(9) 2.5299 ? . . C(11) O(1) 3.502(7) ? . 2_646 C(11) C(13) 2.497(8) ? . . C(11) C(18) 3.027(9) ? . . C(11) H(4) 3.5136 ? . 1_645 C(11) H(9) 1.9356 ? . . C(11) H(14) 2.7588 ? . . C(11) H(16) 3.4227 ? . 2_656 C(12) C(14) 2.468(8) ? . . C(12) C(18) 2.503(9) ? . . C(12) H(8) 1.9725 ? . . C(12) H(10) 2.6238 ? . . C(12) H(10) 3.5859 ? . 2_647 C(12) H(14) 2.6786 ? . . C(12) H(16) 3.2787 ? . 2_656 C(12) H(21) 3.4167 ? . 2_656 C(13) C(15) 2.411(8) ? . . C(13) C(16) 2.794(9) ? . . C(13) C(17) 2.425(9) ? . . C(13) H(8) 2.7112 ? . . C(13) H(9) 2.0616 ? . . C(13) H(10) 2.0408 ? . . C(13) H(10) 3.0743 ? . 2_647 C(13) H(11) 3.2650 ? . . C(13) H(13) 3.2798 ? . . C(13) H(14) 2.0379 ? . . C(13) H(21) 2.9661 ? . 2_656 C(14) C(16) 2.39(1) ? . . C(14) C(17) 2.76(1) ? . . C(14) C(18) 2.39(1) ? . . C(14) H(9) 2.5935 ? . . C(14) H(11) 2.0221 ? . . C(14) H(12) 3.2478 ? . . C(14) H(14) 3.2522 ? . . C(14) H(16) 3.4777 ? . 1_556 C(14) H(21) 3.2561 ? . 1_556 C(14) H(21) 3.0002 ? . 2_656 C(15) O(4) 3.593(9) ? . 2_647 C(15) C(17) 2.38(1) ? . . C(15) C(18) 2.75(1) ? . . C(15) H(9) 3.2017 ? . 2_647 C(15) H(10) 2.0220 ? . . C(15) H(12) 2.0260 ? . . C(15) H(13) 3.2419 ? . . C(15) H(16) 3.3813 ? . 1_556 C(15) H(20) 3.5888 ? . 2_656 C(15) H(21) 3.4592 ? . 2_656 C(16) O(2) 3.496(8) ? . 2_647 C(16) O(4) 3.317(9) ? . 2_647 C(16) C(18) 2.395(9) ? . . C(16) H(7) 3.5419 ? . 2_637 C(16) H(9) 3.0277 ? . 2_647 C(16) H(10) 3.2447 ? . . C(16) H(11) 2.0213 ? . . C(16) H(13) 2.0298 ? . . C(16) H(14) 3.2497 ? . . C(16) H(20) 3.5415 ? . 2_656 C(17) H(9) 3.2814 ? . 2_647 C(17) H(10) 3.3847 ? . 2_647 C(17) H(11) 3.2394 ? . . C(17) H(12) 2.0296 ? . . C(17) H(14) 2.0332 ? . . C(17) H(18) 3.2905 ? . 1_656 C(18) H(8) 2.7860 ? . . C(18) H(9) 3.3167 ? . . C(18) H(10) 3.2528 ? . . C(18) H(10) 2.9038 ? . 2_647 C(18) H(12) 3.2551 ? . . C(18) H(13) 2.0395 ? . . C(18) H(18) 3.3638 ? . 1_656 C(18) H(21) 3.3828 ? . 2_656 C(19) Ho(1) 3.346(5) ? . 2_646 C(19) C(21) 2.463(8) ? . . C(19) H(2) 3.4640 ? . 1_545 C(19) H(4) 3.3859 ? . 2_546 C(19) H(5) 3.0883 ? . 2_536 C(19) H(8) 3.3189 ? . 2_656 C(19) H(11) 3.3887 ? . 1_554 C(19) H(15) 2.1223 ? . . C(19) H(16) 2.5724 ? . . C(20) O(6) 2.377(7) ? . 2_646 C(20) C(22) 2.499(8) ? . . C(20) C(23) 3.024(8) ? . . C(20) H(4) 3.3114 ? . 2_546 C(20) H(5) 2.9751 ? . 2_536 C(20) H(6) 3.3829 ? . 2_536 C(20) H(8) 3.1837 ? . 2_656 C(20) H(14) 3.3470 ? . 2_656 C(20) H(16) 1.9381 ? . . C(20) H(17) 2.7679 ? . . C(21) O(6) 2.824(7) ? . 2_646 C(21) C(23) 2.513(8) ? . . C(21) C(27) 2.470(9) ? . . C(21) H(5) 2.9272 ? . 2_536 C(21) H(10) 3.3195 ? . 1_554 C(21) H(11) 3.4673 ? . 1_554 C(21) H(14) 3.4423 ? . 2_656 C(21) H(15) 1.9611 ? . . C(21) H(17) 2.6845 ? . . C(21) H(21) 2.6242 ? . . C(22) C(24) 2.42(1) ? . . C(22) C(25) 2.786(9) ? . . C(22) C(26) 2.406(9) ? . . C(22) H(10) 3.4911 ? . 1_554 C(22) H(13) 3.3825 ? . 2_656 C(22) H(14) 3.3323 ? . 2_656 C(22) H(15) 2.6840 ? . . C(22) H(16) 2.0813 ? . . C(22) H(17) 2.0502 ? . . C(22) H(18) 3.2820 ? . . C(22) H(18) 3.3070 ? . 2_545 C(22) H(20) 3.2579 ? . . C(22) H(21) 2.0244 ? . . C(23) C(25) 2.40(1) ? . . C(23) C(26) 2.76(1) ? . . C(23) C(27) 2.39(1) ? . . C(23) H(13) 3.1306 ? . 2_656 C(23) H(14) 3.3996 ? . 2_656 C(23) H(15) 2.7467 ? . . C(23) H(16) 3.3203 ? . . C(23) H(18) 2.0419 ? . . C(23) H(18) 3.5514 ? . 2_545 C(23) H(19) 3.2617 ? . . C(23) H(21) 3.2531 ? . . C(24) C(26) 2.37(1) ? . . C(24) C(27) 2.76(1) ? . . C(24) H(13) 3.3386 ? . 1_454 C(24) H(13) 2.9436 ? . 2_656 C(24) H(17) 2.0397 ? . . C(24) H(18) 3.5766 ? . 2_545 C(24) H(19) 2.0348 ? . . C(24) H(20) 3.2316 ? . . C(25) C(27) 2.39(1) ? . . C(25) H(13) 3.0434 ? . 2_656 C(25) H(17) 3.2608 ? . . C(25) H(17) 3.2441 ? . 2_545 C(25) H(18) 2.0369 ? . . C(25) H(18) 3.3316 ? . 2_545 C(25) H(20) 2.0001 ? . . C(25) H(21) 3.2367 ? . . C(26) H(13) 3.2927 ? . 2_656 C(26) H(17) 3.4271 ? . 2_545 C(26) H(18) 3.2298 ? . . C(26) H(18) 3.0536 ? . 2_545 C(26) H(19) 2.0033 ? . . C(26) H(21) 2.0373 ? . . C(27) C(21) 2.470(9) ? . . C(27) C(23) 2.39(1) ? . . C(27) C(24) 2.76(1) ? . . C(27) C(25) 2.39(1) ? . . C(27) H(10) 3.3112 ? . 1_554 C(27) H(13) 3.4615 ? . 2_656 C(27) H(16) 2.6285 ? . . C(27) H(17) 3.2504 ? . . C(27) H(18) 3.0266 ? . 2_545 C(27) H(19) 3.2439 ? . . C(27) H(20) 2.0362 ? . . H(1) O(1) 3.1990 ? . 2_656 H(1) C(6) 3.4262 ? . 2_546 H(1) C(7) 3.4539 ? . 2_546 H(2) O(1) 2.4138 ? . 2_656 H(2) O(3) 3.3697 ? . 1_565 H(2) O(4) 2.6791 ? . 1_565 H(2) O(5) 3.1024 ? . 1_565 H(2) O(6) 3.5430 ? . 2_656 H(2) C(10) 3.0203 ? . 1_565 H(2) C(19) 3.4640 ? . 1_565 H(3) O(5) 3.5091 ? . 2_556 H(3) C(8) 3.4834 ? . 2_546 H(3) C(9) 3.3352 ? . 2_546 H(4) O(2) 3.0507 ? . 2_556 H(4) O(3) 3.1160 ? . 1_465 H(4) O(5) 2.6096 ? . 2_556 H(4) C(1) 3.5081 ? . 2_556 H(4) C(11) 3.5136 ? . 1_465 H(4) C(19) 3.3859 ? . 2_556 H(4) C(20) 3.3114 ? . 2_556 H(5) O(3) 3.4970 ? . 1_465 H(5) O(6) 2.8869 ? . 1_465 H(5) C(1) 3.5875 ? . 2_556 H(5) C(2) 3.5162 ? . 2_556 H(5) C(5) 3.2529 ? . . H(5) C(6) 2.0268 ? . . H(5) C(8) 2.0352 ? . . H(5) C(9) 3.2639 ? . . H(5) C(19) 3.0883 ? . 2_566 H(5) C(20) 2.9751 ? . 2_566 H(5) C(21) 2.9272 ? . 2_566 H(6) C(20) 3.3829 ? . 2_566 H(7) O(2) 3.0360 ? . 1_565 H(7) O(4) 3.0146 ? . 1_565 H(7) C(3) 2.6388 ? . . H(7) C(4) 2.0360 ? . . H(7) C(5) 3.2629 ? . . H(7) C(7) 3.2595 ? . . H(7) C(8) 2.0298 ? . . H(7) C(16) 3.5419 ? . 2_667 H(8) O(1) 3.4682 ? . 2_646 H(8) O(5) 3.1704 ? . 2_646 H(8) C(19) 3.3189 ? . 2_646 H(8) C(20) 3.1837 ? . 2_646 H(9) C(15) 3.2017 ? . 2_657 H(9) C(16) 3.0277 ? . 2_657 H(9) C(17) 3.2814 ? . 2_657 H(10) C(12) 3.5859 ? . 2_657 H(10) C(13) 3.0743 ? . 2_657 H(10) C(17) 3.3847 ? . 2_657 H(10) C(18) 2.9038 ? . 2_657 H(10) C(21) 3.3195 ? . 1_556 H(10) C(22) 3.4911 ? . 1_556 H(10) C(27) 3.3112 ? . 1_556 H(11) O(1) 3.1436 ? . 1_556 H(11) O(2) 3.0631 ? . 2_647 H(11) O(4) 3.3905 ? . 2_647 H(11) O(6) 3.1164 ? . 2_647 H(11) C(1) 3.0464 ? . 2_647 H(11) C(19) 3.3887 ? . 1_556 H(11) C(21) 3.4673 ? . 1_556 H(12) O(2) 2.7766 ? . 2_647 H(12) O(4) 2.8997 ? . 2_647 H(12) C(1) 3.2183 ? . 2_647 H(12) C(2) 3.4430 ? . 2_647 H(12) C(9) 3.3823 ? . 2_637 H(13) C(22) 3.3825 ? . 2_646 H(13) C(23) 3.1306 ? . 2_646 H(13) C(24) 3.3386 ? . 1_656 H(13) C(24) 2.9436 ? . 2_646 H(13) C(25) 3.0434 ? . 2_646 H(13) C(26) 3.2927 ? . 2_646 H(13) C(27) 3.4615 ? . 2_646 H(14) C(20) 3.3470 ? . 2_646 H(14) C(21) 3.4423 ? . 2_646 H(14) C(22) 3.3323 ? . 2_646 H(14) C(23) 3.3996 ? . 2_646 H(15) O(6) 3.2031 ? . 2_646 H(15) C(5) 3.2490 ? . 2_546 H(15) C(6) 3.1663 ? . 2_546 H(16) O(6) 2.4851 ? . 2_646 H(16) C(11) 3.4227 ? . 2_646 H(16) C(12) 3.2787 ? . 2_646 H(16) C(14) 3.4777 ? . 1_554 H(16) C(15) 3.3813 ? . 1_554 H(16) C(19) 2.5724 ? . . H(16) C(20) 1.9381 ? . . H(16) C(22) 2.0813 ? . . H(16) C(23) 3.3203 ? . . H(16) C(27) 2.6285 ? . . H(17) C(25) 3.2441 ? . 2_555 H(17) C(26) 3.4271 ? . 2_555 H(17) C(27) 3.2504 ? . . H(18) C(17) 3.2905 ? . 1_454 H(18) C(18) 3.3638 ? . 1_454 H(18) C(22) 3.3070 ? . 2_555 H(18) C(23) 3.5514 ? . 2_555 H(18) C(24) 3.5766 ? . 2_555 H(18) C(25) 3.3316 ? . 2_555 H(18) C(26) 3.0536 ? . 2_555 H(18) C(27) 3.0266 ? . 2_555 H(19) C(4) 2.9295 ? . 1_544 H(19) C(5) 2.9101 ? . 1_544 H(19) C(6) 2.9991 ? . 1_544 H(19) C(7) 3.1031 ? . 1_544 H(19) C(8) 3.1176 ? . 1_544 H(19) C(9) 3.0423 ? . 1_544 H(19) C(23) 3.2617 ? . . H(19) C(24) 2.0348 ? . . H(19) C(26) 2.0033 ? . . H(19) C(27) 3.2439 ? . . H(20) C(2) 3.3400 ? . 1_544 H(20) C(3) 3.1471 ? . 1_544 H(20) C(4) 3.3300 ? . 1_544 H(20) C(15) 3.5888 ? . 2_646 H(20) C(16) 3.5415 ? . 2_646 H(20) C(27) 2.0362 ? . . H(21) C(12) 3.4167 ? . 2_646 H(21) C(13) 2.9661 ? . 2_646 H(21) C(14) 3.2561 ? . 1_554 H(21) C(14) 3.0002 ? . 2_646 H(21) C(15) 3.4592 ? . 2_646 H(21) C(18) 3.3828 ? . 2_646 Ho(1) Ho(1) 4.122(2) ? . 2_656 Ho(1) Ho(1) 4.122(2) ? 2_646 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(3) H(2) O(1) 2_656 0.95 2.41 2.780(11) 103 ? C(12) H(9) O(4) . 0.95 2.48 2.833(7) 102 ? C(21) H(16) O(6) 2_646 0.95 2.48 2.824(7) 101 ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Yb-wt1267w.cif' #============================================================================== data_Yb-wt1267w _database_code_depnum_ccdc_archive 'CCDC 631229' # Kin-K371-Ybcinnamate #============================================================================== _audit_creation_date 2006-06-29 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 O6 Yb ' _chemical_formula_moiety 'C27 H21 O6 Yb ' _chemical_formula_weight 614.50 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.574(2) _cell_length_b 7.848(2) _cell_length_c 13.043(3) _cell_angle_alpha 90 _cell_angle_beta 94.384(3) _cell_angle_gamma 90 _cell_volume 1181.3(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7370 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 602.00 _exptl_absorpt_coefficient_mu 3.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_T_max 0.670 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7370 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 27.52 _diffrn_measured_fraction_theta_max 0.9736 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.9736 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0\s(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0\s(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2832 _reflns_number_gt 2644 _reflns_threshold_expression I>2.0\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0370 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2648 _refine_ls_number_parameters 329 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.045]' _refine_ls_shift/su_max 0.0230 _refine_diff_density_max 1.73 _refine_diff_density_min -0.97 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 2832 Friedel Pairs' _refine_ls_abs_structure_Flack 0.00(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Yb Yb -0.385 5.549 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Yb(1) Yb 0.46113(3) 0.4310(3) 0.52366(2) 0.02386(7) Uani 1.00 1 d . . . O(1) O 0.5946(6) 0.3630(9) 0.4174(6) 0.041(2) Uani 1.00 1 d . . . O(2) O 0.3267(6) 0.6033(9) 0.5826(5) 0.035(2) Uani 1.00 1 d . . . O(3) O 0.5414(6) 0.1588(9) 0.5860(5) 0.033(2) Uani 1.00 1 d . . . O(4) O 0.4167(6) 0.2931(9) 0.6746(5) 0.036(2) Uani 1.00 1 d . . . O(5) O 0.3318(6) 0.2920(9) 0.4222(5) 0.039(2) Uani 1.00 1 d . . . O(6) O 0.6017(6) 0.5436(10) 0.6285(6) 0.041(2) Uani 1.00 1 d . . . C(1) C 0.3209(9) 0.762(1) 0.5883(7) 0.034(3) Uani 1.00 1 d . . . C(2) C 0.207(2) 0.840(3) 0.6043(13) 0.034(4) Uani 1.00 1 d . . . C(3) C 0.190(2) 1.008(3) 0.608(1) 0.041(4) Uani 1.00 1 d . . . C(4) C 0.0818(9) 1.096(1) 0.6198(8) 0.037(3) Uani 1.00 1 d . . . C(5) C -0.0262(9) 1.016(1) 0.6156(8) 0.042(3) Uani 1.00 1 d . . . C(6) C -0.1268(9) 1.105(2) 0.6306(9) 0.049(3) Uani 1.00 1 d . . . C(7) C -0.1187(12) 1.280(2) 0.6513(10) 0.061(4) Uani 1.00 1 d . . . C(8) C -0.0143(11) 1.360(2) 0.6557(11) 0.060(4) Uani 1.00 1 d . . . C(9) C 0.0840(11) 1.272(2) 0.6390(10) 0.052(3) Uani 1.00 1 d . . . C(10) C 0.4969(8) 0.1869(12) 0.6731(7) 0.031(2) Uani 1.00 1 d . . . C(11) C 0.5531(9) 0.1107(13) 0.7681(7) 0.036(3) Uani 1.00 1 d . . . C(12) C 0.5266(9) 0.1618(13) 0.8600(8) 0.039(3) Uani 1.00 1 d . . . C(13) C 0.5849(9) 0.1160(13) 0.9596(7) 0.037(3) Uani 1.00 1 d . . . C(14) C 0.6877(10) 0.026(2) 0.9701(8) 0.047(3) Uani 1.00 1 d . . . C(15) C 0.7408(11) -0.008(2) 1.0668(9) 0.059(4) Uani 1.00 1 d . . . C(16) C 0.6931(11) 0.047(2) 1.1537(8) 0.054(3) Uani 1.00 1 d . . . C(17) C 0.5926(12) 0.133(2) 1.1448(8) 0.057(4) Uani 1.00 1 d . . . C(18) C 0.5373(10) 0.171(2) 1.0484(8) 0.047(3) Uani 1.00 1 d . . . C(19) C 0.3331(8) 0.1700(12) 0.3589(7) 0.031(2) Uani 1.00 1 d . . . C(20) C 0.2525(9) 0.1800(12) 0.2658(7) 0.034(2) Uani 1.00 1 d . . . C(21) C 0.2620(9) 0.0806(13) 0.1836(8) 0.037(3) Uani 1.00 1 d . . . C(22) C 0.1906(9) 0.085(1) 0.0876(8) 0.038(3) Uani 1.00 1 d . . . C(23) C 0.0824(9) 0.164(2) 0.0772(8) 0.048(3) Uani 1.00 1 d . . . C(24) C 0.018(2) 0.170(3) -0.0165(12) 0.054(5) Uani 1.00 1 d . . . C(25) C 0.0593(12) 0.094(2) -0.1015(9) 0.059(4) Uani 1.00 1 d . . . C(26) C 0.1633(12) 0.013(2) -0.0944(9) 0.062(4) Uani 1.00 1 d . . . C(27) C 0.2296(11) 0.008(2) 0.0019(9) 0.053(3) Uani 1.00 1 d . . . H(1) H 0.1428 0.7661 0.6124 0.041 Uiso 1.00 1 c R . . H(2) H 0.2557 1.0773 0.6015 0.049 Uiso 1.00 1 c R . . H(3) H -0.0309 0.8972 0.6020 0.051 Uiso 1.00 1 c R . . H(4) H -0.1996 1.0491 0.6270 0.058 Uiso 1.00 1 c R . . H(5) H -0.1866 1.3431 0.6624 0.073 Uiso 1.00 1 c R . . H(6) H -0.0098 1.4784 0.6706 0.072 Uiso 1.00 1 c R . . H(7) H 0.1557 1.3313 0.6404 0.062 Uiso 1.00 1 c R . . H(8) H 0.6093 0.0234 0.7629 0.044 Uiso 1.00 1 c R . . H(9) H 0.4624 0.2369 0.8615 0.046 Uiso 1.00 1 c R . . H(10) H 0.7222 -0.0133 0.9106 0.057 Uiso 1.00 1 c R . . H(11) H 0.8111 -0.0712 1.0729 0.070 Uiso 1.00 1 c R . . H(12) H 0.7309 0.0257 1.2197 0.065 Uiso 1.00 1 c R . . H(13) H 0.5582 0.1682 1.2051 0.069 Uiso 1.00 1 c R . . H(14) H 0.4671 0.2340 1.0437 0.056 Uiso 1.00 1 c R . . H(15) H 0.1912 0.2606 0.2642 0.041 Uiso 1.00 1 c R . . H(16) H 0.3222 -0.0019 0.1887 0.045 Uiso 1.00 1 c R . . H(17) H 0.0523 0.2148 0.1357 0.058 Uiso 1.00 1 c R . . H(18) H -0.0547 0.2265 -0.0222 0.065 Uiso 1.00 1 c R . . H(19) H 0.0148 0.0987 -0.1657 0.071 Uiso 1.00 1 c R . . H(20) H 0.1914 -0.0399 -0.1531 0.075 Uiso 1.00 1 c R . . H(21) H 0.3020 -0.0493 0.0071 0.063 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Yb(1) 0.0291(2) 0.0159(1) 0.0261(1) -0.0008(4) -0.00027(10) -0.0002(4) O(1) 0.034(3) 0.045(4) 0.047(4) 0.011(3) 0.016(3) 0.018(3) O(2) 0.046(4) 0.023(3) 0.038(4) 0.004(3) 0.012(3) -0.001(3) O(3) 0.047(4) 0.023(3) 0.030(3) 0.001(3) 0.003(3) 0.001(3) O(4) 0.048(4) 0.028(4) 0.033(3) 0.009(3) 0.005(3) 0.001(3) O(5) 0.040(4) 0.035(4) 0.040(4) 0.002(3) -0.004(3) -0.009(3) O(6) 0.041(4) 0.032(4) 0.047(4) -0.003(3) -0.016(3) -0.003(3) C(1) 0.040(5) 0.040(6) 0.023(4) 0.006(5) -0.001(4) -0.002(4) C(2) 0.029(6) 0.031(8) 0.043(8) -0.004(6) 0.006(5) 0.001(7) C(3) 0.040(8) 0.032(8) 0.050(10) -0.001(7) 0.004(7) 0.001(7) C(4) 0.035(5) 0.030(5) 0.046(6) 0.004(4) -0.000(4) 0.000(4) C(5) 0.045(6) 0.032(6) 0.051(6) 0.000(5) 0.004(5) -0.003(5) C(6) 0.033(5) 0.050(7) 0.063(7) 0.001(5) -0.001(5) 0.001(6) C(7) 0.053(7) 0.064(9) 0.064(8) 0.029(7) 0.001(6) -0.009(7) C(8) 0.065(8) 0.029(5) 0.084(9) 0.013(6) -0.002(7) -0.005(6) C(9) 0.060(7) 0.031(6) 0.063(8) -0.008(5) 0.001(6) -0.002(5) C(10) 0.045(5) 0.019(4) 0.030(4) -0.010(4) 0.004(4) 0.001(4) C(11) 0.048(6) 0.023(5) 0.037(5) 0.007(4) 0.001(4) -0.000(4) C(12) 0.049(6) 0.027(5) 0.041(5) 0.008(5) 0.006(4) 0.009(4) C(13) 0.051(6) 0.027(5) 0.033(5) -0.003(4) 0.001(4) 0.005(4) C(14) 0.057(7) 0.043(7) 0.042(6) 0.009(6) 0.006(5) 0.002(5) C(15) 0.061(7) 0.063(8) 0.050(6) 0.014(6) -0.009(6) 0.005(6) C(16) 0.064(7) 0.061(8) 0.034(5) -0.003(7) -0.009(5) 0.014(6) C(17) 0.074(8) 0.067(9) 0.031(5) -0.007(7) 0.009(5) 0.003(6) C(18) 0.051(6) 0.045(6) 0.047(6) 0.006(6) 0.007(5) 0.004(5) C(19) 0.032(4) 0.024(5) 0.035(5) -0.005(4) -0.007(4) 0.005(4) C(20) 0.041(5) 0.021(5) 0.040(5) 0.002(4) -0.011(4) -0.000(4) C(21) 0.039(5) 0.029(5) 0.043(5) 0.004(4) -0.006(4) 0.010(4) C(22) 0.044(5) 0.031(5) 0.039(5) -0.003(4) -0.003(4) -0.009(4) C(23) 0.043(6) 0.059(7) 0.042(6) 0.001(6) -0.004(4) -0.008(6) C(24) 0.059(11) 0.048(7) 0.053(11) 0.010(7) -0.015(7) -0.006(8) C(25) 0.082(9) 0.052(7) 0.040(6) -0.008(7) -0.022(6) 0.003(6) C(26) 0.079(9) 0.066(8) 0.041(6) -0.005(8) -0.000(6) -0.009(6) C(27) 0.056(7) 0.048(6) 0.053(7) 0.006(6) -0.003(5) -0.002(6) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Yb(1) O(1) 2.218(7) ? . . Yb(1) O(2) 2.242(7) ? . . Yb(1) O(3) 2.443(7) ? . . Yb(1) O(3) 2.289(7) ? . 2_656 Yb(1) O(4) 2.338(7) ? . . Yb(1) O(5) 2.209(7) ? . . Yb(1) O(6) 2.227(7) ? . . O(1) C(1) 1.26(1) ? . 2_646 O(2) C(1) 1.25(1) ? . . O(3) Yb(1) 2.289(7) ? . 2_646 O(3) C(10) 1.30(1) ? . . O(4) C(10) 1.25(1) ? . . O(5) C(19) 1.26(1) ? . . O(6) C(19) 1.25(1) ? . 2_656 C(1) O(1) 1.26(1) ? . 2_656 C(1) C(2) 1.48(2) ? . . C(2) C(3) 1.33(3) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.44(2) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.39(1) ? . . C(4) C(9) 1.41(2) ? . . C(5) C(6) 1.39(2) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.40(2) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.36(2) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.36(2) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . C(10) C(11) 1.48(1) ? . . C(11) C(12) 1.32(1) ? . . C(11) H(8) 0.9500 ? . . C(12) C(13) 1.46(1) ? . . C(12) H(9) 0.9500 ? . . C(13) C(14) 1.38(2) ? . . C(13) C(18) 1.39(2) ? . . C(14) C(15) 1.39(2) ? . . C(14) H(10) 0.9500 ? . . C(15) C(16) 1.37(2) ? . . C(15) H(11) 0.9500 ? . . C(16) C(17) 1.34(2) ? . . C(16) H(12) 0.9500 ? . . C(17) C(18) 1.40(2) ? . . C(17) H(13) 0.9500 ? . . C(18) H(14) 0.9500 ? . . C(19) O(6) 1.25(1) ? . 2_646 C(19) C(20) 1.48(1) ? . . C(20) C(21) 1.34(1) ? . . C(20) H(15) 0.9500 ? . . C(21) C(22) 1.45(1) ? . . C(21) H(16) 0.9500 ? . . C(22) C(23) 1.40(2) ? . . C(22) C(27) 1.38(2) ? . . C(23) C(24) 1.38(2) ? . . C(23) H(17) 0.9500 ? . . C(24) C(25) 1.38(2) ? . . C(24) H(18) 0.9500 ? . . C(25) C(26) 1.36(2) ? . . C(25) H(19) 0.9500 ? . . C(26) C(27) 1.42(2) ? . . C(26) H(20) 0.9500 ? . . C(27) H(21) 0.9500 ? . . H(21) C(27) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Yb(1) O(1) 153.4(3) ? . . . O(3) Yb(1) O(1) 74.5(2) ? . . . O(3) Yb(1) O(1) 76.9(3) ? 2_656 . . O(4) Yb(1) O(1) 128.6(3) ? . . . O(5) Yb(1) O(1) 88.8(3) ? . . . O(6) Yb(1) O(1) 88.2(3) ? . . . Yb(1) O(1) C(1) 140.0(6) ? . . 2_646 O(3) Yb(1) O(2) 132.0(2) ? . . . O(3) Yb(1) O(2) 76.5(2) ? 2_656 . . O(4) Yb(1) O(2) 77.7(2) ? . . . O(5) Yb(1) O(2) 92.7(3) ? . . . O(6) Yb(1) O(2) 92.5(3) ? . . . Yb(1) O(2) C(1) 131.5(7) ? . . . O(3) Yb(1) O(3) 151.3(2) ? 2_656 . . O(4) Yb(1) O(3) 54.4(2) ? . . . O(5) Yb(1) O(3) 89.5(2) ? . . . O(6) Yb(1) O(3) 84.3(2) ? . . . Yb(1) O(3) C(10) 88.7(5) ? . . . Yb(1) O(3) Yb(1) 119.2(3) ? . . 2_646 O(4) Yb(1) O(3) 153.5(2) ? . . 2_656 O(5) Yb(1) O(3) 92.0(2) ? . . 2_656 O(6) Yb(1) O(3) 92.7(3) ? . . 2_656 Yb(1) O(3) C(10) 133.7(6) ? . 2_656 2_656 Yb(1) O(3) Yb(1) 119.2(3) ? . 2_656 2_656 O(5) Yb(1) O(4) 95.4(3) ? . . . O(6) Yb(1) O(4) 82.2(3) ? . . . Yb(1) O(4) C(10) 94.8(6) ? . . . O(6) Yb(1) O(5) 173.6(3) ? . . . Yb(1) O(5) C(19) 136.3(6) ? . . . Yb(1) O(6) C(19) 143.2(6) ? . . 2_656 O(1) C(1) O(2) 125.1(9) ? . 2_646 2_646 O(1) C(1) C(2) 117(1) ? . 2_646 2_646 O(2) C(1) O(1) 125.1(9) ? . . 2_656 O(2) C(1) C(2) 117(1) ? . . . C(10) O(3) Yb(1) 133.7(6) ? . . 2_646 O(3) Yb(1) O(2) 76.5(2) ? . 2_646 2_646 O(3) Yb(1) O(6) 92.7(3) ? . 2_646 2_646 O(3) Yb(1) O(1) 76.9(3) ? . 2_646 2_646 O(3) Yb(1) O(5) 92.0(2) ? . 2_646 2_646 O(3) C(10) O(4) 118.1(8) ? . . . O(3) C(10) C(11) 119.0(8) ? . . . O(4) C(10) C(11) 122.4(8) ? . . . O(5) C(19) O(6) 123.6(8) ? . . 2_646 O(5) C(19) C(20) 117.3(8) ? . . . O(6) C(19) O(5) 123.6(8) ? . 2_656 2_656 O(6) C(19) C(20) 119.1(8) ? . 2_656 2_656 C(2) C(1) O(1) 117(1) ? . . 2_656 C(1) O(1) Yb(1) 140.0(6) ? . 2_656 2_656 C(1) C(2) C(3) 123(1) ? . . . C(1) C(2) H(1) 118.4936 ? . . . H(1) C(2) C(3) 118.4936 ? . . . C(2) C(3) H(2) 116.2838 ? . . . C(2) C(3) C(4) 127(1) ? . . . H(2) C(3) C(4) 116.2837 ? . . . C(3) C(4) C(5) 124(1) ? . . . C(3) C(4) C(9) 119(1) ? . . . C(4) C(5) H(3) 119.0523 ? . . . C(9) C(4) C(5) 116(1) ? . . . C(4) C(5) C(6) 121(1) ? . . . C(4) C(9) H(7) 119.2609 ? . . . C(4) C(9) C(8) 121(1) ? . . . H(3) C(5) C(6) 119.0522 ? . . . C(5) C(6) C(7) 118(1) ? . . . C(5) C(6) H(4) 120.7131 ? . . . C(6) C(7) C(8) 120(1) ? . . . H(4) C(6) C(7) 120.7131 ? . . . C(6) C(7) H(5) 119.7673 ? . . . C(7) C(8) C(9) 120(1) ? . . . C(7) C(8) H(6) 119.6598 ? . . . H(5) C(7) C(8) 119.7675 ? . . . C(8) C(9) H(7) 119.2606 ? . . . H(6) C(8) C(9) 119.6599 ? . . . C(10) C(11) C(12) 121.2(9) ? . . . C(10) C(11) H(8) 119.3822 ? . . . H(8) C(11) C(12) 119.3823 ? . . . C(11) C(12) H(9) 116.2921 ? . . . C(11) C(12) C(13) 127(1) ? . . . H(9) C(12) C(13) 116.2918 ? . . . C(12) C(13) C(14) 123.3(9) ? . . . C(12) C(13) C(18) 118(1) ? . . . C(13) C(14) H(10) 119.7730 ? . . . C(18) C(13) C(14) 118.0(9) ? . . . C(13) C(14) C(15) 120(1) ? . . . C(13) C(18) H(14) 119.9763 ? . . . C(13) C(18) C(17) 120(1) ? . . . H(10) C(14) C(15) 119.7734 ? . . . C(14) C(15) C(16) 120(1) ? . . . C(14) C(15) H(11) 119.5713 ? . . . C(15) C(16) C(17) 119(1) ? . . . H(11) C(15) C(16) 119.5710 ? . . . C(15) C(16) H(12) 120.3368 ? . . . C(16) C(17) C(18) 121(1) ? . . . C(16) C(17) H(13) 119.3571 ? . . . H(12) C(16) C(17) 120.3362 ? . . . C(17) C(18) H(14) 119.9756 ? . . . H(13) C(17) C(18) 119.3573 ? . . . C(19) O(6) Yb(1) 143.2(6) ? . 2_646 2_646 C(20) C(19) O(6) 119.1(8) ? . . 2_646 C(19) C(20) C(21) 122.9(9) ? . . . C(19) C(20) H(15) 118.5264 ? . . . H(15) C(20) C(21) 118.5267 ? . . . C(20) C(21) H(16) 116.4128 ? . . . C(20) C(21) C(22) 127.2(9) ? . . . H(16) C(21) C(22) 116.4131 ? . . . C(21) C(22) C(23) 122.9(9) ? . . . C(21) C(22) C(27) 119(1) ? . . . C(22) C(23) H(17) 119.3490 ? . . . C(27) C(22) C(23) 117(1) ? . . . C(22) C(23) C(24) 121(1) ? . . . C(22) C(27) H(21) 119.3938 ? . . . C(22) C(27) C(26) 121(1) ? . . . H(17) C(23) C(24) 119.3496 ? . . . C(23) C(24) C(25) 120(1) ? . . . C(23) C(24) H(18) 119.9473 ? . . . C(24) C(25) C(26) 120(1) ? . . . H(18) C(24) C(25) 119.9472 ? . . . C(24) C(25) H(19) 119.7339 ? . . . C(25) C(26) C(27) 119(1) ? . . . C(25) C(26) H(20) 120.3780 ? . . . H(19) C(25) C(26) 119.7339 ? . . . C(26) C(27) H(21) 119.3932 ? . . . H(20) C(26) C(27) 120.3781 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Yb(1) O(1) 3.547(8) ? . 2_656 Yb(1) C(1) 3.21(1) ? . . Yb(1) C(1) 3.29(1) ? . 2_646 Yb(1) C(10) 2.742(9) ? . . Yb(1) C(10) 3.323(9) ? . 2_656 Yb(1) C(19) 3.243(9) ? . . Yb(1) C(19) 3.313(9) ? . 2_656 O(1) Yb(1) 3.547(8) ? . 2_646 O(1) O(2) 2.23(1) ? . 2_646 O(1) O(3) 2.83(1) ? . . O(1) O(3) 2.80(1) ? . 2_656 O(1) O(4) 3.58(1) ? . 2_656 O(1) O(5) 3.097(9) ? . . O(1) O(6) 3.09(1) ? . . O(1) O(6) 3.41(1) ? . 2_646 O(1) C(2) 2.35(2) ? . 2_646 O(1) C(3) 2.79(2) ? . 2_646 O(1) C(10) 2.96(1) ? . 2_656 O(1) C(11) 3.45(1) ? . 2_656 O(1) C(19) 3.42(1) ? . . O(1) H(1) 3.1862 ? . 2_646 O(1) H(2) 2.4405 ? . 2_646 O(1) H(8) 3.4394 ? . 2_656 O(1) H(13) 3.1626 ? . 1_554 O(2) O(1) 2.23(1) ? . 2_656 O(2) O(3) 2.81(1) ? . 2_656 O(2) O(4) 2.87(1) ? . . O(2) O(5) 3.22(1) ? . . O(2) O(6) 3.23(1) ? . . O(2) C(2) 2.35(2) ? . . O(2) C(3) 3.57(2) ? . . O(2) C(6) 3.48(1) ? . 2_546 O(2) C(16) 3.49(1) ? . 2_657 O(2) H(1) 2.5377 ? . . O(2) H(4) 3.0330 ? . 2_546 O(2) H(7) 3.0440 ? . 1_545 O(2) H(12) 2.7797 ? . 2_657 O(2) H(13) 3.0229 ? . 2_657 O(3) O(1) 2.80(1) ? . 2_646 O(3) O(2) 2.81(1) ? . 2_646 O(3) O(4) 2.19(1) ? . . O(3) O(5) 3.279(9) ? . . O(3) O(5) 3.24(1) ? . 2_646 O(3) O(6) 3.14(1) ? . . O(3) O(6) 3.269(9) ? . 2_646 O(3) C(1) 2.99(1) ? . 2_646 O(3) C(11) 2.40(1) ? . . O(3) C(12) 3.59(1) ? . . O(3) H(2) 3.3889 ? . 1_545 O(3) H(4) 3.1249 ? . 1_645 O(3) H(5) 3.5376 ? . 1_645 O(3) H(8) 2.6059 ? . . O(4) O(1) 3.58(1) ? . 2_646 O(4) O(5) 3.364(9) ? . . O(4) O(6) 3.00(1) ? . . O(4) C(3) 3.51(2) ? . 1_545 O(4) C(11) 2.39(1) ? . . O(4) C(12) 2.84(1) ? . . O(4) C(16) 3.32(1) ? . 2_657 O(4) C(17) 3.56(1) ? . 2_657 O(4) H(2) 2.6420 ? . 1_545 O(4) H(7) 3.0345 ? . 1_545 O(4) H(8) 3.2213 ? . . O(4) H(9) 2.4930 ? . . O(4) H(12) 2.9177 ? . 2_657 O(4) H(13) 3.3381 ? . 2_657 O(5) O(3) 3.24(1) ? . 2_656 O(5) O(6) 2.22(1) ? . 2_646 O(5) C(6) 3.45(1) ? . 2_546 O(5) C(20) 2.34(1) ? . . O(5) C(21) 3.56(1) ? . . O(5) H(2) 3.0664 ? . 1_545 O(5) H(3) 3.5689 ? . 2_546 O(5) H(4) 2.5827 ? . 2_546 O(5) H(8) 3.1372 ? . 2_656 O(5) H(15) 2.5374 ? . . O(6) O(1) 3.41(1) ? . 2_656 O(6) O(3) 3.269(9) ? . 2_656 O(6) O(5) 2.22(1) ? . 2_656 O(6) C(10) 3.12(1) ? . . O(6) C(20) 2.35(1) ? . 2_656 O(6) C(21) 2.83(1) ? . 2_656 O(6) H(2) 3.5429 ? . 2_646 O(6) H(5) 2.9164 ? . 1_645 O(6) H(13) 3.1153 ? . 2_657 O(6) H(15) 3.1764 ? . 2_656 O(6) H(16) 2.5023 ? . 2_656 C(1) Yb(1) 3.29(1) ? . 2_656 C(1) O(3) 2.99(1) ? . 2_656 C(1) C(3) 2.48(2) ? . . C(1) H(1) 2.1095 ? . . C(1) H(2) 2.5935 ? . . C(1) H(4) 3.4720 ? . 2_546 C(1) H(5) 3.5687 ? . 2_546 C(1) H(12) 3.2111 ? . 2_657 C(1) H(13) 3.0309 ? . 2_657 C(2) O(1) 2.35(2) ? . 2_656 C(2) C(4) 2.49(2) ? . . C(2) C(5) 3.04(2) ? . . C(2) C(7) 3.44(2) ? . 2_546 C(2) H(2) 1.9506 ? . . C(2) H(3) 2.7845 ? . . C(2) H(5) 3.4682 ? . 2_546 C(2) H(12) 3.4078 ? . 2_657 C(2) H(20) 3.3204 ? . 1_566 C(3) O(1) 2.79(2) ? . 2_656 C(3) O(4) 3.51(2) ? . 1_565 C(3) C(5) 2.51(2) ? . . C(3) C(9) 2.46(2) ? . . C(3) H(1) 1.9727 ? . . C(3) H(3) 2.6898 ? . . C(3) H(7) 2.6103 ? . . C(3) H(20) 3.1401 ? . 1_566 C(4) C(6) 2.43(1) ? . . C(4) C(7) 2.79(2) ? . . C(4) C(8) 2.42(2) ? . . C(4) H(1) 2.6838 ? . . C(4) H(2) 2.0505 ? . . C(4) H(3) 2.0326 ? . . C(4) H(4) 3.2857 ? . . C(4) H(6) 3.2707 ? . . C(4) H(7) 2.0475 ? . . C(4) H(19) 2.9594 ? . 1_566 C(4) H(20) 3.3071 ? . 1_566 C(5) C(7) 2.39(2) ? . . C(5) C(8) 2.75(2) ? . . C(5) C(9) 2.39(2) ? . . C(5) H(1) 2.7723 ? . . C(5) H(2) 3.3168 ? . . C(5) H(4) 2.0409 ? . . C(5) H(5) 3.2533 ? . . C(5) H(7) 3.2488 ? . . C(5) H(15) 3.2531 ? . 2_556 C(5) H(19) 2.9283 ? . 1_566 C(6) O(2) 3.48(1) ? . 2_556 C(6) O(5) 3.45(1) ? . 2_556 C(6) C(8) 2.39(2) ? . . C(6) C(9) 2.76(2) ? . . C(6) H(1) 3.4032 ? . 2_556 C(6) H(3) 2.0246 ? . . C(6) H(5) 2.0446 ? . . C(6) H(6) 3.2511 ? . . C(6) H(15) 3.1485 ? . 2_556 C(6) H(19) 3.0127 ? . 1_566 C(7) C(2) 3.44(2) ? . 2_556 C(7) C(9) 2.36(2) ? . . C(7) H(1) 3.4310 ? . 2_556 C(7) H(3) 3.2510 ? . . C(7) H(4) 2.0538 ? . . C(7) H(6) 2.0064 ? . . C(7) H(7) 3.2152 ? . . C(7) H(19) 3.0889 ? . 1_566 C(8) H(3) 3.4533 ? . 2_556 C(8) H(4) 3.2516 ? . . C(8) H(5) 2.0075 ? . . C(8) H(7) 2.0058 ? . . C(8) H(19) 3.1024 ? . 1_566 C(9) H(2) 2.5835 ? . . C(9) H(3) 3.2498 ? . . C(9) H(3) 3.3057 ? . 2_556 C(9) H(5) 3.2191 ? . . C(9) H(6) 2.0097 ? . . C(9) H(12) 3.3682 ? . 2_667 C(9) H(19) 3.0487 ? . 1_566 C(10) Yb(1) 3.323(9) ? . 2_646 C(10) O(1) 2.96(1) ? . 2_646 C(10) C(12) 2.44(1) ? . . C(10) H(2) 3.0008 ? . 1_545 C(10) H(8) 2.1156 ? . . C(10) H(9) 2.5500 ? . . C(11) O(1) 3.45(1) ? . 2_646 C(11) C(13) 2.50(1) ? . . C(11) C(14) 3.03(1) ? . . C(11) H(4) 3.5518 ? . 1_645 C(11) H(9) 1.9400 ? . . C(11) H(10) 2.7704 ? . . C(11) H(16) 3.3941 ? . 2_656 C(12) C(14) 2.50(1) ? . . C(12) C(18) 2.45(1) ? . . C(12) H(8) 1.9707 ? . . C(12) H(10) 2.6871 ? . . C(12) H(14) 2.6054 ? . . C(12) H(14) 3.5841 ? . 2_647 C(12) H(16) 3.2560 ? . 2_656 C(12) H(21) 3.3986 ? . 2_656 C(13) C(15) 2.40(2) ? . . C(13) C(16) 2.79(1) ? . . C(13) C(17) 2.41(1) ? . . C(13) H(8) 2.7017 ? . . C(13) H(9) 2.0667 ? . . C(13) H(10) 2.0296 ? . . C(13) H(11) 3.2567 ? . . C(13) H(13) 3.2662 ? . . C(13) H(14) 2.0366 ? . . C(13) H(14) 3.0579 ? . 2_647 C(13) H(21) 2.9519 ? . 2_656 C(14) C(16) 2.40(2) ? . . C(14) C(17) 2.74(2) ? . . C(14) C(18) 2.38(2) ? . . C(14) H(8) 2.7841 ? . . C(14) H(9) 3.3152 ? . . C(14) H(11) 2.0307 ? . . C(14) H(12) 3.2555 ? . . C(14) H(14) 3.2385 ? . . C(14) H(14) 2.9044 ? . 2_647 C(14) H(18) 3.3671 ? . 1_656 C(14) H(21) 3.3501 ? . 2_656 C(15) C(17) 2.34(2) ? . . C(15) C(18) 2.74(2) ? . . C(15) H(9) 3.2766 ? . 2_647 C(15) H(10) 2.0327 ? . . C(15) H(12) 2.0236 ? . . C(15) H(13) 3.1974 ? . . C(15) H(14) 3.3799 ? . 2_647 C(15) H(18) 3.2820 ? . 1_656 C(16) O(2) 3.49(1) ? . 2_647 C(16) O(4) 3.32(1) ? . 2_647 C(16) C(18) 2.39(2) ? . . C(16) H(7) 3.5261 ? . 2_637 C(16) H(9) 3.0266 ? . 2_647 C(16) H(10) 3.2498 ? . . C(16) H(11) 2.0162 ? . . C(16) H(13) 1.9863 ? . . C(16) H(14) 3.2357 ? . . C(16) H(20) 3.5045 ? . 2_656 C(17) O(4) 3.56(1) ? . 2_647 C(17) H(9) 3.1713 ? . 2_647 C(17) H(11) 3.1942 ? . . C(17) H(12) 1.9957 ? . . C(17) H(14) 2.0458 ? . . C(17) H(16) 3.3929 ? . 1_556 C(17) H(20) 3.5809 ? . 2_656 C(17) H(21) 3.4655 ? . 2_656 C(18) H(9) 2.5772 ? . . C(18) H(10) 3.2381 ? . . C(18) H(12) 3.2464 ? . . C(18) H(13) 2.0397 ? . . C(18) H(16) 3.4755 ? . 1_556 C(18) H(21) 3.2343 ? . 1_556 C(18) H(21) 3.0029 ? . 2_656 C(19) Yb(1) 3.313(9) ? . 2_646 C(19) C(21) 2.47(1) ? . . C(19) H(2) 3.4319 ? . 1_545 C(19) H(4) 3.3640 ? . 2_546 C(19) H(5) 3.0760 ? . 2_536 C(19) H(8) 3.2902 ? . 2_6560 C(19) H(13) 3.4073 ? . 1_554 C(19) H(15) 2.1022 ? . . C(19) H(16) 2.5923 ? . . C(20) O(6) 2.35(1) ? . 2_646 C(20) C(22) 2.49(1) ? . . C(20) C(23) 3.03(1) ? . . C(20) H(4) 3.2946 ? . 2_546 C(20) H(5) 2.9252 ? . 2_536 C(20) H(6) 3.3821 ? . 2_536 C(20) H(8) 3.1712 ? . 2_656 C(20) H(10) 3.3581 ? . 2_656 C(20) H(16) 1.9550 ? . . C(20) H(17) 2.7792 ? . . C(21) O(6) 2.83(1) ? . 2_646 C(21) C(23) 2.50(1) ? . . C(21) C(27) 2.44(2) ? . . C(21) H(5) 2.9220 ? . 2_536 C(21) H(10) 3.4256 ? . 2_656 C(21) H(13) 3.4868 ? . 1_554 C(21) H(14) 3.3279 ? . 1_554 C(21) H(15) 1.9762 ? . . C(21) H(17) 2.6752 ? . . C(21) H(21) 2.5907 ? . . C(22) C(24) 2.42(2) ? . . C(22) C(25) 2.80(2) ? . . C(22) C(26) 2.44(2) ? . . C(22) H(10) 3.3107 ? . 2_656 C(22) H(11) 3.4151 ? . 2_656 C(22) H(14) 3.4952 ? . 1_554 C(22) H(15) 2.6840 ? . . C(22) H(16) 2.0529 ? . . C(22) H(17) 2.0371 ? . . C(22) H(18) 3.2757 ? . . C(22) H(18) 3.3028 ? . 2_545 C(22) H(20) 3.2898 ? . . C(22) H(21) 2.0200 ? . . C(23) C(25) 2.39(2) ? . . C(23) C(26) 2.76(2) ? . . C(23) C(27) 2.37(2) ? . . C(23) H(10) 3.3910 ? . 2_656 C(23) H(11) 3.1685 ? . 2_656 C(23) H(15) 2.7638 ? . . C(23) H(16) 3.3011 ? . . C(23) H(18) 2.0314 ? . . C(23) H(18) 3.5174 ? . 2_545 C(23) H(19) 3.2461 ? . . C(23) H(21) 3.2336 ? . . C(24) C(26) 2.37(2) ? . . C(24) C(27) 2.75(2) ? . . C(24) H(11) 3.3330 ? . 1_454 C(24) H(11) 2.9658 ? . 2_656 C(24) H(17) 2.0256 ? . . C(24) H(18) 3.5378 ? . 2_545 C(24) H(19) 2.0222 ? . . C(24) H(20) 3.2334 ? . . C(25) C(27) 2.40(2) ? . . C(25) H(11) 3.0329 ? . 2_656 C(25) H(17) 3.2425 ? . . C(25) H(17) 3.2628 ? . 2_545 C(25) H(18) 2.0243 ? . . C(25) H(18) 3.3088 ? . 2_545 C(25) H(20) 2.0133 ? . . C(25) H(21) 3.2495 ? . . C(26) H(11) 3.2869 ? . 2_656 C(26) H(17) 3.4333 ? . 2_545 C(26) H(18) 3.2284 ? . . C(26) H(18) 3.0398 ? . 2_545 C(26) H(19) 2.0070 ? . . C(26) H(21) 2.0607 ? . . C(27) H(11) 3.4649 ? . 2_656 C(27) H(14) 3.2819 ? . 1_554 C(27) H(16) 2.5878 ? . . C(27) H(17) 3.2304 ? . . C(27) H(18) 3.0217 ? . 2_545 C(27) H(19) 3.2608 ? . . C(27) H(20) 2.0705 ? . . H(1) O(1) 3.1862 ? . 2_656 H(1) C(6) 3.4032 ? . 2_546 H(1) C(7) 3.4310 ? . 2_546 H(2) O(1) 2.4405 ? . 2_656 H(2) O(3) 3.3889 ? . 1_565 H(2) O(4) 2.6420 ? . 1_565 H(2) O(5) 3.0664 ? . 1_565 H(2) O(6) 3.5429 ? . 2_656 H(2) C(10) 3.0008 ? . 1_565 H(2) C(19) 3.4319 ? . 1_565 H(3) O(5) 3.5689 ? . 2_556 H(3) C(8) 3.4533 ? . 2_546 H(3) C(9) 3.3057 ? . 2_546 H(4) O(2) 3.0330 ? . 2_556 H(4) O(3) 3.1249 ? . 1_465 H(4) O(5) 2.5827 ? . 2_556 H(4) C(1) 3.4720 ? . 2_556 H(4) C(11) 3.5518 ? . 1_465 H(4) C(19) 3.3640 ? . 2_556 H(4) C(20) 3.2946 ? . 2_556 H(5) O(3) 3.5376 ? . 1_465 H(5) O(6) 2.9164 ? . 1_465 H(5) C(1) 3.5687 ? . 2_556 H(5) C(2) 3.4682 ? . 2_556 H(5) C(19) 3.0760 ? . 2_566 H(5) C(20) 2.9252 ? . 2_566 H(5) C(21) 2.9220 ? . 2_566 H(6) C(20) 3.3821 ? . 2_566 H(7) O(2) 3.0440 ? . 1_565 H(7) O(4) 3.0345 ? . 1_565 H(7) C(16) 3.5261 ? . 2_667 H(8) O(1) 3.4394 ? . 2_646 H(8) O(5) 3.1372 ? . 2_646 H(8) C(19) 3.2902 ? . 2_646 H(8) C(20) 3.1712 ? . 2_646 H(9) C(15) 3.2766 ? . 2_657 H(9) C(16) 3.0266 ? . 2_657 H(9) C(17) 3.1713 ? . 2_657 H(10) C(20) 3.3581 ? . 2_646 H(10) C(21) 3.4256 ? . 2_646 H(10) C(22) 3.3107 ? . 2_646 H(10) C(23) 3.3910 ? . 2_646 H(11) C(22) 3.4151 ? . 2_646 H(11) C(23) 3.1685 ? . 2_646 H(11) C(24) 3.3330 ? . 1_656 H(11) C(24) 2.9658 ? . 2_646 H(11) C(25) 3.0329 ? . 2_646 H(11) C(26) 3.2869 ? . 2_646 H(11) C(27) 3.4649 ? . 2_646 H(12) O(2) 2.7797 ? . 2_647 H(12) O(4) 2.9177 ? . 2_647 H(12) C(1) 3.2111 ? . 2_647 H(12) C(2) 3.4078 ? . 2_647 H(12) C(9) 3.3682 ? . 2_637 H(13) O(1) 3.1626 ? . 1_556 H(13) O(2) 3.0229 ? . 2_647 H(13) O(4) 3.3381 ? . 2_647 H(13) O(6) 3.1153 ? . 2_647 H(13) C(1) 3.0309 ? . 2_647 H(13) C(19) 3.4073 ? . 1_556 H(13) C(21) 3.4868 ? . 1_556 H(14) C(12) 3.5841 ? . 2_657 H(14) C(13) 3.0579 ? . 2_657 H(14) C(14) 2.9044 ? . 2_657 H(14) C(15) 3.3799 ? . 2_657 H(14) C(21) 3.3279 ? . 1_556 H(14) C(22) 3.4952 ? . 1_556 H(14) C(27) 3.2819 ? . 1_556 H(15) O(6) 3.1764 ? . 2_646 H(15) C(5) 3.2531 ? . 2_546 H(15) C(6) 3.1485 ? . 2_546 H(16) O(6) 2.5023 ? . 2_646 H(16) C(11) 3.3941 ? . 2_646 H(16) C(12) 3.2560 ? . 2_646 H(16) C(17) 3.3929 ? . 1_554 H(16) C(18) 3.4755 ? . 1_554 H(17) C(25) 3.2628 ? . 2_555 H(17) C(26) 3.4333 ? . 2_555 H(18) C(14) 3.3671 ? . 1_454 H(18) C(15) 3.2820 ? . 1_454 H(18) C(22) 3.3028 ? . 2_555 H(18) C(23) 3.5174 ? . 2_555 H(18) C(24) 3.5378 ? . 2_555 H(18) C(25) 3.3088 ? . 2_555 H(18) C(26) 3.0398 ? . 2_555 H(18) C(27) 3.0217 ? . 2_555 H(19) C(4) 2.9594 ? . 1_544 H(19) C(5) 2.9283 ? . 1_544 H(19) C(6) 3.0127 ? . 1_544 H(19) C(7) 3.0889 ? . 1_544 H(19) C(8) 3.1024 ? . 1_544 H(19) C(9) 3.0487 ? . 1_544 H(20) C(2) 3.3204 ? . 1_544 H(20) C(3) 3.1401 ? . 1_544 H(20) C(4) 3.3071 ? . 1_544 H(20) C(16) 3.5045 ? . 2_646 H(20) C(17) 3.5809 ? . 2_646 H(21) C(12) 3.3986 ? . 2_646 H(21) C(13) 2.9519 ? . 2_646 H(21) C(14) 3.3501 ? . 2_646 H(21) C(17) 3.4655 ? . 2_646 H(21) C(18) 3.2343 ? . 1_554 H(21) C(18) 3.0029 ? . 2_646 H(21) C(21) 2.5907 ? . . H(21) C(22) 2.0200 ? . . H(21) C(23) 3.2336 ? . . H(21) C(25) 3.2495 ? . . H(21) C(26) 2.0607 ? . . Yb(1) Yb(1) 4.083(3) ? . 2_656 Yb(1) Yb(1) 4.083(3) ? 2_646 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(3) H(2) O(1) 2_656 0.94 2.44 2.78(2) 101 ? C(6) H(4) O(5) 2_556 0.95 2.58 3.448(15) 152 ? C(12) H(9) O(4) . 0.95 2.49 2.839(12) 101 ? C(21) H(16) O(6) 2_646 0.95 2.50 2.826(13) 100 ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Y-wt1270w.cif' #============================================================================== data_wt1270w _database_code_depnum_ccdc_archive 'CCDC 631230' #Kin-K361Y-cinnamate #============================================================================== _audit_creation_date 2006-07-03 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 O6 Y ' _chemical_formula_moiety 'C27 H21 O6 Y ' _chemical_formula_weight 530.37 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.5429(10) _cell_length_b 7.9186(7) _cell_length_c 13.0625(11) _cell_angle_alpha 90 _cell_angle_beta 94.139(2) _cell_angle_gamma 90 _cell_volume 1190.8(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7456 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540.00 _exptl_absorpt_coefficient_mu 2.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7456 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.9680 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.9680 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0\s(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0\s(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2840 _reflns_number_gt 2450 _reflns_threshold_expression I>2.0\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0280 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2460 _refine_ls_number_parameters 330 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 1.0000\s(Fo^2^) + 0.005]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.38 _refine_diff_density_min -0.25 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 14.8(42) _refine_ls_abs_structure_details 'Flack (1983). 2840 Friedel Pairs' _refine_ls_abs_structure_Flack 0.131(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Y Y -2.796 3.567 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Y(1) Y 0.46007(3) 0.54206(11) 0.52409(3) 0.02531(8) Uani 1.00 1 d . . . O(1) O 0.5949(3) 0.4678(4) 0.4167(2) 0.0393(9) Uani 1.00 1 d . . . O(2) O 0.3235(3) 0.7152(4) 0.5838(2) 0.0374(9) Uani 1.00 1 d . . . O(3) O 0.5405(3) 0.2688(4) 0.5885(2) 0.0340(8) Uani 1.00 1 d . . . O(4) O 0.4162(3) 0.4032(4) 0.6772(2) 0.0379(9) Uani 1.00 1 d . . . O(5) O 0.3306(3) 0.4017(4) 0.4208(2) 0.0407(9) Uani 1.00 1 d . . . O(6) O 0.6026(3) 0.6544(4) 0.6296(2) 0.0417(9) Uani 1.00 1 d . . . C(1) C 0.3177(4) 0.8736(6) 0.5888(3) 0.0347(13) Uani 1.00 1 d . . . C(2) C 0.2047(5) 0.9499(8) 0.6042(4) 0.036(2) Uani 1.00 1 d . . . C(3) C 0.1877(6) 1.1155(8) 0.6086(5) 0.041(2) Uani 1.00 1 d . . . C(4) C 0.0801(4) 1.2065(6) 0.6216(4) 0.039(1) Uani 1.00 1 d . . . C(5) C -0.0281(4) 1.1294(7) 0.6161(4) 0.044(1) Uani 1.00 1 d . . . C(6) C -0.1277(4) 1.2177(8) 0.6325(4) 0.051(2) Uani 1.00 1 d . . . C(7) C -0.1203(5) 1.3894(7) 0.6535(4) 0.057(2) Uani 1.00 1 d . . . C(8) C -0.0153(5) 1.4689(7) 0.6564(4) 0.065(2) Uani 1.00 1 d . . . C(9) C 0.0843(5) 1.3812(7) 0.6396(4) 0.054(2) Uani 1.00 1 d . . . C(10) C 0.4971(4) 0.3001(5) 0.6746(3) 0.0299(11) Uani 1.00 1 d . . . C(11) C 0.5528(4) 0.2250(6) 0.7688(3) 0.0393(13) Uani 1.00 1 d . . . C(12) C 0.5266(4) 0.2746(6) 0.8609(3) 0.0379(13) Uani 1.00 1 d . . . C(13) C 0.5847(4) 0.2276(6) 0.9605(3) 0.0375(13) Uani 1.00 1 d . . . C(14) C 0.6877(4) 0.1375(7) 0.9707(4) 0.047(2) Uani 1.00 1 d . . . C(15) C 0.7414(5) 0.1030(7) 1.0656(4) 0.055(2) Uani 1.00 1 d . . . C(16) C 0.6932(5) 0.1582(7) 1.1534(4) 0.055(2) Uani 1.00 1 d . . . C(17) C 0.5915(5) 0.2477(8) 1.1446(4) 0.058(2) Uani 1.00 1 d . . . C(18) C 0.5372(4) 0.2832(7) 1.0486(3) 0.046(2) Uani 1.00 1 d . . . C(19) C 0.3319(4) 0.2807(6) 0.3579(3) 0.0334(12) Uani 1.00 1 d . . . C(20) C 0.2533(4) 0.2916(6) 0.2638(3) 0.0363(13) Uani 1.00 1 d . . . C(21) C 0.2621(4) 0.1925(6) 0.1835(3) 0.0362(12) Uani 1.00 1 d . . . C(22) C 0.1898(4) 0.1986(6) 0.0859(3) 0.0371(13) Uani 1.00 1 d . . . C(23) C 0.0831(4) 0.2783(7) 0.0764(4) 0.049(2) Uani 1.00 1 d . . . C(24) C 0.0188(5) 0.2823(11) -0.0166(5) 0.058(2) Uani 1.00 1 d . . . C(25) C 0.0591(5) 0.2063(8) -0.1011(4) 0.064(2) Uani 1.00 1 d . . . C(26) C 0.1644(5) 0.1234(8) -0.0932(4) 0.064(2) Uani 1.00 1 d . . . C(27) C 0.2296(5) 0.1194(7) 0.0001(4) 0.052(2) Uani 1.00 1 d . . . H(1) H 0.1402 0.8772 0.6113 0.043 Uiso 1.00 1 c R . . H(2) H 0.2547 1.1836 0.6026 0.049 Uiso 1.00 1 c R . . H(3) H -0.0336 1.0124 0.6006 0.052 Uiso 1.00 1 c R . . H(4) H -0.2007 1.1618 0.6295 0.061 Uiso 1.00 1 c R . . H(5) H -0.1883 1.4514 0.6659 0.069 Uiso 1.00 1 c R . . H(6) H -0.0110 1.5866 0.6702 0.078 Uiso 1.00 1 c R . . H(7) H 0.1564 1.4391 0.6403 0.065 Uiso 1.00 1 c R . . H(8) H 0.6092 0.1386 0.7632 0.047 Uiso 1.00 1 c R . . H(9) H 0.4625 0.3496 0.8629 0.045 Uiso 1.00 1 c R . . H(10) H 0.7219 0.0989 0.9109 0.057 Uiso 1.00 1 c R . . H(11) H 0.8121 0.0410 1.0709 0.066 Uiso 1.00 1 c R . . H(12) H 0.7302 0.1343 1.2191 0.066 Uiso 1.00 1 c R . . H(13) H 0.5577 0.2859 1.2046 0.069 Uiso 1.00 1 c R . . H(14) H 0.4670 0.3461 1.0435 0.055 Uiso 1.00 1 c R . . H(15) H 0.1934 0.3742 0.2609 0.044 Uiso 1.00 1 c R . . H(16) H 0.3210 0.1086 0.1892 0.043 Uiso 1.00 1 c R . . H(17) H 0.0538 0.3308 0.1346 0.059 Uiso 1.00 1 c R . . H(18) H -0.0541 0.3384 -0.0221 0.069 Uiso 1.00 1 c R . . H(19) H 0.0147 0.2106 -0.1651 0.077 Uiso 1.00 1 c R . . H(20) H 0.1921 0.0691 -0.1515 0.076 Uiso 1.00 1 c R . . H(21) H 0.3021 0.0621 0.0056 0.062 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Y(1) 0.0301(2) 0.0211(2) 0.0243(2) -0.0007(3) -0.00071(12) -0.0006(3) O(1) 0.037(2) 0.043(2) 0.039(2) 0.003(2) 0.010(1) 0.005(2) O(2) 0.041(2) 0.030(2) 0.042(2) 0.005(2) 0.008(2) -0.000(2) O(3) 0.047(2) 0.026(2) 0.029(2) -0.000(2) -0.0004(13) -0.0011(13) O(4) 0.046(2) 0.037(2) 0.031(2) 0.006(2) 0.003(1) 0.004(2) O(5) 0.044(2) 0.039(2) 0.038(2) -0.003(2) -0.008(1) -0.005(2) O(6) 0.043(2) 0.038(2) 0.042(2) -0.005(2) -0.011(2) 0.001(2) C(1) 0.043(3) 0.036(3) 0.025(2) 0.003(2) 0.003(2) -0.002(2) C(2) 0.031(3) 0.032(3) 0.044(4) -0.004(3) 0.009(3) 0.001(3) C(3) 0.038(3) 0.040(3) 0.045(4) -0.005(3) 0.002(3) -0.000(3) C(4) 0.045(3) 0.034(3) 0.040(3) 0.004(2) 0.006(2) -0.004(2) C(5) 0.047(3) 0.036(3) 0.048(3) 0.005(3) 0.001(2) -0.005(2) C(6) 0.038(3) 0.061(4) 0.054(3) 0.008(3) -0.003(2) -0.001(3) C(7) 0.046(3) 0.056(4) 0.069(4) 0.022(3) 0.000(3) -0.004(3) C(8) 0.073(4) 0.035(3) 0.086(4) 0.015(3) 0.007(4) -0.008(3) C(9) 0.053(3) 0.038(3) 0.073(4) -0.006(3) 0.008(3) -0.011(3) C(10) 0.039(3) 0.023(2) 0.027(2) -0.003(2) 0.001(2) -0.001(2) C(11) 0.053(3) 0.031(3) 0.033(2) 0.009(2) -0.000(2) 0.004(2) C(12) 0.047(3) 0.036(3) 0.030(2) 0.001(2) 0.001(2) -0.000(2) C(13) 0.047(3) 0.035(3) 0.030(2) 0.000(2) -0.001(2) 0.002(2) C(14) 0.056(3) 0.049(3) 0.036(3) 0.009(3) 0.001(2) -0.003(2) C(15) 0.054(3) 0.061(4) 0.049(3) 0.009(3) -0.007(3) 0.011(3) C(16) 0.067(4) 0.064(4) 0.033(3) -0.004(3) -0.010(3) 0.013(3) C(17) 0.068(4) 0.076(4) 0.030(3) -0.004(4) 0.009(2) -0.000(3) C(18) 0.052(3) 0.053(3) 0.034(3) 0.010(3) 0.006(2) 0.003(3) C(19) 0.032(3) 0.033(3) 0.035(2) -0.007(2) -0.003(2) 0.004(2) C(20) 0.036(3) 0.034(3) 0.037(3) 0.005(2) -0.009(2) 0.000(2) C(21) 0.036(3) 0.036(3) 0.035(2) 0.003(2) -0.004(2) 0.001(2) C(22) 0.040(3) 0.037(3) 0.034(2) -0.004(2) -0.005(2) 0.003(2) C(23) 0.050(3) 0.058(3) 0.037(3) 0.006(3) -0.008(2) -0.002(3) C(24) 0.049(4) 0.065(4) 0.056(4) 0.003(3) -0.018(3) 0.006(4) C(25) 0.074(4) 0.074(4) 0.041(3) -0.007(4) -0.022(3) 0.002(3) C(26) 0.088(5) 0.067(4) 0.035(3) -0.007(4) 0.001(3) -0.014(3) C(27) 0.059(3) 0.052(3) 0.044(3) 0.004(3) -0.003(3) -0.009(3) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Y(1) O(1) 2.247(3) ? . . Y(1) O(2) 2.270(3) ? . . Y(1) O(3) 2.478(3) ? . . Y(1) O(3) 2.320(3) ? . 2_656 Y(1) O(4) 2.369(3) ? . . Y(1) O(5) 2.236(3) ? . . Y(1) O(6) 2.251(3) ? . . O(1) C(1) 1.260(6) ? . 2_646 O(2) C(1) 1.258(6) ? . . O(3) Y(1) 2.320(3) ? . 2_646 O(3) C(10) 1.288(5) ? . . O(4) C(10) 1.243(5) ? . . O(5) C(19) 1.263(6) ? . . O(6) C(19) 1.257(6) ? . 2_656 C(1) O(1) 1.260(6) ? . 2_656 C(1) C(2) 1.465(8) ? . . C(2) C(3) 1.328(9) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.457(8) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.388(7) ? . . C(4) C(9) 1.403(7) ? . . C(5) C(6) 1.375(7) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.388(8) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.364(8) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.375(8) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . C(10) C(11) 1.471(6) ? . . C(11) C(12) 1.322(6) ? . . C(11) H(8) 0.9500 ? . . C(12) C(13) 1.467(6) ? . . C(12) H(9) 0.9500 ? . . C(13) C(14) 1.385(7) ? . . C(13) C(18) 1.382(6) ? . . C(14) C(15) 1.373(7) ? . . C(14) H(10) 0.9500 ? . . C(15) C(16) 1.381(7) ? . . C(15) H(11) 0.9500 ? . . C(16) C(17) 1.370(8) ? . . C(16) H(12) 0.9500 ? . . C(17) C(18) 1.389(6) ? . . C(17) H(13) 0.9500 ? . . C(18) H(14) 0.9500 ? . . C(19) O(6) 1.257(6) ? . 2_646 C(19) C(20) 1.477(6) ? . . C(20) C(21) 1.320(6) ? . . C(20) H(15) 0.9500 ? . . C(21) C(22) 1.473(6) ? . . C(21) H(16) 0.9500 ? . . C(22) C(23) 1.381(7) ? . . C(22) C(27) 1.391(7) ? . . C(23) C(24) 1.378(7) ? . . C(23) H(17) 0.9500 ? . . C(24) C(25) 1.368(9) ? . . C(24) H(18) 0.9500 ? . . C(25) C(26) 1.378(9) ? . . C(25) H(19) 0.9500 ? . . C(26) C(27) 1.386(7) ? . . C(26) H(20) 0.9500 ? . . C(27) C(22) 1.391(7) ? . . C(27) C(26) 1.386(7) ? . . C(27) H(21) 0.9500 ? . . H(21) C(27) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Y(1) O(1) 154.4(1) ? . . . O(3) Y(1) O(1) 74.0(1) ? . . . O(3) Y(1) O(1) 77.1(1) ? 2_656 . . O(4) Y(1) O(1) 127.3(1) ? . . . O(5) Y(1) O(1) 87.5(1) ? . . . O(6) Y(1) O(1) 88.7(1) ? . . . Y(1) O(1) C(1) 141.5(3) ? . . 2_646 O(3) Y(1) O(2) 131.6(1) ? . . . O(3) Y(1) O(2) 77.3(1) ? 2_656 . . O(4) Y(1) O(2) 78.1(1) ? . . . O(5) Y(1) O(2) 93.3(1) ? . . . O(6) Y(1) O(2) 92.6(1) ? . . . Y(1) O(2) C(1) 131.3(3) ? . . . O(3) Y(1) O(3) 151.0(1) ? 2_65602 . . O(4) Y(1) O(3) 53.5(1) ? . . . O(5) Y(1) O(3) 89.3(1) ? . . . O(6) Y(1) O(3) 84.1(1) ? . . . Y(1) O(3) C(10) 88.2(2) ? . . . Y(1) O(3) Y(1) 118.5(1) ? . . 2_646 O(4) Y(1) O(3) 154.6(1) ? . . 2_656 O(5) Y(1) O(3) 91.8(1) ? . . 2_656 O(6) Y(1) O(3) 92.9(1) ? . . 2_656 Y(1) O(3) C(10) 136.0(3) ? . 2_656 2_656 Y(1) O(3) Y(1) 118.5(1) ? . 2_656 2_656 O(5) Y(1) O(4) 96.0(1) ? . . . O(6) Y(1) O(4) 81.9(1) ? . . . Y(1) O(4) C(10) 94.3(2) ? . . . O(6) Y(1) O(5) 173.1(1) ? . . . Y(1) O(5) C(19) 137.0(3) ? . . . Y(1) O(6) C(19) 143.1(3) ? . . 2_656 O(1) C(1) O(2) 122.8(4) ? . 2_646 2_646 O(1) C(1) C(2) 119.2(4) ? . 2_646 2_646 O(2) C(1) O(1) 122.8(4) ? . . 2_656 O(2) C(1) C(2) 117.9(4) ? . . . C(10) O(3) Y(1) 136.0(3) ? . . 2_646 O(3) Y(1) O(2) 77.3(1) ? . 2_646 2_646 O(3) Y(1) O(6) 92.9(1) ? . 2_646 2_646 O(3) Y(1) O(1) 77.1(1) ? . 2_646 2_646 O(3) Y(1) O(5) 91.8(1) ? . 2_646 2_646 O(3) C(10) O(4) 119.3(4) ? . . . O(3) C(10) C(11) 118.6(4) ? . . . O(4) C(10) C(11) 121.8(4) ? . . . O(5) C(19) O(6) 123.6(4) ? . . 2_646 O(5) C(19) C(20) 117.5(4) ? . . . O(6) C(19) O(5) 123.6(4) ? . 2_656 2_656 O(6) C(19) C(20) 118.9(4) ? . 2_656 2_656 C(2) C(1) O(1) 119.2(4) ? . . 2_656 C(1) O(1) Y(1) 141.5(3) ? . 2_656 2_656 C(1) C(2) C(3) 123.2(5) ? . . . C(1) C(2) H(1) 118.3768 ? . . . H(1) C(2) C(3) 118.3766 ? . . . C(2) C(3) H(2) 115.7261 ? . . . C(2) C(3) C(4) 128.5(6) ? . . . H(2) C(3) C(4) 115.7262 ? . . . C(3) C(4) C(5) 123.3(5) ? . . . C(3) C(4) C(9) 119.2(5) ? . . . C(4) C(5) H(3) 119.0606 ? . . . C(9) C(4) C(5) 117.5(5) ? . . . C(4) C(5) C(6) 121.9(5) ? . . . C(4) C(9) H(7) 119.8223 ? . . . C(4) C(9) C(8) 120.4(5) ? . . . H(3) C(5) C(6) 119.0609 ? . . . C(5) C(6) C(7) 119.2(5) ? . . . C(5) C(6) H(4) 120.4001 ? . . . C(6) C(7) C(8) 120.0(5) ? . . . H(4) C(6) C(7) 120.3999 ? . . . C(6) C(7) H(5) 120.0057 ? . . . C(7) C(8) C(9) 121.0(5) ? . . . C(7) C(8) H(6) 119.5243 ? . . . H(5) C(7) C(8) 120.0059 ? . . . C(8) C(9) H(7) 119.8223 ? . . . H(6) C(8) C(9) 119.5237 ? . . . C(10) C(11) C(12) 121.7(4) ? . . . C(10) C(11) H(8) 119.1440 ? . . . H(8) C(11) C(12) 119.1443 ? . . . C(11) C(12) H(9) 116.1483 ? . . . C(11) C(12) C(13) 127.7(4) ? . . . H(9) C(12) C(13) 116.1480 ? . . . C(12) C(13) C(14) 123.4(4) ? . . . C(12) C(13) C(18) 118.3(4) ? . . . C(13) C(14) H(10) 119.3888 ? . . . C(18) C(13) C(14) 118.2(4) ? . . . C(13) C(14) C(15) 121.2(5) ? . . . C(13) C(18) H(14) 119.7444 ? . . . C(13) C(18) C(17) 120.5(5) ? . . . H(10) C(14) C(15) 119.3893 ? . . . C(14) C(15) C(16) 120.3(5) ? . . . C(14) C(15) H(11) 119.8727 ? . . . C(15) C(16) C(17) 119.3(5) ? . . . H(11) C(15) C(16) 119.8723 ? . . . C(15) C(16) H(12) 120.3705 ? . . . C(16) C(17) C(18) 120.5(5) ? . . . C(16) C(17) H(13) 119.7391 ? . . . H(12) C(16) C(17) 120.3706 ? . . . C(17) C(18) H(14) 119.7449 ? . . . H(13) C(17) C(18) 119.7385 ? . . . C(19) O(6) Y(1) 143.1(3) ? . 2_646 2_646 C(20) C(19) O(6) 118.9(4) ? . . 2_646 C(19) C(20) C(21) 123.3(4) ? . . . C(19) C(20) H(15) 118.3563 ? . . . H(15) C(20) C(21) 118.3556 ? . . . C(20) C(21) H(16) 116.6769 ? . . . C(20) C(21) C(22) 126.6(4) ? . . . H(16) C(21) C(22) 116.6777 ? . . . C(21) C(22) C(23) 122.6(4) ? . . . C(21) C(22) C(27) 118.9(4) ? . . . C(22) C(23) H(17) 119.6709 ? . . . C(27) C(22) C(23) 118.6(4) ? . . . C(22) C(23) C(24) 120.7(5) ? . . . C(22) C(27) H(21) 119.7438 ? . . . C(22) C(27) C(26) 120.5(5) ? . . . H(17) C(23) C(24) 119.6706 ? . . . C(23) C(24) C(25) 120.5(6) ? . . . C(23) C(24) H(18) 119.7267 ? . . . C(24) C(25) C(26) 119.9(5) ? . . . H(18) C(24) C(25) 119.7268 ? . . . C(24) C(25) H(19) 120.0428 ? . . . C(25) C(26) C(27) 119.8(5) ? . . . C(25) C(26) H(20) 120.1045 ? . . . H(19) C(25) C(26) 120.0428 ? . . . C(26) C(27) H(21) 119.7434 ? . . . H(20) C(26) C(27) 120.1040 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Y(1) O(1) 3.527(3) ? . 2_656 Y(1) C(1) 3.241(5) ? . . Y(1) C(1) 3.328(5) ? . 2_646 Y(1) C(10) 2.757(4) ? . . Y(1) C(10) 3.368(4) ? . 2_656 Y(1) C(19) 3.275(4) ? . . Y(1) C(19) 3.344(4) ? . 2_656 O(1) Y(1) 3.527(3) ? . 2_646 O(1) O(2) 2.211(4) ? . 2_646 O(1) O(3) 2.849(4) ? . . O(1) O(3) 2.848(4) ? . 2_656 O(1) O(5) 3.100(4) ? . . O(1) O(6) 3.144(4) ? . . O(1) O(6) 3.395(4) ? . 2_646 O(1) C(2) 2.354(7) ? . 2_646 O(1) C(3) 2.809(7) ? . 2_646 O(1) C(10) 3.048(5) ? . 2_656 O(1) C(11) 3.511(5) ? . 2_656 O(1) C(19) 3.415(5) ? . . O(1) H(1) 3.1871 ? . 2_646 O(1) H(2) 2.4621 ? . 2_646 O(1) H(8) 3.4782 ? . 2_656 O(1) H(13) 3.1243 ? . 1_554 O(2) O(1) 2.211(4) ? . 2_656 O(2) O(3) 2.867(4) ? . 2_656 O(2) O(4) 2.924(4) ? . . O(2) O(5) 3.276(4) ? . . O(2) O(6) 3.270(4) ? . . O(2) C(2) 2.336(7) ? . . O(2) C(3) 3.561(7) ? . . O(2) C(6) 3.488(6) ? . 2_546 O(2) C(16) 3.482(6) ? . 2_657 O(2) H(1) 2.5214 ? . . O(2) H(4) 3.0623 ? . 2_546 O(2) H(7) 3.0408 ? . 1_545 O(2) H(12) 2.7665 ? .2_ 657 O(2) H(13) 3.0471 ? . 2_657 O(3) O(1) 2.848(4) ? . 2_646 O(3) O(2) 2.867(4) ? . 2_646 O(3) O(4) 2.185(4) ? . . O(3) O(5) 3.318(4) ? . . O(3) O(5) 3.272(4) ? . 2_646 O(3) O(6) 3.174(4) ? . . O(3) O(6) 3.314(4) ? . 2_646 O(3) C(1) 3.046(5) ? . 2_646 O(3) C(11) 2.374(5) ? . . O(3) C(12) 3.574(5) ? . . O(3) H(2) 3.3856 ? . 1_545 O(3) H(4) 3.1135 ? . 1_645 O(3) H(5) 3.5292 ? . 1_645 O(3) H(8) 2.5758 ? . . O(4) O(5) 3.423(4) ? . . O(4) O(6) 3.028(5) ? . . O(4) C(3) 3.550(7) ? . 1_545 O(4) C(11) 2.374(5) ? . . O(4) C(12) 2.825(5) ? . . O(4) C(16) 3.313(6) ? . 2_657 O(4) C(17) 3.592(7) ? . 2_657 O(4) H(2) 2.6808 ? . 1_545 O(4) H(7) 3.0155 ? . 1_545 O(4) H(8) 3.2015 ? . . O(4) H(9) 2.4828 ? . . O(4) H(12) 2.8932 ? . 2_657 O(4) H(13) 3.4048 ? . 2_657 O(5) O(3) 3.272(4) ? . 2_656 O(5) O(6) 2.221(5) ? . 2_646 O(5) C(6) 3.463(6) ? . 2_546 O(5) C(20) 2.344(5) ? . . O(5) C(21) 3.553(5) ? . . O(5) H(2) 3.1132 ? . 1_545 O(5) H(3) 3.5299 ? . 2_546 O(5) H(4) 2.6038 ? . 2_546 O(5) H(8) 3.1653 ? . 2_656 O(5) H(15) 2.5374 ? . . O(6) O(1) 3.395(4) ? . 2_656 O(6) O(3) 3.314(4) ? . 2_656 O(6) O(5) 2.221(5) ? . 2_656 O(6) C(10) 3.131(5) ? . . O(6) C(20) 2.357(5) ? . 2_656 O(6) C(21) 2.819(5) ? . 2_656 O(6) H(2) 3.5615 ? . 2_646 O(6) H(5) 2.9096 ? . 1_645 O(6) H(13) 3.1271 ? . 2_657 O(6) H(15) 3.1833 ? . 2_656 O(6) H(16) 2.4925 ? . 2_656 C(1) Y(1) 3.328(5) ? . 2_656 C(1) O(3) 3.046(5) ? . 2_656 C(1) C(3) 2.458(8) ? . . C(1) H(1) 2.0912 ? . . C(1) H(2) 2.5703 ? . . C(1) H(4) 3.4939 ? . 2_546 C(1) H(5) 3.5995 ? . 2_546 C(1) H(12) 3.2247 ? . 2_657 C(1) H(13) 3.0452 ? . 2_657 C(2) O(1) 2.354(7) ? . 2_656 C(2) C(4) 2.509(8) ? . . C(2) C(5) 3.054(8) ? . . C(2) C(7) 3.469(8) ? . 2_546 C(2) H(2) 1.9391 ? . . C(2) H(3) 2.7913 ? . . C(2) H(5) 3.5189 ? . 2_546 C(2) H(12) 3.4481 ? . 2_657 C(2) H(20) 3.3415 ? . 1_566 C(3) O(1) 2.809(7) ? . 2_656 C(3) O(4) 3.550(7) ? . 1_565 C(3) C(5) 2.503(8) ? . . C(3) C(9) 2.467(8) ? . . C(3) H(1) 1.9657 ? . . C(3) H(3) 2.6769 ? . . C(3) H(7) 2.6252 ? . . C(3) H(20) 3.1516 ? . 1_566 C(4) C(6) 2.415(7) ? . . C(4) C(7) 2.786(7) ? . . C(4) C(8) 2.410(8) ? . . C(4) H(1) 2.7042 ? . . C(4) H(2) 2.0558 ? . . C(4) H(3) 2.0270 ? . . C(4) H(4) 3.2701 ? . . C(4) H(6) 3.2656 ? . . C(4) H(7) 2.0490 ? . . C(4) H(19) 2.9394 ? . 1_566 C(4) H(20) 3.3299 ? . 1_566 C(5) C(7) 2.384(8) ? . . C(5) C(8) 2.741(8) ? . . C(5) C(9) 2.387(7) ? . . C(5) H(1) 2.7907 ? . . C(5) H(2) 3.3096 ? . . C(5) H(4) 2.0289 ? . . C(5) H(5) 3.2429 ? . . C(5) H(7) 3.2490 ? . . C(5) H(15) 3.2788 ? . 2_556 C(5) H(19) 2.9364 ? . 1_566 C(6) O(2) 3.488(6) ? . 2_556 C(6) O(5) 3.463(6) ? . 2_556 C(6) C(8) 2.383(8) ? . . C(6) C(9) 2.765(8) ? . . C(6) H(1) 3.4197 ? . 2_556 C(6) H(3) 2.0158 ? . . C(6) H(5) 2.0369 ? . . C(6) H(6) 3.2399 ? . . C(6) H(15) 3.1727 ? . 2_556 C(6) H(19) 3.0113 ? . 1_566 C(7) C(2) 3.469(8) ? . 2_556 C(7) C(9) 2.383(8) ? . . C(7) H(1) 3.4518 ? . 2_556 C(7) H(3) 3.2390 ? . . C(7) H(4) 2.0408 ? . . C(7) H(6) 2.0098 ? . . C(7) H(7) 3.2356 ? . . C(7) H(19) 3.0841 ? . 1_566 C(8) H(3) 3.4607 ? . 2_556 C(8) H(4) 3.2416 ? . . C(8) H(5) 2.0145 ? . . C(8) H(7) 2.0226 ? . . C(8) H(19) 3.1021 ? . 1_566 C(9) H(2) 2.5856 ? . . C(9) H(3) 3.2469 ? . . C(9) H(3) 3.3169 ? . 2_556 C(9) H(5) 3.2384 ? . . C(9) H(6) 2.0197 ? . . C(9) H(12) 3.3815 ? . 2_667 C(9) H(19) 3.0451 ? . 1_566 C(10) Y(1) 3.368(4) ? . 2_646 C(10) O(1) 3.048(5) ? . 2_646 C(10) C(12) 2.441(6) ? . . C(10) H(2) 3.0313 ? . 1_545 C(10) H(8) 2.1043 ? . . C(10) H(9) 2.5499 ? . . C(11) O(1) 3.511(5) ? . 2_646 C(11) C(13) 2.505(6) ? . . C(11) C(14) 3.044(6) ? . . C(11) H(4) 3.5210 ? . 1_645 C(11) H(9) 1.9383 ? . . C(11) H(10) 2.7800 ? . . C(11) H(16) 3.3960 ? . 2_656 C(12) C(14) 2.512(7) ? . . C(12) C(18) 2.446(6) ? . . C(12) H(8) 1.9681 ? . . C(12) H(10) 2.6888 ? . . C(12) H(14) 2.5917 ? . . C(12) H(16) 3.2687 ? . 2_656 C(12) H(21) 3.4112 ? . 2_656 C(13) C(15) 2.403(7) ? . . C(13) C(16) 2.787(6) ? . . C(13) C(17) 2.406(6) ? . . C(13) H(8) 2.7063 ? . . C(13) H(9) 2.0699 ? . . C(13) H(10) 2.0280 ? . . C(13) H(11) 3.2567 ? . . C(13) H(13) 3.2597 ? . . C(13) H(14) 2.0282 ? . . C(13) H(14) 3.0787 ? . 2_647 C(13) H(21) 2.9727 ? . 2_656 C(14) C(16) 2.388(7) ? . . C(14) C(17) 2.742(7) ? . . C(14) C(18) 2.374(7) ? . . C(14) H(8) 2.7957 ? . . C(14) H(9) 3.3210 ? . . C(14) H(11) 2.0212 ? . . C(14) H(12) 3.2465 ? . . C(14) H(14) 3.2363 ? . . C(14) H(14) 2.9155 ? . 2_647 C(14) H(18) 3.3735 ? . 1_656 C(14) H(21) 3.3772 ? . 2_656 C(15) C(17) 2.374(8) ? . . C(15) C(18) 2.751(7) ? . . C(15) H(9) 3.2807 ? . 2_647 C(15) H(10) 2.0165 ? . . C(15) H(12) 2.0341 ? . . C(15) H(13) 3.2329 ? . . C(15) H(14) 3.3852 ? . 2_647 C(15) H(18) 3.2781 ? . 1_656 C(16) O(2) 3.482(6) ? . 2_647 C(16) O(4) 3.313(6) ? . 2_647 C(16) C(18) 2.396(7) ? . . C(16) H(7) 3.5511 ? . 2_637 C(16) H(9) 3.0322 ? . 2_647 C(16) H(10) 3.2418 ? . . C(16) H(11) 2.0292 ? . . C(16) H(13) 2.0173 ? . . C(16) H(14) 3.2487 ? . . C(16) H(20) 3.5138 ? . 2_656 C(17) O(4) 3.592(7) ? . 2_647 C(17) H(9) 3.2140 ? . 2_647 C(17) H(11) 3.2320 ? . . C(17) H(12) 2.0235 ? . . C(17) H(14) 2.0354 ? . . C(17) H(16) 3.4001 ? . 1_556 C(17) H(20) 3.5631 ? . 2_656 C(17) H(21) 3.4496 ? . 2_656 C(18) H(9) 2.5689 ? . . C(18) H(10) 3.2337 ? . . C(18) H(12) 3.2555 ? . . C(18) H(13) 2.0353 ? . . C(18) H(16) 3.4893 ? . 1_556 C(18) H(21) 3.2443 ? . 1_556 C(18) H(21) 3.0011 ? . 2_656 C(19) Y(1) 3.344(4) ? . 2_646 C(19) C(21) 2.462(6) ? . . C(19) H(2) 3.4664 ? . 1_545 C(19) H(4) 3.3858 ? . 2_546 C(19) H(5) 3.0929 ? . 2_536 C(19) H(8) 3.3395 ? . 2_656 C(19) H(13) 3.3994 ? . 1_554 C(19) H(15) 2.1013 ? . . C(19) H(16) 2.5861 ? . . C(20) O(6) 2.357(5) ? . 2_646 C(20) C(22) 2.496(6) ? . . C(20) C(23) 3.027(6) ? . . C(20) H(4) 3.3208 ? . 2_546 C(20) H(5) 2.9604 ? . 2_536 C(20) H(6) 3.3986 ? . 2_536 C(20) H(8) 3.2055 ? . 2_656 C(20) H(10) 3.3625 ? . 2_656 C(20) H(16) 1.9419 ? . . C(20) H(17) 2.7721 ? . . C(21) O(6) 2.819(5) ? . 2_646 C(21) C(23) 2.503(6) ? . . C(21) C(27) 2.466(6) ? . . C(21) H(5) 2.9125 ? . 2_536 C(21) H(10) 3.4565 ? . 2_656 C(21) H(13) 3.4831 ? . 1_554 C(21) H(14) 3.3232 ? . 1_554 C(21) H(15) 1.9586 ? . . C(21) H(17) 2.6767 ? . . C(21) H(21) 2.6147 ? . . C(22) C(24) 2.397(7) ? . . C(22) C(25) 2.777(7) ? . . C(22) C(26) 2.411(7) ? . . C(22) H(10) 3.3294 ? . 2_656 C(22) H(11) 3.3971 ? . 2_656 C(22) H(14) 3.4877 ? . 1_554 C(22) H(15) 2.6728 ? . . C(22) H(16) 2.0802 ? . . C(22) H(17) 2.0270 ? . . C(22) H(18) 3.2512 ? . . C(22) H(18) 3.3306 ? . 2_545 C(22) H(20) 3.2683 ? . . C(22) H(21) 2.0368 ? . . C(23) C(25) 2.384(7) ? . . C(23) C(26) 2.755(7) ? . . C(23) C(27) 2.383(8) ? . . C(23) H(10) 3.3893 ? . 2_656 C(23) H(11) 3.1351 ? . 2_656 C(23) H(15) 2.7495 ? . . C(23) H(16) 3.3063 ? . . C(23) H(18) 2.0245 ? . . C(23) H(18) 3.5655 ? . 2_545 C(23) H(19) 3.2413 ? . . C(23) H(21) 3.2428 ? . . C(24) C(26) 2.377(9) ? . . C(24) C(27) 2.749(9) ? . . C(24) H(11) 3.3237 ? . 1_454 C(24) H(11) 2.9509 ? . 2_656 C(24) H(17) 2.0240 ? . . C(24) H(18) 3.5704 ? . 2_545 C(24) H(19) 2.0186 ? . . C(24) H(20) 3.2348 ? . . C(25) C(27) 2.391(8) ? . . C(25) H(11) 3.0507 ? . 2_656 C(25) H(17) 3.2376 ? . . C(25) H(17) 3.2632 ? . 2_545 C(25) H(18) 2.0156 ? . . C(25) H(18) 3.3301 ? . 2_545 C(25) H(20) 2.0283 ? . . C(25) H(21) 3.2475 ? . . C(26) H(11) 3.3294 ? . 2_656 C(26) H(17) 3.4356 ? . 2_545 C(26) H(18) 3.2340 ? . . C(26) H(18) 3.0420 ? . 2_545 C(26) H(19) 2.0277 ? . . C(26) H(21) 2.0326 ? . . C(27) C(21) 2.466(6) ? . . C(27) C(23) 2.383(8) ? . . C(27) C(24) 2.749(9) ? . . C(27) C(25) 2.391(8) ? . . C(27) H(11) 3.4893 ? . 2_656 C(27) H(14) 3.2902 ? . 1_554 C(27) H(16) 2.6158 ? . . C(27) H(17) 3.2438 ? . . C(27) H(18) 3.0363 ? . 2_545 C(27) H(19) 3.2505 ? . . C(27) H(20) 2.0361 ? . . H(1) O(1) 3.1871 ? . 2_656 H(1) C(6) 3.4197 ? . 2_546 H(1) C(7) 3.4518 ? . 2_546 H(2) O(1) 2.4621 ? . 2_656 H(2) O(3) 3.3856 ? . 1_565 H(2) O(4) 2.6808 ? . 1_565 H(2) O(5) 3.1132 ? . 1_565 H(2) O(6) 3.5615 ? . 2_656 H(2) C(10) 3.0313 ? . 1_565 H(2) C(19) 3.4664 ? . 1_565 H(3) O(5) 3.5299 ? . 2_556 H(3) C(8) 3.4607 ? . 2_546 H(3) C(9) 3.3169 ? . 2_546 H(4) O(2) 3.0623 ? . 2_556 H(4) O(3) 3.1135 ? . 1_465 H(4) O(5) 2.6038 ? . 2_556 H(4) C(1) 3.4939 ? . 2_556 H(4) C(11) 3.5210 ? . 1_465 H(4) C(19) 3.3858 ? . 2_556 H(4) C(20) 3.3208 ? . 2_556 H(5) O(3) 3.5292 ? . 1_465 H(5) O(6) 2.9096 ? . 1_465 H(5) C(1) 3.5995 ? . 2_556 H(5) C(2) 3.5189 ? . 2_556 H(5) C(19) 3.0929 ? . 2_566 H(5) C(20) 2.9604 ? . 2_566 H(5) C(21) 2.9125 ? . 2_566 H(6) C(20) 3.3986 ? . 2_566 H(7) O(2) 3.0408 ? . 1_565 H(7) O(4) 3.0155 ? . 1_565 H(7) C(16) 3.5511 ? . 2_667 H(8) O(1) 3.4782 ? . 2_646 H(8) O(5) 3.1653 ? . 2_646 H(8) C(19) 3.3395 ? . 2_646 H(8) C(20) 3.2055 ? . 2_646 H(9) C(15) 3.2807 ? . 2_657 H(9) C(16) 3.0322 ? . 2_657 H(9) C(17) 3.2140 ? . 2_657 H(10) C(20) 3.3625 ? . 2_646 H(10) C(21) 3.4565 ? . 2_646 H(10) C(22) 3.3294 ? . 2_646 H(10) C(23) 3.3893 ? . 2_646 H(11) C(22) 3.3971 ? . 2_646 H(11) C(23) 3.1351 ? . 2_646 H(11) C(24) 3.3237 ? . 1_656 H(11) C(24) 2.9509 ? . 2_646 H(11) C(25) 3.0507 ? . 2_646 H(11) C(26) 3.3294 ? . 2_646 H(11) C(27) 3.4893 ? . 2_646 H(12) O(2) 2.7665 ? . 2_647 H(12) O(4) 2.8932 ? . 2_647 H(12) C(1) 3.2247 ? . 2_647 H(12) C(2) 3.4481 ? . 2_647 H(12) C(9) 3.3815 ? . 2_637 H(13) O(1) 3.1243 ? . 1_556 H(13) O(2) 3.0471 ? . 2_647 H(13) O(4) 3.4048 ? . 2_647 H(13) O(6) 3.1271 ? . 2_647 H(13) C(1) 3.0452 ? . 2_647 H(13) C(19) 3.3994 ? . 1_556 H(13) C(21) 3.4831 ? . 1_556 H(14) C(13) 3.0787 ? . 2_657 H(14) C(14) 2.9155 ? . 2_657 H(14) C(15) 3.3852 ? . 2_657 H(14) C(21) 3.3232 ? . 1_556 H(14) C(22) 3.4877 ? . 1_556 H(14) C(27) 3.2902 ? . 1_556 H(15) O(6) 3.1833 ? . 2_646 H(15) C(5) 3.2788 ? . 2_546 H(15) C(6) 3.1727 ? . 2_546 H(16) O(6) 2.4925 ? . 2_646 H(16) C(11) 3.3960 ? . 2_646 H(16) C(12) 3.2687 ? . 2_646 H(16) C(17) 3.4001 ? . 1_554 H(16) C(18) 3.4893 ? . 1_554 H(16) C(27) 2.6158 ? . . H(17) C(25) 3.2632 ? . 2_555 H(17) C(26) 3.4356 ? . 2_555 H(17) C(27) 3.2438 ? . . H(18) C(14) 3.3735 ? . 1_454 H(18) C(15) 3.2781 ? . 1_454 H(18) C(22) 3.3306 ? . 2_555 H(18) C(23) 3.5655 ? . 2_555 H(18) C(24) 3.5704 ? . 2_555 H(18) C(25) 3.3301 ? . 2_555 H(18) C(26) 3.0420 ? . 2_555 H(18) C(27) 3.0363 ? . 2_555 H(19) C(4) 2.9394 ? . 1_544 H(19) C(5) 2.9364 ? . 1_544 H(19) C(6) 3.0113 ? . 1_544 H(19) C(7) 3.0841 ? . 1_544 H(19) C(8) 3.1021 ? . 1_544 H(19) C(9) 3.0451 ? . 1_544 H(19) C(27) 3.2505 ? . . H(20) C(2) 3.3415 ? . 1_544 H(20) C(3) 3.1516 ? . 1_544 H(20) C(4) 3.3299 ? . 1_544 H(20) C(16) 3.5138 ? . 2_646 H(20) C(17) 3.5631 ? . 2_646 H(20) C(27) 2.0361 ? . . H(21) C(12) 3.4112 ? . 2_646 H(21) C(13) 2.9727 ? . 2_646 H(21) C(14) 3.3772 ? . 2_646 H(21) C(17) 3.4496 ? . 2_646 H(21) C(18) 3.2443 ? . 1_554 H(21) C(18) 3.0011 ? . 2_646 H(21) C(21) 2.6147 ? . . H(21) C(22) 2.0368 ? . . H(21) C(23) 3.2428 ? . . H(21) C(25) 3.2475 ? . . H(21) C(26) 2.0326 ? . . Y(1) Y(1) 4.124(1) ? . 2_646 Y(1) Y(1) 4.124(1) ? 2_656 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(3) H(2) O(1) 2_656 0.95 2.46 2.810(8) 101 ? C(12) H(9) O(4) . 0.95 2.48 2.824(5) 101 ? C(21) H(16) O(6) 2_646 0.95 2.49 2.818(5) 100 ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Tm-wt1272w.cif' #============================================================================== data_Tm-wt1272w _database_code_depnum_ccdc_archive 'CCDC 631231' # Kin-K370 [Tm(cinnamate)3]n #============================================================================== _audit_creation_date 2006-07-05 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 O6 Tm ' _chemical_formula_moiety 'C27 H21 O6 Tm ' _chemical_formula_weight 610.39 _chemical_melting_point ? _chemical_absolute_configuration ad # 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.564(1) _cell_length_b 7.8702(9) _cell_length_c 13.042(2) _cell_angle_alpha 90 _cell_angle_beta 94.280(2) _cell_angle_gamma 90 _cell_volume 1183.6(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7338 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600.00 _exptl_absorpt_coefficient_mu 3.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.733 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7338 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9661 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9661 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0\s(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0\s(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2814 _reflns_number_gt 2628 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0210 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2631 _refine_ls_number_parameters 329 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + \s(Fo^2^) + 0.0001]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.72 _refine_diff_density_min -0.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 0 Friedel Pairs' _refine_ls_abs_structure_Flack 0.028(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Tm Tm -0.314 5.248 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Tm(1) Tm 0.460760(10) 0.47211(13) 0.523800(10) 0.02447(5) Uani 1.00 1 d . . . O(1) O 0.5942(3) 0.4008(5) 0.4168(3) 0.0376(10) Uani 1.00 1 d . . . O(2) O 0.3252(3) 0.6434(5) 0.5824(3) 0.0387(11) Uani 1.00 1 d . . . O(3) O 0.5407(3) 0.1994(5) 0.5866(2) 0.0315(10) Uani 1.00 1 d . . . O(4) O 0.4165(3) 0.3336(5) 0.6754(3) 0.0382(11) Uani 1.00 1 d . . . O(5) O 0.3309(3) 0.3325(5) 0.4218(3) 0.0390(11) Uani 1.00 1 d . . . O(6) O 0.6024(3) 0.5838(5) 0.6287(3) 0.0404(11) Uani 1.00 1 d . . . C(1) C 0.3203(5) 0.8039(7) 0.5895(4) 0.033(1) Uani 1.00 1 d . . . C(2) C 0.2072(8) 0.8786(12) 0.6053(7) 0.035(2) Uani 1.00 1 d . . . C(3) C 0.1887(8) 1.0451(12) 0.6078(7) 0.037(2) Uani 1.00 1 d . . . C(4) C 0.0815(5) 1.1378(8) 0.6202(4) 0.038(2) Uani 1.00 1 d . . . C(5) C -0.0274(5) 1.0576(8) 0.6162(4) 0.043(2) Uani 1.00 1 d . . . C(6) C -0.1265(5) 1.1455(9) 0.6318(5) 0.049(2) Uani 1.00 1 d . . . C(7) C -0.1211(6) 1.3185(9) 0.6513(6) 0.057(2) Uani 1.00 1 d . . . C(8) C -0.0148(6) 1.3986(9) 0.6562(6) 0.061(2) Uani 1.00 1 d . . . C(9) C 0.0856(6) 1.3130(8) 0.6389(5) 0.052(2) Uani 1.00 1 d . . . C(10) C 0.4967(5) 0.2300(7) 0.6734(4) 0.031(1) Uani 1.00 1 d . . . C(11) C 0.5530(5) 0.1536(8) 0.7682(4) 0.040(2) Uani 1.00 1 d . . . C(12) C 0.5261(5) 0.2027(8) 0.8600(4) 0.039(2) Uani 1.00 1 d . . . C(13) C 0.5844(5) 0.1580(8) 0.9593(4) 0.036(2) Uani 1.00 1 d . . . C(14) C 0.6876(5) 0.0674(8) 0.9701(5) 0.047(2) Uani 1.00 1 d . . . C(15) C 0.7409(6) 0.0341(9) 1.0661(5) 0.055(2) Uani 1.00 1 d . . . C(16) C 0.6922(6) 0.0878(9) 1.1529(5) 0.055(2) Uani 1.00 1 d . . . C(17) C 0.5916(6) 0.1784(10) 1.1441(4) 0.056(2) Uani 1.00 1 d . . . C(18) C 0.5366(5) 0.2135(9) 1.0484(4) 0.046(2) Uani 1.00 1 d . . . C(19) C 0.3331(4) 0.2107(7) 0.3587(4) 0.032(1) Uani 1.00 1 d . . . C(20) C 0.2533(5) 0.2226(7) 0.2649(4) 0.037(2) Uani 1.00 1 d . . . C(21) C 0.2622(5) 0.1234(8) 0.1835(4) 0.037(2) Uani 1.00 1 d . . . C(22) C 0.1894(5) 0.1281(8) 0.0861(4) 0.038(2) Uani 1.00 1 d . . . C(23) C 0.0828(5) 0.2095(9) 0.0764(5) 0.049(2) Uani 1.00 1 d . . . C(24) C 0.0173(8) 0.213(2) -0.0169(6) 0.055(3) Uani 1.00 1 d . . . C(25) C 0.0586(6) 0.1354(10) -0.1013(5) 0.058(2) Uani 1.00 1 d . . . C(26) C 0.1631(7) 0.0555(10) -0.0934(5) 0.061(2) Uani 1.00 1 d . . . C(27) C 0.2302(6) 0.0491(9) 0.0007(5) 0.049(2) Uani 1.00 1 d . . . H(1) H 0.1439 0.8044 0.6142 0.042 Uiso 1.00 1 c R . . H(2) H 0.2550 1.1138 0.6003 0.044 Uiso 1.00 1 c R . . H(3) H -0.0322 0.9392 0.6023 0.051 Uiso 1.00 1 c R . . H(4) H -0.1990 1.0881 0.6294 0.059 Uiso 1.00 1 c R . . H(5) H -0.1897 1.3811 0.6610 0.069 Uiso 1.00 1 c R . . H(6) H -0.0108 1.5163 0.6720 0.074 Uiso 1.00 1 c R . . H(7) H 0.1572 1.3723 0.6396 0.063 Uiso 1.00 1 c R . . H(8) H 0.6097 0.0673 0.7627 0.049 Uiso 1.00 1 c R . . H(9) H 0.4610 0.2760 0.8617 0.047 Uiso 1.00 1 c R . . H(10) H 0.7218 0.0278 0.9106 0.056 Uiso 1.00 1 c R . . H(11) H 0.8121 -0.0266 1.0720 0.066 Uiso 1.00 1 c R . . H(12) H 0.7284 0.0621 1.2188 0.066 Uiso 1.00 1 c R . . H(13) H 0.5587 0.2178 1.2043 0.067 Uiso 1.00 1 c R . . H(14) H 0.4661 0.2758 1.0435 0.056 Uiso 1.00 1 c R . . H(15) H 0.1930 0.3049 0.2628 0.045 Uiso 1.00 1 c R . . H(16) H 0.3220 0.0405 0.1887 0.045 Uiso 1.00 1 c R . . H(17) H 0.0543 0.2634 0.1346 0.059 Uiso 1.00 1 c R . . H(18) H -0.0556 0.2695 -0.0226 0.066 Uiso 1.00 1 c R . . H(19) H 0.0139 0.1376 -0.1654 0.069 Uiso 1.00 1 c R . . H(20) H 0.1911 0.0032 -0.1523 0.073 Uiso 1.00 1 c R . . H(21) H 0.3026 -0.0084 0.0059 0.059 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tm(1) 0.02977(9) 0.02037(9) 0.02285(9) -0.0010(2) -0.00090(6) -0.0001(2) O(1) 0.032(2) 0.045(2) 0.036(2) 0.009(2) 0.008(2) 0.008(2) O(2) 0.044(2) 0.033(2) 0.039(2) 0.001(2) 0.008(2) -0.000(2) O(3) 0.044(2) 0.027(2) 0.022(2) -0.002(2) -0.002(2) 0.000(2) O(4) 0.048(2) 0.034(2) 0.033(2) 0.005(2) 0.004(2) 0.001(2) O(5) 0.043(2) 0.035(2) 0.037(2) -0.001(2) -0.008(2) -0.008(2) O(6) 0.045(2) 0.036(2) 0.038(2) -0.005(2) -0.014(2) 0.000(2) C(1) 0.039(3) 0.036(3) 0.024(3) 0.001(3) 0.004(2) 0.001(2) C(2) 0.034(4) 0.027(4) 0.046(5) 0.000(3) 0.009(3) 0.001(3) C(3) 0.029(4) 0.037(4) 0.044(5) -0.007(3) 0.003(3) 0.001(3) C(4) 0.039(3) 0.033(3) 0.041(3) 0.005(3) 0.001(2) -0.002(3) C(5) 0.043(3) 0.039(3) 0.046(3) 0.006(3) 0.000(3) -0.004(3) C(6) 0.039(3) 0.054(4) 0.053(4) 0.004(3) 0.000(3) -0.003(3) C(7) 0.049(4) 0.059(5) 0.063(4) 0.024(4) -0.001(3) -0.006(4) C(8) 0.066(5) 0.034(3) 0.085(5) 0.011(3) 0.003(4) -0.014(4) C(9) 0.056(4) 0.039(4) 0.062(4) 0.003(3) 0.003(3) -0.001(3) C(10) 0.046(3) 0.020(3) 0.027(3) -0.008(2) -0.003(2) 0.001(2) C(11) 0.056(4) 0.037(3) 0.028(3) 0.005(3) 0.001(3) 0.005(3) C(12) 0.048(3) 0.034(3) 0.035(3) 0.001(3) 0.002(2) 0.001(3) C(13) 0.045(3) 0.033(3) 0.029(3) -0.005(3) -0.000(2) 0.002(2) C(14) 0.053(4) 0.050(4) 0.038(3) 0.010(3) 0.009(3) 0.000(3) C(15) 0.055(4) 0.060(5) 0.048(4) 0.010(3) -0.005(3) 0.010(3) C(16) 0.067(4) 0.067(5) 0.029(3) -0.005(4) -0.009(3) 0.012(3) C(17) 0.064(4) 0.076(5) 0.028(3) -0.003(4) 0.009(3) 0.002(3) C(18) 0.050(3) 0.055(4) 0.034(3) 0.003(3) 0.001(3) 0.004(3) C(19) 0.032(3) 0.030(3) 0.033(3) -0.005(2) -0.001(2) 0.000(2) C(20) 0.040(3) 0.031(3) 0.039(3) -0.002(3) -0.009(2) 0.002(3) C(21) 0.038(3) 0.037(3) 0.036(3) -0.002(3) -0.005(2) 0.002(3) C(22) 0.045(3) 0.034(3) 0.033(3) -0.005(3) -0.006(2) -0.001(3) C(23) 0.050(3) 0.057(4) 0.038(3) 0.003(3) -0.006(3) -0.002(3) C(24) 0.047(6) 0.062(5) 0.053(6) 0.002(4) -0.017(4) 0.001(5) C(25) 0.076(5) 0.061(5) 0.033(3) -0.010(4) -0.020(3) 0.005(3) C(26) 0.080(5) 0.068(5) 0.034(3) 0.002(4) 0.000(3) -0.012(3) C(27) 0.054(4) 0.049(4) 0.044(3) 0.005(3) -0.005(3) -0.012(3) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Tm(1) O(1) 2.229(4) ? . . Tm(1) O(2) 2.244(4) ? . . Tm(1) O(3) 2.453(4) ? . . Tm(1) O(3) 2.296(4) ? . 2_656 Tm(1) O(4) 2.348(4) ? . . Tm(1) O(5) 2.221(4) ? . . Tm(1) O(6) 2.234(4) ? . . O(1) C(1) 1.256(7) ? . 2_646 O(2) C(1) 1.268(7) ? . . O(3) Tm(1) 2.296(4) ? . 2_646 O(3) C(10) 1.298(6) ? . . O(4) C(10) 1.237(7) ? . . O(5) C(19) 1.265(7) ? . . O(6) C(19) 1.249(7) ? . 2_656 C(1) O(1) 1.256(7) ? . 2_656 C(1) C(2) 1.46(1) ? . . C(2) C(3) 1.33(1) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.46(1) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.406(8) ? . . C(4) C(9) 1.400(9) ? . . C(5) C(6) 1.368(9) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.39(1) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.38(1) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.38(1) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . C(10) C(11) 1.481(7) ? . . C(11) C(12) 1.317(8) ? . . C(11) H(8) 0.9500 ? . . C(12) C(13) 1.458(7) ? . . C(12) H(9) 0.9500 ? . . C(13) C(14) 1.388(8) ? . . C(13) C(18) 1.394(8) ? . . C(14) C(15) 1.379(8) ? . . C(14) H(10) 0.9500 ? . . C(15) C(16) 1.368(9) ? . . C(15) H(11) 0.9500 ? . . C(16) C(17) 1.36(1) ? . . C(16) H(12) 0.9500 ? . . C(17) C(18) 1.385(8) ? . . C(17) H(13) 0.9500 ? . . C(18) H(14) 0.9500 ? . . C(19) O(6) 1.249(7) ? . 2_646 C(19) C(20) 1.480(7) ? . . C(20) C(21) 1.328(8) ? . . C(20) H(15) 0.9500 ? . . C(21) C(22) 1.471(7) ? . . C(21) H(16) 0.9500 ? . . C(22) C(23) 1.386(9) ? . . C(22) C(27) 1.389(8) ? . . C(23) C(24) 1.38(1) ? . . C(23) H(17) 0.9500 ? . . C(24) C(25) 1.38(1) ? . . C(24) H(18) 0.9500 ? . . C(25) C(26) 1.36(1) ? . . C(25) H(19) 0.9500 ? . . C(26) C(27) 1.402(9) ? . . C(26) H(20) 0.9500 ? . . C(27) C(22) 1.389(8) ? . . C(27) C(26) 1.402(9) ? . . C(27) H(21) 0.9500 ? . . H(20) C(26) 0.9500 ? . . H(21) C(27) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Tm(1) O(1) 153.9(1) ? . . . O(3) Tm(1) O(1) 74.2(1) ? . . . O(3) Tm(1) O(1) 77.1(1) ? 2_656 . . O(4) Tm(1) O(1) 128.0(1) ? . . . O(5) Tm(1) O(1) 88.2(1) ? . . . O(6) Tm(1) O(1) 88.4(1) ? . . . Tm(1) O(1) C(1) 141.1(3) ? . . 2_646 O(3) Tm(1) O(2) 131.9(1) ? . . . O(3) Tm(1) O(2) 76.9(1) ? 2_656 . . O(4) Tm(1) O(2) 77.9(1) ? . . . O(5) Tm(1) O(2) 92.5(1) ? . . . O(6) Tm(1) O(2) 93.1(1) ? . . . Tm(1) O(2) C(1) 131.3(4) ? . . . O(3) Tm(1) O(3) 151.2(1) ? 2_656 . . O(4) Tm(1) O(3) 54.1(1) ? . . . O(5) Tm(1) O(3) 89.3(1) ? . . . O(6) Tm(1) O(3) 84.2(1) ? . . . Tm(1) O(3) C(10) 88.1(3) ? . . . Tm(1) O(3) Tm(1) 119.2(1) ? . . 2_646 O(4) Tm(1) O(3) 153.9(1) ? . . 2_656 O(5) Tm(1) O(3) 92.1(1) ? . . 2_656 O(6) Tm(1) O(3) 92.7(1) ? . . 2_656 Tm(1) O(3) C(10) 135.0(3) ? . 2_656 2_656 Tm(1) O(3) Tm(1) 119.2(1) ? . 2_656 2_656 O(5) Tm(1) O(4) 95.4(1) ? . . . O(6) Tm(1) O(4) 82.1(1) ? . . . Tm(1) O(4) C(10) 94.4(3) ? . . . O(6) Tm(1) O(5) 173.3(2) ? . . . Tm(1) O(5) C(19) 136.0(3) ? . . . Tm(1) O(6) C(19) 143.0(3) ? . . 2_656 O(1) C(1) O(2) 124.1(5) ? . 2_646 2_646 O(1) C(1) C(2) 118.8(6) ? . 2_646 2_646 O(2) C(1) O(1) 124.1(5) ? . . 2_656 O(2) C(1) C(2) 117.1(6) ? . . . C(10) O(3) Tm(1) 135.0(3) ? . . 2_646 O(3) Tm(1) O(2) 76.9(1) ? . 2_646 2_646 O(3) Tm(1) O(6) 92.7(1) ? . 2_646 2_646 O(3) Tm(1) O(1) 77.1(1) ? . 2_646 2_646 O(3) Tm(1) O(5) 92.1(1) ? . 2_646 2_646 O(3) C(10) O(4) 119.0(4) ? . . . O(3) C(10) C(11) 118.5(5) ? . . . O(4) C(10) C(11) 122.2(5) ? . . . O(5) C(19) O(6) 124.1(5) ? . . 2_646 O(5) C(19) C(20) 116.6(5) ? . . . O(6) C(19) O(5) 124.1(5) ? . 2_656 2_656 O(6) C(19) C(20) 119.3(5) ? . 2_656 2_656 C(2) C(1) O(1) 118.8(6) ? . . 2_656 C(1) O(1) Tm(1) 141.1(3) ? . 2_656 2_656 C(1) C(2) C(3) 123.2(8) ? . . . C(1) C(2) H(1) 118.4141 ? . . . H(1) C(2) C(3) 118.4142 ? . . . C(2) C(3) H(2) 115.2297 ? . . . C(2) C(3) C(4) 129.5(9) ? . . . H(2) C(3) C(4) 115.2293 ? . . . C(3) C(4) C(5) 122.5(6) ? . . . C(3) C(4) C(9) 119.6(6) ? . . . C(4) C(5) H(3) 119.1329 ? . . . C(9) C(4) C(5) 117.8(6) ? . . . C(4) C(5) C(6) 121.7(6) ? . . . C(4) C(9) H(7) 120.2361 ? . . . C(4) C(9) C(8) 119.5(6) ? . . . H(3) C(5) C(6) 119.1330 ? . . . C(5) C(6) C(7) 119.8(6) ? . . . C(5) C(6) H(4) 120.0847 ? . . . C(6) C(7) C(8) 119.1(7) ? . . . H(4) C(6) C(7) 120.0850 ? . . . C(6) C(7) H(5) 120.4736 ? . . . C(7) C(8) C(9) 122.0(7) ? . . . C(7) C(8) H(6) 119.0180 ? . . . H(5) C(7) C(8) 120.4739 ? . . . C(8) C(9) H(7) 120.2359 ? . . . H(6) C(8) C(9) 119.0186 ? . . . C(10) C(11) C(12) 121.4(5) ? . . . C(10) C(11) H(8) 119.3133 ? . . . H(8) C(11) C(12) 119.3125 ? . . . C(11) C(12) H(9) 116.1535 ? . . . C(11) C(12) C(13) 127.7(6) ? . . . H(9) C(12) C(13) 116.1537 ? . . . C(12) C(13) C(14) 123.5(5) ? . . . C(12) C(13) C(18) 118.6(5) ? . . . C(13) C(14) H(10) 119.5836 ? . . . C(18) C(13) C(14) 117.9(5) ? . . . C(13) C(14) C(15) 120.8(6) ? . . . C(13) C(18) H(14) 119.8338 ? . . . C(13) C(18) C(17) 120.3(6) ? . . . H(10) C(14) C(15) 119.5839 ? . . . C(14) C(15) C(16) 120.6(6) ? . . . C(14) C(15) H(11) 119.7209 ? . . . C(15) C(16) C(17) 119.6(6) ? . . . H(11) C(15) C(16) 119.7202 ? . . . C(15) C(16) H(12) 120.1873 ? . . . C(16) C(17) C(18) 120.7(6) ? . . . C(16) C(17) H(13) 119.6261 ? . . . H(12) C(16) C(17) 120.1874 ? . . . C(17) C(18) H(14) 119.8342 ? . . . H(13) C(17) C(18) 119.6267 ? . . . C(19) O(6) Tm(1) 143.0(3) ? . 2_646 2_646 C(20) C(19) O(6) 119.3(5) ? . . 2_646 C(19) C(20) C(21) 122.9(5) ? . . . C(19) C(20) H(15) 118.5675 ? . . . H(15) C(20) C(21) 118.5678 ? . . . C(20) C(21) H(16) 116.4955 ? . . . C(20) C(21) C(22) 127.0(5) ? . . . H(16) C(21) C(22) 116.4953 ? . . . C(21) C(22) C(23) 122.6(5) ? . . . C(21) C(22) C(27) 118.4(5) ? . . . C(22) C(23) H(17) 119.4906 ? . . . C(27) C(22) C(23) 119.1(5) ? . . . C(22) C(23) C(24) 121.0(7) ? . . . C(22) C(27) H(21) 120.4120 ? . . . C(22) C(27) C(26) 119.2(6) ? . . . H(17) C(23) C(24) 119.4900 ? . . . C(23) C(24) C(25) 119.5(8) ? . . . C(23) C(24) H(18) 120.2325 ? . . . C(24) C(25) C(26) 120.3(6) ? . . . H(18) C(24) C(25) 120.2323 ? . . . C(24) C(25) H(19) 119.8405 ? . . . C(25) C(26) C(27) 120.9(6) ? . . . C(25) C(26) H(20) 119.5593 ? . . . H(19) C(25) C(26) 119.8406 ? . . . C(26) C(27) H(21) 120.4119 ? . . . H(20) C(26) C(27) 119.5599 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Tm(1) O(1) 3.530(4) ? . 2_656 Tm(1) C(1) 3.225(6) ? . . Tm(1) C(1) 3.302(6) ? . 2_646 Tm(1) C(10) 2.736(5) ? . . Tm(1) C(10) 3.341(5) ? . 2_656 Tm(1) C(19) 3.252(5) ? . . Tm(1) C(19) 3.318(5) ? . 2_656 O(1) Tm(1) 3.530(4) ? . 2_646 O(1) O(2) 2.230(6) ? . 2_646 O(1) O(3) 2.829(5) ? . . O(1) O(3) 2.819(5) ? . 2_656 O(1) O(5) 3.097(5) ? . . O(1) O(6) 3.112(5) ? . . O(1) O(6) 3.397(5) ? . 2_646 O(1) C(2) 2.34(1) ? . 2_646 O(1) C(3) 2.80(1) ? . 2_646 O(1) C(10) 3.003(6) ? . 2_656 O(1) C(11) 3.473(7) ? . 2_656 O(1) C(19) 3.404(6) ? . . O(1) H(1) 3.1772 ? . 2_646 O(1) H(2) 2.4409 ? . 2_646 O(1) H(8) 3.4536 ? . 2_656 O(1) H(13) 3.1219 ? . 1_554 O(2) O(1) 2.230(6) ? . 2_656 O(2) O(3) 2.822(5) ? . 2_656 O(2) O(4) 2.888(6) ? . . O(2) O(5) 3.224(6) ? . . O(2) O(6) 3.251(6) ? . . O(2) C(2) 2.33(1) ? . . O(2) C(3) 3.56(1) ? . . O(2) C(6) 3.482(7) ? . 2_546 O(2) C(16) 3.501(7) ? . 2_657 O(2) H(1) 2.5116 ? . . O(2) H(4) 3.0571 ? . 2_546 O(2) H(7) 3.0167 ? . 1_545 O(2) H(12) 2.7846 ? . 2_657 O(2) H(13) 3.0538 ? . 2_657 O(3) O(1) 2.819(5) ? . 2_646 O(3) O(2) 2.822(5) ? . 2_646 O(3) O(4) 2.184(5) ? . . O(3) O(5) 3.290(5) ? . . O(3) O(5) 3.253(5) ? . 2_646 O(3) O(6) 3.147(5) ? . . O(3) O(6) 3.279(5) ? . 2_646 O(3) C(1) 3.014(6) ? . 2_646 O(3) C(11) 2.389(6) ? . . O(3) C(12) 3.582(6) ? . . O(3) H(2) 3.3894 ? . 1_545 O(3) H(4) 3.1449 ? . 1_645 O(3) H(5) 3.5011 ? . 1_645 O(3) H(8) 2.5915 ? . . O(4) O(5) 3.381(5) ? . . O(4) O(6) 3.011(6) ? . . O(4) C(3) 3.54(1) ? . 1_545 O(4) C(11) 2.382(7) ? . . O(4) C(12) 2.829(7) ? . . O(4) C(16) 3.319(8) ? . 2_657 O(4) C(17) 3.597(8) ? . 2_657 O(4) H(2) 2.6769 ? . 1_545 O(4) H(7) 3.0154 ? . 1_545 O(4) H(8) 3.2086 ? . . O(4) H(9) 2.4866 ? . . O(4) H(12) 2.8784 ? . 2_657 O(4) H(13) 3.4083 ? . 2_657 O(5) O(3) 3.253(5) ? . 2_656 O(5) O(6) 2.221(6) ? . 2_646 O(5) C(6) 3.450(8) ? . 2_546 O(5) C(20) 2.339(6) ? . . O(5) C(21) 3.554(7) ? . . O(5) H(2) 3.0752 ? . 1_545 O(5) H(3) 3.5464 ? . 2_546 O(5) H(4) 2.5828 ? . 2_546 O(5) H(8) 3.1504 ? . 2_656 O(5) H(15) 2.5296 ? . . O(6) O(1) 3.397(5) ? . 2_656 O(6) O(3) 3.279(5) ? . 2_656 O(6) O(5) 2.221(6) ? . 2_656 O(6) C(10) 3.113(7) ? . . O(6) C(20) 2.358(7) ? . 2_656 O(6) C(21) 2.825(6) ? . 2_656 O(6) H(2) 3.5252 ? . 2_646 O(6) H(5) 2.8903 ? . 1_645 O(6) H(13) 3.1514 ? . 2_657 O(6) H(15) 3.1824 ? . 2_656 O(6) H(16) 2.4984 ? . 2_656 C(1) Tm(1) 3.302(6) ? . 2_656 C(1) O(3) 3.014(6) ? . 2_656 C(1) C(3) 2.46(1) ? . . C(1) H(1) 2.0892 ? . . C(1) H(2) 2.5603 ? . . C(1) H(4) 3.5219 ? . 2_546 C(1) H(5) 3.5486 ? . 2_546 C(1) H(12) 3.2244 ? . 2_657 C(1) H(13) 3.0140 ? . 2_657 C(2) O(1) 2.34(1) ? . 2_656 C(2) C(4) 2.52(1) ? . . C(2) C(5) 3.07(1) ? . . C(2) C(7) 3.45(1) ? . 2_546 C(2) H(2) 1.9349 ? . . C(2) H(3) 2.8063 ? . . C(2) H(5) 3.4644 ? . 2_546 C(2) H(12) 3.4301 ? . 2_657 C(2) H(20) 3.3280 ? . 1_566 C(3) O(1) 2.80(1) ? . 2_656 C(3) O(4) 3.54(1) ? . 1_565 C(3) C(5) 2.51(1) ? . . C(3) C(9) 2.47(1) ? . . C(3) H(1) 1.9670 ? . . C(3) H(3) 2.6822 ? . . C(3) H(7) 2.6378 ? . . C(3) H(20) 3.1442 ? . 1_566 C(4) C(6) 2.423(8) ? . . C(4) C(7) 2.797(9) ? . . C(4) C(8) 2.398(9) ? . . C(4) H(1) 2.7237 ? . . C(4) H(2) 2.0507 ? . . C(4) H(3) 2.0449 ? . . C(4) H(4) 3.2783 ? . . C(4) H(6) 3.2525 ? . . C(4) H(7) 2.0499 ? . . C(4) H(19) 2.9588 ? . 1_566 C(4) H(20) 3.3121 ? . 1_566 C(5) C(7) 2.38(1) ? . . C(5) C(8) 2.74(1) ? . . C(5) C(9) 2.403(9) ? . . C(5) H(1) 2.8108 ? . . C(5) H(2) 3.3175 ? . . C(5) H(4) 2.0187 ? . . C(5) H(5) 3.2420 ? . . C(5) H(7) 3.2691 ? . . C(5) H(15) 3.2507 ? . 2_556 C(5) H(19) 2.9208 ? . 1_566 C(6) O(2) 3.482(7) ? . 2_556 C(6) O(5) 3.450(8) ? . 2_556 C(6) C(8) 2.38(1) ? . . C(6) C(9) 2.78(1) ? . . C(6) H(1) 3.4359 ? . 2_556 C(6) H(3) 2.0094 ? . . C(6) H(5) 2.0390 ? . . C(6) H(6) 3.2373 ? . . C(6) H(15) 3.1345 ? . 2_556 C(6) H(19) 2.9987 ? . 1_566 C(7) C(2) 3.45(1) ? . 2_556 C(7) C(9) 2.41(1) ? . . C(7) H(1) 3.4544 ? . 2_556 C(7) H(3) 3.2365 ? . . C(7) H(4) 2.0353 ? . . C(7) H(6) 2.0183 ? . . C(7) H(7) 3.2611 ? . . C(7) H(19) 3.1024 ? . 1_566 C(8) H(3) 3.4693 ? . 2_556 C(8) H(4) 3.2429 ? . . C(8) H(5) 2.0326 ? . . C(8) H(7) 2.0276 ? . . C(8) H(19) 3.1026 ? . 1_566 C(9) H(2) 2.5873 ? . . C(9) H(3) 3.2618 ? . . C(9) H(3) 3.3125 ? . 2_556 C(9) H(5) 3.2624 ? . . C(9) H(6) 2.0157 ? . . C(9) H(12) 3.3640 ? . 2_667 C(9) H(19) 3.0695 ? . 1_566 C(10) Tm(1) 3.341(5) ? . 2_646 C(10) O(1) 3.003(6) ? . 2_646 C(10) C(12) 2.441(7) ? . . C(10) H(2) 3.0264 ? . 1_545 C(10) H(8) 2.1150 ? . . C(10) H(9) 2.5463 ? . . C(11) O(1) 3.473(7) ? . 2_646 C(11) C(13) 2.492(7) ? . . C(11) C(14) 3.034(8) ? . . C(11) H(4) 3.5420 ? . 1_645 C(11) H(9) 1.9341 ? . . C(11) H(10) 2.7750 ? . . C(11) H(16) 3.3991 ? . 2_656 C(12) C(14) 2.507(8) ? . . C(12) C(18) 2.453(8) ? . . C(12) H(8) 1.9655 ? . . C(12) H(10) 2.6894 ? . . C(12) H(14) 2.6058 ? . . C(12) H(14) 3.5867 ? . 2_647 C(12) H(16) 3.2743 ? . 2_656 C(12) H(21) 3.4112 ? . 2_656 C(13) C(15) 2.406(8) ? . . C(13) C(16) 2.786(8) ? . . C(13) C(17) 2.411(8) ? . . C(13) H(8) 2.6984 ? . . C(13) H(9) 2.0615 ? . . C(13) H(10) 2.0323 ? . . C(13) H(11) 3.2601 ? . . C(13) H(13) 3.2659 ? . . C(13) H(14) 2.0406 ? . . C(13) H(14) 3.0634 ? . 2_647 C(13) H(21) 2.9529 ? . 2_656 C(14) C(16) 2.386(8) ? . . C(14) C(17) 2.743(9) ? . . C(14) C(18) 2.383(9) ? . . C(14) H(8) 2.7865 ? . . C(14) H(9) 3.3177 ? . . C(14) H(11) 2.0258 ? . . C(14) H(12) 3.2438 ? . . C(14) H(14) 3.2458 ? . . C(14) H(14) 2.8993 ? . 2_647 C(14) H(18) 3.3639 ? . 1_656 C(14) H(21) 3.3544 ? . 2_656 C(15) C(17) 2.36(1) ? . . C(15) C(18) 2.747(9) ? . . C(15) H(9) 3.2852 ? . 2_647 C(15) H(10) 2.0245 ? . . C(15) H(12) 2.0203 ? . . C(15) H(13) 3.2175 ? . . C(15) H(14) 3.3756 ? . 2_647 C(15) H(18) 3.2726 ? . 1_656 C(16) O(2) 3.501(7) ? . 2_647 C(16) O(4) 3.319(8) ? . 2_647 C(16) C(18) 2.389(9) ? . . C(16) H(7) 3.5397 ? . 2_637 C(16) H(9) 3.0241 ? . 2_647 C(16) H(10) 3.2386 ? . . C(16) H(11) 2.0157 ? . . C(16) H(13) 2.0096 ? . . C(16) H(14) 3.2413 ? . . C(16) H(20) 3.5367 ? . 2_656 C(17) O(4) 3.597(8) ? . 2_647 C(17) H(9) 3.2241 ? . 2_647 C(17) H(11) 3.2172 ? . . C(17) H(12) 2.0150 ? . . C(17) H(14) 2.0326 ? . . C(17) H(16) 3.3918 ? . 1_556 C(17) H(20) 3.5807 ? . 2_656 C(17) H(21) 3.4295 ? . 2_656 C(18) H(9) 2.5731 ? . . C(18) H(10) 3.2453 ? . . C(18) H(12) 3.2468 ? . . C(18) H(13) 2.0306 ? . . C(18) H(16) 3.4703 ? . 1_556 C(18) H(21) 3.2345 ? . 1_556 C(18) H(21) 2.9908 ? . 2_656 C(19) Tm(1) 3.318(5) ? . 2_646 C(19) C(21) 2.467(7) ? . . C(19) H(2) 3.4284 ? . 1_545 C(19) H(4) 3.3604 ? . 2_546 C(19) H(5) 3.0791 ? . 2_536 C(19) H(8) 3.3134 ? . 2_656 C(19) H(13) 3.4119 ? . 1_554 C(19) H(15) 2.1063 ? . . C(19) H(16) 2.5847 ? . . C(20) O(6) 2.358(7) ? . 2_646 C(20) C(22) 2.505(7) ? . . C(20) C(23) 3.036(8) ? . . C(20) H(4) 3.2712 ? . 2_546 C(20) H(5) 2.9673 ? . 2_536 C(20) H(6) 3.3945 ? . 2_536 C(20) H(8) 3.1759 ? . 2_656 C(20) H(10) 3.3441 ? . 2_656 C(20) H(16) 1.9470 ? . . C(20) H(17) 2.7753 ? . . C(21) O(6) 2.825(6) ? . 2_646 C(21) C(23) 2.506(8) ? . . C(21) C(27) 2.456(8) ? . . C(21) H(5) 2.9501 ? . 2_536 C(21) H(10) 3.4206 ? . 2_656 C(21) H(13) 3.4989 ? . 1_554 C(21) H(14) 3.3127 ? . 1_554 C(21) H(15) 1.9676 ? . . C(21) H(17) 2.6778 ? . . C(21) H(21) 2.6118 ? . . C(22) C(24) 2.41(1) ? . . C(22) C(25) 2.777(8) ? . . C(22) C(26) 2.407(8) ? . . C(22) H(10) 3.3081 ? . 2_656 C(22) H(11) 3.4107 ? . 2_656 C(22) H(14) 3.4877 ? . 1_554 C(22) H(15) 2.6890 ? . . C(22) H(16) 2.0765 ? . . C(22) H(17) 2.0300 ? . . C(22) H(18) 3.2674 ? . . C(22) H(18) 3.2947 ? . 2_545 C(22) H(20) 3.2630 ? . . C(22) H(21) 2.0413 ? . . C(23) C(25) 2.385(9) ? . . C(23) C(26) 2.746(9) ? . . C(23) C(27) 2.392(9) ? . . C(23) H(10) 3.3690 ? . 2_656 C(23) H(11) 3.1443 ? . 2_656 C(23) H(15) 2.7634 ? . . C(23) H(16) 3.3110 ? . . C(23) H(18) 2.0354 ? . . C(23) H(18) 3.5426 ? . 2_545 C(23) H(19) 3.2441 ? . . C(23) H(21) 3.2546 ? . . C(24) C(26) 2.37(1) ? . . C(24) C(27) 2.77(1) ? . . C(24) H(11) 3.3098 ? . 1_454 C(24) H(11) 2.9675 ? . 2_656 C(24) H(17) 2.0281 ? . . C(24) H(18) 3.5544 ? . 2_545 C(24) H(19) 2.0247 ? . . C(24) H(20) 3.2291 ? . . C(25) C(27) 2.402(9) ? . . C(25) H(11) 3.0605 ? . 2_656 C(25) H(17) 3.2409 ? . . C(25) H(17) 3.2225 ? . 2_545 C(25) H(18) 2.0286 ? . . C(25) H(18) 3.3042 ? . 2_545 C(25) H(20) 2.0065 ? . . C(25) H(21) 3.2565 ? . . C(26) H(11) 3.3113 ? . 2_656 C(26) H(17) 3.4197 ? . 2_545 C(26) H(18) 3.2307 ? . . C(26) H(18) 3.0298 ? . 2_545 C(26) H(19) 2.0092 ? . . C(26) H(21) 2.0533 ? . . C(27) C(21) 2.456(8) ? . . C(27) C(23) 2.392(9) ? . . C(27) C(24) 2.77(1) ? . . C(27) C(25) 2.402(9) ? . . C(27) H(11) 3.4951 ? . 2_656 C(27) H(14) 3.2726 ? . 1_554 C(27) H(16) 2.5998 ? . . C(27) H(17) 3.2494 ? . . C(27) H(18) 3.0144 ? . 2_545 C(27) H(19) 3.2591 ? . . C(27) H(20) 2.0449 ? . . H(1) O(1) 3.1772 ? . 2_656 H(1) C(6) 3.4359 ? . 2_546 H(1) C(7) 3.4544 ? . 2_546 H(2) O(1) 2.4409 ? . 2_656 H(2) O(3) 3.3894 ? . 1_565 H(2) O(4) 2.6769 ? . 1_565 H(2) O(5) 3.0752 ? . 1_565 H(2) O(6) 3.5252 ? . 2_656 H(2) C(10) 3.0264 ? . 1_565 H(2) C(19) 3.4284 ? . 1_565 H(3) O(5) 3.5464 ? . 2_556 H(3) C(8) 3.4693 ? . 2_546 H(3) C(9) 3.3125 ? . 2_546 H(4) O(2) 3.0571 ? . 2_556 H(4) O(3) 3.1449 ? . 1_465 H(4) O(5) 2.5828 ? . 2_556 H(4) C(1) 3.5219 ? . 2_556 H(4) C(11) 3.5420 ? . 1_465 H(4) C(19) 3.3604 ? . 2_556 H(4) C(20) 3.2712 ? . 2_556 H(5) O(3) 3.5011 ? . 1_465 H(5) O(6) 2.8903 ? . 1_465 H(5) C(1) 3.5486 ? . 2_556 H(5) C(2) 3.4644 ? . 2_556 H(5) C(19) 3.0791 ? . 2_566 H(5) C(20) 2.9673 ? . 2_566 H(5) C(21) 2.9501 ? . 2_566 H(6) C(20) 3.3945 ? . 2_566 H(7) O(2) 3.0167 ? . 1_565 H(7) O(4) 3.0154 ? . 1_565 H(7) C(16) 3.5397 ? . 2_667 H(8) O(1) 3.4536 ? . 2_646 H(8) O(5) 3.1504 ? . 2_646 H(8) C(19) 3.3134 ? . 2_646 H(8) C(20) 3.1759 ? . 2_646 H(9) C(15) 3.2852 ? . 2_657 H(9) C(16) 3.0241 ? . 2_657 H(9) C(17) 3.2241 ? . 2_657 H(10) C(20) 3.3441 ? . 2_646 H(10) C(21) 3.4206 ? . 2_646 H(10) C(22) 3.3081 ? . 2_646 H(10) C(23) 3.3690 ? . 2_646 H(11) C(22) 3.4107 ? . 2_646 H(11) C(23) 3.1443 ? . 2_646 H(11) C(24) 3.3098 ? . 1_656 H(11) C(24) 2.9675 ? . 2_646 H(11) C(25) 3.0605 ? . 2_646 H(11) C(26) 3.3113 ? . 2_646 H(11) C(27) 3.4951 ? . 2_646 H(12) O(2) 2.7846 ? . 2_647 H(12) O(4) 2.8784 ? . 2_647 H(12) C(1) 3.2244 ? . 2_647 H(12) C(2) 3.4301 ? . 2_647 H(12) C(9) 3.3640 ? . 2_637 H(13) O(1) 3.1219 ? . 1_556 H(13) O(2) 3.0538 ? . 2_647 H(13) O(4) 3.4083 ? . 2_647 H(13) O(6) 3.1514 ? . 2_647 H(13) C(1) 3.0140 ? . 2_647 H(13) C(19) 3.4119 ? . 1_556 H(13) C(21) 3.4989 ? . 1_556 H(14) C(12) 3.5867 ? . 2_657 H(14) C(13) 3.0634 ? . 2_657 H(14) C(14) 2.8993 ? . 2_657 H(14) C(15) 3.3756 ? . 2_657 H(14) C(21) 3.3127 ? . 1_556 H(14) C(22) 3.4877 ? . 1_556 H(14) C(27) 3.2726 ? . 1_556 H(15) O(6) 3.1824 ? . 2_646 H(15) C(5) 3.2507 ? . 2_546 H(15) C(6) 3.1345 ? . 2_546 H(16) O(6) 2.4984 ? . 2_646 H(16) C(11) 3.3991 ? . 2_646 H(16) C(12) 3.2743 ? . 2_646 H(16) C(17) 3.3918 ? . 1_554 H(16) C(18) 3.4703 ? . 1_554 H(16) C(27) 2.5998 ? . . H(17) C(25) 3.2225 ? . 2_555 H(17) C(26) 3.4197 ? . 2_555 H(17) C(27) 3.2494 ? . . H(18) C(14) 3.3639 ? . 1_454 H(18) C(15) 3.2726 ? . 1_454 H(18) C(22) 3.2947 ? . 2_555 H(18) C(23) 3.5426 ? . 2_555 H(18) C(24) 3.5544 ? . 2_555 H(18) C(25) 3.3042 ? . 2_555 H(18) C(26) 3.0298 ? . 2_555 H(18) C(27) 3.0144 ? . 2_555 H(19) C(4) 2.9588 ? . 1_544 H(19) C(5) 2.9208 ? . 1_544 H(19) C(6) 2.9987 ? . 1_544 H(19) C(7) 3.1024 ? . 1_544 H(19) C(8) 3.1026 ? . 1_544 H(19) C(9) 3.0695 ? . 1_544 H(19) C(27) 3.2591 ? . . H(20) C(2) 3.3280 ? . 1_544 H(20) C(3) 3.1442 ? . 1_544 H(20) C(4) 3.3121 ? . 1_544 H(20) C(16) 3.5367 ? . 2_646 H(20) C(17) 3.5807 ? . 2_646 H(20) C(22) 3.2630 ? . . H(20) C(24) 3.2291 ? . . H(20) C(25) 2.0065 ? . . H(20) C(27) 2.0449 ? . . H(21) C(12) 3.4112 ? . 2_646 H(21) C(13) 2.9529 ? . 2_646 H(21) C(14) 3.3544 ? . 2_646 H(21) C(17) 3.4295 ? . 2_646 H(21) C(18) 3.2345 ? . 1_554 H(21) C(18) 2.9908 ? . 2_646 Tm(1) Tm(1) 4.096(1) ? . 2_656 Tm(1) Tm(1) 4.096(1) ? 2_646 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(3) H(2) O(1) 2_656 0.95 2.44 2.796(10) 102 ? C(6) H(4) O(5) 2_556 0.95 2.58 3.449(8) 152 ? C(12) H(9) O(4) . 0.95 2.49 2.830(7) 101 ? C(21) H(16) O(6) 2_646 0.95 2.50 2.824(7) 100 ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Dy-wt1290w.cif' #============================================================================== data_Dy-wt1290w _database_code_depnum_ccdc_archive 'CCDC 631232' # Kin-K367-Dy-cinnamate #============================================================================== _audit_creation_date 2006-07-31 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Dy O6 ' _chemical_formula_moiety 'C27 H21 Dy O6 ' _chemical_formula_weight 603.96 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.5204(11) _cell_length_b 7.9361(7) _cell_length_c 13.0778(12) _cell_angle_alpha 90 _cell_angle_beta 94.049(2) _cell_angle_gamma 90 _cell_volume 1192.7(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6882 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594.00 _exptl_absorpt_coefficient_mu 3.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.471 _exptl_absorpt_correction_T_max 0.621 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6882 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9728 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9728 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0\s(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0\s(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2852 _reflns_number_gt 2719 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0230 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2719 _refine_ls_number_parameters 329 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.015]' _refine_ls_shift/su_max 0.0150 _refine_diff_density_max 0.82 _refine_diff_density_min -0.44 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). ' _refine_ls_abs_structure_Flack -0.04(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Dy Dy -0.189 4.410 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Dy(1) Dy 0.540380(10) 0.48642(13) 0.475720(10) 0.02521(4) Uani 1.00 1 d . . . O(1) O 0.6789(3) 0.3130(5) 0.4168(3) 0.0404(10) Uani 1.00 1 d . . . O(2) O 0.4042(3) 0.5604(5) 0.5837(3) 0.0434(10) Uani 1.00 1 d . . . O(3) O 0.5845(3) 0.6271(5) 0.3219(3) 0.0396(9) Uani 1.00 1 d . . . O(4) O 0.4595(3) 0.7601(4) 0.4108(2) 0.0328(8) Uani 1.00 1 d . . . O(5) O 0.6704(3) 0.6300(5) 0.5789(3) 0.0419(9) Uani 1.00 1 d . . . O(6) O 0.3959(3) 0.3738(5) 0.3697(3) 0.0451(10) Uani 1.00 1 d . . . C(1) C 0.3166(4) 0.6547(6) 0.5889(4) 0.0339(12) Uani 1.00 1 d . . . C(2) C 0.2027(7) 0.5778(11) 0.6035(6) 0.037(2) Uani 1.00 1 d . . . C(3) C 0.1879(7) 0.4129(12) 0.6083(6) 0.040(2) Uani 1.00 1 d . . . C(4) C 0.0785(4) 0.3201(7) 0.6200(4) 0.0398(13) Uani 1.00 1 d . . . C(5) C -0.0290(4) 0.4001(7) 0.6166(4) 0.044(1) Uani 1.00 1 d . . . C(6) C -0.1283(5) 0.3104(9) 0.6329(5) 0.052(2) Uani 1.00 1 d . . . C(7) C -0.1214(6) 0.1393(9) 0.6528(5) 0.058(2) Uani 1.00 1 d . . . C(8) C -0.0166(6) 0.0590(9) 0.6552(6) 0.067(2) Uani 1.00 1 d . . . C(9) C 0.0844(6) 0.1476(8) 0.6387(5) 0.052(2) Uani 1.00 1 d . . . C(10) C 0.5030(4) 0.7281(6) 0.3243(3) 0.0322(11) Uani 1.00 1 d . . . C(11) C 0.4468(5) 0.8038(7) 0.2305(4) 0.0396(13) Uani 1.00 1 d . . . C(12) C 0.4735(4) 0.7543(7) 0.1386(4) 0.0390(13) Uani 1.00 1 d . . . C(13) C 0.4148(4) 0.8001(7) 0.0388(4) 0.0373(12) Uani 1.00 1 d . . . C(14) C 0.4625(5) 0.7440(9) -0.0495(4) 0.049(2) Uani 1.00 1 d . . . C(15) C 0.4085(6) 0.7804(10) -0.1450(4) 0.063(2) Uani 1.00 1 d . . . C(16) C 0.3070(6) 0.8697(9) -0.1530(4) 0.058(2) Uani 1.00 1 d . . . C(17) C 0.2581(5) 0.9244(8) -0.0666(4) 0.056(2) Uani 1.00 1 d . . . C(18) C 0.3133(5) 0.8925(8) 0.0303(4) 0.048(2) Uani 1.00 1 d . . . C(19) C 0.6687(4) 0.7485(6) 0.6426(4) 0.0323(11) Uani 1.00 1 d . . . C(20) C 0.7477(4) 0.7359(6) 0.7370(4) 0.0378(12) Uani 1.00 1 d . . . C(21) C 0.7387(4) 0.8351(7) 0.8176(4) 0.0372(12) Uani 1.00 1 d . . . C(22) C 0.8108(4) 0.8292(7) 0.9148(4) 0.0409(13) Uani 1.00 1 d . . . C(23) C 0.7705(5) 0.9071(9) 1.0001(4) 0.054(2) Uani 1.00 1 d . . . C(24) C 0.8358(6) 0.9033(10) 1.0937(5) 0.066(2) Uani 1.00 1 d . . . C(25) C 0.9417(6) 0.8222(10) 1.1019(5) 0.063(2) Uani 1.00 1 d . . . C(26) C 0.9830(7) 0.745(2) 1.0175(6) 0.060(2) Uani 1.00 1 d . . . C(27) C 0.9178(5) 0.7476(9) 0.9238(4) 0.050(2) Uani 1.00 1 d . . . H(1) H 0.1374 0.6493 0.6097 0.045 Uiso 1.00 1 c R . . H(2) H 0.2557 0.3461 0.6035 0.049 Uiso 1.00 1 c R . . H(3) H -0.0340 0.5175 0.6030 0.052 Uiso 1.00 1 c R . . H(4) H -0.2016 0.3659 0.6305 0.061 Uiso 1.00 1 c R . . H(5) H -0.1898 0.0776 0.6647 0.070 Uiso 1.00 1 c R . . H(6) H -0.0126 -0.0587 0.6682 0.080 Uiso 1.00 1 c R . . H(7) H 0.1571 0.0908 0.6402 0.063 Uiso 1.00 1 c R . . H(8) H 0.3903 0.8899 0.2362 0.048 Uiso 1.00 1 c R . . H(9) H 0.5382 0.6804 0.1367 0.047 Uiso 1.00 1 c R . . H(10) H 0.5325 0.6802 -0.0445 0.059 Uiso 1.00 1 c R . . H(11) H 0.4423 0.7431 -0.2052 0.076 Uiso 1.00 1 c R . . H(12) H 0.2703 0.8940 -0.2187 0.069 Uiso 1.00 1 c R . . H(13) H 0.1865 0.9841 -0.0724 0.067 Uiso 1.00 1 c R . . H(14) H 0.2810 0.9346 0.0901 0.057 Uiso 1.00 1 c R . . H(15) H 0.8074 0.6530 0.7397 0.045 Uiso 1.00 1 c R . . H(16) H 0.6795 0.9187 0.8120 0.044 Uiso 1.00 1 c R . . H(17) H 0.6976 0.9636 0.9947 0.064 Uiso 1.00 1 c R . . H(18) H 0.8073 0.9566 1.1520 0.079 Uiso 1.00 1 c R . . H(19) H 0.9862 0.8196 1.1659 0.074 Uiso 1.00 1 c R . . H(20) H 1.0563 0.6895 1.0232 0.070 Uiso 1.00 1 c R . . H(21) H 0.9465 0.6936 0.8659 0.059 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Dy(1) 0.03054(9) 0.02032(8) 0.02440(8) -0.0005(2) -0.00060(5) -0.0004(2) O(1) 0.045(2) 0.032(2) 0.045(2) 0.005(2) 0.007(2) 0.003(2) O(2) 0.039(2) 0.053(2) 0.039(2) 0.007(2) 0.010(2) 0.010(2) O(3) 0.047(2) 0.037(2) 0.036(2) 0.006(2) 0.006(1) 0.004(2) O(4) 0.045(2) 0.025(2) 0.029(2) -0.000(1) 0.0033(13) -0.0001(13) O(5) 0.044(2) 0.039(2) 0.041(2) -0.001(2) -0.008(1) -0.006(2) O(6) 0.050(2) 0.040(2) 0.044(2) -0.004(2) -0.012(2) -0.003(2) C(1) 0.035(2) 0.037(3) 0.030(2) 0.001(2) 0.005(2) 0.000(2) C(2) 0.035(4) 0.034(4) 0.045(4) 0.003(3) 0.010(3) 0.002(3) C(3) 0.036(4) 0.041(4) 0.046(4) 0.005(3) 0.008(3) 0.001(3) C(4) 0.038(3) 0.034(3) 0.046(3) -0.005(2) 0.002(2) 0.003(2) C(5) 0.043(3) 0.040(3) 0.048(3) -0.004(2) -0.001(2) 0.008(2) C(6) 0.039(3) 0.061(4) 0.054(3) -0.007(3) -0.005(2) 0.007(3) C(7) 0.050(3) 0.057(4) 0.067(4) -0.017(3) 0.000(3) 0.007(3) C(8) 0.076(4) 0.035(3) 0.090(5) -0.016(3) 0.004(4) 0.012(3) C(9) 0.054(3) 0.038(3) 0.066(4) 0.003(3) 0.008(3) 0.003(3) C(10) 0.045(2) 0.022(2) 0.029(2) -0.006(2) 0.001(2) -0.000(2) C(11) 0.053(3) 0.031(3) 0.035(2) 0.006(2) 0.003(2) 0.003(2) C(12) 0.045(3) 0.037(3) 0.034(2) 0.001(2) 0.001(2) 0.007(2) C(13) 0.045(3) 0.037(3) 0.030(2) -0.006(2) -0.000(2) 0.005(2) C(14) 0.055(3) 0.056(4) 0.037(3) 0.002(3) 0.004(2) 0.000(3) C(15) 0.068(4) 0.087(5) 0.034(3) -0.003(4) 0.008(3) -0.002(3) C(16) 0.066(4) 0.071(4) 0.036(3) -0.004(3) -0.007(3) 0.015(3) C(17) 0.056(3) 0.062(4) 0.050(3) 0.007(3) -0.008(3) 0.009(3) C(18) 0.056(3) 0.052(3) 0.036(3) 0.011(3) 0.001(2) -0.002(3) C(19) 0.032(2) 0.027(2) 0.037(2) -0.005(2) -0.006(2) 0.001(2) C(20) 0.038(2) 0.029(2) 0.045(3) 0.001(2) -0.011(2) 0.002(2) C(21) 0.035(2) 0.039(3) 0.036(2) 0.002(2) -0.007(2) 0.002(2) C(22) 0.046(3) 0.039(3) 0.036(3) -0.006(2) -0.010(2) 0.001(2) C(23) 0.058(3) 0.057(4) 0.046(3) 0.003(3) -0.002(3) -0.007(3) C(24) 0.086(5) 0.072(5) 0.040(3) -0.007(4) -0.000(3) -0.011(3) C(25) 0.073(4) 0.074(5) 0.038(3) -0.013(4) -0.020(3) 0.005(3) C(26) 0.050(5) 0.067(4) 0.058(6) 0.000(4) -0.017(3) 0.005(4) C(27) 0.049(3) 0.059(4) 0.040(3) 0.003(3) -0.008(2) -0.003(3) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Dy(1) O(1) 2.283(4) ? . . Dy(1) O(2) 2.261(4) ? . . Dy(1) O(3) 2.387(3) ? . . Dy(1) O(4) 2.489(3) ? . . Dy(1) O(4) 2.329(3) ? . 2_646 Dy(1) O(5) 2.254(3) ? . . Dy(1) O(6) 2.273(4) ? . . O(1) C(1) 1.260(6) ? . 2_646 O(2) C(1) 1.262(6) ? . . O(3) C(10) 1.237(6) ? . . O(4) Dy(1) 2.329(3) ? . 2_656 O(4) C(10) 1.295(5) ? . . O(5) C(19) 1.257(6) ? . . O(6) C(19) 1.246(6) ? . 2_646 C(1) O(1) 1.260(6) ? . 2_656 C(1) C(2) 1.472(9) ? . . C(2) C(3) 1.32(1) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.48(1) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.390(7) ? . . C(4) C(9) 1.391(8) ? . . C(5) C(6) 1.376(8) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.38(1) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.364(9) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.390(9) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . C(10) C(11) 1.474(6) ? . . C(11) C(12) 1.321(7) ? . . C(11) H(8) 0.9500 ? . . C(12) C(13) 1.472(7) ? . . C(12) H(9) 0.9500 ? . . C(13) C(14) 1.387(7) ? . . C(13) C(18) 1.378(8) ? . . C(14) C(15) 1.385(8) ? . . C(14) H(10) 0.9500 ? . . C(15) C(16) 1.36(1) ? . . C(15) H(11) 0.9500 ? . . C(16) C(17) 1.368(9) ? . . C(16) H(12) 0.9500 ? . . C(17) C(18) 1.400(8) ? . . C(17) H(13) 0.9500 ? . . C(18) H(14) 0.9499 ? . . C(19) O(6) 1.246(6) ? . 2_656 C(19) C(20) 1.485(6) ? . . C(20) C(21) 1.326(7) ? . . C(20) H(15) 0.9499 ? . . C(21) C(22) 1.469(7) ? . . C(21) H(16) 0.9500 ? . . C(22) C(23) 1.385(8) ? . . C(22) C(27) 1.390(8) ? . . C(23) C(24) 1.391(8) ? . . C(23) H(17) 0.9501 ? . . C(24) C(25) 1.38(1) ? . . C(24) H(18) 0.9500 ? . . C(25) C(26) 1.38(1) ? . . C(25) H(19) 0.9500 ? . . C(26) C(27) 1.391(9) ? . . C(26) H(20) 0.9500 ? . . C(27) H(21) 0.9499 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Dy(1) O(1) 154.2(1) ? . . . O(3) Dy(1) O(1) 78.6(1) ? . . . O(4) Dy(1) O(1) 131.7(1) ? . . . O(4) Dy(1) O(1) 77.4(1) ? 2_646 . . O(5) Dy(1) O(1) 93.2(1) ? . . . O(6) Dy(1) O(1) 93.2(1) ? . . . Dy(1) O(1) C(1) 130.8(3) ? . . 2_646 O(3) Dy(1) O(2) 127.1(1) ? . . . O(4) Dy(1) O(2) 74.1(1) ? . . . O(4) Dy(1) O(2) 76.8(1) ? 2_646 . . O(5) Dy(1) O(2) 87.5(1) ? . . . O(6) Dy(1) O(2) 88.4(1) ? . . . Dy(1) O(2) C(1) 141.3(3) ? . . . O(4) Dy(1) O(3) 53.2(1) ? . . . O(4) Dy(1) O(3) 155.1(1) ? 2_646 . . O(5) Dy(1) O(3) 95.5(1) ? . . . O(6) Dy(1) O(3) 81.9(1) ? . . . Dy(1) O(3) C(10) 94.3(3) ? . . . O(4) Dy(1) O(4) 150.8(1) ? 2_646 . . O(5) Dy(1) O(4) 88.9(1) ? . . . O(6) Dy(1) O(4) 84.0(1) ? . . . Dy(1) O(4) C(10) 88.2(3) ? . . . Dy(1) O(4) Dy(1) 118.2(1) ? . . 2_656 O(5) Dy(1) O(4) 92.2(1) ? . . 2_646 O(6) Dy(1) O(4) 93.0(1) ? . . 2_646 Dy(1) O(4) C(10) 136.5(3) ? . 2_646 2_646 O(6) Dy(1) O(5) 172.5(1) ? . . . Dy(1) O(5) C(19) 137.2(3) ? . . . Dy(1) O(6) C(19) 142.9(3) ? . . 2_646 O(1) C(1) O(2) 123.5(4) ? . 2_64602 2_646 O(1) C(1) C(2) 117.5(5) ? . 2_64602 2_646 O(2) C(1) O(1) 123.5(4) ? . . 2_656 O(2) C(1) C(2) 119.0(5) ? . . . O(3) C(10) O(4) 119.4(4) ? . . . O(3) C(10) C(11) 122.2(4) ? . . . C(10) O(4) Dy(1) 136.5(3) ? . . 2_656 O(4) Dy(1) O(1) 77.4(1) ? . 2_656 2_656 O(4) Dy(1) O(6) 93.0(1) ? . 2_656 2_656 O(4) Dy(1) O(2) 76.8(1) ? . 2_656 2_656 O(4) Dy(1) O(5) 92.2(1) ? . 2_656 2_656 O(4) C(10) C(11) 118.3(4) ? . . . O(5) C(19) O(6) 123.3(4) ? . . 2_656 O(5) C(19) C(20) 117.5(4) ? . . . O(6) C(19) O(5) 123.3(4) ? . 2_646 2_646 O(6) C(19) C(20) 119.1(4) ? . 2_646 2_646 C(1) O(1) Dy(1) 130.8(3) ? . 2_656 2_656 C(2) C(1) O(1) 117.5(5) ? . . 2_656 C(1) C(2) C(3) 122.4(7) ? . . . C(1) C(2) H(1) 118.8076 ? . . . H(1) C(2) C(3) 118.7854 ? . . . C(2) C(3) H(2) 116.1239 ? . . . C(2) C(3) C(4) 127.8(7) ? . . . H(2) C(3) C(4) 116.1050 ? . . . C(3) C(4) C(5) 122.3(6) ? . . . C(3) C(4) C(9) 118.5(6) ? . . . C(4) C(5) H(3) 119.7491 ? . . . C(9) C(4) C(5) 119.2(5) ? . . . C(4) C(5) C(6) 120.5(5) ? . . . C(4) C(9) H(7) 120.2052 ? . . . C(4) C(9) C(8) 119.6(6) ? . . . H(3) C(5) C(6) 119.7588 ? . . . C(5) C(6) C(7) 119.9(6) ? . . . C(5) C(6) H(4) 120.0529 ? . . . C(6) C(7) C(8) 120.2(6) ? . . . H(4) C(6) C(7) 120.0560 ? . . . C(6) C(7) H(5) 119.9130 ? . . . C(7) C(8) C(9) 120.6(6) ? . . . C(7) C(8) H(6) 119.6829 ? . . . H(5) C(7) C(8) 119.9022 ? . . . C(8) C(9) H(7) 120.2174 ? . . . H(6) C(8) C(9) 119.6791 ? . . . C(10) C(11) C(12) 121.3(5) ? . . . C(10) C(11) H(8) 119.3589 ? . . . H(8) C(11) C(12) 119.3719 ? . . . C(11) C(12) H(9) 116.1697 ? . . . C(11) C(12) C(13) 127.7(5) ? . . . H(9) C(12) C(13) 116.1651 ? . . . C(12) C(13) C(18) 122.5(5) ? . . . C(12) C(13) C(14) 118.4(5) ? . . . C(18) C(13) C(14) 119.2(5) ? . . . C(13) C(14) H(10) 119.8559 ? . . . C(13) C(14) C(15) 120.3(6) ? . . . C(13) C(18) H(14) 120.0645 ? . . . C(13) C(18) C(17) 119.8(5) ? . . . H(10) C(14) C(15) 119.8474 ? . . . C(14) C(15) C(16) 120.4(6) ? . . . C(14) C(15) H(11) 119.8307 ? . . . C(15) C(16) C(17) 120.1(5) ? . . . H(11) C(15) C(16) 119.8161 ? . . . C(15) C(16) H(12) 119.9400 ? . . . C(16) C(17) C(18) 120.2(6) ? . . . C(16) C(17) H(13) 119.9055 ? . . . H(12) C(16) C(17) 119.9600 ? . . . C(17) C(18) H(14) 120.0937 ? . . . H(13) C(17) C(18) 119.8966 ? . . . C(19) O(6) Dy(1) 142.9(3) ? . 2_656 2_656 C(20) C(19) O(6) 119.1(4) ? . . 2_656 C(19) C(20) C(21) 122.9(4) ? . . . C(19) C(20) H(15) 118.5343 ? . . . H(15) C(20) C(21) 118.5452 ? . . . C(20) C(21) H(16) 116.6625 ? . . . C(20) C(21) C(22) 126.7(5) ? . . . H(16) C(21) C(22) 116.6390 ? . . . C(21) C(22) C(27) 122.2(5) ? . . . C(21) C(22) C(23) 118.8(5) ? . . . C(27) C(22) C(23) 119.1(5) ? . . . C(22) C(23) H(17) 119.7426 ? . . . C(22) C(23) C(24) 120.5(6) ? . . . C(22) C(27) H(21) 119.8981 ? . . . C(22) C(27) C(26) 120.2(6) ? . . . H(17) C(23) C(24) 119.7530 ? . . . C(23) C(24) C(25) 120.0(6) ? . . . C(23) C(24) H(18) 119.9965 ? . . . C(24) C(25) C(26) 120.0(6) ? . . . H(18) C(24) C(25) 119.9862 ? . . . C(24) C(25) H(19) 119.9762 ? . . . C(25) C(26) C(27) 120.2(7) ? . . . C(25) C(26) H(20) 119.9032 ? . . . H(19) C(25) C(26) 119.9956 ? . . . C(26) C(27) H(21) 119.9067 ? . . . H(20) C(26) C(27) 119.8951 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Dy(1) O(2) 3.537(4) ? . 2_646 Dy(1) C(1) 3.341(5) ? . . Dy(1) C(1) 3.249(5) ? . 2_646 Dy(1) C(10) 2.769(4) ? . . Dy(1) C(10) 3.388(5) ? . 2_646 Dy(1) C(19) 3.289(5) ? . . Dy(1) C(19) 3.352(4) ? . 2_646 O(1) O(2) 2.221(5) ? . 2_646 O(1) O(3) 2.957(5) ? . . O(1) O(4) 2.883(5) ? . 2_646 O(1) O(5) 3.297(5) ? . . O(1) O(6) 3.310(5) ? . . O(1) C(2) 2.338(9) ? . 2_646 O(1) C(3) 3.55(1) ? . 2_646 O(1) C(6) 3.469(7) ? . 1_655 O(1) C(16) 3.494(7) ? . 2_645 O(1) H(1) 2.5273 ? . 2_646 O(1) H(4) 3.0562 ? . 1_655 O(1) H(7) 3.0304 ? . 2_656 O(1) H(11) 3.0610 ? . 2_645 O(1) H(12) 2.7710 ? . 2_645 O(2) Dy(1) 3.537(4) ? . 2_656 O(2) O(1) 2.221(5) ? . 2_656 O(2) O(4) 2.869(5) ? . . O(2) O(4) 2.852(5) ? . 2_646 O(2) O(5) 3.122(5) ? . . O(2) O(6) 3.162(5) ? . . O(2) O(6) 3.415(5) ? . 2_656 O(2) C(2) 2.358(9) ? . . O(2) C(3) 2.792(9) ? . . O(2) C(10) 3.060(6) ? . 2_646 O(2) C(11) 3.523(6) ? . 2_646 O(2) C(19) 3.432(6) ? . . O(2) H(1) 3.1943 ? . . O(2) H(2) 2.4391 ? . . O(2) H(8) 3.4923 ? . 2_646 O(2) H(11) 3.1221 ? . 1_556 O(3) O(4) 2.186(5) ? . . O(3) O(5) 3.437(5) ? . . O(3) O(6) 3.056(5) ? . . O(3) C(3) 3.538(9) ? . 2_656 O(3) C(11) 2.376(6) ? . . O(3) C(12) 2.822(6) ? . . O(3) C(15) 3.599(8) ? . 2_645 O(3) C(16) 3.317(7) ? . 2_645 O(3) H(2) 2.6664 ? . 2_656 O(3) H(7) 2.9972 ? . 2_656 O(3) H(8) 3.2023 ? . . O(3) H(9) 2.4793 ? . . O(3) H(11) 3.4122 ? . 2_645 O(3) H(12) 2.8914 ? . 2_645 O(4) O(1) 2.883(5) ? . 2_656 O(4) O(2) 2.852(5) ? . 2_656 O(4) O(5) 3.324(4) ? . . O(4) O(5) 3.302(5) ? . 2_656 O(4) O(6) 3.189(5) ? . . O(4) O(6) 3.339(5) ? . 2_656 O(4) C(1) 3.062(6) ? . . O(4) C(11) 2.378(6) ? . . O(4) C(12) 3.576(6) ? . . O(4) H(2) 3.3691 ? . 2_656 O(4) H(4) 3.0984 ? . 2_556 O(4) H(5) 3.5067 ? . 2_556 O(4) H(8) 2.5796 ? . . O(5) O(4) 3.302(5) ? . 2_646 O(5) O(6) 2.203(5) ? . 2_656 O(5) C(6) 3.475(7) ? . 1_655 O(5) C(20) 2.347(6) ? . . O(5) C(21) 3.559(6) ? . . O(5) H(2) 3.1056 ? . 2_656 O(5) H(3) 3.5121 ? . 1_655 O(5) H(4) 2.6231 ? . 1_655 O(5) H(8) 3.1941 ? . 2_646 O(5) H(15) 2.5445 ? . . O(6) O(2) 3.415(5) ? . 2_646 O(6) O(4) 3.339(5) ? . 2_646 O(6) O(5) 2.203(5) ? . 2_646 O(6) C(10) 3.144(6) ? . . O(6) C(20) 2.357(6) ? . 2_646 O(6) C(21) 2.822(6) ? . 2_646 O(6) H(2) 3.5643 ? . . O(6) H(5) 2.8824 ? . 2_556 O(6) H(11) 3.1216 ? . 2_645 O(6) H(15) 3.1827 ? . 2_646 O(6) H(16) 2.4974 ? . 2_646 C(1) Dy(1) 3.249(5) ? . 2_656 C(1) C(3) 2.45(1) ? . . C(1) H(1) 2.1014 ? . . C(1) H(2) 2.5585 ? . . C(1) H(4) 3.5019 ? . 2_556 C(1) H(5) 3.5820 ? . 2_556 C(1) H(11) 3.0477 ? . 1_556 C(1) H(12) 3.2264 ? . 1_556 C(2) O(1) 2.338(9) ? . 2_656 C(2) C(4) 2.51(1) ? . . C(2) C(5) 3.04(1) ? . . C(2) C(7) 3.45(1) ? . 2_556 C(2) H(2) 1.9376 ? . . C(2) H(3) 2.7686 ? . . C(2) H(5) 3.5001 ? . 2_556 C(2) H(12) 3.4723 ? . 1_556 C(2) H(18) 3.3494 ? . 2_647 C(3) O(1) 3.55(1) ? . 2_656 C(3) O(3) 3.538(9) ? . 2_646 C(3) C(5) 2.51(1) ? . . C(3) C(9) 2.47(1) ? . . C(3) H(1) 1.9642 ? . . C(3) H(3) 2.6846 ? . . C(3) H(7) 2.6182 ? . . C(3) H(18) 3.1510 ? . 2_647 C(4) C(6) 2.402(8) ? . . C(4) C(7) 2.771(8) ? . . C(4) C(8) 2.403(9) ? . . C(4) H(1) 2.7050 ? . . C(4) H(2) 2.0787 ? . . C(4) H(3) 2.0359 ? . . C(4) H(4) 3.2590 ? . . C(4) H(6) 3.2599 ? . . C(4) H(7) 2.0414 ? . . C(4) H(18) 3.3524 ? . 2_647 C(4) H(19) 2.9477 ? . 2_647 C(5) C(7) 2.389(9) ? . . C(5) C(8) 2.755(9) ? . . C(5) C(9) 2.399(8) ? . . C(5) H(1) 2.7608 ? . . C(5) H(2) 3.3250 ? . . C(5) H(4) 2.0266 ? . . C(5) H(5) 3.2460 ? . . C(5) H(7) 3.2597 ? . . C(5) H(15) 3.2560 ? . 1_455 C(5) H(19) 2.9232 ? . 2_647 C(6) O(1) 3.469(7) ? . 1_455 C(6) O(5) 3.475(7) ? . 1_455 C(6) C(8) 2.381(9) ? . . C(6) C(9) 2.767(9) ? . . C(6) H(1) 3.4154 ? . 2_546 C(6) H(3) 2.0237 ? . . C(6) H(5) 2.0318 ? . . C(6) H(6) 3.2381 ? . . C(6) H(15) 3.1686 ? . 1_455 C(6) H(19) 3.0007 ? . 2_647 C(7) C(2) 3.45(1) ? . 2_546 C(7) C(9) 2.392(9) ? . . C(7) H(1) 3.4253 ? . 2_546 C(7) H(3) 3.2461 ? . . C(7) H(4) 2.0332 ? . . C(7) H(6) 2.0111 ? . . C(7) H(7) 3.2469 ? . . C(7) H(19) 3.0941 ? . 2_647 C(8) H(3) 3.4817 ? . 2_546 C(8) H(4) 3.2374 ? . . C(8) H(5) 2.0133 ? . . C(8) H(7) 2.0401 ? . . C(8) H(19) 3.1242 ? . 2_647 C(9) H(2) 2.5911 ? . . C(9) H(3) 3.2572 ? . . C(9) H(3) 3.3371 ? . 2_546 C(9) H(5) 3.2488 ? . . C(9) H(6) 2.0349 ? . . C(9) H(12) 3.3986 ? . 1_546 C(9) H(19) 3.0574 ? . 2_647 C(10) Dy(1) 3.388(5) ? . 2_656 C(10) O(2) 3.060(6) ? . 2_656 C(10) C(12) 2.437(6) ? . . C(10) H(2) 3.0206 ? . 2_656 C(10) H(8) 2.1092 ? . . C(10) H(9) 2.5436 ? . . C(11) O(2) 3.523(6) ? . 2_656 C(11) C(13) 2.508(7) ? . . C(11) C(18) 3.024(7) ? . . C(11) H(4) 3.5011 ? . 2_556 C(11) H(9) 1.9380 ? . . C(11) H(14) 2.7577 ? . . C(11) H(16) 3.4144 ? . 2_646 C(12) C(14) 2.456(7) ? . . C(12) C(18) 2.499(7) ? . . C(12) H(8) 1.9697 ? . . C(12) H(10) 2.6025 ? . . C(12) H(10) 3.5961 ? . 2_655 C(12) H(14) 2.6781 ? . . C(12) H(16) 3.2834 ? . 2_646 C(12) H(17) 3.4289 ? . 2_646 C(13) C(15) 2.404(7) ? . . C(13) C(16) 2.775(7) ? . . C(13) C(17) 2.404(8) ? . . C(13) H(8) 2.7123 ? . . C(13) H(9) 2.0744 ? . . C(13) H(10) 2.0343 ? . . C(13) H(10) 3.0774 ? . 2_655 C(13) H(11) 3.2601 ? . . C(13) H(13) 3.2597 ? . . C(13) H(14) 2.0283 ? . . C(13) H(17) 3.5909 ? . 1_554 C(13) H(17) 2.9861 ? . 2_646 C(14) C(16) 2.386(8) ? . . C(14) C(17) 2.751(9) ? . . C(14) C(18) 2.385(8) ? . . C(14) H(9) 2.5777 ? . . C(14) H(11) 2.0324 ? . . C(14) H(12) 3.2437 ? . . C(14) H(14) 3.2458 ? . . C(14) H(16) 3.4775 ? . 1_554 C(14) H(17) 3.2384 ? . 1_554 C(14) H(17) 3.0084 ? . 2_646 C(15) O(3) 3.599(8) ? . 2_655 C(15) C(17) 2.368(9) ? . . C(15) C(18) 2.758(8) ? . . C(15) H(9) 3.2333 ? . 2_655 C(15) H(10) 2.0326 ? . . C(15) H(12) 2.0149 ? . . C(15) H(13) 3.2250 ? . . C(15) H(16) 3.3935 ? . 1_554 C(15) H(17) 3.4664 ? . 2_646 C(15) H(18) 3.5727 ? . 2_646 C(16) O(1) 3.494(7) ? . 2_655 C(16) O(3) 3.317(7) ? . 2_655 C(16) C(18) 2.400(8) ? . . C(16) H(7) 3.5656 ? . 1_564 C(16) H(9) 3.0411 ? . 2_655 C(16) H(10) 3.2401 ? . . C(16) H(11) 2.0137 ? . . C(16) H(13) 2.0178 ? . . C(16) H(14) 3.2549 ? . . C(16) H(18) 3.5338 ? . 2_646 C(17) H(9) 3.2827 ? . 2_655 C(17) H(10) 3.3997 ? . 2_655 C(17) H(11) 3.2251 ? . . C(17) H(12) 2.0183 ? . . C(17) H(14) 2.0485 ? . . C(17) H(20) 3.2631 ? . 1_454 C(18) H(8) 2.7751 ? . . C(18) H(9) 3.3122 ? . . C(18) H(10) 3.2435 ? . . C(18) H(10) 2.8905 ? . 2_655 C(18) H(12) 3.2590 ? . . C(18) H(13) 2.0467 ? . . C(18) H(17) 3.4211 ? . 2_646 C(18) H(20) 3.3668 ? . 1_454 C(19) Dy(1) 3.352(4) ? . 2_656 C(19) C(21) 2.471(6) ? . . C(19) H(2) 3.4798 ? . 2_656 C(19) H(4) 3.3930 ? . 1_655 C(19) H(5) 3.0819 ? . 1_665 C(19) H(8) 3.3508 ? . 2_646 C(19) H(11) 3.3913 ? . 1_556 C(19) H(15) 2.1105 ? . . C(19) H(16) 2.5903 ? . . C(20) O(6) 2.357(6) ? . 2_656 C(20) C(22) 2.499(7) ? . . C(20) C(27) 3.024(7) ? . . C(20) H(4) 3.3193 ? . 1_655 C(20) H(5) 2.9772 ? . 1_665 C(20) H(6) 3.3824 ? . 1_665 C(20) H(8) 3.2046 ? . 2_646 C(20) H(14) 3.3240 ? . 2_646 C(20) H(16) 1.9474 ? . . C(20) H(21) 2.7666 ? . . C(21) O(6) 2.822(6) ? . 2_656 C(21) C(23) 2.456(7) ? . . C(21) C(27) 2.503(7) ? . . C(21) H(5) 2.9348 ? . 1_665 C(21) H(10) 3.3183 ? . 1_556 C(21) H(11) 3.4840 ? . 1_556 C(21) H(14) 3.4135 ? . 2_646 C(21) H(15) 1.9661 ? . . C(21) H(17) 2.6044 ? . . C(21) H(21) 2.6788 ? . . C(22) C(24) 2.410(8) ? . . C(22) C(25) 2.783(8) ? . . C(22) C(26) 2.411(9) ? . . C(22) H(10) 3.4936 ? . 1_556 C(22) H(13) 3.4266 ? . 2_646 C(22) H(14) 3.3044 ? . 2_646 C(22) H(15) 2.6802 ? . . C(22) H(16) 2.0764 ? . . C(22) H(17) 2.0313 ? . . C(22) H(18) 3.2658 ? . . C(22) H(20) 3.2666 ? . . C(22) H(20) 3.3167 ? . 2_757 C(22) H(21) 2.0371 ? . . C(23) C(25) 2.397(9) ? . . C(23) C(26) 2.76(1) ? . . C(23) C(27) 2.391(9) ? . . C(23) H(10) 3.2976 ? . 1_556 C(23) H(13) 3.5135 ? . 2_646 C(23) H(16) 2.6066 ? . . C(23) H(18) 2.0396 ? . . C(23) H(19) 3.2557 ? . . C(23) H(20) 3.0305 ? . 2_757 C(23) H(21) 3.2509 ? . . C(24) C(26) 2.39(1) ? . . C(24) C(27) 2.766(9) ? . . C(24) H(13) 3.3467 ? . 2_646 C(24) H(17) 2.0372 ? . . C(24) H(19) 2.0259 ? . . C(24) H(20) 3.2423 ? . . C(24) H(20) 3.0517 ? . 2_757 C(24) H(21) 3.4195 ? . 2_757 C(25) C(27) 2.400(8) ? . . C(25) H(13) 3.0738 ? . 2_646 C(25) H(17) 3.2522 ? . . C(25) H(18) 2.0260 ? . . C(25) H(20) 2.0259 ? . . C(25) H(20) 3.3439 ? . 2_757 C(25) H(21) 3.2553 ? . . C(25) H(21) 3.2327 ? . 2_757 C(26) H(13) 3.2963 ? . 1_656 C(26) H(13) 2.9686 ? . 2_646 C(26) H(18) 3.2430 ? . . C(26) H(19) 2.0269 ? . . C(26) H(20) 3.5921 ? . 2_757 C(26) H(21) 2.0384 ? . . C(27) H(13) 3.1500 ? . 2_646 C(27) H(14) 3.3748 ? . 2_646 C(27) H(15) 2.7472 ? . . C(27) H(16) 3.3090 ? . . C(27) H(17) 3.2507 ? . . C(27) H(19) 3.2579 ? . . C(27) H(20) 2.0383 ? . . C(27) H(20) 3.5826 ? . 2_757 H(1) O(1) 2.5273 ? . 2_656 H(1) C(6) 3.4154 ? . 2_556 H(1) C(7) 3.4253 ? . 2_556 H(2) O(3) 2.6664 ? . 2_646 H(2) O(4) 3.3691 ? . 2_646 H(2) O(5) 3.1056 ? . 2_646 H(2) C(10) 3.0206 ? . 2_646 H(2) C(19) 3.4798 ? . 2_646 H(3) O(5) 3.5121 ? . 1_455 H(3) C(8) 3.4817 ? . 2_556 H(3) C(9) 3.3371 ? . 2_556 H(4) O(1) 3.0562 ? . 1_455 H(4) O(4) 3.0984 ? . 2_546 H(4) O(5) 2.6231 ? . 1_455 H(4) C(1) 3.5019 ? . 2_546 H(4) C(11) 3.5011 ? . 2_546 H(4) C(19) 3.3930 ? . 1_455 H(4) C(20) 3.3193 ? . 1_455 H(5) O(4) 3.5067 ? . 2_546 H(5) O(6) 2.8824 ? . 2_546 H(5) C(1) 3.5820 ? . 2_546 H(5) C(2) 3.5001 ? . 2_546 H(5) C(19) 3.0819 ? . 1_445 H(5) C(20) 2.9772 ? . 1_445 H(5) C(21) 2.9348 ? . 1_445 H(6) C(20) 3.3824 ? . 1_445 H(7) O(1) 3.0304 ? . 2_646 H(7) O(3) 2.9972 ? . 2_646 H(7) C(16) 3.5656 ? . 1_546 H(8) O(2) 3.4923 ? . 2_656 H(8) O(5) 3.1941 ? . 2_656 H(8) C(19) 3.3508 ? . 2_656 H(8) C(20) 3.2046 ? . 2_656 H(9) C(15) 3.2333 ? . 2_645 H(9) C(16) 3.0411 ? . 2_645 H(9) C(17) 3.2827 ? . 2_645 H(10) C(12) 3.5961 ? . 2_645 H(10) C(13) 3.0774 ? . 2_645 H(10) C(17) 3.3997 ? . 2_645 H(10) C(18) 2.8905 ? . 2_645 H(10) C(21) 3.3183 ? . 1_554 H(10) C(22) 3.4936 ? . 1_554 H(10) C(23) 3.2976 ? . 1_554 H(11) O(1) 3.0610 ? . 2_655 H(11) O(2) 3.1221 ? . 1_554 H(11) O(3) 3.4122 ? . 2_655 H(11) O(6) 3.1216 ? . 2_655 H(11) C(1) 3.0477 ? . 1_554 H(11) C(19) 3.3913 ? . 1_554 H(11) C(21) 3.4840 ? . 1_554 H(12) O(1) 2.7710 ? . 2_655 H(12) O(3) 2.8914 ? . 2_655 H(12) C(1) 3.2264 ? . 1_554 H(12) C(2) 3.4723 ? . 1_554 H(12) C(9) 3.3986 ? . 1_564 H(13) C(22) 3.4266 ? . 2_656 H(13) C(23) 3.5135 ? . 2_656 H(13) C(24) 3.3467 ? . 2_656 H(13) C(25) 3.0738 ? . 2_656 H(13) C(26) 3.2963 ? . 1_454 H(13) C(26) 2.9686 ? . 2_656 H(13) C(27) 3.1500 ? . 2_656 H(14) C(20) 3.3240 ? . 2_656 H(14) C(21) 3.4135 ? . 2_656 H(14) C(22) 3.3044 ? . 2_656 H(14) C(27) 3.3748 ? . 2_656 H(15) O(6) 3.1827 ? . 2_656 H(15) C(5) 3.2560 ? . 1_655 H(15) C(6) 3.1686 ? . 1_655 H(16) O(6) 2.4974 ? . 2_656 H(16) C(11) 3.4144 ? . 2_656 H(16) C(12) 3.2834 ? . 2_656 H(16) C(14) 3.4775 ? . 1_556 H(16) C(15) 3.3935 ? . 1_556 H(17) C(12) 3.4289 ? . 2_656 H(17) C(13) 3.5909 ? . 1_556 H(17) C(13) 2.9861 ? . 2_656 H(17) C(14) 3.2384 ? . 1_556 H(17) C(14) 3.0084 ? . 2_656 H(17) C(15) 3.4664 ? . 2_656 H(17) C(18) 3.4211 ? . 2_656 H(18) C(2) 3.3494 ? . 2_657 H(18) C(3) 3.1510 ? . 2_657 H(18) C(4) 3.3524 ? . 2_657 H(18) C(15) 3.5727 ? . 2_656 H(18) C(16) 3.5338 ? . 2_656 H(19) C(4) 2.9477 ? . 2_657 H(19) C(5) 2.9232 ? . 2_657 H(19) C(6) 3.0007 ? . 2_657 H(19) C(7) 3.0941 ? . 2_657 H(19) C(8) 3.1242 ? . 2_657 H(19) C(9) 3.0574 ? . 2_657 H(20) C(17) 3.2631 ? . 1_656 H(20) C(18) 3.3668 ? . 1_656 H(20) C(22) 3.3167 ? . 2_747 H(20) C(23) 3.0305 ? . 2_747 H(20) C(24) 3.0517 ? . 2_747 H(20) C(25) 3.3439 ? . 2_747 H(20) C(26) 3.5921 ? . 2_747 H(20) C(27) 3.5826 ? . 2_747 H(21) C(24) 3.4195 ? . 2_747 H(21) C(25) 3.2327 ? . 2_747 Dy(1) Dy(1) 4.135(1) ? . 2_656 Dy(1) Dy(1) 4.135(1) ? 2_646 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(3) H(2) O(2) . 0.95 2.44 2.792(9) 102 ? C(12) H(9) O(3) . 0.95 2.48 2.823(6) 101 ? C(21) H(16) O(6) 2_656 0.95 2.50 2.822(6) 100 ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data_La-wt1356w _database_code_depnum_ccdc_archive 'CCDC 632145' # -La-cinnamate (hydrothermal) #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 La O6 ' _chemical_formula_moiety 'C27 H21 La O6 ' _chemical_formula_weight 580.36 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 22.636(2) _cell_length_b 22.636(2) _cell_length_c 7.7554(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3441.4(6) _cell_formula_units_Z 6 _cell_measurement_reflns_used 6925 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728.00 _exptl_absorpt_coefficient_mu 1.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_T_max 0.981 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ' Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6925 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_max 0.9926 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.9926 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1700 _reflns_number_gt 1425 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0340 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1435 _refine_ls_number_parameters 112 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.095]' _refine_ls_shift/su_max 0.0430 _refine_diff_density_max 1.29 _refine_diff_density_min -0.48 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 39.3(73) _refine_ls_abs_structure_details 'Flack (1983). 769 Friedel Pairs' _refine_ls_abs_structure_Flack -0.15(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; La La -0.287 2.452 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 La(1) La 0.0000 0.0000 -0.0000(2) 0.01664(8) Uani 1.00 3 d S . . O(1) O 0.0804(2) 0.0595(2) 0.2647(5) 0.0312(10) Uani 1.00 1 d . . . O(2) O 0.0771(3) 0.1193(2) 0.0456(5) 0.0457(12) Uani 1.00 1 d . . . C(1) C 0.1006(3) 0.1177(3) 0.1914(6) 0.029(1) Uani 1.00 1 d . . . C(2) C 0.1508(3) 0.1810(3) 0.2760(8) 0.035(2) Uani 1.00 1 d . . . C(3) C 0.1657(3) 0.2419(3) 0.2152(8) 0.037(2) Uani 1.00 1 d . . . C(4) C 0.2129(3) 0.3090(3) 0.2907(8) 0.037(2) Uani 1.00 1 d . . . C(5) C 0.2612(4) 0.3186(3) 0.4148(9) 0.045(2) Uani 1.00 1 d . . . C(6) C 0.3036(4) 0.3830(4) 0.4835(10) 0.053(2) Uani 1.00 1 d . . . C(7) C 0.2982(4) 0.4384(4) 0.4300(9) 0.055(2) Uani 1.00 1 d . . . C(8) C 0.2501(4) 0.4293(4) 0.3077(10) 0.056(2) Uani 1.00 1 d . . . C(9) C 0.2078(4) 0.3651(3) 0.2367(9) 0.047(2) Uani 1.00 1 d . . . H(1) H 0.1732 0.1785 0.3769 0.039 Uiso 1.00 1 c R . . H(2) H 0.1435 0.2421 0.1114 0.042 Uiso 1.00 1 c R . . H(3) H 0.2653 0.2809 0.4527 0.050 Uiso 1.00 1 c R . . H(4) H 0.3365 0.3890 0.5679 0.057 Uiso 1.00 1 c R . . H(5) H 0.3274 0.4824 0.4771 0.058 Uiso 1.00 1 c R . . H(6) H 0.2457 0.4671 0.2717 0.066 Uiso 1.00 1 c R . . H(7) H 0.1753 0.3595 0.1512 0.056 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 La(1) 0.0176(2) 0.0176(2) 0.0147(2) 0.00881(7) 0.0000 0.0000 O(1) 0.029(2) 0.027(2) 0.034(2) 0.012(2) 0.002(2) 0.002(2) O(2) 0.057(3) 0.032(2) 0.035(2) 0.012(2) -0.012(2) -0.000(2) C(1) 0.028(3) 0.030(3) 0.025(3) 0.012(2) 0.003(2) 0.001(2) C(2) 0.033(3) 0.030(3) 0.036(3) 0.010(3) -0.004(2) 0.002(2) C(3) 0.036(3) 0.034(3) 0.036(4) 0.014(3) -0.003(3) -0.001(3) C(4) 0.038(3) 0.026(3) 0.041(3) 0.010(3) 0.001(3) -0.000(2) C(5) 0.048(4) 0.033(3) 0.045(4) 0.013(3) -0.005(3) 0.001(3) C(6) 0.050(4) 0.042(4) 0.050(4) 0.009(3) -0.007(4) -0.009(3) C(7) 0.057(5) 0.030(4) 0.058(5) 0.005(3) 0.010(4) -0.009(3) C(8) 0.067(5) 0.030(3) 0.067(5) 0.021(3) 0.017(4) 0.003(3) C(9) 0.052(4) 0.036(3) 0.051(4) 0.020(3) -0.001(3) 0.000(3) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 La(1) O(1) 2.625(4) ? . . La(1) O(1) 2.625(5) ? . 2_555 La(1) O(1) 2.625(4) ? . 3_555 La(1) O(1) 2.450(5) ? . 4_554 La(1) O(1) 2.450(4) ? . 5_554 La(1) O(1) 2.450(4) ? . 6_554 La(1) O(2) 2.397(4) ? . . La(1) O(2) 2.397(5) ? . 2_555 La(1) O(2) 2.397(7) ? . 3_555 O(1) La(1) 2.625(4) ? . . O(1) La(1) 2.625(4) ? . 2_555 O(1) La(1) 2.625(4) ? . 3_555 O(1) La(1) 2.450(4) ? . 4_555 O(1) C(1) 1.289(7) ? . . O(2) La(1) 2.397(4) ? . . O(2) La(1) 2.397(4) ? . 2_555 O(2) La(1) 2.397(4) ? . 3_555 O(2) C(1) 1.257(7) ? . . C(1) C(2) 1.465(7) ? . . C(2) C(3) 1.33(1) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.473(8) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.39(1) ? . . C(4) C(9) 1.40(1) ? . . C(5) C(6) 1.390(9) ? . . C(5) H(3) 0.9501 ? . . C(6) C(7) 1.38(1) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.38(1) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.392(9) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) La(1) O(1) 65.3(1) ? 2_555 . . O(1) La(1) O(1) 65.3(1) ? 3_555 . . O(1) La(1) O(1) 125.1(1) ? 4_554 . . O(1) La(1) O(1) 103.1(1) ? 5_554 . . O(1) La(1) O(1) 161.2(2) ? 6_554 . . O(2) La(1) O(1) 51.6(1) ? . . . O(2) La(1) O(1) 116.3(1) ? 2_555 . . O(2) La(1) O(1) 80.4(2) ? 3_555 . . La(1) O(1) C(1) 88.9(3) ? . . . La(1) O(1) La(1) 99.6(1) ? . . 4_555 O(1) La(1) O(1) 65.3(2) ? 3_555 . 2_555 O(1) La(1) O(1) 103.1(2) ? 4_554 . 2_555 O(1) La(1) O(1) 161.2(1) ? 5_554 . 2_555 O(1) La(1) O(1) 125.1(1) ? 6_554 . 2_555 O(2) La(1) O(1) 80.4(1) ? . . 2_555 O(2) La(1) O(1) 51.6(1) ? 2_555 . 2_555 O(2) La(1) O(1) 116.3(2) ? 3_555 . 2_555 La(1) O(1) C(1) 88.9(4) ? . 2_555 2_555 La(1) O(1) La(1) 99.6(2) ? . 2_555 4_555 O(1) La(1) O(1) 161.2(1) ? 4_554 . 3_555 O(1) La(1) O(1) 125.1(2) ? 5_554 . 3_555 O(1) La(1) O(1) 103.1(1) ? 6_554 . 3_555 O(2) La(1) O(1) 116.3(1) ? . . 3_555 O(2) La(1) O(1) 80.4(2) ? 2_555 . 3_555 O(2) La(1) O(1) 51.6(2) ? 3_555 . 3_555 La(1) O(1) C(1) 88.9(3) ? . 3_555 3_555 La(1) O(1) La(1) 99.6(2) ? . 3_555 4_555 O(1) La(1) O(1) 70.6(2) ? 5_554 . 4_554 O(1) La(1) O(1) 70.6(2) ? 6_554 . 4_554 O(2) La(1) O(1) 73.9(1) ? . . 4_554 O(2) La(1) O(1) 80.8(2) ? 2_555 . 4_554 O(2) La(1) O(1) 140.0(2) ? 3_555 . 4_554 La(1) O(1) C(1) 132.6(4) ? . 4_554 4_554 O(1) La(1) O(1) 70.6(1) ? 6_554 . 5_554 O(2) La(1) O(1) 80.8(2) ? . . 5_554 O(2) La(1) O(1) 140.0(1) ? 2_555 . 5_554 O(2) La(1) O(1) 73.9(2) ? 3_555 . 5_554 La(1) O(1) C(1) 132.6(3) ? . 5_554 5_554 O(2) La(1) O(1) 140.0(1) ? . . 6_554 O(2) La(1) O(1) 73.9(2) ? 2_555 . 6_554 O(2) La(1) O(1) 80.8(2) ? 3_555 . 6_554 La(1) O(1) C(1) 132.6(4) ? . 6_554 6_554 O(2) La(1) O(2) 117.9(2) ? 2_555 . . O(2) La(1) O(2) 117.9(2) ? 3_555 . . La(1) O(2) C(1) 100.4(4) ? . . . O(2) La(1) O(2) 117.9(2) ? 3_555 . 2_555 La(1) O(2) C(1) 100.4(4) ? . 2_555 2_555 La(1) O(2) C(1) 100.4(5) ? . 3_555 3_555 O(1) La(1) O(1) 70.6(2) ? . 4_555 2_555 O(1) La(1) O(1) 70.6(1) ? . 4_555 3_555 C(1) O(1) La(1) 132.6(4) ? . . 4_555 O(1) La(1) O(2) 73.9(2) ? . 4_555 4_555 O(1) La(1) O(2) 80.8(2) ? . 4_555 5_555 O(1) C(1) O(2) 119.1(5) ? . . . O(1) C(1) C(2) 120.4(5) ? . . . O(2) C(1) C(2) 120.5(6) ? . . . C(1) C(2) C(3) 121.7(6) ? . . . C(1) C(2) H(1) 119.1643 ? . . . H(1) C(2) C(3) 119.1681 ? . . . C(2) C(3) H(2) 116.3810 ? . . . C(2) C(3) C(4) 127.2(6) ? . . . H(2) C(3) C(4) 116.3706 ? . . . C(3) C(4) C(5) 123.0(7) ? . . . C(3) C(4) C(9) 118.2(6) ? . . . C(9) C(4) C(5) 118.8(6) ? . . . C(4) C(5) H(3) 119.8199 ? . . . C(4) C(5) C(6) 120.4(8) ? . . . C(4) C(9) C(8) 120.3(8) ? . . . C(4) C(9) H(7) 119.8555 ? . . . H(3) C(5) C(6) 119.8232 ? . . . C(5) C(6) C(7) 120.6(7) ? . . . C(5) C(6) H(4) 119.6840 ? . . . C(6) C(7) C(8) 119.4(6) ? . . . H(4) C(6) C(7) 119.6954 ? . . . C(6) C(7) H(5) 120.3015 ? . . . C(7) C(8) C(9) 120.5(9) ? . . . H(5) C(7) C(8) 120.2876 ? . . . C(7) C(8) H(6) 119.7530 ? . . . C(8) C(9) H(7) 119.8676 ? . . . H(6) C(8) C(9) 119.7446 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 La(1) La(1) 3.878(2) ? . 4_555 La(1) La(1) 3.878(2) ? 4_554 . La(1) La(1) 13.3221(4) ? . 13_554 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Ce-wt1342w.cif' #============================================================================== data_Ce-wt1342w _database_code_depnum_ccdc_archive 'CCDC 632146' # -Sonooe'sCe(S)-cinnamate #============================================================================== _audit_creation_date 2006-12-07 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Ce O6 ' _chemical_formula_moiety 'C27 H21 Ce O6 ' _chemical_formula_weight 581.58 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 22.646(2) _cell_length_b 22.646(2) _cell_length_c 7.9212(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3518.2(5) _cell_formula_units_Z 6 _cell_measurement_reflns_used 7227 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1734.00 _exptl_absorpt_coefficient_mu 1.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.888 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ' Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7227 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9990 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1742 _reflns_number_gt 1493 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0210 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1495 _refine_ls_number_parameters 111 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.0022]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.27 _refine_diff_density_min -0.91 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 783 Friedel Pairs' _refine_ls_abs_structure_Flack -0.02(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ce Ce -0.249 2.633 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ce(1) Ce 0.0000 0.0000 0.00010(10) 0.01796(4) Uani 1.00 3 d S . . O(1) O 0.08118(9) 0.06310(10) 0.2641(2) 0.0249(5) Uani 1.00 1 d . . . O(2) O 0.07945(13) 0.12242(11) 0.0480(3) 0.0402(6) Uani 1.00 1 d . . . C(1) C 0.1013(1) 0.1204(2) 0.1911(3) 0.0264(7) Uani 1.00 1 d . . . C(2) C 0.1517(1) 0.1837(2) 0.2751(4) 0.0296(7) Uani 1.00 1 d . . . C(3) C 0.1671(2) 0.2445(2) 0.2173(4) 0.0335(8) Uani 1.00 1 d . . . C(4) C 0.2141(2) 0.3111(2) 0.2917(4) 0.0336(8) Uani 1.00 1 d . . . C(5) C 0.2610(2) 0.3200(2) 0.4168(4) 0.0410(9) Uani 1.00 1 d . . . C(6) C 0.3034(2) 0.3840(2) 0.4852(5) 0.0497(10) Uani 1.00 1 d . . . C(7) C 0.2987(2) 0.4399(2) 0.4305(5) 0.0543(11) Uani 1.00 1 d . . . C(8) C 0.2532(2) 0.4318(2) 0.3083(5) 0.0521(11) Uani 1.00 1 d . . . C(9) C 0.2110(2) 0.3678(2) 0.2384(4) 0.0440(10) Uani 1.00 1 d . . . H(1) H 0.1738 0.1807 0.3740 0.035 Uiso 1.00 1 c R . . H(2) H 0.1453 0.2451 0.1155 0.040 Uiso 1.00 1 c R . . H(3) H 0.2640 0.2819 0.4557 0.049 Uiso 1.00 1 c R . . H(4) H 0.3356 0.3897 0.5695 0.060 Uiso 1.00 1 c R . . H(5) H 0.3273 0.4836 0.4785 0.065 Uiso 1.00 1 c R . . H(6) H 0.2502 0.4700 0.2704 0.063 Uiso 1.00 1 c R . . H(7) H 0.1795 0.3629 0.1527 0.053 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ce(1) 0.01944(8) 0.01944(8) 0.01500(10) 0.00972(4) 0.0000 0.0000 O(1) 0.0231(9) 0.0204(9) 0.0272(10) 0.0077(8) 0.0028(8) 0.0011(8) O(2) 0.0487(13) 0.0243(11) 0.0324(11) 0.0067(10) -0.0138(10) -0.0006(9) C(1) 0.0230(13) 0.029(2) 0.027(1) 0.0120(12) 0.0030(11) -0.0007(12) C(2) 0.028(1) 0.026(2) 0.027(1) 0.0073(12) -0.0033(11) -0.0008(11) C(3) 0.033(2) 0.030(2) 0.033(2) 0.012(1) -0.0030(12) -0.0017(12) C(4) 0.034(2) 0.024(1) 0.035(2) 0.0088(12) 0.0022(12) -0.0010(11) C(5) 0.041(2) 0.030(2) 0.042(2) 0.009(1) -0.003(1) 0.0015(13) C(6) 0.049(2) 0.040(2) 0.044(2) 0.010(2) -0.008(2) -0.008(2) C(7) 0.056(3) 0.027(2) 0.056(3) 0.003(2) 0.014(2) -0.010(2) C(8) 0.060(2) 0.024(2) 0.068(3) 0.018(2) 0.019(2) 0.001(2) C(9) 0.045(2) 0.033(2) 0.054(2) 0.019(2) 0.000(2) 0.004(2) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ce(1) O(1) 2.678(2) ? . . Ce(1) O(2) 2.466(2) ? . . O(1) Ce(1) 2.508(2) ? . 4_555 O(1) C(1) 1.278(4) ? . . O(2) C(1) 1.247(4) ? . . C(1) C(2) 1.471(4) ? . . C(2) C(3) 1.321(5) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.466(4) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.391(5) ? . . C(4) C(9) 1.387(6) ? . . C(5) C(6) 1.389(4) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.390(6) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.358(6) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.391(4) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Ce(1) O(1) 65.46(6) ? 2_555 . . O(1) Ce(1) O(1) 122.84(6) ? 4_554 . . O(1) Ce(1) O(1) 104.09(6) ? 5_554 . . O(1) Ce(1) O(1) 163.95(8) ? 6_554 . . O(2) Ce(1) O(1) 50.16(7) ? . . . O(2) Ce(1) O(1) 115.27(7) ? 2_555 . . O(2) Ce(1) O(1) 81.55(8) ? 3_555 . . Ce(1) O(1) C(1) 89.4(1) ? . . . Ce(1) O(1) Ce(1) 99.55(5) ? . . 4_555 O(1) Ce(1) O(1) 65.46(8) ? 3_555 . 2_555 O(1) Ce(1) O(1) 104.09(7) ? 4_554 . 2_555 O(1) Ce(1) O(1) 163.95(6) ? 5_554 . 2_555 O(1) Ce(1) O(1) 122.84(6) ? 6_554 . 2_555 O(2) Ce(1) O(1) 81.55(7) ? . . 2_555 O(2) Ce(1) O(1) 50.16(6) ? 2_555 . 2_555 O(2) Ce(1) O(1) 115.27(8) ? 3_555 . 2_555 Ce(1) O(1) C(1) 89.4(2) ? . 2_555 2_555 Ce(1) O(1) Ce(1) 99.55(9) ? . 2_555 4_555 O(1) Ce(1) O(1) 163.95(6) ? 4_554 . 3_555 O(1) Ce(1) O(1) 122.84(8) ? 5_554 . 3_555 O(1) Ce(1) O(1) 104.09(6) ? 6_554 . 3_555 O(2) Ce(1) O(1) 115.27(7) ? . . 3_555 O(2) Ce(1) O(1) 81.55(7) ? 2_555 . 3_555 O(2) Ce(1) O(1) 50.16(8) ? 3_555 . 3_555 Ce(1) O(1) C(1) 89.4(2) ? . 3_555 3_555 Ce(1) O(1) Ce(1) 99.55(8) ? . 3_555 4_555 O(1) Ce(1) O(1) 70.53(8) ? 5_554 . 4_554 O(1) Ce(1) O(1) 70.53(7) ? 6_554 . 4_554 O(2) Ce(1) O(1) 73.09(7) ? . . 4_554 O(2) Ce(1) O(1) 82.41(7) ? 2_555 . 4_554 O(2) Ce(1) O(1) 140.09(8) ? 3_555 . 4_554 Ce(1) O(1) C(1) 134.7(2) ? . 4_554 4_554 O(1) Ce(1) O(1) 70.53(6) ? 6_554 . 5_554 O(2) Ce(1) O(1) 82.41(8) ? . . 5_554 O(2) Ce(1) O(1) 140.09(7) ? 2_555 . 5_554 O(2) Ce(1) O(1) 73.09(8) ? 3_555 . 5_554 Ce(1) O(1) C(1) 134.7(2) ? . 5_554 5_554 O(2) Ce(1) O(1) 140.09(7) ? . . 6_554 O(2) Ce(1) O(1) 73.09(7) ? 2_555 . 6_554 O(2) Ce(1) O(1) 82.41(8) ? 3_555 . 6_554 Ce(1) O(1) C(1) 134.7(2) ? . 6_554 6_554 O(2) Ce(1) O(2) 117.7(1) ? 2_555 . . O(2) Ce(1) O(2) 117.68(9) ? 3_555 . . Ce(1) O(2) C(1) 100.3(2) ? . . . O(2) Ce(1) O(2) 117.68(8) ? 3_555 . 2_555 Ce(1) O(2) C(1) 100.3(2) ? . 2_555 2_555 Ce(1) O(2) C(1) 100.3(3) ? . 3_555 3_555 O(1) Ce(1) O(1) 70.53(7) ? . 4_555 2_555 O(1) Ce(1) O(1) 70.53(6) ? . 4_555 3_555 C(1) O(1) Ce(1) 134.7(2) ? . . 4_555 O(1) Ce(1) O(2) 73.09(8) ? . 4_555 4_555 O(1) Ce(1) O(2) 82.41(8) ? . 4_555 5_555 O(1) C(1) O(2) 120.1(2) ? . . . O(1) C(1) C(2) 119.6(3) ? . . . O(2) C(1) C(2) 120.3(3) ? . . . C(1) C(2) C(3) 122.1(3) ? . . . C(1) C(2) H(1) 118.9538 ? . . . H(1) C(2) C(3) 118.9540 ? . . . C(2) C(3) H(2) 116.1604 ? . . . C(2) C(3) C(4) 127.7(3) ? . . . H(2) C(3) C(4) 116.1611 ? . . . C(3) C(4) C(5) 122.9(3) ? . . . C(3) C(4) C(9) 119.0(3) ? . . . C(9) C(4) C(5) 118.1(3) ? . . . C(4) C(5) H(3) 119.7454 ? . . . C(4) C(5) C(6) 120.5(4) ? . . . C(4) C(9) H(7) 119.4398 ? . . . C(4) C(9) C(8) 121.1(4) ? . . . H(3) C(5) C(6) 119.7451 ? . . . C(5) C(6) C(7) 120.2(4) ? . . . C(5) C(6) H(4) 119.9140 ? . . . C(6) C(7) C(8) 119.7(3) ? . . . H(4) C(6) C(7) 119.9145 ? . . . C(6) C(7) H(5) 120.1290 ? . . . C(7) C(8) C(9) 120.3(4) ? . . . H(5) C(7) C(8) 120.1282 ? . . . C(7) C(8) H(6) 119.8413 ? . . . C(8) C(9) H(7) 119.4390 ? . . . H(6) C(8) C(9) 119.8408 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ce(1) Ce(1) 3.961(1) ? . 4_555 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Nd-wt1353w.cif' #============================================================================== data_Nd-wt1353w _database_code_depnum_ccdc_archive 'CCDC 632147' # -Nd-cinnamate (hydrothermal) 21-12-2006 #============================================================================== _audit_creation_date 2006-12-28 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Nd O6 ' _chemical_formula_moiety 'C27 H21 Nd O6 ' _chemical_formula_weight 585.70 _chemical_melting_point ? _chemical_absolute_configuration ad #''CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 22.657(3) _cell_length_b 22.657(3) _cell_length_c 7.830(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3481.3(9) _cell_formula_units_Z 6 _cell_measurement_reflns_used 7574 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1746.00 _exptl_absorpt_coefficient_mu 2.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.955 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ' Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7574 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.9947 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.9947 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1702 _reflns_number_gt 1234 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0150 _refine_ls_wR_factor_ref 0.0170 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1236 _refine_ls_number_parameters 111 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 0.35\s(Fo^2^) + 0.0001]' _refine_ls_shift/su_max 0.0130 _refine_diff_density_max 0.71 _refine_diff_density_min -0.65 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 758 Friedel Pairs' _refine_ls_abs_structure_Flack -0.04(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Nd Nd -0.194 3.018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Nd(1) Nd 0.0000 0.0000 -0.00002(10) 0.01708(4) Uani 1.00 3 d S . . O(1) O 0.07819(13) 0.12069(12) 0.0460(3) 0.0369(7) Uani 1.00 1 d . . . O(2) O 0.08074(11) 0.06138(11) 0.2633(3) 0.0230(5) Uani 1.00 1 d . . . C(1) C 0.1006(2) 0.1187(2) 0.1898(4) 0.0236(8) Uani 1.00 1 d . . . C(2) C 0.1515(2) 0.1824(2) 0.2743(4) 0.0265(9) Uani 1.00 1 d . . . C(3) C 0.1663(2) 0.2428(2) 0.2163(4) 0.0302(10) Uani 1.00 1 d . . . C(4) C 0.2134(2) 0.3099(2) 0.2910(4) 0.0319(9) Uani 1.00 1 d . . . C(5) C 0.2614(2) 0.3190(2) 0.4154(5) 0.0368(10) Uani 1.00 1 d . . . C(6) C 0.3033(2) 0.3834(2) 0.4828(5) 0.0461(11) Uani 1.00 1 d . . . C(7) C 0.2981(2) 0.4388(2) 0.4306(5) 0.0481(13) Uani 1.00 1 d . . . C(8) C 0.2514(2) 0.4299(2) 0.3083(6) 0.0464(12) Uani 1.00 1 d . . . C(9) C 0.2093(2) 0.3662(2) 0.2377(5) 0.0399(11) Uani 1.00 1 d . . . H(1) H 0.1741 0.1796 0.3734 0.032 Uiso 1.00 1 c R . . H(2) H 0.1439 0.2432 0.1141 0.036 Uiso 1.00 1 c R . . H(3) H 0.2653 0.2813 0.4537 0.044 Uiso 1.00 1 c R . . H(4) H 0.3363 0.3895 0.5664 0.055 Uiso 1.00 1 c R . . H(5) H 0.3266 0.4825 0.4791 0.058 Uiso 1.00 1 c R . . H(6) H 0.2477 0.4678 0.2711 0.056 Uiso 1.00 1 c R . . H(7) H 0.1773 0.3610 0.1521 0.048 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nd(1) 0.01862(7) 0.01862(7) 0.01400(9) 0.00931(4) 0.0000 0.0000 O(1) 0.048(2) 0.0223(12) 0.0271(13) 0.0079(11) -0.0108(11) 0.0017(10) O(2) 0.0209(11) 0.0196(10) 0.0252(11) 0.0076(9) 0.0011(10) -0.0003(10) C(1) 0.022(2) 0.025(2) 0.024(2) 0.012(1) 0.0058(13) -0.0004(13) C(2) 0.027(2) 0.025(2) 0.024(2) 0.010(2) -0.0037(13) -0.0013(13) C(3) 0.029(2) 0.029(2) 0.029(2) 0.012(2) -0.003(1) -0.001(2) C(4) 0.033(2) 0.022(2) 0.034(2) 0.009(1) 0.003(2) -0.001(1) C(5) 0.040(2) 0.028(2) 0.037(2) 0.012(2) -0.002(2) 0.002(2) C(6) 0.042(2) 0.042(2) 0.040(2) 0.010(2) -0.007(2) -0.010(2) C(7) 0.050(3) 0.022(2) 0.051(3) 0.002(2) 0.008(2) -0.009(2) C(8) 0.054(3) 0.023(2) 0.060(3) 0.017(2) 0.017(2) 0.001(2) C(9) 0.040(2) 0.036(2) 0.045(2) 0.019(2) 0.000(2) 0.002(2) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nd(1) Nd(1) 3.915(1) ? . 4_554 Nd(1) Nd(1) 3.915(1) ? . 4_555 Nd(1) Nd(1) 3.915(1) ? . 5_554 Nd(1) Nd(1) 3.915(1) ? . 5_555 Nd(1) Nd(1) 3.915(1) ? . 6_554 Nd(1) Nd(1) 3.915(1) ? . 6_555 Nd(1) O(1) 2.429(2) ? . . Nd(1) O(1) 2.429(3) ? . 2_555 Nd(1) O(1) 2.429(3) ? . 3_555 Nd(1) O(2) 2.644(2) ? . . Nd(1) O(2) 2.644(3) ? . 2_555 Nd(1) O(2) 2.644(2) ? . 3_555 Nd(1) O(2) 2.484(3) ? . 4_554 Nd(1) O(2) 2.484(2) ? . 5_554 Nd(1) O(2) 2.484(2) ? . 6_554 O(1) Nd(1) 2.429(2) ? . . O(1) Nd(1) 2.429(2) ? . 2_555 O(1) Nd(1) 2.429(2) ? . 3_555 O(1) C(1) 1.245(4) ? . . O(2) Nd(1) 2.644(2) ? . . O(2) Nd(1) 2.644(2) ? . 2_555 O(2) Nd(1) 2.644(2) ? . 3_555 O(2) Nd(1) 2.484(2) ? . 4_555 O(2) C(1) 1.280(4) ? . . C(1) C(2) 1.477(4) ? . . C(2) C(3) 1.316(6) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.473(4) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.395(6) ? . . C(4) C(9) 1.390(7) ? . . C(5) C(6) 1.386(5) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.381(8) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.366(7) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.385(5) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Nd(1) Nd(1) Nd(1) 180.0000 ? 4_555 . 4_554 O(1) Nd(1) Nd(1) 98.54(6) ? . . 4_554 O(1) Nd(1) Nd(1) 98.54(6) ? 2_555 . 4_554 O(1) Nd(1) Nd(1) 98.54(6) ? 3_555 . 4_554 O(2) Nd(1) Nd(1) 141.26(5) ? . . 4_554 O(2) Nd(1) Nd(1) 141.26(6) ? 2_555 . 4_554 O(2) Nd(1) Nd(1) 141.26(5) ? 3_555 . 4_554 Nd(1) Nd(1) O(2) 38.74(6) ? . 4_554 4_554 O(2) Nd(1) Nd(1) 41.76(6) ? 4_554 . 4_554 Nd(1) Nd(1) O(2) 38.74(5) ? . 4_554 5_554 O(2) Nd(1) Nd(1) 41.76(6) ? 5_554 . 4_554 Nd(1) Nd(1) O(2) 38.74(5) ? . 4_554 6_554 O(2) Nd(1) Nd(1) 41.76(5) ? 6_554 . 4_554 O(1) Nd(1) Nd(1) 81.46(6) ? . . 555 O(1) Nd(1) Nd(1) 81.46(6) ? 2_555 . 4_555 O(1) Nd(1) Nd(1) 81.46(6) ? 3_555 . 4_555 Nd(1) Nd(1) O(2) 41.76(5) ? . 4_555 . O(2) Nd(1) Nd(1) 38.74(5) ? . . 4_555 Nd(1) Nd(1) O(2) 41.76(6) ? . 4_555 2_555 O(2) Nd(1) Nd(1) 38.74(6) ? 2_555 . 4_555 Nd(1) Nd(1) O(2) 41.76(6) ? . 4_555 3_555 O(2) Nd(1) Nd(1) 38.74(5) ? 3_555 . 4_555 O(2) Nd(1) Nd(1) 138.24(6) ? 4_554 . 4_555 O(2) Nd(1) Nd(1) 138.24(6) ? 5_554 . 4_555 O(2) Nd(1) Nd(1) 138.24(5) ? 6_554 . 4_555 Nd(1) Nd(1) O(1) 98.54(6) ? . 4_555 4_555 Nd(1) Nd(1) O(1) 98.54(6) ? . 4_555 5_555 O(1) Nd(1) O(1) 117.8(1) ? 2_555 . . O(1) Nd(1) O(1) 117.84(9) ? 3_555 . . O(2) Nd(1) O(1) 50.86(8) ? . . . O(2) Nd(1) O(1) 81.11(8) ? 2_555 . . O(2) Nd(1) O(1) 116.00(8) ? 3_555 . . O(2) Nd(1) O(1) 73.38(8) ? 4_554 . . O(2) Nd(1) O(1) 81.59(8) ? 5_554 . . O(2) Nd(1) O(1) 139.85(8) ? 6_554 . . Nd(1) O(1) C(1) 100.1(2) ? . . . O(1) Nd(1) O(1) 117.84(9) ? 3_555 . 555 O(2) Nd(1) O(1) 116.00(8) ? . . 2_555 O(2) Nd(1) O(1) 50.86(7) ? 555 . 555 O(2) Nd(1) O(1) 81.11(8) ? 3_555 . 2_555 O(2) Nd(1) O(1) 81.59(8) ? 4_554 . 2_555 O(2) Nd(1) O(1) 139.85(8) ? 5_554 . 2_555 O(2) Nd(1) O(1) 73.38(8) ? 6_554 . 2_555 Nd(1) O(1) C(1) 100.1(2) ? . 2_555 2_555 O(2) Nd(1) O(1) 81.11(8) ? . . 3_555 O(2) Nd(1) O(1) 116.00(9) ? 2_555 . 3_555 O(2) Nd(1) O(1) 50.86(8) ? 3_555 . 3_555 O(2) Nd(1) O(1) 139.85(9) ? 4_554 . 3_555 O(2) Nd(1) O(1) 73.38(9) ? 5_554 . 3_555 O(2) Nd(1) O(1) 81.59(9) ? 6_554 . 3_555 Nd(1) O(1) C(1) 100.1(3) ? . 3_555 3_555 Nd(1) O(2) Nd(1) 99.51(7) ? . . 4_555 O(2) Nd(1) O(2) 65.62(8) ? 2_555 . . O(2) Nd(1) O(2) 65.62(7) ? 3_555 . . O(2) Nd(1) O(2) 123.84(7) ? 4_554 . . O(2) Nd(1) O(2) 103.54(7) ? 5_554 . . O(2) Nd(1) O(2) 162.7(1) ? 6_554 . . Nd(1) O(2) C(1) 89.0(2) ? . . . Nd(1) O(2) Nd(1) 99.5(1) ? . 2_555 4_555 O(2) Nd(1) O(2) 65.62(9) ? 3_555 . 2_555 O(2) Nd(1) O(2) 103.54(9) ? 4_554 . 2_555 O(2) Nd(1) O(2) 162.68(6) ? 5_554 . 2_555 O(2) Nd(1) O(2) 123.84(7) ? 6_554 . 2_555 Nd(1) O(2) C(1) 89.0(2) ? . 2_555 2_555 Nd(1) O(2) Nd(1) 99.51(9) ? . 3_555 4_555 O(2) Nd(1) O(2) 162.68(7) ? 4_554 . 555 O(2) Nd(1) O(2) 123.84(9) ? 5_554 . 555 O(2) Nd(1) O(2) 103.54(7) ? 6_554 . 555 Nd(1) O(2) C(1) 89.0(2) ? . 3_555 3_555 Nd(1) O(2) Nd(1) 99.5(1) ? . 4_554 4_554 O(2) Nd(1) O(2) 70.44(9) ? 5_554 . 4_554 O(2) Nd(1) O(2) 70.44(8) ? 6_554 . 4_554 Nd(1) O(2) C(1) 133.7(2) ? . 4_554 4_554 Nd(1) O(2) Nd(1) 99.51(9) ? . 5_554 4_554 O(2) Nd(1) O(2) 70.44(7) ? 6_554 . 5_554 Nd(1) O(2) C(1) 133.7(2) ? . 5_554 5_554 Nd(1) O(2) Nd(1) 99.51(7) ? . 6_554 4_554 Nd(1) O(2) C(1) 133.7(3) ? . 6_554 6_554 O(1) C(1) O(2) 120.0(3) ? . . . O(1) C(1) C(2) 120.2(3) ? . . . O(2) Nd(1) O(2) 70.44(8) ? . 4_555 2_555 O(2) Nd(1) O(2) 70.44(7) ? . 4_555 3_555 C(1) O(2) Nd(1) 133.7(3) ? . . 4_555 O(2) Nd(1) O(1) 73.38(8) ? . 4_555 4_555 O(2) Nd(1) O(1) 81.59(9) ? . 4_555 5_555 O(2) C(1) C(2) 119.8(3) ? . . . C(1) C(2) C(3) 122.0(3) ? . . . C(1) C(2) H(1) 119.0080 ? . . . H(1) C(2) C(3) 119.0069 ? . . . C(2) C(3) H(2) 116.1048 ? . . . C(2) C(3) C(4) 127.8(3) ? . . . H(2) C(3) C(4) 116.1047 ? . . . C(3) C(4) C(5) 122.6(4) ? . . . C(3) C(4) C(9) 118.8(4) ? . . . C(9) C(4) C(5) 118.6(3) ? . . . C(4) C(5) H(3) 120.1715 ? . . . C(4) C(5) C(6) 119.7(4) ? . . . C(4) C(9) H(7) 119.7129 ? . . . C(4) C(9) C(8) 120.6(4) ? . . . H(3) C(5) C(6) 120.1717 ? . . . C(5) C(6) C(7) 121.3(4) ? . . . C(5) C(6) H(4) 119.3646 ? . . . C(6) C(7) C(8) 119.0(4) ? . . . H(4) C(6) C(7) 119.3649 ? . . . C(6) C(7) H(5) 120.4946 ? . . . C(7) C(8) C(9) 120.9(5) ? . . . H(5) C(7) C(8) 120.4943 ? . . . C(7) C(8) H(6) 119.5588 ? . . . C(8) C(9) H(7) 119.7134 ? . . . H(6) C(8) C(9) 119.5585 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Nd(1) Nd(1) 3.915(1) ? . 4_555 Nd(1) Nd(1) 3.915(1) ? 4_554 . Nd(1) Nd(1) 13.3391(2) ? . 13_554 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Sm-wt1352w.cif' #============================================================================== data_Sm-wt1352w _database_code_depnum_ccdc_archive 'CCDC 632148' # -Sm-cinnamate(hydrothermal) 20-12-2006 #============================================================================== _audit_creation_date 2006-12-28 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 O6 Sm ' _chemical_formula_moiety 'C27 H21 O6 Sm ' _chemical_formula_weight 591.86 _chemical_melting_point ? _chemical_absolute_configuration ad #''CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 22.646(2) _cell_length_b 22.646(2) _cell_length_c 7.7670(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3449.5(7) _cell_formula_units_Z 6 _cell_measurement_reflns_used 6304 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1758.00 _exptl_absorpt_coefficient_mu 2.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ' Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6304 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9958 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9958 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 5 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1434 _reflns_number_gt 1078 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0150 _refine_ls_wR_factor_ref 0.0180 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1081 _refine_ls_number_parameters 111 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 0.5\s(Fo^2^) + 0.0005]' _refine_ls_shift/su_max 0.0280 _refine_diff_density_max 1.31 _refine_diff_density_min -0.94 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 505 Friedel Pairs' _refine_ls_abs_structure_Flack -0.05(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Sm Sm -0.164 3.442 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Sm(1) Sm 0.0000 0.0000 -0.00004(13) 0.01710(5) Uani 1.00 3 d S . . O(1) O 0.0774(2) 0.1191(1) 0.0455(4) 0.0358(8) Uani 1.00 1 d . . . O(2) O 0.08053(12) 0.06021(12) 0.2649(4) 0.0240(7) Uani 1.00 1 d . . . C(1) C 0.1000(2) 0.1175(2) 0.1906(5) 0.0249(10) Uani 1.00 1 d . . . C(2) C 0.1511(2) 0.1814(2) 0.2755(5) 0.0264(10) Uani 1.00 1 d . . . C(3) C 0.1658(2) 0.2417(2) 0.2160(5) 0.0298(11) Uani 1.00 1 d . . . C(4) C 0.2128(2) 0.3088(2) 0.2903(5) 0.0308(11) Uani 1.00 1 d . . . C(5) C 0.2083(2) 0.3650(2) 0.2381(6) 0.0393(13) Uani 1.00 1 d . . . C(6) C 0.2502(3) 0.4291(2) 0.3080(7) 0.046(2) Uani 1.00 1 d . . . C(7) C 0.2974(2) 0.4384(2) 0.4298(6) 0.046(1) Uani 1.00 1 d . . . C(8) C 0.3033(2) 0.3830(2) 0.4830(6) 0.0462(13) Uani 1.00 1 d . . . C(9) C 0.2613(2) 0.3186(2) 0.4147(5) 0.0348(12) Uani 1.00 1 d . . . H(1) H 0.1740 0.1788 0.3753 0.032 Uiso 1.00 1 c R . . H(2) H 0.1432 0.2419 0.1130 0.036 Uiso 1.00 1 c R . . H(3) H 0.1759 0.3596 0.1528 0.047 Uiso 1.00 1 c R . . H(4) H 0.2461 0.4668 0.2707 0.055 Uiso 1.00 1 c R . . H(5) H 0.3259 0.4822 0.4779 0.055 Uiso 1.00 1 c R . . H(6) H 0.3364 0.3893 0.5669 0.055 Uiso 1.00 1 c R . . H(7) H 0.2655 0.2811 0.4530 0.042 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sm(1) 0.01833(8) 0.01833(8) 0.01464(12) 0.00917(4) 0.0000 0.0000 O(1) 0.044(2) 0.025(1) 0.026(2) 0.0079(12) -0.0120(13) -0.0015(12) O(2) 0.0229(12) 0.0201(12) 0.027(2) 0.0092(10) 0.0018(12) 0.0010(12) C(1) 0.023(2) 0.027(2) 0.026(2) 0.013(2) 0.004(2) -0.001(2) C(2) 0.025(2) 0.024(2) 0.024(2) 0.008(2) -0.004(2) -0.003(2) C(3) 0.028(2) 0.029(2) 0.029(3) 0.012(2) -0.004(2) -0.001(2) C(4) 0.033(2) 0.022(2) 0.030(3) 0.007(2) 0.003(2) -0.000(2) C(5) 0.043(2) 0.033(2) 0.043(3) 0.020(2) 0.000(2) 0.001(2) C(6) 0.054(3) 0.024(2) 0.060(4) 0.019(2) 0.017(3) 0.007(2) C(7) 0.047(3) 0.025(2) 0.048(3) 0.004(2) 0.010(3) -0.009(2) C(8) 0.041(3) 0.039(3) 0.043(3) 0.008(2) -0.007(2) -0.006(2) C(9) 0.036(2) 0.027(2) 0.034(3) 0.010(2) -0.004(2) 0.001(2) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Sm(1) Sm(1) 3.884(1) ? . 4_554 Sm(1) Sm(1) 3.884(1) ? . 4_555 Sm(1) Sm(1) 3.884(1) ? . 5_554 Sm(1) Sm(1) 3.884(1) ? . 5_555 Sm(1) Sm(1) 3.884(1) ? . 6_554 Sm(1) Sm(1) 3.884(1) ? . 6_555 Sm(1) O(1) 2.397(3) ? . . Sm(1) O(1) 2.397(3) ? . 2_555 Sm(1) O(1) 2.397(4) ? . 3_555 Sm(1) O(2) 2.633(3) ? . . Sm(1) O(2) 2.633(3) ? . 2_555 Sm(1) O(2) 2.633(3) ? . 3_555 Sm(1) O(2) 2.456(3) ? . 4_554 Sm(1) O(2) 2.456(3) ? . 5_554 Sm(1) O(2) 2.456(3) ? . 6_554 O(1) Sm(1) 2.397(3) ? . . O(1) Sm(1) 2.397(3) ? . 2_555 O(1) Sm(1) 2.397(3) ? . 3_555 O(1) C(1) 1.245(5) ? . . O(2) Sm(1) 2.633(3) ? . . O(2) Sm(1) 2.633(3) ? . 2_555 O(2) Sm(1) 2.633(3) ? . 3_555 O(2) Sm(1) 2.456(3) ? . 4_555 O(2) C(1) 1.281(5) ? . . C(1) C(2) 1.480(5) ? . . C(2) C(3) 1.319(6) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.468(5) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.389(8) ? . . C(4) C(9) 1.394(6) ? . . C(5) C(6) 1.387(6) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.361(8) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.389(8) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.387(5) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Sm(1) Sm(1) Sm(1) 180.0000 ? 4_555 . 4_554 O(1) Sm(1) Sm(1) 98.49(7) ? . . 4_554 O(1) Sm(1) Sm(1) 98.49(7) ? 2_555 . 4_554 O(1) Sm(1) Sm(1) 98.49(7) ? 3_555 . 4_554 O(2) Sm(1) Sm(1) 141.40(5) ? . . 4_554 O(2) Sm(1) Sm(1) 141.40(7) ? 2_555 . 4_554 O(2) Sm(1) Sm(1) 141.40(6) ? 3_555 . 4_554 Sm(1) Sm(1) O(2) 38.60(7) ? . 4_554 4_554 O(2) Sm(1) Sm(1) 41.98(7) ? 4_554 . 4_554 Sm(1) Sm(1) O(2) 38.60(6) ? . 4_554 5_554 O(2) Sm(1) Sm(1) 41.98(7) ? 5_554 . 4_554 Sm(1) Sm(1) O(2) 38.60(5) ? . 4_554 6_554 O(2) Sm(1) Sm(1) 41.98(6) ? 6_554 . 4_554 O(1) Sm(1) Sm(1) 81.51(7) ? . . 4_555 O(1) Sm(1) Sm(1) 81.51(7) ? 2_555 . 4_555 O(1) Sm(1) Sm(1) 81.51(7) ? 3_555 . 4_555 Sm(1) Sm(1) O(2) 41.98(6) ? . 4_555 . O(2) Sm(1) Sm(1) 38.60(5) ? . . 4_555 Sm(1) Sm(1) O(2) 41.98(7) ? . 4_555 2_555 O(2) Sm(1) Sm(1) 38.60(7) ? 2_555 . 4_555 Sm(1) Sm(1) O(2) 41.98(7) ? . 4_555 3_555 O(2) Sm(1) Sm(1) 38.60(6) ? 3_555 . 4_555 O(2) Sm(1) Sm(1) 138.02(7) ? 4_554 . 4_555 O(2) Sm(1) Sm(1) 138.02(7) ? 5_554 . 4_555 O(2) Sm(1) Sm(1) 138.02(6) ? 6_554 . 4_555 Sm(1) Sm(1) O(1) 98.49(7) ? . 4_555 4_555 Sm(1) Sm(1) O(1) 98.49(7) ? . 4_555 5_555 O(1) Sm(1) O(1) 117.9(1) ? 2_555 . . O(1) Sm(1) O(1) 117.9(1) ? 3_555 . . O(2) Sm(1) O(1) 51.26(9) ? . . . O(2) Sm(1) O(1) 80.76(9) ? 2_555 . . O(2) Sm(1) O(1) 116.11(9) ? 3_555 . . O(2) Sm(1) O(1) 73.73(9) ? 4_554 . . O(2) Sm(1) O(1) 80.91(9) ? 5_554 . . O(2) Sm(1) O(1) 140.1(1) ? 6_554 . . Sm(1) O(1) C(1) 100.4(2) ? . . . O(1) Sm(1) O(1) 117.9(1) ? 3_555 . 2_555 O(2) Sm(1) O(1) 116.1(1) ? . . 2_555 O(2) Sm(1) O(1) 51.26(8) ? 2_555 . 2_555 O(2) Sm(1) O(1) 80.8(1) ? 3_555 . 2_555 O(2) Sm(1) O(1) 80.9(1) ? 4_554 . 2_555 O(2) Sm(1) O(1) 140.1(1) ? 5_554 . 2_555 O(2) Sm(1) O(1) 73.7(1) ? 6_554 . 2_555 Sm(1) O(1) C(1) 100.4(2) ? . 2_555 2_555 O(2) Sm(1) O(1) 80.8(1) ? . . 3_555 O(2) Sm(1) O(1) 116.1(1) ? 2_555 . 3_555 O(2) Sm(1) O(1) 51.3(1) ? 3_555 . 3_555 O(2) Sm(1) O(1) 140.1(1) ? 4_554 . 3_555 O(2) Sm(1) O(1) 73.7(1) ? 5_554 . 3_555 O(2) Sm(1) O(1) 80.9(1) ? 6_554 . 3_555 Sm(1) O(1) C(1) 100.4(3) ? . 3_555 3_555 Sm(1) O(2) Sm(1) 99.42(7) ? . . 4_555 O(2) Sm(1) O(2) 65.41(9) ? 2_555 . . O(2) Sm(1) O(2) 65.41(7) ? 3_555 . . O(2) Sm(1) O(2) 124.54(8) ? 4_554 . . O(2) Sm(1) O(2) 103.11(8) ? 5_554 . . O(2) Sm(1) O(2) 161.6(1) ? 6_554 . . Sm(1) O(2) C(1) 88.3(2) ? . . . Sm(1) O(2) Sm(1) 99.4(1) ? . 2_555 4_555 O(2) Sm(1) O(2) 65.4(1) ? 3_555 . 2_555 O(2) Sm(1) O(2) 103.1(1) ? 4_554 . 2_555 O(2) Sm(1) O(2) 161.65(7) ? 5_554 . 2_555 O(2) Sm(1) O(2) 124.54(8) ? 6_554 . 2_555 Sm(1) O(2) C(1) 88.3(2) ? . 2_555 2_555 Sm(1) O(2) Sm(1) 99.4(1) ? . 3_555 4_555 O(2) Sm(1) O(2) 161.65(8) ? 4_554 . 3_555 O(2) Sm(1) O(2) 124.5(1) ? 5_554 . 3_555 O(2) Sm(1) O(2) 103.11(8) ? 6_554 . 3_555 Sm(1) O(2) C(1) 88.3(2) ? . 3_555 3_555 Sm(1) O(2) Sm(1) 99.4(1) ? . 4_554 4_554 O(2) Sm(1) O(2) 70.8(1) ? 5_554 . 4_554 O(2) Sm(1) O(2) 70.79(9) ? 6_554 . 4_554 Sm(1) O(2) C(1) 132.9(2) ? . 4_554 4_554 Sm(1) O(2) Sm(1) 99.4(1) ? . 5_554 4_554 O(2) Sm(1) O(2) 70.79(8) ? 6_554 . 5_554 Sm(1) O(2) C(1) 132.9(2) ? . 5_554 5_554 Sm(1) O(2) Sm(1) 99.42(7) ? . 6_554 4_554 Sm(1) O(2) C(1) 132.9(3) ? . 6_554 6_554 O(1) C(1) O(2) 119.9(3) ? . . . O(1) C(1) C(2) 120.5(4) ? . . . O(2) Sm(1) O(2) 70.79(9) ? . 4_555 2_555 O(2) Sm(1) O(2) 70.79(8) ? . 4_555 3_555 C(1) O(2) Sm(1) 132.9(3) ? . . 4_555 O(2) Sm(1) O(1) 73.7(1) ? . 4_555 4_555 O(2) Sm(1) O(1) 80.9(1) ? . 4_555 5_555 O(2) C(1) C(2) 119.6(4) ? . . . C(1) C(2) C(3) 121.6(4) ? . . . C(1) C(2) H(1) 119.1812 ? . . . H(1) C(2) C(3) 119.1802 ? . . . C(2) C(3) H(2) 116.1741 ? . . . C(2) C(3) C(4) 127.7(4) ? . . . H(2) C(3) C(4) 116.1752 ? . . . C(3) C(4) C(5) 119.1(4) ? . . . C(3) C(4) C(9) 123.0(4) ? . . . C(9) C(4) C(5) 117.9(4) ? . . . C(4) C(5) C(6) 121.3(5) ? . . . C(4) C(5) H(3) 119.3471 ? . . . C(4) C(9) H(7) 119.8567 ? . . . C(4) C(9) C(8) 120.3(5) ? . . . H(3) C(5) C(6) 119.3477 ? . . . C(5) C(6) C(7) 120.5(5) ? . . . C(5) C(6) H(4) 119.7654 ? . . . C(6) C(7) C(8) 119.3(4) ? . . . H(4) C(6) C(7) 119.7650 ? . . . C(6) C(7) H(5) 120.3417 ? . . . C(7) C(8) C(9) 120.7(5) ? . . . H(5) C(7) C(8) 120.3423 ? . . . C(7) C(8) H(6) 119.6629 ? . . . C(8) C(9) H(7) 119.8565 ? . . . H(6) C(8) C(9) 119.6629 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Sm(1) Sm(1) 3.884(1) ? . 4_555 Sm(1) Sm(1) 3.884(1) ? 4_554 . Sm(1) Sm(1) 13.3284(3) ? . 13_554 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC Lu-wt1349w.cif' #============================================================================== data_Lu-wt1349w _database_code_depnum_ccdc_archive 'CCDC 632149' # -Lu-cinnamate-hydrothermal #============================================================================== _audit_creation_date 2006-12-21 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Lu O6 ' _chemical_formula_moiety 'C27 H21 Lu O6 ' _chemical_formula_weight 616.43 _chemical_melting_point ? _chemical_absolute_configuration ad # 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.589(2) _cell_length_b 7.817(2) _cell_length_c 13.021(3) _cell_angle_alpha 90 _cell_angle_beta 94.354(3) _cell_angle_gamma 90 _cell_volume 1176.1(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7162 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604.00 _exptl_absorpt_coefficient_mu 4.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.558 _exptl_absorpt_correction_T_max 0.919 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ' Bruker SMART 1000 CCD' _diffrn_measurement_method '\w & \f scan' _diffrn_reflns_number 7162 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9771 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9771 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4011 _reflns_number_gt 3754 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0410 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3761 _refine_ls_number_parameters 330 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.05]' _refine_ls_shift/su_max 0.0120 _refine_diff_density_max 2.49 _refine_diff_density_min -1.91 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 14.0(28) _refine_ls_abs_structure_details 'Flack (1983). 1192 Friedel Pairs' _refine_ls_abs_structure_Flack -0.01(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Lu Lu -0.472 5.858 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Lu(1) Lu 0.46131(2) 0.5081(2) 0.52359(2) 0.02318(7) Uani 1.00 1 d . . . O(1) O 0.4058(5) 0.9396(9) 0.5826(5) 0.035(2) Uani 1.00 1 d . . . O(2) O 0.3269(5) 0.6781(9) 0.5816(5) 0.035(2) Uani 1.00 1 d . . . O(3) O 0.5421(5) 0.2349(8) 0.5859(4) 0.032(2) Uani 1.00 1 d . . . O(4) O 0.4176(6) 0.3704(9) 0.6743(5) 0.033(2) Uani 1.00 1 d . . . O(5) O 0.3325(6) 0.3702(9) 0.4234(5) 0.036(2) Uani 1.00 1 d . . . O(6) O 0.6023(6) 0.6189(9) 0.6278(5) 0.038(2) Uani 1.00 1 d . . . C(1) C 0.3208(8) 0.8409(13) 0.5883(6) 0.032(2) Uani 1.00 1 d . . . C(2) C 0.2080(12) 0.916(2) 0.6048(11) 0.032(3) Uani 1.00 1 d . . . C(3) C 0.1891(13) 1.084(2) 0.6074(11) 0.037(3) Uani 1.00 1 d . . . C(4) C 0.0816(8) 1.1729(13) 0.6199(7) 0.033(2) Uani 1.00 1 d . . . C(5) C -0.0251(8) 1.092(1) 0.6154(8) 0.041(3) Uani 1.00 1 d . . . C(6) C -0.1262(9) 1.181(2) 0.6302(8) 0.047(3) Uani 1.00 1 d . . . C(7) C -0.1193(10) 1.356(2) 0.6522(9) 0.053(3) Uani 1.00 1 d . . . C(8) C -0.0142(11) 1.436(2) 0.6558(10) 0.057(4) Uani 1.00 1 d . . . C(9) C 0.0842(10) 1.351(2) 0.6394(9) 0.048(3) Uani 1.00 1 d . . . C(10) C 0.4974(8) 0.2678(12) 0.6727(6) 0.029(2) Uani 1.00 1 d . . . C(11) C 0.5550(9) 0.1865(13) 0.7680(6) 0.036(2) Uani 1.00 1 d . . . C(12) C 0.5253(8) 0.2388(13) 0.8584(7) 0.035(2) Uani 1.00 1 d . . . C(13) C 0.5844(8) 0.1936(13) 0.9590(6) 0.033(2) Uani 1.00 1 d . . . C(14) C 0.6881(10) 0.104(2) 0.9696(8) 0.047(3) Uani 1.00 1 d . . . C(15) C 0.7410(10) 0.071(2) 1.0657(9) 0.054(3) Uani 1.00 1 d . . . C(16) C 0.6933(10) 0.125(2) 1.1533(8) 0.051(3) Uani 1.00 1 d . . . C(17) C 0.5911(11) 0.212(2) 1.1451(7) 0.056(4) Uani 1.00 1 d . . . C(18) C 0.5359(10) 0.248(2) 1.0487(7) 0.044(3) Uani 1.00 1 d . . . C(19) C 0.3341(7) 0.2464(12) 0.3595(6) 0.030(2) Uani 1.00 1 d . . . C(20) C 0.2538(8) 0.2590(13) 0.2651(7) 0.033(2) Uani 1.00 1 d . . . C(21) C 0.2635(8) 0.1572(13) 0.1847(7) 0.035(2) Uani 1.00 1 d . . . C(22) C 0.1890(9) 0.1630(13) 0.0859(7) 0.037(3) Uani 1.00 1 d . . . C(23) C 0.0847(9) 0.244(2) 0.0787(8) 0.045(3) Uani 1.00 1 d . . . C(24) C 0.0176(12) 0.246(2) -0.0163(10) 0.050(4) Uani 1.00 1 d . . . C(25) C 0.0584(11) 0.172(2) -0.1004(8) 0.058(4) Uani 1.00 1 d . . . C(26) C 0.1641(11) 0.091(2) -0.0944(8) 0.055(3) Uani 1.00 1 d . . . C(27) C 0.2290(10) 0.084(2) 0.0008(8) 0.048(3) Uani 1.00 1 d . . . H(1) H 0.1451 0.8415 0.6142 0.038 Uiso 1.00 1 c R . . H(2) H 0.2547 1.1548 0.6002 0.044 Uiso 1.00 1 c R . . H(3) H -0.0292 0.9726 0.6018 0.050 Uiso 1.00 1 c R . . H(4) H -0.1989 1.1246 0.6255 0.057 Uiso 1.00 1 c R . . H(5) H -0.1871 1.4184 0.6645 0.063 Uiso 1.00 1 c R . . H(6) H -0.0104 1.5550 0.6702 0.068 Uiso 1.00 1 c R . . H(7) H 0.1554 1.4117 0.6410 0.058 Uiso 1.00 1 c R . . H(8) H 0.6115 0.0994 0.7630 0.043 Uiso 1.00 1 c R . . H(9) H 0.4601 0.3122 0.8589 0.043 Uiso 1.00 1 c R . . H(10) H 0.7228 0.0654 0.9101 0.056 Uiso 1.00 1 c R . . H(11) H 0.8118 0.0093 1.0716 0.065 Uiso 1.00 1 c R . . H(12) H 0.7314 0.1031 1.2192 0.061 Uiso 1.00 1 c R . . H(13) H 0.5570 0.2474 1.2056 0.067 Uiso 1.00 1 c R . . H(14) H 0.4652 0.3100 1.0439 0.052 Uiso 1.00 1 c R . . H(15) H 0.1939 0.3423 0.2622 0.040 Uiso 1.00 1 c R . . H(16) H 0.3229 0.0733 0.1904 0.041 Uiso 1.00 1 c R . . H(17) H 0.0573 0.2989 0.1373 0.055 Uiso 1.00 1 c R . . H(18) H -0.0562 0.3000 -0.0214 0.060 Uiso 1.00 1 c R . . H(19) H 0.0132 0.1752 -0.1644 0.069 Uiso 1.00 1 c R . . H(20) H 0.1927 0.0402 -0.1538 0.066 Uiso 1.00 1 c R . . H(21) H 0.3009 0.0253 0.0067 0.057 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Lu(1) 0.0286(1) 0.0202(2) 0.01995(13) -0.0007(4) -0.00364(8) -0.0004(3) O(1) 0.032(3) 0.040(4) 0.033(3) -0.012(3) 0.005(3) -0.012(3) O(2) 0.035(3) 0.029(4) 0.041(4) 0.001(3) 0.003(3) 0.003(3) O(3) 0.047(4) 0.029(4) 0.018(3) 0.002(3) -0.002(2) -0.001(2) O(4) 0.045(4) 0.028(4) 0.026(3) 0.005(3) -0.003(3) 0.001(3) O(5) 0.041(4) 0.033(4) 0.033(3) -0.006(3) -0.009(3) -0.008(3) O(6) 0.044(4) 0.032(4) 0.035(3) -0.008(3) -0.017(3) 0.001(3) C(1) 0.037(5) 0.037(5) 0.021(4) 0.007(4) 0.001(3) 0.006(4) C(2) 0.025(6) 0.029(8) 0.041(7) -0.006(5) 0.002(4) -0.001(5) C(3) 0.029(6) 0.042(8) 0.039(7) -0.007(5) 0.001(5) -0.004(5) C(4) 0.034(5) 0.032(5) 0.033(4) 0.004(4) -0.002(4) -0.003(4) C(5) 0.041(5) 0.035(6) 0.046(6) 0.007(4) -0.004(4) -0.005(4) C(6) 0.038(5) 0.051(7) 0.051(6) 0.003(5) -0.005(4) -0.002(5) C(7) 0.044(6) 0.062(8) 0.050(6) 0.022(6) -0.005(5) -0.002(6) C(8) 0.071(8) 0.031(6) 0.069(8) 0.010(6) 0.005(6) -0.003(5) C(9) 0.045(6) 0.036(6) 0.062(7) 0.002(5) -0.000(5) -0.006(5) C(10) 0.040(5) 0.022(5) 0.023(4) -0.007(4) -0.006(3) -0.001(3) C(11) 0.054(6) 0.030(5) 0.023(4) 0.005(5) -0.005(4) 0.003(4) C(12) 0.041(5) 0.035(5) 0.029(4) 0.006(4) -0.004(4) 0.008(4) C(13) 0.041(5) 0.035(6) 0.023(4) 0.001(4) -0.001(3) 0.004(4) C(14) 0.064(7) 0.048(7) 0.029(5) 0.007(5) 0.002(5) -0.006(4) C(15) 0.052(6) 0.056(8) 0.052(6) 0.011(5) -0.010(5) 0.005(5) C(16) 0.057(7) 0.060(8) 0.035(5) 0.002(6) -0.010(5) 0.012(5) C(17) 0.075(8) 0.071(9) 0.022(4) -0.004(7) 0.005(5) -0.007(5) C(18) 0.053(6) 0.047(7) 0.031(5) 0.004(5) 0.002(4) 0.001(5) C(19) 0.027(4) 0.033(5) 0.028(4) -0.003(4) -0.012(3) 0.003(4) C(20) 0.032(4) 0.031(5) 0.032(4) 0.001(4) -0.017(3) -0.000(4) C(21) 0.034(5) 0.033(6) 0.035(5) 0.001(4) -0.010(4) 0.001(4) C(22) 0.043(5) 0.035(6) 0.030(5) -0.005(4) -0.011(4) -0.004(4) C(23) 0.047(6) 0.054(7) 0.034(5) 0.002(5) -0.008(4) -0.007(5) C(24) 0.047(8) 0.057(9) 0.043(9) 0.008(6) -0.018(6) -0.001(7) C(25) 0.069(8) 0.063(8) 0.036(5) -0.013(7) -0.027(5) 0.002(6) C(26) 0.068(7) 0.069(8) 0.027(5) -0.002(6) -0.008(5) -0.013(5) C(27) 0.052(6) 0.049(6) 0.042(6) 0.009(5) -0.006(5) -0.003(5) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Lu(1) O(1) 2.212(6) ? . 2_646 Lu(1) O(2) 2.223(7) ? . . Lu(1) O(3) 2.445(7) ? . . Lu(1) O(3) 2.273(6) ? . 2_656 Lu(1) O(4) 2.328(6) ? . . Lu(1) O(5) 2.190(6) ? . . Lu(1) O(6) 2.219(7) ? . . O(1) Lu(1) 2.212(6) ? . 2_656 O(1) C(1) 1.26(1) ? . . O(2) C(1) 1.28(1) ? . . O(3) Lu(1) 2.273(6) ? . 2_646 O(3) C(10) 1.30(1) ? . . O(4) C(10) 1.23(1) ? . . O(5) C(19) 1.28(1) ? . . O(6) C(19) 1.24(1) ? . 2_656 C(1) C(2) 1.46(2) ? . . C(2) C(3) 1.33(2) ? . . C(2) H(1) 0.9500 ? . . C(3) C(4) 1.45(2) ? . . C(3) H(2) 0.9500 ? . . C(4) C(5) 1.39(1) ? . . C(4) C(9) 1.42(2) ? . . C(5) C(6) 1.39(2) ? . . C(5) H(3) 0.9500 ? . . C(6) C(7) 1.39(2) ? . . C(6) H(4) 0.9500 ? . . C(7) C(8) 1.37(2) ? . . C(7) H(5) 0.9500 ? . . C(8) C(9) 1.35(2) ? . . C(8) H(6) 0.9500 ? . . C(9) H(7) 0.9500 ? . . C(10) C(11) 1.50(1) ? . . C(11) C(12) 1.32(1) ? . . C(11) H(8) 0.9500 ? . . C(12) C(13) 1.47(1) ? . . C(12) H(9) 0.9500 ? . . C(13) C(14) 1.39(2) ? . . C(13) C(18) 1.40(1) ? . . C(14) C(15) 1.38(1) ? . . C(14) H(10) 0.9500 ? . . C(15) C(16) 1.37(2) ? . . C(15) H(11) 0.9500 ? . . C(16) C(17) 1.36(2) ? . . C(16) H(12) 0.9500 ? . . C(17) C(18) 1.39(1) ? . . C(17) H(13) 0.9500 ? . . C(18) H(14) 0.9500 ? . . C(19) O(6) 1.24(1) ? . 2_646 C(19) C(20) 1.49(1) ? . . C(20) C(21) 1.33(1) ? . . C(20) H(15) 0.9500 ? . . C(21) C(22) 1.49(1) ? . . C(21) H(16) 0.9500 ? . . C(22) C(23) 1.36(1) ? . . C(22) C(27) 1.38(1) ? . . C(23) C(24) 1.41(2) ? . . C(23) H(17) 0.9500 ? . . C(24) C(25) 1.36(2) ? . . C(24) H(18) 0.9500 ? . . C(25) C(26) 1.38(2) ? . . C(25) H(19) 0.9500 ? . . C(26) C(27) 1.40(1) ? . . C(26) H(20) 0.9500 ? . . C(27) C(22) 1.38(1) ? . . C(27) C(26) 1.40(1) ? . . C(27) H(21) 0.9500 ? . . H(18) C(24) 0.9500 ? . . H(21) C(27) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Lu(1) O(1) 153.7(3) ? . . 2_646 O(3) Lu(1) O(1) 74.3(2) ? . . 2_646 O(3) Lu(1) O(1) 77.1(2) ? 2_656 . 2_646 O(4) Lu(1) O(1) 128.4(2) ? . . 2_646 O(5) Lu(1) O(1) 89.1(2) ? . . 2_646 O(6) Lu(1) O(1) 87.8(2) ? . . 2_646 Lu(1) O(1) C(1) 140.4(6) ? . 2_646 2_646 O(3) Lu(1) O(2) 132.1(2) ? . . . O(3) Lu(1) O(2) 76.6(2) ? 2_656 . . O(4) Lu(1) O(2) 77.7(2) ? . . . O(5) Lu(1) O(2) 91.9(2) ? . . . O(6) Lu(1) O(2) 93.5(2) ? . . . Lu(1) O(2) C(1) 131.5(6) ? . . . O(3) Lu(1) O(3) 151.3(2) ? 2_656 . . O(4) Lu(1) O(3) 54.5(2) ? . . . O(5) Lu(1) O(3) 89.7(2) ? . . . O(6) Lu(1) O(3) 83.8(2) ? . . . Lu(1) O(3) C(10) 87.0(5) ? . . . Lu(1) O(3) Lu(1) 119.0(2) ? . . 2_646 O(4) Lu(1) O(3) 153.5(2) ? . . 2_656 O(5) Lu(1) O(3) 91.8(2) ? . . 2_656 O(6) Lu(1) O(3) 93.2(2) ? . . 2_656 Lu(1) O(3) C(10) 135.1(6) ? . 2_656 2_656 Lu(1) O(3) Lu(1) 119.0(2) ? . 2_656 2_656 O(5) Lu(1) O(4) 95.3(2) ? . . . O(6) Lu(1) O(4) 82.1(2) ? . . . Lu(1) O(4) C(10) 94.3(5) ? . . . O(6) Lu(1) O(5) 173.4(3) ? . . . Lu(1) O(5) C(19) 135.9(6) ? . . . Lu(1) O(6) C(19) 142.7(6) ? . . 2_656 O(1) Lu(1) O(3) 74.3(2) ? . 2_656 2_656 C(1) O(1) Lu(1) 140.4(6) ? . . 2_656 O(1) Lu(1) O(3) 77.1(2) ? . 2_656 1_565 O(1) Lu(1) O(5) 89.1(2) ? . 2_656 2_656 O(1) Lu(1) O(6) 87.8(2) ? . 2_656 2_656 O(1) C(1) O(2) 124.0(8) ? . . . O(1) C(1) C(2) 118(1) ? . . . O(2) C(1) C(2) 117(1) ? . . . C(10) O(3) Lu(1) 135.1(6) ? . . 2_646 O(3) Lu(1) O(1) 77.1(2) ? . 2_646 1_545 O(3) Lu(1) O(2) 76.6(2) ? . 2_646 2_646 O(3) Lu(1) O(5) 91.8(2) ? . 2_646 2_646 O(3) Lu(1) O(6) 93.2(2) ? . 2_646 2_646 O(3) C(10) O(4) 119.6(7) ? . . . O(3) C(10) C(11) 116.8(8) ? . . . O(4) C(10) C(11) 123.3(8) ? . . . O(5) C(19) O(6) 124.0(8) ? . . 2_646 O(5) C(19) C(20) 116.7(8) ? . . . O(6) C(19) O(5) 124.0(8) ? . 2_656 2_656 O(6) C(19) C(20) 119.3(8) ? . 2_656 2_656 C(1) C(2) C(3) 123(1) ? . . . C(1) C(2) H(1) 118.2783 ? . . . H(1) C(2) C(3) 118.2783 ? . . . C(2) C(3) H(2) 115.8211 ? . . . C(2) C(3) C(4) 128(1) ? . . . H(2) C(3) C(4) 115.8214 ? . . . C(3) C(4) C(5) 123(1) ? . . . C(3) C(4) C(9) 119(1) ? . . . C(4) C(5) H(3) 119.2583 ? . . . C(9) C(4) C(5) 117.6(9) ? . . . C(4) C(5) C(6) 121(1) ? . . . C(4) C(9) H(7) 119.8896 ? . . . C(4) C(9) C(8) 120(1) ? . . . H(3) C(5) C(6) 119.2586 ? . . . C(5) C(6) C(7) 118(1) ? . . . C(5) C(6) H(4) 120.5153 ? . . . C(6) C(7) C(8) 119(1) ? . . . H(4) C(6) C(7) 120.5151 ? . . . C(6) C(7) H(5) 120.2454 ? . . . C(7) C(8) C(9) 122(1) ? . . . C(7) C(8) H(6) 118.9289 ? . . . H(5) C(7) C(8) 120.2452 ? . . . C(8) C(9) H(7) 119.8894 ? . . . H(6) C(8) C(9) 118.9291 ? . . . C(10) C(11) H(8) 120.7539 ? . . . C(10) C(11) C(12) 118.5(9) ? . . . H(8) C(11) C(12) 120.7539 ? . . . C(11) C(12) H(9) 117.0971 ? . . . C(11) C(12) C(13) 125.8(9) ? . . . H(9) C(12) C(13) 117.0969 ? . . . C(12) C(13) C(14) 123.3(8) ? . . . C(12) C(13) C(18) 118.7(9) ? . . . C(13) C(14) H(10) 119.7313 ? . . . C(18) C(13) C(14) 117.9(8) ? . . . C(13) C(14) C(15) 120(1) ? . . . C(13) C(18) H(14) 119.8757 ? . . . C(13) C(18) C(17) 120(1) ? . . . H(10) C(14) C(15) 119.7313 ? . . . C(14) C(15) C(16) 121(1) ? . . . C(14) C(15) H(11) 119.3974 ? . . . C(15) C(16) C(17) 119(1) ? . . . H(11) C(15) C(16) 119.3979 ? . . . C(15) C(16) H(12) 120.2883 ? . . . C(16) C(17) C(18) 120(1) ? . . . C(16) C(17) H(13) 119.6797 ? . . . H(12) C(16) C(17) 120.2889 ? . . . C(17) C(18) H(14) 119.8759 ? . . . H(13) C(17) C(18) 119.6794 ? . . . C(19) O(6) Lu(1) 142.7(6) ? . 2_646 2_646 C(20) C(19) O(6) 119.3(8) ? . . 2_646 C(19) C(20) H(15) 119.0763 ? . . . C(19) C(20) C(21) 121.8(9) ? . . . H(15) C(20) C(21) 119.0760 ? . . . C(20) C(21) H(16) 117.1474 ? . . . C(20) C(21) C(22) 125.7(9) ? . . . H(16) C(21) C(22) 117.1479 ? . . . C(21) C(22) C(23) 121.6(9) ? . . . C(21) C(22) C(27) 118.2(9) ? . . . C(22) C(23) H(17) 120.2237 ? . . . C(27) C(22) C(23) 120.2(9) ? . . . C(22) C(23) C(24) 119(1) ? . . . C(22) C(27) H(21) 119.8396 ? . . . C(22) C(27) C(26) 120(1) ? . . . H(17) C(23) C(24) 120.2233 ? . . . C(23) C(24) C(25) 119(1) ? . . . C(23) C(24) H(18) 120.0042 ? . . . C(24) C(25) C(26) 121(1) ? . . . H(18) C(24) C(25) 120.0036 ? . . . C(24) C(25) H(19) 119.4968 ? . . . C(25) C(26) C(27) 118(1) ? . . . C(25) C(26) H(20) 120.5687 ? . . . H(19) C(25) C(26) 119.4968 ? . . . C(26) C(27) H(21) 119.8390 ? . . . H(20) C(26) C(27) 120.5688 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Lu(1) Lu(1) 4.067(2) ? . 2_656 Lu(1) Lu(1) 4.067(2) ? 2_646 . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================