# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Kwang-hwa Lii' 'Yen-Shen Liu' 'Ming-Feng Tang' _publ_contact_author_name 'Kwang-hwa Lii' _publ_contact_author_email LIIKH@CC.NCU.EDU.TW _publ_section_title ; Rare earth metal squarates incorporating ethylene glycol ligand with a three-dimensional framework structure: RE(C4O4)1.5(C2H6O2) (RE = Y, La-Nd, Sm-Lu) ; # Attachment 'RESqEg.cif' # # Title: Rare Earth Metal Squarates Incorporating Ethylene Glycol Ligand with a Three-Dimensional Framework Structure: # RE(C4O4)1.5(C2H46O2) (RE = Y, La-Nd, Sm-Lu) # # By Yen-Shen Liu, Ming-Feng Tang, and Kwang-Hwa Lii # # E-mail: liikh@cc.ncu.edu.tw # # # Y(C4O4)1.5(C2H6O2) (compound 1) # data_YSqEg _database_code_depnum_ccdc_archive 'CCDC 737270' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Y(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 O8 Y' _chemical_formula_weight 319.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.7516(6) _cell_length_b 12.0784(6) _cell_length_c 12.5437(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.233(2) _cell_angle_gamma 90.00 _cell_volume 1906.94(16) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pillar-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 6.148 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4351 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8444 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.42 _reflns_number_total 1940 _reflns_number_gt 1796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+1.9955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1940 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.272594(13) 0.463317(14) 0.222601(13) 0.01075(8) Uani 1 1 d . . . O1 O 0.23931(11) 0.40979(11) 0.40082(11) 0.0174(3) Uani 1 1 d . . . O2 O 0.20947(12) 0.14669(11) 0.34553(11) 0.0185(3) Uani 1 1 d . . . O3 O 0.36985(12) 0.43259(14) 0.08765(12) 0.0245(3) Uani 1 1 d . . . O4 O 0.59919(12) 0.55187(12) 0.16064(11) 0.0202(3) Uani 1 1 d . . . O5 O 0.37832(12) 0.31529(12) 0.27680(13) 0.0261(4) Uani 1 1 d . . . O6 O 0.37474(13) 0.04994(12) 0.24246(14) 0.0255(4) Uani 1 1 d . . . O7 O 0.14945(14) 0.46597(13) 0.04880(14) 0.0243(4) Uani 1 1 d . . . O8 O 0.15826(14) 0.30837(14) 0.18966(14) 0.0315(4) Uani 1 1 d . . . C1 C 0.24549(15) 0.32168(15) 0.45426(15) 0.0139(4) Uani 1 1 d . . . C2 C 0.23252(15) 0.20306(15) 0.43025(15) 0.0138(4) Uani 1 1 d . . . C3 C 0.44155(16) 0.46981(15) 0.04048(17) 0.0160(4) Uani 1 1 d . . . C4 C 0.54463(16) 0.52235(15) 0.07267(16) 0.0151(4) Uani 1 1 d . . . C5 C 0.44407(15) 0.24488(15) 0.25817(16) 0.0147(4) Uani 1 1 d . . . C6 C 0.44342(15) 0.12448(15) 0.25060(16) 0.0139(4) Uani 1 1 d . . . C7 C 0.0859(2) 0.3692(2) 0.0174(2) 0.0340(6) Uani 1 1 d . . . C8 C 0.0598(2) 0.3194(2) 0.1180(2) 0.0332(6) Uani 1 1 d . . . H7A H 0.130(3) 0.312(3) -0.018(3) 0.068(11) Uiso 1 1 d . . . H7B H 0.018(2) 0.3899(19) -0.028(2) 0.028(6) Uiso 1 1 d . . . H8A H 0.025(2) 0.250(2) 0.103(2) 0.036(7) Uiso 1 1 d . . . H8B H 0.010(2) 0.374(2) 0.151(2) 0.044(8) Uiso 1 1 d . . . H7O H 0.162(2) 0.255(2) 0.218(2) 0.038(9) Uiso 1 1 d . . . H8O H 0.177(3) 0.482(3) 0.005(3) 0.034(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01155(11) 0.01029(11) 0.01035(12) 0.00111(6) 0.00159(7) 0.00150(6) O1 0.0275(8) 0.0111(6) 0.0141(7) 0.0027(5) 0.0045(6) 0.0013(6) O2 0.0293(8) 0.0135(6) 0.0115(7) -0.0025(5) -0.0001(6) -0.0015(6) O3 0.0233(8) 0.0310(8) 0.0217(8) -0.0001(7) 0.0116(6) -0.0022(7) O4 0.0227(8) 0.0221(7) 0.0135(7) -0.0042(6) -0.0041(6) 0.0048(6) O5 0.0266(8) 0.0197(7) 0.0348(9) 0.0076(7) 0.0134(7) 0.0126(7) O6 0.0224(8) 0.0217(8) 0.0342(9) -0.0059(7) 0.0101(7) -0.0112(6) O7 0.0257(9) 0.0302(9) 0.0166(8) 0.0049(7) 0.0020(7) -0.0063(7) O8 0.0405(10) 0.0176(8) 0.0298(9) 0.0106(7) -0.0143(8) -0.0107(7) C1 0.0163(9) 0.0135(9) 0.0122(9) -0.0010(7) 0.0029(7) 0.0009(7) C2 0.0172(9) 0.0123(9) 0.0124(9) -0.0007(7) 0.0035(7) 0.0001(7) C3 0.0166(10) 0.0179(10) 0.0140(10) 0.0006(7) 0.0042(8) 0.0047(8) C4 0.0161(10) 0.0155(9) 0.0137(10) 0.0019(7) 0.0022(8) 0.0041(7) C5 0.0160(10) 0.0129(9) 0.0151(9) 0.0030(7) 0.0024(7) 0.0025(8) C6 0.0153(10) 0.0142(9) 0.0123(9) 0.0001(7) 0.0025(7) -0.0023(8) C7 0.0374(14) 0.0357(13) 0.0246(13) 0.0022(11) -0.0084(11) -0.0098(11) C8 0.0322(13) 0.0275(12) 0.0354(14) 0.0055(11) -0.0081(11) -0.0127(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O6 2.2540(15) 4 ? Y1 O5 2.2765(14) . ? Y1 O4 2.2790(14) 2_655 ? Y1 O3 2.2836(15) . ? Y1 O8 2.3676(16) . ? Y1 O2 2.3981(13) 4 ? Y1 O1 2.4291(14) . ? Y1 O7 2.4741(16) . ? O1 C1 1.253(2) . ? O2 C2 1.257(2) . ? O2 Y1 2.3981(13) 4_545 ? O3 C3 1.250(3) . ? O4 C4 1.258(2) . ? O4 Y1 2.2790(14) 2_655 ? O5 C5 1.242(2) . ? O6 C6 1.249(2) . ? O6 Y1 2.2540(15) 4_545 ? O7 C7 1.441(3) . ? O7 H8O 0.72(3) . ? O8 C8 1.428(3) . ? O8 H7O 0.73(3) . ? C1 C2 1.462(3) 7_556 ? C1 C2 1.468(3) . ? C2 C1 1.462(3) 7_556 ? C3 C4 1.457(3) . ? C3 C4 1.461(3) 5_665 ? C4 C3 1.461(3) 5_665 ? C5 C6 1.457(3) . ? C5 C5 1.473(4) 2_655 ? C6 C6 1.445(4) 2_655 ? C7 C8 1.483(4) . ? C7 H7A 1.03(4) . ? C7 H7B 0.99(2) . ? C8 H8A 0.95(3) . ? C8 H8B 1.05(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Y1 O5 141.14(6) 4 . ? O6 Y1 O4 101.05(6) 4 2_655 ? O5 Y1 O4 81.22(6) . 2_655 ? O6 Y1 O3 142.03(6) 4 . ? O5 Y1 O3 74.20(6) . . ? O4 Y1 O3 97.68(6) 2_655 . ? O6 Y1 O8 83.78(6) 4 . ? O5 Y1 O8 75.52(6) . . ? O4 Y1 O8 147.28(5) 2_655 . ? O3 Y1 O8 97.74(6) . . ? O6 Y1 O2 76.75(5) 4 4 ? O5 Y1 O2 138.25(5) . 4 ? O4 Y1 O2 72.30(5) 2_655 4 ? O3 Y1 O2 77.98(5) . 4 ? O8 Y1 O2 139.39(5) . 4 ? O6 Y1 O1 70.76(5) 4 . ? O5 Y1 O1 72.46(5) . . ? O4 Y1 O1 75.33(5) 2_655 . ? O3 Y1 O1 146.60(5) . . ? O8 Y1 O1 75.91(5) . . ? O2 Y1 O1 127.92(5) 4 . ? O6 Y1 O7 74.59(6) 4 . ? O5 Y1 O7 122.35(6) . . ? O4 Y1 O7 148.07(5) 2_655 . ? O3 Y1 O7 72.08(6) . . ? O8 Y1 O7 64.56(6) . . ? O2 Y1 O7 75.96(5) 4 . ? O1 Y1 O7 129.38(6) . . ? C1 O1 Y1 135.47(13) . . ? C2 O2 Y1 141.17(12) . 4_545 ? C3 O3 Y1 144.89(14) . . ? C4 O4 Y1 132.02(13) . 2_655 ? C5 O5 Y1 150.06(14) . . ? C6 O6 Y1 156.10(14) . 4_545 ? C7 O7 Y1 118.69(13) . . ? C7 O7 H8O 109(3) . . ? Y1 O7 H8O 111(2) . . ? C8 O8 Y1 119.38(13) . . ? C8 O8 H7O 111(2) . . ? Y1 O8 H7O 128(2) . . ? O1 C1 C2 133.57(17) . 7_556 ? O1 C1 C2 136.35(18) . . ? C2 C1 C2 90.07(15) 7_556 . ? O2 C2 C1 135.16(18) . 7_556 ? O2 C2 C1 134.89(18) . . ? C1 C2 C1 89.93(15) 7_556 . ? O3 C3 C4 136.17(19) . . ? O3 C3 C4 134.01(19) . 5_665 ? C4 C3 C4 89.82(16) . 5_665 ? O4 C4 C3 135.6(2) . . ? O4 C4 C3 134.2(2) . 5_665 ? C3 C4 C3 90.18(16) . 5_665 ? O5 C5 C6 134.30(19) . . ? O5 C5 C5 136.37(12) . 2_655 ? C6 C5 C5 89.22(11) . 2_655 ? O6 C6 C6 133.42(12) . 2_655 ? O6 C6 C5 136.17(18) . . ? C6 C6 C5 90.31(11) 2_655 . ? O7 C7 C8 106.8(2) . . ? O7 C7 H7A 110(2) . . ? C8 C7 H7A 108.1(19) . . ? O7 C7 H7B 110.8(14) . . ? C8 C7 H7B 107.5(15) . . ? H7A C7 H7B 114(2) . . ? O8 C8 C7 106.2(2) . . ? O8 C8 H8A 111.8(16) . . ? C7 C8 H8A 110.5(17) . . ? O8 C8 H8B 110.0(15) . . ? C7 C8 H8B 108.0(16) . . ? H8A C8 H8B 110(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.406 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.070 #===End # # La(C4O4)1.5(C2H6O2) (compound 2) # data_LaSqEg _database_code_depnum_ccdc_archive 'CCDC 737271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety La(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 La O8' _chemical_formula_weight 369.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.1606(6) _cell_length_b 12.3974(6) _cell_length_c 12.8717(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.705(2) _cell_angle_gamma 90.00 _cell_volume 2075.92(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 4.145 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6031 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9964 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.37 _reflns_number_total 2586 _reflns_number_gt 2437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+2.7348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2586 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0164 _refine_ls_R_factor_gt 0.0150 _refine_ls_wR_factor_ref 0.0372 _refine_ls_wR_factor_gt 0.0367 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.275049(7) 0.464484(8) 0.223113(8) 0.01306(4) Uani 1 1 d . . . O1 O 0.23722(12) 0.40617(11) 0.40438(10) 0.0228(3) Uani 1 1 d . . . O2 O 0.20265(12) 0.15169(12) 0.34986(11) 0.0238(3) Uani 1 1 d . . . O3 O 0.37517(13) 0.42769(16) 0.08328(14) 0.0366(4) Uani 1 1 d . . . O4 O 0.59088(13) 0.55438(14) 0.15711(12) 0.0309(4) Uani 1 1 d . . . O5 O 0.38280(14) 0.31127(15) 0.27785(16) 0.0417(5) Uani 1 1 d . . . O6 O 0.37807(15) 0.05430(15) 0.24416(17) 0.0434(5) Uani 1 1 d . . . O7 O 0.14838(15) 0.46161(15) 0.04476(14) 0.0340(4) Uani 1 1 d . . . O8 O 0.15262(16) 0.30485(15) 0.18552(15) 0.0420(5) Uani 1 1 d . . . C1 C 0.24462(15) 0.32044(16) 0.45601(14) 0.0171(4) Uani 1 1 d . . . C2 C 0.22937(15) 0.20536(15) 0.43202(14) 0.0172(4) Uani 1 1 d . . . C3 C 0.44388(17) 0.46745(17) 0.03838(16) 0.0232(4) Uani 1 1 d . . . C4 C 0.54048(16) 0.52369(17) 0.07095(16) 0.0218(4) Uani 1 1 d . . . C5 C 0.44626(15) 0.24250(16) 0.25874(16) 0.0200(4) Uani 1 1 d . . . C6 C 0.44524(14) 0.12563(16) 0.25128(16) 0.0192(4) Uani 1 1 d . . . C7 C 0.0872(3) 0.3672(3) 0.0164(2) 0.0489(8) Uani 1 1 d . . . C8 C 0.0598(2) 0.3192(3) 0.1142(2) 0.0477(7) Uani 1 1 d . . . H7A H 0.131(3) 0.308(3) -0.018(3) 0.084(13) Uiso 1 1 d . . . H7B H 0.025(2) 0.385(3) -0.034(3) 0.055(9) Uiso 1 1 d . . . H8A H 0.025(3) 0.246(3) 0.097(3) 0.061(10) Uiso 1 1 d . . . H8B H 0.013(3) 0.382(3) 0.143(3) 0.066(11) Uiso 1 1 d . . . H7O H 0.173(3) 0.481(3) -0.004(3) 0.054(10) Uiso 1 1 d . . . H8O H 0.156(3) 0.254(3) 0.220(3) 0.066(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01510(6) 0.01201(6) 0.01240(6) 0.00236(4) 0.00315(4) 0.00283(4) O1 0.0412(8) 0.0127(7) 0.0157(6) 0.0027(5) 0.0082(6) 0.0023(6) O2 0.0408(8) 0.0162(7) 0.0133(6) -0.0043(5) 0.0009(6) -0.0019(6) O3 0.0355(9) 0.0441(10) 0.0356(9) 0.0002(8) 0.0231(7) -0.0028(8) O4 0.0356(9) 0.0360(9) 0.0183(7) -0.0050(7) -0.0052(6) 0.0103(7) O5 0.0431(10) 0.0296(9) 0.0571(11) 0.0153(8) 0.0232(9) 0.0240(8) O6 0.0375(10) 0.0339(10) 0.0643(13) -0.0119(9) 0.0258(9) -0.0217(8) O7 0.0375(9) 0.0428(11) 0.0205(8) 0.0086(7) 0.0002(7) -0.0085(7) O8 0.0572(12) 0.0245(9) 0.0382(10) 0.0141(8) -0.0126(9) -0.0151(8) C1 0.0240(9) 0.0150(9) 0.0132(8) -0.0009(7) 0.0064(7) 0.0001(7) C2 0.0258(9) 0.0129(9) 0.0133(8) -0.0008(7) 0.0043(7) -0.0005(7) C3 0.0236(10) 0.0305(12) 0.0169(9) 0.0018(8) 0.0070(8) 0.0080(8) C4 0.0226(10) 0.0278(11) 0.0153(9) 0.0008(8) 0.0034(7) 0.0091(8) C5 0.0209(9) 0.0170(10) 0.0224(10) 0.0052(8) 0.0048(7) 0.0051(7) C6 0.0182(9) 0.0187(10) 0.0220(9) 0.0000(8) 0.0075(7) -0.0025(7) C7 0.0570(18) 0.0497(18) 0.0334(14) 0.0020(13) -0.0146(13) -0.0139(14) C8 0.0475(16) 0.0404(16) 0.0495(16) 0.0088(13) -0.0112(13) -0.0201(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O6 2.3948(16) 4 ? La1 O5 2.4110(16) . ? La1 O3 2.4294(16) . ? La1 O4 2.4308(15) 2_655 ? La1 O2 2.5374(14) 4 ? La1 O8 2.5516(18) . ? La1 O1 2.5624(13) . ? La1 O7 2.6253(17) . ? O1 C1 1.249(2) . ? O2 C2 1.254(2) . ? O2 La1 2.5374(14) 4_545 ? O3 C3 1.246(3) . ? O4 C4 1.262(3) . ? O4 La1 2.4308(15) 2_655 ? O5 C5 1.244(2) . ? O6 C6 1.244(2) . ? O6 La1 2.3948(16) 4_545 ? O7 C7 1.436(3) . ? O8 C8 1.423(3) . ? C1 C2 1.465(2) 7_556 ? C1 C2 1.467(3) . ? C2 C1 1.465(2) 7_556 ? C3 C4 1.455(3) . ? C3 C4 1.457(3) 5_665 ? C4 C3 1.457(3) 5_665 ? C5 C6 1.452(3) . ? C5 C5 1.466(4) 2_655 ? C6 C6 1.447(4) 2_655 ? C7 C8 1.485(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 La1 O5 142.03(6) 4 . ? O6 La1 O3 141.52(7) 4 . ? O5 La1 O3 73.00(6) . . ? O6 La1 O4 102.98(7) 4 2_655 ? O5 La1 O4 80.65(7) . 2_655 ? O3 La1 O4 97.64(6) . 2_655 ? O6 La1 O2 77.72(6) 4 4 ? O5 La1 O2 137.13(6) . 4 ? O3 La1 O2 77.96(6) . 4 ? O4 La1 O2 72.66(5) 2_655 4 ? O6 La1 O8 82.53(7) 4 . ? O5 La1 O8 76.76(7) . . ? O3 La1 O8 96.41(7) . . ? O4 La1 O8 148.51(6) 2_655 . ? O2 La1 O8 138.10(5) 4 . ? O6 La1 O1 71.73(6) 4 . ? O5 La1 O1 72.44(5) . . ? O3 La1 O1 145.44(6) . . ? O4 La1 O1 76.95(5) 2_655 . ? O2 La1 O1 130.12(4) 4 . ? O8 La1 O1 75.51(5) . . ? O6 La1 O7 73.76(7) 4 . ? O5 La1 O7 120.82(7) . . ? O3 La1 O7 72.14(6) . . ? O4 La1 O7 149.85(5) 2_655 . ? O2 La1 O7 77.43(5) 4 . ? O8 La1 O7 61.61(6) . . ? O1 La1 O7 127.39(5) . . ? C1 O1 La1 135.57(12) . . ? C2 O2 La1 139.84(13) . 4_545 ? C3 O3 La1 141.48(16) . . ? C4 O4 La1 130.83(14) . 2_655 ? C5 O5 La1 149.89(15) . . ? C6 O6 La1 157.69(16) . 4_545 ? C7 O7 La1 119.38(15) . . ? C8 O8 La1 118.75(16) . . ? O1 C1 C2 134.16(18) . 7_556 ? O1 C1 C2 135.90(18) . . ? C2 C1 C2 89.94(15) 7_556 . ? O2 C2 C1 135.04(18) . 7_556 ? O2 C2 C1 134.87(18) . . ? C1 C2 C1 90.06(15) 7_556 . ? O3 C3 C4 136.0(2) . . ? O3 C3 C4 134.1(2) . 5_665 ? C4 C3 C4 89.83(17) . 5_665 ? O4 C4 C3 135.9(2) . . ? O4 C4 C3 133.9(2) . 5_665 ? C3 C4 C3 90.17(17) . 5_665 ? O5 C5 C6 134.22(19) . . ? O5 C5 C5 136.29(13) . 2_655 ? C6 C5 C5 89.39(10) . 2_655 ? O6 C6 C6 134.24(13) . 2_655 ? O6 C6 C5 135.52(19) . . ? C6 C6 C5 90.13(11) 2_655 . ? O7 C7 C8 108.1(2) . . ? O8 C8 C7 107.6(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.661 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.088 #===End # # Ce(C4O4)1.5(C2H6O2) (compound 3) # data_CeSqEg _database_code_depnum_ccdc_archive 'CCDC 737272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Ce(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Ce O8' _chemical_formula_weight 370.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.0958(5) _cell_length_b 12.3373(5) _cell_length_c 12.8153(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.876(2) _cell_angle_gamma 90.00 _cell_volume 2045.73(14) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 4.480 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6520 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9822 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.38 _reflns_number_total 2534 _reflns_number_gt 2377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+2.2711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2534 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0386 _refine_ls_wR_factor_gt 0.0378 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.274692(7) 0.463838(8) 0.222944(7) 0.01253(4) Uani 1 1 d . . . O1 O 0.23711(11) 0.40712(12) 0.40403(11) 0.0216(3) Uani 1 1 d . . . O2 O 0.20373(12) 0.15087(12) 0.34915(11) 0.0232(3) Uani 1 1 d . . . O3 O 0.37508(12) 0.42798(15) 0.08497(13) 0.0321(4) Uani 1 1 d . . . O4 O 0.59296(12) 0.55445(14) 0.15706(12) 0.0268(3) Uani 1 1 d . . . O5 O 0.38231(13) 0.31173(14) 0.27857(15) 0.0363(4) Uani 1 1 d . . . O6 O 0.37769(13) 0.05317(14) 0.24424(16) 0.0365(4) Uani 1 1 d . . . O7 O 0.14843(14) 0.46224(14) 0.04490(14) 0.0312(4) Uani 1 1 d . . . O8 O 0.15391(16) 0.30502(16) 0.18561(15) 0.0406(5) Uani 1 1 d . . . C1 C 0.24447(14) 0.32047(16) 0.45577(14) 0.0167(4) Uani 1 1 d . . . C2 C 0.22982(14) 0.20513(16) 0.43165(15) 0.0167(4) Uani 1 1 d . . . C3 C 0.44389(16) 0.46792(17) 0.03911(17) 0.0208(4) Uani 1 1 d . . . C4 C 0.54169(16) 0.52372(17) 0.07111(16) 0.0198(4) Uani 1 1 d . . . C5 C 0.44589(14) 0.24255(16) 0.25890(16) 0.0180(4) Uani 1 1 d . . . C6 C 0.44484(13) 0.12546(16) 0.25123(15) 0.0175(4) Uani 1 1 d . . . C7 C 0.0872(2) 0.3673(3) 0.0164(2) 0.0446(7) Uani 1 1 d . . . C8 C 0.0600(2) 0.3190(3) 0.1145(2) 0.0433(7) Uani 1 1 d . . . H7A H 0.130(3) 0.310(3) -0.019(3) 0.078(12) Uiso 1 1 d . . . H7B H 0.022(2) 0.386(3) -0.031(3) 0.053(9) Uiso 1 1 d . . . H8A H 0.024(2) 0.248(3) 0.100(3) 0.057(9) Uiso 1 1 d . . . H8B H 0.013(3) 0.379(3) 0.146(3) 0.063(10) Uiso 1 1 d . . . H7O H 0.178(3) 0.481(3) -0.006(3) 0.062(11) Uiso 1 1 d . . . H8O H 0.157(3) 0.252(3) 0.215(3) 0.064(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01349(6) 0.01230(7) 0.01204(6) 0.00194(3) 0.00276(4) 0.00268(3) O1 0.0365(8) 0.0137(7) 0.0157(7) 0.0024(5) 0.0073(6) 0.0027(6) O2 0.0378(8) 0.0163(7) 0.0145(7) -0.0045(5) 0.0005(6) -0.0029(6) O3 0.0315(8) 0.0382(10) 0.0309(9) 0.0002(7) 0.0182(7) -0.0036(7) O4 0.0292(8) 0.0328(9) 0.0159(7) -0.0038(6) -0.0043(6) 0.0069(6) O5 0.0353(9) 0.0267(9) 0.0508(11) 0.0117(8) 0.0188(8) 0.0193(7) O6 0.0301(8) 0.0293(9) 0.0539(12) -0.0087(8) 0.0189(8) -0.0179(7) O7 0.0342(9) 0.0402(11) 0.0183(8) 0.0066(7) 0.0007(7) -0.0075(7) O8 0.0534(11) 0.0253(10) 0.0362(10) 0.0135(8) -0.0146(8) -0.0143(8) C1 0.0215(8) 0.0157(9) 0.0134(8) -0.0009(7) 0.0040(7) -0.0001(7) C2 0.0223(9) 0.0152(9) 0.0128(9) -0.0003(7) 0.0033(7) 0.0000(7) C3 0.0212(9) 0.0262(12) 0.0162(10) 0.0016(7) 0.0069(8) 0.0054(7) C4 0.0198(9) 0.0243(11) 0.0155(9) 0.0009(8) 0.0027(7) 0.0073(7) C5 0.0172(9) 0.0165(10) 0.0206(9) 0.0057(7) 0.0036(7) 0.0048(7) C6 0.0159(9) 0.0183(10) 0.0190(9) 0.0013(7) 0.0052(7) -0.0022(7) C7 0.0507(16) 0.0464(18) 0.0314(14) 0.0008(12) -0.0109(12) -0.0117(13) C8 0.0429(14) 0.0361(16) 0.0461(16) 0.0072(12) -0.0086(12) -0.0188(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O6 2.3733(15) 4 ? Ce1 O5 2.3887(16) . ? Ce1 O3 2.4017(15) . ? Ce1 O4 2.4075(15) 2_655 ? Ce1 O8 2.5172(18) . ? Ce1 O2 2.5176(15) 4 ? Ce1 O1 2.5436(13) . ? Ce1 O7 2.6031(17) . ? O1 C1 1.254(2) . ? O2 C2 1.254(2) . ? O2 Ce1 2.5176(14) 4_545 ? O3 C3 1.250(3) . ? O4 C4 1.257(3) . ? O4 Ce1 2.4075(15) 2_655 ? O5 C5 1.245(2) . ? O6 C6 1.246(2) . ? O6 Ce1 2.3733(15) 4_545 ? O7 C7 1.434(3) . ? O7 H7O 0.84(4) . ? O8 C8 1.424(3) . ? O8 H8O 0.75(4) . ? C1 C2 1.462(3) . ? C1 C2 1.465(3) 7_556 ? C2 C1 1.465(3) 7_556 ? C3 C4 1.456(3) . ? C3 C4 1.457(3) 5_665 ? C4 C3 1.457(3) 5_665 ? C5 C6 1.448(3) . ? C5 C5 1.470(4) 2_655 ? C6 C6 1.450(3) 2_655 ? C7 C8 1.484(4) . ? C7 H7A 1.05(4) . ? C7 H7B 1.00(3) . ? C8 H8A 0.99(3) . ? C8 H8B 1.07(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ce1 O5 141.76(6) 4 . ? O6 Ce1 O3 141.88(6) 4 . ? O5 Ce1 O3 73.15(6) . . ? O6 Ce1 O4 102.32(6) 4 2_655 ? O5 Ce1 O4 80.83(6) . 2_655 ? O3 Ce1 O4 97.69(6) . 2_655 ? O6 Ce1 O8 82.78(7) 4 . ? O5 Ce1 O8 76.69(7) . . ? O3 Ce1 O8 96.66(7) . . ? O4 Ce1 O8 148.45(6) 2_655 . ? O6 Ce1 O2 77.55(5) 4 4 ? O5 Ce1 O2 137.31(5) . 4 ? O3 Ce1 O2 78.08(6) . 4 ? O4 Ce1 O2 72.44(5) 2_655 4 ? O8 Ce1 O2 138.29(5) . 4 ? O6 Ce1 O1 71.32(6) 4 . ? O5 Ce1 O1 72.54(5) . . ? O3 Ce1 O1 145.69(6) . . ? O4 Ce1 O1 76.50(5) 2_655 . ? O8 Ce1 O1 75.81(6) . . ? O2 Ce1 O1 129.45(5) 4 . ? O6 Ce1 O7 73.80(7) 4 . ? O5 Ce1 O7 121.42(6) . . ? O3 Ce1 O7 72.49(6) . . ? O4 Ce1 O7 149.40(5) 2_655 . ? O8 Ce1 O7 62.09(6) . . ? O2 Ce1 O7 77.14(5) 4 . ? O1 Ce1 O7 127.70(5) . . ? C1 O1 Ce1 135.00(12) . . ? C2 O2 Ce1 140.14(13) . 4_545 ? C3 O3 Ce1 142.13(15) . . ? C4 O4 Ce1 130.87(14) . 2_655 ? C5 O5 Ce1 149.36(15) . . ? C6 O6 Ce1 157.38(15) . 4_545 ? C7 O7 Ce1 118.96(15) . . ? C7 O7 H7O 109(3) . . ? Ce1 O7 H7O 112(3) . . ? C8 O8 Ce1 118.84(16) . . ? C8 O8 H8O 114(3) . . ? Ce1 O8 H8O 127(3) . . ? O1 C1 C2 136.13(18) . . ? O1 C1 C2 133.79(18) . 7_556 ? C2 C1 C2 90.06(15) . 7_556 ? O2 C2 C1 135.05(18) . . ? O2 C2 C1 134.99(19) . 7_556 ? C1 C2 C1 89.94(15) . 7_556 ? O3 C3 C4 136.1(2) . . ? O3 C3 C4 133.9(2) . 5_665 ? C4 C3 C4 89.98(17) . 5_665 ? O4 C4 C3 135.8(2) . . ? O4 C4 C3 134.1(2) . 5_665 ? C3 C4 C3 90.02(17) . 5_665 ? O5 C5 C6 134.27(18) . . ? O5 C5 C5 136.25(13) . 2_655 ? C6 C5 C5 89.36(10) . 2_655 ? O6 C6 C5 135.91(18) . . ? O6 C6 C6 133.87(12) . 2_655 ? C5 C6 C6 90.14(10) . 2_655 ? O7 C7 C8 108.0(2) . . ? O7 C7 H7A 110(2) . . ? C8 C7 H7A 108(2) . . ? O7 C7 H7B 111.0(18) . . ? C8 C7 H7B 108.2(18) . . ? H7A C7 H7B 111(3) . . ? O8 C8 C7 107.1(2) . . ? O8 C8 H8A 110.3(19) . . ? C7 C8 H8A 111.6(19) . . ? O8 C8 H8B 109.2(18) . . ? C7 C8 H8B 105.4(18) . . ? H8A C8 H8B 113(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.613 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.104 #===End # # Pr(C4O4)1.5(C2H6O2) (compound 4) # data_PrSqEg _database_code_depnum_ccdc_archive 'CCDC 737273' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Pr(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 O8 Pr' _chemical_formula_weight 371.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.0212(7) _cell_length_b 12.2987(7) _cell_length_c 12.7671(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.839(2) _cell_angle_gamma 90.00 _cell_volume 2020.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle-like _exptl_crystal_colour olive _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 4.853 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6057 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9905 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.43 _reflns_number_total 2517 _reflns_number_gt 2431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+2.7786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2517 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0417 _refine_ls_wR_factor_gt 0.0413 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.274400(8) 0.463672(8) 0.222702(8) 0.01138(5) Uani 1 1 d . . . O1 O 0.23759(13) 0.40734(11) 0.40330(11) 0.0204(3) Uani 1 1 d . . . O2 O 0.20444(13) 0.15030(12) 0.34874(11) 0.0212(3) Uani 1 1 d . . . O3 O 0.37447(14) 0.42804(15) 0.08509(14) 0.0299(4) Uani 1 1 d . . . O4 O 0.59358(14) 0.55409(14) 0.15756(13) 0.0251(3) Uani 1 1 d . . . O5 O 0.38186(14) 0.31218(14) 0.27870(16) 0.0337(4) Uani 1 1 d . . . O6 O 0.37713(15) 0.05286(14) 0.24392(17) 0.0339(4) Uani 1 1 d . . . O7 O 0.14859(16) 0.46295(14) 0.04554(15) 0.0290(4) Uani 1 1 d . . . O8 O 0.15452(18) 0.30500(15) 0.18591(16) 0.0392(5) Uani 1 1 d . . . C1 C 0.24467(16) 0.32069(15) 0.45543(15) 0.0151(4) Uani 1 1 d . . . C2 C 0.23030(16) 0.20473(15) 0.43146(15) 0.0155(4) Uani 1 1 d . . . C3 C 0.44342(18) 0.46783(16) 0.03921(18) 0.0192(4) Uani 1 1 d . . . C4 C 0.54201(17) 0.52362(17) 0.07139(17) 0.0186(4) Uani 1 1 d . . . C5 C 0.44582(15) 0.24315(16) 0.25901(16) 0.0171(4) Uani 1 1 d . . . C6 C 0.44496(15) 0.12501(15) 0.25091(16) 0.0160(4) Uani 1 1 d . . . C7 C 0.0875(3) 0.3676(3) 0.0161(2) 0.0411(7) Uani 1 1 d . . . C8 C 0.0601(2) 0.3190(2) 0.1146(2) 0.0413(7) Uani 1 1 d . . . H7A H 0.128(3) 0.309(4) -0.016(3) 0.071(12) Uiso 1 1 d . . . H7B H 0.021(3) 0.387(3) -0.033(3) 0.061(11) Uiso 1 1 d . . . H8A H 0.023(3) 0.247(3) 0.099(3) 0.056(10) Uiso 1 1 d . . . H8B H 0.008(3) 0.377(3) 0.147(3) 0.057(11) Uiso 1 1 d . . . H7O H 0.171(3) 0.481(3) 0.000(3) 0.053(12) Uiso 1 1 d . . . H8O H 0.166(3) 0.252(4) 0.209(4) 0.077(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01317(7) 0.01070(7) 0.01060(7) 0.00181(3) 0.00282(4) 0.00261(3) O1 0.0358(9) 0.0123(6) 0.0141(7) 0.0023(5) 0.0063(6) 0.0022(6) O2 0.0358(9) 0.0143(6) 0.0125(7) -0.0034(5) 0.0002(6) -0.0015(6) O3 0.0290(9) 0.0372(9) 0.0278(9) 0.0003(7) 0.0182(7) -0.0041(7) O4 0.0278(9) 0.0300(8) 0.0152(8) -0.0040(6) -0.0045(6) 0.0068(7) O5 0.0336(10) 0.0242(8) 0.0473(11) 0.0114(8) 0.0188(8) 0.0182(7) O6 0.0285(10) 0.0286(8) 0.0483(12) -0.0079(8) 0.0175(9) -0.0171(7) O7 0.0331(10) 0.0363(10) 0.0167(8) 0.0067(6) 0.0007(7) -0.0078(7) O8 0.0527(13) 0.0224(9) 0.0357(10) 0.0133(8) -0.0146(9) -0.0141(8) C1 0.0215(10) 0.0128(8) 0.0113(8) -0.0005(7) 0.0040(7) -0.0004(7) C2 0.0225(10) 0.0126(8) 0.0118(9) -0.0004(7) 0.0034(7) -0.0003(7) C3 0.0195(10) 0.0235(10) 0.0154(10) 0.0014(7) 0.0055(8) 0.0051(7) C4 0.0196(10) 0.0223(9) 0.0137(9) 0.0013(7) 0.0021(8) 0.0062(8) C5 0.0182(10) 0.0147(9) 0.0189(9) 0.0035(7) 0.0045(8) 0.0046(7) C6 0.0163(10) 0.0152(9) 0.0173(9) 0.0008(7) 0.0048(7) -0.0023(7) C7 0.0477(17) 0.0423(15) 0.0282(14) 0.0017(11) -0.0107(12) -0.0096(13) C8 0.0431(16) 0.0337(14) 0.0426(16) 0.0087(12) -0.0075(12) -0.0167(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O6 2.3530(16) 4 ? Pr1 O5 2.3734(16) . ? Pr1 O3 2.3834(16) . ? Pr1 O4 2.3918(16) 2_655 ? Pr1 O8 2.4980(19) . ? Pr1 O2 2.5006(14) 4 ? Pr1 O1 2.5230(14) . ? Pr1 O7 2.5809(19) . ? O1 C1 1.252(2) . ? O2 C2 1.252(2) . ? O2 Pr1 2.5007(14) 4_545 ? O3 C3 1.245(3) . ? O4 C4 1.255(3) . ? O4 Pr1 2.3918(16) 2_655 ? O5 C5 1.242(2) . ? O6 C6 1.245(2) . ? O6 Pr1 2.3530(16) 4_545 ? O7 C7 1.434(3) . ? O7 H7O 0.73(4) . ? O8 C8 1.423(3) . ? O8 H8O 0.73(4) . ? C1 C2 1.465(3) . ? C1 C2 1.465(3) 7_556 ? C2 C1 1.465(3) 7_556 ? C3 C4 1.457(3) 5_665 ? C3 C4 1.458(3) . ? C4 C3 1.457(3) 5_665 ? C5 C6 1.457(3) . ? C5 C5 1.464(4) 2_655 ? C6 C6 1.437(4) 2_655 ? C7 C8 1.485(4) . ? C7 H7A 1.02(4) . ? C7 H7B 1.01(4) . ? C8 H8A 1.02(4) . ? C8 H8B 1.11(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Pr1 O5 141.57(6) 4 . ? O6 Pr1 O3 141.99(7) 4 . ? O5 Pr1 O3 73.38(6) . . ? O6 Pr1 O4 102.00(7) 4 2_655 ? O5 Pr1 O4 80.79(7) . 2_655 ? O3 Pr1 O4 97.81(6) . 2_655 ? O6 Pr1 O8 83.17(7) 4 . ? O5 Pr1 O8 76.46(7) . . ? O3 Pr1 O8 96.57(7) . . ? O4 Pr1 O8 148.25(6) 2_655 . ? O6 Pr1 O2 77.33(6) 4 4 ? O5 Pr1 O2 137.52(6) . 4 ? O3 Pr1 O2 78.26(6) . 4 ? O4 Pr1 O2 72.41(5) 2_655 4 ? O8 Pr1 O2 138.51(6) . 4 ? O6 Pr1 O1 71.35(6) 4 . ? O5 Pr1 O1 72.25(5) . . ? O3 Pr1 O1 145.62(6) . . ? O4 Pr1 O1 76.25(5) 2_655 . ? O8 Pr1 O1 75.90(6) . . ? O2 Pr1 O1 129.23(5) 4 . ? O6 Pr1 O7 73.94(7) 4 . ? O5 Pr1 O7 121.79(7) . . ? O3 Pr1 O7 72.46(7) . . ? O4 Pr1 O7 149.18(5) 2_655 . ? O8 Pr1 O7 62.51(6) . . ? O2 Pr1 O7 76.95(5) 4 . ? O1 Pr1 O7 128.01(6) . . ? C1 O1 Pr1 135.28(12) . . ? C2 O2 Pr1 140.18(13) . 4_545 ? C3 O3 Pr1 142.18(16) . . ? C4 O4 Pr1 131.05(14) . 2_655 ? C5 O5 Pr1 149.14(16) . . ? C6 O6 Pr1 157.57(16) . 4_545 ? C7 O7 Pr1 118.97(15) . . ? C7 O7 H7O 108(3) . . ? Pr1 O7 H7O 115(4) . . ? C8 O8 Pr1 118.63(15) . . ? C8 O8 H8O 118(4) . . ? Pr1 O8 H8O 123(4) . . ? O1 C1 C2 136.14(18) . . ? O1 C1 C2 133.85(18) . 7_556 ? C2 C1 C2 90.00(15) . 7_556 ? O2 C2 C1 134.92(18) . . ? O2 C2 C1 135.06(18) . 7_556 ? C1 C2 C1 90.00(15) . 7_556 ? O3 C3 C4 134.0(2) . 5_665 ? O3 C3 C4 136.0(2) . . ? C4 C3 C4 89.95(18) 5_665 . ? O4 C4 C3 134.1(2) . 5_665 ? O4 C4 C3 135.8(2) . . ? C3 C4 C3 90.05(18) 5_665 . ? O5 C5 C6 134.3(2) . . ? O5 C5 C5 136.41(13) . 2_655 ? C6 C5 C5 89.19(11) . 2_655 ? O6 C6 C6 134.18(13) . 2_655 ? O6 C6 C5 135.5(2) . . ? C6 C6 C5 90.25(11) 2_655 . ? O7 C7 C8 107.6(2) . . ? O7 C7 H7A 113(2) . . ? C8 C7 H7A 105(2) . . ? O7 C7 H7B 111(2) . . ? C8 C7 H7B 109(2) . . ? H7A C7 H7B 112(3) . . ? O8 C8 C7 107.1(2) . . ? O8 C8 H8A 111(2) . . ? C7 C8 H8A 111(2) . . ? O8 C8 H8B 110.7(19) . . ? C7 C8 H8B 107.3(19) . . ? H8A C8 H8B 110(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.519 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.149 #===End # # Nd(C4O4)1.5(C2H6O2) (compound 5) # data_NdSqEg _database_code_depnum_ccdc_archive 'CCDC 737274' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Nd(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Nd O8' _chemical_formula_weight 374.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.9884(5) _cell_length_b 12.2543(5) _cell_length_c 12.7418(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.987(2) _cell_angle_gamma 90.00 _cell_volume 2003.14(14) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour light-purple _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 5.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6532 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14270 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.38 _reflns_number_total 2496 _reflns_number_gt 2302 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+1.4565P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2496 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0156 _refine_ls_wR_factor_ref 0.0387 _refine_ls_wR_factor_gt 0.0378 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.274408(7) 0.463436(8) 0.222617(7) 0.01042(5) Uani 1 1 d . . . O1 O 0.23816(12) 0.40797(12) 0.40302(11) 0.0180(3) Uani 1 1 d . . . O2 O 0.20512(12) 0.14949(12) 0.34812(11) 0.0197(3) Uani 1 1 d . . . O3 O 0.37391(13) 0.42837(15) 0.08542(13) 0.0269(4) Uani 1 1 d . . . O4 O 0.59427(13) 0.55397(13) 0.15825(12) 0.0221(3) Uani 1 1 d . . . O5 O 0.38133(13) 0.31240(14) 0.27872(14) 0.0306(4) Uani 1 1 d . . . O6 O 0.37672(14) 0.05214(14) 0.24365(15) 0.0307(4) Uani 1 1 d . . . O7 O 0.14920(15) 0.46316(14) 0.04585(14) 0.0261(4) Uani 1 1 d . . . O8 O 0.15546(17) 0.30537(17) 0.18615(16) 0.0358(5) Uani 1 1 d . . . C1 C 0.24501(15) 0.32086(17) 0.45508(15) 0.0137(4) Uani 1 1 d . . . C2 C 0.23061(16) 0.20456(17) 0.43132(15) 0.0144(4) Uani 1 1 d . . . C3 C 0.44321(17) 0.46812(17) 0.03945(17) 0.0170(4) Uani 1 1 d . . . C4 C 0.54234(17) 0.52353(17) 0.07147(16) 0.0157(4) Uani 1 1 d . . . C5 C 0.44569(15) 0.24317(17) 0.25886(16) 0.0153(4) Uani 1 1 d . . . C6 C 0.44438(15) 0.12480(17) 0.25086(15) 0.0144(4) Uani 1 1 d . . . C7 C 0.0873(2) 0.3683(3) 0.0163(2) 0.0370(6) Uani 1 1 d . . . C8 C 0.0600(2) 0.3195(3) 0.1152(2) 0.0362(6) Uani 1 1 d . . . H7A H 0.129(3) 0.313(3) -0.014(3) 0.067(11) Uiso 1 1 d . . . H7B H 0.023(2) 0.387(2) -0.033(3) 0.050(9) Uiso 1 1 d . . . H8A H 0.021(2) 0.248(3) 0.101(2) 0.049(9) Uiso 1 1 d . . . H8B H 0.010(2) 0.372(3) 0.151(2) 0.051(9) Uiso 1 1 d . . . H7O H 0.175(3) 0.482(3) 0.004(3) 0.044(10) Uiso 1 1 d . . . H8O H 0.160(3) 0.255(3) 0.213(3) 0.057(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01150(7) 0.00990(7) 0.01012(6) 0.00149(4) 0.00250(4) 0.00213(4) O1 0.0299(8) 0.0112(8) 0.0135(7) 0.0018(6) 0.0059(6) 0.0020(6) O2 0.0331(8) 0.0133(8) 0.0116(7) -0.0035(6) 0.0003(6) -0.0009(6) O3 0.0259(9) 0.0326(10) 0.0259(8) 0.0003(7) 0.0156(7) -0.0030(8) O4 0.0241(9) 0.0255(9) 0.0144(7) -0.0038(6) -0.0039(6) 0.0049(7) O5 0.0294(9) 0.0229(9) 0.0429(10) 0.0096(8) 0.0157(8) 0.0161(7) O6 0.0254(9) 0.0255(10) 0.0446(11) -0.0066(8) 0.0158(8) -0.0147(7) O7 0.0287(9) 0.0317(11) 0.0175(8) 0.0057(7) 0.0021(7) -0.0072(7) O8 0.0468(12) 0.0211(10) 0.0331(10) 0.0126(9) -0.0140(8) -0.0128(9) C1 0.0171(9) 0.0132(10) 0.0111(8) -0.0009(8) 0.0035(7) 0.0004(8) C2 0.0197(10) 0.0122(10) 0.0117(9) -0.0014(7) 0.0032(8) -0.0005(8) C3 0.0171(10) 0.0216(12) 0.0133(9) 0.0014(8) 0.0056(8) 0.0063(8) C4 0.0170(10) 0.0174(11) 0.0127(9) 0.0007(8) 0.0020(8) 0.0051(8) C5 0.0149(10) 0.0147(10) 0.0162(9) 0.0040(8) 0.0024(7) 0.0046(8) C6 0.0138(10) 0.0155(11) 0.0147(9) 0.0003(8) 0.0044(7) -0.0023(8) C7 0.0425(16) 0.0376(17) 0.0262(13) 0.0005(12) -0.0089(12) -0.0105(13) C8 0.0330(15) 0.0315(16) 0.0396(15) 0.0082(12) -0.0082(12) -0.0130(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O6 2.3416(15) 4 ? Nd1 O5 2.3569(16) . ? Nd1 O3 2.3700(14) . ? Nd1 O4 2.3739(16) 2_655 ? Nd1 O8 2.4760(19) . ? Nd1 O2 2.4811(15) 4 ? Nd1 O1 2.5111(13) . ? Nd1 O7 2.5639(18) . ? O1 C1 1.253(2) . ? O2 C2 1.257(2) . ? O2 Nd1 2.4812(15) 4_545 ? O3 C3 1.247(2) . ? O4 C4 1.258(3) . ? O4 Nd1 2.3739(16) 2_655 ? O5 C5 1.244(2) . ? O6 C6 1.244(2) . ? O6 Nd1 2.3416(15) 4_545 ? O7 C7 1.430(3) . ? O7 H7O 0.72(3) . ? O8 C8 1.426(3) . ? O8 H8O 0.70(4) . ? C1 C2 1.463(3) . ? C1 C2 1.466(3) 7_556 ? C2 C1 1.466(3) 7_556 ? C3 C4 1.457(3) . ? C3 C4 1.458(3) 5_665 ? C4 C3 1.458(3) 5_665 ? C5 C6 1.454(3) . ? C5 C5 1.463(4) 2_655 ? C6 C6 1.448(4) 2_655 ? C7 C8 1.486(4) . ? C7 H7A 0.99(4) . ? C7 H7B 0.99(3) . ? C8 H8A 1.01(3) . ? C8 H8B 1.06(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Nd1 O5 141.26(6) 4 . ? O6 Nd1 O3 142.09(6) 4 . ? O5 Nd1 O3 73.62(6) . . ? O6 Nd1 O4 101.82(6) 4 2_655 ? O5 Nd1 O4 80.94(6) . 2_655 ? O3 Nd1 O4 97.83(6) . 2_655 ? O6 Nd1 O8 83.18(7) 4 . ? O5 Nd1 O8 76.31(7) . . ? O3 Nd1 O8 96.65(7) . . ? O4 Nd1 O8 148.27(6) 2_655 . ? O6 Nd1 O2 77.33(5) 4 4 ? O5 Nd1 O2 137.75(6) . 4 ? O3 Nd1 O2 78.28(6) . 4 ? O4 Nd1 O2 72.29(5) 2_655 4 ? O8 Nd1 O2 138.58(6) . 4 ? O6 Nd1 O1 71.05(6) 4 . ? O5 Nd1 O1 72.28(5) . . ? O3 Nd1 O1 145.89(6) . . ? O4 Nd1 O1 76.11(5) 2_655 . ? O8 Nd1 O1 76.07(6) . . ? O2 Nd1 O1 128.85(5) 4 . ? O6 Nd1 O7 74.16(6) 4 . ? O5 Nd1 O7 121.89(6) . . ? O3 Nd1 O7 72.30(6) . . ? O4 Nd1 O7 148.89(5) 2_655 . ? O8 Nd1 O7 62.78(6) . . ? O2 Nd1 O7 76.78(5) 4 . ? O1 Nd1 O7 128.31(5) . . ? C1 O1 Nd1 135.03(12) . . ? C2 O2 Nd1 140.43(14) . 4_545 ? C3 O3 Nd1 142.41(15) . . ? C4 O4 Nd1 131.01(14) . 2_655 ? C5 O5 Nd1 148.91(15) . . ? C6 O6 Nd1 157.11(14) . 4_545 ? C7 O7 Nd1 119.07(15) . . ? C7 O7 H7O 112(3) . . ? Nd1 O7 H7O 110(3) . . ? C8 O8 Nd1 118.59(16) . . ? C8 O8 H8O 115(3) . . ? Nd1 O8 H8O 126(3) . . ? O1 C1 C2 136.42(18) . . ? O1 C1 C2 133.67(18) . 7_556 ? C2 C1 C2 89.89(16) . 7_556 ? O2 C2 C1 134.91(19) . . ? O2 C2 C1 134.96(19) . 7_556 ? C1 C2 C1 90.11(16) . 7_556 ? O3 C3 C4 136.2(2) . . ? O3 C3 C4 134.0(2) . 5_665 ? C4 C3 C4 89.82(17) . 5_665 ? O4 C4 C3 135.51(19) . . ? O4 C4 C3 134.3(2) . 5_665 ? C3 C4 C3 90.18(17) . 5_665 ? O5 C5 C6 133.91(19) . . ? O5 C5 C5 136.54(13) . 2_655 ? C6 C5 C5 89.44(10) . 2_655 ? O6 C6 C6 133.91(12) . 2_655 ? O6 C6 C5 136.01(19) . . ? C6 C6 C5 90.02(11) 2_655 . ? O7 C7 C8 107.6(2) . . ? O7 C7 H7A 110(2) . . ? C8 C7 H7A 106(2) . . ? O7 C7 H7B 111.1(18) . . ? C8 C7 H7B 110.0(18) . . ? H7A C7 H7B 112(3) . . ? O8 C8 C7 106.7(2) . . ? O8 C8 H8A 111.4(17) . . ? C7 C8 H8A 112.1(18) . . ? O8 C8 H8B 109.2(17) . . ? C7 C8 H8B 111.0(17) . . ? H8A C8 H8B 106(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.488 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.119 #===End # # Sm(C4O4)1.5(C2H6O2) (compound 6) # data_SmSqEg _database_code_depnum_ccdc_archive 'CCDC 737275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Sm(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 O8 Sm' _chemical_formula_weight 380.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.9151(8) _cell_length_b 12.2146(7) _cell_length_c 12.6924(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.976(3) _cell_angle_gamma 90.00 _cell_volume 1977.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 5.969 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5749 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9514 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.43 _reflns_number_total 2479 _reflns_number_gt 2303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+2.0955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00193(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2479 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0182 _refine_ls_R_factor_gt 0.0163 _refine_ls_wR_factor_ref 0.0384 _refine_ls_wR_factor_gt 0.0377 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.273835(8) 0.463386(9) 0.222590(7) 0.01056(5) Uani 1 1 d . . . O1 O 0.23833(14) 0.40850(13) 0.40231(12) 0.0180(4) Uani 1 1 d . . . O2 O 0.20655(14) 0.14868(13) 0.34756(12) 0.0199(4) Uani 1 1 d . . . O3 O 0.37277(15) 0.42946(17) 0.08598(14) 0.0268(4) Uani 1 1 d . . . O4 O 0.59561(15) 0.55350(15) 0.15903(13) 0.0220(4) Uani 1 1 d . . . O5 O 0.38044(15) 0.31347(16) 0.27828(15) 0.0283(4) Uani 1 1 d . . . O6 O 0.37623(16) 0.05149(15) 0.24330(16) 0.0291(4) Uani 1 1 d . . . O7 O 0.14923(17) 0.46427(15) 0.04652(15) 0.0257(4) Uani 1 1 d . . . O8 O 0.15625(19) 0.30627(18) 0.18750(17) 0.0352(5) Uani 1 1 d . . . C1 C 0.24496(18) 0.32112(18) 0.45466(16) 0.0138(4) Uani 1 1 d . . . C2 C 0.23085(18) 0.20407(18) 0.43088(16) 0.0142(4) Uani 1 1 d . . . C3 C 0.4427(2) 0.46862(19) 0.03962(18) 0.0165(5) Uani 1 1 d . . . C4 C 0.54265(19) 0.52322(19) 0.07208(17) 0.0160(5) Uani 1 1 d . . . C5 C 0.44493(18) 0.24402(19) 0.25881(17) 0.0154(4) Uani 1 1 d . . . C6 C 0.44404(18) 0.12451(18) 0.25087(16) 0.0136(4) Uani 1 1 d . . . C7 C 0.0868(3) 0.3684(3) 0.0168(2) 0.0365(7) Uani 1 1 d . . . C8 C 0.0606(3) 0.3194(3) 0.1158(2) 0.0367(7) Uani 1 1 d . . . H7A H 0.134(3) 0.317(4) -0.016(3) 0.073(13) Uiso 1 1 d . . . H7B H 0.020(3) 0.389(3) -0.027(3) 0.040(9) Uiso 1 1 d . . . H8A H 0.022(2) 0.249(3) 0.100(3) 0.038(9) Uiso 1 1 d . . . H8B H 0.015(3) 0.377(3) 0.148(3) 0.058(11) Uiso 1 1 d . . . H7O H 0.181(3) 0.484(3) 0.002(3) 0.049(12) Uiso 1 1 d . . . H8O H 0.163(3) 0.260(3) 0.216(3) 0.037(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01134(8) 0.01000(7) 0.01051(7) 0.00137(3) 0.00224(4) 0.00204(4) O1 0.0301(10) 0.0108(8) 0.0140(7) 0.0023(6) 0.0062(6) 0.0022(7) O2 0.0315(10) 0.0141(8) 0.0130(7) -0.0036(6) 0.0003(6) -0.0019(7) O3 0.0252(11) 0.0336(10) 0.0250(9) 0.0002(8) 0.0151(7) -0.0043(9) O4 0.0239(10) 0.0251(9) 0.0147(8) -0.0025(6) -0.0037(6) 0.0051(8) O5 0.0264(10) 0.0213(10) 0.0403(10) 0.0086(8) 0.0148(8) 0.0137(8) O6 0.0257(11) 0.0237(10) 0.0409(11) -0.0077(8) 0.0146(8) -0.0140(8) O7 0.0271(11) 0.0332(11) 0.0165(9) 0.0058(7) 0.0025(7) -0.0080(8) O8 0.0455(14) 0.0209(11) 0.0326(10) 0.0124(9) -0.0140(9) -0.0126(10) C1 0.0163(12) 0.0144(11) 0.0114(9) -0.0011(8) 0.0041(8) 0.0000(9) C2 0.0165(12) 0.0133(11) 0.0132(9) 0.0006(8) 0.0030(8) 0.0006(9) C3 0.0168(13) 0.0196(12) 0.0140(10) 0.0008(8) 0.0052(8) 0.0044(10) C4 0.0161(12) 0.0187(12) 0.0132(10) 0.0020(8) 0.0026(8) 0.0055(9) C5 0.0152(12) 0.0149(11) 0.0164(10) 0.0035(8) 0.0036(8) 0.0035(9) C6 0.0133(11) 0.0131(11) 0.0151(10) 0.0010(8) 0.0041(8) -0.0022(9) C7 0.0386(19) 0.0399(18) 0.0266(14) 0.0022(12) -0.0085(12) -0.0100(15) C8 0.0346(18) 0.0306(16) 0.0405(16) 0.0075(13) -0.0076(13) -0.0136(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O6 2.3159(19) 4 ? Sm1 O5 2.3334(18) . ? Sm1 O3 2.3457(17) . ? Sm1 O4 2.3498(17) 2_655 ? Sm1 O8 2.445(2) . ? Sm1 O2 2.4596(16) 4 ? Sm1 O1 2.4879(15) . ? Sm1 O7 2.5420(18) . ? O1 C1 1.253(3) . ? O2 C2 1.253(3) . ? O2 Sm1 2.4596(16) 4_545 ? O3 C3 1.248(3) . ? O4 C4 1.260(3) . ? O4 Sm1 2.3498(16) 2_655 ? O5 C5 1.241(3) . ? O6 C6 1.243(3) . ? O6 Sm1 2.3159(19) 4_545 ? O7 C7 1.438(3) . ? O7 H7O 0.79(4) . ? O8 C8 1.424(3) . ? O8 H8O 0.67(4) . ? C1 C2 1.467(3) . ? C1 C2 1.470(3) 7_556 ? C2 C1 1.470(3) 7_556 ? C3 C4 1.454(3) . ? C3 C4 1.463(3) 5_665 ? C4 C3 1.463(3) 5_665 ? C5 C6 1.463(3) . ? C5 C5 1.474(5) 2_655 ? C6 C6 1.449(5) 2_655 ? C7 C8 1.479(4) . ? C7 H7A 1.01(4) . ? C7 H7B 0.99(3) . ? C8 H8A 1.00(3) . ? C8 H8B 1.04(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Sm1 O5 141.21(7) 4 . ? O6 Sm1 O3 142.05(7) 4 . ? O5 Sm1 O3 73.83(7) . . ? O6 Sm1 O4 101.58(7) 4 2_655 ? O5 Sm1 O4 80.98(7) . 2_655 ? O3 Sm1 O4 97.82(7) . 2_655 ? O6 Sm1 O8 83.38(8) 4 . ? O5 Sm1 O8 76.09(8) . . ? O3 Sm1 O8 96.96(8) . . ? O4 Sm1 O8 147.95(6) 2_655 . ? O6 Sm1 O2 77.09(6) 4 4 ? O5 Sm1 O2 137.95(6) . 4 ? O3 Sm1 O2 78.24(6) . 4 ? O4 Sm1 O2 72.32(5) 2_655 4 ? O8 Sm1 O2 138.81(6) . 4 ? O6 Sm1 O1 71.00(6) 4 . ? O5 Sm1 O1 72.25(6) . . ? O3 Sm1 O1 146.07(6) . . ? O4 Sm1 O1 75.91(6) 2_655 . ? O8 Sm1 O1 75.96(6) . . ? O2 Sm1 O1 128.61(5) 4 . ? O6 Sm1 O7 74.27(7) 4 . ? O5 Sm1 O7 122.16(7) . . ? O3 Sm1 O7 72.18(7) . . ? O4 Sm1 O7 148.52(6) 2_655 . ? O8 Sm1 O7 63.46(6) . . ? O2 Sm1 O7 76.39(6) 4 . ? O1 Sm1 O7 128.70(6) . . ? C1 O1 Sm1 135.12(14) . . ? C2 O2 Sm1 140.87(15) . 4_545 ? C3 O3 Sm1 143.02(17) . . ? C4 O4 Sm1 131.30(15) . 2_655 ? C5 O5 Sm1 149.22(16) . . ? C6 O6 Sm1 156.77(17) . 4_545 ? C7 O7 Sm1 118.64(15) . . ? C7 O7 H7O 114(3) . . ? Sm1 O7 H7O 107(3) . . ? C8 O8 Sm1 118.70(17) . . ? C8 O8 H8O 118(3) . . ? Sm1 O8 H8O 123(3) . . ? O1 C1 C2 136.48(19) . . ? O1 C1 C2 133.5(2) . 7_556 ? C2 C1 C2 89.99(17) . 7_556 ? O2 C2 C1 135.0(2) . . ? O2 C2 C1 135.0(2) . 7_556 ? C1 C2 C1 90.01(17) . 7_556 ? O3 C3 C4 135.9(2) . . ? O3 C3 C4 134.1(2) . 5_665 ? C4 C3 C4 90.00(19) . 5_665 ? O4 C4 C3 136.0(2) . . ? O4 C4 C3 134.0(2) . 5_665 ? C3 C4 C3 90.00(19) . 5_665 ? O5 C5 C6 134.2(2) . . ? O5 C5 C5 136.39(15) . 2_655 ? C6 C5 C5 89.25(13) . 2_655 ? O6 C6 C6 133.73(14) . 2_655 ? O6 C6 C5 136.0(2) . . ? C6 C6 C5 90.22(13) 2_655 . ? O7 C7 C8 107.5(2) . . ? O7 C7 H7A 106(2) . . ? C8 C7 H7A 109(2) . . ? O7 C7 H7B 110.6(19) . . ? C8 C7 H7B 106.7(19) . . ? H7A C7 H7B 117(3) . . ? O8 C8 C7 107.3(3) . . ? O8 C8 H8A 112.7(18) . . ? C7 C8 H8A 110.3(19) . . ? O8 C8 H8B 108(2) . . ? C7 C8 H8B 106(2) . . ? H8A C8 H8B 112(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.582 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.122 #===End # # Eu(C4O4)1.5(C2H6O2) (compound 7) # data_EuSqEg _database_code_depnum_ccdc_archive 'CCDC 737276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Eu(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Eu O8' _chemical_formula_weight 382.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.8772(5) _cell_length_b 12.1834(5) _cell_length_c 12.6535(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.039(2) _cell_angle_gamma 90.00 _cell_volume 1960.53(14) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 6.429 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5938 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19071 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2444 _reflns_number_gt 2177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2444 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.273634(10) 0.463323(11) 0.222524(11) 0.00977(6) Uani 1 1 d . . . O1 O 0.23862(17) 0.40886(17) 0.40215(16) 0.0165(4) Uani 1 1 d . . . O2 O 0.20675(17) 0.14824(17) 0.34714(16) 0.0177(5) Uani 1 1 d . . . O3 O 0.37233(18) 0.4296(2) 0.08689(19) 0.0248(5) Uani 1 1 d . . . O4 O 0.59634(19) 0.55344(19) 0.15930(18) 0.0205(5) Uani 1 1 d . . . O5 O 0.37980(18) 0.3140(2) 0.2779(2) 0.0279(6) Uani 1 1 d . . . O6 O 0.3756(2) 0.05118(19) 0.2431(2) 0.0276(6) Uani 1 1 d . . . O7 O 0.1492(2) 0.46465(19) 0.0471(2) 0.0250(6) Uani 1 1 d . . . O8 O 0.1567(2) 0.3065(2) 0.1878(2) 0.0335(7) Uani 1 1 d . . . C1 C 0.2453(2) 0.3211(2) 0.4546(2) 0.0127(6) Uani 1 1 d . . . C2 C 0.2316(2) 0.2041(2) 0.4310(2) 0.0133(6) Uani 1 1 d . . . C3 C 0.4430(3) 0.4689(2) 0.0397(3) 0.0164(7) Uani 1 1 d . . . C4 C 0.5435(2) 0.5227(2) 0.0719(3) 0.0157(6) Uani 1 1 d . . . C5 C 0.4446(2) 0.2438(2) 0.2587(2) 0.0135(6) Uani 1 1 d . . . C6 C 0.4440(2) 0.1246(2) 0.2509(2) 0.0133(6) Uani 1 1 d . . . C7 C 0.0871(3) 0.3690(3) 0.0170(3) 0.0352(9) Uani 1 1 d . . . C8 C 0.0603(3) 0.3194(4) 0.1161(3) 0.0333(9) Uani 1 1 d . . . H7A H 0.136(5) 0.312(5) -0.013(5) 0.092(19) Uiso 1 1 d . . . H7B H 0.017(3) 0.389(3) -0.034(3) 0.036(11) Uiso 1 1 d . . . H8A H 0.024(3) 0.252(3) 0.103(3) 0.028(10) Uiso 1 1 d . . . H8B H 0.013(3) 0.375(3) 0.145(3) 0.035(11) Uiso 1 1 d . . . H7O H 0.181(4) 0.479(4) 0.002(4) 0.042(14) Uiso 1 1 d . . . H8O H 0.164(4) 0.248(4) 0.219(4) 0.066(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01094(9) 0.00916(10) 0.00941(9) 0.00131(5) 0.00222(6) 0.00191(5) O1 0.0280(12) 0.0096(11) 0.0125(10) 0.0016(8) 0.0053(9) 0.0026(9) O2 0.0295(12) 0.0124(11) 0.0107(10) -0.0035(8) 0.0016(9) -0.0023(9) O3 0.0229(12) 0.0298(13) 0.0255(13) 0.0012(11) 0.0154(11) -0.0039(10) O4 0.0228(12) 0.0238(13) 0.0128(11) -0.0035(9) -0.0038(9) 0.0047(9) O5 0.0267(13) 0.0210(13) 0.0394(15) 0.0076(11) 0.0158(12) 0.0147(10) O6 0.0233(13) 0.0236(13) 0.0389(16) -0.0078(11) 0.0143(12) -0.0125(10) O7 0.0285(14) 0.0292(15) 0.0167(13) 0.0056(10) 0.0016(11) -0.0065(10) O8 0.0419(15) 0.0213(14) 0.0309(15) 0.0127(12) -0.0146(12) -0.0140(12) C1 0.0136(13) 0.0139(15) 0.0114(14) -0.0002(12) 0.0045(11) 0.0003(11) C2 0.0162(14) 0.0123(15) 0.0117(14) -0.0003(11) 0.0031(12) 0.0009(11) C3 0.0176(15) 0.0195(17) 0.0125(15) 0.0015(11) 0.0038(13) 0.0037(12) C4 0.0163(15) 0.0167(16) 0.0144(15) 0.0003(12) 0.0034(13) 0.0053(12) C5 0.0152(14) 0.0131(15) 0.0129(15) 0.0035(11) 0.0042(12) 0.0030(12) C6 0.0143(14) 0.0137(15) 0.0119(14) 0.0004(11) 0.0022(11) -0.0023(11) C7 0.042(2) 0.037(2) 0.0221(19) 0.0017(17) -0.0090(17) -0.0117(19) C8 0.031(2) 0.027(2) 0.036(2) 0.0080(17) -0.0096(17) -0.0142(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6 2.300(2) 4 ? Eu1 O5 2.317(2) . ? Eu1 O3 2.327(2) . ? Eu1 O4 2.336(2) 2_655 ? Eu1 O8 2.430(3) . ? Eu1 O2 2.447(2) 4 ? Eu1 O1 2.476(2) . ? Eu1 O7 2.526(3) . ? O1 C1 1.254(3) . ? O2 C2 1.259(3) . ? O2 Eu1 2.447(2) 4_545 ? O3 C3 1.259(4) . ? O4 C4 1.261(4) . ? O4 Eu1 2.336(2) 2_655 ? O5 C5 1.245(3) . ? O6 C6 1.249(3) . ? O6 Eu1 2.300(2) 4_545 ? O7 C7 1.430(4) . ? O7 H7O 0.77(5) . ? O8 C8 1.426(4) . ? O8 H8O 0.81(5) . ? C1 C2 1.461(4) . ? C1 C2 1.464(4) 7_556 ? C2 C1 1.464(4) 7_556 ? C3 C4 1.451(5) . ? C3 C4 1.452(4) 5_665 ? C4 C3 1.452(4) 5_665 ? C5 C6 1.456(4) . ? C5 C5 1.476(5) 2_655 ? C6 C6 1.445(5) 2_655 ? C7 C8 1.481(5) . ? C7 H7A 1.05(6) . ? C7 H7B 1.05(4) . ? C8 H8A 0.95(4) . ? C8 H8B 1.02(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Eu1 O5 141.16(8) 4 . ? O6 Eu1 O3 142.28(9) 4 . ? O5 Eu1 O3 73.73(9) . . ? O6 Eu1 O4 101.32(9) 4 2_655 ? O5 Eu1 O4 81.14(9) . 2_655 ? O3 Eu1 O4 97.78(9) . 2_655 ? O6 Eu1 O8 83.56(10) 4 . ? O5 Eu1 O8 75.91(10) . . ? O3 Eu1 O8 97.04(9) . . ? O4 Eu1 O8 147.86(8) 2_655 . ? O6 Eu1 O2 77.08(8) 4 4 ? O5 Eu1 O2 137.95(8) . 4 ? O3 Eu1 O2 78.31(8) . 4 ? O4 Eu1 O2 72.16(7) 2_655 4 ? O8 Eu1 O2 139.04(8) . 4 ? O6 Eu1 O1 70.91(8) 4 . ? O5 Eu1 O1 72.29(7) . . ? O3 Eu1 O1 146.00(8) . . ? O4 Eu1 O1 75.76(7) 2_655 . ? O8 Eu1 O1 76.01(8) . . ? O2 Eu1 O1 128.42(7) 4 . ? O6 Eu1 O7 74.33(10) 4 . ? O5 Eu1 O7 122.25(9) . . ? O3 Eu1 O7 72.39(9) . . ? O4 Eu1 O7 148.38(8) 2_655 . ? O8 Eu1 O7 63.67(8) . . ? O2 Eu1 O7 76.38(7) 4 . ? O1 Eu1 O7 128.80(8) . . ? C1 O1 Eu1 134.96(18) . . ? C2 O2 Eu1 140.8(2) . 4_545 ? C3 O3 Eu1 143.4(2) . . ? C4 O4 Eu1 131.0(2) . 2_655 ? C5 O5 Eu1 149.5(2) . . ? C6 O6 Eu1 156.7(2) . 4_545 ? C7 O7 Eu1 118.6(2) . . ? C7 O7 H7O 109(4) . . ? Eu1 O7 H7O 108(4) . . ? C8 O8 Eu1 118.7(2) . . ? C8 O8 H8O 115(4) . . ? Eu1 O8 H8O 126(4) . . ? O1 C1 C2 136.7(3) . . ? O1 C1 C2 133.5(3) . 7_556 ? C2 C1 C2 89.8(2) . 7_556 ? O2 C2 C1 134.9(3) . . ? O2 C2 C1 134.9(3) . 7_556 ? C1 C2 C1 90.2(2) . 7_556 ? O3 C3 C4 135.9(3) . . ? O3 C3 C4 133.9(3) . 5_665 ? C4 C3 C4 90.2(3) . 5_665 ? O4 C4 C3 135.6(3) . . ? O4 C4 C3 134.5(3) . 5_665 ? C3 C4 C3 89.8(3) . 5_665 ? O5 C5 C6 134.5(3) . . ? O5 C5 C5 136.21(18) . 2_655 ? C6 C5 C5 89.15(15) . 2_655 ? O6 C6 C6 133.76(18) . 2_655 ? O6 C6 C5 135.8(3) . . ? C6 C6 C5 90.36(16) 2_655 . ? O7 C7 C8 107.6(3) . . ? O7 C7 H7A 107(3) . . ? C8 C7 H7A 106(3) . . ? O7 C7 H7B 111(2) . . ? C8 C7 H7B 109(2) . . ? H7A C7 H7B 116(4) . . ? O8 C8 C7 106.7(3) . . ? O8 C8 H8A 112(2) . . ? C7 C8 H8A 112(2) . . ? O8 C8 H8B 110(2) . . ? C7 C8 H8B 105(2) . . ? H8A C8 H8B 110(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.691 _refine_diff_density_min -1.832 _refine_diff_density_rms 0.200 #===End # # Gd(C4O4)1.5(C2H6O2) (compound 8) # data_GdSqEg _database_code_depnum_ccdc_archive 'CCDC 737277' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Gd(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Gd O8' _chemical_formula_weight 387.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.8545(6) _cell_length_b 12.1603(6) _cell_length_c 12.6281(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.143(3) _cell_angle_gamma 90.00 _cell_volume 1948.88(16) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pillar-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 6.837 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6793 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14517 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2437 _reflns_number_gt 1980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+1.6918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00044(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2437 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.273488(14) 0.463300(15) 0.222484(14) 0.01095(7) Uani 1 1 d . . . O1 O 0.2389(2) 0.4088(2) 0.4016(2) 0.0174(6) Uani 1 1 d . . . O2 O 0.2073(2) 0.1476(2) 0.3463(2) 0.0190(6) Uani 1 1 d . . . O3 O 0.3716(2) 0.4306(2) 0.0865(2) 0.0264(7) Uani 1 1 d . . . O4 O 0.5969(2) 0.5527(2) 0.1594(2) 0.0205(6) Uani 1 1 d . . . O5 O 0.3797(2) 0.3137(2) 0.2776(2) 0.0275(7) Uani 1 1 d . . . O6 O 0.3755(2) 0.0505(2) 0.2427(2) 0.0277(7) Uani 1 1 d . . . O7 O 0.1496(2) 0.4648(3) 0.0476(2) 0.0263(7) Uani 1 1 d . . . O8 O 0.1575(3) 0.3068(3) 0.1876(3) 0.0346(9) Uani 1 1 d . . . C1 C 0.2456(3) 0.3211(3) 0.4546(3) 0.0142(8) Uani 1 1 d . . . C2 C 0.2320(3) 0.2035(3) 0.4310(3) 0.0132(8) Uani 1 1 d . . . C3 C 0.4423(3) 0.4693(3) 0.0400(3) 0.0164(8) Uani 1 1 d . . . C4 C 0.5435(3) 0.5224(3) 0.0723(3) 0.0158(8) Uani 1 1 d . . . C5 C 0.4445(3) 0.2439(3) 0.2582(3) 0.0147(8) Uani 1 1 d . . . C6 C 0.4436(3) 0.1244(3) 0.2509(3) 0.0135(8) Uani 1 1 d . . . C7 C 0.0866(4) 0.3697(5) 0.0163(4) 0.0359(12) Uani 1 1 d . . . C8 C 0.0598(4) 0.3190(5) 0.1161(4) 0.0358(12) Uani 1 1 d . . . H7A H 0.134(4) 0.304(4) -0.012(4) 0.057(17) Uiso 1 1 d . . . H7B H 0.018(4) 0.392(4) -0.029(4) 0.044(15) Uiso 1 1 d . . . H8A H 0.014(5) 0.376(5) 0.148(5) 0.09(2) Uiso 1 1 d . . . H8B H 0.022(4) 0.244(4) 0.102(4) 0.038(14) Uiso 1 1 d . . . H7O H 0.177(4) 0.484(4) -0.001(4) 0.029(14) Uiso 1 1 d . . . H8O H 0.160(4) 0.259(4) 0.216(4) 0.026(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01185(10) 0.01091(10) 0.01040(10) 0.00132(8) 0.00274(7) 0.00189(8) O1 0.0279(15) 0.0126(14) 0.0126(14) 0.0042(12) 0.0054(12) 0.0022(12) O2 0.0302(16) 0.0128(14) 0.0133(15) 0.0001(12) 0.0010(12) -0.0008(12) O3 0.0271(16) 0.0322(18) 0.0240(17) -0.0012(14) 0.0169(14) -0.0055(14) O4 0.0195(15) 0.0260(17) 0.0141(15) 0.0001(13) -0.0029(12) 0.0059(13) O5 0.0263(16) 0.0191(16) 0.040(2) 0.0079(15) 0.0149(15) 0.0106(13) O6 0.0231(16) 0.0275(18) 0.0351(18) -0.0053(15) 0.0128(14) -0.0102(14) O7 0.0295(17) 0.0311(19) 0.0182(17) 0.0041(15) 0.0035(14) -0.0068(15) O8 0.046(2) 0.0180(19) 0.034(2) 0.0144(17) -0.0105(17) -0.0123(16) C1 0.0135(19) 0.016(2) 0.014(2) 0.0013(17) 0.0025(16) -0.0002(16) C2 0.0129(18) 0.015(2) 0.0109(19) -0.0008(16) 0.0000(15) -0.0011(15) C3 0.0154(19) 0.020(2) 0.015(2) -0.0015(17) 0.0054(16) 0.0034(17) C4 0.0156(19) 0.020(2) 0.0110(19) -0.0004(17) -0.0013(16) 0.0072(16) C5 0.017(2) 0.0115(19) 0.015(2) 0.0032(16) 0.0027(17) 0.0030(16) C6 0.0145(19) 0.016(2) 0.0107(19) 0.0011(16) 0.0038(15) -0.0028(16) C7 0.038(3) 0.042(3) 0.023(3) 0.000(2) -0.010(2) -0.008(3) C8 0.031(3) 0.032(3) 0.040(3) 0.005(3) -0.007(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O6 2.291(3) 4 ? Gd1 O5 2.314(3) . ? Gd1 O3 2.321(3) . ? Gd1 O4 2.322(3) 2_655 ? Gd1 O8 2.414(3) . ? Gd1 O2 2.430(3) 4 ? Gd1 O1 2.464(2) . ? Gd1 O7 2.509(3) . ? O1 C1 1.255(4) . ? O2 C2 1.264(4) . ? O2 Gd1 2.430(3) 4_545 ? O3 C3 1.250(4) . ? O4 C4 1.256(5) . ? O4 Gd1 2.322(3) 2_655 ? O5 C5 1.242(4) . ? O6 C6 1.248(4) . ? O6 Gd1 2.291(3) 4_545 ? O7 C7 1.431(6) . ? O7 H7O 0.79(4) . ? O8 C8 1.434(6) . ? O8 H8O 0.68(5) . ? C1 C2 1.459(5) 7_556 ? C1 C2 1.465(5) . ? C2 C1 1.459(5) 7_556 ? C3 C4 1.451(5) . ? C3 C4 1.461(5) 5_665 ? C4 C3 1.461(5) 5_665 ? C5 C6 1.456(5) . ? C5 C5 1.473(7) 2_655 ? C6 C6 1.453(7) 2_655 ? C7 C8 1.491(7) . ? C7 H7A 1.09(5) . ? C7 H7B 1.01(5) . ? C8 H8A 1.03(6) . ? C8 H8B 1.03(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Gd1 O5 140.98(10) 4 . ? O6 Gd1 O3 142.21(11) 4 . ? O5 Gd1 O3 73.96(10) . . ? O6 Gd1 O4 101.33(10) 4 2_655 ? O5 Gd1 O4 81.15(11) . 2_655 ? O3 Gd1 O4 97.85(10) . 2_655 ? O6 Gd1 O8 83.62(12) 4 . ? O5 Gd1 O8 75.70(12) . . ? O3 Gd1 O8 97.04(12) . . ? O4 Gd1 O8 147.70(11) 2_655 . ? O6 Gd1 O2 77.14(10) 4 4 ? O5 Gd1 O2 138.06(10) . 4 ? O3 Gd1 O2 78.20(10) . 4 ? O4 Gd1 O2 72.23(9) 2_655 4 ? O8 Gd1 O2 139.15(11) . 4 ? O6 Gd1 O1 70.75(10) 4 . ? O5 Gd1 O1 72.32(9) . . ? O3 Gd1 O1 146.25(10) . . ? O4 Gd1 O1 75.63(9) 2_655 . ? O8 Gd1 O1 76.07(11) . . ? O2 Gd1 O1 128.28(9) 4 . ? O6 Gd1 O7 74.50(11) 4 . ? O5 Gd1 O7 122.13(11) . . ? O3 Gd1 O7 72.16(10) . . ? O4 Gd1 O7 148.46(10) 2_655 . ? O8 Gd1 O7 63.77(11) . . ? O2 Gd1 O7 76.42(10) 4 . ? O1 Gd1 O7 128.91(10) . . ? C1 O1 Gd1 135.3(2) . . ? C2 O2 Gd1 140.6(2) . 4_545 ? C3 O3 Gd1 143.6(3) . . ? C4 O4 Gd1 131.4(3) . 2_655 ? C5 O5 Gd1 149.4(3) . . ? C6 O6 Gd1 156.1(3) . 4_545 ? C7 O7 Gd1 119.3(3) . . ? C7 O7 H7O 109(4) . . ? Gd1 O7 H7O 113(4) . . ? C8 O8 Gd1 119.2(3) . . ? C8 O8 H8O 112(4) . . ? Gd1 O8 H8O 127(4) . . ? O1 C1 C2 133.5(4) . 7_556 ? O1 C1 C2 136.5(4) . . ? C2 C1 C2 90.0(3) 7_556 . ? O2 C2 C1 135.3(4) . 7_556 ? O2 C2 C1 134.7(4) . . ? C1 C2 C1 90.0(3) 7_556 . ? O3 C3 C4 136.2(4) . . ? O3 C3 C4 134.0(4) . 5_665 ? C4 C3 C4 89.9(3) . 5_665 ? O4 C4 C3 135.9(4) . . ? O4 C4 C3 134.0(4) . 5_665 ? C3 C4 C3 90.1(3) . 5_665 ? O5 C5 C6 134.1(3) . . ? O5 C5 C5 136.3(2) . 2_655 ? C6 C5 C5 89.37(19) . 2_655 ? O6 C6 C6 133.4(2) . 2_655 ? O6 C6 C5 136.3(3) . . ? C6 C6 C5 90.18(19) 2_655 . ? O7 C7 C8 107.3(4) . . ? O7 C7 H7A 111(3) . . ? C8 C7 H7A 101(3) . . ? O7 C7 H7B 110(3) . . ? C8 C7 H7B 107(3) . . ? H7A C7 H7B 120(4) . . ? O8 C8 C7 106.2(4) . . ? O8 C8 H8A 108(4) . . ? C7 C8 H8A 106(4) . . ? O8 C8 H8B 111(3) . . ? C7 C8 H8B 112(3) . . ? H8A C8 H8B 112(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.797 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.167 #===End # # Tb(C4O4)1.5(C2H6O2) (compound 9) # data_TbSqEg _database_code_depnum_ccdc_archive 'CCDC 737278' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Tb(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 O8 Tb' _chemical_formula_weight 389.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.8165(5) _cell_length_b 12.1362(5) _cell_length_c 12.5928(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.083(2) _cell_angle_gamma 90.00 _cell_volume 1934.17(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 7.344 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5185 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13757 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.44 _reflns_number_total 2416 _reflns_number_gt 2305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+3.5891P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2416 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0143 _refine_ls_R_factor_gt 0.0133 _refine_ls_wR_factor_ref 0.0322 _refine_ls_wR_factor_gt 0.0319 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.273099(7) 0.463245(7) 0.222515(7) 0.00991(4) Uani 1 1 d . . . O1 O 0.23891(13) 0.40929(12) 0.40139(11) 0.0168(3) Uani 1 1 d . . . O2 O 0.20807(13) 0.14769(12) 0.34644(11) 0.0178(3) Uani 1 1 d . . . O3 O 0.37103(13) 0.43086(15) 0.08696(13) 0.0240(4) Uani 1 1 d . . . O4 O 0.59742(13) 0.55217(13) 0.16015(12) 0.0201(3) Uani 1 1 d . . . O5 O 0.37917(14) 0.31446(14) 0.27751(14) 0.0268(4) Uani 1 1 d . . . O6 O 0.37550(14) 0.05057(14) 0.24238(15) 0.0263(4) Uani 1 1 d . . . O7 O 0.14921(15) 0.46556(14) 0.04799(14) 0.0242(4) Uani 1 1 d . . . O8 O 0.15763(16) 0.30735(16) 0.18891(15) 0.0325(5) Uani 1 1 d . . . C1 C 0.24506(16) 0.32144(17) 0.45419(15) 0.0132(4) Uani 1 1 d . . . C2 C 0.23193(17) 0.20361(17) 0.43034(16) 0.0135(4) Uani 1 1 d . . . C3 C 0.44202(18) 0.46927(17) 0.04007(17) 0.0159(4) Uani 1 1 d . . . C4 C 0.54381(17) 0.52281(17) 0.07262(17) 0.0152(4) Uani 1 1 d . . . C5 C 0.44451(16) 0.24449(17) 0.25838(16) 0.0144(4) Uani 1 1 d . . . C6 C 0.44364(16) 0.12440(17) 0.25060(16) 0.0134(4) Uani 1 1 d . . . C7 C 0.0867(2) 0.3692(2) 0.0172(2) 0.0349(6) Uani 1 1 d . . . C8 C 0.0600(2) 0.3191(2) 0.1171(2) 0.0340(6) Uani 1 1 d . . . H7A H 0.132(3) 0.314(3) -0.015(3) 0.041 Uiso 1 1 d . . . H7B H 0.020(2) 0.385(3) -0.030(3) 0.041 Uiso 1 1 d . . . H8A H 0.014(2) 0.373(3) 0.151(2) 0.041 Uiso 1 1 d . . . H8B H 0.023(2) 0.250(3) 0.098(3) 0.041 Uiso 1 1 d . . . H7O H 0.180(3) 0.481(3) 0.000(3) 0.044(10) Uiso 1 1 d . . . H8O H 0.161(3) 0.256(3) 0.219(3) 0.041(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01064(6) 0.00930(6) 0.00991(5) 0.00127(3) 0.00200(4) 0.00186(3) O1 0.0290(9) 0.0094(7) 0.0128(7) 0.0016(5) 0.0062(6) 0.0017(6) O2 0.0292(9) 0.0126(7) 0.0106(7) -0.0026(5) 0.0000(6) -0.0009(6) O3 0.0227(9) 0.0295(9) 0.0228(8) 0.0009(7) 0.0127(7) -0.0035(7) O4 0.0224(9) 0.0224(8) 0.0133(7) -0.0030(6) -0.0040(6) 0.0045(6) O5 0.0263(9) 0.0193(9) 0.0375(10) 0.0077(7) 0.0140(7) 0.0137(7) O6 0.0230(9) 0.0227(9) 0.0357(10) -0.0065(7) 0.0120(7) -0.0128(7) O7 0.0267(9) 0.0303(10) 0.0150(8) 0.0049(6) 0.0016(7) -0.0060(7) O8 0.0407(11) 0.0197(10) 0.0309(10) 0.0117(8) -0.0134(8) -0.0117(8) C1 0.0175(10) 0.0118(10) 0.0106(9) -0.0015(7) 0.0034(7) 0.0003(8) C2 0.0172(10) 0.0122(10) 0.0110(9) 0.0003(7) 0.0017(7) 0.0005(8) C3 0.0157(10) 0.0175(11) 0.0149(10) 0.0010(7) 0.0038(8) 0.0039(8) C4 0.0161(11) 0.0169(11) 0.0124(9) 0.0010(7) 0.0019(8) 0.0048(8) C5 0.0147(10) 0.0140(10) 0.0145(9) 0.0036(7) 0.0022(7) 0.0031(8) C6 0.0137(10) 0.0127(10) 0.0141(9) 0.0003(7) 0.0033(7) -0.0018(8) C7 0.0407(17) 0.0358(16) 0.0235(13) 0.0008(11) -0.0096(11) -0.0086(13) C8 0.0336(15) 0.0260(14) 0.0386(15) 0.0057(11) -0.0061(11) -0.0115(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6 2.2830(16) 4 ? Tb1 O5 2.3002(16) . ? Tb1 O3 2.3065(16) . ? Tb1 O4 2.3082(16) 2_655 ? Tb1 O8 2.3981(18) . ? Tb1 O2 2.4267(15) 4 ? Tb1 O1 2.4508(14) . ? Tb1 O7 2.5000(17) . ? O1 C1 1.252(2) . ? O2 C2 1.252(2) . ? O2 Tb1 2.4267(15) 4_545 ? O3 C3 1.250(3) . ? O4 C4 1.255(3) . ? O4 Tb1 2.3082(16) 2_655 ? O5 C5 1.243(3) . ? O6 C6 1.244(3) . ? O6 Tb1 2.2830(16) 4_545 ? O7 C7 1.435(3) . ? O7 H7O 0.80(4) . ? O8 C8 1.431(3) . ? O8 H8O 0.73(3) . ? C1 C2 1.465(3) . ? C1 C2 1.469(3) 7_556 ? C2 C1 1.469(3) 7_556 ? C3 C4 1.457(3) . ? C3 C4 1.462(3) 5_665 ? C4 C3 1.462(3) 5_665 ? C5 C6 1.461(3) . ? C5 C5 1.471(4) 2_655 ? C6 C6 1.447(4) 2_655 ? C7 C8 1.485(4) . ? C7 H7A 1.01(3) . ? C7 H7B 0.98(3) . ? C8 H8A 1.03(3) . ? C8 H8B 0.98(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Tb1 O5 141.04(6) 4 . ? O6 Tb1 O3 142.23(6) 4 . ? O5 Tb1 O3 73.99(6) . . ? O6 Tb1 O4 101.33(6) 4 2_655 ? O5 Tb1 O4 80.98(6) . 2_655 ? O3 Tb1 O4 97.65(6) . 2_655 ? O6 Tb1 O8 83.68(7) 4 . ? O5 Tb1 O8 75.68(7) . . ? O3 Tb1 O8 97.33(7) . . ? O4 Tb1 O8 147.47(6) 2_655 . ? O6 Tb1 O2 76.95(6) 4 4 ? O5 Tb1 O2 138.11(6) . 4 ? O3 Tb1 O2 78.22(6) . 4 ? O4 Tb1 O2 72.28(5) 2_655 4 ? O8 Tb1 O2 139.29(6) . 4 ? O6 Tb1 O1 70.76(6) 4 . ? O5 Tb1 O1 72.33(5) . . ? O3 Tb1 O1 146.28(6) . . ? O4 Tb1 O1 75.60(5) 2_655 . ? O8 Tb1 O1 75.91(6) . . ? O2 Tb1 O1 128.14(5) 4 . ? O6 Tb1 O7 74.42(7) 4 . ? O5 Tb1 O7 122.46(6) . . ? O3 Tb1 O7 72.28(6) . . ? O4 Tb1 O7 148.23(5) 2_655 . ? O8 Tb1 O7 64.22(6) . . ? O2 Tb1 O7 76.13(5) 4 . ? O1 Tb1 O7 129.06(6) . . ? C1 O1 Tb1 135.24(13) . . ? C2 O2 Tb1 140.98(14) . 4_545 ? C3 O3 Tb1 143.85(16) . . ? C4 O4 Tb1 131.92(14) . 2_655 ? C5 O5 Tb1 149.59(15) . . ? C6 O6 Tb1 156.12(15) . 4_545 ? C7 O7 Tb1 118.56(14) . . ? C7 O7 H7O 108(3) . . ? Tb1 O7 H7O 110(3) . . ? C8 O8 Tb1 119.13(15) . . ? C8 O8 H8O 112(3) . . ? Tb1 O8 H8O 127(3) . . ? O1 C1 C2 136.59(19) . . ? O1 C1 C2 133.44(19) . 7_556 ? C2 C1 C2 89.97(16) . 7_556 ? O2 C2 C1 134.95(19) . . ? O2 C2 C1 134.99(19) . 7_556 ? C1 C2 C1 90.03(16) . 7_556 ? O3 C3 C4 136.0(2) . . ? O3 C3 C4 134.0(2) . 5_665 ? C4 C3 C4 90.05(17) . 5_665 ? O4 C4 C3 135.7(2) . . ? O4 C4 C3 134.4(2) . 5_665 ? C3 C4 C3 89.95(17) . 5_665 ? O5 C5 C6 134.2(2) . . ? O5 C5 C5 136.43(13) . 2_655 ? C6 C5 C5 89.29(11) . 2_655 ? O6 C6 C6 133.47(13) . 2_655 ? O6 C6 C5 136.2(2) . . ? C6 C6 C5 90.21(11) 2_655 . ? O7 C7 C8 107.4(2) . . ? O7 C7 H7A 108.8(18) . . ? C8 C7 H7A 106.5(18) . . ? O7 C7 H7B 113.5(18) . . ? C8 C7 H7B 107.4(18) . . ? H7A C7 H7B 113(3) . . ? O8 C8 C7 106.3(2) . . ? O8 C8 H8A 107.6(17) . . ? C7 C8 H8A 108.7(18) . . ? O8 C8 H8B 114.1(18) . . ? C7 C8 H8B 108.3(19) . . ? H8A C8 H8B 112(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.590 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.093 #===End # # Dy(C4O4)1.5(C2H6O2) (compound 10) # data_DySqEg _database_code_depnum_ccdc_archive 'CCDC 737279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Dy(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Dy O8' _chemical_formula_weight 392.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.7668(5) _cell_length_b 12.1015(5) _cell_length_c 12.5648(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.094(2) _cell_angle_gamma 90.00 _cell_volume 1916.83(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 7.828 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5019 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15693 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 29.82 _reflns_number_total 2700 _reflns_number_gt 2544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+3.4574P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00170(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2700 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0153 _refine_ls_R_factor_gt 0.0139 _refine_ls_wR_factor_ref 0.0322 _refine_ls_wR_factor_gt 0.0317 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.272914(6) 0.463223(7) 0.222460(7) 0.00971(4) Uani 1 1 d . . . O1 O 0.23904(12) 0.40961(12) 0.40111(11) 0.0164(3) Uani 1 1 d . . . O2 O 0.20857(12) 0.14711(12) 0.34619(11) 0.0182(3) Uani 1 1 d . . . O3 O 0.37056(12) 0.43096(14) 0.08704(13) 0.0231(3) Uani 1 1 d . . . O4 O 0.59815(12) 0.55228(13) 0.16053(12) 0.0196(3) Uani 1 1 d . . . O5 O 0.37852(13) 0.31480(13) 0.27727(14) 0.0261(4) Uani 1 1 d . . . O6 O 0.37498(13) 0.05002(13) 0.24224(15) 0.0254(4) Uani 1 1 d . . . O7 O 0.14914(14) 0.46581(14) 0.04818(14) 0.0231(4) Uani 1 1 d . . . O8 O 0.15803(15) 0.30772(15) 0.18938(15) 0.0314(4) Uani 1 1 d . . . C1 C 0.24523(15) 0.32161(16) 0.45403(15) 0.0127(4) Uani 1 1 d . . . C2 C 0.23217(15) 0.20337(16) 0.43037(15) 0.0129(4) Uani 1 1 d . . . C3 C 0.44166(16) 0.46931(16) 0.04022(17) 0.0152(4) Uani 1 1 d . . . C4 C 0.54459(16) 0.52271(16) 0.07290(16) 0.0142(4) Uani 1 1 d . . . C5 C 0.44386(15) 0.24457(16) 0.25816(16) 0.0138(4) Uani 1 1 d . . . C6 C 0.44306(14) 0.12443(16) 0.25028(15) 0.0125(4) Uani 1 1 d . . . C7 C 0.0864(2) 0.3694(2) 0.0168(2) 0.0326(6) Uani 1 1 d . . . C8 C 0.0598(2) 0.3191(2) 0.1175(2) 0.0310(5) Uani 1 1 d . . . H7A H 0.129(3) 0.314(3) -0.015(3) 0.068(11) Uiso 1 1 d . . . H7B H 0.019(2) 0.389(2) -0.030(2) 0.034(8) Uiso 1 1 d . . . H8A H 0.020(2) 0.247(2) 0.101(2) 0.035(8) Uiso 1 1 d . . . H8B H 0.015(3) 0.376(3) 0.149(3) 0.050(10) Uiso 1 1 d . . . H8O H 0.163(2) 0.252(2) 0.221(2) 0.022(7) Uiso 1 1 d . . . H7O H 0.177(3) 0.485(3) 0.003(3) 0.041(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01069(5) 0.00889(6) 0.00963(5) 0.00113(3) 0.00182(3) 0.00172(3) O1 0.0270(7) 0.0105(7) 0.0123(6) 0.0013(5) 0.0049(6) 0.0015(6) O2 0.0295(8) 0.0129(7) 0.0109(7) -0.0035(5) -0.0008(6) -0.0013(6) O3 0.0222(8) 0.0279(9) 0.0222(8) -0.0003(7) 0.0125(6) -0.0035(7) O4 0.0208(7) 0.0228(8) 0.0131(7) -0.0043(6) -0.0037(6) 0.0046(6) O5 0.0272(8) 0.0179(8) 0.0361(9) 0.0071(7) 0.0142(7) 0.0130(7) O6 0.0219(8) 0.0226(9) 0.0341(9) -0.0061(7) 0.0116(7) -0.0113(6) O7 0.0248(8) 0.0287(10) 0.0152(8) 0.0050(6) 0.0016(7) -0.0067(6) O8 0.0409(10) 0.0177(9) 0.0297(9) 0.0112(7) -0.0129(8) -0.0105(8) C1 0.0167(8) 0.0124(9) 0.0095(8) -0.0007(7) 0.0031(7) 0.0001(7) C2 0.0166(9) 0.0107(9) 0.0113(8) 0.0000(7) 0.0018(7) -0.0007(7) C3 0.0151(9) 0.0178(11) 0.0128(9) 0.0002(7) 0.0029(7) 0.0036(7) C4 0.0147(9) 0.0154(10) 0.0123(9) 0.0010(7) 0.0012(7) 0.0036(7) C5 0.0147(9) 0.0124(9) 0.0145(9) 0.0028(7) 0.0033(7) 0.0029(7) C6 0.0125(8) 0.0128(9) 0.0127(8) 0.0012(7) 0.0032(7) -0.0006(7) C7 0.0348(13) 0.0337(15) 0.0254(12) 0.0002(10) -0.0069(11) -0.0066(11) C8 0.0304(12) 0.0246(13) 0.0342(14) 0.0040(10) -0.0063(10) -0.0104(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O6 2.2649(15) 4 ? Dy1 O5 2.2857(15) . ? Dy1 O4 2.2952(16) 2_655 ? Dy1 O3 2.2961(14) . ? Dy1 O8 2.3817(18) . ? Dy1 O2 2.4117(14) 4 ? Dy1 O1 2.4400(13) . ? Dy1 O7 2.4899(17) . ? O1 C1 1.251(2) . ? O2 C2 1.254(2) . ? O2 Dy1 2.4117(14) 4_545 ? O3 C3 1.247(2) . ? O4 C4 1.253(2) . ? O4 Dy1 2.2952(15) 2_655 ? O5 C5 1.241(2) . ? O6 C6 1.244(2) . ? O6 Dy1 2.2649(15) 4_545 ? O7 C7 1.435(3) . ? O7 H7O 0.75(3) . ? O8 C8 1.431(3) . ? O8 H8O 0.78(3) . ? C1 C2 1.466(3) . ? C1 C2 1.467(3) 7_556 ? C2 C1 1.467(3) 7_556 ? C3 C4 1.463(3) 5_665 ? C3 C4 1.464(3) . ? C4 C3 1.463(3) 5_665 ? C5 C6 1.457(3) . ? C5 C5 1.480(4) 2_655 ? C6 C6 1.455(3) 2_655 ? C7 C8 1.492(4) . ? C7 H7A 0.99(4) . ? C7 H7B 1.00(3) . ? C8 H8A 1.02(3) . ? C8 H8B 1.02(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Dy1 O5 140.87(6) 4 . ? O6 Dy1 O4 101.10(6) 4 2_655 ? O5 Dy1 O4 81.19(6) . 2_655 ? O6 Dy1 O3 142.28(6) 4 . ? O5 Dy1 O3 74.11(6) . . ? O4 Dy1 O3 97.82(6) 2_655 . ? O6 Dy1 O8 83.75(7) 4 . ? O5 Dy1 O8 75.49(7) . . ? O4 Dy1 O8 147.39(6) 2_655 . ? O3 Dy1 O8 97.35(6) . . ? O6 Dy1 O2 76.94(5) 4 4 ? O5 Dy1 O2 138.27(5) . 4 ? O4 Dy1 O2 72.24(5) 2_655 4 ? O3 Dy1 O2 78.26(5) . 4 ? O8 Dy1 O2 139.39(6) . 4 ? O6 Dy1 O1 70.65(6) 4 . ? O5 Dy1 O1 72.29(5) . . ? O4 Dy1 O1 75.46(5) 2_655 . ? O3 Dy1 O1 146.35(6) . . ? O8 Dy1 O1 75.92(6) . . ? O2 Dy1 O1 128.03(5) 4 . ? O6 Dy1 O7 74.55(6) 4 . ? O5 Dy1 O7 122.48(6) . . ? O4 Dy1 O7 148.07(5) 2_655 . ? O3 Dy1 O7 72.17(6) . . ? O8 Dy1 O7 64.45(6) . . ? O2 Dy1 O7 76.01(5) 4 . ? O1 Dy1 O7 129.22(5) . . ? C1 O1 Dy1 135.20(12) . . ? C2 O2 Dy1 141.13(13) . 4_545 ? C3 O3 Dy1 143.85(15) . . ? C4 O4 Dy1 131.70(13) . 2_655 ? C5 O5 Dy1 149.61(14) . . ? C6 O6 Dy1 155.90(14) . 4_545 ? C7 O7 Dy1 118.73(14) . . ? C7 O7 H7O 111(3) . . ? Dy1 O7 H7O 111(3) . . ? C8 O8 Dy1 119.24(15) . . ? C8 O8 H8O 113(2) . . ? Dy1 O8 H8O 127(2) . . ? O1 C1 C2 136.68(18) . . ? O1 C1 C2 133.43(18) . 7_556 ? C2 C1 C2 89.88(15) . 7_556 ? O2 C2 C1 134.88(18) . . ? O2 C2 C1 134.97(18) . 7_556 ? C1 C2 C1 90.12(15) . 7_556 ? O3 C3 C4 133.7(2) . 5_665 ? O3 C3 C4 136.1(2) . . ? C4 C3 C4 90.18(16) 5_665 . ? O4 C4 C3 134.62(19) . 5_665 ? O4 C4 C3 135.54(19) . . ? C3 C4 C3 89.82(16) 5_665 . ? O5 C5 C6 134.34(18) . . ? O5 C5 C5 136.26(12) . 2_655 ? C6 C5 C5 89.27(10) . 2_655 ? O6 C6 C6 133.25(12) . 2_655 ? O6 C6 C5 136.45(18) . . ? C6 C6 C5 90.23(10) 2_655 . ? O7 C7 C8 106.9(2) . . ? O7 C7 H7A 110(2) . . ? C8 C7 H7A 106(2) . . ? O7 C7 H7B 111.5(17) . . ? C8 C7 H7B 107.9(16) . . ? H7A C7 H7B 114(3) . . ? O8 C8 C7 106.2(2) . . ? O8 C8 H8A 114.1(17) . . ? C7 C8 H8A 110.2(17) . . ? O8 C8 H8B 108.5(19) . . ? C7 C8 H8B 105.5(19) . . ? H8A C8 H8B 112(2) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 29.82 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.744 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.102 #===End # # Ho(C4O4)1.5(C2H6O2) (compound 11) # data_HoSqEg _database_code_depnum_ccdc_archive 'CCDC 737280' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Ho(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Ho O8' _chemical_formula_weight 395.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.7571(5) _cell_length_b 12.0918(5) _cell_length_c 12.5485(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.151(2) _cell_angle_gamma 90.00 _cell_volume 1911.05(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 8.312 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5123 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9103 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.37 _reflns_number_total 2384 _reflns_number_gt 2250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+4.4358P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2384 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0404 _refine_ls_wR_factor_gt 0.0398 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.272780(8) 0.463172(9) 0.222446(8) 0.01071(5) Uani 1 1 d . . . O1 O 0.23953(16) 0.40996(15) 0.40090(14) 0.0169(4) Uani 1 1 d . . . O2 O 0.20915(16) 0.14688(15) 0.34579(14) 0.0187(4) Uani 1 1 d . . . O3 O 0.37006(16) 0.43182(19) 0.08730(16) 0.0241(4) Uani 1 1 d . . . O4 O 0.59882(16) 0.55203(17) 0.16074(15) 0.0201(4) Uani 1 1 d . . . O5 O 0.37847(17) 0.31502(18) 0.27713(18) 0.0274(5) Uani 1 1 d . . . O6 O 0.37476(18) 0.04992(17) 0.24225(19) 0.0263(5) Uani 1 1 d . . . O7 O 0.14947(18) 0.46622(17) 0.04845(18) 0.0235(5) Uani 1 1 d . . . O8 O 0.1586(2) 0.30796(19) 0.18966(19) 0.0327(5) Uani 1 1 d . . . C1 C 0.2453(2) 0.3216(2) 0.45383(19) 0.0141(5) Uani 1 1 d . . . C2 C 0.2325(2) 0.2031(2) 0.4302(2) 0.0145(5) Uani 1 1 d . . . C3 C 0.4415(2) 0.4693(2) 0.0402(2) 0.0162(5) Uani 1 1 d . . . C4 C 0.5443(2) 0.5224(2) 0.0729(2) 0.0145(5) Uani 1 1 d . . . C5 C 0.4439(2) 0.2447(2) 0.2583(2) 0.0148(5) Uani 1 1 d . . . C6 C 0.44319(19) 0.1245(2) 0.2506(2) 0.0138(5) Uani 1 1 d . . . C7 C 0.0867(3) 0.3691(3) 0.0170(3) 0.0348(8) Uani 1 1 d . . . C8 C 0.0602(3) 0.3194(3) 0.1177(3) 0.0341(8) Uani 1 1 d . . . H7A H 0.131(4) 0.308(5) -0.017(4) 0.091(18) Uiso 1 1 d . . . H7B H 0.019(3) 0.387(3) -0.029(3) 0.037(10) Uiso 1 1 d . . . H8A H 0.019(3) 0.246(3) 0.098(3) 0.036(10) Uiso 1 1 d . . . H8B H 0.009(3) 0.375(3) 0.150(3) 0.039(11) Uiso 1 1 d . . . H8O H 0.164(3) 0.252(3) 0.222(3) 0.037(11) Uiso 1 1 d . . . H7O H 0.184(4) 0.483(3) 0.001(4) 0.041(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01132(7) 0.01008(7) 0.01049(7) 0.00115(4) 0.00098(4) 0.00167(4) O1 0.0282(10) 0.0106(9) 0.0124(8) 0.0014(7) 0.0045(7) 0.0019(7) O2 0.0295(10) 0.0131(9) 0.0121(9) -0.0034(7) -0.0005(8) -0.0017(8) O3 0.0220(10) 0.0309(11) 0.0217(10) 0.0015(9) 0.0105(8) -0.0034(9) O4 0.0211(10) 0.0233(10) 0.0134(9) -0.0035(7) -0.0050(8) 0.0041(8) O5 0.0284(11) 0.0211(11) 0.0355(12) 0.0075(9) 0.0132(9) 0.0134(9) O6 0.0232(11) 0.0228(11) 0.0350(12) -0.0063(9) 0.0109(9) -0.0122(8) O7 0.0232(11) 0.0298(12) 0.0165(10) 0.0046(8) -0.0002(9) -0.0062(8) O8 0.0421(13) 0.0203(11) 0.0293(12) 0.0115(9) -0.0144(10) -0.0109(10) C1 0.0166(12) 0.0138(12) 0.0119(11) -0.0011(9) 0.0026(9) -0.0007(10) C2 0.0180(12) 0.0128(12) 0.0124(11) 0.0001(9) 0.0022(10) -0.0001(10) C3 0.0163(12) 0.0182(13) 0.0144(12) 0.0009(9) 0.0036(10) 0.0038(10) C4 0.0156(12) 0.0161(13) 0.0115(11) -0.0003(9) 0.0012(10) 0.0047(10) C5 0.0148(12) 0.0154(12) 0.0141(12) 0.0030(9) 0.0018(9) 0.0022(10) C6 0.0146(12) 0.0145(12) 0.0126(11) 0.0007(9) 0.0024(9) -0.0005(10) C7 0.0370(18) 0.038(2) 0.0251(16) 0.0009(14) -0.0084(14) -0.0101(16) C8 0.0315(17) 0.0288(18) 0.0376(18) 0.0067(14) -0.0079(14) -0.0120(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O6 2.259(2) 4 ? Ho1 O5 2.281(2) . ? Ho1 O4 2.2852(19) 2_655 ? Ho1 O3 2.2867(19) . ? Ho1 O8 2.372(2) . ? Ho1 O2 2.4049(18) 4 ? Ho1 O1 2.4311(17) . ? Ho1 O7 2.480(2) . ? O1 C1 1.254(3) . ? O2 C2 1.254(3) . ? O2 Ho1 2.4049(18) 4_545 ? O3 C3 1.248(3) . ? O4 C4 1.258(3) . ? O4 Ho1 2.2852(19) 2_655 ? O5 C5 1.241(3) . ? O6 C6 1.248(3) . ? O6 Ho1 2.259(2) 4_545 ? O7 C7 1.441(4) . ? O7 H7O 0.82(4) . ? O8 C8 1.432(4) . ? O8 H8O 0.79(4) . ? C1 C2 1.467(4) . ? C1 C2 1.469(3) 7_556 ? C2 C1 1.469(3) 7_556 ? C3 C4 1.459(4) . ? C3 C4 1.462(4) 5_665 ? C4 C3 1.462(4) 5_665 ? C5 C6 1.456(4) . ? C5 C5 1.477(5) 2_655 ? C6 C6 1.452(5) 2_655 ? C7 C8 1.487(5) . ? C7 H7A 1.05(6) . ? C7 H7B 0.98(4) . ? C8 H8A 1.05(4) . ? C8 H8B 1.07(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ho1 O5 140.95(8) 4 . ? O6 Ho1 O4 100.98(8) 4 2_655 ? O5 Ho1 O4 81.21(8) . 2_655 ? O6 Ho1 O3 142.16(8) 4 . ? O5 Ho1 O3 74.24(8) . . ? O4 Ho1 O3 97.79(8) 2_655 . ? O6 Ho1 O8 83.88(9) 4 . ? O5 Ho1 O8 75.41(9) . . ? O4 Ho1 O8 147.28(7) 2_655 . ? O3 Ho1 O8 97.53(9) . . ? O6 Ho1 O2 76.76(7) 4 4 ? O5 Ho1 O2 138.32(7) . 4 ? O4 Ho1 O2 72.22(7) 2_655 4 ? O3 Ho1 O2 78.17(7) . 4 ? O8 Ho1 O2 139.49(7) . 4 ? O6 Ho1 O1 70.70(7) 4 . ? O5 Ho1 O1 72.33(7) . . ? O4 Ho1 O1 75.28(7) 2_655 . ? O3 Ho1 O1 146.51(7) . . ? O8 Ho1 O1 75.99(7) . . ? O2 Ho1 O1 127.81(6) 4 . ? O6 Ho1 O7 74.59(8) 4 . ? O5 Ho1 O7 122.57(8) . . ? O4 Ho1 O7 147.92(7) 2_655 . ? O3 Ho1 O7 72.10(8) . . ? O8 Ho1 O7 64.71(7) . . ? O2 Ho1 O7 75.88(6) 4 . ? O1 Ho1 O7 129.47(7) . . ? C1 O1 Ho1 135.17(16) . . ? C2 O2 Ho1 141.10(17) . 4_545 ? C3 O3 Ho1 144.5(2) . . ? C4 O4 Ho1 131.92(17) . 2_655 ? C5 O5 Ho1 149.82(19) . . ? C6 O6 Ho1 155.88(19) . 4_545 ? C7 O7 Ho1 118.45(18) . . ? C7 O7 H7O 110(3) . . ? Ho1 O7 H7O 108(3) . . ? C8 O8 Ho1 119.09(19) . . ? C8 O8 H8O 114(3) . . ? Ho1 O8 H8O 126(3) . . ? O1 C1 C2 136.9(2) . . ? O1 C1 C2 133.2(2) . 7_556 ? C2 C1 C2 90.0(2) . 7_556 ? O2 C2 C1 134.8(2) . . ? O2 C2 C1 135.2(2) . 7_556 ? C1 C2 C1 90.0(2) . 7_556 ? O3 C3 C4 136.0(3) . . ? O3 C3 C4 134.1(3) . 5_665 ? C4 C3 C4 89.9(2) . 5_665 ? O4 C4 C3 135.9(3) . . ? O4 C4 C3 134.0(3) . 5_665 ? C3 C4 C3 90.1(2) . 5_665 ? O5 C5 C6 134.4(2) . . ? O5 C5 C5 136.28(16) . 2_655 ? C6 C5 C5 89.25(14) . 2_655 ? O6 C6 C6 133.27(16) . 2_655 ? O6 C6 C5 136.4(2) . . ? C6 C6 C5 90.26(14) 2_655 . ? O7 C7 C8 106.8(3) . . ? O7 C7 H7A 112(3) . . ? C8 C7 H7A 105(3) . . ? O7 C7 H7B 113(2) . . ? C8 C7 H7B 107(2) . . ? H7A C7 H7B 113(4) . . ? O8 C8 C7 106.3(3) . . ? O8 C8 H8A 115(2) . . ? C7 C8 H8A 109(2) . . ? O8 C8 H8B 111(2) . . ? C7 C8 H8B 108(2) . . ? H8A C8 H8B 108(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.490 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.120 #===End # # Er(C4O4)1.5(C2H6O2) (compound 12) # data_ErSqEg _database_code_depnum_ccdc_archive 'CCDC 737281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Er(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Er O8' _chemical_formula_weight 397.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.7172(5) _cell_length_b 12.0666(5) _cell_length_c 12.5190(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.121(2) _cell_angle_gamma 90.00 _cell_volume 1896.79(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pillar-like _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 8.881 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5054 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9373 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2357 _reflns_number_gt 2227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+2.6834P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2357 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0200 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0489 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.272611(9) 0.463160(9) 0.222451(9) 0.00946(6) Uani 1 1 d . . . O1 O 0.23965(16) 0.41007(16) 0.40060(15) 0.0152(4) Uani 1 1 d . . . O2 O 0.20947(17) 0.14653(16) 0.34538(15) 0.0169(4) Uani 1 1 d . . . O3 O 0.36954(18) 0.4323(2) 0.08784(18) 0.0225(4) Uani 1 1 d . . . O4 O 0.59911(18) 0.55190(18) 0.16114(17) 0.0182(4) Uani 1 1 d . . . O5 O 0.37804(18) 0.31566(19) 0.2772(2) 0.0257(5) Uani 1 1 d . . . O6 O 0.37413(19) 0.04990(18) 0.2418(2) 0.0244(5) Uani 1 1 d . . . O7 O 0.1497(2) 0.46653(17) 0.0488(2) 0.0218(5) Uani 1 1 d . . . O8 O 0.1589(2) 0.3084(2) 0.1902(2) 0.0303(6) Uani 1 1 d . . . C1 C 0.2457(2) 0.3220(2) 0.4538(2) 0.0118(5) Uani 1 1 d . . . C2 C 0.2325(2) 0.2029(2) 0.4300(2) 0.0122(5) Uani 1 1 d . . . C3 C 0.4415(2) 0.4698(2) 0.0401(2) 0.0149(6) Uani 1 1 d . . . C4 C 0.5448(2) 0.5225(2) 0.0731(2) 0.0144(5) Uani 1 1 d . . . C5 C 0.4443(2) 0.2453(2) 0.2583(2) 0.0133(5) Uani 1 1 d . . . C6 C 0.4432(2) 0.1242(2) 0.2503(2) 0.0126(5) Uani 1 1 d . . . C7 C 0.0866(3) 0.3696(3) 0.0176(3) 0.0321(8) Uani 1 1 d . . . C8 C 0.0598(3) 0.3195(3) 0.1182(3) 0.0307(8) Uani 1 1 d . . . H7A H 0.125(4) 0.314(5) -0.020(4) 0.056(14) Uiso 1 1 d . . . H7B H 0.016(3) 0.387(3) -0.029(3) 0.031(10) Uiso 1 1 d . . . H8A H 0.020(3) 0.247(3) 0.101(3) 0.029(10) Uiso 1 1 d . . . H8B H 0.015(3) 0.372(4) 0.154(3) 0.035(11) Uiso 1 1 d . . . H7O H 0.180(4) 0.481(3) -0.003(4) 0.029(11) Uiso 1 1 d . . . H8O H 0.169(4) 0.248(4) 0.216(4) 0.045(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01039(8) 0.00872(8) 0.00934(8) 0.00104(3) 0.00177(5) 0.00156(4) O1 0.0256(10) 0.0086(9) 0.0121(9) 0.0024(7) 0.0046(8) 0.0025(7) O2 0.0283(11) 0.0107(9) 0.0104(9) -0.0028(7) -0.0004(8) -0.0008(8) O3 0.0205(11) 0.0292(11) 0.0205(11) 0.0030(9) 0.0113(9) -0.0037(9) O4 0.0190(10) 0.0214(11) 0.0123(10) -0.0044(8) -0.0038(8) 0.0040(8) O5 0.0262(11) 0.0176(11) 0.0364(13) 0.0069(10) 0.0145(10) 0.0121(9) O6 0.0215(11) 0.0206(11) 0.0335(13) -0.0060(9) 0.0122(10) -0.0113(9) O7 0.0235(12) 0.0266(13) 0.0147(11) 0.0045(8) 0.0009(9) -0.0055(8) O8 0.0376(14) 0.0176(12) 0.0293(12) 0.0100(10) -0.0145(10) -0.0093(10) C1 0.0144(12) 0.0113(12) 0.0102(11) -0.0007(9) 0.0038(9) 0.0001(9) C2 0.0142(12) 0.0107(12) 0.0115(12) -0.0005(9) 0.0018(10) 0.0006(10) C3 0.0166(14) 0.0138(13) 0.0146(14) 0.0019(9) 0.0034(11) 0.0043(10) C4 0.0161(13) 0.0141(13) 0.0126(13) 0.0001(10) 0.0012(11) 0.0043(10) C5 0.0136(13) 0.0119(12) 0.0143(12) 0.0040(10) 0.0024(10) 0.0030(10) C6 0.0151(13) 0.0122(13) 0.0111(12) 0.0003(9) 0.0038(10) -0.0002(10) C7 0.0370(19) 0.0319(19) 0.0230(17) 0.0002(14) -0.0083(15) -0.0087(16) C8 0.0304(18) 0.0267(18) 0.0317(18) 0.0060(14) -0.0054(14) -0.0099(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O6 2.246(2) 4 ? Er1 O5 2.268(2) . ? Er1 O3 2.271(2) . ? Er1 O4 2.276(2) 2_655 ? Er1 O8 2.357(2) . ? Er1 O2 2.3938(19) 4 ? Er1 O1 2.4200(19) . ? Er1 O7 2.469(2) . ? O1 C1 1.250(3) . ? O2 C2 1.254(3) . ? O2 Er1 2.3938(19) 4_545 ? O3 C3 1.254(4) . ? O4 C4 1.255(4) . ? O4 Er1 2.276(2) 2_655 ? O5 C5 1.245(3) . ? O6 C6 1.248(3) . ? O6 Er1 2.246(2) 4_545 ? O7 C7 1.438(4) . ? O7 H7O 0.82(4) . ? O8 C8 1.435(4) . ? O8 H8O 0.80(5) . ? C1 C2 1.467(3) 7_556 ? C1 C2 1.472(4) . ? C2 C1 1.467(3) 7_556 ? C3 C4 1.457(4) 5_665 ? C3 C4 1.460(4) . ? C4 C3 1.457(4) 5_665 ? C5 C5 1.464(5) 2_655 ? C5 C6 1.465(4) . ? C6 C6 1.445(5) 2_655 ? C7 C8 1.484(5) . ? C7 H7A 0.99(5) . ? C7 H7B 1.01(4) . ? C8 H8A 1.02(4) . ? C8 H8B 1.00(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Er1 O5 140.87(8) 4 . ? O6 Er1 O3 142.23(9) 4 . ? O5 Er1 O3 74.39(8) . . ? O6 Er1 O4 100.78(9) 4 2_655 ? O5 Er1 O4 81.16(8) . 2_655 ? O3 Er1 O4 97.71(8) . 2_655 ? O6 Er1 O8 84.06(9) 4 . ? O5 Er1 O8 75.37(10) . . ? O3 Er1 O8 97.68(9) . . ? O4 Er1 O8 147.20(8) 2_655 . ? O6 Er1 O2 76.63(8) 4 4 ? O5 Er1 O2 138.38(8) . 4 ? O3 Er1 O2 78.17(8) . 4 ? O4 Er1 O2 72.14(7) 2_655 4 ? O8 Er1 O2 139.62(7) . 4 ? O6 Er1 O1 70.66(8) 4 . ? O5 Er1 O1 72.20(7) . . ? O3 Er1 O1 146.53(8) . . ? O4 Er1 O1 75.27(7) 2_655 . ? O8 Er1 O1 75.93(8) . . ? O2 Er1 O1 127.72(7) 4 . ? O6 Er1 O7 74.81(9) 4 . ? O5 Er1 O7 122.71(8) . . ? O3 Er1 O7 72.02(9) . . ? O4 Er1 O7 147.76(7) 2_655 . ? O8 Er1 O7 64.95(8) . . ? O2 Er1 O7 75.81(7) 4 . ? O1 Er1 O7 129.65(8) . . ? C1 O1 Er1 135.34(17) . . ? C2 O2 Er1 141.12(18) . 4_545 ? C3 O3 Er1 144.8(2) . . ? C4 O4 Er1 131.92(18) . 2_655 ? C5 O5 Er1 149.7(2) . . ? C6 O6 Er1 156.0(2) . 4_545 ? C7 O7 Er1 118.28(19) . . ? C7 O7 H7O 106(3) . . ? Er1 O7 H7O 113(3) . . ? C8 O8 Er1 119.2(2) . . ? C8 O8 H8O 114(3) . . ? Er1 O8 H8O 127(3) . . ? O1 C1 C2 133.5(2) . 7_556 ? O1 C1 C2 136.6(2) . . ? C2 C1 C2 89.9(2) 7_556 . ? O2 C2 C1 135.1(3) . 7_556 ? O2 C2 C1 134.8(3) . . ? C1 C2 C1 90.1(2) 7_556 . ? O3 C3 C4 134.0(3) . 5_665 ? O3 C3 C4 135.6(3) . . ? C4 C3 C4 90.4(2) 5_665 . ? O4 C4 C3 134.6(3) . 5_665 ? O4 C4 C3 135.8(3) . . ? C3 C4 C3 89.6(2) 5_665 . ? O5 C5 C5 136.56(17) . 2_655 ? O5 C5 C6 134.0(3) . . ? C5 C5 C6 89.37(15) 2_655 . ? O6 C6 C6 133.65(17) . 2_655 ? O6 C6 C5 136.1(3) . . ? C6 C6 C5 90.12(15) 2_655 . ? O7 C7 C8 107.2(3) . . ? O7 C7 H7A 112(3) . . ? C8 C7 H7A 109(3) . . ? O7 C7 H7B 113(2) . . ? C8 C7 H7B 106(2) . . ? H7A C7 H7B 109(4) . . ? O8 C8 C7 105.9(3) . . ? O8 C8 H8A 114(2) . . ? C7 C8 H8A 110(2) . . ? O8 C8 H8B 107(2) . . ? C7 C8 H8B 110(2) . . ? H8A C8 H8B 110(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.377 _refine_diff_density_min -1.603 _refine_diff_density_rms 0.176 #===End # # Tm(C4O4)1.5(C2H6O2) (compound 13) # data_TmSqEg _database_code_depnum_ccdc_archive 'CCDC 737282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Tm(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 O8 Tm' _chemical_formula_weight 399.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.6881(5) _cell_length_b 12.0386(5) _cell_length_c 12.4922(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.185(2) _cell_angle_gamma 90.00 _cell_volume 1883.68(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pillar-like _exptl_crystal_colour light-purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 9.452 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6142 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8249 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2335 _reflns_number_gt 2130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+0.7226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2335 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0185 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0357 _refine_ls_wR_factor_gt 0.0350 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.272358(8) 0.463130(8) 0.222429(8) 0.00922(4) Uani 1 1 d . . . O1 O 0.23977(15) 0.41062(14) 0.40050(14) 0.0151(4) Uani 1 1 d . . . O2 O 0.20983(15) 0.14643(15) 0.34518(14) 0.0167(4) Uani 1 1 d . . . O3 O 0.36902(16) 0.43283(17) 0.08785(16) 0.0223(4) Uani 1 1 d . . . O4 O 0.59977(16) 0.55125(15) 0.16144(15) 0.0181(4) Uani 1 1 d . . . O5 O 0.37770(16) 0.31584(16) 0.27678(17) 0.0246(5) Uani 1 1 d . . . O6 O 0.37421(17) 0.04917(16) 0.24234(17) 0.0229(5) Uani 1 1 d . . . O7 O 0.14948(19) 0.46654(17) 0.04919(18) 0.0214(5) Uani 1 1 d . . . O8 O 0.1587(2) 0.3089(2) 0.19059(19) 0.0306(6) Uani 1 1 d . . . C1 C 0.2456(2) 0.3219(2) 0.4536(2) 0.0119(5) Uani 1 1 d . . . C2 C 0.2330(2) 0.2029(2) 0.4297(2) 0.0122(5) Uani 1 1 d . . . C3 C 0.4414(2) 0.4698(2) 0.0408(2) 0.0140(5) Uani 1 1 d . . . C4 C 0.5447(2) 0.5223(2) 0.0732(2) 0.0135(5) Uani 1 1 d . . . C5 C 0.4437(2) 0.2450(2) 0.2580(2) 0.0128(5) Uani 1 1 d . . . C6 C 0.44289(19) 0.1242(2) 0.2504(2) 0.0113(5) Uani 1 1 d . . . C7 C 0.0861(3) 0.3696(3) 0.0177(3) 0.0314(8) Uani 1 1 d . . . C8 C 0.0598(3) 0.3190(3) 0.1180(3) 0.0305(7) Uani 1 1 d . . . H7A H 0.130(4) 0.312(4) -0.018(4) 0.081(15) Uiso 1 1 d . . . H7B H 0.017(3) 0.387(2) -0.029(3) 0.025(8) Uiso 1 1 d . . . H8A H 0.023(2) 0.246(3) 0.096(2) 0.023(8) Uiso 1 1 d . . . H8B H 0.013(3) 0.375(3) 0.145(3) 0.056(12) Uiso 1 1 d . . . H7O H 0.179(4) 0.479(3) 0.003(3) 0.046(13) Uiso 1 1 d . . . H8O H 0.169(3) 0.258(3) 0.215(3) 0.031(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tm1 0.00969(7) 0.00837(7) 0.00952(6) 0.00102(4) 0.00126(5) 0.00151(4) O1 0.0237(10) 0.0093(9) 0.0123(9) 0.0025(7) 0.0032(8) 0.0006(8) O2 0.0276(11) 0.0124(9) 0.0095(9) -0.0038(7) 0.0008(8) -0.0025(8) O3 0.0193(11) 0.0289(11) 0.0212(11) 0.0003(9) 0.0106(9) -0.0032(9) O4 0.0205(11) 0.0191(10) 0.0124(10) -0.0043(7) -0.0039(8) 0.0036(8) O5 0.0250(11) 0.0170(10) 0.0342(12) 0.0060(9) 0.0120(10) 0.0126(9) O6 0.0210(11) 0.0199(11) 0.0294(12) -0.0056(8) 0.0093(10) -0.0113(8) O7 0.0231(12) 0.0260(12) 0.0149(11) 0.0050(8) 0.0021(9) -0.0063(9) O8 0.0388(14) 0.0166(12) 0.0301(13) 0.0121(10) -0.0139(11) -0.0075(10) C1 0.0134(12) 0.0125(12) 0.0098(12) 0.0006(10) 0.0013(10) 0.0011(10) C2 0.0139(13) 0.0107(12) 0.0118(12) 0.0002(10) 0.0018(10) 0.0000(10) C3 0.0151(13) 0.0162(14) 0.0108(12) -0.0005(9) 0.0026(11) 0.0047(10) C4 0.0133(13) 0.0145(13) 0.0123(13) -0.0004(10) 0.0009(11) 0.0033(10) C5 0.0113(13) 0.0127(13) 0.0143(12) 0.0031(10) 0.0016(11) 0.0020(10) C6 0.0087(12) 0.0121(13) 0.0125(12) 0.0015(9) 0.0001(10) -0.0011(10) C7 0.0321(19) 0.0343(19) 0.0226(16) 0.0011(14) -0.0111(15) -0.0089(16) C8 0.0283(18) 0.0251(18) 0.0335(18) 0.0079(14) -0.0091(15) -0.0089(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 O6 2.2330(19) 4 ? Tm1 O5 2.2587(19) . ? Tm1 O4 2.261(2) 2_655 ? Tm1 O3 2.2631(18) . ? Tm1 O8 2.346(2) . ? Tm1 O2 2.3864(17) 4 ? Tm1 O1 2.4110(17) . ? Tm1 O7 2.457(2) . ? O1 C1 1.253(3) . ? O2 C2 1.251(3) . ? O2 Tm1 2.3864(17) 4_545 ? O3 C3 1.249(3) . ? O4 C4 1.257(3) . ? O4 Tm1 2.261(2) 2_655 ? O5 C5 1.243(3) . ? O6 C6 1.248(3) . ? O6 Tm1 2.2330(19) 4_545 ? O7 C7 1.436(4) . ? O7 H7O 0.75(4) . ? O8 C8 1.431(4) . ? O8 H8O 0.69(3) . ? C1 C2 1.466(3) . ? C1 C2 1.470(3) 7_556 ? C2 C1 1.470(3) 7_556 ? C3 C4 1.452(4) . ? C3 C4 1.466(4) 5_665 ? C4 C3 1.466(4) 5_665 ? C5 C6 1.457(3) . ? C5 C5 1.474(5) 2_655 ? C6 C6 1.451(5) 2_655 ? C7 C8 1.478(5) . ? C7 H7A 1.03(5) . ? C7 H7B 1.00(3) . ? C8 H8A 1.02(3) . ? C8 H8B 0.99(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Tm1 O5 140.93(7) 4 . ? O6 Tm1 O4 101.00(8) 4 2_655 ? O5 Tm1 O4 81.13(7) . 2_655 ? O6 Tm1 O3 142.03(8) 4 . ? O5 Tm1 O3 74.45(7) . . ? O4 Tm1 O3 97.69(7) 2_655 . ? O6 Tm1 O8 83.78(8) 4 . ? O5 Tm1 O8 75.41(9) . . ? O4 Tm1 O8 147.05(7) 2_655 . ? O3 Tm1 O8 97.93(8) . . ? O6 Tm1 O2 76.69(7) 4 4 ? O5 Tm1 O2 138.36(7) . 4 ? O4 Tm1 O2 72.20(6) 2_655 4 ? O3 Tm1 O2 78.05(7) . 4 ? O8 Tm1 O2 139.66(7) . 4 ? O6 Tm1 O1 70.66(7) 4 . ? O5 Tm1 O1 72.38(7) . . ? O4 Tm1 O1 75.06(7) 2_655 . ? O3 Tm1 O1 146.75(7) . . ? O8 Tm1 O1 75.97(7) . . ? O2 Tm1 O1 127.51(6) 4 . ? O6 Tm1 O7 74.60(8) 4 . ? O5 Tm1 O7 122.66(7) . . ? O4 Tm1 O7 147.86(7) 2_655 . ? O3 Tm1 O7 72.02(8) . . ? O8 Tm1 O7 65.00(7) . . ? O2 Tm1 O7 75.85(6) 4 . ? O1 Tm1 O7 129.70(7) . . ? C1 O1 Tm1 135.03(16) . . ? C2 O2 Tm1 141.16(17) . 4_545 ? C3 O3 Tm1 144.96(18) . . ? C4 O4 Tm1 132.41(17) . 2_655 ? C5 O5 Tm1 149.95(18) . . ? C6 O6 Tm1 155.86(17) . 4_545 ? C7 O7 Tm1 118.43(17) . . ? C7 O7 H7O 106(3) . . ? Tm1 O7 H7O 111(4) . . ? C8 O8 Tm1 119.57(19) . . ? C8 O8 H8O 116(3) . . ? Tm1 O8 H8O 124(3) . . ? O1 C1 C2 136.9(2) . . ? O1 C1 C2 133.1(2) . 7_556 ? C2 C1 C2 89.99(19) . 7_556 ? O2 C2 C1 134.9(2) . . ? O2 C2 C1 135.0(2) . 7_556 ? C1 C2 C1 90.01(19) . 7_556 ? O3 C3 C4 136.3(3) . . ? O3 C3 C4 133.8(3) . 5_665 ? C4 C3 C4 89.9(2) . 5_665 ? O4 C4 C3 135.7(3) . . ? O4 C4 C3 134.2(3) . 5_665 ? C3 C4 C3 90.1(2) . 5_665 ? O5 C5 C6 134.3(2) . . ? O5 C5 C5 136.24(16) . 2_655 ? C6 C5 C5 89.32(14) . 2_655 ? O6 C6 C6 133.21(15) . 2_655 ? O6 C6 C5 136.5(2) . . ? C6 C6 C5 90.21(14) 2_655 . ? O7 C7 C8 107.2(3) . . ? O7 C7 H7A 111(3) . . ? C8 C7 H7A 107(2) . . ? O7 C7 H7B 113.3(18) . . ? C8 C7 H7B 106.6(18) . . ? H7A C7 H7B 112(3) . . ? O8 C8 C7 106.1(3) . . ? O8 C8 H8A 114.6(17) . . ? C7 C8 H8A 106.4(17) . . ? O8 C8 H8B 111(2) . . ? C7 C8 H8B 104(2) . . ? H8A C8 H8B 114(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.673 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.119 #===End # # Yb(C4O4)1.5(C2H6O2) (compound 14) # data_YbSqEg _database_code_depnum_ccdc_archive 'CCDC 737283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Yb(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 O8 Yb' _chemical_formula_weight 403.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.6497(15) _cell_length_b 12.0106(14) _cell_length_c 12.4708(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.221(3) _cell_angle_gamma 90.00 _cell_volume 1870.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour light-orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 10.033 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5269 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6839 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2262 _reflns_number_gt 2095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+3.9433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2262 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0489 _refine_ls_wR_factor_gt 0.0478 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.272198(11) 0.463055(11) 0.222348(10) 0.00878(6) Uani 1 1 d . . . O1 O 0.2397(2) 0.41060(19) 0.40022(19) 0.0151(5) Uani 1 1 d . . . O2 O 0.2098(2) 0.1461(2) 0.34481(19) 0.0166(5) Uani 1 1 d . . . O3 O 0.3685(2) 0.4327(2) 0.0881(2) 0.0208(6) Uani 1 1 d . . . O4 O 0.6005(2) 0.5514(2) 0.1619(2) 0.0185(5) Uani 1 1 d . . . O5 O 0.3773(2) 0.3162(2) 0.2768(2) 0.0234(6) Uani 1 1 d . . . O6 O 0.3736(2) 0.0491(2) 0.2422(2) 0.0226(6) Uani 1 1 d . . . O7 O 0.1489(3) 0.4667(2) 0.0492(2) 0.0215(6) Uani 1 1 d . . . O8 O 0.1588(3) 0.3090(3) 0.1906(3) 0.0294(7) Uani 1 1 d . . . C1 C 0.2456(3) 0.3221(3) 0.4537(3) 0.0115(6) Uani 1 1 d . . . C2 C 0.2327(3) 0.2028(3) 0.4297(3) 0.0116(6) Uani 1 1 d . . . C3 C 0.4408(3) 0.4705(3) 0.0408(3) 0.0142(7) Uani 1 1 d . . . C4 C 0.5458(3) 0.5223(3) 0.0734(3) 0.0135(7) Uani 1 1 d . . . C5 C 0.4436(3) 0.2456(3) 0.2579(3) 0.0121(7) Uani 1 1 d . . . C6 C 0.4431(3) 0.1239(3) 0.2506(3) 0.0114(6) Uani 1 1 d . . . C7 C 0.0856(4) 0.3696(4) 0.0169(4) 0.0295(9) Uani 1 1 d . . . C8 C 0.0603(4) 0.3191(4) 0.1191(4) 0.0300(10) Uani 1 1 d . . . H7A H 0.122(4) 0.315(4) -0.018(4) 0.036 Uiso 1 1 d . . . H7B H 0.021(4) 0.387(4) -0.032(4) 0.036 Uiso 1 1 d . . . H8A H 0.005(4) 0.371(4) 0.150(4) 0.036 Uiso 1 1 d . . . H8B H 0.017(4) 0.249(4) 0.105(4) 0.036 Uiso 1 1 d . . . H7O H 0.186(5) 0.485(5) 0.002(5) 0.050(18) Uiso 1 1 d . . . H8O H 0.162(4) 0.256(4) 0.216(4) 0.033(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.00960(9) 0.00730(9) 0.00965(8) 0.00093(5) 0.00217(6) 0.00151(5) O1 0.0246(14) 0.0088(12) 0.0128(11) 0.0028(9) 0.0059(10) 0.0031(10) O2 0.0264(15) 0.0103(12) 0.0131(11) -0.0044(9) 0.0029(11) -0.0011(10) O3 0.0204(14) 0.0241(14) 0.0205(13) 0.0011(11) 0.0112(12) -0.0030(12) O4 0.0202(14) 0.0187(13) 0.0146(12) -0.0044(10) -0.0035(11) 0.0030(11) O5 0.0241(15) 0.0172(13) 0.0314(15) 0.0068(12) 0.0123(13) 0.0124(12) O6 0.0229(15) 0.0174(14) 0.0299(15) -0.0062(11) 0.0111(13) -0.0107(11) O7 0.0227(15) 0.0255(16) 0.0157(13) 0.0053(10) 0.0010(12) -0.0063(11) O8 0.0358(18) 0.0169(15) 0.0295(15) 0.0099(13) -0.0131(14) -0.0109(13) C1 0.0128(16) 0.0109(16) 0.0112(14) 0.0006(12) 0.0028(13) 0.0012(13) C2 0.0119(16) 0.0120(16) 0.0112(14) 0.0004(12) 0.0023(13) -0.0006(13) C3 0.0156(18) 0.0135(18) 0.0140(16) 0.0025(12) 0.0042(14) 0.0041(13) C4 0.0151(18) 0.0131(17) 0.0123(15) 0.0007(12) 0.0025(14) 0.0052(13) C5 0.0124(17) 0.0094(16) 0.0144(15) 0.0034(12) 0.0023(13) 0.0034(13) C6 0.0135(17) 0.0108(16) 0.0106(13) -0.0005(12) 0.0039(13) -0.0014(13) C7 0.031(2) 0.032(2) 0.0223(19) 0.0005(17) -0.0058(18) -0.006(2) C8 0.030(2) 0.023(2) 0.033(2) 0.0053(18) -0.0056(19) -0.0111(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O6 2.219(3) 4 ? Yb1 O5 2.248(3) . ? Yb1 O4 2.249(3) 2_655 ? Yb1 O3 2.253(2) . ? Yb1 O8 2.336(3) . ? Yb1 O2 2.377(2) 4 ? Yb1 O1 2.404(2) . ? Yb1 O7 2.453(3) . ? O1 C1 1.250(4) . ? O2 C2 1.253(4) . ? O2 Yb1 2.377(2) 4_545 ? O3 C3 1.250(4) . ? O4 C4 1.255(4) . ? O4 Yb1 2.249(3) 2_655 ? O5 C5 1.241(4) . ? O6 C6 1.250(4) . ? O6 Yb1 2.219(3) 4_545 ? O7 C7 1.435(5) . ? O7 H7O 0.83(6) . ? O8 C8 1.417(5) . ? O8 H8O 0.71(5) . ? C1 C2 1.466(4) 7_556 ? C1 C2 1.468(5) . ? C2 C1 1.466(4) 7_556 ? C3 C4 1.464(5) . ? C3 C4 1.464(5) 5_665 ? C4 C3 1.464(5) 5_665 ? C5 C6 1.465(5) . ? C5 C5 1.472(7) 2_655 ? C6 C6 1.442(7) 2_655 ? C7 C8 1.492(6) . ? C7 H7A 0.95(5) . ? C7 H7B 0.96(5) . ? C8 H8A 1.05(5) . ? C8 H8B 1.01(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Yb1 O5 140.84(10) 4 . ? O6 Yb1 O4 100.66(11) 4 2_655 ? O5 Yb1 O4 81.29(10) . 2_655 ? O6 Yb1 O3 142.12(11) 4 . ? O5 Yb1 O3 74.51(10) . . ? O4 Yb1 O3 97.84(10) 2_655 . ? O6 Yb1 O8 83.97(12) 4 . ? O5 Yb1 O8 75.35(12) . . ? O4 Yb1 O8 147.12(10) 2_655 . ? O3 Yb1 O8 97.83(11) . . ? O6 Yb1 O2 76.66(9) 4 4 ? O5 Yb1 O2 138.34(10) . 4 ? O4 Yb1 O2 71.97(9) 2_655 4 ? O3 Yb1 O2 78.13(9) . 4 ? O8 Yb1 O2 139.81(10) . 4 ? O6 Yb1 O1 70.59(10) 4 . ? O5 Yb1 O1 72.30(9) . . ? O4 Yb1 O1 75.06(9) 2_655 . ? O3 Yb1 O1 146.73(10) . . ? O8 Yb1 O1 75.98(10) . . ? O2 Yb1 O1 127.44(8) 4 . ? O6 Yb1 O7 74.65(11) 4 . ? O5 Yb1 O7 122.81(10) . . ? O4 Yb1 O7 147.71(9) 2_655 . ? O3 Yb1 O7 72.09(10) . . ? O8 Yb1 O7 65.05(10) . . ? O2 Yb1 O7 75.91(9) 4 . ? O1 Yb1 O7 129.65(10) . . ? C1 O1 Yb1 135.3(2) . . ? C2 O2 Yb1 141.1(2) . 4_545 ? C3 O3 Yb1 144.6(2) . . ? C4 O4 Yb1 132.1(2) . 2_655 ? C5 O5 Yb1 149.7(2) . . ? C6 O6 Yb1 156.0(2) . 4_545 ? C7 O7 Yb1 118.7(2) . . ? C7 O7 H7O 111(4) . . ? Yb1 O7 H7O 106(5) . . ? C8 O8 Yb1 119.6(2) . . ? C8 O8 H8O 110(5) . . ? Yb1 O8 H8O 130(5) . . ? O1 C1 C2 133.5(3) . 7_556 ? O1 C1 C2 136.5(3) . . ? C2 C1 C2 90.0(3) 7_556 . ? O2 C2 C1 135.1(3) . 7_556 ? O2 C2 C1 134.9(3) . . ? C1 C2 C1 90.0(3) 7_556 . ? O3 C3 C4 136.3(3) . . ? O3 C3 C4 133.5(4) . 5_665 ? C4 C3 C4 90.2(3) . 5_665 ? O4 C4 C3 135.3(3) . . ? O4 C4 C3 134.9(4) . 5_665 ? C3 C4 C3 89.8(3) . 5_665 ? O5 C5 C6 134.2(3) . . ? O5 C5 C5 136.4(2) . 2_655 ? C6 C5 C5 89.21(19) . 2_655 ? O6 C6 C6 133.6(2) . 2_655 ? O6 C6 C5 136.0(3) . . ? C6 C6 C5 90.36(19) 2_655 . ? O7 C7 C8 106.1(3) . . ? O7 C7 H7A 114(3) . . ? C8 C7 H7A 107(3) . . ? O7 C7 H7B 112(3) . . ? C8 C7 H7B 111(3) . . ? H7A C7 H7B 107(4) . . ? O8 C8 C7 106.6(4) . . ? O8 C8 H8A 113(3) . . ? C7 C8 H8A 108(3) . . ? O8 C8 H8B 116(3) . . ? C7 C8 H8B 112(3) . . ? H8A C8 H8B 101(4) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.099 _refine_diff_density_min -1.735 _refine_diff_density_rms 0.193 #===End # # Lu(C4O4)1.5(C2H6O2) (compound 15) # data_LuSqEg _database_code_depnum_ccdc_archive 'CCDC 737284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Lu(C4O4)1.5(C2H6O2) _chemical_formula_sum 'C8 H6 Lu O8' _chemical_formula_weight 405.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.6351(5) _cell_length_b 12.0129(5) _cell_length_c 12.4584(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.177(2) _cell_angle_gamma 90.00 _cell_volume 1866.78(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pillar-like _exptl_crystal_colour light-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 10.609 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4797 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8336 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.44 _reflns_number_total 2326 _reflns_number_gt 2234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SHELXTL' _computing_cell_refinement 'Bruker SHELXTL' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+4.7692P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2326 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0156 _refine_ls_R_factor_gt 0.0147 _refine_ls_wR_factor_ref 0.0367 _refine_ls_wR_factor_gt 0.0362 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.272123(7) 0.463111(7) 0.222391(8) 0.00995(4) Uani 1 1 d . . . O1 O 0.23999(15) 0.41073(14) 0.40041(14) 0.0160(4) Uani 1 1 d . . . O2 O 0.21038(15) 0.14582(14) 0.34453(14) 0.0169(4) Uani 1 1 d . . . O3 O 0.36844(16) 0.43336(18) 0.08861(17) 0.0220(4) Uani 1 1 d . . . O4 O 0.60071(16) 0.55093(15) 0.16190(16) 0.0189(4) Uani 1 1 d . . . O5 O 0.37687(16) 0.31630(17) 0.27661(18) 0.0249(4) Uani 1 1 d . . . O6 O 0.37393(17) 0.04883(16) 0.24163(19) 0.0232(4) Uani 1 1 d . . . O7 O 0.14976(18) 0.46722(16) 0.04955(19) 0.0221(4) Uani 1 1 d . . . O8 O 0.15986(19) 0.30935(18) 0.19105(19) 0.0299(5) Uani 1 1 d . . . C1 C 0.24587(19) 0.3222(2) 0.4538(2) 0.0129(4) Uani 1 1 d . . . C2 C 0.23298(19) 0.20257(19) 0.4294(2) 0.0130(4) Uani 1 1 d . . . C3 C 0.4407(2) 0.47004(19) 0.0405(2) 0.0148(5) Uani 1 1 d . . . C4 C 0.5455(2) 0.5220(2) 0.0734(2) 0.0144(5) Uani 1 1 d . . . C5 C 0.44357(18) 0.2454(2) 0.2579(2) 0.0137(5) Uani 1 1 d . . . C6 C 0.44263(18) 0.1239(2) 0.2505(2) 0.0129(4) Uani 1 1 d . . . C7 C 0.0861(3) 0.3697(3) 0.0174(3) 0.0313(7) Uani 1 1 d . . . C8 C 0.0597(3) 0.3192(3) 0.1190(3) 0.0303(7) Uani 1 1 d . . . H7A H 0.126(3) 0.311(3) -0.019(3) 0.036 Uiso 1 1 d . . . H7B H 0.014(3) 0.386(3) -0.029(3) 0.036 Uiso 1 1 d . . . H8A H 0.009(3) 0.374(3) 0.151(3) 0.036 Uiso 1 1 d . . . H8B H 0.021(3) 0.242(3) 0.098(3) 0.036 Uiso 1 1 d . . . H7O H 0.184(4) 0.480(3) 0.005(4) 0.038(12) Uiso 1 1 d . . . H8O H 0.169(3) 0.254(3) 0.223(3) 0.029(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01044(6) 0.00912(6) 0.01014(7) 0.00093(3) 0.00115(4) 0.00146(3) O1 0.0256(9) 0.0103(8) 0.0125(9) 0.0018(6) 0.0040(7) 0.0015(7) O2 0.0266(9) 0.0115(8) 0.0118(9) -0.0037(6) 0.0006(7) -0.0008(7) O3 0.0206(9) 0.0276(10) 0.0199(10) 0.0022(8) 0.0098(8) -0.0023(8) O4 0.0203(9) 0.0202(9) 0.0139(10) -0.0036(7) -0.0043(8) 0.0034(7) O5 0.0254(10) 0.0180(9) 0.0339(12) 0.0065(8) 0.0131(9) 0.0121(8) O6 0.0212(10) 0.0205(10) 0.0298(12) -0.0070(8) 0.0095(9) -0.0110(7) O7 0.0229(10) 0.0268(11) 0.0160(11) 0.0034(7) 0.0013(9) -0.0053(7) O8 0.0377(12) 0.0166(10) 0.0292(12) 0.0107(9) -0.0138(10) -0.0093(9) C1 0.0149(11) 0.0123(11) 0.0115(11) -0.0019(9) 0.0016(9) 0.0002(8) C2 0.0162(11) 0.0116(10) 0.0110(11) -0.0001(9) 0.0015(9) -0.0001(8) C3 0.0159(11) 0.0153(11) 0.0133(13) 0.0006(8) 0.0024(10) 0.0021(8) C4 0.0146(11) 0.0156(11) 0.0127(12) 0.0004(9) 0.0013(9) 0.0037(9) C5 0.0145(11) 0.0136(11) 0.0131(11) 0.0030(9) 0.0022(9) 0.0027(8) C6 0.0142(11) 0.0134(11) 0.0115(11) 0.0000(9) 0.0031(9) -0.0006(8) C7 0.0343(16) 0.0308(16) 0.0245(16) 0.0014(12) -0.0088(13) -0.0087(13) C8 0.0308(15) 0.0250(15) 0.0311(17) 0.0069(12) -0.0072(13) -0.0106(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O6 2.2205(19) 4 ? Lu1 O3 2.2435(19) . ? Lu1 O5 2.2435(19) . ? Lu1 O4 2.2437(19) 2_655 ? Lu1 O8 2.324(2) . ? Lu1 O2 2.3707(17) 4 ? Lu1 O1 2.4014(18) . ? Lu1 O7 2.443(2) . ? O1 C1 1.250(3) . ? O2 C2 1.252(3) . ? O2 Lu1 2.3707(17) 4_545 ? O3 C3 1.250(3) . ? O4 C4 1.256(3) . ? O4 Lu1 2.2437(19) 2_655 ? O5 C5 1.246(3) . ? O6 C6 1.244(3) . ? O6 Lu1 2.2205(19) 4_545 ? O7 C7 1.441(4) . ? O7 H7O 0.78(4) . ? O8 C8 1.435(4) . ? O8 H8O 0.77(4) . ? C1 C2 1.469(3) 7_556 ? C1 C2 1.473(3) . ? C2 C1 1.469(3) 7_556 ? C3 C4 1.460(4) 5_665 ? C3 C4 1.462(4) . ? C4 C3 1.460(4) 5_665 ? C5 C6 1.462(3) . ? C5 C5 1.471(5) 2_655 ? C6 C6 1.452(4) 2_655 ? C7 C8 1.489(5) . ? C7 H7A 1.02(4) . ? C7 H7B 1.01(4) . ? C8 H8A 1.04(4) . ? C8 H8B 1.06(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Lu1 O3 142.24(8) 4 . ? O6 Lu1 O5 140.64(7) 4 . ? O3 Lu1 O5 74.61(8) . . ? O6 Lu1 O4 100.68(8) 4 2_655 ? O3 Lu1 O4 97.73(8) . 2_655 ? O5 Lu1 O4 81.29(8) . 2_655 ? O6 Lu1 O8 84.14(8) 4 . ? O3 Lu1 O8 97.90(8) . . ? O5 Lu1 O8 74.97(8) . . ? O4 Lu1 O8 146.84(7) 2_655 . ? O6 Lu1 O2 76.63(7) 4 4 ? O3 Lu1 O2 78.12(7) . 4 ? O5 Lu1 O2 138.60(7) . 4 ? O4 Lu1 O2 72.14(6) 2_655 4 ? O8 Lu1 O2 139.95(7) . 4 ? O6 Lu1 O1 70.53(7) 4 . ? O3 Lu1 O1 146.72(7) . . ? O5 Lu1 O1 72.21(7) . . ? O4 Lu1 O1 74.87(7) 2_655 . ? O8 Lu1 O1 76.01(7) . . ? O2 Lu1 O1 127.33(6) 4 . ? O6 Lu1 O7 74.87(8) 4 . ? O3 Lu1 O7 71.97(8) . . ? O5 Lu1 O7 122.77(8) . . ? O4 Lu1 O7 147.63(7) 2_655 . ? O8 Lu1 O7 65.44(7) . . ? O2 Lu1 O7 75.68(6) 4 . ? O1 Lu1 O7 130.01(7) . . ? C1 O1 Lu1 135.20(16) . . ? C2 O2 Lu1 141.23(16) . 4_545 ? C3 O3 Lu1 145.55(18) . . ? C4 O4 Lu1 132.40(16) . 2_655 ? C5 O5 Lu1 149.92(19) . . ? C6 O6 Lu1 155.31(18) . 4_545 ? C7 O7 Lu1 118.36(17) . . ? C7 O7 H7O 108(3) . . ? Lu1 O7 H7O 107(3) . . ? C8 O8 Lu1 119.56(17) . . ? C8 O8 H8O 116(3) . . ? Lu1 O8 H8O 124(3) . . ? O1 C1 C2 133.3(2) . 7_556 ? O1 C1 C2 136.5(2) . . ? C2 C1 C2 90.19(19) 7_556 . ? O2 C2 C1 135.0(2) . 7_556 ? O2 C2 C1 135.1(2) . . ? C1 C2 C1 89.81(19) 7_556 . ? O3 C3 C4 134.3(3) . 5_665 ? O3 C3 C4 135.6(3) . . ? C4 C3 C4 90.1(2) 5_665 . ? O4 C4 C3 134.4(3) . 5_665 ? O4 C4 C3 135.7(3) . . ? C3 C4 C3 89.9(2) 5_665 . ? O5 C5 C6 134.0(2) . . ? O5 C5 C5 136.41(15) . 2_655 ? C6 C5 C5 89.42(13) . 2_655 ? O6 C6 C6 133.05(15) . 2_655 ? O6 C6 C5 136.7(2) . . ? C6 C6 C5 90.14(13) 2_655 . ? O7 C7 C8 106.6(3) . . ? O7 C7 H7A 113(2) . . ? C8 C7 H7A 107(2) . . ? O7 C7 H7B 114(2) . . ? C8 C7 H7B 105(2) . . ? H7A C7 H7B 110(3) . . ? O8 C8 C7 105.7(3) . . ? O8 C8 H8A 111(2) . . ? C7 C8 H8A 108(2) . . ? O8 C8 H8B 114(2) . . ? C7 C8 H8B 108(2) . . ? H8A C8 H8B 111(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.668 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.134 #===End