Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Robson, Richard' 'Abrahams, Brendan F.' 'Coleiro, Joseph' 'Ha, Karen' 'Hoskins, Bernard F.' 'Orchard, Simon D.' _publ_contact_author_name 'Prof Richard Robson' _publ_contact_author_address ; School of Chemistry University of Melbourne AUSTRALIA ; _publ_contact_author_email 'R.ROBSON@CHEMISTRY.UNIMELB.EDU.AU' _publ_section_title ; Dihydroxybenzoquinone and Choranilic Acid Derivatives of Rare Earth Metals ; data_la2dhbq3abs97 _database_code_CSD 175597 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(2,5-dihyroxy-1,4-bezoquinonate)dilanthanum(III) octadecahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 La2 O36' _chemical_formula_weight 1124.43 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 'rhombohedral - hexagonal axes' _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.460(4) _cell_length_b 14.460(4) _cell_length_c 18.165(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3289.3(16) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.2 _cell_measurement_theta_max 16.3 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 2.026 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7058 _exptl_absorpt_correction_T_max 0.9562 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 160 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2713 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.1475 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 29.98 _reflns_number_total 2136 _reflns_number_gt 1460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0315P)^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 2136 _refine_ls_number_parameters 115 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.986 _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 La La 0.0000 0.0000 0.24198(4) 0.01709(17) Uani 1 3 d S . . O1 O -0.1295(4) -0.1207(4) 0.3384(3) 0.0288(11) Uani 1 1 d . . . O2 O -0.1813(4) -0.0094(4) 0.2516(3) 0.0256(10) Uani 1 1 d . . . C1 C -0.2281(5) -0.1502(5) 0.3377(3) 0.0206(13) Uani 1 1 d . . . C2 C -0.2565(5) -0.0810(5) 0.2887(3) 0.0210(13) Uani 1 1 d . . . C3 C -0.3617(5) -0.1018(6) 0.2874(4) 0.0239(14) Uani 1 1 d . . . H3 H -0.3797 -0.0604 0.2582 0.10(4) Uiso 1 1 calc R . . O3 O -0.1336(5) -0.1337(5) 0.1514(4) 0.0438(15) Uani 1 1 d D . . HO31 H -0.131(8) -0.177(6) 0.125(4) 0.05(2) Uiso 1 1 d D . . HO32 H -0.174(6) -0.125(8) 0.124(4) 0.05(2) Uiso 1 1 d D . . O4 O -0.1399(5) -0.2957(5) 0.0683(3) 0.0426(14) Uani 1 1 d D . . HO41 H -0.145(8) -0.281(8) 0.026(2) 0.06(2) Uiso 1 1 d D . . HO42 H -0.169(7) -0.357(3) 0.082(5) 0.06(2) Uiso 1 1 d D . . O5 O -0.4773(5) -0.2077(5) 0.1253(3) 0.0435(15) Uani 1 1 d D . . HO51 H -0.497(6) -0.227(6) 0.083(2) 0.030(16) Uiso 1 1 d D . . HO52 H -0.516(5) -0.191(6) 0.147(4) 0.030(16) Uiso 1 1 d D . . O6 O -0.2716(5) -0.0850(5) 0.0766(4) 0.0469(15) Uani 1 1 d D . . HO61 H -0.236(6) -0.021(3) 0.076(5) 0.05(2) Uiso 1 1 d D . . HO62 H -0.327(4) -0.117(6) 0.099(4) 0.05(2) Uiso 1 1 d 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 La 0.01512(19) 0.01512(19) 0.0210(3) 0.000 0.000 0.00756(10) O1 0.022(2) 0.036(3) 0.031(3) 0.006(2) -0.002(2) 0.016(2) O2 0.022(2) 0.021(2) 0.032(3) 0.005(2) -0.002(2) 0.009(2) C1 0.020(3) 0.022(3) 0.022(3) -0.001(3) -0.001(3) 0.012(3) C2 0.024(3) 0.020(3) 0.018(3) -0.003(3) -0.001(3) 0.010(3) C3 0.015(3) 0.027(4) 0.032(4) 0.005(3) -0.003(3) 0.013(3) O3 0.042(4) 0.042(4) 0.056(4) -0.026(3) -0.028(3) 0.027(3) O4 0.047(4) 0.030(3) 0.046(4) -0.002(3) -0.006(3) 0.016(3) O5 0.056(4) 0.052(4) 0.028(3) -0.012(3) -0.007(3) 0.031(3) O6 0.039(4) 0.046(4) 0.054(4) 0.000(3) 0.002(3) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La La 0.0000(13) 3 ? La O1 2.521(5) 2 ? La O1 2.521(5) . ? La O1 2.521(5) 3 ? La O3 2.538(6) . ? La O3 2.538(6) 3 ? La O3 2.539(6) 2 ? La O2 2.562(5) 2 ? La O2 2.562(5) . ? La O2 2.562(5) 3 ? O1 C1 1.267(8) . ? O1 La 2.521(5) 3 ? O2 C2 1.258(8) . ? O2 La 2.562(5) 3 ? C1 C3 1.372(9) 16_445 ? C1 C2 1.542(9) . ? C2 C3 1.394(9) . ? C3 C1 1.372(9) 16_445 ? O3 La 2.538(6) 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 O1 La O1 77.01(17) 2 . ? O1 La O1 77.01(17) 2 3 ? O1 La O1 77.01(17) . 3 ? O1 La O3 134.02(18) 2 . ? O1 La O3 84.5(2) . . ? O1 La O3 138.82(18) 3 . ? O1 La O3 138.82(19) 2 3 ? O1 La O3 134.02(18) . 3 ? O1 La O3 84.5(2) 3 3 ? O3 La O3 82.5(2) . 3 ? O1 La O3 84.5(2) 2 2 ? O1 La O3 138.82(18) . 2 ? O1 La O3 134.01(18) 3 2 ? O3 La O3 82.5(2) . 2 ? O3 La O3 82.5(2) 3 2 ? O1 La O2 61.96(14) 2 2 ? O1 La O2 70.28(15) . 2 ? O1 La O2 131.76(16) 3 2 ? O3 La O2 72.22(17) . 2 ? O3 La O2 143.41(19) 3 2 ? O3 La O2 68.55(18) 2 2 ? O1 La O2 131.76(16) 2 . ? O1 La O2 61.96(14) . . ? O1 La O2 70.28(15) 3 . ? O3 La O2 68.55(18) . . ? O3 La O2 72.23(17) 3 . ? O3 La O2 143.41(19) 2 . ? O2 La O2 119.54(2) 2 . ? O1 La O2 70.28(15) 2 3 ? O1 La O2 131.76(16) . 3 ? O1 La O2 61.96(14) 3 3 ? O3 La O2 143.41(19) . 3 ? O3 La O2 68.55(18) 3 3 ? O3 La O2 72.22(17) 2 3 ? O2 La O2 119.55(3) 2 3 ? O2 La O2 119.54(3) . 3 ? C1 O1 La 123.1(4) . 3 ? C1 O1 La 123.1(4) . . ? C2 O2 La 121.4(4) . 3 ? C2 O2 La 121.4(4) . . ? O1 C1 C3 125.2(6) . 16_445 ? O1 C1 C2 114.1(6) . . ? C3 C1 C2 120.6(6) 16_445 . ? O2 C2 C3 124.7(6) . . ? O2 C2 C1 116.2(6) . . ? C3 C2 C1 119.1(6) . . ? C1 C3 C2 120.3(6) 16_445 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.204 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.217 #===END data_gddhbqabs97 _database_code_CSD 175598 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(2,5-dihyroxy-1,4-bezoquinonate)digadolinium(III) octadecahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Gd2 O36' _chemical_formula_weight 1161.11 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' 'Gd' 'Gd' -0.1653 3.9035 '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' _symmetry_cell_setting 'rhombohedral - hexagonal axes' _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.202(2) _cell_length_b 14.202(2) _cell_length_c 18.106(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3162.7(7) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.6 _cell_measurement_theta_max 13.5 _exptl_crystal_description 'circular plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1734 _exptl_absorpt_coefficient_mu 3.226 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6786 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1641 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1238 _reflns_number_gt 1024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0280P)^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 1238 _refine_ls_number_parameters 115 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.078 _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 Gd1 Gd 0.6667 0.3333 0.07822(2) 0.01703(13) Uani 1 3 d S . . O1 O 0.8378(2) 0.3254(2) 0.08387(16) 0.0237(7) Uani 1 1 d . . . O2 O 0.6716(2) 0.2129(3) 0.16983(17) 0.0245(7) Uani 1 1 d . . . O3 O 0.5403(3) 0.3353(3) -0.0102(2) 0.0385(9) Uani 1 1 d D . . HO31 H 0.500(3) 0.279(2) -0.029(2) 0.025(10) Uiso 1 1 d D . . HO32 H 0.538(4) 0.385(3) -0.029(2) 0.025(10) Uiso 1 1 d D . . C2 C 0.7430(4) 0.1843(3) 0.1705(2) 0.0203(9) Uani 1 1 d . . . C3 C 0.7382(4) 0.1005(4) 0.2127(3) 0.0250(10) Uani 1 1 d . . . H31 H 0.6771 0.0575 0.2413 0.012(10) Uiso 1 1 calc R . . O4 O 0.7528(3) 0.6011(3) -0.0894(3) 0.0447(10) Uani 1 1 d D . . HO41 H 0.6886(19) 0.570(5) -0.091(4) 0.068(16) Uiso 1 1 d D . . HO42 H 0.782(5) 0.659(3) -0.070(4) 0.068(16) Uiso 1 1 d D . . C1 C 0.8418(4) 0.2527(3) 0.1213(2) 0.0200(9) Uani 1 1 d . . . O5 O 0.8107(4) 0.9397(3) 0.0418(2) 0.0435(10) Uani 1 1 d D . . HO51 H 0.839(4) 0.932(5) 0.077(2) 0.048(13) Uiso 1 1 d D . . HO52 H 0.849(4) 0.996(3) 0.022(3) 0.048(13) Uiso 1 1 d D . . O6 O 0.0401(3) 0.5281(4) 0.0980(2) 0.0437(9) Uani 1 1 d D . . HO61 H 0.054(7) 0.517(7) 0.139(2) 0.10(2) Uiso 1 1 d D . . HO62 H -0.013(4) 0.490(6) 0.075(4) 0.10(2) Uiso 1 1 d 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 0.01395(14) 0.01395(14) 0.0232(2) 0.000 0.000 0.00697(7) O1 0.0211(16) 0.0207(17) 0.0339(18) 0.0061(14) 0.0007(13) 0.0139(14) O2 0.0197(16) 0.0270(18) 0.0332(17) 0.0072(14) 0.0039(13) 0.0164(15) O3 0.039(2) 0.023(2) 0.049(2) -0.0015(17) -0.0220(18) 0.0124(18) C2 0.018(2) 0.019(2) 0.023(2) -0.0014(18) -0.0008(18) 0.009(2) C3 0.019(2) 0.023(2) 0.035(3) 0.004(2) 0.005(2) 0.011(2) O4 0.037(2) 0.040(2) 0.056(3) 0.008(2) 0.004(2) 0.018(2) C1 0.019(2) 0.015(2) 0.024(2) -0.0009(17) -0.0022(18) 0.0065(19) O5 0.047(3) 0.045(2) 0.037(2) 0.005(2) -0.0079(19) 0.022(2) O6 0.030(2) 0.041(2) 0.052(3) 0.003(2) 0.003(2) 0.0120(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 Gd1 O2 2.409(3) . ? Gd1 O2 2.409(3) 2_655 ? Gd1 O2 2.409(3) 3_665 ? Gd1 O3 2.415(4) . ? Gd1 O3 2.415(4) 3_665 ? Gd1 O3 2.415(4) 2_655 ? Gd1 O1 2.490(3) . ? Gd1 O1 2.490(3) 2_655 ? Gd1 O1 2.490(3) 3_665 ? O1 C1 1.261(5) . ? O2 C2 1.267(5) . ? O3 HO31 0.79(2) . ? O3 HO32 0.79(2) . ? C2 C3 1.386(6) . ? C2 C1 1.531(6) . ? C3 C1 1.393(6) 13_655 ? C3 H31 0.9300 . ? O4 HO41 0.79(2) . ? O4 HO42 0.80(2) . ? C1 C3 1.393(6) 13_655 ? O5 HO51 0.79(2) . ? O5 HO52 0.79(2) . ? O6 HO61 0.80(2) . ? O6 HO62 0.79(2) . ? 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 O2 Gd1 O2 77.81(11) . 2_655 ? O2 Gd1 O2 77.81(11) . 3_665 ? O2 Gd1 O2 77.81(11) 2_655 3_665 ? O2 Gd1 O3 138.61(12) . . ? O2 Gd1 O3 134.80(11) 2_655 . ? O2 Gd1 O3 85.05(13) 3_665 . ? O2 Gd1 O3 134.80(11) . 3_665 ? O2 Gd1 O3 85.05(13) 2_655 3_665 ? O2 Gd1 O3 138.61(12) 3_665 3_665 ? O3 Gd1 O3 80.88(15) . 3_665 ? O2 Gd1 O3 85.05(13) . 2_655 ? O2 Gd1 O3 138.61(12) 2_655 2_655 ? O2 Gd1 O3 134.80(11) 3_665 2_655 ? O3 Gd1 O3 80.88(15) . 2_655 ? O3 Gd1 O3 80.88(15) 3_665 2_655 ? O2 Gd1 O1 64.15(10) . . ? O2 Gd1 O1 69.93(10) 2_655 . ? O2 Gd1 O1 133.97(10) 3_665 . ? O3 Gd1 O1 140.84(13) . . ? O3 Gd1 O1 70.71(11) 3_665 . ? O3 Gd1 O1 68.69(12) 2_655 . ? O2 Gd1 O1 133.97(10) . 2_655 ? O2 Gd1 O1 64.15(10) 2_655 2_655 ? O2 Gd1 O1 69.93(10) 3_665 2_655 ? O3 Gd1 O1 70.71(11) . 2_655 ? O3 Gd1 O1 68.69(12) 3_665 2_655 ? O3 Gd1 O1 140.84(13) 2_655 2_655 ? O1 Gd1 O1 119.834(10) . 2_655 ? O2 Gd1 O1 69.93(10) . 3_665 ? O2 Gd1 O1 133.97(10) 2_655 3_665 ? O2 Gd1 O1 64.15(10) 3_665 3_665 ? O3 Gd1 O1 68.69(12) . 3_665 ? O3 Gd1 O1 140.84(13) 3_665 3_665 ? O3 Gd1 O1 70.71(11) 2_655 3_665 ? O1 Gd1 O1 119.831(10) . 3_665 ? O1 Gd1 O1 119.832(10) 2_655 3_665 ? C1 O1 Gd1 120.3(3) . . ? C2 O2 Gd1 123.2(3) . . ? Gd1 O3 HO31 116(4) . . ? Gd1 O3 HO32 131(4) . . ? HO31 O3 HO32 113(5) . . ? O2 C2 C3 125.2(4) . . ? O2 C2 C1 114.6(4) . . ? C3 C2 C1 120.1(4) . . ? C2 C3 C1 120.0(4) . 13_655 ? C2 C3 H31 120.0 . . ? C1 C3 H31 120.0 13_655 . ? HO41 O4 HO42 116(7) . . ? O1 C1 C3 124.6(4) . 13_655 ? O1 C1 C2 115.5(4) . . ? C3 C1 C2 119.9(4) 13_655 . ? HO51 O5 HO52 111(6) . . ? HO61 O6 HO62 126(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.299 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.107 #===END data_ybdhbqabs97 _database_code_CSD 175599 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(2,5-dihyroxy-1,4-bezoquinonate)diytterbium(III) octadecahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 O36 Yb2' _chemical_formula_weight 1192.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'rhombohedral - hexagonal axes' _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.062(1) _cell_length_b 14.062(1) _cell_length_c 18.027(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3087.1(4) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.4 _cell_measurement_theta_max 28.3 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1770 _exptl_absorpt_coefficient_mu 9.193 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4817 _exptl_absorpt_correction_T_max 0.8941 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 1714 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.38 _diffrn_reflns_theta_max 74.67 _reflns_number_total 1305 _reflns_number_gt 1095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0504P)^2^+6.9745P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 1305 _refine_ls_number_parameters 115 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.092 _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 Yb Yb 0.0000 0.0000 0.24655(2) 0.01654(16) Uani 1 3 d S . . O1 O 0.1196(3) 0.1229(3) 0.33562(19) 0.0236(7) Uani 1 1 d . . . O2 O 0.0062(3) 0.1772(3) 0.25046(18) 0.0218(7) Uani 1 1 d . . . C1 C 0.1491(4) 0.2246(4) 0.3366(2) 0.0193(9) Uani 1 1 d . . . C2 C 0.0803(4) 0.2557(4) 0.2881(2) 0.0204(10) Uani 1 1 d . . . C3 C 0.1001(4) 0.3630(4) 0.2878(3) 0.0247(10) Uani 1 1 d . . . H1 H 0.0566 0.3814 0.2592 0.035(17) Uiso 1 1 calc R . . O3 O 0.1251(4) 0.1232(4) 0.1603(2) 0.0335(9) Uani 1 1 d D . . HO31 H 0.175(4) 0.124(5) 0.139(3) 0.023(11) Uiso 1 1 d D . . HO32 H 0.120(5) 0.164(4) 0.133(3) 0.023(11) Uiso 1 1 d D . . O4 O 0.2913(4) 0.1390(4) 0.0700(3) 0.0410(10) Uani 1 1 d D . . HO41 H 0.343(6) 0.191(6) 0.087(6) 0.10(3) Uiso 1 1 d D . . HO42 H 0.272(9) 0.142(10) 0.029(3) 0.10(3) Uiso 1 1 d D . . O5 O 0.2048(4) 0.4787(4) 0.1250(2) 0.0409(10) Uani 1 1 d D . . HO51 H 0.237(8) 0.503(8) 0.087(3) 0.10(3) Uiso 1 1 d D . . HO52 H 0.171(7) 0.503(8) 0.144(5) 0.10(3) Uiso 1 1 d D . . O6 O 0.0863(4) 0.2660(4) 0.0779(3) 0.0428(11) Uani 1 1 d . . . HO61 H 0.029(8) 0.244(8) 0.075(5) 0.07(2) Uiso 1 1 d . . . HO62 H 0.119(7) 0.330(7) 0.095(5) 0.07(2) 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 Yb 0.01481(19) 0.01481(19) 0.0200(2) 0.000 0.000 0.00740(9) O1 0.0235(19) 0.0151(17) 0.0304(16) 0.0007(13) -0.0060(14) 0.0083(16) O2 0.0169(17) 0.0138(17) 0.0294(16) -0.0024(13) -0.0053(13) 0.0038(14) C1 0.020(2) 0.019(2) 0.0212(19) 0.0024(17) 0.0023(17) 0.011(2) C2 0.016(2) 0.020(3) 0.0221(19) 0.0003(17) 0.0033(17) 0.007(2) C3 0.026(3) 0.019(2) 0.032(2) 0.0018(19) -0.006(2) 0.013(2) O3 0.036(2) 0.034(2) 0.0371(19) 0.0184(17) 0.0176(17) 0.022(2) O4 0.031(2) 0.039(3) 0.046(2) 0.003(2) 0.006(2) 0.012(2) O5 0.042(3) 0.043(3) 0.037(2) 0.0079(19) 0.011(2) 0.022(2) O6 0.038(3) 0.039(3) 0.053(3) 0.007(2) 0.000(2) 0.021(3) _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 Yb O3 2.338(4) . ? Yb O3 2.338(4) 2 ? Yb O3 2.338(4) 3 ? Yb O1 2.342(3) 2 ? Yb O1 2.342(3) 3 ? Yb O1 2.342(3) . ? Yb O2 2.450(4) . ? Yb O2 2.450(4) 2 ? Yb O2 2.450(4) 3 ? O1 C1 1.274(6) . ? O2 C2 1.271(6) . ? C1 C3 1.378(7) 16 ? C1 C2 1.523(7) . ? C2 C3 1.390(7) . ? C3 C1 1.378(7) 16 ? C3 H1 0.9300 . ? O3 HO31 0.79(3) . ? O3 HO32 0.79(3) . ? O4 HO41 0.79(3) . ? O4 HO42 0.79(3) . ? O5 HO51 0.79(3) . ? O5 HO52 0.79(3) . ? O6 HO61 0.70(9) . ? O6 HO62 0.84(8) . ? 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 O3 Yb O3 80.58(17) . 2 ? O3 Yb O3 80.58(17) . 3 ? O3 Yb O3 80.58(17) 2 3 ? O3 Yb O1 138.14(14) . 2 ? O3 Yb O1 84.99(14) 2 2 ? O3 Yb O1 135.27(14) 3 2 ? O3 Yb O1 135.27(14) . 3 ? O3 Yb O1 138.14(14) 2 3 ? O3 Yb O1 84.99(14) 3 3 ? O1 Yb O1 78.18(13) 2 3 ? O3 Yb O1 84.99(14) . . ? O3 Yb O1 135.27(14) 2 . ? O3 Yb O1 138.14(14) 3 . ? O1 Yb O1 78.18(13) 2 . ? O1 Yb O1 78.18(13) 3 . ? O3 Yb O2 68.57(13) . . ? O3 Yb O2 69.96(13) 2 . ? O3 Yb O2 139.94(14) 3 . ? O1 Yb O2 69.58(12) 2 . ? O1 Yb O2 134.99(12) 3 . ? O1 Yb O2 65.34(11) . . ? O3 Yb O2 139.94(14) . 2 ? O3 Yb O2 68.57(13) 2 2 ? O3 Yb O2 69.96(13) 3 2 ? O1 Yb O2 65.34(11) 2 2 ? O1 Yb O2 69.58(12) 3 2 ? O1 Yb O2 134.99(12) . 2 ? O2 Yb O2 119.919(8) . 2 ? O3 Yb O2 69.96(13) . 3 ? O3 Yb O2 139.94(14) 2 3 ? O3 Yb O2 68.57(13) 3 3 ? O1 Yb O2 134.99(12) 2 3 ? O1 Yb O2 65.34(11) 3 3 ? O1 Yb O2 69.58(12) . 3 ? O2 Yb O2 119.917(8) . 3 ? O2 Yb O2 119.918(8) 2 3 ? C1 O1 Yb 123.3(3) . . ? C2 O2 Yb 119.7(3) . . ? O1 C1 C3 125.5(4) . 16 ? O1 C1 C2 114.7(4) . . ? C3 C1 C2 119.8(4) 16 . ? O2 C2 C3 125.0(5) . . ? O2 C2 C1 114.8(4) . . ? C3 C2 C1 120.2(4) . . ? C1 C3 C2 119.9(5) 16 . ? C1 C3 H1 120.0 16 . ? C2 C3 H1 120.0 . . ? Yb O3 HO31 132(5) . . ? Yb O3 HO32 130(5) . . ? HO31 O3 HO32 95(6) . . ? HO41 O4 HO42 119(10) . . ? HO51 O5 HO52 121(10) . . ? HO61 O6 HO62 113(10) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 74.67 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 1.117 _refine_diff_density_min -1.981 _refine_diff_density_rms 0.127 #===END data_ludhbqabs97 _database_code_CSD 175600 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(2,5-dihyroxy-1,4-bezoquinonate)dilutetium(III) octadecahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Lu2 O36' _chemical_formula_weight 1196.55 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 'rhombohedral - hexagonal axes' _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.026(1) _cell_length_b 14.026(1) _cell_length_c 18.044(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3074.2(4) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.3 _cell_measurement_theta_max 17.1 _exptl_crystal_description 'cylinder' _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min o.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 4.900 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3707 _exptl_absorpt_correction_T_max 0.4245 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2041 _diffrn_reflns_av_R_equivalents 0.0126 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1572 _reflns_number_gt 1458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0117P)^2^+7.4798P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 1572 _refine_ls_number_parameters 115 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0150 _refine_ls_wR_factor_ref 0.0364 _refine_ls_wR_factor_gt 0.0353 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Lu Lu 0.0000 0.0000 0.246461(7) 0.01710(5) Uani 1 3 d S . . O1 O -0.12237(12) -0.11936(13) 0.33483(8) 0.0248(3) Uani 1 1 d . . . O2 O -0.17758(12) -0.00675(12) 0.24960(8) 0.0240(3) Uani 1 1 d . . . C1 C -0.22424(18) -0.14898(18) 0.33651(11) 0.0216(4) Uani 1 1 d . . . C2 C -0.25530(17) -0.07992(17) 0.28757(11) 0.0211(4) Uani 1 1 d . . . C3 C -0.36337(18) -0.09960(19) 0.28770(12) 0.0254(4) Uani 1 1 d . . . H3 H -0.3820 -0.0559 0.2594 0.029(7) Uiso 1 1 calc R . . O3 O -0.12267(16) -0.12548(15) 0.16047(10) 0.0354(4) Uani 1 1 d D . . H31 H -0.124(3) -0.182(2) 0.1400(17) 0.054(7) Uiso 1 1 d D . . H32 H -0.171(2) -0.117(3) 0.1356(17) 0.054(7) Uiso 1 1 d D . . O4 O -0.13837(19) -0.29148(17) 0.07036(12) 0.0468(5) Uani 1 1 d D . . H41 H -0.194(3) -0.359(3) 0.085(3) 0.128(15) Uiso 1 1 d D . . H42 H -0.148(5) -0.276(5) 0.0226(16) 0.128(15) Uiso 1 1 d D . . O5 O -0.47863(19) -0.20437(19) 0.12444(11) 0.0455(5) Uani 1 1 d D . . H51 H -0.516(3) -0.173(3) 0.144(2) 0.083(10) Uiso 1 1 d D . . H52 H -0.505(3) -0.242(3) 0.0828(16) 0.083(10) Uiso 1 1 d D . . O6 O -0.26595(19) -0.08642(19) 0.07778(13) 0.0474(5) Uani 1 1 d D . . H61 H -0.333(2) -0.117(3) 0.100(2) 0.083(10) Uiso 1 1 d D . . H62 H -0.235(3) -0.013(2) 0.077(2) 0.083(10) Uiso 1 1 d 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 Lu 0.01522(6) 0.01522(6) 0.02084(8) 0.000 0.000 0.00761(3) O1 0.0159(7) 0.0267(8) 0.0315(8) 0.0057(6) 0.0015(6) 0.0104(7) O2 0.0178(7) 0.0212(8) 0.0314(8) 0.0050(6) 0.0032(6) 0.0086(6) C1 0.0207(10) 0.0214(10) 0.0234(9) -0.0018(8) -0.0009(8) 0.0111(9) C2 0.0194(10) 0.0187(10) 0.0236(9) -0.0003(8) 0.0010(8) 0.0083(8) C3 0.0214(11) 0.0247(11) 0.0320(11) 0.0053(9) -0.0008(8) 0.0130(9) O3 0.0384(10) 0.0353(10) 0.0404(10) -0.0158(8) -0.0176(8) 0.0243(9) O4 0.0446(12) 0.0346(11) 0.0533(12) -0.0080(9) -0.0048(10) 0.0138(10) O5 0.0521(13) 0.0484(13) 0.0391(10) -0.0119(9) -0.0083(9) 0.0273(11) O6 0.0445(12) 0.0460(12) 0.0528(12) -0.0028(10) -0.0087(10) 0.0236(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 Lu O1 2.3275(15) 3 ? Lu O1 2.3276(15) . ? Lu O1 2.3277(15) 2 ? Lu O3 2.3318(17) 3 ? Lu O3 2.3318(17) . ? Lu O3 2.3318(17) 2 ? Lu O2 2.4454(16) . ? Lu O2 2.4454(16) 3 ? Lu O2 2.4454(16) 2 ? O1 C1 1.273(3) . ? O2 C2 1.262(3) . ? C1 C3 1.382(3) 16_445 ? C1 C2 1.527(3) . ? C2 C3 1.398(3) . ? C3 C1 1.382(3) 16_445 ? C3 H3 0.9300 . ? O3 H31 0.86(2) . ? O3 H32 0.86(2) . ? O4 H41 0.91(2) . ? O4 H42 0.91(2) . ? O5 H51 0.90(2) . ? O5 H52 0.88(2) . ? O6 H61 0.92(2) . ? O6 H62 0.89(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Lu O1 78.23(6) 3 . ? O1 Lu O1 78.23(6) 3 2 ? O1 Lu O1 78.23(6) . 2 ? O1 Lu O3 84.98(6) 3 3 ? O1 Lu O3 135.08(6) . 3 ? O1 Lu O3 138.32(6) 2 3 ? O1 Lu O3 138.33(6) 3 . ? O1 Lu O3 84.98(6) . . ? O1 Lu O3 135.08(6) 2 . ? O3 Lu O3 80.55(8) 3 . ? O1 Lu O3 135.08(6) 3 2 ? O1 Lu O3 138.32(6) . 2 ? O1 Lu O3 84.98(6) 2 2 ? O3 Lu O3 80.55(8) 3 2 ? O3 Lu O3 80.55(8) . 2 ? O1 Lu O2 69.84(5) 3 . ? O1 Lu O2 65.53(5) . . ? O1 Lu O2 135.34(5) 2 . ? O3 Lu O2 69.59(6) 3 . ? O3 Lu O2 68.49(6) . . ? O3 Lu O2 139.61(6) 2 . ? O1 Lu O2 65.53(5) 3 3 ? O1 Lu O2 135.34(5) . 3 ? O1 Lu O2 69.83(5) 2 3 ? O3 Lu O2 68.49(6) 3 3 ? O3 Lu O2 139.61(6) . 3 ? O3 Lu O2 69.59(6) 2 3 ? O2 Lu O2 119.949(3) . 3 ? O1 Lu O2 135.34(5) 3 2 ? O1 Lu O2 69.83(5) . 2 ? O1 Lu O2 65.53(5) 2 2 ? O3 Lu O2 139.61(6) 3 2 ? O3 Lu O2 69.59(6) . 2 ? O3 Lu O2 68.49(6) 2 2 ? O2 Lu O2 119.947(3) . 2 ? O2 Lu O2 119.944(3) 3 2 ? C1 O1 Lu 123.68(13) . . ? C2 O2 Lu 119.54(14) . . ? O1 C1 C3 125.5(2) . 16_445 ? O1 C1 C2 114.14(18) . . ? C3 C1 C2 120.37(19) 16_445 . ? O2 C2 C3 124.9(2) . . ? O2 C2 C1 115.19(18) . . ? C3 C2 C1 119.93(19) . . ? C1 C3 C2 119.7(2) 16_445 . ? C1 C3 H3 120.2 16_445 . ? C2 C3 H3 120.2 . . ? Lu O3 H31 130(2) . . ? Lu O3 H32 125(2) . . ? H31 O3 H32 104(3) . . ? H41 O4 H42 112(5) . . ? H51 O5 H52 117(4) . . ? H61 O6 H62 110(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.479 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.074 #===END data_y2dhbq3abs97 _database_code_CSD 175601 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(2,5-dihyroxy-1,4-bezoquinonate)diyttrium(III) octadecahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 O36 Y2' _chemical_formula_weight 1024.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'rhombohedral - hexagonal axes' _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.113(3) _cell_length_b 14.113(3) _cell_length_c 18.091(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3120.6(12) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.1 _cell_measurement_theta_max 29.3 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 4.730 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8588 _exptl_absorpt_correction_T_max 0.9585 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 160 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1720 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.1272 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 74.95 _reflns_number_total 1300 _reflns_number_gt 813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0280P)^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 1300 _refine_ls_number_parameters 115 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1215 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.055 _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 Y Y 0.0000 0.0000 0.24591(8) 0.0205(3) Uani 1 3 d S . . O1 O -0.1238(4) -0.1202(4) 0.3358(3) 0.0256(11) Uani 1 1 d . . . O2 O -0.1775(4) -0.0077(4) 0.2504(3) 0.0234(10) Uani 1 1 d . . . C1 C -0.2242(6) -0.1489(6) 0.3367(4) 0.0220(15) Uani 1 1 d . . . C2 C -0.2554(6) -0.0803(6) 0.2879(4) 0.0208(15) Uani 1 1 d . . . C3 C -0.3629(5) -0.1009(6) 0.2879(4) 0.0234(16) Uani 1 1 d . . . H3 H -0.3812 -0.0578 0.2591 0.024(19) Uiso 1 1 calc R . . O3 O -0.1243(5) -0.1267(5) 0.1588(3) 0.0381(14) Uani 1 1 d D . . H31 H -0.140(8) -0.193(4) 0.141(5) 0.07(2) Uiso 1 1 d D . . H32 H -0.166(6) -0.102(7) 0.137(5) 0.07(2) Uiso 1 1 d D . . O4 O -0.1393(5) -0.2927(5) 0.0695(4) 0.0470(16) Uani 1 1 d D . . H41 H -0.143(8) -0.284(8) 0.020(2) 0.08(3) Uiso 1 1 d D . . H42 H -0.189(6) -0.359(5) 0.087(5) 0.08(3) Uiso 1 1 d D . . O5 O -0.4779(5) -0.2033(5) 0.1245(3) 0.0435(15) Uani 1 1 d D . . H51 H -0.513(10) -0.225(12) 0.081(4) 0.17(5) Uiso 1 1 d D . . H52 H -0.498(11) -0.264(8) 0.151(7) 0.17(5) Uiso 1 1 d D . . O6 O -0.2670(5) -0.0862(5) 0.0777(4) 0.0467(15) Uani 1 1 d D . . H61 H -0.333(5) -0.124(7) 0.100(5) 0.08(3) Uiso 1 1 d D . . H62 H -0.230(7) -0.014(3) 0.069(5) 0.08(3) Uiso 1 1 d 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 Y 0.0181(3) 0.0181(3) 0.0254(6) 0.000 0.000 0.00903(17) O1 0.016(2) 0.028(3) 0.032(3) 0.007(2) 0.000(2) 0.010(2) O2 0.017(2) 0.018(3) 0.032(3) 0.006(2) 0.002(2) 0.007(2) C1 0.021(4) 0.024(4) 0.021(3) -0.002(3) 0.000(3) 0.012(3) C2 0.024(4) 0.022(4) 0.020(3) 0.000(3) -0.002(3) 0.014(3) C3 0.025(4) 0.020(4) 0.027(4) 0.007(3) 0.000(3) 0.013(3) O3 0.042(4) 0.036(3) 0.047(3) -0.018(3) -0.018(3) 0.027(3) O4 0.047(4) 0.030(3) 0.056(4) -0.008(3) -0.009(3) 0.013(3) O5 0.047(4) 0.045(4) 0.034(3) -0.004(3) -0.010(3) 0.020(3) O6 0.043(4) 0.040(4) 0.053(4) 0.006(3) 0.001(3) 0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y O1 2.369(5) . ? Y O1 2.369(5) 3 ? Y O1 2.369(5) 2 ? Y O3 2.371(6) 3 ? Y O3 2.371(6) 2 ? Y O3 2.371(6) . ? Y O2 2.454(4) . ? Y O2 2.454(4) 3 ? Y O2 2.454(4) 2 ? O1 C1 1.264(8) . ? O1 Y 2.369(5) 3 ? O2 C2 1.262(8) . ? O2 Y 2.454(4) 3 ? C1 C3 1.381(9) 16_445 ? C1 C2 1.528(9) . ? C2 C3 1.395(9) . ? C3 C1 1.381(9) 16_445 ? O3 Y 2.371(6) 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 O1 Y O1 78.06(18) . 3 ? O1 Y O1 78.06(18) . 2 ? O1 Y O1 78.06(18) 3 2 ? O1 Y O3 135.07(17) . 3 ? O1 Y O3 85.03(19) 3 3 ? O1 Y O3 138.36(18) 2 3 ? O1 Y O3 138.36(18) . 2 ? O1 Y O3 135.06(17) 3 2 ? O1 Y O3 85.03(19) 2 2 ? O3 Y O3 80.6(2) 3 2 ? O1 Y O3 85.03(19) . . ? O1 Y O3 138.36(18) 3 . ? O1 Y O3 135.07(17) 2 . ? O3 Y O3 80.6(2) 3 . ? O3 Y O3 80.6(2) 2 . ? O1 Y O2 64.78(15) . . ? O1 Y O2 69.82(16) 3 . ? O1 Y O2 134.62(17) 2 . ? O3 Y O2 70.33(17) 3 . ? O3 Y O2 140.2(2) 2 . ? O3 Y O2 68.55(18) . . ? O1 Y O2 134.62(17) . 3 ? O1 Y O2 64.78(15) 3 3 ? O1 Y O2 69.82(16) 2 3 ? O3 Y O2 68.55(18) 3 3 ? O3 Y O2 70.33(17) 2 3 ? O3 Y O2 140.2(2) . 3 ? O2 Y O2 119.890(14) . 3 ? O1 Y O2 69.82(16) . 2 ? O1 Y O2 134.62(17) 3 2 ? O1 Y O2 64.78(15) 2 2 ? O3 Y O2 140.2(2) 3 2 ? O3 Y O2 68.55(18) 2 2 ? O3 Y O2 70.33(17) . 2 ? O2 Y O2 119.892(14) . 2 ? O2 Y O2 119.888(14) 3 2 ? C1 O1 Y 123.1(4) . 3 ? C1 O1 Y 123.1(4) . . ? C2 O2 Y 120.6(4) . 3 ? C2 O2 Y 120.6(4) . . ? O1 C1 C3 125.7(7) . 16_445 ? O1 C1 C2 114.9(6) . . ? C3 C1 C2 119.4(6) 16_445 . ? O2 C2 C3 125.7(6) . . ? O2 C2 C1 114.5(6) . . ? C3 C2 C1 119.8(6) . . ? C1 C3 C2 120.8(6) 16_445 . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 74.95 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.589 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.130 #===END data_la2can3abs97 _database_code_CSD 175602 _audit_creation_method SHELXL-97 _chemical_name_systematic 'hexaaquatris(chloranilato)dilanthanum(III) heptahydrate' _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Cl6 La2 O25' _chemical_formula_weight 1132.91 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.425(2) _cell_length_b 8.999(3) _cell_length_c 12.447(3) _cell_angle_alpha 72.14(2) _cell_angle_beta 71.60(2) _cell_angle_gamma 84.59(2) _cell_volume 852.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 18.9 _exptl_crystal_description 'irregular hexagonal plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 3.039 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6942 _exptl_absorpt_correction_T_max 0.9235 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4608 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3907 _reflns_number_gt 3456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 3907 _refine_ls_number_parameters 257 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.054 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La La 0.09671(3) 0.39351(3) 0.16284(2) 0.01592(10) Uani 1 d . . . Cl1 Cl 0.38647(16) -0.02417(14) -0.08881(11) 0.0271(3) Uani 1 d . . . Cl2 Cl -0.26144(18) -0.15398(16) 0.36039(13) 0.0354(3) Uani 1 d . . . C1 C -0.0303(6) 0.0348(6) 0.1788(4) 0.0211(9) Uani 1 d . . . C2 C 0.1295(6) 0.0660(6) 0.0729(4) 0.0200(9) Uani 1 d . . . C3 C 0.2071(6) -0.0588(5) 0.0322(4) 0.0202(9) Uani 1 d . . . C4 C 0.1477(6) -0.2109(5) 0.0876(4) 0.0184(9) Uani 1 d . . . C5 C -0.0098(6) -0.2421(5) 0.1942(4) 0.0188(9) Uani 1 d . . . C6 C -0.0872(6) -0.1188(5) 0.2368(4) 0.0208(9) Uani 1 d . . . O1 O -0.0988(5) 0.1545(4) 0.2056(4) 0.0268(8) Uani 1 d . . . O2 O 0.1784(5) 0.2040(4) 0.0300(3) 0.0290(8) Uani 1 d . . . O3 O 0.2139(5) -0.3285(4) 0.0577(3) 0.0254(8) Uani 1 d . . . O4 O -0.0602(5) -0.3807(4) 0.2369(3) 0.0264(8) Uani 1 d . . . Cl3 Cl 0.3051(2) -0.18123(17) 0.37164(13) 0.0430(4) Uani 1 d . . . C7 C -0.0438(6) 0.1567(6) 0.4414(4) 0.0206(9) Uani 1 d . . . C8 C 0.1056(6) 0.0682(6) 0.3836(4) 0.0208(9) Uani 1 d . . . C9 C 0.1390(7) -0.0842(6) 0.4437(4) 0.0242(10) Uani 1 d . . . O5 O -0.0681(5) 0.2919(4) 0.3793(3) 0.0261(8) Uani 1 d . . . O6 O 0.1938(5) 0.1412(4) 0.2813(3) 0.0272(8) Uani 1 d . . . O7 O 0.1666(5) 0.5250(4) -0.0869(3) 0.0245(7) Uani 1 d D . . H71 H 0.217(8) 0.598(6) -0.088(6) 0.037(19) Uiso 1 d D . . H72 H 0.251(7) 0.477(8) -0.108(7) 0.05(2) Uiso 1 d D . . O8 O 0.2496(6) 0.4671(6) 0.2900(4) 0.0403(10) Uani 1 d D . . H81 H 0.176(9) 0.476(11) 0.348(6) 0.07(3) Uiso 1 d D . . H82 H 0.332(9) 0.523(10) 0.260(8) 0.08(3) Uiso 1 d D . . O9 O 0.4128(5) 0.3684(5) 0.0809(4) 0.0369(10) Uani 1 d D . . H91 H 0.495(12) 0.401(15) 0.026(10) 0.15(6) Uiso 1 d D . . H92 H 0.443(17) 0.313(14) 0.136(8) 0.13(5) Uiso 1 d D . . O10 O 0.4340(6) 0.3699(5) 0.8070(4) 0.0455(11) Uani 1 d . . . O11 O 0.4020(8) 0.5477(8) 0.5962(5) 0.0681(17) Uani 1 d . . . O12 O 0.4513(9) 0.7613(10) 0.7112(10) 0.118(4) Uani 1 d . . . O13 O 0.0000 0.5000 0.5000 0.123(6) Uani 1 d S . . 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 La 0.01974(15) 0.00695(14) 0.01813(15) -0.00333(9) -0.00181(10) -0.00085(9) Cl1 0.0283(6) 0.0185(5) 0.0275(6) -0.0070(5) 0.0024(5) -0.0039(5) Cl2 0.0307(7) 0.0246(6) 0.0389(7) -0.0119(5) 0.0091(6) -0.0032(5) C1 0.022(2) 0.014(2) 0.027(2) -0.0082(18) -0.0051(19) -0.0004(18) C2 0.024(2) 0.016(2) 0.020(2) -0.0058(17) -0.0038(18) -0.0042(18) C3 0.023(2) 0.012(2) 0.022(2) -0.0037(17) -0.0028(18) -0.0004(17) C4 0.023(2) 0.013(2) 0.022(2) -0.0087(17) -0.0073(18) 0.0021(17) C5 0.021(2) 0.013(2) 0.022(2) -0.0060(17) -0.0059(18) 0.0010(17) C6 0.020(2) 0.014(2) 0.024(2) -0.0068(18) -0.0001(18) 0.0001(18) O1 0.0268(19) 0.0112(15) 0.041(2) -0.0120(15) -0.0055(16) 0.0021(14) O2 0.041(2) 0.0095(15) 0.0298(19) -0.0059(14) 0.0001(16) -0.0067(15) O3 0.033(2) 0.0093(15) 0.0273(17) -0.0076(13) 0.0020(15) -0.0008(14) O4 0.0297(19) 0.0098(15) 0.0333(19) -0.0071(14) 0.0012(15) -0.0034(14) Cl3 0.0405(8) 0.0302(7) 0.0338(7) -0.0014(6) 0.0098(6) 0.0162(6) C7 0.023(2) 0.014(2) 0.023(2) -0.0058(17) -0.0041(19) 0.0002(18) C8 0.021(2) 0.019(2) 0.021(2) -0.0065(18) -0.0031(18) -0.0014(18) C9 0.026(3) 0.018(2) 0.023(2) -0.0039(19) -0.002(2) 0.0025(19) O5 0.0299(19) 0.0160(17) 0.0217(17) -0.0015(13) 0.0017(14) 0.0040(14) O6 0.0294(19) 0.0179(17) 0.0203(17) 0.0027(13) 0.0024(15) 0.0035(14) O7 0.0232(18) 0.0184(17) 0.0323(19) -0.0105(15) -0.0063(15) 0.0017(14) O8 0.040(3) 0.053(3) 0.033(2) -0.018(2) -0.007(2) -0.014(2) O9 0.025(2) 0.029(2) 0.045(3) -0.0091(19) 0.0040(19) 0.0000(17) O10 0.036(2) 0.030(2) 0.059(3) -0.015(2) 0.003(2) -0.0058(19) O11 0.060(4) 0.092(5) 0.041(3) -0.013(3) -0.010(3) 0.018(3) O12 0.059(4) 0.093(6) 0.241(12) -0.096(7) -0.062(6) 0.031(4) O13 0.197(14) 0.095(8) 0.061(6) -0.046(6) 0.024(7) -0.078(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La O6 2.521(4) . ? La O5 2.528(4) . ? La O9 2.549(4) . ? La O3 2.566(3) 1_565 ? La O4 2.569(3) 1_565 ? La O8 2.588(4) . ? La O2 2.628(4) . ? La O7 2.636(4) 2_565 ? La O1 2.652(4) . ? La O7 2.851(4) . ? Cl1 C3 1.736(5) . ? Cl2 C6 1.728(5) . ? C1 O1 1.259(6) . ? C1 C6 1.399(7) . ? C1 C2 1.534(7) . ? C2 O2 1.244(6) . ? C2 C3 1.394(6) . ? C3 C4 1.390(6) . ? C4 O3 1.253(6) . ? C4 C5 1.526(6) . ? C5 O4 1.253(6) . ? C5 C6 1.394(6) . ? O3 La 2.566(3) 1_545 ? O4 La 2.569(3) 1_545 ? Cl3 C9 1.727(5) . ? C7 O5 1.263(6) . ? C7 C9 1.384(7) 2_556 ? C7 C8 1.526(7) . ? C8 O6 1.259(6) . ? C8 C9 1.397(7) . ? C9 C7 1.384(7) 2_556 ? O7 La 2.636(4) 2_565 ? 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 La O5 62.93(11) . . ? O6 La O9 70.13(14) . . ? O5 La O9 124.25(15) . . ? O6 La O3 136.04(13) . 1_565 ? O5 La O3 125.32(11) . 1_565 ? O9 La O3 73.15(13) . 1_565 ? O6 La O4 128.10(12) . 1_565 ? O5 La O4 70.18(11) . 1_565 ? O9 La O4 126.34(13) . 1_565 ? O3 La O4 61.23(11) 1_565 1_565 ? O6 La O8 73.39(15) . . ? O5 La O8 70.54(14) . . ? O9 La O8 68.60(16) . . ? O3 La O8 71.30(14) 1_565 . ? O4 La O8 71.09(15) 1_565 . ? O6 La O2 72.50(12) . . ? O5 La O2 120.01(11) . . ? O9 La O2 68.11(14) . . ? O3 La O2 114.54(11) 1_565 . ? O4 La O2 156.22(14) 1_565 . ? O8 La O2 131.62(15) . . ? O6 La O7 134.15(12) . 2_565 ? O5 La O7 95.55(12) . 2_565 ? O9 La O7 139.70(14) . 2_565 ? O3 La O7 89.74(12) 1_565 2_565 ? O4 La O7 69.22(12) 1_565 2_565 ? O8 La O7 140.32(14) . 2_565 ? O2 La O7 87.81(13) . 2_565 ? O6 La O1 67.70(13) . . ? O5 La O1 67.63(12) . . ? O9 La O1 119.56(13) . . ? O3 La O1 155.08(13) 1_565 . ? O4 La O1 113.60(11) 1_565 . ? O8 La O1 132.19(14) . . ? O2 La O1 59.22(12) . . ? O7 La O1 66.65(12) 2_565 . ? O6 La O7 130.32(11) . . ? O5 La O7 159.90(12) . . ? O9 La O7 75.68(14) . . ? O3 La O7 58.82(11) 1_565 . ? O4 La O7 101.10(11) 1_565 . ? O8 La O7 124.94(13) . . ? O2 La O7 61.70(11) . . ? O7 La O7 64.35(14) 2_565 . ? O1 La O7 101.56(12) . . ? O1 C1 C6 125.7(5) . . ? O1 C1 C2 115.1(4) . . ? C6 C1 C2 119.2(4) . . ? O2 C2 C3 125.5(5) . . ? O2 C2 C1 115.7(4) . . ? C3 C2 C1 118.8(4) . . ? C4 C3 C2 122.0(4) . . ? C4 C3 Cl1 118.9(4) . . ? C2 C3 Cl1 119.1(4) . . ? O3 C4 C3 125.2(4) . . ? O3 C4 C5 115.7(4) . . ? C3 C4 C5 119.1(4) . . ? O4 C5 C6 124.7(4) . . ? O4 C5 C4 115.8(4) . . ? C6 C5 C4 119.5(4) . . ? C5 C6 C1 121.2(4) . . ? C5 C6 Cl2 119.8(4) . . ? C1 C6 Cl2 118.9(4) . . ? C1 O1 La 117.7(3) . . ? C2 O2 La 119.7(3) . . ? C4 O3 La 123.7(3) . 1_545 ? C5 O4 La 123.5(3) . 1_545 ? O5 C7 C9 125.8(5) . 2_556 ? O5 C7 C8 116.2(4) . . ? C9 C7 C8 118.0(4) 2_556 . ? O6 C8 C9 123.7(5) . . ? O6 C8 C7 116.0(4) . . ? C9 C8 C7 120.4(4) . . ? C7 C9 C8 121.5(5) 2_556 . ? C7 C9 Cl3 120.2(4) 2_556 . ? C8 C9 Cl3 118.3(4) . . ? C7 O5 La 121.5(3) . . ? C8 O6 La 121.7(3) . . ? La O7 La 115.65(14) 2_565 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.102 _refine_diff_density_min -2.654 _refine_diff_density_rms 0.187 #===END data_cecanlsabs97 _database_code_CSD 175603 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(chloranilato)dicerium(III) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 Ce2 Cl6 O30' _chemical_formula_weight 1225.41 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9480(8) _cell_length_b 10.0430(7) _cell_length_c 11.1940(6) _cell_angle_alpha 88.914(5) _cell_angle_beta 85.035(6) _cell_angle_gamma 67.714(6) _cell_volume 1030.83(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.4 _cell_measurement_theta_max 17.3 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 2.665 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6043 _exptl_absorpt_correction_T_max 0.9424 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4 _diffrn_reflns_number 5458 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4732 _reflns_number_gt 4101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0533P)^2^+0.4636P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4732 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.28901(2) 0.72562(2) 0.34583(2) 0.02090(8) Uani 1 1 d . . . Cl1 Cl -0.22312(14) 0.64322(16) 0.30447(13) 0.0457(3) Uani 1 1 d . . . O1 O 0.2403(3) 0.5633(3) 0.5036(3) 0.0296(7) Uani 1 1 d . . . O2 O 0.0473(3) 0.6928(3) 0.3501(3) 0.0314(7) Uani 1 1 d . . . C1 C 0.1291(4) 0.5299(4) 0.5077(4) 0.0231(8) Uani 1 1 d . . . C2 C 0.0201(4) 0.6026(5) 0.4154(4) 0.0250(8) Uani 1 1 d . . . C3 C -0.1015(5) 0.5650(5) 0.4111(4) 0.0289(9) Uani 1 1 d . . . Cl2 Cl 0.35792(15) 1.24395(13) 0.31224(12) 0.0413(3) Uani 1 1 d . . . O3 O 0.4530(3) 0.7537(3) 0.4941(3) 0.0283(7) Uani 1 1 d . . . O4 O 0.3365(4) 0.9555(3) 0.3399(3) 0.0335(7) Uani 1 1 d . . . C4 C 0.4802(4) 0.8656(4) 0.5022(4) 0.0239(8) Uani 1 1 d . . . C5 C 0.4114(5) 0.9830(4) 0.4116(4) 0.0261(9) Uani 1 1 d . . . C6 C 0.4354(5) 1.1116(5) 0.4158(4) 0.0278(9) Uani 1 1 d . . . Cl3 Cl 0.27469(15) 0.34441(15) 0.01455(12) 0.0427(3) Uani 1 1 d . . . O5 O 0.2880(4) 0.5668(4) 0.1791(3) 0.0339(7) Uani 1 1 d . . . O6 O 0.4659(4) 0.7048(3) 0.1655(3) 0.0328(7) Uani 1 1 d . . . C7 C 0.3841(5) 0.5312(5) 0.0930(4) 0.0261(9) Uani 1 1 d . . . C8 C 0.4901(5) 0.6102(5) 0.0856(4) 0.0266(9) Uani 1 1 d . . . C9 C 0.3996(5) 0.4273(5) 0.0054(4) 0.0288(9) Uani 1 1 d . . . O7 O 0.5165(3) 0.4892(3) 0.3549(3) 0.0311(7) Uani 1 1 d . . . O8 O 0.1258(4) 0.8826(4) 0.5216(4) 0.0504(10) Uani 1 1 d . . . O9 O 0.1292(5) 0.9035(4) 0.2081(4) 0.0551(11) Uani 1 1 d . . . O10 O 0.4625(14) 0.9786(13) 0.0816(12) 0.087(3) Uiso 0.50 1 d P . . O11 O 0.0405(12) 0.1968(12) 0.2914(11) 0.104(4) Uiso 0.75(2) 1 d P . . O12 O 0.044(4) 0.200(4) 0.168(3) 0.123(15) Uiso 0.25(2) 1 d P . . O13 O 0.051(5) 0.206(5) 0.354(5) 0.150 Uiso 0.25(2) 1 d P . . O14 O 0.721(4) 0.062(4) 0.050(4) 0.066(12) Uiso 0.17(2) 1 d P . . O15 O 0.608(3) 0.950(3) 0.149(3) 0.131(13) Uiso 0.33(2) 1 d P . . O16 O 1.002(2) 0.747(2) 0.067(2) 0.117(7) Uiso 0.431(15) 1 d P . . O17 O 0.726(3) 0.248(3) 0.172(3) 0.150 Uiso 0.431(15) 1 d P . . O18 O -0.0889(19) 0.3351(18) 0.1166(16) 0.147(7) Uiso 0.569(15) 1 d P . . O19 O 0.9475(13) 0.8099(13) 0.0990(11) 0.078(3) Uiso 0.569(15) 1 d P . . O20 O 0.7949(15) 0.9645(16) 0.3421(18) 0.055(7) Uiso 0.36(4) 1 d P . . O21 O 0.757(3) 0.189(3) 0.249(3) 0.150 Uiso 0.37(2) 1 d P . . O22 O -0.268(3) 0.008(4) 0.007(3) 0.150 Uiso 0.39(3) 1 d P . . O23 O -0.306(5) 0.018(5) 0.122(5) 0.150 Uiso 0.243(19) 1 d P . . O24 O -0.205(4) -0.004(5) 0.285(6) 0.146(18) Uiso 0.31(4) 1 d P . . 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 0.02191(12) 0.02209(12) 0.02334(13) -0.00129(8) -0.00236(8) -0.01340(9) Cl1 0.0379(6) 0.0662(8) 0.0471(7) 0.0261(6) -0.0216(6) -0.0329(6) O1 0.0243(15) 0.0352(16) 0.0360(18) 0.0058(14) -0.0055(13) -0.0184(13) O2 0.0293(16) 0.0371(17) 0.0360(18) 0.0098(14) -0.0071(14) -0.0213(14) C1 0.0175(18) 0.0255(19) 0.029(2) -0.0022(17) -0.0015(16) -0.0115(15) C2 0.0203(19) 0.028(2) 0.028(2) -0.0011(17) 0.0009(17) -0.0118(16) C3 0.022(2) 0.040(2) 0.030(2) 0.0092(19) -0.0091(18) -0.0170(18) Cl2 0.0576(8) 0.0317(6) 0.0458(7) 0.0145(5) -0.0277(6) -0.0252(5) O3 0.0342(16) 0.0212(14) 0.0367(18) 0.0033(13) -0.0107(14) -0.0170(12) O4 0.047(2) 0.0294(16) 0.0348(18) 0.0049(14) -0.0183(16) -0.0235(15) C4 0.0221(19) 0.0220(19) 0.030(2) -0.0002(16) -0.0051(17) -0.0105(15) C5 0.029(2) 0.024(2) 0.031(2) -0.0007(17) -0.0061(18) -0.0144(17) C6 0.036(2) 0.024(2) 0.031(2) 0.0042(17) -0.0114(19) -0.0175(18) Cl3 0.0503(7) 0.0586(8) 0.0384(7) -0.0071(6) 0.0004(6) -0.0428(6) O5 0.0326(17) 0.0458(19) 0.0298(17) -0.0118(15) 0.0051(14) -0.0234(15) O6 0.0431(19) 0.0352(17) 0.0297(17) -0.0074(14) 0.0020(14) -0.0261(15) C7 0.024(2) 0.033(2) 0.025(2) 0.0007(17) -0.0059(17) -0.0153(17) C8 0.033(2) 0.027(2) 0.025(2) 0.0006(17) -0.0060(18) -0.0162(18) C9 0.035(2) 0.034(2) 0.027(2) 0.0006(18) -0.0046(18) -0.0238(19) O7 0.0275(16) 0.0268(15) 0.0409(19) 0.0031(14) -0.0077(14) -0.0116(13) O8 0.049(2) 0.043(2) 0.051(2) -0.0137(18) 0.0123(19) -0.0115(18) O9 0.055(2) 0.051(2) 0.068(3) 0.021(2) -0.035(2) -0.024(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 Ce1 O5 2.481(3) . ? Ce1 O9 2.503(4) . ? Ce1 O3 2.516(3) . ? Ce1 O6 2.518(3) . ? Ce1 O1 2.521(3) . ? Ce1 O4 2.524(3) . ? Ce1 O2 2.545(3) . ? Ce1 O8 2.572(4) . ? Ce1 O7 2.593(3) . ? Cl1 C3 1.731(5) . ? O1 C1 1.269(5) . ? O2 C2 1.246(5) . ? C1 C3 1.391(6) 2_566 ? C1 C2 1.530(6) . ? C2 C3 1.402(6) . ? C3 C1 1.391(6) 2_566 ? Cl2 C6 1.738(5) . ? O3 C4 1.259(5) . ? O4 C5 1.244(5) . ? C4 C6 1.374(6) 2_676 ? C4 C5 1.533(6) . ? C5 C6 1.401(5) . ? C6 C4 1.374(6) 2_676 ? Cl3 C9 1.734(4) . ? O5 C7 1.251(5) . ? O6 C8 1.258(5) . ? C7 C9 1.401(6) . ? C7 C8 1.538(6) . ? C8 C9 1.375(6) 2_665 ? C9 C8 1.375(6) 2_665 ? 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 O5 Ce1 O9 78.47(14) . . ? O5 Ce1 O3 141.38(11) . . ? O9 Ce1 O3 130.78(12) . . ? O5 Ce1 O6 63.30(10) . . ? O9 Ce1 O6 78.63(14) . . ? O3 Ce1 O6 94.82(11) . . ? O5 Ce1 O1 92.86(11) . . ? O9 Ce1 O1 132.75(12) . . ? O3 Ce1 O1 83.11(10) . . ? O6 Ce1 O1 138.04(11) . . ? O5 Ce1 O4 129.84(11) . . ? O9 Ce1 O4 68.83(12) . . ? O3 Ce1 O4 62.65(10) . . ? O6 Ce1 O4 73.49(11) . . ? O1 Ce1 O4 137.24(11) . . ? O5 Ce1 O2 68.48(11) . . ? O9 Ce1 O2 71.17(12) . . ? O3 Ce1 O2 137.83(11) . . ? O6 Ce1 O2 126.92(11) . . ? O1 Ce1 O2 62.59(10) . . ? O4 Ce1 O2 129.05(11) . . ? O5 Ce1 O8 142.29(12) . . ? O9 Ce1 O8 87.51(15) . . ? O3 Ce1 O8 72.30(12) . . ? O6 Ce1 O8 147.52(12) . . ? O1 Ce1 O8 71.40(12) . . ? O4 Ce1 O8 74.13(12) . . ? O2 Ce1 O8 73.88(13) . . ? O5 Ce1 O7 72.55(11) . . ? O9 Ce1 O7 144.38(14) . . ? O3 Ce1 O7 70.02(10) . . ? O6 Ce1 O7 70.13(11) . . ? O1 Ce1 O7 69.87(10) . . ? O4 Ce1 O7 115.96(10) . . ? O2 Ce1 O7 114.97(10) . . ? O8 Ce1 O7 128.11(13) . . ? C1 O1 Ce1 122.6(3) . . ? C2 O2 Ce1 122.1(3) . . ? O1 C1 C3 124.7(4) . 2_566 ? O1 C1 C2 115.7(4) . . ? C3 C1 C2 119.6(3) 2_566 . ? O2 C2 C3 125.2(4) . . ? O2 C2 C1 116.2(4) . . ? C3 C2 C1 118.6(4) . . ? C1 C3 C2 121.7(4) 2_566 . ? C1 C3 Cl1 119.3(3) 2_566 . ? C2 C3 Cl1 119.0(3) . . ? C4 O3 Ce1 122.9(3) . . ? C5 O4 Ce1 122.9(3) . . ? O3 C4 C6 125.2(4) . 2_676 ? O3 C4 C5 115.5(4) . . ? C6 C4 C5 119.4(4) 2_676 . ? O4 C5 C6 125.1(4) . . ? O4 C5 C4 116.0(4) . . ? C6 C5 C4 118.9(4) . . ? C4 C6 C5 121.8(4) 2_676 . ? C4 C6 Cl2 119.6(3) 2_676 . ? C5 C6 Cl2 118.6(3) . . ? C7 O5 Ce1 122.6(3) . . ? C8 O6 Ce1 121.1(3) . . ? O5 C7 C9 124.7(4) . . ? O5 C7 C8 115.9(4) . . ? C9 C7 C8 119.4(4) . . ? O6 C8 C9 126.2(4) . 2_665 ? O6 C8 C7 115.3(4) . . ? C9 C8 C7 118.4(4) 2_665 . ? C8 C9 C7 122.1(4) 2_665 . ? C8 C9 Cl3 119.9(3) 2_665 . ? C7 C9 Cl3 118.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.931 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.135 #===END data_prcanceabs97 _database_code_CSD 175604 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(chloranilato)dipraseodymium(III) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 Cl6 O30 Pr2' _chemical_formula_weight 1226.99 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' 'Cl' 'Cl' 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.899(3) _cell_length_b 9.998(2) _cell_length_c 11.141(4) _cell_angle_alpha 89.07(2) _cell_angle_beta 84.37(3) _cell_angle_gamma 67.93(3) _cell_volume 1016.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.5 _cell_measurement_theta_max 12.9 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 2.860 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8120 _exptl_absorpt_correction_T_max 0.9212 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The crystal was glued on to the end of a thin glass fibre. The crystal was directly exposed to the atmosphere throughout the data collection. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 _diffrn_reflns_number 5367 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4648 _reflns_number_gt 3560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 - Software' _computing_cell_refinement 'CAD4 - Software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1726P)^2^+13.1701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4648 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2677 _refine_ls_wR_factor_gt 0.2406 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Pr1 Pr 0.29067(7) 0.72469(7) 0.34718(6) 0.0196(2) Uani 1 1 d . . . Cl1 Cl -0.2211(4) 0.6435(5) 0.3045(4) 0.0452(10) Uani 1 1 d . . . O1 O 0.2416(10) 0.5641(11) 0.5035(9) 0.028(2) Uani 1 1 d . . . O2 O 0.0502(10) 0.6926(11) 0.3506(10) 0.031(2) Uani 1 1 d . . . C1 C 0.1312(15) 0.5304(15) 0.5066(12) 0.025(3) Uani 1 1 d . . . C2 C 0.0202(14) 0.6025(15) 0.4165(11) 0.024(3) Uani 1 1 d . . . C3 C -0.1003(14) 0.5635(17) 0.4122(12) 0.029(3) Uani 1 1 d . . . Cl2 Cl 0.3600(5) 1.2427(4) 0.3115(4) 0.0418(9) Uani 1 1 d . . . O3 O 0.4523(11) 0.7522(10) 0.4952(9) 0.029(2) Uani 1 1 d . . . O4 O 0.3360(12) 0.9528(10) 0.3412(10) 0.031(2) Uani 1 1 d . . . C4 C 0.4800(14) 0.8652(14) 0.5043(13) 0.024(3) Uani 1 1 d . . . C5 C 0.4089(14) 0.9833(13) 0.4130(12) 0.023(2) Uani 1 1 d . . . C6 C 0.4371(16) 1.1107(15) 0.4144(12) 0.027(3) Uani 1 1 d . . . Cl3 Cl 0.2705(5) 0.3461(5) 0.0158(4) 0.0450(10) Uani 1 1 d . . . O5 O 0.2869(12) 0.5664(12) 0.1832(9) 0.035(2) Uani 1 1 d . . . O6 O 0.4685(12) 0.7036(11) 0.1685(9) 0.032(2) Uani 1 1 d . . . C7 C 0.3848(14) 0.5292(15) 0.0953(13) 0.028(3) Uani 1 1 d . . . C8 C 0.4909(15) 0.6102(15) 0.0864(14) 0.030(3) Uani 1 1 d . . . C9 C 0.3999(19) 0.4265(17) 0.0066(14) 0.036(3) Uani 1 1 d . . . O7 O 0.5170(11) 0.4888(10) 0.3535(10) 0.031(2) Uani 1 1 d . . . O8 O 0.1268(14) 0.8817(14) 0.5194(12) 0.051(3) Uani 1 1 d . . . O9 O 0.1349(15) 0.8993(14) 0.2108(13) 0.053(3) Uani 1 1 d . . . O10 O 0.465(5) 0.980(5) 0.078(4) 0.092(11) Uiso 0.50 1 d P . . O11 O 0.040(4) 0.196(4) 0.285(4) 0.095(12) Uiso 0.69(8) 1 d P . . O12 O 0.057(13) 0.186(12) 0.144(11) 0.16(6) Uiso 0.31(8) 1 d P . . O13 O 0.046(14) 0.219(14) 0.339(14) 0.150 Uiso 0.31(8) 1 d P . . O14 O 0.722(16) 0.071(17) 0.105(17) 0.150 Uiso 0.24(5) 1 d P . . O15 O 0.580(19) 0.952(14) 0.151(12) 0.150 Uiso 0.26(5) 1 d P . . O16 O 1.010(8) 0.746(8) 0.065(6) 0.091(19) Uiso 0.36(4) 1 d P . . O17 O 0.728(10) 0.249(10) 0.159(9) 0.150 Uiso 0.36(4) 1 d P . . O18 O -0.099(6) 0.331(6) 0.117(5) 0.150 Uiso 0.64(4) 1 d P . . O19 O 0.954(4) 0.804(4) 0.095(3) 0.088(10) Uiso 0.64(4) 1 d P . . O20 O 0.797(4) 0.972(4) 0.330(3) 0.076(13) Uiso 0.50(5) 1 d P . . O21 O 0.747(7) 0.193(7) 0.247(7) 0.14(3) Uiso 0.50(5) 1 d P . . O22 O -0.283(8) 0.040(8) 0.021(8) 0.150 Uiso 0.50(7) 1 d P . . O23 O -0.320(13) -0.054(11) 0.139(9) 0.150 Uiso 0.36(7) 1 d P . . 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 0.0218(4) 0.0189(4) 0.0205(4) -0.0017(2) -0.0024(2) -0.0104(2) Cl1 0.040(2) 0.065(3) 0.043(2) 0.0256(19) -0.0213(17) -0.0304(19) O1 0.027(5) 0.037(5) 0.027(5) 0.007(4) -0.009(4) -0.018(4) O2 0.016(4) 0.035(5) 0.044(6) 0.006(5) -0.006(4) -0.010(4) C1 0.029(6) 0.031(7) 0.018(6) -0.007(5) 0.001(5) -0.014(5) C2 0.028(6) 0.031(7) 0.017(6) -0.005(5) 0.008(5) -0.016(5) C3 0.021(6) 0.043(8) 0.022(6) 0.011(6) -0.003(5) -0.012(6) Cl2 0.061(2) 0.0310(18) 0.044(2) 0.0137(16) -0.0266(19) -0.0243(17) O3 0.040(5) 0.021(4) 0.034(5) 0.000(4) -0.015(4) -0.016(4) O4 0.042(6) 0.024(5) 0.036(6) 0.005(4) -0.018(5) -0.018(4) C4 0.023(6) 0.020(6) 0.031(7) 0.007(5) -0.010(5) -0.008(5) C5 0.028(6) 0.018(6) 0.021(6) -0.006(5) 0.003(5) -0.008(5) C6 0.039(7) 0.031(7) 0.019(6) 0.005(5) -0.010(5) -0.022(6) Cl3 0.053(2) 0.060(3) 0.041(2) -0.0070(18) 0.0003(18) -0.044(2) O5 0.041(6) 0.047(6) 0.022(5) -0.015(4) 0.008(4) -0.025(5) O6 0.043(6) 0.027(5) 0.029(5) -0.007(4) 0.004(4) -0.020(4) C7 0.018(6) 0.034(7) 0.027(7) 0.010(6) -0.009(5) -0.002(5) C8 0.028(7) 0.026(6) 0.033(7) 0.001(6) -0.007(6) -0.003(5) C9 0.051(9) 0.037(8) 0.033(8) -0.004(6) 0.000(7) -0.030(7) O7 0.032(5) 0.024(5) 0.041(6) 0.005(4) -0.014(4) -0.012(4) O8 0.049(7) 0.047(7) 0.048(7) -0.017(6) 0.014(6) -0.010(6) O9 0.057(8) 0.046(7) 0.063(9) 0.019(6) -0.034(7) -0.022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O5 2.448(10) . ? Pr1 O9 2.466(12) . ? Pr1 O6 2.481(10) . ? Pr1 O4 2.483(9) . ? Pr1 O1 2.485(9) . ? Pr1 O3 2.494(9) . ? Pr1 O2 2.515(9) . ? Pr1 O8 2.520(11) . ? Pr1 O7 2.577(10) . ? Cl1 C3 1.743(14) . ? O1 C1 1.256(16) . ? O2 C2 1.255(16) . ? C1 C3 1.389(19) 2_566 ? C1 C2 1.526(19) . ? C2 C3 1.393(18) . ? C3 C1 1.389(19) 2_566 ? Cl2 C6 1.733(14) . ? O3 C4 1.266(16) . ? O4 C5 1.242(16) . ? C4 C6 1.361(18) 2_676 ? C4 C5 1.549(18) . ? C5 C6 1.403(17) . ? C6 C4 1.361(18) 2_676 ? Cl3 C9 1.745(15) . ? O5 C7 1.261(17) . ? O6 C8 1.262(17) . ? C7 C9 1.39(2) . ? C7 C8 1.54(2) . ? C8 C9 1.37(2) 2_665 ? C9 C8 1.37(2) 2_665 ? 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 O5 Pr1 O9 78.2(4) . . ? O5 Pr1 O6 64.6(3) . . ? O9 Pr1 O6 78.6(4) . . ? O5 Pr1 O4 130.5(4) . . ? O9 Pr1 O4 68.4(4) . . ? O6 Pr1 O4 73.6(3) . . ? O5 Pr1 O1 92.2(3) . . ? O9 Pr1 O1 133.1(4) . . ? O6 Pr1 O1 137.8(3) . . ? O4 Pr1 O1 137.3(3) . . ? O5 Pr1 O3 141.9(4) . . ? O9 Pr1 O3 131.2(4) . . ? O6 Pr1 O3 94.7(4) . . ? O4 Pr1 O3 63.4(3) . . ? O1 Pr1 O3 82.6(3) . . ? O5 Pr1 O2 67.3(3) . . ? O9 Pr1 O2 70.9(4) . . ? O6 Pr1 O2 126.9(3) . . ? O4 Pr1 O2 128.4(3) . . ? O1 Pr1 O2 63.2(3) . . ? O3 Pr1 O2 138.0(4) . . ? O5 Pr1 O8 141.1(4) . . ? O9 Pr1 O8 87.0(5) . . ? O6 Pr1 O8 147.1(4) . . ? O4 Pr1 O8 73.6(4) . . ? O1 Pr1 O8 72.1(4) . . ? O3 Pr1 O8 72.7(4) . . ? O2 Pr1 O8 73.9(4) . . ? O5 Pr1 O7 72.6(4) . . ? O9 Pr1 O7 143.8(4) . . ? O6 Pr1 O7 69.7(3) . . ? O4 Pr1 O7 116.6(3) . . ? O1 Pr1 O7 69.8(3) . . ? O3 Pr1 O7 70.2(3) . . ? O2 Pr1 O7 115.0(3) . . ? O8 Pr1 O7 129.2(4) . . ? C1 O1 Pr1 122.0(8) . . ? C2 O2 Pr1 122.3(9) . . ? O1 C1 C3 125.0(13) . 2_566 ? O1 C1 C2 117.2(12) . . ? C3 C1 C2 117.7(11) 2_566 . ? O2 C2 C3 126.0(13) . . ? O2 C2 C1 114.5(11) . . ? C3 C2 C1 119.5(12) . . ? C1 C3 C2 122.6(12) 2_566 . ? C1 C3 Cl1 119.2(10) 2_566 . ? C2 C3 Cl1 118.1(10) . . ? C4 O3 Pr1 122.9(8) . . ? C5 O4 Pr1 123.4(9) . . ? O3 C4 C6 125.9(12) . 2_676 ? O3 C4 C5 114.4(11) . . ? C6 C4 C5 119.7(11) 2_676 . ? O4 C5 C6 125.8(13) . . ? O4 C5 C4 115.8(11) . . ? C6 C5 C4 118.2(12) . . ? C4 C6 C5 122.0(12) 2_676 . ? C4 C6 Cl2 119.3(10) 2_676 . ? C5 C6 Cl2 118.7(10) . . ? C7 O5 Pr1 122.0(9) . . ? C8 O6 Pr1 120.9(9) . . ? O5 C7 C9 125.2(14) . . ? O5 C7 C8 115.5(13) . . ? C9 C7 C8 119.2(13) . . ? O6 C8 C9 126.4(14) . 2_665 ? O6 C8 C7 115.6(13) . . ? C9 C8 C7 118.1(13) 2_665 . ? C8 C9 C7 122.7(13) 2_665 . ? C8 C9 Cl3 119.9(11) 2_665 . ? C7 C9 Cl3 117.4(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 6.460 _refine_diff_density_min -1.984 _refine_diff_density_rms 0.389 #===END data_tbcanabs97 _database_code_CSD 175605 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(chloranilato)diterbium(III) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 Cl6 O30 Tb2' _chemical_formula_weight 1263.01 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.796(1) _cell_length_b 9.905(1) _cell_length_c 11.028(2) _cell_angle_alpha 89.75(1) _cell_angle_beta 83.48(1) _cell_angle_gamma 68.40(1) _cell_volume 987.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.2 _cell_measurement_theta_max 13.5 _exptl_crystal_description 'deep purple' _exptl_crystal_colour 'rectangular plate' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.014 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 4.057 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8111 _exptl_absorpt_correction_T_max 0.9509 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3.5 _diffrn_reflns_number 4063 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3471 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3471 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.002 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 0.29164(5) 0.72387(5) 0.35023(5) 0.01856(14) Uani 1 1 d . . . Cl1 Cl -0.2181(3) 0.6397(3) 0.3024(3) 0.0405(7) Uani 1 1 d . . . O1 O 0.2417(6) 0.5683(7) 0.5034(6) 0.0264(15) Uani 1 1 d . . . O2 O 0.0498(7) 0.6975(6) 0.3542(6) 0.0252(15) Uani 1 1 d . . . C1 C 0.1297(9) 0.5325(9) 0.5094(9) 0.023(2) Uani 1 1 d . . . C2 C 0.0212(9) 0.6046(9) 0.4178(8) 0.0193(19) Uani 1 1 d . . . C3 C -0.0999(9) 0.5627(10) 0.4090(8) 0.021(2) Uani 1 1 d . . . Cl2 Cl 0.3611(3) 1.2410(3) 0.3110(3) 0.0388(7) Uani 1 1 d . . . O3 O 0.4500(7) 0.7502(6) 0.4940(6) 0.0279(16) Uani 1 1 d . . . O4 O 0.3361(7) 0.9503(6) 0.3412(6) 0.0287(16) Uani 1 1 d . . . C4 C 0.4781(10) 0.8644(9) 0.5016(9) 0.023(2) Uani 1 1 d . . . C5 C 0.4131(10) 0.9800(9) 0.4112(8) 0.022(2) Uani 1 1 d . . . C6 C 0.4363(10) 1.1094(9) 0.4157(9) 0.026(2) Uani 1 1 d . . . Cl3 Cl 0.2660(3) 0.3462(3) 0.0175(2) 0.0377(6) Uani 1 1 d . . . O5 O 0.2890(7) 0.5639(7) 0.1899(6) 0.0260(15) Uani 1 1 d . . . O6 O 0.4716(7) 0.7028(7) 0.1736(6) 0.0275(15) Uani 1 1 d . . . C7 C 0.3846(10) 0.5297(9) 0.0988(8) 0.021(2) Uani 1 1 d . . . C8 C 0.4946(10) 0.6069(9) 0.0899(9) 0.024(2) Uani 1 1 d . . . C9 C 0.3918(10) 0.4288(10) 0.0078(9) 0.023(2) Uani 1 1 d . . . O7 O 0.5147(6) 0.4929(6) 0.3539(6) 0.0246(14) Uani 1 1 d . . . O8 O 0.1277(7) 0.8830(7) 0.5190(7) 0.0383(18) Uani 1 1 d . . . O9 O 0.1414(7) 0.8912(7) 0.2152(7) 0.0379(18) Uani 1 1 d . . . O10 O 0.457(2) 0.977(2) 0.0762(19) 0.080(6) Uiso 0.50 1 d P . . O11 O 0.036(2) 0.1931(19) 0.280(2) 0.112(6) Uiso 0.83(3) 1 d P . . O12 O 0.051(8) 0.198(8) 0.169(8) 0.10(3) Uiso 0.17(3) 1 d P . . O13 O 0.059(5) 0.197(5) 0.338(5) 0.038(17) Uiso 0.17(3) 1 d P . . O14 O 0.696(6) 0.055(6) 0.026(7) 0.056(19) Uiso 0.19(4) 1 d P . . O15 O 0.630(6) 0.953(6) 0.145(5) 0.16(3) Uiso 0.31(4) 1 d P . . O16 O 1.009(3) 0.757(3) 0.064(2) 0.071(8) Uiso 0.50(3) 1 d P . . O17 O 0.788(6) 0.272(5) 0.162(4) 0.19(2) Uiso 0.50(3) 1 d P . . O18 O -0.095(4) 0.330(4) 0.111(4) 0.166(19) Uiso 0.50(3) 1 d P . . O19 O 0.945(3) 0.816(3) 0.101(2) 0.077(8) Uiso 0.50(3) 1 d P . . O20 O 0.800(3) 0.959(3) 0.337(4) 0.047(15) Uiso 0.35(8) 1 d P . . O21 O 0.759(6) 0.179(6) 0.241(6) 0.150 Uiso 0.33(3) 1 d P . . O22 O -0.245(8) 0.001(8) -0.007(7) 0.150 Uiso 0.35(5) 1 d P . . O23 O -0.265(6) 0.040(6) 0.089(7) 0.150 Uiso 0.38(4) 1 d P . . O24 O -0.199(6) 0.000(10) 0.290(10) 0.150 Uiso 0.32(8) 1 d P . . O25 O 0.284(9) 0.776(9) -0.153(8) 0.08(4) Uiso 0.14(5) 1 d P . . 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 0.0215(2) 0.0185(2) 0.0196(2) -0.00062(16) -0.00276(16) -0.01195(17) Cl1 0.0353(14) 0.0574(17) 0.0422(16) 0.0238(14) -0.0204(13) -0.0285(13) O1 0.023(3) 0.034(4) 0.031(4) 0.008(3) -0.004(3) -0.021(3) O2 0.026(3) 0.026(3) 0.029(4) 0.004(3) -0.001(3) -0.017(3) C1 0.018(4) 0.020(5) 0.032(6) -0.006(4) 0.002(4) -0.009(4) C2 0.022(5) 0.021(5) 0.016(5) 0.001(4) -0.001(4) -0.010(4) C3 0.022(5) 0.026(5) 0.022(5) 0.007(4) -0.008(4) -0.015(4) Cl2 0.0576(17) 0.0279(13) 0.0441(16) 0.0151(12) -0.0268(14) -0.0253(12) O3 0.036(4) 0.019(3) 0.037(4) 0.003(3) -0.010(3) -0.018(3) O4 0.044(4) 0.025(3) 0.028(4) 0.002(3) -0.012(3) -0.023(3) C4 0.028(5) 0.018(4) 0.024(5) -0.009(4) 0.002(4) -0.011(4) C5 0.034(5) 0.023(5) 0.017(5) -0.005(4) -0.006(4) -0.020(4) C6 0.029(5) 0.020(5) 0.033(6) -0.001(4) -0.011(4) -0.011(4) Cl3 0.0457(15) 0.0484(15) 0.0356(15) -0.0042(13) -0.0012(12) -0.0376(13) O5 0.026(3) 0.032(4) 0.028(4) -0.006(3) 0.000(3) -0.020(3) O6 0.035(4) 0.030(4) 0.027(4) 0.002(3) -0.004(3) -0.024(3) C7 0.024(5) 0.020(5) 0.023(5) 0.000(4) -0.002(4) -0.014(4) C8 0.038(5) 0.019(5) 0.023(5) 0.005(4) -0.010(4) -0.019(4) C9 0.025(5) 0.028(5) 0.025(5) -0.005(4) -0.007(4) -0.019(4) O7 0.021(3) 0.024(3) 0.028(4) 0.000(3) 0.002(3) -0.008(3) O8 0.032(4) 0.032(4) 0.040(5) -0.006(3) 0.006(3) -0.002(3) O9 0.035(4) 0.041(4) 0.044(5) 0.010(4) -0.017(4) -0.019(3) _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 O5 2.389(6) . ? Tb1 O1 2.411(6) . ? Tb1 O9 2.411(7) . ? Tb1 O3 2.418(6) . ? Tb1 O6 2.429(6) . ? Tb1 O4 2.437(6) . ? Tb1 O8 2.451(7) . ? Tb1 O2 2.473(6) . ? Tb1 O7 2.520(6) . ? Cl1 C3 1.719(9) . ? O1 C1 1.267(10) . ? O2 C2 1.248(10) . ? C1 C3 1.386(12) 2_566 ? C1 C2 1.529(12) . ? C2 C3 1.406(12) . ? C3 C1 1.385(12) 2_566 ? Cl2 C6 1.746(10) . ? O3 C4 1.264(10) . ? O4 C5 1.245(10) . ? C4 C6 1.392(13) 2_676 ? C4 C5 1.519(13) . ? C5 C6 1.384(12) . ? C6 C4 1.392(13) 2_676 ? Cl3 C9 1.707(9) . ? O5 C7 1.248(10) . ? O6 C8 1.268(11) . ? C7 C9 1.397(12) . ? C7 C8 1.529(11) . ? C8 C9 1.402(13) 2_665 ? C9 C8 1.402(13) 2_665 ? 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 O5 Tb1 O1 91.4(2) . . ? O5 Tb1 O9 78.1(2) . . ? O1 Tb1 O9 133.4(2) . . ? O5 Tb1 O3 141.1(2) . . ? O1 Tb1 O3 82.2(2) . . ? O9 Tb1 O3 132.3(2) . . ? O5 Tb1 O6 65.9(2) . . ? O1 Tb1 O6 137.8(2) . . ? O9 Tb1 O6 78.5(2) . . ? O3 Tb1 O6 93.8(2) . . ? O5 Tb1 O4 130.4(2) . . ? O1 Tb1 O4 138.2(2) . . ? O9 Tb1 O4 68.0(2) . . ? O3 Tb1 O4 64.9(2) . . ? O6 Tb1 O4 72.5(2) . . ? O5 Tb1 O8 140.7(2) . . ? O1 Tb1 O8 73.1(2) . . ? O9 Tb1 O8 86.8(2) . . ? O3 Tb1 O8 73.7(2) . . ? O6 Tb1 O8 145.8(2) . . ? O4 Tb1 O8 73.4(2) . . ? O5 Tb1 O2 67.5(2) . . ? O1 Tb1 O2 64.5(2) . . ? O9 Tb1 O2 69.6(2) . . ? O3 Tb1 O2 138.4(2) . . ? O6 Tb1 O2 127.5(2) . . ? O4 Tb1 O2 126.6(2) . . ? O8 Tb1 O2 73.3(2) . . ? O5 Tb1 O7 72.4(2) . . ? O1 Tb1 O7 69.8(2) . . ? O9 Tb1 O7 143.1(2) . . ? O3 Tb1 O7 69.4(2) . . ? O6 Tb1 O7 69.5(2) . . ? O4 Tb1 O7 116.8(2) . . ? O8 Tb1 O7 130.2(2) . . ? O2 Tb1 O7 116.65(19) . . ? C1 O1 Tb1 123.0(6) . . ? C2 O2 Tb1 120.6(6) . . ? O1 C1 C3 125.4(9) . 2_566 ? O1 C1 C2 114.9(8) . . ? C3 C1 C2 119.7(7) 2_566 . ? O2 C2 C3 124.7(8) . . ? O2 C2 C1 115.7(7) . . ? C3 C2 C1 119.6(8) . . ? C1 C3 C2 120.4(8) 2_566 . ? C1 C3 Cl1 120.0(7) 2_566 . ? C2 C3 Cl1 119.4(7) . . ? C4 O3 Tb1 121.5(6) . . ? C5 O4 Tb1 122.3(6) . . ? O3 C4 C6 125.3(9) . 2_676 ? O3 C4 C5 116.1(8) . . ? C6 C4 C5 118.6(8) 2_676 . ? O4 C5 C6 125.3(9) . . ? O4 C5 C4 115.1(7) . . ? C6 C5 C4 119.5(8) . . ? C5 C6 C4 121.9(9) . 2_676 ? C5 C6 Cl2 118.9(7) . . ? C4 C6 Cl2 119.2(7) 2_676 . ? C7 O5 Tb1 121.8(5) . . ? C8 O6 Tb1 119.9(5) . . ? O5 C7 C9 123.0(8) . . ? O5 C7 C8 116.2(8) . . ? C9 C7 C8 120.8(8) . . ? O6 C8 C9 125.2(8) . 2_665 ? O6 C8 C7 115.2(8) . . ? C9 C8 C7 119.6(8) 2_665 . ? C7 C9 C8 119.5(8) . 2_665 ? C7 C9 Cl3 120.2(7) . . ? C8 C9 Cl3 120.2(7) 2_665 . ? O17 O25 O21 79(8) 2_665 2_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.904 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.193 #===END data_cecanabs97 _database_code_CSD 175606 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(chloranilato)dicerium(III) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 Ce2 Cl6 O30' _chemical_formula_weight 1225.41 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 11.376(2) _cell_length_b 16.598(3) _cell_length_c 11.224(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.83(2) _cell_angle_gamma 90.00 _cell_volume 2116.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.7 _cell_measurement_theta_max 15.4 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 2.596 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5931 _exptl_absorpt_correction_T_max 0.8025 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The crystal was sealed in a Lindeman glass capillary tube along with some mother liquor. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 160 _diffrn_standards_decay_% 6 _diffrn_reflns_number 3084 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2513 _reflns_number_gt 2204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 - Software' _computing_cell_refinement 'CAD4 - Software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0537P)^2^+4.1500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2513 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 Ce1 Ce 0.28350(3) 0.0000 0.15605(3) 0.02447(11) Uani 1 2 d S . . Cl1 Cl 0.44135(11) 0.20515(7) -0.18610(12) 0.0463(3) Uani 1 1 d . . . O1 O 0.3453(3) 0.10136(18) 0.0042(3) 0.0327(7) Uani 1 1 d . . . O2 O 0.1856(3) 0.13780(18) 0.1559(3) 0.0364(7) Uani 1 1 d . . . C1 C 0.3050(3) 0.1717(2) -0.0032(4) 0.0272(8) Uani 1 1 d . . . C2 C 0.2121(3) 0.1929(2) 0.0860(4) 0.0285(8) Uani 1 1 d . . . C3 C 0.3379(4) 0.2297(3) -0.0841(4) 0.0317(9) Uani 1 1 d . . . Cl2 Cl 0.5000 0.19069(9) 0.5000 0.0456(4) Uani 1 2 d S . . O3 O 0.3727(3) 0.07901(18) 0.3284(3) 0.0341(7) Uani 1 1 d . . . C4 C 0.4342(3) 0.0462(2) 0.4115(4) 0.0277(8) Uani 1 1 d . . . C5 C 0.5000 0.0870(4) 0.5000 0.0306(12) Uani 1 2 d S . . O4 O 0.5127(4) 0.0000 0.1426(4) 0.0355(10) Uani 1 2 d S . . O5 O 0.1264(5) 0.0000 -0.0130(5) 0.0558(14) Uani 1 2 d S . . O6 O 0.1168(5) 0.0000 0.2914(6) 0.0604(15) Uani 1 2 d S . . O7 O 0.0805(7) 0.1177(5) 0.8239(9) 0.148(3) Uani 1 1 d . . . O8 O 0.2696(13) 0.0000 0.6773(14) 0.100 Uiso 0.580(18) 2 d SP . . O9 O 0.2768(12) 0.2945(9) 0.5939(14) 0.100 Uiso 0.439(12) 1 d P . . O10 O 0.1985(14) 0.1353(10) 0.6269(15) 0.100 Uiso 0.404(12) 1 d P . . O11 O 0.4354(15) 0.3745(12) 0.5840(16) 0.100 Uiso 0.360(12) 1 d P . . O12 O 0.217(2) 0.2448(14) 0.651(2) 0.100 Uiso 0.293(12) 1 d P . . O13 O 0.335(2) 0.3671(14) 0.507(2) 0.100 Uiso 0.284(11) 1 d P . . 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 0.02786(17) 0.01810(16) 0.02732(18) 0.000 0.00005(11) 0.000 Cl1 0.0540(7) 0.0361(6) 0.0510(7) 0.0079(5) 0.0242(6) 0.0142(5) O1 0.0353(14) 0.0222(14) 0.0412(17) 0.0040(13) 0.0085(13) 0.0059(12) O2 0.0449(17) 0.0271(15) 0.0381(17) 0.0087(14) 0.0115(14) 0.0078(13) C1 0.0291(18) 0.0222(19) 0.030(2) 0.0002(16) 0.0023(15) 0.0045(15) C2 0.0309(19) 0.0217(19) 0.033(2) 0.0019(16) -0.0001(16) 0.0037(15) C3 0.035(2) 0.024(2) 0.037(2) -0.0005(17) 0.0078(17) 0.0079(16) Cl2 0.0730(11) 0.0196(7) 0.0435(9) 0.000 -0.0034(8) 0.000 O3 0.0454(16) 0.0225(14) 0.0335(16) 0.0003(12) -0.0070(13) 0.0055(13) C4 0.0332(19) 0.023(2) 0.0274(19) 0.0000(16) 0.0032(15) 0.0015(15) C5 0.039(3) 0.021(3) 0.032(3) 0.000 0.001(2) 0.000 O4 0.030(2) 0.029(2) 0.048(3) 0.000 0.0040(19) 0.000 O5 0.048(3) 0.055(3) 0.063(4) 0.000 -0.017(3) 0.000 O6 0.058(3) 0.057(3) 0.069(4) 0.000 0.028(3) 0.000 O7 0.126(6) 0.098(5) 0.219(10) 0.038(6) -0.013(6) 0.003(5) _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 2.488(5) . ? Ce1 O3 2.510(3) 2 ? Ce1 O3 2.510(3) . ? Ce1 O1 2.519(3) 2 ? Ce1 O1 2.519(3) . ? Ce1 O5 2.541(5) . ? Ce1 O2 2.544(3) . ? Ce1 O2 2.544(3) 2 ? Ce1 O4 2.619(4) . ? Cl1 C3 1.731(4) . ? O1 C1 1.255(5) . ? O2 C2 1.251(5) . ? C1 C3 1.387(6) . ? C1 C2 1.533(6) . ? C2 C3 1.406(6) 7 ? C3 C2 1.406(6) 7 ? Cl2 C5 1.721(6) . ? O3 C4 1.261(5) . ? C4 C5 1.390(5) . ? C4 C4 1.534(8) 2 ? C5 C4 1.390(5) 6_656 ? 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 O3 79.66(15) . 2 ? O6 Ce1 O3 79.66(15) . . ? O3 Ce1 O3 63.00(13) 2 . ? O6 Ce1 O1 131.27(10) . 2 ? O3 Ce1 O1 93.27(10) 2 2 ? O3 Ce1 O1 139.01(10) . 2 ? O6 Ce1 O1 131.27(10) . . ? O3 Ce1 O1 139.02(10) 2 . ? O3 Ce1 O1 93.27(10) . . ? O1 Ce1 O1 83.79(14) 2 . ? O6 Ce1 O5 85.8(2) . . ? O3 Ce1 O5 144.90(9) 2 . ? O3 Ce1 O5 144.90(9) . . ? O1 Ce1 O5 72.80(12) 2 . ? O1 Ce1 O5 72.80(12) . . ? O6 Ce1 O2 69.73(8) . . ? O3 Ce1 O2 129.10(10) 2 . ? O3 Ce1 O2 72.00(10) . . ? O1 Ce1 O2 137.44(10) 2 . ? O1 Ce1 O2 62.34(9) . . ? O5 Ce1 O2 73.01(9) . . ? O6 Ce1 O2 69.73(8) . 2 ? O3 Ce1 O2 72.00(10) 2 2 ? O3 Ce1 O2 129.10(10) . 2 ? O1 Ce1 O2 62.34(9) 2 2 ? O1 Ce1 O2 137.44(10) . 2 ? O5 Ce1 O2 73.01(9) . 2 ? O2 Ce1 O2 128.08(15) . 2 ? O6 Ce1 O4 145.70(19) . . ? O3 Ce1 O4 71.25(12) 2 . ? O3 Ce1 O4 71.25(12) . . ? O1 Ce1 O4 69.48(10) 2 . ? O1 Ce1 O4 69.48(10) . . ? O5 Ce1 O4 128.50(18) . . ? O2 Ce1 O4 115.91(7) . . ? O2 Ce1 O4 115.91(7) 2 . ? C1 O1 Ce1 123.6(3) . . ? C2 O2 Ce1 122.6(3) . . ? O1 C1 C3 125.4(4) . . ? O1 C1 C2 115.5(4) . . ? C3 C1 C2 119.0(3) . . ? O2 C2 C3 124.6(4) . 7 ? O2 C2 C1 115.9(4) . . ? C3 C2 C1 119.5(4) 7 . ? C1 C3 C2 121.5(4) . 7 ? C1 C3 Cl1 118.9(3) . . ? C2 C3 Cl1 119.5(3) 7 . ? C4 O3 Ce1 122.2(3) . . ? O3 C4 C5 125.3(4) . . ? O3 C4 C4 115.6(2) . 2 ? C5 C4 C4 119.1(3) . 2 ? C4 C5 C4 121.7(5) . 6_656 ? C4 C5 Cl2 119.1(3) . . ? C4 C5 Cl2 119.1(3) 6_656 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.907 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.135 #===END data_y2can3abs93 _database_code_CSD 175607 _audit_creation_method SHELXL _chemical_name_systematic ; hexaaquatris(chloranilato)diyttrium(III) hydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H32 Cl6 O28 Y2' _chemical_formula_weight 1086.96 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.324(2) _cell_length_b 9.882(2) _cell_length_c 11.238(2) _cell_angle_alpha 76.91(2) _cell_angle_beta 77.51(2) _cell_angle_gamma 75.08(2) _cell_volume 960.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.7 _cell_measurement_theta_max 15.2 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method ? _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 3.519 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5810 _exptl_absorpt_correction_T_max 0.7185 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 5216 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4393 _reflns_number_observed 3526 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.5080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 4393 _refine_ls_number_parameters 294 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_obs 0.0396 _refine_ls_wR_factor_all 0.0893 _refine_ls_wR_factor_obs 0.0819 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.071 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.069 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Y1 Y 0.23571(4) 0.33931(3) 0.31639(3) 0.01548(9) Uani 1 d . . Cl1 Cl 0.23490(12) -0.21222(10) 0.34103(10) 0.0383(2) Uani 1 d . . O1 O 0.0437(3) 0.2654(2) 0.4765(2) 0.0233(5) Uani 1 d . . O2 O 0.2279(3) 0.0902(2) 0.3416(2) 0.0243(5) Uani 1 d . . C1 C 0.0137(4) 0.1439(3) 0.4918(3) 0.0189(7) Uani 1 d . . C2 C 0.1252(4) 0.0417(3) 0.4138(3) 0.0192(7) Uani 1 d . . C3 C 0.1054(4) -0.0976(3) 0.4286(3) 0.0239(7) Uani 1 d . . Cl2 Cl 0.70693(10) 0.58333(11) 0.24348(8) 0.0312(2) Uani 1 d . . O3 O 0.2475(3) 0.4179(3) 0.5027(2) 0.0217(5) Uani 1 d . . O4 O 0.4196(3) 0.4763(2) 0.2906(2) 0.0207(5) Uani 1 d . . C4 C 0.3642(4) 0.4538(3) 0.5085(3) 0.0179(7) Uani 1 d . . C5 C 0.4651(4) 0.4898(3) 0.3839(3) 0.0173(6) Uani 1 d . . C6 C 0.5939(4) 0.5365(3) 0.3827(3) 0.0192(7) Uani 1 d . . Cl3 Cl 0.18912(12) 0.73902(11) -0.10731(9) 0.0386(3) Uani 1 d . . O5 O 0.2192(3) 0.5067(2) 0.1188(2) 0.0225(5) Uani 1 d . . O6 O 0.0555(3) 0.3161(3) 0.2082(2) 0.0260(6) Uani 1 d . . C7 C 0.1173(4) 0.5119(3) 0.0597(3) 0.0183(7) Uani 1 d . . C8 C 0.0252(4) 0.3973(3) 0.1093(3) 0.0189(7) Uani 1 d . . C9 C 0.0837(4) 0.6112(4) -0.0457(3) 0.0217(7) Uani 1 d . . O7 O 0.0375(3) 0.5514(3) 0.3433(2) 0.0236(5) Uani 1 d D . H71 H -0.0499(25) 0.5438(51) 0.3672(43) 0.052(11) Uiso 1 d D . H72 H 0.0551(54) 0.5999(45) 0.3860(38) 0.052(11) Uiso 1 d D . O8 O 0.4087(3) 0.2331(3) 0.1619(2) 0.0337(6) Uani 1 d D . H81 H 0.4542(56) 0.2753(52) 0.0996(32) 0.068(13) Uiso 1 d D . H82 H 0.4359(61) 0.1494(24) 0.1548(51) 0.068(13) Uiso 1 d D . O9 O 0.4385(3) 0.1871(3) 0.4225(3) 0.0326(6) Uani 1 d D . H91 H 0.5000(53) 0.1227(45) 0.3934(53) 0.082(15) Uiso 1 d D . H92 H 0.4054(67) 0.1414(58) 0.4878(32) 0.082(15) Uiso 1 d D . O10 O 0.5529(4) 0.3187(4) -0.0661(3) 0.0502(9) Uani 1 d D . H101 H 0.6367(35) 0.3354(68) -0.0785(59) 0.090(16) Uiso 1 d D . H102 H 0.5074(63) 0.3918(41) -0.1046(53) 0.090(16) Uiso 1 d D . O11 O 0.3591(6) 0.0548(5) 0.6650(4) 0.0765(14) Uani 1 d D . H111 H 0.4178(58) 0.0619(69) 0.7073(51) 0.073(15) Uiso 1 d D . H112 H 0.2715(28) 0.0776(64) 0.6979(53) 0.073(15) Uiso 1 d D . O12 O 0.5134(7) -0.0574(5) 0.1351(5) 0.090(2) Uani 1 d D . H121 H 0.5905(33) -0.0547(50) 0.0841(35) 0.034(9) Uiso 1 d D . H122 H 0.4384(39) -0.0684(55) 0.1110(47) 0.034(9) Uiso 1 d D . O13 O 0.0605(7) 0.1372(5) 0.8236(5) 0.0862(14) Uani 1 d D . H131 H 0.0166(89) 0.2199(35) 0.8035(77) 0.128(25) Uiso 1 d D . H132 H 0.1394(54) 0.0941(81) 0.8482(79) 0.128(25) Uiso 1 d D . O14 O 0.1771(6) 0.0519(5) 0.0592(5) 0.108(2) Uani 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 0.0189(2) 0.0157(2) 0.01335(15) -0.00035(10) -0.00569(11) -0.00592(12) Cl1 0.0384(6) 0.0226(4) 0.0478(6) -0.0133(4) 0.0137(5) -0.0074(4) O1 0.0297(14) 0.0172(11) 0.0241(12) -0.0046(9) -0.0004(11) -0.0096(10) O2 0.0251(13) 0.0188(12) 0.0267(13) -0.0029(10) 0.0024(11) -0.0078(10) C1 0.022(2) 0.015(2) 0.020(2) -0.0006(12) -0.0074(13) -0.0038(13) C2 0.021(2) 0.018(2) 0.019(2) -0.0005(12) -0.0053(14) -0.0049(13) C3 0.025(2) 0.015(2) 0.028(2) -0.0067(13) 0.0026(15) -0.0024(14) Cl2 0.0268(5) 0.0526(6) 0.0169(4) -0.0050(4) -0.0005(3) -0.0175(4) O3 0.0198(12) 0.0314(13) 0.0181(11) -0.0057(10) -0.0050(9) -0.0102(10) O4 0.0265(13) 0.0246(12) 0.0153(11) -0.0020(9) -0.0087(10) -0.0104(10) C4 0.019(2) 0.0154(15) 0.020(2) -0.0034(12) -0.0070(13) -0.0013(13) C5 0.019(2) 0.0145(15) 0.018(2) -0.0038(12) -0.0061(13) -0.0009(13) C6 0.020(2) 0.026(2) 0.0122(14) -0.0045(12) -0.0003(13) -0.0067(14) Cl3 0.0481(6) 0.0382(5) 0.0374(5) 0.0138(4) -0.0227(5) -0.0281(5) O5 0.0257(13) 0.0267(13) 0.0188(12) 0.0007(10) -0.0111(10) -0.0102(11) O6 0.0330(14) 0.0283(13) 0.0209(12) 0.0072(10) -0.0157(11) -0.0150(11) C7 0.020(2) 0.020(2) 0.017(2) -0.0055(12) -0.0030(13) -0.0042(13) C8 0.022(2) 0.020(2) 0.015(2) -0.0033(12) -0.0079(13) -0.0019(13) C9 0.028(2) 0.021(2) 0.018(2) 0.0020(13) -0.0073(14) -0.0108(15) O7 0.0222(13) 0.0229(13) 0.0263(13) -0.0062(10) -0.0046(11) -0.0040(11) O8 0.043(2) 0.0250(14) 0.0249(14) -0.0030(11) 0.0080(13) -0.0068(13) O9 0.038(2) 0.0252(14) 0.0319(15) -0.0015(11) -0.0151(13) 0.0017(12) O10 0.043(2) 0.076(2) 0.031(2) 0.019(2) -0.0138(15) -0.030(2) O11 0.102(4) 0.059(3) 0.042(2) -0.006(2) -0.003(2) 0.019(3) O12 0.126(5) 0.063(3) 0.062(3) -0.007(2) 0.001(3) -0.005(3) O13 0.112(4) 0.073(3) 0.075(3) -0.013(3) -0.033(3) -0.010(3) O14 0.122(4) 0.081(3) 0.138(5) -0.039(3) -0.080(4) 0.013(3) _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 O8 2.337(3) . ? Y1 O6 2.359(2) . ? Y1 O4 2.379(2) . ? Y1 O1 2.379(2) . ? Y1 O3 2.425(2) . ? Y1 O2 2.432(2) . ? Y1 O7 2.440(3) . ? Y1 O9 2.441(3) . ? Y1 O5 2.459(2) . ? Cl1 C3 1.731(3) . ? O1 C1 1.268(4) . ? O2 C2 1.237(4) . ? C1 C3 1.374(5) 2_556 ? C1 C2 1.528(5) . ? C2 C3 1.404(4) . ? C3 C1 1.375(5) 2_556 ? Cl2 C6 1.727(3) . ? O3 C4 1.247(4) . ? O4 C5 1.258(4) . ? C4 C6 1.391(4) 2_666 ? C4 C5 1.533(4) . ? C5 C6 1.390(5) . ? C6 C4 1.391(4) 2_666 ? Cl3 C9 1.729(3) . ? O5 C7 1.255(4) . ? O6 C8 1.255(4) . ? C7 C9 1.393(4) . ? C7 C8 1.529(5) . ? C8 C9 1.390(5) 2_565 ? C9 C8 1.390(5) 2_565 ? 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 O8 Y1 O6 83.88(10) . . ? O8 Y1 O4 82.37(9) . . ? O6 Y1 O4 138.93(8) . . ? O8 Y1 O1 134.62(9) . . ? O6 Y1 O1 76.24(8) . . ? O4 Y1 O1 137.12(8) . . ? O8 Y1 O3 136.29(10) . . ? O6 Y1 O3 139.72(9) . . ? O4 Y1 O3 65.70(8) . . ? O1 Y1 O3 71.53(8) . . ? O8 Y1 O2 69.39(9) . . ? O6 Y1 O2 69.67(8) . . ? O4 Y1 O2 137.92(8) . . ? O1 Y1 O2 65.52(8) . . ? O3 Y1 O2 115.68(8) . . ? O8 Y1 O7 141.04(9) . . ? O6 Y1 O7 77.52(9) . . ? O4 Y1 O7 89.56(8) . . ? O1 Y1 O7 73.26(8) . . ? O3 Y1 O7 70.60(8) . . ? O2 Y1 O7 131.87(8) . . ? O8 Y1 O9 75.41(10) . . ? O6 Y1 O9 138.64(9) . . ? O4 Y1 O9 73.55(9) . . ? O1 Y1 O9 93.36(10) . . ? O3 Y1 O9 67.63(9) . . ? O2 Y1 O9 69.62(9) . . ? O7 Y1 O9 138.23(9) . . ? O8 Y1 O5 72.16(9) . . ? O6 Y1 O5 65.77(8) . . ? O4 Y1 O5 73.19(8) . . ? O1 Y1 O5 130.77(8) . . ? O3 Y1 O5 121.27(8) . . ? O2 Y1 O5 122.96(8) . . ? O7 Y1 O5 69.02(8) . . ? O9 Y1 O5 135.86(9) . . ? C1 O1 Y1 122.0(2) . . ? C2 O2 Y1 120.8(2) . . ? O1 C1 C3 126.4(3) . 2_556 ? O1 C1 C2 114.8(3) . . ? C3 C1 C2 118.8(3) 2_556 . ? O2 C2 C3 125.0(3) . . ? O2 C2 C1 116.0(3) . . ? C3 C2 C1 119.0(3) . . ? C1 C3 C2 122.2(3) 2_556 . ? C1 C3 Cl1 119.7(3) 2_556 . ? C2 C3 Cl1 118.1(3) . . ? C4 O3 Y1 118.3(2) . . ? C5 O4 Y1 119.8(2) . . ? O3 C4 C6 125.0(3) . 2_666 ? O3 C4 C5 115.4(3) . . ? C6 C4 C5 119.6(3) 2_666 . ? O4 C5 C6 126.0(3) . . ? O4 C5 C4 115.3(3) . . ? C6 C5 C4 118.6(3) . . ? C5 C6 C4 121.7(3) . 2_666 ? C5 C6 Cl2 119.8(2) . . ? C4 C6 Cl2 118.4(3) 2_666 . ? C7 O5 Y1 119.1(2) . . ? C8 O6 Y1 123.3(2) . . ? O5 C7 C9 125.6(3) . . ? O5 C7 C8 115.9(3) . . ? C9 C7 C8 118.5(3) . . ? O6 C8 C9 124.5(3) . 2_565 ? O6 C8 C7 115.4(3) . . ? C9 C8 C7 120.1(3) 2_565 . ? C8 C9 C7 121.3(3) 2_565 . ? C8 C9 Cl3 118.6(2) 2_565 . ? C7 C9 Cl3 119.9(3) . . ? _refine_diff_density_max 0.643 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.096 #===END data_gdcanabs93 _database_code_CSD 175608 _audit_creation_method SHELXL _chemical_name_systematic ; hexaaquatris(chloranilato)digadolinium(III) hydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H32 Cl6 Gd2 O28' _chemical_formula_weight 1223.65 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.381(1) _cell_length_b 9.941(1) _cell_length_c 11.311(1) _cell_angle_alpha 76.90 (1) _cell_angle_beta 77.15(1) _cell_angle_gamma 74.79(1) _cell_volume 976.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.6 _cell_measurement_theta_max 17.3 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 3.872 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6173 _exptl_absorpt_correction_T_max 0.9165 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4318 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3567 _reflns_number_observed 3202 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0555P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 3567 _refine_ls_number_parameters 289 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_obs 0.0235 _refine_ls_wR_factor_all 0.0586 _refine_ls_wR_factor_obs 0.0559 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.094 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Gd Gd 0.23659(2) 0.33894(2) 0.31586(2) 0.01598(7) Uani 1 d . . O1 O 0.2281(3) 0.0884(3) 0.3422(3) 0.0261(6) Uani 1 d . . O2 O 0.0424(3) 0.2639(3) 0.4777(3) 0.0262(6) Uani 1 d . . C1 C 0.1257(4) 0.0405(4) 0.4142(3) 0.0199(8) Uani 1 d . . C2 C 0.0139(5) 0.1427(4) 0.4919(3) 0.0200(8) Uani 1 d . . C3 C 0.1052(5) -0.0976(4) 0.4281(4) 0.0254(9) Uani 1 d . . Cl1 Cl 0.23332(14) -0.21178(12) 0.34073(12) 0.0412(3) Uani 1 d . . O3 O 0.2179(3) 0.5056(3) 0.1179(2) 0.0234(6) Uani 1 d . . O4 O 0.0559(3) 0.3155(3) 0.2057(3) 0.0283(7) Uani 1 d . . C4 C 0.1173(4) 0.5111(4) 0.0592(3) 0.0198(8) Uani 1 d . . C5 C 0.0249(5) 0.3978(4) 0.1079(3) 0.0210(8) Uani 1 d . . C6 C -0.0837(5) 0.3904(4) 0.0452(4) 0.0233(9) Uani 1 d . . Cl2 Cl -0.18851(15) 0.26309(13) 0.10614(11) 0.0418(3) Uani 1 d . . O5 O 0.2485(3) 0.4189(3) 0.5026(2) 0.0230(6) Uani 1 d . . O6 O 0.4217(3) 0.4778(3) 0.2916(2) 0.0219(6) Uani 1 d . . C7 C 0.3651(4) 0.4554(4) 0.5076(4) 0.0183(8) Uani 1 d . . C8 C 0.4648(4) 0.4912(4) 0.3848(3) 0.0177(8) Uani 1 d . . C9 C 0.4068(4) 0.4636(4) 0.6166(3) 0.0206(8) Uani 1 d . . Cl3 Cl 0.29423(12) 0.41658(13) 0.75523(9) 0.0328(2) Uani 1 d . . O7 O 0.0350(4) 0.5540(3) 0.3437(3) 0.0254(6) Uani 1 d D . H71 H -0.0427(41) 0.5396(58) 0.3710(49) 0.044(17) Uiso 1 d D . H72 H 0.0439(74) 0.5824(63) 0.3989(42) 0.060(20) Uiso 1 d D . O8 O 0.4127(4) 0.2298(4) 0.1597(3) 0.0369(8) Uani 1 d D . H81 H 0.4404(61) 0.2699(52) 0.0956(33) 0.044(16) Uiso 1 d D . H82 H 0.4546(102) 0.1540(47) 0.1780(87) 0.139(41) Uiso 1 d D . O9 O 0.4427(5) 0.1852(4) 0.4220(3) 0.0359(8) Uani 1 d D . H91 H 0.4978(74) 0.1286(64) 0.3878(64) 0.090(28) Uiso 1 d D . H92 H 0.4151(88) 0.1472(74) 0.4857(39) 0.090(29) Uiso 1 d D . O10 O 0.4440(4) 0.6779(4) 0.0673(3) 0.0502(10) Uani 1 d . . O11 O 0.3635(6) 0.0579(4) 0.6673(4) 0.082(2) Uani 1 d . . O12A O 0.4803(22) 0.0588(7) 0.8646(7) 0.068(4) Uani 0.80(4) d P . O12B O 0.5575(52) 0.0671(28) 0.8875(34) 0.053(11) Uani 0.20(4) d P . O13 O 0.0656(7) 0.1379(6) 0.8223(5) 0.091(2) Uani 1 d . . O14A O 0.2059(69) 0.0632(84) 0.0376(53) 0.079(12) Uani 0.37(18) d P . O14B O 0.1549(107) 0.0461(28) 0.0757(85) 0.099(15) Uani 0.63(18) d P . 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 Gd 0.01784(11) 0.01674(10) 0.01543(10) -0.00151(6) -0.00492(7) -0.00691(7) O1 0.026(2) 0.0205(14) 0.031(2) -0.0056(12) 0.0043(13) -0.0103(13) O2 0.033(2) 0.0188(13) 0.0276(15) -0.0049(11) 0.0039(13) -0.0147(13) C1 0.019(2) 0.021(2) 0.021(2) -0.0002(15) -0.004(2) -0.008(2) C2 0.023(2) 0.017(2) 0.022(2) -0.0019(15) -0.005(2) -0.008(2) C3 0.024(2) 0.020(2) 0.031(2) -0.006(2) 0.003(2) -0.008(2) Cl1 0.0393(7) 0.0248(5) 0.0536(7) -0.0172(5) 0.0173(6) -0.0098(5) O3 0.023(2) 0.0293(15) 0.0221(14) -0.0019(11) -0.0098(12) -0.0113(13) O4 0.034(2) 0.031(2) 0.0244(15) 0.0082(12) -0.0153(13) -0.0166(14) C4 0.019(2) 0.023(2) 0.018(2) -0.0087(15) -0.002(2) -0.002(2) C5 0.021(2) 0.022(2) 0.019(2) -0.0035(15) -0.004(2) -0.004(2) C6 0.024(2) 0.025(2) 0.024(2) -0.002(2) -0.007(2) -0.010(2) Cl2 0.0493(8) 0.0425(6) 0.0428(6) 0.0142(5) -0.0237(6) -0.0315(6) O5 0.0190(15) 0.033(2) 0.0215(14) -0.0070(12) -0.0033(12) -0.0113(12) O6 0.024(2) 0.0270(14) 0.0193(13) -0.0025(11) -0.0078(12) -0.0124(12) C7 0.016(2) 0.017(2) 0.024(2) -0.0057(15) -0.005(2) -0.004(2) C8 0.016(2) 0.019(2) 0.019(2) -0.0054(14) -0.006(2) -0.004(2) C9 0.018(2) 0.027(2) 0.017(2) -0.005(2) -0.002(2) -0.006(2) Cl3 0.0271(6) 0.0557(7) 0.0196(5) -0.0066(4) 0.0002(4) -0.0197(5) O7 0.022(2) 0.027(2) 0.028(2) -0.0061(13) -0.0054(14) -0.0053(14) O8 0.043(2) 0.030(2) 0.027(2) -0.0022(14) 0.011(2) -0.008(2) O9 0.044(2) 0.028(2) 0.035(2) -0.003(2) -0.017(2) 0.000(2) O10 0.042(2) 0.075(3) 0.032(2) 0.014(2) -0.007(2) -0.030(2) O11 0.121(4) 0.051(3) 0.048(2) -0.006(2) -0.002(3) 0.014(3) O12A 0.092(10) 0.042(3) 0.066(4) -0.006(3) -0.016(4) -0.008(4) O12B 0.042(19) 0.080(16) 0.042(15) -0.018(10) 0.017(11) -0.036(13) O13 0.113(5) 0.085(4) 0.079(3) -0.015(3) -0.026(3) -0.022(3) O14A 0.049(19) 0.114(22) 0.078(20) -0.050(15) -0.016(15) 0.005(13) O14B 0.098(28) 0.075(8) 0.135(27) -0.028(12) -0.064(26) 0.005(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 Gd O8 2.378(3) . ? Gd O4 2.400(3) . ? Gd O2 2.415(3) . ? Gd O6 2.423(3) . ? Gd O5 2.453(3) . ? Gd O1 2.461(3) . ? Gd O3 2.476(3) . ? Gd O7 2.483(3) . ? Gd O9 2.484(3) . ? O1 C1 1.236(5) . ? O2 C2 1.269(5) . ? C1 C3 1.405(5) . ? C1 C2 1.530(5) . ? C2 C3 1.378(6) 2_556 ? C3 C2 1.378(6) 2_556 ? C3 Cl1 1.725(4) . ? O3 C4 1.252(5) . ? O4 C5 1.259(5) . ? C4 C6 1.390(5) 2_565 ? C4 C5 1.531(5) . ? C5 C6 1.389(6) . ? C6 C4 1.390(5) 2_565 ? C6 Cl2 1.732(4) . ? O5 C7 1.256(5) . ? O6 C8 1.255(5) . ? C7 C9 1.399(5) . ? C7 C8 1.518(5) . ? C8 C9 1.387(5) 2_666 ? C9 C8 1.387(5) 2_666 ? C9 Cl3 1.727(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 O8 Gd O4 83.53(12) . . ? O8 Gd O2 134.14(10) . . ? O4 Gd O2 76.51(10) . . ? O8 Gd O6 83.09(11) . . ? O4 Gd O6 139.11(9) . . ? O2 Gd O6 136.69(9) . . ? O8 Gd O5 136.07(12) . . ? O4 Gd O5 140.31(10) . . ? O2 Gd O5 72.01(9) . . ? O6 Gd O5 64.77(9) . . ? O8 Gd O1 69.48(11) . . ? O4 Gd O1 69.64(10) . . ? O2 Gd O1 64.95(9) . . ? O6 Gd O1 138.33(10) . . ? O5 Gd O1 115.71(9) . . ? O8 Gd O3 72.51(11) . . ? O4 Gd O3 64.92(9) . . ? O2 Gd O3 130.32(10) . . ? O6 Gd O3 74.22(9) . . ? O5 Gd O3 121.44(9) . . ? O1 Gd O3 122.74(9) . . ? O8 Gd O7 141.31(11) . . ? O4 Gd O7 77.75(11) . . ? O2 Gd O7 73.43(10) . . ? O6 Gd O7 89.31(10) . . ? O5 Gd O7 70.61(10) . . ? O1 Gd O7 131.57(10) . . ? O3 Gd O7 68.92(10) . . ? O8 Gd O9 75.12(13) . . ? O4 Gd O9 138.70(11) . . ? O2 Gd O9 93.53(12) . . ? O6 Gd O9 73.21(11) . . ? O5 Gd O9 67.64(11) . . ? O1 Gd O9 69.86(11) . . ? O3 Gd O9 136.13(12) . . ? O7 Gd O9 138.25(11) . . ? C1 O1 Gd 121.1(2) . . ? C2 O2 Gd 121.6(2) . . ? O1 C1 C3 125.1(4) . . ? O1 C1 C2 116.0(3) . . ? C3 C1 C2 118.9(3) . . ? O2 C2 C3 125.4(4) . 2_556 ? O2 C2 C1 115.4(3) . . ? C3 C2 C1 119.2(3) 2_556 . ? C2 C3 C1 121.9(4) 2_556 . ? C2 C3 Cl1 119.8(3) 2_556 . ? C1 C3 Cl1 118.2(3) . . ? C4 O3 Gd 119.9(2) . . ? C5 O4 Gd 123.3(3) . . ? O3 C4 C6 125.9(4) . 2_565 ? O3 C4 C5 116.2(3) . . ? C6 C4 C5 117.9(4) 2_565 . ? O4 C5 C6 124.5(4) . . ? O4 C5 C4 115.1(3) . . ? C6 C5 C4 120.4(3) . . ? C5 C6 C4 121.6(4) . 2_565 ? C5 C6 Cl2 118.6(3) . . ? C4 C6 Cl2 119.6(3) 2_565 . ? C7 O5 Gd 118.5(2) . . ? C8 O6 Gd 119.7(2) . . ? O5 C7 C9 124.6(4) . . ? O5 C7 C8 115.8(3) . . ? C9 C7 C8 119.7(3) . . ? O6 C8 C9 125.4(4) . 2_666 ? O6 C8 C7 115.9(3) . . ? C9 C8 C7 118.8(3) 2_666 . ? C8 C9 C7 121.5(4) 2_666 . ? C8 C9 Cl3 119.9(3) 2_666 . ? C7 C9 Cl3 118.6(3) . . ? _refine_diff_density_max 0.764 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.107 #===END data_lucanabs97 _database_code_CSD 175609 _audit_creation_method SHELXL-97 _chemical_name_systematic ; octaaquatris(chloranilato)dilutetium(III) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl6 Lu2 O24' _chemical_formula_weight 1187.01 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 18.956(8) _cell_length_b 16.680(5) _cell_length_c 10.970(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.97(3) _cell_angle_gamma 90.00 _cell_volume 3239(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.1 _cell_measurement_theta_max 13.3 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.014 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 6.653 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.6196 _exptl_absorpt_correction_T_max 0.9099 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The crystal was glued on to the end of a thin glass fibre. The crystal was directly exposed to the atmosphere throughout the data collection. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3 _diffrn_reflns_number 3647 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.1403 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2915 _reflns_number_gt 1678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 - Software' _computing_cell_refinement 'CAD4 - Software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1190P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2915 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1557 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2303 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Lu1 Lu 0.11592(8) 0.5000 -0.18417(15) 0.0200(4) Uani 1 2 d S . . Cl1 Cl 0.3390(3) 0.3107(4) -0.1821(7) 0.0315(15) Uani 1 1 d . . . Cl2 Cl 0.0246(4) 0.7958(4) -0.1540(9) 0.044(2) Uani 1 1 d . . . O1 O 0.2033(8) 0.4118(9) -0.2102(18) 0.025(4) Uani 1 1 d . . . O2 O 0.0806(9) 0.6296(9) -0.1817(17) 0.029(4) Uani 1 1 d . . . C1 C 0.2006(13) 0.3374(14) -0.188(2) 0.021(5) Uiso 1 1 d . . . C2 C 0.1227(14) 0.6865(16) -0.175(3) 0.029(6) Uiso 1 1 d . . . C3 C 0.1088(14) 0.7658(14) -0.167(3) 0.027(6) Uiso 1 1 d . . . C4 C 0.1644(13) 0.1727(14) -0.152(2) 0.024(5) Uiso 1 1 d . . . C5 C 0.2428(13) 0.1977(13) -0.159(2) 0.018(5) Uiso 1 1 d . . . C6 C 0.2539(15) 0.2797(15) -0.173(3) 0.031(6) Uiso 1 1 d . . . O3 O 0.1555(10) 0.1017(11) -0.1360(19) 0.036(5) Uani 1 1 d . . . O4 O 0.2849(10) 0.1447(9) -0.161(2) 0.041(5) Uani 1 1 d . . . O5 O 0.0969(15) 0.5000 -0.408(3) 0.042(7) Uani 1 2 d S . . O6 O -0.0215(13) 0.5000 -0.293(3) 0.030(6) Uani 1 2 d S . . O7 O 0.0720(12) 0.5000 -0.014(3) 0.031(6) Uani 1 2 d S . . O8 O 0.2189(16) 0.5000 0.007(2) 0.039(7) Uani 1 2 d S . . Lu2 Lu 0.31037(8) 0.5000 0.50321(15) 0.0208(4) Uani 1 2 d S . . Cl3 Cl 0.4142(3) 0.2012(4) 0.5111(7) 0.0321(16) Uani 1 1 d . . . O9 O 0.2150(9) 0.4061(8) 0.4989(15) 0.021(4) Uani 1 1 d . . . O10 O 0.3462(9) 0.3649(9) 0.5002(19) 0.031(4) Uani 1 1 d . . . C7 C 0.2262(12) 0.3329(13) 0.494(2) 0.019(5) Uiso 1 1 d . . . C8 C 0.3063(10) 0.3081(11) 0.4996(19) 0.006(4) Uiso 1 1 d . . . C9 C 0.3255(12) 0.2265(12) 0.502(2) 0.016(5) Uiso 1 1 d . . . O11 O 0.4310(16) 0.5220(19) 0.643(3) 0.033(12) Uani 0.50 1 d P . . O12 O 0.3081(12) 0.5000 0.712(2) 0.023(5) Uani 1 2 d S . . O13 O 0.3845(15) 0.5000 0.374(3) 0.036(6) Uani 1 2 d S . . O14 O 0.2296(15) 0.5000 0.294(2) 0.033(6) Uani 1 2 d S . . O15 O 0.531(2) 0.5000 0.899(4) 0.091(13) Uiso 1 2 d S . . O16 O 0.5000 0.6152(17) 0.5000 0.046(8) Uani 1 2 d S . . O17 O 0.4307(9) 0.1186(11) -0.157(2) 0.045(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.0169(8) 0.0112(7) 0.0336(10) 0.000 0.0110(7) 0.000 Cl1 0.023(3) 0.030(3) 0.046(4) 0.001(3) 0.018(3) 0.000(3) Cl2 0.024(3) 0.026(3) 0.085(6) -0.006(4) 0.023(4) 0.007(3) O1 0.015(7) 0.018(8) 0.051(11) 0.004(8) 0.022(8) -0.003(6) O2 0.024(9) 0.018(8) 0.035(11) -0.013(7) -0.001(8) -0.012(7) O3 0.031(10) 0.028(10) 0.055(13) 0.008(9) 0.025(10) -0.003(8) O4 0.025(8) 0.023(8) 0.085(14) 0.006(11) 0.033(10) 0.013(9) O5 0.040(16) 0.034(14) 0.037(17) 0.000 -0.004(13) 0.000 O6 0.018(12) 0.023(12) 0.051(17) 0.000 0.015(12) 0.000 O7 0.011(11) 0.044(15) 0.044(17) 0.000 0.020(12) 0.000 O8 0.059(19) 0.025(13) 0.024(15) 0.000 0.006(14) 0.000 Lu2 0.0193(8) 0.0106(7) 0.0349(10) 0.000 0.0128(7) 0.000 Cl3 0.018(3) 0.023(3) 0.061(5) -0.001(3) 0.021(3) 0.002(2) O9 0.023(8) 0.013(8) 0.029(10) 0.002(7) 0.013(7) -0.006(7) O10 0.031(10) 0.023(8) 0.053(12) 0.009(9) 0.032(9) 0.007(8) O11 0.012(13) 0.05(3) 0.029(18) 0.008(15) -0.006(13) 0.002(13) O12 0.012(11) 0.027(12) 0.031(14) 0.000 0.009(11) 0.000 O13 0.049(17) 0.026(13) 0.035(16) 0.000 0.018(14) 0.000 O14 0.044(15) 0.024(12) 0.019(13) 0.000 -0.003(12) 0.000 O16 0.015(12) 0.049(17) 0.07(2) 0.000 0.015(14) 0.000 O17 0.023(10) 0.026(10) 0.078(16) 0.013(10) 0.007(10) 0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O2 2.266(15) 2_565 ? Lu1 O2 2.266(15) . ? Lu1 O8 2.30(3) . ? Lu1 O7 2.30(2) . ? Lu1 O1 2.308(15) . ? Lu1 O1 2.308(15) 2_565 ? Lu1 O5 2.35(3) . ? Lu1 O6 2.45(2) . ? Cl1 C6 1.73(3) . ? Cl2 C3 1.73(2) . ? O1 C1 1.27(3) . ? O2 C2 1.23(3) . ? C1 C6 1.36(3) . ? C1 C2 1.58(3) 2_565 ? C2 C3 1.36(4) . ? C2 C1 1.58(3) 2_565 ? C3 C4 1.44(3) 2_565 ? C4 O3 1.22(3) . ? C4 C3 1.44(3) 2_565 ? C4 C5 1.57(3) . ? C5 O4 1.20(3) . ? C5 C6 1.40(3) . ? Lu2 O14 2.26(2) . ? Lu2 O11 2.28(3) . ? Lu2 O11 2.28(3) 2_565 ? Lu2 O12 2.31(2) . ? Lu2 O13 2.33(3) . ? Lu2 O10 2.357(15) 2_565 ? Lu2 O10 2.357(15) . ? Lu2 O9 2.379(14) 2_565 ? Lu2 O9 2.380(14) . ? Cl3 C9 1.70(2) . ? O9 C7 1.24(3) . ? O10 C8 1.21(2) . ? C7 C9 1.41(3) 7_556 ? C7 C8 1.55(3) . ? C8 C9 1.41(3) . ? C9 C7 1.41(3) 7_556 ? 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 O2 Lu1 O2 145.1(8) 2_565 . ? O2 Lu1 O8 98.4(4) 2_565 . ? O2 Lu1 O8 98.5(4) . . ? O2 Lu1 O7 78.2(5) 2_565 . ? O2 Lu1 O7 78.2(5) . . ? O8 Lu1 O7 72.3(9) . . ? O2 Lu1 O1 67.8(6) 2_565 . ? O2 Lu1 O1 146.9(6) . . ? O8 Lu1 O1 72.6(7) . . ? O7 Lu1 O1 125.8(5) . . ? O2 Lu1 O1 146.9(6) 2_565 2_565 ? O2 Lu1 O1 67.8(6) . 2_565 ? O8 Lu1 O1 72.6(7) . 2_565 ? O7 Lu1 O1 125.8(5) . 2_565 ? O1 Lu1 O1 79.2(7) . 2_565 ? O2 Lu1 O5 94.4(5) 2_565 . ? O2 Lu1 O5 94.4(5) . . ? O8 Lu1 O5 135.7(10) . . ? O7 Lu1 O5 152.0(9) . . ? O1 Lu1 O5 73.7(7) . . ? O1 Lu1 O5 73.7(7) 2_565 . ? O2 Lu1 O6 74.8(4) 2_565 . ? O2 Lu1 O6 74.8(4) . . ? O8 Lu1 O6 148.5(10) . . ? O7 Lu1 O6 76.2(8) . . ? O1 Lu1 O6 128.8(5) . . ? O1 Lu1 O6 128.8(5) 2_565 . ? O5 Lu1 O6 75.7(9) . . ? C1 O1 Lu1 121.4(14) . . ? C2 O2 Lu1 123.4(16) . . ? O1 C1 C6 130(2) . . ? O1 C1 C2 111(2) . 2_565 ? C6 C1 C2 119(2) . 2_565 ? O2 C2 C3 128(2) . . ? O2 C2 C1 114(2) . 2_565 ? C3 C2 C1 117(2) . 2_565 ? C2 C3 C4 123(2) . 2_565 ? C2 C3 Cl2 119.7(19) . . ? C4 C3 Cl2 116.5(18) 2_565 . ? O3 C4 C3 125(2) . 2_565 ? O3 C4 C5 117(2) . . ? C3 C4 C5 118(2) 2_565 . ? O4 C5 C6 126(2) . . ? O4 C5 C4 117(2) . . ? C6 C5 C4 117(2) . . ? C1 C6 C5 125(2) . . ? C1 C6 Cl1 116.6(19) . . ? C5 C6 Cl1 118.5(19) . . ? O14 Lu2 O11 146.7(11) . . ? O14 Lu2 O11 146.7(11) . 2_565 ? O11 Lu2 O11 18.5(16) . 2_565 ? O14 Lu2 O12 139.7(9) . . ? O11 Lu2 O12 72.6(10) . . ? O11 Lu2 O12 72.6(10) 2_565 . ? O14 Lu2 O13 73.6(10) . . ? O11 Lu2 O13 74.5(11) . . ? O11 Lu2 O13 74.5(11) 2_565 . ? O12 Lu2 O13 146.7(8) . . ? O14 Lu2 O10 94.6(5) . 2_565 ? O11 Lu2 O10 68.4(9) . 2_565 ? O11 Lu2 O10 86.5(9) 2_565 2_565 ? O12 Lu2 O10 97.0(5) . 2_565 ? O13 Lu2 O10 75.6(4) . 2_565 ? O14 Lu2 O10 94.6(5) . . ? O11 Lu2 O10 86.5(9) . . ? O11 Lu2 O10 68.4(9) 2_565 . ? O12 Lu2 O10 97.0(5) . . ? O13 Lu2 O10 75.6(4) . . ? O10 Lu2 O10 145.9(8) 2_565 . ? O14 Lu2 O9 75.3(6) . 2_565 ? O11 Lu2 O9 118.6(9) . 2_565 ? O11 Lu2 O9 133.6(9) 2_565 2_565 ? O12 Lu2 O9 74.7(5) . 2_565 ? O13 Lu2 O9 127.4(5) . 2_565 ? O10 Lu2 O9 65.8(5) 2_565 2_565 ? O10 Lu2 O9 148.2(5) . 2_565 ? O14 Lu2 O9 75.3(7) . . ? O11 Lu2 O9 133.6(9) . . ? O11 Lu2 O9 118.6(9) 2_565 . ? O12 Lu2 O9 74.7(5) . . ? O13 Lu2 O9 127.4(5) . . ? O10 Lu2 O9 148.2(5) 2_565 . ? O10 Lu2 O9 65.8(5) . . ? O9 Lu2 O9 82.4(7) 2_565 . ? C7 O9 Lu2 120.6(14) . . ? C8 O10 Lu2 124.5(13) . . ? O9 C7 C9 124(2) . 7_556 ? O9 C7 C8 116.0(19) . . ? C9 C7 C8 119.6(19) 7_556 . ? O10 C8 C9 126.8(18) . . ? O10 C8 C7 113.0(17) . . ? C9 C8 C7 120.2(17) . . ? C7 C9 C8 120(2) 7_556 . ? C7 C9 Cl3 120.5(17) 7_556 . ? C8 C9 Cl3 119.1(16) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.910 _refine_diff_density_min -3.714 _refine_diff_density_rms 0.489 #===END data_sccanlabs97 _database_code_CSD 175610 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaaquatris(cholranilato)discandium(III) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cl6 O28 Sc2' _chemical_formula_weight 999.06 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 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' _cell_length_a 9.0560(10) _cell_length_b 19.258(2) _cell_length_c 21.842(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.750(9) _cell_angle_gamma 90.00 _cell_volume 3782.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.6 _cell_measurement_theta_max 17.0 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8809 _exptl_absorpt_correction_T_max 0.9753 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2908 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 22.48 _reflns_number_total 2711 _reflns_number_gt 2030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0772P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(11) _refine_ls_number_reflns 2711 _refine_ls_number_parameters 347 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _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 Sc1 Sc 0.5617(3) 0.18128(14) 0.94906(13) 0.0234(7) Uani 1 1 d . . . Sc2 Sc -0.1354(3) -0.00796(14) 1.10258(12) 0.0225(7) Uani 1 1 d . . . Cl1 Cl 0.9697(4) 0.2975(2) 0.83731(18) 0.0439(12) Uani 1 1 d . . . Cl2 Cl 1.0041(4) 0.2137(2) 1.11893(17) 0.0362(10) Uani 1 1 d . . . Cl3 Cl 0.0163(4) 0.0905(2) 0.89915(18) 0.0396(11) Uani 1 1 d . . . Cl4 Cl 0.4144(4) 0.0798(2) 1.15899(18) 0.0392(11) Uani 1 1 d . . . Cl5 Cl -0.5709(4) -0.0411(2) 0.92351(17) 0.0385(10) Uani 1 1 d . . . Cl6 Cl -0.5504(4) -0.1289(2) 1.20392(17) 0.0388(10) Uani 1 1 d . . . O1 O 0.7507(10) 0.1948(5) 1.0182(5) 0.029(3) Uani 1 1 d . . . O2 O 0.7366(10) 0.2317(5) 0.9059(4) 0.027(2) Uani 1 1 d . . . O3 O 1.2207(10) 0.3214(6) 0.9376(5) 0.033(3) Uani 1 1 d . . . O4 O 1.2288(9) 0.2891(5) 1.0576(5) 0.033(3) Uani 1 1 d . . . O5 O 0.3269(9) 0.1489(5) 0.9352(4) 0.029(2) Uani 1 1 d . . . O6 O 0.4944(9) 0.1349(5) 1.0371(4) 0.028(2) Uani 1 1 d . . . O7 O 0.1001(10) 0.0260(5) 1.1235(5) 0.032(3) Uani 1 1 d . . . O8 O -0.0621(10) 0.0351(5) 1.0207(4) 0.032(3) Uani 1 1 d . . . O9 O -0.3117(9) -0.0602(5) 1.1412(4) 0.029(2) Uani 1 1 d . . . O10 O -0.3208(9) -0.0182(5) 1.0292(4) 0.023(2) Uani 1 1 d . . . O11 O -0.8006(10) -0.1163(5) 0.9826(5) 0.034(3) Uani 1 1 d . . . O12 O -0.7955(10) -0.1514(6) 1.1022(5) 0.034(3) Uani 1 1 d . . . C1 C 0.8660(15) 0.2244(7) 1.0042(6) 0.020(3) Uiso 1 1 d . . . C2 C 0.8592(14) 0.2459(7) 0.9361(6) 0.019(3) Uiso 1 1 d . . . C3 C 0.9793(15) 0.2768(7) 0.9148(6) 0.024(3) Uiso 1 1 d . . . C4 C 1.1074(16) 0.2936(8) 0.9548(7) 0.022(3) Uiso 1 1 d . . . C5 C 1.1152(17) 0.2727(8) 1.0235(7) 0.032(4) Uiso 1 1 d . . . C6 C 0.9921(16) 0.2390(8) 1.0429(7) 0.028(4) Uiso 1 1 d . . . C7 C 0.2662(14) 0.1165(7) 0.9773(6) 0.021(3) Uiso 1 1 d . . . C8 C 0.3628(16) 0.1107(7) 1.0382(6) 0.024(3) Uiso 1 1 d . . . C9 C 0.3079(16) 0.0822(7) 1.0881(7) 0.026(4) Uiso 1 1 d . . . C10 C 0.1639(14) 0.0545(7) 1.0826(6) 0.018(3) Uiso 1 1 d . . . C11 C 0.0683(15) 0.0593(7) 1.0199(6) 0.022(3) Uiso 1 1 d . . . C12 C 0.1259(15) 0.0878(8) 0.9694(7) 0.026(4) Uiso 1 1 d . . . C13 C -0.4323(14) -0.0737(7) 1.1074(6) 0.019(3) Uiso 1 1 d . . . C14 C -0.4396(15) -0.0491(7) 1.0416(6) 0.021(3) Uiso 1 1 d . . . C15 C -0.5661(15) -0.0642(8) 1.0000(6) 0.024(3) Uiso 1 1 d . . . C16 C -0.6878(15) -0.1001(7) 1.0188(6) 0.025(4) Uiso 1 1 d . . . C17 C -0.6832(16) -0.1213(7) 1.0876(6) 0.021(3) Uiso 1 1 d . . . C18 C -0.5553(16) -0.1070(8) 1.1269(7) 0.028(4) Uiso 1 1 d . . . O13 O 0.4923(10) 0.2826(5) 0.9741(5) 0.032(3) Uani 1 1 d . . . O14 O 0.4875(11) 0.1901(6) 0.8527(4) 0.036(3) Uani 1 1 d . . . O15 O 0.6509(11) 0.0829(5) 0.9312(5) 0.034(3) Uani 1 1 d . . . O16 O -0.0683(11) -0.1076(5) 1.0758(5) 0.035(3) Uani 1 1 d . . . O17 O -0.2253(10) 0.0910(5) 1.1207(5) 0.029(2) Uani 1 1 d . . . O18 O -0.0672(12) -0.0213(6) 1.2002(5) 0.039(3) Uani 1 1 d . . . O19 O 0.5895(12) 0.2876(5) 0.7736(5) 0.038(3) Uiso 1 1 d . . . O20 O 0.6177(15) 0.0246(8) 0.8199(6) 0.071(4) Uiso 1 1 d . . . O21 O 0.8066(12) 0.2322(6) 0.6965(5) 0.044(3) Uiso 1 1 d . . . O22 O 0.6180(13) 0.7304(6) 0.6985(5) 0.050(3) Uiso 1 1 d . . . O23 O 0.6022(12) 0.4066(6) 0.8509(5) 0.048(3) Uiso 1 1 d . . . O24 O 0.7170(11) 0.6507(5) 0.7995(5) 0.042(3) Uiso 1 1 d . . . O25 O 0.7897(11) 0.9058(6) 0.8387(5) 0.041(3) Uiso 1 1 d . . . O26 O 0.7091(13) 0.5064(6) 0.7706(6) 0.059(3) Uiso 1 1 d . . . O27 O 0.8053(11) 0.8427(6) 0.7276(5) 0.042(3) Uiso 1 1 d . . . O28 O 0.8289(14) 0.1178(7) 0.7726(6) 0.067(4) 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 Sc1 0.0130(13) 0.0316(18) 0.0251(16) 0.0029(13) 0.0006(12) -0.0060(12) Sc2 0.0153(13) 0.0277(18) 0.0236(15) 0.0029(13) -0.0014(12) -0.0048(12) Cl1 0.035(2) 0.072(3) 0.026(2) 0.007(2) 0.0055(19) -0.011(2) Cl2 0.033(2) 0.047(3) 0.027(2) 0.010(2) -0.0027(18) -0.0151(19) Cl3 0.024(2) 0.063(3) 0.030(2) 0.006(2) -0.0062(18) -0.0131(19) Cl4 0.027(2) 0.063(3) 0.027(2) 0.009(2) -0.0022(18) -0.011(2) Cl5 0.036(2) 0.050(3) 0.027(2) 0.004(2) -0.0035(18) -0.016(2) Cl6 0.035(2) 0.059(3) 0.023(2) 0.006(2) 0.0055(17) -0.011(2) O1 0.014(5) 0.033(6) 0.040(7) 0.007(5) 0.003(5) -0.014(4) O2 0.019(5) 0.041(7) 0.018(5) 0.007(5) -0.007(4) -0.018(5) O3 0.014(5) 0.045(7) 0.040(6) 0.014(5) 0.000(5) -0.010(5) O4 0.015(5) 0.050(7) 0.033(6) -0.004(6) -0.010(5) -0.022(5) O5 0.019(5) 0.042(7) 0.025(5) 0.007(5) 0.000(4) -0.002(5) O6 0.017(5) 0.044(6) 0.024(5) 0.008(5) 0.001(4) -0.007(5) O7 0.021(5) 0.046(7) 0.028(6) 0.012(5) 0.006(5) -0.011(5) O8 0.018(5) 0.051(7) 0.027(6) 0.000(5) 0.005(5) -0.021(5) O9 0.015(5) 0.040(7) 0.031(6) 0.003(5) -0.001(4) -0.008(5) O10 0.021(6) 0.025(6) 0.024(6) 0.009(5) 0.004(5) 0.001(4) O11 0.020(6) 0.038(7) 0.043(7) 0.003(5) -0.003(5) -0.011(5) O12 0.014(5) 0.048(7) 0.040(6) 0.007(6) 0.009(4) -0.006(5) O13 0.016(5) 0.041(7) 0.039(6) -0.004(6) 0.007(5) 0.003(5) O14 0.038(6) 0.050(7) 0.018(6) 0.012(5) 0.003(5) -0.019(5) O15 0.040(6) 0.031(6) 0.034(6) -0.003(5) 0.010(5) -0.011(5) O16 0.030(6) 0.032(6) 0.042(7) -0.008(5) 0.004(5) -0.001(5) O17 0.020(5) 0.027(6) 0.037(6) 0.003(5) -0.005(5) 0.007(4) O18 0.038(7) 0.058(8) 0.019(6) 0.004(6) -0.007(5) -0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 O15 2.114(11) . ? Sc1 O14 2.140(9) . ? Sc1 O13 2.141(10) . ? Sc1 O1 2.161(10) . ? Sc1 O2 2.166(9) . ? Sc1 O5 2.203(9) . ? Sc1 O6 2.267(9) . ? Sc2 O16 2.115(10) . ? Sc2 O17 2.128(10) . ? Sc2 O9 2.142(10) . ? Sc2 O8 2.147(10) . ? Sc2 O18 2.165(10) . ? Sc2 O10 2.190(9) . ? Sc2 O7 2.227(9) . ? Cl1 C3 1.731(14) . ? Cl2 C6 1.721(15) . ? Cl3 C12 1.727(15) . ? Cl4 C9 1.725(15) . ? Cl5 C15 1.724(14) . ? Cl6 C18 1.731(15) . ? O1 C1 1.259(16) . ? O2 C2 1.253(15) . ? O3 C4 1.254(16) . ? O4 C5 1.238(17) . ? O5 C7 1.288(16) . ? O6 C8 1.283(16) . ? O7 C10 1.247(16) . ? O8 C11 1.272(16) . ? O9 C13 1.272(15) . ? O10 C14 1.286(16) . ? O11 C16 1.255(17) . ? O12 C17 1.244(17) . ? C1 C6 1.37(2) . ? C1 C2 1.539(19) . ? C2 C3 1.368(19) . ? C3 C4 1.40(2) . ? C4 C5 1.55(2) . ? C5 C6 1.40(2) . ? C7 C12 1.378(19) . ? C7 C8 1.508(19) . ? C8 C9 1.37(2) . ? C9 C10 1.401(19) . ? C10 C11 1.535(19) . ? C11 C12 1.39(2) . ? C13 C18 1.395(19) . ? C13 C14 1.505(19) . ? C14 C15 1.407(19) . ? C15 C16 1.402(19) . ? C16 C17 1.55(2) . ? C17 C18 1.39(2) . ? 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 O15 Sc1 O14 88.4(4) . . ? O15 Sc1 O13 173.8(4) . . ? O14 Sc1 O13 96.4(4) . . ? O15 Sc1 O1 87.0(4) . . ? O14 Sc1 O1 144.0(4) . . ? O13 Sc1 O1 86.8(4) . . ? O15 Sc1 O2 90.4(4) . . ? O14 Sc1 O2 72.4(4) . . ? O13 Sc1 O2 87.4(4) . . ? O1 Sc1 O2 72.0(3) . . ? O15 Sc1 O5 96.0(4) . . ? O14 Sc1 O5 72.6(4) . . ? O13 Sc1 O5 89.2(4) . . ? O1 Sc1 O5 143.4(4) . . ? O2 Sc1 O5 144.1(4) . . ? O15 Sc1 O6 87.1(4) . . ? O14 Sc1 O6 141.3(4) . . ? O13 Sc1 O6 91.5(4) . . ? O1 Sc1 O6 74.0(4) . . ? O2 Sc1 O6 146.0(3) . . ? O5 Sc1 O6 69.8(3) . . ? O16 Sc2 O17 172.9(4) . . ? O16 Sc2 O9 86.3(4) . . ? O17 Sc2 O9 91.6(4) . . ? O16 Sc2 O8 89.6(4) . . ? O17 Sc2 O8 88.4(4) . . ? O9 Sc2 O8 145.9(4) . . ? O16 Sc2 O18 96.1(4) . . ? O17 Sc2 O18 89.7(4) . . ? O9 Sc2 O18 72.3(4) . . ? O8 Sc2 O18 141.8(4) . . ? O16 Sc2 O10 86.3(4) . . ? O17 Sc2 O10 86.6(4) . . ? O9 Sc2 O10 72.7(4) . . ? O8 Sc2 O10 73.2(4) . . ? O18 Sc2 O10 144.7(4) . . ? O16 Sc2 O7 91.3(4) . . ? O17 Sc2 O7 94.4(4) . . ? O9 Sc2 O7 142.8(4) . . ? O8 Sc2 O7 71.1(3) . . ? O18 Sc2 O7 71.1(4) . . ? O10 Sc2 O7 144.2(4) . . ? C1 O1 Sc1 119.7(9) . . ? C2 O2 Sc1 121.1(9) . . ? C7 O5 Sc1 121.7(8) . . ? C8 O6 Sc1 120.1(8) . . ? C10 O7 Sc2 119.7(9) . . ? C11 O8 Sc2 122.1(9) . . ? C13 O9 Sc2 119.7(9) . . ? C14 O10 Sc2 118.4(9) . . ? O1 C1 C6 126.8(13) . . ? O1 C1 C2 114.6(12) . . ? C6 C1 C2 118.6(13) . . ? O2 C2 C3 127.4(13) . . ? O2 C2 C1 112.5(12) . . ? C3 C2 C1 120.1(12) . . ? C2 C3 C4 121.4(13) . . ? C2 C3 Cl1 118.7(11) . . ? C4 C3 Cl1 119.8(11) . . ? O3 C4 C3 123.9(13) . . ? O3 C4 C5 117.1(12) . . ? C3 C4 C5 118.9(13) . . ? O4 C5 C6 124.9(15) . . ? O4 C5 C4 117.2(14) . . ? C6 C5 C4 117.9(13) . . ? C1 C6 C5 123.1(14) . . ? C1 C6 Cl2 119.5(11) . . ? C5 C6 Cl2 117.4(11) . . ? O5 C7 C12 124.7(13) . . ? O5 C7 C8 114.4(11) . . ? C12 C7 C8 120.8(12) . . ? O6 C8 C9 125.9(13) . . ? O6 C8 C7 113.6(11) . . ? C9 C8 C7 120.4(13) . . ? C8 C9 C10 120.5(13) . . ? C8 C9 Cl4 120.6(11) . . ? C10 C9 Cl4 118.9(11) . . ? O7 C10 C9 127.7(12) . . ? O7 C10 C11 114.0(11) . . ? C9 C10 C11 118.4(12) . . ? O8 C11 C12 126.3(13) . . ? O8 C11 C10 113.2(12) . . ? C12 C11 C10 120.6(12) . . ? C7 C12 C11 119.1(13) . . ? C7 C12 Cl3 121.6(11) . . ? C11 C12 Cl3 119.2(11) . . ? O9 C13 C18 125.3(12) . . ? O9 C13 C14 115.4(12) . . ? C18 C13 C14 119.2(12) . . ? O10 C14 C15 126.6(13) . . ? O10 C14 C13 113.8(12) . . ? C15 C14 C13 119.6(12) . . ? C16 C15 C14 121.4(13) . . ? C16 C15 Cl5 118.7(11) . . ? C14 C15 Cl5 119.9(11) . . ? O11 C16 C15 123.2(13) . . ? O11 C16 C17 118.0(13) . . ? C15 C16 C17 118.7(12) . . ? O12 C17 C18 125.7(13) . . ? O12 C17 C16 116.2(12) . . ? C18 C17 C16 118.1(13) . . ? C17 C18 C13 122.8(13) . . ? C17 C18 Cl6 118.5(11) . . ? C13 C18 Cl6 118.6(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.511 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.094 #===END data_ycan2nrtabs93 _database_code_CSD 100527 _audit_creation_method SHELXL-93 _chemical_name_systematic ; 'Oxonium bis(chloranilate)yttrate.solvate' ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural 'Y(C6O4Cl2)2H3O.8CH3OH' _chemical_formula_analytical ? _chemical_formula_sum 'C20 H35 Cl4 O17 Y' _chemical_formula_weight 778.20 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I41/a' #(No.88) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 11.578(1) _cell_length_b 11.578(1) _cell_length_c 25.391(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3403.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 27 _exptl_crystal_description 'elongated octahedron' _exptl_crystal_colour black _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method ? _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 5.905 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3989 _exptl_absorpt_correction_T_max 0.5094 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device 'Enraf-Nonius CAD4 Diffractometer' _diffrn_measurement_method \w/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 17 _diffrn_reflns_number 1794 _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 60.02 _reflns_number_total 1258 _reflns_number_observed 790 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Extensive regions of disordered solvent in the structure led to poor agreement between observed and calculated structure factors. This problem has been addressed by omitting low angle reflections (resolution > 4 \a). This led to the omission of 14 refelctions. This results in the well localised framework making a relatively stronger contribution to the diffraction data used in the refinement. Four significant peaks of electron density were located in the solvent region of the structure and were assigned as disordered oxygen atoms. Their positions and site occupancies were allowed to refine but the isotropic displacement parameters were fixed. Refinement on F^2^ for ALL reflections except for the 14 lowest angle reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1244 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_obs 0.0808 _refine_ls_wR_factor_all 0.2721 _refine_ls_wR_factor_obs 0.2025 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.126 _refine_ls_restrained_S_all 1.208 _refine_ls_restrained_S_obs 1.126 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Y1 Y 0.5000 0.2500 0.3750 0.0559(7) Uani 1 d S . Cl1 Cl 0.2831(3) 0.1207(3) 0.55246(12) 0.0997(12) Uani 1 d . . O1 O 0.5796(6) 0.0818(6) 0.4074(2) 0.067(2) Uani 1 d . . O2 O 0.4003(5) 0.1779(6) 0.4509(2) 0.063(2) Uani 1 d . . C3 C 0.4010(8) 0.0528(9) 0.5240(4) 0.066(3) Uani 1 d . . C1 C 0.5498(8) 0.0370(9) 0.4515(3) 0.057(2) Uani 1 d . . C2 C 0.4433(8) 0.0965(8) 0.4764(3) 0.055(2) Uani 1 d . . O3 O 0.6338(24) 0.2682(26) 0.0665(11) 0.100 Uiso 0.31(2) d P . O4 O 0.6247(24) 0.3488(23) 0.1006(11) 0.100 Uiso 0.33(2) d P . O5 O 0.4413(34) 0.6093(33) 0.0471(13) 0.100 Uiso 0.25(2) d P . O6 O 0.3520(39) 0.5801(35) 0.0573(15) 0.100 Uiso 0.22(2) d P . 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 0.0640(9) 0.0640(9) 0.0397(9) 0.000 0.000 0.000 Cl1 0.100(2) 0.113(2) 0.086(2) 0.027(2) 0.044(2) 0.046(2) O1 0.079(5) 0.073(4) 0.048(4) 0.004(3) 0.017(3) 0.012(4) O2 0.059(4) 0.076(4) 0.054(4) 0.009(3) 0.012(3) 0.016(3) C3 0.066(6) 0.078(7) 0.053(5) 0.006(5) 0.013(5) 0.020(6) C1 0.056(5) 0.076(7) 0.041(5) -0.006(5) 0.004(4) 0.007(5) C2 0.060(6) 0.067(6) 0.039(4) 0.006(5) -0.006(4) 0.002(5) _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 O1 2.306(7) 2_655 ? Y1 O1 2.306(7) 11_666 ? Y1 O1 2.306(7) 12_656 ? Y1 O1 2.306(7) . yes Y1 O2 2.396(6) 11_666 ? Y1 O2 2.396(6) 2_655 ? Y1 O2 2.396(6) . yes Y1 O2 2.396(6) 12_656 ? Cl1 C3 1.734(9) . yes O1 C1 1.283(10) . yes O2 C2 1.248(10) . yes C3 C1 1.339(13) 9_656 ? C3 C2 1.397(12) . yes C1 C3 1.339(13) 9_656 yes C1 C2 1.547(13) . yes O3 O4 1.28(3) . ? O5 O6 1.12(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 O1 Y1 O1 97.29(10) 2_655 11_666 ? O1 Y1 O1 97.29(10) 2_655 12_656 ? O1 Y1 O1 138.3(3) 11_666 12_656 ? O1 Y1 O1 138.3(3) 2_655 . yes O1 Y1 O1 97.29(10) 11_666 . yes O1 Y1 O1 97.29(10) 12_656 . yes O1 Y1 O2 74.9(2) 2_655 11_666 ? O1 Y1 O2 67.2(2) 11_666 11_666 ? O1 Y1 O2 79.4(2) 12_656 11_666 ? O1 Y1 O2 146.4(2) . 11_666 yes O1 Y1 O2 67.2(2) 2_655 2_655 ? O1 Y1 O2 146.4(2) 11_666 2_655 ? O1 Y1 O2 74.9(2) 12_656 2_655 ? O1 Y1 O2 79.4(2) . 2_655 yes O2 Y1 O2 130.3(2) 11_666 2_655 ? O1 Y1 O2 79.4(2) 2_655 . yes O1 Y1 O2 74.9(2) 11_666 . yes O1 Y1 O2 146.4(2) 12_656 . yes O1 Y1 O2 67.2(2) . . yes O2 Y1 O2 130.3(2) 11_666 . yes O2 Y1 O2 73.0(3) 2_655 . yes O1 Y1 O2 146.4(2) 2_655 12_656 ? O1 Y1 O2 79.4(2) 11_666 12_656 ? O1 Y1 O2 67.2(2) 12_656 12_656 ? O1 Y1 O2 74.9(2) . 12_656 ? O2 Y1 O2 73.0(3) 11_666 12_656 ? O2 Y1 O2 130.3(2) 2_655 12_656 ? O2 Y1 O2 130.3(2) . 12_656 ? C1 O1 Y1 123.0(6) . . yes C2 O2 Y1 119.3(5) . . yes C1 C3 C2 122.2(9) 9_656 . yes C1 C3 Cl1 119.6(7) 9_656 . yes C2 C3 Cl1 118.2(8) . . yes O1 C1 C3 127.3(8) . 9_656 yes O1 C1 C2 113.1(8) . . yes C3 C1 C2 119.7(8) 9_656 . yes O2 C2 C3 125.6(9) . . yes O2 C2 C1 116.2(7) . . yes C3 C2 C1 118.1(8) . . yes _refine_diff_density_max 0.597 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.116 #===END data_thcanabs97 _database_code_CSD 175612 _audit_creation_method SHELXL-97 _chemical_name_systematic ; diaquabis(chloranilato)thorium(IV) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cl4 O14 Th' _chemical_formula_weight 754.06 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Th' 'Th' -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 13.884(1) _cell_length_b 11.522(1) _cell_length_c 12.720(1) _cell_angle_alpha 90.00 _cell_angle_beta 96.231(8) _cell_angle_gamma 90.00 _cell_volume 2022.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.8 _cell_measurement_theta_max 12.4 _exptl_crystal_description 'elongated octahedron' _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 7.972 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6758 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; The data were collected on a crystal exposed to the atmosphere. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method '\w:2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2254 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1781 _reflns_number_gt 1439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software' _computing_cell_refinement 'CAD4 software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1781 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Th Th 0.0000 0.26515(5) 0.2500 0.0236(2) Uani 1 2 d S . . Cl1 Cl 0.39767(19) 0.2663(4) 0.3266(2) 0.0526(9) Uani 1 1 d . . . O1 O 0.1807(5) 0.2879(7) 0.2986(5) 0.0311(18) Uani 1 1 d . . . O2 O 0.0630(5) 0.2976(7) 0.4413(6) 0.041(2) Uani 1 1 d . . . C1 C 0.2188(7) 0.2730(10) 0.3906(8) 0.030(3) Uani 1 1 d . . . C2 C 0.1495(7) 0.2704(11) 0.4744(8) 0.033(3) Uani 1 1 d . . . C3 C 0.3182(7) 0.2552(10) 0.4212(8) 0.031(3) Uani 1 1 d . . . Cl2 Cl -0.2002(2) 0.1019(3) 0.5586(3) 0.0532(10) Uani 1 1 d . . . O3 O 0.0769(5) 0.0848(7) 0.3316(6) 0.0314(19) Uani 1 1 d . . . O4 O -0.0913(5) 0.1640(6) 0.3758(6) 0.0302(18) Uani 1 1 d . . . C4 C 0.0438(7) 0.0402(10) 0.4101(9) 0.030(3) Uani 1 1 d . . . C5 C -0.0525(8) 0.0874(9) 0.4388(9) 0.028(3) Uani 1 1 d . . . C6 C -0.0923(8) 0.0468(10) 0.5229(9) 0.032(3) Uani 1 1 d . . . O5 O 0.0716(6) 0.4383(7) 0.1738(7) 0.046(2) Uani 1 1 d . . . O6 O 0.2679(7) 0.0376(9) 0.2208(8) 0.069(3) Uani 1 1 d . . . O7 O 0.4301(7) 0.0810(11) 0.0755(9) 0.080(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th 0.0168(3) 0.0360(4) 0.0161(3) 0.000 -0.00647(18) 0.000 Cl1 0.0306(13) 0.097(3) 0.0304(15) 0.000(2) 0.0032(11) -0.0047(19) O1 0.021(4) 0.050(5) 0.020(4) 0.005(4) -0.011(3) -0.007(3) O2 0.027(4) 0.067(6) 0.027(4) -0.012(4) -0.011(3) 0.014(4) C1 0.024(5) 0.037(7) 0.028(6) -0.001(6) -0.005(4) 0.003(5) C2 0.024(5) 0.048(7) 0.022(5) -0.008(6) -0.014(4) 0.002(6) C3 0.023(5) 0.046(7) 0.023(5) 0.009(6) -0.003(4) 0.010(6) Cl2 0.0350(17) 0.076(3) 0.050(2) 0.0184(19) 0.0139(15) 0.0212(17) O3 0.019(4) 0.054(5) 0.021(4) 0.008(4) 0.002(3) 0.001(4) O4 0.025(4) 0.041(5) 0.024(4) 0.009(4) -0.001(3) 0.006(4) C4 0.017(5) 0.042(7) 0.030(7) 0.002(6) 0.002(5) 0.000(5) C5 0.026(6) 0.031(7) 0.025(6) 0.011(5) -0.005(5) -0.001(5) C6 0.024(6) 0.040(7) 0.030(7) -0.012(6) -0.006(5) 0.002(5) O5 0.036(5) 0.052(6) 0.049(6) 0.014(5) -0.003(4) -0.014(4) O6 0.051(6) 0.087(8) 0.064(8) 0.007(6) -0.010(5) 0.024(6) O7 0.051(7) 0.113(10) 0.074(8) 0.014(7) -0.003(6) 0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th O4 2.442(7) 2 ? Th O4 2.442(7) . ? Th O5 2.473(8) 2 ? Th O5 2.473(8) . ? Th O3 2.509(7) 2 ? Th O3 2.509(7) . ? Th O2 2.523(7) . ? Th O2 2.523(7) 2 ? Th O1 2.532(6) 2 ? Th O1 2.532(6) . ? Cl1 C3 1.722(10) . ? O1 C1 1.242(11) . ? O2 C2 1.268(11) . ? C1 C3 1.408(13) . ? C1 C2 1.511(14) . ? C2 C3 1.386(13) 7_556 ? C3 C2 1.386(13) 7_556 ? Cl2 C6 1.732(11) . ? O3 C4 1.254(13) . ? O4 C5 1.272(12) . ? C4 C6 1.436(16) 5_556 ? C4 C5 1.525(15) . ? C5 C6 1.340(16) . ? C6 C4 1.436(16) 5_556 ? 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 O4 Th O4 123.0(3) 2 . ? O4 Th O5 154.3(3) 2 2 ? O4 Th O5 82.5(3) . 2 ? O4 Th O5 82.5(3) 2 . ? O4 Th O5 154.3(3) . . ? O5 Th O5 72.5(4) 2 . ? O4 Th O3 64.0(2) 2 2 ? O4 Th O3 69.4(2) . 2 ? O5 Th O3 131.2(3) 2 2 ? O5 Th O3 132.6(3) . 2 ? O4 Th O3 69.4(2) 2 . ? O4 Th O3 64.0(2) . . ? O5 Th O3 132.6(3) 2 . ? O5 Th O3 131.2(2) . . ? O3 Th O3 68.2(3) 2 . ? O4 Th O2 123.5(2) 2 . ? O4 Th O2 65.7(3) . . ? O5 Th O2 67.3(3) 2 . ? O5 Th O2 98.4(3) . . ? O3 Th O2 127.5(3) 2 . ? O3 Th O2 68.7(2) . . ? O4 Th O2 65.7(2) 2 2 ? O4 Th O2 123.5(2) . 2 ? O5 Th O2 98.4(3) 2 2 ? O5 Th O2 67.3(3) . 2 ? O3 Th O2 68.7(2) 2 2 ? O3 Th O2 127.5(3) . 2 ? O2 Th O2 163.0(4) . 2 ? O4 Th O1 117.4(2) 2 2 ? O4 Th O1 68.8(2) . 2 ? O5 Th O1 65.3(2) 2 2 ? O5 Th O1 104.5(3) . 2 ? O3 Th O1 67.6(2) 2 2 ? O3 Th O1 123.6(2) . 2 ? O2 Th O1 116.8(2) . 2 ? O2 Th O1 61.2(2) 2 2 ? O4 Th O1 68.8(2) 2 . ? O4 Th O1 117.4(2) . . ? O5 Th O1 104.5(3) 2 . ? O5 Th O1 65.3(2) . . ? O3 Th O1 123.6(2) 2 . ? O3 Th O1 67.6(2) . . ? O2 Th O1 61.2(2) . . ? O2 Th O1 116.8(2) 2 . ? O1 Th O1 168.1(3) 2 . ? C1 O1 Th 121.6(6) . . ? C2 O2 Th 120.1(6) . . ? O1 C1 C3 125.7(10) . . ? O1 C1 C2 115.4(8) . . ? C3 C1 C2 118.8(9) . . ? O2 C2 C3 124.5(10) . 7_556 ? O2 C2 C1 114.4(9) . . ? C3 C2 C1 121.1(8) 7_556 . ? C2 C3 C1 120.0(9) 7_556 . ? C2 C3 Cl1 121.3(7) 7_556 . ? C1 C3 Cl1 118.6(7) . . ? C4 O3 Th 119.5(7) . . ? C5 O4 Th 122.0(6) . . ? O3 C4 C6 124.8(10) . 5_556 ? O3 C4 C5 116.8(10) . . ? C6 C4 C5 118.3(10) 5_556 . ? O4 C5 C6 124.2(11) . . ? O4 C5 C4 114.8(10) . . ? C6 C5 C4 121.0(10) . . ? C5 C6 C4 120.7(10) . 5_556 ? C5 C6 Cl2 121.6(9) . . ? C4 C6 Cl2 117.6(9) 5_556 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.070 _refine_diff_density_min -1.222 _refine_diff_density_rms 0.237 #===END