Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global #============================================================================== _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Brown, Michael' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Levason, William' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Murray, David C.' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Popham, Michael C.' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Reid, Gillian' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Webster, Michael' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_name 'Professor W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email wxl@soton.ac.uk _publ_contact_author_fax '023 8059 6805' _publ_contact_author_phone '023 8059 3792' _publ_contact_letter ; 23 October 2002 Dear Sirs, This is the cif to accompany paper number B210458J. It contains details of six structures. Yours faithfully, William Levason ; _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_section_title ; Primary and secondary coordination of crown ethers to scandium(III). Synthesis, properties and structures of the reaction products of ScCl3(thf)3, ScCl3.6H2O and Sc(NO3)3.5H2O with crown ethers ; _publ_section_references ; Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Blessing, R. H. (1997). J. Appl. Cryst. 30, 421-426. Hooft, R. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter & R. M. Sweet, pp. 307-326. London: Academic Press. Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXS97. University of Gottingen, Germany. ; #============================================================================== data_d032 _database_code_CSD 196080 _audit_creation_method 'SHELXL-97 + template + hand edit' _chemical_name_systematic ; trichlorotriaquascandium(III)(1,4,7,10,13,16-hexaoxacyclooctadecane) ; _chemical_name_common ? _chemical_formula_moiety 'H6 Cl3 O3 Sc, C12 H24 O6' _chemical_formula_sum 'C12 H30 Cl3 O9 Sc' _chemical_formula_weight 469.67 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 orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 10.7210(10) _cell_length_b 14.8569(15) _cell_length_c 13.2776(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2114.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 21321 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.7854 # shelxl 0.8030 _exptl_absorpt_correction_T_max 0.9492 # shelxl 0.8621 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17374 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2415 _reflns_number_gt 1767 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+1.3890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2415 _refine_ls_number_parameters 125 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.037 _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 Sc1 Sc 0.0000 0.61103(3) 0.7500 0.01656(15) Uani 1 d S . . Cl1 Cl 0.22714(5) 0.60569(3) 0.76034(4) 0.02252(15) Uani 1 d . . . Cl2 Cl 0.0000 0.77437(5) 0.7500 0.0280(2) Uani 1 d S . . O1 O 0.57846(16) 0.16608(9) 0.11545(10) 0.0286(4) Uani 1 d . . . O2 O 0.33290(17) 0.13817(11) 0.05406(11) 0.0316(4) Uani 1 d . . . O3 O 0.26722(15) -0.04506(11) -0.00807(10) 0.0287(4) Uani 1 d . . . O4 O 0.0000 0.46451(13) 0.7500 0.0203(5) Uani 1 d SD . . O5 O 0.01095(16) 0.59069(10) 0.59054(11) 0.0232(4) Uani 1 d D . . C1 C 0.4963(3) 0.23961(15) 0.09971(18) 0.0385(7) Uani 1 d . . . H1A H 0.5009 0.2600 0.0288 0.0410(19) Uiso 1 calc R . . H1B H 0.5195 0.2906 0.1440 0.0410(19) Uiso 1 calc R . . C2 C 0.3689(3) 0.20851(17) 0.12344(16) 0.0418(7) Uani 1 d . . . H2A H 0.3661 0.1853 0.1933 0.0410(19) Uiso 1 calc R . . H2B H 0.3099 0.2595 0.1182 0.0410(19) Uiso 1 calc R . . C3 C 0.2292(2) 0.08849(17) 0.09119(17) 0.0358(6) Uani 1 d . . . H3A H 0.1623 0.1306 0.1118 0.0410(19) Uiso 1 calc R . . H3B H 0.2549 0.0535 0.1511 0.0410(19) Uiso 1 calc R . . C4 C 0.1810(2) 0.02640(18) 0.01276(18) 0.0376(6) Uani 1 d . . . H4A H 0.1008 0.0004 0.0356 0.0410(19) Uiso 1 calc R . . H4B H 0.1650 0.0607 -0.0499 0.0410(19) Uiso 1 calc R . . C5 C 0.2203(2) -0.10308(17) -0.08460(16) 0.0347(6) Uani 1 d . . . H5A H 0.2253 -0.0727 -0.1509 0.0410(19) Uiso 1 calc R . . H5B H 0.1318 -0.1176 -0.0709 0.0410(19) Uiso 1 calc R . . C6 C 0.2952(3) -0.18679(17) -0.08636(17) 0.0401(7) Uani 1 d . . . H6A H 0.2947 -0.2150 -0.0188 0.0410(19) Uiso 1 calc R . . H6B H 0.2584 -0.2299 -0.1348 0.0410(19) Uiso 1 calc R . . H4X H 0.027(2) 0.4316(16) 0.7954(17) 0.0410(19) Uiso 1 d D . . H5X H 0.076(2) 0.5767(19) 0.5640(19) 0.0410(19) Uiso 1 d D . . H5Y H -0.043(2) 0.5992(18) 0.5497(18) 0.0410(19) Uiso 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 Sc1 0.0263(3) 0.0116(3) 0.0118(2) 0.000 0.0000(2) 0.000 Cl1 0.0273(3) 0.0181(2) 0.0222(3) 0.0003(2) -0.0006(2) -0.00213(19) Cl2 0.0347(5) 0.0130(3) 0.0364(4) 0.000 0.0017(3) 0.000 O1 0.0514(11) 0.0176(7) 0.0169(7) 0.0019(6) 0.0020(7) -0.0036(7) O2 0.0455(11) 0.0330(9) 0.0162(7) -0.0020(7) 0.0040(7) 0.0128(8) O3 0.0267(9) 0.0405(9) 0.0189(7) -0.0031(7) -0.0026(6) -0.0014(7) O4 0.0329(13) 0.0122(9) 0.0156(10) 0.000 -0.0071(9) 0.000 O5 0.0300(10) 0.0263(8) 0.0131(7) 0.0018(6) -0.0007(6) 0.0060(7) C1 0.078(2) 0.0175(11) 0.0205(11) -0.0021(9) -0.0055(12) 0.0076(13) C2 0.075(2) 0.0350(13) 0.0155(11) -0.0083(10) -0.0072(12) 0.0332(14) C3 0.0417(16) 0.0421(14) 0.0236(11) 0.0057(10) 0.0081(11) 0.0204(12) C4 0.0235(14) 0.0555(16) 0.0338(13) 0.0115(12) 0.0038(11) 0.0082(12) C5 0.0346(15) 0.0479(15) 0.0217(11) 0.0000(10) -0.0031(10) -0.0178(12) C6 0.0623(19) 0.0378(14) 0.0201(11) -0.0017(10) 0.0064(11) -0.0315(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 O5 2.1419(14) . ? Sc1 O5 2.1419(14) 4_556 ? Sc1 O4 2.1768(19) . ? Sc1 Cl2 2.4267(8) . ? Sc1 Cl1 2.4403(6) 4_556 ? Sc1 Cl1 2.4403(6) . ? O1 C1 1.419(3) . ? O1 C6 1.441(3) 5_655 ? O2 C3 1.422(3) . ? O2 C2 1.446(3) . ? O3 C5 1.424(3) . ? O3 C4 1.435(3) . ? O4 H4X 0.828(16) . ? O5 H5X 0.808(17) . ? O5 H5Y 0.806(17) . ? C1 C2 1.475(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.484(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.480(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O1 1.441(3) 5_655 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 Sc1 O5 163.78(8) . 4_556 ? O5 Sc1 O4 81.89(4) . . ? O5 Sc1 O4 81.89(4) 4_556 . ? O5 Sc1 Cl2 98.11(4) . . ? O5 Sc1 Cl2 98.11(4) 4_556 . ? O4 Sc1 Cl2 180.0 . . ? O5 Sc1 Cl1 89.69(5) . 4_556 ? O5 Sc1 Cl1 89.79(5) 4_556 4_556 ? O4 Sc1 Cl1 88.135(16) . 4_556 ? Cl2 Sc1 Cl1 91.865(16) . 4_556 ? O5 Sc1 Cl1 89.79(5) . . ? O5 Sc1 Cl1 89.69(5) 4_556 . ? O4 Sc1 Cl1 88.136(16) . . ? Cl2 Sc1 Cl1 91.864(16) . . ? Cl1 Sc1 Cl1 176.27(3) 4_556 . ? C1 O1 C6 112.30(18) . 5_655 ? C3 O2 C2 111.29(18) . . ? C5 O3 C4 110.98(19) . . ? Sc1 O4 H4X 126.2(19) . . ? Sc1 O5 H5X 121(2) . . ? Sc1 O5 H5Y 127(2) . . ? H5X O5 H5Y 112(3) . . ? O1 C1 C2 107.58(19) . . ? O1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? O1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? O2 C2 C1 109.73(19) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O2 C3 C4 110.59(18) . . ? O2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? O2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O3 C4 C3 111.7(2) . . ? O3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? O3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? O3 C5 C6 109.2(2) . . ? O3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? O1 C6 C5 109.53(19) 5_655 . ? O1 C6 H6A 109.8 5_655 . ? C5 C6 H6A 109.8 . . ? O1 C6 H6B 109.8 5_655 . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 O1 C1 C2 175.16(17) 5_655 . . . ? C3 O2 C2 C1 162.63(19) . . . . ? O1 C1 C2 O2 -63.6(2) . . . . ? C2 O2 C3 C4 171.12(19) . . . . ? C5 O3 C4 C3 -179.04(18) . . . . ? O2 C3 C4 O3 68.6(2) . . . . ? C4 O3 C5 C6 -166.21(19) . . . . ? O3 C5 C6 O1 -64.8(2) . . . 5_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4X O1 0.828(16) 1.952(17) 2.768(2) 168(3) 3_456 O5 H5X O3 0.808(17) 1.990(17) 2.798(2) 177(3) 2 O5 H5Y O2 0.806(17) 1.998(18) 2.798(2) 172(3) 6_566 _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.879 _refine_diff_density_max 0.367 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.073 #===END OF CIF======================================== data_d052 _database_code_CSD 196081 _audit_creation_method 'SHELXL-97 + template + hand edit' _chemical_name_systematic ; dichloro(1,4,7,10,13,16-hexaoxacyclooctadecane)scandium(III) tetrachloroiron(III) ; _chemical_name_common ? _chemical_formula_moiety 'C12 H24 CL2 O6 Sc 1+, Cl4 Fe 1-' _chemical_formula_sum 'C12 H24 Cl6 Fe O6 Sc' _chemical_formula_weight 577.82 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' 'Fe' 'Fe' 0.3463 0.8444 '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.2026(15) _cell_length_b 11.2156(10) _cell_length_c 21.0990(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4544.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 22453 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.8157 # shelxl 0.6712 _exptl_absorpt_correction_T_max 0.8875 # shelxl 0.7316 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33479 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10116 _reflns_number_gt 7859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.00P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _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 0.095(14) _refine_ls_number_reflns 10116 _refine_ls_number_parameters 470 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 Fe1 Fe 0.67329(3) 0.79152(4) 0.60861(3) 0.02058(11) Uani 1 d . . . Fe2 Fe 0.43079(3) 1.26692(4) 0.61177(3) 0.02312(12) Uani 1 d . . . Sc1 Sc 0.61967(3) 1.24862(5) 0.87101(3) 0.01426(15) Uani 1 d . . . Sc2 Sc 0.36667(3) 0.75361(5) 0.86264(3) 0.01486(15) Uani 1 d . . . Cl1 Cl 0.74527(5) 1.23832(8) 0.88593(4) 0.0222(2) Uani 1 d . . . Cl2 Cl 0.49476(5) 1.26064(7) 0.86016(5) 0.0222(2) Uani 1 d . . . Cl3 Cl 0.49292(5) 0.75500(8) 0.86508(5) 0.0230(2) Uani 1 d . . . Cl4 Cl 0.24171(4) 0.74616(7) 0.86671(4) 0.02151(19) Uani 1 d . . . Cl5 Cl 0.73719(5) 0.64469(8) 0.57408(5) 0.0318(2) Uani 1 d . . . Cl6 Cl 0.72861(5) 0.96324(8) 0.60316(5) 0.0313(2) Uani 1 d . . . Cl7 Cl 0.64466(6) 0.76713(9) 0.70880(4) 0.0327(2) Uani 1 d . . . Cl8 Cl 0.57935(5) 0.79733(10) 0.55032(5) 0.0387(3) Uani 1 d . . . Cl9 Cl 0.34854(6) 1.23500(10) 0.54232(5) 0.0409(3) Uani 1 d . . . Cl10 Cl 0.50513(5) 1.11851(9) 0.61646(5) 0.0347(2) Uani 1 d . . . Cl11 Cl 0.38382(6) 1.28242(9) 0.70566(5) 0.0347(2) Uani 1 d . . . Cl12 Cl 0.48623(6) 1.43299(10) 0.58825(6) 0.0496(3) Uani 1 d . . . O1 O 0.61275(12) 1.1958(2) 0.97099(11) 0.0181(5) Uani 1 d . . . O2 O 0.62084(12) 1.4087(2) 0.93060(10) 0.0186(5) Uani 1 d . . . O3 O 0.62195(12) 1.4081(2) 0.80788(11) 0.0178(5) Uani 1 d . . . O4 O 0.70355(13) 1.3703(2) 0.69571(12) 0.0270(6) Uani 1 d . . . O5 O 0.63681(13) 1.1675(2) 0.77509(11) 0.0189(6) Uani 1 d . . . O6 O 0.60550(12) 1.0537(2) 0.87908(11) 0.0184(5) Uani 1 d . . . O7 O 0.37485(13) 0.6789(2) 0.76325(11) 0.0188(5) Uani 1 d . . . O8 O 0.39451(14) 0.8528(2) 0.66227(11) 0.0265(6) Uani 1 d . . . O9 O 0.35714(12) 0.9162(2) 0.80360(10) 0.0169(5) Uani 1 d . . . O10 O 0.37001(13) 0.9121(2) 0.92406(11) 0.0203(6) Uani 1 d . . . O11 O 0.37166(13) 0.6951(2) 0.96272(11) 0.0202(6) Uani 1 d . . . O12 O 0.36330(12) 0.55783(19) 0.86970(11) 0.0203(5) Uani 1 d . . . C1 C 0.6014(2) 1.2873(3) 1.01858(16) 0.0230(8) Uani 1 d . . . H1A H 0.6184 1.2606 1.0605 0.0222(14) Uiso 1 calc R . . H1B H 0.5513 1.3073 1.0220 0.0222(14) Uiso 1 calc R . . C2 C 0.6421(2) 1.3919(3) 0.99583(16) 0.0226(8) Uani 1 d . . . H2A H 0.6313 1.4636 1.0214 0.0222(14) Uiso 1 calc R . . H2B H 0.6927 1.3759 0.9985 0.0222(14) Uiso 1 calc R . . C3 C 0.6512(2) 1.5132(3) 0.90158(17) 0.0225(9) Uani 1 d . . . H3A H 0.7023 1.5038 0.8972 0.0222(14) Uiso 1 calc R . . H3B H 0.6417 1.5851 0.9274 0.0222(14) Uiso 1 calc R . . C4 C 0.6177(2) 1.5233(3) 0.83819(17) 0.0255(9) Uani 1 d . . . H4A H 0.5684 1.5476 0.8429 0.0222(14) Uiso 1 calc R . . H4B H 0.6420 1.5840 0.8123 0.0222(14) Uiso 1 calc R . . C5 C 0.59035(19) 1.4089(3) 0.74516(16) 0.0210(8) Uani 1 d . . . H5A H 0.5513 1.4666 0.7445 0.0222(14) Uiso 1 calc R . . H5B H 0.5713 1.3289 0.7357 0.0222(14) Uiso 1 calc R . . C6 C 0.6426(2) 1.4425(3) 0.69523(17) 0.0254(9) Uani 1 d . . . H6A H 0.6203 1.4362 0.6531 0.0222(14) Uiso 1 calc R . . H6B H 0.6564 1.5267 0.7015 0.0222(14) Uiso 1 calc R . . C7 C 0.6939(2) 1.2485(3) 0.68016(18) 0.0245(9) Uani 1 d . . . H7A H 0.7287 1.2248 0.6479 0.0222(14) Uiso 1 calc R . . H7B H 0.6470 1.2377 0.6615 0.0222(14) Uiso 1 calc R . . C8 C 0.7010(2) 1.1696(3) 0.73682(17) 0.0222(8) Uani 1 d . . . H8A H 0.7121 1.0876 0.7227 0.0222(14) Uiso 1 calc R . . H8B H 0.7401 1.1982 0.7633 0.0222(14) Uiso 1 calc R . . C9 C 0.5977(2) 1.0577(3) 0.76944(17) 0.0247(9) Uani 1 d . . . H9A H 0.6086 1.0176 0.7288 0.0222(14) Uiso 1 calc R . . H9B H 0.5471 1.0743 0.7708 0.0222(14) Uiso 1 calc R . . C10 C 0.6183(2) 0.9805(4) 0.82387(17) 0.0233(9) Uani 1 d . . . H10A H 0.5897 0.9071 0.8251 0.0222(14) Uiso 1 calc R . . H10B H 0.6680 0.9580 0.8210 0.0222(14) Uiso 1 calc R . . C11 C 0.6207(2) 0.9973(3) 0.93886(16) 0.0237(9) Uani 1 d . . . H11A H 0.6716 0.9894 0.9450 0.0222(14) Uiso 1 calc R . . H11B H 0.5993 0.9170 0.9409 0.0222(14) Uiso 1 calc R . . C12 C 0.5899(2) 1.0772(3) 0.98790(17) 0.0236(8) Uani 1 d . . . H12A H 0.5385 1.0721 0.9875 0.0222(14) Uiso 1 calc R . . H12B H 0.6069 1.0553 1.0307 0.0222(14) Uiso 1 calc R . . C13 C 0.4352(2) 0.6828(3) 0.72088(17) 0.0243(9) Uani 1 d . . . H13A H 0.4261 0.6318 0.6835 0.0222(14) Uiso 1 calc R . . H13B H 0.4763 0.6504 0.7432 0.0222(14) Uiso 1 calc R . . C14 C 0.4505(2) 0.8068(3) 0.69924(18) 0.0267(9) Uani 1 d . . . H14A H 0.4581 0.8587 0.7366 0.0222(14) Uiso 1 calc R . . H14B H 0.4937 0.8068 0.6736 0.0222(14) Uiso 1 calc R . . C15 C 0.3600(2) 0.9543(3) 0.68883(17) 0.0267(9) Uani 1 d . . . H15A H 0.3302 0.9911 0.6558 0.0222(14) Uiso 1 calc R . . H15B H 0.3954 1.0138 0.7015 0.0222(14) Uiso 1 calc R . . C16 C 0.31603(18) 0.9250(3) 0.74492(16) 0.0218(8) Uani 1 d . . . H16A H 0.2801 0.9875 0.7502 0.0222(14) Uiso 1 calc R . . H16B H 0.2919 0.8483 0.7374 0.0222(14) Uiso 1 calc R . . C17 C 0.3623(2) 1.0322(3) 0.83390(17) 0.0228(9) Uani 1 d . . . H17A H 0.3152 1.0647 0.8422 0.0222(14) Uiso 1 calc R . . H17B H 0.3875 1.0886 0.8061 0.0222(14) Uiso 1 calc R . . C18 C 0.4005(2) 1.0157(3) 0.89432(17) 0.0229(9) Uani 1 d . . . H18A H 0.4507 1.0027 0.8862 0.0222(14) Uiso 1 calc R . . H18B H 0.3952 1.0867 0.9218 0.0222(14) Uiso 1 calc R . . C19 C 0.3943(2) 0.8936(4) 0.98805(17) 0.0285(9) Uani 1 d . . . H19A H 0.3824 0.9628 1.0151 0.0222(14) Uiso 1 calc R . . H19B H 0.4454 0.8820 0.9888 0.0222(14) Uiso 1 calc R . . C20 C 0.3576(2) 0.7841(3) 1.01052(17) 0.0261(9) Uani 1 d . . . H20A H 0.3759 0.7584 1.0522 0.0222(14) Uiso 1 calc R . . H20B H 0.3069 0.7985 1.0144 0.0222(14) Uiso 1 calc R . . C21 C 0.3502(2) 0.5757(3) 0.97911(17) 0.0244(9) Uani 1 d . . . H21A H 0.2988 0.5691 0.9796 0.0222(14) Uiso 1 calc R . . H21B H 0.3684 0.5528 1.0213 0.0222(14) Uiso 1 calc R . . C22 C 0.3807(2) 0.4988(3) 0.92840(17) 0.0244(9) Uani 1 d . . . H22A H 0.4319 0.4924 0.9334 0.0222(14) Uiso 1 calc R . . H22B H 0.3604 0.4177 0.9298 0.0222(14) Uiso 1 calc R . . C23 C 0.3688(2) 0.4867(3) 0.81309(17) 0.0202(8) Uani 1 d . . . H23A H 0.3417 0.4120 0.8172 0.0222(14) Uiso 1 calc R . . H23B H 0.4179 0.4665 0.8040 0.0222(14) Uiso 1 calc R . . C24 C 0.3390(2) 0.5650(3) 0.76206(17) 0.0231(8) Uani 1 d . . . H24A H 0.3451 0.5266 0.7202 0.0222(14) Uiso 1 calc R . . H24B H 0.2885 0.5770 0.7693 0.0222(14) Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0224(3) 0.0199(2) 0.0194(2) 0.0009(3) 0.0000(2) 0.0013(2) Fe2 0.0226(3) 0.0266(3) 0.0201(3) 0.0000(3) -0.0002(2) 0.0012(2) Sc1 0.0157(4) 0.0128(3) 0.0143(3) 0.0007(3) 0.0000(3) 0.0003(3) Sc2 0.0161(3) 0.0132(3) 0.0153(3) -0.0014(3) 0.0005(3) -0.0003(3) Cl1 0.0170(5) 0.0247(5) 0.0250(4) 0.0005(4) 0.0007(4) 0.0011(4) Cl2 0.0170(5) 0.0193(4) 0.0303(5) 0.0015(4) -0.0015(4) 0.0004(3) Cl3 0.0164(4) 0.0233(5) 0.0292(5) 0.0006(4) -0.0005(4) 0.0007(4) Cl4 0.0165(4) 0.0186(4) 0.0295(5) -0.0013(4) 0.0021(4) -0.0007(3) Cl5 0.0332(6) 0.0263(5) 0.0359(5) -0.0068(4) 0.0034(5) 0.0042(4) Cl6 0.0376(6) 0.0232(4) 0.0331(5) -0.0056(4) 0.0066(5) -0.0063(4) Cl7 0.0532(7) 0.0247(5) 0.0203(5) 0.0020(4) 0.0067(5) 0.0086(5) Cl8 0.0281(6) 0.0454(6) 0.0427(6) 0.0163(5) -0.0103(5) -0.0048(5) Cl9 0.0391(7) 0.0520(7) 0.0317(5) -0.0144(5) -0.0134(5) 0.0089(5) Cl10 0.0307(5) 0.0373(5) 0.0360(5) 0.0068(5) 0.0103(5) 0.0110(4) Cl11 0.0506(7) 0.0307(5) 0.0227(5) -0.0071(4) 0.0055(5) 0.0077(5) Cl12 0.0353(6) 0.0430(7) 0.0705(8) 0.0265(6) -0.0079(5) -0.0090(5) O1 0.0248(14) 0.0158(13) 0.0138(12) 0.0011(10) 0.0021(10) -0.0025(11) O2 0.0234(14) 0.0165(13) 0.0157(12) -0.0008(10) -0.0017(10) -0.0044(11) O3 0.0226(14) 0.0116(13) 0.0191(12) 0.0013(10) -0.0021(10) 0.0012(10) O4 0.0298(15) 0.0209(14) 0.0301(14) -0.0010(12) 0.0035(12) -0.0029(12) O5 0.0259(15) 0.0138(13) 0.0169(12) -0.0011(10) 0.0042(10) 0.0011(10) O6 0.0226(13) 0.0157(12) 0.0168(12) 0.0000(10) 0.0006(11) 0.0023(10) O7 0.0224(14) 0.0145(13) 0.0196(13) -0.0041(11) 0.0010(10) -0.0004(10) O8 0.0398(17) 0.0253(14) 0.0143(12) -0.0008(11) -0.0010(12) 0.0034(13) O9 0.0209(13) 0.0117(12) 0.0180(12) -0.0019(10) -0.0002(10) 0.0000(10) O10 0.0309(15) 0.0171(13) 0.0128(11) -0.0027(11) 0.0015(11) -0.0042(11) O11 0.0300(15) 0.0159(13) 0.0146(12) 0.0001(11) 0.0011(11) -0.0055(11) O12 0.0293(14) 0.0142(12) 0.0175(12) 0.0000(11) -0.0009(11) -0.0003(10) C1 0.030(2) 0.026(2) 0.0138(17) -0.0005(15) 0.0064(16) 0.0023(18) C2 0.023(2) 0.028(2) 0.0166(18) -0.0062(16) 0.0004(15) -0.0022(17) C3 0.031(2) 0.0134(19) 0.0228(19) -0.0033(15) 0.0059(16) -0.0026(16) C4 0.038(3) 0.012(2) 0.027(2) -0.0019(16) 0.0036(17) 0.0013(17) C5 0.024(2) 0.0204(19) 0.0191(17) 0.0030(15) -0.0046(16) 0.0021(16) C6 0.037(2) 0.0159(19) 0.0231(19) 0.0034(16) -0.0018(18) 0.0029(17) C7 0.028(2) 0.024(2) 0.0219(19) 0.0010(16) 0.0039(17) -0.0029(17) C8 0.025(2) 0.022(2) 0.0195(17) 0.0003(16) 0.0062(16) 0.0037(17) C9 0.036(2) 0.0151(19) 0.0229(19) -0.0034(16) 0.0013(18) -0.0070(17) C10 0.029(2) 0.0143(19) 0.026(2) -0.0055(16) 0.0048(17) 0.0010(17) C11 0.031(2) 0.018(2) 0.022(2) 0.0097(16) -0.0031(17) 0.0038(16) C12 0.029(2) 0.0196(19) 0.0222(18) 0.0054(16) 0.0036(17) -0.0064(17) C13 0.029(2) 0.025(2) 0.0191(19) 0.0017(16) 0.0076(16) 0.0036(17) C14 0.028(2) 0.031(2) 0.0217(19) 0.0011(17) 0.0042(17) -0.0014(18) C15 0.036(2) 0.021(2) 0.0235(19) 0.0049(17) -0.0037(17) 0.0007(18) C16 0.026(2) 0.022(2) 0.0179(18) 0.0027(16) -0.0079(16) -0.0010(16) C17 0.031(2) 0.0127(19) 0.025(2) -0.0035(15) -0.0003(17) -0.0022(17) C18 0.034(2) 0.0109(18) 0.024(2) -0.0024(15) 0.0028(17) -0.0080(17) C19 0.042(3) 0.027(2) 0.0161(18) -0.0016(16) -0.0023(17) -0.0081(19) C20 0.035(2) 0.025(2) 0.0179(19) -0.0041(16) 0.0049(17) -0.0013(18) C21 0.032(2) 0.020(2) 0.0211(19) 0.0044(16) 0.0000(17) -0.0081(17) C22 0.029(2) 0.019(2) 0.026(2) 0.0068(16) -0.0071(17) -0.0042(16) C23 0.027(2) 0.0109(19) 0.023(2) -0.0022(15) 0.0006(16) 0.0005(15) C24 0.029(2) 0.0169(19) 0.0237(19) -0.0084(16) -0.0007(17) -0.0023(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Cl5 2.1791(10) . ? Fe1 Cl8 2.1841(11) . ? Fe1 Cl7 2.2013(11) . ? Fe1 Cl6 2.2025(10) . ? Fe2 Cl11 2.1836(11) . ? Fe2 Cl9 2.1840(12) . ? Fe2 Cl10 2.1950(10) . ? Fe2 Cl12 2.2020(12) . ? Sc1 O2 2.192(2) . ? Sc1 O1 2.195(2) . ? Sc1 O6 2.210(2) . ? Sc1 O3 2.230(2) . ? Sc1 O5 2.243(2) . ? Sc1 Cl2 2.4133(11) . ? Sc1 Cl1 2.4350(11) . ? Sc2 O10 2.200(2) . ? Sc2 O12 2.202(2) . ? Sc2 O11 2.213(2) . ? Sc2 O9 2.216(2) . ? Sc2 O7 2.264(2) . ? Sc2 Cl4 2.4025(11) . ? Sc2 Cl3 2.4249(12) . ? O1 C12 1.445(4) . ? O1 C1 1.452(4) . ? O2 C3 1.446(4) . ? O2 C2 1.448(4) . ? O3 C4 1.444(4) . ? O3 C5 1.456(4) . ? O4 C7 1.417(4) . ? O4 C6 1.423(4) . ? O5 C9 1.448(4) . ? O5 C8 1.473(4) . ? O6 C11 1.441(4) . ? O6 C10 1.446(4) . ? O7 C24 1.452(4) . ? O7 C13 1.464(4) . ? O8 C14 1.426(4) . ? O8 C15 1.432(4) . ? O9 C17 1.453(4) . ? O9 C16 1.472(4) . ? O10 C19 1.443(4) . ? O10 C18 1.445(4) . ? O11 C21 1.443(4) . ? O11 C20 1.444(4) . ? O12 C23 1.440(4) . ? O12 C22 1.444(4) . ? C1 C2 1.489(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.489(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.503(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.493(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.491(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.491(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.493(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.490(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.483(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.493(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.494(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.502(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? 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 Cl5 Fe1 Cl8 107.42(5) . . ? Cl5 Fe1 Cl7 111.58(4) . . ? Cl8 Fe1 Cl7 109.77(5) . . ? Cl5 Fe1 Cl6 111.82(4) . . ? Cl8 Fe1 Cl6 110.05(4) . . ? Cl7 Fe1 Cl6 106.22(4) . . ? Cl11 Fe2 Cl9 108.85(5) . . ? Cl11 Fe2 Cl10 106.74(4) . . ? Cl9 Fe2 Cl10 112.10(5) . . ? Cl11 Fe2 Cl12 109.68(5) . . ? Cl9 Fe2 Cl12 109.70(5) . . ? Cl10 Fe2 Cl12 109.70(5) . . ? O2 Sc1 O1 70.76(9) . . ? O2 Sc1 O6 140.13(9) . . ? O1 Sc1 O6 69.60(9) . . ? O2 Sc1 O3 71.68(8) . . ? O1 Sc1 O3 142.33(9) . . ? O6 Sc1 O3 147.33(9) . . ? O2 Sc1 O5 148.02(9) . . ? O1 Sc1 O5 140.03(9) . . ? O6 Sc1 O5 71.72(8) . . ? O3 Sc1 O5 77.50(9) . . ? O2 Sc1 Cl2 91.08(7) . . ? O1 Sc1 Cl2 92.64(7) . . ? O6 Sc1 Cl2 86.57(7) . . ? O3 Sc1 Cl2 85.30(7) . . ? O5 Sc1 Cl2 94.75(7) . . ? O2 Sc1 Cl1 87.40(7) . . ? O1 Sc1 Cl1 85.58(7) . . ? O6 Sc1 Cl1 93.73(7) . . ? O3 Sc1 Cl1 95.50(7) . . ? O5 Sc1 Cl1 87.25(7) . . ? Cl2 Sc1 Cl1 177.96(5) . . ? O10 Sc2 O12 140.04(9) . . ? O10 Sc2 O11 71.11(9) . . ? O12 Sc2 O11 68.96(9) . . ? O10 Sc2 O9 70.66(8) . . ? O12 Sc2 O9 148.90(9) . . ? O11 Sc2 O9 141.62(9) . . ? O10 Sc2 O7 147.40(9) . . ? O12 Sc2 O7 72.28(9) . . ? O11 Sc2 O7 140.45(9) . . ? O9 Sc2 O7 77.85(9) . . ? O10 Sc2 Cl4 92.07(7) . . ? O12 Sc2 Cl4 86.19(7) . . ? O11 Sc2 Cl4 89.93(7) . . ? O9 Sc2 Cl4 88.06(7) . . ? O7 Sc2 Cl4 95.14(7) . . ? O10 Sc2 Cl3 87.32(7) . . ? O12 Sc2 Cl3 91.97(7) . . ? O11 Sc2 Cl3 86.47(7) . . ? O9 Sc2 Cl3 95.12(7) . . ? O7 Sc2 Cl3 87.29(7) . . ? Cl4 Sc2 Cl3 176.35(4) . . ? C12 O1 C1 115.8(2) . . ? C12 O1 Sc1 120.3(2) . . ? C1 O1 Sc1 118.85(19) . . ? C3 O2 C2 113.2(3) . . ? C3 O2 Sc1 115.18(19) . . ? C2 O2 Sc1 116.2(2) . . ? C4 O3 C5 111.9(3) . . ? C4 O3 Sc1 116.9(2) . . ? C5 O3 Sc1 122.7(2) . . ? C7 O4 C6 116.0(3) . . ? C9 O5 C8 113.7(3) . . ? C9 O5 Sc1 110.1(2) . . ? C8 O5 Sc1 127.6(2) . . ? C11 O6 C10 115.0(3) . . ? C11 O6 Sc1 118.5(2) . . ? C10 O6 Sc1 118.6(2) . . ? C24 O7 C13 113.0(3) . . ? C24 O7 Sc2 107.99(19) . . ? C13 O7 Sc2 127.6(2) . . ? C14 O8 C15 115.1(3) . . ? C17 O9 C16 110.2(3) . . ? C17 O9 Sc2 118.9(2) . . ? C16 O9 Sc2 124.9(2) . . ? C19 O10 C18 113.0(3) . . ? C19 O10 Sc2 116.4(2) . . ? C18 O10 Sc2 113.95(19) . . ? C21 O11 C20 114.9(3) . . ? C21 O11 Sc2 119.43(19) . . ? C20 O11 Sc2 117.0(2) . . ? C23 O12 C22 116.1(3) . . ? C23 O12 Sc2 119.6(2) . . ? C22 O12 Sc2 120.6(2) . . ? O1 C1 C2 104.8(3) . . ? O1 C1 H1A 110.8 . . ? C2 C1 H1A 110.8 . . ? O1 C1 H1B 110.8 . . ? C2 C1 H1B 110.8 . . ? H1A C1 H1B 108.9 . . ? O2 C2 C1 105.1(3) . . ? O2 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O2 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? O2 C3 C4 105.5(3) . . ? O2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.8 . . ? O3 C4 C3 107.8(3) . . ? O3 C4 H4A 110.2 . . ? C3 C4 H4A 110.2 . . ? O3 C4 H4B 110.2 . . ? C3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? O3 C5 C6 111.1(3) . . ? O3 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O3 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O4 C6 C5 113.7(3) . . ? O4 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? O4 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O4 C7 C8 111.9(3) . . ? O4 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? O4 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O5 C8 C7 111.9(3) . . ? O5 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? O5 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? O5 C9 C10 107.0(3) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? O6 C10 C9 104.3(3) . . ? O6 C10 H10A 110.9 . . ? C9 C10 H10A 110.9 . . ? O6 C10 H10B 110.9 . . ? C9 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? O6 C11 C12 105.3(3) . . ? O6 C11 H11A 110.7 . . ? C12 C11 H11A 110.7 . . ? O6 C11 H11B 110.7 . . ? C12 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? O1 C12 C11 105.2(3) . . ? O1 C12 H12A 110.7 . . ? C11 C12 H12A 110.7 . . ? O1 C12 H12B 110.7 . . ? C11 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? O7 C13 C14 111.8(3) . . ? O7 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? O7 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? O8 C14 C13 110.8(3) . . ? O8 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? O8 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O8 C15 C16 113.5(3) . . ? O8 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? O8 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? O9 C16 C15 112.3(3) . . ? O9 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? O9 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? O9 C17 C18 107.5(3) . . ? O9 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O9 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? O10 C18 C17 105.8(3) . . ? O10 C18 H18A 110.6 . . ? C17 C18 H18A 110.6 . . ? O10 C18 H18B 110.6 . . ? C17 C18 H18B 110.6 . . ? H18A C18 H18B 108.7 . . ? O10 C19 C20 105.2(3) . . ? O10 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? O10 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? O11 C20 C19 105.0(3) . . ? O11 C20 H20A 110.7 . . ? C19 C20 H20A 110.7 . . ? O11 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? O11 C21 C22 104.6(3) . . ? O11 C21 H21A 110.8 . . ? C22 C21 H21A 110.8 . . ? O11 C21 H21B 110.8 . . ? C22 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? O12 C22 C21 105.0(3) . . ? O12 C22 H22A 110.8 . . ? C21 C22 H22A 110.8 . . ? O12 C22 H22B 110.8 . . ? C21 C22 H22B 110.8 . . ? H22A C22 H22B 108.8 . . ? O12 C23 C24 104.1(3) . . ? O12 C23 H23A 110.9 . . ? C24 C23 H23A 110.9 . . ? O12 C23 H23B 110.9 . . ? C24 C23 H23B 110.9 . . ? H23A C23 H23B 109.0 . . ? O7 C24 C23 108.7(3) . . ? O7 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O7 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sc1 O1 C12 163.4(3) . . . . ? O6 Sc1 O1 C12 -12.2(2) . . . . ? O3 Sc1 O1 C12 158.9(2) . . . . ? O5 Sc1 O1 C12 -27.4(3) . . . . ? Cl2 Sc1 O1 C12 73.2(2) . . . . ? Cl1 Sc1 O1 C12 -107.8(2) . . . . ? O2 Sc1 O1 C1 9.7(2) . . . . ? O6 Sc1 O1 C1 -165.8(3) . . . . ? O3 Sc1 O1 C1 5.2(3) . . . . ? O5 Sc1 O1 C1 178.9(2) . . . . ? Cl2 Sc1 O1 C1 -80.5(2) . . . . ? Cl1 Sc1 O1 C1 98.5(2) . . . . ? O1 Sc1 O2 C3 157.7(2) . . . . ? O6 Sc1 O2 C3 164.2(2) . . . . ? O3 Sc1 O2 C3 -25.2(2) . . . . ? O5 Sc1 O2 C3 -9.1(3) . . . . ? Cl2 Sc1 O2 C3 -109.9(2) . . . . ? Cl1 Sc1 O2 C3 71.5(2) . . . . ? O1 Sc1 O2 C2 21.9(2) . . . . ? O6 Sc1 O2 C2 28.4(3) . . . . ? O3 Sc1 O2 C2 -161.0(2) . . . . ? O5 Sc1 O2 C2 -144.9(2) . . . . ? Cl2 Sc1 O2 C2 114.3(2) . . . . ? Cl1 Sc1 O2 C2 -64.3(2) . . . . ? O2 Sc1 O3 C4 -4.5(2) . . . . ? O1 Sc1 O3 C4 0.0(3) . . . . ? O6 Sc1 O3 C4 164.4(2) . . . . ? O5 Sc1 O3 C4 -175.8(2) . . . . ? Cl2 Sc1 O3 C4 88.2(2) . . . . ? Cl1 Sc1 O3 C4 -89.9(2) . . . . ? O2 Sc1 O3 C5 -149.7(3) . . . . ? O1 Sc1 O3 C5 -145.2(2) . . . . ? O6 Sc1 O3 C5 19.1(3) . . . . ? O5 Sc1 O3 C5 38.9(2) . . . . ? Cl2 Sc1 O3 C5 -57.0(2) . . . . ? Cl1 Sc1 O3 C5 124.9(2) . . . . ? O2 Sc1 O5 C9 -157.1(2) . . . . ? O1 Sc1 O5 C9 42.5(3) . . . . ? O6 Sc1 O5 C9 27.4(2) . . . . ? O3 Sc1 O5 C9 -141.5(2) . . . . ? Cl2 Sc1 O5 C9 -57.4(2) . . . . ? Cl1 Sc1 O5 C9 122.3(2) . . . . ? O2 Sc1 O5 C8 57.5(3) . . . . ? O1 Sc1 O5 C8 -102.9(3) . . . . ? O6 Sc1 O5 C8 -118.0(3) . . . . ? O3 Sc1 O5 C8 73.1(2) . . . . ? Cl2 Sc1 O5 C8 157.2(2) . . . . ? Cl1 Sc1 O5 C8 -23.1(2) . . . . ? O2 Sc1 O6 C11 -25.0(3) . . . . ? O1 Sc1 O6 C11 -18.5(2) . . . . ? O3 Sc1 O6 C11 171.6(2) . . . . ? O5 Sc1 O6 C11 151.3(2) . . . . ? Cl2 Sc1 O6 C11 -112.6(2) . . . . ? Cl1 Sc1 O6 C11 65.4(2) . . . . ? O2 Sc1 O6 C10 -172.4(2) . . . . ? O1 Sc1 O6 C10 -165.9(2) . . . . ? O3 Sc1 O6 C10 24.2(3) . . . . ? O5 Sc1 O6 C10 3.8(2) . . . . ? Cl2 Sc1 O6 C10 100.0(2) . . . . ? Cl1 Sc1 O6 C10 -82.0(2) . . . . ? O10 Sc2 O7 C24 -157.9(2) . . . . ? O12 Sc2 O7 C24 28.5(2) . . . . ? O11 Sc2 O7 C24 40.3(3) . . . . ? O9 Sc2 O7 C24 -142.8(2) . . . . ? Cl4 Sc2 O7 C24 -55.9(2) . . . . ? Cl3 Sc2 O7 C24 121.4(2) . . . . ? O10 Sc2 O7 C13 61.9(3) . . . . ? O12 Sc2 O7 C13 -111.8(3) . . . . ? O11 Sc2 O7 C13 -100.0(3) . . . . ? O9 Sc2 O7 C13 77.0(3) . . . . ? Cl4 Sc2 O7 C13 163.9(2) . . . . ? Cl3 Sc2 O7 C13 -18.8(2) . . . . ? O10 Sc2 O9 C17 3.6(2) . . . . ? O12 Sc2 O9 C17 175.9(2) . . . . ? O11 Sc2 O9 C17 9.1(3) . . . . ? O7 Sc2 O9 C17 -167.8(2) . . . . ? Cl4 Sc2 O9 C17 96.5(2) . . . . ? Cl3 Sc2 O9 C17 -81.7(2) . . . . ? O10 Sc2 O9 C16 -146.7(3) . . . . ? O12 Sc2 O9 C16 25.6(3) . . . . ? O11 Sc2 O9 C16 -141.2(2) . . . . ? O7 Sc2 O9 C16 41.9(2) . . . . ? Cl4 Sc2 O9 C16 -53.8(2) . . . . ? Cl3 Sc2 O9 C16 128.0(2) . . . . ? O12 Sc2 O10 C19 20.9(3) . . . . ? O11 Sc2 O10 C19 18.2(2) . . . . ? O9 Sc2 O10 C19 -165.4(3) . . . . ? O7 Sc2 O10 C19 -149.7(2) . . . . ? Cl4 Sc2 O10 C19 107.4(2) . . . . ? Cl3 Sc2 O10 C19 -69.0(2) . . . . ? O12 Sc2 O10 C18 155.1(2) . . . . ? O11 Sc2 O10 C18 152.4(2) . . . . ? O9 Sc2 O10 C18 -31.1(2) . . . . ? O7 Sc2 O10 C18 -15.5(3) . . . . ? Cl4 Sc2 O10 C18 -118.3(2) . . . . ? Cl3 Sc2 O10 C18 65.3(2) . . . . ? O10 Sc2 O11 C21 160.3(3) . . . . ? O12 Sc2 O11 C21 -17.9(2) . . . . ? O9 Sc2 O11 C21 154.9(2) . . . . ? O7 Sc2 O11 C21 -29.9(3) . . . . ? Cl4 Sc2 O11 C21 68.1(2) . . . . ? Cl3 Sc2 O11 C21 -111.3(2) . . . . ? O10 Sc2 O11 C20 14.3(2) . . . . ? O12 Sc2 O11 C20 -163.8(3) . . . . ? O9 Sc2 O11 C20 8.9(3) . . . . ? O7 Sc2 O11 C20 -175.9(2) . . . . ? Cl4 Sc2 O11 C20 -77.9(2) . . . . ? Cl3 Sc2 O11 C20 102.7(2) . . . . ? O10 Sc2 O12 C23 -173.6(2) . . . . ? O11 Sc2 O12 C23 -170.9(2) . . . . ? O9 Sc2 O12 C23 17.8(3) . . . . ? O7 Sc2 O12 C23 1.0(2) . . . . ? Cl4 Sc2 O12 C23 97.7(2) . . . . ? Cl3 Sc2 O12 C23 -85.5(2) . . . . ? O10 Sc2 O12 C22 -16.1(3) . . . . ? O11 Sc2 O12 C22 -13.4(2) . . . . ? O9 Sc2 O12 C22 175.4(2) . . . . ? O7 Sc2 O12 C22 158.6(3) . . . . ? Cl4 Sc2 O12 C22 -104.8(2) . . . . ? Cl3 Sc2 O12 C22 72.1(2) . . . . ? C12 O1 C1 C2 168.4(3) . . . . ? Sc1 O1 C1 C2 -36.8(4) . . . . ? C3 O2 C2 C1 175.5(3) . . . . ? Sc1 O2 C2 C1 -47.9(3) . . . . ? O1 C1 C2 O2 50.8(4) . . . . ? C2 O2 C3 C4 -173.8(3) . . . . ? Sc1 O2 C3 C4 49.1(3) . . . . ? C5 O3 C4 C3 -180.0(3) . . . . ? Sc1 O3 C4 C3 31.2(4) . . . . ? O2 C3 C4 O3 -49.4(4) . . . . ? C4 O3 C5 C6 89.3(4) . . . . ? Sc1 O3 C5 C6 -123.9(3) . . . . ? C7 O4 C6 C5 65.4(4) . . . . ? O3 C5 C6 O4 54.3(4) . . . . ? C6 O4 C7 C8 -107.7(4) . . . . ? C9 O5 C8 C7 106.5(3) . . . . ? Sc1 O5 C8 C7 -109.2(3) . . . . ? O4 C7 C8 O5 80.6(4) . . . . ? C8 O5 C9 C10 96.0(3) . . . . ? Sc1 O5 C9 C10 -54.5(3) . . . . ? C11 O6 C10 C9 179.1(3) . . . . ? Sc1 O6 C10 C9 -32.4(3) . . . . ? O5 C9 C10 O6 54.9(4) . . . . ? C10 O6 C11 C12 -168.3(3) . . . . ? Sc1 O6 C11 C12 43.1(3) . . . . ? C1 O1 C12 C11 -168.0(3) . . . . ? Sc1 O1 C12 C11 37.5(3) . . . . ? O6 C11 C12 O1 -47.5(4) . . . . ? C24 O7 C13 C14 153.2(3) . . . . ? Sc2 O7 C13 C14 -68.1(4) . . . . ? C15 O8 C14 C13 116.6(3) . . . . ? O7 C13 C14 O8 -63.7(4) . . . . ? C14 O8 C15 C16 -72.1(4) . . . . ? C17 O9 C16 C15 88.9(4) . . . . ? Sc2 O9 C16 C15 -118.6(3) . . . . ? O8 C15 C16 O9 81.6(4) . . . . ? C16 O9 C17 C18 176.7(3) . . . . ? Sc2 O9 C17 C18 22.3(4) . . . . ? C19 O10 C18 C17 -171.3(3) . . . . ? Sc2 O10 C18 C17 52.9(3) . . . . ? O9 C17 C18 O10 -45.9(4) . . . . ? C18 O10 C19 C20 -179.9(3) . . . . ? Sc2 O10 C19 C20 -45.3(4) . . . . ? C21 O11 C20 C19 170.9(3) . . . . ? Sc2 O11 C20 C19 -41.6(4) . . . . ? O10 C19 C20 O11 52.9(4) . . . . ? C20 O11 C21 C22 -170.6(3) . . . . ? Sc2 O11 C21 C22 42.8(4) . . . . ? C23 O12 C22 C21 -162.8(3) . . . . ? Sc2 O12 C22 C21 38.9(3) . . . . ? O11 C21 C22 O12 -47.6(4) . . . . ? C22 O12 C23 C24 172.8(3) . . . . ? Sc2 O12 C23 C24 -28.6(3) . . . . ? C13 O7 C24 C23 91.9(3) . . . . ? Sc2 O7 C24 C23 -54.7(3) . . . . ? O12 C23 C24 O7 53.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.437 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.093 #===END OF CIF=============================== data_d053 _database_code_CSD 196082 _audit_creation_method 'SHELXL-97 + template + hand edit' _chemical_name_systematic ; tris(O,O'-nitrato)diaquascandium(III)bis(1,4,7,10-tetraoxacyclododecane) ; _chemical_name_common ? _chemical_formula_moiety 'H4 N3 O11 Sc, (C8 H16 O4)2' _chemical_formula_sum 'C16 H36 N3 O19 Sc' _chemical_formula_weight 619.44 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_Int_Tables_number 18 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' _cell_length_a 11.6362(15) _cell_length_b 13.432(3) _cell_length_c 8.7311(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1364.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4106 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.8521 # shelxl 0.9064 _exptl_absorpt_correction_T_max 0.8857 # shelxl 0.9384 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9719 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3109 _reflns_number_gt 2506 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.00P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _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 0.00(3) _refine_ls_number_reflns 3109 _refine_ls_number_parameters 185 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.0000 0.0000 -0.14894(6) 0.01757(14) Uani 1 d S . . O1 O 0.00323(15) -0.07993(10) 0.07775(16) 0.0261(3) Uani 1 d . . . O2 O 0.0000 0.0000 0.2955(2) 0.0582(8) Uani 1 d S . . O3 O 0.12489(12) -0.00262(12) -0.34836(15) 0.0233(3) Uani 1 d . . . O4 O 0.18719(13) 0.01091(13) -0.11712(15) 0.0253(3) Uani 1 d . . . O5 O 0.30885(14) 0.01492(14) -0.30826(18) 0.0322(4) Uani 1 d . . . O6 O 0.00620(17) -0.15251(11) -0.20393(17) 0.0260(4) Uani 1 d D . . O7 O 0.63391(14) 0.74432(12) 0.41747(19) 0.0306(4) Uani 1 d . . . O8 O 0.39932(14) 0.80669(12) 0.39996(17) 0.0262(4) Uani 1 d . . . O9 O 0.37334(13) 0.79473(11) 0.07889(17) 0.0241(4) Uani 1 d . . . O10 O 0.59571(13) 0.86791(11) 0.15627(18) 0.0257(4) Uani 1 d . . . N1 N 0.0000 0.0000 0.1579(3) 0.0295(6) Uani 1 d S . . N2 N 0.21051(16) 0.00798(15) -0.2617(2) 0.0225(4) Uani 1 d . . . C1 C 0.5662(3) 0.77206(19) 0.5470(3) 0.0368(7) Uani 1 d . . . H1A H 0.6172 0.7993 0.6274 0.0372(17) Uiso 1 calc R . . H1B H 0.5283 0.7120 0.5890 0.0372(17) Uiso 1 calc R . . C2 C 0.4762(2) 0.84798(19) 0.5086(3) 0.0359(7) Uani 1 d . . . H2A H 0.4337 0.8672 0.6023 0.0372(17) Uiso 1 calc R . . H2B H 0.5129 0.9084 0.4658 0.0372(17) Uiso 1 calc R . . C3 C 0.3333(2) 0.87931(18) 0.3211(3) 0.0299(6) Uani 1 d . . . H3A H 0.3822 0.9369 0.2934 0.0372(17) Uiso 1 calc R . . H3B H 0.2700 0.9033 0.3871 0.0372(17) Uiso 1 calc R . . C4 C 0.2857(2) 0.8315(2) 0.1793(3) 0.0321(6) Uani 1 d . . . H4A H 0.2349 0.7757 0.2093 0.0372(17) Uiso 1 calc R . . H4B H 0.2383 0.8808 0.1234 0.0372(17) Uiso 1 calc R . . C5 C 0.4342(2) 0.86991(18) -0.0062(3) 0.0282(6) Uani 1 d . . . H5A H 0.4168 0.9365 0.0366 0.0372(17) Uiso 1 calc R . . H5B H 0.4092 0.8689 -0.1145 0.0372(17) Uiso 1 calc R . . C6 C 0.5603(2) 0.85048(17) 0.0031(3) 0.0276(6) Uani 1 d . . . H6A H 0.5769 0.7808 -0.0264 0.0372(17) Uiso 1 calc R . . H6B H 0.6021 0.8953 -0.0676 0.0372(17) Uiso 1 calc R . . C7 C 0.7059(2) 0.8280(2) 0.1930(3) 0.0348(7) Uani 1 d . . . H7A H 0.7673 0.8724 0.1543 0.0372(17) Uiso 1 calc R . . H7B H 0.7155 0.7617 0.1452 0.0372(17) Uiso 1 calc R . . C8 C 0.7133(2) 0.8195(2) 0.3646(3) 0.0371(6) Uani 1 d . . . H8A H 0.7925 0.8013 0.3950 0.0372(17) Uiso 1 calc R . . H8B H 0.6943 0.8843 0.4122 0.0372(17) Uiso 1 calc R . . H6X H 0.037(2) -0.179(2) -0.280(2) 0.0372(17) Uiso 1 d D . . H6Y H -0.0431(19) -0.1877(18) -0.166(3) 0.0372(17) Uiso 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 Sc1 0.0193(3) 0.0145(3) 0.0190(3) 0.000 0.000 0.0000(3) O1 0.0340(9) 0.0214(8) 0.0229(8) 0.0012(5) 0.0008(10) 0.0015(9) O2 0.105(3) 0.0516(17) 0.0175(12) 0.000 0.000 0.012(2) O3 0.0243(8) 0.0250(8) 0.0206(7) 0.0007(9) -0.0013(6) -0.0019(8) O4 0.0252(8) 0.0310(9) 0.0197(8) 0.0001(7) 0.0006(6) -0.0007(8) O5 0.0233(9) 0.0392(11) 0.0342(9) 0.0009(8) 0.0073(7) -0.0013(8) O6 0.0328(10) 0.0162(8) 0.0288(8) -0.0015(6) 0.0075(9) -0.0010(8) O7 0.0312(10) 0.0243(9) 0.0365(10) 0.0011(7) -0.0080(8) 0.0002(8) O8 0.0308(10) 0.0249(9) 0.0228(8) 0.0021(7) 0.0019(7) 0.0003(7) O9 0.0256(9) 0.0200(9) 0.0268(9) 0.0024(6) -0.0034(7) -0.0010(7) O10 0.0232(8) 0.0267(9) 0.0270(8) -0.0009(7) 0.0008(7) 0.0022(7) N1 0.0337(15) 0.0324(15) 0.0223(13) 0.000 0.000 0.0028(16) N2 0.0228(11) 0.0193(10) 0.0253(9) 0.0013(9) 0.0017(8) -0.0009(9) C1 0.0529(18) 0.0344(15) 0.0232(13) 0.0015(10) -0.0116(12) -0.0002(13) C2 0.051(2) 0.0344(14) 0.0221(12) -0.0053(10) -0.0014(12) 0.0052(12) C3 0.0311(14) 0.0286(13) 0.0301(13) 0.0034(10) 0.0047(11) 0.0087(11) C4 0.0222(14) 0.0323(15) 0.0418(16) 0.0055(12) -0.0021(12) 0.0017(11) C5 0.0409(16) 0.0230(12) 0.0208(12) 0.0060(10) -0.0034(12) -0.0032(12) C6 0.0375(16) 0.0241(13) 0.0211(12) 0.0000(10) 0.0076(12) -0.0010(11) C7 0.0202(14) 0.0340(16) 0.0503(17) 0.0031(12) 0.0019(13) 0.0016(12) C8 0.0253(14) 0.0307(14) 0.0553(17) 0.0016(13) -0.0099(12) -0.0035(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 Sc1 O6 2.1053(15) . ? Sc1 O6 2.1053(15) 2 ? Sc1 O4 2.2007(15) . ? Sc1 O4 2.2007(15) 2 ? Sc1 O1 2.2520(15) 2 ? Sc1 O1 2.2520(15) . ? Sc1 O3 2.2681(14) 2 ? Sc1 O3 2.2681(14) . ? Sc1 N2 2.6422(18) 2 ? Sc1 N2 2.6422(18) . ? Sc1 N1 2.679(2) . ? O1 N1 1.2820(19) . ? O2 N1 1.202(3) . ? O3 N2 1.259(2) . ? O4 N2 1.292(2) . ? O5 N2 1.218(2) . ? O6 H6X 0.838(16) . ? O6 H6Y 0.813(16) . ? O7 C1 1.428(3) . ? O7 C8 1.444(3) . ? O8 C2 1.417(3) . ? O8 C3 1.419(3) . ? O9 C4 1.433(3) . ? O9 C5 1.440(3) . ? O10 C6 1.419(3) . ? O10 C7 1.426(3) . ? N1 O1 1.2820(19) 2 ? C1 C2 1.500(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.501(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.492(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.505(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? 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 Sc1 O6 153.64(9) . 2 ? O6 Sc1 O4 93.42(7) . . ? O6 Sc1 O4 89.88(7) 2 . ? O6 Sc1 O4 89.88(7) . 2 ? O6 Sc1 O4 93.42(7) 2 2 ? O4 Sc1 O4 165.49(8) . 2 ? O6 Sc1 O1 131.67(6) . 2 ? O6 Sc1 O1 74.69(5) 2 2 ? O4 Sc1 O1 82.75(6) . 2 ? O4 Sc1 O1 84.51(6) 2 2 ? O6 Sc1 O1 74.69(5) . . ? O6 Sc1 O1 131.67(6) 2 . ? O4 Sc1 O1 84.51(6) . . ? O4 Sc1 O1 82.75(6) 2 . ? O1 Sc1 O1 56.98(7) 2 . ? O6 Sc1 O3 82.07(6) . 2 ? O6 Sc1 O3 77.75(6) 2 2 ? O4 Sc1 O3 136.89(6) . 2 ? O4 Sc1 O3 57.58(5) 2 2 ? O1 Sc1 O3 131.04(6) 2 2 ? O1 Sc1 O3 133.85(6) . 2 ? O6 Sc1 O3 77.75(6) . . ? O6 Sc1 O3 82.07(6) 2 . ? O4 Sc1 O3 57.58(5) . . ? O4 Sc1 O3 136.89(6) 2 . ? O1 Sc1 O3 133.85(6) 2 . ? O1 Sc1 O3 131.04(6) . . ? O3 Sc1 O3 79.72(7) 2 . ? O6 Sc1 N2 84.68(7) . 2 ? O6 Sc1 N2 85.57(7) 2 2 ? O4 Sc1 N2 165.32(6) . 2 ? O4 Sc1 N2 29.17(5) 2 2 ? O1 Sc1 N2 109.36(6) 2 2 ? O1 Sc1 N2 108.89(6) . 2 ? O3 Sc1 N2 28.43(5) 2 2 ? O3 Sc1 N2 107.89(5) . 2 ? O6 Sc1 N2 85.57(7) . . ? O6 Sc1 N2 84.68(7) 2 . ? O4 Sc1 N2 29.17(5) . . ? O4 Sc1 N2 165.32(6) 2 . ? O1 Sc1 N2 108.89(6) 2 . ? O1 Sc1 N2 109.36(6) . . ? O3 Sc1 N2 107.89(5) 2 . ? O3 Sc1 N2 28.43(5) . . ? N2 Sc1 N2 136.24(8) 2 . ? O6 Sc1 N1 103.18(4) . . ? O6 Sc1 N1 103.18(4) 2 . ? O4 Sc1 N1 82.75(4) . . ? O4 Sc1 N1 82.75(4) 2 . ? O1 Sc1 N1 28.49(4) 2 . ? O1 Sc1 N1 28.49(4) . . ? O3 Sc1 N1 140.14(4) 2 . ? O3 Sc1 N1 140.14(4) . . ? N2 Sc1 N1 111.88(4) 2 . ? N2 Sc1 N1 111.88(4) . . ? N1 O1 Sc1 94.58(12) . . ? N2 O3 Sc1 92.53(11) . . ? N2 O4 Sc1 94.73(11) . . ? Sc1 O6 H6X 127.6(19) . . ? Sc1 O6 H6Y 116.7(19) . . ? H6X O6 H6Y 112(3) . . ? C1 O7 C8 115.07(19) . . ? C2 O8 C3 113.40(18) . . ? C4 O9 C5 115.08(18) . . ? C6 O10 C7 114.27(19) . . ? O2 N1 O1 123.07(11) . . ? O2 N1 O1 123.07(11) . 2 ? O1 N1 O1 113.9(2) . 2 ? O2 N1 Sc1 180.0 . . ? O1 N1 Sc1 56.93(11) . . ? O1 N1 Sc1 56.93(11) 2 . ? O5 N2 O3 123.49(17) . . ? O5 N2 O4 121.40(17) . . ? O3 N2 O4 115.11(16) . . ? O5 N2 Sc1 176.87(15) . . ? O3 N2 Sc1 59.05(10) . . ? O4 N2 Sc1 56.11(9) . . ? O7 C1 C2 112.7(2) . . ? O7 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? O7 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O8 C2 C1 108.9(2) . . ? O8 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O8 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O8 C3 C4 107.8(2) . . ? O8 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O8 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.5 . . ? O9 C4 C3 112.9(2) . . ? O9 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? O9 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O9 C5 C6 109.5(2) . . ? O9 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O9 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? O10 C6 C5 107.9(2) . . ? O10 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O10 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? O10 C7 C8 107.7(2) . . ? O10 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? O10 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O7 C8 C7 109.6(2) . . ? O7 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O7 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 O7 C1 C2 71.6(3) . . . . ? C3 O8 C2 C1 -161.8(2) . . . . ? O7 C1 C2 O8 62.1(3) . . . . ? C2 O8 C3 C4 162.1(2) . . . . ? C5 O9 C4 C3 -74.6(3) . . . . ? O8 C3 C4 O9 -59.5(3) . . . . ? C4 O9 C5 C6 133.3(2) . . . . ? C7 O10 C6 C5 164.34(19) . . . . ? O9 C5 C6 O10 -68.4(2) . . . . ? C6 O10 C7 C8 -160.2(2) . . . . ? C1 O7 C8 C7 -134.2(2) . . . . ? O10 C7 C8 O7 67.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6X O7 0.838(16) 1.862(17) 2.684(2) 167(3) 3_455 O6 H6Y O9 0.813(16) 1.896(18) 2.689(2) 165(3) 3_455 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.224 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.061 #===END OF CIF================================= data_d062 _database_code_CSD 196083 _audit_creation_method ' SHELXL-97 + template + hand edit' _chemical_name_systematic ; di(mu-hydroxo)bis((O,O'-nitrato)triaquascandium(III)) dinitrate (1,4,7,10-tetraoxacyclododecane) ; _chemical_name_common ? _chemical_formula_moiety 'H14 N2 O14 Sc2 2+, (N O3 1-)2, C8 H16 O4' _chemical_formula_sum 'C8 H30 N4 O24 Sc2' _chemical_formula_weight 656.28 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5712(15) _cell_length_b 9.2350(15) _cell_length_c 9.862(3) _cell_angle_alpha 85.497(7) _cell_angle_beta 84.869(8) _cell_angle_gamma 69.545(15) _cell_volume 642.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 18452 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.8746 # shelxl 0.8520 _exptl_absorpt_correction_T_max 0.9230 # shelxl 0.9391 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8198 _diffrn_reflns_av_R_equivalents 0.0851 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.45 _reflns_number_total 2801 _reflns_number_gt 2053 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.1240P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # difmap OH & geom CH2 _refine_ls_hydrogen_treatment mixed # H2O H refined with dfix _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2801 _refine_ls_number_parameters 191 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.026 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.30601(6) 0.15309(5) 0.49117(5) 0.01495(15) Uani 1 d . . . O1 O 0.0937(2) 0.12282(18) 0.35887(18) 0.0243(4) Uani 1 d . . . O2 O 0.0079(2) 0.34212(17) 0.45078(16) 0.0188(4) Uani 1 d . . . O3 O -0.1632(3) 0.3075(2) 0.2989(2) 0.0370(5) Uani 1 d . . . O4 O 0.1592(2) 0.08751(19) 0.66557(18) 0.0200(4) Uani 1 d D . . O5 O 0.2895(2) 0.36095(18) 0.59118(18) 0.0197(4) Uani 1 d D . . O6 O 0.4047(2) 0.26185(19) 0.32114(18) 0.0225(4) Uani 1 d D . . O7 O 0.5559(2) 0.06296(17) 0.58418(16) 0.0174(4) Uani 1 d . . . O8 O 0.5032(3) 0.7960(2) -0.06291(18) 0.0302(4) Uani 1 d . . . O9 O 0.2243(3) 1.1116(2) -0.07146(18) 0.0335(5) Uani 1 d . . . O10 O 0.4217(2) 0.55067(18) 0.33665(19) 0.0260(4) Uani 1 d . . . O11 O 0.1623(2) 0.59927(19) 0.23746(19) 0.0297(5) Uani 1 d . . . O12 O 0.2260(2) 0.78663(17) 0.31711(18) 0.0242(4) Uani 1 d . . . N1 N -0.0270(3) 0.2587(2) 0.3666(2) 0.0222(5) Uani 1 d . . . N2 N 0.2677(3) 0.6446(2) 0.2964(2) 0.0195(5) Uani 1 d . . . C1 C 0.3050(4) 0.8414(3) -0.0259(3) 0.0309(6) Uani 1 d . . . H1A H 0.2804 0.7629 0.0399 0.039(2) Uiso 1 calc R . . H1B H 0.2361 0.8468 -0.1080 0.039(2) Uiso 1 calc R . . C2 C 0.2338(4) 0.9970(3) 0.0370(3) 0.0309(6) Uani 1 d . . . H2A H 0.1072 1.0154 0.0838 0.039(2) Uiso 1 calc R . . H2B H 0.3209 1.0012 0.1046 0.039(2) Uiso 1 calc R . . C3 C 0.1962(4) 1.2635(3) -0.0288(3) 0.0366(7) Uani 1 d . . . H3A H 0.1440 1.2727 0.0671 0.039(2) Uiso 1 calc R . . H3B H 0.1040 1.3417 -0.0858 0.039(2) Uiso 1 calc R . . C4 C 0.3779(4) 1.2934(3) -0.0412(3) 0.0354(7) Uani 1 d . . . H4A H 0.4424 1.2652 -0.1321 0.039(2) Uiso 1 calc R . . H4B H 0.3531 1.4049 -0.0318 0.039(2) Uiso 1 calc R . . H4X H 0.191(4) 0.091(3) 0.745(2) 0.039(2) Uiso 1 d D . . H4Y H 0.042(3) 0.114(3) 0.667(3) 0.039(2) Uiso 1 d D . . H5X H 0.200(3) 0.441(2) 0.576(3) 0.039(2) Uiso 1 d D . . H5Y H 0.385(3) 0.382(3) 0.607(3) 0.039(2) Uiso 1 d D . . H6X H 0.424(4) 0.237(3) 0.241(2) 0.039(2) Uiso 1 d D . . H6Y H 0.410(4) 0.346(2) 0.329(3) 0.039(2) Uiso 1 d D . . H7X H 0.5964 0.1450 0.6335 0.039 Uiso 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 0.0134(2) 0.0113(2) 0.0199(3) -0.00238(17) -0.00187(17) -0.00339(17) O1 0.0189(9) 0.0139(9) 0.0370(11) -0.0097(8) -0.0090(8) 0.0016(7) O2 0.0199(8) 0.0131(8) 0.0244(10) -0.0062(7) -0.0055(7) -0.0048(7) O3 0.0267(10) 0.0281(10) 0.0515(13) -0.0125(9) -0.0248(9) 0.0041(8) O4 0.0156(8) 0.0218(9) 0.0226(10) -0.0004(8) -0.0023(7) -0.0062(7) O5 0.0159(9) 0.0118(8) 0.0304(10) -0.0035(7) -0.0061(7) -0.0022(7) O6 0.0302(10) 0.0158(9) 0.0223(10) -0.0039(8) 0.0031(8) -0.0095(8) O7 0.0170(8) 0.0113(8) 0.0237(9) -0.0039(7) -0.0028(7) -0.0035(7) O8 0.0311(10) 0.0400(11) 0.0193(10) -0.0001(8) -0.0029(8) -0.0119(9) O9 0.0388(11) 0.0387(11) 0.0233(11) -0.0013(8) -0.0071(8) -0.0128(9) O10 0.0192(9) 0.0145(9) 0.0450(12) 0.0007(8) -0.0119(8) -0.0047(7) O11 0.0281(10) 0.0228(9) 0.0437(12) -0.0055(8) -0.0149(9) -0.0119(8) O12 0.0197(9) 0.0139(9) 0.0404(11) -0.0047(8) -0.0040(8) -0.0066(7) N1 0.0182(11) 0.0186(11) 0.0289(13) -0.0064(9) -0.0038(9) -0.0034(9) N2 0.0174(10) 0.0157(10) 0.0261(12) -0.0017(9) -0.0010(9) -0.0066(9) C1 0.0287(14) 0.0454(17) 0.0248(15) -0.0020(13) -0.0007(12) -0.0206(13) C2 0.0262(14) 0.0460(17) 0.0239(15) -0.0031(13) -0.0009(11) -0.0165(13) C3 0.0358(17) 0.0346(16) 0.0347(18) -0.0051(13) -0.0106(13) -0.0037(13) C4 0.0443(17) 0.0369(17) 0.0254(16) 0.0024(13) -0.0086(13) -0.0138(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 O7 2.0501(16) . ? Sc1 O7 2.0645(16) 2_656 ? Sc1 O6 2.1011(18) . ? Sc1 O4 2.1275(18) . ? Sc1 O5 2.1865(17) . ? Sc1 O1 2.2609(17) . ? Sc1 O2 2.3658(17) . ? Sc1 N1 2.732(2) . ? Sc1 Sc1 3.2959(11) 2_656 ? O1 N1 1.271(2) . ? O2 N1 1.279(2) . ? O3 N1 1.210(3) . ? O4 H4X 0.850(17) . ? O4 H4Y 0.833(17) . ? O5 H5X 0.822(17) . ? O5 H5Y 0.841(18) . ? O6 H6X 0.825(17) . ? O6 H6Y 0.807(17) . ? O7 Sc1 2.0645(16) 2_656 ? O7 H7X 1.0732 . ? O8 C1 1.431(3) . ? O8 C4 1.435(3) 2_675 ? O9 C2 1.433(3) . ? O9 C3 1.434(3) . ? O10 N2 1.261(3) . ? O11 N2 1.227(3) . ? O12 N2 1.266(2) . ? C1 C2 1.511(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.488(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O8 1.435(3) 2_675 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 O7 Sc1 O7 73.54(7) . 2_656 ? O7 Sc1 O6 97.40(7) . . ? O7 Sc1 O6 91.76(7) 2_656 . ? O7 Sc1 O4 90.72(7) . . ? O7 Sc1 O4 98.88(7) 2_656 . ? O6 Sc1 O4 168.12(7) . . ? O7 Sc1 O5 82.22(6) . . ? O7 Sc1 O5 154.40(7) 2_656 . ? O6 Sc1 O5 83.15(7) . . ? O4 Sc1 O5 89.41(7) . . ? O7 Sc1 O1 149.90(6) . . ? O7 Sc1 O1 76.74(6) 2_656 . ? O6 Sc1 O1 88.12(7) . . ? O4 Sc1 O1 89.18(7) . . ? O5 Sc1 O1 127.87(6) . . ? O7 Sc1 O2 154.51(6) . . ? O7 Sc1 O2 131.90(6) 2_656 . ? O6 Sc1 O2 84.81(7) . . ? O4 Sc1 O2 84.14(6) . . ? O5 Sc1 O2 72.79(6) . . ? O1 Sc1 O2 55.23(6) . . ? O7 Sc1 N1 177.18(6) . . ? O7 Sc1 N1 104.02(6) 2_656 . ? O6 Sc1 N1 84.03(7) . . ? O4 Sc1 N1 88.24(7) . . ? O5 Sc1 N1 100.39(6) . . ? O1 Sc1 N1 27.48(6) . . ? O2 Sc1 N1 27.88(5) . . ? O7 Sc1 Sc1 36.92(4) . 2_656 ? O7 Sc1 Sc1 36.62(4) 2_656 2_656 ? O6 Sc1 Sc1 95.70(5) . 2_656 ? O4 Sc1 Sc1 96.00(5) . 2_656 ? O5 Sc1 Sc1 118.73(5) . 2_656 ? O1 Sc1 Sc1 113.23(5) . 2_656 ? O2 Sc1 Sc1 168.46(4) . 2_656 ? N1 Sc1 Sc1 140.63(5) . 2_656 ? N1 O1 Sc1 97.36(13) . . ? N1 O2 Sc1 92.20(12) . . ? Sc1 O4 H4X 121(2) . . ? Sc1 O4 H4Y 119(2) . . ? H4X O4 H4Y 109(3) . . ? Sc1 O5 H5X 118(2) . . ? Sc1 O5 H5Y 123(2) . . ? H5X O5 H5Y 111(3) . . ? Sc1 O6 H6X 129(2) . . ? Sc1 O6 H6Y 118(2) . . ? H6X O6 H6Y 112(3) . . ? Sc1 O7 Sc1 106.46(7) . 2_656 ? Sc1 O7 H7X 115.2 . . ? Sc1 O7 H7X 135.7 2_656 . ? C1 O8 C4 114.6(2) . 2_675 ? C2 O9 C3 115.0(2) . . ? O3 N1 O1 123.3(2) . . ? O3 N1 O2 121.98(19) . . ? O1 N1 O2 114.67(18) . . ? O3 N1 Sc1 173.02(18) . . ? O1 N1 Sc1 55.16(10) . . ? O2 N1 Sc1 59.91(11) . . ? O11 N2 O10 120.63(19) . . ? O11 N2 O12 121.04(19) . . ? O10 N2 O12 118.3(2) . . ? O8 C1 C2 110.7(2) . . ? O8 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? O8 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O9 C2 C1 107.2(2) . . ? O9 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O9 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? O9 C3 C4 110.5(2) . . ? O9 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? O9 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O8 C4 C3 109.7(2) 2_675 . ? O8 C4 H4A 109.7 2_675 . ? C3 C4 H4A 109.7 . . ? O8 C4 H4B 109.7 2_675 . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 O8 C1 C2 91.0(3) 2_675 . . . ? C3 O9 C2 C1 -168.0(2) . . . . ? O8 C1 C2 O9 74.7(3) . . . . ? C2 O9 C3 C4 101.0(3) . . . . ? O9 C3 C4 O8 -72.1(3) . . . 2_675 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4X O9 0.850(17) 1.879(18) 2.723(3) 172(3) 1_546 O4 H4Y O12 0.833(17) 1.910(18) 2.731(2) 168(3) 2_566 O5 H5X O2 0.822(17) 2.088(18) 2.904(2) 173(3) 2_566 O5 H5Y O10 0.841(18) 1.918(18) 2.751(2) 171(3) 2_666 O6 H6X O8 0.825(17) 1.811(19) 2.625(3) 169(3) 2_665 O6 H6Y O10 0.807(17) 1.926(18) 2.732(2) 176(3) . O7 H7X O12 1.07 1.79 2.776(2) 150.8 2_666 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.340 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.081 #===END OF CIF==================================== data_d064 _database_code_CSD 196084 _audit_creation_method 'SHELXL-97 + template + hand edit' _chemical_name_systematic ; chloro-methylcyanide-(1,4,7,10,13-pentaoxacyclopentadecane)scandium(III) bis(hexachloroantimony(V)) methylcyanide solvate ; _chemical_name_common ? _chemical_formula_moiety 'C14 H23 Cl N O5 Sc 2+, (Cl6 Sb 1-)2, C2 H3 N ' _chemical_formula_sum 'C14 H26 Cl13 N2 O5 Sb2 Sc' _chemical_formula_weight 1051.68 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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 21.209(2) _cell_length_b 13.4224(10) _cell_length_c 24.800(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7060.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 31400 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4064 _exptl_absorpt_coefficient_mu 2.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.7992 # shelxl 0.4411 _exptl_absorpt_correction_T_max 0.8822 # shelxl 0.6702 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38521 _diffrn_reflns_av_R_equivalents 0.1068 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8017 _reflns_number_gt 4920 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU # common U value _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8017 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.003 _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 Sb1 Sb 0.145027(16) 0.09413(2) 0.101881(13) 0.01959(9) Uani 1 d . . . Sb2 Sb 0.291086(15) 0.24671(2) -0.142385(13) 0.01574(9) Uani 1 d . . . Sc1 Sc -0.01444(4) 0.34744(7) -0.11126(4) 0.0146(2) Uani 1 d . . . Cl1 Cl -0.06083(6) 0.50690(9) -0.10507(5) 0.0284(3) Uani 1 d . . . Cl2 Cl 0.09672(7) -0.02659(10) 0.15790(6) 0.0325(3) Uani 1 d . . . Cl3 Cl 0.06806(6) 0.21137(10) 0.12907(5) 0.0246(3) Uani 1 d . . . Cl4 Cl 0.07691(7) 0.04439(11) 0.03044(5) 0.0338(3) Uani 1 d . . . Cl5 Cl 0.19207(6) 0.21559(11) 0.04604(6) 0.0316(3) Uani 1 d . . . Cl6 Cl 0.22119(7) -0.02300(11) 0.07363(6) 0.0395(4) Uani 1 d . . . Cl7 Cl 0.20945(6) 0.14080(10) 0.17505(5) 0.0305(3) Uani 1 d . . . Cl8 Cl 0.28203(7) 0.12073(9) -0.07659(5) 0.0279(3) Uani 1 d . . . Cl9 Cl 0.27701(6) 0.36536(9) -0.07299(5) 0.0227(3) Uani 1 d . . . Cl10 Cl 0.18215(6) 0.23478(10) -0.15972(6) 0.0302(3) Uani 1 d . . . Cl11 Cl 0.29719(6) 0.37877(9) -0.20521(5) 0.0252(3) Uani 1 d . . . Cl12 Cl 0.30924(6) 0.12706(9) -0.21102(5) 0.0227(3) Uani 1 d . . . Cl13 Cl 0.40190(6) 0.25458(10) -0.13020(5) 0.0221(3) Uani 1 d . . . O1 O -0.05408(16) 0.2973(2) -0.03693(13) 0.0222(8) Uani 1 d . . . O2 O -0.10186(15) 0.2716(2) -0.12792(13) 0.0193(8) Uani 1 d . . . O3 O -0.02510(15) 0.3384(2) -0.19789(13) 0.0180(8) Uani 1 d . . . O4 O 0.07179(15) 0.3974(2) -0.14835(12) 0.0175(8) Uani 1 d . . . O5 O 0.05205(15) 0.3805(2) -0.04686(13) 0.0181(8) Uani 1 d . . . N1 N 0.03033(19) 0.1938(3) -0.11440(16) 0.0193(9) Uani 1 d . . . N2 N 0.0588(3) 0.0756(4) -0.2453(2) 0.0462(14) Uani 1 d . . . C1 C -0.1151(2) 0.2456(4) -0.0350(2) 0.0258(13) Uani 1 d . . . H1A H -0.1393 0.2661 -0.0027 0.022(3) Uiso 1 calc R . . H1B H -0.1088 0.1725 -0.0338 0.022(3) Uiso 1 calc R . . C2 C -0.1488(2) 0.2752(4) -0.0852(2) 0.0247(13) Uani 1 d . . . H2A H -0.1838 0.2285 -0.0928 0.022(3) Uiso 1 calc R . . H2B H -0.1662 0.3433 -0.0816 0.022(3) Uiso 1 calc R . . C3 C -0.1274(2) 0.2820(4) -0.18172(19) 0.0240(13) Uani 1 d . . . H3A H -0.1477 0.3479 -0.1862 0.022(3) Uiso 1 calc R . . H3B H -0.1591 0.2295 -0.1889 0.022(3) Uiso 1 calc R . . C4 C -0.0724(2) 0.2716(4) -0.2191(2) 0.0222(12) Uani 1 d . . . H4A H -0.0567 0.2021 -0.2195 0.022(3) Uiso 1 calc R . . H4B H -0.0843 0.2908 -0.2563 0.022(3) Uiso 1 calc R . . C5 C 0.0294(2) 0.3518(4) -0.2320(2) 0.0250(13) Uani 1 d . . . H5A H 0.0167 0.3749 -0.2683 0.022(3) Uiso 1 calc R . . H5B H 0.0531 0.2886 -0.2357 0.022(3) Uiso 1 calc R . . C6 C 0.0688(3) 0.4288(4) -0.20439(18) 0.0228(12) Uani 1 d . . . H6A H 0.1115 0.4315 -0.2204 0.022(3) Uiso 1 calc R . . H6B H 0.0490 0.4954 -0.2074 0.022(3) Uiso 1 calc R . . C7 C 0.1147(2) 0.4542(4) -0.1149(2) 0.0222(12) Uani 1 d . . . H7A H 0.0992 0.5233 -0.1103 0.022(3) Uiso 1 calc R . . H7B H 0.1572 0.4565 -0.1314 0.022(3) Uiso 1 calc R . . C8 C 0.1166(2) 0.4009(4) -0.06178(19) 0.0214(12) Uani 1 d . . . H8A H 0.1406 0.3379 -0.0651 0.022(3) Uiso 1 calc R . . H8B H 0.1372 0.4430 -0.0341 0.022(3) Uiso 1 calc R . . C9 C 0.0469(3) 0.3172(4) 0.00046(19) 0.0253(13) Uani 1 d . . . H9A H 0.0707 0.3462 0.0310 0.022(3) Uiso 1 calc R . . H9B H 0.0638 0.2500 -0.0072 0.022(3) Uiso 1 calc R . . C10 C -0.0210(2) 0.3117(4) 0.0134(2) 0.0278(13) Uani 1 d . . . H10A H -0.0293 0.2554 0.0382 0.022(3) Uiso 1 calc R . . H10B H -0.0351 0.3740 0.0310 0.022(3) Uiso 1 calc R . . C11 C 0.0509(2) 0.1157(4) -0.11505(19) 0.0200(12) Uani 1 d . . . C12 C 0.0782(3) 0.0147(4) -0.1155(2) 0.0358(15) Uani 1 d . . . C13 C 0.1058(3) 0.0839(4) -0.2675(2) 0.0323(14) Uani 1 d . . . C14 C 0.1649(3) 0.0950(4) -0.2955(2) 0.0344(14) 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 Sb1 0.01940(18) 0.01979(19) 0.01959(18) -0.00030(15) -0.00255(16) -0.00002(15) Sb2 0.01501(17) 0.01509(18) 0.01712(18) -0.00034(13) -0.00047(14) 0.00038(15) Sc1 0.0159(5) 0.0144(5) 0.0134(5) 0.0006(4) -0.0001(4) 0.0008(4) Cl1 0.0352(8) 0.0195(7) 0.0306(7) -0.0039(6) -0.0069(7) 0.0102(6) Cl2 0.0391(9) 0.0245(8) 0.0339(8) 0.0079(6) -0.0036(7) -0.0073(6) Cl3 0.0237(7) 0.0268(7) 0.0234(7) 0.0019(6) 0.0021(6) 0.0047(6) Cl4 0.0379(8) 0.0370(9) 0.0265(7) -0.0060(6) -0.0106(7) -0.0033(7) Cl5 0.0229(7) 0.0385(9) 0.0332(8) 0.0125(7) 0.0018(6) -0.0028(6) Cl6 0.0386(9) 0.0342(9) 0.0456(9) -0.0066(7) 0.0014(7) 0.0133(7) Cl7 0.0300(8) 0.0315(8) 0.0301(8) -0.0005(6) -0.0127(6) -0.0020(6) Cl8 0.0401(8) 0.0184(7) 0.0250(7) 0.0048(5) 0.0106(6) 0.0016(6) Cl9 0.0247(7) 0.0198(7) 0.0238(7) -0.0061(5) -0.0008(6) 0.0016(6) Cl10 0.0154(7) 0.0359(8) 0.0393(8) -0.0129(7) -0.0017(6) -0.0004(6) Cl11 0.0331(8) 0.0207(7) 0.0220(7) 0.0055(5) -0.0023(6) 0.0044(6) Cl12 0.0250(7) 0.0214(7) 0.0218(7) -0.0043(5) 0.0002(6) 0.0006(6) Cl13 0.0159(6) 0.0282(7) 0.0221(6) 0.0014(6) -0.0034(5) 0.0004(6) O1 0.025(2) 0.026(2) 0.0158(18) 0.0037(15) 0.0021(16) -0.0026(16) O2 0.0148(18) 0.023(2) 0.0197(18) -0.0035(15) 0.0019(15) -0.0017(15) O3 0.0182(18) 0.0201(19) 0.0158(18) -0.0019(15) 0.0019(15) -0.0023(15) O4 0.0211(19) 0.0167(19) 0.0146(17) 0.0008(14) -0.0015(15) -0.0038(15) O5 0.0185(19) 0.0191(19) 0.0167(18) 0.0021(14) -0.0021(15) 0.0007(15) N1 0.020(2) 0.020(2) 0.018(2) -0.0028(19) 0.0029(19) 0.004(2) N2 0.055(4) 0.054(4) 0.031(3) -0.008(3) -0.009(3) -0.003(3) C1 0.025(3) 0.027(3) 0.026(3) 0.000(3) 0.012(2) -0.004(3) C2 0.017(3) 0.030(3) 0.028(3) -0.007(2) 0.010(2) -0.003(2) C3 0.022(3) 0.029(3) 0.021(3) -0.006(2) -0.009(2) 0.000(2) C4 0.017(3) 0.031(3) 0.019(3) -0.006(2) -0.006(2) -0.003(2) C5 0.025(3) 0.031(3) 0.019(3) 0.002(2) 0.002(2) -0.002(2) C6 0.032(3) 0.027(3) 0.010(2) 0.005(2) -0.002(2) -0.004(2) C7 0.018(3) 0.024(3) 0.025(3) -0.001(2) -0.002(2) -0.004(2) C8 0.020(3) 0.023(3) 0.022(3) -0.002(2) -0.006(2) -0.003(2) C9 0.037(3) 0.026(3) 0.013(3) 0.000(2) -0.002(2) -0.002(3) C10 0.034(3) 0.039(3) 0.011(3) -0.003(2) 0.003(2) -0.003(3) C11 0.019(3) 0.029(3) 0.012(3) -0.001(2) 0.001(2) 0.001(2) C12 0.057(4) 0.013(3) 0.037(3) 0.003(2) 0.004(3) 0.020(3) C13 0.045(4) 0.026(3) 0.025(3) -0.005(3) -0.019(3) -0.001(3) C14 0.029(3) 0.037(4) 0.038(3) 0.001(3) -0.002(3) -0.002(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 Sb1 Cl7 2.3563(13) . ? Sb1 Cl5 2.3603(14) . ? Sb1 Cl6 2.3605(14) . ? Sb1 Cl3 2.3656(13) . ? Sb1 Cl2 2.3676(14) . ? Sb1 Cl4 2.3817(13) . ? Sb2 Cl10 2.3555(13) . ? Sb2 Cl8 2.3577(13) . ? Sb2 Cl11 2.3636(13) . ? Sb2 Cl9 2.3637(12) . ? Sb2 Cl12 2.3716(13) . ? Sb2 Cl13 2.3719(12) . ? Sc1 O1 2.135(3) . ? Sc1 O4 2.154(3) . ? Sc1 O2 2.155(3) . ? Sc1 O3 2.164(3) . ? Sc1 O5 2.176(3) . ? Sc1 N1 2.272(4) . ? Sc1 Cl1 2.3606(15) . ? O1 C10 1.445(6) . ? O1 C1 1.469(6) . ? O2 C3 1.447(5) . ? O2 C2 1.455(6) . ? O3 C5 1.444(6) . ? O3 C4 1.445(5) . ? O4 C7 1.447(6) . ? O4 C6 1.454(5) . ? O5 C8 1.444(6) . ? O5 C9 1.453(6) . ? N1 C11 1.135(6) . ? N2 C13 1.144(7) . ? C1 C2 1.490(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.498(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.493(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.501(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.477(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.474(7) . ? C13 C14 1.442(9) . ? 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 Cl7 Sb1 Cl5 91.32(5) . . ? Cl7 Sb1 Cl6 90.51(5) . . ? Cl5 Sb1 Cl6 89.81(5) . . ? Cl7 Sb1 Cl3 90.22(5) . . ? Cl5 Sb1 Cl3 89.97(5) . . ? Cl6 Sb1 Cl3 179.25(5) . . ? Cl7 Sb1 Cl2 88.91(5) . . ? Cl5 Sb1 Cl2 179.32(5) . . ? Cl6 Sb1 Cl2 90.83(5) . . ? Cl3 Sb1 Cl2 89.39(5) . . ? Cl7 Sb1 Cl4 177.70(5) . . ? Cl5 Sb1 Cl4 90.78(5) . . ? Cl6 Sb1 Cl4 90.44(5) . . ? Cl3 Sb1 Cl4 88.85(5) . . ? Cl2 Sb1 Cl4 88.98(5) . . ? Cl10 Sb2 Cl8 89.87(5) . . ? Cl10 Sb2 Cl11 89.11(5) . . ? Cl8 Sb2 Cl11 176.93(5) . . ? Cl10 Sb2 Cl9 93.14(5) . . ? Cl8 Sb2 Cl9 88.23(5) . . ? Cl11 Sb2 Cl9 88.95(5) . . ? Cl10 Sb2 Cl12 88.98(5) . . ? Cl8 Sb2 Cl12 91.39(5) . . ? Cl11 Sb2 Cl12 91.48(5) . . ? Cl9 Sb2 Cl12 177.84(5) . . ? Cl10 Sb2 Cl13 176.52(5) . . ? Cl8 Sb2 Cl13 91.40(5) . . ? Cl11 Sb2 Cl13 89.79(5) . . ? Cl9 Sb2 Cl13 90.14(4) . . ? Cl12 Sb2 Cl13 87.75(4) . . ? O1 Sc1 O4 143.24(13) . . ? O1 Sc1 O2 71.22(13) . . ? O4 Sc1 O2 142.70(12) . . ? O1 Sc1 O3 143.00(13) . . ? O4 Sc1 O3 71.46(12) . . ? O2 Sc1 O3 72.14(12) . . ? O1 Sc1 O5 71.68(13) . . ? O4 Sc1 O5 72.53(12) . . ? O2 Sc1 O5 142.61(13) . . ? O3 Sc1 O5 143.88(13) . . ? O1 Sc1 N1 84.74(14) . . ? O4 Sc1 N1 85.02(13) . . ? O2 Sc1 N1 85.65(13) . . ? O3 Sc1 N1 87.64(13) . . ? O5 Sc1 N1 86.54(13) . . ? O1 Sc1 Cl1 93.75(10) . . ? O4 Sc1 Cl1 95.70(10) . . ? O2 Sc1 Cl1 94.71(10) . . ? O3 Sc1 Cl1 94.11(9) . . ? O5 Sc1 Cl1 92.14(9) . . ? N1 Sc1 Cl1 178.24(11) . . ? C10 O1 C1 117.5(4) . . ? C10 O1 Sc1 120.9(3) . . ? C1 O1 Sc1 121.6(3) . . ? C3 O2 C2 114.4(4) . . ? C3 O2 Sc1 117.0(3) . . ? C2 O2 Sc1 115.7(3) . . ? C5 O3 C4 114.8(3) . . ? C5 O3 Sc1 119.4(3) . . ? C4 O3 Sc1 118.0(3) . . ? C7 O4 C6 115.0(3) . . ? C7 O4 Sc1 116.9(3) . . ? C6 O4 Sc1 117.5(3) . . ? C8 O5 C9 112.9(4) . . ? C8 O5 Sc1 117.7(3) . . ? C9 O5 Sc1 115.1(3) . . ? C11 N1 Sc1 177.6(4) . . ? O1 C1 C2 105.6(4) . . ? O1 C1 H1A 110.6 . . ? C2 C1 H1A 110.6 . . ? O1 C1 H1B 110.6 . . ? C2 C1 H1B 110.6 . . ? H1A C1 H1B 108.8 . . ? O2 C2 C1 105.8(4) . . ? O2 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? O2 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? O2 C3 C4 105.7(4) . . ? O2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O3 C4 C3 104.9(4) . . ? O3 C4 H4A 110.8 . . ? C3 C4 H4A 110.8 . . ? O3 C4 H4B 110.8 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.8 . . ? O3 C5 C6 105.4(4) . . ? O3 C5 H5A 110.7 . . ? C6 C5 H5A 110.7 . . ? O3 C5 H5B 110.7 . . ? C6 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? O4 C6 C5 105.2(4) . . ? O4 C6 H6A 110.7 . . ? C5 C6 H6A 110.7 . . ? O4 C6 H6B 110.7 . . ? C5 C6 H6B 110.7 . . ? H6A C6 H6B 108.8 . . ? O4 C7 C8 105.6(4) . . ? O4 C7 H7A 110.6 . . ? C8 C7 H7A 110.6 . . ? O4 C7 H7B 110.6 . . ? C8 C7 H7B 110.6 . . ? H7A C7 H7B 108.8 . . ? O5 C8 C7 106.8(4) . . ? O5 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? O5 C8 H8B 110.4 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? O5 C9 C10 106.2(4) . . ? O5 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O5 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O1 C10 C9 106.9(4) . . ? O1 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? O1 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? N1 C11 C12 179.4(4) . . ? N2 C13 C14 179.6(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Sc1 O1 C10 15.3(5) . . . . ? O2 Sc1 O1 C10 176.8(4) . . . . ? O3 Sc1 O1 C10 168.6(3) . . . . ? O5 Sc1 O1 C10 1.6(3) . . . . ? N1 Sc1 O1 C10 89.7(4) . . . . ? Cl1 Sc1 O1 C10 -89.4(3) . . . . ? O4 Sc1 O1 C1 -163.6(3) . . . . ? O2 Sc1 O1 C1 -2.0(3) . . . . ? O3 Sc1 O1 C1 -10.2(4) . . . . ? O5 Sc1 O1 C1 -177.2(4) . . . . ? N1 Sc1 O1 C1 -89.2(3) . . . . ? Cl1 Sc1 O1 C1 91.7(3) . . . . ? O1 Sc1 O2 C3 168.0(3) . . . . ? O4 Sc1 O2 C3 -30.2(4) . . . . ? O3 Sc1 O2 C3 -17.2(3) . . . . ? O5 Sc1 O2 C3 175.4(3) . . . . ? N1 Sc1 O2 C3 -106.1(3) . . . . ? Cl1 Sc1 O2 C3 75.6(3) . . . . ? O1 Sc1 O2 C2 28.7(3) . . . . ? O4 Sc1 O2 C2 -169.5(3) . . . . ? O3 Sc1 O2 C2 -156.5(3) . . . . ? O5 Sc1 O2 C2 36.1(4) . . . . ? N1 Sc1 O2 C2 114.6(3) . . . . ? Cl1 Sc1 O2 C2 -63.7(3) . . . . ? O1 Sc1 O3 C5 -153.3(3) . . . . ? O4 Sc1 O3 C5 10.3(3) . . . . ? O2 Sc1 O3 C5 -161.5(3) . . . . ? O5 Sc1 O3 C5 5.6(4) . . . . ? N1 Sc1 O3 C5 -75.3(3) . . . . ? Cl1 Sc1 O3 C5 104.9(3) . . . . ? O1 Sc1 O3 C4 -5.6(4) . . . . ? O4 Sc1 O3 C4 157.9(3) . . . . ? O2 Sc1 O3 C4 -13.8(3) . . . . ? O5 Sc1 O3 C4 153.3(3) . . . . ? N1 Sc1 O3 C4 72.4(3) . . . . ? Cl1 Sc1 O3 C4 -107.4(3) . . . . ? O1 Sc1 O4 C7 -33.7(4) . . . . ? O2 Sc1 O4 C7 175.9(3) . . . . ? O3 Sc1 O4 C7 162.8(3) . . . . ? O5 Sc1 O4 C7 -20.1(3) . . . . ? N1 Sc1 O4 C7 -108.0(3) . . . . ? Cl1 Sc1 O4 C7 70.4(3) . . . . ? O1 Sc1 O4 C6 -176.6(3) . . . . ? O2 Sc1 O4 C6 32.9(4) . . . . ? O3 Sc1 O4 C6 19.9(3) . . . . ? O5 Sc1 O4 C6 -163.0(3) . . . . ? N1 Sc1 O4 C6 109.1(3) . . . . ? Cl1 Sc1 O4 C6 -72.5(3) . . . . ? O1 Sc1 O5 C8 162.2(3) . . . . ? O4 Sc1 O5 C8 -9.3(3) . . . . ? O2 Sc1 O5 C8 154.8(3) . . . . ? O3 Sc1 O5 C8 -4.6(4) . . . . ? N1 Sc1 O5 C8 76.6(3) . . . . ? Cl1 Sc1 O5 C8 -104.6(3) . . . . ? O1 Sc1 O5 C9 25.2(3) . . . . ? O4 Sc1 O5 C9 -146.3(3) . . . . ? O2 Sc1 O5 C9 17.8(4) . . . . ? O3 Sc1 O5 C9 -141.6(3) . . . . ? N1 Sc1 O5 C9 -60.4(3) . . . . ? Cl1 Sc1 O5 C9 118.4(3) . . . . ? O1 Sc1 N1 C11 31(10) . . . . ? O4 Sc1 N1 C11 176(100) . . . . ? O2 Sc1 N1 C11 -40(10) . . . . ? O3 Sc1 N1 C11 -112(10) . . . . ? O5 Sc1 N1 C11 103(10) . . . . ? Cl1 Sc1 N1 C11 62(11) . . . . ? C10 O1 C1 C2 158.6(4) . . . . ? Sc1 O1 C1 C2 -22.6(5) . . . . ? C3 O2 C2 C1 170.2(4) . . . . ? Sc1 O2 C2 C1 -49.4(5) . . . . ? O1 C1 C2 O2 42.5(5) . . . . ? C2 O2 C3 C4 -177.5(4) . . . . ? Sc1 O2 C3 C4 42.7(5) . . . . ? C5 O3 C4 C3 -171.6(4) . . . . ? Sc1 O3 C4 C3 39.3(5) . . . . ? O2 C3 C4 O3 -49.3(5) . . . . ? C4 O3 C5 C6 175.6(4) . . . . ? Sc1 O3 C5 C6 -35.7(5) . . . . ? C7 O4 C6 C5 172.2(4) . . . . ? Sc1 O4 C6 C5 -44.1(5) . . . . ? O3 C5 C6 O4 47.4(5) . . . . ? C6 O4 C7 C8 -172.6(4) . . . . ? Sc1 O4 C7 C8 43.6(5) . . . . ? C9 O5 C8 C7 172.3(4) . . . . ? Sc1 O5 C8 C7 34.4(5) . . . . ? O4 C7 C8 O5 -47.2(5) . . . . ? C8 O5 C9 C10 174.6(4) . . . . ? Sc1 O5 C9 C10 -46.3(5) . . . . ? C1 O1 C10 C9 152.8(4) . . . . ? Sc1 O1 C10 C9 -26.1(5) . . . . ? O5 C9 C10 O1 43.6(5) . . . . ? Sc1 N1 C11 C12 -112(66) . . . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 0.942 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.170 #===END OF CIF============================== data_scnc4 _database_code_CSD 196085 _audit_creation_method 'SHELXL-97 + template + hand edit' _chemical_name_systematic ; di(mu-hydroxo)bis(bis(O,O'-nitrato)diaquascandium(III)) (bis(1,4,7,10-tetraoxacyclododecane)sodium) nitrate trihydrate ; _chemical_name_common ? _chemical_formula_moiety 'C16 H32 Na O8 1+, N O3 1-, 3(H2 O), H10 N4 O18 Sc2' _chemical_formula_sum 'C16 H48 N5 Na O32 Sc2' _chemical_formula_weight 935.50 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' 'H' 'H' 0.0000 0.0000 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7342(10) _cell_length_b 13.4735(15) _cell_length_c 16.842(3) _cell_angle_alpha 100.341(4) _cell_angle_beta 98.989(4) _cell_angle_gamma 93.665(7) _cell_volume 1917.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13727 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, Blessing' _exptl_absorpt_correction_T_min 0.8798 # shelxl 0.8619 _exptl_absorpt_correction_T_max 0.8954 # shelxl 0.8857 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa ccd area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26054 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6636 _reflns_number_gt 4294 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+1.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # difmap for O-H, geom for C-H _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6636 _refine_ls_number_parameters 493 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1258 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.051 _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 Sc1 Sc 0.30208(7) 0.32531(5) 0.58926(4) 0.01951(19) Uani 1 d . . . Sc2 Sc 0.20283(7) 0.17043(5) 0.40835(4) 0.01871(19) Uani 1 d . . . Na1 Na 0.24798(14) 0.25187(9) 1.00056(8) 0.0188(3) Uani 1 d . . . N1 N 0.5957(4) 0.3286(2) 0.6795(2) 0.0331(8) Uani 1 d . . . N2 N 0.1832(4) 0.4727(2) 0.68902(19) 0.0288(7) Uani 1 d . . . N3 N 0.3232(4) 0.0260(2) 0.30614(19) 0.0265(7) Uani 1 d . . . N4 N -0.0884(3) 0.1698(2) 0.3160(2) 0.0299(8) Uani 1 d . . . N5A N 0.2814(6) 0.6863(4) 0.5558(3) 0.0124(11) Uiso 0.50 d PD . . N5B N 0.2108(7) 0.8113(5) 0.4427(4) 0.0368(16) Uiso 0.50 d PD . . O1 O 0.5676(3) 0.38254(19) 0.62491(16) 0.0307(6) Uani 1 d . . . O2 O 0.4805(3) 0.27404(19) 0.68969(16) 0.0299(6) Uani 1 d . . . O3 O 0.7266(4) 0.3314(3) 0.7191(2) 0.0632(10) Uani 1 d . . . O4 O 0.3250(3) 0.45331(19) 0.70203(15) 0.0292(6) Uani 1 d . . . O5 O 0.0967(3) 0.4126(2) 0.63101(16) 0.0320(6) Uani 1 d . . . O6 O 0.1354(3) 0.5447(2) 0.72905(17) 0.0427(7) Uani 1 d . . . O7 O 0.1871(3) 0.21588(19) 0.64596(14) 0.0264(6) Uani 1 d . . . O8 O 0.3305(3) 0.45250(19) 0.52995(15) 0.0307(6) Uani 1 d . . . O9 O 0.3815(3) 0.21703(18) 0.50885(14) 0.0219(5) Uani 1 d . . . O10 O 0.1226(2) 0.27653(18) 0.48960(14) 0.0214(5) Uani 1 d . . . O11 O 0.1710(3) 0.04101(19) 0.46493(15) 0.0309(6) Uani 1 d . . . O12 O 0.3219(3) 0.28087(18) 0.35395(14) 0.0247(6) Uani 1 d . . . O13 O 0.4091(3) 0.0818(2) 0.36690(15) 0.0294(6) Uani 1 d . . . O14 O 0.1827(3) 0.04749(18) 0.29303(15) 0.0258(6) Uani 1 d . . . O15 O 0.3708(3) -0.0439(2) 0.26325(17) 0.0372(7) Uani 1 d . . . O16 O -0.0620(3) 0.11388(18) 0.36949(16) 0.0277(6) Uani 1 d . . . O17 O 0.0264(3) 0.22643(18) 0.30889(15) 0.0269(6) Uani 1 d . . . O18 O -0.2171(3) 0.1671(2) 0.2745(2) 0.0571(10) Uani 1 d . . . O19 O 0.3482(3) 0.13278(17) 1.08696(14) 0.0213(5) Uani 1 d . . . O20 O 0.0289(3) 0.15073(17) 1.03627(14) 0.0213(5) Uani 1 d . . . O21 O 0.0825(3) 0.36327(17) 1.07937(14) 0.0220(5) Uani 1 d . . . O22 O 0.4016(3) 0.34548(17) 1.12795(14) 0.0226(6) Uani 1 d . . . O23 O 0.5067(3) 0.24675(17) 0.95498(15) 0.0236(6) Uani 1 d . . . O24 O 0.2468(3) 0.10393(17) 0.89199(14) 0.0228(6) Uani 1 d . . . O25 O 0.0541(3) 0.26270(17) 0.88130(15) 0.0251(6) Uani 1 d . . . O26 O 0.3148(3) 0.40438(17) 0.94538(14) 0.0222(5) Uani 1 d . . . O27A O 0.3796(3) 0.6562(2) 0.59525(19) 0.0447(7) Uiso 0.50 d PD . . O28A O 0.3058(5) 0.7693(3) 0.5365(3) 0.0170(10) Uiso 0.50 d P . . O29A O 0.1524(6) 0.6386(4) 0.5389(3) 0.0370(13) Uiso 0.50 d P . . O27B O 0.1193(4) 0.8353(2) 0.40174(19) 0.0466(8) Uiso 0.50 d PD . . O28B O 0.1847(7) 0.7321(5) 0.4634(4) 0.0477(15) Uiso 0.50 d P . . O29B O 0.3425(8) 0.8598(6) 0.4560(5) 0.071(2) Uiso 0.50 d PD . . O30 O 0.1942(3) 0.4629(2) 0.37346(17) 0.0340(6) Uani 1 d . . . O31 O 0.2994(3) 0.0298(2) 0.62053(17) 0.0332(7) Uani 1 d . . . O32A O 0.3796(3) 0.6562(2) 0.59525(19) 0.0447(7) Uiso 0.50 d P . . O32B O 0.1193(4) 0.8353(2) 0.40174(19) 0.0466(8) Uiso 0.50 d P . . C1 C 0.2283(4) 0.0538(3) 1.0840(2) 0.0232(8) Uani 1 d . . . H1A H 0.2627 0.0131 1.1258 0.0227(17) Uiso 1 calc R . . H1B H 0.2118 0.0085 1.0296 0.0227(17) Uiso 1 calc R . . C2 C 0.0764(4) 0.0949(3) 1.0991(2) 0.0212(8) Uani 1 d . . . H2A H -0.0035 0.0385 1.0971 0.0227(17) Uiso 1 calc R . . H2B H 0.0905 0.1396 1.1537 0.0227(17) Uiso 1 calc R . . C3 C -0.0918(4) 0.2139(3) 1.0537(2) 0.0266(8) Uani 1 d . . . H3A H -0.1700 0.1762 1.0764 0.0227(17) Uiso 1 calc R . . H3B H -0.1444 0.2310 1.0021 0.0227(17) Uiso 1 calc R . . C4 C -0.0297(4) 0.3105(3) 1.1137(2) 0.0255(8) Uani 1 d . . . H4A H -0.1156 0.3529 1.1239 0.0227(17) Uiso 1 calc R . . H4B H 0.0194 0.2946 1.1665 0.0227(17) Uiso 1 calc R . . C5 C 0.1812(4) 0.4393(3) 1.1371(2) 0.0261(8) Uani 1 d . . . H5A H 0.1192 0.4749 1.1758 0.0227(17) Uiso 1 calc R . . H5B H 0.2235 0.4897 1.1080 0.0227(17) Uiso 1 calc R . . C6 C 0.3154(4) 0.3970(3) 1.1849(2) 0.0238(8) Uani 1 d . . . H6A H 0.3831 0.4526 1.2233 0.0227(17) Uiso 1 calc R . . H6B H 0.2751 0.3495 1.2170 0.0227(17) Uiso 1 calc R . . C7 C 0.5046(4) 0.2799(3) 1.1630(2) 0.0254(8) Uani 1 d . . . H7A H 0.5559 0.3145 1.2186 0.0227(17) Uiso 1 calc R . . H7B H 0.5867 0.2660 1.1292 0.0227(17) Uiso 1 calc R . . C8 C 0.4191(4) 0.1811(3) 1.1682(2) 0.0224(8) Uani 1 d . . . H8A H 0.4927 0.1372 1.1923 0.0227(17) Uiso 1 calc R . . H8B H 0.3387 0.1937 1.2032 0.0227(17) Uiso 1 calc R . . C9 C 0.5076(4) 0.1729(3) 0.8826(2) 0.0268(8) Uani 1 d . . . H9A H 0.6147 0.1541 0.8798 0.0227(17) Uiso 1 calc R . . H9B H 0.4692 0.2004 0.8332 0.0227(17) Uiso 1 calc R . . C10 C 0.4020(4) 0.0811(3) 0.8868(2) 0.0268(8) Uani 1 d . . . H10A H 0.4010 0.0284 0.8375 0.0227(17) Uiso 1 calc R . . H10B H 0.4445 0.0532 0.9353 0.0227(17) Uiso 1 calc R . . C11 C 0.1557(4) 0.1112(3) 0.8151(2) 0.0255(8) Uani 1 d . . . H11A H 0.1240 0.0427 0.7816 0.0227(17) Uiso 1 calc R . . H11B H 0.2179 0.1501 0.7846 0.0227(17) Uiso 1 calc R . . C12 C 0.0143(4) 0.1638(3) 0.8316(2) 0.0264(8) Uani 1 d . . . H12A H -0.0494 0.1696 0.7789 0.0227(17) Uiso 1 calc R . . H12B H -0.0495 0.1224 0.8596 0.0227(17) Uiso 1 calc R . . C13 C 0.0955(4) 0.3376(3) 0.8361(2) 0.0250(8) Uani 1 d . . . H13A H 0.0011 0.3566 0.8036 0.0227(17) Uiso 1 calc R . . H13B H 0.1656 0.3110 0.7981 0.0227(17) Uiso 1 calc R . . C14 C 0.1767(4) 0.4286(3) 0.8975(2) 0.0258(8) Uani 1 d . . . H14A H 0.2045 0.4827 0.8682 0.0227(17) Uiso 1 calc R . . H14B H 0.1046 0.4547 0.9344 0.0227(17) Uiso 1 calc R . . C15 C 0.4446(4) 0.3993(3) 0.9031(2) 0.0252(8) Uani 1 d . . . H15A H 0.4873 0.4683 0.9007 0.0227(17) Uiso 1 calc R . . H15B H 0.4121 0.3608 0.8464 0.0227(17) Uiso 1 calc R . . C16 C 0.5662(4) 0.3466(3) 0.9498(2) 0.0280(9) Uani 1 d . . . H16A H 0.6582 0.3421 0.9221 0.0227(17) Uiso 1 calc R . . H16B H 0.6002 0.3871 1.0057 0.0227(17) Uiso 1 calc R . . H7X H 0.2296 0.1537 0.6449 0.023 Uiso 1 d . . . H7Y H 0.0982 0.1958 0.6265 0.023 Uiso 1 d . . . H8X H 0.2613 0.4584 0.4816 0.023 Uiso 1 d . . . H8Y H 0.3522 0.5208 0.5626 0.023 Uiso 1 d . . . H9X H 0.4700 0.1937 0.5020 0.023 Uiso 1 d . . . H10X H 0.0311 0.3006 0.4995 0.023 Uiso 1 d . . . H11X H 0.1518 -0.0276 0.4395 0.023 Uiso 1 d . . . H11Y H 0.2320 0.0384 0.5153 0.023 Uiso 1 d . . . H12X H 0.2802 0.3386 0.3575 0.023 Uiso 1 d . . . H12Y H 0.4155 0.3009 0.3760 0.023 Uiso 1 d . . . H30X H 0.2560 0.5204 0.3691 0.023 Uiso 1 d . . . H30Y H 0.0849 0.4602 0.3537 0.023 Uiso 1 d . . . H31X H 0.2450 -0.0212 0.6383 0.023 Uiso 1 d . . . H31Y H 0.3984 0.0292 0.6345 0.023 Uiso 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 0.0167(3) 0.0262(4) 0.0147(4) 0.0036(3) 0.0005(3) 0.0019(3) Sc2 0.0157(3) 0.0251(4) 0.0147(4) 0.0037(3) 0.0009(3) 0.0016(3) Na1 0.0229(7) 0.0182(6) 0.0157(7) 0.0040(5) 0.0032(5) 0.0038(5) N1 0.0274(19) 0.0302(17) 0.036(2) 0.0041(16) -0.0091(16) 0.0031(15) N2 0.0316(19) 0.0359(18) 0.0210(18) 0.0095(15) 0.0040(15) 0.0092(16) N3 0.0260(17) 0.0308(17) 0.0246(19) 0.0103(15) 0.0033(15) 0.0066(15) N4 0.0209(18) 0.0293(17) 0.034(2) 0.0031(15) -0.0099(15) 0.0042(15) O1 0.0240(13) 0.0326(14) 0.0317(16) 0.0051(12) -0.0043(11) -0.0013(11) O2 0.0296(15) 0.0294(14) 0.0275(15) 0.0064(11) -0.0046(12) 0.0006(12) O3 0.0330(17) 0.061(2) 0.080(3) 0.0168(19) -0.0381(17) -0.0068(15) O4 0.0291(14) 0.0344(14) 0.0201(14) -0.0005(11) -0.0029(11) 0.0070(12) O5 0.0234(14) 0.0483(16) 0.0233(15) 0.0024(13) 0.0030(12) 0.0090(13) O6 0.0537(18) 0.0413(16) 0.0357(18) 0.0012(14) 0.0157(14) 0.0229(15) O7 0.0247(13) 0.0361(14) 0.0186(14) 0.0085(11) 0.0023(11) -0.0004(11) O8 0.0298(14) 0.0361(15) 0.0253(15) 0.0102(12) -0.0008(11) -0.0017(12) O9 0.0148(12) 0.0330(13) 0.0173(13) 0.0043(10) 0.0011(10) 0.0046(10) O10 0.0149(11) 0.0332(13) 0.0155(13) 0.0031(10) 0.0017(10) 0.0035(10) O11 0.0311(14) 0.0358(14) 0.0255(15) 0.0137(12) -0.0026(12) -0.0030(12) O12 0.0222(13) 0.0328(13) 0.0190(14) 0.0066(11) 0.0025(10) -0.0007(11) O13 0.0224(13) 0.0426(15) 0.0203(14) 0.0015(12) -0.0006(11) 0.0037(12) O14 0.0220(13) 0.0294(13) 0.0243(15) 0.0018(11) 0.0000(11) 0.0077(11) O15 0.0426(16) 0.0377(15) 0.0331(17) 0.0024(13) 0.0124(13) 0.0168(14) O16 0.0208(13) 0.0308(14) 0.0304(15) 0.0092(12) -0.0021(11) 0.0013(11) O17 0.0259(14) 0.0267(13) 0.0244(15) 0.0036(11) -0.0043(11) -0.0002(12) O18 0.0303(17) 0.059(2) 0.074(2) 0.0275(18) -0.0292(16) -0.0037(15) O19 0.0222(13) 0.0215(12) 0.0184(13) 0.0011(10) 0.0011(10) 0.0012(10) O20 0.0220(12) 0.0194(11) 0.0235(14) 0.0052(10) 0.0036(10) 0.0065(10) O21 0.0258(13) 0.0190(12) 0.0221(14) 0.0046(10) 0.0066(11) 0.0015(10) O22 0.0253(13) 0.0215(12) 0.0212(14) 0.0035(10) 0.0040(10) 0.0055(10) O23 0.0303(14) 0.0174(12) 0.0244(14) 0.0028(10) 0.0085(11) 0.0056(11) O24 0.0304(14) 0.0218(12) 0.0173(13) 0.0045(10) 0.0052(11) 0.0048(11) O25 0.0308(14) 0.0203(12) 0.0242(14) 0.0041(10) 0.0047(11) 0.0026(11) O26 0.0238(13) 0.0215(12) 0.0215(14) 0.0037(10) 0.0039(10) 0.0047(10) O30 0.0233(14) 0.0445(16) 0.0374(17) 0.0171(13) 0.0038(12) 0.0044(12) O31 0.0182(13) 0.0483(16) 0.0380(17) 0.0224(13) 0.0027(12) 0.0044(12) C1 0.028(2) 0.0171(17) 0.024(2) 0.0047(15) 0.0016(16) 0.0029(15) C2 0.0244(18) 0.0209(17) 0.019(2) 0.0064(15) 0.0034(15) 0.0014(15) C3 0.0190(18) 0.0259(19) 0.035(2) 0.0057(16) 0.0034(16) 0.0050(16) C4 0.032(2) 0.0223(18) 0.025(2) 0.0056(15) 0.0114(17) 0.0069(16) C5 0.034(2) 0.0204(18) 0.024(2) 0.0026(15) 0.0092(17) 0.0037(16) C6 0.033(2) 0.0210(17) 0.0163(19) -0.0008(14) 0.0034(16) 0.0046(16) C7 0.0206(18) 0.0259(19) 0.027(2) 0.0020(16) 0.0005(16) 0.0015(16) C8 0.0279(19) 0.0236(18) 0.0147(19) 0.0043(15) -0.0018(15) 0.0071(15) C9 0.032(2) 0.0248(18) 0.025(2) 0.0012(16) 0.0108(17) 0.0095(16) C10 0.034(2) 0.0223(18) 0.026(2) 0.0042(16) 0.0079(17) 0.0104(17) C11 0.039(2) 0.0189(17) 0.0147(19) 0.0004(14) -0.0016(16) -0.0012(16) C12 0.030(2) 0.0210(18) 0.023(2) 0.0008(15) -0.0032(16) -0.0044(16) C13 0.031(2) 0.0226(18) 0.022(2) 0.0086(15) -0.0014(16) 0.0046(16) C14 0.029(2) 0.0202(18) 0.029(2) 0.0092(16) 0.0007(17) 0.0059(16) C15 0.032(2) 0.0202(18) 0.026(2) 0.0053(15) 0.0105(17) 0.0028(16) C16 0.026(2) 0.0204(18) 0.037(2) 0.0037(16) 0.0055(17) -0.0020(16) _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 O9 2.039(2) . ? Sc1 O10 2.087(2) . ? Sc1 O8 2.153(3) . ? Sc1 O7 2.170(2) . ? Sc1 O4 2.298(3) . ? Sc1 O5 2.337(2) . ? Sc1 O2 2.345(2) . ? Sc1 O1 2.346(3) . ? Sc1 N2 2.731(3) . ? Sc1 N1 2.763(3) . ? Sc1 Sc2 3.3242(10) . ? Sc2 O10 2.033(2) . ? Sc2 O9 2.089(2) . ? Sc2 O11 2.155(3) . ? Sc2 O12 2.174(2) . ? Sc2 O14 2.291(2) . ? Sc2 O16 2.341(2) . ? Sc2 O13 2.352(2) . ? Sc2 O17 2.355(2) . ? Sc2 N3 2.735(3) . ? Sc2 N4 2.765(3) . ? Na1 O22 2.431(3) . ? Na1 O25 2.449(3) . ? Na1 O24 2.449(3) . ? Na1 O19 2.465(3) . ? Na1 O26 2.475(3) . ? Na1 O20 2.490(3) . ? Na1 O23 2.499(3) . ? Na1 O21 2.503(3) . ? N1 O3 1.225(4) . ? N1 O2 1.260(4) . ? N1 O1 1.276(4) . ? N2 O6 1.214(4) . ? N2 O5 1.261(4) . ? N2 O4 1.275(4) . ? N3 O15 1.217(4) . ? N3 O13 1.260(4) . ? N3 O14 1.274(4) . ? N4 O18 1.223(4) . ? N4 O17 1.255(4) . ? N4 O16 1.277(4) . ? N5A O27A 1.143(5) . ? N5A O29A 1.226(7) . ? N5A O28A 1.234(7) . ? N5B O27B 1.076(6) . ? N5B O28B 1.200(8) . ? N5B O29B 1.254(7) . ? O7 H7X 0.9362 . ? O7 H7Y 0.8034 . ? O8 H8X 0.9542 . ? O8 H8Y 0.9740 . ? O9 H9X 0.8693 . ? O10 H10X 0.9095 . ? O11 H11X 0.9390 . ? O11 H11Y 0.9364 . ? O12 H12X 0.8761 . ? O12 H12Y 0.8485 . ? O19 C8 1.430(4) . ? O19 C1 1.432(4) . ? O20 C3 1.430(4) . ? O20 C2 1.431(4) . ? O21 C5 1.416(4) . ? O21 C4 1.427(4) . ? O22 C6 1.422(4) . ? O22 C7 1.436(4) . ? O23 C9 1.431(4) . ? O23 C16 1.434(4) . ? O24 C10 1.421(4) . ? O24 C11 1.432(4) . ? O25 C13 1.429(4) . ? O25 C12 1.430(4) . ? O26 C15 1.429(4) . ? O26 C14 1.432(4) . ? O28A O28B 1.480(8) . ? O30 H30X 0.9367 . ? O30 H30Y 0.9565 . ? O31 H31X 0.9291 . ? O31 H31Y 0.8609 . ? C1 C2 1.510(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.518(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.508(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.514(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.502(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.510(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.513(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? 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 O9 Sc1 O10 72.52(9) . . ? O9 Sc1 O8 99.33(10) . . ? O10 Sc1 O8 82.82(10) . . ? O9 Sc1 O7 93.78(10) . . ? O10 Sc1 O7 85.07(9) . . ? O8 Sc1 O7 158.56(10) . . ? O9 Sc1 O4 155.20(9) . . ? O10 Sc1 O4 131.71(9) . . ? O8 Sc1 O4 81.39(10) . . ? O7 Sc1 O4 93.74(10) . . ? O9 Sc1 O5 149.77(10) . . ? O10 Sc1 O5 77.69(9) . . ? O8 Sc1 O5 81.63(10) . . ? O7 Sc1 O5 78.54(9) . . ? O4 Sc1 O5 55.02(9) . . ? O9 Sc1 O2 85.25(9) . . ? O10 Sc1 O2 145.16(9) . . ? O8 Sc1 O2 128.05(10) . . ? O7 Sc1 O2 69.65(9) . . ? O4 Sc1 O2 75.32(9) . . ? O5 Sc1 O2 118.11(10) . . ? O9 Sc1 O1 82.52(9) . . ? O10 Sc1 O1 143.12(9) . . ? O8 Sc1 O1 74.80(9) . . ? O7 Sc1 O1 124.03(9) . . ? O4 Sc1 O1 73.71(9) . . ? O5 Sc1 O1 126.06(10) . . ? O2 Sc1 O1 54.38(9) . . ? O9 Sc1 N2 176.47(9) . . ? O10 Sc1 N2 104.29(9) . . ? O8 Sc1 N2 78.60(10) . . ? O7 Sc1 N2 87.38(9) . . ? O4 Sc1 N2 27.71(9) . . ? O5 Sc1 N2 27.42(9) . . ? O2 Sc1 N2 98.27(9) . . ? O1 Sc1 N2 99.60(10) . . ? O9 Sc1 N1 83.07(9) . . ? O10 Sc1 N1 155.59(10) . . ? O8 Sc1 N1 101.69(10) . . ? O7 Sc1 N1 96.65(10) . . ? O4 Sc1 N1 72.60(9) . . ? O5 Sc1 N1 126.59(10) . . ? O2 Sc1 N1 26.99(9) . . ? O1 Sc1 N1 27.39(9) . . ? N2 Sc1 N1 100.11(10) . . ? O9 Sc1 Sc2 36.86(6) . . ? O10 Sc1 Sc2 35.66(6) . . ? O8 Sc1 Sc2 90.59(7) . . ? O7 Sc1 Sc2 89.81(7) . . ? O4 Sc1 Sc2 166.51(7) . . ? O5 Sc1 Sc2 113.26(7) . . ? O2 Sc1 Sc2 118.06(7) . . ? O1 Sc1 Sc2 114.75(7) . . ? N2 Sc1 Sc2 139.90(7) . . ? N1 Sc1 Sc2 119.93(7) . . ? O10 Sc2 O9 72.61(9) . . ? O10 Sc2 O11 99.18(10) . . ? O9 Sc2 O11 83.20(10) . . ? O10 Sc2 O12 94.37(9) . . ? O9 Sc2 O12 84.75(9) . . ? O11 Sc2 O12 158.26(10) . . ? O10 Sc2 O14 155.28(9) . . ? O9 Sc2 O14 131.78(9) . . ? O11 Sc2 O14 82.38(10) . . ? O12 Sc2 O14 92.36(9) . . ? O10 Sc2 O16 82.87(9) . . ? O9 Sc2 O16 143.89(9) . . ? O11 Sc2 O16 74.85(9) . . ? O12 Sc2 O16 123.98(9) . . ? O14 Sc2 O16 73.68(9) . . ? O10 Sc2 O13 149.83(9) . . ? O9 Sc2 O13 77.51(9) . . ? O11 Sc2 O13 81.11(10) . . ? O12 Sc2 O13 78.66(9) . . ? O14 Sc2 O13 54.89(9) . . ? O16 Sc2 O13 125.45(9) . . ? O10 Sc2 O17 84.83(9) . . ? O9 Sc2 O17 144.50(9) . . ? O11 Sc2 O17 128.20(9) . . ? O12 Sc2 O17 69.72(9) . . ? O14 Sc2 O17 75.27(8) . . ? O16 Sc2 O17 54.28(9) . . ? O13 Sc2 O17 118.88(9) . . ? O10 Sc2 N3 176.76(9) . . ? O9 Sc2 N3 104.36(9) . . ? O11 Sc2 N3 79.18(10) . . ? O12 Sc2 N3 86.40(9) . . ? O14 Sc2 N3 27.59(9) . . ? O16 Sc2 N3 99.31(9) . . ? O13 Sc2 N3 27.38(9) . . ? O17 Sc2 N3 98.38(9) . . ? O10 Sc2 N4 83.37(9) . . ? O9 Sc2 N4 155.97(9) . . ? O11 Sc2 N4 101.77(10) . . ? O12 Sc2 N4 96.59(10) . . ? O14 Sc2 N4 72.23(9) . . ? O16 Sc2 N4 27.39(9) . . ? O13 Sc2 N4 126.36(9) . . ? O17 Sc2 N4 26.89(9) . . ? N3 Sc2 N4 99.67(9) . . ? O10 Sc2 Sc1 36.77(6) . . ? O9 Sc2 Sc1 35.85(6) . . ? O11 Sc2 Sc1 91.94(7) . . ? O12 Sc2 Sc1 88.79(7) . . ? O14 Sc2 Sc1 167.38(6) . . ? O16 Sc2 Sc1 115.80(7) . . ? O13 Sc2 Sc1 113.21(7) . . ? O17 Sc2 Sc1 116.77(6) . . ? N3 Sc2 Sc1 140.21(7) . . ? N4 Sc2 Sc1 120.12(7) . . ? O22 Na1 O25 145.19(9) . . ? O22 Na1 O24 142.31(9) . . ? O25 Na1 O24 70.25(8) . . ? O22 Na1 O19 70.20(8) . . ? O25 Na1 O19 142.31(9) . . ? O24 Na1 O19 81.57(8) . . ? O22 Na1 O26 84.51(9) . . ? O25 Na1 O26 69.75(8) . . ? O24 Na1 O26 107.47(9) . . ? O19 Na1 O26 145.08(9) . . ? O22 Na1 O20 107.51(9) . . ? O25 Na1 O20 82.89(9) . . ? O24 Na1 O20 84.21(9) . . ? O19 Na1 O20 69.50(8) . . ? O26 Na1 O20 143.51(9) . . ? O22 Na1 O23 83.13(9) . . ? O25 Na1 O23 107.32(9) . . ? O24 Na1 O23 69.42(8) . . ? O19 Na1 O23 84.46(8) . . ? O26 Na1 O23 68.51(8) . . ? O20 Na1 O23 145.46(9) . . ? O22 Na1 O21 69.64(8) . . ? O25 Na1 O21 84.57(9) . . ? O24 Na1 O21 145.12(9) . . ? O19 Na1 O21 107.31(9) . . ? O26 Na1 O21 84.72(8) . . ? O20 Na1 O21 68.63(8) . . ? O23 Na1 O21 143.55(9) . . ? O3 N1 O2 123.3(3) . . ? O3 N1 O1 121.2(3) . . ? O2 N1 O1 115.5(3) . . ? O3 N1 Sc1 179.0(3) . . ? O2 N1 Sc1 57.69(16) . . ? O1 N1 Sc1 57.79(16) . . ? O6 N2 O5 122.4(3) . . ? O6 N2 O4 122.4(3) . . ? O5 N2 O4 115.2(3) . . ? O6 N2 Sc1 173.8(3) . . ? O5 N2 Sc1 58.63(16) . . ? O4 N2 Sc1 56.93(16) . . ? O15 N3 O13 122.4(3) . . ? O15 N3 O14 122.4(3) . . ? O13 N3 O14 115.3(3) . . ? O15 N3 Sc2 174.9(2) . . ? O13 N3 Sc2 59.11(16) . . ? O14 N3 Sc2 56.41(16) . . ? O18 N4 O17 122.7(3) . . ? O18 N4 O16 121.7(3) . . ? O17 N4 O16 115.5(3) . . ? O18 N4 Sc2 178.5(3) . . ? O17 N4 Sc2 58.05(15) . . ? O16 N4 Sc2 57.50(15) . . ? O27A N5A O29A 118.9(5) . . ? O27A N5A O28A 118.7(5) . . ? O29A N5A O28A 122.1(5) . . ? O27B N5B O28B 117.0(7) . . ? O27B N5B O29B 118.0(7) . . ? O28B N5B O29B 124.2(7) . . ? N1 O1 Sc1 94.8(2) . . ? N1 O2 Sc1 95.3(2) . . ? N2 O4 Sc1 95.4(2) . . ? N2 O5 Sc1 93.94(19) . . ? Sc1 O7 H7X 116.5 . . ? Sc1 O7 H7Y 117.3 . . ? H7X O7 H7Y 99.5 . . ? Sc1 O8 H8X 121.3 . . ? Sc1 O8 H8Y 119.8 . . ? H8X O8 H8Y 105.7 . . ? Sc1 O9 Sc2 107.29(10) . . ? Sc1 O9 H9X 137.5 . . ? Sc2 O9 H9X 114.3 . . ? Sc2 O10 Sc1 107.57(10) . . ? Sc2 O10 H10X 139.5 . . ? Sc1 O10 H10X 111.9 . . ? Sc2 O11 H11X 128.0 . . ? Sc2 O11 H11Y 120.0 . . ? H11X O11 H11Y 102.7 . . ? Sc2 O12 H12X 113.4 . . ? Sc2 O12 H12Y 116.3 . . ? H12X O12 H12Y 101.0 . . ? N3 O13 Sc2 93.51(18) . . ? N3 O14 Sc2 96.00(19) . . ? N4 O16 Sc2 95.11(19) . . ? N4 O17 Sc2 95.06(19) . . ? C8 O19 C1 113.8(3) . . ? C8 O19 Na1 113.63(18) . . ? C1 O19 Na1 109.50(18) . . ? C3 O20 C2 113.3(3) . . ? C3 O20 Na1 109.89(19) . . ? C2 O20 Na1 113.67(19) . . ? C5 O21 C4 113.9(3) . . ? C5 O21 Na1 108.55(19) . . ? C4 O21 Na1 114.69(18) . . ? C6 O22 C7 112.8(3) . . ? C6 O22 Na1 115.5(2) . . ? C7 O22 Na1 109.14(19) . . ? C9 O23 C16 113.5(3) . . ? C9 O23 Na1 113.9(2) . . ? C16 O23 Na1 110.15(19) . . ? C10 O24 C11 113.9(3) . . ? C10 O24 Na1 109.9(2) . . ? C11 O24 Na1 113.84(19) . . ? C13 O25 C12 113.2(3) . . ? C13 O25 Na1 114.8(2) . . ? C12 O25 Na1 109.09(19) . . ? C15 O26 C14 113.1(3) . . ? C15 O26 Na1 115.41(18) . . ? C14 O26 Na1 108.26(19) . . ? N5A O28A O28B 86.9(4) . . ? N5B O28B O28A 87.6(5) . . ? H30X O30 H30Y 117.0 . . ? H31X O31 H31Y 111.3 . . ? O19 C1 C2 112.3(3) . . ? O19 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? O19 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? O20 C2 C1 107.4(3) . . ? O20 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O20 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O20 C3 C4 112.0(3) . . ? O20 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O20 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O21 C4 C3 108.0(3) . . ? O21 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O21 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? O21 C5 C6 112.7(3) . . ? O21 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? O21 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? O22 C6 C5 108.0(3) . . ? O22 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O22 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? O22 C7 C8 111.8(3) . . ? O22 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? O22 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? O19 C8 C7 107.8(3) . . ? O19 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? O19 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O23 C9 C10 107.3(3) . . ? O23 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O23 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? O24 C10 C9 112.7(3) . . ? O24 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? O24 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? O24 C11 C12 108.4(3) . . ? O24 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? O24 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? O25 C12 C11 112.2(3) . . ? O25 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? O25 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O25 C13 C14 107.2(3) . . ? O25 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? O25 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.5 . . ? O26 C14 C13 112.0(3) . . ? O26 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? O26 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? O26 C15 C16 107.4(3) . . ? O26 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O26 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? O23 C16 C15 111.4(3) . . ? O23 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? O23 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Sc1 Sc2 O10 178.36(16) . . . . ? O8 Sc1 Sc2 O10 -76.77(13) . . . . ? O7 Sc1 Sc2 O10 81.79(13) . . . . ? O4 Sc1 Sc2 O10 -23.6(3) . . . . ? O5 Sc1 Sc2 O10 4.37(13) . . . . ? O2 Sc1 Sc2 O10 148.48(14) . . . . ? O1 Sc1 Sc2 O10 -150.27(14) . . . . ? N2 Sc1 Sc2 O10 -3.91(15) . . . . ? N1 Sc1 Sc2 O10 179.36(14) . . . . ? O10 Sc1 Sc2 O9 -178.36(16) . . . . ? O8 Sc1 Sc2 O9 104.87(13) . . . . ? O7 Sc1 Sc2 O9 -96.56(13) . . . . ? O4 Sc1 Sc2 O9 158.1(3) . . . . ? O5 Sc1 Sc2 O9 -173.99(14) . . . . ? O2 Sc1 Sc2 O9 -29.88(14) . . . . ? O1 Sc1 Sc2 O9 31.37(13) . . . . ? N2 Sc1 Sc2 O9 177.73(15) . . . . ? N1 Sc1 Sc2 O9 1.00(14) . . . . ? O9 Sc1 Sc2 O11 75.58(13) . . . . ? O10 Sc1 Sc2 O11 -102.78(13) . . . . ? O8 Sc1 Sc2 O11 -179.55(9) . . . . ? O7 Sc1 Sc2 O11 -20.99(10) . . . . ? O4 Sc1 Sc2 O11 -126.4(3) . . . . ? O5 Sc1 Sc2 O11 -98.41(10) . . . . ? O2 Sc1 Sc2 O11 45.70(11) . . . . ? O1 Sc1 Sc2 O11 106.94(10) . . . . ? N2 Sc1 Sc2 O11 -106.69(13) . . . . ? N1 Sc1 Sc2 O11 76.58(11) . . . . ? O9 Sc1 Sc2 O12 -82.69(13) . . . . ? O10 Sc1 Sc2 O12 98.95(13) . . . . ? O8 Sc1 Sc2 O12 22.18(9) . . . . ? O7 Sc1 Sc2 O12 -179.25(9) . . . . ? O4 Sc1 Sc2 O12 75.4(3) . . . . ? O5 Sc1 Sc2 O12 103.32(10) . . . . ? O2 Sc1 Sc2 O12 -112.57(10) . . . . ? O1 Sc1 Sc2 O12 -51.32(10) . . . . ? N2 Sc1 Sc2 O12 95.04(13) . . . . ? N1 Sc1 Sc2 O12 -81.69(11) . . . . ? O9 Sc1 Sc2 O14 12.7(3) . . . . ? O10 Sc1 Sc2 O14 -165.6(3) . . . . ? O8 Sc1 Sc2 O14 117.6(3) . . . . ? O7 Sc1 Sc2 O14 -83.8(3) . . . . ? O4 Sc1 Sc2 O14 170.8(4) . . . . ? O5 Sc1 Sc2 O14 -161.3(3) . . . . ? O2 Sc1 Sc2 O14 -17.2(3) . . . . ? O1 Sc1 Sc2 O14 44.1(3) . . . . ? N2 Sc1 Sc2 O14 -169.5(3) . . . . ? N1 Sc1 Sc2 O14 13.7(3) . . . . ? O9 Sc1 Sc2 O16 149.67(13) . . . . ? O10 Sc1 Sc2 O16 -28.69(13) . . . . ? O8 Sc1 Sc2 O16 -105.46(10) . . . . ? O7 Sc1 Sc2 O16 53.10(10) . . . . ? O4 Sc1 Sc2 O16 -52.3(3) . . . . ? O5 Sc1 Sc2 O16 -24.32(11) . . . . ? O2 Sc1 Sc2 O16 119.79(10) . . . . ? O1 Sc1 Sc2 O16 -178.96(10) . . . . ? N2 Sc1 Sc2 O16 -32.60(13) . . . . ? N1 Sc1 Sc2 O16 150.67(11) . . . . ? O9 Sc1 Sc2 O13 -5.58(13) . . . . ? O10 Sc1 Sc2 O13 176.06(13) . . . . ? O8 Sc1 Sc2 O13 99.29(10) . . . . ? O7 Sc1 Sc2 O13 -102.14(10) . . . . ? O4 Sc1 Sc2 O13 152.5(3) . . . . ? O5 Sc1 Sc2 O13 -179.57(10) . . . . ? O2 Sc1 Sc2 O13 -35.46(11) . . . . ? O1 Sc1 Sc2 O13 25.79(11) . . . . ? N2 Sc1 Sc2 O13 172.15(13) . . . . ? N1 Sc1 Sc2 O13 -4.58(12) . . . . ? O9 Sc1 Sc2 O17 -149.18(14) . . . . ? O10 Sc1 Sc2 O17 32.46(13) . . . . ? O8 Sc1 Sc2 O17 -44.31(10) . . . . ? O7 Sc1 Sc2 O17 114.25(10) . . . . ? O4 Sc1 Sc2 O17 8.9(3) . . . . ? O5 Sc1 Sc2 O17 36.83(11) . . . . ? O2 Sc1 Sc2 O17 -179.06(10) . . . . ? O1 Sc1 Sc2 O17 -117.81(10) . . . . ? N2 Sc1 Sc2 O17 28.55(13) . . . . ? N1 Sc1 Sc2 O17 -148.18(11) . . . . ? O9 Sc1 Sc2 N3 0.23(15) . . . . ? O10 Sc1 Sc2 N3 -178.13(15) . . . . ? O8 Sc1 Sc2 N3 105.10(12) . . . . ? O7 Sc1 Sc2 N3 -96.34(12) . . . . ? O4 Sc1 Sc2 N3 158.3(3) . . . . ? O5 Sc1 Sc2 N3 -173.76(13) . . . . ? O2 Sc1 Sc2 N3 -29.65(13) . . . . ? O1 Sc1 Sc2 N3 31.59(13) . . . . ? N2 Sc1 Sc2 N3 177.96(14) . . . . ? N1 Sc1 Sc2 N3 1.23(14) . . . . ? O9 Sc1 Sc2 N4 -179.61(14) . . . . ? O10 Sc1 Sc2 N4 2.03(14) . . . . ? O8 Sc1 Sc2 N4 -74.74(11) . . . . ? O7 Sc1 Sc2 N4 83.82(11) . . . . ? O4 Sc1 Sc2 N4 -21.6(3) . . . . ? O5 Sc1 Sc2 N4 6.40(12) . . . . ? O2 Sc1 Sc2 N4 150.51(12) . . . . ? O1 Sc1 Sc2 N4 -148.25(11) . . . . ? N2 Sc1 Sc2 N4 -1.88(14) . . . . ? N1 Sc1 Sc2 N4 -178.61(12) . . . . ? O9 Sc1 N1 O3 99(18) . . . . ? O10 Sc1 N1 O3 99(17) . . . . ? O8 Sc1 N1 O3 1(18) . . . . ? O7 Sc1 N1 O3 -168(18) . . . . ? O4 Sc1 N1 O3 -76(18) . . . . ? O5 Sc1 N1 O3 -87(18) . . . . ? O2 Sc1 N1 O3 -168(18) . . . . ? O1 Sc1 N1 O3 12(17) . . . . ? N2 Sc1 N1 O3 -80(18) . . . . ? Sc2 Sc1 N1 O3 98(18) . . . . ? O9 Sc1 N1 O2 -93.1(2) . . . . ? O10 Sc1 N1 O2 -92.8(3) . . . . ? O8 Sc1 N1 O2 168.7(2) . . . . ? O7 Sc1 N1 O2 -0.1(2) . . . . ? O4 Sc1 N1 O2 91.7(2) . . . . ? O5 Sc1 N1 O2 80.5(2) . . . . ? O1 Sc1 N1 O2 179.8(3) . . . . ? N2 Sc1 N1 O2 88.4(2) . . . . ? Sc2 Sc1 N1 O2 -93.7(2) . . . . ? O9 Sc1 N1 O1 87.1(2) . . . . ? O10 Sc1 N1 O1 87.4(3) . . . . ? O8 Sc1 N1 O1 -11.1(2) . . . . ? O7 Sc1 N1 O1 -179.9(2) . . . . ? O4 Sc1 N1 O1 -88.0(2) . . . . ? O5 Sc1 N1 O1 -99.3(2) . . . . ? O2 Sc1 N1 O1 -179.8(3) . . . . ? N2 Sc1 N1 O1 -91.4(2) . . . . ? Sc2 Sc1 N1 O1 86.5(2) . . . . ? O9 Sc1 N2 O6 -62(3) . . . . ? O10 Sc1 N2 O6 -87(2) . . . . ? O8 Sc1 N2 O6 -7(2) . . . . ? O7 Sc1 N2 O6 -171(2) . . . . ? O4 Sc1 N2 O6 86(2) . . . . ? O5 Sc1 N2 O6 -101(2) . . . . ? O2 Sc1 N2 O6 120(2) . . . . ? O1 Sc1 N2 O6 65(2) . . . . ? N1 Sc1 N2 O6 93(2) . . . . ? Sc2 Sc1 N2 O6 -84(2) . . . . ? O9 Sc1 N2 O5 39.4(17) . . . . ? O10 Sc1 N2 O5 14.3(2) . . . . ? O8 Sc1 N2 O5 93.8(2) . . . . ? O7 Sc1 N2 O5 -69.9(2) . . . . ? O4 Sc1 N2 O5 -173.0(3) . . . . ? O2 Sc1 N2 O5 -138.9(2) . . . . ? O1 Sc1 N2 O5 166.0(2) . . . . ? N1 Sc1 N2 O5 -166.2(2) . . . . ? Sc2 Sc1 N2 O5 16.7(2) . . . . ? O9 Sc1 N2 O4 -147.6(15) . . . . ? O10 Sc1 N2 O4 -172.62(19) . . . . ? O8 Sc1 N2 O4 -93.2(2) . . . . ? O7 Sc1 N2 O4 103.1(2) . . . . ? O5 Sc1 N2 O4 173.0(3) . . . . ? O2 Sc1 N2 O4 34.1(2) . . . . ? O1 Sc1 N2 O4 -21.0(2) . . . . ? N1 Sc1 N2 O4 6.9(2) . . . . ? Sc2 Sc1 N2 O4 -170.27(16) . . . . ? O10 Sc2 N3 O15 76(3) . . . . ? O9 Sc2 N3 O15 97(3) . . . . ? O11 Sc2 N3 O15 17(3) . . . . ? O12 Sc2 N3 O15 -180(100) . . . . ? O14 Sc2 N3 O15 -78(3) . . . . ? O16 Sc2 N3 O15 -56(3) . . . . ? O13 Sc2 N3 O15 108(3) . . . . ? O17 Sc2 N3 O15 -111(3) . . . . ? N4 Sc2 N3 O15 -84(3) . . . . ? Sc1 Sc2 N3 O15 97(3) . . . . ? O10 Sc2 N3 O13 -31.9(17) . . . . ? O9 Sc2 N3 O13 -11.5(2) . . . . ? O11 Sc2 N3 O13 -91.5(2) . . . . ? O12 Sc2 N3 O13 72.11(19) . . . . ? O14 Sc2 N3 O13 174.2(3) . . . . ? O16 Sc2 N3 O13 -164.03(19) . . . . ? O17 Sc2 N3 O13 140.99(19) . . . . ? N4 Sc2 N3 O13 168.19(19) . . . . ? Sc1 Sc2 N3 O13 -11.7(2) . . . . ? O10 Sc2 N3 O14 153.9(16) . . . . ? O9 Sc2 N3 O14 174.28(19) . . . . ? O11 Sc2 N3 O14 94.26(19) . . . . ? O12 Sc2 N3 O14 -102.08(19) . . . . ? O16 Sc2 N3 O14 21.8(2) . . . . ? O13 Sc2 N3 O14 -174.2(3) . . . . ? O17 Sc2 N3 O14 -33.2(2) . . . . ? N4 Sc2 N3 O14 -6.0(2) . . . . ? Sc1 Sc2 N3 O14 174.14(15) . . . . ? O10 Sc2 N4 O18 -146(11) . . . . ? O9 Sc2 N4 O18 -148(11) . . . . ? O11 Sc2 N4 O18 -48(11) . . . . ? O12 Sc2 N4 O18 120(11) . . . . ? O14 Sc2 N4 O18 30(11) . . . . ? O16 Sc2 N4 O18 -59(11) . . . . ? O13 Sc2 N4 O18 39(11) . . . . ? O17 Sc2 N4 O18 122(11) . . . . ? N3 Sc2 N4 O18 33(11) . . . . ? Sc1 Sc2 N4 O18 -148(11) . . . . ? O10 Sc2 N4 O17 91.6(2) . . . . ? O9 Sc2 N4 O17 89.9(3) . . . . ? O11 Sc2 N4 O17 -170.32(19) . . . . ? O12 Sc2 N4 O17 -2.0(2) . . . . ? O14 Sc2 N4 O17 -92.4(2) . . . . ? O16 Sc2 N4 O17 178.9(3) . . . . ? O13 Sc2 N4 O17 -82.8(2) . . . . ? N3 Sc2 N4 O17 -89.48(19) . . . . ? Sc1 Sc2 N4 O17 90.42(19) . . . . ? O10 Sc2 N4 O16 -87.3(2) . . . . ? O9 Sc2 N4 O16 -89.1(3) . . . . ? O11 Sc2 N4 O16 10.8(2) . . . . ? O12 Sc2 N4 O16 179.06(19) . . . . ? O14 Sc2 N4 O16 88.7(2) . . . . ? O13 Sc2 N4 O16 98.3(2) . . . . ? O17 Sc2 N4 O16 -178.9(3) . . . . ? N3 Sc2 N4 O16 91.6(2) . . . . ? Sc1 Sc2 N4 O16 -88.51(19) . . . . ? O3 N1 O1 Sc1 -179.8(3) . . . . ? O2 N1 O1 Sc1 -0.2(3) . . . . ? O9 Sc1 O1 N1 -89.4(2) . . . . ? O10 Sc1 O1 N1 -136.5(2) . . . . ? O8 Sc1 O1 N1 168.8(2) . . . . ? O7 Sc1 O1 N1 0.1(2) . . . . ? O4 Sc1 O1 N1 83.5(2) . . . . ? O5 Sc1 O1 N1 101.4(2) . . . . ? O2 Sc1 O1 N1 0.13(18) . . . . ? N2 Sc1 O1 N1 93.5(2) . . . . ? Sc2 Sc1 O1 N1 -107.74(19) . . . . ? O3 N1 O2 Sc1 179.8(4) . . . . ? O1 N1 O2 Sc1 0.2(3) . . . . ? O9 Sc1 O2 N1 84.1(2) . . . . ? O10 Sc1 O2 N1 133.7(2) . . . . ? O8 Sc1 O2 N1 -14.1(2) . . . . ? O7 Sc1 O2 N1 179.9(2) . . . . ? O4 Sc1 O2 N1 -80.4(2) . . . . ? O5 Sc1 O2 N1 -116.1(2) . . . . ? O1 Sc1 O2 N1 -0.13(19) . . . . ? N2 Sc1 O2 N1 -96.1(2) . . . . ? Sc2 Sc1 O2 N1 101.51(19) . . . . ? O6 N2 O4 Sc1 -172.6(3) . . . . ? O5 N2 O4 Sc1 6.6(3) . . . . ? O9 Sc1 O4 N2 175.5(2) . . . . ? O10 Sc1 O4 N2 9.6(2) . . . . ? O8 Sc1 O4 N2 81.9(2) . . . . ? O7 Sc1 O4 N2 -77.1(2) . . . . ? O5 Sc1 O4 N2 -3.91(18) . . . . ? O2 Sc1 O4 N2 -145.0(2) . . . . ? O1 Sc1 O4 N2 158.5(2) . . . . ? N1 Sc1 O4 N2 -172.9(2) . . . . ? Sc2 Sc1 O4 N2 27.8(4) . . . . ? O6 N2 O5 Sc1 172.7(3) . . . . ? O4 N2 O5 Sc1 -6.5(3) . . . . ? O9 Sc1 O5 N2 -175.6(2) . . . . ? O10 Sc1 O5 N2 -165.8(2) . . . . ? O8 Sc1 O5 N2 -81.4(2) . . . . ? O7 Sc1 O5 N2 106.8(2) . . . . ? O4 Sc1 O5 N2 3.95(18) . . . . ? O2 Sc1 O5 N2 47.5(2) . . . . ? O1 Sc1 O5 N2 -17.1(2) . . . . ? N1 Sc1 O5 N2 17.0(2) . . . . ? Sc2 Sc1 O5 N2 -168.38(17) . . . . ? O10 Sc1 O9 Sc2 1.00(10) . . . . ? O8 Sc1 O9 Sc2 -78.36(12) . . . . ? O7 Sc1 O9 Sc2 84.62(11) . . . . ? O4 Sc1 O9 Sc2 -168.00(18) . . . . ? O5 Sc1 O9 Sc2 11.0(2) . . . . ? O2 Sc1 O9 Sc2 153.82(12) . . . . ? O1 Sc1 O9 Sc2 -151.52(12) . . . . ? N2 Sc1 O9 Sc2 -24.5(16) . . . . ? N1 Sc1 O9 Sc2 -179.13(12) . . . . ? O10 Sc2 O9 Sc1 -1.03(10) . . . . ? O11 Sc2 O9 Sc1 -102.90(12) . . . . ? O12 Sc2 O9 Sc1 95.23(11) . . . . ? O14 Sc2 O9 Sc1 -176.30(10) . . . . ? O16 Sc2 O9 Sc1 -50.5(2) . . . . ? O13 Sc2 O9 Sc1 174.75(12) . . . . ? O17 Sc2 O9 Sc1 52.0(2) . . . . ? N3 Sc2 O9 Sc1 -179.85(10) . . . . ? N4 Sc2 O9 Sc1 0.8(3) . . . . ? O9 Sc2 O10 Sc1 1.01(10) . . . . ? O11 Sc2 O10 Sc1 80.86(12) . . . . ? O12 Sc2 O10 Sc1 -82.09(11) . . . . ? O14 Sc2 O10 Sc1 172.55(18) . . . . ? O16 Sc2 O10 Sc1 154.18(12) . . . . ? O13 Sc2 O10 Sc1 -7.2(2) . . . . ? O17 Sc2 O10 Sc1 -151.24(11) . . . . ? N3 Sc2 O10 Sc1 21.7(17) . . . . ? N4 Sc2 O10 Sc1 -178.23(12) . . . . ? O9 Sc1 O10 Sc2 -1.03(10) . . . . ? O8 Sc1 O10 Sc2 101.15(12) . . . . ? O7 Sc1 O10 Sc2 -96.57(11) . . . . ? O4 Sc1 O10 Sc2 172.82(10) . . . . ? O5 Sc1 O10 Sc2 -175.89(13) . . . . ? O2 Sc1 O10 Sc2 -53.9(2) . . . . ? O1 Sc1 O10 Sc2 48.6(2) . . . . ? N2 Sc1 O10 Sc2 177.40(10) . . . . ? N1 Sc1 O10 Sc2 -1.3(3) . . . . ? O15 N3 O13 Sc2 -174.3(3) . . . . ? O14 N3 O13 Sc2 5.3(3) . . . . ? O10 Sc2 O13 N3 176.6(2) . . . . ? O9 Sc2 O13 N3 168.6(2) . . . . ? O11 Sc2 O13 N3 83.6(2) . . . . ? O12 Sc2 O13 N3 -104.4(2) . . . . ? O14 Sc2 O13 N3 -3.28(17) . . . . ? O16 Sc2 O13 N3 19.5(2) . . . . ? O17 Sc2 O13 N3 -45.3(2) . . . . ? N4 Sc2 O13 N3 -14.5(2) . . . . ? Sc1 Sc2 O13 N3 171.91(17) . . . . ? O15 N3 O14 Sc2 174.1(3) . . . . ? O13 N3 O14 Sc2 -5.5(3) . . . . ? O10 Sc2 O14 N3 -176.6(2) . . . . ? O9 Sc2 O14 N3 -7.4(2) . . . . ? O11 Sc2 O14 N3 -81.20(19) . . . . ? O12 Sc2 O14 N3 77.62(19) . . . . ? O16 Sc2 O14 N3 -157.6(2) . . . . ? O13 Sc2 O14 N3 3.26(17) . . . . ? O17 Sc2 O14 N3 145.9(2) . . . . ? N4 Sc2 O14 N3 173.8(2) . . . . ? Sc1 Sc2 O14 N3 -17.4(4) . . . . ? O18 N4 O16 Sc2 178.5(3) . . . . ? O17 N4 O16 Sc2 -1.0(3) . . . . ? O10 Sc2 O16 N4 89.3(2) . . . . ? O9 Sc2 O16 N4 136.3(2) . . . . ? O11 Sc2 O16 N4 -169.1(2) . . . . ? O12 Sc2 O16 N4 -1.1(2) . . . . ? O14 Sc2 O16 N4 -82.8(2) . . . . ? O13 Sc2 O16 N4 -102.0(2) . . . . ? O17 Sc2 O16 N4 0.60(18) . . . . ? N3 Sc2 O16 N4 -93.1(2) . . . . ? Sc1 Sc2 O16 N4 106.18(19) . . . . ? O18 N4 O17 Sc2 -178.5(3) . . . . ? O16 N4 O17 Sc2 1.0(3) . . . . ? O10 Sc2 O17 N4 -85.5(2) . . . . ? O9 Sc2 O17 N4 -135.5(2) . . . . ? O11 Sc2 O17 N4 12.1(2) . . . . ? O12 Sc2 O17 N4 177.9(2) . . . . ? O14 Sc2 O17 N4 79.67(19) . . . . ? O16 Sc2 O17 N4 -0.61(18) . . . . ? O13 Sc2 O17 N4 114.2(2) . . . . ? N3 Sc2 O17 N4 94.9(2) . . . . ? Sc1 Sc2 O17 N4 -104.35(18) . . . . ? O22 Na1 O19 C8 9.3(2) . . . . ? O25 Na1 O19 C8 -154.7(2) . . . . ? O24 Na1 O19 C8 163.9(2) . . . . ? O26 Na1 O19 C8 55.4(3) . . . . ? O20 Na1 O19 C8 -109.1(2) . . . . ? O23 Na1 O19 C8 94.0(2) . . . . ? O21 Na1 O19 C8 -50.7(2) . . . . ? O22 Na1 O19 C1 137.8(2) . . . . ? O25 Na1 O19 C1 -26.2(3) . . . . ? O24 Na1 O19 C1 -67.5(2) . . . . ? O26 Na1 O19 C1 -176.05(19) . . . . ? O20 Na1 O19 C1 19.42(19) . . . . ? O23 Na1 O19 C1 -137.5(2) . . . . ? O21 Na1 O19 C1 77.8(2) . . . . ? O22 Na1 O20 C3 79.8(2) . . . . ? O25 Na1 O20 C3 -66.1(2) . . . . ? O24 Na1 O20 C3 -136.9(2) . . . . ? O19 Na1 O20 C3 140.0(2) . . . . ? O26 Na1 O20 C3 -25.2(3) . . . . ? O23 Na1 O20 C3 -176.5(2) . . . . ? O21 Na1 O20 C3 20.8(2) . . . . ? O22 Na1 O20 C2 -48.4(2) . . . . ? O25 Na1 O20 C2 165.7(2) . . . . ? O24 Na1 O20 C2 95.0(2) . . . . ? O19 Na1 O20 C2 11.81(19) . . . . ? O26 Na1 O20 C2 -153.3(2) . . . . ? O23 Na1 O20 C2 55.3(3) . . . . ? O21 Na1 O20 C2 -107.4(2) . . . . ? O22 Na1 O21 C5 19.2(2) . . . . ? O25 Na1 O21 C5 -136.9(2) . . . . ? O24 Na1 O21 C5 179.9(2) . . . . ? O19 Na1 O21 C5 79.6(2) . . . . ? O26 Na1 O21 C5 -66.8(2) . . . . ? O20 Na1 O21 C5 138.6(2) . . . . ? O23 Na1 O21 C5 -24.9(3) . . . . ? O22 Na1 O21 C4 -109.5(2) . . . . ? O25 Na1 O21 C4 94.3(2) . . . . ? O24 Na1 O21 C4 51.2(3) . . . . ? O19 Na1 O21 C4 -49.1(2) . . . . ? O26 Na1 O21 C4 164.4(2) . . . . ? O20 Na1 O21 C4 9.9(2) . . . . ? O23 Na1 O21 C4 -153.7(2) . . . . ? O25 Na1 O22 C6 55.9(3) . . . . ? O24 Na1 O22 C6 -150.8(2) . . . . ? O19 Na1 O22 C6 -107.0(2) . . . . ? O26 Na1 O22 C6 97.5(2) . . . . ? O20 Na1 O22 C6 -47.2(2) . . . . ? O23 Na1 O22 C6 166.5(2) . . . . ? O21 Na1 O22 C6 11.1(2) . . . . ? O25 Na1 O22 C7 -175.7(2) . . . . ? O24 Na1 O22 C7 -22.4(3) . . . . ? O19 Na1 O22 C7 21.4(2) . . . . ? O26 Na1 O22 C7 -134.1(2) . . . . ? O20 Na1 O22 C7 81.2(2) . . . . ? O23 Na1 O22 C7 -65.1(2) . . . . ? O21 Na1 O22 C7 139.5(2) . . . . ? O22 Na1 O23 C9 163.9(2) . . . . ? O25 Na1 O23 C9 -50.2(2) . . . . ? O24 Na1 O23 C9 10.1(2) . . . . ? O19 Na1 O23 C9 93.2(2) . . . . ? O26 Na1 O23 C9 -109.4(2) . . . . ? O20 Na1 O23 C9 52.8(3) . . . . ? O21 Na1 O23 C9 -155.0(2) . . . . ? O22 Na1 O23 C16 -67.3(2) . . . . ? O25 Na1 O23 C16 78.7(2) . . . . ? O24 Na1 O23 C16 139.0(2) . . . . ? O19 Na1 O23 C16 -138.0(2) . . . . ? O26 Na1 O23 C16 19.5(2) . . . . ? O20 Na1 O23 C16 -178.4(2) . . . . ? O21 Na1 O23 C16 -26.1(3) . . . . ? O22 Na1 O24 C10 -25.4(3) . . . . ? O25 Na1 O24 C10 138.8(2) . . . . ? O19 Na1 O24 C10 -66.6(2) . . . . ? O26 Na1 O24 C10 78.7(2) . . . . ? O20 Na1 O24 C10 -136.7(2) . . . . ? O23 Na1 O24 C10 20.6(2) . . . . ? O21 Na1 O24 C10 -174.9(2) . . . . ? O22 Na1 O24 C11 -154.6(2) . . . . ? O25 Na1 O24 C11 9.6(2) . . . . ? O19 Na1 O24 C11 164.2(2) . . . . ? O26 Na1 O24 C11 -50.5(2) . . . . ? O20 Na1 O24 C11 94.1(2) . . . . ? O23 Na1 O24 C11 -108.6(2) . . . . ? O21 Na1 O24 C11 55.9(3) . . . . ? O22 Na1 O25 C13 55.3(3) . . . . ? O24 Na1 O25 C13 -107.8(2) . . . . ? O19 Na1 O25 C13 -151.7(2) . . . . ? O26 Na1 O25 C13 10.4(2) . . . . ? O20 Na1 O25 C13 165.9(2) . . . . ? O23 Na1 O25 C13 -48.0(2) . . . . ? O21 Na1 O25 C13 96.8(2) . . . . ? O22 Na1 O25 C12 -176.5(2) . . . . ? O24 Na1 O25 C12 20.5(2) . . . . ? O19 Na1 O25 C12 -23.5(3) . . . . ? O26 Na1 O25 C12 138.6(2) . . . . ? O20 Na1 O25 C12 -65.9(2) . . . . ? O23 Na1 O25 C12 80.2(2) . . . . ? O21 Na1 O25 C12 -135.0(2) . . . . ? O22 Na1 O26 C15 96.7(2) . . . . ? O25 Na1 O26 C15 -107.2(2) . . . . ? O24 Na1 O26 C15 -46.7(2) . . . . ? O19 Na1 O26 C15 53.8(3) . . . . ? O20 Na1 O26 C15 -151.1(2) . . . . ? O23 Na1 O26 C15 11.9(2) . . . . ? O21 Na1 O26 C15 166.7(2) . . . . ? O22 Na1 O26 C14 -135.4(2) . . . . ? O25 Na1 O26 C14 20.8(2) . . . . ? O24 Na1 O26 C14 81.2(2) . . . . ? O19 Na1 O26 C14 -178.3(2) . . . . ? O20 Na1 O26 C14 -23.1(3) . . . . ? O23 Na1 O26 C14 139.9(2) . . . . ? O21 Na1 O26 C14 -65.4(2) . . . . ? O27A N5A O28A O28B 153.2(5) . . . . ? O29A N5A O28A O28B -32.0(6) . . . . ? O27B N5B O28B O28A -156.6(7) . . . . ? O29B N5B O28B O28A 33.9(9) . . . . ? N5A O28A O28B N5B -178.0(6) . . . . ? C8 O19 C1 C2 79.2(3) . . . . ? Na1 O19 C1 C2 -49.2(3) . . . . ? C3 O20 C2 C1 -165.7(3) . . . . ? Na1 O20 C2 C1 -39.3(3) . . . . ? O19 C1 C2 O20 60.4(4) . . . . ? C2 O20 C3 C4 78.6(4) . . . . ? Na1 O20 C3 C4 -49.7(3) . . . . ? C5 O21 C4 C3 -163.1(3) . . . . ? Na1 O21 C4 C3 -37.2(3) . . . . ? O20 C3 C4 O21 59.0(4) . . . . ? C4 O21 C5 C6 81.8(4) . . . . ? Na1 O21 C5 C6 -47.3(3) . . . . ? C7 O22 C6 C5 -164.3(3) . . . . ? Na1 O22 C6 C5 -37.7(3) . . . . ? O21 C5 C6 O22 58.2(4) . . . . ? C6 O22 C7 C8 79.3(4) . . . . ? Na1 O22 C7 C8 -50.6(3) . . . . ? C1 O19 C8 C7 -163.2(3) . . . . ? Na1 O19 C8 C7 -36.9(3) . . . . ? O22 C7 C8 O19 59.6(4) . . . . ? C16 O23 C9 C10 -164.0(3) . . . . ? Na1 O23 C9 C10 -36.9(3) . . . . ? C11 O24 C10 C9 79.1(4) . . . . ? Na1 O24 C10 C9 -50.0(3) . . . . ? O23 C9 C10 O24 59.2(4) . . . . ? C10 O24 C11 C12 -163.9(3) . . . . ? Na1 O24 C11 C12 -36.8(3) . . . . ? C13 O25 C12 C11 80.1(4) . . . . ? Na1 O25 C12 C11 -49.0(3) . . . . ? O24 C11 C12 O25 58.6(4) . . . . ? C12 O25 C13 C14 -164.3(3) . . . . ? Na1 O25 C13 C14 -38.2(3) . . . . ? C15 O26 C14 C13 78.9(4) . . . . ? Na1 O26 C14 C13 -50.3(3) . . . . ? O25 C13 C14 O26 60.4(4) . . . . ? C14 O26 C15 C16 -165.0(3) . . . . ? Na1 O26 C15 C16 -39.5(3) . . . . ? C9 O23 C16 C15 80.5(4) . . . . ? Na1 O23 C16 C15 -48.5(3) . . . . ? O26 C15 C16 O23 59.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7X O31 0.94 1.81 2.737(4) 168.3 . O7 H7Y O27B 0.80 1.89 2.679(4) 169.2 2_566 O8 H8X O30 0.95 1.84 2.749(4) 158.9 . O8 H8Y O27A 0.97 1.80 2.746(4) 164.0 . O8 H8Y N5A 0.97 2.37 3.168(5) 138.8 . O8 H8Y O29A 0.97 2.47 3.027(6) 116.3 . O9 H9X O29B 0.87 1.92 2.707(8) 150.4 2_666 O9 H9X O28A 0.87 2.21 2.952(5) 142.9 2_666 O10 H10X O29A 0.91 1.92 2.738(6) 148.4 2_566 O10 H10X O28B 0.91 2.12 2.916(7) 145.4 2_566 O11 H11X O27B 0.94 1.83 2.766(4) 173.4 1_545 O11 H11X N5B 0.94 2.27 3.099(7) 146.7 1_545 O11 H11X O29B 0.94 2.34 2.939(8) 121.1 1_545 O11 H11Y O31 0.94 1.80 2.719(4) 164.7 . O12 H12X O30 0.88 1.87 2.746(3) 175.8 . O12 H12Y O27A 0.85 1.81 2.647(4) 169.9 2_666 O30 H30X O1 0.94 1.93 2.842(4) 162.7 2_666 O30 H30Y O6 0.96 2.18 3.102(4) 161.0 2_566 O30 H30Y O5 0.96 2.42 3.132(3) 131.4 2_566 O31 H31X O16 0.93 1.94 2.791(3) 151.8 2_556 O31 H31Y O13 0.86 2.32 3.036(3) 140.8 2_656 O31 H31Y O15 0.86 2.41 3.194(4) 151.5 2_656 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.010 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.079 #===END OF FILE ======================================================