# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- Publish_cifs_merge.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2011-09-08 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_name 'Cheetham, Anthony K.' # Name of author for correspondence _publ_contact_author_address ;Department of Materials Science and Metallurgy The University of Cambridge Cambridge Cambs, UK ; # Address of author for correspondence _publ_contact_author_email akc30@cam.ac.uk _publ_contact_author_fax 441223334567 _publ_contact_author_phone 441223767061 _publ_contact_letter ; Submission dated :2011-09-08 Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as part of a journal submission Chemical Science Cheetham, Anthony K.. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; Layered Inorganic-Organic Frameworks based on the 2,2-Dimethylsuccinate ligand Structural Diversity and its Effect on Nanosheet Exfoliation and Magnetic Properties' ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' P.J.Saines ; ? ; ;Department of Materials Science and Metallurgy The University of Cambridge Cambridge Cambs, UK ; Jin-Chong.Tan ; ? ; ;Department of Materials Science and Metallurgy The University of Cambridge Cambridge Cambs, UK ; H.H.-M.H.Yeung ; ? ; ;Department of Materials Science and Metallurgy The University of Cambridge Cambridge Cambs, UK ; P.Barton ; ? ; ;Materials Department & Materials Research Laboratory University of California Santa Barbara CA, USA ; T.Cheetham ; ? ; ;Department of Materials Science and Metallurgy The University of Cambridge Cambridge Cambs, UK ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_CoDMS1 _database_code_depnum_ccdc_archive 'CCDC 865494' #TrackingRef '- Publish_cifs_merge.cif' _audit_creation_date 2011-09-08T12:55:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H10 Co1 O5' _chemical_formula_sum 'C6 H10 Co1 O5' _chemical_formula_weight 221.08 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c a' _symmetry_space_group_name_Hall '-C 2bc 2' _symmetry_Int_Tables_number 64 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, z' 'x, -y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1, z+1/2' '-x+1/2, -y+1, z+1/2' '-x, -y, -z' 'x, -y, -z' '-x, y-1/2, -z-1/2' 'x, y-1/2, -z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x+1/2, y, -z-1/2' 'x+1/2, y, -z-1/2' _cell_length_a 21.9175(12) _cell_length_b 10.2819(3) _cell_length_c 7.0879(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1597.28(12) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4673 _cell_measurement_theta_min 3.4140 _cell_measurement_theta_max 29.0937 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description sheet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2581 _exptl_crystal_size_mid 0.0872 _exptl_crystal_size_min 0.0267 _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.128 _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_unetI/netI 0.028 _diffrn_reflns_number 13031 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 29.16 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.9959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 1064 _reflns_number_gt 938 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd, 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd, 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd, 2010)' _computing_structure_solution 'DIRDIF-2008 (Beurskens, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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. The largest residual electron density is 1.12 A from O1W and 1.56 A from Co1. This is most likely caused by inadequate absorption correction. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+7.5484P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1064 _refine_ls_number_parameters 72 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.876 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.143 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.27140(6) 0.11252(8) 0.0129(2) Uani 1 2 d S . . O2 O 0.06916(11) 0.1595(2) 0.0151(3) 0.0215(5) Uani 1 1 d . . . C1 C 0.09125(15) 0.1051(3) -0.1263(4) 0.0144(6) Uani 1 1 d . . . C2 C 0.15161(16) 0.0349(3) -0.0965(4) 0.0178(7) Uani 0.50 1 d P . 1 C3 C 0.2010(3) 0.1476(8) -0.0884(10) 0.0257(15) Uani 0.50 1 d P . 1 H3A H 0.2400 0.1114 -0.0560 0.038 Uiso 0.50 1 calc PR . 1 H3B H 0.1892 0.2103 0.0051 0.038 Uiso 0.50 1 calc PR . 1 H3C H 0.2036 0.1891 -0.2094 0.038 Uiso 0.50 1 calc PR . 1 C4 C 0.1691(3) -0.0548(7) -0.2576(10) 0.0224(14) Uani 0.50 1 d P . 1 H4A H 0.1419 -0.1280 -0.2601 0.034 Uiso 0.50 1 calc PR . 1 H4B H 0.2102 -0.0847 -0.2399 0.034 Uiso 0.50 1 calc PR . 1 H4C H 0.1663 -0.0084 -0.3748 0.034 Uiso 0.50 1 calc PR . 1 C2A C 0.15161(16) 0.0349(3) -0.0965(4) 0.0178(7) Uani 0.50 1 d P . 2 H2AA H 0.1849 0.0970 -0.1012 0.021 Uiso 0.50 1 calc PR . 2 H2AB H 0.1577 -0.0282 -0.1964 0.021 Uiso 0.50 1 calc PR . 2 O1 O 0.06721(11) 0.1050(2) -0.2894(3) 0.0175(5) Uani 1 1 d . . . O1W O 0.0000 0.3767(3) -0.1492(5) 0.0148(6) Uani 1 2 d SD . . H1W H 0.0326(12) 0.421(4) -0.138(5) 0.022 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0204(4) 0.0081(3) 0.0101(3) -0.0005(2) 0.000 0.000 O2 0.0320(13) 0.0175(11) 0.0149(11) -0.0017(9) 0.0027(10) 0.0098(10) C1 0.0205(15) 0.0091(14) 0.0136(15) 0.0004(11) -0.0008(11) -0.0021(11) C2 0.0195(15) 0.0200(16) 0.0139(15) 0.0018(12) 0.0006(12) 0.0037(12) C3 0.023(3) 0.030(4) 0.024(3) 0.008(3) -0.001(3) -0.005(3) C4 0.029(3) 0.022(3) 0.017(3) -0.002(3) 0.005(3) 0.009(3) C2A 0.0195(15) 0.0200(16) 0.0139(15) 0.0018(12) 0.0006(12) 0.0037(12) O1 0.0248(12) 0.0138(11) 0.0139(11) 0.0003(8) -0.0026(9) 0.0034(9) O1W 0.0210(16) 0.0072(14) 0.0162(15) -0.0003(12) 0.000 0.000 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Co1 O2 2.025(2) 2 ? Co1 O2 2.025(2) . ? Co1 O1 2.066(2) 3 ? Co1 O1 2.066(2) 4 ? Co1 O1W 2.148(3) . ? Co1 O1W 2.274(3) 3 ? O2 C1 1.245(4) . ? C1 O1 1.271(4) . ? C1 C2 1.522(5) . ? C2 C4 1.517(7) . ? C2 C2 1.544(6) 10 ? C2 C3 1.586(8) . ? O1 Co1 2.066(2) 3_554 ? O1W Co1 2.274(3) 3_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 96.95(14) 2 . ? O2 Co1 O1 176.62(10) 2 3 ? O2 Co1 O1 86.02(10) . 3 ? O2 Co1 O1 86.02(10) 2 4 ? O2 Co1 O1 176.62(10) . 4 ? O1 Co1 O1 90.96(13) 3 4 ? O2 Co1 O1W 89.53(9) 2 . ? O2 Co1 O1W 89.53(9) . . ? O1 Co1 O1W 88.88(9) 3 . ? O1 Co1 O1W 88.88(9) 4 . ? O2 Co1 O1W 82.69(9) 2 3 ? O2 Co1 O1W 82.69(9) . 3 ? O1 Co1 O1W 99.33(8) 3 3 ? O1 Co1 O1W 99.33(8) 4 3 ? O1W Co1 O1W 168.23(10) . 3 ? C1 O2 Co1 145.2(2) . . ? O2 C1 O1 124.8(3) . . ? O2 C1 C2 116.1(3) . . ? O1 C1 C2 119.1(3) . . ? C4 C2 C1 113.8(4) . . ? C4 C2 C2 112.6(4) . 10 ? C1 C2 C2 110.1(2) . 10 ? C4 C2 C3 107.4(4) . . ? C1 C2 C3 104.5(4) . . ? C2 C2 C3 107.9(4) 10 . ? C1 O1 Co1 126.9(2) . 3_554 ? Co1 O1W Co1 107.68(13) . 3_554 ? #==END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_CoDMS2 _database_code_depnum_ccdc_archive 'CCDC 865495' #TrackingRef '- Publish_cifs_merge.cif' _audit_creation_date 2011-04-26T17:39:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H18 Co3 O10' _chemical_formula_sum 'C12 H18 Co3 O10' _chemical_formula_weight 499.0632 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7864(2) _cell_length_b 12.1514(6) _cell_length_c 12.1524(7) _cell_angle_alpha 73.604(5) _cell_angle_beta 81.487(4) _cell_angle_gamma 84.066(3) _cell_volume 808.98(7) _cell_formula_units_Z 2 _cell_measurement_temperature 121(2) _cell_measurement_reflns_used 4276 _cell_measurement_theta_min 3.4604 _cell_measurement_theta_max 29.2461 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description blade _exptl_crystal_colour purple _exptl_crystal_size_max 0.398 _exptl_crystal_size_mid 0.105 _exptl_crystal_size_min 0.057 _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 502 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.092 _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 121(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1183 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_number 7261 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 29.31 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.84 _reflns_number_total 3706 _reflns_number_gt 3140 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd, 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd, 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd, 2010)' _computing_structure_solution 'DIRDIF-2008 (Beurskens, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+7.2123P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3706 _refine_ls_number_parameters 239 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.137 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.155 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.182 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co3 Co 0.77042(12) 0.75215(6) 0.94655(6) 0.01176(18) Uani 1 1 d . . . O12 O 1.1400(7) 0.9706(3) 1.1540(3) 0.0153(8) Uani 1 1 d . . . O4 O 1.3520(7) 0.5832(3) 0.8511(3) 0.0142(8) Uani 1 1 d . . . O3 O 1.1075(7) 0.7179(3) 0.9049(3) 0.0139(8) Uani 1 1 d . . . C2 C 1.0225(9) 0.5714(5) 0.6993(4) 0.0120(10) Uani 1 1 d . . . C6 C 1.1895(9) 0.6589(4) 0.8325(4) 0.0091(9) Uani 1 1 d . . . C5 C 1.0861(9) 0.6826(4) 0.7218(5) 0.0133(10) Uani 1 1 d . . . H5A H 1.1997 0.7220 0.6570 0.016 Uiso 1 1 calc R . . H5B H 0.9435 0.7348 0.7248 0.016 Uiso 1 1 calc R . . C3 C 1.2298(10) 0.5095(5) 0.6437(5) 0.0156(11) Uani 1 1 d . . . H3A H 1.2912 0.5605 0.5693 0.023 Uiso 1 1 calc R . . H3B H 1.1787 0.4401 0.6311 0.023 Uiso 1 1 calc R . . H3C H 1.3527 0.4882 0.6948 0.023 Uiso 1 1 calc R . . C4 C 0.8300(11) 0.6044(5) 0.6183(5) 0.0206(12) Uani 1 1 d . . . H4A H 0.6951 0.6432 0.6541 0.031 Uiso 1 1 calc R . . H4B H 0.7815 0.5348 0.6048 0.031 Uiso 1 1 calc R . . H4C H 0.8912 0.6562 0.5444 0.031 Uiso 1 1 calc R . . C11 C 1.2766(9) 0.8917(4) 1.2055(5) 0.0116(10) Uani 1 1 d . . . C12 C 1.3749(9) 0.9100(5) 1.3102(5) 0.0124(10) Uani 1 1 d . . . C13 C 1.1847(10) 0.9701(5) 1.3794(5) 0.0181(11) Uani 1 1 d . . . H13A H 1.0525 0.9212 1.4092 0.027 Uiso 1 1 calc R . . H13B H 1.1310 1.0437 1.3290 0.027 Uiso 1 1 calc R . . H13C H 1.2493 0.9839 1.4442 0.027 Uiso 1 1 calc R . . C14 C 1.4543(11) 0.7943(5) 1.3897(5) 0.0202(12) Uani 1 1 d . . . H14A H 1.5813 0.7570 1.3474 0.030 Uiso 1 1 calc R . . H14B H 1.3222 0.7449 1.4154 0.030 Uiso 1 1 calc R . . H14C H 1.5103 0.8071 1.4571 0.030 Uiso 1 1 calc R . . C15 C 0.4072(9) 1.0185(5) 0.7347(5) 0.0131(10) Uani 1 1 d . . . H15A H 0.2748 1.0690 0.7579 0.016 Uiso 1 1 calc R . . H15B H 0.3645 0.9930 0.6702 0.016 Uiso 1 1 calc R . . O13 O 0.5921(7) 0.8371(3) 0.8189(3) 0.0150(8) Uani 1 1 d . . . C16 C 0.4366(9) 0.9146(4) 0.8349(4) 0.0091(9) Uani 1 1 d . . . C1 C 1.0892(9) 0.5078(5) 1.1872(5) 0.0121(10) Uani 1 1 d . . . Co1 Co 0.5000 0.5000 1.0000 0.0085(2) Uani 1 2 d S . . O1 O 1.1923(6) 0.4590(3) 1.1126(3) 0.0152(8) Uani 1 1 d . . . Co2 Co 1.22110(12) 0.74628(6) 1.05384(6) 0.00974(18) Uani 1 1 d . . . O2 O 1.0699(7) 0.6141(3) 1.1762(3) 0.0154(8) Uani 1 1 d . . . O11 O 1.3429(7) 0.8003(3) 1.1783(3) 0.0157(8) Uani 1 1 d . . . Co4 Co 0.0000 1.0000 1.0000 0.0089(2) Uani 1 2 d S . . O14 O 0.3148(6) 0.9077(3) 0.9318(3) 0.0120(7) Uani 1 1 d . . . O2H O 0.8845(6) 0.8359(3) 1.0478(3) 0.0107(7) Uani 1 1 d D . . H2H H 0.798(10) 0.816(6) 1.112(3) 0.016 Uiso 1 1 d D . . O1H O 0.5395(6) 0.6497(3) 1.0464(3) 0.0107(7) Uani 1 1 d D . . H1H H 0.593(11) 0.625(5) 1.110(3) 0.016 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co3 0.0064(3) 0.0143(4) 0.0149(4) -0.0039(3) -0.0017(3) -0.0016(3) O12 0.0174(19) 0.0120(18) 0.019(2) -0.0057(15) -0.0084(16) 0.0026(15) O4 0.0123(18) 0.0136(18) 0.0179(19) -0.0066(15) -0.0048(15) 0.0048(15) O3 0.0099(17) 0.0148(19) 0.019(2) -0.0086(16) -0.0029(15) 0.0013(14) C2 0.014(2) 0.014(2) 0.008(2) -0.0026(19) -0.002(2) -0.003(2) C6 0.011(2) 0.007(2) 0.010(2) -0.0010(18) -0.0001(19) -0.0057(18) C5 0.013(2) 0.011(2) 0.014(3) -0.002(2) -0.001(2) -0.001(2) C3 0.015(3) 0.014(3) 0.018(3) -0.006(2) 0.003(2) 0.000(2) C4 0.020(3) 0.021(3) 0.021(3) -0.002(2) -0.008(2) -0.005(2) C11 0.010(2) 0.011(2) 0.013(2) -0.0012(19) -0.001(2) -0.0031(19) C12 0.013(2) 0.015(3) 0.010(2) -0.005(2) -0.001(2) -0.002(2) C13 0.017(3) 0.021(3) 0.016(3) -0.006(2) -0.001(2) 0.000(2) C14 0.028(3) 0.015(3) 0.017(3) -0.001(2) -0.010(2) 0.001(2) C15 0.010(2) 0.014(2) 0.017(3) -0.006(2) -0.001(2) -0.0024(19) O13 0.0115(18) 0.0151(19) 0.018(2) -0.0056(16) -0.0008(15) 0.0008(15) C16 0.007(2) 0.008(2) 0.013(2) -0.0043(19) -0.0002(19) -0.0025(18) C1 0.006(2) 0.018(3) 0.014(3) -0.005(2) -0.0018(19) -0.0015(19) Co1 0.0041(4) 0.0113(5) 0.0098(5) -0.0028(4) -0.0012(4) 0.0010(3) O1 0.0084(17) 0.0158(19) 0.021(2) -0.0039(16) -0.0024(15) 0.0000(15) Co2 0.0078(3) 0.0091(3) 0.0125(4) -0.0033(3) -0.0013(3) -0.0002(2) O2 0.0152(19) 0.0135(19) 0.0153(19) -0.0024(15) 0.0026(15) -0.0017(15) O11 0.0175(19) 0.0133(19) 0.019(2) -0.0068(16) -0.0080(16) 0.0030(15) Co4 0.0052(4) 0.0111(5) 0.0101(5) -0.0021(4) -0.0016(4) 0.0006(3) O14 0.0098(17) 0.0098(17) 0.0160(19) -0.0040(14) 0.0007(15) -0.0002(14) O2H 0.0088(17) 0.0088(17) 0.0146(18) -0.0035(14) 0.0000(14) -0.0032(13) O1H 0.0109(17) 0.0108(17) 0.0113(18) -0.0037(14) -0.0025(14) -0.0015(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Co3 O1H 1.954(4) . ? Co3 O13 1.972(4) . ? Co3 O3 1.973(4) . ? Co3 O2H 2.018(4) . ? O12 C11 1.259(6) . ? O12 Co4 2.073(4) 1_655 ? O4 C6 1.244(6) . ? O4 Co1 2.068(4) 1_655 ? O3 C6 1.295(6) . ? O3 Co2 2.139(4) . ? C2 C3 1.523(7) . ? C2 C1 1.537(7) 2_767 ? C2 C5 1.543(7) . ? C2 C4 1.543(7) . ? C6 C5 1.494(7) . ? C11 O11 1.254(7) . ? C11 C12 1.547(7) . ? C12 C14 1.534(7) . ? C12 C13 1.536(8) . ? C12 C15 1.548(7) 2_777 ? C15 C16 1.502(7) . ? C15 C12 1.548(7) 2_777 ? O13 C16 1.269(6) . ? C16 O14 1.264(6) . ? C1 O2 1.255(7) . ? C1 O1 1.265(7) . ? C1 C2 1.537(7) 2_767 ? Co1 O4 2.068(4) 1_455 ? Co1 O4 2.068(4) 2_767 ? Co1 O1 2.090(4) 2_767 ? Co1 O1 2.090(4) 1_455 ? Co1 O1H 2.094(4) . ? Co1 O1H 2.094(4) 2_667 ? O1 Co1 2.090(4) 1_655 ? Co2 O2 2.028(4) . ? Co2 O11 2.046(4) . ? Co2 O1H 2.084(4) 1_655 ? Co2 O2H 2.132(4) . ? Co2 O14 2.163(4) 1_655 ? Co4 O2H 2.066(4) 2_677 ? Co4 O2H 2.066(4) 1_455 ? Co4 O12 2.073(4) 2_677 ? Co4 O12 2.073(4) 1_455 ? Co4 O14 2.218(4) . ? Co4 O14 2.218(4) 2_577 ? O14 Co2 2.163(4) 1_455 ? O2H Co4 2.066(4) 1_655 ? O1H Co2 2.084(4) 1_455 ? 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 O1H Co3 O13 101.67(16) . . ? O1H Co3 O3 128.70(16) . . ? O13 Co3 O3 116.59(17) . . ? O1H Co3 O2H 106.03(15) . . ? O13 Co3 O2H 120.25(16) . . ? O3 Co3 O2H 83.73(15) . . ? C11 O12 Co4 132.7(4) . 1_655 ? C6 O4 Co1 131.7(4) . 1_655 ? C6 O3 Co3 123.8(3) . . ? C6 O3 Co2 135.3(3) . . ? Co3 O3 Co2 96.49(16) . . ? C3 C2 C1 111.4(4) . 2_767 ? C3 C2 C5 113.2(4) . . ? C1 C2 C5 109.4(4) 2_767 . ? C3 C2 C4 109.0(5) . . ? C1 C2 C4 105.9(4) 2_767 . ? C5 C2 C4 107.6(4) . . ? O4 C6 O3 122.6(5) . . ? O4 C6 C5 118.5(5) . . ? O3 C6 C5 118.9(5) . . ? C6 C5 C2 111.9(4) . . ? O11 C11 O12 125.7(5) . . ? O11 C11 C12 117.0(5) . . ? O12 C11 C12 117.2(5) . . ? C14 C12 C13 108.9(5) . . ? C14 C12 C11 110.4(4) . . ? C13 C12 C11 109.7(4) . . ? C14 C12 C15 107.5(5) . 2_777 ? C13 C12 C15 111.6(4) . 2_777 ? C11 C12 C15 108.6(4) . 2_777 ? C16 C15 C12 115.2(4) . 2_777 ? C16 O13 Co3 119.2(3) . . ? O14 C16 O13 122.2(5) . . ? O14 C16 C15 120.6(5) . . ? O13 C16 C15 117.2(5) . . ? O2 C1 O1 125.8(5) . . ? O2 C1 C2 117.9(5) . 2_767 ? O1 C1 C2 116.3(5) . 2_767 ? O4 Co1 O4 179.999(2) 1_455 2_767 ? O4 Co1 O1 81.38(15) 1_455 2_767 ? O4 Co1 O1 98.62(15) 2_767 2_767 ? O4 Co1 O1 98.62(15) 1_455 1_455 ? O4 Co1 O1 81.38(15) 2_767 1_455 ? O1 Co1 O1 179.999(1) 2_767 1_455 ? O4 Co1 O1H 95.50(15) 1_455 . ? O4 Co1 O1H 84.50(15) 2_767 . ? O1 Co1 O1H 85.19(15) 2_767 . ? O1 Co1 O1H 94.81(15) 1_455 . ? O4 Co1 O1H 84.50(15) 1_455 2_667 ? O4 Co1 O1H 95.50(15) 2_767 2_667 ? O1 Co1 O1H 94.81(15) 2_767 2_667 ? O1 Co1 O1H 85.19(15) 1_455 2_667 ? O1H Co1 O1H 179.999(1) . 2_667 ? C1 O1 Co1 129.2(3) . 1_655 ? O2 Co2 O11 90.69(16) . . ? O2 Co2 O1H 91.30(15) . 1_655 ? O11 Co2 O1H 85.74(15) . 1_655 ? O2 Co2 O2H 88.12(15) . . ? O11 Co2 O2H 100.77(15) . . ? O1H Co2 O2H 173.48(14) 1_655 . ? O2 Co2 O3 98.70(16) . . ? O11 Co2 O3 170.27(16) . . ? O1H Co2 O3 96.53(14) 1_655 . ? O2H Co2 O3 77.15(14) . . ? O2 Co2 O14 167.92(15) . 1_655 ? O11 Co2 O14 88.25(15) . 1_655 ? O1H Co2 O14 100.61(14) 1_655 1_655 ? O2H Co2 O14 80.27(14) . 1_655 ? O3 Co2 O14 82.03(15) . 1_655 ? C1 O2 Co2 131.2(4) . . ? C11 O11 Co2 125.7(3) . . ? O2H Co4 O2H 180.000(1) 2_677 1_455 ? O2H Co4 O12 91.50(15) 2_677 2_677 ? O2H Co4 O12 88.50(15) 1_455 2_677 ? O2H Co4 O12 88.50(15) 2_677 1_455 ? O2H Co4 O12 91.50(15) 1_455 1_455 ? O12 Co4 O12 179.998(2) 2_677 1_455 ? O2H Co4 O14 99.57(14) 2_677 . ? O2H Co4 O14 80.43(14) 1_455 . ? O12 Co4 O14 90.74(15) 2_677 . ? O12 Co4 O14 89.26(15) 1_455 . ? O2H Co4 O14 80.43(14) 2_677 2_577 ? O2H Co4 O14 99.57(14) 1_455 2_577 ? O12 Co4 O14 89.26(15) 2_677 2_577 ? O12 Co4 O14 90.74(15) 1_455 2_577 ? O14 Co4 O14 180.000(1) . 2_577 ? C16 O14 Co2 123.4(3) . 1_455 ? C16 O14 Co4 136.9(3) . . ? Co2 O14 Co4 91.57(14) 1_455 . ? Co3 O2H Co4 127.78(19) . 1_655 ? Co3 O2H Co2 95.38(15) . . ? Co4 O2H Co2 96.86(15) 1_655 . ? Co3 O1H Co2 107.25(17) . 1_455 ? Co3 O1H Co1 116.28(18) . . ? Co2 O1H Co1 110.49(16) 1_455 . ? #==END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_ZnDMS _database_code_depnum_ccdc_archive 'CCDC 865496' #TrackingRef '- Publish_cifs_merge.cif' _audit_creation_date 2011-09-08T11:57:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C36 H50 O26 Zn7' _chemical_formula_moiety 'C36 H50 O26 Zn7' _chemical_formula_weight 1356.35 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5108(8) _cell_length_b 11.5667(10) _cell_length_c 11.9714(10) _cell_angle_alpha 99.347(7) _cell_angle_beta 114.566(8) _cell_angle_gamma 106.545(7) _cell_volume 1201.26(17) _cell_formula_units_Z 1 _cell_measurement_temperature 121(2) _cell_measurement_reflns_used 4648 _cell_measurement_theta_min 3.0965 _cell_measurement_theta_max 29.1079 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3356 _exptl_crystal_size_mid 0.1302 _exptl_crystal_size_min 0.1082 _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.521 _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 0.719 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 121(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_unetI/netI 0.0419 _diffrn_reflns_number 10975 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.1 _diffrn_reflns_theta_max 29.17 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.9984 _diffrn_measured_fraction_theta_max 0.849 _reflns_number_total 5512 _reflns_number_gt 4703 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro, Oxford Diffraction, 2010' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction, 2010' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction, 2010' _computing_structure_solution 'DIRDIF-2008 (Beurskens, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+0.5478P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_number_reflns 5512 _refine_ls_number_parameters 322 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.462 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.77563(3) 0.53434(3) 0.71324(3) 0.01198(7) Uani 1 1 d . . . Zn2 Zn 0.67876(3) 0.29190(3) 0.79503(3) 0.01201(7) Uani 1 1 d . . . Zn3 Zn 1.0000 0.5000 1.0000 0.01129(9) Uani 1 2 d S . . Zn4 Zn 1.52612(3) 0.64581(3) 0.95102(3) 0.01211(7) Uani 1 1 d . . . O1 O 0.68862(18) 0.38818(15) 0.55997(15) 0.0139(3) Uani 1 1 d . . . O1H O 0.78754(18) 0.47889(15) 0.86418(15) 0.0117(3) Uani 1 1 d D . . H1H H 0.752(3) 0.518(2) 0.893(2) 0.018 Uiso 1 1 d D . . O2 O 0.52897(18) 0.26711(17) 0.61295(15) 0.0162(4) Uani 1 1 d . . . O3 O 0.36349(19) 0.37692(16) 0.33869(15) 0.0147(4) Uani 1 1 d . . . O4 O 0.37422(19) 0.36059(17) 0.15661(16) 0.0177(4) Uani 1 1 d . . . O11 O 0.97114(19) 0.66565(16) 0.76917(16) 0.0179(4) Uani 1 1 d . . . O12 O 1.11286(18) 0.67082(15) 0.97267(15) 0.0139(3) Uani 1 1 d . . . O13 O 1.47428(19) 0.79716(16) 0.96382(16) 0.0147(4) Uani 1 1 d . . . O14 O 1.44728(19) 0.75374(16) 1.12611(16) 0.0159(4) Uani 1 1 d . . . O21 O 1.3294(2) 0.51118(18) 0.83306(17) 0.0238(4) Uani 1 1 d . . . O22 O 1.30318(19) 0.33632(18) 0.89285(16) 0.0211(4) Uani 1 1 d . . . O23 O 1.01516(18) 0.39251(16) 0.85332(15) 0.0145(4) Uani 1 1 d . . . O24 O 0.79967(18) 0.21548(15) 0.74796(15) 0.0138(3) Uani 1 1 d . . . C1 C 0.5728(3) 0.2916(2) 0.5326(2) 0.0126(5) Uani 1 1 d . . . C2 C 0.4902(3) 0.1932(2) 0.3978(2) 0.0117(5) Uani 1 1 d . . . C3 C 0.5818(3) 0.1083(2) 0.4089(2) 0.0176(5) Uani 1 1 d . . . H3A H 0.5903 0.0759 0.4794 0.026 Uiso 1 1 calc R . . H3B H 0.6815 0.1577 0.4245 0.026 Uiso 1 1 calc R . . H3C H 0.5305 0.0385 0.3295 0.026 Uiso 1 1 calc R . . C4 C 0.3265(3) 0.1126(2) 0.3600(2) 0.0170(5) Uani 1 1 d . . . H4A H 0.2778 0.0513 0.2752 0.026 Uiso 1 1 calc R . . H4B H 0.2721 0.1668 0.3592 0.026 Uiso 1 1 calc R . . H4C H 0.3268 0.0690 0.4217 0.026 Uiso 1 1 calc R . . C5 C 0.4979(3) 0.2564(2) 0.2964(2) 0.0134(5) Uani 1 1 d . . . H5A H 0.6035 0.3097 0.3278 0.016 Uiso 1 1 calc R . . H5B H 0.4646 0.1900 0.2175 0.016 Uiso 1 1 calc R . . C6 C 0.4064(3) 0.3363(2) 0.2625(2) 0.0122(5) Uani 1 1 d . . . C11 C 1.0850(3) 0.7187(2) 0.8834(2) 0.0122(5) Uani 1 1 d . . . C12 C 1.1897(3) 0.8545(2) 0.9097(2) 0.0130(5) Uani 1 1 d . . . C13 C 1.1083(3) 0.9410(3) 0.9310(3) 0.0234(6) Uani 1 1 d . . . H13A H 1.0137 0.9173 0.8533 0.035 Uiso 1 1 calc R . . H13B H 1.1716 1.0282 0.9516 0.035 Uiso 1 1 calc R . . H13C H 1.0889 0.9312 1.0012 0.035 Uiso 1 1 calc R . . C14 C 1.2125(3) 0.8664(3) 0.7929(2) 0.0210(6) Uani 1 1 d . . . H14A H 1.2609 0.8114 0.7775 0.032 Uiso 1 1 calc R . . H14B H 1.2754 0.9529 0.8107 0.032 Uiso 1 1 calc R . . H14C H 1.1156 0.8422 0.7176 0.032 Uiso 1 1 calc R . . C15 C 1.3416(3) 0.8988(2) 1.0364(2) 0.0120(5) Uani 1 1 d . . . H15A H 1.4073 0.9825 1.0466 0.014 Uiso 1 1 calc R . . H15B H 1.3217 0.9070 1.1088 0.014 Uiso 1 1 calc R . . C16 C 1.4250(3) 0.8114(2) 1.0427(2) 0.0116(5) Uani 1 1 d . . . C21 C 1.2614(3) 0.3951(2) 0.8141(2) 0.0135(5) Uani 1 1 d . . . C22 C 1.1209(3) 0.3153(2) 0.6817(2) 0.0151(5) Uani 1 1 d . . . C23 C 1.0585(3) 0.3985(3) 0.6062(2) 0.0227(6) Uani 1 1 d . . . H23A H 0.9687 0.3453 0.5254 0.034 Uiso 1 1 calc R . . H23B H 1.1339 0.4497 0.5895 0.034 Uiso 1 1 calc R . . H23C H 1.0337 0.4528 0.6561 0.034 Uiso 1 1 calc R . . C24 C 1.1755(3) 0.2367(3) 0.6083(2) 0.0251(6) Uani 1 1 d . . . H24A H 1.2143 0.1844 0.6563 0.038 Uiso 1 1 calc R . . H24B H 1.2544 0.2933 0.5988 0.038 Uiso 1 1 calc R . . H24C H 1.0918 0.1835 0.5241 0.038 Uiso 1 1 calc R . . C25 C 0.9986(3) 0.2214(2) 0.6999(2) 0.0152(5) Uani 1 1 d . . . H25A H 0.9156 0.1656 0.6149 0.018 Uiso 1 1 calc R . . H25B H 1.0427 0.1689 0.7456 0.018 Uiso 1 1 calc R . . C26 C 0.9340(3) 0.2825(2) 0.7731(2) 0.0129(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01187(14) 0.01082(14) 0.01009(13) 0.00332(11) 0.00328(11) 0.00347(11) Zn2 0.01270(14) 0.01295(15) 0.01165(14) 0.00461(11) 0.00721(11) 0.00445(12) Zn3 0.01075(18) 0.0119(2) 0.00828(18) 0.00212(15) 0.00272(15) 0.00416(16) Zn4 0.01196(14) 0.01460(15) 0.01153(13) 0.00603(11) 0.00567(11) 0.00666(12) O1 0.0139(8) 0.0120(9) 0.0128(8) 0.0013(7) 0.0061(7) 0.0034(7) O1H 0.0117(8) 0.0119(9) 0.0109(8) 0.0021(7) 0.0050(7) 0.0054(7) O2 0.0139(8) 0.0235(10) 0.0118(8) 0.0061(7) 0.0069(7) 0.0068(8) O3 0.0194(9) 0.0171(9) 0.0128(8) 0.0063(7) 0.0092(7) 0.0111(8) O4 0.0230(9) 0.0273(10) 0.0151(9) 0.0133(8) 0.0123(8) 0.0183(9) O11 0.0144(9) 0.0171(9) 0.0134(8) 0.0047(7) 0.0031(7) 0.0003(8) O12 0.0118(8) 0.0126(9) 0.0146(8) 0.0053(7) 0.0048(7) 0.0032(7) O13 0.0196(9) 0.0176(9) 0.0156(8) 0.0080(7) 0.0126(7) 0.0112(8) O14 0.0156(9) 0.0221(10) 0.0164(9) 0.0116(7) 0.0101(7) 0.0096(8) O21 0.0150(9) 0.0233(11) 0.0218(10) 0.0066(8) 0.0026(8) 0.0025(8) O22 0.0151(9) 0.0274(11) 0.0174(9) 0.0113(8) 0.0038(8) 0.0077(8) O23 0.0131(8) 0.0149(9) 0.0132(8) 0.0005(7) 0.0070(7) 0.0037(7) O24 0.0108(8) 0.0127(9) 0.0148(8) 0.0021(7) 0.0061(7) 0.0021(7) C1 0.0128(11) 0.0142(12) 0.0131(11) 0.0058(10) 0.0050(10) 0.0095(10) C2 0.0129(11) 0.0109(12) 0.0107(11) 0.0041(9) 0.0047(9) 0.0053(10) C3 0.0210(13) 0.0164(13) 0.0162(12) 0.0056(10) 0.0076(11) 0.0107(11) C4 0.0156(12) 0.0148(13) 0.0136(12) 0.0021(10) 0.0030(10) 0.0045(11) C5 0.0166(12) 0.0170(13) 0.0076(11) 0.0037(9) 0.0056(10) 0.0087(11) C6 0.0123(11) 0.0117(12) 0.0107(11) 0.0039(9) 0.0045(9) 0.0036(10) C11 0.0097(11) 0.0147(12) 0.0150(12) 0.0053(10) 0.0075(10) 0.0060(10) C12 0.0117(11) 0.0123(12) 0.0140(12) 0.0047(10) 0.0047(10) 0.0057(10) C13 0.0162(13) 0.0177(14) 0.0310(15) 0.0046(12) 0.0061(12) 0.0097(12) C14 0.0161(13) 0.0243(15) 0.0151(12) 0.0097(11) 0.0035(11) 0.0022(12) C15 0.0111(11) 0.0120(12) 0.0113(11) 0.0016(9) 0.0059(9) 0.0026(10) C16 0.0074(10) 0.0106(12) 0.0111(11) 0.0017(9) 0.0025(9) 0.0001(9) C21 0.0099(11) 0.0198(13) 0.0137(12) 0.0056(10) 0.0071(10) 0.0076(10) C22 0.0117(12) 0.0209(14) 0.0111(11) 0.0026(10) 0.0048(10) 0.0067(11) C23 0.0167(13) 0.0342(16) 0.0164(13) 0.0118(12) 0.0059(11) 0.0102(12) C24 0.0196(14) 0.0303(16) 0.0180(13) -0.0022(12) 0.0081(11) 0.0073(13) C25 0.0113(11) 0.0169(13) 0.0136(12) 0.0007(10) 0.0045(10) 0.0053(10) C26 0.0138(12) 0.0162(13) 0.0094(11) 0.0061(10) 0.0039(9) 0.0085(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn1 O11 1.9303(17) . ? Zn1 O1 1.9436(16) . ? Zn1 O3 1.9710(17) 2_666 ? Zn1 O1H 1.9815(16) . ? Zn1 Zn2 3.1550(5) . ? Zn2 O14 1.9310(15) 2_767 ? Zn2 O24 1.9461(16) . ? Zn2 O1H 1.9732(17) . ? Zn2 O2 1.9997(16) . ? Zn2 Zn3 3.1272(6) . ? Zn3 O1H 2.0571(17) . ? Zn3 O1H 2.0571(17) 2_767 ? Zn3 O23 2.0715(15) 2_767 ? Zn3 O23 2.0715(15) . ? Zn3 O12 2.1485(16) 2_767 ? Zn3 O12 2.1485(16) . ? Zn3 Zn2 3.1272(6) 2_767 ? Zn4 O22 1.9053(17) 2_867 ? Zn4 O21 1.9285(19) . ? Zn4 O4 1.9744(15) 2_766 ? Zn4 O13 1.9775(17) . ? O1 C1 1.270(3) . ? O2 C1 1.265(3) . ? O3 C6 1.257(3) . ? O3 Zn1 1.9710(17) 2_666 ? O4 C6 1.270(3) . ? O4 Zn4 1.9744(15) 2_766 ? O11 C11 1.275(3) . ? O12 C11 1.249(3) . ? O13 C16 1.261(3) . ? O14 C16 1.268(3) . ? O14 Zn2 1.9310(15) 2_767 ? O21 C21 1.259(3) . ? O22 C21 1.256(3) . ? O22 Zn4 1.9053(17) 2_867 ? O23 C26 1.254(3) . ? O24 C26 1.278(3) . ? C1 C2 1.527(3) . ? C2 C4 1.529(3) . ? C2 C5 1.533(3) . ? C2 C3 1.544(3) . ? C5 C6 1.499(3) . ? C11 C12 1.530(3) . ? C12 C14 1.534(3) . ? C12 C15 1.543(3) . ? C12 C13 1.544(3) . ? C15 C16 1.506(3) . ? C21 C22 1.532(3) . ? C22 C23 1.523(4) . ? C22 C24 1.545(3) . ? C22 C25 1.547(3) . ? C25 C26 1.516(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Zn1 O1 119.24(7) . . ? O11 Zn1 O3 102.92(7) . 2_666 ? O1 Zn1 O3 103.75(7) . 2_666 ? O11 Zn1 O1H 107.35(7) . . ? O1 Zn1 O1H 110.76(7) . . ? O3 Zn1 O1H 112.64(6) 2_666 . ? O11 Zn1 Zn2 132.37(5) . . ? O1 Zn1 Zn2 74.06(5) . . ? O3 Zn1 Zn2 118.66(5) 2_666 . ? O1H Zn1 Zn2 36.99(5) . . ? O14 Zn2 O24 134.07(7) 2_767 . ? O14 Zn2 O1H 107.42(7) 2_767 . ? O24 Zn2 O1H 109.36(7) . . ? O14 Zn2 O2 103.34(7) 2_767 . ? O24 Zn2 O2 95.43(7) . . ? O1H Zn2 O2 101.39(7) . . ? O14 Zn2 Zn3 110.80(5) 2_767 . ? O24 Zn2 Zn3 82.19(5) . . ? O1H Zn2 Zn3 40.09(5) . . ? O2 Zn2 Zn3 134.30(5) . . ? O14 Zn2 Zn1 130.98(5) 2_767 . ? O24 Zn2 Zn1 94.85(5) . . ? O1H Zn2 Zn1 37.17(5) . . ? O2 Zn2 Zn1 68.65(5) . . ? Zn3 Zn2 Zn1 66.133(11) . . ? O1H Zn3 O1H 180.00(11) . 2_767 ? O1H Zn3 O23 91.38(6) . 2_767 ? O1H Zn3 O23 88.62(6) 2_767 2_767 ? O1H Zn3 O23 88.62(6) . . ? O1H Zn3 O23 91.38(6) 2_767 . ? O23 Zn3 O23 179.999(1) 2_767 . ? O1H Zn3 O12 86.71(6) . 2_767 ? O1H Zn3 O12 93.29(6) 2_767 2_767 ? O23 Zn3 O12 89.71(6) 2_767 2_767 ? O23 Zn3 O12 90.29(6) . 2_767 ? O1H Zn3 O12 93.29(6) . . ? O1H Zn3 O12 86.71(6) 2_767 . ? O23 Zn3 O12 90.29(6) 2_767 . ? O23 Zn3 O12 89.71(6) . . ? O12 Zn3 O12 180.0 2_767 . ? O1H Zn3 Zn2 38.15(5) . . ? O1H Zn3 Zn2 141.85(5) 2_767 . ? O23 Zn3 Zn2 109.79(5) 2_767 . ? O23 Zn3 Zn2 70.21(5) . . ? O12 Zn3 Zn2 55.19(4) 2_767 . ? O12 Zn3 Zn2 124.81(4) . . ? O1H Zn3 Zn2 141.85(5) . 2_767 ? O1H Zn3 Zn2 38.15(5) 2_767 2_767 ? O23 Zn3 Zn2 70.21(5) 2_767 2_767 ? O23 Zn3 Zn2 109.79(5) . 2_767 ? O12 Zn3 Zn2 124.81(4) 2_767 2_767 ? O12 Zn3 Zn2 55.19(4) . 2_767 ? Zn2 Zn3 Zn2 180.0 . 2_767 ? O22 Zn4 O21 134.47(8) 2_867 . ? O22 Zn4 O4 95.42(7) 2_867 2_766 ? O21 Zn4 O4 99.77(8) . 2_766 ? O22 Zn4 O13 112.13(8) 2_867 . ? O21 Zn4 O13 101.71(8) . . ? O4 Zn4 O13 111.35(7) 2_766 . ? C1 O1 Zn1 120.43(14) . . ? Zn2 O1H Zn1 105.84(7) . . ? Zn2 O1H Zn3 101.75(7) . . ? Zn1 O1H Zn3 116.14(7) . . ? C1 O2 Zn2 120.87(15) . . ? C6 O3 Zn1 119.92(15) . 2_666 ? C6 O4 Zn4 129.09(16) . 2_766 ? C11 O11 Zn1 128.27(15) . . ? C11 O12 Zn3 136.13(16) . . ? C16 O13 Zn4 112.98(15) . . ? C16 O14 Zn2 125.28(15) . 2_767 ? C21 O21 Zn4 137.89(18) . . ? C21 O22 Zn4 141.06(17) . 2_867 ? C26 O23 Zn3 133.00(14) . . ? C26 O24 Zn2 121.53(15) . . ? O2 C1 O1 124.1(2) . . ? O2 C1 C2 118.0(2) . . ? O1 C1 C2 117.6(2) . . ? C1 C2 C4 111.39(18) . . ? C1 C2 C5 111.22(19) . . ? C4 C2 C5 111.95(19) . . ? C1 C2 C3 104.70(19) . . ? C4 C2 C3 109.9(2) . . ? C5 C2 C3 107.38(18) . . ? C6 C5 C2 116.55(18) . . ? O3 C6 O4 121.9(2) . . ? O3 C6 C5 119.5(2) . . ? O4 C6 C5 118.6(2) . . ? O12 C11 O11 125.6(2) . . ? O12 C11 C12 119.4(2) . . ? O11 C11 C12 114.9(2) . . ? C11 C12 C14 111.12(19) . . ? C11 C12 C15 111.08(19) . . ? C14 C12 C15 112.45(18) . . ? C11 C12 C13 106.18(19) . . ? C14 C12 C13 108.7(2) . . ? C15 C12 C13 106.99(19) . . ? C16 C15 C12 114.62(19) . . ? O13 C16 O14 120.0(2) . . ? O13 C16 C15 118.8(2) . . ? O14 C16 C15 121.18(19) . . ? O22 C21 O21 125.4(2) . . ? O22 C21 C22 116.3(2) . . ? O21 C21 C22 118.2(2) . . ? C23 C22 C21 111.9(2) . . ? C23 C22 C24 110.0(2) . . ? C21 C22 C24 105.31(19) . . ? C23 C22 C25 111.6(2) . . ? C21 C22 C25 109.73(18) . . ? C24 C22 C25 108.0(2) . . ? C26 C25 C22 115.4(2) . . ? O23 C26 O24 125.3(2) . . ? O23 C26 C25 118.4(2) . . ? O24 C26 C25 116.2(2) . . ? #==END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_LiDMS _database_code_depnum_ccdc_archive 'CCDC 865497' #TrackingRef '- Publish_cifs_merge.cif' _audit_creation_date 2012-01-12T11:59:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Dilithium 2,2-dimethylsuccinate ; _chemical_name_common 'Dilithium 2,2-dimethylsuccinate' _chemical_formula_moiety 'C6 H8 Li2 O4' _chemical_formula_sum 'C6 H8 Li2 O4' _chemical_formula_weight 158 _chemical_melting_point 'not measured' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2511(6) _cell_length_b 9.8961(11) _cell_length_c 12.225(2) _cell_angle_alpha 101.862(13) _cell_angle_beta 102.726(13) _cell_angle_gamma 90.012(8) _cell_volume 721.11(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 1710 _cell_measurement_theta_min 3.3268 _cell_measurement_theta_max 28.9606 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_T_min 0.88590 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.1183 _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.1279 _diffrn_reflns_number 3459 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 29.21 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.825 _reflns_number_total 3459 _reflns_number_gt 2384 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury & Diamond' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1766P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 3459 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.12 _refine_ls_R_factor_gt 0.091 _refine_ls_wR_factor_ref 0.2695 _refine_ls_wR_factor_gt 0.2523 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.829 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.152 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li2 Li -0.0962(17) 1.1049(12) 0.5573(9) 0.0124(7) Uani 1 1 d . . . Li3 Li 0.1118(16) 0.6982(12) 0.5984(9) 0.0124(7) Uani 1 1 d . . . Li4 Li 0.3779(17) 1.1424(12) 0.4030(9) 0.0124(7) Uani 1 1 d . . . O5 O 0.3704(7) 1.4331(5) 0.3945(3) 0.0098(5) Uani 1 1 d . . . C8 C 0.1231(9) 1.4102(6) 0.2114(5) 0.0084(3) Uani 1 1 d . . . C11 C 0.3081(9) 1.4154(6) 0.1453(5) 0.0147(5) Uani 1 1 d . . . H11A H 0.2508 1.4479 0.0763 0.022 Uiso 1 1 calc R . . H11B H 0.361 1.3245 0.1261 0.022 Uiso 1 1 calc R . . H11C H 0.4265 1.4771 0.1928 0.022 Uiso 1 1 calc R . . C12 C -0.0680(9) 1.3156(6) 0.1330(5) 0.0147(5) Uani 1 1 d . . . H12A H -0.1236 1.3519 0.0657 0.022 Uiso 1 1 calc R . . H12B H -0.1827 1.3111 0.1732 0.022 Uiso 1 1 calc R . . H12C H -0.0174 1.2246 0.1109 0.022 Uiso 1 1 calc R . . C9 C 0.0521(9) 1.5586(6) 0.2512(5) 0.0084(3) Uani 1 1 d . . . H9A H 0.1765 1.6224 0.262 0.01 Uiso 1 1 calc R . . H9B H -0.0624 1.5799 0.1903 0.01 Uiso 1 1 calc R . . C10 C -0.0320(9) 1.5843(6) 0.3614(5) 0.0084(3) Uani 1 1 d . . . O8 O -0.1571(7) 1.4925(5) 0.3739(4) 0.0098(5) Uani 1 1 d . . . O7 O 0.0208(6) 1.6989(4) 0.4320(4) 0.0098(5) Uani 1 1 d . . . Li1 Li 0.6005(17) 1.5800(12) 0.4425(9) 0.0124(7) Uani 1 1 d . . . O1 O 0.3524(6) 0.8368(4) 0.6682(3) 0.0108(5) Uani 1 1 d . . . O6 O 0.1460(6) 1.2438(4) 0.3316(3) 0.0098(5) Uani 1 1 d . . . O4 O 0.4769(6) 1.2366(4) 0.5666(4) 0.0108(5) Uani 1 1 d . . . O3 O 0.6550(7) 1.0608(5) 0.6231(4) 0.0108(5) Uani 1 1 d . . . O2 O 0.1306(7) 0.9894(5) 0.6046(4) 0.0108(5) Uani 1 1 d . . . C7 C 0.2201(9) 1.3581(6) 0.3189(5) 0.0084(3) Uani 1 1 d . . . C1 C 0.2776(9) 0.9536(6) 0.6790(5) 0.0084(3) Uani 1 1 d . . . C4 C 0.5341(9) 1.1618(6) 0.6386(5) 0.0084(3) Uani 1 1 d . . . C2 C 0.3789(9) 1.0668(6) 0.7876(5) 0.0084(3) Uani 1 1 d . . . C5 C 0.5772(9) 1.0154(6) 0.8616(5) 0.0147(5) Uani 1 1 d . . . H5A H 0.6876 0.9924 0.8183 0.022 Uiso 1 1 calc R . . H5B H 0.5339 0.9349 0.8854 0.022 Uiso 1 1 calc R . . H5C H 0.6352 1.0866 0.9281 0.022 Uiso 1 1 calc R . . C3 C 0.4438(9) 1.1955(6) 0.7467(5) 0.0084(3) Uani 1 1 d . . . H3A H 0.3158 1.2502 0.7323 0.01 Uiso 1 1 calc R . . H3B H 0.5536 1.2516 0.8078 0.01 Uiso 1 1 calc R . . C6 C 0.2004(9) 1.1049(6) 0.8540(5) 0.0147(5) Uani 1 1 d . . . H6A H 0.0774 1.1376 0.8059 0.022 Uiso 1 1 calc R . . H6B H 0.257 1.1762 0.9205 0.022 Uiso 1 1 calc R . . H6C H 0.1543 1.0249 0.8774 0.022 Uiso 1 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 Li2 0.0099(15) 0.011(2) 0.0185(16) 0.007(3) 0.0042(13) 0.004(3) Li3 0.0099(15) 0.011(2) 0.0185(16) 0.007(3) 0.0042(13) 0.004(3) Li4 0.0099(15) 0.011(2) 0.0185(16) 0.007(3) 0.0042(13) 0.004(3) O5 0.0111(11) 0.0045(13) 0.0165(11) 0.0065(11) 0.0048(9) -0.0015(11) C8 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) C11 0.0152(10) 0.0127(12) 0.0182(10) 0.0057(15) 0.0056(8) -0.0007(15) C12 0.0152(10) 0.0127(12) 0.0182(10) 0.0057(15) 0.0056(8) -0.0007(15) C9 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) C10 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) O8 0.0111(11) 0.0045(13) 0.0165(11) 0.0065(11) 0.0048(9) -0.0015(11) O7 0.0111(11) 0.0045(13) 0.0165(11) 0.0065(11) 0.0048(9) -0.0015(11) Li1 0.0099(15) 0.011(2) 0.0185(16) 0.007(3) 0.0042(13) 0.004(3) O1 0.0102(11) 0.0071(13) 0.0178(11) 0.0093(12) 0.0028(8) -0.0002(12) O6 0.0111(11) 0.0045(13) 0.0165(11) 0.0065(11) 0.0048(9) -0.0015(11) O4 0.0102(11) 0.0071(13) 0.0178(11) 0.0093(12) 0.0028(8) -0.0002(12) O3 0.0102(11) 0.0071(13) 0.0178(11) 0.0093(12) 0.0028(8) -0.0002(12) O2 0.0102(11) 0.0071(13) 0.0178(11) 0.0093(12) 0.0028(8) -0.0002(12) C7 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) C1 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) C4 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) C2 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) C5 0.0152(10) 0.0127(12) 0.0182(10) 0.0057(15) 0.0056(8) -0.0007(15) C3 0.0081(6) 0.0040(8) 0.0152(6) 0.0053(11) 0.0037(5) 0.0029(11) C6 0.0152(10) 0.0127(12) 0.0182(10) 0.0057(15) 0.0056(8) -0.0007(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li2 O2 1.887(12) . ? Li2 O7 1.969(12) 2_586 ? Li2 O2 1.971(12) 2_576 ? Li2 O3 1.988(11) 1_455 ? Li2 Li2 2.70(2) 2_576 ? Li2 C4 2.725(12) 1_455 ? Li2 Li3 2.978(16) 2_576 ? Li2 Li4 3.192(16) 2_576 ? Li2 Li4 3.473(15) 1_455 ? Li3 O1 1.955(12) . ? Li3 O7 1.989(11) 1_545 ? Li3 O8 1.994(12) 2_576 ? Li3 O6 2.017(10) 2_576 ? Li3 C7 2.607(12) 2_576 ? Li3 C1 2.638(13) . ? Li3 Li2 2.978(16) 2_576 ? Li3 Li1 3.302(15) 2_676 ? Li3 Li1 3.408(15) 1_445 ? Li3 Li4 3.442(16) 2_576 ? Li4 O6 1.916(12) . ? Li4 O3 1.973(13) 2_676 ? Li4 O4 1.985(11) . ? Li4 O1 2.089(10) 2_676 ? Li4 C7 2.654(13) . ? Li4 C1 2.666(12) 2_676 ? Li4 Li1 2.980(17) 2_686 ? Li4 Li2 3.192(16) 2_576 ? Li4 Li3 3.442(16) 2_576 ? Li4 Li2 3.473(15) 1_655 ? O5 C7 1.274(7) . ? O5 Li1 1.950(12) . ? O5 Li1 1.991(11) 2_686 ? C8 C7 1.512(8) . ? C8 C12 1.532(8) . ? C8 C9 1.546(8) . ? C8 C11 1.556(8) . ? C9 C10 1.525(7) . ? C10 O8 1.253(7) . ? C10 O7 1.269(7) . ? C10 Li1 2.699(11) 1_455 ? O8 Li3 1.994(12) 2_576 ? O8 Li1 2.004(11) 1_455 ? O7 Li2 1.969(12) 2_586 ? O7 Li3 1.989(11) 1_565 ? Li1 O4 1.898(12) 2_686 ? Li1 O5 1.991(11) 2_686 ? Li1 O8 2.004(11) 1_655 ? Li1 C10 2.699(11) 1_655 ? Li1 Li1 2.78(2) 2_686 ? Li1 Li4 2.980(17) 2_686 ? Li1 Li3 3.302(15) 2_676 ? Li1 Li3 3.408(15) 1_665 ? O1 C1 1.240(7) . ? O1 Li4 2.089(10) 2_676 ? O6 C7 1.274(7) . ? O6 Li3 2.017(10) 2_576 ? O4 C4 1.257(7) . ? O4 Li1 1.898(12) 2_686 ? O3 C4 1.262(7) . ? O3 Li4 1.973(13) 2_676 ? O3 Li2 1.988(11) 1_655 ? O2 C1 1.250(7) . ? O2 Li2 1.971(12) 2_576 ? C7 Li3 2.607(12) 2_576 ? C1 C2 1.561(8) . ? C1 Li4 2.666(12) 2_676 ? C4 C3 1.525(7) . ? C4 Li2 2.725(12) 1_655 ? C2 C5 1.520(7) . ? C2 C6 1.523(8) . ? C2 C3 1.545(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li2 O7 118.6(6) . 2_586 ? O2 Li2 O2 91.4(5) . 2_576 ? O7 Li2 O2 107.2(5) 2_586 2_576 ? O2 Li2 O3 106.3(6) . 1_455 ? O7 Li2 O3 117.8(6) 2_586 1_455 ? O2 Li2 O3 112.7(6) 2_576 1_455 ? O2 Li2 Li2 47.0(4) . 2_576 ? O7 Li2 Li2 123.4(7) 2_586 2_576 ? O2 Li2 Li2 44.4(3) 2_576 2_576 ? O3 Li2 Li2 118.6(7) 1_455 2_576 ? O2 Li2 C4 128.4(5) . 1_455 ? O7 Li2 C4 93.4(4) 2_586 1_455 ? O2 Li2 C4 118.2(5) 2_576 1_455 ? O3 Li2 C4 25.4(2) 1_455 1_455 ? Li2 Li2 C4 141.2(7) 2_576 1_455 ? O2 Li2 Li3 129.0(5) . 2_576 ? O7 Li2 Li3 41.5(3) 2_586 2_576 ? O2 Li2 Li3 67.3(4) 2_576 2_576 ? O3 Li2 Li3 124.6(5) 1_455 2_576 ? Li2 Li2 Li3 99.1(6) 2_576 2_576 ? C4 Li2 Li3 102.1(4) 1_455 2_576 ? O2 Li2 Li4 79.9(4) . 2_576 ? O7 Li2 Li4 153.9(5) 2_586 2_576 ? O2 Li2 Li4 89.5(4) 2_576 2_576 ? O3 Li2 Li4 36.1(3) 1_455 2_576 ? Li2 Li2 Li4 82.5(5) 2_576 2_576 ? C4 Li2 Li4 60.7(3) 1_455 2_576 ? Li3 Li2 Li4 141.1(5) 2_576 2_576 ? O2 Li2 Li4 149.6(6) . 1_455 ? O7 Li2 Li4 90.4(4) 2_586 1_455 ? O2 Li2 Li4 69.9(4) 2_576 1_455 ? O3 Li2 Li4 63.0(3) 1_455 1_455 ? Li2 Li2 Li4 110.6(6) 2_576 1_455 ? C4 Li2 Li4 52.0(3) 1_455 1_455 ? Li3 Li2 Li4 66.6(3) 2_576 1_455 ? Li4 Li2 Li4 76.4(4) 2_576 1_455 ? O1 Li3 O7 108.4(5) . 1_545 ? O1 Li3 O8 117.5(5) . 2_576 ? O7 Li3 O8 112.0(6) 1_545 2_576 ? O1 Li3 O6 108.2(6) . 2_576 ? O7 Li3 O6 107.4(5) 1_545 2_576 ? O8 Li3 O6 102.8(5) 2_576 2_576 ? O1 Li3 C7 128.2(5) . 2_576 ? O7 Li3 C7 111.7(5) 1_545 2_576 ? O8 Li3 C7 75.2(4) 2_576 2_576 ? O6 Li3 C7 28.5(2) 2_576 2_576 ? O1 Li3 C1 26.4(2) . . ? O7 Li3 C1 100.3(5) 1_545 . ? O8 Li3 C1 140.8(5) 2_576 . ? O6 Li3 C1 87.6(4) 2_576 . ? C7 Li3 C1 113.6(4) 2_576 . ? O1 Li3 Li2 72.6(4) . 2_576 ? O7 Li3 Li2 41.0(3) 1_545 2_576 ? O8 Li3 Li2 149.1(5) 2_576 2_576 ? O6 Li3 Li2 100.8(5) 2_576 2_576 ? C7 Li3 Li2 123.5(4) 2_576 2_576 ? C1 Li3 Li2 59.4(4) . 2_576 ? O1 Li3 Li1 99.3(4) . 2_676 ? O7 Li3 Li1 93.8(4) 1_545 2_676 ? O8 Li3 Li1 34.4(3) 2_576 2_676 ? O6 Li3 Li1 137.2(5) 2_576 2_676 ? C7 Li3 Li1 109.1(4) 2_576 2_676 ? C1 Li3 Li1 125.4(4) . 2_676 ? Li2 Li3 Li1 118.7(5) 2_576 2_676 ? O1 Li3 Li1 155.5(6) . 1_445 ? O7 Li3 Li1 58.6(3) 1_545 1_445 ? O8 Li3 Li1 87.0(4) 2_576 1_445 ? O6 Li3 Li1 62.2(3) 2_576 1_445 ? C7 Li3 Li1 54.0(3) 2_576 1_445 ? C1 Li3 Li1 130.1(4) . 1_445 ? Li2 Li3 Li1 86.7(3) 2_576 1_445 ? Li1 Li3 Li1 102.2(4) 2_676 1_445 ? O1 Li3 Li4 108.6(4) . 2_576 ? O7 Li3 Li4 81.0(4) 1_545 2_576 ? O8 Li3 Li4 123.0(5) 2_576 2_576 ? O6 Li3 Li4 28.1(3) 2_576 2_576 ? C7 Li3 Li4 49.7(3) 2_576 2_576 ? C1 Li3 Li4 82.7(3) . 2_576 ? Li2 Li3 Li4 74.5(3) 2_576 2_576 ? Li1 Li3 Li4 151.9(4) 2_676 2_576 ? Li1 Li3 Li4 51.6(3) 1_445 2_576 ? O6 Li4 O3 119.8(6) . 2_676 ? O6 Li4 O4 108.3(6) . . ? O3 Li4 O4 114.4(5) 2_676 . ? O6 Li4 O1 107.7(5) . 2_676 ? O3 Li4 O1 100.5(5) 2_676 2_676 ? O4 Li4 O1 104.6(5) . 2_676 ? O6 Li4 C7 26.6(2) . . ? O3 Li4 C7 142.7(5) 2_676 . ? O4 Li4 C7 98.6(5) . . ? O1 Li4 C7 87.0(4) 2_676 . ? O6 Li4 C1 126.9(5) . 2_676 ? O3 Li4 C1 74.4(4) 2_676 2_676 ? O4 Li4 C1 109.7(5) . 2_676 ? O1 Li4 C1 26.9(2) 2_676 2_676 ? C7 Li4 C1 111.7(4) . 2_676 ? O6 Li4 Li1 73.3(4) . 2_686 ? O3 Li4 Li1 150.1(5) 2_676 2_686 ? O4 Li4 Li1 38.8(3) . 2_686 ? O1 Li4 Li1 100.3(5) 2_676 2_686 ? C7 Li4 Li1 59.8(3) . 2_686 ? C1 Li4 Li1 121.4(5) 2_676 2_686 ? O6 Li4 Li2 99.9(4) . 2_576 ? O3 Li4 Li2 36.5(3) 2_676 2_576 ? O4 Li4 Li2 97.0(4) . 2_576 ? O1 Li4 Li2 136.9(5) 2_676 2_576 ? C7 Li4 Li2 126.3(4) . 2_576 ? C1 Li4 Li2 110.5(4) 2_676 2_576 ? Li1 Li4 Li2 119.3(5) 2_686 2_576 ? O6 Li4 Li3 29.8(2) . 2_576 ? O3 Li4 Li3 113.0(5) 2_676 2_576 ? O4 Li4 Li3 87.9(4) . 2_576 ? O1 Li4 Li3 135.4(4) 2_676 2_576 ? C7 Li4 Li3 48.6(2) . 2_576 ? C1 Li4 Li3 156.6(5) 2_676 2_576 ? Li1 Li4 Li3 63.6(3) 2_686 2_576 ? Li2 Li4 Li3 81.2(4) 2_576 2_576 ? O6 Li4 Li2 154.5(6) . 1_655 ? O3 Li4 Li2 85.5(4) 2_676 1_655 ? O4 Li4 Li2 59.0(3) . 1_655 ? O1 Li4 Li2 60.2(3) 2_676 1_655 ? C7 Li4 Li2 128.4(5) . 1_655 ? C1 Li4 Li2 52.3(3) 2_676 1_655 ? Li1 Li4 Li2 86.4(4) 2_686 1_655 ? Li2 Li4 Li2 103.6(4) 2_576 1_655 ? Li3 Li4 Li2 146.9(5) 2_576 1_655 ? C7 O5 Li1 151.9(5) . . ? C7 O5 Li1 117.9(5) . 2_686 ? Li1 O5 Li1 89.9(5) . 2_686 ? C7 C8 C12 112.2(5) . . ? C7 C8 C9 106.6(5) . . ? C12 C8 C9 112.2(5) . . ? C7 C8 C11 107.6(5) . . ? C12 C8 C11 108.8(4) . . ? C9 C8 C11 109.3(5) . . ? C10 C9 C8 115.6(5) . . ? O8 C10 O7 124.2(5) . . ? O8 C10 C9 117.4(5) . . ? O7 C10 C9 118.4(5) . . ? O8 C10 Li1 44.3(4) . 1_455 ? O7 C10 Li1 86.8(4) . 1_455 ? C9 C10 Li1 143.0(5) . 1_455 ? C10 O8 Li3 133.4(5) . 2_576 ? C10 O8 Li1 109.8(5) . 1_455 ? Li3 O8 Li1 111.3(5) 2_576 1_455 ? C10 O7 Li2 143.0(5) . 2_586 ? C10 O7 Li3 118.6(5) . 1_565 ? Li2 O7 Li3 97.6(5) 2_586 1_565 ? O4 Li1 O5 118.9(6) 2_686 . ? O4 Li1 O5 106.6(5) 2_686 2_686 ? O5 Li1 O5 90.1(5) . 2_686 ? O4 Li1 O8 121.2(6) 2_686 1_655 ? O5 Li1 O8 102.6(6) . 1_655 ? O5 Li1 O8 113.4(5) 2_686 1_655 ? O4 Li1 C10 96.8(5) 2_686 1_655 ? O5 Li1 C10 126.0(5) . 1_655 ? O5 Li1 C10 118.6(5) 2_686 1_655 ? O8 Li1 C10 25.9(2) 1_655 1_655 ? O4 Li1 Li1 122.8(7) 2_686 2_686 ? O5 Li1 Li1 45.7(3) . 2_686 ? O5 Li1 Li1 44.5(3) 2_686 2_686 ? O8 Li1 Li1 115.9(7) 1_655 2_686 ? C10 Li1 Li1 138.9(7) 1_655 2_686 ? O4 Li1 Li4 40.9(3) 2_686 2_686 ? O5 Li1 Li4 130.6(5) . 2_686 ? O5 Li1 Li4 68.0(4) 2_686 2_686 ? O8 Li1 Li4 126.5(5) 1_655 2_686 ? C10 Li1 Li4 103.1(4) 1_655 2_686 ? Li1 Li1 Li4 100.9(6) 2_686 2_686 ? O4 Li1 Li3 155.5(5) 2_686 2_676 ? O5 Li1 Li3 78.3(4) . 2_676 ? O5 Li1 Li3 89.7(4) 2_686 2_676 ? O8 Li1 Li3 34.2(3) 1_655 2_676 ? C10 Li1 Li3 58.9(3) 1_655 2_676 ? Li1 Li1 Li3 81.6(5) 2_686 2_676 ? Li4 Li1 Li3 141.0(5) 2_686 2_676 ? O4 Li1 Li3 90.4(5) 2_686 1_665 ? O5 Li1 Li3 148.9(6) . 1_665 ? O5 Li1 Li3 70.0(4) 2_686 1_665 ? O8 Li1 Li3 66.5(4) 1_655 1_665 ? C10 Li1 Li3 53.6(3) 1_655 1_665 ? Li1 Li1 Li3 110.8(6) 2_686 1_665 ? Li4 Li1 Li3 64.8(3) 2_686 1_665 ? Li3 Li1 Li3 77.8(4) 2_676 1_665 ? C1 O1 Li3 109.2(5) . . ? C1 O1 Li4 103.5(5) . 2_676 ? Li3 O1 Li4 123.5(4) . 2_676 ? C7 O6 Li4 111.0(5) . . ? C7 O6 Li3 102.4(5) . 2_576 ? Li4 O6 Li3 122.1(4) . 2_576 ? C4 O4 Li1 141.2(5) . 2_686 ? C4 O4 Li4 117.5(5) . . ? Li1 O4 Li4 100.3(5) 2_686 . ? C4 O3 Li4 136.8(5) . 2_676 ? C4 O3 Li2 112.1(5) . 1_655 ? Li4 O3 Li2 107.4(5) 2_676 1_655 ? C1 O2 Li2 152.3(6) . . ? C1 O2 Li2 119.0(5) . 2_576 ? Li2 O2 Li2 88.6(5) . 2_576 ? O5 C7 O6 122.7(5) . . ? O5 C7 C8 118.0(5) . . ? O6 C7 C8 119.3(5) . . ? O5 C7 Li3 112.3(4) . 2_576 ? O6 C7 Li3 49.1(4) . 2_576 ? C8 C7 Li3 105.9(4) . 2_576 ? O5 C7 Li4 87.8(4) . . ? O6 C7 Li4 42.4(4) . . ? C8 C7 Li4 145.6(5) . . ? Li3 C7 Li4 81.7(4) 2_576 . ? O1 C1 O2 123.7(6) . . ? O1 C1 C2 119.3(5) . . ? O2 C1 C2 117.0(5) . . ? O1 C1 Li3 44.4(4) . . ? O2 C1 Li3 87.5(4) . . ? C2 C1 Li3 146.6(4) . . ? O1 C1 Li4 49.6(4) . 2_676 ? O2 C1 Li4 112.6(4) . 2_676 ? C2 C1 Li4 104.3(4) . 2_676 ? Li3 C1 Li4 84.4(4) . 2_676 ? O4 C4 O3 123.0(5) . . ? O4 C4 C3 116.7(5) . . ? O3 C4 C3 120.3(5) . . ? O4 C4 Li2 89.1(4) . 1_655 ? O3 C4 Li2 42.5(4) . 1_655 ? C3 C4 Li2 144.5(4) . 1_655 ? C5 C2 C6 110.9(4) . . ? C5 C2 C3 110.7(5) . . ? C6 C2 C3 108.5(5) . . ? C5 C2 C1 111.2(5) . . ? C6 C2 C1 107.5(5) . . ? C3 C2 C1 107.9(4) . . ? C4 C3 C2 113.9(5) . . ? 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 C7 C8 C9 C10 -34.1(6) . . . . ? C12 C8 C9 C10 89.1(6) . . . . ? C11 C8 C9 C10 -150.2(5) . . . . ? C8 C9 C10 O8 -42.0(7) . . . . ? C8 C9 C10 O7 141.0(5) . . . . ? C8 C9 C10 Li1 -91.2(8) . . . 1_455 ? O7 C10 O8 Li3 -113.2(7) . . . 2_576 ? C9 C10 O8 Li3 70.0(8) . . . 2_576 ? Li1 C10 O8 Li3 -150.8(8) 1_455 . . 2_576 ? O7 C10 O8 Li1 37.6(8) . . . 1_455 ? C9 C10 O8 Li1 -139.3(5) . . . 1_455 ? O8 C10 O7 Li2 -147.4(7) . . . 2_586 ? C9 C10 O7 Li2 29.4(11) . . . 2_586 ? Li1 C10 O7 Li2 -122.2(8) 1_455 . . 2_586 ? O8 C10 O7 Li3 46.3(8) . . . 1_565 ? C9 C10 O7 Li3 -136.9(5) . . . 1_565 ? Li1 C10 O7 Li3 71.5(5) 1_455 . . 1_565 ? C7 O5 Li1 O4 63.2(13) . . . 2_686 ? Li1 O5 Li1 O4 -109.1(7) 2_686 . . 2_686 ? C7 O5 Li1 O5 172.3(10) . . . 2_686 ? Li1 O5 Li1 O5 0 2_686 . . 2_686 ? C7 O5 Li1 O8 -73.7(12) . . . 1_655 ? Li1 O5 Li1 O8 114.0(6) 2_686 . . 1_655 ? C7 O5 Li1 C10 -61.3(13) . . . 1_655 ? Li1 O5 Li1 C10 126.4(8) 2_686 . . 1_655 ? C7 O5 Li1 Li1 172.3(10) . . . 2_686 ? C7 O5 Li1 Li4 111.7(10) . . . 2_686 ? Li1 O5 Li1 Li4 -60.6(6) 2_686 . . 2_686 ? C7 O5 Li1 Li3 -98.0(10) . . . 2_676 ? Li1 O5 Li1 Li3 89.7(4) 2_686 . . 2_676 ? C7 O5 Li1 Li3 -138.8(10) . . . 1_665 ? Li1 O5 Li1 Li3 49.0(8) 2_686 . . 1_665 ? O7 Li3 O1 C1 75.6(6) 1_545 . . . ? O8 Li3 O1 C1 -156.3(5) 2_576 . . . ? O6 Li3 O1 C1 -40.6(6) 2_576 . . . ? C7 Li3 O1 C1 -63.8(8) 2_576 . . . ? Li2 Li3 O1 C1 55.4(5) 2_576 . . . ? Li1 Li3 O1 C1 172.7(4) 2_676 . . . ? Li1 Li3 O1 C1 21.8(14) 1_445 . . . ? Li4 Li3 O1 C1 -10.9(6) 2_576 . . . ? O7 Li3 O1 Li4 -46.3(8) 1_545 . . 2_676 ? O8 Li3 O1 Li4 81.9(7) 2_576 . . 2_676 ? O6 Li3 O1 Li4 -162.4(4) 2_576 . . 2_676 ? C7 Li3 O1 Li4 174.4(5) 2_576 . . 2_676 ? C1 Li3 O1 Li4 -121.8(7) . . . 2_676 ? Li2 Li3 O1 Li4 -66.4(6) 2_576 . . 2_676 ? Li1 Li3 O1 Li4 50.9(6) 2_676 . . 2_676 ? Li1 Li3 O1 Li4 -100.0(13) 1_445 . . 2_676 ? Li4 Li3 O1 Li4 -132.7(6) 2_576 . . 2_676 ? O3 Li4 O6 C7 -154.5(6) 2_676 . . . ? O4 Li4 O6 C7 71.9(6) . . . . ? O1 Li4 O6 C7 -40.8(7) 2_676 . . . ? C1 Li4 O6 C7 -62.1(8) 2_676 . . . ? Li1 Li4 O6 C7 55.0(5) 2_686 . . . ? Li2 Li4 O6 C7 172.8(4) 2_576 . . . ? Li3 Li4 O6 C7 120.8(7) 2_576 . . . ? Li2 Li4 O6 C7 16.2(13) 1_655 . . . ? O3 Li4 O6 Li3 84.7(7) 2_676 . . 2_576 ? O4 Li4 O6 Li3 -49.0(8) . . . 2_576 ? O1 Li4 O6 Li3 -161.6(5) 2_676 . . 2_576 ? C7 Li4 O6 Li3 -120.8(7) . . . 2_576 ? C1 Li4 O6 Li3 177.1(5) 2_676 . . 2_576 ? Li1 Li4 O6 Li3 -65.8(6) 2_686 . . 2_576 ? Li2 Li4 O6 Li3 51.9(7) 2_576 . . 2_576 ? Li2 Li4 O6 Li3 -104.6(12) 1_655 . . 2_576 ? O6 Li4 O4 C4 144.2(5) . . . . ? O3 Li4 O4 C4 7.7(8) 2_676 . . . ? O1 Li4 O4 C4 -101.2(6) 2_676 . . . ? C7 Li4 O4 C4 169.7(4) . . . . ? C1 Li4 O4 C4 -73.5(6) 2_676 . . . ? Li1 Li4 O4 C4 170.5(6) 2_686 . . . ? Li2 Li4 O4 C4 41.3(6) 2_576 . . . ? Li3 Li4 O4 C4 122.2(4) 2_576 . . . ? Li2 Li4 O4 C4 -60.4(5) 1_655 . . . ? O6 Li4 O4 Li1 -26.3(6) . . . 2_686 ? O3 Li4 O4 Li1 -162.7(6) 2_676 . . 2_686 ? O1 Li4 O4 Li1 88.3(6) 2_676 . . 2_686 ? C7 Li4 O4 Li1 -0.8(5) . . . 2_686 ? C1 Li4 O4 Li1 116.0(5) 2_676 . . 2_686 ? Li2 Li4 O4 Li1 -129.2(5) 2_576 . . 2_686 ? Li3 Li4 O4 Li1 -48.3(4) 2_576 . . 2_686 ? Li2 Li4 O4 Li1 129.2(4) 1_655 . . 2_686 ? O7 Li2 O2 C1 64.6(13) 2_586 . . . ? O2 Li2 O2 C1 175.0(10) 2_576 . . . ? O3 Li2 O2 C1 -70.8(13) 1_455 . . . ? Li2 Li2 O2 C1 175.0(10) 2_576 . . . ? C4 Li2 O2 C1 -56.5(15) 1_455 . . . ? Li3 Li2 O2 C1 113.5(11) 2_576 . . . ? Li4 Li2 O2 C1 -95.7(11) 2_576 . . . ? Li4 Li2 O2 C1 -134.8(11) 1_455 . . . ? O7 Li2 O2 Li2 -110.5(7) 2_586 . . 2_576 ? O2 Li2 O2 Li2 0 2_576 . . 2_576 ? O3 Li2 O2 Li2 114.1(7) 1_455 . . 2_576 ? C4 Li2 O2 Li2 128.4(9) 1_455 . . 2_576 ? Li3 Li2 O2 Li2 -61.5(6) 2_576 . . 2_576 ? Li4 Li2 O2 Li2 89.2(4) 2_576 . . 2_576 ? Li4 Li2 O2 Li2 50.2(8) 1_455 . . 2_576 ? Li1 O5 C7 O6 161.7(9) . . . . ? Li1 O5 C7 O6 -27.1(8) 2_686 . . . ? Li1 O5 C7 C8 -20.0(13) . . . . ? Li1 O5 C7 C8 151.3(5) 2_686 . . . ? Li1 O5 C7 Li3 -143.7(10) . . . 2_576 ? Li1 O5 C7 Li3 27.6(7) 2_686 . . 2_576 ? Li1 O5 C7 Li4 136.2(11) . . . . ? Li1 O5 C7 Li4 -52.5(5) 2_686 . . . ? Li4 O6 C7 O5 -39.5(8) . . . . ? Li3 O6 C7 O5 92.3(6) 2_576 . . . ? Li4 O6 C7 C8 142.2(5) . . . . ? Li3 O6 C7 C8 -86.0(6) 2_576 . . . ? Li4 O6 C7 Li3 -131.9(5) . . . 2_576 ? Li3 O6 C7 Li4 131.9(5) 2_576 . . . ? C12 C8 C7 O5 -175.3(5) . . . . ? C9 C8 C7 O5 -52.1(6) . . . . ? C11 C8 C7 O5 65.0(7) . . . . ? C12 C8 C7 O6 3.1(7) . . . . ? C9 C8 C7 O6 126.3(6) . . . . ? C11 C8 C7 O6 -116.6(6) . . . . ? C12 C8 C7 Li3 -48.5(6) . . . 2_576 ? C9 C8 C7 Li3 74.7(5) . . . 2_576 ? C11 C8 C7 Li3 -168.2(4) . . . 2_576 ? C12 C8 C7 Li4 50.2(9) . . . . ? C9 C8 C7 Li4 173.4(6) . . . . ? C11 C8 C7 Li4 -69.5(9) . . . . ? O6 Li4 C7 O5 147.6(6) . . . . ? O3 Li4 C7 O5 -174.3(9) 2_676 . . . ? O4 Li4 C7 O5 33.4(4) . . . . ? O1 Li4 C7 O5 -70.9(4) 2_676 . . . ? C1 Li4 C7 O5 -81.9(5) 2_676 . . . ? Li1 Li4 C7 O5 32.8(4) 2_686 . . . ? Li2 Li4 C7 O5 138.7(5) 2_576 . . . ? Li3 Li4 C7 O5 112.9(4) 2_576 . . . ? Li2 Li4 C7 O5 -23.6(5) 1_655 . . . ? O3 Li4 C7 O6 38.1(8) 2_676 . . . ? O4 Li4 C7 O6 -114.2(6) . . . . ? O1 Li4 C7 O6 141.5(6) 2_676 . . . ? C1 Li4 C7 O6 130.5(7) 2_676 . . . ? Li1 Li4 C7 O6 -114.8(6) 2_686 . . . ? Li2 Li4 C7 O6 -8.9(5) 2_576 . . . ? Li3 Li4 C7 O6 -34.7(4) 2_576 . . . ? Li2 Li4 C7 O6 -171.2(7) 1_655 . . . ? O6 Li4 C7 C8 -71.5(9) . . . . ? O3 Li4 C7 C8 -33.4(13) 2_676 . . . ? O4 Li4 C7 C8 174.4(7) . . . . ? O1 Li4 C7 C8 70.0(8) 2_676 . . . ? C1 Li4 C7 C8 59.1(9) 2_676 . . . ? Li1 Li4 C7 C8 173.8(8) 2_686 . . . ? Li2 Li4 C7 C8 -80.3(9) 2_576 . . . ? Li3 Li4 C7 C8 -106.1(8) 2_576 . . . ? Li2 Li4 C7 C8 117.4(8) 1_655 . . . ? O6 Li4 C7 Li3 34.7(4) . . . 2_576 ? O3 Li4 C7 Li3 72.7(8) 2_676 . . 2_576 ? O4 Li4 C7 Li3 -79.5(4) . . . 2_576 ? O1 Li4 C7 Li3 176.1(5) 2_676 . . 2_576 ? C1 Li4 C7 Li3 165.2(6) 2_676 . . 2_576 ? Li1 Li4 C7 Li3 -80.1(4) 2_686 . . 2_576 ? Li2 Li4 C7 Li3 25.8(5) 2_576 . . 2_576 ? Li2 Li4 C7 Li3 -136.5(6) 1_655 . . 2_576 ? Li3 O1 C1 O2 -41.0(8) . . . . ? Li4 O1 C1 O2 92.3(6) 2_676 . . . ? Li3 O1 C1 C2 142.7(5) . . . . ? Li4 O1 C1 C2 -84.0(6) 2_676 . . . ? Li4 O1 C1 Li3 133.2(5) 2_676 . . . ? Li3 O1 C1 Li4 -133.2(5) . . . 2_676 ? Li2 O2 C1 O1 159.6(9) . . . . ? Li2 O2 C1 O1 -26.1(8) 2_576 . . . ? Li2 O2 C1 C2 -24.1(13) . . . . ? Li2 O2 C1 C2 150.3(5) 2_576 . . . ? Li2 O2 C1 Li3 132.2(11) . . . . ? Li2 O2 C1 Li3 -53.4(5) 2_576 . . . ? Li2 O2 C1 Li4 -144.9(10) . . . 2_676 ? Li2 O2 C1 Li4 29.4(7) 2_576 . . 2_676 ? O7 Li3 C1 O1 -111.0(6) 1_545 . . . ? O8 Li3 C1 O1 34.3(7) 2_576 . . . ? O6 Li3 C1 O1 141.8(6) 2_576 . . . ? C7 Li3 C1 O1 129.7(7) 2_576 . . . ? Li2 Li3 C1 O1 -114.2(6) 2_576 . . . ? Li1 Li3 C1 O1 -8.8(5) 2_676 . . . ? Li1 Li3 C1 O1 -168.4(7) 1_445 . . . ? Li4 Li3 C1 O1 169.6(6) 2_576 . . . ? O1 Li3 C1 O2 146.9(7) . . . . ? O7 Li3 C1 O2 35.9(4) 1_545 . . . ? O8 Li3 C1 O2 -178.8(8) 2_576 . . . ? O6 Li3 C1 O2 -71.4(4) 2_576 . . . ? C7 Li3 C1 O2 -83.4(5) 2_576 . . . ? Li2 Li3 C1 O2 32.7(4) 2_576 . . . ? Li1 Li3 C1 O2 138.0(5) 2_676 . . . ? Li1 Li3 C1 O2 -21.5(6) 1_445 . . . ? Li4 Li3 C1 O2 -43.5(4) 2_576 . . . ? O1 Li3 C1 C2 -73.8(8) . . . . ? O7 Li3 C1 C2 175.2(6) 1_545 . . . ? O8 Li3 C1 C2 -39.5(12) 2_576 . . . ? O6 Li3 C1 C2 68.0(8) 2_576 . . . ? C7 Li3 C1 C2 55.9(9) 2_576 . . . ? Li2 Li3 C1 C2 172.0(8) 2_576 . . . ? Li1 Li3 C1 C2 -82.7(8) 2_676 . . . ? Li1 Li3 C1 C2 117.8(8) 1_445 . . . ? Li4 Li3 C1 C2 95.8(7) 2_576 . . . ? O1 Li3 C1 Li4 33.9(4) . . . 2_676 ? O7 Li3 C1 Li4 -77.1(4) 1_545 . . 2_676 ? O8 Li3 C1 Li4 68.2(8) 2_576 . . 2_676 ? O6 Li3 C1 Li4 175.7(5) 2_576 . . 2_676 ? C7 Li3 C1 Li4 163.6(5) 2_576 . . 2_676 ? Li2 Li3 C1 Li4 -80.3(4) 2_576 . . 2_676 ? Li1 Li3 C1 Li4 25.1(4) 2_676 . . 2_676 ? Li1 Li3 C1 Li4 -134.5(6) 1_445 . . 2_676 ? Li4 Li3 C1 Li4 -156.5(5) 2_576 . . 2_676 ? Li1 O4 C4 O3 -150.6(7) 2_686 . . . ? Li4 O4 C4 O3 44.4(8) . . . . ? Li1 O4 C4 C3 31.3(10) 2_686 . . . ? Li4 O4 C4 C3 -133.6(5) . . . . ? Li1 O4 C4 Li2 -123.3(7) 2_686 . . 1_655 ? Li4 O4 C4 Li2 71.7(5) . . . 1_655 ? Li4 O3 C4 O4 -111.9(8) 2_676 . . . ? Li2 O3 C4 O4 42.8(8) 1_655 . . . ? Li4 O3 C4 C3 66.1(9) 2_676 . . . ? Li2 O3 C4 C3 -139.2(6) 1_655 . . . ? Li4 O3 C4 Li2 -154.6(9) 2_676 . . 1_655 ? O1 C1 C2 C5 5.1(7) . . . . ? O2 C1 C2 C5 -171.4(5) . . . . ? Li3 C1 C2 C5 55.5(8) . . . . ? Li4 C1 C2 C5 -46.4(5) 2_676 . . . ? O1 C1 C2 C6 -116.5(5) . . . . ? O2 C1 C2 C6 67.0(6) . . . . ? Li3 C1 C2 C6 -66.0(9) . . . . ? Li4 C1 C2 C6 -167.9(4) 2_676 . . . ? O1 C1 C2 C3 126.7(6) . . . . ? O2 C1 C2 C3 -49.8(6) . . . . ? Li3 C1 C2 C3 177.1(6) . . . . ? Li4 C1 C2 C3 75.2(5) 2_676 . . . ? O4 C4 C3 C2 140.8(5) . . . . ? O3 C4 C3 C2 -37.3(7) . . . . ? Li2 C4 C3 C2 -86.7(9) 1_655 . . . ? C5 C2 C3 C4 84.8(6) . . . . ? C6 C2 C3 C4 -153.3(5) . . . . ? C1 C2 C3 C4 -37.1(6) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF