# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- MF3_all6_1.txt' #============================================================================== # SUBMISSION DETAILS # ================== _publ_contact_author_name 'Professor Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; December 2010 Dear Sirs, This file contains crystallographic data in cif format for six structures. It is offered as supporting information to accompany a paper to be submitted shortly. Gillian Reid ; _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Unusual Neutral Ligand Complexes of Arsenic and Antimony Trifluorides ; loop_ _publ_author_name _publ_author_address _publ_author_footnote W.Levason ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? M.E.Light ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? S.Maheshwari ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ; Current address: Department of Pure and Applied Chemistry M.D.S University Ajmer-305009, India ; G.Reid ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? W.Zhang ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? #============================================================================ # 10sm520a CCDC-803403 # 10sm527ax CCDC-803404 # 10sm527b CCDC-803405 # 10sm708b CCDC-803406 # 10sm819a CCDC-803407 # 2010sm715a CCDC-803408 #============================================================================ # 10sm520a data_10sm520a _database_code_depnum_ccdc_archive 'CCDC 803403' #TrackingRef '- MF3_all6_1.txt' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-07-13 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trifluoro(methanediylbis(diphenylphosphane) dioxide)antimony(III) ; # Ph2P(O)CH2P(O)Ph2 = C25H22O2P2 = dppmO2 # methylenebis(diphenylphosphine) dioxide (iLab defaults) seems wrong (mw) # methanediylbis(diphenylphosphane) dioxide (iLab selected options) # methanediylbis(diphenylphosphane) dioxide (chemspider) # [(Diphenylphosphoryl)methyl](diphenyl)phosphine oxide (chemspider synonym) # bis(diphenylphosphino)methane dioxide _chemical_name_common ;trifluoro(methanediylbis(diphenylphosphane) dioxide)antimony(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C25 H22 F3 O2 P2 Sb' _chemical_formula_sum 'C25 H22 F3 O2 P2 Sb' _chemical_formula_weight 595.12 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.4165(15) _cell_length_b 13.335(2) _cell_length_c 15.599(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2374.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3021 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7950 # 0.8888 _exptl_absorpt_correction_T_max 1.0000 # 0.9239 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17960 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5133 _reflns_number_gt 4639 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^)+(0.0000P)^2^+5.3493P] 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 constr _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 0.12(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 5133 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.56504(3) 0.07904(3) 0.07398(2) 0.02189(9) Uani 1 1 d . . . F1 F 0.5446(2) 0.0804(2) 0.19586(16) 0.0256(6) Uani 1 1 d . . . F2 F 0.7162(2) 0.0178(2) 0.0877(2) 0.0315(7) Uani 1 1 d . . . F3 F 0.4925(3) -0.0581(2) 0.0875(2) 0.0355(8) Uani 1 1 d . . . P1 P 0.39719(11) 0.30252(10) 0.13884(9) 0.0203(3) Uani 1 1 d . . . P2 P 0.65062(11) 0.28453(10) 0.19352(9) 0.0205(3) Uani 1 1 d . . . O1 O 0.3939(3) 0.2052(3) 0.0916(2) 0.0234(8) Uani 1 1 d . . . O2 O 0.6625(3) 0.2236(3) 0.1125(2) 0.0213(8) Uani 1 1 d . . . C1 C 0.2569(4) 0.3309(4) 0.1846(3) 0.0207(11) Uani 1 1 d . . . C2 C 0.1586(4) 0.3030(4) 0.1364(4) 0.0271(12) Uani 1 1 d . . . H2 H 0.1674 0.2736 0.0813 0.033 Uiso 1 1 calc R . . C3 C 0.0474(4) 0.3191(4) 0.1710(3) 0.0289(12) Uani 1 1 d . . . H3 H -0.0200 0.3013 0.1388 0.035 Uiso 1 1 calc R . . C4 C 0.0342(4) 0.3608(4) 0.2518(4) 0.0309(13) Uani 1 1 d . . . H4 H -0.0418 0.3701 0.2753 0.037 Uiso 1 1 calc R . . C5 C 0.1319(4) 0.3888(5) 0.2979(4) 0.0329(14) Uani 1 1 d . . . H5 H 0.1230 0.4183 0.3529 0.040 Uiso 1 1 calc R . . C6 C 0.2435(4) 0.3741(4) 0.2645(4) 0.0296(13) Uani 1 1 d . . . H6 H 0.3104 0.3937 0.2965 0.036 Uiso 1 1 calc R . . C7 C 0.4445(4) 0.4045(3) 0.0716(3) 0.0201(9) Uani 1 1 d . . . C8 C 0.4497(5) 0.5024(4) 0.1024(3) 0.0300(12) Uani 1 1 d . . . H8 H 0.4185 0.5187 0.1571 0.036 Uiso 1 1 calc R . . C9 C 0.5010(4) 0.5755(5) 0.0519(3) 0.0317(12) Uani 1 1 d . . . H9 H 0.5055 0.6425 0.0723 0.038 Uiso 1 1 calc R . . C10 C 0.5459(4) 0.5518(4) -0.0282(3) 0.0304(13) Uani 1 1 d . . . H10 H 0.5818 0.6024 -0.0621 0.036 Uiso 1 1 calc R . . C11 C 0.5386(4) 0.4549(4) -0.0589(3) 0.0327(13) Uani 1 1 d . . . H11 H 0.5687 0.4388 -0.1140 0.039 Uiso 1 1 calc R . . C12 C 0.4870(4) 0.3809(4) -0.0088(3) 0.0262(12) Uani 1 1 d . . . H12 H 0.4809 0.3143 -0.0298 0.031 Uiso 1 1 calc R . . C13 C 0.4988(4) 0.3000(4) 0.2276(3) 0.0225(11) Uani 1 1 d . . . H13A H 0.4776 0.2442 0.2665 0.027 Uiso 1 1 calc R . . H13B H 0.4916 0.3633 0.2603 0.027 Uiso 1 1 calc R . . C14 C 0.7111(4) 0.4076(4) 0.1774(3) 0.0226(11) Uani 1 1 d . . . C15 C 0.7045(5) 0.4803(4) 0.2408(3) 0.0250(12) Uani 1 1 d . . . H15 H 0.6659 0.4657 0.2933 0.030 Uiso 1 1 calc R . . C16 C 0.7538(4) 0.5739(5) 0.2281(4) 0.0314(12) Uani 1 1 d . . . H16 H 0.7493 0.6238 0.2715 0.038 Uiso 1 1 calc R . . C17 C 0.8089(5) 0.5934(5) 0.1525(4) 0.0357(14) Uani 1 1 d . . . H17 H 0.8447 0.6571 0.1445 0.043 Uiso 1 1 calc R . . C18 C 0.8145(4) 0.5234(4) 0.0866(4) 0.0319(13) Uani 1 1 d . . . H18 H 0.8508 0.5399 0.0336 0.038 Uiso 1 1 calc R . . C19 C 0.7665(4) 0.4298(5) 0.0994(3) 0.0293(12) Uani 1 1 d . . . H19 H 0.7709 0.3805 0.0556 0.035 Uiso 1 1 calc R . . C20 C 0.7275(4) 0.2303(4) 0.2826(4) 0.0273(12) Uani 1 1 d . . . C21 C 0.8089(4) 0.1550(4) 0.2667(4) 0.0307(13) Uani 1 1 d . . . H21 H 0.8204 0.1301 0.2102 0.037 Uiso 1 1 calc R . . C22 C 0.8732(6) 0.1169(5) 0.3351(5) 0.0459(18) Uani 1 1 d . . . H22 H 0.9301 0.0663 0.3250 0.055 Uiso 1 1 calc R . . C23 C 0.8558(5) 0.1509(4) 0.4156(4) 0.0412(16) Uani 1 1 d . . . H23 H 0.9018 0.1244 0.4610 0.049 Uiso 1 1 calc R . . C24 C 0.7733(5) 0.2228(4) 0.4334(4) 0.0388(14) Uani 1 1 d . . . H24 H 0.7614 0.2449 0.4906 0.047 Uiso 1 1 calc R . . C25 C 0.7062(5) 0.2636(4) 0.3658(4) 0.0325(13) Uani 1 1 d . . . H25 H 0.6478 0.3127 0.3768 0.039 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 Sb1 0.02234(14) 0.02229(16) 0.02105(15) 0.00131(15) 0.00115(15) 0.00113(15) F1 0.0266(15) 0.0287(15) 0.0214(13) -0.0002(13) 0.0008(11) -0.0031(15) F2 0.0259(15) 0.0328(17) 0.0357(19) 0.0060(15) 0.0033(14) 0.0099(13) F3 0.0378(16) 0.0362(19) 0.0323(18) 0.0015(15) 0.0041(14) -0.0092(14) P1 0.0161(6) 0.0229(7) 0.0220(6) -0.0024(5) -0.0014(5) 0.0019(5) P2 0.0148(6) 0.0205(7) 0.0261(7) 0.0022(5) -0.0020(5) 0.0016(5) O1 0.0206(16) 0.0242(18) 0.025(2) -0.0043(15) -0.0031(14) 0.0012(14) O2 0.0191(17) 0.0191(18) 0.0258(19) 0.0002(14) 0.0016(14) -0.0009(15) C1 0.020(2) 0.020(3) 0.022(3) 0.005(2) 0.000(2) -0.001(2) C2 0.022(3) 0.035(3) 0.025(3) 0.000(2) -0.002(2) 0.001(2) C3 0.018(3) 0.035(3) 0.034(3) -0.006(2) -0.003(2) -0.002(2) C4 0.017(3) 0.036(3) 0.041(3) -0.010(3) 0.002(2) -0.001(2) C5 0.017(2) 0.047(4) 0.035(3) -0.011(3) 0.002(2) -0.003(2) C6 0.015(2) 0.033(3) 0.040(3) -0.011(3) 0.002(2) -0.006(2) C7 0.0135(19) 0.028(3) 0.019(2) 0.004(2) 0.002(2) 0.004(2) C8 0.032(3) 0.032(3) 0.026(3) 0.001(2) -0.004(3) 0.000(3) C9 0.032(3) 0.025(3) 0.038(3) -0.001(3) -0.008(2) 0.001(3) C10 0.021(3) 0.037(3) 0.033(3) 0.010(2) 0.000(2) 0.000(2) C11 0.029(3) 0.045(3) 0.025(3) 0.007(2) 0.001(2) 0.009(2) C12 0.024(2) 0.033(3) 0.022(3) -0.002(2) -0.006(2) 0.003(2) C13 0.018(2) 0.021(3) 0.029(3) 0.003(2) -0.003(2) 0.000(2) C14 0.014(2) 0.021(3) 0.033(3) 0.004(2) -0.003(2) 0.004(2) C15 0.028(3) 0.019(3) 0.028(3) 0.002(2) 0.002(2) 0.005(2) C16 0.028(3) 0.022(3) 0.044(3) -0.006(3) -0.008(2) 0.003(3) C17 0.022(3) 0.029(3) 0.057(4) 0.011(3) -0.002(3) -0.001(3) C18 0.021(2) 0.032(3) 0.043(4) 0.012(3) 0.003(3) 0.001(2) C19 0.018(2) 0.031(3) 0.039(3) 0.003(3) 0.000(2) 0.008(2) C20 0.020(2) 0.024(3) 0.037(3) 0.009(2) -0.010(2) -0.002(2) C21 0.018(2) 0.023(3) 0.052(4) -0.001(3) -0.008(3) 0.004(2) C22 0.039(4) 0.030(3) 0.069(5) 0.010(3) -0.023(3) 0.007(3) C23 0.043(3) 0.031(3) 0.049(4) 0.015(3) -0.032(3) -0.010(3) C24 0.045(3) 0.035(3) 0.036(3) 0.006(3) -0.010(3) -0.011(3) C25 0.033(3) 0.024(3) 0.041(3) 0.008(3) -0.012(3) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F1 1.916(3) . ? Sb1 F2 1.921(3) . ? Sb1 F3 2.018(3) . ? Sb1 O2 2.306(3) . ? Sb1 O1 2.593(3) . ? P1 O1 1.493(4) . ? P1 C1 1.794(5) . ? P1 C7 1.800(5) . ? P1 C13 1.807(5) . ? P2 O2 1.508(4) . ? P2 C20 1.795(5) . ? P2 C14 1.797(6) . ? P2 C13 1.825(5) . ? C1 C6 1.380(7) . ? C1 C2 1.402(7) . ? C2 C3 1.396(7) . ? C2 H2 0.9500 . ? C3 C4 1.386(8) . ? C3 H3 0.9500 . ? C4 C5 1.379(7) . ? C4 H4 0.9500 . ? C5 C6 1.390(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.380(7) . ? C7 C8 1.392(7) . ? C8 C9 1.383(8) . ? C8 H8 0.9500 . ? C9 C10 1.388(8) . ? C9 H9 0.9500 . ? C10 C11 1.380(8) . ? C10 H10 0.9500 . ? C11 C12 1.389(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.387(7) . ? C14 C19 1.403(7) . ? C15 C16 1.384(8) . ? C15 H15 0.9500 . ? C16 C17 1.362(8) . ? C16 H16 0.9500 . ? C17 C18 1.390(9) . ? C17 H17 0.9500 . ? C18 C19 1.378(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.391(7) . ? C20 C25 1.392(8) . ? C21 C22 1.391(8) . ? C21 H21 0.9500 . ? C22 C23 1.349(10) . ? C22 H22 0.9500 . ? C23 C24 1.373(9) . ? C23 H23 0.9500 . ? C24 C25 1.412(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Sb1 F2 90.17(13) . . ? F1 Sb1 F3 81.68(13) . . ? F2 Sb1 F3 88.40(13) . . ? F1 Sb1 O2 78.01(12) . . ? F2 Sb1 O2 83.85(13) . . ? F3 Sb1 O2 158.20(12) . . ? F1 Sb1 O1 78.27(12) . . ? F2 Sb1 O1 160.21(12) . . ? F3 Sb1 O1 105.49(12) . . ? O2 Sb1 O1 78.10(11) . . ? O1 P1 C1 110.9(2) . . ? O1 P1 C7 112.1(2) . . ? C1 P1 C7 109.9(2) . . ? O1 P1 C13 112.2(2) . . ? C1 P1 C13 105.8(2) . . ? C7 P1 C13 105.6(2) . . ? O2 P2 C20 112.8(2) . . ? O2 P2 C14 109.8(2) . . ? C20 P2 C14 106.7(2) . . ? O2 P2 C13 113.0(2) . . ? C20 P2 C13 106.5(3) . . ? C14 P2 C13 107.6(2) . . ? P1 O1 Sb1 126.67(18) . . ? P2 O2 Sb1 128.67(19) . . ? C6 C1 C2 120.4(5) . . ? C6 C1 P1 123.1(4) . . ? C2 C1 P1 116.4(4) . . ? C3 C2 C1 118.6(5) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 120.9(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.5(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 119.9(5) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C12 C7 C8 120.8(5) . . ? C12 C7 P1 117.6(4) . . ? C8 C7 P1 121.3(4) . . ? C9 C8 C7 118.8(5) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 120.6(6) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.2(5) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 119.9(5) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? P1 C13 P2 112.9(3) . . ? P1 C13 H13A 109.0 . . ? P2 C13 H13A 109.0 . . ? P1 C13 H13B 109.0 . . ? P2 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C19 119.6(5) . . ? C15 C14 P2 121.2(4) . . ? C19 C14 P2 119.2(4) . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 118.9(6) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 122.3(6) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 118.9(5) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C14 119.8(6) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? C21 C20 C25 120.9(5) . . ? C21 C20 P2 118.6(5) . . ? C25 C20 P2 120.5(4) . . ? C20 C21 C22 118.6(6) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C23 C22 C21 120.9(6) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 121.6(6) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C25 119.4(6) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C20 C25 C24 118.6(5) . . ? C20 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? 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 Sb1 O1 P1 C13 -30.4(3) . . . . ? O1 P1 C13 P2 64.7(3) . . . . ? P1 C13 P2 O2 -31.1(4) . . . . ? C13 P2 O2 Sb1 -42.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.631 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.121 #===END OF CIF ============================================================== # 10sm527ax data_10sm527ax _database_code_depnum_ccdc_archive 'CCDC 803404' #TrackingRef '- MF3_all6_1.txt' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-07-15 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(methanediylbis(dimethylphosphane) dioxide)bis(trifluoroantimony(III)) ; # CH2{P(O)Me2}2 = Me2P(O)CH2P(O)Me2 = C5H14O2P2 # methanediylbis(dimethylphosphane) dioxide (ACD iLab selected options) # methanediylbis(dimethylphosphane) dioxide (chemspider) _chemical_name_common ;bis(methanediylbis(dimethylphosphane) dioxide)bis(trifluoroantimony(iii)) ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H28 F6 O4 P4 Sb2' _chemical_formula_sum 'C10 H28 F6 O4 P4 Sb2' _chemical_formula_structural '(C5 H14 O2 P2)2 (F3 Sb)2' _chemical_formula_weight 693.70 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8949(15) _cell_length_b 8.4721(10) _cell_length_c 16.1193(15) _cell_angle_alpha 90.00 _cell_angle_beta 109.908(5) _cell_angle_gamma 90.00 _cell_volume 2297.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5509 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8896 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25860 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.58 _reflns_number_total 5254 _reflns_number_gt 4644 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^)+(0.0000P)^2^+7.5910P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5254 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.401919(14) 0.89797(3) 0.412306(15) 0.01508(7) Uani 1 1 d . . . Sb2 Sb 0.096822(14) 0.43777(3) 0.451491(15) 0.01591(7) Uani 1 1 d . . . F1 F 0.37411(13) 0.7136(3) 0.33965(13) 0.0211(5) Uani 1 1 d . . . F2 F 0.50975(13) 0.8777(3) 0.40674(15) 0.0263(5) Uani 1 1 d . . . F3 F 0.37918(13) 1.0160(3) 0.30102(14) 0.0246(5) Uani 1 1 d . . . F4 F 0.12143(14) 0.3659(3) 0.35153(14) 0.0269(5) Uani 1 1 d . . . F5 F 0.12005(14) 0.2208(3) 0.49555(16) 0.0296(5) Uani 1 1 d . . . F6 F -0.01269(13) 0.3608(3) 0.39426(16) 0.0313(6) Uani 1 1 d . . . P1 P 0.43635(6) 0.64360(11) 0.60582(6) 0.01593(19) Uani 1 1 d . . . P2 P 0.31195(6) 0.38066(11) 0.51882(6) 0.01609(19) Uani 1 1 d . . . P3 P 0.06333(6) 0.82956(12) 0.38144(6) 0.01655(19) Uani 1 1 d . . . P4 P 0.18972(6) 0.89979(13) 0.29409(6) 0.0192(2) Uani 1 1 d . . . O1 O 0.44873(16) 0.6856(3) 0.52048(16) 0.0217(6) Uani 1 1 d . . . O2 O 0.24080(15) 0.4843(3) 0.50872(17) 0.0221(6) Uani 1 1 d . . . O3 O 0.05348(16) 0.6592(3) 0.35275(16) 0.0215(6) Uani 1 1 d . . . O4 O 0.25975(15) 0.9110(3) 0.37856(16) 0.0200(6) Uani 1 1 d . . . C1 C 0.5262(2) 0.6445(5) 0.6989(2) 0.0227(8) Uani 1 1 d . . . H1A H 0.5649 0.5732 0.6877 0.034 Uiso 1 1 calc R . . H1B H 0.5151 0.6091 0.7513 0.034 Uiso 1 1 calc R . . H1C H 0.5480 0.7517 0.7086 0.034 Uiso 1 1 calc R . . C2 C 0.3691(2) 0.7758(5) 0.6310(3) 0.0243(8) Uani 1 1 d . . . H2A H 0.3188 0.7788 0.5814 0.036 Uiso 1 1 calc R . . H2B H 0.3923 0.8818 0.6414 0.036 Uiso 1 1 calc R . . H2C H 0.3594 0.7391 0.6841 0.036 Uiso 1 1 calc R . . C3 C 0.3995(2) 0.4458(4) 0.6067(2) 0.0166(7) Uani 1 1 d . . . H3A H 0.3890 0.4324 0.6628 0.020 Uiso 1 1 calc R . . H3B H 0.4431 0.3724 0.6087 0.020 Uiso 1 1 calc R . . C4 C 0.3375(3) 0.3689(5) 0.4214(3) 0.0261(9) Uani 1 1 d . . . H4A H 0.3449 0.4756 0.4019 0.039 Uiso 1 1 calc R . . H4B H 0.2948 0.3158 0.3748 0.039 Uiso 1 1 calc R . . H4C H 0.3870 0.3090 0.4338 0.039 Uiso 1 1 calc R . . C5 C 0.2995(2) 0.1825(5) 0.5500(3) 0.0230(8) Uani 1 1 d . . . H5A H 0.2853 0.1835 0.6036 0.035 Uiso 1 1 calc R . . H5B H 0.3492 0.1241 0.5611 0.035 Uiso 1 1 calc R . . H5C H 0.2570 0.1312 0.5022 0.035 Uiso 1 1 calc R . . C6 C -0.0284(2) 0.9213(5) 0.3753(3) 0.0238(9) Uani 1 1 d . . . H6A H -0.0663 0.9120 0.3151 0.036 Uiso 1 1 calc R . . H6B H -0.0190 1.0331 0.3910 0.036 Uiso 1 1 calc R . . H6C H -0.0500 0.8691 0.4164 0.036 Uiso 1 1 calc R . . C7 C 0.1308(2) 0.8491(5) 0.4922(2) 0.0217(8) Uani 1 1 d . . . H7A H 0.1816 0.7995 0.4971 0.033 Uiso 1 1 calc R . . H7B H 0.1083 0.7972 0.5327 0.033 Uiso 1 1 calc R . . H7C H 0.1393 0.9612 0.5074 0.033 Uiso 1 1 calc R . . C8 C 0.0990(2) 0.9517(5) 0.3116(2) 0.0196(8) Uani 1 1 d . . . H8A H 0.0566 0.9566 0.2531 0.024 Uiso 1 1 calc R . . H8B H 0.1055 1.0599 0.3363 0.024 Uiso 1 1 calc R . . C9 C 0.1789(2) 0.7079(5) 0.2465(3) 0.0282(9) Uani 1 1 d . . . H9A H 0.1763 0.6296 0.2902 0.042 Uiso 1 1 calc R . . H9B H 0.2244 0.6850 0.2278 0.042 Uiso 1 1 calc R . . H9C H 0.1298 0.7035 0.1952 0.042 Uiso 1 1 calc R . . C10 C 0.1940(3) 1.0377(6) 0.2116(3) 0.0340(11) Uani 1 1 d . . . H10A H 0.2000 1.1449 0.2360 0.051 Uiso 1 1 calc R . . H10B H 0.1448 1.0312 0.1606 0.051 Uiso 1 1 calc R . . H10C H 0.2394 1.0126 0.1931 0.051 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 Sb1 0.01473(13) 0.01611(13) 0.01414(12) -0.00163(9) 0.00455(9) -0.00105(9) Sb2 0.01523(13) 0.01553(13) 0.01682(12) 0.00110(9) 0.00528(9) 0.00026(9) F1 0.0274(12) 0.0189(11) 0.0160(10) -0.0030(9) 0.0061(9) -0.0012(9) F2 0.0163(11) 0.0318(14) 0.0324(13) -0.0002(10) 0.0102(10) -0.0003(10) F3 0.0283(12) 0.0252(12) 0.0212(11) 0.0069(9) 0.0094(9) -0.0024(10) F4 0.0321(13) 0.0265(13) 0.0239(12) -0.0060(10) 0.0119(10) 0.0010(10) F5 0.0280(13) 0.0175(12) 0.0444(14) 0.0109(11) 0.0135(11) 0.0004(10) F6 0.0178(12) 0.0353(15) 0.0349(13) 0.0048(11) 0.0013(10) -0.0079(11) P1 0.0174(5) 0.0152(5) 0.0137(4) 0.0004(4) 0.0034(4) -0.0004(4) P2 0.0151(5) 0.0148(5) 0.0181(5) -0.0014(4) 0.0053(4) -0.0012(4) P3 0.0152(5) 0.0161(5) 0.0184(4) 0.0017(4) 0.0058(4) 0.0010(4) P4 0.0156(5) 0.0262(5) 0.0159(4) -0.0011(4) 0.0053(4) -0.0041(4) O1 0.0296(15) 0.0205(14) 0.0167(13) 0.0022(11) 0.0100(11) 0.0013(12) O2 0.0186(14) 0.0192(14) 0.0269(14) -0.0009(11) 0.0059(11) 0.0009(11) O3 0.0250(14) 0.0160(14) 0.0194(13) -0.0003(11) 0.0023(11) -0.0013(11) O4 0.0167(13) 0.0259(15) 0.0171(13) -0.0018(11) 0.0056(10) -0.0028(11) C1 0.024(2) 0.025(2) 0.0175(18) 0.0017(16) 0.0049(15) -0.0059(17) C2 0.029(2) 0.023(2) 0.0224(19) 0.0019(16) 0.0096(16) 0.0069(17) C3 0.0169(18) 0.0140(18) 0.0181(18) 0.0007(14) 0.0048(14) -0.0008(14) C4 0.030(2) 0.030(2) 0.0201(19) -0.0064(17) 0.0114(17) -0.0028(18) C5 0.0185(19) 0.018(2) 0.032(2) -0.0002(16) 0.0074(16) -0.0031(16) C6 0.018(2) 0.027(2) 0.030(2) 0.0029(17) 0.0133(17) 0.0032(17) C7 0.022(2) 0.022(2) 0.0203(18) 0.0005(16) 0.0060(15) -0.0031(16) C8 0.0186(19) 0.021(2) 0.0185(18) 0.0034(15) 0.0055(15) 0.0050(16) C9 0.022(2) 0.036(2) 0.027(2) -0.0121(18) 0.0077(17) -0.0023(18) C10 0.022(2) 0.055(3) 0.021(2) 0.012(2) 0.0032(17) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F1 1.914(2) . ? Sb1 F2 1.970(2) . ? Sb1 F3 1.972(2) . ? Sb1 O4 2.416(3) . ? Sb1 O1 2.446(3) . ? Sb2 F4 1.909(2) . ? Sb2 F5 1.964(2) . ? Sb2 F6 1.971(2) . ? Sb2 O3 2.411(3) . ? Sb2 O2 2.455(3) . ? P1 O1 1.508(3) . ? P1 C1 1.787(4) . ? P1 C2 1.789(4) . ? P1 C3 1.803(4) . ? P2 O2 1.509(3) . ? P2 C4 1.783(4) . ? P2 C5 1.788(4) . ? P2 C3 1.804(4) . ? P3 O3 1.508(3) . ? P3 C6 1.788(4) . ? P3 C7 1.790(4) . ? P3 C8 1.798(4) . ? P4 O4 1.507(3) . ? P4 C9 1.780(4) . ? P4 C10 1.791(4) . ? P4 C8 1.795(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 F1 Sb1 F2 87.46(10) . . ? F1 Sb1 F3 85.83(9) . . ? F2 Sb1 F3 84.53(9) . . ? F1 Sb1 O4 82.24(9) . . ? F2 Sb1 O4 165.14(9) . . ? F3 Sb1 O4 84.07(9) . . ? F1 Sb1 O1 77.90(9) . . ? F2 Sb1 O1 82.26(9) . . ? F3 Sb1 O1 159.42(9) . . ? O4 Sb1 O1 105.83(9) . . ? F4 Sb2 F5 85.71(10) . . ? F4 Sb2 F6 88.72(10) . . ? F5 Sb2 F6 85.04(10) . . ? F4 Sb2 O3 78.81(10) . . ? F5 Sb2 O3 161.46(10) . . ? F6 Sb2 O3 84.47(10) . . ? F4 Sb2 O2 81.61(9) . . ? F5 Sb2 O2 87.05(9) . . ? F6 Sb2 O2 167.94(10) . . ? O3 Sb2 O2 100.59(9) . . ? O1 P1 C1 113.25(17) . . ? O1 P1 C2 112.25(17) . . ? C1 P1 C2 106.81(19) . . ? O1 P1 C3 113.22(16) . . ? C1 P1 C3 102.97(18) . . ? C2 P1 C3 107.69(19) . . ? O2 P2 C4 113.44(18) . . ? O2 P2 C5 113.27(17) . . ? C4 P2 C5 106.8(2) . . ? O2 P2 C3 112.45(17) . . ? C4 P2 C3 107.10(19) . . ? C5 P2 C3 103.00(18) . . ? O3 P3 C6 112.96(18) . . ? O3 P3 C7 111.29(17) . . ? C6 P3 C7 108.04(19) . . ? O3 P3 C8 112.86(17) . . ? C6 P3 C8 103.27(18) . . ? C7 P3 C8 107.96(18) . . ? O4 P4 C9 112.46(18) . . ? O4 P4 C10 113.41(18) . . ? C9 P4 C10 107.6(2) . . ? O4 P4 C8 111.15(16) . . ? C9 P4 C8 108.67(19) . . ? C10 P4 C8 103.1(2) . . ? P1 O1 Sb1 134.62(16) . . ? P2 O2 Sb2 133.34(16) . . ? P3 O3 Sb2 124.38(14) . . ? P4 O4 Sb1 133.51(14) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 P2 120.0(2) . . ? P1 C3 H3A 107.3 . . ? P2 C3 H3A 107.3 . . ? P1 C3 H3B 107.3 . . ? P2 C3 H3B 107.3 . . ? H3A C3 H3B 106.9 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P3 C6 H6A 109.5 . . ? P3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P4 C8 P3 119.4(2) . . ? P4 C8 H8A 107.5 . . ? P3 C8 H8A 107.5 . . ? P4 C8 H8B 107.5 . . ? P3 C8 H8B 107.5 . . ? H8A C8 H8B 107.0 . . ? P4 C9 H9A 109.5 . . ? P4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 Sb1 O1 P1 C3 125.0(2) . . . . ? O1 P1 C3 P2 -52.6(3) . . . . ? P1 C3 P2 O2 -57.1(3) . . . . ? C3 P2 O2 Sb2 -153.54(19) . . . . ? Sb2 O3 P3 C8 135.09(18) . . . . ? O3 P3 C8 P4 -55.4(3) . . . . ? P3 C8 P4 O4 -65.0(3) . . . . ? C8 P4 O4 Sb1 -170.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.636 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.139 #===END OF CIF ============================================================== # 10sm527b data_10sm527b _database_code_depnum_ccdc_archive 'CCDC 803405' #TrackingRef '- MF3_all6_1.txt' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-07-13 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Trifluoro(ethane-1,2-diylbis(diphenylphosphine) dioxide)antimony(III) ; # Ph2P(O)CH2CH2P(O)Ph2 = C26H24O2P2 = dppeO2 # ethane-1,2-diylbis(diphenylphosphine) dioxide (iLab defaults) # ethane-1,2-diylbis(diphenylphosphane) dioxide (iLab selected options) _chemical_name_common ;Trifluoro(ethane-1,2-diylbis(diphenylphosphine) dioxide)antimony(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 F3 O2 P2 Sb' _chemical_formula_sum 'C26 H24 F3 O2 P2 Sb' _chemical_formula_weight 609.14 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7891(15) _cell_length_b 11.664(2) _cell_length_c 12.503(2) _cell_angle_alpha 65.839(10) _cell_angle_beta 77.987(10) _cell_angle_gamma 80.634(10) _cell_volume 1269.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5589 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9439 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21763 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.57 _reflns_number_total 5825 _reflns_number_gt 4697 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^)+(0.0000P)^2^+6.5050P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5825 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.72125(4) 0.82917(3) 0.32369(3) 0.01739(11) Uani 1 1 d . . . F1 F 0.9151(3) 0.7826(3) 0.2845(3) 0.0220(7) Uani 1 1 d . . . F2 F 0.7731(3) 1.0046(3) 0.2597(3) 0.0247(7) Uani 1 1 d . . . F3 F 0.7640(4) 0.8129(3) 0.4753(3) 0.0289(7) Uani 1 1 d . . . P1 P 0.85445(13) 0.86803(12) 0.01053(11) 0.0157(3) Uani 1 1 d . . . P2 P 0.77170(13) 0.49001(12) 0.51589(11) 0.0152(3) Uani 1 1 d . . . O1 O 0.7414(4) 0.8682(3) 0.1128(3) 0.0202(8) Uani 1 1 d . . . O2 O 0.7256(4) 0.6048(3) 0.4142(3) 0.0222(8) Uani 1 1 d . . . C1 C 0.9593(5) 0.9999(5) -0.0461(5) 0.0193(11) Uani 1 1 d . . . H1A H 1.0265 0.9974 -0.1164 0.023 Uiso 1 1 calc R . . H1B H 0.8976 1.0792 -0.0721 0.023 Uiso 1 1 calc R . . C2 C 0.7736(5) 0.8751(4) -0.1098(4) 0.0154(10) Uani 1 1 d . . . C3 C 0.6291(6) 0.9047(5) -0.1039(5) 0.0233(12) Uani 1 1 d . . . H3 H 0.5768 0.9270 -0.0411 0.028 Uiso 1 1 calc R . . C4 C 0.5609(7) 0.9015(6) -0.1907(5) 0.0327(14) Uani 1 1 d . . . H4 H 0.4620 0.9184 -0.1852 0.039 Uiso 1 1 calc R . . C5 C 0.6375(7) 0.8741(6) -0.2832(5) 0.0327(14) Uani 1 1 d . . . H5 H 0.5916 0.8745 -0.3433 0.039 Uiso 1 1 calc R . . C6 C 0.7809(7) 0.8456(5) -0.2904(5) 0.0284(13) Uani 1 1 d . . . H6 H 0.8325 0.8248 -0.3543 0.034 Uiso 1 1 calc R . . C7 C 0.8502(6) 0.8472(5) -0.2048(5) 0.0265(12) Uani 1 1 d . . . H7 H 0.9491 0.8294 -0.2108 0.032 Uiso 1 1 calc R . . C8 C 0.9713(5) 0.7263(5) 0.0454(4) 0.0172(10) Uani 1 1 d . . . C9 C 1.1059(6) 0.7254(5) -0.0197(5) 0.0235(12) Uani 1 1 d . . . H9 H 1.1391 0.8011 -0.0803 0.028 Uiso 1 1 calc R . . C10 C 1.1906(6) 0.6126(6) 0.0052(5) 0.0310(13) Uani 1 1 d . . . H10 H 1.2831 0.6115 -0.0371 0.037 Uiso 1 1 calc R . . C11 C 1.1404(6) 0.5017(5) 0.0914(5) 0.0269(13) Uani 1 1 d . . . H11 H 1.1980 0.4246 0.1071 0.032 Uiso 1 1 calc R . . C12 C 1.0075(6) 0.5033(5) 0.1543(5) 0.0238(12) Uani 1 1 d . . . H12 H 0.9737 0.4271 0.2135 0.029 Uiso 1 1 calc R . . C13 C 0.9230(6) 0.6143(5) 0.1322(4) 0.0202(11) Uani 1 1 d . . . H13 H 0.8314 0.6146 0.1764 0.024 Uiso 1 1 calc R . . C14 C 0.9396(5) 0.4978(5) 0.5501(4) 0.0180(11) Uani 1 1 d . . . H14A H 0.9355 0.5738 0.5676 0.022 Uiso 1 1 calc R . . H14B H 0.9580 0.4231 0.6224 0.022 Uiso 1 1 calc R . . C15 C 0.7855(5) 0.3510(5) 0.4846(4) 0.0165(10) Uani 1 1 d . . . C16 C 0.7125(6) 0.3539(5) 0.3991(5) 0.0222(11) Uani 1 1 d . . . H16 H 0.6569 0.4280 0.3586 0.027 Uiso 1 1 calc R . . C17 C 0.7218(7) 0.2474(6) 0.3735(5) 0.0315(14) Uani 1 1 d . . . H17 H 0.6716 0.2486 0.3156 0.038 Uiso 1 1 calc R . . C18 C 0.8033(6) 0.1398(6) 0.4315(5) 0.0304(13) Uani 1 1 d . . . H18 H 0.8085 0.0671 0.4141 0.036 Uiso 1 1 calc R . . C19 C 0.8776(6) 0.1383(5) 0.5152(5) 0.0288(13) Uani 1 1 d . . . H19 H 0.9353 0.0651 0.5541 0.035 Uiso 1 1 calc R . . C20 C 0.8677(6) 0.2432(5) 0.5419(5) 0.0218(11) Uani 1 1 d . . . H20 H 0.9177 0.2415 0.6001 0.026 Uiso 1 1 calc R . . C21 C 0.6525(5) 0.4654(5) 0.6530(5) 0.0187(11) Uani 1 1 d . . . C22 C 0.5851(6) 0.3553(5) 0.7143(5) 0.0257(12) Uani 1 1 d . . . H22 H 0.6000 0.2916 0.6832 0.031 Uiso 1 1 calc R . . C23 C 0.4963(6) 0.3382(5) 0.8205(5) 0.0281(13) Uani 1 1 d . . . H23 H 0.4494 0.2633 0.8618 0.034 Uiso 1 1 calc R . . C24 C 0.4759(6) 0.4305(6) 0.8665(5) 0.0289(13) Uani 1 1 d . . . H24 H 0.4165 0.4181 0.9401 0.035 Uiso 1 1 calc R . . C25 C 0.5419(6) 0.5408(5) 0.8054(5) 0.0238(12) Uani 1 1 d . . . H25 H 0.5267 0.6045 0.8365 0.029 Uiso 1 1 calc R . . C26 C 0.6303(6) 0.5583(5) 0.6985(5) 0.0241(12) Uani 1 1 d . . . H26 H 0.6755 0.6340 0.6565 0.029 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 Sb1 0.02002(18) 0.01787(18) 0.01458(17) -0.00658(13) -0.00251(13) -0.00200(13) F1 0.0183(15) 0.0234(16) 0.0218(15) -0.0056(13) -0.0046(12) -0.0019(13) F2 0.0325(18) 0.0207(16) 0.0221(16) -0.0079(13) -0.0037(14) -0.0077(14) F3 0.044(2) 0.0314(18) 0.0169(15) -0.0125(14) -0.0062(14) -0.0074(15) P1 0.0168(6) 0.0160(6) 0.0152(6) -0.0066(5) -0.0014(5) -0.0041(5) P2 0.0150(6) 0.0146(6) 0.0160(6) -0.0058(5) -0.0017(5) -0.0027(5) O1 0.0196(18) 0.024(2) 0.0184(18) -0.0093(16) -0.0022(15) -0.0029(15) O2 0.026(2) 0.0159(18) 0.0230(19) -0.0054(16) -0.0057(16) -0.0013(15) C1 0.018(3) 0.018(3) 0.022(3) -0.008(2) -0.001(2) -0.004(2) C2 0.019(2) 0.012(2) 0.014(2) -0.0009(19) -0.004(2) -0.005(2) C3 0.024(3) 0.024(3) 0.019(3) -0.005(2) -0.003(2) -0.004(2) C4 0.032(3) 0.033(3) 0.031(3) -0.004(3) -0.016(3) -0.007(3) C5 0.043(4) 0.032(3) 0.028(3) -0.008(3) -0.018(3) -0.010(3) C6 0.041(4) 0.025(3) 0.019(3) -0.008(2) -0.005(3) -0.004(3) C7 0.025(3) 0.031(3) 0.024(3) -0.009(3) -0.003(2) -0.007(2) C8 0.018(2) 0.017(3) 0.018(2) -0.007(2) -0.004(2) -0.003(2) C9 0.027(3) 0.018(3) 0.027(3) -0.010(2) -0.004(2) -0.004(2) C10 0.025(3) 0.032(3) 0.037(3) -0.016(3) 0.001(3) -0.001(3) C11 0.029(3) 0.023(3) 0.031(3) -0.011(3) -0.010(3) 0.002(2) C12 0.033(3) 0.014(3) 0.022(3) -0.004(2) -0.006(2) -0.002(2) C13 0.023(3) 0.021(3) 0.017(2) -0.007(2) -0.002(2) -0.007(2) C14 0.016(2) 0.024(3) 0.019(3) -0.013(2) -0.003(2) -0.001(2) C15 0.021(3) 0.013(2) 0.017(2) -0.006(2) 0.000(2) -0.006(2) C16 0.021(3) 0.021(3) 0.025(3) -0.008(2) -0.003(2) -0.005(2) C17 0.042(4) 0.030(3) 0.035(3) -0.019(3) -0.017(3) -0.004(3) C18 0.036(3) 0.024(3) 0.036(3) -0.016(3) -0.009(3) -0.003(3) C19 0.029(3) 0.023(3) 0.037(3) -0.013(3) -0.008(3) -0.003(2) C20 0.022(3) 0.021(3) 0.025(3) -0.012(2) -0.008(2) 0.002(2) C21 0.013(2) 0.022(3) 0.020(3) -0.006(2) -0.004(2) -0.003(2) C22 0.023(3) 0.025(3) 0.028(3) -0.010(3) 0.000(2) -0.005(2) C23 0.025(3) 0.024(3) 0.028(3) -0.004(2) 0.003(2) -0.008(2) C24 0.023(3) 0.042(4) 0.017(3) -0.011(3) 0.004(2) -0.002(3) C25 0.022(3) 0.032(3) 0.018(3) -0.011(2) 0.000(2) -0.003(2) C26 0.021(3) 0.027(3) 0.022(3) -0.008(2) -0.003(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F1 1.906(3) . ? Sb1 F3 1.952(3) . ? Sb1 F2 1.979(3) . ? Sb1 O2 2.385(4) . ? Sb1 O1 2.456(3) . ? P1 O1 1.507(4) . ? P1 C8 1.798(5) . ? P1 C1 1.800(5) . ? P1 C2 1.808(5) . ? P2 O2 1.504(4) . ? P2 C15 1.797(5) . ? P2 C21 1.805(5) . ? P2 C14 1.807(5) . ? C1 C1 1.533(10) 2_775 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.394(7) . ? C2 C7 1.395(7) . ? C3 C4 1.402(8) . ? C3 H3 0.9500 . ? C4 C5 1.366(9) . ? C4 H4 0.9500 . ? C5 C6 1.382(9) . ? C5 H5 0.9500 . ? C6 C7 1.389(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.391(7) . ? C8 C9 1.398(7) . ? C9 C10 1.391(8) . ? C9 H9 0.9500 . ? C10 C11 1.386(8) . ? C10 H10 0.9500 . ? C11 C12 1.375(8) . ? C11 H11 0.9500 . ? C12 C13 1.376(7) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C14 1.525(9) 2_766 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.384(7) . ? C15 C16 1.390(7) . ? C16 C17 1.389(8) . ? C16 H16 0.9500 . ? C17 C18 1.381(8) . ? C17 H17 0.9500 . ? C18 C19 1.387(8) . ? C18 H18 0.9500 . ? C19 C20 1.378(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.386(7) . ? C21 C22 1.389(8) . ? C22 C23 1.386(8) . ? C22 H22 0.9500 . ? C23 C24 1.385(8) . ? C23 H23 0.9500 . ? C24 C25 1.384(8) . ? C24 H24 0.9500 . ? C25 C26 1.389(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Sb1 F3 87.00(13) . . ? F1 Sb1 F2 86.50(13) . . ? F3 Sb1 F2 86.84(13) . . ? F1 Sb1 O2 79.19(13) . . ? F3 Sb1 O2 84.12(13) . . ? F2 Sb1 O2 163.43(13) . . ? F1 Sb1 O1 77.97(12) . . ? F3 Sb1 O1 162.42(13) . . ? F2 Sb1 O1 83.22(12) . . ? O2 Sb1 O1 101.71(12) . . ? O1 P1 C8 113.4(2) . . ? O1 P1 C1 113.4(2) . . ? C8 P1 C1 107.8(2) . . ? O1 P1 C2 108.9(2) . . ? C8 P1 C2 105.4(2) . . ? C1 P1 C2 107.5(2) . . ? O2 P2 C15 110.7(2) . . ? O2 P2 C21 112.4(2) . . ? C15 P2 C21 108.2(2) . . ? O2 P2 C14 113.9(2) . . ? C15 P2 C14 106.9(2) . . ? C21 P2 C14 104.3(2) . . ? P1 O1 Sb1 138.5(2) . . ? P2 O2 Sb1 143.9(2) . . ? C1 C1 P1 112.5(5) 2_775 . ? C1 C1 H1A 109.1 2_775 . ? P1 C1 H1A 109.1 . . ? C1 C1 H1B 109.1 2_775 . ? P1 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C7 119.6(5) . . ? C3 C2 P1 118.3(4) . . ? C7 C2 P1 122.1(4) . . ? C2 C3 C4 120.0(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.7(6) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 120.4(5) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 119.5(5) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? C13 C8 C9 119.7(5) . . ? C13 C8 P1 119.3(4) . . ? C9 C8 P1 120.8(4) . . ? C10 C9 C8 119.3(5) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 120.2(5) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.1(5) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.5(5) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 120.1(5) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C14 C14 P2 113.2(4) 2_766 . ? C14 C14 H14A 108.9 2_766 . ? P2 C14 H14A 108.9 . . ? C14 C14 H14B 108.9 2_766 . ? P2 C14 H14B 108.9 . . ? H14A C14 H14B 107.8 . . ? C20 C15 C16 119.9(5) . . ? C20 C15 P2 121.7(4) . . ? C16 C15 P2 118.4(4) . . ? C17 C16 C15 119.3(5) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 120.6(5) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.8(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.9(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 120.5(5) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? C26 C21 C22 119.7(5) . . ? C26 C21 P2 118.7(4) . . ? C22 C21 P2 121.6(4) . . ? C23 C22 C21 120.2(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.2(5) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.9(5) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.1(5) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? 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 Sb1 O1 P1 C1 -72.6(4) . . . . ? O1 P1 C1 C1 62.9(5) . . . 2_775 ? Sb1 O2 P2 C14 -38.6(4) . . . . ? O2 P2 C14 C14 -64.2(6) . . . 2_766 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.778 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.171 #===END OF CIF ============================================================== # 10sm708b data_10sm708b _database_code_depnum_ccdc_archive 'CCDC 803406' #TrackingRef '- MF3_all6_1.txt' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-07-22 _audit_author_name 'Zhang, Wenjian' _chemical_name_systematic ; trifluorobis(trimethylarsine oxide)antimony(III) ; _chemical_name_common 'trifluorobis(trimethylarsine oxide)antimony(iii)' _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 As2 F3 O2 Sb' _chemical_formula_sum 'C6 H18 As2 F3 O2 Sb' _chemical_formula_structural '(F3 Sb) (C3 H9 As O)2' _chemical_formula_weight 450.79 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1563(10) _cell_length_b 13.546(2) _cell_length_c 12.4707(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.531(10) _cell_angle_gamma 90.00 _cell_volume 1366.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19553 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 6.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6064 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17429 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3124 _reflns_number_gt 2753 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^)+(0.0187P)^2^+5.1953P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3124 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.40822(3) 0.061802(19) 0.188428(19) 0.01675(8) Uani 1 1 d . . . As1 As -0.01892(5) 0.01583(3) 0.20360(3) 0.02060(11) Uani 1 1 d . . . As2 As 0.52752(5) 0.15937(3) 0.45697(3) 0.01797(10) Uani 1 1 d . . . F1 F 0.2747(3) 0.16619(17) 0.23962(18) 0.0222(5) Uani 1 1 d . . . F2 F 0.2937(3) 0.1010(2) 0.04281(18) 0.0288(6) Uani 1 1 d . . . F3 F 0.5641(3) 0.17270(19) 0.16651(19) 0.0268(5) Uani 1 1 d . . . O1 O 0.1771(3) -0.0228(2) 0.2049(2) 0.0231(6) Uani 1 1 d . . . O2 O 0.5227(3) 0.0673(2) 0.3649(2) 0.0218(6) Uani 1 1 d . . . C1 C -0.0507(6) 0.0894(4) 0.3301(4) 0.0378(12) Uani 1 1 d . . . H1A H -0.0048 0.0524 0.3946 0.057 Uiso 1 1 calc R . . H1B H -0.1692 0.1002 0.3314 0.057 Uiso 1 1 calc R . . H1C H 0.0056 0.1532 0.3289 0.057 Uiso 1 1 calc R . . C2 C -0.1536(5) -0.0998(4) 0.2031(4) 0.0327(10) Uani 1 1 d . . . H2A H -0.1602 -0.1322 0.1324 0.049 Uiso 1 1 calc R . . H2B H -0.2649 -0.0811 0.2172 0.049 Uiso 1 1 calc R . . H2C H -0.1047 -0.1453 0.2595 0.049 Uiso 1 1 calc R . . C3 C -0.0926(5) 0.0974(3) 0.0823(3) 0.0271(9) Uani 1 1 d . . . H3A H -0.0037 0.1426 0.0690 0.041 Uiso 1 1 calc R . . H3B H -0.1892 0.1355 0.0972 0.041 Uiso 1 1 calc R . . H3C H -0.1229 0.0559 0.0184 0.041 Uiso 1 1 calc R . . C4 C 0.5555(5) 0.2857(3) 0.3942(3) 0.0220(8) Uani 1 1 d . . . H4A H 0.6705 0.2933 0.3807 0.033 Uiso 1 1 calc R . . H4B H 0.5286 0.3374 0.4440 0.033 Uiso 1 1 calc R . . H4C H 0.4818 0.2912 0.3258 0.033 Uiso 1 1 calc R . . C5 C 0.7101(5) 0.1356(3) 0.5662(3) 0.0234(8) Uani 1 1 d . . . H5A H 0.7022 0.0686 0.5948 0.035 Uiso 1 1 calc R . . H5B H 0.7081 0.1835 0.6249 0.035 Uiso 1 1 calc R . . H5C H 0.8137 0.1424 0.5350 0.035 Uiso 1 1 calc R . . C6 C 0.3313(5) 0.1576(3) 0.5245(3) 0.0246(9) Uani 1 1 d . . . H6A H 0.2355 0.1704 0.4702 0.037 Uiso 1 1 calc R . . H6B H 0.3382 0.2087 0.5805 0.037 Uiso 1 1 calc R . . H6C H 0.3193 0.0928 0.5575 0.037 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 Sb1 0.01499(13) 0.02034(15) 0.01489(13) -0.00157(9) 0.00188(9) -0.00040(9) As1 0.01555(19) 0.0301(2) 0.01582(19) -0.00055(16) 0.00070(14) -0.00179(16) As2 0.01951(19) 0.0181(2) 0.01569(19) 0.00053(15) 0.00004(14) -0.00011(15) F1 0.0185(11) 0.0220(12) 0.0261(12) -0.0030(9) 0.0026(9) 0.0026(9) F2 0.0311(13) 0.0386(15) 0.0156(11) 0.0037(10) -0.0016(9) -0.0064(11) F3 0.0247(12) 0.0304(14) 0.0262(12) -0.0009(10) 0.0070(9) -0.0080(10) O1 0.0161(13) 0.0272(16) 0.0257(15) 0.0018(12) 0.0016(11) -0.0001(11) O2 0.0234(14) 0.0222(15) 0.0187(14) -0.0009(11) -0.0016(11) 0.0010(11) C1 0.025(2) 0.063(4) 0.026(2) -0.014(2) 0.0043(17) 0.000(2) C2 0.023(2) 0.045(3) 0.030(2) 0.007(2) 0.0004(17) -0.010(2) C3 0.024(2) 0.027(2) 0.031(2) 0.0006(18) 0.0030(16) 0.0060(17) C4 0.028(2) 0.019(2) 0.0185(19) 0.0019(15) 0.0008(15) 0.0022(16) C5 0.026(2) 0.024(2) 0.0183(19) 0.0020(16) -0.0024(15) 0.0024(17) C6 0.0220(19) 0.025(2) 0.027(2) -0.0051(17) 0.0054(16) -0.0031(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 Sb1 F1 1.943(2) . ? Sb1 F2 2.002(2) . ? Sb1 F3 2.010(2) . ? Sb1 O1 2.238(3) . ? Sb1 O2 2.276(3) . ? As1 O1 1.680(3) . ? As1 C3 1.906(4) . ? As1 C1 1.911(4) . ? As1 C2 1.913(5) . ? As2 O2 1.692(3) . ? As2 C6 1.903(4) . ? As2 C4 1.908(4) . ? As2 C5 1.909(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 F1 Sb1 F2 83.69(10) . . ? F1 Sb1 F3 83.83(10) . . ? F2 Sb1 F3 84.63(10) . . ? F1 Sb1 O1 80.07(10) . . ? F2 Sb1 O1 85.46(10) . . ? F3 Sb1 O1 161.91(10) . . ? F1 Sb1 O2 80.50(10) . . ? F2 Sb1 O2 162.12(11) . . ? F3 Sb1 O2 85.42(10) . . ? O1 Sb1 O2 99.89(10) . . ? O1 As1 C3 112.89(16) . . ? O1 As1 C1 112.72(17) . . ? C3 As1 C1 106.9(2) . . ? O1 As1 C2 106.89(18) . . ? C3 As1 C2 110.54(19) . . ? C1 As1 C2 106.8(2) . . ? O2 As2 C6 110.16(16) . . ? O2 As2 C4 112.09(16) . . ? C6 As2 C4 110.20(18) . . ? O2 As2 C5 107.84(16) . . ? C6 As2 C5 107.74(18) . . ? C4 As2 C5 108.67(18) . . ? As1 O1 Sb1 130.64(16) . . ? As2 O2 Sb1 130.58(15) . . ? As1 C1 H1A 109.5 . . ? As1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? As1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? As1 C2 H2A 109.5 . . ? As1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? As1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? As1 C3 H3A 109.5 . . ? As1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? As1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? As2 C4 H4A 109.5 . . ? As2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? As2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? As2 C5 H5A 109.5 . . ? As2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? As2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? As2 C6 H6A 109.5 . . ? As2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? As2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 C3 As1 O1 Sb1 50.9(3) . . . . ? C1 As1 O1 Sb1 -70.3(3) . . . . ? C2 As1 O1 Sb1 172.6(2) . . . . ? F1 Sb1 O1 As1 23.64(19) . . . . ? F2 Sb1 O1 As1 -60.7(2) . . . . ? F3 Sb1 O1 As1 -3.8(5) . . . . ? O2 Sb1 O1 As1 102.1(2) . . . . ? C6 As2 O2 Sb1 85.2(2) . . . . ? C4 As2 O2 Sb1 -37.9(2) . . . . ? C5 As2 O2 Sb1 -157.4(2) . . . . ? F1 Sb1 O2 As2 -23.36(19) . . . . ? F2 Sb1 O2 As2 4.8(5) . . . . ? F3 Sb1 O2 As2 61.1(2) . . . . ? O1 Sb1 O2 As2 -101.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.599 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.147 #===END OF CIF ============================================================== # 10sm819a data_10sm819a _database_code_depnum_ccdc_archive 'CCDC 803407' #TrackingRef '- MF3_all6_1.txt' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-08-28 _audit_author_name 'Mareshwari, Seema' _chemical_name_systematic ; Trifluoro(methanediylbis(dimethylphosphane) dioxide)arsenic(III) ; # CH2{P(O)Me2}2 = Me2P(O)CH2P(O)Me2 = C5H14O2P2 # methylenebis(dimethylphosphine) dioxide (ACD iLab defaults) # [This looks odd to me ? Maybe phosphino ? mw] # methanediylbis(dimethylphosphane) dioxide (ACD iLab selected options) # methanediylbis(dimethylphosphane) dioxide (chemspider) _chemical_name_common ;Trifluoro(methanediylbis(dimethylphosphane) dioxide)arsenic(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C5 H14 As F3 O2 P2' _chemical_formula_sum 'C5 H14 As F3 O2 P2' _chemical_formula_weight 300.02 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7004(10) _cell_length_b 8.1617(15) _cell_length_c 9.7109(15) _cell_angle_alpha 76.455(2) _cell_angle_beta 78.429(2) _cell_angle_gamma 65.015(2) _cell_volume 534.22(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2404 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 3.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7498 # shelxl 0.6050 _exptl_absorpt_correction_T_max 1.0000 # 0.7216 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11357 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.63 _reflns_number_total 2446 _reflns_number_gt 2193 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' # _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^)+(0.0000P)^2^+0.8961P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2446 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.36259(4) 0.90658(3) 0.14921(3) 0.01549(8) Uani 1 1 d . . . P1 P 0.76002(9) 0.47881(8) 0.27712(6) 0.01394(13) Uani 1 1 d . . . P2 P 0.57725(9) 0.22479(8) 0.21744(7) 0.01560(14) Uani 1 1 d . . . F1 F 0.2446(2) 0.7587(2) 0.17659(16) 0.0247(3) Uani 1 1 d . . . F2 F 0.2548(2) 0.9834(2) 0.31216(16) 0.0279(4) Uani 1 1 d . . . F3 F 0.1726(2) 1.0824(2) 0.06064(17) 0.0287(4) Uani 1 1 d . . . O1 O 0.5815(2) 0.6378(2) 0.31763(18) 0.0175(4) Uani 1 1 d . . . O2 O 0.4928(3) 0.2122(2) 0.09546(18) 0.0214(4) Uani 1 1 d . . . C1 C 0.9513(4) 0.5452(3) 0.1813(3) 0.0205(5) Uani 1 1 d . . . H1A H 0.9070 0.6328 0.0949 0.031 Uiso 1 1 calc R . . H1B H 1.0623 0.4365 0.1551 0.031 Uiso 1 1 calc R . . H1C H 0.9891 0.6025 0.2418 0.031 Uiso 1 1 calc R . . C2 C 0.8587(4) 0.3154(3) 0.4294(3) 0.0186(5) Uani 1 1 d . . . H2A H 0.9098 0.3698 0.4831 0.028 Uiso 1 1 calc R . . H2B H 0.9628 0.2060 0.3978 0.028 Uiso 1 1 calc R . . H2C H 0.7573 0.2813 0.4907 0.028 Uiso 1 1 calc R . . C3 C 0.7183(3) 0.3641(3) 0.1560(2) 0.0154(5) Uani 1 1 d . . . H3A H 0.8463 0.2847 0.1142 0.018 Uiso 1 1 calc R . . H3B H 0.6558 0.4598 0.0770 0.018 Uiso 1 1 calc R . . C4 C 0.7378(4) 0.0056(3) 0.2982(3) 0.0239(6) Uani 1 1 d . . . H4A H 0.6708 -0.0780 0.3276 0.036 Uiso 1 1 calc R . . H4B H 0.7802 0.0194 0.3819 0.036 Uiso 1 1 calc R . . H4C H 0.8502 -0.0445 0.2294 0.036 Uiso 1 1 calc R . . C5 C 0.3946(4) 0.3224(4) 0.3547(3) 0.0192(5) Uani 1 1 d . . . H5A H 0.3185 0.4514 0.3190 0.029 Uiso 1 1 calc R . . H5B H 0.4549 0.3143 0.4371 0.029 Uiso 1 1 calc R . . H5C H 0.3100 0.2552 0.3832 0.029 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 As1 0.01606(14) 0.01247(13) 0.01707(13) -0.00193(9) -0.00090(9) -0.00554(10) P1 0.0153(3) 0.0125(3) 0.0144(3) -0.0025(2) -0.0026(2) -0.0053(2) P2 0.0184(3) 0.0142(3) 0.0161(3) -0.0044(2) -0.0019(2) -0.0074(3) F1 0.0230(8) 0.0236(8) 0.0317(9) 0.0027(7) -0.0071(7) -0.0154(7) F2 0.0332(9) 0.0214(8) 0.0222(8) -0.0079(6) 0.0090(7) -0.0073(7) F3 0.0213(8) 0.0205(8) 0.0365(9) 0.0048(7) -0.0088(7) -0.0034(6) O1 0.0183(9) 0.0139(8) 0.0182(8) -0.0037(7) -0.0038(7) -0.0032(7) O2 0.0265(10) 0.0247(10) 0.0185(9) -0.0084(7) -0.0020(8) -0.0130(8) C1 0.0232(14) 0.0197(13) 0.0211(13) -0.0026(10) -0.0017(11) -0.0113(11) C2 0.0194(13) 0.0174(12) 0.0182(12) -0.0027(10) -0.0049(10) -0.0056(10) C3 0.0173(12) 0.0139(12) 0.0149(11) -0.0028(9) -0.0015(9) -0.0062(10) C4 0.0264(14) 0.0150(12) 0.0307(14) -0.0009(11) -0.0068(12) -0.0085(11) C5 0.0199(13) 0.0219(13) 0.0183(12) -0.0054(10) 0.0000(10) -0.0107(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 As1 F1 1.7414(15) . ? As1 F2 1.7562(15) . ? As1 F3 1.7587(15) . ? As1 O1 2.5750(17) . ? As1 O2 2.6327(17) 2_665 ? As1 O2 2.9655(18) 1_565 ? P1 O1 1.4978(17) . ? P1 C2 1.793(2) . ? P1 C1 1.794(3) . ? P1 C3 1.812(2) . ? P2 O2 1.5029(17) . ? P2 C5 1.785(3) . ? P2 C4 1.791(3) . ? P2 C3 1.815(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? 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 F1 As1 F2 92.64(7) . . ? F1 As1 F3 90.48(7) . . ? F2 As1 F3 90.98(8) . . ? F1 As1 O1 80.68(6) . . ? F2 As1 O1 80.86(6) . . ? F3 As1 O1 167.62(7) . . ? F1 As1 O2 84.55(7) . 2_665 ? F2 As1 O2 176.81(7) . 2_665 ? F3 As1 O2 87.54(7) . 2_665 ? O1 As1 O2 100.13(6) . 2_665 ? F1 As1 O2 169.54(6) . 1_565 ? F2 As1 O2 83.93(6) . 1_565 ? F3 As1 O2 79.72(6) . 1_565 ? O1 As1 O2 108.41(5) . 1_565 ? O2 As1 O2 98.57(5) 2_665 1_565 ? O1 P1 C2 112.40(11) . . ? O1 P1 C1 113.11(11) . . ? C2 P1 C1 105.54(12) . . ? O1 P1 C3 111.92(11) . . ? C2 P1 C3 109.54(11) . . ? C1 P1 C3 103.81(11) . . ? O2 P2 C5 111.79(11) . . ? O2 P2 C4 112.51(12) . . ? C5 P2 C4 107.15(13) . . ? O2 P2 C3 110.54(11) . . ? C5 P2 C3 108.43(11) . . ? C4 P2 C3 106.16(12) . . ? P1 O1 As1 127.46(9) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 P2 121.04(13) . . ? P1 C3 H3A 107.1 . . ? P2 C3 H3A 107.1 . . ? P1 C3 H3B 107.1 . . ? P2 C3 H3B 107.1 . . ? H3A C3 H3B 106.8 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? 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 # F1 As1 O1 P1 91.99(13) . . . . ? # F2 As1 O1 P1 -173.79(13) . . . . ? # F3 As1 O1 P1 136.9(3) . . . . ? # O2 As1 O1 P1 9.29(13) 2_665 . . . ? # O2 As1 O1 P1 -93.37(12) 1_565 . . . ? C2 P1 O1 As1 -176.13(11) . . . . ? C1 P1 O1 As1 64.46(15) . . . . ? C3 P1 O1 As1 -52.37(15) . . . . ? O1 P1 C3 P2 -72.06(17) . . . . ? C2 P1 C3 P2 53.30(18) . . . . ? C1 P1 C3 P2 165.63(15) . . . . ? O2 P2 C3 P1 155.86(14) . . . . ? C5 P2 C3 P1 33.00(18) . . . . ? C4 P2 C3 P1 -81.85(17) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.492 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.091 #===END OF CIF ============================================================== # 2010sm715a data_2010sm715a _database_code_depnum_ccdc_archive 'CCDC 803408' #TrackingRef '- MF3_all6_1.txt' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-12-01 _audit_author_name 'Light M. E.' _chemical_name_systematic ; Trifluorobis(triphenylarsine oxide-O)antimony(III) ; # Ph3AsO = C18H16AsO # triphenylarsine oxide (ACD iLab defaults) # triphenylarsane oxide (ACD iLab selected options) _chemical_name_common 'Trifluorobis(triphenylarsine oxide-O)antimony(iii)' _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 As2 F3 O2 Sb' _chemical_formula_sum 'C36 H30 As2 F3 O2 Sb' _chemical_formula_structural '((C6 H5)3 As O)2 (F3 Sb)' _chemical_formula_weight 823.19 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.0551(3) _cell_length_b 32.8259(10) _cell_length_c 10.7878(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.5420(10) _cell_angle_gamma 90.00 _cell_volume 3185.43(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13677 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 2.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7550 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13457 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5159 _reflns_number_gt 4920 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0477P)^2^+27.4166P] 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 constr _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 0.077(15) _chemical_absolute_configuration ad _refine_ls_number_reflns 5159 _refine_ls_number_parameters 398 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 As1 As 0.00567(8) 0.93723(2) -0.11974(8) 0.02289(18) Uani 1 1 d . A . C1 C -0.1370(8) 0.9451(2) -0.0498(8) 0.0231(16) Uani 1 1 d . . . C2 C -0.2245(10) 0.9806(2) -0.0836(9) 0.0326(18) Uani 1 1 d . . . H2 H -0.2088 1.0019 -0.1354 0.039 Uiso 1 1 calc R . . C3 C -0.3340(10) 0.9838(3) -0.0395(10) 0.038(2) Uani 1 1 d . . . H3 H -0.3946 1.0075 -0.0620 0.046 Uiso 1 1 calc R . . C4 C -0.3567(11) 0.9529(3) 0.0373(10) 0.040(2) Uani 1 1 d . . . H4 H -0.4313 0.9556 0.0680 0.047 Uiso 1 1 calc R . . C5 C -0.2707(9) 0.9185(3) 0.0682(9) 0.0338(19) Uani 1 1 d . . . H5 H -0.2880 0.8972 0.1187 0.041 Uiso 1 1 calc R . . C6 C -0.1593(9) 0.9142(2) 0.0276(8) 0.0284(17) Uani 1 1 d . . . H6 H -0.0987 0.8905 0.0522 0.034 Uiso 1 1 calc R . . C7 C 0.1215(9) 0.9863(2) -0.0846(8) 0.0268(17) Uani 1 1 d . . . C8 C 0.0734(10) 1.0180(3) -0.1801(9) 0.0330(18) Uani 1 1 d . . . H8 H -0.0123 1.0151 -0.2665 0.040 Uiso 1 1 calc R . . C9 C 0.1540(10) 1.0535(2) -0.1451(9) 0.0340(19) Uani 1 1 d . . . H9 H 0.1234 1.0755 -0.2091 0.041 Uiso 1 1 calc R . . C10 C 0.2767(10) 1.0580(3) -0.0211(11) 0.039(2) Uani 1 1 d . . . H10 H 0.3292 1.0832 0.0001 0.047 Uiso 1 1 calc R . . C11 C 0.3257(10) 1.0268(3) 0.0739(11) 0.049(3) Uani 1 1 d . . . H11 H 0.4111 1.0303 0.1602 0.059 Uiso 1 1 calc R . . C12 C 0.2482(10) 0.9896(3) 0.0418(10) 0.040(2) Uani 1 1 d . . . H12 H 0.2812 0.9673 0.1046 0.048 Uiso 1 1 calc R . . C13 C -0.1089(8) 0.9278(2) -0.3137(8) 0.0229(16) Uani 1 1 d . . . C14 C -0.0417(9) 0.9263(2) -0.4006(9) 0.0313(18) Uani 1 1 d . . . H14 H 0.0591 0.9344 -0.3684 0.038 Uiso 1 1 calc R . . C15 C -0.1241(10) 0.9127(3) -0.5372(9) 0.0336(19) Uani 1 1 d . . . H15 H -0.0783 0.9107 -0.5973 0.040 Uiso 1 1 calc R . . C16 C -0.2690(10) 0.9024(3) -0.5835(9) 0.036(2) Uani 1 1 d . . . H16 H -0.3246 0.8939 -0.6769 0.043 Uiso 1 1 calc R . . C17 C -0.3373(10) 0.9041(3) -0.4974(9) 0.0322(19) Uani 1 1 d . . . H17 H -0.4386 0.8964 -0.5308 0.039 Uiso 1 1 calc R . . C18 C -0.2571(9) 0.9169(2) -0.3629(8) 0.0301(18) Uani 1 1 d . . . H18 H -0.3034 0.9184 -0.3032 0.036 Uiso 1 1 calc R . . As2 As 0.16078(7) 0.80419(2) 0.33361(7) 0.01853(17) Uani 1 1 d . A . C19 C 0.2681(8) 0.8240(2) 0.5186(7) 0.0211(15) Uani 1 1 d . . . C20 C 0.4237(9) 0.8274(2) 0.5790(8) 0.0241(16) Uani 1 1 d . . . H20 H 0.4775 0.8184 0.5307 0.029 Uiso 1 1 calc R . . C21 C 0.4979(9) 0.8441(2) 0.7117(8) 0.0257(16) Uani 1 1 d . . . H21 H 0.6033 0.8457 0.7554 0.031 Uiso 1 1 calc R . . C22 C 0.4182(10) 0.8584(3) 0.7805(9) 0.0334(19) Uani 1 1 d . . . H22 H 0.4693 0.8706 0.8693 0.040 Uiso 1 1 calc R . . C23 C 0.2656(9) 0.8550(2) 0.7201(8) 0.0284(17) Uani 1 1 d . . . H23 H 0.2125 0.8645 0.7684 0.034 Uiso 1 1 calc R . . C24 C 0.1879(9) 0.8377(2) 0.5886(9) 0.0281(17) Uani 1 1 d . . . H24 H 0.0827 0.8353 0.5474 0.034 Uiso 1 1 calc R . . C25 C -0.0348(8) 0.7887(2) 0.3087(8) 0.0237(16) Uani 1 1 d . . . C26 C -0.1528(8) 0.8138(2) 0.2346(8) 0.0274(17) Uani 1 1 d . . . H26 H -0.1374 0.8379 0.1941 0.033 Uiso 1 1 calc R . . C27 C -0.2919(9) 0.8047(3) 0.2183(9) 0.0340(19) Uani 1 1 d . . . H27 H -0.3726 0.8227 0.1688 0.041 Uiso 1 1 calc R . . C28 C -0.3148(9) 0.7683(3) 0.2759(9) 0.034(2) Uani 1 1 d . . . H28 H -0.4110 0.7614 0.2659 0.041 Uiso 1 1 calc R . . C29 C -0.1955(10) 0.7428(3) 0.3471(10) 0.037(2) Uani 1 1 d . . . H29 H -0.2111 0.7177 0.3826 0.044 Uiso 1 1 calc R . . C30 C -0.0547(9) 0.7529(2) 0.3675(9) 0.0306(18) Uani 1 1 d . . . H30 H 0.0274 0.7359 0.4207 0.037 Uiso 1 1 calc R . . C31 C 0.2551(8) 0.7567(2) 0.3076(8) 0.0203(15) Uani 1 1 d . . . C32 C 0.3394(8) 0.7315(2) 0.4202(8) 0.0238(16) Uani 1 1 d . . . H32 H 0.3523 0.7383 0.5105 0.029 Uiso 1 1 calc R . . C33 C 0.4036(8) 0.6966(2) 0.3995(9) 0.0313(19) Uani 1 1 d . . . H33 H 0.4601 0.6792 0.4755 0.038 Uiso 1 1 calc R . . C34 C 0.3859(9) 0.6867(2) 0.2678(9) 0.0266(17) Uani 1 1 d . . . H34 H 0.4320 0.6630 0.2541 0.032 Uiso 1 1 calc R . . C35 C 0.3017(10) 0.7112(2) 0.1573(8) 0.0273(17) Uani 1 1 d . . . H35 H 0.2879 0.7040 0.0671 0.033 Uiso 1 1 calc R . . C36 C 0.2365(8) 0.7464(2) 0.1759(8) 0.0242(16) Uani 1 1 d . . . H36 H 0.1794 0.7634 0.0990 0.029 Uiso 1 1 calc R . . O1 O 0.1081(6) 0.89590(17) -0.0500(6) 0.0319(13) Uani 1 1 d . . . O2 O 0.1339(6) 0.83998(15) 0.2131(5) 0.0242(11) Uani 1 1 d . . . Sb1A Sb 0.30332(16) 0.87360(6) 0.16122(16) 0.0186(2) Uani 0.3511(12) 1 d P A 1 F1A F 0.461(2) 0.8743(5) 0.083(2) 0.0262(10) Uani 0.3511(12) 1 d P A 1 F2A F 0.450(3) 0.8389(6) 0.305(3) 0.0262(10) Uani 0.3511(12) 1 d P A 1 F3A F 0.2612(13) 0.8290(4) 0.0343(13) 0.0262(10) Uani 0.3511(12) 1 d P A 1 Sb1B Sb 0.29558(8) 0.85540(3) 0.12058(7) 0.0186(2) Uani 0.6489(12) 1 d P A 2 F1B F 0.4605(12) 0.8850(2) 0.0987(11) 0.0262(10) Uani 0.6489(12) 1 d P A 2 F2B F 0.4446(15) 0.8303(3) 0.2920(14) 0.0262(10) Uani 0.6489(12) 1 d P A 2 F3B F 0.3155(7) 0.9033(2) 0.2260(7) 0.0262(10) Uani 0.6489(12) 1 d P A 2 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 As1 0.0234(4) 0.0214(4) 0.0216(4) 0.0009(3) 0.0081(3) -0.0028(3) C1 0.019(4) 0.023(4) 0.031(4) -0.006(3) 0.014(3) -0.005(3) C2 0.049(5) 0.026(4) 0.024(4) -0.003(3) 0.017(4) -0.002(4) C3 0.035(5) 0.034(5) 0.047(6) -0.013(4) 0.020(4) -0.001(4) C4 0.039(5) 0.044(5) 0.050(6) -0.014(4) 0.033(4) -0.006(4) C5 0.035(5) 0.039(5) 0.028(4) 0.004(4) 0.014(4) -0.003(4) C6 0.029(4) 0.027(4) 0.028(4) 0.004(3) 0.012(3) 0.000(3) C7 0.027(4) 0.022(4) 0.032(4) -0.001(3) 0.013(3) -0.009(3) C8 0.044(5) 0.028(4) 0.034(5) 0.005(3) 0.024(4) 0.005(4) C9 0.044(5) 0.026(4) 0.040(5) 0.006(4) 0.026(4) 0.002(4) C10 0.031(5) 0.031(5) 0.054(6) -0.003(4) 0.019(4) -0.016(4) C11 0.031(5) 0.041(5) 0.058(6) -0.002(5) 0.004(4) -0.004(4) C12 0.038(5) 0.027(5) 0.040(5) -0.003(4) 0.003(4) -0.004(4) C13 0.026(4) 0.020(4) 0.023(4) 0.000(3) 0.011(3) 0.000(3) C14 0.027(4) 0.028(4) 0.039(5) 0.003(4) 0.015(4) -0.003(3) C15 0.042(5) 0.033(4) 0.032(5) -0.006(4) 0.021(4) -0.001(4) C16 0.039(5) 0.041(5) 0.032(5) -0.001(4) 0.018(4) 0.000(4) C17 0.031(4) 0.027(4) 0.036(5) -0.006(4) 0.012(4) -0.005(3) C18 0.034(5) 0.027(4) 0.027(4) 0.000(3) 0.011(4) 0.002(3) As2 0.0194(4) 0.0174(3) 0.0159(3) 0.0014(3) 0.0052(3) 0.0008(3) C19 0.024(4) 0.018(4) 0.019(4) 0.000(3) 0.007(3) -0.006(3) C20 0.030(4) 0.020(4) 0.021(4) 0.007(3) 0.010(3) 0.002(3) C21 0.024(4) 0.021(4) 0.026(4) -0.002(3) 0.007(3) -0.002(3) C22 0.039(5) 0.037(5) 0.021(4) -0.006(3) 0.009(4) -0.008(4) C23 0.035(4) 0.029(4) 0.018(4) -0.006(3) 0.008(3) 0.004(3) C24 0.024(4) 0.026(4) 0.032(4) -0.006(3) 0.010(3) 0.000(3) C25 0.017(3) 0.027(4) 0.023(4) -0.008(3) 0.005(3) -0.001(3) C26 0.022(4) 0.036(5) 0.025(4) -0.003(3) 0.012(3) -0.008(3) C27 0.023(4) 0.045(5) 0.034(5) -0.002(4) 0.012(4) 0.002(3) C28 0.028(4) 0.038(5) 0.047(5) -0.014(4) 0.025(4) -0.013(4) C29 0.040(5) 0.030(4) 0.049(6) -0.003(4) 0.027(4) -0.007(4) C30 0.035(4) 0.025(4) 0.030(4) 0.001(3) 0.012(4) -0.005(3) C31 0.023(4) 0.011(3) 0.026(4) 0.003(3) 0.010(3) 0.005(3) C32 0.023(4) 0.020(4) 0.025(4) 0.000(3) 0.007(3) -0.001(3) C33 0.021(4) 0.025(4) 0.035(5) 0.011(3) 0.002(3) -0.001(3) C34 0.029(4) 0.017(4) 0.035(5) -0.004(3) 0.017(4) -0.002(3) C35 0.046(5) 0.017(4) 0.026(4) -0.003(3) 0.023(4) -0.001(3) C36 0.020(4) 0.028(4) 0.021(4) 0.003(3) 0.007(3) 0.000(3) O1 0.033(3) 0.025(3) 0.030(3) 0.005(2) 0.008(2) 0.001(2) O2 0.028(3) 0.022(3) 0.019(3) 0.008(2) 0.007(2) 0.001(2) Sb1A 0.0185(3) 0.0189(5) 0.0178(4) -0.0012(4) 0.0075(3) -0.0008(3) F1A 0.0258(15) 0.027(3) 0.026(2) 0.000(2) 0.0116(15) 0.000(2) F2A 0.0258(15) 0.027(3) 0.026(2) 0.000(2) 0.0116(15) 0.000(2) F3A 0.0258(15) 0.027(3) 0.026(2) 0.000(2) 0.0116(15) 0.000(2) Sb1B 0.0185(3) 0.0189(5) 0.0178(4) -0.0012(4) 0.0075(3) -0.0008(3) F1B 0.0258(15) 0.027(3) 0.026(2) 0.000(2) 0.0116(15) 0.000(2) F2B 0.0258(15) 0.027(3) 0.026(2) 0.000(2) 0.0116(15) 0.000(2) F3B 0.0258(15) 0.027(3) 0.026(2) 0.000(2) 0.0116(15) 0.000(2) _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 As1 O1 1.666(5) . ? As1 C13 1.909(8) . ? As1 C1 1.912(8) . ? As1 C7 1.923(7) . ? C1 C6 1.393(11) . ? C1 C2 1.407(11) . ? C2 C3 1.386(13) . ? C3 C4 1.392(14) . ? C4 C5 1.369(13) . ? C5 C6 1.380(12) . ? C7 C8 1.389(11) . ? C7 C12 1.394(12) . ? C8 C9 1.374(12) . ? C9 C10 1.364(14) . ? C10 C11 1.377(14) . ? C11 C12 1.405(13) . ? C13 C14 1.381(11) . ? C13 C18 1.386(11) . ? C14 C15 1.402(12) . ? C15 C16 1.355(13) . ? C16 C17 1.381(12) . ? C17 C18 1.374(12) . ? As2 O2 1.682(5) . ? As2 C31 1.909(7) . ? As2 C19 1.909(7) . ? As2 C25 1.930(8) . ? C19 C24 1.403(11) . ? C19 C20 1.405(11) . ? C20 C21 1.397(11) . ? C21 C22 1.395(12) . ? C22 C23 1.377(12) . ? C23 C24 1.398(11) . ? C25 C26 1.371(11) . ? C25 C30 1.391(11) . ? C26 C27 1.363(11) . ? C27 C28 1.414(13) . ? C28 C29 1.381(13) . ? C29 C30 1.373(12) . ? C31 C36 1.389(11) . ? C31 C32 1.400(10) . ? C32 C33 1.383(11) . ? C33 C34 1.388(12) . ? C34 C35 1.372(12) . ? C35 C36 1.386(11) . ? O1 Sb1A 2.363(6) . ? O1 Sb1B 2.368(5) . ? O2 Sb1A 2.300(5) . ? O2 Sb1B 2.313(5) . ? Sb1A F3A 1.918(13) . ? Sb1A F2A 1.96(3) . ? Sb1A F1A 2.10(2) . ? Sb1B F3B 1.898(7) . ? Sb1B F2B 1.967(14) . ? Sb1B F1B 2.025(11) . ? 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 # Sb1A O1 Sb1B 17.61(6) . . ? # Sb1A O2 Sb1B 18.07(6) . . ? O1 As1 C13 108.2(3) . . ? O1 As1 C1 110.6(3) . . ? C13 As1 C1 105.2(3) . . ? O1 As1 C7 113.3(3) . . ? C13 As1 C7 111.5(3) . . ? C1 As1 C7 107.7(3) . . ? C6 C1 C2 120.5(7) . . ? C6 C1 As1 119.3(6) . . ? C2 C1 As1 120.1(6) . . ? C3 C2 C1 118.3(8) . . ? C2 C3 C4 121.1(9) . . ? C5 C4 C3 119.4(8) . . ? C4 C5 C6 121.4(8) . . ? C5 C6 C1 119.2(7) . . ? C8 C7 C12 122.0(8) . . ? C8 C7 As1 120.1(6) . . ? C12 C7 As1 117.8(6) . . ? C9 C8 C7 117.7(8) . . ? C10 C9 C8 121.8(8) . . ? C9 C10 C11 121.0(8) . . ? C10 C11 C12 119.3(9) . . ? C7 C12 C11 118.2(8) . . ? C14 C13 C18 119.9(7) . . ? C14 C13 As1 120.8(6) . . ? C18 C13 As1 118.7(6) . . ? C13 C14 C15 119.1(8) . . ? C16 C15 C14 120.0(8) . . ? C15 C16 C17 121.2(8) . . ? C18 C17 C16 119.2(8) . . ? C17 C18 C13 120.5(8) . . ? O2 As2 C31 112.1(3) . . ? O2 As2 C19 113.0(3) . . ? C31 As2 C19 110.2(3) . . ? O2 As2 C25 105.9(3) . . ? C31 As2 C25 107.9(3) . . ? C19 As2 C25 107.5(3) . . ? C24 C19 C20 120.9(7) . . ? C24 C19 As2 118.7(6) . . ? C20 C19 As2 120.3(6) . . ? C21 C20 C19 118.7(7) . . ? C22 C21 C20 120.5(8) . . ? C23 C22 C21 120.3(7) . . ? C22 C23 C24 120.8(8) . . ? C23 C24 C19 118.8(7) . . ? C26 C25 C30 120.7(7) . . ? C26 C25 As2 119.0(6) . . ? C30 C25 As2 120.3(6) . . ? C27 C26 C25 121.0(8) . . ? C26 C27 C28 119.2(8) . . ? C29 C28 C27 119.0(8) . . ? C30 C29 C28 121.3(8) . . ? C29 C30 C25 118.7(8) . . ? C36 C31 C32 119.7(7) . . ? C36 C31 As2 120.0(5) . . ? C32 C31 As2 120.2(6) . . ? C33 C32 C31 119.7(7) . . ? C32 C33 C34 120.2(7) . . ? C35 C34 C33 120.0(7) . . ? C34 C35 C36 120.7(7) . . ? C35 C36 C31 119.6(7) . . ? As1 O1 Sb1A 140.1(3) . . ? As1 O1 Sb1B 157.7(3) . . ? As2 O2 Sb1A 130.0(3) . . ? As2 O2 Sb1B 125.8(3) . . ? F3A Sb1A F2A 88.2(7) . . ? F3A Sb1A F1A 71.8(6) . . ? F2A Sb1A F1A 83.5(10) . . ? F3A Sb1A O2 81.8(4) . . ? F2A Sb1A O2 84.7(8) . . ? F1A Sb1A O2 151.2(5) . . ? F3A Sb1A O1 74.0(4) . . ? F2A Sb1A O1 162.0(6) . . ? F1A Sb1A O1 93.4(6) . . ? O2 Sb1A O1 89.81(19) . . ? F3B Sb1B F2B 87.2(3) . . ? F3B Sb1B F1B 78.4(3) . . ? F2B Sb1B F1B 89.5(5) . . ? F3B Sb1B O2 80.1(2) . . ? F2B Sb1B O2 83.7(4) . . ? F1B Sb1B O2 157.8(3) . . ? F3B Sb1B O1 80.5(2) . . ? F2B Sb1B O1 166.8(3) . . ? F1B Sb1B O1 92.8(3) . . ? O2 Sb1B O1 89.37(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.823 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.109 #===END OF CIF ============================================================== # # 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 FILE =============================================================