# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 0182 _publ_requested_category SC _publ_contact_author_name 'S. Bruce Wild.' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6125 4236 ' _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_email sbw@rsc.anu.edu.au _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Self-Assembly of Square-Planar Halide Complexes of Phosphine-Stabilized Stibenium Salts ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address J.W.Wielandt ; Institut fuer Chemie Karl-Franzens-Univeritaet Graz Schubertstrasse 1, A-8010 Graz, Austria ; N.L.Kilah ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; A.C.Willis ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; S.B.Wild ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; #============================================================================== data_jww8 _database_code_depnum_ccdc_archive 'CCDC 600535' _audit_creation_date 02-05-06 _audit_creation_method CRYSTALS_ver_12-03-99 # 10191610 Compound Wdt 207 _audit_update_record ; 2002-06-05 - Report on C60 H76 Br F18 P7 Sb4 by Anthony C. Willis for J. Wolfram Wielandt and S. Bruce Wild 2002-06-06 - passes checkcif tests with minor warnings ; # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Sb(C~6~H~5~)~2~P(CH~3~)~3~](PF~6~)~0.75~Br~0.25~ is reported. ; _publ_section_comment #Text of the paper ; The crystallographic unit cell contains eight [Sb(C~6~H~5~)~2~P(CH~3~)~3~]^+^ cations, six (PF~6~)^-^ anions and two Br^-^ anions. The cations lie on mirror planes, some of the (PF~6~)^-^s are centred on sites of 2/m symmetry and the remaining (PF~6~)^-^s are centred on sites of 4/m symmetry, and the Br^-^s are on 4/m sites. The F atoms were introduced lying on mirror planes or 4-fold axes and with full-occupancy, but their anisotropic displacement factors refined to unacceptable values. The F atoms, with the exception of F(1), appeared to be disordered, and so were displaced from these symmetry sites and assigned appropriately reduced occupancies. The F atoms were initially refined with isotropic displacement parameters, and then anisotropically. Restraints were imposed upon the anisotropic displacement parameters of F(4) to maintain sensible values. Hydrogen atoms were included at idealized positions and ride on the atoms to which they were bonded. The biggest peaks in the final difference electron density map lie midway between the Sb and Br atoms. An alternative approach is to refine the structure without the (PF~6~)^-^s and apply SQUEEZE within PLATON to remove all the electron density from these regions of the unit cell [van der Sluis, P. and Spek, A.L. (1990) Acta Crystallogr., Sect. A, 46, 194-201], and then further refine the rest of the structure. This method yields agreement factors R = 0.026, wR = 0.029 and S = 0.88, with distances and angles within the cation essentially identical to those presented here. Besides the distances and angles listed in the Tables, there is also a contact distance for Sb1....Br1 of 3.2236(3)\%A, with angles P1---Sb1....Br1 173.29(3)\% and C11---Sb1....Br1 86.59(8)\%. The Br has contacts to four Sb atoms in a square planar arrangement. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms bonded to C ride on the atoms to which they were bonded. ; _publ_section_exptl_prep ; The compound was prepared by JWW and recrystallized from dichloromethane/diethyl ether. ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 15.5328(2) _cell_angle_alpha 90 _cell_length_b 15.5328(2) _cell_angle_beta 90 _cell_length_c 15.5904(3) _cell_angle_gamma 90 _cell_volume 3761.4(1) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/m n c ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y,x,z y,-x,-z -x,-y,z x,y,-z y,-x,z -y,x,-z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,-z+1/2 y+1/2,x+1/2,z+1/2 -y+1/2,-x+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 -y+1/2,-x+1/2,z+1/2 y+1/2,x+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.3740 2.4560 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Sb ' -0.8160 1.5460 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825 4.5909 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C60 H76 Br1 F18 P7 Sb4 ' _chemical_formula_moiety ' 4(C15 H19 P Sb 2+), (F6 P -)3, Br - ' _chemical_compound_source ; ? ; _chemical_formula_weight 1922.96 _cell_measurement_reflns_used 27843 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 200 _cell_formula_units_Z 2 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1878.813 _exptl_absorpt_coefficient_mu 2.181 # Sheldrick geometric definitions 0.62 0.90 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 2 deg at rate 100 sec/frame, crystal-detector distance 28mm, multiple scan sets so over 90 percent of data collected with 4-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 1 0 0.160 -1 -1 0 0.200 1 -1 0 0.120 -1 1 0 0.100 0 0 1 0.020 0 0 -1 0.030 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.509 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 44245 _reflns_number_total 2261 _diffrn_reflns_av_R_equivalents 0.07 # Number of reflections with Friedels Law is 2261 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2165 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_gt 1108 _diffrn_reflns_theta_min 2.613 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_theta_full 27.56 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -0.32 _refine_diff_density_max 0.47 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 1102 _refine_ls_number_parameters 133 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0200 _refine_ls_goodness_of_fit_ref 1.1587 _refine_ls_shift/su_max 0.000105 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.263 0.135 0.125 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Carruthers, J.R. & Watkin, D.J. (1979) Acta Cryst., A35, 698-699. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Sb1 Sb 0.123089(19) 0.16709(2) 0.0000 0.0323 1.0000 Uani S T . . 3 . Br1 Br 0.0000 0.0000 0.0000 0.0376 1.0000 Uani S T . . 3 . P1 P 0.23677(7) 0.28860(8) 0.0000 0.0382 1.0000 Uani S T . . 3 . P2 P 0.5000 0.0000 0.0000 0.0720 1.0000 Uani S T . . 3 . P3 P 0.5000 0.5000 0.0000 0.0338 1.0000 Uani S TU . . 3 . F1 F 0.4026(2) -0.0328(2) 0.0000 0.0896 1.0000 Uani S T . . . . F2 F 0.4935(6) 0.0396(6) -0.0907(8) 0.1431 0.5000 Uani . . . . . . F3 F 0.4682(5) 0.0873(5) 0.0394(7) 0.1294 0.5000 Uani . . . . . . F4 F 0.4608(11) 0.5281(14) -0.0854(6) 0.0822 0.2500 Uani . U . . . . F5 F 0.5218(3) 0.4069(3) -0.0334(4) 0.0899 0.5000 Uani . . . . . . C11 C 0.1842(2) 0.11182(19) 0.1111(2) 0.0346 1.0000 Uani . . . . 3 . C12 C 0.1338(3) 0.1146(2) 0.1847(2) 0.0540 1.0000 Uani . . . . 3 . C13 C 0.1664(4) 0.0856(3) 0.2627(3) 0.0692 1.0000 Uani . . . . 3 . C14 C 0.2481(4) 0.0540(3) 0.2673(3) 0.0638 1.0000 Uani . . . . 3 . C15 C 0.2984(3) 0.0498(2) 0.1955(3) 0.0564 1.0000 Uani . . . . 3 . C16 C 0.2665(2) 0.0787(2) 0.1166(2) 0.0437 1.0000 Uani . . . . 3 . C31 C 0.2223(3) 0.3552(3) 0.0933(3) 0.0707 1.0000 Uani . . . . 3 . C41 C 0.3484(3) 0.2581(4) 0.000000(7) 0.0463 1.0000 Uani S T . . 3 . H121 H 0.0734 0.1367 0.1810 0.0638 1.0000 Uiso R . . . 3 . H131 H 0.1300 0.0882 0.3155 0.0843 1.0000 Uiso R . . . 3 . H141 H 0.2716 0.0342 0.3237 0.0762 1.0000 Uiso R . . . 3 . H151 H 0.3581 0.0263 0.1994 0.0680 1.0000 Uiso R . . . 3 . H161 H 0.3030 0.0751 0.0639 0.0536 1.0000 Uiso R . . . 3 . H311 H 0.2662 0.4023 0.0935 0.0854 1.0000 Uiso R . . . 3 . H312 H 0.1633 0.3808 0.0921 0.0854 1.0000 Uiso R . . . 3 . H313 H 0.2290 0.3193 0.1461 0.0854 1.0000 Uiso R . . . 3 . H411 H 0.3852 0.3109 0.000000 0.0562 1.0000 Uiso RS . . . 3 . H412 H 0.3611 0.2231 0.058788 0.0562 1.0000 Uiso R . . . 3 . 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 0.02413(15) 0.03086(16) 0.04189(17) 0.0000 0.0000 0.00197(13) Br1 0.0291(3) 0.0291(3) 0.0546(6) 0.0000 0.0000 0.0000 P1 0.0337(6) 0.0305(6) 0.0505(8) 0.0000 0.0000 -0.0021(5) P2 0.0278(10) 0.0356(11) 0.153(3) 0.0000 0.0000 0.0052(9) P3 0.0324(7) 0.0324(7) 0.0365(13) 0.0000 0.0000 0.0000 F1 0.0297(17) 0.051(2) 0.188(5) 0.0000 0.0000 0.0000(14) F2 0.077(7) 0.181(14) 0.171(8) 0.075(8) -0.029(8) -0.030(10) F3 0.047(3) 0.063(4) 0.28(2) -0.063(7) 0.019(5) 0.003(2) F4 0.088(8) 0.096(8) 0.063(5) 0.027(7) -0.038(6) 0.012(5) F5 0.062(3) 0.046(2) 0.162(9) -0.039(4) 0.008(3) 0.005(2) C11 0.0385(18) 0.0291(15) 0.0361(17) -0.0021(13) 0.0043(13) -0.0066(12) C12 0.067(3) 0.050(2) 0.0451(19) -0.0054(18) 0.0161(19) 0.0024(19) C13 0.115(4) 0.057(2) 0.036(2) -0.0053(19) 0.017(3) -0.003(3) C14 0.110(4) 0.043(2) 0.038(2) 0.0025(18) -0.017(2) -0.018(2) C15 0.060(2) 0.054(2) 0.055(3) 0.0120(19) -0.022(2) -0.0072(19) C16 0.040(2) 0.048(2) 0.042(2) 0.0078(17) -0.0041(16) -0.0024(16) C31 0.054(3) 0.062(3) 0.095(4) -0.040(3) -0.001(3) 0.002(2) C41 0.029(2) 0.044(3) 0.066(4) 0.0000 0.0000 -0.008(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sb1 . C11 6_555 2.153(3) yes Sb1 . P1 . 2.5846(13) yes Sb1 . C11 . 2.153(3) yes P1 . C31 6_555 1.799(4) yes P1 . C31 . 1.799(4) yes P1 . C41 . 1.798(5) yes P2 . F1 2_655 1.597(3) yes P2 . F3 5_655 1.568(7) yes P2 . F3 2_655 1.568(7) yes P2 . F3 6_555 1.568(7) yes P2 . F2 2_655 1.545(11) yes P2 . F2 5_655 1.545(11) yes P2 . F2 6_555 1.545(11) yes P2 . F1 . 1.597(3) yes P2 . F2 . 1.545(11) yes P2 . F3 . 1.568(7) yes P3 . F5 7_565 1.574(5) yes P3 . F5 8_655 1.574(5) yes P3 . F5 3_655 1.574(5) yes P3 . F5 4_565 1.574(5) yes P3 . F5 2_665 1.574(5) yes P3 . F5 6_555 1.574(5) yes P3 . F5 5_665 1.574(5) yes P3 . F4 5_665 1.528(9) yes P3 . F4 2_665 1.528(9) yes P3 . F4 6_555 1.528(9) yes P3 . F4 4_565 1.528(9) yes P3 . F4 7_565 1.528(9) yes P3 . F4 . 1.528(9) yes P3 . F5 . 1.574(5) yes F2 . F2 5_655 1.246(19) yes F2 . F3 6_555 1.158(13) yes F3 . F3 6_555 1.23(2) yes F4 . F4 5_665 1.500(19) yes F4 . F5 7_565 1.40(2) yes F4 . F5 5_665 1.32(2) yes F4 . F4 7_565 1.061(13) yes F4 . F4 3_655 1.061(13) yes F5 . F5 6_555 1.041(13) yes C11 . C12 . 1.390(5) yes C11 . C16 . 1.381(5) yes C12 . C13 . 1.392(6) yes C12 . H121 . 1.000 no C13 . C14 . 1.364(6) yes C13 . H131 . 1.000 no C14 . C15 . 1.367(6) yes C14 . H141 . 1.000 no C15 . C16 . 1.399(5) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C41 . H412 6_555 1.083 no C41 . H411 . 1.000 no C41 . H412 . 1.083 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 6_555 Sb1 . P1 . 89.43(8) yes C11 6_555 Sb1 . C11 . 107.08(16) yes P1 . Sb1 . C11 . 89.43(8) yes Sb1 . P1 . C31 6_555 109.53(16) yes Sb1 . P1 . C31 . 109.53(16) yes C31 6_555 P1 . C31 . 107.9(4) yes Sb1 . P1 . C41 . 117.80(18) yes C31 6_555 P1 . C41 . 105.80(18) yes C31 . P1 . C41 . 105.80(18) yes F1 2_655 P2 . F3 5_655 88.7(3) yes F1 2_655 P2 . F3 2_655 88.7(3) yes F1 2_655 P2 . F3 6_555 91.3(3) yes F3 5_655 P2 . F3 6_555 179.993 yes F1 2_655 P2 . F2 2_655 93.7(3) yes F3 2_655 P2 . F2 2_655 89.6(6) yes F1 2_655 P2 . F2 5_655 93.7(3) yes F3 5_655 P2 . F2 5_655 89.6(6) yes F3 6_555 P2 . F2 5_655 90.4(6) yes F1 2_655 P2 . F2 6_555 86.3(3) yes F3 5_655 P2 . F2 6_555 90.4(6) yes F3 6_555 P2 . F2 6_555 89.6(6) yes F1 2_655 P2 . F1 . 179.993 yes F3 5_655 P2 . F1 . 91.3(3) yes F3 2_655 P2 . F1 . 91.3(3) yes F3 6_555 P2 . F1 . 88.7(3) yes F2 2_655 P2 . F1 . 86.3(3) yes F1 2_655 P2 . F2 . 86.3(3) yes F3 2_655 P2 . F2 . 90.4(6) yes F2 2_655 P2 . F2 . 179.993 yes F1 2_655 P2 . F3 . 91.3(3) yes F3 2_655 P2 . F3 . 179.993 yes F2 2_655 P2 . F3 . 90.4(6) yes F2 5_655 P2 . F2 6_555 179.993 yes F2 5_655 P2 . F1 . 86.3(3) yes F2 6_555 P2 . F1 . 93.7(3) yes F1 . P2 . F2 . 93.7(3) yes F1 . P2 . F3 . 88.7(3) yes F2 . P2 . F3 . 89.6(6) yes F5 7_565 P3 . F5 8_655 179.993 yes F5 3_655 P3 . F5 4_565 179.993 yes F5 7_565 P3 . F5 2_665 96.28(16) yes F5 8_655 P3 . F5 2_665 83.72(16) yes F5 3_655 P3 . F5 2_665 96.28(16) yes F5 4_565 P3 . F5 2_665 83.72(16) yes F5 7_565 P3 . F5 6_555 96.28(16) yes F5 8_655 P3 . F5 6_555 83.72(16) yes F5 3_655 P3 . F5 6_555 96.28(16) yes F5 4_565 P3 . F5 6_555 83.72(16) yes F5 7_565 P3 . F5 5_665 83.72(16) yes F5 8_655 P3 . F5 5_665 96.28(16) yes F5 3_655 P3 . F5 5_665 83.72(16) yes F5 4_565 P3 . F5 5_665 96.28(16) yes F5 7_565 P3 . F4 5_665 91.0(8) yes F5 8_655 P3 . F4 5_665 89.0(8) yes F5 3_655 P3 . F4 2_665 89.0(8) yes F5 4_565 P3 . F4 2_665 91.0(8) yes F5 2_665 P3 . F4 2_665 93.5(7) yes F5 7_565 P3 . F4 6_555 89.0(8) yes F5 8_655 P3 . F4 6_555 91.0(8) yes F5 3_655 P3 . F4 4_565 86.5(7) yes F5 4_565 P3 . F4 4_565 93.5(7) yes F5 7_565 P3 . F4 7_565 93.5(7) yes F5 8_655 P3 . F4 7_565 86.5(7) yes F5 2_665 P3 . F4 7_565 89.0(8) yes F5 3_655 P3 . F4 . 91.0(8) yes F5 4_565 P3 . F4 . 89.0(8) yes F5 2_665 P3 . F4 . 86.5(7) yes F5 7_565 P3 . F5 . 83.72(16) yes F5 8_655 P3 . F5 . 96.28(16) yes F5 3_655 P3 . F5 . 83.72(16) yes F5 4_565 P3 . F5 . 96.28(16) yes F5 2_665 P3 . F5 . 179.993 yes F5 6_555 P3 . F5 5_665 179.993 yes F5 6_555 P3 . F4 5_665 86.5(7) yes F5 5_665 P3 . F4 5_665 93.5(7) yes F5 6_555 P3 . F4 6_555 93.5(7) yes F5 5_665 P3 . F4 6_555 86.5(7) yes F4 5_665 P3 . F4 6_555 179.992 yes F5 6_555 P3 . F4 4_565 91.0(8) yes F5 5_665 P3 . F4 4_565 89.0(8) yes F4 2_665 P3 . F4 . 179.992 yes F4 2_665 P3 . F5 . 86.5(7) yes F4 7_565 P3 . F5 . 91.0(8) yes F4 . P3 . F5 . 93.5(7) yes Sb1 . C11 . C12 . 113.8(3) yes Sb1 . C11 . C16 . 127.4(2) yes C12 . C11 . C16 . 118.8(3) yes C11 . C12 . C13 . 120.4(4) yes C11 . C12 . H121 . 119.461 no C13 . C12 . H121 . 120.146 no C12 . C13 . C14 . 120.1(4) yes C12 . C13 . H131 . 120.014 no C14 . C13 . H131 . 119.849 no C13 . C14 . C15 . 120.3(4) yes C13 . C14 . H141 . 119.824 no C15 . C14 . H141 . 119.843 no C14 . C15 . C16 . 120.2(4) yes C14 . C15 . H151 . 119.765 no C16 . C15 . H151 . 120.018 no C15 . C16 . C11 . 120.1(4) yes C15 . C16 . H161 . 120.217 no C11 . C16 . H161 . 119.668 no P1 . C31 . H311 . 109.764 no P1 . C31 . H312 . 109.191 no H311 . C31 . H312 . 109.476 no P1 . C31 . H313 . 109.443 no H311 . C31 . H313 . 109.476 no H312 . C31 . H313 . 109.477 no H412 6_555 C41 . P1 . 107.887 no H412 6_555 C41 . H411 . 107.927 no P1 . C41 . H411 . 109.536 no H412 6_555 C41 . H412 . 115.586 no P1 . C41 . H412 . 107.887 no H411 . C41 . H412 . 107.927 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Sb1 Br1 3.2235(3) . . no #------------------------------------------------------------------------------ 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 C11 Sb1 P1 C31 -67.37(18) . . . . no C11 Sb1 P1 C41 53.54(8) . . . . no C11 Sb1 P1 C31 174.45(18) . . . 6_555 no C11 Sb1 P1 C31 -174.45(18) 6_555 . . . no P1 Sb1 C11 C12 113.6(2) . . . . no P1 Sb1 C11 C16 -63.5(3) . . . . no C11 Sb1 C11 C12 -157.2(2) 6_555 . . . no C11 Sb1 C11 C16 25.7(3) 6_555 . . . no Sb1 C11 C12 C13 -176.5(3) . . . . no C16 C11 C12 C13 0.9(5) . . . . no Sb1 C11 C16 C15 176.1(2) . . . . no C12 C11 C16 C15 -0.9(5) . . . . no C11 C12 C13 C14 -0.2(6) . . . . no C12 C13 C14 C15 -0.6(7) . . . . no C13 C14 C15 C16 0.5(6) . . . . no C14 C15 C16 C11 0.2(5) . . . . no #------------------------------------------------------------------------------ #===END data_wolfram1 _database_code_depnum_ccdc_archive 'CCDC 600536' _audit_creation_date 06-17-01 _audit_creation_method CRYSTALS_ver_12-03-99 _audit_update_record ; 2006-01-18 - Report on C60 H76 Cl F18 P7 Sb4 by Nathan L. Kilah for J. Wolfram Wielandt and S. Bruce Wild 2005-02-01 - Passes Checkcif with minor warnings. ; # 9261138 wolfram1 # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #**************************************************************************** # The contents of this file between this point and the next ***** line # are held in the file REFCIF.DAT # This is a character file which you may edit to reflect local conditions # # Items which need looking at are represented by a '?' # Items for which there are choices are prefixed with 'choose from' # # #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Sb(C~6~H~5~)~2~P(CH~3~)~3~](PF~6~)~0.75~Cl~0.25~ is reported. ; _publ_section_comment #Text of the paper ; This compound is isostructural with the bromide complex.The crystallographic unit cell contains eight [Sb(C~6~H~5~)~2~P(CH~3~)~3~]+ cations, six PF~6~- anions and two Cl- anions. The cations lie on mirror planes, some of the (PF~6~)-'s are centred on sites of 2/m symmetry and the remaining (PF~6~)- anions are centred on sites of 4/m symmetry, and the Cl- anions are on 4/m sites. The PF~6~- anions were found to be disordered. One PF~6~- anion was modelled with one whole fluorine atom (F(4)) with the remaining fluorines ((F(5) and F(6)) modelled over two positions of equal occupancy at 90\% to one another. The remaining PF~6~- anion was found to possess greater disorder, with two fluorine atoms on special sites, generating one component of the anion. The remaining electron density was modelled with a sphere, to compensate for the wide spread of electron density due to the symmetry of the site (one fluorine introduced on a non-special site generates eight atoms). Occupancies were refined while the thermal parameters were fixed at averaged values. Restraints were imposed upon the anisotropic displacement parameters of the two individual PF~6~- anions to maintain sensible values. The largest peaks in the final difference maps were located near the disordered PF~6~-. Hydrogen atoms were included at idealised positions and ride on the atoms to which they are bonded. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; Compound prepared by JWW and recrysallised from dichloromethane/diethyl ether. ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; ORTEP3 (Farrugia 1997) ; #============================================================= _cell_length_a 15.4979(2) _cell_angle_alpha 90 _cell_length_b 15.4979(2) _cell_angle_beta 90 _cell_length_c 15.5355(3) _cell_angle_gamma 90 _cell_volume 3731.39(10) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/m n c ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y,x,z y,-x,-z -x,-y,z x,y,-z y,-x,z -y,x,-z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,-z+1/2 y+1/2,x+1/2,z+1/2 -y+1/2,-x+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 -y+1/2,-x+1/2,z+1/2 y+1/2,x+1/2,-z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Sb ' -0.5866 1.5461 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825 4.5909 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C60 H76 Cl1 F18 P7 Sb4 ' _chemical_formula_moiety ' 4(C15 H19 P1 Sb1), 3(F6 P1), Cl ' _chemical_compound_source ; ? ; _chemical_formula_weight 1878.53 _cell_measurement_reflns_used 31538 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 200 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.27 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.47 _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_meas ' not measured ' # Non-dispersive F(000): _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 1.700 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 2.0 deg at rate 10 sec/frame, crystal-detector distance 30mm, multiple scan sets so over 95 percent of data collected with 4-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 -1 0.200 -1 0 1 0.230 -1 1 -1 0.220 0 1 -2 0.150 0 -1 2 0.120 -1 -2 -1 0.200 3 -3 -1 0.200 -7 -3 -2 0.260 -2 1 0 0.270 -2 6 3 0.220 6 7 4 0.150 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 0.662 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_reflns_av_R_equivalents 0.036 # Sheldrick geometric definitions 0.55 0.63 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 56523 _reflns_number_total 2827 # Number of reflections with Friedels Law is 2827 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2729 _diffrn_reflns_theta_min 2.939 _diffrn_reflns_theta_max 30.032 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.032 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -0.93 _refine_diff_density_max 0.98 _refine_ls_number_reflns 1623 _refine_ls_number_restraints 36 _refine_ls_number_parameters 124 #_refine_ls_R_factor_ref 0.0290 _refine_ls_wR_factor_ref 0.0340 _refine_ls_goodness_of_fit_ref 1.1976 #_reflns_number_all 2821 _refine_ls_R_factor_all 0.0497 _refine_ls_wR_factor_all 0.0443 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00\s(I) _reflns_number_gt 1623 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_gt 0.0340 _refine_ls_shift/su_max 0.000112 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.742 0.303 0.476 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo C., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Farrugia, L.J. (1997). J. Appl. Cryst. 30, 565 Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Spek, A.L. (2001) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Watkin D.J. (1994), Acta Cryst, A50, 411-437 ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens #F6 F 0.5000 0.5000 0.0000 0.1227 2.54(12) Uiso DS U P . . . Sb1 Sb 0.12074(2) 0.16241(2) 0.0000 0.0318 1.0000 Uani S T . . . . Cl1 Cl 0.0000 0.0000 0.0000 0.0411 1.0000 Uani S T . . . . P1 P 0.23370(9) 0.28562(9) 0.0000 0.0367 1.0000 Uani S T . . . . P2 P 0.5000 0.0000 0.0000 0.0655 1.0000 Uani DS TU . . . . P3 P 0.5000 0.5000 0.0000 0.0344 1.0000 Uani DS TU . . . . F1 F 0.4019(2) -0.0328(3) 0.0000 0.0812 1.0000 Uani DS TU . . . . F2 F 0.4927(7) 0.0399(7) -0.0911(8) 0.1254 0.5000 Uani D U . . . . F3 F 0.4687(4) 0.0877(5) 0.0406(7) 0.1045 0.5000 Uani D U . . . . F4 F 0.5000 0.5000 0.0992(9) 0.1474 0.63(2) Uani DS TU P . . . F5 F 0.4027(4) 0.4772(4) 0.0000 0.0994 0.63(2) Uani DS TU P . . . C11 C 0.1827(2) 0.1087(2) 0.1119(2) 0.0327 1.0000 Uani . . . . . . C12 C 0.1329(3) 0.1127(3) 0.1865(3) 0.0500 1.0000 Uani . . . . . . C13 C 0.1653(4) 0.0853(4) 0.2645(3) 0.0607 1.0000 Uani . . . . . . C14 C 0.2484(4) 0.0532(3) 0.2696(3) 0.0607 1.0000 Uani . . . . . . C15 C 0.2984(3) 0.0486(3) 0.1965(3) 0.0544 1.0000 Uani . . . . . . C16 C 0.2659(3) 0.0757(3) 0.1174(3) 0.0422 1.0000 Uani . . . . . . C31 C 0.2187(3) 0.3520(3) 0.0939(4) 0.0677 1.0000 Uani . . . . . . C41 C 0.3461(4) 0.2554(4) 0.0000 0.0440 1.0000 Uani S T . . . . H121 H 0.0727 0.1358 0.1835 0.0601 1.0000 Uiso . . . . . . H131 H 0.1287 0.0886 0.3175 0.0725 1.0000 Uiso . . . . . . H141 H 0.2720 0.0335 0.3262 0.0727 1.0000 Uiso . . . . . . H151 H 0.3586 0.0257 0.2002 0.0654 1.0000 Uiso . . . . . . H161 H 0.3024 0.0713 0.0645 0.0506 1.0000 Uiso . . . . . . H311 H 0.2567 0.4039 0.0900 0.0806 1.0000 Uiso . . . . . . H312 H 0.1570 0.3708 0.0973 0.0806 1.0000 Uiso . . . . . . H313 H 0.2337 0.3182 0.1466 0.0806 1.0000 Uiso . . . . . . H411 H 0.3826 0.3085 0.0000 0.0526 1.0000 Uiso . . . . . . H412 H 0.3583 0.2181 -0.0511 0.0526 1.0000 Uiso . . . . . . 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 #F6 0.1227 1.6287 0.0000 0.0000 0.0000 0.0000 Sb1 0.02412(16) 0.03094(17) 0.04019(18) 0.0000 0.0000 0.00335(11) Cl1 0.0361(7) 0.0361(7) 0.0512(15) 0.0000 0.0000 0.0000 P1 0.0320(6) 0.0287(6) 0.0496(7) 0.0000 0.0000 -0.0006(5) P2 0.0253(9) 0.0330(10) 0.138(3) 0.0000 0.0000 0.0060(8) P3 0.0325(7) 0.0325(7) 0.0382(13) 0.0000 0.0000 0.0000 F1 0.0288(17) 0.048(2) 0.167(5) 0.0000 0.0000 0.0018(15) F2 0.083(6) 0.146(10) 0.148(8) 0.049(7) -0.021(7) -0.035(9) F3 0.041(3) 0.058(4) 0.215(12) -0.052(5) 0.014(5) 0.006(3) F4 0.173(8) 0.173(8) 0.095(9) 0.0000 0.0000 0.0000 F5 0.022(3) 0.036(4) 0.240(11) 0.0000 0.0000 -0.002(2) C11 0.0372(18) 0.0306(16) 0.0302(15) -0.0016(13) 0.0017(14) -0.0014(12) C12 0.063(3) 0.047(2) 0.041(2) -0.0021(18) 0.0143(19) 0.0034(19) C13 0.097(4) 0.050(2) 0.035(2) -0.0052(19) 0.014(2) -0.004(3) C14 0.104(4) 0.043(2) 0.034(2) 0.0026(19) -0.014(2) -0.017(2) C15 0.056(3) 0.053(2) 0.054(3) 0.010(2) -0.018(2) -0.003(2) C16 0.0371(19) 0.049(2) 0.041(2) 0.0070(17) -0.0022(17) 0.0003(17) C31 0.054(3) 0.057(3) 0.092(4) -0.036(3) 0.000(3) -0.001(2) C41 0.034(3) 0.035(3) 0.063(4) 0.0000 0.0000 -0.002(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #F4 . F6 . 1.542(14) yes #F5 . F6 . 1.548(6) yes Sb1 . C11 6_555 2.153(4) yes Sb1 . Cl1 . 3.1363(3) yes Sb1 . P1 . 2.5906(14) yes Sb1 . C11 . 2.153(4) yes P1 . C31 6_555 1.799(5) yes P1 . C31 . 1.799(5) yes P1 . C41 . 1.804(6) yes P2 . F1 2_655 1.602(4) yes P2 . F3 6_555 1.575(6) yes P2 . F3 2_655 1.575(6) yes P2 . F3 5_655 1.575(6) yes P2 . F2 2_655 1.548(10) yes P2 . F2 5_655 1.548(10) yes P2 . F2 6_555 1.548(10) yes P2 . F1 . 1.602(4) yes P2 . F2 . 1.548(10) yes P2 . F3 . 1.575(6) yes P3 . F5 4_565 1.548(6) yes P3 . F5 3_655 1.548(6) yes P3 . F5 2_665 1.548(6) yes P3 . F4 2_665 1.542(14) yes P3 . F4 . 1.542(14) yes P3 . F5 . 1.548(6) yes C11 . C12 . 1.394(6) yes C11 . C16 . 1.390(5) yes C12 . C13 . 1.379(7) yes C12 . H121 . 1.000 no C13 . C14 . 1.382(9) yes C13 . H131 . 1.000 no C14 . C15 . 1.377(8) yes C14 . H141 . 1.000 no C15 . C16 . 1.392(6) yes C15 . H151 . 0.999 no C16 . H161 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.002 no C31 . H313 . 1.000 no C41 . H412 6_555 1.000 no C41 . H411 . 0.999 no C41 . H412 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 6_555 Sb1 . Cl1 . 87.45(9) yes C11 6_555 Sb1 . P1 . 89.08(9) yes Cl1 . Sb1 . P1 . 174.12(3) yes C11 6_555 Sb1 . C11 . 107.64(19) yes Cl1 . Sb1 . C11 . 87.45(9) yes P1 . Sb1 . C11 . 89.08(9) yes Sb1 . Cl1 . Sb1 2_555 179.996 yes Sb1 . Cl1 . Sb1 3_555 90.000 yes Sb1 2_555 Cl1 . Sb1 3_555 90.000 yes Sb1 . Cl1 . Sb1 4_555 90.000 yes Sb1 2_555 Cl1 . Sb1 4_555 90.000 yes Sb1 3_555 Cl1 . Sb1 4_555 179.996 yes Sb1 . P1 . C31 6_555 109.51(19) yes Sb1 . P1 . C31 . 109.51(19) yes C31 6_555 P1 . C31 . 108.3(4) yes Sb1 . P1 . C41 . 117.45(19) yes C31 6_555 P1 . C41 . 105.8(2) yes C31 . P1 . C41 . 105.8(2) yes F1 2_655 P2 . F3 6_555 91.1(3) yes F1 2_655 P2 . F3 2_655 88.9(3) yes F3 6_555 P2 . F3 2_655 132.7(8) yes F1 2_655 P2 . F3 5_655 88.9(3) yes F3 6_555 P2 . F3 5_655 179.993 yes F1 2_655 P2 . F2 2_655 93.3(4) yes F3 6_555 P2 . F2 2_655 137.2(5) yes F3 2_655 P2 . F2 2_655 90.0(8) yes F1 2_655 P2 . F2 5_655 93.3(4) yes F3 6_555 P2 . F2 5_655 90.0(8) yes F3 5_655 P2 . F2 5_655 90.0(8) yes F1 2_655 P2 . F2 6_555 86.7(4) yes F3 6_555 P2 . F2 6_555 90.0(8) yes F3 5_655 P2 . F2 6_555 90.0(8) yes F1 2_655 P2 . F1 . 179.993 yes F3 6_555 P2 . F1 . 88.9(3) yes F3 2_655 P2 . F1 . 91.1(3) yes F3 5_655 P2 . F1 . 91.1(3) yes F2 2_655 P2 . F1 . 86.7(4) yes F1 2_655 P2 . F2 . 86.7(4) yes F3 2_655 P2 . F2 . 90.0(8) yes F2 2_655 P2 . F2 . 179.993 yes F1 2_655 P2 . F3 . 91.1(3) yes F3 2_655 P2 . F3 . 179.993 yes F2 2_655 P2 . F3 . 90.0(8) yes F2 5_655 P2 . F2 6_555 179.993 yes F2 5_655 P2 . F1 . 86.7(4) yes F2 6_555 P2 . F1 . 93.3(4) yes F1 . P2 . F2 . 93.3(4) yes F1 . P2 . F3 . 88.9(3) yes F2 . P2 . F3 . 90.0(8) yes F5 4_565 P3 . F5 3_655 179.993 yes F5 4_565 P3 . F5 2_665 90.000 yes F5 3_655 P3 . F5 2_665 90.000 yes F5 4_565 P3 . F4 2_665 90.000 yes F5 3_655 P3 . F4 2_665 90.000 yes F5 2_665 P3 . F4 2_665 90.000 yes F5 4_565 P3 . F4 . 90.000 yes F5 3_655 P3 . F4 . 90.000 yes F5 2_665 P3 . F4 . 90.000 yes F4 2_665 P3 . F4 . 179.993 yes F5 4_565 P3 . F5 . 90.000 yes F5 3_655 P3 . F5 . 90.000 yes F5 2_665 P3 . F5 . 179.993 yes F4 2_665 P3 . F5 . 90.000 yes F4 . P3 . F5 . 90.000 yes Sb1 . C11 . C12 . 114.1(3) yes Sb1 . C11 . C16 . 127.3(3) yes C12 . C11 . C16 . 118.5(4) yes C11 . C12 . C13 . 121.1(5) yes C11 . C12 . H121 . 119.508 no C13 . C12 . H121 . 119.405 no C12 . C13 . C14 . 120.0(5) yes C12 . C13 . H131 . 120.073 no C14 . C13 . H131 . 119.962 no C13 . C14 . C15 . 119.8(4) yes C13 . C14 . H141 . 120.062 no C15 . C14 . H141 . 120.168 no C14 . C15 . C16 . 120.5(5) yes C14 . C15 . H151 . 119.728 no C16 . C15 . H151 . 119.758 no C15 . C16 . C11 . 120.1(4) yes C15 . C16 . H161 . 119.971 no C11 . C16 . H161 . 119.919 no P1 . C31 . H311 . 109.596 no P1 . C31 . H312 . 109.454 no H311 . C31 . H312 . 109.332 no P1 . C31 . H313 . 109.591 no H311 . C31 . H313 . 109.538 no H312 . C31 . H313 . 109.315 no H412 6_555 C41 . P1 . 109.422 no H412 6_555 C41 . H411 . 111.618 no P1 . C41 . H411 . 109.461 no H412 6_555 C41 . H412 . 105.204 no P1 . C41 . H412 . 109.422 no H411 . C41 . H412 . 111.618 no 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 C11 Sb1 P1 C31 -66.9(2) . . . . no C11 Sb1 P1 C41 53.84(8) . . . . no C11 Sb1 P1 C31 174.6(2) . . . 6_555 no C11 Sb1 P1 C31 -174.6(2) 6_555 . . . no P1 Sb1 C11 C12 112.4(3) . . . . no P1 Sb1 C11 C16 -64.2(3) . . . . no C11 Sb1 C11 C12 -158.9(3) 6_555 . . . no C11 Sb1 C11 C16 24.5(4) 6_555 . . . no Sb1 C11 C12 C13 -176.4(4) . . . . no C16 C11 C12 C13 0.5(6) . . . . no Sb1 C11 C16 C15 175.6(3) . . . . no C12 C11 C16 C15 -0.9(6) . . . . no C11 C12 C13 C14 0.0(8) . . . . no C12 C13 C14 C15 -0.1(8) . . . . no C13 C14 C15 C16 -0.2(7) . . . . no C14 C15 C16 C11 0.8(7) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Sb1 Cl1 3.1364(3) . . no Sb1 Sb1 4.4355(4) . 3_555 no #==END