Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Batsanov, Andrei S.' 'Cornet, Stephanie M.' 'Dillon, Keith B.' 'Goeta, Andres E.' 'Hazendonk, Paul' 'Thompson, Amber L.' _publ_contact_author 'Dr Keith B. Dillon' _publ_contact_author_address ; Department of Chemistry University of Durham South Road, Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email K.B.DILLON@DURHAM.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The synthesis and characterisation of some new Group 15 compounds containing the 2,4,6-(CF~3~)~3~C~6~H~2~ (fluoromes = Ar), 2,6-(CF~3~)~2~C~6~H~3~ (fluoroxyl = Ar') or 2,4-(CF~3~)~2~C~6~H~3~ (Ar") ligands ; data_1 _database_code_CSD 189700 _audit_creation_method SHELXL-97 _chemical_name_systematic ; dibromo-(2,4,6-tris-(trifluoromethyl)-phenyl)-phosphane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H2 Br2 F9 P' _chemical_formula_weight 471.90 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.000(1) _cell_length_b 10.501(1) _cell_length_c 16.153(2) _cell_angle_alpha 101.39(1) _cell_angle_beta 98.48(1) _cell_angle_gamma 90.91(1) _cell_volume 1314.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 967 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 6.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1712 _exptl_absorpt_correction_T_max 0.2796 _exptl_absorpt_process_details 'SADABS (Sheldrick,1998); R(int)=0.107 before correction' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.42 cm. ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16039 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 29.00 _reflns_number_total 6864 _reflns_number_gt 5691 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SMART version 5.054 (Bruker, 1998)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. F(4), F(5), F(6) are disordered between 2 positions with occupancies 96% (unprimed) and 4% (primed), the latter were refined with a common isotropic U. F(14), F(15), F(16) are disordered between 2 positions with occupancies refined to 89.8(4)% (unprimed) and 10.2(4)% (primed); anisotropic ADP of opposing atoms constrained to equality. ; _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^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6864 _refine_ls_number_parameters 399 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.070 _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 Br1 Br 0.69028(4) 0.46569(3) 0.133048(19) 0.02578(7) Uani 1 1 d . . . Br2 Br 0.89720(3) 0.77040(3) 0.147537(19) 0.02611(7) Uani 1 1 d . . . P1 P 0.79831(9) 0.64373(7) 0.22558(5) 0.02101(15) Uani 1 1 d . . . C1 C 0.6039(3) 0.7284(2) 0.25494(16) 0.0173(5) Uani 1 1 d . . . C2 C 0.5866(3) 0.7395(3) 0.34218(16) 0.0184(5) Uani 1 1 d . . . C3 C 0.4657(3) 0.8142(3) 0.37951(17) 0.0191(5) Uani 1 1 d . . . H3 H 0.4575 0.8193 0.4381 0.023 Uiso 1 1 d R . . C4 C 0.3568(3) 0.8814(3) 0.33061(17) 0.0197(5) Uani 1 1 d . A . C5 C 0.3621(3) 0.8678(3) 0.24408(17) 0.0198(5) Uani 1 1 d . . . H5 H 0.2834 0.9114 0.2108 0.024 Uiso 1 1 d R . . C6 C 0.4826(3) 0.7912(2) 0.20556(16) 0.0173(5) Uani 1 1 d . . . C7 C 0.7006(4) 0.6706(3) 0.40154(18) 0.0260(6) Uani 1 1 d . . . C8 C 0.2293(4) 0.9662(3) 0.37130(18) 0.0259(6) Uani 1 1 d D . . C9 C 0.4678(3) 0.7899(3) 0.11036(17) 0.0219(5) Uani 1 1 d . . . F1 F 0.7123(2) 0.54353(17) 0.36721(11) 0.0310(4) Uani 1 1 d . . . F2 F 0.6431(2) 0.67448(19) 0.47535(11) 0.0370(4) Uani 1 1 d . . . F3 F 0.8599(2) 0.72326(19) 0.42146(11) 0.0356(4) Uani 1 1 d . . . F4 F 0.2894(3) 1.0238(2) 0.45112(13) 0.0469(6) Uani 0.96 1 d PD A 1 F5 F 0.0903(3) 0.8994(2) 0.37473(17) 0.0614(7) Uani 0.96 1 d PD A 1 F6 F 0.1853(3) 1.0596(2) 0.32958(15) 0.0605(7) Uani 0.96 1 d PD A 1 F4' F 0.080(2) 0.975(3) 0.327(3) 0.058(9) Uiso 0.04 1 d PD A 2 F5' F 0.270(6) 1.0911(13) 0.3987(11) 0.058(9) Uiso 0.04 1 d PD A 2 F6' F 0.180(4) 0.940(4) 0.4411(6) 0.058(9) Uiso 0.04 1 d PD A 2 F7 F 0.5422(2) 0.89813(16) 0.09637(11) 0.0280(4) Uani 1 1 d . . . F8 F 0.3044(2) 0.78851(18) 0.07557(10) 0.0304(4) Uani 1 1 d . . . F9 F 0.5336(2) 0.68796(16) 0.06536(10) 0.0257(3) Uani 1 1 d . . . Br3 Br 0.38423(3) 1.18829(3) 0.122563(19) 0.02554(7) Uani 1 1 d . . . Br4 Br 0.17264(4) 1.47078(3) 0.093164(18) 0.02508(7) Uani 1 1 d . . . P2 P 0.28788(8) 1.36783(7) 0.19345(4) 0.01844(14) Uani 1 1 d . . . C11 C 0.0964(3) 1.3063(2) 0.23202(15) 0.0153(5) Uani 1 1 d . . . C12 C -0.0262(3) 1.2065(2) 0.19194(16) 0.0165(5) Uani 1 1 d . . . C13 C -0.1468(3) 1.1653(2) 0.23677(16) 0.0187(5) Uani 1 1 d . . . H13 H -0.2276 1.0974 0.2088 0.022 Uiso 1 1 d R . . C14 C -0.1487(3) 1.2229(3) 0.32138(17) 0.0186(5) Uani 1 1 d . B . C15 C -0.0353(3) 1.3240(3) 0.36197(16) 0.0188(5) Uani 1 1 d . . . H15 H -0.0389 1.3646 0.4197 0.023 Uiso 1 1 d R . . C16 C 0.0852(3) 1.3662(2) 0.31769(16) 0.0166(5) Uani 1 1 d . . . C17 C -0.0421(3) 1.1318(3) 0.10057(16) 0.0199(5) Uani 1 1 d . . . C18 C -0.2770(4) 1.1725(3) 0.36815(18) 0.0263(6) Uani 1 1 d D . . C19 C 0.2018(3) 1.4802(3) 0.36672(17) 0.0224(6) Uani 1 1 d . . . F11 F 0.0464(2) 1.02253(15) 0.09601(10) 0.0254(3) Uani 1 1 d . . . F12 F -0.2033(2) 1.09161(17) 0.06930(10) 0.0283(4) Uani 1 1 d . . . F13 F 0.0099(2) 1.19941(15) 0.04687(9) 0.0235(3) Uani 1 1 d . . . F14 F -0.2504(4) 1.2187(3) 0.45089(14) 0.0748(12) Uani 0.898(4) 1 d PD B 1 F15 F -0.2783(4) 1.0445(2) 0.35915(18) 0.0577(9) Uani 0.898(4) 1 d PD B 1 F16 F -0.4337(3) 1.1987(4) 0.3393(2) 0.0901(13) Uani 0.898(4) 1 d PD B 1 F14' F -0.3942(14) 1.0890(8) 0.3215(10) 0.0748(12) Uani 0.10 1 d PD B 2 F15' F -0.3581(16) 1.2664(12) 0.4052(6) 0.0577(9) Uani 0.10 1 d PD B 2 F16' F -0.208(2) 1.1097(8) 0.4260(6) 0.0901(13) Uani 0.10 1 d PD B 2 F17 F 0.2032(2) 1.57663(16) 0.32261(11) 0.0288(4) Uani 1 1 d . . . F18 F 0.3630(2) 1.44876(17) 0.38536(10) 0.0283(4) Uani 1 1 d . . . F19 F 0.1533(2) 1.53246(17) 0.44160(11) 0.0335(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.02358(14) 0.01643(13) 0.03787(16) 0.00341(11) 0.00926(11) 0.00130(10) Br2 0.02356(14) 0.02234(14) 0.03507(16) 0.00708(11) 0.01165(11) -0.00216(11) P1 0.0166(3) 0.0211(4) 0.0265(4) 0.0069(3) 0.0041(3) 0.0028(3) C1 0.0160(12) 0.0148(12) 0.0216(12) 0.0045(10) 0.0033(9) 0.0003(9) C2 0.0197(13) 0.0158(12) 0.0195(12) 0.0058(10) 0.0000(10) -0.0029(10) C3 0.0205(13) 0.0192(13) 0.0178(12) 0.0042(10) 0.0031(10) -0.0030(10) C4 0.0175(12) 0.0165(13) 0.0245(13) 0.0025(10) 0.0040(10) -0.0019(10) C5 0.0184(12) 0.0180(13) 0.0225(13) 0.0053(10) 0.0002(10) 0.0004(10) C6 0.0171(12) 0.0155(12) 0.0182(12) 0.0032(10) -0.0001(9) -0.0034(9) C7 0.0260(15) 0.0286(15) 0.0254(14) 0.0113(12) 0.0013(11) 0.0051(12) C8 0.0244(14) 0.0278(15) 0.0249(14) 0.0022(12) 0.0058(11) 0.0046(11) C9 0.0226(13) 0.0207(14) 0.0227(13) 0.0056(11) 0.0029(10) 0.0019(11) F1 0.0356(10) 0.0247(9) 0.0370(10) 0.0141(8) 0.0076(8) 0.0110(7) F2 0.0476(11) 0.0467(12) 0.0237(9) 0.0198(8) 0.0095(8) 0.0172(9) F3 0.0247(9) 0.0444(11) 0.0357(10) 0.0130(9) -0.0082(7) 0.0018(8) F4 0.0473(13) 0.0500(13) 0.0322(11) -0.0142(10) -0.0019(9) 0.0224(10) F5 0.0331(12) 0.0555(15) 0.0887(19) -0.0202(13) 0.0355(12) -0.0108(10) F6 0.0799(18) 0.0652(16) 0.0558(14) 0.0349(13) 0.0371(13) 0.0578(14) F7 0.0380(10) 0.0217(8) 0.0293(9) 0.0120(7) 0.0114(7) 0.0030(7) F8 0.0274(9) 0.0424(11) 0.0205(8) 0.0093(7) -0.0033(7) 0.0067(8) F9 0.0337(9) 0.0233(8) 0.0191(8) 0.0022(6) 0.0034(6) 0.0046(7) Br3 0.02383(14) 0.02075(14) 0.03386(16) 0.00405(11) 0.01185(11) 0.00507(11) Br4 0.02775(15) 0.02155(14) 0.02997(15) 0.01275(11) 0.00723(11) 0.00156(11) P2 0.0179(3) 0.0176(3) 0.0204(3) 0.0037(3) 0.0054(2) -0.0001(2) C11 0.0151(11) 0.0159(12) 0.0163(11) 0.0050(9) 0.0042(9) 0.0034(9) C12 0.0177(12) 0.0149(12) 0.0169(12) 0.0029(9) 0.0026(9) 0.0023(9) C13 0.0198(12) 0.0155(12) 0.0207(12) 0.0038(10) 0.0022(10) -0.0008(10) C14 0.0189(12) 0.0169(13) 0.0210(12) 0.0040(10) 0.0061(10) 0.0015(10) C15 0.0210(13) 0.0190(13) 0.0166(12) 0.0014(10) 0.0064(10) 0.0033(10) C16 0.0169(12) 0.0139(12) 0.0180(12) 0.0010(9) 0.0025(9) 0.0006(9) C17 0.0235(13) 0.0190(13) 0.0175(12) 0.0026(10) 0.0058(10) -0.0016(10) C18 0.0279(15) 0.0266(15) 0.0247(14) 0.0008(12) 0.0115(11) -0.0042(12) C19 0.0231(14) 0.0221(14) 0.0204(13) -0.0011(11) 0.0058(10) -0.0020(11) F11 0.0363(9) 0.0165(8) 0.0227(8) -0.0005(6) 0.0082(7) 0.0008(7) F12 0.0277(9) 0.0364(10) 0.0183(8) 0.0032(7) -0.0003(6) -0.0096(7) F13 0.0318(9) 0.0238(8) 0.0152(7) 0.0050(6) 0.0039(6) -0.0043(7) F14 0.111(3) 0.083(2) 0.0249(12) -0.0138(12) 0.0347(14) -0.0671(19) F15 0.079(2) 0.0297(13) 0.0732(19) 0.0032(12) 0.0504(15) -0.0172(12) F16 0.0306(14) 0.161(4) 0.118(3) 0.101(3) 0.0372(16) 0.0302(17) F14' 0.111(3) 0.083(2) 0.0249(12) -0.0138(12) 0.0347(14) -0.0671(19) F15' 0.079(2) 0.0297(13) 0.0732(19) 0.0032(12) 0.0504(15) -0.0172(12) F16' 0.0306(14) 0.161(4) 0.118(3) 0.101(3) 0.0372(16) 0.0302(17) F17 0.0311(9) 0.0177(8) 0.0367(9) 0.0038(7) 0.0045(7) -0.0042(7) F18 0.0198(8) 0.0369(10) 0.0253(8) 0.0036(7) -0.0015(6) -0.0034(7) F19 0.0366(10) 0.0327(10) 0.0253(9) -0.0118(7) 0.0111(7) -0.0076(8) _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 Br1 P1 2.2228(8) . ? Br2 P1 2.2153(8) . ? P1 C1 1.879(3) . ? C1 C2 1.418(4) . ? C1 C6 1.419(4) . ? C2 C3 1.387(4) . ? C2 C7 1.521(4) . ? C3 C4 1.385(4) . ? C4 C5 1.384(4) . ? C4 C8 1.504(4) . ? C5 C6 1.403(4) . ? C6 C9 1.522(4) . ? C7 F2 1.333(3) . ? C7 F3 1.349(3) . ? C7 F1 1.351(3) . ? C8 F4' 1.312(10) . ? C8 F5' 1.318(10) . ? C8 F5 1.319(3) . ? C8 F6 1.320(4) . ? C8 F6' 1.322(9) . ? C8 F4 1.326(3) . ? C9 F9 1.332(3) . ? C9 F8 1.343(3) . ? C9 F7 1.348(3) . ? Br3 P2 2.2166(8) . ? Br4 P2 2.2194(8) . ? P2 C11 1.887(3) . ? C11 C12 1.411(4) . ? C11 C16 1.419(3) . ? C12 C13 1.400(3) . ? C12 C17 1.515(3) . ? C13 C14 1.383(4) . ? C14 C15 1.378(4) . ? C14 C18 1.508(4) . ? C15 C16 1.397(3) . ? C16 C19 1.518(4) . ? C17 F13 1.331(3) . ? C17 F12 1.343(3) . ? C17 F11 1.353(3) . ? C18 F15' 1.286(9) . ? C18 F16' 1.311(9) . ? C18 F14' 1.312(9) . ? C18 F14 1.313(4) . ? C18 F15 1.323(4) . ? C18 F16 1.324(4) . ? C19 F19 1.341(3) . ? C19 F18 1.342(3) . ? C19 F17 1.349(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 Br2 102.10(8) . . ? C1 P1 Br1 102.52(9) . . ? Br2 P1 Br1 105.35(3) . . ? C2 C1 C6 116.2(2) . . ? C2 C1 P1 113.59(19) . . ? C6 C1 P1 129.93(19) . . ? C3 C2 C1 122.6(2) . . ? C3 C2 C7 115.3(2) . . ? C1 C2 C7 122.1(2) . . ? C4 C3 C2 119.4(2) . . ? C5 C4 C3 120.1(2) . . ? C5 C4 C8 120.1(2) . . ? C3 C4 C8 119.8(2) . . ? C4 C5 C6 120.7(2) . . ? C5 C6 C1 120.6(2) . . ? C5 C6 C9 112.4(2) . . ? C1 C6 C9 126.9(2) . . ? F2 C7 F3 106.5(2) . . ? F2 C7 F1 106.2(2) . . ? F3 C7 F1 106.8(2) . . ? F2 C7 C2 111.9(2) . . ? F3 C7 C2 112.8(2) . . ? F1 C7 C2 112.2(2) . . ? F4' C8 F5' 99(2) . . ? F4' C8 F5 54.4(4) . . ? F5' C8 F5 130(2) . . ? F4' C8 F6 54.6(4) . . ? F5' C8 F6 54.1(4) . . ? F5 C8 F6 107.8(3) . . ? F4' C8 F6' 99(2) . . ? F5' C8 F6' 99(2) . . ? F5 C8 F6' 53.9(4) . . ? F6 C8 F6' 130(2) . . ? F4' C8 F4 129(2) . . ? F5' C8 F4 54.0(4) . . ? F5 C8 F4 106.3(2) . . ? F6 C8 F4 106.7(3) . . ? F6' C8 F4 53.8(4) . . ? F4' C8 C4 120(2) . . ? F5' C8 C4 118(2) . . ? F5 C8 C4 112.2(2) . . ? F6 C8 C4 111.7(2) . . ? F6' C8 C4 118(2) . . ? F4 C8 C4 111.8(2) . . ? F9 C9 F8 106.4(2) . . ? F9 C9 F7 107.5(2) . . ? F8 C9 F7 106.4(2) . . ? F9 C9 C6 114.7(2) . . ? F8 C9 C6 110.2(2) . . ? F7 C9 C6 111.1(2) . . ? C11 P2 Br3 103.22(8) . . ? C11 P2 Br4 102.41(8) . . ? Br3 P2 Br4 104.90(3) . . ? C12 C11 C16 116.7(2) . . ? C12 C11 P2 130.54(18) . . ? C16 C11 P2 112.55(18) . . ? C13 C12 C11 120.9(2) . . ? C13 C12 C17 113.0(2) . . ? C11 C12 C17 126.0(2) . . ? C14 C13 C12 120.4(2) . . ? C15 C14 C13 120.6(2) . . ? C15 C14 C18 120.8(2) . . ? C13 C14 C18 118.6(2) . . ? C14 C15 C16 119.5(2) . . ? C15 C16 C11 121.8(2) . . ? C15 C16 C19 115.9(2) . . ? C11 C16 C19 122.4(2) . . ? F13 C17 F12 106.8(2) . . ? F13 C17 F11 107.7(2) . . ? F12 C17 F11 105.7(2) . . ? F13 C17 C12 114.1(2) . . ? F12 C17 C12 111.1(2) . . ? F11 C17 C12 110.9(2) . . ? F15' C18 F16' 108.3(7) . . ? F15' C18 F14' 105.1(8) . . ? F16' C18 F14' 103.2(8) . . ? F15' C18 F14 56.4(4) . . ? F16' C18 F14 54.8(3) . . ? F14' C18 F14 130.1(9) . . ? F15' C18 F15 137.0(9) . . ? F16' C18 F15 54.8(3) . . ? F14' C18 F15 53.5(3) . . ? F14 C18 F15 105.7(3) . . ? F15' C18 F16 56.0(3) . . ? F16' C18 F16 135.0(9) . . ? F14' C18 F16 53.7(3) . . ? F14 C18 F16 107.2(3) . . ? F15 C18 F16 105.2(3) . . ? F15' C18 C14 110.7(9) . . ? F16' C18 C14 112.5(9) . . ? F14' C18 C14 116.3(9) . . ? F14 C18 C14 113.5(2) . . ? F15 C18 C14 112.2(2) . . ? F16 C18 C14 112.5(3) . . ? F19 C19 F18 106.0(2) . . ? F19 C19 F17 106.5(2) . . ? F18 C19 F17 106.9(2) . . ? F19 C19 C16 111.9(2) . . ? F18 C19 C16 113.6(2) . . ? F17 C19 C16 111.5(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.790 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.114 #======================================================END data_2 _database_code_CSD 189701 _chemical_name_systematic ; Chloro-bis-(2,4,6-tris-trifluoromethyl-phenyl)-phosphane ; _chemical_name_common 'Symmetric phosphorous chloride' _chemical_melting_point ? _chemical_formula_moiety 'C18 H4 Cl F18 P' _chemical_formula_sum 'C18 H4 Cl F18 P' _chemical_formula_weight 628.63 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.0347(6) _cell_length_b 8.5325(6) _cell_length_c 29.833(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.572(2) _cell_angle_gamma 90.00 _cell_volume 2038.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4354 _cell_measurement_theta_min 4.966 _cell_measurement_theta_max 54.826 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.956 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered over half a sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (40 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.53 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% . _diffrn_reflns_number 14831 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4678 _reflns_number_gt 3233 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SMART-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0447P)^2^+1.7213P] 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 4678 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Cl1 Cl 0.46529(9) 0.30914(8) 0.10311(2) 0.02428(17) Uani 1 1 d . . . P1 P 0.29447(9) 0.47186(9) 0.12207(2) 0.01659(16) Uani 1 1 d . . . C11 C 0.2747(3) 0.6130(3) 0.07346(9) 0.0150(5) Uani 1 1 d . . . C12 C 0.2544(3) 0.5560(3) 0.02866(9) 0.0149(5) Uani 1 1 d . . . C13 C 0.2463(3) 0.6575(3) -0.00793(9) 0.0161(6) Uani 1 1 d . . . H13A H 0.2395 0.6171 -0.0370 0.019 Uiso 1 1 calc R . . C14 C 0.2483(3) 0.8179(3) -0.00150(9) 0.0175(6) Uani 1 1 d . . . C15 C 0.2498(3) 0.8777(3) 0.04168(9) 0.0187(6) Uani 1 1 d . . . H15A H 0.2438 0.9854 0.0461 0.022 Uiso 1 1 calc R . . C16 C 0.2602(3) 0.7767(3) 0.07840(9) 0.0172(6) Uani 1 1 d . . . C17 C 0.2245(3) 0.3856(3) 0.01539(9) 0.0172(6) Uani 1 1 d . . . F11 F 0.1227(2) 0.37766(19) -0.02251(5) 0.0205(4) Uani 1 1 d . . . F12 F 0.1489(2) 0.30406(19) 0.04646(5) 0.0205(4) Uani 1 1 d . . . F13 F 0.3635(2) 0.30809(19) 0.00668(5) 0.0216(4) Uani 1 1 d . . . C18 C 0.2387(4) 0.9277(3) -0.04126(10) 0.0198(6) Uani 1 1 d . . . F14 F 0.3885(2) 0.9912(2) -0.04718(6) 0.0323(5) Uani 1 1 d . . . F15 F 0.1344(2) 1.0467(2) -0.03562(6) 0.0288(4) Uani 1 1 d . . . F16 F 0.1874(2) 0.8563(2) -0.07957(6) 0.0314(4) Uani 1 1 d . . . C19 C 0.2528(4) 0.8565(3) 0.12321(10) 0.0216(6) Uani 1 1 d . . . F17 F 0.1654(2) 0.9902(2) 0.11981(6) 0.0305(4) Uani 1 1 d . . . F18 F 0.4035(2) 0.8940(2) 0.14268(6) 0.0273(4) Uani 1 1 d . . . F19 F 0.1774(2) 0.7659(2) 0.15256(5) 0.0253(4) Uani 1 1 d . . . C21 C 0.4432(3) 0.5530(3) 0.16841(9) 0.0166(6) Uani 1 1 d . . . C22 C 0.6044(3) 0.6132(3) 0.16618(9) 0.0166(6) Uani 1 1 d . . . C23 C 0.7055(4) 0.6496(3) 0.20506(9) 0.0188(6) Uani 1 1 d . . . H23A H 0.8111 0.6920 0.2027 0.023 Uiso 1 1 calc R . . C24 C 0.6500(4) 0.6232(3) 0.24682(9) 0.0192(6) Uani 1 1 d . . . C25 C 0.4928(4) 0.5609(3) 0.25046(9) 0.0187(6) Uani 1 1 d . . . H25A H 0.4558 0.5418 0.2787 0.022 Uiso 1 1 calc R . . C26 C 0.3902(3) 0.5267(3) 0.21212(9) 0.0183(6) Uani 1 1 d . . . C27 C 0.6954(4) 0.6392(3) 0.12383(10) 0.0206(6) Uani 1 1 d . . . F21 F 0.8129(2) 0.5303(2) 0.12036(6) 0.0313(4) Uani 1 1 d . . . F22 F 0.7762(2) 0.7769(2) 0.12590(6) 0.0366(5) Uani 1 1 d . . . F23 F 0.6002(2) 0.6391(2) 0.08565(5) 0.0282(4) Uani 1 1 d . . . C28 C 0.7583(4) 0.6585(4) 0.28905(10) 0.0240(7) Uani 1 1 d . . . F24 F 0.7738(4) 0.5386(3) 0.31619(8) 0.0690(9) Uani 1 1 d . . . F25 F 0.9112(3) 0.7026(3) 0.28099(7) 0.0590(7) Uani 1 1 d . . . F26 F 0.6992(3) 0.7762(3) 0.31169(8) 0.0657(8) Uani 1 1 d . . . C29 C 0.2252(4) 0.4485(4) 0.21998(10) 0.0235(6) Uani 1 1 d . . . F27 F 0.2021(2) 0.4378(3) 0.26380(6) 0.0361(5) Uani 1 1 d . . . F28 F 0.0919(2) 0.5236(2) 0.20103(6) 0.0305(4) Uani 1 1 d . . . F29 F 0.2193(2) 0.3005(2) 0.20408(6) 0.0312(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0299(4) 0.0215(4) 0.0206(4) -0.0024(3) -0.0032(3) 0.0085(3) P1 0.0186(4) 0.0173(3) 0.0138(3) 0.0008(3) 0.0006(3) 0.0002(3) C11 0.0114(13) 0.0181(13) 0.0151(13) 0.0003(11) -0.0004(10) 0.0010(10) C12 0.0108(12) 0.0165(13) 0.0177(14) -0.0008(11) 0.0019(10) -0.0002(10) C13 0.0118(13) 0.0220(14) 0.0145(13) -0.0009(11) 0.0010(11) 0.0000(11) C14 0.0149(13) 0.0184(14) 0.0192(14) 0.0013(11) 0.0018(11) 0.0017(11) C15 0.0162(14) 0.0163(14) 0.0236(15) -0.0013(11) 0.0013(12) -0.0001(11) C16 0.0137(13) 0.0179(14) 0.0197(14) -0.0018(11) 0.0004(11) 0.0008(11) C17 0.0163(14) 0.0191(14) 0.0161(13) 0.0009(11) 0.0014(11) 0.0017(11) F11 0.0229(9) 0.0207(8) 0.0171(8) -0.0033(7) -0.0034(7) -0.0026(7) F12 0.0229(9) 0.0198(8) 0.0189(8) 0.0020(7) 0.0022(7) -0.0051(7) F13 0.0203(9) 0.0204(8) 0.0242(9) -0.0033(7) 0.0021(7) 0.0045(7) C18 0.0200(15) 0.0179(14) 0.0217(15) 0.0020(12) 0.0026(12) 0.0028(11) F14 0.0249(10) 0.0354(11) 0.0374(11) 0.0152(8) 0.0067(8) -0.0047(8) F15 0.0348(10) 0.0232(9) 0.0290(10) 0.0080(8) 0.0070(8) 0.0115(8) F16 0.0500(12) 0.0264(9) 0.0170(9) 0.0032(7) -0.0016(8) 0.0011(9) C19 0.0260(16) 0.0180(14) 0.0207(15) -0.0028(12) 0.0004(13) 0.0050(12) F17 0.0451(11) 0.0226(9) 0.0235(9) -0.0038(7) 0.0003(8) 0.0164(8) F18 0.0313(10) 0.0253(9) 0.0237(9) -0.0053(7) -0.0069(8) -0.0033(8) F19 0.0299(10) 0.0275(9) 0.0193(9) -0.0002(7) 0.0061(7) 0.0044(8) C21 0.0181(14) 0.0166(13) 0.0150(13) 0.0017(11) -0.0001(11) 0.0052(11) C22 0.0182(14) 0.0165(13) 0.0155(13) 0.0016(11) 0.0045(11) 0.0013(11) C23 0.0168(14) 0.0178(14) 0.0216(15) 0.0005(11) 0.0000(11) 0.0002(11) C24 0.0249(15) 0.0137(13) 0.0182(14) 0.0004(11) -0.0025(12) 0.0031(11) C25 0.0239(15) 0.0174(14) 0.0150(13) 0.0004(11) 0.0022(11) 0.0038(12) C26 0.0180(14) 0.0182(14) 0.0190(14) 0.0026(11) 0.0035(11) 0.0021(11) C27 0.0164(14) 0.0240(15) 0.0213(15) 0.0035(12) 0.0008(12) 0.0008(12) F21 0.0243(9) 0.0462(11) 0.0245(9) 0.0055(9) 0.0080(8) 0.0136(9) F22 0.0439(12) 0.0362(11) 0.0312(10) 0.0009(9) 0.0126(9) -0.0186(9) F23 0.0186(9) 0.0500(12) 0.0159(8) 0.0067(8) 0.0015(7) -0.0020(8) C28 0.0301(17) 0.0223(15) 0.0187(14) -0.0006(12) -0.0033(13) -0.0009(13) F24 0.104(2) 0.0419(13) 0.0515(14) 0.0259(11) -0.0517(15) -0.0286(13) F25 0.0406(13) 0.104(2) 0.0305(11) -0.0071(12) -0.0075(10) -0.0282(13) F26 0.0678(17) 0.0721(17) 0.0526(15) -0.0422(13) -0.0245(13) 0.0257(14) C29 0.0246(16) 0.0299(17) 0.0165(14) 0.0043(12) 0.0054(12) -0.0031(13) F27 0.0344(11) 0.0574(13) 0.0178(9) 0.0072(9) 0.0089(8) -0.0098(10) F28 0.0183(9) 0.0428(11) 0.0308(10) 0.0060(8) 0.0047(8) 0.0010(8) F29 0.0336(10) 0.0268(10) 0.0337(10) 0.0054(8) 0.0062(8) -0.0092(8) _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 Cl1 P1 2.0628(10) . ? P1 C11 1.882(3) . ? P1 C21 1.885(3) . ? C11 C16 1.411(4) . ? C11 C12 1.420(4) . ? C12 C13 1.391(4) . ? C12 C17 1.521(4) . ? C13 C14 1.382(4) . ? C13 H13A 0.9300 . ? C14 C15 1.385(4) . ? C14 C18 1.509(4) . ? C15 C16 1.391(4) . ? C15 H15A 0.9300 . ? C16 C19 1.506(4) . ? C17 F13 1.341(3) . ? C17 F12 1.342(3) . ? C17 F11 1.343(3) . ? C18 F16 1.331(3) . ? C18 F15 1.336(3) . ? C18 F14 1.345(3) . ? C19 F17 1.339(3) . ? C19 F18 1.339(3) . ? C19 F19 1.347(3) . ? C21 C22 1.400(4) . ? C21 C26 1.421(4) . ? C22 C23 1.397(4) . ? C22 C27 1.526(4) . ? C23 C24 1.375(4) . ? C23 H23A 0.9300 . ? C24 C25 1.383(4) . ? C24 C28 1.504(4) . ? C25 C26 1.387(4) . ? C25 H25A 0.9300 . ? C26 C29 1.518(4) . ? C27 F23 1.321(3) . ? C27 F21 1.334(3) . ? C27 F22 1.341(3) . ? C28 F24 1.305(4) . ? C28 F26 1.319(4) . ? C28 F25 1.324(4) . ? C29 F28 1.335(3) . ? C29 F27 1.338(3) . ? C29 F29 1.349(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 P1 C21 109.87(12) . . ? C11 P1 Cl1 103.68(9) . . ? C21 P1 Cl1 92.95(9) . . ? C16 C11 C12 115.7(2) . . ? C16 C11 P1 123.8(2) . . ? C12 C11 P1 120.2(2) . . ? C13 C12 C11 121.3(2) . . ? C13 C12 C17 113.3(2) . . ? C11 C12 C17 125.2(2) . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 C18 120.4(3) . . ? C15 C14 C18 119.9(3) . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C11 122.1(3) . . ? C15 C16 C19 114.5(2) . . ? C11 C16 C19 123.4(3) . . ? F13 C17 F12 107.9(2) . . ? F13 C17 F11 105.8(2) . . ? F12 C17 F11 106.0(2) . . ? F13 C17 C12 113.9(2) . . ? F12 C17 C12 112.7(2) . . ? F11 C17 C12 109.9(2) . . ? F16 C18 F15 107.6(2) . . ? F16 C18 F14 106.9(2) . . ? F15 C18 F14 106.7(2) . . ? F16 C18 C14 112.6(2) . . ? F15 C18 C14 111.5(2) . . ? F14 C18 C14 111.3(2) . . ? F17 C19 F18 106.3(2) . . ? F17 C19 F19 106.1(2) . . ? F18 C19 F19 107.0(2) . . ? F17 C19 C16 112.1(2) . . ? F18 C19 C16 113.2(2) . . ? F19 C19 C16 111.7(2) . . ? C22 C21 C26 116.6(2) . . ? C22 C21 P1 129.4(2) . . ? C26 C21 P1 113.3(2) . . ? C23 C22 C21 121.4(3) . . ? C23 C22 C27 111.7(2) . . ? C21 C22 C27 126.8(2) . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 C28 121.2(3) . . ? C25 C24 C28 118.9(3) . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 121.4(3) . . ? C25 C26 C29 115.7(2) . . ? C21 C26 C29 122.7(2) . . ? F23 C27 F21 107.3(2) . . ? F23 C27 F22 106.6(2) . . ? F21 C27 F22 105.7(2) . . ? F23 C27 C22 115.5(2) . . ? F21 C27 C22 110.6(2) . . ? F22 C27 C22 110.6(2) . . ? F24 C28 F26 107.4(3) . . ? F24 C28 F25 107.0(3) . . ? F26 C28 F25 104.7(3) . . ? F24 C28 C24 112.5(2) . . ? F26 C28 C24 111.9(3) . . ? F25 C28 C24 112.8(3) . . ? F28 C29 F27 106.1(2) . . ? F28 C29 F29 107.2(2) . . ? F27 C29 F29 106.0(2) . . ? F28 C29 C26 113.9(2) . . ? F27 C29 C26 111.8(2) . . ? F29 C29 C26 111.3(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.750 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.080 #======================================================END data_3 _database_code_CSD 189702 _audit_creation_method SHELXL-97 _chemical_name_systematic ; chloro-bis-(2,4-bis-(trifluoromethyl)-phenyl)-phosphane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H6 Cl F12 P' _chemical_formula_weight 492.63 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 18.734(6) _cell_length_b 8.170(3) _cell_length_c 23.559(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.820(5) _cell_angle_gamma 90.00 _cell_volume 3580.2(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 739 _cell_measurement_theta_min 10.17 _cell_measurement_theta_max 20.99 _exptl_crystal_description 'irregular' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20573 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.70 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 4618 _reflns_number_gt 3420 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SMART version 5.054 (Bruker, 1998)' _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. ; _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^)+(0.0528P)^2^+5.4664P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4618 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.740 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.074 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 Cl1 Cl -0.01608(3) 0.28581(7) 0.24125(2) 0.02290(14) Uani 1 1 d . . . P1 P 0.03564(3) 0.38742(7) 0.17721(2) 0.01765(14) Uani 1 1 d . . . C1 C -0.02130(11) 0.2944(3) 0.11589(9) 0.0171(4) Uani 1 1 d . . . C2 C -0.01632(13) 0.1288(3) 0.10295(10) 0.0224(5) Uani 1 1 d . . . H2 H 0.0166(13) 0.059(3) 0.1240(10) 0.015(6) Uiso 1 1 d . . . C3 C -0.05792(14) 0.0601(3) 0.05648(10) 0.0244(5) Uani 1 1 d . . . H3 H -0.0508(16) -0.050(4) 0.0461(13) 0.039(8) Uiso 1 1 d . . . C4 C -0.10669(13) 0.1570(3) 0.02283(9) 0.0226(5) Uani 1 1 d . . . C41 C -0.14954(15) 0.0846(3) -0.02936(11) 0.0313(6) Uani 1 1 d . . . F1 F -0.16867(14) -0.0680(2) -0.02129(9) 0.0757(8) Uani 1 1 d . . . F2 F -0.20911(8) 0.1681(2) -0.04636(6) 0.0372(4) Uani 1 1 d . . . F3 F -0.11194(10) 0.0872(3) -0.07441(7) 0.0557(6) Uani 1 1 d . . . C5 C -0.11460(13) 0.3210(3) 0.03551(10) 0.0205(5) Uani 1 1 d . . . H5 H -0.1464(15) 0.383(3) 0.0157(12) 0.025(7) Uiso 1 1 d . . . C6 C -0.07166(12) 0.3900(3) 0.08148(9) 0.0184(4) Uani 1 1 d . . . C61 C -0.08118(13) 0.5691(3) 0.09352(10) 0.0226(5) Uani 1 1 d . . . F4 F -0.09852(9) 0.59513(18) 0.14649(6) 0.0325(4) Uani 1 1 d . . . F5 F -0.02148(8) 0.65638(17) 0.08906(7) 0.0349(4) Uani 1 1 d . . . F6 F -0.13350(8) 0.63805(17) 0.05763(6) 0.0310(3) Uani 1 1 d . . . C11 C 0.11642(12) 0.2546(3) 0.18007(9) 0.0168(4) Uani 1 1 d . . . C12 C 0.12616(13) 0.1204(3) 0.21646(10) 0.0215(5) Uani 1 1 d . . . H12 H 0.0909(15) 0.089(3) 0.2355(11) 0.022(7) Uiso 1 1 d . . . C13 C 0.18791(13) 0.0259(3) 0.22049(10) 0.0231(5) Uani 1 1 d . . . H13 H 0.1943(15) -0.065(4) 0.2464(12) 0.030(7) Uiso 1 1 d . . . C14 C 0.24203(12) 0.0652(3) 0.18789(9) 0.0202(5) Uani 1 1 d . . . C141 C 0.30881(12) -0.0376(3) 0.19095(10) 0.0244(5) Uani 1 1 d . . . F7 F 0.30333(10) -0.1574(2) 0.15334(9) 0.0600(6) Uani 1 1 d . . . F8 F 0.36679(8) 0.0486(2) 0.18401(10) 0.0531(5) Uani 1 1 d . . . F9 F 0.32405(10) -0.1090(2) 0.24208(8) 0.0512(5) Uani 1 1 d . . . C15 C 0.23475(13) 0.1994(3) 0.15162(10) 0.0213(5) Uani 1 1 d . . . H15 H 0.2705(14) 0.231(3) 0.1284(11) 0.017(6) Uiso 1 1 d . . . C16 C 0.17260(12) 0.2935(3) 0.14793(9) 0.0194(4) Uani 1 1 d . . . C161 C 0.16910(14) 0.4409(3) 0.10922(11) 0.0290(5) Uani 1 1 d . . . F10 F 0.10548(8) 0.4537(2) 0.07743(7) 0.0455(5) Uani 1 1 d . . . F11 F 0.17845(13) 0.5797(2) 0.13857(8) 0.0609(6) Uani 1 1 d . . . F12 F 0.21791(9) 0.4377(2) 0.07277(7) 0.0438(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0208(3) 0.0289(3) 0.0196(3) 0.0004(2) 0.0046(2) 0.0025(2) P1 0.0179(3) 0.0160(3) 0.0185(3) -0.0002(2) -0.0001(2) 0.0013(2) C1 0.0161(10) 0.0191(10) 0.0159(10) -0.0004(8) 0.0008(8) -0.0014(8) C2 0.0257(12) 0.0198(11) 0.0209(11) 0.0024(9) -0.0002(9) 0.0049(10) C3 0.0294(13) 0.0196(11) 0.0232(11) -0.0020(9) -0.0010(10) 0.0009(10) C4 0.0239(12) 0.0262(12) 0.0170(10) -0.0007(9) 0.0000(9) -0.0018(10) C41 0.0345(15) 0.0304(14) 0.0271(13) -0.0040(10) -0.0047(11) 0.0007(11) F1 0.119(2) 0.0334(10) 0.0595(13) 0.0030(9) -0.0541(13) -0.0230(11) F2 0.0282(8) 0.0544(10) 0.0267(8) -0.0050(7) -0.0066(6) 0.0025(7) F3 0.0391(10) 0.0980(16) 0.0291(9) -0.0281(9) 0.0010(7) 0.0111(10) C5 0.0190(11) 0.0242(12) 0.0178(10) 0.0046(9) -0.0006(9) 0.0035(9) C6 0.0179(10) 0.0194(10) 0.0184(10) 0.0016(8) 0.0041(8) 0.0012(9) C61 0.0201(11) 0.0222(11) 0.0243(11) 0.0020(9) -0.0018(9) 0.0046(9) F4 0.0412(9) 0.0287(8) 0.0270(7) -0.0057(6) 0.0009(6) 0.0121(7) F5 0.0292(8) 0.0183(7) 0.0560(10) 0.0071(7) 0.0005(7) -0.0001(6) F6 0.0314(8) 0.0251(7) 0.0339(8) 0.0029(6) -0.0067(6) 0.0118(6) C11 0.0156(10) 0.0165(10) 0.0176(10) -0.0007(8) -0.0008(8) 0.0008(8) C12 0.0200(11) 0.0225(11) 0.0225(11) 0.0036(9) 0.0044(9) -0.0013(9) C13 0.0235(12) 0.0194(11) 0.0257(12) 0.0061(9) 0.0003(9) 0.0020(9) C14 0.0167(11) 0.0209(11) 0.0219(11) -0.0028(9) -0.0018(9) 0.0018(9) C141 0.0181(11) 0.0266(12) 0.0277(12) -0.0029(10) -0.0014(9) 0.0017(9) F7 0.0421(11) 0.0598(12) 0.0711(13) -0.0433(10) -0.0231(9) 0.0263(9) F8 0.0203(8) 0.0409(10) 0.0996(16) 0.0118(10) 0.0129(9) 0.0054(7) F9 0.0407(10) 0.0696(13) 0.0428(10) 0.0168(9) 0.0031(8) 0.0298(9) C15 0.0184(11) 0.0245(12) 0.0210(11) 0.0008(9) 0.0027(9) -0.0026(9) C16 0.0204(11) 0.0193(11) 0.0182(10) 0.0020(8) 0.0014(8) -0.0010(9) C161 0.0274(13) 0.0314(13) 0.0295(13) 0.0134(11) 0.0087(10) 0.0033(10) F10 0.0255(8) 0.0637(12) 0.0475(10) 0.0376(9) 0.0058(7) 0.0120(8) F11 0.1098(18) 0.0230(9) 0.0519(11) 0.0093(8) 0.0176(11) -0.0113(10) F12 0.0332(9) 0.0572(11) 0.0447(10) 0.0307(8) 0.0202(7) 0.0106(8) _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 Cl1 P1 2.0619(9) . ? P1 C1 1.854(2) . ? P1 C11 1.857(2) . ? C1 C2 1.393(3) . ? C1 C6 1.405(3) . ? C2 C3 1.385(3) . ? C2 H2 0.94(2) . ? C3 C4 1.385(3) . ? C3 H3 0.95(3) . ? C4 C5 1.385(3) . ? C4 C41 1.507(3) . ? C41 F1 1.317(3) . ? C41 F2 1.329(3) . ? C41 F3 1.342(3) . ? C5 C6 1.390(3) . ? C5 H5 0.87(3) . ? C6 C61 1.505(3) . ? C61 F6 1.340(3) . ? C61 F5 1.341(3) . ? C61 F4 1.343(3) . ? C11 C12 1.391(3) . ? C11 C16 1.404(3) . ? C12 C13 1.384(3) . ? C12 H12 0.88(3) . ? C13 C14 1.381(3) . ? C13 H13 0.96(3) . ? C14 C15 1.386(3) . ? C14 C141 1.502(3) . ? C141 F7 1.316(3) . ? C141 F8 1.321(3) . ? C141 F9 1.338(3) . ? C15 C16 1.389(3) . ? C15 H15 0.95(3) . ? C16 C161 1.507(3) . ? C161 F12 1.327(3) . ? C161 F11 1.329(3) . ? C161 F10 1.334(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C11 100.37(10) . . ? C1 P1 Cl1 97.38(7) . . ? C11 P1 Cl1 100.95(7) . . ? C2 C1 C6 118.1(2) . . ? C2 C1 P1 121.43(17) . . ? C6 C1 P1 120.44(16) . . ? C3 C2 C1 121.4(2) . . ? C3 C2 H2 116.3(15) . . ? C1 C2 H2 122.3(15) . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 120.0(18) . . ? C2 C3 H3 120.4(18) . . ? C5 C4 C3 120.7(2) . . ? C5 C4 C41 119.7(2) . . ? C3 C4 C41 119.6(2) . . ? F1 C41 F2 107.2(2) . . ? F1 C41 F3 107.9(2) . . ? F2 C41 F3 104.7(2) . . ? F1 C41 C4 112.4(2) . . ? F2 C41 C4 113.1(2) . . ? F3 C41 C4 111.1(2) . . ? C4 C5 C6 119.6(2) . . ? C4 C5 H5 121.8(18) . . ? C6 C5 H5 118.6(18) . . ? C5 C6 C1 120.7(2) . . ? C5 C6 C61 118.1(2) . . ? C1 C6 C61 121.2(2) . . ? F6 C61 F5 106.35(18) . . ? F6 C61 F4 106.28(18) . . ? F5 C61 F4 106.53(19) . . ? F6 C61 C6 112.57(19) . . ? F5 C61 C6 112.54(19) . . ? F4 C61 C6 112.10(19) . . ? C12 C11 C16 117.3(2) . . ? C12 C11 P1 122.00(17) . . ? C16 C11 P1 120.55(16) . . ? C13 C12 C11 122.0(2) . . ? C13 C12 H12 118.4(17) . . ? C11 C12 H12 119.5(17) . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 119.2(17) . . ? C12 C13 H13 121.1(17) . . ? C13 C14 C15 120.1(2) . . ? C13 C14 C141 120.4(2) . . ? C15 C14 C141 119.5(2) . . ? F7 C141 F8 108.2(2) . . ? F7 C141 F9 105.8(2) . . ? F8 C141 F9 104.7(2) . . ? F7 C141 C14 112.69(19) . . ? F8 C141 C14 112.9(2) . . ? F9 C141 C14 112.0(2) . . ? C14 C15 C16 119.8(2) . . ? C14 C15 H15 123.1(15) . . ? C16 C15 H15 117.1(15) . . ? C15 C16 C11 121.2(2) . . ? C15 C16 C161 117.1(2) . . ? C11 C16 C161 121.7(2) . . ? F12 C161 F11 107.2(2) . . ? F12 C161 F10 106.1(2) . . ? F11 C161 F10 106.2(2) . . ? F12 C161 C16 113.1(2) . . ? F11 C161 C16 111.9(2) . . ? F10 C161 C16 112.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 P1 C1 C2 29.7(2) . . . . ? Cl1 P1 C1 C2 -72.92(19) . . . . ? C11 P1 C1 C6 -151.14(18) . . . . ? Cl1 P1 C1 C6 106.24(17) . . . . ? C6 C1 C2 C3 2.1(3) . . . . ? P1 C1 C2 C3 -178.77(19) . . . . ? C1 C2 C3 C4 -1.5(4) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C2 C3 C4 C41 177.1(2) . . . . ? C5 C4 C41 F1 -145.0(3) . . . . ? C3 C4 C41 F1 37.3(4) . . . . ? C5 C4 C41 F2 -23.4(3) . . . . ? C3 C4 C41 F2 158.8(2) . . . . ? C5 C4 C41 F3 94.0(3) . . . . ? C3 C4 C41 F3 -83.7(3) . . . . ? C3 C4 C5 C6 1.9(3) . . . . ? C41 C4 C5 C6 -175.8(2) . . . . ? C4 C5 C6 C1 -1.3(3) . . . . ? C4 C5 C6 C61 179.3(2) . . . . ? C2 C1 C6 C5 -0.7(3) . . . . ? P1 C1 C6 C5 -179.87(17) . . . . ? C2 C1 C6 C61 178.8(2) . . . . ? P1 C1 C6 C61 -0.4(3) . . . . ? C5 C6 C61 F6 1.9(3) . . . . ? C1 C6 C61 F6 -177.51(19) . . . . ? C5 C6 C61 F5 -118.2(2) . . . . ? C1 C6 C61 F5 62.3(3) . . . . ? C5 C6 C61 F4 121.7(2) . . . . ? C1 C6 C61 F4 -57.8(3) . . . . ? C1 P1 C11 C12 -95.7(2) . . . . ? Cl1 P1 C11 C12 4.0(2) . . . . ? C1 P1 C11 C16 88.63(19) . . . . ? Cl1 P1 C11 C16 -171.68(17) . . . . ? C16 C11 C12 C13 -1.2(3) . . . . ? P1 C11 C12 C13 -176.95(18) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C12 C13 C14 C15 0.5(4) . . . . ? C12 C13 C14 C141 -178.9(2) . . . . ? C13 C14 C141 F7 90.2(3) . . . . ? C15 C14 C141 F7 -89.2(3) . . . . ? C13 C14 C141 F8 -146.8(2) . . . . ? C15 C14 C141 F8 33.8(3) . . . . ? C13 C14 C141 F9 -29.0(3) . . . . ? C15 C14 C141 F9 151.6(2) . . . . ? C13 C14 C15 C16 -0.4(3) . . . . ? C141 C14 C15 C16 179.0(2) . . . . ? C14 C15 C16 C11 -0.5(3) . . . . ? C14 C15 C16 C161 178.0(2) . . . . ? C12 C11 C16 C15 1.2(3) . . . . ? P1 C11 C16 C15 177.08(17) . . . . ? C12 C11 C16 C161 -177.2(2) . . . . ? P1 C11 C16 C161 -1.3(3) . . . . ? C15 C16 C161 F12 16.3(3) . . . . ? C11 C16 C161 F12 -165.2(2) . . . . ? C15 C16 C161 F11 -104.9(3) . . . . ? C11 C16 C161 F11 73.6(3) . . . . ? C15 C16 C161 F10 136.0(2) . . . . ? C11 C16 C161 F10 -45.5(3) . . . . ? #======================================================END data_4 _database_code_CSD 189703 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bromo-bis-(2,4-bis-(trifluoromethyl)-phenyl)-phosphane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H6 Br F12 P' _chemical_formula_weight 537.09 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 19.0725(13) _cell_length_b 8.2148(6) _cell_length_c 23.6350(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.447(4) _cell_angle_gamma 90.00 _cell_volume 3671.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 26.2 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.75 _exptl_crystal_density_meas Not_measured _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 2.444 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.3080 _exptl_absorpt_correction_T_max 0.4851 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997), R(int)=0.064 before correction' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.2000 0.00 0.00 -1.00 0.2000 0.00 1.00 -1.00 0.2500 0.00 -1.00 1.00 0.2500 3.00 0.00 1.00 0.2200 -1.00 0.00 1.00 0.2200 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21699 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 29.00 _reflns_number_total 4879 _reflns_number_gt 4504 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SMART version 5.054 (Bruker, 1998)' _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. One CF~3~ group is rotationally disordered, atoms F(7), F(8) and F(9) occupy two sets of positions, with occupancies 0.9 (A) and 0.1 (B). Atoms in opposite (major and minor) positions were refined with equivalent anisotropic ADP. ; _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^)+(0.0350P)^2^+7.0547P] 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 4879 _refine_ls_number_parameters 280 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.044 _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 Br1 Br 0.483140(9) 0.28393(2) 0.245591(7) 0.02160(6) Uani 1 1 d . . . P1 P 0.53737(2) 0.38906(5) 0.175654(18) 0.01748(9) Uani 1 1 d . . . C1 C 0.47996(9) 0.2933(2) 0.11526(7) 0.0181(3) Uani 1 1 d . . . C2 C 0.48613(10) 0.1283(2) 0.10228(8) 0.0227(3) Uani 1 1 d . . . H2 H 0.5197 0.0631 0.1253 0.027 Uiso 1 1 d R . . C3 C 0.44413(10) 0.0578(2) 0.05630(8) 0.0256(4) Uani 1 1 d . . . H3 H 0.4496 -0.0540 0.0476 0.031 Uiso 1 1 d R . . C4 C 0.39408(10) 0.1520(2) 0.02316(8) 0.0243(3) Uani 1 1 d . . . C41 C 0.35088(12) 0.0786(3) -0.02840(9) 0.0342(5) Uani 1 1 d . . . F1 F 0.33254(14) -0.0733(2) -0.01960(9) 0.0896(8) Uani 1 1 d . . . F2 F 0.29172(7) 0.16018(19) -0.04537(6) 0.0402(3) Uani 1 1 d . . . F3 F 0.38654(8) 0.0812(3) -0.07380(7) 0.0642(5) Uani 1 1 d . . . C5 C 0.38538(10) 0.3153(2) 0.03589(8) 0.0226(3) Uani 1 1 d . . . H5 H 0.3502 0.3784 0.0137 0.027 Uiso 1 1 d R . . C6 C 0.42840(9) 0.3858(2) 0.08122(7) 0.0192(3) Uani 1 1 d . . . C61 C 0.41773(10) 0.5641(2) 0.09324(8) 0.0249(4) Uani 1 1 d . . . F4 F 0.40168(7) 0.58892(15) 0.14629(5) 0.0340(3) Uani 1 1 d . . . F5 F 0.47547(7) 0.65340(15) 0.08823(6) 0.0376(3) Uani 1 1 d . . . F6 F 0.36478(7) 0.63006(15) 0.05768(5) 0.0336(3) Uani 1 1 d . . . C11 C 0.61715(9) 0.2577(2) 0.17874(7) 0.0178(3) Uani 1 1 d . . . C12 C 0.62741(9) 0.1229(2) 0.21484(8) 0.0226(3) Uani 1 1 d . . . H12 H 0.5917 0.0945 0.2376 0.027 Uiso 1 1 d R . . C13 C 0.68883(9) 0.0289(2) 0.21831(8) 0.0247(4) Uani 1 1 d . . . H13 H 0.6946 -0.0626 0.2430 0.030 Uiso 1 1 d R . . C14 C 0.74133(9) 0.0701(2) 0.18546(8) 0.0216(3) Uani 1 1 d D A . C141 C 0.80693(10) -0.0332(2) 0.18807(9) 0.0270(4) Uani 1 1 d D . . F7A F 0.79977(10) -0.1572(3) 0.15353(10) 0.0671(7) Uani 0.90 1 d P A 1 F8A F 0.86316(8) 0.0509(2) 0.17896(13) 0.0681(7) Uani 0.90 1 d P A 1 F9A F 0.82511(10) -0.0964(3) 0.24051(8) 0.0592(5) Uani 0.90 1 d P A 1 F7B F 0.8503(8) -0.010(2) 0.2278(8) 0.0671(7) Uani 0.10 1 d PD A 2 F8B F 0.7907(8) -0.1823(16) 0.1866(10) 0.0681(7) Uani 0.10 1 d PD A 2 F9B F 0.8363(8) -0.011(2) 0.1422(6) 0.0592(5) Uani 0.10 1 d PD A 2 C15 C 0.73329(9) 0.2045(2) 0.14978(8) 0.0225(3) Uani 1 1 d . . . H15 H 0.7695 0.2328 0.1275 0.027 Uiso 1 1 d R A . C16 C 0.67194(9) 0.2982(2) 0.14662(7) 0.0205(3) Uani 1 1 d . A . C161 C 0.66725(11) 0.4462(3) 0.10851(9) 0.0307(4) Uani 1 1 d . . . F10 F 0.60471(7) 0.45599(19) 0.07555(6) 0.0441(4) Uani 1 1 d . A . F11 F 0.67437(10) 0.58420(17) 0.13855(7) 0.0552(4) Uani 1 1 d . A . F12 F 0.71630(7) 0.4470(2) 0.07305(7) 0.0467(4) Uani 1 1 d . A . 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 Br1 0.01991(9) 0.02458(10) 0.02082(9) 0.00114(6) 0.00461(6) 0.00212(6) P1 0.01736(19) 0.01553(19) 0.01903(19) 0.00064(15) 0.00035(15) 0.00103(15) C1 0.0176(7) 0.0181(8) 0.0185(7) 0.0011(6) 0.0023(6) 0.0013(6) C2 0.0252(8) 0.0187(8) 0.0231(8) 0.0006(6) -0.0010(7) 0.0027(6) C3 0.0301(9) 0.0199(8) 0.0255(9) -0.0038(7) -0.0013(7) 0.0010(7) C4 0.0262(8) 0.0263(9) 0.0193(8) -0.0022(7) -0.0010(6) -0.0007(7) C41 0.0391(11) 0.0348(11) 0.0258(9) -0.0068(8) -0.0066(8) 0.0013(9) F1 0.1381(19) 0.0347(8) 0.0744(13) 0.0049(8) -0.0679(13) -0.0255(10) F2 0.0298(6) 0.0581(9) 0.0298(6) -0.0082(6) -0.0069(5) 0.0017(6) F3 0.0406(8) 0.1172(16) 0.0332(7) -0.0348(9) -0.0012(6) 0.0148(9) C5 0.0229(8) 0.0258(8) 0.0183(8) 0.0028(6) -0.0002(6) 0.0032(7) C6 0.0197(7) 0.0184(7) 0.0197(8) 0.0018(6) 0.0027(6) 0.0029(6) C61 0.0252(8) 0.0201(8) 0.0280(9) 0.0017(7) -0.0022(7) 0.0062(7) F4 0.0427(7) 0.0299(6) 0.0280(6) -0.0066(5) 0.0001(5) 0.0129(5) F5 0.0321(6) 0.0188(5) 0.0604(9) 0.0074(5) 0.0000(6) -0.0001(5) F6 0.0351(6) 0.0275(6) 0.0346(6) 0.0025(5) -0.0084(5) 0.0142(5) C11 0.0164(7) 0.0182(7) 0.0183(7) 0.0005(6) 0.0000(6) -0.0003(6) C12 0.0195(8) 0.0227(8) 0.0260(8) 0.0066(7) 0.0046(6) 0.0017(6) C13 0.0213(8) 0.0220(8) 0.0306(9) 0.0067(7) 0.0020(7) 0.0032(7) C14 0.0159(7) 0.0236(8) 0.0246(8) -0.0024(7) -0.0003(6) 0.0019(6) C141 0.0201(8) 0.0282(9) 0.0317(10) -0.0041(8) -0.0001(7) 0.0036(7) F7A 0.0431(10) 0.0667(12) 0.0816(14) -0.0525(12) -0.0287(10) 0.0303(9) F8A 0.0203(7) 0.0462(10) 0.141(2) 0.0215(12) 0.0221(10) 0.0072(7) F9A 0.0470(10) 0.0905(15) 0.0395(9) 0.0158(9) 0.0041(7) 0.0436(10) F7B 0.0431(10) 0.0667(12) 0.0816(14) -0.0525(12) -0.0287(10) 0.0303(9) F8B 0.0203(7) 0.0462(10) 0.141(2) 0.0215(12) 0.0221(10) 0.0072(7) F9B 0.0470(10) 0.0905(15) 0.0395(9) 0.0158(9) 0.0041(7) 0.0436(10) C15 0.0181(7) 0.0264(9) 0.0234(8) -0.0010(7) 0.0037(6) -0.0021(6) C16 0.0198(8) 0.0220(8) 0.0194(8) 0.0026(6) 0.0017(6) -0.0015(6) C161 0.0277(9) 0.0324(10) 0.0335(10) 0.0131(8) 0.0092(8) 0.0019(8) F10 0.0293(6) 0.0612(9) 0.0425(7) 0.0322(7) 0.0072(5) 0.0110(6) F11 0.0848(12) 0.0247(7) 0.0582(10) 0.0110(6) 0.0176(9) -0.0074(7) F12 0.0327(7) 0.0625(9) 0.0488(8) 0.0326(7) 0.0205(6) 0.0096(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 P1 2.2340(5) . ? P1 C1 1.8572(18) . ? P1 C11 1.8591(17) . ? C1 C2 1.398(2) . ? C1 C6 1.409(2) . ? C2 C3 1.390(3) . ? C3 C4 1.389(3) . ? C4 C5 1.389(3) . ? C4 C41 1.506(3) . ? C41 F1 1.319(3) . ? C41 F2 1.329(3) . ? C41 F3 1.343(3) . ? C5 C6 1.389(2) . ? C6 C61 1.510(2) . ? C61 F5 1.341(2) . ? C61 F6 1.342(2) . ? C61 F4 1.344(2) . ? C11 C12 1.396(2) . ? C11 C16 1.409(2) . ? C12 C13 1.396(2) . ? C13 C14 1.386(3) . ? C14 C15 1.386(3) . ? C14 C141 1.507(2) . ? C141 F7B 1.183(12) . ? C141 F8B 1.263(14) . ? C141 F9B 1.295(13) . ? C141 F7A 1.301(3) . ? C141 F8A 1.317(3) . ? C141 F9A 1.347(3) . ? C15 C16 1.394(2) . ? C16 C161 1.508(3) . ? C161 F12 1.334(2) . ? C161 F11 1.335(3) . ? C161 F10 1.340(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C11 100.51(8) . . ? C1 P1 Br1 96.99(6) . . ? C11 P1 Br1 101.63(6) . . ? C2 C1 C6 118.01(16) . . ? C2 C1 P1 121.41(13) . . ? C6 C1 P1 120.58(13) . . ? C3 C2 C1 121.26(17) . . ? C4 C3 C2 119.53(17) . . ? C3 C4 C5 120.57(17) . . ? C3 C4 C41 119.78(18) . . ? C5 C4 C41 119.61(17) . . ? F1 C41 F2 107.0(2) . . ? F1 C41 F3 108.3(2) . . ? F2 C41 F3 104.40(18) . . ? F1 C41 C4 112.33(18) . . ? F2 C41 C4 113.33(18) . . ? F3 C41 C4 111.06(19) . . ? C6 C5 C4 119.63(16) . . ? C5 C6 C1 120.97(16) . . ? C5 C6 C61 117.95(16) . . ? C1 C6 C61 121.08(16) . . ? F5 C61 F6 106.47(15) . . ? F5 C61 F4 106.74(16) . . ? F6 C61 F4 106.20(15) . . ? F5 C61 C6 112.44(15) . . ? F6 C61 C6 112.51(16) . . ? F4 C61 C6 112.03(15) . . ? C12 C11 C16 117.50(16) . . ? C12 C11 P1 122.24(13) . . ? C16 C11 P1 120.15(13) . . ? C11 C12 C13 121.63(17) . . ? C14 C13 C12 119.57(17) . . ? C15 C14 C13 120.29(16) . . ? C15 C14 C141 119.97(17) . . ? C13 C14 C141 119.73(17) . . ? F7B C141 F8B 108.7(10) . . ? F7B C141 F9B 107.9(10) . . ? F8B C141 F9B 104.2(9) . . ? F7B C141 F7A 129.0(7) . . ? F8B C141 F7A 38.6(10) . . ? F9B C141 F7A 66.9(9) . . ? F7B C141 F8A 62.9(11) . . ? F8B C141 F8A 135.0(7) . . ? F9B C141 F8A 48.7(9) . . ? F7A C141 F8A 109.2(2) . . ? F7B C141 F9A 42.5(11) . . ? F8B C141 F9A 71.6(10) . . ? F9B C141 F9A 137.4(6) . . ? F7A C141 F9A 105.6(2) . . ? F8A C141 F9A 103.6(2) . . ? F7B C141 C14 115.7(7) . . ? F8B C141 C14 110.3(7) . . ? F9B C141 C14 109.5(6) . . ? F7A C141 C14 113.34(16) . . ? F8A C141 C14 112.78(17) . . ? F9A C141 C14 111.60(17) . . ? C14 C15 C16 119.89(17) . . ? C15 C16 C11 121.10(16) . . ? C15 C16 C161 117.46(16) . . ? C11 C16 C161 121.43(16) . . ? F12 C161 F11 107.36(18) . . ? F12 C161 F10 106.16(17) . . ? F11 C161 F10 106.22(18) . . ? F12 C161 C16 112.77(17) . . ? F11 C161 C16 111.88(17) . . ? F10 C161 C16 112.03(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.728 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.082 #===============================================END data_5 _database_code_CSD 189704 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,4-fluoromethylbenzene-2,5-fluromethylbenzene arsenic chloride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H6 As Cl F12' _chemical_formula_weight 536.4 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' 'Cl' 'Cl' 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 13.436(3) _cell_length_b 9.055(1) _cell_length_c 14.644(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.98(1) _cell_angle_gamma 90.00 _cell_volume 1749.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 623 _cell_measurement_theta_min 11.93 _cell_measurement_theta_max 23.87 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.043 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 2.219 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.471 _exptl_absorpt_correction_T_max 0.717 _exptl_absorpt_process_details 'XPREP (SHELXTL)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 1.00 0.00 0.090 -1.00 -1.00 0.00 0.090 1.00 -1.00 0.00 0.100 -1.00 1.00 0.00 0.100 0.00 0.00 1.00 0.200 0.00 0.00 -1.00 0.200 _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (20 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.60 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% . _diffrn_reflns_number 4335 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.3 _reflns_number_total 4335 _reflns_number_gt 3749 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SMART version 5.054 (Bruker, 1998)' _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. ; _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^)+(0.0353P)^2^+1.1908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4335 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 As1 As 0.756983(13) 0.75080(2) 0.070713(12) 0.01763(6) Uani 1 1 d . . . Cl1 Cl 0.81292(3) 0.96572(5) 0.13072(3) 0.02388(10) Uani 1 1 d . . . F1 F 1.17919(9) 0.64522(17) -0.13245(9) 0.0396(3) Uani 1 1 d . . . F2 F 1.07907(10) 0.48572(14) -0.21169(10) 0.0367(3) Uani 1 1 d . . . F3 F 1.06843(11) 0.71503(16) -0.25040(10) 0.0384(3) Uani 1 1 d . . . F4 F 0.76988(9) 0.36187(13) -0.11458(10) 0.0366(3) Uani 1 1 d . . . F5 F 0.69977(9) 0.49930(13) -0.02399(8) 0.0278(3) Uani 1 1 d . . . F6 F 0.68345(9) 0.55288(14) -0.16905(8) 0.0303(3) Uani 1 1 d . . . F7 F 0.44207(8) 0.71042(14) 0.11700(8) 0.0268(2) Uani 1 1 d . . . F8 F 0.59531(8) 0.77872(13) 0.17049(7) 0.0226(2) Uani 1 1 d . . . F9 F 0.56603(9) 0.56610(12) 0.10257(8) 0.0274(2) Uani 1 1 d . . . F10 F 0.69027(9) 1.06840(13) -0.20346(8) 0.0280(3) Uani 1 1 d . . . F11 F 0.78926(9) 1.01724(13) -0.07380(8) 0.0262(2) Uani 1 1 d . . . F12 F 0.76410(8) 0.85692(13) -0.18555(7) 0.0244(2) Uani 1 1 d . . . C1 C 0.85701(13) 0.7123(2) -0.01053(12) 0.0188(3) Uani 1 1 d . . . C2 C 0.94895(14) 0.7908(2) 0.00356(13) 0.0214(4) Uani 1 1 d . . . H2 H 0.9612(16) 0.864(2) 0.0490(16) 0.022(5) Uiso 1 1 d . . . C3 C 1.02347(14) 0.7594(2) -0.04816(14) 0.0223(4) Uani 1 1 d . . . H3 H 1.0824(18) 0.814(3) -0.0369(16) 0.027(6) Uiso 1 1 d . . . C4 C 1.00731(13) 0.6480(2) -0.11482(12) 0.0204(4) Uani 1 1 d . . . C5 C 0.91951(14) 0.5638(2) -0.12694(13) 0.0200(3) Uani 1 1 d . . . H5 H 0.9074(17) 0.488(3) -0.1688(17) 0.028(6) Uiso 1 1 d . . . C6 C 0.84508(13) 0.5946(2) -0.07495(12) 0.0184(3) Uani 1 1 d . . . C7 C 1.08356(14) 0.6226(2) -0.17696(14) 0.0243(4) Uani 1 1 d . . . C8 C 0.75026(14) 0.5019(2) -0.09582(13) 0.0206(4) Uani 1 1 d . . . C11 C 0.63402(13) 0.82213(19) -0.01992(12) 0.0164(3) Uani 1 1 d . . . C12 C 0.54109(14) 0.78005(19) 0.00515(12) 0.0179(3) Uani 1 1 d . . . C13 C 0.44789(14) 0.8022(2) -0.05424(13) 0.0215(4) Uani 1 1 d . . . H13 H 0.3865(19) 0.773(3) -0.0345(18) 0.028(6) Uiso 1 1 d . . . C14 C 0.44442(14) 0.8698(2) -0.13980(13) 0.0232(4) Uani 1 1 d . . . H14 H 0.3835(17) 0.880(3) -0.1789(16) 0.024(6) Uiso 1 1 d . . . C15 C 0.53353(14) 0.9201(2) -0.16390(12) 0.0210(4) Uani 1 1 d . . . H15 H 0.5325(17) 0.972(3) -0.2184(16) 0.024(6) Uiso 1 1 d . . . C16 C 0.62739(13) 0.89766(19) -0.10522(12) 0.0179(3) Uani 1 1 d . . . C17 C 0.53602(14) 0.7088(2) 0.09839(13) 0.0200(3) Uani 1 1 d . . . C18 C 0.71801(14) 0.9595(2) -0.14155(12) 0.0201(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.01682(10) 0.02217(10) 0.01327(9) 0.00022(7) 0.00127(6) -0.00114(7) Cl1 0.0227(2) 0.0302(2) 0.0185(2) -0.00859(17) 0.00344(16) -0.00535(17) F1 0.0185(6) 0.0623(9) 0.0380(7) -0.0101(7) 0.0054(5) 0.0024(6) F2 0.0375(7) 0.0319(7) 0.0452(8) -0.0103(6) 0.0198(6) 0.0028(5) F3 0.0415(8) 0.0454(8) 0.0325(7) 0.0129(6) 0.0180(6) 0.0115(6) F4 0.0294(6) 0.0216(6) 0.0591(9) -0.0126(6) 0.0093(6) -0.0038(5) F5 0.0306(6) 0.0320(6) 0.0221(6) -0.0029(5) 0.0081(5) -0.0115(5) F6 0.0247(6) 0.0391(7) 0.0230(6) 0.0039(5) -0.0058(4) -0.0086(5) F7 0.0217(5) 0.0366(6) 0.0236(6) 0.0025(5) 0.0079(4) -0.0066(5) F8 0.0247(6) 0.0283(6) 0.0145(5) -0.0010(4) 0.0031(4) -0.0044(4) F9 0.0377(6) 0.0212(6) 0.0241(6) 0.0035(5) 0.0080(5) 0.0001(5) F10 0.0342(6) 0.0262(6) 0.0246(6) 0.0094(5) 0.0082(5) -0.0005(5) F11 0.0295(6) 0.0283(6) 0.0204(5) -0.0014(5) 0.0036(4) -0.0105(5) F12 0.0256(6) 0.0286(6) 0.0211(5) -0.0016(4) 0.0096(4) 0.0010(4) C1 0.0180(8) 0.0220(8) 0.0157(8) 0.0010(7) 0.0012(6) -0.0001(7) C2 0.0202(9) 0.0232(9) 0.0196(9) -0.0035(7) 0.0006(7) -0.0017(7) C3 0.0177(8) 0.0251(9) 0.0232(9) 0.0006(7) 0.0020(7) -0.0016(7) C4 0.0183(8) 0.0239(9) 0.0186(8) 0.0022(7) 0.0027(6) 0.0045(7) C5 0.0219(8) 0.0206(9) 0.0157(8) -0.0011(7) -0.0007(6) 0.0021(7) C6 0.0175(8) 0.0196(8) 0.0166(8) 0.0023(7) -0.0005(6) -0.0005(6) C7 0.0214(9) 0.0272(10) 0.0246(9) -0.0002(8) 0.0052(7) 0.0033(7) C8 0.0212(9) 0.0215(9) 0.0190(8) -0.0020(7) 0.0033(7) -0.0016(7) C11 0.0178(8) 0.0171(8) 0.0138(8) -0.0017(6) 0.0015(6) -0.0012(6) C12 0.0212(8) 0.0177(8) 0.0145(8) -0.0015(6) 0.0026(6) -0.0020(6) C13 0.0181(8) 0.0247(9) 0.0214(9) -0.0011(7) 0.0032(7) -0.0012(7) C14 0.0201(9) 0.0285(10) 0.0191(9) -0.0014(7) -0.0011(7) 0.0032(7) C15 0.0265(9) 0.0224(9) 0.0137(8) 0.0001(7) 0.0032(7) 0.0034(7) C16 0.0211(8) 0.0173(8) 0.0161(8) -0.0027(6) 0.0055(6) -0.0008(6) C17 0.0211(8) 0.0215(8) 0.0172(8) -0.0009(7) 0.0029(7) -0.0032(7) C18 0.0246(9) 0.0202(9) 0.0156(8) 0.0004(7) 0.0041(7) -0.0014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C1 1.9880(18) . ? As1 C11 2.0182(17) . ? As1 Cl1 2.2074(5) . ? F1 C7 1.341(2) . ? F2 C7 1.337(2) . ? F3 C7 1.347(2) . ? F4 C8 1.334(2) . ? F5 C8 1.356(2) . ? F6 C8 1.342(2) . ? F7 C17 1.341(2) . ? F8 C17 1.353(2) . ? F9 C17 1.351(2) . ? F10 C18 1.343(2) . ? F11 C18 1.346(2) . ? F12 C18 1.347(2) . ? C1 C2 1.406(3) . ? C1 C6 1.412(3) . ? C2 C3 1.395(3) . ? C2 H2 0.93(2) . ? C3 C4 1.392(3) . ? C3 H3 0.92(2) . ? C4 C5 1.388(3) . ? C4 C7 1.512(3) . ? C5 C6 1.396(3) . ? C5 H5 0.91(2) . ? C6 C8 1.507(2) . ? C11 C16 1.412(2) . ? C11 C12 1.419(2) . ? C12 C13 1.396(3) . ? C12 C17 1.523(3) . ? C13 C14 1.387(3) . ? C13 H13 0.96(3) . ? C14 C15 1.388(3) . ? C14 H14 0.91(2) . ? C15 C16 1.399(3) . ? C15 H15 0.92(2) . ? C16 C18 1.525(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 As1 C11 102.98(7) . . ? C1 As1 Cl1 100.08(6) . . ? C11 As1 Cl1 98.84(5) . . ? C2 C1 C6 117.67(17) . . ? C2 C1 As1 119.93(14) . . ? C6 C1 As1 121.89(13) . . ? C3 C2 C1 121.27(18) . . ? C3 C2 H2 119.0(13) . . ? C1 C2 H2 119.7(13) . . ? C4 C3 C2 119.74(18) . . ? C4 C3 H3 122.0(15) . . ? C2 C3 H3 118.3(15) . . ? C5 C4 C3 120.24(17) . . ? C5 C4 C7 119.75(17) . . ? C3 C4 C7 119.97(17) . . ? C4 C5 C6 120.02(17) . . ? C4 C5 H5 122.5(15) . . ? C6 C5 H5 117.5(15) . . ? C5 C6 C1 120.89(16) . . ? C5 C6 C8 116.34(16) . . ? C1 C6 C8 122.67(16) . . ? F2 C7 F1 107.22(16) . . ? F2 C7 F3 106.45(16) . . ? F1 C7 F3 106.14(16) . . ? F2 C7 C4 112.56(16) . . ? F1 C7 C4 112.37(16) . . ? F3 C7 C4 111.67(15) . . ? F4 C8 F6 106.89(15) . . ? F4 C8 F5 106.89(15) . . ? F6 C8 F5 105.57(14) . . ? F4 C8 C6 112.24(15) . . ? F6 C8 C6 112.42(15) . . ? F5 C8 C6 112.38(15) . . ? C16 C11 C12 116.65(15) . . ? C16 C11 As1 129.99(13) . . ? C12 C11 As1 113.23(12) . . ? C13 C12 C11 121.96(17) . . ? C13 C12 C17 115.54(16) . . ? C11 C12 C17 122.51(16) . . ? C14 C13 C12 119.84(17) . . ? C14 C13 H13 120.6(15) . . ? C12 C13 H13 119.5(15) . . ? C13 C14 C15 119.49(17) . . ? C13 C14 H14 119.1(14) . . ? C15 C14 H14 121.5(14) . . ? C14 C15 C16 121.10(17) . . ? C14 C15 H15 121.0(14) . . ? C16 C15 H15 117.9(14) . . ? C15 C16 C11 120.75(16) . . ? C15 C16 C18 114.74(16) . . ? C11 C16 C18 124.50(16) . . ? F7 C17 F9 106.60(15) . . ? F7 C17 F8 105.86(14) . . ? F9 C17 F8 106.62(15) . . ? F7 C17 C12 112.45(15) . . ? F9 C17 C12 112.45(15) . . ? F8 C17 C12 112.39(15) . . ? F10 C18 F11 106.24(14) . . ? F10 C18 F12 106.09(14) . . ? F11 C18 F12 107.05(15) . . ? F10 C18 C16 111.58(15) . . ? F11 C18 C16 112.86(15) . . ? F12 C18 C16 112.56(15) . . ? 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 As1 C1 C2 118.97(15) . . . . ? Cl1 As1 C1 C2 17.37(16) . . . . ? C11 As1 C1 C6 -69.40(16) . . . . ? Cl1 As1 C1 C6 -171.01(14) . . . . ? C6 C1 C2 C3 3.7(3) . . . . ? As1 C1 C2 C3 175.69(15) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -3.0(3) . . . . ? C2 C3 C4 C7 174.56(18) . . . . ? C3 C4 C5 C6 2.7(3) . . . . ? C7 C4 C5 C6 -174.84(17) . . . . ? C4 C5 C6 C1 0.9(3) . . . . ? C4 C5 C6 C8 177.32(16) . . . . ? C2 C1 C6 C5 -4.0(3) . . . . ? As1 C1 C6 C5 -175.79(13) . . . . ? C2 C1 C6 C8 179.78(17) . . . . ? As1 C1 C6 C8 8.0(2) . . . . ? C5 C4 C7 F2 -25.4(2) . . . . ? C3 C4 C7 F2 157.11(17) . . . . ? C5 C4 C7 F1 -146.53(18) . . . . ? C3 C4 C7 F1 35.9(2) . . . . ? C5 C4 C7 F3 94.3(2) . . . . ? C3 C4 C7 F3 -83.2(2) . . . . ? C5 C6 C8 F4 37.2(2) . . . . ? C1 C6 C8 F4 -146.37(17) . . . . ? C5 C6 C8 F6 -83.3(2) . . . . ? C1 C6 C8 F6 93.1(2) . . . . ? C5 C6 C8 F5 157.76(16) . . . . ? C1 C6 C8 F5 -25.9(2) . . . . ? C1 As1 C11 C16 -29.01(17) . . . . ? Cl1 As1 C11 C16 73.56(16) . . . . ? C1 As1 C11 C12 146.61(13) . . . . ? Cl1 As1 C11 C12 -110.82(12) . . . . ? C16 C11 C12 C13 4.5(3) . . . . ? As1 C11 C12 C13 -171.70(15) . . . . ? C16 C11 C12 C17 -175.11(16) . . . . ? As1 C11 C12 C17 8.6(2) . . . . ? C11 C12 C13 C14 -1.3(3) . . . . ? C17 C12 C13 C14 178.37(17) . . . . ? C12 C13 C14 C15 -2.5(3) . . . . ? C13 C14 C15 C16 3.0(3) . . . . ? C14 C15 C16 C11 0.4(3) . . . . ? C14 C15 C16 C18 -179.95(17) . . . . ? C12 C11 C16 C15 -4.1(2) . . . . ? As1 C11 C16 C15 171.42(14) . . . . ? C12 C11 C16 C18 176.35(16) . . . . ? As1 C11 C16 C18 -8.2(3) . . . . ? C13 C12 C17 F7 -14.7(2) . . . . ? C11 C12 C17 F7 165.01(16) . . . . ? C13 C12 C17 F9 105.68(19) . . . . ? C11 C12 C17 F9 -74.6(2) . . . . ? C13 C12 C17 F8 -134.00(17) . . . . ? C11 C12 C17 F8 45.7(2) . . . . ? C15 C16 C18 F10 23.1(2) . . . . ? C11 C16 C18 F10 -157.31(16) . . . . ? C15 C16 C18 F11 142.63(16) . . . . ? C11 C16 C18 F11 -37.8(2) . . . . ? C15 C16 C18 F12 -96.06(19) . . . . ? C11 C16 C18 F12 83.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 1.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.003 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.070 #===============================================END data_6 _database_code_CSD 189705 _chemical_name_systematic ; 2,4-fluoromethylbenzene-2,5-fluromethylbenzene arsenic bromide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H6 As Br F12' _chemical_formula_weight 581.04 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 13.7761(8) _cell_length_b 8.9308(5) _cell_length_c 14.6416(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.6590(10) _cell_angle_gamma 90.00 _cell_volume 1775.84(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4644 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 4.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2790 _exptl_absorpt_correction_T_max 0.4811 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (6 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.53 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% . _diffrn_reflns_number 18290 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4075 _reflns_number_gt 3532 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. ; _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^)+(0.0163P)^2^+1.2630P] 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 4075 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 As1 As 0.247996(14) 0.24830(2) 0.431977(13) 0.01356(6) Uani 1 1 d . . . Br1 Br 0.192524(15) 0.01544(2) 0.368393(14) 0.02122(6) Uani 1 1 d . . . C11 C 0.14912(14) 0.2917(2) 0.51241(13) 0.0144(4) Uani 1 1 d . . . C12 C 0.05934(14) 0.2152(2) 0.49883(14) 0.0176(4) Uani 1 1 d . . . H12A H 0.0489 0.1382 0.4556 0.021 Uiso 1 1 calc R . . C13 C -0.01430(15) 0.2520(2) 0.54847(14) 0.0193(4) Uani 1 1 d . . . H13A H -0.0735 0.1997 0.5385 0.023 Uiso 1 1 calc R . . C14 C 0.00020(14) 0.3667(2) 0.61302(13) 0.0166(4) Uani 1 1 d . . . C15 C 0.08667(14) 0.4489(2) 0.62484(14) 0.0163(4) Uani 1 1 d . . . H15A H 0.0954 0.5284 0.6664 0.020 Uiso 1 1 calc R . . C16 C 0.16037(14) 0.4125(2) 0.57459(13) 0.0150(4) Uani 1 1 d . . . C17 C -0.07578(15) 0.3987(2) 0.67289(15) 0.0212(4) Uani 1 1 d . . . F11 F -0.16764(9) 0.37799(17) 0.62805(9) 0.0328(3) Uani 1 1 d . . . F12 F -0.06547(11) 0.30853(17) 0.74711(10) 0.0385(4) Uani 1 1 d . . . F13 F -0.07105(10) 0.53879(15) 0.70487(10) 0.0338(3) Uani 1 1 d . . . C18 C 0.25295(15) 0.5048(2) 0.59452(14) 0.0187(4) Uani 1 1 d . . . F14 F 0.23485(10) 0.64627(15) 0.61326(11) 0.0384(4) Uani 1 1 d . . . F15 F 0.31619(9) 0.45221(16) 0.66697(9) 0.0300(3) Uani 1 1 d . . . F16 F 0.30316(9) 0.50635(14) 0.52311(8) 0.0246(3) Uani 1 1 d . . . C21 C 0.36531(14) 0.1777(2) 0.52225(13) 0.0129(4) Uani 1 1 d . . . C22 C 0.36940(14) 0.1037(2) 0.60765(13) 0.0140(4) Uani 1 1 d . . . C23 C 0.45950(15) 0.0811(2) 0.66568(14) 0.0181(4) Uani 1 1 d . . . H23A H 0.4608 0.0322 0.7219 0.022 Uiso 1 1 calc R . . C24 C 0.54644(15) 0.1297(2) 0.64131(14) 0.0214(4) Uani 1 1 d . . . H24A H 0.6055 0.1179 0.6819 0.026 Uiso 1 1 calc R . . C25 C 0.54513(15) 0.1960(2) 0.55611(14) 0.0185(4) Uani 1 1 d . . . H25A H 0.6038 0.2258 0.5381 0.022 Uiso 1 1 calc R . . C26 C 0.45607(14) 0.2186(2) 0.49680(13) 0.0138(4) Uani 1 1 d . . . C27 C 0.28069(15) 0.0434(2) 0.64493(14) 0.0179(4) Uani 1 1 d . . . F21 F 0.30606(10) -0.06596(14) 0.70694(9) 0.0275(3) Uani 1 1 d . . . F22 F 0.21151(9) -0.01384(14) 0.57911(8) 0.0238(3) Uani 1 1 d . . . F23 F 0.23681(9) 0.14939(14) 0.68890(8) 0.0238(3) Uani 1 1 d . . . C28 C 0.46302(14) 0.2891(2) 0.40428(14) 0.0178(4) Uani 1 1 d . . . F24 F 0.43455(9) 0.43292(13) 0.39917(8) 0.0245(3) Uani 1 1 d . . . F25 F 0.55488(9) 0.28641(15) 0.38551(8) 0.0246(3) Uani 1 1 d . . . F26 F 0.40728(8) 0.21792(13) 0.33285(8) 0.0189(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.01247(10) 0.01586(11) 0.01229(9) 0.00031(8) 0.00190(7) -0.00140(7) Br1 0.02046(11) 0.02543(12) 0.01849(10) -0.00978(8) 0.00535(8) -0.00716(8) C11 0.0126(9) 0.0159(10) 0.0147(9) 0.0010(8) 0.0024(7) 0.0013(7) C12 0.0166(10) 0.0163(10) 0.0198(10) -0.0032(8) 0.0026(8) -0.0020(8) C13 0.0154(9) 0.0198(11) 0.0231(10) -0.0005(8) 0.0039(8) -0.0017(8) C14 0.0144(9) 0.0187(11) 0.0172(9) 0.0028(8) 0.0041(8) 0.0035(8) C15 0.0171(10) 0.0145(10) 0.0168(10) -0.0005(8) 0.0010(8) 0.0014(8) C16 0.0141(9) 0.0144(10) 0.0154(9) 0.0010(8) -0.0003(7) 0.0003(8) C17 0.0198(10) 0.0218(11) 0.0227(11) 0.0011(9) 0.0054(8) 0.0026(9) F11 0.0152(6) 0.0470(9) 0.0375(8) -0.0058(7) 0.0082(6) 0.0011(6) F12 0.0417(8) 0.0470(9) 0.0319(8) 0.0179(7) 0.0214(6) 0.0155(7) F13 0.0322(7) 0.0288(8) 0.0449(8) -0.0124(6) 0.0191(6) 0.0010(6) C18 0.0185(10) 0.0173(11) 0.0202(10) -0.0038(8) 0.0029(8) -0.0005(8) F14 0.0277(7) 0.0175(7) 0.0723(11) -0.0195(7) 0.0150(7) -0.0058(6) F15 0.0240(7) 0.0398(8) 0.0231(7) 0.0034(6) -0.0051(5) -0.0099(6) F16 0.0244(6) 0.0278(7) 0.0226(6) -0.0039(5) 0.0071(5) -0.0117(5) C21 0.0163(9) 0.0098(9) 0.0125(9) -0.0023(7) 0.0021(7) -0.0006(7) C22 0.0199(10) 0.0100(9) 0.0130(9) -0.0030(7) 0.0056(7) 0.0007(7) C23 0.0246(11) 0.0177(10) 0.0120(9) 0.0010(8) 0.0028(8) 0.0062(8) C24 0.0193(10) 0.0250(12) 0.0181(10) -0.0010(9) -0.0026(8) 0.0051(9) C25 0.0144(9) 0.0192(11) 0.0222(10) -0.0021(8) 0.0040(8) -0.0010(8) C26 0.0164(9) 0.0103(9) 0.0147(9) -0.0017(7) 0.0026(7) -0.0015(7) C27 0.0242(11) 0.0156(10) 0.0147(9) 0.0008(8) 0.0054(8) -0.0011(8) F21 0.0359(7) 0.0237(7) 0.0243(7) 0.0125(5) 0.0089(6) 0.0006(6) F22 0.0274(7) 0.0231(7) 0.0212(6) 0.0001(5) 0.0051(5) -0.0103(5) F23 0.0276(7) 0.0243(7) 0.0227(6) -0.0032(5) 0.0136(5) 0.0004(5) C28 0.0162(10) 0.0172(10) 0.0204(10) 0.0003(8) 0.0046(8) -0.0029(8) F24 0.0362(7) 0.0145(6) 0.0242(6) 0.0044(5) 0.0095(5) -0.0010(5) F25 0.0165(6) 0.0347(7) 0.0245(6) 0.0017(6) 0.0092(5) -0.0064(5) F26 0.0189(6) 0.0242(6) 0.0141(5) -0.0011(5) 0.0042(5) -0.0038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C11 1.9827(19) . ? As1 C21 2.0099(19) . ? As1 Br1 2.3530(3) . ? C11 C12 1.398(3) . ? C11 C16 1.403(3) . ? C12 C13 1.383(3) . ? C12 H12A 0.9300 . ? C13 C14 1.385(3) . ? C13 H13A 0.9300 . ? C14 C15 1.385(3) . ? C14 C17 1.501(3) . ? C15 C16 1.389(3) . ? C15 H15A 0.9300 . ? C16 C18 1.506(3) . ? C17 F13 1.334(2) . ? C17 F11 1.337(2) . ? C17 F12 1.341(2) . ? C18 F14 1.325(2) . ? C18 F15 1.340(2) . ? C18 F16 1.347(2) . ? C21 C22 1.407(3) . ? C21 C26 1.411(3) . ? C22 C23 1.396(3) . ? C22 C27 1.518(3) . ? C23 C24 1.376(3) . ? C23 H23A 0.9300 . ? C24 C25 1.378(3) . ? C24 H24A 0.9300 . ? C25 C26 1.394(3) . ? C25 H25A 0.9300 . ? C26 C28 1.511(3) . ? C27 F22 1.338(2) . ? C27 F21 1.340(2) . ? C27 F23 1.344(2) . ? C28 F25 1.340(2) . ? C28 F24 1.342(2) . ? C28 F26 1.348(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 As1 C21 103.15(8) . . ? C11 As1 Br1 101.43(6) . . ? C21 As1 Br1 98.91(5) . . ? C12 C11 C16 117.83(18) . . ? C12 C11 As1 119.97(15) . . ? C16 C11 As1 121.59(14) . . ? C13 C12 C11 121.26(19) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 119.97(19) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 C15 119.98(19) . . ? C13 C14 C17 120.29(19) . . ? C15 C14 C17 119.69(19) . . ? C14 C15 C16 119.97(19) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C11 120.85(18) . . ? C15 C16 C18 116.10(18) . . ? C11 C16 C18 122.99(18) . . ? F13 C17 F11 106.77(17) . . ? F13 C17 F12 106.65(17) . . ? F11 C17 F12 106.13(17) . . ? F13 C17 C14 112.70(18) . . ? F11 C17 C14 112.47(17) . . ? F12 C17 C14 111.68(17) . . ? F14 C18 F15 106.87(17) . . ? F14 C18 F16 106.85(17) . . ? F15 C18 F16 105.53(16) . . ? F14 C18 C16 112.31(17) . . ? F15 C18 C16 112.25(17) . . ? F16 C18 C16 112.57(16) . . ? C22 C21 C26 116.81(17) . . ? C22 C21 As1 129.76(14) . . ? C26 C21 As1 113.29(13) . . ? C23 C22 C21 120.51(18) . . ? C23 C22 C27 114.65(17) . . ? C21 C22 C27 124.85(17) . . ? C24 C23 C22 121.34(19) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C23 C24 C25 119.37(18) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? C24 C25 C26 120.18(19) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 121.62(18) . . ? C25 C26 C28 115.93(17) . . ? C21 C26 C28 122.45(17) . . ? F22 C27 F21 106.42(16) . . ? F22 C27 F23 106.91(16) . . ? F21 C27 F23 106.02(15) . . ? F22 C27 C22 113.31(16) . . ? F21 C27 C22 111.59(17) . . ? F23 C27 C22 112.13(16) . . ? F25 C28 F24 106.44(16) . . ? F25 C28 F26 105.50(16) . . ? F24 C28 F26 106.55(16) . . ? F25 C28 C26 112.37(16) . . ? F24 C28 C26 112.75(17) . . ? F26 C28 C26 112.68(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.391 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.071 #===============================================END data_7 _database_code_CSD 189706 _chemical_name_systematic ; (2,4-Bis-trifluoromethyl-phenyl)-(2,6-Bis-trifluoromethyl -phenyl)-arsane ; _chemical_name_common 'Arsenic hydride derivative' _chemical_melting_point ? _chemical_formula_moiety 'C16 H7 As F12' _chemical_formula_sum 'C16 H7 As F12' _chemical_formula_weight 502.14 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.1315(10) _cell_length_b 14.9159(18) _cell_length_c 28.272(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.389(2) _cell_angle_gamma 90.00 _cell_volume 3407.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8637 _cell_measurement_theta_min 6.411 _cell_measurement_theta_max 52.957 _exptl_crystal_description shapeless _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (20s exposure) covering 0.3\% in \w. Crystal to detector distance 6 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% . _diffrn_reflns_number 26623 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.25 _reflns_number_total 7075 _reflns_number_gt 5199 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.049 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.049 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. ; _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^)+(0.0384P)^2^+11.1391P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7075 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.193 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.00244(7) 0.73710(4) 0.179068(18) 0.03556(18) Uani 1 1 d . . . H11 H 0.163(7) 0.758(4) 0.1742(19) 0.043 Uiso 1 1 d . . . C11 C -0.0211(6) 0.7811(3) 0.24404(16) 0.0206(9) Uani 1 1 d . . . C12 C -0.0923(6) 0.8651(3) 0.24958(16) 0.0224(10) Uani 1 1 d . . . H12A H -0.1332 0.8983 0.2221 0.027 Uiso 1 1 calc R . . C13 C -0.1049(6) 0.9011(3) 0.29419(16) 0.0230(10) Uani 1 1 d . . . H13A H -0.1531 0.9586 0.2971 0.028 Uiso 1 1 calc R . . C14 C -0.0469(6) 0.8531(3) 0.33440(16) 0.0234(10) Uani 1 1 d . . . C15 C 0.0247(6) 0.7700(3) 0.33029(16) 0.0233(10) Uani 1 1 d . . . H15A H 0.0649 0.7371 0.3580 0.028 Uiso 1 1 calc R . . C16 C 0.0375(5) 0.7345(3) 0.28506(16) 0.0216(9) Uani 1 1 d . . . C17 C -0.0602(6) 0.8934(4) 0.38240(17) 0.0292(11) Uani 1 1 d . . . F11 F -0.0378(6) 0.8333(3) 0.41734(12) 0.0749(14) Uani 1 1 d . . . F12 F -0.2067(4) 0.9301(2) 0.38573(10) 0.0367(7) Uani 1 1 d . . . F13 F 0.0480(4) 0.9595(3) 0.39247(13) 0.0611(12) Uani 1 1 d . . . C18 C 0.1151(6) 0.6424(3) 0.28209(16) 0.0262(11) Uani 1 1 d . . . F14 F 0.1868(4) 0.6136(2) 0.32399(10) 0.0423(8) Uani 1 1 d . . . F15 F 0.2316(4) 0.6419(2) 0.25190(11) 0.0386(7) Uani 1 1 d . . . F16 F 0.0030(4) 0.58039(18) 0.26606(10) 0.0345(7) Uani 1 1 d . . . C21 C -0.1957(6) 0.7973(3) 0.14509(15) 0.0213(10) Uani 1 1 d . . . C22 C -0.1748(6) 0.8751(3) 0.11802(16) 0.0247(10) Uani 1 1 d . . . C23 C -0.3119(6) 0.9176(3) 0.09369(17) 0.0290(11) Uani 1 1 d . . . H23A H -0.2961 0.9696 0.0753 0.035 Uiso 1 1 calc R . . C24 C -0.4698(7) 0.8854(3) 0.09592(18) 0.0320(12) Uani 1 1 d . . . H24A H -0.5622 0.9159 0.0798 0.038 Uiso 1 1 calc R . . C25 C -0.4930(6) 0.8090(3) 0.12148(18) 0.0301(11) Uani 1 1 d . . . H25A H -0.6014 0.7861 0.1227 0.036 Uiso 1 1 calc R . . C26 C -0.3572(6) 0.7652(3) 0.14568(16) 0.0237(10) Uani 1 1 d . . . C27 C -0.0071(7) 0.9158(3) 0.11391(18) 0.0308(11) Uani 1 1 d . . . F21 F -0.0165(4) 0.9904(2) 0.08778(13) 0.0516(9) Uani 1 1 d . . . F22 F 0.0745(4) 0.9385(2) 0.15660(11) 0.0375(7) Uani 1 1 d . . . F23 F 0.0930(4) 0.8597(2) 0.09340(11) 0.0387(7) Uani 1 1 d . . . C28 C -0.3943(7) 0.6797(3) 0.17103(17) 0.0314(12) Uani 1 1 d . . . F24 F -0.5573(4) 0.6644(2) 0.17095(12) 0.0472(9) Uani 1 1 d . . . F25 F -0.3343(5) 0.60744(19) 0.15019(11) 0.0431(8) Uani 1 1 d . . . F26 F -0.3289(4) 0.6776(2) 0.21687(10) 0.0364(7) Uani 1 1 d . . . As31 As -0.5938(4) 0.2161(2) 0.03487(13) 0.0276(5) Uani 0.459(3) 1 d P A 1 H31 H -0.503(14) 0.119(8) 0.040(4) 0.033 Uiso 0.459(3) 1 d P A 1 As32 As -0.5470(3) 0.19427(17) 0.03930(10) 0.0276(5) Uani 0.54 1 d P A 2 H32 H -0.721(13) 0.208(7) 0.034(3) 0.033 Uiso 0.541(3) 1 d P A 2 C31 C -0.5110(5) 0.2627(3) 0.09977(15) 0.0202(9) Uani 1 1 d . . . C32 C -0.4250(6) 0.3446(3) 0.10343(17) 0.0256(10) Uani 1 1 d . A . H32A H -0.3877 0.3697 0.0757 0.031 Uiso 1 1 calc R . . C33 C -0.3932(6) 0.3896(3) 0.14601(17) 0.0236(10) Uani 1 1 d . . . H33A H -0.3349 0.4449 0.1474 0.028 Uiso 1 1 calc R A . C34 C -0.4467(6) 0.3537(3) 0.18686(16) 0.0218(10) Uani 1 1 d . A . C35 C -0.5286(6) 0.2732(3) 0.18497(17) 0.0240(10) Uani 1 1 d . . . H35A H -0.5634 0.2484 0.2132 0.029 Uiso 1 1 calc R A . C36 C -0.5609(6) 0.2275(3) 0.14203(16) 0.0212(9) Uani 1 1 d . A . C37 C -0.4159(6) 0.4048(4) 0.23274(17) 0.0300(11) Uani 1 1 d . . . F31 F -0.5266(4) 0.4691(3) 0.23612(14) 0.0649(12) Uani 1 1 d . A . F32 F -0.4163(7) 0.3523(3) 0.27043(12) 0.0802(15) Uani 1 1 d . A . F33 F -0.2711(4) 0.4466(2) 0.23776(11) 0.0450(9) Uani 1 1 d . A . C38 C -0.6462(6) 0.1387(3) 0.14172(17) 0.0278(11) Uani 1 1 d . . . F34 F -0.7759(4) 0.1339(2) 0.10765(11) 0.0456(9) Uani 1 1 d . A . F35 F -0.5469(4) 0.0708(2) 0.13358(12) 0.0462(8) Uani 1 1 d . A . F36 F -0.7071(4) 0.1204(2) 0.18262(10) 0.0396(8) Uani 1 1 d . A . C41 C -0.4168(6) 0.2722(3) 0.00054(15) 0.0230(10) Uani 1 1 d . . . C42 C -0.4699(6) 0.3497(3) -0.02582(15) 0.0223(10) Uani 1 1 d . A . C43 C -0.3627(6) 0.3966(3) -0.05204(16) 0.0267(11) Uani 1 1 d . . . H43A H -0.4015 0.4481 -0.0696 0.032 Uiso 1 1 calc R A . C44 C -0.2004(7) 0.3691(3) -0.05279(18) 0.0306(11) Uani 1 1 d . A . H44A H -0.1276 0.4020 -0.0704 0.037 Uiso 1 1 calc R . . C45 C -0.1455(6) 0.2936(3) -0.02775(18) 0.0295(11) Uani 1 1 d . . . H45A H -0.0347 0.2738 -0.0284 0.035 Uiso 1 1 calc R A . C46 C -0.2522(6) 0.2458(3) -0.00138(16) 0.0254(10) Uani 1 1 d . A . C47 C -0.6430(7) 0.3848(3) -0.02740(17) 0.0291(11) Uani 1 1 d . . . F41 F -0.6915(4) 0.3980(2) 0.01630(10) 0.0349(7) Uani 1 1 d . A . F42 F -0.6638(4) 0.4642(2) -0.04962(11) 0.0400(8) Uani 1 1 d . A . F43 F -0.7570(4) 0.3292(2) -0.05040(10) 0.0349(7) Uani 1 1 d . A . C48 C -0.1812(7) 0.1626(3) 0.02343(17) 0.0300(11) Uani 1 1 d . . . F44 F -0.2513(4) 0.08626(19) 0.00418(10) 0.0360(7) Uani 1 1 d . A . F45 F -0.0191(4) 0.1540(2) 0.02137(11) 0.0438(8) Uani 1 1 d . A . F46 F -0.2028(4) 0.1613(2) 0.07017(10) 0.0372(7) Uani 1 1 d . A . 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 0.0451(4) 0.0415(3) 0.0191(3) -0.0060(2) -0.0012(2) 0.0231(3) C11 0.025(2) 0.015(2) 0.022(2) -0.0036(17) 0.0028(18) -0.0036(18) C12 0.027(3) 0.019(2) 0.020(2) 0.0038(18) 0.0000(19) 0.0027(19) C13 0.024(2) 0.018(2) 0.027(3) -0.0013(19) 0.0041(19) 0.0001(19) C14 0.023(2) 0.024(2) 0.023(2) -0.0060(19) 0.0029(19) -0.0010(19) C15 0.023(2) 0.024(2) 0.022(2) 0.0016(19) -0.0028(18) -0.0028(19) C16 0.020(2) 0.021(2) 0.024(2) -0.0018(19) 0.0018(18) -0.0005(19) C17 0.029(3) 0.035(3) 0.023(3) -0.006(2) 0.000(2) 0.004(2) F11 0.141(4) 0.063(3) 0.0214(18) 0.0008(17) 0.009(2) 0.049(3) F12 0.0310(17) 0.0493(19) 0.0307(16) -0.0135(14) 0.0071(13) 0.0019(14) F13 0.040(2) 0.084(3) 0.062(2) -0.054(2) 0.0151(17) -0.0225(19) C18 0.035(3) 0.024(3) 0.019(2) -0.0007(19) -0.002(2) 0.002(2) F14 0.064(2) 0.0335(17) 0.0268(16) 0.0048(13) -0.0090(14) 0.0227(16) F15 0.0378(18) 0.0348(18) 0.0451(19) 0.0024(14) 0.0126(14) 0.0151(14) F16 0.0471(19) 0.0177(14) 0.0386(17) -0.0044(12) 0.0040(14) 0.0006(13) C21 0.030(3) 0.019(2) 0.015(2) -0.0058(17) 0.0014(18) 0.0050(19) C22 0.034(3) 0.021(2) 0.019(2) -0.0048(18) 0.003(2) 0.001(2) C23 0.042(3) 0.016(2) 0.028(3) -0.0001(19) -0.001(2) -0.002(2) C24 0.038(3) 0.023(3) 0.032(3) -0.006(2) -0.010(2) 0.002(2) C25 0.029(3) 0.029(3) 0.032(3) -0.011(2) -0.001(2) -0.001(2) C26 0.030(3) 0.020(2) 0.021(2) -0.0108(18) 0.0024(19) -0.005(2) C27 0.038(3) 0.025(3) 0.030(3) 0.000(2) 0.005(2) 0.002(2) F21 0.053(2) 0.0375(19) 0.064(2) 0.0230(17) 0.0064(18) -0.0057(16) F22 0.0338(17) 0.0413(19) 0.0361(17) -0.0107(14) -0.0020(13) -0.0078(14) F23 0.0422(19) 0.0422(19) 0.0343(17) -0.0011(14) 0.0156(14) 0.0003(15) C28 0.040(3) 0.031(3) 0.024(3) -0.002(2) 0.004(2) -0.004(2) F24 0.043(2) 0.053(2) 0.046(2) 0.0057(16) 0.0058(15) -0.0170(16) F25 0.077(2) 0.0187(15) 0.0354(17) -0.0040(13) 0.0136(16) -0.0060(15) F26 0.0503(19) 0.0357(17) 0.0233(15) 0.0012(12) 0.0053(13) -0.0063(14) As31 0.0398(14) 0.0255(13) 0.0182(6) -0.0022(7) 0.0062(8) -0.0129(7) As32 0.0398(14) 0.0255(13) 0.0182(6) -0.0022(7) 0.0062(8) -0.0129(7) C31 0.020(2) 0.023(2) 0.018(2) -0.0029(18) 0.0044(17) -0.0002(19) C32 0.033(3) 0.019(2) 0.026(3) 0.0023(19) 0.007(2) -0.006(2) C33 0.024(2) 0.019(2) 0.028(3) 0.0010(19) 0.0054(19) 0.0007(19) C34 0.022(2) 0.022(2) 0.022(2) -0.0012(18) 0.0025(18) 0.0051(19) C35 0.024(2) 0.024(2) 0.024(2) 0.0023(19) 0.0015(19) 0.004(2) C36 0.025(2) 0.017(2) 0.022(2) 0.0043(18) 0.0017(18) 0.0048(19) C37 0.032(3) 0.034(3) 0.024(3) -0.007(2) 0.005(2) -0.003(2) F31 0.040(2) 0.079(3) 0.074(3) -0.055(2) -0.0067(18) 0.0189(19) F32 0.162(5) 0.059(3) 0.0196(18) -0.0042(17) 0.010(2) -0.047(3) F33 0.0341(18) 0.063(2) 0.0371(18) -0.0218(16) 0.0004(14) -0.0130(16) C38 0.038(3) 0.025(3) 0.022(2) 0.001(2) 0.009(2) -0.001(2) F34 0.053(2) 0.044(2) 0.0374(18) 0.0068(15) -0.0055(15) -0.0259(16) F35 0.060(2) 0.0189(16) 0.063(2) -0.0031(14) 0.0215(18) -0.0015(15) F36 0.061(2) 0.0316(17) 0.0284(16) 0.0022(13) 0.0168(14) -0.0177(15) C41 0.033(3) 0.021(2) 0.015(2) -0.0036(18) 0.0007(18) -0.009(2) C42 0.030(3) 0.020(2) 0.016(2) -0.0056(18) 0.0003(19) -0.005(2) C43 0.039(3) 0.019(2) 0.022(2) 0.0021(19) 0.005(2) -0.001(2) C44 0.036(3) 0.026(3) 0.031(3) 0.001(2) 0.010(2) -0.008(2) C45 0.031(3) 0.024(3) 0.034(3) -0.004(2) 0.003(2) -0.004(2) C46 0.033(3) 0.023(3) 0.019(2) -0.0021(19) -0.0024(19) -0.004(2) C47 0.040(3) 0.026(3) 0.022(2) -0.002(2) 0.005(2) -0.001(2) F41 0.0415(18) 0.0386(18) 0.0259(15) -0.0057(13) 0.0091(13) 0.0048(14) F42 0.049(2) 0.0330(17) 0.0380(18) 0.0079(14) 0.0037(15) 0.0115(15) F43 0.0304(16) 0.0447(18) 0.0298(16) -0.0082(13) 0.0036(12) -0.0042(14) C48 0.040(3) 0.027(3) 0.021(2) 0.000(2) -0.005(2) 0.000(2) F44 0.0494(19) 0.0275(16) 0.0289(16) 0.0039(12) -0.0058(13) -0.0007(14) F45 0.0384(19) 0.049(2) 0.0425(19) 0.0073(15) -0.0040(14) 0.0097(15) F46 0.056(2) 0.0317(17) 0.0212(15) 0.0028(12) -0.0052(13) -0.0006(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C11 1.980(4) . ? As1 C21 1.995(5) . ? As1 H11 1.37(6) . ? C11 C16 1.390(6) . ? C11 C12 1.396(6) . ? C12 C13 1.385(6) . ? C12 H12A 0.9500 . ? C13 C14 1.382(7) . ? C13 H13A 0.9500 . ? C14 C15 1.380(7) . ? C14 C17 1.499(6) . ? C15 C16 1.398(6) . ? C15 H15A 0.9500 . ? C16 C18 1.519(7) . ? C17 F12 1.324(6) . ? C17 F11 1.331(6) . ? C17 F13 1.331(6) . ? C18 F14 1.332(5) . ? C18 F16 1.342(6) . ? C18 F15 1.344(6) . ? C21 C26 1.400(7) . ? C21 C22 1.410(7) . ? C22 C23 1.395(7) . ? C22 C27 1.509(7) . ? C23 C24 1.380(7) . ? C23 H23A 0.9500 . ? C24 C25 1.373(7) . ? C24 H24A 0.9500 . ? C25 C26 1.396(7) . ? C25 H25A 0.9500 . ? C26 C28 1.509(7) . ? C27 F21 1.332(6) . ? C27 F23 1.343(6) . ? C27 F22 1.354(6) . ? C28 F24 1.345(6) . ? C28 F26 1.345(6) . ? C28 F25 1.346(6) . ? As31 C41 2.006(6) . ? As31 C31 2.007(6) . ? As31 H31 1.63(12) . ? As31 H32 1.04(10) . ? As32 C41 1.983(5) . ? As32 C31 1.984(5) . ? As32 H31 1.18(13) . ? As32 H32 1.42(10) . ? C31 C32 1.406(6) . ? C31 C36 1.405(6) . ? C32 C33 1.377(7) . ? C32 H32A 0.9500 . ? C33 C34 1.386(6) . ? C33 H33A 0.9500 . ? C34 C35 1.371(7) . ? C34 C37 1.501(6) . ? C35 C36 1.391(6) . ? C35 H35A 0.9500 . ? C36 C38 1.495(7) . ? C37 F32 1.323(6) . ? C37 F33 1.326(6) . ? C37 F31 1.326(6) . ? C38 F35 1.331(6) . ? C38 F36 1.336(5) . ? C38 F34 1.349(6) . ? C41 C46 1.402(7) . ? C41 C42 1.417(6) . ? C42 C43 1.394(7) . ? C42 C47 1.498(7) . ? C43 C44 1.385(7) . ? C43 H43A 0.9500 . ? C44 C45 1.378(7) . ? C44 H44A 0.9500 . ? C45 C46 1.400(7) . ? C45 H45A 0.9500 . ? C46 C48 1.508(7) . ? C47 F42 1.342(6) . ? C47 F41 1.352(5) . ? C47 F43 1.354(6) . ? C48 F45 1.332(6) . ? C48 F46 1.352(5) . ? C48 F44 1.360(6) . ? 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 C11 As1 C21 98.11(18) . . ? C11 As1 H11 102(2) . . ? C21 As1 H11 126(2) . . ? C16 C11 C12 117.6(4) . . ? C16 C11 As1 123.3(3) . . ? C12 C11 As1 119.1(3) . . ? C13 C12 C11 121.6(4) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 C17 120.7(4) . . ? C13 C14 C17 119.0(4) . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C11 C16 C15 121.4(4) . . ? C11 C16 C18 120.8(4) . . ? C15 C16 C18 117.8(4) . . ? F12 C17 F11 106.0(4) . . ? F12 C17 F13 104.9(4) . . ? F11 C17 F13 107.9(5) . . ? F12 C17 C14 112.7(4) . . ? F11 C17 C14 112.6(4) . . ? F13 C17 C14 112.2(4) . . ? F14 C18 F16 107.0(4) . . ? F14 C18 F15 107.1(4) . . ? F16 C18 F15 106.4(4) . . ? F14 C18 C16 112.7(4) . . ? F16 C18 C16 111.8(4) . . ? F15 C18 C16 111.5(4) . . ? C26 C21 C22 117.3(4) . . ? C26 C21 As1 123.2(3) . . ? C22 C21 As1 119.5(4) . . ? C23 C22 C21 120.3(5) . . ? C23 C22 C27 117.2(4) . . ? C21 C22 C27 122.5(4) . . ? C24 C23 C22 121.0(5) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C25 C24 C23 119.7(5) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 120.0(5) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 121.7(4) . . ? C25 C26 C28 116.1(4) . . ? C21 C26 C28 122.2(4) . . ? F21 C27 F23 106.3(4) . . ? F21 C27 F22 106.2(4) . . ? F23 C27 F22 106.2(4) . . ? F21 C27 C22 112.5(4) . . ? F23 C27 C22 112.2(4) . . ? F22 C27 C22 112.9(4) . . ? F24 C28 F26 106.3(4) . . ? F24 C28 F25 105.5(4) . . ? F26 C28 F25 106.2(4) . . ? F24 C28 C26 113.1(4) . . ? F26 C28 C26 113.5(4) . . ? F25 C28 C26 111.5(4) . . ? C41 As31 C31 96.5(2) . . ? C41 As31 H31 94(4) . . ? C31 As31 H31 97(4) . . ? C41 As31 H32 143(5) . . ? C31 As31 H32 107(5) . . ? H31 As31 H32 110(7) . . ? C41 As32 C31 97.9(2) . . ? C41 As32 H31 113(5) . . ? C31 As32 H31 117(5) . . ? C41 As32 H32 116(4) . . ? C31 As32 H32 94(4) . . ? H31 As32 H32 116(7) . . ? C32 C31 C36 116.7(4) . . ? C32 C31 As32 122.3(3) . . ? C36 C31 As32 120.8(3) . . ? C32 C31 As31 118.8(3) . . ? C36 C31 As31 123.3(4) . . ? As32 C31 As31 14.55(9) . . ? C33 C32 C31 122.1(4) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 119.6(4) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C35 C34 C33 120.1(4) . . ? C35 C34 C37 120.8(4) . . ? C33 C34 C37 119.1(4) . . ? C34 C35 C36 120.4(4) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 C31 121.0(4) . . ? C35 C36 C38 118.8(4) . . ? C31 C36 C38 120.2(4) . . ? F32 C37 F33 105.9(4) . . ? F32 C37 F31 107.9(5) . . ? F33 C37 F31 104.8(4) . . ? F32 C37 C34 112.3(4) . . ? F33 C37 C34 113.1(4) . . ? F31 C37 C34 112.3(4) . . ? F35 C38 F36 106.5(4) . . ? F35 C38 F34 106.1(4) . . ? F36 C38 F34 105.8(4) . . ? F35 C38 C36 112.7(4) . . ? F36 C38 C36 113.1(4) . . ? F34 C38 C36 112.1(4) . . ? C46 C41 C42 116.4(4) . . ? C46 C41 As32 115.4(3) . . ? C42 C41 As32 128.2(4) . . ? C46 C41 As31 129.9(4) . . ? C42 C41 As31 113.7(4) . . ? As32 C41 As31 14.56(9) . . ? C43 C42 C41 121.1(4) . . ? C43 C42 C47 116.7(4) . . ? C41 C42 C47 122.1(4) . . ? C44 C43 C42 120.9(5) . . ? C44 C43 H43A 119.6 . . ? C42 C43 H43A 119.6 . . ? C45 C44 C43 119.3(5) . . ? C45 C44 H44A 120.4 . . ? C43 C44 H44A 120.4 . . ? C44 C45 C46 120.3(5) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C45 C46 C41 121.9(4) . . ? C45 C46 C48 116.0(4) . . ? C41 C46 C48 122.0(4) . . ? F42 C47 F41 105.3(4) . . ? F42 C47 F43 105.7(4) . . ? F41 C47 F43 105.9(4) . . ? F42 C47 C42 113.1(4) . . ? F41 C47 C42 113.1(4) . . ? F43 C47 C42 113.0(4) . . ? F45 C48 F46 106.2(4) . . ? F45 C48 F44 105.9(4) . . ? F46 C48 F44 106.5(4) . . ? F45 C48 C46 112.9(4) . . ? F46 C48 C46 112.4(4) . . ? F44 C48 C46 112.4(4) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 27.25 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.993 _refine_diff_density_min -1.334 _refine_diff_density_rms 0.105 #===============================================END