data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Neil Burford' 'Michael J. Ferguson' 'Robert McDonald' 'Paul J. Ragogna' _publ_contact_author_name 'Prof Neil Burford' _publ_contact_author_address ; Department of Chemistry Dalhousie University Halifax Nova Scotia B3H 4J3 CANADA ; _publ_contact_author_email NEIL.BURFORD@DAL.CA _publ_section_title ; Homoatomic P-P Coordination: A Versatile Synthetic Approach to Polyphosphorus Dications ; data_dal0222 _database_code_CSD 207172 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H46 Cl2 F6 O6 P4 S2' _chemical_formula_sum 'C53 H46 Cl2 F6 O6 P4 S2' _chemical_formula_weight 1151.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3972(8) _cell_length_b 12.8629(12) _cell_length_c 13.6679(12) _cell_angle_alpha 119.8007(16) _cell_angle_beta 95.7002(17) _cell_angle_gamma 104.2389(18) _cell_volume 1340.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 2998 _cell_measurement_theta_min 2.318 _cell_measurement_theta_max 26.317 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.388 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8386 _exptl_absorpt_correction_T_max 0.9334 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6741 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5392 _reflns_number_gt 4092 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+1.4865P] 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 5392 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.01394(9) -0.14836(7) 0.03821(7) 0.0199(2) Uani 1 1 d . . . P2 P -0.10408(9) -0.07998(7) 0.17896(7) 0.0234(2) Uani 1 1 d . . . C1 C 0.0686(3) -0.0171(3) 0.0150(3) 0.0216(6) Uani 1 1 d . . . H1A H 0.1431 0.0590 0.0866 0.026 Uiso 1 1 calc R . . H1B H 0.1190 -0.0412 -0.0495 0.026 Uiso 1 1 calc R . . C11 C -0.1165(4) -0.2914(3) -0.0915(3) 0.0229(6) Uani 1 1 d . . . C12 C -0.0601(4) -0.3834(3) -0.1682(3) 0.0288(7) Uani 1 1 d . . . H12 H 0.0461 -0.3690 -0.1531 0.035 Uiso 1 1 calc R . . C13 C -0.1609(4) -0.4960(3) -0.2667(3) 0.0353(8) Uani 1 1 d . . . H13 H -0.1235 -0.5588 -0.3189 0.042 Uiso 1 1 calc R . . C14 C -0.3158(4) -0.5166(3) -0.2885(3) 0.0391(9) Uani 1 1 d . . . H14 H -0.3844 -0.5944 -0.3548 0.047 Uiso 1 1 calc R . . C15 C -0.3713(4) -0.4237(3) -0.2135(3) 0.0359(8) Uani 1 1 d . . . H15 H -0.4773 -0.4374 -0.2298 0.043 Uiso 1 1 calc R . . C16 C -0.2722(4) -0.3117(3) -0.1155(3) 0.0287(7) Uani 1 1 d . . . H16 H -0.3101 -0.2485 -0.0644 0.034 Uiso 1 1 calc R . . C21 C 0.1798(3) -0.1812(3) 0.0750(3) 0.0220(6) Uani 1 1 d . . . C22 C 0.1606(4) -0.2865(3) 0.0847(3) 0.0301(7) Uani 1 1 d . . . H22 H 0.0613 -0.3411 0.0696 0.036 Uiso 1 1 calc R . . C23 C 0.2867(5) -0.3109(4) 0.1164(4) 0.0412(9) Uani 1 1 d . . . H23 H 0.2745 -0.3820 0.1238 0.049 Uiso 1 1 calc R . . C24 C 0.4303(5) -0.2318(4) 0.1371(4) 0.0477(10) Uani 1 1 d . . . H24 H 0.5168 -0.2495 0.1578 0.057 Uiso 1 1 calc R . . C25 C 0.4499(4) -0.1273(4) 0.1283(3) 0.0419(9) Uani 1 1 d . . . H25 H 0.5497 -0.0730 0.1437 0.050 Uiso 1 1 calc R . . C26 C 0.3256(4) -0.1015(3) 0.0971(3) 0.0292(7) Uani 1 1 d . . . H26 H 0.3390 -0.0296 0.0907 0.035 Uiso 1 1 calc R . . C31 C 0.0586(4) 0.0634(3) 0.2849(3) 0.0241(7) Uani 1 1 d . . . C32 C 0.1976(4) 0.0646(3) 0.3322(3) 0.0304(7) Uani 1 1 d . . . H32 H 0.2116 -0.0133 0.3132 0.037 Uiso 1 1 calc R . . C33 C 0.3155(4) 0.1793(4) 0.4070(3) 0.0395(9) Uani 1 1 d . . . H33 H 0.4101 0.1797 0.4394 0.047 Uiso 1 1 calc R . . C34 C 0.2961(4) 0.2930(3) 0.4347(3) 0.0403(9) Uani 1 1 d . . . H34 H 0.3776 0.3713 0.4853 0.048 Uiso 1 1 calc R . . C35 C 0.1587(4) 0.2928(3) 0.3889(3) 0.0353(8) Uani 1 1 d . . . H35 H 0.1453 0.3712 0.4089 0.042 Uiso 1 1 calc R . . C36 C 0.0402(4) 0.1792(3) 0.3139(3) 0.0288(7) Uani 1 1 d . . . H36 H -0.0540 0.1797 0.2820 0.035 Uiso 1 1 calc R . . C41 C -0.1143(4) -0.1918(3) 0.2257(3) 0.0271(7) Uani 1 1 d . . . C42 C -0.2036(4) -0.3202(3) 0.1484(3) 0.0321(8) Uani 1 1 d . . . H42 H -0.2498 -0.3497 0.0700 0.039 Uiso 1 1 calc R . . C43 C -0.2258(4) -0.4048(3) 0.1847(3) 0.0376(9) Uani 1 1 d . . . H43 H -0.2841 -0.4923 0.1308 0.045 Uiso 1 1 calc R . . C44 C -0.1627(5) -0.3617(4) 0.2998(4) 0.0458(10) Uani 1 1 d . . . H44 H -0.1793 -0.4193 0.3251 0.055 Uiso 1 1 calc R . . C45 C -0.0763(6) -0.2357(4) 0.3773(4) 0.0547(12) Uani 1 1 d . . . H45 H -0.0330 -0.2063 0.4562 0.066 Uiso 1 1 calc R . . C46 C -0.0519(5) -0.1505(3) 0.3404(3) 0.0428(10) Uani 1 1 d . . . H46 H 0.0081 -0.0634 0.3946 0.051 Uiso 1 1 calc R . . S S -0.64362(10) -0.23752(8) -0.19977(8) 0.0295(2) Uani 1 1 d . . . F1 F -0.8579(3) -0.3891(2) -0.3977(2) 0.0655(8) Uani 1 1 d . . . F2 F -0.6898(4) -0.2400(3) -0.3940(2) 0.0688(8) Uani 1 1 d . . . F3 F -0.6361(3) -0.4007(2) -0.4122(2) 0.0642(8) Uani 1 1 d . . . O1 O -0.4826(3) -0.1818(2) -0.1766(3) 0.0450(7) Uani 1 1 d . . . O2 O -0.6898(3) -0.3392(3) -0.1804(3) 0.0458(7) Uani 1 1 d . . . O3 O -0.7253(3) -0.1495(2) -0.1593(2) 0.0391(6) Uani 1 1 d . . . C2 C -0.7093(5) -0.3195(4) -0.3582(3) 0.0421(9) Uani 1 1 d . . . Cl1S Cl 0.6333(4) 0.1102(3) 0.5586(2) 0.1570(11) Uani 1 1 d . . . C1S C 0.5671(14) -0.0126(12) 0.4433(11) 0.082(3) Uiso 0.50 1 d P . . H1SA H 0.6362 -0.0626 0.4298 0.098 Uiso 0.50 1 calc PR . . H1SB H 0.5550 0.0041 0.3802 0.098 Uiso 0.50 1 calc PR . . 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 P1 0.0211(4) 0.0177(4) 0.0231(4) 0.0125(3) 0.0057(3) 0.0068(3) P2 0.0242(4) 0.0214(4) 0.0265(4) 0.0138(3) 0.0082(3) 0.0083(3) C1 0.0248(16) 0.0205(14) 0.0234(15) 0.0139(13) 0.0079(12) 0.0084(12) C11 0.0252(16) 0.0208(15) 0.0244(15) 0.0144(13) 0.0050(12) 0.0061(12) C12 0.0300(17) 0.0268(16) 0.0304(17) 0.0149(14) 0.0088(14) 0.0120(14) C13 0.041(2) 0.0266(17) 0.0299(18) 0.0098(15) 0.0063(15) 0.0124(15) C14 0.038(2) 0.0289(18) 0.035(2) 0.0140(16) -0.0079(16) 0.0006(15) C15 0.0252(17) 0.0366(19) 0.039(2) 0.0193(17) -0.0003(15) 0.0067(15) C16 0.0261(17) 0.0292(17) 0.0306(17) 0.0158(14) 0.0039(13) 0.0111(13) C21 0.0236(15) 0.0223(15) 0.0212(15) 0.0113(12) 0.0056(12) 0.0105(12) C22 0.0308(18) 0.0288(17) 0.0361(19) 0.0199(15) 0.0094(14) 0.0129(14) C23 0.047(2) 0.046(2) 0.049(2) 0.0336(19) 0.0115(18) 0.0247(18) C24 0.033(2) 0.057(3) 0.056(3) 0.031(2) 0.0047(18) 0.0240(19) C25 0.0229(18) 0.046(2) 0.050(2) 0.0241(19) 0.0049(16) 0.0083(16) C26 0.0243(17) 0.0274(17) 0.0327(18) 0.0154(14) 0.0050(13) 0.0067(13) C31 0.0291(17) 0.0230(15) 0.0199(15) 0.0117(13) 0.0073(13) 0.0076(13) C32 0.0330(18) 0.0285(17) 0.0308(18) 0.0150(14) 0.0082(14) 0.0142(14) C33 0.0267(18) 0.040(2) 0.040(2) 0.0156(17) 0.0009(15) 0.0094(15) C34 0.036(2) 0.0302(19) 0.039(2) 0.0136(16) 0.0048(16) 0.0008(15) C35 0.045(2) 0.0241(17) 0.0333(19) 0.0147(15) 0.0077(16) 0.0097(15) C36 0.0355(19) 0.0252(16) 0.0263(17) 0.0147(14) 0.0050(14) 0.0110(14) C41 0.0327(18) 0.0248(16) 0.0311(17) 0.0180(14) 0.0168(14) 0.0115(13) C42 0.0351(19) 0.0284(17) 0.0317(18) 0.0180(15) 0.0072(15) 0.0056(14) C43 0.044(2) 0.0244(17) 0.042(2) 0.0178(16) 0.0175(17) 0.0073(15) C44 0.068(3) 0.034(2) 0.046(2) 0.0296(19) 0.023(2) 0.0139(19) C45 0.090(4) 0.040(2) 0.031(2) 0.0239(18) 0.014(2) 0.007(2) C46 0.066(3) 0.0281(18) 0.0299(19) 0.0166(16) 0.0141(18) 0.0065(17) S 0.0294(4) 0.0232(4) 0.0358(5) 0.0154(4) 0.0098(3) 0.0097(3) F1 0.0407(14) 0.0565(15) 0.0550(16) 0.0047(13) -0.0007(12) 0.0105(12) F2 0.096(2) 0.0773(19) 0.0491(15) 0.0415(15) 0.0257(15) 0.0342(17) F3 0.0586(16) 0.0542(15) 0.0525(15) 0.0057(12) 0.0234(13) 0.0259(13) O1 0.0304(14) 0.0312(13) 0.0647(18) 0.0232(13) 0.0068(12) 0.0052(11) O2 0.0472(16) 0.0404(15) 0.0686(19) 0.0389(14) 0.0260(14) 0.0185(13) O3 0.0479(16) 0.0382(14) 0.0322(13) 0.0144(11) 0.0109(11) 0.0266(12) C2 0.043(2) 0.037(2) 0.036(2) 0.0115(17) 0.0137(17) 0.0152(17) Cl1S 0.196(3) 0.142(2) 0.151(2) 0.0979(18) -0.0069(19) 0.0643(19) _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 P1 C21 1.801(3) . ? P1 C11 1.802(3) . ? P1 C1 1.831(3) . ? P1 P2 2.2195(11) . ? P2 C41 1.828(3) . ? P2 C31 1.831(3) . ? C1 C1 1.543(6) 2 ? C11 C16 1.395(5) . ? C11 C12 1.403(4) . ? C12 C13 1.394(5) . ? C13 C14 1.387(5) . ? C14 C15 1.395(5) . ? C15 C16 1.383(5) . ? C21 C26 1.392(4) . ? C21 C22 1.394(4) . ? C22 C23 1.381(5) . ? C23 C24 1.377(6) . ? C24 C25 1.378(6) . ? C25 C26 1.375(5) . ? C31 C32 1.391(5) . ? C31 C36 1.400(4) . ? C32 C33 1.386(5) . ? C33 C34 1.382(5) . ? C34 C35 1.377(5) . ? C35 C36 1.382(5) . ? C41 C46 1.386(5) . ? C41 C42 1.398(5) . ? C42 C43 1.387(5) . ? C43 C44 1.385(6) . ? C44 C45 1.372(5) . ? C45 C46 1.399(5) . ? S O1 1.432(3) . ? S O2 1.435(3) . ? S O3 1.438(2) . ? S C2 1.824(4) . ? F1 C2 1.341(5) . ? F2 C2 1.319(5) . ? F3 C2 1.341(4) . ? Cl1S C1S 1.488(12) . ? Cl1S C1S 1.979(12) 2_656 ? C1S Cl1S 1.979(12) 2_656 ? 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 C21 P1 C11 108.42(14) . . ? C21 P1 C1 110.08(14) . . ? C11 P1 C1 110.99(14) . . ? C21 P1 P2 114.27(10) . . ? C11 P1 P2 109.46(11) . . ? C1 P1 P2 103.59(10) . . ? C41 P2 C31 105.98(15) . . ? C41 P2 P1 102.55(11) . . ? C31 P2 P1 95.03(10) . . ? C1 C1 P1 112.6(3) 2 . ? C16 C11 C12 120.0(3) . . ? C16 C11 P1 120.8(2) . . ? C12 C11 P1 119.2(2) . . ? C13 C12 C11 119.5(3) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 120.3(3) . . ? C16 C15 C14 120.0(3) . . ? C15 C16 C11 120.1(3) . . ? C26 C21 C22 120.0(3) . . ? C26 C21 P1 121.1(2) . . ? C22 C21 P1 118.9(2) . . ? C23 C22 C21 119.7(3) . . ? C24 C23 C22 119.7(4) . . ? C23 C24 C25 120.9(4) . . ? C26 C25 C24 120.1(3) . . ? C25 C26 C21 119.6(3) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 P2 125.3(2) . . ? C36 C31 P2 115.5(2) . . ? C33 C32 C31 120.1(3) . . ? C34 C33 C32 120.3(3) . . ? C35 C34 C33 120.0(3) . . ? C34 C35 C36 120.3(3) . . ? C35 C36 C31 120.2(3) . . ? C46 C41 C42 118.3(3) . . ? C46 C41 P2 121.7(3) . . ? C42 C41 P2 119.4(3) . . ? C43 C42 C41 120.8(3) . . ? C44 C43 C42 119.9(3) . . ? C45 C44 C43 120.0(3) . . ? C44 C45 C46 120.1(4) . . ? C41 C46 C45 120.7(3) . . ? O1 S O2 114.77(17) . . ? O1 S O3 115.80(16) . . ? O2 S O3 115.06(16) . . ? O1 S C2 103.12(18) . . ? O2 S C2 102.90(18) . . ? O3 S C2 102.49(17) . . ? F2 C2 F1 107.0(4) . . ? F2 C2 F3 107.7(3) . . ? F1 C2 F3 106.4(3) . . ? F2 C2 S 112.6(3) . . ? F1 C2 S 111.5(3) . . ? F3 C2 S 111.3(3) . . ? C1S Cl1S C1S 70.7(7) . 2_656 ? Cl1S C1S Cl1S 109.3(7) . 2_656 ? 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 C21 P1 P2 C41 -46.50(16) . . . . ? C11 P1 P2 C41 75.30(16) . . . . ? C1 P1 P2 C41 -166.26(15) . . . . ? C21 P1 P2 C31 61.13(15) . . . . ? C11 P1 P2 C31 -177.08(15) . . . . ? C1 P1 P2 C31 -58.64(15) . . . . ? C21 P1 C1 C1 -179.1(3) . . . 2 ? C11 P1 C1 C1 60.9(3) . . . 2 ? P2 P1 C1 C1 -56.5(3) . . . 2 ? C21 P1 C11 C16 155.3(3) . . . . ? C1 P1 C11 C16 -83.7(3) . . . . ? P2 P1 C11 C16 30.0(3) . . . . ? C21 P1 C11 C12 -24.1(3) . . . . ? C1 P1 C11 C12 96.9(3) . . . . ? P2 P1 C11 C12 -149.4(2) . . . . ? C16 C11 C12 C13 -1.5(5) . . . . ? P1 C11 C12 C13 177.9(3) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C12 C13 C14 C15 1.3(6) . . . . ? C13 C14 C15 C16 -1.4(6) . . . . ? C14 C15 C16 C11 0.1(5) . . . . ? C12 C11 C16 C15 1.4(5) . . . . ? P1 C11 C16 C15 -178.0(3) . . . . ? C11 P1 C21 C26 129.8(3) . . . . ? C1 P1 C21 C26 8.2(3) . . . . ? P2 P1 C21 C26 -107.8(3) . . . . ? C11 P1 C21 C22 -52.1(3) . . . . ? C1 P1 C21 C22 -173.7(2) . . . . ? P2 P1 C21 C22 70.3(3) . . . . ? C26 C21 C22 C23 0.1(5) . . . . ? P1 C21 C22 C23 -178.0(3) . . . . ? C21 C22 C23 C24 -0.6(6) . . . . ? C22 C23 C24 C25 0.9(6) . . . . ? C23 C24 C25 C26 -0.7(6) . . . . ? C24 C25 C26 C21 0.2(6) . . . . ? C22 C21 C26 C25 0.1(5) . . . . ? P1 C21 C26 C25 178.2(3) . . . . ? C41 P2 C31 C32 40.6(3) . . . . ? P1 P2 C31 C32 -64.0(3) . . . . ? C41 P2 C31 C36 -142.9(2) . . . . ? P1 P2 C31 C36 112.5(2) . . . . ? C36 C31 C32 C33 0.1(5) . . . . ? P2 C31 C32 C33 176.4(3) . . . . ? C31 C32 C33 C34 -0.3(6) . . . . ? C32 C33 C34 C35 0.7(6) . . . . ? C33 C34 C35 C36 -0.8(6) . . . . ? C34 C35 C36 C31 0.6(5) . . . . ? C32 C31 C36 C35 -0.2(5) . . . . ? P2 C31 C36 C35 -177.0(3) . . . . ? C31 P2 C41 C46 23.3(3) . . . . ? P1 P2 C41 C46 122.4(3) . . . . ? C31 P2 C41 C42 -165.2(3) . . . . ? P1 P2 C41 C42 -66.1(3) . . . . ? C46 C41 C42 C43 -1.8(5) . . . . ? P2 C41 C42 C43 -173.6(3) . . . . ? C41 C42 C43 C44 2.0(6) . . . . ? C42 C43 C44 C45 -1.1(7) . . . . ? C43 C44 C45 C46 0.1(7) . . . . ? C42 C41 C46 C45 0.8(6) . . . . ? P2 C41 C46 C45 172.4(3) . . . . ? C44 C45 C46 C41 0.0(7) . . . . ? O1 S C2 F2 -66.1(3) . . . . ? O2 S C2 F2 174.2(3) . . . . ? O3 S C2 F2 54.5(3) . . . . ? O1 S C2 F1 173.6(3) . . . . ? O2 S C2 F1 53.9(3) . . . . ? O3 S C2 F1 -65.8(3) . . . . ? O1 S C2 F3 54.9(3) . . . . ? O2 S C2 F3 -64.7(3) . . . . ? O3 S C2 F3 175.5(3) . . . . ? C1S Cl1S C1S Cl1S 0.0 2_656 . . 2_656 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.230 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.082 data_dal0248 _database_code_CSD 207173 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 F6 O6 P4 S2' _chemical_formula_sum 'C32 H36 F6 O6 P4 S2' _chemical_formula_weight 818.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 8.6372(12) _cell_length_b 13.5443(19) _cell_length_c 15.742(2) _cell_angle_alpha 96.528(3) _cell_angle_beta 93.131(3) _cell_angle_gamma 99.431(2) _cell_volume 1799.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.397 _cell_measurement_theta_max 26.045 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.400 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7896 _exptl_absorpt_correction_T_max 0.9649 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11460 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.32 _reflns_number_total 7168 _reflns_number_gt 4743 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+3.3707P] 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 7168 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.31313(12) 0.08220(8) 0.45711(7) 0.0248(3) Uani 1 1 d . . . P2 P 0.45679(12) 0.21404(8) 0.41233(7) 0.0261(3) Uani 1 1 d . . . C1 C 0.4319(5) 0.0174(3) 0.5228(3) 0.0264(9) Uani 1 1 d . . . H1A H 0.4745 0.0632 0.5754 0.032 Uiso 1 1 calc R . . H1B H 0.3641 -0.0419 0.5403 0.032 Uiso 1 1 calc R . . C2 C 0.1559(5) 0.1126(3) 0.5204(3) 0.0310(10) Uani 1 1 d . . . H2A H 0.0963 0.0506 0.5369 0.037 Uiso 1 1 calc R . . H2B H 0.0858 0.1459 0.4868 0.037 Uiso 1 1 calc R . . H2C H 0.2001 0.1579 0.5721 0.037 Uiso 1 1 calc R . . C3 C 0.2346(5) -0.0040(4) 0.3644(3) 0.0357(11) Uani 1 1 d . . . H3A H 0.1693 -0.0632 0.3821 0.043 Uiso 1 1 calc R . . H3B H 0.3212 -0.0251 0.3332 0.043 Uiso 1 1 calc R . . H3C H 0.1704 0.0292 0.3270 0.043 Uiso 1 1 calc R . . C11 C 0.5944(5) 0.2534(3) 0.5070(3) 0.0243(9) Uani 1 1 d . . . C12 C 0.7536(5) 0.2597(3) 0.4927(3) 0.0312(10) Uani 1 1 d . . . H12 H 0.7837 0.2451 0.4361 0.037 Uiso 1 1 calc R . . C13 C 0.8675(5) 0.2868(3) 0.5597(3) 0.0360(11) Uani 1 1 d . . . H13 H 0.9754 0.2909 0.5491 0.043 Uiso 1 1 calc R . . C14 C 0.8252(5) 0.3082(4) 0.6423(3) 0.0384(11) Uani 1 1 d . . . H14 H 0.9038 0.3271 0.6885 0.046 Uiso 1 1 calc R . . C15 C 0.6666(6) 0.3018(4) 0.6576(3) 0.0378(11) Uani 1 1 d . . . H15 H 0.6373 0.3153 0.7145 0.045 Uiso 1 1 calc R . . C16 C 0.5521(5) 0.2761(3) 0.5908(3) 0.0328(10) Uani 1 1 d . . . H16 H 0.4445 0.2739 0.6015 0.039 Uiso 1 1 calc R . . C21 C 0.3115(5) 0.2986(3) 0.4186(3) 0.0271(9) Uani 1 1 d . . . C22 C 0.1750(5) 0.2723(3) 0.3635(3) 0.0297(9) Uani 1 1 d . . . H22 H 0.1550 0.2085 0.3292 0.036 Uiso 1 1 calc R . . C23 C 0.0688(5) 0.3375(4) 0.3582(3) 0.0350(11) Uani 1 1 d . . . H23 H -0.0243 0.3184 0.3210 0.042 Uiso 1 1 calc R . . C24 C 0.0978(6) 0.4300(4) 0.4068(3) 0.0393(11) Uani 1 1 d . . . H24 H 0.0257 0.4755 0.4026 0.047 Uiso 1 1 calc R . . C25 C 0.2319(6) 0.4572(4) 0.4620(3) 0.0423(12) Uani 1 1 d . . . H25 H 0.2514 0.5213 0.4957 0.051 Uiso 1 1 calc R . . C26 C 0.3385(5) 0.3914(3) 0.4686(3) 0.0338(10) Uani 1 1 d . . . H26 H 0.4297 0.4102 0.5072 0.041 Uiso 1 1 calc R . . P3 P 0.16578(18) 0.41778(11) 0.06373(9) 0.0487(4) Uani 1 1 d . . . P4 P 0.01633(15) 0.28614(12) 0.10663(8) 0.0435(4) Uani 1 1 d . . . C4 C 0.0748(7) 0.4872(5) -0.0136(4) 0.0582(15) Uani 1 1 d . . . H4A H 0.1479 0.5500 -0.0199 0.070 Uiso 1 1 calc R . . H4B H 0.0564 0.4456 -0.0703 0.070 Uiso 1 1 calc R . . C5 C 0.2243(8) 0.5056(4) 0.1587(4) 0.0633(18) Uani 1 1 d . . . H5A H 0.2924 0.5655 0.1440 0.076 Uiso 1 1 calc R . . H5B H 0.2819 0.4738 0.2004 0.076 Uiso 1 1 calc R . . H5C H 0.1307 0.5252 0.1837 0.076 Uiso 1 1 calc R . . C6 C 0.3338(8) 0.3900(5) 0.0121(4) 0.0638(17) Uani 1 1 d . . . H6A H 0.3933 0.4521 -0.0043 0.077 Uiso 1 1 calc R . . H6B H 0.3003 0.3416 -0.0393 0.077 Uiso 1 1 calc R . . H6C H 0.4006 0.3609 0.0513 0.077 Uiso 1 1 calc R . . C31 C -0.1175(5) 0.2452(4) 0.0110(3) 0.0413(12) Uani 1 1 d . . . C32 C -0.2777(5) 0.2299(4) 0.0246(3) 0.0402(11) Uani 1 1 d . . . H32 H -0.3097 0.2372 0.0814 0.048 Uiso 1 1 calc R . . C33 C -0.3902(6) 0.2044(4) -0.0437(3) 0.0421(12) Uani 1 1 d . . . H33 H -0.4989 0.1945 -0.0338 0.050 Uiso 1 1 calc R . . C34 C -0.3435(6) 0.1932(4) -0.1268(3) 0.0476(13) Uani 1 1 d . . . H34 H -0.4207 0.1766 -0.1739 0.057 Uiso 1 1 calc R . . C35 C -0.1868(6) 0.2061(4) -0.1414(3) 0.0496(13) Uani 1 1 d . . . H35 H -0.1559 0.1975 -0.1984 0.060 Uiso 1 1 calc R . . C36 C -0.0732(6) 0.2318(5) -0.0732(3) 0.0504(14) Uani 1 1 d . . . H36 H 0.0352 0.2403 -0.0837 0.060 Uiso 1 1 calc R . . C41 C 0.1621(5) 0.2022(3) 0.1030(3) 0.0324(10) Uani 1 1 d . . . C42 C 0.2918(6) 0.2262(4) 0.1640(3) 0.0376(11) Uani 1 1 d . . . H42 H 0.3031 0.2859 0.2034 0.045 Uiso 1 1 calc R . . C43 C 0.4019(6) 0.1644(4) 0.1673(3) 0.0413(12) Uani 1 1 d . . . H43 H 0.4910 0.1829 0.2075 0.050 Uiso 1 1 calc R . . C44 C 0.3843(6) 0.0755(4) 0.1127(4) 0.0467(13) Uani 1 1 d . . . H44 H 0.4590 0.0317 0.1165 0.056 Uiso 1 1 calc R . . C45 C 0.2583(6) 0.0509(4) 0.0528(4) 0.0528(14) Uani 1 1 d . . . H45 H 0.2472 -0.0097 0.0145 0.063 Uiso 1 1 calc R . . C46 C 0.1466(6) 0.1136(4) 0.0475(4) 0.0469(13) Uani 1 1 d . . . H46 H 0.0597 0.0956 0.0059 0.056 Uiso 1 1 calc R . . S1 S -0.23609(15) 0.05089(11) 0.27278(8) 0.0413(3) Uani 1 1 d . . . S2 S 0.26614(15) 0.39071(12) -0.24240(9) 0.0477(4) Uani 1 1 d . . . F11 F -0.2566(5) -0.0918(5) 0.1451(2) 0.122(2) Uani 1 1 d . . . F12 F -0.0195(4) -0.0214(4) 0.1896(2) 0.0946(15) Uani 1 1 d . . . F13 F -0.1500(6) -0.1258(3) 0.2603(3) 0.0970(14) Uani 1 1 d . . . F21 F 0.3693(5) 0.5765(3) -0.1784(3) 0.1030(15) Uani 1 1 d . . . F22 F 0.4627(5) 0.5329(3) -0.2978(3) 0.0867(13) Uani 1 1 d . . . F23 F 0.2259(6) 0.5602(4) -0.2968(4) 0.1145(18) Uani 1 1 d . . . O11 O -0.1332(4) 0.0710(3) 0.3501(2) 0.0429(8) Uani 1 1 d . . . O12 O -0.3961(4) 0.0065(4) 0.2843(2) 0.0630(12) Uani 1 1 d . . . O13 O -0.2216(6) 0.1264(4) 0.2177(3) 0.0900(17) Uani 1 1 d . . . O21 O 0.2321(4) 0.3431(3) -0.3291(2) 0.0613(11) Uani 1 1 d . . . O22 O 0.1294(5) 0.3953(4) -0.1945(3) 0.0787(15) Uani 1 1 d . . . O23 O 0.3975(5) 0.3654(4) -0.1957(3) 0.0684(12) Uani 1 1 d . . . C10 C -0.1648(7) -0.0552(7) 0.2142(4) 0.069(2) Uani 1 1 d . . . C20 C 0.3320(7) 0.5215(5) -0.2547(4) 0.0624(17) 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 P1 0.0209(5) 0.0253(6) 0.0289(6) 0.0003(4) -0.0012(4) 0.0088(4) P2 0.0236(5) 0.0298(6) 0.0251(6) -0.0002(4) 0.0027(4) 0.0070(4) C1 0.028(2) 0.024(2) 0.030(2) 0.0048(17) -0.0011(18) 0.0127(17) C2 0.024(2) 0.035(2) 0.036(2) 0.007(2) 0.0064(18) 0.0081(18) C3 0.030(2) 0.036(3) 0.040(3) -0.003(2) -0.006(2) 0.009(2) C11 0.022(2) 0.021(2) 0.031(2) -0.0005(17) 0.0047(17) 0.0064(16) C12 0.028(2) 0.029(2) 0.036(2) -0.0005(19) 0.0060(19) 0.0074(18) C13 0.026(2) 0.029(2) 0.054(3) 0.001(2) 0.000(2) 0.0098(19) C14 0.032(2) 0.033(3) 0.046(3) 0.000(2) -0.011(2) 0.002(2) C15 0.042(3) 0.038(3) 0.030(2) -0.004(2) -0.003(2) 0.005(2) C16 0.023(2) 0.039(3) 0.035(2) -0.002(2) 0.0040(18) 0.0045(19) C21 0.026(2) 0.030(2) 0.027(2) 0.0068(18) 0.0042(17) 0.0105(18) C22 0.032(2) 0.032(2) 0.026(2) 0.0044(18) 0.0017(18) 0.0074(19) C23 0.030(2) 0.043(3) 0.035(3) 0.013(2) 0.0013(19) 0.011(2) C24 0.035(3) 0.036(3) 0.052(3) 0.014(2) 0.006(2) 0.015(2) C25 0.040(3) 0.027(2) 0.059(3) -0.001(2) 0.002(2) 0.008(2) C26 0.026(2) 0.030(2) 0.045(3) 0.004(2) 0.001(2) 0.0036(18) P3 0.0593(9) 0.0424(8) 0.0461(8) -0.0088(6) -0.0156(7) 0.0295(7) P4 0.0299(6) 0.0676(9) 0.0317(7) -0.0135(6) -0.0033(5) 0.0199(6) C4 0.056(4) 0.067(4) 0.049(3) 0.000(3) 0.003(3) 0.007(3) C5 0.082(4) 0.047(3) 0.056(4) -0.018(3) -0.030(3) 0.027(3) C6 0.077(4) 0.051(4) 0.068(4) 0.018(3) 0.013(3) 0.015(3) C31 0.029(2) 0.062(3) 0.033(3) -0.008(2) -0.002(2) 0.018(2) C32 0.033(2) 0.046(3) 0.043(3) 0.000(2) 0.002(2) 0.013(2) C33 0.028(2) 0.045(3) 0.052(3) -0.001(2) -0.004(2) 0.011(2) C34 0.043(3) 0.051(3) 0.045(3) 0.001(2) -0.017(2) 0.006(2) C35 0.049(3) 0.062(4) 0.035(3) -0.004(2) 0.000(2) 0.008(3) C36 0.033(3) 0.073(4) 0.041(3) -0.014(3) 0.001(2) 0.011(3) C41 0.025(2) 0.037(3) 0.035(2) 0.002(2) 0.0022(18) 0.0060(19) C42 0.041(3) 0.050(3) 0.022(2) 0.005(2) -0.0011(19) 0.009(2) C43 0.032(2) 0.055(3) 0.037(3) 0.015(2) -0.006(2) 0.008(2) C44 0.039(3) 0.046(3) 0.059(3) 0.013(3) 0.002(2) 0.012(2) C45 0.041(3) 0.042(3) 0.071(4) -0.009(3) 0.000(3) 0.010(2) C46 0.028(2) 0.053(3) 0.056(3) -0.007(3) -0.001(2) 0.006(2) S1 0.0366(7) 0.0585(8) 0.0325(6) 0.0112(6) 0.0024(5) 0.0152(6) S2 0.0290(6) 0.0674(9) 0.0465(8) 0.0049(7) 0.0075(5) 0.0082(6) F11 0.069(3) 0.220(6) 0.055(2) -0.068(3) -0.013(2) 0.028(3) F12 0.046(2) 0.172(5) 0.068(2) -0.008(3) 0.0173(18) 0.035(2) F13 0.140(4) 0.053(2) 0.095(3) -0.016(2) 0.007(3) 0.027(3) F21 0.091(3) 0.088(3) 0.111(4) -0.041(3) -0.019(3) 0.004(2) F22 0.063(2) 0.103(3) 0.096(3) 0.043(3) 0.013(2) -0.005(2) F23 0.097(3) 0.091(3) 0.159(5) 0.017(3) -0.052(3) 0.045(3) O11 0.0426(19) 0.043(2) 0.0402(19) -0.0060(15) -0.0053(15) 0.0110(16) O12 0.0314(19) 0.113(4) 0.046(2) 0.007(2) 0.0070(16) 0.018(2) O13 0.070(3) 0.117(4) 0.101(4) 0.072(3) 0.008(3) 0.029(3) O21 0.047(2) 0.080(3) 0.053(2) -0.013(2) 0.0062(18) 0.012(2) O22 0.037(2) 0.133(4) 0.060(3) -0.007(3) 0.022(2) 0.001(2) O23 0.049(2) 0.089(3) 0.073(3) 0.034(2) -0.002(2) 0.016(2) C10 0.050(4) 0.117(6) 0.034(3) -0.020(4) -0.006(3) 0.019(4) C20 0.046(3) 0.060(4) 0.078(4) -0.003(3) -0.018(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C3 1.788(4) . ? P1 C2 1.801(4) . ? P1 C1 1.810(4) . ? P1 P2 2.2092(16) . ? P2 C11 1.826(4) . ? P2 C21 1.831(4) . ? C1 C1 1.522(8) 2_656 ? C11 C12 1.396(6) . ? C11 C16 1.402(6) . ? C12 C13 1.377(6) . ? C13 C14 1.382(7) . ? C14 C15 1.394(7) . ? C15 C16 1.377(6) . ? C21 C26 1.384(6) . ? C21 C22 1.396(6) . ? C22 C23 1.380(6) . ? C23 C24 1.370(7) . ? C24 C25 1.382(7) . ? C25 C26 1.389(7) . ? P3 C6 1.774(7) . ? P3 C5 1.795(5) . ? P3 C4 1.839(6) . ? P3 P4 2.217(2) . ? P4 C31 1.822(5) . ? P4 C41 1.828(5) . ? C4 C4 1.465(12) 2_565 ? C31 C32 1.397(7) . ? C31 C36 1.400(7) . ? C32 C33 1.382(7) . ? C33 C34 1.390(7) . ? C34 C35 1.372(7) . ? C35 C36 1.387(7) . ? C41 C46 1.385(7) . ? C41 C42 1.405(6) . ? C42 C43 1.368(7) . ? C43 C44 1.379(7) . ? C44 C45 1.371(7) . ? C45 C46 1.390(7) . ? S1 O13 1.409(4) . ? S1 O11 1.439(3) . ? S1 O12 1.444(4) . ? S1 C10 1.829(7) . ? S2 O23 1.428(4) . ? S2 O21 1.435(4) . ? S2 O22 1.441(4) . ? S2 C20 1.805(7) . ? F11 C10 1.309(6) . ? F12 C10 1.356(7) . ? F13 C10 1.282(8) . ? F21 C20 1.333(7) . ? F22 C20 1.345(8) . ? F23 C20 1.312(7) . ? 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 C3 P1 C2 110.0(2) . . ? C3 P1 C1 107.4(2) . . ? C2 P1 C1 106.3(2) . . ? C3 P1 P2 107.45(17) . . ? C2 P1 P2 114.14(16) . . ? C1 P1 P2 111.33(15) . . ? C11 P2 C21 106.54(19) . . ? C11 P2 P1 98.62(14) . . ? C21 P2 P1 98.07(14) . . ? C1 C1 P1 113.2(4) 2_656 . ? C12 C11 C16 118.9(4) . . ? C12 C11 P2 115.8(3) . . ? C16 C11 P2 125.3(3) . . ? C13 C12 C11 120.7(4) . . ? C12 C13 C14 120.2(4) . . ? C13 C14 C15 119.7(4) . . ? C16 C15 C14 120.5(4) . . ? C15 C16 C11 120.0(4) . . ? C26 C21 C22 118.8(4) . . ? C26 C21 P2 122.9(3) . . ? C22 C21 P2 117.9(3) . . ? C23 C22 C21 121.0(4) . . ? C24 C23 C22 119.8(4) . . ? C23 C24 C25 120.0(4) . . ? C24 C25 C26 120.5(5) . . ? C21 C26 C25 119.8(4) . . ? C6 P3 C5 110.3(3) . . ? C6 P3 C4 102.0(3) . . ? C5 P3 C4 106.2(3) . . ? C6 P3 P4 114.9(2) . . ? C5 P3 P4 105.5(2) . . ? C4 P3 P4 117.6(2) . . ? C31 P4 C41 106.4(2) . . ? C31 P4 P3 99.74(19) . . ? C41 P4 P3 97.31(15) . . ? C4 C4 P3 111.7(6) 2_565 . ? C32 C31 C36 118.5(4) . . ? C32 C31 P4 115.8(4) . . ? C36 C31 P4 125.7(4) . . ? C33 C32 C31 120.8(5) . . ? C32 C33 C34 119.6(5) . . ? C35 C34 C33 120.5(5) . . ? C34 C35 C36 120.2(5) . . ? C35 C36 C31 120.3(5) . . ? C46 C41 C42 118.4(4) . . ? C46 C41 P4 123.8(4) . . ? C42 C41 P4 117.6(4) . . ? C43 C42 C41 120.8(5) . . ? C42 C43 C44 120.4(4) . . ? C45 C44 C43 119.6(5) . . ? C44 C45 C46 120.8(5) . . ? C41 C46 C45 120.0(5) . . ? O13 S1 O11 116.4(3) . . ? O13 S1 O12 114.6(3) . . ? O11 S1 O12 114.5(2) . . ? O13 S1 C10 104.9(4) . . ? O11 S1 C10 102.2(2) . . ? O12 S1 C10 101.6(3) . . ? O23 S2 O21 116.5(3) . . ? O23 S2 O22 114.7(3) . . ? O21 S2 O22 114.4(2) . . ? O23 S2 C20 102.8(3) . . ? O21 S2 C20 103.4(3) . . ? O22 S2 C20 102.3(3) . . ? F13 C10 F11 109.8(7) . . ? F13 C10 F12 106.6(6) . . ? F11 C10 F12 108.0(5) . . ? F13 C10 S1 112.8(4) . . ? F11 C10 S1 111.0(5) . . ? F12 C10 S1 108.4(5) . . ? F23 C20 F21 108.6(6) . . ? F23 C20 F22 107.1(6) . . ? F21 C20 F22 106.4(5) . . ? F23 C20 S2 112.6(4) . . ? F21 C20 S2 110.7(5) . . ? F22 C20 S2 111.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 P1 P2 C11 -152.5(2) . . . . ? C2 P1 P2 C11 85.2(2) . . . . ? C1 P1 P2 C11 -35.2(2) . . . . ? C3 P1 P2 C21 99.3(2) . . . . ? C2 P1 P2 C21 -23.0(2) . . . . ? C1 P1 P2 C21 -143.3(2) . . . . ? C3 P1 C1 C1 60.1(5) . . . 2_656 ? C2 P1 C1 C1 177.9(4) . . . 2_656 ? P2 P1 C1 C1 -57.3(4) . . . 2_656 ? C21 P2 C11 C12 -135.3(3) . . . . ? P1 P2 C11 C12 123.6(3) . . . . ? C21 P2 C11 C16 45.3(4) . . . . ? P1 P2 C11 C16 -55.8(4) . . . . ? C16 C11 C12 C13 0.6(6) . . . . ? P2 C11 C12 C13 -178.8(3) . . . . ? C11 C12 C13 C14 0.1(7) . . . . ? C12 C13 C14 C15 0.2(7) . . . . ? C13 C14 C15 C16 -1.1(7) . . . . ? C14 C15 C16 C11 1.8(7) . . . . ? C12 C11 C16 C15 -1.6(7) . . . . ? P2 C11 C16 C15 177.8(4) . . . . ? C11 P2 C21 C26 19.8(4) . . . . ? P1 P2 C21 C26 121.4(4) . . . . ? C11 P2 C21 C22 -167.2(3) . . . . ? P1 P2 C21 C22 -65.7(3) . . . . ? C26 C21 C22 C23 0.3(6) . . . . ? P2 C21 C22 C23 -172.9(3) . . . . ? C21 C22 C23 C24 0.8(7) . . . . ? C22 C23 C24 C25 -1.0(7) . . . . ? C23 C24 C25 C26 0.2(8) . . . . ? C22 C21 C26 C25 -1.2(7) . . . . ? P2 C21 C26 C25 171.8(4) . . . . ? C24 C25 C26 C21 0.9(7) . . . . ? C6 P3 P4 C31 -90.1(3) . . . . ? C5 P3 P4 C31 148.3(3) . . . . ? C4 P3 P4 C31 30.1(3) . . . . ? C6 P3 P4 C41 18.0(3) . . . . ? C5 P3 P4 C41 -103.6(3) . . . . ? C4 P3 P4 C41 138.1(3) . . . . ? C6 P3 C4 C4 176.3(6) . . . 2_565 ? C5 P3 C4 C4 -68.2(7) . . . 2_565 ? P4 P3 C4 C4 49.6(7) . . . 2_565 ? C41 P4 C31 C32 129.8(4) . . . . ? P3 P4 C31 C32 -129.5(4) . . . . ? C41 P4 C31 C36 -52.6(6) . . . . ? P3 P4 C31 C36 48.1(5) . . . . ? C36 C31 C32 C33 -1.4(8) . . . . ? P4 C31 C32 C33 176.3(4) . . . . ? C31 C32 C33 C34 0.3(8) . . . . ? C32 C33 C34 C35 0.8(8) . . . . ? C33 C34 C35 C36 -0.9(9) . . . . ? C34 C35 C36 C31 -0.3(9) . . . . ? C32 C31 C36 C35 1.4(9) . . . . ? P4 C31 C36 C35 -176.1(5) . . . . ? C31 P4 C41 C46 -12.6(5) . . . . ? P3 P4 C41 C46 -115.1(4) . . . . ? C31 P4 C41 C42 171.7(4) . . . . ? P3 P4 C41 C42 69.3(4) . . . . ? C46 C41 C42 C43 1.3(7) . . . . ? P4 C41 C42 C43 177.2(4) . . . . ? C41 C42 C43 C44 -2.3(7) . . . . ? C42 C43 C44 C45 2.2(8) . . . . ? C43 C44 C45 C46 -1.1(9) . . . . ? C42 C41 C46 C45 -0.2(8) . . . . ? P4 C41 C46 C45 -175.9(4) . . . . ? C44 C45 C46 C41 0.2(9) . . . . ? O13 S1 C10 F13 171.1(5) . . . . ? O11 S1 C10 F13 49.2(5) . . . . ? O12 S1 C10 F13 -69.3(5) . . . . ? O13 S1 C10 F11 -65.2(6) . . . . ? O11 S1 C10 F11 173.0(5) . . . . ? O12 S1 C10 F11 54.5(6) . . . . ? O13 S1 C10 F12 53.3(5) . . . . ? O11 S1 C10 F12 -68.6(5) . . . . ? O12 S1 C10 F12 172.9(4) . . . . ? O23 S2 C20 F23 -179.9(5) . . . . ? O21 S2 C20 F23 58.5(6) . . . . ? O22 S2 C20 F23 -60.7(6) . . . . ? O23 S2 C20 F21 -58.1(5) . . . . ? O21 S2 C20 F21 -179.7(4) . . . . ? O22 S2 C20 F21 61.1(5) . . . . ? O23 S2 C20 F22 60.0(5) . . . . ? O21 S2 C20 F22 -61.7(5) . . . . ? O22 S2 C20 F22 179.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.797 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.098 data_dal0302 _database_code_CSD 207174 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H52 Cl8 Ga2 P4' _chemical_formula_sum 'C54 H52 Cl8 Ga2 P4' _chemical_formula_weight 1247.88 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' 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2/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 30.395(4) _cell_length_b 10.1195(12) _cell_length_c 19.465(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.829(2) _cell_angle_gamma 90.00 _cell_volume 5760.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6752 _cell_measurement_theta_min 2.240 _cell_measurement_theta_max 26.353 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.97 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3331 _exptl_absorpt_correction_T_max 0.9052 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15469 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5896 _reflns_number_gt 4077 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+0.0000P] 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 5896 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.11993(3) -0.30480(9) 0.17574(4) 0.0273(2) Uani 1 1 d . . . P2 P 0.09239(3) -0.10577(10) 0.18609(4) 0.0371(2) Uani 1 1 d . . . C1 C 0.07188(11) -0.4142(3) 0.14385(16) 0.0313(7) Uani 1 1 d . . . H1A H 0.0833 -0.5063 0.1475 0.038 Uiso 1 1 calc R . . H1B H 0.0516 -0.4060 0.1756 0.038 Uiso 1 1 calc R . . C2 C 0.04352(11) -0.3893(4) 0.06677(16) 0.0350(8) Uani 1 1 d . . . H2A H 0.0248 -0.3086 0.0649 0.042 Uiso 1 1 calc R . . H2B H 0.0642 -0.3753 0.0360 0.042 Uiso 1 1 calc R . . C3 C 0.01257(11) -0.5063(3) 0.03949(15) 0.0330(8) Uani 1 1 d . . . H3A H -0.0101 -0.5139 0.0674 0.040 Uiso 1 1 calc R . . H3B H 0.0311 -0.5881 0.0470 0.040 Uiso 1 1 calc R . . C11 C 0.15665(11) -0.3721(3) 0.25660(15) 0.0295(7) Uani 1 1 d . . . C12 C 0.19936(11) -0.3154(4) 0.28699(16) 0.0353(8) Uani 1 1 d . . . H12 H 0.2093 -0.2421 0.2647 0.042 Uiso 1 1 calc R . . C13 C 0.22710(12) -0.3665(4) 0.34987(17) 0.0423(9) Uani 1 1 d . . . H13 H 0.2560 -0.3274 0.3710 0.051 Uiso 1 1 calc R . . C14 C 0.21307(13) -0.4737(4) 0.38204(17) 0.0458(10) Uani 1 1 d . . . H14 H 0.2325 -0.5092 0.4248 0.055 Uiso 1 1 calc R . . C15 C 0.17094(14) -0.5292(4) 0.35233(18) 0.0470(10) Uani 1 1 d . . . H15 H 0.1613 -0.6027 0.3749 0.056 Uiso 1 1 calc R . . C16 C 0.14257(12) -0.4792(4) 0.28997(17) 0.0382(8) Uani 1 1 d . . . H16 H 0.1134 -0.5180 0.2698 0.046 Uiso 1 1 calc R . . C21 C 0.15098(11) -0.3027(3) 0.10892(15) 0.0291(7) Uani 1 1 d . . . C22 C 0.18079(12) -0.4054(4) 0.10655(17) 0.0366(8) Uani 1 1 d . . . H22 H 0.1878 -0.4699 0.1434 0.044 Uiso 1 1 calc R . . C23 C 0.20027(13) -0.4131(4) 0.04980(19) 0.0447(9) Uani 1 1 d . . . H23 H 0.2205 -0.4835 0.0476 0.054 Uiso 1 1 calc R . . C24 C 0.19015(13) -0.3188(4) -0.00325(18) 0.0447(9) Uani 1 1 d . . . H24 H 0.2036 -0.3243 -0.0419 0.054 Uiso 1 1 calc R . . C25 C 0.16067(12) -0.2164(4) -0.00080(17) 0.0425(9) Uani 1 1 d . . . H25 H 0.1540 -0.1518 -0.0376 0.051 Uiso 1 1 calc R . . C26 C 0.14070(12) -0.2073(4) 0.05505(16) 0.0354(8) Uani 1 1 d . . . H26 H 0.1203 -0.1370 0.0567 0.043 Uiso 1 1 calc R . . C31 C 0.14292(13) -0.0234(3) 0.24280(17) 0.0384(8) Uani 1 1 d . . . C32 C 0.14530(14) 0.0250(4) 0.31040(19) 0.0479(10) Uani 1 1 d . . . H32 H 0.1210 0.0081 0.3313 0.058 Uiso 1 1 calc R . . C33 C 0.18281(15) 0.0978(4) 0.3475(2) 0.0536(11) Uani 1 1 d . . . H33 H 0.1840 0.1304 0.3938 0.064 Uiso 1 1 calc R . . C34 C 0.21846(15) 0.1238(4) 0.3182(2) 0.0513(10) Uani 1 1 d . . . H34 H 0.2441 0.1733 0.3443 0.062 Uiso 1 1 calc R . . C35 C 0.21669(14) 0.0775(4) 0.25090(19) 0.0447(9) Uani 1 1 d . . . H35 H 0.2412 0.0945 0.2305 0.054 Uiso 1 1 calc R . . C36 C 0.17871(13) 0.0055(4) 0.21291(18) 0.0428(9) Uani 1 1 d . . . H36 H 0.1771 -0.0243 0.1660 0.051 Uiso 1 1 calc R . . C41 C 0.05654(12) -0.1609(4) 0.24276(18) 0.0418(9) Uani 1 1 d . . . C42 C 0.00955(14) -0.1587(5) 0.2097(2) 0.0604(12) Uani 1 1 d . . . H42 H -0.0017 -0.1225 0.1632 0.073 Uiso 1 1 calc R . . C43 C -0.02079(17) -0.2101(6) 0.2456(3) 0.0793(16) Uani 1 1 d . . . H43 H -0.0527 -0.2105 0.2230 0.095 Uiso 1 1 calc R . . C44 C -0.0047(2) -0.2599(5) 0.3133(3) 0.0784(16) Uani 1 1 d . . . H44 H -0.0254 -0.2935 0.3377 0.094 Uiso 1 1 calc R . . C45 C 0.04177(18) -0.2612(4) 0.3461(3) 0.0624(12) Uani 1 1 d . . . H45 H 0.0527 -0.2966 0.3929 0.075 Uiso 1 1 calc R . . C46 C 0.07231(14) -0.2120(4) 0.3118(2) 0.0455(9) Uani 1 1 d . . . H46 H 0.1041 -0.2127 0.3351 0.055 Uiso 1 1 calc R . . Ga Ga 0.120178(15) 0.23047(5) 0.01948(2) 0.04881(16) Uani 1 1 d . . . Cl1 Cl 0.09987(4) 0.40491(12) -0.04520(5) 0.0581(3) Uani 1 1 d . . . Cl2 Cl 0.19127(4) 0.18580(14) 0.02687(6) 0.0729(4) Uani 1 1 d . . . Cl3 Cl 0.11590(5) 0.26107(13) 0.12754(6) 0.0788(4) Uani 1 1 d . . . Cl4 Cl 0.07670(6) 0.07070(15) -0.03160(10) 0.1219(7) 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 P1 0.0284(4) 0.0309(5) 0.0202(4) 0.0007(3) 0.0027(3) -0.0007(4) P2 0.0429(5) 0.0352(5) 0.0298(4) 0.0026(4) 0.0041(4) 0.0071(4) C1 0.0274(17) 0.037(2) 0.0274(15) -0.0022(14) 0.0033(13) -0.0037(14) C2 0.0312(18) 0.041(2) 0.0281(16) 0.0012(15) -0.0006(14) 0.0001(15) C3 0.0250(17) 0.040(2) 0.0308(16) -0.0010(15) 0.0014(14) -0.0020(15) C11 0.0335(18) 0.0328(19) 0.0199(14) 0.0007(13) 0.0036(13) 0.0032(15) C12 0.0316(18) 0.042(2) 0.0302(16) 0.0017(15) 0.0053(14) -0.0013(16) C13 0.034(2) 0.057(3) 0.0294(17) -0.0042(17) -0.0031(15) 0.0063(18) C14 0.052(2) 0.058(3) 0.0235(16) 0.0033(17) 0.0045(16) 0.022(2) C15 0.064(3) 0.045(2) 0.0314(18) 0.0101(17) 0.0109(18) 0.005(2) C16 0.039(2) 0.043(2) 0.0298(16) 0.0027(16) 0.0058(15) -0.0036(17) C21 0.0268(17) 0.0359(19) 0.0228(14) -0.0017(14) 0.0035(13) -0.0073(14) C22 0.038(2) 0.042(2) 0.0291(16) 0.0062(15) 0.0092(15) -0.0001(16) C23 0.041(2) 0.052(2) 0.045(2) -0.0017(18) 0.0195(17) 0.0017(18) C24 0.041(2) 0.064(3) 0.0318(17) 0.0000(18) 0.0151(16) -0.009(2) C25 0.041(2) 0.057(3) 0.0255(16) 0.0087(16) 0.0033(15) -0.0082(19) C26 0.0337(19) 0.042(2) 0.0269(16) 0.0026(15) 0.0027(14) -0.0040(16) C31 0.051(2) 0.0279(19) 0.0332(17) 0.0039(15) 0.0060(16) 0.0044(16) C32 0.063(3) 0.043(2) 0.0404(19) -0.0049(18) 0.0195(19) -0.002(2) C33 0.070(3) 0.050(3) 0.039(2) -0.0126(19) 0.012(2) -0.008(2) C34 0.056(3) 0.039(2) 0.052(2) -0.0035(19) 0.003(2) -0.0025(19) C35 0.051(2) 0.037(2) 0.045(2) -0.0002(17) 0.0122(18) -0.0035(18) C36 0.057(2) 0.035(2) 0.0354(18) 0.0004(16) 0.0111(17) -0.0025(18) C41 0.041(2) 0.042(2) 0.044(2) -0.0088(17) 0.0141(17) 0.0078(17) C42 0.049(3) 0.064(3) 0.065(3) -0.012(2) 0.010(2) 0.015(2) C43 0.043(3) 0.091(4) 0.109(4) -0.023(3) 0.031(3) 0.008(3) C44 0.079(4) 0.073(4) 0.105(4) -0.015(3) 0.062(3) -0.005(3) C45 0.076(3) 0.059(3) 0.063(3) -0.006(2) 0.038(3) 0.001(2) C46 0.051(2) 0.046(2) 0.045(2) -0.0030(18) 0.0225(18) 0.0050(19) Ga 0.0453(3) 0.0467(3) 0.0499(3) 0.0006(2) 0.0052(2) 0.0163(2) Cl1 0.0585(6) 0.0650(7) 0.0565(6) 0.0208(5) 0.0253(5) 0.0194(5) Cl2 0.0529(6) 0.1076(10) 0.0500(6) -0.0192(6) 0.0003(5) 0.0394(7) Cl3 0.1071(10) 0.0794(9) 0.0642(7) 0.0305(6) 0.0475(7) 0.0498(8) Cl4 0.1011(11) 0.0589(9) 0.1516(15) 0.0110(9) -0.0573(10) -0.0054(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 P1 C11 1.797(3) . ? P1 C1 1.803(3) . ? P1 C21 1.804(3) . ? P1 P2 2.2114(13) . ? P2 C31 1.830(4) . ? P2 C41 1.836(4) . ? C1 C2 1.534(4) . ? C2 C3 1.515(5) . ? C3 C3 1.524(6) 5_545 ? C11 C16 1.390(5) . ? C11 C12 1.395(4) . ? C12 C13 1.383(4) . ? C13 C14 1.377(5) . ? C14 C15 1.373(5) . ? C15 C16 1.379(5) . ? C21 C22 1.388(5) . ? C21 C26 1.396(5) . ? C22 C23 1.391(5) . ? C23 C24 1.378(5) . ? C24 C25 1.379(6) . ? C25 C26 1.385(5) . ? C31 C32 1.387(5) . ? C31 C36 1.397(5) . ? C32 C33 1.384(5) . ? C33 C34 1.381(6) . ? C34 C35 1.378(5) . ? C35 C36 1.394(5) . ? C41 C46 1.397(5) . ? C41 C42 1.398(5) . ? C42 C43 1.401(7) . ? C43 C44 1.370(8) . ? C44 C45 1.381(7) . ? C45 C46 1.376(6) . ? Ga Cl4 2.1523(15) . ? Ga Cl1 2.1583(11) . ? Ga Cl3 2.1646(12) . ? Ga Cl2 2.1736(12) . ? 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 C1 108.67(15) . . ? C11 P1 C21 108.31(15) . . ? C1 P1 C21 107.05(15) . . ? C11 P1 P2 115.18(11) . . ? C1 P1 P2 107.43(12) . . ? C21 P1 P2 109.90(12) . . ? C31 P2 C41 108.30(16) . . ? C31 P2 P1 101.17(12) . . ? C41 P2 P1 94.57(13) . . ? C2 C1 P1 115.0(2) . . ? C3 C2 C1 110.1(3) . . ? C2 C3 C3 112.4(3) . 5_545 ? C16 C11 C12 119.5(3) . . ? C16 C11 P1 120.5(2) . . ? C12 C11 P1 120.0(3) . . ? C13 C12 C11 119.6(3) . . ? C14 C13 C12 120.5(3) . . ? C15 C14 C13 120.0(3) . . ? C14 C15 C16 120.5(4) . . ? C15 C16 C11 119.9(3) . . ? C22 C21 C26 120.5(3) . . ? C22 C21 P1 119.3(2) . . ? C26 C21 P1 119.7(3) . . ? C21 C22 C23 119.5(3) . . ? C24 C23 C22 120.0(4) . . ? C23 C24 C25 120.6(3) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 119.2(3) . . ? C32 C31 C36 118.4(3) . . ? C32 C31 P2 123.4(3) . . ? C36 C31 P2 117.7(2) . . ? C33 C32 C31 120.4(4) . . ? C34 C33 C32 120.9(4) . . ? C35 C34 C33 119.8(4) . . ? C34 C35 C36 119.6(4) . . ? C35 C36 C31 121.0(3) . . ? C46 C41 C42 119.2(4) . . ? C46 C41 P2 125.9(3) . . ? C42 C41 P2 114.7(3) . . ? C41 C42 C43 119.6(4) . . ? C44 C43 C42 120.3(5) . . ? C43 C44 C45 120.0(5) . . ? C46 C45 C44 120.8(5) . . ? C45 C46 C41 120.1(4) . . ? Cl4 Ga Cl1 107.64(5) . . ? Cl4 Ga Cl3 111.36(8) . . ? Cl1 Ga Cl3 111.50(5) . . ? Cl4 Ga Cl2 110.39(7) . . ? Cl1 Ga Cl2 109.25(5) . . ? Cl3 Ga Cl2 106.71(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 P1 P2 C31 42.28(17) . . . . ? C1 P1 P2 C31 163.51(15) . . . . ? C21 P1 P2 C31 -80.35(15) . . . . ? C11 P1 P2 C41 -67.40(17) . . . . ? C1 P1 P2 C41 53.83(16) . . . . ? C21 P1 P2 C41 169.97(15) . . . . ? C11 P1 C1 C2 -166.0(2) . . . . ? C21 P1 C1 C2 -49.2(3) . . . . ? P2 P1 C1 C2 68.8(3) . . . . ? P1 C1 C2 C3 165.1(2) . . . . ? C1 C2 C3 C3 -173.7(3) . . . 5_545 ? C1 P1 C11 C16 -9.6(3) . . . . ? C21 P1 C11 C16 -125.5(3) . . . . ? P2 P1 C11 C16 111.0(3) . . . . ? C1 P1 C11 C12 171.5(3) . . . . ? C21 P1 C11 C12 55.5(3) . . . . ? P2 P1 C11 C12 -68.0(3) . . . . ? C16 C11 C12 C13 0.0(5) . . . . ? P1 C11 C12 C13 179.0(3) . . . . ? C11 C12 C13 C14 0.8(5) . . . . ? C12 C13 C14 C15 -1.1(6) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C14 C15 C16 C11 0.2(6) . . . . ? C12 C11 C16 C15 -0.5(5) . . . . ? P1 C11 C16 C15 -179.5(3) . . . . ? C11 P1 C21 C22 36.7(3) . . . . ? C1 P1 C21 C22 -80.3(3) . . . . ? P2 P1 C21 C22 163.3(2) . . . . ? C11 P1 C21 C26 -151.2(3) . . . . ? C1 P1 C21 C26 91.8(3) . . . . ? P2 P1 C21 C26 -24.6(3) . . . . ? C26 C21 C22 C23 -0.3(5) . . . . ? P1 C21 C22 C23 171.8(3) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C22 C23 C24 C25 -0.2(6) . . . . ? C23 C24 C25 C26 -0.2(6) . . . . ? C24 C25 C26 C21 0.3(5) . . . . ? C22 C21 C26 C25 -0.1(5) . . . . ? P1 C21 C26 C25 -172.1(3) . . . . ? C41 P2 C31 C32 -18.8(4) . . . . ? P1 P2 C31 C32 -117.5(3) . . . . ? C41 P2 C31 C36 168.9(3) . . . . ? P1 P2 C31 C36 70.2(3) . . . . ? C36 C31 C32 C33 -1.3(6) . . . . ? P2 C31 C32 C33 -173.5(3) . . . . ? C31 C32 C33 C34 0.0(6) . . . . ? C32 C33 C34 C35 0.4(6) . . . . ? C33 C34 C35 C36 0.4(6) . . . . ? C34 C35 C36 C31 -1.7(6) . . . . ? C32 C31 C36 C35 2.1(5) . . . . ? P2 C31 C36 C35 174.8(3) . . . . ? C31 P2 C41 C46 -37.9(4) . . . . ? P1 P2 C41 C46 65.5(3) . . . . ? C31 P2 C41 C42 147.0(3) . . . . ? P1 P2 C41 C42 -109.6(3) . . . . ? C46 C41 C42 C43 -1.4(6) . . . . ? P2 C41 C42 C43 174.1(4) . . . . ? C41 C42 C43 C44 1.3(7) . . . . ? C42 C43 C44 C45 -0.9(8) . . . . ? C43 C44 C45 C46 0.5(7) . . . . ? C44 C45 C46 C41 -0.6(6) . . . . ? C42 C41 C46 C45 1.0(6) . . . . ? P2 C41 C46 C45 -173.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.675 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.079