# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Neil Burford' _publ_contact_author_email NEIL.BURFORD@DAL.CA _publ_section_title ; Phosphinopnictinophosphonium Frameworks ; loop_ _publ_author_name 'Neil Burford' 'Eamonn Conrad' 'Michael J Ferguson' 'Robert McDonald' 'Ulrike Werner-Zwanziger' # Attachment '[SbCl2_PCy_4][Al2Cl7].CIF' data_dal09c6 _database_code_depnum_ccdc_archive 'CCDC 747678' #TrackingRef '[SbCl2_PCy_4][Al2Cl7].CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Al2 Cl9 P4 Sb' _chemical_formula_weight 951.23 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' Al Al 0.0645 0.0514 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 11.9912(5) _cell_length_b 21.7620(9) _cell_length_c 15.6538(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.0720(10) _cell_angle_gamma 90.00 _cell_volume 4084.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9009 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.13 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4920 _exptl_absorpt_correction_T_max 0.7600 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34739 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.14 _reflns_number_total 9046 _reflns_number_gt 7749 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. 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^)+(0.0373P)^2^+5.2046P] 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 9046 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.006 _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 Sb Sb 0.144762(15) 0.717228(9) 1.202288(11) 0.03405(6) Uani 1 1 d . . . Cl1 Cl 0.22824(7) 0.80675(4) 1.25606(5) 0.05032(19) Uani 1 1 d . . . Cl2 Cl -0.03617(6) 0.75633(5) 1.19191(5) 0.0527(2) Uani 1 1 d . . . P1 P 0.20018(6) 0.75134(3) 1.04844(4) 0.03013(14) Uani 1 1 d . . . P2 P 0.36441(6) 0.71327(4) 1.02006(5) 0.03731(17) Uani 1 1 d . A . P3 P 0.26699(6) 0.62706(4) 1.00354(5) 0.04032(18) Uani 1 1 d . . . P4 P 0.13431(5) 0.68868(3) 0.94973(4) 0.02962(14) Uani 1 1 d . A . C11 C 0.1939(3) 0.83414(13) 1.02690(19) 0.0401(6) Uani 1 1 d . . . H11A H 0.2345 0.8554 1.0748 0.048 Uiso 1 1 calc R . . C12 C 0.2530(5) 0.85024(19) 0.9453(3) 0.0818(15) Uani 1 1 d . . . H12A H 0.2146 0.8301 0.8962 0.098 Uiso 1 1 calc R . . H12B H 0.3306 0.8348 0.9484 0.098 Uiso 1 1 calc R . . C13 C 0.2537(5) 0.9203(2) 0.9317(4) 0.0886(16) Uani 1 1 d . . . H13A H 0.2983 0.9401 0.9780 0.106 Uiso 1 1 calc R . . H13B H 0.2892 0.9300 0.8767 0.106 Uiso 1 1 calc R . . C14 C 0.1389(4) 0.94536(19) 0.9313(3) 0.0747(12) Uani 1 1 d . . . H14A H 0.0966 0.9290 0.8814 0.090 Uiso 1 1 calc R . . H14B H 0.1417 0.9907 0.9260 0.090 Uiso 1 1 calc R . . C15 C 0.0801(5) 0.9284(2) 1.0119(5) 0.123(3) Uani 1 1 d . . . H15A H 0.0025 0.9440 1.0090 0.147 Uiso 1 1 calc R . . H15B H 0.1183 0.9481 1.0613 0.147 Uiso 1 1 calc R . . C16 C 0.0784(4) 0.8576(2) 1.0252(4) 0.099(2) Uani 1 1 d . . . H16A H 0.0419 0.8477 1.0796 0.119 Uiso 1 1 calc R . . H16B H 0.0354 0.8379 0.9781 0.119 Uiso 1 1 calc R . . C21 C 0.4388(2) 0.70975(14) 1.12546(17) 0.0362(6) Uani 1 1 d . . . H21A H 0.3851 0.6983 1.1709 0.043 Uiso 1 1 calc R A . C22 C 0.4861(3) 0.77378(15) 1.14349(19) 0.0405(6) Uani 1 1 d . A . H22A H 0.4241 0.8033 1.1502 0.049 Uiso 1 1 calc R . . H22B H 0.5311 0.7873 1.0946 0.049 Uiso 1 1 calc R . . C23 C 0.5593(3) 0.77332(16) 1.2251(2) 0.0462(7) Uani 1 1 d . . . H23A H 0.5919 0.8146 1.2344 0.055 Uiso 1 1 calc R A . H23B H 0.5127 0.7635 1.2749 0.055 Uiso 1 1 calc R . . C24 C 0.6518(3) 0.72652(16) 1.2186(2) 0.0466(8) Uani 1 1 d . A . H24A H 0.6962 0.7261 1.2725 0.056 Uiso 1 1 calc R . . H24B H 0.7019 0.7383 1.1718 0.056 Uiso 1 1 calc R . . C25 C 0.6051(3) 0.66282(16) 1.2015(2) 0.0492(8) Uani 1 1 d . . . H25A H 0.5612 0.6494 1.2511 0.059 Uiso 1 1 calc R A . H25B H 0.6675 0.6335 1.1948 0.059 Uiso 1 1 calc R . . C26 C 0.5309(2) 0.66157(16) 1.1210(2) 0.0443(7) Uani 1 1 d . A . H26A H 0.5769 0.6695 1.0703 0.053 Uiso 1 1 calc R . . H26B H 0.4970 0.6203 1.1145 0.053 Uiso 1 1 calc R . . C31A C 0.3359(5) 0.6085(3) 0.8940(4) 0.0303(12) Uani 0.50 1 d P A 1 H31A H 0.3301 0.6457 0.8566 0.036 Uiso 0.50 1 calc PR A 1 C32A C 0.4576(5) 0.5922(4) 0.9061(5) 0.0539(18) Uani 0.50 1 d P A 1 H32A H 0.4648 0.5593 0.9495 0.065 Uiso 0.50 1 calc PR A 1 H32B H 0.4987 0.6286 0.9278 0.065 Uiso 0.50 1 calc PR A 1 C33A C 0.5096(7) 0.5707(5) 0.8238(7) 0.068(3) Uani 0.50 1 d P A 1 H33A H 0.5875 0.5577 0.8355 0.082 Uiso 0.50 1 calc PR A 1 H33B H 0.5109 0.6051 0.7825 0.082 Uiso 0.50 1 calc PR A 1 C34A C 0.4437(7) 0.5167(4) 0.7847(6) 0.058(2) Uani 0.50 1 d P A 1 H34A H 0.4766 0.5049 0.7295 0.070 Uiso 0.50 1 calc PR A 1 H34B H 0.4484 0.4808 0.8235 0.070 Uiso 0.50 1 calc PR A 1 C35A C 0.3240(6) 0.5343(4) 0.7708(5) 0.055(2) Uani 0.50 1 d P A 1 H35A H 0.2821 0.4984 0.7484 0.066 Uiso 0.50 1 calc PR A 1 H35B H 0.3193 0.5673 0.7272 0.066 Uiso 0.50 1 calc PR A 1 C36A C 0.2694(5) 0.5567(3) 0.8527(4) 0.0462(15) Uani 0.50 1 d P A 1 H36A H 0.1929 0.5713 0.8391 0.055 Uiso 0.50 1 calc PR A 1 H36B H 0.2638 0.5221 0.8934 0.055 Uiso 0.50 1 calc PR A 1 C31B C 0.3205(6) 0.5806(4) 0.9171(5) 0.0416(15) Uani 0.50 1 d P A 2 H31B H 0.2688 0.5449 0.9086 0.050 Uiso 0.50 1 calc PR A 2 C32B C 0.4337(7) 0.5554(4) 0.9426(5) 0.0564(19) Uani 0.50 1 d P A 2 H32C H 0.4273 0.5314 0.9960 0.068 Uiso 0.50 1 calc PR A 2 H32D H 0.4856 0.5900 0.9540 0.068 Uiso 0.50 1 calc PR A 2 C33B C 0.4815(7) 0.5142(4) 0.8726(6) 0.075(3) Uani 0.50 1 d P A 2 H33C H 0.5572 0.5004 0.8900 0.090 Uiso 0.50 1 calc PR A 2 H33D H 0.4338 0.4774 0.8652 0.090 Uiso 0.50 1 calc PR A 2 C34B C 0.4869(10) 0.5480(6) 0.7905(7) 0.072(3) Uani 0.50 1 d P A 2 H34C H 0.5153 0.5203 0.7458 0.086 Uiso 0.50 1 calc PR A 2 H34D H 0.5398 0.5828 0.7967 0.086 Uiso 0.50 1 calc PR A 2 C35B C 0.3741(10) 0.5723(6) 0.7630(5) 0.088(3) Uani 0.50 1 d P A 2 H35C H 0.3226 0.5375 0.7520 0.105 Uiso 0.50 1 calc PR A 2 H35D H 0.3809 0.5960 0.7095 0.105 Uiso 0.50 1 calc PR A 2 C36B C 0.3259(8) 0.6144(4) 0.8343(6) 0.076(3) Uani 0.50 1 d P A 2 H36C H 0.3739 0.6511 0.8416 0.091 Uiso 0.50 1 calc PR A 2 H36D H 0.2503 0.6284 0.8171 0.091 Uiso 0.50 1 calc PR A 2 C41 C 0.0038(2) 0.65581(12) 0.99299(17) 0.0294(5) Uani 1 1 d . . . H41A H 0.0127 0.6503 1.0562 0.035 Uiso 1 1 calc R A . C42 C -0.0160(2) 0.59284(13) 0.9509(2) 0.0381(6) Uani 1 1 d . A . H42A H -0.0207 0.5977 0.8881 0.046 Uiso 1 1 calc R . . H42B H 0.0474 0.5652 0.9647 0.046 Uiso 1 1 calc R . . C43 C -0.1243(2) 0.56439(14) 0.9828(2) 0.0426(7) Uani 1 1 d . . . H43A H -0.1379 0.5249 0.9531 0.051 Uiso 1 1 calc R A . H43B H -0.1165 0.5558 1.0448 0.051 Uiso 1 1 calc R . . C44 C -0.2232(2) 0.60678(15) 0.9672(2) 0.0453(7) Uani 1 1 d . A . H44A H -0.2905 0.5886 0.9928 0.054 Uiso 1 1 calc R . . H44B H -0.2372 0.6109 0.9050 0.054 Uiso 1 1 calc R . . C45 C -0.2022(2) 0.67033(15) 1.0059(2) 0.0463(7) Uani 1 1 d . . . H45A H -0.2654 0.6977 0.9907 0.056 Uiso 1 1 calc R A . H45B H -0.1983 0.6668 1.0689 0.056 Uiso 1 1 calc R . . C46 C -0.0944(2) 0.69859(13) 0.9744(2) 0.0366(6) Uani 1 1 d . A . H46A H -0.0814 0.7385 1.0031 0.044 Uiso 1 1 calc R . . H46B H -0.1008 0.7061 0.9121 0.044 Uiso 1 1 calc R . . Cl3 Cl 0.26719(8) 0.64365(5) 0.55926(5) 0.0586(2) Uani 1 1 d . . . Cl4 Cl 0.08481(7) 0.70507(4) 0.40258(5) 0.04969(19) Uani 1 1 d . . . Cl5 Cl 0.33121(8) 0.63470(6) 0.34135(6) 0.0745(3) Uani 1 1 d . . . Cl6 Cl 0.10977(10) 0.54929(4) 0.42909(6) 0.0668(3) Uani 1 1 d . B . Cl7A Cl -0.0076(6) 0.58152(19) 0.2286(4) 0.1015(18) Uani 0.65 1 d P B 1 Cl8A Cl -0.0491(4) 0.4416(2) 0.3300(3) 0.0899(9) Uani 0.65 1 d P B 1 Cl9A Cl 0.2163(3) 0.47475(19) 0.2575(3) 0.1390(15) Uani 0.65 1 d P B 1 Cl7B Cl -0.0276(14) 0.5844(6) 0.2389(9) 0.128(4) Uani 0.35 1 d P B 2 Cl8B Cl -0.0010(10) 0.4359(5) 0.3085(6) 0.133(4) Uani 0.35 1 d P B 2 Cl9B Cl 0.2150(6) 0.5190(4) 0.2168(4) 0.147(3) Uani 0.35 1 d P B 2 Al1 Al 0.20596(8) 0.63774(5) 0.43369(6) 0.0422(2) Uani 1 1 d . . . Al2 Al 0.06765(11) 0.51223(6) 0.29709(8) 0.0647(3) 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 Sb 0.03379(10) 0.04077(11) 0.02761(10) 0.00094(7) 0.00156(7) 0.00224(7) Cl1 0.0553(5) 0.0574(5) 0.0382(4) -0.0121(3) -0.0015(3) -0.0083(4) Cl2 0.0348(4) 0.0763(6) 0.0472(4) 0.0002(4) 0.0016(3) 0.0098(4) P1 0.0316(3) 0.0334(3) 0.0253(3) 0.0004(3) -0.0010(2) -0.0020(3) P2 0.0261(3) 0.0581(5) 0.0277(3) -0.0028(3) 0.0002(3) -0.0036(3) P3 0.0321(4) 0.0441(4) 0.0444(4) -0.0118(3) -0.0087(3) 0.0104(3) P4 0.0273(3) 0.0359(4) 0.0255(3) -0.0006(3) -0.0022(2) -0.0001(3) C11 0.0509(17) 0.0333(14) 0.0359(15) -0.0014(12) -0.0036(12) -0.0065(12) C12 0.112(4) 0.050(2) 0.085(3) 0.025(2) 0.048(3) 0.013(2) C13 0.101(4) 0.056(3) 0.111(4) 0.033(3) 0.036(3) -0.001(2) C14 0.095(3) 0.049(2) 0.080(3) 0.022(2) -0.009(2) 0.006(2) C15 0.116(4) 0.056(3) 0.199(7) 0.059(4) 0.077(5) 0.040(3) C16 0.065(3) 0.054(2) 0.180(6) 0.052(3) 0.035(3) 0.016(2) C21 0.0277(13) 0.0531(17) 0.0276(13) -0.0008(12) -0.0008(10) -0.0016(12) C22 0.0372(15) 0.0513(18) 0.0328(14) -0.0036(12) -0.0060(12) -0.0001(13) C23 0.0469(17) 0.058(2) 0.0338(15) -0.0066(14) -0.0097(13) -0.0013(14) C24 0.0343(15) 0.069(2) 0.0363(15) 0.0009(14) -0.0104(12) -0.0050(14) C25 0.0385(16) 0.059(2) 0.0497(18) 0.0036(15) -0.0082(13) 0.0054(14) C26 0.0323(14) 0.0534(18) 0.0471(17) -0.0083(14) -0.0040(12) 0.0010(13) C31A 0.031(3) 0.034(4) 0.027(3) -0.007(3) 0.007(2) 0.000(3) C32A 0.033(3) 0.073(5) 0.056(4) -0.031(4) -0.004(3) 0.004(3) C33A 0.042(4) 0.086(7) 0.078(7) -0.051(6) 0.016(4) -0.005(4) C34A 0.057(5) 0.058(5) 0.060(5) -0.027(4) 0.004(4) 0.003(4) C35A 0.039(4) 0.071(5) 0.054(4) -0.030(4) 0.002(3) -0.010(3) C36A 0.034(3) 0.058(4) 0.046(3) -0.022(3) 0.006(3) -0.011(3) C31B 0.045(4) 0.034(4) 0.046(4) -0.006(3) 0.006(3) 0.006(3) C32B 0.051(4) 0.064(5) 0.054(4) -0.006(4) 0.000(3) 0.031(4) C33B 0.064(5) 0.079(6) 0.083(6) -0.021(5) 0.001(4) 0.038(5) C34B 0.067(7) 0.085(9) 0.065(7) -0.020(6) 0.022(5) 0.019(6) C35B 0.103(8) 0.123(9) 0.038(4) -0.016(5) 0.005(5) 0.052(7) C36B 0.094(7) 0.085(6) 0.049(5) -0.014(4) -0.001(4) 0.054(5) C41 0.0261(12) 0.0336(13) 0.0286(12) 0.0016(10) -0.0011(9) 0.0002(10) C42 0.0341(14) 0.0316(14) 0.0486(17) -0.0030(12) -0.0005(12) 0.0026(11) C43 0.0401(16) 0.0351(15) 0.0524(18) 0.0048(13) -0.0032(13) -0.0065(12) C44 0.0307(14) 0.0488(18) 0.0562(19) 0.0059(15) -0.0012(13) -0.0072(13) C45 0.0305(14) 0.0481(18) 0.060(2) 0.0025(15) 0.0065(13) 0.0051(13) C46 0.0305(13) 0.0342(14) 0.0451(16) 0.0017(12) 0.0004(11) 0.0031(11) Cl3 0.0608(5) 0.0738(6) 0.0408(4) 0.0034(4) -0.0090(4) -0.0130(4) Cl4 0.0530(4) 0.0574(5) 0.0390(4) 0.0013(3) 0.0093(3) 0.0107(4) Cl5 0.0544(5) 0.1147(9) 0.0550(5) 0.0225(5) 0.0202(4) 0.0250(5) Cl6 0.1035(8) 0.0513(5) 0.0453(5) 0.0017(4) -0.0100(5) -0.0206(5) Cl7A 0.162(4) 0.0643(16) 0.0752(19) 0.0339(14) -0.067(3) -0.0457(19) Cl8A 0.135(3) 0.0618(14) 0.0729(19) -0.0069(12) 0.0104(14) -0.0483(16) Cl9A 0.0830(16) 0.174(3) 0.161(3) -0.106(3) 0.0167(19) 0.025(2) Cl7B 0.120(5) 0.159(8) 0.105(6) 0.015(5) -0.036(4) -0.054(5) Cl8B 0.235(12) 0.070(3) 0.093(5) -0.010(3) -0.013(5) -0.066(6) Cl9B 0.131(5) 0.204(7) 0.105(4) -0.093(5) 0.038(4) -0.021(5) Al1 0.0434(5) 0.0492(5) 0.0340(4) 0.0032(4) 0.0031(4) -0.0010(4) Al2 0.0723(8) 0.0673(7) 0.0544(7) -0.0197(6) -0.0023(6) -0.0056(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 Sb Cl2 2.3333(8) . ? Sb Cl1 2.3397(8) . ? Sb P1 2.6178(7) . ? P1 C11 1.834(3) . ? P1 P2 2.1897(10) . ? P1 P4 2.1966(10) . ? P2 C21 1.862(3) . ? P2 P3 2.2226(11) . ? P3 C31B 1.816(7) . ? P3 C31A 1.959(6) . ? P3 P4 2.2336(10) . ? P4 C41 1.860(3) . ? C11 C16 1.476(5) . ? C11 C12 1.513(5) . ? C12 C13 1.540(6) . ? C13 C14 1.481(7) . ? C14 C15 1.503(7) . ? C15 C16 1.553(6) . ? C21 C26 1.525(4) . ? C21 C22 1.529(4) . ? C22 C23 1.537(4) . ? C23 C24 1.511(5) . ? C24 C25 1.517(5) . ? C25 C26 1.530(4) . ? C31A C32A 1.510(9) . ? C31A C36A 1.518(8) . ? C32A C33A 1.516(11) . ? C33A C34A 1.536(11) . ? C34A C35A 1.498(11) . ? C35A C36A 1.530(9) . ? C31B C36B 1.491(12) . ? C31B C32B 1.512(10) . ? C32B C33B 1.534(10) . ? C33B C34B 1.484(15) . ? C34B C35B 1.507(14) . ? C35B C36B 1.563(11) . ? C41 C46 1.524(4) . ? C41 C42 1.537(4) . ? C42 C43 1.531(4) . ? C43 C44 1.519(4) . ? C44 C45 1.529(5) . ? C45 C46 1.522(4) . ? Cl3 Al1 2.0894(12) . ? Cl4 Al1 2.1138(13) . ? Cl5 Al1 2.1050(13) . ? Cl6 Al1 2.2444(13) . ? Cl6 Al2 2.2662(14) . ? Cl7A Al2 2.050(4) . ? Cl8A Al2 2.148(4) . ? Cl9A Al2 2.066(3) . ? Cl7B Al2 2.136(13) . ? Cl8B Al2 1.864(9) . ? Cl9B Al2 2.192(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 Cl2 Sb Cl1 96.45(3) . . ? Cl2 Sb P1 94.83(3) . . ? Cl1 Sb P1 88.89(3) . . ? C11 P1 P2 111.61(11) . . ? C11 P1 P4 117.87(10) . . ? P2 P1 P4 86.29(4) . . ? C11 P1 Sb 115.94(10) . . ? P2 P1 Sb 108.91(3) . . ? P4 P1 Sb 112.15(3) . . ? C21 P2 P1 104.68(9) . . ? C21 P2 P3 108.07(10) . . ? P1 P2 P3 82.55(4) . . ? C31B P3 P2 111.4(3) . . ? C31A P3 P2 92.7(2) . . ? C31B P3 P4 108.2(2) . . ? C31A P3 P4 95.9(2) . . ? P2 P3 P4 84.62(4) . . ? C41 P4 P1 106.06(9) . . ? C41 P4 P3 103.31(9) . . ? P1 P4 P3 82.14(3) . . ? C16 C11 C12 111.0(4) . . ? C16 C11 P1 112.3(2) . . ? C12 C11 P1 111.4(2) . . ? C11 C12 C13 110.5(4) . . ? C14 C13 C12 110.9(4) . . ? C13 C14 C15 110.9(4) . . ? C14 C15 C16 111.3(5) . . ? C11 C16 C15 109.4(4) . . ? C26 C21 C22 111.6(2) . . ? C26 C21 P2 108.8(2) . . ? C22 C21 P2 107.2(2) . . ? C21 C22 C23 110.6(3) . . ? C24 C23 C22 110.9(3) . . ? C23 C24 C25 111.0(3) . . ? C24 C25 C26 111.6(3) . . ? C21 C26 C25 111.2(3) . . ? C32A C31A C36A 112.2(6) . . ? C32A C31A P3 111.2(5) . . ? C36A C31A P3 107.4(4) . . ? C31A C32A C33A 112.2(6) . . ? C32A C33A C34A 111.0(8) . . ? C35A C34A C33A 110.3(8) . . ? C34A C35A C36A 112.6(6) . . ? C31A C36A C35A 111.4(5) . . ? C36B C31B C32B 110.8(7) . . ? C36B C31B P3 113.2(5) . . ? C32B C31B P3 109.4(5) . . ? C31B C32B C33B 111.6(6) . . ? C34B C33B C32B 110.6(8) . . ? C33B C34B C35B 111.5(9) . . ? C34B C35B C36B 110.1(8) . . ? C31B C36B C35B 110.7(7) . . ? C46 C41 C42 110.5(2) . . ? C46 C41 P4 110.32(18) . . ? C42 C41 P4 108.11(18) . . ? C43 C42 C41 110.2(2) . . ? C44 C43 C42 111.5(2) . . ? C43 C44 C45 111.3(3) . . ? C46 C45 C44 111.8(3) . . ? C45 C46 C41 110.4(2) . . ? Al1 Cl6 Al2 116.11(6) . . ? Cl3 Al1 Cl5 113.91(6) . . ? Cl3 Al1 Cl4 113.70(6) . . ? Cl5 Al1 Cl4 111.08(5) . . ? Cl3 Al1 Cl6 104.74(5) . . ? Cl5 Al1 Cl6 108.90(6) . . ? Cl4 Al1 Cl6 103.68(6) . . ? Cl7A Al2 Cl9A 120.5(3) . . ? Cl8B Al2 Cl7B 117.6(5) . . ? Cl7A Al2 Cl8A 111.7(3) . . ? Cl9A Al2 Cl8A 111.08(19) . . ? Cl8B Al2 Cl9B 118.5(4) . . ? Cl7B Al2 Cl9B 97.8(5) . . ? Cl8B Al2 Cl6 108.7(3) . . ? Cl7A Al2 Cl6 107.68(18) . . ? Cl9A Al2 Cl6 103.59(12) . . ? Cl7B Al2 Cl6 103.6(4) . . ? Cl8A Al2 Cl6 99.83(13) . . ? Cl9B Al2 Cl6 109.33(18) . . ? 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 Cl2 Sb P1 C11 60.39(12) . . . . ? Cl1 Sb P1 C11 -35.99(11) . . . . ? Cl2 Sb P1 P2 -172.77(4) . . . . ? Cl1 Sb P1 P2 90.85(4) . . . . ? Cl2 Sb P1 P4 -79.01(4) . . . . ? Cl1 Sb P1 P4 -175.39(4) . . . . ? C11 P1 P2 C21 98.13(14) . . . . ? P4 P1 P2 C21 -143.30(10) . . . . ? Sb P1 P2 C21 -31.14(11) . . . . ? C11 P1 P2 P3 -155.06(11) . . . . ? P4 P1 P2 P3 -36.49(4) . . . . ? Sb P1 P2 P3 75.67(4) . . . . ? C21 P2 P3 C31B -113.6(3) . . . . ? P1 P2 P3 C31B 143.3(3) . . . . ? C21 P2 P3 C31A -125.4(2) . . . . ? P1 P2 P3 C31A 131.6(2) . . . . ? C21 P2 P3 P4 138.96(10) . . . . ? P1 P2 P3 P4 35.89(3) . . . . ? C11 P1 P4 C41 -109.49(14) . . . . ? P2 P1 P4 C41 137.97(9) . . . . ? Sb P1 P4 C41 29.06(9) . . . . ? C11 P1 P4 P3 148.85(12) . . . . ? P2 P1 P4 P3 36.32(4) . . . . ? Sb P1 P4 P3 -72.60(4) . . . . ? C31B P3 P4 C41 108.7(3) . . . . ? C31A P3 P4 C41 127.3(2) . . . . ? P2 P3 P4 C41 -140.52(9) . . . . ? C31B P3 P4 P1 -146.6(3) . . . . ? C31A P3 P4 P1 -127.9(2) . . . . ? P2 P3 P4 P1 -35.79(3) . . . . ? P2 P1 C11 C16 166.0(3) . . . . ? P4 P1 C11 C16 68.5(4) . . . . ? Sb P1 C11 C16 -68.5(4) . . . . ? P2 P1 C11 C12 40.9(3) . . . . ? P4 P1 C11 C12 -56.6(3) . . . . ? Sb P1 C11 C12 166.3(3) . . . . ? C16 C11 C12 C13 58.1(6) . . . . ? P1 C11 C12 C13 -176.1(4) . . . . ? C11 C12 C13 C14 -56.3(6) . . . . ? C12 C13 C14 C15 55.8(6) . . . . ? C13 C14 C15 C16 -56.5(7) . . . . ? C12 C11 C16 C15 -57.9(6) . . . . ? P1 C11 C16 C15 176.8(4) . . . . ? C14 C15 C16 C11 57.3(7) . . . . ? P1 P2 C21 C26 156.92(19) . . . . ? P3 P2 C21 C26 70.1(2) . . . . ? P1 P2 C21 C22 -82.22(19) . . . . ? P3 P2 C21 C22 -169.04(17) . . . . ? C26 C21 C22 C23 -55.0(3) . . . . ? P2 C21 C22 C23 -174.1(2) . . . . ? C21 C22 C23 C24 56.6(4) . . . . ? C22 C23 C24 C25 -57.2(4) . . . . ? C23 C24 C25 C26 56.3(4) . . . . ? C22 C21 C26 C25 54.0(3) . . . . ? P2 C21 C26 C25 172.1(2) . . . . ? C24 C25 C26 C21 -54.4(4) . . . . ? P2 P3 C31A C32A 68.8(6) . . . . ? P4 P3 C31A C32A 153.6(5) . . . . ? P2 P3 C31A C36A -168.1(5) . . . . ? P4 P3 C31A C36A -83.3(5) . . . . ? C36A C31A C32A C33A 53.2(10) . . . . ? P3 C31A C32A C33A 173.5(7) . . . . ? C31A C32A C33A C34A -55.2(12) . . . . ? C32A C33A C34A C35A 56.2(12) . . . . ? C33A C34A C35A C36A -55.9(11) . . . . ? C32A C31A C36A C35A -51.7(9) . . . . ? P3 C31A C36A C35A -174.1(6) . . . . ? C34A C35A C36A C31A 54.0(10) . . . . ? P2 P3 C31B C36B -55.0(7) . . . . ? P4 P3 C31B C36B 36.3(7) . . . . ? P2 P3 C31B C32B 69.1(7) . . . . ? P4 P3 C31B C32B 160.4(6) . . . . ? C36B C31B C32B C33B -56.0(10) . . . . ? P3 C31B C32B C33B 178.4(7) . . . . ? C31B C32B C33B C34B 56.1(12) . . . . ? C32B C33B C34B C35B -56.9(14) . . . . ? C33B C34B C35B C36B 56.9(15) . . . . ? C32B C31B C36B C35B 55.8(11) . . . . ? P3 C31B C36B C35B 179.2(7) . . . . ? C34B C35B C36B C31B -56.3(14) . . . . ? P1 P4 C41 C46 85.25(19) . . . . ? P3 P4 C41 C46 170.77(17) . . . . ? P1 P4 C41 C42 -153.81(16) . . . . ? P3 P4 C41 C42 -68.30(18) . . . . ? C46 C41 C42 C43 -57.9(3) . . . . ? P4 C41 C42 C43 -178.7(2) . . . . ? C41 C42 C43 C44 56.3(3) . . . . ? C42 C43 C44 C45 -54.5(4) . . . . ? C43 C44 C45 C46 54.5(4) . . . . ? C44 C45 C46 C41 -56.1(3) . . . . ? C42 C41 C46 C45 57.8(3) . . . . ? P4 C41 C46 C45 177.3(2) . . . . ? Al2 Cl6 Al1 Cl3 -164.33(7) . . . . ? Al2 Cl6 Al1 Cl5 -42.12(9) . . . . ? Al2 Cl6 Al1 Cl4 76.21(8) . . . . ? Al1 Cl6 Al2 Cl8B 175.3(4) . . . . ? Al1 Cl6 Al2 Cl7A -52.0(2) . . . . ? Al1 Cl6 Al2 Cl9A 76.68(16) . . . . ? Al1 Cl6 Al2 Cl7B -58.9(4) . . . . ? Al1 Cl6 Al2 Cl8A -168.64(17) . . . . ? Al1 Cl6 Al2 Cl9B 44.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.796 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.075 # Attachment '[Sb2Cl2{_PCy_4}2][AlCl4]2.cif' data_dal0903 _database_code_depnum_ccdc_archive 'CCDC 747679' #TrackingRef '[Sb2Cl2{_PCy_4}2][AlCl4]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H88 Cl2 P8 Sb2, 2(Al Cl4), C7 H8' _chemical_formula_sum 'C55 H96 Al2 Cl10 P8 Sb2' _chemical_formula_weight 1657.04 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' Al Al 0.0645 0.0514 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.0664(7) _cell_length_b 21.3906(13) _cell_length_c 14.9019(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.6473(7) _cell_angle_gamma 90.00 _cell_volume 3721.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9973 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.79 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 1.314 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5318 _exptl_absorpt_correction_T_max 0.7931 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28434 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.55 _reflns_number_total 7740 _reflns_number_gt 6589 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. 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^)+(0.0424P)^2^+13.5259P] 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 7740 _refine_ls_number_parameters 318 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 Sb Sb 0.56710(3) 0.475087(14) 0.43941(2) 0.03451(11) Uani 1 1 d . . . Cl1 Cl 0.70909(10) 0.55355(5) 0.48021(9) 0.0388(3) Uani 1 1 d . . . P1 P 0.45358(11) 0.56244(6) 0.30407(8) 0.0342(3) Uani 1 1 d . B . P2 P 0.40307(11) 0.65351(5) 0.35259(9) 0.0353(3) Uani 1 1 d . . . P3 P 0.29199(10) 0.58749(5) 0.40414(8) 0.0325(3) Uani 1 1 d . . . P4 P 0.26604(11) 0.54659(6) 0.26357(9) 0.0350(3) Uani 1 1 d . . . C11 C 0.5096(5) 0.5692(3) 0.1997(4) 0.0490(13) Uani 1 1 d . . . H11A H 0.4956 0.5280 0.1671 0.059 Uiso 0.55 1 calc PR A 1 H11B H 0.5379 0.5268 0.1879 0.059 Uiso 0.45 1 calc PR A 2 C12A C 0.6370(12) 0.5803(7) 0.2227(10) 0.072(4) Uiso 0.55 1 d P B 1 H12A H 0.6772 0.5485 0.2675 0.087 Uiso 0.55 1 calc PR B 1 H12B H 0.6552 0.6221 0.2511 0.087 Uiso 0.55 1 calc PR B 1 C13A C 0.6769(15) 0.5761(8) 0.1316(11) 0.087(4) Uiso 0.55 1 d P B 1 H13A H 0.7603 0.5842 0.1456 0.104 Uiso 0.55 1 calc PR B 1 H13B H 0.6630 0.5332 0.1062 0.104 Uiso 0.55 1 calc PR B 1 C14A C 0.6148(13) 0.6224(7) 0.0594(10) 0.067(4) Uiso 0.55 1 d P B 1 H14A H 0.6393 0.6160 0.0015 0.080 Uiso 0.55 1 calc PR B 1 H14B H 0.6370 0.6653 0.0817 0.080 Uiso 0.55 1 calc PR B 1 C15A C 0.4853(15) 0.6164(9) 0.0382(11) 0.080(4) Uiso 0.55 1 d P B 1 H15A H 0.4612 0.5760 0.0069 0.096 Uiso 0.55 1 calc PR B 1 H15B H 0.4490 0.6504 -0.0043 0.096 Uiso 0.55 1 calc PR B 1 C16A C 0.4450(11) 0.6200(7) 0.1288(9) 0.064(3) Uiso 0.55 1 d P B 1 H16A H 0.3614 0.6127 0.1149 0.077 Uiso 0.55 1 calc PR B 1 H16B H 0.4610 0.6621 0.1565 0.077 Uiso 0.55 1 calc PR B 1 C12B C 0.6137(12) 0.6122(7) 0.2235(9) 0.052(3) Uiso 0.45 1 d P B 2 H12C H 0.6695 0.5970 0.2799 0.062 Uiso 0.45 1 calc PR B 2 H12D H 0.5901 0.6551 0.2355 0.062 Uiso 0.45 1 calc PR B 2 C13B C 0.6689(14) 0.6124(8) 0.1401(11) 0.062(4) Uiso 0.45 1 d P B 2 H13C H 0.6944 0.5699 0.1285 0.074 Uiso 0.45 1 calc PR B 2 H13D H 0.7357 0.6409 0.1521 0.074 Uiso 0.45 1 calc PR B 2 C14B C 0.569(2) 0.6367(10) 0.0522(14) 0.084(6) Uiso 0.45 1 d P B 2 H14C H 0.5314 0.6746 0.0685 0.100 Uiso 0.45 1 calc PR B 2 H14D H 0.6007 0.6462 -0.0014 0.100 Uiso 0.45 1 calc PR B 2 C15B C 0.4878(18) 0.5843(11) 0.0310(15) 0.087(6) Uiso 0.45 1 d P B 2 H15C H 0.5282 0.5440 0.0314 0.104 Uiso 0.45 1 calc PR B 2 H15D H 0.4325 0.5899 -0.0300 0.104 Uiso 0.45 1 calc PR B 2 C16B C 0.4240(12) 0.5877(7) 0.1152(10) 0.054(3) Uiso 0.45 1 d P B 2 H16C H 0.3964 0.6306 0.1214 0.064 Uiso 0.45 1 calc PR B 2 H16D H 0.3577 0.5588 0.1031 0.064 Uiso 0.45 1 calc PR B 2 C21 C 0.5131(4) 0.6762(2) 0.4592(3) 0.0375(11) Uiso 1 1 d . . . H21 H 0.5441 0.6376 0.4945 0.045 Uiso 1 1 calc R . . C22 C 0.6106(4) 0.7106(2) 0.4327(4) 0.0471(13) Uani 1 1 d . . . H22A H 0.5800 0.7471 0.3935 0.057 Uiso 1 1 calc R . . H22B H 0.6482 0.6825 0.3966 0.057 Uiso 1 1 calc R . . C23 C 0.6980(6) 0.7323(3) 0.5209(5) 0.0678(20) Uani 1 1 d . . . H23A H 0.7341 0.6952 0.5563 0.081 Uiso 1 1 calc R . . H23B H 0.7590 0.7567 0.5033 0.081 Uiso 1 1 calc R . . C24 C 0.6446(7) 0.7714(4) 0.5811(5) 0.080(2) Uani 1 1 d . . . H24A H 0.6166 0.8109 0.5487 0.096 Uiso 1 1 calc R . . H24B H 0.7029 0.7820 0.6388 0.096 Uiso 1 1 calc R . . C25 C 0.5463(7) 0.7380(3) 0.6055(4) 0.075(2) Uani 1 1 d . . . H25A H 0.5095 0.7664 0.6418 0.090 Uiso 1 1 calc R . . H25B H 0.5758 0.7012 0.6446 0.090 Uiso 1 1 calc R . . C26 C 0.4575(5) 0.7166(3) 0.5188(4) 0.0502(14) Uani 1 1 d . . . H26A H 0.3965 0.6925 0.5370 0.060 Uiso 1 1 calc R . . H26B H 0.4218 0.7535 0.4828 0.060 Uiso 1 1 calc R . . C31 C 0.1618(4) 0.6284(2) 0.4180(3) 0.0378(11) Uani 1 1 d . . . H31 H 0.1787 0.6427 0.4840 0.045 Uiso 1 1 calc R . . C32 C 0.1315(5) 0.6865(3) 0.3583(5) 0.0564(15) Uani 1 1 d . . . H32A H 0.1162 0.6749 0.2920 0.068 Uiso 1 1 calc R . . H32B H 0.1970 0.7160 0.3725 0.068 Uiso 1 1 calc R . . C33 C 0.0259(6) 0.7183(3) 0.3766(5) 0.0694(19) Uani 1 1 d . . . H33A H 0.0444 0.7342 0.4410 0.083 Uiso 1 1 calc R . . H33B H 0.0042 0.7544 0.3342 0.083 Uiso 1 1 calc R . . C34 C -0.0736(6) 0.6737(4) 0.3622(6) 0.077(2) Uani 1 1 d . . . H34A H -0.1393 0.6951 0.3775 0.092 Uiso 1 1 calc R . . H34B H -0.0971 0.6611 0.2962 0.092 Uiso 1 1 calc R . . C35 C -0.0433(6) 0.6170(4) 0.4213(7) 0.086(3) Uani 1 1 d . . . H35A H -0.1094 0.5880 0.4083 0.103 Uiso 1 1 calc R . . H35B H -0.0272 0.6293 0.4874 0.103 Uiso 1 1 calc R . . C36 C 0.0611(5) 0.5834(3) 0.4040(5) 0.0604(16) Uani 1 1 d . . . H36A H 0.0819 0.5477 0.4473 0.072 Uiso 1 1 calc R . . H36B H 0.0425 0.5668 0.3399 0.072 Uiso 1 1 calc R . . C41 C 0.2477(4) 0.4601(2) 0.2694(3) 0.0343(10) Uani 1 1 d . . . H41 H 0.3073 0.4425 0.3227 0.041 Uiso 1 1 calc R . . C42 C 0.2636(5) 0.4335(2) 0.1774(4) 0.0428(12) Uani 1 1 d . . . H42A H 0.2096 0.4542 0.1246 0.051 Uiso 1 1 calc R . . H42B H 0.3425 0.4420 0.1725 0.051 Uiso 1 1 calc R . . C43 C 0.2418(5) 0.3628(3) 0.1730(4) 0.0527(14) Uani 1 1 d . . . H43A H 0.2470 0.3469 0.1118 0.063 Uiso 1 1 calc R . . H43B H 0.3019 0.3419 0.2212 0.063 Uiso 1 1 calc R . . C44 C 0.1255(5) 0.3466(2) 0.1873(4) 0.0559(15) Uani 1 1 d . . . H44A H 0.0651 0.3625 0.1343 0.067 Uiso 1 1 calc R . . H44B H 0.1177 0.3005 0.1892 0.067 Uiso 1 1 calc R . . C45 C 0.1088(5) 0.3741(2) 0.2758(4) 0.0498(14) Uani 1 1 d . . . H45A H 0.1627 0.3540 0.3292 0.060 Uiso 1 1 calc R . . H45B H 0.0299 0.3651 0.2804 0.060 Uiso 1 1 calc R . . C46 C 0.1282(4) 0.4448(2) 0.2808(4) 0.0411(11) Uani 1 1 d . . . H46A H 0.1204 0.4607 0.3413 0.049 Uiso 1 1 calc R . . H46B H 0.0696 0.4655 0.2311 0.049 Uiso 1 1 calc R . . Cl2 Cl 0.55742(14) 0.38495(9) 0.22969(13) 0.0702(5) Uani 1 1 d . . . Cl3 Cl 0.82213(18) 0.44464(9) 0.33969(15) 0.0839(6) Uani 1 1 d . . . Cl4 Cl 0.7780(3) 0.28589(11) 0.3377(2) 0.1285(11) Uani 1 1 d . . . Cl5 Cl 0.7875(2) 0.36041(15) 0.13448(15) 0.1126(9) Uani 1 1 d . . . Al Al 0.73797(16) 0.36868(8) 0.25838(13) 0.0535(4) Uani 1 1 d . . . C10S C -0.0281(13) 0.5960(6) 0.1104(10) 0.0852(18) Uiso 0.50 1 d PD C -1 H10A H -0.0694 0.6300 0.0719 0.102 Uiso 0.50 1 calc PR C -1 H10B H 0.0445 0.6119 0.1491 0.102 Uiso 0.50 1 calc PR C -1 H10C H -0.0748 0.5796 0.1501 0.102 Uiso 0.50 1 calc PR C -1 C11S C -0.0045(10) 0.5449(5) 0.0493(9) 0.0852(18) Uiso 0.50 1 d PGD C -1 C12S C 0.0807(10) 0.5508(5) 0.0020(9) 0.0852(18) Uiso 0.50 1 d PGD C -1 H12S H 0.1269 0.5873 0.0097 0.102 Uiso 0.50 1 calc PR C -1 C13S C 0.0981(10) 0.5032(6) -0.0564(8) 0.0852(18) Uiso 0.50 1 d PG C -1 H13S H 0.1563 0.5072 -0.0887 0.102 Uiso 0.50 1 calc PR C -1 C14S C 0.0305(11) 0.4498(5) -0.0677(8) 0.0852(18) Uiso 0.50 1 d PG C -1 H14S H 0.0424 0.4173 -0.1076 0.102 Uiso 0.50 1 calc PR C -1 C15S C -0.0547(11) 0.4439(5) -0.0204(9) 0.0852(18) Uiso 0.50 1 d PG C -1 H15S H -0.1009 0.4074 -0.0281 0.102 Uiso 0.50 1 calc PR C -1 C16S C -0.0721(10) 0.4915(5) 0.0381(9) 0.0852(18) Uiso 0.50 1 d PGD C -1 H16S H -0.1303 0.4875 0.0703 0.102 Uiso 0.50 1 calc PR C -1 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 Sb 0.03833(19) 0.03046(17) 0.03361(17) -0.00337(13) 0.00699(13) -0.00121(13) Cl1 0.0357(6) 0.0344(6) 0.0440(6) 0.0024(5) 0.0063(5) -0.0038(5) P1 0.0329(6) 0.0354(6) 0.0314(6) 0.0032(5) 0.0031(5) -0.0013(5) P2 0.0360(7) 0.0264(6) 0.0387(7) 0.0038(5) 0.0005(5) -0.0034(5) P3 0.0333(6) 0.0259(6) 0.0353(6) 0.0017(5) 0.0032(5) -0.0005(5) P4 0.0329(6) 0.0312(6) 0.0357(6) -0.0013(5) -0.0009(5) -0.0019(5) C11 0.050(3) 0.057(3) 0.040(3) 0.005(2) 0.009(2) -0.002(3) C22 0.036(3) 0.035(3) 0.063(3) 0.003(2) -0.003(2) -0.007(2) C23 0.058(4) 0.055(4) 0.070(4) 0.009(3) -0.021(3) -0.021(3) C24 0.090(5) 0.071(5) 0.064(4) -0.015(4) -0.007(4) -0.040(4) C25 0.101(6) 0.072(4) 0.042(3) -0.009(3) -0.001(3) -0.026(4) C26 0.062(4) 0.043(3) 0.039(3) -0.002(2) -0.001(3) -0.008(3) C31 0.037(3) 0.037(3) 0.040(3) 0.001(2) 0.010(2) 0.004(2) C32 0.051(3) 0.045(3) 0.076(4) 0.014(3) 0.022(3) 0.014(3) C33 0.065(4) 0.057(4) 0.090(5) 0.011(4) 0.027(4) 0.026(3) C34 0.041(4) 0.090(5) 0.098(6) -0.011(4) 0.013(4) 0.015(4) C35 0.057(4) 0.072(5) 0.146(8) -0.014(5) 0.059(5) -0.010(4) C36 0.047(3) 0.053(3) 0.091(5) -0.002(3) 0.034(3) -0.004(3) C41 0.031(2) 0.031(2) 0.034(2) -0.0005(19) -0.0050(19) -0.0006(18) C42 0.049(3) 0.034(3) 0.041(3) -0.007(2) 0.004(2) 0.003(2) C43 0.060(4) 0.039(3) 0.053(3) -0.009(2) 0.001(3) 0.004(3) C44 0.057(4) 0.030(3) 0.067(4) -0.008(3) -0.010(3) -0.006(2) C45 0.040(3) 0.041(3) 0.059(3) 0.005(3) -0.004(3) -0.008(2) C46 0.033(3) 0.040(3) 0.045(3) -0.003(2) -0.001(2) -0.003(2) Cl2 0.0578(9) 0.0807(11) 0.0722(10) -0.0236(9) 0.0169(8) 0.0034(8) Cl3 0.0813(12) 0.0734(12) 0.1033(15) -0.0438(11) 0.0347(11) -0.0187(10) Cl4 0.163(3) 0.0682(13) 0.118(2) 0.0148(13) -0.0305(18) 0.0167(15) Cl5 0.0941(15) 0.182(3) 0.0690(12) -0.0356(14) 0.0334(11) 0.0421(16) Al 0.0600(11) 0.0494(10) 0.0498(10) -0.0153(8) 0.0114(8) 0.0090(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 Sb Cl1 2.3654(12) . ? Sb P1 2.8353(12) . ? Sb P3 2.8484(12) 3_666 ? Sb Sb 2.9150(6) 3_666 ? Sb Cl2 3.6489(17) . ? P1 C11 1.851(6) . ? P1 P4 2.2157(17) . ? P1 P2 2.2161(18) . ? P2 C21 1.859(5) . ? P2 P3 2.2139(17) . ? P3 C31 1.856(5) . ? P3 P4 2.2180(18) . ? P3 Sb 2.8484(12) 3_666 ? P4 C41 1.868(5) . ? C11 C16B 1.467(15) . ? C11 C12A 1.507(15) . ? C11 C12B 1.524(15) . ? C11 C16A 1.577(14) . ? C12A C13A 1.55(2) . ? C13A C14A 1.51(2) . ? C14A C15A 1.52(2) . ? C15A C16A 1.55(2) . ? C12B C13B 1.55(2) . ? C13B C14B 1.63(3) . ? C14B C15B 1.47(3) . ? C15B C16B 1.63(2) . ? C21 C26 1.512(7) . ? C21 C22 1.522(7) . ? C22 C23 1.535(8) . ? C23 C24 1.488(11) . ? C24 C25 1.505(10) . ? C25 C26 1.526(8) . ? C31 C32 1.518(7) . ? C31 C36 1.523(7) . ? C32 C33 1.528(8) . ? C33 C34 1.505(10) . ? C34 C35 1.489(11) . ? C35 C36 1.529(8) . ? C41 C46 1.529(7) . ? C41 C42 1.542(7) . ? C42 C43 1.534(7) . ? C43 C44 1.512(9) . ? C44 C45 1.503(8) . ? C45 C46 1.528(7) . ? Cl2 Al 2.140(3) . ? Cl3 Al 2.125(2) . ? Cl4 Al 2.116(3) . ? Cl5 Al 2.087(3) . ? C10S C11S 1.496(4) . ? C11S C12S 1.3900 . ? C11S C16S 1.3900 . ? C12S C13S 1.3900 . ? C13S C14S 1.3900 . ? C14S C15S 1.3900 . ? C15S C16S 1.3900 . ? 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 Cl1 Sb P1 84.46(4) . . ? Cl1 Sb P3 83.07(4) . 3_666 ? P1 Sb P3 166.65(4) . 3_666 ? Cl1 Sb Sb 93.50(3) . 3_666 ? P1 Sb Sb 87.45(3) . 3_666 ? P3 Sb Sb 88.56(3) 3_666 3_666 ? Cl1 Sb Cl2 117.34(4) . . ? P1 Sb Cl2 80.44(4) . . ? P3 Sb Cl2 109.63(4) 3_666 . ? Sb Sb Cl2 145.21(3) 3_666 . ? C11 P1 P4 110.36(19) . . ? C11 P1 P2 113.2(2) . . ? P4 P1 P2 82.95(6) . . ? C11 P1 Sb 115.83(19) . . ? P4 P1 Sb 111.67(6) . . ? P2 P1 Sb 118.06(6) . . ? C21 P2 P3 103.55(16) . . ? C21 P2 P1 108.20(17) . . ? P3 P2 P1 78.06(6) . . ? C31 P3 P2 109.97(16) . . ? C31 P3 P4 111.72(17) . . ? P2 P3 P4 82.95(6) . . ? C31 P3 Sb 118.54(16) . 3_666 ? P2 P3 Sb 107.17(6) . 3_666 ? P4 P3 Sb 120.01(6) . 3_666 ? C41 P4 P1 105.31(16) . . ? C41 P4 P3 109.66(16) . . ? P1 P4 P3 77.98(6) . . ? C16B C11 C12B 113.4(9) . . ? C12A C11 C16A 110.3(8) . . ? C16B C11 P1 114.5(6) . . ? C12A C11 P1 112.9(6) . . ? C12B C11 P1 107.8(6) . . ? C16A C11 P1 113.1(6) . . ? C11 C12A C13A 108.4(11) . . ? C14A C13A C12A 112.1(13) . . ? C13A C14A C15A 113.0(13) . . ? C14A C15A C16A 110.3(13) . . ? C15A C16A C11 109.8(10) . . ? C11 C12B C13B 108.1(11) . . ? C12B C13B C14B 105.4(13) . . ? C15B C14B C13B 104.4(16) . . ? C14B C15B C16B 102.7(16) . . ? C11 C16B C15B 106.4(12) . . ? C26 C21 C22 111.3(4) . . ? C26 C21 P2 108.9(3) . . ? C22 C21 P2 109.6(3) . . ? C21 C22 C23 109.4(5) . . ? C24 C23 C22 112.2(6) . . ? C23 C24 C25 111.5(6) . . ? C24 C25 C26 111.5(6) . . ? C21 C26 C25 110.3(5) . . ? C32 C31 C36 111.9(5) . . ? C32 C31 P3 113.9(4) . . ? C36 C31 P3 110.8(4) . . ? C31 C32 C33 110.3(5) . . ? C34 C33 C32 111.4(6) . . ? C35 C34 C33 111.4(6) . . ? C34 C35 C36 111.9(6) . . ? C31 C36 C35 110.0(5) . . ? C46 C41 C42 110.6(4) . . ? C46 C41 P4 110.1(3) . . ? C42 C41 P4 106.3(3) . . ? C43 C42 C41 110.1(5) . . ? C44 C43 C42 112.1(5) . . ? C45 C44 C43 111.7(4) . . ? C44 C45 C46 112.2(5) . . ? C45 C46 C41 110.2(4) . . ? Al Cl2 Sb 95.99(7) . . ? Cl5 Al Cl4 110.31(15) . . ? Cl5 Al Cl3 111.52(14) . . ? Cl4 Al Cl3 108.23(13) . . ? Cl5 Al Cl2 109.98(11) . . ? Cl4 Al Cl2 108.95(14) . . ? Cl3 Al Cl2 107.77(10) . . ? C12S C11S C16S 120.0 . . ? C12S C11S C10S 121.4(4) . . ? C16S C11S C10S 118.5(4) . . ? C13S C12S C11S 120.0 . . ? C14S C13S C12S 120.0 . . ? C13S C14S C15S 120.0 . . ? C14S C15S C16S 120.0 . . ? C15S C16S C11S 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Sb P1 C11 77.6(2) . . . . ? P3 Sb P1 C11 98.6(3) 3_666 . . . ? Sb Sb P1 C11 171.4(2) 3_666 . . . ? Cl2 Sb P1 C11 -41.4(2) . . . . ? Cl1 Sb P1 P4 -154.92(7) . . . . ? P3 Sb P1 P4 -133.92(15) 3_666 . . . ? Sb Sb P1 P4 -61.15(6) 3_666 . . . ? Cl2 Sb P1 P4 86.11(6) . . . . ? Cl1 Sb P1 P2 -61.36(7) . . . . ? P3 Sb P1 P2 -40.4(2) 3_666 . . . ? Sb Sb P1 P2 32.41(6) 3_666 . . . ? Cl2 Sb P1 P2 179.68(7) . . . . ? C11 P1 P2 C21 -106.0(3) . . . . ? P4 P1 P2 C21 144.83(17) . . . . ? Sb P1 P2 C21 33.99(18) . . . . ? C11 P1 P2 P3 153.5(2) . . . . ? P4 P1 P2 P3 44.32(6) . . . . ? Sb P1 P2 P3 -66.53(6) . . . . ? C21 P2 P3 C31 99.0(2) . . . . ? P1 P2 P3 C31 -154.85(18) . . . . ? C21 P2 P3 P4 -150.36(17) . . . . ? P1 P2 P3 P4 -44.26(6) . . . . ? C21 P2 P3 Sb -31.07(17) . . . 3_666 ? P1 P2 P3 Sb 75.03(6) . . . 3_666 ? C11 P1 P4 C41 96.2(3) . . . . ? P2 P1 P4 C41 -151.59(17) . . . . ? Sb P1 P4 C41 -34.14(17) . . . . ? C11 P1 P4 P3 -156.4(2) . . . . ? P2 P1 P4 P3 -44.23(6) . . . . ? Sb P1 P4 P3 73.22(6) . . . . ? C31 P3 P4 C41 -104.8(2) . . . . ? P2 P3 P4 C41 146.44(17) . . . . ? Sb P3 P4 C41 40.65(18) 3_666 . . . ? C31 P3 P4 P1 153.02(17) . . . . ? P2 P3 P4 P1 44.28(6) . . . . ? Sb P3 P4 P1 -61.51(7) 3_666 . . . ? P4 P1 C11 C16B 22.8(8) . . . . ? P2 P1 C11 C16B -68.1(8) . . . . ? Sb P1 C11 C16B 151.0(7) . . . . ? P4 P1 C11 C12A 179.8(7) . . . . ? P2 P1 C11 C12A 88.8(8) . . . . ? Sb P1 C11 C12A -52.1(8) . . . . ? P4 P1 C11 C12B 150.1(6) . . . . ? P2 P1 C11 C12B 59.2(7) . . . . ? Sb P1 C11 C12B -81.7(7) . . . . ? P4 P1 C11 C16A 53.6(7) . . . . ? P2 P1 C11 C16A -37.4(7) . . . . ? Sb P1 C11 C16A -178.3(6) . . . . ? C16A C11 C12A C13A -60.0(14) . . . . ? P1 C11 C12A C13A 172.3(9) . . . . ? C11 C12A C13A C14A 57.7(17) . . . . ? C12A C13A C14A C15A -55.0(18) . . . . ? C13A C14A C15A C16A 53.4(19) . . . . ? C14A C15A C16A C11 -54.9(17) . . . . ? C12A C11 C16A C15A 60.2(13) . . . . ? P1 C11 C16A C15A -172.2(9) . . . . ? C16B C11 C12B C13B -58.1(14) . . . . ? P1 C11 C12B C13B 174.0(9) . . . . ? C11 C12B C13B C14B 58.6(15) . . . . ? C12B C13B C14B C15B -71.6(19) . . . . ? C13B C14B C15B C16B 73.9(19) . . . . ? C12B C11 C16B C15B 60.9(14) . . . . ? P1 C11 C16B C15B -174.7(10) . . . . ? C14B C15B C16B C11 -69.5(18) . . . . ? P3 P2 C21 C26 -70.1(4) . . . . ? P1 P2 C21 C26 -151.8(3) . . . . ? P3 P2 C21 C22 167.9(3) . . . . ? P1 P2 C21 C22 86.2(4) . . . . ? C26 C21 C22 C23 56.5(6) . . . . ? P2 C21 C22 C23 177.0(4) . . . . ? C21 C22 C23 C24 -55.7(7) . . . . ? C22 C23 C24 C25 55.4(8) . . . . ? C23 C24 C25 C26 -55.1(9) . . . . ? C22 C21 C26 C25 -57.1(6) . . . . ? P2 C21 C26 C25 -178.0(4) . . . . ? C24 C25 C26 C21 55.7(8) . . . . ? P2 P3 C31 C32 23.6(4) . . . . ? P4 P3 C31 C32 -66.7(4) . . . . ? Sb P3 C31 C32 147.3(4) 3_666 . . . ? P2 P3 C31 C36 150.7(4) . . . . ? P4 P3 C31 C36 60.5(4) . . . . ? Sb P3 C31 C36 -85.5(4) 3_666 . . . ? C36 C31 C32 C33 55.3(7) . . . . ? P3 C31 C32 C33 -178.1(5) . . . . ? C31 C32 C33 C34 -55.3(8) . . . . ? C32 C33 C34 C35 56.3(9) . . . . ? C33 C34 C35 C36 -56.6(9) . . . . ? C32 C31 C36 C35 -55.0(7) . . . . ? P3 C31 C36 C35 176.7(5) . . . . ? C34 C35 C36 C31 55.5(9) . . . . ? P1 P4 C41 C46 157.8(3) . . . . ? P3 P4 C41 C46 75.3(3) . . . . ? P1 P4 C41 C42 -82.3(3) . . . . ? P3 P4 C41 C42 -164.8(3) . . . . ? C46 C41 C42 C43 -56.5(5) . . . . ? P4 C41 C42 C43 -176.1(4) . . . . ? C41 C42 C43 C44 55.0(6) . . . . ? C42 C43 C44 C45 -54.3(6) . . . . ? C43 C44 C45 C46 54.8(6) . . . . ? C44 C45 C46 C41 -56.3(6) . . . . ? C42 C41 C46 C45 57.1(5) . . . . ? P4 C41 C46 C45 174.3(4) . . . . ? Cl1 Sb Cl2 Al 45.56(10) . . . . ? P1 Sb Cl2 Al 124.18(9) . . . . ? P3 Sb Cl2 Al -46.75(9) 3_666 . . . ? Sb Sb Cl2 Al -164.57(6) 3_666 . . . ? Sb Cl2 Al Cl5 -150.39(12) . . . . ? Sb Cl2 Al Cl4 88.59(11) . . . . ? Sb Cl2 Al Cl3 -28.63(12) . . . . ? C16S C11S C12S C13S 0.0 . . . . ? C10S C11S C12S C13S -178.0(12) . . . . ? C11S C12S C13S C14S 0.0 . . . . ? C12S C13S C14S C15S 0.0 . . . . ? C13S C14S C15S C16S 0.0 . . . . ? C14S C15S C16S C11S 0.0 . . . . ? C12S C11S C16S C15S 0.0 . . . . ? C10S C11S C16S C15S 178.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.405 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.100 # Attachment '[AN_PCy_4][GaCl4].cif' data_dal0946 _database_code_depnum_ccdc_archive 'CCDC 747680' #TrackingRef '[AN_PCy_4][GaCl4].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H53 As N P4, Cl4 Ga, 0.5(C H2 Cl2)' _chemical_formula_sum 'C36.5 H54 As Cl5 Ga N P4' _chemical_formula_weight 952.58 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' N N 0.0061 0.0033 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2986(8) _cell_length_b 16.5069(12) _cell_length_c 23.6544(17) _cell_angle_alpha 92.1892(9) _cell_angle_beta 100.9413(9) _cell_angle_gamma 96.1712(9) _cell_volume 4298.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8124 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.43 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 1.891 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4893 _exptl_absorpt_correction_T_max 0.7581 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37853 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.56 _reflns_number_total 19554 _reflns_number_gt 14412 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. 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^)+(0.0582P)^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 19554 _refine_ls_number_parameters 884 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 As1A As 0.50230(3) 0.383154(17) -0.002230(12) 0.02889(8) Uani 1 1 d . . . P1A P 0.54864(7) 0.24912(4) 0.03072(3) 0.02383(15) Uani 1 1 d . . . P2A P 0.53313(7) 0.24076(4) 0.12192(3) 0.02576(16) Uani 1 1 d . . . P3A P 0.34053(7) 0.19505(5) 0.08137(3) 0.02882(17) Uani 1 1 d . . . P4A P 0.42737(7) 0.13365(4) 0.01679(3) 0.02730(16) Uani 1 1 d . . . N1A N 0.3862(2) 0.31827(15) -0.13341(10) 0.0293(5) Uani 1 1 d . . . H1NA H 0.3579 0.2868 -0.1650 0.035 Uiso 1 1 calc R . . C11A C 0.7020(3) 0.23572(17) 0.01888(12) 0.0283(6) Uani 1 1 d . . . H11A H 0.7490 0.2912 0.0226 0.034 Uiso 1 1 calc R . . C12A C 0.6990(3) 0.19992(18) -0.04215(13) 0.0332(7) Uani 1 1 d . . . H12A H 0.6563 0.1437 -0.0471 0.040 Uiso 1 1 calc R . . H12B H 0.6543 0.2334 -0.0708 0.040 Uiso 1 1 calc R . . C13A C 0.8281(3) 0.1987(2) -0.05194(15) 0.0433(8) Uani 1 1 d . . . H13A H 0.8683 0.2553 -0.0496 0.052 Uiso 1 1 calc R . . H13B H 0.8257 0.1744 -0.0911 0.052 Uiso 1 1 calc R . . C14A C 0.9023(3) 0.1496(2) -0.00749(17) 0.0524(10) Uani 1 1 d . . . H14A H 0.8685 0.0913 -0.0132 0.063 Uiso 1 1 calc R . . H14B H 0.9872 0.1539 -0.0133 0.063 Uiso 1 1 calc R . . C15A C 0.9005(3) 0.1802(3) 0.05346(17) 0.0543(10) Uani 1 1 d . . . H15A H 0.9464 0.2353 0.0611 0.065 Uiso 1 1 calc R . . H15B H 0.9418 0.1436 0.0809 0.065 Uiso 1 1 calc R . . C16A C 0.7712(3) 0.1841(2) 0.06392(14) 0.0405(8) Uani 1 1 d . . . H16A H 0.7746 0.2087 0.1031 0.049 Uiso 1 1 calc R . . H16B H 0.7279 0.1283 0.0613 0.049 Uiso 1 1 calc R . . C21A C 0.5311(2) 0.34862(16) 0.14723(11) 0.0246(6) Uani 1 1 d . . . H21A H 0.4699 0.3746 0.1197 0.030 Uiso 1 1 calc R . . C22A C 0.6572(3) 0.39449(18) 0.15061(14) 0.0351(7) Uani 1 1 d . . . H22A H 0.6768 0.3953 0.1116 0.042 Uiso 1 1 calc R . . H22B H 0.7183 0.3658 0.1753 0.042 Uiso 1 1 calc R . . C23A C 0.6631(3) 0.48224(19) 0.17551(15) 0.0428(8) Uani 1 1 d . . . H23A H 0.7464 0.5102 0.1789 0.051 Uiso 1 1 calc R . . H23B H 0.6070 0.5124 0.1491 0.051 Uiso 1 1 calc R . . C24A C 0.6281(4) 0.4826(2) 0.23485(15) 0.0510(9) Uani 1 1 d . . . H24A H 0.6892 0.4576 0.2623 0.061 Uiso 1 1 calc R . . H24B H 0.6277 0.5397 0.2493 0.061 Uiso 1 1 calc R . . C25A C 0.5044(4) 0.43605(19) 0.23216(14) 0.0457(9) Uani 1 1 d . . . H25A H 0.4421 0.4648 0.2083 0.055 Uiso 1 1 calc R . . H25B H 0.4865 0.4346 0.2715 0.055 Uiso 1 1 calc R . . C26A C 0.4973(3) 0.34898(17) 0.20671(12) 0.0314(7) Uani 1 1 d . . . H26A H 0.4139 0.3214 0.2035 0.038 Uiso 1 1 calc R . . H26B H 0.5533 0.3183 0.2327 0.038 Uiso 1 1 calc R . . C31A C 0.2964(3) 0.11028(19) 0.12621(14) 0.0394(8) Uani 1 1 d . . . H31A H 0.2178 0.0815 0.1042 0.047 Uiso 1 1 calc R . . C32A C 0.2681(5) 0.1473(2) 0.18150(18) 0.0716(14) Uani 1 1 d . . . H32A H 0.2089 0.1871 0.1719 0.086 Uiso 1 1 calc R . . H32B H 0.3431 0.1764 0.2054 0.086 Uiso 1 1 calc R . . C33A C 0.2150(6) 0.0788(3) 0.2156(2) 0.0953(19) Uani 1 1 d . . . H33A H 0.2010 0.1027 0.2525 0.114 Uiso 1 1 calc R . . H33B H 0.1358 0.0536 0.1931 0.114 Uiso 1 1 calc R . . C34A C 0.2986(5) 0.0146(3) 0.22784(18) 0.0893(19) Uani 1 1 d . . . H34A H 0.2607 -0.0291 0.2484 0.107 Uiso 1 1 calc R . . H34B H 0.3752 0.0388 0.2533 0.107 Uiso 1 1 calc R . . C35A C 0.3266(5) -0.0218(3) 0.17301(19) 0.0815(15) Uani 1 1 d . . . H35A H 0.2514 -0.0507 0.1491 0.098 Uiso 1 1 calc R . . H35B H 0.3853 -0.0620 0.1826 0.098 Uiso 1 1 calc R . . C36A C 0.3806(4) 0.0458(3) 0.13857(19) 0.0686(12) Uani 1 1 d . . . H36A H 0.4599 0.0710 0.1610 0.082 Uiso 1 1 calc R . . H36B H 0.3943 0.0215 0.1018 0.082 Uiso 1 1 calc R . . C41A C 0.3125(3) 0.13191(17) -0.05087(12) 0.0289(6) Uani 1 1 d . . . H41A H 0.2871 0.1877 -0.0568 0.035 Uiso 1 1 calc R . . C42A C 0.3618(3) 0.1021(2) -0.10290(13) 0.0402(8) Uani 1 1 d . . . H42A H 0.4284 0.1426 -0.1095 0.048 Uiso 1 1 calc R . . H42B H 0.3955 0.0499 -0.0948 0.048 Uiso 1 1 calc R . . C43A C 0.2622(3) 0.0899(2) -0.15722(13) 0.0440(8) Uani 1 1 d . . . H43A H 0.2353 0.1433 -0.1679 0.053 Uiso 1 1 calc R . . H43B H 0.2956 0.0673 -0.1895 0.053 Uiso 1 1 calc R . . C44A C 0.1533(3) 0.0321(2) -0.14829(13) 0.0416(8) Uani 1 1 d . . . H44A H 0.0885 0.0288 -0.1832 0.050 Uiso 1 1 calc R . . H44B H 0.1777 -0.0233 -0.1424 0.050 Uiso 1 1 calc R . . C45A C 0.1047(3) 0.0614(2) -0.09646(13) 0.0410(8) Uani 1 1 d . . . H45A H 0.0377 0.0212 -0.0901 0.049 Uiso 1 1 calc R . . H45B H 0.0718 0.1139 -0.1042 0.049 Uiso 1 1 calc R . . C46A C 0.2041(3) 0.07261(19) -0.04219(13) 0.0331(7) Uani 1 1 d . . . H46A H 0.2317 0.0191 -0.0324 0.040 Uiso 1 1 calc R . . H46B H 0.1706 0.0939 -0.0096 0.040 Uiso 1 1 calc R . . C51A C 0.3361(3) 0.35976(17) -0.04081(12) 0.0295(6) Uani 1 1 d . . . C52A C 0.3024(3) 0.33347(17) -0.09895(12) 0.0287(6) Uani 1 1 d . . . C53A C 0.1790(3) 0.32024(19) -0.12433(14) 0.0364(7) Uani 1 1 d . . . H53A H 0.1548 0.3025 -0.1639 0.044 Uiso 1 1 calc R . . C54A C 0.0926(3) 0.3329(2) -0.09199(16) 0.0461(9) Uani 1 1 d . . . H54A H 0.0091 0.3239 -0.1096 0.055 Uiso 1 1 calc R . . C55A C 0.1259(3) 0.3587(2) -0.03394(16) 0.0467(9) Uani 1 1 d . . . H55A H 0.0656 0.3669 -0.0119 0.056 Uiso 1 1 calc R . . C56A C 0.2462(3) 0.37213(19) -0.00895(14) 0.0373(7) Uani 1 1 d . . . H56A H 0.2692 0.3901 0.0306 0.045 Uiso 1 1 calc R . . C61A C 0.5730(3) 0.38093(17) -0.06985(12) 0.0286(6) Uani 1 1 d . . . C62A C 0.5085(3) 0.34698(17) -0.12355(12) 0.0286(6) Uani 1 1 d . . . C63A C 0.5703(3) 0.3422(2) -0.16943(13) 0.0370(7) Uani 1 1 d . . . H63A H 0.5283 0.3185 -0.2059 0.044 Uiso 1 1 calc R . . C64A C 0.6911(3) 0.3715(2) -0.16200(14) 0.0431(8) Uani 1 1 d . . . H64A H 0.7320 0.3672 -0.1934 0.052 Uiso 1 1 calc R . . C65A C 0.7539(3) 0.4072(2) -0.10961(15) 0.0430(8) Uani 1 1 d . . . H65A H 0.8368 0.4286 -0.1052 0.052 Uiso 1 1 calc R . . C66A C 0.6955(3) 0.41143(18) -0.06382(14) 0.0358(7) Uani 1 1 d . . . H66A H 0.7388 0.4354 -0.0276 0.043 Uiso 1 1 calc R . . As1B As 0.53412(3) 0.163367(16) 0.498579(11) 0.02352(7) Uani 1 1 d . . . P1B P 0.51839(6) 0.27060(4) 0.42935(3) 0.01927(14) Uani 1 1 d . . . P2B P 0.58173(6) 0.39235(4) 0.47277(3) 0.02049(14) Uani 1 1 d . . . P3B P 0.75888(6) 0.37286(4) 0.44793(3) 0.02122(14) Uani 1 1 d . . . P4B P 0.64254(6) 0.30417(4) 0.37057(3) 0.02053(14) Uani 1 1 d . . . N1B N 0.6036(2) 0.01550(15) 0.42109(10) 0.0340(6) Uani 1 1 d . . . H1NB H 0.6225 -0.0231 0.3989 0.041 Uiso 1 1 calc R . . C11B C 0.3586(2) 0.26489(16) 0.39117(11) 0.0214(5) Uani 1 1 d . . . H11B H 0.3306 0.2067 0.3775 0.026 Uiso 1 1 calc R . . C12B C 0.2772(2) 0.29072(17) 0.43211(11) 0.0260(6) Uani 1 1 d . . . H12C H 0.2830 0.2548 0.4649 0.031 Uiso 1 1 calc R . . H12D H 0.3053 0.3475 0.4477 0.031 Uiso 1 1 calc R . . C13B C 0.1452(2) 0.28518(19) 0.40034(12) 0.0312(7) Uani 1 1 d . . . H13C H 0.1150 0.2277 0.3874 0.037 Uiso 1 1 calc R . . H13D H 0.0944 0.3039 0.4269 0.037 Uiso 1 1 calc R . . C14B C 0.1344(2) 0.33760(19) 0.34838(13) 0.0316(7) Uani 1 1 d . . . H14C H 0.0490 0.3318 0.3276 0.038 Uiso 1 1 calc R . . H14D H 0.1585 0.3957 0.3617 0.038 Uiso 1 1 calc R . . C15B C 0.2149(3) 0.3123(2) 0.30776(12) 0.0349(7) Uani 1 1 d . . . H15C H 0.1855 0.2560 0.2915 0.042 Uiso 1 1 calc R . . H15D H 0.2094 0.3488 0.2754 0.042 Uiso 1 1 calc R . . C16B C 0.3462(2) 0.31600(19) 0.33835(11) 0.0278(6) Uani 1 1 d . . . H16C H 0.3786 0.3734 0.3505 0.033 Uiso 1 1 calc R . . H16D H 0.3948 0.2956 0.3113 0.033 Uiso 1 1 calc R . . C21B C 0.6059(2) 0.37411(16) 0.55112(11) 0.0209(5) Uani 1 1 d . . . H21B H 0.6478 0.3240 0.5581 0.025 Uiso 1 1 calc R . . C22B C 0.4841(2) 0.36159(18) 0.57058(11) 0.0268(6) Uani 1 1 d . . . H22C H 0.4348 0.3125 0.5496 0.032 Uiso 1 1 calc R . . H22D H 0.4394 0.4092 0.5610 0.032 Uiso 1 1 calc R . . C23B C 0.5024(3) 0.35127(19) 0.63565(12) 0.0336(7) Uani 1 1 d . . . H23C H 0.4228 0.3467 0.6477 0.040 Uiso 1 1 calc R . . H23D H 0.5392 0.3004 0.6448 0.040 Uiso 1 1 calc R . . C24B C 0.5842(3) 0.4235(2) 0.66869(13) 0.0407(8) Uani 1 1 d . . . H24C H 0.5424 0.4732 0.6632 0.049 Uiso 1 1 calc R . . H24D H 0.5991 0.4139 0.7104 0.049 Uiso 1 1 calc R . . C25B C 0.7045(3) 0.4377(2) 0.64932(13) 0.0394(8) Uani 1 1 d . . . H25C H 0.7509 0.3909 0.6593 0.047 Uiso 1 1 calc R . . H25D H 0.7522 0.4873 0.6702 0.047 Uiso 1 1 calc R . . C26B C 0.6874(3) 0.44762(17) 0.58430(12) 0.0286(6) Uani 1 1 d . . . H26C H 0.7674 0.4524 0.5726 0.034 Uiso 1 1 calc R . . H26D H 0.6501 0.4982 0.5748 0.034 Uiso 1 1 calc R . . C31B C 0.7929(2) 0.47208(15) 0.41545(11) 0.0217(5) Uani 1 1 d . . . H31B H 0.7186 0.4841 0.3882 0.026 Uiso 1 1 calc R . . C32B C 0.8291(3) 0.54079(16) 0.46265(12) 0.0255(6) Uani 1 1 d . . . H32C H 0.8983 0.5270 0.4916 0.031 Uiso 1 1 calc R . . H32D H 0.7602 0.5463 0.4824 0.031 Uiso 1 1 calc R . . C33B C 0.8647(3) 0.62207(17) 0.43771(13) 0.0322(7) Uani 1 1 d . . . H33C H 0.7932 0.6386 0.4115 0.039 Uiso 1 1 calc R . . H33D H 0.8913 0.6648 0.4694 0.039 Uiso 1 1 calc R . . C34B C 0.9671(3) 0.61490(18) 0.40452(13) 0.0345(7) Uani 1 1 d . . . H34C H 0.9854 0.6672 0.3870 0.041 Uiso 1 1 calc R . . H34D H 1.0412 0.6040 0.4316 0.041 Uiso 1 1 calc R . . C35B C 0.9324(3) 0.54662(18) 0.35748(13) 0.0323(7) Uani 1 1 d . . . H35C H 1.0022 0.5411 0.3384 0.039 Uiso 1 1 calc R . . H35D H 0.8642 0.5607 0.3280 0.039 Uiso 1 1 calc R . . C36B C 0.8951(3) 0.46502(17) 0.38178(12) 0.0266(6) Uani 1 1 d . . . H36C H 0.9663 0.4475 0.4076 0.032 Uiso 1 1 calc R . . H36D H 0.8676 0.4229 0.3497 0.032 Uiso 1 1 calc R . . C41B C 0.7108(2) 0.21148(15) 0.35308(11) 0.0215(5) Uani 1 1 d . . . H41B H 0.7353 0.1821 0.3889 0.026 Uiso 1 1 calc R . . C42B C 0.6152(3) 0.15658(17) 0.30963(13) 0.0310(6) Uani 1 1 d . . . H42C H 0.5813 0.1888 0.2772 0.037 Uiso 1 1 calc R . . H42D H 0.5480 0.1356 0.3285 0.037 Uiso 1 1 calc R . . C43B C 0.6710(3) 0.08451(18) 0.28627(14) 0.0379(7) Uani 1 1 d . . . H43C H 0.6957 0.0486 0.3179 0.046 Uiso 1 1 calc R . . H43D H 0.6093 0.0521 0.2562 0.046 Uiso 1 1 calc R . . C44B C 0.7811(3) 0.11385(19) 0.26074(13) 0.0385(8) Uani 1 1 d . . . H44C H 0.8166 0.0662 0.2472 0.046 Uiso 1 1 calc R . . H44D H 0.7555 0.1462 0.2271 0.046 Uiso 1 1 calc R . . C45B C 0.8757(3) 0.16566(18) 0.30522(13) 0.0347(7) Uani 1 1 d . . . H45C H 0.9456 0.1851 0.2877 0.042 Uiso 1 1 calc R . . H45D H 0.9051 0.1323 0.3377 0.042 Uiso 1 1 calc R . . C46B C 0.8225(3) 0.23900(17) 0.32785(12) 0.0278(6) Uani 1 1 d . . . H46C H 0.8848 0.2708 0.3580 0.033 Uiso 1 1 calc R . . H46D H 0.7997 0.2749 0.2960 0.033 Uiso 1 1 calc R . . C51B C 0.6887(3) 0.13136(16) 0.49044(12) 0.0266(6) Uani 1 1 d . . . C52B C 0.7006(3) 0.06412(17) 0.45463(12) 0.0309(7) Uani 1 1 d . . . C53B C 0.8185(3) 0.04547(19) 0.45209(14) 0.0379(8) Uani 1 1 d . . . H53B H 0.8284 0.0000 0.4283 0.045 Uiso 1 1 calc R . . C54B C 0.9191(3) 0.0920(2) 0.48352(16) 0.0460(9) Uani 1 1 d . . . H54B H 0.9977 0.0790 0.4805 0.055 Uiso 1 1 calc R . . C55B C 0.9078(3) 0.1581(2) 0.51968(16) 0.0434(8) Uani 1 1 d . . . H55B H 0.9777 0.1897 0.5418 0.052 Uiso 1 1 calc R . . C56B C 0.7926(3) 0.17657(18) 0.52270(13) 0.0335(7) Uani 1 1 d . . . H56B H 0.7839 0.2213 0.5474 0.040 Uiso 1 1 calc R . . C61B C 0.4337(3) 0.07790(16) 0.44907(12) 0.0269(6) Uani 1 1 d . . . C62B C 0.4807(3) 0.01934(17) 0.41774(12) 0.0305(6) Uani 1 1 d . . . C63B C 0.3977(3) -0.03920(19) 0.38125(13) 0.0410(8) Uani 1 1 d . . . H63B H 0.4274 -0.0793 0.3595 0.049 Uiso 1 1 calc R . . C64B C 0.2754(3) -0.0391(2) 0.37664(14) 0.0452(9) Uani 1 1 d . . . H64B H 0.2216 -0.0788 0.3514 0.054 Uiso 1 1 calc R . . C65B C 0.2284(3) 0.0177(2) 0.40789(14) 0.0407(8) Uani 1 1 d . . . H65B H 0.1432 0.0173 0.4043 0.049 Uiso 1 1 calc R . . C66B C 0.3075(3) 0.07478(18) 0.44426(13) 0.0323(7) Uani 1 1 d . . . H66B H 0.2759 0.1131 0.4667 0.039 Uiso 1 1 calc R . . Ga1 Ga 0.25142(3) 0.170406(19) 0.676693(14) 0.03003(8) Uani 1 1 d . . . Cl1 Cl 0.42553(8) 0.13706(6) 0.71864(4) 0.0529(2) Uani 1 1 d . . . Cl2 Cl 0.22615(8) 0.28605(5) 0.71716(3) 0.03970(18) Uani 1 1 d . . . Cl3 Cl 0.25779(9) 0.17982(5) 0.58529(3) 0.0451(2) Uani 1 1 d . . . Cl4 Cl 0.10077(8) 0.07971(5) 0.68131(4) 0.0458(2) Uani 1 1 d . . . Ga2 Ga 0.02703(3) 0.40712(2) 0.158561(14) 0.03364(9) Uani 1 1 d . . . Cl5 Cl -0.08141(8) 0.43112(5) 0.07613(3) 0.0443(2) Uani 1 1 d . . . Cl6 Cl 0.20108(8) 0.37819(7) 0.14406(4) 0.0574(3) Uani 1 1 d . . . Cl7 Cl 0.04779(10) 0.51501(7) 0.21681(4) 0.0609(3) Uani 1 1 d . . . Cl8 Cl -0.05648(8) 0.30345(6) 0.19664(4) 0.0558(3) Uani 1 1 d . . . Cl1S Cl 0.06325(14) 0.82264(10) 0.20817(6) 0.0740(4) Uani 0.80 1 d PD A 1 Cl2S Cl 0.25439(16) 0.76944(9) 0.28994(10) 0.1100(8) Uani 0.80 1 d PD A 1 C1S C 0.0981(6) 0.7580(5) 0.2627(3) 0.0665(15) Uani 0.80 1 d PD A 1 H1SA H 0.0711 0.7008 0.2478 0.080 Uiso 0.80 1 calc PR A 1 H1SB H 0.0546 0.7701 0.2940 0.080 Uiso 0.80 1 calc PR A 1 Cl3S Cl 0.1283(9) 0.7992(6) 0.2066(4) 0.114(2) Uiso 0.20 1 d PD B 2 Cl4S Cl 0.1734(9) 0.7560(5) 0.3227(3) 0.114(2) Uiso 0.20 1 d PD B 2 C2S C 0.071(3) 0.744(3) 0.2571(11) 0.114(2) Uiso 0.20 1 d PD B 2 H2SA H 0.0561 0.6851 0.2439 0.137 Uiso 0.20 1 calc PR B 2 H2SB H -0.0071 0.7619 0.2621 0.137 Uiso 0.20 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1A 0.03937(18) 0.02495(15) 0.02218(15) 0.00094(11) 0.00525(13) 0.00447(13) P1A 0.0284(4) 0.0236(3) 0.0206(3) 0.0002(3) 0.0077(3) 0.0029(3) P2A 0.0328(4) 0.0251(4) 0.0204(3) 0.0013(3) 0.0071(3) 0.0047(3) P3A 0.0326(4) 0.0291(4) 0.0263(4) 0.0003(3) 0.0108(3) 0.0017(3) P4A 0.0324(4) 0.0248(4) 0.0252(4) -0.0004(3) 0.0079(3) 0.0019(3) N1A 0.0297(13) 0.0354(13) 0.0210(12) -0.0048(10) 0.0058(10) -0.0028(10) C11A 0.0270(15) 0.0283(15) 0.0307(15) -0.0036(12) 0.0100(12) 0.0021(12) C12A 0.0392(18) 0.0309(15) 0.0330(16) -0.0005(13) 0.0177(14) 0.0012(13) C13A 0.044(2) 0.0454(19) 0.049(2) 0.0006(16) 0.0295(17) 0.0066(16) C14A 0.045(2) 0.052(2) 0.071(3) 0.0047(19) 0.0291(19) 0.0189(17) C15A 0.039(2) 0.066(3) 0.064(3) 0.014(2) 0.0149(18) 0.0192(18) C16A 0.0379(18) 0.0461(19) 0.0417(18) 0.0110(15) 0.0117(15) 0.0142(15) C21A 0.0281(15) 0.0246(14) 0.0210(13) 0.0007(11) 0.0045(11) 0.0029(11) C22A 0.0291(16) 0.0356(17) 0.0405(18) 0.0047(14) 0.0076(13) 0.0016(13) C23A 0.0367(18) 0.0302(16) 0.057(2) 0.0005(15) 0.0031(16) -0.0068(14) C24A 0.068(3) 0.0335(18) 0.042(2) -0.0108(15) -0.0060(18) -0.0009(17) C25A 0.073(3) 0.0335(17) 0.0349(18) -0.0077(14) 0.0235(17) 0.0046(17) C26A 0.0427(18) 0.0290(15) 0.0236(14) -0.0007(12) 0.0115(13) 0.0003(13) C31A 0.0461(19) 0.0387(18) 0.0321(16) 0.0006(14) 0.0134(15) -0.0101(15) C32A 0.115(4) 0.056(2) 0.055(2) -0.001(2) 0.057(3) -0.013(2) C33A 0.147(5) 0.082(4) 0.070(3) 0.002(3) 0.078(4) -0.026(4) C34A 0.132(5) 0.073(3) 0.045(2) 0.019(2) 0.004(3) -0.054(3) C35A 0.129(5) 0.059(3) 0.058(3) 0.029(2) 0.023(3) 0.001(3) C36A 0.091(3) 0.060(3) 0.065(3) 0.033(2) 0.030(2) 0.016(2) C41A 0.0374(16) 0.0237(14) 0.0244(14) -0.0029(11) 0.0051(12) 0.0014(12) C42A 0.0417(19) 0.0465(19) 0.0321(17) -0.0060(14) 0.0145(14) -0.0072(15) C43A 0.054(2) 0.051(2) 0.0257(16) -0.0057(14) 0.0103(15) -0.0044(17) C44A 0.0442(19) 0.0453(19) 0.0316(17) -0.0116(14) 0.0062(15) -0.0044(15) C45A 0.0371(18) 0.052(2) 0.0313(17) -0.0085(15) 0.0058(14) -0.0009(15) C46A 0.0345(17) 0.0351(16) 0.0301(15) -0.0031(13) 0.0098(13) 0.0017(13) C51A 0.0362(16) 0.0262(14) 0.0283(15) 0.0082(12) 0.0087(13) 0.0069(12) C52A 0.0352(16) 0.0257(14) 0.0276(15) 0.0075(12) 0.0102(13) 0.0048(12) C53A 0.0321(17) 0.0428(18) 0.0349(17) 0.0091(14) 0.0082(14) 0.0022(14) C54A 0.0326(18) 0.054(2) 0.054(2) 0.0132(18) 0.0108(16) 0.0083(16) C55A 0.045(2) 0.054(2) 0.051(2) 0.0123(17) 0.0264(17) 0.0164(17) C56A 0.049(2) 0.0362(17) 0.0327(16) 0.0081(13) 0.0169(15) 0.0143(15) C61A 0.0347(16) 0.0251(14) 0.0268(14) 0.0049(11) 0.0079(12) 0.0028(12) C62A 0.0314(16) 0.0290(15) 0.0283(15) 0.0078(12) 0.0099(12) 0.0066(12) C63A 0.0394(18) 0.0482(19) 0.0251(15) 0.0052(14) 0.0100(13) 0.0052(15) C64A 0.0387(19) 0.058(2) 0.0382(18) 0.0136(16) 0.0197(15) 0.0067(16) C65A 0.0296(17) 0.052(2) 0.048(2) 0.0226(17) 0.0087(15) 0.0002(15) C66A 0.0366(17) 0.0331(16) 0.0349(17) 0.0125(13) 0.0010(14) -0.0015(13) As1B 0.02818(15) 0.02285(14) 0.02084(14) 0.00145(11) 0.00769(11) 0.00364(11) P1B 0.0188(3) 0.0209(3) 0.0187(3) 0.0003(3) 0.0048(3) 0.0030(3) P2B 0.0219(3) 0.0207(3) 0.0197(3) -0.0003(3) 0.0058(3) 0.0034(3) P3B 0.0202(3) 0.0215(3) 0.0220(3) 0.0002(3) 0.0048(3) 0.0017(3) P4B 0.0200(3) 0.0225(3) 0.0200(3) 0.0005(3) 0.0064(3) 0.0029(3) N1B 0.0473(16) 0.0272(13) 0.0312(14) -0.0033(11) 0.0173(12) 0.0055(11) C11B 0.0161(12) 0.0249(13) 0.0227(13) -0.0015(11) 0.0037(10) 0.0009(10) C12B 0.0222(14) 0.0329(15) 0.0231(14) 0.0004(11) 0.0058(11) 0.0024(11) C13B 0.0199(14) 0.0444(18) 0.0295(15) 0.0001(13) 0.0063(12) 0.0023(13) C14B 0.0183(14) 0.0407(17) 0.0349(16) 0.0053(13) 0.0029(12) 0.0033(12) C15B 0.0231(15) 0.056(2) 0.0253(15) 0.0102(14) 0.0018(12) 0.0063(14) C16B 0.0220(14) 0.0416(17) 0.0209(13) 0.0081(12) 0.0046(11) 0.0047(12) C21B 0.0249(13) 0.0208(13) 0.0176(12) -0.0005(10) 0.0042(10) 0.0051(11) C22B 0.0268(14) 0.0309(15) 0.0232(14) -0.0002(11) 0.0059(11) 0.0038(12) C23B 0.0345(17) 0.0434(18) 0.0248(15) 0.0037(13) 0.0116(13) 0.0027(14) C24B 0.061(2) 0.0397(18) 0.0205(15) -0.0031(13) 0.0123(15) -0.0029(16) C25B 0.048(2) 0.0390(18) 0.0247(15) -0.0002(13) -0.0026(14) -0.0081(15) C26B 0.0292(15) 0.0289(15) 0.0253(14) -0.0006(12) 0.0016(12) 0.0002(12) C31B 0.0203(13) 0.0199(13) 0.0252(14) 0.0017(11) 0.0058(11) 0.0017(10) C32B 0.0280(15) 0.0236(14) 0.0252(14) -0.0025(11) 0.0070(12) 0.0020(11) C33B 0.0427(18) 0.0231(14) 0.0298(15) -0.0043(12) 0.0068(13) 0.0022(13) C34B 0.0346(17) 0.0316(16) 0.0345(16) 0.0030(13) 0.0063(13) -0.0082(13) C35B 0.0346(16) 0.0333(16) 0.0308(16) 0.0022(13) 0.0150(13) -0.0024(13) C36B 0.0280(15) 0.0276(14) 0.0260(14) -0.0009(11) 0.0108(12) 0.0027(12) C41B 0.0228(13) 0.0202(13) 0.0226(13) -0.0005(10) 0.0074(11) 0.0037(10) C42B 0.0295(15) 0.0255(14) 0.0366(16) -0.0054(12) 0.0076(13) -0.0021(12) C43B 0.050(2) 0.0244(15) 0.0367(17) -0.0113(13) 0.0040(15) 0.0025(14) C44B 0.059(2) 0.0303(16) 0.0323(16) -0.0021(13) 0.0182(15) 0.0151(15) C45B 0.0388(17) 0.0345(16) 0.0373(17) 0.0017(13) 0.0195(14) 0.0116(14) C46B 0.0278(15) 0.0254(14) 0.0325(15) -0.0002(12) 0.0124(12) 0.0022(12) C51B 0.0313(15) 0.0244(14) 0.0268(14) 0.0082(11) 0.0087(12) 0.0071(12) C52B 0.0423(18) 0.0271(15) 0.0297(15) 0.0107(12) 0.0169(14) 0.0120(13) C53B 0.047(2) 0.0300(16) 0.0471(19) 0.0135(14) 0.0253(16) 0.0175(14) C54B 0.0372(19) 0.0425(19) 0.068(2) 0.0225(18) 0.0239(18) 0.0174(16) C55B 0.0346(18) 0.0342(17) 0.062(2) 0.0111(16) 0.0069(16) 0.0077(14) C56B 0.0357(17) 0.0291(15) 0.0360(17) 0.0044(13) 0.0058(13) 0.0065(13) C61B 0.0348(16) 0.0238(14) 0.0227(14) 0.0043(11) 0.0090(12) -0.0015(12) C62B 0.0454(18) 0.0260(15) 0.0216(14) 0.0060(11) 0.0110(13) 0.0019(13) C63B 0.064(2) 0.0307(16) 0.0277(16) -0.0010(13) 0.0153(16) -0.0060(16) C64B 0.057(2) 0.0402(19) 0.0306(17) -0.0014(14) 0.0033(16) -0.0163(17) C65B 0.0411(19) 0.0424(19) 0.0354(17) 0.0099(15) 0.0045(15) -0.0061(15) C66B 0.0354(17) 0.0298(15) 0.0333(16) 0.0074(13) 0.0112(13) 0.0010(13) Ga1 0.03555(19) 0.02500(16) 0.03176(18) 0.00006(13) 0.01237(14) 0.00367(13) Cl1 0.0381(5) 0.0499(5) 0.0746(6) 0.0193(5) 0.0140(4) 0.0118(4) Cl2 0.0566(5) 0.0312(4) 0.0339(4) -0.0034(3) 0.0135(4) 0.0103(3) Cl3 0.0675(6) 0.0368(4) 0.0331(4) -0.0049(3) 0.0222(4) -0.0043(4) Cl4 0.0424(5) 0.0423(4) 0.0527(5) 0.0040(4) 0.0155(4) -0.0067(4) Ga2 0.02746(17) 0.0488(2) 0.02405(17) 0.00586(15) 0.00423(13) 0.00160(15) Cl5 0.0434(5) 0.0541(5) 0.0305(4) 0.0117(4) -0.0034(3) -0.0010(4) Cl6 0.0445(5) 0.0775(7) 0.0612(6) 0.0218(5) 0.0255(5) 0.0225(5) Cl7 0.0662(6) 0.0766(7) 0.0378(5) -0.0164(5) 0.0131(4) 0.0009(5) Cl8 0.0388(5) 0.0754(6) 0.0505(5) 0.0334(5) 0.0019(4) -0.0046(4) Cl1S 0.0615(9) 0.0873(11) 0.0658(9) 0.0163(8) -0.0041(7) 0.0010(8) Cl2S 0.0796(11) 0.0579(9) 0.1624(19) -0.0249(10) -0.0582(12) 0.0299(8) C1S 0.060(4) 0.065(4) 0.068(4) 0.014(3) 0.001(3) -0.001(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 As1A C51A 1.917(3) . ? As1A C61A 1.919(3) . ? As1A P1A 2.4501(8) . ? P1A C11A 1.842(3) . ? P1A P4A 2.1996(10) . ? P1A P2A 2.2057(10) . ? P2A C21A 1.860(3) . ? P2A P3A 2.2415(11) . ? P3A C31A 1.870(3) . ? P3A P4A 2.2334(10) . ? P4A C41A 1.857(3) . ? N1A C62A 1.385(4) . ? N1A C52A 1.397(4) . ? C11A C12A 1.531(4) . ? C11A C16A 1.538(4) . ? C12A C13A 1.522(4) . ? C13A C14A 1.530(5) . ? C14A C15A 1.514(5) . ? C15A C16A 1.535(5) . ? C21A C26A 1.526(4) . ? C21A C22A 1.527(4) . ? C22A C23A 1.533(4) . ? C23A C24A 1.529(5) . ? C24A C25A 1.510(5) . ? C25A C26A 1.525(4) . ? C31A C36A 1.503(5) . ? C31A C32A 1.525(5) . ? C32A C33A 1.547(5) . ? C33A C34A 1.495(8) . ? C34A C35A 1.510(6) . ? C35A C36A 1.547(5) . ? C41A C42A 1.530(4) . ? C41A C46A 1.534(4) . ? C42A C43A 1.530(4) . ? C43A C44A 1.526(5) . ? C44A C45A 1.519(4) . ? C45A C46A 1.527(4) . ? C51A C52A 1.395(4) . ? C51A C56A 1.402(4) . ? C52A C53A 1.399(4) . ? C53A C54A 1.377(4) . ? C54A C55A 1.390(5) . ? C55A C56A 1.366(5) . ? C61A C66A 1.400(4) . ? C61A C62A 1.402(4) . ? C62A C63A 1.401(4) . ? C63A C64A 1.375(4) . ? C64A C65A 1.381(5) . ? C65A C66A 1.375(5) . ? As1B C61B 1.917(3) . ? As1B C51B 1.920(3) . ? As1B P1B 2.4545(7) . ? P1B C11B 1.850(3) . ? P1B P4B 2.2000(9) . ? P1B P2B 2.2045(9) . ? P2B C21B 1.862(3) . ? P2B P3B 2.2417(9) . ? P3B C31B 1.869(3) . ? P3B P4B 2.2294(9) . ? P4B C41B 1.853(3) . ? N1B C52B 1.380(4) . ? N1B C62B 1.385(4) . ? C11B C16B 1.527(4) . ? C11B C12B 1.536(3) . ? C12B C13B 1.529(4) . ? C13B C14B 1.524(4) . ? C14B C15B 1.519(4) . ? C15B C16B 1.516(4) . ? C21B C22B 1.528(4) . ? C21B C26B 1.533(4) . ? C22B C23B 1.532(4) . ? C23B C24B 1.518(4) . ? C24B C25B 1.513(5) . ? C25B C26B 1.531(4) . ? C31B C32B 1.526(3) . ? C31B C36B 1.533(4) . ? C32B C33B 1.531(4) . ? C33B C34B 1.529(4) . ? C34B C35B 1.519(4) . ? C35B C36B 1.533(4) . ? C41B C46B 1.530(4) . ? C41B C42B 1.530(4) . ? C42B C43B 1.537(4) . ? C43B C44B 1.525(4) . ? C44B C45B 1.513(4) . ? C45B C46B 1.530(4) . ? C51B C56B 1.394(4) . ? C51B C52B 1.404(4) . ? C52B C53B 1.411(4) . ? C53B C54B 1.372(5) . ? C54B C55B 1.391(5) . ? C55B C56B 1.383(4) . ? C61B C62B 1.403(4) . ? C61B C66B 1.405(4) . ? C62B C63B 1.411(4) . ? C63B C64B 1.365(5) . ? C64B C65B 1.382(5) . ? C65B C66B 1.375(4) . ? Ga1 Cl4 2.1647(9) . ? Ga1 Cl1 2.1659(10) . ? Ga1 Cl2 2.1732(8) . ? Ga1 Cl3 2.1876(8) . ? Ga2 Cl6 2.1584(9) . ? Ga2 Cl5 2.1717(8) . ? Ga2 Cl8 2.1733(9) . ? Ga2 Cl7 2.1738(10) . ? Cl1S C1S 1.720(6) . ? Cl2S C1S 1.748(6) . ? Cl3S C2S 1.715(11) . ? Cl4S C2S 1.741(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C51A As1A C61A 97.13(12) . . ? C51A As1A P1A 101.82(8) . . ? C61A As1A P1A 97.93(9) . . ? C11A P1A P4A 112.13(10) . . ? C11A P1A P2A 112.56(10) . . ? P4A P1A P2A 84.78(4) . . ? C11A P1A As1A 107.50(10) . . ? P4A P1A As1A 127.61(4) . . ? P2A P1A As1A 110.12(3) . . ? C21A P2A P1A 103.66(9) . . ? C21A P2A P3A 105.68(9) . . ? P1A P2A P3A 81.70(4) . . ? C31A P3A P4A 103.59(11) . . ? C31A P3A P2A 104.97(11) . . ? P4A P3A P2A 83.16(4) . . ? C41A P4A P1A 111.19(10) . . ? C41A P4A P3A 102.81(10) . . ? P1A P4A P3A 82.01(4) . . ? C62A N1A C52A 127.5(2) . . ? C12A C11A C16A 110.3(2) . . ? C12A C11A P1A 111.6(2) . . ? C16A C11A P1A 113.1(2) . . ? C13A C12A C11A 109.6(3) . . ? C12A C13A C14A 111.8(3) . . ? C15A C14A C13A 111.3(3) . . ? C14A C15A C16A 112.5(3) . . ? C15A C16A C11A 110.0(3) . . ? C26A C21A C22A 110.4(2) . . ? C26A C21A P2A 108.24(18) . . ? C22A C21A P2A 108.64(19) . . ? C21A C22A C23A 110.7(3) . . ? C24A C23A C22A 110.5(3) . . ? C25A C24A C23A 111.2(3) . . ? C24A C25A C26A 111.7(3) . . ? C25A C26A C21A 110.9(2) . . ? C36A C31A C32A 111.6(3) . . ? C36A C31A P3A 117.7(2) . . ? C32A C31A P3A 108.6(2) . . ? C31A C32A C33A 109.6(3) . . ? C34A C33A C32A 111.4(4) . . ? C33A C34A C35A 111.5(4) . . ? C34A C35A C36A 110.5(4) . . ? C31A C36A C35A 110.7(4) . . ? C42A C41A C46A 110.2(2) . . ? C42A C41A P4A 111.2(2) . . ? C46A C41A P4A 105.65(19) . . ? C43A C42A C41A 111.2(3) . . ? C44A C43A C42A 111.7(3) . . ? C45A C44A C43A 111.0(3) . . ? C44A C45A C46A 111.2(3) . . ? C45A C46A C41A 111.2(3) . . ? C52A C51A C56A 119.6(3) . . ? C52A C51A As1A 122.6(2) . . ? C56A C51A As1A 117.8(2) . . ? C51A C52A N1A 123.2(3) . . ? C51A C52A C53A 119.1(3) . . ? N1A C52A C53A 117.8(3) . . ? C54A C53A C52A 120.1(3) . . ? C53A C54A C55A 121.0(3) . . ? C56A C55A C54A 119.2(3) . . ? C55A C56A C51A 121.0(3) . . ? C66A C61A C62A 119.5(3) . . ? C66A C61A As1A 117.7(2) . . ? C62A C61A As1A 122.7(2) . . ? N1A C62A C63A 118.4(3) . . ? N1A C62A C61A 122.9(3) . . ? C63A C62A C61A 118.6(3) . . ? C64A C63A C62A 120.5(3) . . ? C63A C64A C65A 121.0(3) . . ? C66A C65A C64A 119.4(3) . . ? C65A C66A C61A 120.9(3) . . ? C61B As1B C51B 97.76(12) . . ? C61B As1B P1B 97.21(8) . . ? C51B As1B P1B 99.24(8) . . ? C11B P1B P4B 110.55(9) . . ? C11B P1B P2B 111.04(9) . . ? P4B P1B P2B 85.93(3) . . ? C11B P1B As1B 108.47(9) . . ? P4B P1B As1B 127.27(3) . . ? P2B P1B As1B 111.29(3) . . ? C21B P2B P1B 104.41(8) . . ? C21B P2B P3B 104.27(9) . . ? P1B P2B P3B 84.45(3) . . ? C31B P3B P4B 99.06(9) . . ? C31B P3B P2B 99.86(9) . . ? P4B P3B P2B 84.35(3) . . ? C41B P4B P1B 107.63(9) . . ? C41B P4B P3B 109.75(9) . . ? P1B P4B P3B 84.85(3) . . ? C52B N1B C62B 128.7(2) . . ? C16B C11B C12B 110.8(2) . . ? C16B C11B P1B 111.54(17) . . ? C12B C11B P1B 110.88(18) . . ? C13B C12B C11B 110.5(2) . . ? C14B C13B C12B 110.6(2) . . ? C15B C14B C13B 110.8(2) . . ? C16B C15B C14B 111.6(2) . . ? C15B C16B C11B 111.4(2) . . ? C22B C21B C26B 111.2(2) . . ? C22B C21B P2B 110.18(18) . . ? C26B C21B P2B 108.23(18) . . ? C21B C22B C23B 111.0(2) . . ? C24B C23B C22B 110.5(2) . . ? C25B C24B C23B 112.3(3) . . ? C24B C25B C26B 111.7(3) . . ? C25B C26B C21B 110.3(2) . . ? C32B C31B C36B 110.8(2) . . ? C32B C31B P3B 110.08(18) . . ? C36B C31B P3B 109.14(18) . . ? C31B C32B C33B 111.3(2) . . ? C34B C33B C32B 110.9(2) . . ? C35B C34B C33B 111.1(2) . . ? C34B C35B C36B 111.6(2) . . ? C35B C36B C31B 111.3(2) . . ? C46B C41B C42B 111.7(2) . . ? C46B C41B P4B 107.54(18) . . ? C42B C41B P4B 107.83(18) . . ? C41B C42B C43B 110.7(2) . . ? C44B C43B C42B 111.4(2) . . ? C45B C44B C43B 110.6(2) . . ? C44B C45B C46B 110.7(3) . . ? C41B C46B C45B 111.0(2) . . ? C56B C51B C52B 119.5(3) . . ? C56B C51B As1B 117.7(2) . . ? C52B C51B As1B 122.8(2) . . ? N1B C52B C51B 123.9(3) . . ? N1B C52B C53B 117.8(3) . . ? C51B C52B C53B 118.2(3) . . ? C54B C53B C52B 121.0(3) . . ? C53B C54B C55B 121.0(3) . . ? C56B C55B C54B 118.4(3) . . ? C55B C56B C51B 121.9(3) . . ? C62B C61B C66B 119.2(3) . . ? C62B C61B As1B 123.1(2) . . ? C66B C61B As1B 117.7(2) . . ? N1B C62B C61B 123.6(3) . . ? N1B C62B C63B 118.4(3) . . ? C61B C62B C63B 118.0(3) . . ? C64B C63B C62B 121.1(3) . . ? C63B C64B C65B 121.3(3) . . ? C66B C65B C64B 118.7(3) . . ? C65B C66B C61B 121.6(3) . . ? Cl4 Ga1 Cl1 113.39(4) . . ? Cl4 Ga1 Cl2 109.91(4) . . ? Cl1 Ga1 Cl2 107.80(4) . . ? Cl4 Ga1 Cl3 106.89(4) . . ? Cl1 Ga1 Cl3 106.88(4) . . ? Cl2 Ga1 Cl3 112.01(3) . . ? Cl6 Ga2 Cl5 108.13(4) . . ? Cl6 Ga2 Cl8 107.84(4) . . ? Cl5 Ga2 Cl8 111.69(4) . . ? Cl6 Ga2 Cl7 110.94(4) . . ? Cl5 Ga2 Cl7 108.84(4) . . ? Cl8 Ga2 Cl7 109.39(4) . . ? Cl1S C1S Cl2S 110.6(3) . . ? Cl3S C2S Cl4S 110.0(8) . . ? 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 C51A As1A P1A C11A 138.81(13) . . . . ? C61A As1A P1A C11A 39.76(13) . . . . ? C51A As1A P1A P4A 0.95(10) . . . . ? C61A As1A P1A P4A -98.10(10) . . . . ? C51A As1A P1A P2A -98.24(9) . . . . ? C61A As1A P1A P2A 162.71(9) . . . . ? C11A P1A P2A C21A 105.02(14) . . . . ? P4A P1A P2A C21A -143.16(10) . . . . ? As1A P1A P2A C21A -14.91(10) . . . . ? C11A P1A P2A P3A -150.76(10) . . . . ? P4A P1A P2A P3A -38.94(4) . . . . ? As1A P1A P2A P3A 89.31(4) . . . . ? C21A P2A P3A C31A -117.39(14) . . . . ? P1A P2A P3A C31A 140.67(11) . . . . ? C21A P2A P3A P4A 140.32(9) . . . . ? P1A P2A P3A P4A 38.38(3) . . . . ? C11A P1A P4A C41A -107.98(14) . . . . ? P2A P1A P4A C41A 139.77(10) . . . . ? As1A P1A P4A C41A 28.33(11) . . . . ? C11A P1A P4A P3A 151.32(11) . . . . ? P2A P1A P4A P3A 39.07(4) . . . . ? As1A P1A P4A P3A -72.37(5) . . . . ? C31A P3A P4A C41A 107.70(14) . . . . ? P2A P3A P4A C41A -148.49(10) . . . . ? C31A P3A P4A P1A -142.28(12) . . . . ? P2A P3A P4A P1A -38.47(3) . . . . ? P4A P1A C11A C12A 58.1(2) . . . . ? P2A P1A C11A C12A 151.70(18) . . . . ? As1A P1A C11A C12A -86.9(2) . . . . ? P4A P1A C11A C16A -67.0(2) . . . . ? P2A P1A C11A C16A 26.6(2) . . . . ? As1A P1A C11A C16A 148.1(2) . . . . ? C16A C11A C12A C13A -59.5(3) . . . . ? P1A C11A C12A C13A 173.9(2) . . . . ? C11A C12A C13A C14A 57.8(4) . . . . ? C12A C13A C14A C15A -54.5(4) . . . . ? C13A C14A C15A C16A 52.9(4) . . . . ? C14A C15A C16A C11A -54.7(4) . . . . ? C12A C11A C16A C15A 57.7(4) . . . . ? P1A C11A C16A C15A -176.5(2) . . . . ? P1A P2A C21A C26A 169.77(18) . . . . ? P3A P2A C21A C26A 84.71(19) . . . . ? P1A P2A C21A C22A -70.3(2) . . . . ? P3A P2A C21A C22A -155.40(17) . . . . ? C26A C21A C22A C23A -57.3(3) . . . . ? P2A C21A C22A C23A -175.8(2) . . . . ? C21A C22A C23A C24A 56.8(4) . . . . ? C22A C23A C24A C25A -55.8(4) . . . . ? C23A C24A C25A C26A 55.6(4) . . . . ? C24A C25A C26A C21A -55.9(4) . . . . ? C22A C21A C26A C25A 56.5(3) . . . . ? P2A C21A C26A C25A 175.2(2) . . . . ? P4A P3A C31A C36A 36.6(3) . . . . ? P2A P3A C31A C36A -49.8(3) . . . . ? P4A P3A C31A C32A 164.6(3) . . . . ? P2A P3A C31A C32A 78.1(3) . . . . ? C36A C31A C32A C33A -56.1(5) . . . . ? P3A C31A C32A C33A 172.5(4) . . . . ? C31A C32A C33A C34A 55.9(6) . . . . ? C32A C33A C34A C35A -56.9(5) . . . . ? C33A C34A C35A C36A 56.4(6) . . . . ? C32A C31A C36A C35A 56.8(5) . . . . ? P3A C31A C36A C35A -176.7(3) . . . . ? C34A C35A C36A C31A -56.1(6) . . . . ? P1A P4A C41A C42A 86.1(2) . . . . ? P3A P4A C41A C42A 172.35(19) . . . . ? P1A P4A C41A C46A -154.38(16) . . . . ? P3A P4A C41A C46A -68.09(19) . . . . ? C46A C41A C42A C43A 55.6(4) . . . . ? P4A C41A C42A C43A 172.4(2) . . . . ? C41A C42A C43A C44A -55.4(4) . . . . ? C42A C43A C44A C45A 55.0(4) . . . . ? C43A C44A C45A C46A -55.5(4) . . . . ? C44A C45A C46A C41A 56.7(4) . . . . ? C42A C41A C46A C45A -56.4(3) . . . . ? P4A C41A C46A C45A -176.7(2) . . . . ? C61A As1A C51A C52A 11.5(3) . . . . ? P1A As1A C51A C52A -88.2(2) . . . . ? C61A As1A C51A C56A -166.7(2) . . . . ? P1A As1A C51A C56A 93.6(2) . . . . ? C56A C51A C52A N1A -178.8(3) . . . . ? As1A C51A C52A N1A 3.1(4) . . . . ? C56A C51A C52A C53A 0.2(4) . . . . ? As1A C51A C52A C53A -178.0(2) . . . . ? C62A N1A C52A C51A -20.1(4) . . . . ? C62A N1A C52A C53A 160.8(3) . . . . ? C51A C52A C53A C54A -0.2(4) . . . . ? N1A C52A C53A C54A 178.9(3) . . . . ? C52A C53A C54A C55A -0.2(5) . . . . ? C53A C54A C55A C56A 0.5(5) . . . . ? C54A C55A C56A C51A -0.5(5) . . . . ? C52A C51A C56A C55A 0.1(5) . . . . ? As1A C51A C56A C55A 178.4(2) . . . . ? C51A As1A C61A C66A 167.3(2) . . . . ? P1A As1A C61A C66A -89.6(2) . . . . ? C51A As1A C61A C62A -15.6(3) . . . . ? P1A As1A C61A C62A 87.5(2) . . . . ? C52A N1A C62A C63A -164.2(3) . . . . ? C52A N1A C62A C61A 15.5(4) . . . . ? C66A C61A C62A N1A -177.6(3) . . . . ? As1A C61A C62A N1A 5.4(4) . . . . ? C66A C61A C62A C63A 2.1(4) . . . . ? As1A C61A C62A C63A -175.0(2) . . . . ? N1A C62A C63A C64A 178.6(3) . . . . ? C61A C62A C63A C64A -1.1(5) . . . . ? C62A C63A C64A C65A -0.8(5) . . . . ? C63A C64A C65A C66A 1.7(5) . . . . ? C64A C65A C66A C61A -0.7(5) . . . . ? C62A C61A C66A C65A -1.2(5) . . . . ? As1A C61A C66A C65A 176.0(2) . . . . ? C61B As1B P1B C11B 42.87(12) . . . . ? C51B As1B P1B C11B 141.99(12) . . . . ? C61B As1B P1B P4B -93.12(10) . . . . ? C51B As1B P1B P4B 6.00(10) . . . . ? C61B As1B P1B P2B 165.31(9) . . . . ? C51B As1B P1B P2B -95.58(9) . . . . ? C11B P1B P2B C21B 112.82(12) . . . . ? P4B P1B P2B C21B -136.71(9) . . . . ? As1B P1B P2B C21B -8.11(9) . . . . ? C11B P1B P2B P3B -143.83(9) . . . . ? P4B P1B P2B P3B -33.36(3) . . . . ? As1B P1B P2B P3B 95.23(3) . . . . ? C21B P2B P3B C31B -125.31(12) . . . . ? P1B P2B P3B C31B 131.20(9) . . . . ? C21B P2B P3B P4B 136.45(9) . . . . ? P1B P2B P3B P4B 32.96(3) . . . . ? C11B P1B P4B C41B -106.38(13) . . . . ? P2B P1B P4B C41B 142.66(9) . . . . ? As1B P1B P4B C41B 28.89(10) . . . . ? C11B P1B P4B P3B 144.51(9) . . . . ? P2B P1B P4B P3B 33.55(3) . . . . ? As1B P1B P4B P3B -80.23(4) . . . . ? C31B P3B P4B C41B 120.96(12) . . . . ? P2B P3B P4B C41B -139.91(9) . . . . ? C31B P3B P4B P1B -132.13(9) . . . . ? P2B P3B P4B P1B -33.01(3) . . . . ? P4B P1B C11B C16B -23.2(2) . . . . ? P2B P1B C11B C16B 70.38(19) . . . . ? As1B P1B C11B C16B -167.03(17) . . . . ? P4B P1B C11B C12B -147.29(16) . . . . ? P2B P1B C11B C12B -53.7(2) . . . . ? As1B P1B C11B C12B 68.91(19) . . . . ? C16B C11B C12B C13B 56.0(3) . . . . ? P1B C11B C12B C13B -179.55(19) . . . . ? C11B C12B C13B C14B -57.2(3) . . . . ? C12B C13B C14B C15B 57.2(3) . . . . ? C13B C14B C15B C16B -56.3(3) . . . . ? C14B C15B C16B C11B 55.3(3) . . . . ? C12B C11B C16B C15B -55.0(3) . . . . ? P1B C11B C16B C15B -179.0(2) . . . . ? P1B P2B C21B C22B -76.31(18) . . . . ? P3B P2B C21B C22B -164.15(16) . . . . ? P1B P2B C21B C26B 161.89(16) . . . . ? P3B P2B C21B C26B 74.05(18) . . . . ? C26B C21B C22B C23B -56.8(3) . . . . ? P2B C21B C22B C23B -176.81(19) . . . . ? C21B C22B C23B C24B 55.7(3) . . . . ? C22B C23B C24B C25B -55.1(4) . . . . ? C23B C24B C25B C26B 55.2(4) . . . . ? C24B C25B C26B C21B -54.8(3) . . . . ? C22B C21B C26B C25B 55.8(3) . . . . ? P2B C21B C26B C25B 177.0(2) . . . . ? P4B P3B C31B C32B 157.86(17) . . . . ? P2B P3B C31B C32B 72.07(18) . . . . ? P4B P3B C31B C36B -80.39(18) . . . . ? P2B P3B C31B C36B -166.18(17) . . . . ? C36B C31B C32B C33B 55.9(3) . . . . ? P3B C31B C32B C33B 176.70(19) . . . . ? C31B C32B C33B C34B -56.5(3) . . . . ? C32B C33B C34B C35B 56.0(3) . . . . ? C33B C34B C35B C36B -55.4(3) . . . . ? C34B C35B C36B C31B 55.0(3) . . . . ? C32B C31B C36B C35B -55.0(3) . . . . ? P3B C31B C36B C35B -176.29(19) . . . . ? P1B P4B C41B C46B -163.38(16) . . . . ? P3B P4B C41B C46B -72.57(19) . . . . ? P1B P4B C41B C42B 76.04(19) . . . . ? P3B P4B C41B C42B 166.84(16) . . . . ? C46B C41B C42B C43B 53.7(3) . . . . ? P4B C41B C42B C43B 171.6(2) . . . . ? C41B C42B C43B C44B -54.9(3) . . . . ? C42B C43B C44B C45B 57.4(3) . . . . ? C43B C44B C45B C46B -58.0(3) . . . . ? C42B C41B C46B C45B -54.8(3) . . . . ? P4B C41B C46B C45B -173.0(2) . . . . ? C44B C45B C46B C41B 56.8(3) . . . . ? C61B As1B C51B C56B -177.0(2) . . . . ? P1B As1B C51B C56B 84.3(2) . . . . ? C61B As1B C51B C52B 1.7(2) . . . . ? P1B As1B C51B C52B -97.0(2) . . . . ? C62B N1B C52B C51B -3.5(5) . . . . ? C62B N1B C52B C53B 177.3(3) . . . . ? C56B C51B C52B N1B 179.9(3) . . . . ? As1B C51B C52B N1B 1.3(4) . . . . ? C56B C51B C52B C53B -0.9(4) . . . . ? As1B C51B C52B C53B -179.5(2) . . . . ? N1B C52B C53B C54B 178.9(3) . . . . ? C51B C52B C53B C54B -0.3(4) . . . . ? C52B C53B C54B C55B 1.3(5) . . . . ? C53B C54B C55B C56B -0.9(5) . . . . ? C54B C55B C56B C51B -0.4(5) . . . . ? C52B C51B C56B C55B 1.3(4) . . . . ? As1B C51B C56B C55B 180.0(2) . . . . ? C51B As1B C61B C62B -3.5(2) . . . . ? P1B As1B C61B C62B 96.9(2) . . . . ? C51B As1B C61B C66B 176.8(2) . . . . ? P1B As1B C61B C66B -82.8(2) . . . . ? C52B N1B C62B C61B 1.4(4) . . . . ? C52B N1B C62B C63B -178.0(3) . . . . ? C66B C61B C62B N1B -177.7(3) . . . . ? As1B C61B C62B N1B 2.5(4) . . . . ? C66B C61B C62B C63B 1.7(4) . . . . ? As1B C61B C62B C63B -178.0(2) . . . . ? N1B C62B C63B C64B 179.3(3) . . . . ? C61B C62B C63B C64B -0.2(4) . . . . ? C62B C63B C64B C65B -0.7(5) . . . . ? C63B C64B C65B C66B -0.1(5) . . . . ? C64B C65B C66B C61B 1.7(5) . . . . ? C62B C61B C66B C65B -2.6(4) . . . . ? As1B C61B C66B C65B 177.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.896 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.114 # Attachment '[AN_PCy_4][OTf].cif' data_dal0907 _database_code_depnum_ccdc_archive 'CCDC 747681' #TrackingRef '[AN_PCy_4][OTf].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H53 As N P4, C F3 O3 S' _chemical_formula_sum 'C37 H53 As F3 N O3 P4 S' _chemical_formula_weight 847.66 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' N N 0.0061 0.0033 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5413(7) _cell_length_b 11.5635(7) _cell_length_c 15.3553(9) _cell_angle_alpha 99.0907(8) _cell_angle_beta 96.0351(8) _cell_angle_gamma 91.1938(8) _cell_volume 2010.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5124 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.78 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6623 _exptl_absorpt_correction_T_max 0.9246 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16803 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9010 _reflns_number_gt 6730 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. 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^)+(0.0422P)^2^+0.4548P] 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 9010 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 As As 0.22777(2) 0.50914(2) 0.130920(17) 0.02575(8) Uani 1 1 d . . . P1 P 0.23474(6) 0.51464(6) 0.29259(4) 0.02238(15) Uani 1 1 d . . . P2 P 0.14485(6) 0.66820(6) 0.35366(5) 0.02655(16) Uani 1 1 d . . . P3 P 0.32349(6) 0.75179(6) 0.38683(5) 0.02725(16) Uani 1 1 d . . . P4 P 0.38005(6) 0.57067(6) 0.39699(4) 0.02414(15) Uani 1 1 d . . . N N 0.49001(19) 0.42028(19) 0.10966(14) 0.0292(5) Uani 1 1 d . . . H1N H 0.5622 0.3971 0.1113 0.035 Uiso 1 1 calc R . . C11 C 0.1642(2) 0.3758(2) 0.30855(16) 0.0243(5) Uani 1 1 d . . . H11 H 0.1102 0.3472 0.2537 0.029 Uiso 1 1 calc R . . C12 C 0.2546(2) 0.2818(2) 0.31801(18) 0.0290(6) Uani 1 1 d . . . H12A H 0.2996 0.2719 0.2661 0.035 Uiso 1 1 calc R . . H12B H 0.3097 0.3070 0.3719 0.035 Uiso 1 1 calc R . . C13 C 0.1938(3) 0.1650(2) 0.3244(2) 0.0379(7) Uani 1 1 d . . . H13A H 0.1453 0.1360 0.2678 0.045 Uiso 1 1 calc R . . H13B H 0.2534 0.1065 0.3340 0.045 Uiso 1 1 calc R . . C14 C 0.1173(3) 0.1775(2) 0.4000(2) 0.0426(8) Uani 1 1 d . . . H14A H 0.0744 0.1022 0.3990 0.051 Uiso 1 1 calc R . . H14B H 0.1673 0.1956 0.4573 0.051 Uiso 1 1 calc R . . C15 C 0.0308(3) 0.2734(2) 0.3934(2) 0.0416(7) Uani 1 1 d . . . H15A H -0.0122 0.2834 0.4464 0.050 Uiso 1 1 calc R . . H15B H -0.0265 0.2497 0.3406 0.050 Uiso 1 1 calc R . . C16 C 0.0911(2) 0.3902(2) 0.38652(19) 0.0324(6) Uani 1 1 d . . . H16A H 0.0316 0.4492 0.3783 0.039 Uiso 1 1 calc R . . H16B H 0.1418 0.4186 0.4422 0.039 Uiso 1 1 calc R . . C21 C 0.0797(2) 0.7320(2) 0.25712(17) 0.0258(6) Uani 1 1 d . . . H21 H 0.1361 0.7276 0.2117 0.031 Uiso 1 1 calc R . . C22 C -0.0322(2) 0.6611(2) 0.21679(18) 0.0307(6) Uani 1 1 d . . . H22A H -0.0127 0.5795 0.1946 0.037 Uiso 1 1 calc R . . H22B H -0.0853 0.6591 0.2632 0.037 Uiso 1 1 calc R . . C23 C -0.0934(2) 0.7148(2) 0.14071(19) 0.0350(7) Uani 1 1 d . . . H23A H -0.0433 0.7101 0.0919 0.042 Uiso 1 1 calc R . . H23B H -0.1672 0.6698 0.1177 0.042 Uiso 1 1 calc R . . C24 C -0.1194(2) 0.8423(2) 0.1718(2) 0.0393(7) Uani 1 1 d . . . H24A H -0.1560 0.8765 0.1210 0.047 Uiso 1 1 calc R . . H24B H -0.1752 0.8463 0.2169 0.047 Uiso 1 1 calc R . . C25 C -0.0089(3) 0.9130(2) 0.2114(2) 0.0432(8) Uani 1 1 d . . . H25A H -0.0288 0.9945 0.2335 0.052 Uiso 1 1 calc R . . H25B H 0.0437 0.9154 0.1647 0.052 Uiso 1 1 calc R . . C26 C 0.0541(2) 0.8600(2) 0.28764(19) 0.0338(7) Uani 1 1 d . . . H26A H 0.1281 0.9050 0.3096 0.041 Uiso 1 1 calc R . . H26B H 0.0050 0.8654 0.3372 0.041 Uiso 1 1 calc R . . C31 C 0.3177(2) 0.8130(2) 0.50668(17) 0.0294(6) Uani 1 1 d . . . H31 H 0.2834 0.7515 0.5363 0.035 Uiso 1 1 calc R . . C32 C 0.2398(3) 0.9179(3) 0.5138(2) 0.0440(8) Uani 1 1 d . . . H32A H 0.1596 0.8919 0.4878 0.053 Uiso 1 1 calc R . . H32B H 0.2685 0.9758 0.4792 0.053 Uiso 1 1 calc R . . C33 C 0.2373(3) 0.9765(3) 0.6100(2) 0.0534(9) Uani 1 1 d . . . H33A H 0.1901 1.0472 0.6116 0.064 Uiso 1 1 calc R . . H33B H 0.1999 0.9218 0.6431 0.064 Uiso 1 1 calc R . . C34 C 0.3602(3) 1.0112(3) 0.6548(2) 0.0536(9) Uani 1 1 d . . . H34A H 0.3942 1.0727 0.6260 0.064 Uiso 1 1 calc R . . H34B H 0.3563 1.0442 0.7180 0.064 Uiso 1 1 calc R . . C35 C 0.4380(3) 0.9069(3) 0.6489(2) 0.0470(8) Uani 1 1 d . . . H35A H 0.4094 0.8495 0.6839 0.056 Uiso 1 1 calc R . . H35B H 0.5183 0.9332 0.6747 0.056 Uiso 1 1 calc R . . C36 C 0.4400(2) 0.8478(2) 0.55241(19) 0.0362(7) Uani 1 1 d . . . H36A H 0.4779 0.9021 0.5194 0.043 Uiso 1 1 calc R . . H36B H 0.4869 0.7770 0.5511 0.043 Uiso 1 1 calc R . . C41 C 0.5184(2) 0.5561(2) 0.34524(16) 0.0251(6) Uani 1 1 d . . . H41 H 0.5062 0.5781 0.2846 0.030 Uiso 1 1 calc R . . C42 C 0.5555(2) 0.4295(2) 0.33793(18) 0.0308(6) Uani 1 1 d . . . H42A H 0.4973 0.3782 0.2967 0.037 Uiso 1 1 calc R . . H42B H 0.5578 0.4046 0.3968 0.037 Uiso 1 1 calc R . . C43 C 0.6755(2) 0.4149(3) 0.30450(19) 0.0391(7) Uani 1 1 d . . . H43A H 0.6997 0.3335 0.3057 0.047 Uiso 1 1 calc R . . H43B H 0.6705 0.4289 0.2423 0.047 Uiso 1 1 calc R . . C44 C 0.7662(2) 0.4992(3) 0.36084(19) 0.0413(7) Uani 1 1 d . . . H44A H 0.8412 0.4917 0.3349 0.050 Uiso 1 1 calc R . . H44B H 0.7785 0.4789 0.4213 0.050 Uiso 1 1 calc R . . C45 C 0.7285(2) 0.6247(3) 0.3664(2) 0.0405(7) Uani 1 1 d . . . H45A H 0.7229 0.6473 0.3066 0.049 Uiso 1 1 calc R . . H45B H 0.7878 0.6774 0.4054 0.049 Uiso 1 1 calc R . . C46 C 0.6112(2) 0.6393(2) 0.40281(18) 0.0321(6) Uani 1 1 d . . . H46A H 0.5875 0.7212 0.4040 0.038 Uiso 1 1 calc R . . H46B H 0.6181 0.6225 0.4644 0.038 Uiso 1 1 calc R . . C51 C 0.2855(2) 0.3552(2) 0.10380(16) 0.0270(6) Uani 1 1 d . . . C52 C 0.4047(2) 0.3329(2) 0.10197(16) 0.0278(6) Uani 1 1 d . . . C53 C 0.4387(3) 0.2164(2) 0.08980(19) 0.0366(7) Uani 1 1 d . . . H53 H 0.5192 0.2003 0.0904 0.044 Uiso 1 1 calc R . . C54 C 0.3577(3) 0.1252(3) 0.0771(2) 0.0426(8) Uani 1 1 d . . . H54 H 0.3826 0.0468 0.0694 0.051 Uiso 1 1 calc R . . C55 C 0.2386(3) 0.1465(3) 0.07521(19) 0.0403(7) Uani 1 1 d . . . H55 H 0.1825 0.0832 0.0650 0.048 Uiso 1 1 calc R . . C56 C 0.2042(2) 0.2605(2) 0.08847(17) 0.0335(6) Uani 1 1 d . . . H56 H 0.1234 0.2754 0.0872 0.040 Uiso 1 1 calc R . . C61 C 0.3710(2) 0.5946(2) 0.12648(17) 0.0280(6) Uani 1 1 d . . . C62 C 0.4768(2) 0.5397(2) 0.11513(16) 0.0265(6) Uani 1 1 d . . . C63 C 0.5768(2) 0.6090(2) 0.11150(17) 0.0317(6) Uani 1 1 d . . . H63 H 0.6488 0.5729 0.1031 0.038 Uiso 1 1 calc R . . C64 C 0.5713(3) 0.7286(3) 0.11999(19) 0.0373(7) Uani 1 1 d . . . H64 H 0.6400 0.7745 0.1182 0.045 Uiso 1 1 calc R . . C65 C 0.4669(3) 0.7837(3) 0.1311(2) 0.0403(7) Uani 1 1 d . . . H65 H 0.4639 0.8666 0.1373 0.048 Uiso 1 1 calc R . . C66 C 0.3677(2) 0.7163(2) 0.13313(18) 0.0339(6) Uani 1 1 d . . . H66 H 0.2957 0.7534 0.1391 0.041 Uiso 1 1 calc R . . S S 0.84743(6) 0.32294(6) 0.09173(5) 0.03657(18) Uani 1 1 d . . . F1 F 0.9209(2) 0.11085(18) 0.08806(17) 0.0817(7) Uani 1 1 d . . . F2 F 0.7787(3) 0.1504(3) 0.1644(3) 0.1277(12) Uani 1 1 d . . . F3 F 0.7486(3) 0.1222(2) 0.0250(3) 0.1501(16) Uani 1 1 d . . . O1 O 0.73310(17) 0.36745(19) 0.08994(14) 0.0452(5) Uani 1 1 d . . . O2 O 0.8994(3) 0.3245(3) 0.0128(2) 0.1048(12) Uani 1 1 d . . . O3 O 0.9209(2) 0.3575(2) 0.1716(2) 0.0826(10) Uani 1 1 d . . . C1 C 0.8228(3) 0.1695(3) 0.0921(3) 0.0596(10) 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 As 0.02332(15) 0.03025(15) 0.02326(14) 0.00465(11) -0.00014(11) 0.00218(11) P1 0.0229(3) 0.0216(3) 0.0226(3) 0.0039(3) 0.0017(3) 0.0012(3) P2 0.0286(4) 0.0231(3) 0.0283(4) 0.0031(3) 0.0053(3) 0.0041(3) P3 0.0313(4) 0.0226(3) 0.0271(4) 0.0024(3) 0.0027(3) 0.0001(3) P4 0.0255(4) 0.0245(3) 0.0222(3) 0.0031(3) 0.0022(3) 0.0008(3) N 0.0207(11) 0.0341(13) 0.0314(12) 0.0020(10) 0.0011(9) 0.0047(10) C11 0.0241(13) 0.0242(13) 0.0243(13) 0.0060(10) -0.0012(11) -0.0033(11) C12 0.0295(14) 0.0217(13) 0.0347(15) 0.0028(11) 0.0013(12) 0.0003(11) C13 0.0425(17) 0.0227(14) 0.0479(18) 0.0062(13) 0.0032(14) -0.0035(13) C14 0.058(2) 0.0282(15) 0.0417(18) 0.0085(13) 0.0057(15) -0.0113(14) C15 0.0450(18) 0.0329(16) 0.0498(19) 0.0087(14) 0.0162(15) -0.0061(14) C16 0.0322(15) 0.0274(14) 0.0389(16) 0.0075(12) 0.0073(13) -0.0007(12) C21 0.0235(13) 0.0237(13) 0.0302(14) 0.0028(11) 0.0041(11) 0.0028(11) C22 0.0272(14) 0.0260(14) 0.0383(16) 0.0027(12) 0.0054(12) -0.0002(11) C23 0.0264(15) 0.0377(16) 0.0381(16) -0.0005(13) 0.0001(12) -0.0012(12) C24 0.0328(16) 0.0375(17) 0.0456(18) 0.0069(14) -0.0065(14) 0.0054(13) C25 0.0429(18) 0.0289(16) 0.055(2) 0.0108(14) -0.0121(15) 0.0019(13) C26 0.0319(15) 0.0231(14) 0.0437(17) 0.0024(12) -0.0042(13) 0.0038(12) C31 0.0359(15) 0.0236(14) 0.0275(14) 0.0010(11) 0.0031(12) -0.0012(12) C32 0.0470(19) 0.0402(18) 0.0399(18) -0.0074(14) 0.0011(15) 0.0116(15) C33 0.057(2) 0.052(2) 0.0441(19) -0.0150(16) 0.0047(17) 0.0137(17) C34 0.065(2) 0.0392(19) 0.048(2) -0.0178(15) 0.0071(17) -0.0030(17) C35 0.0467(19) 0.051(2) 0.0364(17) -0.0107(15) -0.0012(15) -0.0003(16) C36 0.0352(16) 0.0331(16) 0.0368(16) -0.0033(13) 0.0010(13) 0.0014(13) C41 0.0236(13) 0.0299(14) 0.0214(13) 0.0042(11) 0.0007(10) 0.0005(11) C42 0.0288(14) 0.0319(15) 0.0295(15) -0.0011(12) 0.0025(12) 0.0018(12) C43 0.0324(16) 0.0499(19) 0.0334(16) 0.0011(14) 0.0032(13) 0.0111(14) C44 0.0264(15) 0.063(2) 0.0343(16) 0.0074(15) 0.0018(13) 0.0069(14) C45 0.0290(16) 0.0490(19) 0.0417(17) 0.0025(15) 0.0036(13) -0.0065(14) C46 0.0299(15) 0.0328(15) 0.0325(15) 0.0031(12) 0.0027(12) -0.0037(12) C51 0.0263(14) 0.0295(14) 0.0228(13) -0.0015(11) 0.0002(11) 0.0012(11) C52 0.0304(15) 0.0322(15) 0.0199(13) 0.0035(11) 0.0006(11) -0.0002(12) C53 0.0350(16) 0.0367(16) 0.0367(16) 0.0010(13) 0.0027(13) 0.0087(13) C54 0.054(2) 0.0278(16) 0.0434(18) -0.0019(13) 0.0042(15) 0.0038(14) C55 0.0431(18) 0.0332(16) 0.0397(17) -0.0058(13) 0.0009(14) -0.0073(14) C56 0.0317(15) 0.0385(16) 0.0269(14) -0.0022(12) 0.0003(12) -0.0031(13) C61 0.0270(14) 0.0356(15) 0.0226(13) 0.0099(11) 0.0014(11) -0.0006(12) C62 0.0285(14) 0.0338(15) 0.0169(12) 0.0054(11) -0.0010(10) -0.0001(12) C63 0.0250(14) 0.0437(17) 0.0263(14) 0.0060(12) 0.0021(11) 0.0000(12) C64 0.0337(16) 0.0428(18) 0.0353(16) 0.0097(14) 0.0012(13) -0.0117(14) C65 0.0451(18) 0.0317(16) 0.0461(18) 0.0139(14) 0.0043(15) -0.0021(14) C66 0.0335(16) 0.0348(16) 0.0359(16) 0.0121(13) 0.0048(13) 0.0034(13) S 0.0275(4) 0.0367(4) 0.0464(4) 0.0093(3) 0.0034(3) 0.0059(3) F1 0.0824(17) 0.0493(13) 0.112(2) 0.0121(13) -0.0026(14) 0.0297(12) F2 0.123(2) 0.092(2) 0.201(4) 0.091(2) 0.070(3) 0.0117(17) F3 0.140(3) 0.0533(16) 0.209(4) -0.0497(19) -0.097(3) 0.0120(16) O1 0.0311(11) 0.0558(14) 0.0482(13) 0.0042(11) 0.0056(10) 0.0161(10) O2 0.088(2) 0.149(3) 0.116(3) 0.090(2) 0.074(2) 0.067(2) O3 0.0660(17) 0.0542(16) 0.106(2) -0.0122(15) -0.0513(16) 0.0049(13) C1 0.059(2) 0.046(2) 0.069(3) 0.0046(19) -0.008(2) 0.0084(18) _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 As C51 1.913(3) . ? As C61 1.921(3) . ? As P1 2.4660(7) . ? As O2 3.391(3) 2_665 ? P1 C11 1.847(2) . ? P1 P4 2.2053(9) . ? P1 P2 2.2054(10) . ? P2 C21 1.855(3) . ? P2 P3 2.2327(10) . ? P3 C31 1.873(3) . ? P3 P4 2.2306(10) . ? P4 C41 1.856(3) . ? N C52 1.379(3) . ? N C62 1.383(3) . ? C11 C16 1.526(4) . ? C11 C12 1.535(3) . ? C12 C13 1.531(4) . ? C13 C14 1.522(4) . ? C14 C15 1.515(4) . ? C15 C16 1.530(4) . ? C21 C26 1.524(3) . ? C21 C22 1.533(3) . ? C22 C23 1.524(4) . ? C23 C24 1.523(4) . ? C24 C25 1.516(4) . ? C25 C26 1.530(4) . ? C31 C32 1.522(4) . ? C31 C36 1.525(4) . ? C32 C33 1.529(4) . ? C33 C34 1.526(4) . ? C34 C35 1.516(4) . ? C35 C36 1.533(4) . ? C41 C42 1.524(3) . ? C41 C46 1.531(3) . ? C42 C43 1.530(4) . ? C43 C44 1.515(4) . ? C44 C45 1.515(4) . ? C45 C46 1.520(4) . ? C51 C56 1.402(4) . ? C51 C52 1.408(4) . ? C52 C53 1.401(4) . ? C53 C54 1.371(4) . ? C54 C55 1.399(4) . ? C55 C56 1.375(4) . ? C61 C66 1.397(4) . ? C61 C62 1.402(4) . ? C62 C63 1.402(4) . ? C63 C64 1.372(4) . ? C64 C65 1.388(4) . ? C65 C66 1.376(4) . ? S O2 1.410(3) . ? S O3 1.412(2) . ? S O1 1.425(2) . ? S C1 1.792(4) . ? F1 C1 1.333(4) . ? F2 C1 1.317(5) . ? F3 C1 1.307(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 C51 As C61 97.19(11) . . ? C51 As P1 96.81(8) . . ? C61 As P1 99.66(8) . . ? C51 As O2 127.71(10) . 2_665 ? C61 As O2 87.11(9) . 2_665 ? P1 As O2 133.96(6) . 2_665 ? C11 P1 P4 111.16(8) . . ? C11 P1 P2 111.67(9) . . ? P4 P1 P2 86.11(3) . . ? C11 P1 As 106.35(8) . . ? P4 P1 As 129.11(3) . . ? P2 P1 As 110.59(3) . . ? C21 P2 P1 103.63(9) . . ? C21 P2 P3 105.13(8) . . ? P1 P2 P3 84.94(3) . . ? C31 P3 P4 100.84(9) . . ? C31 P3 P2 99.94(9) . . ? P4 P3 P2 84.86(3) . . ? C41 P4 P1 108.14(8) . . ? C41 P4 P3 105.60(9) . . ? P1 P4 P3 84.99(3) . . ? C52 N C62 128.4(2) . . ? C16 C11 C12 110.7(2) . . ? C16 C11 P1 113.19(18) . . ? C12 C11 P1 110.91(17) . . ? C13 C12 C11 110.2(2) . . ? C14 C13 C12 111.6(2) . . ? C15 C14 C13 111.9(2) . . ? C14 C15 C16 111.8(2) . . ? C11 C16 C15 110.5(2) . . ? C26 C21 C22 111.0(2) . . ? C26 C21 P2 109.20(18) . . ? C22 C21 P2 108.90(17) . . ? C23 C22 C21 111.0(2) . . ? C24 C23 C22 110.6(2) . . ? C25 C24 C23 111.1(2) . . ? C24 C25 C26 111.3(2) . . ? C21 C26 C25 110.8(2) . . ? C32 C31 C36 110.8(2) . . ? C32 C31 P3 109.34(18) . . ? C36 C31 P3 110.46(19) . . ? C31 C32 C33 111.9(3) . . ? C34 C33 C32 111.1(3) . . ? C35 C34 C33 111.3(3) . . ? C34 C35 C36 111.2(3) . . ? C31 C36 C35 112.0(2) . . ? C42 C41 C46 110.8(2) . . ? C42 C41 P4 109.37(17) . . ? C46 C41 P4 108.53(18) . . ? C41 C42 C43 111.6(2) . . ? C44 C43 C42 111.5(2) . . ? C43 C44 C45 111.2(2) . . ? C44 C45 C46 111.2(2) . . ? C45 C46 C41 110.5(2) . . ? C56 C51 C52 119.1(2) . . ? C56 C51 As 117.6(2) . . ? C52 C51 As 123.33(19) . . ? N C52 C53 118.0(2) . . ? N C52 C51 123.2(2) . . ? C53 C52 C51 118.8(2) . . ? C54 C53 C52 121.0(3) . . ? C53 C54 C55 120.6(3) . . ? C56 C55 C54 119.0(3) . . ? C55 C56 C51 121.5(3) . . ? C66 C61 C62 119.3(2) . . ? C66 C61 As 117.9(2) . . ? C62 C61 As 122.8(2) . . ? N C62 C61 123.9(2) . . ? N C62 C63 117.2(2) . . ? C61 C62 C63 118.9(2) . . ? C64 C63 C62 120.5(3) . . ? C63 C64 C65 121.0(3) . . ? C66 C65 C64 119.0(3) . . ? C65 C66 C61 121.3(3) . . ? O2 S O3 116.0(2) . . ? O2 S O1 114.13(15) . . ? O3 S O1 115.61(15) . . ? O2 S C1 102.9(2) . . ? O3 S C1 102.09(17) . . ? O1 S C1 103.42(16) . . ? F3 C1 F2 106.6(4) . . ? F3 C1 F1 107.8(3) . . ? F2 C1 F1 107.1(3) . . ? F3 C1 S 111.4(3) . . ? F2 C1 S 111.5(3) . . ? F1 C1 S 112.1(3) . . ? 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 C51 As P1 C11 -48.43(12) . . . . ? C61 As P1 C11 -146.95(12) . . . . ? O2 As P1 C11 117.70(12) 2_665 . . . ? C51 As P1 P4 87.90(9) . . . . ? C61 As P1 P4 -10.62(9) . . . . ? O2 As P1 P4 -105.97(10) 2_665 . . . ? C51 As P1 P2 -169.85(8) . . . . ? C61 As P1 P2 91.63(9) . . . . ? O2 As P1 P2 -3.72(10) 2_665 . . . ? C11 P1 P2 C21 -112.04(12) . . . . ? P4 P1 P2 C21 136.71(9) . . . . ? As P1 P2 C21 6.18(9) . . . . ? C11 P1 P2 P3 143.59(9) . . . . ? P4 P1 P2 P3 32.35(3) . . . . ? As P1 P2 P3 -98.19(3) . . . . ? C21 P2 P3 C31 125.10(12) . . . . ? P1 P2 P3 C31 -132.13(9) . . . . ? C21 P2 P3 P4 -134.77(9) . . . . ? P1 P2 P3 P4 -32.00(3) . . . . ? C11 P1 P4 C41 111.08(13) . . . . ? P2 P1 P4 C41 -137.17(9) . . . . ? As P1 P4 C41 -23.65(10) . . . . ? C11 P1 P4 P3 -144.13(9) . . . . ? P2 P1 P4 P3 -32.38(3) . . . . ? As P1 P4 P3 81.14(4) . . . . ? C31 P3 P4 C41 -121.39(12) . . . . ? P2 P3 P4 C41 139.45(8) . . . . ? C31 P3 P4 P1 131.16(9) . . . . ? P2 P3 P4 P1 32.00(3) . . . . ? P4 P1 C11 C16 72.61(19) . . . . ? P2 P1 C11 C16 -21.7(2) . . . . ? As P1 C11 C16 -142.46(16) . . . . ? P4 P1 C11 C12 -52.46(19) . . . . ? P2 P1 C11 C12 -146.80(16) . . . . ? As P1 C11 C12 92.48(17) . . . . ? C16 C11 C12 C13 57.6(3) . . . . ? P1 C11 C12 C13 -175.93(19) . . . . ? C11 C12 C13 C14 -55.7(3) . . . . ? C12 C13 C14 C15 54.2(3) . . . . ? C13 C14 C15 C16 -53.9(3) . . . . ? C12 C11 C16 C15 -57.4(3) . . . . ? P1 C11 C16 C15 177.44(19) . . . . ? C14 C15 C16 C11 55.5(3) . . . . ? P1 P2 C21 C26 -159.21(16) . . . . ? P3 P2 C21 C26 -70.84(18) . . . . ? P1 P2 C21 C22 79.41(18) . . . . ? P3 P2 C21 C22 167.78(16) . . . . ? C26 C21 C22 C23 56.1(3) . . . . ? P2 C21 C22 C23 176.38(19) . . . . ? C21 C22 C23 C24 -56.4(3) . . . . ? C22 C23 C24 C25 56.7(3) . . . . ? C23 C24 C25 C26 -56.4(4) . . . . ? C22 C21 C26 C25 -55.3(3) . . . . ? P2 C21 C26 C25 -175.4(2) . . . . ? C24 C25 C26 C21 55.7(3) . . . . ? P4 P3 C31 C32 -159.23(18) . . . . ? P2 P3 C31 C32 -72.6(2) . . . . ? P4 P3 C31 C36 78.57(18) . . . . ? P2 P3 C31 C36 165.18(17) . . . . ? C36 C31 C32 C33 -54.6(4) . . . . ? P3 C31 C32 C33 -176.6(2) . . . . ? C31 C32 C33 C34 55.3(4) . . . . ? C32 C33 C34 C35 -55.4(4) . . . . ? C33 C34 C35 C36 55.2(4) . . . . ? C32 C31 C36 C35 54.3(3) . . . . ? P3 C31 C36 C35 175.7(2) . . . . ? C34 C35 C36 C31 -55.0(3) . . . . ? P1 P4 C41 C42 -82.73(17) . . . . ? P3 P4 C41 C42 -172.50(15) . . . . ? P1 P4 C41 C46 156.26(15) . . . . ? P3 P4 C41 C46 66.48(18) . . . . ? C46 C41 C42 C43 -54.5(3) . . . . ? P4 C41 C42 C43 -174.14(18) . . . . ? C41 C42 C43 C44 54.0(3) . . . . ? C42 C43 C44 C45 -54.9(3) . . . . ? C43 C44 C45 C46 56.9(3) . . . . ? C44 C45 C46 C41 -57.5(3) . . . . ? C42 C41 C46 C45 56.1(3) . . . . ? P4 C41 C46 C45 176.25(19) . . . . ? C61 As C51 C56 -172.0(2) . . . . ? P1 As C51 C56 87.3(2) . . . . ? O2 As C51 C56 -80.1(2) 2_665 . . . ? C61 As C51 C52 10.5(2) . . . . ? P1 As C51 C52 -90.2(2) . . . . ? O2 As C51 C52 102.4(2) 2_665 . . . ? C62 N C52 C53 174.6(2) . . . . ? C62 N C52 C51 -4.0(4) . . . . ? C56 C51 C52 N 175.0(2) . . . . ? As C51 C52 N -7.5(4) . . . . ? C56 C51 C52 C53 -3.6(4) . . . . ? As C51 C52 C53 173.9(2) . . . . ? N C52 C53 C54 -176.6(3) . . . . ? C51 C52 C53 C54 2.0(4) . . . . ? C52 C53 C54 C55 0.5(5) . . . . ? C53 C54 C55 C56 -1.5(5) . . . . ? C54 C55 C56 C51 -0.1(4) . . . . ? C52 C51 C56 C55 2.6(4) . . . . ? As C51 C56 C55 -175.0(2) . . . . ? C51 As C61 C66 173.0(2) . . . . ? P1 As C61 C66 -88.8(2) . . . . ? O2 As C61 C66 45.4(2) 2_665 . . . ? C51 As C61 C62 -5.6(2) . . . . ? P1 As C61 C62 92.6(2) . . . . ? O2 As C61 C62 -133.3(2) 2_665 . . . ? C52 N C62 C61 9.6(4) . . . . ? C52 N C62 C63 -172.3(2) . . . . ? C66 C61 C62 N 178.6(2) . . . . ? As C61 C62 N -2.7(3) . . . . ? C66 C61 C62 C63 0.5(4) . . . . ? As C61 C62 C63 179.17(18) . . . . ? N C62 C63 C64 -177.5(2) . . . . ? C61 C62 C63 C64 0.8(4) . . . . ? C62 C63 C64 C65 -0.9(4) . . . . ? C63 C64 C65 C66 -0.4(4) . . . . ? C64 C65 C66 C61 1.7(4) . . . . ? C62 C61 C66 C65 -1.8(4) . . . . ? As C61 C66 C65 179.5(2) . . . . ? O2 S C1 F3 -63.9(4) . . . . ? O3 S C1 F3 175.5(3) . . . . ? O1 S C1 F3 55.1(4) . . . . ? O2 S C1 F2 177.1(3) . . . . ? O3 S C1 F2 56.6(3) . . . . ? O1 S C1 F2 -63.8(3) . . . . ? O2 S C1 F1 57.0(3) . . . . ? O3 S C1 F1 -63.6(3) . . . . ? O1 S C1 F1 176.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N H1N O1 0.88 2.06 2.920(3) 165.6 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.717 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.069