Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email MANUEL.BASALLOTE@UCA.ES _publ_contact_author_name 'Dr Manuel G. Basallote' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Departamento de Ciencia Materiales e Ingenieria Meralurgica y Quimica Inorganica Universidad de Cádiz Facultad de Ciencias Apartado 40 Puerto Real (Cádiz) 11510 SPAIN ; _publ_section_title ; Synthesis and structure of the incomplete cuboidal clusters [W3Se4H3(dmpe)3]+, [W3Se4H3-x(OH)x(dmpe)3]+ and [W3Se4(OH)3(dmpe)3]+, and the mechanism of the acid-assisted substitution of the coordinated hydrides. ; loop_ _publ_author_name 'Manuel G. Basallote' 'Francisco Estevan' 'Marta Feliz' 'M. Jesus Fernandez-Trujillo' ; D.A.Hoyos ; 'Rosa Llusar' 'Santiago Uriel' 'Cristian Vicent' #===END data_[W3Se4(OH/H2)(dmpe)3]BPh4 _database_code_depnum_ccdc_archive 'CCDC 225461' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H71 B O P6 Se4 W3' _chemical_formula_weight 1656.01 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' B B 0.0013 0.0007 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.097(2) _cell_length_b 11.3593(15) _cell_length_c 33.118(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.760(3) _cell_angle_gamma 90.00 _cell_volume 5613.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 8.927 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? #_Ratio of minimum to maximum apparent transmission 0.559763 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31377 _diffrn_reflns_av_R_equivalents 0.1038 _diffrn_reflns_av_sigmaI/netI 0.1190 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9897 _reflns_number_gt 6007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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^)+(0.0485P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9897 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 W1 W 0.84737(4) 0.92418(5) 0.178307(16) 0.02771(15) Uani 1 1 d . . . W2 W 0.94360(4) 0.98493(5) 0.114618(16) 0.02927(16) Uani 1 1 d . . . W3 W 0.79190(4) 1.11678(5) 0.127375(17) 0.02925(16) Uani 1 1 d . . . Se1 Se 0.78721(9) 0.90779(12) 0.10417(4) 0.0344(3) Uani 1 1 d . . . Se2 Se 1.01171(9) 0.93927(13) 0.18534(4) 0.0368(4) Uani 1 1 d . . . Se3 Se 0.93439(10) 1.20089(12) 0.11337(5) 0.0446(4) Uani 1 1 d . . . Se4 Se 0.80449(10) 1.11810(12) 0.20214(4) 0.0373(4) Uani 1 1 d . . . P1 P 0.8773(3) 0.8644(3) 0.25124(11) 0.0399(10) Uani 1 1 d . . . P2 P 0.6942(3) 0.8476(3) 0.18852(12) 0.0402(10) Uani 1 1 d . . . P3 P 1.0989(3) 1.0197(4) 0.10042(12) 0.0427(10) Uani 1 1 d . . . P4 P 0.9873(3) 0.7816(3) 0.09543(12) 0.0453(11) Uani 1 1 d . . . P5 P 0.7446(3) 1.3238(3) 0.13295(13) 0.0419(10) Uani 1 1 d . . . P6 P 0.7211(3) 1.1587(4) 0.05497(13) 0.0549(12) Uani 1 1 d . . . C1 C 0.9473(11) 0.7369(13) 0.2625(5) 0.069(5) Uani 1 1 d . . . H1A H 1.0042 0.7503 0.2537 0.104 Uiso 1 1 calc R . . H1B H 0.9189 0.6697 0.2484 0.104 Uiso 1 1 calc R . . H1C H 0.9563 0.7224 0.2914 0.104 Uiso 1 1 calc R . . C2 C 0.9277(12) 0.9713(13) 0.2897(4) 0.064(5) Uani 1 1 d . . . H2A H 0.8944 1.0436 0.2864 0.096 Uiso 1 1 calc R . . H2B H 0.9887 0.9859 0.2861 0.096 Uiso 1 1 calc R . . H2C H 0.9264 0.9402 0.3165 0.096 Uiso 1 1 calc R . . C3 C 0.7726(11) 0.8276(18) 0.2694(5) 0.076(6) Uani 1 1 d . . . H3A H 0.7847 0.7690 0.2908 0.092 Uiso 1 1 calc R . . H3B H 0.7500 0.8974 0.2812 0.092 Uiso 1 1 calc R . . C4 C 0.7082(15) 0.786(2) 0.2398(5) 0.115(9) Uani 1 1 d . . . H4A H 0.6513 0.7938 0.2497 0.138 Uiso 1 1 calc R . . H4B H 0.7189 0.7019 0.2373 0.138 Uiso 1 1 calc R . . C5 C 0.6023(10) 0.9434(14) 0.1875(7) 0.095(8) Uani 1 1 d . . . H5A H 0.6202 1.0113 0.2040 0.142 Uiso 1 1 calc R . . H5B H 0.5547 0.9035 0.1981 0.142 Uiso 1 1 calc R . . H5C H 0.5819 0.9676 0.1599 0.142 Uiso 1 1 calc R . . C6 C 0.6503(11) 0.7257(15) 0.1561(6) 0.079(6) Uani 1 1 d . . . H6A H 0.6970 0.6690 0.1548 0.119 Uiso 1 1 calc R . . H6B H 0.6290 0.7544 0.1291 0.119 Uiso 1 1 calc R . . H6C H 0.6019 0.6894 0.1671 0.119 Uiso 1 1 calc R . . C7 C 1.1743(9) 1.1024(14) 0.1359(5) 0.066(5) Uani 1 1 d . . . H7A H 1.1490 1.1784 0.1396 0.099 Uiso 1 1 calc R . . H7B H 1.2301 1.1118 0.1256 0.099 Uiso 1 1 calc R . . H7C H 1.1848 1.0616 0.1616 0.099 Uiso 1 1 calc R . . C8 C 1.1058(12) 1.0944(16) 0.0512(5) 0.077(6) Uani 1 1 d . . . H8A H 1.0666 1.0558 0.0297 0.115 Uiso 1 1 calc R . . H8B H 1.1663 1.0908 0.0456 0.115 Uiso 1 1 calc R . . H8C H 1.0880 1.1752 0.0529 0.115 Uiso 1 1 calc R . . C9 C 1.1530(10) 0.8776(14) 0.0956(5) 0.057(5) Uani 1 1 d . . . H9A H 1.2046 0.8883 0.0817 0.068 Uiso 1 1 calc R . . H9B H 1.1740 0.8460 0.1225 0.068 Uiso 1 1 calc R . . C10 C 1.0888(12) 0.7921(15) 0.0719(5) 0.066(5) Uani 1 1 d . . . H10A H 1.1168 0.7152 0.0718 0.079 Uiso 1 1 calc R . . H10B H 1.0737 0.8185 0.0439 0.079 Uiso 1 1 calc R . . C11 C 1.0135(13) 0.6684(13) 0.1336(5) 0.080(6) Uani 1 1 d . . . H11A H 1.0538 0.6994 0.1563 0.120 Uiso 1 1 calc R . . H11B H 1.0413 0.6031 0.1220 0.120 Uiso 1 1 calc R . . H11C H 0.9594 0.6424 0.1427 0.120 Uiso 1 1 calc R . . C12 C 0.9119(12) 0.6996(16) 0.0571(5) 0.093(7) Uani 1 1 d . . . H12A H 0.8917 0.7500 0.0343 0.139 Uiso 1 1 calc R . . H12B H 0.8612 0.6725 0.0688 0.139 Uiso 1 1 calc R . . H12C H 0.9431 0.6334 0.0480 0.139 Uiso 1 1 calc R . . C13 C 0.8224(10) 1.4277(14) 0.1586(6) 0.079(6) Uani 1 1 d . . . H13A H 0.8787 1.4204 0.1488 0.119 Uiso 1 1 calc R . . H13B H 0.8308 1.4125 0.1875 0.119 Uiso 1 1 calc R . . H13C H 0.7995 1.5059 0.1535 0.119 Uiso 1 1 calc R . . C14 C 0.6430(11) 1.3469(14) 0.1542(5) 0.069(5) Uani 1 1 d . . . H14A H 0.5971 1.2953 0.1411 0.104 Uiso 1 1 calc R . . H14B H 0.6240 1.4272 0.1499 0.104 Uiso 1 1 calc R . . H14C H 0.6539 1.3306 0.1830 0.104 Uiso 1 1 calc R . . C15 C 0.7179(11) 1.3833(15) 0.0799(5) 0.071(5) Uani 1 1 d . . . H15A H 0.6846 1.4562 0.0804 0.085 Uiso 1 1 calc R . . H15B H 0.7732 1.4005 0.0696 0.085 Uiso 1 1 calc R . . C16 C 0.6657(12) 1.3004(13) 0.0531(5) 0.062(5) Uani 1 1 d . . . H16A H 0.6575 1.3303 0.0254 0.074 Uiso 1 1 calc R . . H16B H 0.6070 1.2914 0.0613 0.074 Uiso 1 1 calc R . . C17 C 0.7902(13) 1.1761(17) 0.0155(5) 0.091(7) Uani 1 1 d . . . H17A H 0.8245 1.1057 0.0136 0.136 Uiso 1 1 calc R . . H17B H 0.8300 1.2415 0.0220 0.136 Uiso 1 1 calc R . . H17C H 0.7527 1.1902 -0.0102 0.136 Uiso 1 1 calc R . . C18 C 0.6319(14) 1.0635(16) 0.0316(6) 0.104(8) Uani 1 1 d . . . H18A H 0.5911 1.0491 0.0506 0.157 Uiso 1 1 calc R . . H18B H 0.6567 0.9902 0.0242 0.157 Uiso 1 1 calc R . . H18C H 0.6005 1.1007 0.0076 0.157 Uiso 1 1 calc R . . B1 B 0.6382(12) 0.9998(15) 0.3902(5) 0.045(5) Uani 1 1 d . . . C50 C 0.6359(11) 1.0647(14) 0.3442(5) 0.047(4) Uani 1 1 d . . . C51 C 0.5547(12) 1.0667(16) 0.3159(5) 0.067(5) Uani 1 1 d . . . H51 H 0.5052 1.0252 0.3219 0.080 Uiso 1 1 calc R . . C52 C 0.5481(16) 1.130(2) 0.2792(5) 0.099(8) Uani 1 1 d . . . H52 H 0.4954 1.1302 0.2605 0.119 Uiso 1 1 calc R . . C53 C 0.623(2) 1.194(3) 0.2715(7) 0.134(12) Uani 1 1 d . . . H53 H 0.6212 1.2350 0.2472 0.160 Uiso 1 1 calc R . . C54 C 0.6948(16) 1.194(2) 0.2991(8) 0.104(8) Uani 1 1 d . . . H54 H 0.7425 1.2416 0.2942 0.125 Uiso 1 1 calc R . . C55 C 0.7046(13) 1.1315(15) 0.3338(5) 0.063(5) Uani 1 1 d . . . H55 H 0.7591 1.1334 0.3512 0.076 Uiso 1 1 calc R . . C56 C 0.6091(9) 0.8615(13) 0.3851(4) 0.041(4) Uani 1 1 d . . . C57 C 0.6086(11) 0.7904(14) 0.4204(5) 0.058(5) Uani 1 1 d . . . H57 H 0.6193 0.8281 0.4456 0.070 Uiso 1 1 calc R . . C58 C 0.5944(11) 0.6755(18) 0.4208(6) 0.075(6) Uani 1 1 d . . . H58 H 0.5963 0.6364 0.4456 0.090 Uiso 1 1 calc R . . C59 C 0.5770(14) 0.6145(17) 0.3854(7) 0.089(7) Uani 1 1 d . . . H59 H 0.5668 0.5338 0.3854 0.107 Uiso 1 1 calc R . . C60 C 0.5748(11) 0.6744(18) 0.3497(6) 0.081(7) Uani 1 1 d . . . H60 H 0.5618 0.6339 0.3251 0.097 Uiso 1 1 calc R . . C61 C 0.5918(10) 0.7969(15) 0.3490(5) 0.056(5) Uani 1 1 d . . . H61 H 0.5915 0.8348 0.3241 0.067 Uiso 1 1 calc R . . C62 C 0.5738(9) 1.0849(13) 0.4141(4) 0.038(4) Uani 1 1 d . . . C63 C 0.5846(11) 1.2058(15) 0.4129(5) 0.063(5) Uani 1 1 d . . . H63 H 0.6243 1.2392 0.3973 0.075 Uiso 1 1 calc R . . C64 C 0.5338(12) 1.2777(14) 0.4360(4) 0.058(5) Uani 1 1 d . . . H64 H 0.5433 1.3586 0.4360 0.070 Uiso 1 1 calc R . . C65 C 0.4726(11) 1.2354(18) 0.4580(5) 0.061(5) Uani 1 1 d . . . H65 H 0.4406 1.2854 0.4728 0.073 Uiso 1 1 calc R . . C66 C 0.4594(11) 1.1169(17) 0.4579(5) 0.059(5) Uani 1 1 d . . . H66 H 0.4168 1.0847 0.4722 0.071 Uiso 1 1 calc R . . C67 C 0.5093(11) 1.0444(15) 0.4365(5) 0.059(5) Uani 1 1 d . . . H67 H 0.4991 0.9637 0.4371 0.071 Uiso 1 1 calc R . . C68 C 0.7410(10) 0.9957(12) 0.4150(5) 0.046(4) Uani 1 1 d . . . C69 C 0.7648(10) 1.0286(13) 0.4537(4) 0.049(4) Uani 1 1 d . . . H69 H 0.7226 1.0674 0.4666 0.059 Uiso 1 1 calc R . . C70 C 0.8493(10) 1.0081(15) 0.4761(5) 0.058(5) Uani 1 1 d . . . H70 H 0.8617 1.0326 0.5032 0.070 Uiso 1 1 calc R . . C71 C 0.9139(12) 0.9524(14) 0.4587(5) 0.059(5) Uani 1 1 d . . . H71 H 0.9697 0.9357 0.4737 0.071 Uiso 1 1 calc R . . C72 C 0.8936(11) 0.9218(14) 0.4179(6) 0.063(5) Uani 1 1 d . . . H72 H 0.9364 0.8855 0.4047 0.076 Uiso 1 1 calc R . . C73 C 0.8092(9) 0.9454(12) 0.3969(4) 0.047(4) Uani 1 1 d . . . H73 H 0.7974 0.9267 0.3693 0.056 Uiso 1 1 calc R . . O1 O 0.8514(9) 0.7370(12) 0.1748(4) 0.069(10) Uiso 0.33 1 d PR . . H1 H 0.8824 0.7173 0.1577 0.104 Uiso 0.33 1 calc PR . . O2 O 0.934(2) 0.968(3) 0.0510(10) 0.084(12) Uiso 0.33 1 d P . . H2 H 0.9759 1.0033 0.0432 0.125 Uiso 0.33 1 calc PR . . O3 O 0.660(3) 1.094(4) 0.1170(13) 0.110(15) Uiso 0.33 1 d P . . H3 H 0.6491 1.0249 0.1118 0.165 Uiso 0.33 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0261(3) 0.0279(3) 0.0291(3) 0.0024(2) 0.0041(2) 0.0009(3) W2 0.0309(3) 0.0258(3) 0.0328(3) -0.0001(3) 0.0102(3) 0.0041(3) W3 0.0259(3) 0.0274(3) 0.0351(3) 0.0049(3) 0.0070(2) 0.0040(3) Se1 0.0380(9) 0.0331(8) 0.0311(8) 0.0018(6) 0.0018(7) -0.0029(7) Se2 0.0281(8) 0.0461(9) 0.0356(8) -0.0046(7) 0.0028(7) 0.0054(7) Se3 0.0352(9) 0.0260(8) 0.0767(11) 0.0020(8) 0.0218(8) 0.0003(7) Se4 0.0428(9) 0.0329(8) 0.0378(8) -0.0032(7) 0.0113(7) 0.0023(7) P1 0.039(2) 0.045(2) 0.035(2) 0.0056(18) 0.0022(19) 0.002(2) P2 0.032(2) 0.040(2) 0.048(2) 0.0102(19) 0.0058(19) -0.0022(19) P3 0.033(2) 0.049(3) 0.050(2) -0.003(2) 0.021(2) 0.003(2) P4 0.062(3) 0.036(2) 0.043(2) -0.0091(18) 0.024(2) -0.001(2) P5 0.032(2) 0.031(2) 0.066(3) 0.0055(19) 0.015(2) 0.0037(19) P6 0.060(3) 0.053(3) 0.051(3) 0.008(2) 0.006(2) 0.017(2) C1 0.085(14) 0.056(11) 0.061(11) 0.023(9) -0.008(10) 0.033(10) C2 0.100(15) 0.052(11) 0.035(9) 0.011(8) -0.008(9) 0.003(10) C3 0.057(12) 0.124(18) 0.053(11) 0.035(11) 0.025(10) -0.008(12) C4 0.109(19) 0.19(3) 0.049(12) 0.042(14) 0.019(13) -0.057(18) C5 0.041(11) 0.047(12) 0.20(2) 0.019(13) 0.044(14) 0.002(9) C6 0.059(12) 0.067(13) 0.110(15) 0.019(11) 0.005(11) -0.034(10) C7 0.031(9) 0.075(13) 0.099(14) -0.002(11) 0.034(10) -0.008(9) C8 0.078(14) 0.092(15) 0.073(12) 0.008(11) 0.054(11) -0.001(12) C9 0.028(9) 0.071(12) 0.077(12) 0.019(10) 0.024(9) 0.029(9) C10 0.091(14) 0.062(12) 0.054(11) -0.015(9) 0.042(10) 0.023(11) C11 0.129(18) 0.031(10) 0.092(14) 0.008(9) 0.057(13) 0.005(11) C12 0.094(16) 0.089(15) 0.098(15) -0.063(13) 0.027(13) -0.020(13) C13 0.048(11) 0.045(11) 0.147(19) 0.006(11) 0.022(12) 0.011(9) C14 0.066(12) 0.049(11) 0.101(14) 0.010(10) 0.038(11) 0.014(10) C15 0.054(12) 0.056(12) 0.108(15) 0.032(11) 0.029(11) 0.010(10) C16 0.078(13) 0.046(11) 0.057(11) 0.009(9) -0.005(10) 0.024(10) C17 0.114(17) 0.114(17) 0.051(11) 0.025(11) 0.039(11) 0.052(14) C18 0.13(2) 0.077(15) 0.081(14) 0.008(12) -0.049(14) 0.022(14) B1 0.048(12) 0.038(11) 0.047(11) -0.017(8) 0.004(9) -0.005(9) C50 0.040(10) 0.046(10) 0.055(10) -0.012(8) 0.006(9) -0.004(8) C51 0.066(13) 0.079(13) 0.064(12) 0.015(10) 0.038(11) 0.004(11) C52 0.101(18) 0.15(2) 0.041(12) 0.006(13) 0.004(12) 0.077(17) C53 0.17(3) 0.18(3) 0.072(17) 0.059(18) 0.092(19) 0.04(2) C54 0.10(2) 0.105(19) 0.11(2) 0.012(17) 0.008(16) -0.013(16) C55 0.080(14) 0.071(13) 0.037(10) 0.006(9) 0.006(9) -0.008(11) C56 0.035(9) 0.044(9) 0.042(9) -0.014(8) 0.001(7) 0.014(7) C57 0.056(11) 0.029(10) 0.088(13) 0.022(9) 0.004(10) 0.020(9) C58 0.052(12) 0.094(17) 0.081(14) -0.020(13) 0.016(11) -0.026(12) C59 0.104(18) 0.054(13) 0.102(17) 0.026(13) -0.006(15) 0.003(12) C60 0.054(12) 0.080(15) 0.100(17) -0.054(13) -0.018(12) 0.003(11) C61 0.040(10) 0.060(12) 0.065(12) 0.003(10) 0.002(9) 0.007(9) C62 0.035(9) 0.052(11) 0.026(8) -0.004(7) 0.000(7) 0.012(8) C63 0.066(13) 0.063(13) 0.065(12) 0.013(10) 0.030(10) 0.015(10) C64 0.094(15) 0.037(10) 0.036(9) -0.020(8) -0.015(10) 0.020(10) C65 0.049(11) 0.102(17) 0.035(9) -0.009(10) 0.012(9) 0.001(11) C66 0.043(10) 0.084(14) 0.055(11) -0.018(10) 0.028(9) -0.010(10) C67 0.051(11) 0.055(11) 0.072(12) -0.004(9) 0.008(10) 0.010(9) C68 0.042(10) 0.036(9) 0.060(11) 0.003(8) 0.014(9) -0.008(8) C69 0.036(10) 0.059(11) 0.047(10) 0.002(8) -0.008(8) 0.011(8) C70 0.037(10) 0.076(13) 0.061(11) 0.010(10) 0.002(9) 0.007(9) C71 0.057(12) 0.053(11) 0.067(12) 0.025(9) 0.007(10) 0.003(9) C72 0.050(11) 0.041(10) 0.105(16) 0.023(10) 0.033(11) 0.015(9) C73 0.034(9) 0.060(11) 0.047(9) 0.000(8) 0.012(8) 0.005(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 W1 O1 2.131(14) . ? W1 Se4 2.4597(15) . ? W1 Se2 2.4622(15) . ? W1 P1 2.484(4) . ? W1 Se1 2.4916(14) . ? W1 P2 2.541(4) . ? W1 W3 2.8112(8) . ? W1 W2 2.8229(8) . ? W2 O2 2.10(3) . ? W2 Se3 2.4571(15) . ? W2 Se2 2.4654(15) . ? W2 P3 2.491(4) . ? W2 Se1 2.4925(15) . ? W2 P4 2.510(4) . ? W2 W3 2.8215(8) . ? W3 O3 1.98(4) . ? W3 Se4 2.4544(15) . ? W3 Se3 2.4615(16) . ? W3 P5 2.473(4) . ? W3 Se1 2.4928(15) . ? W3 P6 2.517(4) . ? P1 C1 1.799(14) . ? P1 C3 1.822(16) . ? P1 C2 1.838(15) . ? P2 C5 1.760(16) . ? P2 C6 1.815(17) . ? P2 C4 1.821(17) . ? P3 C7 1.775(15) . ? P3 C9 1.828(15) . ? P3 C8 1.855(15) . ? P4 C11 1.804(15) . ? P4 C12 1.826(15) . ? P4 C10 1.826(16) . ? P5 C13 1.786(16) . ? P5 C14 1.801(16) . ? P5 C15 1.867(17) . ? P6 C17 1.803(17) . ? P6 C18 1.806(19) . ? P6 C16 1.812(15) . ? C3 C4 1.36(2) . ? C9 C10 1.50(2) . ? C15 C16 1.44(2) . ? B1 C56 1.63(2) . ? B1 C68 1.64(2) . ? B1 C62 1.66(2) . ? B1 C50 1.69(2) . ? C50 C55 1.37(2) . ? C50 C51 1.42(2) . ? C51 C52 1.41(2) . ? C52 C53 1.39(3) . ? C53 C54 1.31(3) . ? C54 C55 1.34(3) . ? C56 C61 1.392(19) . ? C56 C57 1.42(2) . ? C57 C58 1.32(2) . ? C58 C59 1.35(2) . ? C59 C60 1.36(2) . ? C60 C61 1.42(2) . ? C62 C63 1.38(2) . ? C62 C67 1.39(2) . ? C63 C64 1.42(2) . ? C64 C65 1.35(2) . ? C65 C66 1.36(2) . ? C66 C67 1.38(2) . ? C68 C69 1.331(19) . ? C68 C73 1.390(19) . ? C69 C70 1.394(18) . ? C70 C71 1.36(2) . ? C71 C72 1.38(2) . ? C72 C73 1.382(19) . ? 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 O1 W1 Se4 157.2(4) . . ? O1 W1 Se2 92.2(4) . . ? Se4 W1 Se2 102.59(5) . . ? O1 W1 P1 77.1(4) . . ? Se4 W1 P1 87.17(10) . . ? Se2 W1 P1 84.03(10) . . ? O1 W1 Se1 83.2(4) . . ? Se4 W1 Se1 107.99(5) . . ? Se2 W1 Se1 108.01(5) . . ? P1 W1 Se1 157.35(10) . . ? O1 W1 P2 72.5(4) . . ? Se4 W1 P2 88.55(10) . . ? Se2 W1 P2 159.30(9) . . ? P1 W1 P2 79.10(13) . . ? Se1 W1 P2 84.44(9) . . ? O1 W1 W3 138.8(4) . . ? Se4 W1 W3 55.02(4) . . ? Se2 W1 W3 101.91(4) . . ? P1 W1 W3 142.18(10) . . ? Se1 W1 W3 55.69(4) . . ? P2 W1 W3 98.77(9) . . ? O1 W1 W2 100.4(4) . . ? Se4 W1 W2 102.20(4) . . ? Se2 W1 W2 55.10(4) . . ? P1 W1 W2 139.09(10) . . ? Se1 W1 W2 55.52(4) . . ? P2 W1 W2 139.95(9) . . ? W3 W1 W2 60.11(2) . . ? O2 W2 Se3 94.6(10) . . ? O2 W2 Se2 152.7(10) . . ? Se3 W2 Se2 103.90(5) . . ? O2 W2 P3 75.3(10) . . ? Se3 W2 P3 83.74(10) . . ? Se2 W2 P3 86.81(10) . . ? O2 W2 Se1 84.9(10) . . ? Se3 W2 Se1 107.38(5) . . ? Se2 W2 Se1 107.88(5) . . ? P3 W2 Se1 158.13(10) . . ? O2 W2 P4 68.9(10) . . ? Se3 W2 P4 158.56(10) . . ? Se2 W2 P4 87.67(10) . . ? P3 W2 P4 78.89(14) . . ? Se1 W2 P4 85.48(11) . . ? O2 W2 W3 105.5(10) . . ? Se3 W2 W3 55.07(4) . . ? Se2 W2 W3 101.54(4) . . ? P3 W2 W3 138.80(10) . . ? Se1 W2 W3 55.54(4) . . ? P4 W2 W3 140.97(10) . . ? O2 W2 W1 139.8(10) . . ? Se3 W2 W1 102.85(4) . . ? Se2 W2 W1 55.00(4) . . ? P3 W2 W1 141.80(10) . . ? Se1 W2 W1 55.49(3) . . ? P4 W2 W1 98.58(9) . . ? W3 W2 W1 59.74(2) . . ? O3 W3 Se4 95.6(12) . . ? O3 W3 Se3 154.1(12) . . ? Se4 W3 Se3 104.60(6) . . ? O3 W3 P5 80.9(13) . . ? Se4 W3 P5 84.13(10) . . ? Se3 W3 P5 85.16(10) . . ? O3 W3 Se1 81.0(12) . . ? Se4 W3 Se1 108.12(5) . . ? Se3 W3 Se1 107.23(5) . . ? P5 W3 Se1 159.01(10) . . ? O3 W3 P6 65.8(12) . . ? Se4 W3 P6 156.39(11) . . ? Se3 W3 P6 90.20(12) . . ? P5 W3 P6 78.81(14) . . ? Se1 W3 P6 84.17(11) . . ? O3 W3 W1 101.7(12) . . ? Se4 W3 W1 55.19(4) . . ? Se3 W3 W1 103.07(4) . . ? P5 W3 W1 139.32(10) . . ? Se1 W3 W1 55.65(3) . . ? P6 W3 W1 139.73(11) . . ? O3 W3 W2 136.1(12) . . ? Se4 W3 W2 102.38(4) . . ? Se3 W3 W2 54.92(4) . . ? P5 W3 W2 140.02(9) . . ? Se1 W3 W2 55.52(4) . . ? P6 W3 W2 101.19(11) . . ? W1 W3 W2 60.15(2) . . ? W1 Se1 W2 69.00(4) . . ? W1 Se1 W3 68.66(4) . . ? W2 Se1 W3 68.94(4) . . ? W1 Se2 W2 69.90(4) . . ? W2 Se3 W3 70.01(4) . . ? W3 Se4 W1 69.79(4) . . ? C1 P1 C3 105.0(9) . . ? C1 P1 C2 102.7(7) . . ? C3 P1 C2 102.3(9) . . ? C1 P1 W1 115.8(6) . . ? C3 P1 W1 110.2(6) . . ? C2 P1 W1 119.2(5) . . ? C5 P2 C6 104.2(9) . . ? C5 P2 C4 103.6(11) . . ? C6 P2 C4 103.8(10) . . ? C5 P2 W1 121.1(6) . . ? C6 P2 W1 116.1(6) . . ? C4 P2 W1 106.1(7) . . ? C7 P3 C9 105.9(8) . . ? C7 P3 C8 102.9(8) . . ? C9 P3 C8 103.9(8) . . ? C7 P3 W2 119.1(5) . . ? C9 P3 W2 108.8(5) . . ? C8 P3 W2 114.8(6) . . ? C11 P4 C12 99.9(9) . . ? C11 P4 C10 103.6(8) . . ? C12 P4 C10 102.2(8) . . ? C11 P4 W2 121.1(6) . . ? C12 P4 W2 119.0(6) . . ? C10 P4 W2 108.5(5) . . ? C13 P5 C14 104.8(8) . . ? C13 P5 C15 103.9(9) . . ? C14 P5 C15 103.9(8) . . ? C13 P5 W3 119.1(5) . . ? C14 P5 W3 116.1(5) . . ? C15 P5 W3 107.3(6) . . ? C17 P6 C18 103.3(10) . . ? C17 P6 C16 101.1(8) . . ? C18 P6 C16 101.9(9) . . ? C17 P6 W3 120.2(6) . . ? C18 P6 W3 118.4(6) . . ? C16 P6 W3 109.1(5) . . ? C4 C3 P1 113.9(14) . . ? C3 C4 P2 120.4(15) . . ? C10 C9 P3 110.8(10) . . ? C9 C10 P4 109.7(10) . . ? C16 C15 P5 111.2(12) . . ? C15 C16 P6 110.7(12) . . ? C56 B1 C68 104.1(12) . . ? C56 B1 C62 116.2(13) . . ? C68 B1 C62 110.8(12) . . ? C56 B1 C50 111.0(12) . . ? C68 B1 C50 110.6(13) . . ? C62 B1 C50 104.1(12) . . ? C55 C50 C51 115.8(15) . . ? C55 C50 B1 123.8(14) . . ? C51 C50 B1 119.8(14) . . ? C52 C51 C50 121.1(18) . . ? C53 C52 C51 118(2) . . ? C54 C53 C52 119(2) . . ? C53 C54 C55 124(2) . . ? C54 C55 C50 121.4(19) . . ? C61 C56 C57 112.5(15) . . ? C61 C56 B1 127.4(14) . . ? C57 C56 B1 119.8(13) . . ? C58 C57 C56 126.1(18) . . ? C57 C58 C59 120(2) . . ? C58 C59 C60 118.2(19) . . ? C59 C60 C61 121.6(18) . . ? C56 C61 C60 121.1(17) . . ? C63 C62 C67 116.0(14) . . ? C63 C62 B1 119.0(14) . . ? C67 C62 B1 124.9(14) . . ? C62 C63 C64 118.7(16) . . ? C65 C64 C63 123.8(17) . . ? C64 C65 C66 117.5(17) . . ? C65 C66 C67 120.1(17) . . ? C66 C67 C62 123.8(16) . . ? C69 C68 C73 114.9(14) . . ? C69 C68 B1 124.8(14) . . ? C73 C68 B1 120.1(13) . . ? C68 C69 C70 123.8(16) . . ? C71 C70 C69 120.6(16) . . ? C70 C71 C72 117.6(16) . . ? C73 C72 C71 119.5(16) . . ? C72 C73 C68 123.4(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.079 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.234 #===END data_[W3Se4(OH)3(dmpe)3]BPh4 _database_code_depnum_ccdc_archive 'CCDC 225462' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H71 B O3 P6 Se4 W3' _chemical_formula_weight 1688.01 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1941(14) _cell_length_b 15.1541(18) _cell_length_c 17.022(2) _cell_angle_alpha 82.358(2) _cell_angle_beta 82.591(3) _cell_angle_gamma 88.462(2) _cell_volume 2837.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 8.833 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? #_Ratio of minimum to maximum apparent transmission 0.563898 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15950 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9996 _reflns_number_gt 6700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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^)+(0.0447P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9996 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _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 W1 W 0.15908(3) 0.83735(2) 0.14909(2) 0.02937(11) Uani 1 1 d . . . W2 W -0.05561(4) 0.78257(3) 0.24573(2) 0.03556(12) Uani 1 1 d . . . W3 W 0.07103(4) 0.93086(3) 0.27722(2) 0.03411(12) Uani 1 1 d . . . Se1 Se 0.14763(10) 0.77378(7) 0.29309(6) 0.0441(3) Uani 1 1 d . . . Se2 Se -0.02810(9) 0.80874(7) 0.09830(6) 0.0409(3) Uani 1 1 d . . . Se3 Se -0.14660(9) 0.92738(7) 0.26817(6) 0.0423(3) Uani 1 1 d . . . Se4 Se 0.13575(9) 1.00013(6) 0.14083(6) 0.0372(2) Uani 1 1 d . . . P1 P 0.2404(2) 0.87337(18) 0.00488(16) 0.0425(7) Uani 1 1 d . . . P2 P 0.2344(3) 0.6842(2) 0.1154(2) 0.0631(9) Uani 1 1 d . . . P3 P -0.2657(3) 0.7438(2) 0.2274(2) 0.0560(8) Uani 1 1 d . . . P4 P -0.1421(3) 0.7256(3) 0.3901(2) 0.0707(10) Uani 1 1 d . . . P5 P 0.0267(3) 1.08862(19) 0.30459(19) 0.0514(8) Uani 1 1 d . . . P6 P 0.2766(3) 0.9784(2) 0.30707(19) 0.0564(8) Uani 1 1 d . . . O1 O 0.3390(5) 0.8364(4) 0.1528(3) 0.0318(15) Uani 1 1 d . . . H1 H 0.3534 0.8600 0.1912 0.048 Uiso 1 1 calc R . . O2 O -0.0435(6) 0.6483(4) 0.2555(4) 0.052(2) Uani 1 1 d . . . H2 H 0.0198 0.6337 0.2304 0.078 Uiso 1 1 calc R . . O3 O 0.0567(6) 0.9193(4) 0.3991(3) 0.0469(18) Uani 1 1 d . . . H3 H 0.0177 0.8748 0.4185 0.070 Uiso 1 1 calc R . . C1 C 0.1286(14) 0.6030(9) 0.0985(10) 0.129(8) Uani 1 1 d . . . H6A H 0.0724 0.5890 0.1459 0.194 Uiso 1 1 calc R . . H6B H 0.1712 0.5500 0.0856 0.194 Uiso 1 1 calc R . . H6C H 0.0857 0.6270 0.0550 0.194 Uiso 1 1 calc R . . C2 C 0.3275(16) 0.6253(10) 0.1857(8) 0.133(7) Uani 1 1 d . . . H5A H 0.2809 0.6132 0.2373 0.199 Uiso 1 1 calc R . . H5B H 0.3953 0.6614 0.1894 0.199 Uiso 1 1 calc R . . H5C H 0.3556 0.5702 0.1674 0.199 Uiso 1 1 calc R . . C3 C 0.3290(12) 0.7029(8) 0.0226(7) 0.079(4) Uani 1 1 d . . . H4A H 0.4065 0.7237 0.0319 0.094 Uiso 1 1 calc R . . H4B H 0.3424 0.6468 0.0011 0.094 Uiso 1 1 calc R . . C4 C 0.2769(12) 0.7710(8) -0.0398(7) 0.069(4) Uani 1 1 d . . . H3A H 0.2050 0.7475 -0.0554 0.083 Uiso 1 1 calc R . . H3B H 0.3354 0.7832 -0.0871 0.083 Uiso 1 1 calc R . . C5 C 0.3819(11) 0.9320(9) -0.0119(8) 0.087(5) Uani 1 1 d . . . H2A H 0.3717 0.9870 0.0104 0.131 Uiso 1 1 calc R . . H2B H 0.4075 0.9441 -0.0683 0.131 Uiso 1 1 calc R . . H2C H 0.4417 0.8959 0.0132 0.131 Uiso 1 1 calc R . . C6 C 0.1519(12) 0.9385(8) -0.0643(6) 0.076(4) Uani 1 1 d . . . H1A H 0.0739 0.9123 -0.0605 0.114 Uiso 1 1 calc R . . H1B H 0.1921 0.9395 -0.1178 0.114 Uiso 1 1 calc R . . H1C H 0.1430 0.9983 -0.0513 0.114 Uiso 1 1 calc R . . C7 C -0.3531(10) 0.8239(8) 0.1699(8) 0.081(4) Uani 1 1 d . . . H7A H -0.3510 0.8806 0.1890 0.121 Uiso 1 1 calc R . . H7B H -0.4350 0.8043 0.1756 0.121 Uiso 1 1 calc R . . H7C H -0.3199 0.8294 0.1146 0.121 Uiso 1 1 calc R . . C8 C -0.2753(11) 0.6399(7) 0.1875(8) 0.078(4) Uani 1 1 d . . . H8A H -0.2303 0.5947 0.2164 0.116 Uiso 1 1 calc R . . H8B H -0.2425 0.6474 0.1321 0.116 Uiso 1 1 calc R . . H8C H -0.3580 0.6226 0.1927 0.116 Uiso 1 1 calc R . . C9 C -0.3539(11) 0.7212(9) 0.3285(8) 0.079(4) Uani 1 1 d . . . H9A H -0.3788 0.7772 0.3476 0.094 Uiso 1 1 calc R . . H9B H -0.4258 0.6884 0.3250 0.094 Uiso 1 1 calc R . . C10 C -0.2815(13) 0.6691(10) 0.3859(8) 0.086(5) Uani 1 1 d . . . H10A H -0.2635 0.6107 0.3697 0.103 Uiso 1 1 calc R . . H10B H -0.3277 0.6611 0.4386 0.103 Uiso 1 1 calc R . . C11 C -0.0542(15) 0.6427(11) 0.4424(9) 0.148(8) Uani 1 1 d . . . H11A H 0.0221 0.6672 0.4477 0.222 Uiso 1 1 calc R . . H11B H -0.0414 0.5926 0.4132 0.222 Uiso 1 1 calc R . . H11C H -0.0962 0.6238 0.4946 0.222 Uiso 1 1 calc R . . C12 C -0.1865(13) 0.8013(11) 0.4618(8) 0.114(6) Uani 1 1 d . . . H12A H -0.1183 0.8356 0.4680 0.170 Uiso 1 1 calc R . . H12B H -0.2162 0.7682 0.5123 0.170 Uiso 1 1 calc R . . H12C H -0.2487 0.8406 0.4434 0.170 Uiso 1 1 calc R . . C13 C 0.3973(10) 1.0091(9) 0.2275(8) 0.080(4) Uani 1 1 d . . . H13A H 0.4162 0.9599 0.1978 0.120 Uiso 1 1 calc R . . H13B H 0.4672 1.0243 0.2499 0.120 Uiso 1 1 calc R . . H13C H 0.3724 1.0594 0.1926 0.120 Uiso 1 1 calc R . . C14 C 0.3500(14) 0.8987(10) 0.3760(9) 0.116(6) Uani 1 1 d . . . H14A H 0.3670 0.8446 0.3530 0.173 Uiso 1 1 calc R . . H14B H 0.2977 0.8863 0.4254 0.173 Uiso 1 1 calc R . . H14C H 0.4239 0.9233 0.3860 0.173 Uiso 1 1 calc R . . C15 C 0.2507(11) 1.0755(9) 0.3580(8) 0.077(4) Uani 1 1 d . . . H15A H 0.2148 1.0579 0.4126 0.093 Uiso 1 1 calc R . . H15B H 0.3268 1.1040 0.3594 0.093 Uiso 1 1 calc R . . C16 C 0.1688(11) 1.1395(8) 0.3160(8) 0.074(4) Uani 1 1 d . . . H16A H 0.2092 1.1621 0.2636 0.089 Uiso 1 1 calc R . . H16B H 0.1518 1.1896 0.3459 0.089 Uiso 1 1 calc R . . C17 C -0.0670(11) 1.0984(9) 0.4005(7) 0.076(4) Uani 1 1 d . . . H17A H -0.0360 1.0592 0.4424 0.114 Uiso 1 1 calc R . . H17B H -0.1484 1.0825 0.3971 0.114 Uiso 1 1 calc R . . H17C H -0.0653 1.1587 0.4121 0.114 Uiso 1 1 calc R . . C18 C -0.0431(11) 1.1659(7) 0.2346(7) 0.073(4) Uani 1 1 d . . . H18A H -0.1187 1.1425 0.2262 0.109 Uiso 1 1 calc R . . H18B H 0.0087 1.1749 0.1847 0.109 Uiso 1 1 calc R . . H18C H -0.0568 1.2217 0.2554 0.109 Uiso 1 1 calc R . . B1 B 0.5342(14) 1.3504(9) 0.2702(9) 0.064(4) Uani 1 1 d . . . C50 C 0.5373(9) 1.2526(6) 0.3245(7) 0.048(3) Uani 1 1 d . . . C51 C 0.6039(9) 1.1816(7) 0.2958(7) 0.053(3) Uani 1 1 d . . . H51 H 0.6393 1.1890 0.2428 0.064 Uiso 1 1 calc R . . C52 C 0.6195(10) 1.1020(7) 0.3416(8) 0.059(3) Uani 1 1 d . . . H52 H 0.6621 1.0560 0.3191 0.071 Uiso 1 1 calc R . . C53 C 0.5732(11) 1.0901(8) 0.4190(8) 0.063(3) Uani 1 1 d . . . H53 H 0.5874 1.0372 0.4511 0.075 Uiso 1 1 calc R . . C54 C 0.5049(10) 1.1566(8) 0.4502(7) 0.061(3) Uani 1 1 d . . . H54 H 0.4685 1.1476 0.5028 0.073 Uiso 1 1 calc R . . C55 C 0.4901(10) 1.2363(7) 0.4039(6) 0.052(3) Uani 1 1 d . . . H55 H 0.4464 1.2814 0.4270 0.063 Uiso 1 1 calc R . . C56 C 0.6770(13) 1.3816(7) 0.2529(10) 0.078(4) Uani 1 1 d . . . C57 C 0.7393(15) 1.3840(11) 0.3205(12) 0.116(6) Uani 1 1 d . . . H57 H 0.6950 1.3743 0.3709 0.139 Uiso 1 1 calc R . . C58 C 0.8653(16) 1.4006(10) 0.3158(13) 0.118(7) Uani 1 1 d . . . H58 H 0.9075 1.3977 0.3597 0.141 Uiso 1 1 calc R . . C59 C 0.917(2) 1.4218(13) 0.2360(19) 0.155(12) Uani 1 1 d . . . H59 H 0.9969 1.4397 0.2285 0.185 Uiso 1 1 calc R . . C60 C 0.866(2) 1.4194(12) 0.1687(15) 0.135(11) Uani 1 1 d . . . H60 H 0.9089 1.4302 0.1180 0.162 Uiso 1 1 calc R . . C61 C 0.7445(15) 1.3999(8) 0.1804(11) 0.106(6) Uani 1 1 d . . . H61 H 0.7060 1.3993 0.1353 0.128 Uiso 1 1 calc R . . C62 C 0.4761(12) 1.3410(9) 0.1894(8) 0.070(4) Uani 1 1 d . . . C63 C 0.4706(17) 1.4166(10) 0.1307(9) 0.112(6) Uani 1 1 d . . . H63 H 0.5091 1.4692 0.1344 0.134 Uiso 1 1 calc R . . C64 C 0.402(2) 1.4087(16) 0.0644(11) 0.144(10) Uani 1 1 d . . . H64 H 0.3985 1.4576 0.0254 0.173 Uiso 1 1 calc R . . C65 C 0.343(2) 1.330(2) 0.0569(14) 0.156(10) Uani 1 1 d . . . H65 H 0.2952 1.3281 0.0162 0.187 Uiso 1 1 calc R . . C66 C 0.3567(17) 1.2585(14) 0.1110(12) 0.128(8) Uani 1 1 d . . . H66 H 0.3243 1.2040 0.1055 0.153 Uiso 1 1 calc R . . C67 C 0.4190(12) 1.2660(11) 0.1743(8) 0.084(5) Uani 1 1 d . . . H67 H 0.4234 1.2152 0.2110 0.100 Uiso 1 1 calc R . . C68 C 0.4458(11) 1.4189(7) 0.3178(7) 0.060(3) Uani 1 1 d . . . C69 C 0.3201(12) 1.4105(8) 0.3244(7) 0.066(4) Uani 1 1 d . . . H69 H 0.2887 1.3676 0.2987 0.079 Uiso 1 1 calc R . . C70 C 0.2404(13) 1.4637(9) 0.3678(8) 0.078(4) Uani 1 1 d . . . H70 H 0.1577 1.4568 0.3701 0.094 Uiso 1 1 calc R . . C71 C 0.2847(15) 1.5257(9) 0.4064(9) 0.085(5) Uani 1 1 d . . . H71 H 0.2322 1.5614 0.4356 0.102 Uiso 1 1 calc R . . C72 C 0.4031(16) 1.5357(9) 0.4026(10) 0.107(6) Uani 1 1 d . . . H72 H 0.4327 1.5782 0.4297 0.128 Uiso 1 1 calc R . . C73 C 0.4837(14) 1.4831(9) 0.3583(9) 0.088(5) Uani 1 1 d . . . H73 H 0.5659 1.4921 0.3564 0.106 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0245(2) 0.0324(2) 0.0308(2) -0.00564(16) -0.00154(17) 0.00720(16) W2 0.0307(2) 0.0313(2) 0.0427(3) -0.00725(17) 0.00499(19) 0.00170(17) W3 0.0300(2) 0.0399(2) 0.0345(2) -0.01271(17) -0.00451(18) 0.00378(18) Se1 0.0448(6) 0.0475(6) 0.0371(6) 0.0010(5) -0.0040(5) 0.0129(5) Se2 0.0346(6) 0.0500(6) 0.0414(6) -0.0178(5) -0.0048(5) -0.0014(5) Se3 0.0295(6) 0.0407(6) 0.0598(7) -0.0222(5) -0.0026(5) 0.0070(4) Se4 0.0367(6) 0.0334(5) 0.0418(6) -0.0062(4) -0.0051(5) 0.0013(4) P1 0.0391(16) 0.0536(18) 0.0325(15) -0.0056(12) 0.0034(13) 0.0016(13) P2 0.072(2) 0.0435(18) 0.067(2) -0.0095(15) 0.0161(18) 0.0218(16) P3 0.0354(17) 0.0501(18) 0.084(2) -0.0242(16) 0.0032(16) -0.0081(14) P4 0.057(2) 0.093(3) 0.052(2) 0.0039(18) 0.0160(18) -0.0052(19) P5 0.0452(18) 0.0514(18) 0.063(2) -0.0309(15) -0.0041(16) 0.0003(14) P6 0.0427(18) 0.072(2) 0.063(2) -0.0266(16) -0.0245(16) 0.0029(16) O1 0.017(3) 0.050(4) 0.029(4) -0.008(3) -0.008(3) 0.007(3) O2 0.047(5) 0.031(4) 0.074(5) -0.015(3) 0.015(4) -0.001(3) O3 0.064(5) 0.057(5) 0.022(4) -0.013(3) -0.004(3) -0.002(4) C1 0.126(14) 0.066(10) 0.185(18) -0.063(11) 0.070(13) -0.023(10) C2 0.20(2) 0.103(13) 0.091(12) -0.014(9) -0.014(12) 0.109(13) C3 0.080(10) 0.074(9) 0.070(9) -0.008(7) 0.026(8) 0.031(7) C4 0.077(9) 0.078(9) 0.052(8) -0.029(7) 0.018(7) 0.007(7) C5 0.063(9) 0.110(12) 0.078(10) -0.002(8) 0.027(8) -0.031(8) C6 0.094(11) 0.087(10) 0.042(7) 0.007(6) -0.007(7) 0.013(8) C7 0.040(7) 0.075(9) 0.131(13) -0.028(8) -0.011(8) -0.001(6) C8 0.069(9) 0.059(8) 0.111(11) -0.032(7) -0.008(8) -0.017(7) C9 0.047(8) 0.087(10) 0.098(11) -0.026(8) 0.026(8) -0.027(7) C10 0.096(12) 0.088(11) 0.066(10) -0.019(8) 0.033(9) -0.030(9) C11 0.125(16) 0.168(18) 0.111(14) 0.092(12) 0.020(12) 0.034(13) C12 0.096(12) 0.177(17) 0.068(10) -0.049(10) 0.036(9) -0.058(12) C13 0.032(7) 0.106(11) 0.111(12) -0.052(9) -0.004(7) -0.004(7) C14 0.111(14) 0.107(13) 0.149(15) -0.014(11) -0.098(12) 0.013(10) C15 0.053(8) 0.098(11) 0.097(11) -0.062(8) -0.020(8) -0.007(8) C16 0.058(8) 0.062(8) 0.107(11) -0.049(8) 0.005(8) -0.003(7) C17 0.055(8) 0.104(11) 0.076(9) -0.049(8) 0.002(7) 0.013(7) C18 0.079(10) 0.039(7) 0.105(11) -0.021(7) -0.023(8) 0.016(6) B1 0.063(10) 0.055(9) 0.068(10) 0.000(7) 0.003(8) 0.013(7) C50 0.036(6) 0.034(6) 0.071(8) -0.008(5) 0.002(6) 0.004(5) C51 0.043(7) 0.056(8) 0.059(8) -0.015(6) 0.008(6) 0.003(6) C52 0.041(7) 0.043(7) 0.098(10) -0.016(7) -0.025(7) 0.009(5) C53 0.054(8) 0.062(8) 0.074(9) 0.004(7) -0.028(7) 0.012(6) C54 0.050(8) 0.073(9) 0.057(8) -0.001(6) -0.004(6) 0.006(6) C55 0.056(8) 0.044(7) 0.054(8) -0.008(5) 0.010(6) 0.004(6) C56 0.075(10) 0.034(7) 0.111(12) -0.008(7) 0.031(10) 0.001(6) C57 0.073(13) 0.117(15) 0.149(18) 0.001(12) 0.003(12) -0.014(10) C58 0.071(12) 0.083(12) 0.19(2) -0.009(12) 0.013(13) 0.013(9) C59 0.110(19) 0.063(12) 0.28(4) -0.064(19) 0.06(2) -0.016(11) C60 0.120(19) 0.071(11) 0.20(3) -0.073(15) 0.097(17) -0.030(12) C61 0.098(13) 0.051(9) 0.161(17) -0.042(9) 0.050(12) -0.017(8) C62 0.058(9) 0.062(9) 0.077(10) 0.004(7) 0.026(7) 0.017(7) C63 0.169(18) 0.085(11) 0.068(10) 0.005(8) 0.006(11) 0.078(11) C64 0.14(2) 0.19(2) 0.071(14) 0.038(14) 0.018(13) 0.123(17) C65 0.15(2) 0.21(3) 0.108(19) -0.05(2) -0.005(16) 0.04(2) C66 0.104(15) 0.156(19) 0.103(15) 0.036(14) 0.005(12) 0.031(13) C67 0.059(9) 0.140(15) 0.041(8) 0.017(8) 0.000(7) 0.011(9) C68 0.054(8) 0.044(7) 0.070(9) 0.006(6) 0.020(7) 0.015(6) C69 0.075(10) 0.051(8) 0.068(9) -0.008(6) 0.005(7) 0.010(7) C70 0.072(10) 0.075(10) 0.075(10) 0.005(8) 0.020(8) 0.023(8) C71 0.095(12) 0.057(9) 0.088(11) -0.008(8) 0.036(10) 0.017(8) C72 0.115(15) 0.060(10) 0.133(15) -0.023(9) 0.046(12) -0.011(10) C73 0.084(11) 0.059(9) 0.116(13) -0.016(8) 0.018(10) -0.011(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 W1 O1 2.023(5) . ? W1 Se2 2.4376(11) . ? W1 Se4 2.4607(10) . ? W1 P1 2.499(3) . ? W1 Se1 2.5000(11) . ? W1 P2 2.559(3) . ? W1 W2 2.8098(6) . ? W1 W3 2.8159(6) . ? W2 O2 2.022(6) . ? W2 Se3 2.4498(10) . ? W2 Se2 2.4683(11) . ? W2 Se1 2.5044(12) . ? W2 P3 2.508(3) . ? W2 P4 2.567(3) . ? W2 W3 2.8346(6) . ? W3 O3 2.045(6) . ? W3 Se4 2.4445(11) . ? W3 Se3 2.4632(11) . ? W3 Se1 2.5008(11) . ? W3 P5 2.520(3) . ? W3 P6 2.561(3) . ? P1 C5 1.809(11) . ? P1 C6 1.811(12) . ? P1 C4 1.831(11) . ? P2 C3 1.779(11) . ? P2 C1 1.805(14) . ? P2 C2 1.817(15) . ? P3 C7 1.804(13) . ? P3 C8 1.806(11) . ? P3 C9 1.864(12) . ? P4 C11 1.789(15) . ? P4 C12 1.800(14) . ? P4 C10 1.815(14) . ? P5 C18 1.795(12) . ? P5 C16 1.830(12) . ? P5 C17 1.845(11) . ? P6 C15 1.803(11) . ? P6 C13 1.808(12) . ? P6 C14 1.825(13) . ? C3 C4 1.539(16) . ? C9 C10 1.483(18) . ? C15 C16 1.494(17) . ? B1 C62 1.62(2) . ? B1 C68 1.635(17) . ? B1 C50 1.642(16) . ? B1 C56 1.66(2) . ? C50 C55 1.378(14) . ? C50 C51 1.398(14) . ? C51 C52 1.367(15) . ? C52 C53 1.343(15) . ? C53 C54 1.370(15) . ? C54 C55 1.371(15) . ? C56 C61 1.360(18) . ? C56 C57 1.43(2) . ? C57 C58 1.43(2) . ? C58 C59 1.41(3) . ? C59 C60 1.35(3) . ? C60 C61 1.38(2) . ? C62 C67 1.386(18) . ? C62 C63 1.423(17) . ? C63 C64 1.46(3) . ? C64 C65 1.41(3) . ? C65 C66 1.35(3) . ? C66 C67 1.38(2) . ? C68 C73 1.371(17) . ? C68 C69 1.405(16) . ? C69 C70 1.393(16) . ? C70 C71 1.354(18) . ? C71 C72 1.33(2) . ? C72 C73 1.402(18) . ? 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 O1 W1 Se2 156.89(17) . . ? O1 W1 Se4 95.23(17) . . ? Se2 W1 Se4 97.14(4) . . ? O1 W1 P1 77.68(17) . . ? Se2 W1 P1 84.56(7) . . ? Se4 W1 P1 82.89(7) . . ? O1 W1 Se1 84.54(16) . . ? Se2 W1 Se1 109.72(4) . . ? Se4 W1 Se1 108.46(4) . . ? P1 W1 Se1 159.81(7) . . ? O1 W1 P2 74.22(19) . . ? Se2 W1 P2 88.01(9) . . ? Se4 W1 P2 160.41(8) . . ? P1 W1 P2 78.78(10) . . ? Se1 W1 P2 87.28(8) . . ? O1 W1 W2 140.27(16) . . ? Se2 W1 W2 55.57(3) . . ? Se4 W1 W2 100.51(3) . . ? P1 W1 W2 140.13(7) . . ? Se1 W1 W2 55.92(3) . . ? P2 W1 W2 97.98(7) . . ? O1 W1 W3 102.41(16) . . ? Se2 W1 W3 100.67(3) . . ? Se4 W1 W3 54.70(3) . . ? P1 W1 W3 137.56(7) . . ? Se1 W1 W3 55.75(3) . . ? P2 W1 W3 142.89(8) . . ? W2 W1 W3 60.512(14) . . ? O2 W2 Se3 156.60(18) . . ? O2 W2 Se2 96.3(2) . . ? Se3 W2 Se2 97.24(4) . . ? O2 W2 Se1 85.1(2) . . ? Se3 W2 Se1 108.33(4) . . ? Se2 W2 Se1 108.58(4) . . ? O2 W2 P3 79.0(2) . . ? Se3 W2 P3 83.75(7) . . ? Se2 W2 P3 83.28(8) . . ? Se1 W2 P3 161.22(8) . . ? O2 W2 P4 74.1(2) . . ? Se3 W2 P4 87.27(9) . . ? Se2 W2 P4 161.17(9) . . ? Se1 W2 P4 87.06(9) . . ? P3 W2 P4 79.03(12) . . ? O2 W2 W1 103.03(18) . . ? Se3 W2 W1 100.37(3) . . ? Se2 W2 W1 54.55(3) . . ? Se1 W2 W1 55.77(3) . . ? P3 W2 W1 137.83(8) . . ? P4 W2 W1 142.68(9) . . ? O2 W2 W3 140.4(2) . . ? Se3 W2 W3 54.99(3) . . ? Se2 W2 W3 99.40(3) . . ? Se1 W2 W3 55.45(3) . . ? P3 W2 W3 138.72(7) . . ? P4 W2 W3 98.14(9) . . ? W1 W2 W3 59.850(14) . . ? O3 W3 Se4 155.28(19) . . ? O3 W3 Se3 96.5(2) . . ? Se4 W3 Se3 97.85(4) . . ? O3 W3 Se1 85.42(19) . . ? Se4 W3 Se1 108.95(3) . . ? Se3 W3 Se1 108.02(4) . . ? O3 W3 P5 77.4(2) . . ? Se4 W3 P5 84.23(8) . . ? Se3 W3 P5 83.83(7) . . ? Se1 W3 P5 160.24(8) . . ? O3 W3 P6 75.2(2) . . ? Se4 W3 P6 85.15(8) . . ? Se3 W3 P6 161.89(8) . . ? Se1 W3 P6 87.61(8) . . ? P5 W3 P6 78.69(10) . . ? O3 W3 W1 140.84(19) . . ? Se4 W3 W1 55.24(3) . . ? Se3 W3 W1 99.87(3) . . ? Se1 W3 W1 55.72(3) . . ? P5 W3 W1 139.46(7) . . ? P6 W3 W1 96.50(7) . . ? O3 W3 W2 104.48(18) . . ? Se4 W3 W2 100.24(3) . . ? Se3 W3 W2 54.54(2) . . ? Se1 W3 W2 55.56(3) . . ? P5 W3 W2 138.37(7) . . ? P6 W3 W2 142.69(8) . . ? W1 W3 W2 59.638(14) . . ? W1 Se1 W3 68.54(3) . . ? W1 Se1 W2 68.31(3) . . ? W3 Se1 W2 68.99(3) . . ? W1 Se2 W2 69.88(3) . . ? W2 Se3 W3 70.47(3) . . ? W3 Se4 W1 70.07(3) . . ? C5 P1 C6 102.6(6) . . ? C5 P1 C4 103.4(6) . . ? C6 P1 C4 104.1(6) . . ? C5 P1 W1 113.8(4) . . ? C6 P1 W1 120.6(4) . . ? C4 P1 W1 110.4(4) . . ? C3 P2 C1 103.4(7) . . ? C3 P2 C2 105.6(7) . . ? C1 P2 C2 105.4(8) . . ? C3 P2 W1 106.6(4) . . ? C1 P2 W1 119.9(5) . . ? C2 P2 W1 114.6(5) . . ? C7 P3 C8 106.2(6) . . ? C7 P3 C9 106.0(6) . . ? C8 P3 C9 102.9(6) . . ? C7 P3 W2 119.0(4) . . ? C8 P3 W2 113.7(4) . . ? C9 P3 W2 107.7(5) . . ? C11 P4 C12 103.8(9) . . ? C11 P4 C10 103.7(8) . . ? C12 P4 C10 102.8(6) . . ? C11 P4 W2 116.1(5) . . ? C12 P4 W2 121.3(5) . . ? C10 P4 W2 107.2(5) . . ? C18 P5 C16 105.8(6) . . ? C18 P5 C17 103.3(6) . . ? C16 P5 C17 103.2(6) . . ? C18 P5 W3 120.4(4) . . ? C16 P5 W3 108.1(4) . . ? C17 P5 W3 114.5(4) . . ? C15 P6 C13 104.9(6) . . ? C15 P6 C14 104.4(7) . . ? C13 P6 C14 102.7(7) . . ? C15 P6 W3 106.9(4) . . ? C13 P6 W3 121.2(4) . . ? C14 P6 W3 115.2(5) . . ? C4 C3 P2 113.6(8) . . ? C3 C4 P1 108.2(8) . . ? C10 C9 P3 111.1(9) . . ? C9 C10 P4 110.7(9) . . ? C16 C15 P6 110.1(8) . . ? C15 C16 P5 112.5(9) . . ? C62 B1 C68 106.0(11) . . ? C62 B1 C50 109.5(11) . . ? C68 B1 C50 110.3(10) . . ? C62 B1 C56 113.1(12) . . ? C68 B1 C56 113.6(11) . . ? C50 B1 C56 104.3(10) . . ? C55 C50 C51 114.3(10) . . ? C55 C50 B1 123.9(10) . . ? C51 C50 B1 121.2(10) . . ? C52 C51 C50 123.3(11) . . ? C53 C52 C51 120.0(11) . . ? C52 C53 C54 119.3(11) . . ? C53 C54 C55 120.1(12) . . ? C54 C55 C50 122.8(10) . . ? C61 C56 C57 115.6(16) . . ? C61 C56 B1 126.9(16) . . ? C57 C56 B1 117.3(13) . . ? C56 C57 C58 124.3(18) . . ? C59 C58 C57 111(2) . . ? C60 C59 C58 128(2) . . ? C59 C60 C61 115(2) . . ? C56 C61 C60 125(2) . . ? C67 C62 C63 114.8(15) . . ? C67 C62 B1 125.4(12) . . ? C63 C62 B1 119.5(14) . . ? C62 C63 C64 117.7(18) . . ? C65 C64 C63 122.8(19) . . ? C66 C65 C64 118(2) . . ? C65 C66 C67 120(2) . . ? C66 C67 C62 127.2(15) . . ? C73 C68 C69 114.5(11) . . ? C73 C68 B1 125.2(13) . . ? C69 C68 B1 120.2(12) . . ? C70 C69 C68 122.8(13) . . ? C71 C70 C69 119.3(14) . . ? C72 C71 C70 120.2(14) . . ? C71 C72 C73 120.7(16) . . ? C68 C73 C72 122.4(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.270 _refine_diff_density_min -1.554 _refine_diff_density_rms 0.181 data_[W3Se4H3(dmpe)3]BPh4 _database_code_depnum_ccdc_archive 'CCDC 225463' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H71 B P6 Se4 W3' _chemical_formula_weight 1640.01 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' B B 0.0013 0.0007 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.081(6) _cell_length_b 11.364(5) _cell_length_c 33.098(16) _cell_angle_alpha 90.00 _cell_angle_beta 98.730(12) _cell_angle_gamma 90.00 _cell_volume 5607(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour prism _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 8.934 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? #_Ratio of minimum to maximum apparent transmission 0.484085 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31351 _diffrn_reflns_av_R_equivalents 0.1280 _diffrn_reflns_av_sigmaI/netI 0.1457 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9883 _reflns_number_gt 5514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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^)+(0.0637P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9883 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 W1 W 0.84721(4) 0.92752(6) 0.17907(2) 0.02943(19) Uani 1 1 d . . . W2 W 0.94403(4) 0.98720(5) 0.11535(2) 0.0325(2) Uani 1 1 d . . . W3 W 0.79287(4) 1.12036(6) 0.12789(2) 0.03123(19) Uani 1 1 d . . . Se1 Se 0.78725(11) 0.91081(14) 0.10485(5) 0.0376(4) Uani 1 1 d . . . Se2 Se 1.01196(11) 0.93822(16) 0.18613(6) 0.0405(4) Uani 1 1 d . . . Se3 Se 0.93499(11) 1.20364(14) 0.11282(6) 0.0458(5) Uani 1 1 d . . . Se4 Se 0.80366(12) 1.12180(14) 0.20282(6) 0.0400(4) Uani 1 1 d . . . P1 P 0.8759(3) 0.8656(4) 0.25203(14) 0.0416(12) Uani 1 1 d . . . P2 P 0.6941(3) 0.8485(4) 0.18821(16) 0.0434(12) Uani 1 1 d . . . P3 P 1.0991(3) 1.0197(4) 0.10038(17) 0.0487(13) Uani 1 1 d . . . P4 P 0.9847(4) 0.7837(4) 0.09448(16) 0.0490(13) Uani 1 1 d . . . P5 P 0.7444(3) 1.3271(4) 0.13282(17) 0.0454(13) Uani 1 1 d . . . P6 P 0.7188(3) 1.1591(4) 0.05564(16) 0.0516(14) Uani 1 1 d . . . C1 C 0.9456(15) 0.7380(18) 0.2637(7) 0.090(8) Uani 1 1 d . . . H1A H 1.0027 0.7510 0.2549 0.136 Uiso 1 1 calc R . . H1B H 0.9171 0.6708 0.2497 0.136 Uiso 1 1 calc R . . H1C H 0.9543 0.7241 0.2926 0.136 Uiso 1 1 calc R . . C2 C 0.9236(13) 0.9731(16) 0.2912(6) 0.069(7) Uani 1 1 d . . . H2A H 0.8897 1.0448 0.2876 0.103 Uiso 1 1 calc R . . H2B H 0.9849 0.9887 0.2884 0.103 Uiso 1 1 calc R . . H2C H 0.9209 0.9416 0.3179 0.103 Uiso 1 1 calc R . . C3 C 0.7688(13) 0.830(2) 0.2692(6) 0.078(7) Uani 1 1 d . . . H3A H 0.7802 0.7742 0.2917 0.094 Uiso 1 1 calc R . . H3B H 0.7445 0.9007 0.2795 0.094 Uiso 1 1 calc R . . C4 C 0.7048(17) 0.782(3) 0.2391(7) 0.114(10) Uani 1 1 d . . . H4A H 0.6470 0.7868 0.2484 0.137 Uiso 1 1 calc R . . H4B H 0.7184 0.6990 0.2365 0.137 Uiso 1 1 calc R . . C5 C 0.6017(12) 0.9411(19) 0.1870(8) 0.097(9) Uani 1 1 d . . . H5A H 0.6186 1.0096 0.2033 0.145 Uiso 1 1 calc R . . H5B H 0.5545 0.9003 0.1976 0.145 Uiso 1 1 calc R . . H5C H 0.5810 0.9647 0.1593 0.145 Uiso 1 1 calc R . . C6 C 0.6513(13) 0.7287(16) 0.1557(7) 0.071(7) Uani 1 1 d . . . H6A H 0.6981 0.6721 0.1545 0.106 Uiso 1 1 calc R . . H6B H 0.6304 0.7579 0.1287 0.106 Uiso 1 1 calc R . . H6C H 0.6025 0.6920 0.1664 0.106 Uiso 1 1 calc R . . C7 C 1.1762(11) 1.1007(18) 0.1364(7) 0.073(7) Uani 1 1 d . . . H7A H 1.1517 1.1770 0.1404 0.109 Uiso 1 1 calc R . . H7B H 1.2320 1.1094 0.1261 0.109 Uiso 1 1 calc R . . H7C H 1.1862 1.0592 0.1619 0.109 Uiso 1 1 calc R . . C8 C 1.1090(13) 1.0924(17) 0.0507(7) 0.073(7) Uani 1 1 d . . . H8A H 1.0699 1.0541 0.0291 0.110 Uiso 1 1 calc R . . H8B H 1.1698 1.0869 0.0456 0.110 Uiso 1 1 calc R . . H8C H 1.0923 1.1738 0.0520 0.110 Uiso 1 1 calc R . . C9 C 1.1529(12) 0.8814(18) 0.0959(8) 0.078(8) Uani 1 1 d . . . H9A H 1.2039 0.8923 0.0816 0.094 Uiso 1 1 calc R . . H9B H 1.1750 0.8511 0.1229 0.094 Uiso 1 1 calc R . . C10 C 1.0881(15) 0.7926(17) 0.0727(7) 0.079(8) Uani 1 1 d . . . H10A H 1.1164 0.7157 0.0739 0.095 Uiso 1 1 calc R . . H10B H 1.0745 0.8158 0.0443 0.095 Uiso 1 1 calc R . . C11 C 1.0066(17) 0.6693(16) 0.1320(8) 0.102(9) Uani 1 1 d . . . H11A H 1.0468 0.6980 0.1551 0.153 Uiso 1 1 calc R . . H11B H 1.0333 0.6032 0.1203 0.153 Uiso 1 1 calc R . . H11C H 0.9513 0.6454 0.1405 0.153 Uiso 1 1 calc R . . C12 C 0.9071(15) 0.710(2) 0.0554(7) 0.097(9) Uani 1 1 d . . . H12A H 0.8887 0.7635 0.0332 0.146 Uiso 1 1 calc R . . H12B H 0.8554 0.6846 0.0668 0.146 Uiso 1 1 calc R . . H12C H 0.9360 0.6431 0.0454 0.146 Uiso 1 1 calc R . . C13 C 0.8222(12) 1.4324(17) 0.1582(7) 0.079(7) Uani 1 1 d . . . H13A H 0.8786 1.4251 0.1483 0.119 Uiso 1 1 calc R . . H13B H 0.8308 1.4181 0.1871 0.119 Uiso 1 1 calc R . . H13C H 0.7990 1.5104 0.1527 0.119 Uiso 1 1 calc R . . C14 C 0.6437(12) 1.3532(17) 0.1538(7) 0.073(7) Uani 1 1 d . . . H14A H 0.5972 1.3020 0.1409 0.110 Uiso 1 1 calc R . . H14B H 0.6255 1.4337 0.1491 0.110 Uiso 1 1 calc R . . H14C H 0.6544 1.3381 0.1827 0.110 Uiso 1 1 calc R . . C15 C 0.7176(14) 1.3856(15) 0.0798(7) 0.071(7) Uani 1 1 d . . . H15A H 0.6846 1.4588 0.0801 0.085 Uiso 1 1 calc R . . H15B H 0.7729 1.4018 0.0692 0.085 Uiso 1 1 calc R . . C16 C 0.6625(13) 1.2979(15) 0.0528(6) 0.061(6) Uani 1 1 d . . . H16A H 0.6535 1.3259 0.0247 0.073 Uiso 1 1 calc R . . H16B H 0.6042 1.2891 0.0614 0.073 Uiso 1 1 calc R . . C17 C 0.7849(14) 1.169(2) 0.0155(6) 0.078(7) Uani 1 1 d . . . H17A H 0.8184 1.0979 0.0143 0.118 Uiso 1 1 calc R . . H17B H 0.8255 1.2345 0.0206 0.118 Uiso 1 1 calc R . . H17C H 0.7463 1.1809 -0.0101 0.118 Uiso 1 1 calc R . . C18 C 0.6251(14) 1.0617(19) 0.0340(7) 0.093(9) Uani 1 1 d . . . H18A H 0.5860 1.0496 0.0539 0.139 Uiso 1 1 calc R . . H18B H 0.6486 0.9874 0.0268 0.139 Uiso 1 1 calc R . . H18C H 0.5922 1.0977 0.0101 0.139 Uiso 1 1 calc R . . B1 B 0.6357(13) 1.0033(17) 0.3883(6) 0.038(5) Uani 1 1 d . . . C50 C 0.6313(12) 1.0644(16) 0.3437(6) 0.046(5) Uani 1 1 d . . . C51 C 0.5535(14) 1.067(2) 0.3159(7) 0.073(7) Uani 1 1 d . . . H51 H 0.5033 1.0281 0.3222 0.087 Uiso 1 1 calc R . . C52 C 0.547(2) 1.126(3) 0.2791(8) 0.109(11) Uani 1 1 d . . . H52 H 0.4953 1.1171 0.2599 0.130 Uiso 1 1 calc R . . C53 C 0.618(3) 1.200(3) 0.2702(10) 0.153(18) Uani 1 1 d . . . H53 H 0.6142 1.2454 0.2465 0.184 Uiso 1 1 calc R . . C54 C 0.688(2) 1.199(3) 0.2976(9) 0.104(10) Uani 1 1 d . . . H54 H 0.7354 1.2466 0.2924 0.125 Uiso 1 1 calc R . . C55 C 0.7029(16) 1.1351(15) 0.3342(6) 0.061(6) Uani 1 1 d . . . H55 H 0.7574 1.1390 0.3516 0.073 Uiso 1 1 calc R . . C56 C 0.6085(11) 0.8626(15) 0.3851(5) 0.041(4) Uani 1 1 d . . . C57 C 0.6102(13) 0.789(2) 0.4224(8) 0.079(7) Uani 1 1 d . . . H57 H 0.6229 0.8249 0.4478 0.095 Uiso 1 1 calc R . . C58 C 0.5948(12) 0.6744(18) 0.4211(8) 0.069(7) Uani 1 1 d . . . H58 H 0.5968 0.6348 0.4458 0.083 Uiso 1 1 calc R . . C59 C 0.5757(16) 0.6094(19) 0.3855(9) 0.088(9) Uani 1 1 d . . . H59 H 0.5644 0.5290 0.3857 0.106 Uiso 1 1 calc R . . C60 C 0.5746(11) 0.6704(19) 0.3500(8) 0.073(8) Uani 1 1 d . . . H60 H 0.5628 0.6292 0.3255 0.087 Uiso 1 1 calc R . . C61 C 0.5907(11) 0.7956(18) 0.3483(6) 0.056(5) Uani 1 1 d . . . H61 H 0.5895 0.8325 0.3232 0.067 Uiso 1 1 calc R . . C62 C 0.5729(11) 1.0866(13) 0.4139(5) 0.038(4) Uani 1 1 d . . . C63 C 0.5837(13) 1.2087(15) 0.4134(6) 0.059(6) Uani 1 1 d . . . H63 H 0.6243 1.2426 0.3984 0.071 Uiso 1 1 calc R . . C64 C 0.5329(14) 1.2796(17) 0.4360(6) 0.062(7) Uani 1 1 d . . . H64 H 0.5415 1.3605 0.4353 0.074 Uiso 1 1 calc R . . C65 C 0.4723(14) 1.239(2) 0.4585(6) 0.061(6) Uani 1 1 d . . . H65 H 0.4412 1.2882 0.4738 0.073 Uiso 1 1 calc R . . C66 C 0.4595(13) 1.1185(19) 0.4576(6) 0.060(6) Uani 1 1 d . . . H66 H 0.4158 1.0862 0.4713 0.072 Uiso 1 1 calc R . . C67 C 0.5112(12) 1.0429(19) 0.4362(7) 0.063(6) Uani 1 1 d . . . H67 H 0.5030 0.9620 0.4374 0.076 Uiso 1 1 calc R . . C68 C 0.7401(11) 0.9962(12) 0.4147(6) 0.042(5) Uani 1 1 d . . . C69 C 0.7645(11) 1.0278(15) 0.4539(6) 0.046(5) Uani 1 1 d . . . H69 H 0.7217 1.0634 0.4674 0.055 Uiso 1 1 calc R . . C70 C 0.8499(12) 1.0104(17) 0.4756(6) 0.055(5) Uani 1 1 d . . . H70 H 0.8635 1.0374 0.5024 0.066 Uiso 1 1 calc R . . C71 C 0.9138(14) 0.9541(16) 0.4580(7) 0.063(6) Uani 1 1 d . . . H71 H 0.9702 0.9369 0.4724 0.075 Uiso 1 1 calc R . . C72 C 0.8901(12) 0.9244(16) 0.4176(7) 0.055(5) Uani 1 1 d . . . H72 H 0.9333 0.8902 0.4041 0.067 Uiso 1 1 calc R . . C73 C 0.8073(11) 0.9420(15) 0.3966(6) 0.044(5) Uani 1 1 d . . . H73 H 0.7947 0.9176 0.3695 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0329(4) 0.0297(4) 0.0264(4) 0.0006(3) 0.0071(3) 0.0010(3) W2 0.0382(4) 0.0304(4) 0.0320(4) -0.0005(3) 0.0150(3) 0.0035(3) W3 0.0319(4) 0.0300(4) 0.0332(4) 0.0039(3) 0.0096(3) 0.0018(3) Se1 0.0483(10) 0.0373(10) 0.0267(10) 0.0015(8) 0.0036(8) -0.0048(8) Se2 0.0343(9) 0.0511(11) 0.0360(11) -0.0027(9) 0.0056(8) 0.0058(8) Se3 0.0426(10) 0.0307(9) 0.0704(15) 0.0028(9) 0.0283(10) -0.0006(8) Se4 0.0454(10) 0.0379(10) 0.0382(11) -0.0044(8) 0.0112(9) 0.0040(8) P1 0.043(3) 0.050(3) 0.031(3) 0.005(2) 0.004(2) 0.002(2) P2 0.035(3) 0.050(3) 0.045(3) 0.010(2) 0.004(2) -0.001(2) P3 0.044(3) 0.050(3) 0.057(4) -0.003(3) 0.026(3) 0.005(2) P4 0.075(4) 0.033(3) 0.045(3) -0.011(2) 0.027(3) 0.002(2) P5 0.038(3) 0.041(3) 0.061(4) 0.007(2) 0.016(3) 0.005(2) P6 0.061(3) 0.050(3) 0.044(3) 0.013(2) 0.008(3) 0.014(3) C1 0.109(19) 0.076(16) 0.079(19) 0.002(14) -0.010(16) 0.024(14) C2 0.078(15) 0.055(13) 0.069(16) 0.028(11) -0.007(12) 0.000(11) C3 0.069(15) 0.14(2) 0.036(14) 0.032(14) 0.027(12) -0.017(14) C4 0.11(2) 0.17(3) 0.057(18) 0.042(18) 0.020(16) -0.05(2) C5 0.038(12) 0.087(17) 0.17(3) -0.005(17) 0.040(15) 0.011(12) C6 0.070(14) 0.053(13) 0.086(18) -0.004(12) 0.002(13) -0.011(11) C7 0.042(12) 0.098(17) 0.081(18) -0.006(13) 0.018(11) -0.029(11) C8 0.059(13) 0.069(15) 0.10(2) 0.002(13) 0.050(13) -0.007(11) C9 0.035(11) 0.072(15) 0.14(2) -0.005(15) 0.036(13) 0.008(11) C10 0.15(2) 0.047(12) 0.064(16) 0.003(11) 0.074(16) 0.033(14) C11 0.17(3) 0.032(12) 0.13(2) -0.008(13) 0.09(2) 0.001(14) C12 0.102(19) 0.095(19) 0.10(2) -0.038(16) 0.020(17) -0.009(15) C13 0.055(13) 0.072(15) 0.11(2) 0.002(14) -0.008(13) 0.007(12) C14 0.063(14) 0.053(13) 0.11(2) -0.002(12) 0.034(14) 0.017(11) C15 0.081(15) 0.040(11) 0.100(19) 0.030(12) 0.043(14) 0.043(11) C16 0.083(15) 0.047(12) 0.047(14) 0.015(10) -0.009(12) 0.022(11) C17 0.101(17) 0.110(18) 0.027(13) 0.009(12) 0.020(12) 0.032(15) C18 0.095(18) 0.084(17) 0.09(2) 0.033(14) -0.029(15) -0.004(14) B1 0.044(12) 0.048(12) 0.021(11) -0.007(9) 0.002(9) 0.001(10) C50 0.037(10) 0.058(12) 0.051(13) -0.004(10) 0.030(10) 0.000(9) C51 0.050(13) 0.115(19) 0.058(16) 0.017(14) 0.021(12) 0.034(13) C52 0.13(3) 0.16(3) 0.038(17) -0.008(17) 0.013(17) 0.07(2) C53 0.27(6) 0.15(3) 0.07(3) 0.03(2) 0.11(3) 0.04(4) C54 0.15(3) 0.10(2) 0.07(2) -0.012(19) 0.03(2) -0.02(2) C55 0.107(18) 0.044(11) 0.033(13) 0.002(10) 0.018(12) 0.012(12) C56 0.039(10) 0.054(11) 0.031(11) -0.014(9) 0.010(9) 0.006(9) C57 0.069(15) 0.075(17) 0.09(2) 0.027(14) 0.016(14) -0.003(13) C58 0.055(13) 0.048(13) 0.10(2) 0.004(13) 0.001(13) -0.013(11) C59 0.10(2) 0.042(13) 0.11(2) 0.013(15) -0.015(18) 0.003(13) C60 0.024(10) 0.067(15) 0.12(2) -0.060(15) -0.004(12) -0.012(10) C61 0.037(11) 0.087(16) 0.043(13) 0.000(11) 0.007(10) 0.008(10) C62 0.033(10) 0.036(10) 0.040(11) -0.005(8) -0.006(9) 0.003(8) C63 0.080(15) 0.044(12) 0.061(15) 0.012(10) 0.036(12) 0.007(11) C64 0.082(15) 0.058(13) 0.040(13) -0.040(11) -0.009(12) 0.031(12) C65 0.064(14) 0.092(18) 0.028(12) -0.013(11) 0.012(11) 0.026(13) C66 0.055(13) 0.080(16) 0.051(14) -0.008(12) 0.027(11) -0.006(12) C67 0.039(11) 0.074(14) 0.085(18) -0.009(12) 0.032(12) 0.008(10) C68 0.054(11) 0.008(8) 0.061(14) 0.004(8) 0.002(10) 0.004(8) C69 0.046(11) 0.056(12) 0.037(12) 0.005(9) 0.009(10) 0.017(9) C70 0.045(12) 0.078(14) 0.040(13) 0.020(11) -0.002(10) 0.008(11) C71 0.052(13) 0.043(12) 0.09(2) 0.011(12) 0.004(13) 0.009(10) C72 0.044(12) 0.055(12) 0.071(17) 0.005(11) 0.021(11) 0.003(10) C73 0.040(11) 0.048(11) 0.047(13) -0.005(9) 0.010(9) 0.004(9) _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 W1 Se2 2.463(2) . ? W1 Se4 2.466(2) . ? W1 P1 2.489(5) . ? W1 Se1 2.493(2) . ? W1 P2 2.538(5) . ? W1 W3 2.8147(13) . ? W1 W2 2.8242(14) . ? W2 Se3 2.464(2) . ? W2 Se2 2.474(2) . ? W2 P3 2.490(5) . ? W2 Se1 2.493(2) . ? W2 P4 2.516(5) . ? W2 W3 2.8191(13) . ? W3 Se4 2.461(2) . ? W3 Se3 2.462(2) . ? W3 P5 2.474(5) . ? W3 Se1 2.498(2) . ? W3 P6 2.520(5) . ? P1 C1 1.799(19) . ? P1 C3 1.837(19) . ? P1 C2 1.845(19) . ? P2 C5 1.743(18) . ? P2 C6 1.794(18) . ? P2 C4 1.83(2) . ? P3 C9 1.785(19) . ? P3 C7 1.788(18) . ? P3 C8 1.87(2) . ? P4 C11 1.79(2) . ? P4 C12 1.81(2) . ? P4 C10 1.82(2) . ? P5 C14 1.79(2) . ? P5 C13 1.794(19) . ? P5 C15 1.86(2) . ? P6 C17 1.78(2) . ? P6 C16 1.787(17) . ? P6 C18 1.85(2) . ? C3 C4 1.39(3) . ? C9 C10 1.53(3) . ? C15 C16 1.50(3) . ? B1 C50 1.62(3) . ? B1 C56 1.65(2) . ? B1 C62 1.66(3) . ? B1 C68 1.68(2) . ? C50 C51 1.38(2) . ? C50 C55 1.42(3) . ? C51 C52 1.38(3) . ? C52 C53 1.44(4) . ? C53 C54 1.28(4) . ? C54 C55 1.40(3) . ? C56 C61 1.43(2) . ? C56 C57 1.49(3) . ? C57 C58 1.32(3) . ? C58 C59 1.38(3) . ? C59 C60 1.36(3) . ? C60 C61 1.45(3) . ? C62 C67 1.37(2) . ? C62 C63 1.40(2) . ? C63 C64 1.40(2) . ? C64 C65 1.35(3) . ? C65 C66 1.38(3) . ? C66 C67 1.42(3) . ? C68 C69 1.35(2) . ? C68 C73 1.40(2) . ? C69 C70 1.39(2) . ? C70 C71 1.36(3) . ? C71 C72 1.37(3) . ? C72 C73 1.35(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 W1 Se4 103.84(6) . . ? Se2 W1 P1 84.13(12) . . ? Se4 W1 P1 87.67(12) . . ? Se2 W1 Se1 107.88(7) . . ? Se4 W1 Se1 107.94(6) . . ? P1 W1 Se1 156.65(12) . . ? Se2 W1 P2 158.28(11) . . ? Se4 W1 P2 89.30(12) . . ? P1 W1 P2 79.14(15) . . ? Se1 W1 P2 83.68(12) . . ? Se2 W1 W3 102.47(5) . . ? Se4 W1 W3 55.07(5) . . ? P1 W1 W3 142.72(11) . . ? Se1 W1 W3 55.76(5) . . ? P2 W1 W3 99.23(11) . . ? Se2 W1 W2 55.28(5) . . ? Se4 W1 W2 102.47(5) . . ? P1 W1 W2 139.38(11) . . ? Se1 W1 W2 55.51(5) . . ? P2 W1 W2 139.19(12) . . ? W3 W1 W2 59.99(3) . . ? Se3 W2 Se2 105.64(7) . . ? Se3 W2 P3 83.92(12) . . ? Se2 W2 P3 87.44(14) . . ? Se3 W2 Se1 107.24(6) . . ? Se2 W2 Se1 107.53(6) . . ? P3 W2 Se1 157.40(13) . . ? Se3 W2 P4 157.33(13) . . ? Se2 W2 P4 88.28(13) . . ? P3 W2 P4 78.83(17) . . ? Se1 W2 P4 84.68(13) . . ? Se3 W2 W3 55.06(5) . . ? Se2 W2 W3 102.07(5) . . ? P3 W2 W3 138.98(12) . . ? Se1 W2 W3 55.69(5) . . ? P4 W2 W3 140.37(13) . . ? Se3 W2 W1 103.46(5) . . ? Se2 W2 W1 54.93(5) . . ? P3 W2 W1 142.35(13) . . ? Se1 W2 W1 55.49(5) . . ? P4 W2 W1 99.17(12) . . ? W3 W2 W1 59.84(3) . . ? Se4 W3 Se3 105.98(7) . . ? Se4 W3 P5 84.39(13) . . ? Se3 W3 P5 85.62(12) . . ? Se4 W3 Se1 107.94(6) . . ? Se3 W3 Se1 107.15(6) . . ? P5 W3 Se1 158.28(12) . . ? Se4 W3 P6 155.14(13) . . ? Se3 W3 P6 90.84(14) . . ? P5 W3 P6 78.68(17) . . ? Se1 W3 P6 83.52(12) . . ? Se4 W3 W1 55.25(5) . . ? Se3 W3 W1 103.79(5) . . ? P5 W3 W1 139.63(13) . . ? Se1 W3 W1 55.58(5) . . ? P6 W3 W1 138.92(12) . . ? Se4 W3 W2 102.76(5) . . ? Se3 W3 W2 55.12(5) . . ? P5 W3 W2 140.67(11) . . ? Se1 W3 W2 55.53(5) . . ? P6 W3 W2 101.88(13) . . ? W1 W3 W2 60.17(3) . . ? W1 Se1 W2 69.00(5) . . ? W1 Se1 W3 68.66(5) . . ? W2 Se1 W3 68.78(5) . . ? W1 Se2 W2 69.79(5) . . ? W3 Se3 W2 69.81(5) . . ? W3 Se4 W1 69.69(5) . . ? C1 P1 C3 105.5(11) . . ? C1 P1 C2 103.3(9) . . ? C3 P1 C2 101.4(10) . . ? C1 P1 W1 116.5(8) . . ? C3 P1 W1 109.4(7) . . ? C2 P1 W1 119.1(6) . . ? C5 P2 C6 103.3(10) . . ? C5 P2 C4 103.3(13) . . ? C6 P2 C4 102.2(12) . . ? C5 P2 W1 121.5(8) . . ? C6 P2 W1 116.6(7) . . ? C4 P2 W1 107.5(8) . . ? C9 P3 C7 104.5(10) . . ? C9 P3 C8 102.6(11) . . ? C7 P3 C8 103.2(10) . . ? C9 P3 W2 109.8(7) . . ? C7 P3 W2 118.6(7) . . ? C8 P3 W2 116.4(6) . . ? C11 P4 C12 101.0(11) . . ? C11 P4 C10 103.7(10) . . ? C12 P4 C10 104.1(11) . . ? C11 P4 W2 120.2(7) . . ? C12 P4 W2 117.5(8) . . ? C10 P4 W2 108.5(6) . . ? C14 P5 C13 104.0(10) . . ? C14 P5 C15 103.4(9) . . ? C13 P5 C15 103.6(10) . . ? C14 P5 W3 117.4(7) . . ? C13 P5 W3 119.0(6) . . ? C15 P5 W3 107.5(6) . . ? C17 P6 C16 102.6(10) . . ? C17 P6 C18 103.3(12) . . ? C16 P6 C18 100.3(10) . . ? C17 P6 W3 120.1(7) . . ? C16 P6 W3 110.1(7) . . ? C18 P6 W3 117.7(7) . . ? C4 C3 P1 114.4(17) . . ? C3 C4 P2 116.9(18) . . ? C10 C9 P3 111.0(13) . . ? C9 C10 P4 111.1(14) . . ? C16 C15 P5 110.2(13) . . ? C15 C16 P6 109.8(12) . . ? C50 B1 C56 112.4(14) . . ? C50 B1 C62 105.8(14) . . ? C56 B1 C62 115.5(15) . . ? C50 B1 C68 113.4(15) . . ? C56 B1 C68 101.0(13) . . ? C62 B1 C68 108.9(13) . . ? C51 C50 C55 115.9(19) . . ? C51 C50 B1 122.1(17) . . ? C55 C50 B1 121.1(16) . . ? C52 C51 C50 123(2) . . ? C51 C52 C53 121(3) . . ? C54 C53 C52 114(3) . . ? C53 C54 C55 128(3) . . ? C54 C55 C50 117(2) . . ? C61 C56 C57 112.5(18) . . ? C61 C56 B1 125.8(17) . . ? C57 C56 B1 121.4(16) . . ? C58 C57 C56 123(2) . . ? C57 C58 C59 124(2) . . ? C60 C59 C58 116(2) . . ? C59 C60 C61 124(2) . . ? C56 C61 C60 120.2(19) . . ? C67 C62 C63 117.2(17) . . ? C67 C62 B1 123.8(16) . . ? C63 C62 B1 119.0(16) . . ? C62 C63 C64 119.4(19) . . ? C65 C64 C63 125(2) . . ? C64 C65 C66 115.7(19) . . ? C65 C66 C67 122(2) . . ? C62 C67 C66 121.4(19) . . ? C69 C68 C73 115.0(16) . . ? C69 C68 B1 125.9(17) . . ? C73 C68 B1 118.8(16) . . ? C68 C69 C70 123.9(18) . . ? C71 C70 C69 120(2) . . ? C70 C71 C72 116.0(18) . . ? C73 C72 C71 123(2) . . ? C72 C73 C68 121.3(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.749 _refine_diff_density_min -1.495 _refine_diff_density_rms 0.319