Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author 'Peter Brueggeller' _publ_contact_author_phone '+43 512 5075115' _publ_contact_author_fax '+43 512 5072934' _publ_contact_author_email Peter.Brueggeller@uibk.ac.at _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' loop_ _publ_author_name 'Thomas Stampfl' 'Rene Gutmann' 'Georg Czermak' 'Christoph Langes' 'Alexander Dumfort' 'Holger Kopacka' 'Karl-Hans Ongania' 'Peter Brueggeller' #============================================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; Regioselective versus complete chalcogen transfer reactions of the bis(bidentate) phosphine cis,trans,cis-1,2,3,4-tetrakis(diphenyl- phosphino)cyclobutane: full characterization of new, hemilabile ligands and their complexes with palladiun(II) and platinum(II) ; #============================================================================ data_I _database_code_CSD 211317 _audit_creation_method SHELXL-97 _chemical_name_systematic 2,3-trans-dppcbS2 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H44 P4 S2' _chemical_formula_weight 856.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6057(2) _cell_length_b 13.0547(2) _cell_length_c 15.4843(2) _cell_angle_alpha 98.1899(9) _cell_angle_beta 107.8746(8) _cell_angle_gamma 109.6632(9) _cell_volume 2196.22(6) _cell_formula_units_Z 2 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 45216 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 1.10 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 218(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 'Kappa CCD' _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_% 0 _diffrn_reflns_number 17807 _diffrn_reflns_av_R_equivalents 0.0124 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5546 _reflns_number_gt 4915 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0654P)^2^+1.9755P] 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 5546 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P -0.63517(6) -0.17310(6) -0.32232(5) 0.03236(19) Uani 1 1 d . . . P2 P -0.64610(6) -0.30651(6) -0.14777(4) 0.02862(19) Uani 1 1 d . . . P3 P -0.94189(6) -0.24857(6) -0.14666(5) 0.03203(19) Uani 1 1 d . . . P4 P -1.03570(6) -0.31814(7) -0.40255(5) 0.0378(2) Uani 1 1 d . . . S1 S -0.52806(7) -0.15550(6) -0.06866(5) 0.0425(2) Uani 1 1 d . . . S2 S -1.08311(7) -0.39388(7) -0.20287(6) 0.0462(2) Uani 1 1 d . . . C1 C -0.7863(2) -0.2724(2) -0.32501(18) 0.0292(6) Uani 1 1 d . . . C2 C -0.7875(2) -0.3109(2) -0.23358(17) 0.0278(6) Uani 1 1 d . . . C3 C -0.8384(2) -0.2234(2) -0.20972(18) 0.0286(6) Uani 1 1 d . . . C4 C -0.8791(2) -0.2212(2) -0.31510(18) 0.0304(6) Uani 1 1 d . . . C11 C -0.6566(2) -0.0404(2) -0.3190(2) 0.0365(6) Uani 1 1 d . . . C12 C -0.6168(3) 0.0312(3) -0.2291(2) 0.0496(8) Uani 1 1 d . . . H12A H -0.5787 0.0115 -0.1764 0.060 Uiso 1 1 calc R . . C13 C -0.6333(4) 0.1302(3) -0.2174(3) 0.0713(11) Uani 1 1 d . . . H13A H -0.6087 0.1760 -0.1571 0.086 Uiso 1 1 calc R . . C14 C -0.6865(4) 0.1614(3) -0.2954(3) 0.0795(12) Uani 1 1 d . . . H14A H -0.6958 0.2294 -0.2878 0.095 Uiso 1 1 calc R . . C15 C -0.7251(4) 0.0928(4) -0.3833(3) 0.0701(11) Uani 1 1 d . . . H15A H -0.7601 0.1148 -0.4355 0.084 Uiso 1 1 calc R . . C16 C -0.7134(3) -0.0091(3) -0.3964(2) 0.0484(8) Uani 1 1 d . . . H16A H -0.7436 -0.0566 -0.4569 0.058 Uiso 1 1 calc R . . C21 C -0.6470(2) -0.2243(2) -0.44390(19) 0.0363(7) Uani 1 1 d . . . C22 C -0.5913(3) -0.1483(3) -0.4876(2) 0.0471(8) Uani 1 1 d . . . H22A H -0.5571 -0.0710 -0.4587 0.057 Uiso 1 1 calc R . . C23 C -0.5866(3) -0.1879(3) -0.5744(2) 0.0562(9) Uani 1 1 d . . . H23A H -0.5490 -0.1364 -0.6027 0.067 Uiso 1 1 calc R . . C24 C -0.6358(3) -0.2996(3) -0.6182(2) 0.0514(8) Uani 1 1 d . . . H24A H -0.6340 -0.3247 -0.6768 0.062 Uiso 1 1 calc R . . C25 C -0.6885(3) -0.3758(3) -0.5753(2) 0.0496(8) Uani 1 1 d . . . H25A H -0.7223 -0.4530 -0.6048 0.060 Uiso 1 1 calc R . . C26 C -0.6914(3) -0.3378(3) -0.4879(2) 0.0419(7) Uani 1 1 d . . . H26A H -0.7241 -0.3904 -0.4584 0.050 Uiso 1 1 calc R . . C31 C -0.5924(2) -0.3817(2) -0.22140(18) 0.0320(6) Uani 1 1 d . . . C32 C -0.6716(3) -0.4871(3) -0.2842(2) 0.0431(7) Uani 1 1 d . . . H32A H -0.7524 -0.5177 -0.2900 0.052 Uiso 1 1 calc R . . C33 C -0.6308(3) -0.5463(3) -0.3380(2) 0.0538(8) Uani 1 1 d . . . H33A H -0.6843 -0.6163 -0.3805 0.065 Uiso 1 1 calc R . . C34 C -0.5116(4) -0.5021(3) -0.3287(3) 0.0597(9) Uani 1 1 d . . . H34A H -0.4844 -0.5421 -0.3652 0.072 Uiso 1 1 calc R . . C35 C -0.4321(3) -0.3993(4) -0.2659(3) 0.0602(10) Uani 1 1 d . . . H35A H -0.3508 -0.3707 -0.2590 0.072 Uiso 1 1 calc R . . C36 C -0.4723(3) -0.3375(3) -0.2124(2) 0.0438(7) Uani 1 1 d . . . H36A H -0.4186 -0.2669 -0.1710 0.053 Uiso 1 1 calc R . . C41 C -0.6891(3) -0.4040(2) -0.07879(19) 0.0365(6) Uani 1 1 d . . . C42 C -0.7996(3) -0.4935(3) -0.1081(2) 0.0549(9) Uani 1 1 d . . . H42A H -0.8608 -0.5042 -0.1649 0.066 Uiso 1 1 calc R . . C43 C -0.8214(4) -0.5685(3) -0.0540(3) 0.0674(10) Uani 1 1 d . . . H43A H -0.8970 -0.6287 -0.0749 0.081 Uiso 1 1 calc R . . C44 C -0.7342(4) -0.5550(4) 0.0284(3) 0.0785(12) Uani 1 1 d . . . H44A H -0.7497 -0.6045 0.0650 0.094 Uiso 1 1 calc R . . C45 C -0.6240(5) -0.4687(5) 0.0572(3) 0.124(2) Uani 1 1 d . . . H45A H -0.5625 -0.4604 0.1130 0.149 Uiso 1 1 calc R . . C46 C -0.6014(4) -0.3920(4) 0.0045(3) 0.0938(16) Uani 1 1 d . . . H46A H -0.5257 -0.3318 0.0263 0.113 Uiso 1 1 calc R . . C51 C -0.8504(3) -0.2320(3) -0.02472(19) 0.0383(7) Uani 1 1 d . . . C52 C -0.8846(3) -0.3185(3) 0.0166(2) 0.0535(8) Uani 1 1 d . . . H52A H -0.9491 -0.3872 -0.0194 0.064 Uiso 1 1 calc R . . C53 C -0.8220(4) -0.3023(4) 0.1121(3) 0.0743(11) Uani 1 1 d . . . H53A H -0.8441 -0.3604 0.1401 0.089 Uiso 1 1 calc R . . C54 C -0.7273(4) -0.2003(4) 0.1649(3) 0.0783(12) Uani 1 1 d . . . H54A H -0.6871 -0.1890 0.2291 0.094 Uiso 1 1 calc R . . C55 C -0.6913(3) -0.1147(4) 0.1241(2) 0.0632(10) Uani 1 1 d . . . H55A H -0.6264 -0.0464 0.1604 0.076 Uiso 1 1 calc R . . C56 C -0.7515(3) -0.1301(3) 0.0296(2) 0.0449(7) Uani 1 1 d . . . H56A H -0.7263 -0.0727 0.0017 0.054 Uiso 1 1 calc R . . C61 C -0.9776(3) -0.1246(2) -0.13816(19) 0.0371(7) Uani 1 1 d . . . C62 C -0.8959(3) -0.0188(3) -0.1320(2) 0.0464(7) Uani 1 1 d . . . H62A H -0.8213 -0.0103 -0.1356 0.056 Uiso 1 1 calc R . . C63 C -0.9249(3) 0.0746(3) -0.1205(2) 0.0562(9) Uani 1 1 d . . . H63A H -0.8702 0.1454 -0.1169 0.067 Uiso 1 1 calc R . . C64 C -1.0354(4) 0.0615(3) -0.1145(2) 0.0596(9) Uani 1 1 d . . . H64A H -1.0547 0.1240 -0.1061 0.072 Uiso 1 1 calc R . . C65 C -1.1168(3) -0.0422(3) -0.1208(2) 0.0576(9) Uani 1 1 d . . . H65A H -1.1912 -0.0499 -0.1171 0.069 Uiso 1 1 calc R . . C66 C -1.0892(3) -0.1367(3) -0.1328(2) 0.0461(7) Uani 1 1 d . . . H66A H -1.1449 -0.2073 -0.1372 0.055 Uiso 1 1 calc R . . C71 C -1.1314(3) -0.2408(3) -0.39074(19) 0.0406(7) Uani 1 1 d . . . C72 C -1.0912(3) -0.1252(3) -0.3583(2) 0.0489(8) Uani 1 1 d . . . H72A H -1.0087 -0.0799 -0.3390 0.059 Uiso 1 1 calc R . . C73 C -1.1713(3) -0.0748(4) -0.3539(2) 0.0626(10) Uani 1 1 d . . . H73A H -1.1423 0.0034 -0.3321 0.075 Uiso 1 1 calc R . . C74 C -1.2924(4) -0.1402(4) -0.3816(3) 0.0678(11) Uani 1 1 d . . . H74A H -1.3457 -0.1066 -0.3774 0.081 Uiso 1 1 calc R . . C75 C -1.3353(3) -0.2542(4) -0.4151(3) 0.0677(11) Uani 1 1 d . . . H75A H -1.4183 -0.2982 -0.4357 0.081 Uiso 1 1 calc R . . C76 C -1.2553(3) -0.3060(3) -0.4190(2) 0.0523(8) Uani 1 1 d . . . H76A H -1.2851 -0.3843 -0.4405 0.063 Uiso 1 1 calc R . . C81 C -1.0138(2) -0.2901(3) -0.51118(19) 0.0404(7) Uani 1 1 d . . . C82 C -1.0319(3) -0.2042(3) -0.5479(2) 0.0564(9) Uani 1 1 d . . . H82A H -1.0522 -0.1529 -0.5154 0.068 Uiso 1 1 calc R . . C83 C -1.0199(4) -0.1934(4) -0.6326(3) 0.0705(11) Uani 1 1 d . . . H83A H -1.0350 -0.1367 -0.6576 0.085 Uiso 1 1 calc R . . C84 C -0.9862(3) -0.2655(4) -0.6796(3) 0.0660(10) Uani 1 1 d . . . H84A H -0.9759 -0.2563 -0.7353 0.079 Uiso 1 1 calc R . . C85 C -0.9676(3) -0.3510(3) -0.6452(2) 0.0576(9) Uani 1 1 d . . . H85A H -0.9443 -0.4000 -0.6771 0.069 Uiso 1 1 calc R . . C86 C -0.9836(3) -0.3645(3) -0.5628(2) 0.0477(8) Uani 1 1 d . . . H86A H -0.9740 -0.4249 -0.5411 0.057 Uiso 1 1 calc R . . H1 H -0.820(3) -0.336(3) -0.380(3) 0.070 Uiso 1 1 d . . . H2 H -0.846(4) -0.382(3) -0.252(3) 0.070 Uiso 1 1 d . . . H3 H -0.780(4) -0.160(3) -0.174(3) 0.070 Uiso 1 1 d . . . H4 H -0.868(3) -0.153(3) -0.325(3) 0.070 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0253(4) 0.0444(4) 0.0314(4) 0.0169(3) 0.0120(3) 0.0150(3) P2 0.0270(4) 0.0359(4) 0.0266(4) 0.0118(3) 0.0105(3) 0.0155(3) P3 0.0317(4) 0.0412(4) 0.0303(4) 0.0113(3) 0.0170(3) 0.0179(3) P4 0.0285(4) 0.0543(5) 0.0328(4) 0.0126(3) 0.0114(3) 0.0193(3) S1 0.0398(4) 0.0410(4) 0.0363(4) 0.0076(3) 0.0068(3) 0.0123(3) S2 0.0414(4) 0.0481(5) 0.0483(5) 0.0134(4) 0.0220(4) 0.0129(4) C1 0.0251(13) 0.0396(15) 0.0275(14) 0.0135(12) 0.0117(11) 0.0153(12) C2 0.0262(14) 0.0362(15) 0.0256(14) 0.0111(11) 0.0123(11) 0.0147(12) C3 0.0263(14) 0.0344(14) 0.0287(14) 0.0101(11) 0.0120(12) 0.0145(12) C4 0.0264(14) 0.0408(15) 0.0317(15) 0.0159(12) 0.0142(12) 0.0176(12) C11 0.0277(14) 0.0393(16) 0.0414(17) 0.0163(13) 0.0119(12) 0.0113(12) C12 0.0458(18) 0.0410(18) 0.0496(19) 0.0131(15) 0.0088(15) 0.0112(14) C13 0.082(3) 0.044(2) 0.072(3) 0.0049(18) 0.017(2) 0.0217(19) C14 0.105(3) 0.049(2) 0.099(3) 0.031(2) 0.042(3) 0.042(2) C15 0.083(3) 0.078(3) 0.080(3) 0.051(2) 0.037(2) 0.052(2) C16 0.0461(18) 0.057(2) 0.0495(19) 0.0269(16) 0.0174(15) 0.0251(16) C21 0.0273(14) 0.0548(19) 0.0362(15) 0.0213(14) 0.0161(12) 0.0205(13) C22 0.0482(18) 0.0514(18) 0.0415(17) 0.0157(14) 0.0231(15) 0.0132(15) C23 0.065(2) 0.066(2) 0.049(2) 0.0286(18) 0.0356(17) 0.0228(18) C24 0.065(2) 0.068(2) 0.0386(17) 0.0206(16) 0.0283(16) 0.0378(19) C25 0.057(2) 0.0563(19) 0.0505(19) 0.0169(16) 0.0287(16) 0.0321(16) C26 0.0455(17) 0.0489(18) 0.0489(18) 0.0246(15) 0.0292(15) 0.0250(14) C31 0.0343(15) 0.0439(16) 0.0312(14) 0.0203(13) 0.0158(12) 0.0244(13) C32 0.0430(17) 0.0460(18) 0.0466(18) 0.0120(14) 0.0237(14) 0.0197(14) C33 0.072(2) 0.0502(19) 0.056(2) 0.0151(16) 0.0356(18) 0.0331(18) C34 0.079(3) 0.074(2) 0.063(2) 0.027(2) 0.046(2) 0.054(2) C35 0.0465(19) 0.095(3) 0.068(2) 0.034(2) 0.0379(19) 0.043(2) C36 0.0354(16) 0.0586(19) 0.0457(17) 0.0206(15) 0.0194(14) 0.0227(15) C41 0.0411(16) 0.0461(17) 0.0327(15) 0.0184(13) 0.0177(13) 0.0233(14) C42 0.050(2) 0.060(2) 0.055(2) 0.0324(17) 0.0180(16) 0.0179(17) C43 0.067(2) 0.063(2) 0.077(3) 0.040(2) 0.036(2) 0.0170(19) C44 0.091(3) 0.091(3) 0.070(3) 0.059(2) 0.037(2) 0.035(3) C45 0.106(4) 0.140(5) 0.074(3) 0.080(3) -0.004(3) 0.003(4) C46 0.072(3) 0.105(3) 0.060(3) 0.053(2) -0.004(2) -0.003(2) C51 0.0418(16) 0.0551(18) 0.0333(15) 0.0146(14) 0.0211(13) 0.0306(15) C52 0.067(2) 0.064(2) 0.0461(19) 0.0263(16) 0.0293(17) 0.0348(18) C53 0.095(3) 0.097(3) 0.055(2) 0.044(2) 0.031(2) 0.055(3) C54 0.088(3) 0.113(4) 0.043(2) 0.027(2) 0.013(2) 0.059(3) C55 0.053(2) 0.090(3) 0.043(2) 0.0063(19) 0.0068(17) 0.041(2) C56 0.0422(17) 0.062(2) 0.0389(17) 0.0125(15) 0.0165(14) 0.0306(16) C61 0.0433(17) 0.0466(17) 0.0289(15) 0.0095(12) 0.0162(13) 0.0253(14) C62 0.0500(18) 0.0510(19) 0.0459(18) 0.0103(14) 0.0210(15) 0.0282(16) C63 0.072(2) 0.051(2) 0.054(2) 0.0131(16) 0.0255(18) 0.0330(18) C64 0.079(3) 0.070(2) 0.052(2) 0.0140(17) 0.0271(18) 0.055(2) C65 0.061(2) 0.080(3) 0.056(2) 0.0164(18) 0.0296(17) 0.050(2) C66 0.0460(18) 0.064(2) 0.0418(17) 0.0145(15) 0.0226(14) 0.0321(16) C71 0.0337(16) 0.067(2) 0.0299(15) 0.0209(14) 0.0137(12) 0.0266(15) C72 0.0409(17) 0.070(2) 0.0417(17) 0.0143(16) 0.0135(14) 0.0319(16) C73 0.066(3) 0.085(3) 0.051(2) 0.0182(18) 0.0196(18) 0.050(2) C74 0.063(3) 0.105(3) 0.069(2) 0.038(2) 0.032(2) 0.061(3) C75 0.0340(18) 0.113(4) 0.075(3) 0.048(2) 0.0267(18) 0.038(2) C76 0.0332(17) 0.077(2) 0.057(2) 0.0328(18) 0.0208(15) 0.0257(16) C81 0.0285(14) 0.0616(19) 0.0321(15) 0.0136(14) 0.0087(12) 0.0215(14) C82 0.064(2) 0.075(2) 0.051(2) 0.0272(18) 0.0306(17) 0.0413(19) C83 0.084(3) 0.095(3) 0.060(2) 0.045(2) 0.038(2) 0.049(2) C84 0.067(2) 0.098(3) 0.045(2) 0.029(2) 0.0321(18) 0.033(2) C85 0.050(2) 0.085(3) 0.0402(19) 0.0106(18) 0.0174(15) 0.0321(19) C86 0.0423(17) 0.066(2) 0.0354(17) 0.0103(15) 0.0113(14) 0.0271(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C11 1.837(3) . ? P1 C21 1.848(3) . ? P1 C1 1.894(3) . ? P2 C31 1.823(3) . ? P2 C41 1.826(3) . ? P2 C2 1.845(3) . ? P2 S1 1.9546(15) . ? P3 C61 1.818(3) . ? P3 C51 1.823(3) . ? P3 C3 1.830(3) . ? P3 S2 1.9575(15) . ? P4 C71 1.846(3) . ? P4 C81 1.852(3) . ? P4 C4 1.877(3) . ? C1 C4 1.564(4) . ? C1 C2 1.571(4) . ? C2 C3 1.540(4) . ? C3 C4 1.561(4) . ? C11 C16 1.387(4) . ? C11 C12 1.397(4) . ? C12 C13 1.372(5) . ? C13 C14 1.379(6) . ? C14 C15 1.358(6) . ? C15 C16 1.380(5) . ? C21 C26 1.376(4) . ? C21 C22 1.397(4) . ? C22 C23 1.396(5) . ? C23 C24 1.350(5) . ? C24 C25 1.373(5) . ? C25 C26 1.390(4) . ? C31 C36 1.381(4) . ? C31 C32 1.390(4) . ? C32 C33 1.380(4) . ? C33 C34 1.368(5) . ? C34 C35 1.370(5) . ? C35 C36 1.391(5) . ? C41 C46 1.364(5) . ? C41 C42 1.370(4) . ? C42 C43 1.389(5) . ? C43 C44 1.346(6) . ? C44 C45 1.349(7) . ? C45 C46 1.390(6) . ? C51 C52 1.384(4) . ? C51 C56 1.397(4) . ? C52 C53 1.392(5) . ? C53 C54 1.375(6) . ? C54 C55 1.375(6) . ? C55 C56 1.375(5) . ? C61 C62 1.387(4) . ? C61 C66 1.391(4) . ? C62 C63 1.389(5) . ? C63 C64 1.379(5) . ? C64 C65 1.364(5) . ? C65 C66 1.393(5) . ? C71 C72 1.379(5) . ? C71 C76 1.391(4) . ? C72 C73 1.390(5) . ? C73 C74 1.364(6) . ? C74 C75 1.358(6) . ? C75 C76 1.401(5) . ? C81 C82 1.381(5) . ? C81 C86 1.393(4) . ? C82 C83 1.387(5) . ? C83 C84 1.364(6) . ? C84 C85 1.361(6) . ? C85 C86 1.377(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 P1 C21 104.88(13) . . ? C11 P1 C1 101.54(12) . . ? C21 P1 C1 101.84(13) . . ? C31 P2 C41 102.01(12) . . ? C31 P2 C2 102.95(12) . . ? C41 P2 C2 107.67(13) . . ? C31 P2 S1 115.34(10) . . ? C41 P2 S1 112.63(10) . . ? C2 P2 S1 114.98(10) . . ? C61 P3 C51 102.94(13) . . ? C61 P3 C3 104.17(13) . . ? C51 P3 C3 106.69(12) . . ? C61 P3 S2 115.15(10) . . ? C51 P3 S2 112.49(11) . . ? C3 P3 S2 114.32(10) . . ? C71 P4 C81 100.49(13) . . ? C71 P4 C4 104.20(13) . . ? C81 P4 C4 98.16(13) . . ? C4 C1 C2 87.92(19) . . ? C4 C1 P1 117.78(19) . . ? C2 C1 P1 117.60(18) . . ? C3 C2 C1 88.38(19) . . ? C3 C2 P2 119.97(19) . . ? C1 C2 P2 119.85(17) . . ? C2 C3 C4 89.16(19) . . ? C2 C3 P3 120.98(19) . . ? C4 C3 P3 123.02(18) . . ? C3 C4 C1 87.88(19) . . ? C3 C4 P4 120.72(19) . . ? C1 C4 P4 109.17(19) . . ? C16 C11 C12 118.4(3) . . ? C16 C11 P1 126.0(2) . . ? C12 C11 P1 115.5(2) . . ? C13 C12 C11 120.9(3) . . ? C12 C13 C14 119.8(4) . . ? C15 C14 C13 119.9(4) . . ? C14 C15 C16 121.2(3) . . ? C15 C16 C11 119.8(3) . . ? C26 C21 C22 117.3(3) . . ? C26 C21 P1 121.8(2) . . ? C22 C21 P1 120.0(2) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 121.2(3) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 C26 120.0(3) . . ? C21 C26 C25 121.7(3) . . ? C36 C31 C32 119.5(3) . . ? C36 C31 P2 120.6(2) . . ? C32 C31 P2 119.8(2) . . ? C33 C32 C31 120.2(3) . . ? C34 C33 C32 120.0(3) . . ? C33 C34 C35 120.4(3) . . ? C34 C35 C36 120.4(3) . . ? C31 C36 C35 119.5(3) . . ? C46 C41 C42 117.8(3) . . ? C46 C41 P2 117.3(3) . . ? C42 C41 P2 124.7(2) . . ? C41 C42 C43 120.8(3) . . ? C44 C43 C42 120.7(4) . . ? C43 C44 C45 119.2(3) . . ? C44 C45 C46 120.7(4) . . ? C41 C46 C45 120.8(4) . . ? C52 C51 C56 119.6(3) . . ? C52 C51 P3 119.5(2) . . ? C56 C51 P3 120.8(2) . . ? C51 C52 C53 119.8(4) . . ? C54 C53 C52 119.7(4) . . ? C55 C54 C53 120.9(3) . . ? C54 C55 C56 119.9(4) . . ? C55 C56 C51 120.1(3) . . ? C62 C61 C66 119.4(3) . . ? C62 C61 P3 122.6(2) . . ? C66 C61 P3 117.9(2) . . ? C61 C62 C63 120.4(3) . . ? C64 C63 C62 119.5(3) . . ? C65 C64 C63 120.7(3) . . ? C64 C65 C66 120.4(3) . . ? C61 C66 C65 119.5(3) . . ? C72 C71 C76 117.8(3) . . ? C72 C71 P4 125.8(2) . . ? C76 C71 P4 116.4(3) . . ? C71 C72 C73 121.4(3) . . ? C74 C73 C72 120.0(4) . . ? C75 C74 C73 120.1(3) . . ? C74 C75 C76 120.4(3) . . ? C71 C76 C75 120.3(4) . . ? C82 C81 C86 117.2(3) . . ? C82 C81 P4 124.7(2) . . ? C86 C81 P4 118.0(2) . . ? C81 C82 C83 120.7(3) . . ? C84 C83 C82 120.4(4) . . ? C85 C84 C83 120.3(3) . . ? C84 C85 C86 119.5(3) . . ? C85 C86 C81 121.8(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 C11 P1 C1 C4 -5.2(2) . . . . ? C21 P1 C1 C4 -113.3(2) . . . . ? C11 P1 C1 C2 -108.5(2) . . . . ? C21 P1 C1 C2 143.5(2) . . . . ? C4 C1 C2 C3 -19.4(2) . . . . ? P1 C1 C2 C3 101.1(2) . . . . ? C4 C1 C2 P2 -143.4(2) . . . . ? P1 C1 C2 P2 -22.9(3) . . . . ? C31 P2 C2 C3 -158.1(2) . . . . ? C41 P2 C2 C3 94.7(2) . . . . ? S1 P2 C2 C3 -31.8(2) . . . . ? C31 P2 C2 C1 -51.0(2) . . . . ? C41 P2 C2 C1 -158.3(2) . . . . ? S1 P2 C2 C1 75.3(2) . . . . ? C1 C2 C3 C4 19.40(19) . . . . ? P2 C2 C3 C4 143.34(19) . . . . ? C1 C2 C3 P3 148.21(19) . . . . ? P2 C2 C3 P3 -87.8(2) . . . . ? C61 P3 C3 C2 -178.8(2) . . . . ? C51 P3 C3 C2 72.7(2) . . . . ? S2 P3 C3 C2 -52.3(2) . . . . ? C61 P3 C3 C4 -67.1(2) . . . . ? C51 P3 C3 C4 -175.6(2) . . . . ? S2 P3 C3 C4 59.4(2) . . . . ? C2 C3 C4 C1 -19.5(2) . . . . ? P3 C3 C4 C1 -146.7(2) . . . . ? C2 C3 C4 P4 91.6(2) . . . . ? P3 C3 C4 P4 -35.6(3) . . . . ? C2 C1 C4 C3 19.1(2) . . . . ? P1 C1 C4 C3 -101.2(2) . . . . ? C2 C1 C4 P4 -102.80(19) . . . . ? P1 C1 C4 P4 136.87(16) . . . . ? C71 P4 C4 C3 86.0(2) . . . . ? C81 P4 C4 C3 -170.9(2) . . . . ? C71 P4 C4 C1 -174.69(17) . . . . ? C81 P4 C4 C1 -71.6(2) . . . . ? C21 P1 C11 C16 21.7(3) . . . . ? C1 P1 C11 C16 -84.0(3) . . . . ? C21 P1 C11 C12 -162.0(2) . . . . ? C1 P1 C11 C12 92.3(2) . . . . ? C16 C11 C12 C13 -0.1(5) . . . . ? P1 C11 C12 C13 -176.8(3) . . . . ? C11 C12 C13 C14 -2.0(6) . . . . ? C12 C13 C14 C15 1.7(7) . . . . ? C13 C14 C15 C16 0.7(7) . . . . ? C14 C15 C16 C11 -2.8(6) . . . . ? C12 C11 C16 C15 2.5(5) . . . . ? P1 C11 C16 C15 178.8(3) . . . . ? C11 P1 C21 C26 -149.4(2) . . . . ? C1 P1 C21 C26 -43.9(3) . . . . ? C11 P1 C21 C22 41.9(3) . . . . ? C1 P1 C21 C22 147.4(2) . . . . ? C26 C21 C22 C23 2.7(4) . . . . ? P1 C21 C22 C23 171.9(3) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? C22 C23 C24 C25 -1.7(5) . . . . ? C23 C24 C25 C26 0.3(5) . . . . ? C22 C21 C26 C25 -4.2(4) . . . . ? P1 C21 C26 C25 -173.2(2) . . . . ? C24 C25 C26 C21 2.8(5) . . . . ? C41 P2 C31 C36 -115.8(2) . . . . ? C2 P2 C31 C36 132.7(2) . . . . ? S1 P2 C31 C36 6.6(2) . . . . ? C41 P2 C31 C32 61.3(2) . . . . ? C2 P2 C31 C32 -50.3(2) . . . . ? S1 P2 C31 C32 -176.34(19) . . . . ? C36 C31 C32 C33 -0.8(4) . . . . ? P2 C31 C32 C33 -177.8(2) . . . . ? C31 C32 C33 C34 0.9(5) . . . . ? C32 C33 C34 C35 0.3(5) . . . . ? C33 C34 C35 C36 -1.5(5) . . . . ? C32 C31 C36 C35 -0.4(4) . . . . ? P2 C31 C36 C35 176.6(2) . . . . ? C34 C35 C36 C31 1.6(5) . . . . ? C31 P2 C41 C46 89.6(3) . . . . ? C2 P2 C41 C46 -162.4(3) . . . . ? S1 P2 C41 C46 -34.6(4) . . . . ? C31 P2 C41 C42 -85.0(3) . . . . ? C2 P2 C41 C42 23.0(3) . . . . ? S1 P2 C41 C42 150.8(3) . . . . ? C46 C41 C42 C43 0.6(6) . . . . ? P2 C41 C42 C43 175.2(3) . . . . ? C41 C42 C43 C44 -0.1(6) . . . . ? C42 C43 C44 C45 -1.3(8) . . . . ? C43 C44 C45 C46 2.2(10) . . . . ? C42 C41 C46 C45 0.3(8) . . . . ? P2 C41 C46 C45 -174.6(5) . . . . ? C44 C45 C46 C41 -1.8(10) . . . . ? C61 P3 C51 C52 125.1(2) . . . . ? C3 P3 C51 C52 -125.5(2) . . . . ? S2 P3 C51 C52 0.6(3) . . . . ? C61 P3 C51 C56 -50.2(2) . . . . ? C3 P3 C51 C56 59.1(2) . . . . ? S2 P3 C51 C56 -174.75(19) . . . . ? C56 C51 C52 C53 1.4(5) . . . . ? P3 C51 C52 C53 -173.9(3) . . . . ? C51 C52 C53 C54 0.5(6) . . . . ? C52 C53 C54 C55 -1.7(6) . . . . ? C53 C54 C55 C56 0.9(6) . . . . ? C54 C55 C56 C51 1.1(5) . . . . ? C52 C51 C56 C55 -2.3(4) . . . . ? P3 C51 C56 C55 173.1(2) . . . . ? C51 P3 C61 C62 80.2(3) . . . . ? C3 P3 C61 C62 -31.1(3) . . . . ? S2 P3 C61 C62 -157.1(2) . . . . ? C51 P3 C61 C66 -96.4(2) . . . . ? C3 P3 C61 C66 152.3(2) . . . . ? S2 P3 C61 C66 26.3(3) . . . . ? C66 C61 C62 C63 0.1(4) . . . . ? P3 C61 C62 C63 -176.5(2) . . . . ? C61 C62 C63 C64 0.5(5) . . . . ? C62 C63 C64 C65 -0.7(5) . . . . ? C63 C64 C65 C66 0.4(5) . . . . ? C62 C61 C66 C65 -0.4(4) . . . . ? P3 C61 C66 C65 176.4(2) . . . . ? C64 C65 C66 C61 0.1(5) . . . . ? C81 P4 C71 C72 -76.6(3) . . . . ? C4 P4 C71 C72 24.7(3) . . . . ? C81 P4 C71 C76 102.1(2) . . . . ? C4 P4 C71 C76 -156.6(2) . . . . ? C76 C71 C72 C73 -0.1(4) . . . . ? P4 C71 C72 C73 178.7(2) . . . . ? C71 C72 C73 C74 0.3(5) . . . . ? C72 C73 C74 C75 -1.3(6) . . . . ? C73 C74 C75 C76 2.0(6) . . . . ? C72 C71 C76 C75 0.8(4) . . . . ? P4 C71 C76 C75 -178.1(3) . . . . ? C74 C75 C76 C71 -1.7(5) . . . . ? C71 P4 C81 C82 18.6(3) . . . . ? C4 P4 C81 C82 -87.6(3) . . . . ? C71 P4 C81 C86 -157.7(2) . . . . ? C4 P4 C81 C86 96.2(2) . . . . ? C86 C81 C82 C83 0.0(5) . . . . ? P4 C81 C82 C83 -176.3(3) . . . . ? C81 C82 C83 C84 -2.2(6) . . . . ? C82 C83 C84 C85 2.1(6) . . . . ? C83 C84 C85 C86 0.3(6) . . . . ? C84 C85 C86 C81 -2.6(5) . . . . ? C82 C81 C86 C85 2.4(5) . . . . ? P4 C81 C86 C85 178.9(2) . . . . ? _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction 0.990 _refine_diff_density_max 1.860 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.049 #===END data_II _database_code_CSD 211318 _audit_creation_method SHELXL-97 _chemical_name_systematic dppcbO4 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 O4 P4 x C7 H8' _chemical_formula_sum 'C59 H52 O4 P4' _chemical_formula_weight 948.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 31.5748(3) _cell_length_b 13.0352(1) _cell_length_c 24.7531(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10188.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 63312 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.924 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 223(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 'Kappa CCD' _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_% 0 _diffrn_reflns_number 43171 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.47 _reflns_number_total 14543 _reflns_number_gt 10328 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0568P)^2^+6.6721P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(6) _refine_ls_number_reflns 14543 _refine_ls_number_parameters 1216 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.271 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.02159(3) 0.70584(7) 0.29984(4) 0.0324(2) Uani 1 1 d . . . P2 P 0.08798(3) 0.43456(8) 0.24473(4) 0.0360(2) Uani 1 1 d . . . P3 P -0.02196(3) 0.35118(7) 0.25663(4) 0.0340(2) Uani 1 1 d . . . P4 P -0.03709(3) 0.62816(7) 0.17995(4) 0.0316(2) Uani 1 1 d . . . O1 O -0.01454(8) 0.6693(2) 0.33312(10) 0.0415(6) Uani 1 1 d . . . O2 O 0.08065(8) 0.4205(2) 0.18608(11) 0.0485(7) Uani 1 1 d . . . O3 O -0.00420(9) 0.2846(2) 0.21385(11) 0.0457(6) Uani 1 1 d . . . O4 O -0.06501(8) 0.69326(19) 0.21366(10) 0.0409(6) Uani 1 1 d . . . C1 C 0.03921(10) 0.6117(3) 0.24979(14) 0.0290(7) Uani 1 1 d . . . C2 C 0.04515(10) 0.5063(3) 0.27880(14) 0.0302(7) Uani 1 1 d . . . C3 C -0.00155(10) 0.4811(3) 0.26285(14) 0.0299(7) Uani 1 1 d . . . C4 C 0.00395(10) 0.5565(3) 0.21452(14) 0.0297(7) Uani 1 1 d . . . H1 H 0.0633(14) 0.636(3) 0.2289(17) 0.050 Uiso 1 1 d . . . H2 H 0.0505(12) 0.513(3) 0.3181(17) 0.050 Uiso 1 1 d . . . H3 H -0.0193(13) 0.513(3) 0.2890(17) 0.050 Uiso 1 1 d . . . H4 H 0.0192(13) 0.520(3) 0.1880(18) 0.050 Uiso 1 1 d . . . C11 C 0.01187(11) 0.8269(3) 0.26610(16) 0.0381(8) Uani 1 1 d . . . C12 C 0.03838(15) 0.8679(3) 0.22798(17) 0.0515(11) Uani 1 1 d . . . H12A H 0.0619 0.8309 0.2165 0.062 Uiso 1 1 calc R . . C13 C 0.03043(18) 0.9639(4) 0.2064(2) 0.0668(13) Uani 1 1 d . . . H13A H 0.0490 0.9922 0.1813 0.080 Uiso 1 1 calc R . . C14 C -0.0050(2) 1.0172(4) 0.2221(2) 0.0724(15) Uani 1 1 d . . . H14A H -0.0106 1.0813 0.2073 0.087 Uiso 1 1 calc R . . C15 C -0.03179(17) 0.9766(4) 0.2591(3) 0.0738(15) Uani 1 1 d . . . H15A H -0.0560 1.0128 0.2689 0.089 Uiso 1 1 calc R . . C16 C -0.02383(14) 0.8820(3) 0.2826(2) 0.0563(12) Uani 1 1 d . . . H16A H -0.0419 0.8557 0.3088 0.068 Uiso 1 1 calc R . . C21 C 0.06760(12) 0.7287(3) 0.34194(16) 0.0404(9) Uani 1 1 d . . . C22 C 0.06404(15) 0.7059(5) 0.39591(19) 0.0777(17) Uani 1 1 d . . . H22A H 0.0395 0.6748 0.4089 0.093 Uiso 1 1 calc R . . C23 C 0.0971(2) 0.7292(6) 0.4314(2) 0.098(2) Uani 1 1 d . . . H23A H 0.0946 0.7120 0.4678 0.118 Uiso 1 1 calc R . . C24 C 0.13249(17) 0.7764(4) 0.4134(2) 0.0672(15) Uani 1 1 d . . . H24A H 0.1536 0.7956 0.4376 0.081 Uiso 1 1 calc R . . C25 C 0.13690(18) 0.7951(5) 0.3605(3) 0.0857(19) Uani 1 1 d . . . H25A H 0.1620 0.8235 0.3477 0.103 Uiso 1 1 calc R . . C26 C 0.10450(18) 0.7726(5) 0.3248(3) 0.0843(19) Uani 1 1 d . . . H26A H 0.1079 0.7876 0.2884 0.101 Uiso 1 1 calc R . . C31 C 0.13551(11) 0.5115(3) 0.25585(19) 0.0485(10) Uani 1 1 d . . . C32 C 0.15407(16) 0.5280(5) 0.3050(3) 0.0878(18) Uani 1 1 d . . . H32A H 0.1421 0.5022 0.3365 0.105 Uiso 1 1 calc R . . C33 C 0.1916(2) 0.5848(6) 0.3065(4) 0.108(2) Uani 1 1 d . . . H33A H 0.2042 0.5970 0.3399 0.130 Uiso 1 1 calc R . . C34 C 0.21008(18) 0.6223(5) 0.2623(5) 0.120(3) Uani 1 1 d . . . H34A H 0.2358 0.6568 0.2645 0.144 Uiso 1 1 calc R . . C35 C 0.1902(2) 0.6088(4) 0.2134(4) 0.112(3) Uani 1 1 d . . . H35A H 0.2016 0.6386 0.1824 0.134 Uiso 1 1 calc R . . C36 C 0.15376(16) 0.5517(4) 0.2099(2) 0.0725(15) Uani 1 1 d . . . H36A H 0.1413 0.5401 0.1764 0.087 Uiso 1 1 calc R . . C41 C 0.09511(12) 0.3151(3) 0.28092(17) 0.0433(9) Uani 1 1 d . . . C42 C 0.09935(15) 0.3094(4) 0.3366(2) 0.0600(12) Uani 1 1 d . . . H42A H 0.0969 0.3687 0.3573 0.072 Uiso 1 1 calc R . . C43 C 0.10706(19) 0.2173(4) 0.3615(2) 0.0736(15) Uani 1 1 d . . . H43A H 0.1102 0.2146 0.3988 0.088 Uiso 1 1 calc R . . C44 C 0.11013(18) 0.1306(4) 0.3320(3) 0.0814(17) Uani 1 1 d . . . H44A H 0.1153 0.0685 0.3492 0.098 Uiso 1 1 calc R . . C45 C 0.10573(16) 0.1332(4) 0.2772(3) 0.0684(14) Uani 1 1 d . . . H45A H 0.1078 0.0729 0.2574 0.082 Uiso 1 1 calc R . . C46 C 0.09803(13) 0.2274(3) 0.2504(2) 0.0556(11) Uani 1 1 d . . . H46A H 0.0950 0.2298 0.2130 0.067 Uiso 1 1 calc R . . C51 C -0.01506(12) 0.2990(3) 0.32358(16) 0.0386(9) Uani 1 1 d . . . C52 C -0.02338(15) 0.3539(4) 0.37067(19) 0.0647(13) Uani 1 1 d . . . H52A H -0.0309 0.4228 0.3685 0.078 Uiso 1 1 calc R . . C53 C -0.0206(2) 0.3074(6) 0.4203(2) 0.094(2) Uani 1 1 d . . . H53A H -0.0265 0.3441 0.4517 0.112 Uiso 1 1 calc R . . C54 C -0.00853(19) 0.2026(5) 0.4232(2) 0.0859(19) Uani 1 1 d . . . H54A H -0.0075 0.1694 0.4564 0.103 Uiso 1 1 calc R . . C55 C 0.0014(2) 0.1519(5) 0.3781(3) 0.0853(18) Uani 1 1 d . . . H55A H 0.0105 0.0842 0.3803 0.102 Uiso 1 1 calc R . . C56 C -0.00175(17) 0.1988(4) 0.3279(2) 0.0611(13) Uani 1 1 d . . . H56A H 0.0052 0.1622 0.2969 0.073 Uiso 1 1 calc R . . C61 C -0.07889(11) 0.3654(3) 0.25008(15) 0.0382(8) Uani 1 1 d . . . C62 C -0.09999(14) 0.2912(4) 0.22043(19) 0.0549(11) Uani 1 1 d . . . H62A H -0.0845 0.2404 0.2029 0.066 Uiso 1 1 calc R . . C63 C -0.14353(16) 0.2912(5) 0.2164(2) 0.0732(15) Uani 1 1 d . . . H63A H -0.1574 0.2417 0.1959 0.088 Uiso 1 1 calc R . . C64 C -0.16639(14) 0.3661(5) 0.2433(2) 0.0753(15) Uani 1 1 d . . . H64A H -0.1958 0.3651 0.2421 0.090 Uiso 1 1 calc R . . C65 C -0.14606(13) 0.4416(4) 0.2718(2) 0.0620(12) Uani 1 1 d . . . H65A H -0.1616 0.4932 0.2885 0.074 Uiso 1 1 calc R . . C66 C -0.10251(12) 0.4410(3) 0.27569(17) 0.0477(10) Uani 1 1 d . . . H66A H -0.0888 0.4916 0.2956 0.057 Uiso 1 1 calc R . . C71 C -0.06710(11) 0.5382(3) 0.13965(14) 0.0355(8) Uani 1 1 d . . . C72 C -0.04944(13) 0.4586(4) 0.11119(19) 0.0588(12) Uani 1 1 d . . . H72A H -0.0205 0.4464 0.1132 0.071 Uiso 1 1 calc R . . C73 C -0.07480(17) 0.3963(4) 0.0794(2) 0.0762(16) Uani 1 1 d . . . H73A H -0.0626 0.3428 0.0600 0.091 Uiso 1 1 calc R . . C74 C -0.11818(16) 0.4126(4) 0.0762(2) 0.0705(14) Uani 1 1 d . . . H74A H -0.1350 0.3715 0.0542 0.085 Uiso 1 1 calc R . . C75 C -0.13557(14) 0.4894(4) 0.1056(2) 0.0690(15) Uani 1 1 d . . . H75A H -0.1647 0.4999 0.1046 0.083 Uiso 1 1 calc R . . C76 C -0.11071(13) 0.5516(4) 0.13700(18) 0.0522(11) Uani 1 1 d . . . H76A H -0.1233 0.6038 0.1569 0.063 Uiso 1 1 calc R . . C81 C -0.00543(12) 0.7011(3) 0.13262(14) 0.0341(8) Uani 1 1 d . . . C82 C 0.03063(15) 0.6638(3) 0.10756(18) 0.0534(11) Uani 1 1 d . . . H82A H 0.0389 0.5963 0.1134 0.064 Uiso 1 1 calc R . . C83 C 0.05461(18) 0.7260(4) 0.0738(2) 0.0672(14) Uani 1 1 d . . . H83A H 0.0791 0.7002 0.0579 0.081 Uiso 1 1 calc R . . C84 C 0.04227(16) 0.8261(3) 0.06372(18) 0.0558(11) Uani 1 1 d . . . H84A H 0.0580 0.8674 0.0405 0.067 Uiso 1 1 calc R . . C85 C 0.00685(15) 0.8634(3) 0.08825(18) 0.0541(11) Uani 1 1 d . . . H85A H -0.0012 0.9310 0.0822 0.065 Uiso 1 1 calc R . . C86 C -0.01739(14) 0.8021(3) 0.12219(17) 0.0471(10) Uani 1 1 d . . . H86A H -0.0417 0.8287 0.1380 0.056 Uiso 1 1 calc R . . P5 P 0.22888(3) 0.30919(7) -0.05484(4) 0.0323(2) Uani 1 1 d . . . P6 P 0.28767(3) 0.38801(7) 0.06241(4) 0.0325(2) Uani 1 1 d . . . P7 P 0.27323(3) 0.66365(7) -0.01779(4) 0.0368(2) Uani 1 1 d . . . P8 P 0.16335(3) 0.58618(7) 0.00028(4) 0.0339(2) Uani 1 1 d . . . O5 O 0.26719(8) 0.3413(2) -0.08611(11) 0.0411(6) Uani 1 1 d . . . O6 O 0.31615(8) 0.3232(2) 0.02951(10) 0.0422(6) Uani 1 1 d . . . O7 O 0.25644(10) 0.7353(2) 0.02344(13) 0.0522(7) Uani 1 1 d . . . O8 O 0.17416(8) 0.6104(2) 0.05699(10) 0.0425(6) Uani 1 1 d . . . C5 C 0.21115(10) 0.4049(3) -0.00518(14) 0.0305(7) Uani 1 1 d . . . C6 C 0.24663(10) 0.4615(3) 0.02791(14) 0.0287(7) Uani 1 1 d . . . C7 C 0.25108(11) 0.5349(3) -0.02157(15) 0.0329(8) Uani 1 1 d . . . C8 C 0.20380(10) 0.5105(3) -0.03512(15) 0.0306(7) Uani 1 1 d . . . H5 H 0.1864(13) 0.376(3) 0.0205(17) 0.050 Uiso 1 1 d . . . H6 H 0.2322(13) 0.498(3) 0.0559(18) 0.050 Uiso 1 1 d . . . H7 H 0.2671(13) 0.501(3) -0.0466(17) 0.050 Uiso 1 1 d . . . H8 H 0.1985(13) 0.512(3) -0.0710(17) 0.050 Uiso 1 1 d . . . C91 C 0.18464(12) 0.2920(3) -0.10041(16) 0.0387(9) Uani 1 1 d . . . C92 C 0.19374(17) 0.2931(4) -0.15414(18) 0.0645(13) Uani 1 1 d . . . H92A H 0.2215 0.3021 -0.1659 0.077 Uiso 1 1 calc R . . C93 C 0.16070(19) 0.2803(5) -0.1915(2) 0.0797(17) Uani 1 1 d . . . H93A H 0.1671 0.2812 -0.2282 0.096 Uiso 1 1 calc R . . C94 C 0.12052(19) 0.2671(4) -0.1766(2) 0.0722(16) Uani 1 1 d . . . H94A H 0.0993 0.2592 -0.2023 0.087 Uiso 1 1 calc R . . C95 C 0.11150(17) 0.2656(5) -0.1239(2) 0.0794(17) Uani 1 1 d . . . H95A H 0.0836 0.2562 -0.1131 0.095 Uiso 1 1 calc R . . C96 C 0.14271(14) 0.2775(4) -0.08446(19) 0.0630(13) Uani 1 1 d . . . H96A H 0.1356 0.2759 -0.0480 0.076 Uiso 1 1 calc R . . C101 C 0.23499(12) 0.1874(3) -0.02112(16) 0.0396(9) Uani 1 1 d . . . C102 C 0.27195(15) 0.1325(3) -0.0314(2) 0.0551(11) Uani 1 1 d . . . H10A H 0.2931 0.1611 -0.0529 0.066 Uiso 1 1 calc R . . C103 C 0.27717(19) 0.0360(4) -0.0100(2) 0.0737(15) Uani 1 1 d . . . H10B H 0.3018 -0.0006 -0.0172 0.088 Uiso 1 1 calc R . . C104 C 0.2473(2) -0.0058(4) 0.0212(2) 0.0778(17) Uani 1 1 d . . . H10C H 0.2512 -0.0716 0.0348 0.093 Uiso 1 1 calc R . . C105 C 0.2107(2) 0.0474(4) 0.0333(2) 0.0756(16) Uani 1 1 d . . . H10D H 0.1904 0.0186 0.0559 0.091 Uiso 1 1 calc R . . C106 C 0.20453(15) 0.1452(3) 0.01123(19) 0.0539(11) Uani 1 1 d . . . H10E H 0.1798 0.1813 0.0185 0.065 Uiso 1 1 calc R . . C111 C 0.25484(11) 0.3132(3) 0.10811(15) 0.0370(8) Uani 1 1 d . . . C112 C 0.21820(15) 0.3514(3) 0.13284(19) 0.0572(12) Uani 1 1 d . . . H11A H 0.2106 0.4198 0.1280 0.069 Uiso 1 1 calc R . . C113 C 0.19348(18) 0.2884(4) 0.1641(2) 0.0707(15) Uani 1 1 d . . . H11B H 0.1689 0.3140 0.1798 0.085 Uiso 1 1 calc R . . C114 C 0.20470(17) 0.1888(4) 0.17242(19) 0.0601(12) Uani 1 1 d . . . H11C H 0.1879 0.1469 0.1939 0.072 Uiso 1 1 calc R . . C115 C 0.23984(17) 0.1512(3) 0.14971(19) 0.0573(12) Uani 1 1 d . . . H11D H 0.2473 0.0831 0.1558 0.069 Uiso 1 1 calc R . . C116 C 0.26567(14) 0.2126(3) 0.11692(18) 0.0460(10) Uani 1 1 d . . . H11E H 0.2900 0.1854 0.1012 0.055 Uiso 1 1 calc R . . C121 C 0.31738(11) 0.4768(3) 0.10465(15) 0.0395(8) Uani 1 1 d . . . C122 C 0.30005(15) 0.5585(4) 0.1322(2) 0.0634(13) Uani 1 1 d . . . H12B H 0.2715 0.5741 0.1280 0.076 Uiso 1 1 calc R . . C123 C 0.32499(18) 0.6173(4) 0.1659(2) 0.0763(15) Uani 1 1 d . . . H12C H 0.3133 0.6732 0.1838 0.092 Uiso 1 1 calc R . . C124 C 0.36680(17) 0.5939(4) 0.1731(2) 0.0733(15) Uani 1 1 d . . . H12D H 0.3834 0.6329 0.1963 0.088 Uiso 1 1 calc R . . C125 C 0.38384(16) 0.5134(4) 0.1461(2) 0.0679(14) Uani 1 1 d . . . H12E H 0.4123 0.4976 0.1510 0.081 Uiso 1 1 calc R . . C126 C 0.35972(12) 0.4545(4) 0.11160(19) 0.0517(11) Uani 1 1 d . . . H12F H 0.3719 0.4000 0.0931 0.062 Uiso 1 1 calc R . . C131 C 0.32970(12) 0.6396(3) -0.01003(16) 0.0476(10) Uani 1 1 d . . . C132 C 0.35234(15) 0.7130(4) 0.0185(2) 0.0684(14) Uani 1 1 d . . . H13B H 0.3389 0.7697 0.0335 0.082 Uiso 1 1 calc R . . C133 C 0.39631(19) 0.6991(6) 0.0242(3) 0.0878(19) Uani 1 1 d . . . H13C H 0.4123 0.7487 0.0419 0.105 Uiso 1 1 calc R . . C134 C 0.41593(16) 0.6128(6) 0.0041(2) 0.0813(17) Uani 1 1 d . . . H13D H 0.4448 0.6029 0.0096 0.098 Uiso 1 1 calc R . . C135 C 0.39315(14) 0.5426(5) -0.0237(2) 0.0697(14) Uani 1 1 d . . . H13E H 0.4068 0.4858 -0.0383 0.084 Uiso 1 1 calc R . . C136 C 0.35036(12) 0.5538(4) -0.03064(18) 0.0523(11) Uani 1 1 d . . . H13F H 0.3351 0.5039 -0.0492 0.063 Uiso 1 1 calc R . . C141 C 0.26679(12) 0.7114(3) -0.08624(18) 0.0454(10) Uani 1 1 d . . . C142 C 0.27801(18) 0.6556(5) -0.13121(19) 0.0732(15) Uani 1 1 d . . . H14B H 0.2882 0.5890 -0.1276 0.088 Uiso 1 1 calc R . . C143 C 0.2740(2) 0.6993(6) -0.1819(2) 0.098(2) Uani 1 1 d . . . H14C H 0.2817 0.6614 -0.2122 0.118 Uiso 1 1 calc R . . C144 C 0.2596(2) 0.7935(6) -0.1884(3) 0.0872(19) Uani 1 1 d . . . H14D H 0.2575 0.8213 -0.2229 0.105 Uiso 1 1 calc R . . C145 C 0.2477(2) 0.8509(5) -0.1441(3) 0.093(2) Uani 1 1 d . . . H14E H 0.2374 0.9172 -0.1488 0.112 Uiso 1 1 calc R . . C146 C 0.25097(18) 0.8094(4) -0.0926(2) 0.0696(14) Uani 1 1 d . . . H14F H 0.2426 0.8473 -0.0627 0.084 Uiso 1 1 calc R . . C151 C 0.15321(11) 0.6976(3) -0.04117(17) 0.0408(9) Uani 1 1 d . . . C152 C 0.14742(15) 0.6924(3) -0.09693(18) 0.0531(11) Uani 1 1 d . . . H15B H 0.1507 0.6299 -0.1146 0.064 Uiso 1 1 calc R . . C153 C 0.13693(19) 0.7788(4) -0.1261(2) 0.0732(15) Uani 1 1 d . . . H15C H 0.1331 0.7747 -0.1633 0.088 Uiso 1 1 calc R . . C154 C 0.13220(19) 0.8715(4) -0.0998(3) 0.0830(17) Uani 1 1 d . . . H15D H 0.1245 0.9298 -0.1191 0.100 Uiso 1 1 calc R . . C155 C 0.13886(19) 0.8774(4) -0.0449(3) 0.0790(17) Uani 1 1 d . . . H15E H 0.1364 0.9403 -0.0275 0.095 Uiso 1 1 calc R . . C156 C 0.14916(14) 0.7913(3) -0.0154(2) 0.0545(11) Uani 1 1 d . . . H15F H 0.1534 0.7961 0.0217 0.065 Uiso 1 1 calc R . . C161 C 0.11574(10) 0.5076(3) -0.00161(15) 0.0367(8) Uani 1 1 d . . . C162 C 0.09187(13) 0.4877(4) -0.04729(18) 0.0542(11) Uani 1 1 d . . . H16B H 0.1004 0.5130 -0.0807 0.065 Uiso 1 1 calc R . . C163 C 0.05510(14) 0.4296(4) -0.0431(2) 0.0622(13) Uani 1 1 d . . . H16C H 0.0383 0.4184 -0.0734 0.075 Uiso 1 1 calc R . . C164 C 0.04364(13) 0.3892(3) 0.0052(2) 0.0583(12) Uani 1 1 d . . . H16D H 0.0194 0.3491 0.0075 0.070 Uiso 1 1 calc R . . C165 C 0.06682(14) 0.4062(3) 0.0500(2) 0.0544(11) Uani 1 1 d . . . H16E H 0.0584 0.3780 0.0828 0.065 Uiso 1 1 calc R . . C166 C 0.10286(13) 0.4650(3) 0.04761(16) 0.0469(9) Uani 1 1 d . . . H16F H 0.1187 0.4765 0.0787 0.056 Uiso 1 1 calc R . . C201 C 0.5613(2) 0.3636(4) 0.0646(3) 0.123(3) Uani 1 1 d G . . C202 C 0.5296(3) 0.3338(4) 0.1003(2) 0.148(4) Uani 1 1 d G . . C203 C 0.4875(2) 0.3340(4) 0.0837(3) 0.152(4) Uani 1 1 d G . . C204 C 0.4771(2) 0.3638(4) 0.0315(4) 0.159(5) Uani 1 1 d G . . C205 C 0.5088(4) 0.3936(4) -0.0042(3) 0.224(8) Uani 1 1 d G . . C206 C 0.5509(3) 0.3935(4) 0.0123(3) 0.169(5) Uiso 1 1 d G . . H20D H 0.5300 0.3143 0.1361 0.203 Uiso 1 1 calc G . . H20E H 0.4643 0.3158 0.1065 0.203 Uiso 1 1 d G . . H20F H 0.4573 0.3587 0.0219 0.203 Uiso 1 1 d G . . H20G H 0.4997 0.4161 -0.0400 0.203 Uiso 1 1 d G . . H20H H 0.5675 0.4136 -0.0106 0.203 Uiso 1 1 d G . . C207 C 0.5959(4) 0.3609(11) 0.0870(7) 0.233(7) Uani 1 1 d . . . H20A H 0.5939 0.3207 0.1194 0.350 Uiso 1 1 calc R . . H20B H 0.6047 0.4293 0.0960 0.350 Uiso 1 1 calc R . . H20C H 0.6164 0.3304 0.0632 0.350 Uiso 1 1 calc R . . C301 C 0.1870(2) 0.8653(5) 0.1715(3) 0.096(2) Uani 1 1 d . . . C302 C 0.1962(4) 0.9074(5) 0.2214(3) 0.134(4) Uani 1 1 d . . . H30D H 0.1749 0.9272 0.2451 0.160 Uiso 1 1 calc R . . C303 C 0.2419(4) 0.9196(6) 0.2356(4) 0.145(4) Uani 1 1 d . . . H30E H 0.2512 0.9488 0.2678 0.175 Uiso 1 1 calc R . . C304 C 0.2679(3) 0.8849(6) 0.1981(4) 0.114(3) Uani 1 1 d . . . H30F H 0.2966 0.8911 0.2059 0.137 Uiso 1 1 calc R . . C305 C 0.2590(3) 0.8428(5) 0.1514(3) 0.0933(19) Uani 1 1 d . . . H30G H 0.2804 0.8217 0.1281 0.112 Uiso 1 1 calc R . . C306 C 0.2189(2) 0.8315(5) 0.1385(3) 0.0893(18) Uani 1 1 d . . . H30H H 0.2120 0.7998 0.1060 0.107 Uiso 1 1 calc R . . C307 C 0.1439(3) 0.8466(10) 0.1524(5) 0.177(5) Uani 1 1 d . . . H30A H 0.1410 0.8721 0.1162 0.265 Uiso 1 1 calc R . . H30B H 0.1242 0.8812 0.1756 0.265 Uiso 1 1 calc R . . H30C H 0.1383 0.7743 0.1528 0.265 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 P1 0.0285(4) 0.0373(5) 0.0316(5) -0.0010(4) -0.0015(4) -0.0026(4) P2 0.0299(4) 0.0442(5) 0.0340(5) 0.0040(4) 0.0015(4) 0.0067(4) P3 0.0333(4) 0.0330(5) 0.0356(5) 0.0019(4) 0.0000(4) -0.0013(4) P4 0.0297(4) 0.0365(5) 0.0284(4) -0.0004(4) -0.0038(4) 0.0034(4) O1 0.0352(13) 0.0525(16) 0.0369(14) -0.0045(12) 0.0049(11) -0.0024(11) O2 0.0482(15) 0.0590(17) 0.0383(14) 0.0040(13) 0.0048(12) 0.0141(13) O3 0.0526(17) 0.0421(15) 0.0425(15) -0.0041(13) 0.0005(13) 0.0034(12) O4 0.0352(13) 0.0485(15) 0.0392(14) -0.0060(12) 0.0007(11) 0.0069(11) C1 0.0248(16) 0.0353(18) 0.0268(17) 0.0054(15) 0.0014(14) -0.0022(13) C2 0.0257(17) 0.038(2) 0.0264(17) 0.0043(15) -0.0013(14) 0.0000(14) C3 0.0280(16) 0.0312(18) 0.0305(19) 0.0010(15) -0.0037(15) -0.0011(14) C4 0.0262(16) 0.0327(18) 0.0303(18) 0.0015(15) -0.0061(14) 0.0014(14) C11 0.041(2) 0.0330(19) 0.040(2) -0.0017(16) -0.0089(17) -0.0023(16) C12 0.066(3) 0.048(2) 0.041(2) 0.0047(19) -0.007(2) -0.006(2) C13 0.091(4) 0.051(3) 0.059(3) 0.009(2) -0.011(3) -0.023(3) C14 0.105(4) 0.037(3) 0.076(4) 0.007(3) -0.029(3) 0.001(3) C15 0.071(3) 0.045(3) 0.105(4) -0.003(3) -0.013(3) 0.012(2) C16 0.048(2) 0.046(3) 0.075(3) -0.003(2) -0.006(2) -0.0024(19) C21 0.040(2) 0.049(2) 0.032(2) -0.0081(17) -0.0085(16) -0.0017(17) C22 0.045(3) 0.146(5) 0.042(3) 0.010(3) -0.007(2) -0.008(3) C23 0.083(4) 0.174(7) 0.038(3) -0.014(4) -0.017(3) 0.016(4) C24 0.055(3) 0.076(3) 0.070(4) -0.029(3) -0.027(3) 0.009(3) C25 0.057(3) 0.098(4) 0.102(5) 0.026(4) -0.040(3) -0.031(3) C26 0.065(3) 0.114(5) 0.075(4) 0.029(3) -0.031(3) -0.041(3) C31 0.0294(18) 0.044(2) 0.072(3) 0.002(2) 0.0067(19) 0.0043(16) C32 0.049(3) 0.122(5) 0.093(4) 0.011(4) -0.022(3) -0.025(3) C33 0.067(4) 0.114(5) 0.144(7) -0.005(5) -0.040(4) -0.021(4) C34 0.037(3) 0.085(5) 0.238(11) -0.019(6) 0.014(5) -0.019(3) C35 0.086(5) 0.059(4) 0.189(9) -0.014(5) 0.055(6) -0.020(3) C36 0.068(3) 0.059(3) 0.090(4) 0.000(3) 0.031(3) -0.005(2) C41 0.0329(19) 0.050(2) 0.046(2) 0.0043(19) -0.0026(17) 0.0080(17) C42 0.064(3) 0.060(3) 0.056(3) 0.010(2) -0.007(2) 0.013(2) C43 0.089(4) 0.073(4) 0.058(3) 0.021(3) -0.010(3) 0.015(3) C44 0.076(4) 0.060(3) 0.109(5) 0.030(3) -0.014(3) 0.013(3) C45 0.065(3) 0.043(3) 0.098(4) -0.010(3) -0.001(3) 0.005(2) C46 0.043(2) 0.053(3) 0.071(3) -0.007(2) -0.001(2) 0.0040(19) C51 0.035(2) 0.044(2) 0.037(2) 0.0067(17) 0.0013(16) -0.0024(17) C52 0.066(3) 0.078(3) 0.050(3) 0.009(2) 0.007(2) 0.027(3) C53 0.104(5) 0.136(6) 0.041(3) 0.018(3) 0.015(3) 0.043(4) C54 0.078(4) 0.119(5) 0.060(4) 0.049(4) 0.010(3) 0.032(4) C55 0.095(4) 0.079(4) 0.081(4) 0.038(3) 0.007(3) 0.018(3) C56 0.078(3) 0.048(3) 0.057(3) 0.014(2) 0.006(2) 0.006(2) C61 0.0360(19) 0.041(2) 0.038(2) 0.0103(17) -0.0034(16) -0.0057(16) C62 0.053(3) 0.057(3) 0.054(3) -0.001(2) -0.010(2) -0.012(2) C63 0.051(3) 0.087(4) 0.081(4) -0.005(3) -0.016(3) -0.019(3) C64 0.034(2) 0.113(4) 0.078(4) 0.017(3) -0.006(2) -0.008(3) C65 0.038(2) 0.080(3) 0.069(3) 0.014(3) 0.001(2) 0.011(2) C66 0.041(2) 0.051(2) 0.052(2) 0.007(2) -0.0001(18) 0.0003(18) C71 0.0327(18) 0.043(2) 0.0306(18) 0.0000(16) -0.0056(15) -0.0013(15) C72 0.043(2) 0.070(3) 0.064(3) -0.026(2) -0.008(2) 0.005(2) C73 0.066(3) 0.078(3) 0.085(4) -0.044(3) -0.010(3) 0.001(3) C74 0.059(3) 0.083(4) 0.070(3) -0.022(3) -0.019(2) -0.014(3) C75 0.036(2) 0.097(4) 0.075(3) -0.021(3) -0.009(2) -0.007(2) C76 0.038(2) 0.067(3) 0.052(3) -0.012(2) -0.0040(19) 0.003(2) C81 0.0374(19) 0.037(2) 0.0274(18) -0.0002(16) -0.0054(15) 0.0013(15) C82 0.064(3) 0.043(2) 0.054(3) 0.003(2) 0.020(2) 0.008(2) C83 0.067(3) 0.067(3) 0.067(3) 0.010(3) 0.027(3) 0.004(3) C84 0.072(3) 0.056(3) 0.039(2) 0.010(2) 0.003(2) -0.016(2) C85 0.066(3) 0.040(2) 0.057(3) 0.017(2) -0.015(2) -0.002(2) C86 0.049(2) 0.046(2) 0.046(2) 0.0081(19) -0.0092(19) 0.0063(18) P5 0.0297(4) 0.0331(5) 0.0341(5) -0.0013(4) -0.0015(4) 0.0002(4) P6 0.0276(4) 0.0376(5) 0.0325(5) -0.0012(4) -0.0025(4) 0.0016(4) P7 0.0374(5) 0.0358(5) 0.0372(5) 0.0017(4) 0.0017(4) -0.0073(4) P8 0.0299(4) 0.0366(5) 0.0351(5) -0.0003(4) 0.0004(4) 0.0033(4) O5 0.0332(13) 0.0459(15) 0.0440(15) -0.0063(12) 0.0060(11) 0.0016(11) O6 0.0374(13) 0.0485(16) 0.0408(15) -0.0069(12) -0.0003(11) 0.0047(12) O7 0.0609(18) 0.0414(16) 0.0543(18) -0.0060(13) 0.0090(15) -0.0069(14) O8 0.0384(13) 0.0502(15) 0.0389(14) -0.0052(12) 0.0008(11) 0.0043(11) C5 0.0252(16) 0.0336(18) 0.0325(19) 0.0001(15) 0.0013(15) -0.0019(14) C6 0.0272(17) 0.0270(18) 0.0318(18) -0.0001(14) -0.0043(14) 0.0010(14) C7 0.0317(18) 0.0307(18) 0.036(2) 0.0013(16) 0.0031(15) -0.0007(14) C8 0.0285(17) 0.0317(18) 0.0315(18) -0.0009(15) -0.0002(14) 0.0018(14) C91 0.037(2) 0.038(2) 0.041(2) -0.0022(17) -0.0070(17) 0.0003(16) C92 0.068(3) 0.085(4) 0.041(2) -0.004(2) -0.003(2) -0.023(3) C93 0.087(4) 0.113(5) 0.038(3) 0.006(3) -0.016(3) -0.030(3) C94 0.069(4) 0.082(4) 0.066(4) 0.003(3) -0.036(3) -0.011(3) C95 0.047(3) 0.121(5) 0.070(4) -0.010(3) -0.018(3) -0.009(3) C96 0.040(2) 0.109(4) 0.040(3) -0.010(3) -0.003(2) -0.003(2) C101 0.048(2) 0.0345(19) 0.037(2) -0.0049(17) -0.0115(17) -0.0015(16) C102 0.054(3) 0.044(2) 0.067(3) -0.005(2) -0.012(2) 0.0100(19) C103 0.093(4) 0.044(3) 0.084(4) -0.005(3) -0.021(3) 0.025(3) C104 0.121(5) 0.039(3) 0.074(4) 0.008(3) -0.031(4) 0.004(3) C105 0.116(5) 0.050(3) 0.060(3) 0.012(2) -0.005(3) -0.024(3) C106 0.058(3) 0.047(2) 0.057(3) 0.005(2) -0.007(2) -0.008(2) C111 0.0358(19) 0.045(2) 0.0304(19) -0.0019(16) -0.0029(16) -0.0056(16) C112 0.065(3) 0.044(2) 0.063(3) 0.008(2) 0.021(2) 0.012(2) C113 0.075(3) 0.075(4) 0.062(3) 0.009(3) 0.037(3) -0.002(3) C114 0.077(3) 0.055(3) 0.049(3) 0.013(2) 0.009(2) -0.011(2) C115 0.080(3) 0.039(2) 0.053(3) 0.011(2) -0.006(2) 0.000(2) C116 0.049(2) 0.041(2) 0.048(2) 0.0064(19) -0.008(2) 0.0067(18) C121 0.0392(19) 0.042(2) 0.037(2) 0.0017(17) -0.0053(16) -0.0055(17) C122 0.055(3) 0.068(3) 0.067(3) -0.030(3) -0.019(2) 0.008(2) C123 0.075(3) 0.076(4) 0.078(4) -0.029(3) -0.019(3) 0.003(3) C124 0.073(3) 0.078(4) 0.069(3) -0.017(3) -0.026(3) -0.023(3) C125 0.046(3) 0.080(4) 0.077(3) -0.003(3) -0.022(2) -0.016(2) C126 0.033(2) 0.056(3) 0.066(3) -0.007(2) -0.004(2) -0.0058(19) C131 0.039(2) 0.066(3) 0.039(2) 0.010(2) -0.0021(18) -0.0161(19) C132 0.054(3) 0.090(4) 0.062(3) -0.004(3) -0.006(2) -0.030(3) C133 0.066(4) 0.120(6) 0.078(4) 0.003(4) -0.028(3) -0.040(4) C134 0.044(3) 0.122(5) 0.078(4) 0.026(4) -0.011(3) -0.017(3) C135 0.040(2) 0.096(4) 0.074(3) 0.030(3) 0.005(2) 0.001(2) C136 0.034(2) 0.064(3) 0.059(3) 0.019(2) 0.0006(19) -0.0071(19) C141 0.033(2) 0.054(3) 0.049(2) 0.010(2) 0.0001(18) -0.0073(18) C142 0.089(4) 0.087(4) 0.044(3) 0.008(3) 0.008(3) 0.030(3) C143 0.112(5) 0.135(6) 0.048(3) 0.025(4) 0.007(3) 0.035(5) C144 0.087(4) 0.116(5) 0.058(4) 0.037(4) -0.004(3) -0.006(4) C145 0.118(5) 0.064(4) 0.097(5) 0.044(4) -0.016(4) -0.012(3) C146 0.095(4) 0.043(3) 0.070(3) 0.013(2) -0.005(3) -0.009(3) C151 0.0313(18) 0.040(2) 0.051(2) 0.0032(18) 0.0010(17) 0.0066(16) C152 0.065(3) 0.051(3) 0.043(2) 0.005(2) -0.013(2) 0.001(2) C153 0.094(4) 0.061(3) 0.065(3) 0.018(3) -0.017(3) 0.000(3) C154 0.089(4) 0.056(3) 0.105(5) 0.032(3) -0.014(3) 0.009(3) C155 0.094(4) 0.033(3) 0.109(5) -0.001(3) -0.007(3) 0.012(2) C156 0.060(3) 0.048(3) 0.056(3) -0.003(2) -0.003(2) 0.007(2) C161 0.0273(17) 0.0365(19) 0.046(2) 0.0019(16) -0.0001(16) 0.0058(14) C162 0.043(2) 0.074(3) 0.046(2) 0.017(2) -0.0088(18) -0.004(2) C163 0.042(2) 0.075(3) 0.070(3) 0.012(3) -0.017(2) -0.015(2) C164 0.033(2) 0.052(3) 0.090(4) 0.005(3) 0.004(2) -0.0064(18) C165 0.057(3) 0.047(2) 0.060(3) 0.006(2) 0.015(2) -0.007(2) C166 0.052(2) 0.048(2) 0.041(2) 0.0016(18) 0.0057(18) 0.0007(18) C201 0.121(6) 0.057(4) 0.191(9) -0.042(5) -0.013(7) 0.000(4) C202 0.178(9) 0.068(5) 0.197(10) -0.054(5) 0.105(9) -0.028(5) C203 0.213(11) 0.069(5) 0.175(10) -0.054(6) -0.038(9) 0.001(6) C204 0.276(14) 0.067(5) 0.134(8) -0.008(5) -0.063(9) 0.003(7) C205 0.45(3) 0.029(4) 0.196(12) -0.017(5) 0.054(15) 0.010(7) C207 0.188(13) 0.204(12) 0.307(19) -0.086(12) -0.077(13) 0.064(10) C301 0.100(5) 0.104(5) 0.084(5) 0.032(4) 0.029(4) 0.018(4) C302 0.287(13) 0.057(4) 0.057(4) 0.013(3) 0.064(6) 0.040(6) C303 0.240(12) 0.067(5) 0.129(8) 0.025(5) -0.079(9) -0.016(6) C304 0.182(9) 0.070(4) 0.091(5) 0.006(4) -0.030(6) 0.015(5) C305 0.120(6) 0.075(4) 0.085(5) 0.011(3) -0.012(4) 0.013(4) C306 0.107(5) 0.086(4) 0.075(4) 0.021(3) 0.024(4) 0.013(4) C307 0.100(6) 0.275(14) 0.155(9) 0.045(9) 0.010(6) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.485(3) . ? P1 C11 1.812(4) . ? P1 C21 1.813(4) . ? P1 C1 1.831(4) . ? P2 O2 1.482(3) . ? P2 C41 1.811(4) . ? P2 C31 1.825(4) . ? P2 C2 1.848(3) . ? P3 O3 1.480(3) . ? P3 C51 1.805(4) . ? P3 C61 1.814(4) . ? P3 C3 1.819(3) . ? P4 O4 1.481(3) . ? P4 C71 1.808(4) . ? P4 C81 1.810(4) . ? P4 C4 1.812(3) . ? C1 C2 1.561(5) . ? C1 C4 1.587(5) . ? C2 C3 1.561(5) . ? C3 C4 1.558(5) . ? C11 C12 1.370(6) . ? C11 C16 1.397(6) . ? C12 C13 1.384(6) . ? C13 C14 1.372(8) . ? C14 C15 1.354(8) . ? C15 C16 1.387(7) . ? C21 C26 1.365(7) . ? C21 C22 1.373(6) . ? C22 C23 1.397(8) . ? C23 C24 1.352(9) . ? C24 C25 1.340(8) . ? C25 C26 1.383(7) . ? C31 C32 1.367(7) . ? C31 C36 1.378(7) . ? C32 C33 1.398(8) . ? C33 C34 1.333(11) . ? C34 C35 1.375(12) . ? C35 C36 1.374(8) . ? C41 C46 1.373(6) . ? C41 C42 1.388(6) . ? C42 C43 1.371(7) . ? C43 C44 1.349(8) . ? C44 C45 1.363(8) . ? C45 C46 1.417(7) . ? C51 C56 1.377(6) . ? C51 C52 1.393(6) . ? C52 C53 1.374(7) . ? C53 C54 1.419(9) . ? C54 C55 1.335(9) . ? C55 C56 1.389(7) . ? C61 C62 1.385(6) . ? C61 C66 1.389(6) . ? C62 C63 1.379(6) . ? C63 C64 1.385(8) . ? C64 C65 1.370(7) . ? C65 C66 1.379(6) . ? C71 C72 1.373(6) . ? C71 C76 1.390(5) . ? C72 C73 1.385(6) . ? C73 C74 1.388(7) . ? C74 C75 1.354(7) . ? C75 C76 1.370(6) . ? C81 C82 1.385(6) . ? C81 C86 1.394(5) . ? C82 C83 1.389(6) . ? C83 C84 1.384(7) . ? C84 C85 1.362(7) . ? C85 C86 1.389(6) . ? P5 O5 1.496(3) . ? P5 C101 1.803(4) . ? P5 C91 1.810(4) . ? P5 C5 1.838(4) . ? P6 O6 1.478(3) . ? P6 C111 1.818(4) . ? P6 C121 1.820(4) . ? P6 C6 1.824(3) . ? P7 O7 1.482(3) . ? P7 C141 1.817(4) . ? P7 C131 1.820(4) . ? P7 C7 1.821(4) . ? P8 O8 1.479(3) . ? P8 C151 1.807(4) . ? P8 C161 1.820(4) . ? P8 C8 1.836(3) . ? C5 C6 1.572(5) . ? C5 C8 1.581(5) . ? C6 C7 1.561(5) . ? C7 C8 1.563(5) . ? C91 C92 1.361(6) . ? C91 C96 1.394(6) . ? C92 C93 1.404(7) . ? C93 C94 1.332(8) . ? C94 C95 1.337(8) . ? C95 C96 1.395(7) . ? C101 C106 1.367(6) . ? C101 C102 1.393(6) . ? C102 C103 1.376(7) . ? C103 C104 1.334(8) . ? C104 C105 1.382(8) . ? C105 C106 1.401(7) . ? C111 C116 1.372(6) . ? C111 C112 1.401(6) . ? C112 C113 1.372(6) . ? C113 C114 1.362(7) . ? C114 C115 1.337(7) . ? C115 C116 1.402(6) . ? C121 C122 1.378(6) . ? C121 C126 1.379(5) . ? C122 C123 1.380(6) . ? C123 C124 1.367(7) . ? C124 C125 1.355(8) . ? C125 C126 1.378(6) . ? C131 C132 1.388(6) . ? C131 C136 1.392(6) . ? C132 C133 1.407(8) . ? C133 C134 1.377(9) . ? C134 C135 1.352(8) . ? C135 C136 1.370(6) . ? C141 C142 1.376(7) . ? C141 C146 1.380(6) . ? C142 C143 1.384(7) . ? C143 C144 1.319(9) . ? C144 C145 1.379(9) . ? C145 C146 1.388(8) . ? C151 C156 1.383(6) . ? C151 C152 1.394(6) . ? C152 C153 1.378(6) . ? C153 C154 1.381(8) . ? C154 C155 1.377(9) . ? C155 C156 1.378(7) . ? C161 C162 1.384(5) . ? C161 C166 1.399(5) . ? C162 C163 1.390(6) . ? C163 C164 1.355(7) . ? C164 C165 1.346(7) . ? C165 C166 1.373(6) . ? C201 C207 1.229(13) . ? C201 C202 1.3900 . ? C201 C206 1.3900 . ? C202 C203 1.3900 . ? C203 C204 1.3900 . ? C204 C205 1.3900 . ? C205 C206 1.3900 . ? C301 C306 1.370(8) . ? C301 C302 1.382(10) . ? C301 C307 1.461(12) . ? C302 C303 1.493(13) . ? C303 C304 1.319(13) . ? C304 C305 1.309(10) . ? C305 C306 1.315(9) . ? 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 P1 C11 113.87(17) . . ? O1 P1 C21 110.45(17) . . ? C11 P1 C21 104.92(18) . . ? O1 P1 C1 113.20(15) . . ? C11 P1 C1 108.88(17) . . ? C21 P1 C1 104.82(17) . . ? O2 P2 C41 113.43(18) . . ? O2 P2 C31 110.13(19) . . ? C41 P2 C31 107.19(18) . . ? O2 P2 C2 113.29(15) . . ? C41 P2 C2 107.50(17) . . ? C31 P2 C2 104.77(17) . . ? O3 P3 C51 112.98(17) . . ? O3 P3 C61 111.82(18) . . ? C51 P3 C61 103.91(17) . . ? O3 P3 C3 118.21(17) . . ? C51 P3 C3 103.31(17) . . ? C61 P3 C3 105.27(16) . . ? O4 P4 C71 111.74(16) . . ? O4 P4 C81 113.11(16) . . ? C71 P4 C81 105.85(17) . . ? O4 P4 C4 117.07(16) . . ? C71 P4 C4 107.50(16) . . ? C81 P4 C4 100.47(16) . . ? C2 C1 C4 86.5(2) . . ? C2 C1 P1 108.4(2) . . ? C4 C1 P1 117.6(2) . . ? C1 C2 C3 87.4(2) . . ? C1 C2 P2 108.9(2) . . ? C3 C2 P2 118.0(2) . . ? C4 C3 C2 87.5(2) . . ? C4 C3 P3 124.2(2) . . ? C2 C3 P3 123.5(2) . . ? C3 C4 C1 86.7(2) . . ? C3 C4 P4 127.4(2) . . ? C1 C4 P4 121.8(2) . . ? C12 C11 C16 119.6(4) . . ? C12 C11 P1 123.6(3) . . ? C16 C11 P1 116.7(3) . . ? C11 C12 C13 120.5(5) . . ? C14 C13 C12 119.7(5) . . ? C15 C14 C13 120.2(4) . . ? C14 C15 C16 121.2(5) . . ? C15 C16 C11 118.7(5) . . ? C26 C21 C22 117.5(4) . . ? C26 C21 P1 125.1(4) . . ? C22 C21 P1 117.3(3) . . ? C21 C22 C23 120.3(5) . . ? C24 C23 C22 120.6(6) . . ? C25 C24 C23 119.4(5) . . ? C24 C25 C26 120.6(6) . . ? C21 C26 C25 121.5(6) . . ? C32 C31 C36 119.6(4) . . ? C32 C31 P2 125.0(4) . . ? C36 C31 P2 115.4(4) . . ? C31 C32 C33 118.2(6) . . ? C34 C33 C32 122.8(7) . . ? C33 C34 C35 118.5(6) . . ? C36 C35 C34 120.4(7) . . ? C35 C36 C31 120.4(7) . . ? C46 C41 C42 119.8(4) . . ? C46 C41 P2 116.8(3) . . ? C42 C41 P2 123.3(3) . . ? C43 C42 C41 120.7(5) . . ? C44 C43 C42 120.2(5) . . ? C43 C44 C45 120.7(5) . . ? C44 C45 C46 120.4(5) . . ? C41 C46 C45 118.3(5) . . ? C56 C51 C52 118.8(4) . . ? C56 C51 P3 117.7(3) . . ? C52 C51 P3 123.5(3) . . ? C53 C52 C51 120.7(5) . . ? C52 C53 C54 119.1(5) . . ? C55 C54 C53 119.8(5) . . ? C54 C55 C56 120.9(5) . . ? C51 C56 C55 120.5(5) . . ? C62 C61 C66 118.6(4) . . ? C62 C61 P3 116.9(3) . . ? C66 C61 P3 124.3(3) . . ? C63 C62 C61 121.2(5) . . ? C62 C63 C64 119.0(5) . . ? C65 C64 C63 120.7(4) . . ? C64 C65 C66 119.9(5) . . ? C65 C66 C61 120.5(4) . . ? C72 C71 C76 118.3(4) . . ? C72 C71 P4 124.1(3) . . ? C76 C71 P4 117.6(3) . . ? C71 C72 C73 120.0(4) . . ? C72 C73 C74 120.9(5) . . ? C75 C74 C73 118.9(4) . . ? C74 C75 C76 120.7(4) . . ? C75 C76 C71 121.3(4) . . ? C82 C81 C86 118.1(4) . . ? C82 C81 P4 124.0(3) . . ? C86 C81 P4 117.8(3) . . ? C81 C82 C83 120.9(4) . . ? C84 C83 C82 120.3(5) . . ? C85 C84 C83 119.1(4) . . ? C84 C85 C86 121.1(4) . . ? C85 C86 C81 120.4(4) . . ? O5 P5 C101 113.51(17) . . ? O5 P5 C91 109.65(17) . . ? C101 P5 C91 105.20(17) . . ? O5 P5 C5 113.75(15) . . ? C101 P5 C5 108.67(17) . . ? C91 P5 C5 105.41(16) . . ? O6 P6 C111 112.53(17) . . ? O6 P6 C121 111.49(16) . . ? C111 P6 C121 106.12(17) . . ? O6 P6 C6 118.31(16) . . ? C111 P6 C6 99.66(17) . . ? C121 P6 C6 107.53(17) . . ? O7 P7 C141 112.71(19) . . ? O7 P7 C131 112.73(19) . . ? C141 P7 C131 105.50(18) . . ? O7 P7 C7 118.63(17) . . ? C141 P7 C7 103.02(18) . . ? C131 P7 C7 102.88(18) . . ? O8 P8 C151 114.09(17) . . ? O8 P8 C161 109.60(16) . . ? C151 P8 C161 106.93(17) . . ? O8 P8 C8 114.04(16) . . ? C151 P8 C8 106.51(17) . . ? C161 P8 C8 105.07(16) . . ? C6 C5 C8 86.6(2) . . ? C6 C5 P5 116.7(2) . . ? C8 C5 P5 108.8(2) . . ? C7 C6 C5 86.7(2) . . ? C7 C6 P6 128.7(2) . . ? C5 C6 P6 120.3(2) . . ? C6 C7 C8 87.6(2) . . ? C6 C7 P7 124.0(3) . . ? C8 C7 P7 124.4(2) . . ? C7 C8 C5 86.3(2) . . ? C7 C8 P8 116.9(2) . . ? C5 C8 P8 110.3(2) . . ? C92 C91 C96 118.6(4) . . ? C92 C91 P5 116.4(3) . . ? C96 C91 P5 125.0(3) . . ? C91 C92 C93 119.0(5) . . ? C94 C93 C92 122.8(5) . . ? C93 C94 C95 118.3(5) . . ? C94 C95 C96 122.1(5) . . ? C91 C96 C95 119.2(4) . . ? C106 C101 C102 119.3(4) . . ? C106 C101 P5 123.4(3) . . ? C102 C101 P5 117.2(3) . . ? C103 C102 C101 120.0(5) . . ? C104 C103 C102 120.8(5) . . ? C103 C104 C105 120.9(5) . . ? C104 C105 C106 119.1(5) . . ? C101 C106 C105 119.9(5) . . ? C116 C111 C112 118.5(4) . . ? C116 C111 P6 118.0(3) . . ? C112 C111 P6 123.5(3) . . ? C113 C112 C111 120.2(4) . . ? C114 C113 C112 120.5(5) . . ? C115 C114 C113 120.2(4) . . ? C114 C115 C116 121.1(4) . . ? C111 C116 C115 119.5(4) . . ? C122 C121 C126 119.1(4) . . ? C122 C121 P6 124.8(3) . . ? C126 C121 P6 115.9(3) . . ? C121 C122 C123 120.1(4) . . ? C124 C123 C122 120.4(5) . . ? C125 C124 C123 119.5(4) . . ? C124 C125 C126 121.1(5) . . ? C125 C126 C121 119.7(4) . . ? C132 C131 C136 119.9(4) . . ? C132 C131 P7 116.1(4) . . ? C136 C131 P7 124.0(3) . . ? C131 C132 C133 118.1(6) . . ? C134 C133 C132 120.8(5) . . ? C135 C134 C133 119.8(5) . . ? C134 C135 C136 121.1(6) . . ? C135 C136 C131 120.1(5) . . ? C142 C141 C146 119.3(4) . . ? C142 C141 P7 123.0(3) . . ? C146 C141 P7 117.7(4) . . ? C141 C142 C143 119.5(5) . . ? C144 C143 C142 121.7(6) . . ? C143 C144 C145 120.1(6) . . ? C144 C145 C146 119.8(6) . . ? C141 C146 C145 119.5(6) . . ? C156 C151 C152 119.1(4) . . ? C156 C151 P8 117.7(3) . . ? C152 C151 P8 123.1(3) . . ? C153 C152 C151 120.7(5) . . ? C152 C153 C154 119.6(5) . . ? C155 C154 C153 119.8(5) . . ? C154 C155 C156 120.9(5) . . ? C155 C156 C151 119.8(5) . . ? C162 C161 C166 118.6(3) . . ? C162 C161 P8 125.2(3) . . ? C166 C161 P8 116.2(3) . . ? C161 C162 C163 119.7(4) . . ? C164 C163 C162 120.1(4) . . ? C165 C164 C163 121.1(4) . . ? C164 C165 C166 120.5(4) . . ? C165 C166 C161 120.0(4) . . ? C207 C201 C202 110.2(11) . . ? C207 C201 C206 129.8(11) . . ? C202 C201 C206 120.0 . . ? C203 C202 C201 120.0 . . ? C202 C203 C204 120.0 . . ? C205 C204 C203 120.0 . . ? C204 C205 C206 120.0 . . ? C205 C206 C201 120.0 . . ? C306 C301 C302 120.4(8) . . ? C306 C301 C307 115.9(8) . . ? C302 C301 C307 123.5(8) . . ? C301 C302 C303 117.1(8) . . ? C304 C303 C302 113.5(9) . . ? C305 C304 C303 129.2(10) . . ? C304 C305 C306 117.9(8) . . ? C305 C306 C301 121.8(7) . . ? 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 O1 P1 C1 C2 -49.3(3) . . . . ? C11 P1 C1 C2 -177.0(2) . . . . ? C21 P1 C1 C2 71.1(3) . . . . ? O1 P1 C1 C4 46.5(3) . . . . ? C11 P1 C1 C4 -81.3(3) . . . . ? C21 P1 C1 C4 166.9(3) . . . . ? C4 C1 C2 C3 -25.6(2) . . . . ? P1 C1 C2 C3 92.4(2) . . . . ? C4 C1 C2 P2 93.2(2) . . . . ? P1 C1 C2 P2 -148.87(17) . . . . ? O2 P2 C2 C1 -55.8(3) . . . . ? C41 P2 C2 C1 178.1(2) . . . . ? C31 P2 C2 C1 64.3(3) . . . . ? O2 P2 C2 C3 41.6(3) . . . . ? C41 P2 C2 C3 -84.6(3) . . . . ? C31 P2 C2 C3 161.6(3) . . . . ? C1 C2 C3 C4 26.0(2) . . . . ? P2 C2 C3 C4 -84.0(3) . . . . ? C1 C2 C3 P3 156.2(3) . . . . ? P2 C2 C3 P3 46.2(4) . . . . ? O3 P3 C3 C4 48.1(3) . . . . ? C51 P3 C3 C4 173.7(3) . . . . ? C61 P3 C3 C4 -77.6(3) . . . . ? O3 P3 C3 C2 -64.7(3) . . . . ? C51 P3 C3 C2 60.9(3) . . . . ? C61 P3 C3 C2 169.6(3) . . . . ? C2 C3 C4 C1 -25.6(2) . . . . ? P3 C3 C4 C1 -155.3(3) . . . . ? C2 C3 C4 P4 -154.0(3) . . . . ? P3 C3 C4 P4 76.4(4) . . . . ? C2 C1 C4 C3 25.6(2) . . . . ? P1 C1 C4 C3 -83.3(3) . . . . ? C2 C1 C4 P4 158.5(3) . . . . ? P1 C1 C4 P4 49.6(4) . . . . ? O4 P4 C4 C3 54.1(4) . . . . ? C71 P4 C4 C3 -72.6(3) . . . . ? C81 P4 C4 C3 177.0(3) . . . . ? O4 P4 C4 C1 -58.8(3) . . . . ? C71 P4 C4 C1 174.5(3) . . . . ? C81 P4 C4 C1 64.1(3) . . . . ? O1 P1 C11 C12 -171.0(3) . . . . ? C21 P1 C11 C12 68.1(4) . . . . ? C1 P1 C11 C12 -43.7(4) . . . . ? O1 P1 C11 C16 12.0(4) . . . . ? C21 P1 C11 C16 -108.8(3) . . . . ? C1 P1 C11 C16 139.4(3) . . . . ? C16 C11 C12 C13 1.0(6) . . . . ? P1 C11 C12 C13 -175.8(3) . . . . ? C11 C12 C13 C14 -1.9(7) . . . . ? C12 C13 C14 C15 0.7(8) . . . . ? C13 C14 C15 C16 1.3(8) . . . . ? C14 C15 C16 C11 -2.1(8) . . . . ? C12 C11 C16 C15 0.9(6) . . . . ? P1 C11 C16 C15 178.0(4) . . . . ? O1 P1 C21 C26 -172.8(5) . . . . ? C11 P1 C21 C26 -49.7(5) . . . . ? C1 P1 C21 C26 64.9(5) . . . . ? O1 P1 C21 C22 2.9(4) . . . . ? C11 P1 C21 C22 126.0(4) . . . . ? C1 P1 C21 C22 -119.3(4) . . . . ? C26 C21 C22 C23 1.2(9) . . . . ? P1 C21 C22 C23 -174.9(5) . . . . ? C21 C22 C23 C24 1.5(10) . . . . ? C22 C23 C24 C25 -4.1(10) . . . . ? C23 C24 C25 C26 4.1(10) . . . . ? C22 C21 C26 C25 -1.2(9) . . . . ? P1 C21 C26 C25 174.6(5) . . . . ? C24 C25 C26 C21 -1.5(11) . . . . ? O2 P2 C31 C32 -171.5(4) . . . . ? C41 P2 C31 C32 -47.7(5) . . . . ? C2 P2 C31 C32 66.3(5) . . . . ? O2 P2 C31 C36 6.3(4) . . . . ? C41 P2 C31 C36 130.2(3) . . . . ? C2 P2 C31 C36 -115.8(3) . . . . ? C36 C31 C32 C33 -0.8(8) . . . . ? P2 C31 C32 C33 177.0(5) . . . . ? C31 C32 C33 C34 -0.7(10) . . . . ? C32 C33 C34 C35 3.3(11) . . . . ? C33 C34 C35 C36 -4.5(11) . . . . ? C34 C35 C36 C31 3.2(9) . . . . ? C32 C31 C36 C35 -0.5(7) . . . . ? P2 C31 C36 C35 -178.5(4) . . . . ? O2 P2 C41 C46 7.4(4) . . . . ? C31 P2 C41 C46 -114.3(3) . . . . ? C2 P2 C41 C46 133.5(3) . . . . ? O2 P2 C41 C42 -175.2(4) . . . . ? C31 P2 C41 C42 63.0(4) . . . . ? C2 P2 C41 C42 -49.2(4) . . . . ? C46 C41 C42 C43 1.0(7) . . . . ? P2 C41 C42 C43 -176.3(4) . . . . ? C41 C42 C43 C44 -0.8(9) . . . . ? C42 C43 C44 C45 0.1(9) . . . . ? C43 C44 C45 C46 0.3(9) . . . . ? C42 C41 C46 C45 -0.5(6) . . . . ? P2 C41 C46 C45 176.9(3) . . . . ? C44 C45 C46 C41 -0.1(7) . . . . ? O3 P3 C51 C56 -11.3(4) . . . . ? C61 P3 C51 C56 110.1(4) . . . . ? C3 P3 C51 C56 -140.2(3) . . . . ? O3 P3 C51 C52 170.2(4) . . . . ? C61 P3 C51 C52 -68.4(4) . . . . ? C3 P3 C51 C52 41.3(4) . . . . ? C56 C51 C52 C53 -3.5(7) . . . . ? P3 C51 C52 C53 175.0(5) . . . . ? C51 C52 C53 C54 0.8(9) . . . . ? C52 C53 C54 C55 2.4(10) . . . . ? C53 C54 C55 C56 -2.9(10) . . . . ? C52 C51 C56 C55 3.0(7) . . . . ? P3 C51 C56 C55 -175.5(4) . . . . ? C54 C55 C56 C51 0.2(9) . . . . ? O3 P3 C61 C62 20.7(4) . . . . ? C51 P3 C61 C62 -101.5(3) . . . . ? C3 P3 C61 C62 150.2(3) . . . . ? O3 P3 C61 C66 -164.0(3) . . . . ? C51 P3 C61 C66 73.9(4) . . . . ? C3 P3 C61 C66 -34.4(4) . . . . ? C66 C61 C62 C63 -0.4(6) . . . . ? P3 C61 C62 C63 175.3(4) . . . . ? C61 C62 C63 C64 -1.1(8) . . . . ? C62 C63 C64 C65 2.6(8) . . . . ? C63 C64 C65 C66 -2.7(8) . . . . ? C64 C65 C66 C61 1.2(7) . . . . ? C62 C61 C66 C65 0.3(6) . . . . ? P3 C61 C66 C65 -175.0(3) . . . . ? O4 P4 C71 C72 -169.6(4) . . . . ? C81 P4 C71 C72 66.9(4) . . . . ? C4 P4 C71 C72 -39.8(4) . . . . ? O4 P4 C71 C76 11.2(4) . . . . ? C81 P4 C71 C76 -112.3(3) . . . . ? C4 P4 C71 C76 141.0(3) . . . . ? C76 C71 C72 C73 2.2(7) . . . . ? P4 C71 C72 C73 -177.0(4) . . . . ? C71 C72 C73 C74 -0.6(9) . . . . ? C72 C73 C74 C75 -1.4(9) . . . . ? C73 C74 C75 C76 1.6(9) . . . . ? C74 C75 C76 C71 0.0(8) . . . . ? C72 C71 C76 C75 -2.0(7) . . . . ? P4 C71 C76 C75 177.3(4) . . . . ? O4 P4 C81 C82 161.6(3) . . . . ? C71 P4 C81 C82 -75.7(4) . . . . ? C4 P4 C81 C82 36.0(4) . . . . ? O4 P4 C81 C86 -16.2(4) . . . . ? C71 P4 C81 C86 106.5(3) . . . . ? C4 P4 C81 C86 -141.8(3) . . . . ? C86 C81 C82 C83 1.2(7) . . . . ? P4 C81 C82 C83 -176.6(4) . . . . ? C81 C82 C83 C84 -1.3(8) . . . . ? C82 C83 C84 C85 1.4(8) . . . . ? C83 C84 C85 C86 -1.3(7) . . . . ? C84 C85 C86 C81 1.1(7) . . . . ? C82 C81 C86 C85 -1.1(6) . . . . ? P4 C81 C86 C85 176.9(3) . . . . ? O5 P5 C5 C6 -40.8(3) . . . . ? C101 P5 C5 C6 86.7(3) . . . . ? C91 P5 C5 C6 -160.9(3) . . . . ? O5 P5 C5 C8 55.0(3) . . . . ? C101 P5 C5 C8 -177.5(2) . . . . ? C91 P5 C5 C8 -65.2(3) . . . . ? C8 C5 C6 C7 -26.5(2) . . . . ? P5 C5 C6 C7 82.9(3) . . . . ? C8 C5 C6 P6 -160.3(3) . . . . ? P5 C5 C6 P6 -50.9(4) . . . . ? O6 P6 C6 C7 -50.9(4) . . . . ? C111 P6 C6 C7 -173.1(3) . . . . ? C121 P6 C6 C7 76.5(3) . . . . ? O6 P6 C6 C5 61.7(3) . . . . ? C111 P6 C6 C5 -60.5(3) . . . . ? C121 P6 C6 C5 -171.0(3) . . . . ? C5 C6 C7 C8 26.8(2) . . . . ? P6 C6 C7 C8 153.7(3) . . . . ? C5 C6 C7 P7 157.6(3) . . . . ? P6 C6 C7 P7 -75.4(4) . . . . ? O7 P7 C7 C6 -51.4(4) . . . . ? C141 P7 C7 C6 -176.6(3) . . . . ? C131 P7 C7 C6 73.8(3) . . . . ? O7 P7 C7 C8 62.3(4) . . . . ? C141 P7 C7 C8 -63.0(3) . . . . ? C131 P7 C7 C8 -172.5(3) . . . . ? C6 C7 C8 C5 -26.6(2) . . . . ? P7 C7 C8 C5 -157.2(3) . . . . ? C6 C7 C8 P8 84.3(3) . . . . ? P7 C7 C8 P8 -46.3(4) . . . . ? C6 C5 C8 C7 26.4(2) . . . . ? P5 C5 C8 C7 -90.7(2) . . . . ? C6 C5 C8 P8 -91.0(2) . . . . ? P5 C5 C8 P8 151.94(17) . . . . ? O8 P8 C8 C7 -36.8(3) . . . . ? C151 P8 C8 C7 90.0(3) . . . . ? C161 P8 C8 C7 -156.8(3) . . . . ? O8 P8 C8 C5 59.6(3) . . . . ? C151 P8 C8 C5 -173.7(2) . . . . ? C161 P8 C8 C5 -60.4(3) . . . . ? O5 P5 C91 C92 10.5(4) . . . . ? C101 P5 C91 C92 -111.9(4) . . . . ? C5 P5 C91 C92 133.3(3) . . . . ? O5 P5 C91 C96 -169.8(4) . . . . ? C101 P5 C91 C96 67.8(4) . . . . ? C5 P5 C91 C96 -47.0(4) . . . . ? C96 C91 C92 C93 0.4(7) . . . . ? P5 C91 C92 C93 -179.9(4) . . . . ? C91 C92 C93 C94 0.0(9) . . . . ? C92 C93 C94 C95 -0.3(10) . . . . ? C93 C94 C95 C96 0.2(10) . . . . ? C92 C91 C96 C95 -0.5(7) . . . . ? P5 C91 C96 C95 179.8(4) . . . . ? C94 C95 C96 C91 0.2(9) . . . . ? O5 P5 C101 C106 177.6(3) . . . . ? C91 P5 C101 C106 -62.5(4) . . . . ? C5 P5 C101 C106 50.0(4) . . . . ? O5 P5 C101 C102 -5.9(4) . . . . ? C91 P5 C101 C102 114.0(3) . . . . ? C5 P5 C101 C102 -133.5(3) . . . . ? C106 C101 C102 C103 1.2(6) . . . . ? P5 C101 C102 C103 -175.5(4) . . . . ? C101 C102 C103 C104 -0.5(8) . . . . ? C102 C103 C104 C105 -1.1(8) . . . . ? C103 C104 C105 C106 1.9(8) . . . . ? C102 C101 C106 C105 -0.3(6) . . . . ? P5 C101 C106 C105 176.1(3) . . . . ? C104 C105 C106 C101 -1.2(7) . . . . ? O6 P6 C111 C116 14.5(4) . . . . ? C121 P6 C111 C116 -107.7(3) . . . . ? C6 P6 C111 C116 140.8(3) . . . . ? O6 P6 C111 C112 -162.6(3) . . . . ? C121 P6 C111 C112 75.2(4) . . . . ? C6 P6 C111 C112 -36.4(4) . . . . ? C116 C111 C112 C113 -1.4(7) . . . . ? P6 C111 C112 C113 175.8(4) . . . . ? C111 C112 C113 C114 1.4(8) . . . . ? C112 C113 C114 C115 -0.5(9) . . . . ? C113 C114 C115 C116 -0.3(8) . . . . ? C112 C111 C116 C115 0.6(6) . . . . ? P6 C111 C116 C115 -176.7(3) . . . . ? C114 C115 C116 C111 0.3(7) . . . . ? O6 P6 C121 C122 167.8(4) . . . . ? C111 P6 C121 C122 -69.4(4) . . . . ? C6 P6 C121 C122 36.6(4) . . . . ? O6 P6 C121 C126 -16.7(4) . . . . ? C111 P6 C121 C126 106.2(3) . . . . ? C6 P6 C121 C126 -147.9(3) . . . . ? C126 C121 C122 C123 0.4(7) . . . . ? P6 C121 C122 C123 175.9(4) . . . . ? C121 C122 C123 C124 -1.3(8) . . . . ? C122 C123 C124 C125 1.1(9) . . . . ? C123 C124 C125 C126 -0.1(9) . . . . ? C124 C125 C126 C121 -0.7(8) . . . . ? C122 C121 C126 C125 0.6(7) . . . . ? P6 C121 C126 C125 -175.3(4) . . . . ? O7 P7 C131 C132 -21.5(4) . . . . ? C141 P7 C131 C132 101.9(4) . . . . ? C7 P7 C131 C132 -150.4(3) . . . . ? O7 P7 C131 C136 158.4(3) . . . . ? C141 P7 C131 C136 -78.2(4) . . . . ? C7 P7 C131 C136 29.4(4) . . . . ? C136 C131 C132 C133 1.9(7) . . . . ? P7 C131 C132 C133 -178.2(4) . . . . ? C131 C132 C133 C134 -2.8(8) . . . . ? C132 C133 C134 C135 3.0(9) . . . . ? C133 C134 C135 C136 -2.3(8) . . . . ? C134 C135 C136 C131 1.4(7) . . . . ? C132 C131 C136 C135 -1.3(6) . . . . ? P7 C131 C136 C135 178.9(3) . . . . ? O7 P7 C141 C142 -176.5(4) . . . . ? C131 P7 C141 C142 60.1(4) . . . . ? C7 P7 C141 C142 -47.5(4) . . . . ? O7 P7 C141 C146 5.3(4) . . . . ? C131 P7 C141 C146 -118.1(4) . . . . ? C7 P7 C141 C146 134.4(4) . . . . ? C146 C141 C142 C143 1.2(8) . . . . ? P7 C141 C142 C143 -176.9(5) . . . . ? C141 C142 C143 C144 -0.1(11) . . . . ? C142 C143 C144 C145 -0.6(12) . . . . ? C143 C144 C145 C146 0.2(11) . . . . ? C142 C141 C146 C145 -1.6(8) . . . . ? P7 C141 C146 C145 176.6(4) . . . . ? C144 C145 C146 C141 0.9(9) . . . . ? O8 P8 C151 C156 -10.8(4) . . . . ? C161 P8 C151 C156 110.5(3) . . . . ? C8 P8 C151 C156 -137.5(3) . . . . ? O8 P8 C151 C152 172.2(3) . . . . ? C161 P8 C151 C152 -66.4(4) . . . . ? C8 P8 C151 C152 45.5(4) . . . . ? C156 C151 C152 C153 -1.4(7) . . . . ? P8 C151 C152 C153 175.6(4) . . . . ? C151 C152 C153 C154 0.2(8) . . . . ? C152 C153 C154 C155 1.4(9) . . . . ? C153 C154 C155 C156 -1.7(9) . . . . ? C154 C155 C156 C151 0.5(8) . . . . ? C152 C151 C156 C155 1.0(7) . . . . ? P8 C151 C156 C155 -176.1(4) . . . . ? O8 P8 C161 C162 166.5(3) . . . . ? C151 P8 C161 C162 42.3(4) . . . . ? C8 P8 C161 C162 -70.6(4) . . . . ? O8 P8 C161 C166 -13.4(3) . . . . ? C151 P8 C161 C166 -137.6(3) . . . . ? C8 P8 C161 C166 109.5(3) . . . . ? C166 C161 C162 C163 2.4(6) . . . . ? P8 C161 C162 C163 -177.5(3) . . . . ? C161 C162 C163 C164 -2.7(7) . . . . ? C162 C163 C164 C165 1.6(8) . . . . ? C163 C164 C165 C166 -0.2(7) . . . . ? C164 C165 C166 C161 -0.1(6) . . . . ? C162 C161 C166 C165 -1.1(6) . . . . ? P8 C161 C166 C165 178.8(3) . . . . ? C207 C201 C202 C203 178.3(8) . . . . ? C206 C201 C202 C203 0.0 . . . . ? C201 C202 C203 C204 0.0 . . . . ? C202 C203 C204 C205 0.0 . . . . ? C203 C204 C205 C206 0.0 . . . . ? C204 C205 C206 C201 0.0 . . . . ? C207 C201 C206 C205 -177.9(9) . . . . ? C202 C201 C206 C205 0.0 . . . . ? C306 C301 C302 C303 3.5(9) . . . . ? C307 C301 C302 C303 178.7(8) . . . . ? C301 C302 C303 C304 -1.8(10) . . . . ? C302 C303 C304 C305 0.3(12) . . . . ? C303 C304 C305 C306 -0.4(12) . . . . ? C304 C305 C306 C301 2.1(9) . . . . ? C302 C301 C306 C305 -3.8(9) . . . . ? C307 C301 C306 C305 -179.3(7) . . . . ? _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction 0.990 _refine_diff_density_max 0.480 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.041 #===END data_III _database_code_CSD 211319 _audit_creation_method SHELXL-97 _chemical_name_systematic dppcbS4 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 P4 S4 x 0.5 C7 H8' _chemical_formula_sum 'C55.5 H48 P4 S4' _chemical_formula_weight 967.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 38.638(3) _cell_length_b 38.638(3) _cell_length_c 13.102(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19560(7) _cell_formula_units_Z 16 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'rectangular solid' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.55 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8080 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12402 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.5 _reflns_number_total 8402 _reflns_number_gt 4018 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Software of the Siemens P4' _computing_data_reduction 'Software of the Siemens P4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0589P)^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 8402 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.003 _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 S1 S 0.40569(3) 0.67423(3) -0.28015(10) 0.0541(3) Uani 1 1 d . . . S2 S 0.37230(3) 0.57519(3) -0.28784(9) 0.0440(3) Uani 1 1 d . . . S3 S 0.34307(3) 0.60646(3) 0.14603(9) 0.0519(3) Uani 1 1 d . . . S4 S 0.27322(3) 0.67333(3) 0.00571(10) 0.0526(3) Uani 1 1 d . . . P1 P 0.35550(3) 0.67557(3) -0.29650(9) 0.0370(3) Uani 1 1 d . . . P2 P 0.33221(2) 0.58455(2) -0.20275(8) 0.0309(2) Uani 1 1 d . . . P3 P 0.37903(3) 0.61929(2) 0.04957(9) 0.0357(3) Uani 1 1 d . . . P4 P 0.31814(3) 0.69659(2) 0.00426(9) 0.0369(3) Uani 1 1 d . . . C1 C 0.33054(9) 0.66282(9) -0.1815(3) 0.0291(9) Uani 1 1 d . . . C2 C 0.33281(9) 0.62564(9) -0.1326(3) 0.0291(9) Uani 1 1 d . . . C3 C 0.36431(9) 0.63835(9) -0.0700(3) 0.0300(9) Uani 1 1 d . . . C4 C 0.34983(9) 0.67635(9) -0.0826(3) 0.0310(9) Uani 1 1 d . . . C11 C 0.33963(11) 0.72002(10) -0.3213(3) 0.0424(10) Uani 1 1 d . . . C12 C 0.36316(13) 0.74385(12) -0.3586(4) 0.0621(14) Uani 1 1 d . . . H12A H 0.3864 0.7379 -0.3644 0.075 Uiso 1 1 calc R . . C13 C 0.35181(17) 0.77739(13) -0.3879(4) 0.0785(17) Uani 1 1 d . . . H13A H 0.3673 0.7935 -0.4140 0.094 Uiso 1 1 calc R . . C14 C 0.31706(16) 0.78553(13) -0.3765(4) 0.0735(16) Uani 1 1 d . . . H14A H 0.3093 0.8075 -0.3946 0.088 Uiso 1 1 calc R . . C15 C 0.29450(14) 0.76227(12) -0.3398(4) 0.0630(14) Uani 1 1 d . . . H15A H 0.2713 0.7682 -0.3331 0.076 Uiso 1 1 calc R . . C16 C 0.30536(11) 0.72948(10) -0.3119(3) 0.0497(12) Uani 1 1 d . . . H16A H 0.2894 0.7137 -0.2866 0.060 Uiso 1 1 calc R . . C21 C 0.34015(10) 0.65186(9) -0.4073(3) 0.0347(9) Uani 1 1 d . . . C22 C 0.36403(11) 0.63702(11) -0.4738(3) 0.0480(11) Uani 1 1 d . . . H22A H 0.3876 0.6383 -0.4592 0.058 Uiso 1 1 calc R . . C23 C 0.35310(13) 0.62057(12) -0.5604(4) 0.0584(13) Uani 1 1 d . . . H23A H 0.3693 0.6110 -0.6046 0.070 Uiso 1 1 calc R . . C24 C 0.31827(13) 0.61795(11) -0.5831(4) 0.0555(12) Uani 1 1 d . . . H24A H 0.3110 0.6066 -0.6419 0.067 Uiso 1 1 calc R . . C25 C 0.29426(11) 0.63242(10) -0.5172(3) 0.0456(11) Uani 1 1 d . . . H25A H 0.2708 0.6309 -0.5322 0.055 Uiso 1 1 calc R . . C26 C 0.30495(10) 0.64919(9) -0.4293(3) 0.0394(10) Uani 1 1 d . . . H26A H 0.2887 0.6586 -0.3850 0.047 Uiso 1 1 calc R . . C31 C 0.29102(9) 0.58484(9) -0.2703(3) 0.0319(9) Uani 1 1 d . . . C32 C 0.28757(11) 0.56323(10) -0.3547(3) 0.0426(10) Uani 1 1 d . . . H32A H 0.3062 0.5499 -0.3763 0.051 Uiso 1 1 calc R . . C33 C 0.25649(12) 0.56153(12) -0.4064(4) 0.0554(13) Uani 1 1 d . . . H33A H 0.2541 0.5469 -0.4623 0.066 Uiso 1 1 calc R . . C34 C 0.22876(12) 0.58168(12) -0.3748(4) 0.0575(13) Uani 1 1 d . . . H34A H 0.2081 0.5811 -0.4114 0.069 Uiso 1 1 calc R . . C35 C 0.23150(10) 0.60244(11) -0.2900(4) 0.0473(11) Uani 1 1 d . . . H35A H 0.2126 0.6152 -0.2677 0.057 Uiso 1 1 calc R . . C36 C 0.26252(9) 0.60420(9) -0.2380(3) 0.0375(10) Uani 1 1 d . . . H36A H 0.2645 0.6184 -0.1810 0.045 Uiso 1 1 calc R . . C41 C 0.32522(9) 0.55218(8) -0.1045(3) 0.0311(9) Uani 1 1 d . . . C42 C 0.34764(11) 0.52440(9) -0.0967(3) 0.0448(11) Uani 1 1 d . . . H42A H 0.3665 0.5228 -0.1405 0.054 Uiso 1 1 calc R . . C43 C 0.34219(13) 0.49928(11) -0.0247(4) 0.0622(14) Uani 1 1 d . . . H43A H 0.3576 0.4809 -0.0193 0.075 Uiso 1 1 calc R . . C44 C 0.31396(13) 0.50094(11) 0.0403(4) 0.0575(13) Uani 1 1 d . . . H44A H 0.3103 0.4835 0.0881 0.069 Uiso 1 1 calc R . . C45 C 0.29127(12) 0.52837(11) 0.0342(3) 0.0515(12) Uani 1 1 d . . . H45A H 0.2726 0.5299 0.0788 0.062 Uiso 1 1 calc R . . C46 C 0.29659(11) 0.55368(10) -0.0390(3) 0.0467(11) Uani 1 1 d . . . H46A H 0.2810 0.5719 -0.0448 0.056 Uiso 1 1 calc R . . C51 C 0.40713(9) 0.58357(9) 0.0139(3) 0.0347(9) Uani 1 1 d . . . C52 C 0.43044(11) 0.58514(10) -0.0666(4) 0.0478(11) Uani 1 1 d . . . H52A H 0.4309 0.6047 -0.1081 0.057 Uiso 1 1 calc R . . C53 C 0.45295(11) 0.55811(11) -0.0860(4) 0.0513(12) Uani 1 1 d . . . H53A H 0.4685 0.5597 -0.1400 0.062 Uiso 1 1 calc R . . C54 C 0.45247(12) 0.52906(11) -0.0261(4) 0.0551(13) Uani 1 1 d . . . H54A H 0.4674 0.5108 -0.0399 0.066 Uiso 1 1 calc R . . C55 C 0.42976(14) 0.52701(11) 0.0545(4) 0.0699(15) Uani 1 1 d . . . H55A H 0.4296 0.5074 0.0959 0.084 Uiso 1 1 calc R . . C56 C 0.40703(12) 0.55406(11) 0.0745(4) 0.0566(13) Uani 1 1 d . . . H56A H 0.3916 0.5524 0.1289 0.068 Uiso 1 1 calc R . . C61 C 0.40998(10) 0.65126(10) 0.0967(4) 0.0456(11) Uani 1 1 d . . . C62 C 0.42933(10) 0.67204(10) 0.0324(4) 0.0552(13) Uani 1 1 d . . . H62A H 0.4258 0.6709 -0.0377 0.066 Uiso 1 1 calc R . . C63 C 0.45397(12) 0.69454(13) 0.0719(6) 0.0798(19) Uani 1 1 d . . . H63A H 0.4669 0.7086 0.0286 0.096 Uiso 1 1 calc R . . C64 C 0.45909(15) 0.69578(15) 0.1754(7) 0.091(2) Uani 1 1 d . . . H64A H 0.4756 0.7108 0.2019 0.109 Uiso 1 1 calc R . . C65 C 0.44027(16) 0.67523(15) 0.2411(5) 0.090(2) Uani 1 1 d . . . H65A H 0.4440 0.6762 0.3112 0.108 Uiso 1 1 calc R . . C66 C 0.41555(13) 0.65289(12) 0.2001(4) 0.0664(15) Uani 1 1 d . . . H66A H 0.4026 0.6389 0.2435 0.080 Uiso 1 1 calc R . . C71 C 0.33605(9) 0.70435(9) 0.1311(3) 0.0352(10) Uani 1 1 d . . . C72 C 0.36460(10) 0.72659(10) 0.1445(3) 0.0423(10) Uani 1 1 d . . . H72A H 0.3761 0.7357 0.0881 0.051 Uiso 1 1 calc R . . C73 C 0.37540(12) 0.73467(11) 0.2421(4) 0.0520(12) Uani 1 1 d . . . H73A H 0.3945 0.7490 0.2515 0.062 Uiso 1 1 calc R . . C74 C 0.35800(12) 0.72163(11) 0.3262(4) 0.0553(12) Uani 1 1 d . . . H74A H 0.3652 0.7274 0.3918 0.066 Uiso 1 1 calc R . . C75 C 0.33013(12) 0.70013(11) 0.3126(4) 0.0552(13) Uani 1 1 d . . . H75A H 0.3184 0.6914 0.3691 0.066 Uiso 1 1 calc R . . C76 C 0.31931(10) 0.69131(10) 0.2151(3) 0.0429(11) Uani 1 1 d . . . H76A H 0.3006 0.6765 0.2066 0.051 Uiso 1 1 calc R . . C81 C 0.31510(11) 0.74101(10) -0.0460(3) 0.0463(11) Uani 1 1 d . . . C82 C 0.34249(13) 0.75925(10) -0.0892(4) 0.0547(12) Uani 1 1 d . . . H82A H 0.3636 0.7482 -0.0995 0.066 Uiso 1 1 calc R . . C83 C 0.33869(16) 0.79360(12) -0.1170(4) 0.0752(17) Uani 1 1 d . . . H83A H 0.3572 0.8056 -0.1454 0.090 Uiso 1 1 calc R . . C84 C 0.3082(2) 0.80964(15) -0.1030(5) 0.101(3) Uani 1 1 d . . . H84A H 0.3058 0.8327 -0.1226 0.121 Uiso 1 1 calc R . . C85 C 0.28040(19) 0.79253(16) -0.0599(5) 0.094(2) Uani 1 1 d . . . H85A H 0.2595 0.8040 -0.0497 0.113 Uiso 1 1 calc R . . C86 C 0.28385(13) 0.75778(12) -0.0319(4) 0.0645(15) Uani 1 1 d . . . H86A H 0.2652 0.7460 -0.0038 0.077 Uiso 1 1 calc R . . C91 C 0.5024(9) 0.7600(5) -0.2226(15) 0.101(7) Uani 0.50 1 d P . . C92 C 0.4791(5) 0.7306(7) -0.2031(16) 0.086(6) Uani 0.50 1 d P . . C93 C 0.4950(8) 0.6985(8) -0.201(2) 0.094(7) Uani 0.50 1 d P . . C94 C 0.5266(5) 0.6923(4) -0.2230(15) 0.084(5) Uani 0.50 1 d P . . C95 C 0.5474(3) 0.7186(5) -0.2508(11) 0.091(4) Uani 0.50 1 d P . . C96 C 0.5362(4) 0.7522(4) -0.2446(11) 0.087(4) Uani 0.50 1 d P . . C97 C 0.4891(15) 0.7980(9) -0.232(4) 0.21(3) Uani 0.50 1 d P . . H1 H 0.3068(11) 0.6703(10) -0.190(3) 0.060 Uiso 1 1 d . . . H2 H 0.3138(10) 0.6258(10) -0.087(3) 0.060 Uiso 1 1 d . . . H3 H 0.3839(10) 0.6373(10) -0.114(3) 0.060 Uiso 1 1 d . . . H4 H 0.3668(10) 0.6919(10) -0.098(3) 0.060 Uiso 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 S1 0.0313(6) 0.0646(7) 0.0663(9) 0.0081(7) 0.0048(6) -0.0080(5) S2 0.0364(5) 0.0443(6) 0.0513(7) 0.0009(5) 0.0091(5) 0.0040(5) S3 0.0575(7) 0.0521(7) 0.0462(7) 0.0031(6) 0.0076(6) 0.0052(6) S4 0.0309(5) 0.0567(7) 0.0703(8) -0.0199(6) 0.0083(6) -0.0043(5) P1 0.0309(5) 0.0342(6) 0.0458(7) 0.0095(5) 0.0040(5) -0.0035(4) P2 0.0301(5) 0.0244(5) 0.0382(6) 0.0005(5) 0.0027(5) 0.0002(4) P3 0.0359(5) 0.0293(5) 0.0419(7) -0.0007(5) -0.0058(5) 0.0032(4) P4 0.0309(5) 0.0288(5) 0.0509(7) -0.0061(5) -0.0007(5) 0.0014(4) C1 0.0278(19) 0.0212(18) 0.038(2) 0.0042(17) 0.0021(18) 0.0016(15) C2 0.0257(19) 0.0234(18) 0.038(2) 0.0031(17) 0.0067(17) -0.0019(15) C3 0.0260(19) 0.0218(17) 0.042(3) -0.0008(18) 0.0004(18) 0.0001(15) C4 0.0230(19) 0.0219(18) 0.048(3) 0.0000(18) -0.0029(18) -0.0058(15) C11 0.055(3) 0.032(2) 0.040(3) 0.0033(19) 0.000(2) -0.006(2) C12 0.066(3) 0.056(3) 0.064(3) 0.013(3) 0.010(3) -0.016(3) C13 0.105(5) 0.051(3) 0.079(4) 0.023(3) 0.007(4) -0.019(3) C14 0.103(5) 0.040(3) 0.077(4) 0.013(3) -0.008(4) -0.002(3) C15 0.079(4) 0.044(3) 0.066(4) 0.003(3) -0.016(3) 0.011(3) C16 0.054(3) 0.033(2) 0.062(3) 0.008(2) -0.007(2) 0.004(2) C21 0.037(2) 0.031(2) 0.036(2) 0.0086(18) 0.0040(19) 0.0000(17) C22 0.043(2) 0.053(3) 0.047(3) 0.007(2) 0.006(2) 0.004(2) C23 0.066(3) 0.064(3) 0.045(3) -0.008(3) 0.009(3) 0.008(3) C24 0.074(3) 0.047(3) 0.046(3) -0.001(2) -0.003(3) -0.003(2) C25 0.049(3) 0.041(2) 0.047(3) 0.009(2) -0.010(2) -0.007(2) C26 0.038(2) 0.030(2) 0.049(3) 0.010(2) 0.004(2) 0.0004(17) C31 0.0296(19) 0.0272(19) 0.039(3) 0.0044(18) 0.0003(18) -0.0025(15) C32 0.045(2) 0.039(2) 0.043(3) -0.003(2) 0.003(2) -0.0050(19) C33 0.057(3) 0.059(3) 0.050(3) -0.011(2) -0.006(3) -0.023(2) C34 0.041(3) 0.063(3) 0.069(4) 0.011(3) -0.012(3) -0.017(2) C35 0.036(2) 0.044(2) 0.062(3) 0.009(2) 0.001(2) -0.0068(19) C36 0.034(2) 0.032(2) 0.046(3) 0.0006(19) -0.004(2) -0.0034(17) C41 0.035(2) 0.0198(17) 0.039(2) -0.0022(17) -0.0019(19) -0.0032(15) C42 0.051(3) 0.030(2) 0.053(3) 0.003(2) 0.001(2) 0.0055(19) C43 0.074(3) 0.034(2) 0.078(4) 0.017(3) 0.002(3) 0.013(2) C44 0.080(4) 0.034(2) 0.058(3) 0.017(2) 0.002(3) -0.005(2) C45 0.066(3) 0.042(2) 0.046(3) 0.006(2) 0.007(2) -0.009(2) C46 0.050(3) 0.033(2) 0.057(3) 0.008(2) 0.007(2) 0.0029(19) C51 0.033(2) 0.0282(19) 0.042(3) -0.0040(19) -0.0134(19) -0.0005(16) C52 0.049(2) 0.033(2) 0.062(3) 0.004(2) 0.001(2) 0.0082(19) C53 0.042(2) 0.049(3) 0.062(3) -0.002(2) 0.005(2) 0.007(2) C54 0.056(3) 0.040(3) 0.070(4) -0.009(3) -0.015(3) 0.018(2) C55 0.102(4) 0.034(2) 0.073(4) 0.010(3) 0.003(3) 0.024(3) C56 0.079(3) 0.044(3) 0.048(3) 0.003(2) 0.004(3) 0.015(2) C61 0.041(2) 0.029(2) 0.067(3) -0.011(2) -0.016(2) 0.0093(18) C62 0.039(2) 0.039(2) 0.088(4) -0.017(3) 0.001(3) 0.003(2) C63 0.041(3) 0.051(3) 0.147(6) -0.043(4) 0.003(3) -0.004(2) C64 0.057(4) 0.061(4) 0.154(7) -0.052(4) -0.037(4) 0.009(3) C65 0.103(5) 0.068(4) 0.098(5) -0.024(4) -0.062(4) 0.010(4) C66 0.072(3) 0.047(3) 0.080(4) -0.011(3) -0.034(3) 0.007(2) C71 0.036(2) 0.0249(19) 0.044(3) -0.0033(18) 0.0033(19) 0.0035(17) C72 0.041(2) 0.040(2) 0.047(3) -0.001(2) 0.001(2) -0.0023(19) C73 0.061(3) 0.042(2) 0.053(3) -0.005(2) -0.008(3) -0.008(2) C74 0.069(3) 0.049(3) 0.047(3) -0.008(2) -0.007(3) 0.001(2) C75 0.073(3) 0.043(3) 0.050(3) 0.003(2) 0.022(3) -0.002(2) C76 0.039(2) 0.034(2) 0.056(3) -0.009(2) 0.006(2) -0.0044(18) C81 0.058(3) 0.037(2) 0.044(3) -0.013(2) -0.017(2) 0.013(2) C82 0.072(3) 0.030(2) 0.062(3) 0.006(2) -0.022(3) -0.001(2) C83 0.110(4) 0.033(3) 0.083(4) 0.006(3) -0.036(4) 0.003(3) C84 0.165(7) 0.041(3) 0.097(5) -0.011(3) -0.064(5) 0.032(4) C85 0.114(5) 0.073(4) 0.095(5) -0.026(4) -0.035(4) 0.064(4) C86 0.075(3) 0.048(3) 0.071(4) -0.017(3) -0.018(3) 0.026(2) C91 0.146(17) 0.084(17) 0.075(12) 0.002(9) 0.052(15) -0.03(2) C92 0.076(12) 0.105(19) 0.077(11) 0.009(10) 0.006(10) -0.024(12) C93 0.107(15) 0.101(16) 0.075(11) -0.002(10) 0.001(10) -0.012(13) C94 0.087(11) 0.086(12) 0.079(10) -0.003(10) -0.002(9) -0.019(10) C95 0.080(9) 0.109(13) 0.085(10) 0.002(9) 0.009(8) 0.000(8) C96 0.113(13) 0.077(10) 0.071(10) 0.006(8) 0.027(9) -0.024(9) C97 0.33(7) 0.10(2) 0.21(4) 0.01(2) 0.08(4) 0.12(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 S1 P1 1.9514(14) . ? S2 P2 1.9426(14) . ? S3 P3 1.9425(16) . ? S4 P4 1.9544(14) . ? P1 C21 1.816(4) . ? P1 C11 1.853(4) . ? P1 C1 1.856(4) . ? P2 C41 1.815(4) . ? P2 C31 1.821(4) . ? P2 C2 1.834(4) . ? P3 C51 1.817(4) . ? P3 C3 1.822(4) . ? P3 C61 1.827(4) . ? P4 C71 1.825(4) . ? P4 C81 1.842(4) . ? P4 C4 1.845(4) . ? C1 C2 1.575(5) . ? C1 C4 1.584(5) . ? C2 C3 1.548(5) . ? C3 C4 1.580(5) . ? C11 C16 1.379(6) . ? C11 C12 1.383(5) . ? C12 C13 1.421(6) . ? C13 C14 1.387(7) . ? C14 C15 1.341(7) . ? C15 C16 1.384(6) . ? C21 C22 1.393(5) . ? C21 C26 1.394(5) . ? C22 C23 1.367(6) . ? C23 C24 1.382(6) . ? C24 C25 1.385(6) . ? C25 C26 1.385(5) . ? C31 C32 1.392(5) . ? C31 C36 1.397(5) . ? C32 C33 1.380(6) . ? C33 C34 1.387(6) . ? C34 C35 1.375(6) . ? C35 C36 1.380(5) . ? C41 C42 1.383(5) . ? C41 C46 1.401(5) . ? C42 C43 1.370(6) . ? C43 C44 1.385(6) . ? C44 C45 1.378(6) . ? C45 C46 1.386(5) . ? C51 C52 1.388(6) . ? C51 C56 1.389(5) . ? C52 C53 1.383(5) . ? C53 C54 1.370(6) . ? C54 C55 1.376(7) . ? C55 C56 1.390(6) . ? C61 C66 1.373(7) . ? C61 C62 1.383(6) . ? C62 C63 1.389(6) . ? C63 C64 1.372(8) . ? C64 C65 1.379(9) . ? C65 C66 1.395(7) . ? C71 C76 1.373(5) . ? C71 C72 1.409(5) . ? C72 C73 1.381(6) . ? C73 C74 1.386(6) . ? C74 C75 1.372(6) . ? C75 C76 1.387(6) . ? C81 C86 1.383(6) . ? C81 C82 1.392(6) . ? C82 C83 1.384(6) . ? C83 C84 1.343(8) . ? C84 C85 1.383(9) . ? C85 C86 1.398(7) . ? C91 C91 0.80(3) 6_564 ? C91 C92 0.84(3) 6_564 ? C91 C96 1.37(4) . ? C91 C92 1.47(3) . ? C91 C97 1.56(4) . ? C91 C96 1.59(3) 6_564 ? C91 C93 1.63(4) 6_564 ? C92 C91 0.84(3) 6_564 ? C92 C96 1.04(2) 6_564 ? C92 C93 1.39(4) . ? C92 C97 1.70(5) 6_564 ? C93 C97 0.75(7) 6_564 ? C93 C94 1.27(4) . ? C93 C91 1.63(4) 6_564 ? C94 C97 0.72(4) 6_564 ? C94 C95 1.35(3) . ? C95 C96 1.37(2) . ? C95 C97 1.57(6) 6_564 ? C96 C92 1.04(2) 6_564 ? C96 C91 1.59(3) 6_564 ? C97 C94 0.72(4) 6_564 ? C97 C93 0.75(7) 6_564 ? C97 C95 1.57(6) 6_564 ? C97 C92 1.70(5) 6_564 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 P1 C11 102.67(18) . . ? C21 P1 C1 110.19(17) . . ? C11 P1 C1 102.52(17) . . ? C21 P1 S1 113.51(13) . . ? C11 P1 S1 111.88(14) . . ? C1 P1 S1 114.86(13) . . ? C41 P2 C31 102.64(16) . . ? C41 P2 C2 104.08(17) . . ? C31 P2 C2 104.42(17) . . ? C41 P2 S2 113.41(13) . . ? C31 P2 S2 114.78(14) . . ? C2 P2 S2 116.02(13) . . ? C51 P3 C3 105.82(18) . . ? C51 P3 C61 102.08(17) . . ? C3 P3 C61 102.80(19) . . ? C51 P3 S3 113.63(14) . . ? C3 P3 S3 116.05(13) . . ? C61 P3 S3 114.90(17) . . ? C71 P4 C81 101.32(18) . . ? C71 P4 C4 112.30(17) . . ? C81 P4 C4 102.53(19) . . ? C71 P4 S4 113.80(14) . . ? C81 P4 S4 112.04(15) . . ? C4 P4 S4 113.60(12) . . ? C2 C1 C4 86.7(3) . . ? C2 C1 P1 122.9(3) . . ? C4 C1 P1 109.4(2) . . ? C3 C2 C1 88.3(3) . . ? C3 C2 P2 123.4(2) . . ? C1 C2 P2 125.8(3) . . ? C2 C3 C4 87.8(3) . . ? C2 C3 P3 125.0(3) . . ? C4 C3 P3 125.2(3) . . ? C3 C4 C1 86.9(3) . . ? C3 C4 P4 124.4(3) . . ? C1 C4 P4 109.4(2) . . ? C16 C11 C12 119.1(4) . . ? C16 C11 P1 123.2(3) . . ? C12 C11 P1 117.5(3) . . ? C11 C12 C13 120.0(5) . . ? C14 C13 C12 118.5(5) . . ? C15 C14 C13 121.0(5) . . ? C14 C15 C16 120.8(5) . . ? C11 C16 C15 120.7(4) . . ? C22 C21 C26 119.1(4) . . ? C22 C21 P1 119.4(3) . . ? C26 C21 P1 121.4(3) . . ? C23 C22 C21 120.4(4) . . ? C22 C23 C24 120.9(4) . . ? C23 C24 C25 119.3(4) . . ? C24 C25 C26 120.5(4) . . ? C25 C26 C21 119.9(4) . . ? C32 C31 C36 119.1(4) . . ? C32 C31 P2 117.8(3) . . ? C36 C31 P2 123.0(3) . . ? C33 C32 C31 120.1(4) . . ? C32 C33 C34 119.9(4) . . ? C35 C34 C33 120.6(4) . . ? C34 C35 C36 119.6(4) . . ? C35 C36 C31 120.6(4) . . ? C42 C41 C46 118.8(4) . . ? C42 C41 P2 119.6(3) . . ? C46 C41 P2 121.6(3) . . ? C43 C42 C41 120.3(4) . . ? C42 C43 C44 120.8(4) . . ? C45 C44 C43 120.1(4) . . ? C44 C45 C46 119.2(4) . . ? C45 C46 C41 120.8(4) . . ? C52 C51 C56 118.2(4) . . ? C52 C51 P3 123.3(3) . . ? C56 C51 P3 118.4(3) . . ? C53 C52 C51 121.0(4) . . ? C54 C53 C52 120.3(4) . . ? C53 C54 C55 119.7(4) . . ? C54 C55 C56 120.3(5) . . ? C51 C56 C55 120.5(5) . . ? C66 C61 C62 119.3(4) . . ? C66 C61 P3 117.8(4) . . ? C62 C61 P3 122.7(4) . . ? C61 C62 C63 120.5(5) . . ? C64 C63 C62 119.3(6) . . ? C63 C64 C65 121.4(6) . . ? C64 C65 C66 118.5(6) . . ? C61 C66 C65 121.1(6) . . ? C76 C71 C72 119.6(4) . . ? C76 C71 P4 119.4(3) . . ? C72 C71 P4 120.7(3) . . ? C73 C72 C71 119.3(4) . . ? C72 C73 C74 120.5(4) . . ? C75 C74 C73 119.8(4) . . ? C74 C75 C76 120.3(4) . . ? C71 C76 C75 120.4(4) . . ? C86 C81 C82 118.8(4) . . ? C86 C81 P4 116.4(4) . . ? C82 C81 P4 124.7(3) . . ? C83 C82 C81 120.8(5) . . ? C84 C83 C82 120.0(6) . . ? C83 C84 C85 121.1(6) . . ? C84 C85 C86 119.5(6) . . ? C81 C86 C85 119.9(5) . . ? C91 C91 C92 128(9) 6_564 6_564 ? C91 C91 C96 90(6) 6_564 . ? C92 C91 C96 49(3) 6_564 . ? C91 C91 C92 27(4) 6_564 . ? C92 C91 C92 143(5) 6_564 . ? C96 C91 C92 116.5(16) . . ? C91 C91 C97 147(7) 6_564 . ? C92 C91 C97 84(4) 6_564 . ? C96 C91 C97 120(2) . . ? C92 C91 C97 123(3) . . ? C91 C91 C96 60(5) 6_564 6_564 ? C92 C91 C96 168(4) 6_564 6_564 ? C96 C91 C96 142.1(15) . 6_564 ? C92 C91 C96 39.6(10) . 6_564 ? C97 C91 C96 87(3) . 6_564 ? C91 C91 C93 166(5) 6_564 6_564 ? C92 C91 C93 58(3) 6_564 6_564 ? C96 C91 C93 101.3(19) . 6_564 ? C92 C91 C93 140(2) . 6_564 ? C97 C91 C93 27(3) . 6_564 ? C96 C91 C93 112(3) 6_564 6_564 ? C91 C92 C96 93(4) 6_564 6_564 ? C91 C92 C93 91(4) 6_564 . ? C96 C92 C93 146(3) 6_564 . ? C91 C92 C91 25(4) 6_564 . ? C96 C92 C91 76.3(17) 6_564 . ? C93 C92 C91 115(2) . . ? C91 C92 C97 66(4) 6_564 6_564 ? C96 C92 C97 135(3) 6_564 6_564 ? C93 C92 C97 26(3) . 6_564 ? C91 C92 C97 91(2) . 6_564 ? C97 C93 C94 29(4) 6_564 . ? C97 C93 C92 101(5) 6_564 . ? C94 C93 C92 126(2) . . ? C97 C93 C91 71(4) 6_564 6_564 ? C94 C93 C91 95.0(19) . 6_564 ? C92 C93 C91 31.0(15) . 6_564 ? C97 C94 C93 31(6) 6_564 . ? C97 C94 C95 94(6) 6_564 . ? C93 C94 C95 120(2) . . ? C94 C95 C96 120.5(14) . . ? C94 C95 C97 27.4(12) . 6_564 ? C96 C95 C97 95.3(15) . 6_564 ? C92 C96 C91 37.7(12) 6_564 . ? C92 C96 C95 145(2) 6_564 . ? C91 C96 C95 121.6(14) . . ? C92 C96 C91 64.1(14) 6_564 6_564 ? C91 C96 C91 30.1(16) . 6_564 ? C95 C96 C91 91.6(15) . 6_564 ? C94 C97 C93 120(9) 6_564 6_564 ? C94 C97 C91 139(7) 6_564 . ? C93 C97 C91 82(5) 6_564 . ? C94 C97 C95 59(5) 6_564 6_564 ? C93 C97 C95 154(7) 6_564 6_564 ? C91 C97 C95 86(3) . 6_564 ? C94 C97 C92 155(6) 6_564 6_564 ? C93 C97 C92 53(4) 6_564 6_564 ? C91 C97 C92 29.5(11) . 6_564 ? C95 C97 C92 115(3) 6_564 6_564 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 P1 C1 C2 67.3(3) . . . . ? C11 P1 C1 C2 176.0(3) . . . . ? S1 P1 C1 C2 -62.4(3) . . . . ? C21 P1 C1 C4 166.2(2) . . . . ? C11 P1 C1 C4 -85.1(3) . . . . ? S1 P1 C1 C4 36.5(3) . . . . ? C4 C1 C2 C3 -24.2(3) . . . . ? P1 C1 C2 C3 86.8(3) . . . . ? C4 C1 C2 P2 -155.2(3) . . . . ? P1 C1 C2 P2 -44.2(4) . . . . ? C41 P2 C2 C3 77.6(3) . . . . ? C31 P2 C2 C3 -175.1(3) . . . . ? S2 P2 C2 C3 -47.7(3) . . . . ? C41 P2 C2 C1 -166.9(3) . . . . ? C31 P2 C2 C1 -59.6(3) . . . . ? S2 P2 C2 C1 67.8(3) . . . . ? C1 C2 C3 C4 24.2(3) . . . . ? P2 C2 C3 C4 157.2(3) . . . . ? C1 C2 C3 P3 156.8(3) . . . . ? P2 C2 C3 P3 -70.3(4) . . . . ? C51 P3 C3 C2 85.4(3) . . . . ? C61 P3 C3 C2 -167.9(3) . . . . ? S3 P3 C3 C2 -41.7(3) . . . . ? C51 P3 C3 C4 -158.9(3) . . . . ? C61 P3 C3 C4 -52.2(3) . . . . ? S3 P3 C3 C4 74.1(3) . . . . ? C2 C3 C4 C1 -24.1(3) . . . . ? P3 C3 C4 C1 -156.5(3) . . . . ? C2 C3 C4 P4 87.3(3) . . . . ? P3 C3 C4 P4 -45.0(4) . . . . ? C2 C1 C4 C3 23.7(3) . . . . ? P1 C1 C4 C3 -100.1(2) . . . . ? C2 C1 C4 P4 -101.8(2) . . . . ? P1 C1 C4 P4 134.4(2) . . . . ? C71 P4 C4 C3 67.6(3) . . . . ? C81 P4 C4 C3 175.6(3) . . . . ? S4 P4 C4 C3 -63.3(3) . . . . ? C71 P4 C4 C1 167.4(2) . . . . ? C81 P4 C4 C1 -84.6(3) . . . . ? S4 P4 C4 C1 36.5(3) . . . . ? C21 P1 C11 C16 73.7(4) . . . . ? C1 P1 C11 C16 -40.6(4) . . . . ? S1 P1 C11 C16 -164.2(3) . . . . ? C21 P1 C11 C12 -101.2(4) . . . . ? C1 P1 C11 C12 144.5(4) . . . . ? S1 P1 C11 C12 20.9(4) . . . . ? C16 C11 C12 C13 -0.9(7) . . . . ? P1 C11 C12 C13 174.2(4) . . . . ? C11 C12 C13 C14 1.0(8) . . . . ? C12 C13 C14 C15 -0.7(9) . . . . ? C13 C14 C15 C16 0.2(9) . . . . ? C12 C11 C16 C15 0.4(7) . . . . ? P1 C11 C16 C15 -174.4(4) . . . . ? C14 C15 C16 C11 0.0(8) . . . . ? C11 P1 C21 C22 116.8(3) . . . . ? C1 P1 C21 C22 -134.6(3) . . . . ? S1 P1 C21 C22 -4.2(4) . . . . ? C11 P1 C21 C26 -60.9(3) . . . . ? C1 P1 C21 C26 47.7(4) . . . . ? S1 P1 C21 C26 178.2(3) . . . . ? C26 C21 C22 C23 1.1(6) . . . . ? P1 C21 C22 C23 -176.7(3) . . . . ? C21 C22 C23 C24 -0.8(7) . . . . ? C22 C23 C24 C25 0.4(7) . . . . ? C23 C24 C25 C26 -0.3(6) . . . . ? C24 C25 C26 C21 0.7(6) . . . . ? C22 C21 C26 C25 -1.0(5) . . . . ? P1 C21 C26 C25 176.7(3) . . . . ? C41 P2 C31 C32 -92.2(3) . . . . ? C2 P2 C31 C32 159.4(3) . . . . ? S2 P2 C31 C32 31.3(3) . . . . ? C41 P2 C31 C36 84.2(3) . . . . ? C2 P2 C31 C36 -24.1(4) . . . . ? S2 P2 C31 C36 -152.3(3) . . . . ? C36 C31 C32 C33 1.1(6) . . . . ? P2 C31 C32 C33 177.7(3) . . . . ? C31 C32 C33 C34 0.7(7) . . . . ? C32 C33 C34 C35 -2.5(7) . . . . ? C33 C34 C35 C36 2.4(6) . . . . ? C34 C35 C36 C31 -0.6(6) . . . . ? C32 C31 C36 C35 -1.1(6) . . . . ? P2 C31 C36 C35 -177.5(3) . . . . ? C31 P2 C41 C42 124.5(3) . . . . ? C2 P2 C41 C42 -126.9(3) . . . . ? S2 P2 C41 C42 0.1(4) . . . . ? C31 P2 C41 C46 -52.4(4) . . . . ? C2 P2 C41 C46 56.2(4) . . . . ? S2 P2 C41 C46 -176.8(3) . . . . ? C46 C41 C42 C43 -1.3(6) . . . . ? P2 C41 C42 C43 -178.3(3) . . . . ? C41 C42 C43 C44 1.0(7) . . . . ? C42 C43 C44 C45 -1.1(8) . . . . ? C43 C44 C45 C46 1.6(7) . . . . ? C44 C45 C46 C41 -1.9(7) . . . . ? C42 C41 C46 C45 1.8(6) . . . . ? P2 C41 C46 C45 178.7(3) . . . . ? C3 P3 C51 C52 39.7(4) . . . . ? C61 P3 C51 C52 -67.5(4) . . . . ? S3 P3 C51 C52 168.2(3) . . . . ? C3 P3 C51 C56 -144.9(3) . . . . ? C61 P3 C51 C56 107.9(4) . . . . ? S3 P3 C51 C56 -16.4(4) . . . . ? C56 C51 C52 C53 0.0(6) . . . . ? P3 C51 C52 C53 175.4(3) . . . . ? C51 C52 C53 C54 0.4(7) . . . . ? C52 C53 C54 C55 -0.8(7) . . . . ? C53 C54 C55 C56 0.9(8) . . . . ? C52 C51 C56 C55 0.1(7) . . . . ? P3 C51 C56 C55 -175.6(4) . . . . ? C54 C55 C56 C51 -0.5(8) . . . . ? C51 P3 C61 C66 -96.5(4) . . . . ? C3 P3 C61 C66 154.0(3) . . . . ? S3 P3 C61 C66 27.0(4) . . . . ? C51 P3 C61 C62 79.4(4) . . . . ? C3 P3 C61 C62 -30.2(4) . . . . ? S3 P3 C61 C62 -157.2(3) . . . . ? C66 C61 C62 C63 -0.5(6) . . . . ? P3 C61 C62 C63 -176.2(3) . . . . ? C61 C62 C63 C64 0.4(7) . . . . ? C62 C63 C64 C65 -0.1(8) . . . . ? C63 C64 C65 C66 -0.1(9) . . . . ? C62 C61 C66 C65 0.2(7) . . . . ? P3 C61 C66 C65 176.2(4) . . . . ? C64 C65 C66 C61 0.1(8) . . . . ? C81 P4 C71 C76 126.0(3) . . . . ? C4 P4 C71 C76 -125.2(3) . . . . ? S4 P4 C71 C76 5.6(3) . . . . ? C81 P4 C71 C72 -47.1(3) . . . . ? C4 P4 C71 C72 61.6(3) . . . . ? S4 P4 C71 C72 -167.5(3) . . . . ? C76 C71 C72 C73 0.5(6) . . . . ? P4 C71 C72 C73 173.6(3) . . . . ? C71 C72 C73 C74 -1.2(6) . . . . ? C72 C73 C74 C75 0.9(7) . . . . ? C73 C74 C75 C76 0.1(7) . . . . ? C72 C71 C76 C75 0.6(6) . . . . ? P4 C71 C76 C75 -172.6(3) . . . . ? C74 C75 C76 C71 -0.9(6) . . . . ? C71 P4 C81 C86 -93.0(4) . . . . ? C4 P4 C81 C86 150.9(3) . . . . ? S4 P4 C81 C86 28.7(4) . . . . ? C71 P4 C81 C82 82.0(4) . . . . ? C4 P4 C81 C82 -34.2(4) . . . . ? S4 P4 C81 C82 -156.4(3) . . . . ? C86 C81 C82 C83 0.5(7) . . . . ? P4 C81 C82 C83 -174.4(4) . . . . ? C81 C82 C83 C84 -0.5(8) . . . . ? C82 C83 C84 C85 0.7(9) . . . . ? C83 C84 C85 C86 -1.0(10) . . . . ? C82 C81 C86 C85 -0.7(7) . . . . ? P4 C81 C86 C85 174.5(4) . . . . ? C84 C85 C86 C81 1.0(9) . . . . ? C92 C91 C92 C91 -69(10) 6_564 . . 6_564 ? C96 C91 C92 C91 -12(5) . . . 6_564 ? C97 C91 C92 C91 160(5) . . . 6_564 ? C96 C91 C92 C91 129(4) 6_564 . . 6_564 ? C93 C91 C92 C91 -172(6) 6_564 . . 6_564 ? C91 C91 C92 C96 -129(4) 6_564 . . 6_564 ? C92 C91 C92 C96 162(6) 6_564 . . 6_564 ? C96 C91 C92 C96 -141(2) . . . 6_564 ? C97 C91 C92 C96 31(4) . . . 6_564 ? C93 C91 C92 C96 59(5) 6_564 . . 6_564 ? C91 C91 C92 C93 17(4) 6_564 . . . ? C92 C91 C92 C93 -52(7) 6_564 . . . ? C96 C91 C92 C93 5(4) . . . . ? C97 C91 C92 C93 177(2) . . . . ? C96 C91 C92 C93 146(3) 6_564 . . . ? C93 C91 C92 C93 -155(4) 6_564 . . . ? C91 C91 C92 C97 7(4) 6_564 . . 6_564 ? C92 C91 C92 C97 -62(7) 6_564 . . 6_564 ? C96 C91 C92 C97 -5(3) . . . 6_564 ? C97 C91 C92 C97 167(4) . . . 6_564 ? C96 C91 C92 C97 136(3) 6_564 . . 6_564 ? C93 C91 C92 C97 -165(4) 6_564 . . 6_564 ? C91 C92 C93 C97 -16(6) 6_564 . . 6_564 ? C96 C92 C93 C97 80(7) 6_564 . . 6_564 ? C91 C92 C93 C97 -23(6) . . . 6_564 ? C91 C92 C93 C94 1(4) 6_564 . . . ? C96 C92 C93 C94 97(4) 6_564 . . . ? C91 C92 C93 C94 -6(4) . . . . ? C97 C92 C93 C94 17(4) 6_564 . . . ? C96 C92 C93 C91 96(5) 6_564 . . 6_564 ? C91 C92 C93 C91 -7.1(9) . . . 6_564 ? C97 C92 C93 C91 16(6) 6_564 . . 6_564 ? C92 C93 C94 C97 -36(8) . . . 6_564 ? C91 C93 C94 C97 -35(9) 6_564 . . 6_564 ? C97 C93 C94 C95 36(9) 6_564 . . . ? C92 C93 C94 C95 0(4) . . . . ? C91 C93 C94 C95 0(2) 6_564 . . . ? C97 C94 C95 C96 25(5) 6_564 . . . ? C93 C94 C95 C96 8(3) . . . . ? C93 C94 C95 C97 -17(5) . . . 6_564 ? C91 C91 C96 C92 -144(4) 6_564 . . 6_564 ? C92 C91 C96 C92 -138(5) . . . 6_564 ? C97 C91 C96 C92 49(3) . . . 6_564 ? C96 C91 C96 C92 -179(6) 6_564 . . 6_564 ? C93 C91 C96 C92 29(3) 6_564 . . 6_564 ? C91 C91 C96 C95 -4(2) 6_564 . . . ? C92 C91 C96 C95 140(3) 6_564 . . . ? C92 C91 C96 C95 2(3) . . . . ? C97 C91 C96 C95 -171(3) . . . . ? C96 C91 C96 C95 -39(4) 6_564 . . . ? C93 C91 C96 C95 168.8(15) 6_564 . . . ? C92 C91 C96 C91 144(4) 6_564 . . 6_564 ? C92 C91 C96 C91 5.3(19) . . . 6_564 ? C97 C91 C96 C91 -167(3) . . . 6_564 ? C96 C91 C96 C91 -35(2) 6_564 . . 6_564 ? C93 C91 C96 C91 172(2) 6_564 . . 6_564 ? C94 C95 C96 C92 34(4) . . . 6_564 ? C97 C95 C96 C92 45(4) 6_564 . . 6_564 ? C94 C95 C96 C91 -8(3) . . . . ? C97 C95 C96 C91 3(3) 6_564 . . . ? C94 C95 C96 C91 -10.1(18) . . . 6_564 ? C97 C95 C96 C91 1(2) 6_564 . . 6_564 ? C91 C91 C97 C94 28(13) 6_564 . . 6_564 ? C92 C91 C97 C94 -141(11) 6_564 . . 6_564 ? C96 C91 C97 C94 -176(10) . . . 6_564 ? C92 C91 C97 C94 12(12) . . . 6_564 ? C96 C91 C97 C94 31(11) 6_564 . . 6_564 ? C93 C91 C97 C94 -127(14) 6_564 . . 6_564 ? C91 C91 C97 C93 155(4) 6_564 . . 6_564 ? C92 C91 C97 C93 -14(6) 6_564 . . 6_564 ? C96 C91 C97 C93 -49(6) . . . 6_564 ? C92 C91 C97 C93 139(5) . . . 6_564 ? C96 C91 C97 C93 158(5) 6_564 . . 6_564 ? C91 C91 C97 C95 -2(5) 6_564 . . 6_564 ? C92 C91 C97 C95 -171(3) 6_564 . . 6_564 ? C96 C91 C97 C95 154(2) . . . 6_564 ? C92 C91 C97 C95 -18(4) . . . 6_564 ? C96 C91 C97 C95 1.0(19) 6_564 . . 6_564 ? C93 C91 C97 C95 -157(7) 6_564 . . 6_564 ? C91 C91 C97 C92 169(4) 6_564 . . 6_564 ? C96 C91 C97 C92 -35(2) . . . 6_564 ? C92 C91 C97 C92 153(5) . . . 6_564 ? C96 C91 C97 C92 172(3) 6_564 . . 6_564 ? C93 C91 C97 C92 14(6) 6_564 . . 6_564 ? _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction 0.990 _refine_diff_density_max 0.240 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.050 #===END data_IV _database_code_CSD 211320 _audit_creation_method SHELXL-97 _chemical_name_systematic dppcbSe4 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 P4 Se4 x 0.5 C7 H8' _chemical_formula_sum 'C55.5 H48 P4 Se4' _chemical_formula_weight 1154.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 38.730(3) _cell_length_b 38.730(3) _cell_length_c 13.281(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19921(4) _cell_formula_units_Z 16 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'rectangular solid' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9232 _exptl_absorpt_coefficient_mu 3.109 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10844 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.2358 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.0 _reflns_number_total 6281 _reflns_number_gt 2168 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Software of the Siemens P4' _computing_data_reduction 'Software of the Siemens P4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0200P)^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 6281 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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 Se1 Se -0.57777(3) -0.51925(3) 0.24852(9) 0.0407(3) Uani 1 1 d . . . Se2 Se -0.64708(3) -0.59004(3) 0.39653(9) 0.0476(4) Uani 1 1 d . . . Se3 Se -0.67918(3) -0.62575(3) -0.03809(8) 0.0371(3) Uani 1 1 d . . . Se4 Se -0.57602(3) -0.65934(3) -0.03074(10) 0.0464(4) Uani 1 1 d . . . P1 P -0.55383(7) -0.56848(7) 0.2490(2) 0.0314(8) Uani 1 1 d . . . P2 P -0.63198(7) -0.62924(7) 0.2970(2) 0.0326(8) Uani 1 1 d . . . P3 P -0.66752(6) -0.58191(7) 0.0480(2) 0.0247(7) Uani 1 1 d . . . P4 P -0.57604(7) -0.60469(6) -0.0469(2) 0.0269(7) Uani 1 1 d . . . C1 C -0.5756(2) -0.6008(2) 0.1653(7) 0.028(3) Uani 1 1 d . . . H1A H -0.5597 -0.6196 0.1476 0.034 Uiso 1 1 calc R . . C2 C -0.6134(2) -0.6146(2) 0.1763(6) 0.020(3) Uani 1 1 d . . . H2A H -0.6151 -0.6343 0.1306 0.024 Uiso 1 1 calc R . . C3 C -0.6258(2) -0.5835(2) 0.1160(7) 0.027(3) Uani 1 1 d . . . H3A H -0.6266 -0.5644 0.1642 0.033 Uiso 1 1 calc R . . C4 C -0.5890(2) -0.5813(2) 0.0663(7) 0.030(3) Uani 1 1 d . . . H4A H -0.5807 -0.5574 0.0646 0.037 Uiso 1 1 calc R . . C11 C -0.5099(2) -0.5666(3) 0.2002(8) 0.035(3) Uani 1 1 d . . . C12 C -0.4912(3) -0.5368(3) 0.2136(9) 0.058(4) Uani 1 1 d . . . H12A H -0.5020 -0.5178 0.2423 0.069 Uiso 1 1 calc R . . C13 C -0.4568(3) -0.5342(3) 0.1859(10) 0.067(4) Uani 1 1 d . . . H13A H -0.4447 -0.5139 0.1976 0.080 Uiso 1 1 calc R . . C14 C -0.4408(3) -0.5622(4) 0.1405(11) 0.079(5) Uani 1 1 d . . . H14A H -0.4178 -0.5606 0.1204 0.095 Uiso 1 1 calc R . . C15 C -0.4585(3) -0.5921(4) 0.1256(9) 0.068(5) Uani 1 1 d . . . H15A H -0.4474 -0.6108 0.0961 0.081 Uiso 1 1 calc R . . C16 C -0.4925(3) -0.5949(3) 0.1532(7) 0.042(3) Uani 1 1 d . . . H16A H -0.5044 -0.6154 0.1414 0.051 Uiso 1 1 calc R . . C21 C -0.5466(2) -0.5864(3) 0.3754(7) 0.028(3) Uani 1 1 d . . . C22 C -0.5242(3) -0.6148(3) 0.3877(9) 0.042(3) Uani 1 1 d . . . H22A H -0.5148 -0.6262 0.3324 0.050 Uiso 1 1 calc R . . C23 C -0.5168(3) -0.6251(3) 0.4844(9) 0.053(4) Uani 1 1 d . . . H23A H -0.5023 -0.6441 0.4940 0.063 Uiso 1 1 calc R . . C24 C -0.5299(3) -0.6084(3) 0.5672(9) 0.048(3) Uani 1 1 d . . . H24A H -0.5243 -0.6160 0.6316 0.057 Uiso 1 1 calc R . . C25 C -0.5511(3) -0.5808(3) 0.5544(9) 0.048(4) Uani 1 1 d . . . H25A H -0.5601 -0.5696 0.6106 0.058 Uiso 1 1 calc R . . C26 C -0.5597(2) -0.5689(3) 0.4572(9) 0.037(3) Uani 1 1 d . . . H26A H -0.5738 -0.5496 0.4486 0.044 Uiso 1 1 calc R . . C31 C -0.5997(3) -0.6594(3) 0.3433(9) 0.034(3) Uani 1 1 d . . . C32 C -0.5781(3) -0.6784(3) 0.2832(9) 0.046(4) Uani 1 1 d . . . H32A H -0.5784 -0.6747 0.2140 0.056 Uiso 1 1 calc R . . C33 C -0.5562(3) -0.7027(3) 0.3218(11) 0.061(4) Uani 1 1 d . . . H33A H -0.5423 -0.7157 0.2792 0.073 Uiso 1 1 calc R . . C34 C -0.5549(4) -0.7077(3) 0.4259(12) 0.073(5) Uani 1 1 d . . . H34A H -0.5394 -0.7233 0.4540 0.088 Uiso 1 1 calc R . . C35 C -0.5762(3) -0.6895(4) 0.4844(11) 0.077(5) Uani 1 1 d . . . H35A H -0.5762 -0.6936 0.5534 0.092 Uiso 1 1 calc R . . C36 C -0.5986(3) -0.6646(3) 0.4454(10) 0.060(4) Uani 1 1 d . . . H36A H -0.6126 -0.6518 0.4881 0.072 Uiso 1 1 calc R . . C41 C -0.6668(2) -0.6583(2) 0.2646(8) 0.023(3) Uani 1 1 d . . . C42 C -0.6651(3) -0.6809(3) 0.1857(8) 0.037(3) Uani 1 1 d . . . H42A H -0.6457 -0.6806 0.1441 0.045 Uiso 1 1 calc R . . C43 C -0.6915(3) -0.7043(3) 0.1660(8) 0.046(3) Uani 1 1 d . . . H43A H -0.6892 -0.7199 0.1130 0.055 Uiso 1 1 calc R . . C44 C -0.7211(3) -0.7048(3) 0.2241(10) 0.052(4) Uani 1 1 d . . . H44A H -0.7391 -0.7201 0.2108 0.062 Uiso 1 1 calc R . . C45 C -0.7228(3) -0.6815(3) 0.3031(9) 0.063(4) Uani 1 1 d . . . H45A H -0.7423 -0.6816 0.3439 0.076 Uiso 1 1 calc R . . C46 C -0.6969(3) -0.6582(3) 0.3238(8) 0.048(4) Uani 1 1 d . . . H46A H -0.6993 -0.6426 0.3765 0.058 Uiso 1 1 calc R . . C51 C -0.6990(2) -0.5733(2) 0.1490(7) 0.020(3) Uani 1 1 d . . . C52 C -0.7259(2) -0.5964(3) 0.1630(7) 0.036(3) Uani 1 1 d . . . H52A H -0.7280 -0.6158 0.1221 0.043 Uiso 1 1 calc R . . C53 C -0.7498(3) -0.5900(3) 0.2399(9) 0.057(4) Uani 1 1 d . . . H53A H -0.7672 -0.6059 0.2528 0.068 Uiso 1 1 calc R . . C54 C -0.7476(3) -0.5611(3) 0.2952(8) 0.045(3) Uani 1 1 d . . . H54A H -0.7641 -0.5570 0.3444 0.054 Uiso 1 1 calc R . . C55 C -0.7217(3) -0.5374(3) 0.2813(8) 0.041(3) Uani 1 1 d . . . H55A H -0.7203 -0.5178 0.3216 0.049 Uiso 1 1 calc R . . C56 C -0.6975(3) -0.5433(3) 0.2057(9) 0.042(3) Uani 1 1 d . . . H56A H -0.6804 -0.5271 0.1931 0.050 Uiso 1 1 calc R . . C61 C -0.6663(2) -0.5416(2) -0.0215(8) 0.024(3) Uani 1 1 d . . . C62 C -0.6879(3) -0.5381(3) -0.1053(8) 0.045(3) Uani 1 1 d . . . H62A H -0.7013 -0.5566 -0.1264 0.054 Uiso 1 1 calc R . . C63 C -0.6894(3) -0.5070(3) -0.1568(8) 0.051(4) Uani 1 1 d . . . H63A H -0.7043 -0.5047 -0.2113 0.061 Uiso 1 1 calc R . . C64 C -0.6687(3) -0.4790(3) -0.1282(8) 0.043(3) Uani 1 1 d . . . H64A H -0.6691 -0.4584 -0.1641 0.051 Uiso 1 1 calc R . . C65 C -0.6481(3) -0.4830(2) -0.0463(8) 0.033(3) Uani 1 1 d . . . H65A H -0.6342 -0.4646 -0.0263 0.039 Uiso 1 1 calc R . . C66 C -0.6469(3) -0.5132(2) 0.0083(7) 0.033(3) Uani 1 1 d . . . H66A H -0.6331 -0.5146 0.0654 0.040 Uiso 1 1 calc R . . C71 C -0.6001(2) -0.5908(2) -0.1559(8) 0.026(3) Uani 1 1 d . . . C72 C -0.6154(3) -0.6138(3) -0.2244(8) 0.039(3) Uani 1 1 d . . . H72A H -0.6150 -0.6373 -0.2107 0.046 Uiso 1 1 calc R . . C73 C -0.6304(3) -0.6027(3) -0.3081(8) 0.050(4) Uani 1 1 d . . . H73A H -0.6394 -0.6187 -0.3531 0.060 Uiso 1 1 calc R . . C74 C -0.6328(3) -0.5679(3) -0.3298(8) 0.051(4) Uani 1 1 d . . . H74A H -0.6442 -0.5607 -0.3879 0.061 Uiso 1 1 calc R . . C75 C -0.6185(2) -0.5436(3) -0.2656(9) 0.040(3) Uani 1 1 d . . . H75A H -0.6199 -0.5201 -0.2799 0.048 Uiso 1 1 calc R . . C76 C -0.6020(2) -0.5554(2) -0.1795(8) 0.029(3) Uani 1 1 d . . . H76A H -0.5919 -0.5394 -0.1361 0.035 Uiso 1 1 calc R . . C81 C -0.5330(2) -0.5886(3) -0.0708(7) 0.031(3) Uani 1 1 d . . . C82 C -0.5231(2) -0.5540(2) -0.0603(7) 0.029(3) Uani 1 1 d . . . H82A H -0.5390 -0.5383 -0.0345 0.035 Uiso 1 1 calc R . . C83 C -0.4907(3) -0.5422(3) -0.0867(8) 0.049(3) Uani 1 1 d . . . H83A H -0.4845 -0.5194 -0.0756 0.059 Uiso 1 1 calc R . . C84 C -0.4678(3) -0.5650(3) -0.1299(8) 0.048(4) Uani 1 1 d . . . H84A H -0.4461 -0.5572 -0.1498 0.057 Uiso 1 1 calc R . . C85 C -0.4765(3) -0.5985(3) -0.1437(9) 0.063(4) Uani 1 1 d . . . H85A H -0.4610 -0.6137 -0.1738 0.076 Uiso 1 1 calc R . . C86 C -0.5086(3) -0.6100(3) -0.1129(8) 0.057(4) Uani 1 1 d . . . H86A H -0.5139 -0.6333 -0.1209 0.068 Uiso 1 1 calc R . . C91 C -0.5000 -0.7500 0.726(4) 0.23(5) Uani 1 2 d S . . C92 C -0.4885(18) -0.7290(13) 0.688(3) 0.20(2) Uani 0.75 1 d P . . C93 C -0.4954(7) -0.6949(5) 0.693(2) 0.112(10) Uani 0.75 1 d P . . C94 C -0.5230(7) -0.6936(7) 0.722(2) 0.110(11) Uani 0.75 1 d P . . C95 C -0.5447(10) -0.7130(7) 0.747(2) 0.143(14) Uani 0.75 1 d P . . C96 C -0.5392(9) -0.7469(11) 0.749(3) 0.191(16) Uani 0.75 1 d P . . 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 Se1 0.0443(8) 0.0286(7) 0.0490(8) -0.0046(6) -0.0113(7) 0.0001(6) Se2 0.0460(8) 0.0593(9) 0.0376(8) -0.0080(7) 0.0037(7) -0.0049(7) Se3 0.0385(7) 0.0344(7) 0.0384(8) -0.0095(6) -0.0005(6) -0.0049(6) Se4 0.0590(8) 0.0246(7) 0.0557(9) -0.0041(7) 0.0134(8) 0.0043(6) P1 0.0260(17) 0.0296(18) 0.039(2) 0.0016(16) -0.0050(16) -0.0011(14) P2 0.0263(18) 0.0405(19) 0.0308(19) 0.0023(17) 0.0009(16) -0.0038(16) P3 0.0222(16) 0.0284(17) 0.0234(18) -0.0041(15) -0.0006(15) -0.0009(13) P4 0.0321(18) 0.0211(16) 0.0275(18) -0.0029(15) 0.0083(16) 0.0039(14) C1 0.014(6) 0.029(6) 0.041(8) 0.000(6) -0.001(6) 0.003(5) C2 0.015(6) 0.021(6) 0.023(7) -0.002(5) -0.007(5) 0.001(5) C3 0.018(6) 0.015(6) 0.050(8) -0.008(6) -0.012(6) 0.003(5) C4 0.020(6) 0.035(7) 0.036(8) -0.015(6) 0.006(6) -0.003(5) C11 0.008(6) 0.061(8) 0.034(8) 0.017(7) -0.009(6) -0.003(6) C12 0.040(8) 0.053(9) 0.081(11) 0.017(8) -0.014(8) -0.020(7) C13 0.053(10) 0.076(11) 0.071(12) 0.028(9) -0.027(9) -0.021(9) C14 0.017(8) 0.115(14) 0.104(14) 0.066(12) 0.004(9) -0.013(9) C15 0.010(7) 0.107(12) 0.085(11) 0.061(10) 0.016(8) 0.014(8) C16 0.042(8) 0.053(8) 0.031(8) 0.008(7) -0.005(7) 0.005(7) C21 0.017(6) 0.041(8) 0.027(8) 0.004(6) 0.004(6) -0.014(6) C22 0.035(7) 0.041(8) 0.049(9) 0.009(7) 0.002(7) 0.017(6) C23 0.072(9) 0.038(8) 0.048(9) -0.015(8) -0.014(8) 0.012(7) C24 0.036(8) 0.066(10) 0.041(9) -0.006(8) -0.010(7) -0.010(7) C25 0.034(8) 0.074(10) 0.036(9) -0.011(8) 0.000(7) 0.024(7) C26 0.025(7) 0.045(8) 0.040(8) -0.010(7) -0.001(7) 0.006(6) C31 0.019(7) 0.036(7) 0.046(9) 0.019(7) -0.004(7) 0.008(6) C32 0.023(7) 0.037(7) 0.079(10) -0.006(8) -0.029(8) -0.010(6) C33 0.037(8) 0.039(8) 0.105(13) -0.003(9) -0.020(9) 0.008(7) C34 0.066(11) 0.053(10) 0.100(15) 0.018(10) -0.066(11) 0.003(8) C35 0.065(11) 0.075(12) 0.090(14) 0.054(11) -0.017(10) -0.027(9) C36 0.041(8) 0.059(9) 0.079(11) 0.052(9) -0.012(8) 0.010(7) C41 0.020(6) 0.024(6) 0.024(7) -0.001(6) 0.001(6) 0.015(5) C42 0.024(7) 0.040(7) 0.047(9) -0.005(7) 0.009(6) 0.010(6) C43 0.038(8) 0.050(8) 0.050(9) 0.003(7) -0.018(7) -0.004(7) C44 0.035(8) 0.060(9) 0.060(10) 0.007(8) -0.005(8) -0.018(7) C45 0.043(9) 0.090(11) 0.056(10) 0.001(9) -0.001(8) -0.014(8) C46 0.037(7) 0.053(8) 0.055(9) 0.001(7) -0.007(7) -0.019(7) C51 0.016(6) 0.022(6) 0.023(7) 0.012(6) 0.008(5) -0.008(5) C52 0.032(7) 0.041(7) 0.034(8) -0.013(6) 0.009(6) -0.003(6) C53 0.039(8) 0.062(9) 0.070(11) 0.002(8) 0.018(8) -0.013(7) C54 0.056(9) 0.063(9) 0.016(7) -0.012(7) 0.014(7) 0.008(8) C55 0.051(8) 0.051(8) 0.021(8) -0.013(7) 0.002(7) 0.000(7) C56 0.046(8) 0.024(7) 0.055(9) 0.009(7) -0.003(7) 0.010(6) C61 0.025(6) 0.020(6) 0.028(8) 0.003(6) -0.005(6) 0.001(5) C62 0.058(9) 0.025(7) 0.052(9) -0.003(7) -0.011(7) 0.017(7) C63 0.060(9) 0.048(8) 0.045(9) -0.001(8) -0.018(7) 0.026(8) C64 0.065(9) 0.027(7) 0.037(9) 0.021(7) 0.016(7) 0.009(7) C65 0.042(7) 0.021(7) 0.035(8) -0.001(6) 0.013(7) -0.007(6) C66 0.047(7) 0.037(7) 0.015(7) 0.019(6) 0.003(6) 0.000(6) C71 0.009(6) 0.022(6) 0.046(8) 0.017(6) 0.002(6) -0.004(5) C72 0.057(8) 0.029(7) 0.030(8) -0.019(7) 0.003(7) -0.019(7) C73 0.060(9) 0.069(10) 0.021(8) -0.001(8) -0.005(7) -0.022(8) C74 0.046(8) 0.085(11) 0.021(8) 0.001(8) -0.003(6) 0.003(8) C75 0.030(7) 0.037(7) 0.052(9) 0.002(7) 0.010(7) 0.014(6) C76 0.033(7) 0.034(7) 0.020(7) 0.004(6) 0.006(6) 0.003(6) C81 0.029(7) 0.034(7) 0.030(7) -0.001(6) 0.012(6) 0.009(6) C82 0.030(7) 0.017(6) 0.041(8) 0.002(6) 0.007(6) 0.018(6) C83 0.033(7) 0.047(8) 0.068(9) -0.002(7) 0.013(7) -0.017(7) C84 0.017(7) 0.061(9) 0.065(10) -0.006(8) 0.017(7) 0.005(7) C85 0.042(9) 0.066(10) 0.082(11) -0.005(9) 0.038(8) 0.014(8) C86 0.058(9) 0.046(8) 0.067(10) -0.016(7) 0.021(8) -0.020(8) C91 0.42(11) 0.19(7) 0.07(4) 0.000 0.000 0.23(8) C92 0.41(8) 0.16(5) 0.03(2) -0.01(2) -0.07(3) 0.06(4) C93 0.063(15) 0.059(15) 0.22(3) 0.003(18) 0.002(19) -0.017(15) C94 0.11(2) 0.12(2) 0.10(2) 0.000(18) -0.03(2) -0.10(2) C95 0.26(4) 0.057(18) 0.12(2) -0.016(19) -0.07(3) 0.00(2) C96 0.18(3) 0.16(3) 0.23(4) 0.03(3) 0.14(3) -0.05(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 Se1 P1 2.120(3) . ? Se2 P2 2.096(3) . ? Se3 P3 2.096(3) . ? Se4 P4 2.128(3) . ? P1 C11 1.823(9) . ? P1 C21 1.838(10) . ? P1 C1 1.875(9) . ? P2 C41 1.807(9) . ? P2 C31 1.819(10) . ? P2 C2 1.847(9) . ? P3 C61 1.813(9) . ? P3 C51 1.843(9) . ? P3 C3 1.854(8) . ? P4 C71 1.804(9) . ? P4 C81 1.809(10) . ? P4 C4 1.826(9) . ? C1 C2 1.564(11) . ? C1 C4 1.603(11) . ? C2 C3 1.522(10) . ? C3 C4 1.570(11) . ? C11 C12 1.371(12) . ? C11 C16 1.431(12) . ? C12 C13 1.385(13) . ? C13 C14 1.391(15) . ? C14 C15 1.357(15) . ? C15 C16 1.373(12) . ? C21 C26 1.377(12) . ? C21 C22 1.411(12) . ? C22 C23 1.376(13) . ? C23 C24 1.373(12) . ? C24 C25 1.361(12) . ? C25 C26 1.411(12) . ? C31 C32 1.369(12) . ? C31 C36 1.371(13) . ? C32 C33 1.368(13) . ? C33 C34 1.397(15) . ? C34 C35 1.334(16) . ? C35 C36 1.396(14) . ? C41 C42 1.368(11) . ? C41 C46 1.406(12) . ? C42 C43 1.393(12) . ? C43 C44 1.383(13) . ? C44 C45 1.384(13) . ? C45 C46 1.379(12) . ? C51 C52 1.384(11) . ? C51 C56 1.387(12) . ? C52 C53 1.401(12) . ? C53 C54 1.342(12) . ? C54 C55 1.370(12) . ? C55 C56 1.392(12) . ? C61 C66 1.391(11) . ? C61 C62 1.399(12) . ? C62 C63 1.386(12) . ? C63 C64 1.400(12) . ? C64 C65 1.358(12) . ? C65 C66 1.376(11) . ? C71 C72 1.404(11) . ? C71 C76 1.409(11) . ? C72 C73 1.325(12) . ? C73 C74 1.383(13) . ? C74 C75 1.386(13) . ? C75 C76 1.388(12) . ? C81 C86 1.378(12) . ? C81 C82 1.400(11) . ? C82 C83 1.379(11) . ? C83 C84 1.376(12) . ? C84 C85 1.356(13) . ? C85 C86 1.382(13) . ? C91 C92 1.06(5) 6_334 ? C91 C92 1.06(5) . ? C91 C96 1.55(3) . ? C91 C96 1.55(3) 6_334 ? C92 C93 1.35(5) . ? C92 C96 1.64(5) 6_334 ? C92 C92 1.86(12) 6_334 ? C92 C94 1.97(7) . ? C93 C94 1.14(3) . ? C94 C95 1.18(3) . ? C95 C96 1.33(4) . ? C96 C92 1.64(5) 6_334 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 P1 C21 101.5(4) . . ? C11 P1 C1 103.7(5) . . ? C21 P1 C1 110.9(4) . . ? C11 P1 Se1 111.8(4) . . ? C21 P1 Se1 114.1(4) . . ? C1 P1 Se1 113.8(3) . . ? C41 P2 C31 101.2(4) . . ? C41 P2 C2 106.0(4) . . ? C31 P2 C2 102.9(5) . . ? C41 P2 Se2 113.1(3) . . ? C31 P2 Se2 116.3(4) . . ? C2 P2 Se2 115.7(3) . . ? C61 P3 C51 103.5(4) . . ? C61 P3 C3 104.7(4) . . ? C51 P3 C3 103.3(4) . . ? C61 P3 Se3 115.1(3) . . ? C51 P3 Se3 113.6(3) . . ? C3 P3 Se3 115.2(3) . . ? C71 P4 C81 103.4(4) . . ? C71 P4 C4 111.8(4) . . ? C81 P4 C4 103.1(4) . . ? C71 P4 Se4 112.2(3) . . ? C81 P4 Se4 111.1(3) . . ? C4 P4 Se4 114.2(3) . . ? C2 C1 C4 86.1(6) . . ? C2 C1 P1 126.3(7) . . ? C4 C1 P1 108.5(6) . . ? C3 C2 C1 88.7(6) . . ? C3 C2 P2 125.2(6) . . ? C1 C2 P2 123.4(6) . . ? C2 C3 C4 88.8(6) . . ? C2 C3 P3 123.9(6) . . ? C4 C3 P3 125.7(7) . . ? C3 C4 C1 85.6(6) . . ? C3 C4 P4 124.6(7) . . ? C1 C4 P4 110.6(6) . . ? C12 C11 C16 117.0(10) . . ? C12 C11 P1 118.6(10) . . ? C16 C11 P1 124.2(8) . . ? C11 C12 C13 122.3(12) . . ? C12 C13 C14 119.2(13) . . ? C15 C14 C13 120.2(12) . . ? C14 C15 C16 121.0(13) . . ? C15 C16 C11 120.4(11) . . ? C26 C21 C22 121.2(10) . . ? C26 C21 P1 118.6(9) . . ? C22 C21 P1 119.6(8) . . ? C23 C22 C21 117.7(11) . . ? C24 C23 C22 122.2(11) . . ? C25 C24 C23 119.6(11) . . ? C24 C25 C26 121.0(11) . . ? C21 C26 C25 118.3(10) . . ? C32 C31 C36 118.6(11) . . ? C32 C31 P2 124.5(9) . . ? C36 C31 P2 116.8(9) . . ? C33 C32 C31 122.0(12) . . ? C32 C33 C34 119.2(13) . . ? C35 C34 C33 118.8(14) . . ? C34 C35 C36 122.1(14) . . ? C31 C36 C35 119.2(12) . . ? C42 C41 C46 118.0(10) . . ? C42 C41 P2 123.0(8) . . ? C46 C41 P2 119.0(8) . . ? C41 C42 C43 121.7(10) . . ? C44 C43 C42 120.9(11) . . ? C43 C44 C45 117.0(11) . . ? C46 C45 C44 122.8(12) . . ? C45 C46 C41 119.5(11) . . ? C52 C51 C56 120.0(9) . . ? C52 C51 P3 118.6(8) . . ? C56 C51 P3 121.3(8) . . ? C51 C52 C53 118.7(10) . . ? C54 C53 C52 120.3(11) . . ? C53 C54 C55 122.1(11) . . ? C54 C55 C56 118.5(10) . . ? C51 C56 C55 120.2(10) . . ? C66 C61 C62 118.0(9) . . ? C66 C61 P3 123.4(8) . . ? C62 C61 P3 118.3(8) . . ? C63 C62 C61 120.2(10) . . ? C62 C63 C64 121.0(11) . . ? C65 C64 C63 117.7(10) . . ? C64 C65 C66 122.5(10) . . ? C65 C66 C61 120.4(10) . . ? C72 C71 C76 116.9(9) . . ? C72 C71 P4 123.3(8) . . ? C76 C71 P4 119.7(8) . . ? C73 C72 C71 121.6(10) . . ? C72 C73 C74 121.4(12) . . ? C73 C74 C75 120.4(11) . . ? C74 C75 C76 118.0(10) . . ? C75 C76 C71 121.8(10) . . ? C86 C81 C82 115.4(10) . . ? C86 C81 P4 119.8(8) . . ? C82 C81 P4 124.4(8) . . ? C83 C82 C81 122.6(9) . . ? C84 C83 C82 118.8(10) . . ? C85 C84 C83 120.7(11) . . ? C84 C85 C86 119.4(11) . . ? C81 C86 C85 122.9(11) . . ? C92 C91 C92 122(9) 6_334 . ? C92 C91 C96 75(3) 6_334 . ? C92 C91 C96 117(4) . . ? C92 C91 C96 117(4) 6_334 6_334 ? C92 C91 C96 75(3) . 6_334 ? C96 C91 C96 157(5) . 6_334 ? C91 C92 C93 130(6) . . ? C91 C92 C96 66(2) . 6_334 ? C93 C92 C96 132(4) . 6_334 ? C91 C92 C92 29(5) . 6_334 ? C93 C92 C92 140(7) . 6_334 ? C96 C92 C92 79(3) 6_334 6_334 ? C91 C92 C94 98(5) . . ? C93 C92 C94 34.1(19) . . ? C96 C92 C94 137(3) 6_334 . ? C92 C92 C94 107(5) 6_334 . ? C94 C93 C92 104(4) . . ? C93 C94 C95 137(4) . . ? C93 C94 C92 42(2) . . ? C95 C94 C92 96(3) . . ? C94 C95 C96 122(4) . . ? C95 C96 C91 103(2) . . ? C95 C96 C92 131(3) . 6_334 ? C91 C96 C92 39(2) . 6_334 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 P1 C1 C2 176.1(8) . . . . ? C21 P1 C1 C2 67.9(9) . . . . ? Se1 P1 C1 C2 -62.3(8) . . . . ? C11 P1 C1 C4 -84.9(6) . . . . ? C21 P1 C1 C4 166.9(6) . . . . ? Se1 P1 C1 C4 36.7(7) . . . . ? C4 C1 C2 C3 -24.5(7) . . . . ? P1 C1 C2 C3 85.7(8) . . . . ? C4 C1 C2 P2 -157.1(7) . . . . ? P1 C1 C2 P2 -46.9(10) . . . . ? C41 P2 C2 C3 87.9(8) . . . . ? C31 P2 C2 C3 -166.3(7) . . . . ? Se2 P2 C2 C3 -38.3(8) . . . . ? C41 P2 C2 C1 -156.4(7) . . . . ? C31 P2 C2 C1 -50.6(8) . . . . ? Se2 P2 C2 C1 77.3(7) . . . . ? C1 C2 C3 C4 25.0(7) . . . . ? P2 C2 C3 C4 156.2(7) . . . . ? C1 C2 C3 P3 158.6(7) . . . . ? P2 C2 C3 P3 -70.2(10) . . . . ? C61 P3 C3 C2 -173.4(8) . . . . ? C51 P3 C3 C2 78.6(8) . . . . ? Se3 P3 C3 C2 -45.9(9) . . . . ? C61 P3 C3 C4 -56.5(9) . . . . ? C51 P3 C3 C4 -164.5(7) . . . . ? Se3 P3 C3 C4 71.0(8) . . . . ? C2 C3 C4 C1 -24.4(7) . . . . ? P3 C3 C4 C1 -156.7(7) . . . . ? C2 C3 C4 P4 87.7(8) . . . . ? P3 C3 C4 P4 -44.5(11) . . . . ? C2 C1 C4 C3 23.8(6) . . . . ? P1 C1 C4 C3 -103.4(6) . . . . ? C2 C1 C4 P4 -101.7(6) . . . . ? P1 C1 C4 P4 131.1(5) . . . . ? C71 P4 C4 C3 64.8(9) . . . . ? C81 P4 C4 C3 175.3(8) . . . . ? Se4 P4 C4 C3 -64.0(8) . . . . ? C71 P4 C4 C1 164.1(6) . . . . ? C81 P4 C4 C1 -85.4(7) . . . . ? Se4 P4 C4 C1 35.3(7) . . . . ? C21 P1 C11 C12 -91.5(9) . . . . ? C1 P1 C11 C12 153.4(9) . . . . ? Se1 P1 C11 C12 30.4(10) . . . . ? C21 P1 C11 C16 84.7(9) . . . . ? C1 P1 C11 C16 -30.4(10) . . . . ? Se1 P1 C11 C16 -153.3(7) . . . . ? C16 C11 C12 C13 -1.7(17) . . . . ? P1 C11 C12 C13 174.8(9) . . . . ? C11 C12 C13 C14 1.7(19) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C14 C15 C16 C11 -1.1(17) . . . . ? C12 C11 C16 C15 1.3(15) . . . . ? P1 C11 C16 C15 -175.0(8) . . . . ? C11 P1 C21 C26 126.2(8) . . . . ? C1 P1 C21 C26 -124.2(8) . . . . ? Se1 P1 C21 C26 5.8(9) . . . . ? C11 P1 C21 C22 -45.3(9) . . . . ? C1 P1 C21 C22 64.3(9) . . . . ? Se1 P1 C21 C22 -165.6(7) . . . . ? C26 C21 C22 C23 2.1(15) . . . . ? P1 C21 C22 C23 173.4(8) . . . . ? C21 C22 C23 C24 -1.1(17) . . . . ? C22 C23 C24 C25 0.3(17) . . . . ? C23 C24 C25 C26 -0.4(16) . . . . ? C22 C21 C26 C25 -2.3(15) . . . . ? P1 C21 C26 C25 -173.6(8) . . . . ? C24 C25 C26 C21 1.4(16) . . . . ? C41 P2 C31 C32 80.9(10) . . . . ? C2 P2 C31 C32 -28.6(10) . . . . ? Se2 P2 C31 C32 -156.1(8) . . . . ? C41 P2 C31 C36 -95.2(9) . . . . ? C2 P2 C31 C36 155.3(9) . . . . ? Se2 P2 C31 C36 27.8(10) . . . . ? C36 C31 C32 C33 1.3(16) . . . . ? P2 C31 C32 C33 -174.8(8) . . . . ? C31 C32 C33 C34 -1.9(17) . . . . ? C32 C33 C34 C35 3(2) . . . . ? C33 C34 C35 C36 -3(2) . . . . ? C32 C31 C36 C35 -1.4(16) . . . . ? P2 C31 C36 C35 175.0(8) . . . . ? C34 C35 C36 C31 2.4(19) . . . . ? C31 P2 C41 C42 -69.2(9) . . . . ? C2 P2 C41 C42 37.8(9) . . . . ? Se2 P2 C41 C42 165.6(7) . . . . ? C31 P2 C41 C46 109.6(8) . . . . ? C2 P2 C41 C46 -143.4(8) . . . . ? Se2 P2 C41 C46 -15.6(9) . . . . ? C46 C41 C42 C43 -2.5(14) . . . . ? P2 C41 C42 C43 176.3(7) . . . . ? C41 C42 C43 C44 2.0(15) . . . . ? C42 C43 C44 C45 -1.2(16) . . . . ? C43 C44 C45 C46 1.0(18) . . . . ? C44 C45 C46 C41 -1.6(17) . . . . ? C42 C41 C46 C45 2.3(15) . . . . ? P2 C41 C46 C45 -176.6(8) . . . . ? C61 P3 C51 C52 128.6(8) . . . . ? C3 P3 C51 C52 -122.5(8) . . . . ? Se3 P3 C51 C52 3.1(8) . . . . ? C61 P3 C51 C56 -47.0(9) . . . . ? C3 P3 C51 C56 62.0(9) . . . . ? Se3 P3 C51 C56 -172.5(7) . . . . ? C56 C51 C52 C53 -4.6(15) . . . . ? P3 C51 C52 C53 179.8(7) . . . . ? C51 C52 C53 C54 3.5(16) . . . . ? C52 C53 C54 C55 -2.1(18) . . . . ? C53 C54 C55 C56 1.7(17) . . . . ? C52 C51 C56 C55 4.3(15) . . . . ? P3 C51 C56 C55 179.8(7) . . . . ? C54 C55 C56 C51 -2.7(16) . . . . ? C51 P3 C61 C66 81.4(9) . . . . ? C3 P3 C61 C66 -26.5(9) . . . . ? Se3 P3 C61 C66 -154.0(7) . . . . ? C51 P3 C61 C62 -93.6(8) . . . . ? C3 P3 C61 C62 158.5(8) . . . . ? Se3 P3 C61 C62 30.9(9) . . . . ? C66 C61 C62 C63 0.7(15) . . . . ? P3 C61 C62 C63 176.0(8) . . . . ? C61 C62 C63 C64 1.8(17) . . . . ? C62 C63 C64 C65 -2.2(16) . . . . ? C63 C64 C65 C66 0.1(16) . . . . ? C64 C65 C66 C61 2.4(16) . . . . ? C62 C61 C66 C65 -2.7(15) . . . . ? P3 C61 C66 C65 -177.8(7) . . . . ? C81 P4 C71 C72 116.8(8) . . . . ? C4 P4 C71 C72 -132.9(8) . . . . ? Se4 P4 C71 C72 -3.1(9) . . . . ? C81 P4 C71 C76 -58.4(8) . . . . ? C4 P4 C71 C76 51.9(8) . . . . ? Se4 P4 C71 C76 -178.3(6) . . . . ? C76 C71 C72 C73 1.1(15) . . . . ? P4 C71 C72 C73 -174.3(8) . . . . ? C71 C72 C73 C74 -2.6(18) . . . . ? C72 C73 C74 C75 2.2(18) . . . . ? C73 C74 C75 C76 -0.4(16) . . . . ? C74 C75 C76 C71 -1.0(14) . . . . ? C72 C71 C76 C75 0.7(14) . . . . ? P4 C71 C76 C75 176.3(7) . . . . ? C71 P4 C81 C86 -96.3(9) . . . . ? C4 P4 C81 C86 147.1(9) . . . . ? Se4 P4 C81 C86 24.3(10) . . . . ? C71 P4 C81 C82 75.9(10) . . . . ? C4 P4 C81 C82 -40.7(10) . . . . ? Se4 P4 C81 C82 -163.5(8) . . . . ? C86 C81 C82 C83 -2.3(16) . . . . ? P4 C81 C82 C83 -174.8(8) . . . . ? C81 C82 C83 C84 3.4(17) . . . . ? C82 C83 C84 C85 -1.8(18) . . . . ? C83 C84 C85 C86 -1(2) . . . . ? C82 C81 C86 C85 -0.4(17) . . . . ? P4 C81 C86 C85 172.4(9) . . . . ? C84 C85 C86 C81 2(2) . . . . ? C92 C91 C92 C93 122(7) 6_334 . . . ? C96 C91 C92 C93 34(10) . . . . ? C96 C91 C92 C93 -125(6) 6_334 . . . ? C92 C91 C92 C96 -112(3) 6_334 . . 6_334 ? C96 C91 C92 C96 159(6) . . . 6_334 ? C96 C91 C92 C92 -89(5) . . . 6_334 ? C96 C91 C92 C92 112(3) 6_334 . . 6_334 ? C92 C91 C92 C94 110(3) 6_334 . . . ? C96 C91 C92 C94 21(6) . . . . ? C96 C91 C92 C94 -138(2) 6_334 . . . ? C91 C92 C93 C94 -23(8) . . . . ? C96 C92 C93 C94 -115(7) 6_334 . . . ? C92 C92 C93 C94 16(5) 6_334 . . . ? C92 C93 C94 C95 1(6) . . . . ? C91 C92 C94 C93 163(6) . . . . ? C96 C92 C94 C93 99(7) 6_334 . . . ? C92 C92 C94 C93 -169(3) 6_334 . . . ? C91 C92 C94 C95 -17(5) . . . . ? C93 C92 C94 C95 -179(4) . . . . ? C96 C92 C94 C95 -80(6) 6_334 . . . ? C92 C92 C94 C95 11(3) 6_334 . . . ? C93 C94 C95 C96 3(7) . . . . ? C92 C94 C95 C96 4(4) . . . . ? C94 C95 C96 C91 6(5) . . . . ? C94 C95 C96 C92 -25(7) . . . 6_334 ? C92 C91 C96 C95 -141(5) 6_334 . . . ? C92 C91 C96 C95 -22(7) . . . . ? C96 C91 C96 C95 94(3) 6_334 . . . ? C92 C91 C96 C92 119(10) . . . 6_334 ? C96 C91 C96 C92 -124(4) 6_334 . . 6_334 ? _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction 0.990 _refine_diff_density_max 0.280 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.070 #===END data_V _database_code_CSD 211321 _audit_creation_method SHELXL-97 _chemical_name_systematic trans-dppcbSe2S2 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 P4 S2 Se2 x 0.5 C7 H8' _chemical_formula_sum 'C55.5 H48 P4 S2 Se2' _chemical_formula_weight 1060.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 38.688(1) _cell_length_b 38.688(1) _cell_length_c 13.1777(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19724(1) _cell_formula_units_Z 16 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 22057 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description 'rectangular solid' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8656 _exptl_absorpt_coefficient_mu 1.748 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 213(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 'Kappa CCD' _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_% 0 _diffrn_reflns_number 17829 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6042 _reflns_number_gt 4499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0370P)^2^+23.8496P] 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 6042 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 P1 P 0.35541(3) 0.32566(3) 0.29795(8) 0.0402(3) Uani 1 1 d . . . P2 P 0.33232(3) 0.41675(3) 0.20215(7) 0.0352(3) Uani 1 1 d . . . P3 P 0.37911(3) 0.38127(3) -0.04784(8) 0.0404(3) Uani 1 1 d . . . P4 P 0.31849(3) 0.30368(3) 0.00030(8) 0.0415(3) Uani 1 1 d . . . Se1 Se 0.4095(3) 0.3230(3) 0.2848(9) 0.0507(14) Uani 0.37 1 d P . . S1 S 0.4058(4) 0.3295(3) 0.2758(12) 0.0424(15) Uani 0.63 1 d P . . Se2 Se 0.37538(6) 0.42851(6) 0.2891(2) 0.0411(6) Uani 0.63 1 d P . . S2 S 0.3744(4) 0.4266(4) 0.2863(12) 0.092(5) Uani 0.37 1 d P . . Se3 Se 0.34070(14) 0.39562(7) -0.1454(3) 0.0443(11) Uani 0.37 1 d P . . S3 S 0.3429(3) 0.39511(19) -0.1462(7) 0.095(3) Uani 0.63 1 d P . . S4 S 0.2752(4) 0.3277(5) -0.0187(11) 0.0340(18) Uani 0.37 1 d P . . Se4 Se 0.26877(9) 0.32738(12) 0.0048(2) 0.0425(6) Uani 0.63 1 d P . . C1 C 0.33104(10) 0.33857(10) 0.1833(3) 0.0336(9) Uani 1 1 d . . . C2 C 0.33304(10) 0.37532(10) 0.1343(3) 0.0331(9) Uani 1 1 d . . . C3 C 0.36451(10) 0.36258(9) 0.0723(3) 0.0347(9) Uani 1 1 d . . . C4 C 0.35016(10) 0.32489(10) 0.0859(3) 0.0364(10) Uani 1 1 d . . . C11 C 0.33897(12) 0.28203(10) 0.3228(3) 0.0442(11) Uani 1 1 d . . . C12 C 0.30459(12) 0.27265(11) 0.3106(3) 0.0514(12) Uani 1 1 d . . . H12A H 0.2891 0.2884 0.2829 0.062 Uiso 1 1 calc R . . C13 C 0.29311(14) 0.24044(13) 0.3388(4) 0.0662(14) Uani 1 1 d . . . H13A H 0.2700 0.2346 0.3303 0.079 Uiso 1 1 calc R . . C14 C 0.31587(18) 0.21667(14) 0.3799(4) 0.0790(17) Uani 1 1 d . . . H14A H 0.3081 0.1948 0.3986 0.095 Uiso 1 1 calc R . . C15 C 0.34977(18) 0.22537(14) 0.3928(4) 0.0822(18) Uani 1 1 d . . . H15A H 0.3650 0.2096 0.4216 0.099 Uiso 1 1 calc R . . C16 C 0.36176(13) 0.25803(13) 0.3630(3) 0.0656(14) Uani 1 1 d . . . H16A H 0.3850 0.2636 0.3701 0.079 Uiso 1 1 calc R . . C21 C 0.34013(11) 0.34978(10) 0.4078(3) 0.0421(10) Uani 1 1 d . . . C22 C 0.36409(12) 0.36435(12) 0.4737(3) 0.0527(12) Uani 1 1 d . . . H22A H 0.3876 0.3630 0.4591 0.063 Uiso 1 1 calc R . . C23 C 0.35304(14) 0.38087(13) 0.5608(3) 0.0609(14) Uani 1 1 d . . . H23A H 0.3691 0.3905 0.6051 0.073 Uiso 1 1 calc R . . C24 C 0.31879(15) 0.38300(12) 0.5818(3) 0.0625(14) Uani 1 1 d . . . H24A H 0.3116 0.3943 0.6403 0.075 Uiso 1 1 calc R . . C25 C 0.29440(13) 0.36862(12) 0.5176(3) 0.0563(12) Uani 1 1 d . . . H25A H 0.2710 0.3702 0.5327 0.068 Uiso 1 1 calc R . . C26 C 0.30544(11) 0.35178(11) 0.4301(3) 0.0452(11) Uani 1 1 d . . . H26A H 0.2893 0.3418 0.3866 0.054 Uiso 1 1 calc R . . C31 C 0.29160(10) 0.41616(10) 0.2712(3) 0.0383(10) Uani 1 1 d . . . C32 C 0.26318(11) 0.39682(11) 0.2408(3) 0.0452(11) Uani 1 1 d . . . H32A H 0.2648 0.3828 0.1837 0.054 Uiso 1 1 calc R . . C33 C 0.23248(11) 0.39825(12) 0.2945(3) 0.0539(12) Uani 1 1 d . . . H33A H 0.2136 0.3851 0.2741 0.065 Uiso 1 1 calc R . . C34 C 0.23016(13) 0.41942(13) 0.3787(4) 0.0638(14) Uani 1 1 d . . . H34A H 0.2098 0.4201 0.4162 0.077 Uiso 1 1 calc R . . C35 C 0.25774(13) 0.43939(13) 0.4069(3) 0.0628(14) Uani 1 1 d . . . H35A H 0.2556 0.4542 0.4621 0.075 Uiso 1 1 calc R . . C36 C 0.28844(12) 0.43783(11) 0.3551(3) 0.0487(11) Uani 1 1 d . . . H36A H 0.3071 0.4512 0.3759 0.058 Uiso 1 1 calc R . . C41 C 0.32421(11) 0.44858(10) 0.1034(3) 0.0399(10) Uani 1 1 d . . . C42 C 0.34684(12) 0.47554(11) 0.0917(3) 0.0552(12) Uani 1 1 d . . . H42A H 0.3663 0.4772 0.1328 0.066 Uiso 1 1 calc R . . C43 C 0.34041(16) 0.50039(13) 0.0180(4) 0.0741(16) Uani 1 1 d . . . H43A H 0.3556 0.5189 0.0103 0.089 Uiso 1 1 calc R . . C44 C 0.31196(15) 0.49795(13) -0.0438(3) 0.0662(15) Uani 1 1 d . . . H44A H 0.3082 0.5145 -0.0938 0.079 Uiso 1 1 calc R . . C45 C 0.28913(13) 0.47143(13) -0.0322(3) 0.0616(13) Uani 1 1 d . . . H45A H 0.2696 0.4701 -0.0733 0.074 Uiso 1 1 calc R . . C46 C 0.29519(12) 0.44634(11) 0.0414(3) 0.0519(12) Uani 1 1 d . . . H46A H 0.2798 0.4281 0.0492 0.062 Uiso 1 1 calc R . . C51 C 0.40765(11) 0.41670(10) -0.0144(3) 0.0413(10) Uani 1 1 d . . . C52 C 0.43137(12) 0.41491(12) 0.0645(4) 0.0559(12) Uani 1 1 d . . . H52A H 0.4320 0.3953 0.1054 0.067 Uiso 1 1 calc R . . C53 C 0.45410(13) 0.44165(13) 0.0834(4) 0.0645(14) Uani 1 1 d . . . H53A H 0.4700 0.4399 0.1362 0.077 Uiso 1 1 calc R . . C54 C 0.45326(14) 0.47079(13) 0.0243(4) 0.0676(15) Uani 1 1 d . . . H54A H 0.4683 0.4890 0.0371 0.081 Uiso 1 1 calc R . . C55 C 0.42995(17) 0.47276(14) -0.0541(4) 0.0856(18) Uani 1 1 d . . . H55A H 0.4296 0.4923 -0.0951 0.103 Uiso 1 1 calc R . . C56 C 0.40701(14) 0.44614(12) -0.0729(4) 0.0701(15) Uani 1 1 d . . . H56A H 0.3911 0.4481 -0.1255 0.084 Uiso 1 1 calc R . . C61 C 0.40949(12) 0.34916(11) -0.0950(3) 0.0483(12) Uani 1 1 d . . . C62 C 0.41523(14) 0.34752(13) -0.1978(4) 0.0725(16) Uani 1 1 d . . . H62A H 0.4023 0.3613 -0.2416 0.087 Uiso 1 1 calc R . . C63 C 0.43998(19) 0.32562(17) -0.2360(5) 0.100(2) Uani 1 1 d . . . H63A H 0.4443 0.3253 -0.3054 0.120 Uiso 1 1 calc R . . C64 C 0.45837(15) 0.30429(16) -0.1734(6) 0.093(2) Uani 1 1 d . . . H64A H 0.4744 0.2890 -0.2003 0.112 Uiso 1 1 calc R . . C65 C 0.45296(13) 0.30564(14) -0.0704(5) 0.0801(17) Uani 1 1 d . . . H65A H 0.4657 0.2915 -0.0275 0.096 Uiso 1 1 calc R . . C66 C 0.42857(11) 0.32803(12) -0.0302(4) 0.0579(13) Uani 1 1 d . . . H66A H 0.4250 0.3289 0.0395 0.069 Uiso 1 1 calc R . . C71 C 0.33625(11) 0.29609(10) -0.1257(3) 0.0421(10) Uani 1 1 d . . . C72 C 0.31924(12) 0.30921(11) -0.2097(3) 0.0517(12) Uani 1 1 d . . . H72A H 0.3002 0.3236 -0.2011 0.062 Uiso 1 1 calc R . . C73 C 0.33046(14) 0.30097(12) -0.3061(3) 0.0608(14) Uani 1 1 d . . . H73A H 0.3191 0.3102 -0.3621 0.073 Uiso 1 1 calc R . . C74 C 0.35795(14) 0.27953(13) -0.3203(3) 0.0633(14) Uani 1 1 d . . . H74A H 0.3651 0.2739 -0.3856 0.076 Uiso 1 1 calc R . . C75 C 0.37519(13) 0.26618(12) -0.2374(3) 0.0599(13) Uani 1 1 d . . . H75A H 0.3942 0.2518 -0.2468 0.072 Uiso 1 1 calc R . . C76 C 0.36423(11) 0.27425(11) -0.1397(3) 0.0496(11) Uani 1 1 d . . . H76A H 0.3757 0.2650 -0.0839 0.060 Uiso 1 1 calc R . . C81 C 0.31638(12) 0.25954(11) 0.0502(3) 0.0472(11) Uani 1 1 d . . . C82 C 0.28569(14) 0.24170(13) 0.0345(4) 0.0683(15) Uani 1 1 d . . . H82A H 0.2669 0.2527 0.0048 0.082 Uiso 1 1 calc R . . C83 C 0.28334(19) 0.20709(16) 0.0639(5) 0.095(2) Uani 1 1 d . . . H83A H 0.2628 0.1951 0.0541 0.114 Uiso 1 1 calc R . . C84 C 0.3114(2) 0.19038(16) 0.1075(5) 0.099(2) Uani 1 1 d . . . H84A H 0.3097 0.1672 0.1256 0.119 Uiso 1 1 calc R . . C85 C 0.34109(17) 0.20798(13) 0.1235(4) 0.0825(18) Uani 1 1 d . . . H85A H 0.3597 0.1970 0.1542 0.099 Uiso 1 1 calc R . . C86 C 0.34399(14) 0.24225(12) 0.0945(4) 0.0629(14) Uani 1 1 d . . . H86A H 0.3647 0.2539 0.1049 0.075 Uiso 1 1 calc R . . C91 C 0.4558(7) 0.2160(5) 0.2488(11) 0.143(10) Uani 0.50 1 d P . . C92 C 0.4664(5) 0.2549(6) 0.2347(12) 0.262(11) Uani 1 1 d . . . C93 C 0.5000 0.2500 0.2201(10) 0.178(8) Uani 1 2 d S . . C94 C 0.4886(7) 0.2874(15) 0.1846(15) 0.26(2) Uani 0.50 1 d P . . C95 C 0.5031(7) 0.3009(4) 0.2112(14) 0.106(9) Uani 0.50 1 d P . . C96 C 0.5282(5) 0.3076(4) 0.2246(10) 0.082(4) Uani 0.50 1 d P . . H1 H 0.3066(10) 0.3306(10) 0.191(3) 0.050 Uiso 1 1 d . . . H2 H 0.3122(10) 0.3761(10) 0.095(3) 0.050 Uiso 1 1 d . . . H3 H 0.3855(10) 0.3645(10) 0.115(3) 0.050 Uiso 1 1 d . . . H4 H 0.3678(10) 0.3092(10) 0.096(3) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0346(7) 0.0404(7) 0.0456(6) 0.0084(5) -0.0023(5) 0.0031(5) P2 0.0361(6) 0.0308(6) 0.0388(6) 0.0008(5) -0.0016(5) 0.0007(5) P3 0.0458(7) 0.0342(6) 0.0414(6) -0.0002(5) 0.0066(5) -0.0027(5) P4 0.0387(7) 0.0337(6) 0.0520(7) -0.0055(5) 0.0014(5) -0.0024(5) Se1 0.028(2) 0.059(3) 0.065(2) 0.0249(19) -0.0079(15) 0.013(2) S1 0.029(3) 0.046(4) 0.052(3) 0.017(3) -0.0131(18) 0.014(2) Se2 0.0340(11) 0.0405(10) 0.0489(15) 0.0011(8) -0.0096(9) -0.0033(8) S2 0.093(10) 0.116(10) 0.066(9) -0.012(7) -0.018(7) -0.005(7) Se3 0.060(2) 0.0347(14) 0.038(2) 0.0021(13) -0.0107(17) -0.0062(14) S3 0.082(6) 0.136(5) 0.066(6) 0.003(4) -0.003(4) -0.007(4) S4 0.012(3) 0.056(3) 0.034(5) -0.015(3) 0.018(2) 0.002(3) Se4 0.0261(13) 0.0520(7) 0.0494(17) -0.0132(11) 0.0037(8) 0.0007(9) C1 0.031(2) 0.028(2) 0.042(2) 0.0034(18) -0.0010(18) -0.0007(18) C2 0.032(2) 0.028(2) 0.039(2) 0.0045(17) -0.0014(18) 0.0010(19) C3 0.033(2) 0.027(2) 0.044(2) 0.0019(18) 0.0033(18) -0.0004(19) C4 0.034(2) 0.034(2) 0.041(2) 0.0020(18) 0.0022(19) 0.0076(19) C11 0.057(3) 0.033(2) 0.042(2) 0.0089(19) 0.002(2) 0.010(2) C12 0.051(3) 0.038(3) 0.065(3) 0.011(2) 0.007(2) -0.001(2) C13 0.072(4) 0.052(3) 0.074(3) 0.010(3) 0.015(3) -0.003(3) C14 0.109(5) 0.046(3) 0.083(4) 0.019(3) 0.010(4) -0.005(3) C15 0.108(5) 0.049(4) 0.089(4) 0.027(3) -0.009(4) 0.022(3) C16 0.065(4) 0.062(4) 0.070(3) 0.017(3) -0.008(3) 0.014(3) C21 0.042(3) 0.043(3) 0.041(2) 0.010(2) 0.000(2) 0.004(2) C22 0.049(3) 0.060(3) 0.049(3) 0.005(2) -0.010(2) -0.007(2) C23 0.071(4) 0.069(4) 0.043(3) 0.000(2) -0.005(2) -0.013(3) C24 0.086(4) 0.055(3) 0.046(3) -0.002(2) 0.010(3) 0.001(3) C25 0.054(3) 0.053(3) 0.062(3) 0.007(2) 0.013(3) 0.003(2) C26 0.047(3) 0.047(3) 0.042(2) 0.005(2) -0.002(2) 0.004(2) C31 0.037(3) 0.034(2) 0.044(2) 0.0080(19) -0.0004(19) 0.006(2) C32 0.043(3) 0.042(3) 0.051(3) 0.004(2) -0.001(2) 0.001(2) C33 0.037(3) 0.059(3) 0.066(3) 0.006(3) -0.001(2) -0.002(2) C34 0.046(3) 0.077(4) 0.068(3) 0.012(3) 0.017(3) 0.019(3) C35 0.063(4) 0.071(4) 0.054(3) -0.002(3) 0.005(3) 0.018(3) C36 0.054(3) 0.047(3) 0.045(3) -0.008(2) 0.000(2) 0.006(2) C41 0.055(3) 0.027(2) 0.037(2) -0.0019(18) 0.000(2) 0.005(2) C42 0.064(3) 0.043(3) 0.058(3) 0.006(2) -0.004(2) -0.008(3) C43 0.105(5) 0.041(3) 0.076(4) 0.014(3) 0.003(3) -0.012(3) C44 0.095(4) 0.052(3) 0.052(3) 0.013(2) -0.001(3) 0.013(3) C45 0.073(4) 0.054(3) 0.058(3) 0.008(3) -0.017(3) 0.006(3) C46 0.058(3) 0.042(3) 0.055(3) 0.008(2) -0.013(2) 0.000(2) C51 0.051(3) 0.028(2) 0.045(2) -0.0026(19) 0.012(2) 0.000(2) C52 0.054(3) 0.042(3) 0.072(3) 0.003(2) 0.003(3) -0.006(2) C53 0.058(3) 0.048(3) 0.088(4) -0.008(3) -0.004(3) -0.009(3) C54 0.068(4) 0.053(3) 0.082(4) -0.016(3) 0.017(3) -0.023(3) C55 0.121(5) 0.057(4) 0.080(4) 0.014(3) 0.001(4) -0.033(3) C56 0.100(5) 0.045(3) 0.065(3) 0.006(2) -0.010(3) -0.023(3) C61 0.052(3) 0.038(3) 0.055(3) -0.011(2) 0.019(2) -0.008(2) C62 0.084(4) 0.060(4) 0.074(4) -0.011(3) 0.034(3) 0.001(3) C63 0.105(6) 0.080(5) 0.116(5) -0.027(4) 0.059(5) -0.010(4) C64 0.060(4) 0.059(4) 0.161(7) -0.053(4) 0.043(4) -0.007(3) C65 0.042(3) 0.061(4) 0.137(5) -0.032(4) -0.002(3) 0.003(3) C66 0.038(3) 0.047(3) 0.089(4) -0.017(3) 0.008(3) -0.003(2) C71 0.046(3) 0.034(2) 0.046(2) -0.006(2) -0.005(2) -0.009(2) C72 0.060(3) 0.040(3) 0.055(3) -0.002(2) -0.008(2) 0.000(2) C73 0.083(4) 0.048(3) 0.051(3) -0.003(2) -0.012(3) -0.004(3) C74 0.082(4) 0.059(3) 0.049(3) -0.012(2) 0.005(3) 0.002(3) C75 0.067(3) 0.051(3) 0.062(3) -0.010(2) 0.011(3) 0.010(3) C76 0.048(3) 0.045(3) 0.055(3) -0.005(2) -0.001(2) 0.004(2) C81 0.056(3) 0.035(3) 0.051(3) -0.006(2) 0.017(2) -0.006(2) C82 0.072(4) 0.053(3) 0.080(4) -0.014(3) 0.016(3) -0.024(3) C83 0.112(6) 0.064(4) 0.109(5) -0.023(4) 0.032(4) -0.046(4) C84 0.141(7) 0.040(4) 0.116(5) 0.005(3) 0.055(5) -0.011(4) C85 0.108(5) 0.039(3) 0.101(4) 0.002(3) 0.036(4) 0.003(3) C86 0.075(4) 0.037(3) 0.076(3) 0.004(2) 0.019(3) 0.002(3) C91 0.30(3) 0.049(9) 0.083(10) -0.006(8) -0.015(12) -0.035(14) C92 0.234(18) 0.37(3) 0.176(13) -0.112(15) -0.050(12) 0.18(2) C93 0.136(15) 0.34(3) 0.062(8) 0.000 0.000 -0.054(16) C94 0.092(17) 0.64(7) 0.041(9) 0.03(2) 0.007(11) 0.17(3) C95 0.16(2) 0.061(10) 0.098(14) -0.008(8) 0.007(13) -0.064(13) C96 0.097(12) 0.076(11) 0.072(8) 0.004(8) -0.003(8) -0.015(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 P1 C21 1.822(4) . ? P1 C11 1.833(4) . ? P1 C1 1.850(4) . ? P1 S1 1.977(17) . ? P1 Se1 2.104(11) . ? P2 C41 1.819(4) . ? P2 C31 1.819(4) . ? P2 C2 1.836(4) . ? P2 S2 2.006(16) . ? P2 Se2 2.073(3) . ? P3 C51 1.815(4) . ? P3 C61 1.819(4) . ? P3 C3 1.830(4) . ? P3 S3 1.983(9) . ? P3 Se3 2.042(5) . ? P4 C71 1.821(4) . ? P4 C81 1.832(4) . ? P4 C4 1.856(4) . ? P4 S4 1.933(17) . ? P4 Se4 2.132(4) . ? C1 C2 1.563(5) . ? C1 C4 1.573(5) . ? C2 C3 1.547(5) . ? C3 C4 1.570(5) . ? C11 C16 1.386(6) . ? C11 C12 1.388(6) . ? C12 C13 1.374(6) . ? C13 C14 1.383(7) . ? C14 C15 1.364(7) . ? C15 C16 1.403(7) . ? C21 C26 1.376(5) . ? C21 C22 1.389(6) . ? C22 C23 1.383(6) . ? C23 C24 1.356(6) . ? C24 C25 1.384(6) . ? C25 C26 1.391(6) . ? C31 C32 1.389(6) . ? C31 C36 1.392(5) . ? C32 C33 1.383(6) . ? C33 C34 1.383(6) . ? C34 C35 1.369(7) . ? C35 C36 1.372(6) . ? C41 C42 1.370(6) . ? C41 C46 1.391(5) . ? C42 C43 1.389(6) . ? C43 C44 1.372(7) . ? C44 C45 1.362(7) . ? C45 C46 1.393(6) . ? C51 C56 1.376(6) . ? C51 C52 1.388(6) . ? C52 C53 1.380(6) . ? C53 C54 1.371(7) . ? C54 C55 1.373(7) . ? C55 C56 1.382(7) . ? C61 C62 1.375(6) . ? C61 C66 1.393(6) . ? C62 C63 1.374(8) . ? C63 C64 1.367(9) . ? C64 C65 1.374(8) . ? C65 C66 1.386(7) . ? C71 C72 1.384(6) . ? C71 C76 1.386(6) . ? C72 C73 1.380(6) . ? C73 C74 1.362(7) . ? C74 C75 1.380(6) . ? C75 C76 1.391(6) . ? C81 C82 1.389(6) . ? C81 C86 1.389(6) . ? C82 C83 1.397(7) . ? C83 C84 1.386(9) . ? C84 C85 1.353(8) . ? C85 C86 1.384(6) . ? C91 C96 1.15(3) 6_554 ? C91 C92 1.57(2) . ? C91 C95 1.79(3) 6_554 ? C92 C93 1.326(16) . ? C92 C94 1.66(4) . ? C93 C92 1.326(16) 6_554 ? C93 C94 1.59(5) 6_554 ? C93 C94 1.59(5) . ? C93 C95 1.978(17) 6_554 ? C93 C95 1.978(17) . ? C94 C95 0.84(5) . ? C94 C96 1.80(4) . ? C95 C96 1.02(2) . ? C95 C91 1.79(3) 6_554 ? C96 C91 1.15(3) 6_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 P1 C11 102.54(19) . . ? C21 P1 C1 110.22(18) . . ? C11 P1 C1 102.58(18) . . ? C21 P1 S1 113.5(5) . . ? C11 P1 S1 116.0(4) . . ? C1 P1 S1 111.2(4) . . ? C21 P1 Se1 114.5(4) . . ? C11 P1 Se1 108.3(3) . . ? C1 P1 Se1 117.0(3) . . ? S1 P1 Se1 8.1(6) . . ? C41 P2 C31 102.53(18) . . ? C41 P2 C2 104.20(17) . . ? C31 P2 C2 104.23(18) . . ? C41 P2 S2 114.0(4) . . ? C31 P2 S2 115.4(5) . . ? C2 P2 S2 115.1(5) . . ? C41 P2 Se2 112.68(15) . . ? C31 P2 Se2 114.97(15) . . ? C2 P2 Se2 116.67(15) . . ? S2 P2 Se2 1.7(5) . . ? C51 P3 C61 101.86(19) . . ? C51 P3 C3 106.02(18) . . ? C61 P3 C3 103.01(19) . . ? C51 P3 S3 112.6(3) . . ? C61 P3 S3 114.7(3) . . ? C3 P3 S3 117.0(3) . . ? C51 P3 Se3 112.98(17) . . ? C61 P3 Se3 116.14(19) . . ? C3 P3 Se3 115.33(19) . . ? S3 P3 Se3 1.8(4) . . ? C71 P4 C81 101.18(18) . . ? C71 P4 C4 112.12(18) . . ? C81 P4 C4 102.9(2) . . ? C71 P4 S4 106.7(4) . . ? C81 P4 S4 117.2(5) . . ? C4 P4 S4 116.0(6) . . ? C71 P4 Se4 115.77(17) . . ? C81 P4 Se4 110.53(18) . . ? C4 P4 Se4 112.87(17) . . ? S4 P4 Se4 9.7(4) . . ? C2 C1 C4 86.9(3) . . ? C2 C1 P1 123.9(3) . . ? C4 C1 P1 109.6(3) . . ? C3 C2 C1 88.1(3) . . ? C3 C2 P2 123.2(3) . . ? C1 C2 P2 126.3(3) . . ? C2 C3 C4 87.6(3) . . ? C2 C3 P3 125.0(3) . . ? C4 C3 P3 125.1(3) . . ? C3 C4 C1 86.9(3) . . ? C3 C4 P4 125.1(3) . . ? C1 C4 P4 109.5(3) . . ? C16 C11 C12 118.6(4) . . ? C16 C11 P1 117.7(4) . . ? C12 C11 P1 123.5(3) . . ? C13 C12 C11 121.0(4) . . ? C12 C13 C14 120.2(5) . . ? C15 C14 C13 119.8(5) . . ? C14 C15 C16 120.3(5) . . ? C11 C16 C15 120.0(5) . . ? C26 C21 C22 119.7(4) . . ? C26 C21 P1 121.0(3) . . ? C22 C21 P1 119.2(3) . . ? C23 C22 C21 120.0(4) . . ? C24 C23 C22 119.9(4) . . ? C23 C24 C25 121.2(4) . . ? C24 C25 C26 119.0(4) . . ? C21 C26 C25 120.2(4) . . ? C32 C31 C36 118.9(4) . . ? C32 C31 P2 123.2(3) . . ? C36 C31 P2 117.7(3) . . ? C33 C32 C31 120.7(4) . . ? C34 C33 C32 119.3(4) . . ? C35 C34 C33 120.1(4) . . ? C34 C35 C36 121.0(5) . . ? C35 C36 C31 119.9(4) . . ? C42 C41 C46 119.8(4) . . ? C42 C41 P2 119.1(3) . . ? C46 C41 P2 121.1(3) . . ? C41 C42 C43 119.4(5) . . ? C44 C43 C42 120.7(5) . . ? C45 C44 C43 120.4(5) . . ? C44 C45 C46 119.6(5) . . ? C41 C46 C45 120.1(4) . . ? C56 C51 C52 118.2(4) . . ? C56 C51 P3 118.5(4) . . ? C52 C51 P3 123.1(3) . . ? C53 C52 C51 121.2(4) . . ? C54 C53 C52 119.9(5) . . ? C53 C54 C55 119.2(5) . . ? C54 C55 C56 121.0(5) . . ? C51 C56 C55 120.3(5) . . ? C62 C61 C66 119.4(4) . . ? C62 C61 P3 118.2(4) . . ? C66 C61 P3 122.3(3) . . ? C63 C62 C61 120.1(6) . . ? C64 C63 C62 120.9(6) . . ? C63 C64 C65 119.6(6) . . ? C64 C65 C66 120.3(6) . . ? C65 C66 C61 119.6(5) . . ? C72 C71 C76 119.3(4) . . ? C72 C71 P4 119.4(3) . . ? C76 C71 P4 120.9(3) . . ? C73 C72 C71 120.1(4) . . ? C74 C73 C72 120.9(4) . . ? C73 C74 C75 119.8(4) . . ? C74 C75 C76 120.1(5) . . ? C71 C76 C75 119.9(4) . . ? C82 C81 C86 118.7(5) . . ? C82 C81 P4 116.6(4) . . ? C86 C81 P4 124.4(4) . . ? C81 C82 C83 119.4(6) . . ? C84 C83 C82 120.7(6) . . ? C85 C84 C83 119.6(6) . . ? C84 C85 C86 120.5(6) . . ? C85 C86 C81 121.0(5) . . ? C96 C91 C92 126(2) 6_554 . ? C96 C91 C95 32.1(12) 6_554 6_554 ? C92 C91 C95 94.8(15) . 6_554 ? C93 C92 C91 97.9(13) . . ? C93 C92 C94 63.0(15) . . ? C91 C92 C94 155(2) . . ? C92 C93 C92 163.3(19) 6_554 . ? C92 C93 C94 68.8(12) 6_554 6_554 ? C92 C93 C94 116.5(14) . 6_554 ? C92 C93 C94 116.5(14) 6_554 . ? C92 C93 C94 68.8(12) . . ? C94 C93 C94 146(2) 6_554 . ? C92 C93 C95 85.8(11) 6_554 6_554 ? C92 C93 C95 95.2(11) . 6_554 ? C94 C93 C95 24.4(13) 6_554 6_554 ? C94 C93 C95 151.1(15) . 6_554 ? C92 C93 C95 95.2(11) 6_554 . ? C92 C93 C95 85.8(11) . . ? C94 C93 C95 151.1(15) 6_554 . ? C94 C93 C95 24.4(13) . . ? C95 C93 C95 173.2(13) 6_554 . ? C95 C94 C93 105(3) . . ? C95 C94 C92 130(3) . . ? C93 C94 C92 48.2(16) . . ? C95 C94 C96 17(2) . . ? C93 C94 C96 94.1(12) . . ? C92 C94 C96 130.7(17) . . ? C94 C95 C96 150(4) . . ? C94 C95 C91 119(4) . 6_554 ? C96 C95 C91 36.8(15) . 6_554 ? C94 C95 C93 51(3) . . ? C96 C95 C93 108(2) . . ? C91 C95 C93 71.0(9) 6_554 . ? C95 C96 C91 111(2) . 6_554 ? C95 C96 C94 14(2) . . ? C91 C96 C94 101(2) 6_554 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 P1 C1 C2 66.2(3) . . . . ? C11 P1 C1 C2 174.8(3) . . . . ? S1 P1 C1 C2 -60.5(5) . . . . ? Se1 P1 C1 C2 -66.8(5) . . . . ? C21 P1 C1 C4 166.0(3) . . . . ? C11 P1 C1 C4 -85.4(3) . . . . ? S1 P1 C1 C4 39.3(5) . . . . ? Se1 P1 C1 C4 33.0(4) . . . . ? C4 C1 C2 C3 -24.3(3) . . . . ? P1 C1 C2 C3 87.4(3) . . . . ? C4 C1 C2 P2 -155.2(3) . . . . ? P1 C1 C2 P2 -43.6(5) . . . . ? C41 P2 C2 C3 78.6(3) . . . . ? C31 P2 C2 C3 -174.3(3) . . . . ? S2 P2 C2 C3 -46.9(6) . . . . ? Se2 P2 C2 C3 -46.3(3) . . . . ? C41 P2 C2 C1 -165.8(3) . . . . ? C31 P2 C2 C1 -58.7(4) . . . . ? S2 P2 C2 C1 68.7(6) . . . . ? Se2 P2 C2 C1 69.3(3) . . . . ? C1 C2 C3 C4 24.3(3) . . . . ? P2 C2 C3 C4 157.6(3) . . . . ? C1 C2 C3 P3 156.5(3) . . . . ? P2 C2 C3 P3 -70.1(4) . . . . ? C51 P3 C3 C2 86.5(4) . . . . ? C61 P3 C3 C2 -166.9(3) . . . . ? S3 P3 C3 C2 -40.1(4) . . . . ? Se3 P3 C3 C2 -39.3(4) . . . . ? C51 P3 C3 C4 -158.2(3) . . . . ? C61 P3 C3 C4 -51.6(4) . . . . ? S3 P3 C3 C4 75.2(4) . . . . ? Se3 P3 C3 C4 76.0(4) . . . . ? C2 C3 C4 C1 -24.1(3) . . . . ? P3 C3 C4 C1 -156.3(3) . . . . ? C2 C3 C4 P4 87.7(3) . . . . ? P3 C3 C4 P4 -44.5(5) . . . . ? C2 C1 C4 C3 23.9(3) . . . . ? P1 C1 C4 C3 -101.1(3) . . . . ? C2 C1 C4 P4 -102.4(3) . . . . ? P1 C1 C4 P4 132.6(2) . . . . ? C71 P4 C4 C3 66.4(4) . . . . ? C81 P4 C4 C3 174.3(3) . . . . ? S4 P4 C4 C3 -56.5(6) . . . . ? Se4 P4 C4 C3 -66.5(3) . . . . ? C71 P4 C4 C1 166.7(3) . . . . ? C81 P4 C4 C1 -85.3(3) . . . . ? S4 P4 C4 C1 43.9(5) . . . . ? Se4 P4 C4 C1 33.8(3) . . . . ? C21 P1 C11 C16 -99.7(4) . . . . ? C1 P1 C11 C16 146.0(3) . . . . ? S1 P1 C11 C16 24.6(6) . . . . ? Se1 P1 C11 C16 21.7(5) . . . . ? C21 P1 C11 C12 75.4(4) . . . . ? C1 P1 C11 C12 -38.9(4) . . . . ? S1 P1 C11 C12 -160.3(6) . . . . ? Se1 P1 C11 C12 -163.2(5) . . . . ? C16 C11 C12 C13 0.8(6) . . . . ? P1 C11 C12 C13 -174.2(3) . . . . ? C11 C12 C13 C14 -0.2(7) . . . . ? C12 C13 C14 C15 0.3(8) . . . . ? C13 C14 C15 C16 -1.2(9) . . . . ? C12 C11 C16 C15 -1.7(7) . . . . ? P1 C11 C16 C15 173.7(4) . . . . ? C14 C15 C16 C11 1.9(8) . . . . ? C11 P1 C21 C26 -58.6(4) . . . . ? C1 P1 C21 C26 50.1(4) . . . . ? S1 P1 C21 C26 175.5(5) . . . . ? Se1 P1 C21 C26 -175.6(4) . . . . ? C11 P1 C21 C22 117.1(3) . . . . ? C1 P1 C21 C22 -134.3(3) . . . . ? S1 P1 C21 C22 -8.8(5) . . . . ? Se1 P1 C21 C22 0.0(5) . . . . ? C26 C21 C22 C23 -0.3(6) . . . . ? P1 C21 C22 C23 -175.9(3) . . . . ? C21 C22 C23 C24 -0.3(7) . . . . ? C22 C23 C24 C25 0.5(7) . . . . ? C23 C24 C25 C26 -0.1(7) . . . . ? C22 C21 C26 C25 0.7(6) . . . . ? P1 C21 C26 C25 176.3(3) . . . . ? C24 C25 C26 C21 -0.5(6) . . . . ? C41 P2 C31 C32 83.2(4) . . . . ? C2 P2 C31 C32 -25.2(4) . . . . ? S2 P2 C31 C32 -152.4(5) . . . . ? Se2 P2 C31 C32 -154.2(3) . . . . ? C41 P2 C31 C36 -92.9(3) . . . . ? C2 P2 C31 C36 158.7(3) . . . . ? S2 P2 C31 C36 31.5(6) . . . . ? Se2 P2 C31 C36 29.7(3) . . . . ? C36 C31 C32 C33 -1.8(6) . . . . ? P2 C31 C32 C33 -177.9(3) . . . . ? C31 C32 C33 C34 0.5(6) . . . . ? C32 C33 C34 C35 1.6(7) . . . . ? C33 C34 C35 C36 -2.5(7) . . . . ? C34 C35 C36 C31 1.2(7) . . . . ? C32 C31 C36 C35 0.9(6) . . . . ? P2 C31 C36 C35 177.2(3) . . . . ? C31 P2 C41 C42 127.0(4) . . . . ? C2 P2 C41 C42 -124.6(4) . . . . ? S2 P2 C41 C42 1.6(6) . . . . ? Se2 P2 C41 C42 2.8(4) . . . . ? C31 P2 C41 C46 -51.7(4) . . . . ? C2 P2 C41 C46 56.8(4) . . . . ? S2 P2 C41 C46 -177.0(6) . . . . ? Se2 P2 C41 C46 -175.8(3) . . . . ? C46 C41 C42 C43 0.1(7) . . . . ? P2 C41 C42 C43 -178.6(4) . . . . ? C41 C42 C43 C44 -0.8(8) . . . . ? C42 C43 C44 C45 1.4(8) . . . . ? C43 C44 C45 C46 -1.3(8) . . . . ? C42 C41 C46 C45 0.0(7) . . . . ? P2 C41 C46 C45 178.6(3) . . . . ? C44 C45 C46 C41 0.6(7) . . . . ? C61 P3 C51 C56 109.5(4) . . . . ? C3 P3 C51 C56 -143.1(4) . . . . ? S3 P3 C51 C56 -13.9(5) . . . . ? Se3 P3 C51 C56 -15.8(4) . . . . ? C61 P3 C51 C52 -67.2(4) . . . . ? C3 P3 C51 C52 40.2(4) . . . . ? S3 P3 C51 C52 169.4(4) . . . . ? Se3 P3 C51 C52 167.5(4) . . . . ? C56 C51 C52 C53 -0.8(7) . . . . ? P3 C51 C52 C53 175.9(4) . . . . ? C51 C52 C53 C54 0.6(7) . . . . ? C52 C53 C54 C55 -0.8(8) . . . . ? C53 C54 C55 C56 1.1(9) . . . . ? C52 C51 C56 C55 1.2(7) . . . . ? P3 C51 C56 C55 -175.7(4) . . . . ? C54 C55 C56 C51 -1.4(9) . . . . ? C51 P3 C61 C62 -95.3(4) . . . . ? C3 P3 C61 C62 155.0(4) . . . . ? S3 P3 C61 C62 26.7(5) . . . . ? Se3 P3 C61 C62 27.9(4) . . . . ? C51 P3 C61 C66 80.4(4) . . . . ? C3 P3 C61 C66 -29.3(4) . . . . ? S3 P3 C61 C66 -157.6(4) . . . . ? Se3 P3 C61 C66 -156.4(3) . . . . ? C66 C61 C62 C63 -1.1(8) . . . . ? P3 C61 C62 C63 174.7(4) . . . . ? C61 C62 C63 C64 2.4(9) . . . . ? C62 C63 C64 C65 -2.4(10) . . . . ? C63 C64 C65 C66 1.2(9) . . . . ? C64 C65 C66 C61 0.1(7) . . . . ? C62 C61 C66 C65 -0.2(7) . . . . ? P3 C61 C66 C65 -175.8(3) . . . . ? C81 P4 C71 C72 126.8(4) . . . . ? C4 P4 C71 C72 -124.1(3) . . . . ? S4 P4 C71 C72 3.8(7) . . . . ? Se4 P4 C71 C72 7.3(4) . . . . ? C81 P4 C71 C76 -45.9(4) . . . . ? C4 P4 C71 C76 63.1(4) . . . . ? S4 P4 C71 C76 -168.9(7) . . . . ? Se4 P4 C71 C76 -165.4(3) . . . . ? C76 C71 C72 C73 -1.0(7) . . . . ? P4 C71 C72 C73 -173.8(3) . . . . ? C71 C72 C73 C74 1.0(7) . . . . ? C72 C73 C74 C75 -0.9(8) . . . . ? C73 C74 C75 C76 0.8(8) . . . . ? C72 C71 C76 C75 0.9(7) . . . . ? P4 C71 C76 C75 173.7(3) . . . . ? C74 C75 C76 C71 -0.8(7) . . . . ? C71 P4 C81 C82 -91.3(4) . . . . ? C4 P4 C81 C82 152.6(3) . . . . ? S4 P4 C81 C82 24.1(6) . . . . ? Se4 P4 C81 C82 31.9(4) . . . . ? C71 P4 C81 C86 83.3(4) . . . . ? C4 P4 C81 C86 -32.7(4) . . . . ? S4 P4 C81 C86 -161.2(6) . . . . ? Se4 P4 C81 C86 -153.5(3) . . . . ? C86 C81 C82 C83 0.2(7) . . . . ? P4 C81 C82 C83 175.2(4) . . . . ? C81 C82 C83 C84 -0.6(8) . . . . ? C82 C83 C84 C85 1.2(9) . . . . ? C83 C84 C85 C86 -1.5(9) . . . . ? C84 C85 C86 C81 1.2(8) . . . . ? C82 C81 C86 C85 -0.5(7) . . . . ? P4 C81 C86 C85 -175.1(4) . . . . ? C96 C91 C92 C93 -18(2) 6_554 . . . ? C95 C91 C92 C93 -9.3(14) 6_554 . . . ? C96 C91 C92 C94 19(5) 6_554 . . . ? C95 C91 C92 C94 28(4) 6_554 . . . ? C91 C92 C93 C92 -84.3(9) . . . 6_554 ? C94 C92 C93 C92 112.1(13) . . . 6_554 ? C91 C92 C93 C94 20.8(17) . . . 6_554 ? C94 C92 C93 C94 -143(2) . . . 6_554 ? C91 C92 C93 C94 163.6(19) . . . . ? C91 C92 C93 C95 8.4(12) . . . 6_554 ? C94 C92 C93 C95 -155.2(16) . . . 6_554 ? C91 C92 C93 C95 -178.3(11) . . . . ? C94 C92 C93 C95 18.1(13) . . . . ? C92 C93 C94 C95 -31(3) 6_554 . . . ? C92 C93 C94 C95 131(3) . . . . ? C94 C93 C94 C95 -122(3) 6_554 . . . ? C95 C93 C94 C95 -169(2) 6_554 . . . ? C92 C93 C94 C92 -163(2) 6_554 . . . ? C94 C93 C94 C92 106.4(13) 6_554 . . . ? C95 C93 C94 C92 60(2) 6_554 . . . ? C95 C93 C94 C92 -131(3) . . . . ? C92 C93 C94 C96 -18.4(18) 6_554 . . . ? C92 C93 C94 C96 144.3(15) . . . . ? C94 C93 C94 C96 -109.3(9) 6_554 . . . ? C95 C93 C94 C96 -155.7(19) 6_554 . . . ? C95 C93 C94 C96 13(2) . . . . ? C93 C92 C94 C95 -72(5) . . . . ? C91 C92 C94 C95 -114(6) . . . . ? C91 C92 C94 C93 -42(4) . . . . ? C93 C92 C94 C96 -50(2) . . . . ? C91 C92 C94 C96 -92(5) . . . . ? C93 C94 C95 C96 51(8) . . . . ? C92 C94 C95 C96 98(6) . . . . ? C93 C94 C95 C91 22(3) . . . 6_554 ? C92 C94 C95 C91 69(5) . . . 6_554 ? C96 C94 C95 C91 -29(6) . . . 6_554 ? C92 C94 C95 C93 47(4) . . . . ? C96 C94 C95 C93 -51(8) . . . . ? C92 C93 C95 C94 152(3) 6_554 . . . ? C92 C93 C95 C94 -45(3) . . . . ? C94 C93 C95 C94 98(5) 6_554 . . . ? C95 C93 C95 C94 54(3) 6_554 . . . ? C92 C93 C95 C96 -4(2) 6_554 . . . ? C92 C93 C95 C96 159.8(19) . . . . ? C94 C93 C95 C96 -58(3) 6_554 . . . ? C94 C93 C95 C96 -156(4) . . . . ? C95 C93 C95 C96 -101.6(16) 6_554 . . . ? C92 C93 C95 C91 -7.7(12) 6_554 . . 6_554 ? C92 C93 C95 C91 155.5(13) . . . 6_554 ? C94 C93 C95 C91 -62(2) 6_554 . . 6_554 ? C94 C93 C95 C91 -160(3) . . . 6_554 ? C95 C93 C95 C91 -105.8(7) 6_554 . . 6_554 ? C94 C95 C96 C91 -46(8) . . . 6_554 ? C93 C95 C96 C91 -7(2) . . . 6_554 ? C91 C95 C96 C94 46(8) 6_554 . . . ? C93 C95 C96 C94 39(7) . . . . ? C93 C94 C96 C95 -131(8) . . . . ? C92 C94 C96 C95 -96(7) . . . . ? C95 C94 C96 C91 137(8) . . . 6_554 ? C93 C94 C96 C91 5.9(16) . . . 6_554 ? C92 C94 C96 C91 41(3) . . . 6_554 ? _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction 0.990 _refine_diff_density_max 0.281 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.049 #===END data_6 _database_code_CSD 211322 _audit_creation_method SHELXL-97 _chemical_name_systematic [Pt2Cl4(2,3-trans-dppcbSe2-P,P',Se,Se')] _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cl4 P4 Pt2 Se2 x 0.5 C52 H44 Cl4 P4 Pt2 x 5.5 C3 H7 N O' _chemical_formula_sum 'C94.5 H104.5 Cl6 N5.5 O5.5 P6 Pt3 Se2' _chemical_formula_weight 2547.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' _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 14.9398(5) _cell_length_b 18.8634(6) _cell_length_c 19.2668(6) _cell_angle_alpha 68.799(2) _cell_angle_beta 80.929(2) _cell_angle_gamma 87.253(2) _cell_volume 4998.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 117578 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 21.491 _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 5.215 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 223(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 'Kappa CCD' _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_% 0 _diffrn_reflns_number 20732 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.998 _diffrn_reflns_theta_max 21.54 _reflns_number_total 10537 _reflns_number_gt 7403 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0336P)^2^+22.3382P] 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 10537 _refine_ls_number_parameters 1145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.007 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 Pt1 Pt 0.39623(3) 0.54823(2) 0.26588(2) 0.03705(13) Uani 1 1 d . . . Pt2 Pt 0.28708(3) 0.11516(2) 0.41651(2) 0.03994(13) Uani 1 1 d . . . Se1 Se 0.42273(7) 0.50190(6) 0.16337(6) 0.0439(3) Uani 1 1 d . . . Se2 Se 0.34770(8) 0.15576(7) 0.28523(6) 0.0511(3) Uani 1 1 d . . . Cl1 Cl 0.50288(19) 0.63939(16) 0.18151(16) 0.0571(8) Uani 1 1 d . . . Cl2 Cl 0.3829(2) 0.61707(16) 0.34530(16) 0.0586(8) Uani 1 1 d . . . Cl3 Cl 0.2198(2) 0.05620(16) 0.54040(15) 0.0580(8) Uani 1 1 d . . . Cl4 Cl 0.2376(2) 0.01221(17) 0.38971(17) 0.0660(9) Uani 1 1 d . . . P1 P 0.30223(18) 0.46154(15) 0.35442(14) 0.0346(6) Uani 1 1 d . . . P2 P 0.30817(18) 0.42661(15) 0.18685(14) 0.0357(7) Uani 1 1 d . . . P3 P 0.45048(18) 0.23785(15) 0.27172(14) 0.0387(7) Uani 1 1 d . . . P4 P 0.32752(18) 0.20867(15) 0.45119(14) 0.0359(7) Uani 1 1 d . . . C1 C 0.2896(7) 0.3630(5) 0.3533(5) 0.030(2) Uani 1 1 d . . . C2 C 0.3103(6) 0.3498(5) 0.2765(5) 0.029(2) Uani 1 1 d . . . C3 C 0.4031(7) 0.3165(5) 0.2988(5) 0.032(2) Uani 1 1 d . . . C4 C 0.3672(7) 0.3068(5) 0.3812(5) 0.030(2) Uani 1 1 d . . . C11 C 0.3356(8) 0.4403(5) 0.4475(6) 0.045(3) Uani 1 1 d . . . C12 C 0.4283(8) 0.4315(6) 0.4525(6) 0.049(3) Uani 1 1 d . . . H12A H 0.4696 0.4347 0.4099 0.058 Uiso 1 1 calc R . . C13 C 0.4591(10) 0.4180(6) 0.5205(7) 0.064(4) Uani 1 1 d . . . H13A H 0.5205 0.4109 0.5242 0.076 Uiso 1 1 calc R . . C14 C 0.3967(12) 0.4154(7) 0.5828(8) 0.077(4) Uani 1 1 d . . . H14A H 0.4159 0.4051 0.6291 0.092 Uiso 1 1 calc R . . C15 C 0.3079(12) 0.4280(8) 0.5761(8) 0.084(4) Uani 1 1 d . . . H15A H 0.2666 0.4277 0.6178 0.101 Uiso 1 1 calc R . . C16 C 0.2781(9) 0.4412(6) 0.5087(6) 0.058(3) Uani 1 1 d . . . H16A H 0.2170 0.4509 0.5051 0.069 Uiso 1 1 calc R . . C21 C 0.1847(6) 0.4932(6) 0.3635(5) 0.037(3) Uani 1 1 d . . . C22 C 0.1157(8) 0.4458(7) 0.4101(6) 0.058(3) Uani 1 1 d . . . H22A H 0.1282 0.3954 0.4370 0.070 Uiso 1 1 calc R . . C23 C 0.0279(9) 0.4717(8) 0.4177(7) 0.074(4) Uani 1 1 d . . . H23A H -0.0180 0.4390 0.4500 0.089 Uiso 1 1 calc R . . C24 C 0.0089(9) 0.5445(9) 0.3783(8) 0.074(4) Uani 1 1 d . . . H24A H -0.0503 0.5618 0.3831 0.089 Uiso 1 1 calc R . . C25 C 0.0765(9) 0.5934(7) 0.3312(7) 0.061(3) Uani 1 1 d . . . H25A H 0.0633 0.6435 0.3037 0.074 Uiso 1 1 calc R . . C26 C 0.1646(7) 0.5671(6) 0.3249(6) 0.044(3) Uani 1 1 d . . . H26A H 0.2107 0.6004 0.2940 0.053 Uiso 1 1 calc R . . C31 C 0.2021(7) 0.4759(6) 0.1869(5) 0.039(3) Uani 1 1 d . . . C32 C 0.1248(8) 0.4371(7) 0.2258(7) 0.060(3) Uani 1 1 d . . . H32A H 0.1276 0.3861 0.2560 0.072 Uiso 1 1 calc R . . C33 C 0.0397(9) 0.4740(9) 0.2209(9) 0.078(4) Uani 1 1 d . . . H33A H -0.0130 0.4479 0.2489 0.094 Uiso 1 1 calc R . . C34 C 0.0361(10) 0.5480(9) 0.1747(9) 0.072(4) Uani 1 1 d . . . H34A H -0.0196 0.5717 0.1681 0.086 Uiso 1 1 calc R . . C35 C 0.1127(13) 0.5862(9) 0.1388(8) 0.092(5) Uani 1 1 d . . . H35A H 0.1096 0.6378 0.1109 0.110 Uiso 1 1 calc R . . C36 C 0.1984(9) 0.5510(7) 0.1417(6) 0.066(4) Uani 1 1 d . . . H36A H 0.2507 0.5779 0.1138 0.079 Uiso 1 1 calc R . . C41 C 0.3137(7) 0.3867(6) 0.1139(5) 0.036(3) Uani 1 1 d . . . C42 C 0.3684(7) 0.4229(7) 0.0447(6) 0.052(3) Uani 1 1 d . . . H42A H 0.4065 0.4634 0.0375 0.063 Uiso 1 1 calc R . . C43 C 0.3633(8) 0.3959(8) -0.0121(6) 0.059(3) Uani 1 1 d . . . H43A H 0.3986 0.4189 -0.0588 0.071 Uiso 1 1 calc R . . C44 C 0.3079(8) 0.3363(8) -0.0019(7) 0.062(3) Uani 1 1 d . . . H44A H 0.3054 0.3203 -0.0419 0.074 Uiso 1 1 calc R . . C45 C 0.2548(9) 0.2991(7) 0.0674(6) 0.058(3) Uani 1 1 d . . . H45A H 0.2181 0.2578 0.0745 0.070 Uiso 1 1 calc R . . C46 C 0.2584(7) 0.3253(6) 0.1247(6) 0.047(3) Uani 1 1 d . . . H46A H 0.2235 0.3016 0.1714 0.057 Uiso 1 1 calc R . . C51 C 0.5015(7) 0.2762(6) 0.1736(6) 0.042(3) Uani 1 1 d . . . C52 C 0.4816(8) 0.2439(7) 0.1238(6) 0.060(3) Uani 1 1 d . . . H52A H 0.4386 0.2050 0.1403 0.072 Uiso 1 1 calc R . . C53 C 0.5241(11) 0.2682(8) 0.0502(8) 0.081(4) Uani 1 1 d . . . H53A H 0.5106 0.2465 0.0167 0.097 Uiso 1 1 calc R . . C54 C 0.5866(12) 0.3250(10) 0.0285(8) 0.092(5) Uani 1 1 d . . . H54A H 0.6150 0.3421 -0.0213 0.110 Uiso 1 1 calc R . . C55 C 0.6107(9) 0.3591(8) 0.0750(8) 0.077(4) Uani 1 1 d . . . H55A H 0.6545 0.3974 0.0577 0.092 Uiso 1 1 calc R . . C56 C 0.5649(8) 0.3326(7) 0.1524(7) 0.064(3) Uani 1 1 d . . . H56A H 0.5785 0.3536 0.1865 0.076 Uiso 1 1 calc R . . C61 C 0.5396(7) 0.1963(6) 0.3254(5) 0.035(2) Uani 1 1 d . . . C62 C 0.5639(7) 0.1231(6) 0.3373(6) 0.044(3) Uani 1 1 d . . . H62A H 0.5324 0.0940 0.3190 0.053 Uiso 1 1 calc R . . C63 C 0.6345(8) 0.0912(7) 0.3761(6) 0.055(3) Uani 1 1 d . . . H63A H 0.6499 0.0408 0.3842 0.067 Uiso 1 1 calc R . . C64 C 0.6820(8) 0.1331(8) 0.4029(7) 0.061(3) Uani 1 1 d . . . H64A H 0.7292 0.1114 0.4296 0.074 Uiso 1 1 calc R . . C65 C 0.6592(8) 0.2083(8) 0.3898(7) 0.068(4) Uani 1 1 d . . . H65A H 0.6918 0.2380 0.4067 0.082 Uiso 1 1 calc R . . C66 C 0.5881(7) 0.2387(7) 0.3518(6) 0.057(3) Uani 1 1 d . . . H66A H 0.5724 0.2890 0.3436 0.069 Uiso 1 1 calc R . . C71 C 0.4208(7) 0.1785(6) 0.5067(5) 0.038(3) Uani 1 1 d . . . C72 C 0.4539(7) 0.1065(6) 0.5230(5) 0.042(3) Uani 1 1 d . . . H72A H 0.4275 0.0731 0.5062 0.050 Uiso 1 1 calc R . . C73 C 0.5248(8) 0.0814(7) 0.5632(6) 0.056(3) Uani 1 1 d . . . H73A H 0.5464 0.0322 0.5731 0.067 Uiso 1 1 calc R . . C74 C 0.5623(9) 0.1293(7) 0.5880(7) 0.070(4) Uani 1 1 d . . . H74A H 0.6099 0.1126 0.6157 0.084 Uiso 1 1 calc R . . C75 C 0.5307(9) 0.2049(8) 0.5729(7) 0.074(4) Uani 1 1 d . . . H75A H 0.5574 0.2381 0.5897 0.088 Uiso 1 1 calc R . . C76 C 0.4598(8) 0.2276(7) 0.5329(6) 0.055(3) Uani 1 1 d . . . H76A H 0.4374 0.2765 0.5230 0.066 Uiso 1 1 calc R . . C81 C 0.2306(8) 0.2330(6) 0.5097(6) 0.051(3) Uani 1 1 d . . . C82 C 0.2392(10) 0.2514(7) 0.5726(6) 0.070(4) Uani 1 1 d . . . H82A H 0.2953 0.2531 0.5871 0.084 Uiso 1 1 calc R . . C83 C 0.1583(15) 0.2672(8) 0.6125(9) 0.103(6) Uani 1 1 d . . . H83A H 0.1623 0.2767 0.6560 0.123 Uiso 1 1 calc R . . C84 C 0.0784(14) 0.2694(10) 0.5932(12) 0.112(8) Uani 1 1 d . . . H84A H 0.0271 0.2814 0.6209 0.134 Uiso 1 1 calc R . . C85 C 0.0732(9) 0.2533(7) 0.5308(9) 0.076(4) Uani 1 1 d . . . H85A H 0.0169 0.2556 0.5153 0.091 Uiso 1 1 calc R . . C86 C 0.1457(8) 0.2342(6) 0.4902(7) 0.056(3) Uani 1 1 d . . . H86A H 0.1383 0.2218 0.4489 0.068 Uiso 1 1 calc R . . Pt3 Pt 0.03937(3) 0.19926(2) 0.91301(2) 0.03704(13) Uani 1 1 d . . . Cl5 Cl 0.0658(2) 0.27924(16) 0.78653(14) 0.0525(7) Uani 1 1 d . . . Cl6 Cl 0.1181(2) 0.28615(17) 0.94302(16) 0.0637(9) Uani 1 1 d . . . P5 P 0.01249(18) 0.12455(15) 1.03330(14) 0.0364(7) Uani 1 1 d . . . P6 P -0.04986(19) 0.12072(15) 0.89101(15) 0.0387(7) Uani 1 1 d . . . C5 C -0.0225(7) 0.0280(5) 1.0404(5) 0.031(2) Uani 1 1 d . . . C6 C -0.0546(7) 0.0265(6) 0.9686(6) 0.033(3) Uani 1 1 d . . . C91 C 0.1076(7) 0.1107(6) 1.0847(6) 0.039(3) Uani 1 1 d . . . C92 C 0.1916(8) 0.1006(6) 1.0484(6) 0.046(3) Uani 1 1 d . . . H92A H 0.1980 0.1030 0.9989 0.055 Uiso 1 1 calc R . . C93 C 0.2666(8) 0.0870(7) 1.0853(7) 0.065(4) Uani 1 1 d . . . H93A H 0.3228 0.0802 1.0601 0.078 Uiso 1 1 calc R . . C94 C 0.2595(9) 0.0835(7) 1.1552(8) 0.069(4) Uani 1 1 d . . . H94A H 0.3102 0.0720 1.1796 0.083 Uiso 1 1 calc R . . C95 C 0.1769(10) 0.0969(7) 1.1932(7) 0.072(4) Uani 1 1 d . . . H95A H 0.1723 0.0963 1.2421 0.086 Uiso 1 1 calc R . . C96 C 0.1014(8) 0.1113(6) 1.1560(6) 0.050(3) Uani 1 1 d . . . H96A H 0.0459 0.1213 1.1800 0.060 Uiso 1 1 calc R . . C101 C -0.0808(7) 0.1555(6) 1.0863(6) 0.045(3) Uani 1 1 d . . . C102 C -0.1302(10) 0.1087(7) 1.1516(8) 0.081(4) Uani 1 1 d . . . H102A H -0.1146 0.0577 1.1703 0.097 Uiso 1 1 calc R . . C103 C -0.2012(11) 0.1334(10) 1.1904(9) 0.107(6) Uani 1 1 d . . . H103B H -0.2327 0.0992 1.2344 0.128 Uiso 1 1 calc R . . C104 C -0.2264(10) 0.2069(11) 1.1658(10) 0.092(5) Uani 1 1 d . . . H104C H -0.2756 0.2240 1.1912 0.111 Uiso 1 1 calc R . . C105 C -0.1773(11) 0.2544(10) 1.1029(10) 0.103(5) Uani 1 1 d . . . H105D H -0.1912 0.3059 1.0858 0.123 Uiso 1 1 calc R . . C106 C -0.1081(9) 0.2289(8) 1.0640(7) 0.073(4) Uani 1 1 d . . . H106E H -0.0777 0.2635 1.0196 0.087 Uiso 1 1 calc R . . C111 C -0.1653(8) 0.1560(6) 0.8928(6) 0.048(3) Uani 1 1 d . . . C112 C -0.1840(10) 0.2257(9) 0.8468(10) 0.118(7) Uani 1 1 d . . . H112A H -0.1365 0.2556 0.8135 0.142 Uiso 1 1 calc R . . C113 C -0.2674(11) 0.2546(10) 0.8465(10) 0.111(6) Uani 1 1 d . . . H113B H -0.2762 0.3031 0.8127 0.133 Uiso 1 1 calc R . . C114 C -0.3356(11) 0.2172(10) 0.8915(10) 0.104(6) Uani 1 1 d . . . H114C H -0.3932 0.2381 0.8899 0.125 Uiso 1 1 calc R . . C115 C -0.3227(13) 0.1470(16) 0.9414(19) 0.32(2) Uani 1 1 d . . . H115D H -0.3707 0.1180 0.9748 0.382 Uiso 1 1 calc R . . C116 C -0.2332(12) 0.1199(12) 0.9405(15) 0.204(13) Uani 1 1 d . . . H116E H -0.2225 0.0730 0.9764 0.245 Uiso 1 1 calc R . . C121 C -0.0230(8) 0.1005(6) 0.8048(6) 0.045(3) Uani 1 1 d . . . C122 C -0.0886(10) 0.0837(7) 0.7723(6) 0.070(4) Uani 1 1 d . . . H122A H -0.1487 0.0821 0.7946 0.084 Uiso 1 1 calc R . . C123 C -0.0678(14) 0.0686(9) 0.7053(9) 0.092(5) Uani 1 1 d . . . H123B H -0.1138 0.0580 0.6830 0.111 Uiso 1 1 calc R . . C124 C 0.0179(15) 0.0697(7) 0.6745(8) 0.080(5) Uani 1 1 d . . . H124C H 0.0316 0.0598 0.6301 0.095 Uiso 1 1 calc R . . C125 C 0.0874(13) 0.0851(7) 0.7060(7) 0.089(5) Uani 1 1 d . . . H125D H 0.1472 0.0845 0.6838 0.107 Uiso 1 1 calc R . . C126 C 0.0669(9) 0.1020(6) 0.7736(7) 0.061(3) Uani 1 1 d . . . H126E H 0.1126 0.1136 0.7955 0.073 Uiso 1 1 calc R . . O1 O 0.1197(7) 0.2543(6) 0.3002(7) 0.105(4) Uani 1 1 d . . . O2 O 0.4119(7) 0.5842(6) 0.6934(8) 0.116(4) Uani 1 1 d . . . O3 O 0.140(3) 0.756(3) 0.547(2) 0.54(4) Uani 1 1 d D . . O4 O 0.5519(13) 0.8685(12) 0.0666(13) 0.252(13) Uani 1 1 d . . . O5 O 0.7661(9) 0.9538(10) 0.1119(9) 0.135(6) Uani 1 1 d . . . O6 O 0.165(3) 0.557(2) -0.063(3) 0.24(2) Uani 0.50 1 d P . . N1 N -0.0022(9) 0.1799(8) 0.3277(8) 0.095(4) Uani 1 1 d . . . N2 N 0.2793(9) 0.5196(7) 0.7506(8) 0.101(4) Uani 1 1 d . . . N3 N 0.2017(11) 0.7446(13) 0.4396(15) 0.142(6) Uani 1 1 d . . . N4 N 0.6048(13) 0.7985(10) 0.1791(12) 0.138(6) Uani 1 1 d . . . N5 N 0.6325(19) 0.9933(15) 0.1768(19) 0.196(10) Uani 1 1 d . . . N6 N 0.038(3) 0.499(2) -0.002(2) 0.129(16) Uani 0.50 1 d P . . C1L C 0.0777(12) 0.1945(10) 0.3301(9) 0.087(5) Uani 1 1 d . . . H1LA H 0.1096 0.1539 0.3590 0.105 Uiso 1 1 calc R . . C2L C -0.0510(17) 0.2388(13) 0.2807(16) 0.219(14) Uani 1 1 d . . . H2LA H -0.0100 0.2704 0.2383 0.329 Uiso 1 1 calc R . . H2LB H -0.0802 0.2689 0.3085 0.329 Uiso 1 1 calc R . . H2LC H -0.0959 0.2174 0.2633 0.329 Uiso 1 1 calc R . . C3L C -0.0467(13) 0.1095(12) 0.3721(16) 0.196(13) Uani 1 1 d . . . H3LA H -0.0102 0.0800 0.4090 0.294 Uiso 1 1 calc R . . H3LB H -0.0556 0.0821 0.3403 0.294 Uiso 1 1 calc R . . H3LC H -0.1044 0.1190 0.3970 0.294 Uiso 1 1 calc R . . C4L C 0.3645(12) 0.5274(10) 0.7274(9) 0.087(4) Uani 1 1 d . . . H4LA H 0.3960 0.4819 0.7381 0.105 Uiso 1 1 calc R . . C5L C 0.224(2) 0.5868(16) 0.731(2) 0.40(3) Uani 1 1 d . . . H5LA H 0.2273 0.6087 0.6770 0.597 Uiso 1 1 calc R . . H5LB H 0.2451 0.6232 0.7488 0.597 Uiso 1 1 calc R . . H5LC H 0.1620 0.5733 0.7533 0.597 Uiso 1 1 calc R . . C6L C 0.2353(13) 0.4489(10) 0.7900(10) 0.140(7) Uani 1 1 d . . . H6LA H 0.2783 0.4087 0.7933 0.209 Uiso 1 1 calc R . . H6LB H 0.1881 0.4434 0.7637 0.209 Uiso 1 1 calc R . . H6LC H 0.2094 0.4463 0.8397 0.209 Uiso 1 1 calc R . . C7L C 0.175(2) 0.7915(15) 0.484(3) 0.26(2) Uani 1 1 d D . . H7LA H 0.1837 0.8439 0.4658 0.312 Uiso 1 1 calc R . . C8L C 0.230(2) 0.7779(16) 0.3541(18) 0.211(13) Uani 1 1 d . . . H8LA H 0.2603 0.8258 0.3404 0.317 Uiso 1 1 calc R . . H8LB H 0.1774 0.7851 0.3297 0.317 Uiso 1 1 calc R . . H8LC H 0.2706 0.7434 0.3385 0.317 Uiso 1 1 calc R . . C9L C 0.1982(17) 0.6639(16) 0.490(2) 0.245(17) Uani 1 1 d . . . H9LA H 0.1639 0.6592 0.5382 0.367 Uiso 1 1 calc R . . H9LB H 0.2587 0.6460 0.4968 0.367 Uiso 1 1 calc R . . H9LC H 0.1698 0.6340 0.4685 0.367 Uiso 1 1 calc R . . C10L C 0.609(2) 0.8295(14) 0.1008(17) 0.167(10) Uani 1 1 d . . . H10F H 0.6604 0.8191 0.0721 0.201 Uiso 1 1 calc R . . C11L C 0.6825(18) 0.7588(17) 0.2151(17) 0.254(18) Uani 1 1 d . . . H11F H 0.7268 0.7483 0.1783 0.381 Uiso 1 1 calc R . . H11G H 0.6619 0.7119 0.2546 0.381 Uiso 1 1 calc R . . H11H H 0.7093 0.7904 0.2359 0.381 Uiso 1 1 calc R . . C12L C 0.5219(17) 0.8090(14) 0.2220(14) 0.201(13) Uani 1 1 d . . . H12F H 0.4902 0.8513 0.1914 0.302 Uiso 1 1 calc R . . H12G H 0.5346 0.8188 0.2650 0.302 Uiso 1 1 calc R . . H12H H 0.4851 0.7639 0.2385 0.302 Uiso 1 1 calc R . . C13L C 0.697(3) 0.9825(17) 0.1185(16) 0.209(17) Uani 1 1 d . . . H13'A H 0.6770 1.0052 0.0720 0.250 Uiso 1 1 calc R . . C14L C 0.662(3) 0.951(3) 0.253(3) 0.37(4) Uani 1 1 d . . . H14'A H 0.7193 0.9706 0.2544 0.557 Uiso 1 1 calc R . . H14B H 0.6674 0.8978 0.2606 0.557 Uiso 1 1 calc R . . H14C H 0.6174 0.9574 0.2919 0.557 Uiso 1 1 calc R . . C15L C 0.538(2) 1.0248(17) 0.182(2) 0.280(19) Uani 1 1 d . . . H15'A H 0.5236 1.0512 0.1328 0.420 Uiso 1 1 calc R . . H15B H 0.5351 1.0593 0.2091 0.420 Uiso 1 1 calc R . . H15C H 0.4956 0.9838 0.2091 0.420 Uiso 1 1 calc R . . C16L C 0.127(6) 0.490(3) -0.015(3) 0.17(3) Uani 0.50 1 d P . . C17L C 0.003(3) 0.432(2) 0.039(2) 0.209(14) Uani 1 1 d . . . H1 H 0.229(6) 0.337(5) 0.385(5) 0.030 Uiso 1 1 d . . . H2 H 0.271(6) 0.314(5) 0.275(5) 0.030 Uiso 1 1 d . . . H3 H 0.459(6) 0.352(5) 0.285(4) 0.030 Uiso 1 1 d . . . H4 H 0.399(6) 0.322(5) 0.407(5) 0.030 Uiso 1 1 d . . . H5 H -0.063(6) 0.009(5) 1.082(5) 0.030 Uiso 1 1 d . . . H6 H -0.101(6) 0.011(5) 0.978(5) 0.030 Uiso 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 Pt1 0.0335(3) 0.0354(3) 0.0376(2) -0.0073(2) -0.0064(2) 0.00066(19) Pt2 0.0366(3) 0.0386(3) 0.0415(2) -0.0108(2) -0.0061(2) 0.0023(2) Se1 0.0431(7) 0.0443(7) 0.0351(6) -0.0070(5) 0.0048(5) -0.0073(5) Se2 0.0552(8) 0.0590(8) 0.0455(7) -0.0283(6) 0.0014(6) -0.0137(6) Cl1 0.0459(18) 0.0486(18) 0.0664(19) -0.0104(15) 0.0005(15) -0.0113(14) Cl2 0.081(2) 0.0491(18) 0.0517(17) -0.0217(15) -0.0163(16) -0.0020(16) Cl3 0.061(2) 0.0465(18) 0.0502(17) -0.0024(14) 0.0023(15) 0.0038(15) Cl4 0.078(2) 0.0508(19) 0.072(2) -0.0186(16) -0.0236(18) -0.0123(16) P1 0.0389(17) 0.0309(15) 0.0310(14) -0.0077(12) -0.0065(13) 0.0043(13) P2 0.0356(16) 0.0384(16) 0.0288(14) -0.0070(13) -0.0058(13) 0.0039(13) P3 0.0363(17) 0.0412(17) 0.0355(15) -0.0127(13) -0.0011(13) 0.0058(13) P4 0.0406(17) 0.0339(16) 0.0279(14) -0.0068(13) -0.0018(13) 0.0068(13) C1 0.027(6) 0.031(6) 0.020(5) 0.001(5) 0.002(5) 0.005(5) C2 0.026(6) 0.025(6) 0.030(6) -0.005(5) 0.002(5) 0.000(4) C3 0.033(6) 0.030(6) 0.031(6) -0.006(5) -0.009(5) 0.001(5) C4 0.035(6) 0.026(6) 0.029(6) -0.009(5) -0.004(5) -0.001(5) C11 0.071(9) 0.029(6) 0.031(6) -0.003(5) -0.013(6) 0.003(6) C12 0.064(9) 0.036(7) 0.048(7) -0.015(6) -0.015(6) 0.001(6) C13 0.097(11) 0.041(8) 0.059(9) -0.013(7) -0.044(9) 0.008(7) C14 0.118(14) 0.064(9) 0.057(9) -0.023(7) -0.026(10) -0.021(9) C15 0.093(13) 0.093(11) 0.067(10) -0.035(8) 0.005(9) -0.024(10) C16 0.073(9) 0.065(8) 0.035(7) -0.015(6) -0.018(7) 0.003(7) C21 0.023(6) 0.042(7) 0.041(6) -0.011(6) 0.003(5) 0.007(5) C22 0.050(8) 0.050(8) 0.060(8) -0.011(7) 0.006(7) 0.014(7) C23 0.046(9) 0.087(11) 0.075(9) -0.024(9) 0.024(7) 0.000(8) C24 0.043(9) 0.089(11) 0.082(10) -0.026(9) -0.008(8) 0.044(9) C25 0.061(9) 0.059(8) 0.063(8) -0.020(7) -0.020(7) 0.029(8) C26 0.042(7) 0.041(7) 0.049(7) -0.017(6) -0.006(6) 0.007(6) C31 0.036(7) 0.048(7) 0.033(6) -0.019(6) -0.002(5) 0.003(6) C32 0.049(8) 0.057(8) 0.079(9) -0.030(7) -0.014(7) 0.006(7) C33 0.048(9) 0.093(12) 0.113(12) -0.058(11) -0.016(8) -0.001(8) C34 0.054(10) 0.071(11) 0.104(12) -0.044(10) -0.028(9) 0.029(8) C35 0.108(14) 0.076(11) 0.075(10) -0.010(9) -0.028(10) 0.059(11) C36 0.064(9) 0.055(9) 0.053(8) 0.003(7) 0.007(7) 0.015(7) C41 0.034(6) 0.046(7) 0.029(6) -0.015(5) -0.006(5) 0.010(6) C42 0.049(8) 0.068(8) 0.033(7) -0.012(6) -0.003(6) 0.003(6) C43 0.050(8) 0.088(10) 0.038(7) -0.025(7) 0.007(6) -0.009(7) C44 0.060(9) 0.090(10) 0.052(8) -0.045(8) -0.014(7) 0.009(8) C45 0.081(9) 0.062(8) 0.039(7) -0.022(7) -0.015(7) -0.011(7) C46 0.048(7) 0.043(7) 0.042(7) -0.003(6) -0.011(6) -0.003(6) C51 0.041(7) 0.045(7) 0.034(6) -0.013(6) 0.002(5) 0.012(6) C52 0.056(8) 0.068(9) 0.039(7) -0.009(7) 0.013(6) 0.012(7) C53 0.103(12) 0.066(10) 0.059(10) -0.013(8) 0.014(9) -0.010(9) C54 0.130(16) 0.083(12) 0.044(8) -0.003(9) -0.015(10) 0.022(11) C55 0.049(8) 0.065(9) 0.073(10) 0.016(8) 0.017(8) 0.004(7) C56 0.054(8) 0.057(9) 0.062(9) -0.010(7) 0.012(7) 0.014(7) C61 0.032(6) 0.032(7) 0.031(6) -0.003(5) 0.006(5) 0.004(5) C62 0.041(7) 0.039(7) 0.049(7) -0.015(6) -0.007(6) 0.009(6) C63 0.054(8) 0.038(7) 0.056(8) -0.004(6) 0.010(7) 0.007(7) C64 0.035(7) 0.060(9) 0.072(9) -0.006(7) -0.007(7) 0.010(7) C65 0.056(9) 0.068(10) 0.080(9) -0.023(8) -0.011(8) -0.020(7) C66 0.033(7) 0.063(8) 0.070(8) -0.018(7) -0.014(7) 0.014(6) C71 0.044(7) 0.037(7) 0.029(6) -0.003(5) -0.015(5) 0.006(5) C72 0.043(7) 0.044(7) 0.035(6) -0.010(5) -0.006(5) 0.002(6) C73 0.062(9) 0.053(8) 0.053(7) -0.021(7) -0.007(7) 0.003(7) C74 0.083(10) 0.053(9) 0.056(8) 0.007(7) -0.022(7) 0.010(8) C75 0.086(10) 0.074(10) 0.070(9) -0.028(8) -0.029(8) -0.013(8) C76 0.073(9) 0.051(8) 0.044(7) -0.012(6) -0.029(7) 0.014(7) C81 0.051(8) 0.043(7) 0.045(7) -0.008(6) 0.012(6) 0.011(6) C82 0.113(12) 0.057(8) 0.035(7) -0.022(6) 0.017(7) -0.002(8) C83 0.155(18) 0.065(10) 0.071(10) -0.040(9) 0.075(13) -0.013(12) C84 0.094(14) 0.079(12) 0.115(16) -0.018(11) 0.084(14) -0.003(11) C85 0.059(10) 0.044(8) 0.090(11) -0.006(8) 0.042(9) 0.007(7) C86 0.053(9) 0.047(8) 0.059(8) -0.016(6) 0.010(7) 0.016(6) Pt3 0.0393(3) 0.0386(3) 0.0303(2) -0.00929(19) -0.0054(2) 0.0032(2) Cl5 0.065(2) 0.0493(18) 0.0335(15) -0.0044(13) -0.0051(14) 0.0010(15) Cl6 0.080(2) 0.0518(19) 0.0585(19) -0.0118(15) -0.0209(17) -0.0229(16) P5 0.0419(17) 0.0382(16) 0.0300(14) -0.0128(13) -0.0065(13) 0.0017(13) P6 0.0411(17) 0.0355(16) 0.0375(16) -0.0096(13) -0.0108(14) 0.0075(13) C5 0.035(7) 0.024(6) 0.031(6) -0.009(5) -0.003(5) 0.000(5) C6 0.025(6) 0.041(7) 0.035(6) -0.017(5) 0.005(5) -0.003(5) C91 0.030(7) 0.052(7) 0.041(7) -0.024(6) -0.004(5) 0.004(5) C92 0.055(8) 0.047(7) 0.031(6) -0.006(5) -0.011(6) -0.010(6) C93 0.040(8) 0.089(10) 0.071(9) -0.031(8) -0.010(7) -0.013(7) C94 0.061(10) 0.086(10) 0.067(10) -0.031(8) -0.026(8) 0.001(8) C95 0.099(12) 0.082(10) 0.045(7) -0.026(7) -0.035(9) 0.001(8) C96 0.057(8) 0.061(8) 0.039(7) -0.027(6) -0.002(6) -0.004(6) C101 0.051(7) 0.045(7) 0.045(7) -0.022(6) -0.010(6) 0.008(6) C102 0.114(12) 0.042(8) 0.075(10) -0.025(8) 0.025(9) 0.013(8) C103 0.101(13) 0.103(14) 0.116(13) -0.068(12) 0.062(11) -0.015(11) C104 0.063(10) 0.102(14) 0.118(14) -0.062(12) 0.016(10) 0.024(10) C105 0.089(12) 0.090(12) 0.115(13) -0.039(11) 0.019(11) 0.042(10) C106 0.080(10) 0.067(10) 0.059(8) -0.022(7) 0.022(7) 0.007(8) C111 0.044(8) 0.049(8) 0.052(7) -0.015(6) -0.017(6) -0.011(6) C112 0.039(10) 0.078(11) 0.159(16) 0.039(11) 0.018(9) 0.000(8) C113 0.049(11) 0.102(13) 0.114(13) 0.033(10) 0.004(10) 0.016(10) C114 0.062(12) 0.106(14) 0.132(15) -0.027(12) -0.034(11) 0.049(11) C115 0.067(14) 0.22(3) 0.41(4) 0.14(3) 0.06(2) 0.102(17) C116 0.070(14) 0.125(17) 0.27(3) 0.078(18) 0.034(16) 0.043(13) C121 0.071(9) 0.034(6) 0.038(6) -0.014(5) -0.028(7) 0.006(6) C122 0.096(11) 0.083(10) 0.047(8) -0.035(7) -0.026(8) -0.007(8) C123 0.120(15) 0.091(12) 0.077(11) -0.036(9) -0.032(11) -0.004(11) C124 0.147(16) 0.047(9) 0.048(9) -0.018(7) -0.015(11) -0.014(10) C125 0.150(16) 0.060(9) 0.043(8) -0.017(7) 0.018(9) 0.010(10) C126 0.068(10) 0.051(8) 0.059(8) -0.021(7) 0.009(7) -0.005(7) O1 0.071(7) 0.071(7) 0.148(10) -0.010(7) -0.010(7) -0.015(6) O2 0.069(7) 0.055(7) 0.197(12) -0.021(8) -0.001(8) -0.002(6) O3 0.24(4) 0.94(11) 0.78(9) -0.68(9) -0.20(5) 0.12(5) O4 0.144(16) 0.187(19) 0.30(3) 0.067(17) -0.059(16) 0.020(13) O5 0.093(10) 0.198(16) 0.128(11) -0.085(11) -0.002(9) 0.028(10) O6 0.28(5) 0.11(3) 0.30(5) -0.07(3) 0.06(4) -0.03(3) N1 0.055(9) 0.093(10) 0.158(13) -0.066(10) -0.032(9) 0.016(8) N2 0.045(8) 0.072(9) 0.154(12) -0.005(8) -0.009(8) 0.004(7) N3 0.090(12) 0.150(18) 0.21(2) -0.087(18) -0.045(14) 0.011(12) N4 0.144(16) 0.131(14) 0.147(15) -0.079(13) 0.046(14) -0.070(13) N5 0.18(2) 0.18(2) 0.26(3) -0.15(2) 0.01(2) -0.007(17) N6 0.17(5) 0.062(19) 0.18(3) -0.03(2) -0.13(4) 0.04(3) C1L 0.066(12) 0.090(13) 0.110(13) -0.041(11) -0.022(10) 0.023(10) C2L 0.21(3) 0.14(2) 0.33(4) -0.07(2) -0.18(3) 0.052(19) C3L 0.088(15) 0.114(17) 0.38(4) -0.10(2) 0.027(19) -0.042(13) C4L 0.073(12) 0.072(12) 0.114(13) -0.035(10) -0.015(10) 0.027(10) C5L 0.14(2) 0.15(2) 0.61(7) 0.12(3) 0.13(3) 0.07(2) C6L 0.122(16) 0.119(16) 0.123(15) 0.010(12) 0.026(12) -0.054(13) C7L 0.09(2) 0.18(2) 0.64(8) -0.27(4) -0.14(3) 0.044(17) C8L 0.23(3) 0.19(3) 0.23(3) -0.08(3) -0.08(3) 0.08(2) C9L 0.13(2) 0.15(2) 0.39(5) -0.03(3) 0.01(2) -0.045(19) C10L 0.17(3) 0.13(2) 0.15(2) -0.033(18) 0.08(2) -0.027(18) C11L 0.17(3) 0.26(3) 0.32(4) -0.05(3) -0.16(3) 0.06(2) C12L 0.19(2) 0.21(3) 0.24(3) -0.17(2) 0.11(2) -0.10(2) C13L 0.32(5) 0.15(3) 0.16(2) -0.10(2) 0.07(3) -0.12(3) C14L 0.29(6) 0.52(9) 0.39(7) -0.32(7) 0.14(5) -0.22(6) C15L 0.22(3) 0.23(3) 0.39(5) -0.16(3) 0.05(3) 0.11(3) C16L 0.25(7) 0.15(5) 0.17(5) -0.10(4) -0.12(6) 0.11(6) C17L 0.27(4) 0.21(3) 0.24(4) -0.17(3) -0.10(3) 0.08(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 Pt1 P1 2.237(3) . ? Pt1 Cl2 2.320(3) . ? Pt1 Cl1 2.359(3) . ? Pt1 Se1 2.4063(12) . ? Pt2 P4 2.237(3) . ? Pt2 Cl3 2.319(3) . ? Pt2 Cl4 2.359(3) . ? Pt2 Se2 2.3975(14) . ? Se1 P2 2.162(3) . ? Se2 P3 2.153(3) . ? P1 C21 1.830(9) . ? P1 C11 1.835(10) . ? P1 C1 1.886(10) . ? P2 C31 1.799(10) . ? P2 C41 1.809(9) . ? P2 C2 1.813(9) . ? P3 C61 1.790(10) . ? P3 C51 1.814(10) . ? P3 C3 1.820(10) . ? P4 C71 1.834(9) . ? P4 C81 1.836(11) . ? P4 C4 1.908(10) . ? C1 C4 1.557(12) . ? C1 C2 1.570(12) . ? C2 C3 1.552(13) . ? C3 C4 1.541(13) . ? C11 C16 1.351(15) . ? C11 C12 1.400(15) . ? C12 C13 1.390(14) . ? C13 C14 1.385(18) . ? C14 C15 1.355(19) . ? C15 C16 1.374(17) . ? C21 C26 1.366(13) . ? C21 C22 1.373(14) . ? C22 C23 1.382(16) . ? C23 C24 1.350(17) . ? C24 C25 1.375(17) . ? C25 C26 1.386(15) . ? C31 C32 1.357(15) . ? C31 C36 1.372(14) . ? C32 C33 1.420(16) . ? C33 C34 1.360(18) . ? C34 C35 1.333(19) . ? C35 C36 1.414(17) . ? C41 C46 1.389(14) . ? C41 C42 1.401(14) . ? C42 C43 1.377(15) . ? C43 C44 1.366(16) . ? C44 C45 1.396(16) . ? C45 C46 1.373(14) . ? C51 C56 1.362(16) . ? C51 C52 1.382(15) . ? C52 C53 1.378(16) . ? C53 C54 1.36(2) . ? C54 C55 1.372(19) . ? C55 C56 1.455(17) . ? C61 C62 1.356(13) . ? C61 C66 1.375(14) . ? C62 C63 1.377(15) . ? C63 C64 1.363(16) . ? C64 C65 1.384(16) . ? C65 C66 1.369(15) . ? C71 C72 1.366(13) . ? C71 C76 1.390(14) . ? C72 C73 1.377(14) . ? C73 C74 1.342(16) . ? C74 C75 1.422(17) . ? C75 C76 1.370(15) . ? C81 C86 1.375(15) . ? C81 C82 1.401(15) . ? C82 C83 1.41(2) . ? C83 C84 1.30(2) . ? C84 C85 1.35(2) . ? C85 C86 1.347(16) . ? Pt3 P5 2.217(3) . ? Pt3 P6 2.230(3) . ? Pt3 Cl5 2.338(3) . ? Pt3 Cl6 2.343(3) . ? P5 C101 1.797(11) . ? P5 C91 1.815(10) . ? P5 C5 1.870(10) . ? P6 C121 1.817(11) . ? P6 C111 1.817(11) . ? P6 C6 1.859(11) . ? C5 C6 1.539(14) 2_557 ? C5 C6 1.542(13) . ? C6 C5 1.539(14) 2_557 ? C91 C96 1.364(13) . ? C91 C92 1.377(14) . ? C92 C93 1.383(14) . ? C93 C94 1.312(16) . ? C94 C95 1.393(17) . ? C95 C96 1.396(15) . ? C101 C106 1.356(15) . ? C101 C102 1.368(16) . ? C102 C103 1.363(18) . ? C103 C104 1.35(2) . ? C104 C105 1.34(2) . ? C105 C106 1.355(17) . ? C111 C116 1.29(2) . ? C111 C112 1.340(17) . ? C112 C113 1.336(19) . ? C113 C114 1.28(2) . ? C114 C115 1.35(2) . ? C115 C116 1.41(2) . ? C121 C122 1.349(15) . ? C121 C126 1.379(15) . ? C122 C123 1.404(18) . ? C123 C124 1.32(2) . ? C124 C125 1.37(2) . ? C125 C126 1.433(16) . ? O1 C1L 1.217(18) . ? O2 C4L 1.224(18) . ? O3 C7L 1.19(2) . ? O4 C10L 1.21(3) . ? O5 C13L 1.16(4) . ? O6 C16L 1.36(7) . ? N1 C1L 1.250(17) . ? N1 C2L 1.41(2) . ? N1 C3L 1.42(2) . ? N2 C4L 1.277(18) . ? N2 C6L 1.408(18) . ? N2 C5L 1.45(2) . ? N3 C7L 1.44(4) . ? N3 C9L 1.48(3) . ? N3 C8L 1.53(3) . ? N4 C10L 1.40(3) . ? N4 C12L 1.42(2) . ? N4 C11L 1.48(2) . ? N5 C13L 1.43(3) . ? N5 C15L 1.51(3) . ? N5 C14L 1.52(5) . ? N6 N6 1.13(9) 2_565 ? N6 C17L 1.30(5) . ? N6 C16L 1.32(7) . ? N6 C17L 1.40(4) 2_565 ? C17L N6 1.40(4) 2_565 ? 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 P1 Pt1 Cl2 87.80(10) . . ? P1 Pt1 Cl1 174.66(10) . . ? Cl2 Pt1 Cl1 88.60(11) . . ? P1 Pt1 Se1 103.93(7) . . ? Cl2 Pt1 Se1 167.78(8) . . ? Cl1 Pt1 Se1 79.93(8) . . ? P4 Pt2 Cl3 86.87(10) . . ? P4 Pt2 Cl4 175.38(11) . . ? Cl3 Pt2 Cl4 88.55(11) . . ? P4 Pt2 Se2 103.67(8) . . ? Cl3 Pt2 Se2 169.46(8) . . ? Cl4 Pt2 Se2 80.92(9) . . ? P2 Se1 Pt1 102.74(8) . . ? P3 Se2 Pt2 103.68(9) . . ? C21 P1 C11 105.1(5) . . ? C21 P1 C1 102.6(5) . . ? C11 P1 C1 101.4(4) . . ? C21 P1 Pt1 113.6(3) . . ? C11 P1 Pt1 110.4(4) . . ? C1 P1 Pt1 121.9(3) . . ? C31 P2 C41 105.9(4) . . ? C31 P2 C2 110.4(5) . . ? C41 P2 C2 108.9(5) . . ? C31 P2 Se1 112.1(4) . . ? C41 P2 Se1 109.9(4) . . ? C2 P2 Se1 109.6(3) . . ? C61 P3 C51 107.1(5) . . ? C61 P3 C3 108.7(4) . . ? C51 P3 C3 108.1(5) . . ? C61 P3 Se2 112.1(4) . . ? C51 P3 Se2 109.1(4) . . ? C3 P3 Se2 111.5(4) . . ? C71 P4 C81 108.2(5) . . ? C71 P4 C4 102.6(5) . . ? C81 P4 C4 101.5(4) . . ? C71 P4 Pt2 110.7(4) . . ? C81 P4 Pt2 109.4(4) . . ? C4 P4 Pt2 123.3(3) . . ? C4 C1 C2 88.3(7) . . ? C4 C1 P1 115.7(7) . . ? C2 C1 P1 119.3(6) . . ? C3 C2 C1 88.1(7) . . ? C3 C2 P2 119.0(7) . . ? C1 C2 P2 122.1(6) . . ? C4 C3 C2 89.5(7) . . ? C4 C3 P3 122.3(7) . . ? C2 C3 P3 119.5(7) . . ? C3 C4 C1 89.0(7) . . ? C3 C4 P4 119.2(7) . . ? C1 C4 P4 114.8(7) . . ? C16 C11 C12 118.4(10) . . ? C16 C11 P1 123.9(9) . . ? C12 C11 P1 117.2(8) . . ? C13 C12 C11 120.6(11) . . ? C14 C13 C12 118.8(13) . . ? C15 C14 C13 119.9(13) . . ? C14 C15 C16 120.8(14) . . ? C11 C16 C15 121.3(12) . . ? C26 C21 C22 118.3(9) . . ? C26 C21 P1 119.5(8) . . ? C22 C21 P1 122.2(8) . . ? C21 C22 C23 121.2(11) . . ? C24 C23 C22 119.8(13) . . ? C23 C24 C25 120.4(11) . . ? C24 C25 C26 119.3(11) . . ? C21 C26 C25 121.0(11) . . ? C32 C31 C36 120.2(10) . . ? C32 C31 P2 120.0(9) . . ? C36 C31 P2 119.5(9) . . ? C31 C32 C33 120.4(12) . . ? C34 C33 C32 119.2(14) . . ? C35 C34 C33 119.7(13) . . ? C34 C35 C36 122.3(14) . . ? C31 C36 C35 117.9(13) . . ? C46 C41 C42 121.2(9) . . ? C46 C41 P2 119.9(8) . . ? C42 C41 P2 118.7(8) . . ? C43 C42 C41 117.0(11) . . ? C44 C43 C42 121.9(11) . . ? C43 C44 C45 121.2(10) . . ? C46 C45 C44 117.9(11) . . ? C45 C46 C41 120.8(11) . . ? C56 C51 C52 121.6(11) . . ? C56 C51 P3 118.2(9) . . ? C52 C51 P3 120.0(9) . . ? C53 C52 C51 121.4(13) . . ? C54 C53 C52 117.4(14) . . ? C53 C54 C55 124.5(14) . . ? C54 C55 C56 117.2(13) . . ? C51 C56 C55 118.0(13) . . ? C62 C61 C66 118.5(9) . . ? C62 C61 P3 120.4(8) . . ? C66 C61 P3 121.0(8) . . ? C61 C62 C63 121.0(11) . . ? C64 C63 C62 120.4(11) . . ? C63 C64 C65 119.3(11) . . ? C66 C65 C64 119.4(12) . . ? C65 C66 C61 121.5(11) . . ? C72 C71 C76 118.4(9) . . ? C72 C71 P4 120.0(8) . . ? C76 C71 P4 121.6(8) . . ? C71 C72 C73 122.4(10) . . ? C74 C73 C72 118.8(11) . . ? C73 C74 C75 121.4(11) . . ? C76 C75 C74 118.0(12) . . ? C75 C76 C71 121.1(11) . . ? C86 C81 C82 118.4(11) . . ? C86 C81 P4 118.4(9) . . ? C82 C81 P4 123.1(10) . . ? C81 C82 C83 116.3(15) . . ? C84 C83 C82 124.9(17) . . ? C83 C84 C85 116.9(17) . . ? C86 C85 C84 123.2(16) . . ? C85 C86 C81 120.2(13) . . ? P5 Pt3 P6 86.83(10) . . ? P5 Pt3 Cl5 179.10(10) . . ? P6 Pt3 Cl5 93.22(10) . . ? P5 Pt3 Cl6 90.90(10) . . ? P6 Pt3 Cl6 173.47(11) . . ? Cl5 Pt3 Cl6 88.96(10) . . ? C101 P5 C91 106.7(5) . . ? C101 P5 C5 104.6(5) . . ? C91 P5 C5 106.6(4) . . ? C101 P5 Pt3 113.4(4) . . ? C91 P5 Pt3 115.6(4) . . ? C5 P5 Pt3 109.3(3) . . ? C121 P6 C111 106.0(5) . . ? C121 P6 C6 105.3(5) . . ? C111 P6 C6 106.0(5) . . ? C121 P6 Pt3 119.6(4) . . ? C111 P6 Pt3 109.7(4) . . ? C6 P6 Pt3 109.4(3) . . ? C6 C5 C6 89.6(7) 2_557 . ? C6 C5 P5 116.3(7) 2_557 . ? C6 C5 P5 113.9(7) . . ? C5 C6 C5 90.4(7) 2_557 . ? C5 C6 P6 115.2(7) 2_557 . ? C5 C6 P6 114.0(7) . . ? C96 C91 C92 118.4(9) . . ? C96 C91 P5 124.2(8) . . ? C92 C91 P5 117.4(7) . . ? C91 C92 C93 120.4(10) . . ? C94 C93 C92 121.0(12) . . ? C93 C94 C95 120.7(12) . . ? C94 C95 C96 118.3(11) . . ? C91 C96 C95 120.9(11) . . ? C106 C101 C102 114.1(11) . . ? C106 C101 P5 121.8(10) . . ? C102 C101 P5 124.1(9) . . ? C103 C102 C101 123.1(13) . . ? C104 C103 C102 120.8(15) . . ? C105 C104 C103 117.3(14) . . ? C104 C105 C106 121.3(15) . . ? C105 C106 C101 123.4(13) . . ? C116 C111 C112 114.8(13) . . ? C116 C111 P6 124.1(11) . . ? C112 C111 P6 120.9(10) . . ? C113 C112 C111 123.2(14) . . ? C114 C113 C112 121.8(15) . . ? C113 C114 C115 119.1(15) . . ? C114 C115 C116 117(2) . . ? C111 C116 C115 124.0(18) . . ? C122 C121 C126 120.6(11) . . ? C122 C121 P6 121.3(10) . . ? C126 C121 P6 118.1(8) . . ? C121 C122 C123 121.3(14) . . ? C124 C123 C122 119.0(15) . . ? C123 C124 C125 122.0(14) . . ? C124 C125 C126 119.4(15) . . ? C121 C126 C125 117.6(13) . . ? C1L N1 C2L 116.9(17) . . ? C1L N1 C3L 123.7(17) . . ? C2L N1 C3L 119.3(17) . . ? C4L N2 C6L 123.9(15) . . ? C4L N2 C5L 118.1(17) . . ? C6L N2 C5L 117.8(17) . . ? C7L N3 C9L 109(3) . . ? C7L N3 C8L 123(3) . . ? C9L N3 C8L 128(2) . . ? C10L N4 C12L 116(2) . . ? C10L N4 C11L 122(2) . . ? C12L N4 C11L 122(2) . . ? C13L N5 C15L 136(4) . . ? C13L N5 C14L 110(3) . . ? C15L N5 C14L 113(3) . . ? N6 N6 C17L 70(5) 2_565 . ? N6 N6 C16L 169(6) 2_565 . ? C17L N6 C16L 108(4) . . ? N6 N6 C17L 61(3) 2_565 2_565 ? C17L N6 C17L 131(5) . 2_565 ? C16L N6 C17L 121(5) . 2_565 ? O1 C1L N1 129.3(16) . . ? O2 C4L N2 131.3(14) . . ? O3 C7L N3 113(4) . . ? O4 C10L N4 126(3) . . ? O5 C13L N5 139(4) . . ? N6 C16L O6 109(5) . . ? N6 C17L N6 49(5) . 2_565 ? 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 P1 Pt1 Se1 P2 20.80(10) . . . . ? Cl2 Pt1 Se1 P2 -142.6(4) . . . . ? Cl1 Pt1 Se1 P2 -162.97(10) . . . . ? P4 Pt2 Se2 P3 19.94(11) . . . . ? Cl3 Pt2 Se2 P3 -158.2(4) . . . . ? Cl4 Pt2 Se2 P3 -160.57(11) . . . . ? Cl2 Pt1 P1 C21 72.1(4) . . . . ? Cl1 Pt1 P1 C21 119.7(11) . . . . ? Se1 Pt1 P1 C21 -104.5(3) . . . . ? Cl2 Pt1 P1 C11 -45.7(4) . . . . ? Cl1 Pt1 P1 C11 1.9(12) . . . . ? Se1 Pt1 P1 C11 137.8(4) . . . . ? Cl2 Pt1 P1 C1 -164.4(3) . . . . ? Cl1 Pt1 P1 C1 -116.8(11) . . . . ? Se1 Pt1 P1 C1 19.1(3) . . . . ? Pt1 Se1 P2 C31 61.1(3) . . . . ? Pt1 Se1 P2 C41 178.7(3) . . . . ? Pt1 Se1 P2 C2 -61.8(3) . . . . ? Pt2 Se2 P3 C61 62.9(3) . . . . ? Pt2 Se2 P3 C51 -178.6(3) . . . . ? Pt2 Se2 P3 C3 -59.2(3) . . . . ? Cl3 Pt2 P4 C71 74.1(4) . . . . ? Cl4 Pt2 P4 C71 80.7(13) . . . . ? Se2 Pt2 P4 C71 -105.5(4) . . . . ? Cl3 Pt2 P4 C81 -45.1(4) . . . . ? Cl4 Pt2 P4 C81 -38.5(14) . . . . ? Se2 Pt2 P4 C81 135.3(4) . . . . ? Cl3 Pt2 P4 C4 -164.1(4) . . . . ? Cl4 Pt2 P4 C4 -157.5(12) . . . . ? Se2 Pt2 P4 C4 16.3(4) . . . . ? C21 P1 C1 C4 -154.0(7) . . . . ? C11 P1 C1 C4 -45.4(8) . . . . ? Pt1 P1 C1 C4 77.5(7) . . . . ? C21 P1 C1 C2 102.6(7) . . . . ? C11 P1 C1 C2 -148.9(7) . . . . ? Pt1 P1 C1 C2 -25.9(8) . . . . ? C4 C1 C2 C3 -16.9(7) . . . . ? P1 C1 C2 C3 101.9(7) . . . . ? C4 C1 C2 P2 -140.3(7) . . . . ? P1 C1 C2 P2 -21.5(11) . . . . ? C31 P2 C2 C3 -160.8(7) . . . . ? C41 P2 C2 C3 83.3(8) . . . . ? Se1 P2 C2 C3 -36.9(8) . . . . ? C31 P2 C2 C1 -53.2(9) . . . . ? C41 P2 C2 C1 -169.1(8) . . . . ? Se1 P2 C2 C1 70.7(8) . . . . ? C1 C2 C3 C4 17.0(7) . . . . ? P2 C2 C3 C4 143.1(7) . . . . ? C1 C2 C3 P3 144.6(7) . . . . ? P2 C2 C3 P3 -89.3(9) . . . . ? C61 P3 C3 C4 -54.5(9) . . . . ? C51 P3 C3 C4 -170.5(8) . . . . ? Se2 P3 C3 C4 69.5(8) . . . . ? C61 P3 C3 C2 -164.8(7) . . . . ? C51 P3 C3 C2 79.2(9) . . . . ? Se2 P3 C3 C2 -40.7(8) . . . . ? C2 C3 C4 C1 -17.2(7) . . . . ? P3 C3 C4 C1 -142.5(8) . . . . ? C2 C3 C4 P4 100.9(8) . . . . ? P3 C3 C4 P4 -24.4(11) . . . . ? C2 C1 C4 C3 17.0(7) . . . . ? P1 C1 C4 C3 -105.0(7) . . . . ? C2 C1 C4 P4 -105.0(7) . . . . ? P1 C1 C4 P4 133.0(6) . . . . ? C71 P4 C4 C3 104.9(8) . . . . ? C81 P4 C4 C3 -143.2(8) . . . . ? Pt2 P4 C4 C3 -20.6(9) . . . . ? C71 P4 C4 C1 -151.5(7) . . . . ? C81 P4 C4 C1 -39.6(8) . . . . ? Pt2 P4 C4 C1 83.0(7) . . . . ? C21 P1 C11 C16 6.5(11) . . . . ? C1 P1 C11 C16 -100.1(10) . . . . ? Pt1 P1 C11 C16 129.4(9) . . . . ? C21 P1 C11 C12 -165.7(8) . . . . ? C1 P1 C11 C12 87.8(8) . . . . ? Pt1 P1 C11 C12 -42.8(8) . . . . ? C16 C11 C12 C13 5.1(15) . . . . ? P1 C11 C12 C13 177.7(8) . . . . ? C11 C12 C13 C14 -1.7(16) . . . . ? C12 C13 C14 C15 -1.8(19) . . . . ? C13 C14 C15 C16 2(2) . . . . ? C12 C11 C16 C15 -5.0(17) . . . . ? P1 C11 C16 C15 -177.1(10) . . . . ? C14 C15 C16 C11 2(2) . . . . ? C11 P1 C21 C26 112.7(8) . . . . ? C1 P1 C21 C26 -141.6(8) . . . . ? Pt1 P1 C21 C26 -8.1(9) . . . . ? C11 P1 C21 C22 -64.9(10) . . . . ? C1 P1 C21 C22 40.7(10) . . . . ? Pt1 P1 C21 C22 174.3(8) . . . . ? C26 C21 C22 C23 0.4(17) . . . . ? P1 C21 C22 C23 178.0(9) . . . . ? C21 C22 C23 C24 0.7(19) . . . . ? C22 C23 C24 C25 -1(2) . . . . ? C23 C24 C25 C26 -0.4(19) . . . . ? C22 C21 C26 C25 -1.5(15) . . . . ? P1 C21 C26 C25 -179.2(8) . . . . ? C24 C25 C26 C21 1.5(17) . . . . ? C41 P2 C31 C32 84.1(9) . . . . ? C2 P2 C31 C32 -33.6(10) . . . . ? Se1 P2 C31 C32 -156.0(8) . . . . ? C41 P2 C31 C36 -89.6(9) . . . . ? C2 P2 C31 C36 152.8(8) . . . . ? Se1 P2 C31 C36 30.3(9) . . . . ? C36 C31 C32 C33 -0.7(17) . . . . ? P2 C31 C32 C33 -174.4(9) . . . . ? C31 C32 C33 C34 2.2(18) . . . . ? C32 C33 C34 C35 -5(2) . . . . ? C33 C34 C35 C36 6(2) . . . . ? C32 C31 C36 C35 1.5(17) . . . . ? P2 C31 C36 C35 175.2(9) . . . . ? C34 C35 C36 C31 -4(2) . . . . ? C31 P2 C41 C46 -72.0(9) . . . . ? C2 P2 C41 C46 46.7(9) . . . . ? Se1 P2 C41 C46 166.7(7) . . . . ? C31 P2 C41 C42 102.5(8) . . . . ? C2 P2 C41 C42 -138.8(8) . . . . ? Se1 P2 C41 C42 -18.8(8) . . . . ? C46 C41 C42 C43 1.4(15) . . . . ? P2 C41 C42 C43 -173.1(8) . . . . ? C41 C42 C43 C44 -0.3(17) . . . . ? C42 C43 C44 C45 -1.2(19) . . . . ? C43 C44 C45 C46 1.4(18) . . . . ? C44 C45 C46 C41 -0.3(16) . . . . ? C42 C41 C46 C45 -1.1(15) . . . . ? P2 C41 C46 C45 173.3(8) . . . . ? C61 P3 C51 C56 -62.2(9) . . . . ? C3 P3 C51 C56 54.8(9) . . . . ? Se2 P3 C51 C56 176.3(8) . . . . ? C61 P3 C51 C52 112.4(9) . . . . ? C3 P3 C51 C52 -130.6(8) . . . . ? Se2 P3 C51 C52 -9.2(9) . . . . ? C56 C51 C52 C53 -1.0(17) . . . . ? P3 C51 C52 C53 -175.3(10) . . . . ? C51 C52 C53 C54 0.1(19) . . . . ? C52 C53 C54 C55 1(2) . . . . ? C53 C54 C55 C56 -1(2) . . . . ? C52 C51 C56 C55 0.9(16) . . . . ? P3 C51 C56 C55 175.3(8) . . . . ? C54 C55 C56 C51 0.0(17) . . . . ? C51 P3 C61 C62 -87.3(9) . . . . ? C3 P3 C61 C62 156.1(8) . . . . ? Se2 P3 C61 C62 32.3(9) . . . . ? C51 P3 C61 C66 89.0(9) . . . . ? C3 P3 C61 C66 -27.6(10) . . . . ? Se2 P3 C61 C66 -151.3(8) . . . . ? C66 C61 C62 C63 1.2(15) . . . . ? P3 C61 C62 C63 177.6(8) . . . . ? C61 C62 C63 C64 -0.5(17) . . . . ? C62 C63 C64 C65 -0.8(18) . . . . ? C63 C64 C65 C66 1.4(18) . . . . ? C64 C65 C66 C61 -0.8(18) . . . . ? C62 C61 C66 C65 -0.5(16) . . . . ? P3 C61 C66 C65 -176.9(9) . . . . ? C81 P4 C71 C72 118.1(9) . . . . ? C4 P4 C71 C72 -135.1(8) . . . . ? Pt2 P4 C71 C72 -1.7(9) . . . . ? C81 P4 C71 C76 -62.1(10) . . . . ? C4 P4 C71 C76 44.7(10) . . . . ? Pt2 P4 C71 C76 178.0(8) . . . . ? C76 C71 C72 C73 -0.9(16) . . . . ? P4 C71 C72 C73 178.8(8) . . . . ? C71 C72 C73 C74 0.6(17) . . . . ? C72 C73 C74 C75 -0.6(19) . . . . ? C73 C74 C75 C76 1(2) . . . . ? C74 C75 C76 C71 -1.0(19) . . . . ? C72 C71 C76 C75 1.1(17) . . . . ? P4 C71 C76 C75 -178.6(9) . . . . ? C71 P4 C81 C86 -160.1(9) . . . . ? C4 P4 C81 C86 92.4(9) . . . . ? Pt2 P4 C81 C86 -39.4(10) . . . . ? C71 P4 C81 C82 20.8(11) . . . . ? C4 P4 C81 C82 -86.7(10) . . . . ? Pt2 P4 C81 C82 141.5(9) . . . . ? C86 C81 C82 C83 2.2(17) . . . . ? P4 C81 C82 C83 -178.7(9) . . . . ? C81 C82 C83 C84 -3(2) . . . . ? C82 C83 C84 C85 2(3) . . . . ? C83 C84 C85 C86 1(2) . . . . ? C84 C85 C86 C81 -2(2) . . . . ? C82 C81 C86 C85 0.5(17) . . . . ? P4 C81 C86 C85 -178.6(9) . . . . ? P6 Pt3 P5 C101 -93.5(4) . . . . ? Cl5 Pt3 P5 C101 -1(7) . . . . ? Cl6 Pt3 P5 C101 80.3(4) . . . . ? P6 Pt3 P5 C91 142.8(4) . . . . ? Cl5 Pt3 P5 C91 -124(7) . . . . ? Cl6 Pt3 P5 C91 -43.3(4) . . . . ? P6 Pt3 P5 C5 22.7(3) . . . . ? Cl5 Pt3 P5 C5 116(7) . . . . ? Cl6 Pt3 P5 C5 -163.5(3) . . . . ? P5 Pt3 P6 C121 -143.9(4) . . . . ? Cl5 Pt3 P6 C121 37.0(4) . . . . ? Cl6 Pt3 P6 C121 146.4(9) . . . . ? P5 Pt3 P6 C111 93.5(4) . . . . ? Cl5 Pt3 P6 C111 -85.6(4) . . . . ? Cl6 Pt3 P6 C111 23.7(10) . . . . ? P5 Pt3 P6 C6 -22.4(3) . . . . ? Cl5 Pt3 P6 C6 158.5(3) . . . . ? Cl6 Pt3 P6 C6 -92.1(9) . . . . ? C101 P5 C5 C6 -154.5(7) . . . 2_557 ? C91 P5 C5 C6 -41.7(8) . . . 2_557 ? Pt3 P5 C5 C6 83.8(7) . . . 2_557 ? C101 P5 C5 C6 103.3(7) . . . . ? C91 P5 C5 C6 -143.8(7) . . . . ? Pt3 P5 C5 C6 -18.3(8) . . . . ? C6 C5 C6 C5 0.000(2) 2_557 . . 2_557 ? P5 C5 C6 C5 118.7(8) . . . 2_557 ? C6 C5 C6 P6 -118.0(8) 2_557 . . . ? P5 C5 C6 P6 0.7(9) . . . . ? C121 P6 C6 C5 44.2(8) . . . 2_557 ? C111 P6 C6 C5 156.3(7) . . . 2_557 ? Pt3 P6 C6 C5 -85.5(7) . . . 2_557 ? C121 P6 C6 C5 146.9(7) . . . . ? C111 P6 C6 C5 -101.1(7) . . . . ? Pt3 P6 C6 C5 17.1(8) . . . . ? C101 P5 C91 C96 10.4(11) . . . . ? C5 P5 C91 C96 -101.0(10) . . . . ? Pt3 P5 C91 C96 137.5(9) . . . . ? C101 P5 C91 C92 -168.2(8) . . . . ? C5 P5 C91 C92 80.5(9) . . . . ? Pt3 P5 C91 C92 -41.1(9) . . . . ? C96 C91 C92 C93 3.7(16) . . . . ? P5 C91 C92 C93 -177.6(9) . . . . ? C91 C92 C93 C94 -0.2(18) . . . . ? C92 C93 C94 C95 -3(2) . . . . ? C93 C94 C95 C96 2(2) . . . . ? C92 C91 C96 C95 -4.2(17) . . . . ? P5 C91 C96 C95 177.2(9) . . . . ? C94 C95 C96 C91 1.3(18) . . . . ? C91 P5 C101 C106 105.1(10) . . . . ? C5 P5 C101 C106 -142.3(10) . . . . ? Pt3 P5 C101 C106 -23.3(11) . . . . ? C91 P5 C101 C102 -75.0(11) . . . . ? C5 P5 C101 C102 37.7(11) . . . . ? Pt3 P5 C101 C102 156.6(10) . . . . ? C106 C101 C102 C103 1(2) . . . . ? P5 C101 C102 C103 -179.3(12) . . . . ? C101 C102 C103 C104 0(3) . . . . ? C102 C103 C104 C105 -2(3) . . . . ? C103 C104 C105 C106 3(3) . . . . ? C104 C105 C106 C101 -3(3) . . . . ? C102 C101 C106 C105 1(2) . . . . ? P5 C101 C106 C105 -179.2(12) . . . . ? C121 P6 C111 C116 112.1(19) . . . . ? C6 P6 C111 C116 0(2) . . . . ? Pt3 P6 C111 C116 -117.5(19) . . . . ? C121 P6 C111 C112 -73.2(13) . . . . ? C6 P6 C111 C112 175.2(12) . . . . ? Pt3 P6 C111 C112 57.3(13) . . . . ? C116 C111 C112 C113 -4(3) . . . . ? P6 C111 C112 C113 -179.3(15) . . . . ? C111 C112 C113 C114 1(3) . . . . ? C112 C113 C114 C115 1(4) . . . . ? C113 C114 C115 C116 0(5) . . . . ? C112 C111 C116 C115 5(4) . . . . ? P6 C111 C116 C115 -180(3) . . . . ? C114 C115 C116 C111 -4(5) . . . . ? C111 P6 C121 C122 -25.7(10) . . . . ? C6 P6 C121 C122 86.4(10) . . . . ? Pt3 P6 C121 C122 -150.2(8) . . . . ? C111 P6 C121 C126 154.8(9) . . . . ? C6 P6 C121 C126 -93.1(9) . . . . ? Pt3 P6 C121 C126 30.3(10) . . . . ? C126 C121 C122 C123 -1.0(18) . . . . ? P6 C121 C122 C123 179.5(10) . . . . ? C121 C122 C123 C124 1(2) . . . . ? C122 C123 C124 C125 0(2) . . . . ? C123 C124 C125 C126 -1(2) . . . . ? C122 C121 C126 C125 -0.2(17) . . . . ? P6 C121 C126 C125 179.3(8) . . . . ? C124 C125 C126 C121 1.3(18) . . . . ? C2L N1 C1L O1 4(3) . . . . ? C3L N1 C1L O1 -172.7(19) . . . . ? C6L N2 C4L O2 -179.4(18) . . . . ? C5L N2 C4L O2 5(4) . . . . ? C9L N3 C7L O3 -13(5) . . . . ? C8L N3 C7L O3 168(4) . . . . ? C12L N4 C10L O4 6(4) . . . . ? C11L N4 C10L O4 -173(3) . . . . ? C15L N5 C13L O5 -172(4) . . . . ? C14L N5 C13L O5 -4(5) . . . . ? N6 N6 C16L O6 98(32) 2_565 . . . ? C17L N6 C16L O6 175(4) . . . . ? C17L N6 C16L O6 5(5) 2_565 . . . ? C16L N6 C17L N6 -168(6) . . . 2_565 ? C17L N6 C17L N6 0.000(3) 2_565 . . 2_565 ? _diffrn_reflns_theta_full 21.54 _diffrn_measured_fraction 0.990 _refine_diff_density_max 1.690 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.100 #============================================================================ #===END