# Copyright The Royal Society of Chemistry, 1998 data_exw28 _audit_creation_date 98-04-28 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety 'C66 H54 P4 PT2' #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C66 H54 P4 PT2' #ActaC _chemical_formula_weight 1361.23 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection ; MSC/AFC diffractometer control software (Molecular Structure Corporation, 1992) ; _computing_cell_refinement ; MSC/AFC diffractometer control software (Molecular Structure Corporation, 1992) ; _computing_data_reduction ; xtal_DIFDAT_SORTRF_ADDREF (Hall and Stewart, 1990) ; _computing_structure_solution ; SIR92 (Altomare et al, 1993), DIRDIF94 (Beurskens et al, 1994) ; _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 14.3450(10) #ActaC _cell_length_b 22.311(3) #ActaC _cell_length_c 17.459(3) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 97.930(10) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 5534.3(13) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 35.21 #ActaC _cell_measurement_theta_max 44.50 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21/c_1 #ActaC _symmetry_space_group_name_Hall -p_2ybc #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _exptl_crystal_description plate #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour needle #ActaC _exptl_crystal_size_max 0.44 #ActaC _exptl_crystal_size_mid 0.08 #ActaC _exptl_crystal_size_min 0.04 #ActaC _exptl_crystal_density_diffrn 1.634 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 2664 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 108.34 #ActaC _exptl_absorpt_correction_type 'psi scan' #ActaC _exptl_absorpt_correction_T_min 0.735 #ActaC _exptl_absorpt_correction_T_max 1.000 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 1.54178 #ActaC _diffrn_radiation_type xray_tube #ActaC _diffrn_radiation_source Cu #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector scintillation #ActaC _diffrn_measurement_device 'Rigaku AFC6R' #ActaC _diffrn_measurement_method theta/2theta #ActaC _diffrn_standards_number 3 #ActaC _diffrn_standards_interval_count 150 #ActaC _diffrn_standards_interval_time ? #ActaC _diffrn_standards_decay_% 0.125 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_obs_criterion 'refl observed if Inet > 3\s(Inet)' _diffrn_reflns_number 8796 #ActaC _diffrn_reflns_av_R_equivalents .074 #ActaC _diffrn_reflns_limit_h_min -16 #ActaC _diffrn_reflns_limit_h_max 15 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 25 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 19 #ActaC _diffrn_reflns_theta_min 1.50 #ActaC _diffrn_reflns_theta_max 60.07 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 264 .017 .009 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 216 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 16 .283 .434 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 PT ? 0 8 -5.233 6.925 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC PT1 .18327(3) .70947(2) .26472(3) .0430(3) Uani ? ? PT2 .33315(4) .63947(3) .29735(4) .0601(4) Uani ? ? P1 .1897(2) .61219(15) .2341(2) .0492(17) Uani ? ? P2 .3889(2) .71768(17) .3727(2) .057(2) Uani ? ? P3 .0361(2) .74216(14) .2279(2) .0485(17) Uani ? ? P4 .4412(3) .5660(2) .2836(3) .088(3) Uani ? ? C1 .1821(9) .5844(6) .1349(6) .060(3) Uiso ? ? C2 .1790(11) .6248(5) .0762(8) .082(5) Uiso ? ? C3 .1844(13) .6050(6) .0006(7) .091(5) Uiso ? ? C4 .2003(15) .5456(7) -.0131(7) .105(6) Uiso ? ? C5 .2089(18) .5054(6) .0469(10) .124(8) Uiso ? ? C6 .1999(13) .5248(6) .1216(8) .091(5) Uiso ? ? C7 .1198(9) .5575(6) .2833(8) .064(4) Uiso ? ? C8 .0516(13) .5221(9) .2420(7) .109(7) Uiso ? ? C9 -.0046(14) .4843(10) .2814(11) .129(8) Uiso ? ? C10 .0077(16) .4834(10) .3614(12) .140(9) Uiso ? ? C11 .0724(17) .5211(11) .4025(8) .133(9) Uiso ? ? C12 .1280(12) .5593(8) .3631(9) .099(6) Uiso ? ? C13 .2481(7) .7911(4) .3056(7) .047(3) Uiso ? ? C14 .2066(6) .8462(5) .2845(8) .054(3) Uiso ? ? C15 .2575(8) .8993(4) .3012(9) .071(4) Uiso ? ? C16 .3508(8) .8968(4) .3371(9) .071(4) Uiso ? ? C17 .3903(7) .8428(5) .3607(9) .069(4) Uiso ? ? C18 .3376(8) .7890(4) .3457(8) .054(3) Uiso ? ? C19 .3641(12) .7080(6) .4741(7) .069(4) Uiso ? ? C20 .3589(13) .7555(5) .5233(9) .091(5) Uiso ? ? C21 .3520(16) .7450(7) .6020(9) .110(7) Uiso ? ? C22 .3483(15) .6882(8) .6285(8) .107(7) Uiso ? ? C23 .3495(17) .6405(6) .5782(11) .124(8) Uiso ? ? C24 .3596(15) .6508(6) .5007(9) .102(6) Uiso ? ? C25 .5161(8) .7325(7) .3860(9) .072(4) Uiso ? ? C26 .5658(13) .7369(11) .4587(9) .130(8) Uiso ? ? C27 .6631(13) .7476(11) .4678(9) .149(10) Uiso ? ? C28 .7095(9) .7480(10) .4047(11) .104(6) Uiso ? ? C29 .6602(11) .7413(11) .3319(9) .112(7) Uiso ? ? C30 .5622(11) .7351(10) .3225(7) .107(7) Uiso ? ? C31 .0132(7) .7843(5) .1371(6) .051(3) Uiso ? ? C32 .0906(6) .8045(6) .1044(7) .058(3) Uiso ? ? C33 .0772(8) .8364(7) .0349(8) .080(5) Uiso ? ? C34 -.0128(10) .8510(7) .0010(8) .082(5) Uiso ? ? C35 -.0904(7) .8309(8) .0338(9) .089(5) Uiso ? ? C36 -.0772(7) .7978(6) .1022(8) .065(4) Uiso ? ? C37 -.0065(8) .7893(5) .3024(6) .047(3) Uiso ? ? C38 -.0681(11) .8370(6) .2861(6) .075(4) Uiso ? ? C39 -.1006(12) .8686(7) .3466(9) .095(6) Uiso ? ? C40 -.0698(12) .8526(7) .4234(7) .086(5) Uiso ? ? C41 -.0084(12) .8052(7) .4396(6) .082(5) Uiso ? ? C42 .0240(10) .7733(6) .3789(7) .068(4) Uiso ? ? C43 -.0544(8) .6832(5) .2129(7) .053(3) Uiso ? ? C44 -.1163(13) .6743(8) .2646(9) .100(6) Uiso ? ? C45 -.1836(13) .6287(10) .2520(11) .122(8) Uiso ? ? C46 -.1863(13) .5924(8) .1886(12) .118(7) Uiso ? ? C47 -.1246(12) .6021(7) .1355(9) .091(5) Uiso ? ? C48 -.0594(10) .6478(7) .1472(8) .076(4) Uiso ? ? C49 .5498(9) .5573(7) .3485(9) .073(4) Uiso ? ? C50 .5489(12) .5724(11) .4249(12) .150(10) Uiso ? ? C51 .6305(18) .5671(15) .4776(10) .216(17) Uiso ? ? C52 .7086(13) .5421(11) .4553(11) .121(8) Uiso ? ? C53 .7082(11) .5241(11) .3803(12) .128(8) Uiso ? ? C54 .6278(13) .5332(10) .3261(8) .106(7) Uiso ? ? C55 .4802(18) .5767(12) .1950(13) .127(8) Uiso ? ? C56 .549(2) .6167(12) .1830(16) .156(11) Uiso ? ? C57 .575(2) .6230(17) .109(2) .209(16) Uiso ? ? C58 .530(3) .591(2) .0488(15) .213(17) Uiso ? ? C59 .458(4) .553(3) .0605(19) .41(4) Uiso ? ? C60 .432(3) .546(2) .134(2) .40(4) Uiso ? ? C61 .3986(13) .4860(7) .2906(11) .105(6) Uiso ? ? C62 .3144(12) .4748(8) .3191(10) .114(7) Uiso ? ? C63 .2826(12) .4161(10) .3235(12) .121(8) Uiso ? ? C64 .342(2) .3684(8) .313(4) .15(2) Uiso ? ? C65 .430(2) .3796(10) .291(4) .15(2) Uiso ? ? C66 .458(2) .4388(12) .279(3) .126(17) Uiso ? ? C66' .4259(19) .4481(12) .2346(17) .081(10) Uiso ? ? C65' .386(3) .3902(13) .226(2) .110(14) Uiso ? ? C64' .315(5) .3726(14) .274(4) .21(4) Uiso ? ? H2 .17321 .66640 .08636 .10000 Uiso ? ? H3 .17700 .63277 -.04111 .10000 Uiso ? ? H4 .20538 .53227 -.06406 .10000 Uiso ? ? H5 .22096 .46432 .03762 .10000 Uiso ? ? H6 .20604 .49702 .16319 .10000 Uiso ? ? H8 .04247 .52327 .18710 .10000 Uiso ? ? H9 -.05089 .45946 .25300 .10000 Uiso ? ? H10 -.02835 .45671 .38797 .10000 Uiso ? ? H11 .07946 .52141 .45744 .10000 Uiso ? ? H12 .17115 .58621 .39128 .10000 Uiso ? ? H14 .14378 .84775 .25884 .10000 Uiso ? ? H15 .22864 .93690 .28817 .10000 Uiso ? ? H16 .38679 .93258 .34510 .10000 Uiso ? ? H17 .45277 .84126 .38712 .10000 Uiso ? ? H20 .35999 .79536 .50439 .10000 Uiso ? ? H21 .35001 .77784 .63635 .10000 Uiso ? ? H22 .34482 .68111 .68167 .10000 Uiso ? ? H23 .34351 .60072 .59624 .10000 Uiso ? ? H24 .36338 .61795 .46672 .10000 Uiso ? ? H26 .53447 .73264 .50290 .10000 Uiso ? ? H27 .69650 .75464 .51782 .10000 Uiso ? ? H28 .77594 .75288 .41110 .10000 Uiso ? ? H29 .69265 .74088 .28798 .10000 Uiso ? ? H30 .52774 .73261 .27205 .10000 Uiso ? ? H32 .15248 .79657 .12931 .10000 Uiso ? ? H33 .12993 .84795 .01084 .10000 Uiso ? ? H34 -.02174 .87484 -.04449 .10000 Uiso ? ? H35 -.15230 .83966 .00944 .10000 Uiso ? ? H36 -.13006 .78462 .12493 .10000 Uiso ? ? H38 -.08821 .84822 .23400 .10000 Uiso ? ? H39 -.14351 .90086 .33538 .10000 Uiso ? ? H40 -.09117 .87443 .46434 .10000 Uiso ? ? H41 .01199 .79403 .49176 .10000 Uiso ? ? H42 .06671 .74093 .39009 .10000 Uiso ? ? H44 -.11364 .69908 .30909 .10000 Uiso ? ? H45 -.22745 .62297 .28744 .10000 Uiso ? ? H46 -.23056 .56056 .18100 .10000 Uiso ? ? H47 -.12721 .57735 .09103 .10000 Uiso ? ? H48 -.01788 .65497 .11026 .10000 Uiso ? ? H50 .49252 .58646 .44163 .10000 Uiso ? ? H51 .63153 .58096 .52913 .10000 Uiso ? ? H52 .76369 .53704 .49174 .10000 Uiso ? ? H53 .76222 .50552 .36503 .10000 Uiso ? ? H54 .62835 .52247 .27347 .10000 Uiso ? ? H56 .57830 .64035 .22474 .10000 Uiso ? ? H57 .62526 .64938 .10115 .10000 Uiso ? ? H58 .54790 .59590 -.00132 .10000 Uiso ? ? H59 .42597 .53048 .01827 .10000 Uiso ? ? H60 .38108 .52072 .14117 .10000 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC PT1 .0387(3) .0429(3) .0475(4) .00219(19) .0069(2) -.0013(2) PT2 .0455(4) .0618(4) .0709(5) .0140(3) .0006(3) -.0157(3) P1 .0455(18) .0484(18) .055(2) .0016(13) .0103(15) -.0042(15) P2 .0383(17) .072(2) .059(2) .0041(15) .0040(15) -.0081(19) P3 .0388(16) .0481(17) .058(2) .0014(13) .0056(14) .0054(16) P4 .056(2) .093(3) .109(4) .024(2) -.009(2) -.036(3) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme 'calc, w=1/(\s^2^(F) + 0.016F^2^)' #ActaC _refine_ls_hydrogen_treatment fixed #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 6022 #ActaC _refine_ls_number_parameters 331 #ActaC _refine_ls_number_restraints 141 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .087 #ActaC _refine_ls_R_factor_obs .066 #ActaC _refine_ls_wR_factor_all .114 #ActaC _refine_ls_wR_factor_obs .104 #ActaC _refine_ls_goodness_of_fit_all 1.403 #ActaC _refine_ls_goodness_of_fit_obs 1.492 #ActaC _refine_ls_shift/esd_max 0.043 #ActaC _refine_ls_shift/esd_mean 0.011 #ActaC _refine_diff_density_min -1.794 #ActaC _refine_diff_density_max 2.627 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC PT1 PT2 2.6549(8) . . ? PT1 P1 2.240(3) . . ? PT1 P3 2.242(3) . . ? PT1 C13 2.123(9) . . ? PT2 P1 2.280(3) . . ? PT2 P2 2.264(4) . . ? PT2 P4 2.291(5) . . ? P1 C1 1.828(11) . . ? P1 C7 1.864(14) . . ? P2 C18 1.788(10) . . ? P2 C19 1.866(13) . . ? P2 C25 1.837(12) . . ? P3 C31 1.834(11) . . ? P3 C37 1.842(11) . . ? P3 C43 1.841(12) . . ? P4 C49 1.806(14) . . ? P4 C55 1.73(3) . . ? P4 C61 1.896(17) . . ? C1 C2 1.361(17) . . ? C1 C6 1.380(18) . . ? C2 C3 1.40(2) . . ? C2 H2 .950(10) . . ? C3 C4 1.37(2) . . ? C3 H3 .950(13) . . ? C4 C5 1.37(2) . . ? C4 H4 .950(14) . . ? C5 C6 1.40(2) . . ? C5 H5 .950(14) . . ? C6 H6 .950(13) . . ? C7 C8 1.38(2) . . ? C7 C12 1.38(2) . . ? C8 C9 1.41(3) . . ? C8 H8 .950(12) . . ? C9 C10 1.38(3) . . ? C9 H9 .95(2) . . ? C10 C11 1.38(3) . . ? C10 H10 .95(2) . . ? C11 C12 1.41(3) . . ? C11 H11 .950(14) . . ? C12 H12 .950(16) . . ? C13 C14 1.392(13) . . ? C13 C18 1.377(15) . . ? C14 C15 1.401(14) . . ? C14 H14 .950(9) . . ? C15 C16 1.398(16) . . ? C15 H15 .950(10) . . ? C16 C17 1.371(16) . . ? C16 H16 .950(10) . . ? C17 C18 1.424(15) . . ? C17 H17 .950(10) . . ? C19 C20 1.372(19) . . ? C19 C24 1.363(19) . . ? C20 C21 1.41(2) . . ? C20 H20 .950(12) . . ? C21 C22 1.35(2) . . ? C21 H21 .950(16) . . ? C22 C23 1.38(2) . . ? C22 H22 .950(14) . . ? C23 C24 1.40(3) . . ? C23 H23 .950(15) . . ? C24 H24 .950(15) . . ? C25 C26 1.37(2) . . ? C25 C30 1.37(2) . . ? C26 C27 1.40(3) . . ? C26 H26 .950(17) . . ? C27 C28 1.36(3) . . ? C27 H27 .950(15) . . ? C28 C29 1.38(2) . . ? C28 H28 .950(13) . . ? C29 C30 1.40(2) . . ? C29 H29 .950(17) . . ? C30 H30 .950(13) . . ? C31 C32 1.391(15) . . ? C31 C36 1.388(14) . . ? C32 C33 1.397(19) . . ? C32 H32 .950(9) . . ? C33 C34 1.383(17) . . ? C33 H33 .950(13) . . ? C34 C35 1.39(2) . . ? C34 H34 .950(14) . . ? C35 C36 1.39(2) . . ? C35 H35 .950(11) . . ? C36 H36 .950(12) . . ? C37 C38 1.387(18) . . ? C37 C42 1.393(15) . . ? C38 C39 1.40(2) . . ? C38 H38 .950(10) . . ? C39 C40 1.40(2) . . ? C39 H39 .950(16) . . ? C40 C41 1.38(2) . . ? C40 H40 .950(15) . . ? C41 C42 1.407(19) . . ? C41 H41 .950(11) . . ? C42 H42 .950(13) . . ? C43 C44 1.36(2) . . ? C43 C48 1.386(19) . . ? C44 C45 1.40(3) . . ? C44 H44 .950(16) . . ? C45 C46 1.37(3) . . ? C45 H45 .95(2) . . ? C46 C47 1.38(3) . . ? C46 H46 .950(18) . . ? C47 C48 1.38(2) . . ? C47 H47 .950(15) . . ? C48 H48 .950(15) . . ? C49 C50 1.38(3) . . ? C49 C54 1.35(2) . . ? C50 C51 1.39(3) . . ? C50 H50 .95(2) . . ? C51 C52 1.36(3) . . ? C51 H51 .95(2) . . ? C52 C53 1.37(3) . . ? C52 H52 .950(18) . . ? C53 C54 1.40(2) . . ? C53 H53 .95(2) . . ? C54 H54 .950(15) . . ? C55 C56 1.36(4) . . ? C55 C60 1.37(4) . . ? C56 C57 1.41(5) . . ? C56 H56 .95(3) . . ? C57 C58 1.35(5) . . ? C57 H57 .95(4) . . ? C58 C59 1.39(8) . . ? C58 H58 .95(3) . . ? C59 C60 1.38(6) . . ? C59 H59 .95(5) . . ? C60 H60 .95(4) . . ? C61 C62 1.39(3) . . ? C61 C66 1.39(3) . . ? C61 C66' 1.39(3) . . ? C62 C63 1.39(3) . . ? C63 C64 1.39(4) . . ? C63 C64' 1.42(6) . . ? C64 C65 1.39(6) . . ? C64 C65' 1.79(8) . . ? C64 C64' .73(9) . . ? C65 C66 1.41(4) . . ? C65 C66' 1.81(5) . . ? C65 C65' 1.25(7) . . ? C65 C64' 1.64(8) . . ? C66 C66' .87(5) . . ? C66 C65' 1.69(5) . . ? C66' C65' 1.42(4) . . ? C65' C64' 1.46(9) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC PT2 PT1 P1 54.72(8) . . . ? PT2 PT1 P3 162.84(8) . . . ? PT2 PT1 C13 97.4(3) . . . ? P1 PT1 P3 108.36(11) . . . ? P1 PT1 C13 151.7(3) . . . ? P3 PT1 C13 99.7(3) . . . ? PT1 PT2 P1 53.35(9) . . . ? PT1 PT2 P2 83.23(9) . . . ? PT1 PT2 P4 159.72(13) . . . ? P1 PT2 P2 135.27(13) . . . ? P1 PT2 P4 109.68(15) . . . ? P2 PT2 P4 114.97(15) . . . ? PT1 P1 PT2 71.93(10) . . . ? PT1 P1 C1 123.7(4) . . . ? PT1 P1 C7 118.8(5) . . . ? PT2 P1 C1 118.8(5) . . . ? PT2 P1 C7 117.3(4) . . . ? C1 P1 C7 104.4(6) . . . ? PT2 P2 C18 115.6(4) . . . ? PT2 P2 C19 111.3(5) . . . ? PT2 P2 C25 118.5(5) . . . ? C18 P2 C19 103.1(6) . . . ? C18 P2 C25 103.8(6) . . . ? C19 P2 C25 102.5(7) . . . ? PT1 P3 C31 117.7(4) . . . ? PT1 P3 C37 112.0(4) . . . ? PT1 P3 C43 115.2(4) . . . ? C31 P3 C37 106.3(5) . . . ? C31 P3 C43 101.8(5) . . . ? C37 P3 C43 102.2(6) . . . ? PT2 P4 C49 123.3(6) . . . ? PT2 P4 C55 107.5(9) . . . ? PT2 P4 C61 115.9(6) . . . ? C49 P4 C55 102.6(10) . . . ? C49 P4 C61 96.6(8) . . . ? C55 P4 C61 109.5(11) . . . ? P1 C1 C2 118.7(9) . . . ? P1 C1 C6 119.8(9) . . . ? C2 C1 C6 119.9(11) . . . ? C1 C2 C3 120.0(11) . . . ? C1 C2 H2 120.0(14) . . . ? C3 C2 H2 120.0(13) . . . ? C2 C3 C4 120.0(12) . . . ? C2 C3 H3 120.0(13) . . . ? C4 C3 H3 120.0(13) . . . ? C3 C4 C5 119.9(13) . . . ? C3 C4 H4 120.0(14) . . . ? C5 C4 H4 120.0(16) . . . ? C4 C5 C6 120.0(13) . . . ? C4 C5 H5 120.0(18) . . . ? C6 C5 H5 120.0(15) . . . ? C1 C6 C5 120.0(12) . . . ? C1 C6 H6 120.0(13) . . . ? C5 C6 H6 120.0(13) . . . ? P1 C7 C8 121.4(11) . . . ? P1 C7 C12 118.0(11) . . . ? C8 C7 C12 119.9(14) . . . ? C7 C8 C9 120.0(13) . . . ? C7 C8 H8 120.0(18) . . . ? C9 C8 H8 120.0(18) . . . ? C8 C9 C10 120.0(18) . . . ? C8 C9 H9 120.0(18) . . . ? C10 C9 H9 120(2) . . . ? C9 C10 C11 120(2) . . . ? C9 C10 H10 120(2) . . . ? C11 C10 H10 120(2) . . . ? C10 C11 C12 120.0(15) . . . ? C10 C11 H11 120(2) . . . ? C12 C11 H11 120(2) . . . ? C7 C12 C11 120.0(14) . . . ? C7 C12 H12 120.0(16) . . . ? C11 C12 H12 120.0(15) . . . ? PT1 C13 C14 121.1(7) . . . ? PT1 C13 C18 118.4(6) . . . ? C14 C13 C18 120.0(8) . . . ? C13 C14 C15 120.0(9) . . . ? C13 C14 H14 120.0(10) . . . ? C15 C14 H14 120.0(10) . . . ? C14 C15 C16 120.0(9) . . . ? C14 C15 H15 120.0(11) . . . ? C16 C15 H15 120.0(10) . . . ? C15 C16 C17 119.9(9) . . . ? C15 C16 H16 120.0(10) . . . ? C17 C16 H16 120.0(11) . . . ? C16 C17 C18 120.0(10) . . . ? C16 C17 H17 120.0(11) . . . ? C18 C17 H17 120.0(11) . . . ? P2 C18 C13 119.1(7) . . . ? P2 C18 C17 120.9(8) . . . ? C13 C18 C17 119.9(8) . . . ? P2 C19 C20 122.6(11) . . . ? P2 C19 C24 117.1(11) . . . ? C20 C19 C24 120.0(13) . . . ? C19 C20 C21 120.0(12) . . . ? C19 C20 H20 120.0(15) . . . ? C21 C20 H20 120.0(14) . . . ? C20 C21 C22 120.0(14) . . . ? C20 C21 H21 120.0(15) . . . ? C22 C21 H21 120.0(16) . . . ? C21 C22 C23 120.0(14) . . . ? C21 C22 H22 120.0(17) . . . ? C23 C22 H22 120.0(18) . . . ? C22 C23 C24 120.0(14) . . . ? C22 C23 H23 120.0(19) . . . ? C24 C23 H23 120.0(16) . . . ? C19 C24 C23 120.0(13) . . . ? C19 C24 H24 120.0(15) . . . ? C23 C24 H24 120.0(14) . . . ? P2 C25 C26 120.7(12) . . . ? P2 C25 C30 119.2(11) . . . ? C26 C25 C30 119.9(13) . . . ? C25 C26 C27 120.0(15) . . . ? C25 C26 H26 120.0(17) . . . ? C27 C26 H26 120.0(15) . . . ? C26 C27 C28 120.0(14) . . . ? C26 C27 H27 120.0(17) . . . ? C28 C27 H27 120.0(18) . . . ? C27 C28 C29 120.0(14) . . . ? C27 C28 H28 120.0(17) . . . ? C29 C28 H28 120.0(18) . . . ? C28 C29 C30 120.0(15) . . . ? C28 C29 H29 120.0(16) . . . ? C30 C29 H29 120.0(14) . . . ? C25 C30 C29 119.9(12) . . . ? C25 C30 H30 120.0(15) . . . ? C29 C30 H30 120.0(15) . . . ? P3 C31 C32 117.6(8) . . . ? P3 C31 C36 122.4(9) . . . ? C32 C31 C36 120.0(10) . . . ? C31 C32 C33 120.0(9) . . . ? C31 C32 H32 120.0(12) . . . ? C33 C32 H32 120.0(11) . . . ? C32 C33 C34 120.0(12) . . . ? C32 C33 H33 120.0(11) . . . ? C34 C33 H33 120.0(14) . . . ? C33 C34 C35 120.0(13) . . . ? C33 C34 H34 120.0(14) . . . ? C35 C34 H34 120.0(13) . . . ? C34 C35 C36 120.0(10) . . . ? C34 C35 H35 120.0(15) . . . ? C36 C35 H35 120.0(13) . . . ? C31 C36 C35 120.0(10) . . . ? C31 C36 H36 120.0(12) . . . ? C35 C36 H36 120.0(10) . . . ? P3 C37 C38 123.9(8) . . . ? P3 C37 C42 116.1(9) . . . ? C38 C37 C42 120.0(10) . . . ? C37 C38 C39 120.0(10) . . . ? C37 C38 H38 120.0(12) . . . ? C39 C38 H38 120.0(14) . . . ? C38 C39 C40 120.0(14) . . . ? C38 C39 H39 120.0(14) . . . ? C40 C39 H39 120.0(15) . . . ? C39 C40 C41 120.0(13) . . . ? C39 C40 H40 120.0(15) . . . ? C41 C40 H40 120.0(12) . . . ? C40 C41 C42 120.0(11) . . . ? C40 C41 H41 120.0(14) . . . ? C42 C41 H41 120.0(15) . . . ? C37 C42 C41 120.0(11) . . . ? C37 C42 H42 120.0(12) . . . ? C41 C42 H42 120.0(12) . . . ? P3 C43 C44 121.3(10) . . . ? P3 C43 C48 118.7(10) . . . ? C44 C43 C48 120.0(12) . . . ? C43 C44 C45 120.0(15) . . . ? C43 C44 H44 120.0(17) . . . ? C45 C44 H44 120.0(18) . . . ? C44 C45 C46 120.0(18) . . . ? C44 C45 H45 120.0(19) . . . ? C46 C45 H45 120(2) . . . ? C45 C46 C47 120.0(17) . . . ? C45 C46 H46 120(2) . . . ? C47 C46 H46 120.0(19) . . . ? C46 C47 C48 120.0(14) . . . ? C46 C47 H47 120.0(16) . . . ? C48 C47 H47 120.0(16) . . . ? C43 C48 C47 120.0(13) . . . ? C43 C48 H48 120.0(14) . . . ? C47 C48 H48 120.0(14) . . . ? P4 C49 C50 117.3(12) . . . ? P4 C49 C54 122.7(12) . . . ? C50 C49 C54 119.9(13) . . . ? C49 C50 C51 120.0(18) . . . ? C49 C50 H50 120.0(17) . . . ? C51 C50 H50 120(2) . . . ? C50 C51 C52 120.0(19) . . . ? C50 C51 H51 120(3) . . . ? C52 C51 H51 120(2) . . . ? C51 C52 C53 120.0(17) . . . ? C51 C52 H52 120(2) . . . ? C53 C52 H52 120(2) . . . ? C52 C53 C54 120.0(18) . . . ? C52 C53 H53 120.0(18) . . . ? C54 C53 H53 120(2) . . . ? C49 C54 C53 120.0(15) . . . ? C49 C54 H54 120.0(16) . . . ? C53 C54 H54 120.0(19) . . . ? P4 C55 C56 124(2) . . . ? P4 C55 C60 116(2) . . . ? C56 C55 C60 120(3) . . . ? C55 C56 C57 120(3) . . . ? C55 C56 H56 120(3) . . . ? C57 C56 H56 120(3) . . . ? C56 C57 C58 120(3) . . . ? C56 C57 H57 120(3) . . . ? C58 C57 H57 120(4) . . . ? C57 C58 C59 120(3) . . . ? C57 C58 H58 120(4) . . . ? C59 C58 H58 120(3) . . . ? C58 C59 C60 120(4) . . . ? C58 C59 H59 120(4) . . . ? C60 C59 H59 120(6) . . . ? C55 C60 C59 120(4) . . . ? C55 C60 H60 120(4) . . . ? C59 C60 H60 120(4) . . . ? P4 C61 C62 119.8(13) . . . ? P4 C61 C66 119.6(17) . . . ? P4 C61 C66' 113.8(17) . . . ? C62 C61 C66 120(2) . . . ? C62 C61 C66' 119.0(18) . . . ? C66 C61 C66' 37(2) . . . ? C61 C62 C63 119.8(16) . . . ? C62 C63 C64 120(2) . . . ? C62 C63 C64' 118(3) . . . ? C64 C63 C64' 30(4) . . . ? C63 C64 C65 120(2) . . . ? C63 C64 C65' 101(3) . . . ? C63 C64 C64' 77(5) . . . ? C65 C64 C65' 44(3) . . . ? C65 C64 C64' 96(9) . . . ? C65' C64 C64' 52(7) . . . ? C64 C65 C66 120(3) . . . ? C64 C65 C66' 110(3) . . . ? C64 C65 C65' 85(4) . . . ? C64 C65 C64' 26(4) . . . ? C66 C65 C66' 28(2) . . . ? C66 C65 C65' 79(3) . . . ? C66 C65 C64' 111(2) . . . ? C66' C65 C65' 51(2) . . . ? C66' C65 C64' 92(3) . . . ? C65' C65 C64' 59(3) . . . ? C61 C66 C65 120(3) . . . ? C61 C66 C66' 72(3) . . . ? C61 C66 C65' 103(2) . . . ? C65 C66 C66' 103(4) . . . ? C65 C66 C65' 46(3) . . . ? C66' C66 C65' 57(3) . . . ? C61 C66' C65 97(2) . . . ? C61 C66' C66 72(3) . . . ? C61 C66' C65' 119(3) . . . ? C65 C66' C66 49(3) . . . ? C65 C66' C65' 43(2) . . . ? C66 C66' C65' 92(3) . . . ? C64 C65' C65 51(3) . . . ? C64 C65' C66 88(3) . . . ? C64 C65' C66' 110(3) . . . ? C64 C65' C64' 23(3) . . . ? C65 C65' C66 55(2) . . . ? C65 C65' C66' 85(3) . . . ? C65 C65' C64' 74(4) . . . ? C66 C65' C66' 31.0(19) . . . ? C66 C65' C64' 106(4) . . . ? C66' C65' C64' 119(3) . . . ? C63 C64' C64 73(6) . . . ? C63 C64' C65 104(4) . . . ? C63 C64' C65' 119(3) . . . ? C64 C64' C65 57(7) . . . ? C64 C64' C65' 104(8) . . . ? C65 C64' C65' 47(3) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_total 8796 #ActaC _reflns_number_observed 6022 #ActaC _reflns_observed_criterion 'refl observed if Inet > 3\s(Inet)' _reflns_d_resolution_high .89 _reflns_d_resolution_low 14.208 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 1.7431 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code ? ? ? ? ? ? ? ? _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; ? name ? institute ? department ? address ? city ? country ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone ? #ActaC _publ_contact_author_fax ? #ActaC _publ_contact_author_email ? #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; Altomare, A., Cascarano, M., Giacovazzo, C., and Guagliardi, A. J. Appl. Crystallogr. 1993, 26, 343 Beurskens, P. T., Admiraal, G., Beurskens, G., Bosman, W. P., de Gelder, R., Israel, R., and Smits, J. M. M. The DIRDIF-94 Program System, Technical Report of the Crystallographic Laboratory, University of Nijmegen, Nijmegen, The Netherlands, 1994. Hall, S. R.; Stewart, J. M. (1990). Editors. Xtal3.4 Reference Manual. Univs. of Western Australia, Australia, and Maryland, USA. Molecular Structure Corporation (1992). MSC/AFC Diffractometer Control Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ?