Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Professor Dr Evamarie Hey-Hawkins' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Leipzig Johannisallee 29 Leipzig 04103 GERMANY ; _publ_contact_author_phone '49 / 341 / 9736121' _publ_contact_author_fax '49 / 341 / 9736199' _publ_contact_author_email hey@rz.uni-leipzig.de _publ_section_title ; Unexpected formation of a novel macrocyclic tetraphosphine - RSSR isomer of 1,9-di-benzyl-3,7,11,15-tetramesityl-1,9-diaza- 3,7,11,15-tetraphosphacyclo-hexadecane. ; loop_ _publ_author_name _publ_author_address ; Naumov, Roman N. ; ; A.E. Arbuzov Institute of Organic and Physical Chemistry Russian Academy of Sciences Kazan Scientific Center Arbuzov str. 8 Kazan Russian Federation, 420088. ; ; Karasik, Andrey A. ; ; A.E. Arbuzov Institute of Organic and Physical Chemistry Russian Academy of Sciences Kazan Scientific Center Arbuzov str. 8 Kazan Russian Federation, 420088. ; ; Sinyashin, Oleg G. ; ; A.E. Arbuzov Institute of Organic and Physical Chemistry Russian Academy of Sciences Kazan Scientific Center Arbuzov str. 8 Kazan Russian Federation, 420088. ; ; Lonnecke, Peter ; ; Institut fur Anorganische Chemie Universitat Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; ; Hey-Hawkins, Evamarie ; ; Institut fur Anorganische Chemie Universitat Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# data_c1628fin _database_code_depnum_ccdc_archive 'CCDC 222159' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H84 N2 P4' _chemical_formula_weight 1029.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9312(14) _cell_length_b 12.909(2) _cell_length_c 14.848(2) _cell_angle_alpha 66.741(3) _cell_angle_beta 80.065(3) _cell_angle_gamma 74.491(3) _cell_volume 1511.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 1554 _cell_measurement_theta_min 2.584 _cell_measurement_theta_max 27.424 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 554 _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15597 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.1428 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7101 _reflns_number_gt 3444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXS-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^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 7101 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1494 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.61619(9) 0.03659(7) 1.12146(6) 0.0331(2) Uani 1 1 d . . . P2 P 0.60501(9) 0.26342(7) 0.71210(6) 0.0348(2) Uani 1 1 d . . . N1 N 0.6693(3) -0.19340(19) 1.23081(17) 0.0333(6) Uani 1 1 d . . . C1 C 0.7427(4) -0.0954(3) 1.2038(2) 0.0358(8) Uani 1 1 d . . . C2 C 0.7200(4) 0.0501(3) 1.0008(2) 0.0381(8) Uani 1 1 d . . . C3 C 0.6336(4) 0.1480(3) 0.9162(2) 0.0361(8) Uani 1 1 d . . . C4 C 0.7121(4) 0.1501(3) 0.8159(2) 0.0377(8) Uani 1 1 d . . . C5 C 0.4675(4) 0.1863(3) 0.6988(2) 0.0377(8) Uani 1 1 d . . . C6 C 0.6460(3) 0.1567(2) 1.1492(2) 0.0315(7) Uani 1 1 d . . . C7 C 0.7885(3) 0.1709(3) 1.1653(2) 0.0410(8) Uani 1 1 d . . . C8 C 0.7915(4) 0.2586(3) 1.1967(3) 0.0494(9) Uani 1 1 d . . . H8 H 0.8878 0.2658 1.2083 0.059 Uiso 1 1 calc R . . C9 C 0.6565(4) 0.3357(3) 1.2114(3) 0.0502(9) Uani 1 1 d . . . C10 C 0.5186(4) 0.3246(3) 1.1911(2) 0.0481(9) Uani 1 1 d . . . H10 H 0.4269 0.3781 1.1982 0.058 Uiso 1 1 calc R . . C11 C 0.5082(3) 0.2377(2) 1.1607(2) 0.0374(8) Uani 1 1 d . . . C12 C 0.9452(3) 0.0951(3) 1.1493(3) 0.0669(12) Uani 1 1 d . . . H12A H 0.9472 0.0802 1.0899 0.100 Uiso 1 1 calc R . . H12B H 0.9609 0.0225 1.2050 0.100 Uiso 1 1 calc R . . H12C H 1.0275 0.1343 1.1426 0.100 Uiso 1 1 calc R . . C13 C 0.6614(5) 0.4264(3) 1.2514(3) 0.0850(14) Uani 1 1 d . . . H13A H 0.5752 0.4921 1.2287 0.127 Uiso 1 1 calc R . . H13B H 0.7590 0.4513 1.2282 0.127 Uiso 1 1 calc R . . H13C H 0.6532 0.3935 1.3227 0.127 Uiso 1 1 calc R . . C14 C 0.3508(3) 0.2334(3) 1.1417(3) 0.0583(10) Uani 1 1 d . . . H14A H 0.2769 0.3044 1.1401 0.087 Uiso 1 1 calc R . . H14B H 0.3165 0.1682 1.1938 0.087 Uiso 1 1 calc R . . H14C H 0.3572 0.2247 1.0791 0.087 Uiso 1 1 calc R . . C15 C 0.7460(3) 0.2725(2) 0.6038(2) 0.0329(7) Uani 1 1 d . . . C16 C 0.7767(3) 0.3831(2) 0.5459(2) 0.0339(7) Uani 1 1 d . . . C17 C 0.8859(3) 0.3969(3) 0.4673(2) 0.0420(8) Uani 1 1 d . . . H17 H 0.9058 0.4709 0.4314 0.050 Uiso 1 1 calc R . . C18 C 0.9690(4) 0.3047(3) 0.4385(2) 0.0449(8) Uani 1 1 d . . . C19 C 0.9355(4) 0.1984(3) 0.4933(2) 0.0464(9) Uani 1 1 d . . . H19 H 0.9884 0.1356 0.4748 0.056 Uiso 1 1 calc R . . C20 C 0.8285(3) 0.1787(2) 0.5739(2) 0.0390(8) Uani 1 1 d . . . C21 C 0.6895(4) 0.4912(2) 0.5665(2) 0.0439(8) Uani 1 1 d . . . H21A H 0.7319 0.5568 0.5217 0.066 Uiso 1 1 calc R . . H21B H 0.7014 0.4799 0.6337 0.066 Uiso 1 1 calc R . . H21C H 0.5799 0.5059 0.5572 0.066 Uiso 1 1 calc R . . C22 C 1.0863(4) 0.3229(3) 0.3504(3) 0.0660(11) Uani 1 1 d . . . H22A H 1.1246 0.2514 0.3385 0.099 Uiso 1 1 calc R . . H22B H 1.1727 0.3463 0.3631 0.099 Uiso 1 1 calc R . . H22C H 1.0370 0.3827 0.2932 0.099 Uiso 1 1 calc R . . C23 C 0.8030(4) 0.0566(3) 0.6249(2) 0.0516(9) Uani 1 1 d . . . H23A H 0.7101 0.0514 0.6030 0.077 Uiso 1 1 calc R . . H23B H 0.7903 0.0374 0.6955 0.077 Uiso 1 1 calc R . . H23C H 0.8923 0.0030 0.6090 0.077 Uiso 1 1 calc R . . C24 C 0.7805(4) -0.3040(3) 1.2726(2) 0.0392(8) Uani 1 1 d . . . C25 C 0.9048(3) -0.3321(2) 1.1978(2) 0.0370(7) Uani 1 1 d . . . C26 C 1.0605(3) -0.3602(3) 1.2150(3) 0.0471(9) Uani 1 1 d . . . H26 H 1.0888 -0.3575 1.2720 0.057 Uiso 1 1 calc R . . C27 C 1.1751(4) -0.3924(3) 1.1497(3) 0.0575(10) Uani 1 1 d . . . H27 H 1.2803 -0.4116 1.1628 0.069 Uiso 1 1 calc R . . C28 C 1.1369(4) -0.3966(3) 1.0667(3) 0.0694(12) Uani 1 1 d . . . H28 H 1.2152 -0.4189 1.0226 0.083 Uiso 1 1 calc R . . C29 C 0.9805(4) -0.3677(3) 1.0474(3) 0.0713(12) Uani 1 1 d . . . H29 H 0.9531 -0.3703 0.9902 0.086 Uiso 1 1 calc R . . C30 C 0.8658(4) -0.3350(3) 1.1127(3) 0.0570(10) Uani 1 1 d . . . H30 H 0.7606 -0.3146 1.0991 0.068 Uiso 1 1 calc R . . C31 C 0.6086(7) 0.0416(7) 0.4263(4) 0.0981(17) Uani 1 1 d . . . H31 H 0.6829 0.0708 0.3757 0.118 Uiso 1 1 calc R . . C32 C 0.4792(8) 0.1157(5) 0.4496(4) 0.0957(15) Uani 1 1 d . . . H32 H 0.4650 0.1957 0.4145 0.115 Uiso 1 1 calc R . . C33 C 0.3724(6) 0.0739(6) 0.5226(4) 0.0894(15) Uani 1 1 d . . . H33 H 0.2848 0.1252 0.5381 0.107 Uiso 1 1 calc R . . H1A H 0.849(3) -0.109(2) 1.167(2) 0.043(8) Uiso 1 1 d . . . H1B H 0.759(3) -0.086(2) 1.264(2) 0.036(8) Uiso 1 1 d . . . H2A H 0.829(3) 0.062(2) 0.9929(18) 0.031(7) Uiso 1 1 d . . . H2B H 0.716(3) -0.021(3) 0.996(2) 0.046(9) Uiso 1 1 d . . . H3A H 0.619(3) 0.225(2) 0.9241(19) 0.040(8) Uiso 1 1 d . . . H3B H 0.526(3) 0.135(2) 0.929(2) 0.041(9) Uiso 1 1 d . . . H4A H 0.813(3) 0.169(2) 0.8106(19) 0.035(8) Uiso 1 1 d . . . H4B H 0.719(3) 0.076(3) 0.814(2) 0.043(8) Uiso 1 1 d . . . H5A H 0.516(3) 0.106(3) 0.716(2) 0.054(9) Uiso 1 1 d . . . H5B H 0.439(3) 0.222(3) 0.626(2) 0.054(9) Uiso 1 1 d . . . H24A H 0.718(3) -0.366(3) 1.306(2) 0.040(8) Uiso 1 1 d . . . H24B H 0.827(4) -0.304(3) 1.332(2) 0.062(10) 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 0.0353(4) 0.0274(4) 0.0361(5) -0.0150(4) -0.0048(4) 0.0005(3) P2 0.0415(5) 0.0284(4) 0.0346(5) -0.0164(4) 0.0002(4) -0.0022(4) N1 0.0361(13) 0.0231(13) 0.0369(16) -0.0105(12) -0.0024(12) -0.0013(11) C1 0.0383(18) 0.0302(17) 0.039(2) -0.0160(16) -0.0056(16) -0.0007(14) C2 0.0397(19) 0.0347(19) 0.040(2) -0.0178(16) -0.0041(16) -0.0018(15) C3 0.043(2) 0.0308(17) 0.0355(19) -0.0163(15) -0.0034(16) -0.0028(15) C4 0.0420(19) 0.0325(18) 0.042(2) -0.0207(16) -0.0024(16) -0.0023(15) C5 0.0461(19) 0.0296(18) 0.035(2) -0.0129(16) 0.0005(16) -0.0049(15) C6 0.0354(16) 0.0250(15) 0.0315(18) -0.0125(14) -0.0005(14) -0.0006(13) C7 0.0388(17) 0.0338(17) 0.052(2) -0.0232(16) -0.0017(15) 0.0000(14) C8 0.0443(19) 0.043(2) 0.070(3) -0.0317(19) -0.0020(18) -0.0080(16) C9 0.056(2) 0.0379(19) 0.064(3) -0.0326(19) 0.0038(18) -0.0071(16) C10 0.048(2) 0.0373(19) 0.057(2) -0.0278(18) 0.0001(17) 0.0070(15) C11 0.0357(16) 0.0328(17) 0.0390(19) -0.0157(15) -0.0024(14) 0.0034(13) C12 0.0338(18) 0.064(2) 0.122(4) -0.061(3) -0.012(2) 0.0035(17) C13 0.082(3) 0.072(3) 0.134(4) -0.080(3) 0.000(3) -0.010(2) C14 0.0363(18) 0.060(2) 0.082(3) -0.042(2) -0.0065(18) 0.0111(16) C15 0.0396(16) 0.0274(16) 0.0320(18) -0.0129(14) -0.0038(14) -0.0040(13) C16 0.0409(17) 0.0292(17) 0.0304(18) -0.0120(15) -0.0012(15) -0.0048(13) C17 0.0472(19) 0.0370(19) 0.038(2) -0.0116(16) 0.0029(17) -0.0105(15) C18 0.0495(19) 0.044(2) 0.039(2) -0.0174(18) 0.0083(17) -0.0113(16) C19 0.058(2) 0.038(2) 0.041(2) -0.0235(18) 0.0102(18) -0.0023(16) C20 0.0497(19) 0.0303(17) 0.039(2) -0.0200(16) 0.0020(16) -0.0047(14) C21 0.056(2) 0.0242(16) 0.046(2) -0.0115(16) -0.0008(17) -0.0036(15) C22 0.068(2) 0.061(3) 0.062(3) -0.026(2) 0.021(2) -0.014(2) C23 0.068(2) 0.0358(19) 0.053(2) -0.0277(18) 0.0116(19) -0.0074(17) C24 0.0451(19) 0.0268(17) 0.038(2) -0.0064(16) -0.0064(17) -0.0016(15) C25 0.0377(17) 0.0243(16) 0.046(2) -0.0130(15) -0.0039(15) -0.0007(13) C26 0.0439(19) 0.0338(19) 0.061(2) -0.0156(18) -0.0111(18) -0.0021(15) C27 0.0375(19) 0.041(2) 0.081(3) -0.015(2) -0.004(2) 0.0004(16) C28 0.058(2) 0.054(2) 0.084(3) -0.032(2) 0.013(2) 0.007(2) C29 0.075(3) 0.078(3) 0.064(3) -0.043(2) -0.002(2) 0.004(2) C30 0.046(2) 0.067(2) 0.064(3) -0.038(2) -0.0089(19) 0.0040(18) C31 0.105(4) 0.148(6) 0.052(3) -0.038(4) 0.003(3) -0.048(4) C32 0.136(5) 0.092(4) 0.062(4) -0.019(3) -0.015(3) -0.039(4) C33 0.098(4) 0.117(5) 0.061(4) -0.046(3) -0.013(3) -0.012(4) _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 C2 1.835(3) . ? P1 C6 1.846(3) . ? P1 C1 1.865(3) . ? P2 C4 1.847(3) . ? P2 C15 1.848(3) . ? P2 C5 1.852(3) . ? N1 C1 1.465(4) . ? N1 C24 1.471(3) . ? N1 C5 1.472(4) 2_657 ? C2 C3 1.526(4) . ? C3 C4 1.526(4) . ? C5 N1 1.472(4) 2_657 ? C6 C7 1.406(4) . ? C6 C11 1.420(3) . ? C7 C8 1.391(4) . ? C7 C12 1.520(4) . ? C8 C9 1.391(4) . ? C9 C10 1.373(4) . ? C9 C13 1.519(4) . ? C10 C11 1.394(4) . ? C11 C14 1.500(4) . ? C15 C16 1.418(4) . ? C15 C20 1.428(4) . ? C16 C17 1.371(4) . ? C16 C21 1.525(4) . ? C17 C18 1.404(4) . ? C18 C19 1.374(4) . ? C18 C22 1.510(4) . ? C19 C20 1.381(4) . ? C20 C23 1.516(4) . ? C24 C25 1.509(4) . ? C25 C26 1.382(4) . ? C25 C30 1.384(4) . ? C26 C27 1.382(4) . ? C27 C28 1.358(5) . ? C28 C29 1.395(5) . ? C29 C30 1.384(4) . ? C31 C33 1.358(7) 2_656 ? C31 C32 1.379(7) . ? C32 C33 1.354(7) . ? C33 C31 1.358(7) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 C6 105.60(15) . . ? C2 P1 C1 101.37(14) . . ? C6 P1 C1 104.82(13) . . ? C4 P2 C15 104.23(14) . . ? C4 P2 C5 100.91(16) . . ? C15 P2 C5 103.50(13) . . ? C1 N1 C24 111.2(2) . . ? C1 N1 C5 111.5(2) . 2_657 ? C24 N1 C5 109.5(2) . 2_657 ? N1 C1 P1 108.79(19) . . ? C3 C2 P1 112.9(2) . . ? C4 C3 C2 112.3(2) . . ? C3 C4 P2 113.3(2) . . ? N1 C5 P2 109.28(19) 2_657 . ? C7 C6 C11 118.1(2) . . ? C7 C6 P1 126.4(2) . . ? C11 C6 P1 115.4(2) . . ? C8 C7 C6 120.2(3) . . ? C8 C7 C12 116.4(3) . . ? C6 C7 C12 123.4(3) . . ? C9 C8 C7 121.9(3) . . ? C10 C9 C8 117.4(3) . . ? C10 C9 C13 121.5(3) . . ? C8 C9 C13 121.0(3) . . ? C9 C10 C11 123.1(3) . . ? C10 C11 C6 119.1(3) . . ? C10 C11 C14 118.3(3) . . ? C6 C11 C14 122.6(3) . . ? C16 C15 C20 117.0(3) . . ? C16 C15 P2 116.6(2) . . ? C20 C15 P2 126.3(2) . . ? C17 C16 C15 120.7(3) . . ? C17 C16 C21 117.1(3) . . ? C15 C16 C21 122.1(3) . . ? C16 C17 C18 122.4(3) . . ? C19 C18 C17 116.6(3) . . ? C19 C18 C22 122.1(3) . . ? C17 C18 C22 121.3(3) . . ? C18 C19 C20 123.7(3) . . ? C19 C20 C15 119.5(3) . . ? C19 C20 C23 117.0(3) . . ? C15 C20 C23 123.5(3) . . ? N1 C24 C25 113.3(3) . . ? C26 C25 C30 118.6(3) . . ? C26 C25 C24 120.3(3) . . ? C30 C25 C24 121.0(3) . . ? C27 C26 C25 120.9(3) . . ? C28 C27 C26 120.5(3) . . ? C27 C28 C29 119.5(3) . . ? C30 C29 C28 119.9(4) . . ? C25 C30 C29 120.5(3) . . ? C33 C31 C32 119.2(5) 2_656 . ? C33 C32 C31 120.5(5) . . ? C32 C33 C31 120.3(5) . 2_656 ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.389 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.056 #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#