Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Stephen Liddle' 'Polly Arnold' _publ_contact_author_name 'Stephen Liddle' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham Nottinghamshire NG7 2RD UNITED KINGDOM ; _publ_contact_author_email STEPHEN.LIDDLE@NOTTINGHAM.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and characterisation of yttrium complexes supported by the ?-diketiminate ligand {ArNC(CH3)CHC(CH3)NAr}- (Ar = 2,6-Pri2C6H3) ; data_2 _database_code_depnum_ccdc_archive 'CCDC 646371' _refine_special_details ; Highly disordered lattice solvent molecules (67 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 375.60 \%A**3, equating to half a molecule of toluene per monomer, molecule in the unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. One beta-carbon atom of the coordinated THF molecule is positionally disordered over two sites. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36.50 H53 I2 N2 O Y' _chemical_formula_sum 'C36.50 H53 I2 N2 O Y' _chemical_formula_weight 878.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9606(8) _cell_length_b 12.3187(7) _cell_length_c 21.1877(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.287(2) _cell_angle_gamma 90.00 _cell_volume 3815.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9924 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.59 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 3.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2052 _exptl_absorpt_correction_T_max 0.2560 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26393 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8706 _reflns_number_gt 7219 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0318P)^2^+3.3389P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8706 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Y1 Y 1.229077(17) 0.45529(2) 0.878251(12) 0.01352(6) Uani 1 1 d . . . I1 I 1.267571(13) 0.402397(16) 1.016156(9) 0.02402(6) Uani 1 1 d . A . I2 I 1.109852(15) 0.35402(2) 0.764913(12) 0.04591(8) Uani 1 1 d . A . N1 N 1.35714(15) 0.38586(17) 0.84921(11) 0.0147(5) Uani 1 1 d . A . N2 N 1.30510(15) 0.61379(17) 0.87917(10) 0.0123(4) Uani 1 1 d . A . C1 C 1.5233(2) 0.3540(3) 0.88478(17) 0.0297(7) Uani 1 1 d . A . H1A H 1.5209 0.2941 0.9148 0.045 Uiso 1 1 calc R . . H1B H 1.5780 0.3979 0.9008 0.045 Uiso 1 1 calc R . . H1C H 1.5256 0.3245 0.8422 0.045 Uiso 1 1 calc R . . C2 C 1.43906(19) 0.4238(2) 0.87934(13) 0.0179(6) Uani 1 1 d . . . C3 C 1.45408(19) 0.5283(2) 0.90595(13) 0.0182(6) Uani 1 1 d . A . H3 H 1.5132 0.5395 0.9323 0.022 Uiso 1 1 calc R . . C4 C 1.39588(19) 0.6189(2) 0.89988(13) 0.0155(5) Uani 1 1 d . . . C5 C 1.4422(2) 0.7270(2) 0.91694(15) 0.0256(7) Uani 1 1 d . A . H5A H 1.4175 0.7803 0.8834 0.038 Uiso 1 1 calc R . . H5B H 1.5082 0.7192 0.9200 0.038 Uiso 1 1 calc R . . H5C H 1.4310 0.7519 0.9585 0.038 Uiso 1 1 calc R . . C6 C 1.35434(19) 0.2875(2) 0.81110(14) 0.0202(6) Uani 1 1 d . . . C7 C 1.3535(2) 0.2981(3) 0.74446(15) 0.0268(7) Uani 1 1 d . A . C8 C 1.3445(3) 0.2034(3) 0.70725(17) 0.0420(9) Uani 1 1 d . . . H8 H 1.3442 0.2083 0.6625 0.050 Uiso 1 1 calc R A . C9 C 1.3362(3) 0.1034(3) 0.7341(2) 0.0493(11) Uani 1 1 d . A . H9 H 1.3293 0.0404 0.7077 0.059 Uiso 1 1 calc R . . C10 C 1.3379(3) 0.0938(3) 0.79901(19) 0.0405(9) Uani 1 1 d . . . H10 H 1.3319 0.0242 0.8169 0.049 Uiso 1 1 calc R A . C11 C 1.3482(2) 0.1855(2) 0.83905(15) 0.0268(7) Uani 1 1 d . A . C12 C 1.3597(2) 0.4077(3) 0.71305(15) 0.0331(8) Uani 1 1 d . . . H12 H 1.3364 0.4629 0.7402 0.040 Uiso 1 1 calc R A . C13 C 1.4573(3) 0.4383(4) 0.7122(3) 0.0642(13) Uani 1 1 d . A . H13A H 1.4842 0.3828 0.6888 0.096 Uiso 1 1 calc R . . H13B H 1.4929 0.4434 0.7567 0.096 Uiso 1 1 calc R . . H13C H 1.4581 0.5086 0.6907 0.096 Uiso 1 1 calc R . . C14 C 1.2999(4) 0.4148(4) 0.6458(2) 0.0693(15) Uani 1 1 d . A . H14A H 1.2980 0.4901 0.6306 0.104 Uiso 1 1 calc R . . H14B H 1.2378 0.3908 0.6468 0.104 Uiso 1 1 calc R . . H14C H 1.3251 0.3683 0.6164 0.104 Uiso 1 1 calc R . . C15 C 1.3492(2) 0.1708(2) 0.91057(16) 0.0300(7) Uani 1 1 d . . . H15 H 1.3667 0.2420 0.9325 0.036 Uiso 1 1 calc R A . C16 C 1.2542(3) 0.1414(3) 0.9206(2) 0.0493(10) Uani 1 1 d . A . H16A H 1.2102 0.1965 0.9003 0.074 Uiso 1 1 calc R . . H16B H 1.2552 0.1382 0.9669 0.074 Uiso 1 1 calc R . . H16C H 1.2363 0.0704 0.9010 0.074 Uiso 1 1 calc R . . C17 C 1.4189(3) 0.0866(3) 0.9423(2) 0.0506(11) Uani 1 1 d . A . H17A H 1.4224 0.0863 0.9890 0.076 Uiso 1 1 calc R . . H17B H 1.4790 0.1046 0.9338 0.076 Uiso 1 1 calc R . . H17C H 1.4001 0.0147 0.9246 0.076 Uiso 1 1 calc R . . C18 C 1.25172(17) 0.7121(2) 0.86697(12) 0.0132(5) Uani 1 1 d . . . C19 C 1.2202(2) 0.7436(2) 0.80209(13) 0.0188(6) Uani 1 1 d . A . C20 C 1.1638(2) 0.8342(2) 0.78920(14) 0.0260(7) Uani 1 1 d . . . H20 H 1.1425 0.8567 0.7457 0.031 Uiso 1 1 calc R A . C21 C 1.1382(2) 0.8917(2) 0.83812(16) 0.0281(7) Uani 1 1 d . A . H21 H 1.1001 0.9538 0.8283 0.034 Uiso 1 1 calc R . . C22 C 1.1679(2) 0.8593(2) 0.90113(14) 0.0224(6) Uani 1 1 d . . . H22 H 1.1489 0.8987 0.9345 0.027 Uiso 1 1 calc R A . C23 C 1.22524(18) 0.7699(2) 0.91706(13) 0.0158(5) Uani 1 1 d . A . C24 C 1.2472(2) 0.6818(3) 0.74695(13) 0.0258(7) Uani 1 1 d . . . H24 H 1.2609 0.6056 0.7622 0.031 Uiso 1 1 calc R A . C25 C 1.3333(3) 0.7268(4) 0.7309(2) 0.0588(12) Uani 1 1 d . A . H25A H 1.3229 0.8020 0.7162 0.088 Uiso 1 1 calc R . . H25B H 1.3503 0.6830 0.6967 0.088 Uiso 1 1 calc R . . H25C H 1.3829 0.7246 0.7695 0.088 Uiso 1 1 calc R . . C26 C 1.1709(3) 0.6760(4) 0.68651(16) 0.0471(10) Uani 1 1 d . A . H26A H 1.1146 0.6503 0.6982 0.071 Uiso 1 1 calc R . . H26B H 1.1885 0.6258 0.6554 0.071 Uiso 1 1 calc R . . H26C H 1.1606 0.7484 0.6671 0.071 Uiso 1 1 calc R . . C27 C 1.2553(2) 0.7399(2) 0.98822(13) 0.0198(6) Uani 1 1 d . . . H27 H 1.3001 0.6788 0.9921 0.024 Uiso 1 1 calc R A . C28 C 1.3022(2) 0.8357(2) 1.02812(15) 0.0296(7) Uani 1 1 d . A . H28A H 1.3532 0.8614 1.0097 0.044 Uiso 1 1 calc R . . H28B H 1.3254 0.8124 1.0728 0.044 Uiso 1 1 calc R . . H28C H 1.2580 0.8947 1.0273 0.044 Uiso 1 1 calc R . . C29 C 1.1736(2) 0.7020(3) 1.01577(15) 0.0311(7) Uani 1 1 d . A . H29A H 1.1299 0.7618 1.0138 0.047 Uiso 1 1 calc R . . H29B H 1.1951 0.6794 1.0608 0.047 Uiso 1 1 calc R . . H29C H 1.1436 0.6406 0.9903 0.047 Uiso 1 1 calc R . . O1 O 1.08646(13) 0.53186(15) 0.88531(9) 0.0194(4) Uani 0.40 1 d P A 1 C30 C 1.0236(2) 0.4635(3) 0.91216(16) 0.0314(7) Uani 0.40 1 d P A 1 H30A H 1.0396 0.4651 0.9600 0.038 Uiso 0.40 1 calc PR A 1 H30B H 1.0264 0.3874 0.8976 0.038 Uiso 0.40 1 calc PR A 1 C31 C 0.9303(2) 0.5096(4) 0.88783(19) 0.0472(10) Uani 0.40 1 d P A 1 H31A H 0.8973 0.4671 0.8504 0.057 Uiso 0.40 1 calc PR A 1 H31B H 0.8946 0.5073 0.9222 0.057 Uiso 0.40 1 calc PR A 1 C32 C 0.9416(5) 0.6178(7) 0.8693(5) 0.0267(17) Uani 0.40 1 d P A 1 H32A H 0.9490 0.6675 0.9068 0.032 Uiso 0.40 1 calc PR A 1 H32B H 0.8890 0.6420 0.8356 0.032 Uiso 0.40 1 calc PR A 1 C33 C 1.0325(2) 0.6121(2) 0.84195(16) 0.0281(7) Uani 0.40 1 d P A 1 H33A H 1.0198 0.5872 0.7965 0.034 Uiso 0.40 1 calc PR A 1 H33B H 1.0638 0.6833 0.8451 0.034 Uiso 0.40 1 calc PR A 1 O1A O 1.08646(13) 0.53186(15) 0.88531(9) 0.0194(4) Uani 0.60 1 d P A 2 C30A C 1.0236(2) 0.4635(3) 0.91216(16) 0.0314(7) Uani 0.60 1 d P A 2 H30C H 1.0396 0.4651 0.9600 0.038 Uiso 0.60 1 calc PR A 2 H30D H 1.0264 0.3874 0.8976 0.038 Uiso 0.60 1 calc PR A 2 C31A C 0.9303(2) 0.5096(4) 0.88783(19) 0.0472(10) Uani 0.60 1 d P A 2 H31C H 0.9116 0.5546 0.9215 0.057 Uiso 0.60 1 calc PR A 2 H31D H 0.8850 0.4507 0.8753 0.057 Uiso 0.60 1 calc PR A 2 C32A C 0.9372(4) 0.5774(5) 0.8304(3) 0.0335(13) Uani 0.60 1 d P A 2 H32C H 0.9209 0.5342 0.7901 0.040 Uiso 0.60 1 calc PR A 2 H32D H 0.8958 0.6409 0.8267 0.040 Uiso 0.60 1 calc PR A 2 C33A C 1.0325(2) 0.6121(2) 0.84195(16) 0.0281(7) Uani 0.60 1 d P A 2 H33C H 1.0394 0.6849 0.8622 0.034 Uiso 0.60 1 calc PR A 2 H33D H 1.0535 0.6157 0.8007 0.034 Uiso 0.60 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01143(13) 0.01508(12) 0.01343(13) -0.00063(10) 0.00122(10) -0.00206(10) I1 0.02545(11) 0.02943(10) 0.01662(10) 0.00679(8) 0.00318(7) 0.00296(8) I2 0.02221(12) 0.06234(17) 0.04530(15) -0.03537(12) -0.01049(10) 0.00337(11) N1 0.0138(11) 0.0147(10) 0.0146(11) -0.0010(9) 0.0009(9) 0.0024(9) N2 0.0128(11) 0.0138(10) 0.0101(10) -0.0001(8) 0.0022(8) -0.0009(8) C1 0.0172(15) 0.0293(16) 0.0395(19) -0.0078(14) -0.0008(13) 0.0046(13) C2 0.0150(13) 0.0232(13) 0.0150(13) 0.0013(11) 0.0021(11) 0.0031(11) C3 0.0115(13) 0.0221(14) 0.0184(14) -0.0007(11) -0.0024(11) -0.0017(11) C4 0.0157(13) 0.0188(13) 0.0113(12) -0.0029(10) 0.0012(10) -0.0031(11) C5 0.0183(15) 0.0238(15) 0.0327(17) -0.0054(13) 0.0011(13) -0.0072(12) C6 0.0146(13) 0.0232(14) 0.0210(14) -0.0075(11) -0.0004(11) 0.0053(11) C7 0.0225(15) 0.0322(16) 0.0241(16) -0.0047(13) 0.0014(12) 0.0108(13) C8 0.045(2) 0.052(2) 0.0251(18) -0.0170(16) -0.0016(16) 0.0172(18) C9 0.056(3) 0.039(2) 0.046(2) -0.0277(18) -0.003(2) 0.0106(19) C10 0.046(2) 0.0222(16) 0.049(2) -0.0143(15) -0.0002(18) 0.0036(15) C11 0.0241(16) 0.0208(14) 0.0327(17) -0.0053(13) 0.0000(13) 0.0010(12) C12 0.042(2) 0.0411(19) 0.0184(15) 0.0010(14) 0.0105(14) 0.0159(16) C13 0.052(3) 0.068(3) 0.075(3) 0.018(3) 0.020(2) -0.002(2) C14 0.073(3) 0.089(4) 0.036(2) 0.025(2) -0.009(2) 0.004(3) C15 0.0391(19) 0.0148(13) 0.0354(18) -0.0005(12) 0.0063(15) -0.0014(13) C16 0.057(3) 0.0332(19) 0.063(3) -0.0062(18) 0.023(2) -0.0172(19) C17 0.074(3) 0.0270(18) 0.045(2) 0.0079(16) 0.000(2) 0.0078(19) C18 0.0108(12) 0.0141(11) 0.0136(12) 0.0019(10) -0.0001(10) -0.0039(10) C19 0.0209(14) 0.0182(13) 0.0152(13) 0.0015(11) -0.0009(11) -0.0067(11) C20 0.0315(17) 0.0226(14) 0.0191(15) 0.0070(12) -0.0057(13) 0.0003(13) C21 0.0261(16) 0.0187(14) 0.0333(18) 0.0026(12) -0.0075(13) 0.0042(12) C22 0.0229(15) 0.0174(13) 0.0245(16) -0.0022(11) -0.0005(12) 0.0020(12) C23 0.0160(13) 0.0136(12) 0.0167(13) 0.0000(10) 0.0009(11) -0.0020(10) C24 0.0342(18) 0.0288(15) 0.0135(14) 0.0017(12) 0.0030(12) -0.0019(14) C25 0.048(3) 0.090(3) 0.044(2) -0.023(2) 0.023(2) -0.020(2) C26 0.051(2) 0.071(3) 0.0166(16) -0.0098(17) 0.0017(16) -0.013(2) C27 0.0264(16) 0.0197(13) 0.0128(13) -0.0037(11) 0.0028(11) 0.0057(12) C28 0.0358(19) 0.0266(15) 0.0225(16) -0.0063(13) -0.0026(14) 0.0043(14) C29 0.040(2) 0.0339(17) 0.0227(16) -0.0023(13) 0.0148(14) -0.0002(15) O1 0.0135(10) 0.0222(10) 0.0224(10) 0.0040(8) 0.0034(8) 0.0024(8) C30 0.0261(17) 0.0373(18) 0.0348(19) 0.0142(15) 0.0151(14) 0.0012(14) C31 0.0218(18) 0.075(3) 0.046(2) 0.024(2) 0.0102(16) 0.0005(19) C32 0.009(4) 0.031(4) 0.041(5) 0.001(4) 0.008(4) 0.006(3) C33 0.0180(15) 0.0256(15) 0.0378(19) 0.0116(13) -0.0008(13) 0.0005(12) O1A 0.0135(10) 0.0222(10) 0.0224(10) 0.0040(8) 0.0034(8) 0.0024(8) C30A 0.0261(17) 0.0373(18) 0.0348(19) 0.0142(15) 0.0151(14) 0.0012(14) C31A 0.0218(18) 0.075(3) 0.046(2) 0.024(2) 0.0102(16) 0.0005(19) C32A 0.018(3) 0.037(3) 0.043(4) 0.014(3) -0.001(3) -0.003(2) C33A 0.0180(15) 0.0256(15) 0.0378(19) 0.0116(13) -0.0008(13) 0.0005(12) _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 Y1 N2 2.258(2) . ? Y1 N1 2.298(2) . ? Y1 O1 2.3665(19) . ? Y1 I1 2.9287(3) . ? Y1 I2 2.9464(3) . ? N1 C2 1.340(4) . ? N1 C6 1.451(3) . ? N2 C4 1.337(3) . ? N2 C18 1.444(3) . ? C1 C2 1.510(4) . ? C2 C3 1.404(4) . ? C3 C4 1.405(4) . ? C4 C5 1.510(4) . ? C6 C11 1.401(4) . ? C6 C7 1.415(4) . ? C7 C8 1.398(4) . ? C7 C12 1.517(5) . ? C8 C9 1.373(6) . ? C9 C10 1.375(6) . ? C10 C11 1.401(4) . ? C11 C15 1.523(5) . ? C12 C13 1.512(6) . ? C12 C14 1.516(5) . ? C15 C17 1.523(5) . ? C15 C16 1.524(5) . ? C18 C23 1.403(4) . ? C18 C19 1.409(4) . ? C19 C20 1.391(4) . ? C19 C24 1.519(4) . ? C20 C21 1.376(5) . ? C21 C22 1.374(4) . ? C22 C23 1.392(4) . ? C23 C27 1.524(4) . ? C24 C25 1.505(5) . ? C24 C26 1.525(4) . ? C27 C28 1.532(4) . ? C27 C29 1.535(4) . ? O1 C30 1.464(4) . ? O1 C33 1.469(3) . ? C30 C31 1.493(5) . ? C31 C32 1.410(9) . ? C32 C33 1.589(8) . ? 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 N2 Y1 N1 82.94(8) . . ? N2 Y1 O1 96.55(7) . . ? N1 Y1 O1 168.34(7) . . ? N2 Y1 I1 101.07(5) . . ? N1 Y1 I1 100.73(5) . . ? O1 Y1 I1 90.81(5) . . ? N2 Y1 I2 126.14(5) . . ? N1 Y1 I2 91.08(5) . . ? O1 Y1 I2 79.79(5) . . ? I1 Y1 I2 132.480(12) . . ? C2 N1 C6 118.1(2) . . ? C2 N1 Y1 118.20(17) . . ? C6 N1 Y1 122.17(17) . . ? C4 N2 C18 120.3(2) . . ? C4 N2 Y1 121.21(17) . . ? C18 N2 Y1 117.76(16) . . ? N1 C2 C3 124.3(2) . . ? N1 C2 C1 120.1(2) . . ? C3 C2 C1 115.6(3) . . ? C2 C3 C4 130.4(3) . . ? N2 C4 C3 124.0(2) . . ? N2 C4 C5 120.2(2) . . ? C3 C4 C5 115.8(2) . . ? C11 C6 C7 121.1(3) . . ? C11 C6 N1 120.7(3) . . ? C7 C6 N1 118.1(3) . . ? C8 C7 C6 117.7(3) . . ? C8 C7 C12 120.2(3) . . ? C6 C7 C12 122.1(3) . . ? C9 C8 C7 121.3(3) . . ? C8 C9 C10 120.5(3) . . ? C9 C10 C11 120.8(3) . . ? C10 C11 C6 118.4(3) . . ? C10 C11 C15 118.9(3) . . ? C6 C11 C15 122.6(3) . . ? C13 C12 C14 110.7(4) . . ? C13 C12 C7 112.1(3) . . ? C14 C12 C7 112.7(3) . . ? C17 C15 C11 112.4(3) . . ? C17 C15 C16 110.3(3) . . ? C11 C15 C16 110.8(3) . . ? C23 C18 C19 120.6(2) . . ? C23 C18 N2 121.6(2) . . ? C19 C18 N2 117.6(2) . . ? C20 C19 C18 118.4(3) . . ? C20 C19 C24 120.0(3) . . ? C18 C19 C24 121.6(3) . . ? C21 C20 C19 121.3(3) . . ? C22 C21 C20 119.9(3) . . ? C21 C22 C23 121.4(3) . . ? C22 C23 C18 118.4(2) . . ? C22 C23 C27 117.9(2) . . ? C18 C23 C27 123.6(2) . . ? C25 C24 C19 111.7(3) . . ? C25 C24 C26 110.6(3) . . ? C19 C24 C26 113.3(3) . . ? C23 C27 C28 111.3(2) . . ? C23 C27 C29 111.0(2) . . ? C28 C27 C29 109.4(2) . . ? C30 O1 C33 108.5(2) . . ? C30 O1 Y1 117.21(16) . . ? C33 O1 Y1 127.69(17) . . ? O1 C30 C31 106.1(3) . . ? C32 C31 C30 107.3(4) . . ? C31 C32 C33 102.9(5) . . ? O1 C33 C32 101.5(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.766 _refine_diff_density_min -2.292 _refine_diff_density_rms 0.094 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 646372' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H51 I2 N2 O2 Y' _chemical_formula_sum 'C33 H51 I2 N2 O2 Y' _chemical_formula_weight 850.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5924(12) _cell_length_b 32.446(4) _cell_length_c 12.0506(15) _cell_angle_alpha 90.00 _cell_angle_beta 106.910(2) _cell_angle_gamma 90.00 _cell_volume 3588.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13564 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 3.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2288 _exptl_absorpt_correction_T_max 0.4740 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38964 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.67 _reflns_number_total 8297 _reflns_number_gt 6878 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0397P)^2^+7.3331P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8297 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Y1 Y 0.43653(4) 0.341850(10) 0.68880(3) 0.01500(9) Uani 1 1 d . . . I1 I 0.38239(3) 0.301519(9) 0.89775(2) 0.02836(9) Uani 1 1 d . . . I2 I 0.75080(3) 0.324992(10) 0.75445(3) 0.03321(10) Uani 1 1 d . . . N1 N 0.4615(4) 0.40891(10) 0.7651(3) 0.0192(7) Uani 1 1 d . . . N2 N 0.4391(3) 0.37811(10) 0.5218(3) 0.0166(6) Uani 1 1 d . . . C1 C 0.5801(5) 0.47777(13) 0.7945(4) 0.0304(10) Uani 1 1 d . . . H1A H 0.5347 0.4794 0.8575 0.046 Uiso 1 1 calc R . . H1B H 0.5473 0.5010 0.7415 0.046 Uiso 1 1 calc R . . H1C H 0.6863 0.4788 0.8270 0.046 Uiso 1 1 calc R . . C2 C 0.5368(4) 0.43760(12) 0.7288(3) 0.0194(8) Uani 1 1 d . . . C3 C 0.5781(4) 0.43552(12) 0.6268(3) 0.0216(8) Uani 1 1 d . . . H3A H 0.6534 0.4541 0.6236 0.026 Uiso 1 1 calc R . . C4 C 0.5268(4) 0.41057(12) 0.5289(3) 0.0185(8) Uani 1 1 d . . . C5 C 0.5731(5) 0.42469(14) 0.4252(4) 0.0292(10) Uani 1 1 d . . . H5A H 0.4927 0.4205 0.3542 0.044 Uiso 1 1 calc R . . H5B H 0.6579 0.4087 0.4206 0.044 Uiso 1 1 calc R . . H5C H 0.5987 0.4540 0.4335 0.044 Uiso 1 1 calc R . . C6 C 0.4240(5) 0.41682(12) 0.8711(4) 0.0273(9) Uani 1 1 d . . . C7 C 0.5333(6) 0.41283(13) 0.9792(4) 0.0346(11) Uani 1 1 d . . . C8 C 0.4905(8) 0.41832(16) 1.0789(5) 0.0480(15) Uani 1 1 d . . . H8A H 0.5610 0.4160 1.1526 0.058 Uiso 1 1 calc R . . C9 C 0.3508(9) 0.42688(16) 1.0733(5) 0.0563(19) Uani 1 1 d . . . H9A H 0.3246 0.4296 1.1431 0.068 Uiso 1 1 calc R . . C10 C 0.2455(7) 0.43172(15) 0.9683(5) 0.0471(15) Uani 1 1 d . . . H10A H 0.1486 0.4383 0.9670 0.056 Uiso 1 1 calc R . . C11 C 0.2799(6) 0.42696(13) 0.8630(4) 0.0331(11) Uani 1 1 d . . . C12 C 0.6926(6) 0.40448(15) 0.9915(4) 0.0380(12) Uani 1 1 d . . . H12A H 0.7046 0.4028 0.9119 0.046 Uiso 1 1 calc R . . C13 C 0.7444(7) 0.36381(16) 1.0535(5) 0.0512(16) Uani 1 1 d . . . H13A H 0.6888 0.3410 1.0082 0.077 Uiso 1 1 calc R . . H13B H 0.7294 0.3643 1.1305 0.077 Uiso 1 1 calc R . . H13C H 0.8482 0.3600 1.0616 0.077 Uiso 1 1 calc R . . C14 C 0.7908(8) 0.43937(17) 1.0571(5) 0.0602(19) Uani 1 1 d . . . H14A H 0.7561 0.4658 1.0198 0.090 Uiso 1 1 calc R . . H14B H 0.8911 0.4346 1.0557 0.090 Uiso 1 1 calc R . . H14C H 0.7877 0.4400 1.1376 0.090 Uiso 1 1 calc R . . C15 C 0.1675(5) 0.43399(14) 0.7465(5) 0.0371(11) Uani 1 1 d . . . H15A H 0.1831 0.4122 0.6926 0.045 Uiso 1 1 calc R . . C16 C 0.1892(6) 0.47591(15) 0.6944(5) 0.0460(13) Uani 1 1 d . . . H16A H 0.2822 0.4759 0.6760 0.069 Uiso 1 1 calc R . . H16B H 0.1898 0.4978 0.7506 0.069 Uiso 1 1 calc R . . H16C H 0.1095 0.4807 0.6234 0.069 Uiso 1 1 calc R . . C17 C 0.0097(7) 0.4302(2) 0.7493(7) 0.0611(19) Uani 1 1 d . . . H17A H -0.0030 0.4041 0.7862 0.092 Uiso 1 1 calc R . . H17B H -0.0558 0.4309 0.6700 0.092 Uiso 1 1 calc R . . H17C H -0.0134 0.4532 0.7937 0.092 Uiso 1 1 calc R . . C18 C 0.3594(4) 0.36529(13) 0.4058(3) 0.0215(8) Uani 1 1 d . . . C19 C 0.4130(5) 0.33531(14) 0.3454(4) 0.0309(10) Uani 1 1 d . . . C20 C 0.3316(6) 0.32585(16) 0.2314(4) 0.0396(13) Uani 1 1 d . . . H20A H 0.3672 0.3058 0.1890 0.048 Uiso 1 1 calc R . . C21 C 0.2008(6) 0.34520(17) 0.1801(4) 0.0431(14) Uani 1 1 d . . . H21A H 0.1482 0.3391 0.1021 0.052 Uiso 1 1 calc R . . C22 C 0.1470(6) 0.37326(16) 0.2417(4) 0.0377(12) Uani 1 1 d . . . H22A H 0.0546 0.3855 0.2067 0.045 Uiso 1 1 calc R . . C23 C 0.2236(4) 0.38433(13) 0.3538(4) 0.0240(9) Uani 1 1 d . . . C24 C 0.5540(6) 0.31212(16) 0.3987(5) 0.0414(12) Uani 1 1 d . . . H24A H 0.5927 0.3201 0.4822 0.050 Uiso 1 1 calc R . . C25 C 0.6694(7) 0.3223(2) 0.3368(8) 0.068(2) Uani 1 1 d . . . H25A H 0.6911 0.3519 0.3439 0.102 Uiso 1 1 calc R . . H25B H 0.6320 0.3149 0.2546 0.102 Uiso 1 1 calc R . . H25C H 0.7585 0.3067 0.3726 0.102 Uiso 1 1 calc R . . C26 C 0.5283(7) 0.26569(17) 0.3912(6) 0.0554(16) Uani 1 1 d . . . H26A H 0.4399 0.2592 0.4128 0.083 Uiso 1 1 calc R . . H26B H 0.6118 0.2517 0.4443 0.083 Uiso 1 1 calc R . . H26C H 0.5167 0.2564 0.3117 0.083 Uiso 1 1 calc R . . C27 C 0.1626(5) 0.41676(14) 0.4173(4) 0.0295(10) Uani 1 1 d . . . H27A H 0.2184 0.4151 0.5013 0.035 Uiso 1 1 calc R . . C28 C 0.1854(6) 0.45986(16) 0.3751(6) 0.0483(14) Uani 1 1 d . . . H28A H 0.2892 0.4641 0.3836 0.072 Uiso 1 1 calc R . . H28B H 0.1522 0.4804 0.4213 0.072 Uiso 1 1 calc R . . H28C H 0.1295 0.4627 0.2933 0.072 Uiso 1 1 calc R . . C29 C 0.0018(5) 0.41040(18) 0.4077(5) 0.0430(13) Uani 1 1 d . . . H29A H -0.0129 0.3823 0.4322 0.064 Uiso 1 1 calc R . . H29B H -0.0569 0.4145 0.3271 0.064 Uiso 1 1 calc R . . H29C H -0.0280 0.4303 0.4577 0.064 Uiso 1 1 calc R . . C30 C 0.0696(5) 0.32881(15) 0.6515(4) 0.0319(10) Uani 1 1 d . . . H30A H -0.0210 0.3397 0.5991 0.048 Uiso 1 1 calc R . . H30B H 0.0998 0.3460 0.7214 0.048 Uiso 1 1 calc R . . H30C H 0.0537 0.3005 0.6733 0.048 Uiso 1 1 calc R . . O1 O 0.1822(3) 0.32920(9) 0.5938(2) 0.0219(6) Uani 1 1 d . . . C31 C 0.1605(5) 0.29659(13) 0.5078(4) 0.0271(9) Uani 1 1 d . . . H31A H 0.1949 0.3058 0.4419 0.033 Uiso 1 1 calc R . . H31B H 0.0555 0.2899 0.4778 0.033 Uiso 1 1 calc R . . C32 C 0.2433(5) 0.25940(13) 0.5621(4) 0.0281(9) Uani 1 1 d . . . H32A H 0.2023 0.2481 0.6223 0.034 Uiso 1 1 calc R . . H32B H 0.2378 0.2378 0.5029 0.034 Uiso 1 1 calc R . . O2 O 0.3914(3) 0.27193(8) 0.6130(3) 0.0250(6) Uani 1 1 d . . . C33 C 0.4812(6) 0.23640(14) 0.6605(5) 0.0420(13) Uani 1 1 d . . . H33A H 0.4810 0.2172 0.5977 0.063 Uiso 1 1 calc R . . H33B H 0.4419 0.2226 0.7173 0.063 Uiso 1 1 calc R . . H33C H 0.5811 0.2455 0.6984 0.063 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 Y1 0.01076(17) 0.01536(17) 0.01830(18) 0.00043(13) 0.00330(13) -0.00065(13) I1 0.02799(16) 0.03276(16) 0.02435(15) 0.00626(11) 0.00766(11) -0.00545(12) I2 0.01293(14) 0.03817(18) 0.0474(2) 0.00556(13) 0.00691(12) 0.00383(11) N1 0.0221(17) 0.0184(15) 0.0160(16) 0.0001(12) 0.0037(13) -0.0014(13) N2 0.0119(15) 0.0223(16) 0.0153(15) -0.0019(12) 0.0034(12) -0.0018(12) C1 0.043(3) 0.024(2) 0.021(2) -0.0029(16) 0.0038(19) -0.0097(19) C2 0.0179(19) 0.0196(18) 0.0182(18) -0.0003(14) 0.0011(15) -0.0012(15) C3 0.0168(19) 0.0230(19) 0.023(2) 0.0006(15) 0.0035(16) -0.0070(16) C4 0.0123(17) 0.0238(19) 0.0191(19) 0.0005(14) 0.0040(14) -0.0014(15) C5 0.032(2) 0.035(2) 0.024(2) -0.0003(17) 0.0136(18) -0.0098(19) C6 0.046(3) 0.0159(18) 0.024(2) -0.0002(15) 0.017(2) -0.0023(18) C7 0.065(3) 0.0187(19) 0.020(2) -0.0030(16) 0.012(2) -0.007(2) C8 0.087(5) 0.034(3) 0.027(3) -0.003(2) 0.024(3) -0.011(3) C9 0.116(6) 0.029(3) 0.039(3) -0.010(2) 0.047(4) -0.020(3) C10 0.064(4) 0.030(3) 0.066(4) -0.012(2) 0.048(3) -0.013(2) C11 0.047(3) 0.020(2) 0.041(3) -0.0046(18) 0.027(2) -0.0052(19) C12 0.044(3) 0.035(3) 0.023(2) 0.0000(18) -0.008(2) -0.005(2) C13 0.060(4) 0.034(3) 0.041(3) 0.003(2) -0.015(3) -0.005(3) C14 0.079(5) 0.038(3) 0.039(3) 0.005(2) -0.022(3) -0.016(3) C15 0.028(2) 0.028(2) 0.061(3) -0.009(2) 0.022(2) 0.0008(19) C16 0.041(3) 0.030(3) 0.065(4) 0.000(2) 0.012(3) 0.010(2) C17 0.038(3) 0.053(4) 0.106(6) -0.019(3) 0.041(4) 0.002(3) C18 0.0172(19) 0.030(2) 0.0181(19) 0.0003(15) 0.0066(15) -0.0079(16) C19 0.031(2) 0.035(2) 0.032(2) -0.0112(18) 0.016(2) -0.016(2) C20 0.053(3) 0.043(3) 0.028(2) -0.014(2) 0.022(2) -0.024(2) C21 0.053(3) 0.051(3) 0.019(2) -0.005(2) 0.001(2) -0.032(3) C22 0.032(3) 0.050(3) 0.023(2) 0.008(2) -0.0032(19) -0.019(2) C23 0.0176(19) 0.030(2) 0.022(2) 0.0039(16) 0.0016(16) -0.0101(17) C24 0.040(3) 0.040(3) 0.049(3) -0.016(2) 0.021(2) 0.000(2) C25 0.044(4) 0.058(4) 0.115(6) -0.020(4) 0.044(4) -0.008(3) C26 0.056(4) 0.043(3) 0.084(5) -0.010(3) 0.047(4) 0.006(3) C27 0.0143(19) 0.039(2) 0.030(2) 0.0113(19) -0.0012(17) 0.0025(18) C28 0.034(3) 0.037(3) 0.078(4) 0.015(3) 0.022(3) 0.005(2) C29 0.021(2) 0.059(3) 0.045(3) 0.016(3) 0.003(2) 0.001(2) C30 0.018(2) 0.040(3) 0.042(3) 0.005(2) 0.015(2) -0.0006(18) O1 0.0134(13) 0.0272(15) 0.0257(15) 0.0006(11) 0.0068(11) -0.0021(11) C31 0.021(2) 0.029(2) 0.029(2) -0.0029(17) 0.0024(17) -0.0089(17) C32 0.023(2) 0.022(2) 0.038(2) -0.0053(17) 0.0077(18) -0.0091(17) O2 0.0182(14) 0.0176(13) 0.0360(17) -0.0052(11) 0.0026(12) -0.0001(11) C33 0.032(3) 0.023(2) 0.067(4) -0.001(2) 0.007(2) 0.009(2) _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 Y1 N2 2.337(3) . ? Y1 N1 2.347(3) . ? Y1 O1 2.410(3) . ? Y1 O2 2.437(3) . ? Y1 I2 2.9369(6) . ? Y1 I1 3.0138(5) . ? N1 C2 1.328(5) . ? N1 C6 1.447(5) . ? N2 C4 1.336(5) . ? N2 C18 1.446(5) . ? C1 C2 1.519(5) . ? C2 C3 1.398(6) . ? C3 C4 1.397(5) . ? C4 C5 1.514(6) . ? C6 C11 1.397(7) . ? C6 C7 1.421(7) . ? C7 C8 1.389(7) . ? C7 C12 1.516(8) . ? C8 C9 1.351(10) . ? C9 C10 1.379(9) . ? C10 C11 1.410(7) . ? C11 C15 1.518(7) . ? C12 C13 1.527(7) . ? C12 C14 1.536(7) . ? C15 C17 1.529(7) . ? C15 C16 1.538(7) . ? C18 C19 1.399(6) . ? C18 C23 1.413(6) . ? C19 C20 1.403(7) . ? C19 C24 1.517(8) . ? C20 C21 1.378(8) . ? C21 C22 1.367(8) . ? C22 C23 1.384(6) . ? C23 C27 1.515(7) . ? C24 C26 1.525(8) . ? C24 C25 1.540(8) . ? C27 C28 1.525(7) . ? C27 C29 1.527(6) . ? C30 O1 1.445(5) . ? O1 C31 1.453(5) . ? C31 C32 1.487(6) . ? C32 O2 1.433(5) . ? O2 C33 1.453(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 N2 Y1 N1 81.10(11) . . ? N2 Y1 O1 86.51(10) . . ? N1 Y1 O1 108.53(11) . . ? N2 Y1 O2 101.00(11) . . ? N1 Y1 O2 175.29(11) . . ? O1 Y1 O2 67.57(10) . . ? N2 Y1 I2 93.37(8) . . ? N1 Y1 I2 95.01(8) . . ? O1 Y1 I2 156.11(7) . . ? O2 Y1 I2 89.09(7) . . ? N2 Y1 I1 170.19(8) . . ? N1 Y1 I1 95.62(8) . . ? O1 Y1 I1 85.78(7) . . ? O2 Y1 I1 81.61(8) . . ? I2 Y1 I1 96.137(14) . . ? C2 N1 C6 117.7(3) . . ? C2 N1 Y1 121.6(3) . . ? C6 N1 Y1 119.2(2) . . ? C4 N2 C18 115.8(3) . . ? C4 N2 Y1 120.4(2) . . ? C18 N2 Y1 123.6(2) . . ? N1 C2 C3 125.2(4) . . ? N1 C2 C1 121.4(4) . . ? C3 C2 C1 113.3(4) . . ? C4 C3 C2 130.5(4) . . ? N2 C4 C3 124.9(4) . . ? N2 C4 C5 121.1(3) . . ? C3 C4 C5 113.9(3) . . ? C11 C6 C7 122.5(4) . . ? C11 C6 N1 118.4(4) . . ? C7 C6 N1 119.1(4) . . ? C8 C7 C6 117.2(5) . . ? C8 C7 C12 118.8(5) . . ? C6 C7 C12 124.0(4) . . ? C9 C8 C7 121.4(6) . . ? C8 C9 C10 121.4(5) . . ? C9 C10 C11 120.8(6) . . ? C6 C11 C10 116.7(5) . . ? C6 C11 C15 121.5(4) . . ? C10 C11 C15 121.8(5) . . ? C7 C12 C13 112.2(5) . . ? C7 C12 C14 111.6(5) . . ? C13 C12 C14 108.8(4) . . ? C11 C15 C17 114.1(5) . . ? C11 C15 C16 111.5(4) . . ? C17 C15 C16 109.4(5) . . ? C19 C18 C23 120.3(4) . . ? C19 C18 N2 122.1(4) . . ? C23 C18 N2 117.5(4) . . ? C18 C19 C20 118.5(5) . . ? C18 C19 C24 122.8(4) . . ? C20 C19 C24 118.7(4) . . ? C21 C20 C19 121.0(5) . . ? C22 C21 C20 119.9(4) . . ? C21 C22 C23 121.7(5) . . ? C22 C23 C18 118.6(4) . . ? C22 C23 C27 120.0(4) . . ? C18 C23 C27 121.5(4) . . ? C19 C24 C26 110.9(5) . . ? C19 C24 C25 111.5(5) . . ? C26 C24 C25 108.1(4) . . ? C23 C27 C28 110.8(4) . . ? C23 C27 C29 113.4(4) . . ? C28 C27 C29 109.8(4) . . ? C30 O1 C31 111.4(3) . . ? C30 O1 Y1 124.6(3) . . ? C31 O1 Y1 112.2(2) . . ? O1 C31 C32 109.3(3) . . ? O2 C32 C31 107.1(3) . . ? C32 O2 C33 110.1(3) . . ? C32 O2 Y1 118.1(2) . . ? C33 O2 Y1 124.8(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.685 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.141 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 646373' _refine_special_details ; Highly disordered lattice solvent molecules (31 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 389.2 \%A**3, equating to one quarter occupancy molecule of iso-hexane per dimer, 1 half occupancy molecule in the unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. One iso-propyl group is rotationally disordered over two sites. The potassium-bound THF molecule is disordered over three sites. Each case of disorder was modelled with a two or three part model, respectively, and restraints and constraints were applied. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C81.50 H119.50 K2 O2 P2' _chemical_formula_sum 'C81.50 H119.50 K2 O2 P2' _chemical_formula_weight 1271.41 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2787(10) _cell_length_b 20.6530(15) _cell_length_c 15.3612(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.600(2) _cell_angle_gamma 90.00 _cell_volume 4076.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5890 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.58 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1385 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8914 _exptl_absorpt_correction_T_max 0.9187 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18780 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5318 _reflns_number_gt 4207 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.1084P)^2^+1.2074P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, PH and Me from difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5318 _refine_ls_number_parameters 479 _refine_ls_number_restraints 112 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1672 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.45361(6) 0.09229(3) 0.41407(4) 0.0535(3) Uani 1 1 d . . . P1 P 0.43925(6) 0.03967(4) 0.60959(5) 0.0453(3) Uani 1 1 d . . . H1P H 0.344(2) 0.0599(14) 0.5765(18) 0.047(8) Uiso 1 1 d . . . C1 C 0.4724(2) 0.08378(13) 0.71452(18) 0.0370(7) Uani 1 1 d . . . C2 C 0.4076(2) 0.12912(13) 0.74326(18) 0.0379(7) Uani 1 1 d . B . C3 C 0.4443(2) 0.16229(14) 0.82395(19) 0.0449(7) Uani 1 1 d . . . H3 H 0.3999 0.1925 0.8424 0.054 Uiso 1 1 calc R B . C4 C 0.5428(2) 0.15264(15) 0.8776(2) 0.0488(8) Uani 1 1 d . B . H4 H 0.5676 0.1776 0.9306 0.059 Uiso 1 1 calc R . . C5 C 0.6050(2) 0.10619(15) 0.85331(19) 0.0445(7) Uani 1 1 d . . . H5 H 0.6723 0.0981 0.8911 0.053 Uiso 1 1 calc R B . C6 C 0.5706(2) 0.07083(14) 0.77408(18) 0.0383(7) Uani 1 1 d . B . C7 C 0.2974(2) 0.14100(13) 0.68990(18) 0.0385(7) Uani 1 1 d . . . C8 C 0.2714(2) 0.19893(14) 0.64130(19) 0.0424(7) Uani 1 1 d . A . C9 C 0.1680(2) 0.20816(15) 0.5932(2) 0.0516(8) Uani 1 1 d . . . H9 H 0.1499 0.2473 0.5606 0.062 Uiso 1 1 calc R B . C10 C 0.0909(2) 0.16254(16) 0.5911(2) 0.0500(8) Uani 1 1 d . B . C11 C 0.1189(2) 0.10649(15) 0.6392(2) 0.0470(8) Uani 1 1 d . . . H11 H 0.0670 0.0748 0.6389 0.056 Uiso 1 1 calc R B . C12 C 0.2201(2) 0.09439(13) 0.68839(19) 0.0397(7) Uani 1 1 d . B . C13 C 0.3525(2) 0.25030(15) 0.6392(2) 0.0518(8) Uani 0.233(13) 1 d PDU A 1 H13 H 0.4023 0.2501 0.7001 0.062 Uiso 0.233(13) 1 calc PR A 1 C14 C 0.4140(13) 0.2283(9) 0.5732(12) 0.058(4) Uani 0.233(13) 1 d PDU A 1 H14A H 0.4452 0.1859 0.5915 0.087 Uiso 0.233(13) 1 calc PR A 1 H14B H 0.4691 0.2598 0.5727 0.087 Uiso 0.233(13) 1 calc PR A 1 H14C H 0.3673 0.2251 0.5128 0.087 Uiso 0.233(13) 1 calc PR A 1 C15 C 0.3083(14) 0.3181(6) 0.6245(19) 0.064(4) Uani 0.233(13) 1 d PDU A 1 H15A H 0.2654 0.3265 0.6668 0.096 Uiso 0.233(13) 1 calc PR A 1 H15B H 0.2654 0.3222 0.5627 0.096 Uiso 0.233(13) 1 calc PR A 1 H15C H 0.3654 0.3495 0.6346 0.096 Uiso 0.233(13) 1 calc PR A 1 C13A C 0.3525(2) 0.25030(15) 0.6392(2) 0.0518(8) Uani 0.767(13) 1 d P A 2 H13A H 0.4211 0.2345 0.6765 0.062 Uiso 0.767(13) 1 calc PR A 2 C14A C 0.3636(7) 0.2623(5) 0.5439(5) 0.099(3) Uani 0.767(13) 1 d P A 2 H14D H 0.3007 0.2836 0.5083 0.149 Uiso 0.767(13) 1 calc PR A 2 H14E H 0.3732 0.2209 0.5160 0.149 Uiso 0.767(13) 1 calc PR A 2 H14F H 0.4241 0.2901 0.5465 0.149 Uiso 0.767(13) 1 calc PR A 2 C15A C 0.3291(6) 0.3142(3) 0.6780(6) 0.075(2) Uani 0.767(13) 1 d P A 2 H15D H 0.3232 0.3075 0.7396 0.113 Uiso 0.767(13) 1 calc PR A 2 H15E H 0.2635 0.3315 0.6411 0.113 Uiso 0.767(13) 1 calc PR A 2 H15F H 0.3855 0.3448 0.6783 0.113 Uiso 0.767(13) 1 calc PR A 2 C16 C -0.0206(2) 0.17253(18) 0.5359(3) 0.0644(10) Uani 1 1 d . . . H16 H -0.0628 0.1373 0.5541 0.077 Uiso 1 1 calc R B . C17 C -0.0302(3) 0.1635(2) 0.4378(3) 0.0841(13) Uani 1 1 d . B . H17A H -0.1036 0.1662 0.4050 0.126 Uiso 1 1 calc R . . H17B H -0.0025 0.1209 0.4276 0.126 Uiso 1 1 calc R . . H17C H 0.0093 0.1974 0.4163 0.126 Uiso 1 1 calc R . . C18 C -0.0666(3) 0.23458(19) 0.5559(3) 0.0730(11) Uani 1 1 d . B . H18A H -0.0261 0.2708 0.5413 0.109 Uiso 1 1 calc R . . H18B H -0.0654 0.2362 0.6199 0.109 Uiso 1 1 calc R . . H18C H -0.1386 0.2377 0.5197 0.109 Uiso 1 1 calc R . . C19 C 0.2431(2) 0.03148(14) 0.7403(2) 0.0460(7) Uani 1 1 d . . . H19 H 0.3202 0.0249 0.7560 0.055 Uiso 1 1 calc R B . C20 C 0.1928(3) -0.02729(16) 0.6858(2) 0.0643(9) Uani 1 1 d . B . H20A H 0.1169 -0.0238 0.6733 0.096 Uiso 1 1 calc R . . H20B H 0.2158 -0.0669 0.7202 0.096 Uiso 1 1 calc R . . H20C H 0.2134 -0.0289 0.6289 0.096 Uiso 1 1 calc R . . C21 C 0.2096(3) 0.03532(19) 0.8277(2) 0.0745(11) Uani 1 1 d . B . H21A H 0.1348 0.0442 0.8144 0.112 Uiso 1 1 calc R . . H21B H 0.2479 0.0702 0.8651 0.112 Uiso 1 1 calc R . . H21C H 0.2246 -0.0059 0.8599 0.112 Uiso 1 1 calc R . . C22 C 0.6336(2) 0.01334(14) 0.75994(18) 0.0400(7) Uani 1 1 d . . . C23 C 0.6185(2) -0.04561(14) 0.80090(19) 0.0438(7) Uani 1 1 d . . . C24 C 0.6806(2) -0.09863(16) 0.7934(2) 0.0521(8) Uani 1 1 d . . . H24 H 0.6702 -0.1382 0.8215 0.063 Uiso 1 1 calc R B . C25 C 0.7570(3) -0.09577(17) 0.7465(3) 0.0589(9) Uani 1 1 d . . . C26 C 0.7686(2) -0.03769(17) 0.7055(2) 0.0585(9) Uani 1 1 d . . . H26 H 0.8199 -0.0349 0.6723 0.070 Uiso 1 1 calc R B . C27 C 0.7090(2) 0.01701(15) 0.7104(2) 0.0461(8) Uani 1 1 d . . . C28 C 0.5388(2) -0.05185(16) 0.8556(2) 0.0523(8) Uani 1 1 d . . . H28 H 0.5008 -0.0097 0.8510 0.063 Uiso 1 1 calc R B . C29 C 0.5919(3) -0.0629(2) 0.9554(2) 0.0770(11) Uani 1 1 d . B . H29A H 0.6330 -0.1029 0.9620 0.115 Uiso 1 1 calc R . . H29B H 0.5388 -0.0667 0.9894 0.115 Uiso 1 1 calc R . . H29C H 0.6377 -0.0263 0.9784 0.115 Uiso 1 1 calc R . . C30 C 0.4590(3) -0.1037(2) 0.8183(3) 0.0729(11) Uani 1 1 d . B . H30A H 0.4238 -0.0934 0.7557 0.109 Uiso 1 1 calc R . . H30B H 0.4077 -0.1055 0.8542 0.109 Uiso 1 1 calc R . . H30C H 0.4938 -0.1457 0.8207 0.109 Uiso 1 1 calc R . . C31 C 0.8255(3) -0.15395(19) 0.7381(3) 0.0816(12) Uani 1 1 d . . . H31 H 0.8961 -0.1369 0.7384 0.098 Uiso 1 1 calc R B . C32 C 0.8392(5) -0.2027(3) 0.8172(4) 0.141(2) Uani 1 1 d . B . H32A H 0.7730 -0.2249 0.8136 0.211 Uiso 1 1 calc R . . H32B H 0.8606 -0.1794 0.8744 0.211 Uiso 1 1 calc R . . H32C H 0.8926 -0.2346 0.8134 0.211 Uiso 1 1 calc R . . C33 C 0.7851(4) -0.1880(3) 0.6521(4) 0.1103(18) Uani 1 1 d . B . H33A H 0.7147 -0.2039 0.6488 0.165 Uiso 1 1 calc R . . H33B H 0.8306 -0.2247 0.6482 0.165 Uiso 1 1 calc R . . H33C H 0.7831 -0.1582 0.6021 0.165 Uiso 1 1 calc R . . C34 C 0.7270(3) 0.08007(16) 0.6663(2) 0.0566(9) Uani 1 1 d . . . H34 H 0.6640 0.1077 0.6608 0.068 Uiso 1 1 calc R B . C35 C 0.8198(3) 0.1161(2) 0.7251(3) 0.0846(13) Uani 1 1 d . B . H35A H 0.8828 0.0899 0.7316 0.127 Uiso 1 1 calc R . . H35B H 0.8076 0.1239 0.7845 0.127 Uiso 1 1 calc R . . H35C H 0.8285 0.1576 0.6969 0.127 Uiso 1 1 calc R . . C36 C 0.7428(3) 0.07062(19) 0.5724(2) 0.0645(9) Uani 1 1 d . B . H36A H 0.7426 0.1129 0.5433 0.097 Uiso 1 1 calc R . . H36B H 0.6864 0.0439 0.5368 0.097 Uiso 1 1 calc R . . H36C H 0.8097 0.0491 0.5767 0.097 Uiso 1 1 calc R . . O1 O 0.5380(2) 0.20497(11) 0.38972(18) 0.0753(7) Uani 0.50 1 d PDU B 1 C37 C 0.4881(3) 0.2610(2) 0.3436(4) 0.0907(14) Uani 0.50 1 d PDU B 1 H37A H 0.4388 0.2796 0.3756 0.109 Uiso 0.50 1 calc PR B 1 H37B H 0.4492 0.2496 0.2816 0.109 Uiso 0.50 1 calc PR B 1 C38 C 0.5718(4) 0.3080(3) 0.3417(4) 0.1173(19) Uani 0.50 1 d PDU B 1 H38A H 0.5875 0.3078 0.2821 0.141 Uiso 0.50 1 calc PR B 1 H38B H 0.5504 0.3523 0.3541 0.141 Uiso 0.50 1 calc PR B 1 C39 C 0.6635(8) 0.2876(5) 0.4119(11) 0.124(3) Uani 0.50 1 d PDU B 1 H39A H 0.6721 0.3149 0.4663 0.149 Uiso 0.50 1 calc PR B 1 H39B H 0.7273 0.2908 0.3900 0.149 Uiso 0.50 1 calc PR B 1 C40 C 0.6424(6) 0.2197(5) 0.4315(10) 0.104(3) Uani 0.50 1 d PDU B 1 H40A H 0.6891 0.1905 0.4088 0.125 Uiso 0.50 1 calc PR B 1 H40B H 0.6557 0.2134 0.4974 0.125 Uiso 0.50 1 calc PR B 1 O1A O 0.5380(2) 0.20497(11) 0.38972(18) 0.0753(7) Uani 0.40 1 d PD B 2 C37A C 0.4881(3) 0.2610(2) 0.3436(4) 0.0907(14) Uani 0.40 1 d PD B 2 H37C H 0.4388 0.2796 0.3756 0.109 Uiso 0.40 1 calc PR B 2 H37D H 0.4492 0.2496 0.2816 0.109 Uiso 0.40 1 calc PR B 2 C38A C 0.5718(4) 0.3080(3) 0.3417(4) 0.1173(19) Uani 0.40 1 d PD B 2 H38C H 0.5544 0.3337 0.2855 0.141 Uiso 0.40 1 calc PR B 2 H38D H 0.5833 0.3379 0.3937 0.141 Uiso 0.40 1 calc PR B 2 C39A C 0.6648(7) 0.2673(7) 0.3466(9) 0.085(5) Uani 0.40 1 d PD B 2 H39C H 0.6751 0.2596 0.2858 0.102 Uiso 0.40 1 calc PR B 2 H39D H 0.7280 0.2881 0.3843 0.102 Uiso 0.40 1 calc PR B 2 C40A C 0.6430(5) 0.2072(6) 0.3867(10) 0.139(10) Uani 0.40 1 d PD B 2 H40C H 0.6582 0.1703 0.3510 0.167 Uiso 0.40 1 calc PR B 2 H40D H 0.6884 0.2036 0.4484 0.167 Uiso 0.40 1 calc PR B 2 O1B O 0.5380(2) 0.20497(11) 0.38972(18) 0.0753(7) Uani 0.10 1 d PDU B 3 C37B C 0.606(3) 0.2236(13) 0.335(2) 0.055(4) Uani 0.10 1 d PDU B 3 H37E H 0.5686 0.2226 0.2704 0.065 Uiso 0.10 1 calc PR B 3 H37F H 0.6661 0.1937 0.3444 0.065 Uiso 0.10 1 calc PR B 3 C38B C 0.643(4) 0.2908(15) 0.362(3) 0.042(4) Uani 0.10 1 d PDU B 3 H38E H 0.6106 0.3216 0.3137 0.050 Uiso 0.10 1 calc PR B 3 H38F H 0.7191 0.2932 0.3724 0.050 Uiso 0.10 1 calc PR B 3 C39B C 0.612(3) 0.3086(10) 0.4468(18) 0.044(4) Uani 0.10 1 d PDU B 3 H39E H 0.6701 0.3288 0.4922 0.053 Uiso 0.10 1 calc PR B 3 H39F H 0.5497 0.3364 0.4355 0.053 Uiso 0.10 1 calc PR B 3 C40B C 0.591(2) 0.2405(10) 0.4700(10) 0.049(4) Uani 0.10 1 d PDU B 3 H40E H 0.6577 0.2186 0.4986 0.059 Uiso 0.10 1 calc PR B 3 H40F H 0.5476 0.2407 0.5136 0.059 Uiso 0.10 1 calc PR B 3 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 K1 0.0758(5) 0.0373(4) 0.0430(4) -0.0003(3) 0.0068(3) -0.0021(3) P1 0.0431(5) 0.0542(5) 0.0365(5) -0.0131(4) 0.0060(3) -0.0016(4) C1 0.0373(15) 0.0366(16) 0.0367(15) -0.0050(12) 0.0084(12) -0.0058(12) C2 0.0376(15) 0.0366(16) 0.0384(16) -0.0030(13) 0.0076(12) -0.0024(12) C3 0.0458(17) 0.0417(17) 0.0464(17) -0.0098(14) 0.0098(14) 0.0042(13) C4 0.0476(18) 0.0533(19) 0.0405(16) -0.0167(15) 0.0017(14) -0.0036(15) C5 0.0364(16) 0.0484(18) 0.0440(17) -0.0109(14) 0.0014(13) -0.0012(13) C6 0.0359(15) 0.0393(16) 0.0389(16) -0.0049(13) 0.0079(12) -0.0030(12) C7 0.0409(15) 0.0376(17) 0.0358(15) -0.0086(13) 0.0077(12) 0.0037(13) C8 0.0408(16) 0.0383(17) 0.0463(17) -0.0031(13) 0.0074(13) -0.0005(13) C9 0.0533(19) 0.0434(18) 0.0554(19) 0.0115(15) 0.0089(15) 0.0054(15) C10 0.0381(16) 0.051(2) 0.0561(19) 0.0018(16) 0.0020(14) -0.0059(14) C11 0.0405(17) 0.0469(19) 0.0521(18) -0.0002(15) 0.0087(14) -0.0064(14) C12 0.0393(16) 0.0390(17) 0.0395(16) -0.0039(13) 0.0075(13) -0.0020(13) C13 0.0467(17) 0.0414(18) 0.064(2) 0.0045(15) 0.0079(15) -0.0017(14) C14 0.053(7) 0.054(8) 0.066(7) 0.002(6) 0.012(6) -0.020(6) C15 0.054(7) 0.037(6) 0.092(9) 0.014(7) 0.002(8) -0.014(5) C13A 0.0467(17) 0.0414(18) 0.064(2) 0.0045(15) 0.0079(15) -0.0017(14) C14A 0.114(6) 0.097(6) 0.102(5) -0.015(4) 0.056(5) -0.044(5) C15A 0.078(4) 0.047(3) 0.098(5) -0.003(3) 0.016(4) -0.012(3) C16 0.0417(18) 0.061(2) 0.081(3) 0.0149(19) -0.0021(17) -0.0046(16) C17 0.063(2) 0.078(3) 0.089(3) -0.013(2) -0.022(2) -0.004(2) C18 0.0438(19) 0.082(3) 0.088(3) 0.014(2) 0.0072(18) 0.0020(18) C19 0.0430(16) 0.0439(18) 0.0498(18) 0.0024(14) 0.0095(13) -0.0005(13) C20 0.074(2) 0.0457(19) 0.070(2) 0.0035(17) 0.0129(18) -0.0115(17) C21 0.102(3) 0.066(2) 0.056(2) 0.0104(19) 0.020(2) 0.013(2) C22 0.0346(15) 0.0421(17) 0.0382(15) -0.0113(13) -0.0005(12) -0.0025(13) C23 0.0412(16) 0.0476(19) 0.0374(16) -0.0032(14) 0.0002(13) 0.0027(14) C24 0.0513(18) 0.0456(19) 0.0527(19) -0.0067(15) 0.0006(15) 0.0040(15) C25 0.0448(18) 0.053(2) 0.076(2) -0.0175(18) 0.0109(17) 0.0034(15) C26 0.0439(18) 0.060(2) 0.077(2) -0.0225(19) 0.0252(16) -0.0056(16) C27 0.0368(15) 0.0486(18) 0.0539(18) -0.0171(15) 0.0130(14) -0.0088(14) C28 0.0544(19) 0.054(2) 0.0496(18) 0.0111(15) 0.0160(15) 0.0085(15) C29 0.091(3) 0.091(3) 0.051(2) 0.016(2) 0.020(2) 0.013(2) C30 0.060(2) 0.078(3) 0.083(3) 0.016(2) 0.024(2) -0.0044(19) C31 0.071(2) 0.059(2) 0.115(3) -0.024(2) 0.023(2) 0.014(2) C32 0.136(5) 0.114(4) 0.156(5) -0.004(4) 0.008(4) 0.078(4) C33 0.085(3) 0.102(4) 0.137(4) -0.048(3) 0.017(3) 0.024(3) C34 0.0507(18) 0.052(2) 0.073(2) -0.0128(17) 0.0257(17) -0.0146(15) C35 0.095(3) 0.079(3) 0.082(3) -0.026(2) 0.028(2) -0.045(2) C36 0.059(2) 0.071(2) 0.065(2) -0.0101(19) 0.0197(17) -0.0181(18) O1 0.0835(18) 0.0506(14) 0.0891(18) 0.0131(13) 0.0166(14) -0.0066(12) C37 0.077(3) 0.073(3) 0.118(4) 0.034(3) 0.018(3) -0.004(2) C38 0.090(4) 0.094(4) 0.155(5) 0.058(3) 0.005(3) -0.019(3) C39 0.090(5) 0.101(6) 0.159(7) 0.059(6) -0.012(5) -0.032(5) C40 0.081(5) 0.080(6) 0.133(7) 0.051(5) -0.005(5) -0.007(4) O1A 0.0835(18) 0.0506(14) 0.0891(18) 0.0131(13) 0.0166(14) -0.0066(12) C37A 0.077(3) 0.073(3) 0.118(4) 0.034(3) 0.018(3) -0.004(2) C38A 0.090(4) 0.094(4) 0.155(5) 0.058(3) 0.005(3) -0.019(3) C39A 0.039(6) 0.141(14) 0.081(8) 0.049(9) 0.024(5) 0.028(7) C40A 0.079(9) 0.081(10) 0.191(19) -0.071(12) -0.089(11) 0.044(8) O1B 0.0835(18) 0.0506(14) 0.0891(18) 0.0131(13) 0.0166(14) -0.0066(12) C37B 0.068(8) 0.038(8) 0.056(7) 0.008(7) 0.012(7) -0.001(8) C38B 0.046(10) 0.036(8) 0.053(9) 0.011(8) 0.031(8) 0.004(8) C39B 0.046(9) 0.034(7) 0.064(9) 0.007(7) 0.038(8) 0.004(7) C40B 0.057(8) 0.037(7) 0.069(7) 0.012(6) 0.045(7) -0.001(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 K1 O1 2.650(2) . ? K1 P1 3.1376(11) 3_656 ? K1 C25 3.230(4) 3_656 ? K1 C24 3.239(3) 3_656 ? K1 P1 3.2445(11) . ? K1 C26 3.259(3) 3_656 ? K1 C23 3.340(3) 3_656 ? K1 C27 3.366(3) 3_656 ? K1 C22 3.418(3) 3_656 ? K1 K1 4.6239(13) 3_656 ? P1 C1 1.807(3) . ? P1 K1 3.1376(11) 3_656 ? C1 C2 1.416(4) . ? C1 C6 1.417(4) . ? C2 C3 1.392(4) . ? C2 C7 1.506(4) . ? C3 C4 1.373(4) . ? C4 C5 1.377(4) . ? C5 C6 1.394(4) . ? C6 C22 1.499(4) . ? C7 C12 1.404(4) . ? C7 C8 1.406(4) . ? C8 C9 1.399(4) . ? C8 C13 1.518(4) . ? C9 C10 1.385(4) . ? C10 C11 1.373(4) . ? C10 C16 1.523(4) . ? C11 C12 1.388(4) . ? C12 C19 1.514(4) . ? C13 C15 1.513(9) . ? C13 C14 1.523(9) . ? C16 C18 1.485(5) . ? C16 C17 1.492(6) . ? C19 C21 1.519(5) . ? C19 C20 1.529(4) . ? C22 C27 1.405(4) . ? C22 C23 1.408(4) . ? C22 K1 3.418(3) 3_656 ? C23 C24 1.392(4) . ? C23 C28 1.514(4) . ? C23 K1 3.340(3) 3_656 ? C24 C25 1.386(5) . ? C24 K1 3.239(3) 3_656 ? C25 C26 1.381(5) . ? C25 C31 1.532(5) . ? C25 K1 3.230(4) 3_656 ? C26 C27 1.392(4) . ? C26 K1 3.259(3) 3_656 ? C27 C34 1.514(5) . ? C27 K1 3.366(3) 3_656 ? C28 C30 1.514(5) . ? C28 C29 1.534(5) . ? C31 C33 1.474(6) . ? C31 C32 1.552(7) . ? C34 C36 1.522(5) . ? C34 C35 1.524(5) . ? O1 C40 1.407(5) . ? O1 C37 1.430(4) . ? C37 C38 1.482(5) . ? C38 C39 1.469(5) . ? C39 C40 1.477(9) . ? C39A C40A 1.446(9) . ? C37B C38B 1.494(11) . ? C38B C39B 1.498(10) . ? C39B C40B 1.496(10) . ? 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 K1 P1 121.76(7) . 3_656 ? O1 K1 C25 100.84(9) . 3_656 ? P1 K1 C25 105.15(6) 3_656 3_656 ? O1 K1 C24 88.44(9) . 3_656 ? P1 K1 C24 94.25(6) 3_656 3_656 ? C25 K1 C24 24.75(9) 3_656 3_656 ? O1 K1 P1 123.40(6) . . ? P1 K1 P1 87.16(3) 3_656 . ? C25 K1 P1 118.22(7) 3_656 . ? C24 K1 P1 141.12(7) 3_656 . ? O1 K1 C26 125.40(9) . 3_656 ? P1 K1 C26 90.38(6) 3_656 3_656 ? C25 K1 C26 24.58(9) 3_656 3_656 ? C24 K1 C26 42.60(9) 3_656 3_656 ? P1 K1 C26 98.61(7) . 3_656 ? O1 K1 C23 98.04(8) . 3_656 ? P1 K1 C23 70.13(5) 3_656 3_656 ? C25 K1 C23 43.46(8) 3_656 3_656 ? C24 K1 C23 24.38(7) 3_656 3_656 ? P1 K1 C23 138.54(6) . 3_656 ? C26 K1 C23 49.43(8) 3_656 3_656 ? O1 K1 C27 137.93(8) . 3_656 ? P1 K1 C27 66.20(5) 3_656 3_656 ? C25 K1 C27 43.39(8) 3_656 3_656 ? C24 K1 C27 49.70(8) 3_656 3_656 ? P1 K1 C27 97.01(6) . 3_656 ? C26 K1 C27 24.18(8) 3_656 3_656 ? C23 K1 C27 42.45(7) 3_656 3_656 ? O1 K1 C22 121.47(8) . 3_656 ? P1 K1 C22 55.18(5) 3_656 3_656 ? C25 K1 C22 50.18(7) 3_656 3_656 ? C24 K1 C22 42.47(8) 3_656 3_656 ? P1 K1 C22 115.01(6) . 3_656 ? C26 K1 C22 42.13(7) 3_656 3_656 ? C23 K1 C22 24.01(7) 3_656 3_656 ? C27 K1 C22 23.89(7) 3_656 3_656 ? O1 K1 K1 138.02(6) . 3_656 ? P1 K1 K1 44.494(19) 3_656 3_656 ? C25 K1 K1 120.61(7) 3_656 3_656 ? C24 K1 K1 126.62(6) 3_656 3_656 ? P1 K1 K1 42.667(18) . 3_656 ? C26 K1 K1 96.29(7) 3_656 3_656 ? C23 K1 K1 107.17(6) 3_656 3_656 ? C27 K1 K1 79.15(6) 3_656 3_656 ? C22 K1 K1 84.79(5) 3_656 3_656 ? C1 P1 K1 121.73(9) . 3_656 ? C1 P1 K1 126.80(9) . . ? K1 P1 K1 92.84(3) 3_656 . ? C2 C1 C6 117.2(2) . . ? C2 C1 P1 125.5(2) . . ? C6 C1 P1 117.3(2) . . ? C3 C2 C1 119.9(2) . . ? C3 C2 C7 118.6(2) . . ? C1 C2 C7 121.4(2) . . ? C4 C3 C2 122.0(3) . . ? C3 C4 C5 118.9(3) . . ? C4 C5 C6 121.0(3) . . ? C5 C6 C1 120.7(3) . . ? C5 C6 C22 118.0(2) . . ? C1 C6 C22 120.8(2) . . ? C12 C7 C8 119.6(2) . . ? C12 C7 C2 120.2(2) . . ? C8 C7 C2 120.2(2) . . ? C9 C8 C7 118.3(3) . . ? C9 C8 C13 120.1(3) . . ? C7 C8 C13 121.7(2) . . ? C10 C9 C8 122.7(3) . . ? C11 C10 C9 117.6(3) . . ? C11 C10 C16 120.4(3) . . ? C9 C10 C16 122.0(3) . . ? C10 C11 C12 122.6(3) . . ? C11 C12 C7 119.3(3) . . ? C11 C12 C19 118.7(3) . . ? C7 C12 C19 122.0(2) . . ? C15 C13 C8 113.5(7) . . ? C15 C13 C14 115.4(11) . . ? C8 C13 C14 107.9(6) . . ? C18 C16 C17 112.5(3) . . ? C18 C16 C10 113.2(3) . . ? C17 C16 C10 111.7(3) . . ? C12 C19 C21 110.8(3) . . ? C12 C19 C20 113.0(3) . . ? C21 C19 C20 109.9(3) . . ? C27 C22 C23 119.3(3) . . ? C27 C22 C6 122.4(3) . . ? C23 C22 C6 118.2(2) . . ? C27 C22 K1 75.98(15) . 3_656 ? C23 C22 K1 74.88(15) . 3_656 ? C6 C22 K1 121.85(16) . 3_656 ? C24 C23 C22 119.3(3) . . ? C24 C23 C28 119.3(3) . . ? C22 C23 C28 121.3(3) . . ? C24 C23 K1 73.73(17) . 3_656 ? C22 C23 K1 81.11(16) . 3_656 ? C28 C23 K1 117.25(18) . 3_656 ? C25 C24 C23 122.4(3) . . ? C25 C24 K1 77.3(2) . 3_656 ? C23 C24 K1 81.89(17) . 3_656 ? C26 C25 C24 117.0(3) . . ? C26 C25 C31 120.4(3) . . ? C24 C25 C31 122.6(4) . . ? C26 C25 K1 78.9(2) . 3_656 ? C24 C25 K1 77.99(18) . 3_656 ? C31 C25 K1 111.8(2) . 3_656 ? C25 C26 C27 123.4(3) . . ? C25 C26 K1 76.54(19) . 3_656 ? C27 C26 K1 82.25(17) . 3_656 ? C26 C27 C22 118.5(3) . . ? C26 C27 C34 121.2(3) . . ? C22 C27 C34 120.2(3) . . ? C26 C27 K1 73.57(17) . 3_656 ? C22 C27 K1 80.13(16) . 3_656 ? C34 C27 K1 118.31(19) . 3_656 ? C23 C28 C30 111.8(3) . . ? C23 C28 C29 111.0(3) . . ? C30 C28 C29 112.0(3) . . ? C33 C31 C25 111.1(4) . . ? C33 C31 C32 109.6(4) . . ? C25 C31 C32 113.5(4) . . ? C27 C34 C36 112.8(3) . . ? C27 C34 C35 110.5(3) . . ? C36 C34 C35 109.9(3) . . ? C40 O1 C37 109.3(4) . . ? C40 O1 K1 121.9(4) . . ? C37 O1 K1 128.4(2) . . ? O1 C37 C38 106.5(4) . . ? C39 C38 C37 106.5(5) . . ? C38 C39 C40 105.0(7) . . ? O1 C40 C39 109.1(6) . . ? C37B C38B C39B 109(2) . . ? C40B C39B C38B 95(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.615 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.053 #===END data_5a _database_code_depnum_ccdc_archive 'CCDC 646374' _refine_special_details ; One iPr group rotationally disordered over 2 sites, occupancies 0.66:0.34. This and two further iPr groups refined with geometry restraints. Other iPr have elongated adps but no reasonable model found and left as anisotropic model. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C73 H107 I N2 O2 P Y' _chemical_formula_sum 'C73 H107 I N2 O2 P Y' _chemical_formula_weight 1291.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 10.1103(6) _cell_length_b 12.5075(7) _cell_length_c 29.0482(16) _cell_angle_alpha 95.484(2) _cell_angle_beta 91.431(2) _cell_angle_gamma 102.875(2) _cell_volume 3560.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7365 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 24.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 1.317 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6485 _exptl_absorpt_correction_T_max 0.7604 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25883 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12463 _reflns_number_gt 9332 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0693P)^2^+2.5681P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, PH and Me from difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12463 _refine_ls_number_parameters 768 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.042 _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 Y1 Y 0.98476(3) 0.30974(3) 0.363406(12) 0.03168(11) Uani 1 1 d . . . I1 I 1.08591(3) 0.29967(3) 0.459701(10) 0.06076(12) Uani 1 1 d . . . C1 C 0.7092(4) 0.0769(3) 0.10719(13) 0.0364(9) Uani 1 1 d . . . C2 C 0.6288(4) -0.0310(3) 0.10296(13) 0.0373(9) Uani 1 1 d . . . C3 C 0.5911(4) -0.0863(3) 0.05898(14) 0.0417(10) Uani 1 1 d . . . H3A H 0.5383 -0.1599 0.0560 0.050 Uiso 1 1 calc R . . C4 C 0.6296(4) -0.0358(3) 0.01990(14) 0.0406(9) Uani 1 1 d . . . H4A H 0.6034 -0.0744 -0.0099 0.049 Uiso 1 1 calc R . . C5 C 0.7062(4) 0.0711(3) 0.02389(13) 0.0382(9) Uani 1 1 d . . . H5A H 0.7311 0.1058 -0.0033 0.046 Uiso 1 1 calc R . . C6 C 0.7475(4) 0.1287(3) 0.06690(13) 0.0351(8) Uani 1 1 d . . . C7 C 0.5815(4) -0.0922(3) 0.14341(13) 0.0375(9) Uani 1 1 d . . . C8 C 0.6574(4) -0.1620(4) 0.16104(17) 0.0524(11) Uani 1 1 d . . . C9 C 0.6057(5) -0.2266(4) 0.19518(17) 0.0565(12) Uani 1 1 d . . . H9A H 0.6563 -0.2748 0.2066 0.068 Uiso 1 1 calc R . . C10 C 0.4832(5) -0.2223(3) 0.21281(15) 0.0566(12) Uani 1 1 d D . . C11 C 0.4119(4) -0.1515(3) 0.19740(15) 0.0482(11) Uani 1 1 d . . . H11A H 0.3284 -0.1470 0.2108 0.058 Uiso 1 1 calc R . . C12 C 0.4578(4) -0.0855(3) 0.16253(13) 0.0374(9) Uani 1 1 d . . . C13 C 0.7952(6) -0.1683(5) 0.1430(2) 0.099(2) Uani 1 1 d D . . H13A H 0.8231 -0.1071 0.1230 0.118 Uiso 1 1 calc R . . C14 C 0.9027(7) -0.1497(8) 0.1840(3) 0.160(5) Uani 1 1 d D . . H14A H 0.9913 -0.1539 0.1720 0.240 Uiso 1 1 calc R . . H14B H 0.8755 -0.2067 0.2050 0.240 Uiso 1 1 calc R . . H14C H 0.9089 -0.0769 0.2008 0.240 Uiso 1 1 calc R . . C15 C 0.7816(10) -0.2758(6) 0.1129(3) 0.208(7) Uani 1 1 d D . . H15A H 0.7154 -0.2798 0.0872 0.312 Uiso 1 1 calc R . . H15B H 0.7505 -0.3375 0.1314 0.312 Uiso 1 1 calc R . . H15C H 0.8699 -0.2800 0.1006 0.312 Uiso 1 1 calc R . . C16 C 0.4122(8) -0.2983(4) 0.24653(17) 0.114(3) Uani 1 1 d D . . H16A H 0.3148 -0.3090 0.2360 0.137 Uiso 1 1 calc R . . C17 C 0.4305(6) -0.4158(4) 0.2416(2) 0.092(2) Uani 1 1 d D . . H17A H 0.4014 -0.4500 0.2102 0.138 Uiso 1 1 calc R . . H17B H 0.3756 -0.4578 0.2640 0.138 Uiso 1 1 calc R . . H17C H 0.5265 -0.4155 0.2475 0.138 Uiso 1 1 calc R . . C18 C 0.4124(9) -0.2447(5) 0.29555(18) 0.140(4) Uani 1 1 d D . . H18A H 0.3946 -0.1710 0.2948 0.210 Uiso 1 1 calc R . . H18B H 0.5011 -0.2386 0.3112 0.210 Uiso 1 1 calc R . . H18C H 0.3416 -0.2898 0.3124 0.210 Uiso 1 1 calc R . . C19 C 0.3710(4) -0.0119(3) 0.14541(14) 0.0433(10) Uani 1 1 d . . . H19A H 0.4258 0.0343 0.1233 0.052 Uiso 1 1 calc R . . C20 C 0.3367(7) 0.0664(5) 0.18381(19) 0.0863(19) Uani 1 1 d . . . H20A H 0.4204 0.1071 0.2009 0.129 Uiso 1 1 calc R . . H20B H 0.2765 0.0244 0.2049 0.129 Uiso 1 1 calc R . . H20C H 0.2911 0.1185 0.1705 0.129 Uiso 1 1 calc R . . C21 C 0.2441(5) -0.0807(5) 0.1181(2) 0.0803(17) Uani 1 1 d . . . H21A H 0.2712 -0.1244 0.0917 0.120 Uiso 1 1 calc R . . H21B H 0.1901 -0.0316 0.1069 0.120 Uiso 1 1 calc R . . H21C H 0.1897 -0.1301 0.1383 0.120 Uiso 1 1 calc R . . C22 C 0.8328(4) 0.2435(3) 0.06982(12) 0.0339(8) Uani 1 1 d . . . C23 C 0.9714(4) 0.2618(3) 0.06236(12) 0.0351(8) Uani 1 1 d . . . C24 C 1.0500(4) 0.3696(3) 0.06784(13) 0.0388(9) Uani 1 1 d . . . H24A H 1.1442 0.3816 0.0625 0.047 Uiso 1 1 calc R . . C25 C 0.9964(4) 0.4586(3) 0.08067(15) 0.0443(10) Uani 1 1 d . . . C26 C 0.8580(4) 0.4390(3) 0.08690(17) 0.0524(11) Uani 1 1 d . . . H26A H 0.8191 0.4999 0.0956 0.063 Uiso 1 1 calc R . . C27 C 0.7739(4) 0.3343(3) 0.08100(15) 0.0431(10) Uani 1 1 d . . . C28 C 1.0393(4) 0.1680(3) 0.04683(14) 0.0423(10) Uani 1 1 d . . . H28A H 0.9789 0.0975 0.0543 0.051 Uiso 1 1 calc R . . C29 C 1.1786(5) 0.1791(4) 0.07130(17) 0.0578(12) Uani 1 1 d . . . H29A H 1.1703 0.1894 0.1049 0.087 Uiso 1 1 calc R . . H29B H 1.2428 0.2428 0.0615 0.087 Uiso 1 1 calc R . . H29C H 1.2116 0.1121 0.0631 0.087 Uiso 1 1 calc R . . C30 C 1.0547(5) 0.1601(4) -0.00549(16) 0.0594(13) Uani 1 1 d . . . H30A H 0.9649 0.1461 -0.0213 0.089 Uiso 1 1 calc R . . H30B H 1.0985 0.0995 -0.0148 0.089 Uiso 1 1 calc R . . H30C H 1.1107 0.2295 -0.0138 0.089 Uiso 1 1 calc R . . C31 C 1.0866(5) 0.5738(3) 0.08906(18) 0.0555(12) Uani 1 1 d . . . H31A H 1.0265 0.6262 0.0962 0.067 Uiso 1 1 calc R . . C32 C 1.1627(9) 0.6075(5) 0.0470(2) 0.116(3) Uani 1 1 d . . . H32A H 1.2189 0.6824 0.0538 0.174 Uiso 1 1 calc R . . H32B H 1.0978 0.6058 0.0212 0.174 Uiso 1 1 calc R . . H32C H 1.2209 0.5563 0.0387 0.174 Uiso 1 1 calc R . . C33 C 1.1819(9) 0.5832(6) 0.1302(2) 0.130(3) Uani 1 1 d . . . H33A H 1.1297 0.5654 0.1575 0.194 Uiso 1 1 calc R . . H33B H 1.2373 0.6586 0.1356 0.194 Uiso 1 1 calc R . . H33C H 1.2412 0.5316 0.1245 0.194 Uiso 1 1 calc R . . C34 C 0.6202(4) 0.3190(4) 0.08348(17) 0.0543(12) Uani 1 1 d . . . H34A H 0.5813 0.2389 0.0855 0.065 Uiso 1 1 calc R . . C35 C 0.5767(5) 0.3832(5) 0.1263(2) 0.0745(16) Uani 1 1 d . . . H35A H 0.6218 0.3672 0.1543 0.112 Uiso 1 1 calc R . . H35B H 0.4780 0.3607 0.1285 0.112 Uiso 1 1 calc R . . H35C H 0.6026 0.4625 0.1234 0.112 Uiso 1 1 calc R . . C36 C 0.5626(5) 0.3484(5) 0.0395(2) 0.0771(16) Uani 1 1 d . . . H36A H 0.5868 0.3030 0.0130 0.116 Uiso 1 1 calc R . . H36B H 0.5998 0.4265 0.0362 0.116 Uiso 1 1 calc R . . H36C H 0.4635 0.3349 0.0405 0.116 Uiso 1 1 calc R . . P1 P 0.74976(12) 0.15304(10) 0.16548(4) 0.0460(3) Uani 1 1 d . . . H1P H 0.764(6) 0.078(5) 0.185(2) 0.103(19) Uiso 1 1 d . . . C37 C 0.9358(6) 0.2054(6) 0.17089(19) 0.0811(17) Uani 1 1 d . . . H37A H 0.9793 0.1528 0.1527 0.097 Uiso 1 1 calc R . . H37B H 0.9594 0.2766 0.1574 0.097 Uiso 1 1 calc R . . C38 C 0.9921(5) 0.2218(5) 0.21969(15) 0.0643(14) Uani 1 1 d . . . H38A H 0.9277 0.2515 0.2396 0.077 Uiso 1 1 calc R . . H38B H 0.9957 0.1487 0.2294 0.077 Uiso 1 1 calc R . . C39 C 1.1247(5) 0.2936(5) 0.22868(19) 0.0720(15) Uani 1 1 d . . . H39A H 1.1172 0.3695 0.2241 0.086 Uiso 1 1 calc R . . H39B H 1.1852 0.2717 0.2050 0.086 Uiso 1 1 calc R . . C40 C 1.1901(5) 0.2966(4) 0.27367(17) 0.0611(13) Uani 1 1 d . . . H40A H 1.2223 0.2278 0.2750 0.073 Uiso 1 1 calc R . . H40B H 1.2708 0.3588 0.2772 0.073 Uiso 1 1 calc R . . O1 O 1.1081(3) 0.3080(2) 0.31080(9) 0.0419(6) Uani 1 1 d . . . O2 O 1.0851(3) 0.5002(2) 0.38132(10) 0.0453(7) Uani 1 1 d . . . C41 C 1.0522(5) 0.5817(4) 0.41593(18) 0.0629(13) Uani 1 1 d . . . H41A H 1.0412 0.5533 0.4466 0.075 Uiso 1 1 calc R . . H41B H 0.9685 0.6042 0.4066 0.075 Uiso 1 1 calc R . . C42 C 1.1755(7) 0.6754(4) 0.4163(2) 0.095(2) Uani 1 1 d . . . H42A H 1.1644 0.7234 0.3919 0.115 Uiso 1 1 calc R . . H42B H 1.1889 0.7205 0.4467 0.115 Uiso 1 1 calc R . . C43 C 1.2893(7) 0.6266(6) 0.4077(2) 0.090(2) Uani 1 1 d . . . H43A H 1.3267 0.6070 0.4367 0.108 Uiso 1 1 calc R . . H43B H 1.3621 0.6772 0.3931 0.108 Uiso 1 1 calc R . . C44 C 1.2315(4) 0.5271(4) 0.37583(19) 0.0621(13) Uani 1 1 d . . . H44A H 1.2513 0.5413 0.3435 0.075 Uiso 1 1 calc R . . H44B H 1.2714 0.4651 0.3834 0.075 Uiso 1 1 calc R . . C45 C 0.5751(4) 0.3049(4) 0.28319(18) 0.0590(12) Uani 1 1 d . . . H45A H 0.5944 0.3855 0.2850 0.088 Uiso 1 1 calc R . . H45B H 0.4917 0.2780 0.2991 0.088 Uiso 1 1 calc R . . H45C H 0.5633 0.2740 0.2507 0.088 Uiso 1 1 calc R . . C46 C 0.6914(4) 0.2697(3) 0.30593(13) 0.0364(9) Uani 1 1 d . . . C47 C 0.6942(4) 0.1586(3) 0.29569(13) 0.0368(9) Uani 1 1 d . . . H47A H 0.6407 0.1225 0.2690 0.044 Uiso 1 1 calc R . . C48 C 0.7634(4) 0.0917(3) 0.31857(12) 0.0346(8) Uani 1 1 d . . . C49 C 0.7240(5) -0.0298(3) 0.30232(15) 0.0505(11) Uani 1 1 d . . . H49A H 0.8061 -0.0577 0.2970 0.076 Uiso 1 1 calc R . . H49B H 0.6683 -0.0412 0.2734 0.076 Uiso 1 1 calc R . . H49C H 0.6718 -0.0693 0.3260 0.076 Uiso 1 1 calc R . . N1 N 0.7819(3) 0.3408(2) 0.33453(10) 0.0321(7) Uani 1 1 d . . . C50 C 0.7608(4) 0.4502(3) 0.34495(14) 0.0395(9) Uani 1 1 d . A . C51 C 0.6935(4) 0.4743(4) 0.38504(15) 0.0476(10) Uani 1 1 d . . . C52 C 0.6800(5) 0.5818(4) 0.39594(18) 0.0634(13) Uani 1 1 d . A . H52A H 0.6335 0.5991 0.4227 0.076 Uiso 1 1 calc R . . C53 C 0.7333(6) 0.6641(4) 0.3684(2) 0.0706(15) Uani 1 1 d . . . H53A H 0.7228 0.7372 0.3763 0.085 Uiso 1 1 calc R A . C54 C 0.8007(5) 0.6406(4) 0.32982(19) 0.0632(13) Uani 1 1 d . A . H54A H 0.8370 0.6980 0.3114 0.076 Uiso 1 1 calc R . . C55 C 0.8173(4) 0.5343(3) 0.31709(15) 0.0477(10) Uani 1 1 d . . . C56 C 0.6379(4) 0.3871(4) 0.41627(14) 0.0541(11) Uani 0.66(2) 1 d PD A 1 H56 H 0.6566 0.3161 0.4023 0.065 Uiso 0.66(2) 1 calc PR A 1 C57 C 0.7038(14) 0.4106(12) 0.4648(3) 0.086(4) Uani 0.66(2) 1 d PD A 1 H57A H 0.8026 0.4219 0.4630 0.129 Uiso 0.66(2) 1 calc PR A 1 H57B H 0.6698 0.3480 0.4825 0.129 Uiso 0.66(2) 1 calc PR A 1 H57C H 0.6817 0.4772 0.4803 0.129 Uiso 0.66(2) 1 calc PR A 1 C58 C 0.4824(7) 0.3699(12) 0.4196(5) 0.092(4) Uani 0.66(2) 1 d PD A 1 H58A H 0.4477 0.3048 0.4357 0.138 Uiso 0.66(2) 1 calc PR A 1 H58B H 0.4394 0.3592 0.3884 0.138 Uiso 0.66(2) 1 calc PR A 1 H58C H 0.4614 0.4349 0.4368 0.138 Uiso 0.66(2) 1 calc PR A 1 C56A C 0.6379(4) 0.3871(4) 0.41627(14) 0.0541(11) Uani 0.34(2) 1 d P A 2 H56A H 0.7060 0.3402 0.4169 0.065 Uiso 0.34(2) 1 calc PR A 2 C57A C 0.628(3) 0.430(2) 0.4665(5) 0.097(10) Uani 0.34(2) 1 d PD A 2 H57D H 0.6933 0.5010 0.4737 0.146 Uiso 0.34(2) 1 calc PR A 2 H57E H 0.6475 0.3772 0.4869 0.146 Uiso 0.34(2) 1 calc PR A 2 H57F H 0.5356 0.4409 0.4714 0.146 Uiso 0.34(2) 1 calc PR A 2 C58A C 0.5069(15) 0.3099(16) 0.3980(6) 0.064(6) Uani 0.34(2) 1 d PD A 2 H58D H 0.5192 0.2759 0.3671 0.096 Uiso 0.34(2) 1 calc PR A 2 H58E H 0.4355 0.3512 0.3963 0.096 Uiso 0.34(2) 1 calc PR A 2 H58F H 0.4808 0.2523 0.4188 0.096 Uiso 0.34(2) 1 calc PR A 2 C59 C 0.8954(5) 0.5123(4) 0.27482(17) 0.0575(12) Uani 1 1 d . A . H59A H 0.9163 0.4382 0.2761 0.069 Uiso 1 1 calc R . . C60 C 1.0278(5) 0.5938(5) 0.2731(2) 0.0817(18) Uani 1 1 d . . . H60A H 1.0825 0.5964 0.3017 0.123 Uiso 1 1 calc R A . H60B H 1.0109 0.6670 0.2699 0.123 Uiso 1 1 calc R . . H60C H 1.0769 0.5714 0.2465 0.123 Uiso 1 1 calc R . . C61 C 0.8149(7) 0.5082(7) 0.2301(2) 0.122(3) Uani 1 1 d . . . H61A H 0.7373 0.4447 0.2277 0.183 Uiso 1 1 calc R A . H61B H 0.8730 0.5011 0.2040 0.183 Uiso 1 1 calc R . . H61C H 0.7821 0.5761 0.2295 0.183 Uiso 1 1 calc R . . N2 N 0.8564(3) 0.1286(2) 0.35334(10) 0.0340(7) Uani 1 1 d . . . C62 C 0.8923(4) 0.0485(3) 0.38135(13) 0.0402(9) Uani 1 1 d . . . C63 C 0.8072(5) 0.0135(3) 0.41744(14) 0.0477(11) Uani 1 1 d . . . C64 C 0.8479(6) -0.0557(4) 0.44677(16) 0.0650(15) Uani 1 1 d . . . H64A H 0.7917 -0.0799 0.4712 0.078 Uiso 1 1 calc R . . C65 C 0.9666(7) -0.0902(4) 0.44163(18) 0.0733(16) Uani 1 1 d . . . H65A H 0.9929 -0.1362 0.4627 0.088 Uiso 1 1 calc R . . C66 C 1.0474(5) -0.0579(4) 0.40581(17) 0.0619(13) Uani 1 1 d . . . H66A H 1.1289 -0.0829 0.4021 0.074 Uiso 1 1 calc R . . C67 C 1.0120(4) 0.0116(3) 0.37449(15) 0.0469(10) Uani 1 1 d . . . C68 C 0.6760(5) 0.0502(4) 0.42525(15) 0.0602(13) Uani 1 1 d . . . H68A H 0.6659 0.1011 0.4015 0.072 Uiso 1 1 calc R . . C69 C 0.6783(6) 0.1131(5) 0.4727(2) 0.091(2) Uani 1 1 d . . . H69A H 0.7551 0.1773 0.4759 0.136 Uiso 1 1 calc R . . H69B H 0.6880 0.0648 0.4967 0.136 Uiso 1 1 calc R . . H69C H 0.5934 0.1378 0.4763 0.136 Uiso 1 1 calc R . . C70 C 0.5512(6) -0.0466(5) 0.4197(2) 0.0880(19) Uani 1 1 d . . . H70A H 0.5435 -0.0825 0.3879 0.132 Uiso 1 1 calc R . . H70B H 0.4693 -0.0192 0.4262 0.132 Uiso 1 1 calc R . . H70C H 0.5612 -0.0999 0.4414 0.132 Uiso 1 1 calc R . . C71 C 1.1030(4) 0.0409(4) 0.33518(17) 0.0543(12) Uani 1 1 d . . . H71A H 1.0653 0.0929 0.3174 0.065 Uiso 1 1 calc R . . C72 C 1.2464(5) 0.0987(5) 0.3528(3) 0.0884(19) Uani 1 1 d . . . H72A H 1.2438 0.1662 0.3726 0.133 Uiso 1 1 calc R . . H72B H 1.3027 0.1174 0.3265 0.133 Uiso 1 1 calc R . . H72C H 1.2850 0.0496 0.3708 0.133 Uiso 1 1 calc R . . C73 C 1.1052(6) -0.0617(4) 0.3022(2) 0.0768(16) Uani 1 1 d . . . H73A H 1.0119 -0.0995 0.2920 0.115 Uiso 1 1 calc R . . H73B H 1.1481 -0.1115 0.3183 0.115 Uiso 1 1 calc R . . H73C H 1.1568 -0.0397 0.2752 0.115 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 Y1 0.03101(19) 0.0298(2) 0.0318(2) 0.00629(15) 0.00133(14) 0.00032(15) I1 0.0813(2) 0.0517(2) 0.03858(17) 0.01355(13) -0.01479(14) -0.00958(16) C1 0.041(2) 0.032(2) 0.034(2) -0.0004(16) 0.0133(16) 0.0023(17) C2 0.041(2) 0.029(2) 0.041(2) 0.0024(17) 0.0149(17) 0.0046(17) C3 0.042(2) 0.027(2) 0.053(2) -0.0011(18) 0.0148(19) 0.0017(17) C4 0.039(2) 0.037(2) 0.039(2) -0.0096(18) 0.0106(17) 0.0014(18) C5 0.039(2) 0.040(2) 0.033(2) 0.0036(17) 0.0123(16) 0.0036(17) C6 0.037(2) 0.029(2) 0.038(2) 0.0010(16) 0.0111(16) 0.0049(16) C7 0.039(2) 0.027(2) 0.042(2) 0.0053(16) 0.0109(17) -0.0028(16) C8 0.049(3) 0.039(2) 0.072(3) 0.018(2) 0.020(2) 0.010(2) C9 0.061(3) 0.042(3) 0.073(3) 0.021(2) 0.013(2) 0.017(2) C10 0.081(3) 0.042(3) 0.049(3) 0.012(2) 0.022(2) 0.012(2) C11 0.051(3) 0.042(2) 0.051(3) 0.007(2) 0.021(2) 0.006(2) C12 0.044(2) 0.027(2) 0.036(2) -0.0018(16) 0.0078(17) 0.0001(17) C13 0.071(4) 0.101(5) 0.153(6) 0.081(5) 0.061(4) 0.047(4) C14 0.059(4) 0.204(10) 0.249(12) 0.142(9) 0.027(6) 0.043(5) C15 0.301(13) 0.114(6) 0.290(13) 0.121(8) 0.259(12) 0.148(8) C16 0.190(8) 0.082(4) 0.093(5) 0.052(4) 0.084(5) 0.053(5) C17 0.091(4) 0.070(4) 0.111(5) 0.042(4) 0.026(4) -0.006(3) C18 0.204(9) 0.101(5) 0.070(4) 0.016(4) 0.038(5) -0.067(6) C19 0.044(2) 0.041(2) 0.044(2) 0.0068(19) 0.0109(18) 0.0052(19) C20 0.137(6) 0.083(4) 0.059(3) 0.004(3) 0.013(3) 0.068(4) C21 0.066(3) 0.066(4) 0.105(5) 0.015(3) -0.019(3) 0.007(3) C22 0.038(2) 0.030(2) 0.0294(19) 0.0007(15) 0.0081(16) -0.0002(16) C23 0.042(2) 0.032(2) 0.0302(19) 0.0047(16) 0.0076(16) 0.0054(17) C24 0.038(2) 0.034(2) 0.041(2) 0.0058(17) 0.0109(17) 0.0004(17) C25 0.040(2) 0.032(2) 0.056(3) 0.0004(19) 0.0073(19) 0.0001(18) C26 0.049(3) 0.030(2) 0.076(3) -0.006(2) 0.008(2) 0.0079(19) C27 0.040(2) 0.035(2) 0.052(2) -0.0002(19) 0.0093(19) 0.0051(18) C28 0.044(2) 0.029(2) 0.052(2) 0.0041(18) 0.0159(19) 0.0032(17) C29 0.057(3) 0.058(3) 0.065(3) 0.009(2) 0.011(2) 0.023(2) C30 0.057(3) 0.062(3) 0.057(3) -0.011(2) 0.016(2) 0.014(2) C31 0.050(3) 0.028(2) 0.082(3) -0.002(2) 0.007(2) -0.0013(19) C32 0.188(8) 0.047(3) 0.078(4) 0.018(3) -0.003(5) -0.050(4) C33 0.184(8) 0.075(4) 0.086(5) 0.001(4) -0.048(5) -0.057(5) C34 0.044(2) 0.042(3) 0.075(3) -0.003(2) 0.012(2) 0.008(2) C35 0.047(3) 0.077(4) 0.095(4) -0.021(3) 0.018(3) 0.015(3) C36 0.045(3) 0.082(4) 0.097(4) 0.005(3) 0.003(3) 0.002(3) P1 0.0538(7) 0.0449(6) 0.0322(5) 0.0002(5) 0.0107(5) -0.0032(5) C37 0.071(4) 0.105(5) 0.058(3) -0.008(3) 0.010(3) 0.008(3) C38 0.072(3) 0.077(4) 0.037(2) 0.002(2) 0.012(2) 0.001(3) C39 0.070(3) 0.090(4) 0.065(3) 0.021(3) 0.031(3) 0.028(3) C40 0.053(3) 0.059(3) 0.068(3) 0.007(2) 0.028(2) 0.003(2) O1 0.0408(15) 0.0401(16) 0.0448(16) 0.0112(12) 0.0154(12) 0.0049(12) O2 0.0485(16) 0.0357(15) 0.0478(16) 0.0070(13) -0.0009(13) 0.0003(13) C41 0.078(3) 0.042(3) 0.063(3) -0.015(2) -0.012(3) 0.012(2) C42 0.131(6) 0.037(3) 0.103(5) -0.010(3) -0.061(4) 0.002(3) C43 0.082(4) 0.103(5) 0.060(3) 0.002(3) 0.003(3) -0.030(4) C44 0.047(3) 0.051(3) 0.081(3) 0.021(3) -0.003(2) -0.013(2) C45 0.044(3) 0.054(3) 0.076(3) -0.001(2) -0.019(2) 0.010(2) C46 0.033(2) 0.039(2) 0.036(2) 0.0018(17) 0.0061(16) 0.0053(17) C47 0.034(2) 0.042(2) 0.0293(19) -0.0014(17) 0.0033(15) -0.0001(17) C48 0.036(2) 0.033(2) 0.032(2) 0.0049(16) 0.0123(16) -0.0004(16) C49 0.063(3) 0.035(2) 0.045(2) -0.0004(19) -0.001(2) -0.003(2) N1 0.0311(16) 0.0315(17) 0.0324(16) 0.0028(13) 0.0035(13) 0.0044(13) C50 0.031(2) 0.038(2) 0.047(2) -0.0018(18) -0.0042(17) 0.0064(17) C51 0.042(2) 0.051(3) 0.049(3) -0.009(2) -0.0011(19) 0.016(2) C52 0.066(3) 0.062(3) 0.063(3) -0.016(3) 0.001(2) 0.025(3) C53 0.080(4) 0.048(3) 0.088(4) -0.012(3) -0.001(3) 0.030(3) C54 0.071(3) 0.041(3) 0.080(4) 0.006(2) 0.001(3) 0.019(2) C55 0.050(2) 0.039(2) 0.056(3) 0.005(2) 0.000(2) 0.013(2) C56 0.053(3) 0.061(3) 0.046(3) -0.007(2) 0.011(2) 0.013(2) C57 0.085(9) 0.105(8) 0.054(5) 0.018(5) -0.006(5) -0.011(8) C58 0.058(6) 0.103(9) 0.108(10) 0.006(8) 0.013(5) 0.003(5) C56A 0.053(3) 0.061(3) 0.046(3) -0.007(2) 0.011(2) 0.013(2) C57A 0.084(17) 0.12(2) 0.058(11) -0.026(12) -0.009(11) -0.027(17) C58A 0.055(10) 0.070(13) 0.058(10) -0.009(8) 0.015(7) -0.003(8) C59 0.075(3) 0.040(3) 0.063(3) 0.018(2) 0.020(3) 0.017(2) C60 0.056(3) 0.115(5) 0.066(3) 0.023(3) 0.002(3) -0.004(3) C61 0.072(4) 0.194(8) 0.067(4) -0.019(5) 0.009(3) -0.027(5) N2 0.0355(17) 0.0351(17) 0.0294(16) 0.0055(13) 0.0046(13) 0.0023(14) C62 0.054(2) 0.026(2) 0.034(2) 0.0074(16) -0.0005(18) -0.0053(18) C63 0.066(3) 0.035(2) 0.035(2) 0.0072(18) 0.006(2) -0.005(2) C64 0.104(4) 0.047(3) 0.036(2) 0.017(2) 0.004(3) -0.004(3) C65 0.111(5) 0.051(3) 0.057(3) 0.027(3) -0.013(3) 0.009(3) C66 0.077(3) 0.047(3) 0.065(3) 0.023(2) -0.007(3) 0.016(2) C67 0.053(3) 0.032(2) 0.056(3) 0.0117(19) -0.002(2) 0.0058(19) C68 0.085(4) 0.052(3) 0.040(2) 0.011(2) 0.027(2) 0.003(3) C69 0.092(4) 0.092(4) 0.070(4) -0.019(3) 0.034(3) -0.010(3) C70 0.076(4) 0.099(5) 0.072(4) -0.008(3) 0.015(3) -0.009(3) C71 0.050(3) 0.046(3) 0.075(3) 0.027(2) 0.013(2) 0.019(2) C72 0.055(3) 0.071(4) 0.143(6) 0.036(4) 0.008(3) 0.011(3) C73 0.088(4) 0.066(4) 0.086(4) 0.020(3) 0.032(3) 0.029(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 Y1 O1 1.998(3) . ? Y1 N1 2.323(3) . ? Y1 N2 2.334(3) . ? Y1 O2 2.373(3) . ? Y1 I1 2.9779(5) . ? C1 C2 1.404(5) . ? C1 C6 1.413(5) . ? C1 P1 1.851(4) . ? C2 C3 1.395(5) . ? C2 C7 1.494(5) . ? C3 C4 1.374(6) . ? C4 C5 1.381(5) . ? C5 C6 1.386(5) . ? C6 C22 1.495(5) . ? C7 C12 1.397(5) . ? C7 C8 1.406(6) . ? C8 C9 1.378(6) . ? C8 C13 1.517(7) . ? C9 C10 1.362(6) . ? C10 C11 1.359(6) . ? C10 C16 1.513(2) . ? C11 C12 1.392(5) . ? C12 C19 1.513(6) . ? C13 C15 1.510(8) . ? C13 C14 1.557(8) . ? C16 C18 1.515(2) . ? C16 C17 1.515(2) . ? C19 C20 1.512(6) . ? C19 C21 1.530(6) . ? C22 C23 1.394(5) . ? C22 C27 1.410(5) . ? C23 C24 1.396(5) . ? C23 C28 1.524(5) . ? C24 C25 1.368(6) . ? C25 C26 1.385(6) . ? C25 C31 1.519(5) . ? C26 C27 1.386(6) . ? C27 C34 1.527(6) . ? C28 C30 1.528(6) . ? C28 C29 1.534(6) . ? C31 C33 1.495(8) . ? C31 C32 1.503(8) . ? C34 C36 1.502(7) . ? C34 C35 1.543(6) . ? P1 C37 1.846(6) . ? C37 C38 1.493(7) . ? C38 C39 1.440(7) . ? C39 C40 1.443(7) . ? C40 O1 1.392(5) . ? O2 C44 1.459(5) . ? O2 C41 1.460(5) . ? C41 C42 1.508(8) . ? C42 C43 1.435(9) . ? C43 C44 1.474(7) . ? C45 C46 1.504(6) . ? C46 N1 1.333(5) . ? C46 C47 1.400(5) . ? C47 C48 1.405(5) . ? C48 N2 1.337(5) . ? C48 C49 1.508(5) . ? N1 C50 1.435(5) . ? C50 C51 1.405(6) . ? C50 C55 1.416(6) . ? C51 C52 1.389(6) . ? C51 C56 1.507(6) . ? C52 C53 1.388(8) . ? C53 C54 1.367(7) . ? C54 C55 1.394(6) . ? C55 C59 1.512(6) . ? C56 C57 1.519(8) . ? C56 C58 1.545(7) . ? C59 C60 1.497(7) . ? C59 C61 1.505(8) . ? N2 C62 1.449(5) . ? C62 C67 1.400(6) . ? C62 C63 1.413(6) . ? C63 C64 1.388(7) . ? C63 C68 1.513(7) . ? C64 C65 1.369(8) . ? C65 C66 1.375(7) . ? C66 C67 1.408(6) . ? C67 C71 1.506(6) . ? C68 C69 1.518(7) . ? C68 C70 1.535(7) . ? C71 C72 1.520(7) . ? C71 C73 1.531(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 N1 107.57(11) . . ? O1 Y1 N2 100.76(11) . . ? N1 Y1 N2 80.55(11) . . ? O1 Y1 O2 88.40(10) . . ? N1 Y1 O2 93.86(10) . . ? N2 Y1 O2 170.35(10) . . ? O1 Y1 I1 120.46(8) . . ? N1 Y1 I1 131.56(7) . . ? N2 Y1 I1 95.61(7) . . ? O2 Y1 I1 82.15(7) . . ? C2 C1 C6 119.5(3) . . ? C2 C1 P1 119.1(3) . . ? C6 C1 P1 121.1(3) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 C7 117.0(3) . . ? C1 C2 C7 123.6(3) . . ? C4 C3 C2 120.8(4) . . ? C3 C4 C5 120.0(4) . . ? C4 C5 C6 121.1(4) . . ? C5 C6 C1 119.1(3) . . ? C5 C6 C22 119.6(3) . . ? C1 C6 C22 121.3(3) . . ? C12 C7 C8 119.2(4) . . ? C12 C7 C2 120.4(4) . . ? C8 C7 C2 120.3(3) . . ? C9 C8 C7 119.6(4) . . ? C9 C8 C13 119.1(4) . . ? C7 C8 C13 121.2(4) . . ? C10 C9 C8 121.0(4) . . ? C11 C10 C9 119.7(4) . . ? C11 C10 C16 115.6(4) . . ? C9 C10 C16 124.5(5) . . ? C10 C11 C12 121.9(4) . . ? C11 C12 C7 118.4(4) . . ? C11 C12 C19 119.4(4) . . ? C7 C12 C19 122.1(3) . . ? C15 C13 C8 108.9(5) . . ? C15 C13 C14 114.4(7) . . ? C8 C13 C14 110.1(5) . . ? C10 C16 C18 114.6(4) . . ? C10 C16 C17 117.1(4) . . ? C18 C16 C17 116.2(5) . . ? C20 C19 C12 112.7(4) . . ? C20 C19 C21 112.2(4) . . ? C12 C19 C21 110.7(4) . . ? C23 C22 C27 119.5(3) . . ? C23 C22 C6 120.5(3) . . ? C27 C22 C6 120.0(3) . . ? C22 C23 C24 119.2(3) . . ? C22 C23 C28 122.0(3) . . ? C24 C23 C28 118.8(3) . . ? C25 C24 C23 122.5(4) . . ? C24 C25 C26 117.5(4) . . ? C24 C25 C31 120.9(4) . . ? C26 C25 C31 121.6(4) . . ? C25 C26 C27 122.9(4) . . ? C26 C27 C22 118.4(4) . . ? C26 C27 C34 120.4(4) . . ? C22 C27 C34 121.1(3) . . ? C23 C28 C30 110.6(4) . . ? C23 C28 C29 113.1(3) . . ? C30 C28 C29 109.2(4) . . ? C33 C31 C32 111.1(5) . . ? C33 C31 C25 110.8(4) . . ? C32 C31 C25 112.1(4) . . ? C36 C34 C27 109.7(4) . . ? C36 C34 C35 111.2(4) . . ? C27 C34 C35 113.7(4) . . ? C37 P1 C1 107.0(2) . . ? C38 C37 P1 113.5(4) . . ? C39 C38 C37 116.7(4) . . ? C38 C39 C40 117.4(4) . . ? O1 C40 C39 114.8(4) . . ? C40 O1 Y1 174.9(3) . . ? C44 O2 C41 108.5(3) . . ? C44 O2 Y1 113.2(3) . . ? C41 O2 Y1 130.7(3) . . ? O2 C41 C42 101.8(4) . . ? C43 C42 C41 106.7(5) . . ? C42 C43 C44 103.6(5) . . ? O2 C44 C43 107.3(5) . . ? N1 C46 C47 123.9(3) . . ? N1 C46 C45 120.9(4) . . ? C47 C46 C45 115.3(3) . . ? C46 C47 C48 130.4(4) . . ? N2 C48 C47 124.5(3) . . ? N2 C48 C49 119.9(4) . . ? C47 C48 C49 115.5(3) . . ? C46 N1 C50 118.1(3) . . ? C46 N1 Y1 125.5(2) . . ? C50 N1 Y1 116.1(2) . . ? C51 C50 C55 120.7(4) . . ? C51 C50 N1 119.1(4) . . ? C55 C50 N1 119.9(3) . . ? C52 C51 C50 118.5(4) . . ? C52 C51 C56 119.9(4) . . ? C50 C51 C56 121.6(4) . . ? C53 C52 C51 121.0(5) . . ? C54 C53 C52 120.3(5) . . ? C53 C54 C55 121.3(5) . . ? C54 C55 C50 118.1(4) . . ? C54 C55 C59 119.6(4) . . ? C50 C55 C59 122.2(4) . . ? C51 C56 C57 113.4(6) . . ? C51 C56 C58 111.7(5) . . ? C57 C56 C58 108.9(7) . . ? C60 C59 C61 108.3(4) . . ? C60 C59 C55 113.5(4) . . ? C61 C59 C55 112.9(4) . . ? C48 N2 C62 117.9(3) . . ? C48 N2 Y1 122.6(2) . . ? C62 N2 Y1 118.8(2) . . ? C67 C62 C63 120.9(4) . . ? C67 C62 N2 120.9(3) . . ? C63 C62 N2 118.1(4) . . ? C64 C63 C62 118.0(5) . . ? C64 C63 C68 119.7(4) . . ? C62 C63 C68 122.2(4) . . ? C65 C64 C63 122.1(5) . . ? C64 C65 C66 119.5(5) . . ? C65 C66 C67 121.5(5) . . ? C62 C67 C66 117.9(4) . . ? C62 C67 C71 123.5(4) . . ? C66 C67 C71 118.7(4) . . ? C63 C68 C69 111.5(5) . . ? C63 C68 C70 112.5(4) . . ? C69 C68 C70 109.1(4) . . ? C67 C71 C72 111.5(4) . . ? C67 C71 C73 110.8(4) . . ? C72 C71 C73 110.4(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.053 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.075 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 646375' _refine_special_details ; The DME molecule is positionally disordered over two sites with occupancies 0.59:0.41. Distance restraints were applied. =CH2 and C-H protons refined with distance restraints. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H106 K N4 O4 Y' _chemical_formula_sum 'C72 H106 K N4 O4 Y' _chemical_formula_weight 1219.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 22.653(4) _cell_length_b 16.124(3) _cell_length_c 20.120(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.668(2) _cell_angle_gamma 90.00 _cell_volume 7002.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4392 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5510 _exptl_absorpt_correction_T_max 0.8199 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19562 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6144 _reflns_number_gt 4648 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0609P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, =CH2, =CH and Me from difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6144 _refine_ls_number_parameters 448 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.988 _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 Y1 Y 1.0000 1.655661(19) 1.2500 0.02035(11) Uani 1 2 d S . . N1 N 1.03503(8) 1.73062(11) 1.17578(10) 0.0235(4) Uani 1 1 d . . . N2 N 0.92870(8) 1.59208(11) 1.16118(10) 0.0249(5) Uani 1 1 d . . . C1 C 1.06474(13) 1.70279(18) 1.07110(15) 0.0411(7) Uani 1 1 d D . . H1A H 1.0682(13) 1.6625(12) 1.0360(11) 0.049 Uiso 1 1 d D . . H1B H 1.0809(12) 1.7588(9) 1.0685(15) 0.049 Uiso 1 1 d D . . C2 C 1.03995(10) 1.67973(15) 1.12135(13) 0.0266(6) Uani 1 1 d . . . C3 C 1.01967(11) 1.59177(15) 1.12047(14) 0.0309(6) Uani 1 1 d D . . H3 H 1.0447(10) 1.5534(12) 1.1037(13) 0.037 Uiso 1 1 d D . . C4 C 0.96967(11) 1.55437(14) 1.13064(14) 0.0299(6) Uani 1 1 d . . . C5 C 0.96021(14) 1.46202(16) 1.11370(18) 0.0499(8) Uani 1 1 d . . . H5A H 0.9857 1.4453 1.0844 0.075 Uiso 1 1 calc R . . H5B H 0.9165 1.4516 1.0888 0.075 Uiso 1 1 calc R . . H5C H 0.9724 1.4299 1.1571 0.075 Uiso 1 1 calc R . . C6 C 1.06112(11) 1.81169(15) 1.17672(12) 0.0250(5) Uani 1 1 d . . . C7 C 1.12369(11) 1.82530(15) 1.21592(13) 0.0305(6) Uani 1 1 d . . . C8 C 1.14812(13) 1.90478(17) 1.21754(16) 0.0448(7) Uani 1 1 d . . . H8 H 1.1896 1.9148 1.2453 0.054 Uiso 1 1 calc R . . C9 C 1.11392(14) 1.96944(17) 1.17997(16) 0.0482(8) Uani 1 1 d . . . H9 H 1.1320 2.0228 1.1811 0.058 Uiso 1 1 calc R . . C10 C 1.05322(13) 1.95592(16) 1.14071(15) 0.0377(7) Uani 1 1 d . A . H10 H 1.0295 2.0004 1.1150 0.045 Uiso 1 1 calc R . . C11 C 1.02627(11) 1.87772(15) 1.13824(13) 0.0278(6) Uani 1 1 d . . . C12 C 1.16457(11) 1.75675(17) 1.25656(14) 0.0346(6) Uani 1 1 d . . . H12 H 1.1429 1.7028 1.2414 0.042 Uiso 1 1 calc R . . C13 C 1.17460(14) 1.76623(18) 1.33439(15) 0.0472(8) Uani 1 1 d . . . H13A H 1.1944 1.8198 1.3502 0.071 Uiso 1 1 calc R . . H13B H 1.2013 1.7213 1.3595 0.071 Uiso 1 1 calc R . . H13C H 1.1346 1.7637 1.3436 0.071 Uiso 1 1 calc R . . C14 C 1.22735(13) 1.7526(2) 1.24322(19) 0.0631(10) Uani 1 1 d . . . H14A H 1.2211 1.7462 1.1931 0.095 Uiso 1 1 calc R . . H14B H 1.2509 1.7052 1.2683 0.095 Uiso 1 1 calc R . . H14C H 1.2504 1.8039 1.2597 0.095 Uiso 1 1 calc R . . C15 C 0.95992(12) 1.86626(15) 1.09175(14) 0.0320(6) Uani 1 1 d . . . H15 H 0.9479 1.8070 1.0949 0.038 Uiso 1 1 calc R . . C16 C 0.91524(13) 1.92077(17) 1.11532(17) 0.0478(8) Uani 1 1 d . . . H16A H 0.9196 1.9095 1.1644 0.072 Uiso 1 1 calc R . . H16B H 0.8727 1.9087 1.0869 0.072 Uiso 1 1 calc R . . H16C H 0.9246 1.9792 1.1098 0.072 Uiso 1 1 calc R . . C17 C 0.95424(15) 1.8854(2) 1.01519(15) 0.0543(8) Uani 1 1 d . . . H17A H 0.9115 1.8760 0.9861 0.081 Uiso 1 1 calc R . . H17B H 0.9821 1.8491 0.9997 0.081 Uiso 1 1 calc R . . H17C H 0.9655 1.9434 1.0110 0.081 Uiso 1 1 calc R . . C18 C 0.86454(11) 1.57320(14) 1.13075(14) 0.0280(6) Uani 1 1 d . . . C19 C 0.83033(12) 1.53521(16) 1.16954(15) 0.0376(7) Uani 1 1 d . . . C20 C 0.76738(12) 1.51941(18) 1.13781(17) 0.0473(8) Uani 1 1 d . . . H20 H 0.7441 1.4934 1.1641 0.057 Uiso 1 1 calc R . . C21 C 0.73837(12) 1.54037(17) 1.06985(17) 0.0462(8) Uani 1 1 d . . . H21 H 0.6957 1.5282 1.0491 0.055 Uiso 1 1 calc R . . C22 C 0.77149(12) 1.57917(17) 1.03190(15) 0.0407(7) Uani 1 1 d . . . H22 H 0.7512 1.5940 0.9848 0.049 Uiso 1 1 calc R . . C23 C 0.83436(11) 1.59731(15) 1.06092(14) 0.0326(6) Uani 1 1 d . . . C24 C 0.85968(13) 1.5084(2) 1.24476(18) 0.0593(10) Uani 1 1 d . . . H24 H 0.8995 1.5395 1.2629 0.071 Uiso 1 1 calc R . . C25 C 0.8757(2) 1.4165(3) 1.2493(3) 0.1096(18) Uani 1 1 d . . . H25A H 0.8926 1.4002 1.2983 0.164 Uiso 1 1 calc R . . H25B H 0.9065 1.4058 1.2251 0.164 Uiso 1 1 calc R . . H25C H 0.8382 1.3841 1.2273 0.164 Uiso 1 1 calc R . . C26 C 0.82130(16) 1.5272(2) 1.29303(18) 0.0666(10) Uani 1 1 d . . . H26A H 0.7849 1.4910 1.2815 0.100 Uiso 1 1 calc R . . H26B H 0.8079 1.5853 1.2873 0.100 Uiso 1 1 calc R . . H26C H 0.8464 1.5176 1.3415 0.100 Uiso 1 1 calc R . . C27 C 0.86751(12) 1.64529(16) 1.01793(14) 0.0375(6) Uani 1 1 d . . . H27 H 0.9081 1.6642 1.0503 0.045 Uiso 1 1 calc R . . C28 C 0.88120(17) 1.5909(2) 0.96216(18) 0.0708(11) Uani 1 1 d . . . H28A H 0.9053 1.5425 0.9843 0.106 Uiso 1 1 calc R . . H28B H 0.9049 1.6229 0.9376 0.106 Uiso 1 1 calc R . . H28C H 0.8421 1.5726 0.9288 0.106 Uiso 1 1 calc R . . C29 C 0.83159(13) 1.72263(19) 0.98380(16) 0.0515(8) Uani 1 1 d . . . H29A H 0.7917 1.7060 0.9511 0.077 Uiso 1 1 calc R . . H29B H 0.8557 1.7529 0.9586 0.077 Uiso 1 1 calc R . . H29C H 0.8244 1.7585 1.0199 0.077 Uiso 1 1 calc R . . K1 K 1.0000 2.05301(5) 1.2500 0.0596(3) Uani 1 2 d S . . C30 C 0.8545(6) 2.1263(13) 1.1546(10) 0.085(6) Uani 0.409(12) 1 d PD A 1 H30A H 0.8305 2.1771 1.1534 0.128 Uiso 0.409(12) 1 calc PR A 1 H30B H 0.8492 2.0894 1.1910 0.128 Uiso 0.409(12) 1 calc PR A 1 H30C H 0.8399 2.0984 1.1093 0.128 Uiso 0.409(12) 1 calc PR A 1 O1 O 0.9180(6) 2.1466(7) 1.1692(4) 0.068(3) Uani 0.409(12) 1 d PD A 1 C31 C 0.9315(9) 2.1912(8) 1.1148(7) 0.072(6) Uani 0.409(12) 1 d PD A 1 H31A H 0.8995 2.2342 1.0966 0.087 Uiso 0.409(12) 1 calc PR A 1 H31B H 0.9308 2.1529 1.0761 0.087 Uiso 0.409(12) 1 calc PR A 1 C32 C 0.9934(7) 2.2309(7) 1.1410(7) 0.083(4) Uani 0.409(12) 1 d PD A 1 H32A H 1.0015 2.2643 1.1034 0.100 Uiso 0.409(12) 1 calc PR A 1 H32B H 0.9945 2.2684 1.1803 0.100 Uiso 0.409(12) 1 calc PR A 1 O2 O 1.0393(6) 2.1689(5) 1.1633(4) 0.061(3) Uani 0.409(12) 1 d PD A 1 C33 C 1.1004(7) 2.2014(6) 1.1819(7) 0.070(4) Uani 0.409(12) 1 d PD A 1 H33A H 1.1060 2.2327 1.1425 0.105 Uiso 0.409(12) 1 calc PR A 1 H33B H 1.1303 2.1557 1.1936 0.105 Uiso 0.409(12) 1 calc PR A 1 H33C H 1.1071 2.2381 1.2223 0.105 Uiso 0.409(12) 1 calc PR A 1 C30A C 0.8235(4) 2.0809(6) 1.1508(4) 0.075(3) Uani 0.591(12) 1 d PD A 2 H30D H 0.7934 2.1247 1.1505 0.112 Uiso 0.591(12) 1 calc PR A 2 H30E H 0.8241 2.0406 1.1875 0.112 Uiso 0.591(12) 1 calc PR A 2 H30F H 0.8117 2.0529 1.1054 0.112 Uiso 0.591(12) 1 calc PR A 2 O1A O 0.8839(4) 2.1168(4) 1.1640(3) 0.056(2) Uani 0.591(12) 1 d PD A 2 C31A C 0.8865(5) 2.1700(5) 1.1095(4) 0.081(3) Uani 0.591(12) 1 d PD A 2 H31C H 0.8504 2.2080 1.0982 0.097 Uiso 0.591(12) 1 calc PR A 2 H31D H 0.8839 2.1367 1.0674 0.097 Uiso 0.591(12) 1 calc PR A 2 C32A C 0.9442(6) 2.2194(6) 1.1284(7) 0.077(5) Uani 0.591(12) 1 d PD A 2 H32C H 0.9452 2.2543 1.0882 0.093 Uiso 0.591(12) 1 calc PR A 2 H32D H 0.9451 2.2566 1.1678 0.093 Uiso 0.591(12) 1 calc PR A 2 O2A O 0.9969(5) 2.1674(3) 1.1474(3) 0.067(2) Uani 0.591(12) 1 d PD A 2 C33A C 1.0531(6) 2.2115(6) 1.1579(5) 0.082(4) Uani 0.591(12) 1 d PD A 2 H33D H 1.0494 2.2487 1.1183 0.123 Uiso 0.591(12) 1 calc PR A 2 H33E H 1.0870 2.1722 1.1617 0.123 Uiso 0.591(12) 1 calc PR A 2 H33F H 1.0619 2.2441 1.2009 0.123 Uiso 0.591(12) 1 calc PR A 2 C34 C 1.27318(16) 1.8293(2) 1.0160(2) 0.0664(10) Uani 1 1 d . . . H34 H 1.2895 1.8836 1.0273 0.080 Uiso 1 1 calc R . . C35 C 1.23218(16) 1.7970(3) 1.04747(19) 0.0665(10) Uani 1 1 d . . . H35 H 1.2194 1.8296 1.0799 0.080 Uiso 1 1 calc R . . C36 C 1.20980(15) 1.7183(3) 1.0322(2) 0.0657(10) Uani 1 1 d . . . H36 H 1.1823 1.6961 1.0551 0.079 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 Y1 0.01294(17) 0.02453(18) 0.02054(19) 0.000 0.00055(13) 0.000 N1 0.0187(10) 0.0297(11) 0.0208(12) -0.0018(9) 0.0041(9) -0.0022(8) N2 0.0137(10) 0.0276(10) 0.0285(12) -0.0051(9) -0.0007(9) -0.0022(8) C1 0.0416(17) 0.0519(18) 0.0341(18) -0.0115(14) 0.0178(15) -0.0036(14) C2 0.0131(12) 0.0395(14) 0.0238(14) -0.0057(11) 0.0007(11) 0.0020(10) C3 0.0205(13) 0.0367(14) 0.0336(16) -0.0126(12) 0.0051(12) 0.0033(11) C4 0.0207(13) 0.0322(14) 0.0300(16) -0.0068(11) -0.0025(12) 0.0011(11) C5 0.0364(17) 0.0373(16) 0.073(2) -0.0191(15) 0.0131(17) -0.0033(13) C6 0.0234(13) 0.0334(13) 0.0185(14) -0.0018(11) 0.0069(11) -0.0066(11) C7 0.0246(13) 0.0423(15) 0.0237(14) 0.0014(11) 0.0059(12) -0.0092(11) C8 0.0307(15) 0.0518(18) 0.0446(19) 0.0062(15) 0.0002(14) -0.0192(14) C9 0.0478(19) 0.0431(16) 0.048(2) 0.0072(15) 0.0069(16) -0.0241(14) C10 0.0402(16) 0.0374(15) 0.0330(17) 0.0061(12) 0.0074(14) -0.0055(12) C11 0.0262(14) 0.0344(13) 0.0225(14) 0.0000(11) 0.0068(12) -0.0032(11) C12 0.0210(13) 0.0469(16) 0.0328(17) -0.0004(13) 0.0034(12) -0.0086(12) C13 0.0488(19) 0.0477(17) 0.0358(19) 0.0037(14) -0.0010(15) -0.0050(14) C14 0.0334(17) 0.088(2) 0.069(3) 0.012(2) 0.0170(18) 0.0042(17) C15 0.0296(14) 0.0344(14) 0.0276(15) 0.0024(11) 0.0022(12) -0.0017(11) C16 0.0358(16) 0.0480(17) 0.055(2) 0.0022(15) 0.0066(15) 0.0039(14) C17 0.0481(19) 0.076(2) 0.0299(18) 0.0074(16) -0.0021(15) -0.0072(17) C18 0.0187(13) 0.0242(12) 0.0361(16) -0.0045(11) 0.0011(12) -0.0031(10) C19 0.0216(14) 0.0389(15) 0.0429(19) 0.0080(13) -0.0040(13) -0.0077(11) C20 0.0246(15) 0.0557(18) 0.054(2) 0.0133(15) 0.0003(15) -0.0135(13) C21 0.0197(14) 0.0534(18) 0.053(2) 0.0015(15) -0.0078(15) -0.0078(13) C22 0.0258(14) 0.0527(17) 0.0332(17) -0.0031(14) -0.0069(13) -0.0038(13) C23 0.0239(14) 0.0374(15) 0.0307(16) -0.0084(12) -0.0005(12) -0.0012(11) C24 0.0243(15) 0.080(2) 0.061(2) 0.0383(19) -0.0050(16) -0.0187(15) C25 0.088(3) 0.115(3) 0.139(4) 0.090(3) 0.055(3) 0.050(3) C26 0.058(2) 0.081(2) 0.049(2) 0.0220(18) -0.0008(19) -0.0294(19) C27 0.0304(14) 0.0561(17) 0.0229(14) -0.0052(13) 0.0033(12) -0.0014(13) C28 0.074(3) 0.101(3) 0.042(2) -0.0207(19) 0.023(2) -0.004(2) C29 0.0403(17) 0.072(2) 0.0337(19) 0.0092(15) -0.0012(15) -0.0069(16) K1 0.1050(9) 0.0385(5) 0.0306(6) 0.000 0.0138(6) 0.000 C30 0.042(10) 0.115(14) 0.083(9) 0.025(9) -0.004(9) 0.040(10) O1 0.059(6) 0.087(6) 0.048(4) 0.019(4) 0.003(4) 0.029(5) C31 0.106(16) 0.046(10) 0.049(8) 0.024(8) -0.002(9) 0.022(9) C32 0.111(15) 0.045(7) 0.088(9) 0.010(6) 0.022(10) 0.013(8) O2 0.070(8) 0.044(5) 0.064(5) 0.020(4) 0.011(5) 0.003(5) C33 0.093(9) 0.045(5) 0.073(8) 0.003(5) 0.025(8) -0.022(6) C30A 0.058(6) 0.093(6) 0.072(5) 0.023(5) 0.019(5) 0.022(4) O1A 0.060(6) 0.063(4) 0.044(4) 0.015(3) 0.013(4) 0.020(4) C31A 0.088(7) 0.074(5) 0.074(6) 0.035(4) 0.015(5) 0.014(5) C32A 0.126(13) 0.032(6) 0.069(7) 0.008(4) 0.022(8) -0.001(5) O2A 0.078(6) 0.051(3) 0.073(4) 0.015(2) 0.025(4) -0.002(3) C33A 0.122(12) 0.058(6) 0.066(6) 0.008(5) 0.029(7) -0.033(8) C34 0.050(2) 0.075(2) 0.065(3) 0.000(2) 0.004(2) 0.0034(18) C35 0.058(2) 0.083(3) 0.057(2) -0.002(2) 0.016(2) 0.018(2) C36 0.0387(19) 0.100(3) 0.061(3) 0.016(2) 0.0193(19) 0.011(2) _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 Y1 N1 2.2451(18) 2_757 ? Y1 N1 2.2451(18) . ? Y1 N2 2.2586(19) . ? Y1 N2 2.2586(19) 2_757 ? Y1 C4 2.812(2) . ? Y1 C4 2.812(2) 2_757 ? Y1 C3 2.959(3) . ? Y1 C3 2.959(3) 2_757 ? Y1 C2 3.015(2) 2_757 ? Y1 C2 3.015(2) . ? N1 C2 1.400(3) . ? N1 C6 1.432(3) . ? N2 C4 1.398(3) . ? N2 C18 1.428(3) . ? C1 C2 1.349(3) . ? C2 C3 1.489(3) . ? C3 C4 1.352(3) . ? C4 C5 1.528(3) . ? C6 C11 1.409(3) . ? C6 C7 1.414(3) . ? C7 C8 1.393(3) . ? C7 C12 1.513(4) . ? C8 C9 1.380(4) . ? C9 C10 1.379(4) . ? C10 C11 1.395(3) . ? C10 K1 3.217(3) . ? C11 C15 1.521(3) . ? C12 C13 1.520(4) . ? C12 C14 1.527(3) . ? C15 C16 1.521(4) . ? C15 C17 1.538(4) . ? C18 C19 1.397(3) . ? C18 C23 1.418(4) . ? C19 C20 1.398(4) . ? C19 C24 1.520(4) . ? C20 C21 1.368(4) . ? C21 C22 1.373(4) . ? C22 C23 1.396(3) . ? C23 C27 1.518(4) . ? C24 C26 1.518(5) . ? C24 C25 1.522(5) . ? C27 C28 1.528(4) . ? C27 C29 1.533(4) . ? K1 O1 2.557(7) 2_757 ? K1 O1 2.557(7) . ? K1 O2A 2.754(5) 2_757 ? K1 O2A 2.754(5) . ? K1 O1A 2.864(8) 2_757 ? K1 O1A 2.864(8) . ? K1 O2 2.875(10) 2_757 ? K1 O2 2.875(10) . ? K1 C10 3.217(3) 2_757 ? K1 C30 3.480(12) 2_757 ? K1 C31 3.493(13) 2_757 ? C30 O1 1.417(9) . ? O1 C31 1.416(9) . ? C31 C32 1.485(9) . ? C32 O2 1.414(5) . ? O2 C33 1.420(8) . ? C30A O1A 1.436(7) . ? O1A C31A 1.408(7) . ? C31A C32A 1.480(8) . ? C32A O2A 1.412(8) . ? O2A C33A 1.417(7) . ? C34 C35 1.375(5) . ? C34 C36 1.381(5) 7_787 ? C35 C36 1.367(5) . ? C36 C34 1.381(5) 7_787 ? 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 N1 Y1 N1 114.85(9) 2_757 . ? N1 Y1 N2 117.29(7) 2_757 . ? N1 Y1 N2 91.74(7) . . ? N1 Y1 N2 91.74(7) 2_757 2_757 ? N1 Y1 N2 117.29(7) . 2_757 ? N2 Y1 N2 126.01(10) . 2_757 ? N1 Y1 C4 146.81(7) 2_757 . ? N1 Y1 C4 77.80(7) . . ? N2 Y1 C4 29.52(7) . . ? N2 Y1 C4 110.05(7) 2_757 . ? N1 Y1 C4 77.80(7) 2_757 2_757 ? N1 Y1 C4 146.81(7) . 2_757 ? N2 Y1 C4 110.05(7) . 2_757 ? N2 Y1 C4 29.52(7) 2_757 2_757 ? C4 Y1 C4 108.97(10) . 2_757 ? N1 Y1 C3 162.06(7) 2_757 . ? N1 Y1 C3 54.80(7) . . ? N2 Y1 C3 53.69(7) . . ? N2 Y1 C3 106.03(7) 2_757 . ? C4 Y1 C3 26.95(7) . . ? C4 Y1 C3 119.14(7) 2_757 . ? N1 Y1 C3 54.80(7) 2_757 2_757 ? N1 Y1 C3 162.06(7) . 2_757 ? N2 Y1 C3 106.03(7) . 2_757 ? N2 Y1 C3 53.69(7) 2_757 2_757 ? C4 Y1 C3 119.14(7) . 2_757 ? C4 Y1 C3 26.95(7) 2_757 2_757 ? C3 Y1 C3 139.25(10) . 2_757 ? N1 Y1 C2 25.96(6) 2_757 2_757 ? N1 Y1 C2 139.51(7) . 2_757 ? N2 Y1 C2 114.13(7) . 2_757 ? N2 Y1 C2 73.02(7) 2_757 2_757 ? C4 Y1 C2 138.49(7) . 2_757 ? C4 Y1 C2 53.18(7) 2_757 2_757 ? C3 Y1 C2 164.90(7) . 2_757 ? C3 Y1 C2 28.85(7) 2_757 2_757 ? N1 Y1 C2 139.51(7) 2_757 . ? N1 Y1 C2 25.96(6) . . ? N2 Y1 C2 73.02(7) . . ? N2 Y1 C2 114.13(7) 2_757 . ? C4 Y1 C2 53.18(7) . . ? C4 Y1 C2 138.49(7) 2_757 . ? C3 Y1 C2 28.85(7) . . ? C3 Y1 C2 164.90(7) 2_757 . ? C2 Y1 C2 165.21(9) 2_757 . ? C2 N1 C6 114.52(18) . . ? C2 N1 Y1 109.44(14) . . ? C6 N1 Y1 135.25(15) . . ? C4 N2 C18 116.35(19) . . ? C4 N2 Y1 97.73(14) . . ? C18 N2 Y1 145.72(15) . . ? C1 C2 N1 125.1(2) . . ? C1 C2 C3 116.8(2) . . ? N1 C2 C3 118.0(2) . . ? C1 C2 Y1 168.6(2) . . ? N1 C2 Y1 44.60(11) . . ? C3 C2 Y1 73.49(13) . . ? C4 C3 C2 133.8(2) . . ? C4 C3 Y1 70.44(15) . . ? C2 C3 Y1 77.66(13) . . ? C3 C4 N2 124.8(2) . . ? C3 C4 C5 117.9(2) . . ? N2 C4 C5 117.1(2) . . ? C3 C4 Y1 82.62(15) . . ? N2 C4 Y1 52.75(11) . . ? C5 C4 Y1 137.6(2) . . ? C11 C6 C7 119.3(2) . . ? C11 C6 N1 121.5(2) . . ? C7 C6 N1 119.2(2) . . ? C8 C7 C6 118.7(2) . . ? C8 C7 C12 119.1(2) . . ? C6 C7 C12 122.2(2) . . ? C9 C8 C7 122.0(3) . . ? C10 C9 C8 119.4(2) . . ? C9 C10 C11 120.8(3) . . ? C9 C10 K1 92.69(18) . . ? C11 C10 K1 102.33(16) . . ? C10 C11 C6 119.8(2) . . ? C10 C11 C15 118.1(2) . . ? C6 C11 C15 122.0(2) . . ? C7 C12 C13 111.0(2) . . ? C7 C12 C14 112.7(2) . . ? C13 C12 C14 109.2(2) . . ? C16 C15 C11 111.4(2) . . ? C16 C15 C17 109.6(2) . . ? C11 C15 C17 111.0(2) . . ? C19 C18 C23 119.4(2) . . ? C19 C18 N2 121.3(2) . . ? C23 C18 N2 119.2(2) . . ? C18 C19 C20 119.1(3) . . ? C18 C19 C24 122.1(2) . . ? C20 C19 C24 118.7(2) . . ? C21 C20 C19 121.7(3) . . ? C20 C21 C22 119.4(3) . . ? C21 C22 C23 121.5(3) . . ? C22 C23 C18 118.7(2) . . ? C22 C23 C27 119.1(2) . . ? C18 C23 C27 122.1(2) . . ? C26 C24 C19 114.7(3) . . ? C26 C24 C25 109.2(3) . . ? C19 C24 C25 111.2(3) . . ? C23 C27 C28 111.8(2) . . ? C23 C27 C29 112.5(2) . . ? C28 C27 C29 109.6(3) . . ? O1 K1 O1 107.7(6) 2_757 . ? O1 K1 O2A 43.9(2) 2_757 2_757 ? O1 K1 O2A 86.0(3) . 2_757 ? O1 K1 O2A 86.0(3) 2_757 . ? O1 K1 O2A 43.9(2) . . ? O2A K1 O2A 95.9(2) 2_757 . ? O1 K1 O1A 17.7(3) 2_757 2_757 ? O1 K1 O1A 121.9(4) . 2_757 ? O2A K1 O1A 59.8(2) 2_757 2_757 ? O2A K1 O1A 91.3(3) . 2_757 ? O1 K1 O1A 121.9(4) 2_757 . ? O1 K1 O1A 17.7(3) . . ? O2A K1 O1A 91.3(3) 2_757 . ? O2A K1 O1A 59.79(19) . . ? O1A K1 O1A 137.9(3) 2_757 . ? O1 K1 O2 61.9(3) 2_757 2_757 ? O1 K1 O2 72.8(3) . 2_757 ? O2A K1 O2 18.55(14) 2_757 2_757 ? O2A K1 O2 94.43(16) . 2_757 ? O1A K1 O2 78.3(2) 2_757 2_757 ? O1A K1 O2 74.7(3) . 2_757 ? O1 K1 O2 72.8(3) 2_757 . ? O1 K1 O2 61.9(3) . . ? O2A K1 O2 94.43(17) 2_757 . ? O2A K1 O2 18.55(14) . . ? O1A K1 O2 74.7(3) 2_757 . ? O1A K1 O2 78.3(2) . . ? O2 K1 O2 98.9(3) 2_757 . ? O1 K1 C10 111.8(3) 2_757 . ? O1 K1 C10 101.70(19) . . ? O2A K1 C10 155.4(2) 2_757 . ? O2A K1 C10 75.11(14) . . ? O1A K1 C10 97.00(16) 2_757 . ? O1A K1 C10 103.15(13) . . ? O2 K1 C10 168.53(17) 2_757 . ? O2 K1 C10 69.67(16) . . ? O1 K1 C10 101.70(19) 2_757 2_757 ? O1 K1 C10 111.8(3) . 2_757 ? O2A K1 C10 75.11(14) 2_757 2_757 ? O2A K1 C10 155.4(2) . 2_757 ? O1A K1 C10 103.15(13) 2_757 2_757 ? O1A K1 C10 97.00(17) . 2_757 ? O2 K1 C10 69.67(16) 2_757 2_757 ? O2 K1 C10 168.53(16) . 2_757 ? C10 K1 C10 121.76(9) . 2_757 ? O1 K1 C30 20.8(3) 2_757 2_757 ? O1 K1 C30 122.3(6) . 2_757 ? O2A K1 C30 63.6(3) 2_757 2_757 ? O2A K1 C30 89.4(5) . 2_757 ? O1A K1 C30 4.0(4) 2_757 2_757 ? O1A K1 C30 138.9(4) . 2_757 ? O2 K1 C30 82.0(3) 2_757 2_757 ? O2 K1 C30 72.4(5) . 2_757 ? C10 K1 C30 93.1(4) . 2_757 ? C10 K1 C30 106.1(4) 2_757 2_757 ? O1 K1 C31 20.5(3) 2_757 2_757 ? O1 K1 C31 100.6(4) . 2_757 ? O2A K1 C31 23.8(3) 2_757 2_757 ? O2A K1 C31 93.5(3) . 2_757 ? O1A K1 C31 36.0(3) 2_757 2_757 ? O1A K1 C31 110.5(4) . 2_757 ? O2 K1 C31 42.2(3) 2_757 2_757 ? O2 K1 C31 84.9(3) . 2_757 ? C10 K1 C31 132.3(3) . 2_757 ? C10 K1 C31 87.0(3) 2_757 2_757 ? C30 K1 C31 39.8(4) 2_757 2_757 ? C31 O1 C30 113.6(12) . . ? C31 O1 K1 120.3(8) . . ? C30 O1 K1 119.4(8) . . ? O1 C31 C32 110.3(12) . . ? O1 C31 K1 39.2(5) . . ? C32 C31 K1 81.4(8) . . ? O2 C32 C31 109.3(12) . . ? C32 O2 C33 112.7(11) . . ? C32 O2 K1 108.7(9) . . ? C33 O2 K1 122.4(6) . . ? C31A O1A C30A 111.3(7) . . ? C31A O1A K1 116.3(6) . . ? C30A O1A K1 128.0(4) . . ? O1A C31A C32A 111.7(9) . . ? O2A C32A C31A 111.1(8) . . ? C32A O2A C33A 113.0(7) . . ? C32A O2A K1 115.3(6) . . ? C33A O2A K1 114.0(6) . . ? C35 C34 C36 119.0(3) . 7_787 ? C36 C35 C34 120.4(3) . . ? C35 C36 C34 120.6(3) . 7_787 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.628 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.057 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 646376' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H104 I2 N4 O2 Y2' _chemical_formula_sum 'C74 H104 I2 N4 O2 Y2' _chemical_formula_weight 1513.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7763(8) _cell_length_b 21.4051(12) _cell_length_c 12.5537(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.384(2) _cell_angle_gamma 90.00 _cell_volume 3662.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7843 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.21 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 2.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5454 _exptl_absorpt_correction_T_max 0.6794 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26102 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6447 _reflns_number_gt 5339 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0545P)^2^+4.5135P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6447 _refine_ls_number_parameters 379 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Y1 Y -0.00045(2) 0.487275(15) 0.64530(3) 0.02081(10) Uani 1 1 d . . . I1 I 0.01411(2) 0.593710(12) 0.80222(2) 0.04046(11) Uani 1 1 d . . . N1 N -0.1183(2) 0.42963(13) 0.7112(2) 0.0229(6) Uani 1 1 d . . . N2 N 0.1084(2) 0.42247(13) 0.7474(2) 0.0226(6) Uani 1 1 d . . . C1 C -0.1812(3) 0.4130(2) 0.8833(3) 0.0354(9) Uani 1 1 d . . . H1A H -0.1537 0.4009 0.9568 0.053 Uiso 1 1 calc R . . H1B H -0.2248 0.3798 0.8506 0.053 Uiso 1 1 calc R . . H1C H -0.2185 0.4518 0.8852 0.053 Uiso 1 1 calc R . . C2 C -0.0993(3) 0.42269(16) 0.8178(3) 0.0240(7) Uani 1 1 d . . . C3 C -0.0052(3) 0.42467(17) 0.8781(3) 0.0266(8) Uani 1 1 d . . . H3A H -0.0055 0.4299 0.9532 0.032 Uiso 1 1 calc R . . C4 C 0.0894(3) 0.42040(16) 0.8491(3) 0.0246(8) Uani 1 1 d . . . C5 C 0.1733(3) 0.4149(2) 0.9416(3) 0.0354(9) Uani 1 1 d . . . H5A H 0.1475 0.4018 1.0068 0.053 Uiso 1 1 calc R . . H5B H 0.2059 0.4555 0.9541 0.053 Uiso 1 1 calc R . . H5C H 0.2206 0.3838 0.9235 0.053 Uiso 1 1 calc R . . C6 C -0.2167(2) 0.41673(17) 0.6577(3) 0.0264(8) Uani 1 1 d . . . C7 C -0.2382(3) 0.35631(18) 0.6158(3) 0.0288(8) Uani 1 1 d . . . C8 C -0.3326(3) 0.3451(2) 0.5629(3) 0.0393(10) Uani 1 1 d . . . H8A H -0.3489 0.3047 0.5345 0.047 Uiso 1 1 calc R . . C9 C -0.4028(3) 0.3912(2) 0.5509(3) 0.0428(11) Uani 1 1 d . . . H9A H -0.4666 0.3826 0.5138 0.051 Uiso 1 1 calc R . . C10 C -0.3808(3) 0.4498(2) 0.5925(3) 0.0412(10) Uani 1 1 d . . . H10A H -0.4299 0.4813 0.5837 0.049 Uiso 1 1 calc R . . C11 C -0.2880(3) 0.46396(19) 0.6473(3) 0.0325(9) Uani 1 1 d . . . C12 C -0.1625(3) 0.30475(19) 0.6293(3) 0.0380(9) Uani 1 1 d . . . H12A H -0.0966 0.3252 0.6424 0.046 Uiso 1 1 calc R . . C13 C -0.1708(5) 0.2639(3) 0.7260(5) 0.0791(19) Uani 1 1 d . . . H13A H -0.1622 0.2896 0.7914 0.119 Uiso 1 1 calc R . . H13B H -0.1198 0.2316 0.7321 0.119 Uiso 1 1 calc R . . H13C H -0.2356 0.2441 0.7173 0.119 Uiso 1 1 calc R . . C14 C -0.1650(4) 0.2644(2) 0.5290(4) 0.0543(12) Uani 1 1 d . . . H14A H -0.1620 0.2912 0.4663 0.081 Uiso 1 1 calc R . . H14B H -0.2258 0.2400 0.5181 0.081 Uiso 1 1 calc R . . H14C H -0.1086 0.2359 0.5382 0.081 Uiso 1 1 calc R . . C15 C -0.2684(3) 0.5294(2) 0.6907(4) 0.0434(11) Uani 1 1 d . . . H15A H -0.2016 0.5295 0.7344 0.052 Uiso 1 1 calc R . . C16 C -0.3416(4) 0.5501(3) 0.7650(5) 0.0642(14) Uani 1 1 d . . . H16A H -0.3411 0.5198 0.8237 0.096 Uiso 1 1 calc R . . H16B H -0.4076 0.5523 0.7237 0.096 Uiso 1 1 calc R . . H16C H -0.3227 0.5913 0.7952 0.096 Uiso 1 1 calc R . . C17 C -0.2668(4) 0.5756(2) 0.5996(5) 0.0599(13) Uani 1 1 d . . . H17A H -0.2184 0.5622 0.5542 0.090 Uiso 1 1 calc R . . H17B H -0.2490 0.6171 0.6294 0.090 Uiso 1 1 calc R . . H17C H -0.3319 0.5775 0.5562 0.090 Uiso 1 1 calc R . . C18 C 0.2044(3) 0.40377(18) 0.7269(3) 0.0281(8) Uani 1 1 d . . . C19 C 0.2783(3) 0.4484(2) 0.7243(3) 0.0382(10) Uani 1 1 d . . . C20 C 0.3690(3) 0.4278(3) 0.7009(4) 0.0524(13) Uani 1 1 d . . . H20A H 0.4201 0.4573 0.6979 0.063 Uiso 1 1 calc R . . C21 C 0.3858(3) 0.3663(3) 0.6823(4) 0.0554(14) Uani 1 1 d . . . H21A H 0.4485 0.3534 0.6675 0.067 Uiso 1 1 calc R . . C22 C 0.3136(3) 0.3229(2) 0.6848(3) 0.0468(11) Uani 1 1 d . . . H22A H 0.3268 0.2803 0.6714 0.056 Uiso 1 1 calc R . . C23 C 0.2208(3) 0.33995(19) 0.7067(3) 0.0315(9) Uani 1 1 d . . . C24 C 0.2610(3) 0.5165(2) 0.7460(4) 0.0441(11) Uani 1 1 d . . . H24A H 0.2032 0.5188 0.7856 0.053 Uiso 1 1 calc R . . C25 C 0.2344(4) 0.5526(2) 0.6409(4) 0.0554(13) Uani 1 1 d . . . H25A H 0.1811 0.5310 0.5951 0.083 Uiso 1 1 calc R . . H25B H 0.2919 0.5552 0.6035 0.083 Uiso 1 1 calc R . . H25C H 0.2130 0.5948 0.6568 0.083 Uiso 1 1 calc R . . C26 C 0.3466(4) 0.5480(3) 0.8161(5) 0.0808(19) Uani 1 1 d . . . H26A H 0.3641 0.5241 0.8827 0.121 Uiso 1 1 calc R . . H26B H 0.3277 0.5905 0.8338 0.121 Uiso 1 1 calc R . . H26C H 0.4032 0.5498 0.7770 0.121 Uiso 1 1 calc R . . C27 C 0.1431(3) 0.29049(18) 0.7112(3) 0.0347(9) Uani 1 1 d . . . H27A H 0.0781 0.3122 0.7009 0.042 Uiso 1 1 calc R . . C28 C 0.1539(4) 0.2580(2) 0.8203(4) 0.0513(12) Uani 1 1 d . . . H28A H 0.1492 0.2890 0.8768 0.077 Uiso 1 1 calc R . . H28B H 0.2178 0.2372 0.8341 0.077 Uiso 1 1 calc R . . H28C H 0.1016 0.2269 0.8202 0.077 Uiso 1 1 calc R . . C29 C 0.1403(4) 0.2419(2) 0.6223(4) 0.0546(13) Uani 1 1 d . . . H29A H 0.1341 0.2630 0.5523 0.082 Uiso 1 1 calc R . . H29B H 0.0840 0.2142 0.6240 0.082 Uiso 1 1 calc R . . H29C H 0.2009 0.2173 0.6332 0.082 Uiso 1 1 calc R . . O1 O 0.02242(18) 0.44327(11) 0.49055(18) 0.0271(5) Uani 1 1 d . . . C30 C 0.0324(3) 0.37758(18) 0.4838(3) 0.0374(9) Uani 1 1 d . . . H30A H -0.0110 0.3620 0.4205 0.056 Uiso 1 1 calc R . . H30B H 0.0145 0.3581 0.5488 0.056 Uiso 1 1 calc R . . H30C H 0.1005 0.3672 0.4773 0.056 Uiso 1 1 calc R . . C31 C 0.4582(7) 0.7928(4) 0.2067(6) 0.124(3) Uani 1 1 d D . . H31A H 0.5112 0.8238 0.2144 0.186 Uiso 1 1 calc R . . H31B H 0.4522 0.7751 0.2774 0.186 Uiso 1 1 calc R . . H31C H 0.3964 0.8130 0.1768 0.186 Uiso 1 1 calc R . . C32 C 0.4794(3) 0.74562(19) 0.1383(3) 0.094(2) Uani 1 1 d GD . . C33 C 0.5561(3) 0.7504(2) 0.0781(4) 0.078(2) Uani 1 1 d GD . . H33A H 0.5945 0.7874 0.0815 0.093 Uiso 1 1 calc R . . C34 C 0.5766(3) 0.7011(3) 0.0129(4) 0.108(3) Uani 1 1 d GD . . H34A H 0.6291 0.7044 -0.0282 0.130 Uiso 1 1 calc R . . C35 C 0.5204(4) 0.6470(2) 0.0079(4) 0.111(3) Uani 1 1 d GD . . H35A H 0.5345 0.6132 -0.0366 0.133 Uiso 1 1 calc R . . C36 C 0.4437(3) 0.64215(19) 0.0681(4) 0.096(2) Uani 1 1 d GD . . H36A H 0.4053 0.6051 0.0647 0.116 Uiso 1 1 calc R . . C37 C 0.4232(2) 0.6915(2) 0.1333(3) 0.082(2) Uani 1 1 d GD . . H37A H 0.3707 0.6882 0.1745 0.099 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 Y1 0.02209(17) 0.02346(18) 0.01730(17) 0.00329(13) 0.00427(13) -0.00069(13) I1 0.0640(2) 0.03280(16) 0.02451(15) -0.00314(10) 0.00618(12) -0.00181(12) N1 0.0213(15) 0.0257(15) 0.0224(16) -0.0005(12) 0.0056(12) -0.0025(12) N2 0.0211(15) 0.0267(15) 0.0203(15) 0.0026(12) 0.0034(12) -0.0010(12) C1 0.031(2) 0.049(3) 0.029(2) 0.0032(18) 0.0134(17) -0.0001(18) C2 0.0265(18) 0.0229(18) 0.0240(19) 0.0024(14) 0.0081(15) 0.0000(14) C3 0.0298(19) 0.032(2) 0.0186(18) 0.0020(15) 0.0046(15) -0.0014(15) C4 0.0251(18) 0.0248(18) 0.0237(18) 0.0045(15) 0.0023(14) -0.0007(14) C5 0.033(2) 0.049(3) 0.022(2) 0.0044(17) -0.0019(16) -0.0022(18) C6 0.0200(17) 0.038(2) 0.0216(18) 0.0038(16) 0.0060(14) -0.0033(15) C7 0.0282(19) 0.038(2) 0.0216(18) -0.0001(16) 0.0081(15) -0.0056(16) C8 0.035(2) 0.052(3) 0.031(2) -0.0050(19) 0.0073(18) -0.014(2) C9 0.023(2) 0.068(3) 0.037(2) 0.002(2) 0.0010(17) -0.011(2) C10 0.022(2) 0.058(3) 0.044(2) 0.004(2) 0.0053(18) 0.0035(19) C11 0.0250(19) 0.043(2) 0.030(2) 0.0031(18) 0.0066(16) 0.0013(17) C12 0.040(2) 0.036(2) 0.037(2) -0.0080(18) 0.0054(18) -0.0006(18) C13 0.121(5) 0.058(3) 0.064(4) 0.017(3) 0.034(4) 0.034(3) C14 0.054(3) 0.055(3) 0.053(3) -0.025(2) 0.007(2) -0.001(2) C15 0.029(2) 0.043(2) 0.057(3) -0.004(2) 0.000(2) 0.0075(18) C16 0.064(3) 0.060(3) 0.069(4) -0.014(3) 0.014(3) 0.015(3) C17 0.061(3) 0.047(3) 0.074(4) 0.001(3) 0.017(3) -0.005(2) C18 0.0194(18) 0.044(2) 0.0210(18) 0.0124(16) 0.0023(14) 0.0029(16) C19 0.025(2) 0.054(3) 0.033(2) 0.0149(19) 0.0004(16) -0.0066(18) C20 0.025(2) 0.077(4) 0.056(3) 0.027(3) 0.009(2) -0.009(2) C21 0.030(2) 0.089(4) 0.051(3) 0.026(3) 0.018(2) 0.018(2) C22 0.044(3) 0.060(3) 0.039(2) 0.017(2) 0.015(2) 0.021(2) C23 0.032(2) 0.042(2) 0.0211(19) 0.0091(17) 0.0060(15) 0.0075(17) C24 0.036(2) 0.053(3) 0.043(3) 0.010(2) 0.0040(19) -0.017(2) C25 0.056(3) 0.052(3) 0.060(3) 0.019(2) 0.015(2) -0.004(2) C26 0.063(4) 0.077(4) 0.095(5) -0.004(4) -0.013(3) -0.026(3) C27 0.042(2) 0.034(2) 0.028(2) 0.0045(17) 0.0066(17) 0.0096(18) C28 0.065(3) 0.051(3) 0.038(2) 0.013(2) 0.008(2) -0.007(2) C29 0.086(4) 0.039(3) 0.041(3) -0.002(2) 0.013(2) 0.010(2) O1 0.0383(14) 0.0247(13) 0.0189(12) 0.0013(10) 0.0060(11) 0.0029(11) C30 0.062(3) 0.027(2) 0.026(2) -0.0033(16) 0.0148(19) -0.0004(19) C31 0.154(8) 0.106(6) 0.090(6) -0.016(5) -0.050(5) 0.038(6) C32 0.091(5) 0.099(5) 0.077(5) 0.019(4) -0.037(4) 0.017(4) C33 0.045(3) 0.117(6) 0.069(4) 0.046(4) -0.001(3) 0.003(3) C34 0.068(4) 0.146(8) 0.106(6) 0.061(6) -0.005(4) -0.004(5) C35 0.090(5) 0.141(8) 0.097(6) 0.018(5) -0.003(5) -0.006(5) C36 0.063(4) 0.138(7) 0.088(5) 0.010(5) 0.011(4) -0.024(4) C37 0.058(3) 0.071(4) 0.106(5) 0.029(4) -0.029(3) -0.028(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 Y1 O1 2.222(2) . ? Y1 O1 2.249(2) 3_566 ? Y1 N1 2.287(3) . ? Y1 N2 2.293(3) . ? Y1 I1 2.9994(4) . ? N1 C2 1.334(4) . ? N1 C6 1.449(4) . ? N2 C4 1.340(5) . ? N2 C18 1.440(4) . ? C1 C2 1.505(5) . ? C2 C3 1.402(5) . ? C3 C4 1.406(5) . ? C4 C5 1.519(5) . ? C6 C11 1.403(5) . ? C6 C7 1.412(5) . ? C7 C8 1.393(5) . ? C7 C12 1.510(5) . ? C8 C9 1.374(6) . ? C9 C10 1.375(6) . ? C10 C11 1.395(5) . ? C11 C15 1.513(6) . ? C12 C13 1.514(7) . ? C12 C14 1.523(6) . ? C15 C17 1.515(7) . ? C15 C16 1.535(6) . ? C18 C19 1.401(5) . ? C18 C23 1.414(5) . ? C19 C20 1.396(6) . ? C19 C24 1.507(6) . ? C20 C21 1.363(7) . ? C21 C22 1.364(7) . ? C22 C23 1.394(6) . ? C23 C27 1.513(6) . ? C24 C26 1.524(6) . ? C24 C25 1.527(6) . ? C27 C29 1.522(6) . ? C27 C28 1.524(5) . ? O1 C30 1.416(4) . ? O1 Y1 2.249(2) 3_566 ? C31 C32 1.384(8) . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 O1 68.78(10) . 3_566 ? O1 Y1 N1 106.61(10) . . ? O1 Y1 N1 127.33(10) 3_566 . ? O1 Y1 N2 93.90(9) . . ? O1 Y1 N2 145.97(9) 3_566 . ? N1 Y1 N2 84.96(10) . . ? O1 Y1 I1 153.08(6) . . ? O1 Y1 I1 89.12(6) 3_566 . ? N1 Y1 I1 98.94(7) . . ? N2 Y1 I1 96.69(7) . . ? C2 N1 C6 118.5(3) . . ? C2 N1 Y1 112.1(2) . . ? C6 N1 Y1 126.9(2) . . ? C4 N2 C18 118.2(3) . . ? C4 N2 Y1 110.5(2) . . ? C18 N2 Y1 127.6(2) . . ? N1 C2 C3 124.7(3) . . ? N1 C2 C1 120.7(3) . . ? C3 C2 C1 114.6(3) . . ? C2 C3 C4 132.6(3) . . ? N2 C4 C3 124.2(3) . . ? N2 C4 C5 119.9(3) . . ? C3 C4 C5 116.0(3) . . ? C11 C6 C7 121.3(3) . . ? C11 C6 N1 120.1(3) . . ? C7 C6 N1 118.6(3) . . ? C8 C7 C6 117.8(4) . . ? C8 C7 C12 120.6(4) . . ? C6 C7 C12 121.6(3) . . ? C9 C8 C7 121.5(4) . . ? C8 C9 C10 120.0(4) . . ? C9 C10 C11 121.4(4) . . ? C10 C11 C6 118.0(4) . . ? C10 C11 C15 118.8(4) . . ? C6 C11 C15 123.2(3) . . ? C7 C12 C13 112.4(4) . . ? C7 C12 C14 112.9(4) . . ? C13 C12 C14 109.9(4) . . ? C11 C15 C17 110.7(4) . . ? C11 C15 C16 112.7(4) . . ? C17 C15 C16 110.8(4) . . ? C19 C18 C23 121.2(3) . . ? C19 C18 N2 120.3(3) . . ? C23 C18 N2 118.5(3) . . ? C20 C19 C18 117.8(4) . . ? C20 C19 C24 120.9(4) . . ? C18 C19 C24 121.3(4) . . ? C21 C20 C19 121.4(4) . . ? C20 C21 C22 120.7(4) . . ? C21 C22 C23 121.3(5) . . ? C22 C23 C18 117.6(4) . . ? C22 C23 C27 119.9(4) . . ? C18 C23 C27 122.4(3) . . ? C19 C24 C26 113.8(4) . . ? C19 C24 C25 111.0(4) . . ? C26 C24 C25 110.0(4) . . ? C23 C27 C29 113.1(3) . . ? C23 C27 C28 112.1(3) . . ? C29 C27 C28 109.6(4) . . ? C30 O1 Y1 120.0(2) . . ? C30 O1 Y1 127.9(2) . 3_566 ? Y1 O1 Y1 111.22(10) . 3_566 ? C31 C32 C33 121.9(5) . . ? C31 C32 C37 118.0(5) . . ? C33 C32 C37 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C37 C36 C35 120.0 . . ? C36 C37 C32 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.034 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.097 #===END