# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C224 H112 N16 O16 Y' _chemical_formula_weight 3372.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 4' _symmetry_space_group_name_Hall 'I 4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 21.5507(5) _cell_length_b 21.5507(5) _cell_length_c 22.5192(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10458.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2978 _cell_measurement_theta_min 3.4991 _cell_measurement_theta_max 63.7715 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3470 _exptl_absorpt_coefficient_mu 0.882 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8433 _exptl_absorpt_correction_T_max 0.9169 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8391 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 63.87 _reflns_number_total 5923 _reflns_number_gt 5368 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.414 1731 481 ' ' 2 0.000 0.000 0.928 22 8 ' ' 3 0.500 0.500 0.914 1731 481 ' ' 4 0.500 0.500 0.428 22 8 ' ' _platon_squeeze_details In this compound, the unit cell includes a large region of disordered solvent molecules, which could not be modeled as discrete atomic sites. We employed PLATON/SQUEEZE to calculate the diffraction contribution of the solvent molecules and, thereby, to produce a set of solvent-free diffraction intensities. The SQUEEZE calculations showed a total solvent accessible area volume of 1731 A^3^ in this compound and the residual electron density amounted to 481 electron per unit cell, corresponding to nearly 8 molecules of CH2Cl2 and 8 molecules of CH3OH (about 2 CH2Cl2 and 2 CH3OH molecules per asymmetric unit). B Alert (a)Ratio of Maximum / Minimum Residual Density .... 5.79 Explain There are some large residual Q peaks nearby the metal atoms Y, leading to large ratio of maximum / minimum residual density. ; _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^)+(0.1018P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.057(16) _refine_ls_number_reflns 5923 _refine_ls_number_parameters 580 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _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 N2A N 0.41675(17) 0.36740(17) 0.55874(19) 0.0384(8) Uani 1 1 d . . . Y1 Y 0.5000 0.5000 0.62691(3) 0.0359(2) Uani 1 4 d S . . C1A C 0.3863(2) 0.4217(2) 0.5602(2) 0.0365(10) Uani 1 1 d . . . C8A C 0.3639(2) 0.5221(2) 0.5593(2) 0.0382(10) Uani 1 1 d . . . C7A C 0.3040(2) 0.4883(2) 0.5542(2) 0.0410(10) Uani 1 1 d . . . C3A C 0.2731(2) 0.3798(2) 0.5565(2) 0.0397(10) Uani 1 1 d . . . H3A H 0.2828 0.3369 0.5585 0.048 Uiso 1 1 calc R . . C2A C 0.3194(2) 0.4262(2) 0.5556(2) 0.0384(10) Uani 1 1 d . . . N1A N 0.41149(17) 0.47962(17) 0.56524(19) 0.0384(8) Uani 1 1 d . . . C4A C 0.2126(2) 0.4012(2) 0.5542(3) 0.0422(10) Uani 1 1 d . . . C6A C 0.2445(2) 0.5087(2) 0.5491(2) 0.0424(11) Uani 1 1 d . . . H6A H 0.2351 0.5517 0.5466 0.051 Uiso 1 1 calc R . . N1 N 0.55166(17) 0.57473(17) 0.68818(18) 0.0369(8) Uani 1 1 d . . . C5A C 0.1975(2) 0.4636(2) 0.5476(3) 0.0432(11) Uani 1 1 d . . . C2 C 0.6359(2) 0.6404(2) 0.6994(2) 0.0419(10) Uani 1 1 d . . . O4 O 0.13742(14) 0.48532(15) 0.54350(18) 0.0447(8) Uani 1 1 d . . . C20A C 0.0203(2) 0.4027(2) 0.6314(3) 0.0480(11) Uani 1 1 d . . . C7 C 0.5833(2) 0.6773(2) 0.7017(2) 0.0406(10) Uani 1 1 d . . . C28A C 0.1210(2) 0.3665(2) 0.6008(3) 0.0472(12) Uani 1 1 d . . . N2 N 0.65397(18) 0.52825(17) 0.69589(19) 0.0392(8) Uani 1 1 d . . . C17A C 0.0131(2) 0.3873(3) 0.4823(3) 0.0495(12) Uani 1 1 d . . . C12A C 0.0130(3) 0.4065(3) 0.4228(3) 0.0567(14) Uani 1 1 d . . . C9A C 0.0983(2) 0.4571(2) 0.5026(3) 0.0457(11) Uani 1 1 d . . . C6 C 0.5873(2) 0.7406(2) 0.7086(2) 0.0443(11) Uani 1 1 d . . . H6 H 0.5510 0.7655 0.7116 0.053 Uiso 1 1 calc R . . C10A C 0.0992(2) 0.4768(2) 0.4438(3) 0.0524(13) Uani 1 1 d . . . H10 H 0.1283 0.5073 0.4313 0.063 Uiso 1 1 calc R . . C26A C 0.0926(3) 0.3585(3) 0.7034(3) 0.0547(13) Uani 1 1 d . . . H26 H 0.1023 0.3466 0.7430 0.066 Uiso 1 1 calc R . . C25A C 0.0349(3) 0.3872(2) 0.6902(3) 0.0520(13) Uani 1 1 d . . . C18A C 0.0565(2) 0.4123(2) 0.5238(3) 0.0450(11) Uani 1 1 d . . . C16A C -0.0314(3) 0.3419(3) 0.4994(3) 0.0584(15) Uani 1 1 d . . . H16 H -0.0312 0.3267 0.5390 0.070 Uiso 1 1 calc R . . C1 C 0.6141(2) 0.5768(2) 0.6937(2) 0.0397(11) Uani 1 1 d . . . C19A C 0.0637(2) 0.3916(2) 0.5849(3) 0.0480(13) Uani 1 1 d . . . C11A C 0.0582(3) 0.4520(3) 0.4038(3) 0.0564(14) Uani 1 1 d . . . H11 H 0.0594 0.4647 0.3634 0.068 Uiso 1 1 calc R . . C21A C -0.0372(2) 0.4337(2) 0.6200(3) 0.0495(12) Uani 1 1 d . . . H21 H -0.0488 0.4436 0.5804 0.059 Uiso 1 1 calc R . . C24A C -0.0075(3) 0.4016(3) 0.7366(3) 0.0561(14) Uani 1 1 d . . . H24 H 0.0010 0.3892 0.7763 0.067 Uiso 1 1 calc R . . C22A C -0.0754(3) 0.4490(3) 0.6660(3) 0.0558(14) Uani 1 1 d . . . H22 H -0.1129 0.4708 0.6581 0.067 Uiso 1 1 calc R . . C14A C -0.0736(4) 0.3407(4) 0.4010(4) 0.081(2) Uani 1 1 d . . . H14 H -0.1036 0.3255 0.3737 0.097 Uiso 1 1 calc R . . C23A C -0.0607(3) 0.4336(3) 0.7236(3) 0.0592(15) Uani 1 1 d . . . H23 H -0.0879 0.4453 0.7548 0.071 Uiso 1 1 calc R . . C13A C -0.0307(3) 0.3822(4) 0.3828(4) 0.0714(17) Uani 1 1 d . . . H13 H -0.0301 0.3951 0.3425 0.086 Uiso 1 1 calc R . . C15A C -0.0740(3) 0.3199(4) 0.4607(4) 0.080(2) Uani 1 1 d . . . H15 H -0.1042 0.2906 0.4734 0.095 Uiso 1 1 calc R . . O3 O 0.16530(15) 0.35593(15) 0.55665(19) 0.0469(8) Uani 1 1 d . . . C8 C 0.5302(2) 0.6350(2) 0.6944(2) 0.0394(10) Uani 1 1 d . . . C27A C 0.1341(3) 0.3480(2) 0.6586(3) 0.0519(13) Uani 1 1 d . . . H27 H 0.1724 0.3280 0.6670 0.062 Uiso 1 1 calc R . . C3 C 0.6947(2) 0.6656(2) 0.7011(2) 0.0412(10) Uani 1 1 d . . . H3AA H 0.7306 0.6400 0.7003 0.049 Uiso 1 1 calc R . . C4 C 0.6995(2) 0.7300(2) 0.7039(2) 0.0422(10) Uani 1 1 d . . . C5 C 0.6461(2) 0.7669(2) 0.7111(3) 0.0450(11) Uani 1 1 d . . . O2 O 0.75844(14) 0.75538(15) 0.70237(18) 0.0463(8) Uani 1 1 d . . . O1 O 0.65006(15) 0.82992(15) 0.71891(18) 0.0478(8) Uani 1 1 d . . . C9 C 0.7704(2) 0.8060(2) 0.6650(3) 0.0460(12) Uani 1 1 d . . . C10 C 0.7884(2) 0.7945(2) 0.6070(3) 0.0495(13) Uani 1 1 d . . . H10B H 0.7884 0.7532 0.5923 0.059 Uiso 1 1 calc R . . C19 C 0.7468(2) 0.8724(2) 0.7501(3) 0.0443(11) Uani 1 1 d . . . C20 C 0.7851(3) 0.8964(2) 0.7966(3) 0.0516(13) Uani 1 1 d . . . C28 C 0.6884(2) 0.8518(2) 0.7651(3) 0.0459(11) Uani 1 1 d . . . C27 C 0.6656(3) 0.8528(2) 0.8215(3) 0.0530(13) Uani 1 1 d . . . H27A H 0.6252 0.8370 0.8293 0.064 Uiso 1 1 calc R . . C18 C 0.7674(2) 0.8655(2) 0.6882(3) 0.0456(11) Uani 1 1 d . . . C17 C 0.7837(3) 0.9165(3) 0.6506(3) 0.0522(13) Uani 1 1 d . . . C25 C 0.7618(3) 0.8990(3) 0.8548(3) 0.0557(13) Uani 1 1 d . . . C11 C 0.8060(3) 0.8425(3) 0.5710(3) 0.0568(14) Uani 1 1 d . . . H11A H 0.8199 0.8340 0.5317 0.068 Uiso 1 1 calc R . . C15 C 0.7938(3) 1.0263(2) 0.6326(4) 0.0713(18) Uani 1 1 d . . . H15A H 0.7904 1.0679 0.6462 0.086 Uiso 1 1 calc R . . C24 C 0.7986(4) 0.9229(3) 0.9007(3) 0.0700(17) Uani 1 1 d . . . H24A H 0.7820 0.9268 0.9396 0.084 Uiso 1 1 calc R . . C26 C 0.7002(3) 0.8760(3) 0.8667(3) 0.0582(14) Uani 1 1 d . . . H26A H 0.6839 0.8772 0.9059 0.070 Uiso 1 1 calc R . . C16 C 0.7771(3) 0.9782(3) 0.6700(3) 0.0609(14) Uani 1 1 d . . . H16A H 0.7614 0.9867 0.7086 0.073 Uiso 1 1 calc R . . C13 C 0.8206(4) 0.9564(3) 0.5555(3) 0.0683(16) Uani 1 1 d . . . H13A H 0.8357 0.9494 0.5165 0.082 Uiso 1 1 calc R . . C12 C 0.8038(3) 0.9042(3) 0.5914(3) 0.0577(15) Uani 1 1 d . . . C22 C 0.8819(3) 0.9371(3) 0.8328(4) 0.0697(17) Uani 1 1 d . . . H22A H 0.9233 0.9503 0.8256 0.084 Uiso 1 1 calc R . . C21 C 0.8475(3) 0.9150(3) 0.7866(3) 0.0614(15) Uani 1 1 d . . . H21A H 0.8650 0.9121 0.7480 0.074 Uiso 1 1 calc R . . C23 C 0.8582(4) 0.9406(4) 0.8896(4) 0.0760(19) Uani 1 1 d . . . H23A H 0.8835 0.9555 0.9211 0.091 Uiso 1 1 calc R . . C14 C 0.8156(4) 1.0148(3) 0.5752(4) 0.078(2) Uani 1 1 d . . . H14A H 0.8268 1.0484 0.5501 0.094 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 N2A 0.0311(19) 0.0329(19) 0.051(2) -0.0003(17) 0.0004(16) 0.0015(14) Y1 0.0306(2) 0.0306(2) 0.0465(4) 0.000 0.000 0.000 C1A 0.033(2) 0.032(2) 0.045(3) -0.003(2) -0.003(2) -0.0057(18) C8A 0.030(2) 0.036(2) 0.049(3) -0.002(2) 0.001(2) 0.0009(17) C7A 0.031(2) 0.043(2) 0.049(3) 0.002(2) 0.001(2) -0.0071(18) C3A 0.037(2) 0.032(2) 0.050(3) -0.001(2) -0.002(2) -0.0037(17) C2A 0.034(2) 0.036(2) 0.045(2) 0.0010(19) 0.001(2) -0.0006(17) N1A 0.0311(18) 0.0305(18) 0.053(2) -0.0006(16) -0.0027(16) 0.0001(14) C4A 0.033(2) 0.036(2) 0.058(3) -0.003(2) 0.003(2) -0.0021(18) C6A 0.032(2) 0.037(2) 0.059(3) -0.003(2) 0.000(2) -0.0012(17) N1 0.037(2) 0.0316(18) 0.042(2) -0.0100(15) -0.0033(16) -0.0015(14) C5A 0.029(2) 0.040(2) 0.060(3) -0.001(2) 0.000(2) -0.0014(18) C2 0.040(2) 0.038(2) 0.048(3) -0.002(2) -0.003(2) 0.0014(19) O4 0.0281(15) 0.0345(16) 0.072(2) -0.0033(16) -0.0009(15) 0.0024(11) C20A 0.040(2) 0.037(2) 0.067(3) 0.003(3) -0.002(3) -0.0083(17) C7 0.035(2) 0.041(2) 0.046(3) -0.003(2) 0.003(2) -0.0022(18) C28A 0.035(2) 0.039(2) 0.068(3) -0.003(2) 0.001(2) -0.007(2) N2 0.037(2) 0.032(2) 0.049(2) -0.0008(16) -0.0034(17) 0.0003(15) C17A 0.031(2) 0.050(3) 0.068(4) 0.004(3) -0.005(2) 0.000(2) C12A 0.044(3) 0.057(3) 0.069(4) -0.007(3) -0.001(3) 0.005(2) C9A 0.030(2) 0.040(2) 0.067(3) -0.002(2) 0.005(2) 0.0014(18) C6 0.039(2) 0.037(2) 0.056(3) -0.008(2) -0.005(2) 0.0056(18) C10A 0.037(2) 0.044(3) 0.076(4) 0.008(3) 0.006(3) 0.003(2) C26A 0.048(3) 0.054(3) 0.062(3) 0.009(3) -0.002(3) -0.003(2) C25A 0.043(3) 0.039(3) 0.074(4) 0.006(2) 0.000(3) -0.006(2) C18A 0.034(2) 0.037(2) 0.064(3) 0.002(2) 0.004(2) 0.0002(18) C16A 0.044(3) 0.052(3) 0.079(4) 0.008(3) -0.003(3) -0.010(2) C1 0.038(2) 0.040(3) 0.041(3) -0.004(2) -0.001(2) -0.0004(19) C19A 0.034(2) 0.032(2) 0.078(4) -0.001(2) 0.000(2) -0.0055(18) C11A 0.053(3) 0.058(3) 0.058(3) 0.010(3) 0.000(3) 0.007(3) C21A 0.034(2) 0.047(2) 0.067(4) 0.008(3) 0.003(3) -0.0004(18) C24A 0.048(3) 0.061(3) 0.060(3) 0.003(3) 0.002(3) -0.006(2) C22A 0.041(3) 0.057(3) 0.070(4) 0.003(3) 0.005(3) -0.004(2) C14A 0.077(5) 0.085(5) 0.080(5) -0.008(4) -0.026(4) -0.018(4) C23A 0.046(3) 0.056(3) 0.075(4) -0.004(3) 0.011(3) -0.009(2) C13A 0.068(4) 0.078(4) 0.069(4) -0.008(3) -0.012(3) -0.006(3) C15A 0.055(4) 0.072(4) 0.112(6) 0.002(4) -0.012(4) -0.022(3) O3 0.0322(16) 0.0360(16) 0.073(2) 0.0006(16) -0.0003(16) -0.0040(12) C8 0.046(3) 0.030(2) 0.043(3) -0.001(2) 0.001(2) -0.0044(19) C27A 0.041(3) 0.039(3) 0.076(4) 0.005(3) -0.003(3) -0.001(2) C3 0.036(2) 0.035(2) 0.053(3) -0.005(2) -0.002(2) -0.0022(18) C4 0.033(2) 0.043(3) 0.050(3) -0.004(2) 0.000(2) 0.0007(18) C5 0.039(2) 0.037(2) 0.059(3) -0.005(2) 0.004(2) 0.0005(19) O2 0.0312(16) 0.0394(17) 0.068(2) -0.0010(16) 0.0037(15) -0.0022(12) O1 0.0376(17) 0.0340(16) 0.072(2) -0.0044(16) -0.0017(16) 0.0018(13) C9 0.035(2) 0.038(2) 0.065(3) 0.002(2) -0.006(2) -0.0071(18) C10 0.046(3) 0.040(3) 0.062(3) -0.010(2) 0.001(2) -0.006(2) C19 0.041(2) 0.030(2) 0.063(3) -0.001(2) 0.001(2) -0.0004(18) C20 0.057(3) 0.035(2) 0.063(3) 0.000(2) -0.007(3) 0.001(2) C28 0.048(3) 0.031(2) 0.059(3) -0.008(2) -0.007(2) 0.0029(19) C27 0.058(3) 0.037(2) 0.065(4) -0.003(2) 0.011(3) 0.002(2) C18 0.040(2) 0.041(3) 0.056(3) -0.001(2) -0.003(2) -0.0033(19) C17 0.051(3) 0.040(3) 0.066(3) 0.004(2) -0.003(3) -0.007(2) C25 0.064(3) 0.041(3) 0.062(4) -0.005(2) -0.004(3) 0.000(2) C11 0.063(3) 0.055(3) 0.053(3) -0.001(3) 0.003(3) 0.004(3) C15 0.079(4) 0.034(2) 0.101(5) 0.003(3) 0.016(4) -0.008(2) C24 0.088(5) 0.065(4) 0.058(4) 0.001(3) -0.015(3) -0.004(3) C26 0.072(4) 0.046(3) 0.057(3) -0.004(2) 0.005(3) 0.009(3) C16 0.059(3) 0.052(3) 0.072(4) -0.002(3) 0.000(3) 0.004(2) C13 0.085(4) 0.062(4) 0.057(3) 0.009(3) 0.005(3) -0.009(3) C12 0.062(3) 0.047(3) 0.064(4) 0.006(3) 0.000(3) -0.010(2) C22 0.062(4) 0.066(4) 0.081(5) -0.005(3) -0.019(3) -0.007(3) C21 0.054(3) 0.049(3) 0.082(4) -0.001(3) -0.008(3) -0.001(2) C23 0.084(5) 0.073(4) 0.071(4) -0.009(3) -0.017(4) -0.010(4) C14 0.100(5) 0.048(3) 0.087(5) 0.012(3) 0.006(4) -0.013(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 N2A C8A 1.319(6) 3_655 ? N2A C1A 1.342(6) . ? Y1 N1 2.395(4) . ? Y1 N1 2.395(4) 3_655 ? Y1 N1 2.395(4) 4_565 ? Y1 N1 2.395(4) 2_665 ? Y1 N1A 2.400(4) 4_565 ? Y1 N1A 2.400(4) 2_665 ? Y1 N1A 2.400(4) . ? Y1 N1A 2.400(4) 3_655 ? C1A N1A 1.366(6) . ? C1A C2A 1.450(7) . ? C8A N2A 1.319(6) 4_565 ? C8A N1A 1.382(6) . ? C8A C7A 1.488(6) . ? C7A C6A 1.361(7) . ? C7A C2A 1.378(7) . ? C3A C4A 1.382(7) . ? C3A C2A 1.412(7) . ? C4A C5A 1.392(7) . ? C4A O3 1.412(6) . ? C6A C5A 1.404(7) . ? N1 C1 1.352(6) . ? N1 C8 1.386(6) . ? C5A O4 1.380(6) . ? C2 C3 1.380(7) . ? C2 C7 1.384(7) . ? C2 C1 1.456(7) . ? O4 C9A 1.388(7) . ? C20A C25A 1.402(10) . ? C20A C19A 1.424(9) . ? C20A C21A 1.432(7) . ? C7 C6 1.376(7) . ? C7 C8 1.471(7) . ? C28A C27A 1.389(9) . ? C28A C19A 1.394(8) . ? C28A O3 1.398(7) . ? N2 C8 1.325(7) 4_565 ? N2 C1 1.354(7) . ? C17A C12A 1.403(10) . ? C17A C16A 1.423(8) . ? C17A C18A 1.427(8) . ? C12A C13A 1.406(10) . ? C12A C11A 1.446(9) . ? C9A C10A 1.392(9) . ? C9A C18A 1.403(7) . ? C6 C5 1.389(7) . ? C10A C11A 1.371(9) . ? C26A C27A 1.367(9) . ? C26A C25A 1.421(8) . ? C25A C24A 1.422(9) . ? C18A C19A 1.456(9) . ? C16A C15A 1.352(10) . ? C21A C22A 1.364(9) . ? C24A C23A 1.369(9) . ? C22A C23A 1.376(10) . ? C14A C13A 1.349(12) . ? C14A C15A 1.417(13) . ? C8 N2 1.325(7) 3_655 ? C3 C4 1.394(7) . ? C4 O2 1.384(6) . ? C4 C5 1.409(7) . ? C5 O1 1.372(6) . ? O2 C9 1.402(7) . ? O1 C28 1.409(7) . ? C9 C10 1.385(9) . ? C9 C18 1.386(8) . ? C10 C11 1.368(9) . ? C19 C28 1.378(8) . ? C19 C20 1.431(8) . ? C19 C18 1.470(8) . ? C20 C25 1.404(9) . ? C20 C21 1.420(9) . ? C28 C27 1.362(9) . ? C27 C26 1.357(9) . ? C18 C17 1.433(8) . ? C17 C16 1.406(9) . ? C17 C12 1.426(9) . ? C25 C24 1.401(10) . ? C25 C26 1.442(9) . ? C11 C12 1.408(9) . ? C15 C16 1.384(10) . ? C15 C14 1.398(13) . ? C24 C23 1.362(12) . ? C13 C14 1.338(11) . ? C13 C12 1.432(10) . ? C22 C21 1.362(10) . ? C22 C23 1.381(12) . ? 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 C8A N2A C1A 122.5(4) 3_655 . ? N1 Y1 N1 70.62(10) . 3_655 ? N1 Y1 N1 70.62(10) . 4_565 ? N1 Y1 N1 109.7(2) 3_655 4_565 ? N1 Y1 N1 109.7(2) . 2_665 ? N1 Y1 N1 70.62(10) 3_655 2_665 ? N1 Y1 N1 70.62(10) 4_565 2_665 ? N1 Y1 N1A 83.34(14) . 4_565 ? N1 Y1 N1A 80.84(14) 3_655 4_565 ? N1 Y1 N1A 145.67(13) 4_565 4_565 ? N1 Y1 N1A 141.51(13) 2_665 4_565 ? N1 Y1 N1A 80.84(14) . 2_665 ? N1 Y1 N1A 141.51(13) 3_655 2_665 ? N1 Y1 N1A 83.34(14) 4_565 2_665 ? N1 Y1 N1A 145.67(13) 2_665 2_665 ? N1A Y1 N1A 70.44(10) 4_565 2_665 ? N1 Y1 N1A 145.67(13) . . ? N1 Y1 N1A 83.34(14) 3_655 . ? N1 Y1 N1A 141.51(13) 4_565 . ? N1 Y1 N1A 80.84(14) 2_665 . ? N1A Y1 N1A 70.44(10) 4_565 . ? N1A Y1 N1A 109.3(2) 2_665 . ? N1 Y1 N1A 141.51(13) . 3_655 ? N1 Y1 N1A 145.67(13) 3_655 3_655 ? N1 Y1 N1A 80.84(13) 4_565 3_655 ? N1 Y1 N1A 83.34(14) 2_665 3_655 ? N1A Y1 N1A 109.3(2) 4_565 3_655 ? N1A Y1 N1A 70.44(10) 2_665 3_655 ? N1A Y1 N1A 70.44(10) . 3_655 ? N2A C1A N1A 127.2(4) . . ? N2A C1A C2A 122.9(4) . . ? N1A C1A C2A 109.9(4) . . ? N2A C8A N1A 128.4(4) 4_565 . ? N2A C8A C7A 122.6(4) 4_565 . ? N1A C8A C7A 109.0(4) . . ? C6A C7A C2A 122.9(4) . . ? C6A C7A C8A 131.7(5) . . ? C2A C7A C8A 105.4(4) . . ? C4A C3A C2A 115.4(4) . . ? C7A C2A C3A 121.2(4) . . ? C7A C2A C1A 107.8(4) . . ? C3A C2A C1A 130.9(4) . . ? C1A N1A C8A 107.7(4) . . ? C1A N1A Y1 122.1(3) . . ? C8A N1A Y1 121.6(3) . . ? C3A C4A C5A 123.1(4) . . ? C3A C4A O3 116.7(4) . . ? C5A C4A O3 120.2(4) . . ? C7A C6A C5A 117.2(4) . . ? C1 N1 C8 107.0(4) . . ? C1 N1 Y1 122.5(3) . . ? C8 N1 Y1 122.3(3) . . ? O4 C5A C4A 123.6(4) . . ? O4 C5A C6A 116.3(4) . . ? C4A C5A C6A 119.9(4) . . ? C3 C2 C7 121.8(4) . . ? C3 C2 C1 131.9(4) . . ? C7 C2 C1 106.3(4) . . ? C5A O4 C9A 117.7(4) . . ? C25A C20A C19A 120.5(5) . . ? C25A C20A C21A 118.4(6) . . ? C19A C20A C21A 121.0(6) . . ? C6 C7 C2 121.4(4) . . ? C6 C7 C8 132.4(4) . . ? C2 C7 C8 106.1(4) . . ? C27A C28A C19A 122.1(5) . . ? C27A C28A O3 118.7(5) . . ? C19A C28A O3 119.0(5) . . ? C8 N2 C1 122.5(4) 4_565 . ? C12A C17A C16A 117.4(5) . . ? C12A C17A C18A 120.9(5) . . ? C16A C17A C18A 121.7(6) . . ? C17A C12A C13A 120.2(6) . . ? C17A C12A C11A 118.9(6) . . ? C13A C12A C11A 120.9(6) . . ? O4 C9A C10A 119.3(4) . . ? O4 C9A C18A 117.8(5) . . ? C10A C9A C18A 122.8(5) . . ? C7 C6 C5 117.8(4) . . ? C11A C10A C9A 119.9(5) . . ? C27A C26A C25A 119.3(6) . . ? C20A C25A C26A 119.8(6) . . ? C20A C25A C24A 119.9(5) . . ? C26A C25A C24A 120.3(6) . . ? C9A C18A C17A 117.3(5) . . ? C9A C18A C19A 117.6(5) . . ? C17A C18A C19A 125.0(5) . . ? C15A C16A C17A 121.7(7) . . ? N1 C1 N2 127.6(4) . . ? N1 C1 C2 111.1(4) . . ? N2 C1 C2 121.3(4) . . ? C28A C19A C20A 117.2(6) . . ? C28A C19A C18A 117.1(5) . . ? C20A C19A C18A 125.0(5) . . ? C10A C11A C12A 120.2(6) . . ? C22A C21A C20A 120.0(6) . . ? C23A C24A C25A 119.4(6) . . ? C21A C22A C23A 121.2(6) . . ? C13A C14A C15A 120.1(7) . . ? C24A C23A C22A 121.1(6) . . ? C14A C13A C12A 120.8(7) . . ? C16A C15A C14A 119.7(7) . . ? C28A O3 C4A 114.2(4) . . ? N2 C8 N1 127.5(4) 3_655 . ? N2 C8 C7 123.1(4) 3_655 . ? N1 C8 C7 109.4(4) . . ? C26A C27A C28A 120.7(5) . . ? C2 C3 C4 117.3(4) . . ? O2 C4 C3 117.4(4) . . ? O2 C4 C5 122.0(4) . . ? C3 C4 C5 120.5(4) . . ? O1 C5 C6 117.8(4) . . ? O1 C5 C4 121.5(4) . . ? C6 C5 C4 120.7(4) . . ? C4 O2 C9 119.5(4) . . ? C5 O1 C28 117.5(4) . . ? C10 C9 C18 122.3(5) . . ? C10 C9 O2 118.5(5) . . ? C18 C9 O2 119.1(5) . . ? C11 C10 C9 120.2(5) . . ? C28 C19 C20 117.7(5) . . ? C28 C19 C18 118.4(5) . . ? C20 C19 C18 123.9(5) . . ? C25 C20 C21 118.4(6) . . ? C25 C20 C19 119.4(5) . . ? C21 C20 C19 122.1(6) . . ? C27 C28 C19 123.6(5) . . ? C27 C28 O1 118.9(5) . . ? C19 C28 O1 117.5(5) . . ? C26 C27 C28 120.4(5) . . ? C9 C18 C17 118.4(5) . . ? C9 C18 C19 117.7(5) . . ? C17 C18 C19 123.9(5) . . ? C16 C17 C12 119.9(6) . . ? C16 C17 C18 121.0(6) . . ? C12 C17 C18 119.0(5) . . ? C24 C25 C20 120.0(6) . . ? C24 C25 C26 120.7(6) . . ? C20 C25 C26 119.3(5) . . ? C10 C11 C12 120.6(6) . . ? C16 C15 C14 121.1(6) . . ? C23 C24 C25 120.2(7) . . ? C27 C26 C25 119.6(6) . . ? C15 C16 C17 119.5(7) . . ? C14 C13 C12 122.1(7) . . ? C11 C12 C17 119.5(6) . . ? C11 C12 C13 123.3(6) . . ? C17 C12 C13 117.2(6) . . ? C21 C22 C23 121.7(7) . . ? C22 C21 C20 119.5(7) . . ? C24 C23 C22 120.2(7) . . ? C13 C14 C15 120.0(6) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 63.87 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.212 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.092 _iucr_refine_instructions_details ; TITL 2 in I4 CELL 1.54178 21.5507 21.5507 22.5192 90.000 90.000 90.000 ZERR 2.00 0.0005 0.0005 0.0014 0.000 0.000 0.000 LATT -2 SYMM - X, - Y, Z SYMM - Y, X, Z SYMM Y, - X, Z SFAC C H N O Y UNIT 448 224 32 32 2 MERG 2 FMAP 2 PLAN 10 SIZE 0.10 0.15 0.20 ACTA BOND L.S. 6 TEMP -120.00 WGHT 0.101800 FVAR 0.43577 N2A 3 0.416748 0.367397 0.558742 11.00000 0.03111 0.03286 = 0.05118 -0.00030 0.00042 0.00155 Y1 5 0.500000 0.500000 0.626909 10.25000 0.03065 0.03065 = 0.04646 0.00000 0.00000 0.00000 C1A 1 0.386331 0.421698 0.560190 11.00000 0.03252 0.03165 = 0.04530 -0.00268 -0.00260 -0.00572 C8A 1 0.363912 0.522141 0.559306 11.00000 0.03015 0.03569 = 0.04870 -0.00216 0.00062 0.00089 C7A 1 0.303996 0.488252 0.554206 11.00000 0.03068 0.04279 = 0.04938 0.00162 0.00054 -0.00709 C3A 1 0.273070 0.379794 0.556498 11.00000 0.03705 0.03165 = 0.05030 -0.00119 -0.00197 -0.00372 AFIX 43 H3A 2 0.282797 0.336852 0.558538 11.00000 -1.20000 AFIX 0 C2A 1 0.319357 0.426187 0.555625 11.00000 0.03377 0.03647 = 0.04486 0.00104 0.00087 -0.00059 N1A 3 0.411494 0.479619 0.565243 11.00000 0.03113 0.03048 = 0.05349 -0.00058 -0.00272 0.00008 C4A 1 0.212636 0.401176 0.554179 11.00000 0.03296 0.03597 = 0.05769 -0.00342 0.00292 -0.00213 C6A 1 0.244485 0.508736 0.549063 11.00000 0.03164 0.03673 = 0.05876 -0.00300 0.00015 -0.00117 AFIX 43 H6A 2 0.235128 0.551736 0.546592 11.00000 -1.20000 AFIX 0 N1 3 0.551659 0.574728 0.688180 11.00000 0.03693 0.03162 = 0.04214 -0.01002 -0.00334 -0.00149 C5A 1 0.197538 0.463617 0.547568 11.00000 0.02915 0.04045 = 0.05996 -0.00149 0.00049 -0.00142 C2 1 0.635854 0.640437 0.699412 11.00000 0.03971 0.03812 = 0.04773 -0.00245 -0.00278 0.00136 O4 4 0.137421 0.485323 0.543498 11.00000 0.02813 0.03447 = 0.07157 -0.00329 -0.00092 0.00241 C20A 1 0.020335 0.402748 0.631410 11.00000 0.04007 0.03713 = 0.06676 0.00317 -0.00211 -0.00827 C7 1 0.583274 0.677253 0.701724 11.00000 0.03459 0.04094 = 0.04640 -0.00252 0.00324 -0.00219 C28A 1 0.120970 0.366450 0.600813 11.00000 0.03472 0.03866 = 0.06829 -0.00343 0.00142 -0.00735 N2 3 0.653969 0.528255 0.695886 11.00000 0.03668 0.03246 = 0.04862 -0.00082 -0.00342 0.00026 C17A 1 0.013134 0.387293 0.482328 11.00000 0.03075 0.05009 = 0.06773 0.00436 -0.00519 -0.00016 C12A 1 0.013028 0.406548 0.422827 11.00000 0.04366 0.05734 = 0.06922 -0.00736 -0.00061 0.00455 C9A 1 0.098300 0.457110 0.502646 11.00000 0.02953 0.04026 = 0.06721 -0.00219 0.00524 0.00143 C6 1 0.587257 0.740578 0.708642 11.00000 0.03925 0.03717 = 0.05649 -0.00785 -0.00515 0.00557 AFIX 43 H6 2 0.551010 0.765469 0.711636 11.00000 -1.20000 AFIX 0 C10A 1 0.099231 0.476783 0.443762 11.00000 0.03669 0.04446 = 0.07615 0.00841 0.00605 0.00307 AFIX 43 H10 2 0.128254 0.507315 0.431334 11.00000 -1.20000 AFIX 0 C26A 1 0.092615 0.358459 0.703404 11.00000 0.04808 0.05350 = 0.06247 0.00893 -0.00204 -0.00285 AFIX 43 H26 2 0.102267 0.346591 0.742969 11.00000 -1.20000 AFIX 0 C25A 1 0.034905 0.387215 0.690222 11.00000 0.04304 0.03865 = 0.07431 0.00616 -0.00005 -0.00589 C18A 1 0.056532 0.412285 0.523750 11.00000 0.03359 0.03729 = 0.06403 0.00164 0.00352 0.00025 C16A 1 -0.031438 0.341923 0.499362 11.00000 0.04385 0.05248 = 0.07887 0.00759 -0.00310 -0.01009 AFIX 43 H16 2 -0.031241 0.326711 0.538956 11.00000 -1.20000 AFIX 0 C1 1 0.614093 0.576773 0.693660 11.00000 0.03806 0.03962 = 0.04137 -0.00412 -0.00107 -0.00036 C19A 1 0.063723 0.391619 0.584921 11.00000 0.03364 0.03220 = 0.07827 -0.00058 0.00012 -0.00546 C11A 1 0.058185 0.452007 0.403754 11.00000 0.05332 0.05758 = 0.05834 0.01020 -0.00025 0.00743 AFIX 43 H11 2 0.059409 0.464737 0.363382 11.00000 -1.20000 AFIX 0 C21A 1 -0.037203 0.433732 0.619989 11.00000 0.03406 0.04712 = 0.06741 0.00810 0.00269 -0.00041 AFIX 43 H21 2 -0.048761 0.443623 0.580395 11.00000 -1.20000 AFIX 0 C24A 1 -0.007497 0.401640 0.736605 11.00000 0.04776 0.06072 = 0.05987 0.00338 0.00162 -0.00574 AFIX 43 H24 2 0.001006 0.389209 0.776252 11.00000 -1.20000 AFIX 0 C22A 1 -0.075417 0.449041 0.665999 11.00000 0.04100 0.05670 = 0.06975 0.00256 0.00539 -0.00434 AFIX 43 H22 2 -0.112890 0.470758 0.658138 11.00000 -1.20000 AFIX 0 C14A 1 -0.073602 0.340727 0.401002 11.00000 0.07726 0.08468 = 0.07991 -0.00831 -0.02615 -0.01781 AFIX 43 H14 2 -0.103561 0.325452 0.373726 11.00000 -1.20000 AFIX 0 C23A 1 -0.060685 0.433607 0.723585 11.00000 0.04606 0.05625 = 0.07535 -0.00416 0.01071 -0.00919 AFIX 43 H23 2 -0.087876 0.445329 0.754837 11.00000 -1.20000 AFIX 0 C13A 1 -0.030728 0.382194 0.382835 11.00000 0.06773 0.07767 = 0.06878 -0.00776 -0.01196 -0.00590 AFIX 43 H13 2 -0.030100 0.395100 0.342502 11.00000 -1.20000 AFIX 0 C15A 1 -0.074044 0.319913 0.460666 11.00000 0.05465 0.07166 = 0.11225 0.00150 -0.01215 -0.02192 AFIX 43 H15 2 -0.104154 0.290610 0.473432 11.00000 -1.20000 AFIX 0 O3 4 0.165301 0.355933 0.556650 11.00000 0.03219 0.03601 = 0.07262 0.00058 -0.00027 -0.00398 C8 1 0.530207 0.635004 0.694440 11.00000 0.04551 0.02958 = 0.04304 -0.00122 0.00058 -0.00436 C27A 1 0.134120 0.348039 0.658571 11.00000 0.04072 0.03937 = 0.07558 0.00506 -0.00321 -0.00106 AFIX 43 H27 2 0.172372 0.327987 0.667019 11.00000 -1.20000 AFIX 0 C3 1 0.694745 0.665559 0.701069 11.00000 0.03554 0.03476 = 0.05328 -0.00470 -0.00240 -0.00223 AFIX 43 H3AA 2 0.730620 0.639954 0.700327 11.00000 -1.20000 AFIX 0 C4 1 0.699472 0.729993 0.703875 11.00000 0.03303 0.04334 = 0.05032 -0.00386 -0.00036 0.00070 C5 1 0.646053 0.766885 0.711102 11.00000 0.03875 0.03743 = 0.05883 -0.00460 0.00399 0.00049 O2 4 0.758441 0.755378 0.702365 11.00000 0.03122 0.03939 = 0.06828 -0.00101 0.00372 -0.00218 O1 4 0.650065 0.829916 0.718906 11.00000 0.03763 0.03397 = 0.07172 -0.00442 -0.00173 0.00179 C9 1 0.770442 0.806035 0.665049 11.00000 0.03494 0.03797 = 0.06499 0.00158 -0.00588 -0.00706 C10 1 0.788384 0.794534 0.607042 11.00000 0.04642 0.04006 = 0.06196 -0.01014 0.00073 -0.00617 AFIX 43 H10B 2 0.788446 0.753247 0.592258 11.00000 -1.20000 AFIX 0 C19 1 0.746818 0.872398 0.750121 11.00000 0.04072 0.02952 = 0.06273 -0.00128 0.00085 -0.00041 C20 1 0.785112 0.896430 0.796642 11.00000 0.05677 0.03468 = 0.06348 -0.00020 -0.00710 0.00123 C28 1 0.688368 0.851759 0.765119 11.00000 0.04761 0.03130 = 0.05866 -0.00786 -0.00718 0.00294 C27 1 0.665595 0.852759 0.821546 11.00000 0.05760 0.03657 = 0.06472 -0.00300 0.01140 0.00163 AFIX 43 H27A 2 0.625222 0.837046 0.829341 11.00000 -1.20000 AFIX 0 C18 1 0.767367 0.865517 0.688215 11.00000 0.03969 0.04078 = 0.05620 -0.00074 -0.00288 -0.00332 C17 1 0.783691 0.916542 0.650551 11.00000 0.05057 0.03983 = 0.06626 0.00396 -0.00272 -0.00709 C25 1 0.761804 0.898983 0.854801 11.00000 0.06374 0.04131 = 0.06200 -0.00541 -0.00376 0.00012 C11 1 0.806020 0.842456 0.570969 11.00000 0.06283 0.05483 = 0.05287 -0.00117 0.00288 0.00444 AFIX 43 H11A 2 0.819889 0.834026 0.531746 11.00000 -1.20000 AFIX 0 C15 1 0.793791 1.026329 0.632619 11.00000 0.07928 0.03363 = 0.10099 0.00315 0.01649 -0.00752 AFIX 43 H15A 2 0.790352 1.067928 0.646183 11.00000 -1.20000 AFIX 0 C24 1 0.798637 0.922934 0.900670 11.00000 0.08769 0.06462 = 0.05782 0.00055 -0.01455 -0.00429 AFIX 43 H24A 2 0.782023 0.926832 0.939567 11.00000 -1.20000 AFIX 0 C26 1 0.700196 0.876047 0.866692 11.00000 0.07195 0.04574 = 0.05686 -0.00359 0.00500 0.00854 AFIX 43 H26A 2 0.683928 0.877232 0.905884 11.00000 -1.20000 AFIX 0 C16 1 0.777148 0.978185 0.670048 11.00000 0.05863 0.05236 = 0.07165 -0.00246 0.00004 0.00434 AFIX 43 H16A 2 0.761429 0.986716 0.708606 11.00000 -1.20000 AFIX 0 C13 1 0.820585 0.956406 0.555494 11.00000 0.08521 0.06238 = 0.05720 0.00856 0.00545 -0.00856 AFIX 43 H13A 2 0.835741 0.949382 0.516455 11.00000 -1.20000 AFIX 0 C12 1 0.803816 0.904176 0.591414 11.00000 0.06190 0.04745 = 0.06366 0.00550 -0.00044 -0.00997 C22 1 0.881884 0.937059 0.832768 11.00000 0.06233 0.06609 = 0.08057 -0.00528 -0.01914 -0.00729 AFIX 43 H22A 2 0.923258 0.950320 0.825637 11.00000 -1.20000 AFIX 0 C21 1 0.847465 0.915006 0.786631 11.00000 0.05368 0.04885 = 0.08178 -0.00062 -0.00842 -0.00062 AFIX 43 H21A 2 0.865041 0.912074 0.748045 11.00000 -1.20000 AFIX 0 C23 1 0.858188 0.940635 0.889629 11.00000 0.08430 0.07255 = 0.07122 -0.00853 -0.01749 -0.00996 AFIX 43 H23A 2 0.883486 0.955479 0.921121 11.00000 -1.20000 AFIX 0 C14 1 0.815577 1.014793 0.575186 11.00000 0.09978 0.04761 = 0.08710 0.01198 0.00563 -0.01339 AFIX 43 H14A 2 0.826834 1.048419 0.550124 11.00000 -1.20000 HKLF 4 REM 2 in I4 REM R1 = 0.0644 for 5368 Fo > 4sig(Fo) and 0.0684 for all 5923 data REM 580 parameters refined using 1 restraints END ; # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.414 1731 481 ' ' 2 0.000 0.000 0.928 22 8 ' ' 3 0.500 0.500 0.914 1731 481 ' ' 4 0.500 0.500 0.428 22 8 ' ' _platon_squeeze_details ; In this compound, the unit cell includes a large region of disordered solvent molecules, which could not be modeled as discrete atomic sites. We employed PLATON/SQUEEZE to calculate the diffraction contribution of the solvent molecules and, thereby, to produce a set of solvent-free diffraction intensities. The SQUEEZE calculations showed a total solvent accessible area volume of 1731 A^3^ in this compound and the residual electron density amounted to 481 electron per unit cell, corresponding to nearly 8 molecules of CH2Cl2 and 8 molecules of CH3OH (about 2 CH2Cl2 and 2 CH3OH molecules per asymmetric unit). ; _database_code_depnum_ccdc_archive 'CCDC 941795' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C224 H112 N16 O16 Y' _chemical_formula_weight 3372.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 4' _symmetry_space_group_name_Hall 'I 4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 21.6634(5) _cell_length_b 21.6634(5) _cell_length_c 22.6033(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10607.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2363 _cell_measurement_theta_min 4.0779 _cell_measurement_theta_max 66.7934 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3470 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8119 _exptl_absorpt_correction_T_max 0.8806 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9570 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 66.90 _reflns_number_total 6246 _reflns_number_gt 4865 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.068 26 7 ' ' 2 0.000 0.000 0.582 1799 335 ' ' 3 0.500 0.500 0.083 1793 335 ' ' 4 0.500 0.500 0.568 26 7 ' ' In this compound, the unit cell includes a large region of disordered solvent molecules, which could not be modeled as discrete atomic sites. We employed PLATON/SQUEEZE to calculate the diffraction contribution of the solvent molecules and, thereby, to produce a set of solvent-free diffraction intensities. The SQUEEZE calculations showed a total solvent accessible area volume of 1789 A^3^ in this compound and the residual electron density amounted to 335 electron per unit cell, corresponding to nearly 8 molecules of CH2Cl2 (about 2 CH2Cl2 molecules per asymmetric unit). B Alert (a)Ratio of Maximum / Minimum Residual Density .... 4.54 Explain There are some large residual Q peaks nearby the metal atoms Y, leading to large ratio of maximum / minimum residual density. ; _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^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.036(19) _refine_ls_number_reflns 6246 _refine_ls_number_parameters 580 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.002 _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 0.0000 1.0000 0.87598(4) 0.0339(2) Uani 1 4 d S . . C2B C 0.1130(2) 1.0779(3) 0.9411(3) 0.0337(13) Uani 1 1 d . . . C5 C 0.1355(3) 0.9772(3) 0.9419(3) 0.0343(13) Uani 1 1 d . . . C6 C 0.1943(2) 1.0104(2) 0.9461(3) 0.0353(12) Uani 1 1 d . . . C8B C 0.2267(2) 1.1183(2) 0.9430(3) 0.0354(12) Uani 1 1 d . . . H8B H 0.2171 1.1611 0.9417 0.042 Uiso 1 1 calc R . . C3B C 0.1808(2) 1.0735(2) 0.9447(3) 0.0334(12) Uani 1 1 d . . . N1B N 0.0888(2) 1.01944(19) 0.9370(2) 0.0375(11) Uani 1 1 d . . . C7B C 0.2875(2) 1.0974(3) 0.9432(3) 0.0383(13) Uani 1 1 d . . . C7 C 0.2549(2) 0.9898(3) 0.9497(3) 0.0375(13) Uani 1 1 d . . . H7 H 0.2642 0.9470 0.9523 0.045 Uiso 1 1 calc R . . N2B N 0.0842(2) 1.1316(2) 0.9428(2) 0.0353(10) Uani 1 1 d . . . N1A N -0.0514(2) 0.9246(2) 0.8142(2) 0.0388(11) Uani 1 1 d . . . C6B C 0.3020(3) 1.0342(3) 0.9492(3) 0.0408(13) Uani 1 1 d . . . C4A C -0.1359(3) 0.8602(3) 0.8018(3) 0.0375(13) Uani 1 1 d . . . O1B O 0.36148(16) 1.01312(17) 0.9516(2) 0.0415(10) Uani 1 1 d . . . C20B C 0.4782(3) 1.0967(3) 0.8650(3) 0.0449(16) Uani 1 1 d . . . C3A C -0.0832(2) 0.8239(3) 0.8000(3) 0.0359(12) Uani 1 1 d . . . C28B C 0.3784(3) 1.1325(3) 0.8952(3) 0.0461(17) Uani 1 1 d . . . N2A N -0.1537(2) 0.9724(2) 0.8061(2) 0.0355(10) Uani 1 1 d . . . C17B C 0.4847(3) 1.1108(3) 1.0146(3) 0.0512(17) Uani 1 1 d . . . C12B C 0.4833(3) 1.0907(3) 1.0731(3) 0.0537(17) Uani 1 1 d . . . C9B C 0.4007(3) 1.0404(3) 0.9925(3) 0.0456(15) Uani 1 1 d . . . C8A C -0.0867(3) 0.7608(3) 0.7914(3) 0.0439(14) Uani 1 1 d . . . H8A H -0.0506 0.7361 0.7884 0.053 Uiso 1 1 calc R . . C10B C 0.3986(3) 1.0200(3) 1.0512(3) 0.0493(16) Uani 1 1 d . . . H10 H 0.3696 0.9896 1.0633 0.059 Uiso 1 1 calc R . . C26B C 0.4066(3) 1.1431(3) 0.7949(3) 0.0541(17) Uani 1 1 d . . . H26 H 0.3970 1.1569 0.7560 0.065 Uiso 1 1 calc R . . C25B C 0.4646(3) 1.1144(3) 0.8057(3) 0.0496(16) Uani 1 1 d . . . C18B C 0.4413(3) 1.0851(3) 0.9722(3) 0.0470(15) Uani 1 1 d . . . C16B C 0.5292(3) 1.1562(3) 0.9979(4) 0.064(2) Uani 1 1 d . . . H16 H 0.5309 1.1700 0.9580 0.077 Uiso 1 1 calc R . . C1A C -0.1146(3) 0.9236(3) 0.8085(3) 0.0359(14) Uani 1 1 d . . . C19B C 0.4345(3) 1.1060(3) 0.9112(3) 0.0452(16) Uani 1 1 d . . . C11B C 0.4393(3) 1.0450(4) 1.0910(3) 0.0582(19) Uani 1 1 d . . . H11 H 0.4384 1.0317 1.1310 0.070 Uiso 1 1 calc R . . C21B C 0.5354(2) 1.0663(3) 0.8752(4) 0.0505(15) Uani 1 1 d . . . H21 H 0.5470 1.0553 0.9144 0.061 Uiso 1 1 calc R . . C24B C 0.5055(4) 1.1005(4) 0.7600(3) 0.0591(19) Uani 1 1 d . . . H24 H 0.4961 1.1124 0.7206 0.071 Uiso 1 1 calc R . . C22B C 0.5736(3) 1.0528(3) 0.8291(3) 0.0540(17) Uani 1 1 d . . . H22 H 0.6110 1.0312 0.8368 0.065 Uiso 1 1 calc R . . C14B C 0.5654(4) 1.1594(5) 1.0970(5) 0.088(3) Uani 1 1 d . . . H14 H 0.5917 1.1777 1.1256 0.106 Uiso 1 1 calc R . . C23B C 0.5598(3) 1.0693(3) 0.7720(4) 0.0617(19) Uani 1 1 d . . . H23 H 0.5875 1.0595 0.7408 0.074 Uiso 1 1 calc R . . C13B C 0.5273(4) 1.1162(4) 1.1133(4) 0.072(2) Uani 1 1 d . . . H13 H 0.5288 1.1014 1.1528 0.086 Uiso 1 1 calc R . . C15B C 0.5683(4) 1.1795(4) 1.0377(4) 0.075(2) Uani 1 1 d . . . H15 H 0.5980 1.2094 1.0262 0.090 Uiso 1 1 calc R . . O2B O 0.33413(18) 1.14165(18) 0.9400(2) 0.0459(10) Uani 1 1 d . . . C2A C -0.0304(3) 0.8661(3) 0.8077(3) 0.0365(13) Uani 1 1 d . . . C27B C 0.3658(3) 1.1510(3) 0.8378(3) 0.0507(17) Uani 1 1 d . . . H27 H 0.3272 1.1698 0.8291 0.061 Uiso 1 1 calc R . . C5A C -0.1947(3) 0.8352(3) 0.7998(3) 0.0403(14) Uani 1 1 d . . . H5A H -0.2305 0.8605 0.8014 0.048 Uiso 1 1 calc R . . C6A C -0.1990(2) 0.7707(3) 0.7951(3) 0.0390(13) Uani 1 1 d . . . C7A C -0.1459(3) 0.7348(3) 0.7874(3) 0.0412(14) Uani 1 1 d . . . O1A O -0.25747(17) 0.74592(18) 0.7934(2) 0.0439(10) Uani 1 1 d . . . O2A O -0.14960(18) 0.67203(18) 0.7780(2) 0.0439(10) Uani 1 1 d . . . C9A C -0.2697(3) 0.6952(3) 0.8310(3) 0.0423(14) Uani 1 1 d . . . C10A C -0.2879(3) 0.7076(3) 0.8891(3) 0.0514(18) Uani 1 1 d . . . H10A H -0.2884 0.7487 0.9038 0.062 Uiso 1 1 calc R . . C19A C -0.2458(3) 0.6295(3) 0.7463(3) 0.0420(14) Uani 1 1 d . . . C20A C -0.2814(3) 0.6041(3) 0.6992(3) 0.0490(16) Uani 1 1 d . . . C28A C -0.1871(3) 0.6516(3) 0.7325(3) 0.0431(14) Uani 1 1 d . . . C27A C -0.1644(3) 0.6511(3) 0.6750(3) 0.0523(17) Uani 1 1 d . . . H27A H -0.1254 0.6693 0.6668 0.063 Uiso 1 1 calc R . . C18A C -0.2665(3) 0.6360(3) 0.8078(3) 0.0466(15) Uani 1 1 d . . . C17A C -0.2824(3) 0.5861(3) 0.8447(3) 0.0477(17) Uani 1 1 d . . . C25A C -0.2583(3) 0.6012(3) 0.6419(3) 0.0543(17) Uani 1 1 d . . . C11A C -0.3051(3) 0.6589(4) 0.9246(3) 0.0589(19) Uani 1 1 d . . . H11A H -0.3188 0.6667 0.9638 0.071 Uiso 1 1 calc R . . C15A C -0.2924(4) 0.4761(3) 0.8622(4) 0.068(2) Uani 1 1 d . . . H15A H -0.2885 0.4347 0.8490 0.082 Uiso 1 1 calc R . . C24A C -0.2920(4) 0.5739(4) 0.5959(3) 0.064(2) Uani 1 1 d . . . H24A H -0.2744 0.5693 0.5577 0.077 Uiso 1 1 calc R . . C26A C -0.1974(4) 0.6250(3) 0.6302(3) 0.0586(18) Uani 1 1 d . . . H26A H -0.1804 0.6224 0.5916 0.070 Uiso 1 1 calc R . . C16A C -0.2761(3) 0.5221(3) 0.8251(4) 0.0584(18) Uani 1 1 d . . . H16A H -0.2607 0.5130 0.7868 0.070 Uiso 1 1 calc R . . C13A C -0.3185(4) 0.5465(4) 0.9394(4) 0.073(2) Uani 1 1 d . . . H13A H -0.3321 0.5541 0.9788 0.088 Uiso 1 1 calc R . . C12A C -0.3026(4) 0.5974(4) 0.9035(3) 0.0569(19) Uani 1 1 d . . . C22A C -0.3766(4) 0.5592(4) 0.6628(4) 0.069(2) Uani 1 1 d . . . H22A H -0.4176 0.5456 0.6698 0.082 Uiso 1 1 calc R . . C21A C -0.3431(3) 0.5843(3) 0.7091(4) 0.0607(19) Uani 1 1 d . . . H21A H -0.3613 0.5883 0.7472 0.073 Uiso 1 1 calc R . . C23A C -0.3523(5) 0.5534(4) 0.6072(4) 0.079(3) Uani 1 1 d . . . H23A H -0.3761 0.5356 0.5763 0.094 Uiso 1 1 calc R . . C14A C -0.3154(5) 0.4872(4) 0.9203(4) 0.080(3) Uani 1 1 d . . . H14A H -0.3282 0.4540 0.9449 0.096 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 0.0284(3) 0.0284(3) 0.0448(6) 0.000 0.000 0.000 C2B 0.027(3) 0.035(3) 0.038(3) 0.002(3) 0.003(3) 0.001(2) C5 0.028(3) 0.032(3) 0.043(3) 0.001(3) 0.003(3) -0.002(2) C6 0.034(3) 0.029(3) 0.044(3) 0.000(3) 0.006(3) -0.002(2) C8B 0.030(3) 0.030(3) 0.046(3) 0.004(3) -0.005(3) -0.002(2) C3B 0.025(3) 0.031(3) 0.044(3) 0.001(3) 0.003(2) 0.002(2) N1B 0.028(2) 0.024(2) 0.060(3) -0.001(2) 0.000(2) -0.0004(18) C7B 0.027(3) 0.033(3) 0.055(3) 0.001(3) 0.003(3) -0.005(2) C7 0.031(3) 0.031(3) 0.050(3) -0.005(3) 0.004(3) 0.000(2) N2B 0.029(2) 0.029(2) 0.048(3) 0.000(2) -0.001(2) -0.0017(18) N1A 0.035(3) 0.034(2) 0.048(3) 0.004(2) 0.000(2) 0.0053(19) C6B 0.027(3) 0.039(3) 0.056(4) 0.001(3) 0.000(3) 0.001(2) C4A 0.034(3) 0.035(3) 0.043(3) -0.002(3) 0.001(3) 0.001(2) O1B 0.0244(18) 0.035(2) 0.065(3) -0.002(2) 0.000(2) 0.0028(15) C20B 0.038(3) 0.037(3) 0.060(4) 0.008(3) 0.000(3) -0.007(2) C3A 0.031(3) 0.036(3) 0.041(3) -0.006(3) 0.000(3) -0.002(2) C28B 0.030(3) 0.037(3) 0.072(5) 0.004(3) -0.001(3) -0.009(2) N2A 0.029(2) 0.032(2) 0.045(3) 0.002(2) 0.000(2) -0.0007(18) C17B 0.039(3) 0.047(4) 0.068(5) 0.007(3) -0.009(3) 0.005(3) C12B 0.045(4) 0.055(4) 0.061(4) -0.003(4) -0.010(3) 0.008(3) C9B 0.028(3) 0.046(3) 0.063(4) 0.001(3) -0.003(3) 0.003(3) C8A 0.033(3) 0.039(3) 0.059(4) -0.004(3) 0.002(3) 0.003(2) C10B 0.031(3) 0.048(4) 0.068(4) 0.011(3) 0.000(3) 0.002(3) C26B 0.049(4) 0.057(4) 0.056(4) 0.009(4) -0.005(4) -0.010(3) C25B 0.047(4) 0.044(4) 0.057(4) 0.009(3) 0.000(3) -0.009(3) C18B 0.033(3) 0.044(3) 0.064(4) -0.001(3) 0.000(3) 0.001(3) C16B 0.043(4) 0.051(4) 0.097(6) 0.002(4) -0.004(4) -0.009(3) C1A 0.040(3) 0.032(3) 0.036(3) 0.001(3) 0.004(3) 0.001(2) C19B 0.033(3) 0.035(3) 0.067(4) 0.002(3) -0.002(3) -0.001(2) C11B 0.054(4) 0.065(5) 0.056(4) 0.010(4) 0.005(4) 0.020(4) C21B 0.032(3) 0.046(3) 0.074(4) 0.007(4) 0.004(4) 0.000(2) C24B 0.059(4) 0.063(5) 0.055(4) 0.003(4) 0.005(4) -0.011(4) C22B 0.040(3) 0.052(4) 0.070(5) 0.007(4) 0.004(4) -0.002(3) C14B 0.075(6) 0.086(7) 0.105(8) -0.012(6) -0.039(6) -0.015(5) C23B 0.052(4) 0.060(4) 0.073(5) 0.003(4) 0.010(4) -0.014(3) C13B 0.077(6) 0.067(5) 0.071(5) -0.008(4) -0.021(5) 0.005(4) C15B 0.066(5) 0.067(5) 0.094(7) 0.006(5) -0.021(5) -0.013(4) O2B 0.033(2) 0.030(2) 0.074(3) 0.000(2) 0.002(2) -0.0024(16) C2A 0.039(3) 0.035(3) 0.036(3) -0.003(3) 0.001(3) 0.001(2) C27B 0.034(3) 0.048(4) 0.070(5) 0.009(4) -0.009(3) -0.006(3) C5A 0.036(3) 0.033(3) 0.053(4) -0.006(3) -0.004(3) 0.002(2) C6A 0.028(3) 0.042(3) 0.047(3) -0.007(3) -0.001(3) -0.005(2) C7A 0.035(3) 0.035(3) 0.054(4) -0.007(3) -0.004(3) -0.004(2) O1A 0.032(2) 0.036(2) 0.064(3) 0.000(2) -0.001(2) -0.0018(16) O2A 0.036(2) 0.033(2) 0.063(3) -0.004(2) -0.008(2) 0.0038(16) C9A 0.039(3) 0.039(3) 0.049(3) -0.005(3) -0.004(3) -0.004(3) C10A 0.050(3) 0.043(3) 0.062(5) -0.007(3) -0.002(3) -0.005(3) C19A 0.049(3) 0.029(3) 0.048(4) 0.000(3) -0.005(3) -0.002(2) C20A 0.055(4) 0.030(3) 0.062(4) -0.001(3) -0.010(3) 0.002(3) C28A 0.046(3) 0.033(3) 0.051(4) -0.005(3) 0.001(3) 0.004(2) C27A 0.051(4) 0.044(4) 0.062(4) 0.004(3) 0.003(3) 0.004(3) C18A 0.039(3) 0.043(3) 0.058(4) 0.000(3) -0.005(3) -0.003(3) C17A 0.060(4) 0.035(3) 0.048(4) 0.000(3) 0.003(3) -0.005(3) C25A 0.058(4) 0.053(4) 0.052(4) -0.004(3) -0.004(4) 0.006(3) C11A 0.057(4) 0.062(4) 0.058(4) -0.006(4) 0.016(4) -0.010(3) C15A 0.085(5) 0.038(3) 0.082(6) 0.000(4) 0.004(5) -0.001(3) C24A 0.069(5) 0.076(5) 0.047(4) -0.009(4) -0.013(4) -0.004(4) C26A 0.065(5) 0.053(4) 0.058(4) -0.003(4) 0.007(4) 0.008(3) C16A 0.057(4) 0.041(4) 0.077(5) 0.005(4) 0.005(4) 0.001(3) C13A 0.079(6) 0.079(6) 0.061(5) 0.006(5) 0.012(5) -0.006(4) C12A 0.062(4) 0.049(4) 0.060(5) 0.006(4) -0.003(4) -0.006(3) C22A 0.062(5) 0.075(5) 0.069(5) -0.010(4) -0.019(4) -0.012(4) C21A 0.051(4) 0.057(4) 0.075(5) -0.001(4) -0.003(4) -0.003(3) C23A 0.091(7) 0.080(6) 0.064(5) -0.018(5) -0.021(5) -0.013(5) C14A 0.095(7) 0.054(5) 0.093(6) 0.023(5) -0.002(5) -0.008(5) _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 N1B 2.405(5) . ? Y1 N1B 2.405(5) 2_575 ? Y1 N1B 2.405(5) 3_665 ? Y1 N1B 2.405(5) 4_465 ? Y1 N1A 2.420(5) 4_465 ? Y1 N1A 2.420(5) . ? Y1 N1A 2.420(5) 2_575 ? Y1 N1A 2.420(5) 3_665 ? C2B N2B 1.320(7) . ? C2B N1B 1.374(7) . ? C2B C3B 1.473(7) . ? C5 N2B 1.333(7) 4_465 ? C5 N1B 1.369(7) . ? C5 C6 1.465(8) . ? C6 C7 1.390(8) . ? C6 C3B 1.398(7) . ? C8B C3B 1.391(7) . ? C8B C7B 1.393(8) . ? C7B O2B 1.396(6) . ? C7B C6B 1.411(8) . ? C7 C6B 1.401(8) . ? N2B C5 1.333(7) 3_665 ? N1A C2A 1.355(7) . ? N1A C1A 1.374(7) . ? C6B O1B 1.369(6) . ? C4A C5A 1.385(8) . ? C4A C3A 1.387(8) . ? C4A C1A 1.458(8) . ? O1B C9B 1.387(8) . ? C20B C21B 1.423(8) . ? C20B C25B 1.424(10) . ? C20B C19B 1.425(9) . ? C3A C8A 1.383(8) . ? C3A C2A 1.473(8) . ? C28B C27B 1.385(10) . ? C28B C19B 1.393(9) . ? C28B O2B 1.409(8) . ? N2A C2A 1.329(7) 4_465 ? N2A C1A 1.356(7) . ? C17B C12B 1.393(10) . ? C17B C16B 1.429(10) . ? C17B C18B 1.452(10) . ? C12B C13B 1.428(10) . ? C12B C11B 1.432(10) . ? C9B C18B 1.387(9) . ? C9B C10B 1.400(10) . ? C8A C7A 1.404(8) . ? C10B C11B 1.371(10) . ? C26B C27B 1.324(10) . ? C26B C25B 1.423(10) . ? C25B C24B 1.394(10) . ? C18B C19B 1.459(10) . ? C16B C15B 1.335(11) . ? C21B C22B 1.362(11) . ? C24B C23B 1.383(11) . ? C22B C23B 1.374(10) . ? C14B C13B 1.299(13) . ? C14B C15B 1.411(14) . ? C2A N2A 1.329(7) 3_665 ? C5A C6A 1.404(8) . ? C6A O1A 1.376(6) . ? C6A C7A 1.400(8) . ? C7A O2A 1.379(7) . ? O1A C9A 1.413(7) . ? O2A C28A 1.382(8) . ? C9A C18A 1.387(9) . ? C9A C10A 1.397(9) . ? C10A C11A 1.376(10) . ? C19A C28A 1.395(9) . ? C19A C20A 1.425(9) . ? C19A C18A 1.468(9) . ? C20A C25A 1.391(10) . ? C20A C21A 1.422(10) . ? C28A C27A 1.389(10) . ? C27A C26A 1.364(10) . ? C18A C17A 1.408(9) . ? C17A C12A 1.421(9) . ? C17A C16A 1.461(9) . ? C25A C24A 1.402(10) . ? C25A C26A 1.438(10) . ? C11A C12A 1.417(10) . ? C15A C16A 1.350(10) . ? C15A C14A 1.424(12) . ? C24A C23A 1.401(12) . ? C13A C14A 1.358(12) . ? C13A C12A 1.413(11) . ? C22A C23A 1.369(12) . ? C22A C21A 1.385(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 N1B Y1 N1B 110.0(2) . 2_575 ? N1B Y1 N1B 70.78(12) . 3_665 ? N1B Y1 N1B 70.78(12) 2_575 3_665 ? N1B Y1 N1B 70.78(12) . 4_465 ? N1B Y1 N1B 70.78(12) 2_575 4_465 ? N1B Y1 N1B 110.0(2) 3_665 4_465 ? N1B Y1 N1A 142.22(15) . 4_465 ? N1B Y1 N1A 82.62(16) 2_575 4_465 ? N1B Y1 N1A 81.05(16) 3_665 4_465 ? N1B Y1 N1A 144.82(15) 4_465 4_465 ? N1B Y1 N1A 144.82(15) . . ? N1B Y1 N1A 81.05(16) 2_575 . ? N1B Y1 N1A 142.22(15) 3_665 . ? N1B Y1 N1A 82.62(16) 4_465 . ? N1A Y1 N1A 70.58(12) 4_465 . ? N1B Y1 N1A 81.05(16) . 2_575 ? N1B Y1 N1A 144.82(15) 2_575 2_575 ? N1B Y1 N1A 82.62(16) 3_665 2_575 ? N1B Y1 N1A 142.22(15) 4_465 2_575 ? N1A Y1 N1A 70.58(12) 4_465 2_575 ? N1A Y1 N1A 109.6(2) . 2_575 ? N1B Y1 N1A 82.62(16) . 3_665 ? N1B Y1 N1A 142.22(15) 2_575 3_665 ? N1B Y1 N1A 144.82(15) 3_665 3_665 ? N1B Y1 N1A 81.05(16) 4_465 3_665 ? N1A Y1 N1A 109.6(2) 4_465 3_665 ? N1A Y1 N1A 70.58(12) . 3_665 ? N1A Y1 N1A 70.58(12) 2_575 3_665 ? N2B C2B N1B 129.3(5) . . ? N2B C2B C3B 121.8(5) . . ? N1B C2B C3B 108.8(5) . . ? N2B C5 N1B 128.4(5) 4_465 . ? N2B C5 C6 122.9(5) 4_465 . ? N1B C5 C6 108.7(5) . . ? C7 C6 C3B 120.9(5) . . ? C7 C6 C5 131.9(5) . . ? C3B C6 C5 107.2(5) . . ? C3B C8B C7B 116.6(5) . . ? C8B C3B C6 122.3(5) . . ? C8B C3B C2B 131.7(5) . . ? C6 C3B C2B 105.9(5) . . ? C5 N1B C2B 109.2(5) . . ? C5 N1B Y1 121.4(4) . . ? C2B N1B Y1 120.3(4) . . ? C8B C7B O2B 117.4(5) . . ? C8B C7B C6B 121.8(5) . . ? O2B C7B C6B 120.7(5) . . ? C6 C7 C6B 117.8(5) . . ? C2B N2B C5 121.8(5) . 3_665 ? C2A N1A C1A 108.0(5) . . ? C2A N1A Y1 122.7(4) . . ? C1A N1A Y1 121.6(4) . . ? O1B C6B C7 117.1(5) . . ? O1B C6B C7B 122.5(5) . . ? C7 C6B C7B 120.3(5) . . ? C5A C4A C3A 122.4(5) . . ? C5A C4A C1A 131.6(5) . . ? C3A C4A C1A 106.0(5) . . ? C6B O1B C9B 117.4(5) . . ? C21B C20B C25B 117.3(7) . . ? C21B C20B C19B 121.6(7) . . ? C25B C20B C19B 120.9(6) . . ? C8A C3A C4A 121.2(5) . . ? C8A C3A C2A 132.2(5) . . ? C4A C3A C2A 106.5(5) . . ? C27B C28B C19B 122.3(6) . . ? C27B C28B O2B 120.0(6) . . ? C19B C28B O2B 117.7(6) . . ? C2A N2A C1A 122.4(5) 4_465 . ? C12B C17B C16B 118.8(7) . . ? C12B C17B C18B 119.5(7) . . ? C16B C17B C18B 121.7(7) . . ? C17B C12B C13B 117.9(7) . . ? C17B C12B C11B 119.8(7) . . ? C13B C12B C11B 122.2(7) . . ? O1B C9B C18B 117.8(6) . . ? O1B C9B C10B 118.6(6) . . ? C18B C9B C10B 123.6(6) . . ? C3A C8A C7A 117.1(5) . . ? C11B C10B C9B 118.4(6) . . ? C27B C26B C25B 121.3(7) . . ? C24B C25B C26B 121.9(7) . . ? C24B C25B C20B 120.4(6) . . ? C26B C25B C20B 117.6(6) . . ? C9B C18B C17B 117.4(7) . . ? C9B C18B C19B 117.7(6) . . ? C17B C18B C19B 124.7(6) . . ? C15B C16B C17B 120.6(9) . . ? N2A C1A N1A 127.8(5) . . ? N2A C1A C4A 122.2(5) . . ? N1A C1A C4A 109.9(5) . . ? C28B C19B C20B 116.6(6) . . ? C28B C19B C18B 117.4(6) . . ? C20B C19B C18B 125.7(6) . . ? C10B C11B C12B 121.1(7) . . ? C22B C21B C20B 120.2(8) . . ? C23B C24B C25B 120.1(7) . . ? C21B C22B C23B 122.1(7) . . ? C13B C14B C15B 121.3(9) . . ? C22B C23B C24B 119.8(7) . . ? C14B C13B C12B 121.5(9) . . ? C16B C15B C14B 119.7(9) . . ? C7B O2B C28B 115.6(5) . . ? N2A C2A N1A 128.4(6) 3_665 . ? N2A C2A C3A 122.1(5) 3_665 . ? N1A C2A C3A 109.4(5) . . ? C26B C27B C28B 121.2(6) . . ? C4A C5A C6A 116.9(5) . . ? O1A C6A C7A 122.4(5) . . ? O1A C6A C5A 116.9(5) . . ? C7A C6A C5A 120.5(5) . . ? O2A C7A C6A 121.3(5) . . ? O2A C7A C8A 117.3(5) . . ? C6A C7A C8A 121.3(5) . . ? C6A O1A C9A 117.4(5) . . ? C7A O2A C28A 117.7(5) . . ? C18A C9A C10A 123.2(6) . . ? C18A C9A O1A 118.8(6) . . ? C10A C9A O1A 117.9(5) . . ? C11A C10A C9A 118.4(6) . . ? C28A C19A C20A 117.3(6) . . ? C28A C19A C18A 117.2(6) . . ? C20A C19A C18A 125.4(6) . . ? C25A C20A C21A 118.2(7) . . ? C25A C20A C19A 121.2(6) . . ? C21A C20A C19A 120.5(7) . . ? O2A C28A C27A 119.4(6) . . ? O2A C28A C19A 118.7(6) . . ? C27A C28A C19A 121.9(6) . . ? C26A C27A C28A 120.8(7) . . ? C9A C18A C17A 118.3(6) . . ? C9A C18A C19A 117.6(6) . . ? C17A C18A C19A 124.1(6) . . ? C18A C17A C12A 119.8(7) . . ? C18A C17A C16A 121.9(6) . . ? C12A C17A C16A 118.3(7) . . ? C20A C25A C24A 121.4(7) . . ? C20A C25A C26A 119.0(7) . . ? C24A C25A C26A 119.6(7) . . ? C10A C11A C12A 121.0(7) . . ? C16A C15A C14A 122.6(7) . . ? C23A C24A C25A 119.0(7) . . ? C27A C26A C25A 119.6(7) . . ? C15A C16A C17A 119.3(7) . . ? C14A C13A C12A 122.8(8) . . ? C13A C12A C11A 122.1(8) . . ? C13A C12A C17A 118.7(8) . . ? C11A C12A C17A 119.2(7) . . ? C23A C22A C21A 122.0(8) . . ? C22A C21A C20A 119.4(8) . . ? C22A C23A C24A 119.7(8) . . ? C13A C14A C15A 118.1(8) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 66.90 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.638 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.069 _iucr_refine_instructions_details ; TITL 11 in I4 CELL 1.54178 21.6634 21.6634 22.6033 90.000 90.000 90.000 ZERR 2.00 0.0005 0.0005 0.0014 0.000 0.000 0.000 LATT -2 SYMM - X, - Y, Z SYMM - Y, X, Z SYMM Y, - X, Z SFAC C H N O Y UNIT 448 224 32 32 2 MERG 2 OMIT 0.00 160.00 FMAP 2 PLAN 10 SIZE 0.15 0.22 0.25 ACTA BOND L.S. 2 TEMP -120.00 WGHT 0.079200 FVAR 0.40726 Y1 5 0.000000 1.000000 0.875978 10.25000 0.02836 0.02836 = 0.04483 0.00000 0.00000 0.00000 C2B 1 0.113017 1.077922 0.941060 11.00000 0.02743 0.03536 = 0.03831 0.00240 0.00310 0.00072 C5 1 0.135544 0.977206 0.941876 11.00000 0.02786 0.03162 = 0.04339 0.00099 0.00294 -0.00151 C6 1 0.194305 1.010367 0.946147 11.00000 0.03360 0.02859 = 0.04367 -0.00028 0.00556 -0.00217 C8B 1 0.226688 1.118320 0.942989 11.00000 0.03035 0.03007 = 0.04580 0.00405 -0.00508 -0.00243 AFIX 43 H8B 2 0.217071 1.161084 0.941720 11.00000 -1.20000 AFIX 0 C3B 1 0.180775 1.073454 0.944745 11.00000 0.02511 0.03142 = 0.04367 0.00058 0.00313 0.00190 N1B 3 0.088833 1.019438 0.937038 11.00000 0.02808 0.02423 = 0.06020 -0.00148 0.00009 -0.00042 C7B 1 0.287466 1.097358 0.943185 11.00000 0.02747 0.03270 = 0.05476 0.00054 0.00329 -0.00533 C7 1 0.254949 0.989781 0.949685 11.00000 0.03095 0.03118 = 0.05050 -0.00458 0.00416 -0.00041 AFIX 43 H7 2 0.264216 0.947007 0.952331 11.00000 -1.20000 AFIX 0 N2B 3 0.084215 1.131608 0.942809 11.00000 0.02896 0.02936 = 0.04759 0.00015 -0.00083 -0.00172 N1A 3 -0.051416 0.924608 0.814240 11.00000 0.03467 0.03364 = 0.04804 0.00372 -0.00024 0.00528 C6B 1 0.301967 1.034171 0.949221 11.00000 0.02736 0.03898 = 0.05613 0.00096 -0.00019 0.00055 C4A 1 -0.135901 0.860175 0.801827 11.00000 0.03421 0.03531 = 0.04293 -0.00210 0.00083 0.00070 O1B 4 0.361482 1.013116 0.951601 11.00000 0.02439 0.03531 = 0.06481 -0.00160 -0.00014 0.00280 C20B 1 0.478237 1.096710 0.864966 11.00000 0.03753 0.03725 = 0.05996 0.00755 0.00042 -0.00658 C3A 1 -0.083158 0.823926 0.799987 11.00000 0.03078 0.03598 = 0.04080 -0.00602 0.00025 -0.00164 C28B 1 0.378356 1.132464 0.895198 11.00000 0.02962 0.03684 = 0.07175 0.00406 -0.00113 -0.00863 N2A 3 -0.153659 0.972387 0.806080 11.00000 0.02891 0.03231 = 0.04522 0.00159 0.00018 -0.00073 C17B 1 0.484663 1.110773 1.014614 11.00000 0.03893 0.04682 = 0.06778 0.00714 -0.00936 0.00475 C12B 1 0.483303 1.090671 1.073127 11.00000 0.04456 0.05516 = 0.06142 -0.00306 -0.00959 0.00828 C9B 1 0.400660 1.040363 0.992498 11.00000 0.02812 0.04567 = 0.06297 0.00083 -0.00252 0.00317 C8A 1 -0.086681 0.760817 0.791436 11.00000 0.03311 0.03935 = 0.05931 -0.00358 0.00200 0.00314 AFIX 43 H8A 2 -0.050584 0.736119 0.788394 11.00000 -1.20000 AFIX 0 C10B 1 0.398551 1.019985 1.051247 11.00000 0.03140 0.04845 = 0.06812 0.01052 0.00047 0.00210 AFIX 43 H10 2 0.369560 0.989576 1.063291 11.00000 -1.20000 AFIX 0 C26B 1 0.406598 1.143111 0.794870 11.00000 0.04936 0.05714 = 0.05569 0.00891 -0.00491 -0.01003 AFIX 43 H26 2 0.396978 1.156891 0.756050 11.00000 -1.20000 AFIX 0 C25B 1 0.464578 1.114376 0.805722 11.00000 0.04709 0.04446 = 0.05728 0.00897 -0.00024 -0.00878 C18B 1 0.441294 1.085118 0.972248 11.00000 0.03299 0.04412 = 0.06396 -0.00066 -0.00003 0.00142 C16B 1 0.529165 1.156216 0.997867 11.00000 0.04340 0.05130 = 0.09681 0.00217 -0.00409 -0.00883 AFIX 43 H16 2 0.530933 1.170014 0.958009 11.00000 -1.20000 AFIX 0 C1A 1 -0.114559 0.923601 0.808492 11.00000 0.03966 0.03180 = 0.03612 0.00135 0.00388 0.00076 C19B 1 0.434535 1.105969 0.911215 11.00000 0.03334 0.03527 = 0.06685 0.00231 -0.00246 -0.00063 C11B 1 0.439321 1.044965 1.090969 11.00000 0.05438 0.06452 = 0.05580 0.01018 0.00508 0.01970 AFIX 43 H11 2 0.438384 1.031728 1.131028 11.00000 -1.20000 AFIX 0 C21B 1 0.535440 1.066262 0.875238 11.00000 0.03152 0.04631 = 0.07377 0.00750 0.00352 -0.00041 AFIX 43 H21 2 0.547044 1.055306 0.914386 11.00000 -1.20000 AFIX 0 C24B 1 0.505513 1.100473 0.760034 11.00000 0.05884 0.06335 = 0.05497 0.00302 0.00466 -0.01108 AFIX 43 H24 2 0.496079 1.112407 0.720615 11.00000 -1.20000 AFIX 0 C22B 1 0.573614 1.052769 0.829146 11.00000 0.03974 0.05187 = 0.07045 0.00659 0.00429 -0.00228 AFIX 43 H22 2 0.610965 1.031209 0.836762 11.00000 -1.20000 AFIX 0 C14B 1 0.565360 1.159371 1.096992 11.00000 0.07454 0.08552 = 0.10453 -0.01235 -0.03850 -0.01464 AFIX 43 H14 2 0.591737 1.177735 1.125586 11.00000 -1.20000 AFIX 0 C23B 1 0.559827 1.069343 0.771994 11.00000 0.05188 0.06007 = 0.07327 0.00325 0.00992 -0.01358 AFIX 43 H23 2 0.587503 1.059456 0.740799 11.00000 -1.20000 AFIX 0 C13B 1 0.527310 1.116246 1.113262 11.00000 0.07663 0.06656 = 0.07133 -0.00797 -0.02073 0.00508 AFIX 43 H13 2 0.528797 1.101381 1.152777 11.00000 -1.20000 AFIX 0 C15B 1 0.568279 1.179465 1.037696 11.00000 0.06571 0.06684 = 0.09351 0.00578 -0.02089 -0.01327 AFIX 43 H15 2 0.597957 1.209419 1.026154 11.00000 -1.20000 AFIX 0 O2B 4 0.334132 1.141649 0.940037 11.00000 0.03290 0.03033 = 0.07437 0.00001 0.00187 -0.00244 C2A 1 -0.030431 0.866060 0.807723 11.00000 0.03872 0.03468 = 0.03599 -0.00254 0.00123 0.00097 C27B 1 0.365808 1.151012 0.837817 11.00000 0.03362 0.04844 = 0.07010 0.00853 -0.00910 -0.00610 AFIX 43 H27 2 0.327217 1.169753 0.829111 11.00000 -1.20000 AFIX 0 C5A 1 -0.194702 0.835210 0.799770 11.00000 0.03581 0.03257 = 0.05257 -0.00609 -0.00444 0.00193 AFIX 43 H5A 2 -0.230462 0.860535 0.801420 11.00000 -1.20000 AFIX 0 C6A 1 -0.199011 0.770747 0.795133 11.00000 0.02794 0.04191 = 0.04723 -0.00726 -0.00138 -0.00520 C7A 1 -0.145901 0.734812 0.787445 11.00000 0.03524 0.03466 = 0.05357 -0.00679 -0.00421 -0.00437 O1A 4 -0.257466 0.745917 0.793438 11.00000 0.03197 0.03569 = 0.06401 0.00006 -0.00124 -0.00181 O2A 4 -0.149600 0.672026 0.777955 11.00000 0.03555 0.03289 = 0.06329 -0.00351 -0.00835 0.00376 C9A 1 -0.269698 0.695238 0.831011 11.00000 0.03927 0.03896 = 0.04875 -0.00546 -0.00366 -0.00397 C10A 1 -0.287874 0.707624 0.889128 11.00000 0.04998 0.04250 = 0.06163 -0.00707 -0.00230 -0.00486 AFIX 43 H10A 2 -0.288355 0.748705 0.903826 11.00000 -1.20000 AFIX 0 C19A 1 -0.245806 0.629504 0.746296 11.00000 0.04860 0.02908 = 0.04821 -0.00026 -0.00502 -0.00184 C20A 1 -0.281413 0.604133 0.699187 11.00000 0.05495 0.03027 = 0.06175 -0.00137 -0.00993 0.00184 C28A 1 -0.187053 0.651630 0.732511 11.00000 0.04614 0.03253 = 0.05054 -0.00518 0.00067 0.00402 C27A 1 -0.164390 0.651138 0.675043 11.00000 0.05088 0.04400 = 0.06199 0.00394 0.00343 0.00359 AFIX 43 H27A 2 -0.125382 0.669255 0.666843 11.00000 -1.20000 AFIX 0 C18A 1 -0.266491 0.636049 0.807806 11.00000 0.03938 0.04286 = 0.05764 -0.00005 -0.00547 -0.00307 C17A 1 -0.282355 0.586109 0.844653 11.00000 0.06037 0.03489 = 0.04776 -0.00031 0.00339 -0.00544 C25A 1 -0.258253 0.601239 0.641853 11.00000 0.05776 0.05291 = 0.05212 -0.00438 -0.00378 0.00590 C11A 1 -0.305056 0.658935 0.924560 11.00000 0.05674 0.06229 = 0.05752 -0.00647 0.01586 -0.00955 AFIX 43 H11A 2 -0.318808 0.666694 0.963770 11.00000 -1.20000 AFIX 0 C15A 1 -0.292443 0.476110 0.862210 11.00000 0.08462 0.03822 = 0.08246 0.00031 0.00364 -0.00097 AFIX 43 H15A 2 -0.288466 0.434655 0.849045 11.00000 -1.20000 AFIX 0 C24A 1 -0.292045 0.573909 0.595920 11.00000 0.06890 0.07584 = 0.04715 -0.00854 -0.01339 -0.00425 AFIX 43 H24A 2 -0.274383 0.569350 0.557699 11.00000 -1.20000 AFIX 0 C26A 1 -0.197434 0.624972 0.630241 11.00000 0.06471 0.05265 = 0.05843 -0.00307 0.00663 0.00760 AFIX 43 H26A 2 -0.180393 0.622433 0.591591 11.00000 -1.20000 AFIX 0 C16A 1 -0.276100 0.522136 0.825135 11.00000 0.05731 0.04134 = 0.07653 0.00513 0.00470 0.00078 AFIX 43 H16A 2 -0.260696 0.513023 0.786765 11.00000 -1.20000 AFIX 0 C13A 1 -0.318540 0.546533 0.939448 11.00000 0.07931 0.07936 = 0.06095 0.00568 0.01241 -0.00642 AFIX 43 H13A 2 -0.332065 0.554148 0.978756 11.00000 -1.20000 AFIX 0 C12A 1 -0.302556 0.597407 0.903478 11.00000 0.06208 0.04898 = 0.05964 0.00640 -0.00250 -0.00621 C22A 1 -0.376567 0.559204 0.662803 11.00000 0.06175 0.07493 = 0.06908 -0.01004 -0.01908 -0.01232 AFIX 43 H22A 2 -0.417599 0.545581 0.669836 11.00000 -1.20000 AFIX 0 C21A 1 -0.343123 0.584336 0.709125 11.00000 0.05061 0.05693 = 0.07456 -0.00144 -0.00305 -0.00287 AFIX 43 H21A 2 -0.361250 0.588315 0.747205 11.00000 -1.20000 AFIX 0 C23A 1 -0.352258 0.553407 0.607186 11.00000 0.09142 0.08042 = 0.06421 -0.01803 -0.02099 -0.01330 AFIX 43 H23A 2 -0.376111 0.535557 0.576345 11.00000 -1.20000 AFIX 0 C14A 1 -0.315406 0.487213 0.920263 11.00000 0.09489 0.05373 = 0.09260 0.02300 -0.00185 -0.00840 AFIX 43 H14A 2 -0.328178 0.454050 0.944888 11.00000 -1.20000 HKLF 4 REM 2 in I4 REM R1 = 0.0609 for 4865 Fo > 4sig(Fo) and 0.0756 for all 6246 data REM 580 parameters refined using 1 restraints END ; # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.068 26 7 ' ' 2 0.000 0.000 0.582 1799 335 ' ' 3 0.500 0.500 0.083 1793 335 ' ' 4 0.500 0.500 0.568 26 7 ' ' _platon_squeeze_details ; In this compound, the unit cell includes a large region of disordered solvent molecules, which could not be modeled as discrete atomic sites. We employed PLATON/SQUEEZE to calculate the diffraction contribution of the solvent molecules and, thereby, to produce a set of solvent-free diffraction intensities. The SQUEEZE calculations showed a total solvent accessible area volume of 1789 A^3^ in this compound and the residual electron density amounted to 335 electron per unit cell, corresponding to nearly 8 molecules of CH2Cl2 (about 2 CH2Cl2 molecules per asymmetric unit). ; _database_code_depnum_ccdc_archive 'CCDC 941796'