# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Herbert Roesky' _publ_contact_author_email HROESKY@GWDG.DE _publ_section_title ; A Rational Design for an Efficient Synthesis of a Monomeric Tin(II) Hydroxide ; loop_ _publ_author_name 'Herbert Roesky' 'Anukul Jana' 'Samuel Prinson' 'Sankaranarayanapillai Sarish' 'Carola Schulzke' # Attachment 'ja62b_ja61.cif' data_ja62b _database_code_depnum_ccdc_archive 'CCDC 740971' #TrackingRef 'ja62b_ja61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H102 Fe2 N6 O9 Sn2' _chemical_formula_weight 1568.70 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 17.298(4) _cell_length_b 20.371(4) _cell_length_c 21.502(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.33(3) _cell_angle_gamma 90.00 _cell_volume 7555(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 61363 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 51.9 _exptl_crystal_description stick _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 1.087 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6452 _exptl_absorpt_correction_T_max 0.9590 _exptl_absorpt_process_details 'face indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDSII _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60413 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.93 _reflns_number_total 14600 _reflns_number_gt 12372 _reflns_threshold_expression >2\s(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+6.5087P] 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_number_reflns 14600 _refine_ls_number_parameters 862 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _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 Sn1 Sn 0.354669(11) 0.220840(9) 0.654668(8) 0.01547(6) Uani 1 1 d . . . Sn2 Sn 0.790425(11) 0.266384(9) 0.515428(8) 0.01562(6) Uani 1 1 d . . . Fe1 Fe 0.21179(2) 0.22272(2) 0.63192(2) 0.02182(10) Uani 1 1 d . . . Fe2 Fe 0.69288(2) 0.24747(2) 0.425862(19) 0.01957(10) Uani 1 1 d . . . O1 O 0.20072(16) 0.08097(13) 0.65351(14) 0.0461(7) Uani 1 1 d . . . O2 O 0.10359(16) 0.25104(16) 0.72618(13) 0.0484(7) Uani 1 1 d . . . O3 O 0.22592(17) 0.36054(14) 0.59440(16) 0.0558(9) Uani 1 1 d . . . O4 O 0.14545(19) 0.19700(19) 0.50517(13) 0.0612(9) Uani 1 1 d . . . O5 O 0.64818(16) 0.12331(13) 0.48312(13) 0.0435(7) Uani 1 1 d . . . O6 O 0.73152(16) 0.18686(15) 0.30865(12) 0.0439(7) Uani 1 1 d . . . O7 O 0.72642(17) 0.37680(13) 0.37475(13) 0.0455(7) Uani 1 1 d . . . O8 O 0.53157(16) 0.29067(18) 0.42584(14) 0.0556(8) Uani 1 1 d . . . O9 O 1.01707(19) 0.52838(15) 0.76939(13) 0.0511(7) Uani 1 1 d . . . N1 N 0.41780(15) 0.21832(13) 0.57972(11) 0.0231(5) Uani 1 1 d . . . N2 N 0.41822(14) 0.15261(12) 0.71532(11) 0.0181(5) Uani 1 1 d . . . N3 N 0.41702(14) 0.29724(12) 0.70720(11) 0.0179(5) Uani 1 1 d . . . N4 N 0.75464(14) 0.30460(13) 0.59511(11) 0.0230(5) Uani 1 1 d . . . N5 N 0.86301(14) 0.18884(12) 0.55563(11) 0.0181(5) Uani 1 1 d . . . N6 N 0.89489(13) 0.32244(12) 0.50857(11) 0.0164(5) Uani 1 1 d . . . C1 C 0.20842(18) 0.13610(18) 0.64659(16) 0.0293(7) Uani 1 1 d . . . C2 C 0.1473(2) 0.24040(18) 0.69160(16) 0.0324(8) Uani 1 1 d . . . C3 C 0.22265(19) 0.30732(18) 0.61144(18) 0.0343(8) Uani 1 1 d . . . C4 C 0.1726(2) 0.2067(2) 0.55460(17) 0.0370(8) Uani 1 1 d . . . C5 C 0.3823(2) 0.21328(18) 0.51634(14) 0.0300(7) Uani 1 1 d . . . H5A H 0.3995 0.2501 0.4915 0.045 Uiso 1 1 calc R . . H5B H 0.3258 0.2145 0.5171 0.045 Uiso 1 1 calc R . . H5C H 0.3978 0.1718 0.4978 0.045 Uiso 1 1 calc R . . C6 C 0.50143(19) 0.21531(18) 0.58154(15) 0.0296(7) Uani 1 1 d . . . H6A H 0.5172 0.1734 0.5641 0.044 Uiso 1 1 calc R . . H6B H 0.5231 0.2190 0.6248 0.044 Uiso 1 1 calc R . . H6C H 0.5207 0.2515 0.5570 0.044 Uiso 1 1 calc R . . C7 C 0.38079(17) 0.36175(14) 0.70401(13) 0.0190(6) Uani 1 1 d . . . C8 C 0.32410(18) 0.37551(15) 0.74576(13) 0.0213(6) Uani 1 1 d . . . C9 C 0.2857(2) 0.43566(16) 0.73985(15) 0.0276(7) Uani 1 1 d . . . H9 H 0.2470 0.4459 0.7674 0.033 Uiso 1 1 calc R . . C10 C 0.3029(2) 0.48074(16) 0.69458(16) 0.0296(7) Uani 1 1 d . . . H10 H 0.2759 0.5213 0.6910 0.036 Uiso 1 1 calc R . . C11 C 0.35917(19) 0.46646(16) 0.65491(14) 0.0254(7) Uani 1 1 d . . . H11 H 0.3708 0.4979 0.6243 0.030 Uiso 1 1 calc R . . C12 C 0.39969(17) 0.40723(15) 0.65815(14) 0.0208(6) Uani 1 1 d . . . C13 C 0.30529(19) 0.32731(16) 0.79668(14) 0.0251(7) Uani 1 1 d . . . H13 H 0.3031 0.2825 0.7778 0.030 Uiso 1 1 calc R . . C14 C 0.2272(2) 0.34022(18) 0.82296(17) 0.0342(8) Uani 1 1 d . . . H14A H 0.2295 0.3817 0.8462 0.051 Uiso 1 1 calc R . . H14B H 0.2151 0.3043 0.8509 0.051 Uiso 1 1 calc R . . H14C H 0.1867 0.3430 0.7886 0.051 Uiso 1 1 calc R . . C15 C 0.3685(2) 0.3264(2) 0.85067(16) 0.0385(9) Uani 1 1 d . . . H15A H 0.4181 0.3139 0.8349 0.058 Uiso 1 1 calc R . . H15B H 0.3546 0.2945 0.8821 0.058 Uiso 1 1 calc R . . H15C H 0.3731 0.3701 0.8695 0.058 Uiso 1 1 calc R . . C16 C 0.46078(19) 0.39499(16) 0.61266(15) 0.0256(7) Uani 1 1 d . . . H16 H 0.4878 0.3529 0.6245 0.031 Uiso 1 1 calc R . . C17 C 0.4233(2) 0.38786(19) 0.54625(15) 0.0343(8) Uani 1 1 d . . . H17A H 0.3861 0.3515 0.5447 0.052 Uiso 1 1 calc R . . H17B H 0.4636 0.3789 0.5176 0.052 Uiso 1 1 calc R . . H17C H 0.3964 0.4286 0.5338 0.052 Uiso 1 1 calc R . . C18 C 0.5216(2) 0.45038(18) 0.61504(19) 0.0380(8) Uani 1 1 d . . . H18A H 0.4965 0.4918 0.6020 0.057 Uiso 1 1 calc R . . H18B H 0.5619 0.4398 0.5869 0.057 Uiso 1 1 calc R . . H18C H 0.5452 0.4548 0.6577 0.057 Uiso 1 1 calc R . . C19 C 0.53313(19) 0.34783(16) 0.76058(16) 0.0281(7) Uani 1 1 d . . . H19A H 0.5705 0.3595 0.7304 0.042 Uiso 1 1 calc R . . H19B H 0.5609 0.3373 0.8008 0.042 Uiso 1 1 calc R . . H19C H 0.4981 0.3849 0.7658 0.042 Uiso 1 1 calc R . . C20 C 0.48661(17) 0.28876(15) 0.73711(13) 0.0193(6) Uani 1 1 d . . . C21 C 0.52125(17) 0.22755(15) 0.74985(13) 0.0208(6) Uani 1 1 d . . . H21 H 0.5747 0.2285 0.7637 0.025 Uiso 1 1 calc R . . C22 C 0.48754(17) 0.16519(15) 0.74486(13) 0.0191(6) Uani 1 1 d . . . C23 C 0.53352(18) 0.10917(16) 0.77540(15) 0.0263(7) Uani 1 1 d . . . H23A H 0.5063 0.0921 0.8103 0.039 Uiso 1 1 calc R . . H23B H 0.5849 0.1250 0.7908 0.039 Uiso 1 1 calc R . . H23C H 0.5391 0.0742 0.7448 0.039 Uiso 1 1 calc R . . C24 C 0.38214(17) 0.08917(14) 0.72350(13) 0.0193(6) Uani 1 1 d . . . C25 C 0.39167(18) 0.03865(15) 0.68030(14) 0.0236(6) Uani 1 1 d . . . C26 C 0.35326(19) -0.02036(15) 0.68853(15) 0.0267(7) Uani 1 1 d . . . H26 H 0.3581 -0.0549 0.6594 0.032 Uiso 1 1 calc R . . C27 C 0.30820(19) -0.02981(16) 0.73826(16) 0.0293(7) Uani 1 1 d . . . H27 H 0.2828 -0.0706 0.7434 0.035 Uiso 1 1 calc R . . C28 C 0.30038(19) 0.02053(16) 0.78046(15) 0.0271(7) Uani 1 1 d . . . H28 H 0.2695 0.0138 0.8146 0.033 Uiso 1 1 calc R . . C29 C 0.33672(18) 0.08070(15) 0.77400(14) 0.0224(6) Uani 1 1 d . . . C30 C 0.4410(2) 0.04668(16) 0.62531(15) 0.0294(7) Uani 1 1 d . . . H30 H 0.4665 0.0907 0.6288 0.035 Uiso 1 1 calc R . . C31 C 0.3905(3) 0.04470(19) 0.56369(16) 0.0427(10) Uani 1 1 d . . . H31A H 0.3641 0.0022 0.5595 0.064 Uiso 1 1 calc R . . H31B H 0.4233 0.0507 0.5289 0.064 Uiso 1 1 calc R . . H31C H 0.3519 0.0799 0.5632 0.064 Uiso 1 1 calc R . . C32 C 0.5049(2) -0.0055(2) 0.6250(2) 0.0432(9) Uani 1 1 d . . . H32A H 0.5365 -0.0042 0.6648 0.065 Uiso 1 1 calc R . . H32B H 0.5378 0.0035 0.5908 0.065 Uiso 1 1 calc R . . H32C H 0.4813 -0.0490 0.6192 0.065 Uiso 1 1 calc R . . C33 C 0.3258(2) 0.13476(16) 0.82146(15) 0.0274(7) Uani 1 1 d . . . H33 H 0.3505 0.1756 0.8064 0.033 Uiso 1 1 calc R . . C34 C 0.3657(2) 0.1176(2) 0.88564(17) 0.0423(9) Uani 1 1 d . . . H34A H 0.3605 0.1545 0.9143 0.063 Uiso 1 1 calc R . . H34B H 0.4208 0.1088 0.8815 0.063 Uiso 1 1 calc R . . H34C H 0.3412 0.0785 0.9021 0.063 Uiso 1 1 calc R . . C35 C 0.2408(2) 0.1493(2) 0.82816(18) 0.0394(9) Uani 1 1 d . . . H35A H 0.2158 0.1623 0.7876 0.059 Uiso 1 1 calc R . . H35B H 0.2363 0.1851 0.8581 0.059 Uiso 1 1 calc R . . H35C H 0.2154 0.1100 0.8431 0.059 Uiso 1 1 calc R . . C36 C 0.66887(19) 0.17142(17) 0.46192(15) 0.0286(7) Uani 1 1 d . . . C37 C 0.71922(19) 0.20924(18) 0.35605(15) 0.0293(7) Uani 1 1 d . . . C38 C 0.71679(19) 0.32671(17) 0.39655(15) 0.0283(7) Uani 1 1 d . . . C39 C 0.5948(2) 0.27353(18) 0.42771(15) 0.0316(8) Uani 1 1 d . . . C40 C 0.67489(19) 0.3242(2) 0.60091(17) 0.0372(8) Uani 1 1 d . . . H40A H 0.6534 0.2988 0.6342 0.056 Uiso 1 1 calc R . . H40B H 0.6443 0.3160 0.5614 0.056 Uiso 1 1 calc R . . H40C H 0.6731 0.3711 0.6110 0.056 Uiso 1 1 calc R . . C41 C 0.8034(2) 0.32030(19) 0.65087(14) 0.0315(7) Uani 1 1 d . . . H41A H 0.8033 0.3679 0.6576 0.047 Uiso 1 1 calc R . . H41B H 0.8565 0.3055 0.6459 0.047 Uiso 1 1 calc R . . H41C H 0.7834 0.2982 0.6868 0.047 Uiso 1 1 calc R . . C42 C 0.89561(16) 0.37236(14) 0.46109(13) 0.0186(6) Uani 1 1 d . . . C43 C 0.86390(17) 0.43459(15) 0.47091(14) 0.0216(6) Uani 1 1 d . . . C44 C 0.86390(19) 0.48078(16) 0.42295(15) 0.0272(7) Uani 1 1 d . . . H44 H 0.8421 0.5230 0.4286 0.033 Uiso 1 1 calc R . . C45 C 0.8949(2) 0.46611(17) 0.36753(15) 0.0292(7) Uani 1 1 d . . . H45 H 0.8945 0.4981 0.3354 0.035 Uiso 1 1 calc R . . C46 C 0.9268(2) 0.40506(17) 0.35856(15) 0.0289(7) Uani 1 1 d . . . H46 H 0.9482 0.3956 0.3202 0.035 Uiso 1 1 calc R . . C47 C 0.92795(18) 0.35687(15) 0.40504(14) 0.0239(6) Uani 1 1 d . . . C48 C 0.8294(2) 0.45344(16) 0.53116(15) 0.0277(7) Uani 1 1 d . . . H48 H 0.8379 0.4161 0.5611 0.033 Uiso 1 1 calc R . . C49 C 0.7416(2) 0.4655(2) 0.5210(2) 0.0429(9) Uani 1 1 d . . . H49A H 0.7317 0.5017 0.4915 0.064 Uiso 1 1 calc R . . H49B H 0.7210 0.4767 0.5609 0.064 Uiso 1 1 calc R . . H49C H 0.7160 0.4257 0.5041 0.064 Uiso 1 1 calc R . . C50 C 0.8692(2) 0.51437(19) 0.56075(17) 0.0402(9) Uani 1 1 d . . . H50A H 0.9255 0.5078 0.5641 0.060 Uiso 1 1 calc R . . H50B H 0.8513 0.5214 0.6024 0.060 Uiso 1 1 calc R . . H50C H 0.8564 0.5528 0.5346 0.060 Uiso 1 1 calc R . . C51 C 0.9649(2) 0.29065(18) 0.39300(16) 0.0343(8) Uani 1 1 d . . . H51 H 0.9580 0.2617 0.4297 0.041 Uiso 1 1 calc R . . C52 C 0.9257(3) 0.2579(2) 0.3354(2) 0.0488(10) Uani 1 1 d . . . H52A H 0.8702 0.2529 0.3406 0.073 Uiso 1 1 calc R . . H52B H 0.9489 0.2147 0.3297 0.073 Uiso 1 1 calc R . . H52C H 0.9326 0.2852 0.2987 0.073 Uiso 1 1 calc R . . C53 C 1.0522(2) 0.2968(2) 0.3851(2) 0.0518(11) Uani 1 1 d . . . H53A H 1.0602 0.3231 0.3480 0.078 Uiso 1 1 calc R . . H53B H 1.0744 0.2529 0.3803 0.078 Uiso 1 1 calc R . . H53C H 1.0778 0.3182 0.4219 0.078 Uiso 1 1 calc R . . C54 C 1.02068(18) 0.36582(16) 0.55011(16) 0.0276(7) Uani 1 1 d . . . H54A H 1.0459 0.3657 0.5108 0.041 Uiso 1 1 calc R . . H54B H 1.0592 0.3565 0.5847 0.041 Uiso 1 1 calc R . . H54C H 0.9975 0.4090 0.5563 0.041 Uiso 1 1 calc R . . C55 C 0.95824(17) 0.31399(15) 0.54777(13) 0.0202(6) Uani 1 1 d . . . C56 C 0.97211(17) 0.25960(15) 0.58577(14) 0.0225(6) Uani 1 1 d . . . H56 H 1.0150 0.2634 0.6158 0.027 Uiso 1 1 calc R . . C57 C 0.93189(17) 0.19961(15) 0.58626(13) 0.0207(6) Uani 1 1 d . . . C58 C 0.9722(2) 0.14501(17) 0.62374(16) 0.0316(8) Uani 1 1 d . . . H58A H 0.9518 0.1428 0.6650 0.047 Uiso 1 1 calc R . . H58B H 1.0281 0.1537 0.6285 0.047 Uiso 1 1 calc R . . H58C H 0.9629 0.1031 0.6020 0.047 Uiso 1 1 calc R . . C59 C 0.83228(17) 0.12269(15) 0.55289(14) 0.0210(6) Uani 1 1 d . . . C60 C 0.8466(2) 0.08354(16) 0.50093(15) 0.0285(7) Uani 1 1 d . . . C61 C 0.8190(2) 0.01939(18) 0.49990(17) 0.0368(8) Uani 1 1 d . . . H61 H 0.8289 -0.0083 0.4658 0.044 Uiso 1 1 calc R . . C62 C 0.7775(2) -0.00500(19) 0.54721(18) 0.0409(9) Uani 1 1 d . . . H62 H 0.7598 -0.0492 0.5457 0.049 Uiso 1 1 calc R . . C63 C 0.7620(2) 0.03442(18) 0.59610(16) 0.0322(8) Uani 1 1 d . . . H63 H 0.7324 0.0175 0.6280 0.039 Uiso 1 1 calc R . . C64 C 0.78877(18) 0.09929(16) 0.60026(14) 0.0250(7) Uani 1 1 d . . . C65 C 0.8902(2) 0.11021(18) 0.44775(16) 0.0340(8) Uani 1 1 d . . . H65 H 0.8786 0.1582 0.4446 0.041 Uiso 1 1 calc R . . C66 C 0.8635(2) 0.0798(2) 0.38512(17) 0.0413(9) Uani 1 1 d . . . H66A H 0.8846 0.0353 0.3828 0.062 Uiso 1 1 calc R . . H66B H 0.8820 0.1066 0.3514 0.062 Uiso 1 1 calc R . . H66C H 0.8068 0.0779 0.3809 0.062 Uiso 1 1 calc R . . C67 C 0.9773(2) 0.1033(3) 0.4595(2) 0.0526(11) Uani 1 1 d . . . H67A H 0.9949 0.1278 0.4972 0.079 Uiso 1 1 calc R . . H67B H 1.0027 0.1208 0.4238 0.079 Uiso 1 1 calc R . . H67C H 0.9907 0.0569 0.4652 0.079 Uiso 1 1 calc R . . C68 C 0.7686(2) 0.14186(18) 0.65461(15) 0.0303(7) Uani 1 1 d . . . H68 H 0.7946 0.1853 0.6503 0.036 Uiso 1 1 calc R . . C69 C 0.7982(3) 0.1128(2) 0.71746(17) 0.0457(10) Uani 1 1 d . . . H69A H 0.7721 0.0709 0.7238 0.069 Uiso 1 1 calc R . . H69B H 0.7872 0.1433 0.7509 0.069 Uiso 1 1 calc R . . H69C H 0.8543 0.1056 0.7180 0.069 Uiso 1 1 calc R . . C70 C 0.6820(2) 0.1543(3) 0.6531(2) 0.0586(13) Uani 1 1 d . . . H70A H 0.6642 0.1746 0.6132 0.088 Uiso 1 1 calc R . . H70B H 0.6710 0.1838 0.6874 0.088 Uiso 1 1 calc R . . H70C H 0.6548 0.1126 0.6577 0.088 Uiso 1 1 calc R . . C089 C 0.9430(3) 0.5080(3) 0.7435(2) 0.0597(13) Uani 1 1 d . . . H08A H 0.9262 0.5354 0.7069 0.072 Uiso 1 1 calc R . . H08B H 0.9041 0.5120 0.7748 0.072 Uiso 1 1 calc R . . C091 C 1.0496(3) 0.4723(2) 0.7997(2) 0.0559(12) Uani 1 1 d . . . H09A H 1.0290 0.4667 0.8411 0.067 Uiso 1 1 calc R . . H09B H 1.1067 0.4764 0.8055 0.067 Uiso 1 1 calc R . . C092 C 0.9518(3) 0.4375(3) 0.7244(2) 0.0705(16) Uani 1 1 d . . . H09C H 0.9545 0.4338 0.6787 0.085 Uiso 1 1 calc R . . H09D H 0.9079 0.4107 0.7371 0.085 Uiso 1 1 calc R . . C094 C 1.0277(3) 0.4160(2) 0.7589(3) 0.0662(14) Uani 1 1 d . . . H09E H 1.0202 0.3759 0.7838 0.079 Uiso 1 1 calc R . . H09F H 1.0677 0.4073 0.7294 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 Sn1 0.01438(10) 0.01497(10) 0.01655(10) 0.00050(7) -0.00227(7) -0.00023(7) Sn2 0.01380(10) 0.01699(10) 0.01590(9) 0.00055(7) -0.00003(7) -0.00047(7) Fe1 0.0158(2) 0.0220(2) 0.0267(2) 0.00048(17) -0.00454(16) -0.00036(16) Fe2 0.0170(2) 0.0219(2) 0.0193(2) 0.00048(16) -0.00213(16) -0.00111(16) O1 0.0375(15) 0.0252(15) 0.0729(19) 0.0050(13) -0.0145(13) -0.0085(11) O2 0.0320(15) 0.075(2) 0.0388(15) -0.0118(14) 0.0044(12) 0.0079(14) O3 0.0410(16) 0.0282(16) 0.093(2) 0.0182(15) -0.0267(16) -0.0010(12) O4 0.0569(19) 0.091(3) 0.0331(15) -0.0030(15) -0.0176(14) -0.0140(18) O5 0.0424(15) 0.0327(15) 0.0535(16) 0.0112(12) -0.0092(12) -0.0136(12) O6 0.0450(16) 0.0550(18) 0.0323(14) -0.0192(12) 0.0064(11) -0.0057(13) O7 0.0502(17) 0.0334(15) 0.0497(16) 0.0190(13) -0.0180(13) -0.0092(12) O8 0.0262(14) 0.089(2) 0.0527(17) 0.0184(16) 0.0069(12) 0.0200(15) O9 0.0601(19) 0.0514(18) 0.0410(15) -0.0030(13) -0.0020(14) -0.0059(15) N1 0.0207(13) 0.0321(15) 0.0166(12) 0.0004(10) 0.0015(9) 0.0002(11) N2 0.0202(12) 0.0154(12) 0.0182(11) 0.0023(9) -0.0026(9) -0.0003(9) N3 0.0188(12) 0.0145(12) 0.0197(11) -0.0013(9) -0.0028(9) 0.0016(9) N4 0.0187(12) 0.0292(15) 0.0213(12) -0.0046(10) 0.0044(10) 0.0006(11) N5 0.0179(12) 0.0182(13) 0.0182(11) 0.0009(9) 0.0019(9) 0.0000(9) N6 0.0140(11) 0.0168(12) 0.0186(11) 0.0015(9) 0.0024(9) -0.0010(9) C1 0.0176(15) 0.032(2) 0.0366(18) -0.0012(14) -0.0056(13) -0.0030(13) C2 0.0238(17) 0.039(2) 0.0330(18) -0.0042(15) -0.0065(14) 0.0009(14) C3 0.0183(16) 0.033(2) 0.050(2) 0.0045(16) -0.0109(14) 0.0026(14) C4 0.0313(19) 0.042(2) 0.0362(19) 0.0014(16) -0.0056(15) -0.0042(16) C5 0.0372(19) 0.0344(19) 0.0179(14) -0.0002(13) -0.0004(13) -0.0031(15) C6 0.0250(16) 0.037(2) 0.0269(16) 0.0001(14) 0.0054(13) -0.0004(14) C7 0.0197(14) 0.0153(14) 0.0210(14) -0.0029(11) -0.0053(11) 0.0006(11) C8 0.0238(15) 0.0194(15) 0.0200(14) -0.0030(11) -0.0023(12) 0.0001(12) C9 0.0313(18) 0.0247(17) 0.0275(16) -0.0028(13) 0.0062(13) 0.0058(13) C10 0.0360(19) 0.0182(16) 0.0345(18) 0.0008(13) 0.0017(14) 0.0085(13) C11 0.0298(17) 0.0194(16) 0.0265(16) 0.0040(12) -0.0008(13) 0.0005(13) C12 0.0212(15) 0.0183(15) 0.0222(14) -0.0009(11) -0.0027(11) -0.0017(12) C13 0.0319(17) 0.0220(16) 0.0216(15) -0.0010(12) 0.0029(13) -0.0003(13) C14 0.042(2) 0.0275(19) 0.0347(18) 0.0010(14) 0.0137(15) 0.0012(15) C15 0.043(2) 0.048(2) 0.0242(17) 0.0055(15) -0.0017(15) 0.0029(17) C16 0.0283(17) 0.0190(16) 0.0302(16) 0.0042(12) 0.0051(13) 0.0024(12) C17 0.043(2) 0.035(2) 0.0258(17) 0.0015(14) 0.0080(15) 0.0048(16) C18 0.0291(18) 0.029(2) 0.056(2) 0.0058(16) 0.0082(16) -0.0008(15) C19 0.0243(16) 0.0236(17) 0.0345(17) -0.0026(13) -0.0097(13) -0.0033(13) C20 0.0187(14) 0.0210(15) 0.0177(13) -0.0001(11) -0.0005(11) -0.0023(11) C21 0.0189(14) 0.0232(16) 0.0196(14) -0.0004(11) -0.0031(11) 0.0009(12) C22 0.0191(14) 0.0222(15) 0.0158(13) 0.0017(11) -0.0005(11) 0.0025(11) C23 0.0220(15) 0.0234(17) 0.0325(17) 0.0068(13) -0.0050(13) 0.0018(12) C24 0.0215(15) 0.0154(14) 0.0200(14) 0.0035(11) -0.0048(11) -0.0007(11) C25 0.0275(16) 0.0176(15) 0.0250(15) 0.0014(12) -0.0035(12) 0.0027(12) C26 0.0313(17) 0.0176(16) 0.0304(16) -0.0022(12) -0.0035(13) 0.0024(13) C27 0.0299(17) 0.0187(16) 0.0384(18) 0.0054(13) -0.0035(14) -0.0066(13) C28 0.0288(17) 0.0225(17) 0.0303(16) 0.0059(13) 0.0037(13) -0.0022(13) C29 0.0228(15) 0.0197(16) 0.0245(15) 0.0046(12) 0.0008(12) 0.0011(12) C30 0.0387(19) 0.0216(17) 0.0284(16) -0.0024(13) 0.0060(14) 0.0025(14) C31 0.070(3) 0.030(2) 0.0276(18) -0.0032(15) 0.0001(18) 0.0011(18) C32 0.048(2) 0.034(2) 0.049(2) -0.0019(17) 0.0170(18) 0.0083(17) C33 0.0378(19) 0.0192(16) 0.0264(16) 0.0010(12) 0.0111(14) -0.0040(13) C34 0.047(2) 0.042(2) 0.036(2) -0.0112(16) -0.0056(17) -0.0013(18) C35 0.040(2) 0.041(2) 0.038(2) -0.0004(16) 0.0101(16) 0.0102(17) C36 0.0246(16) 0.0293(19) 0.0305(17) -0.0010(14) -0.0065(13) -0.0027(14) C37 0.0251(16) 0.0316(18) 0.0305(17) -0.0018(14) -0.0021(13) -0.0047(14) C38 0.0270(17) 0.0316(19) 0.0245(15) 0.0021(14) -0.0085(13) -0.0007(14) C39 0.0259(18) 0.043(2) 0.0257(16) 0.0085(14) 0.0017(13) 0.0045(15) C40 0.0223(17) 0.050(2) 0.041(2) -0.0111(17) 0.0107(14) 0.0045(15) C41 0.0310(18) 0.042(2) 0.0212(15) -0.0082(14) 0.0020(13) -0.0036(15) C42 0.0167(14) 0.0187(15) 0.0201(14) 0.0027(11) -0.0011(11) -0.0030(11) C43 0.0199(15) 0.0196(15) 0.0247(15) 0.0003(12) -0.0021(12) -0.0029(12) C44 0.0285(17) 0.0202(16) 0.0322(17) 0.0045(13) -0.0012(13) -0.0003(13) C45 0.0320(18) 0.0269(18) 0.0281(16) 0.0102(13) -0.0015(13) -0.0046(14) C46 0.0334(18) 0.0307(19) 0.0231(15) 0.0036(13) 0.0060(13) -0.0034(14) C47 0.0269(16) 0.0226(16) 0.0228(15) 0.0028(12) 0.0054(12) -0.0029(12) C48 0.0335(18) 0.0195(16) 0.0309(17) 0.0005(13) 0.0069(14) 0.0036(13) C49 0.037(2) 0.040(2) 0.052(2) -0.0069(18) 0.0112(17) 0.0084(17) C50 0.053(2) 0.033(2) 0.0349(19) -0.0100(15) 0.0065(17) -0.0017(17) C51 0.046(2) 0.0297(19) 0.0298(17) 0.0029(14) 0.0198(15) 0.0072(16) C52 0.041(2) 0.037(2) 0.070(3) -0.020(2) 0.017(2) -0.0030(17) C53 0.036(2) 0.062(3) 0.056(3) -0.013(2) -0.0006(19) 0.018(2) C54 0.0213(16) 0.0270(17) 0.0339(17) 0.0049(13) -0.0027(13) -0.0076(13) C55 0.0168(14) 0.0222(16) 0.0218(14) -0.0012(12) 0.0027(11) -0.0026(11) C56 0.0174(14) 0.0253(16) 0.0242(15) 0.0021(12) -0.0029(11) -0.0010(12) C57 0.0191(14) 0.0235(16) 0.0193(14) 0.0028(12) 0.0000(11) 0.0011(12) C58 0.0271(17) 0.0283(18) 0.0381(18) 0.0121(14) -0.0069(14) -0.0008(14) C59 0.0181(14) 0.0213(15) 0.0230(14) 0.0071(12) -0.0023(11) -0.0001(12) C60 0.0344(18) 0.0224(17) 0.0282(16) 0.0002(13) -0.0004(14) -0.0032(14) C61 0.052(2) 0.0253(19) 0.0332(18) -0.0032(14) 0.0022(16) -0.0087(16) C62 0.055(2) 0.0259(19) 0.040(2) 0.0077(16) -0.0078(17) -0.0164(17) C63 0.0314(18) 0.0322(19) 0.0326(18) 0.0127(14) -0.0014(14) -0.0101(14) C64 0.0217(15) 0.0255(17) 0.0269(16) 0.0084(13) -0.0044(12) -0.0017(12) C65 0.042(2) 0.0251(18) 0.0364(19) -0.0061(14) 0.0130(15) -0.0033(15) C66 0.049(2) 0.044(2) 0.0317(19) -0.0033(16) 0.0088(17) -0.0017(18) C67 0.042(2) 0.069(3) 0.047(2) -0.009(2) 0.0092(19) -0.011(2) C68 0.0323(18) 0.0305(19) 0.0291(17) 0.0098(14) 0.0090(14) 0.0018(14) C69 0.062(3) 0.047(2) 0.0289(19) 0.0014(16) 0.0052(18) 0.003(2) C70 0.034(2) 0.089(4) 0.055(3) -0.001(2) 0.0140(19) 0.012(2) C089 0.046(3) 0.080(4) 0.053(3) 0.016(2) 0.004(2) 0.000(2) C091 0.047(3) 0.064(3) 0.055(3) 0.017(2) -0.003(2) -0.015(2) C092 0.077(4) 0.090(4) 0.045(3) -0.006(3) 0.002(2) -0.042(3) C094 0.076(4) 0.045(3) 0.081(4) 0.016(2) 0.026(3) -0.003(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sn1 N1 2.014(3) . ? Sn1 N2 2.151(2) . ? Sn1 N3 2.163(2) . ? Sn1 Fe1 2.4832(7) . ? Sn2 N4 2.021(2) . ? Sn2 N6 2.152(2) . ? Sn2 N5 2.158(2) . ? Sn2 Fe2 2.4928(9) . ? Fe1 C4 1.777(4) . ? Fe1 C3 1.792(4) . ? Fe1 C1 1.794(4) . ? Fe1 C2 1.799(4) . ? Fe2 C37 1.781(3) . ? Fe2 C39 1.781(3) . ? Fe2 C38 1.793(4) . ? Fe2 C36 1.795(4) . ? O1 C1 1.142(4) . ? O2 C2 1.121(5) . ? O3 C3 1.147(4) . ? O4 C4 1.147(4) . ? O5 C36 1.149(4) . ? O6 C37 1.151(4) . ? O7 C38 1.140(4) . ? O8 C39 1.146(4) . ? O9 C091 1.411(5) . ? O9 C089 1.420(6) . ? N1 C6 1.445(4) . ? N1 C5 1.455(4) . ? N2 C22 1.339(4) . ? N2 C24 1.452(4) . ? N3 C20 1.333(4) . ? N3 C7 1.455(4) . ? N4 C41 1.449(4) . ? N4 C40 1.451(4) . ? N5 C57 1.335(4) . ? N5 C59 1.448(4) . ? N6 C55 1.342(4) . ? N6 C42 1.442(4) . ? C7 C8 1.407(4) . ? C7 C12 1.409(4) . ? C8 C9 1.395(4) . ? C8 C13 1.524(4) . ? C9 C10 1.387(5) . ? C10 C11 1.373(5) . ? C11 C12 1.395(4) . ? C12 C16 1.514(4) . ? C13 C14 1.526(5) . ? C13 C15 1.533(4) . ? C16 C17 1.530(5) . ? C16 C18 1.542(5) . ? C19 C20 1.513(4) . ? C20 C21 1.402(4) . ? C21 C22 1.399(4) . ? C22 C23 1.512(4) . ? C24 C29 1.398(4) . ? C24 C25 1.404(4) . ? C25 C26 1.391(5) . ? C25 C30 1.518(5) . ? C26 C27 1.383(5) . ? C27 C28 1.383(5) . ? C28 C29 1.389(4) . ? C29 C33 1.523(4) . ? C30 C31 1.531(5) . ? C30 C32 1.534(5) . ? C33 C35 1.518(5) . ? C33 C34 1.536(5) . ? C42 C47 1.402(4) . ? C42 C43 1.403(4) . ? C43 C44 1.396(4) . ? C43 C48 1.516(4) . ? C44 C45 1.376(5) . ? C45 C46 1.379(5) . ? C46 C47 1.400(4) . ? C47 C51 1.523(5) . ? C48 C50 1.535(5) . ? C48 C49 1.538(5) . ? C51 C52 1.521(6) . ? C51 C53 1.538(6) . ? C54 C55 1.509(4) . ? C55 C56 1.387(4) . ? C56 C57 1.407(4) . ? C57 C58 1.513(4) . ? C59 C64 1.395(4) . ? C59 C60 1.410(5) . ? C60 C61 1.391(5) . ? C60 C65 1.517(5) . ? C61 C62 1.381(6) . ? C62 C63 1.365(6) . ? C63 C64 1.401(5) . ? C64 C68 1.517(5) . ? C65 C67 1.516(6) . ? C65 C66 1.522(5) . ? C68 C70 1.517(5) . ? C68 C69 1.528(5) . ? C089 C092 1.505(8) . ? C091 C094 1.476(7) . ? C092 C094 1.523(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 N1 Sn1 N2 100.70(10) . . ? N1 Sn1 N3 99.04(10) . . ? N2 Sn1 N3 86.36(9) . . ? N1 Sn1 Fe1 115.74(7) . . ? N2 Sn1 Fe1 125.80(7) . . ? N3 Sn1 Fe1 122.78(7) . . ? N4 Sn2 N6 99.56(10) . . ? N4 Sn2 N5 98.54(10) . . ? N6 Sn2 N5 87.12(9) . . ? N4 Sn2 Fe2 118.80(7) . . ? N6 Sn2 Fe2 123.50(6) . . ? N5 Sn2 Fe2 122.40(7) . . ? C4 Fe1 C3 89.18(17) . . ? C4 Fe1 C1 88.24(17) . . ? C3 Fe1 C1 173.89(17) . . ? C4 Fe1 C2 119.41(16) . . ? C3 Fe1 C2 93.71(18) . . ? C1 Fe1 C2 92.37(17) . . ? C4 Fe1 Sn1 119.00(13) . . ? C3 Fe1 Sn1 86.68(10) . . ? C1 Fe1 Sn1 89.73(10) . . ? C2 Fe1 Sn1 121.58(11) . . ? C37 Fe2 C39 117.00(15) . . ? C37 Fe2 C38 90.97(16) . . ? C39 Fe2 C38 89.13(16) . . ? C37 Fe2 C36 93.95(16) . . ? C39 Fe2 C36 89.76(16) . . ? C38 Fe2 C36 174.92(15) . . ? C37 Fe2 Sn2 121.17(11) . . ? C39 Fe2 Sn2 121.81(11) . . ? C38 Fe2 Sn2 88.38(10) . . ? C36 Fe2 Sn2 87.99(10) . . ? C091 O9 C089 105.2(3) . . ? C6 N1 C5 111.9(3) . . ? C6 N1 Sn1 125.5(2) . . ? C5 N1 Sn1 122.4(2) . . ? C22 N2 C24 119.4(2) . . ? C22 N2 Sn1 124.2(2) . . ? C24 N2 Sn1 116.37(17) . . ? C20 N3 C7 120.7(2) . . ? C20 N3 Sn1 123.7(2) . . ? C7 N3 Sn1 115.42(17) . . ? C41 N4 C40 111.5(3) . . ? C41 N4 Sn2 126.2(2) . . ? C40 N4 Sn2 122.2(2) . . ? C57 N5 C59 118.9(2) . . ? C57 N5 Sn2 123.2(2) . . ? C59 N5 Sn2 117.67(17) . . ? C55 N6 C42 119.0(2) . . ? C55 N6 Sn2 122.61(19) . . ? C42 N6 Sn2 118.36(17) . . ? O1 C1 Fe1 174.7(3) . . ? O2 C2 Fe1 175.9(3) . . ? O3 C3 Fe1 174.8(3) . . ? O4 C4 Fe1 178.1(4) . . ? C8 C7 C12 121.7(3) . . ? C8 C7 N3 117.9(3) . . ? C12 C7 N3 120.3(3) . . ? C9 C8 C7 117.8(3) . . ? C9 C8 C13 120.4(3) . . ? C7 C8 C13 121.8(3) . . ? C10 C9 C8 121.3(3) . . ? C11 C10 C9 119.7(3) . . ? C10 C11 C12 122.0(3) . . ? C11 C12 C7 117.5(3) . . ? C11 C12 C16 118.9(3) . . ? C7 C12 C16 123.6(3) . . ? C8 C13 C14 113.5(3) . . ? C8 C13 C15 111.9(3) . . ? C14 C13 C15 108.8(3) . . ? C12 C16 C17 110.6(3) . . ? C12 C16 C18 111.5(3) . . ? C17 C16 C18 109.9(3) . . ? N3 C20 C21 124.5(3) . . ? N3 C20 C19 119.8(3) . . ? C21 C20 C19 115.7(3) . . ? C22 C21 C20 128.6(3) . . ? N2 C22 C21 124.3(3) . . ? N2 C22 C23 119.0(3) . . ? C21 C22 C23 116.7(2) . . ? C29 C24 C25 121.6(3) . . ? C29 C24 N2 118.4(3) . . ? C25 C24 N2 120.0(3) . . ? C26 C25 C24 117.9(3) . . ? C26 C25 C30 119.6(3) . . ? C24 C25 C30 122.5(3) . . ? C27 C26 C25 121.4(3) . . ? C28 C27 C26 119.5(3) . . ? C27 C28 C29 121.4(3) . . ? C28 C29 C24 118.1(3) . . ? C28 C29 C33 119.4(3) . . ? C24 C29 C33 122.4(3) . . ? C25 C30 C31 110.7(3) . . ? C25 C30 C32 112.1(3) . . ? C31 C30 C32 110.0(3) . . ? C35 C33 C29 112.0(3) . . ? C35 C33 C34 109.4(3) . . ? C29 C33 C34 111.6(3) . . ? O5 C36 Fe2 175.1(3) . . ? O6 C37 Fe2 174.8(3) . . ? O7 C38 Fe2 174.3(3) . . ? O8 C39 Fe2 176.7(3) . . ? C47 C42 C43 121.2(3) . . ? C47 C42 N6 118.4(3) . . ? C43 C42 N6 120.4(3) . . ? C44 C43 C42 118.4(3) . . ? C44 C43 C48 118.8(3) . . ? C42 C43 C48 122.7(3) . . ? C45 C44 C43 121.0(3) . . ? C44 C45 C46 120.2(3) . . ? C45 C46 C47 121.1(3) . . ? C46 C47 C42 118.1(3) . . ? C46 C47 C51 118.9(3) . . ? C42 C47 C51 123.0(3) . . ? C43 C48 C50 111.4(3) . . ? C43 C48 C49 111.6(3) . . ? C50 C48 C49 109.8(3) . . ? C52 C51 C47 111.1(3) . . ? C52 C51 C53 109.1(3) . . ? C47 C51 C53 112.1(3) . . ? N6 C55 C56 124.7(3) . . ? N6 C55 C54 118.7(3) . . ? C56 C55 C54 116.6(3) . . ? C55 C56 C57 129.4(3) . . ? N5 C57 C56 124.2(3) . . ? N5 C57 C58 120.0(3) . . ? C56 C57 C58 115.7(3) . . ? C64 C59 C60 121.5(3) . . ? C64 C59 N5 120.3(3) . . ? C60 C59 N5 118.2(3) . . ? C61 C60 C59 117.6(3) . . ? C61 C60 C65 120.9(3) . . ? C59 C60 C65 121.5(3) . . ? C62 C61 C60 121.6(3) . . ? C63 C62 C61 119.9(3) . . ? C62 C63 C64 121.4(3) . . ? C59 C64 C63 118.0(3) . . ? C59 C64 C68 122.4(3) . . ? C63 C64 C68 119.6(3) . . ? C67 C65 C60 112.7(3) . . ? C67 C65 C66 110.0(3) . . ? C60 C65 C66 112.7(3) . . ? C64 C68 C70 111.3(3) . . ? C64 C68 C69 112.2(3) . . ? C70 C68 C69 110.4(3) . . ? O9 C089 C092 106.2(4) . . ? O9 C091 C094 106.2(4) . . ? C089 C092 C094 104.1(4) . . ? C091 C094 C092 103.8(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.988 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.082 data_ja61 _database_code_depnum_ccdc_archive 'CCDC 740972' #TrackingRef 'ja62b_ja61.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H42 Fe N2 O5 Sn' _chemical_formula_weight 721.23 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 16.132(3) _cell_length_b 10.002(2) _cell_length_c 20.437(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.62(3) _cell_angle_gamma 90.00 _cell_volume 3275.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 27928 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 51.9 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8080 _exptl_absorpt_correction_T_max 0.9307 _exptl_absorpt_process_details 'face indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDSII _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27077 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6328 _reflns_number_gt 5164 _reflns_threshold_expression >2\s(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.5948P] 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_number_reflns 6328 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Sn1 Sn 0.437819(15) 0.31454(2) 0.238771(10) 0.02290(7) Uani 1 1 d . . . Fe1 Fe 0.50140(3) 0.53935(5) 0.25084(2) 0.02934(12) Uani 1 1 d . . . O1 O 0.5958(2) 0.4758(3) 0.37863(14) 0.0501(8) Uani 1 1 d . . . O2 O 0.3285(2) 0.6416(3) 0.2364(2) 0.0655(10) Uani 1 1 d . . . O3 O 0.57077(19) 0.8083(3) 0.26922(17) 0.0543(8) Uani 1 1 d . . . O4 O 0.5861(2) 0.5239(3) 0.13154(15) 0.0552(8) Uani 1 1 d . . . O5 O 0.31476(15) 0.3120(2) 0.21036(11) 0.0300(5) Uani 1 1 d . . . H5 H 0.2958 0.2355 0.2167 0.045 Uiso 1 1 calc R . . N1 N 0.43830(17) 0.1700(3) 0.31532(12) 0.0233(6) Uani 1 1 d . . . N2 N 0.47060(17) 0.1596(2) 0.17540(12) 0.0217(6) Uani 1 1 d . . . C1 C 0.5575(3) 0.4930(4) 0.32856(19) 0.0341(8) Uani 1 1 d . . . C2 C 0.3958(3) 0.5973(4) 0.2424(2) 0.0461(11) Uani 1 1 d . . . C3 C 0.5430(2) 0.7032(4) 0.2621(2) 0.0393(9) Uani 1 1 d . . . C4 C 0.5517(3) 0.5221(3) 0.17778(19) 0.0379(9) Uani 1 1 d . . . C5 C 0.4639(2) 0.2104(3) 0.38294(15) 0.0245(7) Uani 1 1 d . . . C6 C 0.4133(2) 0.2982(3) 0.41383(16) 0.0278(7) Uani 1 1 d . . . C7 C 0.4426(3) 0.3437(3) 0.47685(17) 0.0332(8) Uani 1 1 d . . . H7 H 0.4095 0.4040 0.4987 0.040 Uiso 1 1 calc R . . C8 C 0.5188(2) 0.3022(4) 0.50787(17) 0.0360(8) Uani 1 1 d . . . H8 H 0.5380 0.3350 0.5506 0.043 Uiso 1 1 calc R . . C9 C 0.5672(2) 0.2137(3) 0.47726(17) 0.0325(8) Uani 1 1 d . . . H9 H 0.6191 0.1851 0.4994 0.039 Uiso 1 1 calc R . . C10 C 0.5409(2) 0.1655(3) 0.41420(16) 0.0287(7) Uani 1 1 d . . . C11 C 0.3262(2) 0.3380(4) 0.38353(18) 0.0340(8) Uani 1 1 d . . . H11 H 0.3215 0.3160 0.3355 0.041 Uiso 1 1 calc R . . C12 C 0.3082(3) 0.4862(5) 0.3897(3) 0.0564(12) Uani 1 1 d . . . H12A H 0.3043 0.5081 0.4360 0.085 Uiso 1 1 calc R . . H12B H 0.2553 0.5079 0.3633 0.085 Uiso 1 1 calc R . . H12C H 0.3534 0.5381 0.3738 0.085 Uiso 1 1 calc R . . C13 C 0.2617(3) 0.2548(6) 0.4140(3) 0.0664(15) Uani 1 1 d . . . H13A H 0.2709 0.1598 0.4056 0.100 Uiso 1 1 calc R . . H13B H 0.2056 0.2804 0.3944 0.100 Uiso 1 1 calc R . . H13C H 0.2669 0.2707 0.4616 0.100 Uiso 1 1 calc R . . C14 C 0.5975(2) 0.0695(4) 0.38206(18) 0.0335(8) Uani 1 1 d . . . H14 H 0.5664 0.0370 0.3399 0.040 Uiso 1 1 calc R . . C15 C 0.6761(3) 0.1401(5) 0.3657(2) 0.0484(11) Uani 1 1 d . . . H15A H 0.6606 0.2166 0.3369 0.073 Uiso 1 1 calc R . . H15B H 0.7101 0.0777 0.3431 0.073 Uiso 1 1 calc R . . H15C H 0.7081 0.1715 0.4064 0.073 Uiso 1 1 calc R . . C16 C 0.6209(3) -0.0523(5) 0.4258(2) 0.0571(12) Uani 1 1 d . . . H16A H 0.6580 -0.0243 0.4648 0.086 Uiso 1 1 calc R . . H16B H 0.6496 -0.1184 0.4011 0.086 Uiso 1 1 calc R . . H16C H 0.5702 -0.0922 0.4396 0.086 Uiso 1 1 calc R . . C17 C 0.3867(3) -0.0450(4) 0.35376(18) 0.0363(8) Uani 1 1 d . . . H17A H 0.4293 -0.1145 0.3627 0.054 Uiso 1 1 calc R . . H17B H 0.3327 -0.0867 0.3394 0.054 Uiso 1 1 calc R . . H17C H 0.3826 0.0070 0.3939 0.054 Uiso 1 1 calc R . . C18 C 0.4106(2) 0.0459(3) 0.30055(16) 0.0251(7) Uani 1 1 d . . . C19 C 0.4050(2) -0.0076(3) 0.23694(16) 0.0256(7) Uani 1 1 d . . . H19 H 0.3712 -0.0853 0.2300 0.031 Uiso 1 1 calc R . . C20 C 0.4416(2) 0.0361(3) 0.18230(16) 0.0241(7) Uani 1 1 d . . . C21 C 0.4499(2) -0.0635(3) 0.12802(17) 0.0314(8) Uani 1 1 d . . . H21A H 0.4112 -0.0397 0.0892 0.047 Uiso 1 1 calc R . . H21B H 0.4365 -0.1532 0.1430 0.047 Uiso 1 1 calc R . . H21C H 0.5072 -0.0623 0.1166 0.047 Uiso 1 1 calc R . . C22 C 0.5111(2) 0.1967(3) 0.11799(15) 0.0245(7) Uani 1 1 d . . . C23 C 0.5980(2) 0.1915(4) 0.12176(15) 0.0285(7) Uani 1 1 d . . . C24 C 0.6351(3) 0.2329(4) 0.06673(18) 0.0356(8) Uani 1 1 d . . . H24 H 0.6940 0.2281 0.0674 0.043 Uiso 1 1 calc R . . C25 C 0.5872(3) 0.2807(4) 0.01138(18) 0.0360(9) Uani 1 1 d . . . H25 H 0.6136 0.3107 -0.0252 0.043 Uiso 1 1 calc R . . C26 C 0.5018(3) 0.2855(3) 0.00854(17) 0.0347(9) Uani 1 1 d . . . H26 H 0.4699 0.3192 -0.0299 0.042 Uiso 1 1 calc R . . C27 C 0.4611(2) 0.2417(3) 0.06133(16) 0.0272(7) Uani 1 1 d . . . C28 C 0.6531(2) 0.1427(4) 0.18248(18) 0.0344(8) Uani 1 1 d . . . H28 H 0.6170 0.1297 0.2186 0.041 Uiso 1 1 calc R . . C29 C 0.7200(3) 0.2438(5) 0.2057(2) 0.0607(13) Uani 1 1 d . . . H29A H 0.7585 0.2534 0.1722 0.091 Uiso 1 1 calc R . . H29B H 0.7509 0.2130 0.2471 0.091 Uiso 1 1 calc R . . H29C H 0.6940 0.3303 0.2128 0.091 Uiso 1 1 calc R . . C30 C 0.6940(4) 0.0092(5) 0.1701(3) 0.0623(13) Uani 1 1 d . . . H30A H 0.6507 -0.0579 0.1578 0.093 Uiso 1 1 calc R . . H30B H 0.7286 -0.0195 0.2102 0.093 Uiso 1 1 calc R . . H30C H 0.7291 0.0192 0.1343 0.093 Uiso 1 1 calc R . . C31 C 0.3667(2) 0.2453(4) 0.05481(17) 0.0332(8) Uani 1 1 d . . . H31 H 0.3483 0.2024 0.0949 0.040 Uiso 1 1 calc R . . C32 C 0.3291(3) 0.1652(4) -0.00576(18) 0.0409(9) Uani 1 1 d . . . H32A H 0.3448 0.2071 -0.0459 0.061 Uiso 1 1 calc R . . H32B H 0.2681 0.1640 -0.0073 0.061 Uiso 1 1 calc R . . H32C H 0.3504 0.0733 -0.0027 0.061 Uiso 1 1 calc R . . C33 C 0.3337(3) 0.3894(4) 0.0511(2) 0.0423(9) Uani 1 1 d . . . H33A H 0.3595 0.4401 0.0892 0.063 Uiso 1 1 calc R . . H33B H 0.2730 0.3886 0.0514 0.063 Uiso 1 1 calc R . . H33C H 0.3476 0.4315 0.0105 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 Sn1 0.02746(13) 0.01950(10) 0.02160(11) 0.00004(9) 0.00222(8) 0.00089(10) Fe1 0.0338(3) 0.0205(2) 0.0337(3) -0.00247(19) 0.0036(2) -0.0013(2) O1 0.057(2) 0.0561(18) 0.0344(15) 0.0025(13) -0.0051(14) -0.0171(15) O2 0.038(2) 0.0398(17) 0.117(3) -0.0031(17) 0.0013(19) 0.0085(14) O3 0.0447(18) 0.0276(14) 0.088(2) -0.0100(15) -0.0025(16) -0.0042(14) O4 0.084(3) 0.0442(17) 0.0418(16) 0.0050(13) 0.0251(17) -0.0104(16) O5 0.0290(13) 0.0301(12) 0.0305(12) 0.0038(11) 0.0015(10) 0.0044(11) N1 0.0260(15) 0.0224(13) 0.0211(12) 0.0002(10) 0.0011(11) 0.0009(11) N2 0.0246(15) 0.0218(14) 0.0185(12) -0.0006(10) 0.0011(11) 0.0013(11) C1 0.038(2) 0.0309(18) 0.034(2) -0.0048(15) 0.0068(17) -0.0090(16) C2 0.048(3) 0.0180(17) 0.072(3) -0.0035(17) 0.003(2) -0.0073(18) C3 0.032(2) 0.032(2) 0.054(2) -0.0020(17) 0.0038(18) 0.0046(16) C4 0.052(3) 0.0226(17) 0.038(2) 0.0016(15) 0.0019(19) -0.0068(16) C5 0.0277(19) 0.0268(17) 0.0184(15) 0.0033(12) 0.0003(13) -0.0018(13) C6 0.0302(19) 0.0276(17) 0.0262(16) 0.0038(13) 0.0059(14) -0.0005(14) C7 0.043(2) 0.0335(19) 0.0244(16) -0.0019(13) 0.0077(15) -0.0005(16) C8 0.045(2) 0.040(2) 0.0225(16) -0.0008(15) 0.0009(15) -0.0058(18) C9 0.033(2) 0.035(2) 0.0273(17) 0.0029(14) -0.0037(15) -0.0022(15) C10 0.032(2) 0.0274(17) 0.0270(16) 0.0037(13) 0.0022(14) 0.0002(14) C11 0.030(2) 0.042(2) 0.0310(17) -0.0020(15) 0.0054(15) 0.0066(16) C12 0.050(3) 0.049(3) 0.067(3) -0.007(2) -0.008(2) 0.016(2) C13 0.035(3) 0.081(4) 0.084(4) 0.028(3) 0.012(3) 0.001(2) C14 0.031(2) 0.038(2) 0.0302(18) -0.0014(15) -0.0002(15) 0.0058(16) C15 0.042(3) 0.066(3) 0.038(2) -0.0088(19) 0.0094(19) 0.000(2) C16 0.065(3) 0.049(3) 0.059(3) 0.013(2) 0.011(2) 0.022(2) C17 0.042(2) 0.0346(19) 0.0326(19) 0.0036(15) 0.0064(17) -0.0068(17) C18 0.0240(18) 0.0254(16) 0.0258(16) 0.0030(13) 0.0029(13) -0.0002(13) C19 0.0274(19) 0.0186(15) 0.0303(17) -0.0004(12) 0.0016(14) -0.0043(13) C20 0.0246(18) 0.0195(15) 0.0276(16) 0.0005(12) 0.0002(14) -0.0002(13) C21 0.040(2) 0.0249(17) 0.0300(17) -0.0031(13) 0.0056(16) -0.0038(15) C22 0.0321(19) 0.0212(15) 0.0210(14) -0.0047(12) 0.0063(13) -0.0027(14) C23 0.0308(19) 0.0294(17) 0.0256(16) -0.0046(14) 0.0044(14) -0.0038(16) C24 0.034(2) 0.041(2) 0.0333(19) -0.0015(15) 0.0112(17) -0.0034(16) C25 0.046(2) 0.036(2) 0.0278(18) 0.0006(14) 0.0126(17) -0.0055(16) C26 0.046(2) 0.0345(19) 0.0242(17) 0.0032(14) 0.0065(16) 0.0004(16) C27 0.035(2) 0.0226(16) 0.0238(16) -0.0006(13) 0.0030(15) -0.0008(14) C28 0.027(2) 0.046(2) 0.0299(18) 0.0026(15) 0.0032(15) -0.0016(16) C29 0.054(3) 0.067(3) 0.056(3) 0.009(2) -0.017(2) -0.021(2) C30 0.069(4) 0.057(3) 0.057(3) 0.006(2) -0.011(3) 0.015(2) C31 0.038(2) 0.0353(19) 0.0256(18) 0.0049(14) 0.0012(16) -0.0001(16) C32 0.044(2) 0.042(2) 0.0349(19) 0.0020(16) -0.0047(17) -0.0049(18) C33 0.044(3) 0.044(2) 0.038(2) 0.0063(17) 0.0024(18) 0.0063(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sn1 O5 2.003(2) . ? Sn1 N2 2.125(2) . ? Sn1 N1 2.130(3) . ? Sn1 Fe1 2.4720(7) . ? Fe1 C3 1.776(4) . ? Fe1 C4 1.788(4) . ? Fe1 C2 1.789(5) . ? Fe1 C1 1.796(4) . ? O1 C1 1.146(5) . ? O2 C2 1.166(5) . ? O3 C3 1.145(5) . ? O4 C4 1.150(5) . ? N1 C18 1.341(4) . ? N1 C5 1.454(4) . ? N2 C20 1.334(4) . ? N2 C22 1.455(4) . ? C5 C6 1.398(5) . ? C5 C10 1.404(5) . ? C6 C7 1.396(5) . ? C6 C11 1.522(5) . ? C7 C8 1.381(6) . ? C8 C9 1.377(5) . ? C9 C10 1.396(5) . ? C10 C14 1.525(5) . ? C11 C12 1.518(6) . ? C11 C13 1.520(6) . ? C14 C15 1.521(6) . ? C14 C16 1.533(5) . ? C17 C18 1.501(5) . ? C18 C19 1.399(5) . ? C19 C20 1.392(5) . ? C20 C21 1.508(4) . ? C22 C23 1.397(5) . ? C22 C27 1.407(5) . ? C23 C24 1.396(5) . ? C23 C28 1.521(5) . ? C24 C25 1.380(6) . ? C25 C26 1.373(6) . ? C26 C27 1.397(5) . ? C27 C31 1.512(5) . ? C28 C29 1.515(6) . ? C28 C30 1.523(6) . ? C31 C33 1.535(5) . ? C31 C32 1.540(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 O5 Sn1 N2 97.00(10) . . ? O5 Sn1 N1 97.12(10) . . ? N2 Sn1 N1 88.41(10) . . ? O5 Sn1 Fe1 115.24(7) . . ? N2 Sn1 Fe1 126.49(7) . . ? N1 Sn1 Fe1 125.31(7) . . ? C3 Fe1 C4 89.79(17) . . ? C3 Fe1 C2 93.17(17) . . ? C4 Fe1 C2 118.0(2) . . ? C3 Fe1 C1 88.79(17) . . ? C4 Fe1 C1 118.85(19) . . ? C2 Fe1 C1 123.1(2) . . ? C3 Fe1 Sn1 177.04(13) . . ? C4 Fe1 Sn1 92.97(11) . . ? C2 Fe1 Sn1 84.58(12) . . ? C1 Fe1 Sn1 90.82(11) . . ? C18 N1 C5 121.5(3) . . ? C18 N1 Sn1 119.3(2) . . ? C5 N1 Sn1 119.07(19) . . ? C20 N2 C22 121.1(3) . . ? C20 N2 Sn1 119.7(2) . . ? C22 N2 Sn1 118.12(19) . . ? O1 C1 Fe1 173.5(3) . . ? O2 C2 Fe1 176.5(3) . . ? O3 C3 Fe1 179.2(4) . . ? O4 C4 Fe1 173.3(3) . . ? C6 C5 C10 121.9(3) . . ? C6 C5 N1 119.2(3) . . ? C10 C5 N1 118.9(3) . . ? C7 C6 C5 117.9(3) . . ? C7 C6 C11 119.2(3) . . ? C5 C6 C11 122.7(3) . . ? C8 C7 C6 120.9(3) . . ? C9 C8 C7 120.4(3) . . ? C8 C9 C10 121.0(3) . . ? C9 C10 C5 117.9(3) . . ? C9 C10 C14 118.8(3) . . ? C5 C10 C14 123.2(3) . . ? C12 C11 C13 110.7(4) . . ? C12 C11 C6 113.4(3) . . ? C13 C11 C6 109.5(3) . . ? C15 C14 C10 111.0(3) . . ? C15 C14 C16 110.0(4) . . ? C10 C14 C16 111.6(3) . . ? N1 C18 C19 123.2(3) . . ? N1 C18 C17 120.2(3) . . ? C19 C18 C17 116.5(3) . . ? C20 C19 C18 129.6(3) . . ? N2 C20 C19 124.2(3) . . ? N2 C20 C21 118.1(3) . . ? C19 C20 C21 117.7(3) . . ? C23 C22 C27 122.3(3) . . ? C23 C22 N2 119.1(3) . . ? C27 C22 N2 118.5(3) . . ? C24 C23 C22 117.7(3) . . ? C24 C23 C28 119.2(3) . . ? C22 C23 C28 123.0(3) . . ? C25 C24 C23 120.7(4) . . ? C26 C25 C24 120.8(3) . . ? C25 C26 C27 121.0(3) . . ? C26 C27 C22 117.4(3) . . ? C26 C27 C31 118.8(3) . . ? C22 C27 C31 123.8(3) . . ? C29 C28 C23 111.7(3) . . ? C29 C28 C30 109.3(4) . . ? C23 C28 C30 111.7(3) . . ? C27 C31 C33 111.5(3) . . ? C27 C31 C32 111.0(3) . . ? C33 C31 C32 110.3(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.840 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.081