# 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_Fe2Nx6B2Bu2BC6H4B #TrackingRef '19118_web_deposit_cif_file_0_AnnaV.Vologzhanina_1364900824.im170_corr.cif' _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H70 B4 Fe2 N12 O12, 2(C H2 Cl2)' _chemical_formula_sum 'C52 H74 B4 Cl4 Fe2 N12 O12' _chemical_formula_weight 1355.97 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.866(2) _cell_length_b 13.363(3) _cell_length_c 13.750(5) _cell_angle_alpha 110.849(7) _cell_angle_beta 104.086(7) _cell_angle_gamma 104.756(5) _cell_volume 1522.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 789 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 25.76 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_F_000 706 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_absorpt_coefficient_mu 0.722 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker Apex 2 CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19293 _diffrn_reflns_av_unetI/netI 0.1637 _diffrn_reflns_av_R_equivalents 0.1432 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.706 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5979 _reflns_number_gt 3388 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 2008)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 2008)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5979 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1394 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.71042(8) 0.61167(6) 0.31414(6) 0.01099(18) Uani 1 1 d . . . . . O1 O 0.7516(3) 0.4454(2) 0.1318(3) 0.0156(8) Uani 1 1 d . . . . . O2 O 0.6444(3) 0.8101(3) 0.3098(3) 0.0160(8) Uani 1 1 d . . . . . O3 O 0.7153(3) 0.3846(2) 0.2760(3) 0.0137(8) Uani 1 1 d . . . . . O4 O 0.4739(3) 0.6886(3) 0.3628(3) 0.0149(8) Uani 1 1 d . . . . . O5 O 0.9565(3) 0.5277(2) 0.3132(3) 0.0145(8) Uani 1 1 d . . . . . O6 O 0.7312(3) 0.8169(2) 0.4954(2) 0.0134(8) Uani 1 1 d . . . . . N1 N 0.7123(4) 0.5396(3) 0.1683(3) 0.0137(9) Uani 1 1 d . . . . . N2 N 0.6802(4) 0.7173(3) 0.2570(3) 0.0148(10) Uani 1 1 d . . . . . N3 N 0.6455(4) 0.4621(3) 0.3070(3) 0.0124(9) Uani 1 1 d . . . . . N4 N 0.5234(4) 0.5990(3) 0.3334(3) 0.0133(9) Uani 1 1 d . . . . . N5 N 0.9101(4) 0.6147(3) 0.3656(3) 0.0130(9) Uani 1 1 d . . . . . N6 N 0.7991(4) 0.7424(3) 0.4560(3) 0.0124(9) Uani 1 1 d . . . . . C1 C 0.7038(5) 0.5939(4) 0.1056(4) 0.0112(11) Uani 1 1 d . . . . . C2 C 0.6743(5) 0.6964(4) 0.1555(4) 0.0109(11) Uani 1 1 d . . . . . C3 C 0.6480(5) 0.7696(4) 0.0989(4) 0.0164(12) Uani 1 1 d . . . . . H3A H 0.7317 0.8462 0.1400 0.020 Uiso 1 1 calc R U . . . H3B H 0.5532 0.7814 0.1001 0.020 Uiso 1 1 calc R U . . . C4 C 0.6373(5) 0.7136(4) -0.0227(4) 0.0194(12) Uani 1 1 d . . . . . H4A H 0.5357 0.6527 -0.0698 0.023 Uiso 1 1 calc R U . . . H4B H 0.6513 0.7727 -0.0509 0.023 Uiso 1 1 calc R U . . . C5 C 0.7559(5) 0.6607(4) -0.0327(4) 0.0185(12) Uani 1 1 d . . . . . H5A H 0.7530 0.6326 -0.1105 0.022 Uiso 1 1 calc R U . . . H5B H 0.8573 0.7206 0.0175 0.022 Uiso 1 1 calc R U . . . C6 C 0.7285(5) 0.5610(4) -0.0017(4) 0.0158(12) Uani 1 1 d . . . . . H6A H 0.6390 0.4940 -0.0619 0.019 Uiso 1 1 calc R U . . . H6B H 0.8165 0.5377 0.0049 0.019 Uiso 1 1 calc R U . . . C7 C 0.5151(5) 0.4213(4) 0.3152(4) 0.0105(11) Uani 1 1 d . . . . . C8 C 0.4467(5) 0.5062(4) 0.3367(4) 0.0099(11) Uani 1 1 d . . . . . C9 C 0.3070(5) 0.4868(4) 0.3622(4) 0.0122(11) Uani 1 1 d . . . . . H9A H 0.2227 0.4768 0.2987 0.015 Uiso 1 1 calc R U . . . H9B H 0.3217 0.5555 0.4294 0.015 Uiso 1 1 calc R U . . . C10 C 0.2665(5) 0.3805(4) 0.3831(4) 0.0152(12) Uani 1 1 d . . . . . H10A H 0.1618 0.3589 0.3812 0.018 Uiso 1 1 calc R U . . . H10B H 0.3344 0.3989 0.4585 0.018 Uiso 1 1 calc R U . . . C11 C 0.2800(5) 0.2784(4) 0.2953(4) 0.0139(11) Uani 1 1 d . . . . . H11A H 0.2422 0.2084 0.3059 0.017 Uiso 1 1 calc R U . . . H11B H 0.2175 0.2631 0.2195 0.017 Uiso 1 1 calc R U . . . C12 C 0.4431(5) 0.3043(4) 0.3055(4) 0.0118(11) Uani 1 1 d . . . . . H12A H 0.4998 0.2989 0.3724 0.014 Uiso 1 1 calc R U . . . H12B H 0.4474 0.2457 0.2389 0.014 Uiso 1 1 calc R U . . . C13 C 1.0074(5) 0.6967(4) 0.4622(4) 0.0144(11) Uani 1 1 d . . . . . C14 C 0.9435(5) 0.7779(4) 0.5129(4) 0.0119(11) Uani 1 1 d . . . . . C15 C 1.0374(5) 0.8901(4) 0.6152(4) 0.0156(12) Uani 1 1 d . . . . . H15A H 1.0144 0.8865 0.6803 0.019 Uiso 1 1 calc R U . . . H15B H 1.0127 0.9535 0.6040 0.019 Uiso 1 1 calc R U . . . C16 C 1.2017(5) 0.9141(4) 0.6379(4) 0.0287(14) Uani 1 1 d . . . . . H16A H 1.2290 0.9378 0.5825 0.034 Uiso 1 1 calc R U . . . H16B H 1.2613 0.9796 0.7132 0.034 Uiso 1 1 calc R U . . . C17 C 1.2438(6) 0.8135(4) 0.6327(4) 0.0266(14) Uani 1 1 d . . . . . H17A H 1.2191 0.7910 0.6894 0.032 Uiso 1 1 calc R U . . . H17B H 1.3541 0.8370 0.6521 0.032 Uiso 1 1 calc R U . . . C18 C 1.1646(5) 0.7096(4) 0.5189(4) 0.0164(12) Uani 1 1 d . . . . . H18A H 1.2229 0.7172 0.4709 0.020 Uiso 1 1 calc R U . . . H18B H 1.1621 0.6389 0.5279 0.020 Uiso 1 1 calc R U . . . C19 C 0.8831(5) 0.3209(4) 0.1752(4) 0.0131(9) Uani 1 1 d . . . . . H19A H 0.9593 0.3481 0.1456 0.016 Uiso 1 1 calc R U . . . H19B H 0.9339 0.3058 0.2370 0.016 Uiso 1 1 calc R U . . . C20 C 0.7611(5) 0.2078(4) 0.0828(4) 0.0181(12) Uani 1 1 d . . . . . H20A H 0.6882 0.1777 0.1136 0.022 Uiso 1 1 calc R U . . . H20B H 0.7060 0.2233 0.0228 0.022 Uiso 1 1 calc R U . . . C21 C 0.8201(6) 0.1153(4) 0.0319(5) 0.0371(11) Uani 1 1 d . . . . . H21A H 0.8998 0.1476 0.0072 0.045 Uiso 1 1 calc R U . . . H21B H 0.8668 0.0943 0.0902 0.045 Uiso 1 1 calc R U . . . C22 C 0.6993(6) 0.0068(4) -0.0670(4) 0.0371(11) Uani 1 1 d . . . . . H22A H 0.7452 -0.0479 -0.0977 0.056 Uiso 1 1 calc R U . . . H22B H 0.6514 0.0268 -0.1249 0.056 Uiso 1 1 calc R U . . . H22C H 0.6231 -0.0286 -0.0423 0.056 Uiso 1 1 calc R U . . . C23 C 0.5447(5) 0.9062(4) 0.4542(4) 0.0121(11) Uani 1 1 d . . . . . C24 C 0.5694(5) 0.9595(4) 0.5679(4) 0.0143(11) Uani 1 1 d . . . . . H24A H 0.6167 0.9319 0.6160 0.017 Uiso 1 1 calc R U . . . C25 C 0.4728(5) 0.9493(4) 0.3879(4) 0.0156(12) Uani 1 1 d . . . . . H25A H 0.4523 0.9147 0.3097 0.019 Uiso 1 1 calc R U . . . B1 B 0.8251(6) 0.4212(5) 0.2248(5) 0.0131(9) Uani 1 1 d . . . . . B2 B 0.5977(6) 0.8043(5) 0.4042(5) 0.0140(13) Uani 1 1 d . . . . . C1S C 0.1378(6) 0.7172(4) 0.2393(4) 0.0307(15) Uani 1 1 d . . . . . H1SA H 0.2345 0.7417 0.3004 0.037 Uiso 1 1 calc R U . . . H1SB H 0.0679 0.6445 0.2317 0.037 Uiso 1 1 calc R U . . . Cl1 Cl 0.16870(16) 0.69154(12) 0.11377(12) 0.0355(4) Uani 1 1 d . . . . . Cl2 Cl 0.06106(16) 0.82466(12) 0.27476(13) 0.0371(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0118(4) 0.0091(4) 0.0127(4) 0.0038(3) 0.0060(3) 0.0051(3) O1 0.021(2) 0.0099(18) 0.014(2) 0.0019(15) 0.0064(16) 0.0079(16) O2 0.022(2) 0.0103(18) 0.021(2) 0.0056(16) 0.0122(17) 0.0127(16) O3 0.0139(18) 0.0104(17) 0.019(2) 0.0035(16) 0.0098(16) 0.0087(15) O4 0.0164(19) 0.0118(18) 0.020(2) 0.0041(16) 0.0106(17) 0.0101(16) O5 0.0137(18) 0.0080(17) 0.018(2) -0.0011(15) 0.0084(16) 0.0068(15) O6 0.0125(18) 0.0096(17) 0.018(2) 0.0024(15) 0.0065(16) 0.0076(15) N1 0.015(2) 0.007(2) 0.018(2) 0.0047(19) 0.006(2) 0.0032(18) N2 0.015(2) 0.011(2) 0.019(3) 0.005(2) 0.007(2) 0.0075(19) N3 0.013(2) 0.011(2) 0.017(2) 0.0053(19) 0.008(2) 0.0085(19) N4 0.021(2) 0.006(2) 0.013(2) 0.0013(18) 0.008(2) 0.0073(19) N5 0.017(2) 0.010(2) 0.017(2) 0.0060(19) 0.009(2) 0.0095(19) N6 0.015(2) 0.011(2) 0.016(2) 0.0056(19) 0.009(2) 0.0095(19) C1 0.012(3) 0.013(3) 0.006(3) 0.004(2) 0.003(2) 0.003(2) C2 0.009(3) 0.006(2) 0.011(3) 0.002(2) 0.003(2) -0.002(2) C3 0.021(3) 0.013(3) 0.018(3) 0.008(2) 0.010(3) 0.008(2) C4 0.023(3) 0.018(3) 0.021(3) 0.013(3) 0.008(3) 0.008(3) C5 0.025(3) 0.018(3) 0.010(3) 0.004(2) 0.008(3) 0.005(2) C6 0.014(3) 0.011(3) 0.016(3) 0.001(2) 0.005(2) 0.003(2) C7 0.015(3) 0.008(3) 0.008(3) 0.003(2) 0.004(2) 0.005(2) C8 0.011(3) 0.009(3) 0.008(3) 0.003(2) 0.001(2) 0.006(2) C9 0.015(3) 0.010(3) 0.010(3) 0.000(2) 0.007(2) 0.006(2) C10 0.003(2) 0.022(3) 0.021(3) 0.012(3) 0.004(2) 0.003(2) C11 0.018(3) 0.009(3) 0.017(3) 0.008(2) 0.007(2) 0.005(2) C12 0.014(3) 0.009(3) 0.014(3) 0.007(2) 0.005(2) 0.005(2) C13 0.016(3) 0.010(3) 0.014(3) 0.005(2) 0.003(2) 0.004(2) C14 0.014(3) 0.013(3) 0.014(3) 0.007(2) 0.009(2) 0.009(2) C15 0.015(3) 0.012(3) 0.019(3) 0.003(2) 0.007(3) 0.008(2) C16 0.020(3) 0.017(3) 0.032(4) -0.002(3) 0.003(3) 0.006(3) C17 0.021(3) 0.020(3) 0.032(4) 0.006(3) 0.006(3) 0.009(3) C18 0.015(3) 0.019(3) 0.013(3) 0.007(2) 0.004(2) 0.004(2) C19 0.014(2) 0.010(2) 0.019(2) 0.0066(18) 0.0087(18) 0.0071(17) C20 0.018(3) 0.017(3) 0.013(3) 0.002(2) 0.004(2) 0.005(2) C21 0.047(3) 0.016(2) 0.035(3) -0.0022(19) 0.017(2) 0.010(2) C22 0.047(3) 0.016(2) 0.035(3) -0.0022(19) 0.017(2) 0.010(2) C23 0.008(3) 0.010(3) 0.017(3) 0.005(2) 0.006(2) 0.002(2) C24 0.018(3) 0.010(3) 0.018(3) 0.006(2) 0.008(2) 0.009(2) C25 0.016(3) 0.013(3) 0.016(3) 0.004(2) 0.006(2) 0.006(2) B1 0.014(2) 0.010(2) 0.019(2) 0.0066(18) 0.0087(18) 0.0071(17) B2 0.014(3) 0.010(3) 0.018(3) 0.006(3) 0.007(3) 0.004(3) C1S 0.031(3) 0.037(4) 0.035(4) 0.021(3) 0.022(3) 0.012(3) Cl1 0.0387(9) 0.0399(9) 0.0306(9) 0.0142(8) 0.0180(8) 0.0160(8) Cl2 0.0257(8) 0.0370(9) 0.0374(10) 0.0060(8) 0.0116(7) 0.0103(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 1.894(4) . ? Fe1 N2 1.895(4) . ? Fe1 N3 1.895(4) . ? Fe1 N1 1.898(4) . ? Fe1 N4 1.902(4) . ? Fe1 N5 1.909(4) . ? O1 N1 1.372(4) . ? O1 B1 1.491(6) . ? O2 N2 1.377(4) . ? O2 B2 1.500(6) . ? O3 N3 1.386(4) . ? O3 B1 1.503(6) . ? O4 N4 1.372(4) . ? O4 B2 1.510(6) . ? O5 N5 1.384(4) . ? O5 B1 1.498(6) . ? O6 N6 1.366(4) . ? O6 B2 1.506(6) . ? N1 C1 1.311(5) . ? N2 C2 1.304(5) . ? N3 C7 1.312(5) . ? N4 C8 1.300(5) . ? N5 C13 1.302(5) . ? N6 C14 1.310(5) . ? C1 C2 1.436(6) . ? C1 C6 1.482(6) . ? C2 C3 1.485(6) . ? C3 C4 1.533(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.523(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.518(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.441(6) . ? C7 C12 1.486(6) . ? C8 C9 1.486(6) . ? C9 C10 1.522(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.528(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.516(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.443(6) . ? C13 C18 1.491(6) . ? C14 C15 1.498(6) . ? C15 C16 1.499(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.489(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.513(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.519(6) . ? C19 B1 1.588(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.518(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.516(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.392(6) . ? C23 C24 1.394(6) . ? C23 B2 1.572(7) . ? C24 C25 1.372(6) 2_676 ? C24 H24A 0.9500 . ? C25 C24 1.372(6) 2_676 ? C25 H25A 0.9500 . ? C1S Cl1 1.754(5) . ? C1S Cl2 1.763(5) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? 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 N6 Fe1 N2 85.09(16) . . ? N6 Fe1 N3 118.98(16) . . ? N2 Fe1 N3 150.14(16) . . ? N6 Fe1 N1 147.70(16) . . ? N2 Fe1 N1 78.33(16) . . ? N3 Fe1 N1 86.96(16) . . ? N6 Fe1 N4 86.19(16) . . ? N2 Fe1 N4 86.18(16) . . ? N3 Fe1 N4 78.71(16) . . ? N1 Fe1 N4 119.68(16) . . ? N6 Fe1 N5 78.28(16) . . ? N2 Fe1 N5 118.18(16) . . ? N3 Fe1 N5 85.88(15) . . ? N1 Fe1 N5 85.39(16) . . ? N4 Fe1 N5 149.32(16) . . ? N1 O1 B1 112.8(3) . . ? N2 O2 B2 112.4(3) . . ? N3 O3 B1 112.1(3) . . ? N4 O4 B2 112.3(3) . . ? N5 O5 B1 111.5(3) . . ? N6 O6 B2 112.5(3) . . ? C1 N1 O1 116.3(4) . . ? C1 N1 Fe1 118.6(3) . . ? O1 N1 Fe1 123.8(3) . . ? C2 N2 O2 115.3(4) . . ? C2 N2 Fe1 119.8(3) . . ? O2 N2 Fe1 124.4(3) . . ? C7 N3 O3 116.3(4) . . ? C7 N3 Fe1 119.0(3) . . ? O3 N3 Fe1 123.9(3) . . ? C8 N4 O4 116.0(4) . . ? C8 N4 Fe1 118.7(3) . . ? O4 N4 Fe1 124.3(3) . . ? C13 N5 O5 115.8(4) . . ? C13 N5 Fe1 119.4(3) . . ? O5 N5 Fe1 124.4(3) . . ? C14 N6 O6 115.4(4) . . ? C14 N6 Fe1 119.0(3) . . ? O6 N6 Fe1 124.4(3) . . ? N1 C1 C2 112.0(4) . . ? N1 C1 C6 126.2(4) . . ? C2 C1 C6 121.8(4) . . ? N2 C2 C1 110.8(4) . . ? N2 C2 C3 125.8(4) . . ? C1 C2 C3 123.3(4) . . ? C2 C3 C4 111.2(4) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 111.5(4) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 111.0(4) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C1 C6 C5 111.2(4) . . ? C1 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C1 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C8 111.2(4) . . ? N3 C7 C12 126.3(4) . . ? C8 C7 C12 122.4(4) . . ? N4 C8 C7 112.1(4) . . ? N4 C8 C9 125.9(4) . . ? C7 C8 C9 122.0(4) . . ? C8 C9 C10 111.5(4) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C11 111.4(4) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 110.4(4) . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C7 C12 C11 111.6(4) . . ? C7 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C7 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N5 C13 C14 111.1(4) . . ? N5 C13 C18 127.1(4) . . ? C14 C13 C18 121.8(4) . . ? N6 C14 C13 111.6(4) . . ? N6 C14 C15 126.1(4) . . ? C13 C14 C15 122.2(4) . . ? C14 C15 C16 110.1(4) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 113.7(4) . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C16 C17 C18 113.4(4) . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C13 C18 C17 112.6(4) . . ? C13 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C13 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 B1 115.0(4) . . ? C20 C19 H19A 108.5 . . ? B1 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? B1 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C21 C20 C19 114.1(4) . . ? C21 C20 H20A 108.7 . . ? C19 C20 H20A 108.7 . . ? C21 C20 H20B 108.7 . . ? C19 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C20 113.5(5) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 116.3(4) . . ? C25 C23 B2 121.9(4) . . ? C24 C23 B2 121.8(4) . . ? C25 C24 C23 121.8(5) 2_676 . ? C25 C24 H24A 119.1 2_676 . ? C23 C24 H24A 119.1 . . ? C24 C25 C23 121.9(5) 2_676 . ? C24 C25 H25A 119.1 2_676 . ? C23 C25 H25A 119.1 . . ? O1 B1 O5 109.7(4) . . ? O1 B1 O3 110.7(4) . . ? O5 B1 O3 109.1(4) . . ? O1 B1 C19 108.4(4) . . ? O5 B1 C19 109.4(4) . . ? O3 B1 C19 109.6(4) . . ? O2 B2 O6 109.0(4) . . ? O2 B2 O4 109.6(4) . . ? O6 B2 O4 108.8(4) . . ? O2 B2 C23 110.1(4) . . ? O6 B2 C23 108.2(4) . . ? O4 B2 C23 111.1(4) . . ? Cl1 C1S Cl2 111.9(3) . . ? Cl1 C1S H1SA 109.2 . . ? Cl2 C1S H1SA 109.2 . . ? Cl1 C1S H1SB 109.2 . . ? Cl2 C1S H1SB 109.2 . . ? H1SA C1S H1SB 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 O1 N1 C1 154.0(4) . . . . ? B1 O1 N1 Fe1 -12.8(5) . . . . ? N6 Fe1 N1 C1 -56.2(5) . . . . ? N2 Fe1 N1 C1 4.4(3) . . . . ? N3 Fe1 N1 C1 158.3(4) . . . . ? N4 Fe1 N1 C1 83.1(4) . . . . ? N5 Fe1 N1 C1 -115.6(4) . . . . ? N6 Fe1 N1 O1 110.3(4) . . . . ? N2 Fe1 N1 O1 171.0(3) . . . . ? N3 Fe1 N1 O1 -35.2(3) . . . . ? N4 Fe1 N1 O1 -110.3(3) . . . . ? N5 Fe1 N1 O1 50.9(3) . . . . ? B2 O2 N2 C2 158.9(4) . . . . ? B2 O2 N2 Fe1 -12.9(5) . . . . ? N6 Fe1 N2 C2 152.3(4) . . . . ? N3 Fe1 N2 C2 -61.9(5) . . . . ? N1 Fe1 N2 C2 0.2(3) . . . . ? N4 Fe1 N2 C2 -121.2(4) . . . . ? N5 Fe1 N2 C2 78.4(4) . . . . ? N6 Fe1 N2 O2 -36.2(3) . . . . ? N3 Fe1 N2 O2 109.6(4) . . . . ? N1 Fe1 N2 O2 171.6(3) . . . . ? N4 Fe1 N2 O2 50.3(3) . . . . ? N5 Fe1 N2 O2 -110.1(3) . . . . ? B1 O3 N3 C7 157.0(4) . . . . ? B1 O3 N3 Fe1 -12.7(5) . . . . ? N6 Fe1 N3 C7 80.4(4) . . . . ? N2 Fe1 N3 C7 -59.8(5) . . . . ? N1 Fe1 N3 C7 -119.8(4) . . . . ? N4 Fe1 N3 C7 1.3(3) . . . . ? N5 Fe1 N3 C7 154.6(4) . . . . ? N6 Fe1 N3 O3 -110.1(3) . . . . ? N2 Fe1 N3 O3 109.7(4) . . . . ? N1 Fe1 N3 O3 49.6(3) . . . . ? N4 Fe1 N3 O3 170.7(3) . . . . ? N5 Fe1 N3 O3 -36.0(3) . . . . ? B2 O4 N4 C8 155.7(4) . . . . ? B2 O4 N4 Fe1 -13.3(5) . . . . ? B1 O5 N5 C13 161.4(4) . . . . ? B1 O5 N5 Fe1 -11.1(5) . . . . ? B2 O6 N6 C14 151.7(4) . . . . ? B2 O6 N6 Fe1 -15.5(5) . . . . ? N2 Fe1 N6 C14 -114.0(4) . . . . ? N3 Fe1 N6 C14 84.7(4) . . . . ? N1 Fe1 N6 C14 -55.1(5) . . . . ? N4 Fe1 N6 C14 159.5(4) . . . . ? N5 Fe1 N6 C14 6.1(3) . . . . ? N2 Fe1 N6 O6 52.7(3) . . . . ? N3 Fe1 N6 O6 -108.6(3) . . . . ? N1 Fe1 N6 O6 111.6(4) . . . . ? N4 Fe1 N6 O6 -33.8(3) . . . . ? N5 Fe1 N6 O6 172.8(3) . . . . ? O1 N1 C1 C2 -175.2(3) . . . . ? Fe1 N1 C1 C2 -7.6(5) . . . . ? O1 N1 C1 C6 1.8(7) . . . . ? Fe1 N1 C1 C6 169.3(4) . . . . ? O2 N2 C2 C1 -176.3(3) . . . . ? Fe1 N2 C2 C1 -4.1(5) . . . . ? O2 N2 C2 C3 6.4(6) . . . . ? Fe1 N2 C2 C3 178.6(3) . . . . ? N1 C1 C2 N2 7.2(6) . . . . ? C6 C1 C2 N2 -169.9(4) . . . . ? N1 C1 C2 C3 -175.4(4) . . . . ? C6 C1 C2 C3 7.5(7) . . . . ? N2 C2 C3 C4 -176.0(4) . . . . ? C1 C2 C3 C4 7.0(6) . . . . ? C2 C3 C4 C5 -41.8(5) . . . . ? C3 C4 C5 C6 64.9(5) . . . . ? N1 C1 C6 C5 -162.9(4) . . . . ? C2 C1 C6 C5 13.8(6) . . . . ? C4 C5 C6 C1 -48.6(5) . . . . ? O3 N3 C7 C8 -174.2(3) . . . . ? Fe1 N3 C7 C8 -4.0(5) . . . . ? O3 N3 C7 C12 6.4(7) . . . . ? Fe1 N3 C7 C12 176.6(3) . . . . ? O4 N4 C8 C7 -174.4(4) . . . . ? Fe1 N4 C8 C7 -4.7(5) . . . . ? O4 N4 C8 C9 3.9(6) . . . . ? Fe1 N4 C8 C9 173.6(3) . . . . ? N3 C7 C8 N4 5.4(6) . . . . ? C12 C7 C8 N4 -175.1(4) . . . . ? N3 C7 C8 C9 -173.0(4) . . . . ? C12 C7 C8 C9 6.5(7) . . . . ? N4 C8 C9 C10 -167.8(4) . . . . ? C7 C8 C9 C10 10.3(6) . . . . ? C8 C9 C10 C11 -45.2(5) . . . . ? C9 C10 C11 C12 65.5(5) . . . . ? N3 C7 C12 C11 -168.2(4) . . . . ? C8 C7 C12 C11 12.5(6) . . . . ? C10 C11 C12 C7 -46.8(5) . . . . ? O5 N5 C13 C14 -175.7(4) . . . . ? Fe1 N5 C13 C14 -2.8(5) . . . . ? O5 N5 C13 C18 3.4(7) . . . . ? Fe1 N5 C13 C18 176.3(4) . . . . ? O6 N6 C14 C13 -177.0(4) . . . . ? Fe1 N6 C14 C13 -9.2(5) . . . . ? O6 N6 C14 C15 0.5(7) . . . . ? Fe1 N6 C14 C15 168.3(4) . . . . ? N5 C13 C14 N6 7.4(6) . . . . ? C18 C13 C14 N6 -171.8(4) . . . . ? N5 C13 C14 C15 -170.2(4) . . . . ? C18 C13 C14 C15 10.6(7) . . . . ? N6 C14 C15 C16 -164.7(5) . . . . ? C13 C14 C15 C16 12.5(6) . . . . ? C14 C15 C16 C17 -47.4(6) . . . . ? C15 C16 C17 C18 61.3(6) . . . . ? N5 C13 C18 C17 -178.0(4) . . . . ? C14 C13 C18 C17 1.0(7) . . . . ? C16 C17 C18 C13 -35.3(6) . . . . ? B1 C19 C20 C21 176.5(4) . . . . ? C19 C20 C21 C22 -174.8(4) . . . . ? C25 C23 C24 C25 -1.0(8) . . . 2_676 ? B2 C23 C24 C25 178.0(4) . . . 2_676 ? C24 C23 C25 C24 1.0(8) . . . 2_676 ? B2 C23 C25 C24 -178.0(4) . . . 2_676 ? N1 O1 B1 O5 -53.9(5) . . . . ? N1 O1 B1 O3 66.5(5) . . . . ? N1 O1 B1 C19 -173.3(3) . . . . ? N5 O5 B1 O1 66.3(5) . . . . ? N5 O5 B1 O3 -55.0(5) . . . . ? N5 O5 B1 C19 -174.9(4) . . . . ? N3 O3 B1 O1 -52.3(5) . . . . ? N3 O3 B1 O5 68.5(4) . . . . ? N3 O3 B1 C19 -171.8(4) . . . . ? C20 C19 B1 O1 -59.5(5) . . . . ? C20 C19 B1 O5 -179.1(4) . . . . ? C20 C19 B1 O3 61.4(6) . . . . ? N2 O2 B2 O6 66.5(4) . . . . ? N2 O2 B2 O4 -52.6(5) . . . . ? N2 O2 B2 C23 -175.0(4) . . . . ? N6 O6 B2 O2 -51.3(5) . . . . ? N6 O6 B2 O4 68.2(4) . . . . ? N6 O6 B2 C23 -171.0(3) . . . . ? N4 O4 B2 O2 66.8(5) . . . . ? N4 O4 B2 O6 -52.3(5) . . . . ? N4 O4 B2 C23 -171.3(4) . . . . ? C25 C23 B2 O2 33.0(6) . . . . ? C24 C23 B2 O2 -146.0(4) . . . . ? C25 C23 B2 O6 152.0(4) . . . . ? C24 C23 B2 O6 -27.0(6) . . . . ? C25 C23 B2 O4 -88.6(5) . . . . ? C24 C23 B2 O4 92.4(5) . . . . ? _refine_diff_density_max 0.511 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.106 _shelxl_version_number 2013-2 _shelx_res_file ; TITL 1 in P-1 CELL 0.71073 9.8662 13.3630 13.7497 110.849 104.086 104.756 ZERR 1.00 0.0024 0.0033 0.0053 0.007 0.007 0.005 LATT 1 SFAC C H B Cl Fe N O UNIT 52 74 4 4 2 12 12 TEMP -173.000 omit -4 52 acta conf htab L.S. 8 BOND $h FMAP 2 PLAN 10 WGHT 0.010000 FVAR 0.07977 FE1 5 0.710418 0.611673 0.314143 11.00000 0.01181 0.00907 = 0.01272 0.00375 0.00597 0.00514 O1 7 0.751594 0.445350 0.131821 11.00000 0.02082 0.00995 = 0.01412 0.00191 0.00636 0.00791 O2 7 0.644435 0.810128 0.309774 11.00000 0.02230 0.01032 = 0.02104 0.00555 0.01221 0.01274 O3 7 0.715284 0.384551 0.276046 11.00000 0.01389 0.01041 = 0.01893 0.00346 0.00983 0.00867 O4 7 0.473894 0.688584 0.362776 11.00000 0.01641 0.01179 = 0.01953 0.00407 0.01062 0.01015 O5 7 0.956474 0.527671 0.313213 11.00000 0.01368 0.00803 = 0.01837 -0.00112 0.00842 0.00679 O6 7 0.731201 0.816940 0.495387 11.00000 0.01254 0.00956 = 0.01756 0.00240 0.00652 0.00762 N1 6 0.712273 0.539598 0.168297 11.00000 0.01469 0.00686 = 0.01780 0.00467 0.00556 0.00315 N2 6 0.680157 0.717297 0.256967 11.00000 0.01463 0.01094 = 0.01945 0.00528 0.00687 0.00753 N3 6 0.645531 0.462085 0.306991 11.00000 0.01312 0.01070 = 0.01658 0.00531 0.00780 0.00847 N4 6 0.523355 0.599031 0.333447 11.00000 0.02111 0.00605 = 0.01260 0.00132 0.00791 0.00732 N5 6 0.910055 0.614693 0.365580 11.00000 0.01706 0.00974 = 0.01687 0.00600 0.00876 0.00952 N6 6 0.799062 0.742369 0.455996 11.00000 0.01459 0.01082 = 0.01613 0.00560 0.00851 0.00950 C1 1 0.703784 0.593885 0.105574 11.00000 0.01192 0.01329 = 0.00621 0.00364 0.00275 0.00300 C2 1 0.674262 0.696368 0.155531 11.00000 0.00935 0.00638 = 0.01130 0.00156 0.00328 -0.00165 C3 1 0.647993 0.769616 0.098854 11.00000 0.02148 0.01323 = 0.01845 0.00850 0.00953 0.00843 AFIX 23 H3A 2 0.731696 0.846247 0.140013 11.00000 -1.20000 H3B 2 0.553234 0.781409 0.100100 11.00000 -1.20000 AFIX 0 C4 1 0.637333 0.713631 -0.022737 11.00000 0.02336 0.01766 = 0.02133 0.01328 0.00786 0.00781 AFIX 23 H4A 2 0.535697 0.652742 -0.069816 11.00000 -1.20000 H4B 2 0.651269 0.772696 -0.050904 11.00000 -1.20000 AFIX 0 C5 1 0.755924 0.660709 -0.032676 11.00000 0.02470 0.01767 = 0.01029 0.00395 0.00809 0.00534 AFIX 23 H5A 2 0.753032 0.632572 -0.110485 11.00000 -1.20000 H5B 2 0.857319 0.720564 0.017491 11.00000 -1.20000 AFIX 0 C6 1 0.728497 0.561043 -0.001709 11.00000 0.01385 0.01132 = 0.01640 0.00111 0.00545 0.00331 AFIX 23 H6A 2 0.639020 0.494014 -0.061855 11.00000 -1.20000 H6B 2 0.816540 0.537686 0.004931 11.00000 -1.20000 AFIX 0 C7 1 0.515149 0.421310 0.315217 11.00000 0.01507 0.00823 = 0.00827 0.00334 0.00414 0.00526 C8 1 0.446729 0.506164 0.336660 11.00000 0.01063 0.00946 = 0.00798 0.00255 0.00058 0.00575 C9 1 0.307041 0.486770 0.362228 11.00000 0.01523 0.00968 = 0.01003 0.00017 0.00689 0.00617 AFIX 23 H9A 2 0.222713 0.476820 0.298700 11.00000 -1.20000 H9B 2 0.321686 0.555481 0.429355 11.00000 -1.20000 AFIX 0 C10 1 0.266467 0.380471 0.383120 11.00000 0.00317 0.02222 = 0.02089 0.01174 0.00422 0.00303 AFIX 23 H10A 2 0.161810 0.358860 0.381245 11.00000 -1.20000 H10B 2 0.334425 0.398946 0.458505 11.00000 -1.20000 AFIX 0 C11 1 0.280037 0.278418 0.295342 11.00000 0.01776 0.00888 = 0.01743 0.00832 0.00666 0.00515 AFIX 23 H11A 2 0.242177 0.208426 0.305877 11.00000 -1.20000 H11B 2 0.217507 0.263066 0.219506 11.00000 -1.20000 AFIX 0 C12 1 0.443064 0.304284 0.305515 11.00000 0.01402 0.00937 = 0.01361 0.00666 0.00477 0.00477 AFIX 23 H12A 2 0.499829 0.298945 0.372366 11.00000 -1.20000 H12B 2 0.447414 0.245722 0.238850 11.00000 -1.20000 AFIX 0 C13 1 1.007365 0.696708 0.462209 11.00000 0.01571 0.01045 = 0.01442 0.00511 0.00309 0.00392 C14 1 0.943530 0.777874 0.512861 11.00000 0.01406 0.01337 = 0.01355 0.00657 0.00905 0.00872 C15 1 1.037370 0.890121 0.615198 11.00000 0.01529 0.01173 = 0.01866 0.00307 0.00723 0.00772 AFIX 23 H15A 2 1.014371 0.886532 0.680344 11.00000 -1.20000 H15B 2 1.012701 0.953518 0.604018 11.00000 -1.20000 AFIX 0 C16 1 1.201713 0.914107 0.637897 11.00000 0.01993 0.01740 = 0.03158 -0.00249 0.00292 0.00639 AFIX 23 H16A 2 1.228987 0.937822 0.582540 11.00000 -1.20000 H16B 2 1.261312 0.979639 0.713169 11.00000 -1.20000 AFIX 0 C17 1 1.243768 0.813467 0.632664 11.00000 0.02102 0.02044 = 0.03150 0.00566 0.00613 0.00917 AFIX 23 H17A 2 1.219063 0.791010 0.689406 11.00000 -1.20000 H17B 2 1.354133 0.837009 0.652090 11.00000 -1.20000 AFIX 0 C18 1 1.164591 0.709606 0.518925 11.00000 0.01460 0.01926 = 0.01340 0.00731 0.00430 0.00428 AFIX 23 H18A 2 1.222917 0.717205 0.470914 11.00000 -1.20000 H18B 2 1.162113 0.638949 0.527911 11.00000 -1.20000 AFIX 0 C19 1 0.883050 0.320851 0.175199 11.00000 0.01352 0.00970 = 0.01950 0.00665 0.00871 0.00706 AFIX 23 H19A 2 0.959342 0.348064 0.145568 11.00000 -1.20000 H19B 2 0.933882 0.305830 0.237044 11.00000 -1.20000 AFIX 0 C20 1 0.761103 0.207754 0.082821 11.00000 0.01834 0.01652 = 0.01281 0.00165 0.00440 0.00479 AFIX 23 H20A 2 0.688163 0.177679 0.113581 11.00000 -1.20000 H20B 2 0.706049 0.223275 0.022803 11.00000 -1.20000 AFIX 0 C21 1 0.820129 0.115295 0.031850 11.00000 0.04736 0.01577 = 0.03541 -0.00217 0.01715 0.01013 AFIX 23 H21A 2 0.899795 0.147602 0.007196 11.00000 -1.20000 H21B 2 0.866805 0.094346 0.090214 11.00000 -1.20000 AFIX 0 C22 1 0.699288 0.006813 -0.067010 11.00000 0.04736 0.01577 = 0.03541 -0.00217 0.01715 0.01013 AFIX 137 H22A 2 0.745170 -0.047942 -0.097717 11.00000 -1.50000 H22B 2 0.651450 0.026833 -0.124874 11.00000 -1.50000 H22C 2 0.623136 -0.028573 -0.042340 11.00000 -1.50000 AFIX 0 C23 1 0.544741 0.906152 0.454181 11.00000 0.00760 0.01006 = 0.01737 0.00483 0.00590 0.00202 C24 1 0.569385 0.959494 0.567869 11.00000 0.01850 0.00954 = 0.01794 0.00633 0.00766 0.00902 AFIX 43 H24A 2 0.616688 0.931924 0.616010 11.00000 -1.20000 AFIX 0 C25 1 0.472780 0.949331 0.387873 11.00000 0.01557 0.01321 = 0.01607 0.00428 0.00577 0.00578 AFIX 43 H25A 2 0.452267 0.914672 0.309712 11.00000 -1.20000 AFIX 0 B1 3 0.825123 0.421247 0.224755 11.00000 0.01352 0.00970 = 0.01950 0.00665 0.00871 0.00706 B2 3 0.597707 0.804256 0.404180 11.00000 0.01438 0.01037 = 0.01772 0.00647 0.00655 0.00445 C1S 1 0.137767 0.717211 0.239292 11.00000 0.03090 0.03710 = 0.03518 0.02137 0.02237 0.01221 AFIX 23 H1SA 2 0.234538 0.741653 0.300443 11.00000 -1.20000 H1SB 2 0.067944 0.644549 0.231675 11.00000 -1.20000 AFIX 0 CL1 4 0.168702 0.691536 0.113766 11.00000 0.03870 0.03992 = 0.03058 0.01418 0.01797 0.01603 CL2 4 0.061060 0.824657 0.274759 11.00000 0.02570 0.03702 = 0.03744 0.00602 0.01158 0.01032 HKLF 4 REM 1 in P-1 REM R1 = 0.0640 for 3388 Fo > 4sig(Fo) and 0.1394 for all 5979 data REM 377 parameters refined using 0 restraints END WGHT 0.0242 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z HTAB C6 Cl1_$1 EQIV $2 x-1, y, z HTAB C1S O5_$2 REM Highest difference peak 0.511, deepest hole -0.559, 1-sigma level 0.106 Q1 1 1.2742 0.8632 0.5918 11.00000 0.05 0.51 Q2 1 0.9942 0.0781 -0.1109 11.00000 0.05 0.42 Q3 1 0.7783 0.4412 0.1930 11.00000 0.05 0.42 Q4 1 0.9240 0.1359 0.1651 11.00000 0.05 0.41 Q5 1 0.6806 0.7384 0.1310 11.00000 0.05 0.39 Q6 1 0.8664 0.2505 0.1182 11.00000 0.05 0.39 Q7 1 -0.0664 0.8624 0.2896 11.00000 0.05 0.39 Q8 1 0.9977 1.0685 0.6146 11.00000 0.05 0.38 Q9 1 1.1809 0.8791 0.6906 11.00000 0.05 0.38 Q10 1 1.2184 0.9020 0.4317 11.00000 0.05 0.38 ; _database_code_depnum_ccdc_archive 'CCDC 932044'