# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name P.Deplano _publ_contact_author_name 'Deplano, Paola' _publ_contact_author_email deplano@unica.it # Attachment '- Me2pipto_Ni-Fe_ CIF check CIF.txt' data_esa605s1 _database_code_depnum_ccdc_archive 'CCDC 771140' #TrackingRef '- Me2pipto_Ni-Fe_ CIF check CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H10 N2 O S' _chemical_formula_sum 'C6 H10 N2 O S' _chemical_formula_weight 158.22 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 9.758(4) _cell_length_b 6.731(3) _cell_length_c 11.686(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 767.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 7.19 _cell_measurement_theta_max 14.19 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Walker & Stuart' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Philips PW 1100 diffractometer' _diffrn_measurement_method theta-2-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 1067 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 26.99 _reflns_number_total 962 _reflns_number_gt 565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local program' _computing_cell_refinement 'local program' _computing_data_reduction 'local program' _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for windows' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^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 -0.09(15) _refine_ls_number_reflns 962 _refine_ls_number_parameters 93 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _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 S1 S 0.74971(17) 0.60499(17) 0.89177(10) 0.0554(4) Uani 1 1 d . . . N2 N 0.7532(4) 0.9702(6) 0.8075(3) 0.0357(10) Uani 1 1 d . . . N1 N 0.5471(4) 0.8902(6) 0.6505(3) 0.0380(10) Uani 1 1 d . . . O2 O 0.5805(3) 0.5616(4) 0.6787(3) 0.0459(10) Uani 1 1 d . . . C1 C 0.7060(4) 0.7822(7) 0.8024(4) 0.0325(12) Uani 1 1 d . . . C4 C 0.7198(5) 1.1195(7) 0.7201(4) 0.0435(14) Uani 1 1 d . . . H4A H 0.7783 1.1019 0.6538 0.052 Uiso 1 1 calc R . . H4B H 0.7348 1.2519 0.7504 0.052 Uiso 1 1 calc R . . C3 C 0.5722(5) 1.0949(6) 0.6865(5) 0.0444(13) Uani 1 1 d . . . H3A H 0.5137 1.1274 0.7509 0.053 Uiso 1 1 calc R . . H3B H 0.5505 1.1849 0.6242 0.053 Uiso 1 1 calc R . . C2 C 0.6063(5) 0.7329(7) 0.7045(4) 0.0340(12) Uani 1 1 d . . . C5 C 0.4372(5) 0.8562(8) 0.5674(5) 0.0526(16) Uani 1 1 d . . . H5A H 0.4319 0.7171 0.5499 0.079 Uiso 1 1 calc R . . H5B H 0.4562 0.9294 0.4987 0.079 Uiso 1 1 calc R . . H5C H 0.3516 0.8999 0.5991 0.079 Uiso 1 1 calc R . . C6 C 0.8550(5) 1.0313(6) 0.8945(5) 0.0495(13) Uani 1 1 d . . . H6A H 0.9457 1.0068 0.8660 0.074 Uiso 1 1 calc R . . H6B H 0.8409 0.9562 0.9633 0.074 Uiso 1 1 calc R . . H6C H 0.8445 1.1703 0.9106 0.074 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 S1 0.0737(9) 0.0456(7) 0.0470(7) 0.0121(10) -0.0142(9) 0.0037(9) N2 0.035(2) 0.044(2) 0.028(2) -0.0026(18) 0.000(2) -0.001(2) N1 0.030(2) 0.044(2) 0.040(2) 0.002(2) -0.003(2) -0.001(2) O2 0.057(2) 0.0354(17) 0.045(2) -0.0082(19) -0.011(2) -0.0076(19) C1 0.035(3) 0.031(2) 0.031(3) -0.003(2) 0.005(2) 0.002(2) C4 0.054(3) 0.032(3) 0.044(3) 0.008(2) -0.002(3) -0.011(3) C3 0.050(3) 0.037(3) 0.046(3) 0.011(3) -0.002(3) 0.012(3) C2 0.032(3) 0.039(3) 0.030(3) -0.003(3) 0.006(2) -0.002(3) C5 0.041(3) 0.070(4) 0.048(3) 0.005(3) -0.014(3) -0.009(3) C6 0.040(3) 0.063(3) 0.046(3) -0.010(4) -0.006(3) -0.007(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 S1 C1 1.642(4) . ? N2 C1 1.348(5) . ? N2 C4 1.469(6) . ? N2 C6 1.480(6) . ? N1 C2 1.361(5) . ? N1 C3 1.461(5) . ? N1 C5 1.465(5) . ? O2 C2 1.218(5) . ? C1 C2 1.538(6) . ? C4 C3 1.502(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? 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 C1 N2 C4 122.4(4) . . ? C1 N2 C6 121.4(4) . . ? C4 N2 C6 115.9(4) . . ? C2 N1 C3 121.9(4) . . ? C2 N1 C5 119.8(4) . . ? C3 N1 C5 117.4(4) . . ? N2 C1 C2 116.9(4) . . ? N2 C1 S1 124.4(4) . . ? C2 C1 S1 118.7(3) . . ? N2 C4 C3 108.6(4) . . ? N2 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? N2 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? N1 C3 C4 109.9(4) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O2 C2 N1 122.3(4) . . ? O2 C2 C1 121.3(4) . . ? N1 C2 C1 116.4(4) . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.198 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.052 data_ni509 _database_code_depnum_ccdc_archive 'CCDC 771141' #TrackingRef '- ni509.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 N6 Ni O3 S3 2+, B2 F8 2-' _chemical_formula_sum 'C18 H30 B2 F8 N6 Ni O3 S3' _chemical_formula_weight 706.99 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 12.541(1) _cell_length_b 12.255(1) _cell_length_c 19.659(1) _cell_angle_alpha 90.00 _cell_angle_beta 101.198(3) _cell_angle_gamma 90.00 _cell_volume 2963.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29073 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 31.85 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart APEXII CCD' _diffrn_measurement_method 'Theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 49228 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 31.85 _reflns_number_total 9916 _reflns_number_gt 6733 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two BF4- anions were each disordered in two positions and they were refined with site occupancy factors of 0.68/0.32 and 0.55/0.45, respectively. During the refinement the B-F distance restraint of 1.37 A was applied. ; _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^)+(0.0661P)^2^+0.3702P] 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 9916 _refine_ls_number_parameters 449 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.011 _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 Ni Ni 0.295203(18) 0.106063(18) 0.332241(12) 0.03893(8) Uani 1 1 d . . . S12 S 0.22217(4) -0.07631(4) 0.33357(3) 0.05183(13) Uani 1 1 d . . . S13 S 0.39816(4) 0.09930(4) 0.24049(3) 0.04890(12) Uani 1 1 d . . . S11 S 0.13929(4) 0.18340(4) 0.25944(2) 0.04897(12) Uani 1 1 d . . . O23 O 0.37148(11) 0.25219(11) 0.35213(7) 0.0485(3) Uani 1 1 d . . . N11 N 0.07347(12) 0.22935(14) 0.44392(8) 0.0455(3) Uani 1 1 d . . . O21 O 0.21390(10) 0.14751(11) 0.40948(6) 0.0459(3) Uani 1 1 d . . . N22 N 0.30657(15) -0.20770(14) 0.43797(9) 0.0537(4) Uani 1 1 d . . . O22 O 0.42712(10) 0.03487(10) 0.39700(7) 0.0434(3) Uani 1 1 d . . . N21 N 0.00827(12) 0.31357(13) 0.31169(8) 0.0462(4) Uani 1 1 d . . . C23 C 0.43724(15) 0.28653(14) 0.31746(9) 0.0421(4) Uani 1 1 d . . . N23 N 0.55783(14) 0.24093(15) 0.23890(10) 0.0542(4) Uani 1 1 d . . . N12 N 0.51131(13) -0.11919(13) 0.44097(8) 0.0465(4) Uani 1 1 d . . . C22 C 0.42382(13) -0.06268(15) 0.41345(9) 0.0380(3) Uani 1 1 d . . . C12 C 0.31654(15) -0.12272(14) 0.39899(10) 0.0417(4) Uani 1 1 d . . . C21 C 0.13092(13) 0.20559(14) 0.39650(9) 0.0383(3) Uani 1 1 d . . . C11 C 0.08729(14) 0.24214(14) 0.32273(9) 0.0389(3) Uani 1 1 d . . . C31 C -0.02161(16) 0.30028(18) 0.43049(11) 0.0535(5) Uani 1 1 d . . . H31A H -0.0240 0.3435 0.4715 0.064 Uiso 1 1 calc R . . H31B H -0.0869 0.2560 0.4207 0.064 Uiso 1 1 calc R . . N13 N 0.47664(15) 0.38647(13) 0.32473(9) 0.0514(4) Uani 1 1 d . . . C13 C 0.47189(15) 0.21203(15) 0.26384(9) 0.0433(4) Uani 1 1 d . . . C33 C 0.55112(18) 0.4268(2) 0.28165(13) 0.0614(6) Uani 1 1 d . . . H33A H 0.5948 0.4859 0.3053 0.074 Uiso 1 1 calc R . . H33B H 0.5100 0.4549 0.2383 0.074 Uiso 1 1 calc R . . C41 C -0.0190(2) 0.37421(18) 0.37089(13) 0.0605(6) Uani 1 1 d . . . H41A H -0.0894 0.4088 0.3568 0.073 Uiso 1 1 calc R . . H41B H 0.0346 0.4310 0.3850 0.073 Uiso 1 1 calc R . . C42 C 0.3984(2) -0.2424(2) 0.49172(13) 0.0672(6) Uani 1 1 d . . . H42A H 0.3887 -0.3179 0.5039 0.081 Uiso 1 1 calc R . . H42B H 0.4012 -0.1982 0.5330 0.081 Uiso 1 1 calc R . . C32 C 0.5022(2) -0.23047(19) 0.46598(13) 0.0654(6) Uani 1 1 d . . . H32A H 0.5632 -0.2463 0.5032 0.078 Uiso 1 1 calc R . . H32B H 0.5036 -0.2819 0.4287 0.078 Uiso 1 1 calc R . . C52 C 0.62015(16) -0.0760(2) 0.44188(12) 0.0601(6) Uani 1 1 d . . . H52A H 0.6149 -0.0012 0.4271 0.090 Uiso 1 1 calc R . . H52B H 0.6547 -0.1180 0.4111 0.090 Uiso 1 1 calc R . . H52C H 0.6624 -0.0804 0.4881 0.090 Uiso 1 1 calc R . . C61 C -0.04636(19) 0.3414(2) 0.24154(12) 0.0639(6) Uani 1 1 d . . . H61A H 0.0032 0.3797 0.2185 0.096 Uiso 1 1 calc R . . H61B H -0.1079 0.3870 0.2435 0.096 Uiso 1 1 calc R . . H61C H -0.0703 0.2759 0.2164 0.096 Uiso 1 1 calc R . . C51 C 0.0976(2) 0.1749(3) 0.51108(11) 0.0693(7) Uani 1 1 d . . . H51A H 0.1208 0.1015 0.5051 0.104 Uiso 1 1 calc R . . H51B H 0.0335 0.1738 0.5310 0.104 Uiso 1 1 calc R . . H51C H 0.1543 0.2137 0.5414 0.104 Uiso 1 1 calc R . . C43 C 0.62321(18) 0.3363(2) 0.26754(14) 0.0679(6) Uani 1 1 d . . . H43A H 0.6669 0.3607 0.2348 0.081 Uiso 1 1 calc R . . H43B H 0.6719 0.3157 0.3102 0.081 Uiso 1 1 calc R . . C53 C 0.4361(2) 0.46204(18) 0.37085(14) 0.0695(6) Uani 1 1 d . . . H53A H 0.4723 0.5310 0.3705 0.104 Uiso 1 1 calc R . . H53B H 0.4500 0.4330 0.4171 0.104 Uiso 1 1 calc R . . H53C H 0.3593 0.4719 0.3554 0.104 Uiso 1 1 calc R . . C63 C 0.5995(2) 0.1721(2) 0.18892(13) 0.0738(7) Uani 1 1 d . . . H63A H 0.6289 0.1061 0.2113 0.111 Uiso 1 1 calc R . . H63B H 0.6554 0.2107 0.1717 0.111 Uiso 1 1 calc R . . H63C H 0.5413 0.1546 0.1510 0.111 Uiso 1 1 calc R . . C62 C 0.2033(2) -0.2655(3) 0.43308(15) 0.0835(9) Uani 1 1 d . . . H62A H 0.1448 -0.2193 0.4112 0.125 Uiso 1 1 calc R . . H62B H 0.1931 -0.2846 0.4788 0.125 Uiso 1 1 calc R . . H62C H 0.2042 -0.3307 0.4061 0.125 Uiso 1 1 calc R . . B2 B 0.7500(3) 0.5356(3) 0.45327(18) 0.0724(8) Uani 1 1 d D . . F7 F 0.7192(7) 0.4368(4) 0.4292(4) 0.130(3) Uani 0.545(11) 1 d P A 1 F8 F 0.8598(4) 0.5504(5) 0.4502(4) 0.1081(19) Uani 0.545(11) 1 d P A 1 F6 F 0.7487(10) 0.5516(8) 0.5201(4) 0.189(4) Uani 0.545(11) 1 d P A 1 F5 F 0.6991(7) 0.6203(7) 0.4218(6) 0.167(4) Uani 0.545(11) 1 d P A 1 F5A F 0.6695(9) 0.5191(7) 0.4902(6) 0.146(4) Uani 0.455(11) 1 d PD A 2 F6A F 0.8448(8) 0.5339(9) 0.4925(8) 0.186(5) Uani 0.455(11) 1 d PD A 2 F8A F 0.7444(8) 0.4421(7) 0.4163(5) 0.150(4) Uani 0.455(11) 1 d PD A 2 F7A F 0.7116(8) 0.6126(7) 0.4034(4) 0.124(3) Uani 0.455(11) 1 d PD A 2 B1 B 0.8079(3) 0.0714(3) 0.35355(19) 0.0773(9) Uani 1 1 d D . . F4 F 0.8265(5) 0.1459(6) 0.3076(3) 0.137(2) Uani 0.681(7) 1 d P B 3 F3 F 0.9091(4) 0.0328(4) 0.3782(3) 0.151(2) Uani 0.681(7) 1 d P B 3 F2 F 0.7671(6) 0.1213(5) 0.4006(4) 0.176(4) Uani 0.681(7) 1 d P B 3 F1 F 0.7424(3) -0.0020(4) 0.3159(3) 0.1055(15) Uani 0.681(7) 1 d P B 3 F2A F 0.8363(12) 0.0714(8) 0.4236(4) 0.131(6) Uani 0.319(7) 1 d PD B 4 F1A F 0.7873(9) -0.0440(6) 0.3482(5) 0.101(3) Uani 0.319(7) 1 d PD B 4 F3A F 0.7076(11) 0.1205(12) 0.3512(9) 0.218(9) Uani 0.319(7) 1 d PD B 4 F4A F 0.8700(12) 0.1232(11) 0.3193(6) 0.168(9) Uani 0.319(7) 1 d PD B 4 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 Ni 0.03861(13) 0.03828(13) 0.04065(13) 0.00236(9) 0.00954(9) 0.00390(9) S12 0.0416(2) 0.0475(3) 0.0612(3) 0.0039(2) -0.0027(2) -0.00394(19) S13 0.0551(3) 0.0472(3) 0.0479(3) -0.0052(2) 0.0188(2) -0.0004(2) S11 0.0521(3) 0.0562(3) 0.0383(2) 0.0035(2) 0.00806(19) 0.0120(2) O23 0.0588(8) 0.0407(7) 0.0501(7) -0.0025(6) 0.0208(6) -0.0019(6) N11 0.0403(8) 0.0556(9) 0.0418(8) -0.0013(7) 0.0110(6) 0.0035(7) O21 0.0427(7) 0.0552(8) 0.0406(7) 0.0060(6) 0.0098(5) 0.0125(6) N22 0.0615(10) 0.0506(9) 0.0488(9) 0.0048(7) 0.0099(8) -0.0111(8) O22 0.0376(6) 0.0418(7) 0.0495(7) 0.0050(5) 0.0054(5) -0.0006(5) N21 0.0419(8) 0.0434(8) 0.0524(9) 0.0069(7) 0.0073(7) 0.0073(6) C23 0.0446(9) 0.0380(9) 0.0419(9) 0.0043(7) 0.0040(7) 0.0021(7) N23 0.0476(9) 0.0604(10) 0.0584(10) 0.0094(8) 0.0196(8) 0.0033(8) N12 0.0419(8) 0.0524(9) 0.0438(8) 0.0038(7) 0.0050(6) 0.0091(7) C22 0.0371(8) 0.0428(9) 0.0339(8) 0.0002(7) 0.0066(6) 0.0030(7) C12 0.0441(9) 0.0390(9) 0.0429(9) -0.0017(7) 0.0107(7) -0.0002(7) C21 0.0356(8) 0.0396(9) 0.0397(8) 0.0008(7) 0.0076(7) -0.0005(6) C11 0.0364(8) 0.0373(8) 0.0425(9) 0.0039(7) 0.0062(7) -0.0015(6) C31 0.0422(10) 0.0607(12) 0.0594(12) -0.0106(10) 0.0140(9) 0.0061(9) N13 0.0577(10) 0.0405(9) 0.0541(10) 0.0049(7) 0.0059(8) -0.0055(7) C13 0.0435(9) 0.0459(10) 0.0416(9) 0.0084(7) 0.0105(7) 0.0050(7) C33 0.0535(12) 0.0547(12) 0.0735(15) 0.0124(11) 0.0063(11) -0.0126(10) C41 0.0591(13) 0.0512(12) 0.0741(15) -0.0011(10) 0.0202(11) 0.0148(10) C42 0.0841(17) 0.0556(13) 0.0577(13) 0.0196(10) 0.0034(12) -0.0041(12) C32 0.0722(15) 0.0506(12) 0.0679(14) 0.0134(10) 0.0001(12) 0.0155(11) C52 0.0362(9) 0.0888(16) 0.0536(12) 0.0019(11) 0.0044(8) 0.0094(10) C61 0.0567(12) 0.0648(14) 0.0649(14) 0.0173(11) -0.0015(10) 0.0154(11) C51 0.0649(14) 0.100(2) 0.0468(12) 0.0123(12) 0.0203(10) 0.0161(13) C43 0.0477(12) 0.0705(15) 0.0850(17) 0.0175(13) 0.0120(11) -0.0086(11) C53 0.0972(18) 0.0413(11) 0.0705(15) -0.0073(10) 0.0175(13) -0.0035(11) C63 0.0670(15) 0.0943(19) 0.0695(15) 0.0035(14) 0.0367(13) 0.0060(14) C62 0.0828(18) 0.0864(19) 0.0801(18) 0.0159(15) 0.0134(14) -0.0377(15) B2 0.0732(19) 0.0694(18) 0.077(2) -0.0030(15) 0.0210(16) -0.0096(15) F7 0.161(5) 0.078(3) 0.122(4) 0.029(3) -0.044(4) -0.065(4) F8 0.079(2) 0.106(3) 0.149(5) -0.019(3) 0.046(3) 0.002(2) F6 0.224(9) 0.256(8) 0.119(4) -0.055(5) 0.114(6) -0.056(7) F5 0.136(5) 0.104(4) 0.263(11) 0.025(5) 0.045(6) 0.071(4) F5A 0.158(7) 0.138(6) 0.175(7) 0.025(5) 0.110(6) 0.013(5) F6A 0.109(6) 0.212(9) 0.201(12) -0.066(8) -0.061(7) -0.030(6) F8A 0.146(6) 0.151(7) 0.148(6) -0.071(5) 0.020(5) 0.072(5) F7A 0.163(7) 0.114(6) 0.092(4) 0.039(3) 0.020(4) -0.048(5) B1 0.081(2) 0.0699(19) 0.085(2) -0.0115(17) 0.0245(18) -0.0241(17) F4 0.116(4) 0.154(4) 0.128(3) 0.061(3) -0.011(3) -0.044(3) F3 0.160(4) 0.149(4) 0.123(4) 0.010(3) -0.026(3) 0.034(3) F2 0.221(7) 0.126(5) 0.233(8) -0.110(5) 0.175(6) -0.097(4) F1 0.102(3) 0.096(3) 0.125(3) -0.046(2) 0.040(2) -0.056(2) F2A 0.223(13) 0.094(7) 0.060(4) 0.014(4) -0.014(6) -0.046(7) F1A 0.146(8) 0.076(5) 0.101(6) -0.020(4) 0.072(5) -0.018(4) F3A 0.196(12) 0.199(14) 0.270(17) 0.152(13) 0.067(11) 0.103(11) F4A 0.177(12) 0.217(14) 0.145(10) -0.110(10) 0.120(10) -0.164(11) _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 Ni O23 2.0322(14) . ? Ni O21 2.0505(13) . ? Ni O22 2.0739(12) . ? Ni S11 2.3839(5) . ? Ni S13 2.4150(5) . ? Ni S12 2.4175(6) . ? S12 C12 1.669(2) . ? S13 C13 1.676(2) . ? S11 C11 1.6753(18) . ? O23 C23 1.241(2) . ? N11 C21 1.317(2) . ? N11 C51 1.458(3) . ? N11 C31 1.458(2) . ? O21 C21 1.246(2) . ? N22 C12 1.313(2) . ? N22 C62 1.463(3) . ? N22 C42 1.466(3) . ? O22 C22 1.241(2) . ? N21 C11 1.308(2) . ? N21 C61 1.456(3) . ? N21 C41 1.476(3) . ? C23 N13 1.318(2) . ? C23 C13 1.520(3) . ? N23 C13 1.316(2) . ? N23 C63 1.466(3) . ? N23 C43 1.475(3) . ? N12 C22 1.321(2) . ? N12 C52 1.461(3) . ? N12 C32 1.462(3) . ? C22 C12 1.511(2) . ? C21 C11 1.515(2) . ? C31 C41 1.486(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? N13 C53 1.455(3) . ? N13 C33 1.464(3) . ? C33 C43 1.491(4) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C32 1.492(4) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? B2 F6A 1.285(7) . ? B2 F5 1.310(8) . ? B2 F7 1.330(6) . ? B2 F6 1.331(7) . ? B2 F8A 1.352(7) . ? B2 F5A 1.369(6) . ? B2 F7A 1.378(8) . ? B2 F8 1.401(6) . ? B1 F4A 1.290(8) . ? B1 F2 1.294(5) . ? B1 F4 1.337(6) . ? B1 F1 1.340(5) . ? B1 F3 1.353(6) . ? B1 F2A 1.354(8) . ? B1 F3A 1.388(10) . ? B1 F1A 1.437(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 O23 Ni O21 85.55(5) . . ? O23 Ni O22 87.88(5) . . ? O21 Ni O22 95.84(5) . . ? O23 Ni S11 93.77(4) . . ? O21 Ni S11 83.01(4) . . ? O22 Ni S11 177.90(4) . . ? O23 Ni S13 82.76(4) . . ? O21 Ni S13 167.55(4) . . ? O22 Ni S13 88.03(4) . . ? S11 Ni S13 93.463(19) . . ? O23 Ni S12 167.91(4) . . ? O21 Ni S12 88.68(4) . . ? O22 Ni S12 82.14(4) . . ? S11 Ni S12 96.07(2) . . ? S13 Ni S12 103.59(2) . . ? C12 S12 Ni 96.31(7) . . ? C13 S13 Ni 96.53(7) . . ? C11 S11 Ni 96.73(6) . . ? C23 O23 Ni 122.10(12) . . ? C21 N11 C51 119.64(17) . . ? C21 N11 C31 122.99(16) . . ? C51 N11 C31 117.08(16) . . ? C21 O21 Ni 120.38(11) . . ? C12 N22 C62 121.9(2) . . ? C12 N22 C42 119.99(17) . . ? C62 N22 C42 117.92(18) . . ? C22 O22 Ni 120.14(11) . . ? C11 N21 C61 121.04(18) . . ? C11 N21 C41 119.35(17) . . ? C61 N21 C41 119.36(17) . . ? O23 C23 N13 122.05(18) . . ? O23 C23 C13 119.14(16) . . ? N13 C23 C13 118.80(17) . . ? C13 N23 C63 121.3(2) . . ? C13 N23 C43 120.38(19) . . ? C63 N23 C43 117.87(19) . . ? C22 N12 C52 120.98(17) . . ? C22 N12 C32 120.91(17) . . ? C52 N12 C32 117.90(17) . . ? O22 C22 N12 122.98(17) . . ? O22 C22 C12 119.57(15) . . ? N12 C22 C12 117.39(16) . . ? N22 C12 C22 117.29(17) . . ? N22 C12 S12 125.88(15) . . ? C22 C12 S12 116.82(13) . . ? O21 C21 N11 122.12(16) . . ? O21 C21 C11 119.80(15) . . ? N11 C21 C11 117.83(15) . . ? N21 C11 C21 118.53(16) . . ? N21 C11 S11 123.77(14) . . ? C21 C11 S11 117.62(13) . . ? N11 C31 C41 111.34(17) . . ? N11 C31 H31A 109.4 . . ? C41 C31 H31A 109.4 . . ? N11 C31 H31B 109.4 . . ? C41 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C23 N13 C53 119.35(18) . . ? C23 N13 C33 121.28(19) . . ? C53 N13 C33 119.01(18) . . ? N23 C13 C23 117.49(18) . . ? N23 C13 S13 124.60(16) . . ? C23 C13 S13 117.91(13) . . ? N13 C33 C43 109.51(19) . . ? N13 C33 H33A 109.8 . . ? C43 C33 H33A 109.8 . . ? N13 C33 H33B 109.8 . . ? C43 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? N21 C41 C31 111.01(17) . . ? N21 C41 H41A 109.4 . . ? C31 C41 H41A 109.4 . . ? N21 C41 H41B 109.4 . . ? C31 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? N22 C42 C32 109.99(18) . . ? N22 C42 H42A 109.7 . . ? C32 C42 H42A 109.7 . . ? N22 C42 H42B 109.7 . . ? C32 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? N12 C32 C42 109.61(18) . . ? N12 C32 H32A 109.7 . . ? C42 C32 H32A 109.7 . . ? N12 C32 H32B 109.7 . . ? C42 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? N12 C52 H52A 109.5 . . ? N12 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N12 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N21 C61 H61A 109.5 . . ? N21 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N21 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N11 C51 H51A 109.5 . . ? N11 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N11 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N23 C43 C33 110.40(18) . . ? N23 C43 H43A 109.6 . . ? C33 C43 H43A 109.6 . . ? N23 C43 H43B 109.6 . . ? C33 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? N13 C53 H53A 109.5 . . ? N13 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N13 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N23 C63 H63A 109.5 . . ? N23 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N23 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N22 C62 H62A 109.5 . . ? N22 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N22 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? F6A B2 F5 127.3(8) . . ? F6A B2 F7 111.7(6) . . ? F5 B2 F7 118.2(6) . . ? F6A B2 F6 66.3(6) . . ? F5 B2 F6 104.5(7) . . ? F7 B2 F6 115.3(5) . . ? F6A B2 F8A 104.7(7) . . ? F5 B2 F8A 116.6(8) . . ? F7 B2 F8A 19.2(6) . . ? F6 B2 F8A 130.3(7) . . ? F6A B2 F5A 111.8(7) . . ? F5 B2 F5A 91.5(6) . . ? F7 B2 F5A 82.0(5) . . ? F6 B2 F5A 49.2(4) . . ? F8A B2 F5A 101.2(6) . . ? F6A B2 F7A 126.3(8) . . ? F5 B2 F7A 18.2(7) . . ? F7 B2 F7A 109.5(6) . . ? F6 B2 F7A 122.1(6) . . ? F8A B2 F7A 102.9(7) . . ? F5A B2 F7A 106.6(5) . . ? F6A B2 F8 39.3(7) . . ? F5 B2 F8 105.7(5) . . ? F7 B2 F8 108.8(5) . . ? F6 B2 F8 102.9(5) . . ? F8A B2 F8 92.0(5) . . ? F5A B2 F8 150.9(6) . . ? F7A B2 F8 95.3(5) . . ? F4A B1 F2 120.1(6) . . ? F4A B1 F4 27.1(9) . . ? F2 B1 F4 107.7(6) . . ? F4A B1 F1 114.2(6) . . ? F2 B1 F1 115.2(4) . . ? F4 B1 F1 104.8(5) . . ? F4A B1 F3 74.9(8) . . ? F2 B1 F3 112.5(5) . . ? F4 B1 F3 101.9(4) . . ? F1 B1 F3 113.3(4) . . ? F4A B1 F2A 117.7(7) . . ? F2 B1 F2A 48.3(5) . . ? F4 B1 F2A 129.9(5) . . ? F1 B1 F2A 125.0(5) . . ? F3 B1 F2A 66.0(6) . . ? F4A B1 F3A 113.8(10) . . ? F2 B1 F3A 48.4(7) . . ? F4 B1 F3A 87.5(6) . . ? F1 B1 F3A 79.5(9) . . ? F3 B1 F3A 160.9(8) . . ? F2A B1 F3A 95.2(8) . . ? F4A B1 F1A 124.3(7) . . ? F2 B1 F1A 115.3(5) . . ? F4 B1 F1A 132.5(5) . . ? F1 B1 F1A 38.4(4) . . ? F3 B1 F1A 80.0(6) . . ? F2A B1 F1A 94.8(6) . . ? F3A B1 F1A 106.0(8) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 31.85 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.342 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.054 #END #BEGIN data_fepip _database_code_depnum_ccdc_archive 'CCDC 771142' #TrackingRef '- Me2pipto_Ni-Fe_ CIF check CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Fe N6 O3 S3 2+, B2 F8 2-' _chemical_formula_sum 'C18 H30 B2 F8 Fe N6 O3 S3' _chemical_formula_weight 704.13 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.40(1) _cell_length_b 10.992(8) _cell_length_c 16.20(1) _cell_angle_alpha 90.00 _cell_angle_beta 129.60(2) _cell_angle_gamma 90.00 _cell_volume 2799(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7904 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 24.99 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13694 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2731 _reflns_number_gt 2037 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 fpr windows' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+8.4745P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2731 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 C11 C 0.5823(2) 0.6554(3) 0.4523(3) 0.0416(8) Uani 1 1 d . . . C12 C 0.5463(3) 0.2182(4) 0.2960(4) 0.0559(11) Uani 1 1 d . . . C31 C 0.5042(3) 0.7411(4) 0.5308(3) 0.0513(10) Uani 1 1 d . . . H31A H 0.4843 0.7369 0.5713 0.062 Uiso 1 1 calc R . . H31B H 0.4900 0.8207 0.4975 0.062 Uiso 1 1 calc R . . C32 C 0.5343(4) 0.0063(5) 0.3081(5) 0.0778(16) Uani 1 1 d . . . C41 C 0.5968(3) 0.7237(4) 0.6028(3) 0.0497(9) Uani 1 1 d . . . H41A H 0.6247 0.7912 0.6527 0.060 Uiso 1 1 calc R . . H41B H 0.6117 0.6494 0.6437 0.060 Uiso 1 1 calc R . . C51 C 0.3774(2) 0.6176(4) 0.4020(4) 0.0549(10) Uani 1 1 d . . . H51A H 0.3543 0.5630 0.3430 0.082 Uiso 1 1 calc R . . H51B H 0.3437 0.6903 0.3768 0.082 Uiso 1 1 calc R . . H51C H 0.3768 0.5791 0.4547 0.082 Uiso 1 1 calc R . . C52 C 0.6692(4) 0.1107(9) 0.4351(5) 0.118(3) Uani 1 1 d . . . H52A H 0.6984 0.1810 0.4379 0.177 Uiso 1 1 calc R A . H52B H 0.6944 0.0385 0.4326 0.177 Uiso 1 1 calc R . . H52C H 0.6735 0.1086 0.4977 0.177 Uiso 1 1 calc R . . C61 C 0.7056(3) 0.7697(5) 0.5839(4) 0.0684(13) Uani 1 1 d . . . H61A H 0.7465 0.7064 0.6077 0.103 Uiso 1 1 calc R . . H61B H 0.7245 0.8210 0.6434 0.103 Uiso 1 1 calc R . . H61C H 0.6995 0.8174 0.5298 0.103 Uiso 1 1 calc R . . C21 C 0.4993(2) 0.6031(3) 0.4129(3) 0.0380(8) Uani 1 1 d . . . N11 N 0.46312(19) 0.6480(3) 0.4491(2) 0.0408(7) Uani 1 1 d . . . N12 N 0.5815(2) 0.1165(4) 0.3413(3) 0.0648(10) Uani 1 1 d . A . N21 N 0.62483(19) 0.7165(3) 0.5403(3) 0.0458(7) Uani 1 1 d . . . O21 O 0.46770(17) 0.5221(2) 0.3458(2) 0.0462(6) Uani 1 1 d . A . F1 F 0.6173(2) -0.1368(3) 0.2045(3) 0.0945(10) Uani 1 1 d . . . F2 F 0.6066(3) -0.0064(3) 0.0900(3) 0.1199(15) Uani 1 1 d . . . F3 F 0.6873(3) 0.0378(4) 0.2612(3) 0.1185(14) Uani 1 1 d . . . F4 F 0.7223(3) -0.1055(4) 0.2022(4) 0.1281(15) Uani 1 1 d . . . S11 S 0.61226(7) 0.63290(13) 0.37964(10) 0.0674(4) Uani 1 1 d . A . S12 S 0.61679(17) 0.3321(2) 0.34990(19) 0.0515(5) Uani 0.50 1 d P A 1 O22 O 0.5657(4) 0.3278(5) 0.3098(5) 0.0485(13) Uani 0.50 1 d P A 2 Fe Fe 0.5000 0.48761(7) 0.2500 0.0473(3) Uani 1 2 d S . . B B 0.6582(4) -0.0528(5) 0.1902(5) 0.0697(15) Uani 1 1 d . . . H32A H 0.508(4) -0.001(5) 0.342(5) 0.080(18) Uiso 1 1 d . . . H32B H 0.568(4) -0.055(6) 0.334(5) 0.10(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0376(18) 0.048(2) 0.0389(18) -0.0001(16) 0.0240(16) -0.0052(15) C12 0.072(3) 0.062(3) 0.057(2) -0.010(2) 0.052(2) -0.013(2) C31 0.057(2) 0.051(2) 0.054(2) -0.0100(19) 0.039(2) -0.0030(18) C32 0.079(4) 0.057(3) 0.081(4) 0.011(3) 0.043(3) 0.010(3) C41 0.056(2) 0.051(2) 0.040(2) -0.0058(17) 0.0294(19) -0.0059(18) C51 0.044(2) 0.063(3) 0.063(3) 0.002(2) 0.036(2) -0.0024(19) C52 0.055(3) 0.202(9) 0.066(4) -0.005(5) 0.024(3) -0.003(4) C61 0.046(2) 0.088(4) 0.061(3) -0.015(2) 0.029(2) -0.023(2) C21 0.0416(18) 0.0398(18) 0.0336(17) 0.0021(14) 0.0245(15) -0.0048(15) N11 0.0406(16) 0.0435(17) 0.0401(16) -0.0003(13) 0.0266(14) -0.0022(13) N12 0.050(2) 0.081(3) 0.059(2) -0.003(2) 0.0329(19) -0.0008(19) N21 0.0397(16) 0.0511(18) 0.0420(17) -0.0029(14) 0.0240(14) -0.0066(14) O21 0.0535(16) 0.0500(15) 0.0388(14) -0.0075(11) 0.0312(13) -0.0128(12) F1 0.084(2) 0.087(2) 0.107(3) 0.0030(19) 0.059(2) -0.0077(17) F2 0.108(3) 0.093(3) 0.079(2) 0.0090(19) 0.022(2) -0.012(2) F3 0.130(3) 0.102(3) 0.091(3) -0.029(2) 0.055(2) -0.027(2) F4 0.105(3) 0.128(3) 0.165(4) 0.016(3) 0.093(3) 0.024(3) S11 0.0552(7) 0.1019(10) 0.0610(7) -0.0230(6) 0.0445(6) -0.0243(6) S12 0.0377(11) 0.0577(13) 0.0470(12) 0.0078(10) 0.0214(10) 0.0011(11) O22 0.036(3) 0.052(4) 0.051(3) -0.002(3) 0.025(3) -0.003(3) Fe 0.0578(5) 0.0510(5) 0.0385(4) 0.000 0.0332(4) 0.000 B 0.052(3) 0.054(3) 0.071(4) 0.000(3) 0.024(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 N21 1.288(5) . ? C11 C21 1.493(5) . ? C11 S11 1.654(4) . ? C12 O22 1.243(7) . ? C12 N12 1.278(6) . ? C12 C12 1.483(9) 2_655 ? C12 S12 1.672(5) . ? C31 N11 1.445(5) . ? C31 C41 1.467(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N12 1.421(7) . ? C32 C32 1.464(13) 2_655 ? C32 H32A 0.99(6) . ? C32 H32B 0.85(7) . ? C41 N21 1.450(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C51 N11 1.432(5) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 N12 1.431(7) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C61 N21 1.439(5) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C21 O21 1.222(4) . ? C21 N11 1.297(5) . ? O21 Fe 2.072(3) . ? F1 B 1.361(7) . ? F2 B 1.351(7) . ? F3 B 1.340(7) . ? F4 B 1.328(7) . ? S11 Fe 2.4646(17) . ? S12 Fe 2.511(3) . ? O22 Fe 2.041(6) . ? Fe O22 2.041(6) 2_655 ? Fe O21 2.072(3) 2_655 ? Fe S11 2.4646(17) 2_655 ? Fe S12 2.511(3) 2_655 ? 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 N21 C11 C21 117.0(3) . . ? N21 C11 S11 124.9(3) . . ? C21 C11 S11 118.1(3) . . ? O22 C12 N12 138.3(5) . . ? O22 C12 C12 103.7(4) . 2_655 ? N12 C12 C12 117.8(3) . 2_655 ? O22 C12 S12 27.3(3) . . ? N12 C12 S12 112.0(4) . . ? C12 C12 S12 130.2(2) 2_655 . ? N11 C31 C41 109.7(3) . . ? N11 C31 H31A 109.7 . . ? C41 C31 H31A 109.7 . . ? N11 C31 H31B 109.7 . . ? C41 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? N12 C32 C32 110.4(4) . 2_655 ? N12 C32 H32A 110(3) . . ? C32 C32 H32A 108(4) 2_655 . ? N12 C32 H32B 111(4) . . ? C32 C32 H32B 116(4) 2_655 . ? H32A C32 H32B 101(5) . . ? N21 C41 C31 109.4(3) . . ? N21 C41 H41A 109.8 . . ? C31 C41 H41A 109.8 . . ? N21 C41 H41B 109.8 . . ? C31 C41 H41B 109.8 . . ? H41A C41 H41B 108.2 . . ? N11 C51 H51A 109.5 . . ? N11 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N11 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N12 C52 H52A 109.5 . . ? N12 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N12 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N21 C61 H61A 109.5 . . ? N21 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N21 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O21 C21 N11 123.3(3) . . ? O21 C21 C11 118.2(3) . . ? N11 C21 C11 118.5(3) . . ? C21 N11 C51 121.6(3) . . ? C21 N11 C31 121.2(3) . . ? C51 N11 C31 116.8(3) . . ? C12 N12 C32 122.1(4) . . ? C12 N12 C52 120.9(6) . . ? C32 N12 C52 116.7(6) . . ? C11 N21 C61 120.5(3) . . ? C11 N21 C41 121.0(3) . . ? C61 N21 C41 118.2(3) . . ? C21 O21 Fe 124.0(2) . . ? C11 S11 Fe 97.99(14) . . ? C12 S12 Fe 91.5(2) . . ? C12 O22 Fe 135.4(5) . . ? O22 Fe O22 61.2(4) 2_655 . ? O22 Fe O21 95.00(18) 2_655 . ? O22 Fe O21 103.19(18) . . ? O22 Fe O21 103.19(18) 2_655 2_655 ? O22 Fe O21 95.00(18) . 2_655 ? O21 Fe O21 158.89(15) . 2_655 ? O22 Fe S11 159.15(18) 2_655 . ? O22 Fe S11 100.44(19) . . ? O21 Fe S11 79.01(9) . . ? O21 Fe S11 87.32(9) 2_655 . ? O22 Fe S11 100.44(19) 2_655 2_655 ? O22 Fe S11 159.15(18) . 2_655 ? O21 Fe S11 87.32(9) . 2_655 ? O21 Fe S11 79.01(9) 2_655 2_655 ? S11 Fe S11 99.22(9) . 2_655 ? O22 Fe S12 16.61(17) 2_655 2_655 ? O22 Fe S12 77.6(2) . 2_655 ? O21 Fe S12 89.04(10) . 2_655 ? O21 Fe S12 105.44(10) 2_655 2_655 ? S11 Fe S12 167.19(6) . 2_655 ? S11 Fe S12 84.69(9) 2_655 2_655 ? O22 Fe S12 77.6(2) 2_655 . ? O22 Fe S12 16.61(17) . . ? O21 Fe S12 105.44(10) . . ? O21 Fe S12 89.04(10) 2_655 . ? S11 Fe S12 84.69(9) . . ? S11 Fe S12 167.19(6) 2_655 . ? S12 Fe S12 94.16(13) 2_655 . ? F4 B F3 110.0(5) . . ? F4 B F2 106.3(6) . . ? F3 B F2 109.3(5) . . ? F4 B F1 109.5(5) . . ? F3 B F1 110.0(6) . . ? F2 B F1 111.6(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.702 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.073