#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/21/7112179.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7112179 loop_ _publ_author_name 'Y. Maximilian Klein' 'Natasha F. Sciortino' 'Florence Ragon' 'Catherine E. Housecroft' 'Cameron J. Kepert' 'Suzanne M. Neville' _publ_section_title ; Spin crossover intermediate plateau stabilization in a flexible 2-D Hofmann-type coordination polymer ; _journal_coden_Cambridge 182 _journal_name_full Chem.Commun. _journal_page_first 3838 _journal_paper_doi 10.1039/C4CC01079E _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C18 H12 Fe N12 Pd S2, (H2O, C2H6O)' _chemical_formula_sum 'C20 H20 Fe N12 O2 Pd S2' _chemical_formula_weight 685.85 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date '9 November 2005' _audit_creation_method SHELXL-97 _cell_angle_alpha 69.66(3) _cell_angle_beta 90.02(3) _cell_angle_gamma 74.60(3) _cell_formula_units_Z 2 _cell_length_a 7.0850(14) _cell_length_b 13.334(3) _cell_length_c 14.383(3) _cell_measurement_reflns_used 5899 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 0 _cell_measurement_theta_min 0 _cell_volume 1221.8(6) _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.927 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scan in phi' _diffrn_radiation_monochromator silicon _diffrn_radiation_source 'Australian synchrotron MX2' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 22271 _diffrn_reflns_theta_full 31.42 _diffrn_reflns_theta_max 31.42 _diffrn_reflns_theta_min 1.52 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.543 _exptl_absorpt_correction_T_max 0.9268 _exptl_absorpt_correction_T_min 0.8610 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details sadabs _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.799 _refine_diff_density_min -1.906 _refine_diff_density_rms 0.336 _refine_ls_extinction_coef 0.050(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 367 _refine_ls_number_reflns 5819 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.1000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+36.3338P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2702 _refine_ls_wR_factor_ref 0.2738 _reflns_number_gt 5339 _reflns_number_total 5819 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c4cc01079e3.cif _cod_data_source_block 'global_0' _cod_original_cell_volume 1221.9(4) _cod_original_sg_symbol_Hall 'P -1' _cod_original_sg_symbol_H-M P-1 _cod_original_formula_sum 'C20 H20 Fe N12 Pd S2 O2' _cod_database_code 7112179 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Pd1 Pd -0.51864(10) 1.03734(5) 0.73828(4) 0.0138(3) Uani 1 1 d . . . Fe2 Fe 0.0000 1.0000 0.5000 0.0135(4) Uani 1 2 d S . . C2 C -0.3212(14) 1.0392(8) 0.8362(7) 0.0193(17) Uani 1 1 d . . . N4 N -0.8182(12) 1.0190(6) 0.5881(6) 0.0175(14) Uani 1 1 d . . . N2 N -0.2080(12) 1.0324(7) 0.8965(6) 0.0184(14) Uani 1 1 d . . . C4 C -0.7133(14) 1.0285(7) 0.6433(7) 0.0185(16) Uani 1 1 d . . . C3 C -0.3156(14) 1.0285(7) 0.6434(7) 0.0185(17) Uani 1 1 d . . . N3 N -0.2010(12) 1.0190(6) 0.5887(6) 0.0167(14) Uani 1 1 d . . . Fe1 Fe 0.0000 1.0000 1.0000 0.0141(4) Uani 1 2 d S . . N5 N -0.0786(13) 1.1573(7) 0.9887(7) 0.0256(17) Uani 1 1 d . . . N9 N -0.0812(13) 1.1618(7) 0.4250(7) 0.0227(16) Uani 1 1 d . . . C1 C -0.7164(14) 1.0393(8) 0.8361(7) 0.0183(16) Uani 1 1 d . . . N10 N -0.1185(18) 1.2368(8) 0.4738(9) 0.041(3) Uani 1 1 d . . . C14 C -0.2558(17) 1.5108(9) 0.2167(8) 0.028(2) Uani 1 1 d . B . H14 H -0.2622 1.5203 0.2792 0.034 Uiso 1 1 calc R . . N11 N -0.1646(15) 1.3288(7) 0.3154(7) 0.0282(19) Uani 1 1 d . . . C13 C -0.169(2) 1.3370(9) 0.4056(8) 0.034(3) Uani 1 1 d . . . H13 H -0.2031 1.4047 0.4181 0.041 Uiso 1 1 calc R . . C5 C -0.1198(18) 1.2430(10) 0.9095(11) 0.036(3) Uani 1 1 d . . . H5 H -0.1179 1.2415 0.8439 0.043 Uiso 1 1 calc R . . C12 C -0.1105(18) 1.2201(8) 0.3300(7) 0.028(2) Uani 1 1 d . . . H12 H -0.0955 1.1900 0.2786 0.033 Uiso 1 1 calc R . . N12 N -0.206(2) 1.4114(8) 0.2172(7) 0.045(3) Uani 1 1 d . B . N7 N -0.167(2) 1.3366(9) 0.9313(10) 0.059(4) Uani 1 1 d . . . N6 N -0.100(3) 1.1949(10) 1.0703(9) 0.059(4) Uani 1 1 d . . . N1 N -0.8245(12) 1.0323(6) 0.8965(6) 0.0185(15) Uani 1 1 d . . . C16 C -0.3604(19) 1.7172(9) 0.1258(8) 0.032(2) Uani 1 1 d . B . H16 H -0.3738 1.7368 0.1834 0.039 Uiso 1 1 calc R . . C15 C -0.3024(18) 1.6089(8) 0.1286(8) 0.030(2) Uani 1 1 d . . . C17 C -0.3974(17) 1.7952(8) 0.0279(8) 0.027(2) Uani 1 1 d . . . H17 H -0.3994 1.8711 0.0096 0.032 Uiso 1 1 calc R A 1 C7 C -0.2371(17) 1.4735(8) 0.7831(9) 0.029(2) Uani 1 1 d . . . H7 H -0.2086 1.4136 0.7592 0.034 Uiso 1 1 calc R . . C18A C -0.316(3) 1.7463(17) -0.0369(16) 0.026(4) Uiso 0.50 1 d PU B 2 H18A H -0.3071 1.7873 -0.1047 0.032 Uiso 0.50 1 calc PR B 2 N8 N -0.223(3) 1.4511(10) 0.8690(10) 0.087(7) Uani 1 1 d . . . C8 C -0.2944(16) 1.5854(9) 0.7101(8) 0.027(2) Uani 1 1 d . . . C9 C -0.308(5) 1.6131(13) 0.6146(11) 0.117(12) Uani 1 1 d . . . H9 H -0.2804 1.5592 0.5836 0.140 Uiso 1 1 calc R . . C6 C -0.151(5) 1.2984(14) 1.0343(14) 0.101(10) Uani 1 1 d . . . H6 H -0.1753 1.3452 1.0725 0.122 Uiso 1 1 calc R . . C11 C -0.3922(19) 1.7865(10) 0.6137(8) 0.032(2) Uani 1 1 d . . . H11 H -0.4037 1.8640 0.5916 0.038 Uiso 1 1 calc R C 1 C10 C -0.364(3) 1.7270(11) 0.5598(10) 0.064(5) Uani 1 1 d . . . H10 H -0.3795 1.7573 0.4890 0.077 Uiso 1 1 calc R . . S2B S -0.3742(12) 1.6069(4) 0.0142(4) 0.0330(13) Uani 0.50 1 d PU B 1 S2A S -0.2334(12) 1.6068(4) 0.0145(4) 0.0333(13) Uani 0.50 1 d PU B 2 C18B C -0.431(4) 1.7457(18) -0.0378(17) 0.028(4) Uiso 0.50 1 d PU B 1 H18B H -0.4804 1.7864 -0.1057 0.034 Uiso 0.50 1 calc PR B 1 O1 O -0.1187(18) 1.2373(8) 0.6687(7) 0.049(3) Uani 1 1 d . . . O2A O -0.497(2) 1.5916(10) 0.4044(11) 0.025(3) Uani 0.50 1 d P . . O2B O -0.096(2) 1.5919(10) 0.4049(11) 0.023(3) Uani 0.50 1 d P . . Pd1A Pd -0.481(4) 0.962(2) 0.6154(19) 0.100 Uiso 0.10 1 d P . 4 Fe2A Fe -0.002(7) 1.003(4) 0.648(4) 0.100 Uiso 0.10 1 d P . 4 Fe1A Fe 0.001(7) 1.002(4) 0.848(3) 0.100 Uiso 0.10 1 d P . 4 Pd1B Pd -0.479(4) 0.960(2) 0.9147(19) 0.100 Uiso 0.10 1 d P . 4 S1B S -0.2955(13) 1.7016(5) 0.7352(5) 0.0331(13) Uani 0.50 1 d P . 2 S1A S -0.4066(13) 1.7015(5) 0.7351(5) 0.0325(13) Uani 0.50 1 d P . 1 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 Pd1 0.0169(4) 0.0192(4) 0.0066(3) -0.0060(2) 0.0000(2) -0.0054(2) Fe2 0.0178(9) 0.0172(9) 0.0060(7) -0.0049(6) -0.0003(6) -0.0049(6) C2 0.019(5) 0.022(4) 0.017(4) -0.005(3) 0.007(3) -0.009(3) N4 0.020(4) 0.014(3) 0.017(3) -0.005(3) -0.002(3) -0.003(3) N2 0.018(4) 0.024(4) 0.016(3) -0.010(3) 0.002(3) -0.008(3) C4 0.014(4) 0.020(4) 0.022(4) -0.008(3) 0.007(3) -0.003(3) C3 0.020(5) 0.020(4) 0.016(4) -0.007(3) -0.002(3) -0.008(3) N3 0.019(4) 0.016(3) 0.015(3) -0.007(3) -0.001(3) -0.004(3) Fe1 0.0183(9) 0.0176(9) 0.0067(7) -0.0049(6) -0.0002(6) -0.0049(6) N5 0.023(5) 0.025(4) 0.029(4) -0.009(3) 0.003(3) -0.007(3) N9 0.020(4) 0.022(4) 0.027(4) -0.009(3) 0.002(3) -0.007(3) C1 0.017(4) 0.024(4) 0.016(4) -0.009(3) -0.002(3) -0.006(3) N10 0.051(7) 0.011(4) 0.053(7) -0.008(4) 0.002(5) -0.001(4) C14 0.033(6) 0.026(5) 0.025(5) -0.008(4) 0.005(4) -0.009(4) N11 0.039(6) 0.021(4) 0.022(4) -0.005(3) 0.002(4) -0.008(3) C13 0.061(8) 0.020(5) 0.019(5) -0.008(4) 0.005(5) -0.007(4) C5 0.026(6) 0.030(6) 0.050(7) -0.011(5) 0.006(5) -0.010(4) C12 0.045(7) 0.017(4) 0.012(4) 0.004(3) -0.001(4) -0.004(4) N12 0.093(10) 0.016(4) 0.017(4) -0.002(3) 0.002(5) -0.004(5) N7 0.096(11) 0.020(5) 0.045(7) 0.000(5) 0.001(7) -0.004(6) N6 0.108(12) 0.034(6) 0.028(6) -0.009(5) 0.002(6) -0.010(6) N1 0.017(4) 0.023(4) 0.017(3) -0.008(3) -0.001(3) -0.006(3) C16 0.052(7) 0.030(6) 0.017(5) -0.012(4) 0.004(4) -0.008(5) C15 0.044(7) 0.017(5) 0.022(5) -0.001(4) -0.003(4) -0.006(4) C17 0.038(6) 0.016(4) 0.026(5) -0.010(4) -0.003(4) -0.004(4) C7 0.033(6) 0.015(4) 0.034(6) -0.006(4) 0.002(4) -0.004(4) N8 0.19(2) 0.018(6) 0.034(7) -0.005(5) 0.005(9) -0.006(8) C8 0.027(6) 0.023(5) 0.027(5) -0.005(4) 0.001(4) -0.008(4) C9 0.29(4) 0.025(7) 0.018(7) -0.012(6) 0.000(12) -0.008(12) C6 0.22(3) 0.026(7) 0.049(10) -0.028(7) 0.003(13) -0.007(11) C11 0.044(7) 0.030(5) 0.021(5) -0.010(4) 0.002(4) -0.009(4) C10 0.143(17) 0.028(6) 0.020(6) -0.018(5) 0.003(7) -0.010(8) S2B 0.055(4) 0.022(3) 0.022(3) -0.0091(19) 0.000(2) -0.009(2) S2A 0.055(4) 0.021(2) 0.022(2) -0.0084(19) 0.003(2) -0.007(2) O1 0.077(8) 0.042(5) 0.029(5) -0.017(4) 0.004(4) -0.011(5) O2A 0.034(8) 0.005(5) 0.038(8) -0.009(5) 0.028(6) -0.008(5) O2B 0.028(7) 0.004(5) 0.032(7) -0.007(5) -0.020(6) 0.003(4) S1B 0.044(4) 0.029(3) 0.029(3) -0.014(2) 0.000(3) -0.008(3) S1A 0.040(4) 0.028(3) 0.030(3) -0.013(2) 0.005(3) -0.007(2) 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 Pd1 C3 177.6(4) . . C1 Pd1 C4 90.4(4) . . C3 Pd1 C4 89.9(4) . . C1 Pd1 C2 89.3(4) . . C3 Pd1 C2 90.3(4) . . C4 Pd1 C2 177.6(4) . . C1 Pd1 Pd1A 131.3(7) . . C3 Pd1 Pd1A 48.0(7) . . C4 Pd1 Pd1A 47.9(7) . . C2 Pd1 Pd1A 131.1(7) . . C1 Pd1 Pd1B 49.5(7) . . C3 Pd1 Pd1B 128.8(7) . . C4 Pd1 Pd1B 129.1(7) . . C2 Pd1 Pd1B 49.3(7) . . Pd1A Pd1 Pd1B 133.8(8) . . N4 Fe2 N4 179.998(2) 2_476 1_655 N4 Fe2 N3 91.0(3) 2_476 . N4 Fe2 N3 89.0(3) 1_655 . N4 Fe2 N3 89.0(3) 2_476 2_576 N4 Fe2 N3 91.0(3) 1_655 2_576 N3 Fe2 N3 179.999(2) . 2_576 N4 Fe2 N9 89.9(3) 2_476 . N4 Fe2 N9 90.1(3) 1_655 . N3 Fe2 N9 90.0(3) . . N3 Fe2 N9 90.0(3) 2_576 . N4 Fe2 N9 90.1(3) 2_476 2_576 N4 Fe2 N9 89.9(3) 1_655 2_576 N3 Fe2 N9 90.0(3) . 2_576 N3 Fe2 N9 90.0(3) 2_576 2_576 N9 Fe2 N9 179.999(3) . 2_576 N4 Fe2 Fe2A 45.3(13) 2_476 2_576 N4 Fe2 Fe2A 134.7(13) 1_655 2_576 N3 Fe2 Fe2A 135.0(13) . 2_576 N3 Fe2 Fe2A 45.0(13) 2_576 2_576 N9 Fe2 Fe2A 81.3(12) . 2_576 N9 Fe2 Fe2A 98.7(12) 2_576 2_576 N4 Fe2 Fe2A 134.7(13) 2_476 . N4 Fe2 Fe2A 45.3(13) 1_655 . N3 Fe2 Fe2A 45.0(12) . . N3 Fe2 Fe2A 135.0(13) 2_576 . N9 Fe2 Fe2A 98.7(12) . . N9 Fe2 Fe2A 81.3(12) 2_576 . Fe2A Fe2 Fe2A 180(2) 2_576 . N2 C2 Pd1B 100.2(11) . . N2 C2 Pd1 175.0(8) . . Pd1B C2 Pd1 75.8(9) . . N2 C2 Fe1A 47.3(14) . . Pd1B C2 Fe1A 129.4(15) . . Pd1 C2 Fe1A 133.3(13) . . C4 N4 Fe2A 103.2(19) . 1_455 C4 N4 Fe2 177.6(8) . 1_455 Fe2A N4 Fe2 74.6(17) 1_455 1_455 C4 N4 Pd1A 49.1(9) . . Fe2A N4 Pd1A 138.8(18) 1_455 . Fe2 N4 Pd1A 132.2(8) 1_455 . C2 N2 Fe1A 102.1(18) . . C2 N2 Fe1 172.1(8) . . Fe1A N2 Fe1 74.0(16) . . C2 N2 Pd1B 51.1(8) . . Fe1A N2 Pd1B 132.4(17) . . Fe1 N2 Pd1B 126.6(7) . . N4 C4 Pd1A 101.6(11) . . N4 C4 Pd1 176.5(8) . . Pd1A C4 Pd1 75.2(9) . . N4 C4 Fe2A 45.6(14) . 1_455 Pd1A C4 Fe2A 135.6(15) . 1_455 Pd1 C4 Fe2A 136.3(13) . 1_455 N3 C3 Pd1A 101.8(11) . . N3 C3 Pd1 176.7(8) . . Pd1A C3 Pd1 75.2(9) . . N3 C3 Fe2A 45.2(14) . . Pd1A C3 Fe2A 135.6(15) . . Pd1 C3 Fe2A 136.3(13) . . C3 N3 Fe2A 103.7(19) . . C3 N3 Fe2 178.0(8) . . Fe2A N3 Fe2 74.5(18) . . C3 N3 Pd1A 49.0(8) . . Fe2A N3 Pd1A 139.1(18) . . Fe2 N3 Pd1A 132.0(7) . . N2 Fe1 N2 179.999(3) 2_577 . N2 Fe1 N1 88.5(3) 2_577 2_477 N2 Fe1 N1 91.5(3) . 2_477 N2 Fe1 N1 91.5(3) 2_577 1_655 N2 Fe1 N1 88.5(3) . 1_655 N1 Fe1 N1 180.0(4) 2_477 1_655 N2 Fe1 N5 89.6(4) 2_577 . N2 Fe1 N5 90.4(3) . . N1 Fe1 N5 89.6(4) 2_477 . N1 Fe1 N5 90.4(4) 1_655 . N2 Fe1 N5 90.4(3) 2_577 2_577 N2 Fe1 N5 89.6(4) . 2_577 N1 Fe1 N5 90.4(4) 2_477 2_577 N1 Fe1 N5 89.6(4) 1_655 2_577 N5 Fe1 N5 180.0(5) . 2_577 N2 Fe1 Fe1A 133.2(12) 2_577 . N2 Fe1 Fe1A 46.8(12) . . N1 Fe1 Fe1A 134.0(12) 2_477 . N1 Fe1 Fe1A 46.0(12) 1_655 . N5 Fe1 Fe1A 106.2(12) . . N5 Fe1 Fe1A 73.8(12) 2_577 . N2 Fe1 Fe1A 46.8(12) 2_577 2_577 N2 Fe1 Fe1A 133.2(12) . 2_577 N1 Fe1 Fe1A 46.0(12) 2_477 2_577 N1 Fe1 Fe1A 134.0(13) 1_655 2_577 N5 Fe1 Fe1A 73.8(12) . 2_577 N5 Fe1 Fe1A 106.2(12) 2_577 2_577 Fe1A Fe1 Fe1A 179.999(18) . 2_577 C5 N5 N6 107.4(10) . . C5 N5 Fe1 127.4(9) . . N6 N5 Fe1 125.2(7) . . C12 N9 N10 106.8(9) . . C12 N9 Fe2 132.2(7) . . N10 N9 Fe2 121.0(7) . . N1 C1 Pd1B 100.6(11) . . N1 C1 Pd1 175.0(8) . . Pd1B C1 Pd1 75.9(9) . . N1 C1 Fe1A 46.7(14) . 1_455 Pd1B C1 Fe1A 129.3(15) . 1_455 Pd1 C1 Fe1A 133.1(13) . 1_455 C13 N10 N9 107.4(11) . . N12 C14 C15 124.5(11) . . N12 C14 H14 117.7 . . C15 C14 H14 117.7 . . C12 N11 C13 106.9(9) . . C12 N11 N12 121.2(9) . . C13 N11 N12 131.9(9) . . N10 C13 N11 109.0(10) . . N10 C13 H13 125.5 . . N11 C13 H13 125.5 . . N5 C5 N7 110.5(13) . . N5 C5 H5 124.7 . . N7 C5 H5 124.7 . . N9 C12 N11 109.8(9) . . N9 C12 H12 125.1 . . N11 C12 H12 125.1 . . C14 N12 N11 113.1(10) . . C5 N7 C6 104.3(11) . . C5 N7 N8 131.5(14) . . C6 N7 N8 124.2(13) . . C6 N6 N5 106.8(12) . . C6 N6 Fe1A 175.3(17) . 2_577 N5 N6 Fe1A 77.9(13) . 2_577 C1 N1 Fe1A 102.1(18) . 1_455 C1 N1 Fe1 172.5(8) . 1_455 Fe1A N1 Fe1 74.5(17) 1_455 1_455 C1 N1 Pd1B 50.7(8) . . Fe1A N1 Pd1B 132.1(17) 1_455 . Fe1 N1 Pd1B 126.7(7) 1_455 . C15 C16 C17 112.2(9) . . C15 C16 H16 123.9 . . C17 C16 H16 123.9 . . C16 C15 C14 125.8(11) . . C16 C15 S2A 109.9(8) . . C14 C15 S2A 122.5(9) . . C16 C15 S2B 109.0(8) . . C14 C15 S2B 121.8(8) . . S2A C15 S2B 33.6(4) . . C18A C17 C18B 34.6(12) . . C18A C17 C16 110.6(12) . . C18B C17 C16 110.3(12) . . C18A C17 Pd1B 93.0(13) . 1_564 C18B C17 Pd1B 93.1(13) . 1_564 C16 C17 Pd1B 155.4(10) . 1_564 C18A C17 H17 114.4 . . C18B C17 H17 124.9 . . C16 C17 H17 124.9 . . Pd1B C17 H17 32.6 1_564 . N8 C7 C8 125.1(11) . . N8 C7 H7 117.5 . . C8 C7 H7 117.5 . . C17 C18A S2A 113.5(15) . . C17 C18A H18A 123.3 . . S2A C18A H18A 123.3 . . C7 N8 N7 118.3(13) . . C9 C8 C7 126.6(12) . . C9 C8 S1A 107.5(10) . . C7 C8 S1A 124.6(9) . . C9 C8 S1B 107.3(10) . . C7 C8 S1B 124.2(9) . . S1A C8 S1B 26.7(3) . . C8 C9 C10 115.8(13) . . C8 C9 H9 122.1 . . C10 C9 H9 122.1 . . N6 C6 N7 111.0(13) . . N6 C6 H6 124.5 . . N7 C6 H6 124.5 . . C10 C11 S1B 108.5(10) . . C10 C11 S1A 108.2(10) . . S1B C11 S1A 26.2(3) . . C10 C11 Pd1A 145.9(12) . 1_565 S1B C11 Pd1A 104.9(9) . 1_565 S1A C11 Pd1A 104.8(9) . 1_565 C10 C11 H11 125.9 . . S1B C11 H11 119.7 . . S1A C11 H11 125.9 . . Pd1A C11 H11 22.5 1_565 . C11 C10 C9 113.4(13) . . C11 C10 H10 123.3 . . C9 C10 H10 123.3 . . C18B S2B C15 91.7(9) . . C18A S2A C15 91.3(9) . . C17 C18B S2B 113.0(15) . . C17 C18B H18B 123.5 . . S2B C18B H18B 123.5 . . C4 Pd1A C3 105.5(14) . . C4 Pd1A C11 124.9(14) . 1_545 C3 Pd1A C11 124.4(14) . 1_545 C4 Pd1A N4 29.4(6) . . C3 Pd1A N4 130.2(13) . . C11 Pd1A N4 105.2(11) 1_545 . C4 Pd1A N3 130.1(13) . . C3 Pd1A N3 29.2(6) . . C11 Pd1A N3 104.7(11) 1_545 . N4 Pd1A N3 144.6(12) . . C4 Pd1A Pd1 56.8(8) . . C3 Pd1A Pd1 56.8(8) . . C11 Pd1A Pd1 134.9(12) 1_545 . N4 Pd1A Pd1 86.2(9) . . N3 Pd1A Pd1 85.9(9) . . C4 Pd1A Pd1A 104.6(14) . 2_476 C3 Pd1A Pd1A 104.4(14) . 2_476 C11 Pd1A Pd1A 85.5(11) 1_545 2_476 N4 Pd1A Pd1A 82.0(11) . 2_476 N3 Pd1A Pd1A 82.0(11) . 2_476 Pd1 Pd1A Pd1A 139.7(14) . 2_476 N3 Fe2A N4 118(3) . 1_655 N3 Fe2A Fe2 60.5(16) . . N4 Fe2A Fe2 60.1(16) 1_655 . N3 Fe2A C3 31.1(10) . . N4 Fe2A C3 147(3) 1_655 . Fe2 Fe2A C3 91.5(18) . . N3 Fe2A C4 148(3) . 1_655 N4 Fe2A C4 31.2(10) 1_655 1_655 Fe2 Fe2A C4 91.3(18) . 1_655 C3 Fe2A C4 163(2) . 1_655 N3 Fe2A Fe1A 120(3) . . N4 Fe2A Fe1A 120(3) 1_655 . Fe2 Fe2A Fe1A 179(2) . . C3 Fe2A Fe1A 89.1(19) . . C4 Fe2A Fe1A 88.5(18) 1_655 . N1 Fe1A N2 112(3) 1_655 . N1 Fe1A C1 31.1(9) 1_655 1_655 N2 Fe1A C1 140(3) . 1_655 N1 Fe1A Fe1 59.5(15) 1_655 . N2 Fe1A Fe1 59.2(15) . . C1 Fe1A Fe1 90.4(17) 1_655 . N1 Fe1A C2 140(3) 1_655 . N2 Fe1A C2 30.6(9) . . C1 Fe1A C2 156(2) 1_655 . Fe1 Fe1A C2 89.6(18) . . N1 Fe1A N6 99(2) 1_655 2_577 N2 Fe1A N6 100(2) . 2_577 C1 Fe1A N6 101.7(18) 1_655 2_577 Fe1 Fe1A N6 83.0(16) . 2_577 C2 Fe1A N6 101.8(18) . 2_577 N1 Fe1A Fe2A 121(3) 1_655 . N2 Fe1A Fe2A 120(2) . . C1 Fe1A Fe2A 90.4(19) 1_655 . Fe1 Fe1A Fe2A 179(2) . . C2 Fe1A Fe2A 89.8(18) . . N6 Fe1A Fe2A 96.6(18) 2_577 . C2 Pd1B C1 98.0(12) . . C2 Pd1B C17 129.5(14) . 1_546 C1 Pd1B C17 129.1(14) . 1_546 C2 Pd1B N2 28.7(5) . . C1 Pd1B N2 121.6(13) . . C17 Pd1B N2 109.3(11) 1_546 . C2 Pd1B N1 121.8(12) . . C1 Pd1B N1 28.7(5) . . C17 Pd1B N1 108.7(11) 1_546 . N2 Pd1B N1 136.6(11) . . C2 Pd1B Pd1 54.8(7) . . C1 Pd1B Pd1 54.5(7) . . C17 Pd1B Pd1 136.6(12) 1_546 . N2 Pd1B Pd1 83.5(9) . . N1 Pd1B Pd1 83.2(8) . . C2 Pd1B Pd1B 103.3(14) . 2_477 C1 Pd1B Pd1B 102.7(14) . 2_477 C17 Pd1B Pd1B 85.1(12) 1_546 2_477 N2 Pd1B Pd1B 81.8(11) . 2_477 N1 Pd1B Pd1B 81.2(11) . 2_477 Pd1 Pd1B Pd1B 138.3(14) . 2_477 C8 S1B C11 90.9(6) . . C8 S1A C11 91.0(6) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pd1 C1 1.988(10) . Pd1 C3 1.992(10) . Pd1 C4 1.995(10) . Pd1 C2 1.996(10) . Pd1 Pd1A 2.30(3) . Pd1 Pd1B 2.37(3) . Fe2 N4 1.930(8) 2_476 Fe2 N4 1.930(8) 1_655 Fe2 N3 1.937(8) . Fe2 N3 1.937(8) 2_576 Fe2 N9 1.967(8) . Fe2 N9 1.967(8) 2_576 Fe2 Fe2A 2.15(5) 2_576 Fe2 Fe2A 2.15(5) . C2 N2 1.144(13) . C2 Pd1B 1.85(3) . C2 Fe1A 2.20(5) . N4 C4 1.148(13) . N4 Fe2A 1.58(5) 1_455 N4 Fe2 1.930(8) 1_455 N4 Pd1A 2.29(3) . N2 Fe1A 1.65(5) . N2 Fe1 1.946(8) . N2 Pd1B 2.34(3) . C4 Pd1A 1.77(3) . C4 Fe2A 2.16(5) 1_455 C3 N3 1.144(13) . C3 Pd1A 1.77(3) . C3 Fe2A 2.16(5) . N3 Fe2A 1.58(5) . N3 Pd1A 2.30(3) . Fe1 N2 1.946(8) 2_577 Fe1 N1 1.947(9) 2_477 Fe1 N1 1.947(9) 1_655 Fe1 N5 1.969(9) . Fe1 N5 1.969(9) 2_577 Fe1 Fe1A 2.18(5) . Fe1 Fe1A 2.18(5) 2_577 N5 C5 1.268(16) . N5 N6 1.420(15) . N9 C12 1.301(12) . N9 N10 1.382(13) . C1 N1 1.153(13) . C1 Pd1B 1.86(3) . C1 Fe1A 2.18(5) 1_455 N10 C13 1.307(14) . C14 N12 1.274(15) . C14 C15 1.430(14) . C14 H14 0.9500 . N11 C12 1.336(13) . N11 C13 1.339(14) . N11 N12 1.428(12) . C13 H13 0.9500 . C5 N7 1.348(18) . C5 H5 0.9500 . C12 H12 0.9500 . N7 C6 1.38(2) . N7 N8 1.420(16) . N6 C6 1.24(2) . N6 Fe1A 2.37(5) 2_577 N1 Fe1A 1.63(5) 1_455 N1 Fe1 1.947(8) 1_455 N1 Pd1B 2.36(3) . C16 C15 1.379(15) . C16 C17 1.403(15) . C16 H16 0.9500 . C15 S2A 1.720(13) . C15 S2B 1.733(12) . C17 C18A 1.36(2) . C17 C18B 1.38(2) . C17 Pd1B 2.16(3) 1_564 C17 H17 0.9500 . C7 N8 1.163(18) . C7 C8 1.443(14) . C7 H7 0.9500 . C18A S2A 1.68(2) . C18A H18A 0.9500 . C8 C9 1.288(18) . C8 S1A 1.701(12) . C8 S1B 1.707(12) . C9 C10 1.39(2) . C9 H9 0.9500 . C6 H6 0.9500 . C11 C10 1.270(16) . C11 S1B 1.737(13) . C11 S1A 1.741(13) . C11 Pd1A 2.26(3) 1_565 C11 H11 0.9500 . C10 H10 0.9500 . S2B C18B 1.67(2) . C18B H18B 0.9500 . Pd1A C11 2.26(3) 1_545 Pd1A Pd1A 3.10(5) 2_476 Fe2A N4 1.58(5) 1_655 Fe2A C4 2.16(5) 1_655 Fe2A Fe1A 2.87(7) . Fe1A N1 1.63(5) 1_655 Fe1A C1 2.18(5) 1_655 Fe1A N6 2.37(5) 2_577 Pd1B C17 2.16(3) 1_546 Pd1B Pd1B 2.98(5) 2_477