# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ana Gaspar' _publ_contact_author_email ana.b.gaspar@uv.es loop_ _publ_author_name F.M.Lara A.Gaspar D.Aravena E.Ruiz C.Munoz M.Ohba R.Ohtani ; S.Kitagawa ; J.Real data_1@120K _database_code_depnum_ccdc_archive 'CCDC 859774' #TrackingRef '- 1@120K_CC-COM-02-2012-031048.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8.50 H6 Fe N7 Pt S0.50' _chemical_formula_weight 473.17 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 tetragonal _symmetry_space_group_name_H-M P4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' '-y, -x, -z' 'y, x, -z' 'y, -x, z' '-y, x, z' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' _cell_length_a 7.1910(4) _cell_length_b 7.1910(4) _cell_length_c 6.8020(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 351.73(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 12 _cell_measurement_theta_max 25 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 218 _exptl_absorpt_coefficient_mu 11.030 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5574 _exptl_absorpt_correction_T_max 0.8096 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1182 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 32.30 _reflns_number_total 378 _reflns_number_gt 377 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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 DFIX restraint was used for disordered guest thiourea molecule. ; _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^)+(0.0422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 378 _refine_ls_number_parameters 28 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.083 _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 S S 0.0000 0.147(4) 0.5000 0.060(6) Uiso 0.13 4 d SPD . . N3 N 0.0000 0.5000 0.669(3) 0.041(8) Uiso 0.25 4 d SPD . . C3 C 0.0000 0.376(4) 0.5000 0.046(19) Uiso 0.13 4 d SPD . . Pt Pt 0.0000 0.0000 0.0000 0.01085(16) Uani 1 16 d S . . Fe Fe 0.5000 0.5000 0.0000 0.0075(3) Uani 1 16 d S . . N1 N 0.5000 0.5000 0.2938(10) 0.0119(14) Uani 1 8 d S . . N2 N 0.3093(6) 0.3093(6) 0.0000 0.0113(10) Uani 1 4 d S . . C2 C 0.1957(7) 0.1957(7) 0.0000 0.0132(12) Uani 1 4 d S . . C1 C -0.3427(14) 0.5000 0.6044(12) 0.019(2) Uani 0.50 2 d SP . . 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 Pt 0.00689(19) 0.00689(19) 0.0188(2) 0.000 0.000 0.000 Fe 0.0057(5) 0.0057(5) 0.0110(6) 0.000 0.000 0.000 N1 0.012(2) 0.012(2) 0.012(3) 0.000 0.000 0.000 N2 0.0092(16) 0.0092(16) 0.015(2) 0.000 0.000 0.000(2) C2 0.0096(18) 0.0096(18) 0.020(2) 0.000 0.000 0.003(2) C1 0.016(5) 0.029(5) 0.012(3) 0.000 -0.001(3) 0.000 _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 S S 1.49(4) 5_556 ? S S 1.49(4) 13 ? S C3 1.650(10) . ? S S 2.11(5) 9_556 ? N3 C3 1.451(10) . ? N3 C3 1.451(10) 9_566 ? C3 N3 1.451(10) 9_566 ? C3 C3 1.78(5) 9_566 ? Pt C2 1.991(7) 9 ? Pt C2 1.991(7) . ? Pt C2 1.991(7) 11 ? Pt C2 1.991(7) 3 ? Fe N1 1.999(7) 9_665 ? Fe N1 1.999(7) . ? Fe N2 1.939(6) 9_665 ? Fe N2 1.939(6) . ? Fe N2 1.939(6) 11_655 ? Fe N2 1.939(6) 3_565 ? N1 C1 1.326(10) 9_566 ? N1 C1 1.326(10) 5_656 ? N1 C1 1.326(10) 6_566 ? N1 C1 1.326(10) 10_656 ? N2 C2 1.155(10) . ? C1 N1 1.326(10) 9_566 ? C1 C1 1.421(16) 10_556 ? C1 C1 1.599(15) 14 ? C1 C1 1.599(15) 13_465 ? 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 S S S 90.000(1) 5_556 13 ? S S C3 135.000(3) 5_556 . ? S S C3 135.000(4) 13 . ? S S S 45.000(1) 5_556 9_556 ? S S S 45.0 13 9_556 ? C3 S S 180.000(1) . 9_556 ? C3 N3 C3 76(3) . 9_566 ? N3 C3 N3 104(3) . 9_566 ? N3 C3 S 127.8(13) . . ? N3 C3 S 127.8(13) 9_566 . ? N3 C3 C3 52.2(13) . 9_566 ? N3 C3 C3 52.2(13) 9_566 9_566 ? S C3 C3 180.000(4) . 9_566 ? C2 Pt C2 180.0(2) 9 . ? C2 Pt C2 90.0 9 11 ? C2 Pt C2 90.0 . 11 ? C2 Pt C2 90.0 9 3 ? C2 Pt C2 90.0 . 3 ? C2 Pt C2 180.0 11 3 ? N2 Fe N2 180.0 9_665 . ? N2 Fe N2 90.0 9_665 11_655 ? N2 Fe N2 90.0 . 11_655 ? N2 Fe N2 90.0 9_665 3_565 ? N2 Fe N2 90.0 . 3_565 ? N2 Fe N2 180.0 11_655 3_565 ? N2 Fe N1 90.0 9_665 9_665 ? N2 Fe N1 90.0 . 9_665 ? N2 Fe N1 90.0 11_655 9_665 ? N2 Fe N1 90.0 3_565 9_665 ? N2 Fe N1 90.0 9_665 . ? N2 Fe N1 90.0 . . ? N2 Fe N1 90.0 11_655 . ? N2 Fe N1 90.0 3_565 . ? N1 Fe N1 180.000(1) 9_665 . ? C1 N1 C1 74.2(4) 9_566 5_656 ? C1 N1 C1 74.2(4) 9_566 6_566 ? C1 N1 C1 117.1(9) 5_656 6_566 ? C1 N1 C1 117.1(9) 9_566 10_656 ? C1 N1 C1 74.2(4) 5_656 10_656 ? C1 N1 C1 74.2(4) 6_566 10_656 ? C1 N1 Fe 121.5(4) 9_566 . ? C1 N1 Fe 121.5(4) 5_656 . ? C1 N1 Fe 121.5(4) 6_566 . ? C1 N1 Fe 121.5(4) 10_656 . ? C2 N2 Fe 180.0 . . ? N2 C2 Pt 180.0 . . ? N1 C1 C1 121.5(4) 9_566 10_556 ? N1 C1 C1 52.9(2) 9_566 14 ? C1 C1 C1 90.0 10_556 14 ? N1 C1 C1 52.9(2) 9_566 13_465 ? C1 C1 C1 90.000(1) 10_556 13_465 ? C1 C1 C1 90.000(2) 14 13_465 ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 32.30 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 1.223 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.231 data_2@120K _database_code_depnum_ccdc_archive 'CCDC 859775' #TrackingRef '- 2@120K_CC-COM-02-2012-031048.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8.50 H6 Fe N7 Pd S0.50' _chemical_formula_weight 384.48 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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' '-y, -x, -z' 'y, x, -z' 'y, -x, z' '-y, x, z' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' _cell_length_a 7.2070(12) _cell_length_b 7.2070(12) _cell_length_c 6.798(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 353.09(15) _cell_formula_units_Z 1 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 12 _cell_measurement_theta_max 25 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 186 _exptl_absorpt_coefficient_mu 2.366 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9113 _exptl_absorpt_correction_T_max 0.9542 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1652 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 32.25 _reflns_number_total 401 _reflns_number_gt 198 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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 DFIX restraint was used for disordered guest thiourea molecule. ; _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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 401 _refine_ls_number_parameters 29 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.892 _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 Pd Pd 0.0000 0.0000 0.0000 0.0147(6) Uani 1 16 d S . . Fe Fe 0.5000 0.5000 0.0000 0.0123(10) Uani 1 16 d S . . N2 N 0.3093(10) 0.3093(10) 0.0000 0.012(3) Uani 1 4 d S . . C2 C 0.1957(12) 0.1957(12) 0.0000 0.015(3) Uani 1 4 d S . . N1 N 0.5000 0.5000 -0.2958(19) 0.016(3) Uani 1 8 d S . . C1 C 0.5000 0.657(2) -0.400(2) 0.018(3) Uani 0.50 2 d SP . . S S 0.0000 0.139(4) 0.5000 0.070(12) Uiso 0.13 4 d SPD . . C3 C 0.0000 0.368(4) 0.5000 0.03(2) Uiso 0.13 4 d SPD . . N3 N 0.0000 0.5000 0.340(4) 0.067(14) Uiso 0.25 4 d SPD . . 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 Pd 0.0105(6) 0.0105(6) 0.0229(18) 0.000 0.000 0.000 Fe 0.0133(11) 0.0133(11) 0.010(3) 0.000 0.000 0.000 N2 0.013(3) 0.013(3) 0.011(8) 0.000 0.000 0.003(4) C2 0.013(4) 0.013(4) 0.020(11) 0.000 0.000 0.006(5) N1 0.021(4) 0.021(4) 0.006(7) 0.000 0.000 0.000 C1 0.022(8) 0.016(7) 0.016(9) -0.002(6) 0.000 0.000 _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 Pd C2 1.995(12) . ? Pd C2 1.995(12) 9 ? Pd C2 1.995(12) 11 ? Pd C2 1.995(12) 3 ? Fe N2 1.943(10) 9_665 ? Fe N2 1.943(10) . ? Fe N2 1.943(10) 11_655 ? Fe N2 1.943(10) 3_565 ? Fe N1 2.011(13) 9_665 ? Fe N1 2.011(13) . ? N2 C2 1.158(10) . ? N1 C1 1.335(16) 14_665 ? N1 C1 1.335(16) 2_665 ? N1 C1 1.335(16) . ? N1 C1 1.335(16) 13 ? C1 C1 1.36(3) 10_554 ? C1 C1 1.60(2) 14_665 ? C1 C1 1.60(2) 13 ? S S 1.42(4) 5_556 ? S S 1.42(4) 13 ? S C3 1.644(10) . ? S S 2.01(6) 9_556 ? C3 N3 1.447(10) 9_566 ? C3 N3 1.447(10) . ? C3 C3 1.91(6) 9_566 ? N3 C3 1.447(10) 9_566 ? 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 C2 Pd C2 180.0(4) . 9 ? C2 Pd C2 90.0 . 11 ? C2 Pd C2 90.0 9 11 ? C2 Pd C2 90.0 . 3 ? C2 Pd C2 90.0 9 3 ? C2 Pd C2 180.0(4) 11 3 ? N2 Fe N2 180.0 9_665 . ? N2 Fe N2 90.0 9_665 11_655 ? N2 Fe N2 90.0 . 11_655 ? N2 Fe N2 90.0 9_665 3_565 ? N2 Fe N2 90.0 . 3_565 ? N2 Fe N2 180.0 11_655 3_565 ? N2 Fe N1 90.000(1) 9_665 9_665 ? N2 Fe N1 90.000(1) . 9_665 ? N2 Fe N1 90.0 11_655 9_665 ? N2 Fe N1 90.0 3_565 9_665 ? N2 Fe N1 90.000(1) 9_665 . ? N2 Fe N1 90.000(1) . . ? N2 Fe N1 90.0 11_655 . ? N2 Fe N1 90.0 3_565 . ? N1 Fe N1 180.0 9_665 . ? C2 N2 Fe 180.0(6) . . ? N2 C2 Pd 180.0(10) . . ? C1 N1 C1 73.6(8) 14_665 2_665 ? C1 N1 C1 73.6(8) 14_665 . ? C1 N1 C1 115.9(16) 2_665 . ? C1 N1 C1 115.9(16) 14_665 13 ? C1 N1 C1 73.6(8) 2_665 13 ? C1 N1 C1 73.6(8) . 13 ? C1 N1 Fe 122.0(8) 14_665 . ? C1 N1 Fe 122.0(8) 2_665 . ? C1 N1 Fe 122.0(8) . . ? C1 N1 Fe 122.0(8) 13 . ? N1 C1 C1 122.0(8) . 10_554 ? N1 C1 C1 53.2(4) . 14_665 ? C1 C1 C1 90.0 10_554 14_665 ? N1 C1 C1 53.2(4) . 13 ? C1 C1 C1 90.000(2) 10_554 13 ? C1 C1 C1 90.000(3) 14_665 13 ? S S S 90.000(1) 5_556 13 ? S S C3 135.000(3) 5_556 . ? S S C3 135.000(7) 13 . ? S S S 45.000(2) 5_556 9_556 ? S S S 45.000(1) 13 9_556 ? C3 S S 180.000(2) . 9_556 ? N3 C3 N3 98(3) 9_566 . ? N3 C3 S 131.2(17) 9_566 . ? N3 C3 S 131.2(17) . . ? N3 C3 C3 48.8(17) 9_566 9_566 ? N3 C3 C3 48.8(17) . 9_566 ? S C3 C3 180.000(4) . 9_566 ? C3 N3 C3 82(3) 9_566 . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 32.25 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.351 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.242 # Attachment '- 1@250K_CC-COM-02-2012-031048.txt' data_1@250K _database_code_depnum_ccdc_archive 'CCDC 864040' #TrackingRef '- 1@250K_CC-COM-02-2012-031048.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8.50 H6 Fe N7 Pt S0.50' _chemical_formula_weight 473.17 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' '-y, -x, -z' 'y, x, -z' 'y, -x, z' '-y, x, z' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' _cell_length_a 7.4564(3) _cell_length_b 7.4564(3) _cell_length_c 7.2671(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 404.04(6) _cell_formula_units_Z 1 _cell_measurement_temperature 250(1) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 12 _cell_measurement_theta_max 25 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 218 _exptl_absorpt_coefficient_mu 9.602 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5966 _exptl_absorpt_correction_T_max 0.8312 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1233 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 29.91 _reflns_number_total 357 _reflns_number_gt 338 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPZK' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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 DFIX restraint was used for disordered guest thiourea molecule. ; _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^)+(0.0773P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 357 _refine_ls_number_parameters 25 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.022 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 Pt Pt 0.0000 0.0000 0.0000 0.0305(5) Uani 1 16 d S . . Fe Fe 0.5000 0.5000 0.0000 0.0296(10) Uani 1 16 d S . . N1 N 0.5000 0.5000 0.306(3) 0.039(5) Uani 1 8 d S . . N2 N 0.2976(13) 0.2976(13) 0.0000 0.040(3) Uani 1 4 d S . . C1 C -0.349(3) 0.5000 0.597(4) 0.050(6) Uani 0.50 2 d SP . . C2 C 0.1885(13) 0.1885(13) 0.0000 0.029(3) Uani 1 4 d S . . S S 0.0000 0.1471 0.5000 0.14(3) Uiso 0.13 4 d SPD . . N3 N 0.0000 0.5000 0.6688 0.08(3) Uiso 0.25 4 d SPD . . C3 C 0.0000 0.3765 0.5000 0.08(6) Uiso 0.13 4 d SPD . . 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 Pt 0.0137(4) 0.0137(4) 0.0640(10) 0.000 0.000 0.000 Fe 0.0146(11) 0.0146(11) 0.060(3) 0.000 0.000 0.000 N1 0.025(5) 0.025(5) 0.066(13) 0.000 0.000 0.000 N2 0.025(4) 0.025(4) 0.069(9) 0.000 0.000 -0.002(5) C1 0.029(11) 0.043(12) 0.078(16) 0.000 0.002(12) 0.000 C2 0.016(4) 0.016(4) 0.055(9) 0.000 0.000 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C2 1.988(14) 9 ? Pt C2 1.988(14) . ? Pt C2 1.988(14) 11 ? Pt C2 1.988(14) 3 ? Fe N2 2.134(14) . ? Fe N2 2.134(14) 9_665 ? Fe N2 2.134(14) 3_565 ? Fe N2 2.134(14) 11_655 ? Fe N1 2.23(2) . ? Fe N1 2.23(2) 9_665 ? N1 C1 1.32(3) 9_566 ? N1 C1 1.32(3) 5_656 ? N1 C1 1.32(3) 6_566 ? N1 C1 1.32(3) 10_656 ? C1 N1 1.32(3) 9_566 ? C1 C1 1.42(6) 10_556 ? C1 C1 1.59(3) 14 ? C1 C1 1.59(3) 13_465 ? C2 N2 1.15(2) . ? S S 1.5508 5_556 ? S S 1.5508 13 ? S C3 1.7109 . ? S S 2.1932 9_556 ? N3 C3 1.53379(12) . ? N3 C3 1.53379(12) 9_566 ? C3 N3 1.53379(12) 9_566 ? C3 C3 1.8415 9_566 ? 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 C2 Pt C2 180.0(8) 9 . ? C2 Pt C2 90.0 9 11 ? C2 Pt C2 90.0 . 11 ? C2 Pt C2 90.0 9 3 ? C2 Pt C2 90.0 . 3 ? C2 Pt C2 180.000(1) 11 3 ? N2 Fe N2 180.0 . 9_665 ? N2 Fe N2 90.0 . 3_565 ? N2 Fe N2 90.0 9_665 3_565 ? N2 Fe N2 90.0 . 11_655 ? N2 Fe N2 90.0 9_665 11_655 ? N2 Fe N2 180.000(1) 3_565 11_655 ? N2 Fe N1 90.000(1) . . ? N2 Fe N1 90.000(1) 9_665 . ? N2 Fe N1 90.000(1) 3_565 . ? N2 Fe N1 90.000(1) 11_655 . ? N2 Fe N1 90.000(1) . 9_665 ? N2 Fe N1 90.000(1) 9_665 9_665 ? N2 Fe N1 90.000(1) 3_565 9_665 ? N2 Fe N1 90.000(1) 11_655 9_665 ? N1 Fe N1 180.0 . 9_665 ? N2 C2 Pt 179.997(1) . . ? C1 N1 C1 73.8(14) 9_566 5_656 ? C1 N1 C1 73.8(14) 9_566 6_566 ? C1 N1 C1 116(3) 5_656 6_566 ? C1 N1 C1 116(3) 9_566 10_656 ? C1 N1 C1 73.8(14) 5_656 10_656 ? C1 N1 C1 73.8(14) 6_566 10_656 ? C1 N1 Fe 121.9(15) 9_566 . ? C1 N1 Fe 121.9(15) 5_656 . ? C1 N1 Fe 121.9(15) 6_566 . ? C1 N1 Fe 121.9(15) 10_656 . ? N1 C1 C1 121.9(15) 9_566 10_556 ? N1 C1 C1 53.1(7) 9_566 14 ? C1 C1 C1 90.000(1) 10_556 14 ? N1 C1 C1 53.1(7) 9_566 13_465 ? C1 C1 C1 90.000(1) 10_556 13_465 ? C1 C1 C1 90.000(6) 14 13_465 ? C2 N2 Fe 179.999(1) . . ? S S S 90.0 5_556 13 ? S S C3 135.0 5_556 . ? S S C3 135.0 13 . ? S S S 45.0 5_556 9_556 ? S S S 45.0 13 9_556 ? C3 S S 180.0 . 9_556 ? C3 N3 C3 73.784(7) . 9_566 ? N3 C3 N3 106.216(7) . 9_566 ? N3 C3 S 126.892(4) . . ? N3 C3 S 126.892(4) 9_566 . ? N3 C3 C3 53.108(4) . 9_566 ? N3 C3 C3 53.108(4) 9_566 9_566 ? S C3 C3 180.0 . 9_566 ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 29.91 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 1.604 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.246