# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Bousseksou, Azzedine' _publ_contact_author_email boussek@lcc-toulouse.fr _publ_section_title ; Enhanced porosity in a new 3D Hofmann-like network exhibiting humidity sensitive cooperative spin transitions at room temperature ; loop_ _publ_author_name L.Salmon A.Bousseksou # Attachment '- ja966-acta50_fin.cif' data_ja966-acta50 _database_code_depnum_ccdc_archive 'CCDC 782177' #TrackingRef '- ja966-acta50_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22.08 Fe N7.04 Pt' _chemical_formula_weight 614.74 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/mmm _space_group_name_Hall -P42 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 7.1700(2) _cell_length_b 7.1700(2) _cell_length_c 13.6620(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 702.35(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.02 _cell_measurement_theta_max 32.19 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 297 _exptl_absorpt_coefficient_mu 5.508 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8097 _exptl_absorpt_correction_T_max 0.9470 _exptl_absorpt_process_details scalepack _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 2634 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 32.19 _reflns_number_total 751 _reflns_number_gt 722 _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, 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 overall quality of all data collected was low due to the problems associated with poor quality crystals and the extensive disorder, which are often intrinsic to clathrate complexes. Such disorder can be expected to be significantly worse in this complex, which presents an exceptionally high degree of porosity. The low quality of the data resulted in significant complications during refinement. As such only the metal atoms were refined using an anisotropic model of the atomic displacement parameters. Hydrogen atoms were not included in the refinement. The solvent within the large pores are heavily disordered and have been modeled as such. There is also disorder observed in the coordinated bridging bpac ligand. However, while these issues reduce the quality of the structural model, none of these issues affect the conclusions drawn within the manuscript as to the atomic connectivity or network topology. ; _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^)+(0.1034P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens notdet _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 751 _refine_ls_number_parameters 31 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.858 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.015 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 0.5000 0.5000 0.5000 0.01266(14) Uani 1 16 d S . . Fe Fe 0.0000 0.0000 0.5000 0.0065(2) Uani 1 16 d S . . N1 N 0.0000 0.0000 0.3539(4) 0.0116(11) Uiso 1 8 d S . . N2 N 0.1908(5) 0.1908(5) 0.5000 0.0121(7) Uiso 1 4 d S . . C1 C 0.1613(13) 0.0000 0.3050(6) 0.0209(15) Uiso 0.50 2 d SP . . C2 C 0.1658(14) 0.0000 0.2011(6) 0.0238(16) Uiso 0.50 2 d SP . . C3 C 0.0000 0.0000 0.1482(6) 0.0206(15) Uiso 1 8 d S . . C4 C 0.0000 0.0000 0.0424(7) 0.0261(17) Uiso 1 8 d S . . C5 C 0.3044(6) 0.3044(6) 0.5000 0.0148(9) Uiso 1 4 d S . . N3 N 0.5000 0.2055 0.1679 0.12(6) Uiso 0.13 2 d SP . . C6 C 0.5000 0.2055 0.1679 0.007(4) Uiso 0.13 2 d SPD . . C7 C 0.5000 0.100(3) 0.2578(14) 0.029(4) Uiso 0.25 2 d SP . . C8 C 0.5000 0.115(4) 0.0768(17) 0.039(5) Uiso 0.25 2 d SP . . C9 C 0.5000 0.4147(14) 0.1692 0.6(4) Uiso 0.13 2 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 0.00490(14) 0.00490(14) 0.0282(2) 0.000 0.000 0.000 Fe 0.0052(3) 0.0052(3) 0.0092(5) 0.000 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 Pt C5 1.983(6) . ? Pt C5 1.983(6) 9_666 ? Pt C5 1.983(6) 11_655 ? Pt C5 1.983(6) 3_566 ? Fe N2 1.935(5) . ? Fe N2 1.935(5) 9_556 ? Fe N2 1.935(5) 11 ? Fe N2 1.935(5) 3_556 ? Fe N1 1.996(6) 9_556 ? Fe N1 1.996(6) . ? N1 C1 1.335(9) 14 ? N1 C1 1.335(9) 2 ? N1 C1 1.335(9) . ? N1 C1 1.335(9) 13 ? N2 C5 1.152(8) . ? C1 C2 1.419(12) . ? C1 C1 1.635(13) 14 ? C1 C1 1.635(13) 13 ? C2 C3 1.391(10) . ? C2 C2 1.681(14) 14 ? C2 C2 1.681(14) 13 ? C3 C2 1.391(10) 13 ? C3 C2 1.391(10) 14 ? C3 C2 1.391(10) 2 ? C3 C4 1.446(13) . ? C4 C4 1.16(2) 9 ? N3 C8 1.40(2) . ? N3 C7 1.44(2) . ? N3 C9 1.500(10) . ? C6 C8 1.40(2) . ? C6 C7 1.44(2) . ? C6 C9 1.500(10) . ? C7 C7 1.43(4) 2_655 ? C8 C8 1.65(6) 2_655 ? C9 C9 0.865(14) 14_665 ? C9 C9 0.865(14) 13 ? C9 C9 1.22(2) 2_665 ? 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 C5 Pt C5 180.0 . 9_666 ? C5 Pt C5 90.0 . 11_655 ? C5 Pt C5 90.0 9_666 11_655 ? C5 Pt C5 90.0 . 3_566 ? C5 Pt C5 90.0 9_666 3_566 ? C5 Pt C5 180.0 11_655 3_566 ? N2 Fe N2 180.00(14) . 9_556 ? N2 Fe N2 90.0 . 11 ? N2 Fe N2 90.0 9_556 11 ? N2 Fe N2 90.0 . 3_556 ? N2 Fe N2 90.0 9_556 3_556 ? N2 Fe N2 180.0 11 3_556 ? N2 Fe N1 90.0 . 9_556 ? N2 Fe N1 90.000(1) 9_556 9_556 ? N2 Fe N1 90.0 11 9_556 ? N2 Fe N1 90.0 3_556 9_556 ? N2 Fe N1 90.0 . . ? N2 Fe N1 90.0 9_556 . ? N2 Fe N1 90.0 11 . ? N2 Fe N1 90.0 3_556 . ? N1 Fe N1 180.0 9_556 . ? C1 N1 C1 75.5(4) 14 2 ? C1 N1 C1 75.5(4) 14 . ? C1 N1 C1 120.0(8) 2 . ? C1 N1 C1 120.0(8) 14 13 ? C1 N1 C1 75.5(4) 2 13 ? C1 N1 C1 75.5(4) . 13 ? C1 N1 Fe 120.0(4) 14 . ? C1 N1 Fe 120.0(4) 2 . ? C1 N1 Fe 120.0(4) . . ? C1 N1 Fe 120.0(4) 13 . ? C5 N2 Fe 180.0 . . ? N1 C1 C2 121.3(8) . . ? N1 C1 C1 52.25(19) . 14 ? C2 C1 C1 90.9(4) . 14 ? N1 C1 C1 52.25(19) . 13 ? C2 C1 C1 90.9(4) . 13 ? C1 C1 C1 90.000(1) 14 13 ? C3 C2 C1 120.0(9) . . ? C3 C2 C2 52.8(2) . 14 ? C1 C2 C2 89.1(4) . 14 ? C3 C2 C2 52.8(2) . 13 ? C1 C2 C2 89.1(4) . 13 ? C2 C2 C2 90.000(1) 14 13 ? C2 C3 C2 74.3(4) 13 . ? C2 C3 C2 117.4(9) 13 14 ? C2 C3 C2 74.3(4) . 14 ? C2 C3 C2 74.3(4) 13 2 ? C2 C3 C2 117.4(9) . 2 ? C2 C3 C2 74.3(4) 14 2 ? C2 C3 C4 121.3(5) 13 . ? C2 C3 C4 121.3(5) . . ? C2 C3 C4 121.3(5) 14 . ? C2 C3 C4 121.3(5) 2 . ? C4 C4 C3 180.0 9 . ? N2 C5 Pt 180.0 . . ? C8 N3 C7 120.9(13) . . ? C8 N3 C9 118.1(11) . . ? C7 N3 C9 121.0(8) . . ? C8 C6 C7 120.9(13) . . ? C8 C6 C9 118.1(11) . . ? C7 C6 C9 121.0(8) . . ? C7 C7 N3 121.7(8) 2_655 . ? C7 C7 C6 121.7(8) 2_655 . ? N3 C7 C6 0.0 . . ? C6 C8 N3 0.0 . . ? C6 C8 C8 117.4(11) . 2_655 ? N3 C8 C8 117.4(11) . 2_655 ? C9 C9 C9 90.0 14_665 13 ? C9 C9 C9 45.000(1) 14_665 2_665 ? C9 C9 C9 45.000(1) 13 2_665 ? C9 C9 N3 134.996(1) 14_665 . ? C9 C9 N3 134.996(2) 13 . ? C9 C9 N3 179.322(5) 2_665 . ? C9 C9 C6 134.996(1) 14_665 . ? C9 C9 C6 134.996(2) 13 . ? C9 C9 C6 179.322(5) 2_665 . ? N3 C9 C6 0.0 . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.671 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.191 # Attachment '- ja963-acta50_fin.cif' data_ja963-acta50 _database_code_depnum_ccdc_archive 'CCDC 782178' #TrackingRef '- ja963-acta50_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 Cl1.56 Fe N6 O0.52 Pt' _chemical_formula_weight 626.80 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' 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' 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 _space_group_name_Hall -P42 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 7.2310(8) _cell_length_b 7.2310(8) _cell_length_c 13.812(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 722.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 32.00 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 299 _exptl_absorpt_coefficient_mu 5.492 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7341 _exptl_absorpt_correction_T_max 0.9471 _exptl_absorpt_process_details scalepack _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 1252 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 32.00 _reflns_number_total 664 _reflns_number_gt 596 _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, 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 overall quality of all data collected was low due to the problems associated with poor quality crystals and the extensive disorder, which are often intrinsic to clathrate complexes. Such disorder can be expected to be significantly worse in this complex, which presents an exceptionally high degree of porosity. The low quality of the data resulted in significant complications during refinement. As such only the metal atoms were refined using an anisotropic model of the atomic displacement parameters. Hydrogen atoms were not included in the refinement. The solvent within the large pores are heavily disordered and have been modeled as such. There is also disorder observed in the coordinated bridging bpac ligand. However, while these issues reduce the quality of the structural model, none of these issues affect the conclusions drawn within the manuscript as to the atomic connectivity or network topology. ; _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^)+(0.1610P)^2^+19.4780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens notdet _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 664 _refine_ls_number_parameters 33 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0902 _refine_ls_wR_factor_ref 0.2481 _refine_ls_wR_factor_gt 0.2335 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.026 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 Pt1 Pt 0.0000 0.0000 0.0000 0.0219(6) Uani 1 16 d S . . Fe1 Fe 0.5000 0.5000 0.0000 0.0122(10) Uani 1 16 d S . . N1 N 0.5000 0.5000 0.1463(19) 0.021(5) Uiso 1 8 d S . . N2 N 0.3084(17) 0.3084(17) 0.0000 0.021(3) Uiso 1 4 d S . . C1 C 0.340(6) 0.5000 0.194(3) 0.045(9) Uiso 0.50 2 d SP . . C2 C 0.336(7) 0.5000 0.300(3) 0.050(10) Uiso 0.50 2 d SP . . C3 C 0.5000 0.5000 0.353(3) 0.039(8) Uiso 1 8 d S . . C4 C 0.5000 0.5000 0.456(3) 0.050(10) Uiso 1 8 d S . . C5 C 0.1974(15) 0.1974(15) 0.0000 0.010(3) Uiso 1 4 d S . . C6 C 0.5000 0.0000 0.401(9) 0.07(4) Uiso 0.25 4 d SPD . . C7 C 0.346(12) 0.0000 0.4475(4) 0.047(18) Uiso 0.25 2 d SPD . . Cl1 Cl 0.112(12) 0.0000 0.419(11) 0.16(8) Uiso 0.13 2 d SPD . . Cl2 Cl 0.5000 0.0000 0.275(9) 0.18(7) Uiso 0.13 4 d SPD . . O O 0.5000 0.0000 0.296(9) 0.2(13) 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 Pt1 0.0108(5) 0.0108(5) 0.0440(12) 0.000 0.000 0.000 Fe1 0.0059(11) 0.0059(11) 0.025(3) 0.000 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 Pt1 C5 2.019(15) . ? Pt1 C5 2.019(15) 9 ? Pt1 C5 2.019(15) 11 ? Pt1 C5 2.019(15) 3 ? Fe1 N2 1.959(17) 9_665 ? Fe1 N2 1.959(17) . ? Fe1 N2 1.959(17) 11_655 ? Fe1 N2 1.959(17) 3_565 ? Fe1 N1 2.02(3) 9_665 ? Fe1 N1 2.02(3) . ? N1 C1 1.33(5) 14_665 ? N1 C1 1.33(5) 2_665 ? N1 C1 1.33(5) . ? N1 C1 1.33(5) 13 ? N2 C5 1.14(2) . ? C1 C2 1.46(6) . ? C1 C1 1.63(6) 14_665 ? C1 C1 1.63(6) 13 ? C2 C3 1.40(5) . ? C2 C2 1.68(7) 14_665 ? C2 C2 1.68(7) 13 ? C3 C2 1.40(5) 13 ? C3 C2 1.40(5) 14_665 ? C3 C2 1.40(5) 2_665 ? C3 C4 1.42(7) . ? C4 C4 1.21(10) 9_666 ? C6 C7 1.28(9) 2_655 ? C6 C7 1.28(9) . ? C6 O 1.448(10) . ? C7 C7 1.452(10) 10_556 ? Cl2 O 0.300(14) . ? 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 C5 Pt1 C5 180.0(4) . 9 ? C5 Pt1 C5 90.0 . 11 ? C5 Pt1 C5 90.0 9 11 ? C5 Pt1 C5 90.0 . 3 ? C5 Pt1 C5 90.0 9 3 ? C5 Pt1 C5 180.0(4) 11 3 ? N2 Fe1 N2 180.000(1) 9_665 . ? N2 Fe1 N2 89.998(1) 9_665 11_655 ? N2 Fe1 N2 90.0 . 11_655 ? N2 Fe1 N2 90.0 9_665 3_565 ? N2 Fe1 N2 89.998(1) . 3_565 ? N2 Fe1 N2 180.0 11_655 3_565 ? N2 Fe1 N1 90.0 9_665 9_665 ? N2 Fe1 N1 90.0 . 9_665 ? N2 Fe1 N1 90.0 11_655 9_665 ? N2 Fe1 N1 90.0 3_565 9_665 ? N2 Fe1 N1 90.0 9_665 . ? N2 Fe1 N1 90.0 . . ? N2 Fe1 N1 90.0 11_655 . ? N2 Fe1 N1 90.0 3_565 . ? N1 Fe1 N1 180.000(1) 9_665 . ? C1 N1 C1 75.8(18) 14_665 2_665 ? C1 N1 C1 75.8(18) 14_665 . ? C1 N1 C1 121(4) 2_665 . ? C1 N1 C1 121(4) 14_665 13 ? C1 N1 C1 75.8(18) 2_665 13 ? C1 N1 C1 75.8(18) . 13 ? C1 N1 Fe1 120(2) 14_665 . ? C1 N1 Fe1 120(2) 2_665 . ? C1 N1 Fe1 120(2) . . ? C1 N1 Fe1 120(2) 13 . ? C5 N2 Fe1 179.989(1) . . ? N1 C1 C2 121(4) . . ? N1 C1 C1 52.1(9) . 14_665 ? C2 C1 C1 90.9(19) . 14_665 ? N1 C1 C1 52.1(9) . 13 ? C2 C1 C1 90.9(19) . 13 ? C1 C1 C1 90.000(12) 14_665 13 ? C3 C2 C1 121(4) . . ? C3 C2 C2 53.2(11) . 14_665 ? C1 C2 C2 89.1(19) . 14_665 ? C3 C2 C2 53.2(11) . 13 ? C1 C2 C2 89.1(19) . 13 ? C2 C2 C2 90.000(14) 14_665 13 ? C2 C3 C2 74(2) . 13 ? C2 C3 C2 74(2) . 14_665 ? C2 C3 C2 116(5) 13 14_665 ? C2 C3 C2 116(5) . 2_665 ? C2 C3 C2 74(2) 13 2_665 ? C2 C3 C2 74(2) 14_665 2_665 ? C2 C3 C4 122(2) . . ? C2 C3 C4 122(2) 13 . ? C2 C3 C4 122(2) 14_665 . ? C2 C3 C4 122(2) 2_665 . ? C4 C4 C3 180.000(13) 9_666 . ? N2 C5 Pt1 179.980(1) . . ? C7 C6 C7 120(10) 2_655 . ? C7 C6 O 120(5) 2_655 . ? C7 C6 O 120(5) . . ? C6 C7 C7 120(5) . 10_556 ? Cl2 O C6 180.00(7) . . ? _diffrn_measured_fraction_theta_max 0.819 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.452 _refine_diff_density_min -2.168 _refine_diff_density_rms 0.534 # Attachment '- 1tol_fin.cif' data_fe-bpac-toluene _database_code_depnum_ccdc_archive 'CCDC 817464' #TrackingRef '- 1tol_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.08 H8 Fe N6 Pt' _chemical_formula_weight 620.24 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/mmm _symmetry_space_group_name_hall -P42 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 7.1760(2) _cell_length_b 7.1760(2) _cell_length_c 13.6663(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 703.75(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 2888 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 33.28 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 5.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3498 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.96 _reflns_number_total 429 _reflns_number_gt 427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _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 overall quality of all data collected was low due to the problems associated with poor quality crystals and the extensive disorder, which are often intrinsic to clathrate complexes. Such disorder can be expected to be significantly worse in this complex, which presents an exceptionally high degree of porosity. The solvent within the large pores are heavily disordered and have been modeled as such. There is also disorder observed in the coordinated bridging bpac ligand. However, while these issues reduce the quality of the structural model, none of these issues affect the conclusions drawn within the manuscript as to the atomic connectivity or network topology. ; _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^)+(0.1213P)^2^+19.9669P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 429 _refine_ls_number_parameters 32 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.182 _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 Pt1 Pt 0.0000 0.0000 0.0000 0.0053(6) Uani 1 16 d S . . Fe1 Fe -0.5000 -0.5000 0.0000 0.0047(12) Uani 1 16 d S . . N1 N -0.5000 -0.5000 -0.1470(18) 0.010(5) Uani 1 8 d S . . N2 N -0.310(2) -0.310(2) 0.0000 0.016(3) Uani 1 4 d S . . C5 C -0.194(2) -0.194(2) 0.0000 0.009(4) Uani 1 4 d S . . C3 C -0.5000 -0.5000 -0.352(2) 0.016(3) Uani 1 8 d S . . C4 C -0.5000 -0.5000 -0.456(2) 0.016(3) Uani 1 8 d S . . C12 C 0.0000 -0.382(5) -0.5874(14) 0.12(4) Uiso 0.13 2 d SPD . . C11 C 0.0000 -0.180(5) -0.5784(18) 0.12(4) Uiso 0.13 2 d SPD . . C14 C 0.130(5) -0.130(5) -0.5000 0.12(4) Uiso 0.25 4 d SPD . . C15 C 0.092(14) -0.223(8) -0.4098(18) 0.12(4) Uiso 0.06 1 d PD . . C13 C 0.0000 -0.395(3) -0.4135(12) 0.12(4) Uiso 0.13 2 d SPD . . C16 C 0.0000 -0.5000 -0.5000 0.12(4) Uiso 0.50 8 d SPD . . C17 C 0.0000 -0.5000 -0.3284(14) 0.12(4) Uiso 0.25 4 d SPD . . C2 C -0.334(2) -0.5000 -0.2989(18) 0.016(3) Uani 0.50 2 d SPD . . H2 H -0.2197 -0.5000 -0.3338 0.019 Uiso 0.50 2 d SPD . . C1 C -0.3526 -0.5000 -0.2036 0.044 Uani 0.50 2 d SP . . H1 H -0.2381 -0.5000 -0.1701 0.053 Uiso 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 Pt1 0.0013(7) 0.0013(7) 0.0135(8) 0.000 0.000 0.000 Fe1 0.0031(17) 0.0031(17) 0.008(2) 0.000 0.000 0.000 N1 0.007(7) 0.007(7) 0.016(12) 0.000 0.000 0.000 N2 0.018(4) 0.018(4) 0.012(6) 0.000 0.000 0.000(8) C5 0.008(6) 0.008(6) 0.011(8) 0.000 0.000 0.003(8) C3 0.018(4) 0.018(4) 0.012(6) 0.000 0.000 0.000(8) C4 0.018(4) 0.018(4) 0.012(6) 0.000 0.000 0.000(8) C2 0.018(4) 0.018(4) 0.012(6) 0.000 0.000 0.000(8) C1 0.045 0.045 0.042 0.000 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 Pt1 C5 1.97(2) . ? Pt1 C5 1.97(2) 9 ? Pt1 C5 1.97(2) 11 ? Pt1 C5 1.97(2) 3 ? Fe1 N2 1.93(2) . ? Fe1 N2 1.93(2) 9_445 ? Fe1 N2 1.93(2) 11_455 ? Fe1 N2 1.93(2) 3_545 ? Fe1 N1 2.01(2) . ? Fe1 N1 2.01(2) 9_445 ? N1 C1 1.311(14) 14_445 ? N1 C1 1.311(14) 2_445 ? N1 C1 1.311(14) 13 ? N1 C1 1.311(14) . ? N2 C5 1.17(3) . ? C3 C4 1.42(4) . ? C3 C2 1.39(3) . ? C3 C2 1.39(3) 13 ? C3 C2 1.39(3) 14_445 ? C3 C2 1.39(3) 2_445 ? C4 C4 1.20(6) 9_444 ? C12 C13 0.09(3) 10_554 ? C12 C15 1.31(3) 10_554 ? C12 C15 1.31(3) 4_554 ? C12 C17 1.43(3) 9_544 ? C12 C11 1.45(2) . ? C12 C16 1.47(2) . ? C12 C13 1.61(5) 9_544 ? C12 C12 1.70(7) 2_545 ? C11 C15 0.75(11) 4_554 ? C11 C15 0.75(11) 10_554 ? C11 C14 1.465(19) . ? C11 C14 1.465(19) 11 ? C11 C13 1.54(3) 10_554 ? C11 C15 1.73(3) 5_554 ? C11 C15 1.73(3) 16_554 ? C11 C11 1.83(5) 14 ? C11 C11 1.83(5) 13 ? C14 C15 1.431(14) 10_554 ? C14 C15 1.431(14) 5_554 ? C14 C15 1.431(14) . ? C14 C15 1.431(14) 14 ? C14 C11 1.465(19) 14 ? C14 C11 1.465(19) 5_554 ? C14 C11 1.465(19) 10_554 ? C14 C14 1.86(7) 11 ? C14 C14 1.86(7) 3_554 ? C15 C11 0.75(11) 10_554 ? C15 C12 1.31(3) 10_554 ? C15 C15 1.34(8) 14 ? C15 C15 1.3(2) 11 ? C15 C13 1.394(15) . ? C15 C11 1.73(3) 5_554 ? C13 C12 0.09(3) 10_554 ? C13 C17 1.388(17) . ? C13 C15 1.394(15) 11 ? C13 C16 1.40(2) . ? C13 C13 1.51(5) 2_545 ? C13 C11 1.54(3) 10_554 ? C13 C12 1.61(5) 9_544 ? C16 C13 1.40(2) 9_544 ? C16 C13 1.40(2) 10_554 ? C16 C13 1.40(2) 2_545 ? C16 C12 1.47(2) 2_545 ? C16 C12 1.47(2) 10_554 ? C16 C12 1.47(2) 9_544 ? C17 C13 1.388(17) 2_545 ? C17 C12 1.43(3) 9_544 ? C17 C12 1.43(3) 10_554 ? C17 H2 1.5784 . ? C2 C1 1.31(2) . ? C2 C2 1.68(2) 14_445 ? C2 C2 1.68(2) 13 ? C2 H2 0.9507 . ? C1 C1 1.4964 14_445 ? C1 C1 1.4963 13 ? C1 H1 0.9406 . ? 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 C5 Pt1 C5 180.0(13) . 9 ? C5 Pt1 C5 90.0 . 11 ? C5 Pt1 C5 90.0 9 11 ? C5 Pt1 C5 90.0 . 3 ? C5 Pt1 C5 90.0 9 3 ? C5 Pt1 C5 180.0(6) 11 3 ? N2 Fe1 N2 180.0 . 9_445 ? N2 Fe1 N2 90.0 . 11_455 ? N2 Fe1 N2 90.0 9_445 11_455 ? N2 Fe1 N2 90.0 . 3_545 ? N2 Fe1 N2 90.0 9_445 3_545 ? N2 Fe1 N2 180.000(1) 11_455 3_545 ? N2 Fe1 N1 90.0 . . ? N2 Fe1 N1 90.0 9_445 . ? N2 Fe1 N1 90.0 11_455 . ? N2 Fe1 N1 90.0 3_545 . ? N2 Fe1 N1 90.000(1) . 9_445 ? N2 Fe1 N1 90.000(1) 9_445 9_445 ? N2 Fe1 N1 90.0 11_455 9_445 ? N2 Fe1 N1 90.0 3_545 9_445 ? N1 Fe1 N1 180.0 . 9_445 ? C1 N1 C1 69.6(9) 14_445 2_445 ? C1 N1 C1 107.6(17) 14_445 13 ? C1 N1 C1 69.6(9) 2_445 13 ? C1 N1 C1 69.6(9) 14_445 . ? C1 N1 C1 107.6(17) 2_445 . ? C1 N1 C1 69.6(9) 13 . ? C1 N1 Fe1 126.2(9) 14_445 . ? C1 N1 Fe1 126.2(9) 2_445 . ? C1 N1 Fe1 126.2(9) 13 . ? C1 N1 Fe1 126.2(9) . . ? C5 N2 Fe1 180(2) . . ? N2 C5 Pt1 180.0(17) . . ? C4 C3 C2 121.3(12) . . ? C4 C3 C2 121.3(12) . 13 ? C2 C3 C2 74.3(11) . 13 ? C4 C3 C2 121.3(12) . 14_445 ? C2 C3 C2 74.3(11) . 14_445 ? C2 C3 C2 117(2) 13 14_445 ? C4 C3 C2 121.3(12) . 2_445 ? C2 C3 C2 117(2) . 2_445 ? C2 C3 C2 74.3(11) 13 2_445 ? C2 C3 C2 74.3(11) 14_445 2_445 ? C4 C4 C3 180.000(9) 9_444 . ? C13 C12 C15 149(7) 10_554 10_554 ? C13 C12 C15 149(7) 10_554 4_554 ? C15 C12 C15 60(10) 10_554 4_554 ? C13 C12 C17 61(10) 10_554 9_544 ? C15 C12 C17 119(2) 10_554 9_544 ? C15 C12 C17 119(2) 4_554 9_544 ? C13 C12 C11 167(10) 10_554 . ? C17 C12 C11 131.3(17) 9_544 . ? C13 C12 C16 47(10) 10_554 . ? C15 C12 C16 122(3) 10_554 . ? C15 C12 C16 122(3) 4_554 . ? C17 C12 C16 108(2) 9_544 . ? C11 C12 C16 120.6(18) . . ? C15 C12 C13 150(5) 10_554 9_544 ? C15 C12 C13 150(5) 4_554 9_544 ? C17 C12 C13 54.0(15) 9_544 9_544 ? C11 C12 C13 174.7(17) . 9_544 ? C16 C12 C13 54.1(12) . 9_544 ? C15 C12 C12 150(5) 10_554 2_545 ? C15 C12 C12 150(5) 4_554 2_545 ? C17 C12 C12 53.5(12) 9_544 2_545 ? C11 C12 C12 175.2(10) . 2_545 ? C16 C12 C12 54.6(13) . 2_545 ? C15 C11 C15 124(6) 4_554 10_554 ? C15 C11 C12 64(2) 4_554 . ? C15 C11 C12 64(2) 10_554 . ? C15 C11 C14 145(4) 4_554 . ? C15 C11 C14 73(3) 10_554 . ? C12 C11 C14 108(2) . . ? C15 C11 C14 73(3) 4_554 11 ? C15 C11 C14 145(4) 10_554 11 ? C12 C11 C14 108(2) . 11 ? C14 C11 C14 79(4) . 11 ? C15 C11 C13 64(2) 4_554 10_554 ? C15 C11 C13 64(2) 10_554 10_554 ? C14 C11 C13 107(2) . 10_554 ? C14 C11 C13 107(2) 11 10_554 ? C15 C11 C15 162(5) 4_554 5_554 ? C15 C11 C15 47(4) 10_554 5_554 ? C12 C11 C15 111(4) . 5_554 ? C14 C11 C15 52.4(10) . 5_554 ? C14 C11 C15 125(4) 11 5_554 ? C13 C11 C15 111(4) 10_554 5_554 ? C15 C11 C15 47(4) 4_554 16_554 ? C15 C11 C15 162(5) 10_554 16_554 ? C12 C11 C15 111(4) . 16_554 ? C14 C11 C15 125(4) . 16_554 ? C14 C11 C15 52.4(10) 11 16_554 ? C13 C11 C15 111(4) 10_554 16_554 ? C15 C11 C15 136(7) 5_554 16_554 ? C15 C11 C11 157(2) 4_554 14 ? C15 C11 C11 71(2) 10_554 14 ? C12 C11 C11 134.80(9) . 14 ? C14 C11 C11 51.5(11) . 14 ? C14 C11 C11 106(3) 11 14 ? C13 C11 C11 134.86(9) 10_554 14 ? C15 C11 C11 113(4) 16_554 14 ? C15 C11 C11 71(2) 4_554 13 ? C15 C11 C11 157(2) 10_554 13 ? C12 C11 C11 134.80(9) . 13 ? C14 C11 C11 106(3) . 13 ? C14 C11 C11 51.5(11) 11 13 ? C13 C11 C11 134.86(9) 10_554 13 ? C15 C11 C11 113(4) 5_554 13 ? C15 C11 C11 24(4) 16_554 13 ? C11 C11 C11 90.000(5) 14 13 ? C15 C14 C15 56(3) 10_554 5_554 ? C15 C14 C15 119(3) 10_554 . ? C15 C14 C15 157(10) 5_554 . ? C15 C14 C15 157(10) 10_554 14 ? C15 C14 C15 119(3) 5_554 14 ? C15 C14 C15 56(3) . 14 ? C15 C14 C11 73.4(16) 5_554 . ? C15 C14 C11 113(2) . . ? C15 C14 C11 167(2) 14 . ? C15 C14 C11 73.4(16) 10_554 14 ? C15 C14 C11 30(5) 5_554 14 ? C15 C14 C11 167(2) . 14 ? C15 C14 C11 113(2) 14 14 ? C11 C14 C11 77(2) . 14 ? C15 C14 C11 167(2) 10_554 5_554 ? C15 C14 C11 113(2) 5_554 5_554 ? C15 C14 C11 73.4(16) . 5_554 ? C11 C14 C11 148(5) . 5_554 ? C11 C14 C11 94.1(19) 14 5_554 ? C15 C14 C11 113(2) 10_554 10_554 ? C15 C14 C11 167(2) 5_554 10_554 ? C15 C14 C11 73.4(16) 14 10_554 ? C11 C14 C11 94.1(19) . 10_554 ? C11 C14 C11 148(5) 14 10_554 ? C11 C14 C11 77(2) 5_554 10_554 ? C15 C14 C14 79(5) 10_554 11 ? C15 C14 C14 118(3) 5_554 11 ? C15 C14 C14 79(5) . 11 ? C15 C14 C14 118(3) 14 11 ? C11 C14 C14 50.5(18) . 11 ? C11 C14 C14 104(2) 14 11 ? C11 C14 C14 104(2) 5_554 11 ? C11 C14 C14 50.5(18) 10_554 11 ? C15 C14 C14 118(3) 10_554 3_554 ? C15 C14 C14 79(5) 5_554 3_554 ? C15 C14 C14 118(3) . 3_554 ? C15 C14 C14 79(5) 14 3_554 ? C11 C14 C14 104(2) . 3_554 ? C11 C14 C14 50.5(18) 14 3_554 ? C11 C14 C14 50.5(18) 5_554 3_554 ? C11 C14 C14 104(2) 10_554 3_554 ? C14 C14 C14 90.0 11 3_554 ? C11 C15 C12 85(5) 10_554 10_554 ? C11 C15 C15 109(2) 10_554 14 ? C12 C15 C15 165(5) 10_554 14 ? C11 C15 C15 28(3) 10_554 11 ? C12 C15 C15 60(5) 10_554 11 ? C15 C15 C15 135.000(9) 14 11 ? C11 C15 C13 87(5) 10_554 . ? C15 C15 C13 163(5) 14 . ? C15 C15 C13 62(5) 11 . ? C11 C15 C14 78(4) 10_554 . ? C12 C15 C14 118(3) 10_554 . ? C15 C15 C14 62.1(16) 14 . ? C15 C15 C14 101(5) 11 . ? C13 C15 C14 118.2(19) . . ? C11 C15 C11 85(5) 10_554 5_554 ? C12 C15 C11 169(6) 10_554 5_554 ? C15 C15 C11 24(4) 14 5_554 ? C15 C15 C11 111(4) 11 5_554 ? C13 C15 C11 170(5) . 5_554 ? C14 C15 C11 54.2(10) . 5_554 ? C12 C13 C17 115(10) 10_554 . ? C17 C13 C15 116.7(14) . . ? C17 C13 C15 116.7(14) . 11 ? C15 C13 C15 56(10) . 11 ? C12 C13 C16 130(10) 10_554 . ? C17 C13 C16 114.3(18) . . ? C15 C13 C16 120(3) . . ? C15 C13 C16 120(3) 11 . ? C12 C13 C13 172(10) 10_554 2_545 ? C17 C13 C13 57.0(11) . 2_545 ? C15 C13 C13 152(5) . 2_545 ? C15 C13 C13 152(5) 11 2_545 ? C16 C13 C13 57.4(9) . 2_545 ? C12 C13 C11 12(10) 10_554 10_554 ? C17 C13 C11 127.1(18) . 10_554 ? C16 C13 C11 118.6(17) . 10_554 ? C13 C13 C11 175.9(13) 2_545 10_554 ? C12 C13 C12 172(10) 10_554 9_544 ? C17 C13 C12 56.5(12) . 9_544 ? C15 C13 C12 152(5) . 9_544 ? C15 C13 C12 152(5) 11 9_544 ? C16 C13 C12 57.8(13) . 9_544 ? C13 C13 C12 0.4(11) 2_545 9_544 ? C11 C13 C12 176(2) 10_554 9_544 ? C13 C16 C13 65.3(17) 9_544 10_554 ? C13 C16 C13 180.000(3) 9_544 . ? C13 C16 C13 114.7(17) 10_554 . ? C13 C16 C13 114.7(17) 9_544 2_545 ? C13 C16 C13 180.0(7) 10_554 2_545 ? C13 C16 C13 65.3(17) . 2_545 ? C13 C16 C12 68.1(18) 10_554 2_545 ? C13 C16 C12 177.2(13) . 2_545 ? C13 C16 C12 111.9(18) 2_545 2_545 ? C13 C16 C12 68.1(18) 9_544 . ? C13 C16 C12 111.9(18) . . ? C13 C16 C12 177.2(13) 2_545 . ? C12 C16 C12 71(3) 2_545 . ? C13 C16 C12 177.2(13) 9_544 10_554 ? C13 C16 C12 111.9(18) 10_554 10_554 ? C13 C16 C12 68.1(18) 2_545 10_554 ? C12 C16 C12 180.000(4) 2_545 10_554 ? C12 C16 C12 109(3) . 10_554 ? C13 C16 C12 111.9(18) 9_544 9_544 ? C13 C16 C12 177.2(13) 10_554 9_544 ? C13 C16 C12 68.1(18) . 9_544 ? C12 C16 C12 109(3) 2_545 9_544 ? C12 C16 C12 180.000(3) . 9_544 ? C12 C16 C12 71(3) 10_554 9_544 ? C13 C17 C13 66(2) 2_545 . ? C13 C17 C12 69.5(19) . 9_544 ? C13 C17 C12 69.5(19) 2_545 10_554 ? C12 C17 C12 73(2) 9_544 10_554 ? C13 C17 H2 87.8 2_545 . ? C13 C17 H2 87.8 . . ? C12 C17 H2 87.8 9_544 . ? C12 C17 H2 87.8 10_554 . ? C1 C2 C3 115.6(13) . . ? C1 C2 C2 85.9(6) . 14_445 ? C3 C2 C2 52.8(6) . 14_445 ? C1 C2 C2 85.9(6) . 13 ? C3 C2 C2 52.8(6) . 13 ? C2 C2 C2 90.000(3) 14_445 13 ? C1 C2 H2 125.9 . . ? C3 C2 H2 118.6 . . ? C2 C2 H2 127.7 14_445 . ? C2 C2 H2 127.7 13 . ? N1 C1 C2 132.0(12) . . ? N1 C1 C1 55.2(4) . 14_445 ? C2 C1 C1 94.1(6) . 14_445 ? N1 C1 C1 55.2(4) . 13 ? C2 C1 C1 94.1(6) . 13 ? C1 C1 C1 90.0 14_445 13 ? N1 C1 H1 114.6 . . ? C2 C1 H1 113.4 . . ? C1 C1 H1 128.1 14_445 . ? C1 C1 H1 128.1 13 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.429 _refine_diff_density_min -2.047 _refine_diff_density_rms 0.438