Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jose Real' _publ_contact_author_address ; Department de Quimica Inorganica Universitat de Valencia Institut de Ciencia Molecular Edificio de Institutos de Paterna PO BOx 22085 Valencia 46071 SPAIN ; _publ_contact_author_email JOSE.A.REAL@UV.ES _publ_section_title ; Thermal, Pressure and Light Induced Spin Transition in the Two-Dimensional Coordination Polymer {Fe(pmd)2[Cu(CN)2]2} ; loop_ _publ_author_name 'Jose Real' 'Gloria Agusti' 'Ramon Burriel' 'Miguel Castro' 'Ana B. Gaspar' 'Andres Goeta' ; M.C.Monoz ; 'Jose Alberto Rodriguez-Valamazan' 'Amber L. Thompson' data_030ki _database_code_depnum_ccdc_archive 'CCDC 654145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fe(Pmd)2[Cu(CN)2]2 ; _chemical_name_common Fe(Pmd)2(Cu(CN)2)2 _chemical_melting_point 'not measured' _chemical_formula_moiety 'C12 H8 Cu2 Fe N8' _chemical_formula_sum 'C12 H8 Cu2 Fe N8' _chemical_formula_weight 447.19 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.71(4) _cell_length_b 8.15(11) _cell_length_c 7.98(7) _cell_angle_alpha 110.6(11) _cell_angle_beta 108.1(13) _cell_angle_gamma 99.2(10) _cell_volume 371(6) _cell_formula_units_Z 1 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 271 _cell_measurement_theta_min 5.949 _cell_measurement_theta_max 56.833 _exptl_crystal_description block _exptl_crystal_colour unknown _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 220 _exptl_absorpt_coefficient_mu 3.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8033 _exptl_absorpt_correction_T_max 0.8941 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered a hemisphere of reciprocal Space, by a combination of 1 set of \w scans each set at different \f and/or 2\q angles and each scan (32s exposure) covering 0.3\% in \w. Crystal to detector distance 4.965cm. ; _diffrn_ambient_temperature 30(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker ProteumM with Bede Microsource' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 1259 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1404 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 2 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 29.10 _reflns_number_total 1259 _reflns_number_gt 786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1005P)^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_number_reflns 1259 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1253 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1784 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Fe1 Fe 0.0000 1.0000 1.0000 0.0078(5) Uiso 1 2 d S . . Cu1 Cu -0.4817(2) 0.6301(2) 0.1527(2) 0.0099(4) Uiso 1 1 d . . . N1 N 0.2437(16) 0.8943(17) 1.1305(15) 0.014(2) Uiso 1 1 d . . . C1 C 0.3572(18) 0.8107(19) 1.1566(16) 0.010(2) Uiso 1 1 d . . . N2 N 0.2515(15) 1.2495(16) 1.0819(14) 0.0109(19) Uiso 1 1 d . . . C2 C 0.3575(18) 1.374(2) 1.0902(16) 0.011(2) Uiso 1 1 d . . . N3 N 0.0272(15) 0.8615(16) 0.7115(13) 0.0106(19) Uiso 1 1 d . . . C3 C 0.2028(17) 0.8117(18) 0.6941(16) 0.009(2) Uiso 1 1 d . . . H3 H 0.3332 0.8474 0.8063 0.011 Uiso 1 1 calc R . . C4 C 0.1916(19) 0.706(2) 0.5090(17) 0.014(2) Uiso 1 1 d . . . H4 H 0.3139 0.6690 0.4925 0.017 Uiso 1 1 calc R . . N4 N -0.1741(15) 0.7132(16) 0.3712(14) 0.011(2) Uiso 1 1 d . . . C5 C 0.0007(18) 0.6584(19) 0.3515(17) 0.012(2) Uiso 1 1 d . . . H5 H -0.0096 0.5846 0.2251 0.014 Uiso 1 1 calc R . . C6 C -0.1477(19) 0.812(2) 0.5538(17) 0.014(2) Uiso 1 1 d . . . H6 H -0.2689 0.8511 0.5710 0.017 Uiso 1 1 calc R . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.13(3) 2_577 ? Fe1 N1 2.13(3) . ? Fe1 N2 2.17(4) . ? Fe1 N2 2.17(4) 2_577 ? Fe1 N3 2.26(3) . ? Fe1 N3 2.26(3) 2_577 ? Cu1 C1 1.96(2) 1_454 ? Cu1 C2 2.00(4) 1_444 ? Cu1 N4 2.06(4) . ? Cu1 C2 2.33(2) 2_576 ? Cu1 Cu1 2.52(4) 2_465 ? N1 C1 1.120(19) . ? C1 Cu1 1.96(2) 1_656 ? N2 C2 1.11(2) . ? C2 Cu1 2.00(4) 1_666 ? C2 Cu1 2.33(2) 2_576 ? N3 C6 1.30(3) . ? N3 C3 1.337(16) . ? C3 C4 1.39(3) . ? C3 H3 0.9500 . ? C4 C5 1.37(3) . ? C4 H4 0.9500 . ? N4 C6 1.33(2) . ? N4 C5 1.354(17) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 N1 Fe1 N1 180.000(5) 2_577 . ? N1 Fe1 N2 89.6(13) 2_577 . ? N1 Fe1 N2 90.4(13) . . ? N1 Fe1 N2 90.4(13) 2_577 2_577 ? N1 Fe1 N2 89.6(13) . 2_577 ? N2 Fe1 N2 180.000(1) . 2_577 ? N1 Fe1 N3 90.2(12) 2_577 . ? N1 Fe1 N3 89.8(12) . . ? N2 Fe1 N3 92.0(16) . . ? N2 Fe1 N3 88.0(16) 2_577 . ? N1 Fe1 N3 89.8(12) 2_577 2_577 ? N1 Fe1 N3 90.2(12) . 2_577 ? N2 Fe1 N3 88.0(16) . 2_577 ? N2 Fe1 N3 92.0(16) 2_577 2_577 ? N3 Fe1 N3 180.000(4) . 2_577 ? C1 Cu1 C2 119.1(10) 1_454 1_444 ? C1 Cu1 N4 118.0(13) 1_454 . ? C2 Cu1 N4 110.0(15) 1_444 . ? C1 Cu1 C2 100.9(10) 1_454 2_576 ? C2 Cu1 C2 109.4(12) 1_444 2_576 ? N4 Cu1 C2 95.9(9) . 2_576 ? C1 Cu1 Cu1 124.2(11) 1_454 2_465 ? C2 Cu1 Cu1 60.9(12) 1_444 2_465 ? N4 Cu1 Cu1 111.5(15) . 2_465 ? C2 Cu1 Cu1 48.5(9) 2_576 2_465 ? C1 N1 Fe1 164.2(11) . . ? N1 C1 Cu1 169.2(12) . 1_656 ? C2 N2 Fe1 166.9(9) . . ? N2 C2 Cu1 165.7(11) . 1_666 ? N2 C2 Cu1 122.9(15) . 2_576 ? Cu1 C2 Cu1 70.6(12) 1_666 2_576 ? C6 N3 C3 118.6(13) . . ? C6 N3 Fe1 117.2(12) . . ? C3 N3 Fe1 123.8(15) . . ? N3 C3 C4 119.0(17) . . ? N3 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.5(16) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C6 N4 C5 115.2(17) . . ? C6 N4 Cu1 118.2(15) . . ? C5 N4 Cu1 126.1(11) . . ? N4 C5 C4 121.7(14) . . ? N4 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N3 C6 N4 126.9(15) . . ? N3 C6 H6 116.6 . . ? N4 C6 H6 116.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 N1 C1 77(100) 2_577 . . . ? N2 Fe1 N1 C1 -114(4) . . . . ? N2 Fe1 N1 C1 66(4) 2_577 . . . ? N3 Fe1 N1 C1 -22(4) . . . . ? N3 Fe1 N1 C1 158(4) 2_577 . . . ? Fe1 N1 C1 Cu1 -17(9) . . . 1_656 ? N1 Fe1 N2 C2 -41(5) 2_577 . . . ? N1 Fe1 N2 C2 139(5) . . . . ? N2 Fe1 N2 C2 -85(100) 2_577 . . . ? N3 Fe1 N2 C2 49(5) . . . . ? N3 Fe1 N2 C2 -131(5) 2_577 . . . ? Fe1 N2 C2 Cu1 109(5) . . . 1_666 ? Fe1 N2 C2 Cu1 -50(5) . . . 2_576 ? N1 Fe1 N3 C6 -28.9(11) 2_577 . . . ? N1 Fe1 N3 C6 151.1(11) . . . . ? N2 Fe1 N3 C6 -118.5(15) . . . . ? N2 Fe1 N3 C6 61.5(15) 2_577 . . . ? N3 Fe1 N3 C6 8(100) 2_577 . . . ? N1 Fe1 N3 C3 158.1(11) 2_577 . . . ? N1 Fe1 N3 C3 -21.9(11) . . . . ? N2 Fe1 N3 C3 68.4(15) . . . . ? N2 Fe1 N3 C3 -111.6(15) 2_577 . . . ? N3 Fe1 N3 C3 -165(100) 2_577 . . . ? C6 N3 C3 C4 -1.1(18) . . . . ? Fe1 N3 C3 C4 171.9(10) . . . . ? N3 C3 C4 C5 0.1(19) . . . . ? C1 Cu1 N4 C6 44.7(13) 1_454 . . . ? C2 Cu1 N4 C6 -96.5(14) 1_444 . . . ? C2 Cu1 N4 C6 150.4(11) 2_576 . . . ? Cu1 Cu1 N4 C6 -162.1(9) 2_465 . . . ? C1 Cu1 N4 C5 -143.9(12) 1_454 . . . ? C2 Cu1 N4 C5 74.9(14) 1_444 . . . ? C2 Cu1 N4 C5 -38.2(12) 2_576 . . . ? Cu1 Cu1 N4 C5 9.3(11) 2_465 . . . ? C6 N4 C5 C4 -1.6(18) . . . . ? Cu1 N4 C5 C4 -173.2(10) . . . . ? C3 C4 C5 N4 1(2) . . . . ? C3 N3 C6 N4 1(2) . . . . ? Fe1 N3 C6 N4 -172.7(11) . . . . ? C5 N4 C6 N3 1(2) . . . . ? Cu1 N4 C6 N3 172.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.636 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.636 _refine_diff_density_max 1.734 _refine_diff_density_min -2.154 _refine_diff_density_rms 0.225 # Attachment '090k.cif' data_090k _database_code_depnum_ccdc_archive 'CCDC 654146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fe(Pmd)2[Cu(CN)2]2 ; _chemical_name_common Fe(Pmd)2(Cu(CN)2)2 _chemical_melting_point 'not measured' _chemical_formula_moiety 'C12 H8 Cu2 Fe N8' _chemical_formula_sum 'C12 H8 Cu2 Fe N8' _chemical_formula_weight 447.19 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8434(13) _cell_length_b 7.7006(14) _cell_length_c 7.7696(15) _cell_angle_alpha 109.077(4) _cell_angle_beta 108.194(4) _cell_angle_gamma 99.021(4) _cell_volume 352.00(11) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1160 _cell_measurement_theta_min 6.024 _cell_measurement_theta_max 57.770 _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 220 _exptl_absorpt_coefficient_mu 4.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.8889 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (32s exposure) covering 0.3\% in \w. Crystal to detector distance 4.965cm. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker ProteumM with Bede Microsource' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 3761 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 29.13 _reflns_number_total 1864 _reflns_number_gt 1487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0459P)^2^+1.0734P] 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 1864 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _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 Fe1 Fe 0.0000 1.0000 1.0000 0.0090(2) Uani 1 2 d S . . N1 N 0.2126(7) 0.8816(5) 1.1088(6) 0.0121(8) Uani 1 1 d . . . C1 C 0.3353(8) 0.8015(7) 1.1517(7) 0.0126(9) Uani 1 1 d . . . Cu1 Cu -0.49088(10) 0.62546(8) 0.15683(9) 0.01197(17) Uani 1 1 d . . . N2 N 0.2294(7) 1.2207(6) 1.0547(6) 0.0135(8) Uani 1 1 d . . . C2 C 0.3513(8) 1.3543(7) 1.0777(7) 0.0135(9) Uani 1 1 d . . . N3 N 0.0083(6) 0.8667(5) 0.7301(6) 0.0123(8) Uani 1 1 d . . . C3 C 0.1880(8) 0.8365(7) 0.7059(7) 0.0157(9) Uani 1 1 d . . . H3 H 0.3209 0.8842 0.8167 0.019 Uiso 1 1 calc R . . C4 C 0.1777(8) 0.7349(8) 0.5173(8) 0.0191(10) Uani 1 1 d . . . H4 H 0.3028 0.7096 0.4987 0.023 Uiso 1 1 calc R . . N4 N -0.1939(7) 0.7075(6) 0.3834(6) 0.0136(8) Uani 1 1 d . . . C5 C -0.0144(8) 0.6713(7) 0.3582(7) 0.0159(9) Uani 1 1 d . . . H5 H -0.0219 0.6013 0.2293 0.019 Uiso 1 1 calc R . . C6 C -0.1741(8) 0.8030(7) 0.5694(7) 0.0146(9) Uani 1 1 d . . . H6 H -0.2992 0.8274 0.5886 0.018 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 Fe1 0.0076(4) 0.0083(4) 0.0099(4) 0.0029(3) 0.0034(3) 0.0004(3) N1 0.0142(19) 0.0082(17) 0.0131(18) 0.0019(14) 0.0079(15) 0.0013(15) C1 0.013(2) 0.014(2) 0.008(2) 0.0026(16) 0.0045(17) -0.0008(17) Cu1 0.0105(3) 0.0104(3) 0.0124(3) 0.0025(2) 0.0038(2) 0.0021(2) N2 0.016(2) 0.016(2) 0.0116(18) 0.0064(15) 0.0063(15) 0.0088(16) C2 0.011(2) 0.010(2) 0.014(2) 0.0009(16) 0.0035(17) 0.0015(17) N3 0.0101(18) 0.0104(18) 0.0118(18) 0.0039(14) 0.0004(15) -0.0003(14) C3 0.013(2) 0.019(2) 0.015(2) 0.0075(18) 0.0063(18) 0.0015(18) C4 0.008(2) 0.028(3) 0.020(2) 0.012(2) 0.0031(19) 0.0007(19) N4 0.0113(19) 0.0115(18) 0.0139(18) 0.0032(15) 0.0026(15) 0.0008(14) C5 0.016(2) 0.018(2) 0.014(2) 0.0055(18) 0.0079(19) 0.0045(18) C6 0.010(2) 0.012(2) 0.016(2) 0.0025(18) 0.0007(18) 0.0026(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.951(4) 2_577 ? Fe1 N2 1.951(4) . ? Fe1 N1 1.953(4) . ? Fe1 N1 1.953(4) 2_577 ? Fe1 N3 2.035(4) 2_577 ? Fe1 N3 2.035(4) . ? N1 C1 1.148(7) . ? C1 Cu1 1.941(5) 1_656 ? Cu1 C1 1.941(5) 1_454 ? Cu1 C2 1.986(5) 1_444 ? Cu1 N4 2.065(4) . ? Cu1 C2 2.342(5) 2_576 ? Cu1 Cu1 2.5189(12) 2_465 ? N2 C2 1.142(7) . ? C2 Cu1 1.986(5) 1_666 ? C2 Cu1 2.342(5) 2_576 ? N3 C6 1.339(6) . ? N3 C3 1.344(6) . ? C3 C4 1.390(7) . ? C3 H3 0.9500 . ? C4 C5 1.372(7) . ? C4 H4 0.9500 . ? N4 C6 1.342(6) . ? N4 C5 1.359(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 N2 Fe1 N2 180.000(1) 2_577 . ? N2 Fe1 N1 89.70(16) 2_577 . ? N2 Fe1 N1 90.30(16) . . ? N2 Fe1 N1 90.30(16) 2_577 2_577 ? N2 Fe1 N1 89.70(16) . 2_577 ? N1 Fe1 N1 180.000(2) . 2_577 ? N2 Fe1 N3 89.74(16) 2_577 2_577 ? N2 Fe1 N3 90.26(16) . 2_577 ? N1 Fe1 N3 91.23(16) . 2_577 ? N1 Fe1 N3 88.77(16) 2_577 2_577 ? N2 Fe1 N3 90.26(16) 2_577 . ? N2 Fe1 N3 89.74(16) . . ? N1 Fe1 N3 88.77(16) . . ? N1 Fe1 N3 91.23(16) 2_577 . ? N3 Fe1 N3 180.000(1) 2_577 . ? C1 N1 Fe1 172.4(4) . . ? N1 C1 Cu1 166.1(4) . 1_656 ? C1 Cu1 C2 115.8(2) 1_454 1_444 ? C1 Cu1 N4 120.57(17) 1_454 . ? C2 Cu1 N4 111.64(18) 1_444 . ? C1 Cu1 C2 101.17(18) 1_454 2_576 ? C2 Cu1 C2 109.36(16) 1_444 2_576 ? N4 Cu1 C2 94.67(17) . 2_576 ? C1 Cu1 Cu1 121.57(14) 1_454 2_465 ? C2 Cu1 Cu1 61.29(14) 1_444 2_465 ? N4 Cu1 Cu1 111.49(12) . 2_465 ? C2 Cu1 Cu1 48.07(11) 2_576 2_465 ? C2 N2 Fe1 174.5(4) . . ? N2 C2 Cu1 162.5(4) . 1_666 ? N2 C2 Cu1 123.7(4) . 2_576 ? Cu1 C2 Cu1 70.64(16) 1_666 2_576 ? C6 N3 C3 118.4(4) . . ? C6 N3 Fe1 118.6(3) . . ? C3 N3 Fe1 123.0(3) . . ? N3 C3 C4 119.4(4) . . ? N3 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 N4 C5 116.9(4) . . ? C6 N4 Cu1 118.5(3) . . ? C5 N4 Cu1 124.6(3) . . ? N4 C5 C4 120.6(5) . . ? N4 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? N3 C6 N4 125.0(5) . . ? N3 C6 H6 117.5 . . ? N4 C6 H6 117.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C1 86(3) 2_577 . . . ? N2 Fe1 N1 C1 -94(3) . . . . ? N1 Fe1 N1 C1 27(100) 2_577 . . . ? N3 Fe1 N1 C1 175(3) 2_577 . . . ? N3 Fe1 N1 C1 -5(3) . . . . ? Fe1 N1 C1 Cu1 -19(5) . . . 1_656 ? N2 Fe1 N2 C2 76(100) 2_577 . . . ? N1 Fe1 N2 C2 168(4) . . . . ? N1 Fe1 N2 C2 -12(4) 2_577 . . . ? N3 Fe1 N2 C2 -100(4) 2_577 . . . ? N3 Fe1 N2 C2 80(4) . . . . ? Fe1 N2 C2 Cu1 63(5) . . . 1_666 ? Fe1 N2 C2 Cu1 -79(4) . . . 2_576 ? N2 Fe1 N3 C6 54.4(4) 2_577 . . . ? N2 Fe1 N3 C6 -125.6(4) . . . . ? N1 Fe1 N3 C6 144.1(4) . . . . ? N1 Fe1 N3 C6 -35.9(4) 2_577 . . . ? N3 Fe1 N3 C6 2(100) 2_577 . . . ? N2 Fe1 N3 C3 -124.4(4) 2_577 . . . ? N2 Fe1 N3 C3 55.6(4) . . . . ? N1 Fe1 N3 C3 -34.7(4) . . . . ? N1 Fe1 N3 C3 145.3(4) 2_577 . . . ? N3 Fe1 N3 C3 -177(100) 2_577 . . . ? C6 N3 C3 C4 -2.3(7) . . . . ? Fe1 N3 C3 C4 176.4(4) . . . . ? N3 C3 C4 C5 1.7(8) . . . . ? C1 Cu1 N4 C6 43.6(4) 1_454 . . . ? C2 Cu1 N4 C6 -97.5(4) 1_444 . . . ? C2 Cu1 N4 C6 149.5(4) 2_576 . . . ? Cu1 Cu1 N4 C6 -164.0(3) 2_465 . . . ? C1 Cu1 N4 C5 -136.6(4) 1_454 . . . ? C2 Cu1 N4 C5 82.3(4) 1_444 . . . ? C2 Cu1 N4 C5 -30.7(4) 2_576 . . . ? Cu1 Cu1 N4 C5 15.8(4) 2_465 . . . ? C6 N4 C5 C4 -1.5(7) . . . . ? Cu1 N4 C5 C4 178.6(4) . . . . ? C3 C4 C5 N4 0.3(8) . . . . ? C3 N3 C6 N4 1.1(7) . . . . ? Fe1 N3 C6 N4 -177.8(4) . . . . ? C5 N4 C6 N3 0.9(7) . . . . ? Cu1 N4 C6 N3 -179.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.160 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.185 # Attachment '180k.cif' data_180k _database_code_depnum_ccdc_archive 'CCDC 654147' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fe(Pmd)2[Cu(CN)2]2 ; _chemical_name_common Fe(Pmd)2(Cu(CN)2)2 _chemical_melting_point 'not measured' _chemical_formula_moiety 'C12 H8 Cu2 Fe N8' _chemical_formula_sum 'C12 H8 Cu2 Fe N8' _chemical_formula_weight 447.19 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7584(12) _cell_length_b 8.0796(15) _cell_length_c 7.9862(15) _cell_angle_alpha 110.102(3) _cell_angle_beta 108.500(4) _cell_angle_gamma 99.272(4) _cell_volume 370.06(12) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1189 _cell_measurement_theta_min 5.933 _cell_measurement_theta_max 51.859 _exptl_crystal_description block _exptl_crystal_colour clear_intense_yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 220 _exptl_absorpt_coefficient_mu 3.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8030 _exptl_absorpt_correction_T_max 0.8939 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (32s exposure) covering 0.3\% in \w. Crystal to detector distance 4.965cm. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker ProteumM with Bede Microsource' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 3927 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 29.12 _reflns_number_total 1939 _reflns_number_gt 1395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0262P)^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_number_reflns 1939 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 Fe1 Fe 0.0000 1.0000 1.0000 0.01539(18) Uani 1 2 d S . . Cu1 Cu -0.48379(8) 0.62957(6) 0.15219(7) 0.01935(15) Uani 1 1 d . . . N1 N 0.2414(5) 0.8921(4) 1.1278(5) 0.0228(7) Uani 1 1 d . . . C1 C 0.3544(6) 0.8068(5) 1.1557(5) 0.0201(8) Uani 1 1 d . . . N2 N 0.2504(5) 1.2458(5) 1.0786(5) 0.0225(7) Uani 1 1 d . . . C2 C 0.3588(6) 1.3736(5) 1.0895(6) 0.0213(8) Uani 1 1 d . . . N3 N 0.0257(5) 0.8621(4) 0.7128(5) 0.0192(7) Uani 1 1 d . . . C3 C 0.1992(7) 0.8120(6) 0.6909(6) 0.0267(9) Uani 1 1 d . . . H3 H 0.3300 0.8469 0.8025 0.032 Uiso 1 1 calc R . . C4 C 0.1900(7) 0.7105(6) 0.5084(6) 0.0301(10) Uani 1 1 d . . . H4 H 0.3130 0.6760 0.4924 0.036 Uiso 1 1 calc R . . N4 N -0.1761(5) 0.7120(4) 0.3706(4) 0.0189(7) Uani 1 1 d . . . C5 C -0.0029(6) 0.6608(6) 0.3503(6) 0.0256(9) Uani 1 1 d . . . H5 H -0.0137 0.5884 0.2237 0.031 Uiso 1 1 calc R . . C6 C -0.1516(6) 0.8110(5) 0.5512(6) 0.0223(8) Uani 1 1 d . . . H6 H -0.2730 0.8492 0.5665 0.027 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 Fe1 0.0140(4) 0.0154(4) 0.0157(4) 0.0067(3) 0.0051(3) 0.0032(3) Cu1 0.0190(3) 0.0171(2) 0.0190(3) 0.00554(18) 0.0064(2) 0.00504(18) N1 0.0238(18) 0.0223(17) 0.0221(18) 0.0093(14) 0.0094(15) 0.0065(14) C1 0.021(2) 0.0232(19) 0.0152(19) 0.0077(15) 0.0091(16) 0.0017(16) N2 0.0215(18) 0.0264(17) 0.0203(17) 0.0103(13) 0.0091(15) 0.0068(14) C2 0.018(2) 0.0204(19) 0.020(2) 0.0060(15) 0.0029(16) 0.0072(16) N3 0.0164(16) 0.0207(16) 0.0179(16) 0.0063(13) 0.0072(13) 0.0025(12) C3 0.022(2) 0.033(2) 0.028(2) 0.0144(18) 0.0124(19) 0.0060(17) C4 0.020(2) 0.045(3) 0.028(2) 0.015(2) 0.0126(19) 0.0122(19) N4 0.0165(16) 0.0188(15) 0.0179(17) 0.0070(13) 0.0047(13) 0.0029(12) C5 0.021(2) 0.030(2) 0.021(2) 0.0066(17) 0.0100(17) 0.0044(16) C6 0.022(2) 0.0228(19) 0.021(2) 0.0093(16) 0.0072(17) 0.0083(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.116(3) . ? Fe1 N1 2.116(3) 2_577 ? Fe1 N2 2.142(3) . ? Fe1 N2 2.142(3) 2_577 ? Fe1 N3 2.256(3) . ? Fe1 N3 2.256(3) 2_577 ? Cu1 C1 1.935(4) 1_454 ? Cu1 C2 1.975(4) 1_444 ? Cu1 N4 2.065(3) . ? Cu1 C2 2.334(4) 2_576 ? Cu1 Cu1 2.5211(10) 2_465 ? N1 C1 1.129(5) . ? C1 Cu1 1.935(4) 1_656 ? N2 C2 1.124(5) . ? C2 Cu1 1.975(4) 1_666 ? C2 Cu1 2.334(4) 2_576 ? N3 C6 1.328(5) . ? N3 C3 1.343(5) . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? C4 C5 1.376(6) . ? C4 H4 0.9500 . ? N4 C6 1.327(5) . ? N4 C5 1.341(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 N1 Fe1 N1 180.000(1) . 2_577 ? N1 Fe1 N2 89.94(12) . . ? N1 Fe1 N2 90.06(12) 2_577 . ? N1 Fe1 N2 90.06(12) . 2_577 ? N1 Fe1 N2 89.94(12) 2_577 2_577 ? N2 Fe1 N2 180.000(1) . 2_577 ? N1 Fe1 N3 89.20(12) . . ? N1 Fe1 N3 90.80(12) 2_577 . ? N2 Fe1 N3 91.28(12) . . ? N2 Fe1 N3 88.72(12) 2_577 . ? N1 Fe1 N3 90.80(12) . 2_577 ? N1 Fe1 N3 89.20(12) 2_577 2_577 ? N2 Fe1 N3 88.72(12) . 2_577 ? N2 Fe1 N3 91.28(12) 2_577 2_577 ? N3 Fe1 N3 180.000(1) . 2_577 ? C1 Cu1 C2 118.61(16) 1_454 1_444 ? C1 Cu1 N4 118.59(14) 1_454 . ? C2 Cu1 N4 109.80(14) 1_444 . ? C1 Cu1 C2 102.00(14) 1_454 2_576 ? C2 Cu1 C2 108.94(13) 1_444 2_576 ? N4 Cu1 C2 95.32(13) . 2_576 ? C1 Cu1 Cu1 124.59(12) 1_454 2_465 ? C2 Cu1 Cu1 61.11(12) 1_444 2_465 ? N4 Cu1 Cu1 110.56(9) . 2_465 ? C2 Cu1 Cu1 47.82(9) 2_576 2_465 ? C1 N1 Fe1 165.1(3) . . ? N1 C1 Cu1 169.2(3) . 1_656 ? C2 N2 Fe1 167.8(3) . . ? N2 C2 Cu1 165.7(4) . 1_666 ? N2 C2 Cu1 122.2(3) . 2_576 ? Cu1 C2 Cu1 71.06(13) 1_666 2_576 ? C6 N3 C3 116.7(3) . . ? C6 N3 Fe1 117.6(2) . . ? C3 N3 Fe1 125.4(3) . . ? N3 C3 C4 120.9(4) . . ? N3 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 117.9(4) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C6 N4 C5 116.3(3) . . ? C6 N4 Cu1 117.3(3) . . ? C5 N4 Cu1 126.1(3) . . ? N4 C5 C4 121.6(4) . . ? N4 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? N4 C6 N3 126.5(4) . . ? N4 C6 H6 116.7 . . ? N3 C6 H6 116.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 N1 C1 160(100) 2_577 . . . ? N2 Fe1 N1 C1 -115.6(12) . . . . ? N2 Fe1 N1 C1 64.4(12) 2_577 . . . ? N3 Fe1 N1 C1 -24.3(12) . . . . ? N3 Fe1 N1 C1 155.7(12) 2_577 . . . ? Fe1 N1 C1 Cu1 -6(3) . . . 1_656 ? N1 Fe1 N2 C2 143.7(16) . . . . ? N1 Fe1 N2 C2 -36.3(16) 2_577 . . . ? N2 Fe1 N2 C2 -71(100) 2_577 . . . ? N3 Fe1 N2 C2 54.5(16) . . . . ? N3 Fe1 N2 C2 -125.5(16) 2_577 . . . ? Fe1 N2 C2 Cu1 100.9(19) . . . 1_666 ? Fe1 N2 C2 Cu1 -55.3(17) . . . 2_576 ? N1 Fe1 N3 C6 150.9(3) . . . . ? N1 Fe1 N3 C6 -29.1(3) 2_577 . . . ? N2 Fe1 N3 C6 -119.2(3) . . . . ? N2 Fe1 N3 C6 60.8(3) 2_577 . . . ? N3 Fe1 N3 C6 59(100) 2_577 . . . ? N1 Fe1 N3 C3 -22.8(3) . . . . ? N1 Fe1 N3 C3 157.2(3) 2_577 . . . ? N2 Fe1 N3 C3 67.1(3) . . . . ? N2 Fe1 N3 C3 -112.9(3) 2_577 . . . ? N3 Fe1 N3 C3 -114(100) 2_577 . . . ? C6 N3 C3 C4 -0.8(6) . . . . ? Fe1 N3 C3 C4 172.9(3) . . . . ? N3 C3 C4 C5 -0.7(6) . . . . ? C1 Cu1 N4 C6 43.6(3) 1_454 . . . ? C2 Cu1 N4 C6 -97.3(3) 1_444 . . . ? C2 Cu1 N4 C6 150.4(3) 2_576 . . . ? Cu1 Cu1 N4 C6 -162.9(2) 2_465 . . . ? C1 Cu1 N4 C5 -143.1(3) 1_454 . . . ? C2 Cu1 N4 C5 76.0(3) 1_444 . . . ? C2 Cu1 N4 C5 -36.3(3) 2_576 . . . ? Cu1 Cu1 N4 C5 10.4(3) 2_465 . . . ? C6 N4 C5 C4 -0.8(6) . . . . ? Cu1 N4 C5 C4 -174.1(3) . . . . ? C3 C4 C5 N4 1.5(6) . . . . ? C5 N4 C6 N3 -0.8(6) . . . . ? Cu1 N4 C6 N3 173.1(3) . . . . ? C3 N3 C6 N4 1.6(6) . . . . ? Fe1 N3 C6 N4 -172.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.654 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.127