# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Ivan Bernal' _publ_contact_author_address ; Department of Chemistry University of Houston Houston TX 77204-5003 UNITED STATES OF AMERICA ; _publ_contact_author_email IBERNAL@UH.EDU _publ_section_title ; 57Fe Mossbauer spectroscopy predicts superstructure for K0.08[CuII(N,N'app)Cl]2[FeIII(CN)6]? 0.92H3O?3.08H2O ; loop_ _publ_author_name 'Ivan Bernal' 'C. Matthias Grunert' 'Philipp Gutlich' 'Joachim Kusz' 'Uday Mukhopadhyay' 'Sergey Reiman ' # Attachment 'BER6_300.CIF' data_ber6_300 _database_code_depnum_ccdc_archive 'CCDC 622279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H63.84 Cl2 Cu2 Fe K0.08 N14 O3.92' _chemical_formula_weight 892.43 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' Cl Cl 0.1484 0.1585 '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' Fe Fe 0.3463 0.8444 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.7976(12) _cell_length_b 14.057(3) _cell_length_c 14.7122(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.180(16) _cell_angle_gamma 90.00 _cell_volume 1964.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 8 _cell_measurement_theta_max 27 _exptl_crystal_description polyhedron _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 937 _exptl_absorpt_coefficient_mu 1.632 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 KUMA Diffraction' _diffrn_measurement_method 'profile data from \q/2\q scan' _diffrn_detector_area_resol_mean 'point detector' _diffrn_standards_number 2 _diffrn_standards_interval_count 60 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1909 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.06 _reflns_number_total 1835 _reflns_number_gt 1400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 KUMA Diffraction' _computing_cell_refinement 'KM4 KUMA Diffraction' _computing_data_reduction 'Omnibus-BLP (E.Galdecka,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek,2003)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1997)' _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. Potassium partially-occupied water site with occupancies of 0.08:0.92 ; _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^)+(0.0401P)^2^+16.6374P] 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 1835 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_restrained_S_all 1.226 _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 Cu2 Cu 0.49713(10) 0.5000 1.18641(6) 0.0313(3) Uani 1 2 d S . . Cl2 Cl 0.3124(3) 0.5000 1.0407(2) 0.0764(9) Uani 1 2 d S . . N1 N 0.4116(5) 0.4130(4) 1.2689(3) 0.0498(14) Uani 1 1 d . . . N2 N 0.6176(5) 0.4000(4) 1.1482(4) 0.0468(13) Uani 1 1 d . . . H1N H 0.6252 0.4143 1.0900 0.056 Uiso 1 1 calc R . . H2N H 0.7043 0.4049 1.1865 0.056 Uiso 1 1 calc R . . C1 C 0.5743(8) 0.2999(5) 1.1480(6) 0.068(2) Uani 1 1 d . . . H11 H 0.6464 0.2599 1.1329 0.082 Uiso 1 1 calc R . . H21 H 0.4880 0.2906 1.0998 0.082 Uiso 1 1 calc R . . C2 C 0.5514(9) 0.2709(6) 1.2399(8) 0.087(3) Uani 1 1 d . . . H12 H 0.6296 0.2939 1.2890 0.105 Uiso 1 1 calc R . . H22 H 0.5519 0.2020 1.2431 0.105 Uiso 1 1 calc R . . C3 C 0.4159(9) 0.3069(6) 1.2590(7) 0.077(3) Uani 1 1 d . . . H13 H 0.3379 0.2872 1.2081 0.093 Uiso 1 1 calc R . . H23 H 0.4034 0.2778 1.3161 0.093 Uiso 1 1 calc R . . C4 C 0.2638(7) 0.4455(6) 1.2559(5) 0.061(2) Uani 1 1 d . . . H14 H 0.2255 0.4217 1.3064 0.074 Uiso 1 1 calc R . . H24 H 0.2063 0.4217 1.1970 0.074 Uiso 1 1 calc R . . C8 C 0.4928(8) 0.4455(6) 1.3625(4) 0.072(3) Uani 1 1 d . . . H18 H 0.5886 0.4217 1.3751 0.087 Uiso 1 1 calc R . . H28 H 0.4498 0.4217 1.4108 0.087 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5000 0.5000 0.0278(4) Uani 1 4 d S . . N3 N -0.2133(6) 0.6554(4) 0.5221(4) 0.0516(14) Uani 1 1 d . . . N4 N 0.1353(9) 0.5000 0.7126(6) 0.063(2) Uani 1 2 d S . . C5 C -0.1333(6) 0.5976(4) 0.5143(4) 0.0350(13) Uani 1 1 d . . . C6 C 0.0833(8) 0.5000 0.6336(6) 0.0385(19) Uani 1 2 d S . . O1W O 0.3481(13) 0.1666(7) 1.4935(9) 0.146(4) Uani 0.92 1 d P A 1 K1 K 0.394(4) 0.186(3) 1.469(2) 0.080(9) Uiso 0.08 1 d P . 2 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 Cu2 0.0290(5) 0.0370(6) 0.0289(5) 0.000 0.0089(4) 0.000 Cl2 0.0767(19) 0.088(2) 0.0666(18) 0.000 0.0211(15) 0.000 N1 0.036(3) 0.074(4) 0.039(3) 0.014(3) 0.010(2) -0.006(3) N2 0.036(3) 0.052(3) 0.051(3) -0.012(3) 0.009(2) 0.002(2) C1 0.051(4) 0.049(4) 0.096(6) -0.015(4) 0.001(4) 0.007(4) C2 0.067(5) 0.047(5) 0.132(9) 0.018(5) -0.006(5) 0.004(4) C3 0.066(5) 0.061(5) 0.096(6) 0.035(5) 0.004(4) -0.024(4) C4 0.037(3) 0.107(6) 0.043(3) 0.015(4) 0.015(3) -0.008(4) C8 0.054(4) 0.129(7) 0.031(3) 0.025(4) 0.006(3) -0.005(4) Fe1 0.0281(8) 0.0276(8) 0.0263(8) 0.000 0.0039(6) 0.000 N3 0.049(3) 0.044(3) 0.062(4) -0.004(3) 0.015(3) 0.005(3) N4 0.064(5) 0.077(6) 0.040(5) 0.000 -0.002(4) 0.000 C5 0.037(3) 0.033(3) 0.033(3) -0.002(2) 0.004(2) -0.003(3) C6 0.034(4) 0.045(5) 0.033(5) 0.000 0.001(4) 0.000 O1W 0.177(11) 0.074(7) 0.196(12) 0.015(7) 0.065(9) 0.046(7) _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 Cu2 N2 2.002(5) . ? Cu2 N2 2.002(5) 6_565 ? Cu2 N1 2.041(5) . ? Cu2 N1 2.041(5) 6_565 ? Cu2 Cl2 2.444(3) . ? Cl2 K1 3.29(4) 7_557 ? Cl2 K1 3.29(4) 4_557 ? N1 C8 1.484(8) . ? N1 C4 1.486(8) . ? N1 C3 1.499(10) . ? N2 C1 1.469(9) . ? C1 C2 1.481(12) . ? C2 C3 1.510(12) . ? C4 C4 1.533(16) 6_565 ? C8 C8 1.533(18) 6_565 ? Fe1 C6 1.935(8) . ? Fe1 C6 1.935(8) 5_566 ? Fe1 C5 1.940(6) 6_565 ? Fe1 C5 1.940(6) 5_566 ? Fe1 C5 1.940(6) 2_556 ? Fe1 C5 1.940(6) . ? N3 C5 1.154(7) . ? N3 K1 2.87(4) 5_567 ? N4 C6 1.148(11) . ? K1 K1 2.05(7) 2_658 ? K1 N3 2.87(4) 5_567 ? K1 Cl2 3.29(4) 7_557 ? 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 Cu2 N2 89.2(3) . 6_565 ? N2 Cu2 N1 95.9(2) . . ? N2 Cu2 N1 160.6(2) 6_565 . ? N2 Cu2 N1 160.6(2) . 6_565 ? N2 Cu2 N1 95.9(2) 6_565 6_565 ? N1 Cu2 N1 73.6(3) . 6_565 ? N2 Cu2 Cl2 96.59(16) . . ? N2 Cu2 Cl2 96.59(16) 6_565 . ? N1 Cu2 Cl2 101.41(16) . . ? N1 Cu2 Cl2 101.41(16) 6_565 . ? Cu2 Cl2 K1 110.7(7) . 7_557 ? Cu2 Cl2 K1 110.7(7) . 4_557 ? K1 Cl2 K1 105.4(14) 7_557 4_557 ? C8 N1 C4 108.0(5) . . ? C8 N1 C3 112.0(6) . . ? C4 N1 C3 110.0(6) . . ? C8 N1 Cu2 99.4(4) . . ? C4 N1 Cu2 105.6(4) . . ? C3 N1 Cu2 120.8(5) . . ? C1 N2 Cu2 118.9(4) . . ? N2 C1 C2 111.7(7) . . ? C1 C2 C3 114.5(7) . . ? N1 C3 C2 113.5(6) . . ? N1 C4 C4 107.9(4) . 6_565 ? N1 C8 C8 107.9(4) . 6_565 ? C6 Fe1 C6 179.999(1) . 5_566 ? C6 Fe1 C5 91.0(2) . 6_565 ? C6 Fe1 C5 89.0(2) 5_566 6_565 ? C6 Fe1 C5 89.0(2) . 5_566 ? C6 Fe1 C5 91.0(2) 5_566 5_566 ? C5 Fe1 C5 90.0(3) 6_565 5_566 ? C6 Fe1 C5 89.0(2) . 2_556 ? C6 Fe1 C5 91.0(2) 5_566 2_556 ? C5 Fe1 C5 180.000(1) 6_565 2_556 ? C5 Fe1 C5 90.0(3) 5_566 2_556 ? C6 Fe1 C5 91.0(2) . . ? C6 Fe1 C5 89.0(2) 5_566 . ? C5 Fe1 C5 90.0(3) 6_565 . ? C5 Fe1 C5 179.999(1) 5_566 . ? C5 Fe1 C5 90.0(3) 2_556 . ? C5 N3 K1 173.4(8) . 5_567 ? N3 C5 Fe1 179.4(6) . . ? N4 C6 Fe1 178.6(8) . . ? K1 K1 N3 123.2(12) 2_658 5_567 ? K1 K1 Cl2 124.2(9) 2_658 7_557 ? N3 K1 Cl2 103.7(10) 5_567 7_557 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.728 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.117 # Attachment 'BER6_250.CIF' data_ber6_250 _database_code_depnum_ccdc_archive 'CCDC 622280' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H63.84 Cl2 Cu2 Fe K0.08 N14 O3.92' _chemical_formula_weight 892.43 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' Cl Cl 0.1484 0.1585 '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' Fe Fe 0.3463 0.8444 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.791(2) _cell_length_b 14.033(5) _cell_length_c 14.675(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.16(2) _cell_angle_gamma 90.00 _cell_volume 1955.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 8 _cell_measurement_theta_max 27 _exptl_crystal_description polyhedron _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 937 _exptl_absorpt_coefficient_mu 1.640 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 KUMA Diffraction' _diffrn_measurement_method 'profile data from \q/2\q scan' _diffrn_detector_area_resol_mean 'point detector' _diffrn_standards_number 2 _diffrn_standards_interval_count 60 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1900 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1828 _reflns_number_gt 1398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 KUMA Diffraction' _computing_cell_refinement 'KM4 KUMA Diffraction' _computing_data_reduction 'Omnibus-BLP (E.Galdecka,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek,2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Potassium partially-occupied water site with occupancies of 0.08:0.92 ; _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^)+(0.0420P)^2^+19.5401P] 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 1828 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _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 Cu2 Cu 0.49703(10) 0.5000 1.18614(7) 0.0278(3) Uani 1 2 d S . . Cl2 Cl 0.3122(3) 0.5000 1.0406(2) 0.0690(8) Uani 1 2 d S . . N1 N 0.4117(5) 0.4125(4) 1.2690(4) 0.0439(13) Uani 1 1 d . . . N2 N 0.6181(5) 0.3999(4) 1.1486(4) 0.0425(13) Uani 1 1 d . . . H1N H 0.6269 0.4145 1.0899 0.051 Uiso 1 1 calc R . . H2N H 0.7055 0.4046 1.1880 0.051 Uiso 1 1 calc R . . C1 C 0.5744(8) 0.2999(5) 1.1478(6) 0.062(2) Uani 1 1 d . . . H11 H 0.6469 0.2594 1.1320 0.075 Uiso 1 1 calc R . . H21 H 0.4869 0.2909 1.0990 0.075 Uiso 1 1 calc R . . C2 C 0.5517(9) 0.2700(6) 1.2394(7) 0.079(3) Uani 1 1 d . . . H12 H 0.6312 0.2924 1.2892 0.094 Uiso 1 1 calc R . . H22 H 0.5513 0.2002 1.2419 0.094 Uiso 1 1 calc R . . C3 C 0.4163(8) 0.3067(6) 1.2592(6) 0.067(2) Uani 1 1 d . . . H13 H 0.3370 0.2867 1.2081 0.081 Uiso 1 1 calc R . . H23 H 0.4041 0.2773 1.3173 0.081 Uiso 1 1 calc R . . C4 C 0.2644(6) 0.4457(6) 1.2560(5) 0.0529(19) Uani 1 1 d . . . H14 H 0.2254 0.4218 1.3071 0.064 Uiso 1 1 calc R . . H24 H 0.2060 0.4218 1.1964 0.064 Uiso 1 1 calc R . . C8 C 0.4927(7) 0.4455(6) 1.3632(4) 0.065(2) Uani 1 1 d . . . H18 H 0.5895 0.4215 1.3762 0.078 Uiso 1 1 calc R . . H28 H 0.4489 0.4215 1.4120 0.078 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5000 0.5000 0.0245(4) Uani 1 4 d S . . N3 N -0.2136(6) 0.6553(4) 0.5220(4) 0.0439(13) Uani 1 1 d . . . N4 N 0.1357(9) 0.5000 0.7133(6) 0.054(2) Uani 1 2 d S . . C5 C -0.1328(6) 0.5977(4) 0.5146(4) 0.0297(12) Uani 1 1 d . . . C6 C 0.0828(8) 0.5000 0.6344(6) 0.0316(18) Uani 1 2 d S . . O1 O 0.3472(13) 0.1666(7) 1.4913(9) 0.140(5) Uani 0.92 1 d P A 1 K1 K 0.399(4) 0.186(3) 1.471(2) 0.073(8) Uiso 0.08 1 d P . 2 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 Cu2 0.0257(5) 0.0321(6) 0.0262(5) 0.000 0.0076(4) 0.000 Cl2 0.0676(18) 0.080(2) 0.0611(18) 0.000 0.0184(14) 0.000 N1 0.034(3) 0.061(4) 0.036(3) 0.015(3) 0.007(2) -0.005(3) N2 0.034(3) 0.045(3) 0.047(3) -0.013(3) 0.006(2) 0.003(2) C1 0.044(4) 0.044(4) 0.088(6) -0.024(4) -0.005(4) 0.005(3) C2 0.059(5) 0.039(4) 0.123(8) 0.022(5) -0.006(5) 0.001(4) C3 0.052(4) 0.057(5) 0.084(6) 0.034(4) 0.000(4) -0.017(4) C4 0.028(3) 0.095(6) 0.037(3) 0.011(4) 0.012(3) -0.008(3) C8 0.045(4) 0.122(7) 0.026(3) 0.021(4) 0.004(3) -0.008(4) Fe1 0.0244(8) 0.0246(8) 0.0228(8) 0.000 0.0026(6) 0.000 N3 0.042(3) 0.040(3) 0.051(3) 0.000(3) 0.013(2) 0.006(3) N4 0.059(5) 0.064(6) 0.033(4) 0.000 -0.002(4) 0.000 C5 0.028(3) 0.029(3) 0.031(3) 0.003(2) 0.005(2) -0.002(2) C6 0.029(4) 0.033(4) 0.031(4) 0.000 0.004(3) 0.000 O1 0.165(11) 0.070(7) 0.197(12) 0.015(7) 0.066(9) 0.057(7) _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 Cu2 N2 2.000(5) 6_565 ? Cu2 N2 2.000(5) . ? Cu2 N1 2.045(5) 6_565 ? Cu2 N1 2.045(5) . ? Cu2 Cl2 2.439(3) . ? Cl2 K1 3.30(4) 4_557 ? Cl2 K1 3.31(4) 7_557 ? N1 C4 1.484(8) . ? N1 C8 1.489(8) . ? N1 C3 1.492(10) . ? N2 C1 1.467(9) . ? C1 C2 1.476(12) . ? C2 C3 1.516(12) . ? C4 C4 1.524(16) 6_565 ? C8 C8 1.530(18) 6_565 ? Fe1 C5 1.937(6) 6_565 ? Fe1 C5 1.937(6) 2_556 ? Fe1 C5 1.937(6) . ? Fe1 C5 1.937(6) 5_566 ? Fe1 C6 1.940(8) 5_566 ? Fe1 C6 1.940(8) . ? N3 C5 1.155(7) . ? N3 K1 2.89(4) 5_567 ? N4 C6 1.148(11) . ? K1 K1 1.96(7) 2_658 ? K1 N3 2.89(4) 5_567 ? K1 Cl2 3.31(4) 7_557 ? 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 Cu2 N2 89.2(3) 6_565 . ? N2 Cu2 N1 95.6(2) 6_565 6_565 ? N2 Cu2 N1 160.3(2) . 6_565 ? N2 Cu2 N1 160.3(2) 6_565 . ? N2 Cu2 N1 95.6(2) . . ? N1 Cu2 N1 73.8(3) 6_565 . ? N2 Cu2 Cl2 97.00(16) 6_565 . ? N2 Cu2 Cl2 97.00(16) . . ? N1 Cu2 Cl2 101.38(16) 6_565 . ? N1 Cu2 Cl2 101.38(16) . . ? Cu2 Cl2 K1 111.5(6) . 4_557 ? Cu2 Cl2 K1 111.5(6) . 7_557 ? K1 Cl2 K1 104.3(14) 4_557 7_557 ? C4 N1 C8 107.5(5) . . ? C4 N1 C3 110.6(6) . . ? C8 N1 C3 112.1(6) . . ? C4 N1 Cu2 105.1(4) . . ? C8 N1 Cu2 99.4(4) . . ? C3 N1 Cu2 120.9(5) . . ? C1 N2 Cu2 118.9(5) . . ? N2 C1 C2 111.9(7) . . ? C1 C2 C3 114.3(7) . . ? N1 C3 C2 113.8(6) . . ? N1 C4 C4 108.3(4) . 6_565 ? N1 C8 C8 108.1(4) . 6_565 ? C5 Fe1 C5 179.998(1) 6_565 2_556 ? C5 Fe1 C5 90.1(3) 6_565 . ? C5 Fe1 C5 89.9(3) 2_556 . ? C5 Fe1 C5 89.9(3) 6_565 5_566 ? C5 Fe1 C5 90.1(3) 2_556 5_566 ? C5 Fe1 C5 179.999(1) . 5_566 ? C5 Fe1 C6 89.3(2) 6_565 5_566 ? C5 Fe1 C6 90.7(2) 2_556 5_566 ? C5 Fe1 C6 89.3(2) . 5_566 ? C5 Fe1 C6 90.7(2) 5_566 5_566 ? C5 Fe1 C6 90.7(2) 6_565 . ? C5 Fe1 C6 89.3(2) 2_556 . ? C5 Fe1 C6 90.7(2) . . ? C5 Fe1 C6 89.3(2) 5_566 . ? C6 Fe1 C6 179.999(2) 5_566 . ? C5 N3 K1 173.3(8) . 5_567 ? N3 C5 Fe1 178.8(5) . . ? N4 C6 Fe1 177.9(8) . . ? K1 K1 N3 124.3(11) 2_658 5_567 ? K1 K1 Cl2 125.3(9) 2_658 7_557 ? N3 K1 Cl2 102.8(9) 5_567 7_557 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.718 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.123 # Attachment 'BER6_200.CIF' data_ber6_200 _database_code_depnum_ccdc_archive 'CCDC 622281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H63.84 Cl2 Cu2 Fe K0.08 N14 O3.92' _chemical_formula_weight 892.43 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' Cl Cl 0.1484 0.1585 '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' Fe Fe 0.3463 0.8444 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.786(2) _cell_length_b 13.998(5) _cell_length_c 14.643(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.17(2) _cell_angle_gamma 90.00 _cell_volume 1944.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 8 _cell_measurement_theta_max 27 _exptl_crystal_description polyhedron _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 937 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 KUMA Diffraction' _diffrn_measurement_method 'profile data from \q/2\q scan' _diffrn_detector_area_resol_mean 'point detector' _diffrn_standards_number 2 _diffrn_standards_interval_count 60 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1661 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.95 _reflns_number_total 1589 _reflns_number_gt 1307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 KUMA Diffraction' _computing_cell_refinement 'KM4 KUMA Diffraction' _computing_data_reduction 'Omnibus-BLP (E.Galdecka,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek,2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Potassium partially-occupied water site with occupancies of 0.08:0.92 ; _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^)+(0.0426P)^2^+21.6022P] 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 1589 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.007 _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 Cu2 Cu 0.49712(9) 0.5000 1.18598(6) 0.0226(3) Uani 1 2 d S . . Cl2 Cl 0.3124(3) 0.5000 1.0406(2) 0.0630(8) Uani 1 2 d S . . N1 N 0.4110(5) 0.4125(4) 1.2685(4) 0.0386(13) Uani 1 1 d . . . N2 N 0.6188(5) 0.3996(4) 1.1485(4) 0.0363(13) Uani 1 1 d . . . H1N H 0.6276 0.4142 1.0890 0.044 Uiso 1 1 calc R . . H2N H 0.7072 0.4045 1.1884 0.044 Uiso 1 1 calc R . . C1 C 0.5746(8) 0.2988(5) 1.1481(6) 0.058(2) Uani 1 1 d . . . H11 H 0.6479 0.2576 1.1325 0.070 Uiso 1 1 calc R . . H21 H 0.4863 0.2896 1.0986 0.070 Uiso 1 1 calc R . . C2 C 0.5515(8) 0.2698(5) 1.2402(7) 0.071(3) Uani 1 1 d . . . H12 H 0.6316 0.2929 1.2906 0.085 Uiso 1 1 calc R . . H22 H 0.5511 0.1991 1.2434 0.085 Uiso 1 1 calc R . . C3 C 0.4154(8) 0.3071(5) 1.2592(6) 0.062(2) Uani 1 1 d . . . H13 H 0.3356 0.2867 1.2072 0.075 Uiso 1 1 calc R A 2 H23 H 0.4023 0.2776 1.3180 0.075 Uiso 1 1 calc R A 2 C4 C 0.2639(7) 0.4451(6) 1.2558(5) 0.0474(18) Uani 1 1 d . . . H14 H 0.2249 0.4208 1.3077 0.057 Uiso 1 1 calc R . . H24 H 0.2048 0.4208 1.1955 0.057 Uiso 1 1 calc R . . C8 C 0.4926(7) 0.4455(6) 1.3629(4) 0.059(2) Uani 1 1 d . . . H18 H 0.5905 0.4212 1.3757 0.071 Uiso 1 1 calc R . . H28 H 0.4487 0.4212 1.4124 0.071 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5000 0.5000 0.0206(4) Uani 1 4 d S . . N3 N -0.2142(5) 0.6551(4) 0.5221(4) 0.0367(12) Uani 1 1 d . . . N4 N 0.1358(8) 0.5000 0.7143(5) 0.044(2) Uani 1 2 d S . . C5 C -0.1338(6) 0.5980(4) 0.5148(4) 0.0273(13) Uani 1 1 d . . . C6 C 0.0838(8) 0.5000 0.6351(6) 0.0272(18) Uani 1 2 d S . . O1W O 0.3490(14) 0.1668(7) 1.4893(10) 0.133(5) Uani 0.92 1 d P B 1 K1 K 0.399(4) 0.188(3) 1.473(3) 0.080(11) Uiso 0.08 1 d P . 2 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 Cu2 0.0206(5) 0.0262(5) 0.0213(5) 0.000 0.0057(4) 0.000 Cl2 0.0627(18) 0.072(2) 0.0553(17) 0.000 0.0167(14) 0.000 N1 0.027(3) 0.053(3) 0.034(3) 0.013(3) 0.004(2) -0.005(3) N2 0.029(3) 0.039(3) 0.039(3) -0.013(3) 0.004(2) 0.003(2) C1 0.037(4) 0.041(4) 0.087(6) -0.026(4) -0.004(4) 0.004(3) C2 0.047(5) 0.034(4) 0.117(8) 0.021(5) -0.011(5) 0.000(3) C3 0.044(4) 0.047(5) 0.085(6) 0.037(4) -0.005(4) -0.014(4) C4 0.028(3) 0.084(5) 0.034(3) 0.014(3) 0.012(3) -0.007(3) C8 0.037(4) 0.113(7) 0.025(3) 0.021(4) 0.001(3) -0.012(4) Fe1 0.0207(8) 0.0199(8) 0.0197(8) 0.000 0.0023(6) 0.000 N3 0.035(3) 0.033(3) 0.043(3) -0.002(2) 0.011(2) 0.003(3) N4 0.046(5) 0.055(5) 0.024(4) 0.000 -0.005(4) 0.000 C5 0.025(3) 0.032(3) 0.023(3) -0.001(3) 0.002(2) -0.004(3) C6 0.023(4) 0.027(4) 0.032(5) 0.000 0.006(4) 0.000 O1W 0.165(12) 0.058(7) 0.179(11) 0.003(7) 0.045(9) 0.050(7) _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 Cu2 N2 2.003(5) 6_565 ? Cu2 N2 2.003(5) . ? Cu2 N1 2.041(5) . ? Cu2 N1 2.041(5) 6_565 ? Cu2 Cl2 2.432(3) . ? Cl2 K1 3.32(4) 7_557 ? Cl2 K1 3.32(4) 4_557 ? N1 C4 1.478(8) . ? N1 C3 1.484(10) . ? N1 C8 1.489(8) . ? N2 C1 1.475(9) . ? C1 C2 1.478(12) . ? C2 C3 1.519(12) . ? C3 K1 3.59(4) . ? C4 C4 1.537(16) 6_565 ? C8 C8 1.527(17) 6_565 ? Fe1 C5 1.945(6) . ? Fe1 C5 1.945(6) 5_566 ? Fe1 C5 1.945(6) 2_556 ? Fe1 C5 1.945(6) 6_565 ? Fe1 C6 1.947(8) 5_566 ? Fe1 C6 1.947(8) . ? N3 C5 1.145(7) . ? N3 K1 2.85(5) 5_567 ? N4 C6 1.148(11) . ? K1 K1 1.94(8) 2_658 ? K1 N3 2.85(5) 5_567 ? K1 Cl2 3.33(4) 7_557 ? 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 Cu2 N2 89.1(3) 6_565 . ? N2 Cu2 N1 160.4(2) 6_565 . ? N2 Cu2 N1 95.8(2) . . ? N2 Cu2 N1 95.8(2) 6_565 6_565 ? N2 Cu2 N1 160.4(2) . 6_565 ? N1 Cu2 N1 73.7(3) . 6_565 ? N2 Cu2 Cl2 97.16(16) 6_565 . ? N2 Cu2 Cl2 97.16(16) . . ? N1 Cu2 Cl2 101.07(15) . . ? N1 Cu2 Cl2 101.07(15) 6_565 . ? Cu2 Cl2 K1 111.8(8) . 7_557 ? Cu2 Cl2 K1 111.8(8) . 4_557 ? K1 Cl2 K1 104.8(17) 7_557 4_557 ? C4 N1 C3 110.1(5) . . ? C4 N1 C8 107.8(5) . . ? C3 N1 C8 111.8(6) . . ? C4 N1 Cu2 105.7(4) . . ? C3 N1 Cu2 121.1(5) . . ? C8 N1 Cu2 99.1(4) . . ? C1 N2 Cu2 118.6(4) . . ? N2 C1 C2 111.7(6) . . ? C1 C2 C3 114.2(6) . . ? N1 C3 C2 113.9(6) . . ? N1 C3 K1 111.9(9) . . ? C2 C3 K1 103.3(9) . . ? N1 C4 C4 108.0(4) . 6_565 ? N1 C8 C8 108.0(4) . 6_565 ? C5 Fe1 C5 179.998(1) . 5_566 ? C5 Fe1 C5 90.3(3) . 2_556 ? C5 Fe1 C5 89.7(3) 5_566 2_556 ? C5 Fe1 C5 89.7(3) . 6_565 ? C5 Fe1 C5 90.3(3) 5_566 6_565 ? C5 Fe1 C5 179.999(1) 2_556 6_565 ? C5 Fe1 C6 89.1(2) . 5_566 ? C5 Fe1 C6 90.9(2) 5_566 5_566 ? C5 Fe1 C6 90.9(2) 2_556 5_566 ? C5 Fe1 C6 89.1(2) 6_565 5_566 ? C5 Fe1 C6 90.9(2) . . ? C5 Fe1 C6 89.1(2) 5_566 . ? C5 Fe1 C6 89.1(2) 2_556 . ? C5 Fe1 C6 90.9(2) 6_565 . ? C6 Fe1 C6 179.998(2) 5_566 . ? C5 N3 K1 173.0(9) . 5_567 ? N3 C5 Fe1 178.8(5) . . ? N4 C6 Fe1 178.7(8) . . ? K1 K1 N3 125.4(14) 2_658 5_567 ? K1 K1 Cl2 125.6(10) 2_658 7_557 ? N3 K1 Cl2 102.8(12) 5_567 7_557 ? K1 K1 C3 95(2) 2_658 . ? N3 K1 C3 80.1(11) 5_567 . ? Cl2 K1 C3 118.3(13) 7_557 . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 0.689 _refine_diff_density_min -1.140 _refine_diff_density_rms 0.113 # Attachment 'BER6_150.CIF' data_ber6_150 _database_code_depnum_ccdc_archive 'CCDC 622282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H63.84 Cl2 Cu2 Fe K0.08 N14 O3.92' _chemical_formula_weight 892.43 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' Cl Cl 0.1484 0.1585 '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' Fe Fe 0.3463 0.8444 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.7836(18) _cell_length_b 13.967(5) _cell_length_c 14.6155(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.11(2) _cell_angle_gamma 90.00 _cell_volume 1936.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 8 _cell_measurement_theta_max 27 _exptl_crystal_description polyhedron _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 937 _exptl_absorpt_coefficient_mu 1.655 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 KUMA Diffraction' _diffrn_measurement_method 'profile data from \q/2\q scan' _diffrn_detector_area_resol_mean 'point detector' _diffrn_standards_number 2 _diffrn_standards_interval_count 60 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1243 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 22.24 _reflns_number_total 1187 _reflns_number_gt 1027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 KUMA Diffraction' _computing_cell_refinement 'KM4 KUMA Diffraction' _computing_data_reduction 'Omnibus-BLP (E.Galdecka,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek,2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Potassium partially-occupied water site with occupancies of 0.08:0.92 ; _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^)+(0.0332P)^2^+24.3035P] 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 1187 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _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 Cu2 Cu 0.49734(10) 0.5000 1.18607(7) 0.0176(4) Uani 1 2 d S . . Cl2 Cl 0.3127(3) 0.5000 1.0409(2) 0.0610(9) Uani 1 2 d S . . N1 N 0.4112(5) 0.4124(4) 1.2689(4) 0.0336(14) Uani 1 1 d . . . N2 N 0.6183(5) 0.3991(4) 1.1486(4) 0.0329(14) Uani 1 1 d . . . H1N H 0.6266 0.4134 1.0887 0.040 Uiso 1 1 calc R . . H2N H 0.7069 0.4042 1.1882 0.040 Uiso 1 1 calc R . . C1 C 0.5743(8) 0.2986(5) 1.1490(7) 0.056(3) Uani 1 1 d . . . H11 H 0.6475 0.2572 1.1333 0.067 Uiso 1 1 calc R . . H21 H 0.4859 0.2893 1.0997 0.067 Uiso 1 1 calc R . . C2 C 0.5514(8) 0.2694(6) 1.2413(7) 0.068(3) Uani 1 1 d . . . H12 H 0.6311 0.2930 1.2918 0.082 Uiso 1 1 calc R . . H22 H 0.5515 0.1987 1.2446 0.082 Uiso 1 1 calc R . . C3 C 0.4155(8) 0.3064(6) 1.2594(6) 0.058(3) Uani 1 1 d . . . H13 H 0.3363 0.2861 1.2069 0.070 Uiso 1 1 calc R . . H23 H 0.4015 0.2767 1.3180 0.070 Uiso 1 1 calc R . . C4 C 0.2634(7) 0.4453(6) 1.2556(5) 0.043(2) Uani 1 1 d . . . H14 H 0.2238 0.4210 1.3073 0.052 Uiso 1 1 calc R . . H24 H 0.2049 0.4210 1.1950 0.052 Uiso 1 1 calc R . . C8 C 0.4922(7) 0.4456(6) 1.3638(5) 0.052(2) Uani 1 1 d . . . H18 H 0.5901 0.4213 1.3770 0.062 Uiso 1 1 calc R . . H28 H 0.4477 0.4213 1.4132 0.062 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5000 0.5000 0.0170(5) Uani 1 4 d S . . N3 N -0.2147(6) 0.6558(4) 0.5220(4) 0.0296(13) Uani 1 1 d . . . N4 N 0.1337(9) 0.5000 0.7147(6) 0.035(2) Uani 1 2 d S . . C5 C -0.1335(6) 0.5972(5) 0.5146(4) 0.0206(14) Uani 1 1 d . . . C6 C 0.0818(9) 0.5000 0.6349(7) 0.022(2) Uani 1 2 d S . . O1W O 0.3451(12) 0.1659(7) 1.4833(9) 0.130(4) Uani 0.92 1 d P A 1 K1 K 0.414(3) 0.183(2) 1.490(2) 0.052(8) Uiso 0.08 1 d P . 2 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 Cu2 0.0156(5) 0.0213(6) 0.0161(6) 0.000 0.0041(4) 0.000 Cl2 0.0591(19) 0.068(2) 0.057(2) 0.000 0.0174(16) 0.000 N1 0.021(3) 0.050(4) 0.027(3) 0.015(3) 0.001(2) -0.008(3) N2 0.023(3) 0.039(4) 0.032(3) -0.015(3) -0.002(2) 0.007(3) C1 0.028(4) 0.029(4) 0.099(8) -0.030(5) -0.008(4) 0.004(3) C2 0.046(5) 0.029(5) 0.109(8) 0.023(5) -0.019(5) -0.005(4) C3 0.037(4) 0.052(5) 0.073(6) 0.039(5) -0.011(4) -0.013(4) C4 0.023(3) 0.083(6) 0.027(4) 0.016(4) 0.013(3) -0.007(4) C8 0.031(4) 0.102(7) 0.020(4) 0.020(4) 0.003(3) -0.008(4) Fe1 0.0176(9) 0.0166(9) 0.0151(11) 0.000 0.0005(7) 0.000 N3 0.031(3) 0.027(3) 0.030(3) -0.001(3) 0.006(3) -0.001(3) N4 0.038(5) 0.037(5) 0.027(6) 0.000 0.001(4) 0.000 C5 0.022(3) 0.023(4) 0.016(4) -0.002(3) 0.003(3) -0.005(3) C6 0.023(5) 0.022(5) 0.021(6) 0.000 0.005(5) 0.000 O1W 0.121(9) 0.068(7) 0.182(11) -0.014(7) 0.002(8) 0.050(7) _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 Cu2 N2 2.000(5) 6_565 ? Cu2 N2 2.000(5) . ? Cu2 N1 2.042(5) 6_565 ? Cu2 N1 2.042(5) . ? Cu2 Cl2 2.428(3) . ? Cl2 K1 3.34(3) 4_557 ? Cl2 K1 3.34(3) 7_557 ? N1 C4 1.484(8) . ? N1 C3 1.489(10) . ? N1 C8 1.494(9) . ? N2 C1 1.469(9) . ? C1 C2 1.477(13) . ? C2 C3 1.509(12) . ? C4 C4 1.527(16) 6_565 ? C8 C8 1.520(17) 6_565 ? Fe1 C5 1.931(7) 2_556 ? Fe1 C5 1.931(7) . ? Fe1 C5 1.931(7) 5_566 ? Fe1 C5 1.931(7) 6_565 ? Fe1 C6 1.939(10) 5_566 ? Fe1 C6 1.939(10) . ? N3 C5 1.165(8) . ? N3 K1 2.95(3) 5_567 ? N4 C6 1.153(12) . ? K1 K1 1.64(5) 2_658 ? K1 N3 2.95(3) 5_567 ? K1 Cl2 3.34(3) 7_557 ? 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 Cu2 N2 89.5(3) 6_565 . ? N2 Cu2 N1 95.6(2) 6_565 6_565 ? N2 Cu2 N1 160.3(2) . 6_565 ? N2 Cu2 N1 160.3(2) 6_565 . ? N2 Cu2 N1 95.6(2) . . ? N1 Cu2 N1 73.6(3) 6_565 . ? N2 Cu2 Cl2 97.16(16) 6_565 . ? N2 Cu2 Cl2 97.17(16) . . ? N1 Cu2 Cl2 101.03(16) 6_565 . ? N1 Cu2 Cl2 101.03(16) . . ? Cu2 Cl2 K1 116.4(6) . 4_557 ? Cu2 Cl2 K1 116.4(6) . 7_557 ? K1 Cl2 K1 100.0(11) 4_557 7_557 ? C4 N1 C3 110.1(6) . . ? C4 N1 C8 107.8(6) . . ? C3 N1 C8 112.0(6) . . ? C4 N1 Cu2 105.4(4) . . ? C3 N1 Cu2 121.0(5) . . ? C8 N1 Cu2 99.4(4) . . ? C1 N2 Cu2 118.6(5) . . ? N2 C1 C2 112.1(7) . . ? C1 C2 C3 113.7(7) . . ? N1 C3 C2 113.7(6) . . ? N1 C4 C4 108.1(4) . 6_565 ? N1 C8 C8 108.1(4) . 6_565 ? C5 Fe1 C5 90.7(3) 2_556 . ? C5 Fe1 C5 89.3(3) 2_556 5_566 ? C5 Fe1 C5 179.997(1) . 5_566 ? C5 Fe1 C5 179.999(1) 2_556 6_565 ? C5 Fe1 C5 89.3(3) . 6_565 ? C5 Fe1 C5 90.7(3) 5_566 6_565 ? C5 Fe1 C6 90.6(2) 2_556 5_566 ? C5 Fe1 C6 89.4(2) . 5_566 ? C5 Fe1 C6 90.6(2) 5_566 5_566 ? C5 Fe1 C6 89.4(2) 6_565 5_566 ? C5 Fe1 C6 89.4(2) 2_556 . ? C5 Fe1 C6 90.6(2) . . ? C5 Fe1 C6 89.4(2) 5_566 . ? C5 Fe1 C6 90.6(2) 6_565 . ? C6 Fe1 C6 179.998(2) 5_566 . ? C5 N3 K1 170.3(8) . 5_567 ? N3 C5 Fe1 179.0(5) . . ? N4 C6 Fe1 178.4(8) . . ? K1 K1 N3 130.2(6) 2_658 5_567 ? K1 K1 Cl2 130.0(6) 2_658 7_557 ? N3 K1 Cl2 99.8(8) 5_567 7_557 ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 22.24 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.665 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.097 data_ber6_90 _database_code_depnum_ccdc_archive 'CCDC 622283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H63.84 Cl2 Cu2 Fe K0.08 N14 O3.92' _chemical_formula_weight 892.43 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' Cl Cl 0.1484 0.1585 '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' Fe Fe 0.3463 0.8444 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.8104(12) _cell_length_b 13.967(3) _cell_length_c 14.6291(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.930(16) _cell_angle_gamma 90.00 _cell_volume 1945.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7572 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 32.64 _exptl_crystal_description polyhedron _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 937 _exptl_absorpt_coefficient_mu 1.648 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KM4_CCD_Sapphire3 _diffrn_measurement_method \q-scan _diffrn_detector_area_resol_mean 16.0328 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9683 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 32.65 _reflns_number_total 3415 _reflns_number_gt 3109 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek,2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Potassium partially-occupied water site with occupancies of 0.08:0.92 ; _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^)+(0.0999P)^2^+9.0157P] 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 3415 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1790 _refine_ls_wR_factor_gt 0.1758 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.004 _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 Cu2 Cu 0.49790(4) 0.5000 1.18656(3) 0.01202(14) Uani 1 2 d S . . Cl2 Cl 0.31288(15) 0.5000 1.04096(10) 0.0391(3) Uani 1 2 d S . . N1 N 0.4113(3) 0.4120(2) 1.2697(2) 0.0327(7) Uani 1 1 d . . . N2 N 0.6202(3) 0.3991(2) 1.1494(2) 0.0319(6) Uani 1 1 d . . . H1N H 0.6287 0.4131 1.0896 0.038 Uiso 1 1 calc R . . H2N H 0.7083 0.4044 1.1889 0.038 Uiso 1 1 calc R . . C1 C 0.5752(4) 0.2975(3) 1.1503(5) 0.070(2) Uani 1 1 d . . . H11 H 0.6482 0.2557 1.1350 0.084 Uiso 1 1 calc R . . H21 H 0.4874 0.2881 1.1010 0.084 Uiso 1 1 calc R . . C2 C 0.5512(5) 0.2686(3) 1.2439(6) 0.076(2) Uani 1 1 d . . . H12 H 0.5509 0.1979 1.2479 0.092 Uiso 1 1 calc R . . H22 H 0.6300 0.2925 1.2945 0.092 Uiso 1 1 calc R . . C3 C 0.4153(4) 0.3065(4) 1.2602(5) 0.0671(19) Uani 1 1 d . . . H13 H 0.3375 0.2865 1.2069 0.081 Uiso 1 1 calc R . . H23 H 0.3989 0.2769 1.3181 0.081 Uiso 1 1 calc R . . C4 C 0.2633(3) 0.4452(4) 1.2564(2) 0.0409(10) Uani 1 1 d . . . H14 H 0.2236 0.4209 1.3081 0.049 Uiso 1 1 calc R . . H24 H 0.2051 0.4209 1.1960 0.049 Uiso 1 1 calc R . . C8 C 0.4910(4) 0.4451(4) 1.3639(2) 0.0543(14) Uani 1 1 d . . . H18 H 0.5886 0.4208 1.3771 0.065 Uiso 1 1 calc R . . H28 H 0.4463 0.4208 1.4132 0.065 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5000 0.5000 0.01186(16) Uani 1 4 d S . . N3 N -0.2153(3) 0.65641(19) 0.52200(18) 0.0235(5) Uani 1 1 d . . . N4 N 0.1332(4) 0.5000 0.7153(2) 0.0257(7) Uani 1 2 d S . . C5 C -0.1340(3) 0.59828(18) 0.51425(17) 0.0165(4) Uani 1 1 d . . . C6 C 0.0822(4) 0.5000 0.6350(2) 0.0174(6) Uani 1 2 d S . . OW1 O 0.3439(10) 0.1661(5) 1.4772(7) 0.148(4) Uani 0.92 1 d P A 1 K1 K 0.4078(15) 0.1821(12) 1.4856(10) 0.044(3) Uiso 0.08 1 d P . 2 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 Cu2 0.0106(2) 0.0142(2) 0.0112(2) 0.000 0.00251(14) 0.000 Cl2 0.0372(6) 0.0460(7) 0.0361(6) 0.000 0.0128(5) 0.000 N1 0.0153(10) 0.0519(18) 0.0269(12) 0.0243(12) -0.0028(9) -0.0090(11) N2 0.0153(10) 0.0397(15) 0.0369(14) -0.0221(12) -0.0012(9) 0.0068(10) C1 0.0228(16) 0.0329(19) 0.131(5) -0.050(3) -0.027(2) 0.0128(15) C2 0.036(2) 0.0218(17) 0.142(6) 0.026(3) -0.034(3) -0.0056(15) C3 0.0288(17) 0.047(2) 0.106(4) 0.054(3) -0.022(2) -0.0202(17) C4 0.0145(11) 0.087(3) 0.0206(12) 0.0196(16) 0.0026(9) -0.0102(15) C8 0.0204(13) 0.118(4) 0.0193(13) 0.0286(19) -0.0043(11) -0.0135(19) Fe1 0.0124(3) 0.0119(3) 0.0097(3) 0.000 -0.0003(2) 0.000 N3 0.0240(11) 0.0224(11) 0.0227(10) -0.0024(9) 0.0028(9) 0.0039(9) N4 0.0256(16) 0.0316(18) 0.0160(14) 0.000 -0.0023(12) 0.000 C5 0.0173(10) 0.0166(10) 0.0142(9) -0.0007(8) 0.0014(8) -0.0005(8) C6 0.0180(15) 0.0174(14) 0.0150(14) 0.000 0.0008(11) 0.000 OW1 0.141(7) 0.060(4) 0.201(9) -0.048(5) -0.041(6) 0.060(4) _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 Cu2 N2 2.008(3) 6_565 ? Cu2 N2 2.008(3) . ? Cu2 N1 2.052(3) . ? Cu2 N1 2.052(2) 6_565 ? Cu2 Cl2 2.4434(16) . ? Cl2 K1 3.302(15) 4_557 ? Cl2 K1 3.302(15) 7_557 ? N1 C3 1.483(7) . ? N1 C8 1.484(5) . ? N1 C4 1.492(5) . ? N2 C1 1.487(6) . ? C1 C2 1.500(10) . ? C2 C3 1.506(9) . ? C4 C4 1.530(10) 6_565 ? C8 C8 1.534(12) 6_565 ? Fe1 C6 1.946(3) . ? Fe1 C6 1.946(3) 5_566 ? Fe1 C5 1.947(3) . ? Fe1 C5 1.947(3) 2_556 ? Fe1 C5 1.947(3) 6_565 ? Fe1 C5 1.947(3) 5_566 ? N3 C5 1.162(4) . ? N3 K1 2.927(16) 5_567 ? N4 C6 1.160(5) . ? K1 K1 1.76(3) 2_658 ? K1 N3 2.927(16) 5_567 ? K1 Cl2 3.302(15) 7_557 ? 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 Cu2 N2 89.1(2) 6_565 . ? N2 Cu2 N1 160.09(13) 6_565 . ? N2 Cu2 N1 95.75(15) . . ? N2 Cu2 N1 95.75(15) 6_565 6_565 ? N2 Cu2 N1 160.09(13) . 6_565 ? N1 Cu2 N1 73.6(2) . 6_565 ? N2 Cu2 Cl2 97.51(8) 6_565 . ? N2 Cu2 Cl2 97.51(8) . . ? N1 Cu2 Cl2 100.97(8) . . ? N1 Cu2 Cl2 100.97(8) 6_565 . ? Cu2 Cl2 K1 115.5(3) . 4_557 ? Cu2 Cl2 K1 115.5(3) . 7_557 ? K1 Cl2 K1 100.8(6) 4_557 7_557 ? C3 N1 C8 112.2(3) . . ? C3 N1 C4 110.1(3) . . ? C8 N1 C4 107.6(3) . . ? C3 N1 Cu2 121.0(3) . . ? C8 N1 Cu2 99.4(2) . . ? C4 N1 Cu2 105.4(2) . . ? C1 N2 Cu2 118.0(3) . . ? N2 C1 C2 112.1(4) . . ? C3 C2 C1 112.9(4) . . ? N1 C3 C2 114.1(3) . . ? N1 C4 C4 108.1(2) . 6_565 ? N1 C8 C8 108.1(2) . 6_565 ? C6 Fe1 C6 180.0 . 5_566 ? C6 Fe1 C5 90.96(11) . . ? C6 Fe1 C5 89.04(11) 5_566 . ? C6 Fe1 C5 89.04(11) . 2_556 ? C6 Fe1 C5 90.96(11) 5_566 2_556 ? C5 Fe1 C5 90.31(15) . 2_556 ? C6 Fe1 C5 90.96(11) . 6_565 ? C6 Fe1 C5 89.04(11) 5_566 6_565 ? C5 Fe1 C5 89.69(15) . 6_565 ? C5 Fe1 C5 180.0 2_556 6_565 ? C6 Fe1 C5 89.04(11) . 5_566 ? C6 Fe1 C5 90.96(11) 5_566 5_566 ? C5 Fe1 C5 179.998(1) . 5_566 ? C5 Fe1 C5 89.69(15) 2_556 5_566 ? C5 Fe1 C5 90.31(15) 6_565 5_566 ? C5 N3 K1 170.4(4) . 5_567 ? N3 C5 Fe1 179.2(2) . . ? N4 C6 Fe1 179.0(4) . . ? K1 K1 N3 128.8(3) 2_658 5_567 ? K1 K1 Cl2 129.5(3) 2_658 7_557 ? N3 K1 Cl2 101.0(4) 5_567 7_557 ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.681 _refine_diff_density_min -2.501 _refine_diff_density_rms 0.160