# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_HdmaFe2(H2O)4F6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(F3 Fe H4 O2), C2 H8 N' _chemical_formula_sum 'C2 H16 F6 Fe2 N O4' _chemical_formula_weight 343.86 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, y, -z+1/2' '-x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -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, -y, z-1/2' 'x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z-1/2' 'x+1/2, y+1/2, -z-1/2' _cell_length_a 10.4065(4) _cell_length_b 7.4143(3) _cell_length_c 15.1516(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1169.05(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3814 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 27.66 _exptl_crystal_description parallepiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 2.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.795 _exptl_absorpt_process_details '(SHELX76; Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_reflns_number 10177 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.89 _reflns_number_total 764 _reflns_number_gt 667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0654P)^2^+1.6307P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 764 _refine_ls_number_parameters 51 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.447 _refine_ls_restrained_S_all 1.447 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 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 0.5000 0.5000 0.5000 0.0164(3) Uani 1 4 d S . . Fe2 Fe 0.5000 1.0000 0.5000 0.0163(3) Uani 1 4 d S . . F1 F 0.5000 0.7570(2) 0.54882(17) 0.0236(6) Uani 1 2 d S . . F2 F 0.63082(15) 0.9287(2) 0.41707(11) 0.0272(4) Uani 1 1 d . . . OW1 O 0.36125(18) 0.4262(2) 0.59871(14) 0.0247(5) Uani 1 1 d D . . H1WA H 0.360(4) 0.296(5) 0.600(3) 0.043(10) Uiso 1 1 d D . . H1WB H 0.2821(15) 0.472(4) 0.598(3) 0.049(11) Uiso 1 1 d D . . C1 C 0.3813(7) 0.7462(6) 0.7500 0.0480(14) Uani 1 2 d S . . H1AC H 0.3802 0.8210 0.8014 0.072 Uiso 1 1 d . . . H1BC H 0.3083 0.6695 0.7500 0.072 Uiso 1 2 d S . . N1 N 0.5000 0.6359(7) 0.7500 0.0365(12) Uani 1 4 d S . . H1AN H 0.5000 0.5643 0.7020 0.044 Uiso 0.50 2 calc SPR . . H1BN H 0.5000 0.5643 0.7980 0.044 Uiso 0.50 2 calc SPR . . 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 0.0175(5) 0.0118(5) 0.0200(5) -0.0009(2) 0.000 0.000 Fe2 0.0149(5) 0.0100(5) 0.0239(5) -0.0001(2) 0.000 0.000 F1 0.0333(13) 0.0111(10) 0.0264(13) 0.0005(6) 0.000 0.000 F2 0.0224(8) 0.0202(8) 0.0391(9) -0.0020(6) 0.0104(6) 0.0003(6) OW1 0.0195(9) 0.0186(10) 0.0358(11) 0.0014(7) 0.0059(7) 0.0003(7) C1 0.050(3) 0.058(4) 0.035(3) 0.000 0.000 0.010(2) N1 0.054(3) 0.030(2) 0.025(2) 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 Fe1 F1 2.0442(17) 9_666 ? Fe1 F1 2.0442(17) . ? Fe1 OW1 2.1496(18) . ? Fe1 OW1 2.1496(18) 10_655 ? Fe1 OW1 2.1496(18) 2_566 ? Fe1 OW1 2.1496(19) 9_666 ? Fe2 F2 1.9266(16) . ? Fe2 F2 1.9266(16) 10_655 ? Fe2 F2 1.9266(16) 2_576 ? Fe2 F2 1.9266(16) 9_676 ? Fe2 F1 1.9474(17) . ? Fe2 F1 1.9474(17) 9_676 ? OW1 H1WA 0.96(4) . ? OW1 H1WB 0.892(10) . ? C1 N1 1.481(7) . ? C1 H1AC 0.960 . ? C1 H1BC 0.950 . ? N1 C1 1.481(7) 10_655 ? N1 H1AN 0.9000 . ? N1 H1BN 0.9000 . ? 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 F1 Fe1 F1 180.0 9_666 . ? F1 Fe1 OW1 90.83(7) 9_666 . ? F1 Fe1 OW1 89.17(7) . . ? F1 Fe1 OW1 90.83(7) 9_666 10_655 ? F1 Fe1 OW1 89.17(7) . 10_655 ? OW1 Fe1 OW1 84.40(11) . 10_655 ? F1 Fe1 OW1 89.17(7) 9_666 2_566 ? F1 Fe1 OW1 90.83(7) . 2_566 ? OW1 Fe1 OW1 95.60(11) . 2_566 ? OW1 Fe1 OW1 180.0 10_655 2_566 ? F1 Fe1 OW1 89.17(7) 9_666 9_666 ? F1 Fe1 OW1 90.83(7) . 9_666 ? OW1 Fe1 OW1 180.0 . 9_666 ? OW1 Fe1 OW1 95.60(11) 10_655 9_666 ? OW1 Fe1 OW1 84.40(11) 2_566 9_666 ? F2 Fe2 F2 89.92(10) . 10_655 ? F2 Fe2 F2 90.08(10) . 2_576 ? F2 Fe2 F2 180.0 10_655 2_576 ? F2 Fe2 F2 180.00(7) . 9_676 ? F2 Fe2 F2 90.08(10) 10_655 9_676 ? F2 Fe2 F2 89.92(10) 2_576 9_676 ? F2 Fe2 F1 89.64(7) . . ? F2 Fe2 F1 89.64(7) 10_655 . ? F2 Fe2 F1 90.36(7) 2_576 . ? F2 Fe2 F1 90.36(7) 9_676 . ? F2 Fe2 F1 90.36(7) . 9_676 ? F2 Fe2 F1 90.36(7) 10_655 9_676 ? F2 Fe2 F1 89.64(7) 2_576 9_676 ? F2 Fe2 F1 89.64(7) 9_676 9_676 ? F1 Fe2 F1 180.0 . 9_676 ? Fe2 F1 Fe1 136.47(14) . . ? Fe1 OW1 H1WA 106(2) . . ? Fe1 OW1 H1WB 121(3) . . ? H1WA OW1 H1WB 112(3) . . ? N1 C1 H1AC 109.0 . . ? N1 C1 H1BC 110.0 . . ? H1AC C1 H1BC 110.0 . . ? C1 N1 C1 112.9(5) . 10_655 ? C1 N1 H1AN 109.0 . . ? C1 N1 H1AN 109.0 10_655 . ? C1 N1 H1BN 109.0 . . ? C1 N1 H1BN 109.0 10_655 . ? H1AN N1 H1BN 107.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.750 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.350 _database_code_depnum_ccdc_archive 'CCDC 948601' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_hdmafe2f6ow6ow _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(F3 Fe H4 O2), 2(C2 H8 N), 2(O0.50)' _chemical_formula_sum 'C4 H32 F12 Fe4 N2 O9' _chemical_formula_weight 703.72 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c m ' _symmetry_space_group_name_Hall '-C 2c 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, y, -z+1/2' '-x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -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, -y, z-1/2' 'x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z-1/2' 'x+1/2, y+1/2, -z-1/2' _cell_length_a 10.4281(5) _cell_length_b 7.4326(4) _cell_length_c 15.3291(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1188.13(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1386 _cell_measurement_theta_min 2.419 _cell_measurement_theta_max 69.36 _exptl_crystal_description parallepiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.205 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.104 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 2.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details '(SHELX76; Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_reflns_number 27586 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 33.36 _reflns_number_total 1239 _reflns_number_gt 991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2007)' _computing_data_reduction 'SAINT-Plus (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0403P)^2^+5.0826P] 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 1239 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.290 _refine_ls_restrained_S_all 1.290 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 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 0.5000 0.5000 0.5000 0.01696(18) Uani 1 4 d S . . Fe2 Fe 0.5000 1.0000 0.5000 0.01608(18) Uani 1 4 d S . . F1 F 0.5000 0.7570(2) 0.54779(17) 0.0231(5) Uani 1 2 d S . . F2 F 0.63035(16) 0.9294(2) 0.41655(12) 0.0291(4) Uani 1 1 d . . . OW1 O 0.36143(18) 0.4269(3) 0.59472(14) 0.0263(4) Uani 1 1 d . . . C1 C -0.1174(7) 1.2331(8) 0.7500 0.0510(15) Uani 1 2 d S . . H1A H -0.1351 1.2728 0.6916 0.076 Uiso 0.50 1 calc PR . . H1B H -0.1040 1.3357 0.7869 0.076 Uiso 0.50 1 calc PR . . H1C H -0.1887 1.1644 0.7714 0.076 Uiso 0.50 1 calc PR . . N1 N 0.0000 1.1187(8) 0.7500 0.0511(17) Uani 1 4 d S . . H2A H 0.0000 1.0476 0.7975 0.061 Uiso 0.50 2 calc SPR . . H2B H 0.0000 1.0476 0.7025 0.061 Uiso 0.50 2 calc SPR . . H1 H 0.3532 0.2943 0.5960 0.061 Uiso 1 1 d R . . H2 H 0.2797 0.4486 0.5924 0.061 Uiso 1 1 d R . . OW2 O 0.0000 0.7109(8) 0.7500 0.070(5) Uani 0.50 4 d SPR . . 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 0.0161(3) 0.0123(3) 0.0225(3) -0.0008(2) 0.000 0.000 Fe2 0.0145(3) 0.0108(3) 0.0229(3) -0.0004(2) 0.000 0.000 F1 0.0324(12) 0.0116(8) 0.0253(10) 0.0007(8) 0.000 0.000 F2 0.0255(8) 0.0216(7) 0.0403(9) -0.0020(7) 0.0105(7) -0.0017(6) OW1 0.0197(8) 0.0193(8) 0.0398(10) 0.0006(8) 0.0051(8) 0.0018(7) C1 0.051(3) 0.067(4) 0.035(2) 0.000 0.000 0.008(3) N1 0.076(5) 0.046(4) 0.031(3) 0.000 0.000 0.000 OW2 0.136(15) 0.036(6) 0.037(6) 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 Fe1 F1 2.046(2) 9_666 ? Fe1 F1 2.046(2) . ? Fe1 OW1 2.119(2) 10_655 ? Fe1 OW1 2.119(2) 2_566 ? Fe1 OW1 2.119(2) 9_666 ? Fe1 OW1 2.119(2) . ? Fe2 F2 1.9389(16) 10_655 ? Fe2 F2 1.9389(16) 2_576 ? Fe2 F2 1.9389(16) 9_676 ? Fe2 F2 1.9389(16) . ? Fe2 F1 1.949(2) 9_676 ? Fe2 F1 1.949(2) . ? OW1 H1 0.9896 . ? OW1 H2 0.8682 . ? C1 N1 1.491(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? N1 C1 1.491(7) 10 ? N1 H2A 0.9000 . ? N1 H2B 0.9000 . ? 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 F1 Fe1 F1 180.0 9_666 . ? F1 Fe1 OW1 90.33(7) 9_666 10_655 ? F1 Fe1 OW1 89.67(7) . 10_655 ? F1 Fe1 OW1 89.67(7) 9_666 2_566 ? F1 Fe1 OW1 90.33(7) . 2_566 ? OW1 Fe1 OW1 180.0 10_655 2_566 ? F1 Fe1 OW1 89.67(7) 9_666 9_666 ? F1 Fe1 OW1 90.33(7) . 9_666 ? OW1 Fe1 OW1 94.03(11) 10_655 9_666 ? OW1 Fe1 OW1 85.97(11) 2_566 9_666 ? F1 Fe1 OW1 90.33(7) 9_666 . ? F1 Fe1 OW1 89.67(7) . . ? OW1 Fe1 OW1 85.97(11) 10_655 . ? OW1 Fe1 OW1 94.03(11) 2_566 . ? OW1 Fe1 OW1 180.0 9_666 . ? F2 Fe2 F2 180.0 10_655 2_576 ? F2 Fe2 F2 90.98(11) 10_655 9_676 ? F2 Fe2 F2 89.02(11) 2_576 9_676 ? F2 Fe2 F2 89.02(11) 10_655 . ? F2 Fe2 F2 90.98(11) 2_576 . ? F2 Fe2 F2 180.00(9) 9_676 . ? F2 Fe2 F1 90.16(7) 10_655 9_676 ? F2 Fe2 F1 89.84(7) 2_576 9_676 ? F2 Fe2 F1 89.84(7) 9_676 9_676 ? F2 Fe2 F1 90.16(7) . 9_676 ? F2 Fe2 F1 89.84(7) 10_655 . ? F2 Fe2 F1 90.16(7) 2_576 . ? F2 Fe2 F1 90.16(7) 9_676 . ? F2 Fe2 F1 89.84(7) . . ? F1 Fe2 F1 180.0 9_676 . ? Fe2 F1 Fe1 136.94(14) . . ? Fe1 OW1 H1 109.2 . . ? Fe1 OW1 H2 126.4 . . ? H1 OW1 H2 95.8 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 N1 C1 110.5(6) 10 . ? C1 N1 H2A 109.6 10 . ? C1 N1 H2A 109.6 . . ? C1 N1 H2B 109.6 10 . ? C1 N1 H2B 109.6 . . ? H2A N1 H2B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.159 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.174 _database_code_depnum_ccdc_archive 'CCDC 948602' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FeF5Htaz #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C2 H3 F5 Fe2 N3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C2 H3 F5 Fe2 N3' _chemical_formula_weight 275.77 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe -1.134 3.197 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'I m m a' _symmetry_space_group_name_Hall '-I 2b 2' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z x+1/2,-y+1/2,-z+1/2 -x+1/2,y,-z+1/2 -x,-y+1/2,z -x,-y,-z -x+1/2,y+1/2,z+1/2 x+1/2,-y,z+1/2 x,y+1/2,-z x+1/2,y+1/2,z+1/2 x,-y,-z -x,y+1/2,-z -x+1/2,-y,z+1/2 -x+1/2,-y+1/2,-z+1/2 -x,y,z x,-y+1/2,z x+1/2,y,-z+1/2 _cell_length_a 9.1552(3) _cell_length_b 7.4896(2) _cell_length_c 9.4644(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 648.97(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.822 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions _exptl_crystal_colour purple # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _refine_ls_hydrogen_treatment refxyz _diffrn_ambient_temperature 296(2) _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Panalytical XPERT-PRO' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector ? _diffrn_detector_type ' XCelerator PANanalytical' _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5582 _pd_meas_2theta_range_min 5.11600 _pd_meas_2theta_range_max 99.99300 _pd_meas_2theta_range_inc 0.017001 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 1.5258 _pd_proc_ls_prof_wR_factor 2.0003 _pd_proc_ls_prof_wR_expected 1.8280 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 14.2800 _pd_proc_ls_prof_cwR_factor 8.8686 _pd_proc_ls_prof_cwR_expected 8.1043 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 1.1975 _pd_proc_ls_prof_echi2 1.2381 # Items related to LS refinement _refine_ls_R_I_factor 3.0467 _refine_ls_number_reflns 425 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _reflns_number_total 200 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.9848 _pd_proc_2theta_range_max 99.8618 _pd_proc_2theta_range_inc 0.017001 _pd_proc_wavelength 1.540510 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution ? _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Fe1 0.50000 0.50000 0.50000 0.0139(8) 1.00000 Uiso Fe Fe2 0.75000 0.75000 0.75000 0.0212(8) 1.00000 Uiso Fe F1 0.50000 0.75000 0.4318(5) 0.014(2) 1.00000 Uiso F F2 0.6461(3) 0.5537(4) 0.6367(2) 0.0197(11) 1.00000 Uiso F N1 0.9258(5) 0.75000 0.5845(6) 0.022(3) 1.00000 Uiso N N2 1.00000 0.75000 0.3695(7) 0.022(3) 1.00000 Uiso N C1 0.8845(7) 0.75000 0.4590(9) 0.044(4) 1.00000 Uiso C H1 0.78030 0.75000 0.41930 0.01267 1.00000 Uiso H H2 1.00000 0.75000 0.27110 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 F1 1.9805(15) . ? Fe1 F1 1.9805(15) 5_666 ? Fe1 F2 1.904(2) . ? Fe1 F2 1.904(2) 5_666 ? Fe1 F2 1.904(2) 10_566 ? Fe1 F2 1.904(2) 14_655 ? Fe2 F2 2.053(3) . ? Fe2 F2 2.053(3) 3_656 ? Fe2 F2 2.053(3) 13_666 ? Fe2 F2 2.053(3) 15_565 ? Fe2 N1 2.246(5) . ? Fe2 N1 2.246(5) 3_656 ? N1 N1 1.359(6) 4_765 ? N1 C1 1.247(10) . ? N2 C1 1.355(8) . ? 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 F1 Fe1 F1 89.93(5) . 2_666 ? F1 Fe1 F2 73.90(9) . 3_555 ? F1 Fe1 F2 91.75(13) . 4_666 ? F2 Fe2 F2 89.76(8) . 4_575 ? _refine_diff_density_min -1.95 _database_code_depnum_ccdc_archive 'CCDC 948603' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Fe2F5(taz)(taz-)Hdma _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H5 F5 Fe2 N6 O, C2 H8 N' _chemical_formula_sum 'C6 H13 F5 Fe2 N7 O' _chemical_formula_weight 405.93 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' F F 0.0171 0.0103 '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' _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 8.8392(5) _cell_length_b 9.1948(5) _cell_length_c 9.5877(5) _cell_angle_alpha 82.070(3) _cell_angle_beta 63.699(3) _cell_angle_gamma 89.202(3) _cell_volume 690.91(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4759 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 24.93 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 406 _exptl_absorpt_coefficient_mu 2.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details '(SHELX76; Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_reflns_number 10958 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2409 _reflns_number_gt 2049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2007)' _computing_data_reduction 'SAINT-Plus (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0649P)^2^+0.5129P] 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 2409 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 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 0.32425(7) 0.27136(6) 0.38112(6) 0.01566(19) Uani 1 1 d . . . Fe2 Fe 0.0000 0.0000 0.0000 0.0142(2) Uani 1 2 d S . . Fe3 Fe 0.5000 0.5000 0.0000 0.0155(2) Uani 1 2 d S . . F1 F 0.4751(3) 0.4337(2) 0.2221(2) 0.0223(5) Uani 1 1 d . . . F2 F 0.1494(3) 0.4150(3) 0.4347(3) 0.0260(6) Uani 1 1 d . . . F3 F 0.3709(3) 0.3357(3) 0.5416(3) 0.0275(6) Uani 1 1 d . . . F4 F 0.1617(3) 0.1213(2) 0.5193(2) 0.0247(5) Uani 1 1 d . . . F5 F 0.5015(3) 0.1403(3) 0.3306(3) 0.0293(6) Uani 1 1 d . . . O1 O 0.2102(4) 0.0119(3) -0.2356(3) 0.0261(7) Uani 1 1 d . . . N6 N 0.0976(4) 0.8035(4) 0.0830(4) 0.0193(7) Uani 1 1 d . . . N1 N 0.2656(4) 0.2266(4) 0.1986(4) 0.0197(7) Uani 1 1 d . . . N2 N 0.1536(4) 0.1337(4) 0.0614(4) 0.0211(7) Uani 1 1 d . . . N3 N 0.3285(4) 0.3105(4) 0.0520(4) 0.0199(7) Uani 1 1 d . . . N4 N 0.2846(4) 0.6418(4) 0.0915(4) 0.0238(8) Uani 1 1 d . . . N5 N 0.1320(4) 0.6079(4) 0.2177(4) 0.0225(8) Uani 1 1 d . . . H5 H 0.1092 0.5340 0.2907 0.027 Uiso 1 1 calc R . . N7 N 0.3087(5) 0.6561(4) 0.5018(5) 0.0437(11) Uani 1 1 d . . . H7A H 0.2802 0.5795 0.4675 0.052 Uiso 1 1 calc R . . H7B H 0.4172 0.6484 0.4840 0.052 Uiso 1 1 calc R . . C1 C 0.1631(5) 0.1239(4) 0.1982(4) 0.0213(9) Uani 1 1 d . . . H1 H 0.1035 0.0521 0.2839 0.026 Uiso 1 1 calc R . . C2 C 0.2590(5) 0.2503(4) -0.0243(5) 0.0228(9) Uani 1 1 d . . . H2 H 0.2810 0.2853 -0.1276 0.027 Uiso 1 1 calc R . . C3 C 0.0240(5) 0.7056(4) 0.2111(4) 0.0209(9) Uani 1 1 d . . . H3 H -0.0879 0.7056 0.2859 0.025 Uiso 1 1 calc R . . C4 C 0.2583(4) 0.7608(3) 0.0132(3) 0.0249(10) Uani 1 1 d . . . H4 H 0.3415 0.8103 -0.0804 0.030 Uiso 1 1 calc R . . C5 C 0.2947(4) 0.7963(3) 0.4075(3) 0.0645(18) Uani 1 1 d R . . H5A H 0.1793 0.8060 0.4259 0.097 Uiso 1 1 calc R . . H5B H 0.3647 0.7938 0.2976 0.097 Uiso 1 1 calc R . . H5C H 0.3312 0.8786 0.4388 0.097 Uiso 1 1 calc R . . C6 C 0.2019(4) 0.6460(3) 0.6726(3) 0.0561(15) Uani 1 1 d R . . H6A H 0.2234 0.7321 0.7088 0.084 Uiso 1 1 calc R . . H6B H 0.2277 0.5603 0.7259 0.084 Uiso 1 1 calc R . . H6C H 0.0850 0.6391 0.6944 0.084 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 0.0176(3) 0.0150(3) 0.0144(3) -0.0010(2) -0.0075(2) 0.0035(2) Fe2 0.0156(4) 0.0126(4) 0.0160(4) -0.0013(3) -0.0087(3) 0.0026(3) Fe3 0.0142(4) 0.0142(4) 0.0171(4) 0.0009(3) -0.0069(3) 0.0019(3) F1 0.0255(12) 0.0219(13) 0.0197(11) 0.0021(9) -0.0115(10) -0.0033(9) F2 0.0264(12) 0.0235(13) 0.0230(11) 0.0002(9) -0.0076(10) 0.0105(10) F3 0.0294(13) 0.0338(14) 0.0242(12) -0.0072(10) -0.0155(11) 0.0009(11) F4 0.0262(12) 0.0243(13) 0.0210(11) 0.0028(9) -0.0098(10) -0.0025(10) F5 0.0253(13) 0.0281(14) 0.0306(13) -0.0007(10) -0.0103(11) 0.0113(11) O1 0.0259(15) 0.0300(17) 0.0176(13) 0.0010(11) -0.0067(12) 0.0071(13) N6 0.0208(17) 0.0168(17) 0.0195(16) -0.0006(13) -0.0088(14) 0.0051(14) N1 0.0219(17) 0.0189(18) 0.0178(16) 0.0008(13) -0.0093(14) -0.0019(14) N2 0.0205(17) 0.0213(18) 0.0226(17) 0.0005(14) -0.0116(14) -0.0034(14) N3 0.0215(17) 0.0197(18) 0.0192(16) 0.0016(13) -0.0109(14) -0.0024(14) N4 0.0183(18) 0.0219(19) 0.0236(17) 0.0047(14) -0.0049(14) 0.0055(14) N5 0.0189(17) 0.0214(18) 0.0204(16) 0.0037(13) -0.0047(14) 0.0031(14) N7 0.040(2) 0.031(2) 0.078(3) -0.023(2) -0.038(2) 0.0106(19) C1 0.026(2) 0.021(2) 0.020(2) -0.0006(16) -0.0131(18) -0.0027(17) C2 0.027(2) 0.025(2) 0.0210(19) -0.0003(16) -0.0148(17) -0.0025(18) C3 0.021(2) 0.020(2) 0.0219(19) -0.0020(16) -0.0097(17) 0.0061(16) C4 0.019(2) 0.024(2) 0.023(2) 0.0033(17) -0.0039(17) 0.0073(17) C5 0.088(5) 0.041(4) 0.093(5) -0.024(3) -0.063(4) 0.021(3) C6 0.043(3) 0.047(4) 0.078(4) -0.018(3) -0.024(3) -0.002(3) _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 F5 1.891(2) . ? Fe1 F4 1.894(2) . ? Fe1 F3 1.925(2) . ? Fe1 F2 1.956(2) . ? Fe1 F1 1.989(2) . ? Fe1 N1 2.123(3) . ? Fe2 N2 2.158(3) . ? Fe2 N2 2.158(3) 2 ? Fe2 O1 2.187(3) . ? Fe2 O1 2.187(3) 2 ? Fe2 N6 2.193(3) 1_545 ? Fe2 N6 2.193(3) 2_565 ? Fe3 F1 2.046(2) 2_665 ? Fe3 F1 2.046(2) . ? Fe3 N3 2.179(3) 2_665 ? Fe3 N3 2.179(3) . ? Fe3 N4 2.205(3) 2_665 ? Fe3 N4 2.205(3) . ? N6 C3 1.322(5) . ? N6 C4 1.354(4) . ? N6 Fe2 2.193(3) 1_565 ? N1 C1 1.319(5) . ? N1 N3 1.378(4) . ? N2 C1 1.341(5) . ? N2 C2 1.342(5) . ? N3 C2 1.319(5) . ? N4 C4 1.317(4) . ? N4 N5 1.357(4) . ? N5 C3 1.317(5) . ? N5 H5 0.8600 . ? N7 C6 1.474(5) . ? N7 C5 1.506(5) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? 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 F5 Fe1 F4 92.16(10) . . ? F5 Fe1 F3 91.92(11) . . ? F4 Fe1 F3 94.90(10) . . ? F5 Fe1 F2 176.73(11) . . ? F4 Fe1 F2 90.13(10) . . ? F3 Fe1 F2 85.56(10) . . ? F5 Fe1 F1 92.32(10) . . ? F4 Fe1 F1 172.42(10) . . ? F3 Fe1 F1 91.05(10) . . ? F2 Fe1 F1 85.65(9) . . ? F5 Fe1 N1 93.63(12) . . ? F4 Fe1 N1 88.86(11) . . ? F3 Fe1 N1 173.17(11) . . ? F2 Fe1 N1 88.75(11) . . ? F1 Fe1 N1 84.76(11) . . ? N2 Fe2 N2 180.0 . 2 ? N2 Fe2 O1 88.63(12) . . ? N2 Fe2 O1 91.37(12) 2 . ? N2 Fe2 O1 91.37(12) . 2 ? N2 Fe2 O1 88.63(12) 2 2 ? O1 Fe2 O1 180.0 . 2 ? N2 Fe2 N6 88.90(12) . 1_545 ? N2 Fe2 N6 91.10(12) 2 1_545 ? O1 Fe2 N6 90.84(11) . 1_545 ? O1 Fe2 N6 89.15(11) 2 1_545 ? N2 Fe2 N6 91.10(12) . 2_565 ? N2 Fe2 N6 88.90(12) 2 2_565 ? O1 Fe2 N6 89.16(11) . 2_565 ? O1 Fe2 N6 90.85(11) 2 2_565 ? N6 Fe2 N6 180.00(19) 1_545 2_565 ? F1 Fe3 F1 180.0 2_665 . ? F1 Fe3 N3 84.28(10) 2_665 2_665 ? F1 Fe3 N3 95.71(10) . 2_665 ? F1 Fe3 N3 95.72(10) 2_665 . ? F1 Fe3 N3 84.29(10) . . ? N3 Fe3 N3 180.0 2_665 . ? F1 Fe3 N4 90.86(11) 2_665 2_665 ? F1 Fe3 N4 89.14(11) . 2_665 ? N3 Fe3 N4 90.72(13) 2_665 2_665 ? N3 Fe3 N4 89.28(13) . 2_665 ? F1 Fe3 N4 89.14(11) 2_665 . ? F1 Fe3 N4 90.86(11) . . ? N3 Fe3 N4 89.28(13) 2_665 . ? N3 Fe3 N4 90.72(13) . . ? N4 Fe3 N4 180.0 2_665 . ? Fe1 F1 Fe3 127.77(12) . . ? C3 N6 C4 103.7(3) . . ? C3 N6 Fe2 130.5(3) . 1_565 ? C4 N6 Fe2 125.7(2) . 1_565 ? C1 N1 N3 105.9(3) . . ? C1 N1 Fe1 130.2(2) . . ? N3 N1 Fe1 123.8(3) . . ? C1 N2 C2 102.2(3) . . ? C1 N2 Fe2 128.5(3) . . ? C2 N2 Fe2 129.3(3) . . ? C2 N3 N1 105.4(3) . . ? C2 N3 Fe3 135.5(3) . . ? N1 N3 Fe3 119.1(2) . . ? C4 N4 N5 103.5(3) . . ? C4 N4 Fe3 126.2(2) . . ? N5 N4 Fe3 128.0(2) . . ? C3 N5 N4 109.5(3) . . ? C3 N5 H5 125.3 . . ? N4 N5 H5 125.3 . . ? C6 N7 C5 114.2(3) . . ? C6 N7 H7A 108.7 . . ? C5 N7 H7A 108.7 . . ? C6 N7 H7B 108.7 . . ? C5 N7 H7B 108.7 . . ? H7A N7 H7B 107.6 . . ? N1 C1 N2 113.1(3) . . ? N1 C1 H1 123.5 . . ? N2 C1 H1 123.5 . . ? N3 C2 N2 113.5(3) . . ? N3 C2 H2 123.3 . . ? N2 C2 H2 123.3 . . ? N5 C3 N6 110.3(3) . . ? N5 C3 H3 124.9 . . ? N6 C3 H3 124.9 . . ? N4 C4 N6 113.0(3) . . ? N4 C4 H4 123.5 . . ? N6 C4 H4 123.5 . . ? N7 C5 H5A 109.5 . . ? N7 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N7 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N7 C6 H6A 109.5 . . ? N7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.716 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.302 _database_code_depnum_ccdc_archive 'CCDC 948604' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Fe2F5(taz-2)Hdma _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 F5 Fe2 N6, C2 H8 N' _chemical_formula_sum 'C6 H12 F5 Fe2 N7' _chemical_formula_weight 388.93 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 17.1968(8) _cell_length_b 8.9793(5) _cell_length_c 8.5318(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1317.44(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 773 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 24.94 _exptl_crystal_description platelets _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 2.262 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details '(SHELX76; Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_reflns_number 15710 _diffrn_reflns_av_R_equivalents 0.1562 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _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 2.66 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1245 _reflns_number_gt 842 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0427P)^2^+6.5535P] 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 1245 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 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 0.42845(7) 0.2500 0.31073(15) 0.0207(4) Uani 1 2 d S . . Fe2 Fe 0.22819(7) 0.2500 0.24328(16) 0.0158(3) Uani 1 2 d S . . F1 F 0.4961(3) 0.2500 0.4773(7) 0.0398(16) Uani 1 2 d S . . F2 F 0.3368(3) 0.2500 0.1618(6) 0.0234(12) Uani 1 2 d S . . F3 F 0.4739(2) 0.4041(4) 0.1949(5) 0.0393(11) Uani 1 1 d . . . F4 F 0.1316(3) 0.2500 0.3356(6) 0.0365(15) Uani 1 2 d S . . N1 N 0.2256(3) -0.0909(6) -0.0997(6) 0.0218(12) Uani 1 1 d . . . N2 N 0.1464(3) -0.0892(6) -0.0683(6) 0.0218(12) Uani 1 1 d . . . N3 N 0.2033(3) 0.0805(6) 0.0811(6) 0.0210(12) Uani 1 1 d . . . C1 C 0.1362(4) 0.0140(7) 0.0400(7) 0.0204(14) Uani 1 1 d . . . H1 H 0.0881 0.0380 0.0830 0.024 Uiso 1 1 calc R . . C2 C 0.2573(3) 0.0127(7) -0.0078(6) 0.0199(14) Uani 1 1 d . . . H2 H 0.3101 0.0353 -0.0055 0.024 Uiso 1 1 calc R . . C4 C 0.4012(3) 0.7500(7) 0.1994(6) 0.048(3) Uani 1 2 d SR . . H4A H 0.4031 0.8358 0.2633 0.072 Uiso 1 1 d R . . H4B H 0.3544 0.7500 0.1407 0.072 Uiso 1 2 d SR . . C3 C 0.5386(3) 0.7500(7) 0.1466(6) 0.052(3) Uani 1 2 d SR . . H3AC H 0.5434 0.7500 0.2458 0.078 Uiso 1 2 d SR . . H3BC H 0.5632 0.6736 0.1125 0.078 Uiso 1 1 d R . . N4 N 0.4624(3) 0.7500(7) 0.1006(6) 0.167(10) Uani 1 2 d SR . . H4AN H 0.4564 0.8302 0.0386 0.200 Uiso 0.50 1 calc PR . . H4BN H 0.4564 0.6698 0.0386 0.200 Uiso 0.50 1 calc PR . . 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 0.0165(7) 0.0179(7) 0.0276(8) 0.000 0.0015(6) 0.000 Fe2 0.0161(7) 0.0120(6) 0.0194(7) 0.000 -0.0005(5) 0.000 F1 0.018(3) 0.060(4) 0.042(4) 0.000 -0.007(2) 0.000 F2 0.019(3) 0.024(3) 0.027(3) 0.000 -0.002(2) 0.000 F3 0.036(2) 0.028(2) 0.054(3) 0.0071(19) 0.016(2) -0.0041(19) F4 0.030(3) 0.048(4) 0.032(3) 0.000 0.005(3) 0.000 N1 0.019(3) 0.014(3) 0.032(3) -0.004(2) 0.001(2) 0.001(2) N2 0.017(3) 0.016(3) 0.032(3) -0.002(2) -0.003(2) -0.002(2) N3 0.018(3) 0.020(3) 0.024(3) -0.005(2) 0.000(2) 0.003(3) C1 0.023(3) 0.014(4) 0.024(4) -0.005(3) 0.003(3) -0.002(3) C2 0.017(3) 0.014(3) 0.029(3) -0.007(3) 0.001(3) -0.004(3) C4 0.062(8) 0.042(7) 0.040(7) 0.000 0.003(6) 0.000 C3 0.061(9) 0.060(9) 0.036(7) 0.000 0.001(6) 0.000 N4 0.055(9) 0.40(3) 0.047(9) 0.000 -0.016(7) 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 Fe1 F1 1.837(6) . ? Fe1 F3 1.871(4) . ? Fe1 F3 1.871(4) 7_565 ? Fe1 F2 2.025(5) . ? Fe1 N2 2.193(5) 4 ? Fe1 N2 2.193(5) 6_666 ? Fe2 F4 1.839(5) . ? Fe2 F2 1.992(5) . ? Fe2 N3 2.101(5) 7_565 ? Fe2 N3 2.101(5) . ? Fe2 N1 2.113(5) 6_666 ? Fe2 N1 2.113(5) 4 ? N1 C2 1.333(7) . ? N1 N2 1.389(7) . ? N2 C1 1.321(8) . ? N3 C2 1.345(7) . ? N3 C1 1.346(7) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C4 N4 1.3486 . ? C4 H4A 0.9438 . ? C4 H4B 0.9478 . ? C3 N4 1.3676 . ? C3 H3AC 0.8502 . ? C3 H3BC 0.8572 . ? N4 H4AN 0.9000 . ? N4 H4BN 0.9000 . ? 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 F1 Fe1 F3 98.27(18) . . ? F1 Fe1 F3 98.27(18) . 7_565 ? F3 Fe1 F3 95.4(2) . 7_565 ? F1 Fe1 F2 168.2(2) . . ? F3 Fe1 F2 89.65(17) . . ? F3 Fe1 F2 89.65(17) 7_565 . ? F1 Fe1 N2 90.5(2) . 4 ? F3 Fe1 N2 168.74(19) . 4 ? F3 Fe1 N2 90.39(18) 7_565 4 ? F2 Fe1 N2 80.69(17) . 4 ? F1 Fe1 N2 90.5(2) . 6_666 ? F3 Fe1 N2 90.39(18) . 6_666 ? F3 Fe1 N2 168.74(19) 7_565 6_666 ? F2 Fe1 N2 80.69(17) . 6_666 ? N2 Fe1 N2 82.4(3) 4 6_666 ? F4 Fe2 F2 175.1(3) . . ? F4 Fe2 N3 95.62(19) . 7_565 ? F2 Fe2 N3 87.77(17) . 7_565 ? F4 Fe2 N3 95.61(19) . . ? F2 Fe2 N3 87.78(17) . . ? N3 Fe2 N3 92.8(3) 7_565 . ? F4 Fe2 N1 93.90(19) . 6_666 ? F2 Fe2 N1 82.49(18) . 6_666 ? N3 Fe2 N1 90.2(2) 7_565 6_666 ? N3 Fe2 N1 169.7(2) . 6_666 ? F4 Fe2 N1 93.90(19) . 4 ? F2 Fe2 N1 82.49(18) . 4 ? N3 Fe2 N1 169.7(2) 7_565 4 ? N3 Fe2 N1 90.2(2) . 4 ? N1 Fe2 N1 85.1(3) 6_666 4 ? Fe2 F2 Fe1 120.7(3) . . ? C2 N1 N2 106.3(5) . . ? C2 N1 Fe2 133.7(4) . 6_655 ? N2 N1 Fe2 119.9(4) . 6_655 ? C1 N2 N1 105.9(5) . . ? C1 N2 Fe1 135.5(4) . 6_655 ? N1 N2 Fe1 118.5(4) . 6_655 ? C2 N3 C1 104.2(5) . . ? C2 N3 Fe2 123.9(4) . . ? C1 N3 Fe2 131.9(4) . . ? N2 C1 N3 112.3(5) . . ? N2 C1 H1 123.9 . . ? N3 C1 H1 123.9 . . ? N1 C2 N3 111.4(5) . . ? N1 C2 H2 124.3 . . ? N3 C2 H2 124.3 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.4 . . ? H4A C4 H4B 109.5 . . ? N4 C3 H3AC 112.2 . . ? N4 C3 H3BC 112.1 . . ? H3AC C3 H3BC 106.9 . . ? C4 N4 C3 124.7 . . ? C4 N4 H4AN 106.2 . . ? C3 N4 H4AN 106.2 . . ? C4 N4 H4BN 106.2 . . ? C3 N4 H4BN 106.2 . . ? H4AN N4 H4BN 106.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.663 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 948605'