# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Murray, Keith' _publ_contact_author_email k.s.murray@sci.monash.edu.au _publ_section_title ; Synthesis, structures and spin crossover properties of infinite 3D frameworks of iron(II) containing organodinitrile bridging ligands ; loop_ _publ_author_name K.Murray S.Batten # Attachment '- CIF_for_1.CIF' #============================================================================== data_1_103K #TrackingRef '- CIF_for_1.CIF' _database_code_depnum_ccdc_archive 'CCDC 776735' ############################################################################## # data_1_103K # ############################################################################## #============================================================================# # CHEMICAL DATA # #============================================================================# _chemical_formula_moiety 'C24 H36 Fe N12, 2(Cl4 In)' _chemical_formula_sum 'C24 H36 Cl8 Fe In2 N12 ' _chemical_formula_structural ? _chemical_formula_iupac ? _chemical_formula_weight 1061.74 #=============================================================================# # CRYSTAL DATA # #=============================================================================# _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_int_tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.6031(3) _cell_length_b 14.6031(3) _cell_length_c 36.917(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6817.9(5) _cell_formula_units_Z 6 _cell_measurement_reflns_used 10095 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 24.99 _cell_measurement_temperature 103(2) _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8388 _exptl_absorpt_correction_T_max 0.8388 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' #=============================================================================# # EXPERIMENTAL DATA # #=============================================================================# _diffrn_ambient_temperature 103(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_reflns_number 10095 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_reduction_process ; Lorentz and polarization correction applied ; #=============================================================================# # REFINEMENT DATA # #=============================================================================# _reflns_number_total 2617 _reflns_number_gt 2293 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_number_reflns 2617 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+196.0021P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.845 _refine_diff_density_min -1.509 _refine_diff_density_rms 0.123 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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' _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001) ORTEP (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' #=============================================================================# # ATOMIC COORDINATES AND DISPLANCEMENT PARAMETERS # #=============================================================================# 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 In1 In 0.6667 0.3333 1.01143(3) 0.0485(5) Uani 1 3 d S . . In2 In 1.0000 0.0000 0.82093(3) 0.0369(4) Uani 1 3 d S . . Fe1 Fe 0.3333 -0.3333 0.6667 0.0261(6) Uani 1 6 d S . . Fe2 Fe 0.6667 0.3333 0.8333 0.0212(6) Uani 1 6 d S . . Cl1 Cl 0.7905(4) 0.4996(4) 1.03212(16) 0.182(3) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 0.94904(15) 0.0954(18) Uani 1 3 d S . . Cl3 Cl 1.0000 0.0000 0.88302(18) 0.239(7) Uani 1 3 d S . . Cl4 Cl 0.8536(2) 0.0092(3) 0.80378(15) 0.142(2) Uani 1 1 d . . . N1 N 0.4169(5) -0.2054(5) 0.69754(16) 0.0318(14) Uani 1 1 d . . . N2 N 0.5145(5) 0.0202(5) 0.75256(17) 0.0395(17) Uani 1 1 d . . . N3 N 0.4212(5) -0.0098(5) 0.74709(17) 0.0348(15) Uani 1 1 d . . . N4 N 0.5372(4) 0.2138(4) 0.80116(16) 0.0281(13) Uani 1 1 d . . . C1 C 0.4720(6) -0.1345(6) 0.7145(2) 0.0393(19) Uani 1 1 d . . . C2 C 0.5557(6) -0.0393(6) 0.7333(2) 0.047(2) Uani 1 1 d . . . C3 C 0.3819(5) 0.0553(5) 0.7665(2) 0.040(2) Uani 1 1 d . . . C4 C 0.4709(5) 0.1459(5) 0.78517(19) 0.0296(15) Uani 1 1 d . . . C21 C 0.6099(9) -0.0727(10) 0.7614(3) 0.082(4) Uani 1 1 d . . . H21A H 0.6651 -0.0099 0.7738 0.123 Uiso 1 1 calc R . . H21B H 0.6418 -0.1098 0.7494 0.123 Uiso 1 1 calc R . . H21C H 0.5576 -0.1199 0.7792 0.123 Uiso 1 1 calc R . . C22 C 0.6321(8) 0.0368(7) 0.7039(3) 0.076(3) Uani 1 1 d . . . H22A H 0.6894 0.0996 0.7156 0.114 Uiso 1 1 calc R . . H22B H 0.5932 0.0580 0.6875 0.114 Uiso 1 1 calc R . . H22C H 0.6619 0.0006 0.6900 0.114 Uiso 1 1 calc R . . C31 C 0.3400(7) 0.0977(7) 0.7361(3) 0.051(2) Uani 1 1 d . . . H31A H 0.2814 0.0381 0.7235 0.076 Uiso 1 1 calc R . . H31B H 0.3970 0.1390 0.7189 0.076 Uiso 1 1 calc R . . H31C H 0.3150 0.1427 0.7468 0.076 Uiso 1 1 calc R . . C32 C 0.2993(8) -0.0158(7) 0.7933(3) 0.072(3) Uani 1 1 d . . . H32A H 0.2411 -0.0750 0.7804 0.108 Uiso 1 1 calc R . . H32B H 0.2721 0.0242 0.8062 0.108 Uiso 1 1 calc R . . H32C H 0.3306 -0.0430 0.8106 0.108 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 In1 0.0535(6) 0.0535(6) 0.0386(9) 0.000 0.000 0.0267(3) In2 0.0374(5) 0.0374(5) 0.0359(8) 0.000 0.000 0.0187(2) Fe1 0.0266(8) 0.0266(8) 0.0250(15) 0.000 0.000 0.0133(4) Fe2 0.0216(7) 0.0216(7) 0.0204(14) 0.000 0.000 0.0108(4) Cl1 0.158(4) 0.118(3) 0.232(6) -0.099(4) -0.114(4) 0.041(3) Cl2 0.122(3) 0.122(3) 0.042(3) 0.000 0.000 0.0610(14) Cl3 0.347(11) 0.347(11) 0.024(4) 0.000 0.000 0.173(6) Cl4 0.0490(16) 0.0760(19) 0.297(6) 0.052(3) -0.037(2) 0.0274(15) N1 0.032(3) 0.029(3) 0.035(4) -0.002(3) -0.005(3) 0.016(3) N2 0.027(3) 0.036(3) 0.047(4) -0.017(3) -0.012(3) 0.009(3) N3 0.037(4) 0.027(3) 0.038(4) -0.006(3) -0.003(3) 0.014(3) N4 0.025(3) 0.024(3) 0.032(3) -0.003(3) -0.006(3) 0.010(2) C1 0.041(4) 0.033(4) 0.052(5) 0.001(4) 0.000(4) 0.025(4) C2 0.032(4) 0.042(4) 0.060(6) -0.016(4) -0.005(4) 0.013(3) C3 0.026(4) 0.023(3) 0.067(6) -0.020(4) -0.012(4) 0.008(3) C4 0.031(4) 0.031(4) 0.026(4) 0.000(3) -0.001(3) 0.015(3) C21 0.083(7) 0.104(9) 0.102(9) -0.051(7) -0.049(7) 0.078(7) C22 0.052(6) 0.043(5) 0.105(9) 0.001(5) 0.035(6) 0.003(4) C31 0.045(5) 0.050(5) 0.068(6) -0.026(4) -0.031(4) 0.031(4) C32 0.041(5) 0.045(5) 0.096(8) -0.013(5) 0.023(5) -0.004(4) #=============================================================================# # MOLECULAR GEOMETRY # #=============================================================================# _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 In1 Cl2 2.303(5) . ? In1 Cl1 2.315(4) 3_665 ? In1 Cl1 2.315(4) . ? In1 Cl1 2.315(4) 2_655 ? In2 Cl4 2.297(3) 2_645 ? In2 Cl4 2.297(3) 3_765 ? In2 Cl4 2.297(3) . ? In2 Cl3 2.292(7) . ? Fe1 N1 1.999(6) 2_545 ? Fe1 N1 1.999(6) . ? Fe1 N1 1.999(6) 3_655 ? Fe1 N1 1.999(6) 15_446 ? Fe1 N1 1.999(6) 13_546 ? Fe1 N1 1.999(6) 14_556 ? Fe2 N4 2.175(6) 2_655 ? Fe2 N4 2.175(6) . ? Fe2 N4 2.175(6) 3_665 ? Fe2 N4 2.175(6) 18_546 ? Fe2 N4 2.175(6) 16_656 ? Fe2 N4 2.175(6) 17_556 ? N1 C1 1.131(9) . ? N2 N3 1.221(8) . ? N2 C2 1.465(10) . ? N3 C3 1.514(9) . ? N4 C4 1.144(8) . ? C1 C2 1.486(11) . ? C2 C21 1.526(13) . ? C2 C22 1.556(12) . ? C3 C4 1.481(9) . ? C3 C32 1.503(12) . ? C3 C31 1.547(12) . ? 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 Cl2 In1 Cl1 109.26(17) . 3_665 ? Cl2 In1 Cl1 109.26(17) . . ? Cl1 In1 Cl1 109.68(17) 3_665 . ? Cl2 In1 Cl1 109.26(17) . 2_655 ? Cl1 In1 Cl1 109.68(17) 3_665 2_655 ? Cl1 In1 Cl1 109.68(16) . 2_655 ? Cl4 In2 Cl4 112.71(13) 2_645 3_765 ? Cl4 In2 Cl4 112.71(13) 2_645 . ? Cl4 In2 Cl4 112.71(13) 3_765 . ? Cl4 In2 Cl3 106.00(15) 2_645 . ? Cl4 In2 Cl3 106.00(15) 3_765 . ? Cl4 In2 Cl3 106.00(15) . . ? N1 Fe1 N1 90.7(2) 2_545 . ? N1 Fe1 N1 90.7(2) 2_545 3_655 ? N1 Fe1 N1 90.7(2) . 3_655 ? N1 Fe1 N1 89.3(2) 2_545 15_446 ? N1 Fe1 N1 89.3(2) . 15_446 ? N1 Fe1 N1 179.997(2) 3_655 15_446 ? N1 Fe1 N1 89.3(2) 2_545 13_546 ? N1 Fe1 N1 179.997(1) . 13_546 ? N1 Fe1 N1 89.3(2) 3_655 13_546 ? N1 Fe1 N1 90.7(2) 15_446 13_546 ? N1 Fe1 N1 179.998(2) 2_545 14_556 ? N1 Fe1 N1 89.3(2) . 14_556 ? N1 Fe1 N1 89.3(2) 3_655 14_556 ? N1 Fe1 N1 90.7(2) 15_446 14_556 ? N1 Fe1 N1 90.7(2) 13_546 14_556 ? N4 Fe2 N4 93.0(2) 2_655 . ? N4 Fe2 N4 93.0(2) 2_655 3_665 ? N4 Fe2 N4 93.0(2) . 3_665 ? N4 Fe2 N4 87.0(2) 2_655 18_546 ? N4 Fe2 N4 87.0(2) . 18_546 ? N4 Fe2 N4 179.997(2) 3_665 18_546 ? N4 Fe2 N4 87.0(2) 2_655 16_656 ? N4 Fe2 N4 179.997(1) . 16_656 ? N4 Fe2 N4 87.0(2) 3_665 16_656 ? N4 Fe2 N4 93.0(2) 18_546 16_656 ? N4 Fe2 N4 179.999(3) 2_655 17_556 ? N4 Fe2 N4 87.0(2) . 17_556 ? N4 Fe2 N4 87.0(2) 3_665 17_556 ? N4 Fe2 N4 93.0(2) 18_546 17_556 ? N4 Fe2 N4 93.0(2) 16_656 17_556 ? C1 N1 Fe1 173.6(6) . . ? N3 N2 C2 115.0(6) . . ? N2 N3 C3 113.6(6) . . ? C4 N4 Fe2 175.2(5) . . ? N1 C1 C2 172.3(8) . . ? N2 C2 C1 113.1(6) . . ? N2 C2 C21 107.0(7) . . ? C1 C2 C21 109.5(7) . . ? N2 C2 C22 106.0(7) . . ? C1 C2 C22 107.6(7) . . ? C21 C2 C22 113.7(9) . . ? C4 C3 N3 110.0(6) . . ? C4 C3 C32 110.7(7) . . ? N3 C3 C32 107.6(7) . . ? C4 C3 C31 109.1(6) . . ? N3 C3 C31 105.0(7) . . ? C32 C3 C31 114.2(8) . . ? N4 C4 C3 176.7(8) . . ? #=============================================================================# # Refinement Special Details # #=============================================================================# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The large residual peak (1.845) is located 0.809 Angstroms from Cl3, and is associated with some disorder in the relevant (InCl4)- anion. ; data_1_233K #TrackingRef '- CIF_for_1.CIF' _database_code_depnum_ccdc_archive 'CCDC 776736' ############################################################################## # data_1_233K # ############################################################################## #============================================================================# # CHEMICAL DATA # #============================================================================# _chemical_formula_moiety 'C24 H36 Fe N12, 2(Cl4 In)' _chemical_formula_sum 'C24 H36 Cl8 Fe In2 N12 ' _chemical_formula_structural ? _chemical_formula_iupac ? _chemical_formula_weight 1061.74 #=============================================================================# # CRYSTAL DATA # #=============================================================================# _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_int_tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.7130(10) _cell_length_b 14.7130(10) _cell_length_c 37.436(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7018.1(12) _cell_formula_units_Z 6 _cell_measurement_reflns_used 9731 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 25.00 _cell_measurement_temperature 233(2) _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8428 _exptl_absorpt_correction_T_max 0.8428 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' #=============================================================================# # EXPERIMENTAL DATA # #=============================================================================# _diffrn_ambient_temperature 233(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_reflns_number 9731 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_reduction_process ; Lorentz and polarization correction applied ; #=============================================================================# # REFINEMENT DATA # #=============================================================================# _reflns_number_total 2754 _reflns_number_gt 2269 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_all 1.095 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_number_reflns 2754 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+92.7975P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.727 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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' _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001) ORTEP (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' #=============================================================================# # ATOMIC COORDINATES AND DISPLANCEMENT PARAMETERS # #=============================================================================# 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 In1 In 0.6667 0.3333 1.01009(3) 0.0731(4) Uani 1 3 d S . . In2 In 1.0000 0.0000 0.82073(3) 0.0548(3) Uani 1 3 d S . . Fe1 Fe 0.3333 -0.3333 0.6667 0.0379(5) Uani 1 6 d S . . Fe2 Fe 0.6667 0.3333 0.8333 0.0321(5) Uani 1 6 d S . . Cl1 Cl 0.7920(5) 0.4978(4) 1.02931(19) 0.251(4) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 0.94847(14) 0.125(2) Uani 1 3 d S . . Cl3 Cl 1.0000 0.0000 0.88206(19) 0.285(7) Uani 1 3 d S . . Cl4 Cl 0.8557(3) 0.0098(3) 0.80318(16) 0.168(2) Uani 1 1 d . . . N1 N 0.4202(5) -0.1975(4) 0.69941(16) 0.0478(14) Uani 1 1 d . . . N2 N 0.5189(5) 0.0232(5) 0.75393(18) 0.0592(17) Uani 1 1 d . . . N3 N 0.4267(5) -0.0064(4) 0.74886(16) 0.0481(14) Uani 1 1 d . . . N4 N 0.5394(4) 0.2143(4) 0.80129(15) 0.0414(13) Uani 1 1 d . . . C1 C 0.4765(6) -0.1275(5) 0.7154(2) 0.0467(16) Uani 1 1 d . . . C2 C 0.5602(7) -0.0353(6) 0.7343(3) 0.067(2) Uani 1 1 d . . . C3 C 0.3867(5) 0.0566(5) 0.7671(2) 0.0492(18) Uani 1 1 d . . . C4 C 0.4747(5) 0.1470(5) 0.78621(18) 0.0435(16) Uani 1 1 d . . . C21 C 0.6115(10) -0.0716(11) 0.7618(3) 0.126(6) Uani 1 1 d . . . H21A H 0.6661 -0.0111 0.7743 0.189 Uiso 1 1 calc R . . H21B H 0.6420 -0.1084 0.7498 0.189 Uiso 1 1 calc R . . H21C H 0.5591 -0.1183 0.7788 0.189 Uiso 1 1 calc R . . C22 C 0.6368(8) 0.0409(8) 0.7062(4) 0.126(5) Uani 1 1 d . . . H22A H 0.6924 0.1021 0.7181 0.190 Uiso 1 1 calc R . . H22B H 0.5993 0.0625 0.6902 0.190 Uiso 1 1 calc R . . H22C H 0.6668 0.0061 0.6927 0.190 Uiso 1 1 calc R . . C31 C 0.3436(8) 0.0961(7) 0.7377(3) 0.078(3) Uani 1 1 d . . . H31A H 0.2863 0.0367 0.7256 0.117 Uiso 1 1 calc R . . H31B H 0.3988 0.1370 0.7206 0.117 Uiso 1 1 calc R . . H31C H 0.3182 0.1396 0.7481 0.117 Uiso 1 1 calc R . . C32 C 0.3043(7) -0.0143(7) 0.7936(3) 0.089(3) Uani 1 1 d . . . H32A H 0.2472 -0.0725 0.7810 0.134 Uiso 1 1 calc R . . H32B H 0.2776 0.0250 0.8062 0.134 Uiso 1 1 calc R . . H32C H 0.3351 -0.0411 0.8105 0.134 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 In1 0.0794(5) 0.0794(5) 0.0606(7) 0.000 0.000 0.0397(3) In2 0.0559(4) 0.0559(4) 0.0526(6) 0.000 0.000 0.0280(2) Fe1 0.0400(8) 0.0400(8) 0.0338(12) 0.000 0.000 0.0200(4) Fe2 0.0324(7) 0.0324(7) 0.0315(11) 0.000 0.000 0.0162(3) Cl1 0.238(6) 0.159(4) 0.262(7) -0.086(5) -0.144(6) 0.029(4) Cl2 0.156(3) 0.156(3) 0.063(3) 0.000 0.000 0.0782(17) Cl3 0.403(11) 0.403(11) 0.049(4) 0.000 0.000 0.201(6) Cl4 0.078(2) 0.130(3) 0.306(6) 0.040(3) -0.034(3) 0.060(2) N1 0.053(4) 0.039(3) 0.053(4) -0.010(3) -0.005(3) 0.025(3) N2 0.043(4) 0.049(4) 0.083(5) -0.026(3) -0.021(3) 0.022(3) N3 0.045(3) 0.037(3) 0.056(4) -0.010(3) -0.012(3) 0.016(3) N4 0.045(3) 0.036(3) 0.044(3) -0.007(3) -0.005(3) 0.020(3) C1 0.048(4) 0.038(4) 0.056(4) -0.004(3) -0.005(3) 0.023(3) C2 0.056(5) 0.050(5) 0.091(6) -0.035(4) -0.025(4) 0.024(4) C3 0.040(4) 0.036(4) 0.066(5) -0.018(3) -0.012(3) 0.015(3) C4 0.043(4) 0.040(4) 0.045(4) -0.008(3) -0.003(3) 0.020(3) C21 0.131(10) 0.157(12) 0.147(11) -0.091(10) -0.099(9) 0.115(10) C22 0.066(7) 0.065(7) 0.198(14) -0.022(8) 0.042(8) -0.005(6) C31 0.078(6) 0.070(6) 0.101(7) -0.020(5) -0.041(5) 0.047(5) C32 0.055(5) 0.064(6) 0.119(8) -0.011(6) 0.021(5) 0.008(5) #=============================================================================# # MOLECULAR GEOMETRY # #=============================================================================# _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 In1 Cl2 2.307(5) . ? In1 Cl1 2.305(4) 3_665 ? In1 Cl1 2.305(5) . ? In1 Cl1 2.305(4) 2_655 ? In2 Cl3 2.296(7) . ? In2 Cl4 2.295(3) 2_645 ? In2 Cl4 2.295(3) 3_765 ? In2 Cl4 2.295(3) . ? Fe1 N1 2.139(6) 2_545 ? Fe1 N1 2.139(6) . ? Fe1 N1 2.139(6) 3_655 ? Fe1 N1 2.139(6) 15_446 ? Fe1 N1 2.139(6) 13_546 ? Fe1 N1 2.139(6) 14_556 ? Fe2 N4 2.176(6) 2_655 ? Fe2 N4 2.176(6) . ? Fe2 N4 2.176(6) 3_665 ? Fe2 N4 2.176(6) 18_546 ? Fe2 N4 2.176(6) 16_656 ? Fe2 N4 2.176(6) 17_556 ? N1 C1 1.120(9) . ? N2 N3 1.215(8) . ? N2 C2 1.473(10) . ? N3 C3 1.490(9) . ? N4 C4 1.124(8) . ? C1 C2 1.479(10) . ? C2 C21 1.521(13) . ? C2 C22 1.540(14) . ? C3 C32 1.509(12) . ? C3 C4 1.495(9) . ? C3 C31 1.522(11) . ? 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 Cl2 In1 Cl1 108.2(2) . 3_665 ? Cl2 In1 Cl1 108.2(2) . . ? Cl1 In1 Cl1 110.72(19) 3_665 . ? Cl2 In1 Cl1 108.2(2) . 2_655 ? Cl1 In1 Cl1 110.72(19) 3_665 2_655 ? Cl1 In1 Cl1 110.72(19) . 2_655 ? Cl3 In2 Cl4 106.63(15) . 2_645 ? Cl3 In2 Cl4 106.63(16) . 3_765 ? Cl4 In2 Cl4 112.16(14) 2_645 3_765 ? Cl3 In2 Cl4 106.63(15) . . ? Cl4 In2 Cl4 112.16(14) 2_645 . ? Cl4 In2 Cl4 112.16(14) 3_765 . ? N1 Fe1 N1 90.4(2) 2_545 . ? N1 Fe1 N1 90.4(2) 2_545 3_655 ? N1 Fe1 N1 90.4(2) . 3_655 ? N1 Fe1 N1 89.6(2) 2_545 15_446 ? N1 Fe1 N1 89.6(2) . 15_446 ? N1 Fe1 N1 179.997(2) 3_655 15_446 ? N1 Fe1 N1 89.6(2) 2_545 13_546 ? N1 Fe1 N1 179.998(1) . 13_546 ? N1 Fe1 N1 89.6(2) 3_655 13_546 ? N1 Fe1 N1 90.4(2) 15_446 13_546 ? N1 Fe1 N1 179.998(2) 2_545 14_556 ? N1 Fe1 N1 89.6(2) . 14_556 ? N1 Fe1 N1 89.6(2) 3_655 14_556 ? N1 Fe1 N1 90.4(2) 15_446 14_556 ? N1 Fe1 N1 90.4(2) 13_546 14_556 ? N4 Fe2 N4 92.5(2) 2_655 . ? N4 Fe2 N4 92.5(2) 2_655 3_665 ? N4 Fe2 N4 92.5(2) . 3_665 ? N4 Fe2 N4 87.5(2) 2_655 18_546 ? N4 Fe2 N4 87.5(2) . 18_546 ? N4 Fe2 N4 179.997(2) 3_665 18_546 ? N4 Fe2 N4 87.5(2) 2_655 16_656 ? N4 Fe2 N4 179.997(1) . 16_656 ? N4 Fe2 N4 87.5(2) 3_665 16_656 ? N4 Fe2 N4 92.5(2) 18_546 16_656 ? N4 Fe2 N4 179.998(3) 2_655 17_556 ? N4 Fe2 N4 87.5(2) . 17_556 ? N4 Fe2 N4 87.5(2) 3_665 17_556 ? N4 Fe2 N4 92.5(2) 18_546 17_556 ? N4 Fe2 N4 92.5(2) 16_656 17_556 ? C1 N1 Fe1 171.1(6) . . ? N3 N2 C2 115.2(6) . . ? N2 N3 C3 115.1(6) . . ? C4 N4 Fe2 174.4(6) . . ? N1 C1 C2 173.7(8) . . ? N2 C2 C1 112.2(7) . . ? N2 C2 C21 106.9(7) . . ? C1 C2 C21 109.4(8) . . ? N2 C2 C22 106.3(8) . . ? C1 C2 C22 108.1(8) . . ? C21 C2 C22 114.0(10) . . ? C32 C3 N3 107.5(6) . . ? C32 C3 C4 109.9(7) . . ? N3 C3 C4 109.7(6) . . ? C32 C3 C31 113.3(8) . . ? N3 C3 C31 106.0(6) . . ? C4 C3 C31 110.4(6) . . ? N4 C4 C3 178.4(8) . . ? #=============================================================================# # Refinement Special Details # #=============================================================================# _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. ; # Attachment '- CIF_for_2.CIF' #============================================================================== data_2_103K #TrackingRef '- CIF_for_2.CIF' _database_code_depnum_ccdc_archive 'CCDC 776737' ############################################################################## # data_2_103K # ############################################################################## #============================================================================# # CHEMICAL DATA # #============================================================================# _chemical_formula_moiety 'C24 H36 Fe N12, 2(Cl4 Fe)' _chemical_formula_sum 'C24 H36 Cl8 Fe3 N12 ' _chemical_formula_structural ? _chemical_formula_iupac ? _chemical_formula_weight 943.80 #=============================================================================# # CRYSTAL DATA # #=============================================================================# _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_int_tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.4521(2) _cell_length_b 14.4521(2) _cell_length_c 36.3458(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6574.3(2) _cell_formula_units_Z 6 _cell_measurement_reflns_used 14219 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 27.50 _cell_measurement_temperature 103(2) _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2868 _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8230 _exptl_absorpt_correction_T_max 0.8230 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' #=============================================================================# # EXPERIMENTAL DATA # #=============================================================================# _diffrn_ambient_temperature 103(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_reflns_number 14219 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_reduction_process ; Lorentz and polarization correction applied ; #=============================================================================# # REFINEMENT DATA # #=============================================================================# _reflns_number_total 3369 _reflns_number_gt 2878 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_number_reflns 3369 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+30.1099P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.347 _refine_diff_density_min -1.241 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001) ORTEP (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' #=============================================================================# # ATOMIC COORDINATES AND DISPLANCEMENT PARAMETERS # #=============================================================================# 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 0.3333 -0.3333 0.6667 0.01339(16) Uani 1 6 d S . . Fe2 Fe 0.6667 0.3333 0.8333 0.01098(15) Uani 1 6 d S . . Fe3 Fe 0.6667 0.3333 1.009797(17) 0.02229(15) Uani 1 3 d S . . Fe4 Fe 1.0000 0.0000 0.823896(16) 0.01863(14) Uani 1 3 d S . . Cl1 Cl 0.79702(7) 0.48645(6) 1.02917(3) 0.0591(3) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 0.94983(4) 0.0528(4) Uani 1 3 d S . . Cl3 Cl 1.0000 0.0000 0.88380(4) 0.0924(7) Uani 1 3 d S . . Cl4 Cl 0.86164(6) 0.00853(6) 0.80512(3) 0.0537(3) Uani 1 1 d . . . N1 N 0.41835(15) -0.20807(15) 0.69707(5) 0.0177(4) Uani 1 1 d . . . N2 N 0.51274(15) 0.02164(15) 0.75241(5) 0.0209(4) Uani 1 1 d . . . N3 N 0.41758(15) -0.01068(15) 0.74687(5) 0.0187(4) Uani 1 1 d . . . N4 N 0.53323(15) 0.21647(15) 0.80054(5) 0.0180(4) Uani 1 1 d . . . C1 C 0.47359(18) -0.13359(18) 0.71331(6) 0.0181(5) Uani 1 1 d . . . C2 C 0.55702(18) -0.03668(18) 0.73222(7) 0.0210(5) Uani 1 1 d . . . C3 C 0.37736(18) 0.05334(18) 0.76617(7) 0.0199(5) Uani 1 1 d . . . C4 C 0.46623(18) 0.14623(18) 0.78536(6) 0.0181(5) Uani 1 1 d . . . C21 C 0.6151(2) -0.0681(2) 0.76036(8) 0.0336(6) Uani 1 1 d . . . H21A H 0.6706 -0.0039 0.7726 0.050 Uiso 1 1 calc R . . H21B H 0.6481 -0.1044 0.7478 0.050 Uiso 1 1 calc R . . H21C H 0.5639 -0.1163 0.7787 0.050 Uiso 1 1 calc R . . C22 C 0.6319(2) 0.0408(2) 0.70286(8) 0.0331(6) Uani 1 1 d . . . H22A H 0.6896 0.1042 0.7148 0.050 Uiso 1 1 calc R . . H22B H 0.5915 0.0622 0.6867 0.050 Uiso 1 1 calc R . . H22C H 0.6623 0.0056 0.6882 0.050 Uiso 1 1 calc R . . C31 C 0.3293(2) 0.0912(2) 0.73631(8) 0.0309(6) Uani 1 1 d . . . H31A H 0.2704 0.0290 0.7242 0.046 Uiso 1 1 calc R . . H31B H 0.3843 0.1340 0.7181 0.046 Uiso 1 1 calc R . . H31C H 0.3022 0.1347 0.7475 0.046 Uiso 1 1 calc R . . C32 C 0.2941(2) -0.0194(2) 0.79423(8) 0.0340(6) Uani 1 1 d . . . H32A H 0.2349 -0.0796 0.7815 0.051 Uiso 1 1 calc R . . H32B H 0.2671 0.0211 0.8076 0.051 Uiso 1 1 calc R . . H32C H 0.3269 -0.0464 0.8116 0.051 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 0.0134(2) 0.0134(2) 0.0133(4) 0.000 0.000 0.00672(11) Fe2 0.0108(2) 0.0108(2) 0.0114(4) 0.000 0.000 0.00539(11) Fe3 0.02101(19) 0.02101(19) 0.0249(3) 0.000 0.000 0.01051(10) Fe4 0.01959(19) 0.01959(19) 0.0167(3) 0.000 0.000 0.00980(9) Cl1 0.0458(5) 0.0341(4) 0.0793(6) -0.0058(4) -0.0375(5) 0.0064(4) Cl2 0.0672(6) 0.0672(6) 0.0241(6) 0.000 0.000 0.0336(3) Cl3 0.1293(12) 0.1293(12) 0.0187(7) 0.000 0.000 0.0646(6) Cl4 0.0257(4) 0.0381(4) 0.0995(7) 0.0152(4) -0.0083(4) 0.0177(3) N1 0.0179(9) 0.0194(10) 0.0177(9) 0.0012(8) 0.0000(8) 0.0106(8) N2 0.0188(10) 0.0198(10) 0.0252(11) -0.0041(8) -0.0039(8) 0.0103(8) N3 0.0178(9) 0.0167(9) 0.0224(10) -0.0014(8) -0.0019(8) 0.0092(8) N4 0.0176(9) 0.0172(9) 0.0196(10) -0.0027(8) -0.0019(8) 0.0089(8) C1 0.0190(11) 0.0206(11) 0.0198(11) 0.0036(9) 0.0012(9) 0.0136(10) C2 0.0183(11) 0.0203(11) 0.0266(13) -0.0066(9) -0.0052(9) 0.0113(10) C3 0.0167(11) 0.0156(11) 0.0269(12) -0.0062(9) -0.0029(9) 0.0078(9) C4 0.0182(11) 0.0180(11) 0.0206(11) -0.0006(9) 0.0002(9) 0.0111(9) C21 0.0348(15) 0.0405(16) 0.0368(15) -0.0104(12) -0.0150(12) 0.0271(13) C22 0.0221(13) 0.0257(13) 0.0483(17) 0.0005(12) 0.0063(12) 0.0095(11) C31 0.0318(14) 0.0300(14) 0.0387(16) -0.0144(12) -0.0163(12) 0.0212(12) C32 0.0237(13) 0.0248(13) 0.0429(16) -0.0053(12) 0.0079(12) 0.0043(11) #=============================================================================# # MOLECULAR GEOMETRY # #=============================================================================# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.9452(19) 2_545 ? Fe1 N1 1.9452(19) . ? Fe1 N1 1.9452(19) 3_655 ? Fe1 N1 1.9452(19) 15_446 ? Fe1 N1 1.9451(19) 13_546 ? Fe1 N1 1.9451(19) 14_556 ? Fe2 N4 2.1760(19) 2_655 ? Fe2 N4 2.1760(19) . ? Fe2 N4 2.1760(19) 3_665 ? Fe2 N4 2.1760(19) 18_546 ? Fe2 N4 2.1759(19) 16_656 ? Fe2 N4 2.1759(19) 17_556 ? Fe3 Cl2 2.1794(14) . ? Fe3 Cl1 2.1848(8) 3_665 ? Fe3 Cl1 2.1848(8) . ? Fe3 Cl1 2.1848(8) 2_655 ? Fe4 Cl4 2.1739(7) 2_645 ? Fe4 Cl4 2.1739(7) . ? Fe4 Cl4 2.1739(7) 3_765 ? Fe4 Cl3 2.1773(16) . ? N1 C1 1.134(3) . ? N2 N3 1.228(3) . ? N2 C2 1.482(3) . ? N3 C3 1.491(3) . ? N4 C4 1.136(3) . ? C1 C2 1.483(3) . ? C2 C21 1.529(3) . ? C2 C22 1.534(4) . ? C3 C4 1.488(3) . ? C3 C32 1.526(4) . ? C3 C31 1.530(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 90.91(8) 2_545 . ? N1 Fe1 N1 90.91(8) 2_545 3_655 ? N1 Fe1 N1 90.91(8) . 3_655 ? N1 Fe1 N1 89.09(8) 2_545 15_446 ? N1 Fe1 N1 89.09(8) . 15_446 ? N1 Fe1 N1 179.997(1) 3_655 15_446 ? N1 Fe1 N1 89.09(8) 2_545 13_546 ? N1 Fe1 N1 179.997(1) . 13_546 ? N1 Fe1 N1 89.09(8) 3_655 13_546 ? N1 Fe1 N1 90.91(8) 15_446 13_546 ? N1 Fe1 N1 179.998(1) 2_545 14_556 ? N1 Fe1 N1 89.09(8) . 14_556 ? N1 Fe1 N1 89.09(8) 3_655 14_556 ? N1 Fe1 N1 90.91(8) 15_446 14_556 ? N1 Fe1 N1 90.92(8) 13_546 14_556 ? N4 Fe2 N4 92.87(7) 2_655 . ? N4 Fe2 N4 92.87(7) 2_655 3_665 ? N4 Fe2 N4 92.87(7) . 3_665 ? N4 Fe2 N4 87.13(7) 2_655 18_546 ? N4 Fe2 N4 87.13(7) . 18_546 ? N4 Fe2 N4 179.997(1) 3_665 18_546 ? N4 Fe2 N4 87.13(7) 2_655 16_656 ? N4 Fe2 N4 180.0 . 16_656 ? N4 Fe2 N4 87.13(7) 3_665 16_656 ? N4 Fe2 N4 92.87(7) 18_546 16_656 ? N4 Fe2 N4 180.00(6) 2_655 17_556 ? N4 Fe2 N4 87.13(7) . 17_556 ? N4 Fe2 N4 87.13(7) 3_665 17_556 ? N4 Fe2 N4 92.87(7) 18_546 17_556 ? N4 Fe2 N4 92.87(7) 16_656 17_556 ? Cl2 Fe3 Cl1 108.81(3) . 3_665 ? Cl2 Fe3 Cl1 108.81(3) . . ? Cl1 Fe3 Cl1 110.13(3) 3_665 . ? Cl2 Fe3 Cl1 108.81(3) . 2_655 ? Cl1 Fe3 Cl1 110.13(3) 3_665 2_655 ? Cl1 Fe3 Cl1 110.13(3) . 2_655 ? Cl4 Fe4 Cl4 110.62(3) 2_645 . ? Cl4 Fe4 Cl4 110.62(3) 2_645 3_765 ? Cl4 Fe4 Cl4 110.62(3) . 3_765 ? Cl4 Fe4 Cl3 108.30(3) 2_645 . ? Cl4 Fe4 Cl3 108.30(3) . . ? Cl4 Fe4 Cl3 108.30(3) 3_765 . ? C1 N1 Fe1 175.38(19) . . ? N3 N2 C2 115.00(19) . . ? N2 N3 C3 113.39(19) . . ? C4 N4 Fe2 171.35(18) . . ? N1 C1 C2 172.8(2) . . ? N2 C2 C1 112.84(19) . . ? N2 C2 C21 107.2(2) . . ? C1 C2 C21 109.7(2) . . ? N2 C2 C22 106.05(19) . . ? C1 C2 C22 108.1(2) . . ? C21 C2 C22 113.0(2) . . ? C4 C3 N3 110.61(18) . . ? C4 C3 C32 109.6(2) . . ? N3 C3 C32 107.74(19) . . ? C4 C3 C31 110.6(2) . . ? N3 C3 C31 106.01(19) . . ? C32 C3 C31 112.2(2) . . ? N4 C4 C3 178.9(3) . . ? #=============================================================================# # Refinement Special Details # #=============================================================================# _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. ; data_2_233K #TrackingRef '- CIF_for_2.CIF' _database_code_depnum_ccdc_archive 'CCDC 776738' ############################################################################## # data_2_233K # ############################################################################## #============================================================================# # CHEMICAL DATA # #============================================================================# _chemical_formula_moiety 'C24 H36 Fe N12, 2(Cl4 Fe)' _chemical_formula_sum 'C24 H36 Cl8 Fe3 N12 ' _chemical_formula_structural ? _chemical_formula_iupac ? _chemical_formula_weight 943.80 #=============================================================================# # CRYSTAL DATA # #=============================================================================# _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_int_tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.5996(3) _cell_length_b 14.5996(3) _cell_length_c 36.9669(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6823.8(4) _cell_formula_units_Z 6 _cell_measurement_reflns_used 14333 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 27.50 _cell_measurement_temperature 233(2) _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2868 _exptl_absorpt_coefficient_mu 1.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8345 _exptl_absorpt_correction_T_max 0.8345 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' #=============================================================================# # EXPERIMENTAL DATA # #=============================================================================# _diffrn_ambient_temperature 233(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_reflns_number 14333 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_reduction_process ; Lorentz and polarization correction applied ; #=============================================================================# # REFINEMENT DATA # #=============================================================================# _reflns_number_total 3485 _reflns_number_gt 2338 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_number_reflns 3485 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+22.0682P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.768 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001) ORTEP (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' #=============================================================================# # ATOMIC COORDINATES AND DISPLANCEMENT PARAMETERS # #=============================================================================# 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 0.3333 -0.3333 0.6667 0.0274(2) Uani 1 6 d S . . Fe2 Fe 0.6667 0.3333 0.8333 0.0241(2) Uani 1 6 d S . . Fe3 Fe 0.6667 0.3333 1.00790(3) 0.0531(3) Uani 1 3 d S . . Fe4 Fe 1.0000 0.0000 0.82343(2) 0.0453(2) Uani 1 3 d S . . Cl1 Cl 0.79896(15) 0.48157(13) 1.02631(6) 0.1425(8) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 0.94919(6) 0.0993(8) Uani 1 3 d S . . Cl3 Cl 1.0000 0.0000 0.88138(8) 0.230(3) Uani 1 3 d S . . Cl4 Cl 0.86370(11) 0.00710(13) 0.80493(6) 0.1253(7) Uani 1 1 d . . . N1 N 0.4235(2) -0.1970(2) 0.69954(8) 0.0422(7) Uani 1 1 d . . . N2 N 0.5185(2) 0.0270(2) 0.75375(8) 0.0461(7) Uani 1 1 d . . . N3 N 0.4244(2) -0.0062(2) 0.74864(8) 0.0395(6) Uani 1 1 d . . . N4 N 0.5349(2) 0.2178(2) 0.80117(7) 0.0374(6) Uani 1 1 d . . . C1 C 0.4800(3) -0.1251(3) 0.71524(9) 0.0392(8) Uani 1 1 d . . . C2 C 0.5631(3) -0.0299(3) 0.73382(11) 0.0491(9) Uani 1 1 d . . . C3 C 0.3822(2) 0.0549(2) 0.76743(9) 0.0398(8) Uani 1 1 d . . . C4 C 0.4694(3) 0.1480(2) 0.78624(9) 0.0366(7) Uani 1 1 d . . . C21 C 0.6195(4) -0.0614(4) 0.76134(14) 0.0854(17) Uani 1 1 d . . . H21A H 0.6738 0.0014 0.7734 0.128 Uiso 1 1 calc R . . H21B H 0.6518 -0.0970 0.7491 0.128 Uiso 1 1 calc R . . H21C H 0.5689 -0.1087 0.7791 0.128 Uiso 1 1 calc R . . C22 C 0.6372(3) 0.0474(4) 0.70500(14) 0.0828(15) Uani 1 1 d . . . H22A H 0.6936 0.1094 0.7167 0.124 Uiso 1 1 calc R . . H22B H 0.5975 0.0684 0.6894 0.124 Uiso 1 1 calc R . . H22C H 0.6671 0.0131 0.6907 0.124 Uiso 1 1 calc R . . C31 C 0.3334(3) 0.0903(3) 0.73814(12) 0.0639(12) Uani 1 1 d . . . H31A H 0.2761 0.0287 0.7265 0.096 Uiso 1 1 calc R . . H31B H 0.3868 0.1322 0.7203 0.096 Uiso 1 1 calc R . . H31C H 0.3062 0.1325 0.7489 0.096 Uiso 1 1 calc R . . C32 C 0.3013(3) -0.0182(3) 0.79520(13) 0.0723(13) Uani 1 1 d . . . H32A H 0.2432 -0.0774 0.7829 0.108 Uiso 1 1 calc R . . H32B H 0.2747 0.0205 0.8087 0.108 Uiso 1 1 calc R . . H32C H 0.3347 -0.0444 0.8117 0.108 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 0.0270(3) 0.0270(3) 0.0281(5) 0.000 0.000 0.01352(17) Fe2 0.0230(3) 0.0230(3) 0.0262(5) 0.000 0.000 0.01151(15) Fe3 0.0528(4) 0.0528(4) 0.0537(6) 0.000 0.000 0.02642(19) Fe4 0.0460(3) 0.0460(3) 0.0439(5) 0.000 0.000 0.02299(17) Cl1 0.1184(13) 0.0907(11) 0.1616(17) -0.0130(11) -0.0827(13) 0.0097(10) Cl2 0.1212(13) 0.1212(13) 0.0556(12) 0.000 0.000 0.0606(6) Cl3 0.323(4) 0.323(4) 0.0441(16) 0.000 0.000 0.161(2) Cl4 0.0624(8) 0.1007(11) 0.224(2) 0.0297(12) -0.0156(10) 0.0488(8) N1 0.0453(16) 0.0375(15) 0.0441(16) -0.0094(13) -0.0064(13) 0.0209(14) N2 0.0346(16) 0.0401(16) 0.064(2) -0.0201(14) -0.0150(14) 0.0190(13) N3 0.0370(15) 0.0323(14) 0.0487(16) -0.0095(12) -0.0109(13) 0.0169(12) N4 0.0375(15) 0.0332(14) 0.0395(15) -0.0077(12) -0.0050(12) 0.0162(12) C1 0.0432(19) 0.0349(17) 0.0432(19) -0.0046(15) -0.0058(15) 0.0223(16) C2 0.0394(19) 0.0417(19) 0.068(2) -0.0215(18) -0.0159(17) 0.0221(17) C3 0.0335(17) 0.0303(16) 0.051(2) -0.0116(14) -0.0068(15) 0.0128(14) C4 0.0380(17) 0.0348(17) 0.0396(18) -0.0060(14) -0.0052(14) 0.0203(15) C21 0.085(3) 0.101(4) 0.101(4) -0.047(3) -0.055(3) 0.070(3) C22 0.047(2) 0.060(3) 0.127(4) -0.009(3) 0.018(3) 0.016(2) C31 0.063(3) 0.057(2) 0.083(3) -0.025(2) -0.035(2) 0.039(2) C32 0.053(2) 0.052(3) 0.090(3) -0.002(2) 0.018(2) 0.009(2) #=============================================================================# # MOLECULAR GEOMETRY # #=============================================================================# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.133(3) 2_545 ? Fe1 N1 2.133(3) . ? Fe1 N1 2.133(3) 3_655 ? Fe1 N1 2.133(3) 15_446 ? Fe1 N1 2.133(3) 13_546 ? Fe1 N1 2.133(3) 14_556 ? Fe2 N4 2.171(3) 2_655 ? Fe2 N4 2.171(3) . ? Fe2 N4 2.171(3) 3_665 ? Fe2 N4 2.171(3) 18_546 ? Fe2 N4 2.171(3) 16_656 ? Fe2 N4 2.171(3) 17_556 ? Fe3 Cl1 2.1673(15) 3_665 ? Fe3 Cl1 2.1673(15) . ? Fe3 Cl1 2.1673(15) 2_655 ? Fe3 Cl2 2.170(2) . ? Fe4 Cl3 2.142(3) . ? Fe4 Cl4 2.1550(13) 2_645 ? Fe4 Cl4 2.1550(13) . ? Fe4 Cl4 2.1550(13) 3_765 ? N1 C1 1.120(4) . ? N2 N3 1.222(3) . ? N2 C2 1.483(4) . ? N3 C3 1.486(4) . ? N4 C4 1.133(4) . ? C1 C2 1.479(5) . ? C2 C21 1.517(5) . ? C2 C22 1.535(6) . ? C3 C4 1.490(4) . ? C3 C31 1.521(5) . ? C3 C32 1.526(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 90.76(11) 2_545 . ? N1 Fe1 N1 90.76(11) 2_545 3_655 ? N1 Fe1 N1 90.76(11) . 3_655 ? N1 Fe1 N1 89.24(11) 2_545 15_446 ? N1 Fe1 N1 89.24(11) . 15_446 ? N1 Fe1 N1 179.997(1) 3_655 15_446 ? N1 Fe1 N1 89.24(11) 2_545 13_546 ? N1 Fe1 N1 180.0 . 13_546 ? N1 Fe1 N1 89.24(11) 3_655 13_546 ? N1 Fe1 N1 90.76(11) 15_446 13_546 ? N1 Fe1 N1 179.998(1) 2_545 14_556 ? N1 Fe1 N1 89.24(11) . 14_556 ? N1 Fe1 N1 89.24(11) 3_655 14_556 ? N1 Fe1 N1 90.76(11) 15_446 14_556 ? N1 Fe1 N1 90.77(11) 13_546 14_556 ? N4 Fe2 N4 92.88(10) 2_655 . ? N4 Fe2 N4 92.88(10) 2_655 3_665 ? N4 Fe2 N4 92.88(10) . 3_665 ? N4 Fe2 N4 87.11(10) 2_655 18_546 ? N4 Fe2 N4 87.11(10) . 18_546 ? N4 Fe2 N4 179.997(1) 3_665 18_546 ? N4 Fe2 N4 87.11(10) 2_655 16_656 ? N4 Fe2 N4 179.997(1) . 16_656 ? N4 Fe2 N4 87.12(10) 3_665 16_656 ? N4 Fe2 N4 92.89(10) 18_546 16_656 ? N4 Fe2 N4 179.999(1) 2_655 17_556 ? N4 Fe2 N4 87.11(10) . 17_556 ? N4 Fe2 N4 87.12(10) 3_665 17_556 ? N4 Fe2 N4 92.89(10) 18_546 17_556 ? N4 Fe2 N4 92.89(10) 16_656 17_556 ? Cl1 Fe3 Cl1 110.62(6) 3_665 . ? Cl1 Fe3 Cl1 110.62(6) 3_665 2_655 ? Cl1 Fe3 Cl1 110.62(6) . 2_655 ? Cl1 Fe3 Cl2 108.30(6) 3_665 . ? Cl1 Fe3 Cl2 108.30(6) . . ? Cl1 Fe3 Cl2 108.30(6) 2_655 . ? Cl3 Fe4 Cl4 108.50(6) . 2_645 ? Cl3 Fe4 Cl4 108.50(6) . . ? Cl4 Fe4 Cl4 110.42(6) 2_645 . ? Cl3 Fe4 Cl4 108.50(6) . 3_765 ? Cl4 Fe4 Cl4 110.42(6) 2_645 3_765 ? Cl4 Fe4 Cl4 110.42(6) . 3_765 ? C1 N1 Fe1 172.6(3) . . ? N3 N2 C2 115.0(3) . . ? N2 N3 C3 114.3(3) . . ? C4 N4 Fe2 170.8(3) . . ? N1 C1 C2 174.4(4) . . ? C1 C2 N2 111.9(3) . . ? C1 C2 C21 110.0(3) . . ? N2 C2 C21 107.1(3) . . ? C1 C2 C22 108.3(3) . . ? N2 C2 C22 106.2(3) . . ? C21 C2 C22 113.5(4) . . ? N3 C3 C4 110.1(3) . . ? N3 C3 C31 106.0(3) . . ? C4 C3 C31 110.8(3) . . ? N3 C3 C32 107.6(3) . . ? C4 C3 C32 109.5(3) . . ? C31 C3 C32 112.7(3) . . ? N4 C4 C3 178.7(4) . . ? #=============================================================================# # Refinement Special Details # #=============================================================================# _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. ; # Attachment '- CIF_for_2a.CIF' #============================================================================== data_2a_123K #TrackingRef '- CIF_for_2a.CIF' _database_code_depnum_ccdc_archive 'CCDC 776739' ############################################################################## # data_2a_123K # ############################################################################## #============================================================================# # CHEMICAL DATA # #============================================================================# _chemical_name_systematic ? _chemical_formula_moiety 'C16 H28 Fe N8 O2, 2(Cl4 Fe)' _chemical_formula_sum 'C16 H28 Cl8 Fe3 N8 O2' _chemical_formula_structural ? _chemical_formula_iupac ? _chemical_formula_weight 815.61 #=============================================================================# # CRYSTAL DATA # #=============================================================================# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3413(2) _cell_length_b 12.9995(3) _cell_length_c 14.4027(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.4790(10) _cell_angle_gamma 90.00 _cell_volume 1734.07(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 12762 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 123(2) _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.882 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6505 _exptl_absorpt_correction_T_max 0.9118 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' #=============================================================================# # EXPERIMENTAL DATA # #=============================================================================# _diffrn_ambient_temperature 123(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_reflns_number 12762 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measured_fraction_theta_full 0.966 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_reduction_process ; Lorentz and polarization correction applied ; #=============================================================================# # REFINEMENT DATA # #=============================================================================# _reflns_number_total 3843 _reflns_number_gt 3610 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_number_reflns 3843 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+1.2821P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.446 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001) ORTEP (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' #=============================================================================# # ATOMIC COORDINATES AND DISPLANCEMENT PARAMETERS # #=============================================================================# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.0000 0.5000 0.01285(7) Uani 1 2 d S . . Fe2 Fe 0.14282(2) -0.373072(17) 0.253816(16) 0.01656(6) Uani 1 1 d . . . Cl1 Cl 0.06472(6) -0.28625(4) 0.36856(3) 0.03569(12) Uani 1 1 d . . . Cl2 Cl 0.25056(6) -0.27029(4) 0.16660(4) 0.04009(13) Uani 1 1 d . . . Cl3 Cl -0.04170(6) -0.44244(4) 0.17014(4) 0.04181(14) Uani 1 1 d . . . Cl4 Cl 0.30007(5) -0.48702(4) 0.31705(3) 0.03377(12) Uani 1 1 d . . . O1 O 0.10319(16) -0.04462(11) 0.38661(9) 0.0304(3) Uani 1 1 d D . . N1 N 0.17761(15) 0.09870(10) 0.54938(9) 0.0173(3) Uani 1 1 d . . . N2 N 0.37291(15) 0.24981(10) 0.71724(10) 0.0186(3) Uani 1 1 d . . . N3 N 0.30789(15) 0.18147(10) 0.75329(9) 0.0173(3) Uani 1 1 d . . . N4 N 0.40891(15) 0.36595(10) 0.92412(9) 0.0198(3) Uani 1 1 d . . . C1 C 0.25819(17) 0.15995(12) 0.57773(11) 0.0160(3) Uani 1 1 d . . . C2 C 0.36402(18) 0.24083(12) 0.61326(11) 0.0182(3) Uani 1 1 d . . . C3 C 0.32346(18) 0.18528(11) 0.85742(11) 0.0175(3) Uani 1 1 d . . . C4 C 0.37339(18) 0.28827(12) 0.89324(11) 0.0178(3) Uani 1 1 d . . . C21 C 0.51377(19) 0.21112(15) 0.59067(13) 0.0265(4) Uani 1 1 d . . . H21A H 0.5834 0.2644 0.6142 0.040 Uiso 1 1 calc R . . H21B H 0.5115 0.2046 0.5227 0.040 Uiso 1 1 calc R . . H21C H 0.5425 0.1453 0.6206 0.040 Uiso 1 1 calc R . . C22 C 0.3154(2) 0.34555(13) 0.57240(13) 0.0289(4) Uani 1 1 d . . . H22A H 0.3859 0.3981 0.5964 0.043 Uiso 1 1 calc R . . H22B H 0.2208 0.3628 0.5907 0.043 Uiso 1 1 calc R . . H22C H 0.3084 0.3429 0.5040 0.043 Uiso 1 1 calc R . . C31 C 0.1759(2) 0.16156(14) 0.88687(13) 0.0258(4) Uani 1 1 d . . . H31A H 0.1436 0.0937 0.8631 0.039 Uiso 1 1 calc R . . H31B H 0.1063 0.2138 0.8610 0.039 Uiso 1 1 calc R . . H31C H 0.1830 0.1620 0.9554 0.039 Uiso 1 1 calc R . . C32 C 0.43570(19) 0.10339(12) 0.89218(12) 0.0228(4) Uani 1 1 d . . . H32A H 0.4019 0.0358 0.8685 0.034 Uiso 1 1 calc R . . H32B H 0.4495 0.1024 0.9608 0.034 Uiso 1 1 calc R . . H32C H 0.5276 0.1196 0.8695 0.034 Uiso 1 1 calc R . . H1 H 0.118(2) -0.0082(14) 0.3434(12) 0.027 Uiso 1 1 d D . . H2 H 0.098(2) -0.1048(12) 0.3701(14) 0.027 Uiso 1 1 d D . . 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 0.01684(16) 0.01063(14) 0.00992(15) 0.00158(11) -0.00260(12) -0.00362(11) Fe2 0.01925(12) 0.01488(11) 0.01534(12) -0.00196(8) 0.00146(9) -0.00033(8) Cl1 0.0474(3) 0.0352(2) 0.0273(2) -0.00735(19) 0.0157(2) 0.0091(2) Cl2 0.0376(3) 0.0538(3) 0.0296(3) 0.0144(2) 0.0071(2) -0.0142(2) Cl3 0.0411(3) 0.0275(2) 0.0498(3) 0.0012(2) -0.0210(2) -0.0117(2) Cl4 0.0380(3) 0.0290(2) 0.0325(3) 0.00150(19) -0.0025(2) 0.01348(19) O1 0.0428(8) 0.0298(7) 0.0208(7) -0.0008(6) 0.0129(6) -0.0074(6) N1 0.0200(7) 0.0156(6) 0.0150(7) 0.0002(5) -0.0029(5) -0.0019(5) N2 0.0204(7) 0.0178(6) 0.0170(7) -0.0028(5) -0.0004(5) -0.0043(5) N3 0.0211(7) 0.0147(6) 0.0154(7) -0.0026(5) 0.0003(5) -0.0015(5) N4 0.0234(7) 0.0172(7) 0.0168(7) -0.0021(5) -0.0044(6) 0.0042(5) C1 0.0199(8) 0.0159(7) 0.0117(7) 0.0008(6) -0.0003(6) -0.0001(6) C2 0.0222(8) 0.0169(7) 0.0144(8) -0.0026(6) -0.0013(6) -0.0080(6) C3 0.0241(8) 0.0127(7) 0.0150(8) -0.0025(6) -0.0005(6) -0.0019(6) C4 0.0211(8) 0.0177(8) 0.0137(8) 0.0000(6) -0.0014(6) 0.0032(6) C21 0.0220(9) 0.0343(10) 0.0234(9) -0.0049(7) 0.0039(7) -0.0108(7) C22 0.0422(11) 0.0176(8) 0.0244(9) 0.0017(7) -0.0056(8) -0.0071(7) C31 0.0275(9) 0.0252(8) 0.0258(9) -0.0008(7) 0.0075(7) -0.0029(7) C32 0.0297(9) 0.0161(7) 0.0217(9) -0.0002(6) -0.0003(7) 0.0028(7) #=============================================================================# # MOLECULAR GEOMETRY # #=============================================================================# _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 O1 2.0839(14) 3_556 ? Fe1 O1 2.0839(14) . ? Fe1 N1 2.1442(13) 3_556 ? Fe1 N1 2.1442(13) . ? Fe1 N4 2.1710(13) 4_565 ? Fe1 N4 2.1710(13) 2_546 ? Fe2 Cl3 2.1670(5) . ? Fe2 Cl2 2.1692(5) . ? Fe2 Cl4 2.1985(5) . ? Fe2 Cl1 2.2025(5) . ? N1 C1 1.135(2) . ? N2 N3 1.2288(19) . ? N2 C2 1.494(2) . ? N3 C3 1.489(2) . ? N4 C4 1.135(2) . ? N4 Fe1 2.1710(13) 2_556 ? C1 C2 1.487(2) . ? C2 C21 1.527(2) . ? C2 C22 1.528(2) . ? C3 C4 1.488(2) . ? C3 C31 1.526(2) . ? C3 C32 1.532(2) . ? 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 O1 Fe1 O1 180.0 3_556 . ? O1 Fe1 N1 90.55(5) 3_556 3_556 ? O1 Fe1 N1 89.45(5) . 3_556 ? O1 Fe1 N1 89.45(5) 3_556 . ? O1 Fe1 N1 90.55(5) . . ? N1 Fe1 N1 180.00(5) 3_556 . ? O1 Fe1 N4 88.86(6) 3_556 4_565 ? O1 Fe1 N4 91.14(6) . 4_565 ? N1 Fe1 N4 94.46(5) 3_556 4_565 ? N1 Fe1 N4 85.54(5) . 4_565 ? O1 Fe1 N4 91.14(6) 3_556 2_546 ? O1 Fe1 N4 88.86(6) . 2_546 ? N1 Fe1 N4 85.54(5) 3_556 2_546 ? N1 Fe1 N4 94.46(5) . 2_546 ? N4 Fe1 N4 180.0 4_565 2_546 ? Cl3 Fe2 Cl2 109.25(2) . . ? Cl3 Fe2 Cl4 112.97(2) . . ? Cl2 Fe2 Cl4 108.64(2) . . ? Cl3 Fe2 Cl1 108.26(2) . . ? Cl2 Fe2 Cl1 110.05(2) . . ? Cl4 Fe2 Cl1 107.65(2) . . ? C1 N1 Fe1 171.03(13) . . ? N3 N2 C2 113.65(13) . . ? N2 N3 C3 114.38(13) . . ? C4 N4 Fe1 170.57(13) . 2_556 ? N1 C1 C2 179.04(17) . . ? C1 C2 N2 110.36(13) . . ? C1 C2 C21 109.53(14) . . ? N2 C2 C21 107.49(13) . . ? C1 C2 C22 110.26(13) . . ? N2 C2 C22 106.94(13) . . ? C21 C2 C22 112.20(15) . . ? C4 C3 N3 111.37(13) . . ? C4 C3 C31 109.83(14) . . ? N3 C3 C31 107.46(13) . . ? C4 C3 C32 109.98(13) . . ? N3 C3 C32 106.21(13) . . ? C31 C3 C32 111.93(14) . . ? N4 C4 C3 176.95(18) . . ? #=============================================================================# # Hydrogen Bonds # #=============================================================================# loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H2 Cl1 0.817(15) 2.379(16) 3.1683(15) 163(2) . O1 H1 Cl4 0.808(15) 2.542(17) 3.2667(14) 150.0(19) 2 #=============================================================================# # Refinement Special Details # #=============================================================================# _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. ; # Attachment '- CIF_for_3.CIF' #============================================================================== data_3_123K #TrackingRef '- CIF_for_3.CIF' _database_code_depnum_ccdc_archive 'CCDC 776740' ############################################################################## # data_3_123K # ############################################################################## #============================================================================# # CHEMICAL DATA # #============================================================================# _chemical_formula_moiety 'C42 H60 Fe N12, 2(Cl4 In)' _chemical_formula_sum 'C42 H60 Cl8 Fe In2 N12' _chemical_formula_structural ? _chemical_formula_iupac ? _chemical_formula_weight 1302.12 #=============================================================================# # CRYSTAL DATA # #=============================================================================# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9464(5) _cell_length_b 15.9076(7) _cell_length_c 16.1604(7) _cell_angle_alpha 89.592(2) _cell_angle_beta 89.682(2) _cell_angle_gamma 86.288(2) _cell_volume 2808.0(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 41135 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 25.00 _cell_measurement_temperature 123(2) _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9566 _exptl_absorpt_correction_T_max 0.9566 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' #=============================================================================# # EXPERIMENTAL DATA # #=============================================================================# _diffrn_ambient_temperature 123(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_reflns_number 41135 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measured_fraction_theta_full 0.926 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_reduction_process ; Lorentz and polarization correction applied ; #=============================================================================# # REFINEMENT DATA # #=============================================================================# _reflns_number_total 9828 _reflns_number_gt 8105 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_number_reflns 9828 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+4.8836P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.811 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.083 _refine_ls_extinction_method none 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001) ORTEP (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' #=============================================================================# # ATOMIC COORDINATES AND DISPLANCEMENT PARAMETERS # #=============================================================================# 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 In1 In 1.63520(2) 0.605248(16) 0.250329(15) 0.02511(8) Uani 1 1 d . . . In2 In 1.32984(2) 0.929854(14) 0.251505(14) 0.01826(7) Uani 1 1 d . . . Fe1 Fe 0.97332(4) 0.27936(3) 0.24760(2) 0.00882(10) Uani 1 1 d . . . Cl1 Cl 1.52004(11) 0.73175(7) 0.25747(8) 0.0558(3) Uani 1 1 d . . . Cl2 Cl 1.55372(11) 0.50514(9) 0.33741(8) 0.0662(4) Uani 1 1 d . . . Cl3 Cl 1.63876(12) 0.55725(8) 0.11412(6) 0.0546(3) Uani 1 1 d . . . Cl4 Cl 1.83315(9) 0.62178(12) 0.29490(8) 0.0828(5) Uani 1 1 d . . . Cl5 Cl 1.20476(8) 1.05702(5) 0.24964(6) 0.0317(2) Uani 1 1 d . . . Cl6 Cl 1.19475(8) 0.82380(5) 0.22830(5) 0.02525(19) Uani 1 1 d . . . Cl7 Cl 1.46931(8) 0.94823(5) 0.14309(5) 0.02539(19) Uani 1 1 d . . . Cl8 Cl 1.41520(8) 0.92263(5) 0.38469(5) 0.0265(2) Uani 1 1 d . . . N11 N 1.0103(2) 0.20069(16) 0.14052(16) 0.0155(6) Uani 1 1 d . . . N12 N 0.9883(3) 0.02749(17) 0.02612(18) 0.0254(7) Uani 1 1 d . . . N21 N 0.9394(2) 0.35747(16) 0.35440(16) 0.0149(6) Uani 1 1 d . . . N22 N 0.9671(2) 0.48743(16) 0.52769(15) 0.0159(6) Uani 1 1 d . . . N31 N 0.9533(2) 0.16981(16) 0.32284(16) 0.0154(6) Uani 1 1 d . . . N32 N 0.9995(3) 0.03318(16) 0.48014(16) 0.0217(6) Uani 1 1 d . . . N41 N 0.9993(2) 0.38767(16) 0.17369(16) 0.0158(6) Uani 1 1 d . . . N42 N 1.0423(2) 0.52230(16) 0.00743(16) 0.0171(6) Uani 1 1 d . . . N51 N 1.1670(2) 0.27182(15) 0.27730(15) 0.0142(6) Uani 1 1 d . . . N52 N 1.4883(2) 0.26432(16) 0.28773(16) 0.0158(6) Uani 1 1 d . . . N61 N 0.7796(2) 0.28212(15) 0.22095(15) 0.0146(6) Uani 1 1 d . . . N62 N 0.4599(2) 0.26284(16) 0.21458(16) 0.0156(6) Uani 1 1 d . . . C11 C 1.0362(3) 0.1561(2) 0.0869(2) 0.0191(7) Uani 1 1 d . . . C12 C 1.0671(3) 0.1003(2) 0.0142(2) 0.0197(7) Uani 1 1 d . . . C13 C 1.2038(3) 0.0736(2) 0.0138(2) 0.0233(8) Uani 1 1 d . . . H13B H 1.2263 0.0471 0.0676 0.028 Uiso 1 1 calc R . . H13A H 1.2211 0.0312 -0.0300 0.028 Uiso 1 1 calc R . . C14 C 1.2811(3) 0.1475(2) -0.0013(2) 0.0306(9) Uani 1 1 d . . . H14A H 1.3684 0.1272 -0.0041 0.037 Uiso 1 1 calc R . . H14B H 1.2708 0.1870 0.0456 0.037 Uiso 1 1 calc R . . C15 C 1.2460(4) 0.1939(2) -0.0813(2) 0.0363(10) Uani 1 1 d . . . H15B H 1.2947 0.2439 -0.0873 0.044 Uiso 1 1 calc R . . H15A H 1.2650 0.1564 -0.1289 0.044 Uiso 1 1 calc R . . C16 C 1.1110(4) 0.2214(2) -0.0814(2) 0.0308(9) Uani 1 1 d . . . H16A H 1.0895 0.2475 -0.1356 0.037 Uiso 1 1 calc R . . H16B H 1.0947 0.2646 -0.0383 0.037 Uiso 1 1 calc R . . C17 C 1.0304(3) 0.1487(2) -0.0654(2) 0.0240(8) Uani 1 1 d . . . H17A H 1.0370 0.1097 -0.1129 0.029 Uiso 1 1 calc R . . H17B H 0.9440 0.1708 -0.0608 0.029 Uiso 1 1 calc R . . C21 C 0.9227(3) 0.38692(19) 0.4181(2) 0.0144(7) Uani 1 1 d . . . C22 C 0.8984(3) 0.41333(19) 0.50472(18) 0.0145(7) Uani 1 1 d . . . C23 C 0.9411(3) 0.3393(2) 0.56207(19) 0.0202(7) Uani 1 1 d . . . H23B H 1.0270 0.3210 0.5486 0.024 Uiso 1 1 calc R . . H23A H 0.9382 0.3586 0.6202 0.024 Uiso 1 1 calc R . . C24 C 0.8613(3) 0.2649(2) 0.5531(2) 0.0256(8) Uani 1 1 d . . . H24B H 0.8721 0.2412 0.4969 0.031 Uiso 1 1 calc R . . H24A H 0.8877 0.2204 0.5935 0.031 Uiso 1 1 calc R . . C25 C 0.7274(3) 0.2910(2) 0.5674(2) 0.0313(9) Uani 1 1 d . . . H25A H 0.7151 0.3086 0.6256 0.038 Uiso 1 1 calc R . . H25B H 0.6778 0.2422 0.5577 0.038 Uiso 1 1 calc R . . C26 C 0.6841(3) 0.3629(2) 0.5105(2) 0.0263(8) Uani 1 1 d . . . H26A H 0.5982 0.3808 0.5243 0.032 Uiso 1 1 calc R . . H26B H 0.6863 0.3428 0.4526 0.032 Uiso 1 1 calc R . . C27 C 0.7623(3) 0.4383(2) 0.5172(2) 0.0199(7) Uani 1 1 d . . . H27A H 0.7498 0.4641 0.5724 0.024 Uiso 1 1 calc R . . H27B H 0.7356 0.4810 0.4751 0.024 Uiso 1 1 calc R . . C31 C 0.9428(3) 0.1089(2) 0.35874(19) 0.0163(7) Uani 1 1 d . . . C32 C 0.9181(3) 0.0310(2) 0.40578(19) 0.0177(7) Uani 1 1 d . . . C33 C 0.9458(3) -0.0470(2) 0.3529(2) 0.0213(7) Uani 1 1 d . . . H33A H 0.9368 -0.0981 0.3872 0.026 Uiso 1 1 calc R . . H33B H 1.0316 -0.0480 0.3331 0.026 Uiso 1 1 calc R . . C34 C 0.8601(3) -0.0483(2) 0.2788(2) 0.0303(9) Uani 1 1 d . . . H34B H 0.8762 -0.0010 0.2410 0.036 Uiso 1 1 calc R . . H34A H 0.8767 -0.1015 0.2481 0.036 Uiso 1 1 calc R . . C35 C 0.7272(3) -0.0409(2) 0.3057(2) 0.0354(9) Uani 1 1 d . . . H35A H 0.7086 -0.0919 0.3376 0.042 Uiso 1 1 calc R . . H35B H 0.6744 -0.0378 0.2561 0.042 Uiso 1 1 calc R . . C36 C 0.6985(3) 0.0369(2) 0.3587(2) 0.0311(9) Uani 1 1 d . . . H36B H 0.7066 0.0881 0.3245 0.037 Uiso 1 1 calc R . . H36A H 0.6127 0.0372 0.3785 0.037 Uiso 1 1 calc R . . C37 C 0.7834(3) 0.0391(2) 0.4327(2) 0.0219(8) Uani 1 1 d . . . H37A H 0.7669 -0.0076 0.4711 0.026 Uiso 1 1 calc R . . H37B H 0.7668 0.0927 0.4626 0.026 Uiso 1 1 calc R . . C41 C 1.0364(3) 0.4421(2) 0.13684(18) 0.0138(7) Uani 1 1 d . . . C42 C 1.0946(3) 0.51032(19) 0.09147(18) 0.0145(7) Uani 1 1 d . . . C43 C 1.2317(3) 0.4862(2) 0.0838(2) 0.0196(7) Uani 1 1 d . . . H43B H 1.2435 0.4289 0.0605 0.024 Uiso 1 1 calc R . . H43A H 1.2691 0.5257 0.0450 0.024 Uiso 1 1 calc R . . C44 C 1.2960(3) 0.4884(2) 0.1668(2) 0.0253(8) Uani 1 1 d . . . H44B H 1.2674 0.4430 0.2028 0.030 Uiso 1 1 calc R . . H44A H 1.3852 0.4775 0.1581 0.030 Uiso 1 1 calc R . . C45 C 1.2723(3) 0.5723(2) 0.2098(2) 0.0256(8) Uani 1 1 d . . . H45A H 1.3097 0.6169 0.1772 0.031 Uiso 1 1 calc R . . H45B H 1.3112 0.5696 0.2650 0.031 Uiso 1 1 calc R . . C46 C 1.1360(3) 0.5944(2) 0.21970(19) 0.0196(7) Uani 1 1 d . . . H46A H 1.1233 0.6509 0.2448 0.024 Uiso 1 1 calc R . . H46B H 1.1005 0.5531 0.2575 0.024 Uiso 1 1 calc R . . C47 C 1.0705(3) 0.59405(19) 0.13666(19) 0.0187(7) Uani 1 1 d . . . H47A H 1.0985 0.6403 0.1015 0.022 Uiso 1 1 calc R . . H47B H 0.9813 0.6045 0.1459 0.022 Uiso 1 1 calc R . . C51 C 1.2637(3) 0.26483(18) 0.30367(18) 0.0131(7) Uani 1 1 d . . . C52 C 1.3838(3) 0.25949(19) 0.34614(19) 0.0142(7) Uani 1 1 d . . . C53 C 1.4042(3) 0.1751(2) 0.3920(2) 0.0198(7) Uani 1 1 d . . . H53B H 1.3943 0.1287 0.3527 0.024 Uiso 1 1 calc R . . H53A H 1.4892 0.1696 0.4130 0.024 Uiso 1 1 calc R . . C54 C 1.3163(3) 0.1666(2) 0.4638(2) 0.0272(8) Uani 1 1 d . . . H54A H 1.3378 0.1133 0.4939 0.033 Uiso 1 1 calc R . . H54B H 1.2322 0.1639 0.4422 0.033 Uiso 1 1 calc R . . C55 C 1.3195(4) 0.2399(2) 0.5234(2) 0.0311(9) Uani 1 1 d . . . H55B H 1.2567 0.2343 0.5670 0.037 Uiso 1 1 calc R . . H55A H 1.4006 0.2385 0.5504 0.037 Uiso 1 1 calc R . . C56 C 1.2958(3) 0.3232(2) 0.4788(2) 0.0259(8) Uani 1 1 d . . . H56A H 1.3034 0.3697 0.5185 0.031 Uiso 1 1 calc R . . H56B H 1.2110 0.3272 0.4575 0.031 Uiso 1 1 calc R . . C57 C 1.3850(3) 0.3336(2) 0.40682(19) 0.0183(7) Uani 1 1 d . . . H57A H 1.4688 0.3371 0.4288 0.022 Uiso 1 1 calc R . . H57B H 1.3624 0.3869 0.3770 0.022 Uiso 1 1 calc R . . C61 C 0.6830(3) 0.27394(19) 0.19701(18) 0.0136(7) Uani 1 1 d . . . C62 C 0.5653(3) 0.25946(19) 0.15616(19) 0.0134(7) Uani 1 1 d . . . C63 C 0.5743(3) 0.1702(2) 0.1199(2) 0.0210(7) Uani 1 1 d . . . H63B H 0.6021 0.1295 0.1636 0.025 Uiso 1 1 calc R . . H63A H 0.4921 0.1557 0.1018 0.025 Uiso 1 1 calc R . . C64 C 0.6627(3) 0.1622(2) 0.0467(2) 0.0311(9) Uani 1 1 d . . . H64B H 0.7472 0.1677 0.0666 0.037 Uiso 1 1 calc R . . H64A H 0.6591 0.1056 0.0221 0.037 Uiso 1 1 calc R . . C65 C 0.6326(3) 0.2289(2) -0.0193(2) 0.0322(9) Uani 1 1 d . . . H65B H 0.6950 0.2239 -0.0638 0.039 Uiso 1 1 calc R . . H65A H 0.5521 0.2193 -0.0439 0.039 Uiso 1 1 calc R . . C66 C 0.6292(3) 0.3166(2) 0.0167(2) 0.0255(8) Uani 1 1 d . . . H66A H 0.6055 0.3583 -0.0270 0.031 Uiso 1 1 calc R . . H66B H 0.7120 0.3282 0.0361 0.031 Uiso 1 1 calc R . . C67 C 0.5392(3) 0.3266(2) 0.0885(2) 0.0197(7) Uani 1 1 d . . . H67A H 0.4550 0.3222 0.0676 0.024 Uiso 1 1 calc R . . H67B H 0.5439 0.3833 0.1127 0.024 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 In1 0.01864(13) 0.03763(16) 0.01925(14) -0.00143(11) 0.00022(10) -0.00326(11) In2 0.01880(13) 0.01667(13) 0.01941(13) -0.00188(9) 0.00100(9) -0.00181(9) Fe1 0.0090(2) 0.0097(2) 0.0080(2) 0.00188(17) -0.00058(16) -0.00242(17) Cl1 0.0550(7) 0.0396(6) 0.0717(8) -0.0077(6) 0.0098(6) 0.0055(5) Cl2 0.0544(7) 0.0772(9) 0.0675(8) 0.0514(7) -0.0068(6) -0.0133(6) Cl3 0.0762(8) 0.0611(7) 0.0280(6) -0.0199(5) 0.0085(5) -0.0151(6) Cl4 0.0155(5) 0.1796(16) 0.0547(8) -0.0437(9) -0.0019(5) -0.0115(7) Cl5 0.0313(5) 0.0203(5) 0.0423(6) -0.0017(4) 0.0019(4) 0.0084(4) Cl6 0.0244(4) 0.0245(5) 0.0278(5) -0.0038(4) 0.0001(4) -0.0079(4) Cl7 0.0244(4) 0.0295(5) 0.0226(4) 0.0007(4) 0.0039(3) -0.0050(4) Cl8 0.0323(5) 0.0282(5) 0.0197(4) -0.0012(4) -0.0008(4) -0.0067(4) N11 0.0153(14) 0.0154(14) 0.0160(15) -0.0001(12) -0.0009(11) -0.0012(11) N12 0.0275(16) 0.0227(17) 0.0263(17) -0.0070(12) 0.0011(13) -0.0034(13) N21 0.0159(14) 0.0147(14) 0.0147(15) 0.0010(12) -0.0009(11) -0.0044(11) N22 0.0178(15) 0.0189(15) 0.0114(14) -0.0040(11) -0.0003(10) -0.0055(11) N31 0.0152(14) 0.0148(15) 0.0161(14) 0.0029(12) 0.0026(11) -0.0014(11) N32 0.0276(16) 0.0191(15) 0.0184(15) 0.0058(11) -0.0032(12) -0.0013(13) N41 0.0168(14) 0.0170(15) 0.0138(14) 0.0030(12) -0.0023(11) -0.0021(12) N42 0.0245(15) 0.0144(15) 0.0128(14) 0.0025(11) 0.0016(12) -0.0036(11) N51 0.0150(15) 0.0156(14) 0.0119(13) 0.0017(11) 0.0018(11) -0.0020(11) N52 0.0095(13) 0.0197(15) 0.0181(15) -0.0008(11) 0.0009(11) -0.0003(11) N61 0.0137(15) 0.0147(14) 0.0156(14) -0.0003(11) 0.0015(11) -0.0017(11) N62 0.0098(13) 0.0196(15) 0.0178(15) -0.0005(11) 0.0011(11) -0.0033(11) C11 0.0144(17) 0.0226(19) 0.0201(19) 0.0036(15) -0.0010(14) 0.0001(14) C12 0.0231(18) 0.0164(17) 0.0194(18) -0.0046(14) 0.0026(14) -0.0005(14) C13 0.0225(19) 0.0243(19) 0.0224(19) -0.0032(15) -0.0013(15) 0.0039(15) C14 0.023(2) 0.036(2) 0.034(2) -0.0140(17) 0.0009(16) -0.0041(16) C15 0.041(2) 0.030(2) 0.039(2) -0.0028(18) 0.0097(19) -0.0115(18) C16 0.046(2) 0.0191(19) 0.027(2) 0.0038(15) 0.0011(17) 0.0021(17) C17 0.0232(19) 0.029(2) 0.0189(18) -0.0051(15) -0.0033(14) 0.0037(15) C21 0.0109(16) 0.0137(17) 0.0191(19) 0.0023(14) -0.0023(13) -0.0058(13) C22 0.0157(16) 0.0174(17) 0.0114(16) -0.0058(13) 0.0008(13) -0.0067(13) C23 0.0225(18) 0.0269(19) 0.0109(17) 0.0008(14) 0.0007(13) -0.0003(15) C24 0.042(2) 0.0191(19) 0.0166(18) 0.0017(14) 0.0068(16) -0.0067(16) C25 0.037(2) 0.032(2) 0.028(2) -0.0059(17) 0.0112(17) -0.0212(17) C26 0.0140(17) 0.036(2) 0.031(2) -0.0111(17) 0.0048(15) -0.0104(15) C27 0.0187(17) 0.0211(18) 0.0198(18) -0.0061(14) 0.0011(14) -0.0005(14) C31 0.0154(17) 0.0180(19) 0.0155(17) -0.0002(15) -0.0006(13) -0.0013(14) C32 0.0226(18) 0.0164(17) 0.0142(17) 0.0068(13) -0.0001(13) -0.0040(14) C33 0.0233(18) 0.0164(18) 0.0238(19) 0.0028(14) 0.0019(15) 0.0018(14) C34 0.043(2) 0.028(2) 0.0210(19) -0.0017(16) -0.0042(17) -0.0056(17) C35 0.031(2) 0.039(2) 0.037(2) -0.0011(18) -0.0135(18) -0.0063(18) C36 0.0188(19) 0.030(2) 0.045(2) 0.0093(18) -0.0040(17) -0.0033(16) C37 0.0230(18) 0.0173(18) 0.0254(19) 0.0051(14) 0.0066(15) -0.0014(14) C41 0.0160(16) 0.0152(17) 0.0099(16) -0.0012(13) -0.0001(13) 0.0016(14) C42 0.0223(17) 0.0113(16) 0.0103(16) 0.0044(12) -0.0001(13) -0.0053(13) C43 0.0206(18) 0.0181(18) 0.0209(18) -0.0047(14) 0.0089(14) -0.0065(14) C44 0.0167(18) 0.033(2) 0.026(2) -0.0011(16) 0.0024(15) -0.0024(15) C45 0.0265(19) 0.031(2) 0.0201(19) -0.0045(15) -0.0019(15) -0.0106(16) C46 0.0274(19) 0.0166(17) 0.0155(17) -0.0050(13) 0.0029(14) -0.0052(14) C47 0.0254(18) 0.0131(17) 0.0174(17) 0.0021(13) 0.0039(14) -0.0018(14) C51 0.0142(17) 0.0126(16) 0.0127(16) 0.0020(12) 0.0035(13) -0.0022(13) C52 0.0103(15) 0.0182(17) 0.0142(16) 0.0023(13) -0.0021(12) -0.0015(13) C53 0.0167(17) 0.0190(18) 0.0233(18) 0.0003(14) -0.0008(14) 0.0008(14) C54 0.029(2) 0.023(2) 0.029(2) 0.0121(16) -0.0002(16) -0.0006(16) C55 0.037(2) 0.037(2) 0.0190(19) 0.0069(16) 0.0045(16) 0.0034(18) C56 0.032(2) 0.027(2) 0.0185(18) -0.0025(15) 0.0017(15) 0.0053(16) C57 0.0177(17) 0.0181(18) 0.0196(18) -0.0004(14) -0.0036(14) -0.0034(14) C61 0.0135(17) 0.0129(16) 0.0141(16) 0.0004(13) 0.0025(13) -0.0004(13) C62 0.0063(15) 0.0183(17) 0.0159(17) -0.0006(13) 0.0007(12) -0.0034(12) C63 0.0203(18) 0.0165(18) 0.0269(19) -0.0031(14) -0.0056(14) -0.0045(14) C64 0.028(2) 0.030(2) 0.035(2) -0.0177(17) -0.0030(17) 0.0051(16) C65 0.026(2) 0.051(3) 0.0196(19) -0.0079(17) 0.0032(15) -0.0021(18) C66 0.0231(19) 0.038(2) 0.0160(18) 0.0073(15) 0.0018(14) -0.0051(16) C67 0.0147(17) 0.0227(18) 0.0216(18) 0.0031(14) -0.0024(14) 0.0004(14) #=============================================================================# # MOLECULAR GEOMETRY # #=============================================================================# _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 In1 Cl1 2.3077(11) . ? In1 Cl4 2.3189(11) . ? In1 Cl3 2.3343(10) . ? In1 Cl2 2.3345(11) . ? In2 Cl7 2.3465(8) . ? In2 Cl6 2.3477(8) . ? In2 Cl8 2.3503(9) . ? In2 Cl5 2.3683(9) . ? Fe1 N41 2.123(3) . ? Fe1 N31 2.140(3) . ? Fe1 N21 2.150(3) . ? Fe1 N11 2.164(3) . ? Fe1 N61 2.164(3) . ? Fe1 N51 2.172(3) . ? N11 C11 1.147(4) . ? N12 N12 1.234(5) 2_755 ? N12 C12 1.499(4) . ? N21 C21 1.143(4) . ? N22 N22 1.227(5) 2_766 ? N22 C22 1.489(4) . ? N31 C31 1.138(4) . ? N32 N32 1.231(5) 2_756 ? N32 C32 1.502(4) . ? N41 C41 1.142(4) . ? N42 N42 1.228(5) 2_765 ? N42 C42 1.483(4) . ? N51 C51 1.142(4) . ? N52 N62 1.225(4) 1_655 ? N52 C52 1.484(4) . ? N61 C61 1.143(4) . ? N62 N52 1.225(4) 1_455 ? N62 C62 1.486(4) . ? C11 C12 1.501(5) . ? C12 C13 1.529(5) . ? C12 C17 1.535(5) . ? C13 C14 1.509(5) . ? C14 C15 1.522(5) . ? C15 C16 1.514(5) . ? C16 C17 1.519(5) . ? C21 C22 1.482(4) . ? C22 C27 1.530(4) . ? C22 C23 1.543(4) . ? C23 C24 1.524(5) . ? C24 C25 1.514(5) . ? C25 C26 1.516(5) . ? C26 C27 1.523(5) . ? C31 C32 1.487(4) . ? C32 C33 1.525(4) . ? C32 C37 1.533(4) . ? C33 C34 1.527(5) . ? C34 C35 1.513(5) . ? C35 C36 1.526(5) . ? C36 C37 1.520(5) . ? C41 C42 1.481(4) . ? C42 C43 1.529(4) . ? C42 C47 1.531(4) . ? C43 C44 1.520(5) . ? C44 C45 1.517(5) . ? C45 C46 1.518(5) . ? C46 C47 1.525(4) . ? C51 C52 1.484(4) . ? C52 C53 1.533(4) . ? C52 C57 1.540(4) . ? C53 C54 1.514(5) . ? C54 C55 1.520(5) . ? C55 C56 1.512(5) . ? C56 C57 1.530(5) . ? C61 C62 1.483(4) . ? C62 C63 1.537(4) . ? C62 C67 1.538(4) . ? C63 C64 1.524(5) . ? C64 C65 1.521(5) . ? C65 C66 1.514(5) . ? C66 C67 1.520(5) . ? 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 Cl1 In1 Cl4 110.24(5) . . ? Cl1 In1 Cl3 109.39(5) . . ? Cl4 In1 Cl3 109.91(4) . . ? Cl1 In1 Cl2 110.60(5) . . ? Cl4 In1 Cl2 106.85(5) . . ? Cl3 In1 Cl2 109.82(5) . . ? Cl7 In2 Cl6 114.18(3) . . ? Cl7 In2 Cl8 115.30(3) . . ? Cl6 In2 Cl8 112.72(3) . . ? Cl7 In2 Cl5 103.36(3) . . ? Cl6 In2 Cl5 104.83(3) . . ? Cl8 In2 Cl5 104.88(3) . . ? N41 Fe1 N31 178.16(10) . . ? N41 Fe1 N21 90.36(10) . . ? N31 Fe1 N21 89.71(10) . . ? N41 Fe1 N11 89.60(10) . . ? N31 Fe1 N11 90.30(10) . . ? N21 Fe1 N11 179.17(10) . . ? N41 Fe1 N61 93.02(10) . . ? N31 Fe1 N61 88.82(10) . . ? N21 Fe1 N61 91.18(9) . . ? N11 Fe1 N61 89.65(9) . . ? N41 Fe1 N51 89.36(9) . . ? N31 Fe1 N51 88.81(9) . . ? N21 Fe1 N51 88.93(9) . . ? N11 Fe1 N51 90.24(9) . . ? N61 Fe1 N51 177.62(9) . . ? C11 N11 Fe1 175.3(3) . . ? N12 N12 C12 111.2(3) 2_755 . ? C21 N21 Fe1 168.9(2) . . ? N22 N22 C22 114.1(3) 2_766 . ? C31 N31 Fe1 176.0(2) . . ? N32 N32 C32 111.5(3) 2_756 . ? C41 N41 Fe1 166.9(2) . . ? N42 N42 C42 114.3(3) 2_765 . ? C51 N51 Fe1 170.5(2) . . ? N62 N52 C52 114.3(2) 1_655 . ? C61 N61 Fe1 168.6(2) . . ? N52 N62 C62 114.4(2) 1_455 . ? N11 C11 C12 177.5(3) . . ? N12 C12 C11 104.1(3) . . ? N12 C12 C13 112.8(3) . . ? C11 C12 C13 110.1(3) . . ? N12 C12 C17 110.1(3) . . ? C11 C12 C17 108.6(3) . . ? C13 C12 C17 111.0(3) . . ? C14 C13 C12 111.8(3) . . ? C13 C14 C15 111.7(3) . . ? C16 C15 C14 110.8(3) . . ? C15 C16 C17 112.6(3) . . ? C16 C17 C12 111.8(3) . . ? N21 C21 C22 172.2(3) . . ? C21 C22 N22 112.2(2) . . ? C21 C22 C27 110.4(3) . . ? N22 C22 C27 107.1(2) . . ? C21 C22 C23 107.9(2) . . ? N22 C22 C23 107.9(2) . . ? C27 C22 C23 111.3(3) . . ? C24 C23 C22 111.7(3) . . ? C25 C24 C23 111.4(3) . . ? C24 C25 C26 111.5(3) . . ? C25 C26 C27 112.5(3) . . ? C26 C27 C22 111.8(3) . . ? N31 C31 C32 175.3(3) . . ? C31 C32 N32 104.3(2) . . ? C31 C32 C33 110.8(3) . . ? N32 C32 C33 112.7(3) . . ? C31 C32 C37 107.2(3) . . ? N32 C32 C37 110.1(3) . . ? C33 C32 C37 111.4(3) . . ? C32 C33 C34 111.5(3) . . ? C35 C34 C33 111.4(3) . . ? C34 C35 C36 111.7(3) . . ? C37 C36 C35 111.8(3) . . ? C36 C37 C32 111.4(3) . . ? N41 C41 C42 175.3(3) . . ? C41 C42 N42 111.1(2) . . ? C41 C42 C43 108.4(3) . . ? N42 C42 C43 109.0(2) . . ? C41 C42 C47 110.1(2) . . ? N42 C42 C47 106.7(2) . . ? C43 C42 C47 111.5(3) . . ? C44 C43 C42 112.0(3) . . ? C45 C44 C43 112.2(3) . . ? C44 C45 C46 111.1(3) . . ? C45 C46 C47 111.4(3) . . ? C46 C47 C42 112.0(3) . . ? N51 C51 C52 174.0(3) . . ? C51 C52 N52 112.6(2) . . ? C51 C52 C53 110.6(3) . . ? N52 C52 C53 106.2(2) . . ? C51 C52 C57 107.9(2) . . ? N52 C52 C57 108.7(2) . . ? C53 C52 C57 110.8(3) . . ? C54 C53 C52 112.7(3) . . ? C53 C54 C55 111.8(3) . . ? C56 C55 C54 111.1(3) . . ? C55 C56 C57 112.1(3) . . ? C56 C57 C52 111.5(3) . . ? N61 C61 C62 172.8(3) . . ? C61 C62 N62 113.0(2) . . ? C61 C62 C63 108.3(2) . . ? N62 C62 C63 106.3(2) . . ? C61 C62 C67 109.6(2) . . ? N62 C62 C67 108.2(2) . . ? C63 C62 C67 111.4(3) . . ? C64 C63 C62 112.3(3) . . ? C65 C64 C63 111.9(3) . . ? C66 C65 C64 111.2(3) . . ? C65 C66 C67 111.7(3) . . ? C66 C67 C62 112.0(3) . . ? #=============================================================================# # Refinement Special Details # #=============================================================================# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The unit cell parameters are close to monoclinic, however no satisfactory solution could be obtained in this crystal system, and checking of the final model with cifcheck revealed no higher symmetry. ; # Attachment '- CIF_for_4.CIF' #============================================================================== data_4_123K #TrackingRef '- CIF_for_4.CIF' _database_code_depnum_ccdc_archive 'CCDC 776741' ############################################################################## # data_4_123K # ############################################################################## #============================================================================# # CHEMICAL DATA # #============================================================================# _chemical_formula_moiety 'C42 H60 Fe N12, 2(Cl4 Fe)' _chemical_formula_sum 'C42 H60 Cl8 Fe3 N12' _chemical_formula_structural ? _chemical_formula_iupac ? _chemical_formula_weight 1184.17 #=============================================================================# # CRYSTAL DATA # #=============================================================================# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9068(9) _cell_length_b 15.8580(11) _cell_length_c 16.1047(12) _cell_angle_alpha 89.575(3) _cell_angle_beta 89.485(2) _cell_angle_gamma 85.889(2) _cell_volume 2778.1(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9045 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 25.00 _cell_measurement_temperature 123(2) _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.887 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' _exptl_special_details ; It is noted that the data completeness is lower than desirable (0.93), and that the Rint is higher than 0.1 (0.1157). However, this structure is isostructural and isomorphous with a closely related compound (CCDC 776740) with signifcantly better values for these parameters (with the only difference chemically being (InCl4)- anions in place of the (FeCl4)- anions here), so we believe the solution contained in this cif is correct. ; #=============================================================================# # EXPERIMENTAL DATA # #=============================================================================# _diffrn_ambient_temperature 123(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_reflns_number 13125 _diffrn_reflns_av_R_equivalents 0.1157 _diffrn_reflns_av_sigmaI/netI 0.1334 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measured_fraction_theta_full 0.926 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_reduction_process ; Lorentz and polarization correction applied ; #=============================================================================# # REFINEMENT DATA # #=============================================================================# _reflns_number_total 9045 _reflns_number_gt 6822 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_number_reflns 9045 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+10.8878P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.800 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.145 _refine_ls_extinction_method none 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _computing_data_collection 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_cell_refinement 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_data_reduction 'Bruker Apex2 v2.0 (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001) ORTEP (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' #=============================================================================# # ATOMIC COORDINATES AND DISPLANCEMENT PARAMETERS # #=============================================================================# 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 -0.02574(7) 0.27905(5) 0.74711(5) 0.0146(2) Uani 1 1 d . . . Fe2 Fe 0.67573(8) 0.06527(6) 0.24873(6) 0.0218(2) Uani 1 1 d . . . Fe3 Fe 0.35667(8) 0.40495(7) 0.24855(6) 0.0285(3) Uani 1 1 d . . . Cl1 Cl 0.53991(15) 0.05298(11) 0.34906(10) 0.0310(4) Uani 1 1 d . . . Cl2 Cl 0.79294(16) -0.05384(11) 0.24979(12) 0.0362(4) Uani 1 1 d . . . Cl3 Cl 0.79535(15) 0.16835(11) 0.27086(11) 0.0311(4) Uani 1 1 d . . . Cl4 Cl 0.59140(16) 0.07695(11) 0.12538(10) 0.0325(4) Uani 1 1 d . . . Cl5 Cl 0.4651(2) 0.28533(14) 0.24007(15) 0.0550(6) Uani 1 1 d . . . Cl6 Cl 0.4408(2) 0.50110(18) 0.17277(17) 0.0740(8) Uani 1 1 d . . . Cl7 Cl 0.17211(18) 0.3919(2) 0.20084(15) 0.0707(8) Uani 1 1 d . . . Cl8 Cl 0.3456(2) 0.44469(17) 0.37846(13) 0.0630(7) Uani 1 1 d . . . N11 N 0.0130(5) 0.2003(3) 0.6384(3) 0.0205(11) Uani 1 1 d . . . N12 N -0.0111(5) 0.0276(3) 0.5254(3) 0.0270(13) Uani 1 1 d . . . N21 N -0.0617(5) 0.3573(3) 0.8551(3) 0.0223(12) Uani 1 1 d . . . N22 N -0.0340(5) 0.4873(3) 1.0277(3) 0.0215(11) Uani 1 1 d . . . N31 N -0.0479(5) 0.1680(3) 0.8206(3) 0.0238(12) Uani 1 1 d . . . N32 N -0.0001(5) 0.0334(3) 0.9802(3) 0.0236(12) Uani 1 1 d . . . N41 N 0.0019(5) 0.3882(4) 0.6739(3) 0.0249(12) Uani 1 1 d . . . N42 N 0.0422(5) 0.5231(3) 0.5077(3) 0.0222(12) Uani 1 1 d . . . N51 N 0.1669(4) 0.2700(3) 0.7781(3) 0.0182(11) Uani 1 1 d . . . N52 N 0.4904(4) 0.2642(3) 0.7886(3) 0.0231(12) Uani 1 1 d . . . N61 N -0.2192(5) 0.2827(3) 0.7188(3) 0.0218(12) Uani 1 1 d . . . N62 N -0.5401(4) 0.2626(3) 0.7146(3) 0.0221(12) Uani 1 1 d . . . C11 C 0.0397(5) 0.1565(4) 0.5851(4) 0.0212(14) Uani 1 1 d . . . C12 C 0.0686(6) 0.1004(4) 0.5128(4) 0.0219(14) Uani 1 1 d . . . C13 C 0.2054(6) 0.0700(4) 0.5119(4) 0.0232(14) Uani 1 1 d . . . H13B H 0.2274 0.0434 0.5661 0.028 Uiso 1 1 calc R . . H13A H 0.2208 0.0268 0.4683 0.028 Uiso 1 1 calc R . . C14 C 0.2854(6) 0.1426(4) 0.4955(4) 0.0299(16) Uani 1 1 d . . . H14A H 0.3726 0.1207 0.4925 0.036 Uiso 1 1 calc R . . H14B H 0.2764 0.1830 0.5422 0.036 Uiso 1 1 calc R . . C15 C 0.2503(6) 0.1886(4) 0.4144(5) 0.0321(17) Uani 1 1 d . . . H15B H 0.3015 0.2372 0.4068 0.039 Uiso 1 1 calc R . . H15A H 0.2670 0.1497 0.3672 0.039 Uiso 1 1 calc R . . C16 C 0.1157(6) 0.2199(5) 0.4146(5) 0.0334(17) Uani 1 1 d . . . H16A H 0.0945 0.2454 0.3599 0.040 Uiso 1 1 calc R . . H16B H 0.1015 0.2644 0.4572 0.040 Uiso 1 1 calc R . . C17 C 0.0319(6) 0.1486(4) 0.4329(4) 0.0251(15) Uani 1 1 d . . . H17A H 0.0361 0.1088 0.3857 0.030 Uiso 1 1 calc R . . H17B H -0.0541 0.1726 0.4383 0.030 Uiso 1 1 calc R . . C21 C -0.0785(5) 0.3858(4) 0.9187(4) 0.0169(13) Uani 1 1 d . . . C22 C -0.1016(6) 0.4132(4) 1.0059(4) 0.0216(14) Uani 1 1 d . . . C23 C -0.0584(6) 0.3395(4) 1.0625(4) 0.0248(14) Uani 1 1 d . . . H23A H -0.0604 0.3590 1.1208 0.030 Uiso 1 1 calc R . . H23B H 0.0278 0.3209 1.0483 0.030 Uiso 1 1 calc R . . C24 C -0.1386(6) 0.2636(4) 1.0550(4) 0.0285(15) Uani 1 1 d . . . H24B H -0.1286 0.2391 0.9988 0.034 Uiso 1 1 calc R . . H24A H -0.1116 0.2194 1.0959 0.034 Uiso 1 1 calc R . . C25 C -0.2722(6) 0.2917(4) 1.0703(4) 0.0311(16) Uani 1 1 d . . . H25B H -0.3226 0.2428 1.0635 0.037 Uiso 1 1 calc R . . H25A H -0.2826 0.3115 1.1283 0.037 Uiso 1 1 calc R . . C26 C -0.3179(6) 0.3616(5) 1.0121(5) 0.0327(17) Uani 1 1 d . . . H26A H -0.4048 0.3790 1.0255 0.039 Uiso 1 1 calc R . . H26B H -0.3140 0.3406 0.9543 0.039 Uiso 1 1 calc R . . C27 C -0.2399(6) 0.4381(4) 1.0193(4) 0.0272(15) Uani 1 1 d . . . H27A H -0.2526 0.4634 1.0750 0.033 Uiso 1 1 calc R . . H27B H -0.2675 0.4813 0.9775 0.033 Uiso 1 1 calc R . . C31 C -0.0577(5) 0.1071(4) 0.8577(4) 0.0163(13) Uani 1 1 d . . . C32 C -0.0821(6) 0.0301(4) 0.9061(4) 0.0246(14) Uani 1 1 d . . . C33 C -0.0563(6) -0.0497(4) 0.8530(4) 0.0288(16) Uani 1 1 d . . . H33B H 0.0298 -0.0522 0.8327 0.035 Uiso 1 1 calc R . . H33A H -0.0664 -0.1004 0.8879 0.035 Uiso 1 1 calc R . . C34 C -0.1421(6) -0.0504(4) 0.7793(4) 0.0292(16) Uani 1 1 d . . . H34A H -0.1259 -0.1038 0.7484 0.035 Uiso 1 1 calc R . . H34B H -0.1265 -0.0029 0.7414 0.035 Uiso 1 1 calc R . . C35 C -0.2755(6) -0.0424(5) 0.8083(5) 0.0367(18) Uani 1 1 d . . . H35B H -0.3296 -0.0400 0.7592 0.044 Uiso 1 1 calc R . . H35A H -0.2929 -0.0932 0.8412 0.044 Uiso 1 1 calc R . . C36 C -0.3043(6) 0.0352(5) 0.8602(5) 0.0366(18) Uani 1 1 d . . . H36A H -0.3902 0.0355 0.8808 0.044 Uiso 1 1 calc R . . H36B H -0.2975 0.0862 0.8251 0.044 Uiso 1 1 calc R . . C37 C -0.2181(6) 0.0389(4) 0.9341(4) 0.0220(14) Uani 1 1 d . . . H37A H -0.2339 -0.0071 0.9738 0.026 Uiso 1 1 calc R . . H37B H -0.2348 0.0935 0.9631 0.026 Uiso 1 1 calc R . . C41 C 0.0358(5) 0.4433(4) 0.6375(4) 0.0179(13) Uani 1 1 d . . . C42 C 0.0933(6) 0.5121(4) 0.5916(4) 0.0215(14) Uani 1 1 d . . . C43 C 0.2339(5) 0.4896(4) 0.5832(4) 0.0229(14) Uani 1 1 d . . . H43B H 0.2479 0.4324 0.5592 0.027 Uiso 1 1 calc R . . H43A H 0.2697 0.5301 0.5445 0.027 Uiso 1 1 calc R . . C44 C 0.2984(6) 0.4917(4) 0.6657(4) 0.0305(16) Uani 1 1 d . . . H44A H 0.3881 0.4812 0.6568 0.037 Uiso 1 1 calc R . . H44B H 0.2706 0.4461 0.7021 0.037 Uiso 1 1 calc R . . C45 C 0.2718(6) 0.5771(5) 0.7085(4) 0.0309(16) Uani 1 1 d . . . H45B H 0.3109 0.5754 0.7638 0.037 Uiso 1 1 calc R . . H45A H 0.3079 0.6220 0.6751 0.037 Uiso 1 1 calc R . . C46 C 0.1334(6) 0.5981(4) 0.7186(4) 0.0230(14) Uani 1 1 d . . . H46B H 0.0991 0.5565 0.7569 0.028 Uiso 1 1 calc R . . H46A H 0.1188 0.6548 0.7435 0.028 Uiso 1 1 calc R . . C47 C 0.0678(6) 0.5966(4) 0.6359(4) 0.0245(14) Uani 1 1 d . . . H47A H 0.0951 0.6427 0.5999 0.029 Uiso 1 1 calc R . . H47B H -0.0218 0.6070 0.6453 0.029 Uiso 1 1 calc R . . C51 C 0.2642(6) 0.2644(4) 0.8048(4) 0.0214(14) Uani 1 1 d . . . C52 C 0.3849(5) 0.2592(4) 0.8473(4) 0.0202(13) Uani 1 1 d . . . C53 C 0.4077(6) 0.1746(4) 0.8935(4) 0.0250(14) Uani 1 1 d . . . H53B H 0.3979 0.1278 0.8543 0.030 Uiso 1 1 calc R . . H53A H 0.4933 0.1694 0.9137 0.030 Uiso 1 1 calc R . . C54 C 0.3201(7) 0.1660(4) 0.9669(4) 0.0328(17) Uani 1 1 d . . . H54A H 0.3428 0.1127 0.9971 0.039 Uiso 1 1 calc R . . H54B H 0.2353 0.1633 0.9462 0.039 Uiso 1 1 calc R . . C55 C 0.3237(7) 0.2408(4) 1.0271(4) 0.0342(17) Uani 1 1 d . . . H55B H 0.2619 0.2354 1.0719 0.041 Uiso 1 1 calc R . . H55A H 0.4058 0.2402 1.0529 0.041 Uiso 1 1 calc R . . C56 C 0.2964(6) 0.3239(4) 0.9801(4) 0.0316(17) Uani 1 1 d . . . H56B H 0.2117 0.3259 0.9583 0.038 Uiso 1 1 calc R . . H56A H 0.3012 0.3716 1.0189 0.038 Uiso 1 1 calc R . . C57 C 0.3863(6) 0.3340(4) 0.9083(4) 0.0262(15) Uani 1 1 d . . . H57A H 0.4703 0.3371 0.9303 0.031 Uiso 1 1 calc R . . H57B H 0.3638 0.3876 0.8783 0.031 Uiso 1 1 calc R . . C61 C -0.3175(5) 0.2744(4) 0.6947(4) 0.0190(13) Uani 1 1 d . . . C62 C -0.4361(5) 0.2598(4) 0.6544(4) 0.0201(13) Uani 1 1 d . . . C63 C -0.4645(6) 0.3278(4) 0.5886(4) 0.0243(14) Uani 1 1 d . . . H63B H -0.4590 0.3842 0.6136 0.029 Uiso 1 1 calc R . . H63A H -0.5497 0.3241 0.5690 0.029 Uiso 1 1 calc R . . C64 C -0.3754(7) 0.3185(5) 0.5141(4) 0.0322(16) Uani 1 1 d . . . H64A H -0.4011 0.3606 0.4708 0.039 Uiso 1 1 calc R . . H64B H -0.2916 0.3298 0.5320 0.039 Uiso 1 1 calc R . . C65 C -0.3737(7) 0.2290(5) 0.4776(4) 0.0370(18) Uani 1 1 d . . . H65A H -0.4560 0.2195 0.4555 0.044 Uiso 1 1 calc R . . H65B H -0.3138 0.2239 0.4310 0.044 Uiso 1 1 calc R . . C66 C -0.3390(6) 0.1626(4) 0.5430(4) 0.0318(17) Uani 1 1 d . . . H66B H -0.2539 0.1692 0.5615 0.038 Uiso 1 1 calc R . . H66A H -0.3414 0.1057 0.5184 0.038 Uiso 1 1 calc R . . C67 C -0.4260(6) 0.1700(4) 0.6175(4) 0.0266(15) Uani 1 1 d . . . H67B H -0.3963 0.1291 0.6609 0.032 Uiso 1 1 calc R . . H67A H -0.5086 0.1551 0.6004 0.032 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 0.0101(4) 0.0170(5) 0.0168(4) -0.0022(3) 0.0014(3) -0.0019(3) Fe2 0.0159(5) 0.0226(5) 0.0269(5) -0.0042(4) 0.0023(4) -0.0018(4) Fe3 0.0169(5) 0.0433(6) 0.0258(5) -0.0033(4) 0.0019(4) -0.0065(4) Cl1 0.0225(8) 0.0388(10) 0.0315(9) -0.0019(7) 0.0065(7) -0.0022(7) Cl2 0.0304(10) 0.0271(9) 0.0498(11) -0.0042(8) 0.0050(8) 0.0059(7) Cl3 0.0269(9) 0.0321(9) 0.0352(9) -0.0067(7) 0.0004(7) -0.0080(7) Cl4 0.0308(9) 0.0385(10) 0.0288(9) -0.0013(7) -0.0025(7) -0.0068(8) Cl5 0.0460(13) 0.0459(12) 0.0729(15) -0.0149(11) 0.0061(11) 0.0000(10) Cl6 0.0463(13) 0.092(2) 0.0851(19) 0.0544(16) -0.0103(12) -0.0193(13) Cl7 0.0159(10) 0.135(2) 0.0630(15) -0.0322(15) -0.0003(9) -0.0120(12) Cl8 0.0761(17) 0.0770(17) 0.0378(12) -0.0235(11) 0.0084(11) -0.0168(13) N11 0.015(3) 0.020(3) 0.026(3) -0.004(2) 0.000(2) 0.000(2) N12 0.022(3) 0.026(3) 0.034(3) -0.012(2) 0.004(2) -0.006(2) N21 0.015(3) 0.026(3) 0.025(3) 0.001(2) 0.006(2) 0.000(2) N22 0.022(3) 0.023(3) 0.020(3) -0.003(2) 0.003(2) -0.002(2) N31 0.018(3) 0.025(3) 0.027(3) 0.005(2) 0.001(2) 0.007(2) N32 0.023(3) 0.023(3) 0.025(3) 0.004(2) 0.001(2) -0.003(2) N41 0.020(3) 0.035(3) 0.019(3) 0.010(3) -0.001(2) 0.002(2) N42 0.024(3) 0.022(3) 0.021(3) 0.002(2) 0.003(2) -0.005(2) N51 0.006(3) 0.019(3) 0.029(3) -0.001(2) 0.001(2) -0.001(2) N52 0.010(3) 0.024(3) 0.035(3) -0.005(2) 0.005(2) 0.000(2) N61 0.013(3) 0.026(3) 0.027(3) -0.003(2) 0.004(2) 0.001(2) N62 0.010(2) 0.034(3) 0.023(3) -0.003(2) -0.002(2) -0.005(2) C11 0.011(3) 0.023(3) 0.030(4) -0.004(3) 0.003(3) 0.000(3) C12 0.018(3) 0.019(3) 0.029(3) -0.012(3) -0.002(3) -0.002(3) C13 0.023(3) 0.018(3) 0.028(3) -0.008(3) 0.001(3) 0.003(3) C14 0.021(4) 0.027(4) 0.041(4) -0.011(3) 0.002(3) -0.001(3) C15 0.034(4) 0.023(4) 0.041(4) -0.005(3) 0.009(3) -0.016(3) C16 0.033(4) 0.032(4) 0.035(4) -0.003(3) 0.000(3) 0.002(3) C17 0.014(3) 0.036(4) 0.025(3) -0.013(3) -0.005(3) 0.006(3) C21 0.011(3) 0.016(3) 0.025(3) -0.003(3) 0.004(2) -0.009(2) C22 0.016(3) 0.025(3) 0.024(3) -0.010(3) 0.003(3) -0.002(3) C23 0.022(3) 0.030(4) 0.023(3) -0.006(3) 0.003(3) 0.000(3) C24 0.034(4) 0.021(3) 0.032(4) -0.005(3) 0.006(3) -0.005(3) C25 0.033(4) 0.024(4) 0.039(4) -0.009(3) 0.007(3) -0.019(3) C26 0.011(3) 0.047(5) 0.039(4) -0.013(3) 0.006(3) 0.000(3) C27 0.016(3) 0.033(4) 0.032(4) -0.006(3) 0.007(3) 0.002(3) C31 0.012(3) 0.018(3) 0.021(3) -0.008(3) 0.000(2) -0.009(2) C32 0.018(3) 0.029(4) 0.026(3) 0.004(3) -0.002(3) 0.000(3) C33 0.019(3) 0.031(4) 0.035(4) 0.006(3) 0.001(3) 0.003(3) C34 0.032(4) 0.031(4) 0.024(3) -0.004(3) -0.004(3) 0.004(3) C35 0.025(4) 0.044(5) 0.041(4) -0.001(4) -0.008(3) 0.001(3) C36 0.023(4) 0.033(4) 0.054(5) 0.010(4) 0.006(3) -0.001(3) C37 0.020(3) 0.018(3) 0.029(3) -0.001(3) -0.001(3) -0.005(3) C41 0.017(3) 0.018(3) 0.019(3) -0.006(3) -0.003(2) -0.004(3) C42 0.024(3) 0.025(4) 0.014(3) 0.004(3) 0.006(2) 0.000(3) C43 0.014(3) 0.030(4) 0.025(3) -0.005(3) 0.004(3) -0.007(3) C44 0.012(3) 0.041(4) 0.037(4) -0.006(3) 0.008(3) 0.006(3) C45 0.017(3) 0.044(4) 0.033(4) -0.008(3) 0.001(3) -0.010(3) C46 0.021(3) 0.022(3) 0.026(3) -0.008(3) 0.000(3) -0.003(3) C47 0.025(3) 0.023(3) 0.026(3) 0.004(3) 0.002(3) 0.002(3) C51 0.023(4) 0.023(3) 0.019(3) -0.002(3) 0.006(3) -0.003(3) C52 0.007(3) 0.029(4) 0.024(3) -0.002(3) -0.006(2) 0.000(2) C53 0.022(3) 0.025(4) 0.028(3) -0.008(3) 0.001(3) 0.001(3) C54 0.030(4) 0.028(4) 0.040(4) 0.015(3) 0.008(3) 0.002(3) C55 0.036(4) 0.034(4) 0.032(4) -0.003(3) 0.004(3) 0.004(3) C56 0.027(4) 0.038(4) 0.028(4) -0.002(3) 0.006(3) 0.010(3) C57 0.023(3) 0.026(4) 0.030(4) 0.002(3) 0.000(3) -0.006(3) C61 0.015(3) 0.020(3) 0.022(3) -0.004(3) 0.006(3) -0.002(2) C62 0.010(3) 0.022(3) 0.029(3) -0.005(3) -0.002(2) -0.007(2) C63 0.017(3) 0.022(3) 0.034(4) 0.003(3) 0.006(3) 0.000(3) C64 0.029(4) 0.038(4) 0.029(4) 0.007(3) 0.002(3) -0.004(3) C65 0.026(4) 0.053(5) 0.032(4) -0.008(4) -0.002(3) -0.003(3) C66 0.024(4) 0.032(4) 0.039(4) -0.024(3) -0.004(3) -0.001(3) C67 0.024(4) 0.020(3) 0.037(4) -0.010(3) -0.006(3) -0.006(3) #=============================================================================# # MOLECULAR GEOMETRY # #=============================================================================# _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 N41 2.125(5) . ? Fe1 N31 2.142(5) . ? Fe1 N51 2.159(5) . ? Fe1 N61 2.159(5) . ? Fe1 N21 2.160(5) . ? Fe1 N11 2.179(5) . ? Fe2 Cl3 2.196(2) . ? Fe2 Cl4 2.198(2) . ? Fe2 Cl1 2.1993(18) . ? Fe2 Cl2 2.2036(18) . ? Fe3 Cl5 2.167(2) . ? Fe3 Cl7 2.185(2) . ? Fe3 Cl8 2.189(2) . ? Fe3 Cl6 2.193(2) . ? N11 C11 1.131(8) . ? N12 N12 1.213(10) 2_556 ? N12 C12 1.506(8) . ? N21 C21 1.131(8) . ? N22 N22 1.239(10) 2_567 ? N22 C22 1.479(8) . ? N31 C31 1.143(8) . ? N32 N32 1.232(10) 2_557 ? N32 C32 1.501(8) . ? N41 C41 1.130(8) . ? N42 N42 1.245(11) 2_566 ? N42 C42 1.471(8) . ? N51 C51 1.145(8) . ? N52 N62 1.240(8) 1_655 ? N52 C52 1.489(7) . ? N61 C61 1.160(8) . ? N62 N52 1.240(8) 1_455 ? N62 C62 1.484(8) . ? C11 C12 1.489(8) . ? C12 C17 1.533(9) . ? C12 C13 1.534(8) . ? C13 C14 1.514(9) . ? C13 H13B 0.9900 . ? C13 H13A 0.9900 . ? C14 C15 1.530(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.515(10) . ? C15 H15B 0.9900 . ? C15 H15A 0.9900 . ? C16 C17 1.529(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C21 C22 1.487(8) . ? C22 C23 1.528(9) . ? C22 C27 1.546(8) . ? C23 C24 1.544(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.512(9) . ? C24 H24B 0.9900 . ? C24 H24A 0.9900 . ? C25 C26 1.507(10) . ? C25 H25B 0.9900 . ? C25 H25A 0.9900 . ? C26 C27 1.537(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C31 C32 1.482(8) . ? C32 C33 1.539(9) . ? C32 C37 1.543(8) . ? C33 C34 1.518(9) . ? C33 H33B 0.9900 . ? C33 H33A 0.9900 . ? C34 C35 1.520(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.506(10) . ? C35 H35B 0.9900 . ? C35 H35A 0.9900 . ? C36 C37 1.528(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C41 C42 1.487(8) . ? C42 C47 1.529(9) . ? C42 C43 1.554(8) . ? C43 C44 1.511(9) . ? C43 H43B 0.9900 . ? C43 H43A 0.9900 . ? C44 C45 1.532(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.530(9) . ? C45 H45B 0.9900 . ? C45 H45A 0.9900 . ? C46 C47 1.519(9) . ? C46 H46B 0.9900 . ? C46 H46A 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C51 C52 1.487(9) . ? C52 C53 1.535(9) . ? C52 C57 1.546(9) . ? C53 C54 1.525(9) . ? C53 H53B 0.9900 . ? C53 H53A 0.9900 . ? C54 C55 1.540(10) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.527(9) . ? C55 H55B 0.9900 . ? C55 H55A 0.9900 . ? C56 C57 1.524(9) . ? C56 H56B 0.9900 . ? C56 H56A 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C61 C62 1.485(9) . ? C62 C63 1.525(8) . ? C62 C67 1.543(9) . ? C63 C64 1.538(9) . ? C63 H63B 0.9900 . ? C63 H63A 0.9900 . ? C64 C65 1.538(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.514(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.524(9) . ? C66 H66B 0.9900 . ? C66 H66A 0.9900 . ? C67 H67B 0.9900 . ? C67 H67A 0.9900 . ? 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 N41 Fe1 N31 178.3(2) . . ? N41 Fe1 N51 89.5(2) . . ? N31 Fe1 N51 88.90(19) . . ? N41 Fe1 N61 93.0(2) . . ? N31 Fe1 N61 88.5(2) . . ? N51 Fe1 N61 177.42(19) . . ? N41 Fe1 N21 90.2(2) . . ? N31 Fe1 N21 90.3(2) . . ? N51 Fe1 N21 88.88(19) . . ? N61 Fe1 N21 91.46(19) . . ? N41 Fe1 N11 89.6(2) . . ? N31 Fe1 N11 89.8(2) . . ? N51 Fe1 N11 90.41(19) . . ? N61 Fe1 N11 89.26(19) . . ? N21 Fe1 N11 179.27(19) . . ? Cl3 Fe2 Cl4 111.20(8) . . ? Cl3 Fe2 Cl1 112.31(7) . . ? Cl4 Fe2 Cl1 112.79(8) . . ? Cl3 Fe2 Cl2 107.32(8) . . ? Cl4 Fe2 Cl2 106.96(8) . . ? Cl1 Fe2 Cl2 105.80(8) . . ? Cl5 Fe3 Cl7 110.01(11) . . ? Cl5 Fe3 Cl8 109.23(11) . . ? Cl7 Fe3 Cl8 109.89(10) . . ? Cl5 Fe3 Cl6 110.13(11) . . ? Cl7 Fe3 Cl6 107.61(11) . . ? Cl8 Fe3 Cl6 109.96(12) . . ? C11 N11 Fe1 175.1(5) . . ? N12 N12 C12 111.8(7) 2_556 . ? C21 N21 Fe1 168.4(5) . . ? N22 N22 C22 115.1(6) 2_567 . ? C31 N31 Fe1 177.6(5) . . ? N32 N32 C32 110.2(7) 2_557 . ? C41 N41 Fe1 169.1(5) . . ? N42 N42 C42 114.4(6) 2_566 . ? C51 N51 Fe1 171.4(5) . . ? N62 N52 C52 113.2(5) 1_655 . ? C61 N61 Fe1 169.1(5) . . ? N52 N62 C62 114.7(5) 1_455 . ? N11 C11 C12 177.0(7) . . ? C11 C12 N12 104.5(5) . . ? C11 C12 C17 108.8(5) . . ? N12 C12 C17 110.0(5) . . ? C11 C12 C13 110.5(5) . . ? N12 C12 C13 111.2(5) . . ? C17 C12 C13 111.6(5) . . ? C14 C13 C12 111.2(5) . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? H13B C13 H13A 108.0 . . ? C13 C14 C15 111.3(6) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 111.3(5) . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? H15B C15 H15A 108.0 . . ? C15 C16 C17 111.9(6) . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C12 111.8(5) . . ? C16 C17 H17A 109.2 . . ? C12 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C12 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? N21 C21 C22 173.4(6) . . ? N22 C22 C21 112.5(5) . . ? N22 C22 C23 108.5(5) . . ? C21 C22 C23 107.6(5) . . ? N22 C22 C27 107.2(5) . . ? C21 C22 C27 110.0(5) . . ? C23 C22 C27 111.0(5) . . ? C22 C23 C24 112.4(6) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 110.2(5) . . ? C25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? H24B C24 H24A 108.1 . . ? C26 C25 C24 112.4(5) . . ? C26 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? H25B C25 H25A 107.9 . . ? C25 C26 C27 110.8(6) . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C22 111.8(5) . . ? C26 C27 H27A 109.3 . . ? C22 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C22 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? N31 C31 C32 175.0(6) . . ? C31 C32 N32 104.1(5) . . ? C31 C32 C33 110.8(5) . . ? N32 C32 C33 113.7(5) . . ? C31 C32 C37 107.5(5) . . ? N32 C32 C37 109.8(5) . . ? C33 C32 C37 110.6(5) . . ? C34 C33 C32 111.7(5) . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? H33B C33 H33A 107.9 . . ? C33 C34 C35 110.6(6) . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 112.2(6) . . ? C36 C35 H35B 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35A 109.2 . . ? H35B C35 H35A 107.9 . . ? C35 C36 C37 112.2(6) . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C32 111.3(5) . . ? C36 C37 H37A 109.4 . . ? C32 C37 H37A 109.4 . . ? C36 C37 H37B 109.4 . . ? C32 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? N41 C41 C42 174.1(6) . . ? N42 C42 C41 111.1(5) . . ? N42 C42 C47 106.7(5) . . ? C41 C42 C47 110.7(5) . . ? N42 C42 C43 108.2(5) . . ? C41 C42 C43 109.4(5) . . ? C47 C42 C43 110.8(5) . . ? C44 C43 C42 112.2(5) . . ? C44 C43 H43B 109.2 . . ? C42 C43 H43B 109.2 . . ? C44 C43 H43A 109.2 . . ? C42 C43 H43A 109.2 . . ? H43B C43 H43A 107.9 . . ? C43 C44 C45 111.3(6) . . ? C43 C44 H44A 109.4 . . ? C45 C44 H44A 109.4 . . ? C43 C44 H44B 109.4 . . ? C45 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C44 111.0(5) . . ? C46 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? C46 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? H45B C45 H45A 108.0 . . ? C47 C46 C45 111.6(5) . . ? C47 C46 H46B 109.3 . . ? C45 C46 H46B 109.3 . . ? C47 C46 H46A 109.3 . . ? C45 C46 H46A 109.3 . . ? H46B C46 H46A 108.0 . . ? C46 C47 C42 111.8(5) . . ? C46 C47 H47A 109.3 . . ? C42 C47 H47A 109.3 . . ? C46 C47 H47B 109.3 . . ? C42 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? N51 C51 C52 174.4(6) . . ? C51 C52 N52 112.8(5) . . ? C51 C52 C53 111.1(5) . . ? N52 C52 C53 105.7(5) . . ? C51 C52 C57 108.3(5) . . ? N52 C52 C57 108.2(5) . . ? C53 C52 C57 110.7(5) . . ? C54 C53 C52 112.6(5) . . ? C54 C53 H53B 109.1 . . ? C52 C53 H53B 109.1 . . ? C54 C53 H53A 109.1 . . ? C52 C53 H53A 109.1 . . ? H53B C53 H53A 107.8 . . ? C53 C54 C55 111.7(6) . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C56 C55 C54 109.7(6) . . ? C56 C55 H55B 109.7 . . ? C54 C55 H55B 109.7 . . ? C56 C55 H55A 109.7 . . ? C54 C55 H55A 109.7 . . ? H55B C55 H55A 108.2 . . ? C57 C56 C55 112.0(5) . . ? C57 C56 H56B 109.2 . . ? C55 C56 H56B 109.2 . . ? C57 C56 H56A 109.2 . . ? C55 C56 H56A 109.2 . . ? H56B C56 H56A 107.9 . . ? C56 C57 C52 111.1(6) . . ? C56 C57 H57A 109.4 . . ? C52 C57 H57A 109.4 . . ? C56 C57 H57B 109.4 . . ? C52 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? N61 C61 C62 173.0(6) . . ? N62 C62 C61 112.3(5) . . ? N62 C62 C63 108.1(5) . . ? C61 C62 C63 109.5(5) . . ? N62 C62 C67 106.5(5) . . ? C61 C62 C67 108.2(5) . . ? C63 C62 C67 112.3(5) . . ? C62 C63 C64 111.9(5) . . ? C62 C63 H63B 109.2 . . ? C64 C63 H63B 109.2 . . ? C62 C63 H63A 109.2 . . ? C64 C63 H63A 109.2 . . ? H63B C63 H63A 107.9 . . ? C65 C64 C63 110.8(6) . . ? C65 C64 H64A 109.5 . . ? C63 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? C66 C65 C64 111.0(6) . . ? C66 C65 H65A 109.4 . . ? C64 C65 H65A 109.4 . . ? C66 C65 H65B 109.4 . . ? C64 C65 H65B 109.4 . . ? H65A C65 H65B 108.0 . . ? C65 C66 C67 111.4(5) . . ? C65 C66 H66B 109.3 . . ? C67 C66 H66B 109.3 . . ? C65 C66 H66A 109.3 . . ? C67 C66 H66A 109.3 . . ? H66B C66 H66A 108.0 . . ? C66 C67 C62 112.4(5) . . ? C66 C67 H67B 109.1 . . ? C62 C67 H67B 109.1 . . ? C66 C67 H67A 109.1 . . ? C62 C67 H67A 109.1 . . ? H67B C67 H67A 107.9 . . ? #=============================================================================# # Refinement Special Details # #=============================================================================# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The unit cell parameters are close to monoclinic, however no satisfactory solution could be obtained in this crystal system, and checking of the final model with cifcheck revealed no higher symmetry. ;