# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Galina Matouzenko' 'Caroline Genre' 'Erwann Jeanneau' 'Dominique Luneau' _publ_contact_author_name 'Galina Matouzenko' _publ_contact_author_address ; Laboratoire de Chimie Ecole Normale Sup\'erieure de Lyon 46, all\'ee d'Italie Lyon 69364 FRANCE ; _publ_contact_author_email 'GALINA.MATOUZENKO@ENS-LYON.FR ' _publ_section_title ; A spin-crossover iron(II) coordination polymer with the 8-aminoquinoline ligand: synthesis, crystal structure and magnetic properties of [Fe(aqin)2(bpy)](ClO4)2.2EtOH (aqin = 8-aminoquinoline, bpy= 4,4'-bipyridyl),A spin-crossover iron(II) coordination polymer with the 8-aminoquinoline ligand: synthesis, crystal structure and magnetic properties of [Fe(aqin)2(bpy)](ClO4)2.2EtOH (aqin = 8-aminoquinoline, bpy= 4,4'-bipyridyl) ; # Attachment 'B608679A_80K.cif' data_CRYSTALS_cif_80K _database_code_depnum_ccdc_archive 'CCDC 616015' _audit_creation_date 06-01-13 _audit_creation_method CRYSTALS_ver_12.82 _oxford_structure_analysis_title 'import in C 2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 24.531(5) _cell_length_b 11.147(5) _cell_length_c 17.686(5) _cell_angle_alpha 90 _cell_angle_beta 133.306(5) _cell_angle_gamma 90 _cell_volume 3519(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C28 H24 Cl2 Fe1 N6 O8 # Dc = 1.32 Fooo = 1432.00 Mu = 6.32 M = 349.64 # Found Formula = C28 H24 Cl2 Fe1 N6 O8 # Dc = 1.32 FOOO = 1432.00 Mu = 6.32 M = 349.64 _chemical_formula_sum 'C28 H24 Cl2 Fe1 N6 O8' _chemical_formula_moiety 'C28 H24 Cl2 Fe1 N6 O8' _chemical_compound_source ? _chemical_formula_weight 699.29 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.05 _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.632 # Sheldrick geometric approximatio 0.97 0.97 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9689 _exptl_absorpt_correction_T_max 0.9689 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 4169 _reflns_number_total 4169 _diffrn_reflns_av_R_equivalents 0.053 # Number of reflections with Friedels Law is 4169 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4163 _diffrn_reflns_theta_min 2.154 _diffrn_reflns_theta_max 27.938 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.379 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -32 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.84 _refine_diff_density_max 2.23 _refine_ls_number_reflns 1725 _refine_ls_number_restraints 48 _refine_ls_number_parameters 206 #_refine_ls_R_factor_ref 0.1275 _refine_ls_wR_factor_ref 0.1364 _refine_ls_goodness_of_fit_ref 1.1034 #_reflns_number_all 4155 _refine_ls_R_factor_all 0.1995 _refine_ls_wR_factor_all 0.2011 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 1725 _refine_ls_R_factor_gt 0.1275 _refine_ls_wR_factor_gt 0.1364 _refine_ls_shift/su_max 0.000143 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.00 0.421 0.449 -0.616E-01 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.5000 0.28995(19) 0.7500 0.0330 1.0000 Uani S T . . . . Cl1 Cl 0.74503(19) -0.0194(3) 1.0840(3) 0.0583 1.0000 Uani . . . . . . O2 O 0.7539(7) 0.0882(9) 1.0491(9) 0.0893 1.0000 Uani . . . . . . N4 N 0.5000 -0.5302(11) 0.7500 0.0410 1.0000 Uani S T . . . . O4 O 0.6855(5) -0.0043(9) 1.0825(7) 0.0677 1.0000 Uani . . . . . . C8 C 0.4422(10) 0.3103(10) 0.8457(12) 0.0582 1.0000 Uani . U . . . . C3 C 0.6326(12) 0.3336(12) 1.1094(14) 0.0839 1.0000 Uani . U . . . . N1 N 0.5608(7) 0.2979(8) 0.9003(8) 0.0496 1.0000 Uani . . . . . . C14 C 0.4358(7) -0.3425(10) 0.6782(9) 0.0440 1.0000 Uani . . . . . . C13 C 0.5000 -0.2806(14) 0.7500 0.0421 1.0000 Uani S T . . . . C9 C 0.5176(10) 0.3150(9) 0.9245(12) 0.0627 1.0000 Uani . U . . . . N2 N 0.4131(6) 0.2846(9) 0.7440(8) 0.0517 1.0000 Uani . . . . . . C4 C 0.5528(11) 0.3332(11) 1.0283(13) 0.0718 1.0000 Uani . U . . . . C15 C 0.4379(7) -0.4653(10) 0.6811(9) 0.0410 1.0000 Uani . . . . . . N3 N 0.5000 0.1088(10) 0.7500 0.0336 1.0000 Uani S T . . . . C1 C 0.6344(11) 0.2960(12) 0.9767(13) 0.0751 1.0000 Uani . U . . . . C11 C 0.4541(8) -0.0805(11) 0.6584(9) 0.0614 1.0000 Uani . . . . . . C5 C 0.4986(11) 0.3539(11) 1.0393(13) 0.0700 1.0000 Uani . U . . . . C12 C 0.5000 -0.1441(11) 0.7500 0.0266 1.0000 Uani S T . . . . C10 C 0.4576(8) 0.0424(12) 0.6652(10) 0.0622 1.0000 Uani . . . . . . C6 C 0.4270(12) 0.3434(13) 0.9617(15) 0.0821 1.0000 Uani . U . . . . C7 C 0.3958(10) 0.3273(12) 0.8615(14) 0.0722 1.0000 Uani . U . . . . O1 O 0.8130(7) -0.0455(18) 1.1836(12) 0.1570 1.0000 Uani . . . . . . O3 O 0.7295(9) -0.1113(15) 1.0170(17) 0.1759 1.0000 Uani . . . . . . C2 C 0.6710(12) 0.3168(11) 1.0825(14) 0.0865 1.0000 Uani . U . . . . H31 H 0.6566 0.3443 1.1787 0.0939 1.0000 Uiso R . . . . . H141 H 0.3907 -0.3020 0.6263 0.0611 1.0000 Uiso R . . . . . H151 H 0.3938 -0.5081 0.6328 0.0472 1.0000 Uiso R . . . . . H11 H 0.6639 0.2842 0.9617 0.0751 1.0000 Uiso R . . . . . H111 H 0.4241 -0.1190 0.5948 0.0881 1.0000 Uiso R . . . . . H51 H 0.5181 0.3702 1.1056 0.1540 1.0000 Uiso R . . . . . H101 H 0.4275 0.0825 0.6019 0.0701 1.0000 Uiso R . . . . . H61 H 0.3947 0.3505 0.9719 0.1620 1.0000 Uiso R . . . . . H71 H 0.3441 0.3264 0.8063 0.1481 1.0000 Uiso R . . . . . H201 H 0.7233 0.3198 1.1343 0.0741 1.0000 Uiso R . . . . . H21 H 0.3750 0.3464 0.6934 0.0595 1.0000 Uiso R . . . . . H22 H 0.3893 0.2034 0.7208 0.0595 1.0000 Uiso 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 0.0466(15) 0.0210(10) 0.0370(13) 0.0000 0.0309(13) 0.0000 Cl1 0.054(2) 0.053(2) 0.062(2) 0.0114(16) 0.0374(18) 0.0054(16) O2 0.102(9) 0.059(7) 0.117(9) 0.033(6) 0.080(8) 0.015(6) N4 0.058(9) 0.027(7) 0.055(9) 0.0000 0.046(8) 0.0000 O4 0.064(6) 0.086(7) 0.066(6) 0.008(5) 0.050(5) -0.008(5) C8 0.129(8) 0.022(5) 0.090(6) -0.004(5) 0.101(6) -0.005(6) C3 0.148(9) 0.027(6) 0.082(7) -0.009(6) 0.081(7) -0.003(7) N1 0.090(8) 0.023(4) 0.047(6) -0.001(5) 0.052(6) -0.001(5) C14 0.065(9) 0.028(5) 0.056(7) 0.000(5) 0.049(7) -0.004(6) C13 0.051(11) 0.032(9) 0.052(10) 0.0000 0.039(10) 0.0000 C9 0.131(7) 0.016(4) 0.089(6) -0.003(4) 0.094(5) -0.011(5) N2 0.080(8) 0.033(5) 0.075(7) 0.006(5) 0.066(7) 0.004(5) C4 0.145(9) 0.030(5) 0.085(7) -0.012(5) 0.096(7) -0.017(6) C15 0.053(7) 0.025(5) 0.057(7) -0.007(5) 0.042(7) -0.009(5) N3 0.024(7) 0.021(6) 0.042(8) 0.0000 0.017(7) 0.0000 C1 0.135(6) 0.028(3) 0.094(5) -0.006(4) 0.090(5) -0.007(4) C11 0.085(11) 0.035(7) 0.044(7) -0.016(6) 0.037(8) -0.006(6) C5 0.141(9) 0.026(5) 0.092(7) -0.013(5) 0.099(7) -0.013(6) C12 0.056(10) 0.012(6) 0.033(8) 0.0000 0.039(8) 0.0000 C10 0.081(10) 0.039(7) 0.036(7) 0.008(6) 0.028(8) 0.011(7) C6 0.136(9) 0.046(6) 0.106(8) -0.009(6) 0.099(7) -0.013(7) C7 0.122(8) 0.033(6) 0.115(8) -0.005(6) 0.102(7) -0.001(6) O1 0.058(7) 0.28(2) 0.126(12) 0.130(13) 0.059(8) 0.068(10) O3 0.137(13) 0.118(13) 0.28(2) -0.106(14) 0.147(16) -0.020(10) C2 0.134(9) 0.026(6) 0.087(7) -0.004(5) 0.071(7) -0.005(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1068(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N2 5_656 2.062(10) yes Fe1 . N4 5_666 2.005(13) yes Fe1 . N1 5_656 1.964(9) yes Fe1 . N1 . 1.964(9) yes Fe1 . N2 . 2.062(10) yes Fe1 . N3 . 2.020(12) yes Cl1 . O2 . 1.432(10) yes Cl1 . O4 . 1.454(10) yes Cl1 . O1 . 1.393(12) yes Cl1 . O3 . 1.406(15) yes N4 . C15 5_656 1.335(14) yes N4 . C15 . 1.335(14) yes C8 . C9 . 1.35(2) yes C8 . N2 . 1.436(15) yes C8 . C7 . 1.359(18) yes C3 . C4 . 1.43(2) yes C3 . C2 . 1.33(2) yes C3 . H31 . 0.934 no N1 . C9 . 1.403(17) yes N1 . C1 . 1.32(2) yes C14 . C13 . 1.352(14) yes C14 . C15 . 1.370(15) yes C14 . H141 . 0.937 no C13 . C12 . 1.521(18) yes C9 . C4 . 1.409(19) yes N2 . H21 . 1.000 no N2 . H22 . 1.000 no C4 . C5 . 1.49(2) yes C15 . H151 . 0.928 no N3 . C10 5_656 1.318(14) yes N3 . C10 . 1.318(14) yes C1 . C2 . 1.43(2) yes C1 . H11 . 0.936 no C11 . C12 . 1.375(14) yes C11 . C10 . 1.373(17) yes C11 . H111 . 0.926 no C5 . C6 . 1.29(2) yes C5 . H51 . 0.930 no C10 . H101 . 0.930 no C6 . C7 . 1.38(2) yes C6 . H61 . 0.931 no C7 . H71 . 0.929 no C2 . H201 . 0.935 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 5_656 Fe1 . N4 5_666 91.6(3) yes N2 5_656 Fe1 . N1 5_656 82.5(5) yes N4 5_666 Fe1 . N1 5_656 87.4(3) yes N2 5_656 Fe1 . N1 . 97.6(5) yes N4 5_666 Fe1 . N1 . 87.4(3) yes N1 5_656 Fe1 . N1 . 174.8(5) yes N2 5_656 Fe1 . N2 . 176.7(6) yes N4 5_666 Fe1 . N2 . 91.6(3) yes N1 5_656 Fe1 . N2 . 97.6(5) yes N1 . Fe1 . N2 . 82.5(5) yes N2 5_656 Fe1 . N3 . 88.4(3) yes N4 5_666 Fe1 . N3 . 179.994 yes N1 5_656 Fe1 . N3 . 92.6(3) yes N1 . Fe1 . N3 . 92.6(3) yes N2 . Fe1 . N3 . 88.4(3) yes O2 . Cl1 . O4 . 110.1(6) yes O2 . Cl1 . O1 . 108.4(9) yes O4 . Cl1 . O1 . 111.3(7) yes O2 . Cl1 . O3 . 106.3(11) yes O4 . Cl1 . O3 . 112.3(8) yes O1 . Cl1 . O3 . 108.1(12) yes Fe1 1_545 N4 . C15 5_656 122.8(7) yes Fe1 1_545 N4 . C15 . 122.8(7) yes C15 5_656 N4 . C15 . 114.4(14) yes C9 . C8 . N2 . 116.9(11) yes C9 . C8 . C7 . 122.0(13) yes N2 . C8 . C7 . 121.1(15) yes C4 . C3 . C28 . 117.5(16) yes C4 . C3 . H31 . 121.0 no C2 . C3 . H31 . 121.5 no Fe1 . N1 . C9 . 112.8(10) yes Fe1 . N1 . C1 . 128.5(10) yes C12 . N1 . C1 . 118.6(12) yes C13 . C14 . C15 . 119.0(13) yes C13 . C14 . H141 . 120.4 no C15 . C14 . H141 . 120.5 no C14 5_656 C13 . C14 . 118.6(16) yes C14 5_656 C13 . C12 . 120.7(8) yes C14 . C13 . C12 . 120.7(8) yes N1 . C9 . C8 . 117.8(12) yes N1 . C9 . C4 . 120.1(16) yes C8 . C9 . C4 . 122.1(14) yes C8 . N2 . Fe1 . 108.7(9) yes C8 . N2 . H21 . 110.0 no Fe1 . N2 . H21 . 108.8 no C8 . N2 . H22 . 110.1 no Fe1 . N2 . H22 . 109.7 no H21 . N2 . H22 . 109.5 no C3 . C4 . C9 . 120.1(15) yes C3 . C4 . C5 . 127.0(14) yes C9 . C1 . C5 . 112.9(16) yes C14 . C15 . N4 . 124.5(12) yes C14 . C15 . H151 . 119.3 no N4 . C15 . H151 . 116.2 no Fe1 . N3 . C10 5_656 124.1(7) yes Fe1 . N3 . C10 . 124.1(7) yes C10 5_656 N3 . C10 . 111.7(14) yes N1 . C1 . C2 . 121.9(16) yes N1 . C1 . H11 . 119.5 no C2 . C1 . H11 . 118.6 no C12 . C11 . C10 . 117.4(11) yes C12 . C11 . H111 . 121.3 no C10 . C11 . H111 . 121.2 no C4 . C5 . C6 . 122.0(14) yes C4 . C5 . H51 . 117.4 no C6 . C5 . H51 . 120.5 no C13 . C12 . C11 . 121.0(7) yes C13 . C12 . C11 5_656 121.0(7) yes C11 . C12 . C11 5_656 117.9(13) yes C11 . C10 . N3 . 127.8(12) yes C11 . C10 . H101 . 115.1 no N3 . C10 . H101 . 117.1 no C5 . C6 . C7 . 122.1(16) yes C5 . C6 . H61 . 120.2 no C7 . C6 . H61 . 117.7 no C6 . C7 . C8 . 118.5(17) yes C6 . C7 . H71 . 120.5 no C8 . C7 . H71 . 121.0 no C1 . C2 . C3 . 121.8(19) yes C1 . C2 . H201 . 119.7 no C3 . C2 . H201 . 118.6 no # Attachment 'B608679A_293K.cif' data_CRYSTALS_cif_293K _database_code_depnum_ccdc_archive 'CCDC 616016' _audit_creation_date 06-01-13 _audit_creation_method CRYSTALS_ver_12.82 _oxford_structure_analysis_title 'import in C 2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 25.192(5) _cell_length_b 11.485(5) _cell_length_c 18.005(5) _cell_angle_alpha 90 _cell_angle_beta 133.652(5) _cell_angle_gamma 90 _cell_volume 3769(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C28 H24 Cl2 Fe1 N6 O8 # Dc = 1.23 Fooo = 1432.00 Mu = 5.90 M = 349.64 # Found Formula = C28 H24 Cl2 Fe1 N6 O8 # Dc = 1.23 FOOO = 1432.00 Mu = 5.90 M = 349.64 _chemical_formula_sum 'C28 H24 Cl2 Fe1 N6 O8' _chemical_formula_moiety 'C28 H24 Cl2 Fe1 N6 O8' _chemical_compound_source ? _chemical_formula_weight 699.29 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.05 _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.590 # Sheldrick geometric approximatio 0.97 0.97 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9709 _exptl_absorpt_correction_T_max 0.9709 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 4097 _reflns_number_total 4097 _diffrn_reflns_av_R_equivalents 0.058 # Number of reflections with Friedels Law is 4097 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4221 _diffrn_reflns_theta_min 2.096 _diffrn_reflns_theta_max 27.631 _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.144 _diffrn_measured_fraction_theta_full 0.970 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -31 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.74 _refine_diff_density_max 1.23 _refine_ls_number_reflns 1320 _refine_ls_number_restraints 70 _refine_ls_number_parameters 206 #_refine_ls_R_factor_ref 0.1307 _refine_ls_wR_factor_ref 0.1438 _refine_ls_goodness_of_fit_ref 1.1309 #_reflns_number_all 4084 _refine_ls_R_factor_all 0.2454 _refine_ls_wR_factor_all 0.3139 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 1320 _refine_ls_R_factor_gt 0.1307 _refine_ls_wR_factor_gt 0.1438 _refine_ls_shift/su_max 0.000021 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.11 1.66 1.21 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999). J. App. Cryst. 32, 115-119 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.0000 0.2061(2) 0.2500 0.0466 1.0000 Uani S T . . . . Cl1 Cl -0.2514(3) -0.0160(6) 0.0866(4) 0.0961 1.0000 Uani . . . . . . N4 N 0.0000 0.0129(14) 0.2500 0.0531 1.0000 Uani S T . . . . C15 C 0.0623(10) -0.0465(12) 0.3190(13) 0.0594 1.0000 Uani . . . . . . C14 C 0.0642(8) -0.1694(11) 0.3218(12) 0.0543 1.0000 Uani . . . . . . C13 C 0.0000 -0.2321(14) 0.2500 0.0423 1.0000 Uani S TU . . . . N1 N 0.0653(8) 0.2000(10) 0.4136(9) 0.0671 1.0000 Uani . . . . . . C10 C -0.0415(11) -0.5366(17) 0.1657(12) 0.0937 1.0000 Uani . . . . . . N3 N 0.0000 -0.6029(13) 0.2500 0.0372 1.0000 Uani S T . . . . C11 C -0.0412(12) -0.4247(14) 0.1608(15) 0.0877 1.0000 Uani . . . . . . C12 C 0.0000 -0.3569(17) 0.2500 0.0465 1.0000 Uani S TU . . . . N2 N -0.0842(7) 0.2042(10) 0.2534(9) 0.0584 1.0000 Uani . . . . . . C2 C 0.1732(14) 0.1753(16) 0.5921(17) 0.1021 1.0000 Uani . U . . . . O1 O -0.1844(11) -0.026(2) 0.1811(17) 0.1708 1.0000 Uani . U . . . . C1 C 0.1359(14) 0.1936(15) 0.4871(16) 0.0922 1.0000 Uani . U . . . . O2 O -0.2497(11) 0.078(2) 0.0475(18) 0.1833 1.0000 Uani . U . . . . C3 C 0.1383(15) 0.1621(17) 0.6177(18) 0.1033 1.0000 Uani . U . . . . O4 O -0.3082(12) -0.0035(19) 0.0773(16) 0.1687 1.0000 Uani . U . . . . O3 O -0.2647(12) -0.077(2) 0.014(2) 0.1998 1.0000 Uani . U . . . . C8 C -0.0551(12) 0.1866(12) 0.3515(15) 0.0737 1.0000 Uani . U . . . . C9 C 0.0239(12) 0.1835(11) 0.4375(13) 0.0686 1.0000 Uani . U . . . . C4 C 0.0575(14) 0.1645(15) 0.5373(17) 0.0925 1.0000 Uani . U . . . . C5 C 0.0076(15) 0.1456(17) 0.5538(18) 0.1053 1.0000 Uani . U . . . . C6 C -0.0594(14) 0.1602(17) 0.4770(17) 0.0947 1.0000 Uani . U . . . . C7 C -0.0941(14) 0.1702(14) 0.3764(16) 0.0906 1.0000 Uani . U . . . . H151 H 0.1058 -0.0060 0.3678 0.0791 1.0000 Uiso R . . . . . H141 H 0.1083 -0.2090 0.3708 0.0481 1.0000 Uiso R . . . . . H101 H -0.0753 -0.5742 0.1028 0.0751 1.0000 Uiso R . . . . . H111 H -0.0664 -0.3873 0.0985 0.1091 1.0000 Uiso R . . . . . H201 H 0.2242 0.1731 0.6419 0.1161 1.0000 Uiso R . . . . . H11 H 0.1635 0.2006 0.4703 0.1120 1.0000 Uiso R . . . . . H31 H 0.1628 0.1508 0.6861 0.1160 1.0000 Uiso R . . . . . H51 H 0.0244 0.1276 0.6174 0.1181 1.0000 Uiso R . . . . . H61 H -0.0899 0.1618 0.4892 0.1241 1.0000 Uiso R . . . . . H71 H -0.1450 0.1672 0.3253 0.1120 1.0000 Uiso R . . . . . H22 H -0.1083 0.2713 0.2293 0.0950 1.0000 Uiso R . . . . . H21 H -0.1163 0.1487 0.2120 0.0951 1.0000 Uiso 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 0.062(2) 0.0169(12) 0.060(2) 0.0000 0.0419(19) 0.0000 Cl1 0.067(3) 0.116(4) 0.075(3) 0.005(3) 0.037(3) 0.003(3) N4 0.066(13) 0.042(9) 0.047(11) 0.0000 0.037(11) 0.0000 C15 0.076(12) 0.032(7) 0.067(11) 0.001(7) 0.048(10) -0.003(7) C14 0.053(10) 0.035(7) 0.075(11) 0.008(6) 0.044(9) 0.007(6) C13 0.029(9) 0.035(7) 0.067(10) 0.0000 0.035(8) 0.0000 N1 0.083(10) 0.033(5) 0.047(8) 0.000(6) 0.030(8) 0.010(7) C10 0.089(14) 0.082(13) 0.034(10) -0.026(9) 0.014(10) -0.019(11) N3 0.008(8) 0.053(9) 0.026(9) 0.0000 0.002(8) 0.0000 C11 0.134(18) 0.046(10) 0.097(16) 0.016(9) 0.085(15) 0.007(10) C12 0.034(9) 0.037(7) 0.064(10) 0.0000 0.032(8) 0.0000 N2 0.082(9) 0.045(6) 0.067(8) 0.003(6) 0.059(8) 0.003(7) C2 0.133(10) 0.075(9) 0.090(9) 0.001(7) 0.073(8) -0.005(8) O1 0.116(8) 0.203(12) 0.158(10) 0.013(9) 0.082(8) 0.007(9) C1 0.137(10) 0.067(8) 0.089(8) -0.004(7) 0.084(8) -0.010(8) O2 0.121(10) 0.192(14) 0.165(12) 0.021(11) 0.072(9) 0.009(10) C3 0.141(11) 0.075(8) 0.089(9) 0.003(7) 0.078(8) -0.008(8) O4 0.111(9) 0.213(14) 0.159(11) 0.009(10) 0.085(9) -0.002(10) O3 0.129(11) 0.206(14) 0.173(12) -0.006(11) 0.070(10) 0.021(10) C8 0.118(10) 0.041(7) 0.096(8) -0.009(6) 0.087(7) -0.006(7) C9 0.137(10) 0.043(7) 0.078(8) -0.001(6) 0.094(7) 0.000(7) C4 0.135(10) 0.063(8) 0.093(9) -0.009(7) 0.084(8) -0.003(8) C5 0.143(11) 0.071(8) 0.090(9) -0.001(8) 0.075(8) -0.004(9) C6 0.131(10) 0.087(8) 0.098(9) -0.002(8) 0.091(8) -0.006(8) C7 0.134(8) 0.066(5) 0.090(6) -0.002(5) 0.084(6) -0.005(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1515(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N3 1_565 2.195(15) yes Fe1 . N1 5_555 2.167(12) yes Fe1 . N2 5_555 2.163(11) yes Fe1 . N4 . 2.218(16) yes Fe1 . N1 . 2.167(12) yes Fe1 . N2 . 2.163(11) yes Cl2 . O1 . 1.34(2) yes Cl2 . O2 . 1.30(3) yes Cl2 . O4 . 1.33(2) yes Cl2 . O3 . 1.31(3) yes N4 . C15 5_555 1.334(17) yes N4 . C15 . 1.334(17) yes C15 . C14 . 1.413(18) yes C15 . H151 . 0.928 no C14 . C13 . 1.386(17) yes C14 . H141 . 0.930 no C13 . C12 . 1.43(2) yes N1 . C1 . 1.29(3) yes N1 . C9 . 1.39(2) yes C10 . N3 . 1.34(2) yes C10 . C11 . 1.29(2) yes C10 . H101 . 0.928 no C11 . C12 . 1.40(2) yes C11 . H111 . 0.930 no N2 . C8 . 1.38(2) yes N2 . H22 . 0.887 no N2 . H21 . 0.885 no C2 . C1 . 1.43(3) yes C2 . C3 . 1.25(3) yes C2 . H201 . 0.930 no C1 . H11 . 0.932 no O2 . O3 . 1.83(4) yes C3 . C4 . 1.47(3) yes C3 . H31 . 0.930 no C8 . C9 . 1.45(3) yes C8 . C7 . 1.35(3) yes C9 . C4 . 1.38(2) yes C4 . C5 . 1.50(3) yes C5 . C6 . 1.25(3) yes C5 . H51 . 0.930 no C6 . C7 . 1.37(3) yes C6 . H61 . 0.933 no C7 . H71 . 0.929 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 1_565 Fe1 . N1 5_555 91.8(3) yes N3 1_565 Fe1 . N2 5_555 90.6(3) yes N1 5_555 Fe1 . N2 5_555 78.5(5) yes N3 1_565 Fe1 . N4 . 179.995 yes N1 5_555 Fe1 . N4 . 88.2(3) yes N2 5_555 Fe1 . N4 . 89.4(3) yes N3 1_565 Fe1 . N1 . 91.8(3) yes N1 5_555 Fe1 . N1 . 176.3(6) yes N2 5_555 Fe1 . N1 . 101.4(5) yes N4 . Fe1 . N1 . 88.2(3) yes N3 1_565 Fe1 . N2 . 90.6(3) yes N1 5_555 Fe1 . N2 . 101.4(5) yes N2 5_555 Fe1 . N2 . 178.9(6) yes N4 . Fe1 . N2 . 89.4(3) yes N1 . Fe1 . N2 . 78.5(5) yes O1 . Cl2 . O2 . 105.9(14) yes O1 . Cl2 . O4 . 118.2(14) yes O2 . Cl2 . O4 . 106.0(14) yes O1 . Cl2 . O3 . 117.0(14) yes O2 . Cl2 . O3 . 89.0(18) yes O4 . Cl2 . O3 . 115.0(15) yes Fe1 . N4 . C15 5_555 120.7(9) yes Fe1 . N4 . C15 . 120.7(9) yes C15 5_555 N4 . C15 . 118.5(18) yes N4 . C15 . C14 . 122.3(15) yes N4 . C15 . H151 . 119.2 no C14 . C15 . H151 . 118.5 no C15 . C14 . C13 . 119.8(14) yes C15 . C14 . H141 . 120.8 no C13 . C14 . H141 . 119.4 no C14 5_555 C13 . C14 . 117.4(16) yes C14 5_555 C13 . C12 . 121.3(8) yes C14 . C13 . C12 . 121.3(8) yes Fe1 . N1 . C1 . 127.7(13) yes Fe1 . N1 . C9 . 113.4(11) yes C1 . N1 . C9 . 118.1(15) yes N3 . C10 . C11 . 127.4(16) yes N3 . C10 . H101 . 117.5 no C11 . C10 . H101 . 115.1 no Fe1 1_545 N3 . C10 . 124.7(9) yes Fe1 1_545 N3 . C10 5_555 124.7(9) yes C10 . N3 . C10 5_555 110.6(18) yes C10 . C11 . C12 . 120.8(17) yes C10 . C11 . H111 . 120.8 no C12 . C11 . H111 . 118.4 no C13 . C12 . C11 5_555 123.8(9) yes C13 . C12 . C11 . 123.8(9) yes C11 5_555 C12 . C11 . 112.4(19) yes Fe1 . N2 . C8 . 111.8(11) yes Fe1 . N2 . H22 . 109.3 no C8 . N2 . H22 . 109.5 no Fe1 . N2 . H21 . 109.0 no C8 . N2 . H21 . 110.0 no H22 . N2 . H21 . 107.1 no C1 . C2 . C3 . 121(3) yes C1 . C2 . H201 . 119.2 no C3 . C2 . H201 . 119.7 no C2 . C1 . N1 . 123(2) yes C2 . C1 . H11 . 119.0 no N1 . C1 . H11 . 117.9 no Cl1 . O2 . O3 . 45.8(13) yes C2 . C3 . C4 . 119(2) yes C2 . C3 . H31 . 120.8 no C4 . C3 . H31 . 120.5 no O2 . O3 . Cl2 . 45.3(12) yes N2 . C8 . C9 . 119.6(15) yes N2 . C8 . C7 . 125.5(19) yes C9 . C8 . C7 . 114.9(18) yes C8 . C9 . N1 . 115.9(14) yes C8 . C9 . C4 . 123.5(18) yes N1 . C9 . C4 . 120.6(19) yes C3 . C4 . C9 . 118(2) yes C3 . C4 . C5 . 125.7(20) yes C9 . C4 . C5 . 116(2) yes C4 . C5 . C6 . 116(2) yes C4 . C5 . H51 . 123.2 no C6 . C5 . H51 . 120.7 no C5 . C6 . C7 . 128(2) yes C5 . C6 . H61 . 116.4 no C7 . C6 . H61 . 115.6 no C6 . C7 . C8 . 120(2) yes C6 . C7 . H71 . 119.4 no C8 . C7 . H71 . 120.2 no