#------------------------------------------------------------------------------ #$Date: 2008-04-05 11:13:02 +0300 (Sat, 05 Apr 2008) $ #$Revision: 340 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2102216.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2102216 loop_ _publ_author_name 'Money, Victoria A.' 'Radosavljevic Evans, Ivana' 'Elha\"ik, Jerome' 'Halcrow, Malcolm A.' 'Howard, Judith A. K.' _publ_section_title ; An X-ray powder diffraction study of the spin-crossover transition and structure of bis(2,6-dipyrazol-1-ylpyrazine)iron(II) perchlorate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 41 _journal_page_last 45 _journal_volume 60 _journal_year 2004 _chemical_formula_sum 'C20 Cl2 Fe N12 O8' _chemical_formula_weight 663.05 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _audit_creation_method 'from EXP file using GSAS2CIF' _cell_angle_alpha 90.0 _cell_angle_beta 90.539(7) _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 8.4484(8) _cell_length_b 8.4322(8) _cell_length_c 19.404(2) _cell_volume 1382.2738 _computing_structure_refinement GSAS _computing_structure_solution DASH _refine_ls_goodness_of_fit_all 3.58 _refine_ls_matrix_type full _refine_ls_number_parameters 152 _refine_ls_number_restraints 94 _refine_ls_shift/su_max 0.18 _refine_ls_shift/su_mean 0.04 _[local]_cod_data_source_file bm5003.cif loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_type_symbol Fe1 0.750(4) 0.339(4) 0.2453(14) 0.04712 Uiso 1.0 FE N1 0.524(5) 0.237(7) 0.212(5) 0.01593 Uiso 1.0 N N2 0.486(9) 0.231(7) 0.143(4) 0.01593 Uiso 1.0 N C1 0.413(12) 0.157(8) 0.247(3) 0.01593 Uiso 1.0 C C2 0.300(6) 0.109(6) 0.200(6) 0.01593 Uiso 1.0 C C3 0.346(10) 0.156(8) 0.136(4) 0.01593 Uiso 1.0 C N3 0.765(10) 0.347(7) 0.1345(15) 0.01593 Uiso 1.0 N C4 0.633(8) 0.275(7) 0.115(4) 0.01593 Uiso 1.0 C C5 0.598(7) 0.257(6) 0.045(5) 0.01593 Uiso 1.0 C N11 0.700(11) 0.312(8) -0.001(2) 0.01593 Uiso 1.0 N C7 0.832(9) 0.387(7) 0.019(3) 0.01593 Uiso 1.0 C C8 0.865(7) 0.403(6) 0.089(4) 0.01593 Uiso 1.0 C N4 0.997(15) 0.440(10) 0.131(7) 0.01593 Uiso 1.0 N N5 0.970(9) 0.429(8) 0.201(9) 0.01593 Uiso 1.0 N C9 1.136(18) 0.511(11) 0.122(5) 0.01593 Uiso 1.0 C C10 1.193(6) 0.556(6) 0.186(10) 0.01593 Uiso 1.0 C N6 0.643(8) 0.565(7) 0.280(7) 0.01593 Uiso 1.0 N N7 0.640(8) 0.602(10) 0.349(5) 0.01593 Uiso 1.0 N C11 1.09(2) 0.497(11) 0.234(3) 0.01593 Uiso 1.0 C C12 0.562(10) 0.680(15) 0.245(3) 0.01593 Uiso 1.0 C C13 0.507(6) 0.786(6) 0.292(7) 0.01593 Uiso 1.0 C C14 0.563(10) 0.741(11) 0.356(4) 0.01593 Uiso 1.0 C N8 0.756(13) 0.34(3) 0.3557(15) 0.01593 Uiso 1.0 N C15 0.682(11) 0.462(13) 0.386(10) 0.01593 Uiso 1.0 C C16 0.658(7) 0.458(13) 0.456(10) 0.01593 Uiso 1.0 C N17 0.720(13) 0.34(2) 0.4937(16) 0.01593 Uiso 1.0 N C18 0.789(10) 0.215(12) 0.462(10) 0.01593 Uiso 1.0 C C19 0.806(7) 0.218(14) 0.391(10) 0.01593 Uiso 1.0 C N9 0.860(9) 0.083(10) 0.353(6) 0.01593 Uiso 1.0 N N10 0.830(6) 0.104(8) 0.283(7) 0.01593 Uiso 1.0 N C20 0.929(8) -0.059(13) 0.361(4) 0.01593 Uiso 1.0 C C21 0.949(6) -0.125(5) 0.298(7) 0.01593 Uiso 1.0 C C22 0.878(10) -0.028(16) 0.250(3) 0.01593 Uiso 1.0 C Cl1 0.230(3) 0.357(4) 0.9154(10) 0.07909 Uiso 1.0 CL O1 0.383(5) 0.384(11) 0.890(3) 0.11897 Uiso 1.0 O O2 0.117(8) 0.426(10) 0.870(3) 0.11897 Uiso 1.0 O O3 0.217(9) 0.426(7) 0.9810(18) 0.11897 Uiso 1.0 O O4 0.203(11) 0.196(4) 0.920(4) 0.11897 Uiso 1.0 O Cl2 0.752(3) 0.836(4) 0.5701(11) 0.07909 Uiso 1.0 CL O5 0.595(5) 0.800(10) 0.551(4) 0.11897 Uiso 1.0 O O6 0.756(10) 0.981(8) 0.605(5) 0.11897 Uiso 1.0 O O7 0.811(9) 0.716(10) 0.613(4) 0.11897 Uiso 1.0 O O8 0.844(8) 0.847(12) 0.511(2) 0.11897 Uiso 1.0 O H131 0.4382 0.8798 0.2818 0.0191 Uiso 1.0000 H H31 0.2866 0.1380 0.0919 0.0191 Uiso 1.0000 H H21 0.2009 0.0497 0.2110 0.0191 Uiso 1.0000 H H121 0.5459 0.6855 0.1940 0.0191 Uiso 1.0000 H H141 0.5490 0.8010 0.4000 0.0191 Uiso 1.0000 H H51 0.4979 0.2036 0.0298 0.0191 Uiso 1.0000 H H11 0.4127 0.1361 0.2972 0.0191 Uiso 1.0000 H H71 0.9065 0.4313 -0.0154 0.0191 Uiso 1.0000 H H161 0.5948 0.5431 0.4787 0.0191 Uiso 1.0000 H H91 1.1896 0.5286 0.0769 0.0191 Uiso 1.0000 H H111 1.1082 0.5031 0.2853 0.0191 Uiso 1.0000 H H181 0.8275 0.1220 0.4894 0.0191 Uiso 1.0000 H H101 1.2903 0.6204 0.1953 0.0191 Uiso 1.0000 H H221 0.8643 -0.0511 0.1998 0.0191 Uiso 1.0000 H H201 0.9605 -0.1081 0.4060 0.0191 Uiso 1.0000 H H211 1.0056 -0.2266 0.2882 0.0191 Uiso 1.0000 H loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 N1 1_555 2.187(15) N Fe1 N3 1_555 2.155(15) N Fe1 N5 1_555 2.191(15) N Fe1 N6 1_555 2.221(15) N Fe1 N8 1_555 2.143(15) N Fe1 N10 1_555 2.213(15) N N1 Fe1 1_555 2.187(15) N N1 N2 1_555 1.371(13) N N1 C1 1_555 1.344(16) N N1 C2 1_555 2.191(14) N N1 C3 1_555 2.199(15) N N1 C4 1_555 2.13(12) N N2 N1 1_555 1.371(13) N N2 C1 1_555 2.196(15) N N2 C2 1_555 2.189(14) N N2 C3 1_555 1.346(16) N N2 C4 1_555 1.414(16) N N2 C5 1_555 2.15(10) N C1 N1 1_555 1.344(16) N C1 N2 1_555 2.196(15) N C1 C2 1_555 1.365(14) N C1 C3 1_555 2.205(14) N C2 N1 1_555 2.191(14) N C2 N2 1_555 2.189(14) N C2 C1 1_555 1.365(14) N C2 C3 1_555 1.362(14) N C3 N1 1_555 2.199(15) N C3 N2 1_555 1.346(16) N C3 C1 1_555 2.205(14) N C3 C2 1_555 1.362(14) N N3 Fe1 1_555 2.155(15) N N3 C4 1_555 1.326(16) N N3 C8 1_555 1.320(16) N N3 N4 1_555 2.11(18) N C4 N1 1_555 2.13(12) N C4 N2 1_555 1.414(16) N C4 N3 1_555 1.326(16) N C4 C5 1_555 1.392(16) N C5 N2 1_555 2.15(10) N C5 C4 1_555 1.392(16) N C5 N11 1_555 1.335(16) N N11 C5 1_555 1.335(16) N N11 C7 1_555 1.340(16) N C7 N11 1_555 1.340(16) N C7 C8 1_555 1.376(16) N C8 N3 1_555 1.320(16) N C8 C7 1_555 1.376(16) N C8 N4 1_555 1.412(16) N N4 N3 1_555 2.11(18) N N4 C8 1_555 1.412(16) N N4 N5 1_555 1.372(13) N N4 C9 1_555 1.335(16) N N4 C10 1_555 2.187(15) N N5 Fe1 1_555 2.191(15) N N5 N4 1_555 1.372(13) N N5 C9 1_555 2.191(15) N N5 C10 1_555 2.187(15) N N5 C11 1_555 1.351(16) N C9 N4 1_555 1.335(16) N C9 N5 1_555 2.191(15) N C9 C10 1_555 1.366(14) N C9 C11 1_555 2.205(14) N C10 N4 1_555 2.187(15) N C10 N5 1_555 2.187(15) N C10 C9 1_555 1.366(14) N C10 C11 1_555 1.360(14) N N6 Fe1 1_555 2.221(15) N N6 N7 1_555 1.375(13) N N6 C12 1_555 1.358(16) N N7 N6 1_555 1.375(13) N N7 C13 1_555 2.199(14) N N7 C14 1_555 1.350(16) N N7 C15 1_555 1.431(16) N C11 N5 1_555 1.351(16) N C11 C9 1_555 2.205(14) N C11 C10 1_555 1.360(14) N C12 N6 1_555 1.358(16) N C12 C13 1_555 1.365(14) N C12 C14 1_555 2.208(14) N C13 N7 1_555 2.199(14) N C13 C12 1_555 1.365(14) N C13 C14 1_555 1.365(14) N C14 N7 1_555 1.350(16) N C14 C12 1_555 2.208(14) N C14 C13 1_555 1.365(14) N N8 Fe1 1_555 2.143(15) N N8 C15 1_555 1.327(16) N N8 C19 1_555 1.326(16) N C15 N7 1_555 1.431(16) N C15 N8 1_555 1.327(16) N C15 C16 1_555 1.376(16) N C16 C15 1_555 1.376(16) N C16 N17 1_555 1.344(16) N N17 C16 1_555 1.344(16) N N17 C18 1_555 1.345(16) N C18 N17 1_555 1.345(16) N C18 C19 1_555 1.381(16) N C19 N8 1_555 1.326(16) N C19 C18 1_555 1.381(16) N C19 N9 1_555 1.439(16) N N9 C19 1_555 1.439(16) N N9 N10 1_555 1.380(13) N N9 C20 1_555 1.345(16) N N9 C21 1_555 2.194(14) N N10 Fe1 1_555 2.213(15) N N10 N9 1_555 1.380(13) N N10 C21 1_555 2.195(15) N N10 C22 1_555 1.353(16) N C20 N9 1_555 1.345(16) N C20 C21 1_555 1.365(14) N C20 C22 1_555 2.211(14) N C21 N9 1_555 2.194(14) N C21 N10 1_555 2.195(15) N C21 C20 1_555 1.365(14) N C21 C22 1_555 1.367(14) N C22 N10 1_555 1.353(16) N C22 C20 1_555 2.211(14) N C22 C21 1_555 1.367(14) N Cl1 O1 1_555 1.403(16) N Cl1 O2 1_555 1.414(16) N Cl1 O3 1_555 1.404(16) N Cl1 O4 1_555 1.386(16) N O1 Cl1 1_555 1.403(16) N O2 Cl1 1_555 1.414(16) N O3 Cl1 1_555 1.404(16) N O4 Cl1 1_555 1.386(16) N Cl2 O5 1_555 1.397(16) N Cl2 O6 1_555 1.402(16) N Cl2 O7 1_555 1.401(16) N Cl2 O8 1_555 1.399(16) N O5 Cl2 1_555 1.397(16) N O6 Cl2 1_555 1.402(16) N O7 Cl2 1_555 1.401(16) N O8 Cl2 1_555 1.399(16) N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 N1 C1 1_555 1_555 108.0(4) N N1 N2 C3 1_555 1_555 108.1(3) N N1 N2 C4 1_555 1_555 100(8) N C3 N2 C4 1_555 1_555 149(8) N N1 C1 C2 1_555 1_555 107.9(8) N C1 C2 C3 1_555 1_555 108.0(4) N N2 C3 C2 1_555 1_555 107.9(8) N C4 N3 C8 1_555 1_555 120.8(8) N N2 C4 N3 1_555 1_555 139(7) N N2 C4 C5 1_555 1_555 100(7) N N3 C4 C5 1_555 1_555 120.0(4) N C4 C5 N11 1_555 1_555 119.2(9) N C5 N11 C7 1_555 1_555 120.0(4) N N11 C7 C8 1_555 1_555 120.1(9) N N3 C8 C7 1_555 1_555 119.9(4) N N3 C8 N4 1_555 1_555 101(12) N C7 C8 N4 1_555 1_555 138(12) N C8 N4 N5 1_555 1_555 115(18) N C8 N4 C9 1_555 1_555 136(18) N N5 N4 C9 1_555 1_555 108.1(4) N N4 N5 C11 1_555 1_555 108.1(4) N N4 C9 C10 1_555 1_555 108.1(9) N C9 C10 C11 1_555 1_555 108.0(4) N N7 N6 C12 1_555 1_555 107.9(4) N N6 N7 C14 1_555 1_555 107.9(4) N N6 N7 C15 1_555 1_555 108(14) N C14 N7 C15 1_555 1_555 141(14) N N5 C11 C10 1_555 1_555 107.5(8) N N6 C12 C13 1_555 1_555 107.9(8) N C12 C13 C14 1_555 1_555 107.9(4) N N7 C14 C13 1_555 1_555 108.2(8) N Fe1 N8 C15 1_555 1_555 117(16) N Fe1 N8 C19 1_555 1_555 121(16) N C15 N8 C19 1_555 1_555 121.1(8) N N7 C15 N8 1_555 1_555 121(19) N N7 C15 C16 1_555 1_555 119(19) N N8 C15 C16 1_555 1_555 119.9(4) N C15 C16 N17 1_555 1_555 119.4(10) N C16 N17 C18 1_555 1_555 120.1(4) N N17 C18 C19 1_555 1_555 119.3(9) N N8 C19 C18 1_555 1_555 119.8(4) N N8 C19 N9 1_555 1_555 12E1(2) N C18 C19 N9 1_555 1_555 12E1(2) N C19 N9 N10 1_555 1_555 111(16) N C19 N9 C20 1_555 1_555 141(16) N N10 N9 C20 1_555 1_555 108.0(4) N N9 N10 C22 1_555 1_555 107.9(4) N N9 C20 C21 1_555 1_555 108.1(8) N C20 C21 C22 1_555 1_555 108.0(4) N N10 C22 C21 1_555 1_555 107.6(9) N O1 Cl1 O2 1_555 1_555 109.6(3) N O1 Cl1 O3 1_555 1_555 109.5(3) N O1 Cl1 O4 1_555 1_555 109.4(3) N O2 Cl1 O3 1_555 1_555 109.6(3) N O2 Cl1 O4 1_555 1_555 109.4(3) N O3 Cl1 O4 1_555 1_555 109.4(3) N O5 Cl2 O6 1_555 1_555 109.6(3) N O5 Cl2 O7 1_555 1_555 109.5(3) N O5 Cl2 O8 1_555 1_555 109.4(3) N O6 Cl2 O7 1_555 1_555 109.4(3) N O6 Cl2 O8 1_555 1_555 109.5(3) N O7 Cl2 O8 1_555 1_555 109.5(3) N