# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2298 data_global #============================================================================== #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name ; Dr. Y. Garcia ; _publ_contact_author_address ; Institut für Anorganische Chemie und Analytische Chemie Johannes-Gutenberg Universität Staudingerweg 9 55099 Mainz Germany ; _publ_contact_author_email 'garcia@iacgu7.chemie.uni-mainz.de' _publ_contact_author_fax '+49 6131 3922990' _publ_contact_author_phone '+49 6131 3923899' _publ_requested_journal 'Dalton Transactions' #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A new 3-D polymeric spin transition compound: [tris(1,4-bis(tetrazol-1-yl)butane-N1,N1') iron(II)] bis(perchlorate); loop_ _publ_author_name 'Petra J. van Koningsbruggen' 'Yann Garcia' 'Huub Kooijman' 'Anthony L. Spek' 'Jaap G. Haasnoot' 'Olivier Kahn' 'Jorge Linares' 'Epiphane Codjovi' 'Francois Varret' #=============================================================================== data_S1677A #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; 1,4-bis(tetrazol-1-yl)butane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H10 N8' _chemical_formula_structural ? _chemical_formula_sum 'C6 H10 N8' _chemical_formula_weight 194.22 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 5.3728(10) _cell_length_b 12.4806(10) _cell_length_c 7.2932(17) _cell_angle_alpha 90 _cell_angle_beta 114.880(16) _cell_angle_gamma 90 _cell_volume 443.66(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 204 _exptl_absorpt_coefficient_mu 0.10 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 2227 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 1012 # number of observed reflections (> n sig(I)) _reflns_number_gt 883 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[^' _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment 'H-atom refinement: see text ' _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 1012 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.276 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.066 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv N1 N Uani 0.31701(18) 0.14224(7) 0.26699(13) 1.000 0.0154(3) N2 N Uani 0.57880(19) 0.14885(8) 0.29249(15) 1.000 0.0223(3) N3 N Uani 0.6224(2) 0.24914(8) 0.26804(16) 1.000 0.0238(3) N4 N Uani 0.3936(2) 0.30877(7) 0.22707(14) 1.000 0.0205(3) C1 C Uani 0.2086(2) 0.24010(8) 0.22785(16) 1.000 0.0178(3) C2 C Uani 0.1914(2) 0.03995(8) 0.28249(16) 1.000 0.0194(3) C3 C Uani -0.0462(2) 0.01116(8) 0.08356(16) 1.000 0.0165(3) H1 H Uiso 0.029(3) 0.2551(11) 0.207(2) 1.000 0.026(4) H2A H Uiso 0.340(3) -0.0121(11) 0.323(2) 1.000 0.022(3) H2B H Uiso 0.130(3) 0.0497(10) 0.392(2) 1.000 0.026(3) H3A H Uiso -0.136(3) -0.0519(10) 0.108(2) 1.000 0.020(3) H3B H Uiso -0.183(3) 0.0685(10) 0.042(2) 1.000 0.019(3) 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 N1 0.0136(5) 0.0173(4) 0.0146(4) -0.0023(3) 0.0053(3) -0.0011(3) N2 0.0149(5) 0.0264(5) 0.0255(5) -0.0046(4) 0.0085(4) -0.0003(4) N3 0.0186(5) 0.0267(5) 0.0281(5) -0.0053(4) 0.0119(4) -0.0045(4) N4 0.0198(5) 0.0198(5) 0.0224(5) -0.0023(4) 0.0093(4) -0.0035(4) C1 0.0150(5) 0.0177(5) 0.0207(5) -0.0007(4) 0.0075(4) 0.0001(4) C2 0.0242(6) 0.0162(5) 0.0158(5) 0.0005(4) 0.0064(4) -0.0036(4) C3 0.0170(5) 0.0154(5) 0.0172(5) -0.0013(4) 0.0072(4) -0.0029(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 N2 1.3415(16) . . yes N1 C1 1.3314(14) . . yes N1 C2 1.4705(14) . . yes N2 N3 1.2994(15) . . yes N3 N4 1.3584(16) . . yes N4 C1 1.3143(16) . . yes C2 C3 1.5183(16) . . no C3 C3 1.5228(16) . 3_555 no C1 H1 0.931(17) . . no C2 H2A 0.974(16) . . no C2 H2B 0.992(15) . . no C3 H3A 0.978(14) . . no C3 H3B 0.978(15) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 N1 C1 108.17(9) . . . yes N2 N1 C2 122.08(9) . . . yes C1 N1 C2 129.75(10) . . . yes N1 N2 N3 106.22(10) . . . yes N2 N3 N4 111.05(11) . . . yes N3 N4 C1 104.94(9) . . . yes N1 C1 N4 109.62(10) . . . yes N1 C2 C3 111.14(9) . . . yes C2 C3 C3 112.46(10) . . 3_555 no N1 C1 H1 123.3(9) . . . no N4 C1 H1 127.0(9) . . . no N1 C2 H2A 105.0(9) . . . no N1 C2 H2B 105.9(8) . . . no C3 C2 H2A 112.6(8) . . . no C3 C2 H2B 111.6(9) . . . no H2A C2 H2B 110.2(12) . . . no C2 C3 H3A 107.3(8) . . . no C2 C3 H3B 110.1(8) . . . no H3A C3 H3B 106.3(13) . . . no C3 C3 H3A 110.5(8) 3_555 . . no C3 C3 H3B 110.0(8) 3_555 . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 N3 -0.16(12) . . . . no C2 N1 N2 N3 179.70(10) . . . . no N2 N1 C1 N4 0.20(12) . . . . no C2 N1 C1 N4 -179.65(10) . . . . no N2 N1 C2 C3 -117.63(11) . . . . no C1 N1 C2 C3 62.20(14) . . . . no N1 N2 N3 N4 0.07(12) . . . . no N2 N3 N4 C1 0.04(12) . . . . no N3 N4 C1 N1 -0.15(12) . . . . no N1 C2 C3 C3 65.67(11) . . . 3_555 no C2 C3 C3 C2 180.0(4) . . 3_555 3_555 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N1 N4 3.2620(15) . 4_555 no N3 C1 3.2856(18) . 1_655 no N4 C1 3.4016(16) . 4_554 no N4 N1 3.2620(15) . 4_554 no N1 H3A 2.731(13) . 3_555 no N2 H3B 2.819(15) . 1_655 no N3 H1 2.407(17) . 1_655 no N3 H3B 2.917(13) . 4_655 no N4 H3A 2.791(15) . 2_555 no N4 H2A 2.760(15) . 2_655 no N4 H2B 2.861(13) . 4_554 no N4 H3B 2.898(14) . 4_655 no C1 N3 3.2856(18) . 1_455 no C1 N4 3.4016(16) . 4_555 no C1 H3B 2.907(14) . . no C1 H3A 2.953(13) . 2_555 no C2 H2A 2.940(14) . 3_656 no H1 N3 2.407(17) . 1_455 no H2A N4 2.760(15) . 2_645 no H2A C2 2.940(14) . 3_656 no H2A H2A 2.445(19) . 3_656 no H2A H3B 2.531(19) . 3_555 no H2B N4 2.861(13) . 4_555 no H3A N4 2.791(15) . 2_545 no H3A C1 2.953(13) . 2_545 no H3A N1 2.731(13) . 3_555 no H3B N2 2.819(15) . 1_455 no H3B C1 2.907(14) . . no H3B H2A 2.531(19) . 3_555 no H3B N3 2.917(13) . 4_454 no H3B N4 2.898(14) . 4_454 no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1 N3 0.931(17) 2.407(17) 3.2856(18) 157.4(11) 1_455 yes # End of Crystallographic Information File #===END