# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Prof. Dr. K. M\"uller-Buschbaum Institut f\"ur Anorganische Chemie der Julius-Maximilians-Universit\"at D-97074 W\"urzburg ; _publ_contact_author_email k.mueller-buschbaumh@uni-wuerzburg.de _publ_section_title ; Alkaline Earth Imidazolate Coordination Polymers by Solvent Free Melt Synthesis as Host Lattices for Rare Earth Photoluminescence: x-infinite-[AE(Im)2(ImH)2-3], Mg, Ca, Sr, Ba ; _publ_contact_author_name 'Prof. Dr. K. Muller-Buschbaum' loop_ _publ_author_name 'Alexander Zurawski' 'Larissa Meyer' 'Jens-Christoph Rybak' 'Philipp R. Matthes' 'Klaus Mueller-Buschbaum' data_1 _database_code_depnum_ccdc_archive 'CCDC 844009' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris-imidazolo-di-imidazolato-Magnesium(II) ; _chemical_name_common ; Magnesium(II)-imidazolo-imidazolate coordination polymer ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Mg N10' _chemical_formula_weight 362.70 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.122(5) _cell_length_b 8.3816(17) _cell_length_c 17.332(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.05(3) _cell_angle_gamma 90.00 _cell_volume 3490.5(12) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 10941 _cell_measurement_theta_min 5.14 _cell_measurement_theta_max 50.00 _exptl_crystal_description ingotlike _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; high temperature melt synthesis ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method '1.5 deg omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 10941 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2960 _reflns_number_gt 2060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE SOFTWARE' _computing_cell_refinement 'STOE SOFTWARE' _computing_data_reduction 'STOE SOFTWARE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics POVRAY _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2960 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mg1 Mg 0.2500 0.7500 0.5000 0.0262(3) Uani 1 2 d S . . Mg2 Mg 0.5000 0.5000 0.5000 0.0224(2) Uani 1 2 d S . . N1 N 0.33327(7) 0.6993(2) 0.46188(10) 0.0282(4) Uani 1 1 d . . . N2 N 0.42241(6) 0.6155(2) 0.46432(9) 0.0245(4) Uani 1 1 d . . . N3 N 0.21117(7) 0.6618(2) 0.38969(10) 0.0286(4) Uani 1 1 d . . . N4 N 0.14576(8) 0.5745(3) 0.29858(11) 0.0355(5) Uani 1 1 d . . . N5 N 0.25577(7) 0.9932(2) 0.44744(10) 0.0304(4) Uani 1 1 d . . . N6 N 0.24136(9) 1.2088(3) 0.37642(12) 0.0425(5) Uani 1 1 d . . . N7 N 0.47526(7) 0.3005(2) 0.42171(10) 0.0262(4) Uani 1 1 d . . . N8 N 0.43565(8) 0.1731(3) 0.32021(11) 0.0319(4) Uani 1 1 d . . . N9 N 0.54220(7) 0.6140(2) 0.40524(10) 0.0264(4) Uani 1 1 d . . . N10 N 0.58818(8) 0.7860(3) 0.33947(11) 0.0351(5) Uani 1 1 d . . . C1 C 0.37216(8) 0.5982(3) 0.49137(12) 0.0273(5) Uani 1 1 d . . . C2 C 0.41428(9) 0.7378(3) 0.41239(12) 0.0312(5) Uani 1 1 d . . . C3 C 0.36057(9) 0.7887(3) 0.41116(12) 0.0326(5) Uani 1 1 d . . . C4 C 0.15730(9) 0.6445(3) 0.36725(13) 0.0347(6) Uani 1 1 d . . . C5 C 0.19771(10) 0.5444(3) 0.27481(13) 0.0389(6) Uani 1 1 d . . . C6 C 0.23690(9) 0.5985(3) 0.32967(13) 0.0344(6) Uani 1 1 d . . . C7 C 0.22344(10) 1.0607(3) 0.39127(13) 0.0346(6) Uani 1 1 d . . . C8 C 0.28779(11) 1.2371(4) 0.42436(15) 0.0420(6) Uani 1 1 d . . . H1 H 0.3648(10) 0.516(3) 0.5312(14) 0.036(7) Uiso 1 1 d . . . H2 H 0.4445(11) 0.779(3) 0.3829(14) 0.038(7) Uiso 1 1 d . . . H14 H 0.5933(11) 0.647(4) 0.2417(17) 0.047(7) Uiso 1 1 d . . . H13 H 0.5659(10) 0.828(4) 0.4463(15) 0.041(7) Uiso 1 1 d . . . H3 H 0.3419(10) 0.875(3) 0.3818(14) 0.033(6) Uiso 1 1 d . . . H4 H 0.1281(11) 0.672(3) 0.3999(15) 0.040(7) Uiso 1 1 d . . . H12 H 0.5391(10) 0.135(3) 0.4441(14) 0.039(7) Uiso 1 1 d . . . H7 H 0.1916(11) 1.010(3) 0.3641(14) 0.039(7) Uiso 1 1 d . . . H8 H 0.4086(14) 0.145(4) 0.2755(19) 0.071(10) Uiso 1 1 d . . . H10A H 0.4029(11) 0.383(4) 0.3597(14) 0.039(7) Uiso 1 1 d . . . H6A H 0.2772(12) 0.597(4) 0.3309(15) 0.046(7) Uiso 1 1 d . . . H11 H 0.4897(11) -0.008(4) 0.3250(16) 0.046(8) Uiso 1 1 d . . . H9 H 0.3251(12) 1.078(4) 0.5102(17) 0.057(8) Uiso 1 1 d . . . H5 H 0.2016(11) 0.503(4) 0.2253(17) 0.049(8) Uiso 1 1 d . . . H10 H 0.6048(13) 0.880(4) 0.3283(18) 0.058(9) Uiso 1 1 d . . . H8A H 0.3058(13) 1.335(4) 0.4264(17) 0.057(9) Uiso 1 1 d . . . H15 H 0.5391(12) 0.437(4) 0.3171(16) 0.053(8) Uiso 1 1 d . . . H6 H 0.2254(14) 1.290(5) 0.339(2) 0.070(10) Uiso 1 1 d . . . C9 C 0.29613(10) 1.1049(3) 0.46770(15) 0.0387(6) Uani 1 1 d . . . C10 C 0.43343(9) 0.2996(3) 0.36698(12) 0.0295(5) Uani 1 1 d . . . C11 C 0.48128(9) 0.0858(3) 0.34702(13) 0.0325(5) Uani 1 1 d . . . C12 C 0.50534(9) 0.1651(3) 0.40927(12) 0.0286(5) Uani 1 1 d . . . C13 C 0.56506(9) 0.7561(3) 0.40545(13) 0.0304(5) Uani 1 1 d . . . C14 C 0.58031(10) 0.6533(3) 0.29387(14) 0.0403(6) Uani 1 1 d . . . C15 C 0.55170(9) 0.5487(3) 0.33475(12) 0.0349(6) Uani 1 1 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 Mg1 0.0182(4) 0.0326(7) 0.0272(5) -0.0031(4) -0.0005(4) 0.0047(4) Mg2 0.0176(4) 0.0238(6) 0.0260(5) 0.0010(4) 0.0022(3) 0.0010(4) N1 0.0203(8) 0.0364(13) 0.0274(9) 0.0002(8) -0.0002(7) 0.0056(7) N2 0.0181(8) 0.0282(11) 0.0271(9) -0.0011(7) 0.0019(6) 0.0011(7) N3 0.0255(9) 0.0306(12) 0.0290(9) -0.0011(8) -0.0009(7) 0.0018(7) N4 0.0335(10) 0.0398(14) 0.0317(10) 0.0006(9) -0.0048(8) -0.0072(8) N5 0.0251(9) 0.0317(12) 0.0345(9) -0.0026(8) 0.0045(7) 0.0035(8) N6 0.0517(13) 0.0370(15) 0.0408(11) 0.0033(10) 0.0161(10) 0.0045(10) N7 0.0228(8) 0.0265(12) 0.0295(9) -0.0003(7) 0.0032(7) -0.0009(7) N8 0.0317(9) 0.0313(13) 0.0317(10) -0.0029(8) -0.0035(8) -0.0002(8) N9 0.0228(8) 0.0278(12) 0.0290(9) 0.0031(8) 0.0039(7) 0.0015(7) N10 0.0319(10) 0.0342(14) 0.0402(11) 0.0097(9) 0.0079(8) -0.0019(9) C1 0.0190(9) 0.0305(14) 0.0324(11) -0.0013(10) 0.0016(8) 0.0028(8) C2 0.0251(11) 0.0382(15) 0.0306(11) 0.0070(10) 0.0041(9) 0.0061(9) C3 0.0281(10) 0.0413(17) 0.0285(11) 0.0080(10) 0.0041(9) 0.0120(10) C4 0.0249(11) 0.0413(17) 0.0367(12) -0.0057(10) -0.0049(9) 0.0003(9) C5 0.0414(13) 0.0485(18) 0.0273(11) -0.0042(11) 0.0059(9) -0.0137(11) C6 0.0299(12) 0.0441(17) 0.0294(11) -0.0037(10) 0.0038(9) -0.0055(10) C7 0.0312(12) 0.0378(16) 0.0354(12) 0.0003(10) 0.0074(9) 0.0028(10) C8 0.0448(14) 0.0368(19) 0.0463(14) -0.0083(12) 0.0145(11) -0.0072(12) C9 0.0334(12) 0.0383(17) 0.0450(14) -0.0093(11) 0.0067(10) -0.0033(10) C10 0.0240(10) 0.0323(15) 0.0318(11) -0.0027(10) 0.0004(8) -0.0009(9) C11 0.0365(12) 0.0261(16) 0.0344(12) -0.0034(10) 0.0008(9) 0.0045(10) C12 0.0276(10) 0.0259(14) 0.0319(11) -0.0012(9) 0.0009(9) 0.0015(9) C13 0.0269(11) 0.0293(15) 0.0354(12) 0.0035(10) 0.0049(9) 0.0030(9) C14 0.0431(13) 0.0460(19) 0.0329(12) 0.0055(11) 0.0104(10) -0.0042(11) C15 0.0357(12) 0.0423(17) 0.0276(11) 0.0004(10) 0.0069(9) -0.0043(10) _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 Mg1 N3 2.1827(18) . ? Mg1 N3 2.1827(18) 7_566 ? Mg1 N1 2.2101(17) 7_566 ? Mg1 N1 2.2101(17) . ? Mg1 N5 2.242(2) . ? Mg1 N5 2.242(2) 7_566 ? Mg2 N2 2.1490(17) . ? Mg2 N2 2.1490(17) 5_666 ? Mg2 N7 2.2023(19) 5_666 ? Mg2 N7 2.2023(19) . ? Mg2 N9 2.2226(18) 5_666 ? Mg2 N9 2.2226(18) . ? N1 C1 1.332(3) . ? N1 C3 1.368(3) . ? N2 C1 1.345(3) . ? N2 C2 1.367(3) . ? N3 C4 1.331(3) . ? N3 C6 1.365(3) . ? N4 C4 1.334(3) . ? N4 C5 1.376(3) . ? N5 C7 1.320(3) . ? N5 C9 1.374(3) . ? N6 C7 1.347(4) . ? N6 C8 1.355(4) . ? N7 C10 1.323(3) . ? N7 C12 1.374(3) . ? N8 C10 1.339(3) . ? N8 C11 1.368(3) . ? N9 C13 1.313(3) . ? N9 C15 1.376(3) . ? N10 C13 1.339(3) . ? N10 C14 1.368(4) . ? C2 C3 1.362(3) . ? C5 C6 1.358(3) . ? C8 C9 1.344(4) . ? C11 C12 1.354(3) . ? C14 C15 1.354(4) . ? 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 N3 Mg1 N3 180.0 . 7_566 ? N3 Mg1 N1 89.75(7) . 7_566 ? N3 Mg1 N1 90.25(7) 7_566 7_566 ? N3 Mg1 N1 90.25(7) . . ? N3 Mg1 N1 89.75(7) 7_566 . ? N1 Mg1 N1 180.0 7_566 . ? N3 Mg1 N5 89.39(7) . . ? N3 Mg1 N5 90.61(7) 7_566 . ? N1 Mg1 N5 92.13(7) 7_566 . ? N1 Mg1 N5 87.87(7) . . ? N3 Mg1 N5 90.61(7) . 7_566 ? N3 Mg1 N5 89.39(7) 7_566 7_566 ? N1 Mg1 N5 87.87(7) 7_566 7_566 ? N1 Mg1 N5 92.13(7) . 7_566 ? N5 Mg1 N5 180.00(4) . 7_566 ? N2 Mg2 N2 180.000(1) . 5_666 ? N2 Mg2 N7 90.99(7) . 5_666 ? N2 Mg2 N7 89.01(7) 5_666 5_666 ? N2 Mg2 N7 89.01(7) . . ? N2 Mg2 N7 90.99(7) 5_666 . ? N7 Mg2 N7 180.000(1) 5_666 . ? N2 Mg2 N9 87.84(7) . 5_666 ? N2 Mg2 N9 92.16(6) 5_666 5_666 ? N7 Mg2 N9 89.31(7) 5_666 5_666 ? N7 Mg2 N9 90.69(7) . 5_666 ? N2 Mg2 N9 92.16(6) . . ? N2 Mg2 N9 87.84(6) 5_666 . ? N7 Mg2 N9 90.69(7) 5_666 . ? N7 Mg2 N9 89.31(7) . . ? N9 Mg2 N9 180.000(1) 5_666 . ? C1 N1 C3 103.44(17) . . ? C1 N1 Mg1 129.45(15) . . ? C3 N1 Mg1 126.05(15) . . ? C1 N2 C2 103.21(17) . . ? C1 N2 Mg2 129.78(15) . . ? C2 N2 Mg2 126.74(13) . . ? C4 N3 C6 103.45(18) . . ? C4 N3 Mg1 128.72(15) . . ? C6 N3 Mg1 127.62(14) . . ? C4 N4 C5 102.92(18) . . ? C7 N5 C9 104.8(2) . . ? C7 N5 Mg1 129.46(17) . . ? C9 N5 Mg1 125.70(16) . . ? C7 N6 C8 107.8(2) . . ? C10 N7 C12 105.22(18) . . ? C10 N7 Mg2 126.47(15) . . ? C12 N7 Mg2 127.27(13) . . ? C10 N8 C11 106.96(19) . . ? C13 N9 C15 105.11(19) . . ? C13 N9 Mg2 127.42(15) . . ? C15 N9 Mg2 127.44(17) . . ? C13 N10 C14 107.1(2) . . ? N1 C1 N2 115.1(2) . . ? C3 C2 N2 109.06(19) . . ? C2 C3 N1 109.2(2) . . ? N3 C4 N4 115.5(2) . . ? C6 C5 N4 109.0(2) . . ? C5 C6 N3 109.1(2) . . ? N5 C7 N6 110.9(2) . . ? C9 C8 N6 105.9(2) . . ? C8 C9 N5 110.5(2) . . ? N7 C10 N8 111.7(2) . . ? C12 C11 N8 106.5(2) . . ? C11 C12 N7 109.60(19) . . ? N9 C13 N10 112.0(2) . . ? C15 C14 N10 106.0(2) . . ? C14 C15 N9 109.8(2) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.262 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.047 # Attachment '7174_web_deposit_cif_file_1_Prof.Dr.KlausMueller-Buschbaum_1315931615.Ca-Im_AZ20M.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 844010' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-imidazolo-di-imidazolato-Calcium(II) ; _chemical_name_common ; Calcium(II)-imidazolo-imidazolate network ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Ca N8' _chemical_formula_weight 310.39 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0134(18) _cell_length_b 8.6684(17) _cell_length_c 10.313(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.68(3) _cell_angle_gamma 90.00 _cell_volume 732.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 5888 _cell_measurement_theta_min 4.98 _cell_measurement_theta_max 54.98 _exptl_crystal_description blocklike _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; high-temperature melt synthesis ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method '1.5 deg omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 5888 _diffrn_reflns_av_R_equivalents 0.2005 _diffrn_reflns_av_sigmaI/netI 0.2310 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1674 _reflns_number_gt 678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE SOFTWARE' _computing_cell_refinement 'STOE SOFTWARE' _computing_data_reduction 'STOE SOFTWARE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics POVRAY _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1674 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1428 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Ca1 Ca 0.5000 0.5000 0.5000 0.0270(3) Uani 1 2 d S . . N1 N 0.6206(5) 0.6385(5) 0.7322(3) 0.0339(10) Uani 1 1 d . . . N2 N 0.6321(5) 0.8166(5) 0.8966(4) 0.0389(11) Uani 1 1 d . . . N3 N 0.7402(5) 0.3290(5) 0.5788(4) 0.0417(11) Uani 1 1 d . . . N4 N 0.9779(6) 0.2412(6) 0.6082(5) 0.0625(15) Uani 1 1 d . . . H4 H 1.0692 0.2339 0.6007 0.075 Uiso 1 1 calc R . . C1 C 0.5864(6) 0.7775(6) 0.7578(4) 0.0377(12) Uani 1 1 d . . . H1 H 0.5331 0.8471 0.6844 0.045 Uiso 1 1 calc R . . C3 C 0.6972(6) 0.5709(6) 0.8666(4) 0.0367(12) Uani 1 1 d . . . H3 H 0.7367 0.4705 0.8869 0.044 Uiso 1 1 calc R . . C2 C 0.7026(6) 0.6830(6) 0.9637(4) 0.0364(12) Uani 1 1 d . . . H2 H 0.7485 0.6691 1.0621 0.044 Uiso 1 1 calc R . . C4 C 0.8624(7) 0.3448(7) 0.5451(5) 0.0488(14) Uani 1 1 d . . . H4A H 0.8684 0.4204 0.4835 0.059 Uiso 1 1 calc R . . C6 C 0.7815(8) 0.2037(7) 0.6677(5) 0.0524(15) Uani 1 1 d . . . H6 H 0.7168 0.1622 0.7095 0.063 Uiso 1 1 calc R . . C5 C 0.9268(9) 0.1496(8) 0.6859(6) 0.068(2) Uani 1 1 d . . . H5 H 0.9817 0.0655 0.7412 0.082 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 Ca1 0.0293(7) 0.0350(7) 0.0175(5) 0.0004(7) 0.0104(4) 0.0002(8) N1 0.035(3) 0.036(2) 0.0247(18) -0.0024(17) 0.0076(17) 0.0039(19) N2 0.042(3) 0.049(3) 0.0275(18) -0.0109(18) 0.0155(17) 0.001(2) N3 0.037(3) 0.057(3) 0.031(2) 0.003(2) 0.0139(18) 0.009(2) N4 0.037(3) 0.083(4) 0.060(3) -0.012(3) 0.013(2) 0.010(3) C1 0.041(3) 0.046(3) 0.026(2) 0.002(2) 0.014(2) 0.008(2) C3 0.042(3) 0.034(3) 0.029(2) 0.000(2) 0.010(2) -0.002(2) C2 0.039(3) 0.047(3) 0.023(2) -0.002(2) 0.013(2) 0.005(3) C4 0.046(4) 0.063(4) 0.037(3) 0.003(3) 0.018(2) 0.006(3) C6 0.053(4) 0.062(4) 0.046(3) 0.012(3) 0.024(3) 0.016(3) C5 0.065(5) 0.074(5) 0.053(3) 0.014(3) 0.012(3) 0.032(4) _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. X-H bonds and H-Y-H angles not given due to geometric calculation of H atom positions. ; 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 Ca1 N3 2.465(4) 3_666 ? Ca1 N3 2.465(4) . ? Ca1 N2 2.478(4) 4_575 ? Ca1 N2 2.478(4) 2_646 ? Ca1 N1 2.487(3) 3_666 ? Ca1 N1 2.487(3) . ? N1 C1 1.298(6) . ? N1 C3 1.394(5) . ? N2 C1 1.357(5) . ? N2 C2 1.363(6) . ? N2 Ca1 2.478(4) 2_656 ? N3 C4 1.293(7) . ? N3 C6 1.369(6) . ? N4 C4 1.322(7) . ? N4 C5 1.339(8) . ? C3 C2 1.382(6) . ? C6 C5 1.329(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ca1 N3 180.000(1) 3_666 . ? N3 Ca1 N2 89.21(14) 3_666 4_575 ? N3 Ca1 N2 90.79(14) . 4_575 ? N3 Ca1 N2 90.79(14) 3_666 2_646 ? N3 Ca1 N2 89.21(14) . 2_646 ? N2 Ca1 N2 180.00(15) 4_575 2_646 ? N3 Ca1 N1 90.14(13) 3_666 3_666 ? N3 Ca1 N1 89.86(13) . 3_666 ? N2 Ca1 N1 89.46(13) 4_575 3_666 ? N2 Ca1 N1 90.54(13) 2_646 3_666 ? N3 Ca1 N1 89.86(13) 3_666 . ? N3 Ca1 N1 90.14(13) . . ? N2 Ca1 N1 90.54(13) 4_575 . ? N2 Ca1 N1 89.46(13) 2_646 . ? N1 Ca1 N1 180.000(1) 3_666 . ? C1 N1 C3 104.4(4) . . ? C1 N1 Ca1 126.8(3) . . ? C3 N1 Ca1 126.2(3) . . ? C1 N2 C2 101.2(4) . . ? C1 N2 Ca1 128.7(3) . 2_656 ? C2 N2 Ca1 122.2(3) . 2_656 ? C4 N3 C6 103.9(5) . . ? C4 N3 Ca1 125.2(4) . . ? C6 N3 Ca1 130.8(4) . . ? C4 N4 C5 107.5(6) . . ? N1 C1 N2 117.0(4) . . ? C2 C3 N1 106.1(4) . . ? N2 C2 C3 111.2(4) . . ? N3 C4 N4 112.3(5) . . ? C5 C6 N3 110.5(6) . . ? C6 C5 N4 105.7(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.383 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.087 # Attachment '7175_web_deposit_cif_file_2_ #Prof.Dr.KlausMueller-Buschbaum_1315931615.SrIm_TT_AZ24.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 844011' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-imidazolo-di-imidazolato-Strontium(II) ; _chemical_name_common ; Strontium(II)-imidazolo-imidazolate network ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 N8 Sr' _chemical_formula_weight 357.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 10.562(2) _cell_length_b 10.559(2) _cell_length_c 13.894(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.28(3) _cell_angle_gamma 90.00 _cell_volume 1543.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7634 _cell_measurement_theta_min 7.72 _cell_measurement_theta_max 52.62 _exptl_crystal_description platelike _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 3.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; high-temperature melt synthesis ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXford Xcalibur' _diffrn_measurement_method '1.5 deg omega and theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 7634 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 26.31 _reflns_number_total 3115 _reflns_number_gt 1825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SOFTWARE' _computing_cell_refinement 'BRUKER SOFTWARE' _computing_data_reduction 'BRUKER SOFTWARE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics POVRAY _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3115 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0476 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 0.773 _refine_ls_restrained_S_all 0.773 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Sr1 Sr 0.49539(3) 0.71067(2) 0.74856(3) 0.01531(7) Uani 1 1 d . . . N2 N 0.8384(2) 0.4000(2) 0.74520(17) 0.0232(6) Uani 1 1 d . . . N5 N 0.4550(2) 0.7345(3) 0.55929(19) 0.0288(7) Uani 1 1 d . . . N6 N 0.3535(3) 0.7281(3) 0.4145(2) 0.0336(7) Uani 1 1 d . . . N3 N 0.3285(2) 0.5283(2) 0.72365(18) 0.0255(7) Uani 1 1 d . . . N4 N 0.1778(2) 0.3753(2) 0.71324(18) 0.0270(7) Uani 1 1 d . . . C6 C 0.3710(3) 0.4255(3) 0.6763(2) 0.0287(8) Uani 1 1 d . . . N1 N 0.6864(2) 0.5513(2) 0.74548(18) 0.0220(7) Uani 1 1 d . . . N7 N 0.5292(2) 0.6932(3) 0.93946(19) 0.0288(7) Uani 1 1 d . . . C2 C 0.8576(3) 0.4894(3) 0.6765(2) 0.0247(8) Uani 1 1 d . . . C12 C 0.4811(3) 0.7740(4) 1.0048(3) 0.0382(10) Uani 1 1 d . . . C4 C 0.2122(3) 0.4915(3) 0.7422(2) 0.0250(8) Uani 1 1 d . . . C8 C 0.4320(3) 0.8280(4) 0.4149(3) 0.0335(9) Uani 1 1 d . . . C9 C 0.4944(3) 0.8315(3) 0.5034(3) 0.0324(9) Uani 1 1 d . . . C1 C 0.7345(3) 0.4430(3) 0.7834(2) 0.0228(7) Uani 1 1 d . . . C7 C 0.3699(3) 0.6742(3) 0.5017(3) 0.0347(10) Uani 1 1 d . . . N8 N 0.6071(3) 0.6465(4) 1.0858(2) 0.0465(9) Uani 1 1 d . . . C11 C 0.5289(4) 0.7452(4) 1.0945(3) 0.0395(10) Uani 1 1 d . . . C10 C 0.6057(4) 0.6191(4) 0.9927(3) 0.0432(11) Uani 1 1 d . . . C5 C 0.2811(3) 0.3347(3) 0.6702(2) 0.0275(8) Uani 1 1 d . . . C3 C 0.7665(3) 0.5787(3) 0.6760(2) 0.0282(8) Uani 1 1 d . . . H7 H 0.326(2) 0.604(3) 0.5168(19) 0.026(9) Uiso 1 1 d . . . H3 H 0.755(2) 0.650(3) 0.6346(19) 0.037(9) Uiso 1 1 d . . . H5 H 0.283(3) 0.259(3) 0.641(2) 0.028(9) Uiso 1 1 d . . . H4 H 0.164(2) 0.542(2) 0.7778(17) 0.012(8) Uiso 1 1 d . . . H9 H 0.547(2) 0.886(2) 0.5255(19) 0.022(9) Uiso 1 1 d . . . H12 H 0.425(3) 0.836(3) 0.988(2) 0.040(10) Uiso 1 1 d . . . H2 H 0.922(2) 0.483(2) 0.6345(17) 0.022(8) Uiso 1 1 d . . . H11 H 0.519(3) 0.783(3) 1.149(2) 0.041(10) Uiso 1 1 d . . . H6 H 0.303(3) 0.705(3) 0.372(2) 0.041(11) Uiso 1 1 d . . . H6A H 0.441(3) 0.423(3) 0.6536(19) 0.025(9) Uiso 1 1 d . . . H1 H 0.697(2) 0.404(2) 0.8357(18) 0.019(8) Uiso 1 1 d . . . H10 H 0.637(3) 0.548(3) 0.965(2) 0.074(14) Uiso 1 1 d . . . H8A H 0.437(3) 0.882(3) 0.3655(19) 0.034(9) Uiso 1 1 d . . . H8 H 0.644(3) 0.610(3) 1.126(2) 0.045(13) Uiso 1 1 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 Sr1 0.01302(12) 0.01225(12) 0.02043(12) 0.00075(18) 0.00034(8) -0.00014(17) N2 0.0227(14) 0.0191(16) 0.0280(16) -0.0002(13) 0.0026(12) 0.0043(12) N5 0.0351(16) 0.0274(17) 0.0225(16) 0.0012(13) -0.0050(13) -0.0073(14) N6 0.0308(16) 0.041(2) 0.0269(17) -0.0033(16) -0.0098(14) 0.0002(16) N3 0.0209(15) 0.0191(16) 0.0365(17) -0.0042(14) 0.0033(13) -0.0062(13) N4 0.0195(14) 0.0178(15) 0.0438(18) 0.0005(14) 0.0037(13) -0.0053(12) C6 0.0182(19) 0.032(2) 0.036(2) 0.0036(17) 0.0064(17) -0.0017(17) N1 0.0166(14) 0.0198(16) 0.0298(16) 0.0009(13) 0.0035(12) 0.0027(12) N7 0.0343(16) 0.0295(18) 0.0228(16) 0.0030(13) 0.0043(13) 0.0061(14) C2 0.0239(18) 0.0232(19) 0.0287(19) -0.0025(16) 0.0111(16) 0.0013(15) C12 0.042(2) 0.040(3) 0.031(2) 0.003(2) -0.0019(17) 0.018(2) C4 0.0216(18) 0.0215(19) 0.032(2) -0.0007(16) 0.0026(16) 0.0028(16) C8 0.037(2) 0.034(2) 0.029(2) 0.0079(18) 0.0019(17) 0.0040(18) C9 0.037(2) 0.027(2) 0.032(2) -0.0003(19) -0.0056(17) -0.0087(18) C1 0.0234(19) 0.0197(19) 0.0252(19) 0.0001(15) 0.0016(16) -0.0001(15) C7 0.040(2) 0.030(2) 0.033(2) 0.0018(18) -0.0014(18) -0.0100(18) N8 0.058(2) 0.057(2) 0.024(2) 0.0062(19) -0.0012(16) 0.027(2) C11 0.049(2) 0.049(3) 0.020(2) -0.0090(19) 0.0020(17) 0.0122(19) C10 0.063(3) 0.037(3) 0.031(2) 0.002(2) 0.011(2) 0.019(2) C5 0.0279(19) 0.020(2) 0.035(2) -0.0057(17) 0.0028(16) -0.0018(16) C3 0.0285(19) 0.0184(19) 0.037(2) 0.0054(17) -0.0022(16) 0.0033(16) _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 Sr1 N3 2.613(2) . ? Sr1 N4 2.613(2) 2_556 ? Sr1 N1 2.630(2) . ? Sr1 N5 2.637(3) . ? Sr1 N7 2.650(3) . ? Sr1 N2 2.656(2) 2_656 ? Sr1 C6 3.399(4) . ? Sr1 C3 3.419(3) . ? N2 C1 1.341(3) . ? N2 C2 1.371(4) . ? N2 Sr1 2.656(2) 2_646 ? N5 C7 1.312(4) . ? N5 C9 1.373(4) . ? N6 C7 1.336(4) . ? N6 C8 1.342(4) . ? N3 C4 1.336(4) . ? N3 C6 1.366(4) . ? N4 C4 1.331(4) . ? N4 C5 1.360(4) . ? N4 Sr1 2.613(2) 2_546 ? C6 C5 1.347(4) . ? N1 C1 1.340(3) . ? N1 C3 1.372(4) . ? N7 C10 1.305(4) . ? N7 C12 1.376(4) . ? C2 C3 1.346(4) . ? C12 C11 1.336(5) . ? C8 C9 1.340(5) . ? N8 C10 1.324(4) . ? N8 C11 1.343(4) . ? 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 N3 Sr1 N4 92.33(8) . 2_556 ? N3 Sr1 N1 92.03(8) . . ? N4 Sr1 N1 168.85(8) 2_556 . ? N3 Sr1 N5 83.86(8) . . ? N4 Sr1 N5 95.00(8) 2_556 . ? N1 Sr1 N5 95.66(8) . . ? N3 Sr1 N7 96.22(8) . . ? N4 Sr1 N7 82.84(8) 2_556 . ? N1 Sr1 N7 86.50(9) . . ? N5 Sr1 N7 177.83(9) . . ? N3 Sr1 N2 174.23(8) . 2_656 ? N4 Sr1 N2 88.03(8) 2_556 2_656 ? N1 Sr1 N2 88.65(8) . 2_656 ? N5 Sr1 N2 90.36(8) . 2_656 ? N7 Sr1 N2 89.55(8) . 2_656 ? N3 Sr1 C6 21.59(7) . . ? N4 Sr1 C6 112.97(8) 2_556 . ? N1 Sr1 C6 72.83(8) . . ? N5 Sr1 C6 76.57(8) . . ? N7 Sr1 C6 104.27(8) . . ? N2 Sr1 C6 155.85(8) 2_656 . ? N3 Sr1 C3 103.52(8) . . ? N4 Sr1 C3 162.18(8) 2_556 . ? N1 Sr1 C3 21.57(7) . . ? N5 Sr1 C3 78.92(8) . . ? N7 Sr1 C3 103.14(9) . . ? N2 Sr1 C3 75.38(8) 2_656 . ? C6 Sr1 C3 82.15(8) . . ? C1 N2 C2 102.7(3) . . ? C1 N2 Sr1 143.5(2) . 2_646 ? C2 N2 Sr1 113.69(19) . 2_646 ? C7 N5 C9 104.1(3) . . ? C7 N5 Sr1 126.9(2) . . ? C9 N5 Sr1 127.3(2) . . ? C7 N6 C8 107.6(3) . . ? C4 N3 C6 102.2(3) . . ? C4 N3 Sr1 144.1(2) . . ? C6 N3 Sr1 113.7(2) . . ? C4 N4 C5 102.5(3) . . ? C4 N4 Sr1 136.7(2) . 2_546 ? C5 N4 Sr1 119.0(2) . 2_546 ? C5 C6 N3 109.6(3) . . ? C5 C6 Sr1 154.2(3) . . ? N3 C6 Sr1 44.73(15) . . ? C1 N1 C3 102.7(3) . . ? C1 N1 Sr1 143.5(2) . . ? C3 N1 Sr1 113.63(19) . . ? C10 N7 C12 104.2(3) . . ? C10 N7 Sr1 128.9(2) . . ? C12 N7 Sr1 126.4(2) . . ? C3 C2 N2 109.5(3) . . ? C11 C12 N7 110.1(3) . . ? N4 C4 N3 116.1(3) . . ? C9 C8 N6 106.1(3) . . ? C8 C9 N5 110.5(3) . . ? N2 C1 N1 115.4(3) . . ? N5 C7 N6 111.7(3) . . ? C10 N8 C11 107.8(3) . . ? C12 C11 N8 105.9(3) . . ? N7 C10 N8 111.9(4) . . ? C6 C5 N4 109.7(3) . . ? C2 C3 N1 109.7(3) . . ? C2 C3 Sr1 154.4(3) . . ? N1 C3 Sr1 44.81(15) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.463 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.073 # Attachment '7176_web_deposit_cif_file_3_Prof.Dr.KlausMueller-Buschbaum_1315931615.Ba-Im_AZ23.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 844012' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-imidazolo-di-imidazolato-Barium(II) ; _chemical_name_common ; Barium(II)-imidazolo-imidazolate coordination polymer ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Ba N8' _chemical_formula_weight 407.65 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' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3527(19) _cell_length_b 9.6806(19) _cell_length_c 18.312(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.81(2) _cell_angle_gamma 90.00 _cell_volume 1479.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 12002 _cell_measurement_theta_min 5.16 _cell_measurement_theta_max 60.68 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.691 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; high-temperature melt synthesis ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method '1.5 deg omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 12002 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 30.34 _reflns_number_total 4099 _reflns_number_gt 2733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE SOFTWARE' _computing_cell_refinement 'STOE SOFTWARE' _computing_data_reduction 'STOE SOFTWARE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics POVRAY _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4099 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ba1 Ba -0.00478(3) 0.29019(3) 0.245090(15) 0.01453(11) Uani 1 1 d . . . N1 N -0.0030(6) 0.0590(5) 0.1548(3) 0.0210(9) Uani 1 1 d . . . N2 N 0.1338(5) -0.1154(6) 0.1304(3) 0.0220(9) Uani 1 1 d . . . N3 N 0.0004(6) 0.5611(5) 0.1594(3) 0.0234(10) Uani 1 1 d . . . N4 N 0.1257(5) 0.4066(6) 0.1144(3) 0.0222(10) Uani 1 1 d . . . N5 N 0.3332(5) 0.2468(6) 0.3330(3) 0.0222(10) Uani 1 1 d . . . N6 N 0.5940(5) 0.2784(6) 0.3753(3) 0.0207(9) Uani 1 1 d . . . H6 H 0.6853 0.2925 0.3735 0.025 Uiso 1 1 calc R . . N7 N -0.3488(5) 0.2564(6) 0.1511(3) 0.0234(10) Uani 1 1 d . . . N8 N -0.6083(5) 0.2913(6) 0.1100(3) 0.0202(9) Uani 1 1 d . . . H8 H -0.6995 0.3346 0.0966 0.024 Uiso 1 1 calc R . . C1 C 0.1403(6) -0.0019(7) 0.1741(3) 0.0217(10) Uani 1 1 d . . . H1 H 0.2383 0.0332 0.2155 0.026 Uiso 1 1 calc R . . C2 C -0.0270(5) -0.1289(6) 0.0778(3) 0.0200(10) Uani 1 1 d . . . H2 H -0.0732 -0.2000 0.0383 0.024 Uiso 1 1 calc R . . C3 C -0.1096(7) -0.0235(6) 0.0917(3) 0.0202(11) Uani 1 1 d . . . H3 H -0.2219 -0.0091 0.0627 0.024 Uiso 1 1 calc R . . C4 C 0.1390(6) 0.5087(7) 0.1675(3) 0.0202(10) Uani 1 1 d . . . H4 H 0.2398 0.5409 0.2078 0.024 Uiso 1 1 calc R . . C5 C -0.0365(6) 0.3932(7) 0.0684(3) 0.0240(11) Uani 1 1 d . . . H5 H -0.0876 0.3289 0.0251 0.029 Uiso 1 1 calc R . . C6 C -0.1132(7) 0.4862(7) 0.0942(3) 0.0212(11) Uani 1 1 d . . . H6A H -0.2260 0.4979 0.0714 0.025 Uiso 1 1 calc R . . C7 C -0.4618(6) 0.3507(7) 0.1354(3) 0.0226(11) Uani 1 1 d . . . H7 H -0.4429 0.4474 0.1412 0.027 Uiso 1 1 calc R . . C8 C -0.5874(6) 0.1528(7) 0.1093(3) 0.0228(11) Uani 1 1 d . . . H8A H -0.6681 0.0840 0.0942 0.027 Uiso 1 1 calc R . . C9 C -0.4280(6) 0.1317(7) 0.1344(3) 0.0228(10) Uani 1 1 d . . . H9 H -0.3789 0.0439 0.1396 0.027 Uiso 1 1 calc R . . C10 C 0.4477(6) 0.2694(7) 0.3108(3) 0.0226(11) Uani 1 1 d . . . H10 H 0.4288 0.2784 0.2555 0.027 Uiso 1 1 calc R . . C11 C 0.5733(6) 0.2613(6) 0.4443(3) 0.0225(11) Uani 1 1 d . . . H11 H 0.6545 0.2627 0.4994 0.027 Uiso 1 1 calc R . . C12 C 0.4128(6) 0.2418(6) 0.4183(3) 0.0198(10) Uani 1 1 d . . . H12 H 0.3632 0.2271 0.4529 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 Ba1 0.01360(14) 0.00907(17) 0.02081(15) 0.00005(11) 0.00767(10) -0.00029(11) N1 0.026(2) 0.012(3) 0.027(2) -0.0011(16) 0.0134(18) 0.0025(17) N2 0.0184(18) 0.020(3) 0.029(2) -0.0034(17) 0.0120(15) 0.0027(17) N3 0.032(2) 0.013(3) 0.030(2) -0.0023(17) 0.019(2) -0.0008(18) N4 0.0195(19) 0.019(3) 0.027(2) -0.0039(17) 0.0103(16) -0.0009(16) N5 0.0155(17) 0.027(3) 0.0230(19) 0.0017(16) 0.0073(15) -0.0016(17) N6 0.0127(16) 0.023(3) 0.0249(19) -0.0018(17) 0.0074(14) -0.0006(16) N7 0.0160(18) 0.026(3) 0.029(2) -0.0013(17) 0.0106(16) -0.0006(17) N8 0.0128(16) 0.023(3) 0.0240(19) 0.0018(17) 0.0081(14) 0.0022(16) C1 0.021(2) 0.017(3) 0.027(2) -0.001(2) 0.0108(19) -0.002(2) C2 0.018(2) 0.017(3) 0.026(2) -0.0055(19) 0.0106(17) -0.0002(19) C3 0.021(2) 0.018(3) 0.022(2) 0.0008(17) 0.0105(19) 0.0014(18) C4 0.024(2) 0.013(3) 0.026(2) 0.0001(19) 0.0133(19) -0.004(2) C5 0.022(2) 0.020(3) 0.026(2) -0.0024(19) 0.0079(18) -0.001(2) C6 0.022(2) 0.017(3) 0.026(2) 0.0055(19) 0.0118(19) 0.004(2) C7 0.020(2) 0.020(3) 0.027(2) -0.0026(19) 0.0103(17) -0.0049(19) C8 0.019(2) 0.024(3) 0.026(2) -0.001(2) 0.0106(17) -0.0015(19) C9 0.023(2) 0.019(3) 0.028(2) 0.005(2) 0.0123(18) 0.003(2) C10 0.020(2) 0.026(3) 0.025(2) 0.0008(19) 0.0130(18) -0.0030(19) C11 0.018(2) 0.024(3) 0.023(2) -0.0003(18) 0.0067(17) -0.0008(19) C12 0.022(2) 0.016(3) 0.025(2) -0.0011(17) 0.0134(18) -0.0010(18) _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. X-H bonds and H-Y-H angles not given due to geometric calculation of H atom positions. ; 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 Ba1 N1 2.787(5) . ? Ba1 N3 2.813(5) 2_545 ? Ba1 N5 2.858(4) . ? Ba1 N7 2.903(4) . ? Ba1 N3 3.068(5) . ? Ba1 C1 3.089(6) 2 ? Ba1 C6 3.120(6) . ? Ba1 C4 3.166(6) . ? Ba1 N2 3.158(5) 2 ? Ba1 N1 3.164(5) 2 ? Ba1 C2 3.217(5) 2 ? Ba1 C3 3.232(6) 2 ? N1 C1 1.357(7) . ? N1 C3 1.388(7) . ? N1 Ba1 3.164(5) 2_545 ? N2 C1 1.344(8) . ? N2 C2 1.378(6) . ? N2 Ba1 3.158(5) 2_545 ? N3 C4 1.337(8) . ? N3 C6 1.391(8) . ? N3 Ba1 2.813(5) 2 ? N4 C4 1.352(8) . ? N4 C5 1.369(6) . ? N5 C10 1.324(7) . ? N5 C12 1.396(6) . ? N6 C10 1.348(6) . ? N6 C11 1.372(7) . ? N7 C7 1.326(8) . ? N7 C9 1.377(8) . ? N8 C8 1.355(8) . ? N8 C7 1.360(6) . ? C1 Ba1 3.089(6) 2_545 ? C2 C3 1.371(8) . ? C2 Ba1 3.217(5) 2_545 ? C3 Ba1 3.232(6) 2_545 ? C5 C6 1.361(9) . ? C8 C9 1.363(7) . ? C11 C12 1.368(7) . ? 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 Ba1 N3 74.54(15) . 2_545 ? N1 Ba1 N5 85.12(15) . . ? N3 Ba1 N5 80.30(15) 2_545 . ? N1 Ba1 N7 81.92(15) . . ? N3 Ba1 N7 88.94(15) 2_545 . ? N5 Ba1 N7 164.99(17) . . ? N1 Ba1 N3 112.18(14) . . ? N3 Ba1 N3 173.09(12) 2_545 . ? N5 Ba1 N3 98.35(14) . . ? N7 Ba1 N3 93.54(15) . . ? N1 Ba1 C1 157.07(15) . 2 ? N3 Ba1 C1 96.29(16) 2_545 2 ? N5 Ba1 C1 114.50(14) . 2 ? N7 Ba1 C1 76.87(14) . 2 ? N3 Ba1 C1 78.04(16) . 2 ? N1 Ba1 C6 92.85(16) . . ? N3 Ba1 C6 159.68(15) 2_545 . ? N5 Ba1 C6 115.04(14) . . ? N7 Ba1 C6 73.30(15) . . ? N3 Ba1 C6 25.97(14) . . ? C1 Ba1 C6 89.34(16) 2 . ? N1 Ba1 C4 98.82(16) . . ? N3 Ba1 C4 156.29(15) 2_545 . ? N5 Ba1 C4 76.42(14) . . ? N7 Ba1 C4 113.00(14) . . ? N3 Ba1 C4 24.70(15) . . ? C1 Ba1 C4 97.40(16) 2 . ? C6 Ba1 C4 39.70(14) . . ? N1 Ba1 N2 140.10(14) . 2 ? N3 Ba1 N2 71.48(15) 2_545 2 ? N5 Ba1 N2 108.76(12) . 2 ? N7 Ba1 N2 77.21(12) . 2 ? N3 Ba1 N2 102.78(14) . 2 ? C1 Ba1 N2 24.81(15) 2 2 ? C6 Ba1 N2 112.71(15) . 2 ? C4 Ba1 N2 120.56(15) . 2 ? N1 Ba1 N1 177.60(9) . 2 ? N3 Ba1 N1 107.33(14) 2_545 2 ? N5 Ba1 N1 93.68(14) . 2 ? N7 Ba1 N1 99.54(14) . 2 ? N3 Ba1 N1 65.91(13) . 2 ? C1 Ba1 N1 25.03(14) 2 2 ? C6 Ba1 N1 85.78(15) . 2 ? C4 Ba1 N1 78.87(15) . 2 ? N2 Ba1 N1 42.29(13) 2 2 ? N1 Ba1 C2 140.43(15) . 2 ? N3 Ba1 C2 66.19(15) 2_545 2 ? N5 Ba1 C2 83.82(13) . 2 ? N7 Ba1 C2 101.47(13) . 2 ? N3 Ba1 C2 106.97(14) . 2 ? C1 Ba1 C2 39.60(14) 2 2 ? C6 Ba1 C2 126.16(16) . 2 ? C4 Ba1 C2 115.13(15) . 2 ? N2 Ba1 C2 24.94(11) 2 2 ? N1 Ba1 C2 41.27(14) 2 2 ? N1 Ba1 C3 155.32(14) . 2 ? N3 Ba1 C3 87.65(15) 2_545 2 ? N5 Ba1 C3 74.97(15) . 2 ? N7 Ba1 C3 115.29(14) . 2 ? N3 Ba1 C3 85.46(14) . 2 ? C1 Ba1 C3 39.59(14) 2 2 ? C6 Ba1 C3 108.62(15) . 2 ? C4 Ba1 C3 90.65(15) . 2 ? N2 Ba1 C3 41.03(13) 2 2 ? N1 Ba1 C3 25.04(13) 2 2 ? C2 Ba1 C3 24.55(14) 2 2 ? C1 N1 C3 102.8(5) . . ? C1 N1 Ba1 117.7(4) . . ? C3 N1 Ba1 139.6(4) . . ? C1 N1 Ba1 74.4(3) . 2_545 ? C3 N1 Ba1 80.2(3) . 2_545 ? Ba1 N1 Ba1 108.77(16) . 2_545 ? C1 N2 C2 103.6(4) . . ? C1 N2 Ba1 74.7(3) . 2_545 ? C2 N2 Ba1 79.9(3) . 2_545 ? C4 N3 C6 103.0(5) . . ? C4 N3 Ba1 119.2(4) . 2 ? C6 N3 Ba1 137.4(4) . 2 ? C4 N3 Ba1 81.8(3) . . ? C6 N3 Ba1 79.1(3) . . ? Ba1 N3 Ba1 110.78(17) 2 . ? C4 N4 C5 103.2(5) . . ? C4 N4 Ba1 71.1(3) . . ? C5 N4 Ba1 75.4(3) . . ? C10 N5 C12 104.6(4) . . ? C10 N5 Ba1 130.2(3) . . ? C12 N5 Ba1 122.1(3) . . ? C10 N6 C11 106.8(4) . . ? C7 N7 C9 105.0(4) . . ? C7 N7 Ba1 127.8(4) . . ? C9 N7 Ba1 124.9(4) . . ? C8 N8 C7 107.1(4) . . ? N2 C1 N1 115.2(5) . . ? N2 C1 Ba1 80.5(4) . 2_545 ? N1 C1 Ba1 80.6(3) . 2_545 ? C3 C2 N2 109.2(5) . . ? C3 C2 Ba1 78.3(3) . 2_545 ? N2 C2 Ba1 75.2(3) . 2_545 ? C2 C3 N1 109.2(5) . . ? C2 C3 Ba1 77.1(3) . 2_545 ? N1 C3 Ba1 74.8(3) . 2_545 ? N3 C4 N4 115.3(5) . . ? N3 C4 Ba1 73.6(3) . . ? N4 C4 Ba1 85.1(3) . . ? C6 C5 N4 109.6(5) . . ? C6 C5 Ba1 71.6(3) . . ? N4 C5 Ba1 80.7(3) . . ? C5 C6 N3 108.9(5) . . ? C5 C6 Ba1 83.9(3) . . ? N3 C6 Ba1 74.9(3) . . ? N7 C7 N8 111.4(5) . . ? N8 C8 C9 106.6(5) . . ? C8 C9 N7 109.9(5) . . ? N5 C10 N6 112.6(5) . . ? C12 C11 N6 106.5(4) . . ? C11 C12 N5 109.4(4) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 30.34 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.578 _refine_diff_density_min -1.220 _refine_diff_density_rms 0.232