Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'E. Colacio' _publ_contact_author_address ; Departamento de Quimica Universidad de Granada Facultad de Ciencias Granada 18071 SPAIN ; _publ_contact_author_email ECOLACIO@UGR.ES _publ_section_title ; Synthesis, X-ray structures and Luminescence Properties of Three Multidimensional Metal-Organic Frameworks incorporating the versatile 5-(pyrimidyl)tetrazolato bridging ligand ; loop_ _publ_author_name 'E. Colacio' 'Simona Galli' 'Juan M. Gutierrez-Zorrilla' 'Norberto Masciocchi' ; A.Rodriguez-Dieguez ; 'A. Salinas-Castillo' 'Pablo Vitoria' #============================================================================== data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 632259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(mu4-5-(pyrimidil)tetrazolate)-aquo-sodium(i) ; _chemical_name_common catena-(mu4-5-(pyrimidil)tetrazolate)-aquo-sodium(i) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H5 N6 Na O' _chemical_formula_weight 188.14 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 6.2520(8) _cell_length_b 9.6115(12) _cell_length_c 12.8642(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.816(2) _cell_angle_gamma 90.00 _cell_volume 750.66(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2581 _cell_measurement_theta_min 2.674 _cell_measurement_theta_max 28.148 _exptl_crystal_description prismatic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.998 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4495 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.15 _reflns_number_total 1686 _reflns_number_gt 1563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0327P)^2^+1.6107P] 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 1686 _refine_ls_number_parameters 126 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Na Na 0.43012(16) 0.45693(11) 0.13805(8) 0.0175(3) Uani 1 1 d . . . N1 N 0.7396(3) 0.5955(2) 0.11199(17) 0.0152(4) Uani 1 1 d . . . N2 N 0.8150(4) 0.7269(2) 0.12325(17) 0.0153(5) Uani 1 1 d . . . N3 N 1.0308(3) 0.7264(2) 0.13583(17) 0.0148(4) Uani 1 1 d . . . N4 N 1.1018(3) 0.5943(2) 0.13294(16) 0.0139(4) Uani 1 1 d . . . C5 C 0.9191(4) 0.5174(3) 0.11857(18) 0.0127(5) Uani 1 1 d . . . C6 C 0.9159(4) 0.3645(3) 0.11222(19) 0.0139(5) Uani 1 1 d . . . N7 N 0.7182(3) 0.3030(2) 0.09878(17) 0.0160(5) Uani 1 1 d . . . C8 C 0.7193(4) 0.1645(3) 0.0940(2) 0.0182(5) Uani 1 1 d . . . H8 H 0.5826 0.1166 0.0821 0.022 Uiso 1 1 calc R . . C9 C 0.9103(4) 0.0872(3) 0.1056(2) 0.0175(5) Uani 1 1 d . . . H9 H 0.9082 -0.0116 0.1041 0.021 Uiso 1 1 calc R . . C10 C 1.1046(4) 0.1619(3) 0.1194(2) 0.0174(5) Uani 1 1 d . . . H10 H 1.2393 0.1125 0.1279 0.021 Uiso 1 1 calc R . . N11 N 1.1093(3) 0.3006(2) 0.12129(17) 0.0147(4) Uani 1 1 d . . . O1W O 0.5491(4) 0.3911(2) 0.32034(16) 0.0200(4) Uani 1 1 d . . . H1W H 0.657(8) 0.346(5) 0.336(3) 0.048(13) Uiso 1 1 d . . . H2W H 0.462(7) 0.349(5) 0.337(3) 0.047(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 Na 0.0098(5) 0.0188(5) 0.0253(6) 0.0012(4) 0.0068(4) 0.0008(4) N1 0.0134(10) 0.0138(10) 0.0192(11) 0.0013(8) 0.0055(8) 0.0011(8) N2 0.0142(10) 0.0135(10) 0.0194(11) 0.0000(8) 0.0063(8) 0.0005(8) N3 0.0137(10) 0.0154(11) 0.0156(10) -0.0004(8) 0.0041(8) 0.0011(8) N4 0.0121(10) 0.0149(10) 0.0153(10) -0.0003(8) 0.0041(8) -0.0001(8) C5 0.0109(11) 0.0170(12) 0.0104(11) 0.0007(9) 0.0028(8) 0.0006(9) C6 0.0109(11) 0.0195(12) 0.0121(11) -0.0002(9) 0.0041(9) 0.0011(9) N7 0.0119(10) 0.0174(11) 0.0198(11) -0.0006(8) 0.0060(8) -0.0006(8) C8 0.0159(12) 0.0211(13) 0.0192(13) -0.0004(10) 0.0074(10) -0.0040(10) C9 0.0217(13) 0.0136(12) 0.0196(12) -0.0005(10) 0.0096(10) -0.0012(10) C10 0.0166(12) 0.0202(13) 0.0169(12) 0.0000(10) 0.0069(9) 0.0044(10) N11 0.0123(10) 0.0174(11) 0.0156(10) -0.0003(8) 0.0057(8) 0.0015(8) O1W 0.0125(9) 0.0193(10) 0.0290(11) 0.0021(8) 0.0064(8) -0.0002(8) _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 Na O1W 2.371(2) . ? Na N4 2.428(2) 1_455 ? Na N1 2.437(2) . ? Na N11 2.474(2) 1_455 ? Na N7 2.475(2) . ? Na Na 3.943(2) 3_665 ? N1 C5 1.335(3) . ? N1 N2 1.344(3) . ? N2 N3 1.320(3) . ? N3 N4 1.348(3) . ? N4 C5 1.335(3) . ? N4 Na 2.428(2) 1_655 ? C5 C6 1.472(4) . ? C6 N11 1.336(3) . ? C6 N7 1.343(3) . ? N7 C8 1.333(3) . ? C8 C9 1.384(4) . ? C8 H8 0.9500 . ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 N11 1.334(3) . ? C10 H10 0.9500 . ? N11 Na 2.474(2) 1_655 ? O1W H1W 0.78(5) . ? O1W H2W 0.75(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Na N4 103.61(8) . 1_455 ? O1W Na N1 102.12(8) . . ? N4 Na N1 113.15(8) 1_455 . ? O1W Na N11 88.88(8) . 1_455 ? N4 Na N11 70.45(7) 1_455 1_455 ? N1 Na N11 166.82(8) . 1_455 ? O1W Na N7 88.32(8) . . ? N4 Na N7 166.26(8) 1_455 . ? N1 Na N7 70.00(8) . . ? N11 Na N7 103.50(8) 1_455 . ? O1W Na Na 149.60(7) . 3_665 ? N4 Na Na 103.25(6) 1_455 3_665 ? N1 Na Na 53.65(6) . 3_665 ? N11 Na Na 113.48(7) 1_455 3_665 ? N7 Na Na 67.23(6) . 3_665 ? C5 N1 N2 104.7(2) . . ? C5 N1 Na 111.54(16) . . ? N2 N1 Na 140.18(16) . . ? N3 N2 N1 109.3(2) . . ? N2 N3 N4 109.5(2) . . ? C5 N4 N3 104.4(2) . . ? C5 N4 Na 113.10(16) . 1_655 ? N3 N4 Na 142.43(16) . 1_655 ? N4 C5 N1 112.1(2) . . ? N4 C5 C6 124.1(2) . . ? N1 C5 C6 123.9(2) . . ? N11 C6 N7 126.5(2) . . ? N11 C6 C5 117.0(2) . . ? N7 C6 C5 116.5(2) . . ? C8 N7 C6 115.5(2) . . ? C8 N7 Na 128.21(17) . . ? C6 N7 Na 113.74(16) . . ? N7 C8 C9 123.0(2) . . ? N7 C8 H8 118.5 . . ? C9 C8 H8 118.5 . . ? C8 C9 C10 116.3(2) . . ? C8 C9 H9 121.8 . . ? C10 C9 H9 121.8 . . ? N11 C10 C9 122.4(2) . . ? N11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 N11 C6 116.2(2) . . ? C10 N11 Na 128.53(17) . 1_655 ? C6 N11 Na 115.23(17) . 1_655 ? Na O1W H1W 117(3) . . ? Na O1W H2W 111(3) . . ? H1W O1W H2W 105(4) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.560 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.075 #============================================================================== data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 632260' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-bis(mu4-5-(pyrimidil)tetrazolate)-cadmium(ii) ; _chemical_name_common catena-bis(mu4-5-(pyrimidil)tetrazolate)-cadmium(ii) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 Cd N12' _chemical_formula_weight 406.67 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/nnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z' '-y+1/2, -x+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z' 'y-1/2, x-1/2, z' _cell_length_a 9.0559(3) _cell_length_b 9.0559(3) _cell_length_c 15.7800(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1294.11(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3132 _cell_measurement_theta_min 3.181 _cell_measurement_theta_max 28.232 _exptl_crystal_description prismatic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.878 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Axs APEX automated diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.26_diffrn_measurement_device_type _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7627 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0118 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 28.34 _reflns_number_total 848 _reflns_number_gt 764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0276P)^2^+1.1163P] 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 848 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0585 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.003 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 Cd1 Cd 0.2500 0.2500 0.2500 0.00825(12) Uani 1 4 d S . . N1 N 0.64460(15) -0.04210(15) 0.33904(8) 0.0108(3) Uani 1 1 d . . . C1 C 0.52937(18) 0.02937(18) 0.30528(14) 0.0094(4) Uani 1 2 d S . . C2 C 0.61788(18) 0.11788(18) 0.45800(14) 0.0132(5) Uani 1 2 d S . . H2 H 0.6476 0.1476 0.5132 0.016 Uiso 1 2 calc SR . . C3 C 0.68763(17) 0.00326(18) 0.41631(10) 0.0127(3) Uani 1 1 d . . . H3 H 0.7684 -0.0449 0.4430 0.015 Uiso 1 1 calc R . . N5 N 0.35812(15) -0.03877(16) 0.10718(8) 0.0144(3) Uani 1 1 d . . . N6 N 0.36673(15) 0.03910(15) 0.17988(8) 0.0112(3) Uani 1 1 d . . . C5 C 0.47847(18) -0.02153(18) 0.22167(15) 0.0099(4) Uani 1 2 d S . . 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 Cd1 0.00703(15) 0.00774(15) 0.00999(17) 0.000 0.000 0.000 N1 0.0103(6) 0.0107(6) 0.0113(6) -0.0004(5) -0.0008(5) -0.0002(5) C1 0.0096(6) 0.0096(6) 0.0089(10) 0.0001(6) 0.0001(6) -0.0015(9) C2 0.0155(7) 0.0155(7) 0.0087(9) -0.0009(6) -0.0009(6) -0.0021(9) C3 0.0119(8) 0.0147(8) 0.0115(7) 0.0022(6) -0.0021(6) -0.0011(6) N5 0.0156(7) 0.0156(7) 0.0121(6) -0.0025(5) -0.0023(5) -0.0020(5) N6 0.0116(6) 0.0119(6) 0.0100(6) -0.0008(5) -0.0018(5) -0.0007(5) C5 0.0103(6) 0.0103(6) 0.0090(10) -0.0010(6) -0.0010(6) -0.0025(8) _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 Cd1 N6 2.4473(14) 6 ? Cd1 N6 2.4473(14) . ? Cd1 N6 2.4473(14) 5 ? Cd1 N6 2.4473(14) 2 ? Cd1 N1 2.5357(13) 12_556 ? Cd1 N1 2.5357(13) 16_655 ? Cd1 N1 2.5357(13) 15_565 ? Cd1 N1 2.5357(13) 11_666 ? N1 C1 1.3385(16) . ? N1 C3 1.3443(19) . ? N1 Cd1 2.5357(13) 11_656 ? C1 N1 1.3385(16) 16_655 ? C1 C5 1.472(3) . ? C2 C3 1.3818(19) . ? C2 C3 1.3818(19) 16_655 ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? N5 N5 1.321(3) 16_655 ? N5 N6 1.3489(17) . ? N6 C5 1.3267(18) . ? C5 N6 1.3267(18) 16_655 ? 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 N6 Cd1 N6 128.82(6) 6 . ? N6 Cd1 N6 126.24(6) 6 5 ? N6 Cd1 N6 77.41(6) . 5 ? N6 Cd1 N6 77.41(6) 6 2 ? N6 Cd1 N6 126.24(6) . 2 ? N6 Cd1 N6 128.82(6) 5 2 ? N6 Cd1 N1 149.88(5) 6 12_556 ? N6 Cd1 N1 77.08(4) . 12_556 ? N6 Cd1 N1 68.66(4) 5 12_556 ? N6 Cd1 N1 73.89(4) 2 12_556 ? N6 Cd1 N1 73.89(4) 6 16_655 ? N6 Cd1 N1 68.66(4) . 16_655 ? N6 Cd1 N1 77.08(4) 5 16_655 ? N6 Cd1 N1 149.88(5) 2 16_655 ? N1 Cd1 N1 135.78(6) 12_556 16_655 ? N6 Cd1 N1 77.08(4) 6 15_565 ? N6 Cd1 N1 149.88(5) . 15_565 ? N6 Cd1 N1 73.89(4) 5 15_565 ? N6 Cd1 N1 68.66(4) 2 15_565 ? N1 Cd1 N1 84.11(6) 12_556 15_565 ? N1 Cd1 N1 112.70(6) 16_655 15_565 ? N6 Cd1 N1 68.66(4) 6 11_666 ? N6 Cd1 N1 73.89(4) . 11_666 ? N6 Cd1 N1 149.88(5) 5 11_666 ? N6 Cd1 N1 77.08(4) 2 11_666 ? N1 Cd1 N1 112.70(6) 12_556 11_666 ? N1 Cd1 N1 84.11(6) 16_655 11_666 ? N1 Cd1 N1 135.78(6) 15_565 11_666 ? C1 N1 C3 116.05(15) . . ? C1 N1 Cd1 115.59(11) . 11_656 ? C3 N1 Cd1 128.34(11) . 11_656 ? N1 C1 N1 126.6(2) 16_655 . ? N1 C1 C5 116.71(10) 16_655 . ? N1 C1 C5 116.71(10) . . ? C3 C2 C3 117.4(2) . 16_655 ? C3 C2 H2 121.3 . . ? C3 C2 H2 121.3 16_655 . ? N1 C3 C2 121.93(15) . . ? N1 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? N5 N5 N6 109.19(8) 16_655 . ? C5 N6 N5 104.51(14) . . ? C5 N6 Cd1 115.32(11) . . ? N5 N6 Cd1 140.13(10) . . ? N6 C5 N6 112.6(2) . 16_655 ? N6 C5 C1 123.70(10) . . ? N6 C5 C1 123.70(10) 16_655 . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.558 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.093 #============================================================================== #data_Compound_3 data_3 _database_code_depnum_ccdc_archive 'CCDC 632261' _chemical_name_systematic ; catena-(mu-chloro)-(mu-N,N'-azide)-bis(mu4-5-(pyrimidil)tetrazolate-aquo)- -cadmium(ii) ; _chemical_name_common ; catena-(mu-chloro)-(mu-N,N'-azide)-bis(mu4-5- (pyrimidil)tetrazolate-aquo)--cadmium(ii) ; _chemical_formula_moiety C5H5CdCl0.5N7.5O _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum C5H5CdCl0.5N7.5O _chemical_formula_weight 316.28 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description # _atom_type_scat_dispersion_real # _atom_type_scat_dispersion_imag _atom_type_scat_source C C 'International Tables for Crystallography (Vol. IV)' H H 'International Tables for Crystallography (Vol. IV)' Cl Cl 'International Tables for Crystallography (Vol. IV)' Cd Cd 'International Tables for Crystallography (Vol. IV)' N N 'International Tables for Crystallography (Vol. IV)' O O 'International Tables for Crystallography (Vol. IV)' #============================================================================== # 1.5. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall ? 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+1/2' 'x, y, z' 'x+1/2, -y+1/2, z+1/2' 'x+1/2, y+1/2, z' _cell_length_a 16.10858(80) _cell_length_b 6.60053(31) _cell_length_c 17.24252(89) _cell_angle_alpha 90 _cell_angle_beta 95.1767(44) _cell_angle_gamma 90 _cell_volume 1825.84(16) _cell_formula_units_Z 8 _cell_measurement_temperature 298 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.287 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 12 # perpendicular to # equatorial plane _pd_spec_size_equat 20 # parallel to # scattering vector # in transmission _pd_spec_size_thick 0.2 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology plate-like _pd_char_colour colorless # use ICDD colour descriptions # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # 1.6. EXPERIMENTAL DATA _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _diffrn_ambient_temperature 298 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type 'Bruker AXS D8 Advance' _diffrn_detector scintillator _diffrn_detector_type ? _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. loop_ _diffrn_radiation_type _diffrn_radiation_wavelength CuK\a~1~ 1.54056 CuK\a~2~ 1.54439 _diffrn_radiation_monochromator 'HOPG Graphite' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5001 _pd_meas_2theta_range_min 5 _pd_meas_2theta_range_max 105 _pd_meas_2theta_range_inc 0.02 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'D8 software (Bruker AXS, 2001)' _computing_cell_refinement TOPAS-R _computing_data_reduction TOPAS-R _computing_structure_solution TOPAS-R _computing_structure_refinement TOPAS-R _computing_molecular_graphics ? _computing_publication_material TOPAS-R #============================================================================== # 1.7. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The use of a rigid body description for the 5(pyrimidil)tetrazolate ligand does not allow the derivation of statistically meaningful s.u.'s for its atoms. Only center of mass and rotational angles s.u.'s are available: XYZ 0.7334(6), 0.081(1), -0.9783(6) RX, RY, RZ 77.3(4), 203.8(2), 177.6(7) for the rigid body described by: N1 ux -0.29212 uy 1.93855 uz -0.40308 N2 ux 0.14439 uy 3.20202 uz -0.26242 N3 ux 1.45524 uy 3.19687 uz -0.10526 N4 ux 1.90743 uy 1.92734 uz -0.14146 C5 ux 0.80970 uy 1.18852 uz -0.32089 C6 ux 0.80917 uy -0.28146 uz -0.40021 N7 ux -0.38532 uy -0.87272 uz -0.56814 C8 ux -0.36417 uy -2.20378 uz -0.62805 H8 ux -1.18191 uy -2.66382 uz -0.77698 C9 ux 0.79424 uy -2.94657 uz -0.48327 H9 ux 0.78616 uy -3.89636 uz -0.50156 C10 ux 1.96648 uy -2.22886 uz -0.31018 H10 ux 2.78256 uy -2.70348 uz -0.20419 N11 ux 1.99055 uy -0.89569 uz -0.28700 ; # The next three items are given as text _pd_proc_ls_profile_function 'fundamental parameters' _pd_proc_ls_background_function polynomial _pd_proc_ls_pref_orient_corr ? _pd_proc_ls_prof_R_factor 0.125 _pd_proc_ls_prof_wR_factor 0.159 _pd_proc_ls_prof_wR_expected 0.093 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 1/[Y~i~] _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 30 _refine_ls_number_restraints 2 _refine_ls_number_constraints ? # The following item is 'CHI squared' _refine_ls_goodness_of_fit_all 1.706 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 9 _pd_proc_2theta_range_max 105 _pd_proc_2theta_range_inc 0.02 loop_ _pd_proc_wavelength 1.540562 1.544390 _pd_block_diffractogram_id ? # The id used for the block # containing the powder # pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== # 1.8. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv Cd Cd 8 1.03826(20) -0.08601(51) -1.11902(20) 1 2.763(94) N1 N 8 0.7698294 -0.04653142 -1.074914 1 4.763(94) N2 N 8 0.8313985 -0.07409579 -1.121531 1 4.763(94) N3 N 8 0.9040873 -0.05813371 -1.080027 1 4.763(94) N4 N 8 0.8917047 -0.01996151 -1.005131 1 4.763(94) C5 C 8 0.8089246 -0.01341924 -1.004429 1 4.763(94) C6 C 8 0.765698 0.02821116 -0.934468 1 4.763(94) N7 N 8 0.6820169 0.03163561 -0.9439941 1 4.763(94) C8 C 8 0.6441631 0.07096214 -0.88006 1 4.763(94) H8 H 8 0.5849665 0.07031705 -0.8836295 1 4.763(94) C9 C 8 0.687125 0.1126961 -0.8087124 1 4.763(94) H9 H 8 0.659077 0.1444828 -0.7641031 1 4.763(94) C10 C 8 0.773295 0.1055706 -0.8059167 1 4.763(94) H10 H 8 0.8050036 0.1337947 -0.7579843 1 4.763(94) N11 N 8 0.8133348 0.0605157 -0.8680901 1 4.763(94) Cl1 Cl 4 1.0 -0.2734(19) -1.25 1 4.763(94) N1az N 4 1.0 0.2588(63) -1.25 1 4.763(94) N2az N 8 1.0295(19) 0.2370(48) -1.1774(10) 1 4.763(94) O1w O 8 1.0662(12) -0.4416(36) -1.0726(11) 1 4.763(94) #==============================================================================