Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Goher, Mohamed A. S.' ; Department of Chemistry, Faculty of Science, Alexandria University, P.O.Box 21321 Ibrahimia Alexandria, Egypt ; 'Mautner, Franz A.' ; Institut fur Physikalische und Theoretische Chemie, Technische Universitat Graz Rechbauerstr. 12 A-8010 Graz Austria ; 'Abu-Youssef, Morsy A.M.' ; Department of Chemistry, Faculty of Science, Alexandria University, P.O.Box 21321 Ibrahimia Alexandria, Egypt ; 'Hafez, Ahmed K.' ; Department of Chemistry, Faculty of Science, Alexandria University, P.O.Box 21321 Ibrahimia Alexandria, Egypt ; 'Badr, Afaf M.A.' ; Department of Chemistry, Faculty of Science, Alexandria University, P.O.Box 21321 Ibrahimia Alexandria, Egypt ; _publ_contact_author_name 'Dr Franz A Mautner' _publ_contact_author_address ; Institut fur Physikalische und Theoretische Chemie Technische Universitat Graz Graz 8010 AUSTRIA ; _publ_contact_author_phone '++43 316 873 8234' _publ_contact_author_fax '++43 316 873 8225' _publ_contact_author_email 'mautner@ptc.tu-graz.ac.at' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #==================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and crystal structure of three new 2D polymeric cadmium(II) complexes of some pyridine derivatives with different cadmium(II) azide topologies ; #=================================================================== data_cdacpy _database_code_CSD 180362 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Cd(N3)2(2-acetylpyridine)]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C7 H7 Cd N7 O' _chemical_formula_weight 317.60 _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' 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' 'O' 'O' 0.0106 0.0060 '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/a 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 9.107(4) _cell_length_b 13.696(5) _cell_length_c 9.310(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.11(3) _cell_angle_gamma 90.00 _cell_volume 1059.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 13.5 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method ? _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 2.051 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle diffractometer' _diffrn_measurement_method 'Omega-Scan; delta Omega: 1.10 deg.' _diffrn_standards_number '3 (0 -4 0; -1 -3 1; -2 0 -2)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 5 _diffrn_reflns_number 2395 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.96 _reflns_number_total 1871 _reflns_number_observed 1612 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 21 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+3.0384P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1850 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_obs 0.0435 _refine_ls_wR_factor_all 0.1127 _refine_ls_wR_factor_obs 0.1013 _refine_ls_goodness_of_fit_all 1.087 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.121 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.11616(5) 0.39708(3) 0.10019(5) 0.0156(2) Uani 1 d . . N11 N -0.0295(7) 0.4510(4) -0.1474(6) 0.0219(12) Uani 1 d . . N12 N -0.0017(6) 0.4270(4) -0.2592(7) 0.0191(12) Uani 1 d . . N13 N 0.0210(7) 0.4033(4) -0.3669(7) 0.0285(14) Uani 1 d . . N21 N -0.0535(6) 0.3046(4) 0.1675(7) 0.0253(13) Uani 1 d . . N22 N -0.1786(6) 0.2737(4) 0.0799(6) 0.0199(12) Uani 1 d . . N23 N -0.3052(7) 0.2422(4) -0.0034(7) 0.0254(13) Uani 1 d . . N1 N 0.3153(6) 0.3758(4) 0.3518(6) 0.0184(11) Uani 1 d . . C1 C 0.4704(7) 0.3892(4) 0.3748(8) 0.0186(13) Uani 1 d . . C2 C 0.5952(8) 0.3760(4) 0.5187(8) 0.0201(13) Uani 1 d . . H2 H 0.7006(8) 0.3857(4) 0.5307(8) 0.024 Uiso 1 calc R . C3 C 0.5632(8) 0.3478(5) 0.6472(8) 0.0254(15) Uani 1 d . . H3 H 0.6463(8) 0.3378(5) 0.7457(8) 0.030 Uiso 1 calc R . C4 C 0.4033(8) 0.3350(5) 0.6240(8) 0.0268(15) Uani 1 d . . H4 H 0.3772(8) 0.3172(5) 0.7071(8) 0.032 Uiso 1 calc R . C5 C 0.2843(8) 0.3491(5) 0.4748(8) 0.0234(14) Uani 1 d . . H5 H 0.1777(8) 0.3396(5) 0.4593(8) 0.028 Uiso 1 calc R . C6 C 0.4949(8) 0.4232(4) 0.2313(7) 0.0174(13) Uani 1 d . . O1 O 0.3766(5) 0.4466(3) 0.1118(5) 0.0206(10) Uani 1 d . . C7 C 0.6611(8) 0.4282(5) 0.2382(8) 0.0249(15) Uani 1 d . . H7A H 0.7131(21) 0.3662(11) 0.2708(52) 0.030 Uiso 1 calc R . H7B H 0.7211(18) 0.4775(23) 0.3123(40) 0.030 Uiso 1 calc R . H7C H 0.6563(8) 0.4443(33) 0.1360(15) 0.030 Uiso 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 Cd1 0.0153(2) 0.0161(3) 0.0152(3) 0.0009(2) 0.0060(2) 0.0015(2) N11 0.028(3) 0.024(3) 0.016(3) 0.000(2) 0.012(2) 0.008(2) N12 0.019(3) 0.011(2) 0.022(3) 0.003(2) 0.003(2) -0.003(2) N13 0.035(3) 0.035(3) 0.023(3) -0.003(3) 0.019(3) -0.002(3) N21 0.020(3) 0.032(3) 0.024(3) 0.003(3) 0.008(2) -0.005(2) N22 0.029(3) 0.016(2) 0.017(3) 0.005(2) 0.011(3) 0.002(2) N23 0.027(3) 0.026(3) 0.019(3) 0.005(2) 0.005(2) -0.006(2) N1 0.025(3) 0.013(2) 0.019(3) -0.001(2) 0.012(2) 0.001(2) C1 0.021(3) 0.011(3) 0.023(3) -0.004(3) 0.010(3) 0.003(2) C2 0.018(3) 0.018(3) 0.023(4) -0.007(3) 0.007(3) 0.000(2) C3 0.031(4) 0.019(3) 0.017(3) 0.003(3) 0.001(3) 0.003(3) C4 0.037(4) 0.021(3) 0.022(4) 0.000(3) 0.012(3) -0.002(3) C5 0.025(3) 0.025(3) 0.022(4) -0.002(3) 0.012(3) -0.002(3) C6 0.026(3) 0.012(3) 0.015(3) -0.003(2) 0.009(3) 0.001(2) O1 0.020(2) 0.025(2) 0.019(2) 0.002(2) 0.011(2) 0.001(2) C7 0.026(3) 0.026(3) 0.026(4) -0.004(3) 0.014(3) -0.004(3) _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 Cd1 3.561(1) 3_565 yes Cd1 Cd1 6.080(2) 4_665 yes Cd1 Cd1 6.080(2) 4_565 ? Cd1 N11 2.262(6) . yes Cd1 N21 2.275(6) . yes Cd1 N1 2.322(6) . yes Cd1 N11 2.330(5) 3_565 yes Cd1 N23 2.377(6) 4_665 yes Cd1 O1 2.426(4) . yes N11 N12 1.213(8) . yes N11 Cd1 2.330(5) 3_565 ? N12 N13 1.150(8) . yes N21 N22 1.176(8) . yes N22 N23 1.177(7) . yes N23 Cd1 2.377(6) 4_565 ? N1 O1 2.695(7) . yes N1 C5 1.337(9) . ? N1 C1 1.352(8) . ? C1 C2 1.369(9) . ? C1 C6 1.515(9) . ? C2 C3 1.397(10) . ? C2 H2 0.93 . ? C3 C4 1.392(10) . ? C3 H3 0.93 . ? C4 C5 1.383(9) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? C6 O1 1.234(8) . ? C6 C7 1.490(9) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? 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 N11 Cd1 N21 106.3(2) . . yes N11 Cd1 N1 163.8(2) . . yes N21 Cd1 N1 89.5(2) . . yes N11 Cd1 N11 78.3(2) . 3_565 yes N21 Cd1 N11 97.2(2) . 3_565 yes N1 Cd1 N11 96.2(2) . 3_565 yes N11 Cd1 N23 89.8(2) . 4_665 yes N21 Cd1 N23 90.9(2) . 4_665 yes N1 Cd1 N23 93.9(2) . 4_665 yes N11 Cd1 N23 167.1(2) 3_565 4_665 yes N11 Cd1 O1 96.3(2) . . yes N21 Cd1 O1 154.8(2) . . yes N1 Cd1 O1 69.1(2) . . yes N11 Cd1 O1 98.2(2) 3_565 . yes N23 Cd1 O1 78.0(2) 4_665 . yes N12 N11 Cd1 123.0(4) . . yes N12 N11 Cd1 127.5(4) . 3_565 yes Cd1 N11 Cd1 101.7(2) . 3_565 yes N13 N12 N11 178.3(7) . . yes N22 N21 Cd1 125.8(5) . . yes N23 N22 N21 177.8(7) . . yes N22 N23 Cd1 113.7(4) . 4_565 yes C5 N1 C1 118.3(6) . . ? C5 N1 Cd1 123.2(4) . . ? C1 N1 Cd1 118.5(4) . . ? N1 C1 C2 122.2(6) . . ? N1 C1 C6 115.0(6) . . ? C2 C1 C6 122.7(6) . . ? C1 C2 C3 119.6(6) . . ? C1 C2 H2 120.2(4) . . ? C3 C2 H2 120.2(4) . . ? C4 C3 C2 118.2(6) . . ? C4 C3 H3 120.9(4) . . ? C2 C3 H3 120.9(4) . . ? C5 C4 C3 118.7(7) . . ? C5 C4 H4 120.7(4) . . ? C3 C4 H4 120.7(4) . . ? N1 C5 C4 123.1(7) . . ? N1 C5 H5 118.5(4) . . ? C4 C5 H5 118.5(4) . . ? O1 C6 C7 121.6(6) . . ? O1 C6 C1 119.1(6) . . ? C7 C6 C1 119.3(5) . . ? C6 O1 Cd1 116.4(4) . . ? C6 C7 H7A 109.5(4) . . ? C6 C7 H7B 109.5(4) . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5(4) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 N21 Cd1 N11 N12 -114.7(5) . . . . ? N1 Cd1 N11 N12 79.7(8) . . . . ? N11 Cd1 N11 N12 151.2(6) 3_565 . . . ? N23 Cd1 N11 N12 -23.8(5) 4_665 . . . ? O1 Cd1 N11 N12 54.1(5) . . . . ? N21 Cd1 N11 Cd1 94.2(2) . . . 3_565 ? N1 Cd1 N11 Cd1 -71.5(7) . . . 3_565 ? N11 Cd1 N11 Cd1 0.0 3_565 . . 3_565 ? N23 Cd1 N11 Cd1 -174.9(2) 4_665 . . 3_565 ? O1 Cd1 N11 Cd1 -97.1(2) . . . 3_565 ? Cd1 N11 N12 N13 118.4(208) . . . . ? Cd1 N11 N12 N13 -98.1(209) 3_565 . . . ? N11 Cd1 N21 N22 15.2(6) . . . . ? N1 Cd1 N21 N22 -168.7(6) . . . . ? N11 Cd1 N21 N22 95.1(6) 3_565 . . . ? N23 Cd1 N21 N22 -74.8(6) 4_665 . . . ? O1 Cd1 N21 N22 -137.7(5) . . . . ? Cd1 N21 N22 N23 -162.9(160) . . . . ? N21 N22 N23 Cd1 -41.0(165) . . . 4_565 ? N11 Cd1 N1 C5 146.4(6) . . . . ? N21 Cd1 N1 C5 -19.8(5) . . . . ? N11 Cd1 N1 C5 77.3(5) 3_565 . . . ? N23 Cd1 N1 C5 -110.7(5) 4_665 . . . ? O1 Cd1 N1 C5 173.8(5) . . . . ? N11 Cd1 N1 C1 -34.8(9) . . . . ? N21 Cd1 N1 C1 158.9(4) . . . . ? N11 Cd1 N1 C1 -103.9(4) 3_565 . . . ? N23 Cd1 N1 C1 68.0(4) 4_665 . . . ? O1 Cd1 N1 C1 -7.5(4) . . . . ? C5 N1 C1 C2 0.3(9) . . . . ? Cd1 N1 C1 C2 -178.5(5) . . . . ? C5 N1 C1 C6 -177.7(5) . . . . ? Cd1 N1 C1 C6 3.5(6) . . . . ? N1 C1 C2 C3 -0.1(9) . . . . ? C6 C1 C2 C3 177.7(6) . . . . ? C1 C2 C3 C4 -0.6(9) . . . . ? C2 C3 C4 C5 1.0(10) . . . . ? C1 N1 C5 C4 0.2(9) . . . . ? Cd1 N1 C5 C4 178.9(5) . . . . ? C3 C4 C5 N1 -0.9(10) . . . . ? N1 C1 C6 O1 8.1(8) . . . . ? C2 C1 C6 O1 -169.9(6) . . . . ? N1 C1 C6 C7 -172.4(5) . . . . ? C2 C1 C6 C7 9.6(9) . . . . ? C7 C6 O1 Cd1 165.6(4) . . . . ? C1 C6 O1 Cd1 -14.8(7) . . . . ? N11 Cd1 O1 C6 -175.4(4) . . . . ? N21 Cd1 O1 C6 -21.4(7) . . . . ? N1 Cd1 O1 C6 12.0(4) . . . . ? N11 Cd1 O1 C6 105.5(4) 3_565 . . . ? N23 Cd1 O1 C6 -86.9(4) 4_665 . . . ? _refine_diff_density_max 0.975 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.163 #========================================================== data_cda05a _database_code_CSD 180363 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Cd(N3)2(4-acetylpyridine)2]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H14 Cd N8 O2' _chemical_formula_weight 438.73 _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' 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' 'O' 'O' 0.0106 0.0060 '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/a 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 8.690(3) _cell_length_b 8.522(3) _cell_length_c 11.216(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.81(3) _cell_angle_gamma 90.00 _cell_volume 827.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 9.4 _cell_measurement_theta_max 14.8 _exptl_crystal_description irregular _exptl_crystal_colour 'transparent yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method ? _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.289 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle diffractometer' _diffrn_measurement_method 'Omega-scan; delta Omega: 1.10 deg.' _diffrn_standards_number '3 (2 0 1; 1 -1 2; 1 -1 -1)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 4 _diffrn_reflns_number 1924 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1464 _reflns_number_observed 1198 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+1.3667P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1450 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_obs 0.0431 _refine_ls_wR_factor_all 0.1185 _refine_ls_wR_factor_obs 0.1069 _refine_ls_goodness_of_fit_all 1.084 _refine_ls_goodness_of_fit_obs 1.126 _refine_ls_restrained_S_all 1.120 _refine_ls_restrained_S_obs 1.126 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.5000 0.0134(2) Uani 1 d S . N11 N 0.1515(5) 0.1591(5) 0.6311(4) 0.0197(10) Uani 1 d . . N12 N 0.2169(5) 0.2690(5) 0.5952(4) 0.0162(10) Uani 1 d . . N13 N 0.2798(6) 0.3830(6) 0.5638(4) 0.0259(11) Uani 1 d . . N1 N 0.0222(5) 0.1905(5) 0.3509(4) 0.0146(9) Uani 1 d . . C1 C -0.0189(6) 0.3396(6) 0.3689(5) 0.0163(11) Uani 1 d . . H1 H -0.0712(6) 0.3633(6) 0.4356(5) 0.020 Uiso 1 calc R . C2 C 0.0139(6) 0.4605(6) 0.2913(5) 0.0168(11) Uani 1 d . . H2 H -0.0175(6) 0.5626(6) 0.3056(5) 0.020 Uiso 1 calc R . C3 C 0.0940(6) 0.4268(6) 0.1926(5) 0.0158(11) Uani 1 d . . C4 C 0.1354(7) 0.2723(7) 0.1736(5) 0.0202(12) Uani 1 d . . H4 H 0.1871(7) 0.2456(7) 0.1072(5) 0.024 Uiso 1 calc R . C5 C 0.0995(6) 0.1587(6) 0.2540(5) 0.0191(11) Uani 1 d . . H5 H 0.1296(6) 0.0558(6) 0.2412(5) 0.023 Uiso 1 calc R . C6 C 0.1348(7) 0.5543(6) 0.1051(5) 0.0179(11) Uani 1 d . . O1 O 0.2128(6) 0.5202(5) 0.0244(4) 0.0327(11) Uani 1 d . . C7 C 0.0763(7) 0.7180(6) 0.1215(5) 0.0219(12) Uani 1 d . . H7A H 0.1096(36) 0.7542(17) 0.2005(12) 0.029 Uiso 1 calc R . H7B H -0.0344(7) 0.7182(10) 0.1111(32) 0.029 Uiso 1 calc R . H7C H 0.1164(34) 0.7862(10) 0.0634(22) 0.029 Uiso 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 Cd1 0.0129(3) 0.0134(3) 0.0138(3) 0.0014(2) 0.0005(2) 0.0001(2) N11 0.023(3) 0.019(2) 0.017(2) 0.002(2) -0.001(2) -0.005(2) N12 0.010(2) 0.023(2) 0.015(2) -0.007(2) -0.002(2) 0.003(2) N13 0.026(3) 0.025(2) 0.028(3) -0.005(2) 0.009(2) -0.006(2) N1 0.019(2) 0.014(2) 0.010(2) 0.005(2) -0.001(2) 0.001(2) C1 0.015(3) 0.019(3) 0.016(2) 0.003(2) 0.005(2) 0.004(2) C2 0.019(3) 0.012(2) 0.020(3) 0.000(2) -0.001(2) 0.001(2) C3 0.011(3) 0.021(3) 0.014(3) 0.004(2) -0.004(2) 0.003(2) C4 0.024(3) 0.025(3) 0.012(2) 0.000(2) 0.006(2) 0.006(2) C5 0.022(3) 0.018(3) 0.017(3) 0.000(2) -0.001(2) 0.002(2) C6 0.019(3) 0.022(3) 0.013(3) 0.003(2) 0.000(2) -0.001(2) O1 0.042(3) 0.028(2) 0.030(2) 0.007(2) 0.019(2) 0.003(2) C7 0.032(3) 0.020(3) 0.014(2) 0.003(2) 0.003(2) -0.001(2) _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 Cd1 6.086(2) 4_565 yes Cd1 N13 2.323(5) 4_565 yes Cd1 N13 2.323(5) 2_546 ? Cd1 N11 2.326(4) 3_556 yes Cd1 N11 2.326(4) . ? Cd1 N1 2.351(4) 3_556 yes Cd1 N1 2.351(4) . ? N11 N12 1.184(6) . yes N12 N13 1.183(7) . yes N13 Cd1 2.323(5) 2_556 ? N1 C1 1.340(7) . ? N1 C5 1.351(7) . ? C1 C2 1.393(7) . ? C1 H1 0.93 . ? C2 C3 1.386(8) . ? C2 H2 0.93 . ? C3 C4 1.386(8) . ? C3 C6 1.527(7) . ? C4 C5 1.377(7) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? C6 O1 1.210(7) . ? C6 C7 1.501(8) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? 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 N13 Cd1 N13 180.0 4_565 2_546 ? N13 Cd1 N11 90.4(2) 4_565 3_556 ? N13 Cd1 N11 89.6(2) 2_546 3_556 ? N13 Cd1 N11 89.6(2) 4_565 . ? N13 Cd1 N11 90.4(2) 2_546 . yes N11 Cd1 N11 180.0 3_556 . ? N13 Cd1 N1 87.6(2) 4_565 3_556 ? N13 Cd1 N1 92.4(2) 2_546 3_556 ? N11 Cd1 N1 88.37(15) 3_556 3_556 ? N11 Cd1 N1 91.63(15) . 3_556 yes N13 Cd1 N1 92.4(2) 4_565 . yes N13 Cd1 N1 87.6(2) 2_546 . ? N11 Cd1 N1 91.63(15) 3_556 . ? N11 Cd1 N1 88.37(15) . . ? N1 Cd1 N1 180.0 3_556 . ? N12 N11 Cd1 120.5(3) . . yes N13 N12 N11 176.7(5) . . yes N12 N13 Cd1 149.0(4) . 2_556 yes C1 N1 C5 117.9(4) . . ? C1 N1 Cd1 120.6(3) . . ? C5 N1 Cd1 120.6(3) . . ? N1 C1 C2 122.5(5) . . ? N1 C1 H1 118.8(3) . . ? C2 C1 H1 118.8(3) . . ? C3 C2 C1 119.2(5) . . ? C3 C2 H2 120.4(3) . . ? C1 C2 H2 120.4(3) . . ? C2 C3 C4 118.3(5) . . ? C2 C3 C6 121.7(5) . . ? C4 C3 C6 120.0(5) . . ? C5 C4 C3 119.4(5) . . ? C5 C4 H4 120.3(3) . . ? C3 C4 H4 120.3(3) . . ? N1 C5 C4 122.7(5) . . ? N1 C5 H5 118.6(3) . . ? C4 C5 H5 118.6(3) . . ? O1 C6 C7 122.1(5) . . ? O1 C6 C3 119.0(5) . . ? C7 C6 C3 118.9(5) . . ? C6 C7 H7A 109.5(3) . . ? C6 C7 H7B 109.5(3) . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5(3) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 N13 Cd1 N11 N12 -103.5(4) 4_565 . . . ? N13 Cd1 N11 N12 76.5(4) 2_546 . . . ? N11 Cd1 N11 N12 91.2(1000) 3_556 . . . ? N1 Cd1 N11 N12 168.9(4) 3_556 . . . ? N1 Cd1 N11 N12 -11.1(4) . . . . ? Cd1 N11 N12 N13 134.1(95) . . . . ? N11 N12 N13 Cd1 133.6(92) . . . 2_556 ? N13 Cd1 N1 C1 34.2(4) 4_565 . . . ? N13 Cd1 N1 C1 -145.8(4) 2_546 . . . ? N11 Cd1 N1 C1 124.7(4) 3_556 . . . ? N11 Cd1 N1 C1 -55.3(4) . . . . ? N1 Cd1 N1 C1 -136.3(1000) 3_556 . . . ? N13 Cd1 N1 C5 -156.8(4) 4_565 . . . ? N13 Cd1 N1 C5 23.2(4) 2_546 . . . ? N11 Cd1 N1 C5 -66.2(4) 3_556 . . . ? N11 Cd1 N1 C5 113.8(4) . . . . ? N1 Cd1 N1 C5 32.8(1000) 3_556 . . . ? C5 N1 C1 C2 0.6(8) . . . . ? Cd1 N1 C1 C2 170.0(4) . . . . ? N1 C1 C2 C3 -1.0(8) . . . . ? C1 C2 C3 C4 1.4(8) . . . . ? C1 C2 C3 C6 -179.4(5) . . . . ? C2 C3 C4 C5 -1.5(8) . . . . ? C6 C3 C4 C5 179.3(5) . . . . ? C1 N1 C5 C4 -0.8(8) . . . . ? Cd1 N1 C5 C4 -170.1(4) . . . . ? C3 C4 C5 N1 1.2(8) . . . . ? C2 C3 C6 O1 175.7(6) . . . . ? C4 C3 C6 O1 -5.2(8) . . . . ? C2 C3 C6 C7 -4.6(8) . . . . ? C4 C3 C6 C7 174.6(6) . . . . ? _refine_diff_density_max 1.034 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.137 #========================================================= data_cd4bra _database_code_CSD 180364 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Cd3(N3)6(4-bromopyridine)4]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H16 Br4 Cd3 N22' _chemical_formula_weight 1221.39 _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' 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.814(2) _cell_length_b 9.367(2) _cell_length_c 13.274(5) _cell_angle_alpha 82.08(2) _cell_angle_beta 81.58(2) _cell_angle_gamma 88.91(2) _cell_volume 830.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 7.2 _cell_measurement_theta_max 14.6 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.443 _exptl_crystal_density_method ? _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 6.772 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle diffractometer' _diffrn_measurement_method 'Omega-scan; delta Omega: 1.10 deg.' _diffrn_standards_number '3 (2 0 2; 1 2 3; -1 -2 3)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '90 min' _diffrn_standards_decay_% 4 _diffrn_reflns_number 3319 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2908 _reflns_number_observed 2455 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+0.6019P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2894 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_obs 0.0375 _refine_ls_wR_factor_all 0.0855 _refine_ls_wR_factor_obs 0.0783 _refine_ls_goodness_of_fit_all 1.074 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.094 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.0087(2) Uani 1 d S . Cd2 Cd 0.24906(7) 0.41721(5) -0.02141(4) 0.00851(13) Uani 1 d . . Br1 Br 0.25044(11) 0.10893(8) -0.53489(5) 0.0210(2) Uani 1 d . . N1 N 0.0966(8) 0.0477(6) -0.1780(4) 0.0118(12) Uani 1 d . . C1 C 0.0689(10) 0.1738(7) -0.2344(5) 0.0158(15) Uani 1 d . . H1 H 0.0142(10) 0.2490(7) -0.2006(5) 0.019 Uiso 1 calc R . C2 C 0.1168(10) 0.1989(7) -0.3401(5) 0.0159(15) Uani 1 d . . H2 H 0.0999(10) 0.2893(7) -0.3767(5) 0.019 Uiso 1 calc R . C3 C 0.1908(9) 0.0845(8) -0.3893(5) 0.0147(15) Uani 1 d . . C4 C 0.2213(10) -0.0454(8) -0.3337(5) 0.0168(15) Uani 1 d . . H4 H 0.2739(10) -0.1224(8) -0.3662(5) 0.020 Uiso 1 calc R . C5 C 0.1729(10) -0.0601(7) -0.2295(5) 0.0149(15) Uani 1 d . . H5 H 0.1936(10) -0.1491(7) -0.1919(5) 0.018 Uiso 1 calc R . Br2 Br 0.77732(11) 0.36130(8) -0.50449(5) 0.0191(2) Uani 1 d . . N2 N 0.4410(8) 0.3882(6) -0.1768(4) 0.0115(12) Uani 1 d . . C6 C 0.4946(10) 0.5069(7) -0.2449(6) 0.018(2) Uani 1 d . . H6 H 0.4612(10) 0.5967(7) -0.2250(6) 0.022 Uiso 1 calc R . C7 C 0.5952(10) 0.5019(7) -0.3412(5) 0.0156(15) Uani 1 d . . H7 H 0.6284(10) 0.5861(7) -0.3860(5) 0.019 Uiso 1 calc R . C8 C 0.6464(10) 0.3688(8) -0.3703(5) 0.0142(14) Uani 1 d . . C9 C 0.5999(9) 0.2446(7) -0.3024(5) 0.0142(14) Uani 1 d . . H9 H 0.6352(9) 0.1542(7) -0.3207(5) 0.017 Uiso 1 calc R . C10 C 0.4984(10) 0.2597(7) -0.2057(5) 0.0167(15) Uani 1 d . . H10 H 0.4687(10) 0.1772(7) -0.1587(5) 0.020 Uiso 1 calc R . N11 N -0.0206(8) 0.5008(6) -0.1062(4) 0.0107(11) Uani 1 d . . N12 N 0.0026(8) 0.5563(6) -0.1938(5) 0.0157(13) Uani 1 d . . N13 N 0.0278(10) 0.6103(8) -0.2788(5) 0.034(2) Uani 1 d . . N21 N 0.1964(8) 0.1799(6) 0.0407(4) 0.0125(12) Uani 1 d . . N22 N 0.2740(8) 0.1373(6) 0.1163(4) 0.0127(12) Uani 1 d . . N23 N 0.3454(9) 0.0955(6) 0.1882(5) 0.0196(13) Uani 1 d . . N31 N -0.2553(8) 0.1622(6) -0.0251(5) 0.0154(13) Uani 1 d . . N32 N -0.3288(8) 0.2608(6) 0.0081(4) 0.0096(12) Uani 1 d . . N33 N -0.4113(8) 0.3620(6) 0.0401(4) 0.0112(12) Uani 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 Cd1 0.0078(3) 0.0070(3) 0.0119(3) -0.0023(3) -0.0025(3) 0.0005(2) Cd2 0.0082(2) 0.0062(2) 0.0111(2) -0.0009(2) -0.0017(2) 0.0000(2) Br1 0.0236(4) 0.0231(4) 0.0151(4) -0.0004(3) -0.0008(3) -0.0018(3) N1 0.006(3) 0.015(3) 0.015(3) -0.002(2) -0.004(2) 0.001(2) C1 0.010(3) 0.014(3) 0.023(4) -0.002(3) -0.004(3) -0.002(3) C2 0.013(3) 0.014(3) 0.019(4) 0.004(3) -0.005(3) 0.001(3) C3 0.005(3) 0.027(4) 0.013(3) -0.002(3) -0.003(3) -0.002(3) C4 0.015(4) 0.020(4) 0.015(4) -0.009(3) 0.002(3) 0.001(3) C5 0.019(4) 0.009(3) 0.018(4) -0.003(3) -0.004(3) -0.002(3) Br2 0.0188(4) 0.0255(4) 0.0127(3) -0.0034(3) -0.0008(3) 0.0010(3) N2 0.005(3) 0.011(3) 0.019(3) -0.002(2) -0.005(2) 0.001(2) C6 0.014(4) 0.018(4) 0.021(4) -0.002(3) 0.000(3) 0.001(3) C7 0.018(4) 0.012(3) 0.017(4) 0.004(3) -0.006(3) -0.004(3) C8 0.008(3) 0.028(4) 0.007(3) -0.005(3) -0.001(3) 0.002(3) C9 0.006(3) 0.019(4) 0.021(4) -0.009(3) -0.006(3) 0.003(3) C10 0.017(4) 0.016(4) 0.016(4) 0.002(3) -0.006(3) -0.002(3) N11 0.008(3) 0.013(3) 0.011(3) 0.000(2) -0.003(2) 0.002(2) N12 0.014(3) 0.013(3) 0.023(4) -0.009(3) -0.004(3) 0.000(2) N13 0.032(4) 0.052(5) 0.013(4) 0.003(3) 0.001(3) 0.003(3) N21 0.015(2) 0.007(2) 0.016(2) -0.001(2) -0.005(2) 0.000(2) N22 0.009(2) 0.010(2) 0.018(2) -0.001(2) -0.001(2) -0.004(2) N23 0.018(3) 0.020(3) 0.019(3) 0.007(3) -0.007(3) -0.006(3) N31 0.014(3) 0.011(3) 0.024(3) -0.006(3) -0.009(3) 0.006(2) N32 0.006(3) 0.012(3) 0.011(3) 0.002(2) -0.003(2) -0.002(2) N33 0.009(3) 0.009(3) 0.017(3) -0.005(2) -0.004(2) -0.002(2) _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 N31 2.319(5) 2 yes Cd1 N31 2.319(5) . yes Cd1 N21 2.339(5) 2 yyes Cd1 N21 2.339(5) . yes Cd1 N1 2.341(6) 2 yes Cd1 N1 2.341(6) . yes Cd1 Cd2 4.247(1) . yes Cd1 Cd2 5.718(1) 2_565 yes Cd1 Cd2 5.718(1) 1_545 yes Cd2 Cd2 3.705(1) 2_565 yes Cd2 N21 2.278(5) . yes Cd2 N2 2.322(6) . yes Cd2 N11 2.329(5) 2_565 yes Cd2 N33 2.330(5) 2_565 yes Cd2 N11 2.359(5) . yes N33 Cd2 2.330(5) 2_565 yes N33 Cd2 2.585(5) 1_455 yes Cd2 N33 2.585(5) 1_655 yes Br1 C3 1.899(7) . ? N1 C1 1.334(8) . ? N1 C5 1.351(8) . ? C1 C2 1.381(10) . ? C1 H1 0.93 . ? C2 C3 1.380(10) . ? C2 H2 0.93 . ? C3 C4 1.362(10) . ? C4 C5 1.363(10) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? Br2 C8 1.882(6) . ? N2 C10 1.346(9) . ? N2 C6 1.352(9) . ? C6 C7 1.366(10) . ? C6 H6 0.93 . ? C7 C8 1.379(10) . ? C7 H7 0.93 . ? C8 C9 1.381(10) . ? C9 C10 1.390(10) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? N11 N12 1.195(8) . yes N11 Cd2 2.329(5) 2_565 yes N12 N13 1.161(9) . yes N21 N22 1.217(8) . yes N22 N23 1.152(8) . yes N31 N32 1.152(8) . yes N32 N33 1.190(8) . yes 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 N31 Cd1 N31 180.0 2 . yes N31 Cd1 N21 91.4(2) 2 2 yes N31 Cd1 N21 88.6(2) . 2 yes N31 Cd1 N21 88.6(2) 2 . yes N31 Cd1 N21 91.4(2) . . yes N21 Cd1 N21 180.0 2 . yes N31 Cd1 N1 86.0(2) 2 2 yes N31 Cd1 N1 94.0(2) . 2 yes N21 Cd1 N1 95.6(2) 2 2 yes N21 Cd1 N1 84.4(2) . 2 yes N31 Cd1 N1 94.0(2) 2 . yes N31 Cd1 N1 86.0(2) . . yes N21 Cd1 N1 84.4(2) 2 . yes N21 Cd1 N1 95.6(2) . . yes N1 Cd1 N1 180.0 2 . yes N21 Cd2 N2 98.2(2) . . yes N21 Cd2 N11 94.3(2) . 2_565 yes N2 Cd2 N11 164.1(2) . 2_565 yes N21 Cd2 N33 154.8(2) . 2_565 yes N2 Cd2 N33 84.9(2) . 2_565 yes N11 Cd2 N33 88.0(2) 2_565 2_565 yes N21 Cd2 N11 108.1(2) . . yes N2 Cd2 N11 91.1(2) . . yes N11 Cd2 N11 75.6(2) 2_565 . yes N33 Cd2 N11 96.8(2) 2_565 . yes N21 Cd2 N33 81.9(2) . 1_655 yes N2 Cd2 N33 80.1(2) . 1_655 yes N11 Cd2 N33 111.6(2) 2_565 1_655 yes N33 Cd2 N33 74.0(2) 2_565 1_655 yes N11 Cd2 N33 167.7(2) . 1_655 yes C1 N1 C5 116.7(6) . . ? C1 N1 Cd1 124.0(5) . . ? C5 N1 Cd1 119.1(4) . . ? N1 C1 C2 123.7(7) . . ? N1 C1 H1 118.1(4) . . ? C2 C1 H1 118.1(4) . . ? C3 C2 C1 117.3(6) . . ? C3 C2 H2 121.3(4) . . ? C1 C2 H2 121.3(4) . . ? C4 C3 C2 120.3(6) . . ? C4 C3 Br1 120.0(5) . . ? C2 C3 Br1 119.7(5) . . ? C3 C4 C5 118.5(7) . . ? C3 C4 H4 120.7(4) . . ? C5 C4 H4 120.7(4) . . ? N1 C5 C4 123.4(6) . . ? N1 C5 H5 118.3(4) . . ? C4 C5 H5 118.3(4) . . ? C10 N2 C6 117.1(6) . . ? C10 N2 Cd2 124.3(4) . . ? C6 N2 Cd2 118.5(4) . . ? N2 C6 C7 123.5(7) . . ? N2 C6 H6 118.3(4) . . ? C7 C6 H6 118.3(4) . . ? C6 C7 C8 118.3(6) . . ? C6 C7 H7 120.9(4) . . ? C8 C7 H7 120.9(4) . . ? C7 C8 C9 120.4(6) . . ? C7 C8 Br2 118.4(5) . . ? C9 C8 Br2 121.2(5) . . ? C8 C9 C10 117.4(6) . . ? C8 C9 H9 121.3(4) . . ? C10 C9 H9 121.3(4) . . ? N2 C10 C9 123.2(6) . . ? N2 C10 H10 118.4(4) . . ? C9 C10 H10 118.4(4) . . ? N12 N11 Cd2 123.3(4) . 2_565 yes N12 N11 Cd2 121.9(4) . . yes Cd2 N11 Cd2 104.4(2) 2_565 . yes N13 N12 N11 179.1(7) . . yes N22 N21 Cd2 114.8(4) . . yes N22 N21 Cd1 111.1(4) . . yes Cd2 N21 Cd1 133.8(3) . . yes N23 N22 N21 179.0(7) . . yes N32 N31 Cd1 140.0(5) . . yes N31 N32 N33 177.2(6) . . yes N32 N33 Cd2 120.5(4) . 2_565 yes N32 N33 Cd2 113.9(4) . 1_455 yes Cd2 N33 Cd2 106.0(2) 2_565 1_455 yes 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 N31 Cd1 N1 C1 -149.2(5) 2 . . . ? N31 Cd1 N1 C1 30.8(5) . . . . ? N21 Cd1 N1 C1 119.8(5) 2 . . . ? N21 Cd1 N1 C1 -60.2(5) . . . . ? N1 Cd1 N1 C1 -11.9(450) 2 . . . ? N31 Cd1 N1 C5 35.6(5) 2 . . . ? N31 Cd1 N1 C5 -144.4(5) . . . . ? N21 Cd1 N1 C5 -55.4(5) 2 . . . ? N21 Cd1 N1 C5 124.6(5) . . . . ? N1 Cd1 N1 C5 172.8(451) 2 . . . ? C5 N1 C1 C2 -1.2(10) . . . . ? Cd1 N1 C1 C2 -176.5(5) . . . . ? N1 C1 C2 C3 2.4(10) . . . . ? C1 C2 C3 C4 -2.5(10) . . . . ? C1 C2 C3 Br1 177.6(5) . . . . ? C2 C3 C4 C5 1.5(10) . . . . ? Br1 C3 C4 C5 -178.6(5) . . . . ? C1 N1 C5 C4 0.0(10) . . . . ? Cd1 N1 C5 C4 175.6(5) . . . . ? C3 C4 C5 N1 -0.2(11) . . . . ? N21 Cd2 N2 C10 -3.1(5) . . . . ? N11 Cd2 N2 C10 -144.4(7) 2_565 . . . ? N33 Cd2 N2 C10 151.7(5) 2_565 . . . ? N11 Cd2 N2 C10 -111.6(5) . . . . ? N33 Cd2 N2 C10 77.1(5) 1_655 . . . ? N21 Cd2 N2 C6 174.8(5) . . . . ? N11 Cd2 N2 C6 33.5(10) 2_565 . . . ? N33 Cd2 N2 C6 -30.4(5) 2_565 . . . ? N11 Cd2 N2 C6 66.3(5) . . . . ? N33 Cd2 N2 C6 -105.0(5) 1_655 . . . ? C10 N2 C6 C7 2.8(10) . . . . ? Cd2 N2 C6 C7 -175.3(5) . . . . ? N2 C6 C7 C8 -0.6(10) . . . . ? C6 C7 C8 C9 -1.3(10) . . . . ? C6 C7 C8 Br2 177.9(5) . . . . ? C7 C8 C9 C10 0.9(10) . . . . ? Br2 C8 C9 C10 -178.3(5) . . . . ? C6 N2 C10 C9 -3.2(10) . . . . ? Cd2 N2 C10 C9 174.7(5) . . . . ? C8 C9 C10 N2 1.4(10) . . . . ? N21 Cd2 N11 N12 -124.3(5) . . . . ? N2 Cd2 N11 N12 -25.4(5) . . . . ? N11 Cd2 N11 N12 145.8(6) 2_565 . . . ? N33 Cd2 N11 N12 59.6(5) 2_565 . . . ? N33 Cd2 N11 N12 18.8(12) 1_655 . . . ? N21 Cd2 N11 Cd2 89.9(2) . . . 2_565 ? N2 Cd2 N11 Cd2 -171.2(2) . . . 2_565 ? N11 Cd2 N11 Cd2 0.0 2_565 . . 2_565 ? N33 Cd2 N11 Cd2 -86.2(2) 2_565 . . 2_565 ? N33 Cd2 N11 Cd2 -127.0(8) 1_655 . . 2_565 ? Cd2 N11 N12 N13 131.3(466) 2_565 . . . ? Cd2 N11 N12 N13 -8.0(470) . . . . ? N2 Cd2 N21 N22 113.3(5) . . . . ? N11 Cd2 N21 N22 -76.6(5) 2_565 . . . ? N33 Cd2 N21 N22 17.9(8) 2_565 . . . ? N11 Cd2 N21 N22 -152.8(4) . . . . ? N33 Cd2 N21 N22 34.6(5) 1_655 . . . ? N2 Cd2 N21 Cd1 -73.2(4) . . . . ? N11 Cd2 N21 Cd1 96.9(3) 2_565 . . . ? N33 Cd2 N21 Cd1 -168.6(3) 2_565 . . . ? N11 Cd2 N21 Cd1 20.7(4) . . . . ? N33 Cd2 N21 Cd1 -151.9(4) 1_655 . . . ? N31 Cd1 N21 N22 -45.1(5) 2 . . . ? N31 Cd1 N21 N22 134.9(5) . . . . ? N21 Cd1 N21 N22 154.1(915) 2 . . . ? N1 Cd1 N21 N22 41.0(4) 2 . . . ? N1 Cd1 N21 N22 -139.0(4) . . . . ? N31 Cd1 N21 Cd2 141.3(4) 2 . . . ? N31 Cd1 N21 Cd2 -38.7(4) . . . . ? N21 Cd1 N21 Cd2 -19.6(874) 2 . . . ? N1 Cd1 N21 Cd2 -132.6(4) 2 . . . ? N1 Cd1 N21 Cd2 47.4(4) . . . . ? Cd2 N21 N22 N23 155.7(379) . . . . ? Cd1 N21 N22 N23 -19.2(382) . . . . ? N31 Cd1 N31 N32 -101.8(1000) 2 . . . ? N21 Cd1 N31 N32 143.8(8) 2 . . . ? N21 Cd1 N31 N32 -36.2(8) . . . . ? N1 Cd1 N31 N32 48.3(8) 2 . . . ? N1 Cd1 N31 N32 -131.7(8) . . . . ? Cd1 N31 N32 N33 -166.3(123) . . . . ? N31 N32 N33 Cd2 -126.5(126) . . . 2_565 ? N31 N32 N33 Cd2 1.2(130) . . . 1_455 ? _refine_diff_density_max 0.787 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.170 #========================================================= _eof