Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _audit_creation_date 19-09-2002 _audit_creation_method 'from SHELXL97 CIF and IUCr SHELXL97-template' _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof Jan Reedijk' _publ_contact_author_address ; Leiden Institute of Chemistry Leiden University P.O. Box 9502 Leiden 2596 XT NETHERLANDS ; _publ_contact_author_phone 31(30)2532533 _publ_contact_author_fax 31(30)2533940 _publ_contact_author_email REEDIJK@CHEM.LEIDENUNIV.NL _publ_contact_letter ; 20-03-2002 This CIF (s2529a_ccdc.cif) contains the supplementary crystallographic data for our submission to Dalton Transactions. The CIF describes the crystal structure of \a-[Cu(teeOMe)~2~Br~2~] at three different temperatures (123, 150 and 297 K). If you require any further information, please contact me. Allison Mills ; _publ_requested_journal 'Dalton Trans.' _publ_section_title ; Linkage isomers of dibromobis(1-(2-methoxyethyl)tetrazole)copper(II) containing either a bromide or a unique tetrazole bridge. ; # AUTHOR LIST loop_ _publ_author_name 'Jan Reedijk' 'M. Grunert' 'Jaap G. Haasnoot' 'W. Linert' 'Allison M. Mills' 'Anthony L. Spek' 'A. F. Stassen' # CRYSTAL DATA # STRUCTURE 1 (\a-[Cu(teeOMe)~2~Br~2~], 123 K) data_1_s2529a_123K _database_code_CSD 207021 _chemical_name_systematic ; catena-Poly[[trans-dibromocopper(II)]-bis-\m-1-(2-methoxyethyl)tetrazole- \k^2^N^2^:N^4^] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Br2 Cu N8 O2' _chemical_formula_sum 'C8 H16 Br2 Cu N8 O2' _chemical_formula_weight 479.65 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.955(3) _cell_length_b 8.3625(19) _cell_length_c 8.957(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.909(4) _cell_angle_gamma 90.00 _cell_volume 789.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 973 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 29.9 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_crystal_preparation 'recrystallized from methanol' _exptl_absorpt_coefficient_mu 6.464 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.174 _exptl_absorpt_correction_T_max 0.280 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; \a-isomer, recrystallized from methanol (structure of \b-isomer, recrystallized from ethanol, unknown) ; _diffrn_ambient_temperature 123(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 Smart CCD platform 3-circle' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8047 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2239 _reflns_number_gt 1944 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT, SADABS, XPREP (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL (Bruker AXS, 2000)' _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^)+(0.0475P)^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 'SHELXL (Sheldrick, 1997)' _refine_ls_extinction_coef 0.0043(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2239 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Br1 Br -0.21427(2) 0.09022(2) -0.01580(2) 0.01456(9) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 0.0000 0.01147(10) Uani 1 2 d S . . O8 O 0.40115(18) 0.1193(3) 0.5721(2) 0.0305(4) Uani 1 1 d . . . N1 N 0.14011(18) 0.0725(2) 0.4694(2) 0.0126(4) Uani 1 1 d . . . N2 N 0.06617(18) 0.2029(2) 0.4274(2) 0.0165(4) Uani 1 1 d . . . N3 N 0.01773(18) 0.1958(2) 0.2793(2) 0.0161(4) Uani 1 1 d . . . N4 N 0.05939(17) 0.0618(2) 0.2232(2) 0.0121(3) Uani 1 1 d . . . C5 C 0.1362(2) -0.0125(2) 0.3426(2) 0.0128(4) Uani 1 1 d . . . H5 H 0.1807 -0.1092 0.3387 0.015 Uiso 1 1 calc R . . C6 C 0.2137(2) 0.0440(3) 0.6307(3) 0.0167(4) Uani 1 1 d . . . H6A H 0.2419 -0.0689 0.6427 0.020 Uiso 1 1 calc R . . H6B H 0.1594 0.0633 0.7008 0.020 Uiso 1 1 calc R . . C7 C 0.3279(2) 0.1522(3) 0.6753(3) 0.0201(5) Uani 1 1 d . . . H7A H 0.3010 0.2657 0.6668 0.024 Uiso 1 1 calc R . . H7B H 0.3777 0.1311 0.7836 0.024 Uiso 1 1 calc R . . C9 C 0.5103(3) 0.2186(4) 0.5999(4) 0.0415(8) Uani 1 1 d . . . H9A H 0.4839 0.3309 0.5872 0.062 Uiso 1 1 calc R . . H9B H 0.5584 0.1923 0.5257 0.062 Uiso 1 1 calc R . . H9C H 0.5637 0.2012 0.7058 0.062 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 Br1 0.01430(13) 0.01415(13) 0.01530(13) -0.00139(7) 0.00418(9) 0.00199(7) Cu1 0.01408(19) 0.00984(17) 0.01033(18) -0.00091(12) 0.00306(14) 0.00187(12) O8 0.0195(9) 0.0387(11) 0.0347(11) -0.0053(9) 0.0100(8) -0.0066(8) N1 0.0144(9) 0.0105(8) 0.0131(9) 0.0003(6) 0.0043(7) -0.0009(6) N2 0.0177(9) 0.0138(9) 0.0174(9) -0.0034(7) 0.0038(7) 0.0029(7) N3 0.0204(9) 0.0109(8) 0.0157(9) -0.0036(7) 0.0028(7) 0.0031(7) N4 0.0147(9) 0.0083(8) 0.0136(8) -0.0013(6) 0.0043(7) 0.0006(6) C5 0.0154(10) 0.0093(9) 0.0139(10) -0.0017(7) 0.0046(8) -0.0009(7) C6 0.0212(11) 0.0164(10) 0.0119(10) 0.0018(8) 0.0035(9) -0.0018(8) C7 0.0210(11) 0.0199(11) 0.0162(10) -0.0015(8) -0.0002(9) -0.0032(9) C9 0.0202(13) 0.055(2) 0.0441(18) 0.0124(15) 0.0005(12) -0.0116(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu1 2.4325(7) . . ? Cu1 N4 1.9935(18) . . ? O8 C7 1.407(3) . . ? O8 C9 1.421(4) . . ? N1 N2 1.349(3) . . ? N1 C5 1.331(2) . . ? N1 C6 1.468(3) . . ? N2 N3 1.288(2) . . ? N3 N4 1.357(2) . . ? N4 C5 1.321(3) . . ? C6 C7 1.506(3) . . ? C5 H5 0.9498 . . ? C6 H6A 0.9900 . . ? C6 H6B 0.9894 . . ? C7 H7A 0.9906 . . ? C7 H7B 0.9898 . . ? C9 H9A 0.9800 . . ? C9 H9B 0.9797 . . ? C9 H9C 0.9792 . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Cu1 N4 91.28(5) . . . ? Br1 Cu1 Br1 180.00 . . 3_555 ? Br1 Cu1 N4 88.72(5) . . 3_555 ? Br1 Cu1 N4 88.72(5) 3_555 . . ? N4 Cu1 N4 180.00 . . 3_555 ? Br1 Cu1 N4 91.28(5) 3_555 . 3_555 ? C7 O8 C9 112.0(2) . . . ? N2 N1 C5 108.51(16) . . . ? N2 N1 C6 122.10(17) . . . ? C5 N1 C6 129.33(18) . . . ? N1 N2 N3 107.24(16) . . . ? Cu1 N2 N1 148.41(13) 2_555 . . ? Cu1 N2 N3 103.12(12) 2_555 . . ? N2 N3 N4 109.51(17) . . . ? Cu1 N4 N3 122.34(13) . . . ? Cu1 N4 C5 130.57(14) . . . ? N3 N4 C5 107.03(16) . . . ? N1 C5 N4 107.71(17) . . . ? N1 C6 C7 110.8(2) . . . ? O8 C7 C6 106.9(2) . . . ? N1 C5 H5 126.12 . . . ? N4 C5 H5 126.17 . . . ? N1 C6 H6A 109.42 . . . ? N1 C6 H6B 109.54 . . . ? C7 C6 H6A 109.40 . . . ? C7 C6 H6B 109.50 . . . ? H6A C6 H6B 108.10 . . . ? O8 C7 H7A 110.37 . . . ? O8 C7 H7B 110.40 . . . ? C6 C7 H7A 110.32 . . . ? C6 C7 H7B 110.33 . . . ? H7A C7 H7B 108.58 . . . ? O8 C9 H9A 109.41 . . . ? O8 C9 H9B 109.47 . . . ? O8 C9 H9C 109.49 . . . ? H9A C9 H9B 109.44 . . . ? H9A C9 H9C 109.50 . . . ? H9B C9 H9C 109.52 . . . ? 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 Br1 Cu1 N4 N3 -38.23(16) . . . . ? Br1 Cu1 N4 C5 138.51(19) . . . . ? Br1 Cu1 N4 N3 141.77(16) 3_555 . . . ? Br1 Cu1 N4 C5 -41.49(19) 3_555 . . . ? C9 O8 C7 C6 178.1(2) . . . . ? C6 N1 C5 N4 -178.2(2) . . . . ? N2 N1 C6 C7 -74.7(3) . . . . ? C5 N1 C6 C7 102.1(3) . . . . ? C5 N1 N2 N3 0.7(2) . . . . ? C5 N1 N2 Cu1 -162.7(2) . . . 2_555 ? C6 N1 N2 N3 178.13(19) . . . . ? C6 N1 N2 Cu1 14.7(4) . . . 2_555 ? N2 N1 C5 N4 -1.0(2) . . . . ? Cu1 N2 N3 N4 171.03(13) 2_555 . . . ? N1 N2 N3 N4 -0.1(2) . . . . ? N2 N3 N4 Cu1 176.91(14) . . . . ? N2 N3 N4 C5 -0.5(2) . . . . ? N3 N4 C5 N1 0.9(2) . . . . ? Cu1 N4 C5 N1 -176.19(15) . . . . ? N1 C6 C7 O8 -59.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.228 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.134 #===END # STRUCTURE 2 (\a-[Cu(teeOMe)~2~Br~2~], 150 K) data_2_s2529a_150K _database_code_CSD 207022 _chemical_name_systematic ; catena-Poly[[trans-dibromocopper(II)]-bis-\m-1-(2-methoxyethyl)tetrazole- \k^2^N^2^:N^4^] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Br2 Cu N8 O2' _chemical_formula_sum 'C8 H16 Br2 Cu N8 O2' _chemical_formula_weight 479.65 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.0015(2) _cell_length_b 8.3934(1) _cell_length_c 8.9823(1) _cell_angle_alpha 90.00 _cell_angle_beta 105.989(1) _cell_angle_gamma 90.00 _cell_volume 797.34(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17243 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_crystal_preparation 'recrystallized from methanol' _exptl_absorpt_coefficient_mu 6.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_T_max 0.684 _exptl_absorpt_process_details 'MULABS in PLATON (Spek, 2002)' _exptl_special_details ; \a-isomer, recrystallized from methanol (structure of \b-isomer, recrystallized from ethanol, unknown) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11042 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1817 _reflns_number_gt 1640 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2002)' _computing_publication_material 'PLATON (Spek, 2002)' _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^)+(0.0649P)^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 1817 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Br1 Br -0.21365(2) 0.09049(3) -0.01586(3) 0.01864(14) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 0.0000 0.01483(15) Uani 1 2 d S . . O8 O 0.4010(2) 0.1204(3) 0.5731(3) 0.0390(6) Uani 1 1 d . . . N1 N 0.1406(2) 0.0721(3) 0.4691(3) 0.0160(5) Uani 1 1 d . . . N2 N 0.0669(2) 0.2028(3) 0.4268(3) 0.0196(5) Uani 1 1 d . . . N3 N 0.0184(2) 0.1953(3) 0.2793(3) 0.0197(5) Uani 1 1 d . . . N4 N 0.0594(2) 0.0613(3) 0.2232(3) 0.0155(5) Uani 1 1 d . . . C5 C 0.1358(3) -0.0127(3) 0.3426(3) 0.0165(5) Uani 1 1 d . . . H5 H 0.1796 -0.1095 0.3387 0.020 Uiso 1 1 calc R . . C6 C 0.2136(3) 0.0439(3) 0.6303(3) 0.0212(6) Uani 1 1 d . . . H6A H 0.2416 -0.0686 0.6428 0.025 Uiso 1 1 calc R . . H6B H 0.1593 0.0636 0.6998 0.025 Uiso 1 1 calc R . . C7 C 0.3272(3) 0.1517(4) 0.6748(4) 0.0260(7) Uani 1 1 d . . . H7A H 0.3001 0.2646 0.6664 0.031 Uiso 1 1 calc R . . H7B H 0.3766 0.1307 0.7829 0.031 Uiso 1 1 calc R . . C9 C 0.5097(4) 0.2180(6) 0.6005(5) 0.0556(12) Uani 1 1 d . . . H9A H 0.4848 0.3301 0.6004 0.083 Uiso 1 1 calc R . . H9B H 0.5517 0.2004 0.5189 0.083 Uiso 1 1 calc R . . H9C H 0.5679 0.1911 0.7012 0.083 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 Br1 0.0214(2) 0.01753(19) 0.0165(2) -0.00190(9) 0.00433(14) 0.00248(9) Cu1 0.0213(3) 0.0120(2) 0.0104(3) -0.00115(16) 0.0029(2) 0.00227(16) O8 0.0289(13) 0.0500(14) 0.0379(15) -0.0057(12) 0.0090(11) -0.0061(11) N1 0.0218(12) 0.0140(10) 0.0121(12) 0.0008(8) 0.0043(10) -0.0011(8) N2 0.0260(13) 0.0146(11) 0.0162(12) -0.0035(9) 0.0026(10) 0.0029(9) N3 0.0272(13) 0.0120(10) 0.0182(13) -0.0036(9) 0.0034(10) 0.0033(9) N4 0.0218(12) 0.0099(10) 0.0144(12) -0.0012(9) 0.0046(10) 0.0002(8) C5 0.0201(14) 0.0122(12) 0.0160(13) 0.0000(10) 0.0031(11) -0.0008(10) C6 0.0326(16) 0.0195(13) 0.0092(13) 0.0037(11) 0.0018(12) -0.0001(12) C7 0.0297(16) 0.0245(15) 0.0186(16) -0.0013(12) -0.0019(13) -0.0029(12) C9 0.031(2) 0.076(3) 0.054(3) 0.018(2) 0.0005(18) -0.015(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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu1 2.4367(2) . . ? Cu1 N4 1.997(3) . . ? O8 C7 1.404(4) . . ? O8 C9 1.414(5) . . ? N1 N2 1.355(3) . . ? N1 C5 1.329(4) . . ? N1 C6 1.469(4) . . ? N2 N3 1.286(4) . . ? N3 N4 1.359(4) . . ? N4 C5 1.321(4) . . ? C6 C7 1.505(5) . . ? C5 H5 0.9502 . . ? C6 H6A 0.9900 . . ? C6 H6B 0.9896 . . ? C7 H7A 0.9900 . . ? C7 H7B 0.9892 . . ? C9 H9A 0.9799 . . ? C9 H9B 0.9793 . . ? C9 H9C 0.9798 . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Cu1 N4 91.26(7) . . . ? Br1 Cu1 Br1 180.00 . . 3_555 ? Br1 Cu1 N4 88.74(7) . . 3_555 ? Br1 Cu1 N4 88.74(7) 3_555 . . ? N4 Cu1 N4 180.00 . . 3_555 ? Br1 Cu1 N4 91.26(7) 3_555 . 3_555 ? C7 O8 C9 113.0(3) . . . ? N2 N1 C5 108.3(2) . . . ? N2 N1 C6 122.0(2) . . . ? C5 N1 C6 129.7(2) . . . ? N1 N2 N3 107.2(2) . . . ? Cu1 N2 N1 148.43(19) 2_555 . . ? Cu1 N2 N3 103.28(17) 2_555 . . ? N2 N3 N4 109.7(2) . . . ? Cu1 N4 N3 122.35(19) . . . ? Cu1 N4 C5 130.7(2) . . . ? N3 N4 C5 106.9(2) . . . ? N1 C5 N4 108.0(2) . . . ? N1 C6 C7 110.7(2) . . . ? O8 C7 C6 107.5(3) . . . ? N1 C5 H5 126.03 . . . ? N4 C5 H5 125.99 . . . ? N1 C6 H6A 109.52 . . . ? N1 C6 H6B 109.50 . . . ? C7 C6 H6A 109.49 . . . ? C7 C6 H6B 109.48 . . . ? H6A C6 H6B 108.11 . . . ? O8 C7 H7A 110.21 . . . ? O8 C7 H7B 110.21 . . . ? C6 C7 H7A 110.16 . . . ? C6 C7 H7B 110.19 . . . ? H7A C7 H7B 108.53 . . . ? O8 C9 H9A 109.47 . . . ? O8 C9 H9B 109.46 . . . ? O8 C9 H9C 109.48 . . . ? H9A C9 H9B 109.48 . . . ? H9A C9 H9C 109.48 . . . ? H9B C9 H9C 109.46 . . . ? 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 Br1 Cu1 N4 N3 -38.5(2) . . . . ? Br1 Cu1 N4 C5 138.5(3) . . . . ? Br1 Cu1 N4 N3 141.5(2) 3_555 . . . ? Br1 Cu1 N4 C5 -41.5(3) 3_555 . . . ? C9 O8 C7 C6 178.4(3) . . . . ? C6 N1 C5 N4 -178.4(3) . . . . ? N2 N1 C6 C7 -74.6(3) . . . . ? C5 N1 C6 C7 102.7(3) . . . . ? C5 N1 N2 N3 0.6(3) . . . . ? C5 N1 N2 Cu1 -163.7(3) . . . 2_555 ? C6 N1 N2 N3 178.4(2) . . . . ? C6 N1 N2 Cu1 14.1(5) . . . 2_555 ? N2 N1 C5 N4 -0.9(3) . . . . ? Cu1 N2 N3 N4 171.48(16) 2_555 . . . ? N1 N2 N3 N4 -0.2(3) . . . . ? N2 N3 N4 Cu1 177.25(18) . . . . ? N2 N3 N4 C5 -0.4(3) . . . . ? N3 N4 C5 N1 0.8(3) . . . . ? Cu1 N4 C5 N1 -176.57(19) . . . . ? N1 C6 C7 O8 -58.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.251 _refine_diff_density_min -1.534 _refine_diff_density_rms 0.175 #===END # STRUCTURE 3 (\a-[Cu(teeOMe)~2~Br~2~], 297 K) data_3_s2529_297K _database_code_CSD 207023 _chemical_name_systematic ; catena-Poly[[trans-dibromocopper(II)]-bis-\m-1-(2-methoxyethyl)tetrazole- \k^2^N^2^:N^4^] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Br2 Cu N8 O2' _chemical_formula_sum 'C8 H16 Br2 Cu N8 O2' _chemical_formula_weight 479.65 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.116(7) _cell_length_b 8.489(5) _cell_length_c 9.023(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.293(12) _cell_angle_gamma 90.00 _cell_volume 817.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 910 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 29.9 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.949 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_crystal_preparation 'recrystallized from methanol' _exptl_absorpt_coefficient_mu 6.242 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.177 _exptl_absorpt_correction_T_max 0.290 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; \a-isomer, recrystallized from methanol (structure of \b-isomer, recrystallized from ethanol, unknown) ; _diffrn_ambient_temperature 297(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 Smart CCD platform 3-circle' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5920 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2317 _reflns_number_gt 1990 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT, SADABS, XPREP (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL (Bruker AXS, 2000)' _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^)+(0.0521P)^2^+0.2805P] 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 SHELXL _refine_ls_extinction_coef 0.0095(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2317 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 0.798 _refine_ls_restrained_S_all 0.798 _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 Br1 Br -0.210514(19) 0.09209(3) -0.01560(2) 0.03523(9) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 0.0000 0.02660(10) Uani 1 2 d S . . O8 O 0.4000(2) 0.1231(4) 0.5763(3) 0.0750(7) Uani 1 1 d . . . N1 N 0.14167(16) 0.07242(19) 0.46786(18) 0.0285(3) Uani 1 1 d . . . N2 N 0.07013(18) 0.2023(2) 0.4258(2) 0.0381(4) Uani 1 1 d . . . N3 N 0.02075(18) 0.1946(2) 0.2789(2) 0.0367(4) Uani 1 1 d . . . N4 N 0.05986(16) 0.06131(19) 0.22312(18) 0.0273(3) Uani 1 1 d . . . C5 C 0.13509(19) -0.0123(2) 0.3415(2) 0.0288(4) Uani 1 1 d . . . H5 H 0.1764 -0.1068 0.3376 0.035 Uiso 1 1 calc R . . C6 C 0.2141(2) 0.0440(3) 0.6280(2) 0.0404(5) Uani 1 1 d . . . H6A H 0.2427 -0.0645 0.6391 0.048 Uiso 1 1 calc R . . H6B H 0.1609 0.0601 0.6954 0.048 Uiso 1 1 calc R . . C7 C 0.3248(2) 0.1517(3) 0.6753(3) 0.0492(6) Uani 1 1 d . . . H7A H 0.2973 0.2606 0.6669 0.059 Uiso 1 1 calc R . . H7B H 0.3718 0.1313 0.7815 0.059 Uiso 1 1 calc R . . C9 C 0.5083(3) 0.2223(8) 0.6091(6) 0.1111(19) Uani 1 1 d . . . H9A H 0.4825 0.3306 0.5971 0.167 Uiso 1 1 calc R . . H9B H 0.5566 0.1983 0.5389 0.167 Uiso 1 1 calc R . . H9C H 0.5584 0.2045 0.7132 0.167 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 Br1 0.03124(13) 0.04359(14) 0.02871(12) -0.00384(7) 0.00489(8) 0.00527(8) Cu1 0.03013(17) 0.02995(17) 0.01685(15) -0.00204(11) 0.00186(12) 0.00417(12) O8 0.0424(11) 0.112(2) 0.0681(15) -0.0089(13) 0.0107(10) -0.0086(12) N1 0.0319(8) 0.0327(8) 0.0184(7) -0.0008(6) 0.0031(6) -0.0033(6) N2 0.0437(10) 0.0385(9) 0.0285(8) -0.0098(7) 0.0039(7) 0.0051(8) N3 0.0445(10) 0.0311(8) 0.0289(8) -0.0072(7) 0.0013(7) 0.0073(7) N4 0.0315(8) 0.0268(7) 0.0220(7) -0.0028(6) 0.0050(6) 0.0011(6) C5 0.0324(9) 0.0289(9) 0.0219(8) -0.0021(7) 0.0025(7) 0.0017(7) C6 0.0494(13) 0.0469(12) 0.0193(8) 0.0025(8) 0.0007(8) -0.0050(10) C7 0.0486(13) 0.0577(15) 0.0300(10) -0.0055(10) -0.0073(10) -0.0024(11) C9 0.0445(18) 0.178(5) 0.097(3) 0.032(3) -0.0026(19) -0.031(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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu1 2.4335(15) . . ? Cu1 N4 2.004(2) . . ? O8 C7 1.405(4) . . ? O8 C9 1.430(6) . . ? N1 N2 1.350(3) . . ? N1 C5 1.333(2) . . ? N1 C6 1.463(3) . . ? N2 N3 1.286(3) . . ? N3 N4 1.358(3) . . ? N4 C5 1.315(3) . . ? C6 C7 1.496(4) . . ? C5 H5 0.9299 . . ? C6 H6A 0.9704 . . ? C6 H6B 0.9696 . . ? C7 H7A 0.9699 . . ? C7 H7B 0.9697 . . ? C9 H9A 0.9601 . . ? C9 H9B 0.9601 . . ? C9 H9C 0.9601 . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Cu1 N4 91.01(5) . . . ? Br1 Cu1 Br1 180.00 . . 3_555 ? Br1 Cu1 N4 88.99(5) . . 3_555 ? Br1 Cu1 N4 88.99(5) 3_555 . . ? N4 Cu1 N4 180.00 . . 3_555 ? Br1 Cu1 N4 91.01(5) 3_555 . 3_555 ? C7 O8 C9 112.5(3) . . . ? N2 N1 C5 108.28(15) . . . ? N2 N1 C6 121.99(17) . . . ? C5 N1 C6 129.70(18) . . . ? N1 N2 N3 107.19(16) . . . ? Cu1 N2 N1 149.00(13) 2_555 . . ? Cu1 N2 N3 103.11(12) 2_555 . . ? N2 N3 N4 109.62(17) . . . ? Cu1 N4 N3 122.55(13) . . . ? Cu1 N4 C5 130.46(13) . . . ? N3 N4 C5 106.95(15) . . . ? N1 C5 N4 107.95(16) . . . ? N1 C6 C7 111.20(19) . . . ? O8 C7 C6 107.5(2) . . . ? N1 C5 H5 126.07 . . . ? N4 C5 H5 125.97 . . . ? N1 C6 H6A 109.39 . . . ? N1 C6 H6B 109.43 . . . ? C7 C6 H6A 109.34 . . . ? C7 C6 H6B 109.43 . . . ? H6A C6 H6B 107.99 . . . ? O8 C7 H7A 110.22 . . . ? O8 C7 H7B 110.22 . . . ? C6 C7 H7A 110.14 . . . ? C6 C7 H7B 110.17 . . . ? H7A C7 H7B 108.55 . . . ? O8 C9 H9A 109.45 . . . ? O8 C9 H9B 109.42 . . . ? O8 C9 H9C 109.47 . . . ? H9A C9 H9B 109.48 . . . ? H9A C9 H9C 109.51 . . . ? H9B C9 H9C 109.50 . . . ? 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 Br1 Cu1 N4 N3 -38.66(16) . . . . ? Br1 Cu1 N4 C5 138.55(19) . . . . ? Br1 Cu1 N4 N3 141.34(16) 3_555 . . . ? Br1 Cu1 N4 C5 -41.45(19) 3_555 . . . ? C9 O8 C7 C6 178.9(3) . . . . ? C6 N1 C5 N4 -178.7(2) . . . . ? N2 N1 C6 C7 -72.5(3) . . . . ? C5 N1 C6 C7 105.1(3) . . . . ? C5 N1 N2 N3 0.8(2) . . . . ? C5 N1 N2 Cu1 -166.6(2) . . . 2_555 ? C6 N1 N2 N3 178.85(19) . . . . ? C6 N1 N2 Cu1 11.4(4) . . . 2_555 ? N2 N1 C5 N4 -0.9(2) . . . . ? Cu1 N2 N3 N4 172.88(13) 2_555 . . . ? N1 N2 N3 N4 -0.5(2) . . . . ? N2 N3 N4 Cu1 177.78(14) . . . . ? N2 N3 N4 C5 0.0(2) . . . . ? N3 N4 C5 N1 0.5(2) . . . . ? Cu1 N4 C5 N1 -177.01(14) . . . . ? N1 C6 C7 O8 -59.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.492 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.069 #===END ############################################################################## # End of the CIF # ##############################################################################