data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lars Ohrstrom' _publ_contact_author_address ; Department of Chemical and Biological Engineering Chalmers University of Technology Physcial Chemistry Gothenburg 41296 SWEDEN ; _publ_contact_author_email OHRSTROM@CHALMERS.SE _publ_section_title ; An unusual 3D-topology and dominant ferromagnetic couplings in two Cu(II)-azide coordination polymers ; loop_ _publ_author_name 'Lars Ohrstrom' 'Morsy A. M. Abu-Youssef' 'Albert Escuer' 'Franz A. Mautner' data_swe04a _database_code_depnum_ccdc_archive 'CCDC 670576' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common (Cu3(Methylpyrazine)2(N3)6)n _chemical_formula_moiety 'C10 H12 Cu3 N22' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H12 Cu3 N22' _chemical_formula_weight 631.07 _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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.862(3) _cell_length_b 18.299(7) _cell_length_c 13.333(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.10(7) _cell_angle_gamma 90.00 _cell_volume 2140.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 15.6 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method ? _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 3.007 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.644 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details DIFABS _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 \w-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 2 _diffrn_reflns_number 2796 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2320 _reflns_number_gt 2039 _reflns_threshold_expression >2sigmaI _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 3 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+3.9456P] 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 2317 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_all 0.0775 _refine_ls_wR_factor_ref 0.0714 _refine_ls_goodness_of_fit_all 1.113 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.124 _refine_ls_restrained_S_gt 1.104 _refine_ls_shift/su_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 Cu1 Cu 0.02568(4) 0.07110(2) 0.44163(3) 0.01139(11) Uani 1 d . . Cu2 Cu 0.0000 0.17768(2) 0.2500 0.00972(12) Uani 1 d S . N11 N -0.1094(3) 0.15792(13) 0.3986(2) 0.0125(5) Uani 1 d . . N12 N -0.2405(3) 0.16461(13) 0.4122(2) 0.0191(6) Uani 1 d . . N13 N -0.3656(3) 0.1732(2) 0.4221(3) 0.0411(9) Uani 1 d . . N21 N 0.1315(3) 0.09908(12) 0.3263(2) 0.0132(5) Uani 1 d . . N22 N 0.2130(3) 0.06021(15) 0.2827(2) 0.0252(6) Uani 1 d . . N23 N 0.2928(5) 0.0257(2) 0.2428(3) 0.0637(14) Uani 1 d . . N31 N -0.0939(3) 0.03436(13) 0.5482(2) 0.0137(5) Uani 1 d . . N32 N -0.1393(3) 0.07587(13) 0.6093(2) 0.0190(5) Uani 1 d . . N33 N -0.1847(4) 0.1156(2) 0.6638(3) 0.0351(8) Uani 1 d . . N1 N 0.1865(3) 0.14215(12) 0.5559(2) 0.0123(5) Uani 1 d . . C1 C 0.3386(3) 0.13343(15) 0.5783(2) 0.0122(6) Uani 1 d . . C2 C 0.4259(3) 0.18619(14) 0.6357(2) 0.0119(5) Uani 1 d . . H2 H 0.5312 0.18054 0.6475 0.014 Uiso 1 calc R . N2 N 0.3638(3) 0.24451(12) 0.6743(2) 0.0112(5) Uani 1 d . . C3 C 0.2114(3) 0.25193(15) 0.6542(2) 0.0132(6) Uani 1 d . . H3 H 0.1638 0.29124 0.6809 0.016 Uiso 1 calc R . C4 C 0.1252(3) 0.20111(15) 0.5937(2) 0.0130(6) Uani 1 d . . H4 H 0.0206 0.20834 0.5788 0.016 Uiso 1 calc R . C5 C 0.4111(3) 0.0671(2) 0.5404(2) 0.0179(6) Uani 1 d . . H5A H 0.5093 0.0596 0.5796 0.021 Uiso 1 calc R . H5B H 0.4227 0.0739 0.4705 0.021 Uiso 1 calc R . H5C H 0.3478 0.0253 0.5468 0.021 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 Cu1 0.0117(2) 0.0111(2) 0.0116(2) 0.00105(13) 0.00259(14) 0.00114(12) Cu2 0.0090(2) 0.0098(2) 0.0098(2) 0.000 -0.0008(2) 0.000 N11 0.0109(11) 0.0145(11) 0.0125(12) 0.0019(9) 0.0032(9) 0.0016(9) N12 0.0198(14) 0.0148(12) 0.0232(14) 0.0065(11) 0.0042(11) 0.0025(10) N13 0.0193(15) 0.035(2) 0.073(3) 0.014(2) 0.020(2) 0.0107(13) N21 0.0122(11) 0.0147(11) 0.0131(12) 0.0034(10) 0.0031(10) 0.0024(9) N22 0.032(2) 0.0230(13) 0.0234(15) 0.0118(12) 0.0146(13) 0.0119(12) N23 0.101(3) 0.046(2) 0.059(3) 0.031(2) 0.062(3) 0.050(2) N31 0.0159(12) 0.0127(10) 0.0137(12) 0.0013(10) 0.0065(10) 0.0010(9) N32 0.0197(13) 0.0169(12) 0.0219(14) -0.0019(11) 0.0086(11) -0.0049(10) N33 0.045(2) 0.029(2) 0.036(2) -0.0131(14) 0.023(2) -0.0070(14) N1 0.0118(11) 0.0129(11) 0.0118(12) 0.0005(9) 0.0002(10) -0.0003(9) C1 0.0110(13) 0.0146(12) 0.0109(13) 0.0011(11) 0.0013(11) 0.0009(10) C2 0.0096(12) 0.0134(12) 0.0118(14) -0.0006(11) -0.0012(11) 0.0010(10) N2 0.0109(11) 0.0129(10) 0.0098(12) 0.0003(9) 0.0010(9) -0.0001(9) C3 0.0123(13) 0.0141(13) 0.0133(14) 0.0004(11) 0.0022(12) 0.0026(10) C4 0.0085(12) 0.0157(12) 0.0139(14) 0.0004(11) -0.0012(11) 0.0012(10) C5 0.0125(14) 0.0184(14) 0.022(2) -0.0063(12) 0.0000(12) 0.0019(11) _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 Cu1 N21 1.978(3) . yes Cu1 N31 2.005(3) . yes Cu1 N31 2.021(2) 5_556 yes Cu1 N11 2.023(2) . yes Cu1 N1 2.331(3) . yes Cu2 N21 2.032(2) 2 yes Cu2 N21 2.032(2) . yes Cu2 N2 2.040(2) 7_556 yes Cu2 N2 2.040(2) 8_455 yes Cu2 N11 2.353(3) 2 yes Cu2 N11 2.353(3) . yes N11 N12 1.207(4) . yes N12 N13 1.145(4) . yes N21 N22 1.218(4) . yes N22 N23 1.135(4) . yes N31 N32 1.222(4) . yes N31 Cu1 2.021(2) 5_556 ? N32 N33 1.141(4) . yes N1 C4 1.338(4) . ? N1 C1 1.348(4) . ? C1 C2 1.396(4) . ? C1 C5 1.493(4) . ? C2 N2 1.337(4) . ? C2 H2 0.93 . ? N2 C3 1.346(4) . ? C3 C4 1.387(4) . ? C3 H3 0.93 . ? C4 H4 0.93 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 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 N21 Cu1 N31 173.60(10) . . yes N21 Cu1 N31 97.42(10) . 5_556 yes N31 Cu1 N31 79.36(11) . 5_556 yes N21 Cu1 N11 84.42(10) . . yes N31 Cu1 N11 96.51(10) . . yes N31 Cu1 N11 158.19(10) 5_556 . yes N21 Cu1 N1 92.90(10) . . yes N31 Cu1 N1 93.40(10) . . yes N31 Cu1 N1 109.82(10) 5_556 . yes N11 Cu1 N1 91.73(10) . . yes N21 Cu2 N21 89.87(14) 2 . yes N21 Cu2 N2 178.73(10) 2 7_556 yes N21 Cu2 N2 89.34(10) . 7_556 yes N21 Cu2 N2 89.34(10) 2 8_455 yes N21 Cu2 N2 178.73(10) . 8_455 yes N2 Cu2 N2 91.47(14) 7_556 8_455 yes N21 Cu2 N11 75.22(9) 2 2 yes N21 Cu2 N11 92.15(9) . 2 yes N2 Cu2 N11 103.82(9) 7_556 2 yes N2 Cu2 N11 88.61(9) 8_455 2 yes N21 Cu2 N11 92.15(9) 2 . yes N21 Cu2 N11 75.22(9) . . yes N2 Cu2 N11 88.61(9) 7_556 . yes N2 Cu2 N11 103.82(9) 8_455 . yes N11 Cu2 N11 162.32(11) 2 . yes N12 N11 Cu1 125.5(2) . . yes N12 N11 Cu2 129.1(2) . . yes Cu1 N11 Cu2 93.55(10) . . yes N13 N12 N11 177.1(3) . . yes N22 N21 Cu1 126.7(2) . . yes N22 N21 Cu2 120.8(2) . . yes Cu1 N21 Cu2 105.72(11) . . yes N23 N22 N21 177.7(4) . . yes N32 N31 Cu1 121.3(2) . . yes N32 N31 Cu1 132.2(2) . 5_556 yes Cu1 N31 Cu1 100.64(11) . 5_556 yes N33 N32 N31 177.8(4) . . yes C4 N1 C1 117.3(2) . . ? C4 N1 Cu1 116.9(2) . . ? C1 N1 Cu1 125.4(2) . . ? N1 C1 C2 119.9(3) . . ? N1 C1 C5 119.1(2) . . ? C2 C1 C5 121.0(3) . . ? N2 C2 C1 122.4(3) . . ? N2 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C2 N2 C3 117.4(2) . . ? C2 N2 Cu2 120.0(2) . 7_556 ? C3 N2 Cu2 122.4(2) . 7_556 ? N2 C3 C4 120.2(3) . . ? N2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? N1 C4 C3 122.7(3) . . ? N1 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 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 Cu1 N11 N12 152.5(3) . . . . ? N31 Cu1 N11 N12 -21.1(3) . . . . ? N31 Cu1 N11 N12 56.5(4) 5_556 . . . ? N1 Cu1 N11 N12 -114.7(3) . . . . ? N31 Cu1 N11 Cu2 -88.6(3) 5_556 . . . ? N21 Cu2 N11 N12 -61.3(3) 2 . . . ? N21 Cu2 N11 N12 -150.6(3) . . . . ? N2 Cu2 N11 N12 119.7(3) 7_556 . . . ? N2 Cu2 N11 N12 28.6(3) 8_455 . . . ? N11 Cu2 N11 N12 -105.0(2) 2 . . . ? N11 Cu2 N11 Cu1 38.1(4) 2 . . . ? N31 Cu1 N21 N22 -1.6(3) 5_556 . . . ? N11 Cu1 N21 N22 -159.7(3) . . . . ? N21 Cu2 N21 N22 68.5(2) 2 . . . ? N2 Cu2 N21 N22 -110.5(3) 7_556 . . . ? N11 Cu2 N21 N22 -6.7(2) 2 . . . ? N11 Cu2 N21 N22 160.8(3) . . . . ? N31 Cu1 N31 N32 156.2(3) 5_556 . . . ? N11 Cu1 N31 N32 -45.5(2) . . . . ? N1 Cu1 N31 N32 46.7(2) . . . . ? N21 Cu1 N1 C4 111.3(2) . . . . ? N31 Cu1 N1 C4 -69.9(2) . . . . ? N31 Cu1 N1 C4 -149.8(2) 5_556 . . . ? N11 Cu1 N1 C4 26.8(2) . . . . ? N21 Cu1 N1 C1 -60.9(2) . . . . ? N31 Cu1 N1 C1 117.9(2) . . . . ? N31 Cu1 N1 C1 38.0(2) 5_556 . . . ? N11 Cu1 N1 C1 -145.4(2) . . . . ? C4 N1 C1 C2 -2.2(4) . . . . ? Cu1 N1 C1 C2 170.0(2) . . . . ? C4 N1 C1 C5 178.1(3) . . . . ? Cu1 N1 C1 C5 -9.8(4) . . . . ? N1 C1 C2 N2 3.2(4) . . . . ? C5 C1 C2 N2 -177.1(3) . . . . ? C1 C2 N2 C3 -1.3(4) . . . . ? C1 C2 N2 Cu2 -176.3(2) . . . 7_556 ? C2 N2 C3 C4 -1.4(4) . . . . ? Cu2 N2 C3 C4 173.5(2) 7_556 . . . ? C1 N1 C4 C3 -0.5(4) . . . . ? Cu1 N1 C4 C3 -173.3(2) . . . . ? N2 C3 C4 N1 2.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.99 _refine_diff_density_max 0.515 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.090 data_gcu05a _database_code_depnum_ccdc_archive 'CCDC 670577' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common (Cu(4-Brpy)(N3)2)n _chemical_formula_moiety 'C10 H8 Br2 Cu2 N14' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H8 Br2 Cu2 N14' _chemical_formula_weight 611.20 _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' Cu Cu 0.3201 1.2651 '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 Monoclinic _symmetry_space_group_name_H-M I2/a _symmetry_space_group_name_Hall '-I 2ya' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.925(4) _cell_length_b 9.367(2) _cell_length_c 24.765(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.39(3) _cell_angle_gamma 90.00 _cell_volume 3683.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 5.6 _cell_measurement_theta_max 15.1 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.204 _exptl_crystal_density_method ? _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 6.680 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.193 _exptl_absorpt_correction_T_max 0.669 _exptl_absorpt_process_details DIFABS _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 \w-scans _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 3 _diffrn_reflns_number 4344 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3632 _reflns_number_gt 2980 _reflns_threshold_expression >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 5 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+24.9325P] 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 3627 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_all 0.1283 _refine_ls_wR_factor_ref 0.1134 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.093 _refine_ls_restrained_S_ref 1.072 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.80349(4) 0.05920(8) 0.27680(3) 0.0148(2) Uani 1 d . . Cu2 Cu 0.97992(4) 0.12790(7) 0.23651(3) 0.0133(2) Uani 1 d . . N11 N 0.9214(3) 0.1208(6) 0.3054(2) 0.0187(11) Uani 1 d . . N12 N 0.9538(3) 0.1102(5) 0.3507(2) 0.0143(10) Uani 1 d . . N13 N 0.9836(3) 0.1015(7) 0.3941(2) 0.0304(13) Uani 1 d . . N21 N 0.8645(3) 0.0615(5) 0.2093(2) 0.0178(10) Uani 1 d . . N22 N 0.8407(3) 0.0009(5) 0.1676(2) 0.0151(10) Uani 1 d . . N23 N 0.8167(4) -0.0554(6) 0.1283(2) 0.0285(13) Uani 1 d . . N31 N 0.8210(3) -0.1771(6) 0.2828(2) 0.0214(11) Uani 1 d . . N32 N 0.8667(3) -0.2374(5) 0.2559(2) 0.0156(10) Uani 1 d . . N33 N 0.9127(3) -0.3001(5) 0.2280(2) 0.0168(10) Uani 1 d . . N41 N 0.6944(3) 0.0919(6) 0.2356(2) 0.0194(11) Uani 1 d . . N42 N 0.6290(3) 0.1063(5) 0.2559(2) 0.0157(10) Uani 1 d . . N43 N 0.5636(3) 0.1204(5) 0.2730(2) 0.0176(10) Uani 1 d . . N1 N 1.0225(3) 0.1109(5) 0.1635(2) 0.0150(10) Uani 1 d . . C1 C 1.0367(4) 0.2287(7) 0.1339(3) 0.0214(13) Uani 1 d . . H1 H 1.0244 0.3175 0.1482 0.026 Uiso 1 calc R . C2 C 1.0684(4) 0.2239(7) 0.0838(3) 0.0231(13) Uani 1 d . . H2 H 1.0774 0.3070 0.0646 0.028 Uiso 1 calc R . C3 C 1.0866(4) 0.0895(7) 0.0629(3) 0.0248(14) Uani 1 d . . C4 C 1.0710(4) -0.0335(8) 0.0921(3) 0.0281(15) Uani 1 d . . H4 H 1.0815 -0.1236 0.0784 0.034 Uiso 1 calc R . C5 C 1.0392(4) -0.0172(7) 0.1424(2) 0.0186(12) Uani 1 d . . H5 H 1.0289 -0.0986 0.1623 0.022 Uiso 1 calc R . Br1 Br 1.12705(5) 0.07834(9) -0.00640(3) 0.0380(2) Uani 1 d . . N2 N 0.7542(3) 0.0683(6) 0.3483(2) 0.0191(11) Uani 1 d . . C6 C 0.7223(4) -0.0485(7) 0.3710(3) 0.0248(14) Uani 1 d . . H6 H 0.7302 -0.1367 0.3549 0.030 Uiso 1 calc R . C7 C 0.6784(4) -0.0434(8) 0.4170(3) 0.0254(14) Uani 1 d . . H7 H 0.6571 -0.1258 0.4317 0.030 Uiso 1 calc R . C8 C 0.6676(4) 0.0879(8) 0.4400(2) 0.0242(14) Uani 1 d . . C9 C 0.7000(4) 0.2103(7) 0.4180(3) 0.0240(14) Uani 1 d . . H9 H 0.6931 0.2993 0.4337 0.029 Uiso 1 calc R . C10 C 0.7431(4) 0.1955(7) 0.3715(3) 0.0251(14) Uani 1 d . . H10 H 0.7649 0.2765 0.3560 0.030 Uiso 1 calc R . Br2 Br 0.60647(4) 0.10354(8) 0.50226(3) 0.0279(2) 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 Cu1 0.0112(3) 0.0148(4) 0.0181(4) -0.0014(3) -0.0010(3) 0.0005(3) Cu2 0.0127(3) 0.0091(4) 0.0179(4) -0.0009(3) -0.0006(3) -0.0021(3) N11 0.014(2) 0.016(3) 0.026(3) -0.004(2) -0.001(2) -0.005(2) N12 0.015(2) 0.010(2) 0.018(2) 0.000(2) 0.000(2) 0.001(2) N13 0.027(3) 0.041(4) 0.023(3) 0.005(3) 0.001(2) 0.002(3) N21 0.018(2) 0.014(3) 0.022(3) -0.005(2) 0.003(2) 0.000(2) N22 0.015(2) 0.010(2) 0.021(2) 0.002(2) 0.000(2) 0.000(2) N23 0.033(3) 0.025(3) 0.026(3) -0.005(3) -0.003(2) -0.003(2) N31 0.020(2) 0.014(3) 0.031(3) 0.003(2) 0.004(2) 0.004(2) N32 0.014(2) 0.008(2) 0.024(2) 0.001(2) -0.005(2) -0.002(2) N33 0.018(2) 0.009(2) 0.022(2) -0.001(2) -0.002(2) 0.002(2) N41 0.016(2) 0.022(3) 0.021(3) 0.001(2) 0.002(2) 0.000(2) N42 0.020(2) 0.007(2) 0.019(2) 0.001(2) -0.004(2) 0.000(2) N43 0.015(2) 0.009(2) 0.028(3) -0.001(2) 0.001(2) 0.004(2) N1 0.013(2) 0.012(2) 0.020(2) -0.003(2) -0.001(2) -0.003(2) C1 0.025(3) 0.013(3) 0.027(3) 0.003(2) 0.004(2) -0.003(2) C2 0.026(3) 0.017(3) 0.025(3) 0.008(3) -0.003(3) -0.006(3) C3 0.025(3) 0.027(4) 0.023(3) -0.003(3) 0.006(3) -0.001(3) C4 0.026(3) 0.030(4) 0.028(3) -0.003(3) 0.000(3) 0.006(3) C5 0.022(3) 0.010(3) 0.023(3) -0.002(2) -0.003(2) 0.005(2) Br1 0.0437(4) 0.0431(5) 0.0283(4) -0.0014(3) 0.0106(3) 0.0011(3) N2 0.014(2) 0.020(3) 0.023(3) -0.006(2) -0.001(2) 0.000(2) C6 0.021(3) 0.024(4) 0.029(3) -0.006(3) 0.000(3) -0.004(3) C7 0.019(3) 0.031(4) 0.026(3) 0.003(3) 0.000(2) -0.006(3) C8 0.017(3) 0.037(4) 0.019(3) -0.003(3) 0.002(2) 0.002(3) C9 0.024(3) 0.023(4) 0.024(3) -0.001(3) 0.000(2) 0.008(3) C10 0.025(3) 0.021(4) 0.029(3) 0.004(3) 0.001(3) 0.002(3) Br2 0.0266(3) 0.0335(4) 0.0238(3) -0.0022(3) 0.0034(3) -0.0018(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 Cu1 N41 1.970(5) . yes Cu1 N2 1.993(5) . yes Cu1 N21 1.996(5) . yes Cu1 N11 2.039(5) . yes Cu1 N31 2.235(5) . yes Cu2 N33 1.980(5) 4_655 yes Cu2 N1 1.986(5) . yes Cu2 N11 2.005(5) . yes Cu2 N21 2.007(5) . yes Cu2 N43 2.464(5) 7_655 yes N11 N12 1.203(7) . yes N12 N13 1.144(7) . yes N21 N22 1.214(7) . yes N22 N23 1.146(7) . yes N31 N32 1.168(7) . yes N32 N33 1.198(6) . yes N33 Cu2 1.980(5) 4_645 ? N41 N42 1.199(6) . yes N42 N43 1.161(6) . yes N43 Cu2 2.464(5) 7_655 ? N1 C5 1.344(7) . ? N1 C1 1.353(8) . ? C1 C2 1.375(8) . ? C1 H1 0.93 . ? C2 C3 1.401(9) . ? C2 H2 0.93 . ? C3 C4 1.394(10) . ? C3 Br1 1.881(6) . ? C4 C5 1.387(9) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? N2 C10 1.339(8) . ? N2 C6 1.347(8) . ? C6 C7 1.382(9) . ? C6 H6 0.93 . ? C7 C8 1.372(9) . ? C7 H7 0.93 . ? C8 C9 1.387(9) . ? C8 Br2 1.890(6) . ? C9 C10 1.393(9) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? 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 N41 Cu1 N2 93.5(2) . . yes N41 Cu1 N21 91.8(2) . . yes N2 Cu1 N21 173.3(2) . . yes N41 Cu1 N11 152.6(2) . . yes N2 Cu1 N11 95.4(2) . . yes N21 Cu1 N11 78.0(2) . . yes N41 Cu1 N31 106.8(2) . . yes N2 Cu1 N31 92.3(2) . . yes N21 Cu1 N31 90.0(2) . . yes N11 Cu1 N31 98.6(2) . . yes N33 Cu2 N1 95.1(2) 4_655 . yes N33 Cu2 N11 94.3(2) 4_655 . yes N1 Cu2 N11 170.0(2) . . yes N33 Cu2 N21 172.7(2) 4_655 . yes N1 Cu2 N21 92.2(2) . . yes N11 Cu2 N21 78.6(2) . . yes N33 Cu2 N43 86.8(2) 4_655 7_655 yes N1 Cu2 N43 95.9(2) . 7_655 yes N11 Cu2 N43 88.1(2) . 7_655 yes N21 Cu2 N43 91.2(2) . 7_655 yes N12 N11 Cu2 127.0(4) . . yes N12 N11 Cu1 128.2(4) . . yes Cu2 N11 Cu1 101.0(2) . . yes N13 N12 N11 178.9(6) . . yes N22 N21 Cu1 124.5(4) . . yes N22 N21 Cu2 130.5(4) . . yes Cu1 N21 Cu2 102.4(2) . . yes N23 N22 N21 178.7(6) . . yes N32 N31 Cu1 121.4(4) . . yes N31 N32 N33 179.1(6) . . yes N32 N33 Cu2 117.1(4) . 4_645 yes N42 N41 Cu1 124.1(4) . . yes N43 N42 N41 176.6(6) . . yes N42 N43 Cu2 109.1(4) . 7_655 yes C5 N1 C1 118.1(5) . . ? C5 N1 Cu2 121.1(4) . . ? C1 N1 Cu2 120.7(4) . . ? N1 C1 C2 123.3(6) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 117.7(6) . . ? C1 C2 H2 121.2 . . ? C3 C2 H2 121.2 . . ? C4 C3 C2 120.0(5) . . ? C4 C3 Br1 121.0(5) . . ? C2 C3 Br1 118.9(5) . . ? C5 C4 C3 117.9(6) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? N1 C5 C4 122.9(6) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C10 N2 C6 118.5(5) . . ? C10 N2 Cu1 119.5(4) . . ? C6 N2 Cu1 121.5(4) . . ? N2 C6 C7 123.1(6) . . ? N2 C6 H6 118.4 . . ? C7 C6 H6 118.4 . . ? C8 C7 C6 117.5(6) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 C9 121.0(5) . . ? C7 C8 Br2 119.9(5) . . ? C9 C8 Br2 119.2(5) . . ? C8 C9 C10 117.7(6) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N2 C10 C9 122.2(6) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? 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 N33 Cu2 N11 N12 -24.3(5) 4_655 . . . ? N21 Cu2 N11 N12 157.5(6) . . . . ? N43 Cu2 N11 N12 -110.9(5) 7_655 . . . ? N33 Cu2 N11 Cu1 176.5(2) 4_655 . . . ? N21 Cu2 N11 Cu1 -1.7(2) . . . . ? N43 Cu2 N11 Cu1 89.9(2) 7_655 . . . ? N41 Cu1 N11 N12 132.7(5) . . . . ? N2 Cu1 N11 N12 24.1(5) . . . . ? N21 Cu1 N11 N12 -157.1(6) . . . . ? N31 Cu1 N11 N12 -69.0(5) . . . . ? N41 Cu1 N11 Cu2 -68.5(5) . . . . ? N2 Cu1 N11 Cu2 -177.1(2) . . . . ? N21 Cu1 N11 Cu2 1.7(2) . . . . ? N31 Cu1 N11 Cu2 89.8(2) . . . . ? N41 Cu1 N21 N22 -44.0(5) . . . . ? N11 Cu1 N21 N22 161.6(5) . . . . ? N31 Cu1 N21 N22 62.8(5) . . . . ? N41 Cu1 N21 Cu2 152.7(2) . . . . ? N11 Cu1 N21 Cu2 -1.7(2) . . . . ? N31 Cu1 N21 Cu2 -100.5(2) . . . . ? N1 Cu2 N21 N22 16.1(6) . . . . ? N11 Cu2 N21 N22 -160.1(6) . . . . ? N43 Cu2 N21 N22 112.0(6) 7_655 . . . ? N1 Cu2 N21 Cu1 177.9(2) . . . . ? N11 Cu2 N21 Cu1 1.7(2) . . . . ? N43 Cu2 N21 Cu1 -86.2(2) 7_655 . . . ? N41 Cu1 N31 N32 103.6(5) . . . . ? N2 Cu1 N31 N32 -162.0(5) . . . . ? N21 Cu1 N31 N32 11.8(5) . . . . ? N11 Cu1 N31 N32 -66.1(5) . . . . ? N2 Cu1 N41 N42 -1.2(5) . . . . ? N21 Cu1 N41 N42 -177.3(5) . . . . ? N11 Cu1 N41 N42 -110.2(6) . . . . ? N31 Cu1 N41 N42 92.2(5) . . . . ? N33 Cu2 N1 C5 106.5(4) 4_655 . . . ? N21 Cu2 N1 C5 -74.8(4) . . . . ? N43 Cu2 N1 C5 -166.2(4) 7_655 . . . ? N33 Cu2 N1 C1 -72.5(5) 4_655 . . . ? N21 Cu2 N1 C1 106.1(4) . . . . ? N43 Cu2 N1 C1 14.7(4) 7_655 . . . ? C5 N1 C1 C2 -1.0(9) . . . . ? Cu2 N1 C1 C2 178.1(5) . . . . ? N1 C1 C2 C3 0.0(9) . . . . ? C1 C2 C3 C4 1.2(9) . . . . ? C1 C2 C3 Br1 178.3(5) . . . . ? C2 C3 C4 C5 -1.4(9) . . . . ? Br1 C3 C4 C5 -178.4(5) . . . . ? C1 N1 C5 C4 0.7(8) . . . . ? Cu2 N1 C5 C4 -178.3(4) . . . . ? C3 C4 C5 N1 0.5(9) . . . . ? N41 Cu1 N2 C10 -84.2(5) . . . . ? N11 Cu1 N2 C10 69.9(5) . . . . ? N31 Cu1 N2 C10 168.8(5) . . . . ? N41 Cu1 N2 C6 87.6(5) . . . . ? N11 Cu1 N2 C6 -118.3(5) . . . . ? N31 Cu1 N2 C6 -19.4(5) . . . . ? C10 N2 C6 C7 0.1(9) . . . . ? Cu1 N2 C6 C7 -171.7(5) . . . . ? N2 C6 C7 C8 0.0(10) . . . . ? C6 C7 C8 C9 -0.3(9) . . . . ? C6 C7 C8 Br2 178.8(5) . . . . ? C7 C8 C9 C10 0.5(9) . . . . ? Br2 C8 C9 C10 -178.6(5) . . . . ? C6 N2 C10 C9 0.1(9) . . . . ? Cu1 N2 C10 C9 172.1(5) . . . . ? C8 C9 C10 N2 -0.4(9) . . . . ? _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.00 _refine_diff_density_max 0.645 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.160