Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_ind46fnl _database_code_CSD 159343 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chaudhuri, Nirmalendu Ray' 'Cheng, Jack' 'Das, Debasis' 'El Fallah, Mohamed S.' 'Kumar Maji, Tapas' 'Lu, Tian-Huey' 'Ribas, Joan' 'Sain, Saugata' _publ_contact_author_name 'Prof Nirmalendu Ray Chaudhuri' _publ_contact_author_address ; Department of Chemistry Indian Association for the Cultivation of Science Jadavpur Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICNRC@MAHENDRA.IACS.RES.IN' _publ_section_title ; Exchange interactions in an one dimensional bromo-bridged copper(II) compound having a ladder-like structure ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 Br4 Cu2 N4' _chemical_formula_weight 647.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8176(16) _cell_length_b 11.4131(13) _cell_length_c 13.3206(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.157(2) _cell_angle_gamma 90.00 _cell_volume 1901.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour blue _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 10.638 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.500 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details 'SAINT Ver5 (Sheldrick, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11954 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4573 _reflns_number_gt 3234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for windows(Farrugia,1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0467P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4573 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.34954(4) 0.11771(5) 0.28767(4) 0.03122(14) Uani 1 1 d . . . Cu2 Cu 0.16746(4) -0.12642(5) 0.19012(4) 0.03090(14) Uani 1 1 d . . . Br1 Br 0.21047(4) 0.07684(4) 0.09964(4) 0.03950(14) Uani 1 1 d . . . Br2 Br 0.32568(4) -0.10252(4) 0.36266(4) 0.04614(15) Uani 1 1 d . . . Br3 Br 0.49985(4) 0.08396(5) 0.24721(5) 0.05061(16) Uani 1 1 d . . . Br4 Br 0.04285(4) -0.04560(5) 0.25412(4) 0.04388(15) Uani 1 1 d . . . N1 N 0.4388(3) 0.1945(3) 0.4338(3) 0.0390(9) Uani 1 1 d . . . H1 H 0.5054 0.1623 0.4626 0.047 Uiso 1 1 calc R . . N2 N 0.2397(3) 0.1980(4) 0.3258(3) 0.0463(11) Uani 1 1 d . . . H2 H 0.1736 0.1695 0.2820 0.056 Uiso 1 1 calc R . . N3 N 0.0513(4) -0.1884(4) 0.0493(3) 0.0468(11) Uani 1 1 d . . . H3 H -0.0060 -0.1393 0.0261 0.056 Uiso 1 1 calc R . . N4 N 0.2432(3) -0.2451(4) 0.1393(4) 0.0472(11) Uani 1 1 d . . . H4 H 0.3151 -0.2356 0.1772 0.057 Uiso 1 1 calc R . . C1 C 0.3880(5) 0.1711(5) 0.5101(4) 0.0541(15) Uani 1 1 d . . . H1A H 0.4088 0.2308 0.5672 0.065 Uiso 1 1 calc R . . H1B H 0.4111 0.0956 0.5457 0.065 Uiso 1 1 calc R . . C2 C 0.2660(5) 0.1717(5) 0.4426(4) 0.0529(14) Uani 1 1 d . . . H2A H 0.2369 0.0958 0.4481 0.063 Uiso 1 1 calc R . . H2B H 0.2343 0.2303 0.4722 0.063 Uiso 1 1 calc R . . C3 C 0.4474(5) 0.3217(5) 0.4153(5) 0.0524(14) Uani 1 1 d . . . H3A H 0.4692 0.3320 0.3556 0.063 Uiso 1 1 calc R . . H3B H 0.5020 0.3561 0.4819 0.063 Uiso 1 1 calc R . . C4 C 0.3437(6) 0.3843(5) 0.3865(5) 0.0654(18) Uani 1 1 d . . . H4A H 0.3488 0.4612 0.3582 0.078 Uiso 1 1 calc R . . H4B H 0.3349 0.3959 0.4543 0.078 Uiso 1 1 calc R . . C5 C 0.2442(5) 0.3254(5) 0.3031(5) 0.0646(17) Uani 1 1 d . . . H5A H 0.1819 0.3639 0.3038 0.078 Uiso 1 1 calc R . . H5B H 0.2415 0.3348 0.2296 0.078 Uiso 1 1 calc R . . C6 C 0.0964(6) -0.1897(5) -0.0337(5) 0.069(2) Uani 1 1 d . . . H6A H 0.0892 -0.1127 -0.0669 0.083 Uiso 1 1 calc R . . H6B H 0.0572 -0.2452 -0.0921 0.083 Uiso 1 1 calc R . . C7 C 0.2110(6) -0.2234(6) 0.0202(5) 0.074(2) Uani 1 1 d . . . H7A H 0.2223 -0.2935 -0.0145 0.088 Uiso 1 1 calc R . . H7B H 0.2543 -0.1610 0.0111 0.088 Uiso 1 1 calc R . . C8 C 0.0196(4) -0.3056(5) 0.0728(5) 0.0512(14) Uani 1 1 d . . . H8A H 0.0076 -0.3012 0.1393 0.061 Uiso 1 1 calc R . . H8B H -0.0471 -0.3285 0.0119 0.061 Uiso 1 1 calc R . . C9 C 0.1014(5) -0.3958(4) 0.0882(5) 0.0558(15) Uani 1 1 d . . . H9A H 0.0830 -0.4661 0.1171 0.067 Uiso 1 1 calc R . . H9B H 0.0989 -0.4150 0.0162 0.067 Uiso 1 1 calc R . . C10 C 0.2122(5) -0.3626(4) 0.1629(5) 0.0577(16) Uani 1 1 d . . . H10A H 0.2607 -0.4204 0.1566 0.069 Uiso 1 1 calc R . . H10B H 0.2200 -0.3641 0.2388 0.069 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 Cu1 0.0262(3) 0.0381(3) 0.0302(3) -0.0006(2) 0.0128(2) 0.0017(2) Cu2 0.0288(3) 0.0352(3) 0.0302(3) -0.0022(2) 0.0139(2) -0.0001(2) Br1 0.0385(3) 0.0467(3) 0.0296(2) 0.0066(2) 0.0110(2) -0.0065(2) Br2 0.0385(3) 0.0510(3) 0.0381(3) 0.0104(2) 0.0059(2) -0.0040(2) Br3 0.0380(3) 0.0678(4) 0.0554(3) 0.0042(3) 0.0289(3) 0.0083(2) Br4 0.0401(3) 0.0539(3) 0.0470(3) -0.0012(2) 0.0275(2) 0.0047(2) N1 0.030(2) 0.044(2) 0.039(2) -0.0015(18) 0.0107(18) 0.0001(18) N2 0.028(2) 0.065(3) 0.046(2) -0.015(2) 0.0151(19) 0.002(2) N3 0.045(3) 0.039(2) 0.041(2) -0.0083(19) 0.004(2) 0.0098(19) N4 0.030(2) 0.054(3) 0.063(3) -0.013(2) 0.025(2) -0.0049(19) C1 0.078(4) 0.050(3) 0.043(3) -0.008(3) 0.034(3) -0.010(3) C2 0.061(4) 0.060(4) 0.057(3) -0.015(3) 0.044(3) -0.011(3) C3 0.058(4) 0.044(3) 0.057(3) -0.002(3) 0.026(3) -0.011(3) C4 0.087(5) 0.043(3) 0.078(4) 0.006(3) 0.046(4) 0.011(3) C5 0.061(4) 0.062(4) 0.065(4) 0.004(3) 0.021(3) 0.036(3) C6 0.119(7) 0.046(3) 0.037(3) -0.006(3) 0.028(4) 0.000(4) C7 0.113(6) 0.064(4) 0.082(5) -0.020(3) 0.078(5) -0.009(4) C8 0.035(3) 0.049(3) 0.063(4) -0.014(3) 0.014(3) -0.008(2) C9 0.056(4) 0.039(3) 0.071(4) 0.007(3) 0.026(3) -0.002(3) C10 0.055(4) 0.038(3) 0.072(4) -0.001(3) 0.019(3) 0.014(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 N1 2.009(4) . ? Cu1 N2 2.014(4) . ? Cu1 Br3 2.3883(7) . ? Cu1 Br1 2.4682(7) . ? Cu1 Br2 2.7756(8) . ? Cu2 N4 1.998(4) . ? Cu2 N3 2.009(4) . ? Cu2 Br4 2.4062(7) . ? Cu2 Br2 2.4216(8) . ? Cu2 Br1 2.7923(7) . ? N1 C1 1.484(6) . ? N1 C3 1.486(6) . ? N2 C2 1.470(6) . ? N2 C5 1.492(7) . ? N3 C8 1.482(7) . ? N3 C6 1.482(7) . ? N4 C7 1.475(7) . ? N4 C10 1.482(7) . ? C1 C2 1.537(8) . ? C3 C4 1.497(8) . ? C4 C5 1.509(9) . ? C6 C7 1.484(9) . ? C8 C9 1.477(7) . ? C9 C10 1.477(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 77.00(17) . . ? N1 Cu1 Br3 93.13(12) . . ? N2 Cu1 Br3 162.00(13) . . ? N1 Cu1 Br1 163.35(12) . . ? N2 Cu1 Br1 89.82(12) . . ? Br3 Cu1 Br1 96.72(3) . . ? N1 Cu1 Br2 99.44(11) . . ? N2 Cu1 Br2 95.96(13) . . ? Br3 Cu1 Br2 100.54(3) . . ? Br1 Cu1 Br2 91.93(2) . . ? N4 Cu2 N3 76.71(18) . . ? N4 Cu2 Br4 159.54(12) . . ? N3 Cu2 Br4 93.33(13) . . ? N4 Cu2 Br2 90.37(13) . . ? N3 Cu2 Br2 165.12(12) . . ? Br4 Cu2 Br2 96.54(3) . . ? N4 Cu2 Br1 100.28(13) . . ? N3 Cu2 Br1 96.98(13) . . ? Br4 Cu2 Br1 98.63(2) . . ? Br2 Cu2 Br1 92.53(2) . . ? Cu1 Br1 Cu2 86.31(2) . . ? Cu2 Br2 Cu1 87.59(2) . . ? C1 N1 C3 112.6(4) . . ? C1 N1 Cu1 108.1(3) . . ? C3 N1 Cu1 108.9(3) . . ? C2 N2 C5 113.6(4) . . ? C2 N2 Cu1 107.5(3) . . ? C5 N2 Cu1 107.0(3) . . ? C8 N3 C6 113.8(4) . . ? C8 N3 Cu2 108.1(3) . . ? C6 N3 Cu2 106.1(4) . . ? C7 N4 C10 113.5(4) . . ? C7 N4 Cu2 106.8(3) . . ? C10 N4 Cu2 107.5(3) . . ? N1 C1 C2 108.6(4) . . ? N2 C2 C1 109.6(4) . . ? N1 C3 C4 111.9(5) . . ? C3 C4 C5 116.7(5) . . ? N2 C5 C4 112.8(4) . . ? N3 C6 C7 110.0(5) . . ? N4 C7 C6 109.6(5) . . ? C9 C8 N3 112.4(4) . . ? C10 C9 C8 115.3(5) . . ? C9 C10 N4 113.5(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 N1 Cu1 Br1 Cu2 -124.3(4) . . . . ? N2 Cu1 Br1 Cu2 -86.99(13) . . . . ? Br3 Cu1 Br1 Cu2 109.82(3) . . . . ? Br2 Cu1 Br1 Cu2 8.97(2) . . . . ? N4 Cu2 Br1 Cu1 -101.13(13) . . . . ? N3 Cu2 Br1 Cu1 -178.83(13) . . . . ? Br4 Cu2 Br1 Cu1 86.71(3) . . . . ? Br2 Cu2 Br1 Cu1 -10.30(2) . . . . ? N4 Cu2 Br2 Cu1 109.44(12) . . . . ? N3 Cu2 Br2 Cu1 138.9(5) . . . . ? Br4 Cu2 Br2 Cu1 -89.86(3) . . . . ? Br1 Cu2 Br2 Cu1 9.13(2) . . . . ? N1 Cu1 Br2 Cu2 157.45(12) . . . . ? N2 Cu1 Br2 Cu2 79.68(12) . . . . ? Br3 Cu1 Br2 Cu2 -107.55(3) . . . . ? Br1 Cu1 Br2 Cu2 -10.34(2) . . . . ? N2 Cu1 N1 C1 45.7(3) . . . . ? Br3 Cu1 N1 C1 -149.6(3) . . . . ? Br1 Cu1 N1 C1 84.1(5) . . . . ? Br2 Cu1 N1 C1 -48.3(3) . . . . ? N2 Cu1 N1 C3 -77.0(3) . . . . ? Br3 Cu1 N1 C3 87.8(3) . . . . ? Br1 Cu1 N1 C3 -38.5(6) . . . . ? Br2 Cu1 N1 C3 -170.9(3) . . . . ? N1 Cu1 N2 C2 -46.3(3) . . . . ? Br3 Cu1 N2 C2 -104.3(5) . . . . ? Br1 Cu1 N2 C2 144.0(3) . . . . ? Br2 Cu1 N2 C2 52.1(3) . . . . ? N1 Cu1 N2 C5 76.1(3) . . . . ? Br3 Cu1 N2 C5 18.1(6) . . . . ? Br1 Cu1 N2 C5 -93.6(3) . . . . ? Br2 Cu1 N2 C5 174.4(3) . . . . ? N4 Cu2 N3 C8 76.0(3) . . . . ? Br4 Cu2 N3 C8 -85.9(3) . . . . ? Br2 Cu2 N3 C8 45.6(7) . . . . ? Br1 Cu2 N3 C8 174.9(3) . . . . ? N4 Cu2 N3 C6 -46.5(3) . . . . ? Br4 Cu2 N3 C6 151.5(3) . . . . ? Br2 Cu2 N3 C6 -76.9(7) . . . . ? Br1 Cu2 N3 C6 52.4(3) . . . . ? N3 Cu2 N4 C7 47.1(4) . . . . ? Br4 Cu2 N4 C7 109.5(5) . . . . ? Br2 Cu2 N4 C7 -140.4(3) . . . . ? Br1 Cu2 N4 C7 -47.8(4) . . . . ? N3 Cu2 N4 C10 -75.1(3) . . . . ? Br4 Cu2 N4 C10 -12.6(6) . . . . ? Br2 Cu2 N4 C10 97.5(3) . . . . ? Br1 Cu2 N4 C10 -169.9(3) . . . . ? C3 N1 C1 C2 84.8(5) . . . . ? Cu1 N1 C1 C2 -35.6(5) . . . . ? C5 N2 C2 C1 -80.6(5) . . . . ? Cu1 N2 C2 C1 37.6(5) . . . . ? N1 C1 C2 N2 -1.4(6) . . . . ? C1 N1 C3 C4 -49.0(6) . . . . ? Cu1 N1 C3 C4 70.8(5) . . . . ? N1 C3 C4 C5 -44.4(7) . . . . ? C2 N2 C5 C4 46.5(6) . . . . ? Cu1 N2 C5 C4 -72.0(5) . . . . ? C3 C4 C5 N2 45.9(8) . . . . ? C8 N3 C6 C7 -81.7(6) . . . . ? Cu2 N3 C6 C7 37.1(5) . . . . ? C10 N4 C7 C6 80.5(6) . . . . ? Cu2 N4 C7 C6 -37.8(6) . . . . ? N3 C6 C7 N4 0.2(7) . . . . ? C6 N3 C8 C9 45.1(6) . . . . ? Cu2 N3 C8 C9 -72.6(5) . . . . ? N3 C8 C9 C10 47.3(7) . . . . ? C8 C9 C10 N4 -47.8(7) . . . . ? C7 N4 C10 C9 -45.1(7) . . . . ? Cu2 N4 C10 C9 72.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.837 _refine_diff_density_min -1.096 _refine_diff_density_rms 0.147