# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1592 data_[CuNi(en)]Cl2-0.5H2O #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jan 26 16:40:33 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 738.42 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H25 Br2 Cl2 Cu N4 O2.50 Ni ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.592(4) _cell_length_b 12.132(3) _cell_length_c 11.024(3) _cell_angle_alpha 114.66(2) _cell_angle_beta 101.92(3) _cell_angle_gamma 85.74(2) _cell_volume 1378.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.3 _cell_measurement_theta_max 14.4 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732.00 _exptl_absorpt_coefficient_mu 4.585 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.84 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 0 1 1 1 1 2 1 _diffrn_reflns_number 5115 _reflns_number_total 4852 _reflns_number_gt 3037 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02764 _diffrn_orient_matrix_UB_12 0.05590 _diffrn_orient_matrix_UB_13 0.09753 _diffrn_orient_matrix_UB_21 0.04285 _diffrn_orient_matrix_UB_22 -0.06836 _diffrn_orient_matrix_UB_23 0.01702 _diffrn_orient_matrix_UB_31 0.07194 _diffrn_orient_matrix_UB_32 0.02073 _diffrn_orient_matrix_UB_33 -0.02346 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br -0.0677(1) 0.7407(1) 0.5154(1) 0.0636(5) Uani 1.00 d . . . Br(2) Br 0.3560(1) 0.0417(1) 0.7681(1) 0.0686(5) Uani 1.00 d . . . Cu Cu 0.1929(1) 0.1622(1) 0.1699(1) 0.0370(4) Uani 1.00 d . . . Ni Ni 0.0728(1) -0.1187(1) 0.0378(1) 0.0313(4) Uani 1.00 d . . . Cl(1) Cl 0.1139(2) 0.0082(2) -0.0732(3) 0.0365(8) Uani 1.00 d . . . Cl(2) Cl 0.5834(7) 0.3384(6) 0.617(1) 0.215(4) Uani 0.65 d P . . Cl(3) Cl 0.617(1) 0.506(2) 0.435(2) 0.180(8) Uani 0.35 d P . . O(1) O 0.0339(6) 0.2288(5) 0.1428(6) 0.032(2) Uani 1.00 d . . . O(2) O 0.1599(6) 0.0237(6) 0.2090(7) 0.035(2) Uani 1.00 d . . . O(3) O 0.421(3) 0.418(3) 0.865(3) 0.19(2) Uani 0.50 d P . . N(1) N -0.2128(7) 0.2370(8) 0.0184(9) 0.040(3) Uani 1.00 d . . . N(2) N 0.2561(8) 0.3097(8) 0.1798(9) 0.041(3) Uani 1.00 d . . . N(3) N 0.3590(8) 0.1455(8) 0.2395(10) 0.042(3) Uani 1.00 d . . . N(4) N 0.0565(8) -0.2079(7) 0.1611(8) 0.036(3) Uani 1.00 d . . . C(1) C -0.328(1) 0.173(1) -0.043(1) 0.058(4) Uani 1.00 d . . . C(2) C -0.2043(10) 0.2900(9) 0.170(1) 0.043(3) Uani 1.00 d . . . C(3) C 0.0125(9) 0.3442(9) 0.2213(10) 0.033(3) Uani 1.00 d . . . C(4) C -0.1028(9) 0.3788(9) 0.244(1) 0.035(3) Uani 1.00 d . . . C(5) C -0.125(1) 0.4966(10) 0.332(1) 0.042(4) Uani 1.00 d . . . C(6) C -0.034(1) 0.5803(9) 0.394(1) 0.044(4) Uani 1.00 d . . . C(7) C 0.076(1) 0.5553(9) 0.369(1) 0.045(4) Uani 1.00 d . . . C(8) C 0.1007(10) 0.4351(9) 0.279(1) 0.038(3) Uani 1.00 d . . . C(9) C 0.216(1) 0.4139(9) 0.246(1) 0.041(3) Uani 1.00 d . . . C(10) C 0.377(1) 0.298(1) 0.156(1) 0.057(4) Uani 1.00 d . . . C(11) C 0.440(1) 0.200(1) 0.196(1) 0.063(5) Uani 1.00 d . . . C(12) C 0.3925(9) 0.1295(10) 0.348(1) 0.041(3) Uani 1.00 d . . . C(13) C 0.2105(9) 0.0216(9) 0.329(1) 0.032(3) Uani 1.00 d . . . C(14) C 0.3200(9) 0.0767(9) 0.402(1) 0.035(3) Uani 1.00 d . . . C(15) C 0.3615(10) 0.0809(10) 0.532(1) 0.044(3) Uani 1.00 d . . . C(16) C 0.301(1) 0.027(1) 0.588(1) 0.045(4) Uani 1.00 d . . . C(17) C 0.200(1) -0.0368(10) 0.513(1) 0.043(4) Uani 1.00 d . . . C(18) C 0.1540(9) -0.0424(9) 0.383(1) 0.036(3) Uani 1.00 d . . . C(19) C 0.0444(10) -0.1174(10) 0.300(1) 0.042(4) Uani 1.00 d . . . C(20) C -0.048(1) -0.2905(10) 0.105(1) 0.047(4) Uani 1.00 d . . . C(21) C 0.166(1) -0.2785(10) 0.169(1) 0.050(4) Uani 1.00 d . . . C(22) C 0.209(1) -0.3334(9) 0.033(1) 0.047(4) Uani 1.00 d . . . H(1) H -0.3912 0.2255 -0.0159 0.0674 Uiso 1.00 calc . . . H(2) H -0.3392 0.1363 -0.1397 0.0674 Uiso 1.00 calc . . . H(3) H -0.3301 0.1081 -0.0131 0.0674 Uiso 1.00 calc . . . H(4) H -0.2798 0.3277 0.1895 0.0515 Uiso 1.00 calc . . . H(5) H -0.1978 0.2229 0.1973 0.0515 Uiso 1.00 calc . . . H(6) H -0.2095 0.5133 0.3466 0.0547 Uiso 1.00 calc . . . H(7) H 0.1455 0.6178 0.4156 0.0623 Uiso 1.00 calc . . . H(8) H 0.2721 0.4848 0.2808 0.0516 Uiso 1.00 calc . . . H(9) H 0.3790 0.2775 0.0612 0.0667 Uiso 1.00 calc . . . H(10) H 0.4208 0.3750 0.2075 0.0667 Uiso 1.00 calc . . . H(11) H 0.5085 0.2377 0.2704 0.0772 Uiso 1.00 calc . . . H(12) H 0.4734 0.1417 0.1219 0.0772 Uiso 1.00 calc . . . H(13) H 0.4731 0.1565 0.3997 0.0487 Uiso 1.00 calc . . . H(14) H 0.4350 0.1225 0.5844 0.0556 Uiso 1.00 calc . . . H(15) H 0.1563 -0.0810 0.5470 0.0503 Uiso 1.00 calc . . . H(16) H -0.0205 -0.0631 0.2922 0.0479 Uiso 1.00 calc . . . H(17) H 0.0204 -0.1599 0.3491 0.0479 Uiso 1.00 calc . . . H(18) H -0.1183 -0.2415 0.1032 0.0545 Uiso 1.00 calc . . . H(19) H -0.0449 -0.3468 0.0181 0.0545 Uiso 1.00 calc . . . H(20) H -0.0518 -0.3279 0.1645 0.0545 Uiso 1.00 calc . . . H(21) H 0.2303 -0.2263 0.2390 0.0594 Uiso 1.00 calc . . . H(22) H 0.1547 -0.3415 0.1967 0.0594 Uiso 1.00 calc . . . H(23) H 0.1515 -0.3939 -0.0318 0.0538 Uiso 1.00 calc . . . H(24) H 0.2827 -0.3693 0.0406 0.0538 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.110(1) 0.0291(7) 0.0531(9) 0.0106(7) 0.0401(8) 0.0087(6) Br(2) 0.065(1) 0.099(1) 0.0390(8) 0.0067(8) 0.0071(7) 0.0282(8) Cu 0.0342(8) 0.0302(7) 0.0449(9) -0.0029(6) 0.0083(7) 0.0128(6) Ni 0.0327(8) 0.0266(7) 0.0331(8) 0.0000(6) 0.0090(6) 0.0095(6) Cl(1) 0.038(2) 0.034(1) 0.039(2) 0.002(1) 0.013(1) 0.013(1) Cl(2) 0.134(7) 0.056(4) 0.36(1) -0.069(5) -0.167(8) 0.079(6) Cl(3) 0.08(1) 0.34(3) 0.09(1) -0.05(1) 0.029(9) 0.04(1) O(1) 0.032(4) 0.021(4) 0.034(4) 0.001(3) 0.009(3) 0.003(3) O(2) 0.036(4) 0.032(4) 0.034(4) 0.000(3) 0.004(3) 0.012(3) O(3) 0.24(4) 0.20(3) 0.13(2) 0.14(3) 0.08(2) 0.08(2) N(1) 0.028(5) 0.040(5) 0.043(6) 0.000(4) 0.010(4) 0.007(5) N(2) 0.041(6) 0.036(5) 0.047(6) -0.003(4) 0.013(5) 0.015(5) N(3) 0.035(6) 0.043(6) 0.047(6) -0.002(4) 0.013(5) 0.016(5) N(4) 0.041(6) 0.034(5) 0.033(5) -0.003(4) 0.007(4) 0.013(4) C(1) 0.041(8) 0.056(8) 0.066(9) 0.010(6) 0.015(7) 0.014(7) C(2) 0.041(7) 0.042(7) 0.045(7) 0.008(5) 0.022(6) 0.012(6) C(3) 0.038(7) 0.034(6) 0.025(6) 0.000(5) 0.008(5) 0.010(5) C(4) 0.040(7) 0.030(6) 0.036(6) 0.002(5) 0.012(5) 0.012(5) C(5) 0.052(8) 0.040(7) 0.038(7) 0.005(6) 0.022(6) 0.013(6) C(6) 0.070(9) 0.032(6) 0.029(6) 0.010(6) 0.016(6) 0.008(5) C(7) 0.068(9) 0.027(6) 0.039(7) -0.004(6) 0.012(6) 0.011(5) C(8) 0.043(7) 0.033(6) 0.032(6) -0.004(5) 0.003(5) 0.010(5) C(9) 0.049(8) 0.030(6) 0.041(7) -0.014(5) 0.002(6) 0.012(5) C(10) 0.054(9) 0.050(8) 0.074(10) -0.005(6) 0.027(7) 0.025(7) C(11) 0.045(8) 0.078(10) 0.09(1) 0.011(7) 0.025(8) 0.051(9) C(12) 0.028(6) 0.043(7) 0.047(7) 0.000(5) 0.003(6) 0.016(6) C(13) 0.036(7) 0.028(6) 0.032(6) 0.009(5) 0.015(5) 0.008(5) C(14) 0.033(6) 0.034(6) 0.034(6) 0.005(5) 0.008(5) 0.011(5) C(15) 0.032(7) 0.042(7) 0.047(7) 0.003(5) 0.004(6) 0.008(6) C(16) 0.044(8) 0.054(8) 0.033(6) 0.002(6) 0.011(6) 0.014(6) C(17) 0.044(7) 0.040(7) 0.050(8) 0.010(6) 0.022(6) 0.020(6) C(18) 0.040(7) 0.034(6) 0.027(6) 0.005(5) 0.010(5) 0.006(5) C(19) 0.050(8) 0.045(7) 0.035(7) -0.011(6) 0.016(6) 0.014(5) C(20) 0.056(8) 0.045(7) 0.043(7) -0.019(6) 0.001(6) 0.023(6) C(21) 0.065(9) 0.037(7) 0.042(7) 0.004(6) 0.000(6) 0.017(6) C(22) 0.074(9) 0.029(6) 0.032(7) -0.001(6) 0.010(6) 0.006(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0046(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3037 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.538 _refine_ls_shift/su_max 0.3085 _refine_ls_shift/su_mean 0.0073 _refine_diff_density_min -0.45 _refine_diff_density_max 1.12 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Br(1) Cu 3.735(2) 1_555 2_566 yes Br(1) O(1) 3.570(7) 1_555 2_566 yes Br(1) O(2) 3.490(7) 1_555 2_566 yes Br(1) C(3) 3.40(1) 1_555 2_566 yes Br(1) C(4) 3.70(1) 1_555 2_566 yes Br(1) C(5) 2.84(1) 1_555 1_555 yes Br(1) C(6) 1.91(1) 1_555 1_555 yes Br(1) C(7) 2.82(1) 1_555 1_555 yes Br(1) C(8) 3.79(1) 1_555 2_566 yes Br(1) C(13) 3.215(9) 1_555 2_566 yes Br(1) C(14) 3.57(1) 1_555 2_566 yes Br(1) C(15) 3.96(1) 1_555 2_566 yes Br(1) C(17) 3.91(1) 1_555 2_566 yes Br(1) C(18) 3.48(1) 1_555 2_566 yes Br(1) C(19) 3.91(1) 1_555 1_565 yes Br(2) Cl(1) 3.727(3) 1_555 1_556 yes Br(2) N(3) 3.862(9) 1_555 2_656 yes Br(2) C(1) 3.91(1) 1_555 1_656 yes Br(2) C(11) 3.73(1) 1_555 2_656 yes Br(2) C(12) 3.59(1) 1_555 2_656 yes Br(2) C(15) 2.85(1) 1_555 1_555 yes Br(2) C(16) 1.89(1) 1_555 1_555 yes Br(2) C(17) 2.83(1) 1_555 1_555 yes Cu Ni 3.376(2) 1_555 1_555 yes Cu Ni 3.365(2) 1_555 2_555 yes Cu Cl(1) 2.563(3) 1_555 1_555 yes Cu Cl(1) 3.968(3) 1_555 2_555 yes Cu O(1) 1.972(7) 1_555 1_555 yes Cu O(2) 1.981(7) 1_555 1_555 yes Cu N(2) 1.937(8) 1_555 1_555 yes Cu N(3) 1.950(9) 1_555 1_555 yes Cu C(3) 2.89(1) 1_555 1_555 yes Cu C(8) 3.20(1) 1_555 1_555 yes Cu C(9) 2.83(1) 1_555 1_555 yes Cu C(10) 2.86(1) 1_555 1_555 yes Cu C(11) 2.88(1) 1_555 1_555 yes Cu C(12) 2.83(1) 1_555 1_555 yes Cu C(13) 2.88(1) 1_555 1_555 yes Cu C(14) 3.20(1) 1_555 1_555 yes Cu C(20) 3.98(1) 1_555 2_555 yes Ni Ni 3.540(3) 1_555 2_555 yes Ni Cl(1) 2.453(3) 1_555 1_555 yes Ni Cl(1) 2.472(3) 1_555 2_555 yes Ni O(1) 3.896(6) 1_555 1_555 yes Ni O(1) 2.070(6) 1_555 2_555 yes Ni O(2) 2.078(7) 1_555 1_555 yes Ni O(2) 3.889(7) 1_555 2_555 yes Ni N(1) 2.099(8) 1_555 2_555 yes Ni N(4) 2.101(9) 1_555 1_555 yes Ni C(1) 2.98(1) 1_555 2_555 yes Ni C(2) 2.980(10) 1_555 2_555 yes Ni C(3) 3.056(10) 1_555 2_555 yes Ni C(4) 3.439(10) 1_555 2_555 yes Ni C(13) 3.08(1) 1_555 1_555 yes Ni C(18) 3.45(1) 1_555 1_555 yes Ni C(19) 2.97(1) 1_555 1_555 yes Ni C(20) 3.00(1) 1_555 1_555 yes Ni C(21) 2.90(1) 1_555 1_555 yes Ni C(22) 2.93(1) 1_555 1_555 yes Cl(1) Cl(1) 3.424(5) 1_555 2_555 yes Cl(1) O(1) 2.986(7) 1_555 1_555 yes Cl(1) O(1) 3.185(7) 1_555 2_555 yes Cl(1) O(2) 2.974(8) 1_555 1_555 yes Cl(1) O(2) 3.193(7) 1_555 2_555 yes Cl(1) N(1) 3.352(10) 1_555 2_555 yes Cl(1) N(2) 3.789(9) 1_555 1_555 yes Cl(1) N(3) 3.820(10) 1_555 1_555 yes Cl(1) N(4) 3.341(9) 1_555 2_555 yes Cl(1) C(1) 3.58(1) 1_555 2_555 yes Cl(1) C(2) 3.46(1) 1_555 2_555 yes Cl(1) C(19) 3.45(1) 1_555 2_555 yes Cl(1) C(20) 3.59(1) 1_555 2_555 yes Cl(2) Cl(3) 3.48(2) 1_555 1_555 yes Cl(2) Cl(3) 3.00(2) 1_555 2_666 yes Cl(2) O(3) 3.41(3) 1_555 1_555 yes Cl(2) C(9) 3.53(1) 1_555 2_666 yes Cl(2) C(12) 3.46(1) 1_555 1_555 yes Cl(2) C(15) 3.88(1) 1_555 1_555 yes Cl(2) C(21) 3.58(1) 1_555 2_656 yes Cl(3) Cl(3) 3.35(3) 1_555 2_666 yes Cl(3) O(3) 3.72(3) 1_555 2_666 yes Cl(3) N(2) 3.90(2) 1_555 2_666 yes Cl(3) C(2) 3.87(2) 1_555 1_655 yes Cl(3) C(5) 3.40(2) 1_555 1_655 yes Cl(3) C(7) 3.96(2) 1_555 2_666 yes Cl(3) C(8) 3.93(2) 1_555 2_666 yes Cl(3) C(9) 3.42(2) 1_555 2_666 yes Cl(3) C(10) 3.81(2) 1_555 1_555 yes Cl(3) C(11) 3.95(2) 1_555 1_555 yes O(1) O(2) 3.065(9) 1_555 1_555 yes O(1) N(1) 2.92(1) 1_555 1_555 yes O(1) N(2) 2.71(1) 1_555 1_555 yes O(1) N(3) 3.88(1) 1_555 1_555 yes O(1) N(4) 3.20(1) 1_555 2_555 yes O(1) C(2) 2.85(1) 1_555 1_555 yes O(1) C(3) 1.34(1) 1_555 1_555 yes O(1) C(4) 2.38(1) 1_555 1_555 yes O(1) C(5) 3.65(1) 1_555 1_555 yes O(1) C(7) 3.70(1) 1_555 1_555 yes O(1) C(8) 2.40(1) 1_555 1_555 yes O(1) C(9) 2.90(1) 1_555 1_555 yes O(1) C(20) 3.15(1) 1_555 2_555 yes O(1) C(21) 3.97(1) 1_555 2_555 yes O(1) C(22) 3.54(1) 1_555 2_555 yes O(2) N(1) 3.22(1) 1_555 2_555 yes O(2) N(2) 3.88(1) 1_555 1_555 yes O(2) N(3) 2.72(1) 1_555 1_555 yes O(2) N(4) 2.93(1) 1_555 1_555 yes O(2) C(1) 3.16(1) 1_555 2_555 yes O(2) C(12) 2.90(1) 1_555 1_555 yes O(2) C(13) 1.34(1) 1_555 1_555 yes O(2) C(14) 2.41(1) 1_555 1_555 yes O(2) C(15) 3.65(1) 1_555 1_555 yes O(2) C(17) 3.65(1) 1_555 1_555 yes O(2) C(18) 2.38(1) 1_555 1_555 yes O(2) C(19) 2.84(1) 1_555 1_555 yes O(2) C(21) 3.50(1) 1_555 1_555 yes O(2) C(22) 3.99(1) 1_555 1_555 yes O(3) O(3) 3.09(7) 1_555 2_667 yes O(3) C(5) 3.97(3) 1_555 2_566 yes O(3) C(22) 3.83(3) 1_555 1_566 yes N(1) N(4) 2.85(1) 1_555 2_555 yes N(1) C(1) 1.48(1) 1_555 1_555 yes N(1) C(2) 1.50(1) 1_555 1_555 yes N(1) C(3) 3.03(1) 1_555 1_555 yes N(1) C(4) 2.49(1) 1_555 1_555 yes N(1) C(5) 3.58(1) 1_555 1_555 yes N(1) C(13) 3.81(1) 1_555 2_555 yes N(1) C(20) 3.75(1) 1_555 2_555 yes N(1) C(21) 2.48(1) 1_555 2_555 yes N(1) C(22) 1.50(1) 1_555 2_555 yes N(2) N(3) 2.50(1) 1_555 1_555 yes N(2) C(3) 2.92(1) 1_555 1_555 yes N(2) C(7) 3.65(1) 1_555 1_555 yes N(2) C(8) 2.40(1) 1_555 1_555 yes N(2) C(9) 1.27(1) 1_555 1_555 yes N(2) C(10) 1.47(1) 1_555 1_555 yes N(2) C(11) 2.44(2) 1_555 1_555 yes N(2) C(12) 3.52(2) 1_555 1_555 yes N(2) C(20) 3.47(1) 1_555 2_555 yes N(3) C(1) 3.56(1) 1_555 2_555 yes N(3) C(9) 3.52(1) 1_555 1_555 yes N(3) C(10) 2.43(2) 1_555 1_555 yes N(3) C(11) 1.45(1) 1_555 1_555 yes N(3) C(12) 1.27(1) 1_555 1_555 yes N(3) C(13) 2.92(1) 1_555 1_555 yes N(3) C(14) 2.40(1) 1_555 1_555 yes N(3) C(15) 3.62(2) 1_555 1_555 yes N(4) C(1) 3.76(2) 1_555 2_555 yes N(4) C(3) 3.76(1) 1_555 2_555 yes N(4) C(13) 3.07(1) 1_555 1_555 yes N(4) C(17) 3.64(1) 1_555 1_555 yes N(4) C(18) 2.53(1) 1_555 1_555 yes N(4) C(19) 1.50(1) 1_555 1_555 yes N(4) C(20) 1.48(1) 1_555 1_555 yes N(4) C(21) 1.49(1) 1_555 1_555 yes N(4) C(22) 2.51(1) 1_555 1_555 yes C(1) C(2) 2.38(2) 1_555 1_555 yes C(1) C(4) 3.74(2) 1_555 1_555 yes C(1) C(12) 3.80(2) 1_555 2_555 yes C(1) C(13) 3.53(1) 1_555 2_555 yes C(1) C(14) 3.87(2) 1_555 2_555 yes C(1) C(21) 3.16(2) 1_555 2_555 yes C(1) C(22) 2.42(2) 1_555 2_555 yes C(2) C(3) 2.53(1) 1_555 1_555 yes C(2) C(4) 1.51(1) 1_555 1_555 yes C(2) C(5) 2.50(2) 1_555 1_555 yes C(2) C(6) 3.76(2) 1_555 1_555 yes C(2) C(8) 3.80(2) 1_555 1_555 yes C(2) C(21) 3.79(2) 1_555 2_555 yes C(2) C(22) 2.49(2) 1_555 2_555 yes C(3) C(4) 1.41(1) 1_555 1_555 yes C(3) C(5) 2.43(1) 1_555 1_555 yes C(3) C(6) 2.79(1) 1_555 1_555 yes C(3) C(6) 3.90(1) 1_555 2_566 yes C(3) C(7) 2.46(1) 1_555 1_555 yes C(3) C(8) 1.41(1) 1_555 1_555 yes C(3) C(9) 2.49(1) 1_555 1_555 yes C(3) C(20) 3.48(1) 1_555 2_555 yes C(3) C(22) 3.35(2) 1_555 2_555 yes C(4) C(5) 1.39(1) 1_555 1_555 yes C(4) C(6) 2.39(1) 1_555 1_555 yes C(4) C(6) 3.82(2) 1_555 2_566 yes C(4) C(7) 2.79(2) 1_555 1_555 yes C(4) C(7) 3.95(1) 1_555 2_566 yes C(4) C(8) 2.41(1) 1_555 1_555 yes C(4) C(9) 3.75(2) 1_555 1_555 yes C(4) C(22) 2.88(2) 1_555 2_555 yes C(5) C(6) 1.37(1) 1_555 1_555 yes C(5) C(6) 3.64(2) 1_555 2_566 yes C(5) C(7) 2.39(2) 1_555 1_555 yes C(5) C(7) 3.54(2) 1_555 2_566 yes C(5) C(8) 2.78(2) 1_555 1_555 yes C(5) C(8) 3.98(1) 1_555 2_566 yes C(5) C(22) 3.61(2) 1_555 2_555 yes C(6) C(6) 3.56(2) 1_555 2_566 yes C(6) C(7) 1.34(2) 1_555 1_555 yes C(6) C(7) 3.74(2) 1_555 2_566 yes C(6) C(8) 2.39(2) 1_555 1_555 yes C(6) C(8) 3.92(2) 1_555 2_566 yes C(6) C(9) 3.68(2) 1_555 1_555 yes C(7) C(8) 1.43(1) 1_555 1_555 yes C(7) C(9) 2.45(2) 1_555 1_555 yes C(7) C(21) 3.88(2) 1_555 1_565 yes C(8) C(9) 1.44(1) 1_555 1_555 yes C(8) C(10) 3.74(2) 1_555 1_555 yes C(8) C(20) 3.77(1) 1_555 2_555 yes C(9) C(10) 2.37(2) 1_555 1_555 yes C(9) C(11) 3.49(2) 1_555 1_555 yes C(9) C(20) 3.67(2) 1_555 2_555 yes C(10) C(11) 1.52(2) 1_555 1_555 yes C(10) C(12) 3.48(2) 1_555 1_555 yes C(11) C(12) 2.34(2) 1_555 1_555 yes C(11) C(14) 3.72(2) 1_555 1_555 yes C(12) C(13) 2.49(1) 1_555 1_555 yes C(12) C(14) 1.44(1) 1_555 1_555 yes C(12) C(15) 2.44(2) 1_555 1_555 yes C(12) C(16) 3.71(2) 1_555 1_555 yes C(12) C(16) 3.97(2) 1_555 2_656 yes C(12) C(18) 3.76(2) 1_555 1_555 yes C(13) C(14) 1.40(1) 1_555 1_555 yes C(13) C(15) 2.41(2) 1_555 1_555 yes C(13) C(16) 2.81(2) 1_555 1_555 yes C(13) C(17) 2.44(2) 1_555 1_555 yes C(13) C(18) 1.42(1) 1_555 1_555 yes C(13) C(19) 2.54(1) 1_555 1_555 yes C(13) C(21) 3.34(1) 1_555 1_555 yes C(14) C(15) 1.39(1) 1_555 1_555 yes C(14) C(16) 2.41(2) 1_555 1_555 yes C(14) C(17) 2.78(2) 1_555 1_555 yes C(14) C(18) 2.41(1) 1_555 1_555 yes C(14) C(19) 3.80(1) 1_555 1_555 yes C(15) C(15) 3.68(2) 1_555 2_656 yes C(15) C(16) 1.37(2) 1_555 1_555 yes C(15) C(17) 2.36(2) 1_555 1_555 yes C(15) C(18) 2.75(2) 1_555 1_555 yes C(16) C(17) 1.36(1) 1_555 1_555 yes C(16) C(18) 2.40(2) 1_555 1_555 yes C(16) C(19) 3.77(2) 1_555 1_555 yes C(17) C(18) 1.40(1) 1_555 1_555 yes C(17) C(19) 2.51(2) 1_555 1_555 yes C(17) C(19) 3.77(1) 1_555 2_556 yes C(17) C(21) 3.66(2) 1_555 1_555 yes C(18) C(19) 1.51(1) 1_555 1_555 yes C(18) C(20) 3.78(1) 1_555 1_555 yes C(18) C(21) 2.87(1) 1_555 1_555 yes C(19) C(20) 2.41(1) 1_555 1_555 yes C(19) C(21) 2.45(2) 1_555 1_555 yes C(19) C(22) 3.79(1) 1_555 1_555 yes C(20) C(21) 2.43(2) 1_555 1_555 yes C(20) C(22) 3.19(2) 1_555 1_555 yes C(21) C(22) 1.54(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) O(1) 3.570(7) 1_555 2_566 ? Br(1) O(2) 3.490(7) 1_555 2_566 ? Br(1) C(3) 3.40(1) 1_555 2_566 ? Br(1) C(5) 2.84(1) 1_555 1_555 ? Br(1) C(7) 2.82(1) 1_555 1_555 ? Br(1) C(13) 3.215(9) 1_555 2_566 ? Br(1) C(14) 3.57(1) 1_555 2_566 ? Br(1) C(18) 3.48(1) 1_555 2_566 ? Br(2) C(12) 3.59(1) 1_555 2_656 ? Br(2) C(15) 2.85(1) 1_555 1_555 ? Br(2) C(17) 2.83(1) 1_555 1_555 ? Cu Ni 3.376(2) 1_555 1_555 ? Cu Ni 3.365(2) 1_555 2_555 ? Cu Cl(1) 2.563(3) 1_555 1_555 ? Cu C(3) 2.89(1) 1_555 1_555 ? Cu C(8) 3.20(1) 1_555 1_555 ? Cu C(9) 2.83(1) 1_555 1_555 ? Cu C(10) 2.86(1) 1_555 1_555 ? Cu C(11) 2.88(1) 1_555 1_555 ? Cu C(12) 2.83(1) 1_555 1_555 ? Cu C(13) 2.88(1) 1_555 1_555 ? Cu C(14) 3.20(1) 1_555 1_555 ? Ni Ni 3.540(3) 1_555 2_555 ? Ni C(1) 2.98(1) 1_555 2_555 ? Ni C(2) 2.980(10) 1_555 2_555 ? Ni C(3) 3.056(10) 1_555 2_555 ? Ni C(4) 3.439(10) 1_555 2_555 ? Ni C(13) 3.08(1) 1_555 1_555 ? Ni C(18) 3.45(1) 1_555 1_555 ? Ni C(19) 2.97(1) 1_555 1_555 ? Ni C(20) 3.00(1) 1_555 1_555 ? Ni C(21) 2.90(1) 1_555 1_555 ? Ni C(22) 2.93(1) 1_555 1_555 ? Cl(1) Cl(1) 3.424(5) 1_555 2_555 ? Cl(1) O(1) 2.986(7) 1_555 1_555 ? Cl(1) O(1) 3.185(7) 1_555 2_555 ? Cl(1) O(2) 2.974(8) 1_555 1_555 ? Cl(1) O(2) 3.193(7) 1_555 2_555 ? Cl(1) N(1) 3.352(10) 1_555 2_555 ? Cl(1) N(4) 3.341(9) 1_555 2_555 ? Cl(1) C(1) 3.58(1) 1_555 2_555 ? Cl(1) C(2) 3.46(1) 1_555 2_555 ? Cl(1) C(19) 3.45(1) 1_555 2_555 ? Cl(1) C(20) 3.59(1) 1_555 2_555 ? Cl(2) Cl(3) 3.48(2) 1_555 1_555 ? Cl(2) Cl(3) 3.00(2) 1_555 2_666 ? Cl(2) O(3) 3.41(3) 1_555 1_555 ? Cl(2) C(9) 3.53(1) 1_555 2_666 ? Cl(2) C(12) 3.46(1) 1_555 1_555 ? Cl(2) C(21) 3.58(1) 1_555 2_656 ? Cl(3) Cl(3) 3.35(3) 1_555 2_666 ? Cl(3) C(5) 3.40(2) 1_555 1_655 ? Cl(3) C(9) 3.42(2) 1_555 2_666 ? O(1) O(2) 3.065(9) 1_555 1_555 ? O(1) N(1) 2.92(1) 1_555 1_555 ? O(1) N(2) 2.71(1) 1_555 1_555 ? O(1) N(4) 3.20(1) 1_555 2_555 ? O(1) C(2) 2.85(1) 1_555 1_555 ? O(1) C(9) 2.90(1) 1_555 1_555 ? O(1) C(20) 3.15(1) 1_555 2_555 ? O(1) C(22) 3.54(1) 1_555 2_555 ? O(2) N(1) 3.22(1) 1_555 2_555 ? O(2) N(3) 2.72(1) 1_555 1_555 ? O(2) N(4) 2.93(1) 1_555 1_555 ? O(2) C(1) 3.16(1) 1_555 2_555 ? O(2) C(12) 2.90(1) 1_555 1_555 ? O(2) C(19) 2.84(1) 1_555 1_555 ? O(2) C(21) 3.50(1) 1_555 1_555 ? O(3) O(3) 3.09(7) 1_555 2_667 ? N(1) N(4) 2.85(1) 1_555 2_555 ? N(1) C(3) 3.03(1) 1_555 1_555 ? N(1) C(5) 3.58(1) 1_555 1_555 ? N(2) C(3) 2.92(1) 1_555 1_555 ? N(2) C(12) 3.52(2) 1_555 1_555 ? N(2) C(20) 3.47(1) 1_555 2_555 ? N(3) C(1) 3.56(1) 1_555 2_555 ? N(3) C(9) 3.52(1) 1_555 1_555 ? N(3) C(13) 2.92(1) 1_555 1_555 ? N(4) C(13) 3.07(1) 1_555 1_555 ? N(4) C(18) 2.53(1) 1_555 1_555 ? N(4) C(22) 2.51(1) 1_555 1_555 ? C(1) C(13) 3.53(1) 1_555 2_555 ? C(1) C(21) 3.16(2) 1_555 2_555 ? C(2) C(3) 2.53(1) 1_555 1_555 ? C(3) C(6) 2.79(1) 1_555 1_555 ? C(3) C(20) 3.48(1) 1_555 2_555 ? C(3) C(22) 3.35(2) 1_555 2_555 ? C(4) C(7) 2.79(2) 1_555 1_555 ? C(4) C(22) 2.88(2) 1_555 2_555 ? C(5) C(7) 3.54(2) 1_555 2_566 ? C(5) C(8) 2.78(2) 1_555 1_555 ? C(6) C(6) 3.56(2) 1_555 2_566 ? C(9) C(11) 3.49(2) 1_555 1_555 ? C(10) C(12) 3.48(2) 1_555 1_555 ? C(13) C(16) 2.81(2) 1_555 1_555 ? C(13) C(19) 2.54(1) 1_555 1_555 ? C(13) C(21) 3.34(1) 1_555 1_555 ? C(14) C(17) 2.78(2) 1_555 1_555 ? C(15) C(18) 2.75(2) 1_555 1_555 ? C(17) C(19) 2.51(2) 1_555 1_555 ? C(18) C(21) 2.87(1) 1_555 1_555 ? C(20) C(22) 3.19(2) 1_555 1_555 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' Hisashi Okawa' _publ_contact_author_address ; Department of Chemistry, Faculty of science, Kyushu University, Hakozaki 6-10-1, Higashi-ku, Fukuoka 812-8581, Japan ; _publ_contact_author_email ' okawascc@mbox.nc.kyushu-u.ac.jp ' _publ_contact_author_fax ' 81-92-642-2607 ' _publ_contact_author_phone ' 81-92-642-2596' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chemical Communications' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ;