Crystallographic Information for the 4 structures reported in the Manuscript "New Structural Motifs, Unusual Quenching of the Emission and Second Harmonic Generation of Cu(I) Iodide Polymeric or Oligomeric Adducts with some para-Substituted Pyridines or trans-Stilbazoles" by Elena Cariati, Dominique Roberto, Renato Ugo, Peter Ford, Simona Galli, and Angelo Sironi to be submitted to Inorganic Chemistry. #========================================================================== data_[CuI(N-trans-4-stilbazole)]n, compound 1 in the Manuscript _audit_creation_method SHELXL-97 #========================================================================== # CHEMICAL DATA _chemical_name_systematic ; catena(N-trans-4-stilbazole-iodide-copper(i)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H11 Cu I N' _chemical_formula_sum 'C13 H11 Cu I N' _chemical_formula_weight 371.67 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #========================================================================== # CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 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 15.978(6) _cell_length_b 4.148(2) _cell_length_c 19.338(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.340(10) _cell_angle_gamma 90.00 _cell_volume 1247.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour platelet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 4.197 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2845 _exptl_absorpt_correction_T_max 0.8501 _exptl_absorpt_process_details ? #========================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 area detector' _diffrn_detector 'scintillation counter' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14404 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 30.49 _reflns_number_total 3521 _reflns_number_gt 2298 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2001)' #========================================================================== # DATA REFINEMENT _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^)+(0.0230P)^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 3521 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0481 _refine_ls_wR_factor_gt 0.0452 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.003 #========================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 I I 0.088196(11) 0.05380(4) 0.340634(9) 0.03988(6) Uani 1 1 d . . . Cu Cu 0.01612(2) 0.04838(9) 0.204280(18) 0.04948(10) Uani 1 1 d . . . N1 N 0.10907(14) 0.0514(5) 0.14739(12) 0.0441(5) Uani 1 1 d . . . C2 C 0.18674(19) 0.1847(8) 0.17124(16) 0.0573(8) Uani 1 1 d . . . H2 H 0.2007 0.2643 0.2174 0.069 Uiso 1 1 calc R . . C3 C 0.24646(19) 0.2095(8) 0.13109(15) 0.0584(8) Uani 1 1 d . . . H3 H 0.2994 0.3042 0.1507 0.070 Uiso 1 1 calc R . . C4 C 0.22994(17) 0.0968(6) 0.06201(14) 0.0436(7) Uani 1 1 d . . . C5 C 0.14928(18) -0.0448(7) 0.03739(15) 0.0521(7) Uani 1 1 d . . . H5 H 0.1338 -0.1264 -0.0086 0.063 Uiso 1 1 calc R . . C6 C 0.09319(18) -0.0634(7) 0.08093(14) 0.0508(7) Uani 1 1 d . . . H6 H 0.0404 -0.1626 0.0632 0.061 Uiso 1 1 calc R . . C7 C 0.29369(17) 0.1277(7) 0.01862(15) 0.0494(7) Uani 1 1 d . . . H7 H 0.3438 0.2407 0.0384 0.059 Uiso 1 1 calc R . . C7' C 0.28663(18) 0.0107(6) -0.04548(16) 0.0463(7) Uani 1 1 d . . . H7' H 0.2359 -0.0993 -0.0647 0.056 Uiso 1 1 calc R . . C1' C 0.4637(2) 0.0363(8) -0.1785(2) 0.0689(10) Uani 1 1 d . . . H1' H 0.5026 0.0355 -0.2077 0.083 Uiso 1 1 calc R . . C2' C 0.3847(2) -0.1113(8) -0.20113(17) 0.0651(9) Uani 1 1 d . . . H2' H 0.3698 -0.2079 -0.2457 0.078 Uiso 1 1 calc R . . C3' C 0.32828(19) -0.1144(7) -0.15728(16) 0.0558(8) Uani 1 1 d . . . H3' H 0.2753 -0.2161 -0.1724 0.067 Uiso 1 1 calc R . . C4' C 0.34855(17) 0.0311(6) -0.09081(15) 0.0448(7) Uani 1 1 d . . . C5' C 0.42802(19) 0.1816(7) -0.06965(17) 0.0565(8) Uani 1 1 d . . . H5' H 0.4429 0.2820 -0.0255 0.068 Uiso 1 1 calc R . . C6' C 0.4852(2) 0.1839(8) -0.1134(2) 0.0674(9) Uani 1 1 d . . . H6' H 0.5382 0.2854 -0.0988 0.081 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 I 0.04643(11) 0.03289(9) 0.03617(10) 0.00065(8) 0.00100(7) 0.00245(8) Cu 0.0521(2) 0.0558(2) 0.0421(2) -0.00465(16) 0.01385(17) -0.00372(16) N1 0.0450(13) 0.0492(13) 0.0385(13) -0.0022(10) 0.0102(10) -0.0022(11) C2 0.0540(19) 0.074(2) 0.0451(18) -0.0178(15) 0.0141(15) -0.0158(16) C3 0.0440(18) 0.078(2) 0.0516(19) -0.0167(16) 0.0080(15) -0.0180(15) C4 0.0434(16) 0.0475(17) 0.0414(16) -0.0018(12) 0.0127(13) -0.0010(12) C5 0.0518(18) 0.070(2) 0.0339(15) -0.0085(14) 0.0095(13) -0.0097(15) C6 0.0428(16) 0.069(2) 0.0396(16) -0.0064(14) 0.0075(13) -0.0099(14) C7 0.0407(16) 0.0562(19) 0.0513(18) -0.0046(14) 0.0103(14) -0.0098(13) C7' 0.0394(15) 0.0506(19) 0.0483(17) 0.0033(13) 0.0087(13) 0.0000(12) C1' 0.067(2) 0.074(2) 0.078(3) 0.0174(19) 0.042(2) 0.0107(18) C2' 0.068(2) 0.077(2) 0.053(2) 0.0051(17) 0.0200(18) 0.0111(18) C3' 0.0501(18) 0.071(2) 0.0480(18) 0.0028(15) 0.0141(15) 0.0048(15) C4' 0.0424(16) 0.0454(16) 0.0472(16) 0.0112(13) 0.0116(13) 0.0051(12) C5' 0.0523(19) 0.0609(19) 0.058(2) 0.0004(15) 0.0163(16) -0.0054(15) C6' 0.056(2) 0.071(2) 0.082(3) 0.006(2) 0.0283(19) -0.0081(17) #========================================================================== # MOLECULAR GEOMETRY _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 I Cu 2.6227(11) . ? I Cu 2.6595(9) 2 ? I Cu 2.6943(10) 2_545 ? Cu N1 2.042(2) . ? Cu I 2.6595(9) 2_545 ? Cu I 2.6943(9) 2 ? Cu Cu 2.8485(10) 2 ? Cu Cu 2.8485(10) 2_545 ? N1 C6 1.339(3) . ? N1 C2 1.339(3) . ? C2 C3 1.366(4) . ? C3 C4 1.382(4) . ? C4 C5 1.396(4) . ? C4 C7 1.467(4) . ? C5 C6 1.366(4) . ? C7 C7' 1.312(4) . ? C7' C4' 1.468(4) . ? C1' C6' 1.370(5) . ? C1' C2' 1.380(5) . ? C2' C3' 1.372(4) . ? C3' C4' 1.389(4) . ? C4' C5' 1.389(4) . ? C5' C6' 1.382(4) . ? 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 Cu I Cu 65.262(15) . 2 ? Cu I Cu 64.770(15) . 2_545 ? Cu I Cu 101.57(4) 2 2_545 ? N1 Cu I 109.65(7) . . ? N1 Cu I 107.92(6) . 2_545 ? I Cu I 115.574(18) . 2_545 ? N1 Cu I 107.11(7) . 2 ? I Cu I 114.389(17) . 2 ? I Cu I 101.57(4) 2_545 2 ? N1 Cu Cu 126.02(6) . 2 ? I Cu Cu 57.99(2) . 2 ? I Cu Cu 125.10(3) 2_545 2 ? I Cu Cu 56.40(3) 2 2 ? N1 Cu Cu 126.66(6) . 2_545 ? I Cu Cu 58.83(2) . 2_545 ? I Cu Cu 56.74(3) 2_545 2_545 ? I Cu Cu 125.43(3) 2 2_545 ? Cu Cu Cu 93.46(4) 2 2_545 ? C6 N1 C2 115.6(2) . . ? C6 N1 Cu 120.97(19) . . ? C2 N1 Cu 123.25(19) . . ? N1 C2 C3 123.3(3) . . ? C2 C3 C4 121.4(3) . . ? C3 C4 C5 115.3(3) . . ? C3 C4 C7 121.4(2) . . ? C5 C4 C7 123.3(2) . . ? C6 C5 C4 119.9(3) . . ? N1 C6 C5 124.4(3) . . ? C7' C7 C4 126.1(3) . . ? C7 C7' C4' 128.3(3) . . ? C6' C1' C2' 120.4(3) . . ? C3' C2' C1' 119.4(3) . . ? C2' C3' C4' 121.5(3) . . ? C3' C4' C5' 118.0(3) . . ? C3' C4' C7' 118.8(3) . . ? C5' C4' C7' 123.1(3) . . ? C6' C5' C4' 120.7(3) . . ? C1' C6' C5' 119.9(3) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.419 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.080 #================================================================================= data_[CuI(N-trans-4'-dimethylamino-4-stilbazole)]n, compound 2 in the Manuscript _audit_creation_method SHELXL-97 #================================================================================= # CHEMICAL DATA _chemical_name_systematic ; catena-bis(N-trans-4'-dimethyilamino-4-stilbazole-iodide-copper(i)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 Cu2 I2 N4' _chemical_formula_sum 'C30 H32 Cu2 I2 N4' _chemical_formula_weight 829.48 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' #========================================================================== # CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 7.574(4) _cell_length_b 11.662(6) _cell_length_c 33.970(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3001(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour needle _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 3.501 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? #========================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 area detector' _diffrn_detector 'scintillation counter' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24839 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.03 _reflns_number_total 5394 _reflns_number_gt 4351 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2001)' #========================================================================== # DATA REFINEMENT _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^)+(0.0328P)^2^+44.0095P] 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 SHELXL _refine_ls_extinction_coef 0.00079(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.65(6) _refine_ls_number_reflns 5394 _refine_ls_number_parameters 296 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 #========================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cu1 Cu 0.3918(3) 0.3684(2) 0.50713(7) 0.0603(6) Uani 1 1 d . . . Cu2 Cu 0.6408(4) 0.3676(2) 0.56129(7) 0.0720(7) Uani 1 1 d . . . I1 I 0.55508(11) 0.17075(7) 0.53223(5) 0.0456(2) Uani 1 1 d . . . I2 I 0.53175(14) 0.55843(8) 0.53419(5) 0.0589(3) Uani 1 1 d . . . N11 N 0.4048(15) 0.3701(11) 0.4470(4) 0.041(3) Uani 1 1 d . . . C12 C 0.343(2) 0.2817(13) 0.4259(5) 0.047(4) Uani 1 1 d . . . H12 H 0.2818 0.2237 0.4387 0.056 Uiso 1 1 calc R . . C13 C 0.368(2) 0.2738(14) 0.3859(4) 0.051(4) Uani 1 1 d . . . H13 H 0.3183 0.2130 0.3721 0.061 Uiso 1 1 calc R . . C14 C 0.466(2) 0.3542(15) 0.3660(4) 0.051(4) Uani 1 1 d . . . C15 C 0.526(2) 0.4473(15) 0.3877(5) 0.054(4) Uani 1 1 d . . . H15 H 0.5863 0.5063 0.3752 0.065 Uiso 1 1 calc R . . C16 C 0.495(2) 0.4532(15) 0.4284(4) 0.049(4) Uani 1 1 d . . . H16 H 0.5368 0.5155 0.4427 0.059 Uiso 1 1 calc R . . C17 C 0.499(2) 0.3386(17) 0.3230(5) 0.059(5) Uani 1 1 d . . . H17 H 0.4491 0.2743 0.3112 0.071 Uiso 1 1 calc R . . C17' C 0.591(2) 0.4068(16) 0.3007(5) 0.056(4) Uani 1 1 d . . . H17' H 0.6367 0.4722 0.3125 0.067 Uiso 1 1 calc R . . C14' C 0.629(2) 0.3909(16) 0.2587(4) 0.056(4) Uani 1 1 d . . . C15' C 0.580(2) 0.2975(17) 0.2367(5) 0.057(5) Uani 1 1 d . . . H15' H 0.5148 0.2393 0.2485 0.068 Uiso 1 1 calc R . . C16' C 0.625(2) 0.2876(15) 0.1969(5) 0.051(4) Uani 1 1 d . . . H16' H 0.5906 0.2237 0.1825 0.062 Uiso 1 1 calc R . . C11' C 0.7245(19) 0.3760(17) 0.1787(4) 0.054(4) Uani 1 1 d . . . C12' C 0.773(2) 0.4700(13) 0.2008(4) 0.045(4) Uani 1 1 d . . . H12' H 0.8382 0.5288 0.1892 0.053 Uiso 1 1 calc R . . C13' C 0.726(2) 0.4769(14) 0.2399(5) 0.049(4) Uani 1 1 d . . . H13' H 0.7594 0.5411 0.2543 0.059 Uiso 1 1 calc R . . N12 N 0.7716(18) 0.3619(10) 0.1392(3) 0.044(3) Uani 1 1 d . . . C18 C 0.863(2) 0.4602(17) 0.1192(5) 0.064(5) Uani 1 1 d . . . H181 H 0.8885 0.4397 0.0925 0.077 Uiso 1 1 calc R . . H182 H 0.9704 0.4775 0.1328 0.077 Uiso 1 1 calc R . . H183 H 0.7869 0.5262 0.1196 0.077 Uiso 1 1 calc R . . C19 C 0.728(3) 0.2705(15) 0.1168(5) 0.060(5) Uani 1 1 d . . . H191 H 0.7753 0.2806 0.0907 0.072 Uiso 1 1 calc R . . H192 H 0.6023 0.2637 0.1154 0.072 Uiso 1 1 calc R . . H193 H 0.7770 0.2021 0.1282 0.072 Uiso 1 1 calc R . . N21 N 0.710(5) 0.371(3) 0.6180(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C22 C 0.803(5) 0.289(3) 0.6384(7) 0.0398(11) Uiso 0.539(13) 1 d PD . . C23 C 0.847(4) 0.300(2) 0.6797(7) 0.0398(11) Uiso 0.539(13) 1 d PD . . C24 C 0.779(4) 0.397(2) 0.6996(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C25 C 0.674(4) 0.475(2) 0.6798(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C26 C 0.641(6) 0.453(3) 0.6392(7) 0.0398(11) Uiso 0.539(13) 1 d PD . . C27 C 0.818(3) 0.4094(19) 0.7428(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C27' C 0.910(3) 0.3373(18) 0.7637(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C24' C 0.961(3) 0.348(2) 0.8058(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C25' C 1.064(4) 0.263(3) 0.8242(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C26' C 1.111(4) 0.266(2) 0.8641(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C21' C 1.051(4) 0.360(2) 0.8866(5) 0.0398(11) Uiso 0.539(13) 1 d PD . . C22' C 0.957(4) 0.450(2) 0.8689(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C23' C 0.915(4) 0.443(2) 0.8276(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . N22 N 1.085(3) 0.3637(17) 0.9269(5) 0.0398(11) Uiso 0.539(13) 1 d PD . . C28 C 1.007(4) 0.447(2) 0.9523(6) 0.0398(11) Uiso 0.539(13) 1 d PD . . C29 C 1.179(4) 0.268(2) 0.9448(7) 0.0398(11) Uiso 0.539(13) 1 d PD . . N31 N 0.690(6) 0.370(3) 0.6186(6) 0.0398(11) Uiso 0.461(13) 1 d PD . . C32 C 0.798(6) 0.281(3) 0.6303(7) 0.0398(11) Uiso 0.461(13) 1 d PD . . C33 C 0.859(5) 0.267(3) 0.6703(7) 0.0398(11) Uiso 0.461(13) 1 d PD . . C34 C 0.810(4) 0.352(3) 0.6976(6) 0.0398(11) Uiso 0.461(13) 1 d PD . . C35 C 0.707(5) 0.445(3) 0.6855(7) 0.0398(11) Uiso 0.461(13) 1 d PD . . C36 C 0.664(6) 0.449(3) 0.6447(8) 0.0398(11) Uiso 0.461(13) 1 d PD . . C37 C 0.877(4) 0.340(2) 0.7390(7) 0.0398(11) Uiso 0.461(13) 1 d PD . . C37' C 0.868(4) 0.418(2) 0.7662(7) 0.0398(11) Uiso 0.461(13) 1 d PD . . C34' C 0.935(4) 0.409(3) 0.8072(6) 0.0398(11) Uiso 0.461(13) 1 d PD . . C35' C 1.034(4) 0.314(3) 0.8203(6) 0.0398(11) Uiso 0.461(13) 1 d PD . . C36' C 1.097(4) 0.303(3) 0.8590(6) 0.0398(11) Uiso 0.461(13) 1 d PD . . C31' C 1.054(5) 0.390(2) 0.8859(6) 0.0398(11) Uiso 0.461(13) 1 d PD . . C32' C 0.953(5) 0.486(2) 0.8742(6) 0.0398(11) Uiso 0.461(13) 1 d PD . . C33' C 0.894(4) 0.493(3) 0.8340(7) 0.0398(11) Uiso 0.461(13) 1 d PD . . N32 N 1.118(3) 0.388(2) 0.9244(5) 0.0398(11) Uiso 0.461(13) 1 d PD . . C38 C 1.063(4) 0.472(2) 0.9527(7) 0.0398(11) Uiso 0.461(13) 1 d PD . . C39 C 1.206(4) 0.285(3) 0.9384(8) 0.0398(11) Uiso 0.461(13) 1 d PD . . 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 0.0641(13) 0.0746(16) 0.0423(11) 0.0003(11) -0.0005(10) -0.0107(11) Cu2 0.120(2) 0.0561(15) 0.0397(11) 0.0016(11) -0.0219(13) -0.0124(14) I1 0.0433(4) 0.0516(5) 0.0420(4) -0.0021(8) 0.0034(7) 0.0016(4) I2 0.0766(7) 0.0549(5) 0.0452(5) -0.0024(9) 0.0021(8) -0.0073(5) N11 0.037(7) 0.045(7) 0.041(6) -0.003(6) -0.003(5) 0.006(6) C12 0.049(9) 0.033(9) 0.058(10) -0.002(7) -0.006(8) -0.011(8) C13 0.061(11) 0.046(10) 0.045(9) -0.006(7) -0.012(8) 0.002(9) C14 0.041(8) 0.071(12) 0.040(8) -0.015(8) -0.006(7) 0.001(9) C15 0.052(10) 0.060(11) 0.050(9) 0.005(8) 0.013(8) 0.004(9) C16 0.043(9) 0.055(10) 0.049(9) -0.001(8) 0.002(7) -0.007(8) C17 0.049(10) 0.079(13) 0.049(9) -0.005(9) -0.007(8) 0.013(9) C17' 0.044(9) 0.076(12) 0.048(9) 0.009(9) 0.006(7) -0.001(9) C14' 0.045(9) 0.083(13) 0.040(8) -0.005(9) -0.002(7) 0.015(9) C15' 0.042(9) 0.068(12) 0.060(11) 0.023(9) 0.008(8) 0.006(9) C16' 0.050(9) 0.052(11) 0.052(9) -0.006(8) -0.003(8) -0.003(9) C11' 0.032(8) 0.088(14) 0.043(9) 0.004(9) 0.000(7) 0.004(9) C12' 0.055(9) 0.035(9) 0.044(9) -0.001(7) -0.001(7) -0.007(7) C13' 0.051(10) 0.046(10) 0.050(10) -0.005(7) 0.001(8) -0.011(8) N12 0.061(8) 0.031(7) 0.040(7) 0.000(6) 0.004(6) -0.008(6) C18 0.057(11) 0.087(14) 0.049(10) 0.017(10) 0.000(8) 0.007(10) C19 0.082(14) 0.047(12) 0.052(10) 0.007(9) 0.002(9) -0.007(10) #========================================================================== # MOLECULAR GEOMETRY _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 N11 2.046(12) . ? Cu1 I2 2.623(3) . ? Cu1 Cu2 2.635(3) . ? Cu1 I1 2.728(3) 4_455 ? Cu1 I1 2.751(3) . ? Cu2 N31 1.983(18) . ? Cu2 N21 1.996(17) . ? Cu2 I2 2.546(3) . ? Cu2 I1 2.582(3) . ? I1 Cu1 2.728(3) 4 ? N11 C12 1.339(19) . ? N11 C16 1.341(19) . ? C12 C13 1.37(2) . ? C13 C14 1.37(2) . ? C14 C15 1.39(2) . ? C14 C17 1.49(2) . ? C15 C16 1.41(2) . ? C17 C17' 1.30(2) . ? C17' C14' 1.47(2) . ? C14' C15' 1.37(2) . ? C14' C13' 1.40(2) . ? C15' C16' 1.40(2) . ? C16' C11' 1.42(2) . ? C11' C12' 1.38(2) . ? C11' N12 1.398(19) . ? C12' C13' 1.38(2) . ? N12 C19 1.353(19) . ? N12 C18 1.50(2) . ? N21 C26 1.30(2) . ? N21 C32 1.32(5) . ? N21 C36 1.33(5) . ? N21 C22 1.38(2) . ? C22 C33 1.20(4) . ? C22 N31 1.44(5) . ? C22 C23 1.45(2) . ? C23 C33 0.51(2) . ? C23 C34 0.91(3) . ? C23 C24 1.41(3) . ? C23 C32 1.73(3) . ? C23 C35 2.00(4) . ? C24 C34 0.57(2) . ? C24 C35 0.92(3) . ? C24 C25 1.39(3) . ? C24 C27 1.51(3) . ? C24 C37 1.67(3) . ? C24 C33 1.91(4) . ? C25 C36 1.23(4) . ? C25 C26 1.43(2) . ? C25 C34 1.86(4) . ? C26 N31 1.25(5) . ? C26 C35 1.65(4) . ? C27 C37' 0.88(3) . ? C27 C37 0.94(3) . ? C27 C27' 1.30(2) . ? C27 C34 1.68(3) . ? C27' C37 0.87(3) . ? C27' C37' 0.99(3) . ? C27' C24' 1.49(3) . ? C27' C34' 1.71(3) . ? C24' C34' 0.74(2) . ? C24' C35' 0.84(3) . ? C24' C23' 1.37(3) . ? C24' C25' 1.41(3) . ? C24' C37' 1.72(3) . ? C24' C33' 2.00(4) . ? C25' C35' 0.65(2) . ? C25' C36' 1.30(3) . ? C25' C26' 1.40(2) . ? C26' C21' 1.41(2) . ? C26' C31' 1.68(3) . ? C26' C35' 1.69(3) . ? C21' C36' 1.20(3) . ? C21' N22 1.395(19) . ? C21' C22' 1.41(2) . ? C21' N32 1.42(3) . ? C21' C32' 1.70(3) . ? C22' C31' 1.17(3) . ? C22' C33' 1.37(3) . ? C22' C23' 1.44(2) . ? C23' C33' 0.644(19) . ? C23' C34' 0.81(3) . ? C23' C32' 1.69(3) . ? C23' C35' 1.77(4) . ? N22 C39 1.35(3) . ? N22 C28 1.43(2) . ? N22 C31' 1.45(3) . ? N22 C29 1.45(2) . ? N22 C38 1.55(3) . ? C28 C38 0.52(4) . ? C28 N32 1.44(3) . ? C29 N32 1.63(3) . ? N31 C36 1.30(2) . ? N31 C32 1.38(2) . ? C32 C33 1.45(2) . ? C33 C34 1.41(3) . ? C34 C35 1.39(3) . ? C34 C37 1.51(3) . ? C35 C36 1.43(2) . ? C37 C37' 1.30(2) . ? C37' C34' 1.49(3) . ? C34' C33' 1.37(3) . ? C34' C35' 1.41(3) . ? C35' C36' 1.40(2) . ? C36' C31' 1.41(2) . ? C31' N32 1.40(2) . ? C31' C32' 1.41(2) . ? C32' C33' 1.44(2) . ? N32 C38 1.43(2) . ? N32 C39 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Cu1 I2 108.8(4) . . ? N11 Cu1 Cu2 131.5(4) . . ? I2 Cu1 Cu2 57.93(8) . . ? N11 Cu1 I1 111.0(3) . 4_455 ? I2 Cu1 I1 114.19(9) . 4_455 ? Cu2 Cu1 I1 116.77(10) . 4_455 ? N11 Cu1 I1 107.2(4) . . ? I2 Cu1 I1 114.68(9) . . ? Cu2 Cu1 I1 57.24(8) . . ? I1 Cu1 I1 100.55(8) 4_455 . ? N31 Cu2 N21 4(2) . . ? N31 Cu2 I2 113.9(10) . . ? N21 Cu2 I2 114.5(9) . . ? N31 Cu2 I1 115.7(13) . . ? N21 Cu2 I1 117.0(11) . . ? I2 Cu2 I1 123.88(10) . . ? N31 Cu2 Cu1 145.1(13) . . ? N21 Cu2 Cu1 149.4(11) . . ? I2 Cu2 Cu1 60.81(8) . . ? I1 Cu2 Cu1 63.66(8) . . ? Cu2 I1 Cu1 91.91(9) . 4 ? Cu2 I1 Cu1 59.11(7) . . ? Cu1 I1 Cu1 117.63(8) 4 . ? Cu2 I2 Cu1 61.27(8) . . ? C12 N11 C16 118.7(13) . . ? C12 N11 Cu1 120.7(11) . . ? C16 N11 Cu1 120.0(10) . . ? N11 C12 C13 122.3(15) . . ? C12 C13 C14 121.0(15) . . ? C13 C14 C15 116.6(14) . . ? C13 C14 C17 119.2(15) . . ? C15 C14 C17 124.2(16) . . ? C14 C15 C16 120.5(16) . . ? N11 C16 C15 120.8(15) . . ? C17' C17 C14 125.7(18) . . ? C17 C17' C14' 126.5(18) . . ? C15' C14' C13' 117.5(14) . . ? C15' C14' C17' 125.3(17) . . ? C13' C14' C17' 117.2(16) . . ? C14' C15' C16' 121.7(16) . . ? C15' C16' C11' 119.4(16) . . ? C12' C11' N12 123.1(15) . . ? C12' C11' C16' 119.0(14) . . ? N12 C11' C16' 117.9(15) . . ? C11' C12' C13' 120.0(14) . . ? C12' C13' C14' 122.4(15) . . ? C19 N12 C11' 124.9(14) . . ? C19 N12 C18 117.3(13) . . ? C11' N12 C18 117.6(14) . . ? C26 N21 C32 127.7(19) . . ? C26 N21 C36 11.1(16) . . ? C32 N21 C36 118(2) . . ? C26 N21 C22 115.8(15) . . ? C32 N21 C22 12.1(9) . . ? C36 N21 C22 105.6(17) . . ? C26 N21 Cu2 116.5(15) . . ? C32 N21 Cu2 114.9(18) . . ? C36 N21 Cu2 127(2) . . ? C22 N21 Cu2 127.0(16) . . ? C33 C22 N21 142(2) . . ? C33 C22 N31 141(3) . . ? N21 C22 N31 6(4) . . ? C33 C22 C23 19.3(12) . . ? N21 C22 C23 122.9(17) . . ? N31 C22 C23 122(2) . . ? C33 C23 C34 171(10) . . ? C33 C23 C24 167(5) . . ? C34 C23 C24 13.4(17) . . ? C33 C23 C22 51(4) . . ? C34 C23 C22 130(3) . . ? C24 C23 C22 116.9(17) . . ? C33 C23 C32 49(3) . . ? C34 C23 C32 132(3) . . ? C24 C23 C32 119(2) . . ? C22 C23 C32 2.4(15) . . ? C33 C23 C35 143(4) . . ? C34 C23 C35 36.9(19) . . ? C24 C23 C35 24.1(11) . . ? C22 C23 C35 92.8(15) . . ? C32 C23 C35 95.2(16) . . ? C34 C24 C35 137(4) . . ? C34 C24 C25 140(2) . . ? C35 C24 C25 4(3) . . ? C34 C24 C23 22(2) . . ? C35 C24 C23 117(3) . . ? C25 C24 C23 120.1(16) . . ? C34 C24 C27 97(2) . . ? C35 C24 C27 124(3) . . ? C25 C24 C27 121.4(17) . . ? C23 C24 C27 118.4(17) . . ? C34 C24 C37 63.7(18) . . ? C35 C24 C37 158(3) . . ? C25 C24 C37 155.1(19) . . ? C23 C24 C37 84.6(17) . . ? C27 C24 C37 33.8(11) . . ? C34 C24 C33 24.5(18) . . ? C35 C24 C33 114(2) . . ? C25 C24 C33 116.9(16) . . ? C23 C24 C33 3.5(13) . . ? C27 C24 C33 121.6(16) . . ? C37 C24 C33 87.8(14) . . ? C36 C25 C24 110(2) . . ? C36 C25 C26 7(3) . . ? C24 C25 C26 116.8(17) . . ? C36 C25 C34 99(2) . . ? C24 C25 C34 11.2(8) . . ? C26 C25 C34 105.8(15) . . ? N31 C26 N21 7(4) . . ? N31 C26 C25 129(2) . . ? N21 C26 C25 126.8(17) . . ? N31 C26 C35 113(2) . . ? N21 C26 C35 111.4(17) . . ? C25 C26 C35 15.6(9) . . ? C37' C27 C37 91.0(17) . . ? C37' C27 C27' 49.8(17) . . ? C37 C27 C27' 42.3(13) . . ? C37' C27 C24 166(4) . . ? C37 C27 C24 82.6(13) . . ? C27' C27 C24 124.9(15) . . ? C37' C27 C34 152(2) . . ? C37 C27 C34 63.1(12) . . ? C27' C27 C34 105.4(15) . . ? C24 C27 C34 19.6(9) . . ? C37 C27' C37' 87.7(17) . . ? C37 C27' C27 46.1(17) . . ? C37' C27' C27 42.6(13) . . ? C37 C27' C24' 173(2) . . ? C37' C27' C24' 85.5(13) . . ? C27 C27' C24' 127.3(15) . . ? C37 C27' C34' 148(2) . . ? C37' C27' C34' 60.1(12) . . ? C27 C27' C34' 102.4(15) . . ? C24' C27' C34' 25.5(8) . . ? C34' C24' C35' 126(4) . . ? C34' C24' C23' 29(2) . . ? C35' C24' C23' 104(3) . . ? C34' C24' C25' 143(2) . . ? C35' C24' C25' 17(2) . . ? C23' C24' C25' 117.9(18) . . ? C34' C24' C27' 94.3(15) . . ? C35' C24' C27' 134(3) . . ? C23' C24' C27' 121.6(18) . . ? C25' C24' C27' 120.5(18) . . ? C34' C24' C37' 59.3(14) . . ? C35' C24' C37' 161(4) . . ? C23' C24' C37' 86.7(17) . . ? C25' C24' C37' 154.6(19) . . ? C27' C24' C37' 35.1(11) . . ? C34' C24' C33' 25.1(16) . . ? C35' C24' C33' 107(3) . . ? C23' C24' C33' 4.1(11) . . ? C25' C24' C33' 121.5(16) . . ? C27' C24' C33' 117.9(15) . . ? C37' C24' C33' 82.9(13) . . ? C35' C25' C36' 86(2) . . ? C35' C25' C26' 105(2) . . ? C36' C25' C26' 19.9(13) . . ? C35' C25' C24' 22(3) . . ? C36' C25' C24' 105(2) . . ? C26' C25' C24' 123(2) . . ? C25' C26' C21' 118(2) . . ? C25' C26' C31' 113(2) . . ? C21' C26' C31' 8(2) . . ? C25' C26' C35' 21.8(9) . . ? C21' C26' C35' 96.3(18) . . ? C31' C26' C35' 90.8(17) . . ? C36' C21' N22 137(2) . . ? C36' C21' C26' 19.1(14) . . ? N22 C21' C26' 119.9(16) . . ? C36' C21' C22' 103.2(19) . . ? N22 C21' C22' 119.1(15) . . ? C26' C21' C22' 121.0(16) . . ? C36' C21' N32 137(3) . . ? N22 C21' N32 15.8(15) . . ? C26' C21' N32 124(2) . . ? C22' C21' N32 112.9(19) . . ? C36' C21' C32' 114(2) . . ? N22 C21' C32' 107.1(15) . . ? C26' C21' C32' 132.8(16) . . ? C22' C21' C32' 12.9(10) . . ? N32 C21' C32' 100.1(17) . . ? C31' C22' C33' 150(3) . . ? C31' C22' C21' 12(2) . . ? C33' C22' C21' 144(2) . . ? C31' C22' C23' 125(2) . . ? C33' C22' C23' 26.3(9) . . ? C21' C22' C23' 118.5(19) . . ? C33' C23' C34' 141(5) . . ? C33' C23' C24' 167(4) . . ? C34' C23' C24' 26(2) . . ? C33' C23' C22' 70(2) . . ? C34' C23' C22' 145(3) . . ? C24' C23' C22' 121(2) . . ? C33' C23' C32' 56.5(17) . . ? C34' C23' C32' 156(4) . . ? C24' C23' C32' 135(2) . . ? C22' C23' C32' 14.0(11) . . ? C33' C23' C35' 161(4) . . ? C34' C23' C35' 51(2) . . ? C24' C23' C35' 27.6(12) . . ? C22' C23' C35' 94.6(17) . . ? C32' C23' C35' 107.5(17) . . ? C39 N22 C21' 113(2) . . ? C39 N22 C28 125(2) . . ? C21' N22 C28 122.6(15) . . ? C39 N22 C31' 122(2) . . ? C21' N22 C31' 14.1(15) . . ? C28 N22 C31' 111.6(18) . . ? C39 N22 C29 14(2) . . ? C21' N22 C29 118.4(15) . . ? C28 N22 C29 118.1(14) . . ? C31' N22 C29 130.3(18) . . ? C39 N22 C38 117(2) . . ? C21' N22 C38 124.3(19) . . ? C28 N22 C38 19.4(16) . . ? C31' N22 C38 111(2) . . ? C29 N22 C38 116.2(19) . . ? C38 C28 N22 93(3) . . ? C38 C28 N32 79(3) . . ? N22 C28 N32 15.5(15) . . ? N22 C29 N32 12.9(15) . . ? C26 N31 C36 11.3(16) . . ? C26 N31 C32 126.6(18) . . ? C36 N31 C32 115.6(16) . . ? C26 N31 C22 115(2) . . ? C36 N31 C22 104.0(17) . . ? C32 N31 C22 11.6(9) . . ? C26 N31 Cu2 120(2) . . ? C36 N31 Cu2 130.5(19) . . ? C32 N31 Cu2 112.6(17) . . ? C22 N31 Cu2 124(2) . . ? N21 C32 N31 6(4) . . ? N21 C32 C33 124(2) . . ? N31 C32 C33 123.1(17) . . ? N21 C32 C23 108(2) . . ? N31 C32 C23 108.0(16) . . ? C33 C32 C23 15.3(9) . . ? C23 C33 C22 110(5) . . ? C23 C33 C34 6(6) . . ? C22 C33 C34 110(3) . . ? C23 C33 C32 116(3) . . ? C22 C33 C32 6.5(17) . . ? C34 C33 C32 116.7(17) . . ? C23 C33 C24 10(4) . . ? C22 C33 C24 101(2) . . ? C34 C33 C24 9.6(8) . . ? C32 C33 C24 107.3(15) . . ? C24 C34 C23 145(4) . . ? C24 C34 C35 27(2) . . ? C23 C34 C35 120(3) . . ? C24 C34 C33 146(3) . . ? C23 C34 C33 3(4) . . ? C35 C34 C33 120.2(16) . . ? C24 C34 C37 97(2) . . ? C23 C34 C37 117(3) . . ? C35 C34 C37 123.0(17) . . ? C33 C34 C37 116.8(17) . . ? C24 C34 C27 63.0(18) . . ? C23 C34 C27 150(3) . . ? C35 C34 C27 89.3(18) . . ? C33 C34 C27 150(2) . . ? C37 C34 C27 33.7(11) . . ? C24 C34 C25 28.4(17) . . ? C23 C34 C25 118(3) . . ? C35 C34 C25 1.8(13) . . ? C33 C34 C25 118.5(17) . . ? C37 C34 C25 124.6(16) . . ? C27 C34 C25 90.9(15) . . ? C24 C35 C34 16.2(16) . . ? C24 C35 C36 132(3) . . ? C34 C35 C36 116.6(17) . . ? C24 C35 C26 135(3) . . ? C34 C35 C26 120(2) . . ? C36 C35 C26 4(3) . . ? C24 C35 C23 39.0(19) . . ? C34 C35 C23 23.2(11) . . ? C36 C35 C23 93.4(15) . . ? C26 C35 C23 96.5(17) . . ? C25 C36 N31 145(2) . . ? C25 C36 N21 144(3) . . ? N31 C36 N21 7(4) . . ? C25 C36 C35 18.8(11) . . ? N31 C36 C35 126.8(18) . . ? N21 C36 C35 125(2) . . ? C27' C37 C27 91.6(17) . . ? C27' C37 C37' 49.9(17) . . ? C27 C37 C37' 42.8(13) . . ? C27' C37 C34 175(2) . . ? C27 C37 C34 83.2(13) . . ? C37' C37 C34 125.2(16) . . ? C27' C37 C24 155(2) . . ? C27 C37 C24 63.5(12) . . ? C37' C37 C24 105.5(16) . . ? C34 C37 C24 19.7(9) . . ? C27 C37' C27' 87.5(17) . . ? C27 C37' C37 46.2(17) . . ? C27' C37' C37 42.3(13) . . ? C27 C37' C34' 169(4) . . ? C27' C37' C34' 84.6(13) . . ? C37 C37' C34' 126.9(16) . . ? C27 C37' C24' 146(2) . . ? C27' C37' C24' 59.4(11) . . ? C37 C37' C24' 101.8(15) . . ? C34' C37' C24' 25.2(9) . . ? C24' C34' C23' 124(4) . . ? C24' C34' C33' 142(3) . . ? C23' C34' C33' 17(2) . . ? C24' C34' C35' 29(2) . . ? C23' C34' C35' 102(3) . . ? C33' C34' C35' 118.1(18) . . ? C24' C34' C37' 95.5(16) . . ? C23' C34' C37' 135(3) . . ? C33' C34' C37' 119.9(19) . . ? C35' C34' C37' 122.0(18) . . ? C24' C34' C27' 60.2(14) . . ? C23' C34' C27' 163(4) . . ? C33' C34' C27' 154(2) . . ? C35' C34' C27' 86.9(18) . . ? C37' C34' C27' 35.4(11) . . ? C25' C35' C24' 142(5) . . ? C25' C35' C36' 67(2) . . ? C24' C35' C36' 144(3) . . ? C25' C35' C34' 166(5) . . ? C24' C35' C34' 25(2) . . ? C36' C35' C34' 123(2) . . ? C25' C35' C26' 53.1(17) . . ? C24' C35' C26' 153(4) . . ? C36' C35' C26' 14.2(13) . . ? C34' C35' C26' 136(2) . . ? C25' C35' C23' 158(4) . . ? C24' C35' C23' 49(2) . . ? C36' C35' C23' 96.8(17) . . ? C34' C35' C23' 26.6(12) . . ? C26' C35' C23' 109.3(17) . . ? C21' C36' C25' 149(3) . . ? C21' C36' C35' 126(2) . . ? C25' C36' C35' 27.5(10) . . ? C21' C36' C31' 13(2) . . ? C25' C36' C31' 144(2) . . ? C35' C36' C31' 118(2) . . ? C22' C31' N32 134(2) . . ? C22' C31' C36' 105.2(19) . . ? N32 C31' C36' 121.2(17) . . ? C22' C31' C32' 17.2(14) . . ? N32 C31' C32' 117.5(16) . . ? C36' C31' C32' 121.2(16) . . ? C22' C31' N22 135(3) . . ? N32 C31' N22 15.6(15) . . ? C36' C31' N22 116(2) . . ? C32' C31' N22 122(2) . . ? C22' C31' C26' 118(2) . . ? N32 C31' C26' 108.1(16) . . ? C36' C31' C26' 14.6(12) . . ? C32' C31' C26' 134.3(17) . . ? N22 C31' C26' 101.5(17) . . ? C31' C32' C33' 118.4(19) . . ? C31' C32' C23' 96.6(17) . . ? C33' C32' C23' 21.9(8) . . ? C31' C32' C21' 7(2) . . ? C33' C32' C21' 114.4(19) . . ? C23' C32' C21' 92.5(16) . . ? C23' C33' C22' 83(2) . . ? C23' C33' C34' 22(3) . . ? C22' C33' C34' 104(2) . . ? C23' C33' C32' 102(2) . . ? C22' C33' C32' 18.4(11) . . ? C34' C33' C32' 122(2) . . ? C23' C33' C24' 9(2) . . ? C22' C33' C24' 91.5(19) . . ? C34' C33' C24' 13.2(10) . . ? C32' C33' C24' 109.4(17) . . ? C31' N32 C21' 14.4(16) . . ? C31' N32 C38 121.1(15) . . ? C21' N32 C38 132(2) . . ? C31' N32 C28 114(2) . . ? C21' N32 C28 120(2) . . ? C38 N32 C28 20.7(16) . . ? C31' N32 C39 118.6(16) . . ? C21' N32 C39 105.4(18) . . ? C38 N32 C39 118.5(15) . . ? C28 N32 C39 117(2) . . ? C31' N32 C29 121(2) . . ? C21' N32 C29 106(2) . . ? C38 N32 C29 112.6(19) . . ? C28 N32 C29 107.2(18) . . ? C39 N32 C29 12(2) . . ? C28 C38 N32 81(3) . . ? C28 C38 N22 67(3) . . ? N32 C38 N22 14.3(15) . . ? N22 C39 N32 15.4(16) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 1.836 _refine_diff_density_min -3.064 _refine_diff_density_rms 0.166 #========================================================================== data_[CuI(4-tertbutyl-piridine)]4, compound 3 in the Manuscript _audit_creation_method SHELXL-97 #========================================================================== # CHEMICAL DATA _chemical_name_systematic ; tetrakis((4-tertbutyl-pyridine)-iodide-copper(i)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 Cu4 I4 N4' _chemical_formula_sum 'C36 H52 Cu4 I4 N4' _chemical_formula_weight 1302.58 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #========================================================================== # CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.341(11) _cell_length_b 20.409(9) _cell_length_c 19.177(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9135(7) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4992 _exptl_absorpt_coefficient_mu 4.568 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3227 _exptl_absorpt_correction_T_max 0.8384 _exptl_absorpt_process_details ? #========================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 area detector' _diffrn_detector 'scintillation counter' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33473 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 17.23 _reflns_number_total 2764 _reflns_number_gt 2583 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2001)' #========================================================================== # DATA REFINEMENT _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^)+(0.0438P)^2^+88.0355P] 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 2764 _refine_ls_number_parameters 419 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.003 #========================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 I1 I 0.22336(4) 0.28504(4) -0.08161(5) 0.0660(4) Uani 1 1 d . . . I2 I 0.02702(4) 0.27558(4) -0.07735(5) 0.0657(4) Uani 1 1 d . . . I3 I 0.13025(5) 0.10535(5) -0.02499(6) 0.0832(4) Uani 1 1 d . . . I4 I 0.12511(5) 0.29612(5) 0.11666(5) 0.0766(4) Uani 1 1 d . . . Cu1 Cu 0.12665(8) 0.21628(9) -0.09900(9) 0.0718(6) Uani 1 1 d . . . Cu2 Cu 0.12499(8) 0.32332(9) -0.01872(9) 0.0765(6) Uani 1 1 d . . . Cu3 Cu 0.18303(9) 0.21681(10) 0.02686(10) 0.0868(7) Uani 1 1 d . . . Cu4 Cu 0.07212(9) 0.20721(9) 0.03018(10) 0.0843(7) Uani 1 1 d . . . N1 N 0.1311(8) 0.1871(6) -0.2008(6) 0.062(3) Uani 1 1 d . . . C11 C 0.1790(7) 0.1634(8) -0.2273(11) 0.071(4) Uani 1 1 d . . . H11 H 0.2112 0.1624 -0.1987 0.085 Uiso 1 1 calc R . . C12 C 0.1847(7) 0.1401(7) -0.2943(12) 0.064(4) Uani 1 1 d . . . H12 H 0.2202 0.1250 -0.3093 0.077 Uiso 1 1 calc R . . C13 C 0.1390(9) 0.1388(7) -0.3394(9) 0.058(4) Uani 1 1 d . . . C14 C 0.0897(8) 0.1650(8) -0.3134(10) 0.073(5) Uani 1 1 d . . . H14 H 0.0576 0.1680 -0.3418 0.087 Uiso 1 1 calc R . . C15 C 0.0869(7) 0.1869(7) -0.2461(12) 0.078(5) Uani 1 1 d . . . H15 H 0.0519 0.2029 -0.2304 0.094 Uiso 1 1 calc R . . C16 C 0.1406(8) 0.1142(8) -0.4135(8) 0.073(5) Uani 1 1 d . . . C17 C 0.1975(8) 0.0805(9) -0.4317(8) 0.115(6) Uani 1 1 d . . . H171 H 0.1966 0.0661 -0.4793 0.172 Uiso 1 1 calc R . . H172 H 0.2031 0.0435 -0.4016 0.172 Uiso 1 1 calc R . . H173 H 0.2285 0.1110 -0.4254 0.172 Uiso 1 1 calc R . . C18 C 0.0915(8) 0.0660(8) -0.4263(8) 0.106(6) Uani 1 1 d . . . H181 H 0.0929 0.0508 -0.4736 0.159 Uiso 1 1 calc R . . H182 H 0.0556 0.0875 -0.4179 0.159 Uiso 1 1 calc R . . H183 H 0.0953 0.0293 -0.3952 0.159 Uiso 1 1 calc R . . C19 C 0.1328(7) 0.1723(8) -0.4632(7) 0.090(5) Uani 1 1 d . . . H191 H 0.1340 0.1571 -0.5105 0.135 Uiso 1 1 calc R . . H192 H 0.1631 0.2034 -0.4558 0.135 Uiso 1 1 calc R . . H193 H 0.0966 0.1929 -0.4543 0.135 Uiso 1 1 calc R . . N2 N 0.1208(9) 0.4220(6) -0.0385(5) 0.064(3) Uani 1 1 d . . . C21 C 0.1678(8) 0.4579(12) -0.0547(9) 0.075(5) Uani 1 1 d . . . H21 H 0.2037 0.4387 -0.0498 0.090 Uiso 1 1 calc R . . C22 C 0.1648(8) 0.5201(11) -0.0774(8) 0.070(5) Uani 1 1 d . . . H22 H 0.1987 0.5425 -0.0865 0.085 Uiso 1 1 calc R . . C23 C 0.1139(11) 0.5518(8) -0.0879(7) 0.061(4) Uani 1 1 d . . . C24 C 0.0658(7) 0.5150(11) -0.0687(9) 0.076(5) Uani 1 1 d D . . H24 H 0.0296 0.5340 -0.0712 0.091 Uiso 1 1 calc R . . C25 C 0.0709(9) 0.4524(10) -0.0468(9) 0.083(5) Uani 1 1 d . . . H25 H 0.0376 0.4293 -0.0368 0.100 Uiso 1 1 calc R . . C26 C 0.1096(7) 0.6217(8) -0.1151(9) 0.075(4) Uani 1 1 d . . . C27 C 0.0975(10) 0.6671(8) -0.0555(9) 0.144(9) Uani 1 1 d . . . H271 H 0.0636 0.6528 -0.0315 0.216 Uiso 1 1 calc R . . H272 H 0.0917 0.7107 -0.0731 0.216 Uiso 1 1 calc R . . H273 H 0.1293 0.6670 -0.0239 0.216 Uiso 1 1 calc R . . C28 C 0.0612(8) 0.6266(8) -0.1686(9) 0.119(6) Uani 1 1 d . . . H281 H 0.0258 0.6133 -0.1474 0.179 Uiso 1 1 calc R . . H282 H 0.0695 0.5985 -0.2075 0.179 Uiso 1 1 calc R . . H283 H 0.0579 0.6710 -0.1845 0.179 Uiso 1 1 calc R . . C29 C 0.1639(8) 0.6422(8) -0.1543(10) 0.125(7) Uani 1 1 d . . . H291 H 0.1594 0.6860 -0.1716 0.187 Uiso 1 1 calc R . . H292 H 0.1703 0.6128 -0.1926 0.187 Uiso 1 1 calc R . . H293 H 0.1961 0.6405 -0.1232 0.187 Uiso 1 1 calc R . . N3 N 0.2468(6) 0.1753(8) 0.0818(8) 0.074(4) Uani 1 1 d . . . C31 C 0.2676(8) 0.2003(8) 0.1395(14) 0.098(6) Uani 1 1 d . . . H31 H 0.2526 0.2399 0.1549 0.118 Uiso 1 1 calc R . . C32 C 0.3089(10) 0.1726(11) 0.1776(10) 0.108(7) Uani 1 1 d . . . H32 H 0.3205 0.1936 0.2183 0.130 Uiso 1 1 calc R . . C33 C 0.3346(7) 0.1160(10) 0.1601(9) 0.071(4) Uani 1 1 d . . . C34 C 0.3122(10) 0.0873(10) 0.1010(12) 0.133(8) Uani 1 1 d . . . H34 H 0.3258 0.0470 0.0855 0.160 Uiso 1 1 calc R . . C35 C 0.2688(10) 0.1194(14) 0.0649(10) 0.146(10) Uani 1 1 d . . . H35 H 0.2545 0.0989 0.0253 0.176 Uiso 1 1 calc R . . C36 C 0.3810(7) 0.0802(8) 0.2017(8) 0.081(5) Uani 1 1 d . . . C37 C 0.3701(9) 0.0815(9) 0.2802(17) 0.137(6) Uiso 0.183(18) 1 d PD . . C37A C 0.4184(8) 0.1176(10) 0.2609(12) 0.137(6) Uiso 0.817(18) 1 d PD . . C38 C 0.431(5) 0.111(2) 0.190(2) 0.137(6) Uiso 0.183(18) 1 d PD . . C38A C 0.4294(10) 0.0520(12) 0.1542(13) 0.137(6) Uiso 0.817(18) 1 d PD . . C39 C 0.3763(12) 0.027(2) 0.175(2) 0.137(6) Uiso 0.183(18) 1 d PD . . C39A C 0.3461(10) 0.0340(9) 0.2368(12) 0.137(6) Uiso 0.817(18) 1 d PD . . N4 N 0.0111(5) 0.1640(9) 0.0907(7) 0.068(3) Uani 1 1 d . . . C41 C -0.0146(9) 0.1963(8) 0.1422(13) 0.100(6) Uani 1 1 d . . . H41 H -0.0032 0.2392 0.1510 0.120 Uiso 1 1 calc R . . C42 C -0.0573(9) 0.1699(11) 0.1830(9) 0.099(6) Uani 1 1 d . . . H42 H -0.0734 0.1947 0.2187 0.119 Uiso 1 1 calc R . . C43 C -0.0764(7) 0.1070(10) 0.1714(9) 0.066(4) Uani 1 1 d . . . C44 C -0.0483(9) 0.0752(8) 0.1193(11) 0.074(5) Uani 1 1 d . . . H44 H -0.0586 0.0322 0.1092 0.089 Uiso 1 1 calc R . . C45 C -0.0052(8) 0.1038(11) 0.0807(8) 0.082(5) Uani 1 1 d . . . H45 H 0.0129 0.0791 0.0463 0.098 Uiso 1 1 calc R . . C46 C -0.1247(5) 0.0752(5) 0.2134(7) 0.081(5) Uani 1 1 d D . . C47 C -0.1798(10) 0.1167(12) 0.2052(15) 0.122(5) Uiso 0.250(15) 1 d PD . . C47A C -0.1746(8) 0.0579(9) 0.1635(11) 0.122(5) Uiso 0.750(15) 1 d PD . . C48 C -0.1437(15) 0.0045(8) 0.196(2) 0.122(5) Uiso 0.250(15) 1 d PD . . C48A C -0.0994(10) 0.0131(9) 0.2479(11) 0.122(5) Uiso 0.750(15) 1 d PD . . C49 C -0.112(3) 0.0686(18) 0.2924(11) 0.122(5) Uiso 0.250(15) 1 d PD . . C49A C -0.1483(9) 0.1222(10) 0.2700(10) 0.122(5) Uiso 0.750(15) 1 d PD . . 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 I1 0.0708(7) 0.0652(7) 0.0620(7) -0.0017(5) 0.0007(5) -0.0025(5) I2 0.0666(7) 0.0690(7) 0.0615(7) 0.0016(5) -0.0016(5) 0.0037(5) I3 0.1098(9) 0.0523(7) 0.0874(8) 0.0024(6) 0.0076(7) 0.0042(6) I4 0.1029(9) 0.0767(8) 0.0502(7) -0.0030(5) 0.0005(6) 0.0005(6) Cu1 0.0857(14) 0.0780(14) 0.0517(12) -0.0112(9) -0.0038(10) 0.0023(10) Cu2 0.1029(15) 0.0591(13) 0.0674(13) 0.0040(10) -0.0010(11) 0.0038(11) Cu3 0.0892(15) 0.0980(16) 0.0733(14) 0.0185(11) -0.0145(12) 0.0152(12) Cu4 0.0971(16) 0.0763(14) 0.0796(14) 0.0144(11) 0.0146(12) -0.0039(11) N1 0.065(9) 0.071(8) 0.050(9) -0.004(7) -0.001(11) 0.014(8) C11 0.041(13) 0.098(12) 0.074(16) -0.024(10) -0.011(10) 0.016(9) C12 0.054(14) 0.070(11) 0.069(14) -0.015(10) 0.007(13) 0.014(8) C13 0.056(12) 0.055(10) 0.063(16) 0.003(9) 0.004(14) 0.012(9) C14 0.094(18) 0.098(13) 0.026(12) -0.012(9) -0.020(11) 0.005(12) C15 0.054(12) 0.103(13) 0.079(16) -0.004(12) -0.022(13) 0.017(9) C16 0.129(16) 0.062(11) 0.026(11) 0.000(9) 0.001(10) 0.005(12) C17 0.139(17) 0.132(16) 0.074(12) -0.029(11) 0.010(12) 0.059(14) C18 0.173(18) 0.087(13) 0.057(11) -0.006(10) 0.000(11) -0.032(14) C19 0.125(15) 0.083(13) 0.063(11) -0.001(10) -0.002(10) 0.005(10) N2 0.088(11) 0.052(9) 0.052(8) 0.007(6) 0.003(8) 0.004(12) C21 0.063(15) 0.073(17) 0.088(12) -0.005(11) -0.014(10) -0.005(13) C22 0.079(17) 0.037(13) 0.095(13) -0.006(10) -0.001(10) -0.019(12) C23 0.089(16) 0.039(14) 0.054(10) -0.012(8) 0.003(10) 0.019(15) C24 0.050(13) 0.070(15) 0.109(13) 0.004(11) 0.019(10) 0.015(13) C25 0.086(18) 0.043(14) 0.121(15) 0.026(10) 0.026(11) 0.011(12) C26 0.080(13) 0.056(14) 0.090(13) 0.000(11) 0.009(11) 0.006(10) C27 0.27(3) 0.045(11) 0.116(15) -0.038(12) 0.034(17) 0.025(14) C28 0.164(19) 0.067(12) 0.126(16) 0.002(11) -0.004(16) 0.028(12) C29 0.136(17) 0.084(13) 0.155(18) 0.015(13) 0.026(15) -0.017(12) N3 0.085(10) 0.086(11) 0.052(9) 0.021(8) -0.017(9) 0.023(10) C31 0.083(15) 0.068(12) 0.14(2) 0.005(15) -0.063(13) 0.027(11) C32 0.125(17) 0.072(14) 0.127(17) -0.041(14) -0.063(15) 0.030(13) C33 0.082(13) 0.088(15) 0.043(12) 0.005(11) 0.006(11) -0.004(13) C34 0.16(2) 0.130(17) 0.108(17) -0.043(16) -0.047(16) 0.094(16) C35 0.16(2) 0.17(2) 0.104(17) -0.059(17) -0.054(15) 0.118(19) C36 0.079(11) 0.081(11) 0.082(12) 0.037(10) -0.004(10) -0.003(10) N4 0.093(10) 0.044(10) 0.067(10) 0.009(8) 0.003(9) -0.006(9) C41 0.131(17) 0.046(11) 0.125(16) -0.019(14) 0.048(14) -0.006(13) C42 0.126(16) 0.067(17) 0.105(15) -0.007(13) 0.061(14) -0.003(12) C43 0.096(13) 0.047(14) 0.053(12) 0.001(10) -0.008(12) 0.000(12) C44 0.103(14) 0.056(11) 0.064(12) -0.008(13) -0.010(11) -0.019(13) C45 0.109(15) 0.065(16) 0.072(13) -0.013(11) 0.022(12) -0.023(12) C46 0.101(13) 0.075(11) 0.068(11) -0.003(9) 0.029(10) -0.014(10) #========================================================================== # MOLECULAR GEOMETRY _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 I1 Cu3 2.674(2) . ? I1 Cu1 2.679(2) . ? I1 Cu2 2.708(2) . ? I2 Cu1 2.654(2) . ? I2 Cu4 2.703(2) . ? I2 Cu2 2.728(2) . ? I3 Cu1 2.673(2) . ? I3 Cu4 2.699(2) . ? I3 Cu3 2.771(2) . ? I4 Cu2 2.655(2) . ? I4 Cu3 2.723(2) . ? I4 Cu4 2.752(2) . ? Cu1 N1 2.044(12) . ? Cu1 Cu2 2.673(3) . ? Cu1 Cu3 2.749(3) . ? Cu1 Cu4 2.791(3) . ? Cu2 N2 2.052(12) . ? Cu2 Cu3 2.706(3) . ? Cu2 Cu4 2.832(3) . ? Cu3 N3 2.010(13) . ? Cu3 Cu4 2.597(3) . ? Cu4 N4 2.038(12) . ? N1 C11 1.321(16) . ? N1 C15 1.347(17) . ? C11 C12 1.376(18) . ? C12 C13 1.374(17) . ? C13 C14 1.363(18) . ? C13 C16 1.51(2) . ? C14 C15 1.367(18) . ? C16 C18 1.53(2) . ? C16 C19 1.532(19) . ? C16 C17 1.54(2) . ? N2 C25 1.329(17) . ? N2 C21 1.356(18) . ? C21 C22 1.344(19) . ? C22 C23 1.366(19) . ? C23 C24 1.401(18) . ? C23 C26 1.52(2) . ? C24 C25 1.350(19) . ? C26 C27 1.50(2) . ? C26 C28 1.53(2) . ? C26 C29 1.53(2) . ? N3 C35 1.29(2) . ? N3 C31 1.311(19) . ? C31 C32 1.33(2) . ? C32 C33 1.35(2) . ? C33 C34 1.38(2) . ? C33 C36 1.53(2) . ? C34 C35 1.39(2) . ? C36 C39 1.21(6) . ? C36 C38 1.35(9) . ? C36 C39A 1.42(3) . ? C36 C37 1.53(4) . ? C36 C38A 1.56(3) . ? C36 C37A 1.62(3) . ? C37 C39A 1.395(18) . ? C37 C37A 1.395(18) . ? C37A C38 1.395(18) . ? C38 C38A 1.395(18) . ? C38A C39 1.395(18) . ? C39 C39A 1.395(18) . ? N4 C45 1.301(17) . ? N4 C41 1.330(18) . ? C41 C42 1.38(2) . ? C42 C43 1.377(19) . ? C43 C44 1.361(19) . ? C43 C46 1.530(19) . ? C44 C45 1.378(19) . ? C46 C49 1.548(12) . ? C46 C49A 1.548(12) . ? C46 C47 1.548(12) . ? C46 C47A 1.548(12) . ? C46 C48 1.548(12) . ? C46 C48A 1.548(12) . ? C47 C49A 1.448(12) . ? C47 C47A 1.448(12) . ? C47A C48 1.448(12) . ? C48 C48A 1.448(12) . ? C48A C49 1.448(12) . ? C49 C49A 1.448(12) . ? 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 Cu3 I1 Cu1 61.80(6) . . ? Cu3 I1 Cu2 60.36(6) . . ? Cu1 I1 Cu2 59.49(6) . . ? Cu1 I2 Cu4 62.79(6) . . ? Cu1 I2 Cu2 59.53(6) . . ? Cu4 I2 Cu2 62.84(6) . . ? Cu1 I3 Cu4 62.61(6) . . ? Cu1 I3 Cu3 60.61(6) . . ? Cu4 I3 Cu3 56.67(7) . . ? Cu2 I4 Cu3 60.41(6) . . ? Cu2 I4 Cu4 63.13(6) . . ? Cu3 I4 Cu4 56.63(7) . . ? N1 Cu1 I2 109.0(5) . . ? N1 Cu1 Cu2 142.1(3) . . ? I2 Cu1 Cu2 61.61(6) . . ? N1 Cu1 I3 105.0(3) . . ? I2 Cu1 I3 109.31(7) . . ? Cu2 Cu1 I3 112.76(8) . . ? N1 Cu1 I1 103.2(4) . . ? I2 Cu1 I1 118.68(8) . . ? Cu2 Cu1 I1 60.81(6) . . ? I3 Cu1 I1 110.56(7) . . ? N1 Cu1 Cu3 144.7(5) . . ? I2 Cu1 Cu3 106.27(8) . . ? Cu2 Cu1 Cu3 59.87(7) . . ? I3 Cu1 Cu3 61.46(6) . . ? I1 Cu1 Cu3 59.02(6) . . ? N1 Cu1 Cu4 148.4(4) . . ? I2 Cu1 Cu4 59.46(6) . . ? Cu2 Cu1 Cu4 62.38(7) . . ? I3 Cu1 Cu4 59.14(6) . . ? I1 Cu1 Cu4 107.97(8) . . ? Cu3 Cu1 Cu4 55.90(8) . . ? N2 Cu2 I4 112.7(3) . . ? N2 Cu2 Cu1 134.1(3) . . ? I4 Cu2 Cu1 113.10(8) . . ? N2 Cu2 Cu3 150.7(6) . . ? I4 Cu2 Cu3 61.03(6) . . ? Cu1 Cu2 Cu3 61.47(7) . . ? N2 Cu2 I1 104.0(5) . . ? I4 Cu2 I1 111.98(7) . . ? Cu1 Cu2 I1 59.70(6) . . ? Cu3 Cu2 I1 59.20(6) . . ? N2 Cu2 I2 103.6(5) . . ? I4 Cu2 I2 109.22(7) . . ? Cu1 Cu2 I2 58.86(6) . . ? Cu3 Cu2 I2 105.41(8) . . ? I1 Cu2 I2 115.09(8) . . ? N2 Cu2 Cu4 149.5(6) . . ? I4 Cu2 Cu4 60.10(6) . . ? Cu1 Cu2 Cu4 60.86(7) . . ? Cu3 Cu2 Cu4 55.87(7) . . ? I1 Cu2 Cu4 106.00(8) . . ? I2 Cu2 Cu4 58.15(6) . . ? N3 Cu3 Cu4 133.9(4) . . ? N3 Cu3 I1 111.5(4) . . ? Cu4 Cu3 I1 114.16(8) . . ? N3 Cu3 Cu2 151.4(6) . . ? Cu4 Cu3 Cu2 64.51(7) . . ? I1 Cu3 Cu2 60.44(6) . . ? N3 Cu3 I4 106.6(5) . . ? Cu4 Cu3 I4 62.25(7) . . ? I1 Cu3 I4 110.93(8) . . ? Cu2 Cu3 I4 58.55(6) . . ? N3 Cu3 Cu1 144.4(6) . . ? Cu4 Cu3 Cu1 62.88(7) . . ? I1 Cu3 Cu1 59.18(6) . . ? Cu2 Cu3 Cu1 58.67(6) . . ? I4 Cu3 Cu1 108.66(8) . . ? N3 Cu3 I3 99.9(5) . . ? Cu4 Cu3 I3 60.25(7) . . ? I1 Cu3 I3 107.74(8) . . ? Cu2 Cu3 I3 108.72(8) . . ? I4 Cu3 I3 119.62(8) . . ? Cu1 Cu3 I3 57.93(6) . . ? N4 Cu4 Cu3 138.0(3) . . ? N4 Cu4 I3 103.9(5) . . ? Cu3 Cu4 I3 63.08(7) . . ? N4 Cu4 I2 112.7(3) . . ? Cu3 Cu4 I2 109.30(8) . . ? I3 Cu4 I2 107.12(8) . . ? N4 Cu4 I4 104.8(5) . . ? Cu3 Cu4 I4 61.12(7) . . ? I3 Cu4 I4 121.22(8) . . ? I2 Cu4 I4 107.12(8) . . ? N4 Cu4 Cu1 148.5(5) . . ? Cu3 Cu4 Cu1 61.23(7) . . ? I3 Cu4 Cu1 58.25(6) . . ? I2 Cu4 Cu1 57.74(6) . . ? I4 Cu4 Cu1 106.63(8) . . ? N4 Cu4 Cu2 148.8(5) . . ? Cu3 Cu4 Cu2 59.62(7) . . ? I3 Cu4 Cu2 107.20(8) . . ? I2 Cu4 Cu2 59.01(6) . . ? I4 Cu4 Cu2 56.76(6) . . ? Cu1 Cu4 Cu2 56.76(6) . . ? C11 N1 C15 113.5(12) . . ? C11 N1 Cu1 121.1(14) . . ? C15 N1 Cu1 125.3(15) . . ? N1 C11 C12 124.5(13) . . ? C13 C12 C11 121.4(13) . . ? C14 C13 C12 114.6(14) . . ? C14 C13 C16 119.8(18) . . ? C12 C13 C16 125.5(18) . . ? C13 C14 C15 121.0(14) . . ? N1 C15 C14 124.9(14) . . ? C13 C16 C18 110.3(13) . . ? C13 C16 C19 108.9(12) . . ? C18 C16 C19 108.1(13) . . ? C13 C16 C17 112.5(14) . . ? C18 C16 C17 108.9(14) . . ? C19 C16 C17 107.9(13) . . ? C25 N2 C21 115.4(13) . . ? C25 N2 Cu2 121.5(15) . . ? C21 N2 Cu2 122.3(16) . . ? C22 C21 N2 122.7(15) . . ? C21 C22 C23 122.8(15) . . ? C22 C23 C24 113.8(13) . . ? C22 C23 C26 124(2) . . ? C24 C23 C26 123(2) . . ? C25 C24 C23 121.2(14) . . ? N2 C25 C24 123.9(15) . . ? C27 C26 C23 109.4(13) . . ? C27 C26 C28 109.3(14) . . ? C23 C26 C28 109.9(14) . . ? C27 C26 C29 111.2(15) . . ? C23 C26 C29 111.7(14) . . ? C28 C26 C29 105.3(15) . . ? C35 N3 C31 113.9(15) . . ? C35 N3 Cu3 122.4(16) . . ? C31 N3 Cu3 123.6(15) . . ? N3 C31 C32 124.5(17) . . ? C31 C32 C33 123.2(17) . . ? C32 C33 C34 113.7(15) . . ? C32 C33 C36 126.6(18) . . ? C34 C33 C36 119.6(19) . . ? C33 C34 C35 119.0(16) . . ? N3 C35 C34 125.6(18) . . ? C39 C36 C38 116(2) . . ? C39 C36 C39A 63.6(10) . . ? C38 C36 C39A 153(4) . . ? C39 C36 C37 115.2(17) . . ? C38 C36 C37 107(2) . . ? C39A C36 C37 56.4(9) . . ? C39 C36 C33 98(2) . . ? C38 C36 C33 108(4) . . ? C39A C36 C33 99.1(13) . . ? C37 C36 C33 112.7(15) . . ? C39 C36 C38A 58.9(10) . . ? C38 C36 C38A 56.7(15) . . ? C39A C36 C38A 116.7(16) . . ? C37 C36 C38A 134.6(16) . . ? C33 C36 C38A 112.6(14) . . ? C39 C36 C37A 141(2) . . ? C38 C36 C37A 55.1(13) . . ? C39A C36 C37A 106.8(15) . . ? C37 C36 C37A 52.5(8) . . ? C33 C36 C37A 121.4(14) . . ? C38A C36 C37A 101.1(14) . . ? C39A C37 C37A 122(3) . . ? C39A C37 C36 57.8(16) . . ? C37A C37 C36 67.3(17) . . ? C37 C37A C38 112(4) . . ? C37 C37A C36 60.2(16) . . ? C38 C37A C36 52(4) . . ? C36 C38 C38A 69(3) . . ? C36 C38 C37A 72(3) . . ? C38A C38 C37A 124(4) . . ? C39 C38A C38 102(5) . . ? C39 C38A C36 48(2) . . ? C38 C38A C36 54(4) . . ? C36 C39 C38A 73(3) . . ? C36 C39 C39A 65(2) . . ? C38A C39 C39A 131(5) . . ? C37 C39A C39 112(4) . . ? C37 C39A C36 65.8(18) . . ? C39 C39A C36 51(2) . . ? C45 N4 C41 116.5(14) . . ? C45 N4 Cu4 121.9(16) . . ? C41 N4 Cu4 121.5(15) . . ? N4 C41 C42 123.6(15) . . ? C43 C42 C41 120.5(15) . . ? C44 C43 C42 114.0(15) . . ? C44 C43 C46 122.7(18) . . ? C42 C43 C46 123.3(19) . . ? C43 C44 C45 123.0(14) . . ? N4 C45 C44 122.2(15) . . ? C43 C46 C49 114(3) . . ? C43 C46 C49A 111.6(14) . . ? C49 C46 C49A 55.8(3) . . ? C43 C46 C47 109.0(17) . . ? C49 C46 C47 107.8(15) . . ? C49A C46 C47 55.8(3) . . ? C43 C46 C47A 108.9(13) . . ? C49 C46 C47A 137(3) . . ? C49A C46 C47A 107.9(10) . . ? C47 C46 C47A 55.8(3) . . ? C43 C46 C48 119(2) . . ? C49 C46 C48 101(2) . . ? C49A C46 C48 129(2) . . ? C47 C46 C48 104.5(14) . . ? C47A C46 C48 55.8(3) . . ? C43 C46 C48A 107.0(13) . . ? C49 C46 C48A 55.8(3) . . ? C49A C46 C48A 110.1(9) . . ? C47 C46 C48A 144(2) . . ? C47A C46 C48A 111.4(7) . . ? C48 C46 C48A 55.8(3) . . ? C49A C47 C47A 119.6(9) . . ? C49A C47 C46 62.12(15) . . ? C47A C47 C46 62.12(15) . . ? C48 C47A C47 115.5(15) . . ? C48 C47A C46 62.12(15) . . ? C47 C47A C46 62.12(15) . . ? C48A C48 C47A 124.0(3) . . ? C48A C48 C46 62.12(15) . . ? C47A C48 C46 62.12(16) . . ? C48 C48A C49 111(2) . . ? C48 C48A C46 62.12(15) . . ? C49 C48A C46 62.12(16) . . ? C49A C49 C48A 122.4(10) . . ? C49A C49 C46 62.12(15) . . ? C48A C49 C46 62.12(16) . . ? C49 C49A C47 119.5(14) . . ? C49 C49A C46 62.12(16) . . ? C47 C49A C46 62.12(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 17.23 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.857 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.082 #========================================================================== data_[CuI(4-dimethylaminopyridine)]6, compound 4 in the Manuscript _audit_creation_method SHELXL-97 #========================================================================== # CHEMICAL DATA _chemical_name_systematic ; hexakis(4-dimethylaminopyridine-iodide-copper(i)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H30 Cu3 I3 N6' _chemical_formula_sum 'C21 H30 Cu3 I3 N6' _chemical_formula_weight 937.83 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #========================================================================== # CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 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 14.061(6) _cell_length_b 11.917(5) _cell_length_c 17.848(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.580(10) _cell_angle_gamma 90.00 _cell_volume 2881(2) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 5.430 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3557 _exptl_absorpt_correction_T_max 0.6127 _exptl_absorpt_process_details ? #========================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _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 area detector' _diffrn_detector 'scintillation counter' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32431 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 30.68 _reflns_number_total 8140 _reflns_number_gt 4479 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2001)' #========================================================================== # DATA REFINEMENT _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^)+(0.0267P)^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 8140 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.003 #========================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cu1 Cu 0.31740(4) -0.13713(4) 0.10553(3) 0.05415(13) Uani 1 1 d . . . Cu2 Cu 0.21651(4) 0.02459(4) 0.14547(3) 0.06014(14) Uani 1 1 d . . . Cu3 Cu 0.09177(5) -0.07345(4) 0.00110(3) 0.07253(17) Uani 1 1 d . . . I1 I 0.33424(2) -0.11503(2) 0.250077(14) 0.06260(9) Uani 1 1 d . . . I2 I 0.270293(19) 0.02092(2) 0.007393(14) 0.05020(7) Uani 1 1 d . . . I3 I 0.028908(18) -0.03361(2) 0.125438(14) 0.05176(7) Uani 1 1 d . . . N11 N 0.3556(2) -0.2872(2) 0.07540(16) 0.0449(7) Uani 1 1 d . . . C11 C 0.3448(3) -0.3177(3) 0.0010(2) 0.0491(9) Uani 1 1 d . . . H11 H 0.3276 -0.2621 -0.0368 0.059 Uiso 1 1 calc R . . C12 C 0.3573(3) -0.4240(3) -0.0230(2) 0.0454(9) Uani 1 1 d . . . H12 H 0.3480 -0.4389 -0.0757 0.055 Uiso 1 1 calc R . . C13 C 0.3844(2) -0.5113(3) 0.03198(19) 0.0398(8) Uani 1 1 d . . . C14 C 0.3969(3) -0.4794(3) 0.11015(19) 0.0439(8) Uani 1 1 d . . . H14 H 0.4152 -0.5325 0.1496 0.053 Uiso 1 1 calc R . . C15 C 0.3820(3) -0.3707(3) 0.1277(2) 0.0474(9) Uani 1 1 d . . . H15 H 0.3909 -0.3527 0.1799 0.057 Uiso 1 1 calc R . . N12 N 0.3963(2) -0.6190(2) 0.01116(16) 0.0477(7) Uani 1 1 d . . . C16 C 0.3779(3) -0.6529(3) -0.0702(2) 0.0602(11) Uani 1 1 d . . . H161 H 0.3897 -0.7320 -0.0728 0.072 Uiso 1 1 calc R . . H162 H 0.4212 -0.6125 -0.0938 0.072 Uiso 1 1 calc R . . H163 H 0.3105 -0.6367 -0.0973 0.072 Uiso 1 1 calc R . . C17 C 0.4295(3) -0.7062(3) 0.0688(2) 0.0577(10) Uani 1 1 d . . . H171 H 0.4324 -0.7764 0.0431 0.069 Uiso 1 1 calc R . . H172 H 0.3841 -0.7124 0.1003 0.069 Uiso 1 1 calc R . . H173 H 0.4939 -0.6877 0.1012 0.069 Uiso 1 1 calc R . . N21 N 0.2474(2) 0.1784(2) 0.19395(16) 0.0446(7) Uani 1 1 d . . . C21 C 0.1778(3) 0.2567(3) 0.1898(2) 0.0494(9) Uani 1 1 d . . . H21 H 0.1133 0.2383 0.1630 0.059 Uiso 1 1 calc R . . C22 C 0.1942(3) 0.3620(3) 0.2220(2) 0.0512(9) Uani 1 1 d . . . H22 H 0.1419 0.4117 0.2173 0.061 Uiso 1 1 calc R . . C23 C 0.2909(3) 0.3941(3) 0.26229(19) 0.0456(9) Uani 1 1 d . . . C24 C 0.3638(3) 0.3125(3) 0.2669(2) 0.0477(9) Uani 1 1 d . . . H24 H 0.4290 0.3280 0.2933 0.057 Uiso 1 1 calc R . . C25 C 0.3393(3) 0.2100(3) 0.2325(2) 0.0490(9) Uani 1 1 d . . . H25 H 0.3899 0.1583 0.2361 0.059 Uiso 1 1 calc R . . N22 N 0.3103(3) 0.4985(3) 0.29335(19) 0.0604(9) Uani 1 1 d . . . C26 C 0.4089(4) 0.5290(4) 0.3380(3) 0.0791(14) Uani 1 1 d . . . H261 H 0.4089 0.6051 0.3556 0.095 Uiso 1 1 calc R . . H262 H 0.4535 0.5223 0.3058 0.095 Uiso 1 1 calc R . . H263 H 0.4297 0.4800 0.3820 0.095 Uiso 1 1 calc R . . C27 C 0.2314(4) 0.5796(3) 0.2891(3) 0.0768(14) Uani 1 1 d . . . H271 H 0.2589 0.6480 0.3143 0.092 Uiso 1 1 calc R . . H272 H 0.1849 0.5496 0.3145 0.092 Uiso 1 1 calc R . . H273 H 0.1985 0.5947 0.2355 0.092 Uiso 1 1 calc R . . N31 N 0.0978(2) -0.2390(2) -0.02371(18) 0.0462(7) Uani 1 1 d . . . C31 C 0.0870(3) -0.2774(3) -0.0960(2) 0.0496(9) Uani 1 1 d . . . H31 H 0.0758 -0.2250 -0.1360 0.059 Uiso 1 1 calc R . . C32 C 0.0912(3) -0.3886(3) -0.1155(2) 0.0466(9) Uani 1 1 d . . . H32 H 0.0826 -0.4087 -0.1673 0.056 Uiso 1 1 calc R . . C33 C 0.1084(2) -0.4718(3) -0.0578(2) 0.0424(8) Uani 1 1 d . . . C34 C 0.1201(3) -0.4313(3) 0.0185(2) 0.0472(9) Uani 1 1 d . . . H34 H 0.1317 -0.4814 0.0599 0.057 Uiso 1 1 calc R . . C35 C 0.1144(3) -0.3186(3) 0.0318(2) 0.0487(9) Uani 1 1 d . . . H35 H 0.1226 -0.2954 0.0829 0.058 Uiso 1 1 calc R . . N32 N 0.1139(2) -0.5825(2) -0.07403(19) 0.0555(8) Uani 1 1 d . . . C36 C 0.0940(4) -0.6220(4) -0.1535(3) 0.0834(14) Uani 1 1 d . . . H361 H 0.1021 -0.7020 -0.1536 0.100 Uiso 1 1 calc R . . H362 H 0.1393 -0.5873 -0.1782 0.100 Uiso 1 1 calc R . . H363 H 0.0276 -0.6029 -0.1813 0.100 Uiso 1 1 calc R . . C37 C 0.1372(3) -0.6657(3) -0.0119(3) 0.0652(11) Uani 1 1 d . . . H371 H 0.1388 -0.7390 -0.0338 0.078 Uiso 1 1 calc R . . H372 H 0.0877 -0.6638 0.0161 0.078 Uiso 1 1 calc R . . H373 H 0.2005 -0.6490 0.0230 0.078 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 0.0572(3) 0.0474(3) 0.0566(3) 0.0001(2) 0.0130(2) 0.0049(2) Cu2 0.0660(3) 0.0458(3) 0.0649(3) -0.0103(2) 0.0112(3) 0.0003(2) Cu3 0.0955(5) 0.0467(3) 0.0818(4) -0.0098(3) 0.0349(3) -0.0101(3) I1 0.0840(2) 0.05313(15) 0.04060(14) 0.00022(12) -0.00065(13) 0.01203(14) I2 0.05637(16) 0.04663(14) 0.04757(14) 0.00283(11) 0.01388(12) -0.00687(12) I3 0.05082(16) 0.05191(15) 0.05137(15) -0.00388(12) 0.01167(12) -0.00265(12) N11 0.0473(19) 0.0477(17) 0.0406(17) 0.0039(14) 0.0132(14) 0.0063(14) C11 0.047(2) 0.055(2) 0.047(2) 0.0113(18) 0.0155(18) 0.0056(18) C12 0.046(2) 0.058(2) 0.0352(19) 0.0024(17) 0.0160(17) 0.0016(18) C13 0.0307(18) 0.050(2) 0.0409(19) 0.0001(16) 0.0131(15) -0.0019(15) C14 0.051(2) 0.045(2) 0.0357(19) 0.0051(16) 0.0115(16) 0.0052(18) C15 0.052(2) 0.054(2) 0.0353(19) 0.0016(17) 0.0106(17) 0.0053(18) N12 0.052(2) 0.0530(18) 0.0387(17) -0.0040(14) 0.0141(14) -0.0006(15) C16 0.062(3) 0.067(3) 0.055(2) -0.015(2) 0.020(2) -0.009(2) C17 0.068(3) 0.044(2) 0.060(2) -0.0031(19) 0.015(2) -0.003(2) N21 0.049(2) 0.0411(16) 0.0433(17) -0.0011(13) 0.0120(15) -0.0026(15) C21 0.045(2) 0.046(2) 0.054(2) -0.0011(18) 0.0075(18) -0.0023(18) C22 0.048(2) 0.042(2) 0.063(2) -0.0017(18) 0.014(2) 0.0016(18) C23 0.064(3) 0.041(2) 0.0378(19) 0.0007(16) 0.0229(18) -0.0089(19) C24 0.045(2) 0.049(2) 0.048(2) 0.0030(17) 0.0116(18) -0.0100(18) C25 0.046(2) 0.050(2) 0.053(2) 0.0048(18) 0.0161(19) 0.0023(18) N22 0.072(2) 0.0503(19) 0.063(2) -0.0142(16) 0.0234(18) -0.0145(17) C26 0.100(4) 0.070(3) 0.070(3) -0.017(2) 0.025(3) -0.027(3) C27 0.099(4) 0.047(2) 0.089(3) -0.015(2) 0.034(3) -0.002(2) N31 0.0473(19) 0.0398(16) 0.0524(18) -0.0004(15) 0.0152(15) -0.0053(14) C31 0.048(2) 0.045(2) 0.055(2) 0.0081(18) 0.0120(19) -0.0005(17) C32 0.045(2) 0.049(2) 0.045(2) -0.0008(17) 0.0095(17) 0.0040(18) C33 0.032(2) 0.045(2) 0.051(2) 0.0032(18) 0.0125(16) 0.0032(16) C34 0.046(2) 0.048(2) 0.051(2) 0.0094(17) 0.0175(18) 0.0020(17) C35 0.043(2) 0.054(2) 0.051(2) -0.0054(19) 0.0158(18) -0.0033(18) N32 0.065(2) 0.0395(17) 0.064(2) 0.0018(16) 0.0205(18) 0.0074(16) C36 0.106(4) 0.059(3) 0.085(3) -0.022(3) 0.024(3) 0.004(3) C37 0.057(3) 0.048(2) 0.092(3) 0.011(2) 0.021(2) 0.004(2) #========================================================================== # MOLECULAR GEOMETRY _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 N11 1.983(3) . ? Cu1 I2 2.5358(9) . ? Cu1 I1 2.5403(11) . ? Cu1 Cu2 2.6033(10) . ? Cu2 N21 2.024(3) . ? Cu2 I3 2.6572(12) . ? Cu2 I1 2.7082(9) . ? Cu2 I2 2.7654(11) . ? Cu2 Cu3 2.9416(11) . ? Cu3 N31 2.029(3) . ? Cu3 I3 2.6430(10) . ? Cu3 I2 2.7252(12) . ? Cu3 I3 2.7476(10) 3 ? I3 Cu3 2.7476(10) 3 ? N11 C11 1.345(4) . ? N11 C15 1.346(4) . ? C11 C12 1.364(5) . ? C12 C13 1.410(5) . ? C13 N12 1.359(4) . ? C13 C14 1.411(5) . ? C14 C15 1.363(5) . ? N12 C17 1.449(4) . ? N12 C16 1.461(4) . ? N21 C21 1.340(4) . ? N21 C25 1.344(4) . ? C21 C22 1.374(5) . ? C22 C23 1.410(5) . ? C23 N22 1.359(4) . ? C23 C24 1.400(5) . ? C24 C25 1.369(5) . ? N22 C26 1.448(5) . ? N22 C27 1.458(5) . ? N31 C31 1.339(4) . ? N31 C35 1.346(4) . ? C31 C32 1.375(5) . ? C32 C33 1.404(5) . ? C33 N32 1.357(4) . ? C33 C34 1.412(5) . ? C34 C35 1.371(5) . ? N32 C36 1.448(5) . ? N32 C37 1.457(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Cu1 I2 121.48(9) . . ? N11 Cu1 I1 114.25(8) . . ? I2 Cu1 I1 124.08(3) . . ? N11 Cu1 Cu2 161.64(9) . . ? I2 Cu1 Cu2 65.09(3) . . ? I1 Cu1 Cu2 63.527(19) . . ? N21 Cu2 Cu1 135.86(9) . . ? N21 Cu2 I3 112.64(9) . . ? Cu1 Cu2 I3 111.36(3) . . ? N21 Cu2 I1 103.92(9) . . ? Cu1 Cu2 I1 57.10(3) . . ? I3 Cu2 I1 109.47(3) . . ? N21 Cu2 I2 108.47(8) . . ? Cu1 Cu2 I2 56.274(19) . . ? I3 Cu2 I2 112.04(2) . . ? I1 Cu2 I2 109.99(3) . . ? N21 Cu2 Cu3 138.01(8) . . ? Cu1 Cu2 Cu3 72.95(3) . . ? I3 Cu2 Cu3 56.06(2) . . ? I1 Cu2 Cu3 118.04(3) . . ? I2 Cu2 Cu3 56.95(3) . . ? N31 Cu3 I3 113.64(9) . . ? N31 Cu3 I2 108.55(8) . . ? I3 Cu3 I2 113.79(3) . . ? N31 Cu3 I3 108.97(9) . 3 ? I3 Cu3 I3 109.56(3) . 3 ? I2 Cu3 I3 101.59(3) . 3 ? N31 Cu3 Cu2 121.82(9) . . ? I3 Cu3 Cu2 56.52(3) . . ? I2 Cu3 Cu2 58.27(2) . . ? I3 Cu3 Cu2 128.82(3) 3 . ? Cu1 I1 Cu2 59.37(2) . . ? Cu1 I2 Cu3 77.81(3) . . ? Cu1 I2 Cu2 58.63(2) . . ? Cu3 I2 Cu2 64.78(2) . . ? Cu3 I3 Cu2 67.42(2) . . ? Cu3 I3 Cu3 70.44(3) . 3 ? Cu2 I3 Cu3 111.16(3) . 3 ? C11 N11 C15 115.0(3) . . ? C11 N11 Cu1 123.0(2) . . ? C15 N11 Cu1 121.5(2) . . ? N11 C11 C12 124.9(3) . . ? C11 C12 C13 119.9(3) . . ? N12 C13 C12 122.4(3) . . ? N12 C13 C14 122.2(3) . . ? C12 C13 C14 115.4(3) . . ? C15 C14 C13 119.8(3) . . ? N11 C15 C14 125.0(3) . . ? C13 N12 C17 121.6(3) . . ? C13 N12 C16 122.1(3) . . ? C17 N12 C16 116.3(3) . . ? C21 N21 C25 114.9(3) . . ? C21 N21 Cu2 122.5(2) . . ? C25 N21 Cu2 122.6(2) . . ? N21 C21 C22 125.1(3) . . ? C21 C22 C23 119.5(3) . . ? N22 C23 C24 123.3(4) . . ? N22 C23 C22 121.1(3) . . ? C24 C23 C22 115.6(3) . . ? C25 C24 C23 120.1(3) . . ? N21 C25 C24 124.8(3) . . ? C23 N22 C26 120.8(4) . . ? C23 N22 C27 121.3(3) . . ? C26 N22 C27 117.7(3) . . ? C31 N31 C35 114.9(3) . . ? C31 N31 Cu3 122.8(2) . . ? C35 N31 Cu3 122.2(2) . . ? N31 C31 C32 124.9(3) . . ? C31 C32 C33 120.4(3) . . ? N32 C33 C32 122.6(3) . . ? N32 C33 C34 122.7(3) . . ? C32 C33 C34 114.7(3) . . ? C35 C34 C33 120.4(3) . . ? N31 C35 C34 124.7(3) . . ? C33 N32 C36 121.2(3) . . ? C33 N32 C37 120.8(3) . . ? C36 N32 C37 118.0(3) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 30.68 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.602 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.089 # End of CIF ============================================================