data_w2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Cd I N4, I' _chemical_formula_sum 'C6 H18 Cd I2 N4' _chemical_formula_weight 512.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.8508(2) _cell_length_b 16.6358(3) _cell_length_c 11.0386(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.1790(8) _cell_angle_gamma 90.00 _cell_volume 1435.80(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 20238 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 5.794 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.177 _exptl_absorpt_correction_T_max 0.440 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _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 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20238 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.99 _reflns_number_total 3465 _reflns_number_gt 2657 _reflns_threshold_expression 'I>2sigma(I)' _computing_data_collection 'Kappa CCD server software (Nonius, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al.,1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997); WINGX (Farrugia, 1999) ; _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^)+(0.0701P)^2^+0.8213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0102(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3465 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.26108(5) 0.19852(2) 0.27242(4) 0.04364(17) Uani 1 1 d . . . I1 I 0.29070(6) 0.36297(2) 0.30492(4) 0.06069(19) Uani 1 1 d . . . I2 I 0.73998(6) 0.18566(3) 0.44438(4) 0.06720(19) Uani 1 1 d . . . N1 N 0.2203(6) 0.0548(3) 0.2321(4) 0.0455(10) Uani 1 1 d . . . N2 N 0.4682(6) 0.1660(3) 0.1471(4) 0.0530(12) Uani 1 1 d . . . H1N H 0.4355 0.1821 0.0707 0.064 Uiso 1 1 calc R . . H2N H 0.5663 0.1914 0.1721 0.064 Uiso 1 1 calc R . . N3 N 0.2751(8) 0.1398(4) 0.4606(4) 0.0661(15) Uani 1 1 d . . . H3N H 0.3843 0.1402 0.4935 0.079 Uiso 1 1 calc R . . H4N H 0.2125 0.1688 0.5093 0.079 Uiso 1 1 calc R . . N4 N -0.0095(6) 0.1889(4) 0.1752(6) 0.0648(15) Uani 1 1 d . . . H5N H -0.0872 0.1920 0.2302 0.078 Uiso 1 1 calc R . . H6N H -0.0279 0.2302 0.1229 0.078 Uiso 1 1 calc R . . C1 C 0.3309(8) 0.0329(4) 0.1371(6) 0.0544(14) Uani 1 1 d . . . H1A H 0.2713 0.0439 0.0580 0.065 Uiso 1 1 calc R . . H1B H 0.3546 -0.0243 0.1418 0.065 Uiso 1 1 calc R . . C2 C 0.4967(7) 0.0782(4) 0.1489(5) 0.0551(15) Uani 1 1 d . . . H2A H 0.5617 0.0633 0.2245 0.066 Uiso 1 1 calc R . . H2B H 0.5633 0.0635 0.0824 0.066 Uiso 1 1 calc R . . C3 C 0.2682(11) 0.0127(4) 0.3473(6) 0.0698(18) Uani 1 1 d . . . H3A H 0.3913 0.0058 0.3571 0.084 Uiso 1 1 calc R . . H3B H 0.2163 -0.0403 0.3441 0.084 Uiso 1 1 calc R . . C4 C 0.2127(10) 0.0575(4) 0.4556(6) 0.0682(18) Uani 1 1 d . . . H4A H 0.0888 0.0578 0.4517 0.082 Uiso 1 1 calc R . . H4B H 0.2551 0.0296 0.5294 0.082 Uiso 1 1 calc R . . C5 C 0.0378(8) 0.0446(5) 0.1879(7) 0.0690(19) Uani 1 1 d . . . H5A H -0.0293 0.0401 0.2572 0.083 Uiso 1 1 calc R . . H5B H 0.0242 -0.0049 0.1418 0.083 Uiso 1 1 calc R . . C6 C -0.0294(8) 0.1132(6) 0.1095(6) 0.069(2) Uani 1 1 d . . . H6A H 0.0319 0.1158 0.0372 0.083 Uiso 1 1 calc R . . H6B H -0.1495 0.1044 0.0841 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0553(3) 0.0403(3) 0.0363(2) -0.00158(15) 0.00959(17) 0.00030(16) I1 0.0945(4) 0.0413(3) 0.0467(3) -0.00412(16) 0.0086(2) 0.00338(18) I2 0.0721(3) 0.0788(4) 0.0506(3) -0.0082(2) 0.0044(2) -0.0044(2) N1 0.059(3) 0.043(3) 0.036(2) -0.0008(19) 0.0112(19) -0.007(2) N2 0.049(2) 0.061(3) 0.051(3) -0.003(2) 0.016(2) -0.011(2) N3 0.099(4) 0.069(4) 0.032(3) -0.002(2) 0.011(2) -0.010(3) N4 0.047(3) 0.089(4) 0.058(3) 0.006(3) 0.004(2) 0.008(3) C1 0.070(4) 0.050(3) 0.046(3) -0.008(3) 0.014(3) 0.000(3) C2 0.052(3) 0.063(4) 0.051(3) -0.007(3) 0.008(3) 0.010(3) C3 0.108(5) 0.048(4) 0.056(4) 0.008(3) 0.018(4) 0.001(4) C4 0.101(5) 0.064(4) 0.042(3) 0.011(3) 0.019(3) -0.003(4) C5 0.068(4) 0.075(5) 0.066(4) -0.014(4) 0.019(3) -0.028(4) C6 0.040(3) 0.119(6) 0.048(3) -0.008(4) 0.000(2) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.289(5) . ? Cd1 N2 2.293(5) . ? Cd1 N4 2.297(5) . ? Cd1 N1 2.448(5) . ? Cd1 I1 2.7661(6) . ? N1 C1 1.466(7) . ? N1 C3 1.471(8) . ? N1 C5 1.481(8) . ? N2 C2 1.477(9) . ? N2 H1N 0.9000 . ? N2 H2N 0.9000 . ? N3 C4 1.454(9) . ? N3 H3N 0.9000 . ? N3 H4N 0.9000 . ? N4 C6 1.455(10) . ? N4 H5N 0.9000 . ? N4 H6N 0.9000 . ? C1 C2 1.499(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.506(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.499(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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 N3 Cd1 N2 117.9(2) . . ? N3 Cd1 N4 111.2(2) . . ? N2 Cd1 N4 112.2(2) . . ? N3 Cd1 N1 75.12(17) . . ? N2 Cd1 N1 75.40(17) . . ? N4 Cd1 N1 75.34(19) . . ? N3 Cd1 I1 107.92(14) . . ? N2 Cd1 I1 104.82(13) . . ? N4 Cd1 I1 101.10(16) . . ? N1 Cd1 I1 176.10(11) . . ? C1 N1 C3 112.2(5) . . ? C1 N1 C5 110.8(5) . . ? C3 N1 C5 113.2(5) . . ? C1 N1 Cd1 107.2(3) . . ? C3 N1 Cd1 106.8(4) . . ? C5 N1 Cd1 106.2(4) . . ? C2 N2 Cd1 109.9(3) . . ? C2 N2 H1N 109.7 . . ? Cd1 N2 H1N 109.7 . . ? C2 N2 H2N 109.7 . . ? Cd1 N2 H2N 109.7 . . ? H1N N2 H2N 108.2 . . ? C4 N3 Cd1 112.2(4) . . ? C4 N3 H3N 109.2 . . ? Cd1 N3 H3N 109.2 . . ? C4 N3 H4N 109.2 . . ? Cd1 N3 H4N 109.2 . . ? H3N N3 H4N 107.9 . . ? C6 N4 Cd1 110.3(4) . . ? C6 N4 H5N 109.6 . . ? Cd1 N4 H5N 109.6 . . ? C6 N4 H6N 109.6 . . ? Cd1 N4 H6N 109.6 . . ? H5N N4 H6N 108.1 . . ? N1 C1 C2 112.3(5) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 111.5(5) . . ? N2 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N1 C3 C4 112.4(6) . . ? N1 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N1 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N3 C4 C3 112.1(6) . . ? N3 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C6 112.5(5) . . ? N1 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N4 C6 C5 110.8(5) . . ? N4 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.753 _refine_diff_density_min -1.471 _refine_diff_density_rms 0.188