Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_mesitylene _database_code_CSD 160670 _journal_coden_Cambridge 182 _publ_contact_author_name 'Shin-ichi Nishikiori' _publ_contact_author_address ; Department of Basic Science, Graduate School of Arts and Sciences, The University of Tokyo, Komaba3-8-1, Meguro, Tokyo 153-8902, Japan ; _publ_contact_author_email 'cnskor@mail.ecc.u-tokyo.ac.jp' loop_ _publ_author_name 'Hirofumi Yoshikawa' 'Shin-ichi Nishikiori' 'Roman Luboradzki' 'Kinga Suwinska' 'Janusz Lipkowski' _publ_requested_journal 'Chemical Communications' _audit_creation_method SHELXL _chemical_formula_structural 'Cd3 (C6 N6 Cl2)(C12 N2 H14)(C9 H12)' _chemical_formula_sum 'C27 H26 Cd3 Cl2 N8' _chemical_formula_weight 870.70 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' 'Cd' 'Cd' -0.8075 1.2024 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 23.7905(7) _cell_length_b 8.8535(2) _cell_length_c 15.5522(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3275.75(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4059 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 1.74 _exptl_crystal_density_diffrn 1.77 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 2.108 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius-CCD' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3952 _reflns_number_observed 2739 _reflns_observed_criterion >3sigma(I) _computing_data_collection 'Denzo/Scalepack' _computing_cell_refinement 'Denzo/Scalepack' _computing_data_reduction 'Denzo/Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 for Windows' _refine_special_details ; Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 3sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. All the hydrogen atoms are not determined. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_number_reflns 2739 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_obs 0.0564 _refine_ls_wR_factor_all 0.1639 _refine_ls_wR_factor_obs 0.1133 _refine_ls_goodness_of_fit_all 1.316 _refine_ls_goodness_of_fit_obs 1.104 _refine_ls_restrained_S_all 1.316 _refine_ls_restrained_S_obs 1.104 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.34236(3) 0.75000 0.07154(4) 0.0295(2) Uani 1 d S . Cd2 Cd 0.48122(3) 0.25000 0.16299(4) 0.0352(2) Uani 1 d S . Cd3 Cd 0.26836(3) 0.75000 0.41988(4) 0.0373(2) Uani 1 d S . Cl1 Cl 0.5075(2) 0.25000 0.3179(2) 0.0696(9) Uani 1 d S . Cl2 Cl 0.3713(1) 0.75000 0.4670(2) 0.0610(8) Uani 1 d S . N1 N 0.4028(4) 0.75000 -0.0438(5) 0.047(2) Uani 1 d S . C1 C 0.4422(5) 0.75000 -0.0844(6) 0.042(3) Uani 1 d S . N2 N 0.2983(4) 0.75000 0.2078(5) 0.039(2) Uani 1 d S . C2 C 0.2846(4) 0.75000 0.2781(6) 0.037(2) Uani 1 d S . N3 N 0.4008(3) 0.5543(6) 0.1275(4) 0.044(1) Uani 1 d . . C3 C 0.4284(3) 0.4535(7) 0.1410(4) 0.039(2) Uani 1 d . . N4 N 0.2862(3) 0.5597(6) 0.0107(4) 0.047(2) Uani 1 d . . C4 C 0.2679(3) 0.4588(7) -0.0233(4) 0.042(2) Uani 1 d . . C101 C 0.3372(3) 0.1189(8) 0.2956(5) 0.050(2) Uani 1 d . . C102 C 0.3646(3) 0.1149(7) 0.3749(5) 0.049(2) Uani 1 d . . C103 C 0.3799(4) 0.25000 0.4127(6) 0.036(2) Uani 1 d S . C104 C 0.4157(4) 0.25000 0.4943(6) 0.034(2) Uani 1 d S . C105 C 0.4327(3) 0.1154(8) 0.5305(4) 0.050(2) Uani 1 d . . C106 C 0.4680(4) 0.1160(8) 0.6026(5) 0.053(2) Uani 1 d . . C111 C 0.2985(5) 0.25000 0.1698(6) 0.052(3) Uani 1 d S . C112 C 0.5234(6) 0.25000 0.7136(7) 0.074(4) Uani 1 d S . N101 C 0.3244(4) 0.25000 0.2592(5) 0.042(2) Uani 1 d S . N102 C 0.4844(4) 0.25000 0.6361(6) 0.051(2) Uani 1 d S . C201 C 0.4033(6) 0.25000 0.8499(7) 0.069(4) Uani 1 d S . C202 C 0.3884(4) 0.116(1) 0.8141(6) 0.075(3) Uani 1 d . . C203 C 0.3585(4) 0.113(1) 0.7368(7) 0.071(3) Uani 1 d . . C204 C 0.3445(5) 0.25000 0.6995(8) 0.073(4) Uani 1 d S . C205 C 0.4379(9) 0.25000 0.935(1) 0.16(1) Uani 1 d S . C206 C 0.3392(5) -0.034(1) 0.695(1) 0.155(6) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 0.0334(4) 0.0239(3) 0.0314(4) 0.0 -0.0001(3) 0.0 Cd2 0.0348(5) 0.0276(4) 0.0432(4) 0.0 0.0017(3) 0.0 Cd3 0.0502(6) 0.0269(4) 0.0348(4) 0.0 0.0127(3) 0.0 Cl1 0.075(3) 0.054(2) 0.079(2) 0.0 0.003(2) 0.0 Cl2 0.076(2) 0.033(1) 0.074(2) 0.0 -0.008(2) 0.0 N1 0.043(6) 0.046(5) 0.051(5) 0.0 0.017(5) 0.0 C1 0.056(8) 0.028(5) 0.043(6) 0.0 0.004(5) 0.0 N2 0.049(6) 0.039(5) 0.030(4) 0.0 0.013(4) 0.0 C2 0.040(6) 0.031(5) 0.041(6) 0.0 0.004(5) 0.0 N3 0.046(4) 0.039(3) 0.047(3) 0.005(3) 0.003(3) 0.000(3) C3 0.047(5) 0.028(4) 0.041(4) 0.004(3) -0.003(3) 0.001(3) N4 0.056(4) 0.037(3) 0.048(4) -0.004(3) -0.009(3) -0.004(3) C4 0.052(5) 0.036(4) 0.038(4) 0.000(4) -0.012(4) 0.001(3) C101 0.057(6) 0.043(4) 0.050(4) -0.012(4) -0.005(4) 0.007(4) C102 0.065(6) 0.029(4) 0.052(4) -0.010(4) -0.009(4) -0.002(3) C103 0.038(6) 0.031(5) 0.039(5) 0.0 0.011(5) 0.0 C104 0.040(6) 0.025(5) 0.038(5) 0.0 0.005(5) 0.0 C105 0.068(6) 0.038(4) 0.042(4) 0.012(4) -0.001(4) 0.003(3) C106 0.064(6) 0.048(5) 0.047(4) 0.004(4) 0.002(4) -0.001(4) C111 0.054(8) 0.057(6) 0.044(6) 0.0 -0.014(6) 0.0 C112 0.06(1) 0.11(1) 0.048(7) 0.0 -0.025(6) 0.0 N101 0.049(6) 0.036(5) 0.040(5) 0.0 0.002(4) 0.0 N102 0.047(6) 0.053(6) 0.052(5) 0.0 -0.001(5) 0.0 C201 0.08(1) 0.08(1) 0.049(7) 0.0 -0.002(7) 0.0 C202 0.067(7) 0.062(6) 0.096(7) 0.002(5) 0.011(6) 0.023(6) C203 0.049(6) 0.058(6) 0.106(8) -0.007(4) 0.017(6) -0.009(6) C204 0.046(8) 0.12(1) 0.055(7) 0.0 0.017(6) 0.0 C205 0.17(2) 0.23(3) 0.07(1) 0.0 -0.04(1) 0.0 C206 0.10(1) 0.11(1) 0.26(2) -0.041(8) -0.01(1) -0.10(1) 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 N1 2.300(8) . ? Cd1 N4 2.349(6) . ? Cd1 N4 2.349(6) 8_575 ? Cd1 N2 2.365(7) . ? Cd1 N3 2.386(6) 8_575 ? Cd1 N3 2.386(6) . ? Cd2 C1 2.19(1) 5_665 ? Cd2 C3 2.223(7) 8_565 ? Cd2 C3 2.223(7) . ? Cd2 Cl1 2.489(3) . ? Cd3 C4 2.223(7) 2_565 ? Cd3 C4 2.223(7) 7_666 ? Cd3 C2 2.238(9) . ? Cd3 Cl2 2.556(3) . ? N1 C1 1.13(1) . ? C1 Cd2 2.19(1) 5_665 ? N2 C2 1.14(1) . ? N3 C3 1.128(8) . ? N4 C4 1.126(8) . ? C4 Cd3 2.223(7) 2_564 ? C101 N101 1.327(8) . ? C101 C102 1.395(9) . ? C102 C103 1.382(8) . ? C103 C102 1.382(8) 8_565 ? C103 C104 1.53(1) . ? C104 C105 1.379(8) 8_565 ? C104 C105 1.379(8) . ? C105 C106 1.40(1) . ? C106 N102 1.353(8) . ? C111 N101 1.52(1) . ? C112 N102 1.52(1) . ? N101 C101 1.327(8) 8_565 ? N102 C106 1.353(8) 8_565 ? C201 C202 1.36(1) . ? C201 C202 1.36(1) 8_565 ? C201 C205 1.56(2) . ? C202 C203 1.40(1) . ? C203 C204 1.39(1) . ? C203 C206 1.52(1) . ? C204 C203 1.39(1) 8_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N4 92.4(2) . . ? N1 Cd1 N4 92.4(2) . 8_575 ? N4 Cd1 N4 91.7(3) . 8_575 ? N1 Cd1 N2 167.6(3) . . ? N4 Cd1 N2 96.2(2) . . ? N4 Cd1 N2 96.2(2) 8_575 . ? N1 Cd1 N3 85.4(2) . 8_575 ? N4 Cd1 N3 177.6(2) . 8_575 ? N4 Cd1 N3 87.5(2) 8_575 8_575 ? N2 Cd1 N3 86.1(2) . 8_575 ? N1 Cd1 N3 85.4(2) . . ? N4 Cd1 N3 87.5(2) . . ? N4 Cd1 N3 177.6(2) 8_575 . ? N2 Cd1 N3 86.1(2) . . ? N3 Cd1 N3 93.2(3) 8_575 . ? C1 Cd2 C3 112.6(2) 5_665 8_565 ? C1 Cd2 C3 112.6(2) 5_665 . ? C3 Cd2 C3 108.3(4) 8_565 . ? C1 Cd2 Cl1 109.3(3) 5_665 . ? C3 Cd2 Cl1 106.9(2) 8_565 . ? C3 Cd2 Cl1 106.9(2) . . ? C4 Cd3 C4 112.5(3) 2_565 7_666 ? C4 Cd3 C2 117.3(2) 2_565 . ? C4 Cd3 C2 117.3(2) 7_666 . ? C4 Cd3 Cl2 104.9(2) 2_565 . ? C4 Cd3 Cl2 104.9(2) 7_666 . ? C2 Cd3 Cl2 96.7(3) . . ? C1 N1 Cd1 162.7(9) . . ? N1 C1 Cd2 180.0(6) . 5_665 ? C2 N2 Cd1 170.2(9) . . ? N2 C2 Cd3 173.4(9) . . ? C3 N3 Cd1 169.1(6) . . ? N3 C3 Cd2 177.6(6) . . ? C4 N4 Cd1 168.1(6) . . ? N4 C4 Cd3 175.3(6) . 2_564 ? N101 C101 C102 120.5(7) . . ? C103 C102 C101 118.5(7) . . ? C102 C103 C102 119.9(9) . 8_565 ? C102 C103 C104 120.0(5) . . ? C102 C103 C104 120.0(5) 8_565 . ? C105 C104 C105 119.6(9) 8_565 . ? C105 C104 C103 120.2(5) 8_565 . ? C105 C104 C103 120.2(5) . . ? C104 C105 C106 120.0(7) . . ? N102 C106 C105 119.1(7) . . ? C101 N101 C101 122.0(9) 8_565 . ? C101 N101 C111 118.9(4) 8_565 . ? C101 N101 C111 118.9(4) . . ? C106 N102 C106 122.4(9) . 8_565 ? C106 N102 C112 118.8(5) . . ? C106 N102 C112 118.8(5) 8_565 . ? C202 C201 C202 122(1) . 8_565 ? C202 C201 C205 119.1(6) . . ? C202 C201 C205 119.1(6) 8_565 . ? C201 C202 C203 120.1(9) . . ? C204 C203 C202 117.9(9) . . ? C204 C203 C206 120(1) . . ? C202 C203 C206 122(1) . . ? C203 C204 C203 122(1) 8_565 . ? _refine_diff_density_max 0.94 _refine_diff_density_min -1.06 _refine_diff_density_rms 0.14