Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Krysztof Wozniak' 'Lukasz Dobrzycki' _publ_contact_author_name 'Krysztof Wozniak' _publ_contact_author_address ; Chemistry Department The University of Warsaw ul. Pasteura 1 Warszawa 02093 POLAND ; _publ_contact_author_email KWOZNIAK@CHEM.UW.EDU.PL _publ_requested_journal CrystEngComm _publ_section_title ; Inorganic - Organic hybrid salts of Diaminobenzenes and Related Cations ; data_1+Pb2Cl6 _database_code_depnum_ccdc_archive 'CCDC 659014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl6 N2 Pb2' _chemical_formula_weight 737.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7009(18) _cell_length_b 7.8374(10) _cell_length_c 7.4351(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.238(10) _cell_angle_gamma 90.00 _cell_volume 770.31(16) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description planar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 22.843 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.03 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KM4CCD _diffrn_measurement_method '1 frame' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 13075 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 29.99 _reflns_number_total 2247 _reflns_number_gt 1817 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0423P)^2^+2.4837P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2247 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.329 _refine_ls_restrained_S_all 1.329 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.42243(2) 0.04242(4) 0.24049(4) 0.01962(13) Uani 1 1 d . . . Cl1 Cl 0.41887(16) -0.2006(3) -0.0451(3) 0.0214(4) Uani 1 1 d . . . Cl2 Cl 0.35833(16) 0.3615(3) 0.0801(3) 0.0244(4) Uani 1 1 d . . . Cl3 Cl 0.21359(16) -0.0185(3) 0.1252(3) 0.0263(5) Uani 1 1 d . . . N1 N 0.1985(6) -0.4089(10) 0.2010(12) 0.0255(16) Uani 1 1 d . . . H1A H 0.2045 -0.2932 0.2054 0.038 Uiso 1 1 calc R . . H1B H 0.2434 -0.4535 0.1427 0.038 Uiso 1 1 calc R . . H1C H 0.2115 -0.4510 0.3190 0.038 Uiso 1 1 calc R . . C1 C 0.0964(6) -0.4550(11) 0.0986(13) 0.0207(16) Uani 1 1 d . . . C2 C 0.0785(7) -0.6086(14) 0.0026(17) 0.036(3) Uani 1 1 d . . . H2 H 0.1330 -0.6840 0.0040 0.044 Uiso 1 1 calc R . . C3 C 0.0171(8) -0.3492(14) 0.0934(19) 0.043(3) Uani 1 1 d . . . H3 H 0.0289 -0.2436 0.1583 0.051 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 Pb1 0.02024(18) 0.01903(17) 0.01824(17) -0.00018(13) 0.00268(11) 0.00166(13) Cl1 0.0210(9) 0.0220(9) 0.0210(9) -0.0035(8) 0.0052(8) 0.0005(8) Cl2 0.0229(10) 0.0231(10) 0.0292(10) 0.0072(9) 0.0103(8) 0.0061(8) Cl3 0.0172(9) 0.0271(10) 0.0325(11) -0.0045(9) 0.0026(9) 0.0005(8) N1 0.013(3) 0.030(4) 0.030(4) -0.003(3) -0.001(3) 0.001(3) C1 0.013(4) 0.023(4) 0.025(4) -0.002(4) 0.005(3) -0.001(3) C2 0.019(4) 0.027(5) 0.059(7) -0.019(5) 0.005(5) 0.000(4) C3 0.025(5) 0.031(5) 0.068(8) -0.019(5) 0.004(5) 0.003(4) _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 Pb1 Cl3 2.804(2) . ? Pb1 Cl2 2.810(2) . ? Pb1 Cl1 2.843(2) . ? Pb1 Cl2 2.980(2) 4_566 ? Cl2 Pb1 2.980(2) 4_565 ? N1 C1 1.452(11) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? C1 C3 1.359(13) . ? C1 C2 1.388(13) . ? C2 C3 1.358(14) 3_545 ? C2 H2 0.9500 . ? C3 C2 1.358(14) 3_545 ? C3 H3 0.9500 . ? 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 Cl3 Pb1 Cl2 80.90(7) . . ? Cl3 Pb1 Cl1 80.89(6) . . ? Cl2 Pb1 Cl1 109.69(7) . . ? Cl3 Pb1 Cl2 78.34(7) . 4_566 ? Cl2 Pb1 Cl2 90.34(5) . 4_566 ? Cl1 Pb1 Cl2 148.33(6) . 4_566 ? Pb1 Cl2 Pb1 117.11(7) . 4_565 ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C3 C1 C2 118.9(9) . . ? C3 C1 N1 121.0(9) . . ? C2 C1 N1 120.1(8) . . ? C3 C2 C1 119.8(9) 3_545 . ? C3 C2 H2 120.1 3_545 . ? C1 C2 H2 120.1 . . ? C2 C3 C1 121.3(10) 3_545 . ? C2 C3 H3 119.4 3_545 . ? C1 C3 H3 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl3 Pb1 Cl2 Pb1 -114.20(9) . . . 4_565 ? Cl1 Pb1 Cl2 Pb1 -37.35(10) . . . 4_565 ? Cl2 Pb1 Cl2 Pb1 167.67(6) 4_566 . . 4_565 ? C3 C1 C2 C3 0(2) . . . 3_545 ? N1 C1 C2 C3 -179.8(11) . . . 3_545 ? C2 C1 C3 C2 0(2) . . . 3_545 ? N1 C1 C3 C2 179.8(11) . . . 3_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Cl3 0.91 2.25 3.127(9) 162.9 . N1 H1B Cl2 0.91 2.28 3.143(8) 158.8 1_545 N1 H1C Cl3 0.91 2.28 3.158(9) 161.4 4_556 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.404 _refine_diff_density_min -1.521 _refine_diff_density_rms 0.366 data_1+Hg(II)_aqua_chloride _database_code_depnum_ccdc_archive 'CCDC 659015' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl14 Hg6 N2 O2' _chemical_formula_weight 1842.00 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' O O 0.0106 0.0060 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6706(12) _cell_length_b 10.9982(11) _cell_length_c 14.7910(16) _cell_angle_alpha 95.696(9) _cell_angle_beta 101.053(10) _cell_angle_gamma 99.407(9) _cell_volume 1509.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 31.653 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.02 _exptl_absorpt_correction_T_max 0.23 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 27000 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8503 _reflns_number_gt 5897 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0322P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00095(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8503 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Hg1 Hg 0.72320(3) 1.04818(3) 1.06098(2) 0.02606(8) Uani 1 1 d . . . Hg2 Hg 0.59717(3) 0.08441(3) 0.67942(2) 0.02628(8) Uani 1 1 d . . . Hg3 Hg 0.96647(3) 0.18160(3) 0.86297(2) 0.02661(8) Uani 1 1 d . . . Hg4 Hg 0.82787(3) 0.78743(3) 0.85361(2) 0.02664(8) Uani 1 1 d . . . Hg5 Hg 0.39253(4) 0.73536(4) 0.58771(3) 0.03658(10) Uani 1 1 d . . . Hg6 Hg 0.62361(3) 0.46540(4) 0.67279(2) 0.03019(9) Uani 1 1 d . . . Cl1 Cl 0.5954(2) 0.8854(2) 0.95237(16) 0.0306(5) Uani 1 1 d . . . Cl2 Cl 0.8376(2) 1.2170(2) 1.16754(16) 0.0302(5) Uani 1 1 d . . . Cl3 Cl 0.7905(2) 0.2051(2) 0.64121(17) 0.0349(5) Uani 1 1 d . . . Cl4 Cl 0.4066(2) -0.0333(2) 0.72167(15) 0.0267(4) Uani 1 1 d . . . Cl5 Cl 1.1751(2) 0.1603(2) 0.81560(15) 0.0273(4) Uani 1 1 d . . . Cl6 Cl 0.7481(2) 0.2122(2) 0.89247(16) 0.0330(5) Uani 1 1 d . . . Cl7 Cl 0.8265(2) 0.9214(2) 0.74323(14) 0.0260(4) Uani 1 1 d . . . Cl8 Cl 0.8437(2) 0.6384(2) 0.95209(15) 0.0306(5) Uani 1 1 d . . . Cl9 Cl 0.5652(2) 0.8615(2) 0.52831(14) 0.0254(4) Uani 1 1 d . . . Cl10 Cl 0.1526(2) 0.6409(2) 0.57004(19) 0.0403(6) Uani 1 1 d . . . Cl11 Cl 0.5187(2) 0.65997(19) 0.74295(14) 0.0245(4) Uani 1 1 d . . . Cl12 Cl 0.5000 0.5000 0.5000 0.0521(10) Uani 1 2 d S . . Cl13 Cl 0.8577(2) 0.5708(2) 0.68098(15) 0.0284(4) Uani 1 1 d . . . Cl14 Cl 0.4489(2) 0.30298(19) 0.69436(15) 0.0261(4) Uani 1 1 d . . . Cl15 Cl 1.0000 1.0000 1.0000 0.0218(5) Uani 1 2 d S . . O1A O 0.9773(7) 0.5462(7) 0.1505(5) 0.0355(16) Uani 1 1 d . . . O1B O 0.1054(7) 0.3794(7) 0.6387(5) 0.0390(16) Uani 1 1 d . . . N1A N 0.6934(7) 0.5289(7) 0.1698(5) 0.0271(16) Uani 1 1 d . . . H1CA H 0.6917 0.6013 0.2048 0.041 Uiso 1 1 calc R . . H1AA H 0.7832 0.5295 0.1594 0.041 Uiso 1 1 calc R . . H1BA H 0.6686 0.4638 0.2006 0.041 Uiso 1 1 calc R . . N1B N 0.1431(7) 0.2377(7) 0.4800(6) 0.0316(17) Uani 1 1 d . . . H1AB H 0.1049 0.2591 0.4240 0.047 Uiso 1 1 calc R . . H1BB H 0.2379 0.2366 0.4837 0.047 Uiso 1 1 calc R . . H1CB H 0.1328 0.2942 0.5264 0.047 Uiso 1 1 calc R . . C1A C 0.5920(8) 0.5161(8) 0.0813(5) 0.0214(17) Uani 1 1 d . . . C2A C 0.5157(9) 0.6081(9) 0.0619(6) 0.0283(19) Uani 1 1 d . . . H2A H 0.5282 0.6809 0.1051 0.034 Uiso 1 1 calc R . . C3A C 0.4233(9) 0.5922(8) -0.0198(6) 0.0259(18) Uani 1 1 d . . . H3A H 0.3684 0.6541 -0.0359 0.031 Uiso 1 1 calc R . . C1B C 0.0686(8) 0.1142(8) 0.4896(6) 0.0223(17) Uani 1 1 d . . . C2B C -0.0431(9) 0.0567(9) 0.4213(6) 0.0261(18) Uani 1 1 d . . . H2B H -0.0733 0.0945 0.3677 0.031 Uiso 1 1 calc R . . C3B C -0.1112(9) -0.0583(9) 0.4325(6) 0.0260(18) Uani 1 1 d . . . H3B H -0.1901 -0.1011 0.3854 0.031 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 Hg1 0.02371(15) 0.02341(18) 0.02795(18) -0.00040(13) 0.00230(12) 0.00150(12) Hg2 0.02157(14) 0.02311(18) 0.03455(19) 0.00660(14) 0.00754(13) 0.00175(12) Hg3 0.02257(15) 0.02982(19) 0.02909(18) 0.00498(14) 0.00801(12) 0.00605(13) Hg4 0.03233(16) 0.02333(18) 0.02444(18) 0.00723(13) 0.00500(13) 0.00449(13) Hg5 0.02872(17) 0.0325(2) 0.0485(2) 0.00504(17) 0.01458(16) -0.00163(15) Hg6 0.02470(15) 0.0322(2) 0.03059(19) 0.00525(15) 0.00528(13) -0.00337(14) Cl1 0.0248(9) 0.0265(11) 0.0361(12) -0.0059(9) 0.0026(8) 0.0024(8) Cl2 0.0265(9) 0.0278(12) 0.0317(12) -0.0044(9) 0.0037(8) -0.0003(8) Cl3 0.0259(10) 0.0370(14) 0.0405(13) 0.0126(11) 0.0077(9) -0.0026(9) Cl4 0.0251(9) 0.0226(11) 0.0352(12) 0.0067(9) 0.0125(8) 0.0034(8) Cl5 0.0236(9) 0.0303(12) 0.0297(11) 0.0057(9) 0.0099(8) 0.0042(8) Cl6 0.0275(10) 0.0429(14) 0.0337(12) 0.0077(10) 0.0112(9) 0.0145(9) Cl7 0.0278(9) 0.0263(11) 0.0237(11) 0.0090(8) 0.0021(8) 0.0049(8) Cl8 0.0395(11) 0.0278(12) 0.0291(12) 0.0120(9) 0.0122(9) 0.0090(9) Cl9 0.0248(9) 0.0260(11) 0.0258(11) 0.0044(8) 0.0075(8) 0.0029(8) Cl10 0.0232(10) 0.0373(14) 0.0603(17) 0.0157(12) 0.0076(10) 0.0013(9) Cl11 0.0277(9) 0.0198(10) 0.0256(11) 0.0024(8) 0.0048(8) 0.0041(8) Cl12 0.084(3) 0.050(2) 0.0208(18) 0.0049(16) -0.0072(17) 0.029(2) Cl13 0.0201(8) 0.0296(12) 0.0357(12) 0.0095(9) 0.0060(8) 0.0017(8) Cl14 0.0265(9) 0.0182(10) 0.0338(11) 0.0006(8) 0.0108(8) 0.0013(8) Cl15 0.0208(11) 0.0246(15) 0.0199(14) 0.0043(11) 0.0038(10) 0.0032(10) O1A 0.036(3) 0.041(4) 0.038(4) 0.017(3) 0.015(3) 0.020(3) O1B 0.035(3) 0.037(4) 0.042(4) -0.001(3) 0.002(3) 0.010(3) N1A 0.022(3) 0.029(4) 0.030(4) 0.003(3) 0.006(3) 0.004(3) N1B 0.026(3) 0.030(4) 0.042(5) 0.010(4) 0.010(3) 0.008(3) C1A 0.015(3) 0.028(5) 0.017(4) 0.000(3) 0.004(3) -0.005(3) C2A 0.032(4) 0.029(5) 0.021(5) -0.006(4) 0.001(3) 0.007(4) C3A 0.028(4) 0.021(4) 0.031(5) 0.008(4) 0.007(3) 0.008(3) C1B 0.022(4) 0.025(4) 0.023(4) 0.004(3) 0.008(3) 0.011(3) C2B 0.031(4) 0.033(5) 0.018(4) 0.007(4) 0.005(3) 0.015(4) C3B 0.028(4) 0.029(5) 0.023(4) 0.002(4) 0.005(3) 0.010(4) _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 Hg1 Cl2 2.288(2) . ? Hg1 Cl1 2.293(2) . ? Hg2 Cl4 2.299(2) . ? Hg2 Cl3 2.307(2) . ? Hg3 Cl5 2.2983(19) . ? Hg3 Cl6 2.307(2) . ? Hg4 Cl8 2.302(2) . ? Hg4 Cl7 2.305(2) . ? Hg5 Cl10 2.336(2) . ? Hg5 Cl9 2.352(2) . ? Hg5 Cl11 2.661(2) . ? Hg6 Cl14 2.341(2) . ? Hg6 Cl13 2.344(2) . ? Hg6 Cl12 2.6974(5) . ? Hg6 Cl11 2.712(2) . ? Cl12 Hg6 2.6974(5) 2_666 ? N1A C1A 1.457(10) . ? N1A H1CA 0.9100 . ? N1A H1AA 0.9100 . ? N1A H1BA 0.9100 . ? N1B C1B 1.463(11) . ? N1B H1AB 0.9100 . ? N1B H1BB 0.9100 . ? N1B H1CB 0.9100 . ? C1A C2A 1.368(12) . ? C1A C3A 1.394(12) 2_665 ? C2A C3A 1.335(12) . ? C2A H2A 0.9500 . ? C3A C1A 1.394(12) 2_665 ? C3A H3A 0.9500 . ? C1B C2B 1.348(12) . ? C1B C3B 1.385(12) 2_556 ? C2B C3B 1.368(13) . ? C2B H2B 0.9500 . ? C3B C1B 1.385(12) 2_556 ? C3B H3B 0.9500 . ? 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 Cl2 Hg1 Cl1 176.13(8) . . ? Cl4 Hg2 Cl3 178.43(8) . . ? Cl5 Hg3 Cl6 172.61(8) . . ? Cl8 Hg4 Cl7 172.58(8) . . ? Cl10 Hg5 Cl9 147.59(8) . . ? Cl10 Hg5 Cl11 102.82(8) . . ? Cl9 Hg5 Cl11 109.58(7) . . ? Cl14 Hg6 Cl13 155.44(8) . . ? Cl14 Hg6 Cl12 98.56(6) . . ? Cl13 Hg6 Cl12 99.68(6) . . ? Cl14 Hg6 Cl11 98.78(7) . . ? Cl13 Hg6 Cl11 97.79(7) . . ? Cl12 Hg6 Cl11 89.22(5) . . ? Hg5 Cl11 Hg6 101.12(7) . . ? Hg6 Cl12 Hg6 180.000(1) 2_666 . ? C1A N1A H1CA 109.5 . . ? C1A N1A H1AA 109.5 . . ? H1CA N1A H1AA 109.5 . . ? C1A N1A H1BA 109.5 . . ? H1CA N1A H1BA 109.5 . . ? H1AA N1A H1BA 109.5 . . ? C1B N1B H1AB 109.5 . . ? C1B N1B H1BB 109.5 . . ? H1AB N1B H1BB 109.5 . . ? C1B N1B H1CB 109.5 . . ? H1AB N1B H1CB 109.5 . . ? H1BB N1B H1CB 109.5 . . ? C2A C1A C3A 122.8(8) . 2_665 ? C2A C1A N1A 119.8(7) . . ? C3A C1A N1A 117.4(8) 2_665 . ? C3A C2A C1A 117.8(8) . . ? C3A C2A H2A 121.1 . . ? C1A C2A H2A 121.1 . . ? C2A C3A C1A 119.3(8) . 2_665 ? C2A C3A H3A 120.3 . . ? C1A C3A H3A 120.3 2_665 . ? C2B C1B C3B 120.8(9) . 2_556 ? C2B C1B N1B 118.6(8) . . ? C3B C1B N1B 120.6(8) 2_556 . ? C1B C2B C3B 117.2(8) . . ? C1B C2B H2B 121.4 . . ? C3B C2B H2B 121.4 . . ? C2B C3B C1B 122.0(8) . 2_556 ? C2B C3B H3B 119.0 . . ? C1B C3B H3B 119.0 2_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl10 Hg5 Cl11 Hg6 97.58(9) . . . . ? Cl9 Hg5 Cl11 Hg6 -81.58(8) . . . . ? Cl14 Hg6 Cl11 Hg5 -101.44(8) . . . . ? Cl13 Hg6 Cl11 Hg5 96.75(8) . . . . ? Cl12 Hg6 Cl11 Hg5 -2.90(5) . . . . ? Cl14 Hg6 Cl12 Hg6 136(100) . . . 2_666 ? Cl13 Hg6 Cl12 Hg6 -61(100) . . . 2_666 ? Cl11 Hg6 Cl12 Hg6 37(100) . . . 2_666 ? C3A C1A C2A C3A -0.1(14) 2_665 . . . ? N1A C1A C2A C3A -179.6(7) . . . . ? C1A C2A C3A C1A 0.1(14) . . . 2_665 ? C3B C1B C2B C3B -0.2(13) 2_556 . . . ? N1B C1B C2B C3B -179.6(7) . . . . ? C1B C2B C3B C1B 0.2(13) . . . 2_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1CA Cl14 0.91 2.47 3.241(7) 142.2 2_666 N1A H1CA Cl5 0.91 2.80 3.417(8) 126.5 2_766 N1A H1AA O1A 0.91 1.89 2.793(9) 173.0 . N1A H1BA Cl11 0.91 2.41 3.216(8) 146.9 2_666 N1B H1AB Cl13 0.91 2.57 3.331(8) 141.4 2_666 N1B H1AB Cl10 0.91 2.89 3.338(8) 111.5 2_566 N1B H1BB Cl9 0.91 2.36 3.205(7) 153.9 2_666 N1B H1CB O1B 0.91 1.91 2.803(10) 166.5 . _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.382 _refine_diff_density_min -1.679 _refine_diff_density_rms 0.278 data_2+PbCl4 _database_code_depnum_ccdc_archive 'CCDC 659016' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H14 Cl4 N2 Pb' _chemical_formula_weight 487.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.8696(5) _cell_length_b 11.4163(11) _cell_length_c 21.257(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.871(7) _cell_angle_gamma 90.00 _cell_volume 1416.9(2) _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 prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 12.634 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.41 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 24732 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 30.00 _reflns_number_total 4086 _reflns_number_gt 3175 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0319P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00340(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4086 _refine_ls_number_parameters 144 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0369 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _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 Pb1 Pb 0.30409(2) 0.067760(12) 0.731017(7) 0.02629(6) Uani 1 1 d . . . Cl1 Cl 0.26243(18) 0.05842(10) 0.60493(5) 0.0390(2) Uani 1 1 d . . . Cl2 Cl 0.80436(17) 0.07097(10) 0.72744(5) 0.0422(2) Uani 1 1 d . . . Cl3 Cl 0.2940(2) 0.30970(9) 0.73615(6) 0.0424(2) Uani 1 1 d . . . Cl4 Cl 0.46884(18) 0.06278(10) 0.87466(5) 0.0403(2) Uani 1 1 d . . . N1 N 1.2594(7) 0.1600(4) 0.16038(17) 0.0409(9) Uani 1 1 d . . . H1A H 1.3597 0.1020 0.1582 0.061 Uiso 1 1 calc R . . H1B H 1.1528 0.1385 0.1850 0.061 Uiso 1 1 calc R . . H1C H 1.3316 0.2234 0.1766 0.061 Uiso 1 1 calc R . . N2 N 0.8155(6) 0.2579(3) -0.08299(18) 0.0350(8) Uani 1 1 d D . . C1 C 1.1509(7) 0.1865(4) 0.09673(19) 0.0318(8) Uani 1 1 d . . . C2 C 1.2383(8) 0.2733(4) 0.0611(2) 0.0402(10) Uani 1 1 d . . . H2 H 1.3680 0.3150 0.0768 0.048 Uiso 1 1 calc R . . C3 C 1.1293(8) 0.2975(4) 0.0013(2) 0.0405(10) Uani 1 1 d . . . H3 H 1.1837 0.3563 -0.0235 0.049 Uiso 1 1 calc R . . C4 C 0.9393(7) 0.2327(4) -0.0206(2) 0.0321(9) Uani 1 1 d . . . C5 C 0.8536(8) 0.1466(4) 0.0153(2) 0.0405(10) Uani 1 1 d . . . H5 H 0.7247 0.1043 -0.0004 0.049 Uiso 1 1 calc R . . C6 C 0.9611(8) 0.1231(4) 0.0754(2) 0.0388(10) Uani 1 1 d . . . H6 H 0.9048 0.0654 0.1006 0.047 Uiso 1 1 calc R . . C7 C 0.6831(9) 0.3697(5) -0.0813(3) 0.0528(13) Uani 1 1 d . . . H7A H 0.5845 0.3660 -0.0480 0.079 Uiso 1 1 calc R . . H7B H 0.5924 0.3808 -0.1210 0.079 Uiso 1 1 calc R . . H7C H 0.7874 0.4341 -0.0737 0.079 Uiso 1 1 calc R . . C8 C 0.9625(9) 0.2573(5) -0.1360(2) 0.0479(12) Uani 1 1 d . . . H8A H 1.0583 0.3256 -0.1334 0.072 Uiso 1 1 calc R . . H8B H 0.8674 0.2576 -0.1756 0.072 Uiso 1 1 calc R . . H8C H 1.0564 0.1883 -0.1334 0.072 Uiso 1 1 calc R . . H2N H 0.703(8) 0.196(4) -0.099(3) 0.08(2) Uiso 1 1 d 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02385(8) 0.02147(8) 0.03309(9) 0.00041(6) 0.00068(5) 0.00065(6) Cl1 0.0366(5) 0.0445(6) 0.0360(6) 0.0003(5) 0.0038(4) -0.0001(4) Cl2 0.0263(4) 0.0521(7) 0.0483(6) -0.0042(6) 0.0049(4) 0.0027(5) Cl3 0.0499(6) 0.0244(5) 0.0538(7) -0.0002(5) 0.0101(5) 0.0010(5) Cl4 0.0371(5) 0.0414(6) 0.0413(6) -0.0023(5) -0.0007(4) -0.0056(5) N1 0.041(2) 0.047(2) 0.033(2) -0.0012(17) -0.0029(15) 0.0025(17) N2 0.0333(18) 0.037(2) 0.034(2) 0.0015(15) 0.0005(15) 0.0002(15) C1 0.0283(18) 0.034(2) 0.033(2) -0.0036(17) 0.0009(15) 0.0023(17) C2 0.032(2) 0.042(3) 0.046(3) -0.004(2) -0.0008(18) -0.0110(18) C3 0.040(2) 0.039(3) 0.043(3) 0.010(2) 0.0068(19) -0.0079(19) C4 0.029(2) 0.035(2) 0.032(2) -0.0007(17) 0.0029(16) 0.0024(16) C5 0.035(2) 0.042(3) 0.043(3) -0.001(2) -0.0029(18) -0.0108(19) C6 0.042(2) 0.034(2) 0.040(3) 0.0019(19) 0.0011(19) -0.0093(19) C7 0.050(3) 0.057(3) 0.052(3) 0.012(3) 0.005(2) 0.023(2) C8 0.050(3) 0.060(3) 0.035(3) -0.004(2) 0.010(2) 0.000(2) _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 Pb1 Cl1 2.6684(11) . ? Pb1 Cl3 2.7651(11) . ? Pb1 Cl2 2.9266(10) 1_455 ? Pb1 Cl2 2.9454(10) . ? Cl2 Pb1 2.9266(10) 1_655 ? N1 C1 1.467(5) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N2 C4 1.473(5) . ? N2 C8 1.488(6) . ? N2 C7 1.498(6) . ? N2 H2N 1.002(10) . ? C1 C6 1.367(6) . ? C1 C2 1.377(6) . ? C2 C3 1.393(7) . ? C2 H2 0.9300 . ? C3 C4 1.379(6) . ? C3 H3 0.9300 . ? C4 C5 1.371(6) . ? C5 C6 1.392(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 Cl1 Pb1 Cl3 94.55(4) . . ? Cl1 Pb1 Cl2 89.18(3) . 1_455 ? Cl3 Pb1 Cl2 87.89(3) . 1_455 ? Cl1 Pb1 Cl2 87.92(3) . . ? Cl3 Pb1 Cl2 90.80(3) . . ? Cl2 Pb1 Cl2 176.72(5) 1_455 . ? Pb1 Cl2 Pb1 176.72(5) 1_655 . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C4 N2 C8 114.2(4) . . ? C4 N2 C7 110.7(4) . . ? C8 N2 C7 111.4(4) . . ? C4 N2 H2N 115(4) . . ? C8 N2 H2N 98(4) . . ? C7 N2 H2N 106(4) . . ? C6 C1 C2 122.4(4) . . ? C6 C1 N1 117.3(4) . . ? C2 C1 N1 120.3(4) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 118.8(4) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 121.8(4) . . ? C5 C4 N2 117.7(4) . . ? C3 C4 N2 120.4(4) . . ? C4 C5 C6 119.5(4) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 118.6(4) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pb1 Cl2 Pb1 -151.9(8) . . . 1_655 ? Cl3 Pb1 Cl2 Pb1 113.6(8) . . . 1_655 ? Cl2 Pb1 Cl2 Pb1 179.999(11) 1_455 . . 1_655 ? C6 C1 C2 C3 0.1(7) . . . . ? N1 C1 C2 C3 -179.0(4) . . . . ? C1 C2 C3 C4 -0.8(7) . . . . ? C2 C3 C4 C5 0.9(7) . . . . ? C2 C3 C4 N2 178.3(4) . . . . ? C8 N2 C4 C5 -128.4(5) . . . . ? C7 N2 C4 C5 104.8(5) . . . . ? C8 N2 C4 C3 54.1(6) . . . . ? C7 N2 C4 C3 -72.6(5) . . . . ? C3 C4 C5 C6 -0.3(7) . . . . ? N2 C4 C5 C6 -177.8(4) . . . . ? C2 C1 C6 C5 0.5(7) . . . . ? N1 C1 C6 C5 179.7(4) . . . . ? C4 C5 C6 C1 -0.4(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Cl4 0.89 2.28 3.132(4) 161.0 3_756 N1 H1B Cl3 0.89 2.54 3.328(4) 148.4 4_665 N1 H1C Cl2 0.89 2.60 3.385(4) 148.1 4_665 N1 H1C Cl3 0.89 2.90 3.395(4) 116.8 4_765 N2 H2N Cl4 1.002(10) 2.089(12) 3.088(4) 175(5) 1_554 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.043 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.217 data_2+Hg4Cl10+H2O _database_code_depnum_ccdc_archive 'CCDC 659017' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H14 Cl10 Hg4 N2 O' _chemical_formula_weight 1311.07 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' O O 0.0106 0.0060 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.0672(11) _cell_length_b 19.9418(15) _cell_length_c 11.9459(17) _cell_angle_alpha 90.00 _cell_angle_beta 107.754(11) _cell_angle_gamma 90.00 _cell_volume 2510.9(5) _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 prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 25.449 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.01 _exptl_absorpt_correction_T_max 0.31 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 39980 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7225 _reflns_number_gt 3998 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0274P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00073(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7225 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.002 _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 Hg1 Hg 0.21764(3) 0.582968(12) 0.40352(3) 0.04742(9) Uani 1 1 d . . . Hg2 Hg 0.51747(3) 0.519884(12) 0.69954(3) 0.04757(9) Uani 1 1 d . . . Hg3 Hg 0.13693(3) 0.474119(12) 0.67255(3) 0.04881(9) Uani 1 1 d . . . Hg4 Hg 0.17344(3) 0.521219(13) 1.01334(3) 0.05264(9) Uani 1 1 d . . . Cl1 Cl 0.2925(2) 0.47574(8) 0.46241(16) 0.0491(5) Uani 1 1 d . . . Cl2 Cl 0.16562(19) 0.69443(7) 0.36287(15) 0.0472(5) Uani 1 1 d . . . Cl3 Cl 0.5981(2) 0.41287(8) 0.74748(17) 0.0510(5) Uani 1 1 d . . . Cl4 Cl 0.45689(19) 0.62559(8) 0.62372(15) 0.0456(4) Uani 1 1 d . . . Cl5 Cl 0.34872(17) 0.50843(7) 0.84210(14) 0.0401(4) Uani 1 1 d . . . Cl6 Cl 0.1646(2) 0.35816(7) 0.64741(14) 0.0468(5) Uani 1 1 d . . . Cl7 Cl 0.08472(19) 0.58214(8) 0.59309(16) 0.0493(5) Uani 1 1 d . . . Cl8 Cl -0.01310(18) 0.46061(9) 0.81482(15) 0.0471(4) Uani 1 1 d . . . Cl9 Cl 0.2646(2) 0.42432(8) 1.10606(16) 0.0513(5) Uani 1 1 d . . . Cl10 Cl 0.11058(18) 0.62891(8) 0.94882(16) 0.0463(4) Uani 1 1 d . . . O1S O 0.7536(7) 0.2474(3) 0.3716(5) 0.081(2) Uani 1 1 d . . . N1 N 0.6816(5) 0.3298(2) 1.1792(5) 0.0395(14) Uani 1 1 d . . . H1A H 0.7008 0.3046 1.2437 0.059 Uiso 1 1 calc R . . H1B H 0.6762 0.3726 1.1985 0.059 Uiso 1 1 calc R . . H1C H 0.7419 0.3255 1.1446 0.059 Uiso 1 1 calc R . . N2 N 0.2042(7) 0.2598(3) 0.8644(6) 0.0584(18) Uani 1 1 d . . . H2A H 0.1914 0.2888 0.8031 0.070 Uiso 1 1 calc R . . C1 C 0.5610(7) 0.3084(3) 1.0989(5) 0.0335(15) Uani 1 1 d . . . C2 C 0.4997(8) 0.2532(4) 1.1221(7) 0.053(2) Uani 1 1 d . . . H2 H 0.5354 0.2273 1.1887 0.064 Uiso 1 1 calc R . . C3 C 0.3796(9) 0.2365(4) 1.0417(8) 0.062(2) Uani 1 1 d . . . H3 H 0.3339 0.1998 1.0550 0.074 Uiso 1 1 calc R . . C4 C 0.3339(7) 0.2753(4) 0.9454(6) 0.0459(18) Uani 1 1 d . . . C5 C 0.3958(9) 0.3278(4) 0.9228(7) 0.062(2) Uani 1 1 d . . . H5 H 0.3611 0.3528 0.8549 0.075 Uiso 1 1 calc R . . C6 C 0.5103(9) 0.3452(4) 0.9990(6) 0.055(2) Uani 1 1 d . . . H6 H 0.5540 0.3820 0.9832 0.066 Uiso 1 1 calc R . . C7 C 0.1927(9) 0.1907(3) 0.8116(7) 0.073(3) Uani 1 1 d . . . H7A H 0.2489 0.1867 0.7646 0.110 Uiso 1 1 calc R . . H7C H 0.1069 0.1834 0.7632 0.110 Uiso 1 1 calc R . . H7B H 0.2149 0.1579 0.8733 0.110 Uiso 1 1 calc R . . C8 C 0.1003(8) 0.2725(4) 0.9155(7) 0.063(2) Uani 1 1 d . . . H8A H 0.1037 0.2400 0.9755 0.095 Uiso 1 1 calc R . . H8B H 0.0202 0.2693 0.8550 0.095 Uiso 1 1 calc R . . H8C H 0.1095 0.3167 0.9491 0.095 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 Hg1 0.0553(2) 0.03766(13) 0.05197(18) 0.00635(12) 0.02039(15) 0.00170(14) Hg2 0.0497(2) 0.03852(14) 0.05327(18) 0.00358(12) 0.01393(15) 0.00725(13) Hg3 0.0483(2) 0.03698(13) 0.06126(19) 0.00974(12) 0.01689(15) 0.00257(13) Hg4 0.0517(2) 0.03884(14) 0.06072(19) 0.00931(13) 0.00727(16) -0.00301(14) Cl1 0.0652(14) 0.0351(8) 0.0513(11) 0.0027(7) 0.0239(10) -0.0003(8) Cl2 0.0537(13) 0.0370(8) 0.0461(10) 0.0084(7) 0.0081(9) -0.0026(8) Cl3 0.0609(14) 0.0372(8) 0.0630(12) 0.0077(8) 0.0310(10) 0.0063(8) Cl4 0.0464(12) 0.0410(8) 0.0482(10) 0.0070(7) 0.0124(9) 0.0052(8) Cl5 0.0384(11) 0.0384(8) 0.0417(10) 0.0035(6) 0.0097(8) -0.0017(7) Cl6 0.0636(14) 0.0366(8) 0.0391(10) 0.0023(7) 0.0141(9) 0.0075(8) Cl7 0.0537(13) 0.0424(8) 0.0525(11) 0.0175(8) 0.0170(9) 0.0097(9) Cl8 0.0454(12) 0.0599(10) 0.0410(10) -0.0106(8) 0.0205(9) -0.0156(9) Cl9 0.0600(14) 0.0409(8) 0.0476(11) 0.0047(7) 0.0086(9) 0.0032(9) Cl10 0.0498(13) 0.0373(8) 0.0548(11) 0.0040(7) 0.0205(10) -0.0002(8) O1S 0.122(6) 0.066(3) 0.043(3) 0.010(3) 0.008(4) 0.032(4) N1 0.036(4) 0.034(3) 0.049(3) 0.003(2) 0.015(3) 0.005(3) N2 0.056(5) 0.059(4) 0.053(4) -0.001(3) 0.007(4) -0.004(3) C1 0.031(4) 0.042(3) 0.030(4) 0.001(3) 0.013(3) 0.002(3) C2 0.048(6) 0.058(4) 0.053(5) 0.014(4) 0.015(4) -0.009(4) C3 0.061(7) 0.056(5) 0.078(6) 0.002(4) 0.035(5) -0.019(4) C4 0.039(5) 0.062(4) 0.034(4) -0.007(3) 0.007(4) 0.008(4) C5 0.069(7) 0.065(5) 0.041(5) 0.006(4) -0.002(4) -0.005(5) C6 0.069(7) 0.054(4) 0.039(4) 0.004(3) 0.012(4) -0.004(4) C7 0.072(7) 0.055(5) 0.074(6) -0.022(4) -0.006(5) -0.010(4) C8 0.038(6) 0.092(6) 0.057(5) 0.009(4) 0.012(4) 0.008(5) _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 Hg1 Cl2 2.3103(15) . ? Hg1 Cl1 2.3234(16) . ? Hg2 Cl4 2.3114(16) . ? Hg2 Cl3 2.3165(16) . ? Hg2 Cl5 2.8948(17) . ? Hg3 Cl7 2.3540(15) . ? Hg3 Cl6 2.3638(15) . ? Hg3 Cl5 2.6775(18) . ? Hg3 Cl8 2.7274(17) . ? Hg4 Cl9 2.3015(17) . ? Hg4 Cl10 2.3159(16) . ? Hg4 Cl8 2.8916(18) . ? N1 C1 1.451(8) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N2 C8 1.479(10) . ? N2 C4 1.498(9) . ? N2 C7 1.504(8) . ? N2 H2A 0.9100 . ? C1 C2 1.364(9) . ? C1 C6 1.368(9) . ? C2 C3 1.422(11) . ? C2 H2 0.9300 . ? C3 C4 1.351(10) . ? C3 H3 0.9300 . ? C4 C5 1.322(10) . ? C5 C6 1.361(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7C 0.9600 . ? C7 H7B 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 Cl2 Hg1 Cl1 172.80(7) . . ? Cl4 Hg2 Cl3 168.75(6) . . ? Cl4 Hg2 Cl5 98.07(6) . . ? Cl3 Hg2 Cl5 92.91(5) . . ? Cl7 Hg3 Cl6 150.39(6) . . ? Cl7 Hg3 Cl5 97.00(6) . . ? Cl6 Hg3 Cl5 103.21(6) . . ? Cl7 Hg3 Cl8 102.74(6) . . ? Cl6 Hg3 Cl8 96.30(6) . . ? Cl5 Hg3 Cl8 96.47(5) . . ? Cl9 Hg4 Cl10 169.07(7) . . ? Cl9 Hg4 Cl8 98.18(6) . . ? Cl10 Hg4 Cl8 92.74(6) . . ? Hg3 Cl5 Hg2 98.52(5) . . ? Hg3 Cl8 Hg4 92.97(6) . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C8 N2 C4 114.2(6) . . ? C8 N2 C7 110.7(7) . . ? C4 N2 C7 113.8(6) . . ? C8 N2 H2A 105.8 . . ? C4 N2 H2A 105.8 . . ? C7 N2 H2A 105.8 . . ? C2 C1 C6 120.9(7) . . ? C2 C1 N1 121.2(6) . . ? C6 C1 N1 117.9(6) . . ? C1 C2 C3 118.2(7) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 118.1(7) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C5 C4 C3 123.0(8) . . ? C5 C4 N2 119.1(7) . . ? C3 C4 N2 117.8(7) . . ? C4 C5 C6 120.0(7) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.8(7) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? H7C C7 H7B 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl7 Hg3 Cl5 Hg2 -77.98(6) . . . . ? Cl6 Hg3 Cl5 Hg2 80.23(6) . . . . ? Cl8 Hg3 Cl5 Hg2 178.28(5) . . . . ? Cl4 Hg2 Cl5 Hg3 80.21(6) . . . . ? Cl3 Hg2 Cl5 Hg3 -97.35(6) . . . . ? Cl7 Hg3 Cl8 Hg4 -87.81(7) . . . . ? Cl6 Hg3 Cl8 Hg4 115.01(6) . . . . ? Cl5 Hg3 Cl8 Hg4 10.89(5) . . . . ? Cl9 Hg4 Cl8 Hg3 -96.66(7) . . . . ? Cl10 Hg4 Cl8 Hg3 82.90(6) . . . . ? C6 C1 C2 C3 -2.2(11) . . . . ? N1 C1 C2 C3 177.8(6) . . . . ? C1 C2 C3 C4 1.3(12) . . . . ? C2 C3 C4 C5 0.2(12) . . . . ? C2 C3 C4 N2 -176.7(7) . . . . ? C8 N2 C4 C5 -109.4(8) . . . . ? C7 N2 C4 C5 122.2(8) . . . . ? C8 N2 C4 C3 67.6(9) . . . . ? C7 N2 C4 C3 -60.8(9) . . . . ? C3 C4 C5 C6 -0.8(13) . . . . ? N2 C4 C5 C6 176.0(7) . . . . ? C4 C5 C6 C1 -0.1(12) . . . . ? C2 C1 C6 C5 1.6(11) . . . . ? N1 C1 C6 C5 -178.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1S 0.89 1.85 2.740(7) 173.6 1_556 N1 H1B Cl5 0.89 2.42 3.244(5) 154.1 3_667 N1 H1C Cl10 0.89 2.42 3.232(6) 152.3 3_667 N1 H1C Cl2 0.89 2.82 3.305(5) 115.8 2_646 N2 H2A Cl6 0.91 2.26 3.174(7) 177.6 . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.402 _refine_diff_density_min -2.020 _refine_diff_density_rms 0.261 data_3+PbCl6+H2O _database_code_depnum_ccdc_archive 'CCDC 659018' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H38 Cl6 N4 O Pb' _chemical_formula_weight 770.43 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' O O 0.0106 0.0060 '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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2479(3) _cell_length_b 11.3720(3) _cell_length_c 20.7255(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.632(2) _cell_angle_gamma 90.00 _cell_volume 2886.54(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 6.421 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.2122 _exptl_absorpt_correction_T_max 0.4082 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66967 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 28.72 _reflns_number_total 7228 _reflns_number_gt 6369 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0098P)^2^+0.9328P] 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 0.000497(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7228 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0146 _refine_ls_R_factor_gt 0.0109 _refine_ls_wR_factor_ref 0.0244 _refine_ls_wR_factor_gt 0.0242 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.006 _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 Pb1 Pb 0.481001(4) 0.509315(4) 0.251776(2) 0.00917(2) Uani 1 1 d . . . Cl1 Cl 0.69744(3) 0.46005(3) 0.251406(17) 0.01281(7) Uani 1 1 d . . . Cl2 Cl 0.55261(3) 0.76331(3) 0.222133(18) 0.01468(7) Uani 1 1 d . . . Cl3 Cl 0.47497(3) 0.44595(3) 0.113270(17) 0.01455(7) Uani 1 1 d . . . Cl4 Cl 0.23430(3) 0.53451(3) 0.255505(17) 0.01359(7) Uani 1 1 d . . . Cl5 Cl 0.44285(3) 0.28365(3) 0.280119(18) 0.01507(7) Uani 1 1 d . . . Cl6 Cl 0.51139(3) 0.56479(3) 0.388114(17) 0.01391(7) Uani 1 1 d . . . N1A N 0.69193(10) 0.20030(10) 0.31003(5) 0.0108(2) Uani 1 1 d . . . H1A1 H 0.6419 0.1454 0.2977 0.016 Uiso 1 1 calc R . . H1A2 H 0.7569 0.1848 0.2909 0.016 Uiso 1 1 calc R . . H1A3 H 0.6682 0.2729 0.2979 0.016 Uiso 1 1 calc R . . N2A N 0.75496(10) 0.18005(11) 0.58134(6) 0.0127(3) Uani 1 1 d . . . H2A H 0.8167 0.1336 0.5876 0.015 Uiso 1 1 calc R . . C1A C 0.70619(12) 0.19673(12) 0.38036(7) 0.0103(3) Uani 1 1 d . . . C2A C 0.63525(12) 0.25812(12) 0.41951(7) 0.0124(3) Uani 1 1 d . . . H2A1 H 0.5769 0.3025 0.4013 0.015 Uiso 1 1 calc R . . C3A C 0.65088(12) 0.25368(13) 0.48599(7) 0.0135(3) Uani 1 1 d . . . H3A H 0.6035 0.2953 0.5139 0.016 Uiso 1 1 calc R . . C4A C 0.73678(12) 0.18744(12) 0.51102(7) 0.0112(3) Uani 1 1 d . . . C5A C 0.80740(12) 0.12662(12) 0.47165(7) 0.0123(3) Uani 1 1 d . . . H5A H 0.8658 0.0822 0.4898 0.015 Uiso 1 1 calc R . . C6A C 0.79189(12) 0.13131(12) 0.40514(7) 0.0118(3) Uani 1 1 d . . . H6A H 0.8395 0.0902 0.3772 0.014 Uiso 1 1 calc R . . C7A C 0.77917(14) 0.29719(14) 0.61322(8) 0.0183(3) Uani 1 1 d . . . H7A1 H 0.7122 0.3459 0.6126 0.022 Uiso 1 1 calc R . . H7A2 H 0.8004 0.2837 0.6588 0.022 Uiso 1 1 calc R . . C8A C 0.86937(14) 0.36278(14) 0.57985(8) 0.0233(4) Uani 1 1 d . . . H8A1 H 0.9323 0.3106 0.5745 0.035 Uiso 1 1 calc R . . H8A2 H 0.8910 0.4309 0.6060 0.035 Uiso 1 1 calc R . . H8A3 H 0.8434 0.3895 0.5374 0.035 Uiso 1 1 calc R . . C9A C 0.66345(13) 0.11984(14) 0.61630(7) 0.0176(3) Uani 1 1 d . . . H9A1 H 0.5978 0.1706 0.6147 0.021 Uiso 1 1 calc R . . H9A2 H 0.6847 0.1095 0.6622 0.021 Uiso 1 1 calc R . . C10A C 0.63543(14) 0.00128(14) 0.58772(8) 0.0232(3) Uani 1 1 d . . . H10A H 0.6013 0.0122 0.5451 0.035 Uiso 1 1 calc R . . H10B H 0.5846 -0.0398 0.6161 0.035 Uiso 1 1 calc R . . H10C H 0.7022 -0.0454 0.5833 0.035 Uiso 1 1 calc R . . N1B N 0.19086(10) 0.28575(10) 0.31896(6) 0.0115(2) Uani 1 1 d . . . H1B1 H 0.2314 0.2244 0.3044 0.017 Uiso 1 1 calc R . . H1B2 H 0.2135 0.3534 0.2998 0.017 Uiso 1 1 calc R . . H1B3 H 0.1192 0.2731 0.3091 0.017 Uiso 1 1 calc R . . N2B N 0.25566(10) 0.32037(11) 0.59004(6) 0.0130(3) Uani 1 1 d . . . H2B H 0.3187 0.3651 0.5955 0.016 Uiso 1 1 calc R . . C1B C 0.20449(12) 0.29607(12) 0.38923(7) 0.0106(3) Uani 1 1 d . . . C2B C 0.13441(12) 0.23623(12) 0.42960(7) 0.0123(3) Uani 1 1 d . . . H2B1 H 0.0763 0.1905 0.4121 0.015 Uiso 1 1 calc R . . C3B C 0.15010(12) 0.24376(12) 0.49601(7) 0.0124(3) Uani 1 1 d . . . H3B H 0.1034 0.2028 0.5246 0.015 Uiso 1 1 calc R . . C4B C 0.23529(12) 0.31226(12) 0.51974(7) 0.0114(3) Uani 1 1 d . . . C5B C 0.30422(12) 0.37324(12) 0.47932(7) 0.0131(3) Uani 1 1 d . . . H5B H 0.3616 0.4202 0.4967 0.016 Uiso 1 1 calc R . . C6B C 0.28860(12) 0.36506(12) 0.41311(7) 0.0126(3) Uani 1 1 d . . . H6B H 0.3351 0.4063 0.3845 0.015 Uiso 1 1 calc R . . C7B C 0.16623(13) 0.38326(14) 0.62593(7) 0.0186(3) Uani 1 1 d . . . H7B1 H 0.0997 0.3338 0.6255 0.022 Uiso 1 1 calc R . . H7B2 H 0.1893 0.3941 0.6715 0.022 Uiso 1 1 calc R . . C8B C 0.13950(15) 0.50165(14) 0.59686(8) 0.0243(4) Uani 1 1 d . . . H8B1 H 0.2071 0.5463 0.5908 0.036 Uiso 1 1 calc R . . H8B2 H 0.0913 0.5450 0.6258 0.036 Uiso 1 1 calc R . . H8B3 H 0.1028 0.4905 0.5550 0.036 Uiso 1 1 calc R . . C9B C 0.27788(14) 0.20230(14) 0.62164(8) 0.0195(4) Uani 1 1 d . . . H9B1 H 0.3022 0.2151 0.6668 0.023 Uiso 1 1 calc R . . H9B2 H 0.2094 0.1561 0.6225 0.023 Uiso 1 1 calc R . . C10B C 0.36408(14) 0.13329(14) 0.58637(9) 0.0239(4) Uani 1 1 d . . . H10D H 0.3344 0.1064 0.5448 0.036 Uiso 1 1 calc R . . H10E H 0.3860 0.0651 0.6124 0.036 Uiso 1 1 calc R . . H10F H 0.4277 0.1836 0.5790 0.036 Uiso 1 1 calc R . . O1S O 0.54231(10) 0.03035(11) 0.27366(7) 0.0252(3) Uani 1 1 d . . . H1SA H 0.5512(18) -0.030(2) 0.2592(10) 0.039(7) Uiso 1 1 d . . . H1SB H 0.4786(19) 0.049(2) 0.2626(10) 0.044(7) Uiso 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.00876(3) 0.00898(3) 0.00974(3) -0.00032(2) -0.00076(2) -0.00020(2) Cl1 0.01055(17) 0.01296(16) 0.01492(17) 0.00039(13) 0.00006(13) 0.00003(12) Cl2 0.01197(18) 0.01226(16) 0.01975(19) -0.00021(13) -0.00188(14) -0.00004(13) Cl3 0.01313(18) 0.01775(17) 0.01271(17) -0.00090(13) -0.00204(13) -0.00432(13) Cl4 0.01449(18) 0.01209(16) 0.01416(17) -0.00082(13) -0.00130(13) 0.00124(13) Cl5 0.01214(18) 0.01020(16) 0.02287(19) 0.00099(14) -0.00024(14) -0.00002(13) Cl6 0.01217(18) 0.01686(17) 0.01269(17) -0.00274(13) -0.00026(13) -0.00331(13) N1A 0.0112(6) 0.0119(6) 0.0092(6) 0.0004(5) -0.0001(5) 0.0013(5) N2A 0.0131(7) 0.0163(6) 0.0088(6) -0.0013(5) -0.0014(5) 0.0052(5) C1A 0.0125(8) 0.0103(7) 0.0080(7) 0.0008(5) -0.0008(6) -0.0028(5) C2A 0.0102(7) 0.0131(7) 0.0138(7) 0.0008(6) -0.0019(6) 0.0032(5) C3A 0.0129(8) 0.0154(7) 0.0123(7) -0.0016(6) 0.0014(6) 0.0038(6) C4A 0.0115(7) 0.0136(7) 0.0084(7) 0.0003(5) -0.0010(6) -0.0003(5) C5A 0.0106(8) 0.0132(7) 0.0131(7) 0.0009(6) -0.0012(6) 0.0031(5) C6A 0.0117(8) 0.0122(7) 0.0115(7) -0.0011(6) 0.0018(6) 0.0016(5) C7A 0.0214(9) 0.0190(8) 0.0143(8) -0.0066(6) -0.0039(7) 0.0056(6) C8A 0.0214(9) 0.0202(8) 0.0280(10) -0.0051(7) -0.0037(7) 0.0005(7) C9A 0.0184(9) 0.0235(8) 0.0108(8) 0.0036(6) 0.0032(6) 0.0047(6) C10A 0.0257(9) 0.0230(9) 0.0210(8) 0.0041(7) 0.0037(7) -0.0002(7) N1B 0.0113(6) 0.0132(6) 0.0100(6) -0.0006(5) -0.0008(5) -0.0003(5) N2B 0.0137(7) 0.0165(6) 0.0089(6) 0.0005(5) -0.0014(5) -0.0059(5) C1B 0.0119(8) 0.0114(7) 0.0084(7) -0.0005(5) -0.0012(6) 0.0031(5) C2B 0.0102(7) 0.0128(7) 0.0138(7) -0.0017(6) -0.0020(6) -0.0025(5) C3B 0.0117(8) 0.0142(7) 0.0113(7) 0.0018(6) 0.0014(6) -0.0025(6) C4B 0.0119(7) 0.0132(7) 0.0092(7) -0.0013(5) -0.0012(6) 0.0009(5) C5B 0.0113(8) 0.0143(7) 0.0137(7) -0.0005(6) -0.0019(6) -0.0039(6) C6B 0.0123(8) 0.0135(7) 0.0120(7) 0.0013(6) 0.0013(6) -0.0022(5) C7B 0.0185(9) 0.0259(8) 0.0116(8) -0.0044(6) 0.0032(6) -0.0052(7) C8B 0.0285(9) 0.0216(9) 0.0227(8) -0.0073(7) 0.0044(7) -0.0010(7) C9B 0.0240(9) 0.0210(8) 0.0135(8) 0.0077(6) -0.0060(7) -0.0078(7) C10B 0.0224(9) 0.0187(8) 0.0304(10) 0.0061(7) -0.0070(7) -0.0013(7) O1S 0.0168(7) 0.0155(6) 0.0432(8) -0.0105(6) -0.0035(6) 0.0027(5) _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 Pb1 Cl5 2.6750(4) . ? Pb1 Cl1 2.7096(4) . ? Pb1 Cl6 2.9151(4) . ? Pb1 Cl3 2.9598(4) . ? Pb1 Cl4 3.0369(4) . ? Pb1 Cl2 3.0824(4) . ? N1A C1A 1.4669(18) . ? N1A H1A1 0.9100 . ? N1A H1A2 0.9100 . ? N1A H1A3 0.9100 . ? N2A C4A 1.4743(18) . ? N2A C9A 1.5060(19) . ? N2A C7A 1.5148(19) . ? N2A H2A 0.9300 . ? C1A C6A 1.381(2) . ? C1A C2A 1.384(2) . ? C2A C3A 1.390(2) . ? C2A H2A1 0.9500 . ? C3A C4A 1.390(2) . ? C3A H3A 0.9500 . ? C4A C5A 1.3814(19) . ? C5A C6A 1.390(2) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A C8A 1.507(2) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A C10A 1.511(2) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? N1B C1B 1.4687(18) . ? N1B H1B1 0.9100 . ? N1B H1B2 0.9100 . ? N1B H1B3 0.9100 . ? N2B C4B 1.4783(18) . ? N2B C7B 1.5107(19) . ? N2B C9B 1.5173(19) . ? N2B H2B 0.9300 . ? C1B C6B 1.382(2) . ? C1B C2B 1.384(2) . ? C2B C3B 1.390(2) . ? C2B H2B1 0.9500 . ? C3B C4B 1.388(2) . ? C3B H3B 0.9500 . ? C4B C5B 1.382(2) . ? C5B C6B 1.386(2) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B C8B 1.510(2) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B C10B 1.511(2) . ? C9B H9B1 0.9900 . ? C9B H9B2 0.9900 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? O1S H1SA 0.76(2) . ? O1S H1SB 0.84(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 Cl5 Pb1 Cl1 88.597(11) . . ? Cl5 Pb1 Cl6 90.889(11) . . ? Cl1 Pb1 Cl6 86.160(10) . . ? Cl5 Pb1 Cl3 88.675(11) . . ? Cl1 Pb1 Cl3 87.757(10) . . ? Cl6 Pb1 Cl3 173.910(10) . . ? Cl5 Pb1 Cl4 84.760(10) . . ? Cl1 Pb1 Cl4 173.356(10) . . ? Cl6 Pb1 Cl4 94.092(10) . . ? Cl3 Pb1 Cl4 91.918(10) . . ? Cl5 Pb1 Cl2 173.482(10) . . ? Cl1 Pb1 Cl2 84.990(10) . . ? Cl6 Pb1 Cl2 87.526(10) . . ? Cl3 Pb1 Cl2 92.231(10) . . ? Cl4 Pb1 Cl2 101.654(9) . . ? C1A N1A H1A1 109.5 . . ? C1A N1A H1A2 109.5 . . ? H1A1 N1A H1A2 109.5 . . ? C1A N1A H1A3 109.5 . . ? H1A1 N1A H1A3 109.5 . . ? H1A2 N1A H1A3 109.5 . . ? C4A N2A C9A 113.36(11) . . ? C4A N2A C7A 114.06(11) . . ? C9A N2A C7A 109.46(11) . . ? C4A N2A H2A 106.5 . . ? C9A N2A H2A 106.5 . . ? C7A N2A H2A 106.5 . . ? C6A C1A C2A 122.22(13) . . ? C6A C1A N1A 117.78(13) . . ? C2A C1A N1A 120.00(13) . . ? C1A C2A C3A 118.83(13) . . ? C1A C2A H2A1 120.6 . . ? C3A C2A H2A1 120.6 . . ? C4A C3A C2A 119.02(13) . . ? C4A C3A H3A 120.5 . . ? C2A C3A H3A 120.5 . . ? C5A C4A C3A 121.83(13) . . ? C5A C4A N2A 117.82(12) . . ? C3A C4A N2A 120.35(13) . . ? C4A C5A C6A 119.13(13) . . ? C4A C5A H5A 120.4 . . ? C6A C5A H5A 120.4 . . ? C1A C6A C5A 118.96(13) . . ? C1A C6A H6A 120.5 . . ? C5A C6A H6A 120.5 . . ? C8A C7A N2A 112.09(12) . . ? C8A C7A H7A1 109.2 . . ? N2A C7A H7A1 109.2 . . ? C8A C7A H7A2 109.2 . . ? N2A C7A H7A2 109.2 . . ? H7A1 C7A H7A2 107.9 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? N2A C9A C10A 112.59(12) . . ? N2A C9A H9A1 109.1 . . ? C10A C9A H9A1 109.1 . . ? N2A C9A H9A2 109.1 . . ? C10A C9A H9A2 109.1 . . ? H9A1 C9A H9A2 107.8 . . ? C9A C10A H10A 109.5 . . ? C9A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C1B N1B H1B1 109.5 . . ? C1B N1B H1B2 109.5 . . ? H1B1 N1B H1B2 109.5 . . ? C1B N1B H1B3 109.5 . . ? H1B1 N1B H1B3 109.5 . . ? H1B2 N1B H1B3 109.5 . . ? C4B N2B C7B 113.54(12) . . ? C4B N2B C9B 113.44(11) . . ? C7B N2B C9B 109.51(12) . . ? C4B N2B H2B 106.6 . . ? C7B N2B H2B 106.6 . . ? C9B N2B H2B 106.6 . . ? C6B C1B C2B 121.83(13) . . ? C6B C1B N1B 118.46(13) . . ? C2B C1B N1B 119.71(13) . . ? C1B C2B C3B 119.23(13) . . ? C1B C2B H2B1 120.4 . . ? C3B C2B H2B1 120.4 . . ? C4B C3B C2B 118.72(13) . . ? C4B C3B H3B 120.6 . . ? C2B C3B H3B 120.6 . . ? C5B C4B C3B 121.91(13) . . ? C5B C4B N2B 117.93(12) . . ? C3B C4B N2B 120.16(13) . . ? C4B C5B C6B 119.18(13) . . ? C4B C5B H5B 120.4 . . ? C6B C5B H5B 120.4 . . ? C1B C6B C5B 119.12(13) . . ? C1B C6B H6B 120.4 . . ? C5B C6B H6B 120.4 . . ? C8B C7B N2B 112.39(13) . . ? C8B C7B H7B1 109.1 . . ? N2B C7B H7B1 109.1 . . ? C8B C7B H7B2 109.1 . . ? N2B C7B H7B2 109.1 . . ? H7B1 C7B H7B2 107.9 . . ? C7B C8B H8B1 109.5 . . ? C7B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C10B C9B N2B 111.95(13) . . ? C10B C9B H9B1 109.2 . . ? N2B C9B H9B1 109.2 . . ? C10B C9B H9B2 109.2 . . ? N2B C9B H9B2 109.2 . . ? H9B1 C9B H9B2 107.9 . . ? C9B C10B H10D 109.5 . . ? C9B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C9B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? H1SA O1S H1SB 105(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A C1A C2A C3A 0.0(2) . . . . ? N1A C1A C2A C3A -179.71(13) . . . . ? C1A C2A C3A C4A -0.3(2) . . . . ? C2A C3A C4A C5A 0.4(2) . . . . ? C2A C3A C4A N2A -179.44(13) . . . . ? C9A N2A C4A C5A -115.20(14) . . . . ? C7A N2A C4A C5A 118.63(14) . . . . ? C9A N2A C4A C3A 64.68(17) . . . . ? C7A N2A C4A C3A -61.48(18) . . . . ? C3A C4A C5A C6A -0.3(2) . . . . ? N2A C4A C5A C6A 179.59(13) . . . . ? C2A C1A C6A C5A 0.2(2) . . . . ? N1A C1A C6A C5A 179.87(12) . . . . ? C4A C5A C6A C1A 0.0(2) . . . . ? C4A N2A C7A C8A -51.08(17) . . . . ? C9A N2A C7A C8A -179.26(13) . . . . ? C4A N2A C9A C10A 52.14(16) . . . . ? C7A N2A C9A C10A -179.29(13) . . . . ? C6B C1B C2B C3B -1.2(2) . . . . ? N1B C1B C2B C3B 178.06(12) . . . . ? C1B C2B C3B C4B 0.6(2) . . . . ? C2B C3B C4B C5B 0.3(2) . . . . ? C2B C3B C4B N2B -178.80(13) . . . . ? C7B N2B C4B C5B 113.64(15) . . . . ? C9B N2B C4B C5B -120.50(14) . . . . ? C7B N2B C4B C3B -67.24(17) . . . . ? C9B N2B C4B C3B 58.63(18) . . . . ? C3B C4B C5B C6B -0.6(2) . . . . ? N2B C4B C5B C6B 178.52(13) . . . . ? C2B C1B C6B C5B 0.9(2) . . . . ? N1B C1B C6B C5B -178.36(13) . . . . ? C4B C5B C6B C1B 0.0(2) . . . . ? C4B N2B C7B C8B -51.87(17) . . . . ? C9B N2B C7B C8B -179.80(13) . . . . ? C4B N2B C9B C10B 50.01(17) . . . . ? C7B N2B C9B C10B 178.00(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A1 O1S 0.91 1.85 2.7624(17) 178.4 . N1A H1A2 Cl2 0.91 2.52 3.2854(13) 142.6 2_645 N1A H1A2 Cl1 0.91 2.76 3.3106(12) 119.9 2_645 N1A H1A3 Cl1 0.91 2.37 3.1949(12) 151.6 . N1A H1A3 Cl5 0.91 2.78 3.2477(12) 112.9 . N2A H2A Cl3 0.93 2.20 3.1166(13) 168.6 4_666 N1B H1B1 Cl4 0.91 2.53 3.3788(12) 155.8 2_545 N1B H1B1 Cl5 0.91 2.73 3.1983(13) 113.3 . N1B H1B2 Cl4 0.91 2.27 3.1672(12) 168.2 . N1B H1B3 Cl2 0.91 2.20 3.1027(13) 172.6 2_545 N2B H2B Cl6 0.93 2.25 3.1658(13) 167.6 3_666 O1S H1SA Cl2 0.76(2) 2.47(2) 3.2221(13) 170(2) 1_545 O1S H1SB Cl4 0.84(2) 2.64(2) 3.4352(13) 160(2) 2_545 O1S H1SB Cl5 0.84(2) 2.73(2) 3.1309(13) 111.4(19) . _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.702 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.062 data_4+CuCl4 _database_code_depnum_ccdc_archive 'CCDC 659019' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H20 Cl4 Cu N2' _chemical_formula_weight 385.63 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.7932(6) _cell_length_b 11.6083(4) _cell_length_c 7.8582(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1623.10(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 1.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 21369 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 28.64 _reflns_number_total 3967 _reflns_number_gt 3739 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0261P)^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 SHELXL _refine_ls_extinction_coef 0.0028(3) _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, 1791 Friedel pairs' _refine_ls_abs_structure_Flack 0.005(6) _refine_ls_number_reflns 3967 _refine_ls_number_parameters 223 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0400 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.065 _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 Cu1 Cu 0.443568(9) 0.200929(14) 0.34655(2) 0.01686(5) Uani 1 1 d . . . Cl1 Cl 0.37311(2) 0.28520(3) 0.13478(4) 0.01968(8) Uani 1 1 d . . . Cl2 Cl 0.55437(2) 0.23213(3) 0.46548(5) 0.02083(8) Uani 1 1 d . . . Cl3 Cl 0.37036(2) 0.25428(3) 0.56464(5) 0.01984(8) Uani 1 1 d . . . Cl4 Cl 0.46701(2) 0.04012(3) 0.19922(5) 0.02540(9) Uani 1 1 d . . . N2 N -0.00458(6) 0.29256(9) -0.14766(17) 0.0140(2) Uani 1 1 d . . . H2A H -0.0439 0.2776 -0.0769 0.021 Uiso 1 1 calc R . . H2B H -0.0160 0.2681 -0.2546 0.021 Uiso 1 1 calc R . . H2C H 0.0045 0.3697 -0.1494 0.021 Uiso 1 1 calc R . . C1 C 0.18637(8) 0.12091(13) 0.03402(19) 0.0197(3) Uani 1 1 d . . . C2 C 0.12995(9) 0.05772(14) -0.0412(2) 0.0197(3) Uani 1 1 d . A . C3 C 0.06624(8) 0.11263(13) -0.10421(18) 0.0169(3) Uani 1 1 d . . . C4 C 0.06257(8) 0.23180(13) -0.08649(19) 0.0147(3) Uani 1 1 d . A . C5 C 0.11885(9) 0.29525(14) -0.0108(2) 0.0189(3) Uani 1 1 d . . . C6 C 0.18212(9) 0.23940(14) 0.0509(2) 0.0224(3) Uani 1 1 d . A . C7 C 0.28902(9) -0.02624(15) -0.0096(2) 0.0269(4) Uani 1 1 d . . . C8 C 0.31351(10) 0.02701(18) -0.1731(3) 0.0348(4) Uani 1 1 d . A . N1A N 0.25283(7) 0.06052(13) 0.10633(16) 0.0236(3) Uani 0.860(3) 1 d PD A 1 H1A H 0.2887 0.1160 0.1326 0.028 Uiso 0.860(3) 1 calc PR A 1 C9A C 0.23346(11) -0.00457(17) 0.2720(2) 0.0233(4) Uani 0.860(3) 1 d PDU A 1 H9A1 H 0.1962 -0.0655 0.2467 0.028 Uiso 0.860(3) 1 calc PR A 1 H9A2 H 0.2793 -0.0423 0.3165 0.028 Uiso 0.860(3) 1 calc PR A 1 C10A C 0.20222(11) 0.0748(2) 0.4054(2) 0.0271(5) Uani 0.860(3) 1 d PDU A 1 H10A H 0.2397 0.1337 0.4334 0.041 Uiso 0.860(3) 1 calc PR A 1 H10B H 0.1900 0.0304 0.5078 0.041 Uiso 0.860(3) 1 calc PR A 1 H10C H 0.1566 0.1119 0.3620 0.041 Uiso 0.860(3) 1 calc PR A 1 N1B N 0.25283(7) 0.06052(13) 0.10633(16) 0.0236(3) Uani 0.14 1 d PD A 2 H1B H 0.2864 0.1192 0.0799 0.028 Uiso 0.140(3) 1 calc PR A 2 C9B C 0.2553(6) 0.0828(9) 0.3020(9) 0.0225(11) Uani 0.140(3) 1 d PDU A 2 H9B1 H 0.3044 0.0610 0.3517 0.027 Uiso 0.140(3) 1 calc PR A 2 H9B2 H 0.2441 0.1642 0.3299 0.027 Uiso 0.140(3) 1 calc PR A 2 C10B C 0.1939(6) 0.0041(10) 0.3588(16) 0.0223(19) Uani 0.140(3) 1 d PDU A 2 H10D H 0.1453 0.0426 0.3448 0.033 Uiso 0.140(3) 1 calc PR A 2 H10E H 0.2013 -0.0156 0.4789 0.033 Uiso 0.140(3) 1 calc PR A 2 H10F H 0.1949 -0.0663 0.2901 0.033 Uiso 0.140(3) 1 calc PR A 2 C11 C 0.00381(10) 0.04535(13) -0.1864(2) 0.0234(4) Uani 1 1 d . A . H2 H 0.1313(9) -0.0196(17) -0.048(2) 0.019(4) Uiso 1 1 d . . . H5 H 0.1140(8) 0.3707(16) 0.000(2) 0.014(4) Uiso 1 1 d . . . H6 H 0.2246(11) 0.2819(16) 0.104(3) 0.029(5) Uiso 1 1 d . . . H7A H 0.2544(10) -0.0897(15) -0.029(2) 0.025(4) Uiso 1 1 d . . . H7B H 0.3306(10) -0.0530(16) 0.052(2) 0.030 Uiso 1 1 d . . . H8A H 0.2744(12) 0.0472(18) -0.244(2) 0.037 Uiso 1 1 d . . . H8B H 0.3455(12) -0.0250(19) -0.230(2) 0.037 Uiso 1 1 d . . . H8C H 0.3492(10) 0.0954(16) -0.149(3) 0.037 Uiso 1 1 d . . . H11A H -0.0444(10) 0.0597(18) -0.129(3) 0.037 Uiso 1 1 d . . . H11B H 0.0134(11) -0.0363(18) -0.180(3) 0.037 Uiso 1 1 d . . . H11C H -0.0033(10) 0.0659(17) -0.311(3) 0.037 Uiso 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02146(9) 0.01444(9) 0.01469(8) -0.00202(8) -0.00309(9) 0.00324(6) Cl1 0.02121(18) 0.02083(17) 0.01700(17) -0.00024(14) -0.00436(14) 0.00415(14) Cl2 0.01917(18) 0.02396(19) 0.01937(16) 0.00049(15) -0.00211(14) 0.00417(14) Cl3 0.01854(17) 0.02332(18) 0.01766(17) -0.00146(15) -0.00153(14) 0.00410(15) Cl4 0.0433(2) 0.01292(17) 0.01997(17) -0.00216(14) -0.00283(17) 0.00542(16) N2 0.0146(5) 0.0127(5) 0.0148(5) 0.0009(5) -0.0029(6) 0.0000(4) C1 0.0179(7) 0.0249(8) 0.0164(7) 0.0010(6) -0.0014(5) 0.0084(6) C2 0.0226(8) 0.0177(8) 0.0187(7) 0.0026(6) -0.0008(6) 0.0042(6) C3 0.0185(7) 0.0165(7) 0.0157(7) 0.0014(5) -0.0012(5) 0.0017(6) C4 0.0137(7) 0.0179(7) 0.0127(6) 0.0019(6) -0.0003(5) 0.0019(5) C5 0.0207(7) 0.0160(8) 0.0201(7) -0.0024(6) -0.0016(6) 0.0014(6) C6 0.0165(7) 0.0273(8) 0.0235(8) -0.0043(7) -0.0052(6) -0.0003(6) C7 0.0174(8) 0.0206(8) 0.0426(10) 0.0007(8) -0.0014(7) 0.0040(6) C8 0.0234(8) 0.0483(11) 0.0328(10) -0.0115(9) 0.0020(8) 0.0015(8) N1A 0.0182(7) 0.0342(8) 0.0183(6) 0.0016(5) -0.0035(5) 0.0080(6) C9A 0.0221(10) 0.0244(10) 0.0233(9) 0.0074(8) -0.0049(8) 0.0020(8) C10A 0.0270(10) 0.0335(12) 0.0207(9) -0.0001(8) -0.0028(7) -0.0060(9) N1B 0.0182(7) 0.0342(8) 0.0183(6) 0.0016(5) -0.0035(5) 0.0080(6) C9B 0.022(2) 0.024(2) 0.021(2) 0.007(2) -0.0045(19) 0.003(2) C10B 0.024(4) 0.030(4) 0.013(4) -0.003(4) -0.001(4) 0.001(4) C11 0.0279(8) 0.0129(7) 0.0292(10) 0.0010(6) -0.0089(7) 0.0008(6) _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 Cl2 2.2116(4) . ? Cu1 Cl4 2.2359(4) . ? Cu1 Cl3 2.2398(4) . ? Cu1 Cl1 2.3018(4) . ? N2 C4 1.4684(17) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? C1 C2 1.377(2) . ? C1 C6 1.384(2) . ? C1 N1A 1.4874(18) . ? C2 C3 1.391(2) . ? C2 H2 0.899(19) . ? C3 C4 1.392(2) . ? C3 C11 1.504(2) . ? C4 C5 1.378(2) . ? C5 C6 1.386(2) . ? C5 H5 0.884(18) . ? C6 H6 0.99(2) . ? C7 C8 1.491(3) . ? C7 N1A 1.503(2) . ? C7 H7A 0.972(18) . ? C7 H7B 0.935(19) . ? C8 H8A 0.92(2) . ? C8 H8B 0.94(2) . ? C8 H8C 1.034(19) . ? N1A C9A 1.544(2) . ? N1A H1A 0.9300 . ? C9A C10A 1.502(3) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C9B C10B 1.492(9) . ? C9B H9B1 0.9900 . ? C9B H9B2 0.9900 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11 H11A 0.983(19) . ? C11 H11B 0.96(2) . ? C11 H11C 1.01(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 Cl2 Cu1 Cl4 100.911(16) . . ? Cl2 Cu1 Cl3 98.615(15) . . ? Cl4 Cu1 Cl3 137.349(16) . . ? Cl2 Cu1 Cl1 136.172(16) . . ? Cl4 Cu1 Cl1 94.706(15) . . ? Cl3 Cu1 Cl1 96.830(14) . . ? C4 N2 H2A 109.5 . . ? C4 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C4 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C2 C1 C6 122.05(14) . . ? C2 C1 N1A 119.51(14) . . ? C6 C1 N1A 118.39(14) . . ? C1 C2 C3 120.18(15) . . ? C1 C2 H2 122.6(11) . . ? C3 C2 H2 117.2(11) . . ? C2 C3 C4 117.25(14) . . ? C2 C3 C11 121.10(14) . . ? C4 C3 C11 121.64(13) . . ? C5 C4 C3 122.70(14) . . ? C5 C4 N2 118.42(13) . . ? C3 C4 N2 118.87(13) . . ? C4 C5 C6 119.40(15) . . ? C4 C5 H5 120.0(10) . . ? C6 C5 H5 120.6(10) . . ? C1 C6 C5 118.41(14) . . ? C1 C6 H6 119.5(11) . . ? C5 C6 H6 122.1(11) . . ? C8 C7 N1A 111.70(15) . . ? C8 C7 H7A 111.4(11) . . ? N1A C7 H7A 109.3(10) . . ? C8 C7 H7B 110.5(12) . . ? N1A C7 H7B 104.4(12) . . ? H7A C7 H7B 109.3(15) . . ? C7 C8 H8A 113.8(13) . . ? C7 C8 H8B 108.5(12) . . ? H8A C8 H8B 109.6(17) . . ? C7 C8 H8C 110.0(13) . . ? H8A C8 H8C 112.2(18) . . ? H8B C8 H8C 101.9(16) . . ? C1 N1A C7 115.15(12) . . ? C1 N1A C9A 112.05(12) . . ? C7 N1A C9A 106.18(13) . . ? C1 N1A H1A 107.7 . . ? C7 N1A H1A 107.7 . . ? C9A N1A H1A 107.7 . . ? C10A C9A N1A 111.77(15) . . ? C10A C9A H9A1 109.3 . . ? N1A C9A H9A1 109.3 . . ? C10A C9A H9A2 109.3 . . ? N1A C9A H9A2 109.3 . . ? H9A1 C9A H9A2 107.9 . . ? C10B C9B H9B1 111.8 . . ? C10B C9B H9B2 111.8 . . ? H9B1 C9B H9B2 109.5 . . ? C9B C10B H10D 109.5 . . ? C9B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C9B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C3 C11 H11A 111.0(12) . . ? C3 C11 H11B 110.9(12) . . ? H11A C11 H11B 107.3(16) . . ? C3 C11 H11C 112.6(11) . . ? H11A C11 H11C 107.1(16) . . ? H11B C11 H11C 107.8(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.3(2) . . . . ? N1A C1 C2 C3 177.78(13) . . . . ? C1 C2 C3 C4 -0.4(2) . . . . ? C1 C2 C3 C11 -179.80(14) . . . . ? C2 C3 C4 C5 0.2(2) . . . . ? C11 C3 C4 C5 179.60(15) . . . . ? C2 C3 C4 N2 -178.55(14) . . . . ? C11 C3 C4 N2 0.9(2) . . . . ? C3 C4 C5 C6 0.1(2) . . . . ? N2 C4 C5 C6 178.78(14) . . . . ? C2 C1 C6 C5 -0.1(2) . . . . ? N1A C1 C6 C5 -177.58(14) . . . . ? C4 C5 C6 C1 -0.1(2) . . . . ? C2 C1 N1A C7 49.2(2) . . . . ? C6 C1 N1A C7 -133.22(15) . . . . ? C2 C1 N1A C9A -72.24(19) . . . . ? C6 C1 N1A C9A 105.29(16) . . . . ? C8 C7 N1A C1 57.69(19) . . . . ? C8 C7 N1A C9A -177.70(14) . . . . ? C1 N1A C9A C10A -58.02(19) . . . . ? C7 N1A C9A C10A 175.47(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A Cl1 0.91 2.34 3.2369(13) 168.1 3_455 N2 H2B Cl3 0.91 2.49 3.2185(12) 137.9 3_454 N2 H2B Cl2 0.91 2.53 3.2286(14) 133.9 3_454 N2 H2C Cl4 0.91 2.36 3.1864(12) 150.3 4_554 N1A H1A Cl1 0.93 2.47 3.3813(15) 165.6 . N1B H1B Cl1 0.93 2.51 3.3813(15) 157.1 . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.255 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.046 data_5+CuCl3 _database_code_depnum_ccdc_archive 'CCDC 659020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H17.40 Cl6 Cu2 N2.20' _chemical_formula_weight 508.24 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.2815(2) _cell_length_b 10.2466(6) _cell_length_c 13.9250(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.672(4) _cell_angle_gamma 90.00 _cell_volume 891.88(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 3.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.51 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 12041 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 28.65 _reflns_number_total 2176 _reflns_number_gt 1819 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0280P)^2^+0.4879P] 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 2176 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Cu1 Cu 0.26543(3) 0.55782(2) 0.037956(17) 0.01516(8) Uani 1 1 d . . . Cl1 Cl 0.57652(7) 0.45815(5) 0.10518(3) 0.01931(11) Uani 1 1 d . . . Cl2 Cl 0.22889(8) 0.65628(5) 0.18114(4) 0.02120(12) Uani 1 1 d . . . Cl3 Cl 0.02696(7) 0.34215(5) 0.03793(4) 0.01826(11) Uani 1 1 d . . . N1 N 0.7892(3) 0.94325(18) 0.16480(14) 0.0228(4) Uani 1 1 d . A . C1 C 0.6368(3) 0.9703(2) 0.07916(15) 0.0206(4) Uani 1 1 d . . . C2 C 0.5719(4) 1.0980(2) 0.06454(16) 0.0229(5) Uani 1 1 d . . . C6 C 0.5674(3) 0.8717(2) 0.01563(16) 0.0228(5) Uani 1 1 d . . . C7 C 1.0167(4) 0.9654(2) 0.14286(19) 0.0257(5) Uani 1 1 d . . . C8 C 0.7568(4) 0.8119(2) 0.20872(18) 0.0294(5) Uani 1 1 d . . . N2 N 0.729(3) 0.7020(18) 0.2301(13) 0.022(4) Uiso 0.10 1 d P A 1 H8A H 0.592(5) 0.796(3) 0.219(2) 0.035(8) Uiso 0.90 1 d P . . H8B H 0.849(5) 0.808(3) 0.271(2) 0.036(8) Uiso 0.90 1 d P . . H8C H 0.808(4) 0.736(3) 0.163(2) 0.028(7) Uiso 0.90 1 d P . . H7C H 1.029(4) 1.058(2) 0.1179(18) 0.028(6) Uiso 1 1 d . . . H7A H 1.097(5) 0.952(3) 0.197(2) 0.038(8) Uiso 1 1 d . . . H2 H 0.618(4) 1.164(2) 0.1074(18) 0.027(6) Uiso 1 1 d . . . H7B H 1.047(4) 0.901(2) 0.0924(18) 0.024(6) Uiso 1 1 d . . . H6 H 0.617(4) 0.788(3) 0.0260(19) 0.036(7) Uiso 1 1 d . . . H1N H 0.758(4) 1.010(3) 0.211(2) 0.036(7) Uiso 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01151(12) 0.01799(13) 0.01575(13) 0.00074(9) 0.00020(9) 0.00310(9) Cl1 0.0138(2) 0.0284(3) 0.0154(2) 0.00241(19) 0.00013(18) 0.00595(18) Cl2 0.0256(2) 0.0203(2) 0.0179(2) -0.00113(19) 0.00293(19) 0.0045(2) Cl3 0.0122(2) 0.0183(2) 0.0235(3) 0.00196(19) -0.00201(18) 0.00271(17) N1 0.0213(9) 0.0228(9) 0.0238(10) 0.0006(8) -0.0007(7) 0.0025(7) C1 0.0167(9) 0.0236(10) 0.0208(11) 0.0028(8) -0.0015(8) 0.0013(8) C2 0.0258(11) 0.0207(10) 0.0219(11) -0.0038(9) 0.0001(9) -0.0014(9) C6 0.0227(10) 0.0178(11) 0.0279(12) 0.0013(9) 0.0023(9) 0.0063(8) C7 0.0190(10) 0.0268(12) 0.0307(13) 0.0035(10) -0.0005(10) 0.0016(9) C8 0.0261(12) 0.0333(13) 0.0282(13) 0.0023(10) -0.0004(10) 0.0024(10) _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 Cl2 2.2663(5) . ? Cu1 Cl3 2.2709(5) 3_565 ? Cu1 Cl1 2.3187(5) 3_665 ? Cu1 Cl1 2.3187(5) . ? Cu1 Cl3 2.6697(5) . ? Cl1 Cu1 2.3187(5) 3_665 ? Cl3 Cu1 2.2709(5) 3_565 ? N1 C1 1.480(3) . ? N1 C8 1.500(3) . ? N1 C7 1.508(3) . ? N1 H1N 0.97(3) . ? C1 C2 1.380(3) . ? C1 C6 1.385(3) . ? C2 C6 1.384(3) 3_675 ? C2 H2 0.93(3) . ? C6 C2 1.384(3) 3_675 ? C6 H6 0.91(3) . ? C7 H7C 1.01(3) . ? C7 H7A 0.88(3) . ? C7 H7B 1.00(3) . ? C8 N2 1.182(18) . ? C8 H8A 1.07(3) . ? C8 H8B 1.00(3) . ? C8 H8C 1.07(3) . ? 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 Cl2 Cu1 Cl3 93.49(2) . 3_565 ? Cl2 Cu1 Cl1 151.27(2) . 3_665 ? Cl3 Cu1 Cl1 91.558(19) 3_565 3_665 ? Cl2 Cu1 Cl1 89.740(19) . . ? Cl3 Cu1 Cl1 175.76(2) 3_565 . ? Cl1 Cu1 Cl1 84.294(19) 3_665 . ? Cl2 Cu1 Cl3 105.249(19) . . ? Cl3 Cu1 Cl3 86.880(18) 3_565 . ? Cl1 Cu1 Cl3 103.258(19) 3_665 . ? Cl1 Cu1 Cl3 94.930(18) . . ? Cu1 Cl1 Cu1 95.706(19) 3_665 . ? Cu1 Cl3 Cu1 93.120(18) 3_565 . ? C1 N1 C8 113.17(17) . . ? C1 N1 C7 111.04(18) . . ? C8 N1 C7 112.77(17) . . ? C1 N1 H1N 104.1(16) . . ? C8 N1 H1N 108.6(16) . . ? C7 N1 H1N 106.5(16) . . ? C2 C1 C6 121.88(19) . . ? C2 C1 N1 117.03(19) . . ? C6 C1 N1 121.06(19) . . ? C1 C2 C6 119.1(2) . 3_675 ? C1 C2 H2 121.7(16) . . ? C6 C2 H2 119.3(15) 3_675 . ? C2 C6 C1 119.04(19) 3_675 . ? C2 C6 H6 121.0(17) 3_675 . ? C1 C6 H6 120.0(17) . . ? N1 C7 H7C 108.4(15) . . ? N1 C7 H7A 105.9(19) . . ? H7C C7 H7A 113(2) . . ? N1 C7 H7B 106.9(14) . . ? H7C C7 H7B 111(2) . . ? H7A C7 H7B 112(2) . . ? N2 C8 N1 170.6(9) . . ? N1 C8 H8A 111.3(15) . . ? N1 C8 H8B 107.5(17) . . ? H8A C8 H8B 111(2) . . ? N1 C8 H8C 110.4(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Cu1 Cl1 Cu1 -151.85(2) . . . 3_665 ? Cl3 Cu1 Cl1 Cu1 -12.2(3) 3_565 . . 3_665 ? Cl1 Cu1 Cl1 Cu1 0.0 3_665 . . 3_665 ? Cl3 Cu1 Cl1 Cu1 102.87(2) . . . 3_665 ? Cl2 Cu1 Cl3 Cu1 92.77(2) . . . 3_565 ? Cl3 Cu1 Cl3 Cu1 0.0 3_565 . . 3_565 ? Cl1 Cu1 Cl3 Cu1 -90.87(2) 3_665 . . 3_565 ? Cl1 Cu1 Cl3 Cu1 -176.15(2) . . . 3_565 ? C8 N1 C1 C2 146.4(2) . . . . ? C7 N1 C1 C2 -85.6(2) . . . . ? C8 N1 C1 C6 -35.1(3) . . . . ? C7 N1 C1 C6 92.9(2) . . . . ? C6 C1 C2 C6 0.3(4) . . . 3_675 ? N1 C1 C2 C6 178.8(2) . . . 3_675 ? C2 C1 C6 C2 -0.3(4) . . . 3_675 ? N1 C1 C6 C2 -178.7(2) . . . 3_675 ? C1 N1 C8 N2 45(6) . . . . ? C7 N1 C8 N2 -82(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl2 0.97(3) 2.12(3) 3.071(2) 166(2) 2_655 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.567 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.077 data_6+PbCl4 _database_code_depnum_ccdc_archive 'CCDC 659021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl4 N2 Pb' _chemical_formula_weight 459.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 20.384(2) _cell_length_b 8.4343(9) _cell_length_c 6.9922(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.669(9) _cell_angle_gamma 90.00 _cell_volume 1199.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description planar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 14.913 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.09 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 20662 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3487 _reflns_number_gt 2578 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0143P)^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 SHELXL _refine_ls_extinction_coef 0.00093(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3487 _refine_ls_number_parameters 158 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0298 _refine_ls_wR_factor_gt 0.0283 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.834 _refine_ls_shift/su_max 0.003 _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 Pb1 Pb 0.249000(5) 0.242882(9) 0.256150(13) 0.01360(3) Uani 1 1 d . . . Cl1 Cl 0.22544(4) 0.53399(8) 0.43293(9) 0.02482(15) Uani 1 1 d . . . Cl2 Cl 0.11564(3) 0.14901(7) 0.25934(10) 0.02272(14) Uani 1 1 d . . . Cl3 Cl 0.26821(4) 0.09599(7) 0.61265(9) 0.02290(14) Uani 1 1 d . . . Cl4 Cl 0.38548(3) 0.32273(7) 0.26388(9) 0.02119(13) Uani 1 1 d . . . N1A N 0.38245(13) 0.6876(3) 0.3123(4) 0.0209(5) Uani 1 1 d . . . C1A C 0.44336(14) 0.7707(3) 0.2773(3) 0.0176(5) Uani 1 1 d . . . C2A C 0.44270(15) 0.9340(3) 0.2784(4) 0.0200(6) Uani 1 1 d . . . C3A C 0.5000 1.0154(4) 0.2500 0.0231(8) Uani 1 2 d S . . C4A C 0.5000 0.6850(4) 0.2500 0.0165(7) Uani 1 2 d SD . . N1B N 0.11889(13) 0.7802(3) 0.2049(4) 0.0208(5) Uani 1 1 d . . . C1B C 0.05705(13) 0.6971(3) 0.2308(3) 0.0160(5) Uani 1 1 d . . . C2B C 0.05775(14) 0.5343(3) 0.2286(4) 0.0159(5) Uani 1 1 d . . . C3B C 0.0000 0.4524(4) 0.2500 0.0168(7) Uani 1 2 d S . . C4B C 0.0000 0.7836(4) 0.2500 0.0175(7) Uani 1 2 d S . . H1AA H 0.3773(19) 0.685(4) 0.437(5) 0.039(10) Uiso 1 1 d . . . H1BA H 0.3816(18) 0.599(4) 0.275(5) 0.033(9) Uiso 1 1 d . . . H1CA H 0.349(2) 0.733(4) 0.260(5) 0.027(9) Uiso 1 1 d . . . H2A H 0.4076(18) 0.978(4) 0.293(4) 0.033 Uiso 1 1 d . . . H3A H 0.5000 1.124(5) 0.2500 0.032(12) Uiso 1 2 d S . . H4A H 0.5000 0.571(2) 0.2500 0.038(13) Uiso 1 2 d SD . . H1AB H 0.153(2) 0.711(5) 0.256(5) 0.055(12) Uiso 1 1 d . . . H1BB H 0.1216(18) 0.802(4) 0.089(5) 0.035(10) Uiso 1 1 d . . . H1CB H 0.1183(19) 0.872(4) 0.257(5) 0.038(10) Uiso 1 1 d . . . H2B H 0.0928(17) 0.488(4) 0.219(4) 0.026(9) Uiso 1 1 d . . . H4B H 0.0000 0.892(5) 0.2500 0.032 Uiso 1 2 d S . . H3B H 0.0000 0.341(5) 0.2500 0.032 Uiso 1 2 d S . . 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 Pb1 0.01313(4) 0.01096(4) 0.01675(4) 0.00141(4) 0.00137(3) -0.00013(4) Cl1 0.0298(4) 0.0265(3) 0.0177(3) -0.0063(2) -0.0017(3) 0.0071(3) Cl2 0.0153(3) 0.0145(3) 0.0382(4) -0.0014(3) 0.0001(3) 0.0012(2) Cl3 0.0194(4) 0.0232(3) 0.0257(3) 0.0080(2) -0.0017(3) -0.0034(3) Cl4 0.0168(3) 0.0152(3) 0.0316(3) 0.0011(2) 0.0019(3) 0.0010(2) N1A 0.0181(13) 0.0150(11) 0.0298(13) -0.0003(10) 0.0027(11) 0.0020(10) C1A 0.0165(13) 0.0179(13) 0.0181(10) 0.0004(10) -0.0006(9) -0.0016(10) C2A 0.0164(15) 0.0155(12) 0.0275(13) -0.0015(10) -0.0018(11) 0.0041(10) C3A 0.024(2) 0.0123(16) 0.033(2) 0.000 -0.0020(17) 0.000 C4A 0.018(2) 0.0114(15) 0.0203(17) 0.000 -0.0005(14) 0.000 N1B 0.0151(12) 0.0146(11) 0.0330(13) 0.0026(10) 0.0033(10) -0.0018(9) C1B 0.0135(13) 0.0157(11) 0.0189(11) 0.0004(9) 0.0008(10) -0.0018(10) C2B 0.0133(14) 0.0139(11) 0.0203(12) -0.0007(9) 0.0006(10) 0.0027(10) C3B 0.017(2) 0.0105(15) 0.0226(17) 0.000 -0.0031(15) 0.000 C4B 0.016(2) 0.0113(16) 0.0249(17) 0.000 0.0015(14) 0.000 _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 Pb1 Cl3 2.7887(7) . ? Pb1 Cl1 2.8041(7) . ? Pb1 Cl2 2.8328(8) . ? Pb1 Cl4 2.8595(8) . ? Pb1 Cl1 2.9565(7) 4_565 ? Pb1 Cl3 3.0625(7) 4 ? Cl1 Pb1 2.9565(7) 4_566 ? Cl3 Pb1 3.0625(7) 4_556 ? N1A C1A 1.460(4) . ? N1A H1AA 0.88(4) . ? N1A H1BA 0.79(3) . ? N1A H1CA 0.84(4) . ? C1A C2A 1.378(3) . ? C1A C4A 1.386(3) . ? C2A C3A 1.380(3) . ? C2A H2A 0.82(4) . ? C3A C2A 1.380(3) 2_655 ? C3A H3A 0.92(4) . ? C4A C1A 1.386(3) 2_655 ? C4A H4A 0.960(19) . ? N1B C1B 1.463(4) . ? N1B H1AB 0.96(4) . ? N1B H1BB 0.84(4) . ? N1B H1CB 0.85(4) . ? C1B C2B 1.373(3) . ? C1B C4B 1.386(3) . ? C2B C3B 1.382(3) . ? C2B H2B 0.82(3) . ? C3B C2B 1.382(3) 2 ? C3B H3B 0.94(4) . ? C4B C1B 1.386(3) 2 ? C4B H4B 0.91(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 Cl3 Pb1 Cl1 90.76(2) . . ? Cl3 Pb1 Cl2 87.06(2) . . ? Cl1 Pb1 Cl2 92.85(2) . . ? Cl3 Pb1 Cl4 90.40(2) . . ? Cl1 Pb1 Cl4 88.81(2) . . ? Cl2 Pb1 Cl4 176.979(18) . . ? Cl3 Pb1 Cl1 166.58(2) . 4_565 ? Cl1 Pb1 Cl1 75.852(10) . 4_565 ? Cl2 Pb1 Cl1 94.30(2) . 4_565 ? Cl4 Pb1 Cl1 88.56(2) . 4_565 ? Cl3 Pb1 Cl3 82.221(11) . 4 ? Cl1 Pb1 Cl3 172.17(2) . 4 ? Cl2 Pb1 Cl3 83.375(19) . 4 ? Cl4 Pb1 Cl3 94.667(19) . 4 ? Cl1 Pb1 Cl3 111.19(2) 4_565 4 ? Pb1 Cl1 Pb1 150.49(3) . 4_566 ? Pb1 Cl3 Pb1 133.94(2) . 4_556 ? C1A N1A H1AA 110(2) . . ? C1A N1A H1BA 113(3) . . ? H1AA N1A H1BA 107(3) . . ? C1A N1A H1CA 112(2) . . ? H1AA N1A H1CA 108(3) . . ? H1BA N1A H1CA 107(3) . . ? C2A C1A C4A 122.0(3) . . ? C2A C1A N1A 118.1(3) . . ? C4A C1A N1A 119.9(2) . . ? C1A C2A C3A 119.2(3) . . ? C1A C2A H2A 118(2) . . ? C3A C2A H2A 123(2) . . ? C2A C3A C2A 120.3(4) . 2_655 ? C2A C3A H3A 119.83(17) . . ? C2A C3A H3A 119.83(17) 2_655 . ? C1A C4A C1A 117.2(3) 2_655 . ? C1A C4A H4A 121.42(17) 2_655 . ? C1A C4A H4A 121.42(17) . . ? C1B N1B H1AB 106(3) . . ? C1B N1B H1BB 110(3) . . ? H1AB N1B H1BB 114(3) . . ? C1B N1B H1CB 110(3) . . ? H1AB N1B H1CB 115(3) . . ? H1BB N1B H1CB 103(3) . . ? C2B C1B C4B 122.4(3) . . ? C2B C1B N1B 117.9(2) . . ? C4B C1B N1B 119.7(2) . . ? C1B C2B C3B 119.3(3) . . ? C1B C2B H2B 119(2) . . ? C3B C2B H2B 121(2) . . ? C2B C3B C2B 119.9(3) 2 . ? C2B C3B H3B 120.03(16) 2 . ? C2B C3B H3B 120.03(16) . . ? C1B C4B C1B 116.5(3) 2 . ? C1B C4B H4B 121.73(17) 2 . ? C1B C4B H4B 121.73(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl3 Pb1 Cl1 Pb1 31.79(6) . . . 4_566 ? Cl2 Pb1 Cl1 Pb1 118.89(6) . . . 4_566 ? Cl4 Pb1 Cl1 Pb1 -58.59(6) . . . 4_566 ? Cl1 Pb1 Cl1 Pb1 -147.40(5) 4_565 . . 4_566 ? Cl3 Pb1 Cl1 Pb1 57.96(19) 4 . . 4_566 ? Cl1 Pb1 Cl3 Pb1 151.79(4) . . . 4_556 ? Cl2 Pb1 Cl3 Pb1 58.97(4) . . . 4_556 ? Cl4 Pb1 Cl3 Pb1 -119.39(4) . . . 4_556 ? Cl1 Pb1 Cl3 Pb1 155.17(7) 4_565 . . 4_556 ? Cl3 Pb1 Cl3 Pb1 -24.74(5) 4 . . 4_556 ? C4A C1A C2A C3A 0.5(4) . . . . ? N1A C1A C2A C3A 178.6(2) . . . . ? C1A C2A C3A C2A -0.23(17) . . . 2_655 ? C2A C1A C4A C1A -0.24(18) . . . 2_655 ? N1A C1A C4A C1A -178.3(3) . . . 2_655 ? C4B C1B C2B C3B -1.3(3) . . . . ? N1B C1B C2B C3B -179.1(2) . . . . ? C1B C2B C3B C2B 0.63(17) . . . 2 ? C2B C1B C4B C1B 0.66(17) . . . 2 ? N1B C1B C4B C1B 178.4(3) . . . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1CA Cl3 0.84(4) 2.38(4) 3.207(3) 169(3) 4_565 N1B H1AB Cl1 0.96(4) 2.39(4) 3.336(3) 169(3) . N1B H1CB Cl2 0.85(4) 2.34(4) 3.135(2) 155(3) 1_565 N1A H1BA Cl4 0.79(3) 2.33(3) 3.097(3) 163(3) . N1B H1BB Cl2 0.84(4) 2.34(4) 3.169(3) 173(3) 4_565 N1A H1AA Cl4 0.88(4) 2.28(4) 3.156(3) 169(3) 4_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.688 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.124 data_7+Pb(II)_chlorides+Cl _database_code_depnum_ccdc_archive 'CCDC 659022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C255 H88 Cl17 N33 Pb3' _chemical_formula_weight 2435.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 13.7786(6) _cell_length_b 34.1194(14) _cell_length_c 18.7021(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8792.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4736 _exptl_absorpt_coefficient_mu 6.304 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 130182 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10096 _reflns_number_gt 6051 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0406P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000161(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10096 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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 Pb1 Pb 0.83034(2) 0.2500 0.2500 0.01991(7) Uani 1 2 d S . . Pb2 Pb 0.49618(2) 0.2500 0.2500 0.01923(8) Uani 1 2 d S . . Pb3 Pb 0.7500 0.0000 0.266789(15) 0.02056(8) Uani 1 2 d S . . Cl1 Cl 0.97080(13) 0.23077(5) 0.15163(8) 0.0329(4) Uani 1 1 d . . . Cl2 Cl 0.85618(12) 0.17203(4) 0.29729(7) 0.0265(3) Uani 1 1 d . . . Cl3 Cl 0.65526(11) 0.24612(5) 0.35894(7) 0.0302(3) Uani 1 1 d . . . Cl4 Cl 0.50820(11) 0.16628(4) 0.25964(8) 0.0287(3) Uani 1 1 d . . . Cl5 Cl 0.34634(12) 0.23916(5) 0.14916(8) 0.0322(4) Uani 1 1 d . . . Cl6 Cl 0.73900(11) 0.08192(4) 0.24329(7) 0.0244(3) Uani 1 1 d . . . Cl7 Cl 0.59239(11) -0.00729(5) 0.16572(7) 0.0288(4) Uani 1 1 d . . . Cl8 Cl 0.61147(12) 0.00788(5) 0.38503(8) 0.0351(4) Uani 1 1 d . . . Cl9 Cl 0.2500 0.0000 0.13113(12) 0.0646(9) Uani 1 2 d S . . N1A N 0.7133(4) 0.16099(16) 0.1435(3) 0.0338(14) Uani 1 1 d . . . H1BA H 0.7177 0.1472 0.1831 0.041 Uiso 1 1 calc R . . H1AA H 0.6991 0.1861 0.1455 0.041 Uiso 1 1 calc R . . N2A N 0.7498(4) 0.10479(14) 0.0810(2) 0.0230(10) Uani 1 1 d . . . H2A H 0.7548 0.0931 0.1228 0.028 Uiso 1 1 calc R . . N3A N 0.7839(4) 0.04427(16) 0.0281(3) 0.0322(14) Uani 1 1 d . . . H3AA H 0.7872 0.0338 0.0710 0.039 Uiso 1 1 calc R . . H3BA H 0.7935 0.0296 -0.0100 0.039 Uiso 1 1 calc R . . C1A C 0.7280(4) 0.14388(19) 0.0806(3) 0.0244(14) Uani 1 1 d . . . C2A C 0.7644(4) 0.0825(2) 0.0208(3) 0.0260(14) Uani 1 1 d . . . C3A C 0.7563(5) 0.1017(2) -0.0450(3) 0.0291(15) Uani 1 1 d . . . H3A H 0.7655 0.0877 -0.0884 0.035 Uiso 1 1 calc R . . C4A C 0.7344(5) 0.1418(2) -0.0462(3) 0.0292(16) Uani 1 1 d . . . H4A H 0.7287 0.1547 -0.0911 0.035 Uiso 1 1 calc R . . C5A C 0.7209(4) 0.1631(2) 0.0152(3) 0.0281(15) Uani 1 1 d . . . H5A H 0.7071 0.1904 0.0132 0.034 Uiso 1 1 calc R . . N1B N 0.4611(4) 0.19325(16) 0.0202(3) 0.0325(13) Uani 1 1 d . . . H1AB H 0.4587 0.2067 0.0603 0.039 Uiso 1 1 calc R . . H1BB H 0.4539 0.2053 -0.0210 0.039 Uiso 1 1 calc R . . N2B N 0.4862(4) 0.13744(16) 0.0880(2) 0.0251(12) Uani 1 1 d . . . H2B H 0.4813 0.1524 0.1261 0.030 Uiso 1 1 calc R . . N3B N 0.5109(4) 0.08516(17) 0.1656(3) 0.0385(15) Uani 1 1 d . . . H3AB H 0.5039 0.1015 0.2017 0.046 Uiso 1 1 calc R . . H3BB H 0.5223 0.0602 0.1737 0.046 Uiso 1 1 calc R . . C1B C 0.4754(5) 0.1547(2) 0.0219(3) 0.0267(15) Uani 1 1 d . . . C2B C 0.5040(4) 0.0985(2) 0.0979(3) 0.0286(15) Uani 1 1 d . . . C3B C 0.5142(5) 0.0738(2) 0.0377(4) 0.0342(17) Uani 1 1 d . . . H3B H 0.5275 0.0466 0.0427 0.041 Uiso 1 1 calc R . . C4B C 0.5038(5) 0.0911(2) -0.0290(3) 0.0336(17) Uani 1 1 d . . . H4B H 0.5099 0.0751 -0.0704 0.040 Uiso 1 1 calc R . . C5B C 0.4846(5) 0.1312(2) -0.0377(3) 0.0303(16) Uani 1 1 d . . . H5B H 0.4780 0.1421 -0.0842 0.036 Uiso 1 1 calc R . . N1C N 0.1559(4) 0.20683(17) 0.2772(3) 0.0467(16) Uani 1 1 d . . . H1C1 H 0.0998 0.2185 0.2847 0.056 Uiso 1 1 calc R . . H1C2 H 0.2104 0.2197 0.2844 0.056 Uiso 1 1 calc R . . N2C N 0.0717(4) 0.15041(14) 0.2443(3) 0.0261(11) Uani 1 1 d . . . H2C H 0.0181 0.1641 0.2494 0.031 Uiso 1 1 calc R . . N3C N -0.0272(4) 0.09800(16) 0.2182(3) 0.0330(13) Uani 1 1 d . . . H3AC H -0.0773 0.1136 0.2244 0.040 Uiso 1 1 calc R . . H3BC H -0.0364 0.0733 0.2067 0.040 Uiso 1 1 calc R . . C1C C 0.1583(5) 0.16919(19) 0.2547(3) 0.0311(14) Uani 1 1 d . . . C2C C 0.0632(5) 0.11186(18) 0.2264(3) 0.0247(14) Uani 1 1 d . . . C3C C 0.1464(5) 0.0902(2) 0.2174(3) 0.0319(16) Uani 1 1 d . . . H3C H 0.1432 0.0633 0.2044 0.038 Uiso 1 1 calc R . . C4C C 0.2357(5) 0.1086(2) 0.2278(3) 0.0337(16) Uani 1 1 d . . . H4C H 0.2934 0.0937 0.2223 0.040 Uiso 1 1 calc R . . C5C C 0.2435(4) 0.1478(2) 0.2459(3) 0.0289(14) Uani 1 1 d . . . H5C H 0.3052 0.1598 0.2521 0.035 Uiso 1 1 calc R . . N1D N 0.2929(4) 0.21015(17) 0.5021(3) 0.0366(14) Uani 1 1 d . . . H1BD H 0.2807 0.2174 0.5463 0.044 Uiso 1 1 calc R . . H1AD H 0.2883 0.2273 0.4670 0.044 Uiso 1 1 calc R . . N2D N 0.3251(4) 0.14703(17) 0.5437(2) 0.0306(14) Uani 1 1 d . . . H2D H 0.3126 0.1559 0.5869 0.037 Uiso 1 1 calc R . . N3D N 0.3540(4) 0.08762(17) 0.5968(3) 0.0399(15) Uani 1 1 d . . . H3AD H 0.3418 0.0986 0.6384 0.048 Uiso 1 1 calc R . . H3BD H 0.3695 0.0626 0.5946 0.048 Uiso 1 1 calc R . . C1D C 0.3188(5) 0.1725(2) 0.4879(3) 0.0291(15) Uani 1 1 d . . . C2D C 0.3491(5) 0.1089(2) 0.5367(3) 0.0284(15) Uani 1 1 d . . . C3D C 0.3697(5) 0.0945(2) 0.4693(3) 0.0319(16) Uani 1 1 d . . . H3D H 0.3869 0.0678 0.4627 0.038 Uiso 1 1 calc R . . C4D C 0.3648(5) 0.1196(2) 0.4121(3) 0.0356(17) Uani 1 1 d . . . H4D H 0.3796 0.1101 0.3657 0.043 Uiso 1 1 calc R . . C5D C 0.3389(5) 0.1583(2) 0.4202(3) 0.0337(16) Uani 1 1 d . . . H5D H 0.3347 0.1750 0.3798 0.040 Uiso 1 1 calc R . . N1E N 0.0410(4) 0.21868(18) 0.4958(3) 0.0436(16) Uani 1 1 d . . . H1BE H 0.0393 0.2305 0.5376 0.052 Uiso 1 1 calc R . . H1AE H 0.0285 0.2320 0.4565 0.052 Uiso 1 1 calc R . . N2E N 0.0818(4) 0.16020(17) 0.5539(2) 0.0323(14) Uani 1 1 d . . . H2E H 0.0809 0.1736 0.5941 0.039 Uiso 1 1 calc R . . N3E N 0.1158(4) 0.10676(19) 0.6218(3) 0.0449(17) Uani 1 1 d . . . H3AE H 0.1119 0.1220 0.6596 0.054 Uiso 1 1 calc R . . H3BE H 0.1291 0.0817 0.6269 0.054 Uiso 1 1 calc R . . C1E C 0.0629(5) 0.1798(2) 0.4919(3) 0.0323(16) Uani 1 1 d . . . C2E C 0.1018(5) 0.1215(2) 0.5575(3) 0.0297(16) Uani 1 1 d . . . C3E C 0.1072(5) 0.1007(2) 0.4946(3) 0.0326(16) Uani 1 1 d . . . H3E H 0.1235 0.0736 0.4952 0.039 Uiso 1 1 calc R . . C4E C 0.0890(5) 0.1190(2) 0.4316(3) 0.0355(17) Uani 1 1 d . . . H4E H 0.0932 0.1045 0.3884 0.043 Uiso 1 1 calc R . . C5E C 0.0647(5) 0.1582(2) 0.4291(3) 0.0369(18) Uani 1 1 d . . . H5E H 0.0493 0.1703 0.3848 0.044 Uiso 1 1 calc R . . N1F N 0.4154(4) 0.0036(2) 0.2860(3) 0.0505(17) Uani 1 1 d . . . H1BF H 0.4087 0.0044 0.2393 0.061 Uiso 1 1 calc R . . H1AF H 0.4737 0.0044 0.3052 0.061 Uiso 1 1 calc R . . N2F N 0.2500 0.0000 0.2942(3) 0.0307(17) Uani 1 2 d S . . H2F H 0.2500 0.0000 0.2472 0.037 Uiso 1 2 calc SR . . C1F C 0.3374(4) 0.0011(2) 0.3278(3) 0.0329(14) Uani 1 1 d . . . C3F C 0.3382(5) -0.0008(2) 0.4023(3) 0.0350(15) Uani 1 1 d . . . H3F H 0.3975 -0.0025 0.4281 0.042 Uiso 1 1 calc R . . C4F C 0.2500 0.0000 0.4373(5) 0.040(2) Uani 1 2 d S . . H4F H 0.2500 0.0000 0.4881 0.048 Uiso 1 2 calc SR . . 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 Pb1 0.02077(15) 0.02003(15) 0.01893(13) 0.00345(13) 0.000 0.000 Pb2 0.02024(16) 0.01772(15) 0.01973(15) 0.00165(13) 0.000 0.000 Pb3 0.02191(16) 0.01774(15) 0.02203(14) 0.000 0.000 -0.00153(14) Cl1 0.0423(10) 0.0326(10) 0.0239(7) 0.0012(7) 0.0095(7) 0.0041(8) Cl2 0.0347(9) 0.0201(8) 0.0246(7) 0.0023(6) 0.0023(6) 0.0001(7) Cl3 0.0342(8) 0.0348(10) 0.0218(6) 0.0019(6) -0.0020(6) 0.0006(8) Cl4 0.0306(8) 0.0202(7) 0.0352(8) 0.0020(6) 0.0027(7) 0.0030(6) Cl5 0.0340(9) 0.0378(11) 0.0247(7) -0.0018(6) -0.0037(7) 0.0022(7) Cl6 0.0311(8) 0.0187(7) 0.0235(6) -0.0006(5) 0.0023(7) -0.0018(6) Cl7 0.0319(9) 0.0293(10) 0.0253(7) -0.0003(6) -0.0019(6) 0.0016(7) Cl8 0.0315(9) 0.0411(11) 0.0328(8) -0.0003(7) 0.0031(6) 0.0010(8) Cl9 0.123(3) 0.0486(18) 0.0220(11) 0.000 0.000 0.031(2) N1A 0.051(4) 0.026(3) 0.024(3) -0.003(2) 0.000(2) 0.000(3) N2A 0.024(3) 0.029(3) 0.016(2) 0.0013(19) 0.002(2) -0.003(3) N3A 0.048(4) 0.028(3) 0.021(3) -0.001(2) 0.005(2) -0.001(3) C1A 0.017(4) 0.030(4) 0.026(3) -0.002(3) 0.001(2) -0.002(3) C2A 0.019(3) 0.037(4) 0.021(3) -0.002(3) 0.003(2) -0.008(3) C3A 0.025(4) 0.047(4) 0.016(3) 0.001(2) 0.001(3) -0.002(3) C4A 0.024(4) 0.044(4) 0.020(3) 0.009(3) -0.001(3) -0.003(3) C5A 0.023(4) 0.033(4) 0.028(3) 0.008(3) 0.000(2) 0.001(3) N1B 0.043(4) 0.023(3) 0.032(3) -0.001(2) -0.001(2) -0.005(3) N2B 0.021(3) 0.031(3) 0.024(3) -0.006(2) -0.002(2) -0.001(2) N3B 0.052(4) 0.033(4) 0.030(3) -0.003(3) -0.008(3) 0.007(3) C1B 0.017(3) 0.034(4) 0.029(3) -0.001(3) 0.003(2) -0.003(3) C2B 0.017(3) 0.036(4) 0.033(3) -0.004(3) -0.004(3) 0.000(3) C3B 0.025(4) 0.040(5) 0.038(4) -0.014(3) -0.005(3) 0.001(3) C4B 0.026(4) 0.045(5) 0.030(3) -0.014(3) 0.003(3) 0.000(3) C5B 0.024(4) 0.042(5) 0.025(3) -0.003(3) 0.001(3) -0.001(3) N1C 0.029(3) 0.030(4) 0.081(4) 0.006(3) -0.009(3) -0.008(3) N2C 0.018(2) 0.024(3) 0.036(3) 0.001(2) 0.000(2) -0.001(2) N3C 0.032(3) 0.027(3) 0.040(3) -0.012(2) 0.004(3) -0.006(3) C1C 0.027(3) 0.031(4) 0.035(3) 0.009(3) -0.004(3) -0.003(3) C2C 0.028(3) 0.030(4) 0.016(3) 0.000(2) 0.002(2) 0.000(3) C3C 0.041(4) 0.033(4) 0.023(3) -0.003(3) 0.003(3) 0.009(3) C4C 0.029(4) 0.054(5) 0.019(3) 0.002(3) 0.001(3) 0.016(3) C5C 0.022(3) 0.044(4) 0.021(3) 0.006(2) -0.001(4) 0.001(3) N1D 0.049(4) 0.036(4) 0.025(3) -0.003(3) 0.007(3) 0.001(3) N2D 0.036(4) 0.037(4) 0.018(2) -0.004(2) 0.004(2) -0.004(3) N3D 0.057(4) 0.033(4) 0.030(3) 0.001(3) 0.008(3) 0.001(3) C1D 0.025(4) 0.039(4) 0.023(3) -0.002(3) 0.004(3) -0.005(3) C2D 0.029(4) 0.027(4) 0.030(3) 0.000(3) 0.000(3) -0.004(3) C3D 0.027(4) 0.033(4) 0.035(4) -0.007(3) 0.001(3) -0.002(3) C4D 0.036(4) 0.046(5) 0.025(3) -0.012(3) 0.000(3) 0.001(3) C5D 0.034(4) 0.047(5) 0.020(3) 0.002(3) -0.001(3) -0.001(4) N1E 0.051(4) 0.044(4) 0.035(3) -0.004(3) -0.016(3) 0.017(3) N2E 0.031(3) 0.045(4) 0.021(3) -0.010(2) -0.008(2) 0.011(3) N3E 0.063(5) 0.045(4) 0.027(3) 0.001(3) -0.006(3) 0.021(3) C1E 0.025(4) 0.042(5) 0.030(3) -0.001(3) -0.006(3) 0.006(3) C2E 0.025(4) 0.030(4) 0.034(4) 0.000(3) -0.003(3) 0.005(3) C3E 0.025(4) 0.038(4) 0.035(4) -0.007(3) 0.000(3) 0.005(3) C4E 0.035(4) 0.040(5) 0.031(4) -0.014(3) -0.001(3) 0.005(4) C5E 0.035(4) 0.057(5) 0.019(3) -0.004(3) -0.009(3) 0.005(4) N1F 0.023(3) 0.084(5) 0.044(3) 0.003(4) 0.006(3) -0.011(4) N2F 0.028(4) 0.039(5) 0.026(3) 0.000 0.000 -0.003(4) C1F 0.028(4) 0.039(4) 0.032(3) 0.000(3) 0.000(3) -0.003(4) C3F 0.035(4) 0.042(4) 0.028(3) 0.002(3) -0.007(3) -0.004(4) C4F 0.041(6) 0.042(6) 0.037(5) 0.000 0.000 -0.015(6) _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 Pb1 Cl1 2.7496(15) 4 ? Pb1 Cl1 2.7496(15) . ? Pb1 Cl2 2.8261(15) 4 ? Pb1 Cl2 2.8261(15) . ? Pb2 Cl5 2.8206(16) . ? Pb2 Cl5 2.8206(16) 4 ? Pb2 Cl4 2.8671(15) 4 ? Pb2 Cl4 2.8671(15) . ? Pb2 Cl3 2.9955(15) . ? Pb2 Cl3 2.9955(15) 4 ? Pb3 Cl6 2.8334(14) . ? Pb3 Cl6 2.8334(14) 2_655 ? Pb3 Cl7 2.8898(15) . ? Pb3 Cl7 2.8898(15) 2_655 ? Pb3 Cl8 2.9335(16) . ? Pb3 Cl8 2.9335(16) 2_655 ? N1A C1A 1.328(7) . ? N1A H1BA 0.8800 . ? N1A H1AA 0.8800 . ? N2A C1A 1.367(8) . ? N2A C2A 1.374(7) . ? N2A H2A 0.8800 . ? N3A C2A 1.340(8) . ? N3A H3AA 0.8800 . ? N3A H3BA 0.8800 . ? C1A C5A 1.391(8) . ? C2A C3A 1.398(8) . ? C3A C4A 1.400(9) . ? C3A H3A 0.9500 . ? C4A C5A 1.373(9) . ? C4A H4A 0.9500 . ? C5A H5A 0.9500 . ? N1B C1B 1.330(8) . ? N1B H1AB 0.8800 . ? N1B H1BB 0.8800 . ? N2B C2B 1.365(8) . ? N2B C1B 1.378(8) . ? N2B H2B 0.8800 . ? N3B C2B 1.349(8) . ? N3B H3AB 0.8800 . ? N3B H3BB 0.8800 . ? C1B C5B 1.378(8) . ? C2B C3B 1.413(9) . ? C3B C4B 1.386(9) . ? C3B H3B 0.9500 . ? C4B C5B 1.405(10) . ? C4B H4B 0.9500 . ? C5B H5B 0.9500 . ? N1C C1C 1.352(8) . ? N1C H1C1 0.8800 . ? N1C H1C2 0.8800 . ? N2C C2C 1.362(7) . ? N2C C1C 1.369(8) . ? N2C H2C 0.8800 . ? N3C C2C 1.340(8) . ? N3C H3AC 0.8800 . ? N3C H3BC 0.8800 . ? C1C C5C 1.391(9) . ? C2C C3C 1.375(9) . ? C3C C4C 1.395(9) . ? C3C H3C 0.9500 . ? C4C C5C 1.385(9) . ? C4C H4C 0.9500 . ? C5C H5C 0.9500 . ? N1D C1D 1.358(8) . ? N1D H1BD 0.8800 . ? N1D H1AD 0.8800 . ? N2D C2D 1.348(8) . ? N2D C1D 1.362(8) . ? N2D H2D 0.8800 . ? N3D C2D 1.339(8) . ? N3D H3AD 0.8800 . ? N3D H3BD 0.8800 . ? C1D C5D 1.384(8) . ? C2D C3D 1.383(8) . ? C3D C4D 1.374(9) . ? C3D H3D 0.9500 . ? C4D C5D 1.374(9) . ? C4D H4D 0.9500 . ? C5D H5D 0.9500 . ? N1E C1E 1.362(8) . ? N1E H1BE 0.8800 . ? N1E H1AE 0.8800 . ? N2E C2E 1.352(8) . ? N2E C1E 1.363(8) . ? N2E H2E 0.8800 . ? N3E C2E 1.317(8) . ? N3E H3AE 0.8800 . ? N3E H3BE 0.8800 . ? C1E C5E 1.387(9) . ? C2E C3E 1.376(9) . ? C3E C4E 1.356(9) . ? C3E H3E 0.9500 . ? C4E C5E 1.380(9) . ? C4E H4E 0.9500 . ? C5E H5E 0.9500 . ? N1F C1F 1.331(7) . ? N1F H1BF 0.8800 . ? N1F H1AF 0.8800 . ? N2F C1F 1.358(7) 2 ? N2F C1F 1.358(7) . ? N2F H2F 0.8800 . ? C1F C3F 1.396(8) . ? C3F C4F 1.381(7) . ? C3F H3F 0.9500 . ? C4F C3F 1.381(7) 2 ? C4F H4F 0.9500 . ? 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 Cl1 Pb1 Cl1 90.53(7) 4 . ? Cl1 Pb1 Cl2 84.04(5) 4 4 ? Cl1 Pb1 Cl2 85.79(5) . 4 ? Cl1 Pb1 Cl2 85.79(5) 4 . ? Cl1 Pb1 Cl2 84.04(5) . . ? Cl2 Pb1 Cl2 165.52(7) 4 . ? Cl5 Pb2 Cl5 85.90(7) . 4 ? Cl5 Pb2 Cl4 97.52(4) . 4 ? Cl5 Pb2 Cl4 87.35(5) 4 4 ? Cl5 Pb2 Cl4 87.35(5) . . ? Cl5 Pb2 Cl4 97.52(4) 4 . ? Cl4 Pb2 Cl4 173.38(6) 4 . ? Cl5 Pb2 Cl3 169.92(5) . . ? Cl5 Pb2 Cl3 94.97(4) 4 . ? Cl4 Pb2 Cl3 92.56(4) 4 . ? Cl4 Pb2 Cl3 82.58(5) . . ? Cl5 Pb2 Cl3 94.97(4) . 4 ? Cl5 Pb2 Cl3 169.92(5) 4 4 ? Cl4 Pb2 Cl3 82.58(5) 4 4 ? Cl4 Pb2 Cl3 92.56(4) . 4 ? Cl3 Pb2 Cl3 85.94(6) . 4 ? Cl6 Pb3 Cl6 162.16(5) . 2_655 ? Cl6 Pb3 Cl7 86.75(4) . . ? Cl6 Pb3 Cl7 81.59(4) 2_655 . ? Cl6 Pb3 Cl7 81.59(4) . 2_655 ? Cl6 Pb3 Cl7 86.75(4) 2_655 2_655 ? Cl7 Pb3 Cl7 98.29(6) . 2_655 ? Cl6 Pb3 Cl8 89.53(4) . . ? Cl6 Pb3 Cl8 104.01(5) 2_655 . ? Cl7 Pb3 Cl8 90.69(4) . . ? Cl7 Pb3 Cl8 166.95(4) 2_655 . ? Cl6 Pb3 Cl8 104.01(5) . 2_655 ? Cl6 Pb3 Cl8 89.53(4) 2_655 2_655 ? Cl7 Pb3 Cl8 166.95(4) . 2_655 ? Cl7 Pb3 Cl8 90.69(4) 2_655 2_655 ? Cl8 Pb3 Cl8 82.15(6) . 2_655 ? C1A N1A H1BA 120.0 . . ? C1A N1A H1AA 120.0 . . ? H1BA N1A H1AA 120.0 . . ? C1A N2A C2A 124.6(5) . . ? C1A N2A H2A 117.7 . . ? C2A N2A H2A 117.7 . . ? C2A N3A H3AA 120.0 . . ? C2A N3A H3BA 120.0 . . ? H3AA N3A H3BA 120.0 . . ? N1A C1A N2A 117.3(5) . . ? N1A C1A C5A 124.0(6) . . ? N2A C1A C5A 118.7(5) . . ? N3A C2A N2A 118.9(5) . . ? N3A C2A C3A 124.2(5) . . ? N2A C2A C3A 116.8(6) . . ? C2A C3A C4A 119.3(5) . . ? C2A C3A H3A 120.4 . . ? C4A C3A H3A 120.4 . . ? C5A C4A C3A 122.2(6) . . ? C5A C4A H4A 118.9 . . ? C3A C4A H4A 118.9 . . ? C4A C5A C1A 118.5(6) . . ? C4A C5A H5A 120.8 . . ? C1A C5A H5A 120.8 . . ? C1B N1B H1AB 120.0 . . ? C1B N1B H1BB 120.0 . . ? H1AB N1B H1BB 120.0 . . ? C2B N2B C1B 123.9(5) . . ? C2B N2B H2B 118.1 . . ? C1B N2B H2B 118.1 . . ? C2B N3B H3AB 120.0 . . ? C2B N3B H3BB 120.0 . . ? H3AB N3B H3BB 120.0 . . ? N1B C1B N2B 117.4(6) . . ? N1B C1B C5B 124.7(6) . . ? N2B C1B C5B 117.9(6) . . ? N3B C2B N2B 117.9(6) . . ? N3B C2B C3B 122.7(7) . . ? N2B C2B C3B 119.4(6) . . ? C4B C3B C2B 117.0(7) . . ? C4B C3B H3B 121.5 . . ? C2B C3B H3B 121.5 . . ? C3B C4B C5B 122.5(6) . . ? C3B C4B H4B 118.7 . . ? C5B C4B H4B 118.7 . . ? C1B C5B C4B 119.4(6) . . ? C1B C5B H5B 120.3 . . ? C4B C5B H5B 120.3 . . ? C1C N1C H1C1 120.0 . . ? C1C N1C H1C2 120.0 . . ? H1C1 N1C H1C2 120.0 . . ? C2C N2C C1C 124.2(5) . . ? C2C N2C H2C 117.9 . . ? C1C N2C H2C 117.9 . . ? C2C N3C H3AC 120.0 . . ? C2C N3C H3BC 120.0 . . ? H3AC N3C H3BC 120.0 . . ? N1C C1C N2C 117.8(6) . . ? N1C C1C C5C 123.7(6) . . ? N2C C1C C5C 118.3(6) . . ? N3C C2C N2C 116.7(6) . . ? N3C C2C C3C 124.8(6) . . ? N2C C2C C3C 118.5(6) . . ? C2C C3C C4C 118.5(6) . . ? C2C C3C H3C 120.8 . . ? C4C C3C H3C 120.8 . . ? C5C C4C C3C 122.5(6) . . ? C5C C4C H4C 118.7 . . ? C3C C4C H4C 118.7 . . ? C4C C5C C1C 118.0(6) . . ? C4C C5C H5C 121.0 . . ? C1C C5C H5C 121.0 . . ? C1D N1D H1BD 120.0 . . ? C1D N1D H1AD 120.0 . . ? H1BD N1D H1AD 120.0 . . ? C2D N2D C1D 123.9(5) . . ? C2D N2D H2D 118.0 . . ? C1D N2D H2D 118.0 . . ? C2D N3D H3AD 120.0 . . ? C2D N3D H3BD 120.0 . . ? H3AD N3D H3BD 120.0 . . ? N1D C1D N2D 118.1(5) . . ? N1D C1D C5D 124.3(6) . . ? N2D C1D C5D 117.6(6) . . ? N3D C2D N2D 117.1(6) . . ? N3D C2D C3D 124.1(6) . . ? N2D C2D C3D 118.8(6) . . ? C4D C3D C2D 118.5(7) . . ? C4D C3D H3D 120.7 . . ? C2D C3D H3D 120.7 . . ? C5D C4D C3D 121.7(6) . . ? C5D C4D H4D 119.1 . . ? C3D C4D H4D 119.1 . . ? C4D C5D C1D 119.4(6) . . ? C4D C5D H5D 120.3 . . ? C1D C5D H5D 120.3 . . ? C1E N1E H1BE 120.0 . . ? C1E N1E H1AE 120.0 . . ? H1BE N1E H1AE 120.0 . . ? C2E N2E C1E 124.2(5) . . ? C2E N2E H2E 117.9 . . ? C1E N2E H2E 117.9 . . ? C2E N3E H3AE 120.0 . . ? C2E N3E H3BE 120.0 . . ? H3AE N3E H3BE 120.0 . . ? N1E C1E N2E 118.4(6) . . ? N1E C1E C5E 124.5(6) . . ? N2E C1E C5E 117.1(7) . . ? N3E C2E N2E 116.6(6) . . ? N3E C2E C3E 125.2(7) . . ? N2E C2E C3E 118.2(6) . . ? C4E C3E C2E 119.7(7) . . ? C4E C3E H3E 120.2 . . ? C2E C3E H3E 120.2 . . ? C3E C4E C5E 121.4(6) . . ? C3E C4E H4E 119.3 . . ? C5E C4E H4E 119.3 . . ? C4E C5E C1E 119.4(6) . . ? C4E C5E H5E 120.3 . . ? C1E C5E H5E 120.3 . . ? C1F N1F H1BF 120.0 . . ? C1F N1F H1AF 120.0 . . ? H1BF N1F H1AF 120.0 . . ? C1F N2F C1F 125.0(7) 2 . ? C1F N2F H2F 117.5 2 . ? C1F N2F H2F 117.5 . . ? N1F C1F N2F 116.6(5) . . ? N1F C1F C3F 125.6(6) . . ? N2F C1F C3F 117.9(6) . . ? C4F C3F C1F 117.7(6) . . ? C4F C3F H3F 121.1 . . ? C1F C3F H3F 121.1 . . ? C3F C4F C3F 123.4(8) 2 . ? C3F C4F H4F 118.3 2 . ? C3F C4F H4F 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A N2A C1A N1A 178.2(6) . . . . ? C2A N2A C1A C5A -0.8(9) . . . . ? C1A N2A C2A N3A -179.0(6) . . . . ? C1A N2A C2A C3A 0.1(9) . . . . ? N3A C2A C3A C4A 179.2(6) . . . . ? N2A C2A C3A C4A 0.2(9) . . . . ? C2A C3A C4A C5A 0.3(10) . . . . ? C3A C4A C5A C1A -1.0(10) . . . . ? N1A C1A C5A C4A -177.7(6) . . . . ? N2A C1A C5A C4A 1.2(9) . . . . ? C2B N2B C1B N1B -178.1(6) . . . . ? C2B N2B C1B C5B -0.9(9) . . . . ? C1B N2B C2B N3B -178.6(6) . . . . ? C1B N2B C2B C3B 1.3(9) . . . . ? N3B C2B C3B C4B 178.9(6) . . . . ? N2B C2B C3B C4B -0.9(9) . . . . ? C2B C3B C4B C5B 0.4(10) . . . . ? N1B C1B C5B C4B 177.3(6) . . . . ? N2B C1B C5B C4B 0.3(9) . . . . ? C3B C4B C5B C1B -0.1(10) . . . . ? C2C N2C C1C N1C -175.4(6) . . . . ? C2C N2C C1C C5C 0.7(9) . . . . ? C1C N2C C2C N3C 180.0(5) . . . . ? C1C N2C C2C C3C -0.7(9) . . . . ? N3C C2C C3C C4C -180.0(5) . . . . ? N2C C2C C3C C4C 0.7(8) . . . . ? C2C C3C C4C C5C -0.9(9) . . . . ? C3C C4C C5C C1C 0.8(9) . . . . ? N1C C1C C5C C4C 175.1(6) . . . . ? N2C C1C C5C C4C -0.7(8) . . . . ? C2D N2D C1D N1D 179.4(6) . . . . ? C2D N2D C1D C5D -0.2(10) . . . . ? C1D N2D C2D N3D 178.8(6) . . . . ? C1D N2D C2D C3D 0.5(10) . . . . ? N3D C2D C3D C4D -178.1(7) . . . . ? N2D C2D C3D C4D 0.0(10) . . . . ? C2D C3D C4D C5D -0.8(11) . . . . ? C3D C4D C5D C1D 1.2(11) . . . . ? N1D C1D C5D C4D 179.8(6) . . . . ? N2D C1D C5D C4D -0.6(10) . . . . ? C2E N2E C1E N1E 178.1(6) . . . . ? C2E N2E C1E C5E 0.0(10) . . . . ? C1E N2E C2E N3E -178.2(6) . . . . ? C1E N2E C2E C3E 2.6(10) . . . . ? N3E C2E C3E C4E 178.5(7) . . . . ? N2E C2E C3E C4E -2.3(10) . . . . ? C2E C3E C4E C5E -0.3(11) . . . . ? C3E C4E C5E C1E 2.9(11) . . . . ? N1E C1E C5E C4E 179.3(7) . . . . ? N2E C1E C5E C4E -2.7(10) . . . . ? C1F N2F C1F N1F -177.6(8) 2 . . . ? C1F N2F C1F C3F 3.0(5) 2 . . . ? N1F C1F C3F C4F 174.8(6) . . . . ? N2F C1F C3F C4F -5.9(10) . . . . ? C1F C3F C4F C3F 3.0(5) . . . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1BA Cl6 0.88 2.51 3.300(6) 149.2 . N1A H1BA Cl2 0.88 2.99 3.506(5) 119.7 . N1A H1AA Cl3 0.88 2.39 3.269(6) 175.2 4 N2A H2A Cl6 0.88 2.30 3.137(4) 159.9 . N3A H3AA Cl7 0.88 2.59 3.335(5) 143.0 2_655 N3A H3BA Cl9 0.88 2.55 3.372(5) 155.3 5_655 N1B H1AB Cl5 0.88 2.53 3.282(6) 144.2 . N1B H1BB Cl1 0.88 2.60 3.462(5) 165.6 6 N2B H2B Cl4 0.88 2.57 3.371(5) 152.1 . N3B H3AB Cl4 0.88 2.46 3.279(6) 154.5 . N3B H3BB Cl7 0.88 2.50 3.348(6) 161.9 . N1C H1C1 Cl1 0.88 2.75 3.579(7) 156.9 4_455 N1C H1C2 Cl5 0.88 2.65 3.490(6) 159.9 4 N2C H2C Cl2 0.88 2.42 3.216(5) 151.0 1_455 N3C H3AC Cl2 0.88 2.58 3.339(6) 144.6 1_455 N3C H3AC Cl6 0.88 2.78 3.301(5) 119.7 1_455 N3C H3BC Cl7 0.88 2.50 3.369(5) 169.4 2 N1D H1BD Cl3 0.88 2.66 3.444(5) 148.6 6_556 N1D H1AD Cl5 0.88 2.58 3.396(6) 154.0 4 N2D H2D Cl2 0.88 2.31 3.124(5) 153.0 6_556 N3D H3AD Cl6 0.88 2.69 3.390(5) 137.6 6_556 N3D H3AD Cl2 0.88 2.79 3.496(6) 138.7 6_556 N3D H3BD Cl8 0.88 2.45 3.310(6) 166.1 5_656 N1E H1BE Cl3 0.88 2.57 3.276(6) 138.4 6_556 N1E H1AE Cl1 0.88 2.52 3.393(6) 172.8 4_455 N2E H2E Cl3 0.88 2.82 3.504(6) 135.8 6_556 N2E H2E Cl4 0.88 2.92 3.638(5) 139.4 6_556 N3E H3AE Cl4 0.88 2.57 3.353(6) 148.7 6_556 N3E H3BE Cl8 0.88 2.54 3.377(7) 159.2 6_556 N1F H1BF Cl7 0.88 2.91 3.339(5) 112.0 . N1F H1BF Cl9 0.88 2.98 3.688(6) 138.5 . N1F H1AF Cl8 0.88 2.42 3.278(6) 165.9 . N2F H2F Cl9 0.88 2.17 3.050(7) 180.0 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.880 _refine_diff_density_min -1.612 _refine_diff_density_rms 0.267 data_8+Hg2Cl6+H2O _database_code_depnum_ccdc_archive 'CCDC 659023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H12 Cl6 Hg2 N2 O' _chemical_formula_weight 742.06 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' O O 0.0106 0.0060 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2678(8) _cell_length_b 10.9577(15) _cell_length_c 12.7211(18) _cell_angle_alpha 72.358(12) _cell_angle_beta 79.396(11) _cell_angle_gamma 75.428(12) _cell_volume 800.30(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 20.146 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.0005 _exptl_absorpt_correction_T_max 0.23 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 23105 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 30.00 _reflns_number_total 4601 _reflns_number_gt 4043 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0307P)^2^+0.1955P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0139(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4601 _refine_ls_number_parameters 161 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0439 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.002 _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 Hg1 Hg 0.51122(3) 0.587423(14) 0.836837(12) 0.02265(6) Uani 1 1 d . . . Hg2 Hg 0.01995(2) 0.805181(13) 0.642138(13) 0.02349(6) Uani 1 1 d . . . Cl1 Cl 0.59469(14) 0.45539(9) 0.71396(7) 0.01813(16) Uani 1 1 d . . . Cl2 Cl 0.41511(16) 0.68036(8) 0.98425(7) 0.02124(18) Uani 1 1 d . . . Cl3 Cl 0.43317(14) 0.81846(8) 0.65121(7) 0.01813(16) Uani 1 1 d . . . Cl4 Cl 0.03949(14) 0.66352(8) 0.52122(7) 0.01789(16) Uani 1 1 d . . . Cl5 Cl -0.00885(15) 0.61900(8) 0.82386(7) 0.01904(16) Uani 1 1 d . . . Cl6 Cl -0.16594(16) 1.02079(9) 0.65391(11) 0.0324(2) Uani 1 1 d . . . O1S O 0.5534(4) 0.6585(3) 0.4610(2) 0.0201(5) Uani 1 1 d D . . N1 N 0.7196(5) 0.8794(3) 0.3404(3) 0.0175(6) Uani 1 1 d . . . H1B H 0.8534 0.8688 0.3640 0.026 Uiso 1 1 calc R . . H1C H 0.6476 0.8168 0.3857 0.026 Uiso 1 1 calc R . . H1A H 0.6366 0.9600 0.3423 0.026 Uiso 1 1 calc R . . N2 N 0.8758(5) 0.6247(3) 0.2879(3) 0.0156(6) Uani 1 1 d . . . H2C H 0.8872 0.5560 0.2596 0.023 Uiso 1 1 calc R . . H2A H 0.7639 0.6235 0.3448 0.023 Uiso 1 1 calc R . . H2B H 1.0058 0.6181 0.3134 0.023 Uiso 1 1 calc R . . C1 C 0.7542(5) 0.8677(3) 0.2257(3) 0.0155(6) Uani 1 1 d . . . C2 C 0.7141(6) 0.9816(4) 0.1415(3) 0.0203(7) Uani 1 1 d . . . H2 H 0.6642 1.0636 0.1584 0.024 Uiso 1 1 calc R . . C3 C 0.7471(6) 0.9761(4) 0.0316(3) 0.0228(7) Uani 1 1 d . . . H3 H 0.7209 1.0545 -0.0267 0.027 Uiso 1 1 calc R . . C4 C 0.8184(6) 0.8558(4) 0.0071(3) 0.0229(8) Uani 1 1 d . . . H4 H 0.8399 0.8522 -0.0679 0.027 Uiso 1 1 calc R . . C5 C 0.8583(6) 0.7409(4) 0.0920(3) 0.0183(7) Uani 1 1 d . . . H5 H 0.9056 0.6586 0.0755 0.022 Uiso 1 1 calc R . . C6 C 0.8284(5) 0.7475(3) 0.2008(3) 0.0149(6) Uani 1 1 d . . . H1SA H 0.611(5) 0.646(4) 0.5327(15) 0.022 Uiso 1 1 d D . . H1SB H 0.4139 0.6295(16) 0.4664 0.022 Uiso 1 1 d 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03004(9) 0.02176(8) 0.01772(8) -0.01023(6) -0.00226(6) -0.00261(6) Hg2 0.02899(9) 0.01517(8) 0.02877(9) -0.00900(6) -0.00521(6) -0.00394(6) Cl1 0.0177(4) 0.0223(4) 0.0177(4) -0.0105(3) -0.0021(3) -0.0039(3) Cl2 0.0307(4) 0.0160(4) 0.0170(4) -0.0072(3) -0.0024(3) -0.0019(3) Cl3 0.0193(4) 0.0157(4) 0.0215(4) -0.0069(3) -0.0051(3) -0.0032(3) Cl4 0.0189(4) 0.0185(4) 0.0183(4) -0.0067(3) -0.0040(3) -0.0042(3) Cl5 0.0227(4) 0.0159(4) 0.0189(4) -0.0057(3) -0.0015(3) -0.0041(3) Cl6 0.0188(4) 0.0170(4) 0.0645(8) -0.0159(4) -0.0075(4) -0.0013(3) O1S 0.0185(12) 0.0275(14) 0.0179(12) -0.0089(11) -0.0013(10) -0.0084(10) N1 0.0191(14) 0.0141(13) 0.0211(15) -0.0070(12) -0.0060(12) -0.0010(11) N2 0.0148(13) 0.0109(13) 0.0209(14) -0.0048(11) -0.0026(11) -0.0014(10) C1 0.0127(14) 0.0166(16) 0.0191(16) -0.0067(13) -0.0024(13) -0.0034(12) C2 0.0204(17) 0.0159(16) 0.0259(19) -0.0074(14) -0.0045(14) -0.0027(13) C3 0.0244(18) 0.0195(17) 0.0238(19) -0.0019(15) -0.0053(15) -0.0063(14) C4 0.0232(18) 0.0255(19) 0.0200(17) -0.0057(15) -0.0011(15) -0.0068(15) C5 0.0186(16) 0.0166(16) 0.0212(17) -0.0087(14) -0.0016(14) -0.0025(13) C6 0.0107(14) 0.0150(15) 0.0184(16) -0.0035(13) -0.0021(12) -0.0029(12) _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 Hg1 Cl2 2.3129(9) . ? Hg1 Cl1 2.3451(9) . ? Hg1 Cl3 2.8988(10) . ? Hg2 Cl6 2.3930(10) . ? Hg2 Cl4 2.4643(9) . ? Hg2 Cl5 2.5907(10) . ? Hg2 Cl3 2.6556(9) . ? O1S H1SA 1.001(10) . ? O1S H1SB 0.987(9) . ? N1 C1 1.474(5) . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N1 H1A 0.9100 . ? N2 C6 1.464(4) . ? N2 H2C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? C1 C2 1.378(5) . ? C1 C6 1.394(5) . ? C2 C3 1.394(6) . ? C2 H2 0.9500 . ? C3 C4 1.391(5) . ? C3 H3 0.9500 . ? C4 C5 1.390(5) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? 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 Cl2 Hg1 Cl1 168.62(3) . . ? Cl2 Hg1 Cl3 100.84(3) . . ? Cl1 Hg1 Cl3 89.72(3) . . ? Cl6 Hg2 Cl4 137.55(4) . . ? Cl6 Hg2 Cl5 115.93(4) . . ? Cl4 Hg2 Cl5 93.92(3) . . ? Cl6 Hg2 Cl3 99.27(3) . . ? Cl4 Hg2 Cl3 107.30(3) . . ? Cl5 Hg2 Cl3 95.88(3) . . ? Hg2 Cl3 Hg1 95.15(3) . . ? H1SA O1S H1SB 116.4(14) . . ? C1 N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C1 N1 H1A 109.5 . . ? H1B N1 H1A 109.5 . . ? H1C N1 H1A 109.5 . . ? C6 N2 H2C 109.5 . . ? C6 N2 H2A 109.5 . . ? H2C N2 H2A 109.5 . . ? C6 N2 H2B 109.5 . . ? H2C N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C2 C1 C6 120.0(3) . . ? C2 C1 N1 117.5(3) . . ? C6 C1 N1 122.5(3) . . ? C1 C2 C3 119.8(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.3(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C1 120.6(3) . . ? C5 C6 N2 117.8(3) . . ? C1 C6 N2 121.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl6 Hg2 Cl3 Hg1 125.72(4) . . . . ? Cl4 Hg2 Cl3 Hg1 -87.78(3) . . . . ? Cl5 Hg2 Cl3 Hg1 8.20(3) . . . . ? Cl2 Hg1 Cl3 Hg2 -93.26(3) . . . . ? Cl1 Hg1 Cl3 Hg2 82.49(3) . . . . ? C6 C1 C2 C3 0.3(5) . . . . ? N1 C1 C2 C3 179.1(3) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C4 C5 C6 C1 1.4(5) . . . . ? C4 C5 C6 N2 -178.9(3) . . . . ? C2 C1 C6 C5 -1.3(5) . . . . ? N1 C1 C6 C5 179.9(3) . . . . ? C2 C1 C6 N2 179.1(3) . . . . ? N1 C1 C6 N2 0.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B Cl6 0.91 2.49 3.269(3) 143.4 2_676 N1 H1B Cl4 0.91 2.69 3.305(3) 125.7 1_655 N1 H1C O1S 0.91 1.89 2.780(4) 165.3 . N1 H1A Cl3 0.91 2.38 3.235(3) 156.6 2_676 N1 H1A Cl6 0.91 2.90 3.360(3) 113.1 2_576 N2 H2C Cl5 0.91 2.36 3.254(3) 166.0 2_666 N2 H2A O1S 0.91 1.86 2.747(4) 166.0 . N2 H2B Cl1 0.91 2.42 3.210(3) 144.7 2_766 N2 H2B Cl4 0.91 2.89 3.486(3) 124.6 1_655 O1S H1SB Cl4 0.987(9) 2.29(1) 3.161(3) 146.5(14) . O1S H1SB Cl1 0.987(9) 2.738(11) 3.224(3) 110.9(4) 2_666 O1S H1SA Cl1 1.001(10) 2.60(3) 3.325(3) 129(2) . O1S H1SA Cl3 1.001(10) 2.67(4) 3.276(3) 119(3) . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.922 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.230 data_9+BiCl4 _database_code_depnum_ccdc_archive 'CCDC 659024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Bi Cl4 N3' _chemical_formula_weight 470.92 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4183(5) _cell_length_b 8.2559(6) _cell_length_c 10.1905(7) _cell_angle_alpha 82.378(6) _cell_angle_beta 79.922(5) _cell_angle_gamma 84.856(6) _cell_volume 607.64(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 15.352 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.03 _exptl_absorpt_correction_T_max 0.35 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KM4CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 10541 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 29.99 _reflns_number_total 3410 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0399P)^2^+1.3723P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3410 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 Bi1 Bi 0.21749(2) 0.08332(3) 0.087263(18) 0.02522(7) Uani 1 1 d . . . Cl1 Cl -0.08743(19) 0.22437(18) 0.00341(14) 0.0326(3) Uani 1 1 d . . . Cl2 Cl 0.52589(19) -0.0844(2) 0.17416(13) 0.0382(3) Uani 1 1 d . . . Cl3 Cl 0.0612(2) 0.0335(3) 0.32701(15) 0.0472(4) Uani 1 1 d . . . Cl4 Cl 0.3256(3) 0.3532(2) 0.1110(2) 0.0497(4) Uani 1 1 d . . . N1 N 0.6555(7) 0.2370(6) 0.3059(5) 0.0347(10) Uani 1 1 d . . . H1 H 0.6597 0.2250 0.2209 0.042 Uiso 1 1 calc R . . N2 N 0.6095(7) 0.1895(7) 0.5143(5) 0.0340(11) Uani 1 1 d . . . H2 H 0.5780 0.1401 0.5961 0.041 Uiso 1 1 calc R . . N3 N 0.5914(7) 0.1276(7) 0.4064(5) 0.0370(11) Uani 1 1 d . . . C1 C 0.7141(7) 0.3695(8) 0.3476(6) 0.0329(12) Uani 1 1 d . . . C2 C 0.6817(7) 0.3375(8) 0.4877(6) 0.0327(12) Uani 1 1 d . . . C3 C 0.7219(9) 0.4526(10) 0.5688(8) 0.0466(17) Uani 1 1 d . . . H3 H 0.7020 0.4325 0.6640 0.056 Uiso 1 1 calc R . . C4 C 0.7918(10) 0.5957(10) 0.5006(10) 0.057(2) Uani 1 1 d . . . H4 H 0.8195 0.6770 0.5504 0.068 Uiso 1 1 calc R . . C5 C 0.8232(10) 0.6244(10) 0.3593(10) 0.058(2) Uani 1 1 d . . . H5 H 0.8714 0.7246 0.3172 0.069 Uiso 1 1 calc R . . C6 C 0.7870(9) 0.5138(9) 0.2806(8) 0.0469(16) Uani 1 1 d . . . H6 H 0.8101 0.5340 0.1854 0.056 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 Bi1 0.01908(9) 0.03703(12) 0.01856(9) -0.00112(7) -0.00246(6) -0.00111(7) Cl1 0.0298(6) 0.0363(7) 0.0305(6) 0.0011(5) -0.0076(5) 0.0026(5) Cl2 0.0303(6) 0.0606(9) 0.0183(5) 0.0031(6) -0.0011(5) 0.0093(6) Cl3 0.0352(7) 0.0739(12) 0.0239(6) 0.0063(7) 0.0033(5) 0.0095(7) Cl4 0.0588(10) 0.0404(8) 0.0551(10) -0.0022(7) -0.0231(8) -0.0095(8) N1 0.035(2) 0.036(3) 0.030(2) -0.005(2) -0.002(2) 0.002(2) N2 0.028(2) 0.047(3) 0.022(2) 0.005(2) -0.0008(18) 0.005(2) N3 0.034(2) 0.048(3) 0.027(2) 0.000(2) -0.0038(19) 0.000(2) C1 0.022(2) 0.043(3) 0.029(3) 0.004(2) -0.003(2) 0.005(2) C2 0.022(2) 0.046(3) 0.028(3) -0.001(2) -0.007(2) 0.008(2) C3 0.028(3) 0.064(5) 0.049(4) -0.019(3) -0.012(3) 0.014(3) C4 0.030(3) 0.051(4) 0.092(6) -0.020(4) -0.016(4) 0.007(3) C5 0.034(3) 0.045(4) 0.089(6) 0.005(4) -0.011(4) 0.004(3) C6 0.036(3) 0.049(4) 0.050(4) 0.012(3) -0.005(3) -0.001(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 Bi1 Cl4 2.4897(17) . ? Bi1 Cl3 2.5119(15) . ? Bi1 Cl1 2.6727(13) . ? Bi1 Cl2 2.7840(14) . ? Bi1 Cl2 2.9905(14) 2_655 ? Cl2 Bi1 2.9905(14) 2_655 ? N1 N3 1.323(7) . ? N1 C1 1.356(8) . ? N1 H1 0.8800 . ? N2 N3 1.305(7) . ? N2 C2 1.354(8) . ? N2 H2 0.8800 . ? C1 C6 1.396(9) . ? C1 C2 1.400(8) . ? C2 C3 1.421(9) . ? C3 C4 1.383(12) . ? C3 H3 0.9500 . ? C4 C5 1.409(13) . ? C4 H4 0.9500 . ? C5 C6 1.365(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? 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 Cl4 Bi1 Cl3 94.72(7) . . ? Cl4 Bi1 Cl1 91.94(5) . . ? Cl3 Bi1 Cl1 93.00(5) . . ? Cl4 Bi1 Cl2 91.98(6) . . ? Cl3 Bi1 Cl2 86.38(5) . . ? Cl1 Bi1 Cl2 176.06(5) . . ? Cl4 Bi1 Cl2 88.43(6) . 2_655 ? Cl3 Bi1 Cl2 165.97(5) . 2_655 ? Cl1 Bi1 Cl2 100.56(4) . 2_655 ? Cl2 Bi1 Cl2 79.84(4) . 2_655 ? Bi1 Cl2 Bi1 100.16(4) . 2_655 ? N3 N1 C1 113.0(5) . . ? N3 N1 H1 123.5 . . ? C1 N1 H1 123.5 . . ? N3 N2 C2 113.1(5) . . ? N3 N2 H2 123.4 . . ? C2 N2 H2 123.4 . . ? N2 N3 N1 104.7(5) . . ? N1 C1 C6 133.6(6) . . ? N1 C1 C2 104.1(5) . . ? C6 C1 C2 122.3(6) . . ? N2 C2 C1 105.0(5) . . ? N2 C2 C3 134.1(6) . . ? C1 C2 C3 120.9(6) . . ? C4 C3 C2 115.9(7) . . ? C4 C3 H3 122.0 . . ? C2 C3 H3 122.0 . . ? C3 C4 C5 121.9(8) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 122.6(8) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 116.4(7) . . ? C5 C6 H6 121.8 . . ? C1 C6 H6 121.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl4 Bi1 Cl2 Bi1 -88.05(6) . . . 2_655 ? Cl3 Bi1 Cl2 Bi1 177.34(7) . . . 2_655 ? Cl1 Bi1 Cl2 Bi1 96.3(6) . . . 2_655 ? Cl2 Bi1 Cl2 Bi1 0.0 2_655 . . 2_655 ? C2 N2 N3 N1 0.7(6) . . . . ? C1 N1 N3 N2 -0.3(7) . . . . ? N3 N1 C1 C6 -178.5(6) . . . . ? N3 N1 C1 C2 -0.2(6) . . . . ? N3 N2 C2 C1 -0.9(6) . . . . ? N3 N2 C2 C3 177.9(6) . . . . ? N1 C1 C2 N2 0.6(6) . . . . ? C6 C1 C2 N2 179.1(5) . . . . ? N1 C1 C2 C3 -178.4(5) . . . . ? C6 C1 C2 C3 0.1(9) . . . . ? N2 C2 C3 C4 -178.0(6) . . . . ? C1 C2 C3 C4 0.7(8) . . . . ? C2 C3 C4 C5 -0.7(10) . . . . ? C3 C4 C5 C6 0.0(11) . . . . ? C4 C5 C6 C1 0.8(10) . . . . ? N1 C1 C6 C5 177.2(6) . . . . ? C2 C1 C6 C5 -0.8(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl1 0.88 2.64 3.338(5) 136.8 1_655 N1 H1 Cl2 0.88 2.95 3.409(5) 114.7 . N1 H1 Cl4 0.88 2.95 3.411(6) 114.5 . N2 H2 Cl2 0.88 2.33 3.186(5) 163.9 2_656 N2 H2 N3 0.88 2.64 3.074(8) 111.2 2_656 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.812 _refine_diff_density_min -1.212 _refine_diff_density_rms 0.222 #=END