Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Choudbury, Amitava' 'Krishnamoorthy, Jayaraman' 'Rao, C. N. R.' _publ_contact_author_name 'Prof C N R Rao' _publ_contact_author_address ; Chemistry & Physics of Materials Unit Jawaharlal Nehru Centre for Advanced Scientific Research Jaakur P.O. Bangalore 560 064 INDIA ; _publ_contact_author_email 'CNRRAO@JNCASR.AC.IN' _publ_section_title ; An approach to the synthesis of organically templated open-framework metal sulfates by the amine-sulfate route. ; #compoundI data_sad _database_code_CSD 171678 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2 H7 Cd0.50 Cl N O2.50 S0.50' _chemical_formula_weight 192.77 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Cd' 'Cd' -0.8075 1.2024 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3500(4) _cell_length_b 7.4689(3) _cell_length_c 9.4289(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.1340(10) _cell_angle_gamma 90.00 _cell_volume 591.14(4) _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 'rod shaped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.166 _exptl_crystal_density_method ? _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 2.478 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.764849 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2509 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 23.24 _reflns_number_total 1582 _reflns_number_observed 1539 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0257P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 1582 _refine_ls_number_parameters 144 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_obs 0.0215 _refine_ls_wR_factor_all 0.0543 _refine_ls_wR_factor_obs 0.0541 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.071 _refine_ls_restrained_S_all 1.058 _refine_ls_restrained_S_obs 1.071 _refine_ls_shift/esd_max 0.013 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S 0.19362(11) 0.6041(3) 0.32497(12) 0.0183(2) Uani 1 d . . Cd1 Cd -0.00010(5) 0.36671(13) 0.50656(5) 0.02078(12) Uani 1 d . . O1 O 0.0774(4) 0.5702(6) 0.1639(4) 0.0429(13) Uani 1 d . . O2 O 0.1959(4) 0.4585(5) 0.4307(4) 0.0275(9) Uani 1 d . . O3 O 0.1650(5) 0.7773(6) 0.3833(5) 0.0367(10) Uani 1 d . . O4 O 0.3549(3) 0.6100(11) 0.3308(3) 0.0267(7) Uani 1 d . . Cl1 Cl 0.20118(11) 0.1134(3) 0.66322(11) 0.0258(2) Uani 1 d . . Cl2 Cl -0.11745(12) 0.1250(3) 0.28043(12) 0.0256(3) Uani 1 d . . N1 N 0.2341(4) 0.1036(8) 0.0378(4) 0.0247(8) Uani 1 d . . H1 H 0.1437(4) 0.0944(8) -0.0525(4) 0.030 Uiso 1 calc R . H2 H 0.2840(4) 0.2049(8) 0.0333(4) 0.030 Uiso 1 calc R . C1 C 0.1945(5) 0.1126(12) 0.1744(5) 0.0317(10) Uani 1 d . . H3 H 0.1326(5) 0.0081(12) 0.1739(5) 0.038 Uiso 1 calc R . H4 H 0.1303(5) 0.2181(12) 0.1647(5) 0.038 Uiso 1 calc R . C2 C 0.3436(6) 0.1202(19) 0.3277(5) 0.0433(14) Uani 1 d . . H5 H 0.3983(6) 0.2324(19) 0.3341(5) 0.052 Uiso 1 calc R . H6 H 0.3155(6) 0.1157(19) 0.4152(5) 0.052 Uiso 1 calc R . N2 N 0.4522(5) -0.0318(6) 0.3410(5) 0.0358(12) Uani 1 d . . H7 H 0.5435(5) -0.0195(6) 0.4300(5) 0.043 Uiso 1 calc R . H8 H 0.4062(5) -0.1353(6) 0.3474(5) 0.043 Uiso 1 calc R . C3 C 0.4887(6) -0.0383(8) 0.2026(8) 0.043(2) Uani 1 d . . H9 H 0.5560(6) -0.1407(8) 0.2121(8) 0.051 Uiso 1 calc R . H10 H 0.5460(6) 0.0691(8) 0.2003(8) 0.051 Uiso 1 calc R . C4 C 0.3378(7) -0.0521(9) 0.0528(7) 0.0374(14) Uani 1 d . . H11 H 0.3627(7) -0.0557(9) -0.0368(7) 0.045 Uiso 1 calc R . H12 H 0.2826(7) -0.1619(9) 0.0532(7) 0.045 Uiso 1 calc R . O100 O 0.3596(6) 0.4500(6) 0.0539(6) 0.0395(10) Uani 1 d . . H14 H 0.3494(73) 0.5114(87) 0.1449(87) 0.058(19) Uiso 1 d . . H13 H 0.3286(92) 0.5108(109) -0.0120(97) 0.071(30) Uiso 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 S1 0.0163(5) 0.0216(6) 0.0158(5) 0.0027(6) 0.0059(4) 0.0018(7) Cd1 0.0240(2) 0.0170(2) 0.0221(2) 0.0012(2) 0.01083(13) -0.00032(11) O1 0.024(2) 0.070(4) 0.023(2) -0.005(2) -0.0010(15) 0.003(2) O2 0.030(2) 0.022(2) 0.034(2) 0.009(2) 0.018(2) 0.002(2) O3 0.050(3) 0.021(2) 0.054(3) 0.001(2) 0.037(2) 0.002(2) O4 0.0188(13) 0.030(2) 0.031(2) 0.000(4) 0.0114(13) 0.001(3) Cl1 0.0243(5) 0.0229(5) 0.0234(5) 0.0024(7) 0.0042(4) -0.0011(9) Cl2 0.0301(5) 0.0245(6) 0.0193(5) -0.0002(6) 0.0081(4) -0.0002(8) N1 0.019(2) 0.030(2) 0.018(2) 0.003(2) 0.0017(15) 0.000(3) C1 0.033(2) 0.031(2) 0.036(3) 0.000(4) 0.020(2) -0.002(4) C2 0.071(3) 0.036(3) 0.023(3) -0.006(5) 0.020(3) -0.016(7) N2 0.033(2) 0.030(3) 0.018(2) 0.010(2) -0.013(2) -0.012(2) C3 0.025(3) 0.045(3) 0.052(4) 0.018(3) 0.011(3) 0.012(3) C4 0.045(3) 0.039(3) 0.032(3) 0.003(3) 0.020(3) 0.012(3) O100 0.054(3) 0.034(2) 0.037(3) 0.003(2) 0.026(2) 0.003(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 S1 O1 1.448(3) . ? S1 O2 1.470(4) . ? S1 O3 1.476(5) . ? S1 O4 1.485(3) . ? Cd1 O3 2.305(4) 2_546 ? Cd1 O2 2.344(4) . ? Cd1 Cl1 2.616(2) 2_556 ? Cd1 Cl1 2.618(2) . ? Cd1 Cl2 2.636(2) . ? Cd1 Cl2 2.649(2) 2_556 ? O3 Cd1 2.305(4) 2_556 ? Cl1 Cd1 2.616(2) 2_546 ? Cl2 Cd1 2.649(2) 2_546 ? N1 C4 1.480(8) . ? N1 C1 1.490(6) . ? N1 H1 0.90 . ? N1 H2 0.90 . ? C1 C2 1.504(6) . ? C1 H3 0.97 . ? C1 H4 0.97 . ? C2 N2 1.491(12) . ? C2 H5 0.97 . ? C2 H6 0.97 . ? N2 C3 1.487(8) . ? N2 H7 0.90 . ? N2 H8 0.90 . ? C3 C4 1.497(8) . ? C3 H9 0.97 . ? C3 H10 0.97 . ? C4 H11 0.97 . ? C4 H12 0.97 . ? O100 H14 1.01(8) . ? O100 H13 0.72(8) . ? 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 O1 S1 O2 111.2(3) . . ? O1 S1 O3 111.7(2) . . ? O2 S1 O3 110.3(2) . . ? O1 S1 O4 108.9(2) . . ? O2 S1 O4 106.6(3) . . ? O3 S1 O4 107.9(4) . . ? O3 Cd1 O2 172.0(2) 2_546 . ? O3 Cd1 Cl1 92.10(11) 2_546 2_556 ? O2 Cd1 Cl1 93.16(10) . 2_556 ? O3 Cd1 Cl1 89.65(12) 2_546 . ? O2 Cd1 Cl1 85.36(10) . . ? Cl1 Cd1 Cl1 177.07(4) 2_556 . ? O3 Cd1 Cl2 92.48(12) 2_546 . ? O2 Cd1 Cl2 93.23(10) . . ? Cl1 Cd1 Cl2 93.25(4) 2_556 . ? Cl1 Cd1 Cl2 84.33(7) . . ? O3 Cd1 Cl2 90.33(11) 2_546 2_556 ? O2 Cd1 Cl2 84.23(11) . 2_556 ? Cl1 Cd1 Cl2 84.11(7) 2_556 2_556 ? Cl1 Cd1 Cl2 98.24(4) . 2_556 ? Cl2 Cd1 Cl2 176.21(7) . 2_556 ? S1 O2 Cd1 130.1(2) . . ? S1 O3 Cd1 133.6(3) . 2_556 ? Cd1 Cl1 Cd1 91.11(3) 2_546 . ? Cd1 Cl2 Cd1 89.98(3) . 2_546 ? C4 N1 C1 110.8(5) . . ? C4 N1 H1 109.5(3) . . ? C1 N1 H1 109.5(2) . . ? C4 N1 H2 109.5(3) . . ? C1 N1 H2 109.5(4) . . ? H1 N1 H2 108.1 . . ? N1 C1 C2 110.8(4) . . ? N1 C1 H3 109.5(4) . . ? C2 C1 H3 109.5(6) . . ? N1 C1 H4 109.5(4) . . ? C2 C1 H4 109.5(6) . . ? H3 C1 H4 108.1 . . ? N2 C2 C1 111.2(8) . . ? N2 C2 H5 109.4(4) . . ? C1 C2 H5 109.4(6) . . ? N2 C2 H6 109.4(3) . . ? C1 C2 H6 109.4(3) . . ? H5 C2 H6 108.0 . . ? C3 N2 C2 111.2(4) . . ? C3 N2 H7 109.4(3) . . ? C2 N2 H7 109.4(3) . . ? C3 N2 H8 109.4(3) . . ? C2 N2 H8 109.4(4) . . ? H7 N2 H8 108.0 . . ? N2 C3 C4 110.2(5) . . ? N2 C3 H9 109.6(3) . . ? C4 C3 H9 109.6(3) . . ? N2 C3 H10 109.6(3) . . ? C4 C3 H10 109.6(3) . . ? H9 C3 H10 108.1 . . ? N1 C4 C3 110.0(5) . . ? N1 C4 H11 109.7(3) . . ? C3 C4 H11 109.7(3) . . ? N1 C4 H12 109.7(3) . . ? C3 C4 H12 109.7(3) . . ? H11 C4 H12 108.2 . . ? H14 O100 H13 107.0(72) . . ? _refine_diff_density_max 0.336 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.117 #===END #compoundII data_sad1 _database_code_CSD 171679 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H15 Cd1.50 Cl5 N4 O6 S' _chemical_formula_weight 641.15 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Cd' 'Cd' -0.8075 1.2024 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 12.578(2) _cell_length_b 13.093(4) _cell_length_c 13.006(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.58(2) _cell_angle_gamma 90.00 _cell_volume 2135.0(9) _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 Chunky _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method ? _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 2.261 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.691112 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8916 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 23.28 _reflns_number_total 3216 _reflns_number_observed 2467 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+2.9456P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3216 _refine_ls_number_parameters 246 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_obs 0.0376 _refine_ls_wR_factor_all 0.0946 _refine_ls_wR_factor_obs 0.0864 _refine_ls_goodness_of_fit_all 1.053 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.052 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.75790(5) 0.2500 0.66038(5) 0.0222(2) Uani 1 d S . Cd2 Cd 1.19390(5) 0.2500 0.23874(5) 0.0268(2) Uani 1 d S . Cd3 Cd 0.75897(5) 0.2500 0.26691(5) 0.0307(2) Uani 1 d S . S1 S 0.75906(12) 0.00049(12) 0.76778(11) 0.0210(4) Uani 1 d . . O1 O 0.6932(5) 0.2500 0.8199(4) 0.0282(15) Uani 1 d SD . O2 O 0.7526(3) 0.0711(3) 0.6794(3) 0.0305(11) Uani 1 d . . O3 O 0.8578(3) -0.0614(4) 0.7669(3) 0.0425(13) Uani 1 d . . O4 O 0.6681(3) -0.0706(4) 0.7572(3) 0.0335(12) Uani 1 d . . O5 O 0.7568(4) 0.0555(3) 0.8663(3) 0.0368(12) Uani 1 d . . Cl1 Cl 0.8160(2) 0.2500 0.4746(2) 0.0453(7) Uani 1 d S . Cl2 Cl 0.9529(2) 0.2500 0.7438(2) 0.0566(9) Uani 1 d S . Cl3 Cl 0.5587(2) 0.2500 0.5853(2) 0.0317(6) Uani 1 d S . Cl4 Cl 1.2401(2) 0.2500 0.0591(2) 0.0326(6) Uani 1 d S . Cl5 Cl 1.2625(2) 0.2500 0.4211(2) 0.0299(6) Uani 1 d S . Cl6 Cl 0.9931(2) 0.2500 0.2628(2) 0.0503(7) Uani 1 d S . Cl7 Cl 0.5581(2) 0.2500 0.2661(2) 0.0374(6) Uani 1 d S . Cl8 Cl 0.7706(2) 0.2500 0.0675(2) 0.0418(7) Uani 1 d S . Cl9 Cl 0.78660(14) 0.05195(14) 0.26809(14) 0.0416(5) Uani 1 d . . C1 C 0.4709(5) -0.0018(6) 0.8905(5) 0.035(2) Uani 1 d . . H3 H 0.4350(5) -0.0354(6) 0.8310(5) 0.042 Uiso 1 calc R . H4 H 0.5033(5) 0.0603(6) 0.8669(5) 0.042 Uiso 1 calc R . N1 N 0.5554(4) -0.0701(5) 0.9378(4) 0.0353(14) Uani 1 d . . H1 H 0.6042(4) -0.0815(5) 0.8921(4) 0.042 Uiso 1 calc R . H2 H 0.5263(4) -0.1305(5) 0.9529(4) 0.042 Uiso 1 calc R . C2 C 0.6096(5) -0.0251(6) 1.0340(5) 0.040(2) Uani 1 d . . H5 H 0.6484(5) 0.0358(6) 1.0169(5) 0.048 Uiso 1 calc R . H6 H 0.6604(5) -0.0738(6) 1.0654(5) 0.048 Uiso 1 calc R . C3 C 0.4654(5) -0.0083(5) 0.6034(4) 0.028(2) Uani 1 d . . H9 H 0.4998(5) 0.0494(5) 0.6390(4) 0.034 Uiso 1 calc R . H10 H 0.4241(5) -0.0443(5) 0.6519(4) 0.034 Uiso 1 calc R . N2 N 0.5482(4) -0.0781(4) 0.5666(4) 0.0288(13) Uani 1 d . . H7 H 0.5939(4) -0.0961(4) 0.6203(4) 0.035 Uiso 1 calc R . H8 H 0.5165(4) -0.1353(4) 0.5409(4) 0.035 Uiso 1 calc R . C4 C 0.6082(5) -0.0297(5) 0.4863(5) 0.032(2) Uani 1 d . . H11 H 0.6579(5) -0.0788(5) 0.4614(5) 0.039 Uiso 1 calc R . H12 H 0.6492(5) 0.0272(5) 0.5163(5) 0.039 Uiso 1 calc R . O100 O 0.5285(6) 0.2500 0.9851(6) 0.042(2) Uani 1 d SD . O200 O 0.4341(7) 0.2500 0.7915(6) 0.084(3) Uani 1 d SD . C5 C 0.9935(6) 0.1106(5) -0.0032(5) 0.037(2) Uiso 1 d . . C6 C 0.9304(6) -0.0524(7) 0.0657(6) 0.053(2) Uiso 1 d . . C7 C 1.0568(7) 0.0927(7) 0.5275(6) 0.062(2) Uiso 1 d . . C8 C 1.0099(6) -0.0377(6) 0.3979(5) 0.042(2) Uiso 1 d . . N3 N 0.9592(8) 0.0573(8) 0.0827(7) 0.040(3) Uiso 0.60 d P . N3A N 0.9011(10) 0.0364(10) 0.0379(9) 0.024(3) Uiso 0.40 d P . N4 N 1.0141(8) 0.0531(9) 0.4061(8) 0.051(3) Uiso 0.60 d P . N4A N 1.1033(11) 0.0332(11) 0.4638(10) 0.034(3) Uiso 0.40 d P . O300 O 0.2177(11) 0.2004(11) 0.7430(10) 0.109(7) Uiso 0.51(2) d P . H13 H 0.7036(62) 0.1830(25) 0.8478(54) 0.076(28) Uiso 1 d D . H14 H 0.6044(14) 0.2500 0.9999(80) 0.070(39) Uiso 1 d SD . H15 H 0.5049(103) 0.2500 0.9132(26) 0.110(55) Uiso 1 d SD . H16 H 0.3605(19) 0.2500 0.7673(59) 0.029(25) Uiso 1 d SD . H17 H 0.4838(125) 0.2500 0.7392(113) 0.232(114) Uiso 1 d SD . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0250(4) 0.0229(4) 0.0183(3) 0.000 -0.0008(3) 0.000 Cd2 0.0275(4) 0.0323(4) 0.0204(4) 0.000 0.0014(3) 0.000 Cd3 0.0310(4) 0.0359(5) 0.0248(4) 0.000 0.0008(3) 0.000 S1 0.0197(8) 0.0222(9) 0.0201(8) 0.0012(7) -0.0039(6) -0.0001(7) O1 0.036(4) 0.024(4) 0.025(3) 0.000 0.003(3) 0.000 O2 0.046(3) 0.023(3) 0.021(2) 0.006(2) -0.007(2) -0.002(2) O3 0.024(3) 0.060(4) 0.044(3) 0.014(3) 0.002(2) 0.015(2) O4 0.030(3) 0.047(3) 0.023(2) 0.001(2) -0.001(2) -0.019(2) O5 0.063(3) 0.028(3) 0.018(2) -0.002(2) -0.005(2) -0.002(2) Cl1 0.044(2) 0.073(2) 0.0193(12) 0.000 0.0017(11) 0.000 Cl2 0.030(2) 0.106(3) 0.0325(14) 0.000 -0.0058(12) 0.000 Cl3 0.0291(13) 0.0299(14) 0.0340(13) 0.000 -0.0105(10) 0.000 Cl4 0.0354(14) 0.0380(15) 0.0247(12) 0.000 0.0049(10) 0.000 Cl5 0.0315(14) 0.0302(14) 0.0267(12) 0.000 -0.0054(10) 0.000 Cl6 0.0278(15) 0.068(2) 0.054(2) 0.000 0.0015(13) 0.000 Cl7 0.0317(14) 0.037(2) 0.0433(14) 0.000 0.0045(11) 0.000 Cl8 0.0369(15) 0.066(2) 0.0223(12) 0.000 0.0018(11) 0.000 Cl9 0.0328(10) 0.0378(11) 0.0542(11) -0.0077(9) 0.0023(9) 0.0001(8) C1 0.035(4) 0.044(5) 0.027(4) -0.006(3) 0.005(3) 0.000(4) N1 0.030(3) 0.045(4) 0.034(3) -0.010(3) 0.015(3) -0.002(3) C2 0.028(4) 0.057(5) 0.036(4) -0.010(4) 0.000(3) -0.001(4) C3 0.034(4) 0.027(4) 0.024(4) -0.002(3) -0.001(3) 0.003(3) N2 0.029(3) 0.032(3) 0.023(3) 0.000(2) -0.013(2) 0.003(3) C4 0.027(4) 0.040(4) 0.030(4) 0.000(3) 0.000(3) 0.006(3) O100 0.035(5) 0.043(5) 0.049(5) 0.000 0.009(4) 0.000 O200 0.048(6) 0.162(11) 0.040(5) 0.000 -0.003(5) 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 Cd1 O1 2.288(6) . ? Cd1 O2 2.357(4) 4_565 ? Cd1 O2 2.357(4) . ? Cd1 Cl1 2.579(2) . ? Cd1 Cl2 2.601(3) . ? Cd1 Cl3 2.616(2) . ? Cd2 Cl4 2.452(2) . ? Cd2 Cl5 2.458(2) . ? Cd2 O3 2.552(5) 2_756 ? Cd2 O3 2.552(5) 3_756 ? Cd2 Cl6 2.569(3) . ? Cd3 Cl7 2.525(3) . ? Cd3 Cl8 2.609(2) . ? Cd3 Cl9 2.616(2) . ? Cd3 Cl9 2.616(2) 4_565 ? Cd3 Cl1 2.739(2) . ? Cd3 Cl6 2.950(3) . ? S1 O2 1.472(4) . ? S1 O5 1.472(4) . ? S1 O4 1.472(4) . ? S1 O3 1.483(5) . ? O1 H13 0.955(10) . ? O3 Cd2 2.552(5) 3_756 ? C1 N1 1.484(8) . ? C1 C2 1.507(8) 3_657 ? C1 H3 0.97 . ? C1 H4 0.97 . ? N1 C2 1.497(8) . ? N1 H1 0.90 . ? N1 H2 0.90 . ? C2 C1 1.507(8) 3_657 ? C2 H5 0.97 . ? C2 H6 0.97 . ? C3 N2 1.493(8) . ? C3 C4 1.515(8) 3_656 ? C3 H9 0.97 . ? C3 H10 0.97 . ? N2 C4 1.479(8) . ? N2 H7 0.90 . ? N2 H8 0.90 . ? C4 C3 1.515(8) 3_656 ? C4 H11 0.97 . ? C4 H12 0.97 . ? O100 H14 0.959(10) . ? O100 H15 0.959(10) . ? O200 H16 0.954(10) . ? O200 H17 0.959(10) . ? C5 N3 1.415(11) . ? C5 C6 1.510(10) 3_755 ? C5 N3A 1.637(14) . ? C6 N3A 1.263(14) . ? C6 N3 1.493(13) . ? C6 C5 1.510(10) 3_755 ? C7 N4A 1.309(15) . ? C7 C8 1.515(11) 3_756 ? C7 N4 1.707(13) . ? C8 N4 1.194(12) . ? C8 C7 1.515(11) 3_756 ? C8 N4A 1.677(15) . ? N3 N3A 0.939(13) . ? N4 N4A 1.32(2) . ? O300 O300 1.30(3) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O2 83.68(10) . 4_565 ? O1 Cd1 O2 83.68(10) . . ? O2 Cd1 O2 167.3(2) 4_565 . ? O1 Cd1 Cl1 175.6(2) . . ? O2 Cd1 Cl1 96.36(10) 4_565 . ? O2 Cd1 Cl1 96.36(10) . . ? O1 Cd1 Cl2 90.8(2) . . ? O2 Cd1 Cl2 89.41(10) 4_565 . ? O2 Cd1 Cl2 89.40(10) . . ? Cl1 Cd1 Cl2 93.60(8) . . ? O1 Cd1 Cl3 86.5(2) . . ? O2 Cd1 Cl3 90.29(10) 4_565 . ? O2 Cd1 Cl3 90.29(10) . . ? Cl1 Cd1 Cl3 89.12(8) . . ? Cl2 Cd1 Cl3 177.27(8) . . ? Cl4 Cd2 Cl5 145.84(8) . . ? Cl4 Cd2 O3 92.97(10) . 2_756 ? Cl5 Cd2 O3 95.55(10) . 2_756 ? Cl4 Cd2 O3 92.97(10) . 3_756 ? Cl5 Cd2 O3 95.55(10) . 3_756 ? O3 Cd2 O3 150.6(2) 2_756 3_756 ? Cl4 Cd2 Cl6 115.24(8) . . ? Cl5 Cd2 Cl6 98.92(8) . . ? O3 Cd2 Cl6 75.71(10) 2_756 . ? O3 Cd2 Cl6 75.71(10) 3_756 . ? Cl7 Cd3 Cl8 97.53(8) . . ? Cl7 Cd3 Cl9 97.61(4) . . ? Cl8 Cd3 Cl9 89.30(4) . . ? Cl7 Cd3 Cl9 97.61(4) . 4_565 ? Cl8 Cd3 Cl9 89.30(4) . 4_565 ? Cl9 Cd3 Cl9 164.77(8) . 4_565 ? Cl7 Cd3 Cl1 100.80(8) . . ? Cl8 Cd3 Cl1 161.67(9) . . ? Cl9 Cd3 Cl1 88.28(4) . . ? Cl9 Cd3 Cl1 88.28(4) 4_565 . ? Cl7 Cd3 Cl6 178.72(8) . . ? Cl8 Cd3 Cl6 81.19(8) . . ? Cl9 Cd3 Cl6 82.40(4) . . ? Cl9 Cd3 Cl6 82.40(4) 4_565 . ? Cl1 Cd3 Cl6 80.48(8) . . ? O2 S1 O5 111.6(3) . . ? O2 S1 O4 109.3(2) . . ? O5 S1 O4 108.7(3) . . ? O2 S1 O3 109.3(3) . . ? O5 S1 O3 110.4(3) . . ? O4 S1 O3 107.4(3) . . ? Cd1 O1 H13 107.3(47) . . ? S1 O2 Cd1 134.9(2) . . ? S1 O3 Cd2 108.5(2) . 3_756 ? Cd1 Cl1 Cd3 148.48(11) . . ? Cd2 Cl6 Cd3 174.04(11) . . ? N1 C1 C2 111.5(5) . 3_657 ? N1 C1 H3 109.3(3) . . ? C2 C1 H3 109.3(4) 3_657 . ? N1 C1 H4 109.3(4) . . ? C2 C1 H4 109.3(4) 3_657 . ? H3 C1 H4 108.0 . . ? C1 N1 C2 111.9(5) . . ? C1 N1 H1 109.2(3) . . ? C2 N1 H1 109.2(3) . . ? C1 N1 H2 109.2(4) . . ? C2 N1 H2 109.2(4) . . ? H1 N1 H2 107.9 . . ? N1 C2 C1 110.6(5) . 3_657 ? N1 C2 H5 109.5(4) . . ? C1 C2 H5 109.5(4) 3_657 . ? N1 C2 H6 109.5(4) . . ? C1 C2 H6 109.5(4) 3_657 . ? H5 C2 H6 108.1 . . ? N2 C3 C4 110.7(5) . 3_656 ? N2 C3 H9 109.5(3) . . ? C4 C3 H9 109.5(4) 3_656 . ? N2 C3 H10 109.5(3) . . ? C4 C3 H10 109.5(3) 3_656 . ? H9 C3 H10 108.1 . . ? C4 N2 C3 111.9(5) . . ? C4 N2 H7 109.2(3) . . ? C3 N2 H7 109.2(3) . . ? C4 N2 H8 109.2(3) . . ? C3 N2 H8 109.2(3) . . ? H7 N2 H8 107.9 . . ? N2 C4 C3 111.7(5) . 3_656 ? N2 C4 H11 109.3(3) . . ? C3 C4 H11 109.3(3) 3_656 . ? N2 C4 H12 109.3(3) . . ? C3 C4 H12 109.3(4) 3_656 . ? H11 C4 H12 107.9 . . ? H14 O100 H15 114.9(100) . . ? H16 O200 H17 115.9(100) . . ? N3 C5 C6 115.0(7) . 3_755 ? N3 C5 N3A 34.9(5) . . ? C6 C5 N3A 111.9(7) 3_755 . ? N3A C6 N3 38.7(6) . . ? N3A C6 C5 119.5(9) . 3_755 ? N3 C6 C5 114.1(7) . 3_755 ? N4A C7 C8 114.9(9) . 3_756 ? N4A C7 N4 50.0(7) . . ? C8 C7 N4 107.4(7) 3_756 . ? N4 C8 C7 116.0(9) . 3_756 ? N4 C8 N4A 51.6(7) . . ? C7 C8 N4A 109.7(7) 3_756 . ? N3A N3 C5 85.7(11) . . ? N3A N3 C6 57.3(10) . . ? C5 N3 C6 116.3(8) . . ? N3 N3A C6 84.0(12) . . ? N3 N3A C5 59.5(10) . . ? C6 N3A C5 116.2(10) . . ? C8 N4 N4A 83.3(10) . . ? C8 N4 C7 113.2(9) . . ? N4A N4 C7 49.2(7) . . ? C7 N4A N4 80.8(10) . . ? C7 N4A C8 108.8(10) . . ? N4 N4A C8 45.0(7) . . ? _refine_diff_density_max 1.174 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.126