# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Sun Yat-Sen University 135 Xingang Rd. W. Guangzhou 510275 CHINA ; _publ_contact_author_email CXM@MAIL.SYSU.EDU.CN _publ_section_title ; Single-Crystal-to-Single-Crystal Transformation Involving Release of Bridging Water Molecules and Conversion of Chain Helicity in a Chiral Three-Dimensional Metal-Organic Framework ; loop_ _publ_author_name 'Xiao-Ming Chen' 'He-Zhou Wang' 'Dong-Xu Xue' 'Wei-Xiong Zhang' data_1mpm _database_code_depnum_ccdc_archive 'CCDC 666519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium bct' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Cd N2 O5 S3' _chemical_formula_weight 394.71 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.1461(6) _cell_length_b 10.1964(12) _cell_length_c 20.941(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1098.8(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 block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 2.567 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3275 _exptl_absorpt_correction_T_max 0.6148 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11214 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.97 _reflns_number_total 2156 _reflns_number_gt 2152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.0181P)^2^+0.4390P] 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 0.0030(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.014(18) _refine_ls_number_reflns 2156 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0137 _refine_ls_R_factor_gt 0.0136 _refine_ls_wR_factor_ref 0.0362 _refine_ls_wR_factor_gt 0.0362 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.19695(3) 0.598736(16) 0.037363(8) 0.02373(6) Uani 1 1 d . . . S1 S 0.93390(15) -0.01266(7) -0.26136(3) 0.03670(17) Uani 1 1 d . . . S2 S 0.58034(14) 0.20138(6) -0.20367(3) 0.03044(14) Uani 1 1 d . . . S3 S 0.17831(14) 0.24968(6) -0.09860(3) 0.03051(13) Uani 1 1 d . . . O1 O 0.9014(4) 0.26796(17) -0.39202(8) 0.0311(4) Uani 1 1 d . . . O1W O 0.1353(3) 0.76286(16) 0.04488(8) 0.0255(4) Uani 1 1 d . . . H1WA H 0.0691 0.8018 0.0769 0.031 Uiso 1 1 d R . . H1WB H 0.2685 0.7293 0.0624 0.031 Uiso 1 1 d R . . O2 O 0.6052(4) 0.1203(2) -0.36153(8) 0.0347(4) Uani 1 1 d . . . O3 O 0.0202(3) 0.46199(17) -0.02610(9) 0.0304(4) Uani 1 1 d . . . O4 O 0.3902(3) 0.51969(16) 0.02095(8) 0.0298(4) Uani 1 1 d . . . N1 N 0.6000(5) -0.0371(2) -0.16687(10) 0.0321(5) Uani 1 1 d . . . N2 N 0.4286(5) 0.0249(2) -0.12682(9) 0.0282(5) Uani 1 1 d . . . C1 C 0.8189(5) 0.1747(2) -0.35755(10) 0.0242(5) Uani 1 1 d . . . C2 C 1.0137(5) 0.1311(3) -0.30701(12) 0.0322(6) Uani 1 1 d . . . H2A H 1.0387 0.2032 -0.2774 0.039 Uiso 1 1 calc R . . H2B H 1.1789 0.1156 -0.3280 0.039 Uiso 1 1 calc R . . C3 C 0.6988(5) 0.0430(2) -0.20861(10) 0.0258(5) Uani 1 1 d . . . C4 C 0.3976(5) 0.1491(2) -0.13934(11) 0.0255(5) Uani 1 1 d . . . C5 C 0.4089(5) 0.3578(3) -0.05988(13) 0.0318(6) Uani 1 1 d . . . H5A H 0.5283 0.3069 -0.0340 0.038 Uiso 1 1 calc R . . H5B H 0.5089 0.4048 -0.0918 0.038 Uiso 1 1 calc R . . C6 C 0.2630(5) 0.4546(2) -0.01807(11) 0.0242(5) Uani 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 Cd1 0.02436(10) 0.02402(9) 0.02282(9) -0.00279(6) -0.00121(7) 0.00360(7) S1 0.0451(4) 0.0349(3) 0.0301(3) 0.0102(3) 0.0126(3) 0.0156(3) S2 0.0386(3) 0.0234(3) 0.0293(3) 0.0031(2) 0.0080(3) 0.0020(3) S3 0.0266(3) 0.0325(3) 0.0325(3) -0.0090(2) 0.0038(3) -0.0021(3) O1 0.0271(9) 0.0346(9) 0.0316(9) 0.0121(7) -0.0004(8) 0.0004(8) O1W 0.0216(8) 0.0307(8) 0.0243(8) 0.0001(7) 0.0012(7) 0.0040(6) O2 0.0275(9) 0.0452(11) 0.0314(9) 0.0106(8) -0.0022(7) -0.0050(9) O3 0.0219(8) 0.0324(9) 0.0369(10) -0.0092(7) 0.0025(8) 0.0034(7) O4 0.0274(9) 0.0268(9) 0.0351(9) -0.0080(7) -0.0013(7) -0.0008(7) N1 0.0410(12) 0.0278(10) 0.0274(10) 0.0045(8) 0.0069(10) 0.0049(9) N2 0.0328(11) 0.0274(11) 0.0244(10) -0.0008(8) 0.0038(9) -0.0004(9) C1 0.0244(12) 0.0300(12) 0.0182(10) 0.0005(8) 0.0034(10) 0.0051(10) C2 0.0272(12) 0.0411(15) 0.0283(12) 0.0127(10) 0.0034(10) 0.0015(11) C3 0.0305(12) 0.0248(11) 0.0220(10) -0.0017(9) -0.0001(11) 0.0020(10) C4 0.0266(12) 0.0288(12) 0.0212(10) -0.0034(9) -0.0003(9) -0.0032(10) C5 0.0259(12) 0.0308(12) 0.0387(13) -0.0137(10) -0.0003(11) 0.0039(11) C6 0.0234(13) 0.0202(10) 0.0288(11) 0.0004(9) 0.0033(9) -0.0006(9) _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 O3 2.2269(17) . ? Cd1 O1 2.2676(17) 2_565 ? Cd1 O4 2.2983(17) 1_455 ? Cd1 N2 2.348(2) 4_455 ? Cd1 O1W 2.3882(16) 4_465 ? Cd1 O1W 2.3974(17) . ? S1 C3 1.734(3) . ? S1 C2 1.797(3) . ? S2 C4 1.727(3) . ? S2 C3 1.729(2) . ? S3 C4 1.747(3) . ? S3 C5 1.812(3) . ? O1 C1 1.267(3) . ? O1 Cd1 2.2676(17) 2_564 ? O1W Cd1 2.3882(16) 4_565 ? O2 C1 1.235(3) . ? O3 C6 1.263(3) . ? O4 C6 1.239(3) . ? O4 Cd1 2.2983(17) 1_655 ? N1 C3 1.300(3) . ? N1 N2 1.372(3) . ? N2 C4 1.304(3) . ? N2 Cd1 2.348(2) 4 ? C1 C2 1.524(3) . ? C5 C6 1.518(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 O3 Cd1 O1 175.86(7) . 2_565 ? O3 Cd1 O4 98.92(6) . 1_455 ? O1 Cd1 O4 83.04(6) 2_565 1_455 ? O3 Cd1 N2 90.11(7) . 4_455 ? O1 Cd1 N2 85.93(7) 2_565 4_455 ? O4 Cd1 N2 100.68(7) 1_455 4_455 ? O3 Cd1 O1W 96.96(6) . 4_465 ? O1 Cd1 O1W 87.04(6) 2_565 4_465 ? O4 Cd1 O1W 76.42(6) 1_455 4_465 ? N2 Cd1 O1W 172.68(7) 4_455 4_465 ? O3 Cd1 O1W 96.80(6) . . ? O1 Cd1 O1W 82.51(6) 2_565 . ? O4 Cd1 O1W 156.04(6) 1_455 . ? N2 Cd1 O1W 97.25(7) 4_455 . ? O1W Cd1 O1W 83.84(4) 4_465 . ? C3 S1 C2 103.39(12) . . ? C4 S2 C3 87.17(12) . . ? C4 S3 C5 98.78(12) . . ? C1 O1 Cd1 131.75(17) . 2_564 ? Cd1 O1W Cd1 128.53(7) 4_565 . ? C6 O3 Cd1 117.02(16) . . ? C6 O4 Cd1 140.76(16) . 1_655 ? C3 N1 N2 111.9(2) . . ? C4 N2 N1 113.8(2) . . ? C4 N2 Cd1 130.42(17) . 4 ? N1 N2 Cd1 114.68(14) . 4 ? O2 C1 O1 126.7(2) . . ? O2 C1 C2 120.1(2) . . ? O1 C1 C2 113.2(2) . . ? C1 C2 S1 117.20(19) . . ? N1 C3 S2 114.11(19) . . ? N1 C3 S1 119.73(18) . . ? S2 C3 S1 126.14(14) . . ? N2 C4 S2 113.0(2) . . ? N2 C4 S3 123.4(2) . . ? S2 C4 S3 123.49(15) . . ? C6 C5 S3 109.26(19) . . ? O4 C6 O3 125.3(2) . . ? O4 C6 C5 117.8(2) . . ? O3 C6 C5 116.8(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.393 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.058 # Attachment '2pmm.cif' data_2pmm _database_code_depnum_ccdc_archive 'CCDC 666520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium bct' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 Cd N2 O4 S3' _chemical_formula_weight 376.69 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 4.723(3) _cell_length_b 8.316(6) _cell_length_c 25.618(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1006.2(12) _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 block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 2.789 _exptl_absorpt_correction_T_min 0.8287 _exptl_absorpt_correction_T_max 0.8966 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method '\w scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5685 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1958 _reflns_number_gt 1599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _refine_special_details ; Since 2pmm comes from the dehydrated 1mpm and crystal quality of 2pmm is not as good as before, displacement parameters of C2 atom become unreasonable while refined anisotropically. Therefore, isor instruction is used to restrain its displacement parameters ; _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^)+(0.0523P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(8) _refine_ls_number_reflns 1958 _refine_ls_number_parameters 145 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.078 _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 Cd1 Cd -0.18697(19) -0.15410(10) 0.06271(3) 0.0229(2) Uani 1 1 d . . . S1 S -0.9516(7) 0.4083(4) -0.27485(12) 0.0317(8) Uani 1 1 d . . . S2 S -0.5300(7) 0.2453(4) -0.19880(11) 0.0318(7) Uani 1 1 d . . . S3 S -0.3086(8) 0.2505(3) -0.08713(10) 0.0300(6) Uani 1 1 d . . . O1 O -1.1292(15) 0.3149(8) -0.3739(3) 0.0254(19) Uani 1 1 d . . . O2 O -0.7634(17) 0.1786(9) -0.4025(3) 0.037(2) Uani 1 1 d . . . O3 O -0.211(2) 0.0453(9) 0.0032(3) 0.035(2) Uani 1 1 d . . . O4 O -0.5395(19) -0.1366(9) -0.0115(3) 0.033(2) Uani 1 1 d . . . N1 N -0.846(2) 0.4851(10) -0.1763(3) 0.029(2) Uani 1 1 d . . . N2 N -0.701(3) 0.4487(11) -0.1322(3) 0.034(2) Uani 1 1 d . . . C1 C -0.884(2) 0.2612(13) -0.3695(4) 0.015(2) Uani 1 1 d . . . C2 C -0.726(2) 0.2903(12) -0.3165(4) 0.022(3) Uani 1 1 d U . . H2A H -0.5496 0.3465 -0.3227 0.026 Uiso 1 1 d R . . H2B H -0.6839 0.1881 -0.3000 0.026 Uiso 1 1 d R . . C3 C -0.772(2) 0.3878(11) -0.2156(4) 0.022(3) Uani 1 1 d . . . C4 C -0.525(2) 0.3248(14) -0.1368(4) 0.022(2) Uani 1 1 d . . . C5 C -0.556(3) 0.1043(12) -0.0615(6) 0.036(3) Uani 1 1 d . . . H5A H -0.7141 0.1601 -0.0455 0.043 Uiso 1 1 d R . . H5B H -0.6294 0.0399 -0.0900 0.043 Uiso 1 1 d R . . C6 C -0.421(2) -0.0042(13) -0.0220(4) 0.021(3) Uani 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 Cd1 0.0389(4) 0.0196(4) 0.0102(3) 0.0032(4) 0.0000(4) 0.0039(4) S1 0.0379(18) 0.0387(18) 0.0187(15) -0.0068(13) -0.0082(13) 0.0117(14) S2 0.0459(19) 0.0315(16) 0.0181(15) -0.0048(13) -0.0042(13) 0.0115(16) S3 0.0358(15) 0.0300(15) 0.0242(14) 0.0084(12) -0.0065(14) -0.0052(17) O1 0.028(5) 0.028(5) 0.020(4) 0.005(3) -0.011(3) 0.003(4) O2 0.051(6) 0.042(5) 0.018(4) -0.014(4) -0.006(3) 0.002(4) O3 0.048(6) 0.028(4) 0.029(4) 0.004(3) -0.021(5) -0.010(4) O4 0.067(6) 0.006(4) 0.026(4) 0.005(3) -0.011(4) -0.004(5) N1 0.056(7) 0.021(5) 0.011(4) -0.004(4) 0.000(5) 0.016(5) N2 0.051(6) 0.033(6) 0.018(5) -0.004(4) -0.009(6) 0.013(6) C1 0.017(6) 0.021(5) 0.008(5) 0.004(4) -0.003(4) -0.001(5) C2 0.017(4) 0.023(4) 0.026(4) -0.011(3) 0.003(3) 0.008(3) C3 0.026(7) 0.019(6) 0.020(5) 0.002(4) 0.003(4) -0.002(4) C4 0.027(6) 0.024(6) 0.016(5) 0.000(5) 0.001(4) -0.007(6) C5 0.053(7) 0.022(6) 0.033(6) 0.014(6) -0.014(7) -0.026(5) C6 0.028(6) 0.024(6) 0.010(5) 0.001(4) 0.007(5) 0.005(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 Cd1 O3 2.255(8) . ? Cd1 O1 2.275(7) 2_355 ? Cd1 O4 2.288(8) 4_545 ? Cd1 O2 2.316(8) 2_455 ? Cd1 N2 2.468(9) 4 ? Cd1 O4 2.532(8) . ? Cd1 C6 2.736(11) . ? S1 C3 1.746(11) . ? S1 C2 1.798(10) . ? S2 C3 1.703(10) . ? S2 C4 1.721(10) . ? S3 C4 1.745(11) . ? S3 C5 1.810(11) . ? O1 C1 1.244(11) . ? O1 Cd1 2.275(7) 2_354 ? O2 C1 1.230(12) . ? O2 Cd1 2.316(8) 2_454 ? O3 C6 1.254(13) . ? O4 C6 1.263(13) . ? O4 Cd1 2.288(8) 4_445 ? N1 C3 1.337(12) . ? N1 N2 1.357(13) . ? N2 C4 1.328(14) . ? N2 Cd1 2.468(9) 4_455 ? C1 C2 1.567(13) . ? C5 C6 1.498(15) . ? 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 O3 Cd1 O1 153.5(3) . 2_355 ? O3 Cd1 O4 100.8(3) . 4_545 ? O1 Cd1 O4 94.5(3) 2_355 4_545 ? O3 Cd1 O2 111.8(3) . 2_455 ? O1 Cd1 O2 91.4(3) 2_355 2_455 ? O4 Cd1 O2 82.8(3) 4_545 2_455 ? O3 Cd1 N2 88.7(3) . 4 ? O1 Cd1 N2 83.2(3) 2_355 4 ? O4 Cd1 N2 161.4(3) 4_545 4 ? O2 Cd1 N2 78.9(3) 2_455 4 ? O3 Cd1 O4 54.3(3) . . ? O1 Cd1 O4 108.6(3) 2_355 . ? O4 Cd1 O4 79.25(19) 4_545 . ? O2 Cd1 O4 154.0(3) 2_455 . ? N2 Cd1 O4 119.0(3) 4 . ? O3 Cd1 C6 27.0(3) . . ? O1 Cd1 C6 132.8(3) 2_355 . ? O4 Cd1 C6 90.9(3) 4_545 . ? O2 Cd1 C6 135.8(3) 2_455 . ? N2 Cd1 C6 104.2(3) 4 . ? O4 Cd1 C6 27.4(3) . . ? C3 S1 C2 100.1(5) . . ? C3 S2 C4 88.6(5) . . ? C4 S3 C5 97.1(6) . . ? C1 O1 Cd1 102.1(6) . 2_354 ? C1 O2 Cd1 137.8(7) . 2_454 ? C6 O3 Cd1 98.4(7) . . ? C6 O4 Cd1 132.6(7) . 4_445 ? C6 O4 Cd1 85.3(6) . . ? Cd1 O4 Cd1 125.9(3) 4_445 . ? C3 N1 N2 111.2(9) . . ? C4 N2 N1 114.5(8) . . ? C4 N2 Cd1 125.8(7) . 4_455 ? N1 N2 Cd1 117.4(6) . 4_455 ? O2 C1 O1 124.7(9) . . ? O2 C1 C2 117.4(8) . . ? O1 C1 C2 117.8(9) . . ? C1 C2 S1 108.5(7) . . ? N1 C3 S2 113.9(8) . . ? N1 C3 S1 118.0(8) . . ? S2 C3 S1 127.8(6) . . ? N2 C4 S2 111.8(8) . . ? N2 C4 S3 125.1(8) . . ? S2 C4 S3 123.0(7) . . ? C6 C5 S3 112.0(8) . . ? O3 C6 O4 121.8(10) . . ? O3 C6 C5 119.1(10) . . ? O4 C6 C5 118.7(10) . . ? O3 C6 Cd1 54.6(5) . . ? O4 C6 Cd1 67.3(6) . . ? C5 C6 Cd1 169.2(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.528 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.191 # Attachment '1pmp.cif' data_1pmp _database_code_depnum_ccdc_archive 'CCDC 666521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium bct' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Cd N2 O5 S3' _chemical_formula_weight 394.71 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.1436(6) _cell_length_b 10.1864(12) _cell_length_c 20.945(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1097.4(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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 2.570 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3598 _exptl_absorpt_correction_T_max 0.7311 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3878 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1855 _reflns_number_gt 1836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.0194P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 1855 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0399 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Cd1 Cd 0.19701(4) 0.598741(18) 0.037374(12) 0.02285(8) Uani 1 1 d . . . S1 S -0.93371(19) -0.01270(8) -0.26139(5) 0.0361(2) Uani 1 1 d . . . S2 S -0.58061(17) 0.20152(7) -0.20364(4) 0.0293(2) Uani 1 1 d . . . S3 S -0.17825(18) 0.24976(7) -0.09854(4) 0.02973(19) Uani 1 1 d . . . O1W O 0.3638(4) 0.73698(18) -0.04458(11) 0.0251(5) Uani 1 1 d . . . H1WA H 0.4364 0.7010 -0.0767 0.030 Uiso 1 1 d R . . H1WB H 0.2287 0.7638 -0.0635 0.030 Uiso 1 1 d R . . O1 O -0.9017(4) 0.2678(2) -0.39205(12) 0.0297(6) Uani 1 1 d . . . O2 O -0.6049(5) 0.1201(2) -0.36147(12) 0.0334(6) Uani 1 1 d . . . O3 O -0.0206(4) 0.4623(2) -0.02602(12) 0.0296(6) Uani 1 1 d . . . O4 O -0.3906(4) 0.51941(19) 0.02074(11) 0.0282(5) Uani 1 1 d . . . N1 N -0.5999(5) -0.0370(2) -0.16671(14) 0.0300(7) Uani 1 1 d . . . N2 N -0.4297(6) 0.0248(2) -0.12681(13) 0.0272(7) Uani 1 1 d . . . C1 C -0.8185(7) 0.1748(3) -0.35738(15) 0.0230(7) Uani 1 1 d . . . C2 C -1.0138(7) 0.1309(3) -0.30713(17) 0.0304(8) Uani 1 1 d . . . H2A H -1.1786 0.1150 -0.3283 0.037 Uiso 1 1 calc R . . H2B H -1.0400 0.2031 -0.2776 0.037 Uiso 1 1 calc R . . C3 C -0.6993(7) 0.0429(3) -0.20858(15) 0.0246(7) Uani 1 1 d . . . C4 C -0.3975(6) 0.1488(3) -0.13952(16) 0.0235(7) Uani 1 1 d . . . C5 C -0.4087(7) 0.3576(3) -0.06006(17) 0.0292(8) Uani 1 1 d . . . H5A H -0.5083 0.4047 -0.0920 0.035 Uiso 1 1 calc R . . H5B H -0.5284 0.3066 -0.0343 0.035 Uiso 1 1 calc R . . C6 C -0.2624(6) 0.4544(3) -0.01811(16) 0.0229(8) Uani 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 Cd1 0.02249(12) 0.02301(10) 0.02304(14) -0.00295(10) 0.00131(10) -0.00375(9) S1 0.0437(5) 0.0346(4) 0.0299(6) 0.0103(4) -0.0136(4) -0.0157(4) S2 0.0363(5) 0.0226(3) 0.0290(5) 0.0025(4) -0.0082(4) -0.0020(3) S3 0.0249(4) 0.0321(4) 0.0321(5) -0.0098(3) -0.0027(4) 0.0021(4) O1W 0.0193(11) 0.0306(10) 0.0256(14) 0.0002(10) 0.0023(10) 0.0032(8) O1 0.0249(12) 0.0342(11) 0.0299(15) 0.0108(11) 0.0008(11) -0.0001(9) O2 0.0236(13) 0.0437(13) 0.0329(15) 0.0100(11) 0.0029(11) 0.0056(11) O3 0.0197(11) 0.0316(11) 0.0375(17) -0.0084(10) -0.0021(12) -0.0035(9) O4 0.0247(12) 0.0260(10) 0.0339(15) -0.0079(10) 0.0027(10) 0.0014(9) N1 0.0354(16) 0.0279(13) 0.0267(17) 0.0039(13) -0.0048(14) -0.0053(12) N2 0.0300(15) 0.0277(13) 0.0239(18) -0.0016(12) -0.0034(13) -0.0003(12) C1 0.0222(17) 0.0280(15) 0.0188(18) -0.0009(13) -0.0027(15) -0.0049(14) C2 0.0230(17) 0.0410(18) 0.027(2) 0.0142(15) -0.0042(15) -0.0028(14) C3 0.0271(16) 0.0260(13) 0.0208(18) -0.0024(14) 0.0021(16) -0.0029(14) C4 0.0223(17) 0.0264(14) 0.022(2) -0.0055(13) 0.0036(14) 0.0015(13) C5 0.0222(17) 0.0301(15) 0.035(2) -0.0122(14) 0.0004(15) -0.0042(13) C6 0.0249(19) 0.0176(12) 0.026(2) 0.0007(13) -0.0033(14) 0.0008(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 Cd1 O3 2.224(2) . ? Cd1 O1 2.267(2) 2_465 ? Cd1 O4 2.297(2) 1_655 ? Cd1 N2 2.349(3) 4 ? Cd1 O1W 2.380(2) . ? Cd1 O1W 2.400(2) 4_465 ? S1 C3 1.731(3) . ? S1 C2 1.796(3) . ? S2 C4 1.726(3) . ? S2 C3 1.730(3) . ? S3 C4 1.751(3) . ? S3 C5 1.806(3) . ? O1W Cd1 2.400(2) 4_565 ? O1 C1 1.268(4) . ? O1 Cd1 2.267(2) 2_464 ? O2 C1 1.235(4) . ? O3 C6 1.257(4) . ? O4 C6 1.239(4) . ? O4 Cd1 2.297(2) 1_455 ? N1 C3 1.301(4) . ? N1 N2 1.364(4) . ? N2 C4 1.301(4) . ? N2 Cd1 2.349(3) 4_455 ? C1 C2 1.523(4) . ? C5 C6 1.520(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 O3 Cd1 O1 175.88(9) . 2_465 ? O3 Cd1 O4 98.88(8) . 1_655 ? O1 Cd1 O4 83.16(8) 2_465 1_655 ? O3 Cd1 N2 90.09(9) . 4 ? O1 Cd1 N2 85.99(9) 2_465 4 ? O4 Cd1 N2 100.88(9) 1_655 4 ? O3 Cd1 O1W 96.93(8) . . ? O1 Cd1 O1W 87.03(8) 2_465 . ? O4 Cd1 O1W 76.46(7) 1_655 . ? N2 Cd1 O1W 172.79(9) 4 . ? O3 Cd1 O1W 96.54(7) . 4_465 ? O1 Cd1 O1W 82.68(8) 2_465 4_465 ? O4 Cd1 O1W 156.13(7) 1_655 4_465 ? N2 Cd1 O1W 97.20(8) 4 4_465 ? O1W Cd1 O1W 83.70(5) . 4_465 ? C3 S1 C2 103.54(16) . . ? C4 S2 C3 87.06(15) . . ? C4 S3 C5 98.81(15) . . ? Cd1 O1W Cd1 128.65(9) . 4_565 ? C1 O1 Cd1 131.6(2) . 2_464 ? C6 O3 Cd1 117.3(2) . . ? C6 O4 Cd1 141.2(2) . 1_455 ? C3 N1 N2 112.1(2) . . ? C4 N2 N1 113.8(3) . . ? C4 N2 Cd1 130.4(2) . 4_455 ? N1 N2 Cd1 114.80(18) . 4_455 ? O2 C1 O1 126.7(3) . . ? O2 C1 C2 120.1(3) . . ? O1 C1 C2 113.1(3) . . ? C1 C2 S1 117.2(2) . . ? N1 C3 S2 113.9(2) . . ? N1 C3 S1 120.0(2) . . ? S2 C3 S1 126.11(19) . . ? N2 C4 S2 113.1(3) . . ? N2 C4 S3 123.5(3) . . ? S2 C4 S3 123.39(18) . . ? C6 C5 S3 109.1(2) . . ? O4 C6 O3 125.4(3) . . ? O4 C6 C5 117.6(3) . . ? O3 C6 C5 117.1(3) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.256 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.065 # Attachment '2mpp.cif' data_2mpp _database_code_depnum_ccdc_archive 'CCDC 666522' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cadmium bct' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 Cd N2 O4 S3' _chemical_formula_weight 376.69 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 4.7156(18) _cell_length_b 8.312(3) _cell_length_c 25.557(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1001.8(7) _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 block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 2.802 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7866 _exptl_absorpt_correction_T_max 0.8726 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2907 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1633 _reflns_number_gt 1407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _refine_special_details ; Since 2mpp comes from the dehydrated 1pmp and crystal quality of 2mpp is not as good as before, displacement parameters of some atoms become unreasonable while refined anisotropically. Therefore, isor instruction is used to restrain their displacement parameters ; _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^)+(0.0682P)^2^+21.4669P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.16(15) _refine_ls_number_reflns 1633 _refine_ls_number_parameters 135 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.1896 _refine_ls_wR_factor_gt 0.1844 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_restrained_S_all 1.211 _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 Cd1 Cd 0.1866(4) 0.15408(16) -0.06276(5) 0.0155(4) Uani 1 1 d . . . S1 S 0.9509(15) -0.4087(7) 0.2749(2) 0.0267(15) Uani 1 1 d . . . S2 S 0.5309(14) -0.2441(7) 0.19836(19) 0.0262(15) Uani 1 1 d . . . S3 S 0.3085(16) -0.2512(6) 0.08704(19) 0.0250(13) Uani 1 1 d . . . O1 O 1.129(3) -0.3122(13) 0.3742(4) 0.007(3) Uani 1 1 d U . . O2 O 0.761(3) -0.1782(19) 0.4024(5) 0.031(4) Uani 1 1 d . . . O3 O 0.208(4) -0.0471(17) -0.0036(5) 0.028(3) Uani 1 1 d U . . O4 O 0.538(3) 0.1343(17) 0.0122(5) 0.020(3) Uani 1 1 d U . . N1 N 0.850(4) -0.4848(18) 0.1766(5) 0.016(4) Uani 1 1 d U . . N2 N 0.692(5) -0.4452(19) 0.1319(6) 0.025(4) Uani 1 1 d U . . C1 C 0.889(4) -0.261(2) 0.3695(7) 0.012(4) Uani 1 1 d U . . C2 C 0.725(5) -0.287(2) 0.3168(6) 0.013(4) Uiso 1 1 d . . . H2A H 0.6853 -0.1844 0.3003 0.015 Uiso 1 1 calc R . . H2B H 0.5465 -0.3418 0.3231 0.015 Uiso 1 1 calc R . . C3 C 0.772(4) -0.3875(19) 0.2157(6) 0.010(4) Uiso 1 1 d . . . C4 C 0.521(4) -0.322(2) 0.1360(6) 0.012(4) Uani 1 1 d . . . C5 C 0.567(5) -0.106(2) 0.0614(9) 0.017(4) Uani 1 1 d U . . H5A H 0.6436 -0.0424 0.0900 0.021 Uiso 1 1 calc R . . H5B H 0.7222 -0.1625 0.0448 0.021 Uiso 1 1 calc R . . C6 C 0.428(5) 0.001(2) 0.0232(7) 0.015(4) Uani 1 1 d U . . 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 0.0286(8) 0.0103(6) 0.0074(5) 0.0040(6) 0.0003(7) 0.0038(7) S1 0.033(4) 0.032(3) 0.014(3) -0.006(2) -0.007(3) 0.011(3) S2 0.034(4) 0.034(3) 0.011(2) -0.005(2) -0.005(2) 0.010(3) S3 0.022(3) 0.029(3) 0.024(2) 0.007(2) -0.012(3) -0.004(3) O1 0.004(5) 0.006(4) 0.012(4) 0.004(3) -0.004(4) 0.001(4) O2 0.020(12) 0.044(9) 0.029(7) 0.001(7) -0.009(6) -0.001(8) O3 0.027(5) 0.027(5) 0.029(5) 0.004(4) -0.007(4) -0.003(4) O4 0.023(5) 0.013(5) 0.025(4) 0.000(4) -0.005(4) 0.000(4) N1 0.016(6) 0.019(5) 0.014(5) 0.002(4) 0.002(4) 0.002(4) N2 0.025(6) 0.025(5) 0.024(5) -0.005(4) -0.003(4) -0.001(4) C1 0.012(6) 0.013(5) 0.010(5) 0.001(4) 0.000(4) -0.001(4) C4 0.008(12) 0.018(11) 0.009(8) 0.003(7) -0.002(8) -0.005(9) C5 0.018(6) 0.011(5) 0.023(5) -0.001(4) -0.004(5) -0.012(4) C6 0.015(6) 0.014(6) 0.015(5) 0.004(4) 0.003(4) 0.002(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 Cd1 O1 2.254(11) 2_654 ? Cd1 O3 2.256(13) . ? Cd1 O4 2.292(14) 4_455 ? Cd1 O2 2.300(15) 2_554 ? Cd1 N2 2.478(16) 4_445 ? Cd1 O4 2.539(14) . ? S1 C3 1.740(18) . ? S1 C2 1.817(19) . ? S2 C3 1.708(19) . ? S2 C4 1.722(18) . ? S3 C4 1.707(19) . ? S3 C5 1.837(19) . ? O1 C1 1.21(2) . ? O1 Cd1 2.254(11) 2_655 ? O2 C1 1.24(2) . ? O2 Cd1 2.300(15) 2 ? O3 C6 1.31(3) . ? O4 C6 1.25(2) . ? O4 Cd1 2.292(14) 4 ? N1 C3 1.34(2) . ? N1 N2 1.40(2) . ? N2 C4 1.31(3) . ? N2 Cd1 2.478(16) 4_545 ? C1 C2 1.57(2) . ? C5 C6 1.47(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 O1 Cd1 O3 153.3(6) 2_654 . ? O1 Cd1 O4 94.2(4) 2_654 4_455 ? O3 Cd1 O4 101.8(5) . 4_455 ? O1 Cd1 O2 91.6(5) 2_654 2_554 ? O3 Cd1 O2 111.4(6) . 2_554 ? O4 Cd1 O2 82.6(5) 4_455 2_554 ? O1 Cd1 N2 84.0(5) 2_654 4_445 ? O3 Cd1 N2 87.6(5) . 4_445 ? O4 Cd1 N2 160.6(6) 4_455 4_445 ? O2 Cd1 N2 78.1(6) 2_554 4_445 ? O1 Cd1 O4 108.9(4) 2_654 . ? O3 Cd1 O4 54.4(5) . . ? O4 Cd1 O4 79.9(4) 4_455 . ? O2 Cd1 O4 153.8(5) 2_554 . ? N2 Cd1 O4 119.1(6) 4_445 . ? C3 S1 C2 99.9(9) . . ? C3 S2 C4 89.7(9) . . ? C4 S3 C5 95.6(10) . . ? C1 O1 Cd1 103.2(11) . 2_655 ? C1 O2 Cd1 139.0(14) . 2 ? C6 O3 Cd1 99.1(12) . . ? C6 O4 Cd1 132.7(12) . 4 ? C6 O4 Cd1 87.4(12) . . ? Cd1 O4 Cd1 125.1(6) 4 . ? C3 N1 N2 108.7(16) . . ? C4 N2 N1 116.6(15) . . ? C4 N2 Cd1 126.8(14) . 4_545 ? N1 N2 Cd1 115.0(11) . 4_545 ? O1 C1 O2 125.3(18) . . ? O1 C1 C2 119.9(16) . . ? O2 C1 C2 114.6(17) . . ? C1 C2 S1 107.0(14) . . ? N1 C3 S2 114.3(13) . . ? N1 C3 S1 117.1(14) . . ? S2 C3 S1 128.2(10) . . ? N2 C4 S3 125.0(14) . . ? N2 C4 S2 110.5(14) . . ? S3 C4 S2 124.4(12) . . ? C6 C5 S3 109.8(15) . . ? O4 C6 O3 118.9(17) . . ? O4 C6 C5 119.7(19) . . ? O3 C6 C5 121.0(17) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.955 _refine_diff_density_min -3.342 _refine_diff_density_rms 0.312