# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef '1D.CIF' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wu, Xintao' _publ_contact_author_email wxt@fjirsm.ac.cn _publ_section_title ; Two luminescent enantiomorphic 3D metal-organic frameworks with 3D homochiral double helices ; loop_ _publ_author_name 'Qilong Zhu' 'Tianlu Sheng' 'Ruibiao Fu' 'Chunhong Tan' 'Shengmin Hu' ; Xintao Wu ; # Attachment '1L.CIF' data_1L #TrackingRef '1L.CIF' _database_code_depnum_ccdc_archive 'CCDC 784200' #TrackingRef '1L.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 Cd2 Cl N12 Na3 O18' _chemical_formula_weight 1115.92 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' O O 0.0106 0.0060 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P4(3)32 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'y+3/4, -x+3/4, z+1/4' '-y+3/4, x+1/4, z+3/4' 'x+1/4, z+3/4, -y+3/4' '-x+3/4, z+1/4, y+3/4' '-x+1/4, -z+1/4, -y+1/4' 'x+3/4, -z+3/4, y+1/4' 'z+1/4, y+3/4, -x+3/4' 'z+3/4, -y+3/4, x+1/4' '-z+3/4, y+1/4, x+3/4' '-z+1/4, -y+1/4, -x+1/4' _cell_length_a 15.7838(2) _cell_length_b 15.7838(2) _cell_length_c 15.7838(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3932.19(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12385 _cell_measurement_theta_min 3.1613 _cell_measurement_theta_max 27.4758 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2600 _exptl_crystal_size_mid 0.2600 _exptl_crystal_size_min 0.2600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8589 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30390 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0069 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1516 _reflns_number_gt 1514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 _chemical_absolute_configuration unk _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+3.1822P] 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 0.03(4) _refine_ls_number_reflns 1516 _refine_ls_number_parameters 92 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0550 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.205 _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 0.033740(11) 0.033740(11) 0.033740(11) 0.02466(9) Uani 1 3 d S . . N1 N -0.21261(12) 0.16397(11) 0.28643(13) 0.0214(4) Uani 1 1 d . . . C2 C -0.12716(15) 0.04863(15) 0.11759(15) 0.0217(4) Uani 1 1 d . . . C3 C -0.20422(14) 0.02732(15) 0.17302(14) 0.0201(4) Uani 1 1 d . . . H3A H -0.1845 0.0214 0.2316 0.024 Uiso 1 1 calc R . . C1 C -0.27052(13) 0.15896(13) 0.22520(15) 0.0184(4) Uani 1 1 d . . . N2 N -0.26743(13) 0.09328(13) 0.17136(13) 0.0237(4) Uani 1 1 d . . . H2A H -0.3060 0.0903 0.1330 0.028 Uiso 1 1 calc R . . Na1 Na -0.1250 0.22270(8) -0.02730(8) 0.0436(4) Uani 1 2 d S . . Cl1 Cl 0.1250 0.1250 0.1250 0.0923(10) Uani 1 6 d S . . O2 O -0.12266(16) 0.11511(15) 0.07883(14) 0.0456(6) Uani 1 1 d . . . O1 O -0.07037(12) -0.00864(13) 0.11603(14) 0.0354(5) Uani 1 1 d . . . C4 C -0.24439(17) -0.05655(16) 0.14662(19) 0.0285(5) Uani 1 1 d . . . H4A H -0.2923 -0.0682 0.1822 0.043 Uiso 1 1 calc R . . H4B H -0.2036 -0.1013 0.1523 0.043 Uiso 1 1 calc R . . H4C H -0.2626 -0.0530 0.0887 0.043 Uiso 1 1 calc R . . O1W O -0.2421(4) 0.2849(3) 0.0465(3) 0.157(2) 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 0.02466(9) 0.02466(9) 0.02466(9) 0.00049(7) 0.00049(7) 0.00049(7) N1 0.0195(9) 0.0206(8) 0.0241(10) -0.0043(8) -0.0032(8) 0.0024(7) C2 0.0191(11) 0.0250(11) 0.0209(11) -0.0050(9) 0.0022(8) -0.0014(9) C3 0.0190(11) 0.0211(10) 0.0204(10) -0.0043(9) 0.0015(8) 0.0015(9) C1 0.0161(10) 0.0197(10) 0.0192(10) -0.0014(9) 0.0024(8) -0.0001(8) N2 0.0204(10) 0.0269(10) 0.0240(10) -0.0095(8) -0.0039(7) 0.0050(8) Na1 0.0582(11) 0.0363(5) 0.0363(5) 0.0073(8) -0.0007(5) 0.0007(5) Cl1 0.0923(10) 0.0923(10) 0.0923(10) -0.0373(7) -0.0373(7) -0.0373(7) O2 0.0465(13) 0.0430(13) 0.0473(12) 0.0198(10) 0.0182(10) 0.0031(10) O1 0.0218(9) 0.0322(10) 0.0522(13) -0.0012(9) 0.0106(9) 0.0047(7) C4 0.0271(12) 0.0222(12) 0.0363(14) -0.0030(10) 0.0028(10) -0.0028(9) O1W 0.224(5) 0.129(4) 0.117(3) 0.048(3) 0.105(4) 0.098(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 2.1988(19) . ? Cd1 O1 2.1988(19) 9 ? Cd1 O1 2.1988(19) 5 ? Cd1 Cl1 2.4949(3) . ? N1 C1 1.333(3) . ? N1 C1 1.361(3) 8 ? C2 O2 1.217(3) . ? C2 O1 1.273(3) . ? C2 C3 1.535(3) . ? C3 N2 1.442(3) . ? C3 C4 1.526(3) . ? C1 N2 1.341(3) . ? C1 N1 1.361(3) 11_455 ? Na1 O1W 2.395(4) . ? Na1 O1W 2.395(4) 18_454 ? Na1 O2 2.386(2) . ? Na1 O2 2.386(2) 18_454 ? Na1 O1 2.583(2) 16_454 ? Na1 O1 2.583(2) 9 ? Cl1 Cd1 2.4949(3) 14 ? O1 Na1 2.583(2) 5 ? 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 O1 113.19(5) . 9 ? O1 Cd1 O1 113.19(5) . 5 ? O1 Cd1 O1 113.19(5) 9 5 ? O1 Cd1 Cl1 105.43(6) . . ? O1 Cd1 Cl1 105.43(6) 9 . ? O1 Cd1 Cl1 105.43(6) 5 . ? C1 N1 C1 113.8(2) . 8 ? O2 C2 O1 124.2(2) . . ? O2 C2 C3 121.4(2) . . ? O1 C2 C3 114.4(2) . . ? N2 C3 C4 109.50(19) . . ? N2 C3 C2 112.3(2) . . ? C4 C3 C2 111.33(19) . . ? N2 C1 N1 118.71(19) . . ? N2 C1 N1 115.1(2) . 11_455 ? N1 C1 N1 126.1(2) . 11_455 ? C1 N2 C3 124.9(2) . . ? O1W Na1 O1W 101.3(4) . 18_454 ? O1W Na1 O2 87.82(12) . . ? O1W Na1 O2 92.68(13) 18_454 . ? O1W Na1 O2 92.68(13) . 18_454 ? O1W Na1 O2 87.82(12) 18_454 18_454 ? O2 Na1 O2 179.22(16) . 18_454 ? O1W Na1 O1 82.91(18) . 16_454 ? O1W Na1 O1 160.72(11) 18_454 16_454 ? O2 Na1 O1 106.34(9) . 16_454 ? O2 Na1 O1 73.13(7) 18_454 16_454 ? O1W Na1 O1 160.72(11) . 9 ? O1W Na1 O1 82.91(18) 18_454 9 ? O2 Na1 O1 73.13(7) . 9 ? O2 Na1 O1 106.34(9) 18_454 9 ? O1 Na1 O1 99.35(11) 16_454 9 ? Cd1 Cl1 Cd1 180.000(13) . 14 ? C2 O2 Na1 165.0(2) . . ? C2 O1 Cd1 108.76(17) . . ? C2 O1 Na1 132.65(17) . 5 ? Cd1 O1 Na1 113.88(8) . 5 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.450 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.056 # Attachment '1D.CIF' data_1D #TrackingRef '1D.CIF' _database_code_depnum_ccdc_archive 'CCDC 784201' #TrackingRef '1D.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 Cd2 Cl N12 Na3 O18' _chemical_formula_weight 1115.92 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P4(1)32 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+3/4, x+1/4, -z+1/4' '-y+3/4, -x+3/4, -z+3/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/4' '-x+1/4, z+3/4, y+1/4' '-x+3/4, -z+3/4, -y+3/4' 'x+1/4, -z+1/4, y+3/4' 'z+3/4, y+1/4, -x+1/4' 'z+1/4, -y+1/4, x+3/4' '-z+1/4, y+3/4, x+1/4' '-z+3/4, -y+3/4, -x+3/4' _cell_length_a 15.8103(17) _cell_length_b 15.8103(17) _cell_length_c 15.8103(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3952.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5247 _cell_measurement_theta_min 2.2272 _cell_measurement_theta_max 27.4603 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2200 _exptl_crystal_size_mid 0.2200 _exptl_crystal_size_min 0.2200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 1.266 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8553 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30946 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.43 _reflns_number_total 1518 _reflns_number_gt 1509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 _chemical_absolute_configuration unk _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+2.7315P] 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(4) _refine_ls_number_reflns 1518 _refine_ls_number_parameters 92 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.206 _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 0.533650(12) 0.966350(12) 0.033650(12) 0.02588(11) Uani 1 3 d S . . Na1 Na 0.3750 0.77724(9) -0.02724(9) 0.0438(4) Uani 1 2 d S . . N2 N 0.28735(13) 0.83608(12) 0.28633(15) 0.0225(4) Uani 1 1 d . . . Cl1 Cl 0.6250 0.8750 0.1250 0.0921(11) Uani 1 6 d S . . C1 C 0.37261(17) 0.95145(16) 0.11752(16) 0.0227(5) Uani 1 1 d . . . C4 C 0.22933(15) 0.84112(15) 0.22516(16) 0.0198(5) Uani 1 1 d . . . O2 O 0.37717(17) 0.88486(16) 0.07890(15) 0.0458(6) Uani 1 1 d . . . C2 C 0.29566(15) 0.97265(16) 0.17309(15) 0.0212(5) Uani 1 1 d . . . H2A H 0.3154 0.9786 0.2315 0.025 Uiso 1 1 calc R . . N1 N 0.23249(14) 0.90683(14) 0.17139(15) 0.0251(5) Uani 1 1 d . . . H1A H 0.1940 0.9099 0.1331 0.030 Uiso 1 1 calc R . . C3 C 0.25575(19) 1.05661(18) 0.1465(2) 0.0301(6) Uani 1 1 d . . . H3A H 0.2081 1.0686 0.1821 0.045 Uiso 1 1 calc R . . H3B H 0.2374 1.0529 0.0887 0.045 Uiso 1 1 calc R . . H3C H 0.2967 1.1011 0.1519 0.045 Uiso 1 1 calc R . . O1 O 0.42958(13) 1.00876(14) 0.11604(15) 0.0366(5) Uani 1 1 d . . . O1W O 0.2583(4) 0.7149(3) 0.0465(3) 0.157(3) 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 0.02588(11) 0.02588(11) 0.02588(11) -0.00022(8) 0.00022(8) -0.00022(8) Na1 0.0583(12) 0.0366(6) 0.0366(6) -0.0078(8) -0.0002(6) -0.0002(6) N2 0.0219(10) 0.0206(9) 0.0250(11) 0.0046(8) -0.0027(8) -0.0024(8) Cl1 0.0921(11) 0.0921(11) 0.0921(11) 0.0355(8) -0.0355(8) 0.0355(8) C1 0.0213(12) 0.0250(12) 0.0217(12) 0.0042(10) 0.0021(9) 0.0010(10) C4 0.0178(11) 0.0222(11) 0.0194(12) 0.0016(10) 0.0021(9) -0.0007(9) O2 0.0468(14) 0.0429(14) 0.0476(13) -0.0183(11) 0.0172(11) -0.0033(11) C2 0.0199(12) 0.0230(12) 0.0208(12) 0.0040(9) 0.0014(9) -0.0017(10) N1 0.0212(11) 0.0293(12) 0.0248(11) 0.0095(9) -0.0034(8) -0.0051(9) C3 0.0280(14) 0.0239(14) 0.0384(16) 0.0027(11) 0.0035(11) 0.0029(10) O1 0.0233(10) 0.0337(11) 0.0529(14) 0.0009(10) 0.0115(10) -0.0040(8) O1W 0.221(6) 0.132(4) 0.118(4) -0.048(3) 0.100(4) -0.096(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 2.203(2) 12_664 ? Cd1 O1 2.203(2) . ? Cd1 O1 2.203(2) 6_566 ? Cd1 Cl1 2.5015(4) . ? Na1 O1W 2.395(5) 19 ? Na1 O1W 2.395(5) . ? Na1 O2 2.390(2) 19 ? Na1 O2 2.390(2) . ? Na1 O1 2.586(3) 15_464 ? Na1 O1 2.586(3) 12_664 ? N2 C4 1.335(3) . ? N2 C4 1.363(3) 7_564 ? Cl1 Cd1 2.5015(4) 13_455 ? C1 O2 1.219(3) . ? C1 O1 1.278(3) . ? C1 C2 1.538(3) . ? C4 N1 1.343(3) . ? C4 N2 1.363(3) 10_655 ? C2 N1 1.443(3) . ? C2 C3 1.529(4) . ? O1 Na1 2.586(3) 6_566 ? 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 O1 113.22(5) 12_664 . ? O1 Cd1 O1 113.22(5) 12_664 6_566 ? O1 Cd1 O1 113.22(5) . 6_566 ? O1 Cd1 Cl1 105.40(6) 12_664 . ? O1 Cd1 Cl1 105.40(6) . . ? O1 Cd1 Cl1 105.40(6) 6_566 . ? O1W Na1 O1W 101.1(4) 19 . ? O1W Na1 O2 87.83(13) 19 19 ? O1W Na1 O2 92.67(13) . 19 ? O1W Na1 O2 92.67(13) 19 . ? O1W Na1 O2 87.83(13) . . ? O2 Na1 O2 179.22(17) 19 . ? O1W Na1 O1 160.80(12) 19 15_464 ? O1W Na1 O1 83.05(19) . 15_464 ? O2 Na1 O1 73.19(8) 19 15_464 ? O2 Na1 O1 106.28(9) . 15_464 ? O1W Na1 O1 83.05(19) 19 12_664 ? O1W Na1 O1 160.80(12) . 12_664 ? O2 Na1 O1 106.28(9) 19 12_664 ? O2 Na1 O1 73.19(8) . 12_664 ? O1 Na1 O1 99.24(12) 15_464 12_664 ? C4 N2 C4 113.9(2) . 7_564 ? Cd1 Cl1 Cd1 180.0 13_455 . ? O2 C1 O1 124.2(3) . . ? O2 C1 C2 121.4(2) . . ? O1 C1 C2 114.4(2) . . ? N1 C4 N2 118.6(2) . . ? N1 C4 N2 115.3(2) . 10_655 ? N2 C4 N2 126.0(2) . 10_655 ? C1 O2 Na1 164.9(2) . . ? N1 C2 C3 109.6(2) . . ? N1 C2 C1 112.3(2) . . ? C3 C2 C1 111.0(2) . . ? C4 N1 C2 124.9(2) . . ? C1 O1 Cd1 108.75(18) . . ? C1 O1 Na1 132.68(19) . 6_566 ? Cd1 O1 Na1 113.88(8) . 6_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.426 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.060