# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef 'CCDC No.cif' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Zhan Shi' _publ_contact_author_email zshi@mail.jlu.edu.cn _publ_section_title ; Synthesis, structures and luminescent properties of cadmium(II) coordination polymers based on 3-pyrid-4-ylbenzoic acid, 4-pyrid-4-ylbenzoic acid ligands ; loop_ _publ_author_name 'Xiaojing Zhou.' 'Baiyan Li.' 'Guanghua Li.' 'Qi Zhou.' 'Zhan Shi.' 'Shouhua Feng.' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 866538' #TrackingRef 'CCDC No.cif' # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 -0.004 -0.003 2649 390 ' ' _platon_squeeze_details ; Approximately 49% of the unit cell volume comprises a large region of disordered solvent which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region. SQUEEZE estimated a total count of 390 electrons per unit cell, and thereby produced a set of solvent-free diffraction intensities. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C72 H48 Cd3 K N6 O15' _chemical_formula_sum 'C72 H48 Cd3 K N6 O15' _chemical_formula_weight 1613.46 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' K K 0.2009 0.2494 '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 trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 18.007(3) _cell_length_b 18.007(3) _cell_length_c 19.288(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5415.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3192 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 24.99 _exptl_crystal_description octahedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 0.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1610 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 0.8143 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 42143 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3192 _reflns_number_gt 2737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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^)+(0.0753P)^2^+9.2731P] 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 3192 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1620 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.207233(19) 0.792767(19) 0.7500 0.0527(2) Uani 1 2 d S . . K1 K 0.3333 0.6667 0.7500 0.0369(5) Uani 1 6 d S . . O1 O 0.1332(2) 0.7172(3) 0.65283(17) 0.0654(10) Uani 1 1 d . . . O2 O 0.2271(2) 0.6798(3) 0.68219(17) 0.0650(10) Uani 1 1 d . . . O3 O 0.1285(3) 0.8715(3) 0.7500 0.146(4) Uani 1 2 d S . . N1 N -0.1016(3) 0.5921(3) 0.32220(19) 0.0541(11) Uani 1 1 d . . . C1 C 0.1594(3) 0.6342(3) 0.5720(2) 0.0461(11) Uani 1 1 d . . . C2 C 0.1014(3) 0.6353(3) 0.5254(2) 0.0459(11) Uani 1 1 d . . . H2 H 0.0711 0.6627 0.5377 0.080 Uiso 1 1 calc . . . C3 C 0.0876(3) 0.5965(3) 0.4608(2) 0.0503(12) Uani 1 1 d . . . C4 C 0.1339(5) 0.5567(5) 0.4442(3) 0.0788(19) Uani 1 1 d . . . H4 H 0.1261 0.5305 0.4012 0.080 Uiso 1 1 calc . . . C5 C 0.1914(5) 0.5553(5) 0.4906(3) 0.082(2) Uani 1 1 d . . . H5 H 0.2226 0.5288 0.4784 0.080 Uiso 1 1 calc . . . C6 C 0.2029(4) 0.5926(4) 0.5548(3) 0.0634(15) Uani 1 1 d . . . H6 H 0.2403 0.5897 0.5865 0.080 Uiso 1 1 calc . . . C7 C 0.1744(3) 0.6798(3) 0.6408(2) 0.0510(12) Uani 1 1 d . . . C8 C -0.0527(4) 0.5606(5) 0.3061(3) 0.0779(19) Uani 1 1 d . . . H8 H -0.0598 0.5365 0.2622 0.080 Uiso 1 1 calc . . . C9 C 0.0081(4) 0.5598(5) 0.3480(3) 0.0777(19) Uani 1 1 d . . . H9 H 0.0393 0.5345 0.3326 0.080 Uiso 1 1 calc . . . C10 C 0.0232(3) 0.5961(3) 0.4125(2) 0.0508(12) Uani 1 1 d . . . C11 C -0.0293(5) 0.6270(6) 0.4299(3) 0.102(3) Uani 1 1 d . . . H11 H -0.0241 0.6508 0.4737 0.080 Uiso 1 1 calc . . . C12 C -0.0898(5) 0.6243(6) 0.3851(3) 0.097(3) Uani 1 1 d . . . H12 H -0.1241 0.6462 0.3999 0.080 Uiso 1 1 calc . . . 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 0.0554(3) 0.0554(3) 0.0312(3) 0.00292(16) 0.00292(16) 0.0156(3) K1 0.0426(8) 0.0426(8) 0.0254(10) 0.000 0.000 0.0213(4) O1 0.062(2) 0.088(3) 0.0411(19) -0.0133(17) -0.0038(16) 0.034(2) O2 0.065(2) 0.084(3) 0.0373(18) -0.0056(17) -0.0137(16) 0.031(2) O3 0.120(5) 0.120(5) 0.190(11) 0.039(5) 0.039(5) 0.054(6) N1 0.054(3) 0.075(3) 0.038(2) -0.0084(19) -0.0115(18) 0.036(2) C1 0.043(3) 0.050(3) 0.034(2) -0.0008(19) -0.0042(18) 0.015(2) C2 0.043(3) 0.052(3) 0.038(2) -0.002(2) -0.0047(19) 0.020(2) C3 0.048(3) 0.062(3) 0.039(2) -0.006(2) -0.011(2) 0.027(3) C4 0.095(5) 0.116(5) 0.051(3) -0.037(3) -0.031(3) 0.073(4) C5 0.098(5) 0.120(6) 0.067(4) -0.037(4) -0.032(3) 0.084(5) C6 0.065(4) 0.081(4) 0.047(3) -0.010(3) -0.018(2) 0.039(3) C7 0.039(3) 0.062(3) 0.032(2) 0.004(2) -0.002(2) 0.010(2) C8 0.094(5) 0.126(6) 0.039(3) -0.029(3) -0.023(3) 0.074(5) C9 0.089(4) 0.127(6) 0.047(3) -0.033(3) -0.028(3) 0.076(4) C10 0.049(3) 0.062(3) 0.040(2) -0.009(2) -0.012(2) 0.027(3) C11 0.125(6) 0.165(7) 0.065(4) -0.063(4) -0.050(4) 0.109(6) C12 0.114(6) 0.169(8) 0.060(4) -0.055(4) -0.044(4) 0.108(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 Cd1 O1 2.308(3) . ? Cd1 O1 2.308(3) 4_666 ? Cd1 N1 2.313(4) 9_666 ? Cd1 N1 2.313(4) 12_556 ? Cd1 O3 2.454(10) . ? Cd1 O2 2.590(4) . ? Cd1 O2 2.590(4) 4_666 ? Cd1 K1 3.9328(8) . ? K1 O2 2.424(4) . ? K1 O2 2.424(4) 4_666 ? K1 O2 2.424(4) 3_565 ? K1 O2 2.424(4) 6_566 ? K1 O2 2.424(4) 2_665 ? K1 O2 2.424(4) 5_556 ? K1 Cd1 3.9328(8) 3_565 ? K1 Cd1 3.9328(8) 2_665 ? O1 C7 1.249(7) . ? O2 C7 1.240(6) . ? N1 C8 1.301(7) . ? N1 C12 1.315(7) . ? N1 Cd1 2.313(4) 8_456 ? C1 C6 1.368(8) . ? C1 C2 1.384(6) . ? C1 C7 1.512(6) . ? C2 C3 1.391(6) . ? C2 H2 0.9300 . ? C3 C4 1.381(8) . ? C3 C10 1.484(6) . ? C4 C5 1.379(8) . ? C4 H4 0.9300 . ? C5 C6 1.374(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.368(8) . ? C8 H8 0.9300 . ? C9 C10 1.369(7) . ? C9 H9 0.9300 . ? C10 C11 1.357(8) . ? C11 C12 1.372(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? 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 178.8(2) . 4_666 ? O1 Cd1 N1 88.66(14) . 9_666 ? O1 Cd1 N1 91.39(14) 4_666 9_666 ? O1 Cd1 N1 91.39(14) . 12_556 ? O1 Cd1 N1 88.66(14) 4_666 12_556 ? N1 Cd1 N1 174.9(2) 9_666 12_556 ? O1 Cd1 O3 90.59(11) . . ? O1 Cd1 O3 90.59(11) 4_666 . ? N1 Cd1 O3 87.45(11) 9_666 . ? N1 Cd1 O3 87.45(11) 12_556 . ? O1 Cd1 O2 52.60(13) . . ? O1 Cd1 O2 126.21(14) 4_666 . ? N1 Cd1 O2 89.40(14) 9_666 . ? N1 Cd1 O2 94.68(14) 12_556 . ? O3 Cd1 O2 143.14(8) . . ? O1 Cd1 O2 126.21(14) . 4_666 ? O1 Cd1 O2 52.60(13) 4_666 4_666 ? N1 Cd1 O2 94.68(14) 9_666 4_666 ? N1 Cd1 O2 89.40(14) 12_556 4_666 ? O3 Cd1 O2 143.14(8) . 4_666 ? O2 Cd1 O2 73.73(15) . 4_666 ? O1 Cd1 K1 89.41(11) . . ? O1 Cd1 K1 89.41(11) 4_666 . ? N1 Cd1 K1 92.55(11) 9_666 . ? N1 Cd1 K1 92.55(11) 12_556 . ? O3 Cd1 K1 180.000(13) . . ? O2 Cd1 K1 36.86(8) . . ? O2 Cd1 K1 36.86(8) 4_666 . ? O2 K1 O2 79.72(18) . 4_666 ? O2 K1 O2 93.63(12) . 3_565 ? O2 K1 O2 93.78(19) 4_666 3_565 ? O2 K1 O2 93.78(19) . 6_566 ? O2 K1 O2 93.63(12) 4_666 6_566 ? O2 K1 O2 170.34(19) 3_565 6_566 ? O2 K1 O2 93.63(12) . 2_665 ? O2 K1 O2 170.3(2) 4_666 2_665 ? O2 K1 O2 93.63(12) 3_565 2_665 ? O2 K1 O2 79.72(19) 6_566 2_665 ? O2 K1 O2 170.34(19) . 5_556 ? O2 K1 O2 93.63(12) 4_666 5_556 ? O2 K1 O2 79.72(19) 3_565 5_556 ? O2 K1 O2 93.63(12) 6_566 5_556 ? O2 K1 O2 93.78(19) 2_665 5_556 ? O2 K1 Cd1 39.86(9) . . ? O2 K1 Cd1 39.86(9) 4_666 . ? O2 K1 Cd1 94.83(10) 3_565 . ? O2 K1 Cd1 94.83(10) 6_566 . ? O2 K1 Cd1 133.11(9) 2_665 . ? O2 K1 Cd1 133.11(9) 5_556 . ? O2 K1 Cd1 133.11(9) . 3_565 ? O2 K1 Cd1 94.83(10) 4_666 3_565 ? O2 K1 Cd1 39.86(9) 3_565 3_565 ? O2 K1 Cd1 133.11(9) 6_566 3_565 ? O2 K1 Cd1 94.83(10) 2_665 3_565 ? O2 K1 Cd1 39.86(9) 5_556 3_565 ? Cd1 K1 Cd1 120.0 . 3_565 ? O2 K1 Cd1 94.83(10) . 2_665 ? O2 K1 Cd1 133.11(9) 4_666 2_665 ? O2 K1 Cd1 133.11(9) 3_565 2_665 ? O2 K1 Cd1 39.86(9) 6_566 2_665 ? O2 K1 Cd1 39.86(9) 2_665 2_665 ? O2 K1 Cd1 94.83(10) 5_556 2_665 ? Cd1 K1 Cd1 120.0 . 2_665 ? Cd1 K1 Cd1 120.0 3_565 2_665 ? C7 O1 Cd1 98.3(3) . . ? C7 O2 K1 171.2(4) . . ? C7 O2 Cd1 85.4(3) . . ? K1 O2 Cd1 103.28(12) . . ? C8 N1 C12 114.7(5) . . ? C8 N1 Cd1 123.5(3) . 8_456 ? C12 N1 Cd1 121.7(4) . 8_456 ? C6 C1 C2 119.6(4) . . ? C6 C1 C7 120.9(4) . . ? C2 C1 C7 119.5(5) . . ? C1 C2 C3 121.4(5) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 117.8(4) . . ? C4 C3 C10 121.7(4) . . ? C2 C3 C10 120.5(5) . . ? C5 C4 C3 120.9(5) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C1 C6 C5 119.9(5) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? O2 C7 O1 122.8(5) . . ? O2 C7 C1 119.6(5) . . ? O1 C7 C1 117.6(4) . . ? N1 C8 C9 125.7(5) . . ? N1 C8 H8 117.2 . . ? C9 C8 H8 117.2 . . ? C8 C9 C10 120.0(5) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 114.1(5) . . ? C11 C10 C3 123.1(4) . . ? C9 C10 C3 122.7(5) . . ? C10 C11 C12 122.2(5) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? N1 C12 C11 123.2(6) . . ? N1 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.755 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.087 #=========================END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 866539' #TrackingRef 'CCDC No.cif' # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.015 0.004 0.005 2063.9 167.1 _platon_squeeze_details ; Approximately 54.6% of the unit cell volume comprises a large region of disordered solvent which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region. SQUEEZE estimated a total count of 390 electrons per unit cell, and thereby produced a set of solvent-free diffraction intensities. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C96 H64 Cd4 N8 O16' _chemical_formula_sum 'C96 H64 Cd4 N8 O16' _chemical_formula_weight 2035.15 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' 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' _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 14.498(3) _cell_length_b 14.899(3) _cell_length_c 17.473(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3774.3(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4245 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.46 _exptl_crystal_description octahedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 0.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 0.8143 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 33965 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4245 _reflns_number_gt 3021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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^)+(0.0816P)^2^+0.7604P] 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 0.0257(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4245 _refine_ls_number_parameters 142 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.159 _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 Cd1 Cd 0.7500 0.5000 0.846332(14) 0.04309(18) Uani 1 2 d S . . O1 O 0.39023(18) 0.0417(2) 0.40329(16) 0.0850(8) Uani 1 1 d . . . O2 O 0.2718(2) 0.1275(2) 0.42277(19) 0.0844(9) Uani 1 1 d . . . N1 N 0.66749(17) 0.42067(16) 0.75636(13) 0.0536(6) Uani 1 1 d . . . C1 C 0.7082(3) 0.3666(3) 0.7055(2) 0.0741(10) Uani 1 1 d . . . H1 H 0.7723 0.3638 0.7051 0.080 Uiso 1 1 calc . . . C2 C 0.6606(3) 0.3150(3) 0.65399(19) 0.0731(10) Uani 1 1 d . . . H2 H 0.6930 0.2793 0.6196 0.080 Uiso 1 1 calc . . . C3 C 0.5656(2) 0.3150(2) 0.65217(15) 0.0535(7) Uani 1 1 d . . . C4 C 0.5237(2) 0.3710(3) 0.7063(2) 0.0790(11) Uani 1 1 d . . . H4 H 0.4597 0.3749 0.7084 0.080 Uiso 1 1 calc . . . C5 C 0.5763(2) 0.4202(2) 0.7562(2) 0.0677(9) Uani 1 1 d . . . H5 H 0.5460 0.4553 0.7923 0.080 Uiso 1 1 calc . . . C6 C 0.5114(2) 0.2626(2) 0.59649(16) 0.0553(7) Uani 1 1 d . . . C7 C 0.5482(2) 0.1877(2) 0.5617(2) 0.0652(8) Uani 1 1 d . . . H7 H 0.6080 0.1700 0.5735 0.080 Uiso 1 1 calc . . . C8 C 0.4970(2) 0.1379(3) 0.50904(19) 0.0637(9) Uani 1 1 d . . . H8 H 0.5232 0.0875 0.4864 0.080 Uiso 1 1 calc . . . C9 C 0.4087(2) 0.1623(2) 0.49032(17) 0.0535(7) Uani 1 1 d . . . C10 C 0.3712(3) 0.2363(3) 0.5254(2) 0.0784(10) Uani 1 1 d U . . H10 H 0.3112 0.2533 0.5136 0.080 Uiso 1 1 calc . . . C11 C 0.4212(3) 0.2860(3) 0.5782(2) 0.0800(10) Uani 1 1 d U . . H11 H 0.3941 0.3355 0.6017 0.080 Uiso 1 1 calc . . . C12 C 0.3539(2) 0.1075(2) 0.43480(16) 0.0544(7) 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 0.0427(2) 0.0474(2) 0.0392(2) 0.000 0.000 -0.00220(11) O1 0.0691(17) 0.0877(18) 0.0981(19) -0.0482(16) -0.0226(14) 0.0167(14) O2 0.0683(15) 0.0837(19) 0.101(2) -0.0381(16) -0.0336(15) 0.0170(14) N1 0.0545(15) 0.0585(14) 0.0480(12) -0.0058(11) -0.0050(11) -0.0020(11) C1 0.048(2) 0.097(3) 0.077(2) -0.025(2) -0.0010(17) -0.0016(19) C2 0.058(2) 0.088(3) 0.073(2) -0.0375(19) -0.0023(15) -0.0012(19) C3 0.0551(19) 0.0547(17) 0.0507(16) -0.0097(13) -0.0100(12) 0.0059(14) C4 0.052(2) 0.100(3) 0.085(2) -0.041(2) -0.0085(17) 0.0084(18) C5 0.057(2) 0.080(2) 0.0653(19) -0.0298(18) -0.0053(15) 0.0074(16) C6 0.0545(17) 0.0568(17) 0.0544(16) -0.0120(14) -0.0092(13) 0.0061(14) C7 0.0560(19) 0.0681(19) 0.072(2) -0.0174(17) -0.0131(16) 0.0124(16) C8 0.052(2) 0.063(2) 0.076(2) -0.0235(16) -0.0107(16) 0.0110(13) C9 0.0542(18) 0.0520(15) 0.0541(15) -0.0098(14) -0.0123(13) 0.0085(13) C10 0.0757(13) 0.0787(13) 0.0809(13) -0.0072(9) -0.0087(9) 0.0053(9) C11 0.0789(13) 0.0788(13) 0.0823(13) -0.0128(9) -0.0064(9) 0.0059(9) C12 0.0542(18) 0.0592(17) 0.0499(15) -0.0044(14) -0.0100(13) 0.0026(14) _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 N1 2.302(2) . ? Cd1 N1 2.302(2) 2_665 ? Cd1 O2 2.344(3) 8_666 ? Cd1 O2 2.344(3) 7_666 ? Cd1 O1 2.347(2) 8_666 ? Cd1 O1 2.347(2) 7_666 ? Cd1 C12 2.687(3) 8_666 ? Cd1 C12 2.687(3) 7_666 ? O1 C12 1.242(4) . ? O1 Cd1 2.347(2) 7_565 ? O2 C12 1.245(4) . ? O2 Cd1 2.344(3) 7_565 ? N1 C5 1.321(4) . ? N1 C1 1.337(4) . ? C1 C2 1.371(5) . ? C1 H1 0.9300 . ? C2 C3 1.378(5) . ? C2 H2 0.9300 . ? C3 C4 1.400(4) . ? C3 C6 1.474(4) . ? C4 C5 1.371(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.379(4) . ? C6 C11 1.391(5) . ? C7 C8 1.395(4) . ? C7 H7 0.9300 . ? C8 C9 1.370(4) . ? C8 H8 0.9300 . ? C9 C10 1.373(5) . ? C9 C12 1.497(4) . ? C10 C11 1.388(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 Cd1 2.687(3) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 93.86(12) . 2_665 ? N1 Cd1 O2 137.34(10) . 8_666 ? N1 Cd1 O2 92.46(10) 2_665 8_666 ? N1 Cd1 O2 92.46(10) . 7_666 ? N1 Cd1 O2 137.34(10) 2_665 7_666 ? O2 Cd1 O2 110.52(18) 8_666 7_666 ? N1 Cd1 O1 88.58(9) . 8_666 ? N1 Cd1 O1 127.15(10) 2_665 8_666 ? O2 Cd1 O1 55.07(9) 8_666 8_666 ? O2 Cd1 O1 95.12(12) 7_666 8_666 ? N1 Cd1 O1 127.15(10) . 7_666 ? N1 Cd1 O1 88.58(9) 2_665 7_666 ? O2 Cd1 O1 95.12(12) 8_666 7_666 ? O2 Cd1 O1 55.07(9) 7_666 7_666 ? O1 Cd1 O1 129.83(15) 8_666 7_666 ? N1 Cd1 C12 114.05(10) . 8_666 ? N1 Cd1 C12 112.21(9) 2_665 8_666 ? O2 Cd1 C12 27.59(9) 8_666 8_666 ? O2 Cd1 C12 103.34(11) 7_666 8_666 ? O1 Cd1 C12 27.52(9) 8_666 8_666 ? O1 Cd1 C12 113.52(11) 7_666 8_666 ? N1 Cd1 C12 112.21(9) . 7_666 ? N1 Cd1 C12 114.05(10) 2_665 7_666 ? O2 Cd1 C12 103.34(11) 8_666 7_666 ? O2 Cd1 C12 27.59(9) 7_666 7_666 ? O1 Cd1 C12 113.52(11) 8_666 7_666 ? O1 Cd1 C12 27.52(9) 7_666 7_666 ? C12 Cd1 C12 109.77(13) 8_666 7_666 ? C12 O1 Cd1 91.67(19) . 7_565 ? C12 O2 Cd1 91.8(2) . 7_565 ? C5 N1 C1 115.9(3) . . ? C5 N1 Cd1 121.6(2) . . ? C1 N1 Cd1 122.3(2) . . ? N1 C1 C2 123.5(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 121.2(3) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C2 C3 C4 114.7(3) . . ? C2 C3 C6 123.2(3) . . ? C4 C3 C6 122.0(3) . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? N1 C5 C4 124.1(3) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? C7 C6 C11 117.7(3) . . ? C7 C6 C3 120.9(3) . . ? C11 C6 C3 121.3(3) . . ? C6 C7 C8 121.1(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 118.5(3) . . ? C8 C9 C12 120.4(3) . . ? C10 C9 C12 121.1(3) . . ? C9 C10 C11 121.2(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 120.7(3) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? O1 C12 O2 121.3(3) . . ? O1 C12 C9 119.5(3) . . ? O2 C12 C9 119.1(3) . . ? O1 C12 Cd1 60.81(17) . 7_565 ? O2 C12 Cd1 60.66(17) . 7_565 ? C9 C12 Cd1 174.7(2) . 7_565 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.655 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.082 #=========================END