# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Tong-Bu Lu' _publ_contact_author_email LUTONGBU@MAIL.SYSU.EDU.CN _publ_section_title ; A highly-connected acentric organic-inorganic hybrid material with unique 3D inorganic and 3D organic connectivity ; loop_ _publ_author_name 'Tong-Bu Lu.' 'Miao Meng.' 'Guo-Yu Yang.' 'Di-Chang Zhong.' 'Jie Zhu.' # Attachment '1.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 761076' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Cd7 N16 O14' _chemical_formula_weight 1337.09 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 Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 9.4631(7) _cell_length_b 9.4631(7) _cell_length_c 13.662(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1223.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2302 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.99 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 6.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'sadabs (sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.2186 _exptl_absorpt_correction_T_max 0.3237 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2307 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.97 _reflns_number_total 1169 _reflns_number_gt 1144 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. Some atoms of the ligand have large ADP max/min Ratio, therefore, these atoms are refined with restrain ADP by EADP and ISOR commands. ; _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^)+(0.0289P)^2^+8.1786P] 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(6) _refine_ls_number_reflns 1169 _refine_ls_number_parameters 71 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.092 _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 0.49697(4) 0.71057(4) 0.74534(4) 0.01034(12) Uani 1 1 d . . . Cd2 Cd 0.5000 1.0000 0.94167(4) 0.01177(14) Uani 1 2 d S . . Cd3 Cd 0.0000 1.0000 1.0000 0.01109(19) Uani 1 4 d S . . O1 O 0.2817(5) 0.8507(4) 0.8860(3) 0.0143(8) Uani 1 1 d . A . O2 O 0.0997(5) 0.7770(4) 0.9803(4) 0.0195(10) Uani 1 1 d . A . O3 O 0.6198(4) 0.8714(4) 0.8329(3) 0.0110(9) Uani 1 1 d . . . H3 H 0.6718 0.8228 0.8709 0.013 Uiso 1 1 d R . . O4 O -0.0072(13) 0.9692(7) 0.8394(5) 0.0143(8) Uani 0.50 1 d PU A -1 H4 H 0.0069 1.0572 0.8314 0.017 Uiso 0.50 1 d PR A -1 N1 N 0.3327(7) 0.5738(6) 0.8345(5) 0.0295(6) Uani 1 1 d . . . N2 N 0.3289(7) 0.4321(6) 0.8315(5) 0.0295(6) Uani 1 1 d . . . N3 N 0.2339(7) 0.3880(6) 0.8935(5) 0.0295(6) Uani 1 1 d . . . N4 N 0.1737(7) 0.4974(6) 0.9384(5) 0.0295(6) Uani 1 1 d . . . C1 C 0.2380(9) 0.6094(7) 0.9004(6) 0.0295(6) Uani 1 1 d . A . C2 C 0.2050(9) 0.7599(7) 0.9246(7) 0.0295(6) 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 0.01191(19) 0.00768(19) 0.0114(2) 0.00024(17) -0.00017(19) -0.00017(13) Cd2 0.0181(4) 0.0085(3) 0.0087(3) 0.000 0.000 0.0014(3) Cd3 0.0120(2) 0.0120(2) 0.0093(4) 0.000 0.000 0.000 O1 0.017(2) 0.0105(19) 0.0157(19) 0.0068(14) -0.0005(16) -0.0027(16) O2 0.022(2) 0.012(2) 0.025(3) 0.0006(18) 0.013(2) 0.0039(17) O3 0.009(2) 0.014(2) 0.010(2) 0.0039(16) -0.0022(16) -0.0014(17) O4 0.017(2) 0.0105(19) 0.0157(19) 0.0068(14) -0.0005(16) -0.0027(16) N1 0.0363(16) 0.0104(12) 0.0418(16) 0.0050(10) 0.0232(14) 0.0028(11) N2 0.0363(16) 0.0104(12) 0.0418(16) 0.0050(10) 0.0232(14) 0.0028(11) N3 0.0363(16) 0.0104(12) 0.0418(16) 0.0050(10) 0.0232(14) 0.0028(11) N4 0.0363(16) 0.0104(12) 0.0418(16) 0.0050(10) 0.0232(14) 0.0028(11) C1 0.0363(16) 0.0104(12) 0.0418(16) 0.0050(10) 0.0232(14) 0.0028(11) C2 0.0363(16) 0.0104(12) 0.0418(16) 0.0050(10) 0.0232(14) 0.0028(11) _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 2.258(4) . ? Cd1 O4 2.261(12) 7_456 ? Cd1 O3 2.265(4) 7_466 ? Cd1 N1 2.362(6) . ? Cd1 O4 2.385(11) 8_656 ? Cd1 O1 2.398(4) 8_656 ? Cd1 N2 2.434(6) 2_665 ? Cd2 O3 2.231(4) . ? Cd2 O3 2.231(4) 2_675 ? Cd2 N4 2.321(6) 4_667 ? Cd2 N4 2.321(6) 3_567 ? Cd2 O1 2.616(4) . ? Cd2 O1 2.616(4) 2_675 ? Cd3 O4 2.215(7) 4_667 ? Cd3 O4 2.215(7) 3_467 ? Cd3 O4 2.215(7) . ? Cd3 O4 2.215(7) 2_575 ? Cd3 O2 2.327(4) 4_667 ? Cd3 O2 2.327(4) 3_467 ? Cd3 O2 2.327(4) . ? Cd3 O2 2.327(4) 2_575 ? O1 C2 1.242(9) . ? O1 Cd1 2.398(4) 7_466 ? O2 C2 1.264(9) . ? O3 Cd1 2.265(4) 8_656 ? O3 H3 0.8500 . ? O4 Cd1 2.261(12) 8_556 ? O4 Cd1 2.385(11) 7_466 ? O4 H4 0.8500 . ? N1 C1 1.314(10) . ? N1 N2 1.342(8) . ? N2 N3 1.303(9) . ? N2 Cd1 2.434(6) 2_665 ? N3 N4 1.332(8) . ? N4 C1 1.328(9) . ? N4 Cd2 2.321(6) 3_467 ? C1 C2 1.495(9) . ? 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 O4 154.8(2) . 7_456 ? O3 Cd1 O3 92.4(2) . 7_466 ? O4 Cd1 O3 107.5(2) 7_456 7_466 ? O3 Cd1 N1 115.8(2) . . ? O4 Cd1 N1 73.8(3) 7_456 . ? O3 Cd1 N1 106.7(2) 7_466 . ? O3 Cd1 O4 140.4(2) . 8_656 ? O4 Cd1 O4 14.5(3) 7_456 8_656 ? O3 Cd1 O4 117.0(2) 7_466 8_656 ? N1 Cd1 O4 82.2(3) . 8_656 ? O3 Cd1 O1 84.14(15) . 8_656 ? O4 Cd1 O1 85.7(3) 7_456 8_656 ? O3 Cd1 O1 76.32(15) 7_466 8_656 ? N1 Cd1 O1 159.3(2) . 8_656 ? O4 Cd1 O1 78.4(2) 8_656 8_656 ? O3 Cd1 N2 76.64(18) . 2_665 ? O4 Cd1 N2 81.6(2) 7_456 2_665 ? O3 Cd1 N2 167.54(18) 7_466 2_665 ? N1 Cd1 N2 83.8(2) . 2_665 ? O4 Cd1 N2 70.4(2) 8_656 2_665 ? O1 Cd1 N2 96.4(2) 8_656 2_665 ? O3 Cd2 O3 96.4(2) . 2_675 ? O3 Cd2 N4 148.37(17) . 4_667 ? O3 Cd2 N4 95.1(2) 2_675 4_667 ? O3 Cd2 N4 95.1(2) . 3_567 ? O3 Cd2 N4 148.37(17) 2_675 3_567 ? N4 Cd2 N4 90.2(4) 4_667 3_567 ? O3 Cd2 O1 85.02(14) . . ? O3 Cd2 O1 72.51(13) 2_675 . ? N4 Cd2 O1 126.57(17) 4_667 . ? N4 Cd2 O1 79.31(18) 3_567 . ? O3 Cd2 O1 72.51(13) . 2_675 ? O3 Cd2 O1 85.02(14) 2_675 2_675 ? N4 Cd2 O1 79.31(18) 4_667 2_675 ? N4 Cd2 O1 126.57(17) 3_567 2_675 ? O1 Cd2 O1 146.21(19) . 2_675 ? O4 Cd3 O4 15.5(3) 4_667 3_467 ? O4 Cd3 O4 169.0(2) 4_667 . ? O4 Cd3 O4 169.0(2) 3_467 . ? O4 Cd3 O4 169.0(2) 4_667 2_575 ? O4 Cd3 O4 169.0(2) 3_467 2_575 ? O4 Cd3 O4 15.5(3) . 2_575 ? O4 Cd3 O2 77.2(3) 4_667 4_667 ? O4 Cd3 O2 89.6(3) 3_467 4_667 ? O4 Cd3 O2 101.3(3) . 4_667 ? O4 Cd3 O2 91.9(3) 2_575 4_667 ? O4 Cd3 O2 89.6(3) 4_667 3_467 ? O4 Cd3 O2 77.2(3) 3_467 3_467 ? O4 Cd3 O2 91.9(3) . 3_467 ? O4 Cd3 O2 101.3(3) 2_575 3_467 ? O2 Cd3 O2 166.7(2) 4_667 3_467 ? O4 Cd3 O2 91.9(3) 4_667 . ? O4 Cd3 O2 101.3(3) 3_467 . ? O4 Cd3 O2 77.2(3) . . ? O4 Cd3 O2 89.6(3) 2_575 . ? O2 Cd3 O2 90.77(3) 4_667 . ? O2 Cd3 O2 90.77(3) 3_467 . ? O4 Cd3 O2 101.3(3) 4_667 2_575 ? O4 Cd3 O2 91.9(3) 3_467 2_575 ? O4 Cd3 O2 89.6(3) . 2_575 ? O4 Cd3 O2 77.2(3) 2_575 2_575 ? O2 Cd3 O2 90.77(3) 4_667 2_575 ? O2 Cd3 O2 90.77(3) 3_467 2_575 ? O2 Cd3 O2 166.7(2) . 2_575 ? C2 O1 Cd1 124.7(5) . 7_466 ? C2 O1 Cd2 135.4(5) . . ? Cd1 O1 Cd2 96.58(14) 7_466 . ? C2 O2 Cd3 120.3(4) . . ? Cd2 O3 Cd1 117.32(18) . . ? Cd2 O3 Cd1 112.84(17) . 8_656 ? Cd1 O3 Cd1 117.95(18) . 8_656 ? Cd2 O3 H3 100.5 . . ? Cd1 O3 H3 104.9 . . ? Cd1 O3 H3 99.3 8_656 . ? Cd3 O4 Cd1 121.2(5) . 8_556 ? Cd3 O4 Cd1 115.9(5) . 7_466 ? Cd1 O4 Cd1 118.1(3) 8_556 7_466 ? Cd3 O4 H4 89.6 . . ? Cd1 O4 H4 87.4 8_556 . ? Cd1 O4 H4 70.8 7_466 . ? C1 N1 N2 105.0(6) . . ? C1 N1 Cd1 131.4(5) . . ? N2 N1 Cd1 123.3(4) . . ? N3 N2 N1 108.5(6) . . ? N3 N2 Cd1 127.1(4) . 2_665 ? N1 N2 Cd1 123.4(4) . 2_665 ? N2 N3 N4 110.2(6) . . ? C1 N4 N3 104.1(6) . . ? C1 N4 Cd2 126.3(5) . 3_467 ? N3 N4 Cd2 129.5(4) . 3_467 ? N1 C1 N4 112.0(6) . . ? N1 C1 C2 122.6(7) . . ? N4 C1 C2 125.3(7) . . ? O1 C2 O2 128.9(6) . . ? O1 C2 C1 116.3(6) . . ? O2 C2 C1 114.8(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.821 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.187