# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Mohamed Eddaoudi' 'Victor Ch Krastov' 'Randy Larsena' 'Yunling Liu' _publ_contact_author_name 'Mohamed Eddaoudi' _publ_contact_author_address ; Department of Chemistry University of South Florida 4202 E. Fowler Ave, SCA400 Tampa Florida 33620-5250 UNITED STATES OF AMERICA ; _publ_contact_author_email EDDAOUDI@CAS.USF.EDU _publ_section_title ; Molecular building blocks approach to the assembly of zeolite-like metal-organic frameworks (ZMOFs) with extra-large cavities ; # Attachment 'rho-ZMOF.cif' data_me044a1 _database_code_depnum_ccdc_archive 'CCDC 294663' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H9.58 In N4 O9.58' _chemical_formula_weight 453.95 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Im-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, -y+1/2' '-x+1/2, z+1/2, y+1/2' '-x+1/2, -z+1/2, -y+1/2' 'x+1/2, -z+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, y+1/2, x+1/2' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y+1/2' 'z+1/2, x+1/2, -y+1/2' 'z+1/2, -x+1/2, y+1/2' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z+1/2, x+1/2' '-y+1/2, z+1/2, x+1/2' 'y+1/2, z+1/2, -x+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+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, -y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 31.0622(7) _cell_length_b 31.0622(7) _cell_length_c 31.0622(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 29970.7(12) _cell_formula_units_Z 48 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6209 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 22.93 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10716 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58689 _diffrn_reflns_av_R_equivalents 0.1503 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.06 _reflns_number_total 2043 _reflns_number_gt 878 _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. ; _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^)+(0.0751P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2043 _refine_ls_number_parameters 160 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.027 _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 In1 In 0.10442(2) 0.39558(2) 0.2500 0.1087(4) Uani 1 2 d S . . O1 O 0.08179(19) 0.3265(2) 0.2148(2) 0.130(3) Uani 1 1 d D . . O2 O 0.09952(19) 0.2862(2) 0.1573(2) 0.150(2) Uani 1 1 d D . . H1O2 H 0.1235 0.2842 0.1235 0.225 Uiso 1 2 d SRD . . N1 N 0.1540(2) 0.3798(2) 0.2052(2) 0.117(3) Uani 1 1 d D . . C1 C 0.1050(3) 0.3182(3) 0.1861(3) 0.138(4) Uani 1 1 d D . . C2 C 0.1450(3) 0.3461(3) 0.1784(3) 0.142(4) Uani 1 1 d D . . C3 C 0.1888(3) 0.3965(4) 0.1888(3) 0.133(5) Uani 1 2 d SD . . H3 H 0.2022 0.4206 0.2022 0.159 Uiso 1 2 calc SR . . O3 O 0.0924(2) 0.43085(19) 0.32322(18) 0.110(2) Uani 1 1 d D . . O4 O 0.0400(2) 0.4479(2) 0.36933(18) 0.124(2) Uani 1 1 d D . . H1O4 H 0.0000 0.4437 0.3736 0.187 Uiso 1 2 d SR . . N2 N 0.0364(2) 0.3946(2) 0.2660(2) 0.097(2) Uani 1 1 d D . . C4 C 0.0552(3) 0.4314(3) 0.3335(3) 0.100(3) Uani 1 1 d D . . C5 C 0.0214(2) 0.4139(2) 0.3031(3) 0.092(3) Uani 1 1 d D . . C6 C 0.0000 0.3843(4) 0.2461(4) 0.100(4) Uani 1 2 d SD . . H6 H 0.0000 0.3702 0.2190 0.120 Uiso 1 2 calc SR . . O1X O 0.0000 0.5000 0.5000 0.30(4) Uiso 0.75 16 d SP . . O2X O 0.1606(6) 0.5000 0.3736(6) 0.256(7) Uiso 0.89 2 d SP . . O3X O 0.0000 0.2934(13) 0.0000 0.38(2) Uiso 1.16 8 d SP . . O4X O 0.2705(11) 0.3254(15) 0.2705(11) 0.36(3) Uiso 0.45 2 d SP . . O5X O 0.0000 0.190(4) 0.190(4) 0.38(9) Uiso 0.18 4 d SP . . O6X O 0.0409(14) 0.2089(9) 0.2089(9) 0.249(17) Uiso 0.38 2 d SP . . O7X O 0.2425(9) 0.3202(11) 0.2425(9) 0.275(15) Uiso 0.52 2 d SP . . O8X O 0.205(3) 0.5000 0.418(2) 0.42(4) Uiso 0.33 2 d SP . . O9X O 0.0000 0.1675(19) 0.2388(17) 0.37(3) Uiso 0.42 2 d SP . . O10X O 0.0704(14) 0.2060(14) 0.2662(14) 0.161(15) Uiso 0.17 1 d P . . O11X O 0.347(2) 0.347(2) 0.347(2) 0.43(7) Uiso 0.34 6 d SP . . O12X O 0.130(2) 0.4326(15) 0.4326(15) 0.29(3) Uiso 0.33 2 d SP . . O13X O 0.1218(16) 0.5000 0.3970(15) 0.209(17) Uiso 0.31 2 d SP . . O14X O 0.1000(19) 0.4485(13) 0.4485(13) 0.20(2) Uiso 0.23 2 d SP . . O15X O 0.0000 0.2381(9) 0.2381(9) 0.398(19) Uiso 0.94 4 d SP . . O16X O -0.0216(19) 0.534(2) 0.5000 0.39(6) Uiso 0.33 2 d SP . . O17X O 0.2123(11) 0.2801(18) 0.2123(11) 0.26(2) Uiso 0.31 2 d SP . . O18X O 0.134(2) 0.458(2) 0.4056(19) 0.35(2) Uiso 0.29 1 d P . . O19X O -0.055(8) 0.5000 0.5000 0.47(12) Uiso 0.31 8 d SP . . 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 In1 0.1014(5) 0.1014(5) 0.1232(8) 0.0069(4) 0.0069(4) -0.0049(6) O1 0.109(5) 0.168(7) 0.115(5) -0.050(5) 0.013(4) -0.011(4) O2 0.138(6) 0.139(6) 0.173(6) -0.017(5) 0.008(5) -0.032(5) N1 0.128(7) 0.087(6) 0.138(7) -0.019(5) -0.030(6) -0.012(5) C1 0.179(12) 0.090(7) 0.145(11) -0.039(7) -0.060(9) -0.022(8) C2 0.107(8) 0.141(9) 0.179(10) 0.032(7) -0.018(7) -0.014(6) C3 0.165(9) 0.068(10) 0.165(9) 0.008(7) -0.013(13) 0.008(7) O3 0.108(5) 0.121(5) 0.103(5) 0.002(4) -0.008(4) -0.010(4) O4 0.141(5) 0.144(5) 0.088(4) -0.015(4) -0.002(4) -0.010(4) N2 0.089(5) 0.106(5) 0.097(5) -0.008(4) -0.007(4) -0.007(4) C4 0.117(8) 0.089(7) 0.093(8) 0.006(6) 0.001(7) -0.004(7) C5 0.105(7) 0.088(6) 0.084(6) -0.010(5) 0.004(5) -0.009(4) C6 0.103(10) 0.103(10) 0.093(9) 0.007(7) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 N1 2.131(7) . ? In1 N1 2.131(7) 38 ? In1 N2 2.171(6) 38 ? In1 N2 2.171(6) . ? In1 O1 2.510(6) . ? In1 O1 2.510(6) 38 ? In1 O3 2.552(6) 38 ? In1 O3 2.552(6) . ? O1 C1 1.174(9) . ? O2 C1 1.348(8) . ? N1 C3 1.305(7) . ? N1 C2 1.367(9) . ? C1 C2 1.533(10) . ? C2 C2 1.466(17) 72 ? C3 N1 1.305(7) 72 ? O3 C4 1.199(8) . ? O4 C4 1.314(8) . ? N2 C6 1.328(7) . ? N2 C5 1.379(8) . ? C4 C5 1.512(9) . ? C5 C5 1.327(14) 52 ? C6 N2 1.328(7) 52 ? O1X O16X 1.26(7) 17_556 ? O1X O16X 1.26(7) 67 ? O1X O16X 1.26(7) 3_556 ? O1X O16X 1.26(7) . ? O1X O16X 1.26(7) 51_565 ? O1X O16X 1.26(7) 65_565 ? O1X O16X 1.26(7) 19_566 ? O1X O16X 1.26(7) 49_566 ? O1X O19X 1.7(2) . ? O1X O19X 1.7(2) 49_566 ? O2X O13X 1.41(5) . ? O4X O7X 1.24(5) . ? O5X O6X 1.52(10) 52 ? O5X O6X 1.52(10) . ? O5X O9X 1.67(8) 18 ? O5X O9X 1.67(8) . ? O6X O15X 1.80(4) . ? O12X O18X 1.16(6) . ? O12X O18X 1.16(6) 67 ? O12X O14X 1.17(8) . ? O13X O18X 1.38(6) 51_565 ? O13X O18X 1.38(6) . ? O14X O18X 1.72(7) . ? O14X O18X 1.72(7) 67 ? O15X O6X 1.80(4) 52 ? O16X O16X 1.34(12) 3_556 ? O16X O19X 1.49(16) . ? O16X O16X 1.51(9) 17_556 ? O16X O16X 1.51(9) 67 ? O19X O16X 1.49(16) 67 ? O19X O16X 1.49(16) 17_556 ? O19X O16X 1.49(16) 51_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 In1 N1 95.4(4) . 38 ? N1 In1 N2 93.7(2) . 38 ? N1 In1 N2 148.1(2) 38 38 ? N1 In1 N2 148.1(2) . . ? N1 In1 N2 93.7(2) 38 . ? N2 In1 N2 94.5(3) 38 . ? N1 In1 O1 73.8(2) . . ? N1 In1 O1 74.4(2) 38 . ? N2 In1 O1 137.4(2) 38 . ? N2 In1 O1 79.4(2) . . ? N1 In1 O1 74.4(2) . 38 ? N1 In1 O1 73.8(2) 38 38 ? N2 In1 O1 79.4(2) 38 38 ? N2 In1 O1 137.4(2) . 38 ? O1 In1 O1 132.0(3) . 38 ? N1 In1 O3 76.2(2) . 38 ? N1 In1 O3 141.8(2) 38 38 ? N2 In1 O3 70.1(2) 38 38 ? N2 In1 O3 77.8(2) . 38 ? O1 In1 O3 67.4(2) . 38 ? O1 In1 O3 135.64(19) 38 38 ? N1 In1 O3 141.8(2) . . ? N1 In1 O3 76.2(2) 38 . ? N2 In1 O3 77.8(2) 38 . ? N2 In1 O3 70.1(2) . . ? O1 In1 O3 135.64(19) . . ? O1 In1 O3 67.4(2) 38 . ? O3 In1 O3 132.0(3) 38 . ? C1 O1 In1 110.2(6) . . ? C3 N1 C2 103.6(9) . . ? C3 N1 In1 139.7(7) . . ? C2 N1 In1 115.3(5) . . ? O1 C1 O2 125.9(9) . . ? O1 C1 C2 119.5(8) . . ? O2 C1 C2 114.5(8) . . ? N1 C2 C2 106.7(5) . 72 ? N1 C2 C1 120.1(8) . . ? C2 C2 C1 133.1(5) 72 . ? N1 C3 N1 119.4(13) . 72 ? C4 O3 In1 112.5(5) . . ? C6 N2 C5 101.9(7) . . ? C6 N2 In1 136.5(6) . . ? C5 N2 In1 121.0(5) . . ? O3 C4 O4 125.2(8) . . ? O3 C4 C5 119.9(8) . . ? O4 C4 C5 114.8(8) . . ? C5 C5 N2 109.8(4) 52 . ? C5 C5 C4 134.0(5) 52 . ? N2 C5 C4 116.2(7) . . ? N2 C6 N2 116.7(10) 52 . ? O16X O1X O16X 116(5) 17_556 67 ? O16X O1X O16X 106(3) 17_556 3_556 ? O16X O1X O16X 106(3) 67 3_556 ? O16X O1X O16X 74(3) 17_556 . ? O16X O1X O16X 74(3) 67 . ? O16X O1X O16X 64(5) 3_556 . ? O16X O1X O16X 74(3) 17_556 51_565 ? O16X O1X O16X 74(3) 67 51_565 ? O16X O1X O16X 180.00(2) 3_556 51_565 ? O16X O1X O16X 116(5) . 51_565 ? O16X O1X O16X 180.00(3) 17_556 65_565 ? O16X O1X O16X 64(5) 67 65_565 ? O16X O1X O16X 74(3) 3_556 65_565 ? O16X O1X O16X 106(3) . 65_565 ? O16X O1X O16X 106(3) 51_565 65_565 ? O16X O1X O16X 64(5) 17_556 19_566 ? O16X O1X O16X 180.00(3) 67 19_566 ? O16X O1X O16X 74(3) 3_556 19_566 ? O16X O1X O16X 106(3) . 19_566 ? O16X O1X O16X 106(3) 51_565 19_566 ? O16X O1X O16X 116(5) 65_565 19_566 ? O16X O1X O16X 106(3) 17_556 49_566 ? O16X O1X O16X 106(3) 67 49_566 ? O16X O1X O16X 116(5) 3_556 49_566 ? O16X O1X O16X 180.00(3) . 49_566 ? O16X O1X O16X 64(5) 51_565 49_566 ? O16X O1X O16X 74(3) 65_565 49_566 ? O16X O1X O16X 74(3) 19_566 49_566 ? O16X O1X O19X 58(3) 17_556 . ? O16X O1X O19X 58(3) 67 . ? O16X O1X O19X 122(3) 3_556 . ? O16X O1X O19X 58(3) . . ? O16X O1X O19X 58(3) 51_565 . ? O16X O1X O19X 122(3) 65_565 . ? O16X O1X O19X 122(3) 19_566 . ? O16X O1X O19X 122(3) 49_566 . ? O16X O1X O19X 122(3) 17_556 49_566 ? O16X O1X O19X 122(3) 67 49_566 ? O16X O1X O19X 58(3) 3_556 49_566 ? O16X O1X O19X 122(3) . 49_566 ? O16X O1X O19X 122(3) 51_565 49_566 ? O16X O1X O19X 58(3) 65_565 49_566 ? O16X O1X O19X 58(3) 19_566 49_566 ? O16X O1X O19X 58(3) 49_566 49_566 ? O19X O1X O19X 180.000(13) . 49_566 ? O6X O5X O6X 114(10) 52 . ? O6X O5X O9X 79(5) 52 18 ? O6X O5X O9X 79(5) . 18 ? O6X O5X O9X 79(5) 52 . ? O6X O5X O9X 79(5) . . ? O9X O5X O9X 140(10) 18 . ? O5X O6X O15X 78(7) . . ? O18X O12X O18X 169(10) . 67 ? O18X O12X O14X 95(6) . . ? O18X O12X O14X 95(6) 67 . ? O18X O13X O18X 142(7) 51_565 . ? O18X O13X O2X 83(4) 51_565 . ? O18X O13X O2X 83(4) . . ? O12X O14X O18X 42(3) . . ? O12X O14X O18X 42(3) . 67 ? O18X O14X O18X 84(6) . 67 ? O6X O15X O6X 90(3) 52 . ? O1X O16X O16X 58(3) . 3_556 ? O1X O16X O19X 77(8) . . ? O16X O16X O19X 134(8) 3_556 . ? O1X O16X O16X 53.2(13) . 17_556 ? O16X O16X O16X 90.000(8) 3_556 17_556 ? O19X O16X O16X 60(4) . 17_556 ? O1X O16X O16X 53.2(13) . 67 ? O16X O16X O16X 90.000(9) 3_556 67 ? O19X O16X O16X 60(4) . 67 ? O16X O16X O16X 90.000(17) 17_556 67 ? O12X O18X O13X 140(9) . . ? O12X O18X O14X 43(5) . . ? O13X O18X O14X 99(5) . . ? O16X O19X O16X 61(9) . 67 ? O16X O19X O16X 61(9) . 17_556 ? O16X O19X O16X 91(10) 67 17_556 ? O16X O19X O16X 91(10) . 51_565 ? O16X O19X O16X 61(9) 67 51_565 ? O16X O19X O16X 61(9) 17_556 51_565 ? O16X O19X O1X 46(8) . . ? O16X O19X O1X 46(8) 67 . ? O16X O19X O1X 46(8) 17_556 . ? O16X O19X O1X 46(8) 51_565 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.405 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.080 # Attachment 'sod-ZMOF.cif' data_me070 _database_code_depnum_ccdc_archive 'CCDC 294664' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H4 In N4 O8' _chemical_formula_weight 422.99 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Fd-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+3/4, z+1/2' '-x+3/4, y+1/2, -z+1/4' 'x+1/2, -y+1/4, -z+3/4' 'z, x, y' 'z+1/2, -x+1/4, -y+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+3/4, x+1/2, -y+1/4' 'y, z, x' '-y+3/4, z+1/2, -x+1/4' 'y+1/2, -z+1/4, -x+3/4' '-y+1/4, -z+3/4, x+1/2' 'y+3/4, x+1/4, -z' '-y+1/2, -x+1/2, -z+1/2' 'y+1/4, -x, z+3/4' '-y, x+3/4, z+1/4' 'x+3/4, z+1/4, -y' '-x, z+3/4, y+1/4' '-x+1/2, -z+1/2, -y+1/2' 'x+1/4, -z, y+3/4' 'z+3/4, y+1/4, -x' 'z+1/4, -y, x+3/4' '-z, y+3/4, x+1/4' '-z+1/2, -y+1/2, -x+1/2' 'x, y+1/2, z+1/2' '-x+1/4, -y+5/4, z+1' '-x+3/4, y+1, -z+3/4' 'x+1/2, -y+3/4, -z+5/4' 'z, x+1/2, y+1/2' 'z+1/2, -x+3/4, -y+5/4' '-z+1/4, -x+5/4, y+1' '-z+3/4, x+1, -y+3/4' 'y, z+1/2, x+1/2' '-y+3/4, z+1, -x+3/4' 'y+1/2, -z+3/4, -x+5/4' '-y+1/4, -z+5/4, x+1' 'y+3/4, x+3/4, -z+1/2' '-y+1/2, -x+1, -z+1' 'y+1/4, -x+1/2, z+5/4' '-y, x+5/4, z+3/4' 'x+3/4, z+3/4, -y+1/2' '-x, z+5/4, y+3/4' '-x+1/2, -z+1, -y+1' 'x+1/4, -z+1/2, y+5/4' 'z+3/4, y+3/4, -x+1/2' 'z+1/4, -y+1/2, x+5/4' '-z, y+5/4, x+3/4' '-z+1/2, -y+1, -x+1' 'x+1/2, y, z+1/2' '-x+3/4, -y+3/4, z+1' '-x+5/4, y+1/2, -z+3/4' 'x+1, -y+1/4, -z+5/4' 'z+1/2, x, y+1/2' 'z+1, -x+1/4, -y+5/4' '-z+3/4, -x+3/4, y+1' '-z+5/4, x+1/2, -y+3/4' 'y+1/2, z, x+1/2' '-y+5/4, z+1/2, -x+3/4' 'y+1, -z+1/4, -x+5/4' '-y+3/4, -z+3/4, x+1' 'y+5/4, x+1/4, -z+1/2' '-y+1, -x+1/2, -z+1' 'y+3/4, -x, z+5/4' '-y+1/2, x+3/4, z+3/4' 'x+5/4, z+1/4, -y+1/2' '-x+1/2, z+3/4, y+3/4' '-x+1, -z+1/2, -y+1' 'x+3/4, -z, y+5/4' 'z+5/4, y+1/4, -x+1/2' 'z+3/4, -y, x+5/4' '-z+1/2, y+3/4, x+3/4' '-z+1, -y+1/2, -x+1' 'x+1/2, y+1/2, z' '-x+3/4, -y+5/4, z+1/2' '-x+5/4, y+1, -z+1/4' 'x+1, -y+3/4, -z+3/4' 'z+1/2, x+1/2, y' 'z+1, -x+3/4, -y+3/4' '-z+3/4, -x+5/4, y+1/2' '-z+5/4, x+1, -y+1/4' 'y+1/2, z+1/2, x' '-y+5/4, z+1, -x+1/4' 'y+1, -z+3/4, -x+3/4' '-y+3/4, -z+5/4, x+1/2' 'y+5/4, x+3/4, -z' '-y+1, -x+1, -z+1/2' 'y+3/4, -x+1/2, z+3/4' '-y+1/2, x+5/4, z+1/4' 'x+5/4, z+3/4, -y' '-x+1/2, z+5/4, y+1/4' '-x+1, -z+1, -y+1/2' 'x+3/4, -z+1/2, y+3/4' 'z+5/4, y+3/4, -x' 'z+3/4, -y+1/2, x+3/4' '-z+1/2, y+5/4, x+1/4' '-z+1, -y+1, -x+1/2' '-x, -y, -z' 'x-1/4, y-3/4, -z-1/2' 'x-3/4, -y-1/2, z-1/4' '-x-1/2, y-1/4, z-3/4' '-z, -x, -y' '-z-1/2, x-1/4, y-3/4' 'z-1/4, x-3/4, -y-1/2' 'z-3/4, -x-1/2, y-1/4' '-y, -z, -x' 'y-3/4, -z-1/2, x-1/4' '-y-1/2, z-1/4, x-3/4' 'y-1/4, z-3/4, -x-1/2' '-y-3/4, -x-1/4, z' 'y-1/2, x-1/2, z-1/2' '-y-1/4, x, -z-3/4' 'y, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y' 'x, -z-3/4, -y-1/4' 'x-1/2, z-1/2, y-1/2' '-x-1/4, z, -y-3/4' '-z-3/4, -y-1/4, x' '-z-1/4, y, -x-3/4' 'z, -y-3/4, -x-1/4' 'z-1/2, y-1/2, x-1/2' '-x, -y+1/2, -z+1/2' 'x-1/4, y-1/4, -z' 'x-3/4, -y, z+1/4' '-x-1/2, y+1/4, z-1/4' '-z, -x+1/2, -y+1/2' '-z-1/2, x+1/4, y-1/4' 'z-1/4, x-1/4, -y' 'z-3/4, -x, y+1/4' '-y, -z+1/2, -x+1/2' 'y-3/4, -z, x+1/4' '-y-1/2, z+1/4, x-1/4' 'y-1/4, z-1/4, -x' '-y-3/4, -x+1/4, z+1/2' 'y-1/2, x, z' '-y-1/4, x+1/2, -z-1/4' 'y, -x-1/4, -z+1/4' '-x-3/4, -z+1/4, y+1/2' 'x, -z-1/4, -y+1/4' 'x-1/2, z, y' '-x-1/4, z+1/2, -y-1/4' '-z-3/4, -y+1/4, x+1/2' '-z-1/4, y+1/2, -x-1/4' 'z, -y-1/4, -x+1/4' 'z-1/2, y, x' '-x+1/2, -y, -z+1/2' 'x+1/4, y-3/4, -z' 'x-1/4, -y-1/2, z+1/4' '-x, y-1/4, z-1/4' '-z+1/2, -x, -y+1/2' '-z, x-1/4, y-1/4' 'z+1/4, x-3/4, -y' 'z-1/4, -x-1/2, y+1/4' '-y+1/2, -z, -x+1/2' 'y-1/4, -z-1/2, x+1/4' '-y, z-1/4, x-1/4' 'y+1/4, z-3/4, -x' '-y-1/4, -x-1/4, z+1/2' 'y, x-1/2, z' '-y+1/4, x, -z-1/4' 'y+1/2, -x-3/4, -z+1/4' '-x-1/4, -z-1/4, y+1/2' 'x+1/2, -z-3/4, -y+1/4' 'x, z-1/2, y' '-x+1/4, z, -y-1/4' '-z-1/4, -y-1/4, x+1/2' '-z+1/4, y, -x-1/4' 'z+1/2, -y-3/4, -x+1/4' 'z, y-1/2, x' '-x+1/2, -y+1/2, -z' 'x+1/4, y-1/4, -z-1/2' 'x-1/4, -y, z-1/4' '-x, y+1/4, z-3/4' '-z+1/2, -x+1/2, -y' '-z, x+1/4, y-3/4' 'z+1/4, x-1/4, -y-1/2' 'z-1/4, -x, y-1/4' '-y+1/2, -z+1/2, -x' 'y-1/4, -z, x-1/4' '-y, z+1/4, x-3/4' 'y+1/4, z-1/4, -x-1/2' '-y-1/4, -x+1/4, z' 'y, x, z-1/2' '-y+1/4, x+1/2, -z-3/4' 'y+1/2, -x-1/4, -z-1/4' '-x-1/4, -z+1/4, y' 'x+1/2, -z-1/4, -y-1/4' 'x, z, y-1/2' '-x+1/4, z+1/2, -y-3/4' '-z-1/4, -y+1/4, x' '-z+1/4, y+1/2, -x-3/4' 'z+1/2, -y-1/4, -x-1/4' 'z, y, x-1/2' _cell_length_a 36.0435(11) _cell_length_b 36.0435(11) _cell_length_c 36.0435(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 46825(2) _cell_formula_units_Z 96 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7187 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.63 _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 19680 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23207 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 22.48 _reflns_number_total 1287 _reflns_number_gt 1174 _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. ; _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^)+(0.1296P)^2^+1277.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1287 _refine_ls_number_parameters 167 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.2389 _refine_ls_wR_factor_gt 0.2334 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 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 In1 In 0.11802(2) 0.88198(2) 0.7500 0.0787(5) Uani 1 2 d S . . O1 O 0.1906(3) 0.8605(3) 0.7801(3) 0.102(3) Uani 1 1 d . . . O2 O 0.2296(3) 0.8837(3) 0.8233(3) 0.121(4) Uani 1 1 d . . . N1 N 0.1406(3) 0.9182(3) 0.7936(3) 0.075(3) Uani 1 1 d . . . C1 C 0.1721(3) 0.9134(4) 0.8145(4) 0.084(4) Uani 1 1 d . . . C2 C 0.1983(3) 0.8827(4) 0.8038(4) 0.092(4) Uani 1 1 d . . . C5 C 0.1227(3) 0.9467(3) 0.8094(3) 0.075(3) Uani 1 1 d . . . H5 H 0.1000 0.9559 0.8013 0.112 Uiso 1 1 calc R . . C3 C 0.1723(3) 0.9396(4) 0.8420(4) 0.083(4) Uani 1 1 d . . . N2 N 0.1415(3) 0.9600(3) 0.8380(3) 0.075(3) Uani 1 1 d . . . C4 C 0.1992(4) 0.9497(5) 0.8728(4) 0.097(4) Uani 1 1 d . . . O3 O 0.1884(2) 0.9736(3) 0.8949(3) 0.087(2) Uani 1 1 d . . . O4 O 0.2285(3) 0.9326(3) 0.8726(3) 0.120(4) Uani 1 1 d . . . O1X O 0.0037(19) 0.801(3) 0.757(3) 0.32(5) Uani 0.19 1 d P . . O2X O 0.0415(10) -0.0011(12) 0.7228(18) 0.148(19) Uani 0.26 1 d PU . . O3X O 0.0000 -0.0166(6) 0.7334(6) 0.20(2) Uani 0.42 2 d SP . . O4X O 0.080(5) 0.0641(16) 0.647(3) 0.33(8) Uani 0.22 1 d P . . O5X O 0.0547(8) 0.0228(17) 0.7317(18) 0.207(19) Uani 0.38 1 d PU . . O6X O 0.0685(15) 0.0254(13) 0.6845(14) 0.27(3) Uani 0.35 1 d P . . O7X O 0.0431(19) 0.040(2) 0.6679(14) 0.17(2) Uani 0.24 1 d P . . O8X O -0.056(2) 0.806(2) 0.806(2) 0.25(5) Uani 0.31 3 d SP . . 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 In1 0.0775(6) 0.0775(6) 0.0811(9) -0.0023(5) -0.0023(5) 0.0189(6) O1 0.103(7) 0.107(7) 0.095(7) 0.014(5) 0.019(5) 0.030(6) O2 0.076(6) 0.139(8) 0.148(9) 0.030(7) -0.014(6) 0.043(6) N1 0.076(6) 0.072(6) 0.078(6) 0.000(5) -0.008(5) 0.013(5) C1 0.057(7) 0.094(9) 0.101(9) 0.023(7) -0.011(6) 0.004(6) C2 0.057(7) 0.116(11) 0.102(10) 0.031(9) 0.017(7) 0.024(7) C5 0.067(6) 0.092(8) 0.064(7) -0.007(6) -0.016(5) 0.013(6) C3 0.059(7) 0.101(9) 0.089(9) 0.011(7) -0.023(6) -0.001(7) N2 0.066(6) 0.080(6) 0.077(6) 0.006(5) -0.013(5) 0.003(5) C4 0.069(8) 0.118(11) 0.105(11) 0.032(9) -0.012(7) 0.017(8) O3 0.068(5) 0.099(6) 0.093(6) 0.010(5) -0.019(4) 0.000(4) O4 0.074(6) 0.156(10) 0.130(8) -0.001(7) -0.038(5) 0.022(6) O1X 0.14(5) 0.43(9) 0.40(10) -0.37(8) -0.06(6) -0.06(6) O2X 0.043(18) 0.14(3) 0.26(5) -0.14(3) -0.01(3) 0.013(19) O3X 0.17(3) 0.22(3) 0.22(3) -0.12(3) -0.16(2) 0.16(2) O4X 0.7(2) 0.06(3) 0.20(7) -0.06(4) 0.01(11) -0.02(7) O5X 0.058(16) 0.19(4) 0.37(5) 0.07(4) -0.12(3) 0.01(2) O6X 0.31(5) 0.23(4) 0.27(4) -0.22(3) -0.23(4) 0.18(4) O7X 0.17(5) 0.22(7) 0.11(4) 0.06(4) -0.05(4) 0.04(5) O8X 0.25(5) 0.25(5) 0.25(5) 0.13(6) -0.13(6) -0.13(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 In1 N2 2.170(10) 150_665 ? In1 N2 2.170(10) 164_557 ? In1 N1 2.202(10) . ? In1 N1 2.202(10) 86_556 ? In1 O3 2.292(8) 164_557 ? In1 O3 2.292(8) 150_665 ? O1 C2 1.201(17) . ? O2 C2 1.329(17) . ? N1 C5 1.338(14) . ? N1 C1 1.371(15) . ? C1 C3 1.368(16) . ? C1 C2 1.507(19) . ? C5 N2 1.326(14) . ? C3 N2 1.338(15) . ? C3 C4 1.519(19) . ? N2 In1 2.170(10) 156_466 ? C4 O4 1.224(17) . ? C4 O3 1.235(17) . ? O3 In1 2.292(8) 156_466 ? O2X O5X 1.04(6) . ? O2X O5X 1.38(8) 83_455 ? O2X O3X 1.64(4) . ? O2X O3X 1.82(6) 32_545 ? O3X O3X 1.47(6) 83_455 ? O3X O3X 1.47(6) 32_545 ? O3X O2X 1.64(4) 42_535 ? O3X O2X 1.82(6) 86_446 ? O3X O2X 1.82(6) 83_455 ? O4X O4X 1.74(11) 32_545 ? O4X O4X 1.74(11) 83_455 ? O4X O7X 1.76(14) . ? O5X O2X 1.38(8) 32_545 ? O5X O7X 1.46(7) 32_545 ? O5X O6X 1.71(8) 32_545 ? O5X O5X 1.75(4) 83_455 ? O5X O5X 1.75(4) 32_545 ? O5X O6X 1.77(8) . ? O6X O7X 1.22(6) . ? O6X O7X 1.22(7) 32_545 ? O6X O5X 1.71(8) 83_455 ? O7X O6X 1.22(7) 83_455 ? O7X O5X 1.46(7) 83_455 ? 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 N2 In1 N2 132.3(5) 150_665 164_557 ? N2 In1 N1 96.4(3) 150_665 . ? N2 In1 N1 91.0(3) 164_557 . ? N2 In1 N1 91.0(3) 150_665 86_556 ? N2 In1 N1 96.4(3) 164_557 86_556 ? N1 In1 N1 161.8(5) . 86_556 ? N2 In1 O3 153.0(3) 150_665 164_557 ? N2 In1 O3 74.5(3) 164_557 164_557 ? N1 In1 O3 84.9(3) . 164_557 ? N1 In1 O3 81.1(3) 86_556 164_557 ? N2 In1 O3 74.5(3) 150_665 150_665 ? N2 In1 O3 153.0(3) 164_557 150_665 ? N1 In1 O3 81.1(3) . 150_665 ? N1 In1 O3 84.9(3) 86_556 150_665 ? O3 In1 O3 79.1(5) 164_557 150_665 ? C5 N1 C1 105.3(10) . . ? C5 N1 In1 125.3(7) . . ? C1 N1 In1 128.5(8) . . ? C3 C1 N1 108.4(11) . . ? C3 C1 C2 133.5(12) . . ? N1 C1 C2 118.1(12) . . ? O1 C2 O2 126.1(13) . . ? O1 C2 C1 121.7(13) . . ? O2 C2 C1 112.2(14) . . ? N2 C5 N1 111.1(9) . . ? N2 C3 C1 107.2(10) . . ? N2 C3 C4 118.3(12) . . ? C1 C3 C4 134.5(12) . . ? C5 N2 C3 108.0(10) . . ? C5 N2 In1 136.7(8) . 156_466 ? C3 N2 In1 114.7(8) . 156_466 ? O4 C4 O3 128.8(14) . . ? O4 C4 C3 115.1(15) . . ? O3 C4 C3 116.0(12) . . ? C4 O3 In1 115.9(8) . 156_466 ? O5X O2X O5X 92(6) . 83_455 ? O5X O2X O3X 129(4) . . ? O5X O2X O3X 84(2) 83_455 . ? O5X O2X O3X 86(4) . 32_545 ? O5X O2X O3X 112(3) 83_455 32_545 ? O3X O2X O3X 50(2) . 32_545 ? O3X O3X O3X 60.000(4) 83_455 32_545 ? O3X O3X O2X 100.8(16) 83_455 . ? O3X O3X O2X 71(2) 32_545 . ? O3X O3X O2X 71(2) 83_455 42_535 ? O3X O3X O2X 100.8(16) 32_545 42_535 ? O2X O3X O2X 171(4) . 42_535 ? O3X O3X O2X 93.2(19) 83_455 86_446 ? O3X O3X O2X 58.8(16) 32_545 86_446 ? O2X O3X O2X 111(3) . 86_446 ? O2X O3X O2X 67(3) 42_535 86_446 ? O3X O3X O2X 58.8(16) 83_455 83_455 ? O3X O3X O2X 93.2(19) 32_545 83_455 ? O2X O3X O2X 67(3) . 83_455 ? O2X O3X O2X 111(3) 42_535 83_455 ? O2X O3X O2X 149(4) 86_446 83_455 ? O4X O4X O4X 60.000(13) 32_545 83_455 ? O4X O4X O7X 100(3) 32_545 . ? O4X O4X O7X 86(5) 83_455 . ? O2X O5X O2X 103(5) . 32_545 ? O2X O5X O7X 124(7) . 32_545 ? O2X O5X O7X 121(5) 32_545 32_545 ? O2X O5X O6X 149(6) . 32_545 ? O2X O5X O6X 77(3) 32_545 32_545 ? O7X O5X O6X 44(3) 32_545 32_545 ? O2X O5X O5X 52(5) . 83_455 ? O2X O5X O5X 87(2) 32_545 83_455 ? O7X O5X O5X 95(4) 32_545 83_455 ? O6X O5X O5X 97.3(19) 32_545 83_455 ? O2X O5X O5X 100(3) . 32_545 ? O2X O5X O5X 36(2) 32_545 32_545 ? O7X O5X O5X 97(3) 32_545 32_545 ? O6X O5X O5X 62(3) 32_545 32_545 ? O5X O5X O5X 60.000(8) 83_455 32_545 ? O2X O5X O6X 83(5) . . ? O2X O5X O6X 131(3) 32_545 . ? O7X O5X O6X 43(4) 32_545 . ? O6X O5X O6X 75(4) 32_545 . ? O5X O5X O6X 58(3) 83_455 . ? O5X O5X O6X 95(2) 32_545 . ? O7X O6X O7X 116(6) . 32_545 ? O7X O6X O5X 57(4) . 83_455 ? O7X O6X O5X 107(5) 32_545 83_455 ? O7X O6X O5X 107(5) . . ? O7X O6X O5X 55(4) 32_545 . ? O5X O6X O5X 60(3) 83_455 . ? O6X O7X O6X 122(6) . 83_455 ? O6X O7X O5X 79(5) . 83_455 ? O6X O7X O5X 82(6) 83_455 83_455 ? O6X O7X O4X 82(7) . . ? O6X O7X O4X 102(6) 83_455 . ? O5X O7X O4X 160(6) 83_455 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.946 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.135